
data_Exp2_p1_MHI
_database_code_depnum_ccdc_archive 'CCDC 2521578'
loop_
_audit_author_name
_audit_author_address
'Katarzyna Skrzynska'
;ESRF
France
;
_audit_update_record             
;
2026-01-09 deposited with the CCDC.	2026-01-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_GEOM001_Exp2_p1_MHI         
;
PROBLEM: _geom_bond_atom_site_label_1 is missing
RESPONSE: The structure consists of water and methane molecules held together by hydrogen bonds and van der Waals interactions. There are no classical covalent bonds defined in this structure, therefore the geometry bond list is not applicable.
;
_vrf_GEOM002_Exp2_p1_MHI         
;
PROBLEM: _geom_bond_atom_site_label_2 is missing
RESPONSE: The structure consists of water and methane molecules held together by hydrogen bonds and van der Waals interactions. There are no classical covalent bonds defined in this structure, therefore the geometry bond list is not applicable.
;
_vrf_GEOM003_Exp2_p1_MHI         
;
PROBLEM: _geom_bond_distance is missing
RESPONSE: The structure consists of water and methane molecules held together by hydrogen bonds and van der Waals interactions. There are no classical covalent bonds defined in this structure, therefore the geometry bond list is not applicable.
;
_vrf_GEOM006_Exp2_p1_MHI         
;
PROBLEM: _geom_angle_atom_site_label_2 is missing
RESPONSE: The structure consists of water and methane molecules held together by hydrogen bonds and van der Waals interactions. There are no classical covalent bonds defined in this structure, therefore the geometry bond list is not applicable.
;
_vrf_GEOM007_Exp2_p1_MHI         
;
PROBLEM: _geom_angle_atom_site_label_3 is missing
RESPONSE: The structure consists of water and methane molecules held together by hydrogen bonds and van der Waals interactions. There are no classical covalent bonds defined in this structure, therefore the geometry bond list is not applicable.
;
_vrf_GEOM008_Exp2_p1_MHI         
;
PROBLEM: _geom_angle is missing
RESPONSE: The structure consists of water and methane molecules held together by hydrogen bonds and van der Waals interactions. There are no classical covalent bonds defined in this structure, therefore the geometry bond list is not applicable.
;
_vrf_PLAT049_Exp2_p1_MHI         
;
PROBLEM: Calculated Density Less Than 1.0 gcm-3 .........     0.8563 Check
RESPONSE: The structure consists of an open, porous water framework containing cages populated by methane molecules, resulting in a lower density compared to compact ice phases.
;
# Added during the CSD deposition process: Friday 09 January 2026 10:08 AM
# end Validation Reply Form

_audit_creation_date             2025-12-03
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_shelx_SHELXL_version_number     2019/3
_audit_contact_author_address    ?
_audit_contact_author_email      ?
_audit_contact_author_phone      ?
_publ_contact_author_id_orcid    ?
_publ_section_references         
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common            ?
_chemical_name_systematic        'methane clathrate hydrate'
_chemical_formula_moiety         '46(O), 7.803(C)'
_chemical_formula_sum            'C7.80 O46'
_chemical_formula_weight         829.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0004 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0008 0.0015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           223
_space_group_name_H-M_alt        'P m -3 n'
_space_group_name_Hall           '-P 4n 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'x+1/2, z+1/2, -y+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'x+1/2, -z+1/2, y+1/2'
'z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y-1/2, -x-1/2, z-1/2'
'y-1/2, x-1/2, z-1/2'
'-y-1/2, x-1/2, -z-1/2'
'y-1/2, -x-1/2, -z-1/2'
'-x-1/2, -z-1/2, y-1/2'
'x-1/2, -z-1/2, -y-1/2'
'x-1/2, z-1/2, y-1/2'
'-x-1/2, z-1/2, -y-1/2'
'-z-1/2, -y-1/2, x-1/2'
'-z-1/2, y-1/2, -x-1/2'
'z-1/2, -y-1/2, -x-1/2'
'z-1/2, y-1/2, x-1/2'

