#------------------------------------------------------------------------------ #$Date: 2019-12-04 09:38:15 +0200 (Wed, 04 Dec 2019) $ #$Revision: 244894 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/64/1556422.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_1556422 loop_ _publ_author_name 'Rancan, M.' 'Carlotto, A.' 'Bottaro, G.' 'Armelao, L.' _publ_section_title ; Effect of Coordinating Solvents on the Structure of Cu(II)-4,4'-bipyridine Coordination Polymers ; _journal_name_full Inorganics _journal_page_first 103 _journal_paper_doi 10.3390/inorganics7080103 _journal_volume 7 _journal_year 2019 _chemical_formula_moiety '0.5(C40 H40 Cu2 N8 O4), 2(Cl O4), 2(C4 H9 N O)' _chemical_formula_sum 'C28 H38 Cl2 Cu N6 O12' _chemical_formula_weight 785.08 _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 dual _cell_angle_alpha 90 _cell_angle_beta 91.562(7) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.4924(10) _cell_length_b 11.1385(7) _cell_length_c 22.2237(13) _cell_measurement_reflns_used 3458 _cell_measurement_temperature 301(2) _cell_measurement_theta_max 26.6340 _cell_measurement_theta_min 2.9730 _cell_volume 3586.1(4) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment air _diffrn_ambient_temperature 301(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.0637 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.935 _diffrn_measured_fraction_theta_max 0.832 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -25.00 30.00 0.2000 30.0000 omega____ theta____ kappa____ phi______ frames - -12.3052 -99.0000 60.0000 275 #__ type_ start__ end____ width___ exp.time_ 2 omega -58.00 42.00 0.2000 30.0000 omega____ theta____ kappa____ phi______ frames - 12.3052 -77.0000 90.0000 500 #__ type_ start__ end____ width___ exp.time_ 3 omega -58.00 42.00 0.2000 30.0000 omega____ theta____ kappa____ phi______ frames - 12.3052 -77.0000 0.0000 500 #__ type_ start__ end____ width___ exp.time_ 4 omega 32.00 59.00 0.2000 30.0000 omega____ theta____ kappa____ phi______ frames - 12.3052 -179.0000 -60.0000 135 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0418026000 _diffrn_orient_matrix_UB_12 -0.0058627000 _diffrn_orient_matrix_UB_13 -0.0171315000 _diffrn_orient_matrix_UB_21 -0.0249338000 _diffrn_orient_matrix_UB_22 -0.0033946000 _diffrn_orient_matrix_UB_23 0.0269393000 _diffrn_orient_matrix_UB_31 -0.0052010000 _diffrn_orient_matrix_UB_32 0.0633398000 _diffrn_orient_matrix_UB_33 -0.0001232000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_unetI/netI 0.0365 _diffrn_reflns_Laue_measured_fraction_full 0.935 _diffrn_reflns_Laue_measured_fraction_max 0.832 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 4544 _diffrn_reflns_point_group_measured_fraction_full 0.935 _diffrn_reflns_point_group_measured_fraction_max 0.832 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.650 _diffrn_reflns_theta_min 2.306 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.824 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.82081 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'light blue' _exptl_crystal_density_diffrn 1.454 _exptl_crystal_description block _exptl_crystal_F_000 1628 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.601 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.087 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 231 _refine_ls_number_reflns 4544 _refine_ls_number_restraints 26 _refine_ls_restrained_S_all 1.128 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0576 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1246P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1686 _refine_ls_wR_factor_ref 0.1804 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3771 _reflns_number_total 4544 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file 3.cif _cod_data_source_block 3 _cod_database_code 1556422 _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. ; _diffrn_oxdiff_twin_integration_method simultaneous _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.611(2) 0.389(2) 2. