Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Randolf D. Kohn' 'Garbriele I. Kociok-Kohn' 'M. Mahon' 'Zhida Pan' _publ_contact_author_name 'Dr Randolf D. Kohn' _publ_contact_author_address ; Department of Chemistry University of Bath Claverton Down Bath BA2 7AY UNITED KINGDOM ; _publ_contact_author_email R.D.KOHN@BATH.AC.UK _publ_section_title ; Coordination chemistry of copper(I) and (II) with 2-pyridylmethyl substituted triazacyclohexanes ; #============================================================================== data_pan22 _database_code_CSD 204540 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H97 B4 Cu4 F16 N17 O5' _chemical_formula_weight 1665.89 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' B B 0.0013 0.0007 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 14.9710(2) _cell_length_b 14.4640(2) _cell_length_c 16.7010(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.8570(10) _cell_angle_gamma 90.00 _cell_volume 3616.04(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 38042 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour turquoise _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 1.258 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method \f-rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45486 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8281 _reflns_number_gt 7291 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius program suite version 1.9 (1997)' _computing_cell_refinement 'Collect, Nonius program suite version 1.9 (1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement ; SHELX97-2 Program for Crystal Structure Analysis. G. M. Sheldrick, Institut f. Anorg. Chemie der Universitat, Tammanstrasse 4, D-3400 Gottingen, Germany, 1998. ; _computing_molecular_graphics 'ORTEP3 for Windows - L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material 'SHELX97-2, G. M. Sheldrick' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+3.9910P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8281 _refine_ls_number_parameters 485 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0859 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.245203(15) 0.157634(16) 0.155913(13) 0.01660(7) Uani 1 1 d . . . Cu2 Cu 0.354003(15) 0.304151(16) 0.247436(13) 0.01709(7) Uani 1 1 d . . . O1 O 0.34662(9) 0.17076(9) 0.26213(8) 0.0175(3) Uani 1 1 d . . . H1 H 0.4019 0.1320 0.2641 0.021 Uiso 1 1 calc R . . O2 O 0.26140(9) 0.29051(9) 0.16368(8) 0.0178(3) Uani 1 1 d . . . H2 H 0.2628 0.3295 0.1143 0.021 Uiso 1 1 calc R . . C1 C 0.39543(14) 0.20904(15) 0.04499(13) 0.0243(4) Uani 1 1 d . . . H1A H 0.4328 0.2170 0.0939 0.029 Uiso 1 1 calc R . . H1B H 0.4346 0.1892 0.0009 0.029 Uiso 1 1 calc R . . N1 N 0.32610(11) 0.13795(12) 0.05893(10) 0.0201(3) Uani 1 1 d . . . C11 C 0.37028(14) 0.04826(15) 0.07586(13) 0.0251(4) Uani 1 1 d . . . H11A H 0.4185 0.0568 0.1164 0.030 Uiso 1 1 calc R . . H11B H 0.3971 0.0237 0.0264 0.030 Uiso 1 1 calc R . . C12 C 0.30190(14) -0.01861(15) 0.10654(12) 0.0228(4) Uani 1 1 d . . . C13 C 0.30551(17) -0.11348(16) 0.09514(13) 0.0300(5) Uani 1 1 d . . . H13 H 0.3537 -0.1405 0.0671 0.036 Uiso 1 1 calc R . . C14 C 0.23822(18) -0.16819(16) 0.12507(15) 0.0342(5) Uani 1 1 d . . . H14 H 0.2391 -0.2332 0.1171 0.041 Uiso 1 1 calc R . . C15 C 0.16928(16) -0.12712(16) 0.16697(14) 0.0301(5) Uani 1 1 d . . . H15 H 0.1224 -0.1636 0.1880 0.036 Uiso 1 1 calc R . . C16 C 0.17006(14) -0.03254(15) 0.17748(12) 0.0234(4) Uani 1 1 d . . . H16 H 0.1236 -0.0044 0.2070 0.028 Uiso 1 1 calc R . . N11 N 0.23480(11) 0.02098(12) 0.14705(10) 0.0204(3) Uani 1 1 d . . . C2 C 0.27041(15) 0.12921(16) -0.01535(12) 0.0249(4) Uani 1 1 d . . . H2A H 0.3086 0.1127 -0.0611 0.030 Uiso 1 1 calc R . . H2B H 0.2255 0.0797 -0.0087 0.030 Uiso 1 1 calc R . . N2 N 0.22600(13) 0.21666(14) -0.03092(11) 0.0282(4) Uani 1 1 d . . . C21 C 0.16509(19) 0.2055(2) -0.10119(15) 0.0437(7) Uani 1 1 d . . . H21A H 0.1320 0.1466 -0.0957 0.052 Uiso 1 1 calc R . . H21B H 0.2014 0.2012 -0.1501 0.052 Uiso 1 1 calc R . . C22 C 0.0995(2) 0.2822(3) -0.1114(2) 0.0585(8) Uani 1 1 d . . . H22A H 0.0615 0.2702 -0.1585 0.088 Uiso 1 1 calc R . . H22B H 0.1315 0.3406 -0.1186 0.088 Uiso 1 1 calc R . . H22C H 0.0623 0.2863 -0.0637 0.088 Uiso 1 1 calc R . . N3 N 0.35205(13) 0.29626(13) 0.02419(11) 0.0265(4) Uani 1 1 d . . . C3 C 0.29452(17) 0.28671(17) -0.04681(13) 0.0319(5) Uani 1 1 d . . . H3A H 0.3305 0.2678 -0.0933 0.038 Uiso 1 1 calc R . . H3B H 0.2658 0.3467 -0.0596 0.038 Uiso 1 1 calc R . . C31 C 0.41797(19) 0.37228(18) 0.01800(16) 0.0391(6) Uani 1 1 d . . . H31A H 0.4452 0.3823 0.0717 0.047 Uiso 1 1 calc R . . H31B H 0.3853 0.4295 0.0033 0.047 Uiso 1 1 calc R . . C32 C 0.4934(2) 0.3589(2) -0.0417(2) 0.0642(10) Uani 1 1 d . . . H32A H 0.5325 0.4132 -0.0406 0.096 Uiso 1 1 calc R . . H32B H 0.4679 0.3510 -0.0956 0.096 Uiso 1 1 calc R . . H32C H 0.5280 0.3038 -0.0270 0.096 Uiso 1 1 calc R . . C4 C 0.48582(14) 0.25563(15) 0.38164(12) 0.0249(4) Uani 1 1 d . . . H4A H 0.5370 0.2768 0.4151 0.030 Uiso 1 1 calc R . . H4B H 0.4338 0.2468 0.4167 0.030 Uiso 1 1 calc R . . N4 N 0.46458(11) 0.32581(12) 0.31916(10) 0.0216(3) Uani 1 1 d . . . C41 C 0.44608(16) 0.41571(16) 0.35885(13) 0.0287(5) Uani 1 1 d . . . H41A H 0.5018 0.4412 0.3827 0.034 Uiso 1 1 calc R . . H41B H 0.4025 0.4069 0.4022 0.034 Uiso 1 1 calc R . . C42 C 0.40899(14) 0.48122(15) 0.29703(13) 0.0258(4) Uani 1 1 d . . . C43 C 0.42116(18) 0.57590(17) 0.29973(16) 0.0356(5) Uani 1 1 d . . . H43 H 0.4531 0.6037 0.3430 0.043 Uiso 1 1 calc R . . C44 C 0.38606(19) 0.62953(17) 0.23838(17) 0.0394(6) Uani 1 1 d . . . H44 H 0.3948 0.6946 0.2386 0.047 Uiso 1 1 calc R . . C45 C 0.33809(17) 0.58792(16) 0.17667(15) 0.0329(5) Uani 1 1 d . . . H45 H 0.3135 0.6238 0.1341 0.039 Uiso 1 1 calc R . . C46 C 0.32679(15) 0.49331(15) 0.17834(13) 0.0252(4) Uani 1 1 d . . . H46 H 0.2930 0.4644 0.1368 0.030 Uiso 1 1 calc R . . N41 N 0.36230(11) 0.44076(12) 0.23714(10) 0.0218(3) Uani 1 1 d . . . C5 C 0.54386(14) 0.33514(16) 0.26718(13) 0.0253(4) Uani 1 1 d . . . H5A H 0.5332 0.3841 0.2268 0.030 Uiso 1 1 calc R . . H5B H 0.5969 0.3526 0.3000 0.030 Uiso 1 1 calc R . . N5 N 0.55968(12) 0.24740(14) 0.22754(11) 0.0258(4) Uani 1 1 d . . . C51 C 0.63179(16) 0.2600(2) 0.16920(15) 0.0359(5) Uani 1 1 d . . . H51A H 0.6874 0.2772 0.1983 0.043 Uiso 1 1 calc R . . H51B H 0.6158 0.3116 0.1328 0.043 Uiso 1 1 calc R . . C52 C 0.64918(19) 0.1738(2) 0.11946(17) 0.0490(7) Uani 1 1 d . . . H52A H 0.6975 0.1861 0.0820 0.073 Uiso 1 1 calc R . . H52B H 0.5948 0.1571 0.0894 0.073 Uiso 1 1 calc R . . H52C H 0.6665 0.1226 0.1550 0.073 Uiso 1 1 calc R . . C6 C 0.58359(14) 0.17839(17) 0.28872(13) 0.0278(5) Uani 1 1 d . . . H6A H 0.5968 0.1183 0.2631 0.033 Uiso 1 1 calc R . . H6B H 0.6373 0.1987 0.3192 0.033 Uiso 1 1 calc R . . N6 N 0.50798(12) 0.16872(13) 0.34251(11) 0.0242(4) Uani 1 1 d . . . C61 C 0.51988(16) 0.09288(17) 0.40093(14) 0.0325(5) Uani 1 1 d . . . H61A H 0.5272 0.0345 0.3709 0.039 Uiso 1 1 calc R . . H61B H 0.4643 0.0874 0.4320 0.039 Uiso 1 1 calc R . . C62 C 0.5981(2) 0.1021(2) 0.45980(18) 0.0506(8) Uani 1 1 d . . . H62A H 0.5997 0.0482 0.4954 0.076 Uiso 1 1 calc R . . H62B H 0.5909 0.1584 0.4917 0.076 Uiso 1 1 calc R . . H62C H 0.6541 0.1055 0.4302 0.076 Uiso 1 1 calc R . . B1 B 0.53934(19) -0.1025(2) 0.18559(17) 0.0362(6) Uani 1 1 d . . . F1 F 0.62835(13) -0.1184(2) 0.20064(12) 0.0783(7) Uani 1 1 d . . . F2 F 0.52668(12) -0.08354(14) 0.10475(10) 0.0554(5) Uani 1 1 d . . . F3 F 0.48926(17) -0.17844(15) 0.20485(16) 0.0801(7) Uani 1 1 d . . . F4 F 0.50888(13) -0.02653(15) 0.22801(12) 0.0641(5) Uani 1 1 d . . . B2 B 0.1934(3) 0.5783(3) -0.0193(2) 0.0563(9) Uani 1 1 d D . . F5 F 0.17707(18) 0.5638(2) -0.09794(12) 0.0944(9) Uani 1 1 d . A . F6 F 0.20874(16) 0.49817(15) 0.02161(12) 0.0707(6) Uani 1 1 d . A . F7 F 0.2898(9) 0.594(2) -0.0243(13) 0.185(12) Uani 0.362(17) 1 d PD A 1 F8 F 0.1568(17) 0.6454(8) 0.0157(8) 0.145(8) Uani 0.362(17) 1 d PD A 1 F7A F 0.2492(7) 0.6483(4) -0.0015(4) 0.108(3) Uani 0.638(17) 1 d PD A 2 F8A F 0.1061(5) 0.6038(8) 0.0099(3) 0.113(4) Uani 0.638(17) 1 d PD A 2 C8 C 0.6147(9) 0.5293(8) 0.1832(8) 0.120(6) Uani 0.50 1 d PD . . H8A H 0.5683 0.5174 0.2228 0.179 Uiso 0.50 1 calc PR . . H8B H 0.6184 0.4767 0.1465 0.179 Uiso 0.50 1 calc PR . . H8C H 0.5996 0.5853 0.1529 0.179 Uiso 0.50 1 calc PR . . C7 C 0.6953(14) 0.5411(10) 0.2217(11) 0.170(13) Uani 0.50 1 d PD . . N7 N 0.759(3) 0.5546(16) 0.261(3) 0.305(16) Uani 0.50 1 d PD . . O3 O 0.7500 0.0049(7) 0.2500 0.385(13) Uani 1 2 d S . . 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 0.01750(12) 0.01573(12) 0.01663(12) -0.00125(8) 0.00187(8) -0.00036(8) Cu2 0.01774(12) 0.01571(12) 0.01780(12) 0.00040(8) -0.00060(9) -0.00189(8) O1 0.0164(6) 0.0174(6) 0.0187(6) 0.0010(5) 0.0014(5) 0.0000(5) O2 0.0194(6) 0.0170(6) 0.0170(6) -0.0001(5) 0.0010(5) -0.0004(5) C1 0.0204(9) 0.0277(11) 0.0249(10) -0.0010(8) 0.0071(8) -0.0023(8) N1 0.0200(8) 0.0211(8) 0.0192(8) -0.0001(6) 0.0017(6) 0.0007(7) C11 0.0232(10) 0.0248(10) 0.0274(10) -0.0008(8) 0.0048(8) 0.0060(8) C12 0.0264(10) 0.0236(10) 0.0183(9) -0.0013(8) -0.0008(7) 0.0048(8) C13 0.0382(12) 0.0242(11) 0.0276(11) -0.0047(9) 0.0001(9) 0.0087(9) C14 0.0463(14) 0.0193(10) 0.0367(12) -0.0014(9) -0.0065(11) 0.0023(10) C15 0.0362(12) 0.0228(11) 0.0311(11) 0.0038(9) -0.0040(9) -0.0046(9) C16 0.0270(10) 0.0221(10) 0.0211(9) 0.0003(8) -0.0006(8) -0.0024(8) N11 0.0240(8) 0.0191(8) 0.0181(7) -0.0018(6) 0.0011(6) -0.0002(7) C2 0.0274(10) 0.0297(11) 0.0175(9) -0.0025(8) 0.0007(8) 0.0009(9) N2 0.0303(9) 0.0329(10) 0.0213(8) 0.0008(7) -0.0029(7) 0.0047(8) C21 0.0428(14) 0.0590(18) 0.0290(12) -0.0051(12) -0.0127(11) 0.0125(13) C22 0.0557(19) 0.072(2) 0.0478(17) 0.0072(16) -0.0117(14) 0.0168(17) N3 0.0293(9) 0.0249(9) 0.0255(9) 0.0040(7) 0.0074(7) -0.0023(7) C3 0.0431(13) 0.0325(12) 0.0202(10) 0.0053(9) 0.0051(9) 0.0032(10) C31 0.0464(15) 0.0291(12) 0.0424(14) 0.0007(10) 0.0177(11) -0.0109(11) C32 0.068(2) 0.058(2) 0.068(2) -0.0131(16) 0.0432(18) -0.0286(17) C4 0.0262(10) 0.0293(11) 0.0189(9) 0.0007(8) -0.0038(8) -0.0009(8) N4 0.0212(8) 0.0240(9) 0.0195(8) -0.0017(7) -0.0013(6) -0.0012(7) C41 0.0332(11) 0.0267(11) 0.0261(10) -0.0075(9) -0.0038(9) -0.0012(9) C42 0.0262(10) 0.0236(10) 0.0278(10) -0.0047(8) 