# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. #TrackingRef 'Compound-1c.cif' _journal_coden_Cambridge 0182 _publ_contact_author_name 'Catalina Ruiz-Perez' _publ_contact_author_address ; Laboratorio de Rayos X y Materiales Moleculares Dpto. F\'isica Fundamental II. Facultad de F\'isica Universidad de La Laguna E-38204. La Laguna. Tenerife Spain ; _publ_contact_author_email caruiz@ull.es _publ_author_name 'Catalina Ruiz-Perez' data_Compound1 _database_code_depnum_ccdc_archive 'CCDC 856597' #TrackingRef 'Compound-1c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C124 H134 Cu2 N4 O27 P4' _chemical_formula_weight 2363.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5320(10) _cell_length_b 15.7080(10) _cell_length_c 15.8360(10) _cell_angle_alpha 71.2170(10) _cell_angle_beta 70.9200(10) _cell_angle_gamma 68.9650(10) _cell_volume 2888.2(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.501 _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 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.75130 _diffrn_source synchrotron _diffrn_source_type 'ESRF-CRG BM16' _diffrn_radiation_monochromator 'Si 111' _diffrn_detector 'HUBER ADSC Q210r CCD detector' _diffrn_detector_area_resol_mean 9.6 _diffrn_radiation_detector 'ADSC Q210r CCD (binned mode)' _diffrn_measurement_device_type 'Single-axis HUBER diffractometer' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43483 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 5.34 _diffrn_reflns_theta_max 26.23 _reflns_number_total 9167 _reflns_number_gt 9045 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'mxcube (Gabadinho & McSweeney, 2010' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0514P)^2^+4.7954P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0062(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9167 _refine_ls_number_parameters 735 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1107 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1W O 0.58272(14) 0.40193(13) 0.60133(12) 0.0230(4) Uani 1 1 d . . . O2W O 0.64762(15) 0.99727(12) -0.08174(12) 0.0229(4) Uani 1 1 d . . . O3W O 0.37843(15) 0.76289(14) 0.26144(12) 0.0267(4) Uani 1 1 d . . . O4W O 0.27087(17) 0.94849(15) 0.27116(13) 0.0347(5) Uani 1 1 d . . . O5W O 0.8884(2) 0.73915(16) -0.27263(15) 0.0429(6) Uani 1 1 d . . . O6W O 0.8292(2) 0.92731(18) 0.60778(18) 0.0516(6) Uani 1 1 d . . . O7W O -0.2879(3) 0.9359(2) 0.4835(2) 0.0701(8) Uani 1 1 d . . . O8W O 1.0348(6) 0.9434(6) 0.4983(6) 0.103(3) Uani 0.50 1 d P . . Cu1 Cu 0.71195(2) 0.609183(18) 0.154303(18) 0.01052(11) Uani 1 1 d . . . P3 P 0.54613(4) 0.71344(4) 0.65284(4) 0.00815(14) Uani 1 1 d . . . O4 O 0.63750(13) 0.58777(12) 0.28354(11) 0.0188(4) Uani 1 1 d . . . O2 O 0.54509(13) 0.85451(12) 0.02982(12) 0.0176(4) Uani 1 1 d . . . O1 O 0.58426(12) 0.71779(11) 0.13180(11) 0.0147(3) Uani 1 1 d . . . N2 N 0.83067(14) 0.50606(13) 0.19937(13) 0.0105(4) Uani 1 1 d . . . N1 N 0.76592(14) 0.65042(13) 0.02106(13) 0.0104(4) Uani 1 1 d . . . O6 O 0.86720(13) 0.40254(13) 0.33437(11) 0.0188(4) Uani 1 1 d . . . O3 O 0.73525(13) 0.78477(12) -0.09300(12) 0.0206(4) Uani 1 1 d . . . C001 C 0.52034(17) 0.61849(16) 0.74878(15) 0.0100(4) Uani 1 1 d . . . O5 O 0.65890(14) 0.49798(13) 0.42098(12) 