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#$Date: 2017-01-05 03:58:03 +0200 (Thu, 05 Jan 2017) $
#$Revision: 189857 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/54/4125400.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_4125400
loop_
_publ_author_name
'Beldjoudi, Yassine'
'Arauzo, Ana'
'Palacio, Fernando'
'Pilkington, Melanie'
'Rawson, Jeremy M.'
_publ_section_title
;
 Studies on a "Disappearing Polymorph": Thermal and Magnetic
 Characterization of α-p-NCC6F4CNSSN(•).
;
_journal_issue                   51
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16779
_journal_page_last               16786
_journal_paper_doi               10.1021/jacs.6b10707
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C8 F4 N3 S2'
_chemical_formula_sum            'C8 F4 N3 S2'
_chemical_formula_weight         278.23
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     intrinsic
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                65.67(11)
_cell_angle_beta                 67.56(9)
_cell_angle_gamma                67.47(8)
_cell_formula_units_Z            2
_cell_length_a                   7.755(8)
_cell_length_b                   8.128(12)
_cell_length_c                   9.746(15)
_cell_measurement_reflns_used    4926
_cell_measurement_temperature    343(2)
_cell_measurement_theta_max      27.13
_cell_measurement_theta_min      2.38
_cell_volume                     498.4(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      343(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II with CCD detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1094
_diffrn_reflns_av_unetI/netI     0.0578
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6744
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.132
_diffrn_reflns_theta_min         2.379
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6011
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.854
_exptl_crystal_description       block
_exptl_crystal_F_000             274
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2186
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0752
_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)+(0.0697P)²+1.0705P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2008
_refine_ls_wR_factor_ref         0.2054
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1980
_reflns_number_total             2186
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b10707_si_001.cif
_cod_data_source_block           YBalpha70C_a
_cod_database_code               4125400
_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   0.764
_shelx_estimated_absorpt_t_max   0.994
_shelxl_version_number           2013-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
S1 S 0.73393(17) 0.51968(17) 0.06506(15) 0.0505(4) Uani 1 1 d
S2 S 0.5261(2) 0.75222(16) 0.12173(16) 0.0588(4) Uani 1 1 d
F2 F 0.4269(4) 0.1096(4) 0.2747(3) 0.0524(7) Uani 1 1 d
F3 F 0.2096(4) -0.1049(4) 0.5013(3) 0.0525(7) Uani 1 1 d
F6 F 0.2226(5) 0.5144(4) 0.5784(3) 0.0573(8) Uani 1 1 d
F5 F 0.0088(5) 0.2948(5) 0.8039(3) 0.0612(8) Uani 1 1 d
N1 N 0.6178(5) 0.3682(5) 0.2023(4) 0.0426(9) Uani 1 1 d
N2 N 0.3822(6) 0.6305(5) 0.2636(5) 0.0493(10) Uani 1 1 d
C1 C 0.3320(5) 0.3238(5) 0.4163(4) 0.0306(8) Uani 1 1 d
C0 C 0.4504(6) 0.4470(5) 0.2876(4) 0.0305(8) Uani 1 1 d
C3 C 0.2139(6) 0.0464(5) 0.5205(5) 0.0339(8) Uani 1 1 d
C2 C 0.3255(6) 0.1600(6) 0.4033(5) 0.0336(8) Uani 1 1 d
C4 C 0.1030(6) 0.0881(6) 0.6598(5) 0.0361(9) Uani 1 1 d
C6 C 0.2216(6) 0.3637(6) 0.5549(5) 0.0361(9) Uani 1 1 d
N3 N -0.1144(6) -0.1198(6) 0.8710(6) 0.0622(13) Uani 1 1 d
C5 C 0.1105(6) 0.2501(6) 0.6732(5) 0.0377(9) Uani 1 1 d
C7 C -0.0168(6) -0.0280(7) 0.7786(5) 0.0436(10) Uani 1 1 d
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'
N N 0.0061 0.0033 '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
N1 S1 S2 94.73(19)
N2 S2 S1 94.39(19)
C0 N1 S1 113.4(3)
C0 N2 S2 113.9(3)
C6 C1 C2 116.4(4)
C6 C1 C0 122.1(4)
C2 C1 C0 121.5(4)
N2 C0 N1 123.5(4)
N2 C0 C1 118.0(4)
N1 C0 C1 118.5(4)
F3 C3 C2 119.8(4)
F3 C3 C4 119.2(4)
C2 C3 C4 121.0(4)
F2 C2 C3 117.0(4)
F2 C2 C1 120.9(4)
C3 C2 C1 122.1(4)
C3 C4 C5 117.0(4)
C3 C4 C7 120.4(4)
C5 C4 C7 122.6(4)
F6 C6 C5 117.7(4)
F6 C6 C1 120.4(4)
C5 C6 C1 121.9(4)
F5 C5 C6 119.2(4)
F5 C5 C4 119.2(4)
C6 C5 C4 121.6(4)
N3 C7 C4 178.5(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
S1 N1 1.640(4)
S1 S2 2.079(3)
S2 N2 1.636(4)
F2 C2 1.335(5)
F3 C3 1.332(5)
F6 C6 1.339(5)
F5 C5 1.331(5)
N1 C0 1.328(5)
N2 C0 1.327(6)
C1 C6 1.389(6)
C1 C2 1.410(6)
C1 C0 1.486(5)
C3 C2 1.376(6)
C3 C4 1.401(6)
C4 C5 1.401(6)
C4 C7 1.429(6)
C6 C5 1.378(6)
N3 C7 1.140(6)
