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#$Date: 2025-08-06 00:02:04 +0300 (Wed, 06 Aug 2025) $
#$Revision: 301518 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/47/7134756.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7134756
loop_
_publ_author_name
'Marquardt, Michael'
'Vendier, Laure'
'Sournia-Saquet, Alix'
'Maurel, Vincent'
'Mouesca, Jean-Marie'
'Bastin, Stéphanie'
'Castillo, Ivan'
'César, Vincent'
_publ_section_title
;
 A non-innocent, π-extended N-heterobicyclic carbene-thiolate
 ligand.
;
_journal_issue                   61
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11437
_journal_page_last               11440
_journal_paper_doi               10.1039/d5cc02841h
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C64 H60 Ag2 N8 Ni2 S4, 2(F6 Sb)'
_chemical_formula_sum            'C64 H60 Ag2 F12 N8 Ni2 S4 Sb2'
_chemical_formula_weight         1874.14
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-05-09 deposited with the CCDC.	2025-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.50210(10)
_cell_length_b                   32.2956(4)
_cell_length_c                   41.3195(5)
_cell_measurement_reflns_used    33699
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.6470
_cell_measurement_theta_min      3.4700
_cell_volume                     15348.8(3)
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            49735
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         68.244
_diffrn_reflns_theta_min         3.474
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.673
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_description       needle
_exptl_crystal_F_000             7391
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.270
_refine_diff_density_min         -1.552
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3527
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0527
_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/[σ²(Fo²)+(0.0831P)²+344.4438P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1513
_refine_ls_wR_factor_ref         0.1526
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3370
_reflns_number_total             3527
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5cc02841h2.cif
_cod_data_source_block           20240124EqA
_cod_depositor_comments
'Adding full bibliography for 7134755--7134757.cif.'
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               7134756
_shelx_shelxl_version_number     2019/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+3/4, y+3/4, -z'
'x+3/4, -y, z+3/4'
'x, -y+1/4, -z+1/4'
'x, y+1/2, z+1/2'
'x+3/4, y+5/4, -z+1/2'
'x+3/4, -y+1/2, z+5/4'
'x, -y+3/4, -z+3/4'
'x+1/2, y, z+1/2'
'x+5/4, y+3/4, -z+1/2'
'x+5/4, -y, z+5/4'
'x+1/2, -y+1/4, -z+3/4'
'x+1/2, y+1/2, z'
'x+5/4, y+5/4, -z'
'x+5/4, -y+1/2, z+3/4'
'x+1/2, -y+3/4, -z+1/4'
'-x, -y, -z'
'-x-3/4, -y-3/4, z'
'-x-3/4, y, -z-3/4'
'-x, y-1/4, z-1/4'
'-x, -y+1/2, -z+1/2'
'-x-3/4, -y-1/4, z+1/2'
'-x-3/4, y+1/2, -z-1/4'
'-x, y+1/4, z+1/4'
'-x+1/2, -y, -z+1/2'
'-x-1/4, -y-3/4, z+1/2'
'-x-1/4, y, -z-1/4'
'-x+1/2, y-1/4, z+1/4'
'-x+1/2, -y+1/2, -z'
'-x-1/4, -y-1/4, z'
'-x-1/4, y+1/2, -z-3/4'
'-x+1/2, y+1/4, z-1/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.125000 0.57571(2) 0.625000 0.0402(2) Uani 1 2 d S T P . .
Ni1 Ni 0.34112(10) 0.625000 0.625000 0.0202(3) Uani 1 2 d S T P . .
S1 S 0.33079(11) 0.55698(3) 0.62501(3) 0.0234(3) Uani 1 1 d . . . . .
C8 C 0.3481(4) 0.54715(15) 0.58361(12) 0.0233(9) Uani 1 1 d . . . . .
N1 N 0.3585(3) 0.58256(13) 0.56565(10) 0.0221(8) Uani 1 1 d . . . . .
C10 C 0.3556(4) 0.62149(14) 0.57873(12) 0.0218(10) Uani 1 1 d . . . . .
N2 N 0.3726(3) 0.64614(14) 0.55256(10) 0.0238(9) Uani 1 1 d . . . . .
C12 C 0.3853(5) 0.62398(16) 0.52438(13) 0.0271(11) Uani 1 1 d . . . . .
H12 H 0.397395 0.635238 0.503401 0.032 Uiso 1 1 calc R U . . .
C13 C 0.3775(4) 0.58279(16) 0.53193(13) 0.0255(10) Uani 1 1 d . . . . .
C14 C 0.3863(4) 0.54397(17) 0.51608(14) 0.0304(11) Uani 1 1 d . . . . .
H14 H 0.399892 0.542603 0.493422 0.037 Uiso 1 1 calc R U . . .
