β-(Z)-Selective Alkyne Hydrosilylation by a N,O-Functionalized NHC-based Rhodium(I) Catalyst
Jiménez, M. Victoria; González-Lainez, Miguel; Passarelli, Vincenzo; Pérez-Torrente, Jesús J.; Dalton Transactions  (2023) –; doi:10.1039/D3DT01911J

data_7713576
_publ_section_title
;
 \b-(Z)-Selective Alkyne Hydrosilylation by a N,O-Functionalized NHC-based
 Rhodium(I) Catalyst
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01911J
_journal_year                    2023
_chemical_formula_moiety         'C16 H21 Br N3 O2 Rh'
_chemical_formula_sum            'C16 H21 Br N3 O2 Rh'
_chemical_formula_weight         490.17
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-03-15 deposited with the CCDC.	2023-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.1460(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9388(8)
_cell_length_b                   9.9973(7)
_cell_length_c                   14.8252(10)
_cell_measurement_reflns_used    5227
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.152
_cell_measurement_theta_min      2.494
_cell_volume                     1690.8(2)
_computing_cell_refinement       'APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_collection       'APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  ENCIFER
_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 1.000
_diffrn_measured_fraction_theta_max 0.953
_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  0.0385
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19228
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.538
_diffrn_reflns_theta_min         2.494
_exptl_absorpt_coefficient_mu    3.386
_exptl_absorpt_correction_T_max  0.6656
_exptl_absorpt_correction_T_min  0.5582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Multi-scan correction included in APEX2 package (Bruker AXS, 2008)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_description       prism
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.667
_refine_diff_density_min         -1.196
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         4097
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0367P)^2^+2.9743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0801
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3442
_reflns_number_total             4097
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01911j3.cif
_cod_data_source_block           cmpd_6_VPX83
_cod_depositor_comments
;

2025-04-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C32 H42 Br2 N6 O4 Rh2'
_cod_original_formula_weight         940.35
_cod_original_formula_moiety         'C32 H42 Br2 N6 O4 Rh2'
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7713576
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              62000