Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Andrew M Brodie' _publ_contact_author_address ; Chemistry - IFS Massey University PB 11 222 Palmerston North NEW ZEALAND ; _publ_contact_author_email A.BRODIE@MASSEY.AC.NZ _publ_section_title ; Copper(II) chloride complexes with multimodal ligands based on the cyclotriphosphazene platform ; loop_ _publ_author_name 'Andrew M. Brodie' 'Eric W. Ainscough' 'Craig V. Depree' 'Boujemaa Moubaraki' 'Keith Murray' ; C.A.Otter ; data_cvdcu1 _database_code_depnum_ccdc_archive 'CCDC 275486' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H24 Cl2 Cu N9 O6 P3' _chemical_formula_weight 833.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.028(3) _cell_length_b 11.413(3) _cell_length_c 16.835(4) _cell_angle_alpha 72.850(3) _cell_angle_beta 88.883(3) _cell_angle_gamma 73.213(3) _cell_volume 1758.1(8) _cell_formula_units_Z 2 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 7111 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 26.41 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 846 _exptl_absorpt_coefficient_mu 0.967 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22609 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 26.42 _reflns_number_total 7111 _reflns_number_gt 5742 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0530P)^2^+2.2148P] 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 7111 _refine_ls_number_parameters 460 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1087 _refine_ls_wR_factor_gt 0.1020 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.89502(4) -0.24725(3) 0.30405(2) 0.02007(10) Uani 1 1 d . . . Cl1 Cl 0.70286(8) -0.31834(8) 0.31617(5) 0.03018(18) Uani 1 1 d . . . Cl2 Cl 1.13432(8) -0.30241(7) 0.31556(5) 0.02846(17) Uani 1 1 d . . . P1 P 0.81956(8) 0.03656(7) 0.16390(5) 0.01883(16) Uani 1 1 d . . . P2 P 0.82509(7) 0.04141(7) 0.32710(5) 0.01889(16) Uani 1 1 d . . . P3 P 0.87224(8) 0.24057(7) 0.20066(5) 0.01983(16) Uani 1 1 d . . . O1 O 0.9433(2) -0.05495(19) 0.12937(12) 0.0214(4) Uani 1 1 d . . . O2 O 0.6780(2) 0.0363(2) 0.12270(13) 0.0250(5) Uani 1 1 d . . . O3 O 0.9432(2) -0.05324(19) 0.39811(12) 0.0212(4) Uani 1 1 d . . . O4 O 0.6825(2) 0.0524(2) 0.37207(13) 0.0256(5) Uani 1 1 d . . . O5 O 1.0176(2) 0.27416(19) 0.18729(13) 0.0255(5) Uani 1 1 d . . . O6 O 0.7827(2) 0.38797(19) 0.17329(13) 0.0247(5) Uani 1 1 d . . . N1 N 0.8130(2) -0.0302(2) 0.26064(15) 0.0211(5) Uani 1 1 d . . . N2 N 0.8571(3) 0.1745(2) 0.29549(15) 0.0224(5) Uani 1 1 d . . . N3 N 0.8426(3) 0.1737(2) 0.13568(15) 0.0221(5) Uani 1 1 d . . . N16 N 0.9107(2) -0.2573(2) 0.18384(15) 0.0215(5) Uani 1 1 d . . . N26 N 0.7296(3) 0.0902(3) -0.01549(17) 0.0323(6) Uani 1 1 d . . . N36 N 0.8953(2) -0.2501(2) 0.42683(15) 0.0209(5) Uani 1 1 d . . . N46 N 0.7446(3) 0.1426(3) 0.4667(2) 0.0409(7) Uani 1 1 d . . . N56 N 1.1511(3) 0.0604(3) 0.23914(17) 0.0289(6) Uani 1 1 d . . . N66 N 0.5649(3) 0.4594(3) 0.1052(2) 0.0395(7) Uani 1 1 d . . . C11 C 0.9427(3) -0.1713(3) 0.11977(18) 0.0216(6) Uani 1 1 d . . . C12 C 0.9827(3) -0.1918(3) 0.0451(2) 0.0291(7) Uani 1 1 d . . . H12 H 1.0050 -0.1271 0.0015 0.035 Uiso 1 1 calc R . . C13 C 0.9893(4) -0.3096(3) 0.0358(2) 0.0345(8) Uani 1 1 d . . . H13 H 1.0175 -0.3279 -0.0146 0.041 Uiso 1 1 calc R . . C14 C 0.9542(4) -0.4015(3) 0.1011(2) 0.0310(7) Uani 1 1 d . . . H14 H 0.9574 -0.4828 0.0958 0.037 Uiso 1 1 calc R . . C15 C 0.9151(3) -0.3719(3) 0.1729(2) 0.0262(6) Uani 1 1 d . . . H15 H 0.8899 -0.4340 0.2169 0.031 Uiso 1 1 calc R . . C21 C 0.6335(3) 0.0942(3) 0.03794(19) 0.0266(7) Uani 1 1 d . . . C22 C 0.4902(4) 0.1458(4) 0.0190(2) 0.0389(8) Uani 1 1 d . . . H22 H 0.4261 0.1460 0.0613 0.047 Uiso 1 1 calc R . . C23 C 0.4460(4) 0.1968(4) -0.0647(3) 0.0468(10) Uani 1 1 d . . . H23 H 0.3493 0.2335 -0.0815 0.056 Uiso 1 1 calc R . . C24 C 0.5433(4) 0.1938(4) -0.1234(2) 0.0432(9) Uani 1 1 d . . . H24 H 0.5149 0.2273 -0.1812 0.052 Uiso 1 1 calc R . . C25 C 0.6826(4) 0.1414(4) -0.0967(2) 0.0434(9) Uani 1 1 d . . . H25 H 0.7493 0.1411 -0.1375 0.052 Uiso 1 1 calc R . . C31 C 0.9248(3) -0.1618(3) 0.45570(18) 0.0208(6) Uani 1 1 d . . . C32 C 0.9439(3) -0.1738(3) 0.53887(19) 0.0287(7) Uani 1 1 d . . . H32 H 0.9641 -0.1083 0.5561 0.034 Uiso 1 1 calc R . . C33 C 0.9324(4) -0.2856(3) 0.5966(2) 0.0335(7) Uani 1 1 d . . . H33 H 0.9465 -0.2987 0.6546 0.040 Uiso 1 1 calc R . . C34 C 0.9002(4) -0.3779(3) 0.5688(2) 0.0315(7) Uani 1 1 d . . . H34 H 0.8907 -0.4542 0.6075 0.038 Uiso 1 1 calc R . . C35 C 0.8822(3) -0.3573(3) 0.48451(19) 0.0263(7) Uani 1 1 d . . . H35 H 0.8596 -0.4206 0.4659 0.032 Uiso 1 1 calc R . . C41 C 0.6452(3) 0.1209(3) 0.42981(19) 0.0292(7) Uani 1 1 d . . . C42 C 0.5069(5) 0.1527(5) 0.4451(3) 0.0654(13) Uani 1 1 d U . . H42 H 0.4398 0.1307 0.4179 0.078 Uiso 1 1 calc R . . C43 C 0.4712(7) 0.2195(6) 0.5034(4) 0.0844(17) Uani 1 1 d U . . H43 H 0.3776 0.2423 0.5184 0.101 Uiso 1 1 calc R . . C44 C 0.5723(5) 0.2528(5) 0.5395(3) 0.0563(11) Uani 1 1 d U . . H44 H 0.5484 0.3038 0.5762 0.068 Uiso 1 1 calc R . . C45 C 0.7056(4) 0.2105(4) 0.5211(3) 0.0488(10) Uani 1 1 d . . . H45 H 0.7758 0.2295 0.5478 0.059 Uiso 1 1 calc R . . C51 C 1.1479(3) 0.1823(3) 0.21277(19) 0.0242(6) Uani 1 1 d . . . C52 C 1.2614(3) 0.2294(3) 0.2082(2) 0.0344(8) Uani 1 1 d . . . H52 H 1.2510 0.3188 0.1881 0.041 Uiso 1 1 calc R . . C53 C 1.3912(4) 0.1395(4) 0.2346(3) 0.0439(9) Uani 1 1 d . . . H53 H 1.4728 0.1662 0.2328 0.053 Uiso 1 1 calc R . . C54 C 1.4004(4) 0.0095(4) 0.2636(2) 0.0415(9) Uani 1 1 d . . . H54 H 1.4881 -0.0537 0.2823 0.050 Uiso 1 1 calc R . . C55 C 1.2793(4) -0.0252(3) 0.2647(2) 0.0371(8) Uani 1 1 d . . . H55 H 1.2860 -0.1139 0.2845 0.045 Uiso 1 1 calc R . . C61 C 0.6365(3) 0.4273(3) 0.1766(2) 0.0262(7) Uani 1 1 d . . . C62 C 0.5823(4) 0.4385(3) 0.2507(2) 0.0393(8) Uani 1 1 d . . . H62 H 0.6404 0.4134 0.3004 0.047 Uiso 1 1 calc R . . C63 C 0.4375(4) 0.4886(4) 0.2489(3) 0.0496(10) Uani 1 1 d . . . H63 H 0.3939 0.4978 0.2983 0.060 Uiso 1 1 calc R . . C64 C 0.3589(4) 0.5244(4) 0.1755(3) 0.0515(11) Uani 1 1 d . . . H64 H 0.2604 0.5604 0.1729 0.062 Uiso 1 1 calc R . . C65 C 0.4243(4) 0.5076(4) 0.1057(3) 0.0522(11) Uani 1 1 d . . . H65 H 0.3687 0.5308 0.0553 0.063 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 0.02141(19) 0.01958(18) 0.01809(19) -0.00380(14) 0.00209(13) -0.00633(14) Cl1 0.0273(4) 0.0381(4) 0.0293(4) -0.0098(3) 0.0057(3) -0.0165(3) Cl2 0.0216(4) 0.0318(4) 0.0307(4) -0.0089(3) 0.0029(3) -0.0066(3) P1 0.0202(4) 0.0169(4) 0.0180(4) -0.0030(3) 0.0000(3) -0.0057(3) P2 0.0185(4) 0.0188(4) 0.0184(4) -0.0042(3) 0.0021(3) -0.0054(3) P3 0.0211(4) 0.0157(4) 0.0216(4) -0.0039(3) 0.0014(3) -0.0054(3) O1 0.0238(10) 0.0182(10) 0.0236(11) -0.0072(8) 