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#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/21/1552125.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_1552125
loop_
_publ_author_name
'Leckie, Dominique'
'Stephaniuk, Nadia T.'
'Arauzo, Ana'
'Campo, Javier'
'Rawson, Jeremy M.'
_publ_section_title
;
 Exploring through-bond and through-space magnetic communication in
 1,3,2-dithiazolyl radical complexes
;
_journal_issue                   66
_journal_name_full               'Chemical Communications'
_journal_page_first              9849
_journal_page_last               9852
_journal_paper_doi               10.1039/C9CC04271G
_journal_volume                  55
_journal_year                    2019
_chemical_formula_moiety         'C24 H14 F12 N2 O4 S4 Zn'
_chemical_formula_sum            'C24 H14 F12 N2 O4 S4 Zn'
_chemical_formula_weight         815.98
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-05-07 deposited with the CCDC.    2019-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                99.800(3)
_cell_angle_beta                 97.782(2)
_cell_angle_gamma                91.947(2)
_cell_formula_units_Z            1
_cell_length_a                   8.4587(4)
_cell_length_b                   8.5811(5)
_cell_length_c                   10.6424(5)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.46
_cell_measurement_theta_min      2.41
_cell_volume                     752.91(7)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19983
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.962
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    1.203
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_description       plate
_exptl_crystal_F_000             406
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method Sublimation
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.803
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3441
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0345P)²+1.4642P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1033
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3118
_reflns_number_total             3441
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc04271g2.cif
_cod_data_source_block           JMR_DL055_0m_a
_cod_database_code               1552125
_shelx_shelxl_version_number     2014/7
_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   0.804
_shelx_estimated_absorpt_t_max   0.931
_exptl_absorpt_special_details
;
SADABS 2014/5 Bruker AXS Madison WI USA
;
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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.5000 0.5000 0.5000 0.02122(13) Uani 1 2 d S . P . .
S11 S 0.33170(8) 0.62131(9) 0.22519(7) 0.02800(18) Uani 1 1 d . . . . .
N11 N 0.3071(3) 0.5446(3) 0.3550(3) 0.0315(6) Uani 1 1 d . . . . .
C11 C 0.1310(3) 0.6456(3) 0.1719(3) 0.0223(6) Uani 1 1 d . . . . .
S12 S 0.11890(9) 0.51086(10) 0.37576(7) 0.02967(18) Uani 1 1 d . . . . .
C12 C 0.0749(4) 0.7149(3) 0.0671(3) 0.0271(6) Uani 1 1 d . . . . .
H12 H 0.1476 0.7526 0.0169 0.033 Uiso 1 1 calc R U . . .
C13 C -0.0886(4) 0.7287(4) 0.0361(3) 0.0291(6) Uani 1 1 d . . . . .
C14 C -0.1934(4) 0.6697(4) 0.1113(3) 0.0313(7) Uani 1 1 d . . . . .
H14 H -0.3052 0.6775 0.0895 0.038 Uiso 1 1 calc R U . . .
C15 C -0.1387(4) 0.6012(4) 0.2152(3) 0.0292(6) Uani 1 1 d . . . . .
H15 H -0.2114 0.5623 0.2648 0.035 Uiso 1 1 calc R U . . .
C16 C 0.0254(3) 0.5896(3) 0.2467(3) 0.0239(6) Uani 1 1 d . . . . .
C17 C -0.1532(4) 0.8066(4) -0.0755(3) 0.0396(8) Uani 1 1 d . . . . .
H17A H -0.0662 0.8290 -0.1232 0.059 Uiso 1 1 calc R U . . .
H17B H -0.1998 0.9059 -0.0429 0.059 Uiso 1 1 calc R U . . .
H17C H -0.2357 0.7356 -0.1330 0.059 Uiso 1 1 calc R U . . .
O21 O 0.3662(2) 0.3087(2) 0.52546(19) 0.0243(4) Uani 1 1 d . . . . .
