# Supplementary Material (ESI) for Green Chemistry # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1048 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Joerg Sundermeyer' 'Thomas Linder' 'Benjamin Oelkers' 'Marion Stricker' _publ_contact_author_name 'Joerg Sundermeyer' _publ_contact_author_email JSU@STAFF.UNI-MARBURG.DE _publ_section_title ; Cu(I)/(II) based catalytic ionic liquids, their metallo-laminate solid state structures and catalytic activities in oxidative methanol carbonylation ; # Attachment 'MarionStricker.cif' data_ms001 _database_code_depnum_ccdc_archive 'CCDC 769702' #TrackingRef 'MarionStricker.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(C16 H31 N2), Cl3 Cu, Cl2 Cu' _chemical_formula_sum 'C48 H93 Cl5 Cu2 N6' _chemical_formula_weight 1058.61 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8041(4) _cell_length_b 12.5714(5) _cell_length_c 25.2820(11) _cell_angle_alpha 89.005(3) _cell_angle_beta 89.757(3) _cell_angle_gamma 86.052(3) _cell_volume 2791.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 26636 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 27.16 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.260 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 1.037 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5569 _exptl_absorpt_correction_T_max 0.7103 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43338 _diffrn_reflns_av_R_equivalents 0.0997 _diffrn_reflns_av_sigmaI/netI 0.0903 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 26.78 _reflns_number_total 11820 _reflns_number_gt 7433 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0454P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11820 _refine_ls_number_parameters 556 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0914 _refine_ls_wR_factor_gt 0.0875 _refine_ls_goodness_of_fit_ref 0.815 _refine_ls_restrained_S_all 0.815 _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 C101 C 0.7013(3) 0.5376(2) 0.41485(10) 0.0328(6) Uani 1 1 d . . . H101 H 0.7919 0.5064 0.4014 0.039 Uiso 1 1 calc R . . C102 C 0.5343(3) 0.6196(2) 0.46747(10) 0.0343(6) Uani 1 1 d . . . H102 H 0.4914 0.6541 0.4967 0.041 Uiso 1 1 calc R . . C103 C 0.4609(3) 0.5942(2) 0.42337(10) 0.0354(6) Uani 1 1 d . . . H103 H 0.3581 0.6090 0.4162 0.042 Uiso 1 1 calc R . . C104 C 0.5389(3) 0.5044(2) 0.33716(10) 0.0346(6) Uani 1 1 d . . . H10A H 0.4331 0.4885 0.3343 0.041 Uiso 1 1 calc R . . H10B H 0.6012 0.4389 0.3314 0.041 Uiso 1 1 calc R . . C105 C 0.5741(3) 0.5850(2) 0.29490(10) 0.0342(6) Uani 1 1 d . . . H10C H 0.6793 0.6024 0.2981 0.041 Uiso 1 1 calc R . . H10D H 0.5099 0.6499 0.2999 0.041 Uiso 1 1 calc R . . C106 C 0.5481(3) 0.5426(2) 0.23941(10) 0.0349(6) Uani 1 1 d . . . H10E H 0.6158 0.4795 0.2341 0.042 Uiso 1 1 calc R . . H10F H 0.4443 0.5218 0.2370 0.042 Uiso 1 1 calc R . . C107 C 0.5751(3) 0.6231(2) 0.19617(10) 0.0354(6) Uani 1 1 d . . . H10G H 0.6777 0.6457 0.1996 0.042 Uiso 1 1 calc R . . H10H H 0.5053 0.6852 0.2012 0.042 Uiso 1 1 calc R . . C108 C 0.5553(3) 0.5826(2) 0.14013(10) 0.0343(6) Uani 1 1 d . . . H10I H 0.6290 0.5229 0.1344 0.041 Uiso 1 1 calc R . . H10J H 0.4545 0.5565 0.1372 0.041 Uiso 1 1 calc R . . C109 C 0.5746(3) 0.6660(2) 0.09734(10) 0.0355(6) Uani 1 1 d . . . H10K H 0.6747 0.6930 0.1007 0.043 Uiso 1 1 calc R . . H10L H 0.4997 0.7251 0.1027 0.043 Uiso 1 1 calc R . . C110 C 0.5575(3) 0.6249(2) 0.04160(10) 0.0334(6) Uani 1 1 d . . . H11A H 0.4574 0.5980 0.0382 0.040 Uiso 1 1 calc R . . H11B H 0.6324 0.5658 0.0362 0.040 Uiso 1 1 calc R . . C111 C 0.5772(3) 0.7094(2) -0.00134(10) 0.0344(6) Uani 1 1 d . . . H11C H 0.5030 0.7688 0.0044 0.041 Uiso 1 1 calc R . . H11D H 0.6777 0.7358 0.0019 0.041 Uiso 1 1 calc R . . C112 C 0.5588(3) 0.6696(2) -0.05709(10) 0.0348(6) Uani 1 1 d . . . H11E H 0.6340 0.6109 -0.0630 0.042 Uiso 1 1 calc R . . H11F H 0.4589 0.6423 -0.0602 0.042 Uiso 1 1 calc R . . C113 C 0.5762(3) 0.7540(2) -0.09982(10) 0.0354(6) Uani 1 1 d . . . H11G H 0.6775 0.7793 -0.0976 0.043 Uiso 1 1 calc R . . H11H H 0.5038 0.8139 -0.0931 0.043 Uiso 1 1 calc R . . C114 C 0.5518(3) 0.7157(2) -0.15554(10) 0.0390(6) Uani 1 1 d . . . H11I H 0.6236 0.6554 -0.1623 0.047 Uiso 1 1 calc R . . H11J H 0.4501 0.6912 -0.1580 0.047 Uiso 1 1 calc R . . C115 C 0.5709(4) 0.7997(3) -0.19750(11) 0.0470(7) Uani 1 1 d . . . H11K H 0.5032 0.8610 -0.1904 0.071 Uiso 1 1 calc R . . H11L H 0.5476 0.7720 -0.2314 0.071 Uiso 1 1 calc R . . H11M H 0.6741 0.8199 -0.1975 0.071 Uiso 1 1 calc R . . C116 C 0.8045(3) 0.5904(2) 0.50108(10) 0.0389(7) Uani 1 1 d . . . H11N H 0.8131 0.5251 0.5214 0.058 Uiso 1 1 calc R . . H11O H 0.7790 0.6490 0.5241 0.058 Uiso 1 1 calc R . . H11P H 0.8998 0.6009 0.4838 0.058 Uiso 1 1 calc R . . C201 C 0.2693(3) 0.1792(2) 0.32679(10) 0.0358(6) Uani 1 1 d . . . H201 H 0.3500 0.2139 0.3405 0.043 Uiso 1 1 calc R . . C202 C 0.1363(3) 0.0590(2) 0.28957(11) 0.0379(6) Uani 1 1 d . . . H202 H 0.1113 -0.0034 0.2735 0.045 Uiso 1 1 calc R . . C203 C 0.0404(3) 0.1439(2) 0.30136(10) 0.0368(6) Uani 1 1 d . . . H203 H -0.0637 0.1510 0.2949 0.044 Uiso 1 1 calc R . . C204 C 0.0641(3) 0.3225(2) 0.34476(11) 0.0395(7) Uani 1 1 d . . . H20A H 0.1472 0.3594 0.3594 0.047 Uiso 1 1 calc R . . H20B H -0.0076 0.3107 0.3731 0.047 Uiso 1 1 calc R . . C205 C -0.0138(3) 0.3919(2) 0.30280(10) 0.0362(6) Uani 1 1 d . . . H20C H -0.0662 0.4528 0.3196 0.043 Uiso 1 1 calc R . . H20D H -0.0902 0.3519 0.2860 0.043 Uiso 1 1 calc R . . C206 C 0.0909(3) 0.4320(2) 0.26051(10) 0.0352(6) Uani 1 1 d . . . H20E H 0.1437 0.3715 0.2435 0.042 Uiso 1 1 calc R . . H20F H 0.1668 0.4730 0.2769 0.042 Uiso 1 1 calc R . . C207 C 0.0054(3) 0.5013(2) 0.21879(11) 0.0391(6) Uani 1 1 d . . . H20G H -0.0794 0.4636 0.2062 0.047 Uiso 1 1 calc R . . H20H H -0.0362 0.5661 0.2353 0.047 Uiso 1 1 calc R . . C208 C 0.1014(3) 0.5317(2) 0.17182(11) 0.0403(7) Uani 1 1 d . . . H20I H 0.1528 0.4674 0.1578 0.048 Uiso 1 1 calc R . . H20J H 0.1789 0.5767 0.1839 0.048 Uiso 1 1 calc R . . C209 C 0.0125(3) 0.5896(2) 0.12753(11) 0.0404(7) Uani 1 1 d . . . H20K H -0.0271 0.6587 0.1399 0.048 Uiso 1 1 calc R . . H20L H -0.0735 0.5493 0.1186 0.048 Uiso 1 1 calc R . . C210 C 0.1072(3) 0.6057(2) 0.07812(11) 0.0412(7) Uani 1 1 d . . . H21A H 0.1559 0.5373 0.0681 0.049 Uiso 1 1 calc R . . H21B H 0.1869 0.6522 0.0864 0.049 Uiso 1 1 calc R . . C211 C 0.0177(3) 0.6530(2) 0.03109(11) 0.0398(7) Uani 1 1 d . . . H21C H -0.0662 0.6091 0.0242 0.048 Uiso 1 1 calc R . . H21D H -0.0252 0.7235 0.0401 0.048 Uiso 1 1 calc R . . C212 C 0.1122(3) 0.6615(2) -0.01880(11) 0.0406(7) Uani 1 1 d . . . H21E H 0.1961 0.7052 -0.0116 0.049 Uiso 1 1 calc R . . H21F H 0.1553 0.5909 -0.0275 0.049 Uiso 1 1 calc R . . C213 C 0.0266(3) 0.7083(2) -0.06645(11) 0.0398(7) Uani 1 1 d . . . H21G H -0.0170 0.7789 -0.0579 0.048 Uiso 1 1 calc R . . H21H H -0.0567 0.6644 -0.0741 0.048 Uiso 1 1 calc R . . C214 C 0.1256(3) 0.7164(2) -0.11561(11) 0.0417(7) Uani 1 1 d . . . H21I H 0.2100 0.7590 -0.1076 0.050 Uiso 1 1 calc R . . H21J H 0.1676 0.6455 -0.1244 0.050 Uiso 1 1 calc R . . C215 C 0.0418(4) 0.7650(2) -0.16333(12) 0.0482(7) Uani 1 1 d . . . H21K H -0.0431 0.7240 -0.1712 0.072 Uiso 1 1 calc R . . H21L H 0.1096 0.7649 -0.1932 0.072 Uiso 1 1 calc R . . H21M H 0.0057 0.8370 -0.1558 0.072 Uiso 1 1 calc R . . C216 C 0.4181(3) 0.0131(2) 0.30114(13) 0.0501(8) Uani 1 1 d . . . H21N H 0.4399 0.0013 0.2644 0.075 Uiso 1 1 calc R . . H21O H 0.4042 -0.0539 0.3187 0.075 Uiso 1 1 calc R . . H21P H 0.5015 0.0460 0.3171 0.075 Uiso 1 1 calc R . . C301 C 0.0357(3) 0.8658(2) 0.43536(10) 0.0326(6) Uani 1 1 d . . . H301 H 0.0416 0.7917 0.4366 0.039 Uiso 1 1 calc R . . C302 C 0.0987(3) 1.0316(2) 0.43513(10) 0.0355(6) Uani 1 1 d . . . H302 H 0.1568 1.0906 0.4361 0.043 Uiso 1 1 calc R . . C303 C -0.0538(3) 1.0331(2) 0.43117(10) 0.0374(6) Uani 1 1 d . . . H303 H -0.1208 1.0935 0.4289 0.045 Uiso 1 1 calc R . . C304 C -0.2466(3) 0.8926(2) 0.42387(11) 0.0377(6) Uani 1 1 d . . . H30A H -0.3208 0.9532 0.4254 0.045 Uiso 1 1 calc R . . H30B H -0.2690 0.8433 0.4523 0.045 Uiso 1 1 calc R . . C305 C -0.2590(3) 0.8377(2) 0.37084(10) 0.0345(6) Uani 1 1 d . . . H30C H -0.1971 0.7708 0.3719 0.041 Uiso 1 1 calc R . . H30D H -0.3638 0.8214 0.3655 0.041 Uiso 1 1 calc R . . C306 C -0.2083(3) 0.9048(2) 0.32422(10) 0.0328(6) Uani 1 1 d . . . H30E H -0.0991 0.9104 0.3265 0.039 Uiso 1 1 calc R . . H30F H -0.2567 0.9761 0.3270 0.039 Uiso 1 1 calc R . . C307 C -0.2450(3) 0.8610(2) 0.27006(10) 0.0338(6) Uani 1 1 d . . . H30G H -0.1882 0.7928 0.2655 0.041 Uiso 1 1 calc R . . H30H H -0.3526 0.8490 0.2686 0.041 Uiso 1 1 calc R . . C308 C -0.2063(3) 0.9358(2) 0.22546(10) 0.0359(6) Uani 1 1 d . . . H30I H -0.0973 0.9428 0.2255 0.043 Uiso 1 1 calc R . . H30J H -0.2557 1.0056 0.2322 0.043 Uiso 1 1 calc R . . C309 C -0.2528(3) 0.9012(2) 0.17084(10) 0.0354(6) Uani 1 1 d . . . H30K H -0.2007 0.8326 0.1633 0.042 Uiso 1 1 calc R . . H30L H -0.3614 0.8923 0.1708 0.042 Uiso 1 1 calc R . . C310 C -0.2162(3) 0.9808(2) 0.12743(10) 0.0380(6) Uani 1 1 d . . . H31A H -0.1078 0.9903 0.1282 0.046 Uiso 1 1 calc R . . H31B H -0.2691 1.0490 0.1351 0.046 Uiso 1 1 calc R . . C311 C -0.2587(3) 0.9490(2) 0.07178(10) 0.0365(6) Uani 1 1 d . . . H31C H -0.2045 0.8815 0.0636 0.044 Uiso 1 1 calc R . . H31D H -0.3668 0.9387 0.0709 0.044 Uiso 1 1 calc R . . C312 C -0.2227(3) 1.0306(2) 0.02973(10) 0.0388(6) Uani 1 1 d . . . H31E H -0.1150 1.0419 0.0314 0.047 Uiso 1 1 calc R . . H31F H -0.2783 1.0977 0.0378 0.047 Uiso 1 1 calc R . . C313 C -0.2611(3) 1.0006(2) -0.02654(10) 0.0381(6) Uani 1 1 d . . . H31G H -0.2057 0.9335 -0.0348 0.046 Uiso 1 1 calc R . . H31H H -0.3689 0.9897 -0.0284 0.046 Uiso 1 1 calc R . . C314 C -0.2236(3) 1.0831(2) -0.06787(10) 0.0425(7) Uani 1 1 d . . . H31I H -0.1156 1.0936 -0.0662 0.051 Uiso 1 1 calc R . . H31J H -0.2784 1.1503 -0.0595 0.051 Uiso 1 1 calc R . . C315 C -0.2631(4) 1.0531(3) -0.12401(11) 0.0507(8) Uani 1 1 d . . . H31K H -0.2082 0.9872 -0.1328 0.076 Uiso 1 1 calc R . . H31L H -0.2356 1.1083 -0.1482 0.076 Uiso 1 1 calc R . . H31M H -0.3705 1.0450 -0.1263 0.076 Uiso 1 1 calc R . . C316 C 0.3131(3) 0.8879(2) 0.44103(11) 0.0413(7) Uani 1 1 d . . . H31N H 0.3278 0.8426 0.4718 0.062 Uiso 1 1 calc R . . H31O H 0.3752 0.9474 0.4436 0.062 Uiso 1 1 calc R . . H31P H 0.3415 0.8481 0.4100 0.062 Uiso 1 1 calc R . . N101 N 0.5669(2) 0.54210(16) 0.39068(8) 0.0317(5) Uani 1 1 d . . . N102 N 0.6849(2) 0.58475(16) 0.46121(8) 0.0316(5) Uani 1 1 d . . . N201 N 0.1251(2) 0.21773(17) 0.32458(8) 0.0324(5) Uani 1 1 d . . . N202 N 0.2785(2) 0.08332(18) 0.30617(9) 0.0361(5) Uani 1 1 d . . . N301 N -0.0921(2) 0.92930(17) 0.43116(8) 0.0316(5) Uani 1 1 d . . . N302 N 0.1521(2) 0.92679(16) 0.43740(8) 0.0317(5) Uani 1 1 d . . . Cl1 Cl 0.81476(7) 0.30327(5) 0.46457(2) 0.03480(15) Uani 1 1 d . . . Cl2 Cl 0.43523(8) 0.16554(6) 0.44672(3) 0.04169(17) Uani 1 1 d . . . Cl3 Cl 0.65944(7) 0.22443(5) 0.32362(3) 0.03708(15) Uani 1 1 d . . . Cl4 Cl 0.21111(9) 0.78552(6) 0.25611(3) 0.0533(2) Uani 1 1 d . . . Cl5 Cl 0.06828(7) 0.60496(5) 0.38557(3) 0.03770(16) Uani 1 1 d . . . Cu1 Cu 0.64423(4) 0.23719(3) 0.411111(13) 0.03582(9) Uani 1 1 d . . . Cu2 Cu 0.13552(4) 0.69431(3) 0.319336(13) 0.03823(9) 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 C101 0.0365(14) 0.0325(14) 0.0290(13) -0.0026(11) 0.0041(11) 0.0005(11) C102 0.0345(14) 0.0328(14) 0.0348(14) -0.0040(11) 0.0068(11) 0.0046(11) C103 0.0319(14) 0.0364(15) 0.0372(15) -0.0036(12) 0.0034(11) 0.0037(11) C104 0.0435(15) 0.0326(14) 0.0284(13) -0.0062(11) 0.0007(11) -0.0069(11) C105 0.0407(15) 0.0318(14) 0.0300(14) -0.0037(11) 0.0010(11) -0.0009(11) C106 0.0410(15) 0.0344(14) 0.0298(14) -0.0043(11) 0.0035(11) -0.0066(12) C107 0.0413(15) 0.0342(14) 0.0307(14) -0.0043(11) -0.0005(11) -0.0022(12) C108 0.0348(14) 0.0357(14) 0.0324(14) -0.0059(12) 0.0016(11) -0.0021(11) C109 0.0388(15) 0.0357(15) 0.0321(14) -0.0053(12) 0.0012(11) -0.0026(11) C110 0.0350(14) 0.0355(14) 0.0299(13) -0.0055(11) 0.0020(11) -0.0030(11) C111 0.0394(15) 0.0350(14) 0.0291(13) -0.0037(11) 0.0023(11) -0.0032(11) C112 0.0379(14) 0.0369(15) 0.0295(14) -0.0051(11) 0.0029(11) -0.0011(11) C113 0.0375(14) 0.0372(15) 0.0315(14) -0.0035(12) 0.0021(11) -0.0016(12) C114 0.0378(15) 0.0486(17) 0.0303(14) -0.0059(13) 0.0044(12) -0.0011(12) C115 0.0529(18) 0.0552(19) 0.0331(15) -0.0002(14) 0.0031(13) -0.0052(15) C116 0.0392(15) 0.0431(16) 0.0342(15) -0.0069(12) -0.0058(12) 0.0000(12) C201 0.0368(15) 0.0383(15) 0.0330(14) 0.0033(12) 0.0004(11) -0.0084(12) C202 0.0388(15) 0.0374(15) 0.0379(15) -0.0043(12) 0.0005(12) -0.0042(12) C203 0.0359(14) 0.0347(14) 0.0399(15) -0.0053(12) -0.0001(12) -0.0026(11) C204 0.0455(16) 0.0385(15) 0.0348(15) -0.0126(12) 0.0119(12) -0.0034(12) C205 0.0407(15) 0.0325(14) 0.0361(15) -0.0104(12) 0.0079(12) -0.0052(11) C206 0.0358(14) 0.0328(14) 0.0375(15) -0.0105(12) 0.0049(12) -0.0044(11) C207 0.0369(14) 0.0340(15) 0.0464(16) -0.0093(13) 0.0087(12) -0.0023(12) C208 0.0402(15) 0.0351(15) 0.0454(17) -0.0054(13) 0.0076(13) -0.0013(12) C209 0.0399(15) 0.0362(15) 0.0449(16) -0.0038(13) 0.0058(13) -0.0007(12) C210 0.0416(16) 0.0361(15) 0.0455(16) 0.0007(13) 0.0073(13) -0.0010(12) C211 0.0380(15) 0.0354(15) 0.0456(16) -0.0026(13) 0.0039(13) 0.0017(12) C212 0.0403(15) 0.0365(15) 0.0447(16) -0.0044(13) 0.0056(13) -0.0007(12) C213 0.0399(15) 0.0329(15) 0.0468(17) -0.0053(13) 0.0007(13) -0.0029(12) C214 0.0492(17) 0.0332(15) 0.0426(16) -0.0063(13) 0.0005(13) -0.0015(12) C215 0.0597(19) 0.0410(17) 0.0445(17) -0.0048(14) -0.0059(15) -0.0056(14) C216 0.0339(15) 0.0417(17) 0.073(2) 0.0055(16) 0.0018(15) 0.0068(13) C301 0.0402(15) 0.0276(13) 0.0301(13) -0.0047(11) 0.0020(11) -0.0009(11) C302 0.0456(16) 0.0289(14) 0.0324(14) -0.0031(11) 0.0003(12) -0.0057(11) C303 0.0440(16) 0.0314(14) 0.0366(15) -0.0041(12) 0.0030(12) 0.0011(12) C304 0.0326(14) 0.0435(16) 0.0373(15) -0.0050(13) 0.0049(12) -0.0030(12) C305 0.0343(14) 0.0353(14) 0.0341(14) -0.0040(12) 0.0005(11) -0.0028(11) C306 0.0339(14) 0.0318(14) 0.0325(14) -0.0037(11) -0.0001(11) -0.0013(11) C307 0.0373(14) 0.0313(14) 0.0328(14) -0.0044(11) -0.0015(11) -0.0011(11) C308 0.0391(15) 0.0345(14) 0.0343(14) -0.0044(12) -0.0007(12) -0.0035(11) C309 0.0405(15) 0.0326(14) 0.0332(14) -0.0030(11) -0.0004(12) -0.0020(11) C310 0.0457(16) 0.0342(15) 0.0340(15) -0.0059(12) 0.0021(12) -0.0021(12) C311 0.0399(15) 0.0364(15) 0.0330(14) -0.0050(12) 0.0011(12) 0.0004(12) C312 0.0481(16) 0.0351(15) 0.0331(14) -0.0056(12) 0.0019(12) 0.0000(12) C313 0.0416(15) 0.0382(15) 0.0340(14) -0.0053(12) 0.0009(12) 0.0019(12) C314 0.0531(17) 0.0393(16) 0.0342(15) -0.0037(13) 0.0057(13) 0.0025(13) C315 0.0595(19) 0.057(2) 0.0343(16) -0.0009(14) 0.0042(14) 0.0027(15) C316 0.0350(15) 0.0428(16) 0.0457(16) 0.0023(13) -0.0003(12) -0.0012(12) N101 0.0361(12) 0.0314(11) 0.0275(11) -0.0036(9) 0.0038(9) -0.0012(9) N102 0.0344(11) 0.0316(11) 0.0288(11) -0.0053(9) 0.0038(9) -0.0004(9) N201 0.0329(12) 0.0366(12) 0.0281(11) -0.0058(9) 0.0040(9) -0.0054(9) N202 0.0307(11) 0.0390(13) 0.0385(13) 0.0006(10) 0.0011(10) -0.0015(9) N301 0.0349(12) 0.0336(12) 0.0264(11) -0.0060(9) 0.0017(9) -0.0019(9) N302 0.0374(12) 0.0298(11) 0.0279(11) -0.0023(9) 0.0029(9) -0.0019(9) Cl1 0.0368(3) 0.0344(3) 0.0336(3) -0.0060(3) 0.0029(3) -0.0044(3) Cl2 0.0462(4) 0.0474(4) 0.0334(3) -0.0046(3) 0.0028(3) -0.0168(3) Cl3 0.0355(3) 0.0407(4) 0.0357(3) -0.0096(3) 0.0060(3) -0.0048(3) Cl4 0.0668(5) 0.0386(4) 0.0536(5) 0.0005(3) 0.0180(4) 0.0018(3) Cl5 0.0396(4) 0.0364(4) 0.0375(4) -0.0077(3) 0.0020(3) -0.0037(3) Cu1 0.03891(19) 0.03082(17) 0.03758(19) -0.00621(14) 0.00014(14) 0.00011(14) Cu2 0.04103(19) 0.03413(18) 0.03937(19) -0.00649(15) 0.00437(15) -0.00026(14) _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 C101 N102 1.326(3) . ? C101 N101 1.331(3) . ? C101 H101 0.9300 . ? C102 C103 1.345(3) . ? C102 N102 1.377(3) . ? C102 H102 0.9300 . ? C103 N101 1.382(3) . ? C103 H103 0.9300 . ? C104 N101 1.469(3) . ? C104 C105 1.506(4) . ? C104 H10A 0.9700 . ? C104 H10B 0.9700 . ? C105 C106 1.533(3) . ? C105 H10C 0.9700 . ? C105 H10D 0.9700 . ? C106 C107 1.506(4) . ? C106 H10E 0.9700 . ? C106 H10F 0.9700 . ? C107 C108 1.529(3) . ? C107 H10G 0.9700 . ? C107 H10H 0.9700 . ? C108 C109 1.511(4) . ? C108 H10I 0.9700 . ? C108 H10J 0.9700 . ? C109 C110 1.521(3) . ? C109 H10K 0.9700 . ? C109 H10L 0.9700 . ? C110 C111 1.524(4) . ? C110 H11A 0.9700 . ? C110 H11B 0.9700 . ? C111 C112 1.517(3) . ? C111 H11C 0.9700 . ? C111 H11D 0.9700 . ? C112 C113 1.515(4) . ? C112 H11E 0.9700 . ? C112 H11F 0.9700 . ? C113 C114 1.517(3) . ? C113 H11G 0.9700 . ? C113 H11H 0.9700 . ? C114 C115 1.501(4) . ? C114 H11I 0.9700 . ? C114 H11J 0.9700 . ? C115 H11K 0.9600 . ? C115 H11L 0.9600 . ? C115 H11M 0.9600 . ? C116 N102 1.467(3) . ? C116 H11N 0.9600 . ? C116 H11O 0.9600 . ? C116 H11P 0.9600 . ? C201 N202 1.319(3) . ? C201 N201 1.329(3) . ? C201 H201 0.9300 . ? C202 C203 1.351(3) . ? C202 N202 1.378(3) . ? C202 H202 0.9300 . ? C203 N201 1.371(3) . ? C203 H203 0.9300 . ? C204 N201 1.486(3) . ? C204 C205 1.499(4) . ? C204 H20A 0.9700 . ? C204 H20B 0.9700 . ? C205 C206 1.511(4) . ? C205 H20C 0.9700 . ? C205 H20D 0.9700 . ? C206 C207 1.525(4) . ? C206 H20E 0.9700 . ? C206 H20F 0.9700 . ? C207 C208 1.513(4) . ? C207 H20G 0.9700 . ? C207 H20H 0.9700 . ? C208 C209 1.516(4) . ? C208 H20I 0.9700 . ? C208 H20J 0.9700 . ? C209 C210 1.517(4) . ? C209 H20K 0.9700 . ? C209 H20L 0.9700 . ? C210 C211 1.519(4) . ? C210 H21A 0.9700 . ? C210 H21B 0.9700 . ? C211 C212 1.514(4) . ? C211 H21C 0.9700 . ? C211 H21D 0.9700 . ? C212 C213 1.512(4) . ? C212 H21E 0.9700 . ? C212 H21F 0.9700 . ? C213 C214 1.521(4) . ? C213 H21G 0.9700 . ? C213 H21H 0.9700 . ? C214 C215 1.515(4) . ? C214 H21I 0.9700 . ? C214 H21J 0.9700 . ? C215 H21K 0.9600 . ? C215 H21L 0.9600 . ? C215 H21M 0.9600 . ? C216 N202 1.470(3) . ? C216 H21N 0.9600 . ? C216 H21O 0.9600 . ? C216 H21P 0.9600 . ? C301 N302 1.323(3) . ? C301 N301 1.337(3) . ? C301 H301 0.9300 . ? C302 C303 1.345(4) . ? C302 N302 1.368(3) . ? C302 H302 0.9300 . ? C303 N301 1.370(3) . ? C303 H303 0.9300 . ? C304 N301 1.479(3) . ? C304 C305 1.527(3) . ? C304 H30A 0.9700 . ? C304 H30B 0.9700 . ? C305 C306 1.521(4) . ? C305 H30C 0.9700 . ? C305 H30D 0.9700 . ? C306 C307 1.529(3) . ? C306 H30E 0.9700 . ? C306 H30F 0.9700 . ? C307 C308 1.509(4) . ? C307 H30G 0.9700 . ? C307 H30H 0.9700 . ? C308 C309 1.521(3) . ? C308 H30I 0.9700 . ? C308 H30J 0.9700 . ? C309 C310 1.521(4) . ? C309 H30K 0.9700 . ? C309 H30L 0.9700 . ? C310 C311 1.524(3) . ? C310 H31A 0.9700 . ? C310 H31B 0.9700 . ? C311 C312 1.512(4) . ? C311 H31C 0.9700 . ? C311 H31D 0.9700 . ? C312 C313 1.523(3) . ? C312 H31E 0.9700 . ? C312 H31F 0.9700 . ? C313 C314 1.511(4) . ? C313 H31G 0.9700 . ? C313 H31H 0.9700 . ? C314 C315 1.523(4) . ? C314 H31I 0.9700 . ? C314 H31J 0.9700 . ? C315 H31K 0.9600 . ? C315 H31L 0.9600 . ? C315 H31M 0.9600 . ? C316 N302 1.470(3) . ? C316 H31N 0.9600 . ? C316 H31O 0.9600 . ? C316 H31P 0.9600 . ? Cl1 Cu1 2.2359(7) . ? Cl2 Cu1 2.2790(8) . ? Cl3 Cu1 2.2232(7) . ? Cl4 Cu2 2.0845(9) . ? Cl5 Cu2 2.1057(8) . ? 