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_4130609
_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         'C24 H44 N O2 P2 Rh'
_chemical_formula_sum            'C24 H44 N O2 P2 Rh'
_chemical_formula_weight         543.45
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
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_cell_angle_beta                 101.896(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   13.2372(4)
_cell_length_c                   19.6596(5)
_cell_measurement_reflns_used    16701
_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      2.48
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_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'Crystal Clear (Rigaku)'
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_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
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_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku XtaLabPro'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.454
_diffrn_source                   'fine-focus sealed X-ray tube'
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_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
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_exptl_crystal_description       plate
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_exptl_crystal_size_min          0.060
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_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         7967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0277
_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^)+(0.0305P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6596
_reflns_number_total             7967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b05128_si_002.cif
_cod_data_source_block           complex2
_cod_original_cell_volume        2642.18(13)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4130609
_shelx_estimated_absorpt_t_min   0.846
_shelx_estimated_absorpt_t_max   0.954
_shelxl_version_number           2013-4
_shelx_res_checksum              55499
_shelx_hkl_checksum              82544