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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/4/12/53/4125398.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_4125398
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     direct
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                65.799(3)
_cell_angle_beta                 69.047(4)
_cell_angle_gamma                67.515(3)
_cell_formula_units_Z            2
_cell_length_a                   7.5808(7)
_cell_length_b                   8.0566(7)
_cell_length_c                   9.5091(9)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.59
_cell_measurement_theta_min      2.99
_cell_volume                     475.36(8)
_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-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.992
_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            15325
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.994
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.944
_exptl_crystal_description       block
_exptl_crystal_F_000             274
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.138
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2176
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0628
_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)+5.3156P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1833
_refine_ls_wR_factor_ref         0.1865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1987
_reflns_number_total             2176
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b10707_si_001.cif
_cod_data_source_block           YBalpha_minus100C
_cod_database_code               4125398
_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   0.818
_shelx_estimated_absorpt_t_max   0.932
_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
C0 C 0.9514(7) 0.9491(7) 0.7873(6) 0.0159(9) Uani 1 1 d
S1 S 1.2362(2) 1.02058(19) 0.56243(17) 0.0224(3) Uani 1 1 d
C1 C 0.8324(7) 0.8259(7) 0.9167(6) 0.0154(9) Uani 1 1 d
N1 N 1.1183(7) 0.8694(6) 0.6996(5) 0.0212(9) Uani 1 1 d
S2 S 1.0292(2) 1.25561(19) 0.62296(18) 0.0261(4) Uani 1 1 d
F2 F 0.7179(5) 1.0190(4) 1.0799(4) 0.0232(7) Uani 1 1 d
N2 N 0.8848(7) 1.1340(6) 0.7654(6) 0.0221(10) Uani 1 1 d
C2 C 0.7200(8) 0.8667(7) 1.0553(6) 0.0178(10) Uani 1 1 d
F3 F 0.5051(5) 0.7982(5) 1.3059(4) 0.0271(8) Uani 1 1 d
C3 C 0.6086(8) 0.7518(7) 1.1752(6) 0.0182(10) Uani 1 1 d
C4 C 0.6021(7) 0.5899(7) 1.1602(6) 0.0172(10) Uani 1 1 d
F5 F 0.7117(5) 0.3941(4) 1.0006(4) 0.0240(7) Uani 1 1 d
C5 C 0.7135(7) 0.5472(7) 1.0202(6) 0.0147(9) Uani 1 1 d
F6 F 0.9297(5) 0.6085(5) 0.7736(4) 0.0236(7) Uani 1 1 d
C6 C 0.8264(7) 0.6605(7) 0.9032(6) 0.0164(10) Uani 1 1 d
C7 C 0.4809(8) 0.4741(7) 1.2791(6) 0.0206(11) Uani 1 1 d
N3 N 0.3824(7) 0.3807(7) 1.3714(6) 0.0273(11) 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
N2 C0 N1 123.5(5)
N2 C0 C1 117.8(4)
N1 C0 C1 118.7(4)
N1 S1 S2 94.38(18)
C2 C1 C6 116.3(4)
C2 C1 C0 122.5(5)
C6 C1 C0 121.2(4)
C0 N1 S1 113.7(4)
N2 S2 S1 94.59(17)
C0 N2 S2 113.8(4)
F2 C2 C1 120.7(4)
F2 C2 C3 117.1(5)
C1 C2 C3 122.2(5)
F3 C3 C2 119.3(5)
F3 C3 C4 119.6(5)
C2 C3 C4 121.2(5)
C3 C4 C5 117.4(5)
C3 C4 C7 122.1(5)
C5 C4 C7 120.4(5)
F5 C5 C6 119.5(4)
F5 C5 C4 119.5(4)
C6 C5 C4 120.9(5)
F6 C6 C5 117.1(4)
F6 C6 C1 120.9(4)
C5 C6 C1 122.0(5)
N3 C7 C4 178.2(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C0 N2 1.328(7)
C0 N1 1.331(7)
C0 C1 1.485(7)
S1 N1 1.637(5)
S1 S2 2.0866(19)
C1 C2 1.382(7)
C1 C6 1.408(7)
S2 N2 1.632(5)
F2 C2 1.333(6)
C2 C3 1.384(7)
F3 C3 1.327(6)
C3 C4 1.389(7)
C4 C5 1.398(7)
C4 C7 1.429(7)
F5 C5 1.327(6)
C5 C6 1.375(7)
F6 C6 1.338(6)
C7 N3 1.146(7)