0.0051(8) -0.0075(8) O2 0.0237(11) 0.0262(11) 0.0222(11) -0.0019(9) -0.0031(8) -0.0081(9) O3 0.0198(10) 0.0211(10) 0.0201(10) -0.0020(8) 0.0003(8) -0.0066(8) O4 0.0215(10) 0.0311(12) 0.0257(11) -0.0096(9) 0.0055(9) -0.0091(9) O5 0.0211(10) 0.0214(11) 0.0313(12) -0.0032(9) 0.0018(9) -0.0073(9) O6 0.0236(11) 0.0151(10) 0.0321(12) -0.0042(9) 0.0022(9) -0.0037(8) N1 0.0235(12) 0.0181(12) 0.0196(13) -0.0026(10) 0.0004(10) -0.0059(10) N2 0.0273(13) 0.0180(12) 0.0224(13) -0.0063(10) 0.0018(10) -0.0071(10) N3 0.0286(13) 0.0168(12) 0.0197(12) -0.0031(10) 0.0021(10) -0.0076(10) N16 0.0217(12) 0.0220(12) 0.0195(12) -0.0042(10) 0.0009(10) -0.0069(10) N26 0.0334(15) 0.0393(16) 0.0230(14) -0.0055(12) -0.0035(11) -0.0125(13) N36 0.0189(12) 0.0201(12) 0.0196(12) -0.0023(10) 0.0011(9) -0.0034(10) N46 0.0290(15) 0.060(2) 0.0405(18) -0.0290(16) 0.0094(13) -0.0100(14) N56 0.0289(14) 0.0246(14) 0.0309(15) -0.0064(11) -0.0004(11) -0.0064(11) N66 0.0363(16) 0.0348(16) 0.0436(18) -0.0122(14) -0.0096(14) -0.0035(13) C11 0.0204(14) 0.0194(14) 0.0248(15) -0.0058(12) 0.0009(11) -0.0065(11) C12 0.0391(18) 0.0245(16) 0.0256(16) -0.0074(13) 0.0110(14) -0.0133(14) C13 0.050(2) 0.0302(18) 0.0291(18) -0.0143(15) 0.0141(16) -0.0159(16) C14 0.0440(19) 0.0202(15) 0.0323(18) -0.0105(13) 0.0072(15) -0.0126(14) C15 0.0308(16) 0.0207(15) 0.0266(16) -0.0046(12) 0.0032(13) -0.0096(13) C21 0.0325(17) 0.0220(15) 0.0245(16) -0.0046(12) -0.0076(13) -0.0091(13) C22 0.0310(18) 0.042(2) 0.038(2) -0.0097(17) -0.0064(15) -0.0035(16) C23 0.040(2) 0.041(2) 0.050(2) -0.0099(18) -0.0232(18) -0.0003(17) C24 0.056(2) 0.038(2) 0.0299(19) -0.0022(16) -0.0173(17) -0.0118(18) C25 0.054(2) 0.053(2) 0.0227(18) -0.0049(16) -0.0035(16) -0.0211(19) C31 0.0170(13) 0.0205(14) 0.0204(15) -0.0013(11) 0.0015(11) -0.0037(11) C32 0.0347(17) 0.0306(17) 0.0230(16) -0.0079(13) 0.0007(13) -0.0130(14) C33 0.045(2) 0.0346(18) 0.0185(16) -0.0036(14) 0.0019(14) -0.0123(16) C34 0.0376(18) 0.0240(16) 0.0264(17) 0.0014(13) 0.0029(14) -0.0085(14) C35 0.0277(16) 0.0209(15) 0.0264(16) -0.0030(13) 0.0032(13) -0.0057(12) C41 0.0256(16) 0.0362(18) 0.0215(16) -0.0073(14) 0.0046(12) -0.0046(14) C42 0.0624(15) 0.0706(15) 0.0642(15) -0.0252(10) 0.0045(10) -0.0163(10) C43 0.0820(19) 0.0880(19) 0.0832(19) -0.0305(11) 0.0074(10) -0.0205(11) C44 0.0559(14) 0.0590(14) 0.0537(14) -0.0226(10) 0.0054(9) -0.0108(9) C45 0.043(2) 0.070(3) 0.042(2) -0.035(2) 0.0081(17) -0.012(2) C51 0.0215(14) 0.0275(16) 0.0230(15) -0.0082(13) 0.0031(12) -0.0060(12) C52 0.0301(17) 0.0350(18) 0.041(2) -0.0117(16) 0.0041(15) -0.0138(15) C53 0.0252(17) 0.055(2) 0.055(2) -0.018(2) 0.0042(16) -0.0150(17) C54 0.0245(17) 0.047(2) 0.047(2) -0.0148(18) -0.0041(15) 0.0007(16) C55 0.0383(19) 0.0291(18) 0.039(2) -0.0098(15) -0.0026(15) -0.0030(15) C61 0.0232(15) 0.0159(14) 0.0376(18) -0.0075(13) 0.0017(13) -0.0035(12) C62 0.0370(19) 0.0329(19) 0.044(2) -0.0127(16) 0.0065(16) -0.0034(15) C63 0.039(2) 0.040(2) 0.069(3) -0.020(2) 0.020(2) -0.0072(17) C64 0.0265(18) 0.033(2) 0.089(3) -0.016(2) 0.000(2) -0.0025(15) C65 0.033(2) 0.048(2) 0.070(3) -0.017(2) -0.017(2) -0.0035(18) _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 N36 2.058(3) . ? Cu1 N16 2.061(3) . ? Cu1 N1 2.264(2) . ? Cu1 Cl1 2.2810(9) . ? Cu1 Cl2 2.2947(10) . ? P1 N3 1.579(2) . ? P1 N1 1.591(2) . ? P1 O2 1.593(2) . ? P1 O1 1.597(2) . ? P2 N2 1.578(2) . ? P2 N1 1.593(3) . ? P2 O4 1.595(2) . ? P2 O3 1.598(2) . ? P3 N2 1.577(3) . ? P3 N3 1.583(3) . ? P3 O6 1.592(2) . ? P3 O5 1.607(2) . ? O1 C11 1.386(3) . ? O2 C21 1.404(4) . ? O3 C31 1.387(3) . ? O4 C41 1.401(4) . ? O5 C51 1.399(4) . ? O6 C61 1.409(4) . ? N16 C11 1.332(4) . ? N16 C15 1.362(4) . ? N26 C21 1.306(4) . ? N26 C25 1.351(4) . ? N36 C31 1.344(4) . ? N36 C35 1.359(4) . ? N46 C41 1.304(4) . ? N46 C45 1.349(5) . ? N56 C51 1.321(4) . ? N56 C55 1.357(4) . ? N66 C61 1.310(4) . ? N66 C65 1.358(5) . ? C11 C12 1.377(4) . ? C12 C13 1.381(5) . ? C12 H12 0.9500 . ? C13 C14 1.397(5) . ? C13 H13 0.9500 . ? C14 C15 1.369(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C21 C22 1.389(5) . ? C22 C23 1.383(5) . ? C22 H22 0.9500 . ? C23 C24 1.376(6) . ? C23 H23 0.9500 . ? C24 C25 1.377(5) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C31 C32 1.378(4) . ? C32 C33 1.391(5) . ? C32 H32 0.9500 . ? C33 C34 1.388(5) . ? C33 H33 0.9500 . ? C34 C35 1.375(5) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C41 C42 1.369(6) . ? C42 C43 1.394(7) . ? C42 H42 0.9500 . ? C43 C44 1.387(7) . ? C43 H43 0.9500 . ? C44 C45 1.347(6) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C51 C52 1.385(4) . ? C52 C53 1.388(5) . ? C52 H52 0.9500 . ? C53 C54 1.393(6) . ? C53 H53 0.9500 . ? C54 C55 1.381(5) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C61 C62 1.377(5) . ? C62 C63 1.396(5) . ? C62 H62 0.9500 . ? C63 C64 1.368(6) . ? C63 H63 0.9500 . ? C64 C65 1.370(6) . ? C64 H64 0.9500 . ? C65 H65 0.9500 . ? 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 N36 Cu1 N16 175.01(10) . . ? N36 Cu1 N1 91.22(9) . . ? N16 Cu1 N1 92.68(9) . . ? N36 Cu1 Cl1 91.41(7) . . ? N16 Cu1 Cl1 90.51(7) . . ? N1 Cu1 Cl1 105.86(7) . . ? N36 Cu1 Cl2 88.58(7) . . ? N16 Cu1 Cl2 87.28(7) . . ? N1 Cu1 Cl2 107.57(7) . . ? Cl1 Cu1 Cl2 146.56(4) . . ? N3 P1 N1 118.44(13) . . ? N3 P1 O2 112.30(12) . . ? N1 P1 O2 103.95(12) . . ? N3 P1 O1 106.49(12) . . ? N1 P1 O1 108.75(12) . . ? O2 P1 O1 106.30(12) . . ? N2 P2 N1 118.32(13) . . ? N2 P2 O4 112.13(13) . . ? N1 P2 O4 104.52(12) . . ? N2 P2 O3 107.96(12) . . ? N1 P2 O3 108.33(12) . . ? O4 P2 O3 104.73(11) . . ? N2 P3 N3 117.42(13) . . ? N2 P3 O6 110.47(13) . . ? N3 P3 O6 110.37(13) . . ? N2 P3 O5 111.49(13) . . ? N3 P3 O5 111.61(13) . . ? O6 P3 O5 92.80(11) . . ? C11 O1 P1 125.11(18) . . ? C21 O2 P1 124.36(19) . . ? C31 O3 P2 122.34(18) . . ? C41 O4 P2 122.8(2) . . ? C51 O5 P3 123.30(19) . . ? C61 O6 P3 122.23(18) . . ? P1 N1 P2 120.68(15) . . ? P1 N1 Cu1 115.70(13) . . ? P2 N1 Cu1 116.72(13) . . ? P3 N2 P2 122.45(16) . . ? P1 N3 P3 122.12(16) . . ? C11 N16 C15 116.8(3) . . ? C11 N16 Cu1 125.4(2) . . ? C15 N16 Cu1 116.5(2) . . ? C21 N26 C25 115.6(3) . . ? C31 N36 C35 116.9(3) . . ? C31 N36 Cu1 125.18(19) . . ? C35 N36 Cu1 117.4(2) . . ? C41 N46 C45 116.6(3) . . ? C51 N56 C55 115.5(3) . . ? C61 N66 C65 116.0(3) . . ? N16 C11 C12 124.6(3) . . ? N16 C11 O1 118.5(3) . . ? C12 C11 O1 116.8(3) . . ? C11 C12 C13 117.7(3) . . ? C11 C12 H12 121.2 . . ? C13 C12 H12 121.2 . . ? C12 C13 C14 119.4(3) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C15 C14 C13 118.6(3) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? N16 C15 C14 122.8(3) . . ? N16 C15 H15 118.6 . . ? C14 C15 H15 118.6 . . ? N26 C21 C22 126.3(3) . . ? N26 C21 O2 117.2(3) . . ? C22 C21 