Comparative studies on the contribution of NHS hydrogen bonds in tungsten and molybdenum benzenedithiolate complexes.
Okamura, Taka-Aki; Omi, Yui; Hirano, Yasunori; Onitsuka, Kiyotaka; Dalton transactions (Cambridge, England : 2003) 45 (2016) 15651–15659; doi:10.1039/c6dt02250b

data_7040566
_publ_section_title
;
 Comparative studies on the contribution of NHS hydrogen bonds in tungsten
 and molybdenum benzenedithiolate complexes.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15651
_journal_page_last               15659
_journal_paper_doi               10.1039/c6dt02250b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C53 H91.5 Mo N8.5 O5 S4'
_chemical_formula_sum            'C53 H91.5 Mo N8.5 O5 S4'
_chemical_formula_weight         1152.02
_chemical_name_systematic
;
(NEt4)2[MoO{S2C6H2(NHCO-t-Bu)2}2]-5/2(CH3CN)
;
_chemical_properties_physical    ', Air-sensitive,Oxygen-sensitive'
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-08-27
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-08-27 deposited with the CCDC.
2016-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 127.696(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.769(6)
_cell_length_b                   16.624(3)
_cell_length_c                   26.525(4)
_cell_measurement_reflns_used    36110
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      3.01
_cell_volume                     12829(4)
_computing_cell_refinement       'RAPID AUTO (Rigaku, 2006)'
_computing_data_collection       'RAPID AUTO (Rigaku, 2006)'
_computing_data_reduction        'RAPID AUTO (Rigaku, 2006)'
_computing_molecular_graphics    'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            48881
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.009
_diffrn_source
;
 MicroMax-007HF microfocus rotating anode X-ray generator
;
_exptl_absorpt_coefficient_mu    0.382
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4920
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         11274
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0599
_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^)+(0.0940P)^2^+15.7634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1567
_refine_ls_wR_factor_ref         0.1743
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7920
_reflns_number_total             11274
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02250b2.cif
_cod_data_source_block           3-Mo
_cod_depositor_comments
;Adding full bibliography for 7040564--7040567.cif.

 Adding full bibliography for 7040564--7040567.cif.
;
_cod_original_formula_sum        'C53 H91.50 Mo N8.50 O5 S4'
_cod_database_code               7040566
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.928
_shelx_estimated_absorpt_t_max   0.956
_shelx_res_checksum              25087