Air-Stable, Well-Defined Palladium–BIAN–NHC Chloro Dimer: Fast-Activating, Highly Efficient Catalyst for Cross-Coupling
Zhang, Jin; Li, Tao; Li, Xue; Zhang, Gaopeng; Fang, Shuai; Yan, Wenxuan; Li, Xiangyang; Yang, Xiufang; Ma, Yangmin; Szostak, Michal; Chemical Communications  (2022) –; doi:10.1039/D2CC02253B

data_7130187
_publ_section_title
;
 Air-Stable, Well-Defined Palladium--BIAN--NHC Chloro Dimer:
 Fast-Activating, Highly Efficient Catalyst for Cross-Coupling
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02253B
_journal_year                    2022
_chemical_formula_moiety         'C74 H80 Cl4 N4 Pd2'
_chemical_formula_sum            'C74 H80 Cl4 N4 Pd2'
_chemical_formula_weight         1380.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-03-17 deposited with the CCDC.	2022-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.362(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.932(5)
_cell_length_b                   15.475(4)
_cell_length_c                   22.985(6)
_cell_measurement_reflns_used    6289
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.40
_cell_volume                     6714(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_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  0.0831
_diffrn_reflns_av_unetI/netI     0.0812
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            44065
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         2.148
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6569
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0722 before and 0.0614 after correction.
The Ratio of minimum to maximum transmission is 0.8810.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       block
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     773
_refine_ls_number_reflns         11815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0637P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1488
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7822
_reflns_number_total             11815
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02253b2.cif
_cod_data_source_block           sust_3047_0m
_cod_database_code               7130187
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.923
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C11(H11), C27(H27), C36(H36), C39(H39), C48(H48), C64(H64), C73(H73)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20),
 C21(H21), C32(H32), C33(H33), C34(H34), C42(H42), C43(H43), C44(H44), C53(H53),
  C54(H54), C55(H55), C58(H58), C59(H59), C60(H60), C67(H67), C68(H68), C71(H71)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C35(H35A,H35B,H35C), C37(H37A,H37B,
 H37C), C38(H38C,H38A,H38B), C40(H40A,H40B,H40C), C47(H47A,H47B,H47C), C49(H49A,
 H49B,H49C), C63(H63A,H63B,H63C), C65(H65A,H65B,H65C), C72(H72A,H72B,H72C),
 C74(H74A,H74B,H74C)
;
_shelx_res_checksum              65611
_shelx_hkl_checksum              3769
_olex2_submission_special_instructions 'No special instructions were received'