0.0036(8) -0.0039(8) C43 0.0421(14) 0.0241(11) 0.0407(13) -0.0112(10) 0.0035(11) -0.0064(10) C44 0.0511(15) 0.0169(11) 0.0506(15) -0.0029(10) 0.0132(12) -0.0053(10) C45 0.0400(13) 0.0214(11) 0.0377(12) 0.0056(9) 0.0137(10) 0.0036(9) C46 0.0285(10) 0.0205(10) 0.0267(10) 0.0031(8) 0.0058(8) 0.0013(8) N41 0.0226(8) 0.0186(8) 0.0244(8) -0.0012(7) 0.0024(7) -0.0027(7) C5 0.0188(9) 0.0295(11) 0.0276(10) 0.0014(8) -0.0005(8) -0.0052(8) N5 0.0205(8) 0.0332(10) 0.0236(9) 0.0000(7) 0.0016(7) -0.0001(7) C51 0.0236(11) 0.0530(16) 0.0312(12) 0.0011(11) 0.0061(9) -0.0002(10) C52 0.0365(14) 0.072(2) 0.0389(14) -0.0098(14) 0.0099(11) 0.0094(14) C6 0.0187(9) 0.0351(12) 0.0294(11) 0.0001(9) -0.0023(8) 0.0031(8) N6 0.0221(8) 0.0267(9) 0.0236(8) 0.0018(7) -0.0025(7) 0.0010(7) C61 0.0326(12) 0.0320(12) 0.0326(12) 0.0081(9) -0.0067(9) 0.0004(10) C62 0.0537(17) 0.0493(17) 0.0479(16) 0.0182(13) -0.0264(14) -0.0060(14) B1 0.0327(13) 0.0445(16) 0.0317(13) -0.0039(12) 0.0073(11) 0.0026(12) F1 0.0402(10) 0.146(2) 0.0486(11) 0.0029(12) -0.0020(8) 0.0192(12) F2 0.0553(10) 0.0743(13) 0.0367(8) 0.0012(8) 0.0072(7) 0.0289(9) F3 0.0897(16) 0.0521(12) 0.0991(18) 0.0077(11) 0.0252(14) -0.0145(11) F4 0.0632(12) 0.0676(13) 0.0623(11) -0.0337(10) 0.0244(9) -0.0109(10) B2 0.078(3) 0.055(2) 0.0360(16) 0.0091(15) -0.0117(17) 0.0111(19) F5 0.1065(19) 0.140(2) 0.0359(10) -0.0006(12) -0.0168(11) 0.0487(17) F6 0.0866(15) 0.0645(13) 0.0605(12) 0.0172(10) -0.0149(11) 0.0127(11) F7 0.091(8) 0.26(2) 0.206(16) 0.175(17) -0.062(9) -0.093(11) F8 0.22(2) 0.064(7) 0.148(11) -0.037(6) -0.030(12) 0.051(10) F7A 0.177(8) 0.062(3) 0.085(3) 0.005(3) -0.027(4) -0.028(4) F8A 0.097(4) 0.186(8) 0.056(3) 0.026(3) 0.013(2) 0.087(4) C8 0.122(9) 0.090(8) 0.149(11) 0.085(8) 0.076(9) 0.035(7) C7 0.27(2) 0.046(6) 0.20(2) 0.059(10) 0.21(2) 0.061(10) N7 0.61(5) 0.170(17) 0.15(2) -0.07(3) 0.19(2) -0.04(5) O3 0.256(13) 0.140(9) 0.75(4) 0.000 -0.252(18) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O2 1.9412(14) . ? Cu1 O1 1.9635(13) 2 ? Cu1 N11 1.9881(17) . ? Cu1 N1 2.0567(17) . ? Cu1 O1 2.3254(13) . ? Cu2 O1 1.9483(14) . ? Cu2 O2 1.9646(13) . ? Cu2 N41 1.9874(18) . ? Cu2 N4 2.0529(17) . ? Cu2 O2 2.3032(13) 2 ? O1 Cu1 1.9635(13) 2 ? O1 H1 1.0000 . ? O2 Cu2 2.3032(13) 2 ? O2 H2 1.0000 . ? C1 N3 1.458(3) . ? C1 N1 1.482(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? N1 C11 1.481(3) . ? N1 C2 1.490(3) . ? C11 C12 1.504(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N11 1.347(3) . ? C12 C13 1.387(3) . ? C13 C14 1.381(4) . ? C13 H13 0.9500 . ? C14 C15 1.389(4) . ? C14 H14 0.9500 . ? C15 C16 1.379(3) . ? C15 H15 0.9500 . ? C16 N11 1.346(3) . ? C16 H16 0.9500 . ? C2 N2 1.451(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N2 C3 1.469(3) . ? N2 C21 1.484(3) . ? C21 C22 1.490(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? N3 C3 1.462(3) . ? N3 C31 1.482(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C31 C32 1.529(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C4 N6 1.457(3) . ? C4 N4 1.487(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N4 C5 1.487(3) . ? N4 C41 1.488(3) . ? C41 C42 1.502(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 N41 1.346(3) . ? C42 C43 1.382(3) . ? C43 C44 1.383(4) . ? C43 H43 0.9500 . ? C44 C45 1.385(4) . ? C44 H44 0.9500 . ? C45 C46 1.379(3) . ? C45 H45 0.9500 . ? C46 N41 1.345(3) . ? C46 H46 0.9500 . ? C5 N5 1.452(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? N5 C6 1.469(3) . ? N5 C51 1.476(3) . ? C51 C52 1.523(4) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C6 N6 1.462(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? N6 C61 1.477(3) . ? C61 C62 1.524(3) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? B1 F3 1.371(4) . ? B1 F1 1.372(3) . ? B1 F2 1.388(3) . ? B1 F4 1.388(3) . ? B2 F8 1.262(12) . ? B2 F7A 1.343(7) . ? B2 F5 1.349(4) . ? B2 F6 1.363(4) . ? B2 F8A 1.448(6) . ? B2 F7 1.465(11) . ? C8 C7 1.37(2) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C7 N7 0.77(6) 2_655 ? C7 N7 1.16(2) . ? C7 C7 1.88(5) 2_655 ? N7 N7 0.43(7) 2_655 ? N7 C7 0.77(6) 2_655 ? 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 O2 Cu1 O1 86.89(6) . 2 ? O2 Cu1 N11 177.28(6) . . ? O1 Cu1 N11 95.34(6) 2 . ? O2 Cu1 N1 96.62(6) . . ? O1 Cu1 N1 171.49(6) 2 . ? N11 Cu1 N1 81.38(7) . . ? O2 Cu1 O1 77.80(5) . . ? O1 Cu1 O1 85.20(5) 2 . ? N11 Cu1 O1 100.80(6) . . ? N1 Cu1 O1 103.10(6) . . ? O1 Cu2 O2 87.10(6) . . ? O1 Cu2 N41 177.71(6) . . ? O2 Cu2 N41 94.74(6) . . ? O1 Cu2 N4 97.14(6) . . ? O2 Cu2 N4 170.10(6) . . ? N41 Cu2 N4 81.25(7) . . ? O1 Cu2 O2 77.84(5) . 2 ? O2 Cu2 O2 85.54(5) . 2 ? N41 Cu2 O2 100.92(6) . 2 ? N4 Cu2 O2 104.07(6) . 2 ? Cu2 O1 Cu1 103.01(6) . 2 ? Cu2 O1 Cu1 91.28(5) . . ? Cu1 O1 Cu1 93.90(5) 2 . ? Cu2 O1 H1 120.7 . . ? Cu1 O1 H1 120.7 2 . ? Cu1 O1 H1 120.7 . . ? Cu1 O2 Cu2 103.48(6) . . ? Cu1 O2 Cu2 91.93(5) . 2 ? Cu2 O2 Cu2 93.48(5) . 2 ? Cu1 O2 H2 120.5 . . ? Cu2 O2 H2 120.5 . . ? Cu2 O2 H2 120.5 2 . ? N3 C1 N1 109.10(17) . . ? N3 C1 H1A 109.9 . . ? N1 C1 H1A 109.9 . . ? N3 C1 H1B 109.9 . . ? N1 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? C11 N1 C1 109.02(16) . . ? C11 N1 C2 109.11(16) . . ? C1 N1 C2 108.21(16) . . ? C11 N1 Cu1 103.74(12) . . ? C1 N1 Cu1 116.73(13) . . ? C2 N1 Cu1 109.80(12) . . ? N1 C11 C12 108.90(16) . . ? N1 C11 H11A 109.9 . . ? C12 C11 H11A 109.9 . . ? N1 C11 H11B 109.9 . . ? C12 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? N11 C12 C13 121.4(2) . . ? N11 C12 C11 114.48(18) . . ? C13 C12 C11 124.2(2) . . ? C14 C13 C12 119.2(2) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 119.3(2) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C16 C15 C14 118.9(2) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? N11 C16 C15 121.8(2) . . ? N11 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C16 N11 C12 119.46(19) . . ? C16 N11 Cu1 126.85(14) . . ? C12 N11 Cu1 113.68(14) . . ? N2 C2 N1 108.95(17) . . ? N2 C2 H2A 109.9 . . ? N1 C2 H2A 109.9 . . ? N2 C2 H2B 109.9 . . ? N1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C2 N2 C3 108.32(18) . . ? C2 N2 C21 108.76(19) . . ? C3 N2 C21 110.8(2) . . ? N2 C21 C22 113.9(2) . . ? N2 C21 H21A 108.8 . . ? C22 C21 H21A 108.8 . . ? N2 C21 H21B 108.8 . . ? C22 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C1 N3 C3 111.49(18) . . ? C1 N3 C31 111.33(19) . . ? C3 N3 C31 113.47(19) . . ? N3 C3 N2 108.86(17) . . ? N3 C3 H3A 109.9 . . ? N2 C3 H3A 109.9 . . ? N3 C3 H3B 109.9 . . ? N2 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? N3 C31 C32 116.8(2) . . ? N3 C31 H31A 108.1 . . ? C32 C31 H31A 108.1 . . ? N3 C31 H31B 108.1 . . ? C32 C31 H31B 108.1 . . ? H31A C31 H31B 107.3 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N6 C4 N4 108.77(16) . . ? N6 C4 H4A 109.9 . . ? N4 C4 H4A 109.9 . . ? N6 C4 H4B 109.9 . . ? N4 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? C4 N4 C5 107.92(16) . . ? C4 N4 C41 108.86(16) . . ? C5 N4 C41 109.65(17) . . ? C4 N4 Cu2 117.87(13) . . ? C5 N4 Cu2 108.48(12) . . ? C41 N4 Cu2 103.86(13) . . ? N4 C41 C42 108.34(17) . . ? N4 C41 H41A 110.0 . . ? C42 C41 H41A 110.0 . . ? N4 C41 H41B 110.0 . . ? C42 C41 H41B 110.0 . . ? H41A C41 H41B 108.4 . . ? N41 C42 C43 121.5(2) . . ? N41 C42 C41 114.79(19) . . ? C43 C42 C41 123.7(2) . . ? C42 C43 C44 118.9(2) . . ? C42 C43 H43 120.5 . . ? C44 C43 H43 120.5 . . ? C43 C44 C45 119.7(2) . . ? C43 C44 H44 120.2 . . ? C45 C44 H44 120.2 . . ? C46 C45 C44 118.6(2) . . ? C46 C45 H45 120.7 . . ? C44 C45 H45 120.7 . . ? N41 C46 C45 121.9(2) . . ? N41 C46 H46 119.1 . . ? C45 C46 H46 119.1 . . ? C46 N41 C42 119.49(19) . . ? C46 N41 Cu2 126.91(15) . . ? C42 N41 Cu2 113.61(14) . . ? N5 C5 N4 108.89(17) . . ? N5 C5 H5A 109.9 . . ? N4 C5 H5A 109.9 . . ? N5 C5 H5B 109.9 . . ? N4 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? C5 N5 C6 108.44(17) . . ? C5 N5 C51 108.61(19) . . ? C6 N5 C51 111.70(18) . . ? N5 C51 C52 113.1(2) . . ? N5 C51 H51A 109.0 . . ? C52 C51 H51A 109.0 . . ? N5 C51 H51B 109.0 . . ? C52 C51 H51B 109.0 . . ? H51A C51 H51B 107.8 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N6 C6 N5 108.03(17) . . ? N6 C6 H6A 110.1 . . ? N5 C6 H6A 110.1 . . ? N6 C6 H6B 110.1 . . ? N5 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? C4 N6 C6 112.11(18) . . ? C4 N6 C61 111.74(18) . . ? C6 N6 C61 112.95(18) . . ? N6 C61 C62 116.5(2) . . ? N6 C61 H61A 108.2 . . ? C62 C61 H61A 108.2 . . ? N6 C61 H61B 108.2 . . ? C62 C61 H61B 108.2 . . ? H61A C61 H61B 107.3 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? F3 B1 F1 110.8(3) . . ? F3 B1 F2 108.6(3) . . ? F1 B1 F2 109.2(2) . . ? F3 B1 F4 109.2(2) . . ? F1 B1 F4 111.4(3) . . ? F2 B1 F4 107.4(2) . . ? F8 B2 F7A 65.9(10) . . ? F8 B2 F5 119.8(8) . . ? F7A B2 F5 115.8(4) . . ? F8 B2 F6 119.6(8) . . ? F7A B2 F6 115.5(4) . . ? F5 B2 F6 112.5(3) . . ? F8 B2 F8A 41.3(9) . . ? F7A B2 F8A 107.2(6) . . ? F5 B2 F8A 102.5(4) . . ? F6 B2 F8A 101.2(4) . . ? F8 B2 F7 110.0(11) . . ? F7A B2 F7 44.4(11) . . ? F5 B2 F7 97.6(10) . . ? F6 B2 F7 90.1(7) . . ? F8A B2 F7 150.9(12) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N7 C7 N7 12(6) 2_655 . ? N7 C7 C8 171(3) 2_655 . ? N7 C7 C8 173(3) . . ? N7 C7 C7 16(2) 2_655 2_655 ? N7 C7 C7 10.6(18) . 2_655 ? C8 C7 C7 172.6(8) . 2_655 ? N7 N7 C7 146(10) 2_655 2_655 ? N7 N7 C7 22(10) 2_655 . ? C7 N7 C7 153(4) 2_655 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.939 _refine_diff_density_min -0.661 _refine_diff_density_rms 0.068 #============================================================================== data_pan13 _database_code_CSD 204541 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H55 Cl8 Cu2 N9' _chemical_formula_weight 952.51 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' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 9.3710(2) _cell_length_b 23.2990(5) _cell_length_c 9.9180(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.7720(10) _cell_angle_gamma 90.00 _cell_volume 2119.90(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 73452 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 25.03 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 1.542 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4434 _exptl_absorpt_correction_T_max 0.7480 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method \f-rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 27101 _diffrn_reflns_av_R_equivalents 0.1042 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 25.08 _reflns_number_total 3732 _reflns_number_gt 3317 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius program suite version 1.9 (1997)' _computing_cell_refinement 'Collect, Nonius program suite version 1.9 (1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement ; SHELX97-2 Program for Crystal Structure Analysis. G. M. Sheldrick, Institut f. Anorg. Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998. ; _computing_molecular_graphics 'ORTEP3 for Windows - L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material 'SHELX97-2, G. M. Sheldrick' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1111P)^2^+14.4743P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3732 _refine_ls_number_parameters 220 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0903 _refine_ls_R_factor_gt 0.0818 _refine_ls_wR_factor_ref 0.2164 _refine_ls_wR_factor_gt 0.2091 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.92165(7) 0.05446(3) 0.38627(7) 0.0231(3) Uani 1 1 d . . . Cl1 Cl 1.00999(16) -0.03498(6) 0.34757(14) 0.0274(4) Uani 1 1 d . . . Cl2 Cl 1.11268(17) 0.09901(7) 0.32723(18) 0.0332(4) Uani 1 1 d . . . C1 C 0.7765(7) 0.1614(3) 0.2832(6) 0.0281(13) Uani 1 1 d . . . H1A H 0.8633 0.1701 0.2443 0.034 Uiso 1 1 calc R . . H1B H 0.7122 0.1356 0.2184 0.034 Uiso 1 1 calc R . . N1 N 0.8224(5) 0.1324(2) 0.4189(5) 0.0229(10) Uani 1 1 d . . . C11 C 0.6933(7) 0.1163(3) 0.4756(7) 0.0287(13) Uani 1 1 d . . . H11A H 0.6240 0.1488 0.4658 0.034 Uiso 1 1 calc R . . H11B H 0.7238 0.1072 0.5748 0.034 Uiso 1 1 calc R . . C12 C 0.6205(7) 0.0650(3) 0.3996(7) 0.0322(14) Uani 1 1 d . . . C13 C 0.4727(8) 0.0565(3) 0.3733(9) 0.0412(17) Uani 1 1 d . . . H13 H 0.4106 0.0845 0.4010 0.049 Uiso 1 1 calc R . . C14 C 0.4145(8) 0.0077(3) 0.3071(10) 0.055(2) Uani 1 1 d . . . H14 H 0.3122 0.0014 0.2874 0.066 Uiso 1 1 calc R . . C15 C 0.5098(9) -0.0329(3) 0.2690(11) 0.059(2) Uani 1 1 d . . . H15 H 0.4734 -0.0675 0.2242 0.070 Uiso 1 1 calc R . . C16 C 0.6570(8) -0.0215(3) 0.2980(9) 0.0453(18) Uani 1 1 d . . . H16 H 0.7214 -0.0490 0.2724 0.054 Uiso 1 1 calc R . . N4 N 0.7132(6) 0.0267(2) 0.3606(6) 0.0302(12) Uani 1 1 d . . . C2 C 0.9175(7) 0.1724(2) 0.5126(6) 0.0263(13) Uani 1 1 d . . . H2A H 0.9504 0.1541 0.6037 0.032 Uiso 1 1 calc R . . H2B H 1.0048 0.1816 0.4748 0.032 Uiso 1 1 calc R . . N2 N 0.8374(6) 0.2254(2) 0.5283(5) 0.0294(12) Uani 1 1 d . . . C21 C 0.9294(8) 0.2628(3) 0.6280(7) 0.0375(16) Uani 1 1 d . . . H21A H 1.0093 0.2783 0.5870 0.045 Uiso 1 1 calc R . . H21B H 0.9737 0.2401 0.7103 0.045 Uiso 1 1 calc R . . C22 C 0.8431(10) 0.3126(3) 0.6717(9) 0.055(2) Uani 1 1 d . . . H22A H 0.9088 0.3373 0.7366 0.083 Uiso 1 1 calc R . . H22B H 0.7666 0.2976 0.7162 0.083 Uiso 1 1 calc R . . H22C H 0.7985 0.3351 0.5904 0.083 Uiso 1 1 calc R . . C3 C 0.7956(8) 0.2526(3) 0.3929(7) 0.0336(15) Uani 1 1 d . . . H3A H 0.7451 0.2893 0.4014 0.040 Uiso 1 1 calc R . . H3B H 0.8838 0.2608 0.3557 0.040 Uiso 1 1 calc R . . N3 N 0.6992(6) 0.2143(2) 0.2996(6) 0.0318(12) Uani 1 1 d . . . C32 C 0.5263(10) 0.2066(4) 0.0753(9) 0.061(2) Uani 1 1 d . . . H32A H 0.4921 0.2270 -0.0117 0.092 Uiso 1 1 calc R . . H32B H 0.4444 0.2007 0.1214 0.092 Uiso 1 1 calc R . . H32C H 0.5668 0.1694 0.0567 0.092 Uiso 1 1 calc R . . C31 C 0.6417(9) 0.2415(4) 0.1662(8) 0.0475(19) Uani 1 1 d . . . H31A H 0.7230 0.2479 0.1180 0.057 Uiso 1 1 calc R . . H31B H 0.6007 0.2794 0.1822 0.057 Uiso 1 1 calc R . . C4 C 0.0706(13) -0.0901(4) 0.0293(12) 0.146(8) Uani 1 1 d D . . H4A H 0.0210 -0.0695 0.0939 0.176 Uiso 1 1 calc R . . H4B H -0.0037 -0.1022 -0.0516 0.176 Uiso 1 1 calc R . . Cl3 Cl 0.2041(5) -0.04441(16) -0.0236(3) 0.1106(13) Uani 1 1 d D . . Cl4 Cl 0.1642(6) -0.15035(16) 0.1106(4) 0.1245(16) Uani 1 1 d D . . N5 N 0.1841(12) 0.1340(5) -0.0588(11) 0.031(2) Uiso 0.50 1 d P . . H5A H 0.2115 0.1694 -0.0716 0.037 Uiso 0.50 1 calc PR . . H5B H 0.0912 0.1247 -0.0800 0.037 Uiso 0.50 1 calc PR . . C5 C 0.3004(17) 0.0878(7) 0.0015(16) 0.043(3) Uiso 0.50 1 d P . . H5C H 0.2814 0.0567 -0.0678 0.052 Uiso 0.50 1 calc PR . . H5D H 0.2646 0.0728 0.0820 0.052 Uiso 0.50 1 calc PR . . C6 C 0.470(8) 0.086(4) 0.051(9) 0.33(4) Uiso 0.50 1 d P . . H6A H 0.5000 0.0477 0.0879 0.493 Uiso 0.50 1 calc PR . . H6B H 0.5005 0.1147 0.1237 0.493 Uiso 0.50 1 calc PR . . H6C H 0.5171 0.0942 -0.0264 0.493 Uiso 0.50 1 calc PR . . 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 Cu 0.0203(4) 0.0231(4) 0.0274(4) -0.0013(3) 0.0083(3) 0.0022(3) Cl1 0.0305(8) 0.0275(8) 0.0252(7) -0.0029(6) 0.0086(6) 0.0064(6) Cl2 0.0239(8) 0.0321(8) 0.0475(9) -0.0015(7) 0.0164(7) 0.0000(6) C1 0.032(3) 0.028(3) 0.026(3) 0.000(2) 0.010(3) 0.006(2) N1 0.018(2) 0.024(2) 0.027(3) 0.0004(19) 0.006(2) 0.0025(19) C11 0.025(3) 0.028(3) 0.037(3) -0.001(3) 0.015(3) 0.001(2) C12 0.030(3) 0.029(3) 0.042(4) 0.002(3) 0.015(3) 0.005(3) C13 0.025(4) 0.036(4) 0.064(5) -0.004(3) 0.013(3) 0.002(3) C14 0.019(4) 0.047(4) 0.097(7) -0.013(4) 0.008(4) -0.006(3) C15 0.033(4) 0.035(4) 0.106(8) -0.020(4) 0.009(4) -0.004(3) C16 0.029(4) 0.032(4) 0.074(5) -0.015(3) 0.008(4) 0.000(3) N4 0.024(3) 0.025(3) 0.042(3) -0.002(2) 0.007(2) 0.000(2) C2 0.024(3) 0.023(3) 0.031(3) -0.002(2) 0.005(3) 0.000(2) N2 0.033(3) 0.023(3) 0.034(3) -0.001(2) 0.011(2) 0.002(2) C21 0.043(4) 0.028(3) 0.043(4) -0.003(3) 0.013(3) -0.005(3) C22 0.076(6) 0.037(4) 0.051(5) -0.017(4) 0.008(4) 0.005(4) C3 0.042(4) 0.024(3) 0.037(4) 0.002(3) 0.015(3) 0.006(3) N3 0.033(3) 0.030(3) 0.034(3) 0.002(2) 0.010(2) 0.009(2) C32 0.057(6) 0.076(6) 0.047(5) 0.002(4) -0.002(4) 0.024(5) C31 0.055(5) 0.049(4) 0.038(4) 0.008(3) 0.007(4) 0.017(4) C4 0.26(2) 0.139(15) 0.047(7) -0.023(8) 0.046(10) -0.012(15) Cl3 0.175(4) 0.095(2) 0.0563(16) -0.0093(15) 0.009(2) 0.016(2) Cl4 0.214(5) 0.093(2) 0.089(2) -0.0141(19) 0.085(3) -0.016(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Cu N4 2.024(5) . ? Cu N1 2.095(5) . ? Cu Cl2 2.2477(16) . ? Cu Cl1 2.3034(15) . ? Cu Cl1 2.6258(16) 3_756 ? Cl1 Cu 2.6258(16) 3_756 ? C1 N3 1.455(8) . ? C1 N1 1.489(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? N1 C2 1.479(8) . ? N1 C11 1.483(7) . ? C11 C12 1.500(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N4 1.357(8) . ? C12 C13 1.371(10) . ? C13 C14 1.371(11) . ? C13 H13 0.9500 . ? C14 C15 1.404(11) . ? C14 H14 0.9500 . ? C15 C16 1.376(11) . ? C15 H15 0.9500 . ? C16 N4 1.338(9) . ? C16 H16 0.9500 . ? C2 N2 1.471(8) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N2 C21 1.460(9) . ? N2 C3 1.463(8) . ? C21 C22 1.527(10) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C3 N3 1.458(9) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N3 C31 1.467(9) . ? C32 C31 1.498(13) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C4 Cl4 1.760(9) . ? C4 Cl3 1.801(9) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N5 C5 1.562(18) . ? N5 H5A 0.8800 . ? N5 H5B 0.8800 . ? C5 C6 1.57(7) . ? C5 H5C 0.9900 . ? C5 H5D 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? 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 N4 Cu N1 81.3(2) . . ? N4 Cu Cl2 156.13(17) . . ? N1 Cu Cl2 92.42(14) . . ? N4 Cu Cl1 93.44(15) . . ? N1 Cu Cl1 174.77(14) . . ? Cl2 Cu Cl1 92.41(6) . . ? N4 Cu Cl1 95.86(16) . 3_756 ? N1 Cu Cl1 91.11(14) . 3_756 ? Cl2 Cu Cl1 107.33(6) . 3_756 ? Cl1 Cu Cl1 89.37(5) . 3_756 ? Cu Cl1 Cu 90.63(5) . 3_756 ? N3 C1 N1 110.0(5) . . ? N3 C1 H1A 109.7 . . ? N1 C1 H1A 109.7 . . ? N3 C1 H1B 109.7 . . ? N1 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? C2 N1 C11 110.8(5) . . ? C2 N1 C1 107.9(5) . . ? C11 N1 C1 110.5(5) . . ? C2 N1 Cu 114.4(3) . . ? C11 N1 Cu 105.2(3) . . ? C1 N1 Cu 108.0(3) . . ? N1 C11 C12 109.5(5) . . ? N1 C11 H11A 109.8 . . ? C12 C11 H11A 109.8 . . ? N1 C11 H11B 109.8 . . ? C12 C11 H11B 109.8 . . ? H11A C11 H11B 108.2 . . ? N4 C12 C13 122.1(6) . . ? N4 C12 C11 114.6(6) . . ? C13 C12 C11 123.3(6) . . ? C12 C13 C14 119.9(7) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C13 C14 C15 118.4(7) . . ? C13 C14 H14 120.8 . . ? C15 C14 H14 120.8 . . ? C16 C15 C14 118.6(7) . . ? C16 C15 H15 120.7 . . ? C14 C15 H15 120.7 . . ? N4 C16 C15 122.8(7) . . ? N4 C16 H16 118.6 . . ? C15 C16 H16 118.6 . . ? C16 N4 C12 118.1(6) . . ? C16 N4 Cu 127.2(5) . . ? C12 N4 Cu 114.3(4) . . ? N2 C2 N1 109.9(5) . . ? N2 C2 H2A 109.7 . . ? N1 C2 H2A 109.7 . . ? N2 C2 H2B 109.7 . . ? N1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C21 N2 C3 112.0(5) . . ? C21 N2 C2 109.2(5) . . ? C3 N2 C2 108.2(5) . . ? N2 C21 C22 111.8(6) . . ? N2 C21 H21A 109.2 . . ? C22 C21 H21A 109.2 . . ? N2 C21 H21B 109.2 . . ? C22 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N3 C3 N2 109.5(5) . . ? N3 C3 H3A 109.8 . . ? N2 C3 H3A 109.8 . . ? N3 C3 H3B 109.8 . . ? N2 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? C1 N3 C3 109.3(5) . . ? C1 N3 C31 111.4(5) . . ? C3 N3 C31 112.0(6) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N3 C31 C32 113.3(7) . . ? N3 C31 H31A 108.9 . . ? C32 C31 H31A 108.9 . . ? N3 C31 H31B 108.9 . . ? C32 C31 H31B 108.9 . . ? H31A C31 H31B 107.7 . . ? Cl4 C4 Cl3 107.1(6) . . ? Cl4 C4 H4A 110.3 . . ? Cl3 C4 H4A 110.3 . . ? Cl4 C4 H4B 110.3 . . ? Cl3 C4 H4B 110.3 . . ? H4A C4 H4B 108.5 . . ? C5 N5 H5A 120.0 . . ? C5 N5 H5B 120.0 . . ? H5A N5 H5B 120.0 . . ? N5 C5 C6 136(3) . . ? N5 C5 H5C 103.1 . . ? C6 C5 H5C 103.1 . . ? N5 C5 H5D 103.1 . . ? C6 C5 H5D 103.1 . . ? H5C C5 H5D 105.1 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.950 _refine_diff_density_min -1.782 _refine_diff_density_rms 0.152 #============================================================================== #_eof # End of Crystallographic Information File data_pan16 _database_code_CSD 204542 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H76 B4 Cu4 F16 N20' _chemical_formula_sum 'C62 H76 B4 Cu4 F16 N20' _chemical_formula_weight 1702.83 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' B B 0.0013 0.0007 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4440(3) _cell_length_b 12.3160(4) _cell_length_c 15.6130(5) _cell_angle_alpha 89.6680(17) _cell_angle_beta 76.0910(18) _cell_angle_gamma 73.2270(12) _cell_volume 1862.08(10) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 