#------------------------------------------------------------------------------ #$Date: 2019-12-04 09:38:55 +0200 (Wed, 04 Dec 2019) $ #$Revision: 244896 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/64/1556424.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_1556424 loop_ _publ_author_name 'Rancan, M.' 'Carlotto, A.' 'Bottaro, G.' 'Armelao, L.' _publ_section_title ; Effect of Coordinating Solvents on the Structure of Cu(II)-4,4'-bipyridine Coordination Polymers ; _journal_name_full Inorganics _journal_page_first 103 _journal_paper_doi 10.3390/inorganics7080103 _journal_volume 7 _journal_year 2019 _chemical_formula_moiety '0.5(C40 H40 Cu2 N8 O4), 2(Cl O4), O, 2(C10 H8 N2)' _chemical_formula_sum 'C40 H36 Cl2 Cu N8 O11' _chemical_formula_weight 939.21 _space_group_crystal_system monoclinic _space_group_IT_number 13 _space_group_name_Hall '-P 2yac' _space_group_name_H-M_alt 'P 1 2/n 1' _atom_sites_solution_hydrogens mixed _cell_angle_alpha 90 _cell_angle_beta 106.559(6) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 12.9264(5) _cell_length_b 11.1702(4) _cell_length_c 15.0564(10) _cell_measurement_reflns_used 4617 _cell_measurement_temperature 301.2(8) _cell_measurement_theta_max 28.9540 _cell_measurement_theta_min 2.8400 _cell_volume 2083.84(19) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_environment air _diffrn_ambient_temperature 301.2(8) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1274 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -52.00 49.00 0.2500 15.0000 omega____ theta____ kappa____ phi______ frames - 18.5210 -77.0000 60.0000 404 #__ type_ start__ end____ width___ exp.time_ 2 omega -54.00 44.00 0.2500 15.0000 omega____ theta____ kappa____ phi______ frames - 18.5210 -38.0000 120.0000 392 #__ type_ start__ end____ width___ exp.time_ 3 omega -12.00 89.00 0.2500 15.0000 omega____ theta____ kappa____ phi______ frames - 18.5210 77.0000 -90.0000 404 #__ type_ start__ end____ width___ exp.time_ 4 omega -25.00 23.00 0.2500 15.0000 omega____ theta____ kappa____ phi______ frames - -18.5992 -99.0000 -120.0000 192 #__ type_ start__ end____ width___ exp.time_ 5 omega -26.00 84.00 0.2500 15.0000 omega____ theta____ kappa____ phi______ frames - 18.5210 19.0000 150.0000 440 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0141967000 _diffrn_orient_matrix_UB_12 0.0588992000 _diffrn_orient_matrix_UB_13 0.0168034000 _diffrn_orient_matrix_UB_21 -0.0458667000 _diffrn_orient_matrix_UB_22 0.0227809000 _diffrn_orient_matrix_UB_23 -0.0337393000 _diffrn_orient_matrix_UB_31 -0.0312244000 _diffrn_orient_matrix_UB_32 -0.0068872000 _diffrn_orient_matrix_UB_33 0.0314839000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_unetI/netI 0.0327 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 16348 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 26.314 _diffrn_reflns_theta_min 2.306 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.723 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.63466 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'light blue' _exptl_crystal_density_diffrn 1.497 _exptl_crystal_description block _exptl_crystal_F_000 966 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.616 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.091 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 284 _refine_ls_number_reflns 4235 _refine_ls_number_restraints 26 _refine_ls_restrained_S_all 1.080 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0473 _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^)+(0.0695P)^2^+1.7361P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1279 _refine_ls_wR_factor_ref 0.1334 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3817 _reflns_number_total 4235 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file 5.cif _cod_data_source_block 5 _cod_original_cell_volume 2083.83(19) _cod_database_code 1556424 _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. ; _reflns_odcompleteness_completeness 99.40 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All O(H,H) groups 2. Rigid body (RIGU) restrains O3, Cl1, O4, O2, O5 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 3.a Rotating group: O1(H1A,H1B) 3.b Aromatic/amide H refined with riding coordinates: C6(H6), C7(H7), C4(H4), C5(H5), C10(H10), C11(H11), C2(H2), C1(H1), C14(H14), C12(H12), C15(H15), C13(H13), C20(H20), C18(H18), C21(H21), C19(H19) ; _shelx_res_file ; TITL 5.res in P2/n 5.res created by SHELXL-2018/3 at 13:58:50 on 18-Jul-2019 REM Old 5 in P2/n #13 REM SHELXT solution in P2/n REM R1 0.183, Rweak 0.068, Alpha 0.050, Orientation as input REM Formula