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H,H) groups 3. Rigid body (RIGU) restrains O5, Cl1, O3, O6, O4 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002 4.a Free rotating group: O1(H1A,H1B) 4.b Aromatic/amide H refined with riding coordinates: C10(H10), C1(H1), C5(H5), C2(H2), C4(H4), C11(H11), C7(H7), C6(H6) 4.c Idealised Me refined as rotating group: C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C14(H14A,H14B,H14C) ; _shelx_res_file ; TITL exp_992_twin1_hklf4_a.res in C2/c 3.res created by SHELXL-2018/3 at 16:10:35 on 19-Jul-2019 REM Old TITL exp_992_twin1_hklf4 in C2/c #15 REM SHELXT solution in C2/c REM R1 0.246, Rweak 0.036, Alpha 0.069, Orientation as input REM Formula found by SHELXT: C35 N4 O7 Cl2 Cu CELL 0.71073 14.4924 11.1385 22.2237 90 91.562 90 ZERR 4 0.001 0.0007 0.0013 0 0.007 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Cl Cu N O UNIT 112 152 8 4 24 48 RIGU 0.002 0.002 O5 Cl1 O3 O6 O4 L.S. 50 PLAN 20 BIND Cu1 O1 BOND $H LIST 4 MORE -1 CONF fmap 2 ACTA OMIT -1 1 -14 REM REM REM WGHT 0.124600 BASF 0.38862 FVAR 1.69697 CU1 4 0.500000 -0.014413 0.250000 10.50000 0.05248 0.01247 = 0.01599 0.00000 0.00046 0.00000 CL1 3 0.811710 -0.120245 0.106737 11.00000 0.06481 0.06521 = 0.06556 -0.02051 0.00124 0.00972 N2 5 0.500000 0.168374 0.250000 10.50000 0.04377 0.01915 = 0.02416 0.00000 0.00801 0.00000 N3 5 0.500000 0.801829 0.250000 10.50000 0.03967 0.01449 = 0.02506 0.00000 -0.00560 0.00000 N1 5 0.495399 -0.013764 0.158765 11.00000 0.04294 0.01988 = 0.01484 -0.00140 0.00208 0.00077 AFIX 6 O1 6 0.671260 -0.014716 0.250208 11.00000 0.05155 0.04262 = 0.04486 -0.00774 0.00243 0.00620 H1A 2 0.712270 -0.022507 0.278007 11.00000 -1.50000 H1B 2 0.688996 -0.049745 0.218579 11.00000 -1.50000 AFIX 0 C9 1 0.500000 0.551218 0.250000 10.50000 0.04313 0.01878 = 0.03623 0.00000 0.00158 0.00000 C8 1 0.500000 0.419277 0.250000 10.50000 0.04354 0.01858 = 0.03063 0.00000 -0.00549 0.00000 C10 1 0.569935 0.617103 0.278112 11.00000 0.04935 0.02025 = 0.05901 0.00212 -0.01425 0.00647 AFIX 43 H10 2 0.618779 0.577499 0.297511 11.00000 -1.20000 AFIX 0 C1 1 0.438369 0.058148 0.127433 11.00000 0.04612 0.02812 = 0.02243 0.00527 0.00826 0.01327 AFIX 43 H1 2 0.397301 0.105825 0.148231 11.00000 -1.20000 AFIX 0 C3 1 0.498918 -0.004321 0.033359 11.00000 0.02954 0.02620 = 0.02211 -0.00270 -0.00303 -0.00367 C5 1 0.551762 -0.082793 0.127659 11.00000 0.04878 0.03476 = 0.03179 0.00034 -0.01049 0.01495 AFIX 43 H5 2 0.590858 -0.134958 0.148801 11.00000 -1.20000 AFIX 0 C2 1 0.437791 0.064642 0.066264 11.00000 0.04713 0.03712 = 0.02022 0.00892 0.00037 0.01308 AFIX 43 H2 2 0.396311 0.115461 0.046258 11.00000 -1.20000 AFIX 0 C4 1 0.555314 -0.081225 0.066665 11.00000 0.03923 0.04450 = 0.01795 -0.00363 -0.00171 0.01325 AFIX 43 H4 2 0.595782 -0.132002 0.047195 11.00000 -1.20000 AFIX 0 C11 1 0.567703 0.740487 0.277560 11.00000 0.04911 0.02395 = 0.04416 0.00254 -0.01226 -0.00670 AFIX 43 H11 2 0.615140 0.782559 0.297121 11.00000 -1.20000 AFIX 0 C7 1 0.577086 0.353701 0.235495 11.00000 0.04160 0.02248 = 0.04917 0.00701 0.00374 -0.00596 AFIX 43 H7 2 0.631480 0.393175 0.226336 11.00000 -1.20000 AFIX 0 O2 6 0.748415 -0.095827 0.355897 11.00000 0.07278 0.12581 = 0.05530 0.00527 -0.01036 0.02461 C6 1 0.573965 0.232550 0.234527 11.00000 0.04171 0.02149 = 0.04060 -0.00207 0.00775 0.00652 AFIX 43 H6 2 0.626075 0.191270 0.222444 11.00000 -1.20000 AFIX 0 O3 6 0.775004 -0.023057 0.135520 11.00000 0.10275 0.13262 = 0.19935 -0.07154 -0.04185 0.03313 N4 5 0.838055 -0.157937 0.431211 11.00000 0.06612 0.10742 = 0.07322 0.00150 -0.00916 0.01955 C12 1 0.808583 -0.074070 0.395496 11.00000 0.06372 0.10262 = 0.05188 0.00252 0.00739 0.02128 O5 6 0.907765 -0.129039 0.114486 11.00000 0.06510 0.20453 = 0.10923 -0.03622 0.01280 0.01078 C13 1 0.849043 0.045909 0.402550 11.00000 0.15701 0.10007 = 0.09109 0.00631 0.00755 -0.00071 AFIX 137 H13A 2 0.810725 0.103530 0.381669 11.00000 -1.50000 H13B 2 0.909595 0.046571 0.386082 11.00000 -1.50000 H13C 2 0.853302 0.066192 0.444517 11.00000 -1.50000 AFIX 0 C15 1 0.804901 -0.279053 0.420887 11.00000 0.15142 0.06920 = 0.10164 0.01095 -0.00183 -0.01033 AFIX 137 H15A 2 0.764089 -0.280108 0.386133 11.00000 -1.50000 H15B 2 0.772312 -0.306033 0.455405 11.00000 -1.50000 H15C 2 0.856324 -0.331300 0.414279 11.00000 -1.50000 AFIX 0 C14 1 0.909851 -0.140535 0.477583 11.00000 0.07271 0.14847 = 0.07378 0.01914 -0.01518 0.00545 AFIX 137 H14A 2 0.968271 -0.129628 0.458979 11.00000 -1.50000 H14B 2 0.912754 -0.209734 0.503317 11.00000 -1.50000 H14C 2 0.895823 -0.070781 0.501001 