Selective carbonylation of benzene to benzaldehyde using a phosphorus‒nitrogen PN3P‒rhodium(i) complex
Zhou, Chunhui; Hu, Jinsong; Wang, Yuan; Yao, Changguang; Chakraborty, Priyanka; Li, Huaifeng; Guan, Chao; Huang, Mei-Hui; Huang, Kuo-Wei; Organic Chemistry Frontiers 6 (2019) 721–; doi:10.1039/C8QO00892B

data_1554447
_publ_section_title
;
 Selective carbonylation of benzene to benzaldehyde using a
 phosphorus--nitrogen PN3P--rhodium(i) complex
;
_journal_issue                   6
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              721
_journal_paper_doi               10.1039/C8QO00892B
_journal_volume                  6
_journal_year                    2019
_chemical_formula_sum            'C92 H120 N6 O3 P4 Rh2'
_chemical_formula_weight         1687.64
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-06-04 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 120.9250(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.2408(9)
_cell_length_b                   13.8295(4)
_cell_length_c                   25.4214(7)
_cell_measurement_reflns_used    8674
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      72.2
_cell_measurement_theta_min      3.5
_cell_volume                     8818.6(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  bruker-CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            79256
_diffrn_reflns_theta_full        72.22
_diffrn_reflns_theta_max         72.22
_diffrn_reflns_theta_min         3.52
_exptl_absorpt_coefficient_mu    4.101
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3552.0
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         8674
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+13.8314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0763
_reflns_number_gt                8302
_reflns_number_total             8674
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8qo00892b2.cif
_cod_data_source_block           123
_cod_original_cell_volume        8818.6(4)
_cod_original_sg_symbol_H-M      C_2/c
_cod_database_code               1554447