A Heterobimetallic W-Ni Complex Containing a Redox-Active W[SNS]2 Metalloligand.
Rosenkoetter, Kyle E.; Ziller, Joseph W.; Heyduk, Alan F.; Inorganic chemistry 55 (2016) 6794–6798; doi:10.1021/acs.inorgchem.6b01164

data_4348451
_publ_section_title
;
 A Heterobimetallic W-Ni Complex Containing a Redox-Active W[SNS]2
 Metalloligand.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6794
_journal_page_last               6798
_journal_paper_doi               10.1021/acs.inorgchem.6b01164
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C54 H48 N2 Ni P2 S4 W'
_chemical_formula_weight         1157.68
_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_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 106.7842(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4209(12)
_cell_length_b                   15.6957(9)
_cell_length_c                   16.2513(10)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.99
_cell_measurement_theta_min      2.33
_cell_volume                     4742.8(5)
_computing_cell_refinement       'Bruker SAINT 8.32b, 2013'
_computing_data_collection       'Bruker APEX2 2013.6-2, 2013'
_computing_data_reduction        'Bruker SAINT 8.32b, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL XT 2013/5'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            57922
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.114
_diffrn_reflns_theta_min         1.843
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.104
_exptl_absorpt_correction_T_max  0.6812
_exptl_absorpt_correction_T_min  0.5183
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.281
_exptl_crystal_size_mid          0.266
_exptl_crystal_size_min          0.182
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         12020
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0199
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+2.4021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0444
_refine_ls_wR_factor_ref         0.0455
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10955
_reflns_number_total             12020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01164_si_001.cif
_cod_data_source_block           afh391
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not_measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4348451
_shelx_estimated_absorpt_t_min   0.476
_shelx_estimated_absorpt_t_max   0.602
_shelxl_version_number           2013-3
_shelx_res_checksum              45946
_shelx_hkl_checksum              35099