11.00000 -1.50000 AFIX 0 O6 6 0.779412 -0.144844 0.051786 11.00000 0.10315 0.46624 = 0.10967 -0.13305 0.00386 -0.04627 O4 6 0.772970 -0.205191 0.147856 11.00000 0.12112 0.20022 = 0.29125 0.11252 0.00496 -0.01158 HKLF 5 REM exp_992_twin1_hklf4_a.res in C2/c REM wR2 = 0.1804, GooF = S = 1.117, Restrained GooF = 1.128 for all data REM R1 = 0.0576 for 3771 Fo > 4sig(Fo) and 0.0686 for all 4544 data REM 231 parameters refined using 26 restraints END WGHT 0.1247 0.0000 REM Highest difference peak 0.601, deepest hole -0.396, 1-sigma level 0.087 Q1 1 0.8100 0.0057 0.0921 11.00000 0.05 0.60 Q2 1 0.8955 -0.0215 0.0966 11.00000 0.05 0.48 Q3 1 0.7700 -0.0494 0.0511 11.00000 0.05 0.48 Q4 1 0.8503 -0.0573 0.4269 11.00000 0.05 0.43 Q5 1 0.7735 -0.1877 0.0604 11.00000 0.05 0.42 Q6 1 0.7814 -0.2333 0.0977 11.00000 0.05 0.42 Q7 1 0.4987 -0.0211 0.1966 11.00000 0.05 0.41 Q8 1 0.7706 -0.0137 0.3537 11.00000 0.05 0.41 Q9 1 0.7789 -0.1276 0.1556 11.00000 0.05 0.39 Q10 1 0.5619 0.0060 0.2480 11.00000 0.05 0.39 Q11 1 0.8195 -0.1595 0.0593 11.00000 0.05 0.37 Q12 1 0.5541 0.1978 0.2452 11.00000 0.05 0.37 Q13 1 0.4687 -0.0075 0.0322 11.00000 0.05 0.36 Q14 1 0.5000 0.3875 0.2500 10.50000 0.05 0.36 Q15 1 0.7424 -0.1149 0.3398 11.00000 0.05 0.35 Q16 1 0.8268 -0.0684 0.0501 11.00000 0.05 0.34 Q17 1 0.5928 0.2022 0.2427 11.00000 0.05 0.34 Q18 1 0.4992 -0.0608 0.1424 11.00000 0.05 0.33 Q19 1 0.5032 0.8516 0.2574 11.00000 0.05 0.32 Q20 1 0.5000 0.1185 0.2500 10.50000 0.05 0.31 ; _shelx_res_checksum 38927 _shelx_hkl_file ; 0 0 -4 1729.30 75.9503 -2 0 0 -4 1729.30 75.9503 1 0 0 -6 661145. 3387.72 -2 0 0 -6 661145. 3387.72 1 0 0 8 322332. 2651.09 -2 0 0 8 322332. 2651.09 1 0 0 -10 164425. 1812.01 -2 0 0 -10 164425. 1812.01 1 0 0 12 28956.5 285.071 -2 0 0 12 28956.5 285.071 1 0 0 14 44177.1 239.479 -2 0 0 14 44177.1 239.479 1 0 0 -16 22519.6 203.903 -2 0 0 -16 22519.6 203.903 1 0 0 18 5913.88 328.259 -2 0 0 18 5913.88 328.259 1 0 0 20 11932.6 378.257 -2 0 0 20 11932.6 378.257 1 0 0 22 22259.7 403.586 -2 0 0 22 22259.7 403.586 1 0 0 -24 2144.70 434.685 -2 0 0 -24 2144.70 434.685 1 0 0 -26 3990.99 500.840 -2 0 0 -26 3990.99 500.840 1 0 -2 0 291650. 2335.24 -2 0 2 0 291650. 2335.24 1 0 2 1 198185. 1184.58 -2 0 -2 1 198185. 1184.58 1 0 -2 2 8718.26 98.5703 -2 0 2 2 8718.26 98.5703 1 0 2 3 180448. 1219.55 -2 0 -2 3 180448. 1219.55 1 0 -2 4 2394.98 66.5967 -2 0 2 4 2394.98 66.5967 1 0 2 5 730.489 63.7988 -2 0 -2 5 730.489 63.7988 1 0 2 6 12948.8 95.4829 -2 0 -2 6 12948.8 95.4829 1 0 2 -7 22103.3 148.316 -2 0 -2 -7 22103.3 148.316 1 0 -2 -8 65523.7 179.031 -2 0 2 -8 65523.7 179.031 1 0 -2 9 20874.9 101.952 -2 0 2 9 20874.9 101.952 1 0 2 -10 50186.4 252.268 -2 0 -2 -10 50186.4 252.268 1 0 2 -11 233.553 99.2309 -2 0 -2 -11 233.553 99.2309 1 0 2 -12 14746.4 134.309 -2 0 -2 -12 14746.4 134.309 1 0 2 -13 3883.68 106.501 -2 0 -2 -13 3883.68 106.501 1 0 2 -14 27431.0 205.315 -2 0 -2 -14 27431.0 205.315 1 0 2 15 6231.69 130.726 -2 0 -2 15 6231.69 130.726 1 0 2 16 11825.2 139.993 -2 0 -2 16 11825.2 139.993 1 0 2 -17 440.846 99.5060 -2 0 -2 -17 440.846 99.5060 1 0 -2 -18 16433.2 206.432 -2 0 2 -18 16433.2 206.432 1 0 -2 19 394.133 127.704 -2 0 2 19 394.133 127.704 1 0 2 -20 12267.6 200.833 -2 0 -2 -20 12267.6 200.833 1 0 -2 21 5964.58 218.385 -2 0 2 21 5964.58 218.385 1 0 -2 22 11217.6 357.648 -2 0 2 22 11217.6 357.648 1 0 -2 23 339.981 266.661 -2 0 2 23 339.981 266.661 1 0 -2 24 6667.37 352.484 -2 0 2 24 6667.37 352.484 1 0 -2 -25 940.168 307.129 -2 0 2 -25 940.168 307.129 1 0 -2 -26 3849.31 471.448 -2 0 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11 -7 -6 555.993 271.182 -2 -11 7 -5 555.993 271.182 1 11 -7 -7 1889.93 235.964 -2 -11 7 -6 1889.93 235.964 1 11 -7 -8 1199.61 235.086 -2 -11 7 -7 1199.61 235.086 1 11 -7 -9 3304.44 264.161 -2 -11 7 -8 3304.44 264.161 1 11 -7 -10 1386.19 296.958 -2 -11 7 -9 1386.19 296.958 1 11 -7 -11 4799.39 343.698 -2 -11 7 -10 4799.39 343.698 1 11 -7 -12 553.454 300.219 -2 -11 7 -11 553.454 300.219 1 11 7 -13 1455.23 451.556 -2 -11 -7 -12 1455.23 451.556 1 11 7 -14 928.338 456.032 -2 -11 -7 -13 928.338 456.032 1 11 7 -15 1341.95 475.809 -2 -11 -7 -14 1341.95 475.809 1 11 7 -16 696.653 482.917 -2 -11 -7 -15 696.653 482.917 1 11 -9 8 279.873 387.543 -2 -11 9 9 279.873 387.543 1 11 -9 7 1594.36 399.507 -2 -11 9 8 