Synthesis and characterization of a gold(i) bis(triazolylidene) complex featuring a large [(TpMe2)2K] anion
Priante-Flores, Armando; Salazar-Pereda, Verónica; Rheingold, Arnold L.; Mendoza-Espinosa, Daniel; New Journal of Chemistry 42 (2018) 15533–; doi:10.1039/C8NJ03318H

data_7057608
_publ_section_title
;
 Synthesis and characterization of a gold(i) bis(triazolylidene) complex
 featuring a large [(TpMe2)2K] anion
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15533
_journal_paper_doi               10.1039/C8NJ03318H
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C18 H19 Au I N3'
_chemical_formula_sum            'C18 H19 Au I N3'
_chemical_formula_weight         601.23
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-12-04
_audit_creation_method
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Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-07-25 deposited with the CCDC.
2018-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.0600(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.62530(10)
_cell_length_b                   11.0961(2)
_cell_length_c                   17.7617(2)
_cell_measurement_reflns_used    10057
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      77.2970
_cell_measurement_theta_min      3.9330
_cell_volume                     1892.25(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3659
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega -117.00  -18.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
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  2 omega  -50.00   32.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.4824   38.0000    0.0000 82

  3 omega  -50.00   32.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.4824   38.0000   30.0000 82

  4 omega   18.00   99.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       42.4824 -125.0000  -30.0000 81

  5 omega   41.00   98.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
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  6 omega   38.00   91.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
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  7 omega   38.00   91.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -30.0000 -150.0000 53

  8 omega   31.00  109.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -94.0000   60.0000 78

  9 omega   31.00  109.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -94.0000  120.0000 78

 10 omega   31.00  109.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -94.0000   30.0000 78

 11 omega   41.00  121.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000 -125.0000  150.0000 80

 12 omega   32.00  167.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -15.0000   90.0000 135

 13 omega   88.00  178.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   45.0000  -90.0000 90

 14 omega   41.00   98.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -45.0000  150.0000 57

 15 omega   38.00   91.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -30.0000  -90.0000 53

 16 omega -115.00  -14.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.4824  -57.0000   90.0000 101

 17 omega -119.00  -10.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.4824  -77.0000    0.0000 109

 18 omega   -4.00   83.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       42.4824  -99.0000  120.0000 87

 19 omega   86.00  178.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   30.0000  120.0000 92

 20 omega   31.00  109.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -94.0000 -180.0000 78

 21 omega   61.00  178.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   15.0000   30.0000 117

 22 omega   31.00  109.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -94.0000  -90.0000 78

 23 omega   81.00  178.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   77.0000   30.0000 97

 24 omega   88.00  178.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   45.0000  -60.0000 90

 25 omega   85.00  178.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   61.0000    0.0000 93

 26 omega   85.00  178.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   61.0000 -150.0000 93

 27 omega   61.00  178.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   15.0000 -150.0000 117

 28 omega -119.00  -10.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.4824  -77.0000  -90.0000 109

 29 omega -115.00  -65.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.4824 -138.0000   89.0000 50

 30 omega -119.00  -10.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -      -42.4824  -77.0000 -150.0000 109

 31 omega   85.00  167.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   61.0000  120.0000 82

 32 omega   85.00  178.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   61.0000 -180.0000 93

 33 omega   31.00  109.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -94.0000  -30.0000 78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1414567000
_diffrn_orient_matrix_UB_12      0.0242534000
_diffrn_orient_matrix_UB_13      0.0434364000
_diffrn_orient_matrix_UB_31      -0.0299879000
_diffrn_orient_matrix_UB_32      0.1363960000
_diffrn_orient_matrix_UB_33      -0.0024703000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31955
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.483
_diffrn_reflns_theta_min         4.605
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    27.428
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.110
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.288
_refine_diff_density_min         -1.123
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         4003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+1.3420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0871
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3424
_reflns_number_total             4003
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj03318h2.cif
_cod_data_source_block           dme-25
_cod_depositor_comments
'Adding full bibliography for 7057608--7057610.cif.'
_cod_database_code               7057608
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C12 H26 N6 Au I'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C11(H11), C17(H17), C19(H19), C20(H20), C18(H18), C9(H9)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_olex2_date_sample_data_collection 2017-12-01
_olex2_submission_special_instructions 'No special instructions were received'