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_7040567
_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         'C51 H82 N6 O3 S6 W'
_chemical_formula_sum            'C51 H82 N6 O3 S6 W'
_chemical_formula_weight         1203.43
_chemical_name_systematic
;
(NEt4)2[W(S2C6H3NHCO-t-Bu)3]-CH3CN
;
_chemical_properties_physical    ', Air-sensitive,Oxygen-sensitive'
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_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                 95.752(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4233(4)
_cell_length_b                   28.3088(11)
_cell_length_c                   18.3378(13)
_cell_measurement_reflns_used    32033
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.00
_cell_volume                     5900.2(5)
_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    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0771
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44800
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.000
_diffrn_source
;
 MicroMax-007HF microfocus rotating anode X-ray generator
;
_exptl_absorpt_coefficient_mu    2.213
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.402
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            reddish-purple
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.797
_refine_diff_density_min         -1.077
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         10371
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0584
_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^)+(0.0421P)^2^+25.2278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1401
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8022
_reflns_number_total             10371
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02250b2.cif
_cod_data_source_block           6-CH3CN
_cod_depositor_comments
;Adding full bibliography for 7040564--7040567.cif.

 Adding full bibliography for 7040564--7040567.cif.
;
_cod_database_code               7040567
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.809
_shelx_estimated_absorpt_t_max   0.957
_shelx_res_checksum              9795