Supplementary data for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Vadapalli Chandrasekhar' _publ_contact_author_address ; Department of Chemistry Indian Institute of Technology Kanpur 208 016 INDIA ; _publ_contact_author_email VC@IITK.AC.IN _publ_section_title ; Synthesis, Structure, Magnetism and Nuclease Activity of Tetranuclear Copper(II) Phosphonates Containing Ancillary 2,2'-Bipyridine or 1,10-Phenanthroline Ligands ; loop_ _publ_author_name 'Vadapalli Chandrasekhar' 'Ramachandran Azhakar' 'Ramamoorthy Boomishankar' 'Surajit Ghosh' 'Paul Kogerler' ; T.Senapati ; 'Alexander Steiner' 'Pakkirisamy Thilagar' 'Sandeep Verma' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 641412' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H62 Cl10 Cu4 N10 O12 P2' _chemical_formula_weight 1737.76 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.762(3) _cell_length_b 12.649(4) _cell_length_c 14.253(4) _cell_angle_alpha 67.88(3) _cell_angle_beta 72.84(3) _cell_angle_gamma 84.47(3) _cell_volume 1717.2(8) _cell_formula_units_Z 1 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelopiped _exptl_crystal_colour blue _exptl_crystal_size_max .1 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 1.723 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10919 _diffrn_reflns_av_R_equivalents 0.0747 _diffrn_reflns_av_sigmaI/netI 0.1121 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 24.27 _reflns_number_total 5117 _reflns_number_gt 2857 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0752P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5117 _refine_ls_number_parameters 421 _refine_ls_number_restraints 71 _refine_ls_R_factor_all 0.0955 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1346 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 0.833 _refine_ls_restrained_S_all 0.829 _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 Cu1 Cu -0.03338(8) 0.80276(6) 0.50444(6) 0.0412(2) Uani 1 1 d . . . Cu2 Cu 0.24842(8) 0.92567(6) 0.46385(6) 0.0473(3) Uani 1 1 d . . . N1 N -0.0182(5) 0.7277(4) 0.4001(4) 0.0405(12) Uani 1 1 d . . . N2 N -0.1597(5) 0.6722(4) 0.5940(4) 0.0412(13) Uani 1 1 d . . . N3 N 0.3709(5) 0.9338(4) 0.3268(4) 0.0495(14) Uani 1 1 d . . . N4 N 0.3654(5) 1.0569(4) 0.4366(4) 0.0428(13) Uani 1 1 d . . . N10 N 0.5279(7) 0.3019(5) 0.9867(5) 0.0571(16) Uani 1 1 d . . . O1 O -0.0763(4) 0.8582(3) 0.6178(3) 0.0425(10) Uani 1 1 d . . . O2 O 0.1424(4) 0.9484(4) 0.5859(3) 0.0498(11) Uani 1 1 d . . . O3 O -0.0656(4) 1.0605(3) 0.6035(3) 0.0458(11) Uani 1 1 d . . . O11 O 0.4621(6) 0.3170(5) 0.9238(4) 0.0817(17) Uani 1 1 d . . . O12 O 0.4827(6) 0.3237(5) 1.0676(4) 0.0836(17) Uani 1 1 d . . . O13 O 0.6380(6) 0.2665(5) 0.9641(5) 0.0850(17) Uani 1 1 d . . . P1 P -0.00422(17) 0.94170(13) 0.63797(12) 0.0398(4) Uani 1 1 d . C . C1 C -0.0255(7) 0.8944(6) 0.7771(5) 0.0594(19) Uani 1 1 d DU . . H1 H 0.0003 0.8135 0.7952 0.071 Uiso 1 1 calc R A 1 C2 C -0.1614(8) 0.8861(6) 0.8440(5) 0.064(2) Uani 1 1 d DU C . H2A H -0.2141 0.8420 0.8256 0.076 Uiso 1 1 calc R B 1 H2B H -0.1976 0.9627 0.8310 0.076 Uiso 1 1 calc R B 1 C3 C -0.1672(15) 0.8280(16) 0.9614(9) 0.090(5) Uiso 0.589(10) 1 d PDU C 1 H3A H -0.1472 0.7469 0.9777 0.108 Uiso 0.589(10) 1 calc PR C 1 H3B H -0.2549 0.8341 1.0052 0.108 Uiso 0.589(10) 1 calc PR C 1 C4 C -0.0663(13) 0.8874(17) 0.9860(14) 0.117(6) Uiso 0.589(10) 1 d PDU C 1 H4A H -0.0895 0.9676 0.9724 0.140 Uiso 0.589(10) 1 calc PR C 1 H4B H -0.0705 0.8507 1.0609 0.140 Uiso 0.589(10) 1 calc PR C 1 C5 C 0.0740(12) 0.8814(12) 0.9190(8) 0.068(4) Uiso 0.589(10) 1 d PDU C 1 H5A H 0.1353 0.9186 0.9362 0.082 Uiso 0.589(10) 1 calc PR C 1 H5B H 0.0996 0.8019 0.9310 0.082 Uiso 0.589(10) 1 calc PR C 1 C6 C 0.0709(12) 0.9444(10) 0.8047(8) 0.062(4) Uiso 0.589(10) 1 d PDU C 1 H6A H 0.0500 1.0245 0.7938 0.074 Uiso 0.589(10) 1 calc PR C 1 H6B H 0.1574 0.9422 0.7574 0.074 Uiso 0.589(10) 1 calc PR C 1 C3' C -0.1647(18) 0.8782(19) 0.9552(11) 0.071(6) Uiso 0.411(10) 1 d PDU C 2 H3'1 H -0.2535 0.8615 1.0021 0.085 Uiso 0.411(10) 1 calc PR C 2 H3'2 H -0.1355 0.9507 0.9522 0.085 Uiso 0.411(10) 1 calc PR C 2 C4' C -0.0719(18) 0.7801(19) 0.9971(16) 0.101(8) Uiso 0.411(10) 1 d PDU C 2 H4'1 H -0.0724 0.7735 1.0679 0.121 Uiso 0.411(10) 1 calc PR C 2 H4'2 H -0.1051 0.7077 1.0027 0.121 Uiso 0.411(10) 1 calc PR C 2 C5' C 0.0684(19) 0.800(2) 0.9256(14) 0.100(8) Uiso 0.411(10) 1 d PDU C 2 H5'1 H 0.1230 0.7364 0.9544 0.120 Uiso 0.411(10) 1 calc PR C 2 H5'2 H 0.1042 0.8705 0.9211 0.120 Uiso 0.411(10) 1 calc PR C 2 C6' C 0.0662(19) 0.8084(17) 0.8154(14) 0.092(7) Uiso 0.411(10) 1 d PDU C 2 H6'1 H 0.1534 0.8286 0.7663 0.111 Uiso 0.411(10) 1 calc PR C 2 H6'2 H 0.0411 0.7342 0.8190 0.111 Uiso 0.411(10) 1 calc PR C 2 C11 C 0.0601(7) 0.7611(5) 0.3017(5) 0.0459(16) Uani 1 1 d . . . H11 H 0.1059 0.8307 0.2747 0.055 Uiso 1 1 calc R . . C12 C 0.0776(7) 0.6990(6) 0.2375(5) 0.0519(17) Uani 1 1 d . . . H12 H 0.1350 0.7243 0.1691 0.062 Uiso 1 1 calc R . . C13 C 0.0066(7) 0.5975(6) 0.2783(5) 0.0535(18) Uani 1 1 d . . . H13 H 0.0155 0.5528 0.2369 0.064 Uiso 1 1 calc R . . C14 C -0.0757(7) 0.5626(5) 0.3780(5) 0.0453(16) Uani 1 1 d . . . H14 H -0.1229 0.4936 0.4057 0.054 Uiso 1 1 calc R . . C15 C -0.0895(6) 0.6293(5) 0.4381(5) 0.0374(15) Uani 1 1 d . . . C16 C -0.1733(6) 0.5990(5) 0.5479(5) 0.0403(15) Uani 1 1 d . . . C17 C -0.2591(7) 0.5068(5) 0.5995(5) 0.0472(17) Uani 1 1 d . . . H17 H -0.2672 0.4576 0.5659 0.057 Uiso 1 1 calc R . . C18 C -0.3326(7) 0.4891(6) 0.7017(6) 0.0554(19) Uani 1 1 d . . . H18 H -0.3916 0.4270 0.7384 0.066 Uiso 1 1 calc R . . C19 C -0.3202(7) 0.5613(5) 0.7501(5) 0.0507(17) Uani 1 1 d . . . H19 H -0.3699 0.5498 0.8196 0.061 Uiso 1 1 calc R . . C20 C -0.2310(7) 0.6530(5) 0.6927(5) 0.0482(17) Uani 1 1 d . . . H20 H -0.2212 0.7027 0.7252 0.058 Uiso 1 1 calc R . . C21 C 0.3700(7) 0.8657(6) 0.2739(6) 0.0583(19) Uani 1 1 d . . . H21 H 0.3151 0.8007 0.3087 0.070 Uiso 1 1 calc R . . C22 C 0.4439(8) 0.8849(7) 0.1729(6) 0.068(2) Uani 1 1 d . . . H22 H 0.4383 0.8358 0.1384 0.082 Uiso 1 1 calc R . . C23 C 0.5278(8) 0.9796(7) 0.1223(6) 0.067(2) Uani 1 1 d . . . H23 H 0.5797 0.9955 0.0526 0.080 Uiso 1 1 calc R . . C24 C 0.5344(7) 1.0497(6) 0.1746(5) 0.0597(19) Uani 1 1 d . . . H24 H 0.5926 1.1124 0.1420 0.072 Uiso 1 1 calc R . . C25 C 0.4548(7) 1.0269(5) 0.2755(5) 0.0491(17) Uani 1 1 d . . . C26 C 0.4542(6) 1.0931(5) 0.3409(5) 0.0457(16) Uani 1 1 d . . . C27 C 0.5375(7) 1.1858(6) 0.3097(6) 0.0573(19) Uani 1 1 d . . . H27 H 0.5971 1.2114 0.2422 0.069 Uiso 1 1 calc R . . C28 C 0.5309(8) 1.2393(6) 0.3798(6) 0.063(2) Uani 1 1 d . . . H28 H 0.5856 1.3022 0.3603 0.075 Uiso 1 1 calc R . . C29 C 0.4430(8) 1.1991(6) 0.4789(6) 0.058(2) Uani 1 1 d . . . H29 H 0.4391 1.2326 0.5284 0.070 Uiso 1 1 calc R . . C30 C 0.3617(7) 1.1098(5) 0.5039(5) 0.0495(17) Uani 1 1 d . . . H30 H 0.3007 1.0841 0.5707 0.059 Uiso 1 1 calc R . . C100 C 0.7318(9) 0.4806(9) 0.0417(7) 0.091(3) Uani 1 1 d . . . H10A H 0.6875 0.4171 0.0408 0.109 Uiso 1 1 calc R . . H10B H 0.6730 0.5456 0.0333 0.109 Uiso 1 1 calc R . . Cl1 Cl 0.20417(18) 0.72864(13) 0.52755(15) 0.0592(5) Uani 1 1 d . . . Cl11 Cl 0.8701(3) 0.5171(4) -0.0620(2) 0.1368(13) Uani 1 1 d . . . Cl12 Cl 0.7645(3) 0.4408(3) 0.1641(2) 0.1160(10) Uani 1 1 d . . . C200 C 0.6836(9) 0.6817(7) 0.2476(7) 0.083(3) Uani 1 1 d . . . H20A H 0.6320 0.7054 0.1970 0.099 Uiso 1 1 calc R . . H20B H 0.7588 0.6399 0.2216 0.099 Uiso 1 1 calc R . . Cl21 Cl 0.5895(3) 0.5926(2) 0.36983(19) 0.0959(8) Uani 1 1 d . . . Cl22 Cl 0.7384(2) 0.80415(19) 0.25680(18) 0.0828(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0450(5) 0.0333(4) 0.0484(5) -0.0157(3) -0.0139(4) -0.0075(3) Cu2 0.0434(6) 0.0454(5) 0.0600(5) -0.0252(4) -0.0147(4) -0.0055(4) N1 0.032(3) 0.037(3) 0.053(3) -0.011(2) -0.020(3) -0.003(2) N2 0.044(3) 0.039(3) 0.044(3) -0.017(2) -0.014(3) 0.001(2) N3 0.044(4) 0.049(3) 0.064(4) -0.026(3) -0.022(3) 0.007(3) N4 0.042(3) 0.039(3) 0.053(3) -0.023(3) -0.016(3) 0.004(2) N10 0.062(5) 0.047(3) 0.058(4) -0.015(3) -0.013(4) -0.010(3) O1 0.044(3) 0.036(2) 0.052(2) -0.0185(19) -0.015(2) -0.0082(19) O2 0.042(3) 0.061(3) 0.057(3) -0.029(2) -0.017(2) -0.007(2) O3 0.052(3) 0.034(2) 0.052(3) -0.016(2) -0.014(2) -0.003(2) O11 0.088(5) 0.096(4) 0.083(4) -0.044(3) -0.043(4) 0.010(3) O12 0.107(5) 0.091(4) 0.070(4) -0.048(3) -0.027(3) 0.010(3) O13 0.064(4) 0.093(4) 0.088(4) -0.030(3) -0.010(3) -0.003(3) P1 0.0448(11) 0.0358(8) 0.0423(9) -0.0132(7) -0.0165(8) -0.0069(7) C1 0.061(5) 0.071(5) 0.046(4) -0.019(4) -0.018(4) 0.000(4) C2 0.086(6) 0.059(4) 0.039(4) -0.018(3) -0.004(4) -0.018(4) C11 0.047(4) 0.046(4) 0.046(4) -0.013(3) -0.017(3) -0.006(3) C12 0.047(5) 0.057(4) 0.047(4) -0.017(3) -0.009(3) -0.006(3) C13 0.054(5) 0.054(4) 0.062(5) -0.032(4) -0.020(4) 0.012(4) C14 0.054(5) 0.031(3) 0.056(4) -0.017(3) -0.021(3) 0.002(3) C15 0.040(4) 0.030(3) 0.045(4) -0.011(3) -0.019(3) -0.002(3) C16 0.036(4) 0.040(3) 0.051(4) -0.019(3) -0.018(3) 0.001(3) C17 0.052(5) 0.044(4) 0.046(4) -0.017(3) -0.009(3) -0.012(3) C18 0.045(5) 0.045(4) 0.073(5) -0.012(3) -0.018(4) -0.021(3) C19 0.047(5) 0.051(4) 0.055(4) -0.021(3) -0.011(3) -0.007(3) C20 0.051(5) 0.044(4) 0.054(4) -0.021(3) -0.014(3) -0.006(3) C21 0.048(5) 0.061(4) 0.086(6) -0.041(4) -0.034(4) 0.013(4) C22 0.060(6) 0.093(6) 0.075(5) -0.058(5) -0.024(4) 0.020(5) C23 0.057(6) 0.088(6) 0.066(5) -0.045(5) -0.017(4) 0.018(5) C24 0.052(5) 0.068(5) 0.049(4) -0.016(4) -0.006(4) -0.002(4) C25 0.051(5) 0.041(4) 0.059(4) -0.017(3) -0.021(4) 0.002(3) C26 0.036(4) 0.046(4) 0.054(4) -0.013(3) -0.018(3) -0.002(3) C27 0.048(5) 0.058(4) 0.063(4) -0.016(4) -0.018(4) -0.007(4) C28 0.071(6) 0.047(4) 0.075(5) -0.017(4) -0.028(4) -0.017(4) C29 0.069(6) 0.051(4) 0.072(5) -0.029(4) -0.031(4) -0.004(4) C30 0.045(5) 0.050(4) 0.057(4) -0.023(3) -0.014(3) -0.003(3) C100 0.066(6) 0.109(7) 0.111(7) -0.055(6) -0.024(5) 0.002(5) Cl1 0.0597(13) 0.0381(8) 0.0862(13) -0.0214(9) -0.0311(10) -0.0004(8) Cl11 0.104(2) 0.233(4) 0.0908(19) -0.081(2) -0.0187(16) -0.014(2) Cl12 0.120(2) 0.133(2) 0.0857(17) -0.0476(16) 0.0081(15) -0.0418(18) C200 0.090(7) 0.093(6) 0.103(7) -0.051(5) -0.063(6) 0.009(5) Cl21 0.0944(19) 0.1103(18) 0.0941(17) -0.0375(14) -0.0326(14) -0.0293(15) Cl22 0.0867(17) 0.0774(14) 0.0941(15) -0.0282(12) -0.0437(13) 0.0016(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.914(4) . ? Cu1 O3 1.969(4) 2_576 ? Cu1 N2 2.007(5) . ? Cu1 N1 2.007(5) . ? Cu1 Cl1 2.707(2) . ? Cu2 O2 1.885(4) . ? Cu2 N3 1.980(5) . ? Cu2 N4 2.030(5) . ? Cu2 Cl1 2.3520(19) . ? Cu2 O3 2.396(4) 2_576 ? N1 C11 1.334(8) . ? N1 C15 1.366(7) . ? N2 C20 1.330(8) . ? N2 C16 1.360(7) . ? N3 C21 1.344(8) . ? N3 C25 1.379(8) . ? N4 C30 1.349(7) . ? N4 C26 1.352(8) . ? N10 O13 1.220(8) . ? N10 O12 1.236(7) . ? N10 O11 1.249(8) . ? O1 P1 1.523(4) . ? O2 P1 1.528(5) . ? O3 P1 1.543(4) . ? O3 Cu1 1.969(4) 2_576 ? O3 Cu2 2.396(4) 2_576 ? P1 C1 1.791(6) . ? C1 C6' 1.456(15) . ? C1 C6 1.479(11) . ? C1 C2 1.480(9) . ? C2 C3 1.537(12) . ? C2 C3' 1.539(13) . ? C3 C4 1.564(14) . ? C4 C5 1.542(14) . ? C5 C6 1.529(12) . ? C3' C4' 1.565(16) . ? C4' C5' 1.534(16) . ? C5' C6' 1.540(15) . ? C11 C12 1.378(8) . ? C12 C13 1.391(9) . ? C13 C14 1.364(9) . ? C14 C15 1.383(8) . ? C15 C16 1.480(8) . ? C16 C17 1.384(8) . ? C17 C18 1.380(9) . ? C18 C19 1.371(9) . ? C19 C20 1.405(9) . ? C21 C22 1.365(10) . ? C22 C23 1.395(11) . ? C23 C24 1.374(9) . ? C24 C25 1.376(9) . ? C25 C26 1.468(9) . ? C26 C27 1.396(9) . ? C27 C28 1.386(9) . ? C28 C29 1.382(10) . ? C29 C30 1.368(9) . ? C100 Cl11 1.713(9) . ? C100 Cl12 1.757(10) . ? C200 Cl21 1.741(9) . ? C200 Cl22 1.771(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 O1 Cu1 O3 96.19(16) . 