Nonanuclear zinc-gold [Zn<sub>3</sub>Au<sub>6</sub>] heterobimetallic complexes.
Yadav, Ravi; Dahlen, Milena; Singh, Akhil K.; Sun, Xiaofei; Gamer, Michael T.; Roesky, Peter W.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 8558–8566; doi:10.1039/d1dt01396c

data_7707540
_publ_section_title
;
 Nonanuclear zinc-gold [Zn<sub>3</sub>Au<sub>6</sub>] heterobimetallic
 complexes.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8558
_journal_page_last               8566
_journal_paper_doi               10.1039/d1dt01396c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C134 H100 Au6 Cl6 N4 O12 P6 Zn3, 1[C2H5OH], 2[C3H6O]'
_chemical_formula_sum            'C134 H100 Au6 Cl6 N4 O12 P6 Zn3'
_chemical_formula_weight         3734.60
_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
_audit_creation_date             2020-12-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2020-12-21 deposited with the CCDC.	2021-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                67.913(3)
_cell_angle_beta                 84.830(3)
_cell_angle_gamma                83.908(3)
_cell_formula_units_Z            1
_cell_length_a                   11.1558(5)
_cell_length_b                   17.0682(7)
_cell_length_c                   19.4466(8)
_cell_measurement_reflns_used    46158
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.54
_cell_measurement_theta_min      2.26
_cell_volume                     3406.6(3)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
PLATON (A.L.Spek, 2009)
;
_computing_data_collection       'X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)'
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
PLATON (A.L.Spek, 2009)
;
_computing_molecular_graphics    'Diamond 4, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
MS Word (Microsoft)
Olex2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.844
_diffrn_measurement_details
;
 768 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.844
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31566
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.642
_diffrn_reflns_theta_min         2.264
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    7.197
_exptl_absorpt_correction_T_max  0.6127
_exptl_absorpt_correction_T_min  0.3907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.203
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.057
_refine_diff_density_max         8.431
_refine_diff_density_min         -3.259
_refine_diff_density_rms         0.240
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         16242
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0591
_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^)+(0.0797P)^2^+46.8873P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1581
_refine_ls_wR_factor_ref         0.1651
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13536
_reflns_number_total             16242
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01396c2.cif
_cod_data_source_block           ry300g
_cod_depositor_comments
'Adding full bibliography for 7707538--7707541.cif.'
_cod_database_code               7707540
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.684
_shelx_estimated_absorpt_t_min   0.323
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C32B \\sim C17 \\sim C32 \\sim C35B \\sim C36B \\sim C37B: within 2A with sigma
of 0.005 and sigma for terminal atoms of 0.01 within 2A
C32A \\sim C33 \\sim C34B \\sim C35A \\sim C36A \\sim C37A: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C38B \\sim C39B \\sim C40A \\sim C41A \\sim C42B \\sim C43B: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C38A \\sim C39A \\sim C40B \\sim C41B \\sim C42A \\sim C43A: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C17B \\sim C32B \\sim C38B \\sim P2B \\sim Au2B \\sim Cl2B: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C32A \\sim C38A \\sim P2A \\sim Au2A \\sim Cl2A: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01 within 2A
Uanis(C50) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Au2B) \\sim Ueq, Uanis(Cl2B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Fixed Sof: Au2B(0.33333) Cl2B(0.33333) P2B(0.33333) C32B(0.33333)
 C17(0.33333) H17(0.33333) C32(0.33333) H32(0.33333) C35B(0.33333)
 H35B(0.33333) C36B(0.33333) H36B(0.33333) C37B(0.33333) H37B(0.33333)
 C38B(0.33333) C39B(0.33333) H39B(0.33333) C40A(0.33333) H40A(0.33333)
 C41A(0.33333) H41A(0.33333) C42B(0.33333) H42B(0.33333) C43B(0.33333)
 H43B(0.33333) Au2A(0.66667) Cl2A(0.66667) P2A(0.66667) C32A(0.66667)
 C33(0.66667) H33(0.66667) C34B(0.66667) H34B(0.66667) C35A(0.66667)
 H35A(0.66667) C36A(0.66667) H36A(0.66667) C37A(0.66667) H37A(0.66667)
 C38A(0.66667) C39A(0.66667) H39A(0.66667) C40B(0.66667) H40B(0.66667)
 C41B(0.66667) H41B(0.66667) C42A(0.66667) H42A(0.66667) C43A(0.66667)
 H43A(0.66667)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13),
 C19(H19), C18(H18), C16(H16), C15(H15), C21(H21), C22(H22), C24(H24), C25(H25),
  C27(H27), C28(H28), C30(H30), C31(H31), C17(H17), C32(H32), C35B(H35B),
 C36B(H36B), C37B(H37B), C39B(H39B), C40A(H40A), C41A(H41A), C42B(H42B),
 C43B(H43B), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C51(H51),
 C52(H52), C53(H53), C54(H54), C55(H55), C57(H57), C58(H58), C59(H59), C60(H60),
  C61(H61), C65(H65), C66(H66), C67(H67), C63(H63), C64(H64), C33(H33),
 C34B(H34B), C35A(H35A), C36A(H36A), C37A(H37A), C39A(H39A), C40B(H40B),
 C41B(H41B), C42A(H42A), C43A(H43A)
4.b Fitted hexagon refined as free rotating group:
 C14(C19,C18,C17B,C16,C15), C32B(C17,C32,C35B,C36B,C37B), C38B(C39B,C40A,C41A,
 C42B,C43B), C50(C51,C52,C53,C54,C55), C65(C66,C67,C62,C63,C64), C32A(C33,C34B,
 C35A,C36A,C37A), C38A(C39A,C40B,C41B,C42A,C43A)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 87 electrons were 
found in a volume of 435 A^3 in 2 voids per unit cell. 
This is consistent with the presence of one molecule
ethanol and two molecules of acetone per unit cell 
which account for 90 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              41584
_shelx_hkl_checksum              99991
_shelx_fab_checksum              42594
_olex2_submission_special_instructions 'No special instructions were received'