1594.36 399.507 1 11 -9 6 95.3253 292.744 -2 -11 9 7 95.3253 292.744 1 11 -9 5 678.765 375.027 -2 -11 9 6 678.765 375.027 1 11 -9 4 1119.85 374.054 -2 -11 9 5 1119.85 374.054 1 11 -9 3 2245.71 394.077 -2 -11 9 4 2245.71 394.077 1 -11 9 -2 613.693 282.089 -2 11 -9 -3 613.693 282.089 1 -11 9 -1 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11.2491 108.248 2 5 -3 7 162.901 111.195 2 -5 -3 -8 362.085 42.4287 2 -5 -3 -9 206.304 83.7973 2 5 3 10 6295.36 295.520 2 5 3 11 5412.11 151.586 2 5 3 12 560.319 86.9435 2 5 3 13 14.4494 94.2420 2 5 3 14 6475.07 98.1208 2 5 3 15 2849.31 135.807 2 5 3 16 650.942 262.171 2 5 3 19 687.958 288.980 2 5 3 20 2719.00 307.065 2 5 3 21 545.991 299.631 2 5 -5 -11 585.818 231.512 2 5 -5 -10 4689.80 266.896 2 5 -5 -9 1171.38 221.785 2 5 -5 -8 8450.21 287.555 2 5 -5 -7 4325.21 95.0405 2 5 -5 -6 15709.8 113.539 2 -5 5 5 4962.56 89.4586 2 5 -5 -4 3466.80 91.2449 2 -5 5 3 426.720 89.7240 2 5 -5 -2 1638.95 100.311 2 -5 5 1 837.938 133.969 2 5 -5 0 27691.7 384.288 2 5 5 1 8220.94 125.392 2 5 -5 2 8578.37 105.874 2 5 -5 3 2017.08 203.302 2 5 -5 4 4822.34 224.549 2 -5 -5 -10 3645.56 61.6551 2 -5 -5 -11 2089.46 79.0134 2 -5 -5 -12 5301.39 120.998 2 5 5 13 285.778 103.099 2 -5 -5 -14 10016.1 172.481 2 5 5 15 372.688 304.003 2 5 5 16 783.774 287.893 2 5 5 17 414.403 287.613 2 5 5 18 1029.28 294.056 2 5 5 19 874.329 288.403 2 -5 7 10 9601.91 301.244 2 -5 7 9 123.345 229.230 2 5 -7 -8 5764.78 203.989 2 5 -7 -7 2854.65 180.444 2 -5 7 6 2465.54 162.886 2 5 -7 -5 1543.13 129.017 2 5 -7 -4 9537.63 162.269 2 -5 7 3 35.6198 110.902 2 5 -7 -2 7429.99 188.323 2 5 7 -1 3739.52 157.857 2 5 7 0 13076.8 202.878 2 5 -7 1 12215.9 182.236 2 5 -7 2 5280.77 137.003 2 5 7 3 2847.46 109.121 2 5 7 4 6785.06 130.262 2 5 7 15 826.506 326.673 2 5 7 16 212.803 321.712 2 5 7 17 114.476 334.456 2 5 7 18 1299.13 322.608 2 -5 9 12 116.478 248.045 2 -5 9 11 4368.24 296.184 2 -5 9 10 1239.75 266.868 2 -5 9 9 3035.50 278.130 2 -5 9 8 106.144 220.132 2 -5 9 7 2178.97 194.386 2 5 -9 -6 22.0127 241.920 2 5 -9 -5 2589.90 279.877 2 5 -9 -4 1237.47 262.645 2 5 -9 -3 3847.22 202.969 2 5 -9 -2 1119.00 180.810 2 5 -9 -1 4793.37 309.774 2 5 -9 0 2640.91 287.107 2 5 -9 1 779.265 251.352 2 -5 11 10 1096.00 300.050 2 -5 11 9 1472.98 280.016 2 6 0 -22 5721.00 527.608 2 6 0 -20 5668.02 504.670 2 6 0 -18 2805.01 159.598 2 6 0 -16 2664.72 118.450 2 6 0 -14 25149.8 197.502 2 6 0 -12 22113.8 226.505 2 6 0 -10 5623.20 146.451 2 6 0 -8 5961.42 241.906 2 6 0 -6 24596.4 237.512 2 6 0 -4 13697.0 182.922 2 6 0 -2 30681.7 222.528 2 6 0 0 3199.57 109.952 2 6 0 2 31.8753 80.1772 2 -6 0 -4 15373.4 120.066 2 6 0 6 32910.9 198.551 2 6 0 8 5815.31 117.351 2 6 0 10 1140.74 96.9903 2 6 0 12 19814.3 229.937 2 6 0 14 26282.1 262.830 2 6 0 16 1130.59 367.266 2 6 0 18 7574.79 366.788 2 6 0 20 7333.13 397.803 2 6 0 22 3885.27 349.640 2 6 0 24 1573.42 330.154 2 6 0 26 1495.01 367.184 2 -6 -2 15 2867.23 212.984 2 -6 -2 14 12818.9 200.261 2 6 2 -13-32.3318 175.663 2 6 2 -12 10248.8 287.490 2 6 2 -11 656.556 122.300 2 6 -2 -10 5817.67 76.5410 2 6 -2 -9 1167.06 58.3810 2 6 -2 -8 11751.0 116.496 2 6 -2 -7 1468.66 115.849 2 6 -2 -6 7907.83 142.466 2 6 -2 -5 2485.91 137.006 2 6 -2 -4 20934.9 215.202 2 6 -2 -3 52.7307 84.3195 2 6 -2 -2 31869.1 170.160 2 6 -2 -1 983.490 80.4873 2 6 -2 0 32647.9 135.868 2 -6 2 -1 3.25488 57.5081 2 6 2 2 19316.0 100.996 2 -6 2 -3 399.518 59.7702 2 6 -2 4 30266.7 136.785 2 6 -2 5 2505.75 63.9398 2 -6 -2 -6 10361.1 102.204 2 6 -2 7 5295.03 89.4973 2 6 -2 8 11896.0 111.304 2 6 -2 9 1550.73 84.9158 2 6 -2 10 7955.68 111.963 2 6 2 11 284.334 93.5736 2 6 -2 12 7138.62 122.647 2 6 -2 13 1171.15 100.254 2 6 -2 14 9249.64 134.435 2 6 -2 15 319.834 189.027 2 6 -2 16 188.699 181.643 2 6 -2 17 0.71640 188.617 2 6 -2 18 725.774 276.595 2 6 -2 19 51.1933 263.428 2 6 -2 20 851.886 296.341 2 6 -2 21 130.054 213.211 2 6 -2 22 1212.29 231.780 2 6 -2 23-40.6405 218.251 2 6 2 24 278.226 320.260 2 6 -4 -12 7926.74 315.649 2 6 -4 -11 113.849 235.254 2 6 -4 -10 15281.9 354.263 2 6 -4 -9 880.408 227.583 2 6 -4 -8 1446.22 223.219 2 6 -4 -7 577.679 65.9727 2 6 -4 -6 264.441 85.9977 2 6 -4 -5 7244.95 136.152 2 6 -4 -4 16742.4 129.932 2 6 -4 -3 527.262 101.772 2 6 -4 -2 5402.13 92.7084 2 6 -4 -1 461.095 91.5199 2 6 4 0 17450.1 170.311 2 6 4 1 10365.0 131.350 2 