# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_d:\cage\a _database_code_depnum_ccdc_archive 'CCDC 764790' #TrackingRef '764790.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H108 Cl6 Cu3 N24 O55 P4' _chemical_formula_weight 2572.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' 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 monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.419(6) _cell_length_b 22.7212(5) _cell_length_c 32.410(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.7120(10) _cell_angle_gamma 90.00 _cell_volume 23443(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 19695 _cell_measurement_theta_min 3.0278 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour Blue _exptl_crystal_size_max 0.4500 _exptl_crystal_size_mid 0.4000 _exptl_crystal_size_min 0.3500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10600 _exptl_absorpt_coefficient_mu 0.828 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8161 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _exptl_special_details ; ? ; _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_type 'Smart CCD' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 73699 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.00 _reflns_number_total 20557 _reflns_number_gt 12499 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 2000)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.2000P)^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 20557 _refine_ls_number_parameters 1360 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.1176 _refine_ls_R_factor_gt 0.0877 _refine_ls_wR_factor_ref 0.3022 _refine_ls_wR_factor_gt 0.2534 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.04382(2) 0.04418(3) 0.39450(2) 0.0407(2) Uani 1 1 d . . . Cu2 Cu 0.04797(2) 0.44434(3) 0.39665(2) 0.0428(2) Uani 1 1 d . . . Cu3 Cu 0.18748(2) 0.24669(3) 0.24122(2) 0.0451(2) Uani 1 1 d . . . P1 P 0.15373(5) 0.24230(6) 0.40596(5) 0.0400(3) Uani 1 1 d . . . P3 P 0.10697(5) 0.02393(7) 0.24837(5) 0.0424(3) Uani 1 1 d . . . P2 P -0.05121(5) 0.24546(6) 0.41860(5) 0.0423(4) Uani 1 1 d . . . P4 P 0.10449(5) 0.46729(7) 0.24507(5) 0.0443(4) Uani 1 1 d . . . N1 N 0.18017(14) 0.1797(2) 0.41226(15) 0.0452(11) Uani 1 1 d . . . H1 H 0.2072 0.1824 0.4154 0.054 Uiso 1 1 calc R . . O4 O 0.11593(13) 0.24225(18) 0.36808(13) 0.0498(10) Uani 1 1 d . . . N13 N 0.11715(15) 0.0141(2) 0.20210(15) 0.0511(12) Uani 1 1 d . . . H31 H 0.1436 0.0082 0.2038 0.061 Uiso 1 1 calc R . . N12 N -0.00644(15) 0.4310(2) 0.41162(15) 0.0443(11) Uani 1 1 d . . . N10 N 0.04520(14) 0.1005(2) 0.44336(14) 0.0420(10) Uani 1 1 d . . . N4 N 0.10675(15) 0.05604(19) 0.40659(15) 0.0433(11) Uani 1 1 d . . . N23 N 0.10336(15) 0.4596(2) 0.38388(15) 0.0459(11) Uani 1 1 d . . . N17 N 0.04474(15) -0.0194(2) 0.34997(15) 0.0458(11) Uani 1 1 d . . . N21 N 0.07694(15) 0.5287(2) 0.23799(16) 0.0485(12) Uani 1 1 d . . . H56 H 0.0877 0.5580 0.2556 0.058 Uiso 1 1 calc R . . O6 O 0.08052(13) 0.07558(18) 0.24844(13) 0.0511(10) Uani 1 1 d . . . O5 O -0.03890(15) 0.24609(17) 0.37883(13) 0.0509(10) Uani 1 1 d . . . O7 O 0.07958(13) 0.41418(18) 0.24549(13) 0.0531(10) Uani 1 1 d . . . N18 N 0.20123(15) 0.1705(2) 0.27655(15) 0.0476(11) Uani 1 1 d . . . N7 N -0.08634(16) 0.1952(2) 0.41870(15) 0.0502(12) Uani 1 1 d . . . H16 H -0.0813 0.1739 0.4424 0.060 Uiso 1 1 calc R . . C29 C 0.07474(18) 0.0964(3) 0.48209(18) 0.0473(13) Uani 1 1 d . . . H29 H 0.0942 0.0648 0.4872 0.057 Uiso 1 1 calc R . . N24 N -0.01961(15) 0.5076(2) 0.14674(15) 0.0451(11) Uani 1 1 d . . . C11 C 0.20276(17) 0.3082(2) 0.36969(17) 0.0417(12) Uani 1 1 d . . . N14 N 0.08560(16) -0.0379(2) 0.25722(16) 0.0510(12) Uani 1 1 d . . . H36 H 0.0864 -0.0674 0.2398 0.061 Uiso 1 1 calc R . . N5 N 0.07707(15) 0.3833(2) 0.44251(14) 0.0463(11) Uani 1 1 d . . . C36 C 0.06622(18) -0.0495(2) 0.28925(18) 0.0446(13) Uani 1 1 d . . . N2 N 0.14393(16) 0.25229(18) 0.45205(15) 0.0427(11) Uani 1 1 d . . . H6 H 0.1552 0.2269 0.4728 0.051 Uiso 1 1 calc R . . N3 N 0.18741(15) 0.2938(2) 0.40418(14) 0.0439(11) Uani 1 1 d . . . H11 H 0.1971 0.3150 0.4278 0.053 Uiso 1 1 calc R . . N11 N -0.17139(16) 0.2003(2) 0.31528(15) 0.0491(12) Uani 1 1 d . . . N15 N 0.15313(16) 0.0276(2) 0.28558(16) 0.0505(12) Uani 1 1 d . . . H41 H 0.1607 -0.0034 0.3025 0.061 Uiso 1 1 calc R . . C26 C 0.01790(17) 0.1858(2) 0.46867(17) 0.0428(12) Uani 1 1 d . . . N8 N -0.07190(16) 0.3075(2) 0.42791(17) 0.0528(12) Uani 1 1 d . . . H21 H -0.0950 0.3045 0.4355 0.063 Uiso 1 1 calc R . . N9 N -0.01201(16) 0.2321(2) 0.46216(16) 0.0498(12) Uani 1 1 d . . . H26 H -0.0091 0.2563 0.4841 0.060 Uiso 1 1 calc R . . C56 C 0.03800(19) 0.5391(3) 0.20669(18) 0.0469(13) Uani 1 1 d . . . C31 C 0.08789(18) 0.0142(3) 0.16008(18) 0.0450(13) Uani 1 1 d . . . N16 N 0.01822(15) 0.0267(2) 0.11316(15) 0.0466(11) Uani 1 1 d . . . C40 C 0.06390(18) -0.0081(2) 0.31991(18) 0.0458(13) Uani 1 1 d . . . H40 H 0.0763 0.0295 0.3196 0.055 Uiso 1 1 calc R . . C30 C 0.01729(17) 0.1441(2) 0.43747(17) 0.0436(12) Uani 1 1 d . . . H30 H -0.0041 0.1465 0.4104 0.052 Uiso 1 1 calc R . . C5 C 0.12201(17) 0.1116(2) 0.40594(17) 0.0419(12) Uani 1 1 d . . . H5 H 0.1029 0.1437 0.4003 0.050 Uiso 1 1 calc R . . C15 C 0.19073(19) 0.2790(3) 0.33069(18) 0.0461(13) Uani 1 1 d . . . H15 H 0.1710 0.2478 0.3267 0.055 Uiso 1 1 calc R . . C51 C 0.14155(18) 0.4741(3) 0.33297(18) 0.0455(13) Uani 1 1 d . . . C6 C 0.11916(17) 0.2977(2) 0.46191(17) 0.0422(12) Uani 1 1 d . . . N6 N 0.20583(16) 0.2927(2) 0.29804(14) 0.0471(11) Uani 1 1 d . . . N19 N 0.12647(17) 0.4673(2) 0.20590(16) 0.0525(12) Uani 1 1 d . . . H46 H 0.1236 0.4994 0.1901 0.063 Uiso 1 1 calc R . . N22 N 0.17862(16) 0.3233(2) 0.20691(15) 0.0494(12) Uani 1 1 d . . . C45 C 0.17435(19) 0.1256(3) 0.26978(18) 0.0480(14) Uani 1 1 d . . . H45 H 0.1485 0.1292 0.2472 0.058 Uiso 1 1 calc R . . C1 C 0.16424(17) 0.1229(2) 0.41318(16) 0.0405(12) Uani 1 1 d . . . C46 C 0.14964(18) 0.4203(3) 0.19527(18) 0.0470(13) Uani 1 1 d . . . C41 C 0.18174(18) 0.0745(3) 0.29336(17) 0.0439(13) Uani 1 1 d . . . O1 O 0.02711(16) 0.1154(2) 0.34325(15) 0.0668(12) Uani 1 1 d . . . C35 C 0.04562(17) 0.0256(3) 0.15308(18) 0.0456(13) Uani 1 1 d . . . H35 H 0.0358 0.0329 0.1772 0.055 Uiso 1 1 calc R . . N20 N 0.14334(16) 0.4766(2) 0.28989(16) 0.0512(12) Uani 1 1 d . . . H51 H 0.1681 0.4840 0.2868 0.061 Uiso 1 1 calc R . . O3 O 0.11884(17) 0.2461(2) 0.24195(19) 0.0728(14) Uani 1 1 d . . . C12 C 0.2323(2) 0.3539(3) 0.37543(19) 0.0514(14) Uani 1 1 d . . . H12 H 0.2413 0.3753 0.4018 0.062 Uiso 1 1 calc R . . C55 C 0.10479(18) 0.4617(3) 0.34295(18) 0.0468(13) Uani 1 1 d . . . H55 H 0.0798 0.4546 0.3199 0.056 Uiso 1 1 calc R . . C50 C 0.15654(19) 0.3682(3) 0.21695(18) 0.0468(13) Uani 1 1 d . . . H50 H 0.1453 0.3629 0.2403 0.056 Uiso 1 1 calc R . . C59 C -0.0384(2) 0.5596(3) 0.1467(2) 0.0515(14) Uani 1 1 d . . . H59 H -0.0651 0.5667 0.1262 0.062 Uiso 1 1 calc R . . C42 C 0.2191(2) 0.0701(3) 0.3259(2) 0.0636(17) Uani 1 1 d . . . H42 H 0.2255 0.0356 0.3433 0.076 Uiso 1 1 calc R . . C10 C 0.10003(18) 0.3397(2) 0.43270(18) 0.0458(13) Uani 1 1 d . . . H10 H 0.1029 0.3383 0.4044 0.055 Uiso 1 1 calc R . . C52 C 0.17814(19) 0.4840(3) 0.3669(2) 0.0573(16) Uani 1 1 d . . . H52 H 0.2038 0.4927 0.3612 0.069 Uiso 1 1 calc R . . C20 C -0.13654(18) 0.2132(3) 0.34655(18) 0.0467(13) Uani 1 1 d . . . H20 H -0.1196 0.2450 0.3425 0.056 Uiso 1 1 calc R . . C7 C 0.1158(2) 0.3002(3) 0.50358(19) 0.0527(15) Uani 1 1 d . . . H7 H 0.1292 0.2715 0.5245 0.063 Uiso 1 1 calc R . . C25 C -0.02039(18) 0.3764(3) 0.41447(18) 0.0471(13) Uani 1 1 d . . . H25 H -0.0047 0.3441 0.4090 0.056 Uiso 1 1 calc R . . C2 C 0.19169(19) 0.0751(3) 0.4220(2) 0.0522(14) Uani 1 1 d . . . H2 H 0.2210 0.0808 0.4271 0.063 Uiso 1 1 calc R . . C4 C 0.13400(19) 0.0114(3) 0.4151(2) 0.0508(14) Uani 1 1 d . . . H4 H 0.1238 -0.0276 0.4156 0.061 Uiso 1 1 calc R . . C54 C 0.13917(19) 0.4682(3) 0.41603(19) 0.0492(14) Uani 1 1 d . . . H54 H 0.1387 0.4653 0.4451 0.059 Uiso 1 1 calc R . . C9 C 0.0735(2) 0.3867(3) 0.48212(19) 0.0553(15) Uani 1 1 d . . . H9 H 0.0579 0.4179 0.4892 0.066 Uiso 1 1 calc R . . C60 C 0.01768(18) 0.4975(3) 0.17587(18) 0.0465(13) Uani 1 1 d . . . H60 H 0.0309 0.4605 0.1756 0.056 Uiso 1 1 calc R . . C37 C 0.0478(2) -0.1039(3) 0.2897(2) 0.0600(16) Uani 1 1 d . . . H37 H 0.0489 -0.1335 0.2693 0.072 Uiso 1 1 calc R . . O2 O 0.02981(17) 0.3716(2) 0.34331(16) 0.0751(14) Uani 1 1 d . . . C32 C 0.1025(2) 0.0030(3) 0.1254(2) 0.0580(16) Uani 1 1 d . . . H32 H 0.1314 -0.0047 0.1295 0.070 Uiso 1 1 calc R . . C23 C -0.0647(2) 0.4685(3) 0.4305(2) 0.0629(18) Uani 1 1 d . . . H23 H -0.0798 0.5015 0.4360 