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_4088915
_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            'C34 H34 Ag2 F14 S2 Sb2'
_chemical_formula_weight         1231.97
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4030(7)
_cell_length_b                   14.0758(6)
_cell_length_c                   15.9506(6)
_cell_measurement_reflns_used    9626
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      27.5710
_cell_measurement_theta_min      2.6664
_cell_volume                     3907.3(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 (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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0391
_diffrn_reflns_av_unetI/netI     0.0122
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            168450
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.26
_diffrn_source                   'Mo ImS'
_diffrn_source_type              'micro focus tube'
_exptl_absorpt_coefficient_mu    2.555
_exptl_absorpt_correction_T_max  0.73
_exptl_absorpt_correction_T_min  0.66
_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    2.094
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.226
_exptl_crystal_size_min          0.132
_refine_diff_density_max         1.556
_refine_diff_density_min         -0.981
_refine_ls_abs_structure_details
;
Flack x determined using 3474 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.024(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         7980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0205P)^2^+22.2010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0756
_reflns_number_gt                7915
_reflns_number_total             7980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00564_si_003.cif
_cod_data_source_block           gil8183
_cod_database_code               4088915
_shelx_res_checksum              33611
_shelx_hkl_checksum              47868