# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Dry, Emily' 'Clegg, Jack' 'Breiner, Boris' 'Whitaker, Daniel' 'Stefak, Roman' 'Nitschke, Jonathan' _publ_contact_author_name 'Nitschke, Jonathan' _publ_contact_author_email jrn34@cam.ac.uk _publ_section_title ; Anion templation under pH control of self-assembled [2+2] and [3+3] metallomacrocycles containing a new dicopper(I) motif ; # Attachment '- PLATON report combined.pdf' # Attachment '- combined.CIF' data_jn1031 _database_code_depnum_ccdc_archive 'CCDC 815065' #TrackingRef '- combined.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H44 Cu2 N6 P2, 2(H S O4), 2(C2 H3 N)' _chemical_formula_sum 'C56 H52 Cu2 N8 O8 P2 S2' _chemical_formula_weight 1218.20 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.360(3) _cell_length_b 14.495(3) _cell_length_c 16.258(3) _cell_angle_alpha 95.16(3) _cell_angle_beta 91.69(3) _cell_angle_gamma 105.61(3) _cell_volume 2789.5(10) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 42600 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 0.956 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.812 _exptl_absorpt_correction_T_max 1.007 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 60657 _diffrn_reflns_av_R_equivalents 0.1261 _diffrn_reflns_av_sigmaI/netI 0.1195 _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 -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 27.42 _reflns_number_total 12532 _reflns_number_gt 7020 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-97 (Altomare et al. 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_molecular_graphics ;ORTEP-3 (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material 'enCIFer 1.1 (CCDC, 2005)' _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^)+(0.1173P)^2^+7.9628P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12532 _refine_ls_number_parameters 696 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1474 _refine_ls_R_factor_gt 0.0829 _refine_ls_wR_factor_ref 0.2499 _refine_ls_wR_factor_gt 0.2241 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 C1 C 0.3631(6) 0.4824(5) 0.9268(4) 0.0424(17) Uani 1 1 d . . . C2 C 0.3007(7) 0.3963(5) 0.9506(4) 0.0441(17) Uani 1 1 d . . . H2 H 0.3211 0.3390 0.9340 0.053 Uiso 1 1 calc R . . C3 C 0.2083(7) 0.3912(6) 0.9983(4) 0.0503(19) Uani 1 1 d . . . H3 H 0.1636 0.3303 1.0109 0.060 Uiso 1 1 calc R . . C4 C 0.1816(6) 0.4732(5) 1.0272(4) 0.0404(16) Uani 1 1 d . . . H4 H 0.1267 0.4718 1.0671 0.049 Uiso 1 1 calc R . . C5 C 0.2360(8) 0.5574(6) 0.9969(5) 0.057(2) Uani 1 1 d . . . H5 H 0.2073 0.6118 1.0065 0.068 Uiso 1 1 calc R . . C6 C 0.3331(7) 0.5660(6) 0.9521(5) 0.055(2) Uani 1 1 d . . . H6 H 0.3771 0.6271 0.9394 0.066 Uiso 1 1 calc R . . C7 C 0.5332(6) 0.5544(5) 0.8683(4) 0.0409(17) Uani 1 1 d . . . H7 H 0.5311 0.6148 0.8952 0.049 Uiso 1 1 calc R . . C8 C 0.6257(6) 0.5484(5) 0.8172(4) 0.0370(15) Uani 1 1 d . . . C9 C 0.7066(5) 0.4485(5) 0.7360(4) 0.0335(14) Uani 1 1 d . . . C10 C 0.7989(6) 0.5262(5) 0.7223(4) 0.0377(15) Uani 1 1 d . . . H10 H 0.8573 0.5167 0.6887 0.045 Uiso 1 1 calc R . . C11 C 0.8019(7) 0.6179(5) 0.7597(5) 0.0511(19) Uani 1 1 d . . . H11 H 0.8635 0.6718 0.7532 0.061 Uiso 1 1 calc R . . C12 C 0.7131(7) 0.6282(5) 0.8065(5) 0.0472(18) Uani 1 1 d . . . H12 H 0.7123 0.6900 0.8311 0.057 Uiso 1 1 calc R . . C13 C 0.7847(5) 0.2873(5) 0.7731(4) 0.0318(14) Uani 1 1 d . . . C14 C 0.8822(5) 0.3560(6) 0.8120(4) 0.0389(16) Uani 1 1 d . . . H14 H 0.9008 0.4220 0.8025 0.047 Uiso 1 1 calc R . . C15 C 0.9499(7) 0.3194(6) 0.8661(4) 0.052(2) Uani 1 1 d . . . H15 H 1.0186 0.3609 0.8904 0.063 Uiso 1 1 calc R . . C16 C 0.9172(7) 0.2240(7) 0.8838(5) 0.058(2) Uani 1 1 d . . . H16 H 0.9631 0.2014 0.9206 0.070 Uiso 1 1 calc R . . C17 C 0.8186(8) 0.1619(6) 0.8482(5) 0.058(2) Uani 1 1 d . . . H17 H 0.7963 0.0974 0.8620 0.070 Uiso 1 1 calc R . . C18 C 0.7514(6) 0.1925(5) 0.7926(4) 0.0436(17) Uani 1 1 d . . . H18 H 0.6837 0.1494 0.7682 0.052 Uiso 1 1 calc R . . C19 C 0.7892(5) 0.3448(4) 0.6074(4) 0.0333(14) Uani 1 1 d . . . C20 C 0.8827(6) 0.3106(6) 0.5984(4) 0.0432(17) Uani 1 1 d . . . H20 H 0.9053 0.2770 0.6403 0.052 Uiso 1 1 calc R . . C21 C 0.9437(7) 0.3253(7) 0.5281(5) 0.059(2) Uani 1 1 d . . . H21 H 1.0067 0.3002 0.5213 0.070 Uiso 1 1 calc R . . C22 C 0.9127(7) 0.3766(6) 0.4680(5) 0.055(2) Uani 1 1 d . . . H22 H 0.9556 0.3883 0.4206 0.066 Uiso 1 1 calc R . . C23 C 0.8197(6) 0.4104(6) 0.4770(4) 0.0475(18) Uani 1 1 d . . . H23 H 0.7993 0.4466 0.4362 0.057 Uiso 1 1 calc R . . C24 C 0.7556(6) 0.3921(5) 0.5450(4) 0.0390(16) Uani 1 1 d . . . H24 H 0.6885 0.4119 0.5490 0.047 Uiso 1 1 calc R . . C25 C 0.6410(5) 0.0938(5) 0.5297(4) 0.0351(15) Uani 1 1 d . . . C26 C 0.6359(7) 0.0326(5) 0.5899(5) 0.0473(18) Uani 1 1 d . . . H26 H 0.5860 0.0332 0.6331 0.057 Uiso 1 1 calc R . . C27 C 0.7040(7) -0.0310(6) 0.5881(5) 0.052(2) Uani 1 1 d . . . H27 H 0.6998 -0.0724 0.6307 0.063 Uiso 1 1 calc R . . C28 C 0.7789(5) -0.0347(5) 0.5242(4) 0.0406(16) Uani 1 1 d . . . H28 H 0.8215 -0.0804 0.5212 0.049 Uiso 1 1 calc R . . C29 C 0.7872(7) 0.0319(6) 0.4656(5) 0.053(2) Uani 1 1 d . . . H29 H 0.8409 0.0354 0.4246 0.064 Uiso 1 1 calc R . . C30 C 0.7147(7) 0.0951(6) 0.4674(5) 0.0506(19) Uani 1 1 d . . . H30 H 0.7178 0.1375 0.4258 0.061 Uiso 1 1 calc R . . C31 C 0.5339(6) 0.1902(5) 0.4757(4) 0.0390(16) Uani 1 1 d . . . H31 H 0.5492 0.1692 0.4214 0.047 Uiso 1 1 calc R . . C32 C 0.4659(5) 0.2594(5) 0.4889(4) 0.0346(14) Uani 1 1 d . . . C33 C 0.3827(5) 0.3411(5) 0.5855(4) 0.0315(14) Uani 1 1 d . . . C34 C 0.3433(6) 0.3850(5) 0.5242(4) 0.0410(16) Uani 1 1 d . . . H34 H 0.3010 0.4295 0.5380 0.049 Uiso 1 1 calc R . . C35 C 0.3649(7) 0.3651(6) 0.4430(4) 0.0480(18) Uani 1 1 d . . . H35 H 0.3386 0.3959 0.4005 0.058 Uiso 1 1 calc R . . C36 C 0.4259(6) 0.2990(5) 0.4244(4) 0.0429(17) Uani 1 1 d . . . H36 H 0.4398 0.2815 0.3688 0.051 Uiso 1 1 calc R . . C37 C 0.2162(5) 0.2453(4) 0.6856(4) 0.0287(13) Uani 1 1 d . . . C38 C 0.1842(6) 0.2002(5) 0.7557(4) 0.0398(16) Uani 1 1 d . . . H38 H 0.2320 0.2185 0.8046 0.048 Uiso 1 1 calc R . . C39 C 0.0831(6) 0.1283(6) 0.7563(5) 0.0506(19) Uani 1 1 d . . . H39 H 0.0611 0.0985 0.8051 0.061 Uiso 1 1 calc R . . C40 C 0.0137(6) 0.1007(6) 0.6815(5) 0.0480(18) Uani 1 1 d . . . H40 H -0.0562 0.0528 0.6806 0.058 Uiso 1 1 calc R . . C41 C 0.0474(6) 0.1430(5) 0.6113(5) 0.0458(18) Uani 1 1 d . . . H41 H 0.0018 0.1252 0.5613 0.055 Uiso 1 1 calc R . . C42 C 0.1475(5) 0.2108(4) 0.6147(4) 0.0277(13) Uani 1 1 d . . . H42 H 0.1723 0.2366 0.5647 0.033 Uiso 1 1 calc R . . C43 C 0.2885(5) 0.4512(4) 0.7042(4) 0.0291(13) Uani 1 1 d . . . C44 C 0.1795(6) 0.4490(5) 0.7264(4) 0.0404(16) Uani 1 1 d . . . H44 H 0.1258 0.3889 0.7297 0.048 Uiso 1 1 calc R . . C45 C 0.1497(7) 0.5319(6) 0.7431(5) 0.0500(19) Uani 1 1 d . . . H45 H 0.0754 0.5288 0.7588 0.060 Uiso 1 1 calc R . . C46 C 0.2248(7) 0.6206(6) 0.7380(5) 0.0506(19) Uani 1 1 d . . . H46 H 0.2023 0.6780 0.7494 0.061 Uiso 1 1 calc R . . C47 C 0.3317(7) 0.6251(5) 0.7163(5) 0.0483(18) Uani 1 1 d . . . H47 H 0.3837 0.6859 0.7123 0.058 Uiso 1 1 calc R . . C48 C 0.3652(6) 0.5411(5) 0.7001(4) 0.0397(16) Uani 1 1 d . . . H48 H 0.4403 0.5449 0.6861 0.048 Uiso 1 1 calc R . . C49 C 0.4930(6) 0.1982(5) 0.9019(4) 0.0419(16) Uani 1 1 d . . . C51 C 0.4964(8) 0.1165(6) 0.9454(5) 0.056(2) Uani 1 1 d . . . H51A H 0.4212 0.0864 0.9634 0.084 Uiso 1 1 calc R . . H51B H 0.5494 0.1378 0.9937 0.084 Uiso 1 1 calc R . . H51C H 0.5208 0.0696 0.9084 0.084 Uiso 1 1 calc R . . C52 C 0.3678(6) 0.0585(5) 0.7278(4) 0.0396(16) Uani 1 1 d . . . C53 C 0.2852(8) -0.0171(6) 0.7643(6) 0.062(2) Uani 1 1 d . . . H53A H 0.3217 -0.0646 0.7824 0.092 Uiso 1 1 calc R . . H53B H 0.2241 -0.0488 0.7230 0.092 Uiso 1 1 calc R . . H53C H 0.2545 0.0116 0.8119 0.092 Uiso 1 1 calc R . . N1 N 0.4553(5) 0.4794(4) 0.8773(3) 0.0366(13) Uani 1 1 d . . . N2 N 0.6226(4) 0.4597(4) 0.7809(3) 0.0313(12) Uani 1 1 d . . . N3 N 0.5710(4) 0.1594(4) 0.5373(3) 0.0347(12) Uani 1 1 d . . . N4 N 0.4468(4) 0.2802(4) 0.5687(3) 0.0313(12) Uani 1 1 d . . . N5 N 0.4865(5) 0.2616(4) 0.8647(3) 0.0367(13) Uani 1 1 d . . . N6 N 0.4320(5) 0.1186(4) 0.7021(3) 0.0407(14) Uani 1 1 d . . . N7 N 0.948(2) -0.1702(13) 0.6261(15) 0.083(3) Uani 0.50 1 d PD A 1 C54 C 0.915(3) -0.149(2) 0.6893(17) 0.083(3) Uani 0.50 1 d PD A 1 C55 C 0.900(5) -0.125(4) 0.7739(17) 0.083(3) Uani 0.50 1 d PD A 1 H55A H 0.9735 -0.0945 0.8027 0.125 Uiso 0.50 1 calc PR A 1 H55B H 0.8627 -0.1830 0.7992 0.125 Uiso 0.50 1 calc PR A 1 H55C H 0.8535 -0.0795 0.7783 0.125 Uiso 0.50 1 calc PR A 1 N7A N 0.907(2) -0.1972(13) 0.6150(15) 0.083(3) Uani 0.50 1 d PD B 2 C54A C 0.910(3) -0.163(2) 0.6827(16) 0.083(3) Uani 0.50 1 d PD B 2 C55A C 0.886(5) -0.125(4) 0.7617(16) 0.083(3) Uani 0.50 1 d PD B 2 H55D H 0.8107 -0.1156 0.7590 0.125 Uiso 0.50 1 calc PR B 2 H55E H 0.9417 -0.0635 0.7784 0.125 Uiso 0.50 1 calc PR B 2 H55F H 0.8895 -0.1707 0.8022 0.125 Uiso 0.50 1 calc PR B 2 N8 N 0.9647(9) 0.2989(9) 1.1281(8) 0.085(2) Uani 0.75 1 d PD C 1 C56 C 0.8786(11) 0.2481(11) 1.1027(10) 0.085(2) Uani 0.75 1 d PD C 1 C57 C 0.7708(11) 0.1942(11) 1.0694(10) 0.085(2) Uani 0.75 1 d PD C 1 H57A H 0.7158 0.1927 1.1118 0.127 Uiso 0.75 1 calc PR C 1 H57B H 0.7725 0.1284 1.0511 0.127 Uiso 0.75 1 calc PR C 1 H57C H 0.7494 0.2243 1.0221 0.127 Uiso 0.75 1 calc PR C 1 N8A N 0.952(3) 0.245(3) 1.176(2) 0.085(2) Uani 0.25 1 d PD D 2 C56A C 0.881(3) 0.209(4) 1.125(3) 0.085(2) Uani 0.25 1 d PD D 2 C57A C 0.789(3) 0.175(3) 1.067(2) 0.085(2) Uani 0.25 1 d PD D 2 H57D H 0.7200 0.1805 1.0929 0.127 Uiso 0.25 1 d PR D 2 H57E H 0.7816 0.1069 1.0488 0.127 Uiso 0.25 1 d PR D 2 H57F H 0.8011 0.2124 1.0195 0.127 Uiso 0.25 1 d PR D 2 O1 O 0.9025(5) 0.0049(5) 1.0750(4) 0.0723(17) Uani 1 1 d . . . H1 H 0.9482 0.0450 1.0498 0.108 Uiso 1 1 calc R . . O2 O 0.7599(6) -0.1427(5) 1.0586(4) 0.0762(18) Uani 1 1 d . . . O3 O 0.9203(6) -0.1254(5) 0.9777(4) 0.0723(17) Uani 1 1 d . . . O4 O 0.7839(6) -0.0372(5) 0.9505(4) 0.0746(18) Uani 1 1 d . . . O5 O 0.4962(13) -0.2165(11) 0.8653(8) 0.0816(18) Uani 0.50 1 d P E 1 O6 O 0.6012(17) -0.0552(16) 0.8493(11) 0.0816(18) Uani 0.50 1 d P E 1 H6A H 0.6251 -0.0665 0.8953 0.122 Uiso 0.50 1 calc PR E 1 O7 O 0.5956(16) -0.2160(12) 0.7807(10) 0.0816(18) Uani 0.50 1 d P E 1 O8 O 0.4601(14) -0.1303(12) 0.7459(9) 0.0816(18) Uani 0.50 1 d P E 1 O5A O 0.4559(13) -0.1574(11) 0.8561(8) 0.0816(18) Uani 0.50 1 d P E 2 O6A O 0.6281(18) -0.0467(16) 0.8276(11) 0.0816(18) Uani 0.50 1 d P E 2 H6A1 H 0.6554 -0.0463 0.8756 0.122 Uiso 0.50 1 calc PR E 2 O7A O 0.5020(14) -0.1260(12) 0.7176(9) 0.0816(18) Uani 0.50 1 d P E 2 O8A O 0.6219(16) -0.1908(12) 0.7544(10) 0.0816(18) Uani 0.50 1 d P E 2 P1 P 0.69862(13) 0.32366(12) 0.69506(10) 0.0297(4) Uani 1 1 d . . . P2 P 0.34243(13) 0.34537(12) 0.69386(9) 0.0289(4) Uani 1 1 d . . . S1 S 0.83567(17) -0.07695(15) 1.01366(12) 0.0516(5) Uani 1 1 d . . . S2 S 0.53947(17) -0.14669(15) 