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_7057609
_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         'C36 H38 Au N6, C30 H44 B2 K N12'
_chemical_formula_sum            'C66 H82 Au B2 K N18'
_chemical_formula_weight         1385.18
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-15
_audit_creation_method
;
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                76.639(2)
_cell_angle_beta                 73.137(2)
_cell_angle_gamma                89.372(2)
_cell_formula_units_Z            2
_cell_length_a                   14.1732(3)
_cell_length_b                   15.6010(3)
_cell_length_c                   19.7007(5)
_cell_measurement_reflns_used    31701
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      77.4810
_cell_measurement_theta_min      3.1990
_cell_volume                     4048.63(17)
_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
;
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)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_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 0.992
_diffrn_measurement_details
;
  1 omega  -50.00   32.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.2324   38.0000   30.0000 82

  2 omega  -50.00   32.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.2324   38.0000  -90.0000 82

  3 omega -115.00  -14.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.2324  -57.0000   60.0000 101

  4 omega  -50.00   32.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.2324   38.0000 -180.0000 82

  5 omega -129.00  -32.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.2324  178.0000 -150.0000 97

  6 omega   53.00  129.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       42.2324 -178.0000  -30.0000 76

  7 omega   57.00  131.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       42.2324  178.0000 -180.0000 74

  8 omega   94.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  125.0000   90.0000 84

  9 omega   31.00  109.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -94.0000  -60.0000 78

 10 omega   61.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   15.0000  -30.0000 117

 11 omega   94.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  125.0000  150.0000 84

 12 omega   94.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  125.0000    0.0000 84

 13 omega   38.00   91.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -30.0000  -90.0000 53

 14 omega   38.00   91.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -30.0000  150.0000 53

 15 omega   41.00   98.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -45.0000  -90.0000 57

 16 omega   41.00  121.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000 -125.0000  -60.0000 80

 17 omega   61.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   15.0000  -90.0000 117

 18 omega   41.00  121.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000 -125.0000   30.0000 80

 19 omega   94.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  125.0000  -60.0000 84

 20 omega   38.00   91.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -30.0000   60.0000 53

 21 omega   31.00  109.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -94.0000 -150.0000 78

 22 omega   38.00  147.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -77.0000   30.0000 109

 23 omega   31.00  109.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -94.0000   30.0000 78

 24 omega   41.00  121.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000 -125.0000   90.0000 80

 25 omega   41.00  121.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000 -125.0000  120.0000 80

 26 omega   41.00   98.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -45.0000   30.0000 57

 27 omega   31.00  109.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -94.0000 -180.0000 78

 28 omega   41.00  121.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000 -125.0000 -180.0000 80

 29 omega   88.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   45.0000 -150.0000 90

 30 omega -115.00  -14.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.2324  -57.0000  -30.0000 101

 31 omega -118.00  -10.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.2324  -77.0000  -90.0000 108

 32 omega -118.00  -10.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.2324  -77.0000  150.0000 108

 33 omega -118.00  -10.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.2324  -77.0000   30.0000 108

 34 omega -115.00  -14.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.2324  -57.0000  150.0000 101

 35 omega -117.00  -18.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.2324  -38.0000 -150.0000 99

 36 omega    3.00   30.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       42.2324   95.0000   32.8643 27

 37 omega   85.00  150.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   61.0000  -30.0000 65

 38 omega   81.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   77.0000   90.0000 97

 39 omega   86.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   30.0000   30.0000 92

 40 omega   88.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   45.0000  150.0000 90