_cell_length_a                   11.7177(4)
_cell_length_b                   11.7177(4)
_cell_length_c                   11.7177(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1608.89(16)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    586
_cell_measurement_temperature    296.15
_cell_measurement_pressure       643000(10000)
_cell_measurement_theta_max      15.7280
_cell_measurement_theta_min      2.0390
_shelx_estimated_absorpt_T_max   0.997
_shelx_estimated_absorpt_T_min   0.997
_exptl_absorpt_coefficient_mu    0.027
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.125a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    0.856
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             415
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0848
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2372
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        12.961
_diffrn_reflns_theta_max         14.427
_diffrn_reflns_theta_min         2.239
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    3.00    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0283163000
_diffrn_orient_matrix_UB_12      0.0059070000
_diffrn_orient_matrix_UB_13      -0.0136061000
_diffrn_orient_matrix_UB_21      0.0142655000
_diffrn_orient_matrix_UB_22      0.0187132000
_diffrn_orient_matrix_UB_23      -0.0214975000
_diffrn_orient_matrix_UB_31      0.0041242000
_diffrn_orient_matrix_UB_32      -0.0251441000
_diffrn_orient_matrix_UB_33      -0.0191344000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.3738
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                282
_reflns_number_total             377
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.43.125a (Rigaku OD, 2024)'
_computing_data_collection       
'CrysAlisPro 1.171.43.125a (Rigaku OD, 2024) (IMPORT)'
_computing_data_reduction        'CrysAlisPro 1.171.43.125a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.215
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     15
_refine_ls_number_reflns         377
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0852
_refine_ls_restrained_S_all      1.215
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1801P)²+0.2283P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2980
_refine_ls_wR_factor_ref         0.3265
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.250000 0.000000 0.500000 0.0662(13) Uani 1 8 d S T P . .
O2 O 0.18349(13) 0.18349(13) 0.18349(13) 0.0661(12) Uani 1 3 d S T P . .
O3 O 0.000000 0.30864(19) 0.11627(18) 0.0664(12) Uani 1 2 d S T P . .
C2 C 0.000000 0.000000 0.000000 0.070(4) Uiso 0.90(4) 24 d S . . . .
C1 C 0.250000 0.500000 0.000000 0.143(4) Uiso 1 8 d S . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_axis.id
_axis.system
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source abstract . source . . . 0.99988448 0.00000000 -0.01519966
omega abstract rotation goniometer -1 . 0.24580000 0.00000000 0.00000000
1.00000000
kappa abstract rotation goniometer -1 omega 0.02855000 -0.76604444 0.00000000
0.64278761
phi abstract rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta abstract rotation goniometer -1 . -0.75487000 0.00000000 0.00000000
1.00000000
matrixX abstract general general . phi . 1.00000000 0.00000000 0.00000000
matrixY abstract general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ abstract general general . phi . 0.00000000 0.00000000 1.00000000
dacX abstract translation general . phi . 0.00000000 1.00000000 0.00000000
dacY abstract translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ abstract translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 9.292
_oxdiff_exptl_absorpt_empirical_full_min 0.335

data_Exp2_p2_MHIIa
_database_code_depnum_ccdc_archive 'CCDC 2521549'
loop_
_audit_author_name
_audit_author_address
'Katarzyna Skrzynska'
;ESRF
France
;
_audit_update_record             
;
2026-01-09 deposited with the CCDC.	2026-01-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_GEOM001_Exp2_p2_MHIIa       
;
PROBLEM: _geom_bond_atom_site_label_1 is missing
RESPONSE: The structure consists of water and methane molecules held together by hydrogen bonds and van der Waals interactions. There are no classical covalent bonds defined in this structure, therefore the geometry bond list is not applicable.
;
_vrf_GEOM002_Exp2_p2_MHIIa       
;
PROBLEM: _geom_bond_atom_site_label_2 is missing
RESPONSE: The structure consists of water and methane molecules held together by hydrogen bonds and van der Waals interactions. There are no classical covalent bonds defined in this structure, therefore the geometry bond list is not applicable.
;
_vrf_GEOM003_Exp2_p2_MHIIa       
;
PROBLEM: _geom_bond_distance is missing
RESPONSE: The structure consists of water and methane molecules held together by hydrogen bonds and van der Waals interactions. There are no classical covalent bonds defined in this structure, therefore the geometry bond list is not applicable.
;
_vrf_GEOM006_Exp2_p2_MHIIa       
;
PROBLEM: _geom_angle_atom_site_label_2 is missing
RESPONSE: The structure consists of water and methane molecules held together by hydrogen bonds and van der Waals interactions. There are no classical covalent bonds defined in this structure, therefore the geometry bond list is not applicable.
;
_vrf_GEOM007_Exp2_p2_MHIIa       
;
PROBLEM: _geom_angle_atom_site_label_3 is missing
RESPONSE: The structure consists of water and methane molecules held together by hydrogen bonds and van der Waals interactions. There are no classical covalent bonds defined in this structure, therefore the geometry bond list is not applicable.
;
_vrf_GEOM008_Exp2_p2_MHIIa       
;
PROBLEM: _geom_angle is missing
RESPONSE: The structure consists of water and methane molecules held together by hydrogen bonds and van der Waals interactions. There are no classical covalent bonds defined in this structure, therefore the geometry bond list is not applicable.
;
_vrf_PLAT049_Exp2_p2_MHIIa       
;
PROBLEM: Calculated Density Less Than 1.0 gcm-3 .........     0.8317 Check
RESPONSE: The structure consists of an open, porous water framework containing cages populated by methane molecules, resulting in a lower density compared to compact ice phases.
;
# Added during the CSD deposition process: Friday 09 January 2026 10:11 AM
# end Validation Reply Form

