#------------------------------------------------------------------------------ #$Date: 2024-08-05 20:54:32 +0300 (Mon, 05 Aug 2024) $ #$Revision: 293734 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/19/1571924.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_1571924 loop_ _publ_author_name 'Simms, Megan E.' 'Li, Zhiyao' 'Sibley, Megan M.' 'Ivanov, Alexander S.' 'Lara, Caroline M.' 'Johnstone, Timothy C.' 'Kertesz, Vilmos' 'Fears, Amanda' 'White, Frankie D.' 'Thorek, Daniel L. J.' 'Thiele, Nikki A.' _publ_section_title ; PYTA: a universal chelator for advancing the theranostic palette of nuclear medicine. ; _journal_issue 29 _journal_name_full 'Chemical science' _journal_page_first 11279 _journal_page_last 11286 _journal_paper_doi 10.1039/d3sc06854d _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C26 H32 Cu N6 O8, 4(H2 O)' _chemical_formula_sum 'C26 H40 Cu N6 O12' _chemical_formula_weight 692.18 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary heavy _audit_creation_date 2024-03-11 _audit_creation_method ; Olex2 1.5-beta (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _audit_update_record ; 2024-03-11 deposited with the CCDC. 2024-06-06 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 99.63(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.012(5) _cell_length_b 14.323(5) _cell_length_c 15.919(6) _cell_measurement_reflns_used 6135 _cell_measurement_temperature 300.80 _cell_measurement_theta_max 34.47 _cell_measurement_theta_min 2.35 _cell_volume 2925.0(19) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.5-beta (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-beta (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XS (Sheldrick, 2008)' _diffrn_ambient_temperature 300.80 _diffrn_measured_fraction_theta_full 0.975 _diffrn_measured_fraction_theta_max 0.902 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_unetI/netI 0.0383 _diffrn_reflns_Laue_measured_fraction_full 0.975 _diffrn_reflns_Laue_measured_fraction_max 0.902 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 24964 _diffrn_reflns_point_group_measured_fraction_full 0.975 _diffrn_reflns_point_group_measured_fraction_max 0.902 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 36.761 _diffrn_reflns_theta_min 2.131 _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.822 _exptl_absorpt_correction_T_max 0.7472 _exptl_absorpt_correction_T_min 0.6508 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0935 before and 0.0473 after correction. The Ratio of minimum to maximum transmission is 0.8710. The \l/2 correction factor is Not present. ; _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.572 _exptl_crystal_description 'rect. Prism' _exptl_crystal_F_000 1452 _exptl_crystal_size_max 0.68 _exptl_crystal_size_mid 0.259 _exptl_crystal_size_min 0.246 _refine_diff_density_max 0.437 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.065 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 226 _refine_ls_number_reflns 6606 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.031 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0366 _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^)+(0.0512P)^2^+0.9556P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0928 _refine_ls_wR_factor_ref 0.0985 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5585 _reflns_number_total 6606 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3sc06854d2.cif _cod_data_source_block cypytatry3 _cod_depositor_comments 'Adding full bibliography for 1571923--1571925.cif.' _cod_database_code 1571924 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.823 _shelx_estimated_absorpt_t_min 0.605 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2.a Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B) 2.