#------------------------------------------------------------------------------ #$Date: 2024-01-06 11:51:33 +0200 (Sat, 06 Jan 2024) $ #$Revision: 288902 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247679.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_7247679 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' _audit_creation_date 2022-02-01 _audit_creation_method ; Olex2 1.5 (compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439) ; _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 8.7160(12) _cell_length_b 8.7160(12) _cell_length_c 10.946(2) _cell_measurement_reflns_used 1860 _cell_measurement_temperature 100.15 _cell_measurement_theta_max 33.5 _cell_measurement_theta_min 2.77 _cell_volume 720.15(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)' _diffrn_ambient_temperature 100.15 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device_type MD2M-Maatel _diffrn_measurement_method '\w scans' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.72931 _diffrn_reflns_av_R_equivalents 0.1108 _diffrn_reflns_av_unetI/netI 0.1274 _diffrn_reflns_Laue_measured_fraction_full 0.990 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 7351 _diffrn_reflns_point_group_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_theta_full 25.950 _diffrn_reflns_theta_max 31.245 _diffrn_reflns_theta_min 3.364 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.576 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 2.043 _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 0.456 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.075 _refine_ls_extinction_coef 0.09(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 48 _refine_ls_number_reflns 805 _refine_ls_number_restraints 22 _refine_ls_restrained_S_all 1.117 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0429 _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^)+0.0462P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1355 _refine_ls_wR_factor_ref 0.1371 _reflns_Friedel_coverage 0.000 _reflns_number_gt 759 _reflns_number_total 805 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3cp02633g2.cif _cod_data_source_block xprep _cod_depositor_comments 'Adding full bibliography for 7247679--7247680.cif.' _cod_original_cell_volume 720.1(2) _cod_original_sg_symbol_H-M 'R -3' _cod_database_code 7247679 _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 0.969 _shelx_estimated_absorpt_t_min 0.925 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.337(3) 0.663(3) 2. Restrained distances O1-N1 1.25 with sigma of 0.01 O2-N1 1.25 with sigma of 0.01 3. 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 4. Others Fixed Sof: Cl1(0.83333) N1(0.16666) O1(0.16666) O2(0.16666) ; _shelx_res_file ; TITL r3bar_a.res in R-3 xprep.res created by SHELXL-2018/3 at 11:10:15 on 01-Feb-2022 CELL 0.72931 8.716 8.716 10.946 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 L.S. 20 PLAN 5 SIZE 0.05 0.02 0.02 TEMP -173 CONF LIST 4 MORE -1 fmap 2 acta MERG 2 SHEL 0.7 15 TWIN -1 0 0 0 -1 0 0 0 1 2 REM REM REM WGHT 0.000000 0.046200 EXTI 0.090567 BASF 0.66277 FVAR 0.86724 C1 1 0.181477 0.116790 0.499931 11.00000 