_audit_creation_date             2025-12-03
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_shelx_SHELXL_version_number     2019/3
_audit_contact_author_address    ?
_audit_contact_author_email      ?
_audit_contact_author_phone      ?
_publ_contact_author_id_orcid    ?
_publ_section_references         
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common            ?
_chemical_name_systematic        'methane clathrate hydrate'
_chemical_formula_moiety         '34(O), 5.964(C)'
_chemical_formula_sum            'C5.96 O34'
_chemical_formula_weight         615.58
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0004 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0008 0.0015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           191
_space_group_name_H-M_alt        'P 6/m m m'
_space_group_name_Hall           '-P 6 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
'y, -x+y, z'
'x-y, x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z'
'-x+y, y, -z'
'x, x-y, -z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z'
'x-y, -y, z'
'-x, -x+y, z'

_cell_length_a                   11.9113(17)
_cell_length_b                   11.9113(17)
_cell_length_c                   10.0025(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1229.0(4)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    244
_cell_measurement_temperature    296.15
_cell_measurement_pressure       1080000(20000)
_cell_measurement_theta_max      14.3000
_cell_measurement_theta_min      2.3790
_shelx_estimated_absorpt_T_max   0.997
_shelx_estimated_absorpt_T_min   0.997
_exptl_absorpt_coefficient_mu    0.026
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19045
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.70a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    0.832
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             308
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0728
_diffrn_reflns_Laue_measured_fraction_full 0.828
_diffrn_reflns_Laue_measured_fraction_max 0.834
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1947
_diffrn_reflns_point_group_measured_fraction_full 0.828
_diffrn_reflns_point_group_measured_fraction_max 0.834
_diffrn_reflns_theta_full        12.961
_diffrn_reflns_theta_max         14.429
_diffrn_reflns_theta_min         2.380
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.828
_diffrn_measured_fraction_theta_max 0.834
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -29.00  18.50   0.50    0.50    --    0.00   0.00   0.00   95
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0135194000
_diffrn_orient_matrix_UB_12      -0.0358471000
_diffrn_orient_matrix_UB_13      0.0009300000
_diffrn_orient_matrix_UB_21      0.0117627000
_diffrn_orient_matrix_UB_22      0.0009250000
_diffrn_orient_matrix_UB_23      -0.0348651000
_diffrn_orient_matrix_UB_31      0.0314871000
_diffrn_orient_matrix_UB_32      0.0050503000
_diffrn_orient_matrix_UB_33      0.0134474000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.3738
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                367
_reflns_number_total             551
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.43.70a (Rigaku OD, 2023)'
_computing_data_collection       
'CrysAlisPro 1.171.43.70a (Rigaku OD, 2023) (IMPORT)'
_computing_data_reduction        'CrysAlisPro 1.171.43.70a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.214
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     26
_refine_ls_number_reflns         551
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1194
_refine_ls_R_factor_gt           0.0987
_refine_ls_restrained_S_all      1.214
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2865
_refine_ls_wR_factor_ref         0.3305
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.13291(17) 0.2658(3) 0.000000 0.0642(11) Uani 1 4 d S T P . .
O2 O 0.333333 0.666667 0.1367(3) 0.0638(12) Uani 1 6 d S T P . .
O3 O 0.20845(12) 0.4169(2) 0.2230(2) 0.0680(10) Uani 1 2 d S T P . .
O4 O 0.3864(4) 0.000000 0.36214(19) 0.0926(13) Uani 1 2 d S T P . .
C1 C 0.500000 0.000000 0.000000 0.075(2) Uiso 1 8 d S . P . .
C2 C 0.333333 0.666667 0.500000 0.075(4) Uiso 0.79(3) 12 d S . . . .
C3 C 0.000000 0.000000 0.214(2) 0.131(11) Uiso 0.69(5) 12 d S . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_axis.id
_axis.system
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source abstract . source . . . 0.99988448 0.00000000 -0.01519966
omega abstract rotation goniometer -1 . 0.24580000 0.00000000 0.00000000
1.00000000
kappa abstract rotation goniometer -1 omega 0.02855000 -0.76604444 0.00000000
0.64278761
phi abstract rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta abstract rotation goniometer -1 . -0.75487000 0.00000000 0.00000000
1.00000000
matrixX abstract general general . phi . 1.00000000 0.00000000 0.00000000
matrixY abstract general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ abstract general general . phi . 0.00000000 0.00000000 1.00000000
dacX abstract translation general . phi . 0.00000000 1.00000000 0.00000000
dacY abstract translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ abstract translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.511
_oxdiff_exptl_absorpt_empirical_full_min 0.256

