data_global _publ_contact_author_name 'Martin Lutz' _publ_contact_author_address ; Bijvoet Center for Biomolecular Research Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; _publ_contact_author_email 'm.lutz@uu.nl' _publ_contact_author_fax '[+31] 30 2533940' _publ_contact_author_phone '[+31] 30 2533902' loop_ _publ_author_name _publ_author_address 'Tazelaar, Cornelis G. J.' ; Department of Chemistry and Pharmaceutical Sciences VU University Amsterdam De Boeleaan 1083 1081 HV Amsterdam The Netherlands ; 'Lyaskovskyy, Volodymyr' ; Department of Chemistry and Pharmaceutical Sciences VU University Amsterdam De Boeleaan 1083 1081 HV Amsterdam The Netherlands ; 'van Dijk, Tom' ; Department of Chemistry and Pharmaceutical Sciences VU University Amsterdam De Boeleaan 1083 1081 HV Amsterdam The Netherlands ; 'Broere, Danny L. J.' ; Department of Chemistry and Pharmaceutical Sciences VU University Amsterdam De Boeleaan 1083 1081 HV Amsterdam The Netherlands ; 'Kolfschoten, Ludo A.' ; Department of Chemistry and Pharmaceutical Sciences VU University Amsterdam De Boeleaan 1083 1081 HV Amsterdam The Netherlands ; 'Khiar, Rima Osman Hassan' ; Department of Chemistry and Pharmaceutical Sciences VU University Amsterdam De Boeleaan 1083 1081 HV Amsterdam The Netherlands ; 'Lutz, Martin' ; Bijvoet Center for Biomolecular Research Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'Slootweg, J. Chris' ; Department of Chemistry and Pharmaceutical Sciences VU University Amsterdam De Boeleaan 1083 1081 HV Amsterdam The Netherlands ; 'Lammertsma, Koop' ; Department of Chemistry and Pharmaceutical Sciences VU University Amsterdam De Boeleaan 1083 1081 HV Amsterdam The Netherlands ; data_l0122a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H36 Cu N7 O P, F6 P, C H2 Cl2' _chemical_formula_sum 'C24 H38 Cl2 Cu F6 N7 O P2' _chemical_formula_weight 750.99 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' _symmetry_space_group_name_Hall 'P 2 2ab' 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' _cell_length_a 16.9778(6) _cell_length_b 18.8108(7) _cell_length_c 10.5559(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3371.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9119 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.51 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.51 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 0.965 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.6677 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'SADABS-2008/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa ApexII' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46498 _diffrn_reflns_av_R_equivalents 0.0167 _diffrn_reflns_av_sigmaI/netI 0.0107 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.52 _reflns_number_total 7748 _reflns_number_gt 7525 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Apex' _computing_cell_refinement 'SAINT V7.68A' _computing_data_reduction 'SAINT V7.68A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+1.8717P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.009(10) _refine_ls_number_reflns 7748 _refine_ls_number_parameters 401 _refine_ls_number_restraints 91 _refine_ls_R_factor_all 0.0337 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0936 _refine_ls_wR_factor_gt 0.0925 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.210 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.209347(18) 0.270107(16) 0.45596(3) 0.02568(9) Uani 1 1 d . . . P1 P 0.32594(4) 0.28396(3) 0.69083(6) 0.02219(13) Uani 1 1 d . . . O1 O 0.37863(12) 0.28959(10) 0.79866(19) 0.0327(4) Uani 1 1 d . . . N11 N 0.31361(12) 0.20035(11) 0.6399(2) 0.0224(4) Uani 1 1 d . . . N12 N 0.26610(12) 0.18308(11) 0.5384(2) 0.0219(4) Uani 1 1 d . . . N21 N 0.35747(12) 0.32895(11) 0.5642(2) 0.0234(4) Uani 1 1 d . . . N22 N 0.31850(12) 0.32626(11) 0.4484(2) 0.0232(4) Uani 1 1 d . . . N31 N 0.23570(13) 0.31557(12) 0.7198(2) 0.0249(4) Uani 1 1 d . . . N32 N 0.17569(13) 0.31408(11) 0.6307(2) 0.0231(4) Uani 1 1 d . . . N41 N 0.13997(14) 0.26558(13) 0.3137(2) 0.0308(5) Uani 1 1 d . . . C11 C 0.27306(14) 0.11286(12) 0.5253(2) 0.0217(5) Uani 1 1 d . . . C12 C 0.32524(16) 0.08520(14) 0.6176(3) 0.0268(5) Uani 1 1 d . . . H12 H 0.3401 0.0369 0.6280 0.032 Uiso 1 1 calc R . . C13 C 0.35004(15) 0.14128(13) 0.6887(3) 0.0259(5) Uani 1 1 d . . . H13 H 0.3855 0.1398 0.7583 0.031 Uiso 1 1 calc R . . C14 C 0.22525(15) 0.07317(13) 0.4274(3) 0.0249(5) Uani 1 1 d . . . C15 C 0.2481(2) -0.00581(15) 0.4259(3) 0.0363(6) Uani 1 1 d . . . H15A H 0.3041 -0.0104 0.4046 0.054 Uiso 1 1 calc R . . H15B H 0.2164 -0.0309 0.3626 0.054 Uiso 1 1 calc R . . H15C H 0.2385 -0.0265 0.5098 0.054 Uiso 1 1 calc R . . C16 C 0.23968(18) 0.10302(15) 0.2942(3) 0.0329(6) Uani 1 1 d . . . H16A H 0.2312 0.1545 0.2948 0.049 Uiso 1 1 calc R . . H16B H 0.2031 0.0807 0.2344 0.049 Uiso 1 1 calc R . . H16C H 0.2940 0.0929 0.2684 0.049 Uiso 1 1 calc R . . C17 C 0.13818(16) 0.08048(16) 0.4633(3) 0.0373(6) Uani 1 1 d . . . H17A H 0.1289 0.0572 0.5450 0.056 Uiso 1 1 calc R . . H17B H 0.1055 0.0580 0.3981 0.056 Uiso 1 1 calc R . . H17C H 0.1245 0.1310 0.4699 0.056 Uiso 1 1 calc R . . C21 C 0.36249(16) 0.36485(14) 0.3709(3) 0.0274(5) Uani 1 1 d . . . C22 C 0.42899(16) 0.39273(14) 0.4341(3) 0.0318(6) Uani 1 1 d . . . H22 H 0.4690 0.4219 0.3987 0.038 Uiso 1 1 calc R . . C23 C 0.42436(15) 0.36942(13) 0.5559(3) 0.0295(5) Uani 1 1 d . . . H23 H 0.4605 0.3793 0.6223 0.035 Uiso 1 1 calc R . . C24 C 0.34080(19) 0.37387(16) 0.2326(3) 0.0347(6) Uani 1 1 d . . . C25 C 0.4023(3) 0.4173(3) 0.1643(4) 0.0677(13) Uani 1 1 d . . . H25A H 0.4065 0.4643 0.2041 0.102 Uiso 1 1 calc R . . H25B H 0.3871 0.4229 0.0753 0.102 Uiso 1 1 calc R . . H25C H 0.4533 0.3931 0.1692 0.102 Uiso 1 1 calc R . . C26 C 0.2609(2) 0.4119(2) 0.2221(3) 0.0461(8) Uani 1 1 d . . . H26A H 0.2670 0.4619 0.2462 0.069 Uiso 1 1 calc R . . H26B H 0.2228 0.3890 0.2787 0.069 Uiso 1 1 calc R . . H26C H 0.2418 0.4090 0.1346 0.069 Uiso 1 1 calc R . . C27 C 0.3347(3) 0.2997(2) 0.1720(3) 0.0499(9) Uani 1 1 d . . . H27A H 0.3240 0.3046 0.0812 0.075 Uiso 1 1 calc R . . H27B H 0.2917 0.2731 0.2121 0.075 Uiso 1 1 calc R . . H27C H 0.3844 0.2741 0.1841 0.075 Uiso 1 1 calc R . . C31 C 0.11535(16) 0.34664(13) 0.6861(3) 0.0267(5) Uani 1 1 d . . . C32 C 0.13588(19) 0.37012(16) 0.8089(3) 0.0354(6) Uani 1 1 d . . . H32 H 0.1032 0.3951 0.8669 0.042 Uiso 1 1 calc R . . C33 C 0.2121(2) 0.34977(15) 0.8273(3) 0.0352(6) Uani 1 1 d . . . H33 H 0.2429 0.3579 0.9010 0.042 Uiso 1 1 calc R . . C34 C 0.03737(16) 0.35525(15) 0.6174(3) 0.0328(6) Uani 1 1 d . . . C35 C -0.0232(2) 0.3887(2) 0.7070(4) 0.0528(9) Uani 1 1 d . . . H35A H -0.0305 0.3578 0.7808 0.079 Uiso 1 1 calc R . . H35B H -0.0735 0.3943 0.6625 0.079 Uiso 1 1 calc R . . H35C H -0.0043 0.4353 0.7349 0.079 Uiso 1 1 calc R . . C36 C 0.00713(18) 0.28194(16) 0.5764(3) 0.0401(7) Uani 1 1 d . . . H36A H 0.0435 0.2613 0.5143 0.060 Uiso 1 1 calc R . . H36B H -0.0452 0.2869 0.5382 0.060 Uiso 1 1 calc R . . H36C H 0.0038 0.2507 0.6505 0.060 Uiso 1 1 calc R . . C37 C 0.04857(18) 0.40395(17) 0.5026(3) 0.0391(7) Uani 1 1 d . . . H37A H 0.0655 0.4511 0.5313 0.059 Uiso 1 1 calc R . . H37B H -0.0013 0.4082 0.4566 0.059 Uiso 1 1 calc R . . H37C H 0.0888 0.3838 0.4465 0.059 Uiso 1 1 calc R . . C41 C 0.10174(15) 0.26245(16) 0.2250(3) 0.0287(5) Uani 1 1 d . . . C42 C 0.05390(18) 0.2587(2) 0.1110(3) 0.0403(7) Uani 1 1 d . . . H42A H 0.0881 0.2523 0.0371 0.060 Uiso 1 1 calc R . . H42B H 0.0238 0.3029 0.1017 0.060 Uiso 1 1 calc R . . H42C H 0.0175 0.2185 0.1174 0.060 Uiso 1 1 calc R . . P2 P 0.5000 0.5000 0.84833(10) 0.0384(3) Uani 1 2 d SD . . F1 F 0.40982(12) 0.47625(13) 0.8469(2) 0.0552(6) Uani 1 1 d DU . . F2 F 0.52645(16) 0.41891(13) 0.8448(4) 0.0871(11) Uani 1 1 d DU . . F3 F 0.5000 0.5000 0.6987(2) 0.0438(6) Uani 1 2 d SDU . . F4 F 0.5000 0.5000 0.9962(3) 0.120(2) Uani 1 2 d SDU . . P3 P 0.0000 0.5000 0.10557(11) 0.0407(3) Uani 1 2 d SD . . F5 F -0.0194(4) 0.4208(2) 