Mechanistic insight into the pyridine enhanced α-selectivity in alkyne hydrothiolation catalysed by quinolinolate‒rhodium(i)‒N-heterocyclic carbene complexes
Palacios, Laura; Di Giuseppe, Andrea; Artigas, María José; Polo, Victor; Lahoz, Fernando J.; Castarlenas, Ricardo; Pérez-Torrente, Jesús J.; Oro, Luis A.; Catal. Sci. Technol. 6 (2016) 8548–; doi:10.1039/C6CY01884J

data_1544478
_publ_section_title
;
 Mechanistic insight into the pyridine enhanced \a-selectivity in alkyne
 hydrothiolation catalysed by quinolinolate--rhodium(i)--N-heterocyclic
 carbene complexes
;
_journal_issue                   24
_journal_name_full               'Catal. Sci. Technol.'
_journal_page_first              8548
_journal_paper_doi               10.1039/C6CY01884J
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         'C44 H56 N3 O Rh'
_chemical_formula_sum            'C44 H56 N3 O Rh'
_chemical_formula_weight         745.82
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_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   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-06-14 deposited with the CCDC.
2016-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.684(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4926(16)
_cell_length_b                   17.417(2)
_cell_length_c                   19.109(3)
_cell_measurement_reflns_used    6083
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.45
_cell_measurement_theta_min      2.16
_cell_volume                     3716.4(9)
_computing_cell_refinement       'APEX2 v. 2009.7 (Bruker AXS, 2008)'
_computing_data_collection       'APEX2 v. 2009.7 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 v. 2009.7 (Bruker AXS, 2008)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'Bruker APEX 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  0.0906
_diffrn_reflns_av_unetI/netI     0.0801
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            42370
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         28.414
_diffrn_reflns_theta_min         1.603
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_T_max  0.5281
_exptl_absorpt_correction_T_min  0.4066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Multi-scan correction included in APEX2 package (Bruker AXS, 2008)
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       Block
_exptl_crystal_F_000             1576
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.143
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         8738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0618
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+3.9214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1242
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6104
_reflns_number_total             8738
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cy01884j2.cif
_cod_data_source_block           compnd_5b
_cod_depositor_comments
'Adding full bibliography for 1544478--1544480.cif.'
_cod_original_cell_volume        3716.5(9)
_cod_database_code               1544478
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              17574
_solvent_exptl_crystal_recrystallization_method toluene/n-hexane