An efficient class of bis-NHC salts: applications in Pd-catalyzed reactions under mild reaction conditions
Chiu, Chien-Cheng; Chiu, Hui-Tzu; Lee, Dong-Sheng; Lu, Ta-Jung; RSC Advances 8 (2018) 26407–; doi:10.1039/C8RA04094J

data_7231231
_publ_section_title
;
 An efficient class of bis-NHC salts: applications in Pd-catalyzed
 reactions under mild reaction conditions
;
_journal_issue                   46
_journal_name_full               'RSC Advances'
_journal_page_first              26407
_journal_paper_doi               10.1039/C8RA04094J
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C66 H64 Cl3 N8 O4 Pd2, F6 P, 2(C H2 Cl2)'
_chemical_formula_sum            'C68 H68 Cl7 F6 N8 O4 P Pd2'
_chemical_formula_weight         1667.22
_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
;
2017-05-19 deposited with the CCDC.
2018-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                87.943(3)
_cell_angle_beta                 84.738(3)
_cell_angle_gamma                76.841(3)
_cell_formula_units_Z            2
_cell_length_a                   12.6608(10)
_cell_length_b                   17.1920(14)
_cell_length_c                   18.8963(15)
_cell_measurement_reflns_used    9042
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.409
_cell_measurement_theta_min      2.951
_cell_volume                     3987.7(6)
_computing_cell_refinement       'SAINT V7.34A (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT V7.34A (Bruker AXS, 2006)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 0.997
_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       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            84054
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         2.838
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.7631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.413
_refine_diff_density_min         -2.193
_refine_diff_density_rms         0.181
_refine_ls_extinction_coef       0.0066(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     870
_refine_ls_number_reflns         16416
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1375
_refine_ls_R_factor_gt           0.1096
_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^)+(0.1009P)^2^+76.2741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2830
_refine_ls_wR_factor_ref         0.3036
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12337
_reflns_number_total             16416
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra04094j2.cif
_cod_data_source_block           l1pd
_cod_database_code               7231231
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.831
_shelx_estimated_absorpt_t_max   0.977
_shelx_res_checksum              97162
_shelx_fab_checksum              89568