Structural and Luminescent Properties of Homoleptic Silver(I), Gold(I), and Palladium(II) Complexes with <i>n</i>NHC-<i>tz</i>NHC Heteroditopic Carbene Ligands.
Monticelli, Marco; Baron, Marco; Tubaro, Cristina; Bellemin-Laponnaz, Stéphane; Graiff, Claudia; Bottaro, Gregorio; Armelao, Lidia; Orian, Laura; ACS omega 4 (2019) 4192–4205; doi:10.1021/acsomega.8b03668

data_4515117
_publ_section_title
;
 Structural and Luminescent Properties of Homoleptic Silver(I), Gold(I),
 and Palladium(II) Complexes with <i>n</i>NHC-<i>tz</i>NHC Heteroditopic
 Carbene Ligands.
;
_journal_issue                   2
_journal_name_full               'ACS omega'
_journal_page_first              4192
_journal_page_last               4205
_journal_paper_doi               10.1021/acsomega.8b03668
_journal_volume                  4
_journal_year                    2019
_chemical_formula_moiety
'C19 H23 Ag0.5 Au N6, C19 H22 Ag0.5 Au N6, 3(F6 P), C2 H5 O0.5'
_chemical_formula_sum            'C40 H50 Ag Au2 F18 N12 O0.5 P3'
_chemical_formula_weight         1643.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-12-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-28 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 106.733(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.366(2)
_cell_length_b                   23.882(2)
_cell_length_c                   21.841(2)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21
_cell_measurement_theta_min      5
_cell_volume                     11172.3(17)
_computing_cell_refinement       'APEX-II (2008)'
_computing_data_collection       'APEX-II (2008)'
_computing_data_reduction        'SAINT (2008)'
_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-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0752
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            66312
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.147
_diffrn_reflns_theta_min         1.277
_exptl_absorpt_coefficient_mu    5.776
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.2530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker APEX II SADABS, 2008'
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_description       prism
_exptl_crystal_F_000             6320
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.563
_refine_diff_density_min         -2.029
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         11118
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+59.2277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1399
_refine_ls_wR_factor_ref         0.1671
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6478
_reflns_number_total             11118
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b03668_si_002.cif
_cod_data_source_block           compx
_cod_original_cell_volume        11172.3(18)
_cod_original_formula_sum        'C40 H50 Ag Au2 F18 N12 O0.50 P3'
_cod_database_code               4515117
_shelx_shelxl_version_number     2018/1
_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
 C100-O100
 1.41 with sigma of 0.005
 C100-C101
 1.54 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C6A) = Uanis(C6B) = Uanis(C7A) = Uanis(C7B)
4. Others
 Fixed Sof: H5A(0.5) H5B(0.5) C6A(0.5) H6AA(0.5) H6AB(0.5) C6B(0.5) H6BA(0.5)
 H6BB(0.5) C7A(0.5) H7AA(0.5) H7AB(0.5) C7B(0.5) H7BA(0.5) H7BB(0.5) H22A(0.6)
 H22B(0.6) C23A(0.6) H23A(0.6) H23B(0.6) C23B(0.4) H23C(0.4) H23D(0.4)
 H24A(0.4) H24B(0.4)
 Fixed Uiso: C100(0.17) O100(0.17) C101(0.17)
 Fixed X: C100(0.489399) O100(0.5) C101(0.5584)
 Fixed Y: C100(0.4418) O100(0.430799) C101(0.433)
 Fixed Z: C100(0.8022) O100(0.75) C101(0.853801)
5.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6A(H6AA,H6AB), C6B(H6BA,H6BB), C7A(H7AA,H7AB), C7B(H7BA,H7BB),
 C11(H11A,H11B), C22(H22A,H22B), C23A(H23A,H23B), C23B(H23C,H23D), C24(H24A,
 H24B), C28(H28A,H28B), C100(H10D,H10E)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20),
 C21(H21), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34)
5.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C10(H10A,H10B,H10C), C19(H19A,H19B,H19C), C27(H27A,H27B,
 H27C), C201(H20A,H20B,H20C), C301(H30A,H30B,H30C), C101(H10F,H10G,H10H)
;
_shelx_res_checksum              44494
_shelx_hkl_checksum              95933
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html            ' END'