0.1042(7) 0.180(3) Uani 1 1 d DU . . F6 F 0.0846(3) 0.4836(5) 0.1020(9) 0.247(4) Uani 1 1 d DU . . F7 F 0.0000 0.5000 -0.0377(5) 0.188(4) Uani 1 2 d SDU . . F8 F 0.0000 0.5000 0.2479(5) 0.255(5) Uani 1 2 d SDU . . Cl1 Cl 0.24750(8) 0.17238(6) 0.98540(10) 0.0650(3) Uani 1 1 d . . . Cl2 Cl 0.12972(9) 0.14709(9) 0.79637(12) 0.0802(4) Uani 1 1 d . . . C51 C 0.1820(4) 0.1096(2) 0.9221(5) 0.0745(15) Uani 1 1 d . . . H51A H 0.2116 0.0675 0.8920 0.089 Uiso 1 1 calc R . . H51B H 0.1448 0.0937 0.9886 0.089 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02755(15) 0.02416(15) 0.02535(15) -0.00097(12) -0.00786(12) 0.00129(12) P1 0.0245(3) 0.0186(3) 0.0234(3) -0.0012(2) -0.0071(2) -0.0002(2) O1 0.0386(10) 0.0283(9) 0.0312(10) -0.0033(8) -0.0157(9) -0.0002(8) N11 0.0246(10) 0.0184(9) 0.0241(10) -0.0004(8) -0.0079(8) -0.0001(7) N12 0.0238(9) 0.0194(9) 0.0225(9) -0.0007(8) -0.0049(8) -0.0010(7) N21 0.0227(9) 0.0207(9) 0.0269(11) 0.0000(8) -0.0051(8) -0.0025(8) N22 0.0257(9) 0.0211(9) 0.0227(9) 0.0027(8) -0.0035(8) -0.0012(7) N31 0.0287(10) 0.0242(10) 0.0219(10) -0.0031(8) -0.0051(8) 0.0032(8) N32 0.0235(9) 0.0207(9) 0.0252(10) -0.0009(8) -0.0040(8) 0.0003(8) N41 0.0316(11) 0.0287(11) 0.0319(12) -0.0008(10) -0.0063(9) 0.0014(9) C11 0.0214(10) 0.0172(10) 0.0264(12) 0.0005(9) -0.0003(9) -0.0018(8) C12 0.0267(11) 0.0184(11) 0.0354(14) 0.0030(10) -0.0046(11) 0.0016(9) C13 0.0252(11) 0.0229(11) 0.0296(12) 0.0052(10) -0.0050(10) 0.0013(9) C14 0.0251(12) 0.0197(11) 0.0300(13) -0.0026(9) -0.0034(9) -0.0008(9) C15 0.0468(15) 0.0178(11) 0.0442(16) -0.0058(11) -0.0095(13) 0.0002(11) C16 0.0385(14) 0.0309(13) 0.0292(13) -0.0025(11) -0.0043(12) -0.0009(11) C17 0.0263(13) 0.0376(15) 0.0480(17) -0.0117(14) -0.0025(13) -0.0081(11) C21 0.0281(12) 0.0197(11) 0.0342(14) 0.0026(10) 0.0028(10) 0.0012(9) C22 0.0260(12) 0.0218(11) 0.0476(17) 0.0072(11) 0.0015(12) -0.0037(9) C23 0.0230(11) 0.0214(11) 0.0442(15) -0.0023(11) -0.0061(11) -0.0033(9) C24 0.0398(15) 0.0329(14) 0.0313(14) 0.0102(11) 0.0024(12) 0.0018(12) C25 0.062(2) 0.091(3) 0.050(2) 0.034(2) 0.0107(19) -0.014(2) C26 0.0529(19) 0.0444(17) 0.0409(17) 0.0108(15) -0.0058(15) 0.0077(15) C27 0.068(2) 0.052(2) 0.0302(16) -0.0029(14) 0.0000(15) 0.0164(18) C31 0.0272(12) 0.0183(11) 0.0346(14) -0.0001(10) 0.0031(10) -0.0005(9) C32 0.0422(15) 0.0319(14) 0.0321(14) -0.0049(12) 0.0060(12) 0.0073(12) C33 0.0479(16) 0.0336(13) 0.0242(13) -0.0056(10) -0.0041(12) 0.0084(13) C34 0.0219(12) 0.0281(13) 0.0485(17) -0.0074(12) 0.0033(12) 0.0017(10) C35 0.0298(14) 0.057(2) 0.072(3) -0.016(2) 0.0078(16) 0.0096(14) C36 0.0301(13) 0.0321(14) 0.0579(19) -0.0057(13) -0.0016(13) -0.0082(11) C37 0.0318(14) 0.0318(14) 0.0537(19) 0.0023(13) -0.0124(13) 0.0028(11) C41 0.0259(11) 0.0336(13) 0.0266(12) 0.0019(11) -0.0035(10) 0.0004(10) C42 0.0318(13) 0.063(2) 0.0263(14) 0.0028(14) -0.0074(11) -0.0032(14) P2 0.0385(6) 0.0519(7) 0.0247(5) 0.000 0.000 -0.0159(5) F1 0.0393(10) 0.0778(16) 0.0484(11) -0.0001(11) -0.0009(9) -0.0214(10) F2 0.0697(17) 0.0535(14) 0.138(3) 0.0517(17) -0.0450(18) -0.0100(12) F3 0.0468(14) 0.0558(16) 0.0289(12) 0.000 0.000 0.0086(13) F4 0.110(3) 0.224(6) 0.0246(14) 0.000 0.000 -0.108(4) P3 0.0557(7) 0.0357(6) 0.0308(5) 0.000 0.000 0.0007(5) F5 0.244(6) 0.058(2) 0.239(6) 0.018(3) 0.036(5) -0.040(3) F6 0.095(3) 0.274(7) 0.370(9) 0.047(7) -0.011(5) 0.045(5) F7 0.295(9) 0.201(7) 0.067(3) 0.000 0.000 -0.036(7) F8 0.406(11) 0.299(9) 0.060(3) 0.000 0.000 -0.011(9) Cl1 0.0875(7) 0.0664(6) 0.0410(5) 0.0009(4) 0.0017(5) -0.0152(6) Cl2 0.0835(8) 0.1072(10) 0.0498(6) 0.0029(6) 0.0017(6) -0.0278(7) C51 0.118(4) 0.049(2) 0.057(3) -0.0002(19) 0.002(3) -0.021(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N41 1.911(2) . ? Cu1 N12 2.089(2) . ? Cu1 N32 2.101(2) . ? Cu1 N22 2.134(2) . ? P1 O1 1.4516(19) . ? P1 N21 1.670(2) . ? P1 N31 1.672(2) . ? P1 N11 1.675(2) . ? N11 C13 1.372(3) . ? N11 N12 1.380(3) . ? N12 C11 1.333(3) . ? N21 C23 1.370(3) . ? N21 N22 1.390(3) . ? N22 C21 1.324(3) . ? N31 C33 1.365(3) . ? N31 N32 1.387(3) . ? N32 C31 1.329(3) . ? N41 C41 1.141(4) . ? C11 C12 1.416(3) . ? C11 C14 1.512(3) . ? C12 C13 1.361(4) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C17 1.532(4) . ? C14 C16 1.533(4) . ? C14 C15 1.536(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C21 C22 1.412(4) . ? C21 C24 1.516(4) . ? C22 C23 1.360(4) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.510(5) . ? C24 C27 1.538(5) . ? C24 C26 1.538(5) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C31 C32 1.413(4) . ? C31 C34 1.518(4) . ? C32 C33 1.363(5) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.532(4) . ? C34 C37 1.531(5) . ? C34 C36 1.534(4) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C41 C42 1.453(4) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? P2 F4 1.561(3) . ? P2 F3 1.580(3) . ? P2 F2 1.591(3) . ? P2 F2 1.591(3) 2_665 ? P2 F1 1.5949(19) 2_665 ? P2 F1 1.5950(19) . ? P3 F6 1.470(5) 2_565 ? P3 F6 1.470(5) . ? P3 F8 1.502(6) . ? P3 F7 1.513(6) . ? P3 F5 1.526(4) 2_565 ? P3 F5 1.526(4) . ? Cl1 C51 1.755(5) . ? Cl2 C51 1.746(6) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? 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 N41 Cu1 N12 125.23(9) . . ? N41 Cu1 N32 122.70(9) . . ? N12 Cu1 N32 93.90(8) . . ? N41 Cu1 N22 121.88(10) . . ? N12 Cu1 N22 90.16(8) . . ? N32 Cu1 N22 94.24(8) . . ? O1 P1 N21 113.14(12) . . ? O1 P1 N31 113.30(12) . . ? N21 P1 N31 105.07(11) . . ? O1 P1 N11 113.40(11) . . ? N21 P1 N11 105.01(11) . . ? N31 P1 N11 106.16(11) . . ? C13 N11 N12 111.4(2) . . ? C13 N11 P1 125.70(18) . . ? N12 N11 P1 122.90(16) . . ? C11 N12 N11 105.2(2) . . ? C11 N12 Cu1 140.69(18) . . ? N11 N12 Cu1 114.12(14) . . ? C23 N21 N22 111.0(2) . . ? C23 N21 P1 126.8(2) . . ? N22 N21 P1 122.16(16) . . ? C21 N22 N21 104.7(2) . . ? C21 N22 Cu1 141.61(19) . . ? N21 N22 Cu1 113.49(15) . . ? C33 N31 N32 110.9(2) . . ? C33 N31 P1 126.1(2) . . ? N32 N31 P1 122.83(17) . . ? C31 N32 N31 105.0(2) . . ? C31 N32 Cu1 140.99(19) . . ? N31 N32 Cu1 113.80(16) . . ? C41 N41 Cu1 176.6(2) . . ? N12 C11 C12 110.4(2) . . ? N12 C11 C14 120.8(2) . . ? C12 C11 C14 128.7(2) . . ? C13 C12 C11 106.7(2) . . ? C13 C12 H12 126.6 . . ? C11 C12 H12 126.6 . . ? C12 C13 N11 106.3(2) . . ? C12 C13 H13 126.8 . . ? N11 C13 H13 126.8 . . ? C11 C14 C17 107.7(2) . . ? C11 C14 C16 111.1(2) . . ? C17 C14 C16 110.4(2) . . ? C11 C14 C15 110.4(2) . . ? C17 C14 C15 109.5(2) . . ? C16 C14 C15 107.8(2) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N22 C21 C22 111.3(3) . . ? N22 C21 C24 121.3(3) . . ? C22 C21 C24 127.4(3) . . ? C23 C22 C21 106.3(2) . . ? C23 C22 H22 126.9 . . ? C21 C22 H22 126.9 . . ? C22 C23 N21 106.7(2) . . ? C22 C23 H23 126.7 . . ? N21 C23 H23 126.7 . . ? C25 C24 C21 110.6(3) . . ? C25 C24 C27 109.9(3) . . ? C21 C24 C27 108.4(2) . . ? C25 C24 C26 108.9(3) . . ? C21 C24 C26 109.6(3) . . ? C27 C24 C26 109.4(3) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N32 C31 C32 110.9(2) . . ? N32 C31 C34 120.8(3) . . ? C32 C31 C34 128.3(3) . . ? C33 C32 C31 106.1(3) . . ? C33 C32 H32 127.0 . . ? C31 C32 H32 127.0 . . ? N31 C33 C32 107.0(3) . . ? N31 C33 H33 126.5 . . ? C32 C33 H33 126.5 . . ? C31 C34 C35 109.5(3) . . ? C31 C34 C37 109.5(2) . . ? C35 C34 C37 109.1(3) . . ? C31 C34 C36 109.3(2) . . ? C35 C34 C36 108.6(3) . . ? C37 C34 C36 110.9(3) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N41 C41 C42 179.3(3) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? F4 P2 F3 180.000(1) . . ? F4 P2 F2 91.32(14) . . ? F3 P2 F2 88.67(14) . . ? F4 P2 F2 91.32(14) . 2_665 ? F3 P2 F2 88.68(14) . 2_665 ? F2 P2 F2 177.4(3) . 2_665 ? F4 P2 F1 90.55(9) . 2_665 ? F3 P2 F1 89.45(9) . 2_665 ? F2 P2 F1 89.85(14) . 2_665 ? F2 P2 F1 90.12(14) 2_665 2_665 ? F4 P2 F1 90.55(9) . . ? F3 P2 F1 89.45(9) . . ? F2 P2 F1 90.12(14) . . ? F2 P2 F1 89.85(14) 2_665 . ? F1 P2 F1 178.90(18) 2_665 . ? F6 P3 F6 177.1(8) 2_565 . ? F6 P3 F8 91.5(4) 2_565 . ? F6 P3 F8 91.5(4) . . ? F6 P3 F7 88.5(4) 2_565 . ? F6 P3 F7 88.5(4) . . ? F8 P3 F7 180.000(2) . . ? F6 P3 F5 90.3(5) 2_565 2_565 ? F6 P3 F5 89.6(5) . 