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_7707173
_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         'C18 H44 Cu12 O22 S12, 6(H2 O)'
_chemical_formula_sum            'C18 H56 Cu12 O28 S12'
_chemical_formula_weight         1867.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-04-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-04-01 deposited with the CCDC.	2021-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                72.310(5)
_cell_angle_beta                 82.128(4)
_cell_angle_gamma                60.367(7)
_cell_formula_units_Z            2
_cell_length_a                   12.4249(7)
_cell_length_b                   12.5351(9)
_cell_length_c                   19.7599(9)
_cell_measurement_reflns_used    9165
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      32.8740
_cell_measurement_theta_min      2.4150
_cell_volume                     2548.2(3)
_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_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     75.00 109.00   1.00   12.50    --   30.00  54.00   0.00   34
  2  \w    -73.00  33.00   1.00   12.50    --   30.00  54.00-120.00  106
  3  \w    -73.00  32.00   1.00   12.50    --   30.00  54.00 120.00  105
  4  \w    -73.00  33.00   1.00   12.50    --   30.00  54.00   0.00  106
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0397161000
_diffrn_orient_matrix_UB_12      0.0101900000
_diffrn_orient_matrix_UB_13      0.0294710000
_diffrn_orient_matrix_UB_21      -0.0504526000
_diffrn_orient_matrix_UB_22      0.0164641000
_diffrn_orient_matrix_UB_23      -0.0212348000
_diffrn_orient_matrix_UB_31      0.0138473000
_diffrn_orient_matrix_UB_32      -0.0648677000
_diffrn_orient_matrix_UB_33      0.0100256000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14516
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         2.515
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.470
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43701
_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    2.434
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.721
_refine_diff_density_min         -1.418
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         9038
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0397P)^2^+6.2410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0884
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7634
_reflns_number_total             9038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00782c2.cif
_cod_data_source_block           190108d
_cod_depositor_comments
'Adding full bibliography for 7707172--7707173.cif.'
_cod_database_code               7707173
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.494
_shelx_estimated_absorpt_t_min   0.342
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 S12-O16 = S12-O17 = S12-O18 = S12A-O16A = S12A-O17A = S12A-O18A
 1.46 with sigma of 0.02
 C18-S12 = C18A-S12A = C3-S2 = C3A-S2
 1.78 with sigma of 0.02
 C1-S1 = C1A-S1
 1.83 with sigma of 0.02
 C17-C18 = C17-C18A = C1-C2 = C2-C3 = C1A-C2A = C2A-C3A
 1.53 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C2) = Uanis(C3)
Uanis(O1) = Uanis(O3)
Uanis(O24) = Uanis(O25)
Uanis(C18) = Uanis(C18A)
Uanis(O17) = Uanis(O17A)
Uanis(O18) = Uanis(O18A)
Uanis(S12) = Uanis(S12A)
Uanis(O16) = Uanis(O16A)
Uanis(C1) = Uanis(C1A)
Uanis(C2) = Uanis(C2A)
Uanis(C3) = Uanis(C3A)
4. Others
 Sof(H17C)=Sof(H17D)=Sof(S12A)=Sof(O16A)=Sof(O17A)=Sof(C18A)=Sof(H18C)=
 Sof(H18D)=Sof(O18A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=1-FVAR(1)
 Sof(S12)=Sof(O18)=Sof(O17)=Sof(O16)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H17A)=
 Sof(H17B)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C2)=Sof(H2A)=
 Sof(H2B)=FVAR(1)
5.a Riding coordinates:
 O22(H22A,H22B), O21(H21A,H21B), O26(H26A,H26B), O19(H19A,H19B), O27(H27A,
 H27B), O25(H25A,H25B), O28(H28A,H28B), O24(H24A,H24B)
5.b Free rotating group:
 O23(H23A,H23B)
5.c Rotating group:
 O20(H20A,H20B)
5.d Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C18(H18A,H18B), C15(H15A,H15B), C9(H9A,H9B), C8(H8A,H8B),
 C12(H12A,H12B), C6(H6A,H6B), C4(H4A,H4B), C10(H10A,H10B), C16(H16A,H16B),
 C17(H17C,H17D), C17(H17A,H17B), C7(H7A,H7B), C13(H13A,H13B), C5(H5A,H5B),
 C1(H1A,H1B), C11(H11A,H11B), C3(H3A,H3B), C2(H2A,H2B), C18A(H18C,H18D),
 C2A(H2AA,H2AB), C3A(H3AA,H3AB), C1A(H1AA,H1AB)
;
_shelx_res_checksum              52043
_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 1.815
_oxdiff_exptl_absorpt_empirical_full_min 0.733