The constitutional dynamic chemistry of Au<sub>3</sub>(pyrazolate)<sub>3</sub> complexes.
Eren, Noga; Svecova, Renata; Fadaei-Tirani, Farzaneh; Scopelliti, Rosario; Severin, Kay; Dalton transactions (Cambridge, England : 2003) 54 (2025) 12818–12823; doi:10.1039/d5dt01613d

data_1575436
_publ_section_title
;
 The constitutional dynamic chemistry of
 Au<sub>3</sub>(pyrazolate)<sub>3</sub> complexes.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12818
_journal_page_last               12823
_journal_paper_doi               10.1039/d5dt01613d
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C15 H9 Au3 F12 N6'
_chemical_formula_sum            'C15 H9 Au3 F12 N6'
_chemical_formula_weight         1092.18
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-04-02
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-04-02 deposited with the CCDC.	2025-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.1503(10)
_cell_length_b                   13.9998(6)
_cell_length_c                   6.8863(3)
_cell_measurement_reflns_used    3559
_cell_measurement_temperature    139.99(10)
_cell_measurement_theta_max      73.0010
_cell_measurement_theta_min      3.6780
_cell_volume                     2135.44(16)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      139.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -104.00 -77.00   0.50    0.10    --  -66.84   0.00 120.00   54
  2  \w   -103.00 -73.00   0.50    0.10    --  -66.84   0.00 -30.00   60
  3  \w   -104.00 -75.00   0.50    0.10    --  -66.84   0.00-120.00   58
  4  \w   -104.00 -79.00   0.50    0.10    --  -66.84   0.00-180.00   50
  5  \w   -101.00 -75.00   0.50    0.10    --  -69.31   0.00-150.00   52
  6  \w   -104.00 -74.00   0.50    0.10    --  -69.31   0.00  90.00   60
  7  \w   -107.00 -82.00   0.50    0.10    --  -69.31   0.00 150.00   50
  8  \w    -66.00 -35.00   0.50    0.10    --  -66.84 106.00 -35.00   62
  9  \w    -81.00 -56.00   0.50    0.10    --  -69.31 106.00 -35.00   50
 10  \w    -81.00 -56.00   0.50    0.10    --  -69.31 103.00-128.00   50
 11  \w    -78.00 -43.00   0.50    0.10    --  -66.84 103.00-128.00   70
 12  \w     57.00 117.00   0.50    0.10    --   78.10  15.00 -90.00  120
 13  \w     92.00 123.00   0.50    0.10    --   78.10  15.00   0.00   62
 14  \w     49.00  74.00   0.50    0.10    --   78.10  15.00   0.00   50
 15  \w     40.00  66.00   0.50    0.10    --   69.48-103.00 129.00   52
 16  \w     41.00  66.00   0.50    0.10    --   78.10-103.00 129.00   50
 17  \w     27.00  80.00   0.50    0.10    --   66.21-103.00 129.00  106
 18  \w     45.00  84.00   0.50    0.10    --   78.10 -95.00  90.00   78
 19  \w     36.00  76.00   0.50    0.10    --   69.48 -95.00 -60.00   80
 20  \w     33.00  64.00   0.50    0.10    --   69.48-106.00-134.00   62
 21  \w     43.00  90.00   0.50    0.10    --   78.10-106.00-134.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0055556000
_diffrn_orient_matrix_UB_12      0.1057413000
_diffrn_orient_matrix_UB_13      -0.0591463000
_diffrn_orient_matrix_UB_21      -0.0670113000
_diffrn_orient_matrix_UB_22      0.0008364000
_diffrn_orient_matrix_UB_23      -0.0599169000
_diffrn_orient_matrix_UB_31      -0.0178110000
_diffrn_orient_matrix_UB_32      0.0303079000
_diffrn_orient_matrix_UB_33      0.2073052000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            5164
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.986
_diffrn_reflns_theta_min         3.735
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    39.162
_exptl_absorpt_correction_T_max  0.397
_exptl_absorpt_correction_T_min  0.064
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pale colourless'
_exptl_crystal_density_diffrn    3.397
_exptl_crystal_description       needle
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.374
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.042
_refine_diff_density_max         2.614
_refine_diff_density_min         -2.327
_refine_diff_density_rms         0.391
_refine_ls_extinction_coef       0.00008(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1134
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0540
_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^)+(0.1311P)^2^+0.7028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1557
_refine_ls_wR_factor_ref         0.1650
_reflns_Friedel_coverage         0.000
_reflns_number_gt                999
_reflns_number_total             1134
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 172.5828\% 
around [0.01 1.00 -0.04] (reciprocal) or [0.00 0.98 -0.17] (direct)
Component 3 rotated by 64.6594\% 
around [-0.00 0.00 1.00] (reciprocal) or [-0.00 -0.00 1.00] (direct)
Component 4 rotated by 64.7964\% 
around [-0.54 -0.03 0.84] (reciprocal) or [-0.06 -0.01 1.00] (direct)
;
_cod_data_source_file            d5dt01613d2.cif
_cod_data_source_block           rs-14
_cod_depositor_comments
'Adding full bibliography for 1575436--1575439.cif.'
_cod_database_code               1575436
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C15 H9 N6 F12 Au3'
_shelx_estimated_absorpt_t_max   0.290
_shelx_estimated_absorpt_t_min   0.024
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Fixed Sof: H7A(0.5) H7B(0.5) H7C(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8)
4.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_shelx_res_checksum              26595
_shelx_hkl_checksum              52453
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 6.412
_oxdiff_exptl_absorpt_empirical_full_min 0.258
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               4