found by SHELXT: C50 N4 O5 Cl2 Cu CELL 0.71073 12.926386 11.170186 15.056388 90 106.5587 90 ZERR 2 0.000522 0.000424 0.000961 0 0.0057 0 LATT 1 SYMM 0.5-X,+Y,0.5-Z SFAC C H Cl Cu N O UNIT 80 72 4 2 16 22 RIGU O3 Cl1 O4 O2 O5 L.S. 50 PLAN 10 BIND O1 Cu1 BOND $H LIST 4 MORE -1 CONF fmap 2 acta 52 REM REM REM WGHT 0.069500 1.736100 FVAR 0.39059 CU1 4 0.250000 0.473935 0.250000 10.50000 0.03094 0.01310 = 0.03670 0.00000 0.02475 0.00000 CL1 3 0.583674 0.788262 0.398657 11.00000 0.04918 0.04156 = 0.05276 0.00366 0.01468 -0.00835 N2 5 0.250000 0.656622 0.250000 10.50000 0.02918 0.01728 = 0.03361 0.00000 0.01632 0.00000 O1 6 0.417783 0.483850 0.382566 11.00000 0.03399 0.03148 = 0.04890 0.00217 0.01357 -0.00131 AFIX 7 H1A 2 0.450206 0.554318 0.384843 11.00000 -1.50000 H1B 2 0.467141 0.433105 0.374578 11.00000 -1.50000 AFIX 0 N1 5 0.158473 0.476858 0.342358 11.00000 0.02832 0.02297 = 0.03542 0.00252 0.02084 0.00160 N3 5 0.250000 1.290852 0.250000 10.50000 0.02462 0.01514 = 0.03956 0.00000 0.01618 0.00000 C6 1 0.265936 0.719018 0.328704 11.00000 0.04047 0.02119 = 0.03142 0.00201 0.01558 0.00296 AFIX 43 H6 2 0.277684 0.677070 0.384051 11.00000 -1.20000 AFIX 0 O3 6 0.553759 0.695456 0.451879 11.00000 0.10018 0.07471 = 0.08682 0.01880 0.02262 -0.03158 C7 1 0.265786 0.841857 0.331717 11.00000 0.04289 0.02203 = 0.03111 -0.00325 0.01127 0.00159 AFIX 43 H7 2 0.276153 0.881401 0.387936 11.00000 -1.20000 AFIX 0 C4 1 -0.000405 0.545482 0.378915 11.00000 0.03158 0.04203 = 0.04065 0.00899 0.02169 0.01308 AFIX 43 H4 2 -0.065737 0.586286 0.360042 11.00000 -1.20000 AFIX 0 C5 1 0.062987 0.534534 0.319223 11.00000 0.03653 0.03865 = 0.03551 0.00994 0.02247 0.01063 AFIX 43 H5 2 0.038611 0.568483 0.260547 11.00000 -1.20000 AFIX 0 C9 1 0.250000 1.039554 0.250000 10.50000 0.02870 0.01759 = 0.03572 0.00000 0.01066 0.00000 C10 1 0.317900 1.104357 0.322039 11.00000 0.03595 0.02032 = 0.04169 0.00121 0.00065 0.00330 AFIX 43 H10 2 0.364292 1.064612 0.371968 11.00000 -1.20000 AFIX 0 C3 1 0.033284 0.495757 0.466761 11.00000 0.02650 0.03086 = 0.03397 0.00289 0.01966 0.00336 C11 1 0.316401 1.228250 0.319390 11.00000 0.03333 0.02123 = 0.04198 -0.00527 0.00527 -0.00278 AFIX 43 H11 2 0.363418 1.269993 0.367761 11.00000 -1.20000 AFIX 0 C8 1 0.250000 0.906811 0.250000 10.50000 0.02238 0.01747 = 0.03559 0.00000 0.00652 0.00000 C2 1 0.132865 0.436556 0.490456 11.00000 0.03277 0.04752 = 0.03478 0.01102 0.01958 0.01144 AFIX 43 H2 2 0.159239 0.401768 0.548660 11.00000 -1.20000 AFIX 0 C1 1 0.192092 0.429891 0.426970 11.00000 0.02955 0.03761 = 0.04155 0.00714 0.02202 0.01024 AFIX 43 H1 2 0.258353 0.390808 0.444305 11.00000 -1.20000 AFIX 0 O6 6 0.750000 0.652591 0.250000 10.50000 0.07012 0.09300 = 0.10589 0.00000 0.02089 0.00000 O4 6 0.540359 0.897116 0.419678 11.00000 0.10992 0.05719 = 0.20626 -0.01017 0.06724 0.00170 O2 6 0.536834 0.763034 0.306168 11.00000 0.27168 0.14850 = 0.06113 -0.01018 0.03441 -0.08489 O5 6 0.695555 0.800550 0.424235 11.00000 0.05270 0.09822 = 0.27594 0.04279 0.03997 -0.00884 N4 5 0.591696 0.319843 0.392558 11.00000 0.03695 0.05775 = 0.08260 0.00118 0.01602 0.00410 C14 1 0.604993 0.204270 0.412668 11.00000 0.03760 0.06741 = 0.08217 0.01220 0.02404 0.00035 AFIX 43 H14 2 0.550724 0.164922 0.430512 11.00000 -1.20000 AFIX 0 C12 1 0.671554 0.373636 0.368146 11.00000 0.04863 0.04655 = 0.10419 0.00368 0.01986 0.00043 AFIX 43 H12 2 0.664505 0.454629 0.353340 11.00000 -1.20000 AFIX 0 C16 1 0.777519 0.194356 0.383083 11.00000 0.03509 0.04625 = 0.05058 -0.00802 0.01576 -0.00765 C15 1 0.694428 0.138180 0.408864 11.00000 0.04234 0.04542 = 0.07178 0.00490 0.02381 -0.00265 AFIX 43 H15 2 0.698832 0.057072 0.423407 11.00000 -1.20000 AFIX 0 C17 1 0.875919 0.127738 0.378849 11.00000 0.04103 0.04803 = 0.06062 -0.00830 0.02528 -0.00477 C13 1 0.763753 0.315652 0.363716 11.00000 0.04226 0.04933 = 0.10366 0.00412 0.03031 -0.00945 AFIX 43 H13 2 0.817504 0.358255 0.347547 11.00000 -1.20000 AFIX 0 N5 5 1.066158 0.005958 0.376626 11.00000 0.06698 0.08343 = 0.13371 -0.01937 0.06019 0.00861 C20 1 0.877099 0.006553 0.367054 11.00000 0.05856 0.05941 = 0.11960 -0.03029 0.03512 -0.00917 AFIX 43 H20 2 0.814744 -0.038368 0.360253 11.00000 -1.20000 AFIX 0 C18 1 0.971267 0.185205 0.386628 11.00000 0.05643 0.05431 = 0.23778 -0.03072 0.07479 -0.01301 AFIX 43 H18 2 0.975113 0.268150 0.391872 11.00000 -1.20000 AFIX 0 C21 1 0.973437 -0.048917 0.365359 11.00000 0.08498 0.06573 = 0.13977 -0.03597 0.04858 0.00677 AFIX 43 H21 2 0.971755 -0.131168 0.355474 11.00000 -1.20000 AFIX 0 C19 1 1.062799 0.119384 0.386696 11.00000 0.06214 0.07751 = 0.27150 -0.03103 0.09157 -0.00991 AFIX 43 H19 2 1.126875 