2_565 ? F8 P3 F5 90.5(3) . 2_565 ? F7 P3 F5 89.5(3) . 2_565 ? F6 P3 F5 89.6(5) 2_565 . ? F6 P3 F5 90.3(5) . . ? F8 P3 F5 90.5(3) . . ? F7 P3 F5 89.5(3) . . ? F5 P3 F5 178.9(5) 2_565 . ? Cl2 C51 Cl1 109.8(3) . . ? Cl2 C51 H51A 109.7 . . ? Cl1 C51 H51A 109.7 . . ? Cl2 C51 H51B 109.7 . . ? Cl1 C51 H51B 109.7 . . ? H51A C51 H51B 108.2 . . ? 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 O1 P1 N11 C13 -2.0(3) . . . . ? N21 P1 N11 C13 122.0(2) . . . . ? N31 P1 N11 C13 -127.1(2) . . . . ? O1 P1 N11 N12 -179.85(19) . . . . ? N21 P1 N11 N12 -55.8(2) . . . . ? N31 P1 N11 N12 55.1(2) . . . . ? C13 N11 N12 C11 0.4(3) . . . . ? P1 N11 N12 C11 178.44(18) . . . . ? C13 N11 N12 Cu1 -179.13(17) . . . . ? P1 N11 N12 Cu1 -1.0(3) . . . . ? N41 Cu1 N12 C11 0.4(3) . . . . ? N32 Cu1 N12 C11 135.7(3) . . . . ? N22 Cu1 N12 C11 -130.0(3) . . . . ? N41 Cu1 N12 N11 179.63(16) . . . . ? N32 Cu1 N12 N11 -45.06(17) . . . . ? N22 Cu1 N12 N11 49.20(17) . . . . ? O1 P1 N21 C23 -1.4(3) . . . . ? N31 P1 N21 C23 122.7(2) . . . . ? N11 P1 N21 C23 -125.5(2) . . . . ? O1 P1 N21 N22 175.27(18) . . . . ? N31 P1 N21 N22 -60.6(2) . . . . ? N11 P1 N21 N22 51.1(2) . . . . ? C23 N21 N22 C21 0.3(3) . . . . ? P1 N21 N22 C21 -176.77(18) . . . . ? C23 N21 N22 Cu1 -176.04(16) . . . . ? P1 N21 N22 Cu1 6.8(2) . . . . ? N41 Cu1 N22 C21 0.2(3) . . . . ? N12 Cu1 N22 C21 133.1(3) . . . . ? N32 Cu1 N22 C21 -133.0(3) . . . . ? N41 Cu1 N22 N21 174.56(15) . . . . ? N12 Cu1 N22 N21 -52.52(16) . . . . ? N32 Cu1 N22 N21 41.41(17) . . . . ? O1 P1 N31 C33 5.9(3) . . . . ? N21 P1 N31 C33 -118.1(2) . . . . ? N11 P1 N31 C33 131.0(2) . . . . ? O1 P1 N31 N32 -178.67(19) . . . . ? N21 P1 N31 N32 57.3(2) . . . . ? N11 P1 N31 N32 -53.6(2) . . . . ? C33 N31 N32 C31 -0.9(3) . . . . ? P1 N31 N32 C31 -177.02(18) . . . . ? C33 N31 N32 Cu1 175.11(18) . . . . ? P1 N31 N32 Cu1 -1.0(3) . . . . ? N41 Cu1 N32 C31 -3.0(3) . . . . ? N12 Cu1 N32 C31 -139.9(3) . . . . ? N22 Cu1 N32 C31 129.6(3) . . . . ? N41 Cu1 N32 N31 -176.94(16) . . . . ? N12 Cu1 N32 N31 46.11(17) . . . . ? N22 Cu1 N32 N31 -44.34(17) . . . . ? N11 N12 C11 C12 -0.3(3) . . . . ? Cu1 N12 C11 C12 178.9(2) . . . . ? N11 N12 C11 C14 176.3(2) . . . . ? Cu1 N12 C11 C14 -4.4(4) . . . . ? N12 C11 C12 C13 0.2(3) . . . . ? C14 C11 C12 C13 -176.1(3) . . . . ? C11 C12 C13 N11 0.0(3) . . . . ? N12 N11 C13 C12 -0.2(3) . . . . ? P1 N11 C13 C12 -178.2(2) . . . . ? N12 C11 C14 C17 -64.2(3) . . . . ? C12 C11 C14 C17 111.8(3) . . . . ? N12 C11 C14 C16 56.8(3) . . . . ? C12 C11 C14 C16 -127.2(3) . . . . ? N12 C11 C14 C15 176.3(2) . . . . ? C12 C11 C14 C15 -7.7(4) . . . . ? N21 N22 C21 C22 -0.2(3) . . . . ? Cu1 N22 C21 C22 174.4(2) . . . . ? N21 N22 C21 C24 178.6(2) . . . . ? Cu1 N22 C21 C24 -6.8(4) . . . . ? N22 C21 C22 C23 0.0(3) . . . . ? C24 C21 C22 C23 -178.7(3) . . . . ? C21 C22 C23 N21 0.2(3) . . . . ? N22 N21 C23 C22 -0.3(3) . . . . ? P1 N21 C23 C22 176.63(19) . . . . ? N22 C21 C24 C25 -177.4(3) . . . . ? C22 C21 C24 C25 1.1(4) . . . . ? N22 C21 C24 C27 -56.9(4) . . . . ? C22 C21 C24 C27 121.7(3) . . . . ? N22 C21 C24 C26 62.4(4) . . . . ? C22 C21 C24 C26 -119.0(3) . . . . ? N31 N32 C31 C32 0.9(3) . . . . ? Cu1 N32 C31 C32 -173.4(2) . . . . ? N31 N32 C31 C34 -179.6(2) . . . . ? Cu1 N32 C31 C34 6.1(4) . . . . ? N32 C31 C32 C33 -0.6(3) . . . . ? C34 C31 C32 C33 -180.0(3) . . . . ? N32 N31 C33 C32 0.6(3) . . . . ? P1 N31 C33 C32 176.5(2) . . . . ? C31 C32 C33 N31 0.0(3) . . . . ? N32 C31 C34 C35 175.2(3) . . . . ? C32 C31 C34 C35 -5.5(4) . . . . ? N32 C31 C34 C37 -65.3(3) . . . . ? C32 C31 C34 C37 114.1(3) . . . . ? N32 C31 C34 C36 56.4(3) . . . . ? C32 C31 C34 C36 -124.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.686 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.061 #===END data_l0123a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H30 Cu N7 O P, F6 P' _chemical_formula_sum 'C32 H30 Cu F6 N7 O P2' _chemical_formula_weight 768.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.6120(3) _cell_length_b 23.4829(9) _cell_length_c 17.3556(6) _cell_angle_alpha 90.00 _cell_angle_beta 109.357(2) _cell_angle_gamma 90.00 _cell_volume 3311.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9757 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 27.51 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 0.829 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.6759 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'SADABS-2008/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa ApexII' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57072 _diffrn_reflns_av_R_equivalents 0.0160 _diffrn_reflns_av_sigmaI/netI 0.0097 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.53 _reflns_number_total 7613 _reflns_number_gt 6889 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Apex2' _computing_cell_refinement 'SAINT V7.68A' _computing_data_reduction 'SAINT V7.68A, Sadabs' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+2.5110P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7613 _refine_ls_number_parameters 468 _refine_ls_number_restraints 81 _refine_ls_R_factor_all 0.0337 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0795 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.73632(2) 0.259250(8) 0.237570(12) 0.02197(6) Uani 1 1 d . . . P1 P 0.84279(5) 0.390124(16) 0.26481(2) 0.02038(9) Uani 1 1 d . . . O1 O 0.89142(15) 0.44953(5) 0.27599(8) 0.0273(3) Uani 1 1 d . . . N11 N 0.66990(17) 0.37872(6) 0.18528(8) 0.0228(3) Uani 1 1 d . . . N12 N 0.62143(16) 0.32387(6) 0.15785(8) 0.0217(3) Uani 1 1 d . . . N21 N 0.80343(17) 0.36205(6) 0.34546(8) 0.0222(3) Uani 1 1 d . . . N22 N 0.73994(17) 0.30704(6) 0.33905(8) 0.0215(3) Uani 1 1 d . . . N31 N 0.98767(16) 0.34800(5) 0.24838(8) 0.0208(3) Uani 1 1 d . . . N32 N 0.96728(16) 0.28905(5) 0.24370(8) 0.0206(3) Uani 1 1 d . . . N41 N 0.68646(18) 0.18074(6) 0.22905(9) 0.0253(3) Uani 1 1 d . . . C11 C 0.48163(19) 0.33015(7) 0.09617(9) 0.0216(3) Uani 1 1 d . . . C12 C 0.4356(2) 0.38819(7) 0.08504(10) 0.0265(3) Uani 1 1 d . . . H12 H 0.3391 0.4032 0.0459 0.032 Uiso 1 1 calc R . . C13 C 0.5553(2) 0.41842(7) 0.14091(10) 0.0251(3) Uani 1 1 d . . . C14 C 0.39926(19) 0.28118(7) 0.04676(9) 0.0229(3) Uani 1 1 d . . . C15 C 0.4836(2) 0.23039(7) 0.04761(10) 0.0252(3) Uani 1 1 d . . . H15 H 0.5953 0.2271 0.0815 0.030 Uiso 1 1 calc R . . C16 C 0.4063(2) 0.18460(8) -0.00036(11) 0.0313(4) Uani 1 1 d . . . H16 H 0.4642 0.1500 0.0011 0.038 Uiso 1 1 calc R . . C17 C 0.2433(2) 0.18987(9) -0.05058(11) 0.0370(4) Uani 1 1 d . . . H17 H 0.1896 0.1587 -0.0836 0.044 Uiso 1 1 calc R . . C18 C 0.1593(2) 0.24017(10) -0.05262(11) 0.0368(4) Uani 1 1 d . . . H18 H 0.0482 0.2435 -0.0874 0.044 Uiso 1 1 calc R . . C19 C 0.2354(2) 0.28592(9) -0.00429(10) 0.0301(4) Uani 1 1 d . . . H19 H 0.1765 0.3204 -0.0058 0.036 Uiso 1 1 calc R . . C110 C 0.5727(3) 0.48127(8) 0.15366(14) 0.0385(4) Uani 1 1 d . . . H11A H 0.6675 0.4948 0.1395 0.058 Uiso 1 1 calc R . . H11B H 0.5893 0.4901 0.2110 0.058 Uiso 1 1 calc R . . H11C H 0.4727 0.5002 0.1188 0.058 Uiso 1 1 calc R . . C21 C 0.74667(19) 0.29316(7) 0.41406(10) 0.0220(3) Uani 1 1 d . . . C22 C 0.8136(2) 0.33812(7) 0.46939(10) 0.0257(3) Uani 1 1 d . . . H22 H 0.8301 0.3382 0.5263 0.031 Uiso 1 1 calc R . . C23 C 0.8499(2) 0.38115(7) 0.42581(10) 0.0241(3) Uani 1 1 d . . . C24 C 0.7016(2) 0.23525(7) 0.43083(10) 0.0229(3) Uani 1 1 d . . . C25 C 0.5617(2) 0.20842(8) 0.37910(11) 0.0281(3) Uani 1 1 d . . . H25 H 0.4880 0.2286 0.3344 0.034 Uiso 1 1 calc R . . C26 C 0.5305(2) 0.15212(8) 0.39319(12) 0.0348(4) Uani 1 1 d . . . H26 H 0.4343 0.1338 0.3584 0.042 Uiso 1 1 calc R . . C27 C 0.6387(3) 0.12249(8) 0.45762(13) 0.0363(4) Uani 1 1 d . . . H27 H 0.6186 0.0836 0.4657 0.044 Uiso 1 1 calc R . . C28 C 0.7764(2) 0.14923(8) 0.51039(12) 0.0330(4) Uani 1 1 d . . . H28 H 0.8495 0.1289 0.5551 0.040 Uiso 1 1 calc R . . C29 C 0.8070(2) 0.20580(8) 0.49763(10) 0.0269(3) Uani 1 1 d . . . H29 