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 N102 C101 N101 108.9(2) . . ? N102 C101 H101 125.5 . . ? N101 C101 H101 125.5 . . ? C103 C102 N102 107.2(2) . . ? C103 C102 H102 126.4 . . ? N102 C102 H102 126.4 . . ? C102 C103 N101 107.2(2) . . ? C102 C103 H103 126.4 . . ? N101 C103 H103 126.4 . . ? N101 C104 C105 112.5(2) . . ? N101 C104 H10A 109.1 . . ? C105 C104 H10A 109.1 . . ? N101 C104 H10B 109.1 . . ? C105 C104 H10B 109.1 . . ? H10A C104 H10B 107.8 . . ? C104 C105 C106 111.5(2) . . ? C104 C105 H10C 109.3 . . ? C106 C105 H10C 109.3 . . ? C104 C105 H10D 109.3 . . ? C106 C105 H10D 109.3 . . ? H10C C105 H10D 108.0 . . ? C107 C106 C105 113.0(2) . . ? C107 C106 H10E 109.0 . . ? C105 C106 H10E 109.0 . . ? C107 C106 H10F 109.0 . . ? C105 C106 H10F 109.0 . . ? H10E C106 H10F 107.8 . . ? C106 C107 C108 114.5(2) . . ? C106 C107 H10G 108.6 . . ? C108 C107 H10G 108.6 . . ? C106 C107 H10H 108.6 . . ? C108 C107 H10H 108.6 . . ? H10G C107 H10H 107.6 . . ? C109 C108 C107 113.8(2) . . ? C109 C108 H10I 108.8 . . ? C107 C108 H10I 108.8 . . ? C109 C108 H10J 108.8 . . ? C107 C108 H10J 108.8 . . ? H10I C108 H10J 107.7 . . ? C108 C109 C110 113.7(2) . . ? C108 C109 H10K 108.8 . . ? C110 C109 H10K 108.8 . . ? C108 C109 H10L 108.8 . . ? C110 C109 H10L 108.8 . . ? H10K C109 H10L 107.7 . . ? C109 C110 C111 113.4(2) . . ? C109 C110 H11A 108.9 . . ? C111 C110 H11A 108.9 . . ? C109 C110 H11B 108.9 . . ? C111 C110 H11B 108.9 . . ? H11A C110 H11B 107.7 . . ? C112 C111 C110 113.9(2) . . ? C112 C111 H11C 108.8 . . ? C110 C111 H11C 108.8 . . ? C112 C111 H11D 108.8 . . ? C110 C111 H11D 108.8 . . ? H11C C111 H11D 107.7 . . ? C113 C112 C111 114.0(2) . . ? C113 C112 H11E 108.8 . . ? C111 C112 H11E 108.8 . . ? C113 C112 H11F 108.8 . . ? C111 C112 H11F 108.8 . . ? H11E C112 H11F 107.7 . . ? C112 C113 C114 114.2(2) . . ? C112 C113 H11G 108.7 . . ? C114 C113 H11G 108.7 . . ? C112 C113 H11H 108.7 . . ? C114 C113 H11H 108.7 . . ? H11G C113 H11H 107.6 . . ? C115 C114 C113 113.6(2) . . ? C115 C114 H11I 108.8 . . ? C113 C114 H11I 108.8 . . ? C115 C114 H11J 108.8 . . ? C113 C114 H11J 108.8 . . ? H11I C114 H11J 107.7 . . ? C114 C115 H11K 109.5 . . ? C114 C115 H11L 109.5 . . ? H11K C115 H11L 109.5 . . ? C114 C115 H11M 109.5 . . ? H11K C115 H11M 109.5 . . ? H11L C115 H11M 109.5 . . ? N102 C116 H11N 109.5 . . ? N102 C116 H11O 109.5 . . ? H11N C116 H11O 109.5 . . ? N102 C116 H11P 109.5 . . ? H11N C116 H11P 109.5 . . ? H11O C116 H11P 109.5 . . ? N202 C201 N201 108.3(2) . . ? N202 C201 H201 125.9 . . ? N201 C201 H201 125.9 . . ? C203 C202 N202 106.2(2) . . ? C203 C202 H202 126.9 . . ? N202 C202 H202 126.9 . . ? C202 C203 N201 107.4(2) . . ? C202 C203 H203 126.3 . . ? N201 C203 H203 126.3 . . ? N201 C204 C205 112.9(2) . . ? N201 C204 H20A 109.0 . . ? C205 C204 H20A 109.0 . . ? N201 C204 H20B 109.0 . . ? C205 C204 H20B 109.0 . . ? H20A C204 H20B 107.8 . . ? C204 C205 C206 114.7(2) . . ? C204 C205 H20C 108.6 . . ? C206 C205 H20C 108.6 . . ? C204 C205 H20D 108.6 . . ? C206 C205 H20D 108.6 . . ? H20C C205 H20D 107.6 . . ? C205 C206 C207 112.3(2) . . ? C205 C206 H20E 109.1 . . ? C207 C206 H20E 109.1 . . ? C205 C206 H20F 109.1 . . ? C207 C206 H20F 109.1 . . ? H20E C206 H20F 107.9 . . ? C208 C207 C206 114.5(2) . . ? C208 C207 H20G 108.6 . . ? C206 C207 H20G 108.6 . . ? C208 C207 H20H 108.6 . . ? C206 C207 H20H 108.6 . . ? H20G C207 H20H 107.6 . . ? C207 C208 C209 114.4(2) . . ? C207 C208 H20I 108.7 . . ? C209 C208 H20I 108.7 . . ? C207 C208 H20J 108.7 . . ? C209 C208 H20J 108.7 . . ? H20I C208 H20J 107.6 . . ? C208 C209 C210 113.2(2) . . ? C208 C209 H20K 108.9 . . ? C210 C209 H20K 108.9 . . ? C208 C209 H20L 108.9 . . ? C210 C209 H20L 108.9 . . ? H20K C209 H20L 107.8 . . ? C209 C210 C211 114.5(2) . . ? C209 C210 H21A 108.6 . . ? C211 C210 H21A 108.6 . . ? C209 C210 H21B 108.6 . . ? C211 C210 H21B 108.6 . . ? H21A C210 H21B 107.6 . . ? C212 C211 C210 113.6(2) . . ? C212 C211 H21C 108.8 . . ? C210 C211 H21C 108.8 . . ? C212 C211 H21D 108.8 . . ? C210 C211 H21D 108.8 . . ? H21C C211 H21D 107.7 . . ? C213 C212 C211 115.0(2) . . ? C213 C212 H21E 108.5 . . ? C211 C212 H21E 108.5 . . ? C213 C212 H21F 108.5 . . ? C211 C212 H21F 108.5 . . ? H21E C212 H21F 107.5 . . ? C212 C213 C214 113.4(2) . . ? C212 C213 H21G 108.9 . . ? C214 C213 H21G 108.9 . . ? C212 C213 H21H 108.9 . . ? C214 C213 H21H 108.9 . . ? H21G C213 H21H 107.7 . . ? C215 C214 C213 113.9(2) . . ? C215 C214 H21I 108.8 . . ? C213 C214 H21I 108.8 . . ? C215 C214 H21J 108.8 . . ? C213 C214 H21J 108.8 . . ? H21I C214 H21J 107.7 . . ? C214 C215 H21K 109.5 . . ? C214 C215 H21L 109.5 . . ? H21K C215 H21L 109.5 . . ? C214 C215 H21M 109.5 . . ? H21K C215 H21M 109.5 . . ? H21L C215 H21M 109.5 . . ? N202 C216 H21N 109.5 . . ? N202 C216 H21O 109.5 . . ? H21N C216 H21O 109.5 . . ? N202 C216 H21P 109.5 . . ? H21N C216 H21P 109.5 . . ? H21O C216 H21P 109.5 . . ? N302 C301 N301 108.1(2) . . ? N302 C301 H301 125.9 . . ? N301 C301 H301 125.9 . . ? C303 C302 N302 107.0(2) . . ? C303 C302 H302 126.5 . . ? N302 C302 H302 126.5 . . ? C302 C303 N301 107.3(2) . . ? C302 C303 H303 126.3 . . ? N301 C303 H303 126.3 . . ? N301 C304 C305 110.8(2) . . ? N301 C304 H30A 109.5 . . ? C305 C304 H30A 109.5 . . ? N301 C304 H30B 109.5 . . ? C305 C304 H30B 109.5 . . ? H30A C304 H30B 108.1 . . ? C306 C305 C304 113.2(2) . . ? C306 C305 H30C 108.9 . . ? C304 C305 H30C 108.9 . . ? C306 C305 H30D 108.9 . . ? C304 C305 H30D 108.9 . . ? H30C C305 H30D 107.8 . . ? C305 C306 C307 114.4(2) . . ? C305 C306 H30E 108.7 . . ? C307 C306 H30E 108.7 . . ? C305 C306 H30F 108.7 . . ? C307 C306 H30F 108.7 . . ? H30E C306 H30F 107.6 . . ? C308 C307 C306 112.1(2) . . ? C308 C307 H30G 109.2 . . ? C306 C307 H30G 109.2 . . ? C308 C307 H30H 109.2 . . ? C306 C307 H30H 109.2 . . ? H30G C307 H30H 107.9 . . ? C307 C308 C309 114.7(2) . . ? C307 C308 H30I 108.6 . . ? C309 C308 H30I 108.6 . . ? C307 C308 H30J 108.6 . . ? C309 C308 H30J 108.6 . . ? H30I C308 H30J 107.6 . . ? C310 C309 C308 112.8(2) . . ? C310 C309 H30K 109.0 . . ? C308 C309 H30K 109.0 . . ? C310 C309 H30L 109.0 . . ? C308 C309 H30L 109.0 . . ? H30K C309 H30L 107.8 . . ? C309 C310 C311 114.8(2) . . ? C309 C310 H31A 108.6 . . ? C311 C310 H31A 108.6 . . ? C309 C310 H31B 108.6 . . ? C311 C310 H31B 108.6 . . ? H31A C310 H31B 107.5 . . ? C312 C311 C310 113.4(2) . . ? C312 C311 H31C 108.9 . . ? C310 C311 H31C 108.9 . . ? C312 C311 H31D 108.9 . . ? C310 C311 H31D 108.9 . . ? H31C C311 H31D 107.7 . . ? C311 C312 C313 114.9(2) . . ? C311 C312 H31E 108.6 . . ? C313 C312 H31E 108.6 . . ? C311 C312 H31F 108.6 . . ? C313 C312 H31F 108.6 . . ? H31E C312 H31F 107.5 . . ? C314 C313 C312 113.9(2) . . ? C314 C313 H31G 108.8 . . ? C312 C313 H31G 108.8 . . ? C314 C313 H31H 108.8 . . ? C312 C313 H31H 108.8 . . ? H31G C313 H31H 107.7 . . ? C313 C314 C315 113.7(2) . . ? C313 C314 H31I 108.8 . . ? C315 C314 H31I 108.8 . . ? C313 C314 H31J 108.8 . . ? C315 C314 H31J 108.8 . . ? H31I C314 H31J 107.7 . . ? C314 C315 H31K 109.5 . . ? C314 C315 H31L 109.5 . . ? H31K C315 H31L 109.5 . . ? C314 C315 H31M 109.5 . . ? H31K C315 H31M 109.5 . . ? H31L C315 H31M 109.5 . . ? N302 C316 H31N 109.5 . . ? N302 C316 H31O 109.5 . . ? H31N C316 H31O 109.5 . . ? N302 C316 H31P 109.5 . . ? H31N C316 H31P 109.5 . . ? H31O C316 H31P 109.5 . . ? C101 N101 C103 108.1(2) . . ? C101 N101 C104 125.7(2) . . ? C103 N101 C104 126.1(2) . . ? C101 N102 C102 108.6(2) . . ? C101 N102 C116 125.6(2) . . ? C102 N102 C116 125.7(2) . . ? C201 N201 C203 108.8(2) . . ? C201 N201 C204 125.9(2) . . ? C203 N201 C204 125.3(2) . . ? C201 N202 C202 109.4(2) . . ? C201 N202 C216 125.7(2) . . ? C202 N202 C216 124.9(2) . . ? C301 N301 C303 108.4(2) . . ? C301 N301 C304 125.3(2) . . ? C303 N301 C304 126.2(2) . . ? C301 N302 C302 109.1(2) . . ? C301 N302 C316 125.3(2) . . ? C302 N302 C316 125.6(2) . . ? Cl3 Cu1 Cl1 126.83(3) . . ? Cl3 Cu1 Cl2 113.64(3) . . ? Cl1 Cu1 Cl2 119.45(3) . . ? Cl4 Cu2 Cl5 177.05(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N102 C102 C103 N101 1.1(3) . . . . ? N101 C104 C105 C106 178.5(2) . . . . ? C104 C105 C106 C107 177.3(2) . . . . ? C105 C106 C107 C108 178.1(2) . . . . ? C106 C107 C108 C109 176.9(2) . . . . ? C107 C108 C109 C110 179.0(2) . . . . ? C108 C109 C110 C111 -180.0(2) . . . . ? C109 C110 C111 C112 -179.4(2) . . . . ? C110 C111 C112 C113 179.2(2) . . . . ? C111 C112 C113 C114 -177.8(2) . . . . ? C112 C113 C114 C115 -179.4(2) . . . . ? N202 C202 C203 N201 0.1(3) . . . . ? N201 C204 C205 C206 -68.4(3) . . . . ? C204 C205 C206 C207 179.6(2) . . . . ? C205 C206 C207 C208 -172.4(2) . . . . ? C206 C207 C208 C209 173.2(2) . . . . ? C207 C208 C209 C210 -172.2(2) . . . . ? C208 C209 C210 C211 173.9(2) . . . . ? C209 C210 C211 C212 -176.2(2) . . . . ? C210 C211 C212 C213 180.0(2) . . . . ? C211 C212 C213 C214 179.6(2) . . . . ? C212 C213 C214 C215 -178.9(2) . . . . ? N302 C302 C303 N301 0.1(3) . . . . ? N301 C304 C305 C306 -52.6(3) . . . . ? C304 C305 C306 C307 -169.9(2) . . . . ? C305 C306 C307 C308 174.4(2) . . . . ? C306 C307 C308 C309 -175.0(2) . . . . ? C307 C308 C309 C310 178.2(2) . . . . ? C308 C309 C310 C311 179.3(2) . . . . ? C309 C310 C311 C312 179.2(2) . . . . ? C310 C311 C312 C313 178.9(2) . . . . ? C311 C312 C313 C314 -179.8(2) . . . . ? C312 C313 C314 C315 -179.6(2) . . . . ? N102 C101 N101 C103 -0.2(3) . . . . ? N102 C101 N101 C104 176.2(2) . . . . ? C102 C103 N101 C101 -0.6(3) . . . . ? C102 C103 N101 C104 -176.9(2) . . . . ? C105 C104 N101 C101 -82.7(3) . . . . ? C105 C104 N101 C103 93.0(3) . . . . ? N101 C101 N102 C102 0.9(3) . . . . ? N101 C101 N102 C116 175.9(2) . . . . ? C103 C102 N102 C101 -1.2(3) . . . . ? C103 C102 N102 C116 -176.3(3) . . . . ? N202 C201 N201 C203 -0.5(3) . . . . ? N202 C201 N201 C204 178.4(2) . . . . ? C202 C203 N201 C201 0.2(3) . . . . ? C202 C203 N201 C204 -178.7(2) . . . . ? C205 C204 N201 C201 122.4(3) . . . . ? C205 C204 N201 C203 -58.9(4) . . . . ? N201 C201 N202 C202 0.6(3) . . . . ? N201 C201 N202 C216 -179.8(3) . . . . ? C203 C202 N202 C201 -0.4(3) . . . . ? C203 C202 N202 C216 180.0(3) . . . . ? N302 C301 N301 C303 -0.7(3) . . . . ? N302 C301 N301 C304 175.3(2) . . . . ? C302 C303 N301 C301 0.3(3) . . . . ? C302 C303 N301 C304 -175.6(2) . . . . ? C305 C304 N301 C301 -64.6(3) . . . . ? C305 C304 N301 C303 110.7(3) . . . . ? N301 C301 N302 C302 0.7(3) . . . . ? N301 C301 N302 C316 -178.7(2) . . . . ? C303 C302 N302 C301 -0.5(3) . . . . ? C303 C302 N302 C316 179.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.354 _refine_diff_density_min -0.695 _refine_diff_density_rms 0.067 #===END data_msb1_19 _database_code_depnum_ccdc_archive 'CCDC 769703' #TrackingRef 'MarionStricker.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Department of Chemistry University of Anywhere Sometown Somewhere, UK ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H112 Cu N8, F6 P' _chemical_formula_sum 'C60 H112 Cu F6 N8 P' _chemical_formula_weight 1154.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7007(14) _cell_length_b 13.6056(16) _cell_length_c 21.043(3) _cell_angle_alpha 91.893(10) _cell_angle_beta 94.239(10) _cell_angle_gamma 100.766(10) _cell_volume 3278.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 17724 _cell_measurement_theta_min 22.97 _cell_measurement_theta_max 1.52 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.169 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1252 _exptl_absorpt_coefficient_mu 0.416 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8575 _exptl_absorpt_correction_T_max 1.0014 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; Department of Chemistry University of Anywhere Sometown Somewhere, UK ; _diffrn_ambient_temperature 173(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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate ( 34 cm diameter )' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_measurement_method 'rotation method' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44190 _diffrn_reflns_av_R_equivalents 0.1488 _diffrn_reflns_av_sigmaI/netI 0.1761 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 26.07 _reflns_number_total 12685 _reflns_number_gt 3994 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(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^)+(0.0226P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12685 _refine_ls_number_parameters 726 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2179 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1142 _refine_ls_wR_factor_gt 0.0795 _refine_ls_goodness_of_fit_ref 0.819 _refine_ls_restrained_S_all 0.819 _refine_ls_shift/su_max 0.005 _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 C101 C 0.5661(4) 0.3051(4) 0.4483(2) 0.0658(13) Uani 1 1 d . . . H101 H 0.5364 0.2928 0.4887 0.079 Uiso 1 1 calc R . . C102 C 0.5893(5) 0.3614(4) 0.3546(2) 0.0872(16) Uani 1 1 d . . . H102 H 0.5810 0.3954 0.3163 0.105 Uiso 1 1 calc R . . C103 C 0.6686(4) 0.3025(4) 0.3690(3) 0.0798(15) Uani 1 1 d . . . H103 H 0.7252 0.2884 0.3417 0.096 Uiso 1 1 calc R . . C104 C 0.4210(4) 0.4083(4) 0.4112(2) 0.0794(15) Uani 1 1 d . . . H10K H 0.4265 0.4670 0.3842 0.095 Uiso 1 1 calc R . . H10L H 0.4192 0.4321 0.4560 0.095 Uiso 1 1 calc R . . C105 C 0.3082(4) 0.3341(4) 0.3908(2) 0.0790(15) Uani 1 1 d . . . H10A H 0.2417 0.3677 0.3974 0.095 Uiso 1 1 calc R . . H10B H 0.3025 0.2774 0.4195 0.095 Uiso 1 1 calc R . . C106 C 0.2945(4) 0.2912(4) 0.3214(2) 0.0740(14) Uani 1 1 d . . . H10I H 0.3608 0.2576 0.3142 0.089 Uiso 1 1 calc R . . H10J H 0.2220 0.2399 0.3152 0.089 Uiso 1 1 calc R . . C107 C 0.2897(4) 0.3695(4) 0.2722(2) 0.0757(14) Uani 1 1 d . . . H10E H 0.3581 0.4244 0.2812 0.091 Uiso 1 1 calc R . . H10F H 0.2187 0.3981 0.2765 0.091 Uiso 1 1 calc R . . C108 C 0.2886(4) 0.3288(3) 0.2032(2) 0.0697(13) Uani 1 1 d . . . H10G H 0.3571 0.2965 0.1995 0.084 Uiso 1 1 calc R . . H10H H 0.2175 0.2770 0.1932 0.084 Uiso 1 1 calc R . . C109 C 0.2914(4) 0.4094(4) 0.1549(2) 0.0732(14) Uani 1 1 d . . . H10C H 0.3568 0.4653 0.1683 0.088 Uiso 1 1 calc R . . H10D H 0.2182 0.4359 0.1552 0.088 Uiso 1 1 calc R . . C110 C 0.3051(4) 0.3743(3) 0.0871(2) 0.0713(13) Uani 1 1 d . . . H11G H 0.3764 0.3448 0.0870 0.086 Uiso 1 1 calc R . . H11H H 0.2376 0.3208 0.0727 0.086 Uiso 1 1 calc R . . C111 C 0.3136(4) 0.4568(3) 0.0401(2) 0.0708(13) Uani 1 1 d . . . H11E H 0.3797 0.5112 0.0552 0.085 Uiso 1 1 calc R . . H11F H 0.2413 0.4849 0.0393 0.085 Uiso 1 1 calc R . . C112 C 0.3308(4) 0.4225(3) -0.0274(2) 0.0709(13) Uani 1 1 d . . . H11A H 0.4017 0.3924 -0.0263 0.085 Uiso 1 1 calc R . . H11B H 0.2636 0.3693 -0.0428 0.085 Uiso 1 1 calc R . . C113 C 0.3430(4) 0.5044(3) -0.0751(2) 0.0689(13) Uani 1 1 d . . . H11C H 0.2732 0.5359 -0.0756 0.083 Uiso 1 1 calc R . . H11D H 0.4118 0.5566 -0.0608 0.083 Uiso 1 1 calc R . . C114 C 0.3564(4) 0.4672(4) -0.1421(2) 0.0801(14) Uani 1 1 d . . . H11I H 0.2876 0.4148 -0.1562 0.096 Uiso 1 1 calc R . . H11J H 0.4261 0.4356 -0.1414 0.096 Uiso 1 1 calc R . . C115 C 0.3686(4) 0.5479(4) -0.1908(2) 0.0924(16) Uani 1 1 d . . . H11K H 0.3762 0.5179 -0.2329 0.139 Uiso 1 1 calc R . . H11L H 0.4381 0.5991 -0.1782 0.139 Uiso 1 1 calc R . . H11M H 0.2993 0.5789 -0.1926 0.139 Uiso 1 1 calc R . . C201 C 0.6096(4) 0.1130(4) 0.5860(2) 0.0665(13) Uani 1 1 d . . . H201 H 0.6055 0.1771 0.6038 0.080 Uiso 1 1 calc R . . C202 C 0.5784(4) -0.0495(4) 0.5688(2) 0.0675(13) Uani 1 1 d . . . H202 H 0.5508 -0.1194 0.5716 0.081 Uiso 1 1 calc R . . C203 C 0.6520(4) -0.0049(4) 0.5275(2) 0.0699(13) Uani 1 1 d . . . H203 H 0.6846 -0.0392 0.4954 0.084 Uiso 1 1 calc R . . C204 C 0.4713(4) 0.0138(4) 0.6575(2) 0.0795(15) Uani 1 1 d . . . H20I H 0.3912 -0.0139 0.6387 0.095 Uiso 1 1 calc R . . H20J H 0.4709 0.0806 0.6775 0.095 Uiso 1 1 calc R . . C205 C 0.5047(4) -0.0542(3) 0.7084(2) 0.0666(13) Uani 1 1 d . . . H20C H 0.5891 -0.0342 0.7214 0.080 Uiso 1 1 calc R . . H20D H 0.4905 -0.1239 0.6903 0.080 Uiso 1 1 calc R . . C206 C 0.4365(4) -0.0504(4) 0.7667(2) 0.0745(14) Uani 1 1 d . . . H20K H 0.3523 -0.0618 0.7527 0.089 Uiso 1 1 calc R . . H20L H 0.4581 0.0177 0.7874 0.089 Uiso 1 1 calc R . . C207 C 0.4562(4) -0.1262(4) 0.8160(2) 0.0745(14) Uani 1 1 d . . . H20E H 0.5410 -0.1242 0.8240 0.089 Uiso 1 1 calc R . . H20F H 0.4197 -0.1942 0.7986 0.089 Uiso 1 1 calc R . . C208 C 0.4060(4) -0.1066(3) 0.8789(2) 0.0744(14) Uani 1 1 d . . . H20G H 0.3227 -0.1025 0.8700 0.089 Uiso 1 1 calc R . . H20H H 0.4472 -0.0407 0.8977 0.089 Uiso 1 1 calc R . . C209 C 0.4146(4) -0.1853(3) 0.9279(2) 0.0718(13) Uani 1 1 d . . . H20A H 0.4964 -0.1951 0.9335 0.086 Uiso 1 1 calc R . . H20B H 0.3656 -0.2498 0.9115 0.086 Uiso 1 1 calc R . . C210 C 0.3759(4) -0.1568(3) 0.9927(2) 0.0712(13) Uani 1 1 d . . . H21A H 0.4273 -0.0938 1.0097 0.085 Uiso 1 1 calc R . . H21B H 0.2955 -0.1436 0.9865 0.085 Uiso 1 1 calc R . . C211 C 0.3780(4) -0.2359(4) 1.0420(2) 0.0738(14) Uani 1 1 d . . . H21E H 0.4570 -0.2524 1.0463 0.089 Uiso 1 1 calc R . . H21F H 0.3226 -0.2975 1.0263 0.089 Uiso 1 1 calc R . . C212 C 0.3466(4) -0.2044(4) 1.1078(2) 0.0753(14) Uani 1 1 d . . . H21I H 0.4023 -0.1430 1.1236 0.090 Uiso 1 1 calc R . . H21J H 0.2678 -0.1875 1.1035 0.090 Uiso 1 1 calc R . . C213 C 0.3477(4) -0.2834(3) 1.1575(2) 0.0729(13) Uani 1 1 d . . . H21C H 0.2899 -0.3440 1.1425 0.088 Uiso 1 1 calc R . . H21D H 0.4257 -0.3022 1.1608 0.088 Uiso 1 1 calc R . . C214 C 0.3208(4) -0.2509(4) 1.2234(2) 0.0862(15) Uani 1 1 d . . . H21G H 0.2443 -0.2295 1.2201 0.103 Uiso 1 1 calc R . . H21H H 0.3807 -0.1923 1.2395 0.103 Uiso 1 1 calc R . . C215 C 0.3173(5) -0.3333(4) 1.2716(2) 0.0966(17) Uani 1 1 d . . . H21K H 0.2962 -0.3085 1.3126 0.145 Uiso 1 1 calc R . . H21L H 0.3942 -0.3518 1.2774 0.145 Uiso 1 1 calc R . . H21M H 0.2591 -0.3921 1.2557 0.145 Uiso 1 1 calc R . . C301 C 0.8898(4) 0.0464(4) 0.42591(19) 0.0619(12) Uani 1 1 d . . . H301 H 0.8198 -0.0023 0.4187 0.074 Uiso 1 1 calc R . . C302 C 1.0098(4) 0.1847(4) 0.44773(19) 0.0675(13) Uani 1 1 d . . . H302 H 1.0405 0.2531 0.4592 0.081 Uiso 1 1 calc R . . C303 C 1.0744(4) 0.1146(4) 0.4335(2) 0.0661(13) Uani 1 1 d . . . H303 H 1.1569 0.1251 0.4331 0.079 Uiso 1 1 calc R . . C304 C 1.0235(4) -0.0725(3) 0.4041(2) 0.0688(13) Uani 1 1 d . . . H30K H 0.9697 -0.1240 0.4252 0.083 Uiso 1 1 calc R . . H30L H 1.1042 -0.0747 0.4210 0.083 Uiso 1 1 calc R . . C305 C 1.0110(4) -0.0971(3) 0.3328(2) 0.0666(13) Uani 1 1 d . . . H30G H 0.9338 -0.0859 0.3152 0.080 Uiso 1 1 calc R . . H30H H 1.0128 -0.1690 0.3254 0.080 Uiso 1 1 calc R . . C306 C 1.1066(4) -0.0347(3) 0.2961(2) 0.0686(13) Uani 1 1 d . . . H30I H 1.1115 0.0374 0.3070 0.082 Uiso 1 1 calc R . . H30J H 1.1830 -0.0522 0.3092 0.082 Uiso 1 1 calc R . . C307 C 1.0806(4) -0.0538(3) 0.2243(2) 0.0670(13) Uani 1 1 d . . . H30E H 1.0723 -0.1265 0.2140 0.080 Uiso 1 1 calc R . . H30F H 1.0051 -0.0344 0.2115 0.080 Uiso 1 1 calc R . . C308 C 1.1739(4) 0.0029(3) 0.1855(2) 0.0652(13) Uani 1 1 d . . . H30A H 1.2451 -0.0265 0.1911 0.078 Uiso 1 1 calc R . . H30B H 1.1942 0.0736 0.2018 0.078 Uiso 1 1 calc R . . C309 C 1.1338(4) -0.0006(3) 0.1142(2) 0.0675(13) Uani 1 1 d . . . H30C H 1.1144 -0.0714 0.0981 0.081 Uiso 1 1 calc R . . H30D H 1.0617 0.0275 0.1090 0.081 Uiso 1 1 calc R . . C310 C 1.2244(4) 0.0567(3) 0.0738(2) 0.0670(13) Uani 1 1 d . . . H31C H 1.2946 0.0256 0.0764 0.080 Uiso 1 1 calc R . . H31D H 1.2480 0.1265 0.0915 0.080 Uiso 1 1 calc R . . C311 C 1.1796(4) 0.0582(3) 0.0040(2) 0.0692(13) Uani 1 1 d . . . H31E H 1.1552 -0.0117 -0.0135 0.083 Uiso 1 1 calc R . . H31F H 1.1099 0.0899 0.0014 0.083 Uiso 1 1 calc R . . C312 C 1.2699(4) 0.1143(3) -0.0370(2) 0.0681(13) Uani 1 1 d . . . H31A H 1.2956 0.1836 -0.0188 0.082 Uiso 1 1 calc R . . H31B H 1.3388 0.0816 -0.0352 0.082 Uiso 1 1 calc R . . C313 C 1.2255(4) 0.1183(3) -0.1065(2) 0.0658(13) Uani 1 1 d . . . H31G H 1.1994 0.0491 -0.1249 0.079 Uiso 1 1 calc R . . H31H H 1.1571 0.1516 -0.1086 0.079 Uiso 1 1 calc R . . C314 C 1.3172(4) 0.1739(4) -0.1465(2) 0.0744(14) Uani 1 1 d . . . H31I H 1.3853 0.1402 -0.1446 0.089 Uiso 1 1 calc R . . H31J H 1.3439 0.2429 -0.1278 0.089 Uiso 1 1 calc R . . C315 C 1.2733(4) 0.1794(4) -0.2166(2) 0.0880(16) Uani 1 1 d . . . H31K H 1.3375 0.2126 -0.2403 0.132 Uiso 1 1 calc R . . H31L H 1.2099 0.2175 -0.2192 0.132 Uiso 1 1 calc R . . H31M H 1.2444 0.1114 -0.2352 0.132 Uiso 1 1 calc R . . C401 C 0.9488(5) 0.3444(4) 0.5771(2) 0.0698(14) Uani 1 1 d . . . H401 H 0.9880 0.2918 0.5891 0.084 Uiso 1 1 calc R . . C402 C 0.8307(5) 0.4247(4) 0.5333(3) 0.0943(18) Uani 1 1 d . . . H402 H 0.7669 0.4412 0.5080 0.113 Uiso 1 1 calc R . . C403 C 0.9110(5) 0.4921(4) 0.5695(3) 0.1010(19) Uani 1 1 d . . . H403 H 0.9144 0.5623 0.5737 0.121 Uiso 1 1 calc R . . C404 C 1.0879(4) 0.4822(4) 0.6424(2) 0.0770(14) Uani 1 1 d . . . H40A H 1.1259 0.5465 0.6261 0.092 Uiso 1 1 calc R . . H40B H 1.1448 0.4367 0.6429 0.092 Uiso 1 1 calc R . . C405 C 1.0581(4) 0.5005(4) 0.7106(2) 0.0776(14) Uani 1 1 d . . . H40I H 1.1228 0.5501 0.7326 