#------------------------------------------------------------------------------ #$Date: 2021-01-01 10:40:07 +0200 (Fri, 01 Jan 2021) $ #$Revision: 260342 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/23/2022302.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2022302 loop_ _publ_author_name 'Niu, Xiang-Long' 'Wei, Lin' 'Liu, Jian-Cheng' 'Jia, Wan-He' 'Ma, Jian-Ping' 'Wang, Lei' 'Wang, Jian-Cheng' 'Dong, Yu-Bin' _publ_section_title ; Syntheses and structures of three macrocyclic supramolecular complexes and one Zn^II^-containing coordination polymer generated from a semi-rigid multidentate N-containing ligand ; _journal_coeditor_code OP3008 _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 29 _journal_page_last 39 _journal_paper_doi 10.1107/S2053229620016083 _journal_volume 77 _journal_year 2021 _chemical_formula_iupac 'C12 H10 N6' _chemical_formula_moiety 'C12 H10 N6' _chemical_formula_sum 'C12 H10 N6' _chemical_formula_weight 238.26 _chemical_name_systematic ; 4-{2-[(Pyridin-3-yl)methyl]-2H-tetrazol-5-yl}pyridine ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:54:37, GUI svn.r4466) ; _cell_angle_alpha 90.00 _cell_angle_beta 93.634(6) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 13.7529(8) _cell_length_b 6.6451(4) _cell_length_c 12.2086(9) _cell_measurement_reflns_used 1274 _cell_measurement_temperature 150.00(10) _cell_measurement_theta_max 70.8520 _cell_measurement_theta_min 7.3960 _cell_volume 1113.49(12) _computing_cell_refinement ; CrysAlis PRO (Rigaku OD, 2015) ; _computing_data_collection ; CrysAlis PRO (Rigaku OD, 2015) ; _computing_data_reduction ; CrysAlis PRO (Rigaku OD, 2015) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL97 (Sheldrick, 2008) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _diffrn_ambient_temperature 150.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0793 _diffrn_measured_fraction_theta_full 0.9986 _diffrn_measured_fraction_theta_max 0.9757 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku OD SuperNova Dual source diffractometer with an Eos detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_unetI/netI 0.0437 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 3957 _diffrn_reflns_theta_full 70.94 _diffrn_reflns_theta_max 70.95 _diffrn_reflns_theta_min 3.22 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.763 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.90107 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlis PRO; Rigaku OD, 2015) ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 496 _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.3 _refine_diff_density_max 0.305 _refine_diff_density_min -0.235 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 163 _refine_ls_number_reflns 2096 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.037 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_gt 0.0489 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0683P)^2^+0.2666P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1249 _refine_ls_wR_factor_ref 0.1393 _reflns_number_gt 1698 _reflns_number_total 2096 _reflns_threshold_expression >2sigma(I) _cod_data_source_file op3008sup1.cif _cod_data_source_block L _cod_database_code 2022302 _shelx_res_file ; TITL exp_2263 in P21/c #14 CELL 1.54178 13.7529 6.6451 12.2086 90 93.634 90 ZERR 4 0.0008 0.0004 0.0009 0 0.006 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N UNIT 48 40 24 L.S. 4 PLAN 20 SIZE 0.43 0.42 0.3 BOND $h conf fmap 2 acta REM D:/data/20201129/olex2_exp_2263/exp_2263.hkl WGHT 0.068300 0.266600 FVAR 5.55696 N1 3 0.331804 0.143707 0.221514 11.00000 0.02734 0.02323 = 0.03168 -0.00227 0.00517 -0.00003 N2 3 0.257131 0.144026 0.284269 11.00000 0.02631 0.02134 = 0.03471 -0.00245 0.00641 -0.00109 N3 3 0.281526 0.132866 0.391197 11.00000 0.03262 0.02917 = 0.03128 -0.00175 0.00795 -0.00056 N4 3 0.377326 0.123352 0.400055 11.00000 0.02884 0.02779 = 0.03120 -0.00026 0.00507 0.00086 N5 3 0.049320 -0.302776 0.113988 11.00000 0.03504 0.03760 = 0.03232 -0.00033 0.00286 -0.01039 N6 3 0.705099 0.119608 0.219554 11.00000 0.02899 0.02548 = 0.04229 -0.00018 0.00545 -0.00097 C1 1 0.406410 0.130189 0.296268 11.00000 0.02725 0.01712 = 0.02909 -0.00129 0.00299 -0.00001 C2 1 0.155972 0.172358 0.240774 11.00000 0.02514 0.03006 = 0.04010 -0.00095 0.00562 0.00158 AFIX 23 H2A 2 0.148849 0.305093 0.208190 11.00000 -1.20000 H2B 2 0.112700 0.163789 0.300328 11.00000 -1.20000 AFIX 0 C3 1 0.075011 -0.152944 0.183429 11.00000 0.02962 0.03757 = 0.02440 0.00228 0.00364 -0.00469 AFIX 43 H3 2 0.056080 -0.162326 0.255041 11.00000 -1.20000 AFIX 0 C4 1 0.127885 0.014979 0.155664 11.00000 0.02067 0.02892 = 0.03111 0.00365 0.00063 0.00214 C5 1 0.154923 0.030228 0.048714 11.00000 0.02827 0.03576 = 0.03570 0.00881 0.00458 -0.00371 AFIX 43 H5 2 0.189722 0.141502 0.026622 11.00000 -1.20000 AFIX 0 C6 1 0.129628 -0.121725 -0.024829 11.00000 0.03131 0.04962 = 0.02846 0.00151 0.00535 -0.00460 AFIX 43 H6 2 0.147345 -0.115242 -0.097005 11.00000 -1.20000 AFIX 0 C7 1 0.077209 -0.284128 0.011469 11.00000 0.03210 0.04318 = 0.03177 -0.00430 0.00210 -0.00457 AFIX 43 H7 2 0.060441 -0.386118 -0.038368 11.00000 -1.20000 AFIX 0 C8 1 0.678518 0.114775 0.322688 11.00000 0.03002 0.02666 = 0.03873 -0.00131 -0.00112 0.00166 AFIX 43 H8 2 0.727503 0.109993 0.378752 11.00000 -1.20000 AFIX 0 C9 1 0.582921 0.116399 0.351860 11.00000 0.03317 0.02296 = 0.02984 -0.00284 0.00244 -0.00069 AFIX 43 H9 2 0.568480 0.111133 0.425200 11.00000 -1.20000 AFIX 0 C10 1 0.508939 0.126093 0.268892 11.00000 0.02747 0.01254 = 0.03175 -0.00079 0.00426 -0.00003 C11 1 0.534660 0.132406 0.160822 11.00000 0.03126 0.02031 = 0.03154 0.00219 0.00168 0.00176 AFIX 43 H11 2 0.487186 0.139447 0.103216 11.00000 -1.20000 AFIX 0 C12 1 0.632535 0.127985 0.140745 11.00000 0.03413 0.02299 = 0.03407 0.00225 0.00884 0.00095 AFIX 43 H12 2 0.649105 0.131006 0.068084 11.00000 -1.20000 HKLF 4 REM exp_2263 in P21/c #14 REM R1 = 0.0489 for 1698 Fo > 4sig(Fo) and 0.0600 for all 2096 data REM 163 parameters refined using 0 restraints END WGHT 0.0678 0.2699 REM Highest difference peak 0.305, deepest hole -0.235, 1-sigma level 0.051 Q1 1 0.4613 0.1295 0.2850 11.00000 0.05 0.30 Q2 1 0.5421 0.0360 0.3094 11.00000 0.05 0.16 Q3 1 0.7707 0.1214 0.2040 11.00000 0.05 0.15 Q4 1 0.1426 0.0996 0.1960 11.00000 0.05 0.15 Q5 1 0.0995 -0.2803 -0.0834 11.00000 0.05 0.15 Q6 1 0.6738 -0.1007 0.4329 11.00000 0.05 0.15 Q7 1 0.6608 -0.1617 0.4191 11.00000 0.05 0.15 Q8 1 0.0325 -0.1470 0.2732 11.00000 0.05 0.14 Q9 1 0.3441 0.1317 0.1435 11.00000 0.05 0.14 Q10 1 0.1333 -0.2473 0.0087 11.00000 0.05 0.14 Q11 1 0.5261 -0.0742 0.0576 11.00000 0.05 0.14 Q12 1 0.1105 -0.3302 0.0845 11.00000 0.05 0.14 Q13 1 0.1601 0.0002 0.1241 11.00000 0.05 0.14 Q14 1 0.6079 -0.1052 0.3384 11.00000 0.05 0.14 Q15 1 0.3228 0.2317 0.1555 11.00000 0.05 0.13 Q16 1 0.2207 0.1162 0.4191 11.00000 0.05 0.13 Q17 1 0.4356 0.3305 0.2847 11.00000 0.05 0.13 Q18 1 0.4408 0.0498 0.4542 11.00000 0.05 0.13 Q19 1 0.3634 0.1245 0.4981 11.00000 0.05 0.12 Q20 1 0.6611 0.0844 -0.0332 11.00000 0.05 0.12 REM The information below was added by Olex2. REM REM R1 = 0.0489 for 1698 Fo > 4sig(Fo) and 0.0600 for all 4217 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.30, deepest hole -0.23 REM Mean Shift 0, Max Shift 0. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0600 REM R1_gt = 0.0489 REM wR_ref = 0.1393 REM GOOF = 1.037 REM Shift_max = 0 REM Shift_mean = 0 REM Reflections_all = 4217 REM Reflections_gt = 1698 REM Parameters = n/a REM Hole = 0.30 REM Peak = -0.23 REM Flack = n/a ; loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_disorder_assembly _atom_site_disorder_group N N1 0.33180(11) 0.1437(2) 0.22151(12) 0.0273(4) Uani d . 1 1 . . N N2 0.25713(11) 0.1440(2) 0.28427(12) 0.0273(4) Uani d . 1 1 . . N N3 0.28153(12) 0.1329(2) 0.39120(13) 0.0308(4) Uani d . 1 1 . . N N4 0.37733(12) 0.1234(2) 0.40005(13) 0.0291(4) Uani d . 1 1 . . N N5 0.04932(12) -0.3028(3) 0.11399(13) 0.0350(4) Uani d . 1 1 . . N N6 0.70510(12) 0.1196(2) 0.21955(14) 0.0321(4) Uani d . 1 1 . . C C1 0.40641(13) 0.1302(2) 0.29627(15) 0.0244(4) Uani d . 1 1 . . C C2 0.15597(13) 0.1724(3) 0.24077(16) 0.0316(4) Uani d . 1 1 . . H H2A 0.1488 0.3051 0.2082 0.038 Uiso calc R 1 1 . . H H2B 0.1127 0.1638 0.3003 0.038 Uiso calc R 1 1 . . C C3 0.07501(14) -0.1529(3) 0.18343(15) 0.0304(4) Uani d . 1 1 . . H H3 0.0561 -0.1623 0.2550 0.037 Uiso calc R 1 1 . . C C4 0.12788(12) 0.0150(3) 0.15566(15) 0.0269(4) Uani d . 1 1 . . C C5 0.15492(14) 0.0302(3) 0.04871(15) 0.0331(5) Uani d . 1 1 . . H H5 0.1897 0.1415 0.0266 0.040 Uiso calc R 1 1 . . C C6 0.12963(15) -0.1217(3) -0.02483(16) 0.0363(5) Uani d . 1 1 . . H H6 0.1473 -0.1152 -0.0970 0.044 Uiso calc R 1 1 . . C C7 0.07721(14) -0.2841(3) 0.01147(16) 0.0357(5) Uani d . 1 1 . . H H7 0.0604 -0.3861 -0.0384 0.043 Uiso calc R 1 1 . . C C8 0.67852(14) 0.1148(3) 0.32269(16) 0.0319(4) Uani d . 1 1 . . H H8 0.7275 0.1100 0.3788 0.038 Uiso calc R 1 1 . . C C9 0.58292(14) 0.1164(3) 0.35186(15) 0.0286(4) Uani d . 1 1 . . H H9 0.5685 0.1111 0.4252 0.034 Uiso calc R 1 1 . . C C10 0.50894(13) 0.1261(2) 0.26889(14) 0.0238(4) Uani d . 1 1 . . C C11 0.53466(14) 0.1324(3) 0.16082(15) 0.0277(4) Uani d . 1 1 . . H H11 0.4872 0.1394 0.1032 0.033 Uiso calc R 1 1 . . C C12 0.63253(14) 0.1280(3) 0.14075(16) 0.0301(4) Uani d . 1 1 . . H H12 0.6491 0.1310 0.0681 0.036 Uiso calc R 1 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N1 0.0273(8) 0.0232(8) 0.0317(8) 0.0000(6) 0.0052(6) -0.0023(6) N2 0.0263(8) 0.0213(8) 0.0347(8) -0.0011(6) 0.0064(6) -0.0025(6) N3 0.0326(9) 0.0292(9) 0.0313(8) -0.0006(7) 0.0079(7) -0.0017(6) N4 0.0288(8) 0.0278(8) 0.0312(8) 0.0009(6) 0.0051(6) -0.0003(6) N5 0.0350(9) 0.0376(9) 0.0323(8) -0.0104(7) 0.0029(7) -0.0003(7) N6 0.0290(8) 0.0255(9) 0.0423(9) -0.0010(7) 0.0054(7) -0.0002(7) C1 0.0272(9) 0.0171(8) 0.0291(9) 0.0000(7) 0.0030(7) -0.0013(6) C2 0.0251(9) 0.0301(10) 0.0401(10) 0.0016(8) 0.0056(8) -0.0009(8) C3 0.0296(10) 0.0376(11) 0.0244(9) -0.0047(8) 0.0036(7) 0.0023(8) C4 0.0207(8) 0.0289(10) 0.0311(9) 0.0021(7) 0.0006(7) 0.0037(7) C5 0.0283(9) 0.0358(11) 0.0357(10) -0.0037(8) 0.0046(8) 0.0088(8) C6 0.0313(10) 0.0496(13) 0.0285(10) -0.0046(9) 0.0053(8) 0.0015(8) C7 0.0321(10) 0.0432(12) 0.0318(10) -0.0046(9) 0.0021(8) -0.0043(9) C8 0.0300(10) 0.0267(10) 0.0387(11) 0.0017(8) -0.0011(8) -0.0013(8) C9 0.0332(10) 0.0230(9) 0.0298(9) -0.0007(7) 0.0024(8) -0.0028(7) C10 0.0275(9) 0.0125(9) 0.0318(9) 0.0000(6) 0.0043(7) -0.0008(6) C11 0.0313(10) 0.0203(9) 0.0315(9) 0.0018(7) 0.0017(7) 0.0022(7) C12 0.0341(10) 0.0230(9) 0.0341(10) 0.0009(8) 0.0088(8) 0.0023(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N2 N1 C1 . . 