data_1-57_auto
_audit_creation_date               2026-03-19
_audit_creation_method
;
Olex2 1.5
(compiled 2026.03.18 svn.r0db52de7 for OlexSys, GUI svn.r7521)
;
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
D. Kratzert, I. Krossing, (2018), J. Appl. Cryst. 51, 928-934. 

Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Kratzert, D., Holstein, J.J. & Krossing, I. (2015). J. Appl. Cryst. 48, 933-938.

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

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           'F O4 P Sb, 0.5(H12 N2 O2)'
_chemical_formula_sum              'F H6 N O5 P Sb'
_chemical_formula_weight           271.78
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Sb' 'Sb' -0.5866 1.5461
 '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        'tetragonal'
_space_group_IT_number             87
_space_group_name_H-M_alt          'I 4/m'
_space_group_name_Hall             '-I 4'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, z'
 '-y, x, z'
 'y, -x, z'
 'x+1/2, y+1/2, z+1/2'
 '-x+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'
 '-x, -y, -z'
 'x, y, -z'
 'y, -x, -z'
 '-y, x, -z'
 '-x+1/2, -y+1/2, -z+1/2'
 'x+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'

_cell_length_a                     6.5646(2)
_cell_length_b                     6.5646(2)
_cell_length_c                     14.3955(6)
_cell_angle_alpha                  90
_cell_angle_beta                   90
_cell_angle_gamma                  90
_cell_volume                       620.36(5)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      2622
_cell_measurement_temperature      301.50(10)
_cell_measurement_theta_max        30.2070
_cell_measurement_theta_min        2.8130
_cell_oxdiff_angle_alpha           90.036(2)
_cell_oxdiff_angle_beta            89.988(2)
_cell_oxdiff_angle_gamma           90.000(2)
_cell_oxdiff_length_a              6.56531(18)
_cell_oxdiff_length_b              6.56500(18)
_cell_oxdiff_length_c              14.3933(4)
_cell_oxdiff_measurement_reflns_used  2622
_cell_oxdiff_volume                620.37(3)
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      4.686
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.69226
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.93a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              'clear light'
_exptl_crystal_colour_lustre       clear
_exptl_crystal_colour_modifier     light
_exptl_crystal_colour_primary      ?
_exptl_crystal_density_diffrn      2.910
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               512
_exptl_crystal_size_max            ?
_exptl_crystal_size_mid            ?
_exptl_crystal_size_min            ?
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0380
_diffrn_reflns_av_unetI/netI       0.0243
_diffrn_reflns_Laue_measured_fraction_full  1.000
_diffrn_reflns_Laue_measured_fraction_max  0.912
_diffrn_reflns_limit_h_max         8
_diffrn_reflns_limit_h_min         -9
_diffrn_reflns_limit_k_max         9
_diffrn_reflns_limit_k_min         -9
_diffrn_reflns_limit_l_max         19
_diffrn_reflns_limit_l_min         -19
_diffrn_reflns_number              3473
_diffrn_reflns_point_group_measured_fraction_full  1.000
_diffrn_reflns_point_group_measured_fraction_max  0.912
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           30.532
_diffrn_reflns_theta_min           2.830
_diffrn_ambient_environment        air
_diffrn_ambient_temperature        301.50(10)
_diffrn_detector                   'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean   10.0000
_diffrn_detector_type              HyPix
_diffrn_measured_fraction_theta_full  1.000
_diffrn_measured_fraction_theta_max  0.912
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω     -8.00  24.00   0.50    0.06    --   -8.45 -99.00 150.00   64
  2  ω    -64.00   9.00   0.50    0.06    --    8.21 -37.00 150.00  146
  3  ω     11.00  69.00   0.50    0.06    --    8.21  57.00  90.00  116
  4  ω    -33.00  60.00   0.50    0.06    --   -8.45  77.00 -60.00  186
  5  ω    -16.00  54.00   0.50    0.06    --    8.21  19.00 -30.00  140
  6  ω    -16.00  12.00   0.50    0.06    --   -8.45 -99.00 -90.00   56
;
_diffrn_measurement_device         'four-circle diffractometer'
_diffrn_measurement_device_type    'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method         'ω scans'
_diffrn_orient_matrix_type        
 'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11        0.0772965000
_diffrn_orient_matrix_UB_12        0.0696346000
_diffrn_orient_matrix_UB_13        -0.0132765000
_diffrn_orient_matrix_UB_21        -0.0204133000
_diffrn_orient_matrix_UB_22        -0.0208633000
_diffrn_orient_matrix_UB_23        -0.0474515000
_diffrn_orient_matrix_UB_31        -0.0726681000
_diffrn_orient_matrix_UB_32        0.0799311000
_diffrn_orient_matrix_UB_33        -0.0007775000
_diffrn_oxdiff_digest_hkl
;
01a5bd8422d570da8de1c5a96691d03a8f626f
;
_diffrn_radiation_monochromator    mirror
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             'Mo K\a'
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'Rotating-anode X-ray tube'
_diffrn_source_type                'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  440
_reflns_number_total               458
_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 1.171.43.93a (Rigaku OD, 2023)'
_computing_data_collection        
 'CrysAlisPro system (CCD 43.93a 64-bit (release 17-10-2023))'
_computing_data_reduction          'CrysAlisPro 1.171.43.93a (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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution      'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max           0.459
_refine_diff_density_min           -0.425
_refine_diff_density_rms           0.095
_refine_ls_extinction_coef         0.0069(4)
_refine_ls_extinction_expression  
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_extinction_method       'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref     1.100
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       25
_refine_ls_number_reflns           458
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0164
_refine_ls_R_factor_gt             0.0156
_refine_ls_restrained_S_all        1.100
_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)+(0.0079P)²+0.8777P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0315
_refine_ls_wR_factor_ref           0.0318
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All N(H,H,H) groups
2. Shared sites
{O2, N1}
3. Uiso/Uaniso restraints and constraints
Uanis(O2) = Uanis(N1)
4. Others
 Fixed Sof: O2(0.25) N1(0.25) H1A(0.25) H1B(0.25)
5.a Riding coordinates:
 N1(H2), N1(H1A,H1B)
;
_atom_sites_solution_hydrogens     difmap
_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
 Sb1 Sb 0.500000 0.500000 0.27829(2) 0.01403(12) Uani 1 4 d S T P . .
 P1 P 0.500000 1.000000 0.250000 0.0142(2) Uani 1 4 d S T P . .
 F1 F 0.500000 0.500000 0.41192(16) 0.0203(5) Uani 1 4 d S T P . .
 O1 O 0.5570(2) 0.8196(2) 0.31292(10) 0.0197(3) Uani 1 1 d . . . . .
 O2 O 0.7257(4) 0.8532(4) 0.500000 0.0361(6) Uani 0.5 2 d S T P A 3
 N1 N 0.7257(4) 0.8532(4) 0.500000 0.0361(6) Uani 0.5 2 d S T P B 4
 H2 H 0.647014 0.806995 0.449416 0.054 Uiso 1 1 d R U . . .
 H1A H 0.742091 0.998236 0.500000 0.054 Uiso 0.5 2 d R U P B 4
 H1B H 0.855798 0.786007 0.500000 0.054 Uiso 0.5 2 d R U P B 4


