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_4515116
_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         'C32 H34 Au2 N10, 2(F6 P), C2 H3 N'
_chemical_formula_sum            'C34 H41 Au2 F12 N11 P2'
_chemical_formula_weight         1287.65
_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)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.8310(10)
_cell_angle_gamma                90
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_cell_length_a                   24.845(2)
_cell_length_b                   14.7302(12)
_cell_length_c                   24.302(2)
_cell_measurement_reflns_used    9999
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      4
_cell_volume                     8556.5(12)
_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      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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  0.0571
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            55629
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.754
_diffrn_reflns_theta_min         1.704
_exptl_absorpt_coefficient_mu    7.019
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4230
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker APEX II SADABS, 2008'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.999
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             4944
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.037
_refine_diff_density_min         -2.270
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         10024
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0542
_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^)+(0.0116P)^2^+152.1582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8133
_reflns_number_total             10024
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b03668_si_002.cif
_cod_data_source_block           comp6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        8556.8(12)
_cod_database_code               4515116
_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
 C21-C22A = C22A-C23 = C23-C24 = C21-C22B = C22B-C23
 1.54 with sigma of 0.0035
3. Others
 Fixed Sof: C22A(0.6) H22A(0.6) H22B(0.6) C22B(0.4) H22C(0.4) H22D(0.4)
4.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C22A(H22A,H22B), C22B(H22C,H22D)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C19(H19),
 C20(H20), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32)
4.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C10(H10A,H10B,H10C), C18(H18A,H18B,H18C), C26(H26A,H26B,
 H26C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              40403
_shelx_hkl_checksum              84291
_olex2_submission_special_instructions
'No special instructions were received END'