Synthesis and Reactivity of Phosphine-Quinolinolato Rhodium Complexes: Intermediacy of Vinylidene and (Amino)carbene Complexes in the Catalytic Hydroamination of Terminal Alkynes
Takano, Shotaro; Kochi, Takuya; Kakiuchi, Fumitoshi; Organometallics 35 (2016) 4112–; doi:10.1021/acs.organomet.6b00853

data_4089181
_publ_section_title
;
 Synthesis and Reactivity of Phosphine-Quinolinolato Rhodium Complexes:
 Intermediacy of Vinylidene and (Amino)carbene Complexes in the Catalytic
 Hydroamination of Terminal Alkynes
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              4112
_journal_paper_doi               10.1021/acs.organomet.6b00853
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C23 H17 N O2 P Rh'
_chemical_formula_weight         473.26
_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
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 109.920(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9073(15)
_cell_length_b                   13.9158(16)
_cell_length_c                   12.1176(16)
_cell_measurement_reflns_used    8565
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.30
_cell_volume                     1887.7(4)
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
;
 Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13545
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.297
_exptl_absorpt_coefficient_mu    1.009
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_description       platelet
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.134
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3306
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0199P)^2^+3.8640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0704
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3023
_reflns_number_total             3306
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00853_si_001.cif
_cod_data_source_block           7
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4089181
_shelx_estimated_absorpt_t_min   0.688
_shelx_estimated_absorpt_t_max   0.906
_shelxl_version_number           2013-3
_shelx_res_checksum              2438
_shelx_hkl_checksum              66936