_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
 Sb1 F1 1.924(2) . ?
 Sb1 O1 2.1888(14) 3_655 ?
 Sb1 O1 2.1888(14) 2_665 ?
 Sb1 O1 2.1888(14) 4_565 ?
 Sb1 O1 2.1887(14) . ?
 P1 O1 1.5370(13) . ?
 P1 O1 1.5370(13) 2_675 ?
 P1 O1 1.5370(14) 16_655 ?
 P1 O1 1.5370(14) 15_465 ?
 O2 H2 0.9427 . ?
 O2 H2 1(10) 10_556 ?
 N1 H2 0.9427 . ?
 N1 H2 1(10) 10_556 ?
 N1 H1A 0.9584 . ?
 N1 H1B 0.9614 . ?

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
 F1 Sb1 O1 76.84(4) . . ?
 F1 Sb1 O1 76.84(4) . 4_565 ?
 F1 Sb1 O1 76.84(4) . 2_665 ?
 F1 Sb1 O1 76.84(4) . 3_655 ?
 O1 Sb1 O1 87.027(17) . 3_655 ?
 O1 Sb1 O1 153.67(8) 4_565 3_655 ?
 O1 Sb1 O1 153.67(8) . 2_665 ?
 O1 Sb1 O1 87.027(17) 4_565 2_665 ?
 O1 Sb1 O1 87.027(17) 2_665 3_655 ?
 O1 Sb1 O1 87.027(17) . 4_565 ?
 O1 P1 O1 110.32(5) . 15_465 ?
 O1 P1 O1 107.79(11) . 2_675 ?
 O1 P1 O1 110.32(5) . 16_655 ?
 O1 P1 O1 107.79(11) 15_465 16_655 ?
 O1 P1 O1 110.32(5) 15_465 2_675 ?
 O1 P1 O1 110.32(5) 2_675 16_655 ?
 P1 O1 Sb1 124.25(8) . . ?
 H2 O2 H2 101.2 . 10_556 ?
 H2 N1 H2 101.2 . 10_556 ?
 H2 N1 H1A 112.4 . . ?
 H2 N1 H1B 109.8 . . ?
 H1A N1 H2 112.4 . 10_556 ?
 H1A N1 H1B 110.8 . . ?
 H1B N1 H2 109.8 . 10_556 ?

loop_
  _geom_hbond_atom_site_label_D
  _geom_hbond_atom_site_label_H
  _geom_hbond_atom_site_label_A
  _geom_hbond_distance_DH
  _geom_hbond_distance_HA
  _geom_hbond_distance_DA
  _geom_hbond_angle_DHA
  _geom_hbond_site_symmetry_A
  _geom_hbond_publ_flag
 O2 H2 F1 0.94 2.30 3.029(3) 133.9 . yes
 O2 H2 O1 0.94 2.05 2.9202(18) 152.1 . yes
 N1 H2 F1 0.94 2.30 3.029(3) 133.9 . yes
 N1 H2 O1 0.94 2.05 2.9202(18) 152.1 . yes
 N1 H1A N1 0.96 1.95 2.889(4) 164.5 4_575 yes
 N1 H1B N1 0.96 1.95 2.889(4) 164.4 3_755 yes

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 O1 P1 O1 Sb1 26.37(11) 15_465 . . . ?
 O1 P1 O1 Sb1 146.88(12) 2_675 . . . ?
 O1 P1 O1 Sb1 -92.61(13) 16_655 . . . ?

_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  1.362
_oxdiff_exptl_absorpt_empirical_full_min  0.785

# END of CIF

data_1-8_auto
_audit_creation_date               2026-03-19
_audit_creation_method
;
Olex2 1.5
(compiled 2026.03.18 svn.r0db52de7 for OlexSys, GUI svn.r7521)
;
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
D. Kratzert, I. Krossing, (2018), J. Appl. Cryst. 51, 928-934.

Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Kratzert, D., Holstein, J.J. & Krossing, I. (2015). J. Appl. Cryst. 48, 933-938.

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

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           'F O7 P2 Sb, 2(H4 N)'
_chemical_formula_sum              'F H8 N2 O7 P2 Sb'
_chemical_formula_weight           350.77
_chemical_absolute_configuration   ?
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Sb' 'Sb' -0.5866 1.5461
 '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        'tetragonal'
_space_group_IT_number             100
_space_group_name_H-M_alt          'P 4 b m'
_space_group_name_Hall             'P 4 -2ab'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, z'
 '-y, x, z'
 'y, -x, z'
 'x+1/2, -y+1/2, z'
 '-x+1/2, y+1/2, z'
 '-y+1/2, -x+1/2, z'
 'y+1/2, x+1/2, z'

