Alkylation of Nonbridging Thiolato Groups in an S-bridged CoIIIPdIICoIII Trinuclear Complex: Control of Geometrical Isomerism by Tuning Trans Influence Due to Sulfur Donors
Yu Chikamoto; Masakazu Hirotsu; Tatsuya Kawamoto; Takumi Konno; Chemistry Letters 34 (2005) 362–; doi:10.1246/cl.2005.362

data_8000009
_publ_contact_author
;
     Takumi Konno
  Department of Chemistry, Graduate School of Science, Osaka University, 
Toyonaka, Osaka, 560-0043, Japan
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_publ_section_title
;
 Alkylation of Nonbridging Thiolato Groups in an S-bridged
 CoIIIPdIICoIII Trinuclear Complex: Control of Geometrical Isomerism by
 Tuning Trans Influence Due to Sulfur Donors
;
_journal_issue                   3
_journal_name_full               'Chemistry Letters'
_journal_page_first              362
_journal_paper_doi               10.1246/cl.2005.362
_journal_volume                  34
_journal_year                    2005
_chemical_formula_moiety         'C26 H68 Cl4 Co2 N6 O9 Pd S6'
_chemical_formula_sum            'C26 H68 Cl4 Co2 N6 O9 Pd S6'
_chemical_formula_weight         1167.28
_space_group_IT_number           2
_symmetry_cell_setting           monoclinic
_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
_cell_angle_alpha                111.309(14)
_cell_angle_beta                 98.741(15)
_cell_angle_gamma                104.056(14)
_cell_formula_units_Z            2
_cell_length_a                   13.024(2)
_cell_length_b                   16.762(3)
_cell_length_c                   12.618(2)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      12.9
_cell_volume                     2399.8(8)
_computing_cell_refinement       WinAFC
_computing_data_collection       WinAFC
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.6.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0868
_diffrn_reflns_av_sigmaI/netI    0.1089
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12530
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.59
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.586
_exptl_absorpt_correction_T_max  0.7420
_exptl_absorpt_correction_T_min  0.6146
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.998
_refine_diff_density_min         -1.594
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       0.0022(5)
_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_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         11050
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1497
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0982P)^2^+1.7663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1629
_refine_ls_wR_factor_ref         0.2015
_reflns_number_gt                5486
_reflns_number_total             11050
_reflns_threshold_expression     >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1   '
_cod_database_code               8000009