data_Exp2_p4_MHIIa
_database_code_depnum_ccdc_archive 'CCDC 2521550'
loop_
_audit_author_name
_audit_author_address
'Katarzyna Skrzynska'
;ESRF
France
;
_audit_update_record             
;
2026-01-09 deposited with the CCDC.	2026-01-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_Exp2_p4_MHIIa       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.882 Why?
RESPONSE: The low data completeness is due to the physical restrictions of the Diamond Anvil Cell and specific crystal orientation regarding to the beam.
;
_vrf_PLAT049_Exp2_p4_MHIIa       
;
PROBLEM: Calculated Density Less Than 1.0 gcm-3 .........     0.8778 Check
RESPONSE: The structure consists of an open, porous water framework containing cages populated by methane molecules, resulting in a lower density compared to compact ice phases.
;
# Added during the CSD deposition process: Friday 09 January 2026 10:12 AM
# end Validation Reply Form

_audit_creation_date             2025-12-03
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_shelx_SHELXL_version_number     2019/3
_audit_contact_author_address    ?
_audit_contact_author_email      ?
_audit_contact_author_phone      ?
_publ_contact_author_id_orcid    ?
_publ_section_references         
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common            ?
_chemical_name_systematic        'methane clathrate hydrate'
_chemical_formula_moiety         '34(O), 8.296(C)'
_chemical_formula_sum            'C8.30 O34'
_chemical_formula_weight         643.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0004 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0008 0.0015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           191
_space_group_name_H-M_alt        'P 6/m m m'
_space_group_name_Hall           '-P 6 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
'y, -x+y, z'
'x-y, x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z'
'-x+y, y, -z'
'x, x-y, -z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z'
'x-y, -y, z'
'-x, -x+y, z'

