#------------------------------------------------------------------------------
#$Date: 2024-01-06 10:51:33 +0100 (Sat 06 de Jan de 2024) $
#$Revision: 288902 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/76/7247680.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_7247680
loop_
_publ_author_name
'Gebbia, Jonathan F.'
'Aristizabal, Andrés Henao'
'Negrier, Philippe'
'Aguilà, David'
'Tamarit, Josep Lluis'
'Pardo, Luis Carlos'
_publ_section_title
;
 Dynamics and local ordering of pentachloronitrobenzene: a
 molecular-dynamics investigation.
;
_journal_issue                   44
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              30553
_journal_page_last               30562
_journal_paper_doi               10.1039/d3cp02633g
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C6 Cl5 N1 O2'
_chemical_formula_sum            'C6 Cl5 N O2'
_chemical_formula_weight         295.32
_chemical_name_systematic        Pentachloronitrobenzene
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-09
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-05-30 deposited with the CCDC.	2023-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   8.7440(12)
_cell_length_b                   8.7440(12)
_cell_length_c                   11.068(2)
_cell_measurement_reflns_used    1859
_cell_measurement_temperature    200.15
_cell_measurement_theta_max      33.7
_cell_measurement_theta_min      2.76
_cell_volume                     732.86(19)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      200.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.72931
_diffrn_reflns_av_R_equivalents  0.1362
_diffrn_reflns_av_unetI/netI     0.2130
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4573
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.950
_diffrn_reflns_theta_max         31.391
_diffrn_reflns_theta_min         3.345
_diffrn_source                   'ALBA XALOC beamline'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.549
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.007
_exptl_crystal_description       plate
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         495
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      0.878
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0543
_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/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                382
_reflns_number_total             495
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3cp02633g2.cif
_cod_data_source_block           hexa200
_cod_depositor_comments
'Adding full bibliography for 7247679--7247680.cif.'
_cod_original_cell_volume        732.9(2)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7247680
_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   0.970
_shelx_estimated_absorpt_t_min   0.927
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.286(4)
 0.714(4)
2. Restrained distances
 O1-N1
 1.25 with sigma of 0.01
 O2-N1
 1.25 with sigma of 0.01
3. Rigid bond restraints
 C1, N1
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
4. Uiso/Uaniso restraints and constraints
C1 \\sim N1: within 2A with sigma of 0.012 and sigma for terminal atoms of
0.024 within 2A
5. Rigid body (RIGU) restrains
 C1, N1, O1, O2, Cl1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: Cl1(0.83333) N1(0.16666) O1(0.16666) O2(0.16666)
;
_shelx_res_file
;
TITL hexa200_b.res in R3
    hexa200.res
    created by SHELXL-2018/3 at 08:29:43 on 09-Nov-2022
REM Old TITL hexa200 in R-3
REM SHELXT solution in R3: R1 0.415, Rweak 0.000, Alpha 0.040
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Flack x = 0.329 ( 0.205 ) from 252 Parsons' quotients
REM Formula found by SHELXT: C2 N O Cl2
CELL 0.72931 8.744 8.744 11.068 90 90 120
ZERR 3 0.0012 0.0012 0.0022 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C Cl N O
DISP C 0.0024 0.0017 12.0603
DISP Cl 0.1386 0.1675 724.1588
DISP N 0.0046 0.0035 20.6952
DISP O 0.0086 0.0064 34.4758
UNIT 18 15 3 6
DFIX 1.25 0.01 O1 N1
DFIX 1.25 0.01 O2 N1
RIGU C1 N1 O1 O2 Cl1
SIMU 0.012 0.024 2 C1 N1
DELU 0.003 0.003 C1 N1

L.S. 20
PLAN  58
SIZE 0.05 0.02 0.02
TEMP -73
CONF
LIST 4
MORE -1
fmap 2
acta 51.9
MERG 2
SHEL 0.7 15
TWIN -1 0 0 0 -1 0 0 0 1 2
REM <olex2.extras>
REM <HklSrc "%.\\hexa200.hkl">
REM </olex2.extras>

