# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_908589 _database_code_depnum_ccdc_archive 'CCDC 908589' #TrackingRef '17689_web_deposit_cif_file_0_RSuriyaNarayanan_1360734625.908589.cif' _audit_creation_date 2013-02-05 _audit_creation_method ; Olex2 1.2 (compiled Dec 5 2012 16:20:19, GUI svn.r4385) ; _chemical_name_common spiro(tetrakis-3-pyridyloxy)cyclotriphosphazene _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C32 H24 N7 O6 P3' _chemical_formula_sum 'C32 H24 N7 O6 P3' _chemical_formula_weight 695.49 _chemical_melting_point ? 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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 11.6031(15) _cell_length_b 14.6279(19) _cell_length_c 19.142(3) _cell_angle_alpha 76.683(2) _cell_angle_beta 82.873(2) _cell_angle_gamma 88.340(2) _cell_volume 3137.1(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2666 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 23.48 _cell_measurement_theta_min 2.19 _exptl_absorpt_coefficient_mu 0.248 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.608419 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS v.2.10 (Bruker,2003) was used for absorption correction. R(int) was 0.0781 before and 0.0374 after correction. The Ratio of minimum to maximum transmission is 0.6084. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1432 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_unetI/netI 0.0986 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 17656 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 2.19 _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.977 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 7914 _reflns_number_total 12046 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'SAINT v6.45A (Bruker, 2003)' _computing_data_collection ? _computing_data_reduction 'SAINT v6.45A (Bruker, 2003)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.398 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.086 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 865 _refine_ls_number_reflns 12046 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0966 _refine_ls_R_factor_gt 0.0582 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0676P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1293 _refine_ls_wR_factor_ref 0.1554 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: H2BP of C2BP, H5BP of C5BP, H4BP of C4BP, H3BP of C3BP, H8BP of C8BP, H9BP of C9BP, H10B of C10B, H11B of C11B, H2D of C2D, H5C of C5C, H2C of C2C, H2A of C2A, H4C of C4C, H4B of C4B, H3A of C3A, H5A of C5A, H3C of C3C, H2B of C2B, H5B of C5B, H4A of C4A, H3B of C3B, H11D of C11D, H3X of C3X, H5W of C5W, H2W of C2W, H3W of C3W, H4W of C4W, H5X of C5X, H2Y of C2Y, H3Y of C3Y, H4Y of C4Y, H5Y of C5Y, H4X of C4X, H2X of C2X, H4Z of C4Z, H3Z of C3Z, H2Z of C2Z, H5Z of C5Z, H3D of C3D, H4D of C4D, H5D of C5D, H2DP of C2DP, H5DP of C5DP, H8DP of C8DP, H10D of C10D, H4DP of C4DP, H9DP of C9DP, H3DP of C3DP 2.a Aromatic/amide H refined with riding coordinates: C2BP(H2BP), C3BP(H3BP), C4BP(H4BP), C5BP(H5BP), C8BP(H8BP), C9BP(H9BP), C10B(H10B), C11B(H11B), C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C2B(H2B), C3B(H3B), C4B(H4B), C5B(H5B), C2C(H2C), C3C(H3C), C4C(H4C), C5C(H5C), C2D(H2D), C3D(H3D), C4D(H4D), C5D(H5D), C2DP(H2DP), C3DP(H3DP), C4DP(H4DP), C5DP(H5DP), C8DP(H8DP), C9DP(H9DP), C10D(H10D), C11D(H11D), C2W(H2W), C3W(H3W), C4W(H4W), C5W(H5W), C2X(H2X), C3X(H3X), C4X(H4X), C5X(H5X), C2Y(H2Y), C3Y(H3Y), C4Y(H4Y), C5Y(H5Y), C2Z(H2Z), C3Z(H3Z), C4Z(H4Z), C5Z(H5Z) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 P1 P 0.37182(8) 0.03218(6) 0.74965(5) 0.0182(2) Uani 1 1 d . . . P2 P 0.53141(8) 0.17540(7) 0.72769(5) 0.0189(2) Uani 1 1 d . . . P3 P 0.30314(8) 0.21715(7) 0.70785(5) 0.0192(2) Uani 1 1 d . . . N1 N 0.4978(2) 0.0684(2) 0.75254(15) 0.0188(6) Uani 1 1 d . . . N2 N 0.4333(2) 0.2485(2) 0.70419(15) 0.0204(6) Uani 1 1 d . . . N3 N 0.2758(2) 0.1088(2) 0.72750(15) 0.0199(6) Uani 1 1 d . . . O1 O 0.33731(19) -0.03455(16) 0.82715(12) 0.0194(5) Uani 1 1 d . . . O2 O 0.37039(19) -0.03565(16) 0.69628(12) 0.0208(5) Uani 1 1 d . . . O3 O 0.58714(19) 0.21059(16) 0.78822(12) 0.0216(5) Uani 1 1 d . . . O4 O 0.64052(19) 0.18858(17) 0.66667(12) 0.0221(5) Uani 1 1 d . . . O5 O 0.2594(2) 0.26694(17) 0.63345(12) 0.0230(6) Uani 1 1 d . . . O6 O 0.22052(19) 0.26716(17) 0.76063(12) 0.0219(5) Uani 1 1 d . . . C1BP C 0.2436(3) -0.0976(2) 0.83954(18) 0.0185(7) Uani 1 1 d . . . C2BP C 0.1483(3) -0.0819(3) 0.88597(18) 0.0229(8) Uani 1 1 d . . . H2BP H 0.1447 -0.0283 0.9046 0.028 Uiso 1 1 calc R . . C3BP C 0.0585(3) -0.1456(3) 0.9047(2) 0.0280(9) Uani 1 1 d . . . H3BP H -0.0062 -0.1353 0.9358 0.034 Uiso 1 1 calc R . . C4BP C 0.0652(3) -0.2255(3) 0.8768(2) 0.0304(9) Uani 1 1 d . . . H4BP H 0.0050 -0.2690 0.8894 0.036 Uiso 1 1 calc R . . C5BP C 0.1606(3) -0.2404(3) 0.83066(19) 0.0252(8) Uani 1 1 d . . . H5BP H 0.1635 -0.2939 0.8120 0.030 Uiso 1 1 calc R . . C6BP C 0.2534(3) -0.1772(3) 0.81103(19) 0.0224(8) Uani 1 1 d . . . C7BP C 0.3602(3) -0.1964(2) 0.76506(19) 0.0223(8) Uani 1 1 d . . . C8BP C 0.4076(3) -0.2871(3) 0.7749(2) 0.0269(9) Uani 1 1 d . . . H8BP H 0.3692 -0.3362 0.8086 0.032 Uiso 1 1 calc R . . C9BP C 0.5109(3) -0.3046(3) 0.7352(2) 0.0318(9) Uani 1 1 d . . . H9BP H 0.5407 -0.3653 0.7421 0.038 Uiso 1 1 calc R . . C10B C 0.5692(3) -0.2328(3) 0.6856(2) 0.0330(10) Uani 1 1 d . . . H10B H 0.6391 -0.2447 0.6597 0.040 Uiso 1 1 calc R . . C11B C 0.5238(3) -0.1418(3) 0.67400(19) 0.0269(9) Uani 1 1 d . . . H11B H 0.5626 -0.0925 0.6406 0.032 Uiso 1 1 calc R . . C12B C 0.4196(3) -0.1268(3) 0.71355(19) 0.0223(8) Uani 1 1 d . . . C1A C 0.6684(3) 0.1579(2) 0.82980(19) 0.0225(8) Uani 1 1 d . . . C2A C 0.6330(3) 0.1157(3) 0.9006(2) 0.0287(9) Uani 1 1 d . . . H2A H 0.5556 0.1172 0.9199 0.034 Uiso 1 1 calc R . . C3A C 0.7167(4) 0.0703(3) 0.9428(2) 0.0325(9) Uani 1 1 d . . . H3A H 0.6968 0.0402 0.9910 0.039 Uiso 1 1 calc R . . C4A C 0.8302(4) 0.0715(3) 0.9107(2) 0.0343(10) Uani 1 1 d . . . H4A H 0.8859 0.0416 0.9390 0.041 Uiso 1 1 calc R . . C5A C 0.7840(3) 0.1558(3) 0.8012(2) 0.0262(9) Uani 1 1 d . . . H5A H 0.8059 0.1848 0.7529 0.031 Uiso 1 1 calc R . . N1A N 0.8653(3) 0.1126(2) 0.84202(18) 0.0320(8) Uani 1 1 d . . . C1B C 0.6340(3) 0.1497(3) 0.60652(18) 0.0220(8) Uani 1 1 d . . . C2B C 0.7073(3) 0.0766(3) 0.5976(2) 0.0309(9) Uani 1 1 d . . . H2B H 0.7579 0.0545 0.6318 0.037 Uiso 1 1 calc R . . C3B C 0.6343(3) 0.0714(3) 0.4935(2) 0.0360(10) Uani 1 1 d . . . H3B H 0.6332 0.0442 0.4542 0.043 Uiso 1 1 calc R . . C4B C 0.5604(3) 0.1448(3) 0.4989(2) 0.0375(11) Uani 1 1 d . . . H4B H 0.5113 0.1667 0.4637 0.045 Uiso 1 1 calc R . . C5B C 0.5594(3) 0.1859(3) 0.55680(19) 0.0309(9) Uani 1 1 d . . . H5B H 0.5103 0.2359 0.5620 0.037 Uiso 1 1 calc R . . N1B N 0.7086(3) 0.0365(3) 0.54179(18) 0.0370(8) Uani 1 1 d . . . C1C C 0.1711(3) 0.2269(2) 0.60578(19) 0.0221(8) Uani 1 1 d . . . C2C C 0.0567(3) 0.2297(3) 0.6344(2) 0.0269(8) Uani 1 1 d . . . H2C H 0.0383 0.2582 0.6730 0.032 Uiso 1 1 calc R . . C3C C 0.0015(3) 0.1546(3) 0.5526(2) 0.0304(9) Uani 1 1 d . . . H3C H -0.0571 0.1297 0.5335 0.037 Uiso 1 1 calc R . . C4C C 0.1137(3) 0.1490(3) 0.5207(2) 0.0320(9) Uani 1 1 d . . . H4C H 0.1298 0.1204 0.4820 0.038 Uiso 1 1 calc R . . C5C C 0.2022(3) 0.1869(3) 0.54746(19) 0.0289(9) Uani 1 1 d . . . H5C H 0.2791 0.1855 0.5271 0.035 Uiso 1 1 calc R . . N1C N -0.0294(3) 0.1931(2) 0.60885(17) 0.0329(8) Uani 1 1 d . . . C1D C 0.2293(3) 0.2361(2) 0.83497(18) 0.0208(8) Uani 1 1 d . . . C2D C 0.1436(3) 0.1798(3) 0.87792(19) 0.0256(8) Uani 1 1 d . . . H2D H 0.0821 0.1628 0.8567 0.031 Uiso 1 1 calc R . . C3D C 0.2335(3) 0.1762(3) 0.9782(2) 0.0276(9) Uani 1 1 d . . . H3D H 0.2356 0.1557 1.0278 0.033 Uiso 1 1 calc R . . C4D C 0.3214(3) 0.2338(3) 0.9385(2) 0.0279(9) Uani 1 1 d . . . H4D H 0.3806 0.2517 0.9612 0.033 Uiso 1 1 calc R . . C5D C 0.3212(3) 0.2649(3) 0.86444(19) 0.0249(8) Uani 1 1 d . . . H5D H 0.3799 0.3032 0.8359 0.030 Uiso 1 1 calc R . . N1D N 0.1447(3) 0.1480(2) 0.94946(16) 0.0298(8) Uani 1 1 d . . . P1A P 0.87693(8) 0.63359(6) 0.75561(5) 0.0188(2) Uani 1 1 d . . . P2A P 1.03029(8) 0.48628(7) 0.75349(5) 0.0204(2) Uani 1 1 d . . . P3A P 0.80549(8) 0.46960(7) 0.72639(5) 0.0201(2) Uani 1 1 d . . . N1P N 1.0026(2) 0.5897(2) 0.76181(15) 0.0208(7) Uani 1 1 d . . . N2P N 0.9337(3) 0.4307(2) 0.72957(15) 0.0238(7) Uani 1 1 d . . . N3P N 0.7782(2) 0.5688(2) 0.74393(15) 0.0213(7) Uani 1 1 d . . . O1A O 0.84527(19) 0.67085(16) 0.82679(12) 0.0204(5) Uani 1 1 d . . . O2A O 0.87587(19) 0.72546(16) 0.69267(12) 0.0199(5) Uani 1 1 d . . . O3A O 1.1488(2) 0.48620(17) 0.70201(13) 0.0249(6) Uani 1 1 d . . . O4A O 1.0663(2) 0.42145(17) 0.82581(12) 0.0233(6) Uani 1 1 d . . . O5A O 0.7136(2) 0.39534(17) 0.77476(12) 0.0232(6) Uani 1 1 d . . . O6A O 0.7746(2) 0.46645(17) 0.64883(12) 0.0233(6) Uani 1 1 d . . . C1DP C 0.7628(3) 0.7426(2) 0.83181(18) 0.0194(8) Uani 1 1 d . . . C2DP C 0.6612(3) 0.7189(3) 0.87795(18) 0.0242(8) Uani 1 1 d . . . H2DP H 0.6456 0.6565 0.9011 0.029 Uiso 1 1 calc R . . C3DP C 0.5834(3) 0.7884(3) 0.88923(19) 0.0269(9) Uani 1 1 d . . . H3DP H 0.5147 0.7733 0.9200 0.032 Uiso 1 1 calc R . . C4DP C 0.6077(3) 0.8808(3) 0.85472(19) 0.0261(8) Uani 1 1 d . . . H4DP H 0.5563 0.9281 0.8633 0.031 Uiso 1 1 calc R . . C5DP C 0.7086(3) 0.9031(3) 0.80743(18) 0.0236(8) Uani 1 1 d . . . H5DP H 0.7227 0.9655 0.7836 0.028 Uiso 1 1 calc R . . C6DP C 0.7893(3) 0.8349(2) 0.79448(18) 0.0191(7) Uani 1 1 d . . . C7DP C 0.8957(3) 0.8601(2) 0.74353(18) 0.0197(8) Uani 1 1 d . . . C8DP C 0.9583(3) 0.9418(3) 0.74057(19) 0.0229(8) Uani 1 1 d . . . H8DP H 0.9329 0.9805 0.7717 0.027 Uiso 1 1 calc R . . C9DP C 1.0573(3) 0.9656(3) 0.6919(2) 0.0265(8) Uani 1 1 d . . . H9DP H 1.0986 1.0193 0.6916 0.032 Uiso 1 1 calc R . . C10D C 1.0956(3) 0.9107(3) 0.6440(2) 0.0301(9) Uani 1 1 d . . . H10D H 1.1611 0.9281 0.6107 0.036 Uiso 1 1 calc R . . C11D C 1.0355(3) 0.8293(3) 0.64557(19) 0.0247(8) Uani 1 1 d . . . H11D H 1.0607 0.7912 0.6139 0.030 Uiso 1 1 calc R . . C12D C 0.9385(3) 0.8061(2) 0.69483(18) 0.0194(7) Uani 1 1 d . . . C1W C 1.1541(3) 0.5399(3) 0.63076(19) 0.0233(8) Uani 1 1 d . . . C2W C 1.1956(3) 0.6302(3) 0.6142(2) 0.0285(9) Uani 1 1 d . . . H2W H 1.2169 0.6552 0.6512 0.034 Uiso 1 1 calc R . . C3W C 1.1752(3) 0.6450(3) 0.4951(2) 0.0345(10) Uani 1 1 d . . . H3W H 1.1824 0.6812 0.4479 0.041 Uiso 1 1 calc R . . C4W C 1.1331(3) 0.5554(3) 0.5077(2) 0.0370(10) Uani 1 1 d . . . H4W H 1.1121 0.5318 0.4700 0.044 Uiso 1 1 calc R . . C5W C 1.1223(3) 0.5004(3) 0.5776(2) 0.0333(10) Uani 1 1 d . . . H5W H 1.0946 0.4391 0.5881 0.040 Uiso 1 1 calc R . . N1W N 1.2066(3) 0.6834(2) 0.54713(18) 0.0369(8) Uani 1 1 d . . . C1X C 1.1420(3) 0.4461(2) 0.87003(19) 0.0235(8) Uani 1 1 d . . . C2X C 1.2521(3) 0.4795(3) 0.8437(2) 0.0320(9) Uani 1 1 d . . . H2X H 1.2744 0.4922 0.7940 0.038 Uiso 1 1 calc R . . C3X C 1.2933(4) 0.4765(3) 0.9573(2) 0.0411(11) Uani 1 1 d . . . H3X H 1.3458 0.4863 0.9878 0.049 Uiso 1 1 calc R . . C4X C 1.1844(4) 0.4443(3) 0.9875(2) 0.0409(11) Uani 1 1 d . . . H4X H 1.1640 0.4334 1.0373 0.049 Uiso 1 1 calc R . . C5X C 1.1050(4) 0.4282(3) 0.9430(2) 0.0352(10) Uani 1 1 d . . . H5X H 1.0304 0.4063 0.9616 0.042 Uiso 1 1 calc R . . N1X N 1.3278(3) 0.4943(2) 0.88657(19) 0.0418(9) Uani 1 1 d . . . C1Y C 0.7096(3) 0.3718(3) 0.85019(18) 0.0244(8) Uani 1 1 d . . . C2Y C 0.6080(3) 0.3887(3) 0.8901(2) 0.0304(9) Uani 1 1 d . . . H2Y H 0.5479 0.4192 0.8660 0.037 Uiso 1 1 calc R . . C3Y C 0.6821(4) 0.3198(3) 0.9949(2) 0.0446(12) Uani 1 1 d . . . H3Y H 0.6732 0.3012 1.0451 0.054 Uiso 1 1 calc R . . C4Y C 0.7857(4) 0.3019(3) 0.9585(2) 0.0365(10) Uani 1 1 d . . . H4Y H 0.8455 0.2730 0.9837 0.044 Uiso 1 1 calc R . . C5Y C 0.8010(3) 0.3271(3) 0.8838(2) 0.0298(9) Uani 1 1 d . . . H5Y H 0.8700 0.3144 0.8574 0.036 Uiso 1 1 calc R . . N1Y N 0.5920(3) 0.3626(3) 0.96283(18) 0.0432(9) Uani 1 1 d . . . C1Z C 0.6738(3) 0.5075(3) 0.62192(18) 0.0219(8) Uani 1 1 d . . . C2Z C 0.5718(3) 0.4567(3) 0.6359(2) 0.0315(9) Uani 1 1 d . . . H2Z H 0.5664 0.3965 0.6654 0.038 Uiso 1 1 calc R . . C3Z C 0.4783(4) 0.4998(3) 0.6037(2) 0.0405(11) Uani 1 1 d . . . H3Z H 0.4076 0.4686 0.6112 0.049 Uiso 1 1 calc R . . C4Z C 0.4903(3) 0.5893(3) 0.5605(2) 0.0379(10) Uani 1 1 d . . . H4Z H 0.4261 0.6171 0.5393 0.046 Uiso 1 1 calc R . . C5Z C 0.6790(3) 0.5959(3) 0.57847(19) 0.0275(9) Uani 1 1 d . . . H5Z H 0.7490 0.6284 0.5700 0.033 Uiso 1 1 calc R . . N1Z N 0.5887(3) 0.6380(2) 0.54758(17) 0.0334(8) 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 P1 0.0202(5) 0.0164(5) 0.0184(5) -0.0042(4) -0.0031(4) -0.0009(4) P2 0.0190(4) 0.0182(5) 0.0197(5) -0.0042(4) -0.0035(4) -0.0015(4) P3 0.0201(5) 0.0175(5) 0.0198(5) -0.0028(4) -0.0044(4) 0.0001(4) N1 0.0200(15) 0.0168(15) 0.0212(15) -0.0061(13) -0.0052(12) -0.0002(12) N2 0.0205(15) 0.0152(15) 0.0252(16) -0.0025(13) -0.0057(12) -0.0012(13) N3 0.0210(15) 0.0178(16) 0.0218(16) -0.0055(13) -0.0046(12) -0.0013(13) O1 0.0231(12) 0.0163(13) 0.0197(13) -0.0047(10) -0.0041(10) -0.0028(10) O2 