0.093 Uiso 1 1 calc R . . H40J H 0.9874 0.5309 0.7089 0.093 Uiso 1 1 calc R . . C406 C 1.0368(4) 0.4094(4) 0.7502(2) 0.0773(14) Uani 1 1 d . . . H40K H 1.1055 0.3766 0.7505 0.093 Uiso 1 1 calc R . . H40L H 0.9686 0.3612 0.7301 0.093 Uiso 1 1 calc R . . C407 C 1.0142(4) 0.4346(4) 0.8193(2) 0.0759(14) Uani 1 1 d . . . H40G H 1.0775 0.4895 0.8370 0.091 Uiso 1 1 calc R . . H40H H 0.9401 0.4599 0.8188 0.091 Uiso 1 1 calc R . . C408 C 1.0068(4) 0.3486(3) 0.8634(2) 0.0767(14) Uani 1 1 d . . . H40E H 1.0801 0.3222 0.8636 0.092 Uiso 1 1 calc R . . H40F H 0.9421 0.2942 0.8466 0.092 Uiso 1 1 calc R . . C409 C 0.9869(4) 0.3775(4) 0.9322(2) 0.0746(14) Uani 1 1 d . . . H40C H 1.0497 0.4339 0.9482 0.090 Uiso 1 1 calc R . . H40D H 0.9120 0.4014 0.9320 0.090 Uiso 1 1 calc R . . C410 C 0.9839(4) 0.2932(4) 0.9784(2) 0.0757(14) Uani 1 1 d . . . H41C H 0.9216 0.2364 0.9622 0.091 Uiso 1 1 calc R . . H41D H 1.0591 0.2697 0.9791 0.091 Uiso 1 1 calc R . . C411 C 0.9628(4) 0.3221(4) 1.0460(2) 0.0735(14) Uani 1 1 d . . . H41E H 0.8867 0.3439 1.0456 0.088 Uiso 1 1 calc R . . H41F H 1.0241 0.3798 1.0620 0.088 Uiso 1 1 calc R . . C412 C 0.9628(4) 0.2380(3) 1.0914(2) 0.0736(14) Uani 1 1 d . . . H41A H 1.0394 0.2170 1.0919 0.088 Uiso 1 1 calc R . . H41B H 0.9026 0.1800 1.0746 0.088 Uiso 1 1 calc R . . C413 C 0.9400(4) 0.2632(4) 1.1599(2) 0.0774(14) Uani 1 1 d . . . H41G H 0.9995 0.3215 1.1768 0.093 Uiso 1 1 calc R . . H41H H 0.8627 0.2831 1.1598 0.093 Uiso 1 1 calc R . . C414 C 0.9422(4) 0.1782(4) 1.2041(2) 0.0802(15) Uani 1 1 d . . . H41I H 1.0199 0.1591 1.2049 0.096 Uiso 1 1 calc R . . H41J H 0.8835 0.1194 1.1869 0.096 Uiso 1 1 calc R . . C415 C 0.9174(5) 0.2039(4) 1.2717(2) 0.1077(19) Uani 1 1 d . . . H41K H 0.9179 0.1454 1.2976 0.162 Uiso 1 1 calc R . . H41L H 0.8407 0.2231 1.2713 0.162 Uiso 1 1 calc R . . H41M H 0.9775 0.2597 1.2898 0.162 Uiso 1 1 calc R . . Cu1 Cu 0.76778(5) 0.20235(5) 0.48510(3) 0.0744(2) Uani 1 1 d . . . F1 F 0.3273(3) 0.2239(2) 0.53748(14) 0.1211(11) Uani 1 1 d . A . F6 F 0.3412(3) 0.3687(3) 0.65868(14) 0.1364(13) Uani 1 1 d . A . F2 F 0.4123(17) 0.2467(14) 0.6421(8) 0.100(6) Uani 0.423(18) 1 d P A 1 F3 F 0.225(2) 0.211(3) 0.6227(7) 0.207(12) Uani 0.423(18) 1 d P A 1 F4 F 0.237(3) 0.331(3) 0.5547(8) 0.174(12) Uani 0.423(18) 1 d P A 1 F5 F 0.435(3) 0.364(2) 0.5745(10) 0.201(13) Uani 0.423(18) 1 d P A 1 F2A F 0.360(3) 0.2025(16) 0.6361(8) 0.186(10) Uani 0.577(18) 1 d P A 2 F3A F 0.2080(7) 0.2684(8) 0.6130(8) 0.138(6) Uani 0.577(18) 1 d P A 2 F4A F 0.3031(18) 0.3864(8) 0.5611(7) 0.129(6) Uani 0.577(18) 1 d P A 2 F5A F 0.4647(8) 0.3294(14) 0.5879(8) 0.157(8) Uani 0.577(18) 1 d P A 2 N101 N 0.6555(3) 0.2669(3) 0.42740(18) 0.0662(11) Uani 1 1 d . . . N102 N 0.5244(3) 0.3622(3) 0.40536(18) 0.0667(10) Uani 1 1 d . . . N201 N 0.6732(3) 0.0976(3) 0.53813(17) 0.0657(10) Uani 1 1 d . . . N202 N 0.5516(3) 0.0255(3) 0.60590(17) 0.0654(10) Uani 1 1 d . . . N301 N 0.8931(3) 0.1414(3) 0.44304(16) 0.0644(10) Uani 1 1 d . . . N302 N 0.9979(3) 0.0265(3) 0.41985(16) 0.0596(10) Uani 1 1 d . . . N401 N 0.8533(4) 0.3287(3) 0.53768(19) 0.0709(11) Uani 1 1 d . . . N402 N 0.9864(3) 0.4385(3) 0.59874(18) 0.0694(11) Uani 1 1 d . . . P1 P 0.33224(13) 0.29505(11) 0.59863(7) 0.0758(4) 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 C101 0.061(3) 0.076(4) 0.061(3) 0.002(3) 0.012(3) 0.011(3) C102 0.080(4) 0.117(5) 0.069(4) 0.024(3) 0.024(3) 0.018(4) C103 0.068(4) 0.093(4) 0.084(4) 0.010(3) 0.019(3) 0.024(3) C104 0.075(4) 0.077(4) 0.095(4) 0.002(3) 0.015(3) 0.033(3) C105 0.063(4) 0.100(4) 0.080(4) 0.006(3) 0.013(3) 0.028(3) C106 0.063(3) 0.075(4) 0.086(4) 0.007(3) 0.017(3) 0.012(3) C107 0.073(4) 0.076(4) 0.085(4) 0.011(3) 0.018(3) 0.027(3) C108 0.065(3) 0.073(4) 0.074(3) 0.002(3) 0.012(3) 0.017(3) C109 0.067(3) 0.078(4) 0.080(4) 0.008(3) 0.018(3) 0.023(3) C110 0.069(3) 0.072(4) 0.076(3) 0.001(3) 0.020(3) 0.015(3) C111 0.064(3) 0.071(4) 0.080(4) 0.001(3) 0.017(3) 0.015(3) C112 0.066(3) 0.076(4) 0.074(3) 0.004(3) 0.016(2) 0.016(3) C113 0.063(3) 0.069(3) 0.075(3) 0.002(3) 0.011(3) 0.012(3) C114 0.077(4) 0.086(4) 0.078(4) 0.007(3) 0.017(3) 0.012(3) C115 0.092(4) 0.098(4) 0.086(4) 0.018(3) 0.017(3) 0.011(3) C201 0.072(4) 0.055(4) 0.073(3) -0.007(3) 0.009(3) 0.016(3) C202 0.075(4) 0.048(3) 0.079(3) -0.008(3) 0.004(3) 0.014(3) C203 0.069(3) 0.057(4) 0.086(4) -0.006(3) 0.017(3) 0.015(3) C204 0.077(4) 0.098(4) 0.071(3) 0.011(3) 0.027(3) 0.027(3) C205 0.057(3) 0.063(3) 0.079(3) 0.002(3) 0.009(3) 0.008(3) C206 0.068(3) 0.068(4) 0.089(4) 0.002(3) 0.023(3) 0.011(3) C207 0.078(4) 0.069(4) 0.078(3) 0.000(3) 0.014(3) 0.017(3) C208 0.069(3) 0.070(4) 0.088(4) 0.005(3) 0.020(3) 0.019(3) C209 0.071(3) 0.069(4) 0.077(3) 0.002(3) 0.014(3) 0.016(3) C210 0.064(3) 0.066(3) 0.086(4) 0.006(3) 0.013(3) 0.015(3) C211 0.068(3) 0.073(4) 0.083(4) 0.002(3) 0.013(3) 0.017(3) C212 0.073(3) 0.076(4) 0.080(4) 0.001(3) 0.013(3) 0.019(3) C213 0.071(3) 0.070(4) 0.081(4) -0.002(3) 0.014(3) 0.017(3) C214 0.092(4) 0.079(4) 0.088(4) -0.001(3) 0.012(3) 0.016(3) C215 0.119(5) 0.087(4) 0.081(4) 0.003(3) 0.012(3) 0.010(3) C301 0.057(3) 0.068(4) 0.061(3) -0.005(3) 0.014(2) 0.008(3) C302 0.071(4) 0.063(3) 0.069(3) 0.002(3) 0.017(3) 0.008(3) C303 0.056(3) 0.071(4) 0.071(3) -0.002(3) 0.013(3) 0.008(3) C304 0.075(3) 0.069(4) 0.069(3) 0.004(3) 0.020(3) 0.025(3) C305 0.069(3) 0.065(3) 0.070(3) 0.000(3) 0.019(3) 0.018(3) C306 0.064(3) 0.066(3) 0.075(3) -0.006(3) 0.014(3) 0.009(3) C307 0.069(3) 0.065(3) 0.068(3) 0.001(3) 0.015(3) 0.011(3) C308 0.066(3) 0.064(3) 0.068(3) 0.000(3) 0.013(3) 0.016(3) C309 0.070(3) 0.061(3) 0.075(3) 0.002(3) 0.016(3) 0.017(3) C310 0.074(3) 0.058(3) 0.072(3) -0.001(3) 0.021(3) 0.016(3) C311 0.070(3) 0.068(3) 0.072(3) 0.000(3) 0.017(3) 0.016(3) C312 0.072(3) 0.062(3) 0.074(3) 0.002(3) 0.019(3) 0.017(3) C313 0.066(3) 0.067(3) 0.069(3) 0.006(3) 0.018(3) 0.017(3) C314 0.076(4) 0.077(4) 0.073(4) 0.003(3) 0.018(3) 0.019(3) C315 0.093(4) 0.107(4) 0.073(4) 0.016(3) 0.019(3) 0.035(3) C401 0.085(4) 0.048(4) 0.081(4) -0.004(3) 0.020(3) 0.019(3) C402 0.080(4) 0.072(4) 0.133(5) -0.018(4) -0.010(3) 0.033(4) C403 0.107(5) 0.066(4) 0.132(5) -0.018(4) -0.018(4) 0.034(4) C404 0.070(4) 0.075(4) 0.084(4) -0.012(3) 0.006(3) 0.010(3) C405 0.077(4) 0.078(4) 0.083(4) -0.007(3) 0.012(3) 0.028(3) C406 0.075(4) 0.074(4) 0.085(4) -0.009(3) 0.006(3) 0.023(3) C407 0.080(4) 0.066(4) 0.083(4) -0.016(3) 0.008(3) 0.021(3) C408 0.076(4) 0.060(3) 0.094(4) -0.006(3) 0.010(3) 0.014(3) C409 0.065(3) 0.076(4) 0.084(4) -0.015(3) 0.010(3) 0.017(3) C410 0.071(4) 0.070(4) 0.087(4) -0.003(3) 0.014(3) 0.011(3) C411 0.073(3) 0.073(4) 0.078(4) 0.000(3) 0.015(3) 0.023(3) C412 0.067(3) 0.065(4) 0.089(4) -0.006(3) 0.013(3) 0.011(3) C413 0.070(3) 0.073(4) 0.093(4) -0.003(3) 0.018(3) 0.019(3) C414 0.079(4) 0.068(4) 0.098(4) 0.000(3) 0.025(3) 0.017(3) C415 0.138(5) 0.108(5) 0.090(4) 0.007(3) 0.033(4) 0.048(4) Cu1 0.0671(4) 0.0679(5) 0.0923(5) -0.0020(4) 0.0149(3) 0.0209(3) F1 0.152(3) 0.100(3) 0.108(2) -0.036(2) 0.014(2) 0.022(2) F6 0.173(3) 0.146(3) 0.104(3) -0.035(2) 0.017(2) 0.070(3) F2 0.129(11) 0.101(12) 0.081(7) 0.020(8) -0.021(9) 0.059(9) F3 0.22(2) 0.23(2) 0.103(8) 0.020(12) 0.042(11) -0.141(16) F4 0.23(2) 0.25(3) 0.081(8) -0.032(14) -0.059(12) 0.18(2) F5 0.28(3) 0.160(16) 0.112(11) -0.007(10) 0.110(17) -0.131(17) F2A 0.32(2) 0.122(13) 0.178(13) 0.076(9) 0.141(14) 0.141(16) F3A 0.053(5) 0.097(7) 0.273(16) 0.024(7) 0.073(7) 0.012(5) F4A 0.226(16) 0.069(6) 0.110(9) 0.032(5) 0.050(10) 0.054(7) F5A 0.046(5) 0.227(17) 0.191(14) -0.081(12) 0.033(5) 0.017(7) N101 0.062(3) 0.070(3) 0.073(3) 0.013(2) 0.012(2) 0.024(2) N102 0.069(3) 0.070(3) 0.064(3) 0.009(2) 0.011(2) 0.018(2) N201 0.065(3) 0.059(3) 0.075(3) -0.002(2) 0.011(2) 0.016(2) N202 0.062(3) 0.060(3) 0.077(3) 0.002(2) 0.012(2) 0.015(2) N301 0.059(3) 0.067(3) 0.067(3) -0.004(2) 0.012(2) 0.013(2) N302 0.053(3) 0.061(3) 0.065(3) -0.001(2) 0.015(2) 0.009(2) N401 0.068(3) 0.060(3) 0.084(3) -0.009(2) 0.005(2) 0.015(2) N402 0.068(3) 0.062(3) 0.080(3) -0.008(2) 0.006(2) 0.022(3) P1 0.0799(12) 0.0750(11) 0.0778(10) -0.0015(9) 0.0205(9) 0.0237(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C101 N102 1.336(5) . ? C101 N101 1.347(5) . ? C101 H101 0.9500 . ? C102 N102 1.357(5) . ? C102 C103 1.359(6) . ? C102 H102 0.9500 . ? C103 N101 1.343(5) . ? C103 H103 0.9500 . ? C104 N102 1.473(5) . ? C104 C105 1.528(6) . ? C104 H10K 0.9900 . ? C104 H10L 0.9900 . ? C105 C106 1.540(6) . ? C105 H10A 0.9900 . ? C105 H10B 0.9900 . ? C106 C107 1.517(6) . ? C106 H10I 0.9900 . ? C106 H10J 0.9900 . ? C107 C108 1.534(5) . ? C107 H10E 0.9900 . ? C107 H10F 0.9900 . ? C108 C109 1.518(5) . ? C108 H10G 0.9900 . ? C108 H10H 0.9900 . ? C109 C110 1.519(5) . ? C109 H10C 0.9900 . ? C109 H10D 0.9900 . ? C110 C111 1.516(5) . ? C110 H11G 0.9900 . ? C110 H11H 0.9900 . ? C111 C112 1.520(5) . ? C111 H11E 0.9900 . ? C111 H11F 0.9900 . ? C112 C113 1.518(5) . ? C112 H11A 0.9900 . ? C112 H11B 0.9900 . ? C113 C114 1.512(5) . ? C113 H11C 0.9900 . ? C113 H11D 0.9900 . ? C114 C115 1.521(6) . ? C114 H11I 0.9900 . ? C114 H11J 0.9900 . ? C115 H11K 0.9800 . ? C115 H11L 0.9800 . ? C115 H11M 0.9800 . ? C201 N201 1.329(5) . ? C201 N202 1.351(5) . ? C201 H201 0.9500 . ? C202 C203 1.349(6) . ? C202 N202 1.361(5) . ? C202 H202 0.9500 . ? C203 N201 1.377(5) . ? C203 H203 0.9500 . ? C204 N202 1.481(5) . ? C204 C205 1.515(5) . ? C204 H20I 0.9900 . ? C204 H20J 0.9900 . ? C205 C206 1.517(5) . ? C205 H20C 0.9900 . ? C205 H20D 0.9900 . ? C206 C207 1.521(5) . ? C206 H20K 0.9900 . ? C206 H20L 0.9900 . ? C207 C208 1.522(5) . ? C207 H20E 0.9900 . ? C207 H20F 0.9900 . ? C208 C209 1.523(5) . ? C208 H20G 0.9900 . ? C208 H20H 0.9900 . ? C209 C210 1.529(5) . ? C209 H20A 0.9900 . ? C209 H20B 0.9900 . ? C210 C211 1.522(5) . ? C210 H21A 0.9900 . ? C210 H21B 0.9900 . ? C211 C212 1.526(5) . ? C211 H21E 0.9900 . ? C211 H21F 0.9900 . ? C212 C213 1.526(6) . ? C212 H21I 0.9900 . ? C212 H21J 0.9900 . ? C213 C214 1.513(5) . ? C213 H21C 0.9900 . ? C213 H21D 0.9900 . ? C214 C215 1.533(6) . ? C214 H21G 0.9900 . ? C214 H21H 0.9900 . ? C215 H21K 0.9800 . ? C215 H21L 0.9800 . ? C215 H21M 0.9800 . ? C301 N301 1.323(5) . ? C301 N302 1.356(5) . ? C301 H301 0.9500 . ? C302 C303 1.362(5) . ? C302 N301 1.377(5) . ? C302 H302 0.9500 . ? C303 N302 1.364(5) . ? C303 H303 0.9500 . ? C304 N302 1.466(5) . ? C304 C305 1.518(5) . ? C304 H30K 0.9900 . ? C304 H30L 0.9900 . ? C305 C306 1.544(5) . ? C305 H30G 0.9900 . ? C305 H30H 0.9900 . ? C306 C307 1.522(5) . ? C306 H30I 0.9900 . ? C306 H30J 0.9900 . ? C307 C308 1.520(5) . ? C307 H30E 0.9900 . ? C307 H30F 0.9900 . ? C308 C309 1.535(5) . ? C308 H30A 0.9900 . ? C308 H30B 0.9900 . ? C309 C310 1.525(5) . ? C309 H30C 0.9900 . ? C309 H30D 0.9900 . ? C310 C311 1.525(5) . ? C310 H31C 0.9900 . ? C310 H31D 0.9900 . ? C311 C312 1.523(5) . ? C311 H31E 0.9900 . ? C311 H31F 0.9900 . ? C312 C313 1.522(5) . ? C312 H31A 0.9900 . ? C312 H31B 0.9900 . ? C313 C314 1.518(5) . ? C313 H31G 0.9900 . ? C313 H31H 0.9900 . ? C314 C315 1.535(5) . ? C314 H31I 0.9900 . ? C314 H31J 0.9900 . ? C315 H31K 0.9800 . ? C315 H31L 0.9800 . ? C315 H31M 0.9800 . ? C401 N401 1.321(5) . ? C401 N402 1.327(5) . ? C401 H401 0.9500 . ? C402 C403 1.352(6) . ? C402 N401 1.385(6) . ? C402 H402 0.9500 . ? C403 N402 1.372(6) . ? C403 H403 0.9500 . ? C404 N402 1.465(5) . ? C404 C405 1.524(5) . ? C404 H40A 0.9900 . ? C404 H40B 0.9900 . ? C405 C406 1.510(6) . ? C405 H40I 0.9900 . ? C405 H40J 0.9900 . ? C406 C407 1.535(5) . ? C406 H40K 0.9900 . ? C406 H40L 0.9900 . ? C407 C408 1.513(6) . ? C407 H40G 0.9900 . ? C407 H40H 0.9900 . ? C408 C409 1.532(5) . ? C408 H40E 0.9900 . ? C408 H40F 0.9900 . ? C409 C410 1.525(6) . ? C409 H40C 0.9900 . ? C409 H40D 0.9900 . ? C410 C411 1.512(5) . ? C410 H41C 0.9900 . ? C410 H41D 0.9900 . ? C411 C412 1.515(6) . ? C411 H41E 0.9900 . ? C411 H41F 0.9900 . ? C412 C413 1.525(5) . ? C412 H41A 0.9900 . ? C412 H41B 0.9900 . ? C413 C414 1.511(6) . ? C413 H41G 0.9900 . ? C413 H41H 0.9900 . ? C414 C415 1.515(6) . ? C414 H41I 0.9900 . ? C414 H41J 0.9900 . ? C415 H41K 0.9800 . ? C415 H41L 0.9800 . ? C415 H41M 0.9800 . ? Cu1 N201 2.049(4) . ? Cu1 N301 2.054(4) . ? Cu1 N101 2.058(3) . ? Cu1 N401 2.062(4) . ? F1 P1 1.576(3) . ? F6 P1 1.571(3) . ? F2 P1 1.514(13) . ? F3 P1 1.650(15) . ? F4 P1 1.553(13) . ? F5 P1 1.513(15) . ? F2A P1 1.579(13) . ? F3A P1 1.487(8) . ? F4A P1 1.571(11) . ? F5A P1 1.568(10) . ? 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 N102 C101 N101 111.7(4) . . ? N102 C101 H101 124.1 . . ? N101 C101 H101 124.1 . . ? N102 C102 C103 106.8(4) . . ? N102 C102 H102 126.6 . . ? C103 C102 H102 126.6 . . ? N101 C103 C102 110.4(4) . . ? N101 C103 H103 124.8 . . ? C102 C103 H103 124.8 . . ? N102 C104 C105 111.5(4) . . ? N102 C104 H10K 109.3 . . ? C105 C104 H10K 109.3 . . ? N102 C104 H10L 109.3 . . ? C105 C104 H10L 109.3 . . ? H10K C104 H10L 108.0 . . ? C104 C105 C106 116.5(4) . . ? C104 C105 H10A 108.2 . . ? C106 C105 H10A 108.2 . . ? C104 C105 H10B 108.2 . . ? C106 C105 H10B 108.2 . . ? H10A C105 H10B 107.3 . . ? C107 C106 C105 113.7(4) . . ? C107 C106 H10I 108.8 . . ? C105 C106 H10I 108.8 . . ? C107 C106 H10J 108.8 . . ? C105 C106 H10J 108.8 . . ? H10I C106 H10J 107.7 . . ? C106 C107 C108 113.7(4) . . ? C106 C107 H10E 108.8 . . ? C108 C107 H10E 108.8 . . ? C106 C107 H10F 108.8 . . ? C108 C107 H10F 108.8 . . ? H10E C107 H10F 107.7 . . ? C109 C108 C107 113.0(4) . . ? C109 C108 H10G 109.0 . . ? C107 C108 H10G 109.0 . . ? C109 C108 H10H 109.0 . . ? C107 C108 H10H 109.0 . . ? H10G C108 H10H 107.8 . . ? C108 C109 C110 114.4(4) . . ? C108 C109 H10C 108.7 . . ? C110 C109 H10C 108.7 . . ? C108 C109 H10D 108.7 . . ? C110 C109 H10D 108.7 . . ? H10C C109 H10D 107.6 . . ? C111 C110 C109 113.7(4) . . ? C111 C110 H11G 108.8 . . ? C109 C110 H11G 108.8 . . ? C111 C110 H11H 108.8 . . ? C109 C110 H11H 108.8 . . ? H11G C110 H11H 107.7 . . ? C110 C111 C112 113.8(4) . . ? C110 C111 H11E 108.8 . . ? C112 C111 H11E 108.8 . . ? C110 C111 H11F 108.8 . . ? C112 C111 H11F 108.8 . . ? H11E C111 H11F 107.7 . . ? C113 C112 C111 114.8(4) . . ? C113 C112 H11A 108.6 . . ? C111 C112 H11A 108.6 . . ? C113 C112 H11B 108.6 . . ? C111 C112 H11B 108.6 . . ? H11A C112 H11B 107.5 . . ? C114 C113 C112 113.5(4) . . ? C114 C113 H11C 108.9 . . ? C112 C113 H11C 108.9 . . ? C114 C113 H11D 108.9 . . ? C112 C113 H11D 108.9 . . ? H11C C113 H11D 107.7 . . ? C113 C114 C115 114.5(4) . . ? C113 C114 H11I 108.6 . . ? C115 C114 H11I 108.6 . . ? C113 C114 H11J 108.6 . . ? C115 C114 H11J 108.6 . . ? H11I C114 H11J 107.6 . . ? C114 C115 H11K 109.5 . . ? C114 C115 H11L 109.5 . . ? H11K C115 H11L 109.5 . . ? C114 C115 H11M 109.5 . . ? H11K C115 H11M 109.5 . . ? H11L C115 H11M 109.5 . . ? N201 C201 N202 111.2(4) . . ? N201 C201 H201 124.4 . . ? N202 C201 H201 124.4 . . ? C203 C202 N202 106.2(4) . . ? C203 C202 H202 126.9 . . ? N202 C202 H202 126.9 . . ? C202 C203 N201 110.5(4) . . ? C202 C203 H203 124.7 . . ? N201 C203 H203 124.7 . . ? N202 C204 C205 113.0(4) . . ? N202 C204 H20I 109.0 . . ? C205 C204 H20I 109.0 . . ? N202 C204 H20J 109.0 . . ? C205 C204 H20J 109.0 . . ? H20I C204 H20J 107.8 . . ? C204 C205 C206 112.5(4) . . ? C204 C205 H20C 109.1 . . ? C206 C205 H20C 109.1 . . ? C204 C205 H20D 109.1 . . ? C206 C205 H20D 109.1 . . ? H20C C205 H20D 107.8 . . ? C205 C206 C207 114.6(4) . . ? C205 C206 H20K 108.6 . . ? C207 C206 H20K 108.6 . . ? C205 C206 H20L 108.6 . . ? C207 C206 H20L 108.6 . . ? H20K C206 H20L 107.6 . . ? C206 C207 C208 112.8(4) . . ? C206 C207 H20E 109.0 . . ? C208 C207 H20E 109.0 . . ? C206 C207 H20F 109.0 . . ? C208 C207 H20F 109.0 . . ? H20E C207 H20F 107.8 . . ? C207 C208 C209 114.7(4) . . ? C207 C208 H20G 108.6 . . ? C209 C208 H20G 108.6 . . ? C207 C208 H20H 108.6 . . ? C209 C208 H20H 108.6 . . ? H20G C208 H20H 107.6 . . ? C208 C209 C210 112.9(4) . . ? C208 C209 H20A 109.0 . . ? C210 C209 H20A 109.0 . . ? C208 C209 H20B 109.0 . . ? C210 C209 H20B 109.0 . . ? H20A C209 H20B 107.8 . . ? C211 C210 C209 114.4(4) . . ? C211 C210 H21A 108.7 . . ? C209 C210 H21A 108.7 . . ? C211 C210 H21B 108.7 . . ? C209 C210 H21B 108.7 . . ? H21A C210 H21B 107.6 . . ? C210 C211 C212 114.2(4) . . ? C210 C211 H21E 108.7 . . ? C212 C211 H21E 108.7 . . ? C210 C211 H21F 108.7 . . ? C212 C211 H21F 108.7 . . ? H21E C211 H21F 107.6 . . ? C213 C212 C211 114.6(4) . . ? C213 C212 H21I 108.6 . . ? C211 C212 H21I 108.6 . . ? C213 C212 H21J 108.6 . . ? C211 C212 H21J 108.6 . . ? H21I C212 H21J 107.6 . . ? C214 C213 C212 114.6(4) . . ? C214 C213 H21C 108.6 . . ? C212 C213 H21C 108.6 . . ? C214 C213 H21D 108.6 . . ? C212 C213 H21D 108.6 . . ? H21C C213 H21D 107.6 . . ? C213 C214 C215 113.5(4) . . ? C213 C214 H21G 108.9 . . ? C215 C214 H21G 108.9 . . ? C213 C214 H21H 108.9 . . ? C215 C214 H21H 108.9 . . ? H21G C214 H21H 107.7 . . ? C214 C215 H21K 109.5 . . ? C214 C215 H21L 109.5 . . ? H21K C215 H21L 109.5 . . ? C214 C215 H21M 109.5 . . ? H21K C215 H21M 109.5 . . ? H21L C215 H21M 109.5 . . ? N301 C301 N302 112.1(4) . . ? N301 C301 H301 124.0 . . ? N302 C301 H301 124.0 . . ? C303 C302 N301 109.8(4) . . ? C303 C302 H302 125.1 . . ? N301 C302 H302 125.1 . . ? C302 C303 N302 106.8(4) . . ? C302 C303 H303 126.6 . . ? N302 C303 H303 126.6 . . ? N302 C304 C305 112.3(3) . . ? N302 C304 H30K 109.1 . . ? C305 C304 H30K 109.1 . . ? N302 C304 H30L 109.1 . . ? C305 C304 H30L 109.1 . . ? H30K C304 H30L 107.9 . . ? C304 C305 C306 114.0(4) . . ? C304 C305 H30G 108.7 . . ? C306 C305 H30G 108.7 . . ? C304 C305 H30H 108.7 . . ? C306 C305 H30H 108.7 . . ? H30G C305 H30H 107.6 . . ? C307 C306 C305 111.2(4) . . ? C307 C306 H30I 109.4 . . ? C305 C306 H30I 109.4 . . ? C307 C306 H30J 109.4 . . ? C305 C306 H30J 109.4 . . ? H30I C306 H30J 108.0 . . ? C308 C307 C306 113.8(4) . . ? C308 C307 H30E 108.8 . . ? C306 C307 H30E 108.8 . . ? C308 C307 H30F 108.8 . . ? C306 C307 H30F 108.8 . . ? H30E C307 H30F 107.7 . . ? C307 C308 C309 112.2(4) . . ? C307 C308 H30A 109.2 . . ? C309 C308 H30A 109.2 . . ? C307 C308 H30B 109.2 . . ? C309 C308 H30B 109.2 . . ? H30A C308 H30B 107.9 . . ? C310 C309 C308 113.8(4) . . ? C310 C309 H30C 108.8 . . ? C308 C309 H30C 108.8 . . ? C310 C309 H30D 108.8 . . ? C308 C309 H30D 108.8 . . ? H30C C309 H30D 107.7 . . ? C309 C310 C311 112.8(4) . . ? C309 C310 H31C 109.0 . . ? C311 C310 H31C 109.0 . . ? C309 C310 H31D 109.0 . . ? C311 C310 H31D 109.0 . . ? H31C C310 H31D 107.8 . . ? C312 C311 C310 113.3(4) . . ? C312 C311 H31E 108.9 . . ? C310 C311 H31E 108.9 . . ? C312 C311 H31F 108.9 . . ? C310 C311 H31F 108.9 . . ? H31E C311 H31F 107.7 . . ? C313 C312 C311 113.9(4) . . ? C313 C312 H31A 108.8 . . ? C311 C312 H31A 108.8 . . ? C313 C312 H31B 108.8 . . ? C311 C312 H31B 108.8 . . ? H31A C312 H31B 107.7 . . ? C314 C313 C312 112.9(4) . . ? C314 C313 H31G 109.0 . . ? C312 C313 H31G 109.0 . . ? C314 C313 H31H 109.0 . . ? C312 C313 H31H 109.0 . . ? H31G C313 H31H 107.8 . . ? C313 C314 C315 113.4(4) . . ? C313 C314 H31I 108.9 . . ? C315 C314 H31I 108.9 . . ? C313 C314 H31J 108.9 . . ? C315 C314 H31J 108.9 . . ? H31I C314 H31J 107.7 . . ? C314 C315 H31K 109.5 . . ? C314 C315 H31L 109.5 . . ? H31K C315 H31L 109.5 . . ? C314 C315 H31M 109.5 . . ? H31K C315 H31M 109.5 . . ? H31L C315 H31M 109.5 . . ? N401 C401 N402 115.5(4) . . ? N401 C401 H401 122.3 . . ? N402 C401 H401 122.3 . . ? C403 C402 N401 111.5(5) . . ? C403 C402 H402 124.3 . . ? N401 C402 H402 124.3 . . ? C402 C403 N402 106.1(5) . . ? C402 C403 H403 127.0 . . ? N402 C403 H403 127.0 . . ? N402 C404 C405 113.7(4) . . ? N402 C404 H40A 108.8 . . ? C405 C404 H40A 108.8 . . ? N402 C404 H40B 108.8 . . ? C405 C404 H40B 108.8 . . ? H40A C404 H40B 107.7 . . ? C406 C405 C404 115.8(4) . . ? C406 C405 H40I 108.3 . . ? C404 C405 H40I 108.3 . . ? C406 C405 H40J 108.3 . . ? C404 C405 H40J 108.3 . . ? H40I C405 H40J 107.4 . . ? C405 C406 C407 112.9(4) . . ? C405 C406 H40K 109.0 . . ? C407 C406 H40K 109.0 . . ? C405 C406 H40L 109.0 . . ? C407 C406 H40L 109.0 . . ? H40K C406 H40L 107.8 . . ? C408 C407 C406 115.4(4) . . ? C408 C407 H40G 108.4 . . ? C406 C407 H40G 108.4 . . ? C408 C407 H40H 108.4 . . ? C406 C407 H40H 108.4 . . ? H40G C407 H40H 107.5 . . ? C407 C408 C409 113.7(4) . . ? C407 C408 H40E 108.8 . . ? C409 C408 H40E 108.8 . . ? C407 C408 H40F 108.8 . . ? C409 C408 H40F 108.8 . . ? H40E C408 H40F 107.7 . . ? C410 C409 C408 114.8(4) . . ? C410 C409 H40C 108.6 . . ? C408 C409 H40C 108.6 . . ? C410 C409 H40D 108.6 . . ? C408 C409 H40D 108.6 . . ? H40C C409 H40D 107.5 . . ? C411 C410 C409 114.4(4) . . ? C411 C410 H41C 108.7 . . ? C409 C410 H41C 108.7 . . ? C411 C410 H41D 108.7 . . ? C409 C410 H41D 108.7 . . ? H41C C410 H41D 107.6 . . ? C410 C411 C412 113.5(4) . . ? C410 C411 H41E 108.9 . . ? C412 C411 H41E 108.9 . . ? C410 C411 H41F 108.9 . . ? C412 C411 H41F 108.9 . . ? H41E C411 H41F 107.7 . . ? C411 C412 C413 115.4(4) . . ? C411 C412 H41A 108.4 . . ? C413 C412 H41A 108.4 . . ? C411 C412 H41B 108.4 . . ? C413 C412 H41B 108.4 . . ? H41A C412 H41B 107.5 . . ? C414 C413 C412 114.0(4) . . ? C414 C413 H41G 108.8 . . ? C412 C413 H41G 108.8 . . ? C414 C413 H41H 108.8 . . ? C412 C413 H41H 108.8 . . ? H41G C413 H41H 107.7 . . ? C413 C414 C415 113.3(4) . . ? C413 C414 H41I 108.9 . . ? C415 C414 H41I 108.9 . . ? C413 C414 H41J 108.9 . . ? C415 C414 H41J 108.9 . . ? H41I C414 H41J 107.7 . . ? C414 C415 H41K 109.5 . . ? C414 C415 H41L 109.5 . . ? H41K C415 H41L 109.5 . . ? C414 C415 H41M 109.5 . . ? H41K C415 H41M 109.5 . . ? H41L C415 H41M 109.5 . . ? N201 Cu1 N301 109.61(15) . . ? N201 Cu1 N101 109.43(15) . . ? N301 Cu1 N101 118.02(14) . . ? N201 Cu1 N401 113.80(15) . . ? N301 Cu1 N401 106.86(16) . . ? N101 Cu1 N401 98.88(16) . . ? C103 N101 C101 104.6(4) . . ? C103 N101 Cu1 129.5(3) . . ? C101 N101 Cu1 124.0(3) . . ? C101 N102 C102 106.5(4) . . ? C101 N102 C104 125.4(4) . . ? C102 N102 C104 127.9(4) . . ? C201 N201 C203 104.6(4) . . ? C201 N201 Cu1 128.0(3) . . ? C203 N201 Cu1 127.0(3) . . ? C201 N202 C202 107.4(4) . . ? C201 N202 C204 126.2(4) . . ? C202 N202 C204 126.4(4) . . ? C301 N301 C302 104.9(4) . . ? C301 N301 Cu1 127.9(3) . . ? C302 N301 Cu1 123.8(3) . . ? C301 N302 C303 106.5(4) . . ? C301 N302 C304 125.1(4) . . ? C303 N302 C304 128.4(4) . . ? C401 N401 C402 101.6(4) . . ? C401 N401 Cu1 131.3(4) . . ? C402 N401 Cu1 126.7(4) . . ? C401 N402 C403 105.3(4) . . ? C401 N402 C404 130.0(4) . . ? C403 N402 C404 124.6(5) . . ? F3A P1 F5 153.1(14) . . ? F3A P1 F2 112.7(9) . . ? F5 P1 F2 91.3(13) . . ? F3A P1 F4 60.8(11) . . ? F5 P1 F4 96.1(12) . . ? F2 P1 F4 172.1(13) . . ? F3A P1 F5A 175.6(8) . . ? F2 P1 F5A 66.7(9) . . ? F4 P1 F5A 120.1(13) . . ? F3A P1 F6 83.0(5) . . ? F5 P1 F6 88.9(8) . . ? F2 P1 F6 81.9(7) . . ? F4 P1 F6 101.1(7) . . ? F5A P1 F6 92.5(6) . . ? F3A P1 F4A 89.5(6) . . ? F5 P1 F4A 64.2(12) . . ? F2 P1 F4A 151.8(8) . . ? F5A P1 F4A 89.8(8) . . ? F6 P1 F4A 83.9(6) . . ? F3A P1 F1 98.9(5) . . ? F5 P1 F1 89.0(8) . . ? F2 P1 F1 98.1(7) . . ? F4 P1 F1 79.1(7) . . ? F5A P1 F1 85.5(6) . . ? F6 P1 F1 177.9(2) . . ? F4A P1 F1 95.2(6) . . ? F3A P1 F2A 90.0(9) . . ? F5 P1 F2A 116.4(13) . . ? F4 P1 F2A 143.2(11) . . ? F5A P1 F2A 90.8(9) . . ? F6 P1 F2A 96.4(7) . . ? F4A P1 F2A 179.3(10) . . ? F1 P1 F2A 84.5(7) . . ? F5 P1 F3 174.7(13) . . ? F2 P1 F3 85.8(12) . . ? F4 P1 F3 86.6(11) . . ? F5A P1 F3 150.1(13) . . ? F6 P1 F3 95.1(9) . . ? F4A P1 F3 119.7(12) . . ? F1 P1 F3 87.0(9) . . ? F2A P1 F3 59.7(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N102 C102 C103 N101 -0.3(6) . . . . ? N102 C104 C105 C106 -60.5(5) . . . . ? C104 C105 C106 C107 -63.7(5) . . . . ? C105 C106 C107 C108 174.1(4) . . . . ? C106 C107 C108 C109 -176.4(4) . . . . ? C107 C108 C109 C110 173.0(4) . . . . ? C108 C109 C110 C111 -177.2(4) . . . . ? C109 C110 C111 C112 178.3(4) . . . . ? C110 C111 C112 C113 -178.4(4) . . . . ? C111 C112 C113 C114 -178.3(4) . . . . ? C112 C113 C114 C115 179.9(4) . . . . ? N202 C202 C203 N201 0.6(5) . . . . ? N202 C204 C205 C206 169.2(4) . . . . ? C204 C205 C206 C207 173.2(4) . . . . ? C205 C206 C207 C208 168.6(4) . . . . ? C206 C207 C208 C209 175.2(4) . . . . ? C207 C208 C209 C210 173.5(4) . . . . ? C208 C209 C210 C211 177.3(4) . . . . ? C209 C210 C211 C212 176.4(4) . . . . ? C210 C211 C212 C213 179.6(4) . . . . ? C211 C212 C213 C214 178.0(4) . . . . ? C212 C213 C214 C215 177.5(4) . . . . ? N301 C302 C303 N302 -0.1(5) . . . . ? N302 C304 C305 C306 70.2(5) . . . . ? C304 C305 C306 C307 -173.0(3) . . . . ? C305 C306 C307 C308 -178.0(3) . . . . ? C306 C307 C308 C309 -168.2(3) . . . . ? C307 C308 C309 C310 179.1(3) . . . . ? C308 C309 C310 C311 -176.1(3) . . . . ? C309 C310 C311 C312 -179.4(3) . . . . ? C310 C311 C312 C313 -178.7(3) . . . . ? C311 C312 C313 C314 -179.6(4) . . . . ? C312 C313 C314 C315 -179.5(4) . . . . ? N401 C402 C403 N402 -0.9(7) . . . . ? N402 C404 C405 C406 77.8(5) . . . . ? C404 C405 C406 C407 176.7(4) . . . . ? C405 C406 C407 C408 -172.9(4) . . . . ? C406 C407 C408 C409 178.7(4) . . . . ? C407 C408 C409 C410 -177.7(4) . . . . ? C408 C409 C410 C411 -179.4(4) . . . . ? C409 C410 C411 C412 -178.7(4) . . . . ? C410 C411 C412 C413 -179.1(4) . . . . ? C411 C412 C413 C414 -179.2(4) . . . . ? C412 C413 C414 C415 -179.0(4) . . . . ? C102 C103 N101 C101 0.2(6) . . . . ? C102 C103 N101 Cu1 -164.3(4) . . . . ? N102 C101 N101 C103 -0.1(5) . . . . ? N102 C101 N101 Cu1 165.6(3) . . . . ? N201 Cu1 N101 C103 -147.7(4) . . . . ? N301 Cu1 N101 C103 -21.5(5) . . . . ? N401 Cu1 N101 C103 93.0(4) . . . . ? N201 Cu1 N101 C101 50.4(4) . . . . ? N301 Cu1 N101 C101 176.6(4) . . . . ? N401 Cu1 N101 C101 -68.8(4) . . . . ? N101 C101 N102 C102 -0.1(5) . . . . ? N101 C101 N102 C104 174.8(4) . . . . ? C103 C102 N102 C101 0.3(6) . . . . ? C103 C102 N102 C104 -174.5(5) . . . . ? C105 C104 N102 C101 -82.2(5) . . . . ? C105 C104 N102 C102 91.6(6) . . . . ? N202 C201 N201 C203 0.8(5) . . . . ? N202 C201 N201 Cu1 174.7(3) . . . . ? C202 C203 N201 C201 -0.9(5) . . . . ? C202 C203 N201 Cu1 -174.8(3) . . . . ? N301 Cu1 N201 C201 158.8(4) . . . . ? N101 Cu1 N201 C201 -70.4(4) . . . . ? N401 Cu1 N201 C201 39.2(4) . . . . ? N301 Cu1 N201 C203 -28.7(4) . . . . ? N101 Cu1 N201 C203 102.2(4) . . . . ? N401 Cu1 N201 C203 -148.2(3) . . . . ? N201 C201 N202 C202 -0.5(5) . . . . ? N201 C201 N202 C204 -179.1(4) . . . . ? C203 C202 N202 C201 -0.1(5) . . . . ? C203 C202 N202 C204 178.5(4) . . . . ? C205 C204 N202 C201 -125.3(5) . . . . ? C205 C204 N202 C202 56.4(6) . . . . ? N302 C301 N301 C302 0.4(5) . . . . ? N302 C301 N301 Cu1 -159.2(3) . . . . ? C303 C302 N301 C301 -0.2(5) . . . . ? C303 C302 N301 Cu1 160.6(3) . . . . ? N201 Cu1 N301 C301 28.5(4) . . . . ? N101 Cu1 N301 C301 -97.6(4) . . . . ? N401 Cu1 N301 C301 152.3(4) . . . . ? N201 Cu1 N301 C302 -127.7(3) . . . . ? N101 Cu1 N301 C302 106.2(3) . . . . ? N401 Cu1 N301 C302 -3.9(4) . . . . ? N301 C301 N302 C303 -0.5(5) . . . . ? N301 C301 N302 C304 177.3(4) . . . . ? C302 C303 N302 C301 0.4(5) . . . . ? C302 C303 N302 C304 -177.3(4) . . . . ? C305 C304 N302 C301 84.2(5) . . . . ? C305 C304 N302 C303 -98.5(5) . . . . ? N402 C401 N401 C402 1.5(5) . . . . ? N402 C401 N401 Cu1 173.9(3) . . . . ? C403 C402 N401 C401 -0.3(6) . . . . ? C403 C402 N401 Cu1 -173.2(4) . . . . ? N201 Cu1 N401 C401 75.9(4) . . . . ? N301 Cu1 N401 C401 -45.3(5) . . . . ? N101 Cu1 N401 C401 -168.2(4) . . . . ? N201 Cu1 N401 C402 -113.4(4) . . . . ? N301 Cu1 N401 C402 125.5(4) . . . . ? N101 Cu1 N401 C402 2.5(4) . . . . ? N401 C401 N402 C403 -2.1(6) . . . . ? N401 C401 N402 C404 -179.9(4) . . . . ? C402 C403 N402 C401 1.7(6) . . . . ? C402 C403 N402 C404 179.7(4) . . . . ? C405 C404 N402 C401 -100.6(5) . . . . ? C405 C404 N402 C403 81.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.202 _refine_diff_density_min -0.274 _refine_diff_density_rms 0.038 #===END data_msb1_23 _database_code_depnum_ccdc_archive 'CCDC 769704' #TrackingRef 'MarionStricker.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C90 H168 Cu6 I6 N12' _chemical_formula_sum 'C90 H168 Cu6 I6 N12' _chemical_formula_weight 2561.07 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' I I -0.4742 1.8119 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7553(12) _cell_length_b 13.5795(17) _cell_length_c 20.6572(30) _cell_angle_alpha 106.873(16) _cell_angle_beta 94.154(16) _cell_angle_gamma 95.814(15) _cell_volume 2590.3(6) _cell_formula_units_Z 1 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.05 _cell_measurement_theta_max 26 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1284 _exptl_absorpt_coefficient_mu 3.044 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5264 _exptl_absorpt_correction_T_max 0.6367 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS I' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25669 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 26.05 _reflns_number_total 9463 _reflns_number_gt 7029 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SIR97 (Giacovazzo et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0542P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9463 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0787 _refine_ls_wR_factor_gt 0.0721 _refine_ls_goodness_of_fit_ref 0.880 _refine_ls_restrained_S_all 0.880 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.002 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 C101 C 0.7159(3) 0.2849(3) 0.38918(17) 0.0266(8) Uani 1 1 d . . . H101 H 0.6326 0.2522 0.3636 0.032 Uiso 1 1 calc R . . C102 C 0.8653(3) 0.3881(3) 0.46572(17) 0.0285(8) Uani 1 1 d . . . H102 H 0.9044 0.4417 0.5039 0.034 Uiso 1 1 calc R . . C103 C 0.9363(3) 0.3218(3) 0.42306(17) 0.0303(9) Uani 1 1 d . . . H103 H 1.0318 0.3212 0.4264 0.036 Uiso 1 1 calc R . . C104 C 0.8691(3) 0.1676(3) 0.31887(18) 0.0300(8) Uani 1 1 d . . . H10A H 0.7817 0.1286 0.2956 0.036 Uiso 1 1 calc R . . H10B H 0.9188 0.1223 0.3379 0.036 Uiso 1 1 calc R . . C105 C 0.9537(3) 0.1998(3) 0.26737(18) 0.0287(8) Uani 1 1 d . . . H10C H 0.9005 0.2392 0.2447 0.034 Uiso 1 1 calc R . . H10D H 1.0378 0.2440 0.2908 0.034 Uiso 1 1 calc R . . C106 C 0.9911(3) 0.1045(3) 0.21470(18) 0.0288(8) Uani 1 1 d . . . H10E H 0.9068 0.0595 0.1926 0.035 Uiso 1 1 calc R . . H10F H 1.0460 0.0664 0.2376 0.035 Uiso 1 1 calc R . . C107 C 1.0725(4) 0.1327(3) 0.16060(17) 0.0286(8) Uani 1 1 d . . . H10G H 1.0169 0.1698 0.1372 0.034 Uiso 1 1 calc R . . H10H H 1.1560 0.1788 0.1828 0.034 Uiso 1 1 calc R . . C108 C 1.1126(3) 0.0380(3) 0.10854(17) 0.0290(8) Uani 1 1 d . . . H10I H 1.1688 0.0013 0.1320 0.035 Uiso 1 1 calc R . . H10J H 1.0291 -0.0084 0.0867 0.035 Uiso 1 1 calc R . . C109 C 1.1926(3) 0.0652(3) 0.05406(17) 0.0261(8) Uani 1 1 d . . . H10K H 1.1356 0.1007 0.0300 0.031 Uiso 1 1 calc R . . H10L H 1.2751 0.1127 0.0759 0.031 Uiso 1 1 calc R . . C110 C 1.2353(3) -0.0291(3) 0.00277(17) 0.0286(8) Uani 1 1 d . . . H11A H 1.2918 -0.0649 0.0268 0.034 Uiso 1 1 calc R . . H11B H 1.1529 -0.0764 -0.0194 0.034 Uiso 1 1 calc R . . C111 C 1.3161(3) -0.0010(3) -0.05112(17) 0.0277(8) Uani 1 1 d . . . H11C H 1.3981 0.0467 -0.0288 0.033 Uiso 1 1 calc R . . H11D H 1.2592 0.0346 -0.0751 0.033 Uiso 1 1 calc R . . C112 C 1.3601(3) -0.0947(3) -0.10266(17) 0.0283(8) Uani 1 1 d . . . H11E H 1.2780 -0.1419 -0.1256 0.034 Uiso 1 1 calc R . . H11F H 1.4158 -0.1310 -0.0786 0.034 Uiso 1 1 calc R . . C113 C 1.4430(3) -0.0656(3) -0.15593(18) 0.0292(8) Uani 1 1 d . . . H11G H 1.3864 -0.0306 -0.1806 0.035 Uiso 1 1 calc R . . H11H H 1.5239 -0.0171 -0.1329 0.035 Uiso 1 1 calc R . . C114 C 1.4900(3) -0.1582(3) -0.20655(18) 0.0311(8) Uani 1 1 d . . . H11I H 1.4092 -0.2067 -0.2297 0.037 Uiso 1 1 calc R . . H11J H 1.5466 -0.1933 -0.1820 0.037 Uiso 1 1 calc R . . C115 C 1.5728(4) -0.1281(3) -0.25943(19) 0.0401(10) Uani 1 1 d . . . H11K H 1.5999 -0.1893 -0.2900 0.060 Uiso 1 1 calc R . . H11L H 1.6540 -0.0813 -0.2369 0.060 Uiso 1 1 calc R . . H11M H 1.5166 -0.0949 -0.2847 0.060 Uiso 1 1 calc R . . C201 C 0.1380(3) 0.3937(3) 0.59168(17) 0.0264(8) Uani 1 1 d . . . H201 H 0.1988 0.4535 0.5968 0.032 Uiso 1 1 calc R . . C202 C 0.0424(3) 0.2365(3) 0.55898(18) 0.0298(8) Uani 1 1 d . . . H202 H 0.0254 0.1657 0.5366 0.036 Uiso 1 1 calc R . . C203 C -0.0377(3) 0.2904(3) 0.60290(18) 0.0309(8) Uani 1 1 d . . . H203 H -0.1190 0.2640 0.6162 0.037 Uiso 1 1 calc R . . C204 C -0.0291(4) 0.4819(3) 0.66794(19) 0.0343(9) Uani 1 1 d . . . H20A H -0.0935 0.5074 0.6406 0.041 Uiso 1 1 calc R . . H20B H 0.0478 0.5364 0.6871 0.041 Uiso 1 1 calc R . . C205 C -0.1011(3) 0.4585(3) 0.72513(18) 0.0299(8) Uani 1 1 d . . . H20C H -0.0389 0.4283 0.7506 0.036 Uiso 1 1 calc R . . H20D H -0.1820 0.4077 0.7060 0.036 Uiso 1 1 calc R . . C206 C -0.1457(4) 0.5550(3) 0.77332(18) 0.0305(8) Uani 1 1 d . . . H20E H -0.2049 0.5868 0.7476 0.037 Uiso 1 1 calc R . . H20F H -0.0644 0.6046 0.7940 0.037 Uiso 1 1 calc R . . C207 C -0.2236(4) 0.5295(3) 0.82924(18) 0.0299(8) Uani 1 1 d . . . H20G H -0.3063 0.4817 0.8083 0.036 Uiso 1 1 calc R . . H20H H -0.1655 0.4947 0.8532 0.036 Uiso 1 1 calc R . . C208 C -0.2652(3) 0.6237(3) 0.88032(17) 0.0288(8) Uani 1 1 d . . . H20I H -0.3231 0.6588 0.8564 0.035 Uiso 1 1 calc R . . H20J H -0.1826 0.6714 0.9016 0.035 Uiso 1 1 calc R . . C209 C -0.3435(3) 0.5971(3) 0.93561(18) 0.0291(8) Uani 1 1 d . . . H20K H -0.4262 0.5494 0.9142 0.035 Uiso 1 1 calc R . . H20L H -0.2856 0.5616 0.9593 0.035 Uiso 1 1 calc R . . C210 C -0.3855(3) 0.6905(3) 0.98726(18) 0.0296(8) Uani 1 1 d . . . H21A H -0.4428 0.7263 0.9637 0.036 Uiso 1 1 calc R . . H21B H -0.3028 0.7378 1.0091 0.036 Uiso 1 1 calc R . . C211 C -0.4646(3) 0.6627(3) 1.04170(17) 0.0293(8) Uani 1 1 d . . . H21C H -0.4072 0.6272 1.0655 0.035 Uiso 1 1 calc R . . H21D H -0.5470 0.6150 1.0199 0.035 Uiso 1 1 calc R . . C212 C -0.5074(3) 0.7568(3) 1.09336(18) 0.0285(8) Uani 1 1 d . . . H21E H -0.4249 0.8040 1.1156 0.034 Uiso 1 1 calc R . . H21F H -0.5638 0.7928 1.0694 0.034 Uiso 1 1 calc R . . C213 C -0.5884(3) 0.7292(3) 1.14750(18) 0.0295(8) Uani 1 1 d . . . H21G H -0.6698 0.6807 1.1253 0.035 Uiso 1 1 calc R . . H21H H -0.5312 0.6948 1.1722 0.035 Uiso 1 1 calc R . . C214 C -0.6339(4) 0.8232(3) 1.19790(19) 0.0326(8) Uani 1 1 d . . . H21I H -0.6901 0.8583 1.1732 0.039 Uiso 1 1 calc R . . H21J H -0.5526 0.8713 1.2208 0.039 Uiso 1 1 calc R . . C215 C -0.7170(4) 0.7941(4) 1.25122(19) 0.0406(10) Uani 1 1 d . . . H21K H -0.7434 0.8556 1.2816 0.061 Uiso 1 1 calc R . . H21L H -0.6610 0.7608 1.2766 0.061 Uiso 1 1 calc R . . H21M H -0.7986 0.7475 1.2289 0.061 Uiso 1 1 calc R . . C301 C 0.5888(3) -0.0433(3) 0.37882(18) 0.0287(8) Uani 1 1 d . . . H301 H 0.5041 -0.0762 0.3549 0.034 Uiso 1 1 calc R . . C302 C 0.7430(3) 0.0648(3) 0.44980(18) 0.0313(8) Uani 1 1 d . . . H302 H 0.7849 0.1221 0.4850 0.038 Uiso 1 1 calc R . . C303 C 0.8103(3) -0.0082(3) 0.41227(18) 0.0296(8) Uani 1 1 d . . . H303 H 0.9053 -0.0112 0.4164 0.035 Uiso 1 1 calc R . . C304 C 0.7351(4) -0.1705(3) 0.31319(18) 0.0305(8) Uani 1 1 d . . . H30A H 0.6466 -0.2105 0.2923 0.037 Uiso 1 1 calc R . . H30B H 0.7871 -0.2133 0.3334 0.037 Uiso 1 1 calc R . . C305 C 0.8491(3) -0.2382(3) 0.20534(18) 0.0289(8) Uani 1 1 d . . . H30C H 0.7639 -0.2829 0.1844 0.035 Uiso 1 1 calc R . . H30D H 0.9053 -0.2765 0.2276 0.035 Uiso 1 1 calc R . . C306 C 0.8147(4) -0.1426(3) 0.25852(18) 0.0303(8) Uani 1 1 d . . . H30E H 0.7596 -0.1038 0.2362 0.036 Uiso 1 1 calc R . . H30F H 0.9000 -0.0984 0.2800 0.036 Uiso 1 1 calc R . . C307 C 0.9272(4) -0.2108(3) 0.14983(18) 0.0303(8) Uani 1 1 d . . . H30G H 0.8693 -0.1748 0.1266 0.036 Uiso 1 1 calc R . . H30H H 1.0103 -0.1636 0.1712 0.036 Uiso 1 1 calc R . . C308 C 0.9681(3) -0.3044(3) 0.09759(18) 0.0284(8) Uani 1 1 d . . . H30I H 0.8851 -0.3514 0.0759 0.034 Uiso 1 1 calc R . . H30J H 1.0255 -0.3408 0.1208 0.034 Uiso 1 1 calc R . . C309 C 1.0471(3) -0.2760(3) 0.04282(18) 0.0293(8) Uani 1 1 d . . . H30K H 0.9892 -0.2406 0.0191 0.035 Uiso 1 1 calc R . . H30L H 1.1293 -0.2281 0.0646 0.035 Uiso 1 1 calc R . . C310 C 1.0903(3) -0.3698(3) -0.00894(18) 0.0286(8) Uani 1 1 d . . . H31A H 1.0081 -0.4177 -0.0308 0.034 Uiso 1 1 calc R . . H31B H 1.1481 -0.4052 0.0147 0.034 Uiso 1 1 calc R . . C311 C 1.1693(3) -0.3410(3) -0.06337(18) 0.0300(8) Uani 1 1 d . . . H31C H 1.2513 -0.2931 -0.0413 0.036 Uiso 1 1 calc R . . H31D H 1.1113 -0.3055 -0.0869 0.036 Uiso 1 1 calc R . . C312 C 1.2132(3) -0.4341(3) -0.11559(18) 0.0296(8) Uani 1 1 d . . . H31E H 1.1313 -0.4820 -0.1378 0.035 Uiso 1 1 calc R . . H31F H 1.2711 -0.4698 -0.0922 0.035 Uiso 1 1 calc R . . C313 C 1.2925(4) -0.4041(3) -0.16972(18) 0.0306(8) Uani 1 1 d . . . H31G H 1.2345 -0.3682 -0.1930 0.037 Uiso 1 1 calc R . . H31H H 1.3743 -0.3560 -0.1474 0.037 Uiso 1 1 calc R . . C314 C 1.3372(4) -0.4961(3) -0.22226(19) 0.0349(9) Uani 1 1 d . . . H31I H 1.2556 -0.5436 -0.2455 0.042 Uiso 1 1 calc R . . H31J H 1.3943 -0.5327 -0.1992 0.042 Uiso 1 1 calc R . . C315 C 1.4183(4) -0.4633(4) -0.2748(2) 0.0431(10) Uani 1 1 d . . . H31K H 1.4442 -0.5236 -0.3067 0.065 Uiso 1 1 calc R . . H31L H 1.5002 -0.4174 -0.2521 0.065 Uiso 1 1 calc R . . H31M H 1.3616 -0.4283 -0.2984 0.065 Uiso 1 1 calc R . . N101 N 0.7262(3) 0.3641(2) 0.44394(14) 0.0252(6) Uani 1 1 d . . . N102 N 0.8415(2) 0.2562(2) 0.37430(14) 0.0237(6) Uani 1 1 d . . . N201 N 0.1535(3) 0.3021(2) 0.55213(14) 0.0268(7) Uani 1 1 d . . . N202 N 0.0228(3) 0.3913(2) 0.62429(14) 0.0262(7) Uani 1 1 d . . . N301 N 0.6044(3) 0.0440(2) 0.42959(14) 0.0269(7) Uani 1 1 d . . . N302 N 0.7115(3) -0.0784(2) 0.36615(14) 0.0253(6) Uani 1 1 d . . . Cu1 Cu 0.57118(4) 0.41916(4) 0.49739(2) 0.03631(13) Uani 1 1 d . . . Cu2 Cu 0.30224(4) 0.26721(4) 0.49038(2) 0.03626(13) Uani 1 1 d . . . Cu3 Cu 0.45871(4) 0.12688(4) 0.46643(2) 0.03274(12) Uani 1 1 d . . . I1 I 0.344460(19) 0.396292(19) 0.414864(11) 0.02676(7) Uani 1 1 d . . . I2 I 0.53752(2) 0.281978(19) 0.573229(11) 0.02805(7) Uani 1 1 d . . . I3 I 0.21621(2) 0.07650(2) 0.403882(12) 0.03451(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 C101 0.0151(14) 0.034(2) 0.0283(18) 0.0045(16) 0.0042(12) 0.0054(13) C102 0.0177(15) 0.037(2) 0.0272(18) 0.0041(16) 0.0035(13) 0.0018(14) C103 0.0140(14) 0.050(3) 0.0292(19) 0.0147(17) 0.0027(13) 0.0050(14) C104 0.0329(18) 0.023(2) 0.036(2) 0.0073(16) 0.0144(15) 0.0080(14) C105 0.0308(17) 0.028(2) 0.0305(19) 0.0105(16) 0.0144(14) 0.0073(14) C106 0.0340(18) 0.026(2) 0.0286(19) 0.0088(16) 0.0127(14) 0.0072(14) C107 0.0356(18) 0.025(2) 0.0270(18) 0.0079(15) 0.0125(14) 0.0077(14) C108 0.0328(17) 0.030(2) 0.0257(18) 0.0079(16) 0.0111(14) 0.0075(15) C109 0.0315(17) 0.020(2) 0.0279(18) 0.0073(15) 0.0097(14) 0.0049(14) C110 0.0307(17) 0.025(2) 0.0303(19) 0.0077(16) 0.0112(14) 0.0037(14) C111 0.0345(17) 0.020(2) 0.0285(19) 0.0052(15) 0.0112(14) 0.0034(14) C112 0.0308(17) 0.028(2) 0.0270(18) 0.0066(15) 0.0101(14) 0.0059(14) C113 0.0311(17) 0.026(2) 0.0311(19) 0.0073(16) 0.0112(14) 0.0042(14) C114 0.0315(17) 0.028(2) 0.032(2) 0.0044(16) 0.0106(14) 0.0045(15) C115 0.039(2) 0.044(3) 0.031(2) 0.0017(18) 0.0157(16) 0.0018(17) C201 0.0194(15) 0.033(2) 0.0269(18) 0.0079(16) 0.0049(13) 0.0052(13) C202 0.0237(16) 0.027(2) 0.037(2) 0.0069(16) 0.0049(14) 0.0052(14) C203 0.0238(16) 0.035(3) 0.033(2) 0.0101(17) 0.0065(14) 0.0009(15) C204 0.0369(19) 0.036(3) 0.035(2) 0.0104(17) 0.0153(16) 0.0182(16) C205 0.0324(17) 0.028(2) 0.0324(19) 0.0102(16) 0.0115(14) 0.0086(15) C206 0.0340(18) 0.031(2) 0.0304(19) 0.0107(16) 0.0130(15) 0.0103(15) C207 0.0347(18) 0.025(2) 0.0322(19) 0.0088(16) 0.0133(15) 0.0068(15) C208 0.0326(17) 0.027(2) 0.0292(19) 0.0089(16) 0.0115(14) 0.0066(14) C209 0.0329(17) 0.026(2) 0.0315(19) 0.0108(16) 0.0118(14) 0.0075(14) C210 0.0322(17) 0.027(2) 0.0314(19) 0.0089(16) 0.0123(14) 0.0068(15) C211 0.0316(17) 0.029(2) 0.0285(19) 0.0083(16) 0.0105(14) 0.0067(15) C212 0.0312(17) 0.024(2) 0.0315(19) 0.0090(16) 0.0096(14) 0.0045(14) C213 0.0303(17) 0.031(2) 0.0291(19) 0.0107(16) 0.0104(14) 0.0044(14) C214 0.0335(18) 0.031(2) 0.034(2) 0.0083(17) 0.0093(15) 0.0032(15) C215 0.040(2) 0.048(3) 0.031(2) 0.0055(19) 0.0139(16) 0.0031(18) C301 0.0215(15) 0.029(2) 0.035(2) 0.0059(17) 0.0090(13) 0.0063(14) C302 0.0280(17) 0.036(2) 0.0281(19) 