H 0.8999 0.2246 0.5344 0.032 Uiso 1 1 calc R . . C210 C 0.9210(2) 0.43855(8) 0.45315(11) 0.0322(4) Uani 1 1 d . . . H21A H 0.9412 0.4427 0.5119 0.048 Uiso 1 1 calc R . . H21B H 0.8436 0.4680 0.4234 0.048 Uiso 1 1 calc R . . H21C H 1.0250 0.4427 0.4422 0.048 Uiso 1 1 calc R . . C31 C 1.0974(2) 0.26913(7) 0.22751(9) 0.0215(3) Uani 1 1 d . . . C32 C 1.2011(2) 0.31411(7) 0.22083(11) 0.0265(3) Uani 1 1 d . . . H32 H 1.3008 0.3105 0.2091 0.032 Uiso 1 1 calc R . . C33 C 1.1318(2) 0.36352(7) 0.23439(10) 0.0242(3) Uani 1 1 d . . . C34 C 1.12012(19) 0.20734(7) 0.21853(10) 0.0225(3) Uani 1 1 d . . . C35 C 1.0732(2) 0.16759(7) 0.26642(11) 0.0271(3) Uani 1 1 d . . . H35 H 1.0282 0.1801 0.3066 0.033 Uiso 1 1 calc R . . C36 C 1.0922(2) 0.10978(8) 0.25552(12) 0.0327(4) Uani 1 1 d . . . H36 H 1.0602 0.0829 0.2883 0.039 Uiso 1 1 calc R . . C37 C 1.1576(2) 0.09116(8) 0.19699(12) 0.0338(4) Uani 1 1 d . . . H37 H 1.1679 0.0515 0.1887 0.041 Uiso 1 1 calc R . . C38 C 1.2079(2) 0.13029(8) 0.15065(12) 0.0338(4) Uani 1 1 d . . . H38 H 1.2548 0.1175 0.1113 0.041 Uiso 1 1 calc R . . C39 C 1.1902(2) 0.18826(7) 0.16146(11) 0.0281(3) Uani 1 1 d . . . H39 H 1.2259 0.2150 0.1298 0.034 Uiso 1 1 calc R . . C310 C 1.1927(2) 0.42328(8) 0.23773(13) 0.0346(4) Uani 1 1 d . . . H31A H 1.2936 0.4239 0.2233 0.052 Uiso 1 1 calc R . . H31B H 1.2161 0.4384 0.2931 0.052 Uiso 1 1 calc R . . H31C H 1.1086 0.4468 0.1990 0.052 Uiso 1 1 calc R . . C41 C 0.6691(2) 0.13269(7) 0.22919(10) 0.0279(3) Uani 1 1 d . . . C42 C 0.6521(3) 0.07117(8) 0.23177(14) 0.0437(5) Uani 1 1 d . . . H42A H 0.7098 0.0532 0.1980 0.066 Uiso 1 1 calc R . . H42B H 0.5352 0.0610 0.2107 0.066 Uiso 1 1 calc R . . H42C H 0.6998 0.0579 0.2883 0.066 Uiso 1 1 calc R . . P2 P 0.5000 0.5000 0.5000 0.03681(16) Uani 1 2 d SD . . F1 F 0.3664(2) 0.54638(8) 0.45623(10) 0.0744(5) Uani 1 1 d D A . F2A F 0.5255(10) 0.4851(4) 0.4164(3) 0.100(3) Uani 0.485(13) 1 d PDU A 1 F3A F 0.3471(5) 0.45866(18) 0.4777(8) 0.105(4) Uani 0.485(13) 1 d PDU A 1 F2B F 0.4601(11) 0.4602(2) 0.4247(3) 0.104(3) Uani 0.515(13) 1 d PDU A 2 F3B F 0.3883(8) 0.4644(2) 0.5374(5) 0.078(2) Uani 0.515(13) 1 d PDU A 2 P3 P 0.0000 0.0000 0.5000 0.03347(15) Uani 1 2 d SD . . F4 F 0.1108(2) -0.01501(7) 0.44575(11) 0.0718(5) Uani 1 1 d D . . F5 F 0.1511(2) -0.01482(8) 0.57888(10) 0.0788(6) Uani 1 1 d D . . F6 F 0.05700(18) 0.06416(6) 0.50660(15) 0.0850(7) 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 Cu1 0.02418(11) 0.01603(10) 0.02316(11) -0.00104(7) 0.00443(8) -0.00177(7) P1 0.02182(19) 0.01418(18) 0.02263(19) -0.00028(14) 0.00398(15) 0.00025(14) O1 0.0309(6) 0.0158(5) 0.0328(6) -0.0010(5) 0.0076(5) -0.0010(5) N11 0.0226(6) 0.0165(6) 0.0249(7) 0.0004(5) 0.0019(5) 0.0019(5) N12 0.0218(6) 0.0186(6) 0.0216(6) -0.0006(5) 0.0031(5) -0.0013(5) N21 0.0261(7) 0.0166(6) 0.0224(6) -0.0030(5) 0.0060(5) -0.0027(5) N22 0.0235(6) 0.0169(6) 0.0230(6) -0.0021(5) 0.0061(5) -0.0023(5) N31 0.0207(6) 0.0150(6) 0.0247(6) 0.0010(5) 0.0048(5) -0.0008(5) N32 0.0210(6) 0.0138(6) 0.0243(6) 0.0007(5) 0.0041(5) 0.0003(5) N41 0.0276(7) 0.0219(7) 0.0253(7) -0.0015(5) 0.0073(6) -0.0025(6) C11 0.0183(7) 0.0264(8) 0.0201(7) 0.0028(6) 0.0065(6) 0.0008(6) C12 0.0204(7) 0.0301(9) 0.0275(8) 0.0047(7) 0.0062(6) 0.0058(6) C13 0.0230(8) 0.0241(8) 0.0277(8) 0.0034(6) 0.0079(6) 0.0073(6) C14 0.0200(7) 0.0304(8) 0.0176(7) 0.0022(6) 0.0050(6) -0.0046(6) C15 0.0236(8) 0.0309(8) 0.0202(7) -0.0007(6) 0.0059(6) -0.0056(6) C16 0.0349(9) 0.0334(9) 0.0267(8) -0.0047(7) 0.0118(7) -0.0097(7) C17 0.0365(10) 0.0485(12) 0.0244(9) -0.0090(8) 0.0079(7) -0.0209(9) C18 0.0232(8) 0.0581(13) 0.0237(8) 0.0015(8) 0.0007(7) -0.0129(8) C19 0.0218(8) 0.0421(10) 0.0238(8) 0.0058(7) 0.0041(6) -0.0037(7) C110 0.0366(10) 0.0224(9) 0.0492(11) 0.0030(8) 0.0042(9) 0.0105(7) C21 0.0188(7) 0.0230(8) 0.0234(7) -0.0023(6) 0.0060(6) 0.0006(6) C22 0.0272(8) 0.0268(8) 0.0220(7) -0.0052(6) 0.0065(6) -0.0015(6) C23 0.0230(8) 0.0231(8) 0.0243(8) -0.0062(6) 0.0053(6) -0.0001(6) C24 0.0244(8) 0.0232(8) 0.0239(8) -0.0022(6) 0.0117(6) -0.0013(6) C25 0.0268(8) 0.0313(9) 0.0270(8) -0.0035(7) 0.0101(7) -0.0046(7) C26 0.0384(10) 0.0331(9) 0.0385(10) -0.0115(8) 0.0202(8) -0.0133(8) C27 0.0539(12) 0.0236(9) 0.0428(11) -0.0040(7) 0.0312(10) -0.0051(8) C28 0.0426(10) 0.0287(9) 0.0332(9) 0.0051(7) 0.0197(8) 0.0052(8) C29 0.0281(8) 0.0284(8) 0.0258(8) -0.0002(7) 0.0110(7) 0.0001(7) C210 0.0392(10) 0.0246(8) 0.0304(9) -0.0097(7) 0.0084(8) -0.0069(7) C31 0.0223(7) 0.0202(7) 0.0202(7) 0.0017(6) 0.0045(6) 0.0009(6) C32 0.0265(8) 0.0236(8) 0.0319(9) 0.0021(7) 0.0128(7) -0.0012(6) C33 0.0247(8) 0.0224(8) 0.0251(8) 0.0023(6) 0.0077(6) -0.0027(6) C34 0.0199(7) 0.0188(7) 0.0256(8) 0.0006(6) 0.0031(6) 0.0015(6) C35 0.0258(8) 0.0229(8) 0.0327(9) 0.0023(7) 0.0098(7) 0.0017(6) C36 0.0301(9) 0.0220(8) 0.0440(10) 0.0068(7) 0.0097(8) -0.0001(7) C37 0.0332(9) 0.0191(8) 0.0434(10) -0.0024(7) 0.0049(8) 0.0040(7) C38 0.0372(10) 0.0287(9) 0.0347(9) -0.0046(7) 0.0107(8) 0.0067(8) C39 0.0308(9) 0.0243(8) 0.0296(8) 0.0021(7) 0.0105(7) 0.0031(7) C310 0.0370(10) 0.0219(8) 0.0500(11) 0.0004(8) 0.0212(9) -0.0062(7) C41 0.0317(9) 0.0244(9) 0.0269(8) -0.0005(6) 0.0089(7) -0.0032(7) C42 0.0586(13) 0.0195(9) 0.0501(12) 0.0010(8) 0.0141(10) -0.0072(9) P2 0.0363(4) 0.0323(4) 0.0400(4) 0.0031(3) 0.0102(3) 0.0044(3) F1 0.0731(11) 0.0836(12) 0.0689(10) 0.0286(9) 0.0266(9) 0.0443(9) F2A 0.117(5) 0.133(7) 0.058(2) 0.027(3) 0.038(3) 0.091(5) F3A 0.043(2) 0.049(2) 0.194(10) 0.000(3) 0.002(3) -0.0090(16) F2B 0.172(6) 0.073(3) 0.051(3) -0.025(2) 0.017(3) -0.005(4) F3B 0.058(3) 0.079(3) 0.110(5) 0.042(3) 0.044(3) 0.003(2) P3 0.0216(3) 0.0304(3) 0.0422(4) -0.0070(3) 0.0023(3) -0.0008(2) F4 0.0732(10) 0.0722(11) 0.0865(12) 0.0155(9) 0.0485(10) 0.0304(9) F5 0.0635(10) 0.0929(13) 0.0542(9) -0.0187(9) -0.0149(8) 0.0401(9) F6 0.0423(8) 0.0321(7) 0.177(2) -0.0140(10) 0.0310(10) -0.0057(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N41 1.8876(14) . ? Cu1 N12 2.0710(13) . ? Cu1 N32 2.0778(13) . ? Cu1 N22 2.0799(13) . ? P1 O1 1.4509(12) . ? P1 N21 1.6801(14) . ? P1 N11 1.6828(14) . ? P1 N31 1.6889(14) . ? N11 N12 1.3884(18) . ? N11 C13 1.390(2) . ? N12 C11 1.328(2) . ? N21 C23 1.391(2) . ? N21 N22 1.3928(18) . ? N22 C21 1.325(2) . ? N31 C33 1.390(2) . ? N31 N32 1.3944(17) . ? N32 C31 1.328(2) . ? N41 C41 1.138(2) . ? C11 C12 1.415(2) . ? C11 C14 1.469(2) . ? C12 C13 1.358(2) . ? C12 H12 0.9500 . ? C13 C110 1.493(2) . ? C14 C15 1.394(2) . ? C14 C19 1.400(2) . ? C15 C16 1.387(2) . ? C15 H15 0.9500 . ? C16 C17 1.391(3) . ? C16 H16 0.9500 . ? C17 C18 1.380(3) . ? C17 H17 0.9500 . ? C18 C19 1.387(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C110 H11A 0.9800 . ? C110 H11B 0.9800 . ? C110 H11C 0.9800 . ? C21 C22 1.415(2) . ? C21 C24 1.470(2) . ? C22 C23 1.359(2) . ? C22 H22 0.9500 . ? C23 C210 1.492(2) . ? C24 C25 1.392(2) . ? C24 C29 1.396(2) . ? C25 C26 1.387(3) . ? C25 H25 0.9500 . ? C26 C27 1.383(3) . ? C26 H26 0.9500 . ? C27 C28 1.385(3) . ? C27 H27 0.9500 . ? C28 C29 1.386(3) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C210 H21A 0.9800 . ? C210 H21B 0.9800 . ? C210 H21C 0.9800 . ? C31 C32 1.412(2) . ? C31 C34 1.479(2) . ? C32 C33 1.361(2) . ? C32 H32 0.9500 . ? C33 C310 1.493(2) . ? C34 C39 1.394(2) . ? C34 C35 1.396(2) . ? C35 C36 1.388(2) . ? C35 H35 0.9500 . ? C36 C37 1.386(3) . ? C36 H36 0.9500 . ? C37 C38 1.382(3) . ? C37 H37 0.9500 . ? C38 C39 1.390(2) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C310 H31A 0.9800 . ? C310 H31B 0.9800 . ? C310 H31C 0.9800 . ? C41 C42 1.454(2) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? P2 F2B 1.549(4) 3_666 ? P2 F2B 1.549(4) . ? P2 F3B 1.569(3) . ? P2 F3B 1.569(3) 3_666 ? P2 F2A 1.577(4) 3_666 ? P2 F2A 1.577(4) . ? P2 F3A 1.577(3) . ? P2 F3A 1.577(3) 3_666 ? P2 F1 1.5836(14) 3_666 ? P2 F1 1.5837(14) . ? P3 F6 1.5769(14) 3_556 ? P3 F6 1.5769(14) . ? P3 F5 1.5836(14) . ? P3 F5 1.5836(14) 3_556 ? P3 F4 1.5863(14) . ? P3 F4 1.5863(14) 3_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N41 