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_1570860
_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         'C48 H57 Au3 N6 O3, 1.25[CH2Cl2]'
_chemical_formula_sum            'C49.25 H59.5 Au3 Cl2.5 N6 O3'
_chemical_formula_weight         1463.05
_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             2024-01-14
_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                68.300(5)
_cell_angle_beta                 87.800(5)
_cell_angle_gamma                82.613(5)
_cell_formula_units_Z            2
_cell_length_a                   8.3005(6)
_cell_length_b                   17.0876(10)
_cell_length_c                   19.6636(9)
_cell_measurement_reflns_used    9869
_cell_measurement_temperature    229.99(10)
_cell_measurement_theta_max      72.1590
_cell_measurement_theta_min      2.3880
_cell_volume                     2569.7(3)
_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, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      229.99(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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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     68.00  94.00   0.50    2.00    --   66.15  28.00  21.00   52
  2  \w   -105.00 -68.00   0.50    2.00    --  -66.74 -28.00-140.00   74
  3  \w   -117.00 -92.00   0.50    2.00    --  -69.40 -28.00-140.00   50
  4  \w     85.00 111.00   0.50    2.00    --   69.60  28.00  21.00   52
  5  \w     81.00 126.00   0.50    2.00    --   78.02  28.00  21.00   90
  6  \w     44.00 105.00   0.50    2.00    --   66.15  15.00   0.00  122
  7  \w     28.00  56.00   0.50    2.00    --   66.15 -95.00 120.00   56
  8  \w   -104.00 -74.00   0.50    2.00    --  -66.74   0.00  60.00   60
  9  \w   -104.00 -78.00   0.50    2.00    --  -66.74   0.00-180.00   52
 10  \w   -103.00 -73.00   0.50    2.00    --  -66.74   0.00  90.00   60
 11  \w   -104.00 -73.00   0.50    2.00    --  -66.74   0.00 150.00   62
 12  \w    -66.00 -25.00   0.50    2.00    --  -66.74 125.00  30.00   82
 13  \w   -104.00 -74.00   0.50    2.00    --  -66.74   0.00 -60.00   60
 14  \w    -96.00 -71.00   0.50    2.00    --  -69.40 125.00 150.00   50
 15  \w   -104.00 -79.00   0.50    2.00    --  -69.40   0.00 -30.00   50
 16  \w    -64.00 -35.00   0.50    2.00    --  -69.40 125.00 150.00   58
 17  \w     38.00 115.00   0.50    2.00    --   69.60  15.00 120.00  154
 18  \w     32.00  87.00   0.50    2.00    --   69.60-125.00-150.00  110
 19  \w     32.00  57.00   0.50    2.00    --   69.60 -95.00 -30.00   50
 20  \w     40.00  66.00   0.50    2.00    --   69.60 -95.00  30.00   52
 21  \w     40.00  78.00   0.50    2.00    --   69.60 -95.00   0.00   76
 22  \w     45.00  71.00   0.50    2.00    --   69.60 -95.00 120.00   52
 23  \w     35.00  74.00   0.50    2.00    --   69.60 -95.00  60.00   78
 24  \w   -119.00 -67.00   0.50    2.00    --  -74.00 152.00-159.57  104
 25  \w    -65.00 -40.00   0.50    2.00    --  -74.85 144.00  56.00   50
 26  \w   -114.00 -69.00   0.50    2.00    --  -74.85 144.00  56.00   90
 27  \w    -77.00 -47.00   0.50    2.00    --  -74.85 142.00 -69.21   60
 28  \w   -113.00 -83.00   0.50    2.00    --  -74.85 142.00 -69.21   60
 29  \w   -114.00 -44.00   0.50    2.00    --  -74.85 144.00 157.28  140
 30  \w     47.00 121.00   0.50    2.00    --   78.02  15.00 -90.00  148
 31  \w     43.00 105.00   0.50    2.00    --   78.02-125.00-120.00  124
 32  \w     42.00  67.00   0.50    2.00    --   78.02-125.00 -90.00   50
 33  \w     37.00 104.00   0.50    2.00    --   78.02-125.00-150.00  134
 34  \w     39.00 105.00   0.50    2.00    --   78.02-125.00 120.00  132
 35  \w     80.00 105.00   0.50    2.00    --   78.02-125.00 -30.00   50
 36  \w     41.00  66.00   0.50    2.00    --   78.02-125.00 -30.00   50
 37  \w     46.00 105.00   0.50    2.00    --   78.02-125.00   0.00  118
 38  \w     88.00 123.00   0.50    2.00    --   78.02  15.00-180.00   70
 39  \w     56.00 105.00   0.50    2.00    --   78.02-125.00 -60.00   98
 40  \w     58.00  84.00   0.50    2.00    --   78.02  15.00-180.00   52
 41  \w     59.00 118.00   0.50    2.00    --   78.02  15.00 -30.00  118
 42  \w     80.00 105.00   0.50    2.00    --   78.02-125.00 150.00   50
 43  \w     80.00 105.00   0.50    2.00    --   78.02-125.00  60.00   50
 44  \w     40.00  66.00   0.50    2.00    --   78.02 -95.00  60.00   52
 45  \w     44.00  71.00   0.50    2.00    --   78.02-125.00  60.00   54