C21 C 0.2146(3) 0.0687(3) 0.4758(3) 0.0290(6) Uani 1 1 d D . . . .
F21 F 0.0755(6) 0.1456(7) 0.4662(6) 0.0254(4) Uiso 0.383(3) 1 d D . P A 1
F22 F 0.2434(6) 0.0588(8) 0.6081(5) 0.0254(4) Uiso 0.383(3) 1 d D . P A 1
F23 F 0.1975(6) -0.0710(6) 0.4072(5) 0.0254(4) Uiso 0.383(3) 1 d D . P A 1
F21A F 0.0781(5) 0.1065(6) 0.4214(6) 0.0254(4) Uiso 0.404(3) 1 d D . P A 2
F22A F 0.2098(7) 0.0770(7) 0.6011(5) 0.0254(4) Uiso 0.404(3) 1 d D . P A 2
F23A F 0.2417(7) -0.0877(5) 0.4352(5) 0.0254(4) Uiso 0.404(3) 1 d D . P A 2
F21B F 0.0968(15) 0.0593(18) 0.3689(11) 0.0254(4) Uiso 0.121(3) 1 d D . P A 3
F22B F 0.1518(18) 0.1186(16) 0.5798(11) 0.0254(4) Uiso 0.121(3) 1 d D . P A 3
F23B F 0.2509(18) -0.0834(12) 0.4733(14) 0.0254(4) Uiso 0.121(3) 1 d D . P A 3
F21C F 0.140(2) -0.028(2) 0.3534(18) 0.0254(4) Uiso 0.092(2) 1 d . . P A 4
F22C F 0.230(2) 0.002(2) 0.555(2) 0.0254(4) Uiso 0.092(2) 1 d . . P A 4
F23C F 0.093(2) 0.143(2) 0.511(2) 0.0254(4) Uiso 0.092(2) 1 d . . P A 4
O22 O 0.6005(2) 0.3581(2) 0.35840(19) 0.0251(4) Uani 1 1 d . . . . .
C22 C 0.3507(3) 0.1786(3) 0.4504(3) 0.0209(5) Uani 1 1 d . . . . .
C23 C 0.4329(3) 0.1251(3) 0.3484(3) 0.0230(6) Uani 1 1 d . . . . .
H23 H 0.4085 0.0203 0.3021 0.028 Uiso 1 1 calc R U . . .
C24 C 0.5500(3) 0.2193(3) 0.3111(2) 0.0201(5) Uani 1 1 d . . . . .
F25 F 0.5843(3) -0.0013(2) 0.1462(2) 0.0502(6) Uani 1 1 d . . . . .
C25 C 0.6274(4) 0.1500(4) 0.1925(3) 0.0298(6) Uani 1 1 d . . . . .
F26 F 0.7861(2) 0.1635(3) 0.2193(2) 0.0447(5) Uani 1 1 d . . . . .
F27 F 0.5874(3) 0.2308(3) 0.09717(17) 0.0430(5) 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'
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'
O O 0.0106 0.0060 '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'
Zn Zn 0.2839 1.4301 '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
O21 Zn1 O21 180.0 . 2_666
O21 Zn1 O22 89.97(7) . .
O21 Zn1 O22 90.03(7) 2_666 .
O21 Zn1 O22 90.03(7) . 2_666
O21 Zn1 O22 89.97(7) 2_666 2_666
O22 Zn1 O22 180.0 . 2_666
O21 Zn1 N11 88.73(9) . .
O21 Zn1 N11 91.27(9) 2_666 .
O22 Zn1 N11 89.78(9) . .
O22 Zn1 N11 90.22(9) 2_666 .
O21 Zn1 N11 91.27(9) . 2_666
O21 Zn1 N11 88.73(9) 2_666 2_666
O22 Zn1 N11 90.22(9) . 2_666
O22 Zn1 N11 89.78(9) 2_666 2_666
N11 Zn1 N11 180.0 . 2_666
N11 S11 C11 98.20(13) . .
S12 N11 S11 115.50(16) . .