Cu1 N12 128.13(6) . . ? N41 Cu1 N32 121.47(6) . . ? N12 Cu1 N32 91.41(5) . . ? N41 Cu1 N22 122.17(6) . . ? N12 Cu1 N22 92.30(5) . . ? N32 Cu1 N22 91.69(5) . . ? O1 P1 N21 113.26(7) . . ? O1 P1 N11 113.61(7) . . ? N21 P1 N11 104.65(7) . . ? O1 P1 N31 112.89(7) . . ? N21 P1 N31 105.98(7) . . ? N11 P1 N31 105.70(7) . . ? N12 N11 C13 110.78(13) . . ? N12 N11 P1 120.84(10) . . ? C13 N11 P1 128.33(12) . . ? C11 N12 N11 105.23(13) . . ? C11 N12 Cu1 136.45(11) . . ? N11 N12 Cu1 115.33(9) . . ? C23 N21 N22 110.72(13) . . ? C23 N21 P1 129.66(12) . . ? N22 N21 P1 118.66(10) . . ? C21 N22 N21 105.17(13) . . ? C21 N22 Cu1 133.08(11) . . ? N21 N22 Cu1 117.61(10) . . ? C33 N31 N32 110.64(13) . . ? C33 N31 P1 128.94(11) . . ? N32 N31 P1 120.36(10) . . ? C31 N32 N31 105.27(13) . . ? C31 N32 Cu1 137.01(11) . . ? N31 N32 Cu1 115.93(9) . . ? C41 N41 Cu1 174.03(15) . . ? N12 C11 C12 110.80(14) . . ? N12 C11 C14 121.14(15) . . ? C12 C11 C14 127.97(15) . . ? C13 C12 C11 107.10(14) . . ? C13 C12 H12 126.4 . . ? C11 C12 H12 126.4 . . ? C12 C13 N11 106.05(14) . . ? C12 C13 C110 129.62(16) . . ? N11 C13 C110 124.29(15) . . ? C15 C14 C19 119.14(16) . . ? C15 C14 C11 120.97(14) . . ? C19 C14 C11 119.85(16) . . ? C16 C15 C14 120.82(16) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 119.39(19) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C18 C17 C16 120.28(17) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 120.60(17) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C18 C19 C14 119.76(18) . . ? C18 C19 H19 120.1 . . ? C14 C19 H19 120.1 . . ? C13 C110 H11A 109.5 . . ? C13 C110 H11B 109.5 . . ? H11A C110 H11B 109.5 . . ? C13 C110 H11C 109.5 . . ? H11A C110 H11C 109.5 . . ? H11B C110 H11C 109.5 . . ? N22 C21 C22 111.02(14) . . ? N22 C21 C24 119.61(14) . . ? C22 C21 C24 129.12(15) . . ? C23 C22 C21 107.11(15) . . ? C23 C22 H22 126.4 . . ? C21 C22 H22 126.4 . . ? C22 C23 N21 105.99(14) . . ? C22 C23 C210 129.86(16) . . ? N21 C23 C210 124.15(15) . . ? C25 C24 C29 119.82(16) . . ? C25 C24 C21 121.34(15) . . ? C29 C24 C21 118.74(15) . . ? C26 C25 C24 119.66(17) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C27 C26 C25 120.25(18) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 120.43(17) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C27 C28 C29 119.67(18) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C28 C29 C24 120.10(17) . . ? C28 C29 H29 120.0 . . ? C24 C29 H29 120.0 . . ? C23 C210 H21A 109.5 . . ? C23 C210 H21B 109.5 . . ? H21A C210 H21B 109.5 . . ? C23 C210 H21C 109.5 . . ? H21A C210 H21C 109.5 . . ? H21B C210 H21C 109.5 . . ? N32 C31 C32 110.78(14) . . ? N32 C31 C34 121.22(14) . . ? C32 C31 C34 128.00(15) . . ? C33 C32 C31 107.33(15) . . ? C33 C32 H32 126.3 . . ? C31 C32 H32 126.3 . . ? C32 C33 N31 105.97(14) . . ? C32 C33 C310 129.75(16) . . ? N31 C33 C310 124.24(15) . . ? C39 C34 C35 119.16(15) . . ? C39 C34 C31 119.59(15) . . ? C35 C34 C31 121.25(15) . . ? C36 C35 C34 120.18(17) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C37 C36 C35 120.23(17) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C38 C37 C36 119.94(17) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C39 120.20(18) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C38 C39 C34 120.26(17) . . ? C38 C39 H39 119.9 . . ? C34 C39 H39 119.9 . . ? C33 C310 H31A 109.5 . . ? C33 C310 H31B 109.5 . . ? H31A C310 H31B 109.5 . . ? C33 C310 H31C 109.5 . . ? H31A C310 H31C 109.5 . . ? H31B C310 H31C 109.5 . . ? N41 C41 C42 178.1(2) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? F2B P2 F2B 179.997(3) 3_666 . ? F2B P2 F3B 88.1(3) 3_666 . ? F2B P2 F3B 91.9(3) . . ? F2B P2 F3B 91.9(3) 3_666 3_666 ? F2B P2 F3B 88.1(3) . 3_666 ? F3B P2 F3B 180.0(5) . 3_666 ? F2A P2 F2A 179.997(3) 3_666 . ? F2A P2 F3A 90.2(3) 3_666 . ? F2A P2 F3A 89.8(3) . . ? F2A P2 F3A 89.8(3) 3_666 3_666 ? F2A P2 F3A 90.2(3) . 3_666 ? F3A P2 F3A 179.999(1) . 3_666 ? F2B P2 F1 95.0(2) 3_666 3_666 ? F2B P2 F1 85.0(2) . 3_666 ? F3B P2 F1 83.28(19) . 3_666 ? F3B P2 F1 96.72(19) 3_666 3_666 ? F2A P2 F1 90.70(18) 3_666 3_666 ? F2A P2 F1 89.31(18) . 3_666 ? F3A P2 F1 96.3(2) . 3_666 ? F3A P2 F1 83.7(2) 3_666 3_666 ? F2B P2 F1 85.0(2) 3_666 . ? F2B P2 F1 95.0(2) . . ? F3B P2 F1 96.72(19) . . ? F3B P2 F1 83.28(19) 3_666 . ? F2A P2 F1 89.30(18) 3_666 . ? F2A P2 F1 90.69(18) . . ? F3A P2 F1 83.7(2) . . ? F3A P2 F1 96.3(2) 3_666 . ? F1 P2 F1 179.999(2) 3_666 . ? F6 P3 F6 180.0 3_556 . ? F6 P3 F5 89.98(10) 3_556 . ? F6 P3 F5 90.02(10) . . ? F6 P3 F5 90.02(10) 3_556 3_556 ? F6 P3 F5 89.98(10) . 3_556 ? F5 P3 F5 180.0 . 3_556 ? F6 P3 F4 88.77(10) 3_556 . ? F6 P3 F4 91.23(10) . . ? F5 P3 F4 88.90(9) . . ? F5 P3 F4 91.10(9) 3_556 . ? F6 P3 F4 91.23(10) 3_556 3_556 ? F6 P3 F4 88.77(10) . 3_556 ? F5 P3 F4 91.10(9) . 3_556 ? F5 P3 F4 88.90(9) 3_556 3_556 ? F4 P3 F4 180.0 . 3_556 ? 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 O1 P1 N11 N12 169.28(12) . . . . ? N21 P1 N11 N12 -66.69(13) . . . . ? N31 P1 N11 N12 44.96(14) . . . . ? O1 P1 N11 C13 -13.54(17) . . . . ? N21 P1 N11 C13 110.50(15) . . . . ? N31 P1 N11 C13 -137.85(14) . . . . ? C13 N11 N12 C11 1.64(17) . . . . ? P1 N11 N12 C11 179.28(11) . . . . ? C13 N11 N12 Cu1 -162.09(11) . . . . ? P1 N11 N12 Cu1 15.55(16) . . . . ? N41 Cu1 N12 C11 14.71(19) . . . . ? N32 Cu1 N12 C11 147.80(16) . . . . ? N22 Cu1 N12 C11 -120.45(16) . . . . ? N41 Cu1 N12 N11 171.61(10) . . . . ? N32 Cu1 N12 N11 -55.30(11) . . . . ? N22 Cu1 N12 N11 36.45(11) . . . . ? O1 P1 N21 C23 -18.66(17) . . . . ? N11 P1 N21 C23 -142.91(14) . . . . ? N31 P1 N21 C23 105.63(15) . . . . ? O1 P1 N21 N22 173.72(11) . . . . ? N11 P1 N21 N22 49.47(13) . . . . ? N31 P1 N21 N22 -61.99(13) . . . . ? C23 N21 N22 C21 0.40(17) . . . . ? P1 N21 N22 C21 170.24(11) . . . . ? C23 N21 N22 Cu1 -159.69(11) . . . . ? P1 N21 N22 Cu1 10.14(15) . . . . ? N41 Cu1 N22 C21 16.65(18) . . . . ? N12 Cu1 N22 C21 155.70(15) . . . . ? N32 Cu1 N22 C21 -112.82(15) . . . . ? N41 Cu1 N22 N21 169.92(10) . . . . ? N12 Cu1 N22 N21 -51.03(11) . . . . ? N32 Cu1 N22 N21 40.45(11) . . . . ? O1 P1 N31 C33 -8.88(17) . . . . ? N21 P1 N31 C33 -133.40(14) . . . . ? N11 P1 N31 C33 115.88(14) . . . . ? O1 P1 N31 N32 174.23(11) . . . . ? N21 P1 N31 N32 49.72(13) . . . . ? N11 P1 N31 N32 -61.00(13) . . . . ? C33 N31 N32 C31 0.28(17) . . . . ? P1 N31 N32 C31 177.70(11) . . . . ? C33 N31 N32 Cu1 -167.08(10) . . . . ? P1 N31 N32 Cu1 10.33(15) . . . . ? N41 Cu1 N32 C31 16.91(18) . . . . ? N12 Cu1 N32 C31 -120.76(16) . . . . ? N22 Cu1 N32 C31 146.90(16) . . . . ? N41 Cu1 N32 N31 178.89(10) . . . . ? N12 Cu1 N32 N31 41.22(11) . . . . ? N22 Cu1 N32 N31 -51.12(11) . . . . ? N11 N12 C11 C12 -2.09(17) . . . . ? Cu1 N12 C11 C12 156.35(13) . . . . ? N11 N12 C11 C14 174.93(14) . . . . ? Cu1 N12 C11 C14 -26.6(2) . . . . ? N12 C11 C12 C13 1.83(19) . . . . ? C14 C11 C12 C13 -174.94(15) . . . . ? C11 C12 C13 N11 -0.72(18) . . . . ? C11 C12 C13 C110 176.97(18) . . . . ? N12 N11 C13 C12 -0.54(18) . . . . ? P1 N11 C13 C12 -177.96(13) . . . . ? N12 N11 C13 C110 -178.39(17) . . . . ? P1 N11 C13 C110 4.2(3) . . . . ? N12 C11 C14 C15 -17.6(2) . . . . ? C12 C11 C14 C15 158.91(16) . . . . ? N12 C11 C14 C19 164.72(15) . . . . ? C12 C11 C14 C19 -18.8(2) . . . . ? C19 C14 C15 C16 -1.0(2) . . . . ? C11 C14 C15 C16 -178.72(15) . . . . ? C14 C15 C16 C17 0.8(3) . . . . ? C15 C16 C17 C18 0.0(3) . . . . ? C16 C17 C18 C19 -0.5(3) . . . . ? C17 C18 C19 C14 0.3(3) . . . . ? C15 C14 C19 C18 0.4(2) . . . . ? C11 C14 C19 C18 178.18(15) . . . . ? N21 N22 C21 C22 -0.05(18) . . . . ? Cu1 N22 C21 C22 155.56(12) . . . . ? N21 N22 C21 C24 -174.80(13) . . . . ? Cu1 N22 C21 C24 -19.2(2) . . . . ? N22 C21 C22 C23 -0.33(19) . . . . ? C24 C21 C22 C23 173.80(16) . . . . ? C21 C22 C23 N21 0.55(18) . . . . ? C21 C22 C23 C210 179.28(17) . . . . ? N22 N21 C23 C22 -0.61(18) . . . . ? P1 N21 C23 C22 -169.00(13) . . . . ? N22 N21 C23 C210 -179.43(15) . . . . ? P1 N21 C23 C210 12.2(2) . . . . ? N22 C21 C24 C25 -44.9(2) . . . . ? C22 C21 C24 