O2 116.4(3) . . ? C23 C22 C21 116.4(4) . . ? C23 C22 H22 121.8 . . ? C21 C22 H22 121.8 . . ? C24 C23 C22 119.5(4) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C25 118.6(3) . . ? C23 C24 H24 120.7 . . ? C25 C24 H24 120.7 . . ? N26 C25 C24 123.6(4) . . ? N26 C25 H25 118.2 . . ? C24 C25 H25 118.2 . . ? N36 C31 C32 124.5(3) . . ? N36 C31 O3 118.0(2) . . ? C32 C31 O3 117.4(3) . . ? C31 C32 C33 117.4(3) . . ? C31 C32 H32 121.3 . . ? C33 C32 H32 121.3 . . ? C34 C33 C32 119.5(3) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C35 C34 C33 119.1(3) . . ? C35 C34 H34 120.5 . . ? C33 C34 H34 120.5 . . ? N36 C35 C34 122.6(3) . . ? N36 C35 H35 118.7 . . ? C34 C35 H35 118.7 . . ? N46 C41 C42 126.2(4) . . ? N46 C41 O4 117.8(3) . . ? C42 C41 O4 115.8(3) . . ? C41 C42 C43 115.3(5) . . ? C41 C42 H42 122.3 . . ? C43 C42 H42 122.3 . . ? C44 C43 C42 120.1(6) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C45 C44 C43 118.0(5) . . ? C45 C44 H44 121.0 . . ? C43 C44 H44 121.0 . . ? C44 C45 N46 123.5(4) . . ? C44 C45 H45 118.3 . . ? N46 C45 H45 118.3 . . ? N56 C51 C52 126.5(3) . . ? N56 C51 O5 117.6(3) . . ? C52 C51 O5 116.0(3) . . ? C51 C52 C53 116.6(3) . . ? C51 C52 H52 121.7 . . ? C53 C52 H52 121.7 . . ? C52 C53 C54 119.3(3) . . ? C52 C53 H53 120.3 . . ? C54 C53 H53 120.3 . . ? C55 C54 C53 118.5(3) . . ? C55 C54 H54 120.8 . . ? C53 C54 H54 120.8 . . ? N56 C55 C54 123.6(3) . . ? N56 C55 H55 118.2 . . ? C54 C55 H55 118.2 . . ? N66 C61 C62 126.1(3) . . ? N66 C61 O6 115.1(3) . . ? C62 C61 O6 118.6(3) . . ? C61 C62 C63 116.4(4) . . ? C61 C62 H62 121.8 . . ? C63 C62 H62 121.8 . . ? C64 C63 C62 119.4(4) . . ? C64 C63 H63 120.3 . . ? C62 C63 H63 120.3 . . ? C63 C64 C65 119.0(4) . . ? C63 C64 H64 120.5 . . ? C65 C64 H64 120.5 . . ? N66 C65 C64 123.1(4) . . ? N66 C65 H65 118.4 . . ? C64 C65 H65 118.4 . . ? 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 N3 P1 O1 C11 -161.2(2) . . . . ? N1 P1 O1 C11 70.1(2) . . . . ? O2 P1 O1 C11 -41.3(2) . . . . ? N3 P1 O2 C21 46.1(3) . . . . ? N1 P1 O2 C21 175.3(2) . . . . ? O1 P1 O2 C21 -70.0(2) . . . . ? N2 P2 O3 C31 160.0(2) . . . . ? N1 P2 O3 C31 -70.7(2) . . . . ? O4 P2 O3 C31 40.4(2) . . . . ? N2 P2 O4 C41 -44.3(3) . . . . ? N1 P2 O4 C41 -173.6(2) . . . . ? O3 P2 O4 C41 72.5(2) . . . . ? N2 P3 O5 C51 57.1(3) . . . . ? N3 P3 O5 C51 -76.4(2) . . . . ? O6 P3 O5 C51 170.4(2) . . . . ? N2 P3 O6 C61 -61.5(3) . . . . ? N3 P3 O6 C61 70.0(3) . . . . ? O5 P3 O6 C61 -175.7(2) . . . . ? N3 P1 N1 P2 1.7(2) . . . . ? O2 P1 N1 P2 -123.69(17) . . . . ? O1 P1 N1 P2 123.37(16) . . . . ? N3 P1 N1 Cu1 -148.23(13) . . . . ? O2 P1 N1 Cu1 86.37(14) . . . . ? O1 P1 N1 Cu1 -26.58(16) . . . . ? N2 P2 N1 P1 -5.3(2) . . . . ? O4 P2 N1 P1 120.21(17) . . . . ? O3 P2 N1 P1 -128.54(16) . . . . ? N2 P2 N1 Cu1 144.31(13) . . . . ? O4 P2 N1 Cu1 -90.13(14) . . . . ? O3 P2 N1 Cu1 21.11(16) . . . . ? N36 Cu1 N1 P1 167.37(14) . . . . ? N16 Cu1 N1 P1 -9.52(15) . . . . ? Cl1 Cu1 N1 P1 -100.81(13) . . . . ? Cl2 Cu1 N1 P1 78.47(14) . . . . ? N36 Cu1 N1 P2 16.20(15) . . . . ? N16 Cu1 N1 P2 -160.69(14) . . . . ? Cl1 Cu1 N1 P2 108.02(13) . . . . ? Cl2 Cu1 N1 P2 -72.70(14) . . . . ? N3 P3 N2 P2 4.6(2) . . . . ? O6 P3 N2 P2 132.35(17) . . . . ? O5 P3 N2 P2 -125.94(17) . . . . ? N1 P2 N2 P3 2.1(2) . . . . ? O4 P2 N2 P3 -119.65(18) . . . . ? O3 P2 N2 P3 125.49(17) . . . . ? N1 P1 N3 P3 5.4(2) . . . . ? O2 P1 N3 P3 126.64(17) . . . . ? O1 P1 N3 P3 -117.39(18) . . . . ? N2 P3 N3 P1 -8.5(2) . . . . ? O6 P3 N3 P1 -136.26(17) . . . . ? O5 P3 N3 P1 122.02(17) . . . . ? N36 Cu1 N16 C11 -107.9(11) . . . . ? N1 Cu1 N16 C11 33.5(2) . . . . ? Cl1 Cu1 N16 C11 139.4(2) . . . . ? Cl2 Cu1 N16 C11 -74.0(2) . . . . ? N36 Cu1 N16 C15 58.9(12) . . . . ? N1 Cu1 N16 C15 -159.7(2) . . . . ? Cl1 Cu1 N16 C15 -53.8(2) . . . . ? Cl2 Cu1 N16 C15 92.8(2) . . . . ? N16 Cu1 N36 C31 106.3(11) . . . . ? N1 Cu1 N36 C31 -35.1(2) . . . . ? Cl1 Cu1 N36 C31 -141.0(2) . . . . ? Cl2 Cu1 N36 C31 72.4(2) . . . . ? N16 Cu1 N36 C35 -64.9(12) . . . . ? N1 Cu1 N36 C35 153.7(2) . . . . ? Cl1 Cu1 N36 C35 47.8(2) . . . . ? Cl2 Cu1 N36 C35 -98.8(2) . . . . ? C15 N16 C11 C12 -1.7(4) . . . . ? Cu1 N16 C11 C12 165.0(2) . . . . ? C15 N16 C11 O1 -178.2(2) . . . . ? Cu1 N16 C11 O1 -11.5(4) . . . . ? P1 O1 C11 N16 -50.5(3) . . . . ? P1 O1 C11 C12 132.8(3) . . . . ? N16 C11 C12 C13 0.4(5) . . . . ? O1 C11 C12 C13 176.9(3) . . . . ? C11 C12 C13 C14 0.7(5) . . . . ? C12 C13 C14 C15 -0.5(5) . . . . ? C11 N16 C15 C14 1.9(4) . . . . ? Cu1 N16 C15 C14 -166.0(3) . . . . ? C13 C14 C15 N16 -0.9(5) . . . . ? C25 N26 C21 C22 -0.2(5) . . . . ? C25 N26 C21 O2 176.9(3) . . . . ? P1 O2 C21 N26 35.7(4) . . . . ? P1 O2 C21 C22 -146.9(3) . . . . ? N26 C21 C22 C23 0.4(6) . . . . ? O2 C21 C22 C23 -176.7(3) . . . . ? C21 C22 C23 C24 0.1(6) . . . . ? C22 C23 C24 C25 -0.9(6) . . . . ? C21 N26 C25 C24 -0.7(6) . . . . ? C23 C24 C25 N26 1.2(6) . . . . ? C35 N36 C31 C32 0.8(4) . . . . ? Cu1 N36 C31 C32 -170.4(2) . . . . ? C35 N36 C31 O3 178.0(2) . . . . ? Cu1 N36 C31 O3 6.8(4) . . . . ? P2 O3 C31 N36 57.8(3) . . . . ? P2 O3 C31 C32 -124.8(3) . . . . ? N36 C31 C32 C33 0.3(5) . . . . ? O3 C31 C32 C33 -176.9(3) . . . . ? C31 C32 C33 C34 -1.2(5) . . . . ? C32 C33 C34 C35 0.9(5) . . . . ? C31 N36 C35 C34 -1.2(4) . . . . ? Cu1 N36 C35 C34 170.8(2) . . . . ? C33 C34 C35 N36 0.4(5) . . . . ? C45 N46 C41 C42 -4.8(6) . . . . ? C45 N46 C41 O4 179.0(3) . . . . ? P2 O4 C41 N46 -21.3(4) . . . . ? P2 O4 C41 C42 162.2(3) . . . . ? N46 C41 C42 C43 3.0(7) . . . . ? O4 C41 C42 C43 179.3(4) . . . . ? C41 C42 C43 C44 2.0(8) . . . . ? C42 C43 C44 C45 -4.8(8) . . . . ? C43 C44 C45 N46 3.0(8) . . . . ? C41 N46 C45 C44 1.6(7) . . . . ? C55 N56 C51 C52 0.7(5) . . . . ? C55 N56 C51 O5 -178.8(3) . . . . ? P3 O5 C51 N56 9.0(4) . . . . ? P3 O5 C51 C52 -170.5(2) . . . . ? N56 C51 C52 C53 -0.5(5) . . . . ? O5 C51 C52 C53 179.0(3) . . . . ? C51 C52 C53 C54 -0.1(6) . . . . ? C52 C53 C54 C55 0.3(6) . . . . ? C51 N56 C55 C54 -0.4(5) . . . . ? C53 C54 C55 N56 -0.1(6) . . . . ? C65 N66 C61 C62 -0.2(5) . . . . ? C65 N66 C61 O6 -174.7(3) . . . . ? P3 O6 C61 N66 -100.1(3) . . . . ? P3 O6 C61 C62 84.9(3) . . . . ? N66 C61 C62 C63 0.1(5) . . . . ? O6 C61 C62 C63 174.5(3) . . . . ? C61 C62 C63 C64 -0.7(6) . . . . ? C62 C63 C64 C65 1.3(6) . . . . ? C61 N66 C65 C64 0.9(6) . . . . ? C63 C64 C65 N66 -1.5(6) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.422 _refine_diff_density_min -0.868 _refine_diff_density_rms 0.080 #===END data_cd9 _database_code_depnum_ccdc_archive 'CCDC 275487' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H28 Cl5 Cu F6 N9 O6 P4' _chemical_formula_weight 1113.30 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 27.4168(10) _cell_length_b 14.5940(5) _cell_length_c 10.9247(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4371.