Luminescent early-late-hetero-tetranuclear group IV – Au(i) bisamidinate complexes
Uhlmann, Cedric; Feuerstein, Thomas J.; Seifert, Tim P.; Jung, André P.; Gamer, Michael T.; Köppe, Ralf; Lebedkin, Sergei; Kappes, Manfred M.; Roesky, Peter W.; Dalton Transactions  (2022) –; doi:10.1039/D2DT00458E

data_7710650
_publ_section_title
;
 Luminescent early-late-hetero-tetranuclear group IV -- Au(i) bisamidinate
 complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00458E
_journal_year                    2022
_chemical_formula_moiety         'C74 H88 Au2 Cl2 N4 Zr2, C7 H8, 0.5(C5 H12)'
_chemical_formula_sum            'C83.5 H102 Au2 Cl2 N4 Zr2'
_chemical_formula_weight         1808.96
_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             2021-11-11
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2022-02-14 deposited with the CCDC.	2022-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                85.570(3)
_cell_angle_beta                 73.580(3)
_cell_angle_gamma                78.177(3)
_cell_formula_units_Z            1
_cell_length_a                   10.2511(4)
_cell_length_b                   14.1743(6)
_cell_length_c                   14.8080(5)
_cell_measurement_reflns_used    13911
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.52
_cell_measurement_theta_min      2.03
_cell_volume                     2019.67(14)
_computing_cell_refinement
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 1.78.0.0 (STOE, 2020)
X-Area LANA 1.78.0.0 (STOE, 2020)
;
_computing_molecular_graphics    'Olex2 1.5-alpha (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 1.5-alpha (Dolomanov et al., 2009)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details
;
 186 frames, detector distance = 100 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_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  0.0466
_diffrn_reflns_av_unetI/netI     0.0784
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19024
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.188
_diffrn_reflns_theta_min         2.031
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.981
_exptl_absorpt_correction_T_max  0.6523
_exptl_absorpt_correction_T_min  0.4405
_exptl_absorpt_correction_type   integration
_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.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             903
_exptl_crystal_size_max          0.295
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.066
_refine_diff_density_max         1.007
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         10563
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0582P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1087
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7514
_reflns_number_total             10563
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00458e2.cif
_cod_data_source_block           tjfaj04-2
_cod_original_formula_sum        'C83.50 H102 Au2 Cl2 N4 Zr2'
_cod_database_code               7710650
_shelx_shelxl_version_number     2018/3
_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
 C38C-C39C \\sim C40C-C39C \\sim C40C-C41C \\sim C41C-C42C
 with sigma of 0.005
 C24A-C22A \\sim C24B-C22B \\sim C23A-C22A \\sim C23B-C22B \\sim C26A-C25A
\\sim C25A-C27A \\sim C25B-
 C27B \\sim C26B-C25B
 with sigma of 0.005