0.075 Uiso 1 1 calc R . . C39 C 0.0272(2) -0.0712(3) 0.35021(19) 0.0528(15) Uani 1 1 d . . . H39 H 0.0139 -0.0792 0.3716 0.063 Uiso 1 1 calc R . . C16 C -0.12378(18) 0.1818(2) 0.38537(17) 0.0439(13) Uani 1 1 d . . . C21 C -0.05718(18) 0.3651(2) 0.42526(17) 0.0444(13) Uani 1 1 d . . . C22 C -0.0793(2) 0.4127(3) 0.4329(2) 0.0566(16) Uani 1 1 d . . . H22 H -0.1047 0.4069 0.4399 0.068 Uiso 1 1 calc R . . C58 C -0.0195(2) 0.6030(3) 0.1760(2) 0.0625(17) Uani 1 1 d . . . H58 H -0.0330 0.6399 0.1753 0.075 Uiso 1 1 calc R . . O40 O 0.06985(18) 0.5223(2) 0.45685(16) 0.0771(14) Uani 1 1 d . . . C17 C -0.1496(2) 0.1365(3) 0.3914(2) 0.0594(16) Uani 1 1 d . . . H17 H -0.1426 0.1153 0.4179 0.071 Uiso 1 1 calc R . . C57 C 0.0187(2) 0.5927(3) 0.2063(2) 0.0560(15) Uani 1 1 d . . . H57 H 0.0317 0.6223 0.2267 0.067 Uiso 1 1 calc R . . C38 C 0.0276(3) -0.1142(3) 0.3205(2) 0.0661(19) Uani 1 1 d . . . H38 H 0.0141 -0.1509 0.3211 0.079 Uiso 1 1 calc R . . C24 C -0.0280(2) 0.4768(3) 0.4200(2) 0.0555(15) Uani 1 1 d . . . H24 H -0.0179 0.5156 0.4188 0.067 Uiso 1 1 calc R . . C33 C 0.0732(2) 0.0035(3) 0.0842(2) 0.0656(19) Uani 1 1 d . . . H33 H 0.0820 -0.0049 0.0595 0.079 Uiso 1 1 calc R . . C18 C -0.1848(2) 0.1233(3) 0.3586(2) 0.069(2) Uani 1 1 d . . . H18 H -0.2017 0.0909 0.3614 0.083 Uiso 1 1 calc R . . C44 C 0.2377(2) 0.1642(3) 0.3075(2) 0.0561(15) Uani 1 1 d . . . H44 H 0.2579 0.1948 0.3119 0.067 Uiso 1 1 calc R . . C49 C 0.1946(2) 0.3321(3) 0.1739(2) 0.0568(16) Uani 1 1 d . . . H49 H 0.2103 0.3015 0.1663 0.068 Uiso 1 1 calc R . . C14 C 0.2338(2) 0.3366(3) 0.3036(2) 0.0558(16) Uani 1 1 d . . . H14 H 0.2443 0.3471 0.2805 0.067 Uiso 1 1 calc R . . C8 C 0.0928(2) 0.3442(3) 0.5139(2) 0.0597(17) Uani 1 1 d . . . H8 H 0.0899 0.3464 0.5421 0.072 Uiso 1 1 calc R . . C43 C 0.2472(2) 0.1156(3) 0.3330(2) 0.0640(18) Uani 1 1 d . . . H43 H 0.2731 0.1133 0.3556 0.077 Uiso 1 1 calc R . . C27 C 0.04946(19) 0.1814(3) 0.50811(18) 0.0504(14) Uani 1 1 d . . . H27 H 0.0514 0.2093 0.5305 0.060 Uiso 1 1 calc R . . C13 C 0.2477(2) 0.3666(3) 0.3421(2) 0.0620(18) Uani 1 1 d . . . H13 H 0.2683 0.3965 0.3455 0.074 Uiso 1 1 calc R . . C28 C 0.0776(2) 0.1361(3) 0.51414(19) 0.0541(15) Uani 1 1 d . . . H28 H 0.0993 0.1325 0.5409 0.065 Uiso 1 1 calc R . . C34 C 0.0318(2) 0.0161(3) 0.0793(2) 0.0561(15) Uani 1 1 d . . . H34 H 0.0123 0.0173 0.0510 0.067 Uiso 1 1 calc R . . C47 C 0.1665(2) 0.4286(3) 0.1618(2) 0.0623(17) Uani 1 1 d . . . H47 H 0.1628 0.4647 0.1463 0.075 Uiso 1 1 calc R . . C19 C -0.1961(2) 0.1563(3) 0.3214(2) 0.0575(16) Uani 1 1 d . . . H19 H -0.2218 0.1481 0.2996 0.069 Uiso 1 1 calc R . . C3 C 0.1758(2) 0.0199(3) 0.4230(2) 0.0650(18) Uani 1 1 d . . . H3 H 0.1943 -0.0130 0.4294 0.078 Uiso 1 1 calc R . . C53 C 0.1765(2) 0.4811(3) 0.4084(2) 0.0615(17) Uani 1 1 d . . . H53 H 0.2011 0.4879 0.4320 0.074 Uiso 1 1 calc R . . C48 C 0.1891(3) 0.3829(3) 0.1514(2) 0.0678(19) Uani 1 1 d . . . H48 H 0.2008 0.3873 0.1283 0.081 Uiso 1 1 calc R . . Cl1 Cl 0.30998(6) 0.47552(9) 0.44263(7) 0.0748(5) Uani 1 1 d D . . Cl2 Cl 0.05625(8) -0.09965(9) 0.47074(6) 0.0860(7) Uani 1 1 d D . . Cl3 Cl 0.31530(7) 0.02367(12) 0.44616(7) 0.0894(7) Uani 1 1 d D . . Cl6 Cl 0.24648(12) 0.0012(2) 0.23043(12) 0.1520(15) Uani 1 1 d D . . O44 O 0.2673(2) 0.2472(3) 0.2394(2) 0.106(2) Uani 1 1 d . . . O38 O 0.22788(19) 0.3555(2) 0.48619(16) 0.0848(16) Uani 1 1 d . . . O37 O 0.19614(19) 0.1847(3) 0.52483(18) 0.0880(16) Uani 1 1 d . . . O36 O 0.27230(17) 0.2022(3) 0.43796(19) 0.0879(16) Uani 1 1 d . . . O49 O 0.0000 0.2444(4) 0.2500 0.111(3) Uani 1 2 d S . . O9 O 0.2822(3) 0.4571(4) 0.4641(3) 0.137(3) Uani 1 1 d D . . O33 O 0.0935(3) -0.1369(4) 0.2062(3) 0.163(4) Uani 1 1 d . . . O11 O 0.3290(3) 0.4220(4) 0.4336(4) 0.155(3) Uani 1 1 d D . . O54 O 0.1171(3) 0.6284(4) 0.2880(4) 0.172(4) Uani 1 1 d . . . O24 O 0.0093(3) 0.2930(4) 0.5463(3) 0.173(4) Uani 1 1 d D . . O34 O 0.1861(4) -0.0816(4) 0.3313(4) 0.213(5) Uani 1 1 d . . . O10 O 0.3418(3) 0.5136(5) 0.4643(3) 0.168(4) Uani 1 1 d D . . O8 O 0.2874(3) 0.4979(4) 0.4021(3) 0.161(4) Uani 1 1 d D . . O16 O 0.3516(3) -0.0027(6) 0.4645(4) 0.210(6) Uani 1 1 d D . . O17 O 0.2875(3) -0.0055(5) 0.4138(3) 0.179(4) Uani 1 1 d D . . O41 O -0.1411(4) 0.3025(5) 0.4625(4) 0.204(5) Uani 1 1 d . . . O47 O 0.0000 0.0971(11) 0.2500 0.219(9) Uani 1 2 d S . . O42 O 0.0302(4) 0.2436(6) 0.3516(6) 0.238(7) Uani 1 1 d . . . O55 O 0.1253(4) 0.5756(4) 0.1576(4) 0.196(5) Uani 1 1 d . . . Cl4 Cl 0.34969(9) 0.24811(14) 0.37348(8) 0.1054(9) Uani 1 1 d D . . Cl5 Cl -0.00371(11) 0.34300(14) 0.56048(9) 0.1219(11) Uani 1 1 d D . . O20 O 0.3909(3) 0.2457(5) 0.3927(4) 0.193(6) Uani 1 1 d D . . O21 O 0.3366(5) 0.2581(5) 0.3313(3) 0.201(6) Uani 1 1 d D . . O19 O 0.2995(4) 0.0372(7) 0.4778(3) 0.231(7) Uani 1 1 d D . . O46 O 0.0825(5) 0.3178(6) 0.2977(4) 0.217(6) Uani 1 1 d . . . O35 O 0.3154(5) 0.1363(8) 0.2605(5) 0.269(8) Uani 1 1 d . . . O57 O 0.0485(5) -0.1624(6) 0.1200(3) 0.226(6) Uani 1 1 d . . . O22 O 0.3315(4) 0.1990(5) 0.3844(4) 0.200(5) Uani 1 1 d D . . O53 O 0.0000 0.3910(13) 0.2500 0.257(11) Uani 1 2 d S . . O43 O 0.0818(5) 0.1733(6) 0.2979(4) 0.221(6) Uani 1 1 d . . . O27 O 0.0261(5) 0.3692(6) 0.5946(4) 0.265(8) Uani 1 1 d D . . O52 O 0.0488(5) 0.3185(7) 0.1914(5) 0.309(11) Uani 1 1 d . . . O30 O 0.2726(3) 0.0008(9) 0.2083(4) 0.298(10) Uani 1 1 d D . . O26 O -0.0061(7) 0.3887(7) 0.5293(4) 0.302(10) Uani 1 1 d D . . O25 O -0.0403(4) 0.3479(7) 0.5657(6) 0.280(9) Uani 1 1 d D . . O50 O 0.0581(5) 0.1631(7) 0.1872(5) 0.281(9) Uani 1 1 d . . . O48 O 0.2838(7) 0.2418(8) 0.1610(6) 0.279(9) Uani 1 1 d . . . O23 O 0.3360(6) 0.2851(7) 0.3991(5) 0.254(8) Uani 1 1 d D . . O45 O 0.3097(5) 0.3594(9) 0.2495(7) 0.300(9) Uani 1 1 d . . . O31 O 0.2437(7) 0.0528(5) 0.2437(6) 0.349(13) Uani 1 1 d D . . O18 O 0.3228(6) 0.0681(8) 0.4235(6) 0.372(15) Uani 1 1 d D . . O39 O 0.1387(6) 0.6104(10) 0.4708(8) 0.361(13) Uani 1 1 d . . . O32 O 0.0000 -0.2532(9) 0.2500 0.37(2) Uani 1 2 d S . . O29 O 0.2535(5) -0.0305(10) 0.2668(5) 0.364(14) Uani 1 1 d D . . O14 O 0.0253(3) -0.1375(4) 0.4417(2) 0.187(5) Uani 1 1 d D . . O12 O 0.0302(3) -0.0758(6) 0.4952(4) 0.369(14) Uani 1 1 d D . . O15 O 0.0642(2) -0.04168(17) 0.4564(2) 0.104(2) Uani 1 1 d D . . O13A O 0.0865(2) -0.1147(8) 0.5119(2) 0.159(6) Uani 0.79(4) 1 d PD . . O13B O 0.0811(12) -0.140(2) 0.5030(9) 0.159(6) Uani 0.21(4) 1 d PD . . O28 O 0.2049(4) -0.0070(5) 0.2050(4) 0.186(4) Uiso 1 1 d D . . O56 O -0.1339(12) 0.6553(16) 0.1263(12) 0.518(19) Uiso 1 1 d . . . O51 O 0.2294(13) 0.2678(14) 0.0848(13) 0.49(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0371(4) 0.0463(4) 0.0385(4) -0.0007(3) 0.0111(3) -0.0003(3) Cu2 0.0381(4) 0.0478(4) 0.0420(4) 0.0027(3) 0.0117(3) 0.0036(3) Cu3 0.0468(5) 0.0517(4) 0.0353(4) -0.0053(3) 0.0105(3) -0.0028(3) P1 0.0354(8) 0.0459(8) 0.0368(8) -0.0007(6) 0.0082(6) 0.0009(6) P3 0.0372(8) 0.0483(8) 0.0423(8) -0.0015(6) 0.0132(6) 0.0031(6) P2 0.0416(9) 0.0482(8) 0.0367(8) 0.0024(6) 0.0114(6) 0.0020(6) P4 0.0409(8) 0.0485(8) 0.0435(8) -0.0020(6) 0.0128(7) -0.0047(6) N1 0.033(3) 0.045(3) 0.057(3) -0.005(2) 0.012(2) 0.0023(19) O4 0.038(2) 0.066(3) 0.040(2) -0.0023(17) 0.0027(18) 0.0018(18) N13 0.035(3) 0.074(3) 0.041(3) 0.004(2) 0.007(2) 0.010(2) N12 0.041(3) 0.042(3) 0.050(3) 0.004(2) 0.015(2) 0.008(2) N10 0.038(3) 0.047(3) 0.038(2) 0.003(2) 0.009(2) 0.001(2) N4 0.044(3) 0.043(3) 0.042(2) 0.000(2) 0.012(2) 0.001(2) N23 0.043(3) 0.048(3) 0.045(3) 0.000(2) 0.010(2) 0.002(2) N17 0.046(3) 0.048(3) 0.043(3) 0.002(2) 0.014(2) -0.002(2) N21 0.040(3) 0.044(3) 0.053(3) -0.011(2) 0.002(2) -0.004(2) O6 0.045(2) 0.054(2) 0.056(2) -0.0042(19) 0.0167(19) 0.0067(18) O5 0.058(3) 0.060(3) 0.038(2) 0.0037(17) 0.019(2) 0.0055(19) O7 0.049(2) 0.053(2) 0.056(2) -0.0045(19) 0.014(2) -0.0118(19) N18 0.041(3) 0.054(3) 0.045(3) -0.007(2) 0.009(2) -0.002(2) N7 0.055(3) 0.057(3) 0.034(2) 0.014(2) 0.006(2) -0.003(2) C29 0.038(3) 0.054(3) 0.045(3) 0.006(3) 0.006(3) 0.002(2) N24 0.043(3) 0.046(3) 0.045(3) 0.001(2) 0.011(2) -0.006(2) C11 0.044(3) 0.041(3) 0.037(3) 0.000(2) 0.008(2) -0.003(2) N14 0.057(3) 0.048(3) 0.055(3) -0.015(2) 0.026(3) -0.005(2) N5 0.042(3) 0.056(3) 0.040(2) 0.001(2) 0.012(2) 0.004(2) C36 0.045(3) 0.045(3) 0.045(3) -0.005(2) 0.016(3) -0.001(2) N2 0.043(3) 0.047(3) 0.038(3) 0.0093(19) 0.012(2) 0.0100(19) N3 0.045(3) 0.050(3) 0.036(2) -0.008(2) 0.010(2) -0.008(2) N11 0.050(3) 0.053(3) 0.041(3) 0.007(2) 0.009(2) -0.006(2) N15 0.050(3) 0.050(3) 0.046(3) 0.003(2) 0.007(2) 0.002(2) C26 0.039(3) 0.048(3) 0.039(3) -0.002(2) 0.008(2) 0.001(2) N8 0.050(3) 0.048(3) 0.069(3) 0.002(2) 0.032(3) 0.005(2) N9 0.046(3) 0.055(3) 0.044(3) -0.008(2) 