Syntheses, crystal structures and isomerization kinetics of a series of [Co(dtc)~2~{P(OMe)~3-n~Ph~n~}~2~]^+^ (n = 0–2) complexes (dtc^-^ = N,N-dimethyldithiocarbamate): role of σ-donicity, π-acidity, and cone angle of the P-ligands in the trans influence and trans effect
Iwatsuki, Satoshi; Kashiwamura, Shinsaku; Kashiwabara, Kazuo; Suzuki, Takayoshi; Takagi, Hideo D.; Dalton Transactions  (2003) 2280–2292; doi:10.1039/b301712e

data_7012844
_publ_section_title
;
 Syntheses, crystal structures and isomerization kinetics of a series
 of [Co(dtc)~2~{P(OMe)~3-n~Ph~n~}~2~]^+^ (n = 0--2) complexes
 (dtc^-^ = N,N-dimethyldithiocarbamate): role of \s-donicity, \p-acidity,
 and cone angle of the P-ligands in the trans influence and trans effect
;
_journal_coden_ASTM              DTARAF
_journal_issue                   11
_journal_name_full               'Dalton Transactions'
_journal_page_first              2280
_journal_page_last               2292
_journal_paper_doi               10.1039/b301712e
_journal_year                    2003
_chemical_formula_moiety
'2(C32 H38 Co N2 O2 P2 S4 1+), 2(B F4 1-), (C H4 O)'
_chemical_formula_sum            'C65 H80 B2 Co2 F8 N4 O5 P4 S8'
_chemical_formula_weight         1669.17
_chemical_name_common            trans-[Co(dtc)~2~(PPh~2~(OMe))~2~]BF~4~.0.5MeOH
_chemical_name_systematic
; 
trans-Bis(N,N-dimethyldithiocarbamato)bis(methyl diphenylphosphinito)
cobalt(III) tetrafluoroborate hemimethanol solvate
;
_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                88.261(8)
_cell_angle_beta                 84.228(7)
_cell_angle_gamma                85.066(8)
_cell_formula_units_Z            2
_cell_length_a                   9.6508(5)
_cell_length_b                   10.9697(8)
_cell_length_c                   37.114(3)
_cell_measurement_reflns_used    5443
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      4.2104
_cell_volume                     3893.8(5)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_molecular_graphics    ORTEP
_computing_publication_material  SHELXL-97
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.707
_diffrn_measured_fraction_theta_max 0.707
_diffrn_measurement_details
;
scan:
    Number of images: 900
               Slice: -80.0000 - 100.0000
         Image width: 0.2000
            Exp time: 15.0000
       Rotation axis: Phi
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 85.5886
              2theta: 29.9219
scan:
    Number of images: 260
               Slice: -10.0000 - 42.0000
         Image width: 0.2000
            Exp time: 15.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 0.0000
                 XTD: 85.5886
              2theta: 29.9219
scan:
    Number of images: 260
               Slice: -10.0000 - 42.0000
         Image width: 0.2000
            Exp time: 15.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 90.0000
                 XTD: 85.5886
              2theta: 29.9219
scan:
    Number of images: 260
               Slice: -10.0000 - 42.0000
         Image width: 0.2000
            Exp time: 15.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 180.0000
                 XTD: 85.5886
              2theta: 29.9219
scan:
    Number of images: 260
               Slice: -10.0000 - 42.0000
         Image width: 0.2000
            Exp time: 15.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 270.0000
                 XTD: 85.5886
              2theta: 29.9219
;
_diffrn_measurement_device       'Mercury CCD (2x2 bin mode)'
_diffrn_measurement_device_details
;
AFC7: Eulerian 3-circle
;
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            19442
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         4.21
_diffrn_source_current           180.0000
_diffrn_source_power             9.0000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.790
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.641
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.215
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     897
_refine_ls_number_reflns         12588
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.215
_refine_ls_R_factor_all          0.1202
_refine_ls_R_factor_gt           0.0929
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+14.1476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1756
_refine_ls_wR_factor_ref         0.1879
_reflns_number_gt                10170
_reflns_number_total             12588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            b301712e.txt
_cod_data_source_block           trPPh2OMe
_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 
;
_cod_database_code               7012844