#------------------------------------------------------------------------------ #$Date: 2021-07-21 08:24:53 +0300 (Wed, 21 Jul 2021) $ #$Revision: 267669 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/38/2243876.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_2243876 loop_ _publ_author_name 'Wang, Yiran' 'Nisbet, Matthew L.' 'Poeppelmeier, Kenneth R.' _publ_section_title ; Crystal structures of two copper(I)--6,6'-dimethyl-2,2'-bipyridyl (dmbpy) compounds, [Cu(dmbpy)~2~]~2~[MF~6~]·xH~2~O (M = Zr, Hf; x = 1.134, 0.671) ; _journal_coeditor_code HB7977 _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 819 _journal_page_last 823 _journal_paper_doi 10.1107/S2056989021007295 _journal_volume 77 _journal_year 2021 _chemical_formula_iupac '[Cu (C12 H12 N2)2]2 [Zr F6], 1.134H2 O' _chemical_formula_moiety '2(C24 H24 Cu N4 +), F6 Zr 2-, 1.134(H2 O)' _chemical_formula_sum 'C48 H50.27 Cu2 F6 N8 O1.13 Zr' _chemical_formula_weight 1089.61 _chemical_name_systematic ; Bis[bis(6,6'-dimethyl-2,2'-bipyridine)copper(I)] hexafluoridozirconate(IV) 1.134-hydrate ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _cell_angle_alpha 103.078(2) _cell_angle_beta 104.013(3) _cell_angle_gamma 98.863(2) _cell_formula_units_Z 1 _cell_length_a 8.6219(3) _cell_length_b 10.8064(3) _cell_length_c 12.9992(4) _cell_measurement_reflns_used 10429 _cell_measurement_temperature 100.4(8) _cell_measurement_theta_max 30.5470 _cell_measurement_theta_min 2.2060 _cell_volume 1116.33(6) _computing_cell_refinement ; CrysAlisPro (Rigaku OD, 2020) ; _computing_data_collection ; CrysAlisPro (Rigaku OD, 2020) ; _computing_data_reduction ; CrysAlisPro (Rigaku OD, 2020) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014/5 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100.4(8) _diffrn_detector CCD _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.803 _diffrn_measurement_device 'AFC12 (Right): Kappa 3 circle' _diffrn_measurement_device_type 'Rigaku Saturn724+ (2x2 bin mode)' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_measurement_specimen_support 'Mitegen 50um' _diffrn_radiation_monochromator Confocal _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_unetI/netI 0.0430 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 16573 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.886 _diffrn_reflns_theta_min 1.984 _diffrn_source 'Rotating Anode' _diffrn_source_current 24.0 _diffrn_source_power 1.2 _diffrn_source_voltage 50.0 _exptl_absorpt_coefficient_mu 1.247 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.376 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2020) ; _exptl_crystal_colour 'clear orangish red' _exptl_crystal_density_diffrn 1.621 _exptl_crystal_description needle _exptl_crystal_F_000 555 _exptl_crystal_size_max 0.98 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.589 _refine_diff_density_min -0.538 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 312 _refine_ls_number_reflns 5673 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.072 _refine_ls_R_factor_all 0.0475 _refine_ls_R_factor_gt 0.0351 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+0.3898P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0834 _refine_ls_wR_factor_ref 0.0879 _reflns_number_gt 4588 _reflns_number_total 5673 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL ew1-37b_new_a.res in P-1 ew1-37b_new.res created by SHELXL-2016/6 at 12:33:27 on 28-Jun-2021 REM Old TITL ew1-37b_new in P-1 REM SHELXT solution in P-1 REM R1 0.120, Rweak 0.007, Alpha 0.049, Orientation as input REM Formula found by SHELXT: C50 N8 F6 Cu3 CELL 0.71073 8.6219 10.8064 12.9992 103.078 104.013 98.863 ZERR 1 0.0003 0.0003 0.0004 0.002 0.003 0.002 LATT 1 SFAC C H Cu F N O Zr UNIT 48 50.27 2 6 8 1.13 1 L.S. 100 PLAN 5 SIZE 0.05 0.13 0.98 TEMP -173 CONF BOND $H list 4 MORE -1 fmap 2 53 acta OMIT 0 1 1 OMIT -1 1 0 REM REM REM WGHT 0.039700 0.389800 FVAR 0.44889 0.56682 CU1 3 0.305482 0.354204 0.697561 11.00000 0.02111 0.01747 = 0.01614 0.00225 -0.00092 0.00081 N1 5 0.495250 0.365432 0.828448 11.00000 0.01995 0.01729 = 0.01275 0.00328 0.00218 0.00262 C1 1 0.562342 0.267389 0.852929 11.00000 0.02531 0.02051 = 0.01840 0.00650 0.00733 0.00776 N2 5 0.342385 0.546523 0.776006 11.00000 0.01929 0.01669 = 0.01982 0.00510 0.00155 0.00285 C2 1 0.711980 0.290470 0.932346 11.00000 0.02323 0.02549 = 0.02047 0.01001 0.00949 0.01139 AFIX 43 H2 2 0.756689 0.219858 0.948974 11.00000 -1.20000 AFIX 0 N3 5 0.087288 0.231592 0.615975 11.00000 0.02260 0.01416 = 0.01751 0.00289 0.00217 0.00381 C3 1 0.794723 0.417350 0.986713 11.00000 0.01678 0.03253 = 0.02037 0.01092 0.00359 0.00519 AFIX 43 H3 2 0.898128 0.435022 1.040244 11.00000 -1.20000 AFIX 0 N4 5 0.342304 0.297250 0.544502 11.00000 0.02507 0.02063 = 0.01905 0.00822 0.00664 0.00491 C4 1 0.725698 0.518737 0.962559 11.00000 0.01801 0.02062 = 0.02035 0.00390 0.00227 0.00067 AFIX 43 H4 2 0.780962 0.606656 0.999235 11.00000 -1.20000 AFIX 0 C5 1 0.574508 0.489800 0.883916 11.00000 0.01652 0.01672 = 0.01479 0.00405 0.00511 0.00331 C6 1 0.486935 0.591343 0.856440 11.00000 0.01693 0.01741 = 0.01597 0.00482 0.00579 0.00315 C7 1 0.545035 0.723167 0.911163 11.00000 0.02113 0.01879 = 0.01938 0.00431 0.00642 0.00079 AFIX 43 H7 2 0.649798 0.753655 0.964086 11.00000 -1.20000 AFIX 0 C8 1 0.447207 0.809054 0.886991 11.00000 0.03343 0.01680 = 0.02238 0.00480 0.01232 0.00394 AFIX 43 H8 2 0.484553 0.899537 0.923175 11.00000 -1.20000 AFIX 0 C9 1 0.295461 0.762734 0.810236 11.00000 0.02889 0.02224 = 0.03106 0.01312 0.01281 0.01018 AFIX 43 H9 2 0.224458 0.819860 0.796195 11.00000 -1.20000 AFIX 0 C10 1 0.247607 0.630600 0.753410 11.00000 0.02229 0.02311 = 0.02929 0.01246 0.00371 0.00453 C11 1 0.465318 0.131492 0.792276 11.00000 0.04558 0.01895 = 0.02647 0.00330 -0.00095 0.01036 AFIX 137 H11A 2 0.374488 0.110516 0.822909 11.00000 -1.50000 H11B 2 0.536537 0.069734 0.800414 11.00000 -1.50000 H11C 2 0.421624 0.125560 0.713932 11.00000 -1.50000 AFIX 0 C12 1 0.089726 0.574749 0.662438 11.00000 0.03335 0.02811 = 0.07256 0.01919 -0.01903 0.00291 AFIX 137 H12A 2 0.113803 0.542757 0.592501 11.00000 -1.50000 H12B 2 0.027094 0.642511 0.656716 11.00000 -1.50000 H12C 2 0.025358 0.502569 0.678793 11.00000 -1.50000 AFIX 0 C13 1 -0.035737 0.203741 0.659561 11.00000 0.02303 0.01732 = 0.02452 0.00314 0.00549 0.00526 C14 1 -0.190169 0.133083 0.592567 11.00000 0.02339 0.02037 = 0.04278 0.00567 0.00867 0.00191 AFIX 43 H14 2 -0.276649 0.114742 0.624100 11.00000 -1.20000 AFIX 0 C15 1 -0.216798 0.089905 0.480196 11.00000 0.02469 0.02167 = 0.03822 -0.00170 -0.00588 0.00063 AFIX 43 H15 2 -0.322268 0.042926 0.433723 11.00000 -1.20000 AFIX 0 C16 1 -0.089589 0.115237 0.435569 11.00000 0.03347 0.01948 = 0.02267 0.00069 -0.00542 0.00501 AFIX 43 H16 2 -0.105281 0.084169 0.358515 11.00000 -1.20000 AFIX 0 C17 1 0.062221 0.187221 0.505672 11.00000 0.02757 0.01484 = 0.01697 0.00444 -0.00069 0.00620 C18 1 0.207568 0.218197 0.466769 11.00000 0.03146 0.01957 = 0.01657 0.00772 0.00214 0.00698 C19 1 0.208268 0.168178 0.358586 11.00000 0.04734 0.02258 = 0.01798 0.00651 0.00562 0.00899 AFIX 43 H19 2 0.112010 