#------------------------------------------------------------------------------
#$Date: 2020-10-19 10:35:42 +0300 (Mon, 19 Oct 2020) $
#$Revision: 258458 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/93/4349311.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4349311
loop_
_publ_author_name
'Goettel, James T.'
'Gerken, Michael'
_publ_section_title
;
 Synthesis and Characterization of Adducts between SF₄ and
 Oxygen Bases: Examples of O···S(IV) Chalcogen
 Bonding.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              12441
_journal_page_last               12450
_journal_paper_doi               10.1021/acs.inorgchem.6b02373
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C8 H16 F8 O2 S2'
_chemical_formula_weight         360.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 97.074(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.225(4)
_cell_length_b                   10.798(4)
_cell_length_c                   12.435(4)
_cell_measurement_reflns_used    5957
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.31
_cell_volume                     1495.7(9)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart Apex II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16903
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.641
_diffrn_reflns_theta_min         2.307
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.439
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS (Sheldrick, 2004)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_description       plate
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.501
_exptl_crystal_size_mid          0.314
_exptl_crystal_size_min          0.152
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0047(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         3481
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0384P)²+1.6212P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1193
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2905
_reflns_number_total             3481
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b02373_si_002.cif
_cod_data_source_block           MG12088_0m
_cod_depositor_comments
;

2020-10-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C4 H8 F4 O S'
_cod_original_formula_weight         180.16
_cod_original_formula_units_Z            8
_cod_original_cell_volume        1495.7(8)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4349311
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.810
_shelx_estimated_absorpt_t_max   0.936
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
S1 S 0.79197(5) 0.12944(5) 0.44086(5) 0.03727(17) Uani 1 1 d . .
F1 F 0.87235(15) 0.06025(17) 0.36831(14) 0.0621(5) Uani 1 1 d . .
F2 F 0.86200(15) 0.09785(19) 0.55130(13) 0.0670(5) Uani 1 1 d . .
F3 F 0.88144(17) 0.25122(18) 0.43543(16) 0.0749(6) Uani 1 1 d . .
F4 F 0.71681(18) -0.00014(15) 0.44871(15) 0.0680(5) Uani 1 1 d . .
S2 S 0.52556(6) 0.29627(6) 0.37436(5) 0.04237(18) Uani 1 1 d . .
F5 F 0.45907(17) 0.33628(17) 0.26344(14) 0.0688(5) Uani 1 1 d . .
F6 F 0.44944(15) 0.36924(16) 0.44838(14) 0.0619(5) Uani 1 1 d . .
F7 F 0.60794(17) 0.42237(17) 0.37026(15) 0.0711(5) Uani 1 1 d . .
F8 F 0.42580(18) 0.18330(17) 0.37430(16) 0.0718(5) Uani 1 1 d . .
O1 O 0.66207(17) 0.16954(16) 0.23661(12) 0.0459(4) Uani 1 1 d . .
C1 C 0.6050(2) 0.0719(2) 0.1697(2) 0.0448(6) Uani 1 1 d . .
H1A H 0.5170 0.0738 0.1709 0.054 Uiso 1 1 calc R U
H1B H 0.6356 -0.0100 0.1963 0.054 Uiso 1 1 calc R U
C2 C 0.6351(3) 0.0946(3) 0.0565(2) 0.0484(6) Uani 1 1 d . .
H2A H 0.6918 0.0313 0.0357 0.058 Uiso 1 1 calc R U
H2B H 0.5617 0.0933 0.0034 0.058 Uiso 1 1 calc R U
C3 C 0.6912(4) 0.2197(4) 0.0622(3) 0.0976(16) Uani 1 1 d . .
H3A H 0.7601 0.2213 0.0195 0.117 Uiso 1 1 calc R U
H3B H 0.6321 0.2826 0.0320 0.117 Uiso 1 1 calc R U
C4 C 0.7299(4) 0.2454(3) 0.1706(2) 0.0745(11) Uani 1 1 d . .
H4A H 0.7172 0.3341 0.1858 0.089 Uiso 1 1 calc R U
H4B H 0.8166 0.2270 0.1871 0.089 Uiso 1 1 calc R U
O2 O 0.64497(14) 0.23807(14) 0.57821(12) 0.0352(3) Uani 1 1 d . .
