Hydrogenation of <i>N</i>-Heteroarenes Using Rhodium Precatalysts: Reductive Elimination Leads to Formation of Multimetallic Clusters.
Kim, Sangmin; Loose, Florian; Bezdek, Máté J; Wang, Xiaoping; Chirik, Paul J.; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b09540

data_4127298
_publ_section_title
;
 Hydrogenation of <i>N</i>-Heteroarenes Using Rhodium Precatalysts:
 Reductive Elimination Leads to Formation of Multimetallic Clusters.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b09540
_journal_year                    2019
_chemical_formula_moiety         'C40 H67 Rh5, C2.5 H6'
_chemical_formula_sum            'C42.5 H73 Rh5'
_chemical_formula_weight         1098.55
_chemical_name_common            (\h5-C5Me5)4Rh5H7.0.5pentane
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                92.034(2)
_cell_angle_beta                 111.670(2)
_cell_angle_gamma                111.675(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8773(5)
_cell_length_b                   13.7328(6)
_cell_length_c                   15.6523(7)
_cell_measurement_reflns_used    9239
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      2.74
_cell_volume                     2160.73(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture Photon 100 CMOS'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_source         'I\mS microfocus source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            118002
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.576
_diffrn_reflns_theta_min         2.739
_exptl_absorpt_coefficient_mu    1.870
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS BRUKER AXS'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_description       block
_exptl_crystal_F_000             1106
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.126
_refine_diff_density_max         1.111
_refine_diff_density_min         -0.929
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         13221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0147P)^2^+4.8210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0574
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11716
_reflns_number_total             13221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b09540_si_003.cif
_cod_data_source_block           Rh5H7_xray
_cod_original_formula_sum        'C42.50 H73 Rh5'
_cod_database_code               4127298
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.738
_shelx_estimated_absorpt_t_max   0.799
_shelx_res_checksum              65238
_shelx_hkl_checksum              7994