0.80177(12) 0.0501(5) Uani 1 1 d . . . Cu1 Cu 0.47126(6) 0.36000(6) 0.79501(4) 0.0319(2) Uani 1 1 d D . . Cu2 Cu 0.53476(6) 0.22392(6) 0.65172(4) 0.0313(2) Uani 1 1 d 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 C1 0.049(4) 0.047(4) 0.031(3) -0.009(3) -0.009(3) 0.018(4) C2 0.056(5) 0.043(4) 0.033(3) -0.005(3) -0.004(3) 0.016(4) C3 0.049(5) 0.057(5) 0.040(4) 0.001(4) 0.002(3) 0.007(4) C4 0.025(3) 0.055(5) 0.042(4) -0.001(3) 0.006(3) 0.012(3) C5 0.083(6) 0.043(5) 0.056(5) 0.005(4) 0.035(4) 0.032(4) C6 0.063(5) 0.055(5) 0.054(5) 0.006(4) 0.012(4) 0.027(4) C7 0.040(4) 0.034(4) 0.049(4) -0.008(3) -0.014(3) 0.015(3) C8 0.035(4) 0.032(4) 0.043(4) -0.002(3) -0.012(3) 0.011(3) C9 0.029(3) 0.033(4) 0.037(3) 0.005(3) 0.000(3) 0.006(3) C10 0.032(4) 0.031(4) 0.049(4) 0.014(3) -0.002(3) 0.004(3) C11 0.051(5) 0.037(4) 0.059(5) 0.011(4) 0.001(4) -0.001(4) C12 0.054(5) 0.029(4) 0.053(4) -0.001(3) -0.008(4) 0.004(3) C13 0.027(3) 0.042(4) 0.030(3) 0.007(3) 0.002(2) 0.013(3) C14 0.018(3) 0.070(5) 0.024(3) 0.014(3) -0.005(2) 0.001(3) C15 0.042(4) 0.074(6) 0.044(4) 0.007(4) -0.015(3) 0.021(4) C16 0.053(5) 0.088(7) 0.047(4) 0.023(4) 0.000(4) 0.040(5) C17 0.072(6) 0.053(5) 0.060(5) 0.027(4) 0.005(4) 0.028(5) C18 0.046(4) 0.041(4) 0.047(4) 0.011(3) 0.002(3) 0.015(3) C19 0.033(3) 0.024(3) 0.042(3) 0.004(3) 0.001(3) 0.006(3) C20 0.038(4) 0.058(5) 0.044(4) 0.018(3) 0.009(3) 0.025(4) C21 0.047(5) 0.088(6) 0.054(5) 0.018(4) 0.013(4) 0.037(5) C22 0.059(5) 0.078(6) 0.041(4) 0.021(4) 0.018(4) 0.035(5) C23 0.048(4) 0.064(5) 0.037(4) 0.013(3) 0.006(3) 0.023(4) C24 0.029(3) 0.052(4) 0.039(4) 0.012(3) -0.003(3) 0.015(3) C25 0.026(3) 0.036(4) 0.040(4) -0.010(3) -0.003(3) 0.008(3) C26 0.048(4) 0.043(4) 0.051(4) -0.003(3) 0.007(3) 0.015(4) C27 0.050(5) 0.041(4) 0.062(5) -0.005(4) -0.011(4) 0.011(4) C28 0.025(3) 0.047(4) 0.041(4) -0.011(3) -0.016(3) 0.002(3) C29 0.049(5) 0.069(5) 0.046(4) -0.006(4) -0.003(3) 0.026(4) C30 0.048(5) 0.066(5) 0.043(4) -0.003(4) 0.006(3) 0.027(4) C31 0.035(4) 0.040(4) 0.037(4) -0.009(3) 0.004(3) 0.007(3) C32 0.032(3) 0.041(4) 0.027(3) -0.003(3) -0.003(3) 0.008(3) C33 0.023(3) 0.038(4) 0.031(3) 0.004(3) 0.003(2) 0.003(3) C34 0.039(4) 0.054(4) 0.036(4) 0.008(3) 0.001(3) 0.021(3) C35 0.054(5) 0.055(5) 0.040(4) 0.014(3) -0.008(3) 0.022(4) C36 0.050(4) 0.047(4) 0.030(3) 0.005(3) 0.005(3) 0.009(4) C37 0.026(3) 0.028(3) 0.033(3) -0.002(3) 0.004(2) 0.009(3) C38 0.032(4) 0.041(4) 0.043(4) 0.005(3) -0.003(3) 0.006(3) C39 0.044(4) 0.045(4) 0.060(5) 0.019(4) -0.001(4) 0.004(4) C40 0.030(4) 0.044(4) 0.067(5) 0.008(4) -0.010(3) 0.006(3) C41 0.038(4) 0.042(4) 0.052(4) -0.007(3) -0.013(3) 0.007(3) C42 0.014(3) 0.040(4) 0.026(3) -0.009(3) -0.002(2) 0.006(3) C43 0.022(3) 0.030(3) 0.031(3) 0.003(3) -0.002(2) 0.000(3) C44 0.038(4) 0.038(4) 0.046(4) 0.005(3) 0.011(3) 0.012(3) C45 0.058(5) 0.047(5) 0.055(4) 0.008(4) 0.016(4) 0.029(4) C46 0.061(5) 0.042(4) 0.052(4) 0.000(3) 0.011(4) 0.022(4) C47 0.057(5) 0.029(4) 0.055(4) 0.003(3) -0.003(4) 0.008(3) C48 0.035(4) 0.038(4) 0.047(4) 0.005(3) -0.001(3) 0.011(3) C49 0.043(4) 0.046(4) 0.038(4) 0.002(3) 0.006(3) 0.015(3) C51 0.070(6) 0.060(5) 0.047(4) 0.015(4) -0.002(4) 0.028(4) C52 0.041(4) 0.039(4) 0.040(4) 0.003(3) 0.005(3) 0.013(3) C53 0.065(6) 0.047(5) 0.067(5) 0.015(4) 0.013(4) 0.001(4) N1 0.041(3) 0.038(3) 0.034(3) -0.002(2) -0.006(2) 0.018(3) N2 0.025(3) 0.029(3) 0.039(3) 0.001(2) -0.010(2) 0.007(2) N3 0.028(3) 0.037(3) 0.036(3) -0.004(2) 0.002(2) 0.007(2) N4 0.028(3) 0.033(3) 0.033(3) -0.001(2) -0.004(2) 0.009(2) N5 0.037(3) 0.041(3) 0.027(3) 0.000(2) 0.007(2) 0.003(3) N6 0.041(3) 0.045(4) 0.036(3) -0.002(3) -0.001(3) 0.012(3) N7 0.130(8) 0.043(5) 0.072(5) 0.011(5) 0.029(6) 0.013(5) C54 0.130(8) 0.043(5) 0.072(5) 0.011(5) 0.029(6) 0.013(5) C55 0.130(8) 0.043(5) 0.072(5) 0.011(5) 0.029(6) 0.013(5) N7A 0.130(8) 0.043(5) 0.072(5) 0.011(5) 0.029(6) 0.013(5) C54A 0.130(8) 0.043(5) 0.072(5) 0.011(5) 0.029(6) 0.013(5) C55A 0.130(8) 0.043(5) 0.072(5) 0.011(5) 0.029(6) 0.013(5) N8 0.067(5) 0.109(7) 0.085(5) -0.001(4) 0.004(4) 0.040(5) C56 0.067(5) 0.109(7) 0.085(5) -0.001(4) 0.004(4) 0.040(5) C57 0.067(5) 0.109(7) 0.085(5) -0.001(4) 0.004(4) 0.040(5) N8A 0.067(5) 0.109(7) 0.085(5) -0.001(4) 0.004(4) 0.040(5) C56A 0.067(5) 0.109(7) 0.085(5) -0.001(4) 0.004(4) 0.040(5) C57A 0.067(5) 0.109(7) 0.085(5) -0.001(4) 0.004(4) 0.040(5) O1 0.061(4) 0.079(4) 0.064(4) 0.001(3) 0.006(3) -0.001(3) O2 0.066(4) 0.084(5) 0.073(4) 0.030(4) 0.024(3) 0.003(4) O3 0.083(5) 0.061(4) 0.081(4) 0.012(3) 0.016(3) 0.030(4) O4 0.075(4) 0.071(4) 0.078(4) 0.027(3) -0.016(3) 0.015(3) O5 0.086(5) 0.074(4) 0.074(4) 0.003(3) -0.001(3) 0.005(3) O6 0.086(5) 0.074(4) 0.074(4) 0.003(3) -0.001(3) 0.005(3) O7 0.086(5) 0.074(4) 0.074(4) 0.003(3) -0.001(3) 0.005(3) O8 0.086(5) 0.074(4) 0.074(4) 0.003(3) -0.001(3) 0.005(3) O5A 0.086(5) 0.074(4) 0.074(4) 0.003(3) -0.001(3) 0.005(3) O6A 0.086(5) 0.074(4) 0.074(4) 0.003(3) -0.001(3) 0.005(3) O7A 0.086(5) 0.074(4) 0.074(4) 0.003(3) -0.001(3) 0.005(3) O8A 0.086(5) 0.074(4) 0.074(4) 0.003(3) -0.001(3) 0.005(3) P1 0.0241(8) 0.0307(9) 0.0338(8) 0.0046(7) -0.0037(6) 0.0066(7) P2 0.0235(8) 0.0326(9) 0.0288(8) 0.0021(6) -0.0002(6) 0.0054(7) S1 0.0479(11) 0.0572(12) 0.0529(11) 0.0188(9) 0.0060(9) 0.0151(10) S2 0.0433(11) 0.0591(13) 0.0464(10) -0.0051(9) 0.0021(8) 0.0147(9) Cu1 0.0287(4) 0.0329(4) 0.0325(4) 0.0015(3) -0.0039(3) 0.0065(3) Cu2 0.0262(4) 0.0327(4) 0.0325(4) 0.0006(3) -0.0021(3) 0.0050(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 C1 C2 1.374(11) . ? C1 C6 1.392(10) . ? C1 N1 1.422(9) . ? C2 C3 1.388(11) . ? C2 H2 0.9500 . ? C3 C4 1.365(11) . ? C3 H3 0.9500 . ? C4 C5 1.367(11) . ? C4 H4 0.9500 . ? C5 C6 1.406(11) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 N1 1.266(9) . ? C7 C8 1.449(10) . ? C7 H7 0.9500 . ? C8 N2 1.355(8) . ? C8 C12 1.382(10) . ? C9 N2 1.324(8) . ? C9 C10 1.410(9) . ? C9 P1 1.847(7) . ? C10 C11 1.401(10) . ? C10 H10 0.9500 . ? C11 C12 1.386(11) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.393(10) . ? C13 C14 1.429(9) . ? C13 P1 1.834(6) . ? C14 C15 1.426(9) . ? C14 H14 0.9500 . ? C15 C16 1.391(12) . ? C15 H15 0.9500 . ? C16 C17 1.380(13) . ? C16 H16 0.9500 . ? C17 C18 1.390(10) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.381(9) . ? C19 C24 1.387(9) . ? C19 P1 1.835(7) . ? C20 C21 1.388(10) . ? C20 H20 0.9500 . ? C21 C22 1.385(11) . ? C21 H21 0.9500 . ? C22 C23 1.371(10) . ? C22 H22 0.9500 . ? C23 C24 1.383(10) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.371(10) . ? C25 C30 1.380(10) . ? C25 N3 1.447(8) . ? C26 C27 1.405(10) . ? C26 H26 0.9500 . ? C27 C28 1.418(11) . ? C27 H27 0.9500 . ? C28 C29 1.402(11) . ? C28 H28 0.9500 . ? C29 C30 1.443(11) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 N3 1.255(9) . ? C31 C32 1.478(9) . ? C31 H31 0.9500 . ? C32 N4 1.347(8) . ? C32 C36 1.379(9) . ? C33 N4 1.350(8) . ? C33 C34 1.374(9) . ? C33 P2 1.846(6) . ? C34 C35 1.375(10) . ? C34 H34 0.9500 . ? C35 C36 1.389(10) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.380(9) . ? C37 C42 1.381(8) . ? C37 P2 1.814(6) . ? C38 C39 1.396(10) . ? C38 H38 0.9500 . ? C39 C40 1.428(11) . ? C39 H39 0.9500 . ? C40 C41 1.368(11) . ? C40 H40 0.9500 . ? C41 C42 1.353(9) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.397(9) . ? C43 C48 1.398(9) . ? C43 P2 1.827(6) . ? C44 C45 1.356(10) . ? C44 H44 0.9500 . ? C45 C46 1.380(12) . ? C45 H45 0.9500 . ? C46 C47 1.363(11) . ? C46 H46 0.9500 . ? C47 C48 1.394(10) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 N5 1.163(9) . ? C49 C51 1.443(10) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 N6 1.129(9) . ? C52 C53 1.465(11) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? N1 Cu1 2.146(5) . ? N2 Cu1 2.066(5) . ? N3 Cu2 2.121(5) . ? N4 Cu2 2.064(5) . ? N5 Cu1 1.943(6) . ? N6 Cu2 1.964(7) . ? N7 C54 1.162(12) . ? C54 C55 1.419(12) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? N7A C54A 1.162(12) . ? C54A C55A 1.420(12) . ? C55A H55D 0.9800 . ? C55A H55E 0.9800 . ? C55A H55F 0.9800 . ? N8 C56 1.159(11) . ? C56 C57 1.414(12) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? N8A C56A 1.156(12) . ? C56A C57A 1.413(12) . ? C57A H57D 0.9800 . ? C57A H57E 0.9800 . ? C57A H57F 0.9800 . ? O1 S1 1.515(6) . ? O1 H1 0.8400 . ? O2 S1 1.415(6) . ? O3 S1 1.512(6) . ? O4 S1 1.435(6) . ? O5 S2 1.518(15) . ? O6 S2 1.47(2) . ? O6 H6A 0.8400 . ? O7 S2 1.391(19) . ? O8 S2 1.399(18) . ? O5A S2 1.365(15) . ? O6A S2 1.58(2) . ? O6A H6A1 0.8400 . ? O7A S2 1.513(17) . ? O8A S2 1.532(19) . ? P1 Cu2 2.2012(19) . ? P2 Cu1 2.2103(18) . ? 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 C2 C1 C6 118.8(7) . . ? C2 C1 N1 116.9(6) . . ? C6 C1 N1 124.3(7) . . ? C1 C2 C3 121.5(7) . . ? C1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C4 C3 C2 120.2(8) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 118.1(7) . . ? C3 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? C4 C5 C6 122.0(7) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C1 C6 C5 118.1(8) . . ? C1 C6 H6 120.9 . . ? C5 C6 H6 120.9 . . ? N1 C7 C8 120.3(6) . . ? N1 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? N2 C8 C12 121.5(7) . . ? N2 C8 C7 116.3(6) . . ? C12 C8 C7 122.1(6) . . ? N2 C9 C10 122.4(6) . . ? N2 C9 P1 115.9(5) . . ? C10 C9 P1 121.6(5) . . ? C11 C10 C9 118.1(7) . . ? C11 C10 H10 121.0 . . ? C9 C10 H10 121.0 . . ? C12 C11 C10 118.6(7) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? C8 C12 C11 119.8(7) . . ? C8 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C18 C13 C14 122.3(6) . . ? C18 C13 P1 118.0(5) . . ? C14 C13 P1 119.7(5) . . ? C15 C14 C13 115.8(7) . . ? C15 C14 H14 122.1 . . ? C13 C14 H14 122.1 . . ? C16 C15 C14 121.2(7) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C17 C16 C15 120.5(7) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 120.8(8) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C17 C18 C13 119.0(7) . . ? C17 C18 H18 120.5 . . ? C13 C18 H18 120.5 . . ? C20 C19 C24 119.5(6) . . ? C20 C19 P1 123.5(5) . . ? C24 C19 P1 116.9(5) . . ? C19 C20 C21 120.1(6) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 120.0(7) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C21 119.8(7) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 120.4(7) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C19 120.0(6) . