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_7057610
_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, 2(C15 H22 B K0.5 N6)'
_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
_audit_creation_date             2018-03-01
_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                82.050(2)
_cell_angle_beta                 83.870(2)
_cell_angle_gamma                87.964(2)
_cell_formula_units_Z            2
_cell_length_a                   14.7835(3)
_cell_length_b                   15.7197(3)
_cell_length_c                   16.7848(4)
_cell_measurement_reflns_used    30657
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.3200
_cell_measurement_theta_min      3.4740
_cell_volume                     3840.23(14)
_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 0.998
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_details
;
  1 omega  -84.00   14.00   1.0000   22.6650
omega____ theta____ kappa____ phi______ frames
    -       -9.9610  -37.0000    0.0000 98

  2 omega  -34.00   65.00   1.0000   22.6650
omega____ theta____ kappa____ phi______ frames
    -       -9.9610   37.0000 -180.0000 99

  3 omega  -25.00   31.00   1.0000   22.6650
omega____ theta____ kappa____ phi______ frames
    -       -9.9610  -99.0000  -90.0000 56

  4 omega  -84.00   14.00   1.0000   22.6650
omega____ theta____ kappa____ phi______ frames
    -       -9.9610  -37.0000 -120.0000 98

  5 omega  -86.00   23.00   1.0000   22.6650
omega____ theta____ kappa____ phi______ frames
    -       -9.9610  -77.0000    0.0000 109

  6 omega  -86.00   23.00   1.0000   22.6650
omega____ theta____ kappa____ phi______ frames
    -       -9.9610  -77.0000  -30.0000 109

  7 omega  -25.00   52.00   1.0000   22.6650
omega____ theta____ kappa____ phi______ frames
    -       11.4454  -99.0000  -90.0000 77

  8 omega  -83.00   18.00   1.0000   22.6650
omega____ theta____ kappa____ phi______ frames
    -       -9.9610  -57.0000 -180.0000 101

  9 omega  -56.00   -4.00   1.0000   22.6650
omega____ theta____ kappa____ phi______ frames
    -       -9.9610  108.0000  131.0000 52

 10 omega  -25.00   52.00   1.0000   22.6650
omega____ theta____ kappa____ phi______ frames
    -       11.4454  -99.0000   30.0000 77

 11 omega  -25.00   52.00   1.0000   22.6650
omega____ theta____ kappa____ phi______ frames
    -       11.4454  -99.0000  150.0000 77

 12 omega  -13.00   86.00   1.0000   22.6650
omega____ theta____ kappa____ phi______ frames
    -       11.4454   37.0000 -150.0000 99

 13 omega  -25.00   52.00   1.0000   22.6650
omega____ theta____ kappa____ phi______ frames
    -       11.4454  -99.0000   60.0000 77

 14 omega  -34.00    0.00   1.0000   22.6650
omega____ theta____ kappa____ phi______ frames
    -       -9.9610   37.0000  -30.0000 34