0.114338 0.304771 11.00000 -1.20000 AFIX 0 C20 1 0.351251 0.198142 0.330812 11.00000 0.06023 0.03187 = 0.02447 0.01185 0.02225 0.01633 AFIX 43 H20 2 0.354850 0.164937 0.257431 11.00000 -1.20000 AFIX 0 C21 1 0.488847 0.276687 0.410479 11.00000 0.04646 0.03450 = 0.03565 0.01776 0.02391 0.01698 AFIX 43 H21 2 0.588640 0.296366 0.392590 11.00000 -1.20000 AFIX 0 C22 1 0.481557 0.327049 0.516906 11.00000 0.03036 0.02391 = 0.03096 0.01374 0.01317 0.01071 C23 1 0.001667 0.251387 0.781690 11.00000 0.03089 0.03411 = 0.02784 0.00683 0.01225 0.00446 AFIX 137 H23A 2 0.106137 0.232552 0.816790 11.00000 -1.50000 H23B 2 -0.085860 0.207350 0.805470 11.00000 -1.50000 H23C 2 0.009325 0.345593 0.803131 11.00000 -1.50000 AFIX 0 C24 1 0.626466 0.415078 0.606516 11.00000 0.02582 0.03673 = 0.03836 0.01471 0.01342 0.00340 AFIX 137 H24A 2 0.593595 0.492033 0.643469 11.00000 -1.50000 H24B 2 0.713290 0.442318 0.574399 11.00000 -1.50000 H24C 2 0.667181 0.368394 0.660221 11.00000 -1.50000 AFIX 0 ZR1 7 0.000000 1.000000 1.000000 10.50000 0.01462 0.02394 = 0.03837 0.01715 0.00458 0.00405 F1 4 0.090811 0.995180 0.870820 11.00000 0.03896 0.03548 = 0.05065 0.02095 0.01982 0.01287 F2 4 -0.054732 0.803497 0.959257 11.00000 0.02565 0.01879 = 0.04794 0.01043 0.00340 0.00224 F3 4 0.220274 1.000415 1.094560 11.00000 0.02075 0.02305 = 0.05108 0.00814 -0.00416 0.00523 AFIX 6 O1 6 -0.106235 0.624733 0.806055 21.00000 0.04146 0.03887 = 0.02438 0.00005 0.01169 0.00091 H1A 2 -0.045474 0.641036 0.764081 21.00000 -1.50000 H1B 2 -0.087438 0.692874 0.861724 21.00000 -1.50000 AFIX 0 HKLF 4 REM ew1-37b_new_a.res in P-1 REM R1 = 0.0351 for 4588 Fo > 4sig(Fo) and 0.0475 for all 5673 data REM 312 parameters refined using 0 restraints END WGHT 0.0397 0.3898 REM Highest difference peak 0.589, deepest hole -0.538, 1-sigma level 0.080 Q1 1 0.3826 0.2826 0.6048 11.00000 0.05 0.59 Q2 1 -0.0464 0.7995 0.9004 11.00000 0.05 0.49 Q3 1 0.3134 0.3565 0.6012 11.00000 0.05 0.44 Q4 1 0.5199 0.5371 0.8834 11.00000 0.05 0.44 Q5 1 -0.0118 0.9985 1.0782 11.00000 0.05 0.41 REM The information below was added by Olex2. REM REM R1 = 0.0351 for 4588 Fo > 4sig(Fo) and 0.0475 for all 16577 data REM 312 parameters refined using n/a restraints REM Highest difference peak 0.59, deepest hole -0.54 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0475 REM R1_gt = 0.0351 REM wR_ref = 0.0879 REM GOOF = 1.072 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 16577 REM Reflections_gt = 4588 REM Parameters = 312 REM Hole = -0.54 REM Peak = 0.59 REM Flack = n/a ; _cod_data_source_file hb7977sup1.cif _cod_data_source_block I _cod_database_code 2243876 _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_min 0.375 _shelx_estimated_absorpt_t_max 0.940 _shelx_hkl_file ; 0 0 -2 131.56 5.01 0 0 -3 137.71 5.61 0 0 4 6.05 1.09 0 0 5 8.70 1.68 0 0 5 11.55 1.45 0 0 6 430.27 16.26 0 0 6 443.52 16.05 0 0 7 87.88 5.13 0 0 7 94.94 4.89 0 0 8 4.80 1.96 0 0 -8 7.56 2.20 0 0 8 6.26 1.58 0 0 9 59.83 4.62 0 0 -9 74.43 5.60 0 0 9 66.35 4.39 0 0 -10 359.20 15.23 0 0 10 330.76 13.42 0 0 11 10.04 3.10 0 0 -11 7.55 2.88 0 0 11 11.42 2.48 0 0 12 19.36 3.45 0 0 -12 20.39 3.67 0 0 12 11.67 2.70 0 0 13 80.96 6.42 0 0 13 93.71 6.13 0 0 14 4.45 3.17 0 0 -14 4.32 2.82 0 0 14 4.66 2.59 0 0 -15 8.81 3.40 0 0 -16 9.03 4.19 0 -1 16 -0.35 3.74 0 1 -16 8.01 3.17 0 -1 15 34.81 5.04 0 1 -15 49.55 5.26 0 -1 15 37.19 4.41 0 -1 14 5.89 3.43 0 1 -14 12.73 3.36 0 -1 14 11.62 2.87 0 -1 13 -0.62 3.18 0 1 -13 1.02 2.42 0 -1 13 0.26 2.27 0 -1 12 357.90 15.88 0 1 -12 381.97 16.36 0 -1 12 358.69 15.18 0 -1 11 5.04 2.80 0 1 -11 0.94 2.38 0 -1 11 1.56 1.99 0 -1 10 11.86 2.97 0 1 -10 17.83 3.20 0 -1 10 13.50 2.55 0 -1 9 430.14 16.41 0 -1 9 409.85 16.80 0 -1 8 46.21 3.91 0 -1 7 79.17 4.90 0 -1 6 133.15 6.50 0 -1 5 241.81 8.60 0 1 -4 20.85 1.41 0 -1 4 20.66 1.20 0 1 -3 85.24 3.52 0 -1 3 82.26 3.34 0 1 -3 82.79 3.48 0 1 -2 2731.23 90.46 0 1 -2 2788.26 90.44 0 1 -1 19.39 1.24 0 1 -1 17.39 1.18 0 -1 1 19.04 1.09 0 1 0 34.97 1.73 0 1 0 32.26 1.71 0 -1 -1 -0.13 0.26 0 -1 -1 -0.05 0.24 0 -1 -2 362.11 11.72 0 -1 -2 314.42 11.91 0 -1 -2 331.16 11.65 0 -1 -2 348.36 12.82 0 1 3 312.08 11.34 0 -1 -3 316.07 11.34 0 -1 -3 324.68 11.02 0 1 3 328.87 11.24 0 -1 -3 313.67 11.47 0 1 3 326.05 11.67 0 1 4 15.76 1.54 0 -1 -4 16.04 1.71 0 -1 -4 17.21 1.25 0 1 4 16.41 1.65 0 -1 -4 15.11 1.45 0 1 5 6.51 1.40 0 -1 -5 8.06 2.13 0 -1 -5 9.30 1.77 0 1 5 5.79 1.50 0 1 6 88.50 4.65 0 -1 -6 92.76 5.89 0 -1 -6 90.80 4.78 0 1 6 85.29 4.69 0 1 7 47.29 3.33 0 -1 -7 48.71 4.42 0 1 7 45.10 3.38 0 1 8 487.51 18.04 0 -1 -8 492.90 19.88 0 1 8 451.87 17.85 0 1 9 2.14 1.80 0 -1 -9 2.00 2.15 0 1 9 0.38 1.91 0 1 10 5.71 2.17 0 -1 -10 9.70 2.99 0 1 10 5.43 2.42 0 -1 -11 283.81 13.63 0 1 11 269.58 11.60 0 -1 -12 8.07 3.34 0 -1 -13 70.37 6.50 0 -1 -14 133.37 9.24 0 -1 -15 34.63 5.24 0 -1 -16 2.24 4.30 0 1 16 3.08 3.22 0 -2 17 31.27 5.61 0 -2 16 12.93 4.41 0 2 -16 22.94 3.96 0 -2 15 6.26 4.27 0 2 -15 2.23 2.51 0 -2 15 0.29 2.55 0 -2 14 137.44 8.86 0 2 -14 147.93 8.51 0 -2 14 137.97 8.04 0 -2 13 5.86 3.27 0 2 -13 5.41 2.56 0 -2 13 2.65 2.45 0 -2 12 1.81 3.03 0 2 -12 0.58 2.19 0 -2 12 -0.25 2.11 0 2 -11 216.24 10.58 0 -2 11 203.14 10.57 0 -2 10 7.86 3.09 0 -2 9 29.85 3.67 0 -2 8 639.25 22.16 0 -2 8 664.57 24.39 0 -2 7 1439.59 48.10 0 -2 7 1420.74 49.55 0 -2 6 463.50 16.06 0 2 -6 455.69 16.55 0 2 -5 172.32 7.10 0 -2 5 171.29 6.75 0 2 -4 814.68 28.12 0 -2 4 816.96 27.86 0 2 -4 821.30 28.17 0 2 -3 451.30 16.15 0 2 -3 450.52 16.23 0 2 -2 7.49 1.61 0 2 -2 8.84 1.60 0 2 -2 7.57 1.40 0 -2 1 2953.56 98.12 0 2 -1 3020.81 98.76 0 -2 1 3055.97 98.67 0 -2 1 3063.92 98.02 0 -2 1 3013.77 98.74 0 2 -1 2962.81 98.81 0 -2 1 2917.25 98.00 0 -2 0 331.44 12.76 0 2 0 305.37 12.80 0 -2 0 337.22 12.76 0 2 0 298.89 12.73 0 -2 0 324.18 12.78 0 2 0 298.27 12.83 0 2 1 407.89 15.20 0 -2 -1 415.61 15.13 0 -2 -1 411.89 14.08 0 -2 -1 413.36 14.70 0 -2 -1 401.83 13.94 0 -2 -1 419.81 14.74 0 -2 -2 811.65 26.94 0 2 2 734.64 26.45 0 -2 -2 821.91 26.37 0 -2 -2 804.13 27.90 0 2 2 770.70 27.10 0 -2 -3 1.91 1.02 0 -2 -3 2.72 0.94 0 2 3 2.99 0.80 0 -2 -3 3.83 0.95 0 2 3 2.39 1.10 0 2 3 3.16 1.13 0 2 4 223.82 8.30 0 2 4 216.13 8.64 0 -2 -4 223.94 8.27 0 -2 -4 207.99 8.28 0 -2 -4 217.79 8.72 0 -2 -5 40.97 2.80 0 -2 -5 45.35 2.39 0 2 5 39.54 2.60 0 -2 -5 39.24 2.73 0 -2 -5 39.83 2.64 0 -2 -6 566.00 20.45 0 -2 -6 584.39 22.66 0 -2 -6 571.04 19.88 0 -2 -6 562.30 20.33 0 -2 -7 32.48 3.86 0 -2 -7 30.93 1.91 0 -2 -7 36.87 3.01 0 -2 -8 71.16 5.81 0 -2 -9 364.19 16.77 0 -2 -10 22.79 4.10 0 -2 -11 31.29 4.71 0 2 11 36.09 3.60 0 -2 -12 68.03 6.31 0 2 12 46.15 4.28 0 -2 -13 -0.46 3.05 0 2 13 3.00 2.34 0 -2 -14 31.22 5.22 0 2 14 30.12 4.00 0 -2 -15 14.53 4.74 0 2 15 14.12 3.44 0 -2 -16 72.54 7.58 0 -3 17 9.64 4.87 0 -3 16 80.57 7.53 0 3 -16 85.95 6.06 0 -3 15 2.31 3.90 0 3 -15 0.82 2.23 0 -3 15 -1.83 2.83 0 -3 14 11.97 4.02 0 3 -14 8.89 2.68 0 -3 14 6.16 2.71 0 -3 13 148.53 9.48 0 3 -13 170.82 8.74 0 -3 12 -2.60 3.42 0 3 -12 1.04 2.02 0 -3 11 4.09 0.81 0 -3 11 8.20 3.36 0 -3 10 314.64 11.94 0 -3 10 331.54 14.49 0 -3 9 208.54 8.78 0 -3 9 209.88 10.35 0 -3 8 193.06 8.27 0 -3 8 176.59 9.28 0 