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_4133381
_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         'C54 H36 Mo6 N6 O18 S8'
_chemical_formula_sum            'C54 H34 Mo6 N6 O18 S8'
_chemical_formula_weight         1886.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'dual space'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-08-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.853(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.8186(16)
_cell_length_b                   21.5751(16)
_cell_length_c                   33.513(2)
_cell_measurement_reflns_used    4610
_cell_measurement_temperature    100
_cell_measurement_theta_max      19.566
_cell_measurement_theta_min      2.276
_cell_volume                     17174(2)
_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      100.0
_diffrn_detector_area_resol_mean 10.42
_diffrn_detector_type            'Bruker PHOTON-100 detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1098
_diffrn_reflns_av_unetI/netI     0.0783
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            51225
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        20.867
_diffrn_reflns_theta_max         20.867
_diffrn_reflns_theta_min         2.412
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.099
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_correction_T_min  0.6437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0735 before and 0.0518 after correction. The Ratio of minimum to maximum transmission is 0.8646. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             7392
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         9020
_refine_ls_number_restraints     228
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+51.3682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1261
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6222
_reflns_number_total             9020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09807_si_004.cif
_cod_data_source_block           MOS_4
_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               4133381
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.734
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
N1 \\sim C25 \\sim C29 \\sim C27 \\sim C26 \\sim C28: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
N2 \\sim C34 \\sim C30 \\sim C31 \\sim C33 \\sim C32: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
N3 \\sim C37 \\sim C38 \\sim C35 \\sim C39 \\sim C36: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
N5 \\sim C49 \\sim C45 \\sim C46 \\sim C47 \\sim C48: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
N4 \\sim C40 \\sim C44 \\sim C41 \\sim C42 \\sim C43: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
N6 \\sim C54 \\sim C53 \\sim C50 \\sim C52 \\sim C51: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(C15) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
3.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C8(H8), C16(H16), C12(H12), C20(H20), C4(H4), C54(H54), C53(H53),
 C40(H40), C34(H34), C44(H44), C49(H49), C30(H30), C41(H41), C42(H42), C45(H45),
  C31(H31), C25(H25), C50(H50), C52(H52), C51(H51), C43(H43), C33(H33),
 C37(H37), C32(H32), C29(H29), C38(H38), C27(H27), C35(H35), C26(H26), C39(H39),
  C46(H46), C28(H28), C47(H47), C36(H36), C48(H48)
;
_olex2_submission_special_instructions 'No special instructions were received'