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_7710649
_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 Ti2, 3(C7 H8)'
_chemical_formula_sum            'C95 H112 Au2 Cl2 N4 Ti2'
_chemical_formula_weight         1870.51
_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                81.979(3)
_cell_angle_beta                 73.636(4)
_cell_angle_gamma                73.059(3)
_cell_formula_units_Z            2
_cell_length_a                   15.9924(7)
_cell_length_b                   16.5310(7)
_cell_length_c                   18.2303(8)
_cell_measurement_reflns_used    34219
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.04
_cell_measurement_theta_min      1.62
_cell_volume                     4415.0(3)
_computing_cell_refinement
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.161.0 (STOE, 2020)
;
_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      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.845
_diffrn_measurement_details
;
 751 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  0.0438
_diffrn_reflns_av_unetI/netI     0.0873
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.845
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42976
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.659
_diffrn_reflns_theta_min         1.618
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.593
_exptl_absorpt_correction_T_max  0.5040
_exptl_absorpt_correction_T_min  0.1429
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1892
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.099
_refine_diff_density_max         2.227
_refine_diff_density_min         -1.421
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     986
_refine_ls_number_reflns         21107
_refine_ls_number_restraints     263
_refine_ls_restrained_S_all      2.380
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0556
_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^)+(0.0812P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1479
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12501
_reflns_number_total             21107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00458e2.cif
_cod_data_source_block           tjfaj02-02
_cod_original_cell_volume        4415.0(4)
_cod_database_code               7710649
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.717
_shelx_estimated_absorpt_t_min   0.442
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C83-C82
 1.53 with sigma of 0.02
 C89-C90
 1.53 with sigma of 0.005
 C26-C59
 1.53 with sigma of 0.02
 C88-C82 \\sim C82-C84
 with sigma of 0.005
 C81B-C76B \\sim C81B-C80B
 with sigma of 0.04
 C75-C76 \\sim C82-C83
 with sigma of 0.005
 C25B-C17 \\sim C17-C25A
 with sigma of 0.02
 C92-C93 \\sim C94-C93 \\sim C90-C94 \\sim C89-C90
 with sigma of 0.005
 C95-C89 \\sim C89-C91
 with sigma of 0.005
3. Rigid bond restraints
 C65B, C66B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C25B, C26B, C27B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C25A, C26A, C27A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
C25A \\sim C26A \\sim C27A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C25B \\sim C26B \\sim C27B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C17 \\sim C25B \\sim C26B \\sim C27B: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C17 \\sim C25A \\sim C26A \\sim C27A: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C75B \\sim C76B \\sim C77B \\sim C78B \\sim C79B \\sim C80B \\sim C81B: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C75A \\sim C76A \\sim C77A \\sim C78A \\sim C79A \\sim C80A \\sim C81A: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C50 \\sim C51 \\sim C52: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C47 \\sim C48 \\sim C49: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C59A \\sim C60A \\sim C61A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C59B \\sim C60B \\sim C61B: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C89 \\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C25 \\sim C26 \\sim C27 \\sim C59 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim
