Incorporation of Pendant Bases into Rh(diphosphine)2 Complexes: Synthesis, Thermodynamic Studies, And Catalytic CO2 Hydrogenation Activity of [Rh(P2N2)2](+) Complexes.
Lilio, Alyssia M.; Reineke, Mark H.; Moore, Curtis E.; Rheingold, Arnold L.; Takase, Michael K.; Kubiak, Clifford P.; Journal of the American Chemical Society 137 (2015) 8251–8260; doi:10.1021/jacs.5b04291

data_4123904
_publ_section_title
;
 Incorporation of Pendant Bases into Rh(diphosphine)2 Complexes:
 Synthesis, Thermodynamic Studies, And Catalytic CO2 Hydrogenation
 Activity of [Rh(P2N2)2](+) Complexes.
;
_journal_issue                   25
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8251
_journal_page_last               8260
_journal_paper_doi               10.1021/jacs.5b04291
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C64 H94 B F4 N6 O4 P4 Rh'
_chemical_formula_weight         1325.05
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_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 109.6649(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.7509(9)
_cell_length_b                   13.4975(6)
_cell_length_c                   22.3982(9)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.01
_cell_measurement_theta_min      2.38
_cell_volume                     6476.9(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 v2014.7-1 (Bruker-AXS, 2014)'
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_computing_molecular_graphics    'Bruker SHELXTL'
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_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0944
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_diffrn_reflns_limit_h_max       37
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_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            93916
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.394
_diffrn_reflns_theta_min         2.207
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.7036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/4 (Sheldrick, 2014)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.200
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_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         15651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0543
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+8.9063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.0984
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10799
_reflns_number_total             15651
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b04291_si_005.cif
_cod_data_source_block           P15037
_cod_database_code               4123904
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.920
_shelx_estimated_absorpt_t_max   0.959
_shelx_res_checksum              37503
_shelx_hkl_checksum              97780