C5 C 0.5829(2) 0.1552(2) 0.64360(19) 0.0438(6) Uani 1 1 d . .
H5A H 0.6102 0.0689 0.6358 0.053 Uiso 1 1 calc R U
H5B H 0.4951 0.1590 0.6216 0.053 Uiso 1 1 calc R U
C6 C 0.6133(3) 0.1988(3) 0.7590(2) 0.0503(6) Uani 1 1 d . .
H6A H 0.6870 0.1583 0.7942 0.060 Uiso 1 1 calc R U
H6B H 0.5465 0.1824 0.8021 0.060 Uiso 1 1 calc R U
C7 C 0.6321(3) 0.3363(3) 0.7454(2) 0.0486(6) Uani 1 1 d . .
H7A H 0.5548 0.3814 0.7358 0.058 Uiso 1 1 calc R U
H7B H 0.6840 0.3713 0.8082 0.058 Uiso 1 1 calc R U
C8 C 0.6930(2) 0.3408(2) 0.64408(18) 0.0375(5) Uani 1 1 d . .
H8A H 0.6756 0.4201 0.6054 0.045 Uiso 1 1 calc R U
H8B H 0.7810 0.3324 0.6621 0.045 Uiso 1 1 calc R U
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
F2 S1 F1 98.25(10)
F2 S1 F4 88.15(11)
F1 S1 F4 87.93(10)
F2 S1 F3 88.09(11)
F1 S1 F3 87.68(10)
F4 S1 F3 173.77(11)
F2 S1 O2 79.70(8)
F1 S1 O2 175.99(8)
F4 S1 O2 88.56(7)
F3 S1 O2 95.66(8)
F2 S1 O1 176.04(9)
F1 S1 O1 79.72(8)
F4 S1 O1 88.38(8)
F3 S1 O1 95.20(8)
O2 S1 O1 102.12(6)
F6 S2 F5 98.46(10)
F6 S2 F7 87.18(10)
F5 S2 F7 87.28(10)
F6 S2 F8 87.28(11)
F5 S2 F8 87.33(10)
F7 S2 F8 171.62(11)
F6 S2 O2 79.21(8)
F5 S2 O2 176.75(8)
F7 S2 O2 90.32(8)
F8 S2 O2 94.81(8)
F6 S2 O1 178.47(8)
F5 S2 O1 80.26(9)
F7 S2 O1 91.92(8)
F8 S2 O1 93.49(8)
O2 S2 O1 102.03(6)
C4 O1 C1 108.37(18)
C4 O1 S2 116.03(18)
C1 O1 S2 118.26(15)
C4 O1 S1 110.57(17)
C1 O1 S1 123.64(14)
S2 O1 S1 77.49(5)
O1 C1 C2 106.53(19)
C3 C2 C1 104.2(2)
C4 C3 C2 107.9(3)
C3 C4 O1 108.3(2)
C8 O2 C5 109.19(16)
C8 O2 S1 117.70(12)
C5 O2 S1 116.69(13)
C8 O2 S2 116.54(12)
C5 O2 S2 116.09(14)
S1 O2 S2 77.98(5)
O2 C5 C6 105.90(19)
C5 C6 C7 102.6(2)
C8 C7 C6 102.0(2)
O2 C8 C7 105.89(19)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
S1 F2 1.5344(17)
S1 F1 1.5448(16)
S1 F4 1.6430(17)
S1 F3 1.6610(18)
S1 O2 2.7766(17)
S1 O1 2.8022(19)
S2 F6 1.5465(17)
S2 F5 1.5468(16)
S2 F7 1.6503(19)
S2 F8 1.6557(19)
S2 O2 2.7892(17)
S2 O1 2.793(2)
O1 C4 1.442(3)
O1 C1 1.443(3)
C1 C2 1.508(3)
C2 C3 1.488(4)
C3 C4 1.393(4)
O2 C8 1.443(3)
O2 C5 1.444(3)
C5 C6 1.508(3)
C6 C7 1.512(4)
C7 C8 1.507(3)
