1,3-Dipolar Cycloaddition of Nitrones to Gold(III)-Bound Isocyanides
Anisimova, Tatyana B.; Kinzhalov, Mikhail A.; Kuznetsov, Maxim L.; Guedes da Silva, M. Fátima C.; Zolotarev, Andrey A.; Kukushkin, Vadim Yu.; Pombeiro, Armando J. L.; Luzyanin, Konstantin V.; Organometallics 35 (2016) 3569–; doi:10.1021/acs.organomet.6b00635

data_4089022
_publ_section_title
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 1,3-Dipolar Cycloaddition of Nitrones to Gold(III)-Bound Isocyanides
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              3569
_journal_paper_doi               10.1021/acs.organomet.6b00635
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C14 H20 Au Cl3 N2 O, C H2 Cl2'
_chemical_formula_sum            'C15 H22 Au Cl5 N2 O'
_chemical_formula_weight         620.56
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-04-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                101.664(4)
_cell_angle_beta                 98.710(4)
_cell_angle_gamma                95.481(4)
_cell_formula_units_Z            2
_cell_length_a                   7.5167(4)
_cell_length_b                   9.4910(3)
_cell_length_c                   15.2776(8)
_cell_measurement_reflns_used    5295
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      33.8660
_cell_measurement_theta_min      3.3300
_cell_volume                     1046.11(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3829
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
  1 omega  -20.00   47.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.1623   38.0000  -30.0000 67

  2 omega   36.00  118.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8811 -178.0000 -180.0000 82

  3 omega   -3.00  108.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8811   77.0000    0.0000 111

  4 omega  -17.00   25.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8811  -99.0000 -180.0000 42

  5 omega   12.00   39.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8811   77.0000 -180.0000 27

  6 omega  -49.00   26.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8811  -77.0000  -90.0000 75
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0441692000
_diffrn_orient_matrix_UB_12      0.0061082000
_diffrn_orient_matrix_UB_13      0.0453020000
_diffrn_orient_matrix_UB_21      0.0328360000
_diffrn_orient_matrix_UB_22      0.0735696000
_diffrn_orient_matrix_UB_23      0.0025613000
_diffrn_orient_matrix_UB_31      -0.0790045000
_diffrn_orient_matrix_UB_32      0.0217709000
_diffrn_orient_matrix_UB_33      0.0161136000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9326
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         3.137
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.676
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour
;
;
_exptl_crystal_density_diffrn    1.970
_exptl_crystal_description
;
;
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.499
_refine_diff_density_min         -1.626
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         4715
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0330P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0788
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4230
_reflns_number_total             4715
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00635_si_002.cif
_cod_data_source_block           Compound13
_cod_database_code               4089022
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C20 H10 Au Cl3 O1 N2'
_reflns_odcompleteness_completeness 94.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     35.02
_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.a Ternary CH refined with riding coordinates:
 C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C12(H12), C13(H13)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C11(H11A,H11B,H11C),
 C14(H14A,H14B,H14C)
;
_olex2_submission_special_instructions 'No special instructions were received'