Anin-Fluorosilaphane: The Largestin-Functional Group Is a Uniquely Encapsulated Fluorine Atom
Steven Dell; Nancy J. Vogelaar; Douglas M. Ho; Robert A. Pascal; Journal of the American Chemical Society 120 (1998) 6421–6422; doi:10.1021/ja981009s

data_4116745
_publ_section_title
;
 Anin-Fluorosilaphane: The Largestin-Functional Group Is a Uniquely
 Encapsulated Fluorine Atom
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6421
_journal_page_last               6422
_journal_paper_doi               10.1021/ja981009s
_journal_volume                  120
_journal_year                    1998
_chemical_compound_source        'chemical synthesis'
_chemical_formula_moiety         C~30~H~27~FS~3~Si
_chemical_formula_structural     C~30~H~27~FS~3~Si
_chemical_formula_sum            'C30 H27 F S3 Si'
_chemical_formula_weight         530.79
_chemical_name_common            In-Fluorosilaphane
_chemical_name_systematic
; 
 Tribenzo 6-Fluoro-6-sila-2,10,19-trithia[5(6,14)][11]metacyclophane 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 108.97(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.377(18)
_cell_length_b                   17.267(39)
_cell_length_c                   15.414(22)
_cell_measurement_temperature    298(2)
_cell_volume                     2612(8)
_computing_cell_refinement       SCALEPACK
_computing_data_collection       'Rigaku R-AXIS IIC, Version 2.1'
_computing_data_reduction        DENZO
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Rigaku R-AXIS IIC'
_diffrn_measurement_method
'oscillations; 750~o~ data in 3~o~ and 6~o~ increments'
_diffrn_radiation_monochromator  'double-focusing mirrors'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13353
_diffrn_reflns_theta_max         46.38
_diffrn_reflns_theta_min         5.21
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.230
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.192
_refine_diff_density_min         -0.163
_refine_diff_density_rms         0.028
_refine_ls_extinction_coef       0.0014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.032
_refine_ls_goodness_of_fit_obs   1.044
_refine_ls_hydrogen_treatment    'xyz riding, U(H) = 1.2U(C)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         2196
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.336
_refine_ls_restrained_S_obs      1.044
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_obs          0.0276
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+1.5486P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0948
_refine_ls_wR_factor_obs         0.0724
_reflns_number_observed          2110
_reflns_number_total             2197
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja981009s.cif
_cod_data_source_block           97088f
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+1.5486P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+1.5486P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2611.9(83)
_cod_database_code               4116745