101.32(14) ? N1 N2 N3 . . 114.38(15) ? N1 N2 C2 . . 122.97(15) ? N3 N2 C2 . . 122.43(15) ? N4 N3 N2 . . 105.80(14) ? N3 N4 C1 . . 105.97(15) ? C7 N5 C3 . . 116.31(17) ? C8 N6 C12 . . 116.22(16) ? N1 C1 N4 . . 112.53(16) ? N1 C1 C10 . . 123.62(16) ? N4 C1 C10 . . 123.84(17) ? N2 C2 H2A . . 109.5 ? N2 C2 H2B . . 109.5 ? N2 C2 C4 . . 110.83(15) ? H2A C2 H2B . . 108.1 ? C4 C2 H2A . . 109.5 ? C4 C2 H2B . . 109.5 ? N5 C3 H3 . . 117.8 ? N5 C3 C4 . . 124.39(17) ? C4 C3 H3 . . 117.8 ? C3 C4 C2 . . 120.37(17) ? C5 C4 C2 . . 121.82(17) ? C5 C4 C3 . . 117.80(17) ? C4 C5 H5 . . 120.4 ? C6 C5 C4 . . 119.22(18) ? C6 C5 H5 . . 120.4 ? C5 C6 H6 . . 120.8 ? C5 C6 C7 . . 118.43(18) ? C7 C6 H6 . . 120.8 ? N5 C7 C6 . . 123.85(18) ? N5 C7 H7 . . 118.1 ? C6 C7 H7 . . 118.1 ? N6 C8 H8 . . 117.8 ? N6 C8 C9 . . 124.37(18) ? C9 C8 H8 . . 117.8 ? C8 C9 H9 . . 120.8 ? C8 C9 C10 . . 118.42(18) ? C10 C9 H9 . . 120.8 ? C9 C10 C1 . . 120.22(17) ? C11 C10 C1 . . 121.43(17) ? C11 C10 C9 . . 118.35(17) ? C10 C11 H11 . . 120.8 ? C12 C11 C10 . . 118.50(18) ? C12 C11 H11 . . 120.8 ? N6 C12 C11 . . 124.13(18) ? N6 C12 H12 . . 117.9 ? C11 C12 H12 . . 117.9 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag N1 N2 . 1.320(2) ? N1 C1 . 1.332(2) ? N2 N3 . 1.329(2) ? N2 C2 . 1.469(2) ? N3 N4 . 1.317(2) ? N4 C1 . 1.353(2) ? N5 C3 . 1.340(2) ? N5 C7 . 1.338(2) ? N6 C8 . 1.334(2) ? N6 C12 . 1.343(3) ? C1 C10 . 1.470(2) ? C2 H2A . 0.9700 ? C2 H2B . 0.9700 ? C2 C4 . 1.507(3) ? C3 H3 . 0.9300 ? C3 C4 . 1.386(3) ? C4 C5 . 1.384(3) ? C5 H5 . 0.9300 ? C5 C6 . 1.381(3) ? C6 H6 . 0.9300 ? C6 C7 . 1.386(3) ? C7 H7 . 0.9300 ? C8 H8 . 0.9300 ? C8 C9 . 1.384(3) ? C9 H9 . 0.9300 ? C9 C10 . 1.391(3) ? C10 C11 . 1.388(3) ? C11 H11 . 0.9300 ? C11 C12 . 1.384(3) ? C12 H12 . 0.9300 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C2 H2B N5^i^ 2_545 0.97 2.53 3.4312(2) 154 yes 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag N1 N2 N3 N4 . . . . -0.41(19) ? N1 N2 C2 C4 . . . . 57.6(2) ? N1 C1 C10 C9 . . . . 178.52(16) ? N1 C1 C10 C11 . . . . -1.3(2) ? N2 N1 C1 N4 . . . . -0.20(18) ? N2 N1 C1 C10 . . . . -179.38(15) ? N2 N3 N4 C1 . . . . 0.24(18) ? N2 C2 C4 C3 . . . . 99.1(2) ? N2 C2 C4 C5 . . . . -79.7(2) ? N3 N2 C2 C4 . . . . -127.97(17) ? N3 N4 C1 N1 . . . . -0.03(19) ? N3 N4 C1 C10 . . . . 179.15(15) ? N4 C1 C10 C9 . . . . -0.6(2) ? N4 C1 C10 C11 . . . . 179.65(15) ? N5 C3 C4 C2 . . . . -178.04(18) ? N5 C3 C4 C5 . . . . 0.8(3) ? N6 C8 C9 C10 . . . . -0.8(3) ? C1 N1 N2 N3 . . . . 0.37(18) ? C1 N1 N2 C2 . . . . 175.20(15) ? C1 C10 C11 C12 . . . . -179.98(16) ? C2 N2 N3 N4 . . . . -175.27(15) ? C2 C4 C5 C6 . . . . 178.03(18) ? C3 N5 C7 C6 . . . . -0.1(3) ? C3 C4 C5 C6 . . . . -0.8(3) ? C4 C5 C6 C7 . . . . 0.4(3) ? C5 C6 C7 N5 . . . . 0.1(3) ? C7 N5 C3 C4 . . . . -0.4(3) ? C8 N6 C12 C11 . . . . 0.2(3) ? C8 C9 C10 C1 . . . . -179.39(16) ? C8 C9 C10 C11 . . . . 0.4(2) ? C9 C10 C11 C12 . . . . 0.2(2) ? C10 C11 C12 N6 . . . . -0.6(3) ? C12 N6 C8 C9 . . . . 