2_576 ? O1 Cu1 N2 89.65(18) . . ? O3 Cu1 N2 167.5(2) 2_576 . ? O1 Cu1 N1 169.60(19) . . ? O3 Cu1 N1 93.04(18) 2_576 . ? N2 Cu1 N1 80.38(19) . . ? O1 Cu1 Cl1 94.45(14) . . ? O3 Cu1 Cl1 83.25(14) 2_576 . ? N2 Cu1 Cl1 107.32(16) . . ? N1 Cu1 Cl1 91.36(15) . . ? O2 Cu2 N3 168.5(2) . . ? O2 Cu2 N4 89.40(19) . . ? N3 Cu2 N4 80.0(2) . . ? O2 Cu2 Cl1 95.39(14) . . ? N3 Cu2 Cl1 95.97(16) . . ? N4 Cu2 Cl1 150.23(16) . . ? O2 Cu2 O3 91.58(17) . 2_576 ? N3 Cu2 O3 91.26(19) . 2_576 ? N4 Cu2 O3 126.07(18) . 2_576 ? Cl1 Cu2 O3 83.25(11) . 2_576 ? C11 N1 C15 118.5(5) . . ? C11 N1 Cu1 126.1(4) . . ? C15 N1 Cu1 115.2(4) . . ? C20 N2 C16 118.3(5) . . ? C20 N2 Cu1 125.4(4) . . ? C16 N2 Cu1 116.2(4) . . ? C21 N3 C25 117.1(6) . . ? C21 N3 Cu2 126.4(5) . . ? C25 N3 Cu2 116.1(4) . . ? C30 N4 C26 118.5(5) . . ? C30 N4 Cu2 126.4(4) . . ? C26 N4 Cu2 115.1(4) . . ? O13 N10 O12 121.9(7) . . ? O13 N10 O11 117.5(7) . . ? O12 N10 O11 120.6(7) . . ? P1 O1 Cu1 130.7(3) . . ? P1 O2 Cu2 133.9(3) . . ? P1 O3 Cu1 122.9(3) . 2_576 ? P1 O3 Cu2 116.2(2) . 2_576 ? Cu1 O3 Cu2 99.30(17) 2_576 2_576 ? O1 P1 O2 114.0(2) . . ? O1 P1 O3 109.3(2) . . ? O2 P1 O3 111.1(3) . . ? O1 P1 C1 108.2(3) . . ? O2 P1 C1 106.4(3) . . ? O3 P1 C1 107.7(3) . . ? C6' C1 C6 69.5(10) . . ? C6' C1 C2 118.7(10) . . ? C6 C1 C2 116.4(7) . . ? C6' C1 P1 114.5(8) . . ? C6 C1 P1 113.5(6) . . ? C2 C1 P1 116.0(5) . . ? C1 C2 C3 110.6(8) . . ? C1 C2 C3' 110.5(9) . . ? C3 C2 C3' 22.8(9) . . ? C2 C3 C4 109.2(11) . . ? C5 C4 C3 112.4(13) . . ? C6 C5 C4 104.8(11) . . ? C1 C6 C5 112.5(9) . . ? C2 C3' C4' 107.5(13) . . ? C5' C4' C3' 112.8(16) . . ? C4' C5' C6' 107.8(15) . . ? C1 C6' C5' 110.4(13) . . ? N1 C11 C12 123.6(6) . . ? C11 C12 C13 117.2(6) . . ? C14 C13 C12 120.3(6) . . ? C13 C14 C15 119.7(6) . . ? N1 C15 C14 120.7(6) . . ? N1 C15 C16 114.6(5) . . ? C14 C15 C16 124.5(5) . . ? N2 C16 C17 122.4(6) . . ? N2 C16 C15 113.4(5) . . ? C17 C16 C15 124.2(5) . . ? C18 C17 C16 118.2(6) . . ? C19 C18 C17 120.5(6) . . ? C18 C19 C20 118.0(6) . . ? N2 C20 C19 122.5(6) . . ? N3 C21 C22 124.0(7) . . ? C21 C22 C23 117.9(7) . . ? C24 C23 C22 119.8(7) . . ? C23 C24 C25 119.1(7) . . ? C24 C25 N3 121.9(6) . . ? C24 C25 C26 124.6(6) . . ? N3 C25 C26 113.4(6) . . ? N4 C26 C27 121.3(6) . . ? N4 C26 C25 114.5(5) . . ? C27 C26 C25 124.2(6) . . ? C28 C27 C26 119.0(7) . . ? C29 C28 C27 119.2(6) . . ? C30 C29 C28 119.0(6) . . ? N4 C30 C29 122.8(6) . . ? Cl11 C100 Cl12 112.4(5) . . ? Cu2 Cl1 Cu1 82.27(7) . . ? Cl21 C200 Cl22 111.0(4) . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 24.27 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 0.741 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.091 #===END data_compound2 _database_code_depnum_ccdc_archive 'CCDC 641413' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H74 Cu4 N8 O18 P2' _chemical_formula_weight 1535.39 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' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.747(3) _cell_length_b 17.734(4) _cell_length_c 18.981(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.22(3) _cell_angle_gamma 90.00 _cell_volume 3832.9(15) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelopiped _exptl_crystal_colour blue _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 1.202 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19870 _diffrn_reflns_av_R_equivalents 0.1674 _diffrn_reflns_av_sigmaI/netI 0.1854 _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 -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.10 _diffrn_reflns_theta_max 22.49 _reflns_number_total 4978 _reflns_number_gt 2056 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0790P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4978 _refine_ls_number_parameters 490 _refine_ls_number_restraints 146 _refine_ls_R_factor_all 0.1686 _refine_ls_R_factor_gt 0.0782 _refine_ls_wR_factor_ref 0.1910 _refine_ls_wR_factor_gt 0.1611 _refine_ls_goodness_of_fit_ref 0.868 _refine_ls_restrained_S_all 0.874 _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 Cu1 Cu 0.57921(13) 0.58739(8) 0.60650(7) 0.0585(4) Uani 1 1 d . . . Cu2 Cu 0.31098(13) 0.52482(8) 0.55627(7) 0.0583(4) Uani 1 1 d . . . P1 P 0.5255(3) 0.41980(18) 0.56363(16) 0.0554(8) Uani 1 1 d . . . O1 O 0.6091(6) 0.4822(4) 0.6033(4) 0.0543(19) Uani 1 1 d . . . O2 O 0.3937(6) 0.4321(4) 0.5634(4) 0.056(2) Uani 1 1 d . . . O3 O 0.5391(7) 0.4093(4) 0.4860(3) 0.058(2) Uani 1 1 d . . . O4 O 0.4108(7) 0.5639(4) 0.6485(4) 0.067(2) Uani 1 1 d . . . O5 O 0.3016(8) 0.4945(5) 0.7028(5) 0.079(3) Uani 1 1 d . . . N1 N 0.5834(9) 0.6983(5) 0.6179(5) 0.057(2) Uani 1 1 d . . . N2 N 0.7117(9) 0.5958(6) 0.6971(5) 0.060(3) Uani 1 1 d . . . N3 N 0.2065(9) 0.6142(5) 0.5398(5) 0.060(3) Uani 1 1 d . . . N4 N 0.1779(8) 0.4851(6) 0.4760(5) 0.055(2) Uani 1 1 d . . . C1 C 0.5667(11) 0.3342(6) 0.6128(6) 0.054(3) Uani 1 1 d . . . H1 H 0.5109 0.2944 0.5895 0.065 Uiso 1 1 calc R . . C2 C 0.5618(11) 0.3397(6) 0.6921(6) 0.064(3) Uani 1 1 d . . . H2A H 0.4828 0.3554 0.6944 0.077 Uiso 1 1 calc R . . H2B H 0.6173 0.3784 0.7164 0.077 Uiso 1 1 calc R . . C3 C 0.5920(13) 0.2642(8) 0.7329(7) 0.080(4) Uani 1 1 d . . . H3A H 0.5334 0.2261 0.7112 0.096 Uiso 1 1 calc R . . H3B H 0.5901 0.2706 0.7839 0.096 Uiso 1 1 calc R . . C4 C 0.7156(13) 0.2375(9) 0.7286(7) 0.090(5) Uani 1 1 d . . . H4A H 0.7749 0.2730 0.7548 0.109 Uiso 1 1 calc R . . H4B H 0.7321 0.1880 0.7517 0.109 Uiso 1 1 calc R . . C5 C 0.7226(13) 0.2324(8) 0.6499(8) 0.088(4) Uani 1 1 d . . . H5A H 0.8019 0.2168 0.6481 0.106 Uiso 1 1 calc R . . H5B H 0.6673 0.1941 0.6246 0.106 Uiso 1 1 calc R . . C6 C 0.6941(10) 0.3071(7) 0.6122(6) 0.061(3) Uani 1 1 d . . . H6A H 0.7003 0.3027 0.5619 0.073 Uiso 1 1 calc R . . H6B H 0.7512 0.3449 0.6366 0.073 Uiso 1 1 calc R . . C11 C 0.7728(11) 0.5383(8) 0.7310(7) 0.069(3) Uani 1 1 d . . . H11 H 0.7579 0.4897 0.7112 0.082 Uiso 1 1 calc R . . C12 C 0.8597(13) 0.5482(9) 0.7961(7) 0.085(4) Uani 1 1 d . . . H12A H 0.9023 0.5070 0.8204 0.102 Uiso 1 1 calc R . . C13 C 0.8801(15) 0.6203(10) 0.8231(8) 0.102(5) Uani 1 1 d . . . H13 H 0.9376 0.6285 0.8665 0.122 Uiso 1 1 calc R . . C14 C 0.8172(13) 0.6810(9) 0.7873(8) 0.088(4) Uani 1 1 d . . . H14 H 0.8307 0.7303 0.8056 0.105 Uiso 1 1 calc R . . C15 C 0.7322(11) 0.6658(7) 0.7222(6) 0.061(3) Uani 1 1 d . . . C16 C 0.6583(11) 0.7234(7) 0.6788(7) 0.061(3) Uani 1 1 d . . . C17 C 0.6646(12) 0.8001(8) 0.6950(7) 0.077(4) Uani 1 1 d . . . H17 H 0.7179 0.8176 0.7371 0.092 Uiso 1 1 calc R . . C18 C 0.5909(13) 0.8516(8) 0.6481(9) 0.081(4) Uani 1 1 d . . . H18 H 0.5947 0.9036 0.6580 0.098 Uiso 1 1 calc R . . C19 C 0.5151(13) 0.8237(8) 0.5889(7) 0.081(4) Uani 1 1 d . . . H19 H 0.4643 0.8564 0.5569 0.097 Uiso 1 1 calc R . . C20 C 0.5116(12) 0.7481(7) 0.5750(7) 0.070(4) Uani 1 1 d . . . H20 H 0.4568 0.7300 0.5337 0.084 Uiso 1 1 calc R . . C21 C 0.2290(11) 0.6808(8) 0.5766(7) 0.067(3) Uani 1 1 d . . . H21 H 0.2949 0.6838 0.6164 0.081 Uiso 1 1 calc R . . C22 C 0.1605(14) 0.7429(8) 0.5586(8) 0.080(4) Uani 1 1 d . . . H22 H 0.1783 0.7882 0.5847 0.096 Uiso 1 1 calc R . . C23 C 0.0662(13) 0.7373(8) 0.5020(8) 0.077(4) Uani 1 1 d . . . H23 H 0.0180 0.7799 0.4885 0.093 Uiso 1 1 calc R . . C24 C 0.0380(11) 0.6726(8) 0.4636(7) 0.070(4) Uani 1 1 d . . . H24 H -0.0293 0.6703 0.4247 0.084 Uiso 1 1 calc R . . C25 C 0.1097(12) 0.6101(8) 0.4824(6) 0.069(4) Uani 1 1 d . . . C26 C 0.0944(11) 0.5373(7) 0.4489(6) 0.057(3) Uani 1 1 d . . . C27 C 0.0001(11) 0.5161(9) 0.3930(7) 0.071(4) Uani 1 1 d . . . H27 H -0.0580 0.5518 0.3732 0.085 Uiso 1 1 calc R . . C28 C -0.0101(12) 0.4454(9) 0.3665(7) 0.073(4) Uani 1 1 d . . . H28 H -0.0761 0.4318 0.3296 0.087 Uiso 1 1 calc R . . C29 C 0.0762(12) 0.3932(7) 0.3934(7) 0.065(3) Uani 1 1 d . . . H29 H 0.0722 0.3441 0.3744 0.078 Uiso 1 1 calc R . . C30 C 0.1696(12) 0.4157(8) 0.4497(6) 0.067(3) Uani 1 1 d . . . H30 H 0.2287 0.3806 0.4696 0.081 Uiso 1 1 calc R . . C31 C 0.3886(13) 0.5327(7) 0.7051(6) 0.064(3) Uani 1 1 d . . . C32 C 0.4780(12) 0.5493(7) 0.7760(6) 0.077(4) Uani 1 1 d . . . H32A H 0.5409 0.5125 0.7833 0.116 Uiso 1 1 calc R . . H32B H 0.4402 0.5465 0.8160 0.116 Uiso 1 1 calc R . . H32C H 0.5100 0.5994 0.7740 0.116 Uiso 1 1 calc R . . C41 C 0.0307(18) 0.1536(11) 0.3309(11) 0.147(9) Uani 1 1 d DU . . C42 C -0.0005(17) 0.1521(13) 0.2471(9) 0.151(8) Uani 1 1 d DU . . H42A H -0.0386 0.1990 0.2284 0.227 Uiso 1 1 calc R . . H42B H -0.0532 0.1103 0.2297 0.227 Uiso 1 1 calc R . . H42C H 0.0706 0.1459 0.2304 0.227 Uiso 1 1 calc R . . O41 O -0.0355(16) 0.1168(8) 0.3607(8) 0.174(6) Uani 1 1 d DU . . O42 O 0.0942(11) 0.2046(8) 0.3631(7) 0.133(4) Uani 1 1 d DU . . C51 C 0.2664(17) 0.1865(11) 0.5237(9) 0.143(7) Uani 1 1 d DU . . C52 C 0.358(2) 0.1399(15) 0.5800(13) 0.106(10) Uiso 0.578(19) 1 d PDU A 1 H52A H 0.4162 0.1194 0.5568 0.159 Uiso 0.578(19) 1 calc PR A 1 H52B H 0.3186 0.0989 0.5983 0.159 Uiso 0.578(19) 1 calc PR A 1 H52C H 0.3963 0.1722 0.6200 0.159 Uiso 0.578(19) 1 calc PR A 1 O51 O 0.2583(18) 0.2550(10) 0.5202(11) 0.102(7) Uiso 0.578(19) 1 d PDU A 1 O52 O 0.2053(18) 0.1468(12) 0.4699(10) 0.124(8) Uiso 0.578(19) 1 d PDU A 1 C52' C 0.272(6) 0.0990(14) 0.520(3) 0.19(2) Uiso 0.422(19) 1 d PDU A 2 H52D H 0.2235 0.0815 0.4745 0.291 Uiso 0.422(19) 1 calc PR A 2 H52E H 0.2441 0.0776 0.5601 0.291 Uiso 0.422(19) 1 calc PR A 2 H52F H 0.3528 0.0834 0.5248 0.291 Uiso 0.422(19) 1 calc PR A 2 O51' O 0.305(4) 0.221(2) 0.5835(17) 0.24(2) Uiso 0.422(19) 1 d PDU A 2 O52' O 0.198(3) 0.226(2) 0.4757(18) 0.193(17) Uiso 0.422(19) 1 d PDU A 2 C61 C -0.3082(16) 0.0293(15) 0.5525(11) 0.160(9) Uani 1 1 d DU . . C62 C -0.2088(16) 0.0217(12) 0.6256(13) 0.196(12) Uani 1 1 d DU . . H62A H -0.1533 0.0628 0.6289 0.294 Uiso 1 1 calc R . . H62B H -0.1683 -0.0259 0.6258 0.294 Uiso 1 1 calc R . . H62C H -0.2440 0.0236 0.6667 0.294 Uiso 1 1 calc R . . O61 O -0.2898(13) 0.0548(10) 0.4949(9) 0.184(7) Uani 1 1 d DU . . O62 O -0.4135(13) 0.0127(10) 0.5517(8) 0.177(6) Uani 1 1 d DU . . O70 O 0.2299(9) 0.3488(6) 0.6340(5) 0.113(4) Uani 1 1 d . . . O80 O -0.0552(12) 0.0683(6) 0.4889(8) 0.147(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 Cu1 0.0637(10) 0.0544(8) 0.0579(8) 0.0004(7) 0.0161(7) 0.0015(9) Cu2 0.0576(9) 0.0565(9) 0.0623(8) 0.0017(8) 0.0177(7) 0.0041(8) P1 0.063(2) 0.0503(18) 0.0554(18) 0.0047(15) 0.0187(15) 0.0041(18) O1 0.066(5) 0.042(4) 0.056(4) 0.003(4) 0.017(4) 0.005(4) O2 0.058(5) 0.038(4) 0.075(5) 0.006(3) 0.023(4) 0.004(4) O3 0.078(5) 0.051(4) 0.042(4) 0.004(4) 0.010(4) -0.003(4) O4 0.079(6) 0.071(6) 0.054(5) 0.002(4) 0.022(4) 0.015(5) O5 0.066(6) 0.095(7) 0.082(6) 0.000(5) 0.027(5) -0.013(6) N1 0.056(6) 0.058(6) 0.056(6) -0.004(5) 0.012(5) 0.005(6) N2 0.069(7) 0.054(7) 0.058(6) -0.002(5) 0.016(5) -0.004(6) N3 0.073(7) 0.052(6) 0.063(6) -0.003(5) 0.034(6) -0.005(5) N4 0.049(6) 0.052(6) 0.068(6) -0.008(5) 0.023(5) -0.007(5) C1 