_cell_length_a                   11.8749(10)
_cell_length_b                   11.8749(10)
_cell_length_c                   9.9707(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1217.6(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    264
_cell_measurement_temperature    296.15
_cell_measurement_pressure       1170000(10000)
_cell_measurement_theta_max      12.9460
_cell_measurement_theta_min      1.4910
_shelx_estimated_absorpt_T_max   0.997
_shelx_estimated_absorpt_T_min   0.997
_exptl_absorpt_coefficient_mu    0.027
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.125a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    0.878
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             322
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.882
_diffrn_reflns_Laue_measured_fraction_max 0.878
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2119
_diffrn_reflns_point_group_measured_fraction_full 0.882
_diffrn_reflns_point_group_measured_fraction_max 0.878
_diffrn_reflns_theta_full        12.961
_diffrn_reflns_theta_max         14.405
_diffrn_reflns_theta_min         2.344
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.882
_diffrn_measured_fraction_theta_max 0.878
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -28.50  32.00   0.50    5.00    --    0.00   0.00   0.00  121
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0298923000
_diffrn_orient_matrix_UB_12      0.0029190000
_diffrn_orient_matrix_UB_13      -0.0028926000
_diffrn_orient_matrix_UB_21      -0.0167376000
_diffrn_orient_matrix_UB_22      -0.0315463000
_diffrn_orient_matrix_UB_23      -0.0185001000
_diffrn_orient_matrix_UB_31      -0.0122468000
_diffrn_orient_matrix_UB_32      -0.0177293000
_diffrn_orient_matrix_UB_33      0.0324212000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.3738
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                355
_reflns_number_total             574
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.43.125a (Rigaku OD, 2024)'
_computing_data_collection       
'CrysAlisPro 1.171.43.125a (Rigaku OD, 2024) (IMPORT)'
_computing_data_reduction        'CrysAlisPro 1.171.43.125a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     28
_refine_ls_number_reflns         574
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1137
_refine_ls_R_factor_gt           0.0834
_refine_ls_restrained_S_all      1.123
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1949P)²+0.0861P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2531
_refine_ls_wR_factor_ref         0.3114
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.13280(17) 0.2656(3) 0.000000 0.0636(11) Uani 1 4 d S T P . .
O2 O 0.333333 0.666667 0.1362(3) 0.0636(13) Uani 1 6 d S T P . .
O3 O 0.20842(12) 0.4168(2) 0.2230(2) 0.0675(10) Uani 1 2 d S T P . .
O4 O 0.3854(3) 0.000000 0.3626(2) 0.0885(13) Uani 1 2 d S T P . .
C1 C 0.500000 0.000000 0.000000 0.074(2) Uiso 1 8 d S . P . .
C2 C 0.333333 0.666667 0.500000 0.094(3) Uiso 1 12 d S . P . .
C3 C 0.000000 0.000000 0.224(3) 0.199(9) Uiso 1 12 d S . P . .
C4 C 0.168(5) 0.046(6) 0.500000 0.14(3) Uiso 0.108(18) 2 d S . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C4 C4 0.89(11) 21 ?
C4 C4 1.78(5) 15_556 ?
C4 C4 1.78(5) 14_556 ?
C4 C4 0.95(11) 8_556 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 C4 C4 150.00(4) 21 8_556 ?
C4 C4 C4 14.5(18) 8_556 14_556 ?
C4 C4 C4 135.5(18) 21 14_556 ?
C4 C4 C4 15.5(18) 21 15_556 ?
C4 C4 C4 119.999(17) 15_556 14_556 ?
C4 C4 C4 134.5(18) 8_556 15_556 ?

loop_
_axis.id
_axis.system
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source abstract . source . . . 0.99988448 0.00000000 -0.01519966
omega abstract rotation goniometer -1 . 0.24580000 0.00000000 0.00000000
1.00000000
kappa abstract rotation goniometer -1 omega 0.02855000 -0.76604444 0.00000000
0.64278761
phi abstract rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta abstract rotation goniometer -1 . -0.75487000 0.00000000 0.00000000
1.00000000
matrixX abstract general general . phi . 1.00000000 0.00000000 0.00000000
matrixY abstract general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ abstract general general . phi . 0.00000000 0.00000000 1.00000000
dacX abstract translation general . phi . 0.00000000 1.00000000 0.00000000
dacY abstract translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ abstract translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 10.565
_oxdiff_exptl_absorpt_empirical_full_min 0.525