0.0060(16) 0.0036(14) 0.0058(15) C303 0.0188(15) 0.036(2) 0.035(2) 0.0106(17) 0.0051(14) 0.0045(14) C304 0.0330(17) 0.029(2) 0.033(2) 0.0105(16) 0.0131(15) 0.0089(15) C305 0.0330(17) 0.025(2) 0.0307(19) 0.0086(16) 0.0117(14) 0.0075(14) C306 0.0348(18) 0.028(2) 0.033(2) 0.0119(16) 0.0156(15) 0.0088(15) C307 0.0336(17) 0.028(2) 0.0317(19) 0.0087(16) 0.0131(15) 0.0066(15) C308 0.0318(17) 0.024(2) 0.0318(19) 0.0105(16) 0.0113(14) 0.0050(14) C309 0.0310(17) 0.030(2) 0.0295(19) 0.0113(16) 0.0099(14) 0.0055(15) C310 0.0293(16) 0.027(2) 0.0321(19) 0.0110(16) 0.0103(14) 0.0046(14) C311 0.0310(17) 0.030(2) 0.0300(19) 0.0089(16) 0.0104(14) 0.0054(15) C312 0.0313(17) 0.027(2) 0.0323(19) 0.0092(16) 0.0100(14) 0.0069(14) C313 0.0338(18) 0.025(2) 0.033(2) 0.0080(16) 0.0109(15) 0.0023(15) C314 0.0336(18) 0.037(3) 0.034(2) 0.0072(18) 0.0112(15) 0.0086(16) C315 0.047(2) 0.042(3) 0.036(2) 0.0023(19) 0.0165(17) 0.0030(18) N101 0.0196(12) 0.0290(19) 0.0267(15) 0.0062(13) 0.0054(11) 0.0062(11) N102 0.0204(12) 0.0280(19) 0.0252(15) 0.0086(13) 0.0090(11) 0.0078(11) N201 0.0212(13) 0.033(2) 0.0278(15) 0.0086(14) 0.0074(11) 0.0098(12) N202 0.0236(13) 0.0279(19) 0.0276(15) 0.0065(13) 0.0072(11) 0.0087(12) N301 0.0260(14) 0.0245(19) 0.0265(15) 0.0021(13) 0.0007(11) 0.0039(12) N302 0.0227(13) 0.0255(19) 0.0302(16) 0.0091(13) 0.0107(11) 0.0061(11) Cu1 0.0261(2) 0.0436(3) 0.0360(3) 0.0023(2) 0.00762(18) 0.01464(19) Cu2 0.0280(2) 0.0446(3) 0.0374(3) 0.0081(2) 0.01226(18) 0.0167(2) Cu3 0.0258(2) 0.0331(3) 0.0395(3) 0.0073(2) 0.01081(18) 0.01037(18) I1 0.02103(10) 0.02880(15) 0.02897(12) 0.00626(10) 0.00250(8) 0.00355(8) I2 0.02428(11) 0.03042(16) 0.02989(13) 0.00922(10) 0.00303(8) 0.00500(9) I3 0.02509(11) 0.03695(17) 0.03623(14) 0.00292(11) 0.00599(9) 0.00171(9) _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 C101 N101 1.305(4) . ? C101 N102 1.353(4) . ? C101 H101 0.9300 . ? C102 C103 1.350(5) . ? C102 N101 1.373(4) . ? C102 H102 0.9300 . ? C103 N102 1.357(4) . ? C103 H103 0.9300 . ? C104 N102 1.464(4) . ? C104 C105 1.526(5) . ? C104 H10A 0.9700 . ? C104 H10B 0.9700 . ? C105 C106 1.526(5) . ? C105 H10C 0.9700 . ? C105 H10D 0.9700 . ? C106 C107 1.530(4) . ? C106 H10E 0.9700 . ? C106 H10F 0.9700 . ? C107 C108 1.524(5) . ? C107 H10G 0.9700 . ? C107 H10H 0.9700 . ? C108 C109 1.524(4) . ? C108 H10I 0.9700 . ? C108 H10J 0.9700 . ? C109 C110 1.523(5) . ? C109 H10K 0.9700 . ? C109 H10L 0.9700 . ? C110 C111 1.523(4) . ? C110 H11A 0.9700 . ? C110 H11B 0.9700 . ? C111 C112 1.526(5) . ? C111 H11C 0.9700 . ? C111 H11D 0.9700 . ? C112 C113 1.529(5) . ? C112 H11E 0.9700 . ? C112 H11F 0.9700 . ? C113 C114 1.520(5) . ? C113 H11G 0.9700 . ? C113 H11H 0.9700 . ? C114 C115 1.528(5) . ? C114 H11I 0.9700 . ? C114 H11J 0.9700 . ? C115 H11K 0.9600 . ? C115 H11L 0.9600 . ? C115 H11M 0.9600 . ? C201 N201 1.306(5) . ? C201 N202 1.354(4) . ? C201 H201 0.9300 . ? C202 C203 1.343(5) . ? C202 N201 1.373(5) . ? C202 H202 0.9300 . ? C203 N202 1.367(5) . ? C203 H203 0.9300 . ? C204 N202 1.461(4) . ? C204 C205 1.511(5) . ? C204 H20A 0.9700 . ? C204 H20B 0.9700 . ? C205 C206 1.523(5) . ? C205 H20C 0.9700 . ? C205 H20D 0.9700 . ? C206 C207 1.529(5) . ? C206 H20E 0.9700 . ? C206 H20F 0.9700 . ? C207 C208 1.516(5) . ? C207 H20G 0.9700 . ? C207 H20H 0.9700 . ? C208 C209 1.526(4) . ? C208 H20I 0.9700 . ? C208 H20J 0.9700 . ? C209 C210 1.516(5) . ? C209 H20K 0.9700 . ? C209 H20L 0.9700 . ? C210 C211 1.522(5) . ? C210 H21A 0.9700 . ? C210 H21B 0.9700 . ? C211 C212 1.526(5) . ? C211 H21C 0.9700 . ? C211 H21D 0.9700 . ? C212 C213 1.525(4) . ? C212 H21E 0.9700 . ? C212 H21F 0.9700 . ? C213 C214 1.523(5) . ? C213 H21G 0.9700 . ? C213 H21H 0.9700 . ? C214 C215 1.531(5) . ? C214 H21I 0.9700 . ? C214 H21J 0.9700 . ? C215 H21K 0.9600 . ? C215 H21L 0.9600 . ? C215 H21M 0.9600 . ? C301 N301 1.322(5) . ? C301 N302 1.348(4) . ? C301 H301 0.9300 . ? C302 C303 1.332(5) . ? C302 N301 1.362(4) . ? C302 H302 0.9300 . ? C303 N302 1.378(4) . ? C303 H303 0.9300 . ? C304 N302 1.454(5) . ? C304 C306 1.529(5) . ? C304 H30A 0.9700 . ? C304 H30B 0.9700 . ? C305 C306 1.522(5) . ? C305 C307 1.533(5) . ? C305 H30C 0.9700 . ? C305 H30D 0.9700 . ? C306 H30E 0.9700 . ? C306 H30F 0.9700 . ? C307 C308 1.519(5) . ? C307 H30G 0.9700 . ? C307 H30H 0.9700 . ? C308 C309 1.531(4) . ? C308 H30I 0.9700 . ? C308 H30J 0.9700 . ? C309 C310 1.525(5) . ? C309 H30K 0.9700 . ? C309 H30L 0.9700 . ? C310 C311 1.526(4) . ? C310 H31A 0.9700 . ? C310 H31B 0.9700 . ? C311 C312 1.526(5) . ? C311 H31C 0.9700 . ? C311 H31D 0.9700 . ? C312 C313 1.530(5) . ? C312 H31E 0.9700 . ? C312 H31F 0.9700 . ? C313 C314 1.524(5) . ? C313 H31G 0.9700 . ? C313 H31H 0.9700 . ? C314 C315 1.528(5) . ? C314 H31I 0.9700 . ? C314 H31J 0.9700 . ? C315 H31K 0.9600 . ? C315 H31L 0.9600 . ? C315 H31M 0.9600 . ? N101 Cu1 2.014(3) . ? N201 Cu2 2.004(3) . ? N301 Cu3 1.962(3) . ? Cu1 I1 2.6270(11) . ? Cu1 I1 2.6405(9) 2_666 ? Cu1 Cu1 2.6949(13) 2_666 ? Cu1 I2 2.7709(9) . ? Cu2 Cu3 2.5214(10) . ? Cu2 I1 2.6851(8) . ? Cu2 I3 2.6945(9) . ? Cu2 I2 2.7158(11) . ? Cu3 I3 2.5396(12) . ? Cu3 I2 2.5736(8) . ? I1 Cu1 2.6405(9) 2_666 ? 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 N101 C101 N102 111.5(3) . . ? N101 C101 H101 124.2 . . ? N102 C101 H101 124.2 . . ? C103 C102 N101 109.4(3) . . ? C103 C102 H102 125.3 . . ? N101 C102 H102 125.3 . . ? C102 C103 N102 106.7(3) . . ? C102 C103 H103 126.6 . . ? N102 C103 H103 126.6 . . ? N102 C104 C105 112.8(3) . . ? N102 C104 H10A 109.0 . . ? C105 C104 H10A 109.0 . . ? N102 C104 H10B 109.0 . . ? C105 C104 H10B 109.0 . . ? H10A C104 H10B 107.8 . . ? C106 C105 C104 110.5(3) . . ? C106 C105 H10C 109.5 . . ? C104 C105 H10C 109.5 . . ? C106 C105 H10D 109.5 . . ? C104 C105 H10D 109.5 . . ? H10C C105 H10D 108.1 . . ? C105 C106 C107 112.5(3) . . ? C105 C106 H10E 109.1 . . ? C107 C106 H10E 109.1 . . ? C105 C106 H10F 109.1 . . ? C107 C106 H10F 109.1 . . ? H10E C106 H10F 107.8 . . ? C108 C107 C106 112.8(3) . . ? C108 C107 H10G 109.0 . . ? C106 C107 H10G 109.0 . . ? C108 C107 H10H 109.0 . . ? C106 C107 H10H 109.0 . . ? H10G C107 H10H 107.8 . . ? C109 C108 C107 113.2(3) . . ? C109 C108 H10I 108.9 . . ? C107 C108 H10I 108.9 . . ? C109 C108 H10J 108.9 . . ? C107 C108 H10J 108.9 . . ? H10I C108 H10J 107.7 . . ? C110 C109 C108 113.3(3) . . ? C110 C109 H10K 108.9 . . ? C108 C109 H10K 108.9 . . ? C110 C109 H10L 108.9 . . ? C108 C109 H10L 108.9 . . ? H10K C109 H10L 107.7 . . ? C111 C110 C109 112.9(3) . . ? C111 C110 H11A 109.0 . . ? C109 C110 H11A 109.0 . . ? C111 C110 H11B 109.0 . . ? C109 C110 H11B 109.0 . . ? H11A C110 H11B 107.8 . . ? C110 C111 C112 113.4(3) . . ? C110 C111 H11C 108.9 . . ? C112 C111 H11C 108.9 . . ? C110 C111 H11D 108.9 . . ? C112 C111 H11D 108.9 . . ? H11C C111 H11D 107.7 . . ? C111 C112 C113 113.1(3) . . ? C111 C112 H11E 109.0 . . ? C113 C112 H11E 109.0 . . ? C111 C112 H11F 109.0 . . ? C113 C112 H11F 109.0 . . ? H11E C112 H11F 107.8 . . ? C114 C113 C112 113.4(3) . . ? C114 C113 H11G 108.9 . . ? C112 C113 H11G 108.9 . . ? C114 C113 H11H 108.9 . . ? C112 C113 H11H 108.9 . . ? H11G C113 H11H 107.7 . . ? C113 C114 C115 112.9(3) . . ? C113 C114 H11I 109.0 . . ? C115 C114 H11I 109.0 . . ? C113 C114 H11J 109.0 . . ? C115 C114 H11J 109.0 . . ? H11I C114 H11J 107.8 . . ? C114 C115 H11K 109.5 . . ? C114 C115 H11L 109.5 . . ? H11K C115 H11L 109.5 . . ? C114 C115 H11M 109.5 . . ? H11K C115 H11M 109.5 . . ? H11L C115 H11M 109.5 . . ? N201 C201 N202 111.9(3) . . ? N201 C201 H201 124.1 . . ? N202 C201 H201 124.1 . . ? C203 C202 N201 109.6(4) . . ? C203 C202 H202 125.2 . . ? N201 C202 H202 125.2 . . ? C202 C203 N202 107.0(3) . . ? C202 C203 H203 126.5 . . ? N202 C203 H203 126.5 . . ? N202 C204 C205 112.6(3) . . ? N202 C204 H20A 109.1 . . ? C205 C204 H20A 109.1 . . ? N202 C204 H20B 109.1 . . ? C205 C204 H20B 109.1 . . ? H20A C204 H20B 107.8 . . ? C204 C205 C206 112.3(3) . . ? C204 C205 H20C 109.1 . . ? C206 C205 H20C 109.1 . . ? C204 C205 H20D 109.1 . . ? C206 C205 H20D 109.1 . . ? H20C C205 H20D 107.9 . . ? C205 C206 C207 111.8(3) . . ? C205 C206 H20E 109.3 . . ? C207 C206 H20E 109.3 . . ? C205 C206 H20F 109.3 . . ? C207 C206 H20F 109.3 . . ? H20E C206 H20F 107.9 . . ? C208 C207 C206 113.9(3) . . ? C208 C207 H20G 108.8 . . ? C206 C207 H20G 108.8 . . ? C208 C207 H20H 108.8 . . ? C206 C207 H20H 108.8 . . ? H20G C207 H20H 107.7 . . ? C207 C208 C209 113.3(3) . . ? C207 C208 H20I 108.9 . . ? C209 C208 H20I 108.9 . . ? C207 C208 H20J 108.9 . . ? C209 C208 H20J 108.9 . . ? H20I C208 H20J 107.7 . . ? C210 C209 C208 114.0(3) . . ? C210 C209 H20K 108.8 . . ? C208 C209 H20K 108.8 . . ? C210 C209 H20L 108.8 . . ? C208 C209 H20L 108.8 . . ? H20K C209 H20L 107.6 . . ? C209 C210 C211 113.4(3) . . ? C209 C210 H21A 108.9 . . ? C211 C210 H21A 108.9 . . ? C209 C210 H21B 108.9 . . ? C211 C210 H21B 108.9 . . ? H21A C210 H21B 107.7 . . ? C210 C211 C212 113.3(3) . . ? C210 C211 H21C 108.9 . . ? C212 C211 H21C 108.9 . . ? C210 C211 H21D 108.9 . . ? C212 C211 H21D 108.9 . . ? H21C C211 H21D 107.7 . . ? C213 C212 C211 113.5(3) . . ? C213 C212 H21E 108.9 . . ? C211 C212 H21E 108.9 . . ? C213 C212 H21F 108.9 . . ? C211 C212 H21F 108.9 . . ? H21E C212 H21F 107.7 . . ? C214 C213 C212 113.2(3) . . ? C214 C213 H21G 108.9 . . ? C212 C213 H21G 108.9 . . ? C214 C213 H21H 108.9 . . ? C212 C213 H21H 108.9 . . ? H21G C213 H21H 107.7 . . ? C213 C214 C215 112.6(3) . . ? C213 C214 H21I 109.1 . . ? C215 C214 H21I 109.1 . . ? C213 C214 H21J 109.1 . . ? C215 C214 H21J 109.1 . . ? H21I C214 H21J 107.8 . . ? C214 C215 H21K 109.5 . . ? C214 C215 H21L 109.5 . . ? H21K C215 H21L 109.5 . . ? C214 C215 H21M 109.5 . . ? H21K C215 H21M 109.5 . . ? H21L C215 H21M 109.5 . . ? N301 C301 N302 111.3(3) . . ? N301 C301 H301 124.4 . . ? N302 C301 H301 124.4 . . ? C303 C302 N301 110.7(3) . . ? C303 C302 H302 124.6 . . ? N301 C302 H302 124.7 . . ? C302 C303 N302 106.4(3) . . ? C302 C303 H303 126.8 . . ? N302 C303 H303 126.8 . . ? N302 C304 C306 111.7(3) . . ? N302 C304 H30A 109.3 . . ? C306 C304 H30A 109.3 . . ? N302 C304 H30B 109.3 . . ? C306 C304 H30B 109.3 . . ? H30A C304 H30B 107.9 . . ? C306 C305 C307 112.5(3) . . ? C306 C305 H30C 109.1 . . ? C307 C305 H30C 109.1 . . ? C306 C305 H30D 109.1 . . ? C307 C305 H30D 109.1 . . ? H30C C305 H30D 107.8 . . ? C305 C306 C304 112.3(3) . . ? C305 C306 H30E 109.1 . . ? C304 C306 H30E 109.1 . . ? C305 C306 H30F 109.1 . . ? C304 C306 H30F 109.1 . . ? H30E C306 H30F 107.9 . . ? C308 C307 C305 113.7(3) . . ? C308 C307 H30G 108.8 . . ? C305 C307 H30G 108.8 . . ? C308 C307 H30H 108.8 . . ? C305 C307 H30H 108.8 . . ? H30G C307 H30H 107.7 . . ? C307 C308 C309 113.2(3) . . ? C307 C308 H30I 108.9 . . ? C309 C308 H30I 108.9 . . ? C307 C308 H30J 108.9 . . ? C309 C308 H30J 108.9 . . ? H30I C308 H30J 107.7 . . ? C310 C309 C308 113.2(3) . . ? C310 C309 H30K 108.9 . . ? C308 C309 H30K 108.9 . . ? C310 C309 H30L 108.9 . . ? C308 C309 H30L 108.9 . . ? H30K C309 H30L 107.7 . . ? C309 C310 C311 113.0(3) . . ? C309 C310 H31A 109.0 . . ? C311 C310 H31A 109.0 . . ? C309 C310 H31B 109.0 . . ? C311 C310 H31B 109.0 . . ? H31A C310 H31B 107.8 . . ? C310 C311 C312 113.7(3) . . ? C310 C311 H31C 108.8 . . ? C312 C311 H31C 108.8 . . ? C310 C311 H31D 108.8 . . ? C312 C311 H31D 108.8 . . ? H31C C311 H31D 107.7 . . ? C311 C312 C313 113.1(3) . . ? C311 C312 H31E 109.0 . . ? C313 C312 H31E 109.0 . . ? C311 C312 H31F 109.0 . . ? C313 C312 H31F 109.0 . . ? H31E C312 H31F 107.8 . . ? C314 C313 C312 113.8(3) . . ? C314 C313 H31G 108.8 . . ? C312 C313 H31G 108.8 . . ? C314 C313 H31H 108.8 . . ? C312 C313 H31H 108.8 . . ? H31G C313 H31H 107.7 . . ? C313 C314 C315 112.4(3) . . ? C313 C314 H31I 109.1 . . ? C315 C314 H31I 109.1 . . ? C313 C314 H31J 109.1 . . ? C315 C314 H31J 109.1 . . ? H31I C314 H31J 107.9 . . ? C314 C315 H31K 109.5 . . ? C314 C315 H31L 109.5 . . ? H31K C315 H31L 109.5 . . ? C314 C315 H31M 109.5 . . ? H31K C315 H31M 109.5 . . ? H31L C315 H31M 109.5 . . ? C101 N101 C102 105.6(3) . . ? C101 N101 Cu1 127.1(2) . . ? C102 N101 Cu1 126.0(2) . . ? C103 N102 C101 106.7(3) . . ? C103 N102 C104 126.6(3) . . ? C101 N102 C104 126.6(3) . . ? C201 N201 C202 105.5(3) . . ? C201 N201 Cu2 126.8(2) . . ? C202 N201 Cu2 127.6(3) . . ? C201 N202 C203 106.0(3) . . ? C201 N202 C204 125.2(3) . . ? C203 N202 C204 128.6(3) . . ? C301 N301 C302 105.3(3) . . ? C301 N301 Cu3 127.1(2) . . ? C302 N301 Cu3 127.6(2) . . ? C301 N302 C303 106.3(3) . . ? C301 N302 C304 126.8(3) . . ? C303 N302 C304 126.9(3) . . ? N101 Cu1 I1 110.00(9) . . ? N101 Cu1 I1 110.80(9) . 2_666 ? I1 Cu1 I1 118.46(2) . 2_666 ? N101 Cu1 Cu1 132.95(10) . 2_666 ? I1 Cu1 Cu1 59.48(2) . 2_666 ? I1 Cu1 Cu1 58.98(3) 2_666 2_666 ? N101 Cu1 I2 100.61(9) . . ? I1 Cu1 I2 108.95(2) . . ? I1 Cu1 I2 106.44(3) 2_666 . ? Cu1 Cu1 I2 126.43(3) 2_666 . ? N201 Cu2 Cu3 134.20(9) . . ? N201 Cu2 I1 113.62(9) . . ? Cu3 Cu2 I1 112.18(3) . . ? N201 Cu2 I3 106.51(9) . . ? Cu3 Cu2 I3 58.16(3) . . ? I1 Cu2 I3 107.26(3) . . ? N201 Cu2 I2 105.72(9) . . ? Cu3 Cu2 I2 58.73(2) . . ? I1 Cu2 I2 108.89(2) . . ? I3 Cu2 I2 115.00(2) . . ? N301 Cu3 Cu2 161.50(10) . . ? N301 Cu3 I3 118.15(9) . . ? Cu2 Cu3 I3 64.34(3) . . ? N301 Cu3 I2 115.46(9) . . ? Cu2 Cu3 I2 64.41(3) . . ? I3 Cu3 I2 126.352(19) . . ? Cu1 I1 Cu1 61.54(2) . 2_666 ? Cu1 I1 Cu2 72.36(2) . . ? Cu1 I1 Cu2 105.59(3) 2_666 . ? Cu3 I2 Cu2 56.862(19) . . ? Cu3 I2 Cu1 92.45(3) . . ? Cu2 I2 Cu1 69.72(2) . . ? Cu3 I3 Cu2 57.504(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N101 C102 C103 N102 0.2(4) . . . . ? N102 C104 C105 C106 174.6(3) . . . . ? C104 C105 C106 C107 178.3(3) . . . . ? C105 C106 C107 C108 179.0(3) . . . . ? C106 C107 C108 C109 179.5(3) . . . . ? C107 C108 C109 C110 178.8(3) . . . . ? C108 C109 C110 C111 -179.6(3) . . . . ? C109 C110 C111 C112 179.7(3) . . . . ? C110 C111 C112 C113 -179.1(3) . . . . ? C111 C112 C113 C114 178.7(3) . . . . ? C112 C113 C114 C115 -179.9(3) . . . . ? N201 C202 C203 N202 0.0(4) . . . . ? N202 C204 C205 C206 175.9(3) . . . . ? C204 C205 C206 C207 177.7(3) . . . . ? C205 C206 C207 C208 177.6(3) . . . . ? C206 C207 C208 C209 179.7(3) . . . . ? C207 C208 C209 C210 179.8(3) . . . . ? C208 C209 C210 C211 179.4(3) . . . . ? C209 C210 C211 C212 -179.7(3) . . . . ? C210 C211 C212 C213 179.2(3) . . . . ? C211 C212 C213 C214 -178.6(3) . . . . ? C212 C213 C214 C215 179.1(3) . . . . ? N301 C302 C303 N302 0.1(4) . . . . ? C307 C305 C306 C304 179.2(3) . . . . ? N302 C304 C306 C305 176.0(3) . . . . ? C306 C305 C307 C308 177.7(3) . . . . ? C305 C307 C308 C309 -179.5(3) . . . . ? C307 C308 C309 C310 179.0(3) . . . . ? C308 C309 C310 C311 -179.9(3) . . . . ? C309 C310 C311 C312 -180.0(3) . . . . ? C310 C311 C312 C313 -179.9(3) . . . . ? C311 C312 C313 C314 180.0(3) . . . . ? C312 C313 C314 C315 -179.0(3) . . . . ? N102 C101 N101 C102 0.0(4) . . . . ? N102 C101 N101 Cu1 -167.5(2) . . . . ? C103 C102 N101 C101 -0.1(4) . . . . ? C103 C102 N101 Cu1 167.5(3) . . . . ? C102 C103 N102 C101 -0.1(4) . . . . ? C102 C103 N102 C104 -176.6(3) . . . . ? N101 C101 N102 C103 0.1(4) . . . . ? N101 C101 N102 C104 176.6(3) . . . . ? C105 C104 N102 C103 -66.9(5) . . . . ? C105 C104 N102 C101 117.3(4) . . . . ? N202 C201 N201 C202 0.3(4) . . . . ? N202 C201 N201 Cu2 177.0(2) . . . . ? C203 C202 N201 C201 -0.2(4) . . . . ? C203 C202 N201 Cu2 -176.8(2) . . . . ? N201 C201 N202 C203 -0.3(4) . . . . ? N201 C201 N202 C204 -175.1(3) . . . . ? C202 C203 N202 C201 0.2(4) . . . . ? C202 C203 N202 C204 174.7(3) . . . . ? C205 C204 N202 C201 -147.9(3) . . . . ? C205 C204 N202 C203 38.6(5) . . . . ? N302 C301 N301 C302 0.0(4) . . . . ? N302 C301 N301 Cu3 178.9(2) . . . . ? C303 C302 N301 C301 -0.1(4) . . . . ? C303 C302 N301 Cu3 -179.0(3) . . . . ? N301 C301 N302 C303 0.1(4) . . . . ? N301 C301 N302 C304 -178.4(3) . . . . ? C302 C303 N302 C301 -0.1(4) . . . . ? C302 C303 N302 C304 178.4(3) . . . . ? C306 C304 N302 C301 111.6(4) . . . . ? C306 C304 N302 C303 -66.6(5) . . . . ? C101 N101 Cu1 I1 -34.4(3) . . . . ? C102 N101 Cu1 I1 160.5(3) . . . . ? C101 N101 Cu1 I1 -167.3(3) . . . 2_666 ? C102 N101 Cu1 I1 27.6(3) . . . 2_666 ? C101 N101 Cu1 Cu1 -100.9(3) . . . 2_666 ? C102 N101 Cu1 Cu1 94.1(3) . . . 2_666 ? C101 N101 Cu1 I2 80.4(3) . . . . ? C102 N101 Cu1 I2 -84.6(3) . . . . ? C201 N201 Cu2 Cu3 134.2(3) . . . . ? C202 N201 Cu2 Cu3 -49.9(3) . . . . ? C201 N201 Cu2 I1 -46.5(3) . . . . ? C202 N201 Cu2 I1 129.4(3) . . . . ? C201 N201 Cu2 I3 -164.4(3) . . . . ? C202 N201 Cu2 I3 11.5(3) . . . . ? C201 N201 Cu2 I2 72.8(3) . . . . ? C202 N201 Cu2 I2 -111.3(3) . . . . ? C301 N301 Cu3 Cu2 -100.5(4) . . . . ? C302 N301 Cu3 Cu2 78.2(4) . . . . ? C301 N301 Cu3 I3 -7.5(4) . . . . ? C302 N301 Cu3 I3 171.2(3) . . . . ? C301 N301 Cu3 I2 174.4(3) . . . . ? C302 N301 Cu3 I2 -6.9(3) . . . . ? N201 Cu2 Cu3 N301 -175.5(3) . . . . ? I1 Cu2 Cu3 N301 5.2(3) . . . . ? I3 Cu2 Cu3 N301 102.3(3) . . . . ? I2 Cu2 Cu3 N301 -94.1(3) . . . . ? N201 Cu2 Cu3 I3 82.12(12) . . . . ? I1 Cu2 Cu3 I3 -97.12(3) . . . . ? I2 Cu2 Cu3 I3 163.588(19) . . . . ? N201 Cu2 Cu3 I2 -81.47(12) . . . . ? I1 Cu2 Cu3 I2 99.29(3) . . . . ? I3 Cu2 Cu3 I2 -163.588(19) . . . . ? N101 Cu1 I1 Cu1 -128.84(10) . . . 2_666 ? I1 Cu1 I1 Cu1 0.0 2_666 . . 2_666 ? I2 Cu1 I1 Cu1 121.76(3) . . . 2_666 ? N101 Cu1 I1 Cu2 111.62(10) . . . . ? I1 Cu1 I1 Cu2 -119.54(3) 2_666 . . . ? Cu1 Cu1 I1 Cu2 -119.54(3) 2_666 . . . ? I2 Cu1 I1 Cu2 2.221(15) . . . . ? N201 Cu2 I1 Cu1 115.27(10) . . . . ? Cu3 Cu2 I1 Cu1 -65.33(4) . . . . ? I3 Cu2 I1 Cu1 -127.300(19) . . . . ? I2 Cu2 I1 Cu1 -2.265(16) . . . . ? N201 Cu2 I1 Cu1 62.70(9) . . . 2_666 ? Cu3 Cu2 I1 Cu1 -117.89(3) . . . 2_666 ? I3 Cu2 I1 Cu1 -179.866(13) . . . 2_666 ? I2 Cu2 I1 Cu1 -54.83(2) . . . 2_666 ? N301 Cu3 I2 Cu2 159.48(11) . . . . ? I3 Cu3 I2 Cu2 -18.43(2) . . . . ? N301 Cu3 I2 Cu1 95.72(10) . . . . ? Cu2 Cu3 I2 Cu1 -63.75(2) . . . . ? I3 Cu3 I2 Cu1 -82.19(3) . . . . ? N201 Cu2 I2 Cu3 132.56(10) . . . . ? I1 Cu2 I2 Cu3 -105.01(3) . . . . ? I3 Cu2 I2 Cu3 15.358(18) . . . . ? N201 Cu2 I2 Cu1 -120.25(10) . . . . ? Cu3 Cu2 I2 Cu1 107.19(3) . . . . ? I1 Cu2 I2 Cu1 2.182(15) . . . . ? I3 Cu2 I2 Cu1 122.55(3) . . . . ? N101 Cu1 I2 Cu3 -64.64(9) . . . . ? I1 Cu1 I2 Cu3 50.963(19) . . . . ? I1 Cu1 I2 Cu3 179.764(14) 2_666 . . . ? Cu1 Cu1 I2 Cu3 116.51(4) 2_666 . . . ? N101 Cu1 I2 Cu2 -117.84(9) . . . . ? I1 Cu1 I2 Cu2 -2.231(15) . . . . ? I1 Cu1 I2 Cu2 126.570(19) 2_666 . . . ? Cu1 Cu1 I2 Cu2 63.31(4) 2_666 . . . ? N301 Cu3 I3 Cu2 -159.42(11) . . . . ? I2 Cu3 I3 Cu2 18.45(2) . . . . ? N201 Cu2 I3 Cu3 -132.21(9) . . . . ? I1 Cu2 I3 Cu3 105.81(2) . . . . ? I2 Cu2 I3 Cu3 -15.454(18) . . . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 1.364 _refine_diff_density_min -1.517 _refine_diff_density_rms 0.128 #===END data_msc03b _database_code_depnum_ccdc_archive 'CCDC 769705' #TrackingRef 'MarionStricker.