The Sulfur‒Fluorine Gauche Effect in Coinage-Metal Complexes: Augmenting Conformational Equilibria by Complexation
Santschi, Nico; Thiehoff, Christian; Holland, Mareike C.; Daniliuc, Constantin G.; Houk, K. N.; Gilmour, Ryan; Organometallics 35 (2016) 3040–; doi:10.1021/acs.organomet.6b00564

data_4088914
_publ_section_title
;
 The Sulfur--Fluorine Gauche Effect in Coinage-Metal Complexes: Augmenting
 Conformational Equilibria by Complexation
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              3040
_journal_paper_doi               10.1021/acs.organomet.6b00564
_journal_volume                  35
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_sum            'C17.66667 H18.33333 Au Cl2.33333 F S'
_chemical_formula_weight         561.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 99.640(3)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   8.0568(5)
_cell_length_b                   14.4365(8)
_cell_length_c                   24.0039(16)
_cell_measurement_reflns_used    9805
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      26.4054
_cell_measurement_theta_min      2.5642
_cell_volume                     2752.5(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection
;
APEX2 v.2014.1-1 (Bruker AXS Inc., 2014)

;
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XP (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'MX mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1288
_diffrn_reflns_av_unetI/netI     0.0618
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            92891
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.56
_diffrn_source                   'Mo ImS'
_diffrn_source_type              'micro focus tube'
_exptl_absorpt_coefficient_mu    8.475
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Bruker AXS (2014). SADABS, Version 2014/2, Bruker AXS Inc., Madison, Wisconsin,
USA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.032
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.305
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.029
_refine_diff_density_max         1.206
_refine_diff_density_min         -1.661
_refine_ls_abs_structure_details
;
Flack x determined using 3813 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.042(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         10066
_refine_ls_number_restraints     319
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0392
_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^)+14.1143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0678
_reflns_number_gt                9031
_reflns_number_total             10066
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00564_si_003.cif
_cod_data_source_block           gil8164
_cod_depositor_comments
;

2020-06-17
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C53 H55 Au3 Cl7 F3 S3'
_cod_original_formula_weight         1684.20
_cod_original_formula_units_Z            2
_cod_database_code               4088914
_shelx_res_checksum              57920
_shelx_hkl_checksum              4110