0.007(2) 0.005(2) C56 0.047(3) 0.048(3) 0.047(3) -0.002(3) 0.017(3) -0.003(3) C31 0.041(3) 0.053(3) 0.042(3) -0.001(2) 0.015(2) 0.000(2) N16 0.041(3) 0.060(3) 0.041(3) -0.006(2) 0.016(2) 0.001(2) C40 0.043(3) 0.047(3) 0.048(3) -0.002(3) 0.015(3) -0.004(2) C30 0.039(3) 0.050(3) 0.037(3) -0.001(2) 0.005(2) -0.001(2) C5 0.039(3) 0.039(3) 0.047(3) 0.001(2) 0.012(2) 0.004(2) C15 0.050(3) 0.042(3) 0.047(3) -0.005(3) 0.017(3) -0.008(3) C51 0.035(3) 0.055(3) 0.044(3) 0.001(3) 0.008(2) 0.000(2) C6 0.032(3) 0.052(3) 0.040(3) 0.001(2) 0.007(2) 0.001(2) N6 0.051(3) 0.051(3) 0.038(2) -0.004(2) 0.012(2) -0.009(2) N19 0.063(3) 0.051(3) 0.048(3) 0.004(2) 0.023(3) 0.001(2) N22 0.053(3) 0.055(3) 0.043(3) -0.005(2) 0.019(2) -0.001(2) C45 0.045(3) 0.058(4) 0.039(3) -0.005(3) 0.009(3) 0.000(3) C1 0.038(3) 0.046(3) 0.038(3) -0.002(2) 0.011(2) 0.000(2) C46 0.045(3) 0.053(3) 0.042(3) -0.003(3) 0.012(3) -0.005(3) C41 0.040(3) 0.051(3) 0.039(3) -0.002(2) 0.009(2) 0.003(2) O1 0.067(3) 0.070(3) 0.059(3) 0.014(2) 0.013(2) 0.002(2) C35 0.037(3) 0.057(3) 0.041(3) -0.003(3) 0.009(2) 0.001(2) N20 0.038(3) 0.070(3) 0.048(3) -0.005(2) 0.016(2) -0.008(2) O3 0.054(3) 0.088(4) 0.079(4) -0.011(2) 0.024(3) -0.005(2) C12 0.054(4) 0.050(3) 0.044(3) -0.005(3) 0.006(3) -0.011(3) C55 0.041(3) 0.059(4) 0.039(3) 0.001(3) 0.011(2) -0.001(3) C50 0.052(4) 0.051(3) 0.040(3) -0.001(2) 0.018(3) 0.001(3) C59 0.047(4) 0.054(4) 0.051(3) 0.007(3) 0.011(3) 0.007(3) C42 0.056(4) 0.073(5) 0.056(4) 0.013(3) 0.009(3) 0.004(3) C10 0.047(3) 0.053(3) 0.039(3) 0.004(3) 0.014(3) 0.006(3) C52 0.034(3) 0.077(4) 0.056(4) -0.003(3) 0.007(3) -0.005(3) C20 0.044(3) 0.048(3) 0.045(3) 0.008(3) 0.010(3) -0.004(2) C7 0.057(4) 0.061(4) 0.042(3) 0.006(3) 0.017(3) 0.002(3) C25 0.044(3) 0.050(3) 0.050(3) 0.002(3) 0.019(3) 0.007(3) C2 0.040(3) 0.053(4) 0.059(4) -0.001(3) 0.009(3) 0.000(3) C4 0.043(3) 0.049(3) 0.059(4) 0.003(3) 0.013(3) 0.001(3) C54 0.042(3) 0.064(4) 0.039(3) -0.001(3) 0.008(3) 0.001(3) C9 0.061(4) 0.065(4) 0.042(3) -0.001(3) 0.020(3) 0.011(3) C60 0.042(3) 0.044(3) 0.049(3) -0.001(3) 0.009(3) 0.005(2) C37 0.073(5) 0.045(3) 0.063(4) -0.004(3) 0.023(4) -0.005(3) O2 0.084(4) 0.072(3) 0.062(3) -0.014(2) 0.012(3) 0.003(3) C32 0.043(4) 0.085(5) 0.050(3) 0.001(3) 0.018(3) 0.010(3) C23 0.069(5) 0.056(4) 0.076(5) -0.001(3) 0.041(4) 0.016(3) C39 0.066(4) 0.052(4) 0.045(3) 0.002(3) 0.024(3) -0.006(3) C16 0.046(3) 0.051(3) 0.034(3) 0.005(2) 0.012(2) 0.000(2) C21 0.043(3) 0.049(3) 0.043(3) 0.002(2) 0.014(2) 0.002(2) C22 0.051(4) 0.063(4) 0.060(4) 0.000(3) 0.024(3) 0.012(3) C58 0.078(5) 0.043(3) 0.065(4) -0.002(3) 0.020(4) 0.007(3) O40 0.084(4) 0.073(3) 0.072(3) -0.012(3) 0.020(3) 0.010(3) C17 0.067(4) 0.062(4) 0.045(3) 0.013(3) 0.010(3) -0.007(3) C57 0.061(4) 0.042(3) 0.063(4) -0.007(3) 0.016(3) -0.006(3) C38 0.093(6) 0.044(3) 0.066(4) -0.001(3) 0.031(4) -0.018(3) C24 0.063(4) 0.050(3) 0.058(4) -0.001(3) 0.024(3) 0.006(3) C33 0.054(4) 0.102(6) 0.046(3) -0.009(3) 0.024(3) 0.009(4) C18 0.067(5) 0.077(5) 0.062(4) 0.017(4) 0.020(4) -0.027(4) C44 0.043(4) 0.067(4) 0.050(3) -0.009(3) 0.000(3) -0.006(3) C49 0.062(4) 0.066(4) 0.050(3) -0.003(3) 0.027(3) 0.006(3) C14 0.059(4) 0.065(4) 0.045(3) 0.000(3) 0.018(3) -0.017(3) C8 0.063(4) 0.077(4) 0.040(3) 0.004(3) 0.017(3) 0.014(3) C43 0.047(4) 0.081(5) 0.048(4) 0.004(3) -0.009(3) 0.003(3) C27 0.049(4) 0.059(4) 0.039(3) -0.004(3) 0.008(3) 0.003(3) C13 0.064(4) 0.073(4) 0.050(4) -0.007(3) 0.019(3) -0.029(3) C28 0.048(4) 0.069(4) 0.038(3) 0.003(3) 0.002(3) 0.006(3) C34 0.051(4) 0.074(4) 0.042(3) -0.002(3) 0.012(3) 0.005(3) C47 0.075(5) 0.062(4) 0.057(4) 0.009(3) 0.030(4) -0.002(3) C19 0.049(4) 0.069(4) 0.051(3) 0.007(3) 0.009(3) -0.013(3) C3 0.053(4) 0.053(4) 0.082(5) 0.008(3) 0.010(4) 0.016(3) C53 0.044(4) 0.083(5) 0.050(4) -0.007(3) 0.004(3) -0.002(3) C48 0.086(5) 0.074(5) 0.058(4) 0.009(3) 0.042(4) 0.000(4) Cl1 0.0502(10) 0.0839(13) 0.0799(12) 0.0148(10) 0.0044(9) -0.0198(9) Cl2 0.1130(18) 0.0763(13) 0.0558(10) 0.0154(9) 0.0065(11) -0.0184(11) Cl3 0.0733(14) 0.1086(17) 0.0742(13) -0.0202(12) 0.0043(11) 0.0279(12) Cl6 0.115(3) 0.196(4) 0.135(3) -0.022(2) 0.023(2) 0.076(3) O44 0.092(5) 0.125(6) 0.097(5) -0.002(3) 0.023(4) -0.004(4) O38 0.100(4) 0.082(4) 0.064(3) -0.016(3) 0.013(3) -0.009(3) O37 0.087(4) 0.089(4) 0.077(3) 0.030(3) 0.010(3) 0.019(3) O36 0.059(3) 0.111(4) 0.090(4) 0.008(3) 0.018(3) -0.002(3) O49 0.099(8) 0.126(8) 0.103(7) 0.000 0.023(6) 0.000 O9 0.155(8) 0.143(7) 0.130(6) -0.003(5) 0.067(6) -0.044(6) O33 0.207(10) 0.121(6) 0.192(9) -0.080(6) 0.108(8) -0.015(6) O11 0.120(7) 0.112(6) 0.225(10) 0.001(6) 0.041(7) 0.024(5) O54 0.121(7) 0.135(7) 0.234(11) -0.085(7) 0.014(7) -0.027(5) O24 0.206(10) 0.125(7) 0.184(9) -0.075(6) 0.054(8) 0.028(6) O34 0.234(13) 0.124(7) 0.215(11) 0.022(7) -0.029(9) 0.035(8) O10 0.116(7) 0.193(9) 0.177(8) -0.057(7) 0.016(6) -0.078(7) O8 0.144(8) 0.169(8) 0.126(6) 0.064(6) -0.022(5) -0.035(6) O16 0.110(7) 0.322(16) 0.203(10) 0.080(10) 0.055(7) 0.120(9) O17 0.178(10) 0.203(10) 0.115(6) -0.055(6) -0.017(6) 0.002(8) O41 0.189(10) 0.184(10) 0.318(15) -0.011(9) 0.196(11) -0.015(8) O47 0.107(11) 0.38(3) 0.172(13) 0.000 0.052(10) 0.000 O42 0.109(9) 0.303(18) 0.33(2) -0.015(12) 0.104(11) -0.002(8) O55 0.271(14) 0.119(7) 0.241(11) 0.044(7) 0.141(11) -0.008(7) Cl4 0.0701(16) 0.166(3) 0.0700(15) 0.0076(14) 0.0065(12) -0.0070(14) Cl5 0.155(3) 0.123(2) 0.0914(17) -0.0251(16) 0.0432(18) 0.0508(19) O20 0.084(7) 0.283(15) 0.182(10) 0.065(8) -0.006(7) -0.038(7) O21 0.213(13) 0.292(15) 0.070(6) 0.015(6) 0.000(6) -0.035(9) O19 0.185(11) 0.341(17) 0.151(9) -0.113(10) 0.027(8) 0.095(11) O46 0.267(15) 0.200(11) 0.208(11) 0.113(9) 0.109(11) 0.082(10) O35 0.232(16) 0.32(2) 0.275(17) -0.064(15) 0.111(14) 0.047(14) O57 0.260(15) 0.257(14) 0.136(8) -0.022(8) 0.021(9) 0.105(12) O22 0.202(11) 0.249(13) 0.165(9) -0.010(8) 0.083(8) -0.124(10) O53 0.128(13) 0.47(4) 0.178(15) 0.000 0.060(12) 0.000 O43 0.281(16) 0.197(11) 0.181(10) -0.114(9) 0.064(10) -0.046(10) O27 0.37(2) 0.230(14) 0.195(12) -0.131(11) 0.088(13) -0.019(14) O52 0.267(17) 0.279(16) 0.288(17) -0.171(14) -0.052(13) 0.101(14) O30 0.092(7) 0.60(3) 0.242(13) -0.059(16) 0.107(8) 0.083(12) O26 0.48(3) 0.259(17) 0.143(10) 0.067(11) 0.060(14) 0.051(17) O25 0.199(13) 0.309(18) 0.42(2) -0.152(17) 0.226(16) -0.038(12) O50 0.277(17) 0.234(14) 0.246(14) 0.135(12) -0.050(12) -0.083(12) O48 0.30(2) 0.36(2) 0.224(16) 0.023(12) 0.154(17) 0.045(15) O23 0.31(2) 0.247(16) 0.214(13) -0.001(12) 0.093(13) 0.121(15) O45 0.218(16) 0.34(2) 0.39(2) 0.008(18) 0.151(17) -0.081(15) O31 0.63(4) 0.147(10) 0.41(2) -0.003(13) 0.36(3) 0.133(17) O18 0.38(3) 0.288(19) 0.294(19) 0.175(16) -0.125(18) -0.160(18) O39 0.251(18) 0.37(2) 0.51(3) -0.21(2) 0.19(2) -0.059(17) O32 0.41(5) 0.18(2) 0.40(4) 0.000 -0.03(4) 0.000 O29 0.268(19) 0.48(3) 0.296(19) 0.27(2) 0.016(15) 0.16(2) O14 0.237(12) 0.173(9) 0.116(6) 0.029(6) 0.001(7) -0.091(9) O12 0.42(3) 0.40(3) 0.42(3) 0.18(2) 0.34(3) 0.13(2) O15 0.100(5) 0.098(4) 0.100(4) 0.043(4) 0.011(4) -0.014(4) O13A 0.242(12) 0.101(10) 0.079(5) 0.042(6) -0.034(6) -0.071(8) O13B 0.242(12) 0.101(10) 0.079(5) 0.042(6) -0.034(6) -0.071(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 Cu1 N10 2.025(4) . ? Cu1 N4 2.036(5) . ? Cu1 N17 2.048(5) . ? Cu1 N16 2.051(5) 2 ? Cu1 O1 2.263(4) . ? Cu2 N24 2.033(5) 2 ? Cu2 N12 2.042(5) . ? Cu2 N23 2.045(5) . ? Cu2 N5 2.048(5) . ? Cu2 O2 2.334(5) . ? Cu3 N11 2.038(5) 2 ? Cu3 N22 2.038(5) . ? Cu3 N6 2.043(4) . ? Cu3 N18 2.049(5) . ? Cu3 O3 2.301(5) . ? P1 O4 1.469(4) . ? P1 N3 1.636(5) . ? P1 N2 1.640(5) . ? P1 N1 1.654(5) . ? P3 O6 1.470(4) . ? P3 N14 1.641(5) . ? P3 N15 1.646(5) . ? P3 N13 1.651(5) . ? P2 O5 1.467(4) . ? P2 N9 1.636(5) . ? P2 N8 1.637(5) . ? P2 N7 1.638(5) . ? P4 O7 1.468(4) . ? P4 N20 1.641(5) . ? P4 N19 1.649(5) . ? P4 N21 1.649(5) . ? N1 C1 1.400(7) . ? N13 C31 1.414(7) . ? N12 C25 1.338(7) . ? N12 C24 1.341(7) . ? N10 C30 1.333(7) . ? N10 C29 1.343(7) . ? N4 C4 1.335(7) . ? N4 C5 1.364(7) . ? N23 C54 1.341(8) . ? N23 C55 1.343(7) . ? N17 C39 1.316(7) . ? N17 C40 1.343(7) . ? N21 C56 1.406(7) . ? N18 C44 1.331(8) . ? N18 C45 1.333(7) . ? N7 C16 1.415(7) . ? C29 C28 1.357(9) . ? N24 C60 1.335(7) . ? N24 C59 1.336(7) . ? N24 Cu2 2.033(5) 2 ? C11 C15 1.376(8) . ? C11 N3 1.404(7) . ? C11 C12 1.405(8) . ? N14 C36 1.405(7) . ? N5 C9 1.327(7) . ? N5 C10 1.350(7) . ? C36 C37 1.384(8) . ? C36 C40 1.388(8) . ? N2 C6 1.419(7) . ? N11 C20 1.324(7) . ? N11 C19 1.349(8) . ? N11 Cu3 2.038(5) 2 ? N15 C41 1.404(7) . ? C26 C30 1.382(8) . ? C26 C27 1.392(8) . ? C26 N9 1.421(7) . ? N8 C21 1.410(7) . ? C56 C57 1.376(8) . ? C56 C60 1.394(8) . ? C31 