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C16 H31 N2), Br8 Cu4' _chemical_formula_sum 'C64 H124 Br8 Cu4 N8' _chemical_formula_weight 1899.15 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' Br Br -0.2901 2.4595 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3068(13) _cell_length_b 16.172(2) _cell_length_c 25.595(4) _cell_angle_alpha 73.875(17) _cell_angle_beta 87.515(17) _cell_angle_gamma 87.742(17) _cell_volume 4093.0(10) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 6115 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 21.65 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 4.969 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4021 _exptl_absorpt_correction_T_max 0.5082 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS I' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40859 _diffrn_reflns_av_R_equivalents 0.2262 _diffrn_reflns_av_sigmaI/netI 0.4514 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 26.06 _reflns_number_total 14954 _reflns_number_gt 3090 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _publ_section_exptl_refinement ; The ratio of observed to unique reflections is low (21%) due to a weakly diffracting crystal. ; _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^)+(0.0366P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14954 _refine_ls_number_parameters 765 _refine_ls_number_restraints 87 _refine_ls_R_factor_all 0.2416 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1803 _refine_ls_wR_factor_gt 0.1339 _refine_ls_goodness_of_fit_ref 0.604 _refine_ls_restrained_S_all 0.603 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.002 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 C101 C 0.753(2) 0.7695(10) 0.6170(9) 0.066(6) Uani 1 1 d . . . H101 H 0.7638 0.8175 0.6307 0.079 Uiso 1 1 calc R . . C102 C 0.681(2) 0.6501(13) 0.6072(9) 0.082(7) Uani 1 1 d . . . H102 H 0.6338 0.5994 0.6115 0.098 Uiso 1 1 calc R . . C103 C 0.775(2) 0.6787(10) 0.5739(10) 0.078(7) Uani 1 1 d . . . H103 H 0.8075 0.6488 0.5488 0.094 Uiso 1 1 calc R . . C104 C 0.9277(18) 0.8118(11) 0.5432(9) 0.072(6) Uani 1 1 d . . . H10A H 0.9744 0.7826 0.5190 0.108 Uiso 1 1 calc R . . H10B H 0.9889 0.8251 0.5678 0.108 Uiso 1 1 calc R . . H10C H 0.8868 0.8654 0.5215 0.108 Uiso 1 1 calc R . . C105 C 0.570(2) 0.7086(10) 0.6812(8) 0.079(7) Uani 1 1 d . . . H10D H 0.4850 0.6925 0.6711 0.095 Uiso 1 1 calc R . . H10E H 0.5596 0.7661 0.6877 0.095 Uiso 1 1 calc R . . C106 C 0.6137(16) 0.6436(10) 0.7325(7) 0.054(5) Uani 1 1 d . . . H10F H 0.6938 0.6637 0.7445 0.065 Uiso 1 1 calc R . . H10G H 0.6352 0.5882 0.7243 0.065 Uiso 1 1 calc R . . C107 C 0.512(2) 0.6288(11) 0.7785(8) 0.083(7) Uani 1 1 d . . . H10H H 0.4266 0.6220 0.7640 0.099 Uiso 1 1 calc R . . H10I H 0.5049 0.6805 0.7922 0.099 Uiso 1 1 calc R . . C108 C 0.541(2) 0.5500(12) 0.8262(9) 0.079(6) Uani 1 1 d . . . H10J H 0.5484 0.4988 0.8121 0.095 Uiso 1 1 calc R . . H10K H 0.6260 0.5573 0.8403 0.095 Uiso 1 1 calc R . . C109 C 0.444(2) 0.5322(13) 0.8721(8) 0.086(7) Uani 1 1 d . . . H10L H 0.3595 0.5201 0.8595 0.103 Uiso 1 1 calc R . . H10M H 0.4326 0.5834 0.8861 0.103 Uiso 1 1 calc R . . C110 C 0.4921(19) 0.4516(11) 0.9196(9) 0.073(6) Uani 1 1 d . . . H11A H 0.5107 0.4021 0.9045 0.088 Uiso 1 1 calc R . . H11B H 0.5742 0.4657 0.9335 0.088 Uiso 1 1 calc R . . C111 C 0.3929(18) 0.4251(11) 0.9671(8) 0.062(5) Uani 1 1 d . . . H11C H 0.3752 0.4740 0.9828 0.075 Uiso 1 1 calc R . . H11D H 0.3104 0.4113 0.9534 0.075 Uiso 1 1 calc R . . C112 C 0.4400(19) 0.3492(11) 1.0101(8) 0.069(6) Uani 1 1 d . . . H11E H 0.5268 0.3615 1.0208 0.082 Uiso 1 1 calc R . . H11F H 0.4505 0.2995 0.9947 0.082 Uiso 1 1 calc R . . C113 C 0.3521(18) 0.3240(11) 1.0607(7) 0.062(5) Uani 1 1 d . . . H11G H 0.2646 0.3131 1.0500 0.075 Uiso 1 1 calc R . . H11H H 0.3436 0.3730 1.0769 0.075 Uiso 1 1 calc R . . C114 C 0.4019(19) 0.2420(10) 1.1051(8) 0.066(5) Uani 1 1 d . . . H11I H 0.4105 0.1930 1.0890 0.079 Uiso 1 1 calc R . . H11J H 0.4894 0.2529 1.1159 0.079 Uiso 1 1 calc R . . C115 C 0.317(2) 0.2182(13) 1.1536(8) 0.084(6) Uani 1 1 d . . . H11K H 0.2318 0.2009 1.1441 0.100 Uiso 1 1 calc R . . H11L H 0.3018 0.2681 1.1686 0.100 Uiso 1 1 calc R . . C116 C 0.380(3) 0.1430(13) 1.1963(9) 0.109(9) Uani 1 1 d . . . H11M H 0.3578 0.1484 1.2328 0.163 Uiso 1 1 calc R . . H11N H 0.4750 0.1443 1.1904 0.163 Uiso 1 1 calc R . . H11O H 0.3490 0.0884 1.1928 0.163 Uiso 1 1 calc R . . C201 C -0.036(2) -0.0981(12) 1.3699(10) 0.097(8) Uani 1 1 d . . . H201 H 0.0315 -0.0584 1.3583 0.117 Uiso 1 1 calc R . . C202 C -0.160(2) -0.2191(12) 1.3870(9) 0.081(7) Uani 1 1 d . . . H202 H -0.1903 -0.2740 1.3872 0.097 Uiso 1 1 calc R . . C203 C -0.222(2) -0.1630(10) 1.4118(8) 0.066(6) Uani 1 1 d . . . H203 H -0.3002 -0.1713 1.4336 0.079 Uiso 1 1 calc R . . C204 C -0.1746(19) -0.0048(9) 1.4091(8) 0.065(5) Uani 1 1 d . . . H20A H -0.2626 0.0151 1.3977 0.098 Uiso 1 1 calc R . . H20B H -0.1119 0.0374 1.3889 0.098 Uiso 1 1 calc R . . H20C H -0.1685 -0.0114 1.4482 0.098 Uiso 1 1 calc R . . C205 C 0.044(2) -0.2235(11) 1.3277(9) 0.076(5) Uani 1 1 d U . . H20D H 0.1338 -0.2087 1.3327 0.092 Uiso 1 1 calc R . . H20E H 0.0378 -0.2869 1.3411 0.092 Uiso 1 1 calc R . . C206 C 0.018(3) -0.1964(14) 1.2691(11) 0.115(7) Uani 1 1 d U . . H20F H -0.0774 -0.1939 1.2648 0.138 Uiso 1 1 calc R . . H20G H 0.0549 -0.2408 1.2524 0.138 Uiso 1 1 calc R . . C207 C 0.072(3) -0.1100(13) 1.2383(11) 0.114(8) Uani 1 1 d U . . H20H H 0.0285 -0.0659 1.2536 0.137 Uiso 1 1 calc R . . H20I H 0.1652 -0.1115 1.2466 0.137 Uiso 1 1 calc R . . C208 C 0.063(3) -0.0806(17) 1.1811(13) 0.147(9) Uani 1 1 d U . . H20J H 0.1002 -0.1301 1.1691 0.177 Uiso 1 1 calc R . . H20K H -0.0312 -0.0810 1.1759 0.177 Uiso 1 1 calc R . . C209 C 0.100(3) -0.0160(16) 1.1424(13) 0.126(8) Uani 1 1 d U . . H20L H 0.1931 -0.0169 1.1498 0.151 Uiso 1 1 calc R . . H20M H 0.0617 0.0315 1.1562 0.151 Uiso 1 1 calc R . . C210 C 0.103(3) 0.0227(17) 1.0893(14) 0.153(10) Uani 1 1 d U . . H21A H 0.0089 0.0264 1.0826 0.184 Uiso 1 1 calc R . . H21B H 0.1355 -0.0262 1.0757 0.184 Uiso 1 1 calc R . . C211 C 0.143(3) 0.0881(16) 1.0475(13) 0.140(9) Uani 1 1 d U . . H21C H 0.2382 0.0836 1.0510 0.169 Uiso 1 1 calc R . . H21D H 0.1154 0.1387 1.0604 0.169 Uiso 1 1 calc R . . C212 C 0.131(3) 0.1212(16) 0.9902(13) 0.137(9) Uani 1 1 d U . . H21E H 0.1551 0.0723 0.9752 0.164 Uiso 1 1 calc R . . H21F H 0.0366 0.1321 0.9846 0.164 Uiso 1 1 calc R . . C213 C 0.186(3) 0.1872(18) 0.9574(15) 0.173(12) Uani 1 1 d U . . H21G H 0.2801 0.1779 0.9647 0.207 Uiso 1 1 calc R . . H21H H 0.1578 0.2366 0.9713 0.207 Uiso 1 1 calc R . . C214 C 0.181(4) 0.2169(19) 0.9031(15) 0.178(12) Uani 1 1 d U . . H21I H 0.0866 0.2269 0.8968 0.214 Uiso 1 1 calc R . . H21J H 0.2055 0.1660 0.8902 0.214 Uiso 1 1 calc R . . C215 C 0.239(4) 0.286(2) 0.8636(15) 0.203(14) Uani 1 1 d U . . H21K H 0.3331 0.2768 0.8699 0.243 Uiso 1 1 calc R . . H21L H 0.2135 0.3375 0.8762 0.243 Uiso 1 1 calc R . . C216 C 0.232(4) 0.3174(17) 0.8035(13) 0.181(14) Uani 1 1 d U . . H21M H 0.2562 0.3778 0.7910 0.272 Uiso 1 1 calc R . . H21N H 0.1425 0.3123 0.7929 0.272 Uiso 1 1 calc R . . H21O H 0.2910 0.2825 0.7867 0.272 Uiso 1 1 calc R . . C301 C 0.4743(19) 0.6916(11) 0.3424(9) 0.069(6) Uani 1 1 d . . . H301 H 0.5215 0.6581 0.3224 0.083 Uiso 1 1 calc R . . C302 C 0.4143(18) 0.7971(9) 0.3724(8) 0.053(5) Uani 1 1 d . . . H302 H 0.4108 0.8529 0.3779 0.064 Uiso 1 1 calc R . . C303 C 0.340(2) 0.7331(12) 0.3994(8) 0.071(6) Uani 1 1 d . . . H303 H 0.2738 0.7352 0.4262 0.085 Uiso 1 1 calc R . . C304 C 0.3423(17) 0.5729(9) 0.4021(8) 0.062(5) Uani 1 1 d . . . H30A H 0.2475 0.5703 0.4067 0.093 Uiso 1 1 calc R . . H30B H 0.3817 0.5495 0.4375 0.093 Uiso 1 1 calc R . . H30C H 0.3729 0.5389 0.3775 0.093 Uiso 1 1 calc R . . C305 C 0.5786(17) 0.8270(9) 0.2969(7) 0.050(5) Uani 1 1 d . . . H30D H 0.6603 0.7946 0.2929 0.060 Uiso 1 1 calc R . . H30E H 0.6008 0.8766 0.3100 0.060 Uiso 1 1 calc R . . C306 C 0.5194(17) 0.8599(10) 0.2422(8) 0.058(5) Uani 1 1 d . . . H30F H 0.4351 0.8896 0.2461 0.070 Uiso 1 1 calc R . . H30G H 0.5028 0.8109 0.2275 0.070 Uiso 1 1 calc R . . C307 C 0.6094(19) 0.9224(10) 0.2026(8) 0.072(6) Uani 1 1 d . . . H30H H 0.6961 0.8942 0.2014 0.086 Uiso 1 1 calc R . . H30I H 0.6198 0.9736 0.2159 0.086 Uiso 1 1 calc R . . C308 C 0.555(2) 0.9518(11) 0.1436(7) 0.065(5) Uani 1 1 d . . . H30J H 0.4659 0.9766 0.1447 0.078 Uiso 1 1 calc R . . H30K H 0.5517 0.9017 0.1286 0.078 Uiso 1 1 calc R . . C309 C 0.649(2) 1.0227(11) 0.1059(10) 0.100(8) Uani 1 1 d . . . H30L H 0.6510 1.0727 0.1210 0.120 Uiso 1 1 calc R . . H30M H 0.7387 0.9979 0.1062 0.120 Uiso 1 1 calc R . . C310 C 0.606(2) 1.0518(11) 0.0496(9) 0.072(6) Uani 1 1 d . . . H31A H 0.5158 1.0742 0.0502 0.086 Uiso 1 1 calc R . . H31B H 0.6057 1.0010 0.0351 0.086 Uiso 1 1 calc R . . C311 C 0.6895(19) 1.1227(10) 0.0091(9) 0.072(7) Uani 1 1 d . . . H31C H 0.6920 1.1734 0.0235 0.087 Uiso 1 1 calc R . . H31D H 0.7797 1.1001 0.0072 0.087 Uiso 1 1 calc R . . C312 C 0.638(2) 1.1513(10) -0.0478(8) 0.077(6) Uani 1 1 d . . . H31E H 0.5477 1.1741 -0.0471 0.092 Uiso 1 1 calc R . . H31F H 0.6396 1.1024 -0.0641 0.092 Uiso 1 1 calc R . . C313 C 0.7307(18) 1.2241(10) -0.0817(8) 0.063(5) Uani 1 1 d . . . H31G H 0.8212 1.2011 -0.0812 0.075 Uiso 1 1 calc R . . H31H H 0.7282 1.2727 -0.0651 0.075 Uiso 1 1 calc R . . C314 C 0.6844(19) 1.2581(12) -0.1441(8) 0.069(6) Uani 1 1 d . . . H31I H 0.6851 1.2088 -0.1600 0.083 Uiso 1 1 calc R . . H31J H 0.5939 1.2811 -0.1442 0.083 Uiso 1 1 calc R . . C315 C 0.769(2) 1.3268(12) -0.1792(10) 0.096(8) Uani 1 1 d . . . H31K H 0.7724 1.3743 -0.1619 0.115 Uiso 1 1 calc R . . H31L H 0.8585 1.3025 -0.1805 0.115 Uiso 1 1 calc R . . C316 C 0.726(3) 1.3631(14) -0.2360(10) 0.106(9) Uani 1 1 d . . . H31M H 0.7751 1.4144 -0.2539 0.159 Uiso 1 1 calc R . . H31N H 0.6329 1.3787 -0.2353 0.159 Uiso 1 1 calc R . . H31O H 0.7403 1.3199 -0.2561 0.159 Uiso 1 1 calc R . . C401 C 0.170(2) 0.6712(10) 0.6191(9) 0.076(7) Uani 1 1 d . . . H401 H 0.1457 0.6183 0.6137 0.092 Uiso 1 1 calc R . . C402 C 0.195(2) 0.7735(11) 0.6546(10) 0.078(7) Uani 1 1 d . . . H402 H 0.1903 0.8078 0.6793 0.094 Uiso 1 1 calc R . . C403 C 0.278(2) 0.7834(10) 0.6131(9) 0.058(5) Uani 1 1 d . . . H403 H 0.3382 0.8280 0.6008 0.070 Uiso 1 1 calc R . . C404 C 0.338(2) 0.6943(11) 0.5454(9) 0.075(6) Uani 1 1 d . . . H40A H 0.4306 0.7026 0.5491 0.113 Uiso 1 1 calc R . . H40B H 0.3096 0.7311 0.5103 0.113 Uiso 1 1 calc R . . H40C H 0.3245 0.6338 0.5474 0.113 Uiso 1 1 calc R . . C405 C 0.014(2) 0.6682(9) 0.6985(9) 0.075(6) Uani 1 1 d . . . H40D H -0.0436 0.6330 0.6838 0.090 Uiso 1 1 calc R . . H40E H -0.0396 0.7148 0.7075 0.090 Uiso 1 1 calc R . . C406 C 0.0761(18) 0.6121(10) 0.7496(9) 0.068(6) Uani 1 1 d . . . H40F H 0.1234 0.5624 0.7415 0.081 Uiso 1 1 calc R . . H40G H 0.1389 0.6458 0.7628 0.081 Uiso 1 1 calc R . . C407 C -0.0298(19) 0.5804(10) 0.7930(8) 0.065(6) Uani 1 1 d . . . H40H H -0.0967 0.5515 0.7784 0.078 Uiso 1 1 calc R . . H40I H -0.0720 0.6301 0.8031 0.078 Uiso 1 1 calc R . . C408 C 0.0286(19) 0.5157(12) 0.8449(8) 0.069(5) Uani 1 1 d . . . H40J H 0.0575 0.4619 0.8360 0.083 Uiso 1 1 calc R . . H40K H 0.1056 0.5411 0.8556 0.083 Uiso 1 1 calc R . . C409 C -0.069(2) 0.4949(11) 0.8919(9) 0.083(7) Uani 1 1 d . . . H40L H -0.1514 0.4791 0.8793 0.100 Uiso 1 1 calc R . . H40M H -0.0865 0.5469 0.9046 0.100 Uiso 1 1 calc R . . C410 C -0.021(2) 0.4197(12) 0.9404(8) 0.076(6) Uani 1 1 d . . . H41A H -0.0066 0.3670 0.9282 0.091 Uiso 1 1 calc R . . H41B H 0.0633 0.4345 0.9522 0.091 Uiso 1 1 calc R . . C411 C -0.120(2) 0.4018(12) 0.9891(9) 0.081(6) Uani 1 1 d . . . H41C H -0.1308 0.4535 1.0026 0.097 Uiso 1 1 calc R . . H41D H -0.2059 0.3904 0.9767 0.097 Uiso 1 1 calc R . . C412 C -0.078(2) 0.3266(13) 1.0344(9) 0.081(6) Uani 1 1 d . . . H41E H 0.0076 0.3389 1.0461 0.098 Uiso 1 1 calc R . . H41F H -0.0660 0.2759 1.0199 0.098 Uiso 1 1 calc R . . C413 C -0.174(2) 0.3015(11) 1.0867(9) 0.073(6) Uani 1 1 d . . . H41G H -0.1831 0.3514 1.1021 0.088 Uiso 1 1 calc R . . H41H H -0.2609 0.2919 1.0747 0.088 Uiso 1 1 calc R . . C414 C -0.135(2) 0.2237(14) 1.1313(9) 0.086(7) Uani 1 1 d . . . H41I H -0.1239 0.1740 1.1159 0.103 Uiso 1 1 calc R . . H41J H -0.0500 0.2339 1.1444 0.103 Uiso 1 1 calc R . . C415 C -0.227(3) 0.2011(15) 1.1778(9) 0.102(8) Uani 1 1 d . . . H41K H -0.3136 0.1938 1.1646 0.122 Uiso 1 1 calc R . . H41L H -0.2347 0.2494 1.1946 0.122 Uiso 1 1 calc R . . C416 C -0.186(2) 0.1136(13) 1.2240(8) 0.094(7) Uani 1 1 d . . . H41M H -0.2510 0.1029 1.2542 0.141 Uiso 1 1 calc R . . H41N H -0.1010 0.1203 1.2376 0.141 Uiso 1 1 calc R . . H41O H -0.1824 0.0649 1.2082 0.141 Uiso 1 1 calc R . . N101 N 0.6661(15) 0.7124(7) 0.6362(7) 0.060(4) Uani 1 1 d . . . N102 N 0.8254(15) 0.7545(8) 0.5758(6) 0.055(4) Uani 1 1 d . . . N201 N -0.0481(17) -0.1830(8) 1.3617(7) 0.071(5) Uani 1 1 d . . . N202 N -0.1447(15) -0.0906(7) 1.3977(6) 0.056(4) Uani 1 1 d . . . N301 N 0.4960(15) 0.7729(7) 0.3362(7) 0.065(5) Uani 1 1 d . . . N302 N 0.3779(16) 0.6590(8) 0.3800(7) 0.065(5) Uani 1 1 d . . . N401 N 0.1156(16) 0.7059(8) 0.6569(8) 0.076(5) Uani 1 1 d . . . N402 N 0.2600(14) 0.7180(8) 0.5913(7) 0.055(4) Uani 1 1 d . . . Cu1 Cu 0.4219(2) -0.01214(12) 1.45352(10) 0.0676(7) Uani 1 1 d . . . Cu2 Cu 0.2662(2) 0.01871(12) 1.36890(10) 0.0637(7) Uani 1 1 d . . . Cu3 Cu 0.2528(2) 0.46203(12) 0.62561(11) 0.0707(7) Uani 1 1 d . . . Cu4 Cu 0.0854(2) 0.47398(12) 0.54538(11) 0.0670(7) Uani 1 1 d . . . Br1 Br 0.56196(19) -0.11878(9) 1.51564(8) 0.0580(5) Uani 1 1 d . . . Br2 Br 0.2005(2) -0.07695(11) 1.45510(9) 0.0652(6) Uani 1 1 d . . . Br3 Br 0.4963(2) 0.03117(10) 1.35149(8) 0.0635(6) Uani 1 1 d . . . Br4 Br 0.1099(2) 0.09699(10) 1.30948(9) 0.0648(6) Uani 1 1 d . . . Br5 Br 0.3917(2) 0.50896(10) 0.68124(9) 0.0664(6) Uani 1 1 d . . . Br6 Br 0.0200(2) 0.45902(11) 0.64541(9) 0.0682(6) Uani 1 1 d . . . Br7 Br 0.3222(2) 0.42222(11) 0.54610(9) 0.0671(6) Uani 1 1 d . . . Br8 Br 0.05278(18) 0.62306(9) 0.48741(8) 0.0558(5) 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 C101 0.062(15) 0.052(10) 0.090(17) -0.024(11) -0.042(13) -0.004(10) C102 0.10(2) 0.082(14) 0.075(17) -0.047(13) 0.033(15) -0.009(13) C103 0.099(19) 0.037(9) 0.11(2) -0.038(11) -0.041(16) 0.004(10) C104 0.058(15) 0.073(12) 0.096(17) -0.040(12) 0.002(12) -0.022(10) C105 0.111(19) 0.040(9) 0.068(15) 0.008(9) 0.038(14) 0.002(10) C106 0.044(12) 0.062(10) 0.071(14) -0.042(10) 0.002(10) -0.011(8) C107 0.13(2) 0.055(10) 0.059(15) -0.011(10) 0.014(14) 0.021(11) C108 0.082(17) 0.087(14) 0.065(15) -0.021(12) 0.020(13) 0.008(11) C109 0.071(17) 0.108(16) 0.062(15) -0.001(12) -0.009(13) 0.029(12) C110 0.056(15) 0.069(11) 0.089(17) -0.014(11) 0.013(13) -0.005(10) C111 0.052(14) 0.089(13) 0.055(13) -0.035(11) -0.007(11) 0.002(10) C112 0.047(14) 0.078(12) 0.073(15) -0.014(11) 0.011(11) 0.017(9) C113 0.048(14) 0.076(11) 0.055(13) -0.006(10) -0.008(11) 0.004(9) C114 0.067(15) 0.054(10) 0.071(15) -0.009(10) 0.003(12) 0.010(9) C115 0.092(19) 0.109(16) 0.044(14) -0.014(12) 0.008(13) 0.002(13) C116 0.15(3) 0.094(15) 0.066(17) -0.007(13) 0.047(16) 0.025(15) C201 0.076(17) 0.067(12) 0.12(2) 0.019(12) 0.027(15) 0.051(11) C202 0.091(18) 0.067(12) 0.091(18) -0.033(12) 0.023(14) -0.033(12) C203 0.075(16) 0.044(9) 0.065(14) 0.008(9) 0.006(11) -0.006(9) C204 0.079(16) 0.057(10) 0.068(14) -0.028(10) -0.014(11) -0.003(9) C205 0.055(14) 0.073(11) 0.102(12) -0.026(9) -0.038(12) 0.039(9) C206 0.16(2) 0.100(12) 0.097(12) -0.043(10) -0.009(14) 0.004(13) C207 0.125(18) 0.086(11) 0.117(13) -0.021(10) 0.041(15) 0.060(11) C208 0.20(2) 0.117(16) 0.113(13) -0.028(11) 0.055(18) 0.047(16) C209 0.16(2) 0.099(15) 0.122(14) -0.044(11) 0.055(19) -0.010(15) C210 0.20(2) 0.098(15) 0.139(15) -0.019(12) 0.07(2) 0.052(16) C211 0.18(2) 0.100(15) 0.131(14) -0.029(11) 0.066(19) 0.033(15) C212 0.21(2) 0.090(14) 0.124(14) -0.058(11) 0.056(19) -0.001(15) C213 0.19(2) 0.107(16) 0.177(18) 0.009(14) 0.09(2) 0.070(15) C214 0.22(3) 0.114(18) 0.172(18) -0.022(14) 0.09(2) 0.059(17) C215 0.27(3) 0.132(19) 0.168(19) -0.006(15) 0.13(2) 0.08(2) C216 0.27(4) 0.121(19) 0.156(18) -0.064(14) 0.10(3) 0.04(2) C301 0.065(15) 0.062(11) 0.081(16) -0.024(11) 0.026(13) -0.006(10) C302 0.063(13) 0.026(7) 0.073(14) -0.019(8) 0.015(11) -0.001(8) C303 0.074(16) 0.088(13) 0.056(14) -0.033(11) 0.005(12) 0.003(11) C304 0.060(14) 0.041(9) 0.098(16) -0.038(10) -0.016(11) -0.001(8) C305 0.054(13) 0.038(8) 0.055(13) -0.010(8) -0.006(10) 0.003(8) C306 0.044(13) 0.066(10) 0.068(14) -0.024(10) 0.003(11) -0.003(8) C307 0.073(16) 0.045(9) 0.081(16) 0.007(9) 0.012(12) -0.006(9) C308 0.079(16) 0.071(11) 0.052(13) -0.028(10) -0.004(11) -0.010(10) C309 0.12(2) 0.041(10) 0.11(2) 0.015(11) -0.014(17) 0.006(11) C310 0.074(16) 0.057(10) 0.078(16) -0.006(10) 0.007(13) -0.027(10) C311 0.079(16) 0.059(10) 0.089(17) -0.039(11) 0.040(13) -0.027(10) C312 0.100(18) 0.060(11) 0.051(14) 0.014(9) 0.008(12) 0.020(10) C313 0.059(14) 0.062(10) 0.062(14) -0.011(10) 0.011(11) -0.012(9) C314 0.044(13) 0.096(13) 0.072(16) -0.030(12) 0.002(11) -0.014(10) C315 0.13(2) 0.062(12) 0.10(2) -0.039(13) 0.039(17) -0.031(13) C316 0.13(2) 0.129(18) 0.074(18) -0.052(15) -0.018(16) 0.076(16) C401 0.094(17) 0.044(9) 0.094(17) -0.026(10) 0.048(14) -0.046(10) C402 0.091(18) 0.050(11) 0.100(19) -0.030(12) -0.012(15) 0.019(11) C403 0.052(15) 0.054(10) 0.071(15) -0.017(10) -0.040(12) 0.017(9) C404 0.073(17) 0.069(12) 0.084(17) -0.018(11) -0.020(13) -0.011(10) C405 0.102(18) 0.024(8) 0.089(17) 0.000(9) -0.004(14) 0.013(9) C406 0.060(14) 0.040(9) 0.108(18) -0.030(11) 0.005(13) -0.001(9) C407 0.069(16) 0.065(11) 0.068(15) -0.023(10) -0.035(12) 0.004(10) C408 0.059(15) 0.087(13) 0.055(14) -0.015(11) 0.016(11) 0.002(10) C409 0.090(18) 0.067(12) 0.092(18) -0.024(12) 0.003(15) 0.013(11) C410 0.061(15) 0.091(13) 0.075(16) -0.025(12) -0.001(13) 0.017(11) C411 0.083(17) 0.073(12) 0.085(17) -0.023(12) 0.007(14) -0.002(11) C412 0.060(16) 0.104(15) 0.084(18) -0.034(14) 0.009(13) 0.008(12) C413 0.083(16) 0.063(11) 0.093(17) -0.051(12) 0.010(14) -0.023(10) C414 0.069(17) 0.127(17) 0.063(16) -0.034(14) -0.015(13) 0.041(13) C415 0.12(2) 0.14(2) 0.062(17) -0.052(16) 0.031(16) -0.037(16) C416 0.11(2) 0.113(16) 0.043(14) -0.003(12) 0.006(13) 0.001(14) N101 0.065(12) 0.036(7) 0.090(13) -0.036(8) -0.017(10) -0.005(7) N102 0.056(11) 0.049(8) 0.055(11) -0.008(7) -0.019(9) 0.010(7) N201 0.064(13) 0.046(8) 0.101(14) -0.016(9) -0.030(11) 0.018(8) N202 0.058(11) 0.047(7) 0.075(11) -0.033(8) -0.002(9) -0.016(7) N301 0.074(12) 0.031(7) 0.082(12) -0.009(8) 0.010(10) 0.016(7) N302 0.070(12) 0.056(8) 0.085(13) -0.045(9) -0.022(10) 0.027(8) N401 0.081(13) 0.037(8) 0.107(15) -0.017(9) 0.009(11) -0.003(8) N402 0.041(10) 0.055(8) 0.075(12) -0.024(8) -0.020(9) 0.007(7) Cu1 0.0737(19) 0.0533(12) 0.0731(18) -0.0134(12) -0.0064(14) 0.0048(11) Cu2 0.0658(18) 0.0462(11) 0.0803(19) -0.0196(11) -0.0083(14) 0.0057(10) Cu3 0.0793(19) 0.0459(11) 0.089(2) -0.0201(12) -0.0157(15) -0.0027(11) Cu4 0.0680(18) 0.0519(12) 0.0835(19) -0.0223(12) -0.0023(14) -0.0045(10) Br1 0.0597(14) 0.0406(8) 0.0714(14) -0.0114(9) -0.0053(11) 0.0012(8) Br2 0.0553(14) 0.0599(10) 0.0763(15) -0.0115(10) -0.0014(11) -0.0063(9) Br3 0.0641(15) 0.0572(10) 0.0654(14) -0.0109(9) 0.0018(11) -0.0032(9) Br4 0.0656(15) 0.0523(9) 0.0758(15) -0.0160(9) -0.0088(11) 0.0024(9) Br5 0.0647(15) 0.0580(10) 0.0814(16) -0.0273(10) -0.0055(12) 0.0018(9) Br6 0.0723(16) 0.0588(10) 0.0775(16) -0.0253(10) 0.0065(12) -0.0148(9) Br7 0.0581(15) 0.0618(11) 0.0787(16) -0.0148(10) -0.0011(12) -0.0042(9) Br8 0.0526(13) 0.0457(9) 0.0720(14) -0.0210(9) -0.0008(10) -0.0033(8) _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 C101 N101 1.29(2) . ? C101 N102 1.34(2) . ? C101 H101 0.9500 . ? C102 C103 1.27(3) . ? C102 N101 1.41(2) . ? C102 H102 0.9500 . ? C103 N102 1.367(19) . ? C103 H103 0.9500 . ? C104 N102 1.50(2) . ? C104 H10A 0.9800 . ? C104 H10B 0.9800 . ? C104 H10C 0.9800 . ? C105 N101 1.47(2) . ? C105 C106 1.51(2) . ? C105 H10D 0.9900 . ? C105 H10E 0.9900 . ? C106 C107 1.52(2) . ? C106 H10F 0.9900 . ? C106 H10G 0.9900 . ? C107 C108 1.53(3) . ? C107 H10H 0.9900 . ? C107 H10I 0.9900 . ? C108 C109 1.48(3) . ? C108 H10J 0.9900 . ? C108 H10K 0.9900 . ? C109 C110 1.59(3) . ? C109 H10L 0.9900 . ? C109 H10M 0.9900 . ? C110 C111 1.53(2) . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.48(2) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 C113 1.52(2) . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 C114 1.57(2) . ? C113 H11G 0.9900 . ? C113 H11H 0.9900 . ? C114 C115 1.46(2) . ? C114 H11I 0.9900 . ? C114 H11J 0.9900 . ? C115 C116 1.54(3) . ? C115 H11K 0.9900 . ? C115 H11L 0.9900 . ? C116 H11M 0.9800 . ? C116 H11N 0.9800 . ? C116 H11O 0.9800 . ? C201 N202 1.32(2) . ? C201 N201 1.46(2) . ? C201 H201 0.9500 . ? C202 C203 1.37(2) . ? C202 N201 1.37(2) . ? C202 H202 0.9500 . ? C203 N202 1.40(2) . ? C203 H203 0.9500 . ? C204 N202 1.512(17) . ? C204 H20A 0.9800 . ? C204 H20B 0.9800 . ? C204 H20C 0.9800 . ? C205 C206 1.47(3) . ? C205 N201 1.51(2) . ? C205 H20D 0.9900 . ? C205 H20E 0.9900 . ? C206 C207 1.52(3) . ? C206 H20F 0.9900 . ? C206 H20G 0.9900 . ? C207 C208 1.41(3) . ? C207 H20H 0.9900 . ? C207 H20I 0.9900 . ? C208 C209 1.28(3) . ? C208 H20J 0.9900 . ? C208 H20K 0.9900 . ? C209 C210 1.33(4) . ? C209 H20L 0.9900 . ? C209 H20M 0.9900 . ? C210 C211 1.34(3) . ? C210 H21A 0.9900 . ? C210 H21B 0.9900 . ? C211 C212 1.42(4) . ? C211 H21C 0.9900 . ? C211 H21D 0.9900 . ? C212 C213 1.29(3) . ? C212 H21E 0.9900 . ? C212 H21F 0.9900 . ? C213 C214 1.34(4) . ? C213 H21G 0.9900 . ? C213 H21H 0.9900 . ? C214 C215 1.42(4) . ? C214 H21I 0.9900 . ? C214 H21J 0.9900 . ? C215 C216 1.49(4) . ? C215 H21K 0.9900 . ? C215 H21L 0.9900 . ? C216 H21M 0.9800 . ? C216 H21N 0.9800 . ? C216 H21O 0.9800 . ? C301 N301 1.306(18) . ? C301 N302 1.37(2) . ? C301 H301 0.9500 . ? C302 C303 1.33(2) . ? C302 N301 1.35(2) . ? C302 H302 0.9500 . ? C303 N302 1.454(19) . ? C303 H303 0.9500 . ? C304 N302 1.41(2) . ? C304 H30A 0.9800 . ? C304 H30B 0.9800 . ? C304 H30C 0.9800 . ? C305 N301 1.41(2) . ? C305 C306 1.50(2) . ? C305 H30D 0.9900 . ? C305 H30E 0.9900 . ? C306 C307 1.53(2) . ? C306 H30F 0.9900 . ? C306 H30G 0.9900 . ? C307 C308 1.57(3) . ? C307 H30H 0.9900 . ? C307 H30I 0.9900 . ? C308 C309 1.61(3) . ? C308 H30J 0.9900 . ? C308 H30K 0.9900 . ? C309 C310 1.47(3) . ? C309 H30L 0.9900 . ? C309 H30M 0.9900 . ? C310 C311 1.57(2) . ? C310 H31A 0.9900 . ? C310 H31B 0.9900 . ? C311 C312 1.51(3) . ? C311 H31C 0.9900 . ? C311 H31D 0.9900 . ? C312 C313 1.58(2) . ? C312 H31E 0.9900 . ? C312 H31F 0.9900 . ? C313 C314 1.63(3) . ? C313 H31G 0.9900 . ? C313 H31H 0.9900 . ? C314 C315 1.50(2) . ? C314 H31I 0.9900 . ? C314 H31J 0.9900 . ? C315 C316 1.49(3) . ? C315 H31K 0.9900 . ? C315 H31L 0.9900 . ? C316 H31M 0.9800 . ? C316 H31N 0.9800 . ? C316 H31O 0.9800 . ? C401 N402 1.28(2) . ? C401 N401 1.34(2) . ? C401 H401 0.9500 . ? C402 C403 1.31(3) . ? C402 N401 1.38(2) . ? C402 H402 0.9500 . ? C403 N402 1.346(19) . ? C403 H403 0.9500 . ? C404 N402 1.52(2) . ? C404 H40A 0.9800 . ? C404 H40B 0.9800 . ? C404 H40C 0.9800 . ? C405 N401 1.48(2) . ? C405 C406 1.52(3) . ? C405 H40D 0.9900 . ? C405 H40E 0.9900 . ? C406 C407 1.52(3) . ? C406 H40F 0.9900 . ? C406 H40G 0.9900 . ? C407 C408 1.57(2) . ? C407 H40H 0.9900 . ? C407 H40I 0.9900 . ? C408 C409 1.51(3) . ? C408 H40J 0.9900 . ? C408 H40K 0.9900 . ? C409 C410 1.56(3) . ? C409 H40L 0.9900 . ? C409 H40M 0.9900 . ? C410 C411 1.55(3) . ? C410 H41A 0.9900 . ? C410 H41B 0.9900 . ? C411 C412 1.49(3) . ? C411 H41C 0.9900 . ? C411 H41D 0.9900 . ? C412 C413 1.60(3) . ? C412 H41E 0.9900 . ? C412 H41F 0.9900 . ? C413 C414 1.50(3) . ? C413 H41G 0.9900 . ? C413 H41H 0.9900 . ? C414 C415 1.46(3) . ? C414 H41I 0.9900 . ? C414 H41J 0.9900 . ? C415 C416 1.63(3) . ? C415 H41K 0.9900 . ? C415 H41L 0.9900 . ? C416 H41M 0.9800 . ? C416 H41N 0.9800 . ? C416 H41O 0.9800 . ? Cu1 Br1 2.463(3) . ? Cu1 Br1 2.470(2) 2_658 ? Cu1 Br2 2.542(3) . ? Cu1 Br3 2.598(3) . ? Cu1 Cu2 2.674(4) . ? Cu1 Cu1 3.052(5) 2_658 ? Cu2 Br4 2.343(3) . ? Cu2 Br3 2.401(3) . ? Cu2 Br2 2.403(3) . ? Cu3 Br5 2.349(3) . ? Cu3 Br7 2.373(3) . ? Cu3 Br6 2.431(3) . ? Cu3 Cu4 2.700(4) . ? Cu4 Br8 2.474(3) . ? Cu4 Br8 2.491(3) 2_566 ? Cu4 Br7 2.548(3) . ? Cu4 Br6 2.567(3) . ? Cu4 Cu4 2.890(5) 2_566 ? Br1 Cu1 2.470(2) 2_658 ? Br8 Cu4 2.491(3) 2_566 ? 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 N101 C101 N102 113.6(15) . . ? N101 C101 H101 123.2 . . ? N102 C101 H101 123.2 . . ? C103 C102 N101 102.7(19) . . ? C103 C102 H102 128.7 . . ? N101 C102 H102 128.7 . . ? C102 C103 N102 117(2) . . ? C102 C103 H103 121.6 . . ? N102 C103 H103 121.6 . . ? N102 C104 H10A 109.5 . . ? N102 C104 H10B 109.5 . . ? H10A C104 H10B 109.5 . . ? N102 C104 H10C 109.5 . . ? H10A C104 H10C 109.5 . . ? H10B C104 H10C 109.5 . . ? N101 C105 C106 110.5(16) . . ? N101 C105 H10D 109.6 . . ? C106 C105 H10D 109.6 . . ? N101 C105 H10E 109.6 . . ? C106 C105 H10E 109.6 . . ? H10D C105 H10E 108.1 . . ? C105 C106 C107 113.1(15) . . ? C105 C106 H10F 109.0 . . ? C107 C106 H10F 109.0 . . ? C105 C106 H10G 109.0 . . ? C107 C106 H10G 109.0 . . ? H10F C106 H10G 107.8 . . ? C106 C107 C108 113.9(16) . . ? C106 C107 H10H 108.8 . . ? C108 C107 H10H 108.8 . . ? C106 C107 H10I 108.8 . . ? C108 C107 H10I 108.8 . . ? H10H C107 H10I 107.7 . . ? C109 C108 C107 116.4(17) . . ? C109 C108 H10J 108.2 . . ? C107 C108 H10J 108.2 . . ? C109 C108 H10K 108.2 . . ? C107 C108 H10K 108.2 . . ? H10J C108 H10K 107.4 . . ? C108 C109 C110 110.2(16) . . ? C108 C109 H10L 109.6 . . ? C110 C109 H10L 109.6 . . ? C108 C109 H10M 109.6 . . ? C110 C109 H10M 109.6 . . ? H10L C109 H10M 108.1 . . ? C111 C110 C109 113.2(16) . . ? C111 C110 H11A 108.9 . . ? C109 C110 H11A 108.9 . . ? C111 C110 H11B 108.9 . . ? C109 C110 H11B 108.9 . . ? H11A C110 H11B 107.7 . . ? C112 C111 C110 111.7(16) . . ? C112 C111 H11C 109.3 . . ? C110 C111 H11C 109.3 . . ? C112 C111 H11D 109.3 . . ? C110 C111 H11D 109.3 . . ? H11C C111 H11D 107.9 . . ? C111 C112 C113 114.7(15) . . ? C111 C112 H11E 108.6 . . ? C113 C112 H11E 108.6 . . ? C111 C112 H11F 108.6 . . ? C113 C112 H11F 108.6 . . ? H11E C112 H11F 107.6 . . ? C112 C113 C114 113.9(15) . . ? C112 C113 H11G 108.8 . . ? C114 C113 H11G 108.8 . . ? C112 C113 H11H 108.8 . . ? C114 C113 H11H 108.8 . . ? H11G C113 H11H 107.7 . . ? C115 C114 C113 113.5(16) . . ? C115 C114 H11I 108.9 . . ? C113 C114 H11I 108.9 . . ? C115 C114 H11J 108.9 . . ? C113 C114 H11J 108.9 . . ? H11I C114 H11J 107.7 . . ? C114 C115 C116 109.2(18) . . ? C114 C115 H11K 109.8 . . ? C116 C115 H11K 109.8 . . ? C114 C115 H11L 109.8 . . ? C116 C115 H11L 109.8 . . ? H11K C115 H11L 108.3 . . ? C115 C116 H11M 109.5 . . ? C115 C116 H11N 109.5 . . ? H11M C116 H11N 109.5 . . ? C115 C116 H11O 109.5 . . ? H11M C116 H11O 109.5 . . ? H11N C116 H11O 109.5 . . ? N202 C201 N201 101.9(18) . . ? N202 C201 H201 129.1 . . ? N201 C201 H201 129.1 . . ? C203 C202 N201 108.7(16) . . ? C203 C202 H202 125.7 . . ? N201 C202 H202 125.7 . . ? C202 C203 N202 104.2(17) . . ? C202 C203 H203 127.9 . . ? N202 C203 H203 127.9 . . ? N202 C204 H20A 109.5 . . ? N202 C204 H20B 109.5 . . ? H20A C204 H20B 109.5 . . ? N202 C204 H20C 109.5 . . ? H20A C204 H20C 109.5 . . ? H20B C204 H20C 109.5 . . ? C206 C205 N201 114.0(16) . . ? C206 C205 H20D 108.8 . . ? N201 C205 H20D 108.8 . . ? C206 C205 H20E 108.8 . . ? N201 C205 H20E 108.8 . . ? H20D C205 H20E 107.7 . . ? C205 C206 C207 115(2) . . ? C205 C206 H20F 108.6 . . ? C207 C206 H20F 108.6 . . ? C205 C206 H20G 108.6 . . ? C207 C206 H20G 108.6 . . ? H20F C206 H20G 107.6 . . ? C208 C207 C206 120(3) . . ? C208 C207 H20H 107.3 . . ? C206 C207 H20H 107.3 . . ? C208 C207 H20I 107.4 . . ? C206 C207 H20I 107.3 . . ? H20H C207 H20I 106.9 . . ? C209 C208 C207 138(3) . . ? C209 C208 H20J 102.6 . . ? C207 C208 H20J 102.6 . . ? C209 C208 H20K 102.7 . . ? C207 C208 H20K 102.7 . . ? H20J C208 H20K 105.0 . . ? C208 C209 C210 148(3) . . ? C208 C209 H20L 99.9 . . ? C210 C209 H20L 99.9 . . ? C208 C209 H20M 99.9 . . ? C210 C209 H20M 99.9 . . ? H20L C209 H20M 104.1 . . ? C209 C210 C211 149(4) . . ? C209 C210 H21A 99.4 . . ? C211 C210 H21A 99.4 . . ? C209 C210 H21B 99.4 . . ? C211 C210 H21B 99.4 . . ? H21A C210 H21B 104.0 . . ? C210 C211 C212 141(3) . . ? C210 C211 H21C 101.9 . . ? C212 C211 H21C 101.8 . . ? C210 C211 H21D 101.8 . . ? C212 C211 H21D 101.9 . . ? H21C C211 H21D 104.7 . . ? C213 C212 C211 128(3) . . ? C213 C212 H21E 105.2 . . ? C211 C212 H21E 105.2 . . ? C213 C212 H21F 105.2 . . ? C211 C212 H21F 105.2 . . ? H21E C212 H21F 105.9 . . ? C212 C213 C214 129(4) . . ? C212 C213 H21G 105.0 . . ? C214 C213 H21G 105.0 . . ? C212 C213 H21H 105.0 . . ? C214 C213 H21H 105.0 . . ? H21G C213 H21H 105.9 . . ? C213 C214 C215 134(4) . . ? C213 C214 H21I 103.7 . . ? C215 C214 H21I 103.8 . . ? C213 C214 H21J 103.7 . . ? C215 C214 H21J 103.8 . . ? H21I C214 H21J 105.4 . . ? C214 C215 C216 133(4) . . ? C214 C215 H21K 104.1 . . ? C216 C215 H21K 104.1 . . ? C214 C215 H21L 104.1 . . ? C216 C215 H21L 104.1 . . ? H21K C215 H21L 105.5 . . ? C215 C216 H21M 109.5 . . ? C215 C216 H21N 109.5 . . ? H21M C216 H21N 109.5 . . ? C215 C216 H21O 109.5 . . ? H21M C216 H21O 109.5 . . ? H21N C216 H21O 109.5 . . ? N301 C301 N302 114.2(15) . . ? N301 C301 H301 122.9 . . ? N302 C301 H301 122.9 . . ? C303 C302 N301 111.5(13) . . ? C303 C302 H302 124.3 . . ? N301 C302 H302 124.3 . . ? C302 C303 N302 106.7(17) . . ? C302 C303 H303 126.6 . . ? N302 C303 H303 126.6 . . ? N302 C304 H30A 109.5 . . ? N302 C304 H30B 109.5 . . ? H30A C304 H30B 109.5 . . ? N302 C304 H30C 109.5 . . ? H30A C304 H30C 109.5 . . ? H30B C304 H30C 109.5 . . ? N301 C305 C306 113.3(15) . . ? N301 C305 H30D 108.9 . . ? C306 C305 H30D 108.9 . . ? N301 C305 H30E 108.9 . . ? C306 C305 H30E 108.9 . . ? H30D C305 H30E 107.7 . . ? C305 C306 C307 110.8(15) . . ? C305 C306 H30F 109.5 . . ? C307 C306 H30F 109.5 . . ? C305 C306 H30G 109.5 . . ? C307 C306 H30G 109.5 . . ? H30F C306 H30G 108.1 . . ? C306 C307 C308 111.8(16) . . ? C306 C307 H30H 109.2 . . ? C308 C307 H30H 109.3 . . ? C306 C307 H30I 109.2 . . ? C308 C307 H30I 109.3 . . ? H30H C307 H30I 107.9 . . ? C307 C308 C309 108.5(16) . . ? C307 C308 H30J 110.0 . . ? C309 C308 H30J 110.0 . . ? C307 C308 H30K 110.0 . . ? C309 C308 H30K 110.0 . . ? H30J C308 H30K 108.4 . . ? C310 C309 C308 111.7(18) . . ? C310 C309 H30L 109.3 . . ? C308 C309 H30L 109.3 . . ? C310 C309 H30M 109.3 . . ? C308 C309 H30M 109.3 . . ? H30L C309 H30M 107.9 . . ? C309 C310 C311 116.3(17) . . ? C309 C310 H31A 108.2 . . ? C311 C310 H31A 108.2 . . ? C309 C310 H31B 108.2 . . ? C311 C310 H31B 108.2 . . ? H31A C310 H31B 107.4 . . ? C312 C311 C310 113.6(16) . . ? C312 C311 H31C 108.8 . . ? C310 C311 H31C 108.8 . . ? C312 C311 H31D 108.8 . . ? C310 C311 H31D 108.8 . . ? H31C C311 H31D 107.7 . . ? C311 C312 C313 106.2(17) . . ? C311 C312 H31E 110.5 . . ? C313 C312 H31E 110.5 . . ? C311 C312 H31F 110.5 . . ? C313 C312 H31F 110.5 . . ? H31E C312 H31F 108.7 . . ? C312 C313 C314 109.8(15) . . ? C312 C313 H31G 109.7 . . ? C314 C313 H31G 109.7 . . ? C312 C313 H31H 109.7 . . ? C314 C313 H31H 109.7 . . ? H31G C313 H31H 108.2 . . ? C315 C314 C313 112.9(17) . . ? C315 C314 H31I 109.0 . . ? C313 C314 H31I 109.0 . . ? C315 C314 H31J 109.0 . . ? C313 C314 H31J 109.0 . . ? H31I C314 H31J 107.8 . . ? C316 C315 C314 115(2) . . ? C316 C315 H31K 108.6 . . ? C314 C315 H31K 108.6 . . ? C316 C315 H31L 108.6 . . ? C314 C315 H31L 108.6 . . ? H31K C315 H31L 107.6 . . ? C315 C316 H31M 109.5 . . ? C315 C316 H31N 109.5 . . ? H31M C316 H31N 109.5 . . ? C315 C316 H31O 109.5 . . ? H31M C316 H31O 109.5 . . ? H31N C316 H31O 109.5 . . ? N402 C401 N401 111.7(15) . . ? N402 C401 H401 124.1 . . ? N401 C401 H401 124.1 . . ? C403 C402 N401 109.8(19) . . ? C403 C402 H402 125.1 . . ? N401 C402 H402 125.1 . . ? C402 C403 N402 106.7(19) . . ? C402 C403 H403 126.7 . . ? N402 C403 H403 126.7 . . ? N402 C404 H40A 109.5 . . ? N402 C404 H40B 109.5 . . ? H40A C404 H40B 109.5 . . ? N402 C404 H40C 109.5 . . ? H40A C404 H40C 109.5 . . ? H40B C404 H40C 109.5 . . ? N401 C405 C406 110.2(17) . . ? N401 C405 H40D 109.6 . . ? C406 C405 H40D 109.6 . . ? N401 C405 H40E 109.6 . . ? C406 C405 H40E 109.6 . . ? H40D C405 H40E 108.1 . . ? C407 C406 C405 108.9(16) . . ? C407 C406 H40F 109.9 . . ? C405 C406 H40F 109.9 . . ? C407 C406 H40G 109.9 . . ? C405 C406 H40G 109.9 . . ? H40F C406 H40G 108.3 . . ? C406 C407 C408 110.6(16) . . ? C406 C407 H40H 109.5 . . ? C408 C407 H40H 109.5 . . ? C406 C407 H40I 109.5 . . ? C408 C407 H40I 109.5 . . ? H40H C407 H40I 108.1 . . ? C409 C408 C407 111.8(17) . . ? C409 C408 H40J 109.3 . . ? C407 C408 H40J 109.3 . . ? C409 C408 H40K 109.3 . . ? C407 C408 H40K 109.3 . . ? H40J C408 H40K 107.9 . . ? C408 C409 C410 112.4(17) . . ? C408 C409 H40L 109.1 . . ? C410 C409 H40L 109.1 . . ? C408 C409 H40M 109.1 . . ? C410 C409 H40M 109.1 . . ? H40L C409 H40M 107.9 . . ? C411 C410 C409 111.4(16) . . ? C411 C410 H41A 109.3 . . ? C409 C410 H41A 109.3 . . ? C411 C410 H41B 109.3 . . ? C409 C410 H41B 109.3 . . ? H41A C410 H41B 108.0 . . ? C412 C411 C410 111.5(17) . . ? C412 C411 H41C 109.3 . . ? C410 C411 H41C 109.3 . . ? C412 C411 H41D 109.3 . . ? C410 C411 H41D 109.3 . . ? H41C C411 H41D 108.0 . . ? C411 C412 C413 116.0(17) . . ? C411 C412 H41E 108.3 . . ? C413 C412 H41E 108.3 . . ? C411 C412 H41F 108.3 . . ? C413 C412 H41F 108.3 . . ? H41E C412 H41F 107.4 . . ? C414 C413 C412 116.3(17) . . ? C414 C413 H41G 108.2 . . ? C412 C413 H41G 108.2 . . ? C414 C413 H41H 108.2 . . ? C412 C413 H41H 108.2 . . ? H41G C413 H41H 107.4 . . ? C415 C414 C413 114.9(19) . . ? C415 C414 H41I 108.5 . . ? C413 C414 H41I 108.5 . . ? C415 C414 H41J 108.5 . . ? C413 C414 H41J 108.5 . . ? H41I C414 H41J 107.5 . . ? C414 C415 C416 114(2) . . ? C414 C415 H41K 108.8 . . ? C416 C415 H41K 108.8 . . ? C414 C415 H41L 108.8 . . ? C416 C415 H41L 108.8 . . ? H41K C415 H41L 107.7 . . ? C415 C416 H41M 109.5 . . ? C415 C416 H41N 109.5 . . ? H41M C416 H41N 109.5 . . ? C415 C416 H41O 109.5 . . ? H41M C416 H41O 109.5 . . ? H41N C416 H41O 109.5 . . ? C101 N101 C102 107.2(18) . . ? C101 N101 C105 128.2(15) . . ? C102 N101 C105 124.6(16) . . ? C101 N102 C103 99.8(17) . . ? C101 N102 C104 125.8(14) . . ? C103 N102 C104 134.3(18) . . ? C202 N201 C201 109.5(16) . . ? C202 N201 C205 124.5(15) . . ? C201 N201 C205 125.9(18) . . ? C201 N202 C203 115.5(16) . . ? C201 N202 C204 117.4(15) . . ? C203 N202 C204 127.0(16) . . ? C301 N301 C302 105.7(15) . . ? C301 N301 C305 127.7(15) . . ? C302 N301 C305 126.5(12) . . ? C301 N302 C304 129.0(14) . . ? C301 N302 C303 101.9(14) . . ? C304 N302 C303 128.0(17) . . ? C401 N401 C402 102.7(17) . . ? C401 N401 C405 127.2(14) . . ? C402 N401 C405 128.8(19) . . ? C401 N402 C403 108.3(17) . . ? C401 N402 C404 122.9(14) . . ? C403 N402 C404 128.5(17) . . ? Br1 Cu1 Br1 103.58(10) . 2_658 ? Br1 Cu1 Br2 108.28(10) . . ? Br1 Cu1 Br2 119.05(11) 2_658 . ? Br1 Cu1 Br3 116.09(11) . . ? Br1 Cu1 Br3 105.88(10) 2_658 . ? Br2 Cu1 Br3 104.54(11) . . ? Br1 Cu1 Cu2 146.17(10) . . ? Br1 Cu1 Cu2 110.25(10) 2_658 . ? Br2 Cu1 Cu2 54.80(9) . . ? Br3 Cu1 Cu2 54.14(9) . . ? Br1 Cu1 Cu1 51.89(8) . 2_658 ? Br1 Cu1 Cu1 51.69(7) 2_658 2_658 ? Br2 Cu1 Cu1 130.25(15) . 2_658 ? Br3 Cu1 Cu1 125.21(14) . 2_658 ? Cu2 Cu1 Cu1 161.94(11) . 2_658 ? Br4 Cu2 Br3 124.03(13) . . ? Br4 Cu2 Br2 120.29(12) . . ? Br3 Cu2 Br2 115.63(12) . . ? Br4 Cu2 Cu1 155.06(10) . . ? Br3 Cu2 Cu1 61.31(9) . . ? Br2 Cu2 Cu1 59.80(9) . . ? Br5 Cu3 Br7 124.33(13) . . ? Br5 Cu3 Br6 120.01(12) . . ? Br7 Cu3 Br6 115.59(12) . . ? Br5 Cu3 Cu4 157.96(10) . . ? Br7 Cu3 Cu4 59.87(9) . . ? Br6 Cu3 Cu4 59.75(9) . . ? Br8 Cu4 Br8 108.80(11) . 2_566 ? Br8 Cu4 Br7 112.61(11) . . ? Br8 Cu4 Br7 110.12(9) 2_566 . ? Br8 Cu4 Br6 112.18(10) . . ? Br8 Cu4 Br6 107.72(10) 2_566 . ? Br7 Cu4 Br6 105.28(12) . . ? Br8 Cu4 Cu3 113.03(10) . . ? Br8 Cu4 Cu3 138.17(11) 2_566 . ? Br7 Cu4 Cu3 53.68(9) . . ? Br6 Cu4 Cu3 54.90(9) . . ? Br8 Cu4 Cu4 54.68(8) . 2_566 ? Br8 Cu4 Cu4 54.12(8) 2_566 2_566 ? Br7 Cu4 Cu4 128.72(15) . 2_566 ? Br6 Cu4 Cu4 125.83(14) . 2_566 ? Cu3 Cu4 Cu4 167.67(12) . 2_566 ? Cu1 Br1 Cu1 76.42(10) . 2_658 ? Cu2 Br2 Cu1 65.41(9) . . ? Cu2 Br3 Cu1 64.55(10) . . ? Cu3 Br6 Cu4 65.35(10) . . ? Cu3 Br7 Cu4 66.45(10) . . ? Cu4 Br8 Cu4 71.20(11) . 2_566 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N101 C102 C103 N102 -1(3) . . . . ? N101 C105 C106 C107 -173.2(15) . . . . ? C105 C106 C107 C108 167.2(17) . . . . ? C106 C107 C108 C109 -179.7(19) . . . . ? C107 C108 C109 C110 -176.8(18) . . . . ? C108 C109 C110 C111 -175.9(18) . . . . ? C109 C110 C111 C112 179.2(17) . . . . ? C110 C111 C112 C113 174.8(16) . . . . ? C111 C112 C113 C114 178.4(16) . . . . ? C112 C113 C114 C115 -179.9(18) . . . . ? C113 C114 C115 C116 -174.7(18) . . . . ? N201 C202 C203 N202 3(2) . . . . ? N201 C205 C206 C207 81(3) . . . . ? C205 C206 C207 C208 174(2) . . . . ? C206 C207 C208 C209 -177(4) . . . . ? C207 C208 C209 C210 179(4) . . . . ? C208 C209 C210 C211 -177(5) . . . . ? C209 C210 C211 C212 -177(4) . . . . ? C210 C211 C212 C213 -177(3) . . . . ? C211 C212 C213 C214 177(3) . . . . ? C212 C213 C214 C215 -178(3) . . . . ? C213 C214 C215 C216 180(3) . . . . ? N301 C302 C303 N302 1(2) . . . . ? N301 C305 C306 C307 176.3(13) . . . . ? C305 C306 C307 C308 175.1(14) . . . . ? C306 C307 C308 C309 175.6(15) . . . . ? C307 C308 C309 C310 178.6(16) . . . . ? C308 C309 C310 C311 178.8(15) . . . . ? C309 C310 C311 C312 -178.6(17) . . . . ? C310 C311 C312 C313 178.2(14) . . . . ? C311 C312 C313 C314 179.1(14) . . . . ? C312 C313 C314 C315 -179.2(16) . . . . ? C313 C314 C315 C316 -176.8(15) . . . . ? N401 C402 C403 N402 -5(2) . . . . ? N401 C405 C406 C407 175.4(13) . . . . ? C405 C406 C407 C408 175.1(14) . . . . ? C406 C407 C408 C409 170.3(15) . . . . ? C407 C408 C409 C410 170.5(16) . . . . ? C408 C409 C410 C411 177.8(18) . . . . ? C409 C410 C411 C412 176.8(18) . . . . ? C410 C411 C412 C413 -179.5(17) . . . . ? C411 C412 C413 C414 177.4(19) . . . . ? C412 C413 C414 C415 -178.2(18) . . . . ? C413 C414 C415 C416 176.9(18) . . . . ? N102 C101 N101 C102 2(2) . . . . ? N102 C101 N101 C105 180.0(17) . . . . ? C103 C102 N101 C101 -1(2) . . . . ? C103 C102 N101 C105 -178.9(19) . . . . ? C106 C105 N101 C101 -102(2) . . . . ? C106 C105 N101 C102 76(2) . . . . ? N101 C101 N102 C103 -2(2) . . . . ? N101 C101 N102 C104 176.1(16) . . . . ? C102 C103 N102 C101 2(3) . . . . ? C102 C103 N102 C104 -176(2) . . . . ? C203 C202 N201 C201 -1(2) . . . . ? C203 C202 N201 C205 -177.0(16) . . . . ? N202 C201 N201 C202 -2(2) . . . . ? N202 C201 N201 C205 174.3(17) . . . . ? C206 C205 N201 C202 93(3) . . . . ? C206 C205 N201 C201 -83(3) . . . . ? N201 C201 N202 C203 4(2) . . . . ? N201 C201 N202 C204 -173.8(14) . . . . ? C202 C203 N202 C201 -5(2) . . . . ? C202 C203 N202 C204 173.0(17) . . . . ? N302 C301 N301 C302 2(2) . . . . ? N302 C301 N301 C305 -172.7(18) . . . . ? C303 C302 N301 C301 -2(2) . . . . ? C303 C302 N301 C305 172.7(18) . . . . ? C306 C305 N301 C301 79(2) . . . . ? C306 C305 N301 C302 -94(2) . . . . ? N301 C301 N302 C304 -170.0(16) . . . . ? N301 C301 N302 C303 -1(2) . . . . ? C302 C303 N302 C301 0(2) . . . . ? C302 C303 N302 C304 168.8(17) . . . . ? N402 C401 N401 C402 -9(2) . . . . ? N402 C401 N401 C405 -176.5(19) . . . . ? C403 C402 N401 C401 8(2) . . . . ? C403 C402 N401 C405 175.9(18) . . . . ? C406 C405 N401 C401 88(2) . . . . ? C406 C405 N401 C402 -76(2) . . . . ? N401 C401 N402 C403 6(2) . . . . ? N401 C401 N402 C404 -179.7(16) . . . . ? C402 C403 N402 C401 0(2) . . . . ? C402 C403 N402 C404 -174.3(18) . . . . ? Br1 Cu1 Cu2 Br4 166.3(2) . . . . ? Br1 Cu1 Cu2 Br4 -14.3(4) 2_658 . . . ? Br2 Cu1 Cu2 Br4 97.6(3) . . . . ? Br3 Cu1 Cu2 Br4 -109.7(3) . . . . ? Cu1 Cu1 Cu2 Br4 -15.2(7) 2_658 . . . ? Br1 Cu1 Cu2 Br3 -84.0(2) . . . . ? Br1 Cu1 Cu2 Br3 95.35(11) 2_658 . . . ? Br2 Cu1 Cu2 Br3 -152.74(9) . . . . ? Cu1 Cu1 Cu2 Br3 94.5(5) 2_658 . . . ? Br1 Cu1 Cu2 Br2 68.7(2) . . . . ? Br1 Cu1 Cu2 Br2 -111.91(12) 2_658 . . . ? Br3 Cu1 Cu2 Br2 152.74(9) . . . . ? Cu1 Cu1 Cu2 Br2 -112.8(5) 2_658 . . . ? Br5 Cu3 Cu4 Br8 5.8(4) . . . . ? Br7 Cu3 Cu4 Br8 -101.88(12) . . . . ? Br6 Cu3 Cu4 Br8 101.69(11) . . . . ? Br5 Cu3 Cu4 Br8 -172.7(3) . . . 2_566 ? Br7 Cu3 Cu4 Br8 79.57(18) . . . 2_566 ? Br6 Cu3 Cu4 Br8 -76.86(18) . . . 2_566 ? Br5 Cu3 Cu4 Br7 107.7(4) . . . . ? Br6 Cu3 Cu4 Br7 -156.42(10) . . . . ? Br5 Cu3 Cu4 Br6 -95.9(4) . . . . ? Br7 Cu3 Cu4 Br6 156.42(10) . . . . ? Br5 Cu3 Cu4 Cu4 1.9(10) . . . 2_566 ? Br7 Cu3 Cu4 Cu4 -105.8(7) . . . 2_566 ? Br6 Cu3 Cu4 Cu4 97.8(7) . . . 2_566 ? Br1 Cu1 Br1 Cu1 0.000(2) 2_658 . . 2_658 ? Br2 Cu1 Br1 Cu1 -127.29(14) . . . 2_658 ? Br3 Cu1 Br1 Cu1 115.58(14) . . . 2_658 ? Cu2 Cu1 Br1 Cu1 179.4(3) . . . 