6 4 2 4677.02 75.1009 2 6 -4 3 1387.78 188.952 2 6 -4 4 7472.54 248.672 2 -6 -4 -11 426.054 60.7163 2 -6 -4 -12 1143.52 92.1012 2 6 -4 13 717.747 259.172 2 6 -4 14 2763.65 301.130 2 6 -4 15 165.173 199.197 2 6 -4 16 1423.63 302.702 2 6 -4 17 1429.20 300.787 2 6 4 18 2773.05 313.555 2 6 4 20 617.949 306.114 2 6 -6 -12 2333.92 272.814 2 6 -6 -11 5212.02 303.858 2 6 -6 -10 8986.58 328.059 2 6 -6 -9 2174.93 257.005 2 6 -6 -8 2003.71 169.141 2 6 -6 -7 492.991 85.0987 2 6 -6 -6 2152.24 97.8898 2 6 -6 -5 7364.09 164.352 2 -6 6 4 4079.72 119.449 2 6 -6 -3 4486.02 158.434 2 6 -6 -2 9418.51 185.295 2 6 -6 -1 874.834 223.855 2 6 -6 0 19166.8 382.035 2 6 6 1 6499.28 135.632 2 6 -6 2 2525.27 89.3671 2 6 6 3 4927.41 76.2148 2 6 -6 4 6211.79 273.133 2 6 6 18 364.560 319.291 2 6 6 20 477.641 312.898 2 6 -8 -13 20.7636 255.113 2 6 -8 -12 90.3688 254.611 2 6 -8 -11 1855.18 279.673 2 6 -8 -10 1861.59 191.496 2 6 -8 -9 141.418 249.998 2 6 -8 -8 1573.83 264.109 2 6 -8 -7 141.724 245.703 2 6 -8 -6 4.51424 243.999 2 6 -8 -5 30.6343 156.473 2 6 -8 -4 201.915 145.612 2 -6 8 3 54.4357 119.403 2 6 -8 -2 226.791 119.856 2 6 -8 -1 529.445 118.725 2 6 -8 0 2426.11 129.759 2 6 -8 1 14.0332 241.468 2 6 -8 2 1252.36 256.322 2 6 -10 -7 1579.11 295.809 2 6 -10 -6 1594.45 293.093 2 6 -10 -5 255.441 281.129 2 6 -10 -4 1909.85 306.068 2 6 -10 -3 3795.76 216.827 2 6 -10 -2 580.512 197.640 2 6 -10 -1 9423.88 258.993 2 6 -10 0 4323.20 220.405 2 6 -10 1 1163.74 263.083 2 6 -10 3 1272.39 286.309 2 6 -12 1 1208.48 350.160 2 -7 -1 15 408.133 116.874 2 7 1 -14 8704.55 170.566 2 7 -1 -13 1682.27 113.888 2 7 1 -11 25.5099 93.6295 2 7 -1 -10 2553.13 115.430 2 7 1 -9 65.1047 186.190 2 7 -1 -8 7655.78 279.459 2 7 -1 -7 2933.86 153.126 2 7 -1 -6 2169.62 117.576 2 7 -1 -5 138.056 87.5325 2 7 -1 -4 6686.17 111.843 2 7 -1 -3 3593.52 98.2283 2 7 -1 -2 6917.27 106.789 2 7 -1 -1 1698.61 84.2870 2 7 -1 0 23281.1 133.994 2 7 1 1 5085.88 83.7455 2 -7 1 -2 12602.7 102.931 2 -7 1 -3 766.384 64.0687 2 -7 1 -4 7695.28 85.6741 2 -7 1 -5 20.4998 67.5591 2 -7 -1 -6 30.4222 77.7187 2 7 -1 7 53.7765 73.6695 2 7 -1 8 11704.3 119.618 2 7 -1 9 4808.27 112.836 2 7 -1 10 7300.03 161.063 2 7 -1 11 75.2352 113.373 2 7 -1 12 1735.74 125.656 2 7 1 13 498.516 167.994 2 7 1 14 8303.71 146.586 2 7 -1 15 732.653 175.658 2 7 -1 17 181.341 290.095 2 7 -1 21 311.456 298.977 2 7 -1 22 605.568 308.105 2 7 -1 23 94.3850 312.713 2 7 -1 24 455.128 321.618 2 7 1 25 103.793 330.320 2 7 -3 -9 14.8050 61.4398 2 7 -3 -8 735.205 216.527 2 7 -3 -7 748.925 209.479 2 7 -3 -6 1099.69 205.046 2 7 -3 -5 1384.35 200.166 2 7 -3 -4 1253.33 189.163 2 7 -3 -3 3945.01 142.947 2 7 -3 -2 3279.60 135.034 2 7 -3 -1 829.597 98.1076 2 7 -3 0 422.649 87.6731 2 -7 3 -1 9408.12 120.546 2 -7 3 -2 131.892 67.8888 2 -7 3 -3 18.6417 52.8044 2 7 -3 4 1238.97 183.765 2 7 -3 5 2152.95 194.518 2 -7 -3 -11 26.2677 89.7869 2 7 3 12 5477.62 210.557 2 7 3 13 382.726 169.596 2 7 -3 17 5.53571 266.909 2 7 -3 18 766.073 294.002 2 7 -3 19 134.707 279.007 2 7 -3 20 1471.73 319.013 2 7 -3 21 67.9131 326.275 2 7 -3 22 786.562 336.507 2 7 3 24 266.158 349.351 2 7 -5 -9 3660.23 279.777 2 7 -5 -8 2951.12 90.6203 2 7 -5 -7 417.860 96.7531 2 7 -5 -6 41.8449 98.7818 2 7 -5 -5 454.075 217.363 2 7 -5 -4 2782.24 160.487 2 7 -5 -3 655.667 210.463 2 7 -5 -2 13131.0 333.890 2 7 5 -1 3543.84 141.960 2 7 5 0 12320.2 170.874 2 7 -5 1 2070.91 225.057 2 7 5 2 62.3070 59.2359 2 7 -5 3 149.855 207.087 2 7 -5 4 3689.72 246.331 2 7 -5 5 994.246 202.056 2 7 5 21 278.020 305.151 2 7 -7 -10 2616.13 281.267 2 7 -7 -9 3227.03 293.466 2 7 -7 -7 466.175 135.896 2 7 -7 -6 5933.55 162.085 2 7 -7 -5 173.502 133.037 2 7 -7 -4 2147.46 270.555 2 7 -7 -3 3951.90 289.936 2 7 -7 -2 1742.78 262.367 2 7 -7 -1 10135.1 347.828 2 7 7 0 20061.3 228.527 2 7 -7 1 1213.23 259.084 2 7 7 2 3078.18 104.211 2 7 -7 3 464.514 242.701 2 7 -7 4 1307.24 246.025 2 7 -9 -5 734.487 240.254 2 7 -9 -4 702.530 209.074 2 7 -9 1 1844.08 292.930 2 8 0 -20 5495.88 466.061 2 8 0 -18 4889.13 243.955 2 8 0 -16 291.313 207.915 2 8 0 -14 5905.11 219.042 2 8 0 -12 4576.68 203.334 2 8 0 -10 18378.4 454.594 2 8 0 -8 817.997 295.933 2 8 0 -6 1276.87 282.233 2 8 0 -4 18833.9 244.951 2 8 0 -2 170.224 122.422 2 8 0 0 1511.79 117.295 2 8 0 2 28816.2 205.873 2 -8 0 -4 5016.11 114.952 2 -8 0 -6 9713.85 154.098 