Bottom-Up Construction of a CO2-Based Cycle for the Photocarbonylation of Benzene, Promoted by a Rhodium(I) Pincer Complex.
Anaby, Aviel; Feller, Moran; Ben-David, Yehoshoa; Leitus, Gregory; Diskin-Posner, Yael; Shimon, Linda J. W.; Milstein, David; Journal of the American Chemical Society 138 (2016) 9941–9950; doi:10.1021/jacs.6b05128

data_4130610
_publ_section_title
;
 Bottom-Up Construction of a CO2-Based Cycle for the Photocarbonylation of
 Benzene, Promoted by a Rhodium(I) Pincer Complex.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9941
_journal_page_last               9950
_journal_paper_doi               10.1021/jacs.6b05128
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C24 H42 N O P2 Rh'
_chemical_formula_weight         525.43
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.417(2)
_cell_length_b                   29.009(5)
_cell_length_c                   15.317(3)
_cell_measurement_reflns_used    1.92
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      45932
_cell_measurement_theta_min      28.46
_cell_volume                     5072.9(16)
_computing_cell_refinement       'APEX 2'
_computing_data_collection       'Bruker APEX-2'
_computing_data_reduction        'APEX 2'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX - II KappaCCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31646
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.733
_diffrn_reflns_theta_min         2.631
_exptl_absorpt_coefficient_mu    0.814
_exptl_absorpt_correction_T_max  0.9604
_exptl_absorpt_correction_T_min  0.7922
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker APEX-2'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       plate
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.329
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Flack x determined using 3745 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         10199
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+6.0036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0822
_reflns_Friedel_coverage         0.831
_reflns_Friedel_fraction_full    0.909
_reflns_Friedel_fraction_max     0.895
_reflns_number_gt                9019
_reflns_number_total             10199
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b05128_si_002.cif
_cod_data_source_block           complex3
_cod_original_cell_volume        5073.1(16)
_cod_database_code               4130610
_shelx_estimated_absorpt_t_min   0.792
_shelx_estimated_absorpt_t_max   0.960
_shelxl_version_number           2014/6
_shelx_res_checksum              13390
_shelx_hkl_checksum              20713