Redox Behavior of Rhodium 9,10-Phenanthrenediimine Complexes
David W. Shaffer; Scott A. Ryken; Ryan A. Zarkesh; Alan F. Heyduk; Inorganic Chemistry 50 (2011) 13–21; doi:10.1021/ic1007632

data_4324074
_publ_section_title
;
 Redox Behavior of Rhodium 9,10-Phenanthrenediimine Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13
_journal_page_last               21
_journal_paper_doi               10.1021/ic1007632
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C67 H99 K N4 O9 Rh'
_chemical_formula_weight         1246.51
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.2230(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5891(7)
_cell_length_b                   24.1291(13)
_cell_length_c                   22.6328(12)
_cell_measurement_reflns_used    9228
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.14
_cell_measurement_theta_min      2.28
_cell_volume                     6633.8(6)
_computing_cell_refinement       'Bruker SMART/SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0446
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            76342
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.26
_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_count 'initial 50 frames recollected'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    0.376
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2660
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.081
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     833
_refine_ls_number_reflns         15768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0373P)^2^+3.3311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0874
_reflns_number_gt                11895
_reflns_number_total             15768
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1007632_si_002_2.cif
_cod_data_source_block           afh197
_cod_database_code               4324074