Redox-Noninnocent Behavior of Tris(2-pyridylmethyl)amine Bound to a Lewis Acidic Rh(III) Ion Induced by C-H Deprotonation.
Kotani, Hiroaki; Sugiyama, Takumi; Ishizuka, Tomoya; Shiota, Yoshihito; Yoshizawa, Kazunari; Kojima, Takahiko; Journal of the American Chemical Society 137 (2015) 11222–11225; doi:10.1021/jacs.5b06237

data_4129455
_publ_section_title
;
 Redox-Noninnocent Behavior of Tris(2-pyridylmethyl)amine Bound to a Lewis
 Acidic Rh(III) Ion Induced by C-H Deprotonation.
;
_journal_issue                   35
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11222
_journal_page_last               11225
_journal_paper_doi               10.1021/jacs.5b06237
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C24 H24 Cl2 F6 N4 O6 P Rh'
_chemical_formula_weight         783.25
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   27.044(4)
_cell_length_b                   37.900(6)
_cell_length_c                   12.5753(18)
_cell_measurement_temperature    120(2)
_cell_volume                     12889(3)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'APEX2 v2009.11-0'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            71479
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.728
_diffrn_reflns_theta_min         1.075
_exptl_absorpt_coefficient_mu    0.823
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             6272
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.180
_refine_diff_density_max         2.211
_refine_diff_density_min         -1.360
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     839
_refine_ls_number_reflns         15612
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.289
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+35.6114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.1059
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13661
_reflns_number_total             15612
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            '[RhCl2(COOMeTPA)](PF6).cif'
_cod_data_source_block           Sugi7
_cod_database_code               4129455
_shelx_estimated_absorpt_t_min   0.779
_shelx_estimated_absorpt_t_max   0.866
_shelxl_version_number           2013-4
_shelx_res_checksum              44402
_shelx_hkl_checksum              94660