0.0230(4) Uani 1 1 d . . . C002 C 0.57981(18) 0.80701(17) 0.75808(16) 0.0136(5) Uani 1 1 d . . . H002 H 0.6251 0.7494 0.7813 0.016 Uiso 1 1 calc R . . C003 C 0.94858(19) 0.69248(16) 0.02376(16) 0.0141(5) Uani 1 1 d . . . H00A H 1.0191 0.6856 0.0307 0.021 Uiso 1 1 calc R . . H00B H 0.9026 0.6741 0.0829 0.021 Uiso 1 1 calc R . . H00C H 0.9165 0.7568 -0.0035 0.021 Uiso 1 1 calc R . . C004 C 0.52443(17) 0.81443(16) 0.69392(15) 0.0102(4) Uani 1 1 d . . . C005 C 0.68348(17) 0.67612(16) 0.58678(15) 0.0108(4) Uani 1 1 d . . . C006 C 0.93520(17) 0.46312(15) 0.14788(14) 0.0082(4) Uani 1 1 d . . . C007 C 0.60347(17) 0.77432(16) 0.05311(16) 0.0118(5) Uani 1 1 d . . . C008 C 0.96035(17) 0.63116(15) -0.03713(14) 0.0084(4) Uani 1 1 d . . . C009 C 0.30637(19) 0.80294(18) 0.47450(16) 0.0163(5) Uani 1 1 d . . . H009 H 0.2553 0.8241 0.4394 0.020 Uiso 1 1 calc R . . C010 C 0.86709(17) 0.61257(15) -0.03846(14) 0.0087(4) Uani 1 1 d . . . C011 C 0.87004(17) 0.56219(15) -0.09814(15) 0.0094(4) Uani 1 1 d . . . C012 C 0.29248(18) 0.73662(16) 0.55640(15) 0.0130(5) Uani 1 1 d . . . H012 H 0.2334 0.7123 0.5752 0.016 Uiso 1 1 calc R . . C013 C 0.49711(19) 0.97096(17) 0.75373(17) 0.0171(5) Uani 1 1 d . . . H013 H 0.4889 1.0238 0.7728 0.021 Uiso 1 1 calc R . . C014 C 0.45992(18) 0.63431(17) 0.83517(16) 0.0150(5) Uani 1 1 d . . . H014 H 0.4340 0.6948 0.8446 0.018 Uiso 1 1 calc R . . C015 C 0.56696(19) 0.88570(17) 0.78680(17) 0.0167(5) Uani 1 1 d . . . H015 H 0.6050 0.8814 0.8281 0.020 Uiso 1 1 calc R . . C016 C 0.43962(19) 0.97825(17) 0.69271(17) 0.0162(5) Uani 1 1 d . . . H016 H 0.3919 1.0355 0.6719 0.019 Uiso 1 1 calc R . . C017 C 0.45548(17) 0.74265(16) 0.58085(15) 0.0102(4) Uani 1 1 d . . . C018 C 0.76692(18) 0.55337(17) -0.10742(16) 0.0152(5) Uani 1 1 d . . . H01A H 0.7051 0.5865 -0.0676 0.023 Uiso 1 1 calc R . . H01B H 0.7692 0.4884 -0.0907 0.023 Uiso 1 1 calc R . . H01C H 0.7607 0.5796 -0.1699 0.023 Uiso 1 1 calc R . . C019 C 0.93991(17) 0.40603(15) 0.09360(15) 0.0091(4) Uani 1 1 d . . . C020 C 0.36651(17) 0.70635(16) 0.61060(15) 0.0112(4) Uani 1 1 d . . . H020 H 0.3569 0.6624 0.6661 0.013 Uiso 1 1 calc R . . C021 C 1.02925(17) 0.47763(15) 0.15276(14) 0.0087(4) Uani 1 1 d . . . C022 C 0.55812(19) 0.52796(17) 0.73468(16) 0.0151(5) Uani 1 1 d . . . H022 H 0.5975 0.5174 0.6769 0.018 Uiso 1 1 calc R . . C023 C 0.70321(18) 0.62770(16) 0.51984(15) 0.0126(5) Uani 1 1 d . . . H023 H 0.6456 0.6185 0.5075 0.015 Uiso 1 1 calc R . . C024 C 0.47137(19) 0.80708(18) 0.49703(16) 0.0170(5) Uani 1 1 d . . . H024 H 0.5324 0.8291 0.4765 0.020 Uiso 1 1 calc R . . C025 C 0.80793(18) 0.46917(16) 0.28965(16) 0.0123(5) Uani 1 1 d . . . C026 C 0.71021(17) 0.73636(16) -0.01477(16) 0.0118(5) Uani 1 1 d . . . C027 C 0.45307(18) 0.90022(16) 0.66235(15) 0.0132(5) Uani 1 1 d . . . H027 H 0.4146 0.9051 0.6211 0.016 Uiso 1 1 calc R . . C028 C 1.02396(19) 0.53218(17) 0.21788(16) 0.0144(5) Uani 1 1 d . . . H02A H 0.9499 0.5676 0.2381 0.022 Uiso 1 1 calc R . . H02B H 1.0685 0.5742 0.1869 0.022 Uiso 1 1 calc R . . H02C H 1.0502 0.4895 0.2700 0.022 Uiso 1 1 calc R . . C029 C 0.8756(2) 0.65437(19) 0.55741(17) 0.0213(5) Uani 1 1 d . . . H029 H 0.9337 0.6624 0.5702 0.026 Uiso 1 1 calc R . . C030 C 0.80951(19) 0.59370(17) 0.47213(16) 0.0164(5) Uani 1 