0.068(8) 0.040(6) 0.058(7) 0.005(5) 0.020(6) -0.004(6) C2 0.073(9) 0.051(7) 0.073(8) 0.013(6) 0.025(6) 0.011(7) C3 0.097(11) 0.078(10) 0.070(8) 0.022(7) 0.029(8) 0.006(8) C4 0.091(11) 0.103(12) 0.086(10) 0.031(9) 0.039(8) 0.025(9) C5 0.083(10) 0.081(10) 0.105(11) 0.018(9) 0.032(9) 0.024(9) C6 0.059(8) 0.065(8) 0.062(7) 0.008(6) 0.022(6) 0.010(7) C11 0.059(8) 0.072(9) 0.074(8) 0.007(7) 0.015(7) -0.006(8) C12 0.082(10) 0.083(11) 0.081(9) 0.002(8) 0.001(8) -0.002(9) C13 0.107(13) 0.095(12) 0.086(10) -0.022(10) -0.010(9) -0.002(11) C14 0.085(10) 0.069(10) 0.101(11) -0.017(9) 0.008(9) -0.005(9) C15 0.058(8) 0.067(9) 0.060(7) -0.004(7) 0.015(6) 0.001(7) C16 0.064(8) 0.055(8) 0.071(8) -0.003(7) 0.031(7) -0.005(7) C17 0.071(9) 0.064(9) 0.090(9) -0.020(8) 0.009(7) 0.003(8) C18 0.079(10) 0.053(8) 0.118(12) -0.002(9) 0.036(9) 0.011(8) C19 0.101(11) 0.062(9) 0.075(9) -0.001(7) 0.011(8) 0.002(8) C20 0.086(10) 0.059(9) 0.067(8) 0.001(7) 0.022(7) 0.006(8) C21 0.055(8) 0.076(9) 0.075(8) 0.003(8) 0.023(6) 0.007(8) C22 0.090(11) 0.075(10) 0.077(9) 0.001(8) 0.027(8) 0.016(9) C23 0.078(10) 0.055(9) 0.102(11) 0.007(8) 0.028(9) 0.009(8) C24 0.057(8) 0.068(9) 0.080(9) 0.022(8) 0.009(7) 0.012(8) C25 0.065(8) 0.101(11) 0.039(6) -0.005(7) 0.007(6) 0.003(8) C26 0.062(8) 0.060(8) 0.053(7) 0.001(6) 0.020(6) 0.006(7) C27 0.066(9) 0.087(11) 0.061(8) 0.011(8) 0.016(7) -0.008(8) C28 0.069(9) 0.089(11) 0.061(8) -0.006(8) 0.017(7) -0.025(9) C29 0.077(9) 0.055(8) 0.068(8) -0.004(6) 0.029(7) -0.007(7) C30 0.080(9) 0.066(8) 0.058(7) -0.004(7) 0.021(7) -0.007(8) C31 0.076(9) 0.058(8) 0.062(8) 0.000(7) 0.024(7) 0.008(8) C32 0.095(10) 0.081(10) 0.055(7) 0.003(6) 0.018(7) -0.007(8) C41 0.16(2) 0.115(16) 0.20(2) -0.046(15) 0.126(17) -0.066(14) C42 0.127(15) 0.22(2) 0.112(13) -0.036(14) 0.041(11) 0.011(16) O41 0.196(16) 0.129(12) 0.200(15) -0.023(10) 0.052(12) 0.000(11) O42 0.121(10) 0.132(11) 0.158(11) 0.014(9) 0.057(8) -0.010(9) C51 0.128(15) 0.190(19) 0.091(12) -0.033(13) -0.010(11) -0.035(15) C61 0.145(19) 0.21(2) 0.126(16) 0.083(16) 0.039(15) 0.057(18) C62 0.093(14) 0.102(15) 0.37(4) -0.03(2) 0.021(19) -0.019(13) O61 0.156(13) 0.197(16) 0.191(14) 0.068(12) 0.028(12) 0.046(11) O62 0.110(10) 0.240(18) 0.198(14) -0.013(12) 0.070(10) -0.001(12) O70 0.086(7) 0.123(9) 0.112(8) 0.052(7) -0.010(6) -0.022(7) O80 0.159(12) 0.093(9) 0.203(13) 0.011(8) 0.072(10) 0.022(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 O1 1.902(7) . ? Cu1 O3 1.954(7) 3_666 ? Cu1 N1 1.978(9) . ? Cu1 N2 2.022(9) . ? Cu1 O4 2.344(9) . ? Cu2 O2 1.898(7) . ? Cu2 O4 1.977(8) . ? Cu2 N3 1.982(10) . ? Cu2 N4 2.023(9) . ? Cu2 O3 2.409(8) 3_666 ? P1 O3 1.532(7) . ? P1 O1 1.547(8) . ? P1 O2 1.563(8) . ? P1 C1 1.786(10) . ? O3 Cu1 1.954(7) 3_666 ? O3 Cu2 2.409(8) 3_666 ? O4 C31 1.292(14) . ? O5 C31 1.218(14) . ? N1 C16 1.345(14) . ? N1 C20 1.348(14) . ? N2 C11 1.319(15) . ? N2 C15 1.329(15) . ? N3 C21 1.365(15) . ? N3 C25 1.370(14) . ? N4 C30 1.322(14) . ? N4 C26 1.356(14) . ? C1 C2 1.523(15) . ? C1 C6 1.573(16) . ? C2 C3 1.544(15) . ? C3 C4 1.549(18) . ? C4 C5 1.518(18) . ? C5 C6 1.505(16) . ? C11 C12 1.407(16) . ? C12 C13 1.375(19) . ? C13 C14 1.385(19) . ? C14 C15 1.410(17) . ? C15 C16 1.458(16) . ? C16 C17 1.392(16) . ? C17 C18 1.414(17) . ? C18 C19 1.345(17) . ? C19 C20 1.365(17) . ? C21 C22 1.357(17) . ? C22 C23 1.343(18) . ? C23 C24 1.356(17) . ? C24 C25 1.385(17) . ? C25 C26 1.431(17) . ? C26 C27 1.384(16) . ? C27 C28 1.344(17) . ? C28 C29 1.375(17) . ? C29 C30 1.388(16) . ? C31 C32 1.518(16) . ? C41 O42 1.235(13) . ? C41 O41 1.252(14) . ? C41 C42 1.542(19) . ? C51 O51 1.219(14) . ? C51 O52' 1.268(16) . ? C51 O51' 1.275(16) . ? C51 O52 1.302(14) . ? C51 C52 1.554(19) . ? C51 C52' 1.55(2) . ? C61 O61 1.249(13) . ? C61 O62 1.267(14) . ? C61 C62 1.584(19) . ? 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 Cu1 O3 95.6(3) . 3_666 ? O1 Cu1 N1 168.2(4) . . ? O3 Cu1 N1 93.5(4) 3_666 . ? O1 Cu1 N2 89.4(4) . . ? O3 Cu1 N2 172.3(4) 3_666 . ? N1 Cu1 N2 80.8(4) . . ? O1 Cu1 O4 90.9(3) . . ? O3 Cu1 O4 80.6(3) 3_666 . ? N1 Cu1 O4 98.0(3) . . ? N2 Cu1 O4 105.2(3) . . ? O2 Cu2 O4 93.4(3) . . ? O2 Cu2 N3 172.1(4) . . ? O4 Cu2 N3 93.9(4) . . ? O2 Cu2 N4 92.2(4) . . ? O4 Cu2 N4 165.8(4) . . ? N3 Cu2 N4 80.0(4) . . ? O2 Cu2 O3 92.4(3) . 3_666 ? O4 Cu2 O3 78.5(3) . 3_666 ? N3 Cu2 O3 92.0(3) . 3_666 ? N4 Cu2 O3 114.3(3) . 3_666 ? O3 P1 O1 110.6(4) . . ? O3 P1 O2 110.6(4) . . ? O1 P1 O2 114.3(4) . . ? O3 P1 C1 108.7(5) . . ? O1 P1 C1 107.2(5) . . ? O2 P1 C1 105.1(5) . . ? P1 O1 Cu1 128.1(4) . . ? P1 O2 Cu2 127.6(4) . . ? P1 O3 Cu1 129.9(5) . 3_666 ? P1 O3 Cu2 121.2(4) . 3_666 ? Cu1 O3 Cu2 95.9(3) 3_666 3_666 ? C31 O4 Cu2 112.9(8) . . ? C31 O4 Cu1 136.0(8) . . ? Cu2 O4 Cu1 97.4(3) . . ? C16 N1 C20 118.9(10) . . ? C16 N1 Cu1 114.6(8) . . ? C20 N1 Cu1 126.2(8) . . ? C11 N2 C15 121.2(10) . . ? C11 N2 Cu1 124.8(9) . . ? C15 N2 Cu1 114.0(8) . . ? C21 N3 C25 118.1(11) . . ? C21 N3 Cu2 125.2(9) . . ? C25 N3 Cu2 116.4(8) . . ? C30 N4 C26 120.9(10) . . ? C30 N4 Cu2 125.5(9) . . ? C26 N4 Cu2 113.6(7) . . ? C2 C1 C6 107.1(9) . . ? C2 C1 P1 113.0(8) . . ? C6 C1 P1 113.1(8) . . ? C1 C2 C3 112.3(10) . . ? C2 C3 C4 109.9(11) . . ? C5 C4 C3 110.4(11) . . ? C6 C5 C4 110.8(12) . . ? C5 C6 C1 111.5(10) . . ? N2 C11 C12 121.5(13) . . ? C13 C12 C11 117.7(14) . . ? C12 C13 C14 121.1(13) . . ? C13 C14 C15 117.3(13) . . ? N2 C15 C14 121.3(12) . . ? N2 C15 C16 114.9(11) . . ? C14 C15 C16 123.8(13) . . ? N1 C16 C17 120.0(12) . . ? N1 C16 C15 115.3(11) . . ? C17 C16 C15 124.7(12) . . ? C16 C17 C18 120.2(12) . . ? C19 C18 C17 117.7(13) . . ? C18 C19 C20 120.4(13) . . ? N1 C20 C19 122.8(12) . . ? C22 C21 N3 123.0(12) . . ? C23 C22 C21 117.6(14) . . ? C22 C23 C24 122.5(13) . . ? C23 C24 C25 119.0(12) . . ? N3 C25 C24 119.8(12) . . ? N3 C25 C26 113.0(12) . . ? C24 C25 C26 127.3(12) . . ? N4 C26 C27 118.2(11) . . ? N4 C26 C25 116.6(10) . . ? C27 C26 C25 125.2(12) . . ? C28 C27 C26 121.5(13) . . ? C27 C28 C29 119.9(12) . . ? C28 C29 C30 117.6(12) . . ? N4 C30 C29 121.9(12) . . ? O5 C31 O4 123.2(12) . . ? O5 C31 C32 122.1(12) . . ? O4 C31 C32 114.7(12) . . ? O42 C41 O41 121.7(17) . . ? O42 C41 C42 119.0(15) . . ? O41 C41 C42 116.1(16) . . ? O51 C51 O52' 52(2) . . ? O51 C51 O51' 64.5(19) . . ? O52' C51 O51' 113(2) . . ? O51 C51 O52 118.3(17) . . ? O52' C51 O52 66.6(17) . . ? O51' C51 O52 166(3) . . ? O51 C51 C52 126.9(15) . . ? O52' C51 C52 176(3) . . ? O51' C51 C52 67(2) . . ? O52 C51 C52 114.0(15) . . ? O51 C51 C52' 175(2) . . ? O52' C51 C52' 123(2) . . ? O51' C51 C52' 121(2) . . ? O52 C51 C52' 56.7(19) . . ? C52 C51 C52' 57.8(19) . . ? O61 C61 O62 116.8(17) . . ? O61 C61 C62 123.2(16) . . ? O62 C61 C62 119.9(15) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.466 _refine_diff_density_min -0.548 _refine_diff_density_rms 0.084 #===END data_compound3 _database_code_depnum_ccdc_archive 'CCDC 641414' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H67 Cu4 N11 O22 P2' _chemical_formula_weight 1514.27 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.3151(10) _cell_length_b 15.0690(11) _cell_length_c 32.232(2) _cell_angle_alpha 81.0510(10) _cell_angle_beta 87.4410(10) _cell_angle_gamma 78.3510(10) _cell_volume 6256.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Parellelopiped _exptl_crystal_colour blue _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3112 _exptl_absorpt_coefficient_mu 1.478 _exptl_absorpt_correction_type emprical _exptl_absorpt_correction_T_min 0.807 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _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 'Bruker Smart Apex' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46469 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 4.09 _diffrn_reflns_theta_max 25.03 _reflns_number_total 21846 _reflns_number_gt 18154 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0906P)^2^+25.6735P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21846 _refine_ls_number_parameters 1652 _refine_ls_number_restraints 1866 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0646 _refine_ls_wR_factor_ref 0.1834 _refine_ls_wR_factor_gt 0.1749 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.028 _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 0.85865(5) 0.65105(4) 0.653805(19) 0.02360(14) Uani 1 1 d . . . Cu2 Cu 0.87990(5) 0.71984(4) 0.54228(2) 0.02568(15) Uani 1 1 d . . . Cu3 Cu 0.65913(5) 0.92355(4) 0.640615(19) 0.02354(14) Uani 1 1 d . . . Cu4 Cu 0.69287(5) 0.90191(5) 0.536014(19) 0.02591(15) Uani 1 1 d . . . Cu5 Cu 0.66602(5) 0.90188(5) 0.81929(2) 0.03501(17) Uani 1 1 d . . . Cu6 Cu 0.73205(7) 0.87375(8) 0.92717(3) 0.0606(3) Uani 1 1 d . . . Cu7 Cu 0.85181(5) 0.61919(5) 0.82908(2) 0.03114(16) Uani 1 1 d . . . Cu8 Cu 0.82837(7) 0.65397(8) 0.93387(3) 0.0627(3) Uani 1 1 d . . . P1 P 0.65207(10) 0.74303(10) 0.60561(4) 0.0241(3) Uani 1 1 d U B . P2 P 0.88459(10) 0.84410(9) 0.61209(4) 0.0233(3) Uani 1 1 d U . . P3 P 0.64898(12) 0.70957(13) 0.87085(5) 0.0402(4) Uani 1 1 d U . . P4 P 0.88129(11) 0.80847(11) 0.85223(4) 0.0315(3) Uani 1 1 d U . . O1 O 0.9298(3) 0.7996(3) 0.57449(11) 0.0277(7) Uani 1 1 d U . . O2 O 0.8798(3) 0.7750(2) 0.65225(11) 0.0249(7) Uani 1 1 d U . . O3 O 0.7781(3) 0.9055(3) 0.60267(11) 0.0255(7) Uani 1 1 d U . . O4 O 0.6329(3) 0.8003(2) 0.64181(11) 0.0254(7) Uani 1 1 d U . . O5 O 0.6321(3) 0.8019(3) 0.56283(11) 0.0283(7) Uani 1 1 d U . . O6 O 0.7607(3) 0.6835(2) 0.60819(11) 0.0258(7) Uani 1 1 d U . . O7 O 0.7284(3) 0.6760(3) 0.70657(11) 0.0298(8) Uani 1 1 d . . . O8 O 0.7431(3) 0.8843(3) 0.70215(11) 0.0287(7) Uani 1 1 d . . . O9 O 0.7897(3) 0.8190(3) 0.50919(11) 0.0294(8) Uani 1 1 d . . . H9 H 0.7940 0.8262 0.4794 0.035 Uiso 1 1 calc R . . O10 O 0.7048(3) 0.6717(3) 0.83258(12) 0.0358(8) Uani 1 1 d U . . O11 O 0.6448(3) 0.8121(3) 0.86784(13) 0.0421(10) Uani 1 1 d U . . O12 O 0.6952(4) 0.6565(4) 0.91163(14) 0.0515(11) Uani 1 1 d U . . O13 O 0.8897(3) 0.7041(3) 0.86237(12) 0.0344(8) Uani 1 1 d U . . O14 O 0.8506(3) 0.8538(3) 0.89069(13) 0.0405(9) Uani 1 1 d U . . O15 O 0.8103(3) 0.8495(3) 0.81448(11) 0.0315(8) Uani 1 1 d U . . O16 O 0.6277(3) 0.8100(3) 0.77001(12) 0.0342(8) Uani 1 1 d . . . O17 O 0.8626(3) 0.7065(3) 0.76590(11) 0.0310(8) Uani 1 1 d . . . O18 O 0.7740(4) 0.7576(5) 0.96037(15) 0.0724(16) Uani 1 1 d . . . H18 H 0.7679 0.7514 0.9901 0.087 Uiso 1 1 calc R . . N1 N 0.8660(4) 0.5166(3) 0.65549(15) 0.0302(9) Uani 1 1 d U . . N2 N 0.9825(3) 0.6021(3) 0.69032(14) 0.0286(9) Uani 1 1 d U . . N3 N 0.8272(3) 0.6226(3) 0.51933(14) 0.0302(9) Uani 1 1 d U . . N4 N 0.9831(3) 0.6083(3) 0.56677(14) 0.0279(9) Uani 1 1 d U . . N5 N 0.5246(3) 0.9606(3) 0.66951(14) 0.0263(9) Uani 1 1 d U . . N6 N 0.6488(3) 1.0602(3) 0.63207(14) 0.0283(9) Uani 1 1 d U . . N7 N 0.5654(3) 0.9945(3) 0.54594(14) 0.0278(9) Uani 1 1 d U . . N8 N 0.7414(3) 1.0181(3) 0.51289(13) 0.0278(9) Uani 1 1 d U . . N9 N 0.5243(4) 0.9770(4) 0.82281(17) 0.0425(12) Uani 1 1 d U . . N10 N 0.6834(4) 1.0138(4) 0.77872(16) 0.0398(11) Uani 1 1 d U . . N11 N 0.5918(5) 0.9007(8) 0.9530(2) 0.103(3) Uani 1 1 d U . . N12 N 0.6872(5) 1.0040(6) 0.8988(2) 0.073(2) Uani 1 1 d U . . N13 N 0.9713(5) 0.6407(8) 0.9529(2) 0.102(3) Uani 1 1 d U . . N14 N 0.8791(5) 0.5200(6) 0.9268(2) 0.076(2) Uani 1 1 d U . . N15 N 0.9938(4) 