 15 omega  -25.00   52.00   1.0000   22.6650
omega____ theta____ kappa____ phi______ frames
    -       11.4454  -99.0000  -30.0000 77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0226590000
_diffrn_orient_matrix_UB_12      0.0398492000
_diffrn_orient_matrix_UB_13      0.0045041000
_diffrn_orient_matrix_UB_21      0.0073062000
_diffrn_orient_matrix_UB_22      -0.0056181000
_diffrn_orient_matrix_UB_23      0.0415026000
_diffrn_orient_matrix_UB_31      0.0419855000
_diffrn_orient_matrix_UB_32      0.0213793000
_diffrn_orient_matrix_UB_33      -0.0098665000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            138342
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.808
_diffrn_reflns_theta_min         2.985
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.017
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70746
_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    1.198
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
TITL dme-21_a.res in P-1
CELL   14.7835   15.7197   16.7848     82.05     83.87     87.96
SPGR P-1
Q101 0.328 0.691 0.437 !       1.56 eA-3
Q102 0.331 0.683 0.467 !       1.53 eA-3
Q103 0.358 0.711 0.421 !       1.48 eA-3
C104 0.286 0.180-0.004 !       1.48 eA-3
C105 0.313 0.146 0.014 !       1.42 eA-3
Q106 0.354 0.715 0.453 !       1.42 eA-3
C107 0.704 0.889 0.059 !       1.33 eA-3
C108 0.338 0.072 0.046 !       1.33 eA-3
C109 0.685 0.921 0.015 !       1.32 eA-3
C110 0.683 0.858 0.030 !       1.28 eA-3
C111 0.644 0.910 0.038 !       1.27 eA-3
C112 0.673 0.891 0.012 !       1.24 eA-3
C113 0.719 0.911 0.028 !       1.21 eA-3
C114 0.731 0.941 0.009 !       1.20 eA-3
C115 0.717 0.836 0.067 !       1.19 eA-3
C116 0.349 0.107 0.011 !       1.18 eA-3
Q117 0.597 0.282 0.499 !       1.15 eA-3
C118 0.745 0.784 0.033 !       1.09 eA-3
C119 0.354 0.031 0.023 !       1.09 eA-3
Q120 0.329 0.638 0.403 !       1.09 eA-3
Q121 0.671 0.262 0.489 !       1.09 eA-3
C122 0.705 0.981 0.014 !       1.08 eA-3
C123 0.645 0.968 0.007 !       1.07 eA-3
C124 0.273 0.044 0.032 !       1.06 eA-3
Q125 0.300 0.624 0.458 !       0.99 eA-3
Q126 0.361 0.687 0.373 !       0.97 eA-3
C127 0.421 0.017 0.007 !       0.97 eA-3
Q128 0.298 0.686 0.386 !       0.95 eA-3
Q129 0.361 0.771 0.485 !       0.88 eA-3
C130 0.743 0.763 0.084 !       0.86 eA-3
Q131 0.374 0.770 0.384 !       0.85 eA-3
Q132 0.630 0.323 0.484 !       0.85 eA-3
Q133 0.265 0.705 0.438 !       0.84 eA-3
Q134 0.689 0.359 0.506 !       0.82 eA-3
Q135 0.378 0.740 0.376 !       0.82 eA-3
Q136 0.500 0.500 0.000 !       0.82 eA-3
Q137 0.422 0.684 0.405 !       0.80 eA-3
Q138 0.329 0.738 0.374 !       0.78 eA-3
Q139 0.711 0.320 0.486 !       0.77 eA-3
C140 0.716 0.818 0.120 !       0.76 eA-3
C141 0.692 0.744 0.079 !       0.75 eA-3
Q142 0.342 0.641 0.348 !       0.75 eA-3
Q143 0.290 0.752 0.485 !       0.75 eA-3
Q144 0.268 0.720 0.483 !       0.75 eA-3
C145 0.756 0.855 0.113 !       0.74 eA-3
Q146 0.375 0.625 0.488 !       0.72 eA-3
Q147 0.735 0.407 0.498 !       0.72 eA-3
C148 0.450 0.994 0.032 !       0.71 eA-3
Q149 0.397 0.761 0.448 !       0.71 eA-3
C150 0.501 0.009 0.035 !       0.71 eA-3
Q151 0.082 0.078 0.393 !       0.70 eA-3
Q152 0.781 0.388 0.303 !       0.70 eA-3
Q153 0.016 0.045 0.252 !       0.69 eA-3
Q154 0.234 0.688 0.310 !       0.69 eA-3