C15 C 0.3750(4) 0.50880(17) 0.53379(14) 0.0312(12) Uani 1 1 d . . . . .
H15 H 0.379727 0.482786 0.523139 0.037 Uiso 1 1 calc R U . . .
C16 C 0.3560(4) 0.50971(16) 0.56838(13) 0.0285(11) Uani 1 1 d . . . . .
H16 H 0.349182 0.484690 0.580319 0.034 Uiso 1 1 calc R U . . .
C17 C 0.3795(4) 0.69093(16) 0.55254(12) 0.0250(10) Uani 1 1 d . . . . .
C18 C 0.2789(5) 0.71320(17) 0.54509(12) 0.0303(11) Uani 1 1 d . . . . .
C19 C 0.2874(6) 0.75587(18) 0.54518(14) 0.0402(14) Uani 1 1 d . . . . .
H19 H 0.220533 0.771943 0.540276 0.048 Uiso 1 1 calc R U . . .
C20 C 0.3916(6) 0.77597(18) 0.55228(15) 0.0422(15) Uani 1 1 d . . . . .
C21 C 0.4898(6) 0.75251(16) 0.55975(14) 0.0379(13) Uani 1 1 d . . . . .
H21 H 0.560441 0.766180 0.564994 0.045 Uiso 1 1 calc R U . . .
C22 C 0.4862(5) 0.70959(15) 0.55966(12) 0.0283(10) Uani 1 1 d . . . . .
C23 C 0.5922(5) 0.68435(18) 0.56850(15) 0.0371(12) Uani 1 1 d . . . . .
H23A H 0.659531 0.702713 0.570666 0.056 Uiso 1 1 calc R U . . .
H23B H 0.607260 0.663897 0.551485 0.056 Uiso 1 1 calc R U . . .
H23C H 0.578400 0.670058 0.589066 0.056 Uiso 1 1 calc R U . . .
C24 C 0.3986(8) 0.8230(2) 0.5533(2) 0.064(2) Uani 1 1 d . . . . .
H24A H 0.457025 0.832584 0.537794 0.096 Uiso 1 1 calc R U . . .
H24B H 0.420579 0.831894 0.575169 0.096 Uiso 1 1 calc R U . . .
H24C H 0.322691 0.834752 0.547736 0.096 Uiso 1 1 calc R U . . .
C25 C 0.1669(5) 0.6915(2) 0.53782(15) 0.0414(14) Uani 1 1 d . . . . .
H25A H 0.179285 0.671253 0.520502 0.062 Uiso 1 1 calc R U . . .
H25B H 0.108656 0.711825 0.530889 0.062 Uiso 1 1 calc R U . . .
H25C H 0.139289 0.677261 0.557299 0.062 Uiso 1 1 calc R U . . .
Sb1 Sb 0.375000 0.375000 0.54774(2) 0.03142(19) Uani 1 2 d S T P . .
F1A F 0.2644(9) 0.4148(3) 0.5570(3) 0.0673(11) Uiso 0.5 1 d . . P A 1
F2A F 0.4887(9) 0.4157(3) 0.5473(2) 0.0673(11) Uiso 0.5 1 d . . P A 1
F3A F 0.375000 0.375000 0.5927(4) 0.0673(11) Uiso 0.5 2 d S . P A 1
F4A F 0.375000 0.375000 0.5038(4) 0.0673(11) Uiso 0.5 2 d S . P A 1
F4B F 0.4016(17) 0.3376(6) 0.5129(5) 0.0673(11) Uiso 0.25 1 d . . P B 2
F3B F 0.4076(17) 0.3362(6) 0.5791(5) 0.0673(11) Uiso 0.25 1 d . . P A 2
F2B F 0.5273(9) 0.3948(3) 0.5452(2) 0.0673(11) Uiso 0.5 1 d . . P A 2
F1B F 0.2551(9) 0.4140(3) 0.5401(3) 0.0673(11) Uiso 0.5 1 d . . P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0180 0.0090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0730 0.0530 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0310 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0030 0.5090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.0560 5.8950 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3330 0.5570 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1310 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Ag1 S1 151.33(6) . 19_657 ?
S1 Ag1 Ni1 46.97(3) . . ?
S1 Ag1 Ni1 161.70(4) 19_657 . ?
S1 Ag1 Ni1 161.70(4) . 18_675 ?
S1 Ag1 Ni1 46.97(3) 19_657 18_675 ?
Ni1 Ag1 Ni1 114.73(4) . 18_675 ?
S1 Ag1 Ag1 104.34(3) . 18_675 ?
S1 Ag1 Ag1 104.34(3) 19_657 18_675 ?