23422 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 25.03 _exptl_crystal_description wedge _exptl_crystal_colour 'orange yellow' _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 1.220 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method \f-rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23629 _diffrn_reflns_av_R_equivalents 0.0714 _diffrn_reflns_av_sigmaI/netI 0.0641 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.09 _reflns_number_total 6560 _reflns_number_gt 4839 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius program suite version 1.9 (1997)' _computing_cell_refinement 'Collect, Nonius program suite version 1.9 (1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement ; SHELX97-2 Program for Crystal Structure Analysis. G. M. Sheldrick, Institut f. Anorg. Chemie der Universitat, Tammanstrasse 4, D-3400 Gottingen, Germany, 1998. ; _computing_molecular_graphics 'ORTEP3 for Windows - L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material 'SHELX97-2, G. M. Sheldrick' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0968P)^2^+0.5088P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6560 _refine_ls_number_parameters 517 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0764 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1537 _refine_ls_wR_factor_gt 0.1366 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.94317(5) 0.74864(4) 0.36896(3) 0.03314(17) Uani 1 1 d . . . Cu2 Cu 1.54918(5) 0.52218(4) 0.20536(3) 0.03839(17) Uani 1 1 d . . . C1 C 1.3613(4) 0.4678(3) 0.3916(2) 0.0308(8) Uani 1 1 d . . . H1A H 1.4468 0.4162 0.4030 0.037 Uiso 1 1 calc R . . H1B H 1.3256 0.4245 0.3545 0.037 Uiso 1 1 calc R . . N1 N 1.3923(3) 0.5642(2) 0.34472(19) 0.0295(7) Uani 1 1 d . . . C11 C 1.4708(4) 0.6170(3) 0.3889(2) 0.0316(8) Uani 1 1 d . . . H11A H 1.5424 0.5568 0.4078 0.038 Uiso 1 1 calc R . . H11B H 1.4078 0.6631 0.4425 0.038 Uiso 1 1 calc R . . C12 C 1.5390(4) 0.6919(3) 0.3292(2) 0.0319(8) Uani 1 1 d . . . C13 C 1.5502(4) 0.7924(3) 0.3619(3) 0.0352(9) Uani 1 1 d . . . H13 H 1.5062 0.8202 0.4215 0.042 Uiso 1 1 calc R . . C14 C 1.6268(4) 0.8516(3) 0.3062(3) 0.0429(10) Uani 1 1 d . . . H14 H 1.6389 0.9190 0.3276 0.051 Uiso 1 1 calc R . . C15 C 1.6851(4) 0.8111(3) 0.2191(3) 0.0417(10) Uani 1 1 d . . . H15 H 1.7372 0.8506 0.1795 0.050 Uiso 1 1 calc R . . C16 C 1.6665(4) 0.7127(3) 0.1906(3) 0.0382(9) Uani 1 1 d . . . H16 H 1.7057 0.6861 0.1303 0.046 Uiso 1 1 calc R . . N11 N 1.5954(3) 0.6522(3) 0.2439(2) 0.0331(7) Uani 1 1 d . . . C2 C 1.2636(4) 0.6418(3) 0.3304(2) 0.0301(8) Uani 1 1 d . . . H2A H 1.2836 0.7109 0.3055 0.036 Uiso 1 1 calc R . . H2B H 1.2347 0.6045 0.2855 0.036 Uiso 1 1 calc R . . N2 N 1.1469(3) 0.6769(2) 0.40911(19) 0.0280(6) Uani 1 1 d . . . C21 C 1.1474(4) 0.7707(3) 0.4677(3) 0.0329(8) Uani 1 1 d . . . H21A H 1.1865 0.8252 0.4314 0.040 Uiso 1 1 calc R . . H21B H 1.2070 0.7397 0.5080 0.040 Uiso 1 1 calc R . . C22 C 1.0038(4) 0.8323(3) 0.5215(3) 0.0363(9) Uani 1 1 d . . . C23 C 0.9851(5) 0.8885(4) 0.6009(3) 0.0547(12) Uani 1 1 d . . . H23 H 1.0623 0.8875 0.6233 0.066 Uiso 1 1 calc R . . C24 C 0.8521(5) 0.9472(5) 0.6486(4) 0.0672(15) Uani 1 1 d . . . H24 H 0.8372 0.9882 0.7033 0.081 Uiso 1 1 calc R . . C25 C 0.7428(5) 0.9446(4) 0.6151(3) 0.0581(12) Uani 1 1 d . . . H25 H 0.6507 0.9818 0.6472 0.070 Uiso 1 1 calc R . . C26 C 0.7681(4) 0.8882(3) 0.5354(3) 0.0431(10) Uani 1 1 d . . . H26 H 0.6917 0.8880 0.5125 0.052 Uiso 1 1 calc R . . N21 N 0.8965(3) 0.8323(2) 0.4870(2) 0.0329(7) Uani 1 1 d . . . C3 C 1.1299(4) 0.5775(3) 0.4564(2) 0.0288(8) Uani 1 1 d . . . H3A H 1.0976 0.5301 0.4204 0.035 Uiso 1 1 calc R . . H3B H 1.0582 0.6028 0.5126 0.035 Uiso 1 1 calc R . . N3 N 1.2581(3) 0.5086(2) 0.47583(19) 0.0273(6) Uani 1 1 d . . . C31 C 0.7676(4) 0.5839(3) 0.4705(2) 0.0288(8) Uani 1 1 d . . . H31A H 0.8268 0.6188 0.4948 0.035 Uiso 1 1 calc R . . H31B H 0.6788 0.6429 0.4738 0.035 Uiso 1 1 calc R . . C32 C 0.8371(3) 0.5437(3) 0.3747(2) 0.0282(8) Uani 1 1 d . . . C33 C 0.8307(4) 0.4437(3) 0.3393(3) 0.0343(8) Uani 1 1 d . . . H33 H 0.7824 0.3985 0.3754 0.041 Uiso 1 1 calc R . . C34 C 0.8944(4) 0.4090(4) 0.2513(3) 0.0415(9) Uani 1 1 d . . . H34 H 0.8923 0.3395 0.2266 0.050 Uiso 1 1 calc R . . C35 C 0.9615(4) 0.4780(4) 0.2001(3) 0.0432(10) Uani 1 1 d . . . H35 H 1.0059 0.4569 0.1395 0.052 Uiso 1 1 calc R . . C36 C 0.9624(4) 0.5778(3) 0.2387(2) 0.0369(9) Uani 1 1 d . . . H36 H 1.0064 0.6257 0.2028 0.044 Uiso 1 1 calc R . . N31 N 0.9035(3) 0.6114(3) 0.3259(2) 0.0309(7) Uani 1 1 d . . . N4 N 0.9860(4) 0.8416(3) 0.2678(2) 0.0441(8) Uani 1 1 d . . . C41 C 0.9930(5) 0.9046(4) 0.2154(3) 0.0489(11) Uani 1 1 d . . . C42 C 0.9982(7) 0.9889(5) 0.1487(4) 0.0835(19) Uani 1 1 d . . . H42A H 0.9496 1.0653 0.1770 0.125 Uiso 1 1 calc R . . H42B H 0.9539 0.9737 0.1033 0.125 Uiso 1 1 calc R . . H42C H 1.0947 0.9839 0.1211 0.125 Uiso 1 1 calc R . . N5 N 1.6166(4) 0.3532(3) 0.1685(2) 0.0428(8) Uani 1 1 d . . . H5A H 1.7004 0.3361 0.1275 0.051 Uiso 1 1 calc R . . H5B H 1.6281 0.3121 0.2169 0.051 Uiso 1 1 calc R . . C51 C 1.5151(5) 0.3224(4) 0.1301(3) 0.0467(10) Uani 1 1 d . . . H51A H 1.4593 0.2862 0.1750 0.056 Uiso 1 1 calc R . . H51B H 1.5651 0.2658 0.0795 0.056 Uiso 1 1 calc R . . C52 C 1.4206(4) 0.4215(4) 0.0991(2) 0.0407(10) Uani 1 1 d . . . C53 C 1.3308(5) 0.4069(4) 0.0493(3) 0.0494(11) Uani 1 1 d . . . H53 H 1.3318 0.3327 0.0324 0.059 Uiso 1 1 calc R . . C54 C 1.2415(5) 0.5005(5) 0.0253(3) 0.0523(12) Uani 1 1 d . . . H54 H 1.1801 0.4913 -0.0082 0.063 Uiso 1 1 calc R . . C55 C 1.2410(5) 0.6075(4) 0.0499(3) 0.0461(10) Uani 1 1 d . . . H55 H 1.1800 0.6734 0.0339 0.055 Uiso 1 1 calc R . . C56 C 1.3330(4) 0.6159(4) 0.0989(3) 0.0419(10) Uani 1 1 d . . . H56 H 1.3340 0.6895 0.1159 0.050 Uiso 1 1 calc R . . N51 N 1.4201(3) 0.5256(3) 0.1232(2) 0.0368(7) Uani 1 1 d . . . N6 N 0.3548(6) 0.8812(4) 0.1513(5) 0.108(2) Uani 1 1 d . . . C61 C 0.4071(7) 0.9502(5) 0.1373(5) 0.0800(18) Uani 1 1 d . . . C62 C 0.4741(9) 1.0385(5) 0.1223(5) 0.101(2) Uani 1 1 d . . . H62A H 0.4171 1.1026 0.0977 0.152 Uiso 1 1 calc R . . H62B H 0.5646 1.0087 0.0805 0.152 Uiso 1 1 calc R . . H62C H 0.4859 1.0641 0.1784 0.152 Uiso 1 1 calc R . . B1 B 0.6262(5) 0.1611(4) 0.3550(3) 0.0408(11) Uani 1 1 d . . . F1 F 0.6797(15) 0.2509(11) 0.3415(7) 0.073(3) Uani 0.554(12) 1 d P A 1 F2 F 0.5956(18) 0.1368(10) 0.2809(7) 0.115(6) Uani 0.554(12) 1 d P A 1 F3 F 0.7134(9) 0.0708(5) 0.3807(8) 0.093(4) Uani 0.554(12) 1 d P A 1 F4 F 0.5104(8) 0.1932(8) 0.4195(6) 0.115(4) Uani 0.554(12) 1 d P A 1 F1A F 0.6483(19) 0.2558(12) 0.3840(13) 0.099(6) Uani 0.446(12) 1 d P A 2 F2A F 0.5178(14) 0.1898(10) 0.3150(10) 0.094(5) Uani 0.446(12) 1 d P A 2 F3A F 0.7345(11) 0.0934(9) 0.2985(9) 0.114(6) Uani 0.446(12) 1 d P A 2 F4A F 0.5848(12) 0.1009(8) 0.4244(5) 0.085(4) Uani 0.446(12) 1 d P A 2 B2 B 0.9169(6) 0.7814(4) -0.0328(3) 0.0501(13) Uani 1 1 d . . . F5 F 0.8502(4) 0.7913(3) -0.1013(3) 0.0932(11) Uani 1 1 d . . . F6 F 0.8575(5) 0.8740(3) 0.0228(3) 0.1203(17) Uani 1 1 d . . . F7 F 1.0529(3) 0.7734(3) -0.0736(2) 0.0710(8) Uani 1 1 d . . . F8 F 0.9120(3) 0.6819(2) 0.00766(19) 0.0662(8) Uani 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 0.0267(3) 0.0377(3) 0.0403(3) 0.0106(2) -0.0144(2) -0.0129(2) Cu2 0.0380(3) 0.0453(3) 0.0386(3) 0.0042(2) -0.0137(2) -0.0192(2) C1 0.0234(19) 0.0337(18) 0.0367(19) 0.0063(16) -0.0087(16) -0.0098(15) N1 0.0215(16) 0.0390(16) 0.0324(15) 0.0068(13) -0.0105(13) -0.0130(13) C11 0.0201(19) 0.043(2) 0.0343(19) 0.0067(16) -0.0103(15) -0.0112(16) C12 0.0174(18) 0.039(2) 0.039(2) 0.0077(16) -0.0096(15) -0.0072(15) C13 0.025(2) 0.040(2) 0.043(2) 0.0024(17) -0.0142(17) -0.0077(16) C14 0.035(2) 0.036(2) 0.065(3) 0.009(2) -0.022(2) -0.0151(18) C15 0.034(2) 0.046(2) 0.053(2) 0.021(2) -0.0170(19) -0.0193(18) C16 0.029(2) 0.051(2) 0.039(2) 0.0126(18) -0.0107(17) -0.0168(18) N11 0.0240(17) 0.0416(17) 0.0376(17) 0.0081(14) -0.0089(13) -0.0150(14) C2 0.0225(19) 0.0391(19) 0.0341(19) 0.0119(16) -0.0137(15) -0.0122(15) N2 0.0193(15) 0.0322(15) 0.0356(16) 0.0086(13) -0.0104(13) -0.0097(12) C21 0.024(2) 0.0346(19) 0.044(2) 0.0036(16) -0.0128(16) -0.0114(15) C22 0.031(2) 0.0323(19) 0.049(2) 0.0036(17) -0.0138(18) -0.0115(16) C23 0.038(3) 0.064(3) 0.062(3) -0.015(2) -0.020(2) -0.010(2) C24 0.047(3) 0.079(3) 0.066(3) -0.031(3) -0.015(3) -0.002(3) C25 0.036(3) 0.056(3) 0.072(3) -0.013(2) -0.009(2) -0.001(2) C26 0.028(2) 0.045(2) 0.058(3) 0.003(2) -0.0149(19) -0.0077(18) N21 0.0240(17) 0.0350(16) 0.0426(17) 0.0073(14) -0.0142(14) -0.0084(13) C3 0.0202(18) 0.0349(18) 0.0348(18) 0.0063(15) -0.0100(15) -0.0112(15) N3 0.0190(15) 0.0318(15) 0.0333(15) 0.0104(12) -0.0082(12) -0.0096(12) C31 0.0239(19) 0.0315(18) 0.0349(19) 0.0059(15) -0.0108(15) -0.0114(15) C32 0.0164(17) 0.0351(18) 0.0350(19) 0.0100(15) -0.0106(15) -0.0074(14) C33 0.027(2) 0.041(2) 0.040(2) 0.0082(17) -0.0109(16) -0.0152(16) C34 0.039(2) 0.045(2) 0.043(2) -0.0018(18) -0.0115(19) -0.0161(18) C35 0.033(2) 0.059(3) 0.036(2) -0.0025(19) -0.0039(17) -0.0143(19) C36 0.029(2) 0.048(2) 0.036(2) 0.0086(18) -0.0054(17) -0.0169(17) N31 0.0199(16) 0.0397(16) 0.0363(17) 0.0081(14) -0.0091(13) -0.0122(13) N4 0.042(2) 0.049(2) 0.051(2) 0.0182(18) -0.0205(17) -0.0219(16) C41 0.047(3) 0.059(3) 0.056(3) 0.025(2) -0.027(2) -0.029(2) C42 0.103(5) 0.098(4) 0.089(4) 0.064(4) -0.055(4) -0.066(4) N5 0.044(2) 0.0487(19) 0.0387(18) 0.0088(15) -0.0132(16) -0.0169(16) C51 0.055(3) 0.045(2) 0.048(2) 0.006(2) -0.018(2) -0.022(2) C52 0.043(2) 0.054(2) 0.032(2) 0.0061(18) -0.0047(18) -0.029(2) C53 0.054(3) 0.064(3) 0.043(2) 0.003(2) -0.016(2) -0.034(2) C54 0.041(3) 0.089(3) 0.040(2) 0.009(2) -0.016(2) -0.036(3) C55 0.037(2) 0.069(3) 0.036(2) 0.014(2) -0.0112(18) -0.019(2) C56 0.039(2) 0.054(2) 0.039(2) 0.0115(19) -0.0120(18) -0.020(2) N51 0.0368(19) 0.0464(19) 0.0338(16) 0.0084(15) -0.0106(14) -0.0209(15) N6 0.080(4) 0.057(3) 0.195(7) -0.005(4) -0.047(4) -0.022(3) C61 0.068(4) 0.055(3) 0.124(5) -0.006(3) -0.043(4) -0.014(3) C62 0.139(7) 0.077(4) 0.131(6) 0.035(4) -0.084(5) -0.060(4) B1 0.038(3) 0.039(2) 0.046(3) 0.003(2) -0.012(2) -0.012(2) F1 0.091(7) 0.066(6) 0.100(7) 0.032(6) -0.059(6) -0.056(5) F2 0.233(18) 0.103(8) 0.076(6) 0.041(5) -0.096(8) -0.107(10) F3 0.083(6) 0.047(3) 0.181(11) 