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_4516004
_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         'C32 H34 Ag2 Br2 N4'
_chemical_formula_sum            'C32 H34 Ag2 Br2 N4'
_chemical_formula_weight         850.19
_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             2018-01-08
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.5640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0472(10)
_cell_length_b                   12.5773(10)
_cell_length_c                   18.2141(15)
_cell_measurement_reflns_used    5863
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.24
_cell_volume                     2988.8(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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0356
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14879
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.968
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.013
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6062
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1338 before and 0.0314 after correction. The Ratio of minimum to maximum transmission is 0.8129. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.889
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.979
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         5263
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0298P)^2^+9.3659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0782
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4400
_reflns_number_total             5263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b00205_si_004.cif
_cod_data_source_block           n111219b
_cod_database_code               4516004
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.623
_shelx_estimated_absorpt_t_min   0.584
_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.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C11(H11A,H11B), C22(H22A,H22B), C30(H30A,H30B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C7(H7), C8(H8), C9(H9), C25(H25), C26(H26), C27(H27),
 C28(H28), C31(H31)
2.c X=CH2 refined with riding coordinates:
 C1(H1A,H1B), C32(H32A,H32B)
2.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C)
;
_shelx_res_checksum              66804
_shelx_hkl_checksum              41726
_olex2_submission_special_instructions 'No special instructions were received'