A methyl-coordinated Rh^<b>III^</b> ion in methylpentaamminerhodium(III)‒chloropentaamminerhodium(III)‒dithionate (0.73/2.27/3)
Harris, Pernille; Kofod, Pauli; Acta Crystallographica Section E 58 (2002) m460–m462; doi:10.1107/S1600536802013466

data_2201420
_publ_section_title
;
 A methyl-coordinated Rh^<b>III^</b> ion in
 methylpentaamminerhodium(III)--chloropentaamminerhodium(III)--dithionate
 (0.73/2.27/3)
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m460
_journal_page_last               m462
_journal_paper_doi               10.1107/S1600536802013466
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac
'[Rh (C H3) (N H3)5 ]0.73 [Rh Cl (N H3)5]2.27 (S2 O6)3'
_chemical_formula_moiety         '0.73Rh N5 C H18, 2.27Rh N5 Cl H15, 3S2 O6'
_chemical_formula_sum            'C0.73 H47.19 Cl2.27 N15 O18 Rh3 S6'
_chemical_formula_weight         1135.58
_chemical_name_systematic        ?
_space_group_IT_number           8
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'I -2y'
_symmetry_space_group_name_H-M   'I 1 m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 97.290(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.271(2)
_cell_length_b                   27.205(3)
_cell_length_c                   9.871(2)
_cell_measurement_reflns_used    474
_cell_measurement_temperature    122.0(10)
_cell_measurement_theta_max      31.0
_cell_measurement_theta_min      4.4
_cell_volume                     1670.4(7)
_computing_cell_refinement       'DIRAX (Duisenberg, 1992)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction
;
EvalCCD (Duisenberg, 1998) and DREAD (Blessing, 1987)
;
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      122.0(10)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\q and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            34422
_diffrn_reflns_theta_full        35.02
_diffrn_reflns_theta_max         35.02
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.109
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Gaussian integration (Coppens, 1970)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.299
_refine_diff_density_min         -1.680
_refine_ls_abs_structure_details 'Flack (1983), 0000 Friedel pairs'
_refine_ls_abs_structure_Flack   0.43(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         7322
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0598P)^2^+6.9449P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1020
_reflns_number_gt                7148
_reflns_number_total             7322
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cm6013.cif
_cod_data_source_block           I
_cod_original_cell_volume        1670.4
_cod_original_sg_symbol_H-M      'I m'
_cod_database_code               2201420
_cod_database_fobs_code          2201420