1 d . . . H030 H 0.8233 0.5613 0.4277 0.020 Uiso 1 1 calc R . . C031 C 0.69229(18) 0.52138(17) 0.33714(16) 0.0151(5) Uani 1 1 d . . . C032 C 0.4775(2) 0.46966(18) 0.89282(17) 0.0181(5) Uani 1 1 d . . . H032 H 0.4635 0.4197 0.9413 0.022 Uiso 1 1 calc R . . C033 C 0.43871(19) 0.55985(18) 0.90687(16) 0.0170(5) Uani 1 1 d . . . H033 H 0.3984 0.5702 0.9646 0.020 Uiso 1 1 calc R . . C034 C 0.83605(18) 0.38677(17) 0.09938(16) 0.0143(5) Uani 1 1 d . . . H03A H 0.7860 0.4440 0.0755 0.021 Uiso 1 1 calc R . . H03B H 0.8039 0.3622 0.1623 0.021 Uiso 1 1 calc R . . H03C H 0.8523 0.3419 0.0640 0.021 Uiso 1 1 calc R . . C035 C 0.77018(19) 0.68922(18) 0.60556(16) 0.0169(5) Uani 1 1 d . . . H035 H 0.7572 0.7212 0.6502 0.020 Uiso 1 1 calc R . . C036 C 0.5368(2) 0.45352(18) 0.80702(18) 0.0204(5) Uani 1 1 d . . . H036 H 0.5624 0.3930 0.7979 0.024 Uiso 1 1 calc R . . C037 C 0.89529(19) 0.60773(18) 0.49035(17) 0.0192(5) Uani 1 1 d . . . H037 H 0.9663 0.5857 0.4574 0.023 Uiso 1 1 calc R . . C038 C 0.3956(2) 0.83824(19) 0.44410(16) 0.0195(5) Uani 1 1 d . . . H038 H 0.4046 0.8824 0.3887 0.023 Uiso 1 1 calc R . . P2 P 0.01964(4) 0.86774(4) 0.20014(4) 0.00899(14) Uani 1 1 d . . . C039 C -0.10249(17) 0.84816(16) 0.19835(15) 0.0106(4) Uani 1 1 d . . . C040 C 0.12271(18) 0.85306(15) 0.09596(15) 0.0115(4) Uani 1 1 d . . . C041 C -0.01551(18) 0.98391(16) 0.21575(15) 0.0113(4) Uani 1 1 d . . . C042 C 0.07288(18) 0.78557(16) 0.29431(16) 0.0127(5) Uani 1 1 d . . . C043 C -0.16040(18) 0.90758(16) 0.13235(16) 0.0125(5) Uani 1 1 d . . . H043 H -0.1349 0.9561 0.0892 0.015 Uiso 1 1 calc R . . C044 C -0.1367(2) 1.09918(18) 0.30088(18) 0.0203(5) Uani 1 1 d . . . H044 H -0.2008 1.1195 0.3434 0.024 Uiso 1 1 calc R . . C045 C 0.13181(19) 0.69404(17) 0.28614(17) 0.0171(5) Uani 1 1 d . . . H045 H 0.1446 0.6765 0.2319 0.021 Uiso 1 1 calc R . . C046 C 0.0301(2) 1.12486(18) 0.19553(17) 0.0187(5) Uani 1 1 d . . . H046 H 0.0768 1.1626 0.1674 0.022 Uiso 1 1 calc R . . C047 C -0.11245(19) 1.01407(17) 0.27900(16) 0.0161(5) Uani 1 1 d . . . H047 H -0.1604 0.9774 0.3063 0.019 Uiso 1 1 calc R . . C048 C -0.29467(18) 0.82330(17) 0.19673(17) 0.0158(5) Uani 1 1 d . . . H048 H -0.3590 0.8147 0.1963 0.019 Uiso 1 1 calc R . . C049 C 0.05615(19) 1.03943(17) 0.17346(16) 0.0142(5) Uani 1 1 d . . . H049 H 0.1205 1.0194 0.1311 0.017 Uiso 1 1 calc R . . C050 C 0.09833(18) 0.85046(15) 0.01793(16) 0.0122(5) Uani 1 1 d . . . H050 H 0.0280 0.8529 0.0198 0.015 Uiso 1 1 calc R . . C051 C -0.25556(18) 0.89421(17) 0.13123(16) 0.0149(5) Uani 1 1 d . . . H051 H -0.2932 0.9328 0.0866 0.018 Uiso 1 1 calc R . . C052 C 0.17939(19) 0.84418(16) -0.06245(16) 0.0154(5) Uani 1 1 d . . . H052 H 0.1636 0.8417 -0.1144 0.018 Uiso 1 1 calc R . . C053 C -0.0653(2) 1.15409(18) 0.25928(18) 0.0208(5) Uani 1 1 d . . . H053 H -0.0817 1.2110 0.2743 0.025 Uiso 1 1 calc R . . C054 C -0.23865(19) 0.76527(17) 0.26280(17) 0.0170(5) Uani 1 1 d . . . H054 H -0.2658 0.7181 0.3069 0.020 Uiso 1 1 calc R . . C055 C 0.15234(19) 0.6553(2) 0.44065(18) 0.0220(6) Uani 1 1 d . . . H055 H 0.1791 0.6117 0.4896 0.026 Uiso 1 1 calc R . . C056 C -0.14190(19) 0.77697(17) 0.26381(16) 0.0143(5) Uani 1 1 d . . . H056 H -0.1039 0.7374 0.3080 0.017 Uiso 1 1 calc R . . C057 C 0.0539(2) 0.81164(18) 0.37570(16) 