#------------------------------------------------------------------------------
#$Date: 2016-03-21 16:24:09 +0100 (lun 21 de mar de 2016) $
#$Revision: 178781 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/35/4103516.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_4103516
loop_
_publ_author_name
'Kristina Lekin'
'Stephen M. Winter'
'Laura E. Downie'
'Xuezhao Bao'
'John S. Tse'
'Serge Desgreniers'
'Richard A. Secco'
'Paul A. Dube'
'Richard T. Oakley'
_publ_section_title
;
 Hysteretic Spin Crossover between a Bisdithiazolyl Radical and Its
 Hypervalent σ-Dimer
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16212
_journal_page_last               16224
_journal_paper_doi               10.1021/ja106768z
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C7 H5 F N3 S4'
_chemical_formula_weight         278.38
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           113
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2ab'
_symmetry_space_group_name_H-M   'P -4 21 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.8542(7)
_cell_length_b                   15.8542(7)
_cell_length_c                   4.1273(3)
_cell_measurement_reflns_used    2225
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.87
_cell_volume                     1037.42(10)
_computing_cell_refinement       ApexII
_computing_data_collection       ApexII
_computing_data_reduction        ApexII
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            5066
_diffrn_reflns_theta_full        26.35
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    0.895
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.495
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         1095
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0313P)²+0.4428P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0730
_reflns_number_gt                1051
_reflns_number_total             1095
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja106768z_si_002.cif
_cod_data_source_block           fbpet_0m
_cod_database_code               4103516
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
S1 S 0.10494(4) 0.93362(4) 0.7631(2) 0.0400(2) Uani 1 1 d .
S2 S 0.22007(5) 0.96589(4) 0.5406(2) 0.0433(2) Uani 1 1 d .
N2 N 0.23849(13) 0.73849(13) 0.9363(8) 0.0301(7) Uani 1 2 d S
C1 C 0.20885(16) 0.81652(15) 0.8339(6) 0.0286(6) Uani 1 1 d .
C3 C 0.34277(16) 0.84277(16) 0.5641(11) 0.0352(9) Uani 1 2 d S
F1 F 0.39544(12) 0.89544(12) 0.3831(7) 0.0541(7) Uani 1 2 d S
N1 N 0.13262(14) 0.83994(14) 0.9072(7) 0.0346(6) Uani 1 1 d .
C4 C 0.18518(17) 0.68518(17) 1.1409(10) 0.0340(9) Uani 1 2 d S
H4B H 0.1516 0.7208 1.2780 0.041 Uiso 1 1 d R
C2 C 0.26320(16) 0.86986(16) 0.6489(7) 0.0313(6) Uani 1 1 d .
C5 C 0.12748(18) 0.62748(18) 0.9561(12) 0.0478(11) Uani 1 2 d S
H5A H 0.0945 0.5945 1.1044 0.072 Uiso 1 2 d SR
H5B H 0.0906 0.6602 0.8221 0.072 Uiso 1 1 d R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0317(3) 0.0306(3) 0.0577(4) -0.0015(3) 0.0000(4) 0.0046(3)
S2 0.0402(4) 0.0280(3) 0.0616(5) 0.0075(3) 0.0036(4) 0.0028(3)
N2 0.0280(9) 0.0280(9) 0.0345(17) 0.0015(10) 0.0015(10) -0.0012(12)
C1 0.0296(13) 0.0246(12) 0.0316(15) -0.0043(10) -0.0023(10) -0.0007(10)
C3 0.0312(12) 0.0312(12) 0.043(2) 0.0045(12) 0.0045(12) -0.0038(15)
F1 0.0474(9) 0.0474(9) 0.0674(17) 0.0152(9) 0.0152(9) 0.0068(12)
N1 0.0286(11) 0.0293(11) 0.0460(15) -0.0014(10) 0.0023(10) 0.0017(9)
C4 0.0353(12) 0.0353(12) 0.0315(19) 0.0063(11) 0.0063(11) -0.0006(16)
C2 0.0312(13) 0.0244(12) 0.0383(15) -0.0002(10) 0.0011(11) 0.0007(10)
C5 0.0455(15) 0.0455(15) 0.052(3) 0.0032(14) 0.0032(14) -0.0160(19)
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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 S1 S2 98.31(9) . .
C2 S2 S1 90.92(10) . .
C1 N2 C1 120.6(3) 8_455 .
C1 N2 C4 119.64(16) 8_455 .
C1 N2 C4 119.64(16) . .
N1 C1 N2 119.9(2) . .
N1 C1 C2 121.1(2) . .
N2 C1 C2 119.1(2) . .
C2 C3 C2 120.4(4) . 8_455
C2 C3 F1 119.77(18) . .
C2 C3 F1 119.78(18) 8_455 .
C1 N1 S1 114.72(19) . .
N2 C4 C5 114.2(4) . .
C3 C2 C1 120.2(3) . .
C3 C2 S2 124.9(2) . .
C1 C2 S2 114.91(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 N1 1.659(2) .
S1 S2 2.1064(11) .
S2 C2 1.728(3) .
N2 C1 1.389(3) 8_455
N2 C1 1.389(3) .
N2 C4 1.463(5) .
C1 N1 1.300(3) .
C1 C2 1.428(4) .
C3 C2 1.378(3) .
C3 C2 1.378(3) 8_455
C3 F1 1.398(4) .
C4 C5 1.502(6) .