0.5400(3) 0.83222(15) 0.0336(10) Uani 1 1 d U . . N16 N 0.8237(4) 0.5104(4) 0.80694(16) 0.0384(11) Uani 1 1 d U . . C1 C 0.5596(4) 0.6686(4) 0.61189(17) 0.0291(11) Uani 1 1 d U . . H1 H 0.5796 0.6236 0.5917 0.035 Uiso 1 1 calc R A 1 C2 C 0.4478(10) 0.7257(9) 0.5995(4) 0.040(3) Uiso 0.518(8) 1 d PU B 1 H2A H 0.4283 0.7747 0.6172 0.048 Uiso 0.518(8) 1 calc PR B 1 H2B H 0.4487 0.7551 0.5698 0.048 Uiso 0.518(8) 1 calc PR B 1 C3 C 0.3667(11) 0.6634(10) 0.6053(5) 0.046(3) Uiso 0.518(8) 1 d PU B 1 H3A H 0.2972 0.7019 0.6010 0.055 Uiso 0.518(8) 1 calc PR B 1 H3B H 0.3788 0.6214 0.5841 0.055 Uiso 0.518(8) 1 calc PR B 1 C4 C 0.3722(11) 0.6090(10) 0.6481(5) 0.054(3) Uiso 0.518(8) 1 d PU B 1 H4A H 0.3214 0.5686 0.6504 0.064 Uiso 0.518(8) 1 calc PR B 1 H4B H 0.3527 0.6514 0.6690 0.064 Uiso 0.518(8) 1 calc PR B 1 C5 C 0.4776(11) 0.5502(10) 0.6590(5) 0.054(3) Uiso 0.518(8) 1 d PU B 1 H5A H 0.4965 0.5042 0.6397 0.065 Uiso 0.518(8) 1 calc PR B 1 H5B H 0.4772 0.5176 0.6881 0.065 Uiso 0.518(8) 1 calc PR B 1 C6 C 0.5555(9) 0.6151(8) 0.6544(4) 0.037(3) Uiso 0.518(8) 1 d PU B 1 H6A H 0.5373 0.6582 0.6750 0.044 Uiso 0.518(8) 1 calc PR B 1 H6B H 0.6246 0.5781 0.6614 0.044 Uiso 0.518(8) 1 calc PR B 1 C2' C 0.4513(10) 0.7178(9) 0.6179(4) 0.033(3) Uiso 0.482(8) 1 d PU B 2 H2'1 H 0.4310 0.7652 0.5933 0.040 Uiso 0.482(8) 1 calc PR B 2 H2'2 H 0.4471 0.7489 0.6430 0.040 Uiso 0.482(8) 1 calc PR B 2 C3' C 0.3771(11) 0.6505(10) 0.6235(5) 0.040(3) Uiso 0.482(8) 1 d PU B 2 H3'1 H 0.3910 0.6084 0.6503 0.048 Uiso 0.482(8) 1 calc PR B 2 H3'2 H 0.3056 0.6849 0.6245 0.048 Uiso 0.482(8) 1 calc PR B 2 C4' C 0.3895(11) 0.5959(10) 0.5877(4) 0.045(3) Uiso 0.482(8) 1 d PU B 2 H4'1 H 0.3668 0.6377 0.5615 0.054 Uiso 0.482(8) 1 calc PR B 2 H4'2 H 0.3443 0.5505 0.5929 0.054 Uiso 0.482(8) 1 calc PR B 2 C5' C 0.4984(11) 0.5462(10) 0.5815(5) 0.050(3) Uiso 0.482(8) 1 d PU B 2 H5'1 H 0.5025 0.5143 0.5567 0.060 Uiso 0.482(8) 1 calc PR B 2 H5'2 H 0.5197 0.4997 0.6064 0.060 Uiso 0.482(8) 1 calc PR B 2 C6' C 0.5702(11) 0.6149(9) 0.5751(4) 0.042(3) Uiso 0.482(8) 1 d PU B 2 H6'1 H 0.6420 0.5819 0.5728 0.050 Uiso 0.482(8) 1 calc PR B 2 H6'2 H 0.5531 0.6577 0.5487 0.050 Uiso 0.482(8) 1 calc PR B 2 C7 C 0.9725(4) 0.9163(4) 0.62139(17) 0.0273(10) Uani 1 1 d U . . H7 H 0.9668 0.9669 0.5970 0.033 Uiso 1 1 calc R . . C8 C 1.0846(4) 0.8651(4) 0.62272(19) 0.0314(11) Uani 1 1 d U . . H8A H 1.0947 0.8169 0.6476 0.038 Uiso 1 1 calc R . . H8B H 1.1009 0.8351 0.5973 0.038 Uiso 1 1 calc R . . C9 C 1.1567(4) 0.9311(4) 0.6247(2) 0.0355(12) Uani 1 1 d U . . H9A H 1.1504 0.9766 0.5988 0.043 Uiso 1 1 calc R . . H9B H 1.2284 0.8967 0.6265 0.043 Uiso 1 1 calc R . . C10 C 1.1310(5) 0.9807(5) 0.6628(2) 0.0414(13) Uani 1 1 d U . . H10A H 1.1460 0.9360 0.6888 0.050 Uiso 1 1 calc R . . H10B H 1.1750 1.0266 0.6623 0.050 Uiso 1 1 calc R . . C11 C 1.0193(5) 1.0283(4) 0.6635(2) 0.0400(13) Uani 1 1 d U . . H11A H 1.0063 1.0782 0.6393 0.048 Uiso 1 1 calc R . . H11B H 1.0044 1.0560 0.6895 0.048 Uiso 1 1 calc R . . C12 C 0.9480(4) 0.9615(4) 0.66131(18) 0.0322(11) Uani 1 1 d U . . H12A H 0.8758 0.9947 0.6609 0.039 Uiso 1 1 calc R . . H12B H 0.9572 0.9138 0.6864 0.039 Uiso 1 1 calc R . . C20 C 0.8018(5) 0.4795(4) 0.6358(2) 0.0421(14) Uani 1 1 d U . . H20 H 0.7467 0.5188 0.6204 0.051 Uiso 1 1 calc R . . C21 C 0.8133(5) 0.3864(5) 0.6374(3) 0.0524(17) Uani 1 1 d U . . H21 H 0.7664 0.3617 0.6234 0.063 Uiso 1 1 calc R . . C22 C 0.8928(6) 0.3300(5) 0.6593(2) 0.0508(16) Uani 1 1 d U . . H22 H 0.9023 0.2655 0.6604 0.061 Uiso 1 1 calc R . . C23 C 0.9599(5) 0.3673(4) 0.6800(2) 0.0466(15) Uani 1 1 d U . . H23 H 1.0151 0.3289 0.6957 0.056 Uiso 1 1 calc R . . C24 C 0.9446(5) 0.4613(4) 0.67719(18) 0.0347(12) Uani 1 1 d U . . C25 C 1.0126(5) 0.5100(4) 0.69583(18) 0.0350(12) Uani 1 1 d U . . C26 C 1.1045(5) 0.4671(5) 0.7157(2) 0.0461(14) Uani 1 1 d U . . H26 H 1.1252 0.4023 0.7195 0.055 Uiso 1 1 calc R . . C27 C 1.1644(5) 0.5200(5) 0.7298(2) 0.0469(15) Uani 1 1 d U . . H27 H 1.2278 0.4920 0.7429 0.056 Uiso 1 1 calc R . . C28 C 1.1330(5) 0.6132(5) 0.72494(19) 0.0401(13) Uani 1 1 d U . . H28 H 1.1736 0.6504 0.7349 0.048 Uiso 1 1 calc R . . C29 C 1.0408(4) 0.6522(4) 0.70521(17) 0.0337(12) Uani 1 1 d U . . H29 H 1.0181 0.7168 0.7022 0.040 Uiso 1 1 calc R . . C30 C 0.7433(4) 0.6375(4) 0.49575(18) 0.0355(12) Uani 1 1 d U . . H30 H 0.7093 0.6990 0.4870 0.043 Uiso 1 1 calc R . . C31 C 0.7043(5) 0.5682(5) 0.4838(2) 0.0455(15) Uani 1 1 d U . . H31 H 0.6450 0.5810 0.4669 0.055 Uiso 1 1 calc R . . C32 C 0.7531(6) 0.4801(5) 0.4968(2) 0.0497(16) Uani 1 1 d U . . H32 H 0.7272 0.4307 0.4891 0.060 Uiso 1 1 calc R . . C33 C 0.8404(5) 0.4620(5) 0.5213(2) 0.0431(14) Uani 1 1 d U . . H33 H 0.8745 0.4008 0.5306 0.052 Uiso 1 1 calc R . . C34 C 0.8762(4) 0.5358(4) 0.53182(17) 0.0310(11) Uani 1 1 d U . . C35 C 0.9675(4) 0.5273(4) 0.55763(17) 0.0295(11) Uani 1 1 d U . . C36 C 1.0319(5) 0.4453(4) 0.5720(2) 0.0395(13) Uani 1 1 d U . . H36 H 1.0189 0.3891 0.5657 0.047 Uiso 1 1 calc R . . C37 C 1.1157(5) 0.4462(5) 0.5958(2) 0.0454(14) Uani 1 1 d U . . H37 H 1.1610 0.3907 0.6061 0.054 Uiso 1 1 calc R . . C38 C 1.1325(5) 0.5293(5) 0.6042(2) 0.0415(13) Uani 1 1 d U . . H38 H 1.1899 0.5315 0.6202 0.050 Uiso 1 1 calc R . . C39 C 1.0657(4) 0.6081(4) 0.58925(17) 0.0324(11) Uani 1 1 d U . . H39 H 1.0782 0.6649 0.5950 0.039 Uiso 1 1 calc R . . C40 C 0.4674(4) 0.9035(4) 0.68926(17) 0.0312(11) Uani 1 1 d U . . H40 H 0.4886 0.8397 0.6883 0.037 Uiso 1 1 calc R . . C41 C 0.3786(4) 0.9335(4) 0.71109(19) 0.0355(12) Uani 1 1 d U . . H41 H 0.3402 0.8909 0.7253 0.043 Uiso 1 1 calc R . . C42 C 0.3466(4) 1.0253(4) 0.7120(2) 0.0380(13) Uani 1 1 d U . . H42 H 0.2854 1.0474 0.7266 0.046 Uiso 1 1 calc R . . C43 C 0.4040(4) 1.0853(4) 0.6915(2) 0.0365(12) Uani 1 1 d U . . H43 H 0.3826 1.1493 0.6916 0.044 Uiso 1 1 calc R . . C44 C 0.4941(4) 1.0511(4) 0.67054(18) 0.0314(11) Uani 1 1 d U . . C45 C 0.5625(4) 1.1078(4) 0.64806(18) 0.0313(11) Uani 1 1 d U . . C46 C 0.5425(5) 1.2027(4) 0.6429(2) 0.0447(14) Uani 1 1 d U . . H46 H 0.4813 1.2351 0.6541 0.054 Uiso 1 1 calc R . . C47 C 0.6121(5) 1.2495(5) 0.6213(2) 0.0479(15) Uani 1 1 d U . . H47 H 0.5991 1.3146 0.6173 0.057 Uiso 1 1 calc R . . C48 C 0.7010(5) 1.2008(4) 0.6055(2) 0.0425(14) Uani 1 1 d U . . H48 H 0.7503 1.2317 0.5907 0.051 Uiso 1 1 calc R . . C49 C 0.7169(4) 1.1062(4) 0.61167(18) 0.0329(12) Uani 1 1 d U . . H49 H 0.7782 1.0727 0.6010 0.039 Uiso 1 1 calc R . . C50 C 0.4786(4) 0.9749(4) 0.56438(17) 0.0306(11) Uani 1 1 d U . . H50 H 0.4738 0.9126 0.5726 0.037 Uiso 1 1 calc R . . C51 C 0.3959(4) 1.0427(4) 0.57174(18) 0.0366(12) Uani 1 1 d U . . H51 H 0.3354 1.0270 0.5851 0.044 Uiso 1 1 calc R . . C52 C 0.4022(4) 1.1326(5) 0.5596(2) 0.0400(13) Uani 1 1 d U . . H52 H 0.3467 1.1801 0.5651 0.048 Uiso 1 1 calc R . . C53 C 0.4902(5) 1.1537(4) 0.53928(19) 0.0366(12) Uani 1 1 d U . . H53 H 0.4949 1.2156 0.5295 0.044 Uiso 1 1 calc R . . C54 C 0.5714(4) 1.0826(4) 0.53347(16) 0.0286(11) Uani 1 1 d U . . C55 C 0.6727(4) 1.0967(4) 0.51454(17) 0.0291(11) Uani 1 1 d U . . C56 C 0.6966(5) 1.1815(4) 0.50202(19) 0.0361(12) Uani 1 1 d U . . H56 H 0.6464 1.2358 0.5027 0.043 Uiso 1 1 calc R . . C57 C 0.7960(5) 1.1857(4) 0.4883(2) 0.0394(13) Uani 1 1 d U . . H57 H 0.8149 1.2433 0.4797 0.047 Uiso 1 1 calc R . . C58 C 0.8667(5) 1.1061(4) 0.48717(19) 0.0372(12) Uani 1 1 d U . . H58 H 0.9353 1.1079 0.4781 0.045 Uiso 1 1 calc R . . C59 C 0.8366(4) 1.0235(4) 0.49945(17) 0.0321(11) Uani 1 1 d U . . H59 H 0.8854 0.9684 0.4983 0.039 Uiso 1 1 calc R . . C60 C 0.5179(5) 0.6962(7) 0.8693(3) 0.064(2) Uani 1 1 d U . . H60 H 0.4862 0.7414 0.8451 0.077 Uiso 1 1 calc R . . C61 C 0.4570(5) 0.7236(7) 0.9086(3) 0.067(2) Uani 1 1 d U . . H61A H 0.4678 0.7843 0.9134 0.081 Uiso 1 1 calc R . . H61B H 0.4819 0.6784 0.9335 0.081 Uiso 1 1 calc R . . C62 C 0.3414(7) 0.7276(9) 0.9030(4) 0.094(3) Uani 1 1 d U . . H62 H 0.2889 0.7800 0.9046 0.113 Uiso 1 1 calc R . . C63 C 0.3257(8) 0.6436(9) 0.8951(4) 0.109(4) Uani 1 1 d U . . H63A H 0.2515 0.6476 0.8912 0.131 Uiso 1 1 calc R . . H63B H 0.3475 0.5967 0.9198 0.131 Uiso 1 1 calc R . . C64 C 0.3852(7) 0.6129(9) 0.8556(4) 0.104(4) Uani 1 1 d U . . H64A H 0.3605 0.6569 0.8303 0.125 Uiso 1 1 calc R . . H64B H 0.3739 0.5517 0.8518 0.125 Uiso 1 1 calc R . . C65 C 0.5035(8) 0.6090(9) 0.8617(4) 0.104(3) Uani 1 1 d U . . H65A H 0.5293 0.5617 0.8858 0.125 Uiso 1 1 calc R . . H65B H 0.5425 0.5926 0.8362 0.125 Uiso 1 1 calc R . . C66 C 1.0081(5) 0.8299(5) 0.83759(19) 0.0380(13) Uani 1 1 d U . . H66 H 1.0563 0.7895 0.8588 0.046 Uiso 1 1 calc R . . C67 C 1.0464(5) 0.8046(5) 0.79436(18) 0.0373(12) Uani 1 1 d U . . H67A H 1.0441 0.7396 0.7936 0.045 Uiso 1 1 calc R . . H67B H 1.0009 0.8429 0.7722 0.045 Uiso 1 1 calc R . . C68 C 1.1556(5) 0.8193(6) 0.7859(2) 0.0528(17) Uani 1 1 d U . . H68A H 1.2021 0.7755 0.8061 0.063 Uiso 1 1 calc R . . H68B H 1.1772 0.8067 0.7573 0.063 Uiso 1 1 calc R . . C69 C 1.1650(6) 0.9144(6) 0.7897(2) 0.0569(17) Uani 1 1 d U . . H69A H 1.1246 0.9578 0.7674 0.068 Uiso 1 1 calc R . . H69B H 1.2377 0.9201 0.7856 0.068 Uiso 1 1 calc R . . C70 C 1.1271(6) 0.9399(6) 0.8325(2) 0.0536(16) Uani 1 1 d U . . H70A H 1.1302 1.0047 0.8333 0.064 Uiso 1 1 calc R . . H70B H 1.1720 0.9011 0.8548 0.064 Uiso 1 1 calc R . . C71 C 1.0162(5) 0.9260(5) 0.8406(2) 0.0491(15) Uani 1 1 d U . . H71A H 0.9934 0.9401 0.8690 0.059 Uiso 1 1 calc R . . H71B H 0.9705 0.9688 0.8198 0.059 Uiso 1 1 calc R . . C80 C 0.4483(5) 0.9529(5) 0.8472(2) 0.0497(16) Uani 1 1 d U . . H80 H 0.4592 0.8944 0.8641 0.060 Uiso 1 1 calc R . . C81 C 0.3533(5) 1.0107(6) 0.8486(3) 0.061(2) Uani 1 1 d U . . H81 H 0.3004 0.9925 0.8666 0.073 Uiso 1 1 calc R . . C82 C 0.3368(6) 1.0943(6) 0.8236(3) 0.068(2) Uani 1 1 d U . . H82 H 0.2717 1.1341 0.8239 0.081 Uiso 1 1 calc R . . C83 C 0.4139(6) 1.1206(6) 0.7983(3) 0.0589(19) Uani 1 1 d U . . H83 H 0.4034 1.1786 0.7809 0.071 Uiso 1 1 calc R . . C84 C 0.5086(5) 1.0602(5) 0.7985(2) 0.0474(16) Uani 1 1 d U . . C85 C 0.5987(5) 1.0818(5) 0.7740(2) 0.0461(15) Uani 1 1 d U . . C86 C 0.6013(6) 1.1647(5) 0.7489(2) 0.0565(18) Uani 1 1 d U . . H86 H 0.5413 1.2114 0.7454 0.068 Uiso 1 1 calc R . . C87 C 0.6920(6) 1.1790(5) 0.7288(2) 0.0568(18) Uani 1 1 d U . . H87 H 0.6950 1.2357 0.7117 0.068 Uiso 1 1 calc R . . C88 C 0.7781(6) 1.1099(5) 0.7340(2) 0.0505(16) Uani 1 1 d U . . H88 H 0.8413 1.1182 0.7206 0.061 Uiso 1 1 calc R . . C89 C 0.7699(5) 1.0287(5) 0.75893(19) 0.0419(14) Uani 1 1 d U . . H89 H 0.8289 0.9809 0.7622 0.050 Uiso 1 1 calc R . . C90 C 0.5504(8) 0.8412(13) 0.9786(3) 0.131(5) Uani 1 1 d U . . H90 H 0.5898 0.7822 0.9881 0.157 Uiso 1 1 calc R . . C91 C 0.4452(10) 0.8654(15) 0.9922(4) 0.160(6) Uani 1 1 d U . . H91 H 0.4144 0.8246 1.0118 0.192 Uiso 1 1 calc R . . C92 C 0.3908(8) 0.9514(15) 0.9752(4) 0.156(7) Uani 1 1 d U . . H92 H 0.3205 0.9686 0.9827 0.188 Uiso 1 1 calc R . . C93 C 0.4332(7) 1.0096(14) 0.9490(4) 0.158(6) Uani 1 1 d U . . H93 H 0.3939 1.0678 0.9381 0.189 Uiso 1 1 calc R . . C94 C 0.5363(7) 0.9856(11) 0.9375(3) 0.115(4) Uani 1 1 d U . . C95 C 0.5912(7) 1.0460(9) 0.9080(3) 0.100(4) Uani 1 1 d U . . C96 C 0.5536(8) 1.1384(9) 0.8912(4) 0.112(5) Uani 1 1 d U . . H96 H 0.4864 1.1687 0.8977 0.134 Uiso 1 1 calc R . . C97 C 0.6177(12) 1.1826(10) 0.8653(5) 0.128(5) Uani 