0.037(4) -0.086(7) -0.024(3) F4 0.085(6) 0.104(7) 0.113(6) 0.012(5) 0.040(5) -0.015(5) F1A 0.094(11) 0.036(5) 0.187(17) -0.018(9) -0.100(12) 0.002(5) F2A 0.105(9) 0.076(7) 0.149(13) 0.031(7) -0.097(9) -0.047(6) F3A 0.078(7) 0.090(6) 0.133(11) -0.032(7) 0.044(7) -0.020(5) F4A 0.114(10) 0.091(7) 0.050(4) 0.022(4) -0.022(4) -0.031(7) B2 0.056(3) 0.052(3) 0.045(3) 0.003(2) -0.005(2) -0.026(3) F5 0.087(3) 0.101(3) 0.116(3) 0.030(2) -0.062(2) -0.036(2) F6 0.172(4) 0.076(2) 0.088(2) -0.022(2) 0.031(3) -0.051(3) F7 0.0528(18) 0.085(2) 0.081(2) 0.0389(17) -0.0180(15) -0.0289(15) F8 0.070(2) 0.0693(17) 0.0682(18) 0.0177(15) -0.0106(15) -0.0399(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N4 1.986(3) . ? Cu1 N21 2.000(3) . ? Cu1 N31 2.008(3) . ? Cu1 N2 2.291(3) . ? Cu2 N11 1.938(3) . ? Cu2 N5 2.033(3) . ? Cu2 N51 2.064(3) . ? Cu2 N1 2.344(3) . ? C1 N1 1.466(4) . ? C1 N3 1.469(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? N1 C11 1.469(5) . ? N1 C2 1.473(4) . ? C11 C12 1.509(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N11 1.351(5) . ? C12 C13 1.388(5) . ? C13 C14 1.387(6) . ? C13 H13 0.9500 . ? C14 C15 1.379(6) . ? C14 H14 0.9500 . ? C15 C16 1.374(6) . ? C15 H15 0.9500 . ? C16 N11 1.347(5) . ? C16 H16 0.9500 . ? C2 N2 1.471(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N2 C3 1.458(4) . ? N2 C21 1.480(5) . ? C21 C22 1.508(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 N21 1.354(5) . ? C22 C23 1.368(6) . ? C23 C24 1.391(7) . ? C23 H23 0.9500 . ? C24 C25 1.373(7) . ? C24 H24 0.9500 . ? C25 C26 1.359(6) . ? C25 H25 0.9500 . ? C26 N21 1.352(5) . ? C26 H26 0.9500 . ? C3 N3 1.463(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N3 C31 1.459(4) 2_766 ? C31 N3 1.459(4) 2_766 ? C31 C32 1.512(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 N31 1.353(4) . ? C32 C33 1.379(5) . ? C33 C34 1.384(6) . ? C33 H33 0.9500 . ? C34 C35 1.384(6) . ? C34 H34 0.9500 . ? C35 C36 1.376(6) . ? C35 H35 0.9500 . ? C36 N31 1.363(5) . ? C36 H36 0.9500 . ? N4 C41 1.127(5) . ? C41 C42 1.469(6) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? N5 C51 1.471(6) . ? N5 H5A 0.9200 . ? N5 H5B 0.9200 . ? C51 C52 1.492(6) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 N51 1.337(5) . ? C52 C53 1.401(6) . ? C53 C54 1.372(7) . ? C53 H53 0.9500 . ? C54 C55 1.372(7) . ? C54 H54 0.9500 . ? C55 C56 1.390(6) . ? C55 H55 0.9500 . ? C56 N51 1.337(5) . ? C56 H56 0.9500 . ? N6 C61 1.129(8) . ? C61 C62 1.444(9) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? B1 F3A 1.318(9) . ? B1 F2 1.329(10) . ? B1 F4 1.333(8) . ? B1 F3 1.347(7) . ? B1 F1A 1.354(16) . ? B1 F4A 1.365(9) . ? B1 F1 1.370(13) . ? B1 F2A 1.378(12) . ? B2 F6 1.336(6) . ? B2 F8 1.384(6) . ? B2 F7 1.385(6) . ? B2 F5 1.398(7) . ? 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 N4 Cu1 N21 113.63(13) . . ? N4 Cu1 N31 109.30(13) . . ? N21 Cu1 N31 134.07(12) . . ? N4 Cu1 N2 105.16(12) . . ? N21 Cu1 N2 79.58(11) . . ? N31 Cu1 N2 104.47(11) . . ? N11 Cu2 N5 146.42(14) . . ? N11 Cu2 N51 125.57(13) . . ? N5 Cu2 N51 83.08(14) . . ? N11 Cu2 N1 81.13(11) . . ? N5 Cu2 N1 112.54(12) . . ? N51 Cu2 N1 101.74(11) . . ? N1 C1 N3 110.0(3) . . ? N1 C1 H1A 109.7 . . ? N3 C1 H1A 109.7 . . ? N1 C1 H1B 109.7 . . ? N3 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? C1 N1 C11 111.4(3) . . ? C1 N1 C2 109.1(3) . . ? C11 N1 C2 115.3(3) . . ? C1 N1 Cu2 116.8(2) . . ? C11 N1 Cu2 98.0(2) . . ? C2 N1 Cu2 106.0(2) . . ? N1 C11 C12 111.9(3) . . ? N1 C11 H11A 109.2 . . ? C12 C11 H11A 109.2 . . ? N1 C11 H11B 109.2 . . ? C12 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? N11 C12 C13 122.2(3) . . ? N11 C12 C11 116.3(3) . . ? C13 C12 C11 121.5(3) . . ? C14 C13 C12 119.0(4) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C15 C14 C13 119.0(4) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? C16 C15 C14 118.9(4) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? N11 C16 C15 123.2(4) . . ? N11 C16 H16 118.4 . . ? C15 C16 H16 118.4 . . ? C16 N11 C12 117.7(3) . . ? C16 N11 Cu2 125.1(3) . . ? C12 N11 Cu2 116.8(2) . . ? N2 C2 N1 115.9(3) . . ? N2 C2 H2A 108.3 . . ? N1 C2 H2A 108.3 . . ? N2 C2 H2B 108.3 . . ? N1 C2 H2B 108.3 . . ? H2A C2 H2B 107.4 . . ? C3 N2 C2 109.8(3) . . ? C3 N2 C21 112.9(3) . . ? C2 N2 C21 116.0(3) . . ? C3 N2 Cu1 103.9(2) . . ? C2 N2 Cu1 110.6(2) . . ? C21 N2 Cu1 102.6(2) . . ? N2 C21 C22 111.5(3) . . ? N2 C21 H21A 109.3 . . ? C22 C21 H21A 109.3 . . ? N2 C21 H21B 109.3 . . ? C22 C21 H21B 109.3 . . ? H21A C21 H21B 108.0 . . ? N21 C22 C23 122.0(4) . . ? N21 C22 C21 117.7(3) . . ? C23 C22 C21 120.3(4) . . ? C22 C23 C24 119.5(4) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C25 C24 C23 118.6(4) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? C26 C25 C24 119.1(4) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? N21 C26 C25 123.3(4) . . ? N21 C26 H26 118.3 . . ? C25 C26 H26 118.3 . . ? C26 N21 C22 117.4(3) . . ? C26 N21 Cu1 126.0(3) . . ? C22 N21 Cu1 116.6(3) . . ? N2 C3 N3 112.5(3) . . ? N2 C3 H3A 109.1 . . ? N3 C3 H3A 109.1 . . ? N2 C3 H3B 109.1 . . ? N3 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? C31 N3 C3 110.0(3) 2_766 . ? C31 N3 C1 112.7(3) 2_766 . ? C3 N3 C1 108.3(3) . . ? N3 C31 C32 112.2(3) 2_766 . ? N3 C31 H31A 109.2 2_766 . ? C32 C31 H31A 109.2 . . ? N3 C31 H31B 109.2 2_766 . ? C32 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? N31 C32 C33 122.1(3) . . ? N31 C32 C31 116.7(3) . . ? C33 C32 C31 121.2(3) . . ? C32 C33 C34 120.1(3) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 118.5(4) . . ? C35 C34 H34 120.7 . . ? C33 C34 H34 120.7 . . ? C36 C35 C34 118.8(4) . . ? C36 C35 H35 120.6 . . ? C34 C35 H35 120.6 . . ? N31 C36 C35 123.4(3) . . ? N31 C36 H36 118.3 . . ? C35 C36 H36 118.3 . . ? C32 N31 C36 117.1(3) . . ? C32 N31 Cu1 127.5(2) . . ? C36 N31 Cu1 115.1(2) . . ? C41 N4 Cu1 170.5(4) . . ? N4 C41 C42 178.4(6) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C51 N5 Cu2 109.6(3) . . ? C51 N5 H5A 109.8 . . ? Cu2 N5 H5A 109.8 . . ? C51 N5 H5B 109.8 . . ? Cu2 N5 H5B 109.8 . . ? H5A N5 H5B 108.2 . . ? N5 C51 C52 113.4(3) . . ? N5 C51 H51A 108.9 . . ? C52 C51 H51A 108.9 . . ? N5 C51 H51B 108.9 . . ? C52 C51 H51B 108.9 . . ? H51A C51 H51B 107.7 . . ? N51 C52 C53 120.7(4) . . ? N51 C52 C51 117.8(4) . . ? C53 C52 C51 121.5(4) . . ? C54 C53 C52 119.5(4) . . ? C54 C53 H53 120.2 . . ? C52 C53 H53 120.2 . . ? C53 C54 C55 119.9(4) . . ? C53 C54 H54 120.0 . . ? C55 C54 H54 120.0 . . ? C54 C55 C56 117.6(4) . . ? C54 C55 H55 121.2 . . ? C56 C55 H55 121.2 . . ? N51 C56 C55 123.2(4) . . ? N51 C56 H56 118.4 . . ? C55 C56 H56 118.4 . . ? C52 N51 C56 119.0(4) . . ? C52 N51 Cu2 112.4(3) . . ? C56 N51 Cu2 128.3(3) . . ? N6 C61 C62 178.2(8) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? F3A B1 F2 68.4(8) . . ? F3A B1 F4 159.3(7) . . ? F2 B1 F4 109.0(9) . . ? F3A B1 F3 58.0(7) . . ? F2 B1 F3 112.2(7) . . ? F4 B1 F3 107.7(7) . . ? F3A B1 F1A 113.8(10) . . ? F2 B1 F1A 131.1(9) . . ? F4 B1 F1A 83.9(10) . . ? F3 B1 F1A 107.6(8) . . ? F3A B1 F4A 108.8(8) . . ? F2 B1 F4A 114.4(7) . . ? F4 B1 F4A 52.4(5) . . ? F3 B1 F4A 57.1(6) . . ? F1A B1 F4A 110.6(9) . . ? F3A B1 F1 91.8(8) . . ? F2 B1 F1 108.0(7) . . ? F4 B1 F1 108.2(7) . . ? F3 B1 F1 111.7(8) . . ? F1A B1 F1 28.1(9) . . ? F4A B1 F1 137.2(7) . . ? F3A B1 F2A 108.2(9) . . ? F2 B1 F2A 40.0(6) . . ? F4 B1 F2A 73.1(8) . . ? F3 B1 F2A 141.8(7) . . ? F1A B1 F2A 110.4(8) . . ? F4A B1 F2A 104.7(8) . . ? F1 B1 F2A 103.6(8) . . ? F6 B2 F8 113.0(4) . . ? F6 B2 F7 111.4(4) . . ? F8 B2 F7 109.1(4) . . ? F6 B2 F5 108.7(5) . . ? F8 B2 F5 109.0(4) . . ? F7 B2 F5 105.3(4) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.636 _refine_diff_density_min -0.934 _refine_diff_density_rms 0.103 #============================================================================== #_eof # End of Crystallographic Information File data_pan17 _database_code_CSD 204543 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C21 H24 Cu N6),(B F4)' _chemical_formula_sum 'C21 H24 B Cu F4 N6' _chemical_formula_weight 510.81 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 18.6920(16) _cell_length_b 10.6070(6) _cell_length_c 24.0520(18) _cell_angle_alpha 90.00 _cell_angle_beta 111.354(3) _cell_angle_gamma 90.00 _cell_volume 4441.3(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7523 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 1.039 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method \f-rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13703 _diffrn_reflns_av_R_equivalents 0.2619 _diffrn_reflns_av_sigmaI/netI 0.3750 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.21 _reflns_number_total 7326 _reflns_number_gt 2478 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius program suite version 1.9 (1997)' _computing_cell_refinement 'Collect, Nonius program suite version 1.9 (1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement ; SHELX97-2 Program for Crystal Structure Analysis. G. M. Sheldrick, Institut f. Anorg. Chemie der Universitat, Tammanstrasse 4, D-3400 Gottingen, Germany, 1998. ; _computing_molecular_graphics 'ORTEP3 for Windows - L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material 'SHELX97-2, G. M. Sheldrick' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1713P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0016(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7326 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.3460 _refine_ls_R_factor_gt 0.1475 _refine_ls_wR_factor_ref 0.3689 _refine_ls_wR_factor_gt 0.3040 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.30568(11) 0.76246(19) -0.03990(8) 0.0527(7) Uani 1 1 d . . . C1 C 0.2738(9) 0.5232(13) 0.0268(6) 0.054(5) Uani 1 1 d . . . H1A H 0.2540 0.4951 -0.0153 0.065 Uiso 1 1 calc R . . H1B H 0.2303 0.5615 0.0349 0.065 Uiso 1 1 calc R . . N1 N 0.3319(6) 0.6224(14) 0.0335(5) 0.054(4) Uani 1 1 d . . . C11 C 0.3508(8) 0.7016(14) 0.0887(6) 0.044(4) Uiso 1 1 d . . . H11A H 0.3034 0.7209 0.0963 0.053 Uiso 1 1 calc R . . H11B H 0.3864 0.6554 0.1236 0.053 Uiso 1 1 calc R . . C12 C 0.3875(8) 0.8210(15) 0.0796(6) 0.040(4) Uani 1 1 d . . . C13 C 0.4220(8) 0.903(2) 0.1270(8) 0.067(5) Uani 1 1 d . . . H13 H 0.4201 0.8821 0.1649 0.081 Uiso 1 1 calc R . . C14 C 0.4574(8) 1.0077(16) 0.1217(7) 