0.5(3) ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 1 0 0 24428.4 368.732 2 0 0 2281.15 123.098 3 0 0 14182.9 379.035 4 0 0 151593 2036.87 5 0 0 157466 2261.41 6 0 0 -56.0493 48.7769 -7 0 0 11164.7 593.512 7 0 0 9812.3 535.514 8 0 0 990.019 192.445 -8 0 0 1128.57 204.21 -9 0 0 45311.1 1468.63 -10 0 0 6105.42 544.92 -11 0 0 6908.22 615.148 -11 0 0 8251.3 613.251 -12 0 0 401.047 160.157 -12 0 0 501.74 139.187 -12 0 0 333.444 117.491 -13 0 0 1090.45 236.17 -14 0 0 2511.52 347.149 -15 0 0 3774.87 393.658 -16 0 0 1.28455 53.7824 0 -1 0 6.01378 15.7529 1 -1 0 2399.34 157.401 -1 -1 0 2296.81 87.1122 2 -1 0 33340.8 745.159 3 -1 0 182053 2470.37 3 1 0 182719 2232.45 4 -1 0 68322.4 1309.65 -4 1 0 72090.6 1251.47 4 1 0 68036.6 872.614 4 1 0 68873.7 1164.33 5 1 0 69575.2 1292.78 5 -1 0 69201.2 1421.44 -5 1 0 70569.1 1357.02 5 1 0 69947.5 993.783 5 -1 0 65679.4 1162.26 6 1 0 217.234 75.1612 -6 1 0 285.049 93.348 -7 1 0 21686 838.767 7 1 0 20480.7 772.689 -8 1 0 16836 802.539 8 1 0 16293.9 750.882 -9 1 0 5880.52 506.726 9 1 0 5769.98 481.866 -10 -1 0 189.705 82.6639 -10 1 0 136.283 59.962 -11 1 0 815.102 210.41 -11 -1 0 729.706 186.593 -11 -1 0 617.608 172.981 -12 -1 0 3251.15 445.974 -12 -1 0 3248.53 381.212 -12 1 0 3212.07 420.328 -12 -1 0 3243.53 392.445 -13 -1 0 4107.47 437.165 -13 1 0 3546.85 430.025 -14 -1 0 -4.85816 67.9393 -14 1 0 51.111 28.9653 -15 1 0 96.9614 53.4978 -15 -1 0 81.8944 56.5508 -16 1 0 1751.74 233.713 -16 -1 0 1552.59 207.193 0 -2 0 23040.9 588.804 0 -2 0 20545 512.227 1 -2 0 10231.6 423.447 -1 -2 0 8538.67 290.339 -1 -2 0 9814.4 304.472 -1 -2 0 8817.57 339.427 1 2 0 9087.34 262.15 2 2 0 12542.3 432.794 -2 -2 0 12016.8 398.02 -2 -2 0 11528.2 377.807 3 2 0 21150.5 610.29 3 -2 0 22782.2 758.113 4 2 0 10162.4 435.888 5 2 0 701.313 123.699 6 2 0 8082.24 462.973 7 2 0 17599 759.757 8 2 0 8422.27 548.615 9 2 0 3505.13 375.366 -10 -2 0 561.417 160.592 -10 2 0 599.417 160.625 -11 2 0 935.88 220.592 -11 -2 0 946.625 206.29 -11 -2 0 582.219 179.806 11 -2 0 701.481 192.671 -12 2 0 1530.03 274.806 -13 2 0 5.02072 28.1951 -13 -2 0 334.011 119.31 -14 2 0 121.6 87.3503 -15 2 0 57.5822 79.7736 -16 2 0 86.5913 44.8195 0 -3 0 87.5993 39.7735 1 -3 0 61.6569 32 -1 -3 0 8.05937 19.3223 1 -3 0 94.4325 40.7333 -1 -3 0 35.405 34.1207 -2 -3 0 6636.73 347.889 2 3 0 6930.71 395.443 -2 -3 0 6429.22 324.182 2 -3 0 6387.26 328.744 3 -3 0 20.2303 31.1004 -3 -3 0 37.0721 28.8743 3 3 0 10.2628 20.7885 -4 -3 0 1808.63 204.591 4 3 0 1849.57 219.956 5 3 0 720.73 152.351 -5 -3 0 624.131 131.382 -6 -3 0 15189.5 679.884 6 3 0 15149.2 705.773 7 3 0 5722.9 455.444 -7 -3 0 6567.72 471.346 -8 -3 0 3168.62 348.772 8 3 0 2598.8 316.882 -9 -3 0 227.263 118.305 9 -3 0 170.02 106.119 10 -3 0 1550.03 330.961 -10 -3 0 1459.48 263.702 11 -3 0 1633.06 329.363 12 -3 0 160.111 62.5191 -13 3 0 57.5253 45.1161 13 -3 0 -43.0805 77.0843 -14 -3 0 61.5527 32.6244 -15 -3 0 235.531 68.2241 -1 -4 0 123220 2128.17 1 -4 0 126451 2127.78 2 -4 0 5976.8 382.377 -2 -4 0 4910.33 360.024 2 4 0 6170.26 442.834 3 4 0 29662.7 1016.02 4 4 0 99.8086 49.1466 -5 -4 0 6718.68 460.374 5 4 0 6828.57 505.882 -6 -4 0 -21.1548 41.8917 6 4 0 7.86628 37.9868 7 -4 0 276.84 120.931 -7 -4 0 71.4718 59.6594 7 4 0 116.416 58.8687 8 -4 0 825.133 223.238 -8 -4 0 690.981 159.025 -9 -4 0 4606.68 455.078 9 -4 0 4762.81 571.482 10 -4 0 2147.15 386.711 11 -4 0 121.848 87.2825 12 -4 0 159.38 82.0498 13 -4 0 -35.9578 60.414 -13 -4 0 -55.5214 43.5497 14 -4 0 28.5402 33.8113 -14 -4 0 15.2418 36.9968 1 5 0 2318.4 303.716 2 5 0 5217.71 468.27 3 -5 0 11355.5 792.617 3 -5 0 12186.1 834.46 3 5 0 9597.62 649.246 4 5 0 453.257 132.364 4 -5 0 673.399 