Bifunctional N-heterocyclic carbene ligands for Cu-catalyzed direct C‒H carboxylation with CO2
Park, Da-Ae; Ryu, Ji Yeon; Lee, Junseong; Hong, Sukwon; RSC Advances 7 (2017) 52496–; doi:10.1039/C7RA11414A

data_7229560
_publ_section_title
;
 Bifunctional N-heterocyclic carbene ligands for Cu-catalyzed direct C--H
 carboxylation with CO2
;
_journal_issue                   83
_journal_name_full               'RSC Advances'
_journal_page_first              52496
_journal_paper_doi               10.1039/C7RA11414A
_journal_volume                  7
_journal_year                    2017
_chemical_formula_sum            'C25 H26 Cl Cu N2'
_chemical_formula_weight         453.47
_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-2014/7
_audit_update_record
;
2017-09-27 deposited with the CCDC.
2017-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                89.092(6)
_cell_angle_beta                 82.857(4)
_cell_angle_gamma                74.117(4)
_cell_formula_units_Z            6
_cell_length_a                   9.9670(8)
_cell_length_b                   18.1432(16)
_cell_length_c                   20.1268(16)
_cell_measurement_temperature    293(2)
_cell_volume                     3472.8(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_unetI/netI     0.0868
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39386
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.636
_diffrn_reflns_theta_min         1.167
_exptl_absorpt_coefficient_mu    1.071
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_description       needle
_exptl_crystal_F_000             1416
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1604
_refine_ls_number_reflns         12486
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1252
_refine_ls_R_factor_gt           0.0636
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0158P)^2^+1.6099P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.1021
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7180
_reflns_number_total             12486
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra11414a2.cif
_cod_data_source_block           hsw2-1
_cod_database_code               7229560
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              9571