_cell_length_a                     8.5826(3)
_cell_length_b                     8.5826(3)
_cell_length_c                     5.8491(3)
_cell_angle_alpha                  90
_cell_angle_beta                   90
_cell_angle_gamma                  90
_cell_volume                       430.85(4)
_cell_formula_units_Z              2
_cell_measurement_reflns_used      2750
_cell_measurement_temperature      293(2)
_cell_measurement_theta_max        27.8540
_cell_measurement_theta_min        3.3500
_cell_oxdiff_angle_alpha           89.983(4)
_cell_oxdiff_angle_beta            89.991(4)
_cell_oxdiff_angle_gamma           89.976(4)
_cell_oxdiff_length_a              8.5809(4)
_cell_oxdiff_length_b              8.5825(4)
_cell_oxdiff_length_c              5.8503(2)
_cell_oxdiff_measurement_reflns_used  2750
_cell_oxdiff_volume                430.85(3)
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      3.604
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.68383
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.143a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              'clear light colourless'
_exptl_crystal_colour_lustre       clear
_exptl_crystal_colour_modifier     light
_exptl_crystal_colour_primary      colourless
_exptl_crystal_density_diffrn      2.704
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               336
_exptl_crystal_size_max            ?
_exptl_crystal_size_mid            ?
_exptl_crystal_size_min            ?
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0444
_diffrn_reflns_av_unetI/netI       0.0260
_diffrn_reflns_Laue_measured_fraction_full  1.000
_diffrn_reflns_Laue_measured_fraction_max  0.916
_diffrn_reflns_limit_h_max         12
_diffrn_reflns_limit_h_min         -11
_diffrn_reflns_limit_k_max         12
_diffrn_reflns_limit_k_min         -11
_diffrn_reflns_limit_l_max         8
_diffrn_reflns_limit_l_min         -6
_diffrn_reflns_number              5041
_diffrn_reflns_point_group_measured_fraction_full  0.965
_diffrn_reflns_point_group_measured_fraction_max  0.816
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           30.876
_diffrn_reflns_theta_min           3.357
_diffrn_ambient_temperature        293(2)
_diffrn_detector                   'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean   10.0000
_diffrn_detector_type              HyPix
_diffrn_measured_fraction_theta_full  1.000
_diffrn_measured_fraction_theta_max  0.916
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω     -1.00  28.00   0.50    0.78    --    5.85  57.00-150.00   58
  2  ω     31.00  78.00   0.50    0.78    --    5.85  57.00-150.00   94
  3  ω    -65.00 -13.00   0.50    0.78    --    5.85 -57.00 -90.00  104
  4  ω    -24.00  38.00   0.50    0.78    --    5.85 -95.00 112.00  124
  5  ω    -20.00   5.00   0.50    0.78    --   -6.08 -95.00 112.00   50
  6  ω    -21.00  21.00   0.50    0.78    --   -6.08 -99.00  60.00   84
  7  ω    -21.00  27.00   0.50    0.78    --   -6.08 -99.00 -60.00   96
  8  ω    -34.00  28.00   0.50    0.78    --   -6.08  95.00-136.00  124
;
_diffrn_measurement_device         'four-circle diffractometer'
_diffrn_measurement_device_type    'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method         'ω scans'
_diffrn_orient_matrix_type        
 'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11        0.0663009000
_diffrn_orient_matrix_UB_12        0.0401308000
_diffrn_orient_matrix_UB_13        0.0420600000
_diffrn_orient_matrix_UB_21        0.0452959000
_diffrn_orient_matrix_UB_22        -0.0686113000
_diffrn_orient_matrix_UB_23        -0.0126326000
_diffrn_orient_matrix_UB_31        0.0196270000
_diffrn_orient_matrix_UB_32        0.0226320000
_diffrn_orient_matrix_UB_33        -0.1130076000
_diffrn_radiation_monochromator    mirror
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             'Mo K\a'
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'Rotating-anode X-ray tube'
_diffrn_source_type                'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage           0.638
_reflns_Friedel_fraction_full      0.922
_reflns_Friedel_fraction_max       0.696
_reflns_number_gt                  545
_reflns_number_total               606
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         'CrysAlisPro 1.171.43.143a (Rigaku OD, 2024)'
_computing_data_collection        
 'CrysAlisPro system (CCD 43.143a 64-bit (release 25-10-2024))'
_computing_data_reduction          'CrysAlisPro 1.171.43.143a (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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution      'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max           0.366
_refine_diff_density_min           -0.415
_refine_diff_density_rms           0.083
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack     0.19(6)
_refine_ls_extinction_coef         0.0030(8)
_refine_ls_extinction_expression  
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_extinction_method       'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref     1.221
_refine_ls_hydrogen_treatment      refU
_refine_ls_matrix_type             full
_refine_ls_number_parameters       55
_refine_ls_number_reflns           606
_refine_ls_number_restraints       1
_refine_ls_R_factor_all            0.0309
_refine_ls_R_factor_gt             0.0244
_refine_ls_restrained_S_all        1.220
_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)+(0.0061P)²+0.2986P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0398
_refine_ls_wR_factor_ref           0.0411
_refine_special_details
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.81(6)
 0.19(6)
2. Others
 Sof(O2A)=1-FVAR(1)
 Sof(O2)=FVAR(1)
 Fixed Sof: O3(0.25)
3.a Riding coordinates:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens     difmap
_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
 Sb1 Sb 0.500000 0.500000 0.59112(16) 0.03554(19) Uani 1 4 d S T P . .
 P1 P 0.62236(13) 0.87764(13) 0.5539(3) 0.0286(4) Uani 1 2 d S T P . .
 O1 O 0.6314(4) 0.8686(4) 0.3011(9) 0.0452(13) Uani 1 2 d S T P A .
 O2 O 0.608(5) 0.724(2) 0.668(5) 0.058(8) Uani 0.47(6) 1 d . . P A 1
 F1 F 0.500000 0.500000 0.9187(9) 0.0403(14) Uani 1 4 d S T P A .
 O2A O 0.533(4) 0.7458(17) 0.673(5) 0.056(7) Uani 0.53(6) 1 d . . P A 2
 O3 O 0.5336(6) 1.0336(6) 0.6276(17) 0.030(3) Uani 0.5 2 d S T P A 2
 N1 N 0.3269(4) 0.8269(4) 1.0517(10) 0.0324(12) Uani 1 2 d S T P . .
 H1A H 0.344735 0.844736 1.214101 0.19(7) Uiso 1 2 d R . P . .
 H1B H 0.424069 0.795990 0.982939 0.12(3) Uiso 1 1 d R . . . .
 H1C H 0.247703 0.747704 1.037921 0.07(3) Uiso 1 2 d R . 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_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Sb1 O2 2.178(14) 2_665 ?
 Sb1 O2 2.178(14) 4_565 ?
 Sb1 O2 2.178(14) 3_655 ?
 Sb1 O2 2.178(14) . ?
 Sb1 F1 1.916(5) . ?
 Sb1 O2A 2.181(12) . ?
 Sb1 O2A 2.181(12) 4_565 ?
 Sb1 O2A 2.181(12) 2_665 ?
 Sb1 O2A 2.181(12) 3_655 ?
 P1 O1 1.483(5) . ?
 P1 O2 1.484(13) 7_665 ?
 P1 O2 1.484(13) . ?
 P1 O2A 1.534(11) . ?
 P1 O2A 1.534(11) 7_665 ?
 P1 O3 1.599(4) 2_675 ?
 P1 O3 1.599(4) . ?
 O3 O3 0.816(14) 2_675 ?
 N1 H1A 0.9744 . ?
 N1 H1B 0.9631 . ?
 N1 H1C 0.9645 . ?