2 -8 0 -8 2256.03 160.159 2 8 0 10 15383.9 211.323 2 8 0 12 11412.3 231.622 2 8 0 14 527.105 207.896 2 8 0 16 8.45443 366.869 2 8 0 18 10191.7 513.507 2 8 0 20 2394.88 489.821 2 8 0 22 760.122 444.798 2 8 -2 -11 252.497 139.905 2 8 -2 -6 497.821 205.747 2 8 -2 -4 7394.02 263.516 2 8 -2 -3 1897.68 139.303 2 8 -2 -2 4391.26 144.263 2 8 -2 -1 2154.59 110.863 2 8 2 0 6751.11 128.829 2 8 2 1 1503.35 98.5436 2 -8 2 -2 6076.46 117.018 2 -8 2 -3 6764.94 115.373 2 -8 2 -4 5685.11 107.465 2 8 -2 5 2238.50 190.097 2 -8 2 -6-15.5380 180.667 2 8 2 11 3369.96 229.096 2 8 -4 -9 966.493 81.5030 2 8 -4 -8 2640.09 121.576 2 8 -4 -6 2027.81 240.016 2 8 -4 -5 168.031 204.776 2 8 -4 -4 278.775 212.992 2 8 -4 -3 509.714 210.549 2 8 -4 -2 886.822 137.618 2 8 4 -1 1148.42 135.600 2 8 4 0 13068.5 177.526 2 8 4 1 88.6563 96.9760 2 8 4 2 21.2865 72.0071 2 8 -4 3 109.791 42.5404 2 8 -4 4 22.7629 194.746 2 8 -4 5 141.882 200.615 2 8 -4 16 73.7850 276.275 2 8 -4 17 115.765 288.385 2 8 -4 18 131.844 306.648 2 -8 6 4 833.823 222.327 2 8 6 0 11850.5 216.731 2 8 6 1 3630.28 117.912 2 8 6 2 663.196 61.7568 2 8 6 21 984.880 379.266 2 9 -1 9 4.52079 242.824 2 9 3 3 1174.72 111.651 2 9 3 4 77.0233 85.7121 2 9 5 1 1371.73 119.637 2 9 5 2 1640.62 79.2600 2 9 5 21 198.524 352.718 2 10 0 -18 762.807 197.997 2 10 0 -16 72.8037 344.558 2 10 0 -14 17441.1 484.805 2 10 0 -12 7249.06 228.005 2 10 0 -10 48.1420 296.386 2 10 0 -8 2428.53 304.345 2 10 0 -6 8395.88 350.333 2 10 0 -4 4554.64 306.682 2 10 0 -2 3122.10 286.787 2 10 0 0 9657.53 226.133 2 10 0 2 2638.06 151.658 2 -10 0 -4 4630.70 160.661 2 -10 0 -6 1588.91 136.804 2 -10 0 -8 15408.0 264.952 2 -10 0 -10 1613.34 186.602 2 10 0 12 1640.38 361.953 2 10 0 14 10247.6 471.193 2 10 0 16 93.8303 374.096 2 10 0 18 785.113 377.517 2 10 -2 5 259.575 235.739 2 11 1 15 302.619 292.710 2 12 0 -16 1800.98 381.158 2 12 0 -14 2476.44 371.593 2 12 0 -12 854.565 346.492 2 12 0 -10 518.805 369.646 2 12 0 -8 7857.13 379.382 2 12 0 -6 1237.18 308.126 2 12 0 -4 4396.58 323.304 2 12 0 -2 8706.91 334.798 2 12 0 0 14818.7 305.566 2 12 0 2 4428.98 250.528 2 12 0 4 10031.6 273.478 2 12 0 6 4347.67 233.298 2 12 0 8 217.765 422.145 2 12 0 10 5447.44 447.954 2 12 0 12 534.143 411.974 2 12 0 14 187.146 383.297 2 12 0 16 2.57216 415.742 2 14 0 -14 208.439 400.873 2 14 0 -12 1108.78 405.970 2 14 0 -10 1856.46 401.210 2 14 0 -8 135.672 369.364 2 14 0 -6 928.824 364.921 2 14 0 -4 4913.19 289.972 2 14 0 -2 2446.01 291.869 2 14 0 0 4091.17 299.759 2 14 0 2 2187.37 277.530 2 14 0 4 3108.54 279.735 2 14 0 6 1675.31 247.709 2 14 0 8 1708.68 498.444 2 14 0 10 3485.10 501.687 2 14 -2 5 314.317 259.315 2 15 -1 0 1059.48 279.855 2 15 -1 1 66.2769 255.192 2 15 -1 3 8.38807 249.279 2 15 -1 4 434.606 249.938 2 15 -1 5 135.551 238.651 2 15 -1 9 6.84049 302.310 2 15 -3 2 176.152 276.781 2 15 -3 3 101.199 280.184 2 15 -3 4 34.5251 270.516 2 15 -3 5 270.567 265.413 2 15 -3 6-63.9767 255.916 2 15 -5 1 447.976 318.312 2 15 -5 5 60.5885 291.641 2 16 0 -10 488.904 448.652 2 16 0 -8 730.667 449.075 2 16 0 -6 912.629 324.578 2 16 0 -4 91.0709 252.559 2 16 0 -2 1138.48 260.711 2 16 0 0 4213.01 287.603 2 16 0 2 893.230 509.503 2 16 0 4 369.195 525.538 2 16 -2 -2 98.4078 293.580 2 16 -2 -1 226.259 294.847 2 16 -2 0 982.965 295.752 2 16 -2 1 179.276 280.715 2 16 -2 2 123.777 279.682 2 16 -2 3 17.9833 231.520 2 16 -2 4 61.7566 269.836 2 16 -2 5 64.7827 267.092 2 16 -4 0 279.102 312.406 2 16 -4 1 69.6901 312.643 2 16 -4 2 141.855 314.185 2 16 -4 3 30.5963 307.936 2 16 -4 4 561.070 303.433 2 16 -4 5-4.45133 293.990 2 17 1 -10 743.182 359.632 2 17 1 -9 98.2310 340.163 2 17 -1 -8 170.652 227.836 2 17 -1 -7 308.776 333.054 2 17 -1 -6 299.069 323.892 2 17 -1 -5 241.424 329.203 2 17 -1 -4 8.09204 313.183 2 17 -1 -3 144.311 310.139 2 17 -1 -2 259.040 308.804 2 17 -1 -1 2.57840 306.761 2 17 -3 -3 59.0220 317.758 2 17 -3 -2 245.157 328.687 2 17 -3 -1 81.6515 313.364 2 17 -3 0 272.713 313.429 2 17 -3 1 184.092 312.909 2 17 -3 2 5.87476 319.161 2 17 -3 3 52.4692 307.399 2 17 -3 4 146.967 303.939 2 18 -2 -1-62.1710 335.205 2 ; _shelx_hkl_checksum 93942 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 -0.01441(7) 0.250000 0.0270(3) Uani 1 2 d S T P . . Cl1 Cl 0.81171(13) -0.12024(19) 0.10674(9) 0.0652(6) Uani 1 1 d . U . . . N2 N 0.500000 0.1684(5) 0.250000 