Synthesis and Stereochemistry of Homoleptic Transition Metal Thiobenzoate Complexes, (Ph4P)[M(SC{O}Ph)3] (M = Mn, Co, and Ni)
Rema Devy; Jagadese J. Vittal; Philip A. W. Dean; Inorganic Chemistry 37 (1998) 6939–6941; doi:10.1021/ic980394j

data_4323242
_publ_contact_author
; 
     Dr. Jagadese J. Vittal
     Department of Chemistry
     National University of Singapore
     SINGAPORE 119 260
;
_publ_contact_author_email       chmjjv@.nus.sg
_publ_contact_author_fax         '(65) 779 1691'
_publ_contact_author_phone       '(65) 874 2975'
_publ_section_title
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 Synthesis and Stereochemistry of Homoleptic Transition Metal Thiobenzoate
 Complexes, (Ph4P)[M(SC{O}Ph)3] (M = Mn, Co, and Ni)
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6939
_journal_page_last               6941
_journal_paper_doi               10.1021/ic980394j
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source        'see text'
_chemical_formula_moiety         '(Ph~4~P)[Mn(SCOPh)~3~] '
_chemical_formula_sum            'C45 H35 Mn O3 P S3'
_chemical_formula_weight         805.82
_chemical_name_systematic
; 
Tetraphenylphosphonium tri(thiobenzoato-O,S)manganate(II)' 
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   13.2996(5)
_cell_length_b                   13.2996(5)
_cell_length_c                   19.9335(11)
_cell_measurement_reflns_used    3108
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.35
_cell_measurement_theta_min      2.04
_cell_volume                     3053.5(2)
_computing_cell_refinement       'SAINR (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measurement_device       'Siemens SMART CCD System'
_diffrn_measurement_method       'frames \w scans'
_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  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            6366
_diffrn_reflns_theta_max         29.35
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_T_max  0.90773
_exptl_absorpt_correction_T_min  0.3539
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'orange yellow'
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       'big blocks cut into cube'
_exptl_crystal_F_000             1251
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_coef       0.0025(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.042
_refine_ls_goodness_of_fit_obs   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2250
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_restrained_S_obs      1.128
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_obs          0.0532
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+2.2732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1436
_refine_ls_wR_factor_obs         0.1315
_reflns_number_observed          1646
_reflns_number_total             2250
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980394j_2.cif
_cod_data_source_block           jj2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+2.2732P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+2.2732P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4323242