Completely stereoselective synthesis of a chiral tetra(tertiary phosphine). Crystal and molecular structure of [OC-6-22-(R*,R*)]-(±)-dichloro{1,2-bis[(2-dimethylphosphinophenyl)methylphosphino]benzene-P,P ',P ″,P ‴}cobalt(III) hexafluorophosphate †
Chatterjee, Swarup; Doyle, Roy; Hockless, David C. R.; Salem, Geoffrey; Willis, Anthony C.; Journal of the Chemical Society, Dalton Transactions  (2000) 1829–; doi:10.1039/b002662j

data_7009677
_publ_section_title
;
 Completely stereoselective synthesis of a chiral tetra(tertiary
 phosphine). Crystal and molecular structure of
 [OC-6-22-(R*,R*)]-(+-)-dichloro{1,2-bis[(2-dimethylphosphinophenyl)methylphosphino]benzene-P,P&#x200A;',P&#x200A;&#x2033;,P&#x200A;&#x2034;}cobalt(III)
 hexafluorophosphate&#x200A;&#x2020;
;
_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1829
_journal_paper_doi               10.1039/b002662j
_journal_year                    2000
_chemical_formula_moiety         'C24 H30 Cl2 Co P4 +, P F6 - '
_chemical_formula_sum            'C24 H30 Cl2 Co F6 P5'
_chemical_formula_weight         717.20
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_audit_creation_date             1999-02-07
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
?
;
_cell_angle_alpha                90
_cell_angle_beta                 95.75(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.630(4)
_cell_length_b                   19.034(4)
_cell_length_c                   12.745(4)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      9.0
_cell_measurement_theta_min      5.9
_cell_volume                     3048.5(15)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1993)
;
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC6S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.05608
_diffrn_orient_matrix_UB_12      0.03190
_diffrn_orient_matrix_UB_13      0.03437
_diffrn_orient_matrix_UB_21      0.04737
_diffrn_orient_matrix_UB_22      -0.04137
_diffrn_orient_matrix_UB_23      0.01723
_diffrn_orient_matrix_UB_31      0.03072
_diffrn_orient_matrix_UB_32      0.00557
_diffrn_orient_matrix_UB_33      -0.06885
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.02435
_diffrn_reflns_av_sigmaI/netI    0.080
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5846
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0.08
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.047
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1456.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.63
_refine_diff_density_min         -0.45
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.600
_refine_ls_goodness_of_fit_ref   1.887
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     343
_refine_ls_number_reflns         3206
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.0380
_refine_ls_shift/su_mean         0.0030
_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_all         0.0518
_refine_ls_wR_factor_ref         0.0461
_reflns_number_gt                3206
_reflns_number_total             5582
_reflns_threshold_expression     I>2.00\s(I)
_cod_data_source_file            b002662j.txt
_cod_data_source_block           salem1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00010|Fo|^2^]' 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) + 0.00010|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3048(1)
_cod_original_sg_symbol_H-M      'P 21/a     '
_cod_original_formula_sum        'C24 H30 Cl2 Co F6 P5 '
_cod_database_code               7009677