0.0289(15) Uani 1 2 d S T P . . N3 N 0.500000 0.8018(5) 0.250000 0.0265(14) Uani 1 2 d S T P . . N1 N 0.4954(3) -0.0138(3) 0.15876(16) 0.0259(9) Uani 1 1 d . . . . . O1 O 0.6713(3) -0.0147(4) 0.2502(2) 0.0463(10) Uani 1 1 d . . . . . H1A H 0.712270 -0.022507 0.278007 0.069 Uiso 1 1 d G . . . . H1B H 0.688996 -0.049745 0.218579 0.069 Uiso 1 1 d G . . . . C9 C 0.500000 0.5512(6) 0.250000 0.0327(18) Uani 1 2 d S T P . . C8 C 0.500000 0.4193(6) 0.250000 0.0310(18) Uani 1 2 d S T P . . C10 C 0.5699(4) 0.6171(5) 0.2781(3) 0.0432(16) Uani 1 1 d . . . . . H10 H 0.618779 0.577499 0.297511 0.052 Uiso 1 1 calc R . . . . C1 C 0.4384(4) 0.0581(5) 0.1274(2) 0.0321(13) Uani 1 1 d . . . . . H1 H 0.397301 0.105825 0.148231 0.039 Uiso 1 1 calc R . . . . C3 C 0.4989(3) -0.0043(4) 0.0334(2) 0.0260(11) Uani 1 1 d . . . . . C5 C 0.5518(4) -0.0828(5) 0.1277(3) 0.0387(15) Uani 1 1 d . . . . . H5 H 0.590858 -0.134958 0.148801 0.046 Uiso 1 1 calc R . . . . C2 C 0.4378(4) 0.0646(5) 0.0663(2) 0.0348(14) Uani 1 1 d . . . . . H2 H 0.396311 0.115461 0.046258 0.042 Uiso 1 1 calc R . . . . C4 C 0.5553(4) -0.0812(5) 0.0667(2) 0.0339(14) Uani 1 1 d . . . . . H4 H 0.595782 -0.132002 0.047195 0.041 Uiso 1 1 calc R . . . . C11 C 0.5677(4) 0.7405(5) 0.2776(3) 0.0393(15) Uani 1 1 d . . . . . H11 H 0.615140 0.782559 0.297121 0.047 Uiso 1 1 calc R . . . . C7 C 0.5771(4) 0.3537(5) 0.2355(3) 0.0377(15) Uani 1 1 d . . . . . H7 H 0.631480 0.393175 0.226336 0.045 Uiso 1 1 calc R . . . . O2 O 0.7484(4) -0.0958(6) 0.3559(2) 0.0848(19) Uani 1 1 d . . . . . C6 C 0.5740(4) 0.2326(5) 0.2345(3) 0.0345(15) Uani 1 1 d . . . . . H6 H 0.626075 0.191270 0.222444 0.041 Uiso 1 1 calc R . . . . O3 O 0.7750(5) -0.0231(7) 0.1355(4) 0.146(3) Uani 1 1 d . U . . . N4 N 0.8381(4) -0.1579(8) 0.4312(3) 0.082(2) Uani 1 1 d . . . . . C12 C 0.8086(6) -0.0741(9) 0.3955(4) 0.073(2) Uani 1 1 d . . . . . O5 O 0.9078(4) -0.1290(8) 0.1145(3) 0.126(3) Uani 1 1 d . U . . . C13 C 0.8490(8) 0.0459(10) 0.4025(5) 0.116(4) Uani 1 1 d . . . . . H13A H 0.810725 0.103530 0.381669 0.174 Uiso 1 1 calc GR . . . . H13B H 0.909595 0.046571 0.386082 0.174 Uiso 1 1 calc GR . . . . H13C H 0.853302 0.066192 0.444517 0.174 Uiso 1 1 calc GR . . . . C15 C 0.8049(7) -0.2791(9) 0.4209(5) 0.108(3) Uani 1 1 d . . . . . H15A H 0.764089 -0.280108 0.386133 0.161 Uiso 1 1 calc GR . . . . H15B H 0.772312 -0.306033 0.455405 0.161 Uiso 1 1 calc GR . . . . H15C H 0.856324 -0.331300 0.414279 0.161 Uiso 1 1 calc GR . . . . C14 C 0.9099(6) -0.1405(10) 0.4776(4) 0.099(3) Uani 1 1 d . . . . . H14A H 0.968271 -0.129628 0.458979 0.148 Uiso 1 1 calc GR . . . . H14B H 0.912754 -0.209734 0.503317 0.148 Uiso 1 1 calc GR . . . . H14C H 0.895823 -0.070781 0.501001 0.148 Uiso 1 1 calc GR . . . . O6 O 0.7794(5) -0.1448(14) 0.0518(4) 0.226(6) Uani 1 1 d . U . . . O4 O 0.7730(6) -0.2052(10) 0.1479(6) 0.204(5) Uani 1 1 d . U . . . 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 0.0525(7) 0.0125(4) 0.0160(4) 0.000 0.0005(4) 0.000 Cl1 0.0648(13) 0.0652(13) 0.0656(13) -0.0205(10) 0.0012(10) 0.0097(10) N2 0.044(4) 0.019(3) 0.024(3) 0.000 0.008(3) 0.000 N3 0.040(4) 0.014(3) 0.025(3) 0.000 -0.006(3) 0.000 N1 0.043(2) 0.0199(19) 0.0148(19) -0.0014(17) 0.002(2) 0.0008(19) O1 0.052(3) 0.043(2) 0.045(2) -0.008(2) 0.002(2) 0.006(2) C9 0.043(5) 0.019(3) 0.036(4) 0.000 0.002(4) 0.000 C8 0.044(5) 0.019(4) 0.031(4) 0.000 -0.005(4) 0.000 C10 0.049(4) 0.020(3) 0.059(4) 0.002(3) -0.014(3) 0.006(3) C1 0.046(4) 0.028(3) 0.022(3) 0.005(3) 0.008(2) 0.013(3) C3 0.030(3) 0.026(3) 0.022(2) -0.003(2) -0.003(2) -0.004(2) C5 0.049(4) 0.035(3) 0.032(3) 0.000(3) -0.010(3) 0.015(3) C2 0.047(4) 0.037(3) 0.020(3) 0.009(3) 0.000(3) 0.013(3) C4 0.039(3) 0.044(4) 0.018(3) -0.004(3) -0.002(2) 0.013(3) C11 0.049(4) 0.024(3) 0.044(4) 0.003(3) -0.012(3) -0.007(3) C7 0.042(4) 0.022(3) 0.049(4) 0.007(3) 0.004(3) -0.006(3) O2 0.073(4) 0.126(6) 0.055(4) 0.005(3) -0.010(3) 0.025(3) C6 0.042(4) 0.021(3) 0.041(4) -0.002(2) 0.008(3) 0.007(3) O3 0.103(5) 0.133(6) 0.199(9) -0.072(6) -0.042(5) 0.033(4) N4 0.066(5) 0.107(7) 0.073(5) 0.002(5) -0.009(4) 0.020(4) C12 0.064(5) 0.103(8) 0.052(5) 0.003(5) 0.007(4) 0.021(5) O5 0.065(4) 0.205(8) 0.109(5) -0.036(5) 0.013(3) 0.011(4) C13 0.157(11) 0.100(9) 0.091(8) 0.006(7) 0.008(7) -0.001(8) C15 0.151(10) 0.069(7) 0.102(8) 0.011(6) -0.002(7) -0.010(6) C14 0.073(6) 0.148(9) 0.074(6) 0.019(6) -0.015(5) 0.005(6) O6 0.103(6) 0.466(18) 0.110(6) -0.133(7) 0.004(4) -0.046(8) O4 0.121(6) 0.200(8) 0.291(11) 0.113(10) 0.005(7) -0.012(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 N2 Cu1 N3 180.0 . 