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_4330568
_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
'C30 H26 Cl N7 Rh, 2(C H2 Cl2), C F3 O3 S, 0.88(C6 H14)'
_chemical_formula_sum            'C38.3 H42.37 Cl5 F3 N7 O3 Rh S'
_chemical_formula_weight         1018.00
_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             2011-09-15
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.09.07 svn.r1971, GUI svn.r3853)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 105.548(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9796(4)
_cell_length_b                   32.8756(7)
_cell_length_c                   9.1507(3)
_cell_measurement_reflns_used    12616
_cell_measurement_temperature    99.9
_cell_measurement_theta_max      73.7292
_cell_measurement_theta_min      3.3417
_cell_volume                     4341.5(2)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_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
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
  1 omega -126.00   17.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1487    0.0000   60.0000 143

  2 omega  -80.00  -19.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1487  125.0000  -30.0000 61

  3 omega   41.00   81.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       40.1487 -125.0000  -90.0000 40

  4 omega   47.00   75.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000    0.0000 28

  5 omega   39.00   76.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000   90.0000 37

  6 omega   48.00  135.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -77.0000  -90.0000 87

  7 omega   80.00  138.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   45.0000   60.0000 58

  8 omega   96.00  160.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  125.0000    0.0000 64

  9 omega   33.00   63.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000  -90.0000 30

 10 omega   39.00   72.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000  150.0000 33

 11 omega   33.00   64.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000  -60.0000 31

 12 omega   37.00   76.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000  120.0000 39

 13 omega   94.00  168.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  125.0000 -120.0000 74

 14 omega -119.00   -6.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1487  -77.0000  -30.0000 113

 15 omega -119.00   -6.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1487  -77.0000   60.0000 113

 16 omega -116.00  -14.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1487  -37.0000 -150.0000 102

 17 omega   46.00   71.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   15.0000 -120.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0231462000
_diffrn_orient_matrix_UB_12      -0.0409171000
_diffrn_orient_matrix_UB_13      0.0444164000
_diffrn_orient_matrix_UB_21      0.0569771000
_diffrn_orient_matrix_UB_22      0.0191920000
_diffrn_orient_matrix_UB_23      0.0970394000
_diffrn_orient_matrix_UB_31      -0.1634482000
_diffrn_orient_matrix_UB_32      0.0125009000
_diffrn_orient_matrix_UB_33      -0.0031041000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0728
_diffrn_reflns_av_unetI/netI     0.1184
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23654
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.7292
_diffrn_reflns_theta_min         3.3417
_diffrn_source                   'SuperNova (Cu) x-ray Source'
_exptl_absorpt_coefficient_mu    6.961
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.148
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       plate
_exptl_crystal_F_000             2073
_exptl_crystal_size_max          0.4689
_exptl_crystal_size_mid          0.2479
_exptl_crystal_size_min          0.0202
_refine_diff_density_max         4.384
_refine_diff_density_min         -1.504
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.236
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         8539
_refine_ls_number_restraints     181
_refine_ls_restrained_S_all      1.225
_refine_ls_R_factor_all          0.1414
_refine_ls_R_factor_gt           0.1329
_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^)+(0.0180P)^2^+143.4890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2990
_refine_ls_wR_factor_ref         0.3025
_reflns_number_gt                7560
_reflns_number_total             8539
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300772h_si_003_11.cif
_cod_data_source_block           9_gard10u
_cod_original_cell_volume        4341.48(19)
_cod_original_formula_sum        'C38.30 H42.37 Cl5 F3 N7 O3 Rh S'
_cod_database_code               4330568
_chemical_oxdiff_formula         'C33 H30 N7 Cl4 Rh S O3 F3'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97