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_4133382
_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         'C60 H126 Br10 Mo6 N6 S18'
_chemical_formula_sum            'C60 H126 Br10 Mo6 N6 S18'
_chemical_formula_weight         2883.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           66
_space_group_name_Hall           '-C 2 2c'
_space_group_name_H-M_alt        'C c c m'
_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                   12.4938(5)
_cell_length_b                   42.4264(17)
_cell_length_c                   22.2065(10)
_cell_measurement_reflns_used    5269
_cell_measurement_temperature    100
_cell_measurement_theta_max      50.32
_cell_measurement_theta_min      3.69
_cell_volume                     11770.9(9)
_computing_cell_refinement       'SAINT V8.38A Bruker-AXS, Madison WI'
_computing_data_collection       'SAINT V8.38A 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    'SHELXT-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.42
_diffrn_detector_type            'Bruker PHOTON-100 detector'
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_Laue_measured_fraction_full 0.903
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10683
_diffrn_reflns_point_group_measured_fraction_full 0.903
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        50.422
_diffrn_reflns_theta_max         50.422
_diffrn_reflns_theta_min         3.981
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.440
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.5258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.0912 before and 0.0562 after correction. The Ratio of minimum to maximum transmission is 0.7011. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    2.297
_exptl_crystal_description       block
_exptl_crystal_F_000             7818
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.129
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2891
_refine_ls_number_restraints     113
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1392
_refine_ls_R_factor_gt           0.1048
_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^)+(0.1200P)^2^+657.6979P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2558
_refine_ls_wR_factor_ref         0.2766
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2050
_reflns_number_total             2891
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09807_si_002.cif
_cod_data_source_block           MOS_2
_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_database_code               4133382
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6-C5 = C4-C5 = C3-C4 = C3-C2 = C2-C1 = C1-C6
 1.39 with sigma of 0.02
 C9-C10
 1.54 with sigma of 0.02
 C15-N2 = N2-C17
 1.51 with sigma of 0.02
 C16-C15 = C18-C17
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C2 \\sim C1 \\sim C6 \\sim C5 \\sim C4 \\sim C3: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C5, C4, C2, C3, C6, C1, Br4, S7, S6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C4(0.5) H4(0.5) C2(0.5) H2(0.5) C3(0.5) C6(0.5) C1(0.5) H1(0.5)
 Br4(0.5) S7(0.5)
 Fixed Uiso: N2(0.2) C17(0.2)
6.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C9(H9A,H9B), C13(H13A,H13B), C7(H7A,H7B), C17(H17A,H17B),
 C15(H15A,H15B)
6.b Me refined with riding coordinates:
 C12(H12A,H12B,H12C), C8(H8A,H8B,H8C), C14(H14A,H14B,H14C), C10(H10A,H10B,
 H10C), C18(H18A,H18B,H18C), C16(H16A,H16B,H16C)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C2(H2), C1(H1)
;
_olex2_submission_special_instructions 'No special instructions were received'