Studies on a "Disappearing Polymorph": Thermal and Magnetic Characterization of α-p-NCC6F4CNSSN(•).
Beldjoudi, Yassine; Arauzo, Ana; Palacio, Fernando; Pilkington, Melanie; Rawson, Jeremy M.; Journal of the American Chemical Society 138 (2016) 16779–16786; doi:10.1021/jacs.6b10707

data_4125398
_publ_section_title
;
 Studies on a &quot;Disappearing Polymorph&quot;: Thermal and Magnetic
 Characterization of \a-p-NCC6F4CNSSN(&#x2022;).
;
_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/[\s^2^(Fo^2^)+5.3156P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(I)'
_cod_data_source_file            ja6b10707_si_001.cif
_cod_data_source_block           YBalpha_minus100C
_cod_database_code               4125398
_shelx_estimated_absorpt_t_min   0.818
_shelx_estimated_absorpt_t_max   0.932
_shelxl_version_number           2013-3
_shelx_res_checksum              16203
_shelx_hkl_checksum              20647