Two 6/10-connected Cu<sub>12</sub>S<sub>6</sub> cluster-based organic frameworks: crystal structure and proton conduction.
Li, Jia-Ming; Xu, Tian-Yang; Zhao, Ya-Li; Hu, Xing-Liang; He, Kun-Huan; Dalton transactions (Cambridge, England : 2003) 50 (2021) 7484–7495; doi:10.1039/d1dt00782c

data_7707172
_publ_section_title
;
 Two 6/10-connected Cu<sub>12</sub>S<sub>6</sub> cluster-based organic
 frameworks: crystal structure and proton conduction.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7484
_journal_page_last               7495
_journal_paper_doi               10.1039/d1dt00782c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C12 H30 Cu12 O21 S12'
_chemical_formula_sum            'C12 H30 Cu12 O21 S12'
_chemical_formula_weight         1657.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-04-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-04-20 deposited with the CCDC.	2021-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.951(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8921(4)
_cell_length_b                   17.7132(6)
_cell_length_c                   18.9516(7)
_cell_measurement_reflns_used    9832
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      32.6230
_cell_measurement_theta_min      2.4830
_cell_volume                     3962.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -14.00  12.00   1.00   10.00    --   30.00  54.00 -60.00   26
  2  \w     51.00  92.00   1.00   10.00    --   30.00  54.00 -60.00   41
  3  \w     16.00  42.00   1.00   10.00    --   30.00  54.00-150.00   26
  4  \w    -63.00 119.00   1.00   10.00    --   30.00  54.00 120.00  182
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16906
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.097
_diffrn_reflns_theta_max         25.097
_diffrn_reflns_theta_min         2.452
_exptl_absorpt_coefficient_mu    7.004
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.778
_exptl_crystal_description       block
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.844
_refine_diff_density_min         -1.387
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         7036
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0317
_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/[\s^2^(Fo^2^)+(0.0369P)^2^+4.3695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0787
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5847
_reflns_number_total             7036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00782c2.cif
_cod_data_source_block           190108c
_cod_depositor_comments
'Adding full bibliography for 7707172--7707173.cif.'
_cod_database_code               7707172
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.420
_shelx_estimated_absorpt_t_min   0.273
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 S3-O4 = S3-O5 = S3-O6
 1.45 with sigma of 0.02
 S3A-O4A = S3A-O5A = S3A-O6A
 1.45 with sigma of 0.02
 C3-C4 = C3A-C4A
 1.53 with sigma of 0.02
 C3-S3 = C3-S3A
 1.78 with sigma of 0.02
 C4-S4 = C4A-S4
 1.83 with sigma of 0.02
 O7-Cu4 \\sim O7-Cu4A
 with sigma of 0.02
 S5-Cu4 \\sim S5-Cu4A
 with sigma of 0.02
 S4-Cu4 \\sim S4-Cu4A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C4) = Uanis(C4A) = Uanis(C3) = Uanis(C3A)
Uanis(Cu4) = Uanis(Cu4A)
4. Others
 Sof(S3A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C4A)=
 Sof(H4AA)=Sof(H4AB)=1-FVAR(1)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(S3)=Sof(O4)=Sof(O5)=
 Sof(O6)=FVAR(1)
 Sof(Cu4A)=1-FVAR(2)
 Sof(Cu4)=FVAR(2)
5.a Rotating group:
 O7(H7A,H7B), O15(H15A,H15B), O14(H14A,H14B)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7C,H7D), C12(H12A,H12B), C5(H5A,H5B), C8(H8A,H8B), C11(H11A,
 H11B), C1(H1A,H1B), C2(H2A,H2B), C10(H10A,H10B), C3(H3A,H3B), C9(H9A,H9B),
 C4(H4A,H4B), C3A(H3AA,H3AB), C4A(H4AA,H4AB)
;
_shelx_res_checksum              20610
_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
;