0.0258(13) 0.0185(13) 0.0192(13) -0.0061(11) -0.0037(10) 0.0007(11) O3 0.0232(13) 0.0175(13) 0.0266(14) -0.0077(11) -0.0072(11) 0.0005(11) O4 0.0225(13) 0.0225(14) 0.0211(13) -0.0050(11) -0.0006(10) -0.0023(11) O5 0.0247(13) 0.0226(14) 0.0212(13) -0.0004(11) -0.0096(10) -0.0010(11) O6 0.0238(13) 0.0212(14) 0.0216(13) -0.0053(11) -0.0066(10) 0.0037(11) C1BP 0.0202(17) 0.0157(18) 0.0189(18) 0.0007(15) -0.0075(14) -0.0034(15) C2BP 0.029(2) 0.024(2) 0.0149(18) -0.0013(15) -0.0050(15) 0.0016(16) C3BP 0.0232(19) 0.035(2) 0.023(2) 0.0012(17) -0.0042(16) -0.0035(17) C4BP 0.028(2) 0.033(2) 0.026(2) 0.0068(18) -0.0118(17) -0.0121(18) C5BP 0.031(2) 0.019(2) 0.026(2) -0.0012(16) -0.0134(17) -0.0046(16) C6BP 0.0239(18) 0.0205(19) 0.0220(19) 0.0000(16) -0.0088(15) -0.0035(16) C7BP 0.0278(19) 0.0174(19) 0.0236(19) -0.0052(16) -0.0093(16) 0.0000(16) C8BP 0.036(2) 0.0170(19) 0.031(2) -0.0057(17) -0.0161(18) 0.0014(17) C9BP 0.038(2) 0.028(2) 0.037(2) -0.018(2) -0.0151(19) 0.0097(19) C10B 0.030(2) 0.044(3) 0.034(2) -0.026(2) -0.0089(18) 0.011(2) C11B 0.0261(19) 0.032(2) 0.025(2) -0.0102(18) -0.0059(16) -0.0009(17) C12B 0.0238(18) 0.024(2) 0.0230(19) -0.0090(16) -0.0112(15) 0.0022(16) C1A 0.0289(19) 0.0169(19) 0.027(2) -0.0099(16) -0.0138(16) 0.0013(16) C2A 0.031(2) 0.027(2) 0.031(2) -0.0103(18) -0.0081(17) 0.0002(18) C3A 0.043(2) 0.027(2) 0.030(2) -0.0080(18) -0.0158(19) -0.0003(19) C4A 0.041(2) 0.031(2) 0.038(2) -0.017(2) -0.018(2) 0.013(2) C5A 0.0235(19) 0.028(2) 0.032(2) -0.0148(18) -0.0069(16) 0.0000(17) N1A 0.0262(17) 0.037(2) 0.039(2) -0.0199(17) -0.0110(15) 0.0072(15) C1B 0.0215(18) 0.027(2) 0.0178(18) -0.0065(16) 0.0021(15) -0.0053(16) C2B 0.027(2) 0.042(3) 0.024(2) -0.0094(19) -0.0009(16) 0.0002(19) C3B 0.032(2) 0.055(3) 0.025(2) -0.018(2) 0.0036(18) -0.010(2) C4B 0.030(2) 0.060(3) 0.025(2) -0.012(2) -0.0052(18) -0.005(2) C5B 0.030(2) 0.038(2) 0.023(2) -0.0052(18) -0.0015(17) 0.0020(19) N1B 0.0354(19) 0.042(2) 0.035(2) -0.0151(17) 0.0020(16) 0.0010(17) C1C 0.0278(19) 0.0155(18) 0.0225(19) -0.0005(15) -0.0089(16) 0.0012(16) C2C 0.028(2) 0.026(2) 0.027(2) -0.0058(17) -0.0063(16) 0.0047(17) C3C 0.034(2) 0.033(2) 0.025(2) -0.0024(18) -0.0123(17) -0.0019(19) C4C 0.038(2) 0.036(2) 0.025(2) -0.0119(19) -0.0063(18) -0.0008(19) C5C 0.027(2) 0.035(2) 0.023(2) -0.0056(18) -0.0008(16) -0.0021(18) N1C 0.0282(18) 0.035(2) 0.035(2) -0.0036(16) -0.0092(15) 0.0030(16) C1D 0.0243(18) 0.0211(19) 0.0191(18) -0.0097(16) -0.0028(15) 0.0077(16) C2D 0.0235(19) 0.029(2) 0.026(2) -0.0089(17) -0.0045(16) -0.0013(17) C3D 0.032(2) 0.030(2) 0.022(2) -0.0062(17) -0.0078(17) 0.0027(18) C4D 0.028(2) 0.032(2) 0.028(2) -0.0152(18) -0.0061(17) 0.0009(18) C5D 0.0233(19) 0.025(2) 0.026(2) -0.0078(17) 0.0019(16) 0.0031(16) N1D 0.0301(18) 0.035(2) 0.0238(17) -0.0084(15) 0.0015(14) -0.0030(15) P1A 0.0222(5) 0.0163(5) 0.0177(5) -0.0033(4) -0.0037(4) 0.0015(4) P2A 0.0218(5) 0.0197(5) 0.0200(5) -0.0044(4) -0.0045(4) 0.0040(4) P3A 0.0234(5) 0.0178(5) 0.0198(5) -0.0043(4) -0.0058(4) 0.0007(4) N1P 0.0226(15) 0.0187(16) 0.0212(16) -0.0037(13) -0.0042(12) -0.0016(13) N2P 0.0298(17) 0.0184(16) 0.0263(17) -0.0088(14) -0.0097(13) 0.0058(14) N3P 0.0222(15) 0.0180(16) 0.0244(16) -0.0041(13) -0.0072(13) 0.0026(13) O1A 0.0264(13) 0.0155(13) 0.0193(12) -0.0035(10) -0.0040(10) 0.0022(11) O2A 0.0252(13) 0.0166(13) 0.0183(12) -0.0043(10) -0.0037(10) -0.0004(10) O3A 0.0256(13) 0.0254(14) 0.0222(13) -0.0021(11) -0.0052(11) 0.0065(11) O4A 0.0246(13) 0.0236(14) 0.0219(13) -0.0032(11) -0.0078(10) 0.0010(11) O5A 0.0278(13) 0.0197(13) 0.0234(13) -0.0046(11) -0.0082(11) -0.0039(11) O6A 0.0266(13) 0.0258(14) 0.0208(13) -0.0095(11) -0.0085(11) 0.0041(11) C1DP 0.0234(18) 0.0189(19) 0.0187(18) -0.0079(15) -0.0069(15) 0.0041(15) C2DP 0.028(2) 0.024(2) 0.0209(19) -0.0040(16) -0.0079(16) -0.0024(17) C3DP 0.0230(19) 0.037(2) 0.022(2) -0.0082(18) -0.0047(16) 0.0029(18) C4DP 0.0235(19) 0.032(2) 0.025(2) -0.0099(18) -0.0077(16) 0.0054(17) C5DP 0.0266(19) 0.024(2) 0.0222(19) -0.0076(16) -0.0063(16) -0.0019(16) C6DP 0.0206(17) 0.0173(18) 0.0217(19) -0.0065(15) -0.0074(15) 0.0000(15) C7DP 0.0221(18) 0.0184(19) 0.0168(18) 0.0006(15) -0.0051(14) 0.0028(15) C8DP 0.0267(19) 0.0186(19) 0.025(2) -0.0039(16) -0.0108(16) 0.0020(16) C9DP 0.0251(19) 0.021(2) 0.032(2) 0.0005(17) -0.0106(17) -0.0016(16) C10D 0.026(2) 0.034(2) 0.028(2) -0.0018(18) -0.0014(17) -0.0007(18) C11D 0.0256(19) 0.026(2) 0.0221(19) -0.0043(16) -0.0026(16) 0.0016(17) C12D 0.0245(18) 0.0129(17) 0.0194(18) 0.0000(14) -0.0051(15) 0.0024(15) C1W 0.0207(18) 0.027(2) 0.0205(19) -0.0033(16) -0.0010(15) 0.0069(16) C2W 0.029(2) 0.031(2) 0.025(2) -0.0056(18) -0.0030(17) 0.0003(18) C3W 0.031(2) 0.045(3) 0.022(2) 0.0006(19) 0.0009(17) 0.012(2) C4W 0.039(2) 0.053(3) 0.021(2) -0.011(2) -0.0062(18) -0.002(2) C5W 0.046(2) 0.033(2) 0.023(2) -0.0082(18) -0.0037(18) -0.003(2) N1W 0.041(2) 0.034(2) 0.032(2) -0.0020(16) 0.0030(16) -0.0013(17) C1X 0.031(2) 0.0162(19) 0.025(2) -0.0050(16) -0.0091(16) 0.0052(16) C2X 0.036(2) 0.026(2) 0.032(2) 0.0015(18) -0.0131(18) -0.0025(18) C3X 0.055(3) 0.032(2) 0.043(3) -0.007(2) -0.032(2) -0.003(2) C4X 0.050(3) 0.046(3) 0.029(2) -0.008(2) -0.017(2) 0.014(2) C5X 0.034(2) 0.041(3) 0.031(2) -0.006(2) -0.0070(18) 0.009(2) N1X 0.047(2) 0.033(2) 0.044(2) 0.0053(17) -0.0254(18) -0.0094(18) C1Y 0.037(2) 0.021(2) 0.0157(18) -0.0015(15) -0.0080(16) -0.0094(17) C2Y 0.033(2) 0.032(2) 0.026(2) -0.0027(18) -0.0055(17) -0.0088(18) C3Y 0.061(3) 0.048(3) 0.024(2) 0.003(2) -0.015(2) -0.025(2) C4Y 0.043(2) 0.037(3) 0.028(2) 0.0044(19) -0.018(2) -0.012(2) C5Y 0.039(2) 0.019(2) 0.032(2) -0.0022(17) -0.0123(18) -0.0057(18) N1Y 0.047(2) 0.056(3) 0.0258(19) -0.0069(18) -0.0020(17) -0.016(2) C1Z 0.0247(19) 0.026(2) 0.0171(18) -0.0057(16) -0.0075(15) 0.0035(16) C2Z 0.032(2) 0.028(2) 0.034(2) -0.0044(18) -0.0074(18) -0.0027(18) C3Z 0.027(2) 0.052(3) 0.042(3) -0.007(2) -0.0110(19) -0.003(2) C4Z 0.028(2) 0.049(3) 0.037(2) -0.008(2) -0.0091(19) 0.012(2) C5Z 0.030(2) 0.026(2) 0.027(2) -0.0052(17) -0.0048(17) -0.0001(17) N1Z 0.0356(19) 0.035(2) 0.0278(18) -0.0031(16) -0.0067(15) 0.0138(17) _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 P1 N1 1.581(3) . ? P1 N3 1.582(3) . ? P1 O1 1.588(2) . ? P1 O2 1.581(2) . ? P2 N1 1.573(3) . ? P2 N2 1.575(3) . ? P2 O3 1.583(2) . ? P2 O4 1.596(2) . ? P3 N2 1.579(3) . ? P3 N3 1.574(3) . ? P3 O5 1.580(2) . ? P3 O6 1.592(2) . ? O1 C1BP 1.408(4) . ? O2 C12B 1.418(4) . ? O3 C1A 1.407(4) . ? O4 C1B 1.407(4) . ? O5 C1C 1.409(4) . ? O6 C1D 1.406(4) . ? C1BP C2BP 1.379(5) . ? C1BP C6BP 1.392(5) . ? C2BP C3BP 1.376(5) . ? C3BP C4BP 1.388(5) . ? C4BP C5BP 1.373(5) . ? C5BP C6BP 1.398(5) . ? C6BP C7BP 1.487(5) . ? C7BP C8BP 1.401(5) . ? C7BP C12B 1.376(5) . ? C8BP C9BP 1.389(5) . ? C9BP C10B 1.373(6) . ? C10B C11B 1.397(5) . ? C11B C12B 1.385(5) . ? C1A C2A 1.370(5) . ? C1A C5A 1.387(5) . ? C2A C3A 1.395(5) . ? C3A C4A 1.381(5) . ? C4A N1A 1.331(5) . ? C5A N1A 1.349(5) . ? C1B C2B 1.375(5) . ? C1B C5B 1.372(5) . ? C2B N1B 1.330(5) . ? C3B C4B 1.369(6) . ? C3B N1B 1.346(5) . ? C4B C5B 1.376(5) . ? C1C C2C 1.375(5) . ? C1C C5C 1.381(5) . ? C2C N1C 1.340(5) . ? C3C C4C 1.376(5) . ? C3C N1C 1.333(5) . ? C4C C5C 1.385(5) . ? C1D C2D 1.369(5) . ? C1D C5D 1.384(5) . ? C2D N1D 1.342(4) . ? C3D C4D 1.374(5) . ? C3D N1D 1.343(5) . ? C4D C5D 1.387(5) . ? P1A N1P 1.583(3) . ? P1A N3P 1.576(3) . ? P1A O1A 1.579(2) . ? P1A O2A 1.586(2) . ? P2A N1P 1.577(3) . ? P2A N2P 1.574(3) . ? P2A O3A 1.590(3) . ? P2A O4A 1.583(2) . ? P3A N2P 1.580(3) . ? P3A N3P 1.578(3) . ? P3A O5A 1.591(3) . ? P3A O6A 1.581(2) . ? O1A C1DP 1.411(4) . ? O2A C12D 1.414(4) . ? O3A C1W 1.403(4) . ? O4A C1X 1.401(4) . ? O5A C1Y 1.400(4) . ? O6A C1Z 1.401(4) . ? C1DP C2DP 1.383(5) . ? C1DP C6DP 1.398(5) . ? C2DP C3DP 1.377(5) . ? C3DP C4DP 1.381(5) . ? C4DP C5DP 1.385(5) . ? C5DP C6DP 1.392(5) . ? C6DP C7DP 1.474(5) . ? C7DP C8DP 1.403(5) . ? C7DP C12D 1.393(4) . ? C8DP C9DP 1.384(5) . ? C9DP C10D 1.379(5) . ? C10D C11D 1.390(5) . ? C11D C12D 1.373(5) . ? C1W C2W 1.373(5) . ? C1W C5W 1.371(5) . ? C2W N1W 1.331(5) . ? C3W C4W 1.371(6) . ? C3W N1W 1.342(5) . ? C4W C5W 1.386(5) . ? C1X C2X 1.374(5) . ? C1X C5X 1.376(5) . ? C2X N1X 1.328(5) . ? C3X C4X 1.372(6) . ? C3X N1X 1.330(5) . ? C4X C5X 1.390(5) . ? C1Y C2Y 1.371(5) . ? C1Y C5Y 1.380(5) . ? C2Y N1Y 1.347(5) . ? C3Y C4Y 1.363(6) . ? C3Y N1Y 1.344(5) . ? C4Y C5Y 1.382(5) . ? C1Z C2Z 1.380(5) . ? C1Z C5Z 1.365(5) . ? C2Z C3Z 1.377(5) . ? C3Z C4Z 1.379(6) . ? C4Z N1Z 1.330(5) . ? C5Z N1Z 1.332(4) . ? 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 P1 N3 117.38(16) . . ? N1 P1 O1 104.59(14) . . ? N1 P1 O2 112.85(14) . . ? N3 P1 O1 112.58(14) . . ? O2 P1 N3 105.15(14) . . ? O2 P1 O1 103.59(13) . . ? N1 P2 N2 118.24(15) . . ? N1 P2 O3 111.70(14) . . ? N1 P2 O4 109.46(14) . . ? N2 P2 O3 105.62(14) . . ? N2 P2 O4 110.76(14) . . ? O3 P2 O4 99.38(13) . . ? N2 P3 O5 107.04(14) . . ? N2 P3 O6 110.25(14) . . ? N3 P3 N2 118.00(15) . . ? N3 P3 O5 111.15(14) . . ? N3 P3 O6 109.30(14) . . ? O5 P3 O6 99.51(13) . . ? P2 N1 P1 122.12(18) . . ? P2 N2 P3 121.63(19) . . ? P3 N3 P1 122.17(18) . . ? C1BP O1 P1 120.9(2) . . ? C12B O2 P1 120.1(2) . . ? C1A O3 P2 123.3(2) . . ? C1B O4 P2 117.9(2) . . ? C1C O5 P3 121.2(2) . . ? C1D O6 P3 116.5(2) . . ? C2BP C1BP O1 117.4(3) . . ? C2BP C1BP C6BP 122.1(3) . . ? C6BP C1BP O1 120.1(3) . . ? C3BP C2BP C1BP 119.8(3) . . ? C2BP C3BP C4BP 119.5(3) . . ? C5BP C4BP C3BP 120.2(4) . . ? C4BP C5BP C6BP 121.6(4) . . ? C1BP C6BP C5BP 116.8(3) . . ? C1BP C6BP C7BP 121.5(3) . . ? C5BP C6BP C7BP 121.7(3) . . ? C8BP C7BP C6BP 120.6(3) . . ? C12B C7BP C6BP 122.4(3) . . ? C12B C7BP C8BP 117.0(3) . . ? C9BP C8BP C7BP 121.0(4) . . ? C10B C9BP C8BP 120.3(4) . . ? C9BP C10B C11B 120.1(4) . . ? C12B C11B C10B 118.3(4) . . ? C7BP C12B O2 119.5(3) . . ? C7BP C12B C11B 123.3(3) . . ? C11B C12B O2 117.1(3) . . ? C2A C1A O3 118.6(3) . . ? C2A C1A C5A 120.9(3) . . ? C5A C1A O3 120.2(3) . . ? C1A C2A C3A 117.9(4) . . ? C4A C3A C2A 117.9(4) . . ? N1A C4A C3A 124.5(4) . . ? N1A C5A C1A 121.3(4) . . ? C4A N1A C5A 117.5(3) . . ? C2B C1B O4 118.2(3) . . ? C5B C1B O4 120.8(3) . . ? C5B C1B C2B 120.9(3) . . ? N1B C2B C1B 122.4(4) . . ? N1B C3B C4B 123.7(4) . . ? C3B C4B C5B 119.4(4) . . ? C1B C5B C4B 117.0(4) . . ? C2B N1B C3B 116.6(3) . . ? C2C C1C O5 121.3(3) . . ? C2C C1C C5C 120.6(3) . . ? C5C C1C O5 118.1(3) . . ? N1C C2C C1C 122.8(3) . . ? N1C C3C C4C 124.8(4) . . ? C3C C4C C5C 118.7(4) . . ? C1C C5C C4C 117.0(3) . . ? C3C N1C C2C 116.2(3) . . ? C2D C1D O6 119.0(3) . . ? C2D C1D C5D 120.7(3) . . ? C5D C1D O6 120.3(3) . . ? N1D C2D C1D 122.7(3) . . ? N1D C3D C4D 123.7(3) . . ? C3D C4D C5D 119.4(3) . . ? C1D C5D C4D 116.8(4) . . ? C2D N1D C3D 116.6(3) . . ? N1P P1A O2A 112.72(14) . . ? N3P P1A N1P 117.64(16) . . ? N3P P1A O1A 111.63(14) . . ? N3P P1A O2A 105.54(14) . . ? O1A P1A N1P 104.81(14) . . ? O1A P1A O2A 103.76(12) . . ? N1P P2A O3A 109.02(15) . . ? N1P P2A O4A 111.64(14) . . ? N2P P2A N1P 118.32(15) . . ? N2P P2A O3A 110.55(15) . . ? N2P P2A O4A 105.96(15) . . ? O4A P2A O3A 99.76(13) . . ? N2P P3A O5A 111.32(15) . . ? N2P P3A O6A 105.71(14) . . ? N3P P3A N2P 118.02(16) . . ? N3P P3A O5A 109.02(14) . . ? N3P P3A O6A 111.72(14) . . ? O6A P3A O5A 99.45(13) . . ? P2A N1P P1A 121.58(18) . . ? P2A N2P P3A 121.35(18) . . ? P1A N3P P3A 121.92(18) . . ? C1DP O1A P1A 122.7(2) . . ? C12D O2A P1A 120.3(2) . . ? C1W O3A P2A 117.8(2) . . ? C1X O4A P2A 125.9(2) . . ? C1Y O5A P3A 120.8(2) . . ? C1Z O6A P3A 122.5(2) . . ? C2DP C1DP O1A 117.8(3) . . ? C2DP C1DP C6DP 122.6(3) . . ? C6DP C1DP O1A 119.5(3) . . ? C3DP C2DP C1DP 119.4(4) . . ? C2DP C3DP C4DP 119.8(4) . . ? C3DP C4DP C5DP 120.1(4) . . ? C4DP C5DP C6DP 121.9(4) . . ? C1DP C6DP C7DP 122.7(3) . . ? C5DP C6DP C1DP 116.2(3) . . ? C5DP C6DP C7DP 121.0(3) . . ? C8DP C7DP C6DP 121.2(3) . . ? C12D C7DP C6DP 122.5(3) . . ? C12D C7DP C8DP 116.2(3) . . ? C9DP C8DP C7DP 120.9(3) . . ? C10D C9DP C8DP 120.8(4) . . ? C9DP C10D C11D 119.6(4) . . ? C12D C11D C10D 118.7(3) . . ? C7DP C12D O2A 118.9(3) . . ? C11D C12D O2A 117.4(3) . . ? C11D C12D C7DP 123.7(3) . . ? C2W C1W O3A 119.8(3) . . ? C5W C1W O3A 119.7(3) . . ? C5W C1W C2W 120.4(4) . . ? N1W C2W C1W 122.6(4) . . ? N1W C3W C4W 123.4(4) . . ? C3W C4W C5W 119.1(4) . . ? C1W C5W C4W 117.4(4) . . ? C2W N1W C3W 117.1(4) . . ? C2X C1X O4A 122.3(3) . . ? C2X C1X C5X 120.6(3) . . ? C5X C1X O4A 116.9(3) . . ? N1X C2X C1X 122.3(4) . . ? N1X C3X C4X 123.5(4) . . ? C3X C4X C5X 119.2(4) . . ? C1X C5X C4X 116.7(4) . . ? C2X N1X C3X 117.6(4) . . ? C2Y C1Y O5A 117.6(3) . . ? C2Y C1Y C5Y 120.6(3) . . ? C5Y C1Y O5A 121.6(3) . . ? N1Y C2Y C1Y 122.4(4) . . ? N1Y C3Y C4Y 124.2(4) . . ? C3Y C4Y C5Y 119.3(4) . . ? C1Y C5Y C4Y 117.1(4) . . ? C3Y N1Y C2Y 116.4(4) . . ? C2Z C1Z O6A 120.0(3) . . ? C5Z C1Z O6A 119.5(3) . . ? C5Z C1Z C2Z 120.4(3) . . ? C3Z C2Z C1Z 116.6(4) . . ? C2Z C3Z C4Z 119.7(4) . . ? N1Z C4Z C3Z 123.4(4) . . ? N1Z C5Z C1Z 123.2(4) . . ? C4Z N1Z C5Z 116.8(4) . . ? data_908590 _database_code_depnum_ccdc_archive 'CCDC 908590' #TrackingRef '17690_web_deposit_cif_file_1_RSuriyaNarayanan_1360734625.908590.