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_4129454
_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            'C18 H17 Cl2 N4 Rh'
_chemical_formula_weight         463.17
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 91.072(2)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   10.6249(18)
_cell_length_b                   24.156(4)
_cell_length_c                   28.702(5)
_cell_measurement_temperature    120(2)
_cell_volume                     7365(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_device_type  'APEX2 v2009.11-0'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.894
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            41951
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.668
_diffrn_reflns_theta_min         1.102
_exptl_absorpt_coefficient_mu    0.919
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.730
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         16981
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+27.7001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1427
_refine_ls_wR_factor_ref         0.1498
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12935
_reflns_number_total             16981
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            '[RhIII(L1-H5)(Cl)2].cif'
_cod_data_source_block           Sugi8
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4129454
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.898
_shelx_estimated_absorpt_t_max   0.982
_shelx_res_checksum              48332
_shelx_hkl_checksum              96088