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_4087309
_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         'C39 H44 Au Cl N4, C H2 Cl2'
_chemical_formula_sum            'C40 H46 Au Cl3 N4'
_chemical_formula_weight         886.12
_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
_atom_sites_solution_primary     direct
_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                 106.018(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.2606(9)
_cell_length_b                   15.3724(7)
_cell_length_c                   12.0815(6)
_cell_measurement_reflns_used    8926
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.0640
_cell_measurement_theta_min      3.1760
_cell_volume                     3795.3(3)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.919
_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_unetI/netI     0.0647
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11248
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.218
_diffrn_reflns_theta_min         2.990
_exptl_absorpt_coefficient_mu    4.121
_exptl_absorpt_correction_T_max  0.823
_exptl_absorpt_correction_T_min  0.274
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_description       needle
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.479
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.039
_refine_diff_density_max         1.876
_refine_diff_density_min         -1.496
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         11248
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0871P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1321
_refine_ls_wR_factor_ref         0.1386
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7951
_reflns_number_total             11248
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00172_si_002.cif
_cod_data_source_block           str1878_twin1_hklf4
_cod_database_code               4087309
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6063(11) 0.3937(11)
2. 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
3. Uiso/Uaniso restraints and constraints
Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C33) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C2(H2A,H2B), C7(H7A,H7B), C3(H3A,H3B), C8(H8A,H8B), C4(H4A,H4B),
 C1G(H1GA,H1GB)
4.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C31(H31), C29(H29), C30(H30), C13(H13), C18(H18), C21(H21), C26(H26)
4.c Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C37(H37A,H37B,H37C), C9(H9A,H9B,
 H9C), C35(H35A,H35B,H35C), C5(H5A,H5B,H5C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C)
;
_shelx_res_checksum              41785
_shelx_hkl_checksum              64042
_olex2_submission_special_instructions 'No special instructions were received'