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_4330563
_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         'Cl4 Sb, C25 H23 Cl2 N6 Rh, 2(C1 H2 Cl2)'
_chemical_formula_sum            'C27 H27 Cl10 N6 Rh Sb'
_chemical_formula_weight         1014.71
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-02-17
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 105.369(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.2675(4)
_cell_length_b                   15.4317(3)
_cell_length_c                   15.2760(4)
_cell_measurement_reflns_used    12884
_cell_measurement_temperature    100.2(2)
_cell_measurement_theta_max      73.7409
_cell_measurement_theta_min      3.5272
_cell_volume                     3697.68(16)
_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      100.2(2)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
  1 omega  -42.00   24.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6694   37.0000   90.0000 66

  2 omega  -49.00   28.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6694   37.0000  -30.0000 77

  3 omega   67.00  124.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.6694  168.0000  -56.0000 57

  4 omega   58.00   97.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.6694 -129.0000  119.0000 39

  5 omega   70.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.6694   37.0000 -150.0000 26

  6 omega   23.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0171  -94.0000 -120.0000 86

  7 omega   43.00   83.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0171  -30.0000 -180.0000 40

  8 omega   83.00  174.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0171   45.0000  150.0000 91

  9 omega  126.00  165.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0171   45.0000    0.0000 39

 10 omega   94.00  120.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0171   45.0000    0.0000 26

 11 omega   40.00   78.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0171  -30.0000   30.0000 38

 12 omega   37.00  108.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0171 -115.0000   68.0000 71

 13 omega   35.00   99.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0171  -45.0000 -120.0000 64

 14 omega    7.00  119.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.6694   77.0000   30.0000 112

 15 omega   11.00  115.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.6694   57.0000  150.0000 104

 16 omega   11.00  115.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.6694   57.0000  -30.0000 104

 17 omega   32.00   99.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0171  -45.0000   90.0000 67

 18 omega   76.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0171   30.0000   90.0000 102

 19 omega   73.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0171   77.0000 -180.0000 105

 20 omega   77.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0171   61.0000  -30.0000 101

 21 omega   23.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0171  -94.0000   90.0000 86

 22 omega   46.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0171   15.0000  -60.0000 132

 23 omega   49.00  123.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.6694 -168.0000 -123.0000 74

 24 omega   65.00  105.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.6694  168.0000   76.0000 40

 25 omega    7.00  119.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.6694   77.0000 -150.0000 112
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0900810000
_diffrn_orient_matrix_UB_12      -0.0397062000
_diffrn_orient_matrix_UB_13      0.0281099000
_diffrn_orient_matrix_UB_21      0.0388921000
_diffrn_orient_matrix_UB_22      0.0901214000
_diffrn_orient_matrix_UB_23      -0.0059163000
_diffrn_orient_matrix_UB_31      0.0042179000
_diffrn_orient_matrix_UB_32      0.0164126000
_diffrn_orient_matrix_UB_33      0.1005754000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            39390
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.90
_diffrn_reflns_theta_min         4.02
_diffrn_source                   'SuperNova (Cu) x-ray Source'
_exptl_absorpt_coefficient_mu    16.300
_exptl_absorpt_correction_T_max  0.763
_exptl_absorpt_correction_T_min  0.126
_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    1.823
_exptl_crystal_description       needle
_exptl_crystal_F_000             1988
_exptl_crystal_size_max          0.4659
_exptl_crystal_size_mid          0.0298
_exptl_crystal_size_min          0.0225
_refine_diff_density_max         2.141
_refine_diff_density_min         -1.621
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         7374
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0480P)^2^+10.9335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.0985
_reflns_number_gt                6405
_reflns_number_total             7374
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300772h_si_003_06.cif
_cod_data_source_block           cis3_ox_gard12r
_cod_original_cell_volume        3697.66(15)
_cod_database_code               4330563
_chemical_oxdiff_formula         'C25 H23 N6 Sb Cl8 Rh'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97