0.050(4) Uani 1 1 d . . . H14 H 0.4870 1.0541 0.1563 0.060 Uiso 1 1 calc R . . C15 C 0.4510(9) 1.0487(14) 0.0665(7) 0.054(5) Uani 1 1 d . . . H15 H 0.4688 1.1292 0.0599 0.064 Uiso 1 1 calc R . . C16 C 0.4171(9) 0.9654(19) 0.0210(9) 0.067(6) Uani 1 1 d . . . H16 H 0.4189 0.9845 -0.0171 0.080 Uiso 1 1 calc R . . N11 N 0.3817(7) 0.8592(13) 0.0262(5) 0.049(4) Uani 1 1 d . . . C2 C 0.4071(8) 0.5619(14) 0.0321(7) 0.043(4) Uani 1 1 d . . . H2A H 0.3973 0.5237 -0.0075 0.052 Uiso 1 1 calc R . . H2B H 0.4470 0.6277 0.0389 0.052 Uiso 1 1 calc R . . N2 N 0.4349(6) 0.4635(12) 0.0791(6) 0.048(4) Uani 1 1 d . . . C21 C 0.5055(8) 0.4146(17) 0.0853(7) 0.056(5) Uani 1 1 d . . . H21A H 0.5373 0.4829 0.0784 0.067 Uiso 1 1 calc R . . H21B H 0.4982 0.3501 0.0540 0.067 Uiso 1 1 calc R . . C22 C 0.5492(10) 0.3550(19) 0.1457(11) 0.073(6) Uani 1 1 d . . . C23 C 0.5481(10) 0.413(2) 0.1993(10) 0.079(6) Uani 1 1 d . . . H23 H 0.5236 0.4916 0.2001 0.095 Uiso 1 1 calc R . . C24 C 0.5853(13) 0.345(2) 0.2478(9) 0.082(7) Uani 1 1 d . . . H24 H 0.5835 0.3748 0.2846 0.098 Uiso 1 1 calc R . . C25 C 0.6225(12) 0.246(3) 0.2494(10) 0.088(7) Uani 1 1 d . . . H25 H 0.6492 0.2063 0.2866 0.106 Uiso 1 1 calc R . . C26 C 0.6250(11) 0.195(2) 0.1973(12) 0.098(8) Uani 1 1 d . . . H26 H 0.6536 0.1200 0.1992 0.117 Uiso 1 1 calc R . . N21 N 0.5860(7) 0.2510(15) 0.1419(6) 0.061(4) Uani 1 1 d . . . C3 C 0.3734(8) 0.3673(15) 0.0629(7) 0.049(4) Uani 1 1 d . . . H3A H 0.3640 0.3383 0.0217 0.059 Uiso 1 1 calc R . . H3B H 0.3920 0.2940 0.0897 0.059 Uiso 1 1 calc R . . N3 N 0.2999(7) 0.4085(13) 0.0659(6) 0.058(4) Uani 1 1 d . . . C31 C 0.1934(10) 0.9261(15) -0.1289(6) 0.057(5) Uani 1 1 d . . . H31A H 0.2365 0.9784 -0.1304 0.068 Uiso 1 1 calc R . . H31B H 0.1447 0.9696 -0.1516 0.068 Uiso 1 1 calc R . . C32 C 0.1953(9) 0.7945(16) -0.1565(8) 0.060(5) Uani 1 1 d . . . C33 C 0.1501(9) 0.7683(14) -0.2150(6) 0.051(5) Uani 1 1 d . . . H33 H 0.1142 0.8300 -0.2372 0.061 Uiso 1 1 calc R . . C34 C 0.1548(10) 0.6592(18) -0.2419(7) 0.062(5) Uani 1 1 d . . . H34 H 0.1225 0.6399 -0.2818 0.074 Uiso 1 1 calc R . . C35 C 0.2145(9) 0.5714(15) -0.2041(7) 0.057(5) Uani 1 1 d . . . H35 H 0.2245 0.4944 -0.2201 0.069 Uiso 1 1 calc R . . C36 C 0.2544(10) 0.6025(15) -0.1469(7) 0.053(5) Uani 1 1 d . . . H36 H 0.2901 0.5426 -0.1230 0.064 Uiso 1 1 calc R . . N31 N 0.2473(6) 0.7129(13) -0.1208(6) 0.050(4) Uani 1 1 d . . . Cu2 Cu 0.65595(11) 0.77636(18) 0.45937(8) 0.0476(7) Uani 1 1 d . . . C4 C 0.6839(8) 1.1739(16) 0.5616(7) 0.049(4) Uani 1 1 d . . . H4A H 0.6547 1.2033 0.5205 0.059 Uiso 1 1 calc R . . H4B H 0.6904 1.2468 0.5887 0.059 Uiso 1 1 calc R . . N4 N 0.7592(7) 1.1332(10) 0.5646(5) 0.045(3) Uani 1 1 d . . . C41 C 0.6873(8) 0.6061(14) 0.3725(7) 0.050(4) Uani 1 1 d . . . H41A H 0.6454 0.5493 0.3728 0.060 Uiso 1 1 calc R . . H41B H 0.7156 0.5648 0.3498 0.060 Uiso 1 1 calc R . . C42 C 0.6541(8) 0.7322(18) 0.3435(7) 0.057(5) Uani 1 1 d . . . C43 C 0.6377(9) 0.7422(17) 0.2838(7) 0.051(4) Uani 1 1 d . . . H43 H 0.6486 0.6781 0.2605 0.062 Uiso 1 1 calc R . . C44 C 0.6042(9) 0.853(2) 0.2611(9) 0.072(6) Uani 1 1 d . . . H44 H 0.5993 0.8722 0.2213 0.086 Uiso 1 1 calc R . . C45 C 0.5777(11) 0.9379(19) 0.2884(8) 0.069(6) Uani 1 1 d . . . H45 H 0.5470 1.0074 0.2683 0.083 Uiso 1 1 calc R . . C46 C 0.5978(8) 0.9178(12) 0.3483(6) 0.038(4) Uani 1 1 d . . . H46 H 0.5869 0.9813 0.3720 0.045 Uiso 1 1 calc R . . N41 N 0.6323(7) 0.8117(14) 0.3749(5) 0.050(4) Uani 1 1 d . . . C5 C 0.7431(7) 1.0117(13) 0.5257(6) 0.036(3) Uiso 1 1 d . . . H5A H 0.7251 1.0374 0.4833 0.044 Uiso 1 1 calc R . . H5B H 0.7924 0.9665 0.5346 0.044 Uiso 1 1 calc R . . N5 N 0.6880(8) 0.9241(13) 0.5328(5) 0.054(4) Uani 1 1 d . . . C51 C 0.7232(8) 0.8348(15) 0.5868(7) 0.048(4) Uani 1 1 d . . . H51A H 0.7769 0.8152 0.5916 0.058 Uiso 1 1 calc R . . H51B H 0.7239 0.8778 0.6235 0.058 Uiso 1 1 calc R . . C52 C 0.6798(7) 0.7178(15) 0.5793(6) 0.040(4) Uani 1 1 d . . . C53 C 0.6820(11) 0.6462(19) 0.6299(9) 0.072(6) Uani 1 1 d . . . H53 H 0.7088 0.6763 0.6693 0.086 Uiso 1 1 calc R . . C54 C 0.6444(9) 0.532(2) 0.6204(8) 0.077(6) Uani 1 1 d . . . H54 H 0.6463 0.4808 0.6533 0.092 Uiso 1 1 calc R . . C55 C 0.6044(7) 0.4935(15) 0.5638(8) 0.048(4) Uani 1 1 d . . . H55 H 0.5771 0.4160 0.5567 0.057 Uiso 1 1 calc R . . C56 C 0.6040(8) 0.5679(15) 0.5168(8) 0.047(4) Uani 1 1 d . . . H56 H 0.5763 0.5396 0.4773 0.057 Uiso 1 1 calc R . . N51 N 0.6414(8) 0.6797(15) 0.5246(6) 0.061(4) Uani 1 1 d . . . C6 C 0.6213(9) 0.9818(13) 0.5322(7) 0.042(4) Uani 1 1 d . . . H6A H 0.5869 0.9178 0.5392 0.051 Uiso 1 1 calc R . . H6B H 0.5942 1.0200 0.4925 0.051 Uiso 1 1 calc R . . N6 N 0.6382(6) 1.0776(12) 0.5774(5) 0.043(3) Uani 1 1 d . . . C61 C 0.5706(8) 1.1345(18) 0.5841(7) 0.060(5) Uani 1 1 d . . . H61A H 0.5340 1.0655 0.5819 0.072 Uiso 1 1 calc R . . H61B H 0.5460 1.1891 0.5489 0.072 Uiso 1 1 calc R . . C62 C 0.5787(8) 1.2116(15) 0.6387(7) 0.040(4) Uani 1 1 d . . . C63 C 0.6362(11) 1.195(2) 0.6921(8) 0.090(7) Uani 1 1 d . . . H63 H 0.6720 1.1285 0.6957 0.108 Uiso 1 1 calc R . . C64 C 0.6457(12) 1.270(2) 0.7429(7) 0.077(6) Uani 1 1 d . . . H64 H 0.6900 1.2675 0.7785 0.092 Uiso 1 1 calc R . . C65 C 0.5862(12) 1.346(2) 0.7355(9) 0.077(7) Uani 1 1 d . . . H65 H 0.5820 1.3850 0.7697 0.092 Uiso 1 1 calc R . . C66 C 0.5376(11) 1.3674(19) 0.6877(9) 0.070(5) Uani 1 1 d . . . H66 H 0.5030 1.4349 0.6847 0.084 Uiso 1 1 calc R . . N61 N 0.5286(9) 1.2951(13) 0.6335(6) 0.067(4) Uani 1 1 d . . . B1 B 0.1436(11) 0.743(3) 0.1104(8) 0.062(7) Uani 1 1 d . . . F1 F 0.1861(7) 0.8107(15) 0.0903(7) 0.136(6) Uani 1 1 d . . . F2 F 0.0764(7) 0.7470(12) 0.0584(7) 0.123(5) Uani 1 1 d . . . F3 F 0.1625(8) 0.6315(13) 0.1258(7) 0.137(6) Uani 1 1 d . . . F4 F 0.1289(12) 0.8202(14) 0.1535(7) 0.181(8) Uani 1 1 d . . . B2 B 0.0433(14) 0.241(2) 0.3923(8) 0.060(6) Uani 1 1 d . . . F5 F 0.0175(6) 0.2606(13) 0.4386(6) 0.111(5) Uani 1 1 d . . . F6 F -0.0096(9) 0.272(3) 0.3449(9) 0.257(14) Uani 1 1 d . . . F7 F 0.1118(6) 0.2969(11) 0.4013(6) 0.104(4) Uani 1 1 d . . . F8 F 0.0538(10) 0.1229(17) 0.3924(9) 0.168(7) Uani 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 0.0740(15) 0.0441(14) 0.0294(11) -0.0012(9) 0.0062(9) 0.0018(10) C1 0.060(11) 0.033(10) 0.029(8) 0.008(7) -0.031(7) -0.007(8) N1 0.033(8) 0.088(12) 0.035(8) -0.014(7) 0.004(6) -0.001(7) C12 0.042(9) 0.066(11) 0.012(7) -0.010(7) 0.010(6) 0.009(8) C13 0.036(10) 0.102(16) 0.058(12) 0.006(11) 0.009(8) -0.022(10) C14 0.035(9) 0.064(13) 0.045(10) 0.004(9) 0.007(7) -0.004(9) C15 0.088(13) 0.020(9) 0.036(10) -0.019(7) 0.002(9) -0.013(8) C16 0.050(11) 0.076(15) 0.080(14) 0.027(12) 0.029(10) 0.042(11) N11 0.050(8) 0.057(10) 0.035(8) 0.005(6) 0.011(6) -0.015(7) C2 0.038(9) 0.048(11) 0.041(9) 0.012(7) 0.011(7) 0.013(8) N2 0.032(8) 0.050(9) 0.074(10) 0.004(7) 0.034(7) -0.005(6) C21 0.023(9) 0.076(14) 0.063(12) 0.000(10) 0.008(8) -0.006(8) C22 0.046(12) 0.052(14) 0.12(2) 0.004(12) 0.035(12) -0.001(10) C23 0.046(12) 0.107(18) 0.080(15) -0.002(14) 0.020(11) 0.005(11) C24 0.093(17) 0.049(15) 0.071(15) 0.013(12) -0.010(12) -0.023(12) C25 0.065(15) 0.11(2) 0.071(16) 0.013(15) -0.003(11) -0.021(14) C26 0.080(16) 0.077(17) 0.098(19) 0.026(14) -0.014(13) 0.019(12) N21 0.045(8) 0.085(12) 0.054(9) 0.004(8) 0.018(7) 0.017(8) C3 0.051(10) 0.050(11) 0.044(9) 0.009(8) 0.015(8) -0.013(9) N3 0.047(8) 0.057(10) 0.070(10) 0.031(8) 0.022(7) 0.024(7) C31 0.075(12) 0.057(12) 0.019(8) -0.015(7) -0.006(8) -0.012(9) C32 0.058(11) 0.063(13) 0.076(13) 0.024(10) 0.044(10) 0.048(10) C33 0.084(12) 0.024(9) 0.029(8) -0.006(7) 0.001(8) 0.004(8) C34 0.073(12) 0.065(13) 0.041(10) 0.004(9) 0.014(8) 0.016(10) C35 0.068(12) 0.036(11) 0.061(12) -0.031(9) 0.014(9) 0.004(9) C36 0.085(13) 0.024(10) 0.062(12) -0.001(8) 0.039(10) 0.008(8) N31 0.028(7) 0.066(10) 0.063(9) 0.004(8) 0.023(6) 0.006(7) Cu2 0.0631(14) 0.0462(14) 0.0319(11) -0.0016(9) 0.0156(9) -0.0015(10) C4 0.035(9) 0.064(12) 0.044(9) -0.004(8) 0.010(7) 0.023(8) N4 0.071(9) 0.022(7) 0.044(8) -0.008(6) 0.023(7) -0.024(6) C41 0.053(10) 0.036(10) 0.054(10) 0.012(8) 0.011(8) 0.001(8) C42 0.034(9) 0.086(14) 0.042(10) -0.013(10) 0.002(7) 0.024(9) C43 0.054(10) 0.064(13) 0.042(10) 0.001(9) 0.025(8) 0.007(9) C44 0.039(11) 0.13(2) 0.061(12) 0.023(13) 0.035(9) 0.003(12) C45 0.091(14) 0.067(14) 0.045(11) -0.009(10) 0.020(10) -0.007(11) C46 0.052(10) 0.015(8) 0.030(8) -0.004(6) -0.005(7) 0.013(7) N41 0.055(8) 0.073(11) 0.024(6) -0.020(7) 0.017(6) 0.002(8) N5 0.082(10) 0.065(10) 0.024(7) 0.003(6) 0.030(7) 0.000(8) C51 0.031(9) 0.058(12) 0.064(11) 0.002(9) 0.027(8) -0.015(8) C52 0.024(8) 0.053(11) 0.038(9) -0.010(8) 0.006(6) 0.015(7) C53 0.082(14) 0.065(15) 0.085(14) 0.033(11) 0.049(11) 0.005(11) C54 0.037(11) 0.119(19) 0.062(13) 0.024(11) 0.003(9) -0.033(11) C55 0.022(8) 0.054(12) 0.069(12) 0.011(9) 0.018(8) -0.011(7) C56 0.051(10) 0.027(10) 0.073(12) 0.007(9) 0.033(9) 0.001(8) N51 0.079(10) 0.071(11) 0.038(8) 0.001(7) 0.028(7) 0.019(9) C6 0.066(11) 0.013(9) 0.054(10) 0.005(7) 0.028(8) 0.009(8) N6 0.009(6) 0.069(10) 0.052(8) 0.004(7) 0.012(6) -0.011(6) C61 0.039(10) 0.102(16) 0.044(10) -0.006(9) 0.021(8) -0.022(9) C62 0.038(9) 0.043(11) 0.052(10) 0.022(8) 0.031(8) 0.017(8) C63 0.064(13) 0.15(2) 0.049(13) 0.009(13) 0.009(10) 0.005(13) C64 0.067(14) 0.121(19) 0.029(10) 0.018(11) 0.000(9) -0.010(13) C65 0.055(13) 0.13(2) 0.040(12) 0.014(11) 0.007(10) -0.026(13) C66 0.073(13) 0.096(16) 0.060(13) -0.014(11) 0.049(11) 0.006(11) N61 0.083(11) 0.038(10) 0.068(10) -0.018(7) 0.013(8) -0.009(8) B1 0.041(12) 0.12(2) 0.036(10) -0.027(13) 0.027(10) -0.006(13) F1 0.106(10) 0.177(15) 0.155(14) 0.018(11) 0.083(10) -0.028(10) F2 0.083(8) 0.105(10) 0.150(13) -0.008(9) 0.005(8) -0.004(7) F3 0.140(12) 0.088(11) 0.159(14) 0.041(9) 0.025(9) 0.066(9) F4 0.37(2) 0.093(11) 0.123(13) 0.029(9) 0.140(15) 0.081(14) B2 0.100(19) 0.059(16) 0.025(9) -0.019(10) 0.026(11) -0.040(14) F5 0.066(7) 0.143(12) 0.113(10) -0.060(9) 0.019(7) -0.015(7) F6 0.106(13) 0.45(4) 0.154(18) 0.15(2) -0.030(11) 0.011(16) F7 0.074(8) 0.081(9) 0.168(13) 0.045(8) 0.060(8) 0.015(7) F8 0.178(15) 0.117(14) 0.25(2) -0.022(13) 0.120(15) -0.038(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N31 1.924(13) . ? Cu1 N11 1.988(12) . ? Cu1 N1 2.221(14) . ? Cu1 N3 2.406(14) 2 ? C1 N1 1.479(19) . ? C1 N3 