3 -7 610.17 21.82 0 -3 7 586.45 21.02 0 -3 6 181.04 7.48 0 3 -6 168.40 7.83 0 3 -5 210.48 8.94 0 -3 5 210.30 8.57 0 3 -5 201.14 8.93 0 3 -4 1.10 1.25 0 3 -4 1.85 1.36 0 3 -4 2.75 1.32 0 -3 4 0.65 1.12 0 3 -3 29.19 2.12 0 3 -3 29.85 1.82 0 3 -3 31.33 2.67 0 3 -3 29.63 2.61 0 3 -2 1.26 0.75 0 3 -2 2.26 1.51 0 3 -2 0.89 1.30 0 3 -2 1.36 0.98 0 -3 1 373.11 13.64 0 -3 1 354.52 13.02 0 -3 1 397.30 14.34 0 3 -1 375.85 14.45 0 3 -1 386.71 14.40 0 -3 1 398.11 14.25 0 -3 0 541.55 21.25 0 -3 0 544.47 21.17 0 3 0 502.31 21.26 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32.77 4.78 0 8 -8 43.85 4.11 0 8 -7 282.70 14.85 0 -8 7 302.60 14.13 0 8 -7 305.74 12.66 0 8 -7 286.51 12.21 0 -8 6 73.65 6.00 0 8 -6 70.78 6.51 0 8 -6 60.30 4.47 0 8 -6 62.10 6.14 0 8 -6 70.47 4.40 0 -8 5 24.36 3.88 0 8 -5 21.99 3.02 0 -8 5 17.90 3.30 0 8 -5 21.09 4.02 0 8 -5 25.26 4.16 0 8 -5 24.70 2.28 0 8 -4 224.14 10.36 0 8 -4 204.85 11.63 0 8 -4 198.90 8.15 0 8 -4 219.69 12.03 0 8 -3 2.31 2.09 0 8 -3 6.43 2.83 0 8 -3 -0.41 2.61 0 8 -3 3.57 1.12 0 -8 3 2.05 2.73 0 8 -2 170.35 9.43 0 -8 2 186.58 9.15 0 -8 2 167.84 8.01 0 8 -2 161.85 6.70 0 8 -2 182.80 10.68 0 8 -2 193.13 10.90 0 -8 2 203.27 10.31 0 8 -1 551.80 21.89 0 -8 1 552.11 21.14 0 -8 1 524.50 18.90 0 -8 1 586.83 22.06 0 8 0 347.88 16.55 0 -8 0 356.15 15.66 0 8 0 374.44 16.66 0 8 0 322.34 13.17 0 -8 0 336.57 12.90 0 8 0 311.52 16.25 0 -8 0 394.84 16.30 0 8 1 0.42 2.80 0 -8 -1 -0.71 2.38 0 -8 -1 1.35 2.59 0 8 1 -0.87 3.17 0 8 1 1.67 2.87 0 -8 -1 1.32 1.21 0 -8 -2 8.12 3.14 0 -8 -2 5.11 1.93 0 -8 -2 6.25 2.92 0 8 2 3.94 3.11 0 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10 266.87 9.82 2 1 -9 17.19 1.88 -2 -1 9 19.53 2.01 -2 -1 8 6.20 1.35 2 1 -8 6.77 1.29 -2 -1 7 291.73 11.60 2 1 -7 310.90 12.06 2 1 -7 298.25 10.86 -2 -1 6 115.36 5.75 2 1 -6 130.78 6.28 2 1 -5 11.60 1.89 -2 -1 5 9.00 1.66 -2 -1 5 12.24 1.09 -2 -1 4 5338.72 176.14 2 1 -4 5366.12 176.37 2 1 -3 7484.85 245.69 -2 -1 2 77.75 4.51 2 1 -2 76.21 4.48 -2 -1 1 13.04 1.73 -2 -1 1 13.19 2.10 2 1 -1 14.61 2.15 -2 -1 1 12.22 1.14 2 1 0 592.58 22.86 -2 -1 0 597.20 22.91 2 1 0 642.96 21.07 2 1 0 627.33 22.45 -2 -1 0 612.29 22.31 -2 -1 0 660.67 21.03 -2 -1 0 574.03 22.88 -2 -1 -1 162.76 6.85 -2 -1 -1 159.51 5.69 -2 -1 -1 164.14 7.34 -2 -1 -1 162.59 7.46 2 1 1 166.90 7.51 -2 -1 -2 0.59 1.12 2 1 2 -0.17 1.29 -2 -1 -2 1.22 1.25 2 1 3 275.34 11.09 -2 -1 -3 260.42 11.22 -2 -1 -3 264.69 10.77 -2 -1 -3 266.76 10.72 2 1 4 19.63 2.30 2 1 4 20.69 2.43 2 1 4 20.92 2.74 -2 -1 -4 15.57 2.35 -2 -1 -4 19.20 2.58 -2 -1 -4 20.75 2.12 2 1 5 59.62 3.78 2 1 5 63.31 4.59 -2 -1 -5 54.67 4.10 2 1 5 54.38 3.88 -2 -1 -5 53.26 4.05 -2 -1 -5 53.47 3.31 2 1 6 210.53 9.68 -2 -1 -6 215.93 8.86 -2 -1 -6 195.14 9.54 2 1 6 224.00 10.42 2 1 7 687.20 25.59 -2 -1 -7 659.51 23.10 2 1 7 645.30 24.66 -2 -1 -7 619.76 24.61 -2 -1 -7 676.64 23.22 2 1 8 316.34 13.94 -2 -1 -8 299.28 10.83 2 1 8 297.16 13.16 -2 -1 -8 303.90 13.27 -2 -1 -8 297.75 10.85 -2 -1 -9 329.87 15.14 2 1 9 367.20 15.88 2 1 9 354.45 15.12 -2 -1 -10 73.27 6.00 2 1 10 79.75 6.34 2 1 10 76.31 5.72 2 1 11 5.71 3.03 -2 -1 -11 6.97 3.78 2 1 11 4.85 2.85 2 1 12 9.27 3.25 -2 -1 -12 8.37 4.19 2 1 12 5.77 3.04 -2 -1 -13 68.53 7.65 2 1 13 51.69 5.49 -2 -1 -14 0.56 4.03 2 1 14 2.47 3.16 -2 -1 -15 1.71 3.93 2 1 15 -1.85 3.63 -2 -2 18 -0.75 4.12 -2 -2 17 5.40 4.24 2 2 -16 59.52 4.02 -2 -2 16 47.66 5.65 2 2 -15 144.51 6.74 -2 -2 15 126.29 6.78 -2 -2 15 145.64 8.82 2 2 -14 3.54 1.81 -2 -2 14 1.45 1.80 -2 -2 14 3.48 3.47 -2 -2 13 84.73 6.47 2 2 -13 79.39 4.45 -2 -2 12 80.96 3.34 2 2 -12 81.81 4.24 -2 -2 11 16.92 3.47 2 2 -11 22.68 2.07 -2 -2 11 22.87 2.02 2 2 -10 34.26 2.30 -2 -2 10 37.93 2.75 -2 -2 10 33.39 2.80 -2 -2 10 39.42 2.85 2 2 -9 258.78 9.50 -2 -2 9 269.42 10.70 -2 -2 9 267.73 10.90 -2 -2 9 256.90 10.74 -2 -2 8 45.31 3.36 -2 -2 8 42.27 3.41 -2 -2 7 74.70 4.58 -2 -2 7 71.68 4.63 2 2 -6 882.61 32.41 -2 -2 6 928.71 32.28 -2 -2 5 1216.48 42.51 2 2 -5 1220.88 42.65 2 2 -4 212.53 9.70 2 2 -3 21.33 2.70 -2 -2 2 293.58 12.37 2 2 -2 303.80 12.52 -2 -2 2 291.32 10.91 -2 -2 1 386.72 15.68 2 2 -1 396.78 15.87 -2 -2 1 404.95 14.88 -2 -2 1 397.64 13.91 -2 -2 0 109.87 5.31 -2 -2 0 107.17 5.89 -2 -2 0 113.44 6.10 -2 -2 -1 741.90 27.05 -2 -2 -1 732.73 27.03 -2 -2 -1 750.03 26.12 2 2 2 199.57 9.37 -2 -2 -2 205.55 9.21 -2 -2 -2 192.73 8.44 -2 -2 -2 213.31 9.46 2 2 3 14.54 2.05 -2 -2 -3 12.30 2.28 2 2 3 13.35 2.36 -2 -2 -3 17.54 2.41 2 2 4 339.67 14.16 -2 -2 -4 307.39 13.62 -2 -2 -4 330.67 13.35 2 2 4 356.90 13.37 -2 -2 -4 309.24 13.02 -2 -2 -4 327.24 13.21 2 2 5 235.50 11.25 -2 -2 -5 236.79 10.93 -2 -2 -5 239.48 10.22 2 2 5 252.82 10.58 -2 -2 -5 234.41 10.49 -2 -2 -5 233.42 10.07 -2 -2 -6 164.20 7.27 2 2 6 156.11 8.60 -2 -2 -6 155.91 8.27 2 2 6 169.55 8.09 -2 -2 -6 162.08 7.48 -2 -2 -6 146.51 7.86 -2 -2 -6 155.97 7.29 -2 -2 -7 392.20 15.06 -2 -2 -7 401.10 15.17 2 2 7 452.60 17.81 2 2 7 438.64 16.70 -2 -2 -7 372.92 16.36 -2 -2 -7 416.05 15.30 2 2 8 29.10 3.55 -2 -2 -8 37.07 4.13 -2 -2 -8 34.31 2.43 2 2 9 2.11 2.28 -2 -2 -9 1.55 3.02 -2 -2 -9 -0.26 2.85 -2 -2 -9 0.82 0.84 2 2 10 -0.56 2.43 -2 -2 -10 1.65 3.47 -2 -2 -10 0.29 3.05 2 2 11 235.18 11.87 -2 -2 -11 239.59 12.17 -2 -2 -12 0.57 3.65 2 2 12 -0.65 2.70 -2 -2 -13 19.25 4.99 2 2 13 24.71 4.20 -2 -2 -14 22.63 5.77 2 2 14 13.26 3.92 2 2 15 35.43 5.04 -2 -3 18 4.35 4.30 -2 -3 17 31.32 5.61 -2 -3 16 0.75 3.95 -2 -3 15 16.57 4.46 -2 -3 14 135.92 8.76 -2 -3 13 2.33 3.31 -2 -3 12 2.88 3.15 -2 -3 12 7.23 1.64 -2 -3 12 6.35 1.53 -2 -3 11 298.03 11.96 -2 -3 11 285.90 11.78 -2 -3 11 300.09 11.78 -2 -3 10 0.19 1.58 -2 -3 10 0.92 1.48 -2 -3 10 0.17 1.68 -2 -3 9 121.91 6.59 -2 -3 9 121.88 6.61 -2 -3 9 118.86 6.43 -2 -3 8 384.19 15.93 -2 -3 8 403.85 16.05 -2 -3 8 397.34 15.86 -2 -3 7 744.21 27.70 -2 -3 7 749.48 27.54 -2 -3 6 3.11 2.01 -2 -3 6 1.84 1.89 -2 -3 5 363.37 15.41 -2 -3 5 384.98 15.68 -2 -3 4 198.96 7.49 -2 -3 3 124.46 5.81 -2 -3 2 0.83 0.81 -2 -3 2 0.24 1.69 2 3 -2 -0.25 1.69 -2 -3 2 0.24 1.75 2 3 -1 573.50 22.36 -2 -3 1 569.63 22.21 -2 -3 1 581.19 22.19 -2 -3 0 88.77 5.72 -2 -3 0 81.76 5.51 -2 -3 0 84.75 4.74 -2 -3 -1 99.82 6.15 -2 -3 -1 96.16 5.19 -2 -3 -1 100.37 6.06 -2 -3 -1 108.41 6.34 2 3 2 1917.01 63.91 -2 -3 -2 1915.17 63.60 -2 -3 -2 1879.93 64.78 -2 -3 -2 1895.94 64.91 -2 -3 -2 1786.02 64.78 -2 -3 -3 90.40 4.94 2 3 3 79.59 4.97 -2 -3 -3 84.03 5.38 -2 -3 -3 90.90 5.75 -2 -3 -3 86.76 5.68 -2 -3 -4 7.75 2.10 2 3 4 8.86 1.97 -2 -3 -4 6.89 1.91 -2 -3 -4 7.73 2.02 -2 -3 -4 10.19 2.27 -2 -3 -5 831.61 29.83 -2 -3 -5 790.67 30.30 -2 -3 -5 813.36 29.55 2 3 5 863.72 29.77 -2 -3 -5 805.86 29.53 -2 -3 -5 798.11 29.72 -2 -3 -6 727.78 26.24 -2 -3 -6 695.35 27.12 -2 -3 -6 729.70 26.04 2 3 6 770.20 26.68 -2 -3 -6 649.97 26.35 -2 -3 -6 724.14 26.25 -2 -3 -7 23.56 2.76 -2 -3 -7 28.58 4.93 -2 -3 -7 28.48 3.59 2 3 7 28.50 3.37 -2 -3 -7 28.09 2.70 -2 -3 -7 24.42 3.67 -2 -3 -7 26.94 2.69 -2 -3 -8 25.91 2.51 -2 -3 -8 36.97 5.49 2 3 8 29.54 3.51 -2 -3 -8 38.05 4.24 -2 -3 -8 29.75 2.73 2 3 9 46.21 4.47 -2 -3 -9 51.94 6.52 -2 -3 -9 51.08 4.83 -2 -3 -9 50.71 3.01 -2 -3 -10 21.12 3.79 -2 -3 -10 15.89 4.33 2 3 10 17.03 3.37 -2 -3 -11 5.96 3.47 -2 -3 -11 5.79 4.23 2 3 11 5.10 2.85 -2 -3 -12 92.29 8.59 2 3 12 64.43 5.86 -2 -3 -13 8.01 4.62 2 3 13 7.56 3.48 2 3 14 10.24 3.76 -2 -4 18 -0.84 4.69 -2 -4 17 9.52 5.03 -2 -4 16 32.21 5.66 -2 -4 15 20.53 4.87 -2 -4 14 6.04 4.17 -2 -4 14 14.62 1.94 -2 -4 13 165.20 10.10 -2 -4 13 168.07 7.88 -2 -4 13 180.74 7.71 -2 -4 12 3.12 2.05 -2 -4 12 4.78 1.92 -2 -4 11 117.43 6.30 -2 -4 11 115.63 6.69 -2 -4 11 111.84 6.28 -2 -4 10 257.67 11.32 -2 -4 10 246.45 11.41 -2 -4 10 264.23 11.88 -2 -4 9 8.00 2.34 -2 -4 9 7.05 2.23 -2 -4 9 6.49 2.25 -2 -4 8 0.80 1.64 -2 -4 8 1.00 1.82 -2 -4 8 1.12 2.03 2 4 -7 448.75 18.01 -2 -4 7 466.81 19.02 -2 -4 7 461.46 19.15 -2 -4 7 486.12 18.89 -2 -4 6 136.68 7.99 -2 -4 6 139.89 7.87 2 4 -6 129.91 6.72 -2 -4 6 142.03 7.79 -2 -4 5 40.16 3.93 -2 -4 5 43.22 4.34 -2 -4 5 40.21 4.09 -2 -4 5 40.02 2.09 -2 -4 4 111.48 4.89 -2 -4 4 94.81 5.54 -2 -4 3 445.10 16.75 -2 -4 3 434.78 18.67 -2 -4 3 461.38 16.84 -2 -4 2 144.89 6.45 -2 -4 2 140.88 7.24 2 4 -2 149.43 5.51 -2 -4 2 150.83 8.52 -2 -4 2 150.24 8.32 -2 -4 1 173.35 9.35 -2 -4 1 185.17 9.86 2 4 -1 201.28 6.69 -2 -4 1 188.56 10.06 -2 -4 0 1567.21 55.59 -2 -4 0 1597.06 54.24 -2 -4 0 1574.82 55.95 -2 -4 0 1600.35 55.86 -2 -4 0 1582.32 55.72 -2 -4 -1 -0.63 1.97 -2 -4 -1 1.75 2.00 -2 -4 -1 1.02 1.49 -2 -4 -1 0.66 0.34 -2 -4 -1 2.16 1.88 -2 -4 -1 -0.29 1.76 -2 -4 -2 178.38 9.89 -2 -4 -2 187.04 10.66 -2 -4 -2 179.66 9.63 -2 -4 -2 204.14 8.91 -2 -4 -2 205.56 7.01 -2 -4 -2 200.43 10.06 -2 -4 -2 197.61 10.14 -2 -4 -3 414.48 17.68 -2 -4 -3 440.38 17.54 -2 -4 -3 417.83 16.31 -2 -4 -3 432.51 19.13 -2 -4 -3 434.44 17.88 -2 -4 -3 411.80 17.56 -2 -4 -4 213.42 10.65 -2 -4 -4 207.34 10.07 2 4 4 211.50 9.81 -2 -4 -4 214.07 12.00 -2 -4 -4 219.17 10.47 -2 -4 -4 213.47 10.57 -2 -4 -5 144.16 7.47 2 4 5 149.86 7.69 -2 -4 -5 139.78 7.53 -2 -4 -5 131.19 8.07 -2 -4 -5 149.86 7.80 -2 -4 -5 132.88 7.78 -2 -4 -6 3.55 1.90 -2 -4 -6 4.21 2.43 -2 -4 -6 2.30 1.90 2 4 6 5.02 2.28 -2 -4 -6 4.23 2.60 -2 -4 -6 4.51 2.11 -2 -4 -7 139.81 8.61 -2 -4 -7 169.50 7.85 2 4 7 165.08 8.51 -2 -4 -7 159.47 8.45 -2 -4 -7 159.28 8.13 -2 -4 -8 147.42 10.58 -2 -4 -8 147.36 8.57 2 4 8 152.17 8.21 -2 -4 -8 147.74 7.36 -2 -4 -8 146.38 8.15 -2 -4 -8 145.44 6.97 -2 -4 -9 15.36 2.17 -2 -4 -9 12.97 4.11 -2 -4 -9 16.06 3.56 -2 -4 -9 13.79 2.28 2 4 9 18.45 3.31 -2 -4 -10 219.55 10.92 -2 -4 -10 237.00 14.14 2 4 10 212.76 10.90 -2 -4 -11 1.74 3.45 -2 -4 -11 4.29 4.10 2 4 11 2.46 2.61 -2 -4 -12 34.82 6.42 2 4 12 41.96 4.79 2 4 13 57.74 5.67 -2 -5 17 1.77 4.82 -2 -5 16 -2.58 4.61 -2 -5 15 97.87 8.30 -2 -5 15 99.87 5.23 -2 -5 14 -5.34 4.52 -2 -5 14 -2.04 2.04 -2 -5 14 3.82 1.90 -2 -5 13 0.25 2.13 -2 -5 13 2.52 1.91 -2 -5 12 325.44 14.74 -2 -5 12 352.54 14.29 -2 -5 11 9.94 2.51 -2 -5 11 14.41 2.69 -2 -5 11 13.83 3.19 2 5 -10 159.07 9.01 -2 -5 10 167.50 8.66 -2 -5 10 157.17 8.76 -2 -5 10 175.40 9.44 2 5 -9 131.94 7.40 -2 -5 9 129.74 7.53 -2 -5 9 123.45 7.86 -2 -5 9 120.86 7.47 -2 -5 8 95.16 6.33 -2 -5 8 97.40 6.56 -2 -5 8 91.21 6.67 2 5 -8 92.27 5.94 2 5 -7 14.73 2.48 -2 -5 7 20.55 3.22 -2 -5 7 13.38 2.82 -2 -5 7 16.95 3.15 -2 -5 6 749.02 28.92 -2 -5 6 735.43 28.61 2 5 -6 709.09 26.40 -2 -5 6 781.95 28.51 2 5 -5 361.26 13.66 -2 -5 5 371.59 15.85 -2 -5 5 342.78 12.89 -2 -5 5 367.75 16.29 -2 -5 4 11.67 2.25 -2 -5 4 16.23 1.93 -2 -5 3 249.09 10.34 -2 -5 3 229.25 10.31 -2 -5 3 251.80 12.07 -2 -5 3 238.54 12.23 -2 -5 3 258.52 12.35 2 5 -3 241.93 9.06 -2 -5 2 2132.87 72.80 -2 -5 2 2002.09 73.75 2 5 -2 2241.03 71.15 -2 -5 2 2063.88 75.53 -2 -5 2 2105.68 75.55 -2 -5 2 2090.55 75.16 -2 -5 1 85.08 5.47 -2 -5 1 90.57 6.09 2 5 -1 65.28 2.69 -2 -5 1 78.67 6.08 -2 -5 1 84.00 6.11 -2 -5 0 28.66 3.58 -2 -5 0 30.05 3.02 -2 -5 0 26.39 3.68 -2 -5 0 23.20 3.47 -2 -5 0 30.71 3.84 -2 -5 -1 663.54 26.43 -2 -5 -1 692.66 24.39 -2 -5 -1 687.36 25.99 -2 -5 -1 705.26 26.56 -2 -5 -1 666.30 26.24 -2 -5 -1 648.60 21.89 -2 -5 -2 48.56 5.07 -2 -5 -2 45.12 4.54 -2 -5 -2 53.62 4.72 -2 -5 -2 46.72 3.67 -2 -5 -2 52.12 2.12 -2 -5 -2 57.61 5.09 -2 -5 -2 46.31 4.53 -2 -5 -3 26.66 3.76 -2 -5 -3 26.00 4.18 -2 -5 -3 21.60 3.53 -2 -5 -3 29.74 3.69 -2 -5 -3 26.60 2.86 -2 -5 -3 27.36 1.61 -2 -5 -3 32.34 3.72 -2 -5 -4 88.69 6.47 -2 -5 -4 99.90 6.34 -2 -5 -4 85.64 7.42 -2 -5 -4 86.38 6.48 -2 -5 -4 89.76 6.22 -2 -5 -5 69.71 6.00 -2 -5 -5 72.68 5.35 -2 -5 -5 74.02 5.23 -2 -5 -5 75.81 7.08 -2 -5 -5 73.08 5.48 -2 -5 -5 87.24 6.19 -2 -5 -6 3.70 2.53 -2 -5 -6 6.70 2.25 -2 -5 -6 6.12 2.76 -2 -5 -6 7.49 2.69 -2 -5 -7 1.66 2.60 -2 -5 -7 1.54 1.96 2 5 7 -0.27 2.30 -2 -5 -7 0.26 2.67 -2 -5 -7 1.39 2.19 -2 -5 -8 193.65 12.44 -2 -5 -8 166.09 9.83 -2 -5 -8 189.42 8.73 2 5 8 179.74 9.50 -2 -5 -8 195.83 9.55 -2 -5 -8 179.37 9.16 -2 -5 -9 28.20 5.42 -2 -5 -9 19.94 3.79 2 5 9 16.86 3.42 -2 -5 -9 19.84 2.85 -2 -5 -9 23.62 3.88 -2 -5 -9 21.46 2.78 -2 -5 -10 16.70 3.69 -2 -5 -10 15.61 5.06 2 5 10 16.88 3.50 -2 -5 -11 88.37 9.16 2 5 11 86.96 6.59 2 5 12 2.55 3.01 -2 -6 16 -3.22 4.94 -2 -6 15 24.09 3.54 -2 -6 15 24.05 5.45 -2 -6 14 150.23 7.73 -2 -6 14 139.41 8.27 -2 -6 14 143.88 10.09 -2 -6 13 35.16 3.86 -2 -6 13 20.75 3.60 -2 -6 12 1.05 2.31 -2 -6 12 1.71 2.61 2 6 -12 1.63 3.03 2 6 -11 251.45 12.43 -2 -6 11 262.54 12.33 -2 -6 11 277.77 13.42 -2 -6 10 96.61 6.61 -2 -6 10 108.91 7.05 -2 -6 10 92.67 7.18 2 6 -10 102.83 6.60 -2 -6 9 -0.62 2.65 2 6 -9 -1.23 2.23 -2 -6 9 -1.33 2.29 -2 -6 9 -0.76 2.46 -2 -6 8 409.29 17.90 2 6 -8 415.85 16.66 -2 -6 8 406.92 18.71 -2 -6 8 436.37 18.49 -2 -6 7 229.69 11.43 2 6 -7 209.98 9.62 -2 -6 7 221.32 11.91 -2 -6 7 212.79 11.41 -2 -6 6 164.49 9.29 -2 -6 6 161.75 9.49 -2 -6 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142.32 9.84 4 -8 -6 136.36 6.44 -4 8 6 152.28 9.15 -4 8 5 447.44 20.01 4 -8 -5 416.36 15.74 -4 8 5 468.64 19.56 -4 8 4 7.04 3.19 4 -8 -4 7.46 1.78 -4 8 4 3.01 2.86 -4 8 3 128.23 8.66 4 -8 -3 123.51 5.74 -4 8 3 132.66 8.62 -4 8 2 73.62 6.10 -4 8 2 68.39 6.05 4 -8 -2 71.66 3.77 4 -8 -2 56.30 3.60 4 -8 -1 46.74 3.39 -4 8 1 48.60 4.38 4 -8 -1 35.74 3.02 4 -8 0 3.53 2.18 4 -8 0 1.30 1.53 -4 8 0 0.54 1.83 -4 8 -1 525.32 21.27 -4 8 -1 520.87 22.15 4 -8 1 502.40 18.76 4 -8 1 515.38 19.85 4 -8 1 533.17 19.80 -4 8 -2 44.00 4.40 4 -8 2 45.56 3.48 -4 8 -2 50.08 5.36 4 -8 2 48.93 4.34 4 -8 2 43.31 4.37 4 -8 3 3.87 2.91 -4 8 -3 7.14 2.94 4 -8 3 -0.75 3.51 4 -8 3 3.39 1.90 4 -8 4 290.63 13.70 4 -8 4 331.99 15.33 -4 8 -4 292.13 14.55 4 -8 5 216.27 10.82 -4 8 -5 179.25 8.20 -4 8 -5 205.83 11.12 4 -8 6 31.26 4.86 -4 8 -6 27.13 2.92 -4 8 -6 40.17 4.86 4 -8 7 5.09 3.60 -4 8 -7 2.69 2.00 -4 8 -7 4.54 2.91 -4 8 -8 181.59 8.18 -4 8 -8 194.39 10.89 -4 8 -8 195.13 9.19 -4 8 -9 13.05 2.76 -4 8 -9 8.40 2.26 -4 8 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3.59 5 -9 3 1.48 2.86 -5 9 -3 4.82 2.90 5 -9 3 -2.87 3.28 -5 9 -3 2.21 2.85 5 -9 4 179.27 10.12 5 -9 4 196.79 11.95 -5 9 -4 169.27 10.80 5 -9 5 9.14 3.82 -5 9 -5 10.81 2.43 -5 9 -5 11.39 3.62 5 -9 6 8.34 3.91 -5 9 -6 12.67 2.21 -5 9 -6 7.45 3.57 5 -9 7 38.45 5.51 -5 9 -7 37.82 3.45 -5 9 -7 38.37 5.28 5 -9 8 99.33 8.03 -5 9 -8 73.26 5.05 -5 9 -8 89.75 7.59 5 -9 9 10.55 4.68 -5 9 -9 6.03 2.48 -5 9 -9 14.82 4.17 -5 9 -10 -2.21 2.87 5 -9 10 6.27 