Gold Catalysts with Polyaromatic-NHC ligands. Enhancement of Activity by Addition of Pyrene
Ibáñez, Susana; Poyatos, Macarena; Peris, Eduardo; Organometallics 36 (2017) 1447–; doi:10.1021/acs.organomet.7b00172

data_4087308
_publ_section_title
;
 Gold Catalysts with Polyaromatic-NHC ligands. Enhancement of Activity by
 Addition of Pyrene
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1447
_journal_paper_doi               10.1021/acs.organomet.7b00172
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C33 H42 Au Cl N2'
_chemical_formula_sum            'C33 H42 Au Cl N2'
_chemical_formula_weight         699.10
_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
_audit_creation_date             2017-01-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.854(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9193(5)
_cell_length_b                   13.3743(4)
_cell_length_c                   17.9921(6)
_cell_measurement_reflns_used    21384
_cell_measurement_temperature    200.0(3)
_cell_measurement_theta_max      29.0050
_cell_measurement_theta_min      3.2410
_cell_volume                     3018.36(19)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      200.0(3)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.947
_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    -20.00  30.25   0.67    7.50    --  -10.50 -99.00-180.00   75
  2  \w    -20.00  51.69   0.67    7.50    --   11.36 -99.00 -60.00  107
  3  \w    -15.00  87.51   0.67    7.50    --   11.36  37.00-150.00  153
  4  \w    -18.00  84.51   0.67    7.50    --   11.36  57.00  90.00  153
  5  \w    -65.00  37.51   0.67    7.50    --   11.36 -37.00 -30.00  153
  6  \w    -67.00  44.22   0.67    7.50    --   11.36 -77.00-120.00  166
  7  \w    -70.00  57.30   0.67    7.50    --   11.36 -19.00-150.00  190
  8  \w    -20.00  16.18   0.67    7.50    --  -10.50 -99.00 -90.00   54
  9  \w    -65.00  37.51   0.67    7.50    --   11.36 -37.00  90.00  153
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            63612
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.222
_diffrn_reflns_theta_min         2.930
_exptl_absorpt_coefficient_mu    4.986
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       prism
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.131
_refine_diff_density_max         1.030
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         7777
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+3.6760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6600
_reflns_number_total             7777
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00172_si_002.cif
_cod_data_source_block           str1877
_cod_original_cell_volume        3018.33(18)
_cod_database_code               4087308
_shelx_shelxl_version_number     2014/7
_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 Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C6(H6A,H6B), C3(H3A,H3B), C4(H4A,H4B), C8(H8A,H8B), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C15(H15), C12(H12), C23(H23), C24(H24), C25(H25)
2.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C29(H29A,H29B,H29C), C27(H27A,H27B,H27C), C31(H31A,H31B,
 H31C), C28(H28A,H28B,H28C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C32(H32A,H32B,
 H32C)
;
_shelx_res_checksum              5046
_shelx_hkl_checksum              78453
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;