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H48 Cl8 Cu4 N14 O12 P6, 8(C H Cl3)' _chemical_formula_sum 'C72 H56 Cl32 Cu4 N14 O12 P6 ' _chemical_formula_weight 2883.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.015(2) _cell_length_b 13.723(2) _cell_length_c 15.691(2) _cell_angle_alpha 79.250(3) _cell_angle_beta 77.262(3) _cell_angle_gamma 81.256(3) _cell_volume 2667.6(7) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2588 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 24.31 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.795 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 1.740 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.361007 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_wavelength 0.71073 _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14859 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_unetI/netI 0.0979 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10216 _reflns_number_gt 6626 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0902P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10216 _refine_ls_number_parameters 631 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1019 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1737 _refine_ls_wR_factor_gt 0.1427 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.981 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8453(5) 0.0144(5) 0.6909(4) 0.0172(13) Uani 1 1 d . . . C2 C 0.9105(5) -0.0381(5) 0.7469(4) 0.0182(13) Uani 1 1 d . . . H2 H 0.9603 -0.0051 0.7636 0.022 Uiso 1 1 calc R . . C3 C 0.8352(5) -0.1818(5) 0.7523(4) 0.0200(14) Uani 1 1 d . . . H3 H 0.8323 -0.2511 0.7731 0.024 Uiso 1 1 calc R . . C4 C 0.7679(5) -0.1329(5) 0.6967(4) 0.0246(15) Uani 1 1 d . . . H4 H 0.7187 -0.1674 0.6809 0.029 Uiso 1 1 calc R . . C5 C 0.7744(5) -0.0319(5) 0.6644(4) 0.0224(15) Uani 1 1 d . . . H5 H 0.7308 0.0040 0.6250 0.027 Uiso 1 1 calc R . . C7 C 1.1636(5) -0.2302(5) 0.9673(4) 0.0198(14) Uani 1 1 d . . . H7 H 1.1635 -0.1604 0.9479 0.024 Uiso 1 1 calc R . . C8 C 1.0973(5) -0.3765(5) 0.9721(4) 0.0203(14) Uani 1 1 d . . . H8 H 1.0485 -0.4113 0.9560 0.024 Uiso 1 1 calc R . . C9 C 1.1655(5) -0.4290(5) 1.0248(4) 0.0288(16) Uani 1 1 d . . . H9 H 1.1641 -0.4987 1.0440 0.035 Uiso 1 1 calc R . . C11 C 0.7661(5) 0.2788(5) 0.9793(4) 0.0188(14) Uani 1 1 d . . . C12 C 0.9362(5) -0.2003(5) 1.1727(4) 0.0194(14) Uani 1 1 d . . . H12 H 0.9427 -0.1316 1.1513 0.023 Uiso 1 1 calc R . . C13 C 0.8836(5) -0.3499(4) 1.1594(4) 0.0193(14) Uani 1 1 d . . . H13 H 0.8526 -0.3873 1.1285 0.023 Uiso 1 1 calc R . . C14 C 0.9217(5) -0.3972(5) 1.2334(4) 0.0227(15) Uani 1 1 d . . . H14 H 0.9162 -0.4664 1.2528 0.027 Uiso 1 1 calc R . . C15 C 0.7652(5) 0.3800(5) 0.9510(4) 0.0237(15) Uani 1 1 d . . . H15 H 0.7169 0.4149 0.9153 0.028 Uiso 1 1 calc R . . C16 C 0.6126(5) 0.0452(4) 0.8993(4) 0.0173(13) Uani 1 1 d . . . C17 C 0.6926(4) -0.0067(5) 0.9402(4) 0.0172(13) Uani 1 1 d . . . H17 H 0.7460 0.0276 0.9499 0.021 Uiso 1 1 calc R . . C18 C 0.6202(5) -0.1548(4) 0.9515(4) 0.0176(13) Uani 1 1 d . . . H18 H 0.6232 -0.2252 0.9685 0.021 Uiso 1 1 calc R . . C19 C 0.5381(5) -0.1033(5) 0.9115(4) 0.0208(14) Uani 1 1 d . . . H19 H 0.4842 -0.1382 0.9033 0.025 Uiso 1 1 calc R . . C20 C 0.5350(5) -0.0024(5) 0.8838(4) 0.0204(14) Uani 1 1 d . . . H20 H 0.4806 0.0335 0.8549 0.024 Uiso 1 1 calc R . . C21 C 0.6584(5) 0.5521(4) 0.7110(4) 0.0202(14) Uani 1 1 d . . . C22 C 0.6417(6) 0.5972(5) 0.7848(5) 0.0303(17) Uani 1 1 d . . . H22 H 0.6836 0.5748 0.8287 0.036 Uiso 1 1 calc R . . C23 C 0.5615(6) 0.6770(5) 0.7935(5) 0.0351(18) Uani 1 1 d . . . H23 H 0.5459 0.7072 0.8454 0.042 Uiso 1 1 calc R . . C24 C 0.5045(6) 0.7122(5) 0.7266(5) 0.0324(17) Uani 1 1 d . . . H24 H 0.4504 0.7667 0.7326 0.039 Uiso 1 1 calc R . . C25 C 0.5264(5) 0.6685(5) 0.6526(5) 0.0282(16) Uani 1 1 d . . . H25 H 0.4886 0.6949 0.6065 0.034 Uiso 1 1 calc R . . C26 C 0.6033(5) 0.5854(4) 0.6423(4) 0.0181(13) Uani 1 1 d . . . C27 C 0.6259(5) 0.5367(5) 0.5620(4) 0.0212(14) Uani 1 1 d . . . C28 C 0.6348(5) 0.5914(5) 0.4764(4) 0.0257(15) Uani 1 1 d . . . H28 H 0.6234 0.6622 0.4694 0.031 Uiso 1 1 calc R . . C29 C 0.6595(5) 0.5460(5) 0.4025(4) 0.0288(17) Uani 1 1 d . . . H29 H 0.6649 0.5851 0.3453 0.035 Uiso 1 1 calc R . . C30 C 0.6764(5) 0.4428(5) 0.4119(4) 0.0275(16) Uani 1 1 d . . . H30 H 0.6949 0.4112 0.3607 0.033 Uiso 1 1 calc R . . C31 C 0.6667(5) 0.3846(5) 0.4961(4) 0.0255(15) Uani 1 1 d . . . H31 H 0.6767 0.3137 0.5033 0.031 Uiso 1 1 calc R . . C32 C 0.6418(5) 0.4343(5) 0.5684(4) 0.0176(13) Uani 1 1 d . . . C33 C 0.5714(6) 0.9058(5) 0.3508(4) 0.0279(16) Uani 1 1 d . . . H33 H 0.6321 0.9031 0.2992 0.033 Uiso 1 1 calc R . . C34 C 0.5843(5) 0.5716(5) 0.1549(4) 0.0240(15) Uani 1 1 d . . . H34 H 0.5186 0.5560 0.1993 0.029 Uiso 1 1 calc R . . C35 C 0.0283(5) 0.3252(5) 0.4208(5) 0.0288(16) Uani 1 1 d . . . H35 H 0.0437 0.3297 0.3550 0.035 Uiso 1 1 calc R . . C36 C 0.8163(5) 0.0984(5) 0.3686(4) 0.0241(15) Uani 1 1 d . . . H36 H 0.8604 0.1553 0.3516 0.029 Uiso 1 1 calc R . . C6AA C 1.0253(4) 0.2452(4) 0.7532(4) 0.0165(13) Uani 1 1 d . . . C10C C 1.0324(5) 0.3456(5) 0.7202(4) 0.0246(15) Uani 1 1 d . . . H10C H 1.0069 0.3772 0.6684 0.030 Uiso 1 1 calc R . . Cl1 Cl 1.07471(13) -0.31541(12) 0.76318(10) 0.0246(4) Uani 1 1 d . . . Cl2 Cl 0.95536(11) -0.08088(11) 0.94288(10) 0.0179(3) Uani 1 1 d . . . Cl3 Cl 0.83780(12) -0.30602(11) 0.95977(10) 0.0197(3) Uani 1 1 d . . . Cl4 Cl 0.72813(12) -0.06882(12) 1.13951(10) 0.0237(4) Uani 1 1 d . . . Cl5 Cl 0.6223(2) 0.87780(16) 0.44840(15) 0.0650(7) Uani 1 1 d . . . Cl6 Cl 0.50256(15) 1.02594(14) 0.34063(15) 0.0450(5) Uani 1 1 d . . . Cl7 Cl 0.48842(15) 0.81580(14) 0.34947(13) 0.0379(5) Uani 1 1 d . . . Cl8 Cl 0.61346(13) 0.68793(12) 0.16611(11) 0.0264(4) Uani 1 1 d . . . Cl9 Cl 0.55917(13) 0.57264(13) 0.04778(11) 0.0314(4) Uani 1 1 d . . . Cl10 Cl 0.68726(13) 0.47636(12) 0.17670(11) 0.0291(4) Uani 1 1 d . . . Cl11 Cl 0.14859(15) 0.32866(16) 0.45580(15) 0.0482(5) Uani 1 1 d . . . Cl12 Cl -0.06341(15) 0.42633(14) 0.44934(12) 0.0384(5) Uani 1 1 d . . . Cl13 Cl -0.02174(14) 0.21131(13) 0.46829(12) 0.0338(4) Uani 1 1 d . . . Cl14 Cl 0.69289(14) 0.13823(13) 0.43251(12) 0.0344(4) Uani 1 1 d . . . Cl15 Cl 0.79934(14) 0.06135(14) 0.27151(11) 0.0322(4) Uani 1 1 d . . . Cl16 Cl 0.88283(13) -0.00121(13) 0.43191(11) 0.0305(4) Uani 1 1 d . . . Cu1 Cu 0.99824(6) -0.20976(6) 0.86166(5) 0.0185(2) Uani 1 1 d . . . Cu2 Cu 0.80203(6) -0.17557(5) 1.04067(5) 0.01722(19) Uani 1 1 d . . . N1 N 0.8181(4) 0.3012(4) 0.6690(3) 0.0170(11) Uani 1 1 d . . . N2 N 0.8055(4) 0.1629(4) 0.8169(3) 0.0184(11) Uani 1 1 d . . . N3 N 0.6573(4) 0.3222(4) 0.8080(3) 0.0213(12) Uani 1 1 d . . . N4 N 0.9036(4) -0.1362(4) 0.7780(3) 0.0195(12) Uani 1 1 d . . . N5 N 1.0970(4) -0.2778(4) 0.9425(3) 0.0164(11) Uani 1 1 d . . . N6 N 0.8891(4) -0.2517(4) 1.1294(3) 0.0185(11) Uani 1 1 d . . . N7 N 0.6949(4) -0.1067(4) 0.9663(3) 0.0195(12) Uani 1 1 d . . . O1 O 0.7419(3) 0.4725(3) 0.7028(3) 0.0184(9) Uani 1 1 d . . . O2 O 0.6249(3) 0.3763(3) 0.6533(3) 0.0192(10) Uani 1 1 d . . . O3 O 0.8515(3) 0.1145(3) 0.6579(3) 0.0194(10) Uani 1 1 d . . . O4 O 0.9843(3) 0.1856(3) 0.7086(3) 0.0176(9) Uani 1 1 d . . . O5 O 0.6956(3) 0.2238(3) 0.9593(3) 0.0180(9) Uani 1 1 d . . . O6AA O 0.6048(3) 0.1492(3) 0.8739(3) 0.0201(10) Uani 1 1 d . . . P1 P 0.71372(12) 0.36226(12) 0.71062(11) 0.0170(4) Uani 1 1 d . . . P2 P 0.85947(12) 0.19546(12) 0.71656(10) 0.0170(4) Uani 1 1 d . . . P3 P 0.69617(12) 0.21727(12) 0.85873(10) 0.0170(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.012(3) 0.018(3) 0.020(3) -0.002(3) -0.004(2) 0.003(3) C2 0.014(3) 0.019(3) 0.020(3) -0.002(3) -0.004(3) 0.002(3) C3 0.024(4) 0.011(3) 0.025(3) 0.002(3) -0.006(3) -0.004(3) C4 0.026(4) 0.023(4) 0.029(4) -0.007(3) -0.014(3) 0.002(3) C5 0.021(3) 0.020(4) 0.024(4) -0.002(3) -0.007(3) 0.006(3) C7 0.022(3) 0.016(3) 0.020(3) -0.001(3) -0.007(3) 0.005(3) C8 0.015(3) 0.017(3) 0.030(4) -0.006(3) -0.004(3) 0.000(3) C9 0.038(4) 0.012(3) 0.039(4) -0.003(3) -0.020(3) 0.006(3) C11 0.013(3) 0.026(4) 0.015(3) -0.004(3) -0.001(2) 0.003(3) C12 0.020(3) 0.016(3) 0.018(3) -0.003(3) 0.001(3) 0.008(3) C13 0.019(3) 0.012(3) 0.027(4) 0.002(3) -0.008(3) -0.001(3) C14 0.017(3) 0.015(3) 0.037(4) 0.000(3) -0.013(3) 0.001(3) C15 0.034(4) 0.010(3) 0.030(4) -0.001(3) -0.020(3) 0.007(3) C16 0.017(3) 0.012(3) 0.021(3) 0.001(3) -0.004(3) 0.000(3) C17 0.008(3) 0.026(4) 0.020(3) -0.008(3) -0.005(2) -0.001(3) C18 0.021(3) 0.008(3) 0.023(3) 0.000(3) -0.004(3) -0.003(3) C19 0.023(3) 0.019(4) 0.021(3) -0.001(3) -0.010(3) 0.001(3) C20 0.017(3) 0.026(4) 0.022(3) -0.007(3) -0.013(3) 0.001(3) C21 0.024(3) 0.010(3) 0.024(3) 0.002(3) -0.006(3) 0.001(3) C22 0.041(4) 0.012(3) 0.040(4) 0.000(3) -0.015(3) -0.004(3) C23 0.048(5) 0.019(4) 0.038(4) -0.008(3) -0.004(4) -0.006(3) C24 0.031(4) 0.010(3) 0.054(5) -0.003(3) -0.011(4) 0.007(3) C25 0.024(4) 0.019(4) 0.042(4) 0.001(3) -0.012(3) 0.001(3) C26 0.017(3) 0.012(3) 0.023(3) 0.004(3) -0.003(3) -0.006(3) C27 0.014(3) 0.019(3) 0.031(4) 0.004(3) -0.010(3) -0.004(3) C28 0.025(4) 0.021(4) 0.034(4) 0.003(3) -0.017(3) -0.003(3) C29 0.024(4) 0.033(4) 0.029(4) 0.012(3) -0.015(3) -0.009(3) C30 0.020(4) 0.042(5) 0.024(4) -0.011(3) -0.007(3) -0.005(3) C31 0.015(3) 0.029(4) 0.035(4) -0.006(3) -0.009(3) -0.003(3) C32 0.013(3) 0.020(3) 0.021(3) 0.002(3) -0.010(3) 0.001(3) C33 0.036(4) 0.017(4) 0.029(4) -0.001(3) -0.005(3) -0.003(3) C34 0.020(3) 0.030(4) 0.022(3) -0.007(3) -0.005(3) 0.003(3) C35 0.026(4) 0.031(4) 0.031(4) -0.006(3) -0.010(3) -0.001(3) C36 0.032(4) 0.014(3) 0.027(4) -0.006(3) -0.011(3) 0.004(3) C6AA 0.010(3) 0.016(3) 0.025(3) -0.001(3) -0.007(3) -0.003(2) C10C 0.023(4) 0.018(4) 0.032(4) 0.003(3) -0.014(3) 0.004(3) Cl1 0.0285(9) 0.0191(8) 0.0269(9) -0.0069(7) -0.0104(7) 0.0063(7) Cl2 0.0187(8) 0.0124(8) 0.0233(8) -0.0036(6) -0.0081(6) 0.0029(6) Cl3 0.0218(8) 0.0144(8) 0.0237(8) -0.0034(6) -0.0072(6) -0.0001(6) Cl4 0.0194(8) 0.0276(9) 0.0262(9) -0.0101(7) -0.0103(6) 0.0066(7) Cl5 0.116(2) 0.0349(12) 0.0627(15) 0.0113(10) -0.0598(15) -0.0272(13) Cl6 0.0316(10) 0.0241(10) 0.0811(15) -0.0085(10) -0.0180(10) 0.0023(8) Cl7 0.0411(11) 0.0290(10) 0.0479(12) -0.0111(9) -0.0101(9) -0.0091(8) Cl8 0.0243(9) 0.0251(9) 0.0318(9) -0.0082(7) -0.0109(7) 0.0037(7) Cl9 0.0311(10) 0.0342(10) 0.0335(10) -0.0094(8) -0.0146(8) -0.0008(8) Cl10 0.0309(9) 0.0227(9) 0.0329(10) -0.0010(7) -0.0115(7) 0.0020(7) Cl11 0.0304(11) 0.0507(13) 0.0692(15) -0.0096(11) -0.0179(10) -0.0101(9) Cl12 0.0378(11) 0.0314(11) 0.0438(11) -0.0007(8) -0.0103(9) -0.0002(8) Cl13 0.0395(11) 0.0269(10) 0.0368(10) 0.0031(8) -0.0143(8) -0.0097(8) Cl14 0.0301(10) 0.0297(10) 0.0445(11) -0.0144(8) -0.0094(8) 0.0063(8) Cl15 0.0321(10) 0.0380(11) 0.0300(10) -0.0092(8) -0.0111(8) -0.0031(8) Cl16 0.0276(9) 0.0296(10) 0.0324(10) -0.0013(8) -0.0087(7) 0.0026(7) Cu1 0.0195(4) 0.0139(4) 0.0233(4) -0.0036(3) -0.0097(3) 0.0029(3) Cu2 0.0166(4) 0.0131(4) 0.0228(4) -0.0017(3) -0.0092(3) 0.0020(3) N1 0.019(3) 0.010(3) 0.021(3) 0.002(2) -0.008(2) 0.001(2) N2 0.017(3) 0.017(3) 0.020(3) -0.002(2) -0.006(2) 0.004(2) N3 0.022(3) 0.013(3) 0.030(3) -0.005(2) -0.011(2) 0.005(2) N4 0.016(3) 0.023(3) 0.022(3) -0.008(2) -0.006(2) 0.000(2) N5 0.016(3) 0.014(3) 0.020(3) -0.007(2) -0.005(2) 0.005(2) N6 0.013(3) 0.020(3) 0.024(3) -0.006(2) -0.007(2) -0.002(2) N7 0.020(3) 0.014(3) 0.026(3) -0.002(2) -0.007(2) -0.004(2) O1 0.014(2) 0.014(2) 0.027(2) -0.0011(18) -0.0082(18) -0.0003(18) O2 0.017(2) 0.017(2) 0.024(2) 0.0026(18) -0.0118(18) 0.0013(18) O3 0.021(2) 0.015(2) 0.025(2) -0.0034(19) -0.0118(19) 0.0015(18) O4 0.012(2) 0.017(2) 0.027(2) -0.0047(18) -0.0087(18) -0.0005(17) O5 0.013(2) 0.017(2) 0.024(2) -0.0007(18) -0.0070(18) -0.0001(18) O6AA 0.022(2) 0.010(2) 0.027(2) 0.0031(18) -0.0088(19) 0.0024(18) P1 0.0152(8) 0.0142(8) 0.0218(9) 0.0000(7) -0.0086(7) 0.0009(6) P2 0.0152(8) 0.0138(8) 0.0216(9) -0.0002(7) -0.0080(7) 0.0027(6) P3 0.0169(8) 0.0127(8) 0.0214(9) -0.0015(7) -0.0073(7) 0.0018(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 C1 C5 1.369(9) . ? C1 O3 1.383(7) . ? C1 C2 1.385(8) . ? C2 N4 1.353(8) . ? C2 H2 0.9500 . ? C3 N4 1.330(8) . ? C3 C4 1.385(8) . ? C3 H3 0.9500 . ? C4 C5 1.393(9) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C7 N5 1.321(8) . ? C7 C11 1.389(8) 2_757 ? C7 H7 0.9500 . ? C8 N5 1.347(8) . ? C8 C9 1.377(8) . ? C8 H8 0.9500 . ? C9 C15 1.356(9) 2_757 ? C9 H9 0.9500 . ? C11 C15 1.375(9) . ? C11 C7 1.389(8) 2_757 ? C11 O5 1.393(7) . ? C12 N6 1.352(8) . ? C12 C6AA 1.371(8) 2_757 ? C12 H12 0.9500 . ? C13 N6 1.349(8) . ? C13 C14 1.375(8) . ? C13 H13 0.9500 . ? C14 C10C 1.378(9) 2_757 ? C14 H14 0.9500 . ? C15 C9 1.356(9) 2_757 ? C15 H15 0.9500 . ? C16 C20 1.368(8) . ? C16 C17 1.379(8) . ? C16 O6AA 1.403(7) . ? C17 N7 1.354(8) . ? C17 H17 0.9500 . ? C18 N7 1.338(8) . ? C18 C19 1.391(8) . ? C18 H18 0.9500 . ? C19 C20 1.369(9) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.373(9) . ? C21 C26 1.394(8) . ? C21 O1 1.421(7) . ? C22 C23 1.397(9) . ? C22 H22 0.9500 . ? C23 C24 1.390(10) . ? C23 H23 0.9500 . ? C24 C25 1.360(10) . ? C24 H24 0.9500 . ? C25 C26 1.407(8) . ? C25 H25 0.9500 . ? C26 C27 1.487(9) . ? C27 C32 1.376(9) . ? C27 C28 1.400(9) . ? C28 C29 1.371(10) . ? C28 H28 0.9500 . ? C29 C30 1.385(10) . ? C29 H29 0.9500 . ? C30 C31 1.402(9) . ? C30 H30 0.9500 . ? C31 C32 1.385(9) . ? C31 H31 0.9500 . ? C32 O2 1.409(7) . ? C33 Cl6 1.750(7) . ? C33 Cl5 1.756(7) . ? C33 Cl7 1.765(7) . ? C33 H33 1.0000 . ? C34 Cl8 1.744(7) . ? C34 Cl10 1.767(6) . ? C34 Cl9 1.779(6) . ? C34 H34 1.0000 . ? C35 Cl12 1.744(7) . ? C35 Cl13 1.755(7) . ? C35 Cl11 1.780(7) . ? C35 H35 1.0000 . ? C36 Cl15 1.762(6) . ? C36 Cl14 1.764(6) . ? C36 Cl16 1.765(6) . ? C36 H36 1.0000 . ? C6AA C12 1.371(8) 2_757 ? C6AA C10C 1.388(8) . ? C6AA O4 1.398(7) . ? C10C C14 1.378(9) 2_757 ? C10C H10C 0.9500 . ? Cl1 Cu1 2.2802(17) . ? Cl2 Cu1 2.3002(16) . ? Cl2 Cu2 2.5923(17) . ? Cl3 Cu2 2.3167(17) . ? Cl3 Cu1 2.6716(17) . ? Cl4 Cu2 2.2886(17) . ? Cu1 N5 2.012(5) . ? Cu1 N4 2.025(5) . ? Cu2 N7 2.025(5) . ? Cu2 N6 2.027(5) . ? N1 P1 1.563(5) . ? N1 P2 1.577(5) . ? N2 P3 1.568(5) . ? N2 P2 1.587(5) . ? N3 P3 1.578(5) . ? N3 P1 1.579(5) . ? O1 P1 1.587(4) . ? O2 P1 1.585(4) . ? O3 P2 1.598(4) . ? O4 P2 1.589(4) . ? O5 P3 1.595(4) . ? O6AA P3 1.572(4) . ? 