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C5(H5), C6(H6) ; _shelx_res_file ; TITL CyPytaTry3 in C2/c #15 cypytatry3.res created by SHELXL-2018/3 at 06:05:03 on 11-Mar-2024 REM reset to C2/c #15 CELL 0.71073 13.0122 14.3225 15.9191 90 99.6283 90 ZERR 4 0.0049 0.0051 0.0062 0 0.0207 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H N O Cu UNIT 104 160 24 48 4 L.S. 20 PLAN 10 SIZE 0.246 0.259 0.68 TEMP 27.65 CONF BOND MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.051200 0.955600 FVAR 0.12018 CU1 5 0.500000 0.825942 0.750000 10.50000 0.02172 0.01844 = 0.02188 0.00000 0.00187 0.00000 O1 4 0.357527 0.754072 1.063267 11.00000 0.04627 0.04601 = 0.03066 0.00731 0.01113 -0.00246 O2 4 0.328334 0.897729 1.018304 11.00000 0.05637 0.04208 = 0.03883 -0.00158 0.02210 0.00597 O3 4 0.138638 0.775575 0.568937 11.00000 0.03646 0.04097 = 0.04659 0.00172 -0.00991 -0.00896 O4 4 0.131220 0.929447 0.558033 11.00000 0.03881 0.04302 = 0.13091 0.01759 -0.02588 -0.00027 N1 3 0.500000 0.690284 0.750000 10.50000 0.02519 0.01992 = 0.02707 0.00000 0.00417 0.00000 N2 3 0.500000 0.965266 0.750000 10.50000 0.02344 0.01922 = 0.02336 0.00000 0.00365 0.00000 N3 3 0.338533 0.795893 0.681593 11.00000 0.02514 0.02346 = 0.02243 -0.00093 0.00122 -0.00222 N4 3 0.407216 0.864278 0.862656 11.00000 0.02512 0.02304 = 0.02138 -0.00084 0.00306 0.00032 C1 1 0.575326 0.643876 0.801484 11.00000 0.02851 0.02305 = 0.03310 0.00508 0.00830 0.00355 C2 1 0.576413 0.547228 0.803535 11.00000 0.04262 0.02385 = 0.06236 0.01131 0.01350 0.00725 AFIX 43 H2 2 0.627611 0.515258 0.840254 11.00000 -1.20000 AFIX 0 C3 1 0.500000 0.499373 0.750000 10.50000 0.05262 0.01810 = 0.08297 0.00000 0.01706 0.00000 AFIX 43 H3 2 0.500001 0.434440 0.750000 10.50000 -1.20000 AFIX 0 C4 1 0.471749 1.012959 0.815774 11.00000 0.02526 0.02126 = 0.02724 -0.00398 0.00297 0.00006 C5 1 0.468503 1.109656 0.816463 11.00000 0.03771 0.02219 = 0.03977 -0.00695 0.00402 0.00134 AFIX 43 H5 2 0.445553 1.141387 0.860821 11.00000 -1.20000 AFIX 0 C6 1 0.500000 1.158223 0.750000 10.50000 0.04268 0.01832 = 0.05118 0.00000 0.00421 0.00000 AFIX 43 H6 2 0.499999 1.223156 0.749999 10.50000 -1.20000 AFIX 0 C7 1 0.447336 0.957039 0.890031 11.00000 0.03267 0.02636 = 0.02406 -0.00624 0.00624 -0.00143 AFIX 23 H7A 2 0.509981 0.950364 0.932182 11.00000 -1.20000 H7B 2 0.395907 0.990002 0.916400 11.00000 -1.20000 AFIX 0 C8 1 0.416933 0.796464 0.932534 11.00000 0.03064 0.02890 = 0.02333 0.00246 0.00531 0.00367 AFIX 23 H8A 2 0.490496 0.787622 0.954216 11.00000 -1.20000 H8B 2 0.389665 0.737138 0.909287 11.00000 -1.20000 AFIX 0 C9 1 0.362344 0.820988 1.007672 11.00000 0.03169 0.03737 = 0.02385 0.00022 0.00545 -0.00273 C10 1 0.345330 0.702247 0.643356 11.00000 0.03255 0.02799 = 0.02902 -0.00815 -0.00004 -0.00575 AFIX 23 H10A 2 0.364421 0.708604 0.587285 11.00000 -1.20000 H10B 2 0.277866 0.671822 0.636887 11.00000 -1.20000 AFIX 0 C11 1 0.294351 0.865024 0.616059 11.00000 0.02756 0.03140 = 0.02724 0.00556 -0.00091 -0.00292 AFIX 23 H11A 2 0.333838 0.861812 0.569574 11.00000 -1.20000 H11B 2 0.304709 0.926879 0.640844 11.00000 -1.20000 AFIX 0 C12 1 0.177809 0.853865 0.578638 11.00000 0.02904 0.03796 = 0.03125 0.00312 -0.00357 -0.00258 C13 1 0.299351 0.870415 0.814896 11.00000 0.02397 0.02808 = 0.02549 0.00027 0.00384 0.00319 AFIX 23 H13A 2 0.290333 0.929380 0.784584 11.00000 -1.20000 H13B 2 0.250437 0.868655 0.854647 11.00000 -1.20000 AFIX 0 C14 1 0.276088 0.790673 0.751830 11.00000 0.02565 0.02896 = 0.02546 0.00046 0.00312 -0.00523 AFIX 23 H14A 2 0.290624 0.731933 0.781792 11.00000 -1.20000 H14B 2 0.202556 0.791638 0.727615 11.00000 -1.20000 AFIX 0 O6 4 0.274671 0.583199 0.834699 11.00000 0.08478 0.04833 = 