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 8774 _cell_measurement_theta_min 1.58 _cell_measurement_theta_max 27.53 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2236 _exptl_absorpt_coefficient_mu 1.032 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6653 _exptl_absorpt_correction_T_max 0.8360 _exptl_absorpt_process_details 'blessing, acta cryst. 1995, A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8774 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 27.53 _reflns_number_total 8774 _reflns_number_gt 7400 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0245P)^2^+3.3934P] 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 -0.001(11) _refine_ls_number_reflns 8774 _refine_ls_number_parameters 568 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.0859 _refine_ls_wR_factor_gt 0.0774 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.193133(15) 0.12194(3) 0.79059(4) 0.02777(10) Uani 1 1 d . . . Cl1 Cl 0.21686(3) -0.02321(6) 0.81190(10) 0.0360(2) Uani 1 1 d . . . P1 P 0.14774(3) 0.30279(6) 0.88585(9) 0.0269(2) Uani 1 1 d . . . P2 P 0.18049(4) 0.30053(6) 0.64218(9) 0.0278(2) Uani 1 1 d . . . P3 P 0.14259(4) 0.45730(6) 0.74246(10) 0.0319(2) Uani 1 1 d . . . N1 N 0.17176(10) 0.25165(17) 0.7716(3) 0.0256(6) Uani 1 1 d . . . N2 N 0.15860(12) 0.3990(2) 0.6273(3) 0.0314(7) Uani 1 1 d . . . N3 N 0.13380(11) 0.4049(2) 0.8681(3) 0.0345(7) Uani 1 1 d . . . O1 O 0.09980(9) 0.25408(17) 0.9328(2) 0.0314(6) Uani 1 1 d . . . O2 O 0.18251(10) 0.28498(17) 0.9992(2) 0.0324(6) Uani 1 1 d . . . O3 O 0.16042(10) 0.23209(16) 0.5415(2) 0.0321(6) Uani 1 1 d . . . O4 O 0.23572(9) 0.30691(17) 0.6037(2) 0.0332(6) Uani 1 1 d . . . O5 O 0.09767(10) 0.51978(17) 0.7090(3) 0.0380(7) Uani 1 1 d . . . O6 O 0.17873(9) 0.54109(16) 0.7634(2) 0.0360(7) Uani 1 1 d . . . N16 N 0.12651(12) 0.1038(2) 0.9425(3) 0.0333(7) Uani 1 1 d . . . N26 N 0.23879(11) 0.1752(2) 0.9326(3) 0.0311(7) Uani 1 1 d . . . N36 N 0.14336(11) 0.0959(2) 0.6457(3) 0.0280(7) Uani 1 1 d . . . N46 N 0.25783(12) 0.1567(2) 0.6406(3) 0.0344(7) Uani 1 1 d . . . N56 N 0.04700(13) 0.4007(2) 0.6521(4) 0.0475(9) Uani 1 1 d . . . N66 N 0.24244(11) 0.4423(2) 0.8067(4) 0.0388(7) Uani 1 1 d . . . C11 C 0.09778(13) 0.1674(2) 0.9869(3) 0.0278(8) Uani 1 1 d . . . C12 C 0.06447(14) 0.1569(3) 1.0794(4) 0.0363(9) Uani 1 1 d . . . H12 H 0.0459 0.2065 1.1086 0.044 Uiso 1 1 calc R . . C13 C 0.05950(16) 0.0702(3) 1.1274(4) 0.0416(10) Uani 1 1 d . . . H13 H 0.0372 0.0591 1.1911 0.050 Uiso 1 1 calc R . . C14 C 0.08740(15) 0.0000(3) 1.0814(4) 0.0392(10) Uani 1 1 d . . . H14 H 0.0839 -0.0600 1.1115 0.047 Uiso 1 1 calc R . . C15 C 0.12055(15) 0.0191(3) 0.9906(4) 0.0369(9) Uani 1 1 d . . . H15 H 0.1400 -0.0290 0.9605 0.044 Uiso 1 1 calc R . . C21 C 0.22947(14) 0.2499(2) 0.9990(3) 0.0305(8) Uani 1 1 d . . . C22 C 0.26296(16) 0.2936(3) 1.0740(4) 0.0389(9) Uani 1 1 d . . . H22 H 0.2546 0.3472 1.1167 0.047 Uiso 1 1 calc R . . C23 C 0.30885(17) 0.2562(3) 1.0843(4) 0.0471(12) Uani 1 1 d . . . H23 H 0.3324 0.2833 1.1354 0.057 Uiso 1 1 calc R . . C24 C 0.31974(15) 0.1781(3) 1.0180(4) 0.0473(11) Uani 1 1 d . . . H24 H 0.3509 0.1515 1.0230 0.057 Uiso 1 1 calc R . . C25 C 0.28460(15) 0.1399(3) 0.9451(4) 0.0389(9) Uani 1 1 d . . . H25 H 0.2924 0.0865 0.9013 0.047 Uiso 1 1 calc R . . C31 C 0.13013(14) 0.1575(2) 0.5619(3) 0.0288(8) Uani 1 1 d . . . C32 C 0.09004(15) 0.1500(3) 0.4874(4) 0.0378(9) Uani 1 1 d . . . H32 H 0.0819 0.1966 0.4317 0.045 Uiso 1 1 calc R . . C33 C 0.06205(16) 0.0716(3) 0.4970(4) 0.0426(10) Uani 1 1 d . . . H33 H 0.0344 0.0637 0.4474 0.051 Uiso 1 1 calc R . . C34 C 0.07515(16) 0.0057(3) 0.5798(4) 0.0408(10) Uani 1 1 d . . . H34 H 0.0570 -0.0487 0.5865 0.049 Uiso 1 1 calc R . . C35 C 0.11528(15) 0.0203(3) 0.6530(4) 0.0359(9) Uani 1 1 d . . . H35 H 0.1235 -0.0248 0.7110 0.043 Uiso 1 1 calc R . . C41 C 0.26745(13) 0.2342(3) 0.5847(3) 0.0307(8) Uani 1 1 d . . . C42 C 0.30693(16) 0.2518(3) 0.5106(4) 0.0436(11) Uani 1 1 d . . . H42 H 0.3114 0.3093 0.4735 0.052 Uiso 1 1 calc R . . C43 C 0.33955(16) 0.1812(3) 0.4936(5) 0.0544(13) Uani 1 1 d . . . H43 H 0.3672 0.1894 0.4439 0.065 Uiso 1 1 calc R . . C44 C 0.33108(15) 0.0978(3) 0.5506(4) 0.0436(10) Uani 1 1 d . . . H44 H 0.3531 0.0489 0.5412 0.052 Uiso 1 1 calc R . . C45 C 0.29051(14) 0.0880(3) 0.6199(4) 0.0366(9) Uani 1 1 d . . . H45 H 0.2845 0.0305 0.6558 0.044 Uiso 1 1 calc R . . C51 C 0.05483(14) 0.4891(3) 0.6556(4) 0.0366(9) Uani 1 1 d . . . C52 C 0.02447(16) 0.5561(3) 0.6088(4) 0.0461(11) Uani 1 1 d . . . H52 H 0.0319 0.6187 0.6164 0.055 Uiso 1 1 calc R . . C53 C -0.01720(19) 0.5266(4) 0.5503(5) 0.0716(17) Uani 1 1 d . . . H53 H -0.0394 0.5690 0.5174 0.086 Uiso 1 1 calc R . . C54 C -0.02578(18) 0.4329(5) 0.5409(6) 0.078(2) Uani 1 1 d . . . H54 H -0.0532 0.4108 0.4986 0.094 Uiso 1 1 calc R . . C55 C 0.00620(19) 0.3742(4) 0.5937(5) 0.0654(16) Uani 1 1 d . . . H55 H -0.0006 0.3111 0.5894 0.078 Uiso 1 1 calc R . . C61 C 0.22813(13) 0.5268(2) 0.7863(4) 0.0359(8) Uani 1 1 d . . . C62 C 0.25803(15) 0.6033(3) 0.7835(4) 0.0445(10) Uani 1 1 d . . . H62 H 0.2454 0.6624 0.7701 0.053 Uiso 1 1 calc R . . C63 C 0.30706(15) 0.5887(3) 0.8013(5) 0.0531(11) Uani 1 1 d . . . H63 H 0.3290 0.6382 0.8000 0.064 Uiso 1 1 calc R . . C64 C 0.32383(15) 0.5002(3) 0.8210(4) 0.0510(11) Uani 1 1 d . . . H64 H 0.3573 0.4886 0.8322 0.061 Uiso 1 1 calc R . . C65 C 0.29075(15) 0.4303(3) 0.8239(4) 0.0465(11) Uani 1 1 d . . . H65 H 0.3022 0.3706 0.8387 0.056 Uiso 1 1 calc R . . P4 P 0.05020(3) 0.79531(6) 0.81338(10) 0.0311(2) Uani 1 1 d . . . F11 F 0.04847(9) 0.79299(17) 0.6658(2) 0.0465(6) Uani 1 1 d . . . F12 F -0.00602(8) 0.76598(16) 0.8171(3) 0.0507(6) Uani 1 1 d . . . F13 F 0.05169(10) 0.79766(16) 0.9586(2) 0.0453(6) Uani 1 1 d . . . F14 F 0.06574(8) 0.69040(13) 0.8145(2) 0.0436(6) Uani 1 1 d . . . F15 F 0.10613(7) 0.82537(14) 0.8082(3) 0.0457(6) Uani 1 1 d . . . F16 F 0.03462(8) 0.90097(13) 0.8111(2) 0.0437(5) Uani 1 1 d . . . C100 C 0.40668(19) 0.9081(3) 0.8496(4) 0.0562(13) Uani 1 1 d . . . H10A H 0.3959 0.8912 0.9321 0.067 Uiso 1 1 calc R . . H10B H 0.4407 0.8887 0.8404 0.067 Uiso 1 1 calc R . . C200 C 0.0331(3) 0.7756(4) 0.3535(6) 0.093(2) Uani 1 1 d . . . H20A H 0.0347 0.7818 0.4427 0.112 Uiso 1 1 calc R . . H20B H 0.0158 0.7186 0.3347 0.112 Uiso 1 1 calc R . . Cl10 Cl 0.37043(6) 0.85148(10) 0.74062(14) 0.0798(4) Uani 1 1 d . . . Cl11 Cl 0.40267(6) 1.02737(9) 0.83147(13) 0.0722(4) Uani 1 1 d . . . Cl20 Cl 0.09200(7) 0.76981(12) 0.2943(3) 0.1246(8) Uani 1 1 d . . . Cl21 Cl 0.00062(6) 0.86819(11) 0.2927(2) 0.0943(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0307(2) 