C32 1.378(8) . ? C31 C35 1.386(8) . ? N16 C34 1.331(7) . ? N16 C35 1.339(7) . ? N16 Cu1 2.051(5) 2 ? C5 C1 1.383(8) . ? C15 N6 1.340(7) . ? C51 C55 1.391(8) . ? C51 C52 1.391(8) . ? C51 N20 1.416(7) . ? C6 C10 1.359(8) . ? C6 C7 1.391(8) . ? N6 C14 1.341(8) . ? N19 C46 1.422(8) . ? N22 C49 1.348(7) . ? N22 C50 1.355(7) . ? C45 C41 1.370(8) . ? C1 C2 1.394(8) . ? C46 C50 1.361(8) . ? C46 C47 1.380(8) . ? C41 C42 1.372(9) . ? C12 C13 1.363(8) . ? C59 C58 1.382(9) . ? C42 C43 1.368(10) . ? C52 C53 1.366(9) . ? C20 C16 1.396(8) . ? C7 C8 1.363(9) . ? C25 C21 1.401(8) . ? C2 C3 1.368(9) . ? C4 C3 1.355(9) . ? C54 C53 1.376(9) . ? C9 C8 1.417(9) . ? C37 C38 1.383(9) . ? C32 C33 1.396(9) . ? C23 C22 1.370(9) . ? C23 C24 1.380(9) . ? C39 C38 1.376(9) . ? C16 C17 1.393(8) . ? C21 C22 1.375(8) . ? C58 C57 1.374(10) . ? C17 C18 1.358(9) . ? C33 C34 1.376(9) . ? C18 C19 1.372(9) . ? C44 C43 1.357(9) . ? C49 C48 1.347(10) . ? C14 C13 1.371(9) . ? C27 C28 1.366(9) . ? C47 C48 1.385(10) . ? Cl1 O10 1.384(7) . ? Cl1 O9 1.385(7) . ? Cl1 O8 1.398(7) . ? Cl1 O11 1.443(8) . ? Cl2 O15 1.4479(10) . ? Cl2 O13A 1.4490(10) . ? Cl2 O14 1.4492(10) . ? Cl2 O13B 1.4497(10) . ? Cl2 O12 1.4515(10) . ? Cl3 O18 1.318(11) . ? Cl3 O16 1.321(7) . ? Cl3 O19 1.325(9) . ? Cl3 O17 1.345(8) . ? Cl6 O31 1.262(10) . ? Cl6 O30 1.289(8) . ? Cl6 O29 1.341(11) . ? Cl6 O28 1.396(10) . ? O24 Cl5 1.347(7) . ? Cl4 O21 1.323(8) . ? Cl4 O20 1.329(9) . ? Cl4 O23 1.355(11) . ? Cl4 O22 1.368(9) . ? Cl5 O25 1.289(9) . ? Cl5 O27 1.379(11) . ? Cl5 O26 1.433(11) . ? O13A O13B 0.65(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N10 Cu1 N4 89.40(18) . . ? N10 Cu1 N17 173.99(18) . . ? N4 Cu1 N17 89.59(18) . . ? N10 Cu1 N16 89.92(19) . 2 ? N4 Cu1 N16 174.76(18) . 2 ? N17 Cu1 N16 90.55(19) . 2 ? N10 Cu1 O1 93.69(18) . . ? N4 Cu1 O1 93.23(18) . . ? N17 Cu1 O1 92.28(18) . . ? N16 Cu1 O1 92.00(18) 2 . ? N24 Cu2 N12 90.46(19) 2 . ? N24 Cu2 N23 90.01(19) 2 . ? N12 Cu2 N23 177.72(19) . . ? N24 Cu2 N5 177.45(19) 2 . ? N12 Cu2 N5 89.29(18) . . ? N23 Cu2 N5 90.15(19) . . ? N24 Cu2 O2 91.54(18) 2 . ? N12 Cu2 O2 91.20(19) . . ? N23 Cu2 O2 91.01(19) . . ? N5 Cu2 O2 91.01(19) . . ? N11 Cu3 N22 89.80(18) 2 . ? N11 Cu3 N6 177.9(2) 2 . ? N22 Cu3 N6 90.48(19) . . ? N11 Cu3 N18 91.04(19) 2 . ? N22 Cu3 N18 175.6(2) . . ? N6 Cu3 N18 88.52(18) . . ? N11 Cu3 O3 90.9(2) 2 . ? N22 Cu3 O3 91.76(19) . . ? N6 Cu3 O3 91.17(19) . . ? N18 Cu3 O3 92.53(19) . . ? O4 P1 N3 113.4(2) . . ? O4 P1 N2 113.7(3) . . ? N3 P1 N2 105.3(2) . . ? O4 P1 N1 113.2(2) . . ? N3 P1 N1 105.8(2) . . ? N2 P1 N1 104.7(2) . . ? O6 P3 N14 113.0(3) . . ? O6 P3 N15 112.9(3) . . ? N14 P3 N15 106.0(3) . . ? O6 P3 N13 113.6(3) . . ? N14 P3 N13 105.3(3) . . ? N15 P3 N13 105.4(3) . . ? O5 P2 N9 113.3(3) . . ? O5 P2 N8 113.6(2) . . ? N9 P2 N8 105.9(3) . . ? O5 P2 N7 113.6(3) . . ? N9 P2 N7 104.8(3) . . ? N8 P2 N7 104.8(3) . . ? O7 P4 N20 113.3(3) . . ? O7 P4 N19 113.2(3) . . ? N20 P4 N19 105.3(3) . . ? O7 P4 N21 113.8(3) . . ? N20 P4 N21 105.8(3) . . ? N19 P4 N21 104.7(3) . . ? C1 N1 P1 127.1(4) . . ? C31 N13 P3 127.0(4) . . ? C25 N12 C24 119.0(5) . . ? C25 N12 Cu2 120.5(4) . . ? C24 N12 Cu2 120.4(4) . . ? C30 N10 C29 117.9(5) . . ? C30 N10 Cu1 120.6(4) . . ? C29 N10 Cu1 121.5(4) . . ? C4 N4 C5 118.2(5) . . ? C4 N4 Cu1 122.6(4) . . ? C5 N4 Cu1 119.2(4) . . ? C54 N23 C55 118.1(5) . . ? C54 N23 Cu2 121.1(4) . . ? C55 N23 Cu2 120.8(4) . . ? C39 N17 C40 119.1(5) . . ? C39 N17 Cu1 121.6(4) . . ? C40 N17 Cu1 119.3(4) . . ? C56 N21 P4 126.7(4) . . ? C44 N18 C45 117.3(5) . . ? C44 N18 Cu3 120.7(4) . . ? C45 N18 Cu3 122.0(4) . . ? C16 N7 P2 128.1(4) . . ? N10 C29 C28 122.0(6) . . ? C60 N24 C59 119.4(5) . . ? C60 N24 Cu2 120.4(4) . 2 ? C59 N24 Cu2 120.2(4) . 2 ? C15 C11 N3 122.9(5) . . ? C15 C11 C12 118.4(5) . . ? N3 C11 C12 118.7(5) . . ? C36 N14 P3 127.7(4) . . ? C9 N5 C10 119.6(5) . . ? C9 N5 Cu2 120.1(4) . . ? C10 N5 Cu2 120.3(4) . . ? C37 C36 C40 118.4(5) . . ? C37 C36 N14 118.8(5) . . ? C40 C36 N14 122.8(5) . . ? C6 N2 P1 126.7(4) . . ? C11 N3 P1 128.1(4) . . ? C20 N11 C19 119.1(5) . . ? C20 N11 Cu3 120.2(4) . 2 ? C19 N11 Cu3 120.7(4) . 2 ? C41 N15 P3 127.3(4) . . ? C30 C26 C27 117.4(5) . . ? C30 C26 N9 123.1(5) . . ? C27 C26 N9 119.5(5) . . ? C21 N8 P2 127.8(4) . . ? C26 N9 P2 127.5(4) . . ? C57 C56 C60 118.0(6) . . ? C57 C56 N21 119.0(5) . . ? C60 C56 N21 123.0(5) . . ? C32 C31 C35 119.9(5) . . ? C32 C31 N13 118.1(5) . . ? C35 C31 N13 122.0(5) . . ? C34 N16 C35 119.3(5) . . ? C34 N16 Cu1 121.4(4) . 2 ? C35 N16 Cu1 119.3(4) . 2 ? N17 C40 C36 122.2(5) . . ? N10 C30 C26 123.4(5) . . ? N4 C5 C1 122.4(5) . . ? N6 C15 C11 122.5(5) . . ? C55 C51 C52 118.4(5) . . ? C55 C51 N20 122.8(5) . . ? C52 C51 N20 118.8(5) . . ? C10 C6 C7 119.3(5) . . ? C10 C6 N2 122.5(5) . . ? C7 C6 N2 118.2(5) . . ? C15 N6 C14 118.8(5) . . ? C15 N6 Cu3 120.7(4) . . ? C14 N6 Cu3 120.5(4) . . ? C46 N19 P4 126.1(4) . . ? C49 N22 C50 117.1(5) . . ? C49 N22 Cu3 122.2(4) . . ? C50 N22 Cu3 120.7(4) . . ? N18 C45 C41 123.9(6) . . ? C5 C1 C2 117.7(5) . . ? C5 C1 N1 122.9(5) . . ? C2 C1 N1 119.4(5) . . ? C50 C46 C47 118.7(6) . . ? C50 C46 N19 123.2(5) . . ? C47 C46 N19 118.1(5) . . ? C45 C41 C42 117.3(6) . . ? C45 C41 N15 123.1(5) . . ? C42 C41 N15 119.5(5) . . ? N16 C35 C31 121.7(5) . . ? C51 N20 P4 127.4(4) . . ? C13 C12 C11 118.1(5) . . ? N23 C55 C51 122.4(5) . . ? N22 C50 C46 123.4(5) . . ? N24 C59 C58 120.9(6) . . ? C43 C42 C41 119.4(6) . . ? N5 C10 C6 122.2(5) . . ? C53 C52 C51 118.8(6) . . ? N11 C20 C16 122.2(5) . . ? C8 C7 C6 119.1(6) . . ? N12 C25 C21 122.6(5) . . ? C3 C2 C1 118.9(6) . . ? N4 C4 C3 122.0(6) . . ? N23 C54 C53 122.4(6) . . ? N5 C9 C8 120.7(6) . . ? N24 C60 C56 122.4(5) . . ? C38 C37 C36 118.4(6) . . ? C31 C32 C33 117.4(6) . . ? C22 C23 C24 119.9(6) . . ? N17 C39 C38 122.2(6) . . ? C17 C16 C20 118.2(5) . . ? C17 C16 N7 119.6(5) . . ? C20 C16 N7 122.3(5) . . ? C22 C21 C25 117.5(5) . . ? C22 C21 N8 120.2(5) . . ? C25 C21 N8 122.3(5) . . ? C23 C22 C21 119.9(6) . . ? C57 C58 C59 120.0(6) . . ? C18 C17 C16 118.6(6) . . ? C58 C57 C56 119.2(6) . . ? C39 C38 C37 119.7(6) . . ? N12 C24 C23 121.2(6) . . ? C34 C33 C32 120.0(6) . . ? C17 C18 C19 120.5(6) . . ? N18 C44 C43 122.5(6) . . ? C48 C49 N22 122.4(6) . . ? N6 C14 C13 121.4(5) . . ? C7 C8 C9 119.1(6) . . ? C44 C43 C42 119.5(6) . . ? C28 C27 C26 118.8(5) . . ? C12 C13 C14 120.7(6) . . ? C29 C28 C27 120.4(6) . . ? N16 C34 C33 121.7(6) . . ? C46 C47 C48 118.2(6) . . ? N11 C19 C18 121.2(6) . . ? C4 C3 C2 120.8(6) . . ? C52 C53 C54 119.9(6) . . ? C49 C48 C47 120.3(6) . . ? O10 Cl1 O9 117.6(6) . . ? O10 Cl1 O8 111.2(6) . . ? O9 Cl1 O8 109.3(6) . . ? O10 Cl1 O11 108.2(6) . . ? O9 Cl1 O11 104.6(6) . . ? O8 Cl1 O11 105.1(7) . . ? O15 Cl2 O13A 111.4(8) . . ? O15 Cl2 O14 119.7(5) . . ? O13A Cl2 O14 128.2(8) . . ? O15 Cl2 O13B 133(2) . . ? O13A Cl2 O13B 25.9(18) . . ? O14 Cl2 O13B 103(2) . . ? O15 Cl2 O12 92.0(7) . . ? O13A Cl2 O12 87.16(8) . . ? O14 Cl2 O12 98.58(9) . . ? O13B Cl2 O12 98.63(9) . . ? O18 Cl3 O16 107.1(11) . . ? O18 Cl3 O19 116.2(14) . . ? O16 Cl3 O19 106.6(7) . . ? O18 Cl3 O17 98.4(9) . . ? O16 Cl3 O17 116.7(9) . . ? O19 Cl3 O17 111.9(8) . . ? O31 Cl6 O30 109.2(13) . . ? O31 Cl6 O29 102.2(14) . . ? O30 Cl6 O29 121.4(11) . . ? O31 Cl6 O28 99.3(12) . . ? O30 Cl6 O28 113.0(8) . . ? O29 Cl6 O28 108.9(11) . . ? O21 Cl4 O20 117.5(9) . . ? O21 Cl4 O23 117.4(9) . . ? O20 Cl4 O23 103.5(10) . . ? O21 Cl4 O22 112.0(8) . . ? O20 Cl4 O22 109.0(8) . . ? O23 Cl4 O22 94.9(10) . . ? O25 Cl5 O24 122.4(9) . . ? O25 Cl5 O27 110.0(9) . . ? O24 Cl5 O27 114.1(8) . . ? O25 Cl5 O26 100.2(12) . . ? O24 Cl5 O26 109.0(9) . . ? O27 Cl5 O26 97.1(11) . . ? O13B O13A Cl2 77.1(9) . . ? O13A O13B Cl2 77.0(9) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.657 _refine_diff_density_min -1.230 _refine_diff_density_rms 0.140 data_c:\lining58\1 _database_code_depnum_ccdc_archive 'CCDC 764791' #TrackingRef '764791.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H104 Cl6 Cu3 N24 O26 P4' _chemical_formula_weight 2104.