0.0171(5) Uani 1 1 d . . . H057 H 0.0148 0.8726 0.3812 0.021 Uiso 1 1 calc R . . C058 C 0.30922(19) 0.84186(18) 0.01240(19) 0.0207(5) Uani 1 1 d . . . H058 H 0.3799 0.8389 0.0102 0.025 Uiso 1 1 calc R . . C059 C 0.28427(19) 0.84152(17) -0.06543(17) 0.0180(5) Uani 1 1 d . . . H059 H 0.3378 0.8395 -0.1200 0.022 Uiso 1 1 calc R . . C060 C 0.0937(2) 0.74582(19) 0.44839(17) 0.0206(5) Uani 1 1 d . . . H060 H 0.0808 0.7629 0.5029 0.025 Uiso 1 1 calc R . . C061 C 0.22940(19) 0.84658(18) 0.09376(18) 0.0186(5) Uani 1 1 d . . . H061 H 0.2467 0.8454 0.1464 0.022 Uiso 1 1 calc R . . C062 C 0.17113(19) 0.62947(19) 0.35959(18) 0.0222(5) Uani 1 1 d . . . H062 H 0.2104 0.5684 0.3545 0.027 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1W 0.0151(8) 0.0284(11) 0.0212(9) -0.0079(8) -0.0008(7) -0.0026(7) O2W 0.0270(9) 0.0134(9) 0.0248(9) -0.0046(8) -0.0013(8) -0.0062(7) O3W 0.0269(10) 0.0296(11) 0.0185(9) -0.0076(8) 0.0028(7) -0.0077(8) O4W 0.0398(12) 0.0328(12) 0.0220(10) -0.0022(9) -0.0098(9) -0.0011(9) O5W 0.0822(17) 0.0320(13) 0.0374(12) 0.0138(10) -0.0419(12) -0.0368(12) O6W 0.0546(15) 0.0357(14) 0.0527(15) -0.0009(12) -0.0085(12) -0.0114(11) O7W 0.082(2) 0.069(2) 0.0505(16) 0.0181(15) -0.0264(15) -0.0309(17) O8W 0.084(5) 0.105(6) 0.104(6) -0.037(5) 0.018(4) -0.036(5) Cu1 0.00797(16) 0.00932(17) 0.01233(17) -0.00287(12) -0.00142(11) -0.00082(11) P3 0.0088(3) 0.0079(3) 0.0088(3) -0.0015(2) -0.0037(2) -0.0025(2) O4 0.0103(8) 0.0224(10) 0.0184(9) -0.0074(8) 0.0014(7) -0.0007(7) O2 0.0108(8) 0.0117(9) 0.0258(9) -0.0038(8) -0.0055(7) 0.0026(7) O1 0.0097(7) 0.0114(8) 0.0199(8) -0.0042(7) -0.0006(6) -0.0017(6) N2 0.0092(9) 0.0093(10) 0.0107(9) -0.0022(8) -0.0002(7) -0.0020(7) N1 0.0082(9) 0.0076(10) 0.0127(9) -0.0026(8) -0.0010(7) -0.0002(7) O6 0.0171(8) 0.0225(10) 0.0112(8) 0.0027(7) -0.0026(7) -0.0056(7) O3 0.0145(8) 0.0163(9) 0.0180(9) 0.0048(8) -0.0037(7) 0.0024(7) C001 0.0073(10) 0.0122(12) 0.0117(10) -0.0015(9) -0.0045(8) -0.0034(8) O5 0.0244(9) 0.0281(11) 0.0150(9) -0.0080(8) 0.0057(7) -0.0123(8) C002 0.0143(11) 0.0101(12) 0.0167(11) -0.0023(10) -0.0087(9) 0.0000(9) C003 0.0163(11) 0.0104(12) 0.0165(11) -0.0045(10) -0.0035(9) -0.0041(9) C004 0.0106(10) 0.0086(11) 0.0117(10) -0.0023(9) -0.0024(8) -0.0032(8) C005 0.0108(10) 0.0095(11) 0.0098(10) 0.0013(9) -0.0022(8) -0.0037(8) C006 0.0084(10) 0.0042(11) 0.0072(10) 0.0023(9) -0.0021(8) 0.0007(8) C007 0.0087(10) 0.0101(12) 0.0194(12) -0.0054(10) -0.0043(9) -0.0032(9) C008 0.0123(10) 0.0022(10) 0.0083(10) 0.0031(9) -0.0045(8) -0.0010(8) C009 0.0185(12) 0.0211(13) 0.0147(11) -0.0057(10) -0.0090(9) -0.0060(10) C010 0.0099(10) 0.0033(11) 0.0079(10) 0.0027(9) -0.0023(8) 0.0005(8) C011 0.0098(10) 0.0067(11) 0.0097(10) 0.0026(9) -0.0039(8) -0.0027(8) C012 0.0129(11) 0.0156(12) 0.0139(11) -0.0058(10) -0.0039(9) -0.0052(9) C013 0.0165(11) 0.0129(12) 0.0238(12) -0.0091(11) -0.0021(10) -0.0046(9) C014 0.0156(11) 0.0138(12) 0.0154(11) -0.0057(10) -0.0024(9) -0.0030(9) C015 0.0167(11) 0.0180(13) 0.0196(12) -0.0081(11) -0.0071(9) -0.0040(10) C016 0.0162(11) 0.0078(12) 0.0200(12) 0.0003(10) -0.0051(9) -0.0007(9) C017 0.0117(10) 0.0102(11) 0.0111(10) -0.0037(9) -0.0054(8) -0.0024(8) C018 0.0108(11) 0.0183(13) 0.0173(11) -0.0052(10) -0.0036(9) -0.0037(9) C019 