Magnetic Bistability in Naphtho-1,3,2-dithiazolyl: Solid State Interconversion of a Thiazyl π-Radical and Its N-N σ-Bonded Dimer.
Bates, Demetris; Robertson, Craig M.; Leitch, Alicea A.; Dube, Paul A.; Oakley, Richard T.; Journal of the American Chemical Society 140 (2018) 3846–3849; doi:10.1021/jacs.7b13699

data_4131996
_publ_section_title
;
 Magnetic Bistability in Naphtho-1,3,2-dithiazolyl: Solid State
 Interconversion of a Thiazyl \p-Radical and Its N-N \s-Bonded Dimer.
;
_journal_issue                   11
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3846
_journal_page_last               3849
_journal_paper_doi               10.1021/jacs.7b13699
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         '1(C10 H6 N S2)'
_chemical_formula_sum            'C10 H6 N S2'
_chemical_formula_weight         204.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-12-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                77.104(11)
_cell_angle_beta                 86.491(11)
_cell_angle_gamma                75.335(11)
_cell_formula_units_Z            4
_cell_length_a                   9.431(4)
_cell_length_b                   9.479(4)
_cell_length_c                   10.550(5)
_cell_measurement_reflns_used    2368
_cell_measurement_temperature    225(2)
_cell_measurement_theta_max      26.06
_cell_measurement_theta_min      2.68
_cell_volume                     889.4(7)
_computing_cell_refinement       'SAINT V8.30C (?, 2016)'
_computing_data_reduction        'SAINT V8.30C (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      225
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku Micromax007HF'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0858
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9137
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.383
_diffrn_reflns_theta_min         1.980
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1038 before and 0.0708 after correction.
The Ratio of minimum to maximum transmission is 0.6319.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       irregular
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         3604
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1367
_refine_ls_R_factor_gt           0.0842
_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^)+(0.0860P)^2^+1.7854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2197
_refine_ls_wR_factor_ref         0.2509
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2170
_reflns_number_total             3604
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b13699_si_005.cif
_cod_data_source_block           HT-225_recovered
_cod_original_cell_volume        889.3(7)
_cod_database_code               4131996
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.855
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N1-S6
 1.6 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim
C29 \\sim C30: within 1.7A with sigma of 0.005 and sigma for terminal atoms of
0.08
C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim
C39 \\sim C40: within 1.7A with sigma of 0.005 and sigma for terminal atoms of
0.08
Uanis(S6) \\sim Ueq, Uanis(S5) \\sim Ueq: with sigma of 0.008 and sigma for
terminal atoms of 0.01
Uanis(N1) = Uanis(N3)
Uanis(N2) = Uanis(N4)
4. Others
 Sof(S8)=Sof(S7)=Sof(C32)=Sof(H32)=Sof(C31)=Sof(C40)=Sof(C39)=Sof(H39)=
 Sof(C38)=Sof(C33)=Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35)=Sof(C36)=Sof(H36)=
 Sof(C37)=Sof(H37)=Sof(N4)=1-FVAR(1)
 Sof(S3)=Sof(S4)=Sof(C13)=Sof(C18)=Sof(C11)=Sof(C20)=Sof(C12)=Sof(H12)=
 Sof(C19)=Sof(H19)=Sof(N2)=Sof(C17)=Sof(H17)=Sof(C16)=Sof(H16)=Sof(C14)=
 Sof(H14)=Sof(C15)=Sof(H15)=FVAR(1)
 Sof(S5)=Sof(S6)=Sof(C22)=Sof(H22)=Sof(C21)=Sof(C30)=Sof(C29)=Sof(H29)=
 Sof(C28)=Sof(C23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26)=
 Sof(C27)=Sof(H27)=Sof(N3)=1-FVAR(2)
 Sof(S2)=Sof(S1)=Sof(N1)=Sof(C10)=Sof(C3)=Sof(C8)=Sof(C1)=Sof(C2)=Sof(H2)=
 Sof(C9)=Sof(H9)=Sof(C4)=Sof(H4)=Sof(C7)=Sof(H7)=Sof(C5)=Sof(H5)=Sof(C6)=
 Sof(H6)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C9(H9), C4(H4), C12(H12), C19(H19), C7(H7), C17(H17), C5(H5), C6(H6),
 C16(H16), C14(H14), C15(H15), C22(H22), C29(H29), C24(H24), C25(H25), C26(H26),
  C27(H27), C32(H32), C39(H39), C34(H34), C35(H35), C36(H36), C37(H37)
5.b Naphthalene refined as free rotating group:
 C22(C21,C30,C29,C28,C23,C24,C25,C26,C27), C32(C31,C40,C39,C38,C33,C34,C35,C36,
 C37)
;
_shelx_res_checksum              51141
_shelx_hkl_checksum              32254
_olex2_submission_special_instructions 'No special instructions were received'