#------------------------------------------------------------------------------
#$Date: 2021-11-06 19:48:07 +0100 (Sat 06 de Nov de 2021) $
#$Revision: 270360 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/89/7128970.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_7128970
loop_
_publ_author_name
'Robertson, Craig M.'
'Winter, Stephen M.'
'Howard, Judith A. K.'
'Probert, Michael R.'
'Oakley, Richard T.'
_publ_section_title
;
 Low temperature insights into the crystal and magnetic structure of a
 neutral radical ferromagnet.
;
_journal_issue                   79
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10238
_journal_page_last               10241
_journal_paper_doi               10.1039/d1cc03842g
_journal_volume                  57
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C7 H5 Cl N3 Se4'
_chemical_formula_sum            'C7 H5 Cl N3 Se4'
_chemical_formula_weight         482.43
_space_group_crystal_system      tetragonal
_space_group_IT_number           113
_space_group_name_Hall           'P -4 2ab'
_space_group_name_H-M_alt        'P -4 21 m'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2021-01-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-14 deposited with the CCDC.	2021-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1915(4)
_cell_length_b                   16.1915(4)
_cell_length_c                   4.07570(10)
_cell_measurement_reflns_used    6541
_cell_measurement_temperature    1.85
_cell_measurement_theta_max      30.18
_cell_measurement_theta_min      2.52
_cell_volume                     1068.50(5)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      1.85
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            16949
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.461
_diffrn_reflns_theta_min         1.779
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.949
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6352
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.999
_exptl_crystal_description       needle
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.152
_refine_ls_abs_structure_details
;
 Flack x determined using 552 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.046(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         1663
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0187P)²+0.5141P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0408
_refine_ls_wR_factor_ref         0.0431
_reflns_Friedel_coverage         0.668
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.962
_reflns_number_gt                1484
_reflns_number_total             1663
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cc03842g2.cif
_cod_data_source_block           'data_2ka_0m'
_cod_depositor_comments          'Adding full bibliography for 7128970.cif.'
_cod_original_cell_volume        1068.50(6)
_cod_database_code               7128970
_shelx_shelxl_version_number     2018/3
_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_max   0.442
_shelx_estimated_absorpt_t_min   0.128
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Riding coordinates:
 C3(H3)
;
_shelx_res_file
;
TITL data_2KA_0m in P-42(1)m
    data_2ka_0m.res
    created by SHELXL-2018/3 at 11:22:15 on 22-Jan-2021
CELL 0.71073 16.1915 16.1915 4.0757 90 90 90
ZERR 4 0.0004 0.0004 0.0001 0 0 0
LATT -1
SYMM -X,-Y,+Z
SYMM +Y,-X,-Z
SYMM -Y,+X,-Z
SYMM 0.5-X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,-Z
SYMM 0.5-Y,0.5-X,+Z
SYMM 0.5+Y,0.5+X,+Z
SFAC C H Cl N Se
UNIT 28 20 4 12 16

L.S. 50
PLAN  2
SIZE 0.25 0.075 0.07
TEMP -271.15
BOND
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\data_2KA_0m.hkl">
REM </olex2.extras>

WGHT    0.018700    0.514100
FVAR       0.09694
SE1   5    0.940678    0.102396    0.260041    11.00000    0.00595    0.00571 =
         0.00589    0.00026    0.00024    0.00031
SE2   5    0.978838    0.229332    0.016428    11.00000    0.00604    0.00645 =
         0.00639    0.00064    0.00033    0.00016
CL1   3    0.915704    0.415704   -0.134946    10.50000    0.00743    0.00743 =
         0.00823    0.00187    0.00187   -0.00033
N1    4    0.841100    0.139765    0.412382    11.00000    0.00749    0.00703 =
         0.00312    0.00054    0.00211    0.00137
C2    1    0.823454    0.216546    0.336563    11.00000    0.00726    0.00786 =
         0.00231   -0.00119   -0.00030    0.00022
N2    4    0.747921    0.247921    0.443710    10.50000    0.00729    0.00729 =
         0.00386    0.00079    0.00079   -0.00098
C1    1    0.876200    0.271280    0.153462    11.00000    0.00391    0.01131 =
         0.00745   -0.00300   -0.00096    0.00120
C3    1    0.696242    0.196242    0.661359    10.50000    0.00824    0.00824 =
         0.00826    0.00199    0.00199   -0.00079
AFIX   3
H3    2    0.733062    0.162350    0.801459    11.00000   -1.20000
AFIX   0
C0AA  1    0.849892    0.349892    0.077082    10.50000    0.00925    0.00925 =
         0.00672   -0.00202   -0.00202   -0.00095
C4    1    0.638421    0.138421    0.476347    10.50000    0.01016    0.01016 =
         0.01040    0.00165    0.00165   -0.00058
H4A   2    0.667729    0.101421    0.327711    11.00000    0.01597
H4B   2    0.610087    0.110087    0.638182    10.50000    0.02476
HKLF 4




