NHC Pd(II) and Ag(I) Complexes: Synthesis, Structure, and Catalytic Activity in Three Types of C-C Coupling Reactions.
Liu, Qing-Xiang; Hu, Ze-Liang; Yu, Shao-Cong; Zhao, Zhi-Xiang; Wei, Deng-Che; Li, Hui-Long; ACS omega 3 (2018) 4035–4047; doi:10.1021/acsomega.8b00205

data_4516005
_publ_section_title
;
 NHC Pd(II) and Ag(I) Complexes: Synthesis, Structure, and Catalytic
 Activity in Three Types of C-C Coupling Reactions.
;
_journal_issue                   4
_journal_name_full               'ACS omega'
_journal_page_first              4035
_journal_page_last               4047
_journal_paper_doi               10.1021/acsomega.8b00205
_journal_volume                  3
_journal_year                    2018
_chemical_formula_moiety         'C30 H34 Cl4 N4 Pd2'
_chemical_formula_sum            'C30 H34 Cl4 N4 Pd2'
_chemical_formula_weight         805.21
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-13
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.02.02 svn.r3481 for OlexSys, GUI svn.r5470)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.4640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0687(14)
_cell_length_b                   8.9504(6)
_cell_length_c                   18.1404(13)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.56
_cell_volume                     3124.8(4)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0151
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15329
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.003
_diffrn_reflns_theta_max         25.003
_diffrn_reflns_theta_min         2.116
_exptl_absorpt_coefficient_mu    1.520
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_description       block
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.285
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         5460
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0567P)^2^+9.4858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1166
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4857
_reflns_number_total             5460
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b00205_si_002.cif
_cod_data_source_block           90530a
_cod_database_code               4516005
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.771
_shelx_estimated_absorpt_t_min   0.676
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H20B-H10A
 2.05 with sigma of 0.001
 H20A-H19C
 2.05 with sigma of 0.001
 H19A-H21B
 2.05 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Riding coordinates:
 C17(H17A,H17B,H17C)
4.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B), C21(H21A,H21B), C29(H29A,H29B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C24(H24), C25(H25), C26(H26), C27(H27)
4.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C30(H30A,H30B,H30C)
;
_olex2_submission_special_instructions 'No special instructions were received'