Ni1 Ag1 Ag1 57.365(17) . 18_675 ?
Ni1 Ag1 Ag1 57.365(18) 18_675 18_675 ?
C10 Ni1 C10 170.1(3) . 4_566 ?
C10 Ni1 S1 93.63(14) . 4_566 ?
C10 Ni1 S1 86.91(14) 4_566 4_566 ?
C10 Ni1 S1 86.91(14) . . ?
C10 Ni1 S1 93.63(14) 4_566 . ?
S1 Ni1 S1 173.81(9) 4_566 . ?
C10 Ni1 N1 25.74(16) . . ?
C10 Ni1 N1 152.68(16) 4_566 . ?
S1 Ni1 N1 119.31(9) 4_566 . ?
S1 Ni1 N1 61.19(9) . . ?
C10 Ni1 N1 152.69(17) . 4_566 ?
C10 Ni1 N1 25.74(16) 4_566 4_566 ?
S1 Ni1 N1 61.19(9) 4_566 4_566 ?
S1 Ni1 N1 119.31(9) . 4_566 ?
N1 Ni1 N1 171.87(17) . 4_566 ?
C10 Ni1 Ag1 92.36(15) . . ?
C10 Ni1 Ag1 96.01(15) 4_566 . ?
S1 Ni1 Ag1 119.54(6) 4_566 . ?
S1 Ni1 Ag1 54.27(4) . . ?
N1 Ni1 Ag1 78.30(8) . . ?
N1 Ni1 Ag1 108.79(9) 4_566 . ?
C10 Ni1 Ag1 96.02(15) . 18_675 ?
C10 Ni1 Ag1 92.36(15) 4_566 18_675 ?
S1 Ni1 Ag1 54.27(4) 4_566 18_675 ?
S1 Ni1 Ag1 119.54(6) . 18_675 ?
N1 Ni1 Ag1 108.79(9) . 18_675 ?
N1 Ni1 Ag1 78.30(8) 4_566 18_675 ?
Ag1 Ni1 Ag1 65.27(3) . 18_675 ?
C8 S1 Ni1 100.05(16) . . ?
C8 S1 Ag1 98.89(16) . . ?
Ni1 S1 Ag1 78.76(5) . . ?
C16 C8 N1 118.9(5) . . ?
C16 C8 S1 128.2(4) . . ?
N1 C8 S1 112.8(4) . . ?
C8 N1 C10 123.4(4) . . ?
C8 N1 C13 123.6(4) . . ?
C10 N1 C13 112.9(4) . . ?
C8 N1 Ni1 85.9(3) . . ?
C10 N1 Ni1 37.6(2) . . ?
C13 N1 Ni1 150.3(3) . . ?
N2 C10 N1 102.8(4) . . ?
N2 C10 Ni1 140.4(4) . . ?
N1 C10 Ni1 116.7(3) . . ?
C10 N2 C12 112.6(4) . . ?
C10 N2 C17 126.5(4) . . ?
C12 N2 C17 120.9(4) . . ?
C13 C12 N2 107.8(5) . . ?
C12 C13 N1 103.9(4) . . ?
C12 C13 C14 138.5(5) . . ?
N1 C13 C14 117.6(5) . . ?
C15 C14 C13 118.9(5) . . ?
C14 C15 C16 122.0(5) . . ?
C8 C16 C15 118.9(5) . . ?
C18 C17 C22 123.5(5) . . ?
C18 C17 N2 118.0(4) . . ?
C22 C17 N2 118.6(4) . . ?
C19 C18 C17 117.0(5) . . ?
C19 C18 C25 121.9(5) . . ?
C17 C18 C25 121.1(5) . . ?
C18 C19 C20 121.7(6) . . ?
C19 C20 C21 119.3(5) . . ?
C19 C20 C24 121.1(6) . . ?
C21 C20 C24 119.5(7) . . ?
C22 C21 C20 121.2(6) . . ?
C21 C22 C17 117.2(5) . . ?
C21 C22 C23 121.0(5) . . ?
C17 C22 C23 121.8(5) . . ?
F4A Sb1 F3B 134.7(6) . 30_665 ?
F3B Sb1 F3B 90.6(12) 30_665 . ?
F4A Sb1 F1A 102.0(3) . 30_665 ?
F4A Sb1 F1A 102.0(3) . . ?
F1A Sb1 F1A 156.1(7) 30_665 . ?
F4A Sb1 F2A 89.4(3) . . ?
F1A Sb1 F2A 90.5(5) 30_665 . ?
F1A Sb1 F2A 89.7(5) . . ?
F4A Sb1 F2A 89.4(3) . 30_665 ?
F1A Sb1 F2A 89.7(5) 30_665 30_665 ?
