Octahedral Monodithiolene Complexes of Cobalt(III) and Chromium(III). Spectroscopic and Density Functional Theoretical Characterization of S,S'-Coordinated Benzene-1,2-dithiolate(1-) π Radicals.
Carsten Milsmann; Eberhard Bothe; Eckhard Bill; Thomas Weyhermüller; Karl Wieghardt; Inorganic Chemistry 48 (2009) 6211–6221; doi:10.1021/ic900515j

data_4302545
_publ_section_title
;
Octahedral Monodithiolene Complexes of Cobalt(III) and Chromium(III).
Spectroscopic and Density Functional Theoretical Characterization
of S,S'-Coordinated Benzene-1,2-dithiolate(1-) \p Radicals.
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6211
_journal_page_last               6221
_journal_paper_doi               10.1021/ic900515j
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         '2(C12 H22 Cr N4 S2), Cl, F6 P, 2(H2 O)'
_chemical_formula_sum            'C24 H48 Cl Cr2 F6 N8 O2 P S4'
_chemical_formula_weight         893.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 96.073(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.0883(2)
_cell_length_b                   14.6485(4)
_cell_length_c                   17.4787(5)
_cell_measurement_temperature    100(2)
_cell_volume                     1804.68(9)
_computing_cell_refinement       'Bruker AXS Collect Software'
_computing_data_collection       'Bruker AXS Collect Software'
_computing_data_reduction        'Bruker AXS Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker-Nonius KappaCsCD'
_diffrn_measurement_method
'935 images at 1.0 deg. stepwise rotation in omega and phi, 45 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode, 50 kV, 80 mA'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_sigmaI/netI    0.0785
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            52074
_diffrn_reflns_theta_full        33.17
_diffrn_reflns_theta_max         33.17
_diffrn_reflns_theta_min         4.53
_exptl_absorpt_coefficient_mu    1.021
_exptl_absorpt_correction_T_max  0.9603
_exptl_absorpt_correction_T_min  0.8376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Vers. 2006/1, Bruker AXS (2006)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent parallelepiped'
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.017(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         13684
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+0.2971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0701
_reflns_number_gt                10966
_reflns_number_total             13684
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900515j_si_001_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

2020-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         446.68
_cod_original_formula_moiety
'C12 H22 Cr N4 S2, 0.5(Cl), 0.5(F6 P), (H2 O)'
_cod_original_formula_units_Z            4
_cod_original_formula_sum        'C12 H24 Cl0.50 Cr F3 N4 O P0.50 S2'
_cod_database_code               4302545