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
 O2 Sb1 O2 87.6(3) 2_665 4_565 ?
 O2 Sb1 O2 87.6(3) 4_565 . ?
 O2 Sb1 O2 156.2(17) 2_665 . ?
 O2 Sb1 O2 156.2(17) 4_565 3_655 ?
 O2 Sb1 O2 87.6(3) 2_665 3_655 ?
 O2 Sb1 O2 87.6(3) . 3_655 ?
 O2 Sb1 O2A 70.0(4) 2_665 3_655 ?
 O2 Sb1 O2A 149.6(3) . 2_665 ?
 O2 Sb1 O2A 149.6(3) 4_565 3_655 ?
 O2 Sb1 O2A 104.6(4) . 3_655 ?
 O2 Sb1 O2A 17.7(4) 3_655 3_655 ?
 O2 Sb1 O2A 17.7(4) 4_565 4_565 ?
 O2 Sb1 O2A 104.6(4) 2_665 4_565 ?
 O2 Sb1 O2A 104.6(4) 3_655 2_665 ?
 O2 Sb1 O2A 149.6(3) 3_655 4_565 ?
 O2 Sb1 O2A 70.0(4) 4_565 2_665 ?
 O2 Sb1 O2A 17.7(4) 2_665 2_665 ?
 O2 Sb1 O2A 70.0(4) . 4_565 ?
 F1 Sb1 O2 78.1(8) . . ?
 F1 Sb1 O2 78.1(8) . 3_655 ?
 F1 Sb1 O2 78.1(8) . 2_665 ?
 F1 Sb1 O2 78.1(8) . 4_565 ?
 F1 Sb1 O2A 77.4(7) . . ?
 F1 Sb1 O2A 77.4(7) . 2_665 ?
 F1 Sb1 O2A 77.4(7) . 3_655 ?
 F1 Sb1 O2A 77.4(7) . 4_565 ?
 O2A Sb1 O2A 154.8(15) 4_565 3_655 ?
 O2A Sb1 O2A 87.3(3) 2_665 3_655 ?
 O2A Sb1 O2A 87.3(3) 4_565 . ?
 O2A Sb1 O2A 154.8(15) 2_665 . ?
 O2A Sb1 O2A 87.3(3) 4_565 2_665 ?
 O2A Sb1 O2A 87.3(3) 3_655 . ?
 O1 P1 O2 113.9(14) . 7_665 ?
 O1 P1 O2 113.9(14) . . ?
 O1 P1 O2A 116.0(10) . . ?
 O1 P1 O2A 116.0(11) . 7_665 ?
 O1 P1 O3 109.7(4) . 2_675 ?
 O1 P1 O3 109.7(4) . . ?
 O2 P1 O2 87.1(17) 7_665 . ?
 O2 P1 O2A 25.7(6) 7_665 7_665 ?
 O2 P1 O2A 107.8(19) . 7_665 ?
 O2 P1 O3 103.4(19) . 2_675 ?
 O2 P1 O3 125.7(19) 7_665 2_675 ?
 O2A P1 O3 79.0(10) . 2_675 ?
 O2A P1 O3 104.8(7) 7_665 2_675 ?
 O2A P1 O3 79.0(10) 7_665 . ?
 O2A P1 O3 104.8(7) . . ?
 O3 P1 O3 29.6(5) 2_675 . ?
 P1 O2 Sb1 136.7(8) . . ?
 P1 O2A Sb1 132.8(6) . . ?
 P1 O3 P1 136.4(5) 2_675 . ?
 O3 O3 P1 75.2(2) 2_675 . ?
 H1A N1 H1B 108.3 . . ?
 H1A N1 H1C 107.6 . . ?
 H1B N1 H1C 112.4 . . ?

loop_
  _geom_hbond_atom_site_label_D
  _geom_hbond_atom_site_label_H
  _geom_hbond_atom_site_label_A
  _geom_hbond_distance_DH
  _geom_hbond_distance_HA
  _geom_hbond_distance_DA
  _geom_hbond_angle_DHA
  _geom_hbond_site_symmetry_A
  _geom_hbond_publ_flag
 N1 H1A O1 0.97 2.52 3.015(6) 111.3 1_556 yes
 N1 H1A O1 0.97 2.52 3.015(6) 111.3 2_676 yes
 N1 H1B O2 0.96 2.50 3.41(5) 157.0 . yes
 N1 H1B O2A 0.96 2.09 2.919(10) 143.8 . yes
 N1 H1C O1 0.96 2.09 2.785(7) 127.7 3_656 yes
 N1 H1C O2 0.96 2.49 2.962(12) 110.1 3_655 yes
 N1 H1C O2 0.96 2.49 2.962(12) 110.1 5_465 yes

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 O1 P1 O2 Sb1 -33(5) . . . . ?
 O1 P1 O2A Sb1 32(4) . . . . ?
 O1 P1 O3 P1 46.8(9) . . . 2_675 ?
 O1 P1 O3 O3 95.43(13) . . . 2_675 ?
 O2 P1 O2 Sb1 -148(2) 7_665 . . . ?
 O2A P1 O2A Sb1 -120.6(19) 7_665 . . . ?
 O2A P1 O3 P1 160.7(16) 7_665 . . 2_675 ?
 O2A P1 O3 P1 -78.5(18) . . . 2_675 ?
 O2A P1 O3 O3 -29.8(15) . . . 2_675 ?
 O2A P1 O3 O3 -150.7(13) 7_665 . . 2_675 ?
 O3 P1 O2A Sb1 153(3) . . . . ?
 O3 P1 O2A Sb1 139(3) 2_675 . . . ?
 O3 P1 O3 P1 -48.7(9) 2_675 . . 2_675 ?

