Linking Molybdenum-Sulfur Clusters for Electrocatalytic Hydrogen Evolution.
Ji, Zhe; Trickett, Christopher; Pei, Xiaokun; Yaghi, Omar M.; Journal of the American Chemical Society 140 (2018) 13618–13622; doi:10.1021/jacs.8b09807

data_4133383
_publ_section_title
;
 Linking Molybdenum-Sulfur Clusters for Electrocatalytic Hydrogen
 Evolution.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13618
_journal_page_last               13622
_journal_paper_doi               10.1021/jacs.8b09807
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C9 H5 Br6 Mo6 S20'
_chemical_formula_sum            'C9 H5.5 Br6 Mo6 S20'
_chemical_formula_weight         1809.93
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-08-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.418(18)
_cell_length_b                   12.370(8)
_cell_length_c                   21.063(13)
_cell_measurement_reflns_used    468
_cell_measurement_temperature    100
_cell_measurement_theta_max      14.92
_cell_measurement_theta_min      2.31
_cell_volume                     7925(8)
_computing_cell_refinement       'SAINT V8.37A Bruker-AXS, Madison WI'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.38A Bruker-AXS, Madison WI'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.42
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.878
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.2063
_diffrn_reflns_av_unetI/netI     0.2310
_diffrn_reflns_Laue_measured_fraction_full 0.878
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3776
_diffrn_reflns_point_group_measured_fraction_full 0.713
_diffrn_reflns_point_group_measured_fraction_max 0.712
_diffrn_reflns_theta_full        14.996
_diffrn_reflns_theta_max         14.996
_diffrn_reflns_theta_min         2.206
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.637
_exptl_absorpt_correction_T_max  0.7439
_exptl_absorpt_correction_T_min  0.4945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1073 before and 0.0780 after correction. The Ratio of minimum to maximum transmission is 0.6647. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_description       block
_exptl_crystal_F_000             3366
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.008
_exptl_crystal_size_min          0.008
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.40(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.823
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         1761
_refine_ls_number_restraints     564
_refine_ls_restrained_S_all      0.718
_refine_ls_R_factor_all          0.1253
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0083P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.1099
_reflns_Friedel_coverage         0.542
_reflns_Friedel_fraction_full    0.530
_reflns_Friedel_fraction_max     0.529
_reflns_number_gt                859
_reflns_number_total             1761
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09807_si_001.cif
_cod_data_source_block           MOS_1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        7926(8)
_cod_original_formula_sum        'C9 H5.50 Br6 Mo6 S20'
_cod_database_code               4133383
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.896
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C8-C9 = C8-C7_$1 = C12_$1-C7_$1 = C12_$1-C11_$1 = C10-C11_$1 = C10-C9
 1.39 with sigma of 0.02
 C4-C3 = C2-C3 = C1-C2 = C6_$3-C1 = C6_$3-C5 = C5-C4
 1.39 with sigma of 0.02
 C18_$1-C13 = C14-C13 = C14-C15 = C15-C16 = C16-C17_$1 = C18_$1-C17_$1
 1.39 with sigma of 0.02
 C12_$1-C8 \\sim C8-C10
 with sigma of 0.02
 C8-C10 \\sim C10-C12_$1
 with sigma of 0.02
 C11_$1-C7_$1 \\sim C7_$1-C9
 with sigma of 0.02
 C7_$1-C9 \\sim C9-C11_$1
 with sigma of 0.02
 C12_$1-C8 \\sim C7_$1-C9
 with sigma of 0.02
 C18_$1-C14 \\sim C14-C16
 with sigma of 0.02
 C14-C16 \\sim C16-C18_$1
 with sigma of 0.02
 C4-C2 \\sim C2-C6_$3
 with sigma of 0.02
 C2-C6_$3 \\sim C6_$3-C4
 with sigma of 0.02
 C3-C1 \\sim C1-C5
 with sigma of 0.02
 C1-C5 \\sim C5-C3
 with sigma of 0.02
 C4-C2 \\sim C3-C1
 with sigma of 0.02
 C13-C15 \\sim C15-C17_$1
 with sigma of 0.02
 C17_$1-C13 \\sim C13-C15
 with sigma of 0.02
 C18_$1-C14 \\sim C13-C15
 with sigma of 0.02
 C16-S6 \\sim C18_$1-S5_$1
 with sigma of 0.02
 S6-C15 \\sim S5_$1-C13 \\sim S4-C9 \\sim S3_$1-C7_$1 \\sim S2-C5 \\sim S1_$1-C1
 with sigma of 0.02
 S4-C10 \\sim C12_$1-S3_$1
 with sigma of 0.02
3. Restrained planarity
 C9, C8, C10, C7_$1, C11_$1, C12_$1, S3_$1, S4
 with sigma of 0.1
 C3, C4, S2, C5, C2, C1, C6_$3, S1_$1
 with sigma of 0.1
 C16, C14, C13, C15, C17_$1, C18_$1, S5_$1, S6
 with sigma of 0.1
4. Rigid body (RIGU) restrains
 Mo1, Mo3, Mo2, Br1, Br2, Br3, S12, S14, S9, S13, S7, S11, S10, S5, S1, S3,
 Mo6, Mo4, Mo5, Br4, Br5, S17, S4, S19, S16, Br6, S6, S20, S15, S18, S2, S8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C11(0.5) H11(0.5) C9(0.5) C7(0.5) C8(0.5) H8(0.5) C12(0.5)
 C10(0.5) H10(0.5) C16(0.5) H16(0.5) C14(0.5) H14(0.5) C17(0.5) H17(0.5)
 C13(0.5) C18(0.5) C15(0.5) C3(0.5) H3(0.5) C4(0.5) H4(0.5) C5(0.5) C2(0.5)
 H2(0.5) C1(0.5) C6(0.5) H6(0.5)
 Fixed Uiso: C11(0.1) C9(0.1) C7(0.1) C8(0.1) C12(0.1) C10(0.1) C16(0.08)
 C14(0.08) C17(0.08) C13(0.08) C18(0.08) C15(0.08) C3(0.1) C4(0.1) C5(0.1)
 C2(0.1) C1(0.1) C6(0.1)
6.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C8(H8), C10(H10), C16(H16), C14(H14), C17(H17), C3(H3), C4(H4),
 C2(H2), C6(H6)
;
_olex2_submission_special_instructions 'No special instructions were received'