From metallic gold to [Au(NHC)2](+) complexes: an easy, one-pot method.
Lozada-Rodríguez, Leticia; Pelayo-Vázquez, José B; Rangel-Salas, Irma I; Alvarado-Rodríguez, José G; Peregrina-Lucano, A Aarón; Pérez-Centeno, Armando; López-Dellamary-Toral, Fernando A; Cortes-Llamas, Sara A; Dalton transactions (Cambridge, England : 2003) 46 (2017) 3809–3811; doi:10.1039/c7dt00322f

data_7041970
_publ_section_title
;
 From metallic gold to [Au(NHC)2](+) complexes: an easy, one-pot method.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3809
_journal_page_last               3811
_journal_paper_doi               10.1039/c7dt00322f
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         '1(C12 H20 Au N4), C24 H20 B'
_chemical_formula_sum            'C36 H40 Au B N4'
_chemical_formula_weight         736.49
_chemical_melting_point          411
_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     direct
_audit_creation_date             2016-05-10
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-12-15 deposited with the CCDC.
2017-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                65.28(3)
_cell_angle_beta                 78.17(3)
_cell_angle_gamma                81.27(3)
_cell_formula_units_Z            2
_cell_length_a                   11.566(2)
_cell_length_b                   11.987(2)
_cell_length_c                   13.298(3)
_cell_measurement_reflns_used    16653
_cell_measurement_temperature    293
_cell_measurement_theta_max      26.4260
_cell_measurement_theta_min      3.5740
_cell_volume                     1634.6(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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
_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 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -17.00  84.60   0.80   15.00    --   11.45  57.00 -60.00  127
  2  \w    -13.00  85.40   0.80   15.00    --   11.45  37.00-150.00  123
  3  \w    -17.00  84.60   0.80   15.00    --   11.45  57.00  60.00  127
  4  \w    -61.00  39.00   0.80   15.00    --   11.45 -57.00 -90.00  125
  5  \w    -33.00  49.40   0.80   15.00    --   11.45 -92.00 136.33  103
  6  \w    -25.00  51.00   0.80   15.00    --   11.45 -99.00  30.00   95
  7  \w    -10.00  62.00   0.80   15.00    --   11.45-117.00 -96.79   90
  8  \w    -82.00 -34.00   0.80   15.00    --   -9.96 149.00  86.56   60
  9  \w    -62.00 -14.00   0.80   15.00    --   -9.96 118.00 -95.70   60
 10  \w    -25.00  31.00   0.80   15.00    --   -9.96 -99.00 -60.00   70
 11  \w    -67.00 -19.00   0.80   15.00    --   -9.96 126.00 -54.44   60
 12  \w    -34.00  64.40   0.80   15.00    --   -9.96  37.00 150.00  123
 13  \w    -25.00  51.00   0.80   15.00    --   11.45 -99.00  90.00   95
 14  \w    -38.00  62.00   0.80   15.00    --   -9.96  57.00-120.00  125
 15  \w    -87.00 -39.00   0.80   15.00    --   -9.96 156.00-169.05   60
 16  \w    -85.00 -37.00   0.80   15.00    --   -9.96 153.00-108.81   60
 17  \w    -77.00 -19.40   0.80   15.00    --   11.45   0.00-150.00   72
 18  \w    -77.00  99.00   0.80   15.00    --   11.45   0.00-180.00  220
 19  \w    -65.00  43.00   0.80   15.00    --   11.45 -77.00  90.00  135
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0261084000
_diffrn_orient_matrix_UB_12      -0.0320857000
_diffrn_orient_matrix_UB_13      -0.0229218000
_diffrn_orient_matrix_UB_21      0.0439802000
_diffrn_orient_matrix_UB_22      -0.0494070000
_diffrn_orient_matrix_UB_23      0.0164387000
_diffrn_orient_matrix_UB_31      -0.0364974000
_diffrn_orient_matrix_UB_32      -0.0282258000
_diffrn_orient_matrix_UB_33      0.0523477000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            62940
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.297
_diffrn_reflns_theta_min         3.171
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.530
_exptl_absorpt_correction_T_max  0.05419
_exptl_absorpt_correction_T_min  0.03468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         5941
_refine_ls_number_restraints     242
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0263
_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^)+(0.0224P)^2^+0.9851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0641
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4545
_reflns_number_total             5941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00322f2.cif
_cod_data_source_block           2i_16scl11mo
_cod_depositor_comments
'Adding full bibliography for 7041969--7041974.cif.'