_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  1.652
_oxdiff_exptl_absorpt_empirical_full_min  0.763
loop_
  _twin_individual_id
  _twin_individual_mass_fraction_refined
 1 0.81(6)
 2 0.19(6)

# END of CIF

data_ly6-22-3
_audit_creation_date               2026-03-31
_audit_creation_method
;
Olex2 1.5
(compiled 2026.03.20 svn.r2bc28608 for OlexSys, GUI svn.r7530)
;
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_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          ?
_chemical_formula_moiety           'F5 H O3 P Sb2, H4 N'
_chemical_formula_sum              'F5 H5 N O3 P Sb2'
_chemical_formula_weight           436.52
_chemical_absolute_configuration   ?
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Sb' 'Sb' -0.5866 1.5461
 '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        'orthorhombic'
_space_group_IT_number             29
_space_group_name_H-M_alt          'P c a 21'
_space_group_name_Hall             'P 2c -2ac'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, z+1/2'
 'x+1/2, -y, z'
 '-x+1/2, y, z+1/2'

_cell_length_a                     8.9350(2)
_cell_length_b                     10.0427(3)
_cell_length_c                     8.8719(2)
_cell_angle_alpha                  90
_cell_angle_beta                   90
_cell_angle_gamma                  90
_cell_volume                       796.09(4)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      1777
_cell_measurement_temperature      293(2)
_cell_measurement_theta_max        28.3720
_cell_measurement_theta_min        3.8180
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      7.048
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.45583
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              'clear light colourless'
_exptl_crystal_colour_lustre       clear
_exptl_crystal_colour_modifier     light
_exptl_crystal_colour_primary      colourless
_exptl_crystal_density_diffrn      3.642
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               792
_exptl_crystal_size_max            ?
_exptl_crystal_size_mid            ?
_exptl_crystal_size_min            ?
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0350
_diffrn_reflns_av_unetI/netI       0.0510
_diffrn_reflns_Laue_measured_fraction_full  0.997
_diffrn_reflns_Laue_measured_fraction_max  0.998
_diffrn_reflns_limit_h_max         5
_diffrn_reflns_limit_h_min         -11
_diffrn_reflns_limit_k_max         12
_diffrn_reflns_limit_k_min         -6
_diffrn_reflns_limit_l_max         10
_diffrn_reflns_limit_l_min         -11
_diffrn_reflns_number              2751
_diffrn_reflns_point_group_measured_fraction_full  0.964
_diffrn_reflns_point_group_measured_fraction_max  0.959
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           26.364
_diffrn_reflns_theta_min           3.820
_diffrn_ambient_temperature        293(2)
_diffrn_detector                   'CCD plate'
_diffrn_detector_area_resol_mean   15.9595
_diffrn_detector_type              EosS2
_diffrn_measured_fraction_theta_full  0.997
_diffrn_measured_fraction_theta_max  0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -20.00  35.00   1.00    8.77    --   17.16 -99.00-120.00   55
  2  ω      1.00  85.00   1.00    8.77    --   17.16  77.00  30.00   84
  3  ω    -37.00  19.00   1.00    8.77    --  -17.39  38.00-150.00   56
;
_diffrn_measurement_device         'four-circle diffractometer'
_diffrn_measurement_device_type    'New Gemini, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method         'ω scans'
_diffrn_orient_matrix_type        
 'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11        0.0403867000
_diffrn_orient_matrix_UB_12        -0.0608155000
_diffrn_orient_matrix_UB_13        -0.0003171000
_diffrn_orient_matrix_UB_21        0.0678623000
_diffrn_orient_matrix_UB_22        0.0356548000
_diffrn_orient_matrix_UB_23        0.0096970000
_diffrn_orient_matrix_UB_31        -0.0081168000
_diffrn_orient_matrix_UB_32        -0.0045818000
_diffrn_orient_matrix_UB_33        0.0793362000
_diffrn_radiation_monochromator    graphite
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             'Mo K\a'
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'fine-focus sealed X-ray tube'
_diffrn_source_type                'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage           0.794
_reflns_Friedel_fraction_full      0.925
_reflns_Friedel_fraction_max       0.914
_reflns_number_gt                  1495
_reflns_number_total               1559
_reflns_odcompleteness_completeness  99.39
_reflns_odcompleteness_iscentric   1
_reflns_odcompleteness_theta       26.32
_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 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection         'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction          'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics      'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement    'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution      'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max           0.728
_refine_diff_density_min           -1.043
_refine_diff_density_rms           0.211
_refine_ls_abs_structure_details
;
 Flack x determined using 611 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack     -0.05(5)
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.110
_refine_ls_hydrogen_treatment      mixed
_refine_ls_matrix_type             full
_refine_ls_number_parameters       113
_refine_ls_number_reflns           1559
_refine_ls_number_restraints       11
_refine_ls_R_factor_all            0.0376
_refine_ls_R_factor_gt             0.0357
_refine_ls_restrained_S_all        1.118
_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)+(0.0279P)²+5.1870P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0848
_refine_ls_wR_factor_ref           0.0869
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All H(H) groups
2. Restrained distances
 H1B-H1D
 1.4 with sigma of 0.02
 H1B-H1A
 1.4 with sigma of 0.02
 H1D-H1A
 1.4 with sigma of 0.02
 H1B-H1C
 1.4 with sigma of 0.02
 H1D-H1C
 1.4 with sigma of 0.02
 H1A-H1C
 1.4 with sigma of 0.02
 N1-H1D = N1-H1C = N1-H1A = N1-H1B
 0.9 with sigma of 0.01
3.a Riding coordinates:
 O3(H1,H1A,H1B,H1C,H1D)
;
_atom_sites_solution_hydrogens     difmap
_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
 Sb1 Sb 0.45392(10) 0.32287(9) 0.18535(13) 0.0196(2) Uani 1 1 d . . . . .
 Sb2 Sb 0.49387(11) 0.23675(9) 0.64045(15) 0.0234(3) Uani 1 1 d . . . . .
 P1 P 0.2075(4) 0.4917(4) 0.3931(5) 0.0207(8) Uani 1 1 d . . . . .
 F1 F 0.2827(10) 0.1814(8) 0.1438(10) 0.034(2) Uani 1 1 d . . . . .
 F2 F 0.5224(12) 0.2028(12) 0.3704(12) 0.037(3) Uani 1 1 d . . . . .
 F3 F 0.4987(12) 0.1975(12) 0.8561(13) 0.036(3) Uani 1 1 d . . . . .
 F4 F 0.7103(10) 0.2093(9) 0.6409(13) 0.039(2) Uani 1 1 d . . . . .
 O1 O 0.3012(12) 0.3728(11) 0.3441(12) 0.026(2) Uani 1 1 d . . . . .
 F5 F 0.4804(11) 0.0447(8) 0.6174(12) 0.035(2) Uani 1 1 d . . . . .
 O2 O 0.1670(14) 0.4781(11) 0.5575(13) 0.032(3) Uani 1 1 d . . . . .
 N1 N 0.7506(14) 0.0043(11) 0.3908(14) 0.032(3) Uani 1 1 d D . . . .
 O3 O 0.0696(12) 0.5081(10) 0.2936(11) 0.032(3) Uani 1 1 d . . . . .
 H1 H 0.289349 0.598657 0.378882 0.06(6) Uiso 1 1 d R . . . .
 H1A H 0.804630 0.051616 0.454282 0.04(5) Uiso 1 1 d DR . . . .
 H1B H 0.681481 -0.039555 0.440891 0.2(2) Uiso 1 1 d DR . . . .
 H1C H 0.809406 -0.052519 0.344249 0.272 Uiso 1 1 d DR U . . .
 H1D H 0.708247 0.057531 0.324985 0.6(7) Uiso 1 1 d DR . . . .