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? C26 C25 C30 120.3(6) . . ? C26 C25 N3 117.2(6) . . ? C30 C25 N3 122.3(7) . . ? C25 C26 C27 120.5(7) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C26 C27 C28 121.5(8) . . ? C26 C27 H27 119.2 . . ? C28 C27 H27 119.2 . . ? C29 C28 C27 117.1(7) . . ? C29 C28 H28 121.4 . . ? C27 C28 H28 121.4 . . ? C28 C29 C30 120.3(7) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C25 C30 C29 120.0(7) . . ? C25 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? N3 C31 C32 119.2(6) . . ? N3 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? N4 C32 C36 123.3(6) . . ? N4 C32 C31 114.4(6) . . ? C36 C32 C31 122.3(6) . . ? N4 C33 C34 121.5(6) . . ? N4 C33 P2 112.8(4) . . ? C34 C33 P2 125.3(5) . . ? C33 C34 C35 120.4(6) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C34 C35 C36 118.6(6) . . ? C34 C35 H35 120.7 . . ? C36 C35 H35 120.7 . . ? C32 C36 C35 118.2(6) . . ? C32 C36 H36 120.9 . . ? C35 C36 H36 120.9 . . ? C38 C37 C42 116.6(6) . . ? C38 C37 P2 118.0(5) . . ? C42 C37 P2 125.4(5) . . ? C37 C38 C39 121.5(6) . . ? C37 C38 H38 119.3 . . ? C39 C38 H38 119.3 . . ? C38 C39 C40 118.3(7) . . ? C38 C39 H39 120.9 . . ? C40 C39 H39 120.9 . . ? C41 C40 C39 120.2(7) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C42 C41 C40 118.3(6) . . ? C42 C41 H41 120.8 . . ? C40 C41 H41 120.8 . . ? C41 C42 C37 124.8(6) . . ? C41 C42 H42 117.6 . . ? C37 C42 H42 117.6 . . ? C44 C43 C48 118.0(6) . . ? C44 C43 P2 123.9(5) . . ? C48 C43 P2 117.5(5) . . ? C45 C44 C43 120.6(7) . . ? C45 C44 H44 119.7 . . ? C43 C44 H44 119.7 . . ? C44 C45 C46 121.4(8) . . ? C44 C45 H45 119.3 . . ? C46 C45 H45 119.3 . . ? C47 C46 C45 119.3(7) . . ? C47 C46 H46 120.4 . . ? C45 C46 H46 120.4 . . ? C46 C47 C48 120.5(7) . . ? C46 C47 H47 119.7 . . ? C48 C47 H47 119.7 . . ? C47 C48 C43 120.1(7) . . ? C47 C48 H48 120.0 . . ? C43 C48 H48 120.0 . . ? N5 C49 C51 177.1(8) . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N6 C52 C53 177.7(8) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C7 N1 C1 121.9(6) . . ? C7 N1 Cu1 110.6(5) . . ? C1 N1 Cu1 126.8(5) . . ? C9 N2 C8 119.4(6) . . ? C9 N2 Cu1 128.2(4) . . ? C8 N2 Cu1 112.0(4) . . ? C31 N3 C25 122.5(6) . . ? C31 N3 Cu2 113.2(4) . . ? C25 N3 Cu2 124.0(4) . . ? C32 N4 C33 117.8(5) . . ? C32 N4 Cu2 114.1(4) . . ? C33 N4 Cu2 127.8(4) . . ? C49 N5 Cu1 175.4(5) . . ? C52 N6 Cu2 175.7(6) . . ? N7 C54 C55 166(3) . . ? N7A C54A C55A 167(3) . . ? C54A C55A H55D 109.5 . . ? C54A C55A H55E 109.5 . . ? H55D C55A H55E 109.5 . . ? C54A C55A H55F 109.5 . . ? H55D C55A H55F 109.5 . . ? H55E C55A H55F 109.5 . . ? N8 C56 C57 174.4(18) . . ? C56 C57 H57D 125.5 . . ? C56 C57 H57E 104.6 . . ? H57A C57 H57E 110.5 . . ? H57C C57 H57E 113.2 . . ? N8A C56A C57A 173(4) . . ? C56A C57A H57D 109.6 . . ? C56A C57A H57E 109.2 . . ? H57D C57A H57E 109.5 . . ? C56A C57A H57F 109.6 . . ? H57D C57A H57F 109.5 . . ? H57E C57A H57F 109.5 . . ? S1 O1 H1 109.5 . . ? S2 O6 H6A 109.5 . . ? S2 O6A H6A1 109.5 . . ? C13 P1 C19 103.9(3) . . ? C13 P1 C9 102.1(3) . . ? C19 P1 C9 100.9(3) . . ? C13 P1 Cu2 118.6(2) . . ? C19 P1 Cu2 109.3(2) . . ? C9 P1 Cu2 119.8(2) . . ? C37 P2 C43 103.6(3) . . ? C37 P2 C33 100.2(3) . . ? C43 P2 C33 102.6(3) . . ? C37 P2 Cu1 120.0(2) . . ? C43 P2 Cu1 108.55(19) . . ? C33 P2 Cu1 119.6(2) . . ? O2 S1 O4 115.0(4) . . ? O2 S1 O3 108.8(4) . . ? O4 S1 O3 110.8(4) . . ? O2 S1 O1 107.6(4) . . ? O4 S1 O1 108.5(4) . . ? O3 S1 O1 105.7(4) . . ? O5A S2 O7 124.2(9) . . ? O5A S2 O8 85.0(9) . . ? O7 S2 O8 120.4(10) . . ? O5A S2 O6 90.0(9) . . ? O7 S2 O6 119.3(13) . . ? O8 S2 O6 109.9(13) . . ? O5A S2 O7A 112.3(9) . . ? O7 S2 O7A 101.7(9) . . ? O6 S2 O7A 109.0(10) . . ? O5A S2 O5 45.3(7) . . ? O7 S2 O5 79.8(9) . . ? O8 S2 O5 117.4(9) . . ? O6 S2 O5 106.0(9) . . ? O7A S2 O5 138.2(8) . . ? O5A S2 O8A 148.3(9) . . ? O7A S2 O8A 85.0(9) . . ? O5 S2 O8A 104.0(9) . . ? O5A S2 O6A 107.9(9) . . ? O7 S2 O6A 109.4(10) . . ? O8 S2 O6A 107.1(11) . . ? O7A S2 O6A 98.2(10) . . ? O5 S2 O6A 121.0(9) . . ? O8A S2 O6A 94.9(10) . . ? N5 Cu1 N2 112.9(2) . . ? N5 Cu1 N1 106.1(2) . . ? N2 Cu1 N1 79.4(2) . . ? N5 Cu1 P2 127.07(17) . . ? N2 Cu1 P2 114.47(15) . . ? N1 Cu1 P2 104.48(15) . . ? N6 Cu2 N4 110.3(2) . . ? N6 Cu2 N3 104.8(2) . . ? N4 Cu2 N3 78.5(2) . . ? N6 Cu2 P1 132.28(17) . . ? N4 Cu2 P1 112.90(16) . . ? N3 Cu2 P1 102.58(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.6(10) . . . . ? N1 C1 C2 C3 -179.4(6) . . . . ? C1 C2 C3 C4 -4.1(11) . . . . ? C2 C3 C4 C5 10.5(11) . . . . ? C3 C4 C5 C6 -13.9(12) . . . . ? C2 C1 C6 C5 -3.6(11) . . . . ? N1 C1 C6 C5 176.3(7) . . . . ? C4 C5 C6 C1 10.5(13) . . . . ? N1 C7 C8 N2 0.0(9) . . . . ? N1 C7 C8 C12 -179.3(6) . . . . ? N2 C9 C10 C11 1.6(10) . . . . ? P1 C9 C10 C11 -176.1(5) . . . . ? C9 C10 C11 C12 -1.6(10) . . . . ? N2 C8 C12 C11 -2.0(10) . . . . ? C7 C8 C12 C11 177.3(6) . . . . ? C10 C11 C12 C8 1.8(11) . . . . ? C18 C13 C14 C15 6.1(10) . . . . ? P1 C13 C14 C15 -174.3(5) . . . . ? C13 C14 C15 C16 -4.6(11) . . . . ? C14 C15 C16 C17 0.9(12) . . . . ? C15 C16 C17 C18 1.6(13) . . . . ? C16 C17 C18 C13 -0.2(12) . . . . ? C14 C13 C18 C17 -3.8(10) . . . . ? P1 C13 C18 C17 176.6(6) . . . . ? C24 C19 C20 C21 1.4(11) . . . . ? P1 C19 C20 C21 176.6(6) . . . . ? C19 C20 C21 C22 1.7(13) . . . . ? C20 C21 C22 C23 -1.8(14) . . . . ? C21 C22 C23 C24 -1.2(13) . . . . ? C22 C23 C24 C19 4.3(12) . . . . ? C20 C19 C24 C23 -4.4(11) . . . . ? P1 C19 C24 C23 -180.0(6) . . . . ? C30 C25 C26 C27 -1.3(11) . . . . ? N3 C25 C26 C27 -178.0(6) . . . . ? C25 C26 C27 C28 -0.6(11) . . . . ? C26 C27 C28 C29 3.9(10) . . . . ? C27 C28 C29 C30 -5.2(10) . . . . ? C26 C25 C30 C29 -0.1(11) . . . . ? N3 C25 C30 C29 176.4(6) . . . . ? C28 C29 C30 C25 3.5(11) . . . . ? N3 C31 C32 N4 -2.5(9) . . . . ? N3 C31 C32 C36 177.5(7) . . . . ? N4 C33 C34 C35 2.5(11) . . . . ? P2 C33 C34 C35 -169.8(6) . . . . ? C33 C34 C35 C36 0.7(11) . . . . ? N4 C32 C36 C35 1.4(11) . . . . ? C31 C32 C36 C35 -178.6(7) . . . . ? C34 C35 C36 C32 -2.6(11) . . . . ? C42 C37 C38 C39 -4.6(10) . . . . ? P2 C37 C38 C39 174.3(6) . . . . ? C37 C38 C39 C40 1.2(11) . . . . ? C38 C39 C40 C41 1.2(11) . . . . ? C39 C40 C41 C42 0.1(11) . . . . ? C40 C41 C42 C37 -4.0(10) . . . . ? C38 C37 C42 C41 6.2(9) . . . . ? P2 C37 C42 C41 -172.6(5) . . . . ? C48 C43 C44 C45 0.1(10) . . . . ? P2 C43 C44 C45 171.5(6) . . . . ? C43 C44 C45 C46 0.8(11) . . . . ? C44 C45 C46 C47 -0.7(12) . . . . ? C45 C46 C47 C48 -0.4(12) . . . . ? C46 C47 C48 C43 1.3(11) . . . . ? C44 C43 C48 C47 -1.1(10) . . . . ? P2 C43 C48 C47 -173.1(5) . . . . ? C8 C7 N1 C1 -179.9(5) . . . . ? C8 C7 N1 Cu1 -8.5(7) . . . . ? C2 C1 N1 C7 -162.9(6) . . . . ? C6 C1 N1 C7 17.2(10) . . . . ? C2 C1 N1 Cu1 27.2(8) . . . . ? C6 C1 N1 Cu1 -152.8(6) . . . . ? C10 C9 N2 C8 -1.8(9) . . . . ? P1 C9 N2 C8 176.1(4) . . . . ? C10 C9 N2 Cu1 170.8(4) . . . . ? P1 C9 N2 Cu1 -11.3(7) . . . . ? C12 C8 N2 C9 1.9(9) . . . . ? C7 C8 N2 C9 -177.4(5) . . . . ? C12 C8 N2 Cu1 -171.8(5) . . . . ? C7 C8 N2 Cu1 8.9(7) . . . . ? C32 C31 N3 C25 -178.1(6) . . . . ? C32 C31 N3 Cu2 -3.9(8) . . . . ? C26 C25 N3 C31 -151.5(7) . . . . ? C30 C25 N3 C31 31.9(10) . . . . ? C26 C25 N3 Cu2 35.0(8) . . . . ? C30 C25 N3 Cu2 -141.6(6) . . . . ? C36 C32 N4 C33 1.7(10) . . . . ? C31 C32 N4 C33 -178.3(6) . . . . ? C36 C32 N4 Cu2 -172.3(5) . . . . ? C31 C32 N4 Cu2 7.7(7) . . . . ? C34 C33 N4 C32 -3.7(9) . . . . ? P2 C33 N4 C32 169.5(5) . . . . ? C34 C33 N4 Cu2 169.4(5) . . . . ? P2 C33 N4 Cu2 -17.4(7) . . . . ? C18 C13 P1 C19 -111.7(5) . . . . ? C14 C13 P1 C19 68.7(5) . . . . ? C18 C13 P1 C9 143.7(5) . . . . ? C14 C13 P1 C9 -35.9(6) . . . . ? C18 C13 P1 Cu2 9.7(6) . . . . ? C14 C13 P1 Cu2 -169.9(4) . . . . ? C20 C19 P1 C13 17.3(7) . . . . ? C24 C19 P1 C13 -167.3(5) . . . . ? C20 C19 P1 C9 122.8(6) . . . . ? C24 C19 P1 C9 -61.8(6) . . . . ? C20 C19 P1 Cu2 -110.1(6) . . . . ? C24 C19 P1 Cu2 65.3(5) . . . . ? N2 C9 P1 C13 -95.5(5) . . . . ? C10 C9 P1 C13 82.4(6) . . . . ? N2 C9 P1 C19 157.6(5) . . . . ? C10 C9 P1 C19 -24.5(6) . . . . ? N2 C9 P1 Cu2 37.8(5) . . . . ? C10 C9 P1 Cu2 -144.3(5) . . . . ? C38 C37 P2 C43 -99.2(5) . . . . ? C42 C37 P2 C43 79.7(5) . . . . ? C38 C37 P2 C33 155.1(5) . . . . ? C42 C37 P2 C33 -26.1(6) . . . . ? C38 C37 P2 Cu1 22.0(6) . . . . ? C42 C37 P2 Cu1 -159.2(4) . . . . ? C44 C43 P2 C37 17.5(6) . . . . ? C48 C43 P2 C37 -171.0(5) . . . . ? C44 C43 P2 C33 121.4(6) . . . . ? C48 C43 P2 C33 -67.1(5) . . . . ? C44 C43 P2 Cu1 -111.1(5) . . . . ? C48 C43 P2 Cu1 60.4(5) . . . . ? N4 C33 P2 C37 -86.6(5) . . . . ? C34 C33 P2 C37 86.3(6) . . . . ? N4 C33 P2 C43 166.9(4) . . . . ? C34 C33 P2 C43 -20.3(7) . . . . ? N4 C33 P2 Cu1 46.7(5) . . . . ? C34 C33 P2 Cu1 -140.4(5) . . . . ? C9 N2 Cu1 N5 73.8(5) . . . . ? C8 N2 Cu1 N5 -113.1(4) . . . . ? C9 N2 Cu1 N1 177.0(5) . . . . ? C8 N2 Cu1 N1 -9.9(4) . . . . ? C9 N2 Cu1 P2 -81.8(5) . . . . ? C8 N2 Cu1 P2 91.3(4) . . . . ? C7 N1 Cu1 N5 120.9(5) . . . . ? C1 N1 Cu1 N5 -68.2(5) . . . . ? C7 N1 Cu1 N2 10.0(4) . . . . ? C1 N1 Cu1 N2 -179.1(5) . . . . ? C7 N1 Cu1 P2 -102.8(4) . . . . ? C1 N1 Cu1 P2 68.1(5) . . . . ? C37 P2 Cu1 N5 16.0(3) . . . . ? C43 P2 Cu1 N5 134.7(3) . . . . ? C33 P2 Cu1 N5 -108.2(3) . . . . ? C37 P2 Cu1 N2 167.6(3) . . . . ? C43 P2 Cu1 N2 -73.7(3) . . . . ? C33 P2 Cu1 N2 43.3(3) . . . . ? C37 P2 Cu1 N1 -107.7(3) . . . . ? C43 P2 Cu1 N1 11.0(3) . . . . ? C33 P2 Cu1 N1 128.1(3) . . . . ? C32 N4 Cu2 N6 -109.2(5) . . . . ? C33 N4 Cu2 N6 77.5(6) . . . . ? C32 N4 Cu2 N3 -7.4(4) . . . . ? C33 N4 Cu2 N3 179.3(6) . . . . ? C32 N4 Cu2 P1 91.6(4) . . . . ? C33 N4 Cu2 P1 -81.8(5) . . . . ? C31 N3 Cu2 N6 114.3(5) . . . . ? C25 N3 Cu2 N6 -71.6(5) . . . . ? C31 N3 Cu2 N4 6.1(5) . . . . ? C25 N3 Cu2 N4 -179.9(5) . . . . ? C31 N3 Cu2 P1 -105.1(5) . . . . ? C25 N3 Cu2 P1 68.9(5) . . . . ? C13 P1 Cu2 N6 23.7(3) . . . . ? C19 P1 Cu2 N6 142.3(3) . . . . ? C9 P1 Cu2 N6 -102.2(3) . . . . ? C13 P1 Cu2 N4 177.0(3) . . . . ? C19 P1 Cu2 N4 -64.3(3) . . . . ? C9 P1 Cu2 N4 51.2(3) . . . . ? C13 P1 Cu2 N3 -100.3(3) . . . . ? C19 P1 Cu2 N3 18.4(3) . . . . ? C9 P1 Cu2 N3 133.9(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O3 0.84 1.82 2.628(9) 160.5 2_757 O1 H1 S1 0.84 2.83 3.517(7) 140.6 2_757 O6 H6A O4 0.84 2.05 2.69(2) 132.5 . O6A H6A1 O4 0.84 1.94 2.70(2) 150.1 . _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.441 _refine_diff_density_min -0.705 _refine_diff_density_rms 0.128 data_jn1027 _database_code_depnum_ccdc_archive 'CCDC 815066' #TrackingRef '- combined.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C104 H80 Cu4 N8 O4 P4, 2(B F4), 1.5(H2 O), 2(C4 H10 O), (C2 H3 N) ; _chemical_formula_sum 'C114 H106 B2 Cu4 F8 N9 O7.50 P4' _chemical_formula_weight 2273.74 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 orthorhombic _symmetry_space_group_name_H-M pbam _symmetry_space_group_name_Hall '-P 2 2ab' _symmetry_Int_Tables_number 55 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y, -z' '-x-1/2, y-1/2, z' 'x-1/2, -y-1/2, z' _cell_length_a 12.147(2) _cell_length_b 18.712(4) _cell_length_c 23.253(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5285.3(18) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 125741 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 28.28 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2342 _exptl_absorpt_coefficient_mu 0.930 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.775 _exptl_absorpt_correction_T_max 0.906 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 51480 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0193 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.67 _diffrn_reflns_theta_max 28.27 _reflns_number_total 6686 _reflns_number_gt 6023 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-97 (Altomare et al. 