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 35.332(7) _cell_length_b 18.535(3) _cell_length_c 35.992(7) _cell_angle_alpha 90.00 _cell_angle_beta 115.187(3) _cell_angle_gamma 90.00 _cell_volume 21330(7) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Blue _exptl_crystal_size_max 0.4300 _exptl_crystal_size_mid 0.4000 _exptl_crystal_size_min 0.3400 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8712 _exptl_absorpt_coefficient_mu 0.875 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9047 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _exptl_special_details ; ? ; _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_type 'Smart CCD' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65323 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 25.00 _reflns_number_total 18630 _reflns_number_gt 13596 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 2000)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.3000P)^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 18630 _refine_ls_number_parameters 1090 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1424 _refine_ls_R_factor_gt 0.1209 _refine_ls_wR_factor_ref 0.4016 _refine_ls_wR_factor_gt 0.3528 _refine_ls_goodness_of_fit_ref 1.158 _refine_ls_restrained_S_all 1.158 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.5000 0.54643(5) 0.2500 0.0508(3) Uani 1 2 d S . . Cu2 Cu 0.5000 -0.16886(5) 0.2500 0.0555(3) Uani 1 2 d S . . Cu3 Cu 0.45848(3) 0.18704(4) 0.40407(3) 0.0699(3) Uani 1 1 d . . . Cu4 Cu 0.69547(3) 0.19040(4) 0.37329(3) 0.0675(3) Uani 1 1 d . . . Cl4 Cl 0.5000 0.68878(8) 0.2500 0.0607(5) Uani 1 2 d S . . P3 P 0.62945(5) 0.37772(8) 0.23215(5) 0.0571(4) Uani 1 1 d . . . P4 P 0.58150(5) 0.38179(8) 0.40051(5) 0.0599(4) Uani 1 1 d . . . P1 P 0.37066(5) -0.00084(8) 0.26672(5) 0.0627(4) Uani 1 1 d . . . N24 N 0.49866(14) 0.5406(2) 0.30623(14) 0.0543(10) Uani 1 1 d . . . N4 N 0.47300(15) -0.1629(2) 0.29008(15) 0.0574(11) Uani 1 1 d . . . N18 N 0.56367(14) 0.5403(2) 0.27700(14) 0.0560(10) Uani 1 1 d . . . N12 N 0.68227(16) 0.1644(3) 0.42136(17) 0.0659(12) Uani 1 1 d . . . N15 N 0.64965(15) 0.4392(3) 0.26815(16) 0.0662(12) Uani 1 1 d . . . H41 H 0.6771 0.4421 0.2799 0.079 Uiso 1 1 calc R . . N7 N 0.55112(16) -0.0493(3) 0.41302(18) 0.0705(13) Uani 1 1 d . . . H16 H 0.5549 -0.0962 0.4166 0.085 Uiso 1 1 calc R . . N19 N 0.60037(17) 0.3380(3) 0.44502(17) 0.0711(14) Uani 1 1 d . . . H46 H 0.6261 0.3482 0.4626 0.085 Uiso 1 1 calc R . . N2 N 0.34127(17) -0.0446(3) 0.22455(17) 0.0699(13) Uani 1 1 d . . . H6 H 0.3393 -0.0915 0.2271 0.084 Uiso 1 1 calc R . . C41 C 0.62799(16) 0.4885(3) 0.28259(17) 0.0560(12) Uani 1 1 d . . . N22 N 0.69263(16) 0.2979(3) 0.38475(17) 0.0646(12) Uani 1 1 d . . . N17 N 0.70918(16) 0.2144(3) 0.32545(17) 0.0666(12) Uani 1 1 d . . . N16 N 0.55731(17) 0.2948(3) 0.10359(16) 0.0678(13) Uani 1 1 d . . . C45 C 0.58419(16) 0.4923(3) 0.26490(18) 0.0572(12) Uani 1 1 d . . . H45 H 0.5686 0.4594 0.2436 0.069 Uiso 1 1 calc R . . C26 C 0.64396(19) 0.0912(3) 0.44923(18) 0.0639(14) Uani 1 1 d . . . C11 C 0.42141(18) -0.1118(3) 0.30936(18) 0.0608(13) Uani 1 1 d . . . N5 N 0.30170(16) 0.0833(3) 0.13860(17) 0.0679(13) Uani 1 1 d . . . C52 C 0.4980(2) 0.5389(3) 0.3829(2) 0.0703(16) Uani 1 1 d . . . H52 H 0.4973 0.5384 0.4091 0.084 Uiso 1 1 calc R . . N23 N 0.51815(17) 0.2130(3) 0.44340(16) 0.0671(12) Uani 1 1 d . . . C36 C 0.59051(18) 0.3933(3) 0.14902(19) 0.0630(14) Uani 1 1 d . . . N6 N 0.39758(17) 0.1609(3) 0.36764(18) 0.0674(13) Uani 1 1 d . . . C5 C 0.38839(19) 0.1144(3) 0.3369(2) 0.0657(15) Uani 1 1 d . . . H5 H 0.4107 0.0929 0.3327 0.079 Uiso 1 1 calc R . . N1 N 0.38912(17) -0.0626(3) 0.30290(18) 0.0723(14) Uani 1 1 d . . . H11 H 0.3774 -0.0651 0.3201 0.087 Uiso 1 1 calc R . . C43 C 0.62849(19) 0.5844(3) 0.3268(2) 0.0690(16) Uani 1 1 d . . . H43 H 0.6433 0.6170 0.3486 0.083 Uiso 1 1 calc R . . C15 C 0.44260(18) -0.1147(3) 0.28414(19) 0.0608(13) Uani 1 1 d . . . H15 H 0.4352 -0.0814 0.2621 0.073 Uiso 1 1 calc R . . C44 C 0.58566(18) 0.5844(3) 0.30841(18) 0.0603(13) Uani 1 1 d . . . H44 H 0.5710 0.6167 0.3182 0.072 Uiso 1 1 calc R . . C14 C 0.48470(19) -0.2076(3) 0.3219(2) 0.0629(14) Uani 1 1 d . . . H14 H 0.5064 -0.2413 0.3260 0.075 Uiso 1 1 calc R . . C34 C 0.7411(2) 0.1822(3) 0.3217(2) 0.0720(17) Uani 1 1 d . . . H34 H 0.7573 0.1477 0.3417 0.086 Uiso 1 1 calc R . . C13 C 0.4668(2) -0.2070(4) 0.3489(2) 0.0740(17) Uani 1 1 d . . . H13 H 0.4765 -0.2390 0.3717 0.089 Uiso 1 1 calc R . . C42 C 0.65010(19) 0.5355(3) 0.3133(2) 0.0710(16) Uani 1 1 d . . . H42 H 0.6798 0.5352 0.3253 0.085 Uiso 1 1 calc R . . N11 N 0.47238(16) 0.0796(3) 0.41481(17) 0.0685(13) Uani 1 1 d . . . C30 C 0.65352(18) 0.1144(3) 0.41698(19) 0.0635(14) Uani 1 1 d . . . H30 H 0.6387 0.0934 0.3907 0.076 Uiso 1 1 calc R . . C55 C 0.52318(18) 0.4939(3) 0.33564(17) 0.0572(12) Uani 1 1 d . . . H55 H 0.5405 0.4616 0.3294 0.069 Uiso 1 1 calc R . . C53 C 0.4735(2) 0.5860(3) 0.3525(2) 0.0712(16) Uani 1 1 d . . . H53 H 0.4554 0.6184 0.3577 0.085 Uiso 1 1 calc R . . C46 C 0.5788(2) 0.2862(3) 0.45709(19) 0.0655(14) Uani 1 1 d . . . C50 C 0.53887(19) 0.2638(3) 0.43214(18) 0.0658(14) Uani 1 1 d . . . H50 H 0.5251 0.2849 0.4057 0.079 Uiso 1 1 calc R . . C19 C 0.4516(3) 0.0375(4) 0.4288(3) 0.090(2) Uani 1 1 d . . . H19 H 0.4306 0.0585 0.4353 0.108 Uiso 1 1 calc R . . C16 C 0.51706(19) -0.0200(3) 0.41793(19) 0.0650(14) Uani 1 1 d . . . C54 C 0.47467(19) 0.5870(3) 0.3155(2) 0.0631(14) Uani 1 1 d . . . H54 H 0.4582 0.6212 0.2955 0.076 Uiso 1 1 calc R . . C39 C 0.5485(3) 0.3370(4) 0.0712(2) 0.087(2) Uani 1 1 d . . . H39 H 0.5338 0.3184 0.0442 0.105 Uiso 1 1 calc R . . C40 C 0.5773(2) 0.3225(3) 0.1416(2) 0.0651(15) Uani 1 1 d . . . H40 H 0.5825 0.2918 0.1644 0.078 Uiso 1 1 calc R . . C38 C 0.5612(3) 0.4107(4) 0.0773(2) 0.089(2) Uani 1 1 d . . . H38 H 0.5552 0.4407 0.0540 0.107 Uiso 1 1 calc R . . C37 C 0.5812(2) 0.4386(4) 0.1147(2) 0.0771(18) Uani 1 1 d . . . H37 H 0.5891 0.4880 0.1182 0.092 Uiso 1 1 calc R . . C35 C 0.68606(19) 0.2620(3) 0.2969(2) 0.0648(14) Uani 1 1 d . . . H35 H 0.6632 0.2841 0.2997 0.078 Uiso 1 1 calc R . . C47 C 0.5976(2) 0.2563(4) 0.4955(2) 0.0826(19) Uani 1 1 d . . . H47 H 0.6248 0.2713 0.5141 0.099 Uiso 1 1 calc R . . C27 C 0.6675(3) 0.1211(4) 0.4881(2) 0.087(2) Uani 1 1 d . . . H27 H 0.6636 0.1052 0.5113 0.105 Uiso 1 1 calc R . . C18 C 0.4588(3) -0.0365(5) 0.4348(3) 0.114(3) Uani 1 1 d . . . H18 H 0.4400 -0.0665 0.4403 0.136 Uiso 1 1 calc R . . C12 C 0.4341(2) -0.1594(4) 0.3429(2) 0.0767(17) Uani 1 1 d . . . H12 H 0.4209 -0.1591 0.3610 0.092 Uiso 1 1 calc R . . C29 C 0.7029(2) 0.1938(4) 0.4587(2) 0.0790(19) Uani 1 1 d . . . H29 H 0.7231 0.2302 0.4623 0.095 Uiso 1 1 calc R . . C4 C 0.3664(3) 0.1910(4) 0.3737(3) 0.085(2) Uani 1 1 d . . . H4 H 0.3728 0.2247 0.3955 0.102 Uiso 1 1 calc R . . C49 C 0.5375(3) 0.1848(4) 0.4811(2) 0.0786(19) Uani 1 1 d . . . H49 H 0.5231 0.1500 0.4897 0.094 Uiso 1 1 calc R . . C20 C 0.5054(2) 0.0513(3) 0.4102(2) 0.0678(15) Uani 1 1 d . . . H20 H 0.5213 0.0820 0.4011 0.081 Uiso 1 1 calc R . . C17 C 0.4940(2) -0.0657(4) 0.4324(3) 0.088(2) Uani 1 1 d . . . H17 H 0.5023 -0.1142 0.4401 0.106 Uiso 1 1 calc R . . C33 C 0.7515(2) 0.1977(4) 0.2893(3) 0.083(2) Uani 1 1 d . . . H33 H 0.7743 0.1741 0.2871 0.100 Uiso 1 1 calc R . . C28 C 0.6958(3) 0.1730(5) 0.4920(2) 0.093(2) Uani 1 1 d . . . H28 H 0.7110 0.1953 0.5179 0.112 Uiso 1 1 calc R . . C3 C 0.3249(3) 0.1746(5) 0.3492(3) 0.105(3) Uani 1 1 d . . . H3 H 0.3031 0.1965 0.3541 0.126 Uiso 1 1 calc R . . C48 C 0.5767(3) 0.2040(5) 0.5073(2) 0.099(3) Uani 1 1 d . . . H48 H 0.5899 0.1819 0.5335 0.118 Uiso 1 1 calc R . . P2 P 0.58476(5) -0.00515(8) 0.40120(5) 0.0609(4) Uani 1 1 d . . . O3 O 0.59700(13) 0.3336(2) 0.23668(14) 0.0680(10) Uani 1 1 d . . . O4 O 0.56129(14) 0.3354(2) 0.36399(13) 0.0686(10) Uani 1 1 d . . . O1 O 0.40372(14) 0.0427(2) 0.26271(15) 0.0741(11) Uani 1 1 d . . . O2 O 0.56541(14) 0.0424(2) 0.36465(14) 0.0700(11) Uani 1 1 d . . . N10 N 0.55795(14) -0.1639(2) 0.29843(15) 0.0587(11) Uani 1 1 d . . . N14 N 0.66964(17) 0.3315(3) 0.23347(17) 0.0669(12) Uani 1 1 d . . . H31 H 0.6770 0.3393 0.2133 0.080 Uiso 1 1 calc R . . N13 N 0.61223(16) 0.4215(3) 0.18842(16) 0.0654(12) Uani 1 1 d . . . H36 H 0.6173 0.4681 0.1900 0.078 Uiso 1 1 calc R . . N9 N 0.61490(15) -0.0673(3) 0.39607(16) 0.0668(13) Uani 1 1 d . . . H21 H 0.6399 -0.0713 0.4165 0.080 Uiso 1 1 calc R . . C25 C 0.56770(16) -0.1176(3) 0.32920(17) 0.0544(12) Uani 1 1 d . . . H25 H 0.5470 -0.0837 0.3278 0.065 Uiso 1 1 calc R . . N21 N 0.62139(17) 0.4272(3) 0.40114(16) 0.0666(12) Uani 1 1 d . . . H56 H 0.6211 0.4743 0.4043 0.080 Uiso 1 1 calc R . . C56 C 0.65671(18) 0.3975(3) 0.39707(17) 0.0605(13) Uani 1 1 d . . . N8 N 0.61378(17) 0.0388(3) 0.44345(16) 0.0693(13) Uani 1 1 d . . . H26 H 0.6097 0.0278 0.4652 0.083 Uiso 1 1 calc R . . C6 C 0.31934(19) -0.0171(3) 0.1857(2) 0.0664(15) Uani 1 1 d . . . N3 N 0.33751(16) 0.0455(3) 0.27792(19) 0.0715(14) Uani 1 1 d . . . H1 H 0.3108 0.0386 0.2622 0.086 Uiso 1 1 calc R . . N20 N 0.54969(16) 0.4438(3) 0.40473(16) 0.0653(12) Uani 1 1 d . . . H51 H 0.5488 0.4473 0.4287 0.078 Uiso 1 1 calc R . . C51 C 0.52398(17) 0.4916(3) 0.37371(18) 0.0580(13) Uani 1 1 d . . . C21 C 0.60590(17) -0.1152(3) 