0.02279(18) 0.0298(2) 0.0007(2) 0.0008(2) 0.00268(17) Cl1 0.0383(5) 0.0258(4) 0.0440(6) 0.0056(4) 0.0086(5) 0.0065(3) P1 0.0272(5) 0.0248(4) 0.0288(5) -0.0019(4) 0.0016(4) 0.0003(4) P2 0.0334(5) 0.0227(4) 0.0274(5) 0.0013(4) 0.0013(4) 0.0001(4) P3 0.0343(5) 0.0213(4) 0.0400(5) -0.0016(4) -0.0044(4) 0.0020(4) N1 0.0272(14) 0.0220(13) 0.0277(17) -0.0007(12) -0.0004(12) 0.0025(11) N2 0.0387(18) 0.0249(15) 0.0305(18) 0.0022(13) -0.0015(14) 0.0029(13) N3 0.0363(18) 0.0270(16) 0.040(2) -0.0066(14) 0.0041(15) 0.0039(14) O1 0.0264(13) 0.0281(13) 0.0398(15) 0.0004(11) 0.0064(11) 0.0012(10) O2 0.0342(14) 0.0357(14) 0.0273(14) -0.0067(12) -0.0013(11) 0.0043(11) O3 0.0444(15) 0.0270(13) 0.0250(14) 0.0011(10) -0.0003(11) -0.0053(11) O4 0.0321(14) 0.0250(13) 0.0424(16) 0.0028(11) 0.0106(12) -0.0008(11) O5 0.0367(14) 0.0240(13) 0.0532(18) -0.0062(12) -0.0122(12) 0.0049(12) O6 0.0364(14) 0.0235(12) 0.0482(19) 0.0016(11) -0.0077(12) -0.0017(10) N16 0.0370(18) 0.0294(17) 0.0334(18) -0.0022(14) 0.0062(14) -0.0008(14) N26 0.0286(16) 0.0356(17) 0.0290(17) 0.0026(14) 0.0021(13) 0.0001(14) N36 0.0348(17) 0.0253(15) 0.0239(16) -0.0009(12) 0.0026(14) -0.0024(13) N46 0.0363(18) 0.0296(16) 0.0371(19) 0.0011(15) 0.0064(15) 0.0020(14) N56 0.048(2) 0.0375(19) 0.057(2) -0.0118(17) 0.0058(19) -0.0105(17) N66 0.0357(17) 0.0333(15) 0.047(2) 0.0020(17) -0.0045(17) -0.0004(13) C11 0.0242(18) 0.0297(19) 0.029(2) 0.0003(15) 0.0011(15) -0.0028(15) C12 0.029(2) 0.042(2) 0.037(2) -0.0028(19) 0.0093(17) -0.0022(17) C13 0.039(2) 0.054(3) 0.032(2) 0.003(2) 0.0113(18) -0.007(2) C14 0.042(2) 0.035(2) 0.040(2) 0.0063(18) 0.0057(19) -0.0114(19) C15 0.047(2) 0.0268(19) 0.037(2) 0.0014(17) 0.0081(19) 0.0018(17) C21 0.034(2) 0.0320(19) 0.0259(19) 0.0056(16) 0.0004(16) 0.0002(16) C22 0.046(2) 0.037(2) 0.033(2) 0.0022(17) -0.0053(18) -0.0063(19) C23 0.041(3) 0.055(3) 0.046(3) 0.007(2) -0.010(2) -0.012(2) C24 0.028(2) 0.066(3) 0.048(3) 0.012(2) -0.003(2) 0.002(2) C25 0.035(2) 0.044(2) 0.037(2) 0.0043(18) -0.0034(18) 0.0072(19) C31 0.036(2) 0.0251(18) 0.026(2) -0.0024(15) 0.0015(16) -0.0007(15) C32 0.044(2) 0.033(2) 0.036(2) 0.0014(17) -0.0009(19) 0.0029(18) C33 0.038(2) 0.048(3) 0.042(3) 0.003(2) -0.0034(19) -0.005(2) C34 0.046(2) 0.039(2) 0.038(2) 0.0007(18) 0.002(2) -0.0107(19) C35 0.044(2) 0.030(2) 0.033(2) 0.0026(17) 0.0012(18) -0.0027(17) C41 0.0280(19) 0.0298(19) 0.035(2) -0.0019(16) 0.0016(16) -0.0026(16) C42 0.039(3) 0.041(3) 0.051(3) 0.006(2) 0.014(2) -0.0074(19) C43 0.038(2) 0.053(3) 0.072(4) 0.006(2) 0.026(2) 0.001(2) C44 0.037(2) 0.046(2) 0.048(3) 0.001(2) 0.011(2) 0.0056(19) C45 0.037(2) 0.033(2) 0.040(2) 0.0022(18) 0.0062(18) 0.0018(18) C51 0.031(2) 0.040(2) 0.038(2) -0.0131(18) -0.0003(17) -0.0009(17) C52 0.044(3) 0.048(3) 0.046(3) -0.010(2) -0.006(2) 0.012(2) C53 0.049(3) 0.098(4) 0.067(4) -0.030(3) -0.023(3) 0.023(3) C54 0.032(3) 0.112(5) 0.091(5) -0.059(4) 0.001(3) -0.007(3) C55 0.048(3) 0.069(3) 0.080(4) -0.036(3) 0.015(3) -0.026(3) C61 0.0374(19) 0.0371(19) 0.033(2) 0.0035(18) -0.0090(18) -0.0044(16) C62 0.049(2) 0.039(2) 0.046(3) 0.011(2) -0.012(2) -0.0082(18) C63 0.047(2) 0.059(3) 0.053(3) 0.007(3) -0.013(3) -0.022(2) C64 0.037(2) 0.066(3) 0.050(3) 0.007(2) -0.006(2) -0.004(2) C65 0.042(2) 0.048(2) 0.049(3) 0.006(2) 0.000(2) 0.0064(19) P4 0.0299(4) 0.0292(4) 0.0344(6) 0.0045(4) -0.0022(4) 0.0013(4) F11 0.0605(17) 0.0480(14) 0.0309(13) 0.0032(11) -0.0033(11) 0.0021(12) F12 0.0323(11) 0.0596(14) 0.0602(17) 0.0071(14) -0.0037(13) -0.0062(10) F13 0.0651(17) 0.0413(14) 0.0297(13) 0.0036(10) -0.0014(12) -0.0058(13) F14 0.0522(13) 0.0301(10) 0.0485(15) -0.0015(11) -0.0129(13) 0.0045(9) F15 0.0308(11) 0.0435(12) 0.0628(16) 0.0024(13) -0.0017(12) -0.0033(9) F16 0.0498(13) 0.0326(11) 0.0485(15) 0.0047(12) 0.0041(13) 0.0108(9) C100 0.075(3) 0.055(3) 0.038(3) -0.001(2) -0.010(2) 0.006(3) C200 0.138(6) 0.073(4) 0.067(4) 0.018(3) 0.012(4) -0.009(4) Cl10 0.1060(12) 0.0698(9) 0.0635(9) -0.0127(7) -0.0211(9) -0.0096(8) Cl11 0.0944(10) 0.0578(7) 0.0644(9) -0.0020(6) -0.0060(8) -0.0035(7) Cl20 0.0959(12) 0.0897(11) 0.188(2) 0.0434(16) -0.0321(16) 0.0122(10) Cl21 0.0929(11) 0.0849(9) 0.1050(12) 0.0368(10) 0.0372(11) 0.0109(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.993(3) . ? Cu1 N36 2.124(3) . ? Cu1 N26 2.140(3) . ? Cu1 Cl1 2.2281(9) . ? Cu1 N46 2.467(3) . ? Cu1 N16 2.482(3) . ? P1 N3 1.550(3) . ? P1 O1 1.580(3) . ? P1 O2 1.584(3) . ? P1 N1 1.597(3) . ? P2 N2 1.566(3) . ? P2 O4 1.574(3) . ? P2 O3 1.585(3) . ? P2 N1 1.601(3) . ? P3 O5 1.575(3) . ? P3 N2 1.581(3) . ? P3 N3 1.589(3) . ? P3 O6 1.591(3) . ? O1 C11 1.397(4) . ? O2 C21 1.385(4) . ? O3 C31 1.388(4) . ? O4 C41 1.388(4) . ? O5 C51 1.386(5) . ? O6 C61 1.393(4) . ? N16 C11 1.311(5) . ? N16 C15 1.353(5) . ? N26 C21 1.334(5) . ? N26 C25 1.364(5) . ? N36 C31 1.334(5) . ? N36 C35 1.348(5) . ? N46 C41 1.312(5) . ? N46 C45 1.364(5) . ? N56 C51 1.308(5) . ? N56 C55 1.345(6) . ? N66 C61 1.313(4) . ? N66 C65 1.349(5) . ? C11 C12 1.371(5) . ? C12 C13 1.377(6) . ? C12 H12 0.9400 . ? C13 C14 1.374(6) . ? C13 H13 0.9400 . ? C14 C15 1.374(5) . ? C14 H14 0.9400 . ? C15 H15 0.9400 . ? C21 C22 1.386(5) . ? C22 C23 1.376(6) . ? C22 H22 0.9400 . ? C23 C24 1.383(7) . ? C23 H23 0.9400 . ? C24 C25 1.369(6) . ? C24 H24 0.9400 . ? C25 H25 0.9400 . ? C31 C32 1.372(5) . ? C32 C33 1.381(6) . ? C32 H32 0.9400 . ? C33 C34 1.368(6) . ? C33 H33 0.9400 . ? C34 C35 1.377(6) . ? C34 H34 0.9400 . ? C35 H35 0.9400 . ? C41 C42 1.376(5) . ? C42 C43 1.377(6) . ? C42 H42 0.9400 . ? C43 C44 1.387(6) . ? C43 H43 0.9400 . ? C44 C45 1.353(6) . ? C44 H44 0.9400 . ? C45 H45 0.9400 . ? C51 C52 1.383(6) . ? C52 C53 1.378(6) . ? C52 H52 0.9400 . ? C53 C54 1.391(8) . ? C53 H53 0.9400 . ? C54 C55 1.356(8) . ? C54 H54 0.9400 . ? C55 H55 0.9400 . ? C61 C62 1.385(5) . ? C62 C63 1.375(6) . ? C62 H62 0.9400 . ? C63 C64 1.388(6) . ? C63 H63 0.9400 . ? C64 C65 1.365(6) . ? C64 H64 0.9400 . ? C65 H65 0.9400 . ? P4 F13 1.588(2) . ? P4 F14 1.589(2) . ? P4 F15 1.596(2) . ? P4 F12 1.600(2) . ? P4 F16 1.600(2) . ? P4 F11 1.614(3) . ? C100 Cl11 1.756(5) . ? C100 Cl10 1.757(5) . ? C100 H10A 0.9800 . ? C100 H10B 0.9800 . ? C200 Cl20 1.742(7) . ? C200 Cl21 1.749(6) . ? C200 H20A 0.9800 . ? C200 H20B 0.9800 . ? 