Synthesis and Characterization of N-Trifluoromethyl N-Heterocyclic Carbene Ligands and Their Complexes
Engl, Pascal S.; Senn, Remo; Otth, Elisabeth; Togni, Antonio; Organometallics 34 (2015) 1384–; doi:10.1021/acs.organomet.5b00137

data_4087458
_publ_section_title
;
 Synthesis and Characterization of N-Trifluoromethyl N-Heterocyclic
 Carbene Ligands and Their Complexes
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1384
_journal_paper_doi               10.1021/acs.organomet.5b00137
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C9 H7 Au Cl F3 N2'
_chemical_formula_sum            'C9 H7 Au Cl F3 N2'
_chemical_formula_weight         432.58
_chemical_melting_point          324
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-12-04
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.303(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.0300(15)
_cell_length_b                   6.5561(11)
_cell_length_c                   9.5756(16)
_cell_measurement_reflns_used    3336
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.98
_cell_measurement_theta_min      2.24
_cell_volume                     538.21(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10085
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.988
_diffrn_reflns_theta_min         2.240
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.927
_exptl_absorpt_correction_T_max  0.9978
_exptl_absorpt_correction_T_min  0.5362
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'SADABS 2004/1'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.669
_exptl_crystal_description       plate
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.048
_refine_diff_density_max         1.888
_refine_diff_density_min         -1.749
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         1852
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0264
_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^)+(0.0272P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0566
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1648
_reflns_number_total             1852
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00137_si_002.cif
_cod_data_source_block           Compound_9a
_cod_database_code               4087458
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.555
_shelx_estimated_absorpt_t_min   0.295
_olex2_refinement_description
;
1. Others
 Fixed Sof: H9A(0.5) H9B(0.5) H9C(0.5)
 Fixed U12: Au1(0) Cl1(0) C1(0) C2(0) N1(0) F2(0) C5(0) C4(0) C3(0) N2(0)
 C8(0) C7(0) C9(0) C6(0)
 Fixed U23: Au1(0) Cl1(0) C1(0) C2(0) N1(0) F2(0) C5(0) C4(0) C3(0) N2(0)
 C8(0) C7(0) C9(0) C6(0)
 Fixed Uiso: H5(0.029) H4(0.022) H7(0.023) H9A(0.035) H9B(0.035) H9C(0.035)
 H6(0.032)
 Fixed X: H5(0.4505) H4(0.4324) H7(0.9223) H9A(1.1305) H9B(1.1151) H9C(1.1526)
 H6(0.6883)
 Fixed Y: Au1(0.25) Cl1(0.25) C1(0.25) C2(0.25) N1(0.25) F2(0.25) C5(0.25)
 H5(0.25) C4(0.25) H4(0.25) C3(0.25) N2(0.25) C8(0.25) C7(0.25) H7(0.25)
 C9(0.25) H9A(0.3902) H9B(0.1675) H9C(0.1923) C6(0.25) H6(0.25)
 Fixed Z: H5(-0.2246) H4(0.0155) H7(-0.0717) H9A(0.235) H9B(0.1634)
 H9C(0.3374) H6(-0.2653)
;
_shelx_res_checksum              7893
_shelx_hkl_checksum              47138
_olex2_submission_special_instructions 'No special instructions were received'