C25 141.44(18) . . . . ? N22 C21 C24 C29 131.49(17) . . . . ? C22 C21 C24 C29 -42.2(2) . . . . ? C29 C24 C25 C26 -1.6(2) . . . . ? C21 C24 C25 C26 174.71(15) . . . . ? C24 C25 C26 C27 -0.9(3) . . . . ? C25 C26 C27 C28 2.2(3) . . . . ? C26 C27 C28 C29 -1.0(3) . . . . ? C27 C28 C29 C24 -1.5(3) . . . . ? C25 C24 C29 C28 2.8(2) . . . . ? C21 C24 C29 C28 -173.62(15) . . . . ? N31 N32 C31 C32 -0.55(17) . . . . ? Cu1 N32 C31 C32 162.69(13) . . . . ? N31 N32 C31 C34 179.57(13) . . . . ? Cu1 N32 C31 C34 -17.2(2) . . . . ? N32 C31 C32 C33 0.6(2) . . . . ? C34 C31 C32 C33 -179.50(16) . . . . ? C31 C32 C33 N31 -0.42(19) . . . . ? C31 C32 C33 C310 177.43(18) . . . . ? N32 N31 C33 C32 0.10(18) . . . . ? P1 N31 C33 C32 -177.03(12) . . . . ? N32 N31 C33 C310 -177.91(16) . . . . ? P1 N31 C33 C310 5.0(2) . . . . ? N32 C31 C34 C39 144.12(16) . . . . ? C32 C31 C34 C39 -35.7(2) . . . . ? N32 C31 C34 C35 -36.1(2) . . . . ? C32 C31 C34 C35 144.03(18) . . . . ? C39 C34 C35 C36 -1.8(3) . . . . ? C31 C34 C35 C36 178.47(16) . . . . ? C34 C35 C36 C37 -0.1(3) . . . . ? C35 C36 C37 C38 1.6(3) . . . . ? C36 C37 C38 C39 -1.3(3) . . . . ? C37 C38 C39 C34 -0.6(3) . . . . ? C35 C34 C39 C38 2.1(3) . . . . ? C31 C34 C39 C38 -178.13(16) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.626 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.051 #===END data_s4103a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H36 Cu N6 O P2, P F6, 2(C H2 Cl2)' _chemical_formula_sum 'C35 H40 Cl4 Cu F6 N6 O P3' _chemical_formula_weight 972.98 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0739(3) _cell_length_b 12.6624(3) _cell_length_c 15.9619(2) _cell_angle_alpha 102.223(1) _cell_angle_beta 106.463(1) _cell_angle_gamma 91.278(1) _cell_volume 2089.69(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 17080 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 0.958 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 0.84 _exptl_absorpt_process_details 'Twinabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40560 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0091 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.46 _reflns_number_total 9572 _reflns_number_gt 8587 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Peakref' _computing_data_reduction 'Pixel15, Twinabs' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+1.4923P] 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 9572 _refine_ls_number_parameters 531 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0937 _refine_ls_wR_factor_gt 0.0887 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.186 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.40628(2) 0.73993(2) 0.247508(15) 0.01963(7) Uani 1 1 d . . . P1 P 0.57405(5) 0.74293(4) 0.44991(3) 0.01912(11) Uani 1 1 d . . . P2 P 0.29778(5) 0.74357(4) 0.11089(3) 0.01840(11) Uani 1 1 d . . . O1 O 0.64920(15) 0.74399(14) 0.54085(10) 0.0278(3) Uani 1 1 d . . . N11 N 0.41877(16) 0.71293(14) 0.43154(11) 0.0207(3) Uani 1 1 d . . . N12 N 0.33302(16) 0.71939(14) 0.35045(11) 0.0203(3) Uani 1 1 d . . . N21 N 0.61522(16) 0.65323(14) 0.37179(12) 0.0215(3) Uani 1 1 d . . . N22 N 0.54028(17) 0.63151(15) 0.28249(12) 0.0228(4) Uani 1 1 d . . . N31 N 0.58402(16) 0.86330(14) 0.42300(11) 0.0192(3) Uani 1 1 d . . . N32 N 0.52704(16) 0.87273(14) 0.33562(11) 0.0201(3) Uani 1 1 d . . . C11 C 0.2204(2) 0.69590(17) 0.35883(14) 0.0221(4) Uani 1 1 d . . . C12 C 0.2312(2) 0.67558(18) 0.44373(15) 0.0260(4) Uani 1 1 d . . . H12 H 0.1635 0.6581 0.4654 0.031 Uiso 1 1 calc R . . C13 C 0.3562(2) 0.68557(17) 0.48898(14) 0.0226(4) Uani 1 1 d . . . C14 C 0.1037(2) 0.6893(2) 0.28300(16) 0.0314(5) Uani 1 1 d . . . H14A H 0.1103 0.7474 0.2521 0.047 Uiso 1 1 calc R . . H14B H 0.0304 0.6975 0.3061 0.047 Uiso 1 1 calc R . . H14C H 0.0932 0.6188 0.2408 0.047 Uiso 1 1 calc R . . C15 C 0.4205(2) 0.6711(2) 0.58111(16) 0.0337(5) Uani 1 1 d . . . H15A H 0.3569 0.6583 0.6107 0.051 Uiso 1 1 calc R . . H15B H 0.4757 0.7366 0.6160 0.051 Uiso 1 1 calc R . . H15C H 0.4712 0.6087 0.5771 0.051 Uiso 1 1 calc R . . C21 C 0.5914(2) 0.55202(18) 0.24006(15) 0.0261(4) Uani 1 1 d . . . C22 C 0.6992(2) 0.52276(19) 0.29973(17) 0.0292(5) Uani 1 1 d . . . H22 H 0.7521 0.4684 0.2847 0.035 Uiso 1 1 calc R . . C23 C 0.7136(2) 0.58615(18) 0.38205(16) 0.0259(4) Uani 1 1 d . . . C24 C 0.5355(3) 0.5026(2) 0.14283(17) 0.0393(6) Uani 1 1 d . . . H24A H 0.4555 0.5334 0.1202 0.059 Uiso 1 1 calc R . . H24B H 0.5200 0.4240 0.1340 0.059 Uiso 1 1 calc R . . H24C H 0.5941 0.5180 0.1102 0.059 Uiso 1 1 calc R . . C25 C 0.8111(2) 0.5879(2) 0.46903(18) 0.0373(6) Uani 1 1 d . . . H25A H 0.7707 0.5649 0.5102 0.056 Uiso 1 1 calc R . . H25B H 0.8519 0.6617 0.4954 0.056 Uiso 1 1 calc R . . H25C H 0.8747 0.5384 0.4585 0.056 Uiso 1 1 calc R . . C31 C 0.5619(2) 0.97304(17) 0.33447(14) 0.0227(4) Uani 1 1 d . . . C32 C 0.6401(2) 1.02873(17) 0.41959(15) 0.0261(4) Uani 1 1 d . . . H32 H 0.6765 1.1015 0.4352 0.031 Uiso 1 1 calc R . . C33 C 0.65376(19) 0.95892(17) 0.47500(14) 0.0222(4) Uani 1 1 d . . . C34 C 0.5220(3) 1.0151(2) 0.25152(17) 0.0337(5) Uani 1 1 d . . . H34A H 0.5046 0.9545 0.1989 0.051 Uiso 1 1 calc R . . H34B H 0.5897 1.0657 0.2507 0.051 Uiso 1 1 calc R . . H34C H 0.4455 1.0529 0.2503 0.051 Uiso 1 1 calc R . . C35 C 0.7258(2) 0.9758(2) 0.57182(15) 0.0319(5) Uani 1 1 d . . . H35A H 0.7626 1.0511 0.5948 0.048 Uiso 1 1 calc R . . H35B H 0.7935 0.9269 0.5787 0.048 Uiso 1 1 calc R . . H35C H 0.6687 0.9605 0.6056 0.048 Uiso 1 1 calc R . . C41 C 0.1655(2) 0.82818(17) 0.10410(14) 0.0210(4) Uani 1 1 d . . . C42 C 0.0594(2) 0.81353(19) 0.02938(15) 0.0268(4) Uani 1 1 d . . . H42 H 0.0552 0.7591 -0.0227 0.032 Uiso 1 1 calc R . . C43 C -0.0400(2) 0.8778(2) 0.03056(18) 0.0347(5) Uani 1 1 d . . . H43 H -0.1121 0.8672 -0.0207 0.042 Uiso 1 1 calc R . . C44 C -0.0349(3) 0.9574(2) 0.10592(19) 0.0359(5) Uani 1 1 d . . . H44 H -0.1039 1.0004 0.1068 0.043 Uiso 1 1 calc R . . C45 C 0.0707(3) 0.9743(2) 0.18004(17) 0.0353(5) Uani 1 1 d . . . H45 H 0.0753 1.0300 0.2314 0.042 Uiso 1 1 calc R . . C46 C 0.1699(2) 0.90946(19) 0.17911(15) 0.0289(5) Uani 1 1 d . . . H46 H 0.2419 0.9207 0.2304 0.035 Uiso 1 1 calc R . . C51 C 0.22668(19) 0.61250(17) 0.03838(14) 0.0209(4) Uani 1 1 d . . . C52 C 0.1986(2) 0.5899(2) -0.05515(14) 0.0277(5) Uani 1 1 d . . . H52 H 0.2140 0.6450 -0.0840 0.033 Uiso 1 1 calc R . . C53 C 0.1484(2) 0.4872(2) -0.10570(16) 0.0341(5) Uani 1 1 d . . . H53 H 0.1293 0.4724 -0.1692 0.041 Uiso 1 1 calc R . . C54 C 0.1258(2) 0.4060(2) -0.06453(17) 0.0338(5) Uani 1 1 d . . . H54 H 0.0921 0.3356 -0.0996 0.041 Uiso 1 1 calc R . . C55 C 0.1524(2) 0.4279(2) 0.02778(17) 0.0320(5) Uani 1 1 d . . . H55 H 0.1362 0.3727 0.0562 0.038 Uiso 1 1 calc R . . C56 C 0.2029(2) 0.53062(18) 0.07888(15) 0.0253(4) Uani 1 1 d . . . H56 H 0.2213 0.5451 0.1423 0.030 Uiso 1 1 calc R . . C61 C 0.3918(2) 0.79308(18) 0.04788(14) 0.0234(4) Uani 1 1 d . . . C62 C 0.3425(2) 0.8474(2) -0.01980(17) 0.0376(6) Uani 1 1 d . . . H62 H 0.2564 0.8627 -0.0336 0.045 Uiso 1 1 calc R . . C63 C 0.4186(3) 0.8790(3) -0.0669(2) 0.0532(8) Uani 1 1 d . . . H63 H 0.3844 0.9161 -0.1130 0.064 Uiso 1 1 calc R . . C64 C 0.5430(3) 0.8574(3) -0.0478(2) 0.0571(9) Uani 1 1 d . . . H64 H 0.5945 0.8797 -0.0805 0.068 Uiso 1 1 calc R . . C65 C 0.5937(3) 0.8029(3) 0.0193(2) 0.0504(7) Uani 1 1 d . . . H65 H 0.6797 0.7873 0.0323 0.060 Uiso 1 1 calc R . . C66 C 0.5181(2) 0.7715(2) 0.06730(18) 0.0349(5) Uani 1 1 d . . . H66 H 0.5529 0.7350 0.1137 0.042 Uiso 1 1 calc R . . P3 P 0.88459(6) 0.22732(5) 0.29884(4) 0.03359(15) Uani 1 1 d . . . F1 F 0.9196(2) 0.2331(2) 0.20934(14) 0.0751(7) Uani 1 1 d . . . F2 F 1.02184(15) 0.18965(15) 0.33894(11) 0.0460(4) Uani 1 1 d . . . F3 F 0.8499(2) 0.2137(3) 0.38566(15) 0.0930(9) Uani 1 1 d . . . F4 F 0.74763(17) 0.26469(15) 0.25907(14) 0.0591(5) Uani 1 1 d . . . F5 F 0.83154(18) 0.10469(14) 0.25303(15) 0.0596(5) Uani 1 1 d . . . F6 F 0.9386(2) 0.34797(17) 0.3432(2) 0.1075(12) Uani 1 1 d . . . Cl1 Cl 0.03945(9) 0.14274(6) 0.55437(5) 