 41 omega   86.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   30.0000   90.0000 92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0751950000
_diffrn_orient_matrix_UB_12      -0.0713748000
_diffrn_orient_matrix_UB_13      -0.0108591000
_diffrn_orient_matrix_UB_21      0.0483522000
_diffrn_orient_matrix_UB_22      0.0519317000
_diffrn_orient_matrix_UB_23      -0.0793123000
_diffrn_orient_matrix_UB_31      0.0703923000
_diffrn_orient_matrix_UB_32      0.0504722000
_diffrn_orient_matrix_UB_33      0.0258824000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            84684
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.639
_diffrn_reflns_theta_min         2.917
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.223
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35249
_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    1.136
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
TITL dme-32_a.res in P-1
CELL   14.1732   15.6010   19.7007     76.64     73.14     89.37
SPGR P-1
C101 0.814 0.618 0.418 !       2.33 eA-3
C102 0.784 0.494 0.440 !       2.19 eA-3
C103 0.909 0.582 0.423 !       2.17 eA-3
Q104 0.923 0.715 0.216 !       2.14 eA-3
Q105 0.374 0.138 0.318 !       2.04 eA-3
C106 0.844 0.466 0.445 !       2.04 eA-3
C107 0.560 0.627 0.112 !       1.99 eA-3
Q108 0.886 0.659 0.201 !       1.97 eA-3
C109 0.906 0.508 0.438 !       1.96 eA-3
C110 0.375 0.803 0.106 !       1.85 eA-3
C111 0.513 0.714 0.111 !       1.83 eA-3
C112 0.451 0.712 0.140 !       1.62 eA-3
C113 0.409 0.721 0.115 !       1.61 eA-3
Q114 0.921 0.641 0.237 !       1.38 eA-3
Q115 0.114 0.107 0.221 !       1.31 eA-3
Q116 0.711 0.264 0.218 !       1.25 eA-3
Q117 0.940 0.679 0.176 !       1.20 eA-3
C118 0.668 0.642 0.081 !       1.08 eA-3
Q119 0.503 0.841 0.217 !       0.71 eA-3
Q120 0.251 0.921 0.362 !       0.65 eA-3
Q121 0.890 0.500 0.180 !       0.62 eA-3
Q122 0.120 0.096 0.330 !       0.60 eA-3
Q123 0.171 0.247 0.314 !       0.60 eA-3
Q124 0.520 0.035 0.280 !       0.59 eA-3
Q125 0.201 0.169 0.198 !       0.59 eA-3
Q126 0.972 0.878 0.174 !       0.58 eA-3
Q127 0.503 0.924 0.370 !       0.57 eA-3
C128 0.874 0.743 0.415 !       0.57 eA-3
Q129 0.471 0.934 0.333 !       0.56 eA-3
Q130 0.418 0.095 0.108 !       0.56 eA-3
Q131 0.455 0.343 0.360 !       0.56 eA-3
Q132 0.263 0.295 0.264 !       0.55 eA-3
Q133 0.453 0.195 0.127 !       0.55 eA-3
Q134 0.280 0.143 0.194 !       0.54 eA-3
Q135 0.178 0.064 0.380 !       0.53 eA-3
Q136 0.815 0.550 0.228 !       0.53 eA-3
Q137 0.630 0.193 0.224 !       0.52 eA-3
Q138 0.459 0.191 0.369 !       0.52 eA-3
Q139 0.737 0.472 0.203 !       0.51 eA-3
Q140 0.154 0.728 0.347 !       0.51 eA-3
Q141 0.796 0.904 0.191 !       0.50 eA-3
;
_refine_diff_density_max         1.278
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     813
_refine_ls_number_reflns         17089
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+2.3210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15198
_reflns_number_total             17089
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj03318h2.cif
_cod_data_source_block           dme-32
_cod_depositor_comments
'Adding full bibliography for 7057608--7057610.cif.'
_cod_original_cell_volume        4048.64(16)
_cod_database_code               7057609
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C12 H26 N5 Au K'
_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 B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B2(H2), B1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C51(H51), C56(H56), C61(H61), C29(H29), C21(H21), C41(H41), C35(H35),
 C66(H66), C46(H46), C10(H10), C17(H17), C39(H39), C8(H8), C27(H27), C20(H20),
 C38(H38), C37(H37), C18(H18), C36(H36), C19(H19)
2.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C15(H15A,H15B,H15C), C63(H63A,H63B,H63C), C54(H54A,H54B,
 H54C), C49(H49A,H49B,H49C), C32(H32A,H32B,H32C), C58(H58A,H58B,H58C), C53(H53A,
 H53B,H53C), C31(H31A,H31B,H31C), C14(H14A,H14B,H14C), C48(H48A,H48B,H48C),
 C12(H12A,H12B,H12C), C59(H59A,H59B,H59C), C69(H69A,H69B,H69C), C64(H64A,H64B,
 H64C), C43(H43A,H43B,H43C), C68(H68A,H68B,H68C), C44(H44A,H44B,H44C), C13(H13A,
 H13B,H13C), C33(H33A,H33B,H33C)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'