0.36312(18) 0.0596(13) Uani 1 1 d . . . C60 C 0.6590(2) 0.3262(3) 0.38849(19) 0.0630(14) Uani 1 1 d . . . H60 H 0.6363 0.2954 0.3850 0.076 Uiso 1 1 calc R . . C1 C 0.3477(2) 0.0958(3) 0.3106(2) 0.0676(15) Uani 1 1 d . . . C22 C 0.63611(18) -0.1636(3) 0.3633(2) 0.0681(15) Uani 1 1 d . . . H22 H 0.6631 -0.1640 0.3856 0.082 Uiso 1 1 calc R . . C10 C 0.32250(19) 0.0560(3) 0.1758(2) 0.0651(14) Uani 1 1 d . . . H10 H 0.3405 0.0870 0.1970 0.078 Uiso 1 1 calc R . . C57 C 0.6904(2) 0.4430(3) 0.4018(2) 0.0744(17) Uani 1 1 d . . . H57 H 0.6897 0.4928 0.4077 0.089 Uiso 1 1 calc R . . C9 C 0.2761(2) 0.0394(4) 0.1078(2) 0.0786(19) Uani 1 1 d . . . H9 H 0.2609 0.0587 0.0810 0.094 Uiso 1 1 calc R . . C59 C 0.7245(2) 0.3414(4) 0.3892(2) 0.0719(16) Uani 1 1 d . . . H59 H 0.7482 0.3224 0.3864 0.086 Uiso 1 1 calc R . . C32 C 0.7276(2) 0.2487(4) 0.2600(3) 0.0788(18) Uani 1 1 d . . . H32 H 0.7345 0.2613 0.2380 0.095 Uiso 1 1 calc R . . C23 C 0.6271(2) -0.2104(4) 0.3315(2) 0.0756(18) Uani 1 1 d . . . H23 H 0.6477 -0.2438 0.3319 0.091 Uiso 1 1 calc R . . C7 C 0.2936(2) -0.0604(3) 0.1542(2) 0.0746(17) Uani 1 1 d . . . H7 H 0.2906 -0.1098 0.1594 0.089 Uiso 1 1 calc R . . C24 C 0.58806(19) -0.2094(3) 0.2987(2) 0.0672(15) Uani 1 1 d . . . H24 H 0.5823 -0.2409 0.2761 0.081 Uiso 1 1 calc R . . C31 C 0.6936(2) 0.2806(3) 0.2634(2) 0.0670(15) Uani 1 1 d . . . C2 C 0.3158(2) 0.1262(4) 0.3178(3) 0.087(2) Uani 1 1 d . . . H2 H 0.2875 0.1136 0.3010 0.104 Uiso 1 1 calc R . . C8 C 0.2718(2) -0.0330(4) 0.1148(3) 0.088(2) Uani 1 1 d . . . H8 H 0.2543 -0.0634 0.0931 0.106 Uiso 1 1 calc R . . C58 C 0.7233(2) 0.4148(4) 0.3978(3) 0.084(2) Uani 1 1 d . . . H58 H 0.7461 0.4450 0.4008 0.100 Uiso 1 1 calc R . . Cl1 Cl 0.47885(12) 0.18643(15) 0.34104(13) 0.1396(11) Uani 1 1 d . . . Cl5 Cl 0.78152(13) 0.19269(18) 0.42331(12) 0.1519(13) Uani 1 1 d . . . Cl6 Cl 0.56241(17) 0.1837(2) 0.02383(17) 0.1842(17) Uani 1 1 d . . . O9 O 0.5000 0.1888(4) 0.2500 0.109(3) Uani 1 2 d S . . O20 O 0.6851(2) 0.3992(5) 0.5058(2) 0.166(4) Uani 1 1 d . . . Cl7 Cl 0.5080(3) 0.2837(5) -0.04558(19) 0.283(4) Uani 1 1 d . . . O10 O 0.3479(3) 0.5736(4) 0.3049(3) 0.171(4) Uani 1 1 d . . . O27 O 0.7554(3) 1.0096(5) 0.2721(3) 0.162(3) Uani 1 1 d . . . O12 O 0.2909(3) 0.3714(4) 0.3222(3) 0.148(3) Uani 1 1 d . . . O19 O 0.5541(4) 0.4690(5) 0.4896(2) 0.177(4) Uani 1 1 d . . . O13 O 0.2561(2) 0.4644(5) 0.1902(3) 0.141(3) Uani 1 1 d . . . O23 O 0.6283(5) 0.5794(5) 0.4298(4) 0.204(5) Uani 1 1 d . . . O16 O 0.5759(4) -0.1978(5) 0.4340(4) 0.189(5) Uani 1 1 d . . . O26 O 0.6913(5) 0.8108(6) 0.2662(5) 0.242(7) Uani 1 1 d . . . O14 O 0.6157(6) 0.0275(8) 0.0217(5) 0.265(8) Uani 1 1 d . . . O7 O 0.5338(4) 0.2714(7) 0.3127(4) 0.111(4) Uani 0.50 1 d P . . O17 O 0.6950(4) -0.0939(10) 0.4692(4) 0.254(7) Uani 1 1 d . . . O28 O 0.6737(5) 0.8828(9) 0.1572(12) 0.61(3) Uani 1 1 d . . . O6 O 0.5000 0.3960(12) 0.2500 0.225(8) Uani 1 2 d S . . O24 O 0.8347(4) 0.2852(10) 0.3981(4) 0.245(6) Uani 1 1 d . . . O11 O 0.4200(7) 0.1867(5) 0.2623(9) 0.340(15) Uani 1 1 d . . . Cl3 Cl 0.61120(19) 0.18971(19) 0.32346(17) 0.1860(19) Uani 1 1 d . . . Cl2 Cl 0.5000 -0.0159(12) 0.2500 0.379(8) Uani 1 2 d S . . O8 O 0.5368(4) 0.1033(7) 0.3132(4) 0.108(3) Uani 0.50 1 d P . . O15 O 0.5809(12) -0.327(2) 0.3915(11) 0.49(2) Uiso 1 1 d . . . O5 O 0.3746(9) 0.6804(14) 0.2859(9) 0.384(15) Uiso 1 1 d . . . O18 O 0.5479(7) 0.3928(11) 0.5517(6) 0.296(8) Uiso 1 1 d . . . O21 O 0.5886(7) 0.6189(13) 0.4849(6) 0.317(9) Uiso 1 1 d . . . O22 O 0.7316(8) 0.5250(14) 0.5034(8) 0.353(11) Uiso 1 1 d . . . O25 O 0.7128(11) 0.6959(16) 0.3103(11) 0.430(17) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0546(5) 0.0453(5) 0.0492(5) 0.000 0.0188(4) 0.000 Cu2 0.0547(5) 0.0498(5) 0.0578(6) 0.000 0.0198(4) 0.000 Cu3 0.0746(5) 0.0567(5) 0.0731(6) 0.0076(3) 0.0262(4) 0.0048(3) Cu4 0.0822(6) 0.0510(5) 0.0669(5) -0.0011(3) 0.0295(4) -0.0018(3) Cl4 0.0717(12) 0.0344(9) 0.0712(13) 0.000 0.0258(10) 0.000 P3 0.0600(8) 0.0496(8) 0.0611(9) -0.0013(6) 0.0251(7) 0.0000(6) P4 0.0667(9) 0.0528(8) 0.0532(8) 0.0055(6) 0.0186(7) 0.0043(6) P1 0.0674(9) 0.0518(8) 0.0706(10) 0.0076(7) 0.0310(8) 0.0079(6) N24 0.062(2) 0.041(2) 0.056(3) 0.0010(19) 0.021(2) 0.0091(18) N4 0.062(3) 0.044(2) 0.064(3) 0.001(2) 0.025(2) 0.0037(19) N18 0.065(3) 0.045(2) 0.057(3) -0.005(2) 0.025(2) -0.0017(19) N12 0.070(3) 0.051(2) 0.066(3) -0.004(2) 0.019(2) -0.011(2) N15 0.055(2) 0.068(3) 0.071(3) -0.016(2) 0.022(2) -0.004(2) N7 0.069(3) 0.051(3) 0.091(4) 0.005(3) 0.033(3) -0.002(2) N19 0.071(3) 0.061(3) 0.063(3) 0.013(2) 0.010(2) 0.000(2) N2 0.087(3) 0.046(2) 0.077(4) 0.004(2) 0.035(3) 0.002(2) C41 0.055(3) 0.049(3) 0.056(3) 0.003(2) 0.016(2) 0.002(2) N22 0.068(3) 0.054(2) 0.069(3) 0.000(2) 0.025(2) -0.003(2) N17 0.064(3) 0.055(3) 0.078(3) -0.002(3) 0.027(2) -0.003(2) N16 0.074(3) 0.066(3) 0.060(3) -0.004(2) 0.026(2) -0.004(2) C45 0.055(3) 0.049(3) 0.063(3) -0.005(2) 0.021(2) -0.003(2) C26 0.069(3) 0.060(3) 0.055(3) -0.011(3) 0.019(3) -0.006(3) C11 0.069(3) 0.051(3) 0.062(3) 0.009(3) 0.029(3) 0.008(2) N5 0.071(3) 0.057(3) 0.066(3) 0.002(2) 0.019(2) 0.001(2) C52 0.090(4) 0.059(3) 0.066(4) 0.001(3) 0.039(3) 0.015(3) N23 0.075(3) 0.060(3) 0.062(3) 0.009(2) 0.024(2) 0.003(2) C36 0.065(3) 0.063(3) 0.065(3) 0.003(3) 0.031(3) -0.002(3) N6 0.074(3) 0.054(3) 0.080(3) 0.003(3) 0.038(3) 0.006(2) C5 0.065(3) 0.054(3) 0.087(4) 0.003(3) 0.039(3) 0.009(2) N1 0.083(3) 0.070(3) 0.074(3) 0.021(3) 0.043(3) 0.016(3) C43 0.067(3) 0.056(3) 0.066(4) -0.012(3) 0.011(3) -0.004(3) C15 0.068(3) 0.052(3) 0.064(3) 0.010(3) 0.029(3) 0.009(2) C44 0.069(3) 0.044(3) 0.061(3) -0.005(2) 0.022(3) 0.001(2) C14 0.064(3) 0.046(3) 0.070(4) 0.008(3) 0.021(3) 0.009(2) C34 0.063(3) 0.063(4) 0.087(5) 0.008(3) 0.029(3) 0.012(3) C13 0.095(5) 0.064(3) 0.066(4) 0.019(3) 0.037(4) 0.023(3) C42 0.055(3) 0.065(3) 0.080(4) -0.008(3) 0.016(3) -0.001(3) N11 0.071(3) 0.064(3) 0.072(3) 0.012(2) 0.033(3) 0.005(2) C30 0.064(3) 0.059(3) 0.057(3) -0.006(3) 0.015(3) -0.003(3) C55 0.068(3) 0.054(3) 0.049(3) 0.000(2) 0.024(2) 0.005(2) C53 0.088(4) 0.058(3) 0.085(4) 0.006(3) 0.054(4) 0.015(3) C46 0.077(4) 0.054(3) 0.058(3) 0.009(3) 0.022(3) -0.001(3) C50 0.076(4) 0.063(3) 0.052(3) 0.013(3) 0.020(3) 0.012(3) C19 0.108(5) 0.080(5) 0.111(6) 0.024(4) 0.074(5) 0.011(4) C16 0.076(4) 0.054(3) 0.069(4) 0.004(3) 0.034(3) -0.004(3) C54 0.072(3) 0.050(3) 0.075(4) 0.002(3) 0.039(3) 0.011(3) C39 0.121(6) 0.078(4) 0.067(4) 0.000(4) 0.044(4) -0.019(4) C40 0.075(4) 0.057(3) 0.062(4) 0.004(3) 0.029(3) -0.007(3) C38 0.116(6) 0.090(5) 0.062(4) 0.024(4) 0.038(4) -0.011(4) C37 0.100(5) 0.060(3) 0.078(4) 0.010(3) 0.044(4) -0.011(3) C35 0.070(3) 0.057(3) 0.075(4) -0.001(3) 0.037(3) 0.003(3) C47 0.082(4) 0.091(5) 0.059(4) 0.002(3) 0.015(3) -0.005(4) C27 0.106(5) 0.087(5) 0.060(4) -0.010(4) 0.026(4) -0.021(4) C18 0.135(7) 0.096(6) 0.157(9) 0.060(6) 0.108(7) 0.031(5) C12 0.097(5) 0.067(4) 0.075(4) 0.014(3) 0.046(4) 0.007(3) C29 0.074(4) 0.072(4) 0.077(5) -0.010(3) 0.018(3) -0.020(3) C4 0.094(5) 0.082(5) 0.090(5) -0.019(4) 0.050(4) -0.003(4) C49 0.089(5) 0.075(4) 0.067(4) 0.016(3) 0.028(4) -0.004(3) C20 0.075(4) 0.054(3) 0.076(4) 0.008(3) 0.034(3) -0.006(3) C17 0.093(5) 0.074(4) 0.114(6) 0.034(4) 0.060(5) 0.015(4) C33 0.071(4) 0.080(4) 0.106(6) 0.006(4) 0.045(4) 0.018(3) C28 0.103(5) 0.107(6) 0.051(4) -0.018(4) 0.014(4) -0.039(5) C3 0.075(5) 0.109(6) 0.159(9) -0.041(6) 0.077(6) -0.001(4) C48 0.113(6) 0.100(5) 0.062(4) 0.030(4) 0.018(4) -0.011(5) P2 0.0634(8) 0.0526(8) 0.0601(9) -0.0008(6) 0.0200(7) -0.0034(6) O3 0.064(2) 0.064(2) 0.081(3) 0.000(2) 0.035(2) -0.0052(19) O4 0.075(3) 0.067(2) 0.055(2) -0.003(2) 0.019(2) 0.001(2) O1 0.076(3) 0.068(3) 0.081(3) 0.003(2) 0.037(2) 0.005(2) O2 0.074(2) 0.066(2) 0.063(2) 0.004(2) 0.022(2) 0.0015(19) N10 0.059(3) 0.044(2) 0.067(3) 0.000(2) 0.020(2) 0.0034(19) N14 0.072(3) 0.064(3) 0.070(3) 0.000(3) 0.036(3) 0.008(2) N13 0.078(3) 0.047(2) 0.070(3) 0.001(2) 0.031(3) -0.006(2) N9 0.054(2) 0.074(3) 0.058(3) -0.007(2) 0.010(2) 0.001(2) C25 0.051(3) 0.051(3) 0.062(3) -0.002(2) 0.024(2) 0.006(2) N21 0.080(3) 0.049(2) 0.071(3) -0.002(2) 0.034(3) 0.000(2) C56 0.068(3) 0.050(3) 0.055(3) 0.003(2) 0.018(3) -0.002(2) N8 0.084(3) 0.063(3) 0.058(3) -0.003(2) 0.028(3) -0.014(2) C6 0.067(3) 0.052(3) 0.083(4) -0.004(3) 0.034(3) 0.001(3) N3 0.063(3) 0.062(3) 0.088(4) -0.002(3) 0.031(3) 0.008(2) N20 0.076(3) 0.067(3) 0.056(3) 0.009(2) 0.031(2) 0.014(2) C51 0.064(3) 0.047(3) 0.063(3) 0.006(2) 0.027(3) 0.002(2) C21 0.056(3) 0.048(3) 0.064(3) 0.003(2) 0.015(3) -0.001(2) C60 0.070(4) 0.052(3) 0.062(3) -0.002(3) 0.024(3) -0.006(3) C1 0.074(4) 0.054(3) 0.077(4) 0.009(3) 