Tuning the Reactivity of an Actor Ligand for Tandem CO2 and C-H Activations: From Spectator Metals to Metal-Free
Vincent T. Annibale; Daniel A. Dalessandro; Datong Song; Journal of the American Chemical Society 135 (2013) 16175–16183; doi:10.1021/ja4073832

data_4121013
_publ_section_title
;
 Tuning the Reactivity of an Actor Ligand for Tandem CO2 and C-H
 Activations: From Spectator Metals to Metal-Free
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16175
_journal_page_last               16183
_journal_paper_doi               10.1021/ja4073832
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C114 H96 N2 O2 P4 Rh2'
_chemical_formula_weight         1855.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                86.638(4)
_cell_angle_beta                 82.439(4)
_cell_angle_gamma                86.857(4)
_cell_formula_units_Z            2
_cell_length_a                   13.1773(10)
_cell_length_b                   13.8413(11)
_cell_length_c                   25.516(2)
_cell_measurement_reflns_used    16099
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      1.475
_cell_volume                     4600.3(6)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.992
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0942
_diffrn_reflns_av_unetI/netI     0.1087
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            63422
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.475
_exptl_absorpt_coefficient_mu    0.482
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6585
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker Apex 2'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.269
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1093
_refine_ls_number_reflns         16099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1169
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+12.2991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1590
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10411
_reflns_number_total             16099
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja4073832_si_002_2.cif
_cod_data_source_block           compound6
_cod_original_cell_volume        4600.2(6)
_cod_database_code               4121013
_shelxl_version_number           2013-4
_shelx_res_checksum              67087