Oxidative Additions of cyclo-Octasulfur and cyclo-Octaselenium to the Cobalt(II) Complex of 1,3-Bis(dimethylphosphino)propane (dmpp): Crystal Structures and Spectroscopic Properties of [Co(S2O)(dmpp)2]PF6 and [Co(Se2)(dmpp)2]BF4
Takayoshi Suzuki; Naoki Tsuji; Kazuo Kashiwabara; Kazuyuki Tatsumi; Inorganic Chemistry 39 (2000) 3938–3941; doi:10.1021/ic000289l

data_4321261
_publ_section_title
;
 Oxidative Additions of cyclo-Octasulfur and cyclo-Octaselenium to the
 Cobalt(II) Complex of 1,3-Bis(dimethylphosphino)propane (dmpp): Crystal
 Structures and Spectroscopic Properties of [Co(S2O)(dmpp)2]PF6 and
 [Co(Se2)(dmpp)2]BF4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3938
_journal_page_last               3941
_journal_paper_doi               10.1021/ic000289l
_journal_volume                  39
_journal_year                    2000
_chemical_compound_source
' Recrystallized from nitromethane/diethyl ether'
_chemical_formula_analytical     'C14 H36 Co F6 O P5 S2'
_chemical_formula_moiety         'C14 H36 Co O P4 S2 1+, F6 P 1-'
_chemical_formula_structural     '(Co (C7 H18 P2)2 (O S2)) (F6 P)'
_chemical_formula_sum            'C14 H36 Co F6 O P5 S2'
_chemical_formula_weight         612.35
_chemical_melting_point          ?
_chemical_name_common            '[Co(S~2~OS,S')(dmpp)~2~]PF~6~'
_chemical_name_systematic
;
Bis{1,3-bis(dimethylphosphino)propane}{oxodisulfido(2-)-S,S'}cobalt(III)
hexafluorophosphate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             'Tue Jul 21 12:42:30 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 98.05(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.652(5)
_cell_length_b                   11.792(3)
_cell_length_c                   16.253(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      12.3
_cell_measurement_theta_min      10.3
_cell_volume                     2590.7(13)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_molecular_graphics    'teXsan ORTEP'
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC5S'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.065
_diffrn_reflns_av_sigmaI/netI    0.147
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7846
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.27
_diffrn_standards_decay_%        -4.45
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.181
_exptl_absorpt_correction_T_max  0.783
_exptl_absorpt_correction_T_min  0.690
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   Coppens_numerical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1264.00
_exptl_crystal_size_max          0.620
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.88
_refine_diff_density_min         -0.70
_refine_ls_abs_structure_details centrosymmetric
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.970
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3407
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.0117
_refine_ls_shift/su_mean         0.0004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0628
_reflns_number_gt                3407
_reflns_number_total             7559
_reflns_threshold_expression     'I > 3.0\(I)'
_cod_data_source_file            ic000289l_1.cif
_cod_data_source_block           3PF6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2590(1)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4321261