Q155 0.435 0.688 0.438 !       0.69 eA-3
Q156 0.424 0.721 0.468 !       0.69 eA-3
Q157 1.000 1.000 0.500 !       0.68 eA-3
Q158 0.281 0.813 0.474 !       0.68 eA-3
C159 0.610 0.008 0.041 !       0.67 eA-3
Q160 0.765 0.316 0.449 !       0.67 eA-3
Q161 0.223 0.689 0.403 !       0.67 eA-3
Q162 0.307 0.039 0.097 !       0.65 eA-3
Q163 0.419 0.812 0.406 !       0.64 eA-3
C164 0.517 0.965 0.062 !       0.64 eA-3
Q165 0.424 0.737 0.423 !       0.63 eA-3
Q166 0.200 0.718 0.359 !       0.63 eA-3
Q167 0.389 0.563 0.457 !       0.63 eA-3
Q168 0.433 0.595 0.421 !       0.63 eA-3
Q169 0.450 0.875 0.126 !       0.63 eA-3
Q170 0.344 0.779 0.420 !       0.61 eA-3
Q171 0.438 0.784 0.487 !       0.61 eA-3
Q172 0.621 0.358 0.435 !       0.61 eA-3
Q173 0.785 0.721 0.113 !       0.61 eA-3
Q174 0.157 0.157 0.266 !       0.61 eA-3
C175 0.518 0.964 0.011 !       0.60 eA-3
Q176 0.610 0.223 0.474 !       0.60 eA-3
Q177 0.185 0.132 0.442 !       0.59 eA-3
Q178 0.754 0.223 0.498 !       0.58 eA-3
Q179 0.422 0.593 0.486 !       0.58 eA-3
C180 0.647 0.765 0.052 !       0.57 eA-3
Q181 0.785 0.324 0.503 !       0.57 eA-3
Q182 0.762 0.717 0.060 !       0.57 eA-3
Q183 0.505 0.127 0.435 !       0.57 eA-3
Q184 0.751 0.361 0.475 !       0.56 eA-3
Q185 0.688 0.200 0.483 !       0.56 eA-3
Q186 0.372 0.535 0.405 !       0.56 eA-3
Q187 0.409 0.861 0.359 !       0.56 eA-3
Q188 0.858 0.422 0.268 !       0.56 eA-3
Q189 0.345 0.611 0.476 !       0.56 eA-3
Q190 0.375 0.588 0.393 !       0.55 eA-3
Q191 0.362 0.840 0.264 !       0.55 eA-3
Q192 0.394 0.636 0.416 !       0.55 eA-3
Q193 0.297 0.578 0.479 !       0.54 eA-3
Q194 0.236 0.768 0.389 !       0.54 eA-3
Q195 0.471 0.564 0.437 !       0.54 eA-3
Q196 0.799 0.990 0.188 !       0.54 eA-3
Q197 0.875 0.198 0.487 !       0.53 eA-3
Q198 0.551 0.217 0.406 !       0.53 eA-3
Q199 0.636 0.142 0.473 !       0.53 eA-3
;
_refine_diff_density_max         0.653
_refine_diff_density_min         -1.702
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     816
_refine_ls_number_reflns         20309
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0356P)^2^+2.2075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13247
_reflns_number_total             20309
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj03318h2.cif
_cod_data_source_block           dme-21
_cod_depositor_comments
'Adding full bibliography for 7057608--7057610.cif.'
_cod_database_code               7057610
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C21 H16 N5 Au'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 B1(H1), B2(H2)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C4(H4), C13(H13), C37(H37), C019(H019), C52(H52), C62(H62),
 C31(H31), C47(H47), C22(H22), C24(H24), C5(H5), C29(H29), C23(H23), C7(H7),
 C6(H6), C42(H42), C26(H26), C57(H57), C25(H25)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C17(H17A,H17B,H17C), C8(H8A,H8B,H8C), C40(H40A,H40B,
 H40C), C16(H16A,H16B,H16C), C64(H64A,H64B,H64C), C15(H15A,H15B,H15C), C39(H39A,
 H39B,H39C), C54(H54A,H54B,H54C), C33(H33A,H33B,H33C), C55(H55A,H55B,H55C),
 C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C35(H35A,H35B,H35C), C65(H65A,H65B,
 H65C), C44(H44A,H44B,H44C), C34(H34A,H34B,H34C), C60(H60A,H60B,H60C), C59(H59A,
 H59B,H59C), C45(H45A,H45B,H45C)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'