0.161508 0.394746 11.00000 -1.20000 AFIX 0 HKLF 4 REM 5.res in P2/n REM wR2 = 0.1334, GooF = S = 1.081, Restrained GooF = 1.080 for all data REM R1 = 0.0473 for 3817 Fo > 4sig(Fo) and 0.0522 for all 4235 data REM 284 parameters refined using 26 restraints END WGHT 0.0695 1.7359 REM Highest difference peak 0.616, deepest hole -0.711, 1-sigma level 0.091 Q1 1 0.5246 0.8697 0.3418 11.00000 0.05 0.62 Q2 1 0.5060 0.7685 0.2978 11.00000 0.05 0.57 Q3 1 0.1987 0.4758 0.1836 11.00000 0.05 0.49 Q4 1 0.5969 0.7034 0.3421 11.00000 0.05 0.47 Q5 1 0.5775 0.6616 0.4006 11.00000 0.05 0.45 Q6 1 0.6195 0.8574 0.4688 11.00000 0.05 0.43 Q7 1 0.6537 0.8209 0.4764 11.00000 0.05 0.42 Q8 1 0.6065 0.8282 0.3136 11.00000 0.05 0.39 Q9 1 0.2559 0.5397 0.2034 11.00000 0.05 0.39 Q10 1 0.2767 0.8825 0.2966 11.00000 0.05 0.38 ; _shelx_res_checksum 49823 _shelx_hkl_file ; 0 0 2 424.63 5.80 0 0 -2 487.44 5.75 0 0 -3 0.83 0.29 0 0 3 0.38 0.23 0 0 -3 0.70 0.36 0 0 4 4874.10 45.43 0 0 -4 4366.64 44.57 0 0 5 0.45 0.50 0 0 -5 -0.14 0.45 0 0 -5 -0.20 0.22 0 0 5 0.16 0.29 0 0 6 770.23 12.19 0 0 -6 723.77 12.39 0 0 -7 0.16 0.75 0 0 -7 0.13 0.26 0 0 7 0.01 0.29 0 0 -8 896.87 13.98 0 0 8 845.68 15.29 0 0 -9 0.36 0.57 0 0 9 -0.45 0.60 0 0 10 23.06 2.60 0 0 -10 27.05 2.52 0 0 -11 0.10 0.71 0 0 11 0.96 0.83 0 0 -12 179.06 7.36 0 0 -12 173.46 7.02 0 0 12 172.04 7.68 0 0 -13 1.01 0.92 0 0 -13 1.57 1.17 0 0 -14 415.92 12.79 0 0 -14 391.72 11.89 0 0 -15 2.25 1.31 0 0 -15 0.97 1.22 0 0 -16 59.00 5.11 0 0 -16 54.46 4.74 0 0 -17 0.59 0.86 0 0 -17 0.19 0.77 0 0 -18 2.44 1.66 0 0 -18 1.14 0.77 0 1 -1 2.19 0.32 0 -1 1 1.37 0.25 0 -1 1 1.85 0.30 0 1 2 132.40 2.51 0 -1 2 90.20 2.46 0 -1 2 148.13 3.22 0 -1 -2 141.95 2.66 0 -1 -2 133.55 2.51 0 1 -2 127.78 2.79 0 1 -2 104.36 2.68 0 -1 3 136.36 3.45 0 -1 3 90.76 2.64 0 1 -3 104.90 2.81 0 -1 -3 129.74 2.95 0 -1 -3 95.00 3.21 0 1 3 123.84 2.82 0 1 -3 130.58 3.26 0 1 -4 1599.33 16.22 0 1 -4 1510.87 16.06 0 -1 4 1125.64 14.67 0 -1 -4 1107.57 15.38 0 -1 -4 1483.45 15.28 0 1 4 1517.15 15.30 0 -1 -5 180.14 5.26 0 1 -5 231.63 5.42 0 -1 -5 234.14 5.20 0 1 5 234.87 5.13 0 1 -5 155.78 4.60 0 -1 5 179.29 4.85 0 1 -5 254.85 5.72 0 1 6 6.78 1.07 0 1 -6 10.54 1.28 0 1 -6 5.31 0.90 0 -1 -6 8.87 1.11 0 1 -6 8.74 1.07 0 1 6 10.59 1.16 0 -1 6 6.52 0.99 0 -1 -6 7.70 1.17 0 -1 7 97.94 4.15 0 -1 -7 92.65 4.28 0 1 -7 133.80 4.67 0 -1 -7 124.10 4.38 0 1 -7 119.06 4.48 0 1 -8 199.01 6.05 0 -1 -8 198.20 6.00 0 1 -8 194.49 6.12 0 -1 9 51.35 3.58 0 -1 -9 60.19 3.48 0 1 -9 58.27 3.54 0 1 -9 60.17 3.55 0 -1 -10 185.70 6.68 0 1 -10 177.79 6.60 0 -1 10 155.39 6.25 0 1 -10 194.83 6.97 0 -1 -11 2.62 0.98 0 1 -11 0.80 0.90 0 1 -11 0.70 0.55 0 -1 11 1.35 0.88 0 -1 -12 31.20 3.11 0 1 -12 30.25 2.96 0 -1 12 29.29 3.07 0 1 -12 32.42 2.92 0 1 -13 15.15 2.14 0 -1 13 13.18 2.34 0 1 -13 11.39 1.68 0 -1 -13 15.39 2.20 0 1 -14 20.45 2.91 0 1 -14 19.82 2.66 0 -1 -14 19.79 2.72 0 -1 14 20.87 2.90 0 -1 -15 -0.31 0.93 0 1 -15 -0.48 0.87 0 -1 -15 0.86 0.72 0 1 -16 19.11 2.59 0 -1 -16 16.64 2.43 0 -1 -16 24.32 3.43 0 1 -16 27.21 3.77 0 -1 -17 23.27 3.24 0 -1 -17 25.85 3.74 0 1 -17 24.66 3.41 0 1 -17 22.91 3.33 0 -2 0 21.20 1.23 0 -2 -1 9.28 0.77 0 2 -1 9.59 0.71 0 -2 1 8.98 0.83 0 2 1 9.60 0.80 0 -2 -2 185.91 3.74 0 2 2 196.34 3.50 0 2 2 195.46 4.03 0 -2 2 199.50 4.41 0 2 -2 189.04 3.92 0 -2 3 62.24 2.64 0 -2 -3 86.68 2.68 0 2 3 82.57 2.35 0 2 -3 63.18 2.54 0 -2 3 91.46 3.17 0 -2 -3 81.93 2.42 0 2 3 90.85 2.75 0 2 -3 80.12 2.73 0 -2 -4 417.54 6.72 0 2 -4 396.51 7.38 0 -2 4 455.81 8.09 0 2 4 423.20 6.68 0 2 -4 437.82 7.67 0 -2 -4 373.80 8.23 0 -2 -4 433.11 6.92 0 -2 -5 7.71 0.99 0 2 5 7.57 0.88 0 2 5 6.04 0.56 0 2 -5 5.49 0.92 0 2 -5 6.14 0.99 0 2 -5 6.86 1.05 0 -2 -5 6.65 0.86 0 -2 5 5.44 0.76 0 -2 5 8.55 1.20 0 -2 -5 5.05 0.98 0 2 -6 3.46 0.84 0 -2 -6 5.78 0.85 0 -2 -6 5.41 1.05 0 -2 6 3.83 0.70 0 -2 -6 6.72 0.98 0 2 6 3.16 0.44 0 2 -6 6.48 0.99 0 2 6 7.38 1.05 0 2 -6 5.83 1.07 0 2 -7 22.32 2.00 0 -2 -7 26.17 1.91 0 2 -7 29.96 2.38 0 2 -7 22.71 1.88 0 -2 7 21.63 2.04 0 -2 -7 29.80 2.07 0 2 -8 467.22 10.19 0 2 -8 487.44 10.42 0 -2 8 423.53 9.93 0 -2 -8 510.45 10.09 0 2 -8 553.78 11.37 0 2 -9 7.88 1.44 0 -2 -9 9.39 1.45 0 2 -9 9.02 1.49 0 -2 9 6.78 1.27 0 2 -10 386.02 10.44 0 -2 10 345.70 9.95 0 -2 -10 360.06 9.38 0 2 -10 352.28 9.81 0 2 -11 3.05 0.57 0 2 -11 4.50 0.58 0 -2 11 7.06 1.48 0 2 -11 7.56 1.54 0 2 -11 7.21 1.46 0 -2 -11 7.84 1.47 0 -2 -12 17.20 2.30 0 -2 12 13.54 2.11 0 2 -12 13.97 1.93 0 2 -12 15.87 2.15 0 2 -13 6.16 1.43 0 2 -13 5.52 1.10 0 -2 13 6.16 1.67 0 -2 -13 8.34 1.50 0 -2 -13 7.15 1.36 0 -2 14 0.39 0.71 0 2 -14 2.15 1.14 0 -2 -14 0.14 0.62 0 -2 -14 1.36 1.37 0 2 -14 1.32 0.70 0 -2 -15 6.81 1.86 0 -2 -15 5.93 1.43 0 2 -15 4.81 1.55 0 2 -15 5.43 1.81 0 -2 -16 42.97 4.41 0 2 -16 34.62 3.88 0 2 -16 36.63 4.15 0 -2 -16 45.15 4.06 0 2 -17 1.85 1.65 0 -2 -17 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244.58 8.27 2 -3 -10 255.73 6.21 2 3 -10 240.33 8.15 -2 -3 10 239.38 6.34 2 -3 -9 3.39 0.67 -2 -3 9 1.77 0.56 2 3 -9 2.63 0.58 -2 3 9 2.72 0.59 2 3 -9 2.43 0.49 2 -3 -9 0.32 0.76 2 3 -9 5.46 1.26 -2 3 8 0.65 0.40 -2 3 8 0.44 0.35 -2 -3 8 0.20 0.28 2 3 -8 -0.41 0.56 2 3 -8 1.02 0.89 2 -3 -8 0.52 0.38 2 -3 -8 -0.28 0.46 -2 -3 7 10.96 1.05 2 -3 -7 15.81 1.27 -2 3 7 12.31 1.27 2 3 -7 15.40 1.79 2 -3 -7 14.31 1.19 -2 3 7 16.75 1.43 -2 -3 6 7.62 0.89 2 -3 -6 9.66 0.86 -2 3 6 10.44 1.14 2 -3 -6 10.01 0.92 -2 3 6 8.46 0.89 2 3 -6 10.33 1.27 -2 -3 5 34.09 1.89 -2 3 5 38.88 2.20 2 3 -5 37.45 2.51 2 -3 -5 37.19 1.51 -2 3 5 38.09 1.49 2 -3 -5 36.64 1.51 2 3 -5 31.79 2.38 -2 3 5 41.76 1.69 -2 -3 4 190.96 5.77 -2 3 4 153.90 2.62 -2 3 4 164.90 4.45 2 3 -4 145.17 4.79 2 -3 -4 161.88 3.33 -2 -3 4 162.63 5.06 -2 3 4 168.26 3.62 2 -3 -4 153.36 2.82 2 -3 -3 88.89 2.43 -2 -3 3 101.48 3.79 -2 3 3 95.82 2.58 -2 3 3 93.88 3.32 -2 -3 3 92.83 3.66 2 -3 -2 12.23 0.91 -2 3 2 12.17 1.19 -2 3 2 11.16 0.94 -2 -3 2 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164.00 6.84 5 6 -10 135.06 7.13 5 6 -9 19.98 2.64 -5 6 9 21.51 2.52 5 6 -9 18.66 2.33 -5 -6 9 18.55 1.73 5 6 -8 107.50 5.91 -5 -6 8 113.70 6.35 5 6 -8 107.45 6.10 -5 -6 8 91.72 4.15 -5 6 8 110.56 5.63 -5 6 8 89.47 2.81 -5 -6 7 40.04 3.59 5 6 -7 35.22 3.50 -5 6 7 37.24 3.22 -5 6 7 40.75 2.08 -5 -6 6 543.80 13.76 5 6 -6 513.62 12.94 -5 6 6 538.20 9.16 -5 6 6 532.04 12.61 -5 -6 6 565.88 11.43 5 -6 -5 13.15 2.05 -5 -6 5 12.18 1.92 -5 6 5 11.79 1.33 -5 6 5 11.64 1.86 5 -6 -4 197.01 8.03 -5 -6 4 185.06 7.52 -5 6 4 198.65 5.87 -5 6 4 193.72 7.25 -5 6 3 0.67 0.62 5 -6 -3 1.57 0.76 -5 -6 3 1.16 0.69 -5 6 2 6.97 1.47 5 -6 -2 7.15 1.60 -5 -6 2 8.02 1.64 -5 6 2 5.24 0.70 5 -6 -1 67.20 5.01 5 -6 -1 51.96 2.25 -5 -6 1 55.51 4.12 -5 6 1 52.49 2.25 -5 6 1 52.06 3.66 5 -6 0 3.08 0.82 5 -6 0 2.32 1.02 -5 6 0 1.48 0.67 -5 -6 0 2.08 0.92 -5 6 0 1.60 0.53 -5 6 -1 245.74 8.19 -5 -6 -1 250.32 8.71 -5 6 -1 233.16 5.93 5 -6 2 93.18 6.18 -5 -6 -2 104.98 5.71 -5 6 -2 103.92 4.16 -5 6 -2 101.85 5.15 5 -6 3 34.04 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7.06 1.39 -5 -7 -5 7.16 1.66 -5 7 -5 8.45 1.62 5 -7 6 86.01 6.83 -5 7 -6 81.06 5.02 -5 -7 -6 84.85 5.67 -5 7 -6 75.60 4.62 -5 7 -7 2.86 0.70 -5 7 -7 6.55 1.77 -5 -7 -7 5.99 1.60 -5 7 -8 23.96 2.70 5 -7 8 30.67 4.13 -5 -7 -8 27.29 3.39 -5 7 -8 27.02 3.21 5 -7 9 116.91 8.22 -5 -7 -9 104.37 6.76 -5 7 -9 98.66 5.94 -5 7 -9 97.52 5.57 5 -7 10 22.44 3.65 -5 7 -10 16.26 2.19 -5 7 -10 16.23 2.74 -5 -7 -10 21.94 3.17 5 -7 11 2.62 1.90 -5 7 -11 -0.47 1.03 -5 -7 -11 0.76 0.98 5 -7 12 1.78 0.82 -5 7 -12 -0.16 1.22 -5 -7 -12 1.46 1.17 5 8 -15 1.85 1.83 5 8 -15 0.28 1.44 5 8 -14 38.57 4.70 5 8 -14 39.17 4.69 5 8 -13 1.63 1.64 5 8 -13 3.96 2.08 5 8 -12 3.64 1.43 -5 8 12 1.51 0.71 5 8 -12 -0.02 1.54 5 8 -11 35.22 4.15 -5 8 11 38.89 3.74 5 8 -11 31.90 4.03 5 8 -10 3.23 1.74 -5 8 10 2.09 1.16 5 8 -9 121.90 7.11 -5 8 9 115.79 6.43 5 8 -8 65.37 5.10 -5 -8 8 51.71 3.94 -5 -8 8 60.36 5.14 -5 8 8 61.65 4.72 -5 -8 7 68.25 5.34 5 8 -7 70.98 5.10 -5 8 7 71.50 4.97 -5 8 6 149.93 7.47 -5 -8 6 143.29 7.70 -5 8 5 116.32 6.36 5 -8 -5 108.49 6.74 -5 -8 5 109.50 6.69 -5 -8 4 31.07 3.42 5 -8 -4 30.82 3.60 -5 8 4 29.91 3.16 5 -8 -3 4.27 1.42 -5 -8 3 3.18 1.02 -5 8 3 4.83 1.35 -5 -8 2 44.89 4.06 5 -8 -2 44.97 4.43 -5 8 2 43.13 3.76 5 -8 -1 267.81 11.43 -5 8 1 267.63 5.62 -5 8 1 281.19 9.79 -5 -8 1 292.48 10.69 5 -8 0 61.38 5.54 -5 -8 0 62.40 4.85 -5 8 0 58.20 2.84 -5 8 0 62.53 4.60 -5 -8 -1 1.82 0.62 5 -8 1 2.58 1.20 -5 8 -1 3.24 1.05 -5 8 -1 2.48 0.89 5 -8 2 7.54 2.36 -5 -8 -2 6.10 1.66 -5 8 -2 6.19 1.33 -5 8 -2 6.77 1.15 5 -8 3 231.59 10.95 -5 -8 -3 256.45 10.01 -5 8 -3 250.73 7.34 -5 8 -3 243.51 9.23 5 -8 4 2.27 1.28 -5 8 -4 1.18 0.88 -5 -8 -4 -1.09 0.77 -5 8 -4 0.55 0.80 5 -8 5 53.89 5.59 -5 -8 -5 64.73 4.94 -5 8 -5 63.22 4.71 -5 8 -5 62.33 4.06 5 -8 6 70.86 6.63 -5 8 -6 70.37 4.94 -5 -8 -6 76.97 5.58 -5 8 -6 76.34 4.71 5 -8 7 8.57 2.75 -5 8 -7 8.76 1.75 -5 -8 -7 10.38 2.10 -5 8 -7 9.96 1.93 -5 8 -8 8.10 1.74 5 -8 8 6.60 2.42 -5 -8 -8 6.35 1.88 -5 8 -8 7.49 1.75 -5 8 -9 3.69 1.45 -5 -8 -9 5.22 1.58 -5 8 -9 5.11 1.71 5 -8 10 9.18 2.51 -5 8 -10 4.35 1.34 -5 8 -10 7.31 1.92 -5 -8 -10 6.15 1.81 5 -8 11 0.54 0.89 -5 8 -11 2.03 1.05 -5 -8 -11 2.37 1.50 5 9 -14 5.42 1.49 5 9 -13 32.60 4.35 5 9 -12 33.75 4.10 -5 9 12 29.35 3.51 5 9 -11 -1.03 1.09 -5 9 11 