WGHT    0.000000
BASF   0.71430
FVAR       0.47371
C1    1    0.180886    0.116204    0.499435    11.00000    0.02676    0.02992 =
         0.10138    0.00037   -0.00041    0.01234
PART 1
CL1   2    0.405609    0.260763    0.499943    10.83333    0.02546    0.03675 =
         0.16924    0.00021    0.00175    0.01171
PART -1
N1    3    0.369544    0.247995    0.498366    10.16666    0.01385    0.05810 =
         0.09153    0.00188   -0.00215    0.02173
O1    4    0.428073    0.285411    0.394355    10.16666    0.06666    0.10938 =
         0.08881   -0.00048    0.00465    0.00804
O2    4    0.444253    0.257760    0.593977    10.16666    0.08242    0.11472 =
         0.12552    0.01792   -0.05863    0.01268
HKLF 4




REM  hexa200_b.res in R3
REM wR2 = 0.1395, GooF = S = 0.882, Restrained GooF = 0.878 for all data
REM R1 = 0.0543 for 382 Fo > 4sig(Fo) and 0.0580 for all 495 data
REM 47 parameters refined using 29 restraints

END

WGHT      0.0000      0.0000

REM Highest difference peak  0.258,  deepest hole -0.380,  1-sigma level  0.091
Q1    1   0.1464  0.0268  0.5024  11.00000  0.05    0.26
Q2    1   0.6667  0.3333  0.6442  10.33333  0.05    0.24
Q3    1   0.3625  0.4083  0.4015  11.00000  0.05    0.19
Q4    1   0.4959  0.1490  0.6415  11.00000  0.05    0.19
Q5    1   0.3313  0.3556  0.3381  11.00000  0.05    0.19
Q6    1   0.6667  0.3333  0.3333  10.16667  0.05    0.18
Q7    1   0.4091  0.4519  0.3262  11.00000  0.05    0.18
Q8    1   0.5468  0.2555  0.6659  11.00000  0.05    0.17
Q9    1   0.2902  0.1640  0.4984  11.00000  0.05    0.17
Q10   1   0.5695  0.3168  0.3195  11.00000  0.05    0.17
Q11   1   0.2650  0.1716  0.3443  11.00000  0.05    0.17
Q12   1   0.2031  0.2322  0.6109  11.00000  0.05    0.14
Q13   1   0.3976  0.1529  0.4932  11.00000  0.05    0.14
Q14   1   0.4531  0.0841  0.5012  11.00000  0.05    0.13
Q15   1   0.4589  0.2200  0.6779  11.00000  0.05    0.13
Q16   1   0.3457  0.3210  0.6092  11.00000  0.05    0.13
Q17   1   0.3802  0.2068  0.3178  11.00000  0.05    0.12
Q18   1   0.5803  0.4738  0.5850  11.00000  0.05    0.12
Q19   1   0.3576  0.1249  0.6404  11.00000  0.05    0.12
Q20   1   0.6667  0.3333  0.5460  10.33333  0.05    0.12
Q21   1   0.2823  0.2244  0.4923  11.00000  0.05    0.12
Q22   1   0.4510  0.3245  0.3160  11.00000  0.05    0.11
Q23   1   0.5365  0.3684  0.6645  11.00000  0.05    0.10
Q24   1   0.1747  0.1313  0.4195  11.00000  0.05    0.10
Q25   1   0.4488  0.1905  0.3605  11.00000  0.05    0.08
Q26   1   0.4536  0.4476  0.4858  11.00000  0.05    0.07
Q27   1   0.4214  0.3202  0.6838  11.00000  0.05    0.06
Q28   1   0.3827  0.3705  0.5166  11.00000  0.05    0.05
Q29   1   0.5484  0.2056  0.4926  11.00000  0.05    0.04
