#------------------------------------------------------------------------------
#$Date: 2019-11-25 16:30:42 +0200 (Mon, 25 Nov 2019) $
#$Revision: 241329 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/10/4131007.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4131007
loop_
_publ_author_name
'Garrett, Benjamin R.'
'Click, Kevin A.'
'Durr, Christopher B.'
'Hadad, Christopher M.'
'Wu, Yiying'
_publ_section_title
;
 [MoO(S₂)₂L]¹⁻ (L = picolinate or
 pyrimidine-2-carboxylate) Complexes as MoSₓ-Inspired
 Electrocatalysts for Hydrogen Production in Aqueous Solution.
;
_journal_issue                   41
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13726
_journal_page_last               13731
_journal_paper_doi               10.1021/jacs.6b08652
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C14 H24 Mo N2 O3 S4'
_chemical_formula_weight         492.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 109.872(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6807(10)
_cell_length_b                   12.2202(10)
_cell_length_c                   13.4341(10)
_cell_measurement_reflns_used    3283
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.32
_cell_volume                     1957.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11555
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.047
_diffrn_reflns_theta_max         25.047
_diffrn_reflns_theta_min         2.319
_exptl_absorpt_coefficient_mu    1.112
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       plate
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3458
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0278
_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/[σ²(Fo²)+(0.0359P)²+0.4317P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2883
_reflns_number_total             3458
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b08652_si_003.cif
_cod_data_source_block           pic_07_13_2016_0m_a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4131007
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.851
_shelx_estimated_absorpt_t_max   0.936
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Mo1 Mo 0.43156(2) 0.29211(2) 0.58284(2) 0.01928(9) Uani 1 1 d . .
S1 S 0.45381(7) 0.44320(6) 0.70863(6) 0.0290(2) Uani 1 1 d . .
S2 S 0.53599(7) 0.29967(7) 0.76632(6) 0.0282(2) Uani 1 1 d . .
S3 S 0.47073(7) 0.10295(6) 0.59894(6) 0.0293(2) Uani 1 1 d . .
S4 S 0.36147(7) 0.14517(6) 0.45257(6) 0.0296(2) Uani 1 1 d . .
O1 O 0.52577(17) 0.33938(16) 0.52986(15) 0.0239(5) Uani 1 1 d . .
O2 O 0.27234(17) 0.27186(17) 0.60598(16) 0.0254(5) Uani 1 1 d . .
O3 O 0.09009(19) 0.3161(2) 0.55702(18) 0.0416(6) Uani 1 1 d . .
N1 N 0.3073(2) 0.39638(19) 0.46490(18) 0.0207(5) Uani 1 1 d . .
N2 N 0.7543(2) 0.19145(18) 0.42509(19) 0.0197(6) Uani 1 1 d . .
C1 C 0.1825(3) 0.3215(3) 0.5486(2) 0.0261(7) Uani 1 1 d . .
C2 C 0.2012(3) 0.3944(2) 0.4649(2) 0.0232(7) Uani 1 1 d . .
C3 C 0.1175(3) 0.4554(2) 0.3934(3) 0.0308(8) Uani 1 1 d . .
H3 H 0.0432 0.4541 0.3949 0.037 Uiso 1 1 calc R U
C4 C 0.1442(3) 0.5186(3) 0.3196(2) 0.0320(8) Uani 1 1 d . .
H4 H 0.0876 0.5601 0.2689 0.038 Uiso 1 1 calc R U
C5 C 0.2523(3) 0.5210(2) 0.3199(2) 0.0308(8) Uani 1 1 d . .
H5 H 0.2718 0.5646 0.2703 0.037 Uiso 1 1 calc R U
C6 C 0.3326(3) 0.4586(2) 0.3938(2) 0.0255(7) Uani 1 1 d . .
H6 H 0.4077 0.4598 0.3942 0.031 Uiso 1 1 calc R U
C7 C 0.7043(3) 0.1564(3) 0.5080(2) 0.0259(7) Uani 1 1 d . .