0.06639 0.01454 0.04149 0.01282 H6A 2 0.238904 0.600389 0.874906 11.00000 0.07376 H6B 2 0.316491 0.541468 0.871258 11.00000 0.07256 O5 4 0.426427 0.596739 1.034255 11.00000 0.04118 0.04188 = 0.09327 -0.00010 -0.00800 0.00037 H5A 2 0.495207 0.591713 1.042192 11.00000 0.06807 H5B 2 0.407321 0.574697 0.997899 11.00000 0.10605 H1 2 0.386526 0.702767 1.049847 11.00000 0.06279 HKLF 4 REM CyPytaTry3 in C2/c #15 REM wR2 = 0.098525, GooF = S = 1.03075, Restrained GooF = 1.03075 for all data REM R1 = 0.036574 for 5585 Fo > 4sig(Fo) and 0.046102 for all 6606 data REM 226 parameters refined using 0 restraints END WGHT 0.0512 0.9556 REM Highest difference peak 0.437, deepest hole -0.349, 1-sigma level 0.065 Q1 1 0.5210 1.1337 0.7208 11.00000 0.05 0.44 Q2 1 0.1266 0.7934 0.6015 11.00000 0.05 0.43 Q3 1 0.4641 0.9851 0.8529 11.00000 0.05 0.42 Q4 1 0.1331 0.9168 0.6014 11.00000 0.05 0.39 Q5 1 0.4807 0.9930 0.7811 11.00000 0.05 0.36 Q6 1 0.5241 0.6747 0.7769 11.00000 0.05 0.35 Q7 1 0.5758 0.5982 0.8001 11.00000 0.05 0.35 Q8 1 0.3793 0.6775 0.6729 11.00000 0.05 0.35 Q9 1 0.4607 1.0597 0.8084 11.00000 0.05 0.34 Q10 1 0.4788 0.8224 0.7047 11.00000 0.05 0.34 ; _shelx_res_checksum 36927 _shelx_hkl_file ; 2 0 0 289.74 10.74 4 0 0 0.49 0.09 -4 0 0 0.53 0.09 -4 0 0 0.49 0.10 4 0 0 0.54 0.07 -4 0 0 0.39 0.07 6 0 0 390.08 17.74 -8 0 0 63.44 2.05 -8 0 0 62.61 2.03 -10 0 0 31.92 1.20 -10 0 0 32.51 1.23 -12 0 0 58.65 2.05 -12 0 0 56.77 2.01 -14 0 0 92.15 3.04 -14 0 0 89.36 3.09 -16 0 0 3.08 0.51 -16 0 0 4.02 0.57 -18 0 0 1.06 0.38 -18 0 0 0.65 0.37 -20 0 0 1.20 0.42 -20 0 0 2.63 0.51 1 -1 0 159.60 6.53 -1 1 0 175.68 6.70 1 1 0 156.17 6.23 3 -1 0 144.69 7.51 3 1 0 139.38 7.11 5 -1 0 358.80 16.21 5 1 0 362.62 15.82 -7 -1 0 27.50 1.00 -7 -1 0 28.47 0.96 -7 1 0 28.47 1.00 -7 1 0 28.13 1.01 -9 -1 0 7.03 0.42 -9 -1 0 7.74 0.46 -9 1 0 7.97 0.45 -9 1 0 7.07 0.43 -11 -1 0 7.41 0.52 -11 -1 0 7.83 0.49 -11 1 0 7.62 0.50 -11 1 0 6.82 0.48 -13 -1 0 1.65 0.36 -13 -1 0 1.34 0.29 -13 1 0 1.46 0.32 -13 1 0 0.69 0.25 -15 -1 0 0.00 0.27 -15 -1 0 0.18 0.23 -15 1 0 0.03 0.23 -15 1 0 -0.01 0.21 -17 -1 0 0.42 0.28 -17 -1 0 0.06 0.33 -17 1 0 0.43 0.30 -17 1 0 0.50 0.32 -19 -1 0 3.34 0.59 -19 -1 0 5.45 0.74 -19 1 0 4.69 0.71 -19 1 0 3.51 0.56 -21 -1 0 0.66 0.41 -21 1 0 1.65 0.82 -2 -2 0 158.07 8.12 2 -2 0 168.84 8.05 2 2 0 157.08 7.38 -2 2 0 148.56 7.75 4 -2 0 145.51 8.59 4 2 0 142.75 8.02 -4 2 0 131.64 8.21 6 -2 0 167.05 10.77 6 2 0 169.26 10.12 -6 2 0 165.10 11.89 -8 -2 0 69.09 2.23 -8 2 0 67.14 2.18 -10 -2 0 1.38 0.28 -10 -2 0 1.30 0.25 -10 2 0 0.86 0.21 -10 2 0 1.91 0.29 -12 -2 0 17.95 0.90 -12 -2 0 19.11 0.85 -12 2 0 16.11 0.83 -12 2 0 17.96 0.85 -14 -2 0 22.40 1.03 -14 -2 0 21.53 1.10 -14 2 0 21.00 1.03 -14 2 0 23.93 1.07 -16 -2 0 -0.02 0.28 -16 -2 0 0.19 0.26 -16 2 0 0.22 0.25 -16 2 0 -0.14 0.22 -18 -2 0 1.30 0.38 -18 -2 0 1.49 0.46 -18 2 0 1.75 0.42 -20 -2 0 0.70 0.43 -20 2 0 1.42 0.46 -20 2 0 1.91 0.45 -1 -3 0 262.59 11.26 1 -3 0 275.58 12.01 1 3 0 266.18 11.35 -1 3 0 259.09 11.79 -3 -3 0 0.69 0.05 -3 -3 0 1.35 0.16 3 -3 0 0.89 0.08 3 3 0 0.70 0.07 -3 3 0 0.72 0.08 -3 3 0 0.89 0.11 3 3 0 0.75 0.06 5 -3 0 108.88 8.21 -5 3 0 107.93 8.09 5 3 0 104.84 7.43 -7 -3 0 24.69 0.86 -7 -3 0 26.18 0.93 7 -3 0 25.36 0.80 -7 -3 0 25.70 0.79 -7 -3 0 26.18 0.99 -7 3 0 25.16 0.94 -7 3 0 26.60 0.91 7 3 0 25.75 0.78 -7 3 0 24.73 0.80 -11 -3 0 34.96 1.68 -11 -3 0 34.12 1.39 -11 3 0 36.21 1.32 -13 -3 0 20.99 1.06 -13 -3 0 22.02 0.97 -13 3 0 21.27 0.98 -13 3 0 20.83 0.99 -15 -3 0 10.55 0.70 -15 -3 0 11.23 0.83 -15 3 0 11.01 0.72 -15 3 0 11.09 0.73 -17 -3 0 0.40 0.39 -17 3 0 0.68 0.33 -17 3 0 0.40 0.28 -19 -3 0 3.21 0.61 -19 3 0 5.75 0.73 -21 -3 0 0.48 0.58 -2 -4 0 20.99 0.73 2 -4 0 19.94 0.66 -2 -4 0 19.55 0.66 -2 4 0 20.50 