Small-molecule activation at Au(iii): metallacycle construction from ethylene, water, and acetonitrile.
Holmsen, Marte Sofie Martinsen; Nova, Ainara; Balcells, David; Langseth, Eirin; Øien-Ødegaard, Sigurd; Tråseth, Eline Aasen; Heyn, Richard H.; Tilset, Mats; Dalton transactions (Cambridge, England : 2003) 45 (2016) 14719–14724; doi:10.1039/c6dt01648k

data_7039459
_publ_section_title
;
 Small-molecule activation at Au(iii): metallacycle construction from
 ethylene, water, and acetonitrile.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14719
_journal_page_last               14724
_journal_paper_doi               10.1039/c6dt01648k
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C16 H18 Au N2 O, C2 F3 O2'
_chemical_formula_sum            'C18 H18 Au F3 N2 O3'
_chemical_formula_weight         564.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2n'
_space_group_name_H-M_alt        'P 1 1 21/n'
_symmetry_space_group_name_Hall  '-P 2n'
_symmetry_space_group_name_H-M   'P 1 1 21/n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-12-21 deposited with the CCDC.
2016-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 89.9973(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.1906(6)
_cell_length_b                   12.6491(10)
_cell_length_c                   19.3960(16)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.64
_cell_measurement_theta_min      2.65
_cell_volume                     1764.2(2)
_computing_cell_refinement       'APEX2 v2014.11-0 (Bruker-AXS, 2014)'
_computing_data_collection       'APEX2 v2014.11-0 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker-AXS, 2014)'
_computing_molecular_graphics    'Diamond v4.0.1 (Brandenburg, 2014)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_detector                 'Bruker PHOTON100 area detector'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture, CMOS detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            28613
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.617
_diffrn_reflns_theta_min         2.646
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.391
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.3406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1022 before and 0.0516 after correction.
The Ratio of minimum to maximum transmission is 0.4564.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.125
_exptl_crystal_description       prism
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.472
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.077
_exptl_transmission_factor_max   1.0000
_exptl_transmission_factor_min   0.4564
_refine_diff_density_max         0.789
_refine_diff_density_min         -1.515
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         5951
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0187
_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^)+(0.0043P)^2^+0.9651P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0415
_refine_ls_wR_factor_ref         0.0424
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5610
_reflns_number_total             5951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01648k2.cif
_cod_data_source_block           msh-246-mp_sx
_cod_depositor_comments
'Adding full bibliography for 7039458--7039459.cif.'
_cod_database_code               7039459
_shelx_estimated_absorpt_t_max   0.564
_shelx_estimated_absorpt_t_min   0.110
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5112(6) 0.4888(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C17(H17A,H17B)
3.b Aromatic/amide H refined with riding coordinates:
 N5(H5), C10(H10), C11(H11), C12(H12), C18(H18), C7(H7), C13(H13), C15(H15)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              75365
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'