H7A H 0.6364 0.2010 0.4988 0.031 Uiso 1 1 calc R U
H7B H 0.6801 0.0792 0.4945 0.031 Uiso 1 1 calc R U
C8 C 0.7808(3) 0.1665(3) 0.6214(2) 0.0362(8) Uani 1 1 d . .
H8A H 0.8452 0.1176 0.6337 0.054 Uiso 1 1 calc R U
H8B H 0.7397 0.1462 0.6687 0.054 Uiso 1 1 calc R U
H8C H 0.8071 0.2422 0.6356 0.054 Uiso 1 1 calc R U
C9 C 0.8587(2) 0.1257(2) 0.4339(3) 0.0278(7) Uani 1 1 d . .
H9A H 0.9194 0.1478 0.4995 0.033 Uiso 1 1 calc R U
H9B H 0.8830 0.1446 0.3734 0.033 Uiso 1 1 calc R U
C10 C 0.8441(3) 0.0024(2) 0.4357(3) 0.0344(8) Uani 1 1 d . .
H10A H 0.8334 -0.0190 0.5019 0.052 Uiso 1 1 calc R U
H10B H 0.9111 -0.0338 0.4306 0.052 Uiso 1 1 calc R U
H10C H 0.7784 -0.0196 0.3756 0.052 Uiso 1 1 calc R U
C11 C 0.7865(3) 0.3118(2) 0.4415(2) 0.0271(7) Uani 1 1 d . .
H11A H 0.7232 0.3527 0.4511 0.033 Uiso 1 1 calc R U
H11B H 0.8514 0.3191 0.5078 0.033 Uiso 1 1 calc R U
C12 C 0.8163(3) 0.3648(3) 0.3526(3) 0.0343(8) Uani 1 1 d . .
H12A H 0.8776 0.3241 0.3410 0.052 Uiso 1 1 calc R U
H12B H 0.8398 0.4406 0.3717 0.052 Uiso 1 1 calc R U
H12C H 0.7506 0.3640 0.2877 0.052 Uiso 1 1 calc R U
C13 C 0.6687(3) 0.1728(3) 0.3166(2) 0.0274(7) Uani 1 1 d . .
H13A H 0.6461 0.0949 0.3106 0.033 Uiso 1 1 calc R U
H13B H 0.7047 0.1870 0.2630 0.033 Uiso 1 1 calc R U
C14 C 0.5636(3) 0.2430(3) 0.2904(3) 0.0348(8) Uani 1 1 d . .
H14A H 0.5202 0.2210 0.3351 0.052 Uiso 1 1 calc R U
H14B H 0.5180 0.2330 0.2157 0.052 Uiso 1 1 calc R U
H14C H 0.5850 0.3201 0.3034 0.052 Uiso 1 1 calc R U
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O1 Mo1 O2 158.61(9)
O1 Mo1 N1 86.27(9)
O2 Mo1 N1 72.34(8)
O1 Mo1 S3 102.54(7)
O2 Mo1 S3 93.01(6)
N1 Mo1 S3 134.82(6)
O1 Mo1 S2 101.54(7)
O2 Mo1 S2 94.24(6)
N1 Mo1 S2 136.93(6)
S3 Mo1 S2 85.24(3)
O1 Mo1 S4 94.96(7)
O2 Mo1 S4 83.63(6)
N1 Mo1 S4 85.05(6)
S3 Mo1 S4 50.37(3)
S2 Mo1 S4 135.17(3)
O1 Mo1 S1 95.78(7)
O2 Mo1 S1 83.18(6)
N1 Mo1 S1 86.97(6)
S3 Mo1 S1 134.66(3)
S2 Mo1 S1 50.33(3)
S4 Mo1 S1 166.16(3)
S2 S1 Mo1 62.73(3)
S1 S2 Mo1 66.93(3)
S4 S3 Mo1 67.21(3)
S3 S4 Mo1 62.42(3)
C1 O2 Mo1 122.64(19)
C6 N1 C2 119.4(3)
C6 N1 Mo1 123.4(2)
C2 N1 Mo1 117.23(19)
C13 N2 C9 108.5(2)