0.70 2 4 0 20.29 0.63 2 4 0 20.74 0.66 -2 4 0 20.51 0.67 4 -4 0 62.76 6.15 -4 -4 0 62.08 5.66 4 4 0 64.53 5.65 -4 4 0 65.99 6.27 6 -4 0 17.60 0.60 -6 -4 0 17.46 0.74 -6 -4 0 17.76 0.59 -6 -4 0 18.37 0.61 -6 4 0 17.27 0.71 -6 4 0 18.11 0.66 6 4 0 17.45 0.58 -6 4 0 18.54 0.61 -8 -4 0 58.78 1.72 -8 -4 0 58.57 1.97 8 -4 0 56.06 1.73 -8 4 0 58.26 1.85 -8 4 0 58.41 1.91 -8 4 0 55.47 1.73 -10 -4 0 57.86 2.02 10 -4 0 55.92 1.69 -10 4 0 55.76 1.94 -10 4 0 56.83 1.89 -12 -4 0 5.72 0.62 -12 4 0 4.71 0.41 -12 4 0 5.85 0.56 -14 -4 0 0.13 0.30 -14 4 0 0.07 0.23 -16 -4 0 2.39 0.52 -16 4 0 3.10 0.48 -16 4 0 2.13 0.42 -18 -4 0 0.37 0.38 -18 4 0 0.24 0.29 -18 4 0 0.26 0.33 -20 -4 0 0.40 0.39 -1 -5 0 155.30 9.52 -1 -5 0 155.61 9.71 1 -5 0 183.48 11.01 -1 5 0 148.04 9.71 -3 -5 0 108.32 8.00 3 -5 0 118.37 8.92 -3 5 0 129.52 10.51 3 5 0 113.19 8.07 -5 -5 0 0.18 0.05 -5 -5 0 0.26 0.13 5 5 0 0.21 0.06 -5 5 0 0.27 0.08 -5 5 0 0.31 0.12 5 5 0 0.28 0.06 -7 -5 0 0.11 0.15 -7 -5 0 0.08 0.06 -7 5 0 0.14 0.11 -7 5 0 0.24 0.12 7 5 0 0.08 0.06 -7 5 0 0.08 0.07 -9 -5 0 21.96 0.76 -9 -5 0 24.39 0.83 -9 -5 0 23.36 1.03 -9 5 0 22.54 0.78 9 5 0 23.16 0.75 -9 5 0 22.32 0.88 -9 5 0 24.23 0.96 -11 -5 0 2.77 0.48 11 -5 0 2.14 0.15 -11 5 0 2.59 0.33 -11 5 0 2.87 0.40 -13 -5 0 28.91 1.37 -13 5 0 28.90 1.25 -13 5 0 29.53 1.20 -15 -5 0 2.40 0.52 -15 5 0 1.83 0.36 -15 5 0 1.99 0.43 -17 -5 0 3.05 0.61 -17 5 0 4.98 0.61 -17 5 0 3.08 0.51 -19 -5 0 0.00 0.40 -19 5 0 0.15 0.29 -19 5 0 -0.44 0.30 0 -6 0 9.35 0.43 0 6 0 9.35 0.39 0 6 0 8.96 0.38 2 -6 0 350.08 18.38 -2 6 0 387.27 18.89 4 -6 0 309.58 17.07 -4 -6 0 257.93 14.74 4 6 0 293.31 15.31 -4 6 0 248.16 15.62 6 -6 0 108.54 10.06 -6 -6 0 95.74 8.68 6 6 0 97.97 8.56 -6 6 0 102.93 10.87 -8 -6 0 36.38 1.43 -8 -6 0 37.93 1.20 -8 6 0 36.23 1.35 8 6 0 37.38 1.18 -8 6 0 37.90 1.21 -8 6 0 36.67 1.27 -10 -6 0 90.15 3.12 -10 -6 0 90.52 2.74 -10 6 0 88.57 2.81 -10 6 0 87.63 2.69 -12 -6 0 35.85 1.54 -12 6 0 34.30 1.32 -12 6 0 35.87 1.43 -14 -6 0 7.60 0.71 -14 6 0 7.75 0.62 -14 6 0 6.90 0.52 -16 -6 0 6.25 0.80 -16 6 0 5.51 0.53 -16 6 0 6.52 0.70 -18 -6 0 2.49 0.62 -18 6 0 3.65 0.54 -18 6 0 3.52 0.57 -20 -6 0 1.26 0.53 -1 -7 0 108.70 8.97 1 -7 0 110.35 9.68 -1 -7 0 130.63 10.13 -1 7 0 117.83 9.66 -3 -7 0 2.52 0.13 -3 -7 0 3.12 0.34 -3 7 0 2.22 0.19 3 7 0 2.20 0.18 -3 7 0 2.67 0.26 -5 -7 0 0.16 0.05 -5 -7 0 0.19 0.16 5 7 0 0.20 0.09 -5 7 0 0.09 0.11 -5 7 0 0.03 0.08 5 7 0 0.10 0.05 -7 -7 0 11.05 0.42 -7 -7 0 10.97 0.64 -7 7 0 11.56 0.51 -7 7 0 10.84 0.48 -7 7 0 11.52 0.58 -9 -7 0 32.58 1.24 -9 -7 0 31.20 1.31 -9 7 0 30.59 1.22 9 7 0 30.61 1.03 -9 7 0 30.33 1.06 -9 7 0 31.19 1.12 -11 -7 0 1.56 0.39 -11 7 0 1.09 0.28 -11 7 0 0.96 0.15 11 7 0 0.76 0.13 -11 7 0 1.16 0.24 -13 -7 0 1.86 0.47 -13 7 0 2.26 0.34 -13 7 0 0.84 0.29 -15 -7 0 5.83 1.19 -15 7 0 6.14 0.51 -15 7 0 5.97 0.66 -17 -7 0 3.24 0.68 -17 7 0 1.97 0.46 -17 7 0 3.92 0.52 -19 -7 0 0.11 0.42 -19 7 0 0.60 0.38 0 -8 0 26.15 0.99 0 8 0 26.85 0.94 0 8 0 26.20 0.93 -2 -8 0 39.14 1.36 -2 -8 0 37.37 1.16 -2 8 0 36.20 1.27 -2 8 0 37.96 1.25 2 8 0 36.15 1.23 -4 -8 0 17.28 0.79 -4 -8 0 17.16 0.57 -4 8 0 16.74 0.72 -4 8 0 18.27 0.68 4 8 0 17.44 0.66 -6 -8 0 19.27 0.91 -6 -8 0 19.45 0.64 6 8 0 18.44 0.71 6 8 0 19.53 0.65 -6 8 0 20.75 0.75 -6 8 0 19.48 0.83 -8 -8 0 68.67 2.39 -8 -8 0 67.89 2.06 -8 8 0 67.42 2.28 8 8 0 67.01 2.10 -8 8 0 67.27 2.14 -10 -8 0 0.24 0.28 -10 -8 0 0.82 0.14 10 8 0 0.85 0.14 -10 8 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-6 23 0.42 0.27 -6 6 23 1.06 0.27 -6 6 23 0.49 0.32 -4 -6 23 -0.08 0.21 -4 6 23 -0.01 0.27 -4 6 23 -0.10 0.15 -2 -6 23 0.33 0.27 -2 6 23 0.21 0.32 -2 6 23 0.47 0.19 0 -6 23 2.65 0.43 0 6 23 2.50 0.48 2 -6 23 3.45 0.52 2 6 23 3.81 0.58 -11 -7 23 1.51 0.47 -9 -7 23 6.09 