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_molecular_graphics ;ORTEP-3 (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material 'enCIFer 1.1 (CCDC, 2005)' _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^)+(0.0337P)^2^+6.5054P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6686 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.0967 _refine_ls_wR_factor_gt 0.0940 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.119 _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 C1 C -0.21972(16) -0.20214(10) 0.29781(9) 0.0235(4) Uani 1 1 d . . . C2 C -0.21882(19) -0.18146(12) 0.35528(9) 0.0322(5) Uani 1 1 d . . . H2 H -0.1698 -0.1451 0.3679 0.039 Uiso 1 1 calc R . . C3 C -0.2893(2) -0.21381(14) 0.39411(10) 0.0390(5) Uani 1 1 d . . . H3 H -0.2879 -0.2000 0.4334 0.047 Uiso 1 1 calc R . . C4 C -0.3619(2) -0.26615(13) 0.37602(11) 0.0361(5) Uani 1 1 d . . . H4 H -0.4093 -0.2888 0.4029 0.043 Uiso 1 1 calc R . . C5 C -0.36499(19) -0.28534(12) 0.31856(11) 0.0339(5) Uani 1 1 d . . . H5 H -0.4156 -0.3208 0.3060 0.041 Uiso 1 1 calc R . . C6 C -0.29491(18) -0.25328(12) 0.27920(10) 0.0301(4) Uani 1 1 d . . . H6 H -0.2982 -0.2662 0.2397 0.036 Uiso 1 1 calc R . . C7 C -0.10463(17) -0.20128(11) 0.21627(9) 0.0252(4) Uani 1 1 d . . . H7 H -0.1396 -0.2438 0.2033 0.030 Uiso 1 1 calc R . . C8 C -0.01187(17) -0.17087(10) 0.18403(8) 0.0231(4) Uani 1 1 d . . . C9 C 0.12327(16) -0.08332(10) 0.18153(8) 0.0215(4) Uani 1 1 d . . . C10 C 0.16532(18) -0.11119(12) 0.13040(9) 0.0298(4) Uani 1 1 d . . . H10 H 0.2276 -0.0898 0.1126 0.036 Uiso 1 1 calc R . . C11 C 0.1154(2) -0.17040(13) 0.10580(10) 0.0351(5) Uani 1 1 d . . . H11 H 0.1425 -0.1898 0.0708 0.042 Uiso 1 1 calc R . . C12 C 0.02545(19) -0.20091(12) 0.13289(9) 0.0311(5) Uani 1 1 d . . . H12 H -0.0101 -0.2415 0.1169 0.037 Uiso 1 1 calc R . . C13 C 0.25275(17) 0.04242(10) 0.16508(8) 0.0228(4) Uani 1 1 d . . . C14 C 0.18860(19) 0.07127(12) 0.12109(9) 0.0296(4) Uani 1 1 d . . . H14 H 0.1128 0.0591 0.1186 0.036 Uiso 1 1 calc R . . C15 C 0.2339(2) 0.11744(13) 0.08090(9) 0.0358(5) Uani 1 1 d . . . H15 H 0.1891 0.1372 0.0514 0.043 Uiso 1 1 calc R . . C16 C 0.3443(2) 0.13456(13) 0.08393(10) 0.0396(6) Uani 1 1 d . . . H16 H 0.3756 0.1664 0.0567 0.048 Uiso 1 1 calc R . . C17 C 0.4086(2) 0.10555(15) 0.12622(12) 0.0438(6) Uani 1 1 d . . . H17 H 0.4849 0.1165 0.1274 0.053 Uiso 1 1 calc R . . C18 C 0.36377(19) 0.06017(13) 0.16758(11) 0.0345(5) Uani 1 1 d . . . H18 H 0.4089 0.0415 0.1974 0.041 Uiso 1 1 calc R . . C19 C 0.29161(17) -0.05016(11) 0.26281(9) 0.0253(4) Uani 1 1 d . . . C20 C 0.36702(19) -0.09722(13) 0.23837(11) 0.0347(5) Uani 1 1 d . . . H20 H 0.3620 -0.1085 0.1986 0.042 Uiso 1 1 calc R . . C21 C 0.4492(2) -0.12778(15) 0.27145(14) 0.0461(6) Uani 1 1 d . . . H21 H 0.5002 -0.1600 0.2544 0.055 Uiso 1 1 calc R . . C22 C 0.4569(3) -0.1117(2) 0.32835(15) 0.0647(9) Uani 1 1 d . . . H22 H 0.5139 -0.1322 0.3509 0.078 Uiso 1 1 calc R . . C23 C 0.3828(4) -0.0660(3) 0.35317(15) 0.0871(15) Uani 1 1 d . . . H23 H 0.3883 -0.0551 0.3930 0.104 Uiso 1 1 calc R . . C24 C 0.2991(3) -0.03517(19) 0.32031(12) 0.0566(8) Uani 1 1 d . . . H24 H 0.2474 -0.0039 0.3378 0.068 Uiso 1 1 calc R . . C25 C 0.0000 0.0000 0.37504(11) 0.0187(5) Uani 1 2 d S . . C26 C 0.0000 0.0000 0.43983(11) 0.0196(5) Uani 1 2 d S . . C27 C 0.01992(17) 0.06290(10) 0.47006(8) 0.0229(4) Uani 1 1 d . . . H27 H 0.0336 0.1060 0.4497 0.028 Uiso 1 1 calc R . . C28 C 0.3344(5) 0.0472(3) 0.5000 0.0821(18) Uani 1 2 d S . . H28A H 0.2800 0.0816 0.5143 0.123 Uiso 0.50 1 calc PR . . H28B H 0.3558 0.0602 0.4607 0.123 Uiso 0.50 1 calc PR . . H28C H 0.3994 0.0479 0.5249 0.123 Uiso 0.50 1 calc PR . . C29 C 0.2854(4) -0.0260(3) 0.5000 0.0681(14) Uani 1 2 d S . . H29A H 0.2386 -0.0324 0.5345 0.082 Uiso 0.50 1 calc PR . . H29B H 0.2386 -0.0324 0.4655 0.082 Uiso 0.50 1 calc PR . . C30 C 0.3312(5) -0.1483(3) 0.5000 0.091(2) Uani 1 2 d S . . H30A H 0.2852 -0.1565 0.4655 0.109 Uiso 0.50 1 calc PR . . H30B H 0.2852 -0.1565 0.5345 0.109 Uiso 0.50 1 calc PR . . C31 C 0.4270(5) -0.1991(3) 0.5000 0.0811(17) Uani 1 2 d S . . H31A H 0.4655 -0.1961 0.4630 0.122 Uiso 0.50 1 calc PR . . H31B H 0.4002 -0.2479 0.5058 0.122 Uiso 0.50 1 calc PR . . H31C H 0.4777 -0.1863 0.5311 0.122 Uiso 0.50 1 calc PR . . C32 C 0.3382(8) -0.0238(4) 0.0000 0.0423(17) Uani 0.50 2 d SP . . C33 C 0.4555(8) -0.0121(5) 0.0000 0.059(2) Uani 0.50 2 d SP . . H33A H 0.4814 -0.0066 -0.0397 0.088 Uiso 0.25 1 calc PR . . H33B H 0.4923 -0.0531 0.0178 0.088 Uiso 0.25 1 calc PR . . H33C H 0.4725 0.0313 0.0219 0.088 Uiso 0.25 1 calc PR . . N3 N 0.2444(7) -0.0329(4) 0.0000 0.0529(17) Uani 0.50 2 d SP . . O2W O 0.0000 0.0000 0.0377(8) 0.081(5) Uiso 0.25 2 d SP . 1 O1W O 0.0332(14) -0.0293(10) 0.0000 0.053(4) Uiso 0.25 2 d SP . 2 O3W O -0.017(2) 0.0383(15) 0.0193(11) 0.073(7) Uiso 0.125 1 d P . 3 B1 B 0.3740(4) -0.2054(3) 0.0000 0.0468(11) Uani 1 2 d S . . N1 N -0.13795(14) -0.16999(9) 0.26202(7) 0.0218(3) Uani 1 1 d . . . N2 N 0.03498(13) -0.11216(8) 0.20761(7) 0.0193(3) Uani 1 1 d . . . O1 O -0.02526(13) -0.05766(7) 0.35043(6) 0.0240(3) Uani 1 1 d . . . O2 O 0.3712(2) -0.07769(16) 0.5000 0.0496(7) Uani 1 2 d S . . F1 F 0.27158(17) -0.23667(11) 0.0000 0.0402(5) Uani 1 2 d S . . F2 F 0.38691(18) -0.16784(13) 0.05067(10) 0.0801(7) Uani 1 1 d . . . F3 F 0.4547(2) -0.2582(3) 0.0000 0.0964(13) Uani 1 2 d S . . P1 P 0.18264(4) -0.00747(3) 0.22120(2) 0.01873(10) Uani 1 1 d . . . Cu1 Cu -0.067333(19) -0.062622(12) 0.267068(9) 0.01907(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0239(9) 0.0198(9) 0.0267(9) -0.0013(7) 0.0002(8) -0.0009(7) C2 0.0361(11) 0.0326(11) 0.0278(10) -0.0039(9) 0.0013(9) -0.0111(9) C3 0.0458(14) 0.0434(13) 0.0279(11) -0.0020(10) 0.0057(10) -0.0107(11) C4 0.0334(11) 0.0355(12) 0.0393(12) 0.0042(10) 0.0087(10) -0.0075(10) C5 0.0285(10) 0.0298(11) 0.0435(13) -0.0043(9) 0.0024(10) -0.0098(9) C6 0.0264(10) 0.0306(11) 0.0333(11) -0.0061(9) -0.0001(9) -0.0054(8) C7 0.0277(10) 0.0212(9) 0.0266(9) -0.0048(8) -0.0006(8) -0.0034(8) C8 0.0267(9) 0.0198(9) 0.0228(9) -0.0032(7) -0.0006(8) 0.0001(7) C9 0.0236(9) 0.0201(8) 0.0207(9) -0.0006(7) 0.0013(7) 0.0021(7) C10 0.0319(11) 0.0303(10) 0.0271(10) -0.0052(8) 0.0099(9) -0.0011(9) C11 0.0439(13) 0.0341(11) 0.0275(10) -0.0110(9) 0.0107(10) -0.0016(10) C12 0.0383(12) 0.0271(10) 0.0278(10) -0.0102(8) 0.0029(9) -0.0017(9) C13 0.0262(9) 0.0205(9) 0.0217(9) 0.0005(7) 0.0043(8) 0.0005(7) C14 0.0312(11) 0.0351(11) 0.0225(9) 0.0033(8) 0.0028(8) 0.0022(9) C15 0.0466(13) 0.0383(12) 0.0226(10) 0.0072(9) 0.0025(9) 0.0034(11) C16 0.0532(15) 0.0338(12) 0.0319(12) 0.0085(9) 0.0107(11) -0.0072(11) C17 0.0374(13) 0.0455(14) 0.0487(15) 0.0141(12) 0.0044(11) -0.0132(11) C18 0.0283(11) 0.0364(12) 0.0387(12) 0.0113(10) -0.0016(9) -0.0069(9) C19 0.0223(9) 0.0252(9) 0.0284(10) 0.0054(8) -0.0016(8) 0.0013(8) C20 0.0299(11) 0.0309(11) 0.0432(13) 0.0017(9) -0.0009(10) 0.0062(9) C21 0.0334(12) 0.0359(13) 0.0691(19) 0.0088(12) -0.0052(12) 0.0092(10) C22 0.0522(17) 0.078(2) 0.064(2) 0.0169(18) -0.0201(16) 0.0251(17) C23 0.086(3) 0.134(4) 0.0416(17) -0.004(2) -0.0284(18) 0.052(3) C24 0.0577(17) 0.080(2) 0.0320(13) -0.0058(13) -0.0123(12) 0.0345(17) C25 0.0203(12) 0.0215(12) 0.0143(11) 0.000 0.000 -0.0011(10) C26 0.0221(12) 0.0216(12) 0.0151(11) 0.000 0.000 -0.0019(10) C27 0.0311(10) 0.0202(9) 0.0175(9) 0.0013(7) 0.0003(7) -0.0026(8) C28 0.064(3) 0.057(3) 0.126(5) 0.000 0.000 0.006(3) C29 0.037(2) 0.067(3) 0.101(4) 0.000 0.000 0.004(2) C30 0.058(3) 0.052(3) 0.164(7) 0.000 0.000 -0.006(2) C31 0.083(4) 0.061(3) 0.100(4) 0.000 0.000 0.009(3) C32 0.064(5) 0.033(3) 0.031(3) 0.000 0.000 0.008(3) C33 0.068(6) 0.042(5) 0.066(5) 0.000 0.000 0.002(4) N3 0.066(5) 0.049(4) 0.044(4) 0.000 0.000 0.016(4) B1 0.034(2) 0.073(3) 0.034(2) 0.000 0.000 -0.014(2) N1 0.0237(8) 0.0198(7) 0.0220(8) -0.0011(6) -0.0006(6) -0.0018(6) N2 0.0199(7) 0.0189(7) 0.0191(7) -0.0009(6) 0.0005(6) 0.0009(6) O1 0.0349(8) 0.0222(7) 0.0149(6) -0.0004(5) -0.0027(6) -0.0037(6) O2 0.0379(14) 0.0545(16) 0.0564(17) 0.000 0.000 0.0004(12) F1 0.0375(11) 0.0453(12) 0.0377(10) 0.000 0.000 -0.0095(9) F2 0.0752(13) 0.0905(16) 0.0746(13) -0.0315(12) -0.0176(11) -0.0219(12) F3 0.0505(16) 0.185(4) 0.0535(16) 0.000 0.000 0.048(2) P1 0.0195(2) 0.0187(2) 0.0180(2) 0.00082(17) 0.00131(17) 0.00077(17) Cu1 0.02335(12) 0.01864(12) 0.01522(11) -0.00086(8) -0.00104(8) 0.00137(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.391(3) . ? C1 C6 1.392(3) . ? C1 N1 1.429(3) . ? C2 C3 1.384(3) . ? C2 H2 0.9500 . ? C3 C4 1.383(3) . ? C3 H3 0.9500 . ? C4 C5 1.384(3) . ? C4 H4 0.9500 . ? C5 C6 1.387(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 N1 1.280(3) . ? C7 C8 1.468(3) . ? C7 H7 0.9500 . ? C8 N2 1.353(2) . ? C8 C12 1.391(3) . ? C9 N2 1.345(2) . ? C9 C10 1.395(3) . ? C9 P1 1.840(2) . ? C10 C11 1.387(3) . ? C10 H10 0.9500 . ? C11 C12 1.384(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.390(3) . ? C13 C14 1.395(3) . ? C13 P1 1.817(2) . ? C14 C15 1.386(3) . ? C14 H14 0.9500 . ? C15 C16 1.381(4) . ? C15 H15 0.9500 . ? C16 C17 1.368(4) . ? C16 H16 0.9500 . ? C17 C18 1.394(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.369(3) . ? C19 C20 1.392(3) . ? C19 P1 1.824(2) . ? C20 C21 1.384(3) . ? C20 H20 0.9500 . ? C21 C22 1.360(5) . ? C21 H21 0.9500 . ? C22 C23 1.370(5) . ? C22 H22 0.9500 . ? C23 C24 1.396(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 O1 1.2592(17) . ? C25 O1 1.2592(17) 2 ? C25 C26 1.507(3) . ? C26 C27 1.392(2) . ? C26 C27 1.392(2) 2 ? C27 C27 1.392(4) 6_556 ? C27 H27 0.9500 . ? C28 C29 1.494(7) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 O2 1.422(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 O2 1.408(6) . ? C30 C31 1.501(8) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 N3 1.152(11) . ? C32 C33 1.441(13) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? B1 F1 1.374(5) . ? B1 F2 1.381(3) . ? B1 F2 1.381(3) 6 ? B1 F3 1.391(6) . ? N1 Cu1 2.1877(17) . ? N2 Cu1 2.0773(16) . ? O1 Cu1 2.0069(14) . ? P1 Cu1 2.1954(6) 2 ? Cu1 P1 2.1954(6) 2 ? Cu1 Cu1 2.8580(6) 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 C2 C1 C6 119.7(2) . . ? C2 C1 N1 115.91(18) . . ? C6 C1 N1 124.37(19) . . ? C3 C2 C1 120.0(2) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 120.4(2) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 119.7(2) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C6 120.5(2) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C1 119.7(2) . . ? C5 C6 H6 120.2 . . ? C1 C6 H6 120.2 . . ? N1 C7 C8 119.32(18) . . ? N1 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? N2 C8 C12 122.50(19) . . ? N2 C8 C7 115.50(17) . . ? C12 C8 C7 122.00(18) . . ? N2 C9 C10 121.75(18) . . ? N2 C9 P1 113.33(14) . . ? C10 C9 P1 124.89(16) . . ? C11 C10 C9 119.3(2) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C12 C11 C10 119.2(2) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C11 C12 C8 118.6(2) . . ? C11 C12 H12 120.7 . . ? C8 C12 H12 120.7 . . ? C18 C13 C14 118.70(19) . . ? C18 C13 P1 123.20(16) . . ? C14 C13 P1 117.64(16) . . ? C15 C14 C13 120.9(2) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C16 C15 C14 119.7(2) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C17 C16 C15 119.9(2) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 121.0(2) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C13 C18 C17 119.7(2) . . ? C13 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C24 C19 C20 119.0(2) . . ? C24 C19 P1 118.45(18) . . ? C20 C19 P1 122.55(17) . . ? C21 C20 C19 120.6(2) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C22 C21 C20 119.9(3) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 120.2(3) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C24 120.4(3) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C19 C24 C23 119.9(3) . . ? C19 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? O1 C25 O1 125.9(2) . 