1 1 d U . . H97 H 0.5938 1.2447 0.8533 0.153 Uiso 1 1 calc R . . C98 C 0.7121(10) 1.1417(8) 0.8563(4) 0.102(4) Uani 1 1 d U . . H98 H 0.7560 1.1738 0.8386 0.122 Uiso 1 1 calc R . . C99 C 0.7445(8) 1.0525(6) 0.8733(3) 0.075(2) Uani 1 1 d U . . H99 H 0.8120 1.0231 0.8665 0.090 Uiso 1 1 calc R . . C100 C 1.0085(8) 0.7077(12) 0.9645(3) 0.119(5) Uani 1 1 d U . . H100 H 0.9660 0.7666 0.9641 0.142 Uiso 1 1 calc R . . C101 C 1.1102(9) 0.6925(14) 0.9772(3) 0.146(6) Uani 1 1 d U . . H101 H 1.1378 0.7407 0.9851 0.175 Uiso 1 1 calc R . . C102 C 1.1675(8) 0.6092(13) 0.9780(3) 0.137(6) Uani 1 1 d U . . H102 H 1.2359 0.5983 0.9876 0.165 Uiso 1 1 calc R . . C103 C 1.1314(7) 0.5369(12) 0.9654(3) 0.133(5) Uani 1 1 d U . . H103 H 1.1745 0.4783 0.9657 0.159 Uiso 1 1 calc R . . C104 C 1.0283(6) 0.5536(9) 0.9520(3) 0.099(4) Uani 1 1 d U . . C105 C 0.9752(7) 0.4900(9) 0.9377(3) 0.096(3) Uani 1 1 d U . . C106 C 1.0255(9) 0.3972(9) 0.9346(3) 0.099(4) Uani 1 1 d U . . H106 H 1.0952 0.3740 0.9420 0.119 Uiso 1 1 calc R . . C107 C 0.9674(9) 0.3464(9) 0.9206(3) 0.102(4) Uani 1 1 d U . . H107 H 0.9979 0.2849 0.9178 0.122 Uiso 1 1 calc R . . C108 C 0.8673(10) 0.3764(9) 0.9101(3) 0.104(4) Uani 1 1 d U . . H108 H 0.8287 0.3369 0.9008 0.125 Uiso 1 1 calc R . . C109 C 0.8231(8) 0.4673(7) 0.9136(3) 0.077(2) Uani 1 1 d U . . H109 H 0.7534 0.4910 0.9064 0.092 Uiso 1 1 calc R . . C110 C 1.0776(5) 0.5601(5) 0.84687(19) 0.0401(13) Uani 1 1 d U . . H110 H 1.0728 0.6178 0.8560 0.048 Uiso 1 1 calc R . . C111 C 1.1718(5) 0.4993(5) 0.8492(2) 0.0469(15) Uani 1 1 d U . . H111 H 1.2302 0.5158 0.8594 0.056 Uiso 1 1 calc R . . C112 C 1.1793(5) 0.4161(6) 0.8365(2) 0.0544(17) Uani 1 1 d U . . H112 H 1.2430 0.3739 0.8377 0.065 Uiso 1 1 calc R . . C113 C 1.0932(5) 0.3939(5) 0.8218(2) 0.0496(15) Uani 1 1 d U . . H113 H 1.0963 0.3358 0.8133 0.060 Uiso 1 1 calc R . . C114 C 1.0021(5) 0.4579(4) 0.81976(19) 0.0389(13) Uani 1 1 d U . . C115 C 0.9046(5) 0.4416(5) 0.8047(2) 0.0426(14) Uani 1 1 d U . . C116 C 0.8951(7) 0.3626(5) 0.7898(3) 0.0630(19) Uani 1 1 d U . . H116 H 0.9531 0.3146 0.7884 0.076 Uiso 1 1 calc R . . C117 C 0.8009(7) 0.3543(6) 0.7771(3) 0.066(2) Uani 1 1 d U . . H117 H 0.7928 0.3001 0.7671 0.079 Uiso 1 1 calc R . . C118 C 0.7181(6) 0.4249(6) 0.7790(3) 0.0630(19) Uani 1 1 d U . . H118 H 0.6524 0.4204 0.7703 0.076 Uiso 1 1 calc R . . C119 C 0.7321(5) 0.5016(5) 0.7938(2) 0.0481(15) Uani 1 1 d U . . H119 H 0.6751 0.5507 0.7948 0.058 Uiso 1 1 calc R . . N30 N 0.0075(4) 0.7885(3) 0.45215(15) 0.0375(11) Uani 1 1 d DU . . O31 O 0.0720(4) 0.7710(4) 0.42433(16) 0.0643(14) Uani 1 1 d DU . . O32 O -0.0618(4) 0.8591(3) 0.44631(16) 0.0643(14) Uani 1 1 d DU . . O33 O 0.0126(3) 0.7371(3) 0.48614(12) 0.0360(8) Uani 1 1 d DU . . N40 N 0.5605(8) 0.4461(7) 0.5450(3) 0.049(3) Uani 0.50 1 d PDU C -1 O41 O 0.5584(6) 0.3702(6) 0.5310(3) 0.0384(18) Uani 0.50 1 d PDU C -1 O42 O 0.6198(8) 0.4504(7) 0.5729(3) 0.057(2) Uani 0.50 1 d PDU C -1 O43 O 0.4967(8) 0.5185(7) 0.5321(4) 0.068(3) Uani 0.50 1 d PDU C -1 N50 N 0.3465(7) 0.3279(7) 0.7102(3) 0.059(2) Uiso 0.676(9) 1 d PDU D 1 O51 O 0.4248(7) 0.3412(7) 0.7185(3) 0.085(3) Uiso 0.676(9) 1 d PDU D 1 O52 O 0.2936(8) 0.2985(7) 0.7393(3) 0.093(3) Uiso 0.676(9) 1 d PDU D 1 O53 O 0.3111(10) 0.3377(9) 0.6721(3) 0.107(4) Uiso 0.676(9) 1 d PDU D 1 N50' N 0.356(3) 0.365(3) 0.6243(12) 0.172(16) Uiso 0.324(9) 1 d PDU D 2 O51' O 0.428(3) 0.388(3) 0.6023(12) 0.194(16) Uiso 0.324(9) 1 d PDU D 2 O52' O 0.319(5) 0.303(4) 0.6146(19) 0.31(3) Uiso 0.324(9) 1 d PDU D 2 O53' O 0.349(3) 0.393(3) 0.6592(11) 0.180(14) Uiso 0.324(9) 1 d PDU D 2 N60 N 0.4556(6) 0.6705(7) 0.7565(3) 0.040(3) Uani 0.50 1 d PDU E 1 O61 O 0.4430(7) 0.7534(6) 0.7591(3) 0.049(2) Uani 0.50 1 d PDU E 1 O62 O 0.3781(8) 0.6361(9) 0.7567(4) 0.072(4) Uani 0.50 1 d PDU E 1 O63 O 0.5441(6) 0.6234(7) 0.7554(3) 0.052(2) Uani 0.50 1 d PDU E 1 N60' N 0.4815(9) 0.6339(8) 0.7371(4) 0.068(4) Uani 0.50 1 d PDU F 2 O61' O 0.4763(10) 0.7144(7) 0.7415(4) 0.078(4) Uani 0.50 1 d PDU F 2 O62' O 0.4005(8) 0.6026(9) 0.7421(4) 0.078(4) Uani 0.50 1 d PDU F 2 O63' O 0.5650(8) 0.5857(9) 0.7269(5) 0.089(4) Uani 0.50 1 d PDU F 2 N70 N 1.0109(8) 0.1534(7) 0.7806(3) 0.071(3) Uiso 0.706(7) 1 d PDU G 1 O71 O 1.0895(8) 0.1836(8) 0.7930(3) 0.100(3) Uiso 0.706(7) 1 d PDU G 1 O72 O 0.9454(8) 0.1405(8) 0.8060(3) 0.101(3) Uiso 0.706(7) 1 d PDU G 1 O73 O 1.0020(8) 0.1519(7) 0.7455(3) 0.087(3) Uiso 0.706(7) 1 d PDU G 1 N70' N 0.9722(19) 0.161(2) 0.8587(6) 0.093(8) Uiso 0.294(7) 1 d PDU G 2 O71' O 1.053(2) 0.176(3) 0.8396(10) 0.165(14) Uiso 0.294(7) 1 d PDU G 2 O72' O 0.9032(19) 0.1514(19) 0.8354(8) 0.106(8) Uiso 0.294(7) 1 d PDU G 2 O73' O 0.9707(13) 0.1341(12) 0.8956(5) 0.055(4) Uiso 0.294(7) 1 d PDU G 2 N80 N 0.2801(11) 0.2703(9) 0.9290(4) 0.088(4) Uiso 0.585(8) 1 d PDU H 1 O81 O 0.3073(9) 0.3404(7) 0.9344(3) 0.080(3) Uiso 0.585(8) 1 d PDU H 1 O82 O 0.2244(11) 0.2292(9) 0.9531(4) 0.102(4) Uiso 0.585(8) 1 d PDU H 1 O83 O 0.3055(10) 0.2336(9) 0.8959(4) 0.094(4) Uiso 0.585(8) 1 d PDU H 1 N80' N 0.203(2) 0.1450(17) 0.9305(9) 0.137(10) Uiso 0.415(8) 1 d PDU H 2 O81' O 0.1642(16) 0.0788(14) 0.9264(6) 0.109(6) Uiso 0.415(8) 1 d PDU H 2 O82' O 0.180(4) 0.182(3) 0.9622(11) 0.31(2) Uiso 0.415(8) 1 d PDU H 2 O83' O 0.217(3) 0.197(2) 0.8972(10) 0.243(16) Uiso 0.415(8) 1 d PDU H 2 O19 O 0.8258(7) 0.9435(8) 0.9743(3) 0.130(3) Uani 1 1 d . . . O20 O 0.1919(5) 1.2093(5) 0.6108(3) 0.103(2) Uani 1 1 d . . . O21 O 0.192(2) 0.2313(19) 0.7208(9) 0.184(9) Uiso 0.50 1 d PU . . O21' O 0.1609(9) 0.2021(8) 0.6962(4) 0.061(2) Uiso 0.50 1 d PU . . O22 O 0.8161(13) 0.1446(12) 0.9552(5) 0.110(5) Uiso 0.50 1 d P . . O22' O 0.4548(9) 0.3770(8) 0.8715(4) 0.064(3) Uiso 0.50 1 d P . . O23 O 0.4328(8) 0.4288(7) 0.7863(3) 0.051(2) Uiso 0.50 1 d P . . O23' O 0.5688(15) 0.4107(13) 0.6894(6) 0.127(5) Uiso 0.50 1 d P . . O24 O 0.616(2) 0.370(2) 0.9292(9) 0.173(8) Uiso 0.50 1 d PU . . O24' O 0.648(2) 0.3052(18) 0.9361(8) 0.155(7) Uiso 0.50 1 d PU . . O25 N 0.579(2) 0.4249(18) 0.9878(8) 0.084 Uiso 0.33 1 d P . . O25' O 0.6436(14) 0.5828(12) 0.9930(6) 0.064 Uiso 0.33 1 d PU . . O25" O 0.6236(16) 0.5432(14) 0.9810(6) 0.079 Uiso 0.33 1 d PU . . 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 0.0194(3) 0.0257(3) 0.0267(3) -0.0063(2) 0.0000(2) -0.0050(2) Cu2 0.0220(3) 0.0300(3) 0.0275(3) -0.0099(2) 0.0023(2) -0.0073(2) Cu3 0.0184(3) 0.0277(3) 0.0250(3) -0.0073(2) -0.0005(2) -0.0033(2) Cu4 0.0197(3) 0.0334(3) 0.0258(3) -0.0068(2) 0.0006(2) -0.0063(2) Cu5 0.0259(3) 0.0470(4) 0.0325(3) -0.0143(3) -0.0031(3) -0.0011(3) Cu6 0.0336(4) 0.1072(8) 0.0419(4) -0.0275(5) 0.0091(3) -0.0059(4) Cu7 0.0211(3) 0.0421(4) 0.0299(3) -0.0018(3) -0.0027(2) -0.0078(3) Cu8 0.0362(4) 0.1103(8) 0.0321(4) 0.0109(4) -0.0012(3) -0.0089(4) P1 0.0191(6) 0.0316(7) 0.0236(6) -0.0073(5) 0.0008(5) -0.0077(5) P2 0.0176(6) 0.0277(6) 0.0268(6) -0.0088(5) 0.0002(5) -0.0060(5) P3 0.0225(7) 0.0649(10) 0.0347(7) -0.0064(7) 0.0032(6) -0.0135(7) P4 0.0216(6) 0.0477(8) 0.0268(6) -0.0101(6) 0.0009(5) -0.0078(6) O1 0.0211(17) 0.0339(19) 0.0324(18) -0.0132(15) 0.0039(14) -0.0104(14) O2 0.0194(16) 0.0284(18) 0.0284(17) -0.0087(14) -0.0019(13) -0.0048(14) O3 0.0180(16) 0.0330(19) 0.0262(17) -0.0079(14) 0.0004(13) -0.0043(14) O4 0.0186(16) 0.0303(18) 0.0282(17) -0.0076(14) 0.0011(13) -0.0046(14) O5 0.0216(17) 0.039(2) 0.0273(17) -0.0052(15) -0.0015(13) -0.0112(15) O6 0.0213(17) 0.0313(18) 0.0271(17) -0.0111(14) 0.0016(13) -0.0061(14) O7 0.0231(17) 0.038(2) 0.0298(18) -0.0065(15) -0.0014(14) -0.0073(15) O8 0.0258(18) 0.0334(19) 0.0289(17) -0.0112(15) -0.0051(14) -0.0050(15) O9 0.0265(18) 0.035(2) 0.0261(17) -0.0082(15) 0.0013(14) -0.0030(15) O10 0.0222(18) 0.049(2) 0.036(2) -0.0063(17) 0.0002(15) -0.0086(16) O11 0.027(2) 0.066(3) 0.033(2) -0.0116(19) 0.0028(15) -0.0070(18) O12 0.040(2) 0.078(3) 0.034(2) 0.002(2) 0.0026(18) -0.016(2) O13 0.0248(18) 0.051(2) 0.0282(18) -0.0066(16) -0.0040(14) -0.0081(16) O14 0.028(2) 0.062(3) 0.035(2) -0.0147(18) 0.0023(16) -0.0106(18) O15 0.0259(18) 0.040(2) 0.0282(18) -0.0092(15) 0.0016(14) -0.0032(15) O16 0.0293(19) 0.046(2) 0.0287(18) -0.0115(16) 0.0010(15) -0.0066(16) O17 0.0229(18) 0.043(2) 0.0256(17) -0.0028(15) -0.0008(14) -0.0049(15) O18 0.066(3) 0.126(5) 0.032(2) -0.004(3) -0.001(2) -0.040(3) N1 0.028(2) 0.029(2) 0.035(2) -0.0064(18) 0.0075(18) -0.0084(18) N2 0.025(2) 0.032(2) 0.029(2) -0.0074(18) -0.0018(17) -0.0005(18) N3 0.027(2) 0.039(3) 0.028(2) -0.0129(18) 0.0067(17) -0.0112(19) N4 0.023(2) 0.033(2) 0.029(2) -0.0085(18) 0.0070(17) -0.0082(18) N5 0.019(2) 0.031(2) 0.029(2) -0.0093(17) -0.0027(16) -0.0021(17) N6 0.028(2) 0.030(2) 0.029(2) -0.0089(17) -0.0044(17) -0.0071(18) N7 0.019(2) 0.039(2) 0.027(2) -0.0082(18) -0.0023(16) -0.0067(18) N8 0.020(2) 0.038(2) 0.026(2) -0.0071(18) 0.0004(16) -0.0049(18) N9 0.029(2) 0.055(3) 0.047(3) -0.028(2) -0.006(2) 0.000(2) N10 0.040(3) 0.040(3) 0.040(3) -0.015(2) -0.013(2) -0.001(2) N11 0.034(3) 0.229(10) 0.067(4) -0.093(6) 0.016(3) -0.026(5) N12 0.045(3) 0.108(5) 0.071(4) -0.067(4) -0.020(3) 0.014(3) N13 0.037(4) 0.215(10) 0.034(3) 0.037(4) -0.003(3) -0.021(5) N14 0.045(4) 0.119(6) 0.043(3) 0.033(4) 0.008(3) -0.001(4) N15 0.026(2) 0.044(3) 0.031(2) 0.0014(19) -0.0016(18) -0.010(2) N16 0.029(2) 0.044(3) 0.043(3) -0.004(2) -0.008(2) -0.010(2) C1 0.025(3) 0.037(3) 0.029(2) -0.012(2) 0.005(2) -0.011(2) C7 0.021(2) 0.031(3) 0.032(3) -0.008(2) -0.0015(19) -0.007(2) C8 0.022(2) 0.034(3) 0.041(3) -0.006(2) 0.000(2) -0.011(2) C9 0.021(3) 0.041(3) 0.047(3) -0.007(2) -0.003(2) -0.010(2) C10 0.035(3) 0.047(3) 0.048(3) -0.009(3) -0.007(3) -0.020(3) C11 0.037(3) 0.043(3) 0.047(3) -0.018(3) -0.004(2) -0.014(3) C12 0.024(3) 0.038(3) 0.038(3) -0.015(2) -0.004(2) -0.006(2) C20 0.030(3) 0.039(3) 0.063(4) -0.016(3) 0.003(3) -0.014(2) C21 0.042(4) 0.038(3) 0.085(5) -0.019(3) 0.008(3) -0.019(3) C22 0.058(4) 0.027(3) 0.070(4) -0.011(3) 0.011(3) -0.014(3) C23 0.048(4) 0.031(3) 0.055(4) 0.000(3) 0.002(3) -0.001(3) C24 0.033(3) 0.031(3) 0.037(3) -0.001(2) 0.004(2) -0.003(2) C25 0.033(3) 0.036(3) 0.034(3) -0.006(2) 0.002(2) 0.000(2) C26 0.041(3) 0.039(3) 0.053(4) -0.004(3) -0.008(3) 0.003(3) C27 0.031(3) 0.053(4) 0.050(3) -0.007(3) -0.013(3) 0.010(3) C28 0.030(3) 0.052(4) 0.038(3) -0.015(3) -0.008(2) 0.000(3) C29 0.028(3) 0.043(3) 0.028(3) -0.009(2) 0.002(2) -0.003(2) C30 0.029(3) 0.046(3) 0.033(3) -0.016(2) 0.003(2) -0.007(2) C31 0.042(3) 0.067(4) 0.038(3) -0.019(3) 0.004(3) -0.027(3) C32 0.057(4) 0.059(4) 0.046(3) -0.025(3) 0.005(3) -0.033(3) C33 0.056(4) 0.039(3) 0.040(3) -0.013(3) 0.008(3) -0.020(3) C34 0.036(3) 0.036(3) 0.026(2) -0.015(2) 0.012(2) -0.012(2) C35 0.033(3) 0.028(3) 0.028(2) -0.008(2) 0.013(2) -0.008(2) C36 0.041(3) 0.033(3) 0.044(3) -0.008(2) 0.011(3) -0.008(2) C37 0.039(3) 0.043(3) 0.047(3) 0.002(3) 0.007(3) 0.000(3) C38 0.026(3) 0.050(4) 0.047(3) -0.004(3) -0.001(2) -0.007(3) C39 0.026(3) 0.039(3) 0.033(3) -0.008(2) 0.007(2) -0.009(2) C40 0.029(3) 0.032(3) 0.031(3) -0.007(2) 0.000(2) -0.002(2) C41 0.025(3) 0.044(3) 0.039(3) -0.013(2) 0.002(2) -0.008(2) C42 0.020(3) 0.047(3) 0.048(3) -0.019(3) 0.005(2) -0.003(2) C43 0.027(3) 0.032(3) 0.051(3) -0.018(2) 0.002(2) 0.000(2) C44 0.024(3) 0.038(3) 0.035(3) -0.014(2) -0.006(2) -0.004(2) C45 0.024(3) 0.034(3) 