4.75 -5 9 -10 0.83 3.04 -5 9 -10 2.15 3.38 -5 9 -11 115.60 8.83 -5 8 11 80.97 7.03 -5 8 10 5.11 3.20 -5 8 10 4.90 3.18 -5 8 9 1.55 3.00 -5 8 8 129.64 8.72 -5 8 7 1.97 3.08 -5 8 6 261.94 13.15 5 -8 -6 237.16 9.93 -5 8 6 251.05 13.64 -5 8 5 23.57 4.25 5 -8 -5 18.11 2.28 -5 8 5 25.15 4.52 -5 8 4 84.39 6.82 -5 8 4 104.12 7.50 5 -8 -3 28.89 2.28 -5 8 3 38.68 4.88 5 -8 -3 28.87 2.56 -5 8 3 37.54 4.83 -5 8 2 18.42 3.80 -5 8 2 12.23 3.41 5 -8 -2 10.26 1.98 5 -8 -1 161.37 7.41 5 -8 0 0.34 1.22 -5 8 0 1.94 2.65 5 -8 0 -0.58 2.07 5 -8 0 3.76 1.90 -5 8 -1 9.85 2.96 -5 8 -1 8.15 3.36 5 -8 1 8.55 2.72 5 -8 1 9.63 2.42 5 -8 1 7.51 1.80 -5 8 -2 254.07 13.26 5 -8 2 280.91 12.12 5 -8 2 288.80 12.18 -5 8 -2 226.52 10.12 5 -8 2 257.04 10.46 5 -8 3 31.22 4.25 -5 8 -3 30.01 2.65 5 -8 3 34.95 4.80 -5 8 -3 38.36 4.85 5 -8 4 5.94 3.28 -5 8 -4 4.27 1.97 5 -8 4 3.47 4.48 -5 8 -4 5.11 2.77 5 -8 5 86.25 6.75 -5 8 -5 75.13 4.47 -5 8 -5 85.25 6.85 5 -8 6 264.12 12.96 -5 8 -6 231.00 10.03 -5 8 -6 240.34 12.81 5 -8 7 12.98 4.32 -5 8 -7 9.76 2.33 -5 8 -7 9.10 3.39 5 -8 8 12.97 4.26 -5 8 -8 14.50 2.78 -5 8 -8 13.37 3.55 -5 8 -9 144.18 7.02 -5 8 -9 175.18 10.17 -5 8 -9 158.56 8.17 5 -8 9 183.23 11.10 -5 8 -10 41.34 5.17 -5 8 -10 38.97 4.13 5 -8 10 35.90 6.01 -5 8 -11 13.61 4.07 -5 8 -11 21.14 3.57 5 -8 11 18.05 5.23 -5 7 12 0.32 2.83 -5 7 11 9.87 3.40 5 -7 -11 9.54 3.31 -5 7 11 14.41 3.40 -5 7 10 36.15 4.71 -5 7 9 6.26 2.97 -5 7 8 30.17 4.80 -5 7 8 29.06 4.29 -5 7 7 16.32 3.53 5 -7 -7 17.21 2.56 -5 7 7 14.76 3.76 -5 7 6 100.06 7.36 5 -7 -6 102.88 5.30 -5 7 6 106.72 7.89 -5 7 5 18.97 3.75 5 -7 -5 19.87 2.28 -5 7 5 23.68 4.17 -5 7 4 179.49 10.34 -5 7 4 199.49 10.73 5 -7 -4 181.04 7.75 -5 7 3 266.76 12.66 5 -7 -3 219.31 9.02 5 -7 -3 226.73 9.48 -5 7 3 273.98 12.59 5 -7 -2 6.09 1.59 -5 7 2 9.88 3.12 5 -7 -2 8.64 1.65 -5 7 1 3.79 2.43 -5 7 1 4.30 2.33 5 -7 -1 4.51 1.67 5 -7 0 399.71 14.46 -5 7 0 383.14 17.71 5 -7 0 412.03 15.87 -5 7 0 391.02 15.51 5 -7 0 412.81 15.38 5 -7 1 144.30 6.13 -5 7 -1 140.06 8.75 5 -7 1 133.15 6.98 -5 7 -1 127.56 6.31 5 -7 1 144.97 7.52 -5 7 -2 13.95 3.71 5 -7 2 7.85 2.69 -5 7 -2 10.32 1.72 5 -7 2 12.49 2.98 -5 7 -3 183.33 10.57 -5 7 -3 180.34 8.13 5 -7 3 220.78 11.23 5 -7 3 211.95 10.32 -5 7 -4 257.30 12.90 -5 7 -4 251.43 10.31 5 -7 4 263.73 12.56 -5 7 -5 5.58 3.00 -5 7 -5 1.70 1.54 5 -7 5 6.52 3.31 -5 7 -6 162.68 9.63 -5 7 -6 159.81 7.57 5 -7 6 170.34 9.96 -5 7 -7 252.11 12.82 5 -7 7 268.37 13.42 -5 7 -7 241.14 10.71 -5 7 -8 9.97 3.23 -5 7 -8 15.25 2.17 5 -7 8 14.12 4.27 -5 7 -8 19.47 2.93 -5 7 -9 29.03 2.99 5 -7 9 36.25 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6.31 -5 6 -3 -0.55 3.12 5 -6 3 4.20 2.67 -5 6 -3 3.79 1.60 5 -6 4 6.34 2.86 -5 6 -4 8.13 1.64 5 -6 5 187.34 9.98 -5 6 -5 164.82 7.50 -5 6 -5 165.09 9.47 -5 6 -6 38.04 2.46 5 -6 6 34.67 4.75 -5 6 -6 33.12 3.10 -5 6 -6 39.96 4.44 -5 6 -7 22.80 2.40 5 -6 7 22.61 4.07 -5 6 -7 19.62 2.65 -5 6 -7 16.02 3.55 -5 6 -8 187.44 8.20 -5 6 -8 178.37 8.76 5 -6 8 182.12 10.78 -5 6 -8 180.04 9.90 -5 6 -9 2.06 2.10 -5 6 -9 1.98 2.15 5 -6 9 2.07 3.92 -5 6 -9 2.83 2.71 -5 6 -10 7.28 2.95 -5 6 -10 9.14 3.06 -5 6 -10 3.89 2.55 5 -6 10 5.68 4.22 5 -6 10 4.91 2.98 5 -6 11 158.96 9.21 -5 6 -11 179.01 9.43 -5 6 -11 160.26 9.05 5 -6 12 2.42 2.66 -5 6 -12 5.59 3.24 -5 5 13 2.06 2.37 5 -5 -12 -0.28 2.47 -5 5 12 0.51 2.34 5 -5 -11 103.36 7.18 -5 5 11 129.89 9.18 -5 5 11 118.55 7.19 5 -5 -10 29.12 3.96 -5 5 10 25.08 4.46 -5 5 10 26.58 3.77 -5 5 9 -1.58 2.88 5 -5 -9 0.32 2.28 -5 5 9 3.37 2.59 5 -5 -9 -3.83 3.11 -5 5 8 31.89 4.43 5 -5 -8 27.95 3.50 5 -5 -7 186.61 8.19 -5 5 7 196.02 10.05 5 -5 -6 58.02 3.96 -5 5 6 56.89 5.18 5 -5 -6 52.34 3.30 5 -5 -5 43.71 3.21 5 -5 -5 46.13 3.33 -5 5 4 660.95 25.25 -5 5 4 641.57 22.40 5 -5 -4 646.53 22.70 -5 5 3 31.87 3.72 -5 5 3 35.80 2.68 5 -5 -3 27.07 2.22 5 -5 -3 26.37 2.53 -5 5 2 50.63 3.62 5 -5 -2 61.74 3.39 5 -5 -2 53.95 3.64 -5 5 1 432.49 16.63 -5 5 1 458.96 16.91 5 -5 -1 419.46 16.51 5 -5 0 123.83 4.84 -5 5 0 125.11 5.89 -5 5 0 125.20 6.65 -5 5 -1 48.45 4.28 -5 5 -1 43.38 2.78 -5 5 -2 309.29 13.00 -5 5 -2 285.81 11.01 5 -5 2 288.33 12.65 -5 5 -3 799.37 29.09 5 -5 3 869.21 29.64 5 -5 3 790.91 28.89 -5 5 -4 -0.24 1.22 5 -5 4 -0.83 2.48 -5 5 -4 1.43 3.14 -5 5 -5 99.78 4.38 -5 5 -5 109.44 7.39 5 -5 5 109.76 7.25 -5 5 -5 98.68 5.20 5 -5 6 -1.32 3.02 -5 5 -6 -1.17 1.77 -5 5 -6 1.22 1.35 -5 5 -7 81.19 4.69 5 -5 7 85.86 7.02 -5 5 -7 90.29 5.29 -5 5 -8 1.35 2.03 5 -5 8 3.85 3.29 -5 5 -8 -0.71 2.03 5 -5 8 -0.32 2.35 5 -5 8 1.50 3.27 -5 5 -8 -0.84 2.30 5 -5 9 286.97 14.59 5 -5 9 275.79 13.36 -5 5 -9 268.75 12.83 -5 5 -9 313.25 12.99 5 -5 10 5.00 2.73 -5 5 -10 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9.18 2.34 -6 9 -7 16.48 4.29 6 -9 8 61.70 6.95 -6 9 -8 56.20 4.27 -6 9 -8 73.98 7.00 6 -9 9 165.05 11.08 -6 9 -9 157.51 7.94 -6 9 -9 139.55 10.19 -6 9 -10 9.52 4.25 6 -9 12 106.60 8.44 -6 8 12 0.75 3.46 -6 8 11 2.76 3.47 -6 8 10 16.71 4.15 -6 8 9 43.26 5.43 -6 8 8 55.62 6.14 -6 8 7 8.39 3.54 -6 8 6 121.40 8.74 -6 8 5 6.22 3.49 -6 8 4 21.99 4.28 -6 8 4 21.97 4.34 6 -8 -4 21.77 2.60 -6 8 3 113.64 8.29 6 -8 -3 105.44 5.31 6 -8 -3 103.79 5.37 -6 8 3 123.04 8.29 6 -8 -2 5.34 1.85 6 -8 -2 5.19 1.91 -6 8 2 7.26 3.24 6 -8 -1 4.62 2.00 -6 8 1 5.89 3.16 6 -8 -1 4.85 1.94 -6 8 1 3.64 2.79 6 -8 0 119.30 5.43 -6 8 0 114.32 8.43 -6 8 0 104.47 6.44 6 -8 0 121.21 6.41 6 -8 1 2.73 1.60 6 -8 1 -0.24 2.12 -6 8 -1 1.53 1.90 -6 8 -1 6.60 3.22 -6 8 -2 5.36 3.17 6 -8 2 2.69 2.54 6 -8 2 1.69 2.54 -6 8 -2 3.45 1.81 6 -8 3 261.39 12.02 -6 8 -3 266.83 13.30 6 -8 4 148.30 8.81 -6 8 -4 125.63 6.41 -6 8 -4 146.76 9.29 6 -8 5 17.51 4.01 -6 8 -5 13.66 2.57 -6 8 -5 13.13 3.77 6 -8 6 172.23 10.20 -6 8 -6 192.73 10.73 6 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10 -2 -4 -0.87 1.84 10 -2 -3 74.90 8.71 10 -2 -3 80.59 4.90 10 -2 -2 254.26 11.10 10 -2 -1 12.10 4.33 10 -2 -1 9.65 2.89 10 -2 -1 17.08 5.43 10 -2 0 4.94 4.04 10 -2 0 1.90 3.06 10 -2 0 4.79 4.26 10 -2 1 194.00 14.00 10 -2 1 210.42 12.79 10 -2 2 15.06 5.24 10 -2 2 16.20 4.69 10 -2 3 18.42 5.61 10 -2 4 26.33 6.26 10 -2 5 35.94 6.65 10 -1 -13 7.16 5.09 10 -1 -12 2.66 4.38 10 -1 -11 51.11 7.45 -10 1 11 53.21 5.48 10 -1 -10 4.08 4.18 -10 1 10 4.75 3.30 10 -1 -9 4.11 4.10 10 -1 -9 -0.30 1.90 -10 1 9 0.65 3.19 10 -1 -8 38.69 6.61 -10 1 8 31.78 4.69 10 -1 -8 32.18 2.59 10 -1 -7 8.90 2.15 10 -1 -7 23.58 5.56 10 -1 -6 2.46 1.71 10 -1 -6 1.39 3.93 10 -1 -5 77.78 4.41 10 -1 -5 98.90 9.73 10 -1 -4 151.93 7.05 10 -1 -4 178.60 12.91 10 -1 -3 0.65 1.88 10 -1 -2 17.32 2.84 10 -1 -1 129.51 7.40 10 -1 -1 143.06 11.53 10 -1 0 4.21 4.53 10 -1 0 0.52 3.89 10 -1 1 12.57 5.21 10 -1 1 14.80 4.82 10 -1 2 24.35 6.06 10 -1 3 3.45 4.30 10 -1 4 19.16 6.17 10 -1 5 5.40 4.75 10 0 -13 32.61 6.54 10 0 -12 2.05 4.84 10 0 -11 -3.46 5.00 10 0 -10 63.44 4.65 10 0 -10 80.24 9.08 10 0 -9 12.34 2.19 10 0 -9 21.06 5.80 10 0 -8 7.76 4.82 10 0 -8 8.35 1.98 10 0 -7 58.11 7.93 10 0 -7 53.48 3.76 10 0 -6 32.02 6.21 10 0 -6 26.26 2.51 10 0 -5 2.85 4.27 10 0 -5 1.04 1.59 10 0 -4 -0.71 4.04 10 0 -4 3.32 1.69 10 0 -3 99.63 5.50 10 0 -2 20.71 3.08 10 0 -2 23.64 5.81 10 0 -1 5.02 4.73 10 0 0 151.06 12.24 10 