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_4516003
_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         'C38 H36 Ag2 Br2 N6, C H2 Cl2'
_chemical_formula_sum            'C39 H38 Ag2 Br2 Cl2 N6'
_chemical_formula_weight         1037.21
_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   geom
_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                 108.026(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4181(6)
_cell_length_b                   29.944(2)
_cell_length_c                   15.6855(9)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.44
_cell_measurement_theta_min      2.46
_cell_volume                     3759.8(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      173.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18959
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.927
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.348
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1029 before and 0.0425 after correction. The Ratio of minimum to maximum transmission is 0.6688. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         4.565
_refine_diff_density_min         -3.036
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         6595
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0748
_refine_ls_shift/su_max          0.000
_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^+107.0080P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1795
_refine_ls_wR_factor_ref         0.1822
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6065
_reflns_number_total             6595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b00205_si_003.cif
_cod_data_source_block           n110331a
_cod_database_code               4516003
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.670
_shelx_estimated_absorpt_t_min   0.634
_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
 Cl1-Cl2 = Cl1'-Cl2'
 2.92 with sigma of 0.01
 C39-Cl1 = C39-Cl2 = C39'-Cl1' = C39'-Cl2'
 1.78 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C39) \\sim Ueq, Uanis(C39') \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(C24) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C16) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.005
Uanis(Cl1) = Uanis(Cl1')
Uanis(C39) = Uanis(C39')
Uanis(Cl2) = Uanis(Cl2')
4. Others
 Sof(C39')=Sof(H39C)=Sof(H39D)=Sof(Cl1')=Sof(Cl2')=1-FVAR(1)
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(Cl1)=Sof(Cl2)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C14(H14A,H14B), C25(H25A,H25B), C33(H33A,H33B), C39(H39A,H39B),
 C39'(H39C,H39D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12),
 C28(H28), C29(H29), C30(H30), C31(H31), C35(H35), C36(H36), C37(H37), C38(H38)
5.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C)
;
_olex2_submission_special_instructions 'No special instructions were received'