0.0100(10) 0.0051(11) 0.0104(10) 0.0026(9) -0.0043(8) -0.0022(8) C020 0.0125(10) 0.0118(12) 0.0104(10) -0.0046(9) -0.0016(8) -0.0041(9) C021 0.0122(10) 0.0042(11) 0.0074(10) 0.0027(9) -0.0045(8) -0.0016(8) C022 0.0164(11) 0.0128(12) 0.0154(11) -0.0053(10) -0.0002(9) -0.0048(9) C023 0.0149(11) 0.0106(12) 0.0116(11) 0.0007(9) -0.0041(9) -0.0049(9) C024 0.0182(12) 0.0220(14) 0.0143(11) 0.0004(10) -0.0060(9) -0.0121(10) C025 0.0113(11) 0.0126(12) 0.0147(11) -0.0042(10) -0.0009(9) -0.0062(9) C026 0.0073(10) 0.0121(12) 0.0169(11) -0.0037(10) -0.0040(9) -0.0024(9) C027 0.0129(11) 0.0132(12) 0.0132(11) -0.0005(10) -0.0050(9) -0.0040(9) C028 0.0163(11) 0.0147(12) 0.0144(11) -0.0054(10) -0.0043(9) -0.0044(9) C029 0.0129(12) 0.0280(15) 0.0227(13) -0.0001(12) -0.0050(10) -0.0101(10) C030 0.0194(12) 0.0131(12) 0.0118(11) -0.0011(10) -0.0003(9) -0.0037(10) C031 0.0144(11) 0.0188(13) 0.0164(12) -0.0092(11) 0.0019(9) -0.0103(10) C032 0.0204(12) 0.0170(13) 0.0171(12) 0.0043(10) -0.0057(10) -0.0118(10) C033 0.0162(11) 0.0238(14) 0.0109(11) -0.0030(10) -0.0004(9) -0.0089(10) C034 0.0115(11) 0.0136(12) 0.0185(12) -0.0035(10) -0.0031(9) -0.0050(9) C035 0.0160(12) 0.0215(14) 0.0157(11) -0.0037(10) -0.0038(9) -0.0086(10) C036 0.0233(13) 0.0124(13) 0.0254(13) -0.0047(11) -0.0022(10) -0.0079(10) C037 0.0121(11) 0.0184(13) 0.0171(12) 0.0029(11) 0.0010(9) -0.0031(9) C038 0.0264(13) 0.0227(14) 0.0120(11) 0.0041(10) -0.0097(10) -0.0123(11) P2 0.0106(3) 0.0073(3) 0.0110(3) -0.0015(2) -0.0059(2) -0.0023(2) C039 0.0104(10) 0.0094(11) 0.0149(11) -0.0058(9) -0.0049(9) -0.0017(8) C040 0.0132(11) 0.0071(11) 0.0154(11) -0.0026(9) -0.0045(9) -0.0031(8) C041 0.0161(11) 0.0084(11) 0.0125(11) -0.0014(9) -0.0097(9) -0.0024(9) C042 0.0112(10) 0.0138(12) 0.0158(11) 0.0017(10) -0.0089(9) -0.0062(9) C043 0.0139(11) 0.0090(11) 0.0150(11) -0.0031(10) -0.0053(9) -0.0017(9) C044 0.0200(12) 0.0198(14) 0.0233(13) -0.0120(11) -0.0060(10) -0.0011(10) C045 0.0135(11) 0.0168(13) 0.0192(12) -0.0006(10) -0.0063(9) -0.0033(9) C046 0.0264(13) 0.0146(13) 0.0221(12) -0.0018(11) -0.0124(10) -0.0100(10) C047 0.0164(11) 0.0160(13) 0.0181(12) -0.0047(10) -0.0053(9) -0.0054(9) C048 0.0102(11) 0.0170(13) 0.0261(13) -0.0143(11) -0.0050(9) -0.0017(9) C049 0.0163(11) 0.0148(13) 0.0144(11) -0.0014(10) -0.0074(9) -0.0062(9) C050 0.0148(11) 0.0066(11) 0.0172(11) -0.0015(9) -0.0070(9) -0.0035(9) C051 0.0127(11) 0.0146(12) 0.0197(12) -0.0076(10) -0.0096(9) 0.0020(9) C052 0.0217(12) 0.0096(12) 0.0158(11) -0.0052(10) -0.0051(9) -0.0029(9) C053 0.0286(13) 0.0134(13) 0.0274(13) -0.0081(11) -0.0155(11) -0.0029(10) C054 0.0163(11) 0.0142(13) 0.0225(12) -0.0059(11) -0.0022(10) -0.0073(9) C055 0.0142(12) 0.0289(15) 0.0215(13) 0.0108(11) -0.0116(10) -0.0126(10) C056 0.0157(11) 0.0114(12) 0.0160(11) -0.0012(10) -0.0067(9) -0.0034(9) C057 0.0204(12) 0.0175(13) 0.0188(12) -0.0005(10) -0.0109(10) -0.0091(10) C058 0.0108(11) 0.0209(14) 0.0330(14) -0.0133(12) -0.0030(10) -0.0032(10) C059 0.0179(12) 0.0115(12) 0.0220(12) -0.0085(11) 0.0029(10) -0.0041(9) C060 0.0229(13) 0.0289(15) 0.0160(12) 0.0043(11) -0.0117(10) -0.0162(11) C061 0.0148(12) 0.0224(14) 0.0248(13) -0.0112(11) -0.0075(10) -0.0049(10) C062 0.0126(11) 0.0170(13) 0.0297(14) 