Mechanistic study of the rhodium-catalyzed carboxylation of simple aromatic compounds with carbon dioxide
Suga, Takuya; Saitou, Takanobu; Takaya, Jun; Iwasawa, Nobuharu; Chem. Sci. 8 (2017) 1454–; doi:10.1039/C6SC03838G

data_1544287
_publ_section_title
;
 Mechanistic study of the rhodium-catalyzed carboxylation of simple
 aromatic compounds with carbon dioxide
;
_journal_issue                   2
_journal_name_full               'Chem. Sci.'
_journal_page_first              1454
_journal_paper_doi               10.1039/C6SC03838G
_journal_volume                  8
_journal_year                    2017
_chemical_formula_sum            'C50 H86 P3 Rh'
_chemical_formula_weight         883.01
_chemical_name_systematic
; 
 ? 
;
_chemical_properties_physical    ', Air-sensitive,Oxygen-sensitive'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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
;
2016-08-10 deposited with the CCDC.
2016-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.7248(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4706(12)
_cell_length_b                   22.650(3)
_cell_length_c                   19.939(2)
_cell_measurement_reflns_used    11283
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.4816
_cell_measurement_theta_min      3.0630
_cell_volume                     4674.0(9)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2009)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2009)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2009)'
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn724+ CCD'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            57824
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    0.501
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9104
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.582
_refine_diff_density_min         -1.035
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         10687
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0728P)^2^+5.6485P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1462
_reflns_number_gt                8948
_reflns_number_total             10687
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6sc03838g2.cif
_cod_data_source_block           crystalclear
_cod_depositor_comments          'Adding full bibliography for 1544287.cif.'
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               1544287