 C25B-C17B \\sim C25A-C17A \\sim C22B-C21B \\sim C22A-C21A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C25A \\sim C26A \\sim C27A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: H10A(0.5) H10(0.5) C11A(0.5) H11A(0.5) H11B(0.5) H11C(0.5)
 C12A(0.5) H12A(0.5) H12B(0.5) H12C(0.5) C16A(0.5) C21A(0.5) C20A(0.5)
 H20A(0.5) C19A(0.5) H19A(0.5) C18A(0.5) H18A(0.5) C17A(0.5) C22A(0.5)
 H22A(0.5) C23A(0.5) H23A(0.5) H23B(0.5) H23C(0.5) C24A(0.5) H24A(0.5)
 H24B(0.5) H24C(0.5) C25A(0.5) H25A(0.5) C26A(0.5) H26A(0.5) H26B(0.5)
 H26C(0.5) C27A(0.5) H27A(0.5) H27B(0.5) H27C(0.5) C32A(0.5) H32A(0.5)
 C28A(0.5) H28A(0.5) C29A(0.5) H29A(0.5) C30A(0.5) H30A(0.5) C31A(0.5)
 H31A(0.5) C11B(0.5) H11D(0.5) H11E(0.5) H11F(0.5) C12B(0.5) H12D(0.5)
 H12E(0.5) H12F(0.5) C16B(0.5) C21B(0.5) C20B(0.5) H20B(0.5) C19B(0.5)
 H19B(0.5) C18B(0.5) H18B(0.5) C17B(0.5) C22B(0.5) H22B(0.5) C23B(0.5)
 H23D(0.5) H23E(0.5) H23F(0.5) C24B(0.5) H24D(0.5) H24E(0.5) H24F(0.5)
 C25B(0.5) H25B(0.5) C26B(0.5) H26D(0.5) H26E(0.5) H26F(0.5) C27B(0.5)
 H27D(0.5) H27E(0.5) H27F(0.5) C37B(0.5) H37B(0.5) C33B(0.5) H33B(0.5)
 C34B(0.5) H34B(0.5) C35B(0.5) H35B(0.5) C36B(0.5) H36B(0.5) C37A(0.5)
 H37A(0.5) C33A(0.5) H33A(0.5) C34A(0.5) H34A(0.5) C35A(0.5) H35A(0.5)
 C36A(0.5) H36A(0.5) C38A(0.3) H38D(0.3) H38E(0.3) H38F(0.3) C39A(0.3)
 C44A(0.3) H44A(0.3) C43A(0.3) H43A(0.3) C42A(0.3) H42D(0.3) C41A(0.3)
 H41C(0.3) C40A(0.3) H40C(0.3) C32B(0.5) H32B(0.5) C28B(0.5) H28B(0.5)
 C29B(0.5) H29B(0.5) C30B(0.5) H30B(0.5) C31B(0.5) H31B(0.5) C38B(0.2)
 H38G(0.2) H38H(0.2) H38I(0.2) C40B(0.2) H40D(0.2) C39B(0.2) C44B(0.2)
 H44B(0.2) C43B(0.2) H43B(0.2) C42B(0.2) H42E(0.2) C41B(0.2) H41D(0.2)
 C38C(0.25) H38A(0.25) H38B(0.25) H38C(0.25) C39C(0.25) H39A(0.25) H39B(0.25)
 C40C(0.25) H40A(0.25) H40B(0.25) C41C(0.25) H41A(0.25) H41B(0.25) C42C(0.25)
 H42A(0.25) H42B(0.25) H42C(0.25)
5.a Ternary CH refined with riding coordinates:
 C10(H10A), C10(H10), C13(H13), C22A(H22A), C25A(H25A), C22B(H22B), C25B(H25B)
5.b Secondary CH2 refined with riding coordinates:
 C39C(H39A,H39B), C40C(H40A,H40B), C41C(H41A,H41B)
5.c Me refined with riding coordinates:
 C23A(H23A,H23B,H23C), C24A(H24A,H24B,H24C), C23B(H23D,H23E,H23F), C24B(H24D,
 H24E,H24F)
5.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C20A(H20A), C19A(H19A), C18A(H18A), C32A(H32A),
 C28A(H28A), C29A(H29A), C30A(H30A), C31A(H31A), C20B(H20B), C19B(H19B),
 C18B(H18B), C37B(H37B), C33B(H33B), C34B(H34B), C35B(H35B), C36B(H36B),
 C37A(H37A), C33A(H33A), C34A(H34A), C35A(H35A), C36A(H36A), C44A(H44A),
 C43A(H43A), C42A(H42D), C41A(H41C), C40A(H40C), C32B(H32B), C28B(H28B),
 C29B(H29B), C30B(H30B), C31B(H31B), C40B(H40D), C44B(H44B), C43B(H43B),
 C42B(H42E), C41B(H41D)
5.e Fitted pentagon refined as free rotating group:
 C32A(C28A,C29A,C30A,C31A), C37B(C33B,C34B,C35B,C36B), C37A(C33A,C34A,C35A,
 C36A), C32B(C28B,C29B,C30B,C31B)
5.f Fitted hexagon refined as free rotating group:
 C16A(C21A,C20A,C19A,C18A,C17A), C16B(C21B,C20B,C19B,C18B,C17B), C39A(C44A,
 C43A,C42A,C41A,C40A), C40B(C39B,C44B,C43B,C42B,C41B)
5.g Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C11A(H11A,H11B,H11C), C12A(H12A,
 H12B,H12C), C26A(H26A,H26B,H26C), C27A(H27A,H27B,H27C), C11B(H11D,H11E,H11F),
 C12B(H12D,H12E,H12F), C26B(H26D,H26E,H26F), C27B(H27D,H27E,H27F), C38A(H38D,
 H38E,H38F), C38B(H38G,H38H,H38I), C38C(H38A,H38B,H38C), C42C(H42A,H42B,H42C)
;
_shelx_res_checksum              64841
_olex2_submission_special_instructions 'No special instructions were received'