Square Planar Bis{3,6-bis(trimethylsilyl)benzene-1,2-dithiolato}metal Complexes of CrII, CoIII, and RhII: An Experimental and Density Functional Theoretical Study
Flávio Luiz Benedito; Taras Petrenko; Eckhard Bill; Thomas Weyhermüller; Karl Wieghardt; Inorganic Chemistry 48 (2009) 10913–10925; doi:10.1021/ic9008976

data_4303649
_publ_section_title
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Square Planar Bis{3,6-bis(trimethylsilyl)benzene-1,2-dithiolato}metal
Complexes of CrII, CoIII, and RhII: An Experimental and Density Functional
Theoretical Study
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10913
_journal_page_last               10925
_journal_paper_doi               10.1021/ic9008976
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety
'2 (C16 H36 N), (C24 H40 Cr S4 Si4), 4 (C2 H3 N)'
_chemical_formula_sum            'C64 H124 Cr N6 S4 Si4'
_chemical_formula_weight         1270.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.243(4)
_cell_angle_beta                 81.856(4)
_cell_angle_gamma                74.004(4)
_cell_formula_units_Z            2
_cell_length_a                   14.4962(6)
_cell_length_b                   14.7533(6)
_cell_length_c                   19.0960(8)
_cell_measurement_temperature    100(2)
_cell_volume                     3849.6(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Buker-Nonius KappaCCD'
_diffrn_measurement_method
'1816 images at 0.5 deg. stepwise rotation in omega and phi, 120 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  0.0593
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            67365
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    0.357
_exptl_absorpt_correction_T_max  0.9311
_exptl_absorpt_correction_T_min  0.8846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent parallelepiped'
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.193
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         15106
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+8.4889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.1755
_reflns_number_gt                11336
_reflns_number_total             15106
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9008976_si_002_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_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 
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_cod_database_code               4303649