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_1570859
_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'
_chemical_formula_sum            'C48 H57 Au3 N6 O3'
_chemical_formula_weight         1356.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-07-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-07-25 deposited with the CCDC.	2024-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.696(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0056(4)
_cell_length_b                   29.2892(6)
_cell_length_c                   8.03827(16)
_cell_measurement_reflns_used    18163
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      34.2750
_cell_measurement_theta_min      2.0370
_cell_volume                     4686.75(16)
_computing_cell_refinement       'CrysAlisPro 1.171.42.75a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.75a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.75a (Rigaku OD, 2022)'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     10.00  44.00   0.50   10.00    --   -0.82  47.00 174.90   68
  2  \w      8.00  39.00   0.50   10.00    --   -0.82  65.00 -83.06   62
  3  \w     -3.00  25.00   0.50   10.00    --   -0.82  95.00  18.80   56
  4  \w      9.00  34.00   0.50   10.00    --   -0.82  58.00   0.18   50
  5  \w    -13.00  12.00   0.50   10.00    --   -0.82 102.00-153.41   50
  6  \w    -12.00  34.00   0.50   10.00    --  -14.00  28.00 168.21   92
  7  \w     -8.00  25.00   0.50   10.00    --  -18.00  30.00  38.77   66
  8  \w    -49.00 -24.00   0.50   10.00    --  -18.00 135.00  33.12   50
;
_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      0.0318511000
_diffrn_orient_matrix_UB_12      0.0012465000
_diffrn_orient_matrix_UB_13      0.0470848000
_diffrn_orient_matrix_UB_21      -0.0024116000
_diffrn_orient_matrix_UB_22      0.0241692000
_diffrn_orient_matrix_UB_23      0.0012453000
_diffrn_orient_matrix_UB_31      -0.0157753000
_diffrn_orient_matrix_UB_32      -0.0011874000
_diffrn_orient_matrix_UB_33      0.0750888000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            54089
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.046
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.414
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_correction_T_min  0.361
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.75a (Rigaku Oxford Diffraction, 2022)
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    1.923
_exptl_crystal_description       needle
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.569
_refine_diff_density_min         -1.494
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         14329
_refine_ls_number_restraints     564
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0197P)^2^+6.2292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0519
_refine_ls_wR_factor_ref         0.0575
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10387
_reflns_number_total             14329
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06280e2.cif
_cod_data_source_block           ne_02_15_mo
_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        4686.76(17)
_cod_database_code               1570859
_shelx_shelxl_version_number     2019/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C48 H57 Au3 N6 O3'
_shelx_estimated_absorpt_t_max   0.705
_shelx_estimated_absorpt_t_min   0.113
_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
 O2A-C29 = C29-O2B
 1.2 with sigma of 0.01
 C7B-C2 \\sim C2-C7A
 with sigma of 0.02
 O3A-C45 \\sim O3B-C45
 with sigma of 0.02
 O1A-C13A \\sim O1B-C13B
 with sigma of 0.02
 C13A-C11A \\sim C11B-C13B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7A \\sim C8A \\sim C9A
\\sim C10A \\sim C11A \\sim C12A \\sim C7B \\sim C12B \\sim C11B \\sim C10B
\\sim C9B \\sim C8B \\sim C13A \\sim C13B \\sim C14 \\sim C15A \\sim C15B \\sim
C16A \\sim C16B \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22
\\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30
\\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38
\\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46
\\sim C47 \\sim C48 \\sim O1A \\sim O1B \\sim O2A \\sim O2B \\sim O3A \\sim
O3B: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within
2A
4. Others
 Sof(O1B)=Sof(C7B)=Sof(C12B)=Sof(H12B)=Sof(C11B)=Sof(C10B)=Sof(H10B)=Sof(C9B)=
 Sof(H9B)=Sof(C8B)=Sof(H8B)=Sof(C13B)=Sof(H13B)=1-FVAR(1)
 Sof(O1A)=Sof(C7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=
 Sof(C11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13A)=FVAR(1)
 Sof(O2B)=Sof(H29A)=1-FVAR(2)
 Sof(O2A)=Sof(H29)=FVAR(2)
 Sof(O3B)=Sof(H45A)=1-FVAR(3)
 Sof(O3A)=Sof(H45)=FVAR(3)
 Sof(H14A)=Sof(C15B)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16B)=Sof(H16D)=
 Sof(H16E)=Sof(H16F)=1-FVAR(4)
 Sof(H14)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16A)=Sof(H16A)=
 Sof(H16B)=Sof(H16C)=FVAR(4)
5.a Ternary CH refined with riding coordinates:
 C4(H4), C14(H14), C14(H14A), C20(H20), C30(H30), C36(H36), C46(H46)
5.b Aromatic/amide H refined with riding coordinates:
 C8A(H8A), C9A(H9A), C10A(H10A), C12A(H12A), C12B(H12B), C10B(H10B), C9B(H9B),
 C8B(H8B), C13A(H13A), C13B(H13B), C24(H24), C25(H25), C26(H26), C28(H28),
 C29(H29), C29(H29A), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45),
 C45(H45A)
5.c Fitted hexagon refined as free rotating group:
 C7A(C8A,C9A,C10A,C11A,C12A), C7B(C12B,C11B,C10B,C9B,C8B)
5.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C15A(H15A,H15B,H15C), C15B(H15D,H15E,H15F),
 C16A(H16A,H16B,H16C), C16B(H16D,H16E,H16F), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              84596
_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 1.190
_oxdiff_exptl_absorpt_empirical_full_min 0.776