C13 N2 C7 108.8(2)
C9 N2 C7 111.4(2)
C13 N2 C11 110.8(2)
C9 N2 C11 108.4(2)
C7 N2 C11 108.9(2)
O3 C1 O2 127.0(3)
O3 C1 C2 120.0(3)
O2 C1 C2 113.0(3)
N1 C2 C3 121.5(3)
N1 C2 C1 114.8(3)
C3 C2 C1 123.8(3)
C2 C3 C4 118.8(3)
C2 C3 H3 120.6
C4 C3 H3 120.6
C5 C4 C3 119.8(3)
C5 C4 H4 120.1
C3 C4 H4 120.1
C4 C5 C6 118.8(3)
C4 C5 H5 120.6
C6 C5 H5 120.6
N1 C6 C5 121.8(3)
N1 C6 H6 119.1
C5 C6 H6 119.1
C8 C7 N2 115.6(2)
C8 C7 H7A 108.4
N2 C7 H7A 108.4
C8 C7 H7B 108.4
N2 C7 H7B 108.4
H7A C7 H7B 107.4
C7 C8 H8A 109.5
C7 C8 H8B 109.5
H8A C8 H8B 109.5
C7 C8 H8C 109.5
H8A C8 H8C 109.5
H8B C8 H8C 109.5
N2 C9 C10 114.7(2)
N2 C9 H9A 108.6
C10 C9 H9A 108.6
N2 C9 H9B 108.6
C10 C9 H9B 108.6
H9A C9 H9B 107.6
C9 C10 H10A 109.5
C9 C10 H10B 109.5
H10A C10 H10B 109.5
C9 C10 H10C 109.5
H10A C10 H10C 109.5
H10B C10 H10C 109.5
C12 C11 N2 115.2(2)
C12 C11 H11A 108.5
N2 C11 H11A 108.5
C12 C11 H11B 108.5
N2 C11 H11B 108.5
H11A C11 H11B 107.5
C11 C12 H12A 109.5
C11 C12 H12B 109.5
H12A C12 H12B 109.5
C11 C12 H12C 109.5
H12A C12 H12C 109.5
H12B C12 H12C 109.5
N2 C13 C14 115.1(2)
N2 C13 H13A 108.5
C14 C13 H13A 108.5
N2 C13 H13B 108.5
C14 C13 H13B 108.5
H13A C13 H13B 107.5
C13 C14 H14A 109.5
C13 C14 H14B 109.5
H14A C14 H14B 109.5
C13 C14 H14C 109.5
H14A C14 H14C 109.5
H14B C14 H14C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Mo1 O1 1.687(2)
Mo1 O2 2.159(2)
Mo1 N1 2.218(2)
Mo1 S3 2.3587(8)
Mo1 S2 2.3705(8)
Mo1 S4 2.4534(8)
Mo1 S1 2.4536(8)
S1 S2 2.0528(11)
S3 S4 2.0495(12)
O2 C1 1.290(4)
O3 C1 1.217(4)
N1 C6 1.342(4)
N1 C2 1.346(4)
N2 C13 1.509(4)
N2 C9 1.519(4)
N2 C7 1.519(4)
N2 C11 1.522(3)
C1 C2 1.516(4)
C2 C3 1.382(4)
C3 C4 1.387(4)
C3 H3 0.9500
C4 C5 1.370(5)
C4 H4 0.9500
C5 C6 1.385(4)
C5 H5 0.9500
C6 H6 0.9500
C7 C8 1.508(4)
C7 H7A 0.9900
C7 H7B 0.9900
C8 H8A 0.9800
C8 H8B 0.9800
C8 H8C 0.9800
C9 C10 1.519(4)
C9 H9A 0.9900
C9 H9B 0.9900
C10 H10A 0.9800
C10 H10B 0.9800
C10 H10C 0.9800
C11 C12 1.515(4)
C11 H11A 0.9900
C11 H11B 0.9900
C12 H12A 0.9800
C12 H12B 0.9800
C12 H12C 0.9800
C13 C14 1.521(4)
C13 H13A 0.9900
C13 H13B 0.9900
C14 H14A 0.9800
C14 H14B 0.9800
C14 H14C 0.9800
