Group 11 complexes of a bulky triazene ligand.
George, Tanner; Grant, Tamika; Munhoz, Isadora Schumann; Do, Thai; Masuda, Jason D.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 13107–13118; doi:10.1039/d4dt01561d

data_7716679
_publ_section_title
;
 Group 11 complexes of a bulky triazene ligand.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13107
_journal_page_last               13118
_journal_paper_doi               10.1039/d4dt01561d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C51 H63 Au Cl N5, C6 D6'
_chemical_formula_sum            'C57 H63 Au Cl D6 N5'
_chemical_formula_weight         1062.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-13
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-03-17 deposited with the CCDC.	2024-07-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.2860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6309(2)
_cell_length_b                   19.3993(5)
_cell_length_c                   25.4245(7)
_cell_measurement_reflns_used    9708
_cell_measurement_temperature    100
_cell_measurement_theta_max      35.99
_cell_measurement_theta_min      2.24
_cell_volume                     5174.6(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker AXS Inc., 2018)'
_computing_data_collection       'APEX4 (Bruker AXS Inc., 2021)'
_computing_data_reduction        'SAINT V8.40A (Bruker AXS Inc., 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 '100 \\times 140 mm^2^ CMOS sensor'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '\k--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            163551
_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         28.500
_diffrn_reflns_theta_min         1.933
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\mS 3.0'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.935
_exptl_absorpt_correction_T_max  0.0300
_exptl_absorpt_correction_T_min  0.0057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0871 before and 0.0577 after correction.
The Ratio of minimum to maximum transmission is 0.1900.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       prism
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.740
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         13114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0352P)^2^+11.5571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0888
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11721
_reflns_number_total             13114
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01561d2.cif
_cod_data_source_block           spherical
_cod_depositor_comments
'Adding full bibliography for 7716674--7716682.cif.'
_cod_database_code               7716679
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.821
_shelx_estimated_absorpt_t_min   0.564
_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. Others
 Fixed Sof: C56(0.5) D56(0.5) C57(0.5) D57(0.5) C52(0.5) D52(0.5) C53(0.5)
 D53(0.5) C54(0.5) D54(0.5) C55(0.5) D55(0.5)
3.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C25(H25), C22(H22)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
3.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C20(H20), C6(H6), C19(H19), C7(H7), C47(H47), C30(H30), C8(H8),
 C31(H31), C45(H45), C32(H32), C36(H36), C38(H38), C58(D58), C59(D59), C60(D60),
  C56(D56), C57(D57), C52(D52), C53(D53), C54(D54), C55(D55)
3.d Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C27(H27A,H27B,H27C), C42(H42A,H42B,H42C), C41(H41A,H41B,
 H41C), C40(H40A,H40B,H40C), C23(H23A,H23B,H23C), C51(H51A,H51B,H51C), C15(H15A,
 H15B,H15C), C26(H26A,H26B,H26C), C50(H50A,H50B,H50C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C24(H24A,H24B,H24C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              28698
_shelx_hkl_checksum              4729
_olex2_submission_special_instructions 'No special instructions were received'