data_Exp2_p5_MHIIb
_database_code_depnum_ccdc_archive 'CCDC 2521551'
loop_
_audit_author_name
_audit_author_address
'Katarzyna Skrzynska'
;ESRF
France
;
_audit_update_record             
;
2026-01-09 deposited with the CCDC.	2026-01-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_GEOM001_Exp2_p5_MHIIb       
;
PROBLEM: _geom_bond_atom_site_label_1 is missing
RESPONSE: The structure consists of water and methane molecules held together by hydrogen bonds and van der Waals interactions. There are no classical covalent bonds defined in this structure, therefore the geometry bond list is not applicable.
;
_vrf_GEOM002_Exp2_p5_MHIIb       
;
PROBLEM: _geom_bond_atom_site_label_2 is missing
RESPONSE: The structure consists of water and methane molecules held together by hydrogen bonds and van der Waals interactions. There are no classical covalent bonds defined in this structure, therefore the geometry bond list is not applicable.
;
_vrf_GEOM003_Exp2_p5_MHIIb       
;
PROBLEM: _geom_bond_distance is missing
RESPONSE: The structure consists of water and methane molecules held together by hydrogen bonds and van der Waals interactions. There are no classical covalent bonds defined in this structure, therefore the geometry bond list is not applicable.
;
_vrf_GEOM006_Exp2_p5_MHIIb       
;
PROBLEM: _geom_angle_atom_site_label_2 is missing
RESPONSE: The structure consists of water and methane molecules held together by hydrogen bonds and van der Waals interactions. There are no classical covalent bonds defined in this structure, therefore the geometry bond list is not applicable.
;
_vrf_GEOM007_Exp2_p5_MHIIb       
;
PROBLEM: _geom_angle_atom_site_label_3 is missing
RESPONSE: The structure consists of water and methane molecules held together by hydrogen bonds and van der Waals interactions. There are no classical covalent bonds defined in this structure, therefore the geometry bond list is not applicable.
;
_vrf_GEOM008_Exp2_p5_MHIIb       
;
PROBLEM: _geom_angle is missing
RESPONSE: The structure consists of water and methane molecules held together by hydrogen bonds and van der Waals interactions. There are no classical covalent bonds defined in this structure, therefore the geometry bond list is not applicable.
;
_vrf_PLAT029_Exp2_p5_MHIIb       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.868 Why?
RESPONSE: The low data completeness is due to the physical restrictions of the Diamond Anvil Cell and specific crystal orientation regarding to the beam.
;
_vrf_PLAT049_Exp2_p5_MHIIb       
;
PROBLEM: Calculated Density Less Than 1.0 gcm-3 .........     0.9029 Check
RESPONSE: The structure consists of an open, porous water framework containing cages populated by methane molecules, resulting in a lower density compared to compact ice phases.
;
# Added during the CSD deposition process: Friday 09 January 2026 10:20 AM
# end Validation Reply Form

_audit_creation_date             2025-12-03
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_shelx_SHELXL_version_number     2019/3
_audit_contact_author_address    ?
_audit_contact_author_email      ?
_audit_contact_author_phone      ?
_publ_contact_author_id_orcid    ?
_publ_section_references         
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common            ?
_chemical_name_systematic        'methane clathrate hydrate'
_chemical_formula_moiety         '34(O), 9.121(C)'
_chemical_formula_sum            'C9.12 O34'
_chemical_formula_weight         653.53
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0004 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0008 0.0015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           189
_space_group_name_H-M_alt        'P -6 2 m'
_space_group_name_Hall           'P -6 -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, z'
'x-y, -y, z'
'-x, -x+y, z'