0.72 -9 7 23 7.79 0.61 -7 -7 23 3.95 0.50 -7 7 23 4.81 0.50 -7 7 23 3.61 0.57 -5 -7 23 0.04 0.23 -5 7 23 0.04 0.17 -5 7 23 0.33 0.31 -3 -7 23 4.19 0.52 -3 7 23 4.07 0.60 -1 -7 23 6.79 0.67 -1 7 23 6.99 0.75 1 -7 23 3.81 0.53 1 7 23 4.36 0.59 -10 -8 23 0.30 0.35 -10 8 23 0.45 0.28 -6 8 23 2.55 0.36 -6 8 23 2.83 0.52 -4 -8 23 0.10 0.26 -4 8 23 0.56 0.33 -2 -8 23 4.61 0.56 -2 8 23 4.20 0.58 0 -8 23 1.55 0.36 0 8 23 0.77 0.40 -9 9 23 7.89 0.62 -7 9 23 -0.06 0.19 -10 0 24 6.26 0.76 -10 0 24 6.60 0.76 -8 0 24 1.97 0.54 -8 0 24 2.15 0.50 -8 0 24 2.62 0.43 -6 0 24 2.43 0.60 -6 0 24 2.95 0.56 -6 0 24 3.18 0.55 -4 0 24 17.02 1.09 -4 0 24 14.16 0.94 -4 0 24 15.46 0.84 -2 0 24 0.36 0.33 -2 0 24 1.22 0.40 -2 0 24 0.96 0.29 0 0 24 -0.08 0.20 0 0 24 0.40 0.32 2 0 24 3.80 0.62 2 0 24 3.44 0.43 -9 -1 24 1.13 0.65 -9 -1 24 2.32 0.47 -9 -1 24 1.55 0.40 -9 1 24 1.94 0.39 -9 1 24 1.75 0.43 -9 1 24 0.91 0.42 -7 -1 24 1.63 0.36 -7 -1 24 1.45 0.44 -7 -1 24 2.12 0.50 -7 1 24 1.47 0.44 -7 1 24 1.96 0.46 -7 1 24 2.06 0.36 -5 -1 24 0.22 0.32 -5 -1 24 0.67 0.36 -5 1 24 0.43 0.35 -5 1 24 0.30 0.24 -5 1 24 0.14 0.33 -3 -1 24 0.09 0.34 -3 -1 24 0.52 0.26 -3 -1 24 -0.10 0.28 -3 1 24 0.27 0.23 -3 1 24 0.14 0.27 -3 1 24 0.59 0.35 -1 -1 24 -0.01 0.21 -1 -1 24 0.11 0.31 -1 1 24 0.28 0.34 -1 1 24 -0.08 0.18 1 -1 24 -0.16 0.26 1 -1 24 0.01 0.21 1 1 24 0.08 0.32 1 1 24 0.00 0.21 3 -1 24 2.04 0.69 3 -1 24 1.01 0.44 3 1 24 1.49 0.61 3 1 24 1.31 0.30 5 -1 24 0.12 0.23 -10 -2 24 0.96 0.40 -10 2 24 0.97 0.45 -8 -2 24 -0.06 0.22 -8 -2 24 -0.42 0.26 -8 -2 24 0.05 0.31 -8 2 24 -0.40 0.26 -8 2 24 0.14 0.23 -8 2 24 -0.06 0.35 -6 -2 24 0.87 0.38 -6 -2 24 0.45 0.33 -6 -2 24 0.73 0.28 -6 2 24 1.06 0.43 -6 2 24 0.69 0.36 -6 2 24 1.03 0.42 -4 -2 24 6.86 0.94 -4 -2 24 7.56 0.84 -4 -2 24 7.83 0.66 -4 2 24 7.47 0.83 -4 2 24 6.71 0.54 -4 2 24 8.11 0.85 -2 -2 24 0.04 0.33 -2 -2 24 0.23 0.35 -2 2 24 0.47 0.35 -2 2 24 0.27 0.22 0 -2 24 0.73 0.37 0 -2 24 1.19 0.53 0 2 24 -0.06 0.27 0 2 24 0.56 0.23 2 -2 24 3.89 0.64 2 -2 24 3.79 0.48 2 2 24 3.67 0.41 2 2 24 3.66 0.60 4 -2 24 2.28 0.39 -9 -3 24 1.64 0.43 -9 3 24 0.24 0.39 -9 3 24 0.45 0.27 -9 3 24 1.05 0.43 -7 -3 24 3.60 0.49 -7 -3 24 2.69 0.53 -7 -3 24 3.01 0.52 -7 3 24 3.15 0.49 -7 3 24 2.56 0.51 -5 -3 24 4.11 0.50 -5 -3 24 3.43 0.53 -5 3 24 3.17 0.59 -5 3 24 3.88 0.46 -5 3 24 3.07 0.56 -3 -3 24 2.24 0.40 -3 3 24 2.27 0.35 -3 3 24 2.19 0.47 -1 -3 24 2.03 0.45 -1 3 24 2.14 0.49 -1 3 24 2.82 0.37 1 -3 24 1.12 0.33 1 3 24 1.49 0.43 1 3 24 1.50 0.29 3 -3 24 4.16 0.52 -10 -4 24 1.19 0.44 -8 -4 24 0.29 0.32 -8 4 24 0.05 0.31 -8 4 24 0.07 0.21 -8 4 24 0.12 0.38 -6 -4 24 1.27 0.37 -6 -4 24 1.33 0.36 -6 4 24 0.93 0.29 -6 4 24 1.53 0.42 -4 -4 24 -0.21 0.19 -4 4 24 0.25 0.32 -4 4 24 0.16 0.20 -2 -4 24 5.08 0.58 -2 4 24 4.08 0.62 -2 4 24 3.52 0.41 0 -4 24 1.25 0.34 0 4 24 0.80 0.28 0 4 24 1.11 0.37 2 -4 24 0.07 0.24 -9 5 24 2.64 0.41 -7 -5 24 0.91 0.37 -7 5 24 1.22 0.59 -7 5 24 0.22 0.39 -7 5 24 0.91 0.33 -5 -5 24 2.56 0.41 -5 5 24 2.87 0.39 -5 5 24 2.32 0.49 -3 -5 24 0.16 0.29 -3 5 24 0.10 0.30 -3 5 24 0.28 0.20 -1 -5 24 0.14 0.26 -1 5 24 -0.02 0.25 1 -5 24 4.40 0.56 -10 -6 24 0.48 0.33 -8 6 24 1.44 0.32 -6 6 24 6.84 0.54 -4 -6 24 1.83 0.38 -4 6 24 1.39 0.69 -4 6 24 1.66 0.30 -2 -6 24 2.03 0.40 0 -6 24 3.83 0.71 -7 7 24 0.87 0.27 -5 7 24 0.36 0.20 -8 8 24 4.73 0.50 -8 0 25 0.18 0.34 -6 0 25 -0.06 0.31 -6 0 25 -0.23 0.20 -4 0 25 -0.09 0.23 -4 0 25 0.04 0.30 -2 0 25 -0.05 0.21 0 0 25 -0.14 0.19 2 0 25 0.00 0.22 -9 -1 25 0.17 0.35 -7 1 25 1.65 0.34 -7 1 25 1.08 0.43 -5 -1 25 4.39 0.62 -5 -1 25 4.46 0.52 -5 1 25 4.46 0.50 -5 1 25 3.96 0.61 -3 -1 25 5.11 0.55 -3 1 25 4.54 0.51 -3 1 25 4.22 0.62 -1 -1 25 2.52 0.41 -1 1 25 2.43 0.43 1 -1 25 0.12 0.24 1 1 25 0.44 0.23 3 -1 25 1.47 0.37 -8 -2 25 0.40 0.34 -8 2 25 -0.06 0.33 -6 -2 25 1.28 0.42 -6 2 25 0.69 0.28 -6 2 25 0.62 0.41 -4 -2 25 1.17 0.31 -4 2 25 0.13 0.36 -4 2 25 0.74 0.27 -2 -2 25 3.78 0.50 -2 2 25 3.84 0.61 0 -2 25 0.10 0.24 2 -2 25 1.16 0.41 -9 -3 25 0.44 0.32 -7 -3 25 0.55 0.36 -7 3 25 0.41 0.24 -7 3 25 0.31 0.37 -5 3 25 0.99 0.28 -5 3 25 0.91 0.44 -3 -3 25 -0.24 0.22 -1 -3 25 0.46 0.27 -1 3 25 0.37 0.22 -8 -4 25 0.07 0.28 -6 4 25 0.30 0.22 -6 4 25 0.99 0.45 -2 4 25 0.73 0.24 -9 -5 25 0.89 0.41 -7 5 25 0.55 0.24 -5 5 25 0.81 0.26 -3 5 25 2.84 0.43 -6 6 25 0.56 0.22 -7 7 25 0.83 0.36 -6 0 26 5.37 0.71 -7 -1 26 2.12 0.51 -5 1 26 1.25 0.45 -1 1 26 2.05 0.41 -4 2 26 1.12 0.44 -2 2 26 0.35 0.21 -3 3 26 1.16 0.44 -3 3 26 1.53 0.30 -4 4 26 0.65 0.22 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 39176 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, 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 0.500000 0.82594(2) 0.750000 0.02088(5) Uani 1 2 d S T P . . O1 O 0.35753(9) 0.75407(8) 1.06327(6) 0.0404(2) Uani 1 1 d . . . . . O2 O 0.32833(9) 0.89773(7) 1.01830(7) 0.0441(2) Uani 1 1 d . . . . . O3 O 0.13864(8) 0.77558(7) 0.56894(7) 0.0433(2) Uani 1 1 d . . . . . O4 O 0.13122(10) 0.92945(9) 0.55803(12) 0.0755(5) Uani 1 1 d . . . . . N1 N 0.500000 0.69028(8) 0.750000 0.0241(2) Uani 1 2 d S T P . . N2 N 0.500000 0.96527(8) 0.750000 0.0220(2) Uani 1 2 d S T P . . N3 N 0.33853(7) 0.79589(6) 0.68159(5) 0.02399(15) Uani 1 1 d . . . . . N4 N 0.40722(7) 0.86428(6) 0.86266(5) 0.02327(15) Uani 1 1 d . . . . . C1 C 0.57533(9) 0.64388(7) 0.80148(7) 0.02786(19) Uani 1 1 d . . . . . C2 C 0.57641(12) 0.54723(8) 0.80354(11) 0.0424(3) Uani 1 1 d . . . . . H2 H 0.627611 0.515258 0.840254 0.051 Uiso 1 1 calc R U . . . C3 C 0.500000 0.49937(12) 0.750000 0.0506(5) Uani 1 2 d S T P . . H3 H 0.500001 0.434440 0.750000 0.061 Uiso 1 2 calc R U P . . C4 C 0.47175(8) 1.01296(7) 0.81577(6) 0.02475(17) Uani 1 1 d . . . . . C5 C 0.46850(10) 1.10966(7) 0.81646(8) 0.0335(2) Uani 1 1 d . . . . . H5 H 0.445553 1.141387 0.860821 0.040 Uiso 1 1 calc R U . . . C6 C 0.500000 1.15822(11) 0.750000 0.0378(4) Uani 1 2 d S T P . . H6 H 0.499999 1.223156 0.749999 0.045 Uiso 1 2 calc R U P . . C7 C 0.44734(9) 0.95704(7) 0.89003(6) 0.02753(19) Uani 1 1 d . . . . . H7A H 0.509981 0.950364 0.932182 0.033 Uiso 1 1 calc R U . . . H7B H 0.395907 0.990002 0.916400 0.033 Uiso 1 1 calc R U . . . C8 C 0.41693(9) 0.79646(8) 0.93253(6) 0.02753(18) Uani 1 1 d . . . . . H8A H 0.490496 0.787622 0.954216 0.033 Uiso 1 1 calc R U . . . H8B H 0.389665 0.737138 0.909287 0.033 Uiso 1 1 calc R U . . . C9 C 0.36234(10) 0.82099(8) 1.00767(7) 0.0309(2) Uani 1 1 d . . . . . C10 C 0.34533(9) 0.70225(8) 0.64336(7) 0.0304(2) Uani 1 1 d . . . . . H10A H 0.364421 0.708604 0.587285 0.037 Uiso 1 1 calc R U . . . H10B H 0.277866 0.671822 0.636887 0.037 Uiso 1 1 calc R U . . . C11 C 0.29435(9) 0.86502(8) 0.61606(7) 0.0294(2) Uani 1 1 d . . . . . H11A H 0.333838 0.861812 0.569574 0.035 Uiso 1 1 calc R U . . . H11B H 0.304709 0.926879 0.640844 0.035 Uiso 1 1 calc R U . . . C12 C 0.17781(10) 0.85387(9) 0.57864(8) 0.0337(2) Uani 1 1 d . . . . . C13 C 0.29935(8) 0.87041(7) 0.81490(6) 0.02588(18) Uani 1 1 d . . . . . H13A H 0.290333 0.929380 0.784584 0.031 Uiso 1 1 calc R U . . . H13B H 0.250437 0.868655 0.854647 0.031 Uiso 1 1 calc R U . . . C14 C 0.27609(8) 0.79067(8) 0.75183(7) 0.02682(18) Uani 1 1 d . . . . . H14A H 0.290624 0.731933 0.781792 0.032 Uiso 1 1 calc R U . . . H14B H 0.202556 0.791638 0.727615 0.032 Uiso 1 1 calc R U . . . O6 O 0.27467(13) 0.58320(9) 0.83470(9) 0.0632(4) Uani 1 1 d . . . . . H6A H 0.239(2) 0.6004(17) 0.8749(17) 0.074(7) Uiso 1 1 d . . . . . H6B H 0.3165(19) 0.5415(18) 0.8713(16) 0.073(7) Uiso 1 1 d . . . . . O5 O 0.42643(11) 0.59674(10) 1.03426(12) 0.0610(4) Uani 1 1 d . . . . . H5A H 0.495(2) 0.5917(16) 1.0422(15) 0.068(7) Uiso 1 1 d . . . . . H5B H 0.407(3) 0.575(2) 0.998(2) 0.106(13) Uiso 1 1 d . . . . . H1 H 0.3865(19) 0.7028(17) 1.0498(15) 0.063(6) Uiso 1 1 d . . . . . 