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 C5 C1 O3 117.6(5) . . ? C5 C1 C2 121.0(6) . . ? O3 C1 C2 121.3(5) . . ? N4 C2 C1 120.3(6) . . ? N4 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? N4 C3 C4 123.0(6) . . ? N4 C3 H3 118.5 . . ? C4 C3 H3 118.5 . . ? C3 C4 C5 118.3(6) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? C1 C5 C4 118.2(6) . . ? C1 C5 H5 120.9 . . ? C4 C5 H5 120.9 . . ? N5 C7 C11 122.2(6) . 2_757 ? N5 C7 H7 118.9 . . ? C11 C7 H7 118.9 2_757 . ? N5 C8 C9 122.6(6) . . ? N5 C8 H8 118.7 . . ? C9 C8 H8 118.7 . . ? C15 C9 C8 119.3(6) 2_757 . ? C15 C9 H9 120.4 2_757 . ? C8 C9 H9 120.4 . . ? C15 C11 C7 119.3(6) . 2_757 ? C15 C11 O5 122.2(5) . . ? C7 C11 O5 118.5(6) 2_757 . ? N6 C12 C6AA 121.4(6) . 2_757 ? N6 C12 H12 119.3 . . ? C6AA C12 H12 119.3 2_757 . ? N6 C13 C14 121.7(6) . . ? N6 C13 H13 119.2 . . ? C14 C13 H13 119.2 . . ? C13 C14 C10C 120.9(6) . 2_757 ? C13 C14 H14 119.5 . . ? C10C C14 H14 119.5 2_757 . ? C9 C15 C11 118.7(6) 2_757 . ? C9 C15 H15 120.6 2_757 . ? C11 C15 H15 120.6 . . ? C20 C16 C17 121.3(6) . . ? C20 C16 O6AA 116.8(5) . . ? C17 C16 O6AA 121.9(5) . . ? N7 C17 C16 119.9(6) . . ? N7 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? N7 C18 C19 121.0(6) . . ? N7 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C20 C19 C18 120.1(6) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C16 C20 C19 117.9(6) . . ? C16 C20 H20 121.0 . . ? C19 C20 H20 121.0 . . ? C22 C21 C26 123.2(6) . . ? C22 C21 O1 117.2(5) . . ? C26 C21 O1 119.4(5) . . ? C21 C22 C23 118.3(7) . . ? C21 C22 H22 120.9 . . ? C23 C22 H22 120.9 . . ? C24 C23 C22 120.2(7) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C25 C24 C23 119.9(6) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 122.0(6) . . ? C24 C25 H25 119.0 . . ? C26 C25 H25 119.0 . . ? C21 C26 C25 116.2(6) . . ? C21 C26 C27 121.7(5) . . ? C25 C26 C27 122.0(6) . . ? C32 C27 C28 116.5(6) . . ? C32 C27 C26 121.1(6) . . ? C28 C27 C26 122.4(6) . . ? C29 C28 C27 122.1(6) . . ? C29 C28 H28 118.9 . . ? C27 C28 H28 118.9 . . ? C28 C29 C30 119.5(6) . . ? C28 C29 H29 120.2 . . ? C30 C29 H29 120.2 . . ? C29 C30 C31 120.6(6) . . ? C29 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C32 C31 C30 117.4(6) . . ? C32 C31 H31 121.3 . . ? C30 C31 H31 121.3 . . ? C27 C32 C31 123.8(6) . . ? C27 C32 O2 118.4(5) . . ? C31 C32 O2 117.7(6) . . ? Cl6 C33 Cl5 110.9(4) . . ? Cl6 C33 Cl7 110.8(4) . . ? Cl5 C33 Cl7 109.9(4) . . ? Cl6 C33 H33 108.4 . . ? Cl5 C33 H33 108.4 . . ? Cl7 C33 H33 108.4 . . ? Cl8 C34 Cl10 111.5(4) . . ? Cl8 C34 Cl9 111.3(4) . . ? Cl10 C34 Cl9 110.0(3) . . ? Cl8 C34 H34 108.0 . . ? Cl10 C34 H34 108.0 . . ? Cl9 C34 H34 108.0 . . ? Cl12 C35 Cl13 111.3(4) . . ? Cl12 C35 Cl11 110.3(4) . . ? Cl13 C35 Cl11 109.4(4) . . ? Cl12 C35 H35 108.6 . . ? Cl13 C35 H35 108.6 . . ? Cl11 C35 H35 108.6 . . ? Cl15 C36 Cl14 110.8(4) . . ? Cl15 C36 Cl16 110.2(3) . . ? Cl14 C36 Cl16 109.7(4) . . ? Cl15 C36 H36 108.7 . . ? Cl14 C36 H36 108.7 . . ? Cl16 C36 H36 108.7 . . ? C12 C6AA C10C 121.1(6) 2_757 . ? C12 C6AA O4 118.0(5) 2_757 . ? C10C C6AA O4 120.8(5) . . ? C14 C10C C6AA 116.5(6) 2_757 . ? C14 C10C H10C 121.7 2_757 . ? C6AA C10C H10C 121.7 . . ? Cu1 Cl2 Cu2 88.00(6) . . ? Cu2 Cl3 Cu1 85.79(5) . . ? N5 Cu1 N4 177.3(2) . . ? N5 Cu1 Cl1 89.82(14) . . ? N4 Cu1 Cl1 90.49(15) . . ? N5 Cu1 Cl2 89.08(14) . . ? N4 Cu1 Cl2 89.95(15) . . ? Cl1 Cu1 Cl2 165.73(7) . . ? N5 Cu1 Cl3 92.00(15) . . ? N4 Cu1 Cl3 90.61(15) . . ? Cl1 Cu1 Cl3 102.01(6) . . ? Cl2 Cu1 Cl3 92.25(6) . . ? N7 Cu2 N6 171.0(2) . . ? N7 Cu2 Cl4 87.60(15) . . ? N6 Cu2 Cl4 88.58(15) . . ? N7 Cu2 Cl3 89.75(15) . . ? N6 Cu2 Cl3 91.76(15) . . ? Cl4 Cu2 Cl3 164.54(7) . . ? N7 Cu2 Cl2 93.78(15) . . ? N6 Cu2 Cl2 95.01(15) . . ? Cl4 Cu2 Cl2 101.44(6) . . ? Cl3 Cu2 Cl2 93.93(6) . . ? P1 N1 P2 121.7(3) . . ? P3 N2 P2 121.1(3) . . ? P3 N3 P1 121.5(3) . . ? C3 N4 C2 119.0(5) . . ? C3 N4 Cu1 121.8(4) . . ? C2 N4 Cu1 119.2(4) . . ? C7 N5 C8 117.9(5) . . ? C7 N5 Cu1 122.9(4) . . ? C8 N5 Cu1 119.3(4) . . ? C13 N6 C12 118.3(5) . . ? C13 N6 Cu2 121.1(4) . . ? C12 N6 Cu2 119.2(4) . . ? C18 N7 C17 119.8(5) . . ? C18 N7 Cu2 121.8(4) . . ? C17 N7 Cu2 118.0(4) . . ? C21 O1 P1 119.2(4) . . ? C32 O2 P1 118.9(4) . . ? C1 O3 P2 123.7(4) . . ? C6AA O4 P2 118.5(4) . . ? C11 O5 P3 120.1(4) . . ? C16 O6AA P3 126.8(4) . . ? N1 P1 N3 118.2(3) . . ? N1 P1 O2 112.4(3) . . ? N3 P1 O2 105.2(3) . . ? N1 P1 O1 105.9(3) . . ? N3 P1 O1 111.1(3) . . ? O2 P1 O1 103.3(2) . . ? N1 P2 N2 117.3(3) . . ? N1 P2 O4 110.5(3) . . ? N2 P2 O4 109.0(2) . . ? N1 P2 O3 107.8(2) . . ? N2 P2 O3 110.7(3) . . ? O4 P2 O3 100.3(2) . . ? N2 P3 O6AA 111.2(3) . . ? N2 P3 N3 117.6(3) . . ? O6AA P3 N3 107.3(3) . . ? N2 P3 O5 109.3(2) . . ? O6AA P3 O5 99.1(2) . . ? N3 P3 O5 110.8(3) . . ? 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 C5 C1 C2 N4 -1.4(9) . . . . ? O3 C1 C2 N4 -179.5(5) . . . . ? N4 C3 C4 C5 1.7(10) . . . . ? O3 C1 C5 C4 179.5(5) . . . . ? C2 C1 C5 C4 1.3(9) . . . . ? C3 C4 C5 C1 -1.4(9) . . . . ? N5 C8 C9 C15 0.6(10) . . . 2_757 ? N6 C13 C14 C10C -0.3(10) . . . 2_757 ? C7 C11 C15 C9 1.0(9) 2_757 . . 2_757 ? O5 C11 C15 C9 178.3(6) . . . 2_757 ? C20 C16 C17 N7 -0.4(9) . . . . ? O6AA C16 C17 N7 177.7(5) . . . . ? N7 C18 C19 C20 2.3(9) . . . . ? C17 C16 C20 C19 1.0(9) . . . . ? O6AA C16 C20 C19 -177.2(5) . . . . ? C18 C19 C20 C16 -1.9(9) . . . . ? C26 C21 C22 C23 3.7(10) . . . . ? O1 C21 C22 C23 178.7(6) . . . . ? C21 C22 C23 C24 -3.3(11) . . . . ? C22 C23 C24 C25 0.4(11) . . . . ? C23 C24 C25 C26 2.3(11) . . . . ? C22 C21 C26 C25 -1.1(10) . . . . ? O1 C21 C26 C25 -176.0(5) . . . . ? C22 C21 C26 C27 177.9(6) . . . . ? O1 C21 C26 C27 3.0(9) . . . . ? C24 C25 C26 C21 -2.0(10) . . . . ? C24 C25 C26 C27 179.0(6) . . . . ? C21 C26 C27 C32 42.8(9) . . . . ? C25 C26 C27 C32 -138.3(6) . . . . ? C21 C26 C27 C28 -135.7(6) . . . . ? C25 C26 C27 C28 43.3(9) . . . . ? C32 C27 C28 C29 -0.9(9) . . . . ? C26 C27 C28 C29 177.6(6) . . . . ? C27 C28 C29 C30 -0.1(10) . . . . ? C28 C29 C30 C31 1.2(10) . . . . ? C29 C30 C31 C32 -1.3(9) . . . . ? C28 C27 C32 C31 0.8(9) . . . . ? C26 C27 C32 C31 -177.7(6) . . . . ? C28 C27 C32 O2 -174.7(5) . . . . ? C26 C27 C32 O2 6.7(8) . . . . ? C30 C31 C32 C27 0.3(9) . . . . ? C30 C31 C32 O2 175.8(5) . . . . ? C12 C6AA C10C C14 -0.9(9) 2_757 . . 2_757 ? O4 C6AA C10C C14 -177.1(5) . . . 2_757 ? Cu2 Cl2 Cu1 N5 -90.77(15) . . . . ? Cu2 Cl2 Cu1 N4 91.79(15) . . . . ? Cu2 Cl2 Cu1 Cl1 -176.4(2) . . . . ? Cu2 Cl2 Cu1 Cl3 1.19(5) . . . . ? Cu2 Cl3 Cu1 N5 87.82(14) . . . . ? Cu2 Cl3 Cu1 N4 -91.31(15) . . . . ? Cu2 Cl3 Cu1 Cl1 178.06(5) . . . . ? Cu2 Cl3 Cu1 Cl2 -1.33(5) . . . . ? Cu1 Cl3 Cu2 N7 94.96(15) . . . . ? Cu1 Cl3 Cu2 N6 -93.96(15) . . . . ? Cu1 Cl3 Cu2 Cl4 175.0(2) . . . . ? Cu1 Cl3 Cu2 Cl2 1.19(5) . . . . ? Cu1 Cl2 Cu2 N7 -91.38(15) . . . . ? Cu1 Cl2 Cu2 N6 90.74(15) . . . . ? Cu1 Cl2 Cu2 Cl4 -179.69(5) . . . . ? Cu1 Cl2 Cu2 Cl3 -1.37(6) . . . . ? C4 C3 N4 C2 -1.8(9) . . . . ? C4 C3 N4 Cu1 178.6(5) . . . . ? C1 C2 N4 C3 1.6(9) . . . . ? C1 C2 N4 Cu1 -178.8(4) . . . . ? N5 Cu1 N4 C3 157(4) . . . . ? Cl1 Cu1 N4 C3 60.7(5) . . . . ? Cl2 Cu1 N4 C3 -133.6(5) . . . . ? Cl3 Cu1 N4 C3 -41.4(5) . . . . ? N5 Cu1 N4 C2 -23(4) . . . . ? Cl1 Cu1 N4 C2 -119.0(4) . . . . ? Cl2 Cu1 N4 C2 46.7(4) . . . . ? Cl3 Cu1 N4 C2 139.0(4) . . . . ? C11 C7 N5 C8 1.2(9) 2_757 . . . ? C11 C7 N5 Cu1 -177.7(4) 2_757 . . . ? C9 C8 N5 C7 -1.6(9) . . . . ? C9 C8 N5 Cu1 177.4(5) . . . . ? N4 Cu1 N5 C7 24(4) . . . . ? Cl1 Cu1 N5 C7 120.5(5) . . . . ? Cl2 Cu1 N5 C7 -45.2(5) . . . . ? Cl3 Cu1 N5 C7 -137.5(4) . . . . ? N4 Cu1 N5 C8 -155(4) . . . . ? Cl1 Cu1 N5 C8 -58.4(4) . . . . ? Cl2 Cu1 N5 C8 135.9(4) . . . . ? Cl3 Cu1 N5 C8 43.6(4) . . . . ? C14 C13 N6 C12 1.8(9) . . . . ? C14 C13 N6 Cu2 -164.6(5) . . . . ? C6AA C12 N6 C13 -2.0(8) 2_757 . . . ? C6AA C12 N6 Cu2 164.7(4) 2_757 . . . ? N7 Cu2 N6 C13 57.5(15) . . . . ? Cl4 Cu2 N6 C13 122.5(5) . . . . ? Cl3 Cu2 N6 C13 -42.0(5) . . . . ? Cl2 Cu2 N6 C13 -136.1(4) . . . . ? N7 Cu2 N6 C12 -108.8(13) . . . . ? Cl4 Cu2 N6 C12 -43.8(4) . . . . ? Cl3 Cu2 N6 C12 151.7(4) . . . . ? Cl2 Cu2 N6 C12 57.6(4) . . . . ? C19 C18 N7 C17 -1.7(9) . . . . ? C19 C18 N7 Cu2 170.5(4) . . . . ? C16 C17 N7 C18 0.8(9) . . . . ? C16 C17 N7 Cu2 -171.8(4) . . . . ? N6 Cu2 N7 C18 -50.4(15) . . . . ? Cl4 Cu2 N7 C18 -115.5(5) . . . . ? Cl3 Cu2 N7 C18 49.3(5) . . . . ? Cl2 Cu2 N7 C18 143.2(5) . . . . ? N6 Cu2 N7 C17 122.0(12) . . . . ? Cl4 Cu2 N7 C17 56.9(4) . . . . ? Cl3 Cu2 N7 C17 -138.4(4) . . . . ? Cl2 Cu2 N7 C17 -44.4(4) . . . . ? C22 C21 O1 P1 111.7(6) . . . . ? C26 C21 O1 P1 -73.0(6) . . . . ? C27 C32 O2 P1 -78.8(6) . . . . ? C31 C32 O2 P1 105.4(5) . . . . ? C5 C1 O3 P2 137.1(5) . . . . ? C2 C1 O3 P2 -44.7(7) . . . . ? C12 C6AA O4 P2 106.9(5) 2_757 . . . ? C10C C6AA O4 P2 -76.8(6) . . . . ? C15 C11 O5 P3 61.5(7) . . . . ? C7 C11 O5 P3 -121.2(5) 2_757 . . . ? C20 C16 O6AA P3 -161.3(4) . . . . ? C17 C16 O6AA P3 20.6(8) . . . . ? P2 N1 P1 N3 7.9(5) . . . . ? P2 N1 P1 O2 -114.9(4) . . . . ? P2 N1 P1 O1 133.1(3) . . . . ? P3 N3 P1 N1 -7.3(5) . . . . ? P3 N3 P1 O2 119.1(4) . . . . ? P3 N3 P1 O1 -129.8(3) . . . . ? C32 O2 P1 N1 -66.0(5) . . . . ? C32 O2 P1 N3 164.1(4) . . . . ? C32 O2 P1 O1 47.6(5) . . . . ? C21 O1 P1 N1 162.0(4) . . . . ? C21 O1 P1 N3 -68.5(5) . . . . ? C21 O1 P1 O2 43.7(4) . . . . ? P1 N1 P2 N2 -12.6(5) . . . . ? P1 N1 P2 O4 -138.3(3) . . . . ? P1 N1 P2 O3 113.1(4) . . . . ? P3 N2 P2 N1 17.2(5) . . . . ? P3 N2 P2 O4 143.5(3) . . . . ? P3 N2 P2 O3 -107.1(4) . . . . ? C6AA O4 P2 N1 67.3(5) . . . . ? C6AA O4 P2 N2 -62.9(5) . . . . ? C6AA O4 P2 O3 -179.2(4) . . . . ? C1 O3 P2 N1 -156.9(4) . . . . ? C1 O3 P2 N2 -27.4(5) . . . . ? C1 O3 P2 O4 87.5(4) . . . . ? P2 N2 P3 O6AA 107.5(4) . . . . ? P2 N2 P3 N3 -16.6(5) . . . . ? P2 N2 P3 O5 -144.1(3) . . . . ? C16 O6AA P3 N2 35.8(5) . . . . ? C16 O6AA P3 N3 165.6(5) . . . . ? C16 O6AA P3 O5 -79.1(5) . . . . ? P1 N3 P3 N2 11.6(5) . . . . ? P1 N3 P3 O6AA -114.5(4) . . . . ? P1 N3 P3 O5 138.3(3) . . . . ? C11 O5 P3 N2 63.8(5) . . . . ? C11 O5 P3 O6AA -179.8(4) . . . . ? C11 O5 P3 N3 -67.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.254 _refine_diff_density_min -0.704 _refine_diff_density_rms 0.164 data_908591 _database_code_depnum_ccdc_archive 'CCDC 908591' #TrackingRef '17691_web_deposit_cif_file_2_RSuriyaNarayanan_1360734625.908591.cif' _audit_creation_date 2013-02-05 _audit_creation_method ; Olex2 1.2 (compiled Dec 5 2012 16:20:19, GUI svn.r4385) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C64 H48 Ag4 N14 O12 P6, 2(C H4 O), 3(N O3), 2(H2 O), 2(C1.5 N O2)' _chemical_formula_sum 'C69 H60 Ag4 N19 O29 P6' _chemical_formula_weight 2236.66 _chemical_melting_point ? 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z+1/2' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x, -y, z-1/2' 7 '-x+1/2, -y+1/2, -z' 8 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.730(2) _cell_length_b 11.791(3) _cell_length_c 26.394(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.26(3) _cell_angle_gamma 90.00 _cell_volume 7987.0(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8096 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.26 _cell_measurement_theta_min 2.32 _exptl_absorpt_coefficient_mu 1.184 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.628292 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS v.2.10 (Bruker,2003) was used for absorption correction. R(int) was 0.0967 before and 0.0262 after correction. The Ratio of minimum to maximum transmission is 0.6283. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.860 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 4468 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_unetI/netI 0.0529 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 21219 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 2.32 _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.980 _diffrn_measured_fraction_theta_max 0.980 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 6579 _reflns_number_total 7720 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'SAINT v6.45A (Bruker, 2003)' _computing_data_collection ? _computing_data_reduction 'SAINT v6.45A (Bruker, 2003)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 1.138 _refine_diff_density_min -0.930 _refine_diff_density_rms 0.114 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 612 _refine_ls_number_reflns 7720 _refine_ls_number_restraints 76 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0452 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+19.3021P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1143 _refine_ls_wR_factor_ref 0.1199 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: H4 of C4, H3 of C3, H8 of C8, H2 of C2, H5 of C5, H10 of C10, H9 of C9, H11 of C11, H20 of C20, H25 of C25, H16 of C16, H30 of C30, H19 of C19, H27 of C27, H15 of C15, H31 of C31, H17 of C17, H22 of C22, H24 of C24, H26 of C26, H29 of C29, H14 of C14, H21 of C21, H32 of C32 At 1.5 times of: H13 of O13, {H33A,H33B,H33C} of C33, {H12A,H12B} of O12 2. Restrained distances N10-C34 = N10-C37 = N10-C36 = N10-O15 = N10-O16 = N10-O14 1.24 with sigma of 0.02 N10-C34 1.26 with sigma of 0.02 N10-C34 = N10-C37 = N10-C36 = N10-O15 = N10-O16 = N10-O14 1.26 with sigma of 0.02 O18-C36 1.46 with sigma of 0.02 N10-C34 = N10-C37 = N10-C36 = N10-O15 = N10-O16 = N10-O14 1.26 with sigma of 0.02 N10-C34 1.26 with sigma of 0.02 N10-C34 1.26 with sigma of 0.02 N10-C34 1.26 with sigma of 0.02 N10-C34 1.26 with sigma of 0.02 O18-C36 1.46 with sigma of 0.02 C34-C37 2.1 with sigma of 0.04 C36-C34 2 with sigma of 0.04 C34-C36 2 with sigma of 0.04 C36-C37 2 with sigma of 0.04 C34-C37 2 with sigma of 0.04 C37-C34 1.8 with sigma of 0.04 C37-C34 1.8 with sigma of 0.04 C37-O18 2 with sigma of 0.04 C37-C34 2 with sigma of 0.04 3. Uiso/Uaniso restraints and constraints Uanis(N10) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O14) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O15) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C37) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C36) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O16) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C34) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C36) = Uanis(O16) Uanis(C37) = Uanis(O15) 4. Others Fixed Sof: O7(0.5) O8A(0.5) O8B(0.5) C34(0.5) O18(0.5) C37(0.5) C36(0.5) O15(0.5) O16(0.5) O14(0.5) 5.a Free rotating group: O12(H12A,H12B) 5.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32) 5.c Idealised Me refined as rotating group: C33(H33A,H33B,H33C) 5.d Idealised tetrahedral OH refined as rotating group: O13(H13) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Ag1 Ag 0.111099(13) 0.69211(3) -0.061535(14) 0.02940(11) Uani 1 1 d . . . Ag2 Ag 0.134742(13) 0.95848(3) -0.050188(13) 0.02971(11) Uani 1 1 d . . . C1 C 0.34078(17) 0.7909(4) 0.36956(18) 0.0266(9) Uani 1 1 d . . . C2 C 0.38659(18) 0.8382(4) 0.3702(2) 0.0377(11) Uani 1 1 d . . . H2 H 0.3953 0.8358 0.3395 0.045 Uiso 1 1 calc R . . C3 C 0.4192(2) 0.8895(4) 0.4183(3) 0.0501(15) Uani 1 1 d . . . H3 H 0.4501 0.9227 0.4198 0.060 Uiso 1 1 calc R . . C4 C 0.4066(2) 0.8922(5) 0.4639(3) 0.0593(19) Uani 1 1 d . . . H4 H 0.4288 0.9270 0.4958 0.071 Uiso 1 1 calc R . . C5 C 0.3613(2) 0.8432(4) 0.4618(2) 0.0446(13) Uani 1 1 d . . . H5 H 0.3533 0.8447 0.4929 0.054 Uiso 1 1 calc R . . C6 C 0.32652(19) 0.7906(4) 0.41427(19) 0.0327(10) Uani 1 1 d . . . C7 C 0.2782(2) 0.7352(4) 0.41354(18) 0.0310(10) Uani 1 1 d . . . C8 C 0.2777(3) 0.6732(4) 0.4587(2) 0.0480(15) Uani 1 1 d . . . H8 H 0.3082 0.6660 0.4897 0.058 Uiso 1 1 calc R . . C9 C 0.2319(3) 0.6222(4) 0.4576(3) 0.060(2) Uani 1 1 d . . . H9 H 0.2327 0.5784 0.4872 0.072 Uiso 1 1 calc R . . C10 C 0.1863(3) 0.6352(4) 0.4141(3) 0.0532(17) Uani 1 1 d . . . H10 H 0.1558 0.6038 0.4150 0.064 Uiso 1 1 calc R . . C11 C 0.1851(2) 0.6946(4) 0.3689(2) 0.0380(12) Uani 1 1 d . . . H11 H 0.1540 0.7028 0.3388 0.046 Uiso 1 1 calc R . . C12 C 0.23104(18) 0.7426(3) 0.36889(18) 0.0264(9) Uani 1 1 d . . . C13 C 0.11594(15) 0.6630(3) 0.10652(17) 0.0222(8) Uani 1 1 d . . . C14 C 0.12919(16) 0.6675(3) 0.06117(18) 0.0241(9) Uani 1 1 d . . . H14 H 0.1631 0.6507 0.0648 0.029 Uiso 1 1 calc R . . C15 C 0.04492(17) 0.7201(4) 0.00742(19) 0.0308(10) Uani 1 1 d . . . H15 H 0.0203 0.7398 -0.0267 0.037 Uiso 1 1 calc R . . C16 C 0.03025(17) 0.7170(4) 0.0517(2) 0.0352(11) Uani 1 1 d . . . H16 H -0.0038 0.7343 0.0472 0.042 Uiso 1 1 calc R . . C17 C 0.06587(16) 0.6882(4) 0.10237(19) 0.0289(10) Uani 1 1 d . . . H17 H 0.0567 0.6857 0.1328 0.035 Uiso 1 1 calc R . . C18 C 0.28649(15) 0.5688(3) 0.16560(16) 0.0193(8) Uani 1 1 d . . . C19 C 0.17187(15) 0.6222(3) -0.13205(17) 0.0210(8) Uani 1 1 d . . . H19 H 0.2003 0.6321 -0.0993 0.025 Uiso 1 1 calc R . . C20 C 0.08426(17) 0.6419(4) -0.18380(18) 0.0304(10) Uani 1 1 d . . . H20 H 0.0513 0.6654 -0.1868 0.037 Uiso 1 1 calc R . . C21 C 0.09002(17) 0.5937(4) -0.22880(19) 0.0307(10) Uani 1 1 d . . . H21 H 0.0615 0.5868 -0.2616 0.037 Uiso 1 1 calc R . . C22 C 0.32638(17) 0.5765(4) 0.21647(18) 0.0257(9) Uani 1 1 d . . . H22 H 0.3195 0.5821 0.2482 0.031 Uiso 1 1 calc R . . C23 C 0.14794(15) 0.9915(3) 0.11951(16) 0.0185(8) Uani 1 1 d . . . C24 C 0.15701(15) 0.9675(3) 0.07234(17) 0.0211(8) Uani 1 1 d . . . H24 H 0.1890 0.9375 0.0752 0.025 Uiso 1 1 calc R . . C25 C 0.07454(17) 1.0316(4) 0.01941(19) 0.0305(10) Uani 1 1 d . . . H25 H 0.0495 1.0472 -0.0150 0.037 Uiso 1 1 calc R . . C26 C 0.06331(17) 1.0551(4) 0.06464(19) 0.0346(11) Uani 1 1 d . . . H26 H 0.0310 1.0844 0.0608 0.042 Uiso 1 1 calc R . . C27 C 0.10055(16) 1.0348(4) 0.11582(18) 0.0267(9) Uani 1 1 d . . . H27 H 0.0939 1.0499 0.1472 0.032 Uiso 1 1 calc R . . C28 C 0.32065(15) 0.9272(3) 0.17592(17) 0.0200(8) Uani 1 1 d . . . C29 C 0.20298(16) 0.9398(3) -0.11900(17) 0.0215(8) Uani 1 1 d . . . H29 H 0.2305 0.9429 -0.0851 0.026 Uiso 1 1 calc R . . C30 C 0.11469(17) 0.9362(4) -0.17022(18) 0.0283(9) Uani 1 1 d . . . H30 H 0.0806 0.9390 -0.1720 0.034 Uiso 1 1 calc R . . C31 C 0.12307(17) 0.9245(4) -0.21836(18) 0.0283(9) Uani 1 1 d . . . H31 H 0.0951 0.9175 -0.2516 0.034 Uiso 1 1 calc R . . C32 C 0.36130(16) 0.9444(3) 0.22477(17) 0.0242(9) Uani 1 1 d . . . H32 H 0.3565 0.9800 0.2540 0.029 Uiso 1 1 calc R . . C33 C 0.0703(5) 0.1967(6) 0.7415(4) 0.107(4) Uani 1 1 d . . . H33A H 0.0967 0.1823 0.7270 0.160 Uiso 1 1 calc R . . H33B H 0.0377 0.1658 0.7171 0.160 Uiso 1 1 calc R . . H33C H 0.0800 0.1616 0.7768 0.160 Uiso 1 1 calc R . . N1 N 0.22848(13) 0.6659(3) 0.24601(14) 0.0217(7) Uani 1 1 d . . . N2 N 0.21926(12) 0.7808(3) 0.15445(13) 0.0191(7) Uani 1 1 d . . . N3 N 0.25782(13) 0.8868(3) 0.25236(14) 0.0198(7) Uani 1 1 d . . . N4 N 0.09383(13) 0.6956(3) 0.01190(14) 0.0234(7) Uani 1 1 d . . . N5 N 0.12462(13) 0.6560(3) -0.13559(14) 0.0252(7) Uani 1 1 d . . . N6 N 0.12033(13) 0.9871(3) 0.02281(14) 0.0233(7) Uani 1 1 d . . . N7 N 0.15369(14) 0.9437(3) -0.12121(15) 0.0255(8) Uani 1 1 d . . . N9 N 0.50173(14) 0.6402(4) 0.35250(17) 0.0381(10) Uani 1 1 d . . . O1 O 0.31048(11) 0.7300(2) 0.32209(11) 0.0233(6) Uani 1 1 d . . . O2 O 0.22716(11) 0.8080(2) 0.32317(11) 0.0219(6) Uani 1 1 d . . . O3 O 0.15121(10) 0.6303(2) 0.15798(12) 0.0245(6) Uani 1 1 d . . . O4 O 0.23407(11) 0.5661(2) 0.15920(11) 0.0205(6) Uani 1 1 d . . . O5 O 0.27051(10) 0.9675(2) 0.16704(11) 0.0198(6) Uani 1 1 d . . . O6 O 0.18503(10) 0.9768(2) 0.17177(11) 0.0201(6) Uani 1 1 d . . . O9 O 0.47886(16) 0.7267(4) 0.3292(2) 0.0681(13) Uani 1 1 d . . . O10 O 0.48921(14) 0.5441(4) 0.32989(17) 0.0548(11) Uani 1 1 d . . . O11 O 0.53759(12) 0.6447(3) 0.39950(13) 0.0388(8) Uani 1 1 d . . . O12 O 0.05758(18) 0.1289(4) 0.90037(17) 0.0577(11) Uani 1 1 d G . . H12A H 0.0332 0.0870 0.8796 0.087 Uiso 1 1 d G . . H12B H 0.0576 0.1914 0.8843 0.087 Uiso 1 1 d G . . O13 O 0.06514(18) 0.3121(4) 0.7465(2) 0.0713(14) Uani 1 1 d . . . H13 H 0.0399 0.3247 0.7546 0.107 Uiso 1 1 calc R . . P1 P 0.25463(4) 0.77283(8) 0.28275(4) 0.0195(2) Uani 1 1 d . . . P2 P 0.21054(4) 0.66799(8) 0.18234(4) 0.0189(2) Uani 1 1 d . . . P3 P 0.23418(4) 0.89516(8) 0.18852(4) 0.0179(2) Uani 1 1 d . . . N8 N 0.2500 0.7500 0.0000 0.0371(14) Uani 1 2 d S . . O7 O 0.2847(2) 0.8350(6) -0.0003(3) 0.0324(14) Uani 0.50 1 d P A -1 O8A O 0.2331(3) 0.8435(6) 0.0088(3) 0.0412(17) Uani 0.50 1 d P A -1 O8B O 0.2127(3) 0.7746(8) 0.0051(3) 0.048(2) Uani 0.50 1 d P A -1 C34 C 0.0318(5) 0.3308(10) 0.8369(6) 0.053(4) Uani 0.50 1 d PDU . . O18 O 0.0249(3) 0.5505(6) 0.8983(3) 0.0457(18) Uani 0.50 1 d PD . . C37 C -0.0047(11) 0.468(3) 0.8360(13) 0.106(4) Uani 0.50 1 d PDU B 1 C36 C 0.0571(16) 0.447(3) 0.9105(7) 0.105(5) Uani 0.50 1 d PDU B 1 O15 O -0.0040(7) 0.4476(19) 0.8251(8) 0.106(4) Uani 0.50 1 d PDU B 2 O16 O 0.0637(10) 0.4633(17) 0.9090(6) 0.105(5) Uani 0.50 1 d PDU B 2 O14 O 0.0563(5) 0.3414(7) 0.8434(4) 0.060(3) Uani 0.50 1 d PDU B . N10 N 0.0388(3) 0.4194(8) 0.8620(3) 0.134(3) Uani 1 1 d DU B . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.03076(19) 0.0363(2) 0.0278(2) -0.00132(14) 0.01871(15) 0.00556(14) Ag2 0.02529(19) 0.0456(2) 0.02368(19) -0.00579(14) 0.01541(14) -0.00303(14) C1 0.028(2) 0.022(2) 0.024(2) 0.0004(17) 0.0042(18) 0.0058(17) C2 0.033(2) 0.027(2) 0.044(3) 0.012(2) 0.004(2) 0.007(2) C3 0.031(3) 0.028(3) 0.068(4) 0.004(3) -0.008(3) 0.001(2) C4 0.057(4) 0.033(3) 0.054(4) -0.009(3) -0.018(3) 0.019(3) C5 0.052(3) 0.034(3) 0.033(3) -0.004(2) -0.001(2) 0.016(3) C6 0.041(3) 0.024(2) 0.027(2) 0.0018(19) 0.007(2) 0.015(2) C7 0.053(3) 0.020(2) 0.027(2) 0.0015(18) 0.023(2) 0.010(2) C8 0.094(4) 0.031(3) 0.032(3) 0.008(2) 0.039(3) 0.025(3) C9 0.130(6) 0.021(2) 0.070(4) 0.015(3) 0.085(5) 0.019(3) C10 0.095(5) 0.026(3) 0.072(4) -0.007(3) 0.070(4) -0.007(3) C11 0.057(3) 0.028(2) 0.048(3) -0.015(2) 0.041(3) -0.011(2) C12 0.043(3) 0.021(2) 0.025(2) 0.0010(17) 0.025(2) 0.0052(19) C13 0.0204(19) 0.0199(19) 0.030(2) -0.0061(17) 0.0136(17) -0.0057(16) C14 0.0199(19) 0.026(2) 0.032(2) -0.0063(18) 0.0150(18) 0.0007(17) C15 0.020(2) 0.042(3) 0.031(2) -0.005(2) 0.0105(18) 0.0000(19) C16 0.018(2) 0.054(3) 0.039(3) -0.009(2) 0.017(2) -0.002(2) C17 0.023(2) 0.040(3) 0.030(2) -0.007(2) 0.0183(19) -0.0073(19) C18 0.0207(19) 0.0140(18) 0.026(2) 0.0019(16) 0.0115(17) 0.0004(15) C19 0.0207(19) 0.022(2) 0.022(2) 0.0018(16) 0.0098(16) -0.0004(16) C20 0.023(2) 0.038(2) 0.032(2) 0.003(2) 0.0125(19) 0.0072(19) C21 0.022(2) 0.042(3) 0.027(2) 0.000(2) 0.0075(18) 0.0011(19) C22 0.029(2) 0.029(2) 0.025(2) 0.0020(18) 0.0164(19) 0.0005(18) C23 0.0161(18) 0.0197(19) 0.022(2) -0.0015(16) 0.0096(16) -0.0026(15) C24 0.0175(19) 0.024(2) 0.025(2) -0.0009(16) 0.0115(17) -0.0006(16) C25 0.018(2) 0.047(3) 0.025(2) -0.005(2) 0.0072(18) 0.0030(19) C26 0.015(2) 0.056(3) 0.033(3) -0.008(2) 0.0099(19) 0.006(2) C27 0.019(2) 0.036(2) 0.026(2) -0.0070(19) 0.0099(18) 0.0024(17) C28 0.0212(19) 0.0158(18) 0.028(2) 0.0015(16) 0.0150(17) 0.0002(15) C29 0.023(2) 0.023(2) 0.020(2) 0.0010(16) 0.0097(17) 0.0015(16) C30 0.021(2) 0.037(2) 0.031(2) 0.004(2) 0.0139(18) 0.0019(18) C31 0.025(2) 0.034(2) 0.025(2) 0.0008(19) 0.0087(18) 0.0026(19) C32 0.027(2) 0.026(2) 0.023(2) -0.0018(17) 0.0133(18) -0.0008(17) C33 0.191(11) 0.051(5) 0.093(7) -0.012(4) 0.070(7) -0.007(5) N1 0.0269(17) 0.0174(16) 0.0254(19) 0.0026(14) 0.0153(15) 0.0018(14) N2 0.0210(16) 0.0188(16) 0.0215(18) -0.0006(14) 0.0126(14) 0.0018(13) N3 0.0234(17) 0.0155(16) 0.0247(18) -0.0017(13) 0.0138(14) -0.0005(13) N4 0.0192(16) 0.0287(19) 0.0258(19) -0.0071(15) 0.0125(15) -0.0029(14) N5 0.0246(17) 0.0270(18) 0.0258(19) 0.0028(15) 0.0115(15) 0.0062(15) N6 0.0164(16) 0.0316(19) 0.0223(18) -0.0029(15) 0.0076(14) -0.0015(14) N7 0.0226(18) 0.034(2) 0.0243(19) -0.0001(15) 0.0134(15) -0.0006(15) N9 0.0184(18) 0.062(3) 0.039(2) 0.008(2) 0.0162(18) -0.0041(19) O1 0.0233(14) 0.0248(15) 0.0238(15) 0.0018(12) 0.0113(12) 0.0031(12) O2 0.0255(14) 0.0230(14) 0.0238(15) 0.0000(11) 0.0168(12) 0.0044(11) O3 0.0209(14) 0.0280(15) 0.0299(16) -0.0004(13) 0.0158(13) -0.0039(12) O4 0.0217(14) 0.0202(13) 0.0247(15) -0.0002(11) 0.0147(12) 0.0006(11) O5 0.0195(14) 0.0190(13) 0.0246(15) 0.0023(11) 0.0124(12) 0.0018(11) O6 0.0193(14) 0.0242(14) 0.0191(14) 0.0007(11) 0.0100(11) 0.0050(11) O9 0.037(2) 0.085(3) 0.081(3) 0.035(3) 0.020(2) 0.012(2) O10 0.0299(19) 0.082(3) 0.054(2) -0.021(2) 0.0184(18) -0.0161(19) O11 0.0260(16) 0.058(2) 0.0334(19) -0.0021(17) 0.0124(14) -0.0046(16) O12 0.072(3) 0.052(2) 0.059(3) 0.003(2) 0.036(2) 0.012(2) O13 0.056(3) 0.054(3) 0.109(4) 0.010(2) 0.036(3) 0.007(2) P1 0.0219(5) 0.0195(5) 0.0213(5) 0.0010(4) 0.0131(4) 0.0026(4) P2 0.0194(5) 0.0192(5) 0.0227(5) -0.0004(4) 0.0131(4) 0.0004(4) P3 0.0181(5) 0.0184(5) 0.0207(5) 0.0007(4) 0.0114(4) 0.0015(4) N8 0.041(4) 0.040(4) 0.024(3) -0.006(3) 0.005(3) 0.005(3) O7 0.029(3) 0.039(4) 0.028(3) 0.002(3) 