_cell_length_a                   11.8160(8)
_cell_length_b                   11.8160(8)
_cell_length_c                   9.9420(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1202.11(18)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    295
_cell_measurement_temperature    296.15
_cell_measurement_pressure       1450000(20000)
_cell_measurement_theta_max      14.0610
_cell_measurement_theta_min      1.8140
_shelx_estimated_absorpt_T_max   0.997
_shelx_estimated_absorpt_T_min   0.997
_exptl_absorpt_coefficient_mu    0.028
_exptl_absorpt_correction_T_max  0.99925
_exptl_absorpt_correction_T_min  0.99925
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.125a (Rigaku Oxford Diffraction, 2024)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    0.903
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             327
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_crystal_size_rad          0.400
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.868
_diffrn_reflns_Laue_measured_fraction_max 0.859
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1351
_diffrn_reflns_point_group_measured_fraction_full 0.760
_diffrn_reflns_point_group_measured_fraction_max 0.748
_diffrn_reflns_theta_full        12.961
_diffrn_reflns_theta_max         14.429
_diffrn_reflns_theta_min         2.396
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.868
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -29.00  18.00   0.50    5.00    --    0.00   0.00   0.00   94
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0152690000
_diffrn_orient_matrix_UB_12      0.0197363000
_diffrn_orient_matrix_UB_13      0.0105635000
_diffrn_orient_matrix_UB_21      0.0296020000
_diffrn_orient_matrix_UB_22      0.0304081000
_diffrn_orient_matrix_UB_23      -0.0118181000
_diffrn_orient_matrix_UB_31      -0.0149868000
_diffrn_orient_matrix_UB_32      -0.0044418000
_diffrn_orient_matrix_UB_33      -0.0340774000
_diffrn_oxdiff_ac3_digest_hkl    419daae6b47d6b490acebce9b1267f05453751
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.3738
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.536
_reflns_Friedel_fraction_full    0.614
_reflns_Friedel_fraction_max     0.604
_reflns_number_gt                583
_reflns_number_total             860
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.43.125a (Rigaku OD, 2024)'
_computing_data_collection       
'CrysAlisPro 1.171.43.125a (Rigaku OD, 2024) (IMPORT)'
_computing_data_reduction        'CrysAlisPro 1.171.43.125a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 
;
 Flack x determined using 146 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -10.0(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         860
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1125
_refine_ls_R_factor_gt           0.0884
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1689P)²+0.0989P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2454
_refine_ls_wR_factor_ref         0.2778
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.1332(6) 0.2678(4) 0.500000 0.0605(11) Uani 1 2 d S T P . .
O2 O 0.333333 0.666667 0.3639(3) 0.0580(12) Uani 1 3 d S T P . .
O3 O 0.2042(4) 0.4175(3) 0.2765(3) 0.0655(10) Uani 1 1 d . . . . .
O4 O 0.6360(8) 0.000000 0.1365(6) 0.094(3) Uani 1 2 d S T P . .
O5 O 0.4073(7) 0.000000 0.1391(6) 0.086(2) Uani 1 2 d S T P . .
C1 C 0.5061(12) 0.000000 0.500000 0.067(2) Uiso 1 4 d S . P . .
C2 C 0.333333 0.666667 0.000000 0.082(3) Uiso 1 6 d S . P . .
C4 C 0.174(3) 0.000000 0.000000 0.151(18) Uiso 0.71(8) 4 d S . . . .
C3 C 0.000000 0.000000 0.7109(18) 0.120(5) Uiso 1 6 d S . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_axis.id
_axis.system
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source abstract . source . . . 0.99988448 0.00000000 -0.01519966
omega abstract rotation goniometer -1 . 0.24580000 0.00000000 0.00000000
1.00000000
kappa abstract rotation goniometer -1 omega 0.02855000 -0.76604444 0.00000000
0.64278761
phi abstract rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta abstract rotation goniometer -1 . -0.75487000 0.00000000 0.00000000
1.00000000
matrixX abstract general general . phi . 1.00000000 0.00000000 0.00000000
matrixY abstract general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ abstract general general . phi . 0.00000000 0.00000000 1.00000000
dacX abstract translation general . phi . 0.00000000 1.00000000 0.00000000
dacY abstract translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ abstract translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.851
_oxdiff_exptl_absorpt_empirical_full_min 0.621

data_Exp2_p3_decompression_MHIIa
_database_code_depnum_ccdc_archive 'CCDC 2521552'
loop_
_audit_author_name
_audit_author_address
'Katarzyna Skrzynska'
;ESRF
France
;
_audit_update_record             
;
2026-01-09 deposited with the CCDC.	2026-01-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_Exp2_p3_decompression_MHIIa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.821 Why?
RESPONSE: The low data completeness is due to the physical restrictions of the Diamond Anvil Cell and specific crystal orientation regarding to the beam.
;
_vrf_PLAT049_Exp2_p3_decompression_MHIIa 
;
PROBLEM: Calculated Density Less Than 1.0 gcm-3 .........     0.8755 Check
RESPONSE: The structure consists of an open, porous water framework containing cages populated by methane molecules, resulting in a lower density compared to compact ice phases.
;
# Added during the CSD deposition process: Friday 09 January 2026 10:16 AM
# end Validation Reply Form

_audit_creation_date             2025-12-03
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_shelx_SHELXL_version_number     2019/3
_audit_contact_author_address    ?
_audit_contact_author_email      ?
_audit_contact_author_phone      ?
_publ_contact_author_id_orcid    ?
_publ_section_references         
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common            ?
_chemical_name_systematic        'methane clathrate hydrate'
_chemical_formula_moiety         '34(O), 8.021(C)'
_chemical_formula_sum            'C8.02 O34'
_chemical_formula_weight         640.32
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0004 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0008 0.0015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           191
_space_group_name_H-M_alt        'P 6/m m m'
_space_group_name_Hall           '-P 6 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
'y, -x+y, z'
'x-y, x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z'
'-x+y, y, -z'
'x, x-y, -z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z'
'x-y, -y, z'
'-x, -x+y, z'