_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
 Sb1 F1 2.120(8) . ?
 Sb1 F2 2.127(11) . ?
 Sb1 O1 2.024(11) . ?
 Sb1 O2 2.210(12) 4_554 ?
 Sb1 O3 2.207(10) 3_565 ?
 Sb2 F1 2.533(9) 4 ?
 Sb2 F2 2.433(11) . ?
 Sb2 F3 1.954(11) . ?
 Sb2 F4 1.953(9) . ?
 Sb2 F5 1.943(8) . ?
 P1 O1 1.521(11) . ?
 P1 O2 1.510(12) . ?
 P1 O3 1.525(10) . ?
 P1 H1 1.3056 . ?
 N1 H1A 0.8810 . ?
 N1 H1B 0.8786 . ?
 N1 H1C 0.8790 . ?
 N1 H1D 0.8777 . ?

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
 F1 Sb1 F2 87.8(4) . . ?
 F1 Sb1 O2 91.8(4) . 4_554 ?
 F1 Sb1 O3 158.3(4) . 3_565 ?
 F2 Sb1 O2 159.5(4) . 4_554 ?
 F2 Sb1 O3 88.0(4) . 3_565 ?
 O1 Sb1 F1 78.5(4) . . ?
 O1 Sb1 F2 78.3(4) . . ?
 O1 Sb1 O2 81.5(4) . 4_554 ?
 O1 Sb1 O3 79.8(4) . 3_565 ?
 O3 Sb1 O2 84.8(4) 3_565 4_554 ?
 F2 Sb2 F1 94.8(3) . 4 ?
 F3 Sb2 F1 88.1(4) . 4 ?
 F3 Sb2 F2 159.0(4) . . ?
 F4 Sb2 F1 159.2(3) . 4 ?
 F4 Sb2 F2 83.0(4) . . ?
 F4 Sb2 F3 87.0(4) . . ?
 F5 Sb2 F1 73.9(3) . 4 ?
 F5 Sb2 F2 76.3(4) . . ?
 F5 Sb2 F3 84.5(5) . . ?
 F5 Sb2 F4 85.5(4) . . ?
 O1 P1 O3 111.4(7) . . ?
 O1 P1 H1 108.1 . . ?
 O2 P1 O1 109.7(7) . . ?
 O2 P1 O3 112.1(7) . . ?
 O2 P1 H1 107.6 . . ?
 O3 P1 H1 107.9 . . ?
 Sb1 F1 Sb2 124.0(4) . 4_554 ?
 Sb1 F2 Sb2 130.6(5) . . ?
 P1 O1 Sb1 139.8(7) . . ?
 P1 O2 Sb1 132.6(7) . 4 ?
 H1A N1 H1B 109.4 . . ?
 H1A N1 H1C 108.8 . . ?
 H1A N1 H1D 109.4 . . ?
 H1B N1 H1C 109.4 . . ?
 H1B N1 H1D 109.8 . . ?
 H1C N1 H1D 109.9 . . ?
 P1 O3 Sb1 135.5(7) . 3_465 ?

loop_
  _geom_hbond_atom_site_label_D
  _geom_hbond_atom_site_label_H
  _geom_hbond_atom_site_label_A
  _geom_hbond_distance_DH
  _geom_hbond_distance_HA
  _geom_hbond_distance_DA
  _geom_hbond_angle_DHA
  _geom_hbond_site_symmetry_A
  _geom_hbond_publ_flag
 N1 H1A F3 0.88 2.45 2.980(17) 119.3 4_654 yes
 N1 H1A F4 0.88 2.44 3.048(16) 126.4 . yes
 N1 H1A F5 0.88 2.34 2.915(16) 122.6 3 yes
 N1 H1B F1 0.88 2.32 2.933(16) 127.1 2_655 yes
 N1 H1B F3 0.88 2.38 3.027(17) 130.5 2_654 yes
 N1 H1B F5 0.88 2.53 3.167(16) 130.1 . yes
 N1 H1C F1 0.88 2.21 2.892(15) 133.9 3 yes
 N1 H1C F2 0.88 2.44 3.203(17) 145.4 3 yes
 N1 H1D F2 0.88 2.25 2.857(16) 126.5 . yes
 N1 H1D F4 0.88 2.35 3.046(17) 136.4 4_654 yes

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 O1 P1 O2 Sb1 -58.1(11) . . . 4 ?
 O1 P1 O3 Sb1 -137.0(8) . . . 3_465 ?
 O2 P1 O1 Sb1 -155.9(10) . . . . ?
 O2 P1 O3 Sb1 99.7(10) . . . 3_465 ?
 O3 P1 O1 Sb1 79.5(12) . . . . ?
 O3 P1 O2 Sb1 66.1(11) . . . 4 ?

