Trinuclear gold chains and octanuclear copper gyrobifastigia stabilized using a fluorinated pyridyl ligand.
Phan, Vo Quang Huy; Vanga, Mukundam; Diroll, Benjamin T.; Muñoz-Castro, Alvaro; Dias, H. V. Rasika; Dalton transactions (Cambridge, England : 2003) 54 (2025) 15717–15725; doi:10.1039/d5dt02150b

data_7719502
_publ_section_title
;
 Trinuclear gold chains and octanuclear copper gyrobifastigia stabilized
 using a fluorinated pyridyl ligand.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15717
_journal_page_last               15725
_journal_paper_doi               10.1039/d5dt02150b
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C18 H9 Au3 F9 N3'
_chemical_formula_sum            'C18 H9 Au3 F9 N3'
_chemical_formula_weight         1029.18
_space_group_crystal_system      hexagonal
_space_group_IT_number           170
_space_group_name_Hall           'P 65'
_space_group_name_H-M_alt        'P 65'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2025-03-28
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-06-28 deposited with the CCDC.	2025-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   12.7975(3)
_cell_length_b                   12.7975(3)
_cell_length_c                   21.1838(7)
_cell_measurement_reflns_used    9859
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      30.47
_cell_measurement_theta_min      2.66
_cell_volume                     3004.59(14)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'PHOTON II 7 CPAD'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest Photon II 7'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    '0.6 mm double-pinhole'
_diffrn_radiation_detector       'PHOTON II 7 CPAD'
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            38747
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.685
_diffrn_reflns_theta_min         2.660
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_type              'KFF MO-2KC-90'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.013
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.2904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1373 before and 0.0751 after correction.
The Ratio of minimum to maximum transmission is 0.3892.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rods
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.054
_refine_diff_density_min         -2.324
_refine_diff_density_rms         0.286
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.21(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         5171
_refine_ls_number_restraints     562
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0474
_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^)+117.5217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1123
_reflns_Friedel_coverage         0.948
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                4757
_reflns_number_total             5171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02150b2.cif
_cod_data_source_block           hrd115_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7719502--7719504.cif.
;
_cod_original_cell_volume        3004.59(16)
_cod_database_code               7719502
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.473
_shelx_estimated_absorpt_t_min   0.085
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.79(6)
 0.21(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 C18A-C17A \\sim C18-C17 \\sim C6A-C5A \\sim C6-C5 \\sim C12-C11 \\sim C12A-C11A
 with sigma of 0.004
4. Rigid bond restraints
 N1, N3, N2, N3A, N1A, N2A, C5, C4, C3, C2, C1, C17, C16, C15, C14, C13, C6,
 C18, C11, C10, C9, C8, C7, C12, C18A, C13A, C14A, C15A, C16A, C17A, C6A, C12A,
 C1A, C2A, C3A, C4A, C5A, C7A, C8A, C9A, C10A, C11A, F3, F9, F7, F8, F1, F2, F4,
  F5, F6, F9A, F8A, F7A, F3A, F2A, F4A, F6A, F1A, F5A
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
5. Uiso/Uaniso restraints and constraints
C5 \\sim C4 \\sim C3 \\sim C2 \\sim C1 \\sim C17 \\sim C16 \\sim C15 \\sim C14
\\sim C13 \\sim C6 \\sim C18 \\sim C11 \\sim C10 \\sim C9 \\sim C8 \\sim C7
\\sim C12 \\sim C18A \\sim C13A \\sim C14A \\sim C15A \\sim C16A \\sim C17A
\\sim C6A \\sim C12A \\sim C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim
C7A \\sim C8A \\sim C9A \\sim C10A \\sim C11A: within 1.7A with sigma of 0.005
and sigma for terminal atoms of 0.005 within 1.7A
Uanis(N1) \\sim Ueq, Uanis(N1A) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N2A)
\\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N3A) \\sim Ueq: with sigma of 0.008 and
sigma for terminal atoms of 0.008
6. Others
 Fixed Sof: Au2A(0.5) Au1(0.5) Au2(0.5) Au3(0.5) Au1A(0.5) Au3A(0.5) N1(0.5)
 C5(0.5) C4(0.5) H4(0.5) C3(0.5) H3(0.5) C2(0.5) H2(0.5) C1(0.5) N3(0.5)
 C17(0.5) C16(0.5) H16(0.5) C15(0.5) H15(0.5) C14(0.5) H14(0.5) C13(0.5)
 F3(0.5) F9(0.5) F7(0.5) F8(0.5) F1(0.5) F2(0.5) C6(0.5) C18(0.5) N2(0.5)
 C11(0.5) C10(0.5) H10(0.5) C9(0.5) H9(0.5) C8(0.5) H8(0.5) C7(0.5) F4(0.5)
 F5(0.5) F6(0.5) C12(0.5) F9A(0.5) F8A(0.5) F7A(0.5) C18A(0.5) N3A(0.5)
 C13A(0.5) C14A(0.5) H14A(0.5) C15A(0.5) H15A(0.5) C16A(0.5) H16A(0.5)
 C17A(0.5) F3A(0.5) F2A(0.5) F4A(0.5) C6A(0.5) F6A(0.5) F1A(0.5) F5A(0.5)
 C12A(0.5) N1A(0.5) C1A(0.5) C2A(0.5) H2A(0.5) C3A(0.5) H3A(0.5) C4A(0.5)
 H4A(0.5) C5A(0.5) N2A(0.5) C7A(0.5) C8A(0.5) H8A(0.5) C9A(0.5) H9A(0.5)
 C10A(0.5) H10A(0.5) C11A(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C2(H2), C16(H16), C15(H15), C14(H14), C10(H10), C9(H9),
 C8(H8), C14A(H14A), C15A(H15A), C16A(H16A), C2A(H2A), C3A(H3A), C4A(H4A),
 C8A(H8A), C9A(H9A), C10A(H10A)
7.b Fitted hexagon refined as free rotating group:
 N1(C5,C4,C3,C2,C1), N3(C17,C16,C15,C14,C13), N2(C11,C10,C9,C8,C7), N3A(C13A,
 C14A,C15A,C16A,C17A), N1A(C1A,C2A,C3A,C4A,C5A), N2A(C7A,C8A,C9A,C10A,C11A)
;
_shelx_res_checksum              89110
_olex2_submission_special_instructions 'No special instructions were received'