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 N1 Cu1 N36 84.47(11) . . ? N1 Cu1 N26 84.41(12) . . ? N36 Cu1 N26 168.87(12) . . ? N1 Cu1 Cl1 179.87(9) . . ? N36 Cu1 Cl1 95.45(8) . . ? N26 Cu1 Cl1 95.67(9) . . ? N1 Cu1 N46 86.95(11) . . ? N36 Cu1 N46 90.22(11) . . ? N26 Cu1 N46 89.21(11) . . ? Cl1 Cu1 N46 93.15(8) . . ? N1 Cu1 N16 87.41(11) . . ? N36 Cu1 N16 90.35(11) . . ? N26 Cu1 N16 89.12(11) . . ? Cl1 Cu1 N16 92.49(8) . . ? N46 Cu1 N16 174.25(11) . . ? N3 P1 O1 105.53(16) . . ? N3 P1 O2 113.84(16) . . ? O1 P1 O2 99.97(15) . . ? N3 P1 N1 116.92(16) . . ? O1 P1 N1 112.75(15) . . ? O2 P1 N1 106.63(14) . . ? N2 P2 O4 106.65(16) . . ? N2 P2 O3 111.93(16) . . ? O4 P2 O3 100.72(15) . . ? N2 P2 N1 116.31(16) . . ? O4 P2 N1 113.93(15) . . ? O3 P2 N1 106.28(14) . . ? O5 P3 N2 110.09(16) . . ? O5 P3 N3 111.14(17) . . ? N2 P3 N3 118.04(16) . . ? O5 P3 O6 94.33(13) . . ? N2 P3 O6 110.81(16) . . ? N3 P3 O6 109.89(16) . . ? P1 N1 P2 122.93(17) . . ? P1 N1 Cu1 118.94(16) . . ? P2 N1 Cu1 118.12(15) . . ? P2 N2 P3 121.2(2) . . ? P1 N3 P3 122.2(2) . . ? C11 O1 P1 125.3(2) . . ? C21 O2 P1 128.2(2) . . ? C31 O3 P2 126.2(2) . . ? C41 O4 P2 126.7(2) . . ? C51 O5 P3 125.0(2) . . ? C61 O6 P3 121.1(2) . . ? C11 N16 C15 115.5(3) . . ? C11 N16 Cu1 127.9(2) . . ? C15 N16 Cu1 116.5(3) . . ? C21 N26 C25 115.5(3) . . ? C21 N26 Cu1 125.4(3) . . ? C25 N26 Cu1 118.3(3) . . ? C31 N36 C35 115.9(3) . . ? C31 N36 Cu1 124.4(2) . . ? C35 N36 Cu1 118.0(3) . . ? C41 N46 C45 115.1(3) . . ? C41 N46 Cu1 129.1(3) . . ? C45 N46 Cu1 115.5(3) . . ? C51 N56 C55 115.8(4) . . ? C61 N66 C65 116.1(3) . . ? N16 C11 C12 126.4(4) . . ? N16 C11 O1 117.5(3) . . ? C12 C11 O1 116.0(3) . . ? C11 C12 C13 116.7(4) . . ? C11 C12 H12 121.6 . . ? C13 C12 H12 121.6 . . ? C14 C13 C12 119.4(4) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 118.8(4) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? N16 C15 C14 123.1(4) . . ? N16 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? N26 C21 O2 118.7(3) . . ? N26 C21 C22 124.7(4) . . ? O2 C21 C22 116.4(3) . . ? C23 C22 C21 118.2(4) . . ? C23 C22 H22 120.9 . . ? C21 C22 H22 120.9 . . ? C22 C23 C24 118.8(4) . . ? C22 C23 H23 120.6 . . ? C24 C23 H23 120.6 . . ? C25 C24 C23 119.2(4) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? N26 C25 C24 123.6(4) . . ? N26 C25 H25 118.2 . . ? C24 C25 H25 118.2 . . ? N36 C31 C32 124.9(3) . . ? N36 C31 O3 118.5(3) . . ? C32 C31 O3 116.5(3) . . ? C31 C32 C33 117.8(4) . . ? C31 C32 H32 121.1 . . ? C33 C32 H32 121.1 . . ? C34 C33 C32 119.1(4) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C33 C34 C35 119.0(4) . . ? C33 C34 H34 120.5 . . ? C35 C34 H34 120.5 . . ? N36 C35 C34 123.2(4) . . ? N36 C35 H35 118.4 . . ? C34 C35 H35 118.4 . . ? N46 C41 C42 126.4(4) . . ? N46 C41 O4 117.6(3) . . ? C42 C41 O4 116.0(3) . . ? C41 C42 C43 116.8(4) . . ? C41 C42 H42 121.6 . . ? C43 C42 H42 121.6 . . ? C42 C43 C44 119.2(4) . . ? C42 C43 H43 120.4 . . ? C44 C43 H43 120.4 . . ? C45 C44 C43 118.8(4) . . ? C45 C44 H44 120.6 . . ? C43 C44 H44 120.6 . . ? C44 C45 N46 123.7(4) . . ? C44 C45 H45 118.1 . . ? N46 C45 H45 118.1 . . ? N56 C51 C52 126.0(4) . . ? N56 C51 O5 118.0(4) . . ? C52 C51 O5 115.9(4) . . ? C53 C52 C51 116.7(5) . . ? C53 C52 H52 121.7 . . ? C51 C52 H52 121.7 . . ? C52 C53 C54 118.8(5) . . ? C52 C53 H53 120.6 . . ? C54 C53 H53 120.6 . . ? C55 C54 C53 118.7(5) . . ? C55 C54 H54 120.6 . . ? C53 C54 H54 120.6 . . ? N56 C55 C54 123.9(5) . . ? N56 C55 H55 118.0 . . ? C54 C55 H55 118.0 . . ? N66 C61 C62 125.7(4) . . ? N66 C61 O6 117.5(3) . . ? C62 C61 O6 116.8(3) . . ? C63 C62 C61 116.8(4) . . ? C63 C62 H62 121.6 . . ? C61 C62 H62 121.6 . . ? C62 C63 C64 119.4(4) . . ? C62 C63 H63 120.3 . . ? C64 C63 H63 120.3 . . ? C65 C64 C63 118.6(4) . . ? C65 C64 H64 120.7 . . ? C63 C64 H64 120.7 . . ? N66 C65 C64 123.5(4) . . ? N66 C65 H65 118.3 . . ? C64 C65 H65 118.3 . . ? F13 P4 F14 90.35(14) . . ? F13 P4 F15 90.28(15) . . ? F14 P4 F15 90.44(12) . . ? F13 P4 F12 90.31(15) . . ? F14 P4 F12 90.02(13) . . ? F15 P4 F12 179.25(16) . . ? F13 P4 F16 90.08(14) . . ? F14 P4 F16 179.57(17) . . ? F15 P4 F16 89.49(12) . . ? F12 P4 F16 90.05(12) . . ? F13 P4 F11 179.79(15) . . ? F14 P4 F11 89.75(14) . . ? F15 P4 F11 89.91(15) . . ? F12 P4 F11 89.50(15) . . ? F16 P4 F11 89.82(13) . . ? Cl11 C100 Cl10 110.8(3) . . ? Cl11 C100 H10A 109.5 . . ? Cl10 C100 H10A 109.5 . . ? Cl11 C100 H10B 109.5 . . ? Cl10 C100 H10B 109.5 . . ? H10A C100 H10B 108.1 . . ? Cl20 C200 Cl21 111.6(3) . . ? Cl20 C200 H20A 109.3 . . ? Cl21 C200 H20A 109.3 . . ? Cl20 C200 H20B 109.3 . . ? Cl21 C200 H20B 109.3 . . ? H20A C200 H20B 108.0 . . ? 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 N3 P1 N1 P2 -1.4(3) . . . . ? O1 P1 N1 P2 121.2(2) . . . . ? O2 P1 N1 P2 -130.0(2) . . . . ? N3 P1 N1 Cu1 177.42(17) . . . . ? O1 P1 N1 Cu1 -60.0(2) . . . . ? O2 P1 N1 Cu1 48.7(2) . . . . ? N2 P2 N1 P1 -6.9(3) . . . . ? O4 P2 N1 P1 117.7(2) . . . . ? O3 P2 N1 P1 -132.3(2) . . . . ? N2 P2 N1 Cu1 174.25(16) . . . . ? O4 P2 N1 Cu1 -61.1(2) . . . . ? O3 P2 N1 Cu1 48.9(2) . . . . ? N36 Cu1 N1 P1 120.96(19) . . . . ? N26 Cu1 N1 P1 -59.02(18) . . . . ? Cl1 Cu1 N1 P1 69(84) . . . . ? N46 Cu1 N1 P1 -148.52(18) . . . . ? N16 Cu1 N1 P1 30.36(18) . . . . ? N36 Cu1 N1 P2 -60.18(18) . . . . ? N26 Cu1 N1 P2 119.84(18) . . . . ? Cl1 Cu1 N1 P2 -112(92) . . . . ? N46 Cu1 N1 P2 30.33(18) . . . . ? N16 Cu1 N1 P2 -150.79(18) . . . . ? O4 P2 N2 P3 -111.4(2) . . . . ? O3 P2 N2 P3 139.3(2) . . . . ? N1 P2 N2 P3 16.9(3) . . . . ? O5 P3 N2 P2 -147.4(2) . . . . ? N3 P3 N2 P2 -18.4(3) . . . . ? O6 P3 N2 P2 109.6(2) . . . . ? O1 P1 N3 P3 -126.1(2) . . . . ? O2 P1 N3 P3 125.3(2) . . . . ? N1 P1 N3 P3 0.1(3) . . . . ? O5 P3 N3 P1 137.9(2) . . . . ? N2 P3 N3 P1 9.4(3) . . . . ? O6 P3 N3 P1 -119.0(2) . . . . ? N3 P1 O1 C11 -164.7(3) . . . . ? O2 P1 O1 C11 -46.4(3) . . . . ? N1 P1 O1 C11 66.5(3) . . . . ? N3 P1 O2 C21 -117.7(3) . . . . ? O1 P1 O2 C21 130.3(3) . . . . ? N1 P1 O2 C21 12.8(3) . . . . ? N2 P2 O3 C31 -112.6(3) . . . . ? O4 P2 O3 C31 134.4(3) . . . . ? N1 P2 O3 C31 15.4(3) . . . . ? N2 P2 O4 C41 -169.5(3) . . . . ? O3 P2 O4 C41 -52.5(3) . . . . ? N1 P2 O4 C41 60.8(3) . . . . ? N2 P3 O5 C51 52.3(4) . . . . ? N3 P3 O5 C51 -80.4(4) . . . . ? O6 P3 O5 C51 166.4(3) . . . . ? O5 P3 O6 C61 -174.1(3) . . . . ? N2 P3 O6 C61 -60.7(3) . . . . ? N3 P3 O6 C61 71.5(3) . . . . ? N1 Cu1 N16 C11 -6.5(3) . . . . ? N36 Cu1 N16 C11 -90.9(3) . . . . ? N26 Cu1 N16 C11 78.0(3) . . . . ? Cl1 Cu1 N16 C11 173.6(3) . . . . ? N46 Cu1 N16 C11 4.8(13) . . . . ? N1 Cu1 N16 C15 177.4(3) . . . . ? N36 Cu1 N16 C15 92.9(3) . . . . ? N26 Cu1 N16 C15 -98.2(3) . . . . ? Cl1 Cu1 N16 C15 -2.6(3) . . . . ? N46 Cu1 N16 C15 -171.4(10) . . . . ? N1 Cu1 N26 C21 27.5(3) . . . . ? N36 Cu1 N26 C21 27.4(8) . . . . ? Cl1 Cu1 N26 C21 -152.4(3) . . . . ? N46 Cu1 N26 C21 114.5(3) . . . . ? N16 Cu1 N26 C21 -60.0(3) . . . . ? N1 Cu1 N26 C25 -141.5(3) . . . . ? N36 Cu1 N26 C25 -141.6(5) . . . . ? Cl1 Cu1 N26 C25 38.6(3) . . . . ? N46 Cu1 N26 C25 -54.5(3) . . . . ? N16 Cu1 N26 C25 131.0(3) . . . . ? N1 Cu1 N36 C31 26.0(3) . . . . ? N26 Cu1 N36 C31 26.1(8) . . . . ? Cl1 Cu1 N36 C31 -154.1(3) . . . . ? N46 Cu1 N36 C31 -60.9(3) . . . . ? N16 Cu1 N36 C31 113.4(3) . . . . ? N1 Cu1 N36 C35 -138.8(3) . . . . ? N26 Cu1 N36 C35 -138.7(6) . . . . ? Cl1 Cu1 N36 C35 41.1(3) . . . . ? N46 Cu1 N36 C35 134.3(3) . . . . ? N16 Cu1 N36 C35 -51.4(3) . . . . ? N1 Cu1 N46 C41 0.7(3) . . . . ? N36 Cu1 N46 C41 85.1(3) . . . . ? N26 Cu1 N46 C41 -83.7(4) . . . . ? Cl1 Cu1 N46 C41 -179.4(3) . . . . ? N16 Cu1 N46 C41 -10.6(14) . . . . ? N1 Cu1 N46 C45 175.0(3) . . . . ? N36 Cu1 N46 C45 -100.5(3) . . . . ? N26 Cu1 N46 C45 90.6(3) . . . . ? Cl1 Cu1 N46 C45 -5.1(3) . . . . ? N16 Cu1 N46 C45 163.7(10) . . . . ? C15 N16 C11 C12 3.0(6) . . . . ? Cu1 N16 C11 C12 -173.2(3) . . . . ? C15 N16 C11 O1 -174.8(3) . . . . ? Cu1 N16 C11 O1 9.0(5) . . . . ? P1 O1 C11 N16 -38.4(5) . . . . ? P1 O1 C11 C12 143.6(3) . . . . ? N16 C11 C12 C13 -2.5(6) . . . . ? O1 C11 C12 C13 175.3(3) . . . . ? C11 C12 C13 C14 -0.1(6) . . . . ? C12 C13 C14 C15 1.8(6) . . . . ? C11 N16 C15 C14 -1.1(6) . . . . ? Cu1 N16 C15 C14 175.6(3) . . . . ? C13 C14 C15 N16 -1.2(7) . . . . ? C25 N26 C21 O2 -174.5(3) . . . . ? Cu1 N26 C21 O2 16.2(5) . . . . ? C25 N26 C21 C22 2.0(5) . . . . ? Cu1 N26 C21 C22 -167.3(3) . . . . ? P1 O2 C21 N26 -46.7(5) . . . . ? P1 O2 C21 C22 136.5(3) . . . . ? N26 C21 C22 C23 -2.0(6) . . . . ? O2 C21 C22 C23 174.6(4) . . . . ? C21 C22 C23 C24 1.1(6) . . . . ? C22 C23 C24 C25 -0.5(7) . . . . ? C21 N26 C25 C24 -1.3(6) . . . . ? Cu1 N26 C25 C24 168.8(3) . . . . ? C23 C24 C25 N26 0.6(7) . . . . ? C35 N36 C31 C32 2.0(6) . . . . ? Cu1 N36 C31 C32 -163.1(3) . . . . ? C35 N36 C31 O3 -173.5(3) . . . . ? Cu1 N36 C31 O3 21.4(5) . . . . ? P2 O3 C31 N36 -52.9(4) . . . . ? P2 O3 C31 C32 131.3(3) . . . . ? N36 C31 C32 C33 -2.1(6) . . . . ? O3 C31 C32 C33 173.4(3) . . . . ? C31 C32 C33 C34 0.3(6) . . . . ? C32 C33 C34 C35 1.4(7) . . . . ? C31 N36 C35 C34 -0.1(6) . . . . ? Cu1 N36 C35 C34 166.0(3) . . . . ? C33 C34 C35 N36 -1.6(7) . . . . ? C45 N46 C41 C42 -1.0(6) . . . . ? Cu1 N46 C41 C42 173.3(3) . . . . ? C45 N46 C41 O4 -179.2(3) . . . . ? Cu1 N46 C41 O4 -4.9(5) . . . . ? P2 O4 C41 N46 -24.7(5) . . . . ? P2 O4 C41 C42 156.9(3) . . . . ? N46 C41 C42 C43 0.0(7) . . . . ? O4 C41 C42 C43 178.2(4) . . . . ? C41 C42 C43 C44 0.1(7) . . . . ? C42 C43 C44 C45 1.0(8) . . . . ? C43 C44 C45 N46 -2.2(7) . . . . ? C41 N46 C45 C44 2.1(6) . . . . ? Cu1 N46 C45 C44 -173.0(3) . . . . ? C55 N56 C51 C52 2.2(7) . . . . ? C55 N56 C51 O5 -176.6(4) . . . . ? P3 O5 C51 N56 12.8(6) . . . . ? P3 O5 C51 C52 -166.1(3) . . . . ? N56 C51 C52 C53 -1.8(7) . . . . ? O5 C51 C52 C53 177.1(4) . . . . ? C51 C52 C53 C54 -0.7(8) . . . . ? C52 C53 C54 C55 2.6(9) . . . . ? C51 N56 C55 C54 -0.1(8) . . . . ? C53 C54 C55 N56 -2.3(9) . . . . ? C65 N66 C61 C62 -1.4(7) . . . . ? C65 N66 C61 O6 177.6(4) . . . . ? P3 O6 C61 N66 -9.3(5) . . . . ? P3 O6 C61 C62 169.8(3) . . . . ? N66 C61 C62 C63 1.4(8) . . . . ? O6 C61 C62 C63 -177.5(4) . . . . ? C61 C62 C63 C64 -0.2(8) . . . . ? C62 C63 C64 C65 -0.9(8) . . . . ? C61 N66 C65 C64 0.1(7) . . . . ? C63 C64 C65 N66 1.0(8) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.409 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.072 #===END data_cdmecu _database_code_depnum_ccdc_archive 'CCDC 275488' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37.75 H37.75 Cl9.25 Cu2 N9 O6 P3' _chemical_formula_weight 1261.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.215(8) _cell_length_b 17.897(5) _cell_length_c 16.594(4) _cell_angle_alpha 90.00 _cell_angle_beta 121.937(4) _cell_angle_gamma 90.00 _cell_volume 6607(3) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 4318 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 22.50 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.96 _exptl_crystal_size_mid 0.54 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2572 _exptl_absorpt_coefficient_mu 1.131 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Electron density from 7CHCl3 molecules per unit cell removed using Platon / Squeeze. Corrections to F000, mu, Dcalc and molecular weight included in cif. ; _diffrn_ambient_temperature 168(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30794 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4318 _reflns_number_gt 3776 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+12.2566P] 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 4318 _refine_ls_number_parameters 273 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.1106 _refine_ls_wR_factor_gt 0.1079 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 1.049732(18) 0.29386(2) 0.60829(3) 0.02679(16) Uani 1 1 d . . . Cl1 Cl 1.14657(4) 0.33534(6) 0.68364(7) 0.0425(3) Uani 1 1 d . . . Cl2 Cl 0.96221(4) 0.28835(5) 0.46346(6) 0.0367(2) Uani 1 1 d . . . P1 P 1.04050(4) 0.14930(5) 0.72150(6) 0.0240(2) Uani 1 1 d . . . P2 P 1.0000 0.28321(6) 0.7500 0.0205(3) Uani 1 2 d S . . O1 O 1.02381(10) 0.11700(13) 0.62153(16) 0.0294(6) Uani 1 1 d . . . O2 O 1.10890(10) 0.12435(12) 0.78186(16) 0.0277(5) Uani 1 1 d . . . O3 O 1.04594(9) 0.33863(12) 0.83170(15) 0.0232(5) Uani 1 1 d . . . N1 N 1.03615(11) 0.23826(14) 0.71471(18) 0.0227(6) Uani 1 1 d . . . N2 N 1.0000 0.1069(2) 0.7500 0.0296(9) Uani 1 2 d S . . N16 N 1.07532(13) 0.19527(16) 0.5761(2) 0.0309(7) Uani 1 1 d . . . N26 N 1.11885(13) 0.17961(17) 0.9151(2) 0.0316(7) Uani 1 1 d . . . N36 N 1.02043(12) 0.39445(15) 0.63334(19) 0.0270(7) Uani 1 1 d . . . C11 C 1.05890(15) 0.12675(19) 0.5824(2) 0.0284(8) Uani 1 1 d . . . C12 C 1.07150(17) 0.0636(2) 0.5493(3) 0.0399(10) Uani 1 1 d . . . H12 H 1.0586 0.0159 0.5567 0.048 Uiso 1 1 calc R . . C13 C 1.10349(18) 0.0708(2) 0.5049(3) 0.0451(10) Uani 1 1 d . . . C14 C 1.12185(18) 0.1418(2) 0.4987(3) 0.0452(10) Uani 1 1 d . . . H14 H 1.1447 0.1490 0.4701 0.054 Uiso 1 1 calc R . . C15 C 1.10734(19) 0.2012(2) 0.5331(3) 0.0405(10) Uani 1 1 d . . . H15 H 1.1201 0.2494 0.5270 0.049 Uiso 1 1 calc R . . C17 C 1.1189(3) 0.0037(3) 0.4678(4) 0.0736(16) Uani 1 1 d . . . H17A H 1.1421 0.0193 0.4399 0.110 Uiso 1 1 calc R . . H17B H 1.0818 -0.0210 0.4192 0.110 Uiso 1 1 calc R . . H17C H 1.1428 -0.0313 0.5200 0.110 Uiso 1 1 calc R . . C21 C 1.14599(15) 0.14610(18) 0.8774(2) 0.0278(8) Uani 1 1 d . . . C22 C 1.20596(16) 0.1291(2) 0.9215(3) 0.0333(9) Uani 1 1 d . . . H22 H 1.2219 0.1053 0.8883 0.040 Uiso 1 1 calc R . . C23 C 1.24218(17) 0.1479(2) 1.0159(3) 0.0420(10) Uani 1 1 d . . . C24 C 1.21555(17) 0.1832(2) 1.0592(3) 0.0425(10) Uani 1 1 d . . . H24 H 1.2391 0.1967 1.1244 0.051 Uiso 1 1 calc R . . C25 C 1.15500(18) 0.1985(2) 1.0075(3) 0.0404(10) Uani 1 1 d . . . H25 H 1.1378 0.2235 1.0381 0.048 Uiso 1 1 calc R . . C27 C 1.30876(17) 0.1303(3) 1.0711(3) 0.0621(13) Uani 1 1 d . . . H27A H 1.3194 