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 0.02172(9) 0.01844(8) 0.02188(8) 0.000 0.00187(5) 0.000 O1 0.0463(5) 0.0460(5) 0.0307(4) 0.0073(4) 0.0111(4) -0.0025(4) O2 0.0564(6) 0.0421(5) 0.0388(5) -0.0016(4) 0.0221(4) 0.0060(4) O3 0.0365(5) 0.0410(5) 0.0466(5) 0.0017(4) -0.0099(4) -0.0090(4) O4 0.0388(6) 0.0430(6) 0.1309(13) 0.0176(7) -0.0259(7) -0.0003(5) N1 0.0252(5) 0.0199(4) 0.0271(5) 0.000 0.0042(4) 0.000 N2 0.0234(5) 0.0192(4) 0.0234(5) 0.000 0.0037(4) 0.000 N3 0.0251(4) 0.0235(3) 0.0224(3) -0.0009(3) 0.0012(3) -0.0022(3) N4 0.0251(4) 0.0230(3) 0.0214(3) -0.0008(3) 0.0031(3) 0.0003(3) C1 0.0285(5) 0.0231(4) 0.0331(5) 0.0051(4) 0.0083(4) 0.0036(4) C2 0.0426(7) 0.0239(5) 0.0624(8) 0.0113(5) 0.0135(6) 0.0072(4) C3 0.0526(12) 0.0181(6) 0.0830(16) 0.000 0.0171(11) 0.000 C4 0.0253(4) 0.0213(4) 0.0272(4) -0.0040(3) 0.0030(3) 0.0001(3) C5 0.0377(6) 0.0222(4) 0.0398(6) -0.0069(4) 0.0040(4) 0.0013(4) C6 0.0427(9) 0.0183(6) 0.0512(10) 0.000 0.0042(8) 0.000 C7 0.0327(5) 0.0264(4) 0.0241(4) -0.0062(3) 0.0062(3) -0.0014(4) C8 0.0306(5) 0.0289(4) 0.0233(4) 0.0025(3) 0.0053(3) 0.0037(4) C9 0.0317(5) 0.0374(5) 0.0239(4) 0.0002(4) 0.0054(4) -0.0027(4) C10 0.0325(5) 0.0280(4) 0.0290(5) -0.0082(4) 0.0000(4) -0.0058(4) C11 0.0276(5) 0.0314(5) 0.0272(4) 0.0056(4) -0.0009(3) -0.0029(4) C12 0.0290(5) 0.0380(5) 0.0313(5) 0.0031(4) -0.0036(4) -0.0026(4) C13 0.0240(4) 0.0281(4) 0.0255(4) 0.0003(3) 0.0038(3) 0.0032(3) C14 0.0257(4) 0.0290(4) 0.0255(4) 0.0005(3) 0.0031(3) -0.0052(4) O6 0.0848(10) 0.0483(6) 0.0664(8) 0.0145(6) 0.0415(8) 0.0128(6) O5 0.0412(7) 0.0419(6) 0.0933(11) -0.0001(6) -0.0080(7) 0.0004(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' 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' Cu Cu 0.3201 1.2651 '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 0.00 0.00 -1.00 0.2230 0.00 0.00 1.00 0.2670 -1.00 -1.00 0.00 0.2000 1.00 1.00 0.00 0.1530 -1.00 -1.00 -1.00 0.2620 0.00 1.00 0.00 0.1110 0.00 -1.00 0.00 0.1530 -1.00 1.00 -1.00 0.2900 0.00 1.00 1.00 0.2050 -1.00 1.00 1.00 0.1210 1.00 -1.00 -1.00 0.0750 -1.00 0.00 -1.00 0.3110 1.00 0.00 1.00 0.3390 -1.00 0.00 1.00 0.1300 1.00 0.00 -1.00 0.1180 -1.00 -1.00 1.00 0.1160 1.00 1.00 -1.00 0.1230 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N2 180.0 . . ? N1 Cu1 N3 78.93(2) . 2_656 ? N1 Cu1 N3 78.93(2) . . ? N1 Cu1 N4 103.30(2) . 2_656 ? N1 Cu1 N4 103.30(2) . . ? N2 Cu1 N3 101.07(2) . 2_656 ? N2 Cu1 N3 101.07(2) . . ? N2 Cu1 N4 76.70(2) . . ? N2 Cu1 N4 76.70(2) . 2_656 ? N3 Cu1 N3 157.85(5) 2_656 . ? N3 Cu1 N4 103.30(4) . 2_656 ? N3 Cu1 N4 81.86(4) . . ? N3 Cu1 N4 103.30(4) 2_656 . ? N3 Cu1 N4 81.86(4) 2_656 2_656 ? N4 Cu1 N4 153.41(4) . 2_656 ? C9 O1 H1 112.3(15) . . ? C1 N1 Cu1 119.65(7) 2_656 . ? C1 N1 Cu1 119.65(7) . . ? C1 N1 C1 120.71(13) . 2_656 ? C4 N2 Cu1 120.36(6) . . ? C4 N2 Cu1 120.36(6) 2_656 . ? C4 N2 C4 119.29(12) . 2_656 ? C10 N3 Cu1 104.95(7) . . ? C10 N3 C11 110.99(9) . . ? C10 N3 C14 109.90(8) . . ? C11 N3 Cu1 115.81(7) . . ? C11 N3 C14 111.44(9) . . ? C14 N3 Cu1 103.28(7) . . ? C7 N4 Cu1 103.41(6) . . ? C7 N4 C13 110.98(8) . . ? C8 N4 Cu1 115.30(7) . . ? C8 N4 C7 113.16(9) . . ? C8 N4 C13 112.48(8) . . ? C13 N4 Cu1 100.53(6) . . ? N1 C1 C2 120.83(12) . . ? N1 C1 C10 116.33(10) . 2_656 ? C2 C1 C10 122.83(11) . 2_656 ? C1 C2 H2 120.7 . . ? C3 C2 C1 118.61(13) . . ? C3 C2 H2 120.7 . . ? C2 C3 C2 120.39(16) 2_656 . ? C2 C3 H3 119.8 2_656 . ? C2 C3 H3 119.8 . . ? N2 C4 C5 121.59(10) . . ? N2 C4 C7 117.39(9) . . ? C5 C4 C7 120.99(9) . . ? C4 C5 H5 120.6 . . ? C6 C5 C4 118.87(11) . . ? C6 C5 H5 120.6 . . ? C5 C6 C5 119.67(15) . 