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_4330564
_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         'C26 H33 Cl2 N5 P Rh, 0.18(C H2 Cl2)'
_chemical_formula_sum            'C26.18 H33.35 Cl2.35 N5 P Rh'
_chemical_formula_weight         635.33
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-03-29
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   31.8629(6)
_cell_length_b                   31.8629(6)
_cell_length_c                   10.9579(3)
_cell_measurement_reflns_used    8016
_cell_measurement_temperature    102.1
_cell_measurement_theta_max      29.5831
_cell_measurement_theta_min      3.6099
_cell_volume                     11124.9(4)
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      102.1
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_details
;
  1 omega  -61.00   42.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6697  -77.0000   60.0000 103

  2 omega  -22.00   30.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6697   77.0000   30.0000 52

  3 omega   11.00   79.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6697 -142.0000 -102.0000 68
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0057967000
_diffrn_orient_matrix_UB_12      0.0205958000
_diffrn_orient_matrix_UB_13      -0.0180078000
_diffrn_orient_matrix_UB_21      0.0005717000
_diffrn_orient_matrix_UB_22      0.0062666000
_diffrn_orient_matrix_UB_23      0.0620701000
_diffrn_orient_matrix_UB_31      0.0214798000
_diffrn_orient_matrix_UB_32      -0.0057119000
_diffrn_orient_matrix_UB_33      0.0032392000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            32752
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.65
_diffrn_reflns_theta_min         3.62
_diffrn_source                   'SuperNova (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.903
_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    1.517
_exptl_crystal_description       needle
_exptl_crystal_F_000             5206
_exptl_crystal_size_max          0.2166
_exptl_crystal_size_mid          0.0426
_exptl_crystal_size_min          0.0294
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         7234
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0186P)^2^+25.8188P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0716
_reflns_number_gt                5607
_reflns_number_total             7234
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300772h_si_003_07.cif
_cod_data_source_block           trans4_gard12f
_cod_database_code               4330564
_chemical_oxdiff_formula         'C26 H33 N5 P Cl2 Rh'
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32