2_658 ? Br4 Cu2 Br2 Cu1 -151.05(12) . . . . ? Br3 Cu2 Br2 Cu1 26.46(9) . . . . ? Br1 Cu1 Br2 Cu2 -146.89(11) . . . . ? Br1 Cu1 Br2 Cu2 95.32(13) 2_658 . . . ? Br3 Cu1 Br2 Cu2 -22.55(8) . . . . ? Cu1 Cu1 Br2 Cu2 158.00(16) 2_658 . . . ? Br4 Cu2 Br3 Cu1 151.36(13) . . . . ? Br2 Cu2 Br3 Cu1 -26.04(9) . . . . ? Br1 Cu1 Br3 Cu2 141.93(11) . . . . ? Br1 Cu1 Br3 Cu2 -103.79(11) 2_658 . . . ? Br2 Cu1 Br3 Cu2 22.74(8) . . . . ? Cu1 Cu1 Br3 Cu2 -157.77(14) 2_658 . . . ? Br5 Cu3 Br6 Cu4 154.47(13) . . . . ? Br7 Cu3 Br6 Cu4 -22.55(10) . . . . ? Br8 Cu4 Br6 Cu3 -103.28(12) . . . . ? Br8 Cu4 Br6 Cu3 137.01(11) 2_566 . . . ? Br7 Cu4 Br6 Cu3 19.51(8) . . . . ? Cu4 Cu4 Br6 Cu3 -164.88(15) 2_566 . . . ? Br5 Cu3 Br7 Cu4 -154.35(14) . . . . ? Br6 Cu3 Br7 Cu4 22.52(10) . . . . ? Br8 Cu4 Br7 Cu3 102.69(12) . . . . ? Br8 Cu4 Br7 Cu3 -135.68(13) 2_566 . . . ? Br6 Cu4 Br7 Cu3 -19.83(8) . . . . ? Cu4 Cu4 Br7 Cu3 164.74(16) 2_566 . . . ? Br8 Cu4 Br8 Cu4 0.0 2_566 . . 2_566 ? Br7 Cu4 Br8 Cu4 122.37(15) . . . 2_566 ? Br6 Cu4 Br8 Cu4 -119.08(15) . . . 2_566 ? Cu3 Cu4 Br8 Cu4 -178.98(17) . . . 2_566 ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.899 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.124 #===END data_msb1_15 _database_code_depnum_ccdc_archive 'CCDC 769706' #TrackingRef 'MarionStricker.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H56 Cu N4, Br2 Cu' _chemical_formula_sum 'C30 H56 Br2 Cu2 N4' _chemical_formula_weight 759.69 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.002(3) _cell_length_b 9.454(3) _cell_length_c 20.757(6) _cell_angle_alpha 85.74(2) _cell_angle_beta 87.75(3) _cell_angle_gamma 78.95(3) _cell_volume 1728.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 2718 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 25.79 _exptl_crystal_description 'square plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 3.566 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5518 _exptl_absorpt_correction_T_max 0.7843 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'STOE IPDS I' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21313 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1160 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 26.04 _reflns_number_total 21313 _reflns_number_gt 11785 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _publ_section_exptl_refinement ;Refinement of twinned data was carried out via hklf5-file, thus reflections were not merged, resulting in a high (formal) ratio of unique to expected reflections (3.13). ; _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^)+(0.1203P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21313 _refine_ls_number_parameters 346 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1405 _refine_ls_R_factor_gt 0.0810 _refine_ls_wR_factor_ref 0.2386 _refine_ls_wR_factor_gt 0.1996 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _refine_ls_shift/su_max 0.003 _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 C101 C 0.5694(8) 0.9784(7) 0.0921(4) 0.0315(17) Uani 1 1 d . . . H101 H 0.5388 1.0653 0.1134 0.038 Uiso 1 1 calc R . . C102 C 0.5853(9) 0.7565(7) 0.0641(4) 0.0333(17) Uani 1 1 d . . . H102 H 0.5698 0.6600 0.0631 0.040 Uiso 1 1 calc R . . C103 C 0.6758(12) 0.8191(8) 0.0245(4) 0.054(3) Uani 1 1 d . . . H103 H 0.7342 0.7755 -0.0104 0.064 Uiso 1 1 calc R . . C104 C 0.4076(9) 0.8355(7) 0.1594(4) 0.0361(18) Uani 1 1 d . . . H10A H 0.3190 0.8067 0.1409 0.043 Uiso 1 1 calc R . . H10B H 0.3719 0.9290 0.1787 0.043 Uiso 1 1 calc R . . C105 C 0.4701(8) 0.7236(7) 0.2120(3) 0.0294(16) Uani 1 1 d . . . H10C H 0.5523 0.7564 0.2337 0.035 Uiso 1 1 calc R . . H10D H 0.5137 0.6318 0.1925 0.035 Uiso 1 1 calc R . . C106 C 0.3474(9) 0.6978(8) 0.2619(4) 0.0356(18) Uani 1 1 d . . . H10E H 0.3020 0.7907 0.2801 0.043 Uiso 1 1 calc R . . H10F H 0.2666 0.6635 0.2400 0.043 Uiso 1 1 calc R . . C107 C 0.4047(9) 0.5901(8) 0.3161(4) 0.0331(17) Uani 1 1 d . . . H10G H 0.4865 0.6240 0.3376 0.040 Uiso 1 1 calc R . . H10H H 0.4492 0.4970 0.2979 0.040 Uiso 1 1 calc R . . C108 C 0.2825(9) 0.5642(7) 0.3672(4) 0.0353(17) Uani 1 1 d . . . H10I H 0.2373 0.6573 0.3853 0.042 Uiso 1 1 calc R . . H10J H 0.2012 0.5292 0.3460 0.042 Uiso 1 1 calc R . . C109 C 0.3430(9) 0.4549(8) 0.4227(4) 0.0363(18) Uani 1 1 d . . . H10K H 0.4240 0.4901 0.4441 0.044 Uiso 1 1 calc R . . H10L H 0.3885 0.3619 0.4046 0.044 Uiso 1 1 calc R . . C110 C 0.2201(9) 0.4286(8) 0.4737(4) 0.0360(17) Uani 1 1 d . . . H11A H 0.1758 0.5211 0.4925 0.043 Uiso 1 1 calc R . . H11B H 0.1383 0.3946 0.4524 0.043 Uiso 1 1 calc R . . C111 C 0.2815(8) 0.3195(7) 0.5270(4) 0.0313(16) Uani 1 1 d . . . H11C H 0.3633 0.3537 0.5483 0.038 Uiso 1 1 calc R . . H11D H 0.3263 0.2273 0.5080 0.038 Uiso 1 1 calc R . . C112 C 0.1593(9) 0.2919(7) 0.5783(4) 0.0364(18) Uani 1 1 d . . . H11E H 0.1141 0.3843 0.5970 0.044 Uiso 1 1 calc R . . H11F H 0.0778 0.2574 0.5569 0.044 Uiso 1 1 calc R . . C113 C 0.2206(9) 0.1813(7) 0.6330(4) 0.0364(18) Uani 1 1 d . . . H11G H 0.2669 0.0894 0.6142 0.044 Uiso 1 1 calc R . . H11H H 0.3013 0.2165 0.6546 0.044 Uiso 1 1 calc R . . C114 C 0.1004(11) 0.1520(9) 0.6836(4) 0.046(2) Uani 1 1 d . . . H11I H 0.0521 0.2440 0.7019 0.055 Uiso 1 1 calc R . . H11J H 0.0210 0.1138 0.6625 0.055 Uiso 1 1 calc R . . C115 C 0.1655(12) 0.0456(9) 0.7377(4) 0.055(2) Uani 1 1 d . . . H11K H 0.0848 0.0313 0.7692 0.083 Uiso 1 1 calc R . . H11L H 0.2437 0.0832 0.7590 0.083 Uiso 1 1 calc R . . H11M H 0.2102 -0.0468 0.7201 0.083 Uiso 1 1 calc R . . C201 C 0.9574(9) 1.2485(7) -0.0865(4) 0.0396(19) Uani 1 1 d . . . H201 H 1.0207 1.1609 -0.0977 0.048 Uiso 1 1 calc R . . C202 C 0.7820(11) 1.4038(8) -0.0414(5) 0.053(2) Uani 1 1 d . . . H202 H 0.6988 1.4449 -0.0149 0.064 Uiso 1 1 calc R . . C203 C 0.8673(11) 1.4792(7) -0.0835(4) 0.054(3) Uani 1 1 d . . . H203 H 0.8526 1.5811 -0.0915 0.065 Uiso 1 1 calc R . . C204 C 1.0931(9) 1.4136(7) -0.1572(4) 0.0351(17) Uani 1 1 d . . . H20A H 1.1485 1.3220 -0.1736 0.042 Uiso 1 1 calc R . . H20B H 1.1662 1.4574 -0.1346 0.042 Uiso 1 1 calc R . . C205 C 1.0304(9) 1.5159(7) -0.2143(3) 0.0327(16) Uani 1 1 d . . . H20C H 0.9562 1.4730 -0.2366 0.039 Uiso 1 1 calc R . . H20D H 0.9766 1.6084 -0.1981 0.039 Uiso 1 1 calc R . . C206 C 1.1542(9) 1.5453(8) -0.2621(4) 0.0402(19) Uani 1 1 d . . . H20E H 1.2310 1.5829 -0.2390 0.048 Uiso 1 1 calc R . . H20F H 1.2045 1.4531 -0.2796 0.048 Uiso 1 1 calc R . . C207 C 1.0979(9) 1.6513(8) -0.3173(4) 0.0360(18) Uani 1 1 d . . . H20G H 1.0489 1.7437 -0.2996 0.043 Uiso 1 1 calc R . . H20H H 1.0196 1.6143 -0.3397 0.043 Uiso 1 1 calc R . . C208 C 1.2189(8) 1.6812(7) -0.3667(4) 0.0328(16) Uani 1 1 d . . . H20I H 1.2666 1.5896 -0.3854 0.039 Uiso 1 1 calc R . . H20J H 1.2983 1.7170 -0.3445 0.039 Uiso 1 1 calc R . . C209 C 1.1581(8) 1.7917(8) -0.4215(4) 0.0339(17) Uani 1 1 d . . . H20K H 1.1135 1.8845 -0.4030 0.041 Uiso 1 1 calc R . . H20L H 1.0765 1.7576 -0.4429 0.041 Uiso 1 1 calc R . . C210 C 1.2806(9) 1.8173(8) -0.4721(4) 0.0358(17) Uani 1 1 d . . . H21A H 1.3623 1.8514 -0.4507 0.043 Uiso 1 1 calc R . . H21B H 1.3250 1.7247 -0.4907 0.043 Uiso 1 1 calc R . . C211 C 1.2186(9) 1.9281(7) -0.5265(4) 0.0371(18) Uani 1 1 d . . . H21C H 1.1738 2.0205 -0.5077 0.044 Uiso 1 1 calc R . . H21D H 1.1369 1.8938 -0.5478 0.044 Uiso 1 1 calc R . . C212 C 1.3394(8) 1.9555(7) -0.5775(4) 0.0348(17) Uani 1 1 d . . . H21E H 1.4207 1.9906 -0.5563 0.042 Uiso 1 1 calc R . . H21F H 1.3848 1.8630 -0.5960 0.042 Uiso 1 1 calc R . . C213 C 1.2780(9) 2.0647(8) -0.6321(4) 0.0368(18) Uani 1 1 d . . . H21G H 1.2331 2.1574 -0.6136 0.044 Uiso 1 1 calc R . . H21H H 1.1962 2.0299 -0.6531 0.044 Uiso 1 1 calc R . . C214 C 1.3992(9) 2.0915(8) -0.6835(4) 0.041(2) Uani 1 1 d . . . H21I H 1.4808 2.1268 -0.6626 0.049 Uiso 1 1 calc R . . H21J H 1.4443 1.9989 -0.7020 0.049 Uiso 1 1 calc R . . C215 C 1.3367(12) 2.2000(9) -0.7377(4) 0.054(2) Uani 1 1 d . . . H21K H 1.2692 2.1584 -0.7635 0.081 Uiso 1 1 calc R . . H21L H 1.4204 2.2243 -0.7652 0.081 Uiso 1 1 calc R . . H21M H 1.2800 2.2876 -0.7194 0.081 Uiso 1 1 calc R . . N101 N 0.6717(7) 0.9606(6) 0.0423(3) 0.0371(15) Uani 1 1 d . . . N102 N 0.5171(7) 0.8553(5) 0.1072(3) 0.0319(14) Uani 1 1 d . . . N201 N 0.8405(8) 1.2575(6) -0.0449(3) 0.0384(15) Uani 1 1 d . . . N202 N 0.9734(7) 1.3820(6) -0.1106(3) 0.0334(14) Uani 1 1 d . . . Cu3 Cu 0.76564(13) 1.10502(10) 0.00053(5) 0.0445(3) Uani 1 1 d . . . Cu4 Cu 0.82246(14) 1.23037(11) 0.11197(6) 0.0465(3) Uani 1 1 d . . . Br1 Br 1.06581(10) 1.11889(8) 0.11211(5) 0.0474(3) Uani 1 1 d . . . Br2 Br 0.58329(10) 1.35302(7) 0.11714(5) 0.0458(2) 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 C101 0.032(4) 0.025(3) 0.040(5) -0.003(3) -0.006(3) -0.011(3) C102 0.036(4) 0.028(3) 0.038(4) 0.008(3) 0.001(3) -0.018(3) C103 0.089(7) 0.035(4) 0.030(5) 0.018(4) 0.020(5) -0.006(4) C104 0.044(5) 0.037(4) 0.029(4) 0.001(3) 0.000(4) -0.014(3) C105 0.037(4) 0.029(3) 0.025(4) -0.006(3) -0.002(3) -0.010(3) C106 0.037(5) 0.037(3) 0.033(4) -0.004(3) 0.006(3) -0.010(3) C107 0.032(4) 0.041(4) 0.029(4) 0.009(3) 0.002(3) -0.018(3) C108 0.035(4) 0.037(3) 0.037(5) -0.002(3) 0.004(4) -0.016(3) C109 0.032(4) 0.039(4) 0.039(5) -0.001(3) 0.008(4) -0.013(3) C110 0.039(5) 0.044(4) 0.028(4) -0.001(3) 0.004(3) -0.015(3) C111 0.029(4) 0.034(3) 0.030(4) 0.000(3) 0.004(3) -0.006(3) C112 0.039(5) 0.036(4) 0.037(5) -0.008(3) 0.009(4) -0.016(3) C113 0.044(5) 0.032(3) 0.036(5) 0.005(3) -0.006(4) -0.016(3) C114 0.061(6) 0.043(4) 0.037(5) 0.004(4) 0.009(4) -0.022(4) C115 0.064(6) 0.054(5) 0.048(6) 0.005(4) 0.014(5) -0.016(5) C201 0.032(4) 0.033(3) 0.050(5) 0.011(3) 0.004(4) -0.004(3) C202 0.068(6) 0.031(4) 0.063(6) 0.003(4) 0.015(5) -0.018(4) C203 0.082(7) 0.018(3) 0.057(6) 0.013(3) 0.016(5) -0.008(4) C204 0.031(4) 0.035(3) 0.039(5) 0.002(3) 0.001(3) -0.008(3) C205 0.037(4) 0.035(3) 0.028(4) 0.006(3) 0.002(3) -0.016(3) C206 0.044(5) 0.049(4) 0.028(4) 0.007(3) 0.004(4) -0.012(4) C207 0.033(4) 0.033(3) 0.039(5) 0.001(3) 0.002(3) 0.000(3) C208 0.030(4) 0.034(3) 0.035(5) -0.001(3) 0.004(3) -0.009(3) C209 0.031(4) 0.042(4) 0.030(4) 0.001(3) 0.001(3) -0.011(3) C210 0.036(4) 0.038(3) 0.034(5) 0.002(3) 0.001(4) -0.012(3) C211 0.043(5) 0.037(4) 0.032(4) 0.002(3) -0.002(4) -0.012(3) C212 0.028(4) 0.034(3) 0.041(5) 0.002(3) 0.004(3) -0.004(3) C213 0.039(5) 0.041(4) 0.032(4) 0.002(3) 0.003(4) -0.017(3) C214 0.041(5) 0.043(4) 0.043(5) -0.009(4) 0.006(4) -0.015(4) C215 0.065(7) 0.055(5) 0.040(5) 0.011(4) -0.001(5) -0.012(5) N101 0.040(4) 0.033(3) 0.038(4) 0.008(3) -0.007(3) -0.012(3) N102 0.040(4) 0.026(3) 0.036(4) 0.012(3) -0.004(3) -0.025(2) N201 0.054(4) 0.036(3) 0.029(3) 0.003(3) -0.013(3) -0.017(3) N202 0.029(3) 0.032(3) 0.039(4) 0.008(3) 0.002(3) -0.008(2) Cu3 0.0556(6) 0.0430(5) 0.0400(6) 0.0139(5) -0.0048(5) -0.0279(4) Cu4 0.0537(6) 0.0401(4) 0.0484(6) -0.0016(5) 0.0002(6) -0.0164(4) Br1 0.0519(6) 0.0359(4) 0.0545(6) 0.0026(4) 0.0026(5) -0.0117(4) Br2 0.0509(6) 0.0343(4) 0.0538(6) -0.0058(4) 0.0114(5) -0.0133(4) _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 C101 N102 1.349(7) . ? C101 N101 1.356(10) . ? C101 H101 0.9500 . ? C102 C103 1.322(10) . ? C102 N102 1.383(9) . ? C102 H102 0.9500 . ? C103 N101 1.408(10) . ? C103 H103 0.9500 . ? C104 N102 1.462(9) . ? C104 C105 1.508(10) . ? C104 H10A 0.9900 . ? C104 H10B 0.9900 . ? C105 C106 1.526(10) . ? C105 H10C 0.9900 . ? C105 H10D 0.9900 . ? C106 C107 1.498(10) . ? C106 H10E 0.9900 . ? C106 H10F 0.9900 . ? C107 C108 1.539(10) . ? C107 H10G 0.9900 . ? C107 H10H 0.9900 . ? C108 C109 1.532(11) . ? C108 H10I 0.9900 . ? C108 H10J 0.9900 . ? C109 C110 1.543(10) . ? C109 H10K 0.9900 . ? C109 H10L 0.9900 . ? C110 C111 1.501(10) . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.547(10) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 C113 1.529(11) . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 C114 1.528(11) . ? C113 H11G 0.9900 . ? C113 H11H 0.9900 . ? C114 C115 1.508(12) . ? C114 H11I 0.9900 . ? C114 H11J 0.9900 . ? C115 H11K 0.9800 . ? C115 H11L 0.9800 . ? C115 H11M 0.9800 . ? C201 N201 1.328(10) . ? C201 N202 1.355(8) . ? C201 H201 0.9500 . ? C202 C203 1.388(11) . ? C202 N201 1.389(10) . ? C202 H202 0.9500 . ? C203 N202 1.331(10) . ? C203 H203 0.9500 . ? C204 N202 1.478(9) . ? C204 C205 1.527(10) . ? C204 H20A 0.9900 . ? C204 H20B 0.9900 . ? C205 C206 1.515(10) . ? C205 H20C 0.9900 . ? C205 H20D 0.9900 . ? C206 C207 1.502(11) . ? C206 H20E 0.9900 . ? C206 H20F 0.9900 . ? C207 C208 1.517(10) . ? C207 H20G 0.9900 . ? C207 H20H 0.9900 . ? C208 C209 1.529(10) . ? C208 H20I 0.9900 . ? C208 H20J 0.9900 . ? C209 C210 1.533(10) . ? C209 H20K 0.9900 . ? C209 H20L 0.9900 . ? C210 C211 1.528(11) . ? C210 H21A 0.9900 . ? C210 H21B 0.9900 . ? C211 C212 1.532(10) . ? C211 H21C 0.9900 . ? C211 H21D 0.9900 . ? C212 C213 1.520(11) . ? C212 H21E 0.9900 . ? C212 H21F 0.9900 . ? C213 C214 1.540(10) . ? C213 H21G 0.9900 . ? C213 H21H 0.9900 . ? C214 C215 1.513(12) . ? C214 H21I 0.9900 . ? C214 H21J 0.9900 . ? C215 H21K 0.9800 . ? C215 H21L 0.9800 . ? C215 H21M 0.9800 . ? N101 Cu3 1.881(6) . ? N201 Cu3 1.882(6) . ? Cu3 Cu4 2.7838(17) . ? Cu4 Br1 2.2415(17) . ? Cu4 Br2 2.2438(17) . ? 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 N102 C101 N101 110.3(6) . . ? N102 C101 H101 124.8 . . ? N101 C101 H101 124.8 . . ? C103 C102 N102 108.3(6) . . ? C103 C102 H102 125.8 . . ? N102 C102 H102 125.8 . . ? C102 C103 N101 109.2(7) . . ? C102 C103 H103 125.4 . . ? N101 C103 H103 125.4 . . ? N102 C104 C105 113.7(6) . . ? N102 C104 H10A 108.8 . . ? C105 C104 H10A 108.8 . . ? N102 C104 H10B 108.8 . . ? C105 C104 H10B 108.8 . . ? H10A C104 H10B 107.7 . . ? C104 C105 C106 111.4(6) . . ? C104 C105 H10C 109.3 . . ? C106 C105 H10C 109.3 . . ? C104 C105 H10D 109.3 . . ? C106 C105 H10D 109.3 . . ? H10C C105 H10D 108.0 . . ? C107 C106 C105 113.5(6) . . ? C107 C106 H10E 108.9 . . ? C105 C106 H10E 108.9 . . ? C107 C106 H10F 108.9 . . ? C105 C106 H10F 108.9 . . ? H10E C106 H10F 107.7 . . ? C106 C107 C108 114.0(6) . . ? C106 C107 H10G 108.7 . . ? C108 C107 H10G 108.7 . . ? C106 C107 H10H 108.7 . . ? C108 C107 H10H 108.7 . . ? H10G C107 H10H 107.6 . . ? C109 C108 C107 113.4(6) . . ? C109 C108 H10I 108.9 . . ? C107 C108 H10I 108.9 . . ? C109 C108 H10J 108.9 . . ? C107 C108 H10J 108.9 . . ? H10I C108 H10J 107.7 . . ? C108 C109 C110 113.4(6) . . ? C108 C109 H10K 108.9 . . ? C110 C109 H10K 108.9 . . ? C108 C109 H10L 108.9 . . ? C110 C109 H10L 108.9 . . ? H10K C109 H10L 107.7 . . ? C111 C110 C109 112.4(6) . . ? C111 C110 H11A 109.1 . . ? C109 C110 H11A 109.1 . . ? C111 C110 H11B 109.1 . . ? C109 C110 H11B 109.1 . . ? H11A C110 H11B 107.9 . . ? C110 C111 C112 112.8(6) . . ? C110 C111 H11C 109.0 . . ? C112 C111 H11C 109.0 . . ? C110 C111 H11D 109.0 . . ? C112 C111 H11D 109.0 . . ? H11C C111 H11D 107.8 . . ? C113 C112 C111 113.3(7) . . ? C113 C112 H11E 108.9 . . ? C111 C112 H11E 108.9 . . ? C113 C112 H11F 108.9 . . ? C111 C112 H11F 108.9 . . ? H11E C112 H11F 107.7 . . ? C114 C113 C112 113.8(7) . . ? C114 C113 H11G 108.8 . . ? C112 C113 H11G 108.8 . . ? C114 C113 H11H 108.8 . . ? C112 C113 H11H 108.8 . . ? H11G C113 H11H 107.7 . . ? C115 C114 C113 112.4(8) . . ? C115 C114 H11I 109.1 . . ? C113 C114 H11I 109.1 . . ? C115 C114 H11J 109.1 . . ? C113 C114 H11J 109.1 . . ? H11I C114 H11J 107.9 . . ? C114 C115 H11K 109.5 . . ? C114 C115 H11L 109.5 . . ? H11K C115 H11L 109.5 . . ? C114 C115 H11M 109.5 . . ? H11K C115 H11M 109.5 . . ? H11L C115 H11M 109.5 . . ? N201 C201 N202 110.3(6) . . ? N201 C201 H201 124.8 . . ? N202 C201 H201 124.8 . . ? C203 C202 N201 107.6(8) . . ? C203 C202 H202 126.2 . . ? N201 C202 H202 126.2 . . ? N202 C203 C202 107.2(6) . . ? N202 C203 H203 126.4 . . ? C202 C203 H203 126.4 . . ? N202 C204 C205 112.6(6) . . ? N202 C204 H20A 109.1 . . ? C205 C204 H20A 109.1 . . ? N202 C204 H20B 109.1 . . ? C205 C204 H20B 109.1 . . ? H20A C204 H20B 107.8 . . ? C206 C205 C204 112.0(7) . . ? C206 C205 H20C 109.2 . . ? C204 C205 H20C 109.2 . . ? C206 C205 H20D 109.2 . . ? C204 C205 H20D 109.2 . . ? H20C C205 H20D 107.9 . . ? C207 C206 C205 113.6(7) . . ? C207 C206 H20E 108.9 . . ? C205 C206 H20E 108.9 . . ? C207 C206 H20F 108.9 . . ? C205 C206 H20F 108.9 . . ? H20E C206 H20F 107.7 . . ? C206 C207 C208 114.9(7) . . ? C206 C207 H20G 108.5 . . ? C208 C207 H20G 108.5 . . ? C206 C207 H20H 108.5 . . ? C208 C207 H20H 108.5 . . ? H20G C207 H20H 107.5 . . ? C207 C208 C209 113.5(6) . . ? C207 C208 H20I 108.9 . . ? C209 C208 H20I 108.9 . . ? C207 C208 H20J 108.9 . . ? C209 C208 H20J 108.9 . . ? H20I C208 H20J 107.7 . . ? C208 C209 C210 112.9(6) . . ? C208 C209 H20K 109.0 . . ? C210 C209 H20K 109.0 . . ? C208 C209 H20L 109.0 . . ? C210 C209 H20L 109.0 . . ? H20K C209 H20L 107.8 . . ? C211 C210 C209 112.4(6) . . ? C211 C210 H21A 109.1 . . ? C209 C210 H21A 109.1 . . ? C211 C210 H21B 109.1 . . ? C209 C210 H21B 109.1 . . ? H21A C210 H21B 107.9 . . ? C210 C211 C212 113.2(6) . . ? C210 C211 H21C 108.9 . . ? C212 C211 H21C 108.9 . . ? C210 C211 H21D 108.9 . . ? C212 C211 H21D 108.9 . . ? H21C C211 H21D 107.7 . . ? C213 C212 C211 113.4(6) . . ? C213 C212 H21E 108.9 . . ? C211 C212 H21E 108.9 . . ? C213 C212 H21F 108.9 . . ? C211 C212 H21F 108.9 . . ? H21E C212 H21F 107.7 . . ? C212 C213 C214 113.4(7) . . ? C212 C213 H21G 108.9 . . ? C214 C213 H21G 108.9 . . ? C212 C213 H21H 108.9 . . ? C214 C213 H21H 108.9 . . ? H21G C213 H21H 107.7 . . ? C215 C214 C213 112.9(7) . . ? C215 C214 H21I 109.0 . . ? C213 C214 H21I 109.0 . . ? C215 C214 H21J 109.0 . . ? C213 C214 H21J 109.0 . . ? H21I C214 H21J 107.8 . . ? C214 C215 H21K 109.5 . . ? C214 C215 H21L 109.5 . . ? H21K C215 H21L 109.5 . . ? C214 C215 H21M 109.5 . . ? H21K C215 H21M 109.5 . . ? H21L C215 H21M 109.5 . . ? C101 N101 C103 105.1(6) . . ? C101 N101 Cu3 126.0(5) . . ? C103 N101 Cu3 128.5(5) . . ? C101 N102 C102 107.0(6) . . ? C101 N102 C104 124.9(6) . . ? C102 N102 C104 128.1(5) . . ? C201 N201 C202 106.2(6) . . ? C201 N201 Cu3 127.8(5) . . ? C202 N201 Cu3 126.0(6) . . ? C203 N202 C201 108.6(6) . . ? C203 N202 C204 126.0(6) . . ? C201 N202 C204 125.3(6) . . ? N101 Cu3 N201 174.2(3) . . ? N101 Cu3 Cu4 96.5(2) . . ? N201 Cu3 Cu4 85.93(18) . . ? Br1 Cu4 Br2 175.70(6) . . ? Br1 Cu4 Cu3 92.67(6) . . ? Br2 Cu4 Cu3 91.48(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N102 C102 C103 N101 1.6(10) . . . . ? N102 C104 C105 C106 -174.9(6) . . . . ? C104 C105 C106 C107 -178.6(6) . . . . ? C105 C106 C107 C108 179.4(6) . . . . ? C106 C107 C108 C109 -179.4(6) . . . . ? C107 C108 C109 C110 -179.8(6) . . . . ? C108 C109 C110 C111 179.1(6) . . . . ? C109 C110 C111 C112 -179.8(6) . . . . ? C110 C111 C112 C113 -179.7(6) . . . . ? C111 C112 C113 C114 -179.3(6) . . . . ? C112 C113 C114 C115 -178.5(7) . . . . ? N201 C202 C203 N202 -0.6(11) . . . . ? N202 C204 C205 C206 -179.1(6) . . . . ? C204 C205 C206 C207 -177.1(6) . . . . ? C205 C206 C207 C208 -179.0(6) . . . . ? C206 C207 C208 C209 -178.9(6) . . . . ? C207 C208 C209 C210 -178.2(6) . . . . ? C208 C209 C210 C211 -179.9(6) . . . . ? C209 C210 C211 C212 179.9(6) . . . . ? C210 C211 C212 C213 179.5(6) . . . . ? C211 C212 C213 C214 -179.7(6) . . . . ? C212 C213 C214 C215 179.8(7) . . . . ? N102 C101 N101 C103 2.8(9) . . . . ? N102 C101 N101 Cu3 175.6(5) . . . . ? C102 C103 N101 C101 -2.7(10) . . . . ? C102 C103 N101 Cu3 -175.3(6) . . . . ? N101 C101 N102 C102 -1.8(8) . . . . ? N101 C101 N102 C104 178.7(7) . . . . ? C103 C102 N102 C101 0.1(9) . . . . ? C103 C102 N102 C104 179.5(8) . . . . ? C105 C104 N102 C101 -116.3(7) . . . . ? C105 C104 N102 C102 64.4(10) . . . . ? N202 C201 N201 C202 -1.5(9) . . . . ? N202 C201 N201 Cu3 178.3(5) . . . . ? C203 C202 N201 C201 1.3(11) . . . . ? C203 C202 N201 Cu3 -178.4(6) . . . . ? C202 C203 N202 C201 -0.3(11) . . . . ? C202 C203 N202 C204 -177.9(8) . . . . ? N201 C201 N202 C203 1.1(10) . . . . ? N201 C201 N202 C204 178.8(7) . . . . ? C205 C204 N202 C203 -51.9(11) . . . . ? C205 C204 N202 C201 130.9(8) . . . . ? C101 N101 Cu3 N201 -71(3) . . . . ? C103 N101 Cu3 N201 100(3) . . . . ? C101 N101 Cu3 Cu4 42.6(6) . . . . ? C103 N101 Cu3 Cu4 -146.3(7) . . . . ? C201 N201 Cu3 N101 -124(3) . . . . ? C202 N201 Cu3 N101 55(3) . . . . ? C201 N201 Cu3 Cu4 121.0(7) . . . . ? C202 N201 Cu3 Cu4 -59.3(7) . . . . ? N101 Cu3 Cu4 Br1 100.8(2) . . . . ? N201 Cu3 Cu4 Br1 -84.5(2) . . . . ? N101 Cu3 Cu4 Br2 -80.3(2) . . . . ? N201 Cu3 Cu4 Br2 94.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 1.368 _refine_diff_density_min -1.396 _refine_diff_density_rms 0.172 #===END