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_7229559
_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            'C27.5 H32 Cl Cu N2 O3.5'
_chemical_formula_weight         545.54
_chemical_name_systematic
;
 ?
;
_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
_audit_update_record
;
2017-09-26 deposited with the CCDC.
2017-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                99.8551(8)
_cell_angle_beta                 103.2083(8)
_cell_angle_gamma                116.2178(7)
_cell_formula_units_Z            2
_cell_length_a                   10.6797(2)
_cell_length_b                   11.1444(2)
_cell_length_c                   13.1053(2)
_cell_measurement_reflns_used    5976
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.20
_cell_measurement_theta_min      2.20
_cell_volume                     1294.49(4)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17569
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.376
_diffrn_reflns_theta_min         2.144
_exptl_absorpt_coefficient_mu    0.981
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       block
_exptl_crystal_F_000             570
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         4739
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0707P)^2^+1.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1329
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3521
_reflns_number_total             4739
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra11414a2.cif
_cod_data_source_block           hsw33_1-1
_cod_original_formula_sum        'C27.50 H32 Cl Cu N2 O3.50'
_cod_database_code               7229559
_shelxl_version_number           2014-3
_shelx_res_checksum              58748