Q30   1   0.5775  0.4102  0.4968  11.00000  0.05    0.03
Q31   1   0.0000  0.0000  0.5000  10.16667  0.05    0.02
Q32   1   0.5402  0.3851  0.5538  11.00000  0.05    0.02
Q33   1   0.5007  0.2657  0.4850  11.00000  0.05    0.01
;
_shelx_res_checksum              28297
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
C1 C 0.1809(2) 0.11620(18) 0.4994(2) 0.0535(5) Uani 1 1 d . U . . .
Cl1 Cl 0.40561(10) 0.26076(15) 0.49994(15) 0.0789(6) Uani 0.8333 1 d . . P A 1
N1 N 0.3695(17) 0.248(2) 0.4984(10) 0.053(3) Uani 0.1667 1 d D U P A -1
O1 O 0.4281(16) 0.285(2) 0.3944(11) 0.104(6) Uani 0.1667 1 d D . P A -1
O2 O 0.444(2) 0.258(2) 0.5940(17) 0.124(7) Uani 0.1667 1 d D . P A -1
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
C1 0.0268(7) 0.0299(8) 0.1014(13) 0.0004(7) -0.0004(6) 0.0123(6)
Cl1 0.0255(5) 0.0367(5) 0.1692(13) 0.0002(4) 0.0017(4) 0.0117(3)
N1 0.014(3) 0.058(6) 0.092(5) 0.002(5) -0.002(3) 0.022(3)
O1 0.067(7) 0.109(12) 0.089(6) 0.000(5) 0.005(5) 0.008(6)
O2 0.082(9) 0.115(11) 0.126(9) 0.018(7) -0.059(8) 0.013(8)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0024 0.0017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1386 0.1675 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0046 0.0035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0086 0.0064 '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
C1 C1 C1 119.994(7) 11_556 12_556 ?
C1 C1 Cl1 119.94(11) 12_556 . ?
C1 C1 Cl1 120.05(11) 11_556 . ?
C1 C1 N1 123.6(8) 11_556 . ?
C1 C1 N1 116.4(8) 12_556 . ?
N1 C1 Cl1 3.6(8) . . ?
O1 Cl1 C1 98.9(6) . . ?
O2 Cl1 C1 103.7(9) . . ?
O2 Cl1 O1 155.8(12) . . ?
O1 N1 C1 111.7(11) . . ?
O2 N1 C1 113.5(12) . . ?
O2 N1 O1 130.6(19) . . ?
Cl1 O1 N1 13.0(7) . . ?
Cl1 O2 N1 12.3(7) . . ?
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
C1 C1 1.3882(15) 11_556 ?
C1 C1 1.3882(15) 12_556 ?
C1 Cl1 1.7249(17) . ?
C1 N1 1.466(13) . ?
Cl1 O1 1.187(12) . ?
Cl1 O2 1.099(13) . ?
N1 O1 1.236(10) . ?
N1 O2 1.224(9) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C1 Cl1 O1 95.0(9) 11_556 . . . ?
C1 C1 Cl1 O1 -86.4(10) 12_556 . . . ?
C1 C1 Cl1 O2 -76.3(15) 11_556 . . . ?
C1 C1 Cl1 O2 102.3(14) 12_556 . . . ?
C1 C1 N1 O1 88.8(16) 11_556 . . . ?
C1 C1 N1 O1 -91.8(17) 12_556 . . . ?
C1 C1 N1 O2 -71(2) 11_556 . . . ?
C1 C1 N1 O2 108(2) 12_556 . . . ?
C1 Cl1 O1 N1 19(4) . . . . ?
C1 Cl1 O2 N1 -19(5) . . . . ?
C1 N1 O1 Cl1 -156(6) . . . . ?
C1 N1 O2 Cl1 156(6) . . . . ?
Cl1 C1 N1 O1 99(9) . . . . ?
Cl1 C1 N1 O2 -61(8) . . . . ?
N1 C1 Cl1 O1 -75(8) . . . . ?
N1 C1 Cl1 O2 113(9) . . . . ?
O1 Cl1 O2 N1 -177(6) . . . . ?
O1 N1 O2 Cl1 1(3) . . . . ?
O2 Cl1 O1 N1 178(6) . . . . ?
O2 N1 O1 Cl1 -1(3) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.286(4)
2 0.714(4)