0.01977 0.02228 = 0.06736 -0.00006 0.00026 0.00923 PART 1 CL1 2 0.406815 0.263011 0.500366 10.83333 0.01852 0.02504 = 0.11691 -0.00027 0.00096 0.00878 PART -1 N1 3 0.369268 0.242033 0.496594 10.16666 0.01153 0.03926 = 0.06323 0.00833 0.00150 0.01205 O1 4 0.430689 0.294860 0.392527 10.16666 0.05276 0.07480 = 0.05363 0.00571 0.01125 0.00929 O2 4 0.448801 0.261528 0.590044 10.16666 0.04703 0.09763 = 0.07951 0.03043 -0.03544 -0.00254 HKLF 4 REM r3bar_a.res in R-3 REM wR2 = 0.1371, GooF = S = 1.107, Restrained GooF = 1.117 for all data REM R1 = 0.0429 for 759 Fo > 4sig(Fo) and 0.0435 for all 805 data REM 48 parameters refined using 22 restraints END WGHT 0.0000 0.0462 REM Highest difference peak 0.456, deepest hole -0.330, 1-sigma level 0.075 Q1 1 0.0000 0.0000 0.5000 10.16667 0.05 0.43 Q2 1 0.1208 0.1420 0.4964 11.00000 0.05 0.31 Q3 1 0.0000 0.0000 0.4109 10.33333 0.05 0.26 Q4 1 0.5725 0.5025 0.4411 11.00000 0.05 0.20 Q5 1 0.3557 0.4290 0.4895 11.00000 0.05 0.20 ; _shelx_res_checksum 25816 _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 0.18148(17) 0.11679(13) 0.49993(14) 0.0370(5) Uani 1 1 d . . . . . Cl1 Cl 0.40682(15) 0.26301(17) 0.50037(13) 0.0544(5) Uani 0.8333 1 d . . P A 1 N1 N 0.369(2) 0.242(3) 0.4966(11) 0.038(3) Uani 0.1667 1 d D . P A -1 O1 O 0.4307(11) 0.2949(13) 0.3925(8) 0.070(3) Uani 0.1667 1 d D . P A -1 O2 O 0.4488(14) 0.2615(18) 0.5900(11) 0.092(4) 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 0.0198(7) 0.0223(7) 0.0674(8) -0.0001(4) 0.0003(4) 0.0092(5) Cl1 0.0185(6) 0.0250(5) 0.1169(8) -0.0003(2) 0.0010(2) 0.0088(3) N1 0.012(6) 0.039(8) 0.063(5) 0.008(4) 0.001(3) 0.012(5) O1 0.053(5) 0.075(6) 0.054(3) 0.006(3) 0.011(3) 0.009(4) O2 0.047(5) 0.098(8) 0.080(5) 0.030(5) -0.035(4) -0.003(5) 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 120.000(1) 11_556 12_556 ? C1 C1 Cl1 119.66(9) 12_556 . ? C1 C1 Cl1 120.34(9) 11_556 . ? C1 C1 N1 121.5(8) 11_556 . ? C1 C1 N1 118.5(8) 12_556 . ? N1 C1 Cl1 2.0(5) . . ? O1 Cl1 C1 99.7(4) . . ? O2 Cl1 C1 105.6(6) . . ? O2 Cl1 O1 153.7(8) . . ? O1 N1 C1 114.7(11) . . ? O2 N1 C1 116.2(11) . . ? O2 N1 O1 128.1(16) . . ? Cl1 O1 N1 13.3(7) . . ? Cl1 O2 N1 12.5(8) . . ? 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 1.3885(13) 11_556 ? C1 C1 1.3885(13) 12_556 ? C1 Cl1 1.7259(17) . ? C1 N1 1.444(16) . ? Cl1 O1 1.207(9) . ? Cl1 O2 1.050(8) . ? N1 O1 1.245(11) . ? N1 O2 1.199(11) . ? 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 96.9(5) 11_556 . . . ? C1 C1 Cl1 O1 -83.4(5) 12_556 . . . ? C1 C1 Cl1 O2 -75.7(11) 11_556 . . . ? C1 C1 Cl1 O2 104.0(11) 12_556 . . . ? C1 C1 N1 O1 94.3(14) 11_556 . . . ? C1 C1 N1 O1 -84.1(16) 12_556 . . . ? C1 C1 N1 O2 -75(2) 11_556 . . . ? C1 C1 N1 O2 106.2(19) 12_556 . . . ? C1 Cl1 O1 N1 5(4) . . . . ? C1 Cl1 O2 N1 -4(5) . . . . ? C1 N1 O1 Cl1 -174(5) . . . . ? C1 N1 O2 Cl1 175(6) . . . . ? Cl1 C1 N1 O1 149(25) . . . . ? Cl1 C1 N1 O2 -20(22) . . . . ? N1 C1 Cl1 O1 -29(24) . . . . ? N1 C1 Cl1 O2 158(24) . . . . ? O1 Cl1 O2 N1 -168(5) . . . . ? O1 N1 O2 Cl1 7(3) . . . . ? O2 Cl1 O1 N1 169(5) . . . . ? O2 N1 O1 Cl1 -6(2) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.337(3) 2 0.663(3)