0 1 6.44 4.51 10 0 2 5.70 4.55 10 0 3 29.04 6.53 10 0 4 30.80 6.82 10 1 -12 45.98 7.41 10 1 -11 0.71 4.43 10 1 -10 -0.72 5.02 10 1 -10 -0.17 1.92 10 1 -9 60.32 8.36 10 1 -8 58.79 3.78 10 1 -8 80.35 9.05 -10 -1 8 80.39 7.30 10 1 -7 1.47 4.45 10 1 -7 -0.12 1.68 -10 -1 7 2.81 3.86 10 1 -6 16.91 5.71 10 1 -6 9.70 1.70 -10 -1 6 14.32 4.60 10 1 -5 53.81 7.78 10 1 -5 53.63 3.44 -10 -1 5 64.51 7.32 10 1 -4 -0.74 4.66 10 1 -4 2.71 1.70 10 1 -3 -1.22 1.96 10 1 -2 53.39 7.88 10 1 -1 -1.48 4.84 10 1 0 2.22 4.31 10 1 1 45.09 7.39 10 1 2 49.74 7.65 -10 -2 11 18.78 4.45 10 2 -10 7.39 5.05 -10 -2 10 14.88 4.24 10 2 -9 0.75 4.41 10 2 -9 1.13 1.75 -10 -2 9 1.37 3.61 10 2 -8 24.08 6.15 10 2 -8 19.72 2.29 -10 -2 8 33.36 5.57 10 2 -7 59.20 8.29 10 2 -7 42.01 3.31 -10 -2 7 70.12 7.44 10 2 -6 -1.53 4.50 10 2 -6 -0.09 1.39 -10 -2 6 -0.53 3.82 10 2 -5 0.76 4.70 10 2 -5 1.15 1.49 -10 -2 5 0.55 4.04 10 2 -4 59.19 3.83 -10 -2 4 78.79 8.12 -10 -2 3 5.27 4.27 -10 -2 2 35.57 6.32 10 2 -2 31.40 6.57 10 2 -1 167.62 13.05 -10 -2 1 133.86 11.28 10 2 0 60.64 8.44 -10 -3 12 -0.41 3.67 -10 -3 11 -0.89 3.45 -10 -3 10 55.22 6.64 -10 -3 9 43.83 6.53 -10 -3 8 -2.11 3.89 -10 -3 7 0.55 4.08 10 3 -7 -1.57 4.56 10 3 -6 142.44 12.64 -10 -3 6 147.23 11.15 10 3 -5 3.16 4.85 -10 -3 5 2.34 4.19 -10 -3 4 73.43 8.21 -10 -3 3 82.30 8.81 -10 -4 12 22.02 5.31 -10 -4 11 49.99 6.58 -10 -4 10 6.87 4.51 -10 -4 9 27.63 5.98 -10 -4 8 95.16 9.13 -10 -4 7 14.81 5.00 -10 -4 6 3.66 4.33 -10 -4 5 108.09 9.98 -10 -5 12 5.85 4.62 -10 -5 11 21.26 5.84 -10 -5 10 11.15 5.08 -10 -5 9 6.68 4.86 -10 -5 8 31.88 6.51 11 -7 -1 18.15 4.71 11 -7 0 112.60 8.90 11 -6 -2 80.02 7.51 11 -6 -1 -4.06 4.00 11 -6 0 -0.47 3.82 11 -5 -2 18.15 4.66 11 -5 -1 43.09 6.03 11 -5 0 8.83 4.35 -11 5 -3 -3.66 3.91 11 -4 -1 28.78 5.45 11 -4 0 127.83 10.05 11 -2 -2 54.75 4.87 11 -2 -1 91.98 6.74 11 -1 -5 3.07 2.10 11 -1 -4 5.66 2.26 11 -1 -3 43.75 4.19 11 0 -6 15.73 2.51 -11 -2 9 3.49 4.25 -11 -2 8 -1.58 4.25 -11 -2 7 16.05 5.17 -11 -2 6 98.80 9.60 -11 -3 10 0.51 4.11 -11 -3 9 34.58 6.00 -11 -3 8 81.02 8.66 0 0 0 0.00 0.00 TITL ew1-37b_new in P-1 REM P-1 (#2 in standard setting) CELL 0.71073 8.621878 10.806386 12.999176 103.0780 104.0133 98.8630 ZERR 1.00 0.000265 0.000279 0.000447 0.0025 0.0028 0.0023 LATT 1 SFAC C H N O F Cu Zr UNIT 48.00 52.00 8.00 1.20 6.00 2.00 1.00 REM CrysAlisPro recorded range (K): Min=99.8; max=100.9; aver:100.4 TEMP -173 SIZE 0.05 0.13 0.98 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 40675 _shelx_res_file ; TITL ew1-37b_new_a.res in P-1 ew1-37b_new.res created by SHELXL-2016/6 at 12:33:27 on 28-Jun-2021 REM Old TITL ew1-37b_new in P-1 REM SHELXT solution in P-1 REM R1 0.120, Rweak 0.007, Alpha 0.049, Orientation as input REM Formula found by SHELXT: C50 N8 F6 Cu3 CELL 0.71073 8.6219 10.8064 12.9992 103.078 104.013 98.863 ZERR 1 0.0003 0.0003 0.0004 0.002 0.003 0.002 LATT 1 SFAC C H Cu F N O Zr UNIT 48 50.27 2 6 8 1.13 1 L.S. 100 PLAN 5 SIZE 0.05 0.13 0.98 TEMP -173 CONF BOND $H list 4 MORE -1 fmap 2 53 acta OMIT 0 1 1 OMIT -1 1 0 REM REM REM WGHT 0.039700 0.389800 FVAR 0.44889 0.56682 CU1 3 0.305482 0.354204 0.697561 11.00000 0.02111 0.01747 = 0.01614 0.00225 -0.00092 0.00081 N1 5 0.495250 0.365432 0.828448 11.00000 0.01995 0.01729 = 0.01275 0.00328 0.00218 0.00262 C1 1 0.562342 0.267389 0.852929 11.00000 0.02531 0.02051 = 0.01840 0.00650 0.00733 0.00776 N2 5 0.342385 0.546523 0.776006 11.00000 0.01929 0.01669 = 0.01982 0.00510 0.00155 0.00285 C2 1 0.711980 0.290470 0.932346 11.00000 0.02323 0.02549 = 0.02047 0.01001 0.00949 0.01139 AFIX 43 H2 2 0.756689 0.219858 0.948974 11.00000 -1.20000 AFIX 0 N3 5 0.087288 0.231592 0.615975 11.00000 0.02260 0.01416 = 0.01751 0.00289 0.00217 0.00381 C3 1 0.794723 0.417350 0.986713 11.00000 0.01678 0.03253 = 0.02037 0.01092 0.00359 0.00519 AFIX 43 H3 2 0.898128 0.435022 1.040244 11.00000 -1.20000 AFIX 0 N4 5 0.342304 0.297250 0.544502 11.00000 0.02507 0.02063 = 0.01905 0.00822 0.00664 0.00491 C4 1 0.725698 0.518737 0.962559 11.00000 0.01801 0.02062 = 0.02035 0.00390 0.00227 0.00067 AFIX 43 H4 2 0.780962 0.606656 0.999235 11.00000 -1.20000 AFIX 0 C5 1 0.574508 0.489800 0.883916 11.00000 0.01652 0.01672 = 0.01479 0.00405 0.00511 0.00331 C6 1 0.486935 0.591343 0.856440 11.00000 0.01693 0.01741 = 0.01597 0.00482 0.00579 0.00315 C7 1 0.545035 0.723167 0.911163 11.00000 0.02113 0.01879 = 0.01938 0.00431 0.00642 0.00079 AFIX 43 H7 2 0.649798 0.753655 0.964086 11.00000 -1.20000 AFIX 0 C8 1 0.447207 0.809054 0.886991 11.00000 0.03343 0.01680 = 0.02238 0.00480 0.01232 0.00394 AFIX 43 H8 2 0.484553 0.899537 0.923175 11.00000 -1.20000 AFIX 0 C9 1 0.295461 0.762734 0.810236 11.00000 0.02889 0.02224 = 0.03106 0.01312 0.01281 0.01018 AFIX 43 H9 2 0.224458 0.819860 0.796195 11.00000 -1.20000 AFIX 0 C10 1 0.247607 0.630600 0.753410 11.00000 0.02229 0.02311 = 0.02929 0.01246 0.00371 0.00453 C11 1 0.465318 0.131492 0.792276 11.00000 0.04558 0.01895 = 0.02647 0.00330 -0.00095 0.01036 AFIX 137 H11A 2 0.374488 0.110516 0.822909 11.00000 -1.50000 H11B 2 0.536537 0.069734 0.800414 11.00000 -1.50000 H11C 2 0.421624 0.125560 0.713932 11.00000 -1.50000 AFIX 0 C12 1 0.089726 0.574749 0.662438 11.00000 0.03335 0.02811 = 0.07256 0.01919 -0.01903 0.00291 AFIX 137 H12A 2 0.113803 0.542757 0.592501 11.00000 -1.50000 H12B 2 0.027094 0.642511 0.656716 11.00000 -1.50000 H12C 2 0.025358 0.502569 0.678793 11.00000 -1.50000 AFIX 0 C13 1 -0.035737 0.203741 0.659561 11.00000 0.02303 0.01732 = 0.02452 0.00314 0.00549 0.00526 C14 1 -0.190169 0.133083 0.592567 11.00000 0.02339 0.02037 = 0.04278 0.00567 0.00867 0.00191 AFIX 43 H14 2 -0.276649 0.114742 0.624100 11.00000 -1.20000 AFIX 0 C15 1 -0.216798 0.089905 0.480196 11.00000 0.02469 0.02167 = 0.03822 -0.00170 -0.00588 0.00063 AFIX 43 H15 2 -0.322268 0.042926 0.433723 11.00000 -1.20000 AFIX 0 C16 1 -0.089589 0.115237 0.435569 11.00000 0.03347 0.01948 = 0.02267 0.00069 -0.00542 0.00501 AFIX 43 H16 2 -0.105281 0.084169 0.358515 11.00000 -1.20000 AFIX 0 C17 1 0.062221 0.187221 0.505672 11.00000 0.02757 0.01484 = 0.01697 0.00444 -0.00069 0.00620 C18 1 0.207568 0.218197 0.466769 11.00000 0.03146 0.01957 = 0.01657 0.00772 0.00214 0.00698 C19 1 0.208268 0.168178 0.358586 11.00000 0.04734 0.02258 = 0.01798 0.00651 0.00562 0.00899 AFIX 43 H19 2 0.112010 0.114338 0.304771 11.00000 -1.20000 AFIX 0 C20 1 0.351251 0.198142 0.330812 11.00000 0.06023 0.03187 = 0.02447 0.01185 0.02225 0.01633 AFIX 43 H20 2 0.354850 0.164937 0.257431 11.00000 -1.20000 AFIX 0 C21 1 0.488847 0.276687 0.410479 11.00000 0.04646 0.03450 = 0.03565 0.01776 0.02391 0.01698 AFIX 43 H21 2 0.588640 0.296366 0.392590 11.00000 -1.20000 AFIX 0 C22 1 0.481557 0.327049 0.516906 11.00000 0.03036 0.02391 = 0.03096 0.01374 0.01317 0.01071 C23 1 0.001667 0.251387 0.781690 11.00000 0.03089 0.03411 = 0.02784 0.00683 0.01225 0.00446 AFIX 137 H23A 2 0.106137 0.232552 0.816790 11.00000 -1.50000 H23B 2 -0.085860 0.207350 0.805470 11.00000 -1.50000 H23C 2 0.009325 0.345593 0.803131 11.00000 -1.50000 AFIX 0 C24 1 0.626466 0.415078 0.606516 11.00000 0.02582 0.03673 = 0.03836 0.01471 0.01342 0.00340 AFIX 137 H24A 2 0.593595 0.492033 