0.039(3) -0.017(2) -0.002(2) -0.003(2) C46 0.036(3) 0.038(3) 0.064(4) -0.021(3) 0.009(3) -0.008(3) C47 0.051(4) 0.034(3) 0.063(4) -0.018(3) 0.003(3) -0.012(3) C48 0.048(3) 0.042(3) 0.046(3) -0.015(3) 0.006(3) -0.024(3) C49 0.027(3) 0.043(3) 0.033(3) -0.015(2) 0.002(2) -0.012(2) C50 0.023(3) 0.043(3) 0.027(2) -0.006(2) -0.003(2) -0.009(2) C51 0.021(3) 0.054(4) 0.034(3) -0.002(2) -0.002(2) -0.008(2) C52 0.024(3) 0.046(3) 0.044(3) -0.002(3) -0.002(2) 0.006(2) C53 0.031(3) 0.038(3) 0.039(3) -0.001(2) -0.001(2) -0.006(2) C54 0.024(2) 0.035(3) 0.027(2) -0.005(2) -0.0040(19) -0.004(2) C55 0.026(3) 0.036(3) 0.027(2) -0.009(2) -0.002(2) -0.007(2) C56 0.030(3) 0.038(3) 0.041(3) -0.009(2) 0.000(2) -0.005(2) C57 0.037(3) 0.041(3) 0.043(3) -0.008(3) 0.003(2) -0.017(3) C58 0.027(3) 0.047(3) 0.040(3) -0.008(3) 0.005(2) -0.012(2) C59 0.023(3) 0.040(3) 0.033(3) -0.008(2) 0.001(2) -0.006(2) C60 0.032(3) 0.104(6) 0.070(5) -0.038(4) 0.014(3) -0.030(4) C61 0.033(3) 0.115(7) 0.060(4) -0.025(4) 0.017(3) -0.026(4) C62 0.043(4) 0.145(9) 0.113(7) -0.064(7) 0.029(5) -0.035(5) C63 0.059(5) 0.132(9) 0.155(9) -0.061(8) 0.061(6) -0.046(6) C64 0.050(5) 0.145(9) 0.151(9) -0.082(7) 0.039(5) -0.059(5) C65 0.061(5) 0.140(9) 0.129(8) -0.052(7) 0.046(5) -0.048(6) C66 0.029(3) 0.054(4) 0.035(3) -0.015(3) 0.001(2) -0.013(3) C67 0.031(3) 0.050(3) 0.034(3) -0.013(2) 0.004(2) -0.011(2) C68 0.041(4) 0.072(5) 0.056(4) -0.029(3) 0.019(3) -0.026(3) C69 0.052(4) 0.065(4) 0.058(4) -0.012(3) 0.014(3) -0.021(3) C70 0.047(4) 0.062(4) 0.059(4) -0.018(3) 0.011(3) -0.022(3) C71 0.039(3) 0.056(4) 0.053(4) -0.014(3) 0.002(3) -0.008(3) C80 0.031(3) 0.068(4) 0.056(4) -0.035(3) -0.006(3) -0.004(3) C81 0.032(3) 0.084(5) 0.077(5) -0.053(4) -0.004(3) -0.004(3) C82 0.039(4) 0.082(5) 0.086(5) -0.053(5) -0.018(4) 0.014(4) C83 0.046(4) 0.060(4) 0.071(5) -0.029(4) -0.020(3) 0.009(3) C84 0.039(3) 0.049(4) 0.057(4) -0.030(3) -0.018(3) 0.006(3) C85 0.046(4) 0.043(3) 0.053(4) -0.020(3) -0.020(3) -0.001(3) C86 0.065(4) 0.037(3) 0.069(4) -0.016(3) -0.032(4) 0.002(3) C87 0.074(5) 0.044(4) 0.058(4) -0.009(3) -0.025(4) -0.018(3) C88 0.060(4) 0.044(4) 0.050(4) -0.012(3) -0.015(3) -0.010(3) C89 0.043(3) 0.048(4) 0.038(3) -0.016(3) -0.006(3) -0.008(3) C90 0.054(5) 0.302(15) 0.080(6) -0.110(8) 0.038(5) -0.082(7) C91 0.079(7) 0.360(19) 0.103(8) -0.156(11) 0.046(6) -0.106(10) C92 0.043(6) 0.347(19) 0.123(9) -0.169(12) 0.022(5) -0.046(8) C93 0.034(5) 0.343(18) 0.122(8) -0.166(11) 0.003(5) 0.001(7) C94 0.036(4) 0.236(12) 0.088(6) -0.123(8) -0.014(4) 0.017(6) C95 0.051(5) 0.167(9) 0.087(6) -0.096(7) -0.028(4) 0.030(5) C96 0.069(6) 0.151(10) 0.113(8) -0.106(8) -0.048(5) 0.056(6) C97 0.130(10) 0.125(9) 0.127(10) -0.080(8) -0.054(8) 0.036(8) C98 0.118(8) 0.085(7) 0.096(7) -0.042(5) -0.050(6) 0.023(6) C99 0.074(6) 0.071(5) 0.084(6) -0.043(5) -0.027(4) 0.007(4) C100 0.061(5) 0.268(14) 0.035(4) 0.021(6) -0.010(4) -0.084(7) C101 0.068(6) 0.321(18) 0.047(5) 0.042(8) -0.013(5) -0.087(9) C102 0.053(6) 0.307(18) 0.044(5) 0.046(8) -0.013(4) -0.069(8) C103 0.045(5) 0.272(15) 0.052(5) 0.061(7) 0.000(4) -0.028(7) C104 0.033(4) 0.187(10) 0.042(4) 0.055(5) 0.007(3) 0.002(5) C105 0.058(5) 0.153(9) 0.048(4) 0.042(5) 0.015(4) 0.000(5) C106 0.077(6) 0.141(10) 0.051(5) 0.035(5) 0.011(4) 0.005(6) C107 0.093(7) 0.120(9) 0.065(6) 0.024(6) 0.019(5) 0.009(6) C108 0.106(8) 0.117(8) 0.065(5) 0.025(5) 0.022(5) 0.001(7) C109 0.071(5) 0.093(6) 0.054(4) 0.015(4) 0.010(4) -0.011(5) C110 0.029(3) 0.053(4) 0.039(3) -0.002(3) -0.004(2) -0.012(3) C111 0.027(3) 0.057(4) 0.056(4) -0.010(3) -0.008(3) -0.004(3) C112 0.032(3) 0.066(4) 0.061(4) -0.011(3) -0.010(3) 0.004(3) C113 0.042(4) 0.050(4) 0.055(4) -0.007(3) -0.011(3) -0.004(3) C114 0.033(3) 0.043(3) 0.038(3) 0.002(2) -0.007(2) -0.005(2) C115 0.041(3) 0.041(3) 0.045(3) -0.001(3) -0.012(3) -0.007(3) C116 0.061(4) 0.046(4) 0.083(5) -0.009(4) -0.025(4) -0.009(3) C117 0.065(5) 0.048(4) 0.091(6) -0.012(4) -0.025(4) -0.018(4) C118 0.044(4) 0.068(5) 0.083(5) -0.008(4) -0.023(4) -0.021(3) C119 0.035(3) 0.055(4) 0.057(4) -0.006(3) -0.012(3) -0.014(3) N30 0.036(3) 0.038(3) 0.038(3) -0.005(2) 0.013(2) -0.009(2) O31 0.056(3) 0.069(3) 0.053(3) -0.001(2) 0.031(2) 0.008(2) O32 0.065(3) 0.052(3) 0.056(3) 0.012(2) 0.029(2) 0.014(2) O33 0.030(2) 0.038(2) 0.040(2) -0.0047(17) 0.0089(16) -0.0079(16) N40 0.040(6) 0.060(7) 0.047(6) 0.001(5) 0.008(5) -0.018(5) O41 0.025(4) 0.049(5) 0.040(4) -0.026(4) 0.003(3) 0.007(3) O42 0.068(6) 0.070(6) 0.044(5) -0.011(4) -0.007(4) -0.039(5) O43 0.052(6) 0.071(7) 0.092(8) -0.031(6) 0.003(5) -0.025(5) N60 0.025(5) 0.060(8) 0.036(6) -0.005(5) -0.004(4) -0.013(5) O61 0.036(5) 0.043(6) 0.067(6) -0.001(4) -0.006(4) -0.007(4) O62 0.039(6) 0.115(10) 0.075(7) -0.038(7) -0.003(5) -0.023(6) O63 0.029(5) 0.088(7) 0.039(5) -0.008(5) -0.005(4) -0.010(5) N60' 0.053(8) 0.079(10) 0.068(9) 0.018(7) -0.016(7) -0.022(7) O61' 0.082(9) 0.039(6) 0.112(10) 0.020(6) -0.021(7) -0.029(6) O62' 0.052(7) 0.105(10) 0.091(9) -0.002(8) -0.006(6) -0.055(7) O63' 0.052(7) 0.106(10) 0.107(10) 0.027(8) -0.012(6) -0.039(7) O19 0.107(6) 0.215(10) 0.081(5) -0.058(5) -0.006(4) -0.035(6) O20 0.059(4) 0.079(4) 0.167(7) -0.013(4) 0.004(4) -0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.937(4) . ? Cu1 O6 1.948(4) . ? Cu1 N1 2.001(5) . ? Cu1 N2 2.016(4) . ? Cu1 O7 2.390(4) . ? Cu2 O9 1.925(4) . ? Cu2 O1 1.933(4) . ? Cu2 N3 1.997(5) . ? Cu2 N4 2.022(5) . ? Cu3 O4 1.952(4) . ? Cu3 O3 1.958(3) . ? Cu3 N5 2.000(4) . ? Cu3 N6 2.011(5) . ? Cu3 O8 2.258(4) . ? Cu4 O9 1.886(4) . ? Cu4 O5 1.923(4) . ? Cu4 N8 2.011(5) . ? Cu4 N7 2.016(5) . ? Cu5 O15 1.933(4) . ? Cu5 O11 1.953(5) . ? Cu5 N9 2.004(5) . ? Cu5 N10 2.013(6) . ? Cu5 O16 2.397(4) . ? Cu6 O18 1.897(7) . ? Cu6 O14 1.928(4) . ? Cu6 N11 2.002(7) . ? Cu6 N12 2.015(9) . ? Cu7 O13 1.944(4) . ? Cu7 O10 1.963(4) . ? Cu7 N16 1.993(5) . ? Cu7 N15 2.019(5) . ? Cu7 O17 2.262(4) . ? Cu8 O18 1.896(7) . ? Cu8 O12 1.933(5) . ? Cu8 N13 1.988(7) . ? Cu8 N14 2.041(9) . ? P1 O5 1.522(4) . ? P1 O6 1.538(4) . ? P1 O4 1.539(4) . ? P1 C1 1.811(6) . ? P2 O1 1.518(4) . ? P2 O2 1.538(4) . ? P2 O3 1.543(4) . ? P2 C7 1.814(5) . ? P3 O12 1.514(5) . ? P3 O11 1.522(5) . ? P3 O10 1.538(4) . ? P3 C60 1.801(7) . ? P4 O14 1.508(4) . ? P4 O13 1.539(5) . ? P4 O15 1.546(4) . ? P4 C66 1.812(6) . ? N1 C20 1.340(8) . ? N1 C24 1.346(8) . ? N2 C29 1.336(8) . ? N2 C25 1.350(7) . ? N3 C30 1.341(7) . ? N3 C34 1.347(8) . ? N4 C39 1.343(7) . ? N4 C35 1.356(7) . ? N5 C40 1.333(7) . ? N5 C44 1.347(7) . ? N6 C49 1.340(7) . ? N6 C45 1.353(7) . ? N7 C50 1.341(7) . ? N7 C54 1.343(7) . ? N8 C59 1.335(7) . ? N8 C55 1.349(7) . ? N9 C80 1.327(9) . ? N9 C84 1.355(9) . ? N10 C89 1.333(9) . ? N10 C85 1.359(8) . ? N11 C90 1.309(17) . ? N11 C94 1.374(17) . ? N12 C99 1.332(13) . ? N12 C95 1.350(10) . ? N13 C100 1.319(16) . ? N13 C104 1.381(15) . ? N14 C105 1.313(11) . ? N14 C109 1.318(13) . ? N15 C110 1.337(8) . ? N15 C114 1.342(8) . ? N16 C115 1.344(8) . ? N16 C119 1.346(8) . ? C1 C6 1.483(13) . ? C1 C2' 1.502(14) . ? C1 C6' 1.522(14) . ? C1 C2 1.597(14) . ? C2 C3 1.555(19) . ? C3 C4 1.487(19) . ? C4 C5 1.52(2) . ? C5 C6 1.551(18) . ? C2' C3' 1.540(19) . ? C3' C4' 1.50(2) . ? C4' C5' 1.51(2) . ? C5' C6' 1.53(2) . ? C7 C8 1.535(7) . ? C7 C12 1.540(7) . ? C8 C9 1.525(8) . ? C9 C10 1.525(9) . ? C10 C11 1.516(9) . ? C11 C12 1.527(8) . ? C20 C21 1.373(9) . ? C21 C22 1.364(11) . ? C22 C23 1.390(10) . ? C23 C24 1.379(9) . ? C24 C25 1.475(9) . ? C25 C26 1.396(9) . ? C26 C27 1.370(10) . ? C27 C28 1.368(9) . ? C28 C29 1.386(8) . ? C30 C31 1.367(9) . ? C31 C32 1.365(10) . ? C32 C33 1.392(10) . ? C33 C34 1.387(8) . ? C34 C35 1.477(8) . ? C35 C36 1.382(8) . ? C36 C37 1.385(10) . ? C37 C38 1.383(10) . ? C38 C39 1.366(9) . ? C40 C41 1.381(8) . ? C41 C42 1.368(9) . ? C42 C43 1.372(9) . ? C43 C44 1.395(8) . ? C44 C45 1.466(8) . ? C45 C46 1.385(9) . ? C46 C47 1.376(10) . ? C47 C48 1.382(10) . ? C48 C49 1.381(9) . ? C50 C51 1.382(8) . ? C51 C52 1.369(9) . ? C52 C53 1.387(9) . ? C53 C54 1.389(8) . ? C54 C55 1.497(8) . ? C55 C56 1.374(8) . ? C56 C57 1.386(9) . ? C57 C58 1.371(9) . ? C58 C59 1.379(9) . ? C60 C65 1.423(14) . ? C60 C61 1.539(10) . ? C61 C62 1.545(11) . ? C62 C63 1.387(15) . ? C63 C64 1.552(14) . ? C64 C65 1.585(13) . ? C66 C71 1.492(10) . ? C66 C67 1.540(8) . ? C67 C68 1.522(9) . ? C68 C69 1.488(10) . ? C69 C70 1.526(10) . ? C70 C71 1.538(10) . ? C80 C81 1.386(10) . ? C81 C82 1.368(13) . ? C82 C83 1.366(12) . ? C83 C84 1.398(9) . ? C84 C85 1.469(11) . ? C85 C86 1.385(10) . ? C86 C87 1.383(12) . ? C87 C88 1.381(11) . ? C88 C89 1.377(10) . ? C90 C91 1.441(15) . ? C91 C92 1.39(3) . ? C92 C93 1.31(2) . ? C93 C94 1.396(13) . ? C94 C95 1.483(19) . ? C95 C96 1.411(18) . ? C96 C97 1.36(2) . ? C97 C98 1.325(17) . ? C98 C99 1.359(14) . ? C100 C101 1.395(14) . ? C101 C102 1.33(2) . ? C102 C103 1.40(2) . ? C103 C104 1.419(13) . ? C104 C105 1.439(18) . ? C105 C106 1.439(16) . ? C106 C107 1.328(17) . ? C107 C108 1.358(16) . ? C108 C109 1.396(15) . ? C110 C111 1.393(9) . ? C111 C112 1.362(10) . ? C112 C113 1.379(10) . ? C113 C114 1.386(9) . ? C114 C115 1.485(9) . ? C115 C116 1.381(10) . ? C116 C117 1.372(11) . ? C117 C118 1.376(12) . ? C118 C119 1.364(11) . ? N30 O31 1.234(6) . ? N30 O33 1.235(6) . ? N30 O32 1.256(6) . ? N40 O42 1.240(10) . ? N40 O43 1.265(11) . ? N40 O41 1.299(10) . ? N50 O51 1.151(10) . ? N50 O52 1.228(10) . ? N50 O53 1.313(10) . ? N50' O51' 1.237(15) . ? N50' O52' 1.240(15) . ? N50' O53' 1.253(15) . ? N60 O61 1.241(11) . ? N60 O62 1.245(11) . ? N60 O63 1.249(10) . ? N60' O61' 1.231(12) . ? N60' O62' 1.256(11) . ? N60' O63' 1.261(12) . ? N70 O73 1.145(10) . ? N70 O72 1.193(10) . ? N70 O71 1.322(10) . ? N70' O73' 1.195(14) . ? N70' O72' 1.254(14) . ? N70' O71' 1.255(14) . ? N80 O81 1.223(11) . ? N80 O82 1.233(12) . ? N80 O83 1.278(12) . ? N80' O81' 1.236(14) . ? N80' O82' 1.239(15) . ? N80' O83' 1.261(15) . ? O21 O21' 1.10(3) . ? O24 O24' 0.97(3) . ? O25' O25" 0.85(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 O6 94.44(15) . . ? O2 Cu1 N1 169.08(17) . . ? O6 Cu1 N1 92.87(18) . . ? O2 Cu1 N2 90.48(17) . . ? O6 Cu1 N2 165.76(16) . . ? N1 Cu1 N2 80.56(19) . . ? O2 Cu1 O7 89.84(14) . . ? O6 Cu1 O7 93.28(14) . . ? N1 Cu1 O7 97.82(16) . . ? N2 Cu1 O7 100.10(16) . . ? O9 Cu2 O1 93.75(16) . . ? O9 Cu2 N3 94.04(18) . . ? O1 Cu2 N3 169.29(18) . . ? O9 Cu2 N4 169.49(16) . . ? O1 Cu2 N4 93.17(17) . . ? N3 Cu2 N4 80.19(19) . . ? O4 Cu3 O3 94.45(15) . . ? O4 Cu3 N5 90.38(17) . . ? O3 Cu3 N5 168.25(17) . . ? O4 Cu3 N6 164.49(17) . . ? O3 Cu3 N6 92.43(17) . . ? N5 Cu3 N6 80.41(19) . . ? O4 Cu3 O8 92.59(14) . . ? O3 Cu3 O8 98.29(14) . . ? N5 Cu3 O8 92.18(16) . . ? N6 Cu3 O8 100.16(16) . . ? O9 Cu4 O5 89.71(16) . . ? O9 Cu4 N8 98.71(17) . . ? O5 Cu4 N8 171.57(17) . . ? O9 Cu4 N7 160.46(17) . . ? O5 Cu4 N7 91.91(18) . . ? N8 Cu4 N7 80.32(18) . . ? O15 Cu5 O11 93.34(17) . . ? O15 Cu5 N9 170.1(2) . . ? O11 Cu5 N9 93.7(2) . . ? O15 Cu5 N10 90.89(19) . . ? O11 Cu5 N10 167.23(19) . . ? N9 Cu5 N10 80.8(2) . . ? O15 Cu5 O16 90.02(15) . . ? O11 Cu5 O16 93.27(17) . . ? N9 Cu5 O16 96.51(17) . . ? N10 Cu5 O16 98.77(17) . . ? O18 Cu6 O14 91.9(2) . . ? O18 Cu6 N11 95.8(4) . . ? O14 Cu6 N11 167.2(3) . . ? O18 Cu6 N12 172.7(2) . . ? O14 Cu6 N12 92.1(3) . . ? N11 Cu6 N12 81.3(4) . . ? O13 Cu7 O10 