0.011(3) -0.003(3) O8A 0.050(5) 0.030(4) 0.040(4) -0.006(3) 0.013(4) 0.013(4) O8B 0.026(4) 0.061(6) 0.067(6) -0.007(4) 0.027(4) 0.001(4) C34 0.043(6) 0.063(8) 0.055(7) -0.011(6) 0.020(6) -0.024(6) O18 0.043(4) 0.057(5) 0.043(4) -0.016(4) 0.023(4) -0.009(4) C37 0.089(5) 0.106(6) 0.108(7) 0.016(5) 0.022(5) -0.001(4) C36 0.107(7) 0.115(7) 0.080(5) -0.002(4) 0.021(4) -0.033(6) O15 0.089(5) 0.106(6) 0.108(7) 0.016(5) 0.022(5) -0.001(4) O16 0.107(7) 0.115(7) 0.080(5) -0.002(4) 0.021(4) -0.033(6) O14 0.096(7) 0.030(4) 0.050(5) -0.012(4) 0.022(5) -0.030(5) N10 0.103(6) 0.164(7) 0.124(7) 0.061(6) 0.030(5) -0.008(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 Ag1 Ag2 3.1993(5) . ? Ag1 N4 2.166(3) . ? Ag1 N5 2.167(3) . ? Ag2 N6 2.138(3) . ? Ag2 N7 2.137(3) . ? C1 C2 1.381(7) . ? C1 C6 1.379(7) . ? C1 O1 1.412(5) . ? C2 H2 0.9300 . ? C2 C3 1.388(7) . ? C3 H3 0.9300 . ? C3 C4 1.372(9) . ? C4 H4 0.9300 . ? C4 C5 1.364(9) . ? C5 H5 0.9300 . ? C5 C6 1.405(7) . ? C6 C7 1.485(7) . ? C7 C8 1.403(6) . ? C7 C12 1.392(7) . ? C8 H8 0.9300 . ? C8 C9 1.396(9) . ? C9 H9 0.9300 . ? C9 C10 1.356(10) . ? C10 H10 0.9300 . ? C10 C11 1.373(8) . ? C11 H11 0.9300 . ? C11 C12 1.395(7) . ? C12 O2 1.401(5) . ? C13 C14 1.380(6) . ? C13 C17 1.383(6) . ? C13 O3 1.394(5) . ? C14 H14 0.9300 . ? C14 N4 1.340(6) . ? C15 H15 0.9300 . ? C15 C16 1.376(6) . ? C15 N4 1.348(5) . ? C16 H16 0.9300 . ? C16 C17 1.371(7) . ? C17 H17 0.9300 . ? C18 C22 1.382(6) . ? C18 C29 1.371(6) 7_565 ? C18 O4 1.399(5) . ? C19 H19 0.9300 . ? C19 C28 1.380(6) 7_565 ? C19 N5 1.339(5) . ? C20 H20 0.9300 . ? C20 C21 1.379(6) . ? C20 N5 1.349(6) . ? C21 H21 0.9300 . ? C21 C32 1.388(6) 7_565 ? C22 H22 0.9300 . ? C22 C31 1.383(6) 7_565 ? C23 C24 1.390(5) . ? C23 C27 1.378(5) . ? C23 O6 1.384(5) . ? C24 H24 0.9300 . ? C24 N6 1.337(5) . ? C25 H25 0.9300 . ? C25 C26 1.372(6) . ? C25 N6 1.345(5) . ? C26 H26 0.9300 . ? C26 C27 1.375(6) . ? C27 H27 0.9300 . ? C28 C19 1.380(6) 7_565 ? C28 C32 1.368(6) . ? C28 O5 1.403(5) . ? C29 C18 1.371(6) 7_565 ? C29 H29 0.9300 . ? C29 N7 1.347(5) . ? C30 H30 0.9300 . ? C30 C31 1.382(6) . ? C30 N7 1.338(6) . ? C31 C22 1.383(6) 7_565 ? C31 H31 0.9300 . ? C32 C21 1.388(6) 7_565 ? C32 H32 0.9300 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C33 O13 1.380(8) . ? N1 P1 1.589(3) . ? N1 P2 1.562(4) . ? N2 P2 1.583(3) . ? N2 P3 1.586(3) . ? N3 P1 1.585(3) . ? N3 P3 1.563(3) . ? N9 O9 1.234(6) . ? N9 O10 1.266(6) . ? N9 O11 1.263(5) . ? O1 P1 1.585(3) . ? O2 P1 1.583(3) . ? O3 P2 1.586(3) . ? O4 P2 1.595(3) . ? O5 P3 1.580(3) . ? O6 P3 1.588(3) . ? O12 H12A 0.8495 . ? O12 H12B 0.8501 . ? O13 H13 0.8200 . ? N8 O7 1.391(6) 7_565 ? N8 O7 1.391(6) . ? N8 O8A 1.254(6) . ? N8 O8A 1.254(6) 7_565 ? N8 O8B 1.130(7) . ? N8 O8B 1.130(7) 7_565 ? O7 O8A 1.540(10) . ? O8A O8B 0.975(10) . ? C34 C37 1.900(16) . ? C34 O15 1.66(2) . ? C34 O14 0.649(14) . ? C34 N10 1.213(7) . ? O18 C37 1.82(2) . ? O18 C36 1.478(14) . ? O18 O16 1.44(2) . ? C37 N10 1.273(11) . ? C36 N10 1.228(11) . ? O15 N10 1.262(10) . ? O16 N10 1.278(10) . ? O14 N10 1.227(10) . ? 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 N4 Ag1 Ag2 90.27(9) . . ? N4 Ag1 N5 169.49(13) . . ? N5 Ag1 Ag2 100.24(10) . . ? N6 Ag2 Ag1 97.91(9) . . ? N7 Ag2 Ag1 87.01(9) . . ? N7 Ag2 N6 174.61(13) . . ? C2 C1 O1 116.8(4) . . ? C6 C1 C2 123.4(4) . . ? C6 C1 O1 119.4(4) . . ? C1 C2 H2 121.2 . . ? C1 C2 C3 117.6(5) . . ? C3 C2 H2 121.2 . . ? C2 C3 H3 119.4 . . ? C4 C3 C2 121.2(6) . . ? C4 C3 H3 119.4 . . ? C3 C4 H4 120.3 . . ? C5 C4 C3 119.4(5) . . ? C5 C4 H4 120.3 . . ? C4 C5 H5 118.9 . . ? C4 C5 C6 122.2(6) . . ? C6 C5 H5 118.9 . . ? C1 C6 C5 116.1(5) . . ? C1 C6 C7 122.7(4) . . ? C5 C6 C7 121.2(5) . . ? C8 C7 C6 121.1(5) . . ? C12 C7 C6 122.5(4) . . ? C12 C7 C8 116.4(5) . . ? C7 C8 H8 119.7 . . ? C9 C8 C7 120.5(6) . . ? C9 C8 H8 119.7 . . ? C8 C9 H9 119.4 . . ? C10 C9 C8 121.3(5) . . ? C10 C9 H9 119.4 . . ? C9 C10 H10 120.0 . . ? C9 C10 C11 120.0(6) . . ? C11 C10 H10 120.0 . . ? C10 C11 H11 120.4 . . ? C10 C11 C12 119.1(6) . . ? C12 C11 H11 120.4 . . ? C7 C12 C11 122.6(4) . . ? C7 C12 O2 120.3(4) . . ? C11 C12 O2 116.9(4) . . ? C14 C13 C17 120.8(4) . . ? C14 C13 O3 122.5(3) . . ? C17 C13 O3 116.7(4) . . ? C13 C14 H14 119.5 . . ? N4 C14 C13 120.9(4) . . ? N4 C14 H14 119.5 . . ? C16 C15 H15 119.0 . . ? N4 C15 H15 119.0 . . ? N4 C15 C16 122.1(4) . . ? C15 C16 H16 120.0 . . ? C17 C16 C15 120.0(4) . . ? C17 C16 H16 120.0 . . ? C13 C17 H17 121.3 . . ? C16 C17 C13 117.5(4) . . ? C16 C17 H17 121.3 . . ? C22 C18 O4 122.1(3) . . ? C29 C18 C22 120.8(4) 7_565 . ? C29 C18 O4 117.0(4) 7_565 . ? C28 C19 H19 119.3 7_565 . ? N5 C19 H19 119.3 . . ? N5 C19 C28 121.4(4) . 7_565 ? C21 C20 H20 118.7 . . ? N5 C20 H20 118.7 . . ? N5 C20 C21 122.5(4) . . ? C20 C21 H21 120.2 . . ? C20 C21 C32 119.6(4) . 7_565 ? C32 C21 H21 120.2 7_565 . ? C18 C22 H22 121.3 . . ? C18 C22 C31 117.5(4) . 7_565 ? C31 C22 H22 121.3 7_565 . ? C27 C23 C24 120.2(4) . . ? C27 C23 O6 116.5(3) . . ? O6 C23 C24 123.3(3) . . ? C23 C24 H24 119.6 . . ? N6 C24 C23 120.8(4) . . ? N6 C24 H24 119.6 . . ? C26 C25 H25 118.6 . . ? N6 C25 H25 118.6 . . ? N6 C25 C26 122.7(4) . . ? C25 C26 H26 120.5 . . ? C25 C26 C27 119.1(4) . . ? C27 C26 H26 120.5 . . ? C23 C27 H27 120.8 . . ? C26 C27 C23 118.4(4) . . ? C26 C27 H27 120.8 . . ? C19 C28 O5 117.2(4) 7_565 . ? C32 C28 C19 121.4(4) . 7_565 ? C32 C28 O5 121.2(3) . . ? C18 C29 H29 119.3 7_565 . ? N7 C29 C18 121.4(4) . 7_565 ? N7 C29 H29 119.3 . . ? C31 C30 H30 118.7 . . ? N7 C30 H30 118.7 . . ? N7 C30 C31 122.6(4) . . ? C22 C31 H31 120.4 7_565 . ? C30 C31 C22 119.2(4) . 7_565 ? C30 C31 H31 120.4 . . ? C21 C32 H32 121.5 7_565 . ? C28 C32 C21 117.0(4) . 7_565 ? C28 C32 H32 121.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O13 C33 H33A 109.5 . . ? O13 C33 H33B 109.5 . . ? O13 C33 H33C 109.5 . . ? P2 N1 P1 122.0(2) . . ? P2 N2 P3 120.3(2) . . ? P3 N3 P1 121.2(2) . . ? C14 N4 Ag1 122.4(3) . . ? C14 N4 C15 118.7(4) . . ? C15 N4 Ag1 118.8(3) . . ? C19 N5 Ag1 119.6(3) . . ? C19 N5 C20 118.0(4) . . ? C20 N5 Ag1 120.6(3) . . ? C24 N6 Ag2 121.4(3) . . ? C24 N6 C25 118.8(4) . . ? C25 N6 Ag2 119.7(3) . . ? C29 N7 Ag2 123.2(3) . . ? C30 N7 Ag2 118.4(3) . . ? C30 N7 C29 118.4(4) . . ? O9 N9 O10 120.5(4) . . ? O9 N9 O11 121.2(5) . . ? O11 N9 O10 118.3(4) . . ? C1 O1 P1 121.6(3) . . ? C12 O2 P1 122.5(2) . . ? C13 O3 P2 123.7(2) . . ? C18 O4 P2 119.6(2) . . ? C28 O5 P3 118.9(2) . . ? C23 O6 P3 126.1(2) . . ? H12A O12 H12B 109.5 . . ? C33 O13 H13 109.5 . . ? N3 P1 N1 117.67(18) . . ? N3 P1 O1 111.94(17) . . ? O1 P1 N1 104.69(16) . . ? O2 P1 N1 113.22(17) . . ? O2 P1 N3 104.63(16) . . ? O2 P1 O1 104.01(15) . . ? N1 P2 N2 118.12(18) . . ? N1 P2 O3 106.87(17) . . ? N1 P2 O4 112.98(16) . . ? N2 P2 O3 111.39(17) . . ? N2 P2 O4 107.36(16) . . ? O3 P2 O4 98.38(15) . . ? N2 P3 O6 110.19(16) . . ? N3 P3 N2 118.07(17) . . ? N3 P3 O5 110.91(17) . . ? N3 P3 O6 107.68(16) . . ? O5 P3 N2 108.68(16) . . ? O5 P3 O6 99.76(14) . . ? O7 N8 O7 179.996(1) . 7_565 ? O8A N8 O7 71.0(5) 7_565 7_565 ? O8A N8 O7 109.0(5) . 7_565 ? O8A N8 O7 109.0(5) 7_565 . ? O8A N8 O7 71.0(5) . . ? O8A N8 O8A 179.995(2) . 7_565 ? O8B N8 O7 61.2(5) 7_565 . ? O8B N8 O7 118.8(5) . . ? O8B N8 O7 61.2(5) . 7_565 ? O8B N8 O7 118.8(5) 7_565 7_565 ? O8B N8 O8A 47.9(5) 7_565 7_565 ? O8B N8 O8A 132.1(5) . 7_565 ? O8B N8 O8A 132.1(5) 7_565 . ? O8B N8 O8A 47.9(5) . . ? O8B N8 O8B 180.0(8) 7_565 . ? N8 O7 O8A 50.3(3) . . ? N8 O8A O7 58.7(4) . . ? O8B O8A N8 59.4(6) . . ? O8B O8A O7 117.9(8) . . ? O8A O8B N8 72.7(6) . . ? O15 C34 C37 9.4(15) . . ? O14 C34 C37 109.9(17) . . ? O14 C34 O15 113(2) . . ? O14 C34 N10 75.8(11) . . ? N10 C34 C37 41.3(7) . . ? N10 C34 O15 49.3(8) . . ? C36 O18 C37 77.3(8) . . ? O16 O18 C37 80.9(7) . . ? O16 O18 C36 11(3) . . ? O18 C37 C34 112.9(9) . . ? N10 C37 C34 39.0(6) . . ? N10 C37 O18 75.0(10) . . ? N10 C36 O18 90.6(10) . . ? N10 O15 C34 46.7(7) . . ? N10 O16 O18 90.5(11) . . ? C34 O14 N10 73.4(11) . . ? C34 N10 C37 99.7(12) . . ? C34 N10 C36 135.4(17) . . ? C34 N10 O15 84.0(14) . . ? C34 N10 O16 142.6(13) . . ? C34 N10 O14 30.8(7) . . ? C37 N10 O16 113.4(16) . . ? C36 N10 C37 112.4(17) . . ? C36 N10 O15 129.4(18) . . ? C36 N10 O16 13(4) . . ? O15 N10 C37 17.2(19) . . ? O15 N10 O16 130.4(15) . . ? O14 N10 C37 123.9(14) . . ? O14 N10 C36 122.8(13) . . ? O14 N10 O15 106.7(13) . . ? O14 N10 O16 122.7(13) . . ? 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 Ag1 Ag2 N6 C24 83.4(3) . . . . ? Ag1 Ag2 N6 C25 -100.3(3) . . . . ? Ag1 Ag2 N7 C29 -101.5(3) . . . . ? Ag1 Ag2 N7 C30 77.3(3) . . . . ? Ag2 Ag1 N4 C14 -96.9(3) . . . . ? Ag2 Ag1 N4 C15 87.3(3) . . . . ? Ag2 Ag1 N5 C19 92.6(3) . . . . ? Ag2 Ag1 N5 C20 -102.7(3) . . . . ? C1 C2 C3 C4 0.6(7) . . . . ? C1 C6 C7 C8 139.4(5) . . . . ? C1 C6 C7 C12 -41.4(6) . . . . ? C1 O1 P1 N1 -164.3(3) . . . . ? C1 O1 P1 N3 67.1(3) . . . . ? C1 O1 P1 O2 -45.3(3) . . . . ? C2 C1 C6 C5 0.8(6) . . . . ? C2 C1 C6 C7 -177.4(4) . . . . ? C2 C1 O1 P1 -113.9(4) . . . . ? C2 C3 C4 C5 0.2(8) . . . . ? C3 C4 C5 C6 -0.6(8) . . . . ? C4 C5 C6 C1 0.1(7) . . . . ? C4 C5 C6 C7 178.3(4) . . . . ? C5 C6 C7 C8 -38.6(6) . . . . ? C5 C6 C7 C12 140.6(4) . . . . ? C6 C1 C2 C3 -1.2(7) . . . . ? C6 C1 O1 P1 72.6(5) . . . . ? C6 C7 C8 C9 179.6(4) . . . . ? C6 C7 C12 C11 -177.3(4) . . . . ? C6 C7 C12 O2 -2.7(6) . . . . ? C7 C8 C9 C10 -3.0(7) . . . . ? C7 C12 O2 P1 69.6(5) . . . . ? C8 C7 C12 C11 1.9(6) . . . . ? C8 C7 C12 O2 176.5(4) . . . . ? C8 C9 C10 C11 3.4(8) . . . . ? C9 C10 C11 C12 -1.1(7) . . . . ? C10 C11 C12 C7 -1.6(7) . . . . ? C10 C11 C12 O2 -176.4(4) . . . . ? C11 C12 O2 P1 -115.6(4) . . . . ? C12 C7 C8 C9 0.3(6) . . . . ? C12 O2 P1 N1 70.9(4) . . . . ? C12 O2 P1 N3 -159.8(3) . . . . ? C12 O2 P1 O1 -42.2(3) . . . . ? C13 C14 N4 Ag1 -175.5(3) . . . . ? C13 C14 N4 C15 0.3(6) . . . . ? C13 O3 P2 N1 153.3(3) . . . . ? C13 O3 P2 N2 23.0(3) . . . . ? C13 O3 P2 O4 -89.5(3) . . . . ? C14 C13 C17 C16 0.3(6) . . . . ? C14 C13 O3 P2 40.7(5) . . . . ? C15 C16 C17 C13 -0.1(7) . . . . ? C16 C15 N4 Ag1 175.9(4) . . . . ? C16 C15 N4 C14 -0.1(6) . . . . ? C17 C13 C14 N4 -0.4(6) . . . . ? C17 C13 O3 P2 -141.1(3) . . . . ? C18 C29 N7 Ag2 -179.4(3) 7_565 . . . ? C18 C29 N7 C30 1.7(6) 7_565 . . . ? C18 O4 P2 N1 -74.4(3) . . . . ? C18 O4 P2 N2 57.6(3) . . . . ? C18 O4 P2 O3 173.2(3) . . . . ? C19 C28 C32 C21 -2.3(6) 7_565 . . 7_565 ? C19 C28 O5 P3 102.7(4) 7_565 . . . ? C21 C20 N5 Ag1 -164.6(4) . . . . ? C21 C20 N5 C19 0.3(6) . . . . ? C22 C18 O4 P2 57.9(4) . . . . ? C23 C24 N6 Ag2 177.0(3) . . . . ? C23 C24 N6 C25 0.7(6) . . . . ? C23 O6 P3 N2 -38.1(3) . . . . ? C23 O6 P3 N3 -168.1(3) . . . . ? C23 O6 P3 O5 76.1(3) . . . . ? C24 C23 C27 C26 -1.1(6) . . . . ? C24 C23 O6 P3 -22.3(5) . . . . ? C25 C26 C27 C23 0.1(7) . . . . ? C26 C25 N6 Ag2 -178.1(4) . . . . ? C26 C25 N6 C24 -1.8(7) . . . . ? C27 C23 C24 N6 0.8(6) . . . . ? C27 C23 O6 P3 159.2(3) . . . . ? C28 C19 N5 Ag1 164.3(3) 7_565 . . . ? C28 C19 N5 C20 -0.8(6) 7_565 . . . ? C28 O5 P3 N2 -67.4(3) . . . . ? C28 O5 P3 N3 64.0(3) . . . . ? C28 O5 P3 O6 177.3(3) . . . . ? C29 C18 C22 C31 0.1(6) 7_565 . . 7_565 ? C29 C18 O4 P2 -123.8(3) 7_565 . . . ? C31 C30 N7 Ag2 -178.9(3) . . . . ? C31 C30 N7 C29 0.0(6) . . . . ? C32 C28 O5 P3 -82.4(4) . . . . ? N4 Ag1 Ag2 N6 0.16(12) . . . . ? N4 Ag1 Ag2 N7 177.96(13) . . . . ? N4 Ag1 N5 C19 -89.7(8) . . . . ? N4 Ag1 N5 C20 75.0(8) . . . . ? N4 C15 C16 C17 0.0(7) . . . . ? N5 Ag1 Ag2 N6 179.75(12) . . . . ? N5 Ag1 Ag2 N7 -2.44(13) . . . . ? N5 Ag1 N4 C14 85.3(8) . . . . ? N5 Ag1 N4 C15 -90.5(8) . . . . ? N5 C20 C21 C32 1.4(7) . . . 7_565 ? N6 Ag2 N7 C29 54.6(15) . . . . ? N6 Ag2 N7 C30 -126.5(14) . . . . ? N6 C25 C26 C27 1.4(7) . . . . ? N7 Ag2 N6 C24 -72.5(15) . . . . ? N7 Ag2 N6 C25 103.8(14) . . . . ? N7 C30 C31 C22 -1.8(7) . . . 7_565 ? O1 C1 C2 C3 -174.3(4) . . . . ? O1 C1 C6 C5 173.7(4) . . . . ? O1 C1 C6 C7 -4.4(6) . . . . ? O3 C13 C14 N4 177.7(3) . . . . ? O3 C13 C17 C16 -177.9(4) . . . . ? O4 C18 C22 C31 178.3(4) . . . 7_565 ? O5 C28 C32 C21 -176.9(4) . . . 