_olex2_date_sample_data_collection  2021-12-13
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max  1.727
_oxdiff_exptl_absorpt_empirical_full_min  0.715


# END of CIF

data_2-23_auto
_audit_creation_date               2024-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_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          ?
_chemical_formula_moiety           'As O3 Sb'
_chemical_formula_sum              'As O3 Sb'
_chemical_formula_weight           244.67
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Sb' 'Sb' -0.5866 1.5461
 '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        'monoclinic'
_space_group_IT_number             14
_space_group_name_H-M_alt          'P 1 21/n 1'
_space_group_name_Hall             '-P 2yn'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                     4.5687(3)
_cell_length_b                     13.1151(10)
_cell_length_c                     5.4155(4)
_cell_angle_alpha                  90
_cell_angle_beta                   94.900(7)
_cell_angle_gamma                  90
_cell_volume                       323.31(4)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      2302
_cell_measurement_temperature      299.13(10)
_cell_measurement_theta_max        30.1830
_cell_measurement_theta_min        3.0980
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      18.481
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.05183
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              colourless
_exptl_crystal_colour_primary      colourless
_exptl_crystal_density_diffrn      5.027
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               432
_exptl_crystal_size_max            ?
_exptl_crystal_size_mid            ?
_exptl_crystal_size_min            ?
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0416
_diffrn_reflns_av_unetI/netI       0.0359
_diffrn_reflns_Laue_measured_fraction_full  1.000
_diffrn_reflns_Laue_measured_fraction_max  0.816
_diffrn_reflns_limit_h_max         5
_diffrn_reflns_limit_h_min         -5
_diffrn_reflns_limit_k_max         16
_diffrn_reflns_limit_k_min         -17
_diffrn_reflns_limit_l_max         7
_diffrn_reflns_limit_l_min         -7
_diffrn_reflns_number              3240
_diffrn_reflns_point_group_measured_fraction_full  1.000
_diffrn_reflns_point_group_measured_fraction_max  0.816
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           30.627
_diffrn_reflns_theta_min           3.106
_diffrn_ambient_environment        air
_diffrn_ambient_temperature        299.13(10)
_diffrn_detector                   'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean   10.0000
_diffrn_detector_type              HyPix
_diffrn_measured_fraction_theta_full  1.000
_diffrn_measured_fraction_theta_max  0.816
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω      2.00  78.00   0.50    0.05    --    4.52  37.00 -30.00  152
  2  ω    -17.00  67.00   0.50    0.05    --    4.52  77.00  60.00  168
  3  ω    -43.00  -4.00   0.50    0.05    --    4.52 -19.00 120.00   78
  4  ω    -21.00  23.00   0.50    0.05    --    4.52 -99.00 -90.00   88
  5  ω    -21.00  27.00   0.50    0.05    --    4.52 -99.00-120.00   96
;
_diffrn_measurement_device         'four-circle diffractometer'
_diffrn_measurement_device_type    'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method         'ω scans'
_diffrn_orient_matrix_type        
 'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11        -0.0714628000
_diffrn_orient_matrix_UB_12        -0.0210953000
_diffrn_orient_matrix_UB_13        -0.1097535000
_diffrn_orient_matrix_UB_21        0.0022210000
_diffrn_orient_matrix_UB_22        0.0484016000
_diffrn_orient_matrix_UB_23        -0.0581913000
_diffrn_orient_matrix_UB_31        0.1385001000
_diffrn_orient_matrix_UB_32        -0.0117218000
_diffrn_orient_matrix_UB_33        -0.0429064000
_diffrn_oxdiff_digest_frames
;
01598a900748b8318886049e44fef25c84000903222
;
_diffrn_oxdiff_digest_hkl
;
01b93aafffdfd729fc6008844488d1e7945dc0
;
_diffrn_radiation_monochromator    mirror
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'Rotating-anode X-ray tube'
_diffrn_source_type                'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  755
_reflns_number_total               818
_reflns_odcompleteness_completeness  99.86
_reflns_odcompleteness_iscentric   1
_reflns_odcompleteness_theta       26.32
_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 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection         'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction          'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           1.246
_refine_diff_density_min           -2.195
_refine_diff_density_rms           0.476
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.102
_refine_ls_hydrogen_treatment      undef
_refine_ls_matrix_type             full
_refine_ls_number_parameters       46
_refine_ls_number_reflns           818
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0348
_refine_ls_R_factor_gt             0.0320
_refine_ls_restrained_S_all        1.102
_refine_ls_shift/su_max            0.001
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0482P)²+0.0192P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0785
_refine_ls_wR_factor_ref           0.0806
_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
 Sb1 Sb 0.50548(8) 0.85415(3) 0.82953(7) 0.01297(17) Uani 1 1 d . . . . .
 As1 As 0.53482(12) 0.59605(4) 0.75631(11) 0.01080(18) Uani 1 1 d . . . . .
 O1 O 0.6121(9) 0.6399(3) 0.4569(9) 0.0168(9) Uani 1 1 d . . . . .
 O2 O 0.1510(8) 0.5955(3) 0.6670(8) 0.0168(9) Uani 1 1 d . . . . .
 O3 O 0.5659(10) 0.7109(3) 0.9311(8) 0.0195(9) Uani 1 1 d . . . . .


_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
 Sb1 O1 1.981(4) 4_576 ?
 Sb1 O2 2.003(4) 4_676 ?
 Sb1 O3 1.970(4) . ?
 As1 O1 1.784(5) . ?
 As1 O2 1.779(4) . ?
 As1 O3 1.778(4) . ?

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
 O1 Sb1 O2 84.80(17) 4_576 4_676 ?
 O3 Sb1 O1 92.87(18) . 4_576 ?
 O3 Sb1 O2 91.85(18) . 4_676 ?
 O2 As1 O1 91.22(19) . . ?
 O3 As1 O1 101.4(2) . . ?
 O3 As1 O2 100.4(2) . . ?
 As1 O1 Sb1 125.8(2) . 4_675 ?
 As1 O2 Sb1 119.3(2) . 4_575 ?
 As1 O3 Sb1 131.0(2) . . ?