0.78 1.12 5 9 -10 71.53 5.72 -5 9 10 69.24 5.28 -5 9 9 1.04 0.92 5 9 -9 0.90 1.32 5 9 -8 265.57 10.73 -5 -9 8 245.14 11.06 -5 9 8 249.84 10.07 5 9 -7 -0.19 0.93 -5 -9 7 -0.44 0.82 -5 9 7 1.16 0.87 -5 -9 6 53.54 4.84 -5 9 6 58.24 4.84 5 -9 -5 27.50 3.54 -5 -9 5 33.43 3.89 -5 9 5 32.96 3.47 5 -9 -4 24.93 3.44 -5 -9 4 22.97 3.09 -5 9 4 24.87 3.01 5 -9 -3 3.55 1.50 -5 -9 3 3.36 1.48 -5 9 3 5.11 1.53 5 -9 -2 183.27 9.58 -5 -9 2 194.38 9.07 -5 9 2 197.53 8.66 5 -9 -1 51.88 5.20 -5 -9 1 57.04 4.84 -5 9 1 57.16 4.59 -5 -9 0 119.41 7.11 5 -9 0 113.22 7.93 -5 9 0 104.08 3.92 -5 9 0 111.79 6.49 5 -9 1 15.98 2.95 -5 -9 -1 21.43 3.06 -5 9 -1 19.72 1.86 -5 9 -1 18.24 2.64 5 -9 2 23.08 3.73 -5 -9 -2 25.54 3.36 -5 9 -2 23.46 2.09 -5 9 -2 24.67 3.06 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7.36 1.92 -14 3 6 8.42 2.36 14 -3 -5 6.79 1.74 -14 -3 5 4.70 1.33 -14 3 5 7.26 2.06 14 3 -5 6.81 1.88 14 -3 -4 26.79 3.69 -14 -3 4 25.71 3.56 14 3 -4 26.53 4.11 -14 3 4 24.69 3.58 -14 3 3 -0.74 0.73 14 -3 -3 0.52 0.73 -14 -3 3 -1.06 1.18 -14 3 3 1.89 1.34 14 3 -3 -0.18 0.78 -14 3 2 10.38 1.97 14 -3 -2 11.42 2.65 -14 -3 2 9.37 2.29 -14 3 2 9.29 2.13 14 3 -2 8.38 2.54 14 -3 -1 2.54 1.50 -14 3 1 1.31 0.87 -14 -3 1 1.06 1.08 -14 3 1 1.51 1.26 14 3 -1 0.60 1.09 -14 3 0 0.79 1.24 -14 -3 0 1.44 1.18 -14 3 0 -0.08 0.71 14 3 0 -0.46 1.09 14 -3 1 0.68 0.87 -14 3 -1 0.42 0.55 -14 3 -1 0.99 0.62 -14 -3 -1 1.91 1.53 14 3 1 -0.37 1.22 14 -3 2 1.94 1.56 -14 3 -2 0.46 0.62 -14 3 -2 -0.03 0.86 -14 -3 -2 1.26 1.38 14 3 2 0.40 0.99 14 -3 3 11.11 3.10 -14 3 -3 8.53 2.13 -14 3 -3 9.49 2.27 -14 -3 -3 12.74 2.58 14 3 3 13.82 3.56 14 4 -11 2.26 1.14 -14 4 11 0.59 0.88 -14 4 10 64.43 6.07 -14 4 9 34.99 4.46 14 -4 -8 4.35 1.55 -14 -4 8 6.92 1.77 -14 4 8 8.07 2.24 14 -4 -7 51.25 5.08 -14 -4 7 53.70 5.11 -14 4 7 53.66 5.45 -14 4 6 13.67 2.77 14 -4 -6 11.54 2.51 -14 -4 6 11.89 2.38 -14 4 5 2.88 1.64 14 -4 -5 1.44 1.07 -14 -4 5 2.73 1.47 14 -4 -4 79.36 6.75 -14 -4 4 73.85 6.09 -14 4 4 73.53 6.19 -14 4 3 0.40 0.98 14 -4 -3 0.17 0.73 -14 -4 3 -0.50 0.95 14 4 -3 1.68 1.44 -14 4 2 2.40 1.11 14 -4 -2 1.65 0.99 -14 4 2 2.74 1.32 -14 -4 2 2.31 1.65 14 4 -2 1.44 1.37 14 -4 -1 81.87 7.14 -14 4 1 72.44 6.15 -14 -4 1 72.38 6.09 -14 4 1 76.15 5.59 14 4 -1 85.79 7.75 -14 4 0 1.39 1.29 14 -4 0 1.59 1.33 -14 4 0 1.58 1.09 -14 -4 0 1.45 1.51 14 4 0 1.44 1.07 -14 4 -1 0.53 1.03 14 -4 1 1.73 1.61 -14 4 -1 0.27 0.90 -14 -4 -1 4.12 1.89 14 4 1 -0.43 1.23 -14 4 -2 5.04 1.95 14 -4 2 4.99 2.10 -14 4 -2 3.25 1.31 -14 -4 -2 3.71 1.50 14 4 2 5.46 2.09 -14 5 10 26.70 3.94 -14 -5 9 41.75 4.53 -14 5 9 39.74 4.71 14 -5 -8 57.47 5.46 -14 -5 8 62.07 5.54 -14 5 8 61.35 5.86 14 -5 -7 28.08 3.91 -14 -5 7 31.91 3.99 -14 5 7 34.78 4.36 -14 5 6 6.78 2.01 14 -5 -6 5.45 1.86 -14 -5 6 6.77 1.97 14 -5 -5 12.75 2.71 -14 5 5 16.12 2.97 -14 -5 5 12.23 2.55 14 -5 -4 39.22 4.78 -14 -5 4 39.01 4.56 -14 5 4 36.06 4.44 14 -5 -3 15.42 3.04 -14 5 3 13.62 2.84 -14 -5 3 11.46 2.56 14 -5 -2 30.35 4.46 -14 5 2 23.99 3.43 -14 -5 2 27.37 3.87 14 -5 -1 47.26 5.54 -14 -5 1 45.06 5.11 -14 5 1 42.99 4.62 14 5 -1 49.99 5.94 -14 5 1 41.47 4.02 14 -5 0 23.11 4.10 -14 5 0 21.36 3.27 -14 5 0 23.28 3.14 -14 -5 0 23.71 3.74 14 5 0 27.93 4.80 14 -5 1 15.48 3.47 -14 5 -1 11.05 2.52 -14 -5 -1 13.82 2.77 14 5 1 13.56 3.44 -14 -6 9 47.61 5.13 -14 6 9 42.15 4.88 14 -6 -8 27.78 3.96 -14 6 8 26.66 3.94 -14 -6 8 24.37 3.74 14 -6 -7 16.55 2.97 -14 6 7 19.11 3.33 -14 -6 7 14.47 2.90 14 -6 -6 0.79 0.89 -14 6 6 3.26 1.46 -14 -6 6 0.77 0.75 -14 6 5 12.09 2.62 -14 -6 5 12.88 2.91 14 -6 -4 36.07 4.82 -14 -6 4 32.73 4.33 -14 6 4 35.58 4.36 14 -6 -3 15.03 3.11 -14 6 3 15.81 2.92 -14 -6 3 14.64 2.96 14 -6 -2 5.70 1.93 -14 6 2 4.89 1.49 -14 -6 2 4.50 1.72 14 -6 -1 3.13 1.38 -14 6 1 2.75 1.45 -14 -6 1 3.44 1.73 -15 0 11 7.87 2.39 -15 0 10 0.40 0.84 -15 0 9 35.17 4.58 -15 0 8 -0.27 0.95 -15 0 7 60.98 5.96 15 0 -6 0.40 0.53 -15 0 6 0.56 1.39 -15 0 5 45.81 5.14 15 0 -5 55.43 5.63 15 0 -4 0.03 0.64 -15 0 4 -0.66 0.82 -15 0 4 0.59 1.03 -15 0 3 60.53 5.85 -15 0 3 68.75 5.70 15 0 -3 71.22 6.85 15 0 -2 1.58 1.32 -15 0 2 0.56 0.92 -15 0 2 1.41 1.13 -15 0 1 101.46 7.67 -15 0 1 105.38 7.42 -15 0 0 0.67 1.09 15 0 0 -0.55 0.85 -15 0 0 1.75 1.36 -15 0 -1 28.77 3.93 -15 0 -1 25.56 3.68 15 0 1 32.46 5.17 -15 1 11 2.04 1.29 -15 -1 10 15.82 3.24 -15 1 10 13.34 2.92 -15 -1 9 33.77 4.33 -15 1 9 33.12 4.38 -15 -1 8 1.99 1.17 -15 1 8 3.10 1.09 -15 -1 7 33.86 4.44 -15 1 7 36.40 4.58 15 -1 -6 -0.59 0.53 -15 -1 6 -0.51 1.09 -15 1 6 1.25 1.35 -15 -1 5 37.48 4.69 -15 1 5 42.15 4.92 -15 -1 5 47.66 4.46 15 1 -5 52.36 5.48 15 -1 -5 48.76 5.11 15 1 -4 0.13 0.54 15 -1 -4 0.02 0.46 -15 -1 