Molecular imine cages with π-basic Au<sub>3</sub>(pyrazolate) faces.
Eren, Noga; Fadaei-Tirani, Farzaneh; Scopelliti, Rosario; Severin, Kay; Chemical science 15 (2024) 3539–3544; doi:10.1039/d3sc06280e

data_1570861
_publ_section_title
;
 Molecular imine cages with &#x3c0;-basic Au<sub>3</sub>(pyrazolate)
 faces.
;
_journal_issue                   10
_journal_name_full               'Chemical science'
_journal_page_first              3539
_journal_page_last               3544
_journal_paper_doi               10.1039/d3sc06280e
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C105 H132 Au6 N18, 4[CH2Cl2]'
_chemical_formula_sum            'C109 H140 Au6 Cl8 N18'
_chemical_formula_weight         3167.78
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-01-09
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-14 deposited with the CCDC.	2024-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                94.8137(12)
_cell_angle_beta                 107.0463(15)
_cell_angle_gamma                107.4465(15)
_cell_formula_units_Z            2
_cell_length_a                   15.6340(3)
_cell_length_b                   17.1978(2)
_cell_length_c                   25.4548(4)
_cell_measurement_reflns_used    32375
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      71.7530
_cell_measurement_theta_min      1.8320
_cell_volume                     6130.61(19)
_computing_cell_refinement       'CrysAlisPro 1.171.43.100a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.104a 64-bit (release 22-12-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.100a (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, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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   -114.00 -59.00   0.50    0.50    --  -74.75 144.00-159.67  110
  2  \w    -74.00 -40.00   0.50    0.50    --  -74.75 143.00 -20.04   68
  3  \w   -111.00 -36.00   0.50    0.50    --  -74.75 144.00  94.23  150
  4  \w   -113.00 -85.00   0.50    0.50    --  -74.75 143.00 151.47   56
  5  \w    -60.00 -34.00   0.50    0.50    --  -74.75 143.00 151.47   52
  6  \w    -74.00 -28.00   0.50    0.50    --  -69.26 125.00 150.00   92
  7  \w    -96.00 -29.00   0.50    0.50    --  -69.26 125.00  60.00  134
  8  \w    -79.00 -37.00   0.50    0.50    --  -74.75 143.00  16.07   84
  9  \w   -111.00 -85.00   0.50    0.50    --  -74.75 143.00  16.07   52
 10  \w   -112.00 -40.00   0.50    0.50    --  -74.75 142.00 -64.14  144
 11  \w    -96.00 -44.00   0.50    0.50    --  -69.26 125.00 -90.00  104
 12  \w    -72.00 -38.00   0.50    0.50    --  -69.26   0.00 150.00   68
 13  \w    -56.00 -29.00   0.50    0.50    --  -66.85   0.00  60.00   54
 14  \w   -112.00 -78.00   0.50    0.50    --  -66.85 -15.00-120.00   68
 15  \w    -65.00 -34.00   0.50    0.50    --  -69.26   0.00-150.00   62
 16  \w     37.00  96.00   0.50    0.50    --   66.10  15.00-120.00  118
 17  \w     42.00 115.00   0.50    0.50    --   69.46  15.00 -30.00  146
 18  \w     86.00 114.00   0.50    0.50    --   69.46  15.00  30.00   56
 19  \w     80.00 111.00   0.50    0.50    --   69.46  15.00  60.00   62
 20  \w     80.00 111.00   0.50    0.50    --   69.46  15.00 120.00   62
 21  \w     45.00  74.00   0.50    0.50    --   69.46  15.00 120.00   58
 22  \w     39.00  64.00   0.50    0.50    --   69.46  15.00  60.00   50
 23  \w     46.00  75.00   0.50    0.50    --   69.46  15.00  30.00   58
 24  \w     49.00 122.00   0.50    0.50    --   78.01  15.00  30.00  146
 25  \w     42.00 106.00   0.50    0.50    --   78.01   0.00 120.00  128
 26  \w     47.00 108.00   0.50    0.50    --   78.01  15.00 -30.00  122
 27  \w     54.00  79.00   0.50    0.50    --   78.01  15.00 -90.00   50
 28  \w     54.00 110.00   0.50    0.50    --   78.01  15.00-180.00  112
 29  \w     30.00  67.00   0.50    0.50    --   66.10 -95.00-120.00   74
 30  \w     61.00  96.00   0.50    0.50    --   69.46-125.00 -30.00   70
 31  \w     41.00  95.00   0.50    0.50    --   69.46-125.00  30.00  108
 32  \w     55.00 105.00   0.50    0.50    --   78.01-125.00 150.00  100
 33  \w     48.00  73.00   0.50    0.50    --   78.01-125.00  60.00   50
 34  \w     43.00  68.00   0.50    0.50    --   78.01-125.00   0.00   50
 35  \w     79.00 104.00   0.50    0.50    --   78.01-125.00   0.00   50
 36  \w     45.00 104.00   0.50    0.50    --   78.01-125.00 -30.00  118
 37  \w     44.00 105.00   0.50    0.50    --   78.01-125.00 -90.00  122
 38  \w     80.00 105.00   0.50    0.50    --   78.01-125.00-150.00   50
 39  \w     78.00 105.00   0.50    0.50    --   78.01-125.00-120.00   54
 40  \w     80.00 105.00   0.50    0.50    --   78.01-125.00  30.00   50
 41  \w     80.00 105.00   0.50    0.50    --   78.01-125.00  60.00   50