1_545 N2 Cu1 O1 90.08(10) . . N3 Cu1 O1 89.92(10) 1_545 . N1 Cu1 N2 89.80(11) 2_655 . N1 Cu1 N2 89.80(11) . . N1 Cu1 N3 90.20(11) 2_655 1_545 N1 Cu1 N3 90.20(11) . 1_545 N1 Cu1 N1 179.6(2) 2_655 . N1 Cu1 O1 90.43(18) . . N1 Cu1 O1 89.57(18) 2_655 . O3 Cl1 O5 113.2(4) . . O3 Cl1 O4 93.4(7) . . O5 Cl1 O4 106.2(5) . . O6 Cl1 O3 117.5(7) . . O6 Cl1 O5 115.1(5) . . O6 Cl1 O4 108.4(7) . . C6 N2 Cu1 122.2(3) 2_655 . C6 N2 Cu1 122.2(3) . . C6 N2 C6 115.6(6) . 2_655 C11 N3 Cu1 120.9(3) . 1_565 C11 N3 Cu1 120.9(3) 2_655 1_565 C11 N3 C11 118.2(7) 2_655 . C1 N1 Cu1 121.8(3) . . C5 N1 Cu1 120.9(4) . . C5 N1 C1 117.2(4) . . Cu1 O1 H1A 132.9 . . Cu1 O1 H1B 108.9 . . H1A O1 H1B 109.5 . . C10 C9 C8 122.0(3) 2_655 . C10 C9 C8 122.0(3) . . C10 C9 C10 116.1(7) 2_655 . C7 C8 C9 122.0(3) 2_655 . C7 C8 C9 122.0(3) . . C7 C8 C7 116.1(7) 2_655 . C9 C10 H10 119.7 . . C11 C10 C9 120.6(6) . . C11 C10 H10 119.7 . . N1 C1 H1 118.6 . . N1 C1 C2 122.7(5) . . C2 C1 H1 118.6 . . C2 C3 C3 121.2(6) . 5_655 C4 C3 C3 123.0(6) . 5_655 C4 C3 C2 115.8(4) . . N1 C5 H5 118.2 . . N1 C5 C4 123.5(5) . . C4 C5 H5 118.2 . . C1 C2 C3 120.5(5) . . C1 C2 H2 119.7 . . C3 C2 H2 119.7 . . C3 C4 H4 119.9 . . C5 C4 C3 120.2(5) . . C5 C4 H4 119.9 . . N3 C11 C10 122.3(6) . . N3 C11 H11 118.9 . . C10 C11 H11 118.9 . . C8 C7 H7 119.8 . . C6 C7 C8 120.4(6) . . C6 C7 H7 119.8 . . N2 C6 C7 123.7(5) . . N2 C6 H6 118.1 . . C7 C6 H6 118.1 . . C12 N4 C15 118.3(8) . . C12 N4 C14 123.8(9) . . C15 N4 C14 117.6(8) . . O2 C12 N4 120.5(10) . . O2 C12 C13 121.5(9) . . N4 C12 C13 118.0(9) . . C12 C13 H13A 109.5 . . C12 C13 H13B 109.5 . . C12 C13 H13C 109.5 . . H13A C13 H13B 109.5 . . H13A C13 H13C 109.5 . . H13B C13 H13C 109.5 . . N4 C15 H15A 109.5 . . N4 C15 H15B 109.5 . . N4 C15 H15C 109.5 . . H15A C15 H15B 109.5 . . H15A C15 H15C 109.5 . . H15B C15 H15C 109.5 . . N4 C14 H14A 109.5 . . N4 C14 H14B 109.5 . . N4 C14 H14C 109.5 . . H14A C14 H14B 109.5 . . H14A C14 H14C 109.5 . . H14B C14 H14C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cu1 N2 2.036(6) . Cu1 N3 2.047(5) 1_545 Cu1 N1 2.027(3) 2_655 Cu1 N1 2.027(3) . Cu1 O1 2.482(4) . Cl1 O3 1.372(7) . Cl1 O5 1.401(6) . Cl1 O6 1.325(8) . Cl1 O4 1.440(10) . N2 C6 1.341(6) 2_655 N2 C6 1.341(6) . N3 C11 1.331(6) . N3 C11 1.331(6) 2_655 N1 C1 1.333(7) . N1 C5 1.329(7) . O1 H1A 0.8500 . O1 H1B 0.8498 . C9 C8 1.470(9) . C9 C10 1.386(7) 2_655 C9 C10 1.386(7) . C8 C7 1.380(7) 2_655 C8 C7 1.380(7) . C10 H10 0.9300 . C10 C11 1.375(8) . C1 H1 0.9300 . C1 C2 1.361(7) . C3 C3 1.487(9) 5_655 C3 C2 1.395(7) . C3 C4 1.384(7) . C5 H5 0.9300 . C5 C4 1.358(8) . C2 H2 0.9300 . C4 H4 0.9300 . C11 H11 0.9300 . C7 H7 0.9300 . C7 C6 1.350(7) . O2 C12 1.246(9) . C6 H6 0.9300 . N4 C12 1.291(11) . N4 C15 1.448(11) . N4 C14 1.457(10) . C12 C13 1.466(13) . C13 H13A 0.9600 . C13 H13B 0.9600 . C13 H13C 0.9600 . C15 H15A 0.9600 . C15 H15B 0.9600 . C15 H15C 0.9600 . C14 H14A 0.9600 . C14 H14B 0.9600 . C14 H14C 0.9600 . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Cu1 N2 C6 C7 -178.3(4) . . . . Cu1 N3 C11 C10 -179.7(5) 1_565 . . . Cu1 N1 C1 C2 176.3(4) . . . . Cu1 N1 C5 C4 -176.2(4) . . . . N1 C1 C2 C3 -0.7(9) . . . . N1 C5 C4 C3 0.5(9) . . . . C9 C8 C7 C6 -178.4(4) . . . . C9 C10 C11 N3 -0.7(9) . . . . C8 C9 C10 C11 -179.7(4) . . . . C8 C7 C6 N2 -3.4(8) . . . . C10 C9 C8 C7 132.0(4) 2_655 . . . C10 C9 C8 C7 -48.0(4) 2_655 . . 2_655 C10 C9 C8 C7 -48.0(4) . . . . C10 C9 C8 C7 131.9(4) . . . 2_655 C10 C9 C10 C11 0.3(4) 2_655 . . . C1 N1 C5 C4 1.6(9) . . . . C3 C3 C2 C1 -178.2(6) 5_655 . . . C3 C3 C4 C5 178.3(6) 5_655 . . . C5 N1 C1 C2 -1.5(9) . . . . C2 C3 C4 C5 -2.6(8) . . . . C4 C3 C2 C1 2.7(8) . . . . C11 N3 C11 C10 0.3(5) 2_655 . . . C7 C8 C7 C6 1.6(4) 2_655 . . . C6 N2 C6 C7 1.7(4) 2_655 . . . C15 N4 C12 O2 4.9(12) . . . . C15 N4 C12 C13 -174.2(8) . . . . C14 N4 C12 O2 178.4(7) . . . . C14 N4 C12 C13 -0.7(12) . . . . loop_ _diffrn_oxdiff_twin_id _diffrn_oxdiff_twin_ratio _diffrn_oxdiff_twin_reflns_isolated _diffrn_oxdiff_twin_reflns_overlapped 1 0.5796 1446 7359 2 0.4204 1448 7359