4 -0.94 0.94 -15 1 4 1.45 1.65 -15 -1 4 0.03 0.78 15 1 -3 19.23 3.63 15 -1 -3 14.41 2.90 -15 -1 3 14.76 2.80 -15 1 3 14.90 2.90 -15 -1 3 15.52 2.64 -15 1 3 17.73 2.68 15 1 -2 1.58 0.76 15 -1 -2 0.45 0.49 -15 -1 2 0.24 0.65 -15 1 2 2.29 1.69 -15 -1 2 -0.01 1.12 -15 1 2 2.22 1.22 -15 1 1 8.13 1.91 15 1 -1 4.46 1.87 15 -1 -1 4.58 1.51 -15 -1 1 4.83 1.48 -15 1 1 3.70 1.39 -15 -1 1 4.73 1.75 15 1 0 -1.28 0.95 -15 1 0 -0.37 0.64 15 -1 0 0.45 1.02 -15 -1 0 -0.63 1.04 -15 1 0 -0.66 0.55 -15 -1 0 0.30 0.73 15 1 1 0.35 1.03 15 -1 1 3.20 1.91 -15 1 -1 1.60 1.17 -15 -1 -1 1.08 0.65 -15 1 -1 0.07 0.67 -15 2 11 51.43 5.58 -15 2 10 1.58 1.48 -15 2 9 78.78 6.84 -15 2 8 12.82 2.78 -15 2 7 2.97 1.31 -15 2 6 41.23 4.78 15 -2 -6 51.09 5.25 -15 2 5 35.57 4.56 -15 -2 5 37.32 4.29 15 -2 -5 37.87 4.64 15 2 -4 -0.45 0.77 -15 2 4 -1.38 1.47 -15 -2 4 0.37 0.83 -15 2 3 67.40 6.29 -15 -2 3 68.72 5.83 15 2 -3 70.40 6.81 15 -2 -3 73.64 6.94 15 2 -2 0.35 1.02 -15 2 2 1.87 1.25 15 -2 -2 0.73 0.51 -15 2 2 0.26 0.80 -15 -2 2 -1.03 0.59 15 2 -1 2.62 1.71 -15 2 1 -0.08 1.05 15 -2 -1 3.53 1.77 -15 2 1 1.42 0.94 -15 -2 1 2.40 1.52 15 2 0 2.83 1.87 -15 2 0 4.90 1.53 15 -2 0 2.81 1.44 -15 2 0 4.86 1.79 -15 -2 0 3.71 1.46 15 2 1 2.76 1.71 15 -2 1 -0.31 0.68 -15 2 -1 1.29 0.91 -15 2 -1 1.38 1.13 -15 -2 -1 0.71 0.65 -15 3 10 6.39 2.33 -15 3 9 7.24 2.14 -15 3 8 1.98 1.56 15 -3 -7 16.59 2.83 -15 3 7 19.47 3.41 15 -3 -6 12.71 2.61 -15 -3 6 11.41 2.42 -15 3 6 12.33 2.68 15 -3 -5 20.90 3.41 -15 -3 5 19.10 2.94 -15 3 5 16.15 3.10 15 -3 -4 1.76 0.81 -15 -3 4 0.39 0.94 -15 3 4 1.36 1.56 15 3 -4 4.36 1.80 15 -3 -3 9.57 2.54 -15 -3 3 8.17 2.36 -15 3 3 6.47 1.92 15 3 -3 10.53 2.72 15 -3 -2 1.58 0.85 -15 -3 2 1.27 0.91 -15 3 2 0.32 0.95 15 3 -2 1.80 1.24 -15 3 1 2.10 1.17 15 -3 -1 3.44 1.82 -15 -3 1 3.32 1.37 -15 3 1 3.11 1.28 15 3 -1 2.24 1.50 -15 3 0 2.13 1.00 -15 3 0 1.21 0.73 -15 -3 0 1.86 1.36 15 3 0 2.27 2.11 -15 4 9 13.69 3.07 -15 4 8 12.09 2.79 15 -4 -7 50.14 5.13 -15 -4 7 49.78 5.14 -15 4 7 52.63 5.60 15 -4 -6 22.30 3.50 -15 -4 6 23.44 3.50 -15 4 6 18.60 3.30 15 -4 -5 14.22 2.78 -15 -4 5 13.35 2.80 -15 4 5 13.99 2.78 15 -4 -4 2.69 1.56 -15 -4 4 2.89 1.52 -15 4 4 4.72 1.75 15 -4 -3 10.50 2.54 -15 -4 3 6.96 2.05 15 4 -3 9.30 2.80 -15 4 3 10.43 2.53 15 -4 -2 2.00 1.27 -15 -4 2 1.46 0.85 15 4 -2 2.35 1.46 -15 4 2 1.85 1.41 15 -4 -1 5.47 2.18 -15 -4 1 5.19 1.59 15 4 -1 5.26 2.12 -15 4 1 3.67 1.64 15 -5 -6 37.46 4.81 -15 -5 6 41.12 4.85 -15 5 6 42.05 4.99 -15 5 5 12.99 2.88 15 -5 -5 13.11 2.83 -15 -5 5 12.50 2.65 -15 5 4 15.03 2.98 15 -5 -4 15.70 3.15 -15 -5 4 16.69 3.26 -16 0 7 -1.10 0.87 -16 0 6 31.28 4.46 16 0 -5 -0.23 0.85 -16 0 5 0.69 1.01 -16 0 4 48.11 5.44 16 0 -4 52.81 5.85 -16 -1 7 2.22 1.36 -16 1 7 0.19 1.36 -16 -1 6 49.17 5.61 -16 1 6 48.22 5.42 16 -1 -5 5.99 1.88 -16 -1 5 4.14 1.49 -16 1 5 6.24 1.77 16 -1 -4 20.04 3.53 -16 -1 4 21.57 3.49 -16 1 4 19.22 3.36 16 1 -4 23.52 3.90 0 0 0 0.00 0.00 TITL exp_984_rint02_frame50_d08 in P2/n REM P2/n (#13 in standard setting) CELL 0.71073 12.926386 11.170186 15.056388 90.0000 106.5587 90.0000 ZERR 5.00 0.000522 0.000424 0.000961 0.0000 0.0057 0.0000 LATT 1 SYMM -x+1/2, y,-z+1/2 SFAC C H N O Cl Cu UNIT 50.00 40.00 10.00 40.00 10.00 5.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 64179 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' 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 Cu1 Cu 0.250000 0.47394(3) 0.250000 0.02379(15) Uani 1 2 d S T P . . Cl1 Cl 0.58367(6) 0.78826(7) 0.39866(5) 0.0478(2) Uani 1 1 d . U . . . N2 N 0.250000 0.6566(2) 0.250000 0.0252(6) Uani 1 2 d S T P . . O1 O 0.41778(15) 0.48385(17) 0.38257(14) 0.0378(4) Uani 1 1 d . . . . . H1A H 0.450206 0.554318 0.384843 0.057 Uiso 1 1 d GR . . . . H1B H 0.467141 0.433105 0.374578 0.057 Uiso 1 1 d GR . . . . N1 N 0.15847(16) 0.47686(17) 0.34236(14) 0.0265(4) Uani 1 1 d . . . . . N3 N 0.250000 1.2909(2) 0.250000 0.0250(6) Uani 1 2 d S T P . . C6 C 0.2659(2) 0.7190(2) 0.32870(17) 0.0299(5) Uani 1 1 d . . . . . H6 H 0.277684 0.677070 0.384051 0.036 Uiso 1 1 calc R . . . . O3 O 0.5538(3) 0.6955(3) 0.4519(2) 0.0881(10) Uani 1 1 d . U . . . C7 C 0.2658(2) 0.8419(2) 0.33172(17) 0.0319(5) Uani 1 1 d . . . . . H7 H 0.276153 0.881401 0.387936 0.038 Uiso 1 1 calc R . . . . C4 C -0.0004(2) 0.5455(3) 0.37892(19) 0.0357(6) Uani 1 1 d . . . . . H4 H -0.065737 0.586286 0.360042 0.043 Uiso 1 1 calc R . . . . C5 C 0.0630(2) 0.5345(2) 0.31922(19) 0.0344(6) Uani 1 1 d . . . . . H5 H 0.038611 0.568483 0.260547 0.041 Uiso 1 1 calc R . . . . C9 C 0.250000 1.0396(3) 0.250000 0.0270(7) Uani 1 2 d S T P . . C10 C 0.3179(2) 1.1044(2) 0.32204(18) 0.0348(6) Uani 1 1 d . . . . . H10 H 0.364292 1.064612 0.371968 0.042 Uiso 1 1 calc R . . . . C3 C 0.03328(19) 0.4958(2) 0.46676(17) 0.0282(5) Uani 1 1 d . . . . . C11 C 0.3164(2) 1.2282(2) 0.31939(18) 0.0333(6) Uani 1 1 d . . . . . H11 H 0.363418 1.269993 0.367761 0.040 Uiso 1 1 calc R . . . . C8 C 0.250000 0.9068(3) 0.250000 0.0255(7) Uani 1 2 d S T P . . C2 C 0.1329(2) 0.4366(3) 0.49046(18) 0.0363(6) Uani 1 1 d . . . . . H2 H 0.159239 0.401768 0.548660 0.044 Uiso 1 1 calc R . . . . C1 C 0.1921(2) 0.4299(2) 0.42697(18) 0.0338(6) Uani 1 1 d . . . . . H1 H 0.258353 0.390808 0.444305 0.041 Uiso 1 1 calc R . . . . O6 O 0.750000 0.6526(5) 0.250000 0.0905(13) Uani 1 2 d S T P . . O4 O 0.5404(3) 0.8971(3) 0.4197(4) 0.1199(14) Uani 1 1 d . U . . . O2 O 0.5368(5) 0.7630(5) 0.3062(3) 0.163(2) Uani 1 1 d . U . . . O5 O 0.6956(3) 0.8006(4) 0.4242(4) 0.144(2) Uani 1 1 d . U . . . N4 N 0.5917(2) 0.3198(3) 0.3926(2) 0.0593(8) Uani 1 1 d . . . . . C14 C 0.6050(3) 0.2043(4) 0.4127(3) 0.0609(9) Uani 1 1 d . . . . . H14 H 0.550724 0.164922 0.430512 0.073 Uiso 1 1 calc R . . . . C12 C 0.6716(3) 0.3736(3) 0.3681(3) 0.0669(10) Uani 1 1 d . . . . . H12 H 0.664505 0.454629 0.353340 0.080 Uiso 1 1 calc R . . . . C16 C 0.7775(2) 0.1944(3) 0.3831(2) 0.0432(7) Uani 1 1 d . . . . . C15 C 0.6944(2) 0.1382(3) 0.4089(2) 0.0516(8) Uani 1 1 d . . . . . H15 H 0.698832 0.057072 0.423407 0.062 Uiso 1 1 calc R . . . . C17 C 0.8759(2) 0.1277(3) 0.3788(2) 0.0477(7) Uani 1 1 d . . . . . C13 C 0.7638(3) 0.3157(3) 0.3637(3) 0.0631(10) Uani 1 1 d . . . . . H13 H 0.817504 0.358255 0.347547 0.076 Uiso 1 1 calc R . . . . N5 N 1.0662(3) 0.0060(4) 0.3766(3) 0.0882(13) Uani 1 1 d . . . . . C20 C 0.8771(3) 0.0066(4) 0.3671(4) 0.0772(13) Uani 1 1 d . . . . . H20 H 0.814744 -0.038368 0.360253 0.093 Uiso 1 1 calc R . . . . C18 C 0.9713(3) 0.1852(4) 0.3866(5) 0.109(2) Uani 1 1 d . . . . . H18 H 0.975113 0.268150 0.391872 0.131 Uiso 1 1 calc R . . . . C21 C 0.9734(4) -0.0489(4) 0.3654(4) 0.0934(17) Uani 1 1 d . . . . . H21 H 0.971755 -0.131168 0.355474 0.112 Uiso 1 1 calc R . . . . C19 C 1.0628(4) 0.1194(5) 0.3867(6) 0.128(3) Uani 1 1 d . . . . . H19 H 1.126875 0.161508 0.394746 0.154 Uiso 1 1 calc R . . . . 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 Cu1 0.0309(2) 0.0131(2) 0.0367(2) 0.000 0.02475(18) 0.000 Cl1 0.0492(4) 0.0416(4) 0.0528(4) 0.0037(3) 0.0147(3) -0.0083(3) N2 0.0292(13) 0.0173(13) 0.0336(14) 0.000 0.0163(11) 0.000 O1 0.0340(10) 0.0315(10) 0.0489(11) 0.0022(8) 0.0136(8) -0.0013(7) N1 0.0283(10) 0.0230(10) 0.0354(11) 0.0025(8) 0.0208(8) 0.0016(8) N3 0.0246(13) 0.0151(12) 0.0396(15) 0.000 0.0162(11) 0.000 C6 0.0405(13) 0.0212(11) 0.0314(12) 0.0020(9) 0.0156(10) 0.0030(10) O3 0.100(2) 0.075(2) 0.087(2) 0.0188(16) 0.0226(17) -0.0316(18) C7 0.0429(14) 0.0220(12) 0.0311(12) -0.0033(10) 0.0113(10) 0.0016(10) C4 0.0316(12) 0.0420(15) 0.0407(14) 0.0090(11) 0.0217(11) 0.0131(11) C5 0.0365(13) 0.0387(15) 0.0355(13) 0.0099(11) 0.0225(11) 0.0106(11) C9 0.0287(16) 0.0176(16) 0.0357(18) 0.000 0.0107(14) 0.000 C10 0.0360(13) 0.0203(12) 0.0417(14) 0.0012(10) 0.0006(11) 0.0033(10) C3 0.0265(11) 0.0309(12) 0.0340(12) 0.0029(10) 0.0197(10) 0.0034(9) C11 0.0333(12) 0.0212(12) 0.0420(14) -0.0053(10) 0.0053(11) -0.0028(10) C8 0.0224(14) 0.0175(15) 0.0356(17) 0.000 0.0065(13) 0.000 C2 0.0328(13) 0.0475(16) 0.0348(13) 0.0110(12) 0.0196(11) 0.0114(12) C1 0.0296(12) 0.0376(14) 0.0416(14) 0.0071(11) 0.0220(11) 0.0102(10) O6 0.070(3) 0.093(3) 0.106(3) 0.000 0.021(2) 0.000 O4 0.110(3) 0.057(2) 0.206(4) -0.010(2) 0.067(3) 0.0017(19) O2 0.272(6) 0.149(4) 0.061(2) -0.010(2) 0.034(3) -0.085(4) O5 0.0527(18) 0.098(3) 0.276(6) 0.043(3) 0.040(3) -0.0088(18) N4 0.0369(13) 0.0577(18) 0.083(2) 0.0012(15) 0.0160(13) 0.0041(12) C14 0.0376(16) 0.067(2) 0.082(2) 0.0122(19) 0.0240(16) 0.0004(15) C12 0.0486(18) 0.047(2) 0.104(3) 0.0037(19) 0.0199(19) 0.0004(16) C16 0.0351(14) 0.0463(17) 0.0506(16) -0.0080(13) 0.0158(12) -0.0077(12) C15 0.0423(16) 0.0454(18) 0.072(2) 0.0049(16) 0.0238(15) -0.0026(14) C17 0.0410(15) 0.0480(18) 0.0606(19) -0.0083(14) 0.0253(14) -0.0048(13) C13 0.0423(17) 0.049(2) 0.104(3) 0.0041(19) 0.0303(18) -0.0094(15) N5 0.067(2) 0.083(3) 0.134(4) -0.019(3) 0.060(2) 0.009(2) C20 0.059(2) 0.059(2) 0.120(4) -0.030(2) 0.035(2) -0.0092(19) C18 0.056(2) 0.054(2) 0.238(7) -0.031(3) 0.075(3) -0.0130(19) C21 0.085(3) 0.066(3) 0.140(5) -0.036(3) 0.049(3) 0.007(2) C19 0.062(3) 0.078(3) 0.271(9) -0.031(4) 0.092(4) -0.010(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' Cu Cu 0.3201 1.2651 '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' 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 N2 Cu1 O1 87.46(4) . . N2 Cu1 N1 89.09(5) . . N2 Cu1 N1 89.09(5) . 