_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  17.315
_oxdiff_exptl_absorpt_empirical_full_min  0.474

# END of CIF

data_mo_ext074_0m_a
_audit_creation_date               2026-03-20
_audit_creation_method
;
Olex2 1.5
(compiled 2026.03.18 svn.r0db52de7 for OlexSys, GUI svn.r7521)
;
_shelx_SHELXL_version_number       '2014/7'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_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. (2008). Acta Cryst. A64, 112-122.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           '2(As1 O1.5), 1(Br), 2(H2 N0.5)'
_chemical_formula_sum              'As2 H4 Br N O3'
_chemical_formula_weight           295.79
_chemical_absolute_configuration   ?
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Br' 'Br' -0.2901 2.4595
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 '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             186
_space_group_name_H-M_alt          'P 63 m c'
_space_group_name_Hall             'P 6c -2c'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-y, x-y, z'
 '-x+y, -x, z'
 '-x, -y, z+1/2'
 'y, -x+y, z+1/2'
 'x-y, x, z+1/2'
 '-y, -x, z'
 '-x+y, y, z'
 'x, x-y, z'
 'y, x, z+1/2'
 'x-y, -y, z+1/2'
 '-x, -x+y, z+1/2'

_cell_length_a                     5.2576(5)
_cell_length_b                     5.2576(5)
_cell_length_c                     12.4246(18)
_cell_angle_alpha                  90
_cell_angle_beta                   90
_cell_angle_gamma                  120
_cell_volume                       297.43(7)
_cell_formula_units_Z              2
_cell_measurement_reflns_used      288
_cell_measurement_temperature      289(2)
_cell_measurement_theta_max        25.12
_cell_measurement_theta_min        3.28
_shelx_estimated_absorpt_T_max     0.775
_shelx_estimated_absorpt_T_min     0.390
_exptl_absorpt_coefficient_mu      17.859
_exptl_absorpt_correction_T_max    0.7461
_exptl_absorpt_correction_T_min    0.5230
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details    
 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1421 before and 0.0692 after correction. The Ratio of minimum to maximum transmission is 0.7010. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              colourless
_exptl_crystal_colour_primary      colourless
_exptl_crystal_density_diffrn      3.303
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         plate
_exptl_crystal_F_000               272
_exptl_crystal_size_max            0.065
_exptl_crystal_size_mid            0.065
_exptl_crystal_size_min            0.015
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0722
_diffrn_reflns_av_unetI/netI       0.0624
_diffrn_reflns_Laue_measured_fraction_full  0.992
_diffrn_reflns_Laue_measured_fraction_max  0.992
_diffrn_reflns_limit_h_max         6
_diffrn_reflns_limit_h_min         -5
_diffrn_reflns_limit_k_max         6
_diffrn_reflns_limit_k_min         -6
_diffrn_reflns_limit_l_max         14
_diffrn_reflns_limit_l_min         -14
_diffrn_reflns_number              1085
_diffrn_reflns_point_group_measured_fraction_full  0.996
_diffrn_reflns_point_group_measured_fraction_max  0.996
_diffrn_reflns_theta_full          25.001
_diffrn_reflns_theta_max           25.001
_diffrn_reflns_theta_min           3.279
_diffrn_ambient_temperature        289.5
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.992
_diffrn_measured_fraction_theta_max  0.992
_diffrn_measurement_device_type    'Bruker APEX-II CCD'
_diffrn_measurement_method         'φ and ω scans'
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     ?
_diffrn_standards_number           0
_reflns_Friedel_coverage           0.906
_reflns_Friedel_fraction_full      1.000
_reflns_Friedel_fraction_max       1.000
_reflns_number_gt                  194
_reflns_number_total               240
_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         'SAINT V8.40A (?, 2016)'
_computing_data_collection         ?
_computing_data_reduction          'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics      'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement    'XL (Sheldrick, 2008)'
_computing_structure_solution      ?
_refine_diff_density_max           2.721
_refine_diff_density_min           -0.819
_refine_diff_density_rms           0.258
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack     0.43(15)
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.141
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       20
_refine_ls_number_reflns           240
_refine_ls_number_restraints       7
_refine_ls_R_factor_all            0.0634
_refine_ls_R_factor_gt             0.0474
_refine_ls_restrained_S_all        1.125
_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)+(0.0610P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1088
_refine_ls_wR_factor_ref           0.1177
_refine_special_details
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.57156
 0.42844
2. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
3.a Riding coordinates:
 N1(H1A,H1B)
;
_atom_sites_solution_hydrogens     difmap
_atom_sites_solution_primary       ?
_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
 As2 As 0.3333 0.6667 0.6058(3) 0.0076(9) Uani 1 6 d S T P . .
 As1 As 0.0000 1.0000 0.6036(5) 0.0105(10) Uani 1 6 d S T P . .
 Br1 Br -0.3333 1.3333 0.4766(3) 0.0281(15) Uani 1 6 d S T P . .
 O1 O 0.166(2) 0.834(2) 0.6830(13) 0.015(4) Uani 1 2 d S T P . .
 N1 N 0.3333 0.6667 0.314(3) 0.041(11) Uani 1 6 d S TU P . .
 H1A H 0.3333 0.6667 0.2426 0.049 Uiso 1 6 d RS T P . .
 H1B H 0.1408 0.5704 0.3266 0.049 Uiso 1 2 d RS T 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_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 As2 O1 1.800(18) . ?
 As2 O1 1.800(18) 3_565 ?
 As2 O1 1.800(18) 2_665 ?
 As1 O1 1.806(18) . ?
 As1 O1 1.806(18) 2_675 ?
 As1 O1 1.806(18) 3_465 ?

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
 O1 As2 O1 94.2(7) . 3_565 ?
 O1 As2 O1 94.2(7) . 2_665 ?
 O1 As2 O1 94.2(7) 3_565 2_665 ?
 O1 As1 O1 93.0(7) 2_675 3_465 ?
 O1 As1 O1 93.0(7) . 2_675 ?
 O1 As1 O1 93.0(7) . 3_465 ?
 As2 O1 As1 114.7(8) . . ?

_olex2_submission_special_instructions  'No special instructions were received'
loop_
  _twin_individual_id
  _twin_individual_mass_fraction_refined
 1 0.57156
 2 0.42844

# END of CIF
