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_4121017
_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            'C12 H10 N2'
_chemical_formula_weight         182.22
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
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_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.9342(5)
_cell_length_b                   11.5883(4)
_cell_length_c                   11.6742(3)
_cell_measurement_reflns_used    3160
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.999
_cell_measurement_theta_min      1.527
_cell_volume                     1803.60(10)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13226
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.527
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker Apex 2'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       Block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0616P)^2^+0.3500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.1151
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2583
_reflns_number_total             3160
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja4073832_si_002_6.cif
_cod_data_source_block           compound10
_cod_database_code               4121017
_shelxl_version_number           2013-4
_shelx_res_checksum              16060