F1A Sb1 F2A 90.5(5) . 30_665 ?
F2A Sb1 F2A 178.9(6) . 30_665 ?
F4A Sb1 F3A 180.0 . . ?
F1A Sb1 F3A 78.0(3) 30_665 . ?
F1A Sb1 F3A 78.0(3) . . ?
F2A Sb1 F3A 90.6(3) . . ?
F2A Sb1 F3A 90.6(3) 30_665 . ?
F4A Sb1 F2B 86.8(3) . 30_665 ?
F1A Sb1 F2B 114.8(4) 30_665 30_665 ?
F1A Sb1 F2B 66.7(4) . 30_665 ?
F2A Sb1 F2B 154.6(4) . 30_665 ?
F2A Sb1 F2B 25.2(3) 30_665 30_665 ?
F3A Sb1 F2B 93.2(3) . 30_665 ?
F3B Sb1 F2B 89.8(7) 30_665 . ?
F3B Sb1 F2B 94.7(7) . . ?
F2B Sb1 F2B 173.5(6) 30_665 . ?
F3B Sb1 F1B 61.1(7) 30_665 . ?
F3B Sb1 F1B 136.0(7) . . ?
F2B Sb1 F1B 62.4(4) 30_665 . ?
F2B Sb1 F1B 116.4(4) . . ?
F4A Sb1 F1B 80.4(3) . 30_665 ?
F3B Sb1 F1B 136.0(7) 30_665 30_665 ?
F3B Sb1 F1B 61.1(7) . 30_665 ?
F1A Sb1 F1B 21.8(4) 30_665 30_665 ?
F1A Sb1 F1B 176.4(5) . 30_665 ?
F2A Sb1 F1B 87.5(5) . 30_665 ?
F2A Sb1 F1B 92.3(5) 30_665 30_665 ?
F3A Sb1 F1B 99.6(3) . 30_665 ?
F2B Sb1 F1B 116.4(4) 30_665 30_665 ?
F2B Sb1 F1B 62.4(4) . 30_665 ?
F1B Sb1 F1B 160.7(6) . 30_665 ?
F1B F4B Sb1 65.6(8) 30_665 . ?
Sb1 F3B F1B 60.9(7) . 30_665 ?
Sb1 F2B F1B 59.5(4) . 30_665 ?
F4B F1B Sb1 66.2(8) 30_665 . ?
Sb1 F1B F3B 58.0(7) . 30_665 ?
Sb1 F1B F2B 58.1(4) . 30_665 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 S1 2.4431(13) . ?
Ag1 S1 2.4432(13) 19_657 ?
Ag1 Ni1 2.9519(11) . ?
Ag1 Ni1 2.9519(11) 18_675 ?
Ag1 Ag1 3.1839(15) 18_675 ?
Ni1 C10 1.923(5) . ?
Ni1 C10 1.923(5) 4_566 ?
Ni1 S1 2.2001(11) 4_566 ?
Ni1 S1 2.2001(11) . ?
Ni1 N1 2.817(4) . ?
Ni1 N1 2.817(4) 4_566 ?
S1 C8 1.751(5) . ?
C8 C16 1.366(7) . ?
C8 N1 1.369(6) . ?
N1 C10 1.369(6) . ?
N1 C13 1.410(7) . ?
C10 N2 1.357(7) . ?
N2 C12 1.375(7) . ?
N2 C17 1.449(7) . ?
C12 C13 1.369(8) . ?
C13 C14 1.418(7) . ?
C14 C15 1.358(8) . ?
C15 C16 1.446(8) . ?
C17 C18 1.397(7) . ?
C17 C22 1.399(7) . ?
C18 C19 1.381(8) . ?
C18 C25 1.497(8) . ?
C19 C20 1.394(10) . ?
C20 C21 1.394(9) . ?
C20 C24 1.521(8) . ?
C21 C22 1.387(7) . ?
C22 C23 1.511(8) . ?
Sb1 F4A 1.814(15) . ?
Sb1 F3B 1.84(2) 30_665 ?
Sb1 F3B 1.841(19) . ?
Sb1 F1A 1.848(10) 30_665 ?
Sb1 F1A 1.848(10) . ?
Sb1 F2A 1.854(10) . ?
Sb1 F2A 1.854(10) 30_665 ?
Sb1 F3A 1.860(15) . ?
Sb1 F2B 1.867(10) 30_665 ?
Sb1 F2B 1.867(10) . ?
Sb1 F1B 1.895(10) . ?
Sb1 F1B 1.895(10) 30_665 ?
F4B F1B 1.55(2) 30_665 ?
F3B F1B 1.90(2) 30_665 ?
F2B F1B 1.948(13) 30_665 ?