93.24(17) . . ? O13 Cu7 N16 166.36(19) . . ? O10 Cu7 N16 91.66(19) . . ? O13 Cu7 N15 92.66(18) . . ? O10 Cu7 N15 167.41(19) . . ? N16 Cu7 N15 80.2(2) . . ? O13 Cu7 O17 96.31(16) . . ? O10 Cu7 O17 90.19(15) . . ? N16 Cu7 O17 96.39(18) . . ? N15 Cu7 O17 100.20(16) . . ? O18 Cu8 O12 90.8(2) . . ? O18 Cu8 N13 95.5(4) . . ? O12 Cu8 N13 173.7(4) . . ? O18 Cu8 N14 159.3(2) . . ? O12 Cu8 N14 92.3(3) . . ? N13 Cu8 N14 82.1(4) . . ? O5 P1 O6 111.9(2) . . ? O5 P1 O4 112.3(2) . . ? O6 P1 O4 110.4(2) . . ? O5 P1 C1 106.1(2) . . ? O6 P1 C1 108.7(2) . . ? O4 P1 C1 107.1(2) . . ? O1 P2 O2 113.4(2) . . ? O1 P2 O3 111.9(2) . . ? O2 P2 O3 110.4(2) . . ? O1 P2 C7 104.8(2) . . ? O2 P2 C7 107.6(2) . . ? O3 P2 C7 108.4(2) . . ? O12 P3 O11 112.3(3) . . ? O12 P3 O10 111.5(3) . . ? O11 P3 O10 111.3(2) . . ? O12 P3 C60 108.4(4) . . ? O11 P3 C60 106.0(4) . . ? O10 P3 C60 107.1(3) . . ? O14 P4 O13 111.2(2) . . ? O14 P4 O15 113.3(2) . . ? O13 P4 O15 111.0(2) . . ? O14 P4 C66 105.6(3) . . ? O13 P4 C66 107.7(3) . . ? O15 P4 C66 107.7(3) . . ? P2 O1 Cu2 131.7(2) . . ? P2 O2 Cu1 125.1(2) . . ? P2 O3 Cu3 128.0(2) . . ? P1 O4 Cu3 126.4(2) . . ? P1 O5 Cu4 130.3(2) . . ? P1 O6 Cu1 130.8(2) . . ? Cu4 O9 Cu2 119.90(19) . . ? P3 O10 Cu7 125.5(2) . . ? P3 O11 Cu5 129.9(3) . . ? P3 O12 Cu8 128.0(3) . . ? P4 O13 Cu7 130.0(2) . . ? P4 O14 Cu6 137.4(3) . . ? P4 O15 Cu5 124.4(2) . . ? Cu8 O18 Cu6 119.6(3) . . ? C20 N1 C24 119.2(5) . . ? C20 N1 Cu1 125.2(4) . . ? C24 N1 Cu1 115.6(4) . . ? C29 N2 C25 119.1(5) . . ? C29 N2 Cu1 126.0(4) . . ? C25 N2 Cu1 114.6(4) . . ? C30 N3 C34 119.1(5) . . ? C30 N3 Cu2 124.7(4) . . ? C34 N3 Cu2 116.0(4) . . ? C39 N4 C35 118.4(5) . . ? C39 N4 Cu2 126.4(4) . . ? C35 N4 Cu2 115.2(4) . . ? C40 N5 C44 118.8(5) . . ? C40 N5 Cu3 125.5(4) . . ? C44 N5 Cu3 115.5(4) . . ? C49 N6 C45 118.8(5) . . ? C49 N6 Cu3 126.3(4) . . ? C45 N6 Cu3 114.8(4) . . ? C50 N7 C54 119.0(5) . . ? C50 N7 Cu4 125.4(4) . . ? C54 N7 Cu4 115.5(4) . . ? C59 N8 C55 118.3(5) . . ? C59 N8 Cu4 125.6(4) . . ? C55 N8 Cu4 115.9(4) . . ? C80 N9 C84 119.2(6) . . ? C80 N9 Cu5 125.8(5) . . ? C84 N9 Cu5 115.0(5) . . ? C89 N10 C85 118.6(6) . . ? C89 N10 Cu5 126.5(4) . . ? C85 N10 Cu5 114.8(5) . . ? C90 N11 C94 121.6(9) . . ? C90 N11 Cu6 124.7(10) . . ? C94 N11 Cu6 113.3(8) . . ? C99 N12 C95 117.8(10) . . ? C99 N12 Cu6 126.1(6) . . ? C95 N12 Cu6 116.1(9) . . ? C100 N13 C104 123.6(9) . . ? C100 N13 Cu8 124.0(9) . . ? C104 N13 Cu8 112.4(8) . . ? C105 N14 C109 122.6(11) . . ? C105 N14 Cu8 112.3(9) . . ? C109 N14 Cu8 125.2(6) . . ? C110 N15 C114 117.9(5) . . ? C110 N15 Cu7 126.5(5) . . ? C114 N15 Cu7 115.5(4) . . ? C115 N16 C119 118.5(6) . . ? C115 N16 Cu7 115.9(4) . . ? C119 N16 Cu7 125.5(5) . . ? C6 C1 C2' 89.5(8) . . ? C6 C1 C6' 116.5(8) . . ? C2' C1 C6' 112.1(8) . . ? C6 C1 C2 109.3(8) . . ? C2' C1 C2 21.7(5) . . ? C6' C1 C2 94.6(8) . . ? C6 C1 P1 114.7(6) . . ? C2' C1 P1 113.6(6) . . ? C6' C1 P1 109.3(6) . . ? C2 C1 P1 110.6(6) . . ? C3 C2 C1 111.5(10) . . ? C4 C3 C2 110.9(12) . . ? C3 C4 C5 113.9(12) . . ? C4 C5 C6 107.5(12) . . ? C1 C6 C5 114.0(10) . . ? C1 C2' C3' 110.9(10) . . ? C4' C3' C2' 110.4(12) . . ? C3' C4' C5' 113.5(12) . . ? C4' C5' C6' 109.7(12) . . ? C1 C6' C5' 110.1(10) . . ? C8 C7 C12 108.9(4) . . ? C8 C7 P2 112.4(4) . . ? C12 C7 P2 114.2(4) . . ? C9 C8 C7 110.6(5) . . ? C8 C9 C10 110.7(5) . . ? C11 C10 C9 111.6(5) . . ? C10 C11 C12 111.4(5) . . ? C11 C12 C7 109.7(5) . . ? N1 C20 C21 122.0(6) . . ? C22 C21 C20 119.1(7) . . ? C21 C22 C23 119.7(6) . . ? C24 C23 C22 118.5(6) . . ? N1 C24 C23 121.5(6) . . ? N1 C24 C25 114.3(5) . . ? C23 C24 C25 124.2(6) . . ? N2 C25 C26 121.0(6) . . ? N2 C25 C24 114.8(5) . . ? C26 C25 C24 124.1(6) . . ? C27 C26 C25 118.9(6) . . ? C28 C27 C26 120.1(6) . . ? C27 C28 C29 118.6(6) . . ? N2 C29 C28 122.3(6) . . ? N3 C30 C31 122.9(6) . . ? C32 C31 C30 118.2(6) . . ? C31 C32 C33 120.5(6) . . ? C34 C33 C32 118.2(6) . . ? N3 C34 C33 121.2(6) . . ? N3 C34 C35 114.5(5) . . ? C33 C34 C35 124.3(6) . . ? N4 C35 C36 121.8(6) . . ? N4 C35 C34 113.9(5) . . ? C36 C35 C34 124.2(5) . . ? C35 C36 C37 118.8(6) . . ? C38 C37 C36 119.0(6) . . ? C39 C38 C37 119.4(6) . . ? N4 C39 C38 122.4(6) . . ? N5 C40 C41 122.4(5) . . ? C42 C41 C40 119.2(6) . . ? C41 C42 C43 119.2(5) . . ? C42 C43 C44 119.3(6) . . ? N5 C44 C43 121.1(5) . . ? N5 C44 C45 114.5(5) . . ? C43 C44 C45 124.5(5) . . ? N6 C45 C46 121.4(5) . . ? N6 C45 C44 114.6(5) . . ? C46 C45 C44 124.0(5) . . ? C47 C46 C45 119.4(6) . . ? C46 C47 C48 119.3(6) . . ? C49 C48 C47 118.8(6) . . ? N6 C49 C48 122.4(5) . . ? N7 C50 C51 122.0(6) . . ? C52 C51 C50 119.2(6) . . ? C51 C52 C53 119.4(6) . . ? C52 C53 C54 118.6(6) . . ? N7 C54 C53 121.7(5) . . ? N7 C54 C55 114.5(5) . . ? C53 C54 C55 123.7(5) . . ? N8 C55 C56 122.5(5) . . ? N8 C55 C54 113.7(5) . . ? C56 C55 C54 123.7(5) . . ? C55 C56 C57 118.3(6) . . ? C58 C57 C56 119.6(6) . . ? C57 C58 C59 118.8(6) . . ? N8 C59 C58 122.5(5) . . ? C65 C60 C61 110.7(8) . . ? C65 C60 P3 115.9(7) . . ? C61 C60 P3 111.5(5) . . ? C60 C61 C62 110.3(7) . . ? C63 C62 C61 110.1(10) . . ? C62 C63 C64 112.7(9) . . ? C63 C64 C65 108.6(9) . . ? C60 C65 C64 109.3(9) . . ? C71 C66 C67 110.9(5) . . ? C71 C66 P4 111.9(4) . . ? C67 C66 P4 114.1(4) . . ? C68 C67 C66 110.4(5) . . ? C69 C68 C67 111.9(6) . . ? C68 C69 C70 111.7(6) . . ? C69 C70 C71 110.1(6) . . ? C66 C71 C70 110.9(6) . . ? N9 C80 C81 121.8(8) . . ? C82 C81 C80 119.2(8) . . ? C83 C82 C81 120.0(7) . . ? C82 C83 C84 118.5(8) . . ? N9 C84 C83 121.3(7) . . ? N9 C84 C85 114.9(6) . . ? C83 C84 C85 123.8(7) . . ? N10 C85 C86 121.0(7) . . ? N10 C85 C84 114.5(6) . . ? C86 C85 C84 124.5(7) . . ? C87 C86 C85 119.5(7) . . ? C88 C87 C86 119.3(7) . . ? C89 C88 C87 118.3(8) . . ? N10 C89 C88 123.4(7) . . ? N11 C90 C91 120.0(16) . . ? C92 C91 C90 116.7(16) . . ? C93 C92 C91 122.3(11) . . ? C92 C93 C94 119.7(17) . . ? N11 C94 C93 119.6(15) . . ? N11 C94 C95 116.4(8) . . ? C93 C94 C95 124.0(14) . . ? N12 C95 C96 120.7(13) . . ? N12 C95 C94 112.6(11) . . ? C96 C95 C94 126.6(10) . . ? C97 C96 C95 117.4(10) . . ? C98 C97 C96 122.0(14) . . ? C97 C98 C99 118.3(15) . . ? N12 C99 C98 123.9(10) . . ? N13 C100 C101 120.2(16) . . ? C102 C101 C100 118.6(16) . . ? C101 C102 C103 122.8(11) . . ? C102 C103 C104 118.0(15) . . ? N13 C104 C103 116.7(14) . . ? N13 C104 C105 115.7(8) . . ? C103 C104 C105 127.6(13) . . ? N14 C105 C104 117.6(11) . . ? N14 C105 C106 120.7(13) . . ? C104 C105 C106 121.7(10) . . ? C107 C106 C105 115.1(11) . . ? C106 C107 C108 124.4(13) . . ? C107 C108 C109 117.7(14) . . ? N14 C109 C108 119.4(11) . . ? N15 C110 C111 122.3(6) . . ? C112 C111 C110 119.3(6) . . ? C111 C112 C113 119.1(7) . . ? C112 C113 C114 118.7(7) . . ? N15 C114 C113 122.6(6) . . ? N15 C114 C115 113.8(5) . . ? C113 C114 C115 123.6(6) . . ? N16 C115 C116 121.5(6) . . ? N16 C115 C114 114.5(6) . . ? C116 C115 C114 124.0(6) . . ? C117 C116 C115 119.1(8) . . ? C116 C117 C118 119.5(8) . . ? C119 C118 C117 118.8(7) . . ? N16 C119 C118 122.5(7) . . ? O31 N30 O33 119.7(5) . . ? O31 N30 O32 120.3(5) . . ? O33 N30 O32 120.0(5) . . ? O42 N40 O43 117.0(10) . . ? O42 N40 O41 122.5(10) . . ? O43 N40 O41 120.4(10) . . ? O51 N50 O52 117.4(10) . . ? O51 N50 O53 125.3(11) . . ? O52 N50 O53 117.2(10) . . ? O51' N50' O52' 117(3) . . ? O51' N50' O53' 113(2) . . ? O52' N50' O53' 127(3) . . ? O61 N60 O62 118.0(10) . . ? O61 N60 O63 120.2(9) . . ? O62 N60 O63 121.8(11) . . ? O61' N60' O62' 117.8(13) . . ? O61' N60' O63' 120.7(12) . . ? O62' N60' O63' 121.5(13) . . ? O73 N70 O72 122.6(11) . . ? O73 N70 O71 119.2(11) . . ? O72 N70 O71 117.4(10) . . ? O73' N70' O72' 121(2) . . ? O73' N70' O71' 122(2) . . ? O72' N70' O71' 115(2) . . ? O81 N80 O82 125.3(13) . . ? O81 N80 O83 121.7(13) . . ? O82 N80 O83 112.9(12) . . ? O81' N80' O82' 118(2) . . ? O81' N80' O83' 116(2) . . ? O82' N80' O83' 116(2) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.293 _refine_diff_density_min -0.963 _refine_diff_density_rms 0.117 #===END data_compound4 _database_code_depnum_ccdc_archive 'CCDC 641415' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H65 Cu4 N11 O21 P2' _chemical_formula_weight 1592.33 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' 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 24.125(5) _cell_length_b 15.624(2) _cell_length_c 18.860(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.76(2) _cell_angle_gamma 90.00 _cell_volume 6807(2) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelopiped _exptl_crystal_colour blue _exptl_crystal_size_max .1 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3264 _exptl_absorpt_coefficient_mu 1.361 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15756 _diffrn_reflns_av_R_equivalents 0.0702 _diffrn_reflns_av_sigmaI/netI 0.0678 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.10 _diffrn_reflns_theta_max 22.49 _reflns_number_total 4429 _reflns_number_gt 3093 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0918P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4429 _refine_ls_number_parameters 507 _refine_ls_number_restraints 190 _refine_ls_R_factor_all 0.0695 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1325 _refine_ls_wR_factor_gt 0.1243 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu -0.00188(3) 0.57744(5) 0.16320(4) 0.0338(2) Uani 1 1 d . . . Cu2 Cu 0.01566(3) 0.79815(5) 0.14386(4) 0.0322(2) Uani 1 1 d . . . P1 P 0.07933(7) 0.71504(10) 0.29630(8) 0.0301(4) Uani 1 1 d . . . N1 N 0.0699(2) 0.5255(3) 0.1487(3) 0.0388(13) Uani 1 1 d . . . N2 N -0.0120(2) 0.6167(3) 0.0577(3) 0.0370(13) Uani 1 1 d . . . N3 N 0.0754(2) 0.7906(3) 0.0880(3) 0.0368(12) Uani 1 1 d . . . N4 N -0.0253(2) 0.8677(3) 0.0547(3) 0.0360(12) Uani 1 1 d . . . O1 O 0.05221(16) 0.7060(2) 0.2120(2) 0.0324(9) Uani 1 1 d . . . O2 O 0.07246(17) 0.6333(3) 0.3367(2) 0.0367(10) Uani 1 1 d . . . O3 O 0.05480(17) 0.7940(2) 0.3258(2) 0.0320(9) Uani 1 1 d . . . O4 O 0.0000 0.5137(4) 0.2500 0.0473(16) Uani 1 2 d S . . H4 H 0.0000 0.4535 0.2500 0.057 Uiso 1 2 calc SR . . O5 O 0.0555(2) 0.9119(3) 0.2165(3) 0.0486(12) Uani 1 1 d D . . H5V H 0.053(4) 0.894(5) 0.257(3) 0.073 Uiso 1 1 d D . . H5W H 0.092(2) 0.913(5) 0.225(5) 0.073 Uiso 1 1 d D . . C1 C 0.1559(3) 0.7317(4) 0.3131(3) 0.0342(14) Uani 1 1 d . . . H1 H 0.1607 0.7763 0.2780 0.041 Uiso 1 1 calc R . . C2 C 0.1864(3) 0.6516(5) 0.2977(4) 0.0528(18) Uani 1 1 d . . . H2A H 0.1690 0.6339 0.2462 0.063 Uiso 1 1 calc R . . H2B H 0.1806 0.6052 0.3298 0.063 Uiso 1 1 calc R . . C3 C 0.2510(3) 0.6663(6) 0.3110(6) 0.078(3) Uani 1 1 d . . . H3A H 0.2696 0.6120 0.3049 0.093 Uiso 1 1 calc R . . H3B H 0.2569 0.7065 0.2740 0.093 Uiso 1 1 calc R . . C4 C 0.2788(4) 0.7008(7) 0.3864(6) 0.085(3) Uani 1 1 d . . . H4A H 0.2772 0.6576 0.4234 0.102 Uiso 1 1 calc R . . H4B H 0.3197 0.7130 0.3917 0.102 Uiso 1 1 calc R . . C5 C 0.2499(3) 0.7804(6) 0.4008(5) 0.070(2) Uani 1 1 d . . . H5A H 0.2542 0.8253 0.3665 0.084 Uiso 1 1 calc R . . H5B H 0.2686 0.8002 0.4513 0.084 Uiso 1 1 calc R . . C6 C 0.1858(3) 0.7644(5) 0.3910(4) 0.0534(19) Uani 1 1 d . . . H6A H 0.1815 0.7221 0.4275 0.064 Uiso 1 1 calc R . . H6B H 0.1673 0.8176 0.3998 0.064 Uiso 1 1 calc R . . C7 C 0.1110(3) 0.4816(4) 0.1963(4) 0.0542(19) Uani 1 1 d . . . H7 H 0.1063 0.4686 0.2429 0.065 Uiso 1 1 calc R . . C8 