 
data_THF-MeOH-H2O_10_hydrate
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C3.17 H20.67 O7.83' 
_chemical_formula_weight          184.20

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'  -0.0001   0.0005
 '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'
 'O'  'O'   0.0018   0.0018
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_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'
 
_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.
;
 
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                    11.8229(9)
_cell_length_b                    11.8229(9)
_cell_length_c                    11.949(4)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      1446.5(6)
_cell_formula_units_Z             6
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        ?
_exptl_crystal_colour             ?
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.269          
_exptl_crystal_F_000              614
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_absorpt_coefficient_mu     0.045
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.40998
_diffrn_radiation_type            ?
_diffrn_source                    ?
_diffrn_measurement_device_type   ?
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             2024
_diffrn_reflns_av_unetI/netI      0.0574
_diffrn_reflns_av_R_equivalents   0.0335
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -9
_diffrn_reflns_limit_l_max        7
_diffrn_reflns_theta_min          1.987
_diffrn_reflns_theta_max          13.949
_diffrn_reflns_theta_full         13.949
_diffrn_measured_fraction_theta_max   0.648
_diffrn_measured_fraction_theta_full  0.648
_diffrn_reflns_Laue_measured_fraction_max    0.648
_diffrn_reflns_Laue_measured_fraction_full   0.648
_diffrn_reflns_point_group_measured_fraction_max   0.648
_diffrn_reflns_point_group_measured_fraction_full  0.648
_reflns_number_total              354
_reflns_number_gt                 262
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_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.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    .
_refine_ls_hydrogen_treatment     undef
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          354
_refine_ls_number_parameters      33
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1371
_refine_ls_R_factor_gt            0.1231
_refine_ls_wR_factor_ref          0.4608
_refine_ls_wR_factor_gt           0.4251
_refine_ls_goodness_of_fit_ref    2.003
_refine_ls_restrained_S_all       2.003
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
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 0.7327(6) 0.8664(3) 0.5000 0.076(3) Uiso 1 4 d S . P . .
O2 O 0.5812(4) 0.7906(2) 0.3159(5) 0.079(2) Uiso 1 2 d S . P . .
O3 O 0.3333 0.6667 0.3900(11) 0.076(3) Uiso 1 6 d S . P . .
O4 O 0.6170(4) 0.6170(4) 0.1924(6) 0.086(3) Uiso 1 2 d S . P . .
O5 O 0.7379(14) 0.7379(14) 0.0000 0.164(8) Uani 1 4 d S T P . .
C1 C 0.5000 1.0000 0.5000 0.29(2) Uani 2.44(7) 8 d S T P . .
C2 C 0.234(6) 0.617(3) 0.0000 0.26(2) Uiso 0.94(5) 4 d S . P . .
C3 C 0.286(2) 0.572(4) 0.0000 0.241(19) Uiso 0.94(5) 4 d S . P . .
C5 C 0.9443(9) 0.8885(19) 0.211(3) 0.191(10) Uiso 1.00(5) 2 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_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C2 C3 1.00(3) 3_565 ?
C2 C3 1.00(3) . ?
C2 C2 1.77(11) 2_665 ?
C2 C2 1.77(12) 3_565 ?
C2 C3 1.99(7) 2_665 ?
C3 C2 1.00(4) 2_665 ?
C3 C3 1.69(8) 3_565 ?
C3 C3 1.69(8) 2_665 ?
C3 C2 1.99(7) 3_565 ?
C5 C5 1.141(19) 6_655 ?
C5 C5 1.141(19) 5_565 ?
C5 C5 1.98(3) 2_765 ?
C5 C5 1.98(3) 3_675 ?
 
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
C3 C2 C3 116(9) 3_565 . ?
C3 C2 C2 88(4) 3_565 2_665 ?
C3 C2 C2 28(4) . 2_665 ?
C3 C2 C2 28(4) 3_565 3_565 ?
C3 C2 C2 88(4) . 3_565 ?
C2 C2 C2 59.999(6) 2_665 3_565 ?
C3 C2 C3 58(4) 3_565 2_665 ?
C3 C2 C3 58(4) . 2_665 ?
C2 C2 C3 29.999(1) 2_665 2_665 ?
C2 C2 C3 30.000(2) 3_565 2_665 ?
C2 C3 C2 124(9) . 2_665 ?
C2 C3 C3 32(4) . 3_565 ?
C2 C3 C3 92(4) 2_665 3_565 ?
C2 C3 C3 92(4) . 2_665 ?
C2 C3 C3 32(4) 2_665 2_665 ?
C3 C3 C3 60.000(4) 3_565 2_665 ?
C2 C3 C2 62(4) . 3_565 ?
C2 C3 C2 62(4) 2_665 3_565 ?
C3 C3 C2 30.000(5) 3_565 3_565 ?
C3 C3 C2 30.001(2) 2_665 3_565 ?
C5 C5 C5 120.00(2) 6_655 5_565 ?
C5 C5 C5 30.000(2) 6_655 2_765 ?
C5 C5 C5 89.999(14) 5_565 2_765 ?
C5 C5 C5 89.999(9) 6_655 3_675 ?
C5 C5 C5 30.000(8) 5_565 3_675 ?
C5 C5 C5 60.000(1) 2_765 3_675 ?
 
_refine_diff_density_max    0.393
_refine_diff_density_min   -0.315
_refine_diff_density_rms    0.064



