Syntheses and Electronic Properties of Rhodium(III) Complexes Bearing a Redox-Active Ligand
Sarath Wanniarachchi; Brendan J. Liddle; Brandon Kizer; Jeewantha S. Hewage; Sergey V. Lindeman; James R. Gardinier; Inorganic Chemistry 51 (2012) 10572–10580; doi:10.1021/ic300772h

data_4330561
_publ_contact_author_name
;
;
_publ_section_title
;
 Syntheses and Electronic Properties of Rhodium(III) Complexes Bearing a
 Redox-Active Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10572
_journal_page_last               10580
_journal_paper_doi               10.1021/ic300772h
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'Cl6 Sb, C25 H23 Cl2 N6 Rh, C H2 Cl2'
_chemical_formula_sum            'C26 H25 Cl10 N6 Rh Sb'
_chemical_formula_weight         1000.68
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2012-02-16
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                76.730(3)
_cell_angle_beta                 72.153(3)
_cell_angle_gamma                82.555(3)
_cell_formula_units_Z            2
_cell_length_a                   10.8699(4)
_cell_length_b                   12.7774(4)
_cell_length_c                   13.9834(4)
_cell_measurement_reflns_used    14770
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.5033
_cell_measurement_theta_min      3.5220
_cell_volume                     1795.64(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_details
;
  1 omega    0.00   90.00   1.0000   23.5600
omega____ theta____ kappa____ phi______ frames
    -       11.6800   77.0000 -150.0000 90

  2 omega  -17.00   87.00   1.0000   23.5600
omega____ theta____ kappa____ phi______ frames
    -       11.6800   77.0000    0.0000 104

  3 omega  -43.00   67.00   1.0000   23.5600
omega____ theta____ kappa____ phi______ frames
    -      -11.8363   77.0000   90.0000 110

  4 omega   -1.00   67.00   1.0000   23.5600
omega____ theta____ kappa____ phi______ frames
    -       11.6800 -122.0000   80.0000 68

  5 omega  -18.00   86.00   1.0000   23.5600
omega____ theta____ kappa____ phi______ frames
    -       11.6800   57.0000  120.0000 104

  6 omega   35.00  102.00   1.0000   23.5600
omega____ theta____ kappa____ phi______ frames
    -       11.6800  178.0000 -120.0000 67

  7 omega  -20.00   54.00   1.0000   23.5600
omega____ theta____ kappa____ phi______ frames
    -       11.6800  -99.0000  -30.0000 74

  8 omega  -18.00   86.00   1.0000   23.5600
omega____ theta____ kappa____ phi______ frames
    -       11.6800   57.0000    0.0000 104

  9 omega  -20.00   54.00   1.0000   23.5600
omega____ theta____ kappa____ phi______ frames
    -       11.6800  -99.0000  -90.0000 74

 10 omega  -62.00  -20.00   1.0000   23.5600
omega____ theta____ kappa____ phi______ frames
    -       11.6800  -57.0000  -30.0000 42
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0459367000
_diffrn_orient_matrix_UB_12      0.0082807000
_diffrn_orient_matrix_UB_13      -0.0281478000
_diffrn_orient_matrix_UB_21      -0.0510712000
_diffrn_orient_matrix_UB_22      -0.0019763000
_diffrn_orient_matrix_UB_23      0.0462467000
_diffrn_orient_matrix_UB_31      0.0005037000
_diffrn_orient_matrix_UB_32      0.0565143000
_diffrn_orient_matrix_UB_33      -0.0053228000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            40654
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         3.53
_diffrn_source                   'SuperNova (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    1.985
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.718
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_description       needle
_exptl_crystal_F_000             978
_exptl_crystal_size_max          0.2649
_exptl_crystal_size_mid          0.0937
_exptl_crystal_size_min          0.0272
_refine_diff_density_max         1.921
_refine_diff_density_min         -1.510
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         9202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0228P)^2^+4.4669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0770
_reflns_number_gt                7593
_reflns_number_total             9202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300772h_si_003_04.cif
_cod_data_source_block           trans3_ox_gard12u
_cod_original_cell_volume        1795.65(10)
_cod_database_code               4330561
_chemical_oxdiff_formula         'C25 H23 N6 Sb Cl8 Rh C H2 Cl2'
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32