 42  \w     77.00 105.00   0.50    0.50    --   78.01-125.00  90.00   56
 43  \w     38.00  67.00   0.50    0.50    --   78.01-125.00  90.00   58
 44  \w     33.00  59.00   0.50    0.50    --   69.46 -95.00 150.00   52
 45  \w     46.00  73.00   0.50    0.50    --   66.10 -95.00  60.00   54
 46  \w     28.00  62.00   0.50    0.50    --   66.10 -95.00  30.00   68
 47  \w     32.00  57.00   0.50    0.50    --   69.46 -95.00 -30.00   50
 48  \w     38.00  63.00   0.50    0.50    --   69.46 -95.00 -90.00   50
 49  \w     38.00  64.00   0.50    0.50    --   66.10 -95.00-180.00   52
 50  \w     33.00  78.00   0.50    0.50    --   69.46 -95.00-150.00   90
 51  \w     34.00  72.00   0.50    0.50    --   66.10 -95.00  90.00   76
 52  \w     28.00  72.00   0.50    0.50    --   66.10 -95.00 150.00   88
;
_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      -0.0322533000
_diffrn_orient_matrix_UB_12      0.0645627000
_diffrn_orient_matrix_UB_13      -0.0313735000
_diffrn_orient_matrix_UB_21      0.1043257000
_diffrn_orient_matrix_UB_22      0.0495537000
_diffrn_orient_matrix_UB_23      0.0078484000
_diffrn_orient_matrix_UB_31      -0.0095973000
_diffrn_orient_matrix_UB_32      -0.0501735000
_diffrn_orient_matrix_UB_33      -0.0557558000
_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  0.0674
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            105980
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         1.848
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.148
_exptl_absorpt_correction_T_max  0.787
_exptl_absorpt_correction_T_min  0.385
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.100a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on Gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_description       prism
_exptl_crystal_F_000             3060
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.430
_refine_diff_density_min         -1.494
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1293
_refine_ls_number_reflns         21590
_refine_ls_number_restraints     2281
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0446
_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/[\s^2^(Fo^2^)+(0.0639P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1119
_refine_ls_wR_factor_ref         0.1184
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16251
_reflns_number_total             21590
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06280e2.cif
_cod_data_source_block           ne02_16_cu
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Gaussian' was
changed to 'gaussian' 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 1570859--1570865.cif.
;
_cod_original_cell_volume        6130.60(18)
_cod_database_code               1570861
_shelx_shelxl_version_number     2019/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C109 H140 Au6 Cl8 N18'
_shelx_estimated_absorpt_t_max   0.659
_shelx_estimated_absorpt_t_min   0.313
_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. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 2A
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: Au1A(0.87) Au1B(0.08) Au1C(0.05) Au2A(0.87) Au2B(0.08) Au2C(0.05)
 Au3A(0.87) Au3B(0.08) Au3C(0.05) Au4A(0.87) Au4B(0.08) Au4C(0.05) Au5A(0.87)
 Au5B(0.08) Au5C(0.05) Au6A(0.87) Au6B(0.08) Au6C(0.05)
5.a Ternary CH refined with riding coordinates:
 C4(H4), C7(H7), C30(H30), C33(H33), C39(H39), C42(H42), C65(H65), C68(H68),
 C74(H74), C77(H77), C100(H100), C103(H103)
5.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C52(H52A,H52B), C53(H53A,
 H53B), C54(H54A,H54B), C87(H87A,H87B), C88(H88A,H88B), C89(H89A,H89B)
5.c Me refined with riding coordinates:
 C43(H43A,H43B,H43C)
5.d Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C14(H14), C15(H15), C16(H16), C20(H20), C22(H22),
 C24(H24), C25(H25), C26(H26), C46(H46), C48(H48), C49(H49), C50(H50), C51(H51),
  C55(H55), C57(H57), C58(H58), C59(H59), C61(H61), C81(H81), C83(H83),
 C84(H84), C85(H85), C86(H86), C90(H90), C92(H92), C94(H94), C95(H95), C96(H96)
5.e Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C31(H31A,
 H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C),
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C44(H44A,H44B,H44C), C66(H66A,H66B,
 H66C), C67(H67A,H67B,H67C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C75(H75A,
 H75B,H75C), C76(H76A,H76B,H76C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C),
 C101(H10A,H10B,H10C), C102(H10D,H10E,H10F), C104(H10G,H10H,H10I), C105(H10J,
 H10K,H10L)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              13372
_shelx_fab_checksum              50655
_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 3.685
_oxdiff_exptl_absorpt_empirical_full_min 0.455