_cell_length_a                   11.868(2)
_cell_length_b                   11.868(2)
_cell_length_c                   9.9674(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1215.8(4)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    146
_cell_measurement_temperature    296.15
_cell_measurement_pressure       1140000(30000)
_cell_measurement_theta_max      14.3600
_cell_measurement_theta_min      2.0850
_shelx_estimated_absorpt_T_max   0.997
_shelx_estimated_absorpt_T_min   0.997
_exptl_absorpt_coefficient_mu    0.027
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24011
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.70a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    0.875
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.821
_diffrn_reflns_Laue_measured_fraction_max 0.820
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1265
_diffrn_reflns_point_group_measured_fraction_full 0.821
_diffrn_reflns_point_group_measured_fraction_max 0.820
_diffrn_reflns_theta_full        12.961
_diffrn_reflns_theta_max         14.412
_diffrn_reflns_theta_min         2.345
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.821
_diffrn_measured_fraction_theta_max 0.820
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -29.00  18.00   0.50    3.00    --    0.00   0.00   0.00   94
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0327228000
_diffrn_orient_matrix_UB_12      0.0029432000
_diffrn_orient_matrix_UB_13      0.0034572000
_diffrn_orient_matrix_UB_21      -0.0151884000
_diffrn_orient_matrix_UB_22      -0.0323534000
_diffrn_orient_matrix_UB_23      0.0169020000
_diffrn_orient_matrix_UB_31      -0.0043387000
_diffrn_orient_matrix_UB_32      -0.0162077000
_diffrn_orient_matrix_UB_33      -0.0332573000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.3738
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                249
_reflns_number_total             536
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.43.70a (Rigaku OD, 2023)'
_computing_data_collection       
'CrysAlisPro 1.171.43.70a (Rigaku OD, 2023) (IMPORT)'
_computing_data_reduction        'CrysAlisPro 1.171.43.70a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     30
_refine_ls_number_reflns         536
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1328
_refine_ls_R_factor_gt           0.0786
_refine_ls_restrained_S_all      0.982
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1839P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2354
_refine_ls_wR_factor_ref         0.2949
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.1338(2) 0.2677(5) 0.000000 0.0691(14) Uani 1 4 d S T P . .
O2 O 0.333333 0.666667 0.1362(4) 0.0642(15) Uani 1 6 d S T P . .
O3 O 0.20782(17) 0.4156(3) 0.2230(3) 0.0745(13) Uani 1 2 d S T P . .
O4 O 0.3842(4) 0.000000 0.3620(3) 0.0946(16) Uani 1 2 d S T P . .
C1 C 0.500000 0.000000 0.000000 0.077(3) Uiso 1 8 d S . P . .
C2 C 0.333333 0.666667 0.500000 0.093(6) Uiso 0.95(4) 12 d S . . . .
C3 C 0.000000 0.000000 0.209(3) 0.160(19) Uiso 0.75(8) 12 d S . . . .
C4 C 0.190(5) 0.046(6) 0.500000 0.14(3) Uiso 0.14(2) 2 d S . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C4 C4 0.94(12) 8_556 ?
C4 C4 1.17(11) 21 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 C4 C4 150.00(3) 8_556 21 ?

loop_
_axis.id
_axis.system
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source abstract . source . . . 0.99988448 0.00000000 -0.01519966
omega abstract rotation goniometer -1 . 0.24580000 0.00000000 0.00000000
1.00000000
kappa abstract rotation goniometer -1 omega 0.02855000 -0.76604444 0.00000000
0.64278761
phi abstract rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta abstract rotation goniometer -1 . -0.75487000 0.00000000 0.00000000
1.00000000
matrixX abstract general general . phi . 1.00000000 0.00000000 0.00000000
matrixY abstract general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ abstract general general . phi . 0.00000000 0.00000000 1.00000000
dacX abstract translation general . phi . 0.00000000 1.00000000 0.00000000
dacY abstract translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ abstract translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.948
_oxdiff_exptl_absorpt_empirical_full_min 0.604