2 N2 Cu1 N3 180.0 . 1_545 N1 Cu1 O1 90.22(7) 2 . N1 Cu1 O1 89.70(7) . . N1 Cu1 N1 178.19(11) . 2 N3 Cu1 O1 92.54(4) 1_545 . N3 Cu1 N1 90.91(5) 1_545 . N3 Cu1 N1 90.91(5) 1_545 2 O4 Cl1 O3 108.1(2) . . O2 Cl1 O3 107.9(2) . . O2 Cl1 O4 108.3(4) . . O2 Cl1 O5 114.9(4) . . O5 Cl1 O3 110.0(2) . . O5 Cl1 O4 107.5(3) . . C6 N2 Cu1 121.36(14) . . C6 N2 Cu1 121.36(14) 2 . C6 N2 C6 117.3(3) 2 . Cu1 O1 H1A 111.3 . . Cu1 O1 H1B 111.0 . . H1A O1 H1B 102.8 . . C5 N1 Cu1 119.44(16) . . C1 N1 Cu1 122.98(16) . . C1 N1 C5 117.5(2) . . C11 N3 Cu1 121.35(14) . 1_565 C11 N3 Cu1 121.36(14) 2 1_565 C11 N3 C11 117.3(3) 2 . N2 C6 H6 118.4 . . N2 C6 C7 123.2(2) . . C7 C6 H6 118.4 . . C6 C7 H7 120.2 . . C6 C7 C8 119.5(2) . . C8 C7 H7 120.2 . . C5 C4 H4 119.9 . . C5 C4 C3 120.1(2) . . C3 C4 H4 119.9 . . N1 C5 C4 122.9(2) . . N1 C5 H5 118.6 . . C4 C5 H5 118.6 . . C10 C9 C10 117.2(3) 2 . C10 C9 C8 121.42(15) 2 . C10 C9 C8 121.42(15) . . C9 C10 H10 120.1 . . C11 C10 C9 119.9(2) . . C11 C10 H10 120.1 . . C4 C3 C3 121.9(3) . 3_566 C4 C3 C2 116.7(2) . . C2 C3 C3 121.4(3) . 3_566 N3 C11 C10 122.9(2) . . N3 C11 H11 118.6 . . C10 C11 H11 118.6 . . C7 C8 C7 117.2(3) 2 . C7 C8 C9 121.40(15) . . C7 C8 C9 121.41(15) 2 . C3 C2 H2 120.1 . . C1 C2 C3 119.9(2) . . C1 C2 H2 120.1 . . N1 C1 C2 123.0(2) . . N1 C1 H1 118.5 . . C2 C1 H1 118.5 . . C14 N4 C12 116.2(3) . . N4 C14 H14 117.8 . . N4 C14 C15 124.4(3) . . C15 C14 H14 117.8 . . N4 C12 H12 118.3 . . N4 C12 C13 123.4(4) . . C13 C12 H12 118.3 . . C15 C16 C17 121.5(3) . . C13 C16 C15 115.9(3) . . C13 C16 C17 122.6(3) . . C14 C15 C16 119.4(3) . . C14 C15 H15 120.3 . . C16 C15 H15 120.3 . . C20 C17 C16 122.8(3) . . C18 C17 C16 121.5(3) . . C18 C17 C20 115.7(3) . . C12 C13 C16 120.7(3) . . C12 C13 H13 119.6 . . C16 C13 H13 119.6 . . C19 N5 C21 114.7(4) . . C17 C20 H20 120.5 . . C17 C20 C21 119.0(4) . . C21 C20 H20 120.5 . . C17 C18 H18 120.1 . . C17 C18 C19 119.9(4) . . C19 C18 H18 120.1 . . N5 C21 C20 125.2(4) . . N5 C21 H21 117.4 . . C20 C21 H21 117.4 . . N5 C19 C18 125.5(4) . . N5 C19 H19 117.2 . . C18 C19 H19 117.2 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cu1 N2 2.041(3) . Cu1 O1 2.4965(19) . Cu1 N1 2.0670(19) . Cu1 N1 2.0670(19) 2 Cu1 N3 2.045(3) 1_545 Cl1 O3 1.429(3) . Cl1 O4 1.412(4) . Cl1 O2 1.380(4) . Cl1 O5 1.393(3) . N2 C6 1.339(3) 2 N2 C6 1.339(3) . O1 H1A 0.8878 . O1 H1B 0.8869 . N1 C5 1.347(3) . N1 C1 1.331(3) . N3 C11 1.344(3) 2 N3 C11 1.344(3) . C6 H6 0.9300 . C6 C7 1.373(3) . C7 H7 0.9300 . C7 C8 1.392(3) . C4 H4 0.9300 . C4 C5 1.383(4) . C4 C3 1.385(4) . C5 H5 0.9300 . C9 C10 1.389(3) . C9 C10 1.389(3) 2 C9 C8 1.483(5) . C10 H10 0.9300 . C10 C11 1.384(3) . C3 C3 1.497(4) 3_566 C3 C2 1.400(3) . C11 H11 0.9300 . C2 H2 0.9300 . C2 C1 1.387(3) . C1 H1 0.9300 . N4 C14 1.326(5) . N4 C12 1.333(5) . C14 H14 0.9300 . C14 C15 1.387(5) . C12 H12 0.9300 . C12 C13 1.375(5) . C16 C15 1.391(4) . C16 C17 1.491(4) . C16 C13 1.387(5) . C15 H15 0.9300 . C17 C20 1.366(5) . C17 C18 1.365(5) . C13 H13 0.9300 . N5 C21 1.313(6) . N5 C19 1.278(6) . C20 H20 0.9300 . C20 C21 1.398(6) . C18 H18 0.9300 . C18 C19 1.393(6) . C21 H21 0.9300 . C19 H19 0.9300 . 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 Cu1 N2 C6 C7 -179.51(19) . . . . Cu1 N1 C5 C4 -176.8(2) . . . . Cu1 N1 C1 C2 177.0(2) . . . . Cu1 N3 C11 C10 179.4(2) 1_565 . . . N2 C6 C7 C8 -1.0(4) . . . . C6 N2 C6 C7 0.49(19) 2 . . . C6 C7 C8 C7 0.45(17) . . . 2 C6 C7 C8 C9 -179.55(17) . . . . C4 C3 C2 C1 -0.1(4) . . . . C5 N1 C1 C2 0.9(4) . . . . C5 C4 C3 C3 -179.3(3) . . . 3_566 C5 C4 C3 C2 0.5(4) . . . . C9 C10 C11 N3 1.1(4) . . . . C10 C9 C10 C11 -0.54(19) 2 . . . C10 C9 C8 C7 35.76(19) . . . . C10 C9 C8 C7 -144.24(19) 2 . . . C10 C9 C8 C7 35.76(19) 2 . . 2 C10 C9 C8 C7 -144.24(19) . . . 2 C3 C4 C5 N1 -0.2(4) . . . . C3 C3 C2 C1 179.7(3) 3_566 . . . C3 C2 C1 N1 -0.6(4) . . . . C11 N3 C11 C10 -0.6(2) 2 . . . C8 C9 C10 C11 179.46(19) . . . . C1 N1 C5 C4 -0.6(4) . . . . N4 C14 C15 C16 0.5(6) . . . . N4 C12 C13 C16 1.4(7) . . . . C14 N4 C12 C13 -0.3(6) . . . . C12 N4 C14 C15 -0.6(6) . . . . C16 C17 C20 C21 -179.0(4) . . . . C16 C17 C18 C19 177.0(6) . . . . C15 C16 C17 C20 23.8(5) . . . . C15 C16 C17 C18 -156.2(5) . . . . C15 C16 C13 C12 -1.5(6) . . . . C17 C16 C15 C14 179.4(3) . . . . C17 C16 C13 C12 179.8(3) . . . . C17 C20 C21 N5 1.8(9) . . . . C17 C18 C19 N5 2.6(12) . . . . C13 C16 C15 C14 0.6(5) . . . . C13 C16 C17 C20 -157.6(4) . . . . C13 C16 C17 C18 22.4(6) . . . . C20 C17 C18 C19 -3.0(9) . . . . C18 C17 C20 C21 1.0(7) . . . . C21 N5 C19 C18 0.1(11) . . . . C19 N5 C21 C20 -2.3(10) . . . .