0.0054(12) -0.0077(10) -0.0031(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 O8W O8W 1.697(17) 2_776 ? Cu1 O4 1.9413(16) . ? Cu1 N2 1.9624(19) . ? Cu1 N1 1.9639(19) . ? Cu1 O1 1.9793(16) . ? P3 C017 1.786(2) . ? P3 C001 1.795(2) . ? P3 C004 1.798(2) . ? P3 C005 1.798(2) . ? O4 C031 1.282(3) . ? O2 C007 1.234(3) . ? O1 C007 1.285(3) . ? N2 C025 1.335(3) . ? N2 C006 1.427(3) . ? N1 C026 1.330(3) . ? N1 C010 1.431(3) . ? O6 C025 1.238(3) . ? O3 C026 1.238(3) . ? C001 C014 1.394(3) . ? C001 C022 1.393(3) . ? O5 C031 1.231(3) . ? C002 C015 1.386(3) . ? C002 C004 1.402(3) . ? C002 H002 0.9300 . ? C003 C008 1.507(3) . ? C003 H00A 0.9600 . ? C003 H00B 0.9600 . ? C003 H00C 0.9600 . ? C004 C027 1.395(3) . ? C005 C035 1.396(3) . ? C005 C023 1.401(3) . ? C006 C021 1.401(3) . ? C006 C019 1.402(3) . ? C007 C026 1.542(3) . ? C008 C019 1.394(3) 2_765 ? C008 C010 1.401(3) . ? C009 C012 1.383(3) . ? C009 C038 1.388(3) . ? C009 H009 0.9300 . ? C010 C011 1.398(3) . ? C011 C021 1.401(3) 2_765 ? C011 C018 1.508(3) . ? C012 C020 1.387(3) . ? C012 H012 0.9300 . ? C013 C016 1.381(4) . ? C013 C015 1.387(4) . ? C013 H013 0.9300 . ? C014 C033 1.383(3) . ? C014 H014 0.9300 . ? C015 H015 0.9300 . ? C016 C027 1.389(3) . ? C016 H016 0.9300 . ? C017 C024 1.392(3) . ? C017 C020 1.395(3) . ? C018 H01A 0.9600 . ? C018 H01B 0.9600 . ? C018 H01C 0.9600 . ? C019 C008 1.394(3) 2_765 ? C019 C034 1.509(3) . ? C020 H020 0.9300 . ? C021 C011 1.401(3) 2_765 ? C021 C028 1.510(3) . ? C022 C036 1.388(4) . ? C022 H022 0.9300 . ? C023 C030 1.387(3) . ? C023 H023 0.9300 . ? C024 C038 1.389(3) . ? C024 H024 0.9300 . ? C025 C031 1.547(3) . ? C027 H027 0.9300 . ? C028 H02A 0.9600 . ? C028 H02B 0.9600 . ? C028 H02C 0.9600 . ? C029 C037 1.383(4) . ? C029 C035 1.383(3) . ? C029 H029 0.9300 . ? C030 C037 1.387(4) . ? C030 H030 0.9300 . ? C032 C036 1.385(4) . ? C032 C033 1.387(4) . ? C032 H032 0.9300 . ? C033 H033 0.9300 . ? C034 H03A 0.9600 . ? C034 H03B 0.9600 . ? C034 H03C 0.9600 . ? C035 H035 0.9300 . ? C036 H036 0.9300 . ? C037 H037 0.9300 . ? C038 H038 0.9300 . ? P2 C042 1.790(2) . ? P2 C041 1.791(2) . ? P2 C039 1.796(2) . ? P2 C040 1.797(2) . ? C039 C056 1.389(3) . ? C039 C043 1.400(3) . ? C040 C050 1.395(3) . ? C040 C061 1.400(3) . ? C041 C047 1.396(3) . ? C041 C049 1.398(3) . ? C042 C057 1.394(3) . ? C042 C045 1.396(3) . ? C043 C051 1.383(3) . ? C043 H043 0.9300 . ? C044 C047 1.387(3) . ? C044 C053 1.388(4) . ? C044 H044 0.9300 . ? C045 C062 1.386(4) . ? C045 H045 0.9300 . ? C046 C053 1.385(4) . ? C046 C049 1.389(3) . ? C046 H046 0.9300 . ? C047 H047 0.9300 . ? C048 C054 1.381(4) . ? C048 C051 1.385(4) . ? C048 H048 0.9300 . ? C049 H049 0.9300 . ? C050 C052 1.387(3) . ? C050 H050 0.9300 . ? C051 H051 0.9300 . ? C052 C059 1.390(3) . ? C052 H052 0.9300 . ? C053 H053 0.9300 . ? C054 C056 1.392(3) . ? C054 H054 0.9300 . ? C055 C060 1.381(4) . ? C055 C062 1.387(4) . ? C055 H055 0.9300 . ? C056 H056 0.9300 . ? C057 C060 1.387(4) . ? C057 H057 0.9300 . ? C058 C059 1.382(4) . ? C058 C061 1.388(4) . ? C058 H058 0.9300 . ? C059 H059 0.9300 . ? C060 H060 0.9300 . ? C061 H061 0.9300 . ? C062 H062 0.9300 . ? 