0.034(3) 0.008(3) C22 0.057(3) 0.061(3) 0.076(4) -0.008(3) 0.018(3) 0.003(3) C10 0.071(3) 0.044(3) 0.076(4) 0.005(3) 0.027(3) 0.001(2) C57 0.075(4) 0.056(3) 0.083(4) 0.000(3) 0.024(3) -0.010(3) C9 0.072(4) 0.067(4) 0.075(4) -0.008(3) 0.010(3) -0.008(3) C59 0.063(3) 0.070(4) 0.080(4) -0.002(3) 0.028(3) -0.005(3) C32 0.076(4) 0.072(4) 0.104(5) 0.004(4) 0.054(4) 0.010(3) C23 0.060(3) 0.059(3) 0.105(5) -0.007(4) 0.032(3) 0.006(3) C7 0.075(4) 0.056(3) 0.093(5) -0.009(3) 0.037(4) -0.016(3) C24 0.067(3) 0.050(3) 0.081(4) 0.000(3) 0.027(3) 0.007(3) C31 0.071(3) 0.051(3) 0.080(4) -0.002(3) 0.032(3) 0.000(3) C2 0.066(4) 0.086(5) 0.115(6) -0.010(4) 0.044(4) 0.005(3) C8 0.083(4) 0.061(4) 0.095(5) -0.016(4) 0.014(4) -0.023(3) C58 0.073(4) 0.071(4) 0.102(5) -0.010(4) 0.034(4) -0.025(3) Cl1 0.152(3) 0.103(2) 0.152(3) 0.0034(16) 0.053(2) -0.0002(15) Cl5 0.159(3) 0.130(2) 0.134(3) 0.0020(18) 0.030(2) -0.0134(18) Cl6 0.189(4) 0.187(4) 0.172(4) -0.018(3) 0.073(3) -0.012(3) O9 0.133(7) 0.074(5) 0.133(8) 0.000 0.068(6) 0.000 O20 0.115(5) 0.180(7) 0.105(5) 0.073(5) -0.048(4) -0.050(5) Cl7 0.403(11) 0.282(7) 0.165(5) 0.017(5) 0.123(6) 0.032(8) O10 0.164(7) 0.094(5) 0.199(9) -0.019(5) 0.024(7) 0.044(5) O27 0.123(5) 0.173(8) 0.208(9) 0.047(7) 0.089(6) 0.050(5) O12 0.184(7) 0.122(5) 0.204(8) -0.034(5) 0.145(7) -0.010(5) O19 0.286(12) 0.143(7) 0.078(4) -0.034(4) 0.056(6) 0.006(7) O13 0.101(4) 0.152(6) 0.175(8) 0.009(6) 0.065(5) 0.020(4) O23 0.311(14) 0.101(5) 0.255(13) -0.049(7) 0.174(12) 0.013(7) O16 0.238(12) 0.114(6) 0.222(11) 0.069(6) 0.104(10) 0.052(6) O26 0.255(14) 0.195(11) 0.355(19) -0.101(11) 0.205(14) 0.033(9) O14 0.41(2) 0.248(13) 0.294(16) -0.044(11) 0.306(17) 0.023(13) O7 0.117(9) 0.096(8) 0.122(10) -0.006(7) 0.052(8) -0.003(7) O17 0.189(10) 0.345(18) 0.134(8) -0.003(10) -0.022(7) 0.083(11) O28 0.221(13) 0.278(17) 1.47(9) -0.41(3) 0.50(3) -0.145(14) O6 0.162(12) 0.25(2) 0.239(19) 0.000 0.060(13) 0.000 O24 0.155(9) 0.355(17) 0.152(9) -0.019(11) -0.006(7) 0.005(10) O11 0.36(2) 0.104(8) 0.69(5) 0.078(13) 0.35(3) 0.033(9) Cl3 0.240(5) 0.124(3) 0.193(4) -0.001(2) 0.091(4) -0.008(2) Cl2 0.258(12) 0.49(2) 0.363(19) 0.000 0.110(13) 0.000 O8 0.113(8) 0.102(8) 0.095(8) -0.004(7) 0.032(7) -0.001(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N18 2.039(5) 2_655 ? Cu1 N18 2.039(5) . ? Cu1 N24 2.047(5) 2_655 ? Cu1 N24 2.047(5) . ? Cu1 Cl4 2.6384(18) . ? Cu2 N4 2.043(5) 2_655 ? Cu2 N4 2.043(5) . ? Cu2 N10 2.050(5) . ? Cu2 N10 2.050(5) 2_655 ? Cu2 Cl4 2.6387(18) 1_545 ? Cu3 N23 2.035(5) . ? Cu3 N6 2.045(6) . ? Cu3 N11 2.048(5) . ? Cu3 N16 2.060(6) 2_655 ? Cu3 Cl1 2.656(4) . ? Cu4 N17 2.027(6) . ? Cu4 N12 2.032(6) . ? Cu4 N5 2.043(5) 2_655 ? Cu4 N22 2.046(5) . ? Cu4 Cl3 2.745(6) . ? Cl4 Cu2 2.6387(18) 1_565 ? P3 O3 1.472(4) . ? P3 N13 1.640(5) . ? P3 N14 1.642(5) . ? P3 N15 1.643(5) . ? P4 O4 1.475(5) . ? P4 N21 1.634(5) . ? P4 N20 1.659(5) . ? P4 N19 1.661(5) . ? P1 O1 1.477(5) . ? P1 N3 1.635(5) . ? P1 N2 1.643(6) . ? P1 N1 1.647(5) . ? N24 C54 1.346(7) . ? N24 C55 1.356(7) . ? N4 C14 1.329(8) . ? N4 C15 1.342(7) . ? N18 C45 1.334(7) . ? N18 C44 1.342(7) . ? N12 C30 1.334(8) . ? N12 C29 1.340(9) . ? N15 C41 1.424(7) . ? N7 C16 1.398(8) . ? N7 P2 1.641(5) . ? N19 C46 1.405(8) . ? N2 C6 1.376(9) . ? C41 C42 1.361(8) . ? C41 C45 1.402(8) . ? N22 C59 1.339(8) . ? N22 C60 1.356(8) . ? N17 C35 1.336(8) . ? N17 C34 1.335(9) . ? N16 C39 1.328(9) . ? N16 C40 1.345(8) . ? N16 Cu3 2.060(5) 2_655 ? C26 N8 1.390(8) . ? C26 C27 1.403(9) . ? C26 C30 1.407(9) . ? C11 N1 1.400(8) . ? C11 C15 1.402(8) . ? C11 C12 1.406(9) . ? N5 C10 1.324(8) . ? N5 C9 1.363(8) . ? N5 Cu4 2.043(5) 2_655 ? C52 C53 1.380(9) . ? C52 C51 1.408(8) . ? N23 C49 1.338(9) . ? N23 C50 1.356(8) . ? C36 C40 1.380(8) . ? C36 N13 1.395(8) . ? C36 C37 1.413(9) . ? N6 C5 1.330(8) . ? N6 C4 1.335(9) . ? C5 C1 1.388(9) . ? C43 C44 1.370(9) . ? C43 C42 1.400(9) . ? C14 C13 1.368(10) . ? C34 C33 1.392(11) . ? C13 C12 1.394(10) . ? N11 C19 1.311(9) . ? N11 C20 1.353(8) . ? C55 C51 1.359(8) . ? C53 C54 1.350(9) . ? C46 C47 1.372(9) . ? C46 C50 1.375(9) . ? C19 C18 1.395(11) . ? C16 C20 1.377(8) . ? C16 C17 1.417(9) . ? C39 C38 1.426(11) . ? C38 C37 1.329(10) . ? C35 C31 1.385(9) . ? C47 C48 1.389(11) . ? C27 C28 1.353(10) . ? C18 C17 1.392(11) . ? C29 C28 1.379(11) . ? C4 C3 1.385(13) . ? C49 C48 1.350(12) . ? C33 C32 1.401(10) . ? C3 C2 1.370(12) . ? P2 O2 1.486(5) . ? P2 N9 1.632(5) . ? P2 N8 1.644(5) . ? N10 C25 1.326(7) . ? N10 C24 1.354(8) . ? N14 C31 1.411(8) . ? N9 C21 1.405(8) . ? C25 C21 1.383(8) . ? N21 C56 1.428(8) . ? C56 C60 1.367(8) . ? C56 C57 1.408(9) . ? C6 C7 1.369(9) . ? C6 C10 1.417(8) . ? N3 C1 1.422(9) . ? N20 C51 1.412(7) . ? C21 C22 1.394(8) . ? C1 C2 1.380(9) . ? C22 C23 1.359(10) . ? C57 C58 1.336(10) . ? C9 C8 1.384(10) . ? C59 C58 1.400(10) . ? C32 C31 1.389(9) . ? C23 C24 1.384(10) . ? C7 C8 1.389(11) . ? 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 N18 Cu1 N18 173.7(2) 2_655 . ? N18 Cu1 N24 90.62(18) 2_655 2_655 ? N18 Cu1 N24 89.04(18) . 2_655 ? N18 Cu1 N24 89.04(19) 2_655 . ? N18 Cu1 N24 90.62(18) . . ? N24 Cu1 N24 173.9(2) 2_655 . ? N18 Cu1 Cl4 93.17(12) 2_655 . ? N18 Cu1 Cl4 93.17(12) . . ? N24 Cu1 Cl4 93.04(12) 2_655 . ? N24 Cu1 Cl4 93.04(12) . . ? N4 Cu2 N4 173.8(3) 2_655 . ? N4 Cu2 N10 90.0(2) 2_655 . ? N4 Cu2 N10 89.7(2) . . ? N4 Cu2 N10 89.7(2) 2_655 2_655 ? N4 Cu2 N10 90.0(2) . 2_655 ? N10 Cu2 N10 174.9(3) . 2_655 ? N4 Cu2 Cl4 93.11(13) 2_655 1_545 ? N4 Cu2 Cl4 93.11(13) . 1_545 ? N10 Cu2 Cl4 92.55(13) . 1_545 ? N10 Cu2 Cl4 92.55(13) 2_655 1_545 ? N23 Cu3 N6 176.4(2) . . ? N23 Cu3 N11 90.3(2) . . ? N6 Cu3 N11 89.6(2) . . ? N23 Cu3 N16 90.3(2) . 2_655 ? N6 Cu3 N16 89.6(2) . 2_655 ? N11 Cu3 N16 175.8(2) . 2_655 ? N23 Cu3 Cl1 91.02(18) . . ? N6 Cu3 Cl1 92.58(18) . . ? N11 Cu3 Cl1 91.53(17) . . ? N16 Cu3 Cl1 92.65(17) 2_655 . ? N17 Cu4 N12 178.9(2) . . ? N17 Cu4 N5 89.1(2) . 2_655 ? N12 Cu4 N5 89.8(2) . 2_655 ? N17 Cu4 N22 90.4(2) . . ? N12 Cu4 N22 90.6(2) . . ? N5 Cu4 N22 179.5(2) 2_655 . ? N17 Cu4 Cl3 91.77(19) . . ? N12 Cu4 Cl3 88.69(19) . . ? N5 Cu4 Cl3 89.70(17) 2_655 . ? N22 Cu4 Cl3 90.21(17) . . ? Cu2 Cl4 Cu1 180.0 1_565 . ? O3 P3 N13 113.1(3) . . ? O3 P3 N14 114.3(3) . . ? N13 P3 N14 104.4(3) . . ? O3 P3 N15 113.3(3) . . ? N13 P3 N15 105.8(3) . . ? N14 P3 N15 105.0(3) . . ? O4 P4 N21 113.6(3) . . ? O4 P4 N20 113.3(3) . . ? N21 P4 N20 104.8(3) . . ? O4 P4 N19 114.7(3) . . ? N21 P4 N19 104.4(3) . . ? N20 P4 N19 105.0(3) . . ? O1 P1 N3 114.6(3) . . ? O1 P1 N2 113.3(3) . . ? N3 P1 N2 104.4(3) . . ? O1 P1 N1 113.2(3) . . ? N3 P1 N1 104.7(3) . . ? N2 P1 N1 105.6(3) . . ? C54 N24 C55 118.3(5) . . ? C54 N24 Cu1 119.6(4) . . ? C55 N24 Cu1 122.0(4) . . ? C14 N4 C15 119.1(5) . . ? C14 N4 Cu2 120.5(4) . . ? C15 N4 Cu2 120.4(4) . . ? C45 N18 C44 118.8(5) . . ? C45 N18 Cu1 121.6(4) . . ? C44 N18 Cu1 119.6(4) . . ? C30 N12 C29 117.5(6) . . ? C30 N12 Cu4 120.2(4) . . ? C29 N12 Cu4 122.2(4) . . ? C41 N15 P3 127.7(4) . . ? C16 N7 P2 126.6(4) . . ? C46 N19 P4 125.7(4) . . ? C6 N2 P1 128.2(4) . . ? C42 C41 C45 118.5(5) . . ? C42 C41 N15 119.6(5) . . ? C45 C41 N15 121.8(5) . . ? C59 N22 C60 118.9(5) . . ? C59 N22 Cu4 120.0(5) . . ? C60 N22 Cu4 121.1(4) . . ? C35 N17 C34 119.0(6) . . ? C35 N17 Cu4 120.6(4) . . ? C34 N17 Cu4 120.4(5) . . ? C39 N16 C40 119.6(6) . . ? C39 N16 Cu3 120.3(5) . 2_655 ? C40 N16 Cu3 120.1(4) . 2_655 ? N18 C45 C41 122.2(5) . . ? N8 C26 C27 121.1(6) . . ? N8 C26 C30 121.9(5) . . ? C27 C26 C30 117.0(6) . . ? N1 C11 C15 122.6(5) . . ? N1 C11 C12 119.4(6) . . ? C15 C11 C12 117.9(5) . . ? C10 N5 C9 119.1(5) . . ? C10 N5 Cu4 121.9(4) . 2_655 ? C9 N5 Cu4 119.0(4) . 