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_4330569
_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
'C42 H35 N8 Rh, 2(C F3 O3 S), 0.5(C4 H8 O), 0.5(C4 H10 O), 0.37(O)'
_chemical_formula_sum            'C48 H44 F6 N8 O7.37 Rh S2'
_chemical_formula_weight         1131.86
_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             2011-09-15
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.09.07 svn.r1971, GUI svn.r3853)
;
_cell_angle_alpha                101.271(3)
_cell_angle_beta                 94.018(3)
_cell_angle_gamma                94.028(3)
_cell_formula_units_Z            2
_cell_length_a                   9.1543(3)
_cell_length_b                   11.7994(5)
_cell_length_c                   22.4495(9)
_cell_measurement_reflns_used    10302
_cell_measurement_temperature    101.7
_cell_measurement_theta_max      73.9603
_cell_measurement_theta_min      3.8309
_cell_volume                     2363.53(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_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    'smtbx-flip (Bourhis, 2008)'
_diffrn_ambient_temperature      101.7
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
  1 omega -111.00  -15.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5237  -37.0000   60.0000 96

  2 omega  -63.00   35.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5237   37.0000 -120.0000 98

  3 omega  -90.00   -6.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5237  125.0000  -30.0000 84

  4 omega   32.00   57.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5237   37.0000  -30.0000 25

  5 omega   40.00   88.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5237 -125.0000  -90.0000 48

  6 omega   59.00  105.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5237   37.0000  -30.0000 46

  7 omega   34.00   77.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000 -120.0000 43

  8 omega   41.00   75.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000 -180.0000 34

  9 omega   67.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   15.0000  120.0000 111

 10 omega   99.00  162.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   45.0000  150.0000 63

 11 omega  103.00  165.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  125.0000  150.0000 62

 12 omega   35.00  113.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378 -113.0000   -1.0000 78

 13 omega   84.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   45.0000 -150.0000 74

 14 omega   34.00   67.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000  120.0000 33

 15 omega   43.00  121.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -77.0000  120.0000 78

 16 omega   32.00   77.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000   60.0000 45

 17 omega   47.00   77.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000  -60.0000 30

 18 omega   34.00  116.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378 -113.0000  104.0000 82

 19 omega   33.00  116.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378 -131.0000  -52.0000 83

 20 omega -121.00    0.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5237  -22.0000  -79.0000 121

 21 omega  -96.00   -2.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5237  125.0000 -120.0000 94

 22 omega -119.00   -7.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5237  -77.0000 -150.0000 112

 23 omega    1.00   28.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5237   92.0000   22.0000 27

 24 omega  -38.00   74.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5237  -77.0000   90.0000 112

 25 omega -140.00  -28.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000  -77.0000  150.0000 112

 26 omega -139.00  -93.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000  -75.0000  -80.0000 46

 27 omega -140.00  -28.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000  -76.0000   45.0000 112

 28 omega   79.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   45.0000 -120.0000 99

 29 omega   29.00  116.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378 -113.0000  104.0000 87

 30 omega   46.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   15.0000    0.0000 132

 31 omega   73.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   77.0000  -30.0000 105

 32 omega   73.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   77.0000  120.0000 105

 33 omega   79.00  164.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   45.0000 -180.0000 85

 34 omega   73.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   77.0000   30.0000 105
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1675564000
_diffrn_orient_matrix_UB_12      0.0073531000
_diffrn_orient_matrix_UB_13      -0.0017663000
_diffrn_orient_matrix_UB_21      0.0221987000
_diffrn_orient_matrix_UB_22      0.1307533000
_diffrn_orient_matrix_UB_23      0.0002976000
_diffrn_orient_matrix_UB_31      -0.0101994000
_diffrn_orient_matrix_UB_32      -0.0265451000
_diffrn_orient_matrix_UB_33      -0.0702080000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36987
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         74.13
_diffrn_reflns_theta_min         3.83
_diffrn_source                   'SuperNova (Cu) x-ray Source'
_exptl_absorpt_coefficient_mu    4.501
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_correction_T_min  0.498
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_description       plate
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.2268
_exptl_crystal_size_mid          0.1315
_exptl_crystal_size_min          0.0172
_refine_diff_density_max         1.800
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         9383
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+3.0789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1143
_reflns_number_gt                7784
_reflns_number_total             9383
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300772h_si_003_12.cif
_cod_data_source_block           10_gard12d
_cod_original_cell_volume        2363.52(16)
_cod_database_code               4330569
_chemical_oxdiff_formula         'C45 N8 H35 O6 F6 S2 Rh'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97