Hydride‒Rhodium(III)-N-Heterocyclic Carbene Catalyst for Tandem Alkylation/Alkenylation via C‒H Activation
Azpíroz, Ramón; Di Giuseppe, Andrea; Urriolabeitia, Asier; Passarelli, Vincenzo; Polo, Victor; Pérez-Torrente, Jesús J.; Oro, Luis A.; Castarlenas, Ricardo; ACS Catalysis 9 (2019) 9372–; doi:10.1021/acscatal.9b01233

data_4514637
_publ_section_title
;
 Hydride--Rhodium(III)-N-Heterocyclic Carbene Catalyst for Tandem
 Alkylation/Alkenylation via C--H Activation
;
_journal_issue                   10
_journal_name_full               'ACS Catalysis'
_journal_page_first              9372
_journal_paper_doi               10.1021/acscatal.9b01233
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         '4 (C38 H45 Cl N3 Rh), C7 H8'
_chemical_formula_sum            'C159 H188 Cl4 N12 Rh4'
_chemical_formula_weight         2820.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 102.7880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.2298(10)
_cell_length_b                   14.0027(6)
_cell_length_c                   23.0551(11)
_cell_measurement_reflns_used    9855
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.865
_cell_measurement_theta_min      2.323
_cell_volume                     6998.5(5)
_computing_cell_refinement       'SAINT+ v. 6.45 (Bruker AXS, 2003)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.45 (Bruker AXS, 2003)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.12, BrukerAXS'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.0481
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            140709
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.702
_diffrn_reflns_theta_min         1.442
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS: Area-Detector Absorption Correction. (1996)  Bruker-AXS 
 within SAINT+ package, v. 6.45.   
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       prism
_exptl_crystal_F_000             2948
_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         17219
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+4.9754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0752
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14449
_reflns_number_total             17219
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b01233_si_003.cif
_cod_data_source_block           cmpd_2_VPX38_RAL
_cod_database_code               4514637
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              51130
_shelx_hkl_checksum              38296