7_565 ? O6 C23 C24 N6 -177.7(3) . . . . ? O6 C23 C27 C26 177.4(4) . . . . ? P1 N1 P2 N2 0.2(3) . . . . ? P1 N1 P2 O3 -126.2(2) . . . . ? P1 N1 P2 O4 126.7(2) . . . . ? P1 N3 P3 N2 -14.6(3) . . . . ? P1 N3 P3 O5 -140.9(2) . . . . ? P1 N3 P3 O6 110.9(2) . . . . ? P2 N1 P1 N3 5.1(3) . . . . ? P2 N1 P1 O1 -119.9(2) . . . . ? P2 N1 P1 O2 127.4(2) . . . . ? P2 N2 P3 N3 20.1(3) . . . . ? P2 N2 P3 O5 147.5(2) . . . . ? P2 N2 P3 O6 -104.2(2) . . . . ? P3 N2 P2 N1 -13.0(3) . . . . ? P3 N2 P2 O3 111.3(2) . . . . ? P3 N2 P2 O4 -142.1(2) . . . . ? P3 N3 P1 N1 2.3(3) . . . . ? P3 N3 P1 O1 123.6(2) . . . . ? P3 N3 P1 O2 -124.3(2) . . . . ? N8 O7 O8A O8B -4.1(8) . . . . ? O7 N8 O7 O8A -8.8(4) 7_565 . . . ? O7 N8 O8A O7 180.0 7_565 . . . ? O7 N8 O8A O8B -4.3(8) 7_565 . . . ? O7 N8 O8A O8B 175.7(8) . . . . ? O7 N8 O8B O8A 175.4(9) 7_565 . . . ? O7 N8 O8B O8A -4.6(9) . . . . ? O7 O8A O8B N8 4.1(8) . . . . ? O8A N8 O7 O8A 180.0 7_565 . . . ? O8A N8 O8A O7 -60.4(9) 7_565 . . . ? O8A N8 O8A O8B 115.3(14) 7_565 . . . ? O8A N8 O8B O8A -180.0 7_565 . . . ? O8B N8 O7 O8A 3.6(7) . . . . ? O8B N8 O7 O8A -176.4(7) 7_565 . . . ? O8B N8 O8A O7 -175.7(8) . . . . ? O8B N8 O8A O7 4.3(8) 7_565 . . . ? O8B N8 O8A O8B 180.0 7_565 . . . ? O8B N8 O8B O8A 179.5(6) 7_565 . . . ? C34 C37 N10 C36 -148(3) . . . . ? C34 C37 N10 O15 25(13) . . . . ? C34 C37 N10 O16 -162(3) . . . . ? C34 C37 N10 O14 20.8(16) . . . . ? C34 O15 N10 C37 -155(13) . . . . ? C34 O15 N10 C36 -147(4) . . . . ? C34 O15 N10 O16 -164(3) . . . . ? C34 O15 N10 O14 21.1(12) . . . . ? C34 O14 N10 C37 -43(4) . . . . ? C34 O14 N10 C36 125(4) . . . . ? C34 O14 N10 O15 -44(3) . . . . ? C34 O14 N10 O16 140(3) . . . . ? O18 C37 N10 C34 165.9(12) . . . . ? O18 C37 N10 C36 18(3) . . . . ? O18 C37 N10 O15 -169(13) . . . . ? O18 C37 N10 O16 4(3) . . . . ? O18 C37 N10 O14 -173.3(12) . . . . ? O18 C36 N10 C34 -153.5(15) . . . . ? O18 C36 N10 C37 -21(4) . . . . ? O18 C36 N10 O15 -24(5) . . . . ? O18 C36 N10 O16 76(6) . . . . ? O18 C36 N10 O14 169.7(12) . . . . ? O18 O16 N10 C34 -154.7(19) . . . . ? O18 O16 N10 C37 -5(3) . . . . ? O18 O16 N10 C36 -93(8) . . . . ? O18 O16 N10 O15 -2(3) . . . . ? O18 O16 N10 O14 172.5(11) . . . . ? C37 C34 O15 N10 30(14) . . . . ? C37 C34 O14 N10 23.8(17) . . . . ? C37 C34 N10 C36 136(4) . . . . ? C37 C34 N10 O15 -7(4) . . . . ? C37 C34 N10 O16 152(4) . . . . ? C37 C34 N10 O14 -145(3) . . . . ? C37 O18 C36 N10 14(3) . . . . ? C37 O18 O16 N10 3(2) . . . . ? C36 O18 C37 C34 -4(3) . . . . ? C36 O18 C37 N10 -14(3) . . . . ? C36 O18 O16 N10 73(4) . . . . ? O15 C34 C37 O18 -160(17) . . . . ? O15 C34 C37 N10 -145(17) . . . . ? O15 C34 O14 N10 33.5(15) . . . . ? O15 C34 N10 C37 7(4) . . . . ? O15 C34 N10 C36 143(4) . . . . ? O15 C34 N10 O16 159(3) . . . . ? O15 C34 N10 O14 -138(3) . . . . ? O16 O18 C37 C34 6(3) . . . . ? O16 O18 C37 N10 -3(2) . . . . ? O16 O18 C36 N10 -94(7) . . . . ? O14 C34 C37 O18 -51(4) . . . . ? O14 C34 C37 N10 -36(3) . . . . ? O14 C34 O15 N10 -45(2) . . . . ? O14 C34 N10 C37 145(3) . . . . ? O14 C34 N10 C36 -79(4) . . . . ? O14 C34 N10 O15 138(3) . . . . ? O14 C34 N10 O16 -63(4) . . . . ? N10 C34 C37 O18 -14.8(13) . . . . ? data_908592 _database_code_depnum_ccdc_archive 'CCDC 908592' #TrackingRef '17692_web_deposit_cif_file_3_RSuriyaNarayanan_1360734625.908592.cif' _vrf_PLAT601_908592 ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 217.00 A**3 RESPONSE: Disordered water molecules were omitted by using PLATON/SQUEEZE ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H24 Cl4 N7 O6 P3 Zn2' _chemical_formula_sum 'C32 H24 Cl4 N7 O6 P3 Zn2' _chemical_formula_weight 968.03 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' Zn Zn 0.2839 1.4301 '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 _symmetry_space_group_name_Hall '-C 2yc' 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 22.167(4) _cell_length_b 14.195(3) _cell_length_c 15.405(3) _cell_angle_alpha 90.00 _cell_angle_beta 122.04(3) _cell_angle_gamma 90.00 _cell_volume 4108.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4688 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 28.28 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 1.594 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.614 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 4033 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11241 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_unetI/netI 0.0410 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4033 _reflns_number_gt 3439 _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^)+(0.0570P)^2^+1.8087P] 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 4003 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.1009 _refine_ls_wR_factor_gt 0.0956 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 Zn1 Zn 0.243079(15) -0.000771(19) 0.35348(2) 0.01830(12) Uani 1 1 d . . . Cl1 Cl 0.19337(4) 0.01270(4) 0.18594(5) 0.02512(17) Uani 1 1 d . . . Cl2 Cl 0.18383(4) -0.01853(5) 0.43141(6) 0.03038(18) Uani 1 1 d . . . P1 P 0.5000 -0.02843(6) 0.2500 0.0153(2) Uani 1 2 d S . . P2 P 0.48111(3) -0.19715(4) 0.32211(5) 0.01518(16) Uani 1 1 d . . . N1 N 0.5000 -0.2507(2) 0.2500 0.0170(6) Uani 1 2 d S . . N2 N 0.48168(10) -0.08606(14) 0.32098(15) 0.0166(4) Uani 1 1 d . . . O1 O 0.56253(8) 0.04002(12) 0.32525(12) 0.0176(4) Uani 1 1 d . . . O2 O 0.40667(8) -0.23629(12) 0.29717(13) 0.0175(4) Uani 1 1 d . . . O3 O 0.52850(8) -0.23423(12) 0.43687(13) 0.0180(4) Uani 1 1 d . . . C1 C 0.57988(13) 0.11888(17) 0.28698(18) 0.0189(5) Uani 1 1 d . . . C2 C 0.53404(13) 0.19552(17) 0.25161(19) 0.0213(5) Uani 1 1 d . . . C3 C 0.55598(16) 0.27474(19) 0.2220(2) 0.0285(6) Uani 1 1 d . . . H3 H 0.5266 0.3274 0.1971 0.034 Uiso 1 1 calc R . . C4 C 0.62094(17) 0.2763(2) 0.2289(2) 0.0347(7) Uani 1 1 d . . . H4 H 0.6345 0.3296 0.2082 0.042 Uiso 1 1 calc R . . C5 C 0.66572(15) 0.1992(2) 0.2665(2) 0.0312(7) Uani 1 1 d . . . H5 H 0.7097 0.2012 0.2725 0.037 Uiso 1 1 calc R . . C6 C 0.64507(14) 0.11852(19) 0.29541(19) 0.0235(6) Uani 1 1 d . . . H6 H 0.6744 0.0658 0.3198 0.028 Uiso 1 1 calc R . . C7 C 0.38023(12) -0.21506(17) 0.36023(18) 0.0171(5) Uani 1 1 d . . . C8 C 0.34148(12) -0.13364(17) 0.34107(18) 0.0181(5) Uani 1 1 d . . . H8 H 0.3364 -0.0921 0.2909 0.022 Uiso 1 1 calc R . . C9 C 0.31796(13) -0.17456(18) 0.46544(19) 0.0208(5) Uani 1 1 d . . . H9 H 0.2959 -0.1613 0.5013 0.025 Uiso 1 1 calc R . . C10 C 0.35680(13) -0.25659(19) 0.4877(2) 0.0223(6) Uani 1 1 d . . . H10 H 0.3614 -0.2970 0.5384 0.027 Uiso 1 1 calc R . . C11 C 0.38881(13) -0.27822(18) 0.4339(2) 0.0210(5) Uani 1 1 d . . . H11 H 0.4151 -0.3332 0.4469 0.025 Uiso 1 1 calc R . . N3 N 0.31066(10) -0.11353(14) 0.39474(15) 0.0178(4) Uani 1 1 d . . . C12B C 0.60229(12) -0.22284(17) 0.49251(18) 0.0171(5) Uani 1 1 d . . . C13B C 0.36795(12) 0.13504(16) 0.47161(17) 0.0160(5) Uani 1 1 d . . . H13B H 0.3974 0.0829 0.4874 0.019 Uiso 1 1 calc R . . C14B C 0.25563(13) 0.20073(18) 0.39111(19) 0.0203(5) Uani 1 1 d . . . H14B H 0.2065 0.1932 0.3511 0.024 Uiso 1 1 calc R . . C15B C 0.28269(14) 0.28992(18) 0.4240(2) 0.0228(6) Uani 1 1 d . . . H15B H 0.2524 0.3413 0.4063 0.027 Uiso 1 1 calc R . . C16B C 0.35598(13) 0.30189(18) 0.48400(19) 0.0203(5) Uani 1 1 d . . . H16B H 0.3761 0.3611 0.5074 0.024 Uiso 1 1 calc R . . N4 N 0.29708(10) 0.12399(14) 0.41421(15) 0.0174(4) 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 Zn1 0.01797(18) 0.01813(19) 0.0188(2) -0.00192(11) 0.00976(15) -0.00008(11) Cl1 0.0265(4) 0.0242(3) 0.0178(3) -0.0002(2) 0.0071(3) 0.0016(2) Cl2 0.0386(4) 0.0247(4) 0.0438(4) -0.0032(3) 0.0326(4) -0.0010(3) P1 0.0155(4) 0.0120(4) 0.0163(4) 0.000 0.0070(4) 0.000 P2 0.0152(3) 0.0130(3) 0.0172(3) -0.0002(2) 0.0085(3) -0.0008(2) N1 0.0174(14) 0.0137(14) 0.0216(15) 0.000 0.0116(13) 0.000 N2 0.0179(10) 0.0129(10) 0.0186(10) -0.0007(8) 0.0094(9) -0.0005(8) O1 0.0180(9) 0.0137(8) 0.0183(9) -0.0015(7) 0.0078(8) -0.0027(7) O2 0.0162(8) 0.0178(9) 0.0198(9) -0.0044(7) 0.0103(7) -0.0028(7) O3 0.0153(8) 0.0190(9) 0.0178(9) 0.0029(7) 0.0075(7) -0.0006(7) C1 0.0249(13) 0.0154(12) 0.0164(12) -0.0050(10) 0.0110(11) -0.0061(10) C2 0.0271(14) 0.0188(13) 0.0161(12) -0.0041(10) 0.0102(11) -0.0040(10) C3 0.0396(16) 0.0174(14) 0.0259(14) -0.0021(11) 0.0156(13) -0.0083(12) C4 0.0544(19) 0.0268(16) 0.0283(15) -0.0059(12) 0.0256(15) -0.0209(14) C5 0.0313(15) 0.0412(18) 0.0270(15) -0.0147(13) 0.0195(13) -0.0189(13) C6 0.0249(13) 0.0244(14) 0.0223(13) -0.0114(11) 0.0132(12) -0.0066(11) C7 0.0139(11) 0.0189(13) 0.0174(12) -0.0044(10) 0.0076(10) -0.0045(9) C8 0.0186(12) 0.0193(13) 0.0176(12) 0.0024(10) 0.0105(10) -0.0009(9) C9 0.0223(13) 0.0245(14) 0.0176(12) -0.0024(10) 0.0120(11) -0.0035(10) C10 0.0238(13) 0.0227(14) 0.0197(13) 0.0036(10) 0.0111(11) -0.0020(10) C11 0.0185(12) 0.0175(13) 0.0249(13) -0.0008(10) 0.0101(11) -0.0006(10) N3 0.0182(10) 0.0181(11) 0.0168(10) -0.0005(8) 0.0090(9) 0.0000(8) C12B 0.0180(12) 0.0192(13) 0.0145(11) 0.0007(10) 0.0088(10) -0.0017(9) C13B 0.0192(12) 0.0143(12) 0.0153(11) 0.0021(9) 0.0097(10) 0.0029(9) C14B 0.0186(13) 0.0231(14) 0.0183(13) 0.0002(10) 0.0092(11) 0.0027(10) C15B 0.0255(13) 0.0193(13) 0.0234(13) 0.0042(10) 0.0127(12) 0.0072(10) C16B 0.0256(13) 0.0153(13) 0.0209(13) 0.0001(10) 0.0130(11) -0.0006(10) N4 0.0179(10) 0.0183(11) 0.0142(10) -0.0005(8) 0.0072(9) -0.0006(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 Zn1 N3 2.049(2) . ? Zn1 N4 2.063(2) . ? Zn1 Cl1 2.2123(10) . ? Zn1 Cl2 2.2141(8) . ? P1 N2 1.581(2) 2_655 ? P1 N2 1.581(2) . ? P1 O1 1.5825(17) . ? P1 O1 1.5826(17) 2_655 ? P2 N1 1.5751(15) . ? P2 N2 1.577(2) . ? P2 O2 1.5833(17) . ? P2 O3 1.5924(18) . ? N1 P2 1.5751(15) 2_655 ? O1 C1 1.410(3) . ? O2 C7 1.408(3) . ? O3 C12B 1.396(3) . ? C1 C6 1.381(3) . ? C1 C2 1.388(4) . ? C2 C3 1.395(4) . ? C2 C2 1.484(5) 2_655 ? C3 C4 1.386(4) . ? C3 H3 0.9300 . ? C4 C5 1.382(4) . ? C4 H4 0.9300 . ? C5 C6 1.391(4) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.375(3) . ? C7 C11 1.378(3) . ? C8 N3 1.353(3) . ? C8 H8 0.9300 . ? C9 N3 1.333(3) . ? C9 C10 1.379(4) . ? C9 H9 0.9300 . ? C10 C11 1.381(4) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12B C16B 1.375(3) 5_656 ? C12B C13B 1.381(3) 5_656 ? C13B N4 1.342(3) . ? C13B C12B 1.381(3) 5_656 ? C13B H13B 0.9300 . ? C14B N4 1.346(3) . ? C14B C15B 1.377(4) . ? C14B H14B 0.9300 . ? C15B C16B 1.389(4) . ? C15B H15B 0.9300 . ? C16B C12B 1.375(3) 5_656 ? C16B H16B 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Zn1 N4 112.15(8) . . ? N3 Zn1 Cl1 105.01(6) . . ? N4 Zn1 Cl1 105.36(6) . . ? N3 Zn1 Cl2 106.81(6) . . ? N4 Zn1 Cl2 102.72(6) . . ? Cl1 Zn1 Cl2 124.81(4) . . ? N2 P1 N2 117.70(15) 2_655 . ? N2 P1 O1 112.19(9) 2_655 . ? N2 P1 O1 104.93(9) . . ? N2 P1 O1 104.93(9) 2_655 2_655 ? N2 P1 O1 112.18(9) . 2_655 ? O1 P1 O1 104.24(13) . 2_655 ? N1 P2 N2 117.93(12) . . ? N1 P2 O2 107.00(9) . . ? N2 P2 O2 111.19(10) . . ? N1 P2 O3 110.97(9) . . ? N2 P2 O3 109.77(10) . . ? O2 P2 O3 98.17(9) . . ? P2 N1 P2 122.26(18) 2_655 . ? P2 N2 P1 122.09(13) . . ? C1 O1 P1 120.55(15) . . ? C7 O2 P2 121.29(15) . . ? C12B O3 P2 120.75(15) . . ? C6 C1 C2 123.5(2) . . ? C6 C1 O1 117.5(2) . . ? C2 C1 O1 118.8(2) . . ? C1 C2 C3 116.8(2) . . ? C1 C2 C2 122.22(17) . 2_655 ? C3 C2 C2 120.96(18) . 2_655 ? C4 C3 C2 121.1(3) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C5 C4 C3 120.4(3) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 120.1(3) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C1 C6 C5 118.2(3) . . ? C1 C6 H6 120.9 . . ? C5 C6 H6 120.9 . . ? C8 C7 C11 121.4(2) . . ? C8 C7 O2 118.2(2) . . ? C11 C7 O2 120.2(2) . . ? N3 C8 C7 120.4(2) . . ? N3 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? N3 C9 C10 122.7(2) . . ? N3 C9 H9 118.6 . . ? C10 C9 H9 118.6 . . ? C9 C10 C11 119.4(2) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C7 C11 C10 117.3(2) . . ? C7 C11 H11 121.3 . . ? C10 C11 H11 121.3 . . ? C9 N3 C8 118.7(2) . . ? C9 N3 Zn1 120.87(16) . . ? C8 N3 Zn1 119.88(16) . . ? C16B C12B C13B 121.3(2) 5_656 5_656 ? C16B C12B O3 118.2(2) 5_656 . ? C13B C12B O3 120.4(2) 5_656 . ? N4 C13B C12B 120.9(2) . 5_656 ? N4 C13B H13B 119.6 . . ? C12B C13B H13B 119.6 5_656 . ? N4 C14B C15B 122.9(2) . . ? N4 C14B H14B 118.5 . . ? C15B C14B H14B 118.5 . . ? C14B C15B C16B 119.0(2) . . ? C14B C15B H15B 120.5 . . ? C16B C15B H15B 120.5 . . ? C12B C16B C15B 117.5(2) 5_656 . ? C12B C16B H16B 121.3 5_656 . ? C15B C16B H16B 121.3 . . ? C13B N4 C14B 118.4(2) . . ? C13B N4 Zn1 126.44(16) . . ? C14B N4 Zn1 115.12(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 P2 N1 P2 -0.17(8) . . . 2_655 ? O2 P2 N1 P2 125.98(8) . . . 2_655 ? O3 P2 N1 P2 -127.98(8) . . . 2_655 ? N1 P2 N2 P1 0.35(17) . . . . ? O2 P2 N2 P1 -123.73(13) . . . . ? O3 P2 N2 P1 128.73(13) . . . . ? N2 P1 N2 P2 -0.18(9) 2_655 . . . ? O1 P1 N2 P2 -125.73(14) . . . . ? O1 P1 N2 P2 121.72(14) 2_655 . . . ? N2 P1 O1 C1 68.10(19) 2_655 . . . ? N2 P1 O1 C1 -162.97(17) . . . . ? O1 P1 O1 C1 -44.88(14) 2_655 . . . ? N1 P2 O2 C7 168.86(17) . . . . ? N2 P2 O2 C7 -61.1(2) . . . . ? O3 P2 O2 C7 53.91(18) . . . . ? N1 P2 O3 C12B 63.56(19) . . . . ? N2 P2 O3 C12B -68.57(19) . . . . ? O2 P2 O3 C12B 175.35(17) . . . . ? P1 O1 C1 C6 -113.0(2) . . . . ? P1 O1 C1 C2 72.6(3) . . . . ? C6 C1 C2 C3 1.1(4) . . . . ? O1 C1 C2 C3 175.1(2) . . . . ? C6 C1 C2 C2 -176.8(3) . . . 2_655 ? O1 C1 C2 C2 -2.8(4) . . . 2_655 ? C1 C2 C3 C4 -0.7(4) . . . . ? C2 C2 C3 C4 177.3(3) 2_655 . . . ? C2 C3 C4 C5 -0.6(4) . . . . ? C3 C4 C5 C6 1.5(4) . . . . ? C2 C1 C6 C5 -0.3(4) . . . . ? O1 C1 C6 C5 -174.3(2) . . . . ? C4 C5 C6 C1 -1.1(4) . . . . ? P2 O2 C7 C8 87.2(2) . . . . ? P2 O2 C7 C11 -97.5(2) . . . . ? C11 C7 C8 N3 0.0(4) . . . . ? O2 C7 C8 N3 175.3(2) . . . . ? N3 C9 C10 C11 -1.1(4) . . . . ? C8 C7 C11 C10 0.1(4) . . . . ? O2 C7 C11 C10 -175.0(2) . . . . ? C9 C10 C11 C7 0.4(4) . . . . ? C10 C9 N3 C8 1.3(4) . . . . ? C10 C9 N3 Zn1 172.88(19) . . . . ? C7 C8 N3 C9 -0.7(3) . . . . ? C7 C8 N3 Zn1 -172.41(17) . . . . ? N4 Zn1 N3 C9 104.89(19) . . . . ? Cl1 Zn1 N3 C9 -141.20(18) . . . . ? Cl2 Zn1 N3 C9 -6.9(2) . . . . ? N4 Zn1 N3 C8 -83.62(19) . . . . ? Cl1 Zn1 N3 C8 30.29(18) . . . . ? Cl2 Zn1 N3 C8 164.58(16) . . . . ? P2 O3 C12B C16B -111.3(2) . . . 