C65 \\sim C66: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
5. Others
 Fixed Sof: 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) 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)
 Ti2B(0.5) Cl2A(0.5) C59A(0.5) H59A(0.5) C60A(0.5) H60A(0.5) H60B(0.5)
 H60C(0.5) C61A(0.5) H61A(0.5) H61B(0.5) H61C(0.5) C67A(0.5) H67A(0.5)
 C66A(0.5) H66A(0.5) C65A(0.5) H65A(0.5) C69A(0.5) H69A(0.5) C68A(0.5)
 H68A(0.5) C71A(0.5) H71A(0.5) C70A(0.5) H70A(0.5) C74A(0.5) H74A(0.5)
 C73A(0.5) H73A(0.5) C72A(0.5) H72A(0.5) Ti2A(0.5) Cl2B(0.5) C59B(0.5)
 H59B(0.5) C60B(0.5) H60D(0.5) H60E(0.5) H60F(0.5) C61B(0.5) H61D(0.5)
 H61E(0.5) H61F(0.5) C69B(0.5) H69B(0.5) C68B(0.5) H68B(0.5) C67B(0.5)
 H67B(0.5) C66B(0.5) H66B(0.5) C65B(0.5) H65B(0.5) C71B(0.5) H71B(0.5)
 C72B(0.5) H72B(0.5) C73B(0.5) H73B(0.5) C74B(0.5) H74B(0.5) C70B(0.5)
 H70B(0.5) C26(0.75) C25(0.75) H25(0.75) C27(0.75) H27(0.75) C61(0.75)
 H61(0.75) C65(0.75) H65(0.75) C66(0.75) H66(0.75) C59(0.75) H59C(0.75)
 H59D(0.75) H59E(0.75) C75A(0.5) C80A(0.5) H80A(0.5) C79A(0.5) H79A(0.5)
 C78A(0.5) H78A(0.5) C77A(0.5) H77A(0.5) C76A(0.5) H76A(0.5) C81A(0.5)
 H81A(0.5) H81B(0.5) H81C(0.5) C75B(0.5) C76B(0.5) H76B(0.5) C77B(0.5)
 H77B(0.5) C78B(0.5) H78B(0.5) C79B(0.5) H79B(0.5) C80B(0.5) H80B(0.5)
 C81B(0.5) H81D(0.5) H81E(0.5) H81F(0.5) C82(0.45) H82A(0.45) H82B(0.45)
 H82C(0.45) C86(0.45) H86(0.45) C85(0.45) H85(0.45) C84(0.45) H84(0.45)
 C83(0.45) C88(0.45) H88(0.45) C87(0.45) H87(0.45) C89(0.3) H89A(0.3) H89B(0.3)
 H89C(0.3) C95(0.3) H95(0.3) C94(0.3) H94(0.3) C93(0.3) H93(0.3) C92(0.3)
 H92(0.3) C91(0.3) H91(0.3) C90(0.3) C75(0.5) H75A(0.5) H75B(0.5) H75C(0.5)
 C78(0.5) H78(0.5) C79(0.5) H79(0.5) C80(0.5) H80(0.5) C81(0.5) H81(0.5)
 C76(0.5) C77(0.5) H77(0.5)
6.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25A(H25A), C25B(H25B), C47(H47), C50(H50),
 C62(H62), C59A(H59A), C59B(H59B)
6.b Me refined with riding coordinates:
 C59(H59C,H59D,H59E), C82(H82A,H82B,H82C), C89(H89A,H89B,H89C), C75(H75A,H75B,
 H75C)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C28(H28), C29(H29),
 C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37),
  C43(H43), C44(H44), C45(H45), C55(H55), C56(H56), C57(H57), C67A(H67A),
 C66A(H66A), C65A(H65A), C69A(H69A), C68A(H68A), C71A(H71A), C70A(H70A),
 C74A(H74A), C73A(H73A), C72A(H72A), C69B(H69B), C68B(H68B), C67B(H67B),
 C66B(H66B), C65B(H65B), C71B(H71B), C72B(H72B), C73B(H73B), C74B(H74B),
 C70B(H70B), C25(H25), C27(H27), C61(H61), C65(H65), C66(H66), C80A(H80A),
 C79A(H79A), C78A(H78A), C77A(H77A), C76A(H76A), C76B(H76B), C77B(H77B),
 C78B(H78B), C79B(H79B), C80B(H80B), C86(H86), C85(H85), C84(H84), C88(H88),
 C87(H87), C95(H95), C94(H94), C93(H93), C92(H92), C91(H91), C78(H78), C79(H79),
  C80(H80), C81(H81), C77(H77)
6.d Fitted pentagon refined as free rotating group:
 C67A(C66A,C65A,C69A,C68A), C71A(C70A,C74A,C73A,C72A), C69B(C68B,C67B,C66B,
 C65B), C71B(C72B,C73B,C74B,C70B)
6.e Fitted hexagon refined as free rotating group:
 C26(C25,C27,C61,C65,C66), C75A(C80A,C79A,C78A,C77A,C76A), C75B(C76B,C77B,C78B,
 C79B,C80B), C86(C85,C84,C83,C88,C87), C95(C94,C93,C92,C91,C90), C78(C79,C80,
 C81,C76,C77)
6.f Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26A(H26A,H26B,H26C),
 C27A(H27A,H27B,H27C), C26B(H26D,H26E,H26F), C27B(H27D,H27E,H27F), C48(H48A,
 H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C),
 C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C60A(H60A,H60B,H60C), C61A(H61A,H61B,
 H61C), C60B(H60D,H60E,H60F), C61B(H61D,H61E,H61F), C81A(H81A,H81B,H81C),
 C81B(H81D,H81E,H81F)
;
_shelx_res_checksum              35497
_olex2_submission_special_instructions 'No special instructions were received'