195.433 4 -5 0 803.272 217.548 5 5 0 1.29789 38.2386 5 -5 0 17.2345 34.7122 5 -5 0 24.305 41.0132 6 -5 0 2754.12 431.13 6 5 0 2176.62 320.777 6 -5 0 2302.21 367.399 7 -5 0 3537.86 433.551 7 -5 0 3715.64 503.102 8 -5 0 2898.48 383.559 8 -5 0 3265.86 469.778 9 -5 0 68.0229 84.0101 10 -5 0 73.1708 90.3265 -11 -5 0 1406.56 218.641 11 -5 0 1379.22 263.943 12 -5 0 1500.93 246.295 -12 -5 0 1662.03 207.568 -13 -5 0 2548.53 215.913 0 -6 0 17210.3 962.324 0 6 0 16274.6 908.611 -1 -6 0 2117.75 328.235 1 -6 0 1647.34 292.116 2 -6 0 214.193 100.742 -2 -6 0 381.657 126.058 3 -6 0 1448.23 297.696 4 -6 0 586.337 183.641 5 -6 0 956.285 233.394 6 -6 0 113.627 85.0979 7 -6 0 44.9088 63.4456 8 -6 0 289.211 121.706 -8 -6 0 197.753 70.3466 -9 -6 0 465.422 103.935 -10 -6 0 2760.79 243.463 -11 -6 0 14.5634 18.3402 0 -7 0 -61.3761 64.1875 1 -7 0 5507.25 495.388 2 -7 0 204.813 106.064 3 -7 0 -34.8533 71.1985 3 -7 0 55.3776 31.9293 4 -7 0 730.117 160.214 4 -7 0 1063.07 209.192 5 -7 0 3401 350.15 5 -7 0 3233.03 360.01 6 -7 0 7143.83 501.88 6 -7 0 6118.54 458.692 7 -7 0 1851.54 233.062 7 -7 0 2300.38 257.471 8 -7 0 247.635 73.8795 -16 0 1 -79.5261 68.7036 -15 0 1 -15.4642 33.7551 -14 0 1 -42.4758 52.522 -13 0 1 17.4117 29.8721 -12 0 1 26.2231 46.9326 -12 0 1 -7.56021 69.1439 -11 0 1 26.1716 80.4503 -11 0 1 -48.0451 90.1829 -10 0 1 49.5638 45.8157 9 0 -1 -102.224 52.0001 -9 0 1 34.506 45.3657 8 0 -1 -5.99431 42.4094 -8 0 1 40.4035 54.018 7 0 -1 -0.85802 30.8384 6 0 -1 23.9389 23.3056 -5 0 1 26.3624 36.301 5 0 -1 32.9609 36.9307 4 0 -1 8.35135 25.0052 -4 0 1 0.62268 17.4174 -3 0 1 -36.0896 24.2848 2 0 -1 22.3468 18.3109 1 0 -1 51.3738 18.634 0 0 1 -0.63132 8.97797 1 0 1 -1.9472 14.4124 -2 0 -1 -1.0773 13.4807 4 0 1 6.77118 20.0412 -4 0 -1 35.412 36.3701 4 0 1 0.08048 19.1266 5 0 1 8.72267 21.1326 -5 0 -1 16.5337 18.2313 -6 0 -1 16.6187 29.9934 6 0 1 -1.617 29.7532 6 0 1 -39.7693 46.1656 7 0 1 44.7689 59.1188 -7 0 -1 -41.8902 41.4469 -8 0 -1 26.4963 38.0903 -9 0 -1 1.90844 42.5455 -10 0 -1 28.3058 76.9832 -11 0 -1 -49.1074 80.1511 -11 0 -1 60.4998 47.9384 -11 0 -1 43.1685 51.2412 -12 0 -1 71.0664 60.8808 -13 0 -1 -42.2308 50.0929 -14 0 -1 21.1905 49.0023 -15 0 -1 -33.2498 61.6702 -16 0 -1 35.8153 46.3465 -16 1 1 4502.71 374.818 -16 -1 1 3965.25 331.269 -15 -1 1 -33.4299 26.0248 -15 1 1 59.1786 68.9228 -14 1 1 143.074 108.978 -14 -1 1 44.7877 56.3887 -13 -1 1 1077.89 224.94 -13 1 1 1446.22 269.094 -12 -1 1 130.946 95.5877 -12 1 1 320.08 135.899 -12 -1 1 195.355 93.7885 -11 -1 1 8447.18 707.889 11 1 -1 8623.77 697.44 -11 -1 1 7609.53 592.425 -11 1 1 8180.12 682.79 -11 1 1 9240.24 651.066 -10 -1 1 3901.04 458.026 -10 1 1 3959.56 441.708 10 1 -1 3648.06 421.345 -9 1 1 10516.5 676.87 9 1 -1 10492.6 670.211 8 1 -1 14374.2 731.088 -8 1 1 14534.9 736.501 7 1 -1 10529.2 569.945 -7 1 1 10128.6 572.238 -6 1 1 44065 1149.85 6 1 -1 47714.2 1157.68 5 1 -1 30573.5 820.99 -5 1 1 29382.4 828.529 -5 -1 1 27930.6 617.773 -4 -1 1 25014.9 528.038 4 1 -1 27044.6 692.56 -4 1 1 26721.1 801.629 -3 1 1 79941.6 1236.12 -2 -1 1 44508.7 659.108 -2 -1 1 43182.2 666.586 -1 -1 1 126321 1506.42 -1 1 1 130123 1656.75 1 1 -1 128158 1521.13 0 1 -1 3150.1 162.988 1 1 1 996.024 67.1312 2 1 1 54895.4 638.19 3 1 1 80668.4 969.156 3 -1 1 98075.1 1300.38 -4 -1 -1 26440.5 537.911 -4 1 -1 28636.9 755.141 4 -1 1 29138.8 696.736 4 1 1 27819.4 642.361 4 -1 1 28421.5 826.627 -5 1 -1 174.029 65.9276 5 1 1 292.232 71.8967 5 -1 1 239.206 71.3511 5 -1 1 286.218 99.7101 