2_656 ? C5 C6 H6 120.2 . . ? C5 C6 H6 120.2 2_656 . ? N4 C7 C4 111.10(8) . . ? N4 C7 H7A 109.4 . . ? N4 C7 H7B 109.4 . . ? C4 C7 H7A 109.4 . . ? C4 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? N4 C8 H8A 108.1 . . ? N4 C8 H8B 108.1 . . ? N4 C8 C9 116.65(9) . . ? H8A C8 H8B 107.3 . . ? C9 C8 H8A 108.1 . . ? C9 C8 H8B 108.1 . . ? O1 C9 C8 116.10(11) . . ? O2 C9 O1 120.67(11) . . ? O2 C9 C8 123.19(10) . . ? N3 C10 C1 110.36(9) . 2_656 ? N3 C10 H10A 109.6 . . ? N3 C10 H10B 109.6 . . ? C1 C10 H10A 109.6 2_656 . ? C1 C10 H10B 109.6 2_656 . ? H10A C10 H10B 108.1 . . ? N3 C11 H11A 108.2 . . ? N3 C11 H11B 108.2 . . ? N3 C11 C12 116.30(9) . . ? H11A C11 H11B 107.4 . . ? C12 C11 H11A 108.2 . . ? C12 C11 H11B 108.2 . . ? O3 C12 O4 125.47(13) . . ? O3 C12 C11 120.18(12) . . ? O4 C12 C11 114.31(12) . . ? N4 C13 H13A 109.4 . . ? N4 C13 H13B 109.4 . . ? N4 C13 C14 111.20(8) . . ? H13A C13 H13B 108.0 . . ? C14 C13 H13A 109.4 . . ? C14 C13 H13B 109.4 . . ? N3 C14 C13 112.66(8) . . ? N3 C14 H14A 109.1 . . ? N3 C14 H14B 109.1 . . ? C13 C14 H14A 109.1 . . ? C13 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? H6A O6 H6B 93(2) . . ? H5A O5 H5B 108(3) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.9430(14) . ? Cu1 N2 1.9955(13) . ? Cu1 N3 2.2406(12) . ? Cu1 N3 2.2406(12) 2_656 ? Cu1 N4 2.3874(11) . ? Cu1 N4 2.3874(11) 2_656 ? O1 C9 1.3131(15) . ? O1 H1 0.87(2) . ? O2 C9 1.2073(16) . ? O3 C12 1.2307(17) . ? O4 C12 1.2572(18) . ? N1 C1 1.3437(13) 2_656 ? N1 C1 1.3437(13) . ? N2 C4 1.3516(12) . ? N2 C4 1.3517(12) 2_656 ? N3 C10 1.4816(14) . ? N3 C11 1.4828(14) . ? N3 C14 1.4899(14) . ? N4 C7 1.4668(14) . ? N4 C8 1.4662(14) . ? N4 C13 1.4828(15) . ? C1 C2 1.3846(17) . ? C1 C10 1.4942(17) 2_656 ? C2 H2 0.9300 . ? C2 C3 1.3789(19) . ? C3 H3 0.9300 . ? C4 C5 1.3857(15) . ? C4 C7 1.5051(15) . ? C5 H5 0.9300 . ? C5 C6 1.3843(15) . ? C6 H6 0.9300 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 C9 1.5307(16) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 C12 1.5420(17) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 C14 1.5173(15) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? O6 H6A 0.89(3) . ? O6 H6B 0.94(3) . ? O5 H5A 0.89(3) . ? O5 H5B 0.67(3) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu1 N1 C1 C2 179.17(9) . . . . ? Cu1 N1 C1 C10 0.53(11) . . . 2_656 ? Cu1 N2 C4 C5 -178.35(8) . . . . ? Cu1 N2 C4 C7 3.70(11) . . . . ? Cu1 N3 C10 C1 32.08(10) . . . 2_656 ? Cu1 N3 C11 C12 -170.68(8) . . . . ? Cu1 N3 C14 C13 46.19(9) . . . . ? Cu1 N4 C7 C4 34.18(10) . . . . ? Cu1 N4 C8 C9 177.39(8) . . . . ? Cu1 N4 C13 C14 43.38(8) . . . . ? N1 C1 C2 C3 1.63(17) . . . . ? N2 C4 C5 C6 -3.25(16) . . . . ? N2 C4 C7 N4 -29.06(13) . . . . ? N3 C11 C12 O3 -34.43(17) . . . . ? N3 C11 C12 O4 147.56(14) . . . . ? N4 C8 C9 O1 169.72(10) . . . . ? N4 C8 C9 O2 -12.84(18) . . . . ? N4 C13 C14 N3 -66.74(11) . . . . ? C1 N1 C1 C2 -0.83(9) 2_656 . . . ? C1 N1 C1 C10 -179.48(11) 2_656 . . 2_656 ? C1 C2 C3 C2 -0.79(8) . . . 2_656 ? C4 N2 C4 C5 1.65(8) 2_656 . . . ? C4 N2 C4 C7 -176.30(11) 2_656 . . . ? C4 C5 C6 C5 1.56(8) . . . 2_656 ? C5 C4 C7 N4 152.98(10) . . . . ? C7 N4 C8 C9 58.63(13) . . . . ? C7 N4 C13 C14 152.28(8) . . . . ? C7 C4 C5 C6 174.63(9) . . . . ? C8 N4 C7 C4 159.61(9) . . . . ? C8 N4 C13 C14 -79.80(10) . . . . ? C10 N3 C11 C12 69.81(13) . . . . ? C10 N3 C14 C13 157.74(9) . . . . ? C10 C1 C2 C3 -179.82(10) 2_656 . . . ? C11 N3 C10 C1 157.89(9) . . . 2_656 ? C11 N3 C14 C13 -78.79(11) . . . . ? C13 N4 C7 C4 -72.83(11) . . . . ? C13 N4 C8 C9 -68.13(12) . . . . ? C14 N3 C10 C1 -78.38(11) . . . 2_656 ? C14 N3 C11 C12 -53.03(13) . . . . ?