[Bis(diphenylphosphino)methane]bis(pyridine-2-thiolato <i>N</i>-oxide)cobalt(III) perchlorate diethyl ether solvate
Xu, Hong-Wu; Chen, Zhong-Ning; Wu, Ji-Gui; Acta Crystallographica Section E 58 (2002) m672–m673; doi:10.1107/S1600536802019311

data_2201589
_publ_section_title
;
 [Bis(diphenylphosphino)methane]bis(pyridine-2-thiolato
 <i>N</i>-oxide)cobalt(III) perchlorate diethyl ether solvate
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m672
_journal_page_last               m673
_journal_paper_doi               10.1107/S1600536802019311
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac
'[Co (C5 H4 N O S)2 (C25 H22 P2)] Cl O4, C4 H10 O'
_chemical_formula_moiety         'C35 H30 Co N2 O2 P2 S2 +, Cl O4 -, C4 H10 O'
_chemical_formula_sum            'C39 H40 Cl Co N2 O7 P2 S2'
_chemical_formula_weight         869.17
_chemical_name_systematic
;
[Bis(diphenylphosphino)methane]bis(pyridine-2-thiolato N-oxide)cobalt(III)
perchlorate diethyl ether solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.572(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.730(3)
_cell_length_b                   16.873(4)
_cell_length_c                   18.864(4)
_cell_measurement_reflns_used    4947
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.61
_cell_volume                     4016.5(16)
_computing_cell_refinement       'SMART and SAINT (Siemens, 1994)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'XPREP (Siemens, 1994)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Siemens, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0568
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12116
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_T_max  0.816
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          .34
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .28
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.475
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         6918
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.1246
_refine_ls_R_factor_gt           0.0814
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0203P)^2^+18.3746P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1508
_refine_ls_wR_factor_ref         0.1768
_reflns_number_gt                4927
_reflns_number_total             6918
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob6185.cif
_cod_data_source_block           I
_cod_original_cell_volume        4016.8(16)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2201589
_cod_database_fobs_code          2201589