Separation and Optical Resolution of a Pair of atrop Diastereomers of the Octahedral Rhodium(III) Complex with a Nine-Membered S,S-Chelate Ring
Nobuto Yoshinari; Takumi Konno; Inorganic Chemistry 47 (2008) 7450–7452; doi:10.1021/ic800910e

data_4305978
_publ_contact_author
;
     Takumi Konno
  Department of Chemistry, Graduate School of Science, Osaka University, 
Toyonaka, Osaka, 560-0043, Japan
;
_publ_contact_author_email       ' konno@chem.sci.osaka-u.ac.jp '
_publ_contact_author_fax         ' +81-6-6850-5765 '
_publ_contact_author_phone       ' +81-6-6850-5765 '
_publ_section_title
;
Separation and Optical Resolution of a Pair of atrop Diastereomers of the
Octahedral Rhodium(III) Complex with a Nine-Membered S,S-Chelate Ring
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7450
_journal_page_last               7452
_journal_paper_doi               10.1021/ic800910e
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         '(C20 H40 N3 Rh S3), 2Cl, 4.7(H2 O)'
_chemical_formula_sum            'C20 H48.7 Cl2 N3 O4.35 Rh S3'
_chemical_formula_weight         670.91
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      13
_symmetry_space_group_name_Hall  '-P 2ya'
_symmetry_space_group_name_H-M   'P 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.449(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            14
_cell_length_a                   18.478(3)
_cell_length_b                   22.337(4)
_cell_length_c                   24.275(3)
_cell_measurement_reflns_used    38932
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.0
_cell_volume                     9883(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics    'CrystalStructure 3.6.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1083
_diffrn_reflns_av_sigmaI/netI    0.0868
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            93261
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    1.049
_exptl_absorpt_correction_T_max  0.9494
_exptl_absorpt_correction_T_min  0.6791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             4921
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.204
_refine_diff_density_min         -1.213
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    'riding models'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1148
_refine_ls_number_reflns         22466
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1349
_refine_ls_R_factor_gt           0.0793
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+38.8586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1777
_refine_ls_wR_factor_ref         0.2051
_reflns_number_gt                13779
_reflns_number_total             22466
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800910e_si_002_1.cif
_cod_data_source_block           '[1a]'
_cod_original_cell_volume        9884(3)
_cod_original_formula_sum        'C20 H48.70 Cl2 N3 O4.35 Rh S3'
_cod_database_code               4305978