2 ? O1 C25 C26 117.03(12) . . ? O1 C25 C26 117.03(12) 2 . ? C27 C26 C27 119.4(2) . 2 ? C27 C26 C25 120.32(12) . . ? C27 C26 C25 120.32(12) 2 . ? C26 C27 C27 120.32(12) . 6_556 ? C26 C27 H27 119.8 . . ? C27 C27 H27 119.8 6_556 . ? C29 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C29 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O2 C29 C28 109.4(4) . . ? O2 C29 H29A 109.8 . . ? C28 C29 H29A 109.8 . . ? O2 C29 H29B 109.8 . . ? C28 C29 H29B 109.8 . . ? H29A C29 H29B 108.3 . . ? O2 C30 C31 109.0(4) . . ? O2 C30 H30A 109.9 . . ? C31 C30 H30A 109.9 . . ? O2 C30 H30B 109.9 . . ? C31 C30 H30B 109.9 . . ? H30A C30 H30B 108.3 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 C33 179.9(9) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? F1 B1 F2 108.6(2) . . ? F1 B1 F2 108.6(2) . 6 ? F2 B1 F2 117.1(4) . 6 ? F1 B1 F3 109.7(4) . . ? F2 B1 F3 106.3(3) . . ? F2 B1 F3 106.3(3) 6 . ? C7 N1 C1 120.75(17) . . ? C7 N1 Cu1 109.92(13) . . ? C1 N1 Cu1 128.90(13) . . ? C9 N2 C8 118.58(16) . . ? C9 N2 Cu1 126.73(13) . . ? C8 N2 Cu1 112.35(13) . . ? C25 O1 Cu1 122.73(13) . . ? C30 O2 C29 112.7(4) . . ? C13 P1 C19 105.42(10) . . ? C13 P1 C9 102.71(9) . . ? C19 P1 C9 102.27(9) . . ? C13 P1 Cu1 109.95(7) . 2 ? C19 P1 Cu1 117.84(7) . 2 ? C9 P1 Cu1 117.02(7) . 2 ? O1 Cu1 N2 120.74(6) . . ? O1 Cu1 N1 101.20(6) . . ? N2 Cu1 N1 77.82(6) . . ? O1 Cu1 P1 127.16(4) . 2 ? N2 Cu1 P1 108.96(5) . 2 ? N1 Cu1 P1 105.81(5) . 2 ? O1 Cu1 Cu1 79.41(4) . 2 ? N2 Cu1 Cu1 91.34(5) . 2 ? N1 Cu1 Cu1 167.82(5) . 2 ? P1 Cu1 Cu1 82.83(2) 2 2 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 2.7(4) . . . . ? N1 C1 C2 C3 -175.0(2) . . . . ? C1 C2 C3 C4 -0.8(4) . . . . ? C2 C3 C4 C5 -1.0(4) . . . . ? C3 C4 C5 C6 1.0(4) . . . . ? C4 C5 C6 C1 0.9(4) . . . . ? C2 C1 C6 C5 -2.7(3) . . . . ? N1 C1 C6 C5 174.7(2) . . . . ? N1 C7 C8 N2 2.8(3) . . . . ? N1 C7 C8 C12 -177.6(2) . . . . ? N2 C9 C10 C11 -0.3(3) . . . . ? P1 C9 C10 C11 177.52(18) . . . . ? C9 C10 C11 C12 -0.6(4) . . . . ? C10 C11 C12 C8 0.1(4) . . . . ? N2 C8 C12 C11 1.4(3) . . . . ? C7 C8 C12 C11 -178.2(2) . . . . ? C18 C13 C14 C15 -0.7(3) . . . . ? P1 C13 C14 C15 171.72(18) . . . . ? C13 C14 C15 C16 0.8(4) . . . . ? C14 C15 C16 C17 0.5(4) . . . . ? C15 C16 C17 C18 -1.7(4) . . . . ? C14 C13 C18 C17 -0.5(4) . . . . ? P1 C13 C18 C17 -172.5(2) . . . . ? C16 C17 C18 C13 1.8(4) . . . . ? C24 C19 C20 C21 -0.8(4) . . . . ? P1 C19 C20 C21 179.25(19) . . . . ? C19 C20 C21 C22 -0.2(4) . . . . ? C20 C21 C22 C23 0.7(6) . . . . ? C21 C22 C23 C24 -0.3(7) . . . . ? C20 C19 C24 C23 1.2(5) . . . . ? P1 C19 C24 C23 -178.8(3) . . . . ? C22 C23 C24 C19 -0.7(7) . . . . ? O1 C25 C26 C27 -175.74(13) . . . . ? O1 C25 C26 C27 4.26(13) 2 . . . ? O1 C25 C26 C27 4.26(13) . . . 2 ? O1 C25 C26 C27 -175.74(13) 2 . . 2 ? C27 C26 C27 C27 0.0 2 . . 6_556 ? C25 C26 C27 C27 180.0 . . . 6_556 ? C8 C7 N1 C1 -173.10(18) . . . . ? C8 C7 N1 Cu1 13.7(2) . . . . ? C2 C1 N1 C7 154.8(2) . . . . ? C6 C1 N1 C7 -22.7(3) . . . . ? C2 C1 N1 Cu1 -33.4(3) . . . . ? C6 C1 N1 Cu1 149.05(17) . . . . ? C10 C9 N2 C8 1.7(3) . . . . ? P1 C9 N2 C8 -176.33(14) . . . . ? C10 C9 N2 Cu1 -159.49(16) . . . . ? P1 C9 N2 Cu1 22.4(2) . . . . ? C12 C8 N2 C9 -2.3(3) . . . . ? C7 C8 N2 C9 177.29(17) . . . . ? C12 C8 N2 Cu1 161.51(17) . . . . ? C7 C8 N2 Cu1 -18.9(2) . . . . ? O1 C25 O1 Cu1 -16.03(7) 2 . . . ? C26 C25 O1 Cu1 163.97(7) . . . . ? C31 C30 O2 C29 180.0 . . . . ? C28 C29 O2 C30 180.0 . . . . ? C18 C13 P1 C19 -18.0(2) . . . . ? C14 C13 P1 C19 169.92(16) . . . . ? C18 C13 P1 C9 -124.74(19) . . . . ? C14 C13 P1 C9 63.16(18) . . . . ? C18 C13 P1 Cu1 110.00(18) . . . 2 ? C14 C13 P1 Cu1 -62.10(17) . . . 2 ? C24 C19 P1 C13 121.2(2) . . . . ? C20 C19 P1 C13 -58.9(2) . . . . ? C24 C19 P1 C9 -131.8(2) . . . . ? C20 C19 P1 C9 48.2(2) . . . . ? C24 C19 P1 Cu1 -1.9(3) . . . 2 ? C20 C19 P1 Cu1 178.03(16) . . . 2 ? N2 C9 P1 C13 -155.76(14) . . . . ? C10 C9 P1 C13 26.2(2) . . . . ? N2 C9 P1 C19 95.08(15) . . . . ? C10 C9 P1 C19 -82.91(19) . . . . ? N2 C9 P1 Cu1 -35.26(16) . . . 2 ? C10 C9 P1 Cu1 146.74(16) . . . 2 ? C25 O1 Cu1 N2 111.30(12) . . . . ? C25 O1 Cu1 N1 -166.31(12) . . . . ? C25 O1 Cu1 P1 -46.41(14) . . . 2 ? C25 O1 Cu1 Cu1 26.08(11) . . . 2 ? C9 N2 Cu1 O1 -82.34(17) . . . . ? C8 N2 Cu1 O1 115.46(13) . . . . ? C9 N2 Cu1 N1 -178.24(17) . . . . ? C8 N2 Cu1 N1 19.55(13) . . . . ? C9 N2 Cu1 P1 79.02(16) . . . 2 ? C8 N2 Cu1 P1 -83.19(13) . . . 2 ? C9 N2 Cu1 Cu1 -3.87(16) . . . 2 ? C8 N2 Cu1 Cu1 -166.07(13) . . . 2 ? C7 N1 Cu1 O1 -137.26(14) . . . . ? C1 N1 Cu1 O1 50.26(17) . . . . ? C7 N1 Cu1 N2 -17.89(14) . . . . ? C1 N1 Cu1 N2 169.62(17) . . . . ? C7 N1 Cu1 P1 88.63(14) . . . 2 ? C1 N1 Cu1 P1 -83.86(16) . . . 2 ? C7 N1 Cu1 Cu1 -45.6(3) . . . 2 ? C1 N1 Cu1 Cu1 141.95(17) . . . 2 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.870 _refine_diff_density_min -0.731 _refine_diff_density_rms 0.063 data_squeezed _database_code_depnum_ccdc_archive 'CCDC 815067' #TrackingRef '- combined.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C116 H100 Cu4 N8 O12 P4, 4(C2 H3 N), 2(B F4)' _chemical_formula_sum ' C124 H112 B2 Cu4 F8 N12 O12 P4 ' _chemical_formula_weight 2513.92 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 _symmetry_space_group_name_Hall '-P 1' _symmetry_Inl_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.583(2) _cell_length_b 16.843(3) _cell_length_c 19.661(4) _cell_angle_alpha 66.03(3) _cell_angle_beta 78.91(3) _cell_angle_gamma 88.69(3) _cell_volume 3433.1(14) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 101124 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 28.28 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.216 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1294 _exptl_absorpt_coefficient_mu 0.725 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.698 _exptl_absorpt_correction_T_max 0.935 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.026 0.000 1.000 390 50 ' ' 2 0.349 0.209 0.390 9 1 ' ' 3 0.650 0.791 0.610 9 1 ' ' _platon_squeeze_details ; ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 61240 _diffrn_reflns_av_R_equivalents 0.0748 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.66 _diffrn_reflns_theta_max 25.03 _reflns_number_total 12082 _reflns_number_gt 8932 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-97 (Altomare et al. 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_molecular_graphics ;ORTEP-3 (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material 'enCIFer 1.1 (CCDC, 2005)' _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^)+(0.1399P)^2^+5.7730P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12082 _refine_ls_number_parameters 727 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.1050 _refine_ls_R_factor_gt 0.0812 _refine_ls_wR_factor_ref 0.2437 _refine_ls_wR_factor_gt 0.2255 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.065 _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 C1 C 0.8720(5) 0.3339(4) 0.1738(3) 0.0457(13) Uani 1 1 d . . . C2 C 0.8066(7) 0.2598(5) 0.1859(4) 0.0663(18) Uani 1 1 d . . . H2 H 0.7860 0.2150 0.2357 0.080 Uiso 1 1 calc R . . C3 C 0.7709(7) 0.2506(7) 0.1259(5) 0.086(2) Uani 1 1 d . . . H3 H 0.7286 0.1986 0.1346 0.103 Uiso 1 1 calc R . . C4 C 0.7960(8) 0.3150(7) 0.0552(5) 0.086(2) Uani 1 1 d . . . H4 H 0.7678 0.3093 0.0150 0.103 Uiso 1 1 calc R . . C5 C 0.8606(8) 0.3869(6) 0.0415(4) 0.083(2) Uani 1 1 d . . . H5 H 0.8787 0.4315 -0.0085 0.100 Uiso 1 1 calc R . . C6 C 0.9014(7) 0.3967(5) 0.1002(4) 0.0691(19) Uani 1 1 d . . . H6 H 0.9497 0.4468 0.0894 0.083 Uiso 1 1 calc R . . C7 C 0.9885(5) 0.4496(4) 0.2181(3) 0.0421(12) Uani 1 1 d . . . C8 C 0.9174(5) 0.5175(4) 0.2144(3) 0.0484(13) Uani 1 1 d . . . H8 H 0.8346 0.5060 0.2316 0.058 Uiso 1 1 calc R . . C9 C 0.9653(6) 0.6026(4) 0.1861(3) 0.0548(15) Uani 1 1 d . . . H9 H 0.9152 0.6485 0.1846 0.066 Uiso 1 1 calc R . . C10 C 1.0838(6) 0.6202(4) 0.1604(3) 0.0548(16) Uani 1 1 d . . . H10 H 1.1168 0.6783 0.1398 0.066 Uiso 1 1 calc R . . C11 C 1.1553(6) 0.5521(4) 0.1648(3) 0.0546(15) Uani 1 1 d . . . H11 H 1.2380 0.5639 0.1475 0.066 Uiso 1 1 calc R . . C12 C 1.1088(5) 0.4671(4) 0.1939(3) 0.0497(14) Uani 1 1 d . . . H12 H 1.1594 0.4210 0.1973 0.060 Uiso 1 1 calc R . . C13 C 1.0291(5) 0.2640(3) 0.2749(3) 0.0413(12) Uani 1 1 d . . . C14 C 1.1123(5) 0.1553(4) 0.3644(3) 0.0450(13) Uani 1 1 d . . . C15 C 1.2007(6) 0.1488(4) 0.3092(4) 0.0574(15) Uani 1 1 d . . . H15 H 1.2611 0.1097 0.3229 0.069 Uiso 1 1 calc R . . C16 C 1.2003(5) 0.2006(4) 0.2327(4) 0.0543(15) Uani 1 1 d . . . H16 H 1.2581 0.1955 0.1935 0.065 Uiso 1 1 calc R . . C17 C 1.1140(5) 0.2592(4) 0.2156(3) 0.0502(14) Uani 1 1 d . . . H17 H 1.1122 0.2959 0.1643 0.060 Uiso 1 1 calc R . . C18 C 1.1063(5) 0.1004(4) 0.4454(3) 0.0486(14) Uani 1 1 d . . . H18 H 1.1614 0.0573 0.4610 0.058 Uiso 1 1 calc R . . C19 C 1.0179(6) 0.0636(4) 0.5736(3) 0.0527(15) Uani 1 1 d . . . C20 C 0.9123(7) 0.0699(4) 0.6206(3) 0.0612(17) Uani 1 1 d . . . H20 H 0.8522 0.1030 0.5973 0.073 Uiso 1 1 calc R . . C21 C 0.8929(8) 0.0300(4) 0.6991(4) 0.071(2) Uani 1 1 d . . . H21 H 0.8211 0.0366 0.7285 0.085 Uiso 1 1 calc R . . C22 C 0.9762(9) -0.0187(5) 0.7341(4) 0.075(2) Uani 1 1 d . . . C23 C 1.0811(10) -0.0275(5) 0.6893(5) 0.093(3) Uani 1 1 d . . . H23 H 1.1395 -0.0617 0.7137 0.112 Uiso 1 1 calc R . . C24 C 1.1036(8) 0.0135(5) 0.6077(4) 0.073(2) Uani 1 1 d . . . H24 H 1.1750 0.0063 0.5782 0.087 Uiso 1 1 calc R . . C25 C 0.152(2) 0.0368(16) 0.1452(13) 0.0984(17) Uani 0.50 1 d P A 1 H25A H 0.2245 0.0570 0.1547 0.118 Uiso 0.50 1 calc PR A 1 H25B H 0.1517 -0.0272 0.1624 0.118 Uiso 0.50 1 calc PR A 1 C26 C 0.150(2) 0.0793(12) 0.0617(10) 0.0984(17) Uani 0.50 1 d P A 1 H26A H 0.0713 0.0701 0.0521 0.118 Uiso 0.50 1 calc PR A 1 H26B H 0.2103 0.0571 0.0320 0.118 Uiso 0.50 1 calc PR A 1 C27A C 0.091(3) 0.2444(13) 0.0100(10) 0.0984(17) Uani 0.50 1 d P B 2 H27A H 0.0393 0.2445 -0.0244 0.118 Uiso 0.50 1 calc PR B 2 H27B H 0.0401 0.2374 0.0589 0.118 Uiso 0.50 1 calc PR B 2 C28 C 0.1512(10) 0.3230(7) -0.0202(4) 0.109(4) Uani 1 1 d . . . H28A H 0.2085 0.3222 -0.0643 0.130 Uiso 1 1 calc R B 1 H28B H 0.0911 0.3647 -0.0388 0.130 Uiso 1 1 calc R B 1 C29 C 0.2945(6) 0.4128(5) -0.0126(4) 0.069(2) Uani 1 1 d . . . H29A H 0.2613 0.4616 -0.0506 0.083 Uiso 1 1 calc R B 1 H29B H 0.3611 0.3927 -0.0402 0.083 Uiso 1 1 calc R B 1 C30 C 0.3383(7) 0.4436(5) 0.0392(4) 0.0685(19) Uani 1 1 d . B . H30A H 0.3969 0.4935 0.0097 0.082 Uiso 1 1 calc R C 1 H30B H 0.2722 0.4626 0.0681 0.082 Uiso 1 1 calc R C 1 C31 C 0.4437(5) 0.3865(4) 0.1427(3) 0.0523(14) Uani 1 1 d . . . C32 C 0.4593(5) 0.4657(4) 0.1444(3) 0.0498(14) Uani 1 1 d . . . H32 H 0.4301 0.5158 0.1095 0.060 Uiso 1 1 calc R . . C33 C 0.5180(5) 0.4731(4) 0.1975(3) 0.0497(14) Uani 1 1 d . . . H33 H 0.5313 0.5285 0.1975 0.060 Uiso 1 1 calc R B . C34 C 0.5573(5) 0.3986(4) 0.2508(3) 0.0473(13) Uani 1 1 d . . . C35 C 0.5413(6) 0.3197(4) 0.2467(4) 0.0555(15) Uani 1 1 d . . . H35 H 0.5704 0.2692 0.2812 0.067 Uiso 1 1 calc R B . C36 C 0.4848(7) 0.3124(5) 0.1945(4) 0.0670(19) Uani 1 1 d . . . H36 H 0.4736 0.2572 0.1933 0.080 Uiso 1 1 calc R . . C37 C 0.5926(5) 0.4543(4) 0.3364(3) 0.0483(14) Uani 1 1 d . B . H37 H 0.5320 0.4931 0.3225 0.058 Uiso 1 1 calc R . . C38 C 0.6576(5) 0.4566(4) 0.3927(3) 0.0444(12) Uani 1 1 d . B . C39 C 0.8037(5) 0.3971(4) 0.4601(3) 0.0424(12) Uani 1 1 d . . . C40 C 0.7827(5) 0.4527(4) 0.4973(3) 0.0523(14) Uani 1 1 d . . . H40 H 0.8279 0.4503 0.5336 0.063 Uiso 1 1 calc R . . C41 C 0.6969(6) 0.5109(5) 0.4812(4) 0.0617(17) Uani 1 1 d . . . H41 H 0.6808 0.5487 0.5064 0.074 Uiso 1 1 calc R . . C42 C 0.6340(5) 0.5132(5) 0.4271(4) 0.0579(16) Uani 1 1 d . . . H42 H 0.5751 0.5537 0.4140 0.070 Uiso 1 1 calc R . . C43 C 1.0527(5) 0.3902(3) 0.4164(3) 0.0409(12) Uani 1 1 d . . . C44 C 1.0553(5) 0.4819(4) 0.3819(3) 0.0452(13) Uani 1 1 d . . . H44 H 0.9856 0.5110 0.3884 0.054 Uiso 1 1 calc R . . C45 C 1.1593(6) 0.5293(4) 0.3384(3) 0.0525(14) Uani 1 1 d . . . H45 H 1.1606 0.5911 0.3154 0.063 Uiso 1 1 calc R . . C46 C 1.2599(6) 0.4884(4) 0.3283(4) 0.0606(16) Uani 1 1 d . . . H46 H 1.3304 0.5220 0.2979 0.073 Uiso 1 1 calc R . . C47 C 1.2608(6) 0.3975(5) 0.3623(4) 0.0651(18) Uani 1 1 d . . . H47 H 1.3315 0.3690 0.3568 0.078 Uiso 1 1 calc R . . C48 C 1.1549(5) 0.3500(4) 0.4043(4) 0.0557(15) Uani 1 1 d . . . H48 H 1.1531 0.2882 0.4252 0.067 Uiso 1 1 calc R . . C49 C 0.9349(7) 0.2962(4) 0.5714(3) 0.0574(16) Uani 1 1 d . . . C50 C 1.0385(8) 0.3114(5) 0.5902(4) 0.075(2) Uani 1 1 d . . . H50 H 1.1066 0.3383 0.5521 0.090 Uiso 1 1 calc R . . C51 C 1.0396(14) 0.2851(8) 0.6695(7) 0.118(4) Uani 1 1 d . . . H51 H 1.1088 0.2972 0.6837 0.142 Uiso 1 1 calc R . . C52 C 0.9453(16) 0.2439(7) 0.7236(6) 0.117(5) Uani 1 1 d . . . H52 H 0.9502 0.2235 0.7756 0.140 Uiso 1 1 calc R . . C53 C 0.8448(13) 0.2316(5) 0.7049(5) 0.106(4) Uani 1 1 d . . . H53 H 0.7778 0.2050 0.7441 0.127 Uiso 1 1 calc R . . C54 C 0.8347(9) 0.2571(5) 0.6279(4) 0.078(2) Uani 1 1 d . . . H54 H 0.7625 0.2478 0.6153 0.094 Uiso 1 1 calc R . . C55 C 0.6819(5) 0.1392(3) 0.4453(3) 0.0419(12) Uani 1 1 d . . . C56 C 0.5880(5) 0.0666(3) 0.4735(3) 0.0416(12) Uani 1 1 d . . . C57 C 0.5130(6) 0.0643(4) 0.4274(3) 0.0569(16) Uani 1 1 d . . . H57 H 0.5222 0.1081 0.3772 0.068 Uiso 1 1 calc R . . C58 C 0.5760(5) 0.0014(4) 0.5460(3) 0.0498(14) Uani 1 1 d . . . H58 H 0.6285 0.0016 0.5776 0.060 Uiso 1 1 calc R . . N1 N 1.0281(4) 0.2127(3) 0.3476(2) 0.0383(10) Uani 1 1 d . . . N2 N 1.0261(4) 0.1115(3) 0.4944(3) 0.0438(11) Uani 1 1 d . . . N3 N 0.6169(4) 0.4007(3) 0.3063(3) 0.0453(11) Uani 1 1 d . . . N4 N 0.7410(4) 0.3983(3) 0.4086(2) 0.0387(10) Uani 1 1 d . . . O1 O 0.044(2) 0.061(2) 0.1890(18) 0.0984(17) Uani 0.50 1 d PD . 1 O2 O 0.1791(18) 0.1811(10) 0.0416(7) 0.0984(17) Uani 0.50 1 d P A 1 O3 O 0.2082(5) 0.3448(4) 0.0275(3) 0.0947(19) Uani 1 1 d . B 1 O4 O 0.3914(5) 0.3723(3) 0.0898(3) 0.0737(14) Uani 1 1 d . B 1 O1A O 0.0189(19) 0.059(2) 0.1923(18) 0.0984(17) Uani 0.50 1 d PD . 2 O2A O 0.1659(17) 0.1654(10) 0.0244(7) 0.0984(17) Uani 0.50 1 d P B 2 C25A C 0.109(2) 0.0460(16) 0.1406(13) 0.0984(17) Uani 0.50 1 d P B 2 H25C H 0.1068 -0.0161 0.1491 0.118 Uiso 0.50 1 calc PR B 2 H25D H 0.1863 0.0614 0.1478 0.118 Uiso 0.50 1 calc PR B 2 C26A C 0.093(2) 0.1007(13) 0.0629(11) 0.0984(17) Uani 0.50 1 d P B 2 H26C H 0.0973 0.0633 0.0347 0.118 Uiso 0.50 1 calc PR B 2 H26D H 0.0132 0.1222 0.0662 0.118 Uiso 0.50 1 calc PR B 2 C27 C 0.087(3) 0.2205(13) 0.0373(10) 0.0984(17) Uani 0.50 1 d P A 1 H27C H 0.0439 0.2165 0.0874 0.118 Uiso 0.50 1 calc PR A 1 H27D H 0.0332 0.2005 0.0129 0.118 Uiso 0.50 1 calc PR A 1 O5 O 0.6622(4) 0.2095(3) 0.3946(2) 0.0565(11) Uani 1 1 d . . . O6 O 0.7705(3) 0.1247(2) 0.4749(2) 0.0491(10) Uani 1 1 d . . . B1 B 1.4947(11) 0.0115(7) 0.2349(6) 0.255(5) Uani 1 1 d D . . F2 F 1.517(2) 0.0012(14) 0.1681(9) 0.255(5) Uani 0.50 1 d PD D 1 F1 F 1.4412(18) 0.0882(10) 0.2268(12) 0.255(5) Uani 0.50 1 d PD D 1 F3 F 1.6002(15) 0.0133(16) 0.2587(13) 0.255(5) Uani 0.50 1 d PD D 1 F4 F 1.421(2) -0.0574(11) 0.2913(11) 0.255(5) Uani 0.50 1 d PD D 1 F7 F 1.5924(16) 0.0439(14) 0.1755(10) 0.255(5) Uani 0.50 1 d PD D 2 F5 F 1.4572(18) 0.0756(11) 0.2587(12) 0.255(5) Uani 0.50 1 d PD D 2 F6 F 1.4054(17) -0.0124(15) 0.2069(13) 0.255(5) Uani 0.50 1 d PD D 2 F8 F 1.524(2) -0.0602(12) 0.2929(9) 0.255(5) Uani 0.50 1 d PD D 2 C60 C 0.5355(11) 0.2644(9) -0.0298(11) 0.066(4) Uani 0.50 1 d P . . N5 N 0.5839(11) 0.3120(9) -0.0810(11) 0.096(5) Uani 0.50 1 d P . . C59 C 0.4598(17) 0.2004(11) 0.0416(10) 0.088(5) Uani 0.50 1 d P . . H59A H 0.3943 0.2300 0.0589 0.132 Uiso 0.50 1 calc PR . . H59B H 0.5070 0.1760 0.0809 0.132 Uiso 0.50 1 calc PR . . H59C H 0.4286 0.1535 0.0316 0.132 Uiso 0.50 1 calc PR . . C61 C 0.5748(19) 0.7487(15) 0.4486(12) 0.040(5) Uiso 0.25 1 d P . . N6 N 0.531(3) 0.704(2) 0.4507(17) 0.087(8) Uiso 0.25 1 d P . . C62 C 0.640(4) 0.817(3) 0.450(2) 0.099(11) Uiso 0.25 1 d P . . H62A H 0.7230 0.8155 0.4281 0.148 Uiso 0.25 1 calc PR . . H62B H 0.6325 0.8097 0.5027 0.148 Uiso 0.25 1 calc PR . . H62C H 0.6098 0.8724 0.4205 0.148 Uiso 0.25 1 calc PR . . N7 N 0.672(2) 0.6571(15) 0.2274(13) 0.064(6) Uiso 0.25 1 d P . . C63 C 0.600(3) 0.700(2) 0.230(2) 0.086(9) Uiso 0.25 1 d P . . C64 C 0.473(3) 0.716(3) 0.256(2) 0.100(11) Uiso 0.25 1 d P . . H64A H 0.4206 0.6932 0.2339 0.150 Uiso 0.25 1 calc PR . . H64B H 0.4640 0.7788 0.2407 0.150 Uiso 0.25 1 calc PR . . H64C H 0.4513 0.6866 0.3120 0.150 Uiso 0.25 1 calc PR . . P1 P 0.91216(12) 0.34159(9) 0.25632(7) 0.0378(3) Uani 1 1 d . . . P2 P 0.92148(12) 0.32056(9) 0.47368(8) 0.0397(3) Uani 1 1 d . . . Cu1 Cu 0.76065(5) 0.32198(4) 0.34724(3) 0.0391(2) Uani 1 1 d D B . Cu2 Cu 0.90985(5) 0.20929(4) 0.44517(3) 0.0384(2) Uani 1 1 d D B . 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 C1 0.045(3) 0.049(3) 0.045(3) -0.018(3) -0.017(2) 0.005(3) C2 0.078(5) 0.066(4) 0.058(4) -0.024(3) -0.020(3) -0.014(4) C3 0.075(5) 0.115(7) 0.091(6) -0.061(6) -0.026(4) -0.013(5) C4 0.091(6) 0.120(7) 0.066(5) -0.051(5) -0.030(4) 0.001(5) C5 0.111(7) 0.086(6) 0.057(4) -0.025(4) -0.036(4) 0.008(5) C6 0.089(5) 0.067(4) 0.047(3) -0.013(3) -0.027(3) -0.002(4) C7 0.051(3) 0.043(3) 0.028(2) -0.010(2) -0.008(2) -0.008(2) C8 0.051(3) 0.042(3) 0.044(3) -0.008(2) -0.010(3) -0.005(3) C9 0.070(4) 0.040(3) 0.050(3) -0.011(3) -0.020(3) 0.006(3) C10 0.078(4) 0.041(3) 0.042(3) -0.012(3) -0.012(3) -0.018(3) C11 0.052(3) 0.057(4) 0.049(3) -0.017(3) -0.005(3) -0.014(3) C12 0.047(3) 0.056(3) 0.047(3) -0.022(3) -0.010(3) -0.002(3) C13 0.040(3) 0.039(3) 0.046(3) -0.017(2) -0.013(2) -0.004(2) C14 0.048(3) 0.041(3) 0.047(3) -0.017(2) -0.013(3) 0.003(2) C15 0.059(4) 0.051(4) 0.065(4) -0.023(3) -0.020(3) 0.015(3) C16 0.048(3) 0.057(4) 0.054(3) -0.023(3) 0.000(3) 0.005(3) C17 0.059(4) 0.050(3) 0.044(3) -0.022(3) -0.009(3) 0.001(3) C18 0.054(3) 0.042(3) 0.055(3) -0.019(3) -0.029(3) 0.011(3) C19 0.081(4) 0.036(3) 0.048(3) -0.015(3) -0.034(3) 0.011(3) C20 0.087(5) 0.046(3) 0.044(3) -0.009(3) -0.020(3) 0.001(3) C21 0.110(6) 0.052(4) 0.046(3) -0.014(3) -0.018(4) -0.001(4) C22 0.134(7) 0.050(4) 0.050(4) -0.021(3) -0.038(5) 0.016(4) C23 0.153(9) 0.063(5) 0.074(5) -0.017(4) -0.075(6) 0.038(5) C24 0.104(6) 0.060(4) 0.063(4) -0.024(3) -0.041(4) 0.025(4) C25 0.158(5) 0.078(3) 0.060(2) -0.0192(19) -0.043(4) 0.014(3) C26 0.158(5) 0.078(3) 0.060(2) -0.0192(19) -0.043(4) 0.014(3) C27A 0.158(5) 0.078(3) 0.060(2) -0.0192(19) -0.043(4) 0.014(3) C28 0.131(8) 0.124(8) 0.051(4) 0.000(5) -0.047(5) -0.043(6) C29 0.059(4) 0.093(5) 0.043(3) -0.012(3) -0.016(3) -0.003(4) C30 0.071(4) 0.082(5) 0.047(3) -0.015(3) -0.025(3) 0.005(4) C31 0.047(3) 0.064(4) 0.042(3) -0.014(3) -0.015(3) 0.001(3) C32 0.044(3) 0.056(4) 0.040(3) -0.010(3) -0.010(2) 0.005(3) C33 0.041(3) 0.050(3) 0.049(3) -0.012(3) -0.009(2) 0.002(3) C34 0.032(3) 0.060(4) 0.040(3) -0.009(3) -0.008(2) -0.006(2) C35 0.059(4) 0.048(3) 0.055(3) -0.010(3) -0.028(3) -0.003(3) C36 0.078(5) 0.053(4) 0.068(4) -0.014(3) -0.036(4) -0.004(3) C37 0.038(3) 0.057(4) 0.044(3) -0.016(3) -0.007(2) 0.008(3) C38 0.038(3) 0.049(3) 0.046(3) -0.021(3) -0.005(2) 0.000(2) C39 0.041(3) 0.044(3) 0.039(3) -0.014(2) -0.006(2) -0.008(2) C40 0.054(3) 0.060(4) 0.052(3) -0.030(3) -0.016(3) 0.008(3) C41 0.058(4) 0.069(4) 0.070(4) -0.041(4) -0.008(3) 0.001(3) C42 0.042(3) 0.066(4) 0.069(4) -0.031(3) -0.015(3) 0.010(3) C43 0.041(3) 0.042(3) 0.042(3) -0.015(2) -0.017(2) -0.007(2) C44 0.051(3) 0.046(3) 0.044(3) -0.022(3) -0.013(2) -0.001(3) C45 0.060(4) 0.047(3) 0.049(3) -0.016(3) -0.014(3) -0.009(3) C46 0.048(4) 0.063(4) 0.066(4) -0.025(3) -0.003(3) -0.016(3) C47 0.045(3) 0.061(4) 0.093(5) -0.037(4) -0.010(3) 0.002(3) C48 0.046(3) 0.046(3) 0.081(4) -0.029(3) -0.020(3) 0.003(3) C49 0.098(5) 0.036(3) 0.041(3) -0.012(3) -0.029(3) 0.009(3) C50 0.108(6) 0.072(5) 0.070(4) -0.039(4) -0.057(4) 0.035(4) C51 0.196(13) 0.108(8) 0.108(8) -0.071(7) -0.108(9) 0.073(9) C52 0.230(15) 0.081(7) 0.055(5) -0.032(5) -0.059(8) 0.057(8) C53 0.206(13) 0.056(5) 0.045(4) -0.017(4) -0.008(6) 0.010(6) C54 0.123(7) 0.058(4) 0.047(4) -0.018(3) -0.009(4) -0.005(4) C55 0.042(3) 0.038(3) 0.037(3) -0.006(2) -0.008(2) -0.012(2) C56 0.040(3) 0.036(3) 0.042(3) -0.006(2) -0.013(2) -0.006(2) C57 0.060(4) 0.052(3) 0.038(3) 0.007(3) -0.019(3) -0.024(3) C58 0.047(3) 0.048(3) 0.046(3) -0.004(3) -0.019(3) -0.013(3) N1 0.040(2) 0.035(2) 0.039(2) -0.0118(18) -0.0106(18) -0.0023(19) N2 0.054(3) 0.033(2) 0.044(2) -0.011(2) -0.020(2) -0.001(2) N3 0.035(2) 0.048(3) 