S12 N11 Zn1 119.40(13) . .
S11 N11 Zn1 125.01(13) . .
C12 C11 C16 120.9(3) . .
C12 C11 S11 125.4(2) . .
C16 C11 S11 113.7(2) . .
N11 S12 C16 98.41(13) . .
C11 C12 C13 119.5(3) . .
C11 C12 H12 120.2 . .
C13 C12 H12 120.2 . .
C12 C13 C14 118.9(3) . .
C12 C13 C17 120.8(3) . .
C14 C13 C17 120.3(3) . .
C15 C14 C13 121.9(3) . .
C15 C14 H14 119.1 . .
C13 C14 H14 119.1 . .
C14 C15 C16 118.9(3) . .
C14 C15 H15 120.6 . .
C16 C15 H15 120.6 . .
C15 C16 C11 119.9(3) . .
C15 C16 S12 126.1(2) . .
C11 C16 S12 114.0(2) . .
C13 C17 H17A 109.5 . .
C13 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C13 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C22 O21 Zn1 124.03(17) . .
F22C C21 F23C 95.9(14) . .
F21A C21 F22A 109.0(4) . .
F22B C21 F23B 109.3(8) . .
F23 C21 F21 111.6(4) . .
F21A C21 F23A 111.8(4) . .
F22A C21 F23A 103.2(4) . .
F22B C21 F21B 108.7(8) . .
F23B C21 F21B 103.0(7) . .
F23 C21 F22 110.1(4) . .
F21 C21 F22 102.8(3) . .
F22C C21 F21C 113.2(13) . .
F23C C21 F21C 100.1(12) . .
C21 F22C F23C 46.2(10) . .
C21 F23C F22C 37.9(8) . .
C24 O22 Zn1 123.50(17) . .
O21 C22 C23 129.4(2) . .
O21 C22 C21 112.6(2) . .
C23 C22 C21 117.9(2) . .
C22 C23 C24 122.6(3) . .
C22 C23 H23 118.7 . .
C24 C23 H23 118.7 . .
O22 C24 C23 129.2(2) . .
O22 C24 C25 112.9(2) . .
C23 C24 C25 117.9(2) . .
F25 C25 F26 108.0(3) . .
F25 C25 F27 107.1(3) . .
F26 C25 F27 106.7(2) . .
F25 C25 C24 113.9(2) . .
F26 C25 C24 110.9(2) . .
F27 C25 C24 109.9(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O21 2.0391(18) .
Zn1 O21 2.0391(18) 2_666
Zn1 O22 2.0661(19) .
Zn1 O22 2.0661(19) 2_666
Zn1 N11 2.180(3) .
Zn1 N11 2.180(3) 2_666
S11 N11 1.662(3) .
S11 C11 1.747(3) .
N11 S12 1.659(3) .
C11 C12 1.387(4) .
C11 C16 1.398(4) .
S12 C16 1.739(3) .
C12 C13 1.392(4) .
C12 H12 0.9500 .
C13 C14 1.408(4) .
C13 C17 1.508(5) .
C14 C15 1.373(5) .
C14 H14 0.9500 .
C15 C16 1.394(4) .
C15 H15 0.9500 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
O21 C22 1.249(3) .
C21 F22C 1.095(19) .
C21 F23 1.286(5) .
C21 F23C 1.29(2) .
C21 F21A 1.298(5) .
C21 F22B 1.305(8) .
C21 F22A 1.329(5) .
C21 F23B 1.347(8) .
C21 F21 1.369(5) .
C21 F23A 1.375(5) .
C21 F21B 1.397(8) .
C21 F22 1.413(6) .
C21 F21C 1.469(19) .
F22C F23C 1.77(3) .
O22 C24 1.248(3) .
C22 C23 1.389(4) .
C23 C24 1.398(4) .
C23 H23 0.9500 .
C24 C25 1.540(4) .
F25 C25 1.327(4) .
C25 F26 1.331(4) .
C25 F27 1.337(4) .