2_655 ? C53 C52 C51 117.3(6) . . ? C49 N23 C50 117.8(6) . . ? C49 N23 Cu3 122.9(5) . . ? C50 N23 Cu3 119.2(4) . . ? C40 C36 N13 123.2(6) . . ? C40 C36 C37 117.5(6) . . ? N13 C36 C37 119.3(5) . . ? C5 N6 C4 118.8(6) . . ? C5 N6 Cu3 120.3(4) . . ? C4 N6 Cu3 120.9(5) . . ? N6 C5 C1 122.9(5) . . ? C11 N1 P1 127.2(4) . . ? C44 C43 C42 119.1(6) . . ? N4 C15 C11 122.3(5) . . ? N18 C44 C43 122.1(5) . . ? N4 C14 C13 122.7(5) . . ? N17 C34 C33 121.8(6) . . ? C14 C13 C12 119.8(6) . . ? C41 C42 C43 119.2(5) . . ? C19 N11 C20 118.1(6) . . ? C19 N11 Cu3 121.5(5) . . ? C20 N11 Cu3 120.3(4) . . ? N12 C30 C26 123.6(6) . . ? N24 C55 C51 122.7(5) . . ? C54 C53 C52 121.3(6) . . ? C47 C46 C50 117.3(6) . . ? C47 C46 N19 119.6(6) . . ? C50 C46 N19 123.1(5) . . ? N23 C50 C46 123.3(5) . . ? N11 C19 C18 123.2(7) . . ? C20 C16 N7 123.1(6) . . ? C20 C16 C17 118.6(6) . . ? N7 C16 C17 118.3(6) . . ? N24 C54 C53 121.6(6) . . ? N16 C39 C38 119.2(7) . . ? N16 C40 C36 123.3(6) . . ? C37 C38 C39 121.7(6) . . ? C38 C37 C36 118.7(6) . . ? N17 C35 C31 123.6(6) . . ? C46 C47 C48 119.8(7) . . ? C28 C27 C26 118.8(7) . . ? C19 C18 C17 118.9(7) . . ? C13 C12 C11 118.1(6) . . ? N12 C29 C28 122.4(6) . . ? N6 C4 C3 121.9(7) . . ? N23 C49 C48 122.3(7) . . ? N11 C20 C16 123.1(6) . . ? C18 C17 C16 117.3(6) . . ? C34 C33 C32 118.8(6) . . ? C27 C28 C29 120.6(6) . . ? C2 C3 C4 118.9(6) . . ? C49 C48 C47 119.5(7) . . ? O2 P2 N9 113.3(3) . . ? O2 P2 N7 114.4(3) . . ? N9 P2 N7 104.9(3) . . ? O2 P2 N8 113.3(3) . . ? N9 P2 N8 105.9(3) . . ? N7 P2 N8 104.1(3) . . ? C25 N10 C24 118.2(5) . . ? C25 N10 Cu2 123.3(4) . . ? C24 N10 Cu2 118.4(4) . . ? C31 N14 P3 127.0(5) . . ? C36 N13 P3 127.5(4) . . ? C21 N9 P2 128.1(4) . . ? N10 C25 C21 124.6(5) . . ? C56 N21 P4 125.9(4) . . ? C60 C56 C57 118.5(6) . . ? C60 C56 N21 122.4(5) . . ? C57 C56 N21 119.1(5) . . ? C26 N8 P2 128.4(5) . . ? C7 C6 N2 120.9(6) . . ? C7 C6 C10 116.6(6) . . ? N2 C6 C10 122.5(6) . . ? C1 N3 P1 126.4(4) . . ? C51 N20 P4 126.5(4) . . ? C55 C51 C52 118.9(5) . . ? C55 C51 N20 123.2(5) . . ? C52 C51 N20 117.9(5) . . ? C25 C21 C22 116.1(5) . . ? C25 C21 N9 123.5(5) . . ? C22 C21 N9 120.4(5) . . ? N22 C60 C56 122.4(6) . . ? C2 C1 C5 117.6(6) . . ? C2 C1 N3 119.0(6) . . ? C5 C1 N3 123.4(5) . . ? C23 C22 C21 120.2(6) . . ? N5 C10 C6 123.3(6) . . ? C58 C57 C56 118.8(6) . . ? N5 C9 C8 121.0(7) . . ? N22 C59 C58 120.5(6) . . ? C31 C32 C33 119.1(7) . . ? C22 C23 C24 120.0(6) . . ? C6 C7 C8 121.0(6) . . ? N10 C24 C23 120.7(6) . . ? C35 C31 C32 117.7(6) . . ? C35 C31 N14 123.8(6) . . ? C32 C31 N14 118.5(6) . . ? C3 C2 C1 119.9(7) . . ? C9 C8 C7 119.0(6) . . ? C57 C58 C59 121.0(6) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.026 _refine_diff_density_min -1.180 _refine_diff_density_rms 0.163 data_c:\xyr-1-10-\1 _database_code_depnum_ccdc_archive 'CCDC 765355' #TrackingRef '765355.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H17 N6 O2 P' _chemical_formula_weight 344.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.689(2) _cell_length_b 12.097(3) _cell_length_c 16.266(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1709.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.7600 _exptl_crystal_size_mid 0.5000 _exptl_crystal_size_min 0.1600 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.181 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9298 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _exptl_special_details ; ? ; _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_type 'Smart CCD' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13269 _diffrn_reflns_av_R_equivalents 0.0237 _diffrn_reflns_av_sigmaI/netI 0.0221 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3878 _reflns_number_gt 3681 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 2000)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1028P)^2^+0.3920P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(12) _refine_ls_number_reflns 3878 _refine_ls_number_parameters 212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1511 _refine_ls_wR_factor_gt 0.1453 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.61254(6) 0.64756(5) 0.22326(3) 0.03067(17) Uani 1 1 d . . . O1 O 0.68472(19) 0.54093(14) 0.24448(11) 0.0392(4) Uani 1 1 d . . . N1 N 0.4358(2) 0.63761(19) 0.18972(12) 0.0377(4) Uani 1 1 d . . . H1 H 0.4140 0.6751 0.1449 0.045 Uiso 1 1 calc R . . C1 C 0.3148(2) 0.57637(19) 0.22392(16) 0.0357(5) Uani 1 1 d . . . N2 N 0.6029(2) 0.73602(18) 0.29999(12) 0.0373(4) Uani 1 1 d . . . H2A H 0.5118 0.7658 0.3082 0.045 Uiso 1 1 calc R . . C10 C 0.8735(3) 0.7448(3) 0.34194(19) 0.0488(6) Uani 1 1 d . . . H10 H 0.8996 0.6998 0.2962 0.059 Uiso 1 1 calc R . . C11 C 0.7340(3) 0.6735(2) 0.07008(14) 0.0371(5) Uani 1 1 d . . . C13 C 0.8396(4) 0.7127(3) -0.06231(15) 0.0521(7) Uani 1 1 d . . . H13 H 0.8900 0.7625 -0.0986 0.062 Uiso 1 1 calc R . . N3 N 0.7030(3) 0.71454(17) 0.14927(12) 0.0382(4) Uani 1 1 d . . . H3A H 0.7347 0.7820 0.1604 0.046 Uiso 1 1 calc R . . N5 N 0.9884(3) 0.7799(3) 0.3911(2) 0.0630(7) Uani 1 1 d . . . C6 C 0.7185(3) 0.7707(2) 0.35406(14) 0.0380(5) Uani 1 1 d . . . C7 C 0.6816(4) 0.8329(3) 0.42270(16) 0.0529(7) Uani 1 1 d . . . H7 H 0.5777 0.8522 0.4340 0.064 Uiso 1 1 calc R . . C2 C 0.1687(3) 0.5839(3) 0.1886(2) 0.0555(7) Uani 1 1 d . . . H2 H 0.1517 0.6306 0.1426 0.067 Uiso 1 1 calc R . . C12 C 0.8073(4) 0.7424(3) 0.01496(16) 0.0515(7) Uani 1 1 d . . . H12 H 0.8362 0.8142 0.0328 0.062 Uiso 1 1 calc R . . C14 C 0.7992(4) 0.6115(3) -0.08747(17) 0.0598(8) Uani 1 1 d . . . H14 H 0.8204 0.5901 -0.1425 0.072 Uiso 1 1 calc R . . N4 N 0.2163(3) 0.4472(2) 0.3218(2) 0.0654(8) Uani 1 1 d . . . C5 C 0.3318(3) 0.5075(2) 0.29074(18) 0.0477(6) Uani 1 1 d . . . H5 H 0.4301 0.5026 0.3160 0.057 Uiso 1 1 calc R . . C4 C 0.0780(4) 0.4569(3) 0.2862(3) 0.0722(12) Uani 1 1 d . . . H4 H -0.0050 0.4149 0.3079 0.087 Uiso 1 1 calc R . . C8 C 0.7987(5) 0.8664(4) 0.4744(2) 0.0738(10) Uani 1 1 d . . . H8 H 0.7753 0.9074 0.5226 0.089 Uiso 1 1 calc R . . C3 C 0.0505(3) 0.5235(3) 0.2208(3) 0.0665(10) Uani 1 1 d . . . H3 H -0.0497 0.5281 0.1976 0.080 Uiso 1 1 calc R . . C15 C 0.6947(4) 0.5684(2) 0.04395(16) 0.0490(7) Uani 1 1 d . . . H15 H 0.6455 0.5182 0.0803 0.059 Uiso 1 1 calc R . . N6 N 0.7281(5) 0.5376(3) -0.03584(19) 0.0707(9) Uani 1 1 d . . . C9 C 0.9463(4) 0.8410(4) 0.4566(2) 0.0695(10) Uani 1 1 d . . . H9 H 1.0247 0.8677 0.4922 0.083 Uiso 1 1 calc R . . O2 O 0.6955(3) 0.3286(2) 0.16917(15) 0.0662(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0257(2) 0.0374(3) 0.0289(3) 0.0041(2) 0.00255(19) -0.0011(2) O1 0.0324(8) 0.0404(9) 0.0449(9) 0.0063(7) 0.0010(7) 0.0032(7) N1 0.0295(9) 0.0486(11) 0.0350(9) 0.0098(9) -0.0037(7) -0.0023(8) C1 0.0256(10) 0.0383(11) 0.0433(11) -0.0042(10) 0.0011(9) -0.0002(8) N2 0.0283(9) 0.0524(11) 0.0311(8) -0.0030(8) 0.0041(7) 0.0023(8) C10 0.0369(13) 0.0568(15) 0.0526(14) -0.0039(12) -0.0025(11) -0.0010(12) C11 0.0378(11) 0.0423(12) 0.0311(10) 0.0020(9) 0.0051(8) 0.0015(9) C13 0.0640(18) 0.0611(16) 0.0311(11) 0.0068(12) 0.0204(12) -0.0018(14) N3 0.0450(11) 0.0364(10) 0.0334(9) -0.0012(8) 0.0105(9) -0.0070(9) N5 0.0450(14) 0.0713(17) 0.0726(17) 0.0047(15) -0.0200(13) -0.0087(13) C6 0.0370(11) 0.0457(13) 0.0313(10) 0.0036(9) 0.0001(9) -0.0054(10) C7 0.0552(16) 0.0635(17) 0.0402(12) -0.0085(13) 0.0036(12) -0.0026(14) C2 0.0332(13) 0.0513(15) 0.082(2) -0.0009(15) -0.0122(13) 0.0033(11) C12 0.0639(18) 0.0501(14) 0.0404(14) 0.0043(11) 0.0145(13) -0.0055(14) C14 0.0638(19) 0.084(2) 0.0315(11) -0.0042(13) 0.0104(12) 0.0092(17) N4 0.0536(15) 0.0531(14) 0.089(2) 0.0155(14) 0.0256(15) -0.0058(12) C5 0.0362(12) 0.0529(15) 0.0541(14) 0.0095(12) 0.0051(11) -0.0056(11) C4 0.0395(14) 0.0517(16) 0.126(3) -0.007(2) 0.0313(18) -0.0090(12) C8 0.080(2) 0.088(3) 0.0534(17) -0.0190(18) -0.0118(17) -0.007(2) C3 0.0285(12) 0.0559(17) 0.115(3) -0.013(2) 0.0025(16) -0.0038(12) C15 0.0667(19) 0.0422(13) 0.0382(12) 0.0013(11) 0.0029(12) -0.0036(13) N6 0.089(2) 0.0673(18) 0.0552(15) -0.0086(13) -0.0051(15) 0.0066(17) C9 0.068(2) 0.074(2) 0.067(2) -0.0041(19) -0.0278(17) -0.0130(19) _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 P1 O1 1.4753(18) . ? P1 N1 1.634(2) . ? P1 N2 1.646(2) . ? P1 N3 1.650(2) . ? N1 C1 1.401(3) . ? C1 C5 1.377(4) . ? C1 C2 1.396(4) . ? N2 C6 1.399(3) . ? C10 N5 1.348(4) . ? C10 C6 1.397(4) . ? C11 C12 1.380(4) . ? C11 C15 1.384(4) . ? C11 N3 1.406(3) . ? C13 C12 1.337(4) . ? C13 C14 1.338(5) . ? N5 C9 1.347(5) . ? C6 C7 1.384(4) . ? C7 C8 1.381(5) . ? C2 C3 1.364(5) . ? C14 N6 1.373(5) . ? N4 C4 1.339(5) . ? N4 C5 1.340(3) . ? C4 C3 1.357(6) . ? C8 C9 1.350(6) . ? C15 N6 1.381(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 P1 N1 114.40(11) . . ? O1 P1 N2 114.38(11) . . ? N1 P1 N2 104.66(11) . . ? O1 P1 N3 113.42(11) . . ? N1 P1 N3 103.91(11) . . ? N2 P1 N3 104.96(11) . . ? C1 N1 P1 127.70(16) . . ? C5 C1 C2 117.5(2) . . ? C5 C1 N1 123.5(2) . . ? C2 C1 N1 119.0(2) . . ? C6 N2 P1 129.39(18) . . ? N5 C10 C6 124.1(3) . . ? C12 C11 C15 118.0(2) . . ? C12 C11 N3 118.1(2) . . ? C15 C11 N3 124.0(2) . . ? C12 C13 C14 118.6(3) . . ? C11 N3 P1 125.87(17) . . ? C9 N5 C10 116.2(3) . . ? C7 C6 C10 117.3(3) . . ? C7 C6 N2 120.2(2) . . ? C10 C6 N2 122.5(2) . . ? C8 C7 C6 118.7(3) . . ? C3 C2 C1 119.5(3) . . ? C13 C12 C11 123.1(3) . . ? C13 C14 N6 121.8(3) . . ? C4 N4 C5 117.4(3) . . ? N4 C5 C1 123.2(3) . . ? N4 C4 C3 123.3(3) . . ? C9 C8 C7 120.2(3) . . ? C4 C3 C2 119.1(3) . . ? N6 C15 C11 119.0(3) . . ? C14 N6 C15 119.6(3) . . ? N5 C9 C8 123.5(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.565 _refine_diff_density_min -0.529 _refine_diff_density_rms 0.171