_cod_database_code               7041970
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H5A,H5B} of C5, {H51C,H51D} of C51A, {H5AA,H5AB} of C5A
 At 1.5 times of:
  All C(H,H,H) groups, {H51A,H51B} of C51
2. Restrained distances
 Au1-C1 \\sim Au1-C11 \\sim Au1A-C1A \\sim Au1-C11A
 with sigma of 0.02
3. Rigid bond restraints
 C1, N1, C2, C3, N2, C4, C5, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, C11, N11, C21, C31, N21, C41, C51, C61
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1A, N11A, C21A, C31A, N21A, C41A, C51A, C61A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1A, C11A, N11A, C21A, C31A, N21A, C41A, C51A, C61A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim N1 \\sim C2 \\sim C3 \\sim N2: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C4 \\sim C5 \\sim C6: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08
C11 \\sim N11 \\sim C21 \\sim C31 \\sim N21: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C41 \\sim C51 \\sim C61: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C1A \\sim N1A \\sim C2A \\sim C3A \\sim N2A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C4A \\sim C5A \\sim C6A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C1A \\sim C11A \\sim N11A \\sim C21A \\sim C31A \\sim N21A: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C41A \\sim C51A \\sim C61A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
5. Same fragment restrains
{Au1A, C1A, N1A, C2A, C3A, N2A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as
{Au1, C1, N1, C2, C3, N2, C4, C5, C6}
{C11A, N11A, C21A, C31A, N21A, C41A, C51A, C61A} sigma for 1-2: 0.02, 1-3: 0.04
as
{C11, N11, C21, C31, N21, C41, C51, C61}
6. Others
 Sof(Au1A)=Sof(C1A)=Sof(N1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(N2A)=
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C6A)=
 Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C11A)=Sof(N11A)=Sof(C21A)=Sof(H21A)=
 Sof(C31A)=Sof(H31A)=Sof(N21A)=Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=
 Sof(C51A)=Sof(H51C)=Sof(H51D)=Sof(C61A)=Sof(H61D)=Sof(H61E)=Sof(H61F)=1-FVAR(1)
 Sof(Au1)=Sof(C1)=Sof(N1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(N2)=Sof(C4)=
 Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(H6C)=Sof(C11)=Sof(N11)=Sof(C21)=Sof(H21)=Sof(C31)=Sof(H31)=Sof(N21)=
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(C61)=
 Sof(H61A)=Sof(H61B)=Sof(H61C)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C51(H51A,H51B), C5A(H5AA,H5AB), C51A(H51C,H51D)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C21(H21), C31(H31), C2A(H2A), C3A(H3A), C21A(H21A),
 C31A(H31A), C91(H91), C92(H92), C93(H93), C94(H94), C95(H95), C97(H97),
 C98(H98), C99(H99), C70(H70), C71(H71), C73(H73), C74(H74), C75(H75), C76(H76),
  C77(H77), C79(H79), C80(H80), C81(H81), C82(H82), C83(H83)
7.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C41(H41A,H41B,H41C), C61(H61A,H61B,H61C),
 C4A(H4AA,H4AB,H4AC), C6A(H6AA,H6AB,H6AC), C41A(H41D,H41E,H41F), C61A(H61D,H61E,
 H61F)
;
_shelx_res_checksum              98944