0.043(2) -0.009(2) -0.0085(19) -0.003(2) N4 0.036(2) 0.037(2) 0.039(2) -0.0117(19) -0.0077(18) -0.0014(19) O1 0.158(5) 0.078(3) 0.060(2) -0.0192(19) -0.043(4) 0.014(3) O2 0.158(5) 0.078(3) 0.060(2) -0.0192(19) -0.043(4) 0.014(3) O3 0.085(4) 0.131(5) 0.050(3) -0.015(3) -0.017(3) -0.041(4) O4 0.083(3) 0.079(3) 0.065(3) -0.020(2) -0.047(3) 0.009(3) O1A 0.158(5) 0.078(3) 0.060(2) -0.0192(19) -0.043(4) 0.014(3) O2A 0.158(5) 0.078(3) 0.060(2) -0.0192(19) -0.043(4) 0.014(3) C25A 0.158(5) 0.078(3) 0.060(2) -0.0192(19) -0.043(4) 0.014(3) C26A 0.158(5) 0.078(3) 0.060(2) -0.0192(19) -0.043(4) 0.014(3) C27 0.158(5) 0.078(3) 0.060(2) -0.0192(19) -0.043(4) 0.014(3) O5 0.057(2) 0.042(2) 0.056(2) 0.0007(19) -0.023(2) -0.0182(19) O6 0.047(2) 0.041(2) 0.052(2) -0.0063(17) -0.0192(18) -0.0122(17) B1 0.233(10) 0.299(11) 0.208(8) -0.092(8) -0.020(8) 0.087(9) F2 0.233(10) 0.299(11) 0.208(8) -0.092(8) -0.020(8) 0.087(9) F1 0.233(10) 0.299(11) 0.208(8) -0.092(8) -0.020(8) 0.087(9) F3 0.233(10) 0.299(11) 0.208(8) -0.092(8) -0.020(8) 0.087(9) F4 0.233(10) 0.299(11) 0.208(8) -0.092(8) -0.020(8) 0.087(9) F7 0.233(10) 0.299(11) 0.208(8) -0.092(8) -0.020(8) 0.087(9) F5 0.233(10) 0.299(11) 0.208(8) -0.092(8) -0.020(8) 0.087(9) F6 0.233(10) 0.299(11) 0.208(8) -0.092(8) -0.020(8) 0.087(9) F8 0.233(10) 0.299(11) 0.208(8) -0.092(8) -0.020(8) 0.087(9) C60 0.039(7) 0.034(7) 0.137(14) -0.044(8) -0.027(8) 0.008(6) N5 0.053(7) 0.046(7) 0.164(15) -0.040(8) 0.026(8) -0.016(6) C59 0.102(13) 0.067(10) 0.083(11) -0.016(8) -0.025(10) 0.031(9) P1 0.0411(7) 0.0352(7) 0.0330(6) -0.0084(5) -0.0097(5) -0.0031(6) P2 0.0440(8) 0.0382(7) 0.0384(7) -0.0142(6) -0.0148(6) -0.0015(6) Cu1 0.0390(4) 0.0357(4) 0.0375(3) -0.0091(3) -0.0088(3) -0.0047(3) Cu2 0.0407(4) 0.0346(4) 0.0379(3) -0.0105(3) -0.0124(3) -0.0054(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 C1 C6 1.382(9) . ? C1 C2 1.386(9) . ? C1 P1 1.825(6) . ? C2 C3 1.388(10) . ? C2 H2 0.9500 . ? C3 C4 1.352(12) . ? C3 H3 0.9500 . ? C4 C5 1.340(12) . ? C4 H4 0.9500 . ? C5 C6 1.396(10) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.379(8) . ? C7 C8 1.380(8) . ? C7 P1 1.833(5) . ? C8 C9 1.393(8) . ? C8 H8 0.9500 . ? C9 C10 1.363(9) . ? C9 H9 0.9500 . ? C10 C11 1.382(10) . ? C10 H10 0.9500 . ? C11 C12 1.386(8) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 N1 1.335(7) . ? C13 C17 1.401(8) . ? C13 P1 1.843(6) . ? C14 N1 1.347(7) . ? C14 C15 1.379(9) . ? C14 C18 1.471(8) . ? C15 C16 1.401(9) . ? C15 H15 0.9500 . ? C16 C17 1.378(9) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 N2 1.274(8) . ? C18 H18 0.9500 . ? C19 C24 1.381(9) . ? C19 C20 1.415(10) . ? C19 N2 1.417(7) . ? C20 C21 1.383(9) . ? C20 H20 0.9500 . ? C21 C22 1.356(11) . ? C21 H21 0.9500 . ? C22 O1A 1.34(3) 2_656 ? C22 O1 1.36(3) 2_656 ? C22 C23 1.399(13) . ? C23 C24 1.438(11) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.51(3) . ? C25 O1 1.53(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O2 1.62(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27A C28 1.35(2) . ? C27A O2A 1.53(3) . ? C27A H27A 0.9900 . ? C27A H27B 0.9900 . ? C28 O3 1.407(9) . ? C28 C27 1.72(2) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O3 1.395(9) . ? C29 C30 1.484(10) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 O4 1.430(8) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.365(9) . ? C31 C36 1.396(9) . ? C31 O4 1.399(7) . ? C32 C33 1.396(8) . ? C32 H32 0.9500 . ? C33 C34 1.403(8) . ? C33 H33 0.9500 . ? C34 C35 1.383(9) . ? C34 N3 1.410(7) . ? C35 C36 1.365(9) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 N3 1.267(8) . ? C37 C38 1.467(8) . ? C37 H37 0.9500 . ? C38 N4 1.348(7) . ? C38 C42 1.372(9) . ? C39 N4 1.350(7) . ? C39 C40 1.396(8) . ? C39 P2 1.837(6) . ? C40 C41 1.368(9) . ? C40 H40 0.9500 . ? C41 C42 1.387(9) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C48 1.380(8) . ? C43 C44 1.409(8) . ? C43 P2 1.818(5) . ? C44 C45 1.383(8) . ? C44 H44 0.9500 . ? C45 C46 1.364(9) . ? C45 H45 0.9500 . ? C46 C47 1.401(10) . ? C46 H46 0.9500 . ? C47 C48 1.395(9) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C50 1.379(10) . ? C49 C54 1.399(11) . ? C49 P2 1.833(6) . ? C50 C51 1.440(13) . ? C50 H50 0.9500 . ? C51 C52 1.340(18) . ? C51 H51 0.9500 . ? C52 C53 1.331(17) . ? C52 H52 0.9500 . ? C53 C54 1.424(12) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 O6 1.246(6) . ? C55 O5 1.251(6) . ? C55 C56 1.504(7) . ? C56 C57 1.381(8) . ? C56 C58 1.385(7) . ? C57 C58 1.392(8) 2_656 ? C57 H57 0.9500 . ? C58 C57 1.392(8) 2_656 ? C58 H58 0.9500 . ? N1 Cu2 2.113(4) . ? N2 Cu2 2.137(5) . ? N3 Cu1 2.174(5) . ? N4 Cu1 2.073(4) . ? O1 C22 1.36(3) 2_656 ? O2 C27 1.25(3) . ? O1A C22 1.34(3) 2_656 ? O1A C25A 1.39(4) . ? O2A C26A 1.26(3) . ? C25A C26A 1.47(3) . ? C25A H25C 0.9900 . ? C25A H25D 0.9900 . ? C26A H26C 0.9900 . ? C26A H26D 0.9900 . ? C27 H27C 0.9900 . ? C27 H27D 0.9900 . ? O5 Cu1 2.003(4) . ? O6 Cu2 2.011(4) . ? B1 F2 1.369(10) . ? B1 F8 1.371(10) . ? B1 F5 1.373(10) . ? B1 F1 1.383(10) . ? B1 F4 1.391(10) . ? B1 F7 1.394(10) . ? B1 F3 1.395(10) . ? B1 F6 1.398(10) . ? C60 N5 1.06(2) . ? C60 C59 1.50(2) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C61 N6 0.90(3) . ? C61 C62 1.40(4) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? N7 C63 1.10(4) . ? C63 C64 1.53(5) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? P1 Cu1 2.1736(17) . ? P2 Cu2 2.1768(15) . ? Cu1 Cu2 2.9083(14) . ? 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 C6 C1 C2 117.6(6) . . ? C6 C1 P1 124.9(5) . . ? C2 C1 P1 117.5(5) . . ? C1 C2 C3 120.4(7) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C4 C3 C2 120.6(8) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C5 C4 C3 120.3(7) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 120.5(8) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C1 C6 C5 120.5(7) . . ? C1 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C12 C7 C8 118.8(5) . . ? C12 C7 P1 125.4(5) . . ? C8 C7 P1 115.7(4) . . ? C7 C8 C9 121.0(6) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C10 C9 C8 120.1(6) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 118.9(5) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C10 C11 C12 121.4(6) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C7 C12 C11 119.7(6) . . ? C7 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? N1 C13 C17 121.9(5) . . ? N1 C13 P1 116.4(4) . . ? C17 C13 P1 121.7(4) . . ? N1 C14 C15 122.4(5) . . ? N1 C14 C18 116.3(5) . . ? C15 C14 C18 121.3(5) . . ? C14 C15 C16 119.1(6) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? C17 C16 C15 118.4(6) . . ? C17 C16 H16 120.8 . . ? C15 C16 H16 120.8 . . ? C16 C17 C13 119.3(5) . . ? C16 C17 H17 120.3 . . ? C13 C17 H17 120.3 . . ? N2 C18 C14 119.0(5) . . ? N2 C18 H18 120.5 . . ? C14 C18 H18 120.5 . . ? C24 C19 C20 118.4(6) . . ? C24 C19 N2 125.8(6) . . ? C20 C19 N2 115.8(5) . . ? C21 C20 C19 122.7(7) . . ? C21 C20 H20 118.6 . . ? C19 C20 H20 118.6 . . ? C22 C21 C20 120.1(8) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? O1A C22 C21 131.2(15) 2_656 . ? C21 C22 O1 120.6(15) . 2_656 ? O1A C22 C23 110.0(14) 2_656 . ? C21 C22 C23 118.7(7) . . ? O1 C22 C23 120.7(14) 2_656 . ? C22 C23 C24 122.4(7) . . ? C22 C23 H23 118.8 . . ? C24 C23 H23 118.8 . . ? C19 C24 C23 117.7(8) . . ? C19 C24 H24 121.1 . . ? C23 C24 H24 121.1 . . ? C26 C25 O1 108.7(18) . . ? C26 C25 H25A 109.9 . . ? O1 C25 H25A 109.9 . . ? C26 C25 H25B 109.9 . . ? O1 C25 H25B 109.9 . . ? H25A C25 H25B 108.3 . . ? C25 C26 O2 102.0(16) . . ? C25 C26 H26A 111.4 . . ? O2 C26 H26A 111.4 . . ? C25 C26 H26B 111.4 . . ? O2 C26 H26B 111.4 . . ? H26A C26 H26B 109.2 . . ? C28 C27A O2A 116(2) . . ? C28 C27A H27A 108.2 . . ? O2A C27A H27A 108.2 . . ? C28 C27A H27B 108.2 . . ? O2A C27A H27B 108.2 . . ? H27A C27A H27B 107.4 . . ? C27A C28 O3 117.5(10) . . ? O3 C28 C27 103.9(8) . . ? C27A C28 H28A 104.0 . . ? O3 C28 H28A 111.0 . . ? C27 C28 H28A 111.0 . . ? C27A C28 H28B 103.8 . . ? O3 C28 H28B 111.0 . . ? C27 C28 H28B 111.0 . . ? H28A C28 H28B 109.0 . . ? O3 C29 C30 111.2(6) . . ? O3 C29 H29A 109.4 . . ? C30 C29 H29A 109.4 . . ? O3 C29 H29B 109.4 . . ? C30 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? O4 C30 C29 107.1(6) . . ? O4 C30 H30A 110.3 . . ? C29 C30 H30A 110.3 . . ? O4 C30 H30B 110.3 . . ? C29 C30 H30B 110.3 . . ? H30A C30 H30B 108.5 . . ? C32 C31 C36 120.4(6) . . ? C32 C31 O4 124.8(5) . . ? C36 C31 O4 114.8(6) . . ? C31 C32 C33 120.0(5) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 C34 120.0(6) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 118.3(5) . . ? C35 C34 N3 118.2(5) . . ? C33 C34 N3 123.4(6) . . ? C36 C35 C34 121.7(6) . . ? C36 C35 H35 119.1 . . ? C34 C35 H35 119.1 . . ? C35 C36 C31 119.5(6) . . ? C35 C36 H36 120.3 . . ? C31 C36 H36 120.3 . . ? N3 C37 C38 120.3(5) . . ? N3 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? N4 C38 C42 122.8(5) . . ? N4 C38 C37 114.9(5) . . ? C42 C38 C37 122.3(5) . . ? N4 C39 C40 121.9(5) . . ? N4 C39 P2 114.7(4) . . ? C40 C39 P2 123.4(4) . . ? C41 C40 C39 119.7(6) . . ? C41 C40 H40 120.2 . . ? C39 C40 H40 120.2 . . ? C40 C41 C42 118.4(6) . . ? C40 C41 H41 120.8 . . ? C42 C41 H41 120.8 . . ? C38 C42 C41 119.5(6) . . ? C38 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C48 C43 C44 118.5(5) . . ? C48 C43 P2 117.3(4) . . ? C44 C43 P2 124.2(4) . . ? C45 C44 C43 120.0(6) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C46 C45 C44 120.7(6) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C45 C46 C47 120.8(6) . . ? C45 C46 H46 119.6 . . ? C47 C46 H46 119.6 . . ? C48 C47 C46 118.1(6) . . ? C48 C47 H47 120.9 . . ? C46 C47 H47 120.9 . . ? C43 C48 C47 121.8(6) . . ? C43 C48 H48 119.1 . . ? C47 C48 H48 119.1 . . ? C50 C49 C54 120.8(6) . . ? C50 C49 P2 122.9(6) . . ? C54 C49 P2 116.3(5) . . ? C49 C50 C51 117.7(10) . . ? C49 C50 H50 121.2 . . ? C51 C50 H50 121.2 . . ? C52 C51 C50 121.5(11) . . ? C52 C51 H51 119.3 . . ? C50 C51 H51 119.3 . . ? C53 C52 C51 120.3(9) . . ? C53 C52 H52 119.8 . . ? C51 C52 H52 119.8 . . ? C52 C53 C54 122.0(11) . . ? C52 C53 H53 119.0 . . ? C54 C53 H53 119.0 . . ? C49 C54 C53 117.6(9) . . ? C49 C54 H54 121.2 . . ? C53 C54 H54 121.2 . . ? O6 C55 O5 126.0(5) . . ? O6 C55 C56 117.8(4) . . ? O5 C55 C56 116.2(5) . . ? C57 C56 C58 119.4(5) . . ? C57 C56 C55 120.4(5) . . ? C58 C56 C55 120.1(5) . . ? C56 C57 C58 120.6(5) . 2_656 ? C56 C57 H57 119.7 . . ? C58 C57 H57 119.7 2_656 . ? C56 C58 C57 119.9(5) . 