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_1554446
_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            'C31 H44 N3 P2 Rh'
_chemical_formula_weight         623.54
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 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                 106.2308(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9778(7)
_cell_length_b                   16.1480(10)
_cell_length_c                   17.5888(11)
_cell_measurement_reflns_used    9521
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      66.80
_cell_measurement_theta_min      2.62
_cell_volume                     2993.7(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      230(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20033
_diffrn_reflns_theta_full        66.90
_diffrn_reflns_theta_max         66.90
_diffrn_reflns_theta_min         4.28
_exptl_absorpt_coefficient_mu    5.798
_exptl_absorpt_correction_T_max  0.4767
_exptl_absorpt_correction_T_min  0.3901
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.00021(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         5214
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0462P)^2^+2.7520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                5064
_reflns_number_total             5214
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8qo00892b2.cif
_cod_data_source_block           0708_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               1554446