 46  \w     88.00 113.00   0.50    2.00    --   78.02  15.00 120.00   50
 47  \w     49.00  76.00   0.50    2.00    --   78.02-125.00-180.00   54
;
_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      -0.0331178000
_diffrn_orient_matrix_UB_12      0.0866310000
_diffrn_orient_matrix_UB_13      0.0086335000
_diffrn_orient_matrix_UB_21      0.1701534000
_diffrn_orient_matrix_UB_22      0.0204049000
_diffrn_orient_matrix_UB_23      -0.0299032000
_diffrn_orient_matrix_UB_31      -0.0705708000
_diffrn_orient_matrix_UB_32      0.0404882000
_diffrn_orient_matrix_UB_33      -0.0783715000
_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  0.0979
_diffrn_reflns_av_unetI/netI     0.1046
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34529
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         2.418
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.334
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.140
_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
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.891
_exptl_crystal_description       needle
_exptl_crystal_F_000             1401
_exptl_crystal_size_max          0.406
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.008
_refine_diff_density_max         1.914
_refine_diff_density_min         -2.617
_refine_diff_density_rms         0.311
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         9020
_refine_ls_number_restraints     649
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.1083
_refine_ls_R_factor_gt           0.0609
_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^)+(0.1169P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1546
_refine_ls_wR_factor_ref         0.1994
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5489
_reflns_number_total             9020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06280e2.cif
_cod_data_source_block           ne0245
_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_formula_sum        'C49.25 H59.50 Au3 Cl2.50 N6 O3'
_cod_database_code               1570860
_shelx_shelxl_version_number     2019/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C49.25 H59.50 Au3 Cl2.50 N6 O3'
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.054
_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
 C39-C34 = C29-C26
 1.5 with sigma of 0.02
 O2A-C29 = O2B-C29
 1.2 with sigma of 0.02
 C38A-C36 = C38B-C36 = C37A-C36 = C37B-C36
 1.54 with sigma of 0.02
 O3A-C45 \\sim O3B-C45
 with sigma of 0.01
 O1A-C13 \\sim O1B-C13
 with sigma of 0.01
 C38A-C37A \\sim C38B-C37B
 with sigma of 0.02
3. Restrained planarity
 O2A, C23, C24, C25, C26, C27, C28, C29
 with sigma of 0.1
 O1A, O1B, C7, C8, C9, C10, C11, C12, C13
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O1A \\sim O1B \\sim O2A \\sim O2B \\sim O3A \\sim O3B \\sim C13 \\sim C29 \\sim
C45: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within
2A
C36 \\sim C37A \\sim C37B \\sim C38A \\sim C38B: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01 within 2A
C46 \\sim C47 \\sim C48: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01 within 2A
5. 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
6. Others
 Sof(O3B)=Sof(H45A)=1-FVAR(1)
 Sof(O3A)=Sof(H45)=FVAR(1)
 Sof(O1B)=Sof(H13A)=1-FVAR(2)
 Sof(O1A)=Sof(H13)=FVAR(2)
 Sof(O2B)=Sof(H29A)=1-FVAR(3)
 Sof(O2A)=Sof(H29)=FVAR(3)
 Sof(H36A)=Sof(C37B)=Sof(H37D)=Sof(H37E)=Sof(H37F)=Sof(C38B)=Sof(H38D)=
 Sof(H38E)=Sof(H38F)=1-FVAR(4)
 Sof(H36)=Sof(C37A)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38A)=Sof(H38A)=
 Sof(H38B)=Sof(H38C)=FVAR(4)
7.a Ternary CH refined with riding coordinates:
 C4(H4), C14(H14), C20(H20), C30(H30), C36(H36), C36(H36A), C46(H46)
7.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C11(H11), C9(H9), C8(H8), C13(H13), C13(H13A), C28(H28), C27(H27),
 C25(H25), C24(H24), C29(H29), C29(H29A), C44(H44), C43(H43), C41(H41),
 C40(H40), C45(H45), C45(H45A)
7.c Fitted hexagon refined as free rotating group:
 C7(C12,C11,C10,C9,C8), C23(C28,C27,C26,C25,C24), C39(C44,C43,C42,C41,C40)
7.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C37A(H37A,H37B,H37C), C37B(H37D,H37E,H37F), C38A(H38A,H38B,H38C),
 C38B(H38D,H38E,H38F), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              98291
_shelx_fab_checksum              8536
_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 4.123
_oxdiff_exptl_absorpt_empirical_full_min 0.438