REM  data_2KA_0m in P-42(1)m
REM wR2 = 0.043059, GooF = S = 1.04930, Restrained GooF = 1.04930 for all data
REM R1 = 0.025178 for 1484 Fo > 4sig(Fo) and 0.035753 for all 1663 data
REM 83 parameters refined using 0 restraints

END

WGHT      0.0187      0.5139

REM Highest difference peak  0.691,  deepest hole -0.651,  1-sigma level  0.152
Q1    1   0.7812  0.2310  0.8556  11.00000  0.05    0.69
Q2    1   0.8882  0.3882 -0.1465  10.50000  0.05    0.64
;
_shelx_res_checksum              84443
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_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_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
Se1 Se 0.94068(2) 0.10240(2) 0.26004(13) 0.00585(10) Uani 1 1 d . . . . .
Se2 Se 0.97884(3) 0.22933(2) 0.01643(13) 0.00629(10) Uani 1 1 d . . . . .
Cl1 Cl 0.91570(6) 0.41570(6) -0.1349(4) 0.0077(3) Uani 1 2 d S T P . .
N1 N 0.8411(2) 0.1398(2) 0.4124(10) 0.0059(8) Uani 1 1 d . . . . .
C2 C 0.8235(3) 0.2165(3) 0.3366(11) 0.0058(9) Uani 1 1 d . . . . .
N2 N 0.7479(2) 0.2479(2) 0.4437(15) 0.0061(12) Uani 1 2 d S T P . .
C1 C 0.8762(3) 0.2713(3) 0.1535(12) 0.0076(9) Uani 1 1 d . . . . .
C3 C 0.6962(3) 0.1962(3) 0.6614(17) 0.0083(14) Uani 1 2 d S T P . .
H3 H 0.733062 0.162350 0.801459 0.010 Uiso 1 1 d R . . . .
C0AA C 0.8499(3) 0.3499(3) 0.0771(17) 0.0084(14) Uani 1 2 d S T P . .
C4 C 0.6384(3) 0.1384(3) 0.476(2) 0.0102(13) Uani 1 2 d S T P . .
H4A H 0.668(3) 0.101(3) 0.328(16) 0.016(15) Uiso 1 1 d . . . . .
H4B H 0.610(3) 0.110(3) 0.64(2) 0.02(2) Uiso 1 2 d S T P . .
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
Se1 0.00595(18) 0.00571(18) 0.0059(2) 0.0003(2) 0.0002(2) 0.00031(15)
Se2 0.00604(19) 0.00645(19) 0.0064(2) 0.0006(2) 0.00033(19) 0.00016(15)
Cl1 0.0074(4) 0.0074(4) 0.0082(8) 0.0019(4) 0.0019(4) -0.0003(5)
N1 0.0075(18) 0.0070(17) 0.003(2) 0.0005(15) 0.0021(15) 0.0014(14)
C2 0.007(2) 0.008(2) 0.002(2) -0.0012(16) -0.0003(16) 0.0002(16)
N2 0.0073(15) 0.0073(15) 0.004(3) 0.0008(14) 0.0008(14) -0.0010(18)
C1 0.0039(19) 0.011(2) 0.007(2) -0.0030(18) -0.0010(16) 0.0012(16)
C3 0.0082(18) 0.0082(18) 0.008(4) 0.0020(17) 0.0020(17) -0.001(2)
C0AA 0.0093(18) 0.0093(18) 0.007(4) -0.0020(18) -0.0020(18) -0.001(2)
C4 0.0102(18) 0.0102(18) 0.010(4) 0.002(2) 0.002(2) -0.001(2)
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'
Cl Cl 0.1484 0.1585 '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'
Se Se -0.0929 2.2259 '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
_geom_angle_publ_flag
N1 Se1 Se2 94.89(11) . . ?
C1 Se2 Se1 87.61(15) . . ?
C2 N1 Se1 115.1(3) . . ?
N1 C2 N2 117.5(4) . . ?
N1 C2 C1 125.2(4) . . ?
N2 C2 C1 117.3(4) . . ?
C2 N2 C2 122.7(6) 8_545 . ?
C2 N2 C3 118.6(3) 8_545 . ?
C2 N2 C3 118.6(3) . . ?
C2 C1 Se2 117.1(3) . . ?
C0AA C1 Se2 122.7(4) . . ?
C0AA C1 C2 120.2(5) . . ?
N2 C3 C4 113.5(6) . . ?
C1 C0AA Cl1 119.3(3) 8_545 . ?
C1 C0AA Cl1 119.3(3) . . ?
C1 C0AA C1 121.3(6) . 8_545 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Se1 Se2 2.3647(6) . ?
Se1 N1 1.831(4) . ?
Se2 C1 1.880(4) . ?
Cl1 C0AA 1.737(7) . ?
N1 C2 1.313(6) . ?
C2 N2 1.394(5) . ?
C2 C1 1.439(6) . ?
N2 C3 1.479(8) . ?
C1 C0AA 1.378(6) . ?
C3 C4 1.524(9) . ?