C 0.1619(3) 0.4534(5) 0.1801(6) 0.067(2) Uani 1 1 d . . . H8 H 0.1907 0.4230 0.2153 0.081 Uiso 1 1 calc R . . C9 C 0.1678(4) 0.4715(5) 0.1123(6) 0.071(3) Uani 1 1 d . . . H9 H 0.2013 0.4531 0.1008 0.086 Uiso 1 1 calc R . . C10 C 0.1255(3) 0.5168(5) 0.0592(5) 0.057(2) Uani 1 1 d . . . C11 C 0.1269(4) 0.5375(5) -0.0140(6) 0.072(3) Uani 1 1 d . . . H11 H 0.1586 0.5197 -0.0297 0.086 Uiso 1 1 calc R . . C12 C 0.0845(5) 0.5815(5) -0.0607(5) 0.070(3) Uani 1 1 d . . . H12 H 0.0869 0.5932 -0.1086 0.084 Uiso 1 1 calc R . . C13 C 0.0352(4) 0.6113(5) -0.0400(4) 0.052(2) Uani 1 1 d . . . C14 C -0.0107(4) 0.6595(5) -0.0847(4) 0.061(2) Uani 1 1 d . . . H14 H -0.0106 0.6750 -0.1328 0.073 Uiso 1 1 calc R . . C15 C -0.0552(4) 0.6836(5) -0.0591(4) 0.057(2) Uani 1 1 d . . . H15 H -0.0862 0.7153 -0.0894 0.069 Uiso 1 1 calc R . . C16 C -0.0549(3) 0.6614(4) 0.0127(4) 0.0439(16) Uani 1 1 d . . . H16 H -0.0861 0.6785 0.0299 0.053 Uiso 1 1 calc R . . C17 C 0.0772(3) 0.5432(4) 0.0816(4) 0.0420(17) Uani 1 1 d . . . C18 C 0.0327(3) 0.5915(4) 0.0317(4) 0.0404(16) Uani 1 1 d . . . C19 C 0.1262(3) 0.7510(4) 0.1068(4) 0.0445(17) Uani 1 1 d . . . H19 H 0.1391 0.7252 0.1537 0.053 Uiso 1 1 calc R . . C20 C 0.1617(3) 0.7461(5) 0.0590(4) 0.0544(19) Uani 1 1 d . . . H20 H 0.1974 0.7172 0.0736 0.065 Uiso 1 1 calc R . . C21 C 0.1431(4) 0.7842(5) -0.0090(4) 0.056(2) Uani 1 1 d . . . H21 H 0.1663 0.7812 -0.0415 0.068 Uiso 1 1 calc R . . C22 C 0.0907(3) 0.8271(4) -0.0308(4) 0.0456(17) Uani 1 1 d . . . C23 C 0.0666(4) 0.8686(5) -0.1004(4) 0.061(2) Uani 1 1 d . . . H23 H 0.0879 0.8688 -0.1350 0.073 Uiso 1 1 calc R . . C24 C 0.0149(4) 0.9072(5) -0.1182(4) 0.062(2) Uani 1 1 d . . . H24 H 0.0008 0.9330 -0.1650 0.074 Uiso 1 1 calc R . . C25 C -0.0193(3) 0.9100(4) -0.0675(4) 0.0458(18) Uani 1 1 d . . . C26 C -0.0736(3) 0.9473(5) -0.0814(4) 0.056(2) Uani 1 1 d . . . H26 H -0.0910 0.9730 -0.1275 0.067 Uiso 1 1 calc R . . C27 C -0.1020(3) 0.9466(4) -0.0281(4) 0.0497(18) Uani 1 1 d . . . H27 H -0.1383 0.9733 -0.0369 0.060 Uiso 1 1 calc R . . C28 C -0.0767(3) 0.9061(4) 0.0391(4) 0.0450(17) Uani 1 1 d . . . H28 H -0.0967 0.9059 0.0751 0.054 Uiso 1 1 calc R . . C29 C 0.0578(3) 0.8288(4) 0.0197(4) 0.0388(16) Uani 1 1 d . . . C30 C 0.0029(3) 0.8699(4) 0.0018(4) 0.0384(16) Uani 1 1 d . . . N5 N 0.1300(8) 0.7453(10) 0.7815(10) 0.096(6) Uani 0.50 1 d PDU . . O51 O 0.1723(7) 0.7514(12) 0.8178(8) 0.110(6) Uani 0.50 1 d PDU . . O52 O 0.0985(12) 0.6914(14) 0.7828(16) 0.227(11) Uani 0.50 1 d PDU . . O53 O 0.1074(9) 0.7950(13) 0.7427(10) 0.156(7) Uani 0.50 1 d PDU . . N6 N 0.2489(15) 0.9271(19) 1.0761(13) 0.193(12) Uani 0.50 1 d PDU . . O61 O 0.2296(8) 0.9660(14) 1.0215(14) 0.172(8) Uani 0.50 1 d PDU . . O62 O 0.2463(7) 0.9215(11) 1.1320(9) 0.122(6) Uani 0.50 1 d PDU . . O63 O 0.2774(12) 0.8701(17) 1.0680(16) 0.237(12) Uani 0.50 1 d PDU . . N7 N 0.2060(8) 0.9466(12) 0.8989(11) 0.123(7) Uani 0.50 1 d PDU . . O71 O 0.1969(8) 1.0105(12) 0.9198(14) 0.164(7) Uani 0.50 1 d PDU . . O72 O 0.2288(10) 0.9012(16) 0.9443(13) 0.201(10) Uani 0.50 1 d PDU . . O73 O 0.2013(8) 0.9219(11) 0.8432(9) 0.119(6) Uani 0.50 1 d PDU . . O10 O 0.1719(3) 0.9451(6) 0.2290(5) 0.146(4) Uani 1 1 d . . . O11 O 0.0296(8) 0.6744(9) 0.7619(8) 0.119(8) Uani 0.50 1 d P . . 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 0.0385(5) 0.0324(4) 0.0320(4) -0.0025(3) 0.0125(3) 0.0038(3) Cu2 0.0339(4) 0.0324(4) 0.0320(4) 0.0018(3) 0.0124(3) -0.0002(3) P1 0.0293(9) 0.0300(9) 0.0314(8) 0.0019(7) 0.0096(7) 0.0007(7) N1 0.043(3) 0.036(3) 0.037(3) -0.009(3) 0.010(3) 0.002(3) N2 0.040(3) 0.032(3) 0.039(3) -0.012(2) 0.010(3) -0.007(3) N3 0.042(3) 0.034(3) 0.034(3) 0.000(2) 0.011(2) -0.002(3) N4 0.039(3) 0.033(3) 0.039(3) 0.000(2) 0.016(3) -0.005(3) O1 0.030(2) 0.032(2) 0.035(2) -0.0008(18) 0.0098(18) 0.0021(18) O2 0.034(2) 0.038(2) 0.038(2) 0.010(2) 0.0095(19) -0.0009(19) O3 0.034(2) 0.032(2) 0.031(2) -0.0039(18) 0.0108(18) -0.0022(19) O4 0.070(5) 0.032(3) 0.044(4) 0.000 0.022(3) 0.000 O5 0.054(3) 0.042(3) 0.047(3) 0.007(2) 0.009(3) -0.008(2) C1 0.032(3) 0.033(3) 0.038(3) 0.004(3) 0.012(3) -0.001(3) C2 0.042(4) 0.046(4) 0.072(5) 0.002(4) 0.019(4) 0.007(3) C3 0.038(5) 0.081(6) 0.124(8) -0.002(6) 0.037(5) 0.007(4) C4 0.036(5) 0.095(7) 0.115(8) 0.026(6) 0.006(5) -0.001(5) C5 0.047(5) 0.081(6) 0.073(6) 0.008(5) 0.002(4) -0.016(5) C6 0.029(4) 0.075(5) 0.050(4) -0.003(4) 0.002(3) -0.007(4) C7 0.055(5) 0.042(4) 0.060(5) -0.011(4) 0.008(4) 0.004(4) C8 0.042(5) 0.049(5) 0.106(7) -0.012(5) 0.013(5) 0.015(4) C9 0.052(5) 0.050(5) 0.122(8) -0.025(5) 0.042(6) -0.004(4) C10 0.056(5) 0.037(4) 0.089(6) -0.018(4) 0.040(5) -0.006(4) C11 0.084(7) 0.049(5) 0.111(8) -0.019(5) 0.074(6) -0.009(5) C12 0.111(8) 0.048(5) 0.076(6) -0.017(5) 0.067(6) -0.021(5) C13 0.077(6) 0.044(4) 0.046(4) -0.013(4) 0.033(4) -0.020(4) C14 0.104(7) 0.043(4) 0.038(4) -0.006(4) 0.027(5) -0.024(5) C15 0.080(6) 0.046(5) 0.035(4) 0.003(3) 0.001(4) -0.011(4) C16 0.047(4) 0.035(4) 0.041(4) -0.006(3) 0.000(3) -0.002(3) C17 0.044(4) 0.031(3) 0.056(4) -0.013(3) 0.023(4) -0.003(3) C18 0.050(4) 0.034(4) 0.043(4) -0.013(3) 0.021(3) -0.011(3) C19 0.041(4) 0.052(4) 0.044(4) -0.001(3) 0.017(3) -0.002(4) C20 0.046(4) 0.058(5) 0.066(5) -0.012(4) 0.028(4) -0.004(4) C21 0.071(5) 0.058(5) 0.055(5) -0.009(4) 0.041(4) -0.017(4) C22 0.057(5) 0.045(4) 0.044(4) -0.006(3) 0.028(4) -0.008(4) C23 0.085(6) 0.063(5) 0.048(5) 0.000(4) 0.040(5) -0.013(5) C24 0.088(7) 0.060(5) 0.040(4) 0.006(4) 0.022(4) -0.020(5) C25 0.062(5) 0.039(4) 0.034(4) 0.001(3) 0.011(3) -0.016(4) C26 0.066(5) 0.041(4) 0.047(4) 0.018(3) -0.002(4) -0.010(4) C27 0.047(4) 0.044(4) 0.054(4) 0.014(4) 0.008(4) -0.005(3) C28 0.045(4) 0.035(4) 0.053(4) 0.005(3) 0.011(3) -0.005(3) C29 0.043(4) 0.034(4) 0.043(4) -0.004(3) 0.018(3) -0.009(3) C30 0.051(4) 0.026(3) 0.039(4) -0.003(3) 0.014(3) -0.012(3) N5 0.162(15) 0.050(9) 0.112(13) -0.024(9) 0.098(12) -0.027(10) O51 0.115(11) 0.162(13) 0.078(9) -0.001(9) 0.069(9) 0.008(10) O52 0.28(2) 0.222(19) 0.200(17) -0.053(15) 0.104(16) -0.001(17) O53 0.215(16) 0.141(14) 0.134(13) 0.008(11) 0.085(12) 0.030(13) N6 0.152(17) 0.159(17) 0.257(19) -0.021(16) 0.038(15) -0.038(14) O61 0.089(11) 0.164(15) 0.272(18) -0.056(15) 0.066(13) -0.012(11) O62 0.126(11) 0.135(11) 0.106(10) -0.074(9) 0.036(9) -0.084(9) O63 0.194(18) 0.186(18) 0.32(2) 0.053(16) 0.059(16) -0.024(15) N7 0.076(11) 0.103(14) 0.218(17) 0.036(14) 0.084(13) -0.005(10) O71 0.117(12) 0.103(11) 0.312(19) -0.047(13) 0.124(13) -0.007(10) O72 0.144(15) 0.201(17) 0.29(2) 0.033(15) 0.110(15) -0.039(13) O73 0.130(12) 0.131(12) 0.121(11) -0.036(10) 0.077(10) -0.029(10) O10 0.088(5) 0.154(8) 0.164(8) 0.066(6) -0.013(5) -0.051(5) O11 0.23(2) 0.087(9) 0.040(9) -0.007(7) 0.041(14) -0.006(10) _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 O4 1.906(3) . ? Cu1 O2 1.914(4) 2 ? Cu1 N1 2.002(5) . ? Cu1 N2 2.028(5) . ? Cu1 O1 2.428(4) . ? Cu2 O3 1.945(4) 2 ? Cu2 O1 1.961(4) . ? Cu2 N4 2.007(5) . ? Cu2 N3 2.019(5) . ? Cu2 O5 2.280(5) . ? P1 O2 1.520(4) . ? P1 O3 1.540(4) . ? P1 O1 1.542(4) . ? P1 C1 1.802(6) . ? N1 C7 1.320(9) . ? N1 C17 1.356(8) . ? N2 C16 1.331(8) . ? N2 C18 1.365(8) . ? N3 C19 1.327(8) . ? N3 C29 1.371(8) . ? N4 C28 1.332(8) . ? N4 C30 1.361(8) . ? O2 Cu1 1.914(4) 2 ? O3 Cu2 1.945(4) 2 ? O4 Cu1 1.906(3) 2 ? C1 C2 1.521(9) . ? C1 C6 1.526(9) . ? C2 C3 1.524(10) . ? C3 C4 1.489(14) . ? C4 C5 1.487(13) . ? C5 C6 1.526(10) . ? C7 C8 1.420(11) . ? C8 C9 1.355(12) . ? C9 C10 1.398(12) . ? C10 C17 1.412(9) . ? C10 C11 1.426(12) . ? C11 C12 1.332(13) . ? C12 C13 1.433(11) . ? C13 C14 1.402(11) . ? C13 C18 1.404(9) . ? C14 C15 1.352(11) . ? C15 C16 1.396(10) . ? C17 C18 1.423(10) . ? C19 C20 1.413(9) . ? C20 C21 1.367(11) . ? C21 C22 1.386(11) . ? C22 C29 1.404(9) . ? C22 C23 1.429(11) . ? C23 C24 1.337(11) . ? C24 C25 1.433(10) . ? C25 C26 1.388(11) . ? C25 C30 1.408(9) . ? C26 C27 1.369(10) . ? C27 C28 1.391(9) . ? C29 C30 1.423(9) . ? N5 O51 1.057(14) . ? N5 O53 1.099(14) . ? N5 O52 1.140(15) . ? O52 O11 1.61(3) . ? O52 O53 1.827(19) . ? N6 O62 1.078(15) . ? N6 O63 1.162(17) . ? N6 O61 1.169(15) . ? O61 O72 1.77(3) . ? O62 O63 1.78(2) . ? N7 O73 1.094(14) . ? N7 O71 1.119(14) . ? N7 O72 1.127(15) . ? O11 O11 1.37(4) 2_556 ? 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 O4 Cu1 O2 92.19(15) . 2 ? O4 Cu1 N1 95.62(18) . . ? O2 Cu1 N1 172.0(2) 2 . ? O4 Cu1 N2 165.2(2) . . ? O2 Cu1 N2 90.43(19) 2 . ? N1 Cu1 N2 81.6(2) . . ? O4 Cu1 O1 103.29(16) . . ? O2 Cu1 O1 90.19(15) 2 . ? N1 Cu1 O1 89.75(17) . . ? N2 Cu1 O1 91.23(16) . . ? O3 Cu2 O1 92.81(16) 2 . ? O3 Cu2 N4 90.21(18) 2 . ? O1 Cu2 N4 165.04(18) . . ? O3 Cu2 N3 165.39(19) 2 . ? O1 Cu2 N3 92.59(19) . . ? N4 Cu2 N3 81.2(2) . . ? O3 Cu2 O5 95.83(17) 2 . ? O1 Cu2 O5 98.44(17) . . ? N4 Cu2 O5 95.82(19) . . ? N3 Cu2 O5 96.79(19) . . ? O2 P1 O3 112.5(2) . . ? O2 P1 O1 111.4(2) . . ? O3 P1 O1 110.7(2) . . ? O2 P1 C1 106.7(3) . . ? O3 P1 C1 107.6(3) . . ? O1 P1 C1 107.6(2) . . ? C7 N1 C17 117.9(6) . . ? C7 N1 Cu1 128.8(5) . . ? C17 N1 Cu1 113.2(4) . . ? C16 N2 C18 118.1(6) . . ? C16 N2 Cu1 129.5(4) . . ? C18 N2 Cu1 112.4(4) . . ? C19 N3 C29 117.8(5) . . ? C19 N3 Cu2 129.1(4) . . ? C29 N3 Cu2 113.0(4) . . ? C28 N4 C30 117.2(5) . . ? C28 N4 Cu2 129.1(4) . . ? C30 N4 Cu2 113.5(4) . . ? P1 O1 Cu2 125.8(2) . . ? P1 O1 Cu1 119.2(2) . . ? Cu2 O1 Cu1 105.55(16) . . ? P1 O2 Cu1 127.5(2) . 2 ? P1 O3 Cu2 126.3(2) . 2 ? Cu1 O4 Cu1 117.0(3) 2 . ? C2 C1 C6 109.8(6) . . ? C2 C1 P1 112.0(4) . . ? C6 C1 P1 113.1(4) . . ? C1 C2 C3 111.8(6) . . ? C4 C3 C2 111.7(7) . . ? C5 C4 C3 111.8(8) . . ? C4 C5 C6 110.7(7) . . ? C1 C6 C5 110.5(6) . . ? N1 C7 C8 122.7(8) . . ? C9 C8 C7 118.1(8) . . ? C8 C9 C10 121.9(7) . . ? C9 C10 C17 115.3(7) . . ? C9 C10 C11 126.4(8) . . ? C17 C10 C11 118.3(8) . . ? C12 C11 C10 122.0(7) . . ? C11 C12 C13 121.7(8) . . ? C14 C13 C18 116.9(7) . . ? C14 C13 C12 125.7(7) . . ? C18 C13 C12 117.4(8) . . ? C15 C14 C13 120.3(7) . . ? C14 C15 C16 119.7(8) . . ? N2 C16 C15 122.3(7) . . ? N1 C17 C10 124.1(7) . . ? N1 C17 C18 116.7(5) . . ? C10 C17 C18 119.2(6) . . ? N2 C18 C13 122.6(7) . . ? N2 C18 C17 116.0(6) . . ? C13 C18 C17 121.3(6) . . ? N3 C19 C20 122.5(7) . . ? C21 C20 C19 118.8(7) . . ? C20 C21 C22 120.8(6) . . ? C21 C22 C29 117.0(6) . . ? C21 C22 C23 125.9(6) . . ? C29 C22 C23 117.1(7) . . ? C24 C23 C22 122.5(7) . . ? C23 C24 C25 121.4(7) . . ? C26 C25 C30 116.6(6) . . ? C26 C25 C24 125.6(7) . . ? C30 C25 C24 117.8(7) . . ? C27 C26 C25 120.3(6) . . ? C26 C27 C28 119.4(7) . . ? N4 C28 C27 122.8(6) . . ? N3 C29 C22 123.1(6) . . ? N3 C29 C30 115.8(5) . . ? C22 C29 C30 121.1(6) . . ? N4 C30 C25 123.7(6) . . ? N4 C30 C29 116.2(6) . . ? C25 C30 C29 120.1(6) . . ? O51 N5 O53 124.7(17) . . ? O51 N5 O52 125(2) . . ? O53 N5 O52 109.3(16) . . ? N5 O52 O11 140(2) . . ? N5 O52 O53 34.6(9) . . ? O11 O52 O53 106.3(19) . . ? N5 O53 O52 36.1(9) . . ? O62 N6 O63 106(2) . . ? O62 N6 O61 141(3) . . ? O63 N6 O61 113(2) . . ? N6 O61 O72 109(2) . . ? N6 O62 O63 38.8(11) . . ? N6 O63 O62 35.6(10) . . ? O73 N7 O71 133(2) . . ? O73 N7 O72 113.6(19) . . ? O71 N7 O72 113(2) . . ? N7 O72 O61 99(2) . . ? O11 O11 O52 169.6(13) 2_556 . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.656 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.090 #===END