0.1057 1.0291 0.093 Uiso 1 1 calc R . . H27B H 1.3182 0.0970 1.1241 0.093 Uiso 1 1 calc R . . H27C H 1.3318 0.1767 1.0957 0.093 Uiso 1 1 calc R . . C31 C 1.02591(14) 0.40173(17) 0.8555(2) 0.0221(7) Uani 1 1 d . . . C32 C 1.05512(15) 0.46749(19) 0.8637(2) 0.0283(8) Uani 1 1 d . . . H32 H 1.0891 0.4682 0.8574 0.034 Uiso 1 1 calc R . . C33 C 1.03431(16) 0.53272(19) 0.8812(3) 0.0333(9) Uani 1 1 d . . . C34 C 1.01614(17) 0.5270(2) 0.6122(3) 0.0369(9) Uani 1 1 d . . . H34 H 1.0333 0.5706 0.6034 0.044 Uiso 1 1 calc R . . C35 C 1.04123(16) 0.4587(2) 0.6183(3) 0.0334(9) Uani 1 1 d . . . H35 H 1.0750 0.4563 0.6117 0.040 Uiso 1 1 calc R . . C37 C 1.0650(2) 0.6066(2) 0.8926(4) 0.0528(11) Uani 1 1 d . . . H37C H 1.0995 0.5993 0.8855 0.079 Uiso 1 1 calc R . . H37B H 1.0789 0.6270 0.9557 0.079 Uiso 1 1 calc R . . H37A H 1.0366 0.6415 0.8439 0.079 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 0.0287(3) 0.0251(3) 0.0303(3) 0.00017(17) 0.0182(2) 0.00220(17) Cl1 0.0298(5) 0.0479(6) 0.0493(6) -0.0069(5) 0.0205(5) -0.0030(4) Cl2 0.0351(5) 0.0351(5) 0.0343(5) 0.0006(4) 0.0145(4) -0.0037(4) P1 0.0240(5) 0.0199(5) 0.0280(5) -0.0008(4) 0.0137(4) 0.0012(4) P2 0.0189(6) 0.0193(6) 0.0225(6) 0.000 0.0103(5) 0.000 O1 0.0301(13) 0.0279(13) 0.0328(14) -0.0071(10) 0.0184(11) -0.0027(10) O2 0.0246(12) 0.0280(13) 0.0300(13) 0.0003(10) 0.0141(11) 0.0063(10) O3 0.0197(11) 0.0214(12) 0.0278(13) -0.0041(10) 0.0121(10) -0.0010(9) N1 0.0241(15) 0.0187(14) 0.0245(15) -0.0002(12) 0.0124(13) 0.0006(11) N2 0.032(2) 0.022(2) 0.039(2) 0.000 0.021(2) 0.000 N16 0.0351(17) 0.0315(18) 0.0323(17) -0.0018(13) 0.0220(15) 0.0039(13) N26 0.0283(16) 0.0349(17) 0.0313(18) 0.0013(13) 0.0155(15) 0.0044(13) N36 0.0285(16) 0.0271(16) 0.0291(16) 0.0015(12) 0.0178(14) 0.0009(13) C11 0.0252(18) 0.034(2) 0.0232(18) -0.0050(15) 0.0108(16) 0.0009(15) C12 0.042(2) 0.032(2) 0.044(2) -0.0102(18) 0.021(2) -0.0003(17) C13 0.047(2) 0.049(3) 0.047(2) -0.014(2) 0.030(2) 0.001(2) C14 0.049(2) 0.053(3) 0.049(3) -0.007(2) 0.036(2) 0.003(2) C15 0.053(2) 0.037(2) 0.047(2) 0.0020(18) 0.036(2) 0.0063(19) C17 0.092(4) 0.056(3) 0.103(4) -0.033(3) 0.072(4) -0.003(3) C21 0.0261(19) 0.0233(18) 0.031(2) 0.0037(15) 0.0131(17) 0.0023(15) C22 0.030(2) 0.035(2) 0.039(2) 0.0045(17) 0.0210(18) 0.0041(16) C23 0.029(2) 0.048(2) 0.043(2) 0.009(2) 0.015(2) 0.0027(18) C24 0.032(2) 0.051(2) 0.033(2) -0.0009(19) 0.0100(19) 0.0018(19) C25 0.039(2) 0.046(2) 0.036(2) -0.0010(18) 0.019(2) 0.0063(18) C27 0.024(2) 0.096(4) 0.051(3) 0.003(3) 0.009(2) 0.011(2) C31 0.0215(17) 0.0214(18) 0.0200(17) -0.0010(13) 0.0086(14) 0.0021(14) C32 0.0238(18) 0.029(2) 0.0318(19) -0.0010(15) 0.0147(16) -0.0011(15) C33 0.037(2) 0.027(2) 0.033(2) -0.0055(16) 0.0169(18) -0.0026(16) C34 0.045(2) 0.027(2) 0.044(2) 0.0045(17) 0.0275(19) -0.0036(17) C35 0.036(2) 0.032(2) 0.041(2) 0.0008(17) 0.0261(19) -0.0035(17) C37 0.061(3) 0.028(2) 0.081(3) -0.011(2) 0.045(3) -0.008(2) _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 N16 2.056(3) . ? Cu1 N36 2.084(3) . ? Cu1 N1 2.214(3) . ? Cu1 Cl1 2.2805(12) . ? Cu1 Cl2 2.2839(11) . ? P1 N2 1.568(2) . ? P1 O1 1.584(2) . ? P1 O2 1.587(2) . ? P1 N1 1.596(3) . ? P2 N1 1.573(3) . ? P2 N1 1.573(3) 2_756 ? P2 O3 1.595(2) . ? P2 O3 1.595(2) 2_756 ? O1 C11 1.390(4) . ? O2 C21 1.407(4) . ? O3 C31 1.388(4) . ? N2 P1 1.568(2) 2_756 ? N16 C11 1.322(5) . ? N16 C15 1.364(5) . ? N26 C21 1.315(4) . ? N26 C25 1.351(5) . ? N36 C31 1.328(4) 2_756 ? N36 C35 1.351(4) . ? C11 C12 1.371(5) . ? C12 C13 1.385(6) . ? C12 H12 0.9500 . ? C13 C14 1.382(6) . ? C13 C17 1.500(6) . ? C14 C15 1.352(5) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C21 C22 1.372(5) . ? C22 C23 1.376(5) . ? C22 H22 0.9500 . ? C23 C24 1.391(6) . ? C23 C27 1.515(5) . ? C24 C25 1.375(6) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C31 N36 1.328(4) 2_756 ? C31 C32 1.371(5) . ? C32 C33 1.383(5) . ? C32 H32 0.9500 . ? C33 C34 1.388(5) 2_756 ? C33 C37 1.506(5) . ? C34 C35 1.365(5) . ? C34 C33 1.388(5) 2_756 ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C37 H37C 0.9800 . ? C37 H37B 0.9800 . ? C37 H37A 0.9800 . ? 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 N16 Cu1 N36 177.00(11) . . ? N16 Cu1 N1 91.92(10) . . ? N36 Cu1 N1 89.85(10) . . ? N16 Cu1 Cl1 90.02(9) . . ? N36 Cu1 Cl1 91.73(8) . . ? N1 Cu1 Cl1 108.12(8) . . ? N16 Cu1 Cl2 88.51(9) . . ? N36 Cu1 Cl2 88.63(8) . . ? N1 Cu1 Cl2 108.91(8) . . ? Cl1 Cu1 Cl2 142.97(4) . . ? N2 P1 O1 106.45(12) . . ? N2 P1 O2 113.13(12) . . ? O1 P1 O2 98.76(12) . . ? N2 P1 N1 118.03(16) . . ? O1 P1 N1 108.68(13) . . ? O2 P1 N1 109.87(13) . . ? N1 P2 N1 118.5(2) . 2_756 ? N1 P2 O3 107.55(12) . . ? N1 P2 O3 109.52(12) 2_756 . ? N1 P2 O3 109.52(12) . 2_756 ? N1 P2 O3 107.55(12) 2_756 2_756 ? O3 P2 O3 103.11(17) . 2_756 ? C11 O1 P1 124.0(2) . . ? C21 O2 P1 120.7(2) . . ? C31 O3 P2 121.23(19) . . ? P2 N1 P1 121.23(17) . . ? P2 N1 Cu1 116.73(14) . . ? P1 N1 Cu1 117.98(14) . . ? P1 N2 P1 122.1(3) 2_756 . ? C11 N16 C15 115.4(3) . . ? C11 N16 Cu1 127.7(2) . . ? C15 N16 Cu1 116.4(2) . . ? C21 N26 C25 115.0(3) . . ? C31 N36 C35 115.5(3) 2_756 . ? C31 N36 Cu1 125.0(2) 2_756 . ? C35 N36 Cu1 118.1(2) . . ? N16 C11 C12 125.2(3) . . ? N16 C11 O1 118.5(3) . . ? C12 C11 O1 116.3(3) . . ? C11 C12 C13 118.5(4) . . ? C11 C12 H12 120.7 . . ? C13 C12 H12 120.7 . . ? C14 C13 C12 117.3(3) . . ? C14 C13 C17 121.8(4) . . ? C12 C13 C17 120.9(4) . . ? C15 C14 C13 120.2(4) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 N16 123.3(4) . . ? C14 C15 H15 118.3 . . ? N16 C15 H15 118.3 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N26 C21 C22 127.0(3) . . ? N26 C21 O2 115.9(3) . . ? C22 C21 O2 117.0(3) . . ? C21 C22 C23 117.4(3) . . ? C21 C22 H22 121.3 . . ? C23 C22 H22 121.3 . . ? C22 C23 C24 117.8(3) . . ? C22 C23 C27 121.2(4) . . ? C24 C23 C27 121.0(4) . . ? C25 C24 C23 119.8(4) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? N26 C25 C24 122.9(4) . . ? N26 C25 H25 118.5 . . ? C24 C25 H25 118.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N36 C31 C32 125.1(3) 2_756 . ? N36 C31 O3 118.1(3) 2_756 . ? C32 C31 O3 116.8(3) . . ? C31 C32 C33 118.9(3) . . ? C31 C32 H32 120.5 . . ? C33 C32 H32 120.5 . . ? C32 C33 C34 116.9(3) . 2_756 ? C32 C33 C37 121.6(3) . . ? C34 C33 C37 121.5(3) 2_756 . ? C35 C34 C33 120.1(3) . 2_756 ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 2_756 . ? N36 C35 C34 123.4(3) . . ? N36 C35 H35 118.3 . . ? C34 C35 H35 118.3 . . ? C33 C37 H37C 109.5 . . ? C33 C37 H37B 109.5 . . ? H37C C37 H37B 109.5 . . ? C33 C37 H37A 109.5 . . ? H37C C37 H37A 109.5 . . ? H37B C37 H37A 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.353 _refine_diff_density_min -0.280 _refine_diff_density_rms 0.075 #===END