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_4130611
_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_moiety         'C30 H48 N O P2 Rh'
_chemical_formula_sum            'C30 H48 N O P2 Rh'
_chemical_formula_weight         603.54
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                93.68(3)
_cell_angle_beta                 106.38(3)
_cell_angle_gamma                91.70(3)
_cell_formula_units_Z            4
_cell_length_a                   10.532(2)
_cell_length_b                   17.220(3)
_cell_length_c                   17.597(4)
_cell_measurement_reflns_used    39222
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
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_computing_cell_refinement       'Software Bruker KappaApex CCD'
_computing_data_collection       'Software Bruker KappaApex CCD'
_computing_data_reduction        'Software Bruker KappaApex CCD'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker KappaApex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
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_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
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_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.573
_diffrn_reflns_theta_min         2.632
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker Apex2'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       prism
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.150
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_refine_diff_density_max         0.703
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         13663
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+2.1027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.0626
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11377
_reflns_number_total             13663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b05128_si_002.cif
_cod_data_source_block           complex5
_cod_original_cell_volume        3051.8(11)
_cod_database_code               4130611
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.881
_shelx_estimated_absorpt_t_max   0.947
_shelx_res_checksum              10724
_shelx_hkl_checksum              98724