0.0553(2) Uani 1 1 d D . . Cl2 Cl 0.20328(7) 0.17879(8) 0.73702(6) 0.0615(2) Uani 1 1 d D . . C71 C 0.0948(3) 0.0870(2) 0.64870(18) 0.0419(6) Uani 1 1 d D . . H71A H 0.0224 0.0667 0.6687 0.050 Uiso 1 1 calc R . . H71B H 0.1357 0.0202 0.6321 0.050 Uiso 1 1 calc R . . Cl3A Cl 0.3067(4) 0.2436(3) 0.19769(14) 0.0625(11) Uani 0.544(8) 1 d PDU A 1 Cl4A Cl 0.2688(7) 0.4464(3) 0.3032(3) 0.0901(15) Uani 0.544(8) 1 d PDU A 1 Cl3B Cl 0.2605(4) 0.2134(2) 0.2143(3) 0.0741(9) Uani 0.456(8) 1 d PDU A 2 Cl4B Cl 0.3132(3) 0.4431(3) 0.2890(3) 0.0484(9) Uani 0.456(8) 1 d PDU A 2 C81 C 0.2188(3) 0.3169(2) 0.27204(19) 0.0482(7) Uani 1 1 d D . . H81A H 0.1273 0.3081 0.2398 0.058 Uiso 0.544(8) 1 calc PR A 1 H81B H 0.2317 0.2860 0.3256 0.058 Uiso 0.544(8) 1 calc PR A 1 H81C H 0.2230 0.3030 0.3315 0.058 Uiso 0.456(8) 1 calc PR A 2 H81D H 0.1296 0.3261 0.2420 0.058 Uiso 0.456(8) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02008(13) 0.02276(13) 0.01386(12) 0.00314(9) 0.00235(9) 0.00154(9) P1 0.0191(2) 0.0211(2) 0.0160(2) 0.00549(19) 0.00249(19) 0.00067(19) P2 0.0185(2) 0.0215(2) 0.0133(2) 0.00231(18) 0.00289(18) 0.00009(19) O1 0.0268(8) 0.0353(9) 0.0187(7) 0.0097(6) 0.0001(6) 0.0009(6) N11 0.0206(8) 0.0241(8) 0.0167(8) 0.0064(7) 0.0036(6) -0.0007(7) N12 0.0185(8) 0.0244(9) 0.0165(8) 0.0048(7) 0.0026(6) 0.0010(6) N21 0.0209(8) 0.0213(8) 0.0211(8) 0.0055(7) 0.0034(7) 0.0045(7) N22 0.0222(9) 0.0241(9) 0.0193(8) 0.0015(7) 0.0037(7) 0.0033(7) N31 0.0203(8) 0.0193(8) 0.0152(8) 0.0030(6) 0.0015(6) -0.0011(6) N32 0.0231(8) 0.0204(8) 0.0153(8) 0.0048(6) 0.0032(6) -0.0005(7) C11 0.0210(10) 0.0214(10) 0.0229(10) 0.0016(8) 0.0077(8) 0.0008(8) C12 0.0258(11) 0.0269(11) 0.0281(11) 0.0055(9) 0.0129(9) -0.0004(8) C13 0.0282(11) 0.0220(10) 0.0201(10) 0.0050(8) 0.0108(8) 0.0009(8) C14 0.0201(10) 0.0447(14) 0.0274(11) 0.0060(10) 0.0053(9) 0.0019(9) C15 0.0359(13) 0.0466(14) 0.0245(11) 0.0176(10) 0.0113(10) 0.0034(11) C21 0.0251(11) 0.0237(10) 0.0294(11) 0.0030(9) 0.0101(9) 0.0039(8) C22 0.0295(11) 0.0240(11) 0.0368(12) 0.0092(9) 0.0121(10) 0.0095(9) C23 0.0246(10) 0.0221(10) 0.0343(12) 0.0130(9) 0.0089(9) 0.0076(8) C24 0.0376(14) 0.0393(14) 0.0324(13) -0.0076(11) 0.0082(11) 0.0099(11) C25 0.0348(13) 0.0394(14) 0.0374(13) 0.0156(11) 0.0040(11) 0.0151(11) C31 0.0233(10) 0.0201(9) 0.0253(10) 0.0057(8) 0.0077(8) 0.0009(8) C32 0.0259(11) 0.0177(9) 0.0309(11) 0.0015(8) 0.0057(9) -0.0018(8) C33 0.0200(10) 0.0213(10) 0.0204(10) -0.0029(8) 0.0044(8) -0.0016(8) C34 0.0414(14) 0.0280(12) 0.0324(12) 0.0147(10) 0.0065(10) -0.0023(10) C35 0.0324(12) 0.0321(12) 0.0214(11) -0.0031(9) -0.0004(9) -0.0039(9) C41 0.0223(10) 0.0219(10) 0.0202(9) 0.0063(8) 0.0073(8) 0.0011(8) C42 0.0253(11) 0.0283(11) 0.0243(10) 0.0052(9) 0.0038(8) 0.0016(8) C43 0.0267(12) 0.0378(13) 0.0381(13) 0.0133(11) 0.0037(10) 0.0057(10) C44 0.0367(13) 0.0339(13) 0.0458(14) 0.0178(11) 0.0188(11) 0.0155(10) C45 0.0477(15) 0.0304(12) 0.0312(12) 0.0052(10) 0.0175(11) 0.0122(11) C46 0.0340(12) 0.0286(11) 0.0220(10) 0.0033(9) 0.0067(9) 0.0046(9) C51 0.0168(9) 0.0239(10) 0.0193(9) 0.0020(8) 0.0035(7) 0.0016(7) C52 0.0278(11) 0.0329(12) 0.0191(10) 0.0011(9) 0.0060(8) -0.0043(9) C53 0.0335(12) 0.0393(13) 0.0229(11) -0.0054(10) 0.0078(9) -0.0073(10) C54 0.0278(12) 0.0277(11) 0.0361(13) -0.0055(10) 0.0037(10) -0.0041(9) C55 0.0313(12) 0.0261(11) 0.0347(12) 0.0069(9) 0.0041(10) -0.0018(9) C56 0.0254(10) 0.0257(10) 0.0222(10) 0.0045(8) 0.0037(8) 0.0007(8) C61 0.0246(10) 0.0267(10) 0.0161(9) 0.0006(8) 0.0053(8) -0.0053(8) C62 0.0323(13) 0.0539(16) 0.0281(12) 0.0189(11) 0.0047(10) -0.0067(11) C63 0.0512(18) 0.077(2) 0.0364(15) 0.0290(15) 0.0110(13) -0.0125(16) C64 0.0554(19) 0.079(2) 0.0483(18) 0.0208(17) 0.0307(15) -0.0103(17) C65 0.0350(15) 0.066(2) 0.0591(19) 0.0144(16) 0.0276(14) 0.0012(13) C66 0.0292(12) 0.0426(14) 0.0354(13) 0.0102(11) 0.0127(10) 0.0009(10) P3 0.0334(3) 0.0325(3) 0.0310(3) 0.0048(3) 0.0046(3) 0.0112(3) F1 0.0564(12) 0.126(2) 0.0498(11) 0.0479(13) 0.0071(9) -0.0026(12) F2 0.0360(8) 0.0592(10) 0.0408(9) 0.0136(8) 0.0057(7) 0.0189(7) F3 0.0734(15) 0.174(3) 0.0482(12) 0.0323(15) 0.0358(11) 0.0471(17) F4 0.0427(10) 0.0482(10) 0.0672(12) -0.0009(9) -0.0050(8) 0.0224(8) F5 0.0506(11) 0.0363(9) 0.0811(14) 0.0052(9) 0.0080(10) 0.0070(8) F6 0.0794(16) 0.0354(11) 0.140(2) -0.0163(13) -0.0489(16) 0.0137(10) Cl1 0.0853(6) 0.0439(4) 0.0425(4) 0.0138(3) 0.0236(4) 0.0208(4) Cl2 0.0327(4) 0.0722(6) 0.0651(5) -0.0002(4) 0.0033(3) 0.0058(3) C71 0.0412(15) 0.0422(15) 0.0448(15) 0.0135(12) 0.0138(12) 0.0058(12) Cl3A 0.0723(18) 0.0650(15) 0.0398(9) -0.0030(9) 0.0093(8) 0.0309(13) Cl4A 0.179(4) 0.0365(11) 0.0456(11) 0.0065(8) 0.019(2) 0.041(2) Cl3B 0.103(2) 0.0443(12) 0.0691(16) -0.0215(10) 0.0432(17) -0.0120(14) Cl4B 0.0588(15) 0.0278(11) 0.0461(17) 0.0141(10) -0.0083(10) 0.0001(9) C81 0.0459(16) 0.0626(19) 0.0398(15) 0.0267(14) 0.0075(12) 0.0064(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N22 2.0843(18) . ? Cu1 N12 2.0863(17) . ? Cu1 N32 2.1039(17) . ? Cu1 P2 2.1820(5) . ? P1 O1 1.4513(15) . ? P1 N21 1.6729(18) . ? P1 N31 1.6781(18) . ? P1 N11 1.6808(18) . ? P2 C61 1.822(2) . ? P2 C51 1.824(2) . ? P2 C41 1.826(2) . ? N11 C13 1.387(3) . ? N11 N12 1.391(2) . ? N12 C11 1.325(3) . ? N21 C23 1.390(3) . ? N21 N22 1.396(2) . ? N22 C21 1.322(3) . ? N31 C33 1.386(3) . ? N31 N32 1.390(2) . ? N32 C31 1.325(3) . ? C11 C12 1.405(3) . ? C11 C14 1.487(3) . ? C12 C13 1.357(3) . ? C12 H12 0.9500 . ? C13 C15 1.493(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C21 C22 1.412(3) . ? C21 C24 1.487(3) . ? C22 C23 1.351(3) . ? C22 H22 0.9500 . ? C23 C25 1.494(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C31 C32 1.412(3) . ? C31 C34 1.487(3) . ? C32 C33 1.359(3) . ? C32 H32 0.9500 . ? C33 C35 1.491(3) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C41 C46 1.392(3) . ? C41 C42 1.392(3) . ? C42 C43 1.386(3) . ? C42 H42 0.9500 . ? C43 C44 1.382(4) . ? C43 H43 0.9500 . ? C44 C45 1.382(4) . ? C44 H44 0.9500 . ? C45 C46 1.387(3) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C51 C56 1.390(3) . ? C51 C52 1.400(3) . ? C52 C53 1.386(3) . ? C52 H52 0.9500 . ? C53 C54 1.386(4) . ? C53 H53 0.9500 . ? C54 C55 1.383(4) . ? C54 H54 0.9500 . ? C55 C56 1.389(3) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C61 C66 1.391(3) . ? C61 C62 1.391(3) . ? C62 C63 1.381(4) . ? C62 H62 0.9500 . ? C63 C64 1.370(5) . ? C63 H63 0.9500 . ? C64 C65 1.389(5) . ? C64 H64 0.9500 . ? C65 C66 1.386(4) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? P3 F6 1.567(2) . ? P3 F3 1.580(2) . ? P3 F5 1.5893(19) . ? P3 F4 1.5939(17) . ? P3 F1 1.598(2) . ? P3 F2 1.5992(16) . ? Cl1 C71 1.757(3) . ? Cl2 C71 1.751(3) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? Cl3A C81 1.857(4) . ? Cl4A C81 1.643(5) . ? Cl3B C81 1.593(4) . ? Cl4B C81 1.817(4) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C81 H81C 0.9900 . ? C81 H81D 0.9900 . ? 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 N22 Cu1 N12 90.00(7) . . ? N22 Cu1 N32 91.91(7) . . ? N12 Cu1 N32 89.74(7) . . ? N22 Cu1 P2 125.39(5) . . ? N12 Cu1 P2 126.45(5) . . ? N32 Cu1 P2 122.77(5) . . ? O1 P1 N21 113.44(9) . . ? O1 P1 N31 112.98(9) . . ? N21 P1 N31 105.80(9) . . ? O1 P1 N11 113.18(9) . . ? N21 P1 N11 105.83(9) . . ? N31 P1 N11 104.87(9) . . ? C61 P2 C51 102.68(10) . . ? C61 P2 C41 105.57(10) . . ? C51 P2 C41 104.16(9) . . ? C61 P2 Cu1 113.52(7) . . ? C51 P2 Cu1 115.52(7) . . ? C41 P2 Cu1 114.13(7) . . ? C13 N11 N12 110.68(16) . . ? C13 N11 P1 129.29(15) . . ? N12 N11 P1 119.96(13) . . ? C11 N12 N11 105.00(17) . . ? C11 N12 Cu1 136.89(14) . . ? N11 N12 Cu1 117.43(13) . . ? C23 N21 N22 110.53(17) . . ? C23 N21 P1 129.27(15) . . ? N22 N21 P1 120.02(13) . . ? C21 N22 N21 105.18(17) . . ? C21 N22 Cu1 136.93(15) . . ? N21 N22 Cu1 116.91(13) . . ? C33 N31 N32 111.14(16) . . ? C33 N31 P1 128.73(15) . . ? N32 N31 P1 119.83(13) . . ? C31 N32 N31 104.96(16) . . ? C31 N32 Cu1 137.53(14) . . ? N31 N32 Cu1 117.34(12) . . ? N12 C11 C12 111.08(19) . . ? N12 C11 C14 120.91(19) . . ? C12 C11 C14 128.0(2) . . ? C13 C12 C11 107.28(19) . . ? C13 C12 H12 126.4 . . ? C11 C12 H12 126.4 . . ? C12 C13 N11 105.95(18) . . ? C12 C13 C15 129.7(2) . . ? N11 C13 C15 124.3(2) . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N22 C21 C22 110.8(2) . . ? N22 C21 C24 121.7(2) . . ? C22 C21 C24 127.5(2) . . ? C23 C22 C21 107.6(2) . . ? C23 C22 H22 126.2 . . ? C21 C22 H22 126.2 . . ? C22 C23 N21 105.91(19) . . ? C22 C23 C25 129.6(2) . . ? N21 C23 C25 124.5(2) . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N32 C31 C32 110.92(19) . . ? N32 C31 C34 121.8(2) . . ? C32 C31 C34 127.2(2) . . ? C33 C32 C31 107.31(19) . . ? C33 C32 H32 126.3 . . ? C31 C32 H32 126.3 . . ? C32 C33 N31 105.67(18) . . ? C32 C33 C35 129.8(2) . . ? N31 C33 C35 124.6(2) . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C46 C41 C42 118.6(2) . . ? C46 C41 P2 117.78(16) . . ? C42 C41 P2 123.62(17) . . ? C43 C42 C41 120.4(2) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C44 C43 C42 120.3(2) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C45 C44 C43 120.0(2) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C44 C45 C46 119.7(2) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? C45 C46 C41 121.0(2) . . ? C45 C46 H46 119.5 . . ? C41 C46 H46 119.5 . . ? C56 C51 C52 118.9(2) . . ? C56 C51 P2 117.83(16) . . ? C52 C51 P2 123.28(17) . . ? C53 C52 C51 120.0(2) . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C52 C53 C54 120.6(2) . . ? C52 C53 H53 119.7 . . ? C54 C53 H53 119.7 . . ? C55 C54 C53 119.7(2) . . ? C55 C54 H54 120.2 . . ? C53 C54 H54 120.2 . . ? C54 C55 C56 120.0(2) . . ? C54 C55 H55 120.0 . . ? C56 C55 H55 120.0 . . ? C55 C56 C51 120.8(2) . . ? C55 C56 H56 119.6 . . ? C51 C56 H56 119.6 . . ? C66 C61 C62 119.2(2) . . ? C66 C61 P2 117.46(17) . . ? C62 C61 P2 123.33(18) . . ? C63 C62 C61 120.0(3) . . ? C63 C62 H62 120.0 . . ? C61 C62 H62 120.0 . . ? C64 C63 C62 120.7(3) . . ? C64 C63 H63 119.6 . . ? C62 C63 H63 119.6 . . ? C63 C64 C65 120.1(3) . . ? C63 C64 H64 120.0 . . ? C65 C64 H64 120.0 . . ? C66 C65 C64 119.6(3) . . ? C66 C65 H65 120.2 . . ? C64 C65 H65 120.2 . . ? C65 C66 C61 120.5(3) . . ? C65 C66 H66 119.8 . . ? C61 C66 H66 119.8 . . ? F6 P3 F3 91.79(19) . . ? F6 P3 F5 179.04(17) . . ? F3 P3 F5 88.99(15) . . ? F6 P3 F4 90.98(11) . . ? F3 P3 F4 90.38(12) . . ? F5 P3 F4 89.58(10) . . ? F6 P3 F1 91.50(18) . . ? F3 P3 F1 176.46(16) . . ? F5 P3 F1 87.71(13) . . ? F4 P3 F1 90.88(12) . . ? F6 P3 F2 89.09(11) . . ? F3 P3 F2 89.46(11) . . ? F5 P3 F2 90.36(10) . . ? F4 P3 F2 179.83(13) . . ? F1 P3 F2 89.28(11) . . ? Cl2 C71 Cl1 111.42(16) . . ? Cl2 C71 H71A 109.3 . . ? Cl1 C71 H71A 109.3 . . ? Cl2 C71 H71B 109.3 . . ? Cl1 C71 H71B 109.3 . . ? H71A C71 H71B 108.0 . . ? Cl3B C81 Cl4B 115.0(2) . . ? Cl4A C81 Cl3A 109.9(2) . . ? Cl4A C81 H81A 109.7 . . ? Cl3A C81 H81A 109.7 . . ? Cl4A C81 H81B 109.7 . . ? Cl3A C81 H81B 109.7 . . ? H81A C81 H81B 108.2 . . ? Cl3B C81 H81C 108.5 . . ? Cl4B C81 H81C 108.5 . . ? Cl3B C81 H81D 108.5 . . ? Cl4B C81 H81D 108.5 . . ? H81C C81 H81D 107.5 . . ? 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 N22 Cu1 P2 C61 -71.43(10) . . . . ? N12 Cu1 P2 C61 166.92(10) . . . . ? N32 Cu1 P2 C61 48.97(10) . . . . ? N22 Cu1 P2 C51 46.80(10) . . . . ? N12 Cu1 P2 C51 -74.85(10) . . . . ? N32 Cu1 P2 C51 167.20(9) . . . . ? N22 Cu1 P2 C41 167.53(10) . . . . ? N12 Cu1 P2 C41 45.88(10) . . . . ? N32 Cu1 P2 C41 -72.07(10) . . . . ? O1 P1 N11 C13 -2.9(2) . . . . ? N21 P1 N11 C13 121.90(19) . . . . ? N31 P1 N11 C13 -126.51(19) . . . . ? O1 P1 N11 N12 173.56(15) . . . . ? N21 P1 N11 N12 -61.61(17) . . . . ? N31 P1 N11 N12 49.98(17) . . . . ? C13 N11 N12 C11 -0.2(2) . . . . ? P1 N11 N12 C11 -177.30(14) . . . . ? C13 N11 N12 Cu1 -172.35(13) . . . . ? P1 N11 N12 Cu1 10.6(2) . . . . ? N22 Cu1 N12 C11 -128.7(2) . . . . ? N32 Cu1 N12 C11 139.4(2) . . . . ? P2 Cu1 N12 C11 7.3(2) . . . . ? N22 Cu1 N12 N11 40.15(14) . . . . ? N32 Cu1 N12 N11 -51.76(14) . . . . ? P2 Cu1 N12 N11 176.21(11) . . . . ? O1 P1 N21 C23 -4.0(2) . . . . ? N31 P1 N21 C23 120.42(19) . . . . ? N11 P1 N21 C23 -128.64(19) . . . . ? O1 P1 N21 N22 170.71(15) . . . . ? N31 P1 N21 N22 -64.89(17) . . . . ? N11 P1 N21 N22 46.04(17) . . . . ? C23 N21 N22 C21 0.8(2) . . . . ? P1 N21 N22 C21 -174.82(15) . . . . ? C23 N21 N22 Cu1 -169.78(14) . . . . ? P1 N21 N22 Cu1 14.6(2) . . . . ? N12 Cu1 N22 C21 139.5(2) . . . . ? N32 Cu1 N22 C21 -130.8(2) . . . . ? P2 Cu1 N22 C21 2.7(3) . . . . ? N12 Cu1 N22 N21 -53.88(15) . . . . ? N32 Cu1 N22 N21 35.86(15) . . . . ? P2 Cu1 N22 N21 169.34(11) . . . . ? O1 P1 N31 C33 0.8(2) . . . . ? N21 P1 N31 C33 -123.92(18) . . . . ? N11 P1 N31 C33 124.46(18) . . . . ? O1 P1 N31 N32 173.94(14) . . . . ? N21 P1 N31 N32 49.26(17) . . . . ? N11 P1 N31 N32 -62.36(16) . . . . ? C33 N31 N32 C31 0.1(2) . . . . ? P1 N31 N32 C31 -174.21(15) . . . . ? C33 N31 N32 Cu1 -175.91(13) . . . . ? P1 N31 N32 Cu1 9.8(2) . . . . ? N22 Cu1 N32 C31 136.5(2) . . . . ? N12 Cu1 N32 C31 -133.5(2) . . . . ? P2 Cu1 N32 C31 1.2(2) . . . . ? N22 Cu1 N32 N31 -49.23(14) . . . . ? N12 Cu1 N32 N31 40.76(14) . . . . ? P2 Cu1 N32 N31 175.48(11) . . . . ? N11 N12 C11 C12 0.7(2) . . . . ? Cu1 N12 C11 C12 170.43(16) . . . . ? N11 N12 C11 C14 -177.02(19) . . . . ? Cu1 N12 C11 C14 -7.2(3) . . . . ? N12 C11 C12 C13 -0.9(3) . . . . ? C14 C11 C12 C13 176.6(2) . . . . ? C11 C12 C13 N11 0.7(2) . . . . ? C11 C12 C13 C15 -179.0(2) . . . . ? N12 N11 C13 C12 -0.3(2) . . . . ? P1 N11 C13 C12 176.42(16) . . . . ? N12 N11 C13 C15 179.4(2) . . . . ? P1 N11 C13 C15 -3.8(3) . . . . ? N21 N22 C21 C22 -0.9(2) . . . . ? Cu1 N22 C21 C22 166.76(17) . . . . ? N21 N22 C21 C24 177.8(2) . . . . ? Cu1 N22 C21 C24 -14.5(4) . . . . ? N22 C21 C22 C23 0.7(3) . . . . ? C24 C21 C22 C23 -177.9(2) . . . . ? C21 C22 C23 N21 -0.2(3) . . . . ? C21 C22 C23 C25 179.3(2) . . . . ? N22 N21 C23 C22 -0.4(2) . . . . ? P1 N21 C23 C22 174.72(17) . . . . ? N22 N21 C23 C25 -179.9(2) . . . . ? P1 N21 C23 C25 -4.8(3) . . . . ? N31 N32 C31 C32 -0.2(2) . . . . ? Cu1 N32 C31 C32 174.55(16) . . . . ? N31 N32 C31 C34 178.9(2) . . . . ? Cu1 N32 C31 C34 -6.4(4) . . . . ? N32 C31 C32 C33 0.2(3) . . . . ? C34 C31 C32 C33 -178.8(2) . . . . ? C31 C32 C33 N31 -0.2(2) . . . . ? C31 C32 C33 C35 -179.7(2) . . . . ? N32 N31 C33 C32 0.0(2) . . . . ? P1 N31 C33 C32 173.70(16) . . . . ? N32 N31 C33 C35 179.6(2) . . . . ? P1 N31 C33 C35 -6.7(3) . . . . ? C61 P2 C41 C46 -103.23(18) . . . . ? C51 P2 C41 C46 149.00(18) . . . . ? Cu1 P2 C41 C46 22.14(19) . . . . ? C61 P2 C41 C42 78.8(2) . . . . ? C51 P2 C41 C42 -28.9(2) . . . . ? Cu1 P2 C41 C42 -155.80(16) . . . . ? C46 C41 C42 C43 -0.8(3) . . . . ? P2 C41 C42 C43 177.07(18) . . . . ? C41 C42 C43 C44 0.1(4) . . . . ? C42 C43 C44 C45 1.1(4) . . . . ? C43 C44 C45 C46 -1.5(4) . . . . ? C44 C45 C46 C41 0.7(4) . . . . ? C42 C41 C46 C45 0.4(3) . . . . ? P2 C41 C46 C45 -177.61(19) . . . . ? C61 P2 C51 C56 148.37(17) . . . . ? C41 P2 C51 C56 -101.73(18) . . . . ? Cu1 P2 C51 C56 24.27(19) . . . . ? C61 P2 C51 C52 -29.8(2) . . . . ? C41 P2 C51 C52 80.1(2) . . . . ? Cu1 P2 C51 C52 -153.86(16) . . . . ? C56 C51 C52 C53 -0.2(3) . . . . ? P2 C51 C52 C53 177.89(18) . . . . ? C51 C52 C53 C54 -0.2(4) . . . . ? C52 C53 C54 C55 0.6(4) . . . . ? C53 C54 C55 C56 -0.7(4) . . . . ? C54 C55 C56 C51 0.3(4) . . . . ? C52 C51 C56 C55 0.2(3) . . . . ? P2 C51 C56 C55 -178.04(18) . . . . ? C51 P2 C61 C66 -93.48(19) . . . . ? C41 P2 C61 C66 157.68(18) . . . . ? Cu1 P2 C61 C66 31.9(2) . . . . ? C51 P2 C61 C62 84.3(2) . . . . ? C41 P2 C61 C62 -24.6(2) . . . . ? Cu1 P2 C61 C62 -150.30(19) . . . . ? C66 C61 C62 C63 0.1(4) . . . . ? P2 C61 C62 C63 -177.6(2) . . . . ? C61 C62 C63 C64 0.0(5) . . . . ? C62 C63 C64 C65 0.2(6) . . . . ? C63 C64 C65 C66 -0.6(5) . . . . ? C64 C65 C66 C61 0.8(5) . . . . ? C62 C61 C66 C65 -0.5(4) . . . . ? P2 C61 C66 C65 177.3(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.867 _refine_diff_density_min -0.721 _refine_diff_density_rms 0.069 #===END