6 -1 1 19511.1 672.735 -6 1 -1 17526.1 697.395 6 1 1 18155.6 630.558 7 1 1 32606.6 967.242 7 -1 1 32414.2 956.973 -8 1 -1 -17.7606 45.9811 -8 -1 -1 -9.53914 58.8991 8 1 1 46.8973 53.5287 -9 -1 -1 35.6142 34.2005 -10 -1 -1 4331.84 456.921 -10 -1 -1 4890.4 440.704 -11 -1 -1 2142.33 336.718 -11 -1 -1 2136.37 300.374 -11 1 -1 1917.05 323.701 -11 -1 -1 2254.25 318.998 -12 -1 -1 933.514 229.35 -12 -1 -1 1196.48 242.495 -12 -1 -1 985.297 202.647 -12 1 -1 1409 274.593 -13 1 -1 216.929 107.978 -13 -1 -1 144.98 69.7021 -14 1 -1 1216.17 247.831 -14 -1 -1 1110.49 220.271 -15 -1 -1 197.59 85.4874 -15 1 -1 262.594 106.63 -16 1 -1 4210.09 356.235 -16 -1 -1 3275.05 289.505 -16 2 1 16.2306 42.224 -15 2 1 15.8375 42.416 -14 2 1 26.1343 47.2267 -14 -2 1 144.945 78.5709 -13 -2 1 5541.39 473.595 -13 2 1 6771.8 559.554 13 -2 -1 6646.99 617.043 12 -2 -1 1528.6 307.764 -12 2 1 1994.72 309.513 -12 -2 1 1635.48 261.026 -11 2 1 488.783 161.08 11 -2 -1 629.294 188.388 -11 -2 1 536.254 164.808 -11 -2 1 581.909 202.464 -11 -2 1 536.887 157.536 11 2 -1 538.248 178.233 -10 2 1 7376.78 557.854 10 -2 -1 7194.07 652.917 10 2 -1 7077.12 605.523 9 2 -1 145.593 97.6962 8 2 -1 6192.62 487.767 7 2 -1 -14.0564 46.5745 6 2 -1 2796.2 282.117 5 2 -1 40083.3 1033.58 4 2 -1 71.9227 39.4268 3 2 -1 24790.6 678.116 -3 -2 1 23370.5 628.821 -2 -2 1 90978.7 1478.76 -2 -2 1 92490.9 1468.53 2 2 -1 96434.9 1519.17 2 2 -1 97047.4 1213.38 1 -2 -1 100726 1376.87 1 -2 -1 102522 1381.95 0 -2 -1 993582 10078.2 0 2 -1 999999 10222.5 -1 -2 -1 439708 4608.07 -1 -2 -1 434984 4754.42 -1 -2 -1 435406 4661.81 2 2 1 3109.78 202.305 2 -2 1 3673.55 285.828 -2 -2 -1 3024.68 206.833 -3 -2 -1 25276.3 675.208 3 2 1 25408 654.573 -4 -2 -1 110.988 36.8528 4 2 1 96.8417 44.7368 -5 -2 -1 2350.97 224.357 5 2 1 2479.32 219.465 6 2 1 19764.7 712.228 -6 -2 -1 22072.2 766.479 7 2 1 52471.7 1325.15 -7 -2 -1 60172.7 1424.36 -8 -2 -1 2148.79 270.611 -9 -2 -1 32868.3 1162.74 -10 2 -1 8691.26 632.491 -10 -2 -1 8137.53 647.981 -10 -2 -1 9296.23 632.923 -11 2 -1 21737.4 1053.38 -11 -2 -1 24450 1085.86 -11 -2 -1 21393.5 1095.09 -12 2 -1 2.68471 71.161 -13 2 -1 1128.92 240.609 -13 -2 -1 1318.24 211.162 -14 2 -1 1423.71 249.227 -15 2 -1 276.981 97.2007 -15 -3 1 308.008 75.957 14 -3 -1 -21.1473 26.4522 13 -3 -1 4908.37 513.216 12 -3 -1 12.4865 40.4642 11 -3 -1 5359.74 599.102 10 3 -1 1035.35 252.969 10 -3 -1 984.362 263.151 -10 -3 1 1153.52 228.169 9 -3 -1 2824.67 415.866 -9 -3 1 2485.57 327.324 9 3 -1 2483.35 342.829 -8 -3 1 2076.32 275.026 8 3 -1 1665.23 280.003 -7 -3 1 19867.6 810.958 7 3 -1 17948.9 842.965 6 3 -1 18064.8 811.466 -6 -3 1 17310.6 711.967 5 3 -1 41.8449 48.1274 -5 -3 1 95.975 48.5969 -4 -3 1 3075.81 256.105 4 3 -1 3508.9 303.565 3 3 -1 13809.6 592.869 -3 -3 1 11980.5 531.742 -3 -3 1 12994 491.428 2 -3 -1 10.7031 19.8256 2 3 -1 35.558 28.2899 -2 -3 1 38.3587 45.7389 -2 -3 1 18.3488 33.1293 1 -3 -1 1775.53 167.444 -1 -3 1 1581.57 180.351 0 -3 -1 32581.6 763.638 0 3 -1 35431.8 887.972 0 -3 1 34727.2 875.729 -1 3 -1 23732.9 786.036 1 -3 1 24626.1 709.967 -1 -3 -1 23785 659.04 -1 -3 -1 23793 647.674 -2 -3 -1 952.463 122.321 -2 -3 -1 842.37 127.305 2 3 1 933.199 135.96 3 3 1 1184.73 164.144 -3 -3 -1 1188.93 157.96 -4 -3 -1 482.111 112.228 4 3 1 487.233 109.248 5 3 1 146.21 79.7851 -5 -3 -1 131.976 62.3548 6 3 1 -26.4415 53.7278 -6 -3 -1 -15.1218 24.8506 -7 -3 -1 1155.08 207.905 -8 -3 -1 941.753 201.812 -9 -3 -1 12738.4 755.029 9 -3 1 11023 817.573 10 -3 1 