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 N2 82.86(7) . . ? O4 Cu1 N1 170.08(7) . . ? N2 Cu1 N1 106.91(8) . . ? O4 Cu1 O1 87.71(7) . . ? N2 Cu1 O1 169.36(7) . . ? N1 Cu1 O1 82.40(7) . . ? C017 P3 C001 110.00(10) . . ? C017 P3 C004 108.87(10) . . ? C001 P3 C004 109.42(10) . . ? C017 P3 C005 108.23(10) . . ? C001 P3 C005 108.55(10) . . ? C004 P3 C005 111.74(10) . . ? C031 O4 Cu1 115.36(14) . . ? C007 O1 Cu1 113.29(13) . . ? C025 N2 C006 116.34(18) . . ? C025 N2 Cu1 115.06(14) . . ? C006 N2 Cu1 128.52(14) . . ? C026 N1 C010 114.79(18) . . ? C026 N1 Cu1 113.68(14) . . ? C010 N1 Cu1 129.92(15) . . ? C014 C001 C022 120.0(2) . . ? C014 C001 P3 121.36(18) . . ? C022 C001 P3 118.63(17) . . ? C015 C002 C004 119.9(2) . . ? C015 C002 H002 120.1 . . ? C004 C002 H002 120.1 . . ? C008 C003 H00A 109.5 . . ? C008 C003 H00B 109.5 . . ? H00A C003 H00B 109.5 . . ? C008 C003 H00C 109.5 . . ? H00A C003 H00C 109.5 . . ? H00B C003 H00C 109.5 . . ? C027 C004 C002 119.7(2) . . ? C027 C004 P3 120.52(17) . . ? C002 C004 P3 119.77(18) . . ? C035 C005 C023 120.2(2) . . ? C035 C005 P3 121.01(17) . . ? C023 C005 P3 118.66(16) . . ? C021 C006 C019 121.82(19) . . ? C021 C006 N2 120.40(18) . . ? C019 C006 N2 117.78(18) . . ? O2 C007 O1 125.4(2) . . ? O2 C007 C026 119.4(2) . . ? O1 C007 C026 115.17(19) . . ? C019 C008 C010 118.86(19) 2_765 . ? C019 C008 C003 122.43(19) 2_765 . ? C010 C008 C003 118.69(19) . . ? C012 C009 C038 120.8(2) . . ? C012 C009 H009 119.6 . . ? C038 C009 H009 119.6 . . ? C011 C010 C008 122.00(19) . . ? C011 C010 N1 120.12(19) . . ? C008 C010 N1 117.82(18) . . ? C010 C011 C021 118.99(19) . 2_765 ? C010 C011 C018 121.31(19) . . ? C021 C011 C018 119.65(19) 2_765 . ? C009 C012 C020 120.1(2) . . ? C009 C012 H012 119.9 . . ? C020 C012 H012 119.9 . . ? C016 C013 C015 120.7(2) . . ? C016 C013 H013 119.7 . . ? C015 C013 H013 119.7 . . ? C033 C014 C001 119.8(2) . . ? C033 C014 H014 120.1 . . ? C001 C014 H014 120.1 . . ? C002 C015 C013 119.8(2) . . ? C002 C015 H015 120.1 . . ? C013 C015 H015 120.1 . . ? C013 C016 C027 120.1(2) . . ? C013 C016 H016 120.0 . . ? C027 C016 H016 120.0 . . ? C024 C017 C020 120.7(2) . . ? C024 C017 P3 118.57(17) . . ? C020 C017 P3 120.64(18) . . ? C011 C018 H01A 109.5 . . ? C011 C018 H01B 109.5 . . ? H01A C018 H01B 109.5 . . ? C011 C018 H01C 109.5 . . ? H01A C018 H01C 109.5 . . ? H01B C018 H01C 109.5 . . ? C008 C019 C006 119.16(19) 2_765 . ? C008 C019 C034 122.57(19) 2_765 . ? C006 C019 C034 118.27(19) . . ? C012 C020 C017 119.2(2) . . ? C012 C020 H020 120.4 . . ? C017 C020 H020 120.4 . . ? C011 C021 C006 118.84(19) 2_765 . ? C011 C021 C028 119.99(19) 2_765 . ? C006 C021 C028 121.14(19) . . ? C036 C022 C001 119.9(2) . . ? C036 C022 H022 120.0 . . ? C001 C022 H022 120.0 . . ? C030 C023 C005 119.3(2) . . ? C030 C023 H023 120.4 . . ? C005 C023 H023 120.4 . . ? C038 C024 C017 119.6(2) . . ? C038 C024 H024 120.2 . . ? C017 C024 H024 120.2 . . ? O6 C025 N2 127.7(2) . . ? O6 C025 C031 121.1(2) . . ? N2 C025 C031 111.2(2) . . ? O3 C026 N1 127.3(2) . . ? O3 C026 C007 120.2(2) . . ? N1 C026 C007 112.48(19) . . ? C016 C027 C004 119.8(2) . . ? C016 C027 H027 120.1 . . ? C004 C027 H027 120.1 . . ? C021 C028 H02A 109.5 . . ? C021 C028 H02B 109.5 . . ? H02A C028 H02B 109.5 . . ? C021 C028 H02C 109.5 . . ? H02A C028 H02C 109.5 . . ? H02B C028 H02C 109.5 . . ? C037 C029 C035 120.4(2) . . ? C037 C029 H029 119.8 . . ? C035 C029 H029 119.8 . . ? C037 C030 C023 120.3(2) . . ? C037 C030 H030 119.8 . . ? C023 C030 H030 119.8 . . ? O5 C031 O4 124.6(2) . . ? O5 C031 C025 119.9(2) . . ? O4 C031 C025 115.48(19) . . ? C036 C032 C033 120.4(2) . . ? C036 C032 H032 119.8 . . ? C033 C032 H032 119.8 . . ? C014 C033 C032 120.1(2) . . ? C014 C033 H033 120.0 . . ? C032 C033 H033 120.0 . . ? C019 C034 H03A 109.5 . . ? C019 C034 H03B 109.5 . . ? H03A C034 H03B 109.5 . . ? C019 C034 H03C 109.5 . . ? H03A C034 H03C 109.5 . . ? H03B C034 H03C 109.5 . . ? C029 C035 C005 119.6(2) . . ? C029 C035 H035 120.2 . . ? C005 C035 H035 120.2 . . ? C032 C036 C022 119.8(2) . . ? C032 C036 H036 120.1 . . ? C022 C036 H036 120.1 . . ? C029 C037 C030 120.2(2) . . ? C029 C037 H037 119.9 . . ? C030 C037 H037 119.9 . . ? C009 C038 C024 119.5(2) . . ? C009 C038 H038 120.2 . . ? C024 C038 H038 120.2 . . ? C042 P2 C041 108.87(10) . . ? C042 P2 C039 109.97(10) . . ? C041 P2 C039 107.78(10) . . ? C042 P2 C040 108.06(11) . . ? C041 P2 C040 111.07(10) . . ? C039 P2 C040 111.07(10) . . ? C056 C039 C043 119.9(2) . . ? C056 C039 P2 120.61(17) . . ? C043 C039 P2 119.47(17) . . ? C050 C040 C061 120.0(2) . . ? C050 C040 P2 121.84(17) . . ? C061 C040 P2 118.14(17) . . ? C047 C041 C049 120.5(2) . . ? C047 C041 P2 117.66(17) . . ? C049 C041 P2 121.52(18) . . ? C057 C042 C045 120.2(2) . . ? C057 C042 P2 120.67(18) . . ? C045 C042 P2 119.16(17) . . ? C051 C043 C039 120.0(2) . . ? C051 C043 H043 120.0 . . ? C039 C043 H043 120.0 . . ? C047 C044 C053 120.0(2) . . ? C047 C044 H044 120.0 . . ? C053 C044 H044 120.0 . . ? C062 C045 C042 119.5(2) . . ? C062 C045 H045 120.3 . . ? C042 C045 H045 120.3 . . ? C053 C046 C049 120.2(2) . . ? C053 C046 H046 119.9 . . ? C049 C046 H046 119.9 . . ? C044 C047 C041 119.5(2) . . ? C044 C047 H047 120.2 . . ? C041 C047 H047 120.2 . . ? C054 C048 C051 120.3(2) . . ? C054 C048 H048 119.8 . . ? C051 C048 H048 119.8 . . ? C046 C049 C041 119.2(2) . . ? C046 C049 H049 120.4 . . ? C041 C049 H049 120.4 . . ? C052 C050 C040 119.8(2) . . ? C052 C050 H050 120.1 . . ? C040 C050 H050 120.1 . . ? C043 C051 C048 119.9(2) . . ? C043 C051 H051 120.1 . . ? C048 C051 H051 120.1 . . ? C050 C052 C059 120.0(2) . . ? C050 C052 H052 120.0 . . ? C059 C052 H052 120.0 . . ? C046 C053 C044 120.5(2) . . ? C046 C053 H053 119.7 . . ? C044 C053 H053 119.7 . . ? C048 C054 C056 120.4(2) . . ? C048 C054 H054 119.8 . . ? C056 C054 H054 119.8 . . ? C060 C055 C062 119.8(2) . . ? C060 C055 H055 120.1 . . ? C062 C055 H055 120.1 . . ? C039 C056 C054 119.5(2) . . ? C039 C056 H056 120.3 . . ? C054 C056 H056 120.3 . . ? C060 C057 C042 119.4(2) . . ? C060 C057 H057 120.3 . . ? C042 C057 H057 120.3 . . ? C059 C058 C061 120.3(2) . . ? C059 C058 H058 119.8 . . ? C061 C058 H058 119.8 . . ? C058 C059 C052 120.3(2) . . ? C058 C059 H059 119.9 . . ? C052 C059 H059 119.9 . . ? C055 C060 C057 120.7(2) . . ? C055 C060 H060 119.6 . . ? C057 C060 H060 119.6 . . ? C058 C061 C040 119.5(2) . . ? C058 C061 H061 120.3 . . ? C040 C061 H061 120.3 . . ? C045 C062 C055 120.5(2) . . ? C045 C062 H062 119.8 . . ? C055 C062 H062 119.8 . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 26.23 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 1.414 _refine_diff_density_min -0.661 _refine_diff_density_rms 0.068