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_4133380
_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
'0.5(Br3 Mo3 S10), 0.5(Br3 Mo3 S9.5), 0.25(S)'
_chemical_formula_sum            'Br3 Mo3 S10'
_chemical_formula_weight         848.15
_chemical_name_common            MOS-1
_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_primary     'intrinsic phasing'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                90
_cell_angle_beta                 119.55(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.246(6)
_cell_length_b                   15.3192(14)
_cell_length_c                   24.560(6)
_cell_measurement_reflns_used    3028
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.253
_cell_measurement_theta_min      2.098
_cell_volume                     7936(4)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd., Version 171.37.33
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd., Version 171.37.33
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd., 171.37.33
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
and local programs
;
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  SHELXL-2014/6
_computing_structure_solution    'SHELXT 2014/4'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'PILATUS3 6M'
_diffrn_measurement_method       '\f shutterless scans'
_diffrn_radiation_monochromator  'double crystal, Si(111)'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.91165
_diffrn_reflns_av_R_equivalents  0.0843
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18880
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        19.000
_diffrn_reflns_theta_max         19.253
_diffrn_reflns_theta_min         2.098
_diffrn_source
;
Advanced Light Source, Station 5.0.2
;
_exptl_absorpt_coefficient_mu    8.745
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   absscale
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       Block
_exptl_crystal_F_000             3128
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.058
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.268
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         3028
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.279
_refine_ls_R_factor_all          0.2033
_refine_ls_R_factor_gt           0.1687
_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^)+(0.2000P)^2^+150.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4416
_refine_ls_wR_factor_ref         0.4714
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1841
_reflns_number_total             3028
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09807_si_003.cif
_cod_data_source_block           MOS_3
_cod_database_code               4133380
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.880
_shelx_estimated_absorpt_t_min   0.721
_olex2_refinement_description
;
1. Shared sites
{Br6A, S13B}
{Br6B, S13A}
{Br5A, S12B}
{Br5B, S12A}
2. Restrained distances
 Br5A-S12A
 3.1 with sigma of 0.02
 S15-S16A
 2 with sigma of 0.02
 S18A-S17A
 2 with sigma of 0.02
 S20B-S19B
 2 with sigma of 0.02
 S15-S16B
 2 with sigma of 0.02
 S18B-S17B
 2 with sigma of 0.02
 Br4B-S11
 3 with sigma of 0.02
 S6_$2-Br1
 3.6 with sigma of 0.02
 S20A-S19A
 2 with sigma of 0.02
 Br1-S8_$2
 3.6 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(S6) \\sim Ueq, Uanis(S5) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(Br6B) = Uanis(S13A)
Uanis(Br5A) = Uanis(S12B)
Uanis(Br5B) = Uanis(S12A)
Uanis(S17B) = Uanis(S17A)
Uanis(S16B) = Uanis(S15) = Uanis(S16A)
Uanis(S18B) = Uanis(S17B)
Uanis(S20B) = Uanis(S19B)
Uanis(S14B) = Uanis(S14A) = Uanis(Mo6B) = Uanis(Mo6A)
Uanis(Br6A) = Uanis(S13B)
Uanis(S19A) = Uanis(S19B)
Uanis(S18A) = Uanis(S17A)
Uanis(S20A) = Uanis(S19A)
Uanis(S7) = Uanis(S8)
4. Rigid body (RIGU) restrains
 S9, Mo3, S4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S18A, Mo4, S16A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Mo6A, S18A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Mo4, S18B, Mo6B, S20B, S17B, S13B, S16B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S5, S6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S9, S10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Mo4, S13A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S19A, Mo6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Mo5, S19B, S12B, Br5B, S12A, S16A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S1, Mo1, S8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Br6A(0.5) S13B(0.5) Br4B(0.5) Br6B(0.5) S13A(0.5) S14A(0.5)
 S17A(0.5) S17B(0.5) Mo6A(0.5) Mo6B(0.5) Br4A(0.5) Br5A(0.5) S12B(0.5)
 S12A(0.5) Br5B(0.5) S19A(0.5) S20A(0.5) S19B(0.5) S16A(0.5) S18A(0.5)
 S14B(0.5) S16B(0.5) S18B(0.5) S20B(0.5)
;
_olex2_submission_special_instructions 'No special instructions were received'