1921.72 350.693 -10 -3 -1 1598.17 280.866 11 -3 1 14558.9 944.046 -11 3 -1 14925.9 842.985 -12 3 -1 624.161 170.542 12 -3 1 839.39 219.354 -13 3 -1 2395.96 313.146 -13 -3 -1 3095.19 328.547 -14 -3 -1 185.374 59.8989 -14 3 -1 246.167 80.7356 15 -3 1 123.538 62.1961 -14 -4 1 307.078 87.9453 14 -4 -1 177.833 80.214 13 -4 -1 -5.90074 48.7258 12 -4 -1 80.9375 74.0935 11 -4 -1 -0.73014 66.1273 10 -4 -1 1541.27 314.558 -9 -4 1 88.4544 65.975 9 4 -1 -209.733 124.076 9 -4 -1 -100.614 105.545 -8 -4 1 647.994 166.903 8 -4 -1 950.874 247.959 8 4 -1 755.666 181.258 7 -4 -1 233.021 119.204 -7 -4 1 107.378 63.5468 7 4 -1 109.788 88.5626 6 4 -1 772.373 182.824 5 4 -1 1378.52 228.769 4 4 -1 1337.6 217.111 -3 -4 1 554.454 136.888 3 4 -1 769.991 165.375 -2 -4 1 1207.26 188.893 2 4 -1 2213.39 269.202 -1 -4 1 333.098 101.181 -1 -4 1 455.646 137.179 1 4 -1 482.088 129.746 0 -4 1 5072.11 384.911 1 -4 1 524.312 123.835 2 4 1 4.78243 18.687 2 -4 1 -14.3642 29.5148 3 4 1 2057.61 253.138 3 -4 1 1537.75 200.507 -4 -4 -1 8603.76 513.2 4 4 1 7933.66 518.65 -5 -4 -1 3800.64 360.24 5 4 1 3542.24 348.658 -6 -4 -1 6038.12 478.434 -7 -4 -1 264.929 109.09 7 -4 1 419.263 165.472 8 -4 1 254.008 144.661 -8 -4 -1 201.283 102.181 9 -4 1 2209.69 389.417 -9 -4 -1 1950.61 305.889 10 -4 1 2931.8 430.489 11 -4 1 -67.3813 82.0346 11 -4 1 -57.838 66.0782 -12 -4 -1 86.1771 40.4366 12 -4 1 121.469 76.9138 -13 -4 -1 287.291 90.4753 13 -4 1 164.67 84.4245 -14 -4 -1 862.989 131.646 -13 -5 1 14.4511 23.6635 13 -5 -1 -61.0197 51.2901 12 -5 -1 19.0546 43.305 -12 -5 1 33.4351 39.8755 11 -5 -1 116.406 71.1876 10 -5 -1 1128.51 259.49 9 -5 -1 54.5808 39.6573 8 -5 -1 44.3013 73.114 8 -5 -1 26.2293 38.6171 7 -5 -1 10894 793.026 7 -5 -1 10339.1 834.348 6 -5 -1 8977.5 763.737 6 -5 -1 9245.03 742.74 6 5 -1 7675.31 618.601 5 -5 -1 543.513 185.773 5 5 -1 226.412 129.809 5 -5 -1 433.841 178.025 4 5 -1 1769.5 291.358 4 -5 -1 1994.29 340.342 4 -5 -1 2214.44 360.832 3 -5 -1 -10.2258 90.4471 3 -5 -1 -114.955 93.7824 3 5 -1 44.7621 47.3132 2 5 -1 2610.61 344.294 -2 -5 1 2357.4 285.356 -1 -5 1 -72.4539 84.983 1 5 -1 11.3506 48.6791 0 5 -1 329.002 91.0157 0 -5 1 267.118 101.198 1 5 1 19816.9 906.72 1 -5 1 19560.7 874.302 2 5 1 2664.17 336.123 3 -5 1 188.545 99.0482 3 -5 1 269.234 121.989 3 5 1 132.597 66.31 4 5 1 5.44961 26.894 4 -5 1 133.265 115.636 4 -5 1 50.2033 72.9952 5 -5 1 9006.01 765.923 5 -5 1 8138.94 683.588 6 -5 1 13390.4 866.875 6 -5 1 14004.3 967.907 7 -5 1 272.305 152.907 7 -5 1 183.995 88.5232 8 -5 1 1198.14 286.798 9 -5 1 37.5111 50.6287 -9 -5 -1 119.4 48.9952 -10 -5 -1 129.308 58.8622 10 -5 1 197.617 100.596 11 -5 1 863.242 206.763 -11 -5 -1 756.112 154.872 -12 -5 -1 2245.56 237.033 -13 -5 -1 -27.6811 29.4906 -11 -6 1 135.637 43.9872 -10 -6 1 17.8534 27.4945 -9 -6 1 856.453 144.971 9 -6 -1 813.838 165.594 9 -6 -1 839.335 196.954 8 -6 -1 2758.29 388.532 -8 -6 1 2858.49 282.918 8 -6 -1 2734.3 344.02 7 -6 -1 36.3255 41.1616 7 -6 -1 -61.8455 101.373 6 -6 -1 188.197 125.421 6 -6 -1 52.9354 63.2288 5 -6 -1 1993.02 360.147 5 -6 -1 2252.86 372.947 4 -6 -1 2431.53 375.899 3 -6 -1 17676.5 1050.7 2 -6 -1 -91.0712 70.5984 -2 -6 1 -77.4425 107.587 -1 -6 1 9476.98 700.094 1 -6 -1 9811.88 750.791 0 -6 1 54391.5 1779.08 0 -6 1 52004.8 1650.23 0 -6 -1 55966.8 1796.13 1 -6 1 95644.3 2457.9 -1 -6 -1 94221.3 2340.38 1 -6 1 92046.4 2323 2 -6 1 4755.12 513.872 2 -6 1 4291.78 474.37 3 -6 1 -60.7917 95.1377 4 -6 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