0.643469 11.00000 -1.50000 H24B 2 0.713290 0.442318 0.574399 11.00000 -1.50000 H24C 2 0.667181 0.368394 0.660221 11.00000 -1.50000 AFIX 0 ZR1 7 0.000000 1.000000 1.000000 10.50000 0.01462 0.02394 = 0.03837 0.01715 0.00458 0.00405 F1 4 0.090811 0.995180 0.870820 11.00000 0.03896 0.03548 = 0.05065 0.02095 0.01982 0.01287 F2 4 -0.054732 0.803497 0.959257 11.00000 0.02565 0.01879 = 0.04794 0.01043 0.00340 0.00224 F3 4 0.220274 1.000415 1.094560 11.00000 0.02075 0.02305 = 0.05108 0.00814 -0.00416 0.00523 AFIX 6 O1 6 -0.106235 0.624733 0.806055 21.00000 0.04146 0.03887 = 0.02438 0.00005 0.01169 0.00091 H1A 2 -0.045474 0.641036 0.764081 21.00000 -1.50000 H1B 2 -0.087438 0.692874 0.861724 21.00000 -1.50000 AFIX 0 HKLF 4 REM ew1-37b_new_a.res in P-1 REM R1 = 0.0351 for 4588 Fo > 4sig(Fo) and 0.0475 for all 5673 data REM 312 parameters refined using 0 restraints END WGHT 0.0397 0.3898 REM Highest difference peak 0.589, deepest hole -0.538, 1-sigma level 0.080 Q1 1 0.3826 0.2826 0.6048 11.00000 0.05 0.59 Q2 1 -0.0464 0.7995 0.9004 11.00000 0.05 0.49 Q3 1 0.3134 0.3565 0.6012 11.00000 0.05 0.44 Q4 1 0.5199 0.5371 0.8834 11.00000 0.05 0.44 Q5 1 -0.0118 0.9985 1.0782 11.00000 0.05 0.41 ; _shelx_res_checksum 1173 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu1 0.30548(3) 0.35420(2) 0.69756(2) 0.02018(8) Uani d 1 . . N N1 0.4953(2) 0.36543(16) 0.82845(13) 0.0174(3) Uani d 1 . . C C1 0.5623(3) 0.26739(19) 0.85293(17) 0.0207(4) Uani d 1 . . N N2 0.3424(2) 0.54652(16) 0.77601(14) 0.0195(3) Uani d 1 . . C C2 0.7120(3) 0.2905(2) 0.93235(17) 0.0212(4) Uani d 1 . . H H2 0.756689 0.219858 0.948974 0.025 Uiso calc 1 . . N N3 0.0873(2) 0.23159(15) 0.61598(14) 0.0190(3) Uani d 1 . . C C3 0.7947(3) 0.4174(2) 0.98671(17) 0.0230(4) Uani d 1 . . H H3 0.898128 0.435022 1.040244 0.028 Uiso calc 1 . . N N4 0.3423(2) 0.29725(16) 0.54450(14) 0.0211(4) Uani d 1 . . C C4 0.7257(2) 0.5187(2) 0.96256(17) 0.0210(4) Uani d 1 . . H H4 0.780962 0.606656 0.999235 0.025 Uiso calc 1 . . C C5 0.5745(2) 0.48980(18) 0.88392(16) 0.0160(4) Uani d 1 . . C C6 0.4869(2) 0.59134(18) 0.85644(16) 0.0166(4) Uani d 1 . . C C7 0.5450(3) 0.72317(19) 0.91116(17) 0.0202(4) Uani d 1 . . H H7 0.649798 0.753655 0.964086 0.024 Uiso calc 1 . . C C8 0.4472(3) 0.8091(2) 0.88699(18) 0.0237(4) Uani d 1 . . H H8 0.484553 0.899537 0.923175 0.028 Uiso calc 1 . . C C9 0.2955(3) 0.7627(2) 0.81024(19) 0.0251(4) Uani d 1 . . H H9 0.224458 0.819860 0.796195 0.030 Uiso calc 1 . . C C10 0.2476(3) 0.6306(2) 0.75341(19) 0.0247(4) Uani d 1 . . C C11 0.4653(3) 0.1315(2) 0.7923(2) 0.0325(5) Uani d 1 . . H H11A 0.374488 0.110516 0.822909 0.049 Uiso calc 1 . . H H11B 0.536537 0.069734 0.800414 0.049 Uiso calc 1 . . H H11C 0.421624 0.125560 0.713932 0.049 Uiso calc 1 . . C C12 0.0897(3) 0.5747(3) 0.6624(3) 0.0505(8) Uani d 1 . . H H12A 0.113803 0.542757 0.592501 0.076 Uiso calc 1 . . H H12B 0.027094 0.642511 0.656716 0.076 Uiso calc 1 . . H H12C 0.025358 0.502569 0.678793 0.076 Uiso calc 1 . . C C13 -0.0357(3) 0.20374(19) 0.65956(18) 0.0222(4) Uani d 1 . . C C14 -0.1902(3) 0.1331(2) 0.5926(2) 0.0299(5) Uani d 1 . . H H14 -0.276649 0.114742 0.624100 0.036 Uiso calc 1 . . C C15 -0.2168(3) 0.0899(2) 0.4802(2) 0.0331(6) Uani d 1 . . H H15 -0.322268 0.042926 0.433723 0.040 Uiso calc 1 . . C C16 -0.0896(3) 0.1152(2) 0.43557(19) 0.0286(5) Uani d 1 . . H H16 -0.105281 0.084169 0.358515 0.034 Uiso calc 1 . . C C17 0.0622(3) 0.18722(18) 0.50567(17) 0.0209(4) Uani d 1 . . C C18 0.2076(3) 0.2182(2) 0.46677(17) 0.0228(4) Uani d 1 . . C C19 0.2083(3) 0.1682(2) 0.35859(18) 0.0297(5) Uani d 1 . . H H19 0.112010 0.114338 0.304771 0.036 Uiso calc 1 . . C C20 0.3513(4) 0.1981(2) 0.3308(2) 0.0356(6) Uani d 1 . . H H20 0.354850 0.164937 0.257431 0.043 Uiso calc 1 . . C C21 0.4888(3) 0.2767(2) 0.4105(2) 0.0344(5) Uani d 1 . . H H21 0.588640 0.296366 0.392590 0.041 Uiso calc 1 . . C C22 0.4816(3) 0.3270(2) 0.51691(19) 0.0260(5) Uani d 1 . . C C23 0.0017(3) 0.2514(2) 0.78169(19) 0.0308(5) Uani d 1 . . H H23A 0.106137 0.232552 0.816790 0.046 Uiso calc 1 . . H H23B -0.085860 0.207350 0.805470 0.046 Uiso calc 1 . . H H23C 0.009325 0.345593 0.803131 0.046 Uiso calc 1 . . C C24 0.6265(3) 0.4151(2) 0.6065(2) 0.0325(5) Uani d 1 . . H H24A 0.593595 0.492033 0.643469 0.049 Uiso calc 1 . . H H24B 0.713290 0.442318 0.574399 0.049 Uiso calc 1 . . H H24C 0.667181 0.368394 0.660221 0.049 Uiso calc 1 . . Zr Zr1 0.000000 1.000000 1.000000 0.02476(9) Uani d 1 . . F F1 0.09081(18) 0.99518(14) 0.87082(13) 0.0384(3) Uani d 1 . . F F2 -0.05473(16) 0.80350(12) 0.95926(12) 0.0322(3) Uani d 1 . . F F3 0.22027(15) 1.00042(12) 1.09456(13) 0.0346(3) Uani d 1 . . O O1 -0.1062(4) 0.6247(3) 0.8061(3) 0.0369(11) Uani d 0.567(6) . . H H1A -0.045474 0.641036 0.764081 0.055 Uiso d 0.567(6) . . H H1B -0.087438 0.692874 0.861724 0.055 Uiso d 0.567(6) . . 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 Cu1 0.02111(14) 0.01747(13) 0.01614(13) 0.00081(10) -0.00092(10) 0.00225(9) N1 0.0200(8) 0.0173(8) 0.0128(8) 0.0026(7) 0.0022(6) 0.0033(6) C1 0.0253(10) 0.0205(10) 0.0184(10) 0.0078(8) 0.0073(8) 0.0065(8) N2 0.0193(8) 0.0167(8) 0.0198(9) 0.0029(7) 0.0016(7) 0.0051(6) C2 0.0232(10) 0.0255(10) 0.0205(10) 0.0114(8) 0.0095(8) 0.0100(8) N3 0.0226(9) 0.0142(8) 0.0175(8) 0.0038(7) 0.0022(7) 0.0029(6) C3 0.0168(9) 0.0325(11) 0.0204(10) 0.0052(8) 0.0036(8) 0.0109(9) N4 0.0251(9) 0.0206(8) 0.0191(9) 0.0049(7) 0.0066(7) 0.0082(7) C4 0.0180(10) 0.0206(10) 0.0203(10) 0.0007(8) 0.0023(8) 0.0039(8) C5 0.0165(9) 0.0167(9) 0.0148(9) 0.0033(7) 0.0051(7) 0.0040(7) C6 0.0169(9) 0.0174(9) 0.0160(9) 0.0031(7) 0.0058(7) 0.0048(7) C7 0.0211(10) 0.0188(9) 0.0194(10) 0.0008(8) 0.0064(8) 0.0043(8) C8 0.0334(12) 0.0168(9) 0.0224(11) 0.0039(9) 0.0123(9) 0.0048(8) C9 0.0289(11) 0.0222(10) 0.0311(12) 0.0102(9) 0.0128(9) 0.0131(9) C10 0.0223(10) 0.0231(10) 0.0293(12) 0.0045(8) 0.0037(9) 0.0125(9) C11 0.0456(14) 0.0190(10) 0.0265(12) 0.0104(10) -0.0010(10) 0.0033(9) C12 0.0333(14) 0.0281(13) 0.073(2) 0.0029(11) -0.0190(14) 0.0192(13) C13 0.0230(10) 0.0173(9) 0.0245(11) 0.0053(8) 0.0055(8) 0.0031(8) C14 0.0234(11) 0.0204(10) 0.0428(14) 0.0019(9) 0.0087(10) 0.0057(10) C15 0.0247(12) 0.0217(11) 0.0382(14) 0.0006(9) -0.0059(10) -0.0017(10) C16 0.0335(12) 0.0195(10) 0.0227(11) 0.0050(9) -0.0054(9) 0.0007(8) C17 0.0276(11) 0.0148(9) 0.0170(10) 0.0062(8) -0.0007(8) 0.0044(7) C18 0.0315(11) 0.0196(10) 0.0166(10) 0.0070(9) 0.0021(8) 0.0077(8) C19 0.0473(14) 0.0226(11) 0.0180(11) 0.0090(10) 0.0056(10) 0.0065(9) C20 0.0602(17) 0.0319(12) 0.0245(12) 0.0163(12) 0.0222(12) 0.0118(10) C21 0.0465(15) 0.0345(13) 0.0357(14) 0.0170(11) 0.0239(12) 0.0178(11) C22 0.0304(11) 0.0239(10) 0.0310(12) 0.0107(9) 0.0132(9) 0.0137(9) C23 0.0309(12) 0.0341(12) 0.0278(12) 0.0045(10) 0.0122(10) 0.0068(10) C24 0.0258(12) 0.0367(13) 0.0384(14) 0.0034(10) 0.0134(10) 0.0147(11) Zr1 0.01462(14) 0.02394(15) 0.03837(19) 0.00405(11) 0.00458(12) 0.01715(13) F1 0.0390(8) 0.0355(8) 0.0507(9) 0.0129(6) 0.0198(7) 0.0209(7) F2 0.0256(7) 0.0188(6) 0.0479(9) 0.0022(5) 0.0034(6) 0.0104(6) F3 0.0207(6) 0.0230(6) 0.0511(9) 0.0052(5) -0.0042(6) 0.0081(6) O1 0.041(2) 0.0389(19) 0.0244(17) 0.0009(14) 0.0117(14) 0.0001(13) 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 1 0 0.0228 -1 0 0 0.0579 1 -1 0 0.0266 1 0 0 0.0336 0 -1 -1 0.2936 1 1 0 0.0559 -1 1 1 0.2513 1 -1 -1 0.2532 0 1 1 0.2783 1 1 -1 0.2558 0 0 -1 0.4563 1 -1 1 0.2027 0 -1 0 0.0535 -1 0 1 0.3071 0 1 0 0.0604 0 -1 1 0.3390 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 N1 Cu1 N2 . . 