1.507(17) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? N1 C11 1.501(19) . ? N1 C2 1.557(17) . ? C11 C12 1.49(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N11 1.313(18) . ? C12 C13 1.39(2) . ? C13 C14 1.33(2) . ? C13 H13 0.9500 . ? C14 C15 1.36(2) . ? C14 H14 0.9500 . ? C15 C16 1.37(2) . ? C15 H15 0.9500 . ? C16 N11 1.34(2) . ? C16 H16 0.9500 . ? C2 N2 1.485(18) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N2 C21 1.373(17) . ? N2 C3 1.480(17) . ? C21 C22 1.52(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 N21 1.32(2) . ? C22 C23 1.44(3) . ? C23 C24 1.33(3) . ? C23 H23 0.9500 . ? C24 C25 1.25(3) . ? C24 H24 0.9500 . ? C25 C26 1.38(3) . ? C25 H25 0.9500 . ? C26 N21 1.40(2) . ? C26 H26 0.9500 . ? C3 N3 1.467(19) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N3 C31 1.48(2) 2_545 ? N3 Cu1 2.406(14) 2_545 ? C31 N3 1.48(2) 2 ? C31 C32 1.55(2) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 N31 1.351(18) . ? C32 C33 1.38(2) . ? C33 C34 1.34(2) . ? C33 H33 0.9500 . ? C34 C35 1.48(2) . ? C34 H34 0.9500 . ? C35 C36 1.34(2) . ? C35 H35 0.9500 . ? C36 N31 1.358(19) . ? C36 H36 0.9500 . ? Cu2 N41 1.953(12) . ? Cu2 N51 1.975(14) . ? Cu2 N5 2.273(13) . ? Cu2 N4 2.412(12) 2_646 ? C4 N4 1.449(17) . ? C4 N6 1.468(19) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N4 C41 1.507(17) 2_656 ? N4 C5 1.555(17) . ? N4 Cu2 2.412(12) 2_656 ? C41 N4 1.507(17) 2_646 ? C41 C42 1.53(2) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 N41 1.292(19) . ? C42 C43 1.36(2) . ? C43 C44 1.35(2) . ? C43 H43 0.9500 . ? C44 C45 1.31(2) . ? C44 H44 0.9500 . ? C45 C46 1.37(2) . ? C45 H45 0.9500 . ? C46 N41 1.337(17) . ? C46 H46 0.9500 . ? C5 N5 1.443(18) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? N5 C6 1.384(17) . ? N5 C51 1.547(19) . ? C51 C52 1.46(2) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 N51 1.311(17) . ? C52 C53 1.42(2) . ? C53 C54 1.38(2) . ? C53 H53 0.9500 . ? C54 C55 1.36(2) . ? C54 H54 0.9500 . ? C55 C56 1.38(2) . ? C55 H55 0.9500 . ? C56 N51 1.355(19) . ? C56 H56 0.9500 . ? C6 N6 1.437(18) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? N6 C61 1.462(19) . ? C61 C62 1.51(2) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 N61 1.262(18) . ? C62 C63 1.35(2) . ? C63 C64 1.42(3) . ? C63 H63 0.9500 . ? C64 C65 1.33(3) . ? C64 H64 0.9500 . ? C65 C66 1.20(2) . ? C65 H65 0.9500 . ? C66 N61 1.47(2) . ? C66 H66 0.9500 . ? B1 F3 1.26(3) . ? B1 F1 1.29(2) . ? B1 F2 1.41(2) . ? B1 F4 1.42(2) . ? B2 F6 1.25(2) . ? B2 F8 1.27(3) . ? B2 F7 1.35(2) . ? B2 F5 1.38(2) . ? 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 N31 Cu1 N11 157.8(6) . . ? N31 Cu1 N1 120.0(5) . . ? N11 Cu1 N1 79.8(5) . . ? N31 Cu1 N3 78.7(5) . 2 ? N11 Cu1 N3 98.9(5) . 2 ? N1 Cu1 N3 124.1(5) . 2 ? N1 C1 N3 116.7(11) . . ? N1 C1 H1A 108.1 . . ? N3 C1 H1A 108.1 . . ? N1 C1 H1B 108.1 . . ? N3 C1 H1B 108.1 . . ? H1A C1 H1B 107.3 . . ? C1 N1 C11 114.9(12) . . ? C1 N1 C2 109.7(13) . . ? C11 N1 C2 109.0(10) . . ? C1 N1 Cu1 116.7(7) . . ? C11 N1 Cu1 104.0(10) . . ? C2 N1 Cu1 101.5(9) . . ? C12 C11 N1 108.5(12) . . ? C12 C11 H11A 110.0 . . ? N1 C11 H11A 110.0 . . ? C12 C11 H11B 110.0 . . ? N1 C11 H11B 110.0 . . ? H11A C11 H11B 108.4 . . ? N11 C12 C13 117.3(16) . . ? N11 C12 C11 121.8(13) . . ? C13 C12 C11 120.5(14) . . ? C14 C13 C12 123.0(17) . . ? C14 C13 H13 118.5 . . ? C12 C13 H13 118.5 . . ? C13 C14 C15 119.4(16) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C14 C15 C16 115.2(17) . . ? C14 C15 H15 122.4 . . ? C16 C15 H15 122.4 . . ? N11 C16 C15 124.7(18) . . ? N11 C16 H16 117.6 . . ? C15 C16 H16 117.6 . . ? C12 N11 C16 119.0(14) . . ? C12 N11 Cu1 113.8(11) . . ? C16 N11 Cu1 126.5(12) . . ? N2 C2 N1 110.0(12) . . ? N2 C2 H2A 109.7 . . ? N1 C2 H2A 109.7 . . ? N2 C2 H2B 109.7 . . ? N1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C21 N2 C3 113.1(13) . . ? C21 N2 C2 113.9(12) . . ? C3 N2 C2 105.1(11) . . ? N2 C21 C22 115.0(15) . . ? N2 C21 H21A 108.5 . . ? C22 C21 H21A 108.5 . . ? N2 C21 H21B 108.5 . . ? C22 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? N21 C22 C23 127(2) . . ? N21 C22 C21 113.2(19) . . ? C23 C22 C21 119.9(18) . . ? C24 C23 C22 112(2) . . ? C24 C23 H23 123.9 . . ? C22 C23 H23 123.9 . . ? C25 C24 C23 126(3) . . ? C25 C24 H24 117.0 . . ? C23 C24 H24 117.0 . . ? C24 C25 C26 120(2) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 N21 121(2) . . ? C25 C26 H26 119.4 . . ? N21 C26 H26 119.4 . . ? C22 N21 C26 113.1(18) . . ? N3 C3 N2 115.7(13) . . ? N3 C3 H3A 108.4 . . ? N2 C3 H3A 108.4 . . ? N3 C3 H3B 108.4 . . ? N2 C3 H3B 108.4 . . ? H3A C3 H3B 107.4 . . ? C3 N3 C31 110.8(12) . 2_545 ? C3 N3 C1 107.8(13) . . ? C31 N3 C1 115.0(13) 2_545 . ? C3 N3 Cu1 119.3(10) . 2_545 ? C31 N3 Cu1 95.9(9) 2_545 2_545 ? C1 N3 Cu1 108.0(8) . 2_545 ? N3 C31 C32 108.5(13) 2 . ? N3 C31 H31A 110.0 2 . ? C32 C31 H31A 110.0 . . ? N3 C31 H31B 110.0 2 . ? C32 C31 H31B 110.0 . . ? H31A C31 H31B 108.4 . . ? N31 C32 C33 123.5(16) . . ? N31 C32 C31 115.2(15) . . ? C33 C32 C31 121.1(13) . . ? C34 C33 C32 122.8(14) . . ? C34 C33 H33 118.6 . . ? C32 C33 H33 118.6 . . ? C33 C34 C35 114.3(14) . . ? C33 C34 H34 122.9 . . ? C35 C34 H34 122.9 . . ? C36 C35 C34 119.1(15) . . ? C36 C35 H35 120.5 . . ? C34 C35 H35 120.5 . . ? C35 C36 N31 125.0(15) . . ? C35 C36 H36 117.5 . . ? N31 C36 H36 117.5 . . ? C32 N31 C36 115.2(15) . . ? C32 N31 Cu1 118.7(12) . . ? C36 N31 Cu1 126.1(11) . . ? N41 Cu2 N51 152.0(6) . . ? N41 Cu2 N5 124.9(5) . . ? N51 Cu2 N5 79.3(5) . . ? N41 Cu2 N4 78.0(5) . 2_646 ? N51 Cu2 N4 99.0(5) . 2_646 ? N5 Cu2 N4 127.6(5) . 2_646 ? N4 C4 N6 115.3(12) . . ? N4 C4 H4A 108.5 . . ? N6 C4 H4A 108.5 . . ? N4 C4 H4B 108.5 . . ? N6 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? C4 N4 C41 112.6(12) . 2_656 ? C4 N4 C5 104.2(10) . . ? C41 N4 C5 111.0(11) 2_656 . ? C4 N4 Cu2 120.8(10) . 2_656 ? C41 N4 Cu2 96.1(8) 2_656 2_656 ? C5 N4 Cu2 112.2(9) . 2_656 ? N4 C41 C42 107.6(12) 2_646 . ? N4 C41 H41A 110.2 2_646 . ? C42 C41 H41A 110.2 . . ? N4 C41 H41B 110.2 2_646 . ? C42 C41 H41B 110.2 . . ? H41A C41 H41B 108.5 . . ? N41 C42 C43 124.6(16) . . ? N41 C42 C41 117.8(15) . . ? C43 C42 C41 116.6(15) . . ? C44 C43 C42 112.8(17) . . ? C44 C43 H43 123.6 . . ? C42 C43 H43 123.6 . . ? C45 C44 C43 126.7(19) . . ? C45 C44 H44 116.7 . . ? C43 C44 H44 116.7 . . ? C44 C45 C46 114.4(18) . . ? C44 C45 H45 122.8 . . ? C46 C45 H45 122.8 . . ? N41 C46 C45 122.3(14) . . ? N41 C46 H46 118.9 . . ? C45 C46 H46 118.9 . . ? C42 N41 C46 118.1(14) . . ? C42 N41 Cu2 118.8(12) . . ? C46 N41 Cu2 123.0(10) . . ? N5 C5 N4 116.9(12) . . ? N5 C5 H5A 108.1 . . ? N4 C5 H5A 108.1 . . ? N5 C5 H5B 108.1 . . ? N4 C5 H5B 108.1 . . ? H5A C5 H5B 107.3 . . ? C6 N5 C5 113.2(13) . . ? C6 N5 C51 112.7(12) . . ? C5 N5 C51 113.0(11) . . ? C6 N5 Cu2 108.3(9) . . ? C5 N5 Cu2 110.4(9) . . ? C51 N5 Cu2 98.1(9) . . ? C52 C51 N5 111.7(12) . . ? C52 C51 H51A 109.3 . . ? N5 C51 H51A 109.3 . . ? C52 C51 H51B 109.3 . . ? N5 C51 H51B 109.3 . . ? H51A C51 H51B 107.9 . . ? N51 C52 C53 121.8(17) . . ? N51 C52 C51 117.7(15) . . ? C53 C52 C51 120.5(14) . . ? C54 C53 C52 118.2(19) . . ? C54 C53 H53 120.9 . . ? C52 C53 H53 120.9 . . ? C55 C54 C53 119.6(18) . . ? C55 C54 H54 120.2 . . ? C53 C54 H54 120.2 . . ? C54 C55 C56 119.2(16) . . ? C54 C55 H55 120.4 . . ? C56 C55 H55 120.4 . . ? N51 C56 C55 122.6(16) . . ? N51 C56 H56 118.7 . . ? C55 C56 H56 118.7 . . ? C52 N51 C56 118.5(15) . . ? C52 N51 Cu2 116.9(13) . . ? C56 N51 Cu2 123.9(11) . . ? N5 C6 N6 110.8(12) . . ? N5 C6 H6A 109.5 . . ? N6 C6 H6A 109.5 . . ? N5 C6 H6B 109.5 . . ? N6 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C6 N6 C61 114.6(11) . . ? C6 N6 C4 106.5(12) . . ? C61 N6 C4 110.5(12) . . ? N6 C61 C62 120.3(12) . . ? N6 C61 H61A 107.3 . . ? C62 C61 H61A 107.3 . . ? N6 C61 H61B 107.3 . . ? C62 C61 H61B 107.3 . . ? H61A C61 H61B 106.9 . . ? N61 C62 C63 119.5(17) . . ? N61 C62 C61 117.3(14) . . ? C63 C62 C61 123.1(16) . . ? C62 C63 C64 123(2) . . ? C62 C63 H63 118.4 . . ? C64 C63 H63 118.4 . . ? C65 C64 C63 113.0(16) . . ? C65 C64 H64 123.5 . . ? C63 C64 H64 123.5 . . ? C66 C65 C64 123(2) . . ? C66 C65 H65 118.4 . . ? C64 C65 H65 118.4 . . ? C65 C66 N61 124(2) . . ? C65 C66 H66 118.2 . . ? N61 C66 H66 118.2 . . ? C62 N61 C66 116.0(15) . . ? F3 B1 F1 119.2(19) . . ? F3 B1 F2 110.6(19) . . ? F1 B1 F2 97.1(18) . . ? F3 B1 F4 115.8(19) . . ? F1 B1 F4 105(2) . . ? F2 B1 F4 106.5(18) . . ? F6 B2 F8 109(2) . . ? F6 B2 F7 114.9(19) . . ? F8 B2 F7 107(2) . . ? F6 B2 F5 108(2) . . ? F8 B2 F5 104.1(18) . . ? F7 B2 F5 113.3(14) . . ? _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 25.21 _diffrn_measured_fraction_theta_full 0.914 _refine_diff_density_max 1.493 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.136 #============================================================================== #_eof # End of Crystallographic Information File #============================================================================== data_pan12 _database_code_CSD 204544 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H24 Cl2 Cu N6' _chemical_formula_sum 'C21 H24 Cl2 Cu N6' _chemical_formula_weight 494.90 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' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.56100(10) _cell_length_b 15.7360(3) _cell_length_c 15.8740(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.0570(7) _cell_angle_gamma 90.00 _cell_volume 2138.48(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 21162 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.5 _exptl_crystal_description rhombohedral _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1020 _exptl_absorpt_coefficient_mu 1.293 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7821 _exptl_absorpt_correction_T_max 0.8007 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method \f-rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 31384 _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.35 _diffrn_reflns_theta_max 27.53 _reflns_number_total 4893 _reflns_number_gt 4305 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius program suite version 1.9 (1997)' _computing_cell_refinement 'Collect, Nonius program suite version 1.9 (1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement ; SHELX97-2 Program for Crystal Structure Analysis. G. M. Sheldrick, Institut f. Anorg. Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998. ; _computing_molecular_graphics 'ORTEP3 for Windows - L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material 'SHELX97-2, G. M. Sheldrick' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+1.4344P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4893 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0793 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.62391(2) 0.178761(13) 1.035637(13) 0.01698(7) Uani 1 1 d . . . Cl1 Cl 0.65412(5) 0.31179(3) 1.11715(3) 0.02482(11) Uani 1 1 d . . . Cl2 Cl 0.38457(5) 0.11788(4) 1.06698(3) 0.03376(13) Uani 1 1 d . . . C1 C 0.9036(2) 0.26321(11) 0.93394(11) 0.0207(3) Uani 1 1 d . . . H1A H 0.8816 0.3147 0.9678 0.025 Uiso 1 1 calc R . . H1B H 1.0178 0.2603 0.9248 0.025 Uiso 1 1 calc R . . N1 N 0.82565(17) 0.27073(9) 0.85275(9) 0.0200(3) Uani 1 1 d . . . C11 C 0.8916(2) 0.34238(12) 0.80586(12) 0.0250(4) Uani 1 1 d . . . H11A H 0.8431 0.3445 0.7493 0.030 Uiso 1 1 calc R . . H11B H 1.0050 0.3329 0.7982 0.030 Uiso 1 1 calc R . . C12 C 0.8672(2) 0.42670(12) 0.84898(12) 0.0240(4) Uani 1 1 d . . . N11 N 0.9956(2) 0.47225(12) 0.86434(11) 0.0310(4) Uani 1 1 d . . . C13 C 0.7005(3) 0.53550(15) 0.90381(17) 0.0406(5) Uani 1 1 d . . . H13 H 0.5997 0.5569 0.9170 0.049 Uiso 1 1 calc R . . C14 C 0.8347(3) 0.58397(14) 0.91861(14) 0.0374(5) Uani 1 1 d . . . H14 H 0.8270 0.6396 0.9416 0.045 Uiso 1 1 calc R . . C15 C 0.9758(3) 0.55012(15) 0.89956(13) 0.0346(5) Uani 1 1 d . . . H15 H 1.0664 0.5829 0.9116 0.041 Uiso 1 1 calc R . . C16 C 0.7191(2) 0.45521(14) 0.86925(15) 0.0356(5) Uani 1 1 d . . . H16 H 0.6308 0.4200 0.8596 0.043 Uiso 1 1 calc R . . C2 C 0.8490(2) 0.19266(12) 0.80269(12) 0.0235(4) Uani 1 1 d . . . H2A H 0.7912 0.1975 0.7488 0.028 Uiso 1 1 calc R . . H2B H 0.9613 0.1861 0.7895 0.028 Uiso 1 1 calc R . . N2 N 0.79488(18) 0.11871(10) 0.84815(10) 0.0218(3) Uani 1 1 d . . . C21 C 0.6247(2) 0.10612(12) 0.84895(12) 0.0227(4) Uani 1 1 d . . . H21A H 0.5996 0.0666 0.8955 0.027 Uiso 1 1 calc R . . H21B H 0.5950 0.0775 0.7957 0.027 Uiso 1 1 calc R . . C22 C 0.5227(2) 0.18387(11) 0.85866(11) 0.0206(3) Uani 1 1 d . . . N21 N 0.52059(16) 0.22536(10) 0.93325(9) 0.0193(3) Uani 1 1 d . . . C23 C 0.4312(2) 0.29439(12) 0.94202(12) 0.0222(4) Uani 1 1 d . . . H23 H 0.4329 0.3238 0.9943 0.027 Uiso 1 1 calc R . . C24 C 0.3360(2) 0.32488(13) 0.87793(12) 0.0258(4) Uani 1 1 d . . . H24 H 0.2740 0.3743 0.8858 0.031 Uiso 1 1 calc R . . C25 C 0.3341(2) 0.28112(13) 0.80221(12) 0.0265(4) Uani 1 1 d . . . H25 H 0.2681 0.2992 0.7575 0.032 Uiso 1 1 calc R . . C26 C 0.4290(2) 0.21108(13) 0.79239(12) 0.0246(4) Uani 1 1 d . . . H26 H 0.4304 0.1814 0.7403 0.030 Uiso 1 1 calc R . . C3 C 0.8753(2) 0.11050(11) 0.92684(11) 0.0210(3) Uani 1 1 d . . . H3A H 0.9883 0.1026 0.9160 0.025 Uiso 1 1 calc R . . H3B H 0.8367 0.0594 0.9566 0.025 Uiso 1 1 calc R . . N3 N 0.85268(16) 0.18693(9) 0.98196(9) 0.0173(3) Uani 1 1 d . . . C31 C 0.9574(2) 0.18098(11) 1.05613(11) 0.0203(3) Uani 1 1 d . . . H31A H 0.9607 0.2364 1.0856 0.024 Uiso 1 1 calc R . . H31B H 1.0647 0.1670 1.0375 0.024 Uiso 1 1 calc R . . C32 C 0.8995(2) 0.11357(11) 1.11515(11) 0.0190(3) Uani 1 1 d . . . N31 N 0.74240(17) 0.10395(9) 1.11700(9) 0.0188(3) Uani 1 1 d . . . C33 C 0.6812(2) 0.04750(12) 1.17122(11) 0.0227(4) Uani 1 1 d . . . H33 H 0.5709 0.0412 1.1735 0.027 Uiso 1 1 calc R . . C34 C 0.7731(2) -0.00191(12) 1.22408(12) 0.0249(4) Uani 1 1 d . . . H34 H 0.7266 -0.0411 1.2620 0.030 Uiso 1 1 calc R . . C35 C 0.9334(2) 0.00705(12) 1.22047(12) 0.0254(4) Uani 1 1 d . . . H35 H 0.9987 -0.0267 1.2554 0.031 Uiso 1 1 calc R . . C36 C 0.9982(2) 0.06565(12) 1.16551(11) 0.0232(4) Uani 1 1 d . . . H36 H 1.1082 0.0728 1.1624 0.028 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.01493(11) 0.01986(12) 0.01614(11) 0.00067(8) -0.00022(8) 0.00051(7) Cl1 0.0272(2) 0.0249(2) 0.0224(2) -0.00564(16) -0.00390(16) 0.00415(16) Cl2 0.0174(2) 0.0464(3) 0.0375(3) 0.0170(2) 0.00091(18) -0.00311(19) C1 0.0212(8) 0.0197(8) 0.0212(8) 0.0015(7) 0.0011(6) -0.0026(6) N1 0.0228(7) 0.0193(7) 0.0179(7) 0.0013(6) 0.0024(5) -0.0017(6) C11 0.0275(9) 0.0233(9) 0.0241(9) 0.0038(7) 0.0051(7) -0.0015(7) C12 0.0284(9) 0.0222(9) 0.0213(9) 0.0052(7) 0.0014(7) -0.0006(7) N11 0.0308(9) 0.0325(9) 0.0296(9) -0.0007(7) 0.0040(7) -0.0048(7) C13 0.0326(11) 0.0341(12) 0.0551(14) -0.0108(10) -0.0028(10) 0.0045(9) C14 0.0486(13) 0.0271(11) 0.0366(12) -0.0075(9) 0.0000(10) -0.0021(9) C15 0.0352(11) 0.0389(12) 0.0296(10) -0.0059(9) 0.0054(8) -0.0168(9) C16 0.0264(10) 0.0305(11) 0.0498(13) -0.0059(10) -0.0038(9) -0.0022(8) C2 0.0250(9) 0.0242(9) 0.0212(9) -0.0016(7) 0.0046(7) 0.0005(7) N2 0.0235(7) 0.0205(7) 0.0213(7) -0.0015(6) 0.0023(6) -0.0003(6) C21 0.0261(9) 0.0205(9) 0.0214(8) -0.0024(7) -0.0015(7) -0.0028(7) C22 0.0193(8) 0.0232(9) 0.0193(8) 0.0002(7) -0.0006(6) -0.0053(6) N21 0.0160(7) 0.0230(7) 0.0189(7) 0.0007(6) -0.0005(5) -0.0013(6) C23 0.0190(8) 0.0253(9) 0.0224(9) -0.0006(7) 0.0007(7) 0.0016(7) C24 0.0201(9) 0.0297(10) 0.0276(10) 0.0052(8) 0.0000(7) 0.0023(7) C25 0.0221(9) 0.0351(10) 0.0225(9) 0.0080(8) -0.0031(7) -0.0016(8) C26 0.0259(9) 0.0289(10) 0.0191(8) 0.0018(7) -0.0039(7) -0.0050(7) C3 0.0221(8) 0.0188(8) 0.0221(9) -0.0031(7) 0.0035(6) 0.0035(7) N3 0.0173(7) 0.0173(7) 0.0173(7) -0.0002(5) 0.0005(5) -0.0007(5) C31 0.0165(8) 0.0236(9) 0.0207(8) 0.0011(7) -0.0013(6) 0.0000(6) C32 0.0191(8) 0.0194(8) 0.0185(8) -0.0031(6) 0.0011(6) 0.0014(6) N31 0.0175(7) 0.0194(7) 0.0193(7) -0.0008(6) 0.0006(5) -0.0004(5) C33 0.0227(9) 0.0223(9) 0.0231(9) 0.0013(7) 0.0006(7) -0.0020(7) C34 0.0326(10) 0.0198(9) 0.0222(9) 0.0028(7) 0.0018(7) -0.0011(7) C35 0.0303(10) 0.0232(9) 0.0227(9) -0.0002(7) -0.0013(7) 0.0078(7) C36 0.0206(8) 0.0263(9) 0.0227(9) -0.0016(7) -0.0007(7) 0.0050(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Cu N21 1.9896(14) . ? Cu N31 2.0200(15) . ? Cu N3 2.1405(15) . ? Cu Cl2 2.3164(5) . ? Cu Cl1 2.4743(5) . ? C1 N1 1.455(2) . ? C1 N3 1.487(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? N1 C11 1.465(2) . ? N1 C2 1.477(2) . ? C11 C12 1.508(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N11 1.335(3) . ? C12 C16 1.383(3) . ? N11 C15 1.358(3) . ? C13 C16 1.387(3) . ? C13 C14 1.399(3) . ? C13 H13 0.9500 . ? C14 C15 1.355(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C2 N2 1.446(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N2 C3 1.432(2) . ? N2 C21 1.470(2) . ? C21 C22 1.511(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 N21 1.352(2) . ? C22 C26 1.390(2) . ? N21 C23 1.336(2) . ? C23 C24 1.388(3) . ? C23 H23 0.9500 . ? C24 C25 1.385(3) . ? C24 H24 0.9500 . ? C25 C26 1.378(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C3 N3 1.500(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N3 C31 1.482(2) . ? C31 C32 1.500(2) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 N31 1.354(2) . ? C32 C36 1.386(2) . ? N31 C33 1.344(2) . ? C33 C34 1.388(3) . ? C33 H33 0.9500 . ? C34 C35 1.381(3) . ? C34 H34 0.9500 . ? C35 C36 1.386(3) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? 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 N21 Cu N31 163.66(6) . . ? N21 Cu N3 93.38(6) . . ? N31 Cu N3 80.24(6) . . ? N21 Cu Cl2 86.29(4) . . ? N31 Cu Cl2 93.75(4) . . ? N3 Cu Cl2 156.96(4) . . ? N21 Cu Cl1 99.30(5) . . ? N31 Cu Cl1 96.12(4) . . ? N3 Cu Cl1 93.56(4) . . ? Cl2 Cu Cl1 109.24(2) . . ? N1 C1 N3 112.66(14) . . ? N1 C1 H1A 109.1 . . ? N3 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? N3 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? C1 N1 C11 109.63(14) . . ? C1 N1 C2 110.30(14) . . ? C11 N1 C2 108.33(14) . . ? N1 C11 C12 113.14(15) . . ? N1 C11 H11A 108.9 . . ? C12 C11 H11A 108.9 . . ? N1 C11 H11B 108.9 . . ? C12 C11 H11B 108.9 . . ? H11A C11 H11B 107.8 . . ? N11 C12 C16 122.58(19) . . ? N11 C12 C11 116.15(17) . . ? C16 C12 C11 121.25(18) . . ? C12 N11 C15 117.17(18) . . ? C16 C13 C14 117.9(2) . . ? C16 C13 H13 121.0 . . ? C14 C13 H13 121.0 . . ? C15 C14 C13 118.7(2) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C14 C15 N11 123.94(19) . . ? C14 C15 H15 118.0 . . ? N11 C15 H15 118.0 . . ? C12 C16 C13 119.6(2) . . ? C12 C16 H16 120.2 . . ? C13 C16 H16 120.2 . . ? N2 C2 N1 110.94(14) . . ? N2 C2 H2A 109.5 . . ? N1 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 108.0 . . ? C3 N2 C2 110.74(15) . . ? C3 N2 C21 117.14(15) . . ? C2 N2 C21 115.51(15) . . ? N2 C21 C22 117.67(15) . . ? N2 C21 H21A 107.9 . . ? C22 C21 H21A 107.9 . . ? N2 C21 H21B 107.9 . . ? C22 C21 H21B 107.9 . . ? H21A C21 H21B 107.2 . . ? N21 C22 C26 120.37(17) . . ? N21 C22 C21 119.25(16) . . ? C26 C22 C21 120.36(16) . . ? C23 N21 C22 119.48(15) . . ? C23 N21 Cu 117.95(12) . . ? C22 N21 Cu 122.07(12) . . ? N21 C23 C24 122.71(17) . . ? N21 C23 H23 118.6 . . ? C24 C23 H23 118.6 . . ? C25 C24 C23 118.06(18) . . ? C25 C24 H24 121.0 . . ? C23 C24 H24 121.0 . . ? C26 C25 C24 119.29(17) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C25 C26 C22 120.05(18) . . ? C25 C26 H26 120.0 . . ? C22 C26 H26 120.0 . . ? N2 C3 N3 111.98(14) . . ? N2 C3 H3A 109.2 . . ? N3 C3 H3A 109.2 . . ? N2 C3 H3B 109.2 . . ? N3 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C31 N3 C1 106.31(13) . . ? C31 N3 C3 109.53(13) . . ? C1 N3 C3 108.06(14) . . ? C31 N3 Cu 103.47(10) . . ? C1 N3 Cu 121.40(11) . . ? C3 N3 Cu 107.63(10) . . ? N3 C31 C32 109.92(14) . . ? N3 C31 H31A 109.7 . . ? C32 C31 H31A 109.7 . . ? N3 C31 H31B 109.7 . . ? C32 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? N31 C32 C36 122.14(17) . . ? N31 C32 C31 114.95(15) . . ? C36 C32 C31 122.90(16) . . ? C33 N31 C32 118.43(15) . . ? C33 N31 Cu 126.79(12) . . ? C32 N31 Cu 114.78(12) . . ? N31 C33 C34 122.43(17) . . ? N31 C33 H33 118.8 . . ? C34 C33 H33 118.8 . . ? C35 C34 C33 118.73(17) . . ? C35 C34 H34 120.6 . . ? C33 C34 H34 120.6 . . ? C34 C35 C36 119.53(17) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C35 C36 C32 118.73(17) . . ? C35 C36 H36 120.6 . . ? C32 C36 H36 120.6 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.717 _refine_diff_density_min -0.511 _refine_diff_density_rms 0.064 #============================================================================== #_eof # End of Crystallographic Information File