2_656 ? C56 C58 H58 120.0 . . ? C57 C58 H58 120.0 2_656 . ? C13 N1 C14 118.9(5) . . ? C13 N1 Cu2 128.3(4) . . ? C14 N1 Cu2 112.9(3) . . ? C18 N2 C19 122.1(5) . . ? C18 N2 Cu2 113.4(4) . . ? C19 N2 Cu2 124.5(4) . . ? C37 N3 C34 121.2(5) . . ? C37 N3 Cu1 111.8(4) . . ? C34 N3 Cu1 127.0(4) . . ? C38 N4 C39 117.7(5) . . ? C38 N4 Cu1 115.0(3) . . ? C39 N4 Cu1 127.3(4) . . ? C22 O1 C25 116(2) 2_656 . ? C27 O2 C26 109.7(18) . . ? C29 O3 C28 113.0(6) . . ? C31 O4 C30 117.9(5) . . ? C22 O1A C25A 117(2) 2_656 . ? C26A O2A C27A 104.7(19) . . ? O1A C25A C26A 109(2) . . ? O1A C25A H25C 109.9 . . ? C26A C25A H25C 109.9 . . ? O1A C25A H25D 109.9 . . ? C26A C25A H25D 109.9 . . ? H25C C25A H25D 108.3 . . ? O2A C26A C25A 117(2) . . ? O2A C26A H26C 108.0 . . ? C25A C26A H26C 108.0 . . ? O2A C26A H26D 108.0 . . ? C25A C26A H26D 108.0 . . ? H26C C26A H26D 107.3 . . ? O2 C27 C28 97.1(19) . . ? O2 C27 H27C 112.3 . . ? C28 C27 H27C 112.3 . . ? O2 C27 H27D 112.3 . . ? C28 C27 H27D 112.3 . . ? H27C C27 H27D 109.9 . . ? C55 O5 Cu1 128.0(4) . . ? C55 O6 Cu2 125.5(3) . . ? F2 B1 F8 111.0(12) . . ? F2 B1 F5 137.3(12) . . ? F8 B1 F5 111.6(6) . . ? F2 B1 F1 111.5(6) . . ? F8 B1 F1 137.2(12) . . ? F2 B1 F4 110.4(6) . . ? F8 B1 F4 51.0(10) . . ? F5 B1 F4 98.4(13) . . ? F1 B1 F4 108.4(6) . . ? F2 B1 F7 52.0(10) . . ? F8 B1 F7 109.6(6) . . ? F5 B1 F7 109.4(6) . . ? F1 B1 F7 99.8(13) . . ? F4 B1 F7 151.3(12) . . ? F2 B1 F3 109.8(6) . . ? F8 B1 F3 60.1(11) . . ? F5 B1 F3 89.1(12) . . ? F1 B1 F3 108.3(6) . . ? F4 B1 F3 108.3(6) . . ? F7 B1 F3 66.2(10) . . ? F2 B1 F6 57.9(10) . . ? F8 B1 F6 109.5(6) . . ? F5 B1 F6 109.1(6) . . ? F1 B1 F6 89.5(12) . . ? F4 B1 F6 68.3(10) . . ? F7 B1 F6 107.6(6) . . ? F3 B1 F6 161.7(12) . . ? N5 C60 C59 176.1(16) . . ? C60 C59 H59A 109.5 . . ? C60 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C60 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N6 C61 C62 177(4) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N7 C63 C64 152(4) . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C1 P1 C7 104.1(2) . . ? C1 P1 C13 101.3(3) . . ? C7 P1 C13 105.2(3) . . ? C1 P1 Cu1 112.55(19) . . ? C7 P1 Cu1 113.64(19) . . ? C13 P1 Cu1 118.43(18) . . ? C43 P2 C49 103.7(3) . . ? C43 P2 C39 103.0(2) . . ? C49 P2 C39 101.9(3) . . ? C43 P2 Cu2 110.52(19) . . ? C49 P2 Cu2 116.4(2) . . ? C39 P2 Cu2 119.43(18) . . ? O5 Cu1 N4 116.02(18) . . ? O5 Cu1 P1 119.91(15) . . ? N4 Cu1 P1 121.68(12) . . ? O5 Cu1 N3 94.28(17) . . ? N4 Cu1 N3 78.04(18) . . ? P1 Cu1 N3 112.05(13) . . ? O5 Cu1 Cu2 79.31(12) . . ? N4 Cu1 Cu2 90.56(12) . . ? P1 Cu1 Cu2 84.61(5) . . ? N3 Cu1 Cu2 163.02(13) . . ? O6 Cu2 N1 111.95(17) . . ? O6 Cu2 N2 94.63(17) . . ? N1 Cu2 N2 78.42(18) . . ? O6 Cu2 P2 127.61(13) . . ? N1 Cu2 P2 116.80(12) . . ? N2 Cu2 P2 112.44(13) . . ? O6 Cu2 Cu1 80.98(11) . . ? N1 Cu2 Cu1 89.09(12) . . ? N2 Cu2 Cu1 164.20(13) . . ? P2 Cu2 Cu1 81.76(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.0(11) . . . . ? P1 C1 C2 C3 178.6(6) . . . . ? C1 C2 C3 C4 -2.3(13) . . . . ? C2 C3 C4 C5 3.2(14) . . . . ? C3 C4 C5 C6 -0.8(14) . . . . ? C2 C1 C6 C5 3.4(11) . . . . ? P1 C1 C6 C5 -176.3(6) . . . . ? C4 C5 C6 C1 -2.6(13) . . . . ? C12 C7 C8 C9 0.9(8) . . . . ? P1 C7 C8 C9 -179.7(4) . . . . ? C7 C8 C9 C10 0.8(9) . . . . ? C8 C9 C10 C11 -1.6(9) . . . . ? C9 C10 C11 C12 0.6(9) . . . . ? C8 C7 C12 C11 -1.8(8) . . . . ? P1 C7 C12 C11 178.8(4) . . . . ? C10 C11 C12 C7 1.1(9) . . . . ? N1 C14 C15 C16 -3.1(9) . . . . ? C18 C14 C15 C16 178.0(6) . . . . ? C14 C15 C16 C17 2.9(9) . . . . ? C15 C16 C17 C13 -1.0(9) . . . . ? N1 C13 C17 C16 -0.9(8) . . . . ? P1 C13 C17 C16 179.4(5) . . . . ? N1 C14 C18 N2 -2.1(8) . . . . ? C15 C14 C18 N2 176.9(6) . . . . ? C24 C19 C20 C21 1.7(10) . . . . ? N2 C19 C20 C21 -177.3(6) . . . . ? C19 C20 C21 C22 -0.9(11) . . . . ? C20 C21 C22 O1A 175.8(14) . . . 2_656 ? C20 C21 C22 O1 -177.6(12) . . . 2_656 ? C20 C21 C22 C23 -0.1(11) . . . . ? O1A C22 C23 C24 -176.5(12) 2_656 . . . ? C21 C22 C23 C24 0.2(13) . . . . ? O1 C22 C23 C24 177.7(12) 2_656 . . . ? C20 C19 C24 C23 -1.5(10) . . . . ? N2 C19 C24 C23 177.3(6) . . . . ? C22 C23 C24 C19 0.7(12) . . . . ? O1 C25 C26 O2 71(2) . . . . ? O2A C27A C28 O3 -73.1(19) . . . . ? O2A C27A C28 C27 -73(7) . . . . ? O3 C29 C30 O4 62.4(8) . . . . ? C36 C31 C32 C33 0.9(9) . . . . ? O4 C31 C32 C33 -176.8(6) . . . . ? C31 C32 C33 C34 -2.3(8) . . . . ? C32 C33 C34 C35 3.1(8) . . . . ? C32 C33 C34 N3 -179.8(5) . . . . ? C33 C34 C35 C36 -2.6(10) . . . . ? N3 C34 C35 C36 -179.8(6) . . . . ? C34 C35 C36 C31 1.2(11) . . . . ? C32 C31 C36 C35 -0.3(10) . . . . ? O4 C31 C36 C35 177.6(6) . . . . ? N3 C37 C38 N4 -0.4(8) . . . . ? N3 C37 C38 C42 -179.7(6) . . . . ? N4 C39 C40 C41 -0.4(9) . . . . ? P2 C39 C40 C41 176.7(5) . . . . ? C39 C40 C41 C42 -0.8(10) . . . . ? N4 C38 C42 C41 -0.7(9) . . . . ? C37 C38 C42 C41 178.6(6) . . . . ? C40 C41 C42 C38 1.3(10) . . . . ? C48 C43 C44 C45 -1.4(8) . . . . ? P2 C43 C44 C45 -179.1(4) . . . . ? C43 C44 C45 C46 0.2(9) . . . . ? C44 C45 C46 C47 -0.7(10) . . . . ? C45 C46 C47 C48 2.3(11) . . . . ? C44 C43 C48 C47 3.2(9) . . . . ? P2 C43 C48 C47 -178.9(5) . . . . ? C46 C47 C48 C43 -3.6(10) . . . . ? C54 C49 C50 C51 0.4(10) . . . . ? P2 C49 C50 C51 -176.7(6) . . . . ? C49 C50 C51 C52 2.8(13) . . . . ? C50 C51 C52 C53 -4.6(16) . . . . ? C51 C52 C53 C54 3.3(16) . . . . ? C50 C49 C54 C53 -1.6(10) . . . . ? P2 C49 C54 C53 175.6(6) . . . . ? C52 C53 C54 C49 -0.1(13) . . . . ? O6 C55 C56 C57 -155.4(6) . . . . ? O5 C55 C56 C57 25.7(8) . . . . ? O6 C55 C56 C58 24.7(8) . . . . ? O5 C55 C56 C58 -154.1(6) . . . . ? C58 C56 C57 C58 1.6(11) . . . 2_656 ? C55 C56 C57 C58 -178.3(6) . . . 2_656 ? C57 C56 C58 C57 -1.5(11) . . . 2_656 ? C55 C56 C58 C57 178.3(6) . . . 2_656 ? C17 C13 N1 C14 0.8(7) . . . . ? P1 C13 N1 C14 -179.4(4) . . . . ? C17 C13 N1 Cu2 179.7(4) . . . . ? P1 C13 N1 Cu2 -0.5(6) . . . . ? C15 C14 N1 C13 1.2(8) . . . . ? C18 C14 N1 C13 -179.8(5) . . . . ? C15 C14 N1 Cu2 -177.9(5) . . . . ? C18 C14 N1 Cu2 1.1(6) . . . . ? C14 C18 N2 C19 -177.3(5) . . . . ? C14 C18 N2 Cu2 1.9(7) . . . . ? C24 C19 N2 C18 13.1(9) . . . . ? C20 C19 N2 C18 -168.0(5) . . . . ? C24 C19 N2 Cu2 -166.0(5) . . . . ? C20 C19 N2 Cu2 12.9(7) . . . . ? C38 C37 N3 C34 -178.6(5) . . . . ? C38 C37 N3 Cu1 -1.0(6) . . . . ? C35 C34 N3 C37 -148.7(6) . . . . ? C33 C34 N3 C37 34.2(8) . . . . ? C35 C34 N3 Cu1 34.1(7) . . . . ? C33 C34 N3 Cu1 -143.0(5) . . . . ? C42 C38 N4 C39 -0.5(8) . . . . ? C37 C38 N4 C39 -179.8(5) . . . . ? C42 C38 N4 Cu1 -179.0(5) . . . . ? C37 C38 N4 Cu1 1.7(6) . . . . ? C40 C39 N4 C38 1.0(7) . . . . ? P2 C39 N4 C38 -176.3(4) . . . . ? C40 C39 N4 Cu1 179.3(4) . . . . ? P2 C39 N4 Cu1 2.0(6) . . . . ? C26 C25 O1 C22 171.6(16) . . . 2_656 ? C25 C26 O2 C27 -102.1(19) . . . . ? C30 C29 O3 C28 170.5(8) . . . . ? C27A C28 O3 C29 161.9(15) . . . . ? C27 C28 O3 C29 161.8(12) . . . . ? C32 C31 O4 C30 -7.5(9) . . . . ? C36 C31 O4 C30 174.8(6) . . . . ? C29 C30 O4 C31 177.6(6) . . . . ? C28 C27A O2A C26A 169.9(15) . . . . ? C22 O1A C25A C26A -175.6(18) 2_656 . . . ? C27A O2A C26A C25A -116(2) . . . . ? O1A C25A C26A O2A 108(3) . . . . ? C26 O2 C27 C28 -156.3(11) . . . . ? C27A C28 C27 O2 110(8) . . . . ? O3 C28 C27 O2 -70.7(14) . . . . ? O6 C55 O5 Cu1 -2.3(9) . . . . ? C56 C55 O5 Cu1 176.4(4) . . . . ? O5 C55 O6 Cu2 -3.3(9) . . . . ? C56 C55 O6 Cu2 178.0(4) . . . . ? C6 C1 P1 C7 2.9(7) . . . . ? C2 C1 P1 C7 -176.7(5) . . . . ? C6 C1 P1 C13 -106.1(6) . . . . ? C2 C1 P1 C13 74.3(6) . . . . ? C6 C1 P1 Cu1 126.5(6) . . . . ? C2 C1 P1 Cu1 -53.2(6) . . . . ? C12 C7 P1 C1 -93.7(5) . . . . ? C8 C7 P1 C1 86.8(4) . . . . ? C12 C7 P1 C13 12.3(5) . . . . ? C8 C7 P1 C13 -167.1(4) . . . . ? C12 C7 P1 Cu1 143.5(4) . . . . ? C8 C7 P1 Cu1 -36.0(4) . . . . ? N1 C13 P1 C1 -138.9(4) . . . . ? C17 C13 P1 C1 40.9(5) . . . . ? N1 C13 P1 C7 112.9(4) . . . . ? C17 C13 P1 C7 -67.3(5) . . . . ? N1 C13 P1 Cu1 -15.4(5) . . . . ? C17 C13 P1 Cu1 164.4(4) . . . . ? C48 C43 P2 C49 84.6(5) . . . . ? C44 C43 P2 C49 -97.7(5) . . . . ? C48 C43 P2 C39 -169.4(5) . . . . ? C44 C43 P2 C39 8.3(5) . . . . ? C48 C43 P2 Cu2 -40.8(5) . . . . ? C44 C43 P2 Cu2 137.0(4) . . . . ? C50 C49 P2 C43 -14.7(6) . . . . ? C54 C49 P2 C43 168.1(5) . . . . ? C50 C49 P2 C39 -121.5(6) . . . . ? C54 C49 P2 C39 61.4(6) . . . . ? C50 C49 P2 Cu2 106.8(5) . . . . ? C54 C49 P2 Cu2 -70.3(6) . . . . ? N4 C39 P2 C43 99.5(4) . . . . ? C40 C39 P2 C43 -77.8(5) . . . . ? N4 C39 P2 C49 -153.3(4) . . . . ? C40 C39 P2 C49 29.4(6) . . . . ? N4 C39 P2 Cu2 -23.4(4) . . . . ? C40 C39 P2 Cu2 159.3(4) . . . . ? C55 O5 Cu1 N4 -81.0(5) . . . . ? C55 O5 Cu1 P1 81.7(5) . . . . ? C55 O5 Cu1 N3 -159.8(5) . . . . ? C55 O5 Cu1 Cu2 4.3(5) . . . . ? C38 N4 Cu1 O5 -90.6(4) . . . . ? C39 N4 Cu1 O5 91.1(4) . . . . ? C38 N4 Cu1 P1 107.0(3) . . . . ? C39 N4 Cu1 P1 -71.3(4) . . . . ? C38 N4 Cu1 N3 -1.7(4) . . . . ? C39 N4 Cu1 N3 -180.0(4) . . . . ? C38 N4 Cu1 Cu2 -169.0(3) . . . . ? C39 N4 Cu1 Cu2 12.7(4) . . . . ? C1 P1 Cu1 O5 60.1(2) . . . . ? C7 P1 Cu1 O5 178.2(2) . . . . ? C13 P1 Cu1 O5 -57.6(2) . . . . ? C1 P1 Cu1 N4 -138.2(2) . . . . ? C7 P1 Cu1 N4 -20.1(2) . . . . ? C13 P1 Cu1 N4 104.1(2) . . . . ? C1 P1 Cu1 N3 -48.9(3) . . . . ? C7 P1 Cu1 N3 69.1(2) . . . . ? C13 P1 Cu1 N3 -166.6(2) . . . . ? C1 P1 Cu1 Cu2 134.5(2) . . . . ? C7 P1 Cu1 Cu2 -107.45(19) . . . . ? C13 P1 Cu1 Cu2 16.80(19) . . . . ? C37 N3 Cu1 O5 117.1(4) . . . . ? C34 N3 Cu1 O5 -65.4(4) . . . . ? C37 N3 Cu1 N4 1.4(4) . . . . ? C34 N3 Cu1 N4 178.9(4) . . . . ? C37 N3 Cu1 P1 -118.1(4) . . . . ? C34 N3 Cu1 P1 59.3(4) . . . . ? C37 N3 Cu1 Cu2 50.2(7) . . . . ? C34 N3 Cu1 Cu2 -132.4(4) . . . . ? C55 O6 Cu2 N1 -80.6(5) . . . . ? C55 O6 Cu2 N2 -160.0(5) . . . . ? C55 O6 Cu2 P2 76.9(5) . . . . ? C55 O6 Cu2 Cu1 4.7(5) . . . . ? C13 N1 Cu2 O6 90.5(4) . . . . ? C14 N1 Cu2 O6 -90.5(4) . . . . ? C13 N1 Cu2 N2 -179.1(4) . . . . ? C14 N1 Cu2 N2 -0.1(3) . . . . ? C13 N1 Cu2 P2 -69.7(4) . . . . ? C14 N1 Cu2 P2 109.3(3) . . . . ? C13 N1 Cu2 Cu1 10.6(4) . . . . ? C14 N1 Cu2 Cu1 -170.4(3) . . . . ? C18 N2 Cu2 O6 110.5(4) . . . . ? C19 N2 Cu2 O6 -70.3(4) . . . . ? C18 N2 Cu2 N1 -1.0(4) . . . . ? C19 N2 Cu2 N1 178.2(5) . . . . ? C18 N2 Cu2 P2 -115.4(4) . . . . ? C19 N2 Cu2 P2 63.8(4) . . . . ? C18 N2 Cu2 Cu1 37.4(7) . . . . ? C19 N2 Cu2 Cu1 -143.3(4) . . . . ? C43 P2 Cu2 O6 -167.1(2) . . . . ? C49 P2 Cu2 O6 75.0(3) . . . . ? C39 P2 Cu2 O6 -48.0(2) . . . . ? C43 P2 Cu2 N1 -10.5(2) . . . . ? C49 P2 Cu2 N1 -128.4(3) . . . . ? C39 P2 Cu2 N1 108.6(2) . . . . ? C43 P2 Cu2 N2 77.5(2) . . . . ? C49 P2 Cu2 N2 -40.4(3) . . . . ? C39 P2 Cu2 N2 -163.4(2) . . . . ? C43 P2 Cu2 Cu1 -95.30(18) . . . . ? C49 P2 Cu2 Cu1 146.9(3) . . . . ? C39 P2 Cu2 Cu1 23.86(19) . . . . ? O5 Cu1 Cu2 O6 -3.55(18) . . . . ? N4 Cu1 Cu2 O6 112.85(17) . . . . ? P1 Cu1 Cu2 O6 -125.38(13) . . . . ? N3 Cu1 Cu2 O6 65.5(5) . . . . ? O5 Cu1 Cu2 N1 108.85(18) . . . . ? N4 Cu1 Cu2 N1 -134.75(16) . . . . ? P1 Cu1 Cu2 N1 -12.98(12) . . . . ? N3 Cu1 Cu2 N1 177.9(5) . . . . ? O5 Cu1 Cu2 N2 71.3(5) . . . . ? N4 Cu1 Cu2 N2 -172.3(5) . . . . ? P1 Cu1 Cu2 N2 -50.5(5) . . . . ? N3 Cu1 Cu2 N2 140.4(6) . . . . ? O5 Cu1 Cu2 P2 -133.89(15) . . . . ? N4 Cu1 Cu2 P2 -17.50(12) . . . . ? P1 Cu1 Cu2 P2 104.27(6) . . . . ? N3 Cu1 Cu2 P2 -64.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.306 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.110