81.40(7) y N1 Cu1 N4 . . 116.24(7) y N2 Cu1 N4 . . 120.45(7) y N3 Cu1 N1 . . 136.29(7) y N3 Cu1 N2 . . 126.16(7) y N3 Cu1 N4 . . 81.05(7) y C1 N1 Cu1 . . 127.37(14) ? C1 N1 C5 . . 119.06(17) ? C5 N1 Cu1 . . 112.61(13) ? N1 C1 C2 . . 121.76(18) ? N1 C1 C11 . . 116.67(19) ? C2 C1 C11 . . 121.55(19) ? C6 N2 Cu1 . . 112.50(13) ? C10 N2 Cu1 . . 128.32(14) ? C10 N2 C6 . . 119.07(17) ? C1 C2 H2 . . 120.5 ? C3 C2 C1 . . 119.10(19) ? C3 C2 H2 . . 120.5 ? C13 N3 Cu1 . . 125.56(14) ? C13 N3 C17 . . 119.66(18) ? C17 N3 Cu1 . . 114.36(14) ? C2 C3 H3 . . 120.3 ? C2 C3 C4 . . 119.43(19) ? C4 C3 H3 . . 120.3 ? C18 N4 Cu1 . . 113.01(14) ? C22 N4 Cu1 . . 127.62(15) ? C22 N4 C18 . . 119.34(19) ? C3 C4 H4 . . 120.5 ? C3 C4 C5 . . 118.94(18) ? C5 C4 H4 . . 120.5 ? N1 C5 C4 . . 121.67(18) ? N1 C5 C6 . . 115.42(17) ? C4 C5 C6 . . 122.90(17) ? N2 C6 C5 . . 115.28(16) ? N2 C6 C7 . . 121.72(18) ? C7 C6 C5 . . 122.97(18) ? C6 C7 H7 . . 120.6 ? C8 C7 C6 . . 118.70(19) ? C8 C7 H7 . . 120.6 ? C7 C8 H8 . . 120.1 ? C9 C8 C7 . . 119.71(19) ? C9 C8 H8 . . 120.1 ? C8 C9 H9 . . 120.5 ? C8 C9 C10 . . 119.0(2) ? C10 C9 H9 . . 120.5 ? N2 C10 C9 . . 121.56(19) ? N2 C10 C12 . . 116.3(2) ? C9 C10 C12 . . 122.1(2) ? C1 C11 H11A . . 109.5 ? C1 C11 H11B . . 109.5 ? C1 C11 H11C . . 109.5 ? H11A C11 H11B . . 109.5 ? H11A C11 H11C . . 109.5 ? H11B C11 H11C . . 109.5 ? C10 C12 H12A . . 109.5 ? C10 C12 H12B . . 109.5 ? C10 C12 H12C . . 109.5 ? H12A C12 H12B . . 109.5 ? H12A C12 H12C . . 109.5 ? H12B C12 H12C . . 109.5 ? N3 C13 C14 . . 120.9(2) ? N3 C13 C23 . . 116.93(18) ? C14 C13 C23 . . 122.2(2) ? C13 C14 H14 . . 120.2 ? C15 C14 C13 . . 119.6(2) ? C15 C14 H14 . . 120.2 ? C14 C15 H15 . . 120.2 ? C14 C15 C16 . . 119.7(2) ? C16 C15 H15 . . 120.2 ? C15 C16 H16 . . 120.7 ? C15 C16 C17 . . 118.7(2) ? C17 C16 H16 . . 120.7 ? N3 C17 C16 . . 121.5(2) ? N3 C17 C18 . . 115.35(18) ? C16 C17 C18 . . 123.1(2) ? N4 C18 C17 . . 115.47(18) ? N4 C18 C19 . . 121.7(2) ? C19 C18 C17 . . 122.8(2) ? C18 C19 H19 . . 120.6 ? C20 C19 C18 . . 118.8(2) ? C20 C19 H19 . . 120.6 ? C19 C20 H20 . . 120.3 ? C21 C20 C19 . . 119.4(2) ? C21 C20 H20 . . 120.3 ? C20 C21 H21 . . 120.0 ? C20 C21 C22 . . 119.9(2) ? C22 C21 H21 . . 120.0 ? N4 C22 C21 . . 120.8(2) ? N4 C22 C24 . . 116.8(2) ? C21 C22 C24 . . 122.3(2) ? C13 C23 H23A . . 109.5 ? C13 C23 H23B . . 109.5 ? C13 C23 H23C . . 109.5 ? H23A C23 H23B . . 109.5 ? H23A C23 H23C . . 109.5 ? H23B C23 H23C . . 109.5 ? C22 C24 H24A . . 109.5 ? C22 C24 H24B . . 109.5 ? C22 C24 H24C . . 109.5 ? H24A C24 H24B . . 109.5 ? H24A C24 H24C . . 109.5 ? H24B C24 H24C . . 109.5 ? F1 Zr1 F1 2_577 . 180.00(9) ? F1 Zr1 F2 . 2_577 89.69(6) ? F1 Zr1 F2 . . 90.31(6) ? F1 Zr1 F2 2_577 . 89.69(6) ? F1 Zr1 F2 2_577 2_577 90.31(6) ? F2 Zr1 F2 . 2_577 180.0 ? F3 Zr1 F1 2_577 . 89.90(6) ? F3 Zr1 F1 . 2_577 89.90(6) ? F3 Zr1 F1 . . 90.10(6) ? F3 Zr1 F1 2_577 2_577 90.10(6) ? F3 Zr1 F2 2_577 2_577 89.43(5) ? F3 Zr1 F2 . . 89.43(5) ? F3 Zr1 F2 . 2_577 90.57(5) ? F3 Zr1 F2 2_577 . 90.57(5) ? F3 Zr1 F3 2_577 . 180.0 ? H1A O1 H1B . . 109.5 ? 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 Cu1 N1 . 2.0208(16) y Cu1 N2 . 2.0348(17) y Cu1 N3 . 2.0123(17) y Cu1 N4 . 2.0616(18) y N1 C1 . 1.346(3) ? N1 C5 . 1.354(2) ? C1 C2 . 1.390(3) ? C1 C11 . 1.502(3) ? N2 C6 . 1.355(2) ? N2 C10 . 1.346(3) ? C2 H2 . 0.9500 ? C2 C3 . 1.380(3) ? N3 C13 . 1.344(3) ? N3 C17 . 1.356(3) ? C3 H3 . 0.9500 ? C3 C4 . 1.385(3) ? N4 C18 . 1.355(3) ? N4 C22 . 1.347(3) ? C4 H4 . 0.9500 ? C4 C5 . 1.388(3) ? C5 C6 . 1.485(3) ? C6 C7 . 1.391(3) ? C7 H7 . 0.9500 ? C7 C8 . 1.384(3) ? C8 H8 . 0.9500 ? C8 C9 . 1.378(3) ? C9 H9 . 0.9500 ? C9 C10 . 1.396(3) ? C10 C12 . 1.503(3) ? C11 H11A . 0.9800 ? C11 H11B . 0.9800 ? C11 H11C . 0.9800 ? C12 H12A . 0.9800 ? C12 H12B . 0.9800 ? C12 H12C . 0.9800 ? C13 C14 . 1.392(3) ? C13 C23 . 1.490(3) ? C14 H14 . 0.9500 ? C14 C15 . 1.379(4) ? C15 H15 . 0.9500 ? C15 C16 . 1.379(4) ? C16 H16 . 0.9500 ? C16 C17 . 1.392(3) ? C17 C18 . 1.481(3) ? C18 C19 . 1.390(3) ? C19 H19 . 0.9500 ? C19 C20 . 1.379(4) ? C20 H20 . 0.9500 ? C20 C21 . 1.377(4) ? C21 H21 . 0.9500 ? C21 C22 . 1.388(3) ? C22 C24 . 1.500(3) ? C23 H23A . 0.9800 ? C23 H23B . 0.9800 ? C23 H23C . 0.9800 ? C24 H24A . 0.9800 ? C24 H24B . 0.9800 ? C24 H24C . 0.9800 ? Zr1 F1 . 2.0113(15) y Zr1 F1 2_577 2.0113(15) ? Zr1 F2 2_577 2.0183(12) ? Zr1 F2 . 2.0183(12) y Zr1 F3 . 1.9955(13) y Zr1 F3 2_577 1.9955(13) ? O1 H1A . 0.8699 ? O1 H1B . 0.8703 ? 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 O1 H1B F2 . 0.87 1.47 2.337(4) 177 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 Cu1 N1 C1 C2 . . . . 166.88(15) ? Cu1 N1 C1 C11 . . . . -14.7(3) ? Cu1 N1 C5 C4 . . . . -167.35(15) ? Cu1 N1 C5 C6 . . . . 14.0(2) ? Cu1 N2 C6 C5 . . . . -9.8(2) ? Cu1 N2 C6 C7 . . . . 172.18(15) ? Cu1 N2 C10 C9 . . . . -175.40(16) ? Cu1 N2 C10 C12 . . . . 3.4(3) ? Cu1 N3 C13 C14 . . . . 170.26(16) ? Cu1 N3 C13 C23 . . . . -10.0(3) ? Cu1 N3 C17 C16 . . . . -171.70(16) ? Cu1 N3 C17 C18 . . . . 9.7(2) ? Cu1 N4 C18 C17 . . . . -0.4(2) ? Cu1 N4 C18 C19 . . . . -179.26(16) ? Cu1 N4 C22 C21 . . . . 177.41(16) ? Cu1 N4 C22 C24 . . . . -1.9(3) ? N1 C1 C2 C3 . . . . -0.7(3) ? N1 C5 C6 N2 . . . . -2.7(3) ? N1 C5 C6 C7 . . . . 175.24(18) ? C1 N1 C5 C4 . . . . 2.3(3) ? C1 N1 C5 C6 . . . . -176.43(18) ? C1 C2 C3 C4 . . . . 1.2(3) ? N2 C6 C7 C8 . . . . 4.0(3) ? C2 C3 C4 C5 . . . . 0.0(3) ? N3 C13 C14 C15 . . . . 0.7(3) ? N3 C17 C18 N4 . . . . -6.1(3) ? N3 C17 C18 C19 . . . . 172.72(19) ? C3 C4 C5 N1 . . . . -1.7(3) ? C3 C4 C5 C6 . . . . 176.86(19) ? N4 C18 C19 C20 . . . . 1.3(3) ? C4 C5 C6 N2 . . . . 178.58(18) ? C4 C5 C6 C7 . . . . -3.4(3) ? C5 N1 C1 C2 . . . . -1.0(3) ? C5 N1 C1 C11 . . . . 177.37(19) ? C5 C6 C7 C8 . . . . -173.85(19) ? C6 N2 C10 C9 . . . . 0.5(3) ? C6 N2 C10 C12 . . . . 179.4(2) ? C6 C7 C8 C9 . . . . 0.2(3) ? C7 C8 C9 C10 . . . . -3.8(3) ? C8 C9 C10 N2 . . . . 3.6(3) ? C8 C9 C10 C12 . . . . -175.2(2) ? C10 N2 C6 C5 . . . . 173.65(18) ? C10 N2 C6 C7 . . . . -4.4(3) ? C11 C1 C2 C3 . . . . -179.0(2) ? C13 N3 C17 C16 . . . . 1.3(3) ? C13 N3 C17 C18 . . . . -177.34(18) ? C13 C14 C15 C16 . . . . 1.1(4) ? C14 C15 C16 C17 . . . . -1.7(3) ? C15 C16 C17 N3 . . . . 0.5(3) ? C15 C16 C17 C18 . . . . 179.0(2) ? C16 C17 C18 N4 . . . . 175.31(19) ? C16 C17 C18 C19 . . . . -5.9(3) ? C17 N3 C13 C14 . . . . -1.9(3) ? C17 N3 C13 C23 . . . . 177.87(19) ? C17 C18 C19 C20 . . . . -177.4(2) ? C18 N4 C22 C21 . . . . -0.7(3) ? C18 N4 C22 C24 . . . . 179.95(19) ? C18 C19 C20 C21 . . . . -0.2(3) ? C19 C20 C21 C22 . . . . -1.4(4) ? C20 C21 C22 N4 . . . . 1.8(3) ? C20 C21 C22 C24 . . . . -178.8(2) ? C22 N4 C18 C17 . . . . 177.93(18) ? C22 N4 C18 C19 . . . . -0.9(3) ? C23 C13 C14 C15 . . . . -179.0(2) ? _cod_database_fobs_code 2243876