5_656 ? P2 O3 C12B C13B 72.8(3) . . . 5_656 ? N4 C14B C15B C16B -0.2(4) . . . . ? C14B C15B C16B C12B -0.2(4) . . . 5_656 ? C12B C13B N4 C14B 1.0(3) 5_656 . . . ? C12B C13B N4 Zn1 179.73(17) 5_656 . . . ? C15B C14B N4 C13B -0.2(4) . . . . ? C15B C14B N4 Zn1 -179.12(19) . . . . ? N3 Zn1 N4 C13B 2.1(2) . . . . ? Cl1 Zn1 N4 C13B -111.61(18) . . . . ? Cl2 Zn1 N4 C13B 116.41(18) . . . . ? N3 Zn1 N4 C14B -179.13(16) . . . . ? Cl1 Zn1 N4 C14B 67.18(17) . . . . ? Cl2 Zn1 N4 C14B -64.80(17) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.018 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.085 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 34 3 ' ' 2 0.500 -0.043 0.250 45 11 ' ' 3 0.000 0.000 0.500 34 3 ' ' 4 0.500 0.042 0.750 45 11 ' ' 5 0.500 0.500 0.000 34 3 ' ' 6 0.500 0.500 0.500 34 3 ' ' 7 0.000 0.457 0.250 45 11 ' ' 8 1.000 0.542 0.750 45 11 ' ' _platon_squeeze_details ; ; data_908593 _database_code_depnum_ccdc_archive 'CCDC 908593' #TrackingRef '17693_web_deposit_cif_file_4_RSuriyaNarayanan_1360734625.908593.cif' _vrf_PLAT601_908593 ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 717.00 A**3 RESPONSE: Disordered water and methanol molecules were omitted by using OLEX-2/Mask ; _audit_creation_date 2013-02-11 _audit_creation_method ; Olex2 1.2 (compiled Dec 5 2012 16:20:19, GUI svn.r4385) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C68 H65 Cd3 N20 O35 P6' _chemical_formula_sum 'C68 H65 Cd3 N20 O35 P6' _chemical_formula_weight 2245.42 _chemical_melting_point ? 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z+1/2' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x, -y, z-1/2' 7 '-x+1/2, -y+1/2, -z' 8 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.787(3) _cell_length_b 11.9727(12) _cell_length_c 29.607(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.856(3) _cell_angle_gamma 90.00 _cell_volume 9814.4(18) _cell_formula_units_Z 4 _cell_measurement_reflns_used 5300 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.33 _cell_measurement_theta_min 2.27 _exptl_absorpt_coefficient_mu 0.829 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.644612 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS v.2.10 (Bruker,2003) was used for absorption correction. R(int) was 0.0668 before and 0.0345 after correction. The Ratio of minimum to maximum transmission is 0.6446. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 4508 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_unetI/netI 0.0854 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_number 32500 _diffrn_reflns_theta_full 28.37 _diffrn_reflns_theta_max 28.37 _diffrn_reflns_theta_min 2.00 _diffrn_ambient_temperature 100.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 8123 _reflns_number_total 12185 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'SAINT v6.45A (Bruker, 2003)' _computing_data_collection ? _computing_data_reduction 'SAINT v6.45A (Bruker, 2003)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 1.940 _refine_diff_density_min -1.957 _refine_diff_density_rms 0.171 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 602 _refine_ls_number_reflns 12185 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1105 _refine_ls_R_factor_gt 0.0739 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0990P)^2^+60.6492P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1908 _refine_ls_wR_factor_ref 0.2243 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: H17 of C17, H16 of C16, H19 of C19, H20 of C20, H25 of C25, H27 of C27, H24 of C24, H26 of C26, H21 of C21, H11 of C11, H14 of C14, H15 of C15, H22 of C22, H4 of C4, H2 of C2, H5 of C5, H8 of C8, H3 of C3, H9 of C9, H10 of C10, H15A of P3, H32 of C32, H31 of C31, H30 of C30, H29 of C29 At 1.5 times of: H7 of O7, H11A of P3, {H36A,H36B,H36C} of C36, {H35A,H35B,H35C} of C35 2. Restrained distances O11-H11A 0.83 with sigma of 0.02 O15-H15A 0.83 with sigma of 0.02 H15A-O15 0.83 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(O18) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 4. Others Fixed Sof: H7(0.5) 5.a Me refined with riding coordinates: C35(H35A,H35B,H35C), C36(H36A,H36B,H36C) 5.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32) 5.c Tetrahedral OH refined with riding coordinates: O7(H7) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3569(2) 0.7469(5) 0.3299(2) 0.0295(12) Uani 1 1 d . . . C2 C 0.4012(2) 0.7937(5) 0.3270(2) 0.0352(14) Uani 1 1 d . . . H2 H 0.4198 0.7774 0.3023 0.042 Uiso 1 1 calc R . . C3 C 0.4186(3) 0.8672(5) 0.3618(3) 0.0435(17) Uani 1 1 d . . . H3 H 0.4495 0.9005 0.3609 0.052 Uiso 1 1 calc R . . C4 C 0.3911(3) 0.8909(6) 0.3968(3) 0.051(2) Uani 1 1 d . . . H4 H 0.4033 0.9397 0.4203 0.062 Uiso 1 1 calc R . . C5 C 0.3452(3) 0.8438(5) 0.3982(2) 0.0422(17) Uani 1 1 d . . . H5 H 0.3262 0.8630 0.4222 0.051 Uiso 1 1 calc R . . C6 C 0.3270(2) 0.7697(5) 0.3651(2) 0.0328(13) Uani 1 1 d . . . C7 C 0.2795(2) 0.7183(5) 0.3660(2) 0.0345(14) Uani 1 1 d . . . C8 C 0.2621(3) 0.6817(6) 0.4070(2) 0.0427(16) Uani 1 1 d . . . H8 H 0.2826 0.6884 0.4342 0.051 Uiso 1 1 calc R . . C9 C 0.2162(3) 0.6360(6) 0.4091(3) 0.0484(19) Uani 1 1 d . . . H9 H 0.2060 0.6107 0.4372 0.058 Uiso 1 1 calc R . . C10 C 0.1857(3) 0.6281(6) 0.3699(3) 0.0449(17) Uani 1 1 d . . . H10 H 0.1542 0.5979 0.3709 0.054 Uiso 1 1 calc R . . C11 C 0.2012(2) 0.6643(5) 0.3292(2) 0.0363(14) Uani 1 1 d . . . H11 H 0.1803 0.6592 0.3022 0.044 Uiso 1 1 calc R . . C12 C 0.2468(2) 0.7075(5) 0.3278(2) 0.0307(13) Uani 1 1 d . . . C13 C 0.1876(2) 0.5553(5) 0.1748(2) 0.0286(12) Uani 1 1 d . . . C14 C 0.1638(2) 0.5434(6) 0.2140(2) 0.0351(14) Uani 1 1 d . . . H14 H 0.1779 0.4969 0.2375 0.042 Uiso 1 1 calc R . . C15 C 0.1034(3) 0.6582(6) 0.1849(4) 0.064(3) Uani 1 1 d . . . H15 H 0.0741 0.6968 0.1886 0.077 Uiso 1 1 calc R . . C16 C 0.1239(3) 0.6707(6) 0.1447(3) 0.053(2) Uani 1 1 d . . . H16 H 0.1084 0.7139 0.1208 0.064 Uiso 1 1 calc R . . C17 C 0.1678(2) 0.6189(5) 0.1398(2) 0.0367(14) Uani 1 1 d . . . H17 H 0.1836 0.6275 0.1128 0.044 Uiso 1 1 calc R . . C18 C 0.3554(2) 0.4210(5) 0.1691(2) 0.0264(11) Uani 1 1 d . . . C19 C 0.3929(2) 0.4231(4) 0.2019(2) 0.0256(11) Uani 1 1 d . . . H19 H 0.3860 0.4350 0.2324 0.031 Uiso 1 1 calc R . . C20 C 0.4471(2) 0.3937(5) 0.1491(2) 0.0379(15) Uani 1 1 d . . . H20 H 0.4794 0.3842 0.1418 0.046 Uiso 1 1 calc R . . C21 C 0.4114(3) 0.3910(6) 0.1147(2) 0.0447(17) Uani 1 1 d . . . H21 H 0.4191 0.3784 0.0845 0.054 Uiso 1 1 calc R . . C22 C 0.3641(2) 0.4066(6) 0.1237(2) 0.0354(14) Uani 1 1 d . . . H22 H 0.3386 0.4076 0.1002 0.042 Uiso 1 1 calc R . . C23 C 0.2528(2) 0.8723(5) 0.1341(2) 0.0276(12) Uani 1 1 d . . . C24 C 0.2695(2) 0.6393(5) -0.0912(2) 0.0335(13) Uani 1 1 d . . . H24 H 0.2516 0.6670 -0.0677 0.040 Uiso 1 1 calc R . . C25 C 0.3411(2) 0.5764(5) -0.1160(2) 0.0323(13) Uani 1 1 d . . . H25 H 0.3742 0.5584 -0.1095 0.039 Uiso 1 1 calc R . . C26 C 0.3204(2) 0.5644(5) -0.1601(2) 0.0319(13) Uani 1 1 d . . . H26 H 0.3391 0.5395 -0.1835 0.038 Uiso 1 1 calc R . . C27 C 0.2720(2) 0.5893(5) -0.16931(19) 0.0289(12) Uani 1 1 d . . . H27 H 0.2564 0.5804 -0.1989 0.035 Uiso 1 1 calc R . . C28 C 0.4001(2) 0.7190(5) 0.13126(18) 0.0274(12) Uani 1 1 d . . . C29 C 0.3756(2) 0.7027(5) 0.08874(19) 0.0304(13) Uani 1 1 d . . . H29 H 0.3419 0.7172 0.0845 0.037 Uiso 1 1 calc R . . C30 C 0.4467(3) 0.6477(7) 0.0601(2) 0.0484(19) Uani 1 1 d . . . H30 H 0.4633 0.6235 0.0352 0.058 Uiso 1 1 calc R . . C31 C 0.4724(2) 0.6617(7) 0.1012(2) 0.0430(17) Uani 1 1 d . . . H31 H 0.5060 0.6453 0.1045 0.052 Uiso 1 1 calc R . . C32 C 0.4493(2) 0.6999(6) 0.1379(2) 0.0342(14) Uani 1 1 d . . . H32 H 0.4666 0.7126 0.1665 0.041 Uiso 1 1 calc R . . C35 C 0.3557(4) 0.9069(10) 0.0000(4) 0.093(4) Uani 1 1 d . . . H35A H 0.3356 0.9740 -0.0039 0.139 Uiso 1 1 calc R . . H35B H 0.3835 0.9138 -0.0181 0.139 Uiso 1 1 calc R . . H35C H 0.3671 0.8985 0.0321 0.139 Uiso 1 1 calc R . . C36 C 0.4013(5) 0.3622(10) -0.0310(5) 0.114(5) Uani 1 1 d . . . H36A H 0.4327 0.3286 -0.0353 0.171 Uiso 1 1 calc R . . H36B H 0.3791 0.3484 -0.0579 0.171 Uiso 1 1 calc R . . H36C H 0.3882 0.3290 -0.0044 0.171 Uiso 1 1 calc R . . Cd1 Cd 0.5000 0.41566(5) 0.2500 0.03096(17) Uani 1 2 d S . . Cd2 Cd 0.355498(17) 0.63027(5) -0.012824(15) 0.04298(17) Uani 1 1 d . . . N1 N 0.28274(17) 0.5737(4) 0.24023(17) 0.0290(10) Uani 1 1 d . . . N2 N 0.29877(17) 0.6355(4) 0.15547(16) 0.0258(10) Uani 1 1 d . . . N3 N 0.31498(17) 0.7823(4) 0.22454(16) 0.0277(10) Uani 1 1 d . . . N4 N 0.1226(2) 0.5933(5) 0.2201(2) 0.0489(15) Uani 1 1 d . . . N5 N 0.43925(19) 0.4092(4) 0.19326(18) 0.0313(11) Uani 1 1 d . . . N6 N 0.31569(19) 0.6126(4) -0.08209(17) 0.0327(11) Uani 1 1 d . . . N7 N 0.39936(18) 0.6664(5) 0.05342(18) 0.0374(13) Uani 1 1 d . . . N8 N 0.55363(17) 0.5128(4) 0.18308(17) 0.0303(11) Uani 1 1 d . . . N9 N 0.2750(3) 0.5280(6) 0.0289(2) 0.0564(17) Uani 1 1 d . . . N10 N 0.4633(4) 0.6801(9) -0.0599(3) 0.080(3) Uani 1 1 d . . . O1 O 0.34175(14) 0.6656(3) 0.29706(13) 0.0274(8) Uani 1 1 d . . . O2 O 0.25953(15) 0.7505(3) 0.28595(13) 0.0291(9) Uani 1 1 d . . . O3 O 0.22947(14) 0.4955(3) 0.17047(13) 0.0277(8) Uani 1 1 d . . . O4 O 0.30821(14) 0.4277(3) 0.18085(14) 0.0285(9) Uani 1 1 d . . . O5 O 0.30243(14) 0.8471(3) 0.14075(13) 0.0253(8) Uani 1 1 d . . . O6 O 0.37723(14) 0.7572(3) 0.16796(13) 0.0291(9) Uani 1 1 d . . . O7 O 0.5000 0.2246(5) 0.2500 0.0453(17) Uani 1 2 d S . . H7 H 0.4752 0.2012 0.2347 0.068 Uiso 0.50 1 calc PR . . O8 O 0.57020(16) 0.5495(4) 0.14906(16) 0.0385(10) Uani 1 1 d . . . O9 O 0.55920(15) 0.4108(4) 0.19405(16) 0.0368(10) Uani 1 1 d . . . O10 O 0.52967(16) 0.5734(4) 0.20795(16) 0.0375(10) Uani 1 1 d . . . O11 O 0.3294(2) 0.8163(5) -0.0138(2) 0.0602(15) Uani 1 1 d D . . O12 O 0.27084(19) 0.6308(5) 0.01812(17) 0.0502(13) Uani 1 1 d . . . O13 O 0.2431(3) 0.4796(6) 0.0457(3) 0.088(2) Uani 1 1 d . . . O14 O 0.3141(2) 0.4801(5) 0.02144(19) 0.0610(15) Uani 1 1 d . . . O15 O 0.4069(3) 0.4791(7) -0.0244(3) 0.083(2) Uani 1 1 d D . . O16 O 0.4230(2) 0.7156(6) -0.04840(18) 0.0606(16) Uani 1 1 d . . . O17 O 0.4814(3) 0.5862(7) -0.0517(3) 0.093(2) Uani 1 1 d . . . O18 O 0.4873(4) 0.7482(10) -0.0823(4) 0.148(4) Uani 1 1 d U . . P1 P 0.29950(5) 0.69142(12) 0.25942(5) 0.0250(3) Uani 1 1 d . . . P2 P 0.28102(5) 0.54195(12) 0.18796(5) 0.0235(3) Uani 1 1 d . . . P3 P 0.32109(5) 0.74950(12) 0.17398(5) 0.0237(3) Uani 1 1 d . . . H15A H 0.429(2) 0.521(5) -0.033(2) 0.028 Uiso 1 1 d D . . H11A H 0.3023(13) 0.842(6) -0.010(2) 0.036 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.036(3) 0.020(3) 0.031(3) 0.000(2) -0.008(2) 0.001(2) C2 0.034(3) 0.025(3) 0.043(4) 0.000(3) -0.015(3) 0.001(2) C3 0.036(4) 0.031(3) 0.061(5) -0.005(3) -0.012(3) -0.003(3) C4 0.065(5) 0.041(4) 0.043(4) -0.006(3) -0.021(4) -0.001(4) C5 0.065(5) 0.031(3) 0.029(3) -0.002(3) -0.006(3) 0.012(3) C6 0.048(4) 0.023(3) 0.027(3) 0.004(2) 0.000(3) 0.007(2) C7 0.046(4) 0.029(3) 0.029(3) -0.003(2) 0.007(3) 0.006(3) C8 0.060(5) 0.037(4) 0.031(3) 0.009(3) 0.005(3) 0.010(3) C9 0.065(5) 0.038(4) 0.047(4) 0.004(3) 0.032(4) 0.006(3) C10 0.055(4) 0.032(3) 0.051(4) 0.000(3) 0.027(4) -0.001(3) C11 0.031(3) 0.034(3) 0.045(4) -0.006(3) 0.009(3) 0.001(3) C12 0.044(4) 0.020(3) 0.030(3) 0.002(2) 0.012(3) 0.004(2) C13 0.018(3) 0.024(3) 0.042(3) 0.001(2) -0.006(2) -0.001(2) C14 0.027(3) 0.039(3) 0.040(4) 0.003(3) 0.005(3) 0.000(3) C15 0.036(4) 0.025(4) 0.131(9) -0.013(4) 0.005(5) -0.003(3) C16 0.041(4) 0.027(3) 0.088(6) 0.025(4) -0.018(4) -0.005(3) C17 0.028(3) 0.036(3) 0.045(4) 0.013(3) 0.001(3) -0.004(3) C18 0.023(3) 0.023(3) 0.033(3) 0.004(2) 0.005(2) 0.001(2) C19 0.025(3) 0.022(3) 0.031(3) -0.001(2) 0.004(2) 0.003(2) C20 0.023(3) 0.038(3) 0.053(4) -0.021(3) 0.006(3) -0.004(2) C21 0.053(4) 0.048(4) 0.034(4) -0.012(3) 0.012(3) -0.011(3) C22 0.031(3) 0.043(4) 0.031(3) -0.005(3) -0.003(3) 0.000(3) C23 0.029(3) 0.024(3) 0.029(3) 0.003(2) 0.001(2) 0.004(2) C24 0.038(3) 0.035(3) 0.028(3) -0.004(3) 0.010(3) 0.001(3) C25 0.033(3) 0.029(3) 0.035(3) 0.004(2) 0.004(3) 0.007(2) C26 0.038(3) 0.031(3) 0.027(3) -0.005(2) 0.001(2) -0.001(2) C27 0.033(3) 0.032(3) 0.022(3) 0.000(2) 0.002(2) 0.005(2) C28 0.029(3) 0.032(3) 0.019(3) 0.003(2) -0.007(2) 0.001(2) C29 0.026(3) 0.041(3) 0.024(3) 0.007(2) -0.003(2) 0.001(2) C30 0.038(4) 0.079(5) 0.029(3) -0.003(3) 0.009(3) 0.017(4) C31 0.028(3) 0.069(5) 0.031(3) 0.004(3) -0.002(3) 0.012(3) C32 0.028(3) 0.045(4) 0.027(3) 0.007(3) -0.010(2) -0.004(3) C35 0.077(8) 0.088(8) 0.113(9) 0.035(7) 0.010(7) -0.001(6) C36 0.101(10) 0.090(9) 0.154(13) -0.055(9) 0.030(9) 0.008(7) Cd1 0.0214(3) 0.0318(3) 0.0392(4) 0.000 -0.0007(2) 0.000 Cd2 0.0317(3) 0.0726(4) 0.0240(2) -0.0037(2) -0.00132(18) 0.0161(2) N1 0.026(2) 0.033(3) 0.028(3) 0.002(2) 0.0016(19) -0.002(2) N2 0.025(2) 0.029(2) 0.024(2) -0.0051(19) 0.0028(18) 0.0014(18) N3 0.028(2) 0.027(2) 0.027(3) 0.0009(19) -0.0012(19) 0.0000(19) N4 0.032(3) 0.047(4) 0.068(4) 0.004(3) 0.008(3) 0.001(3) N5 0.032(3) 0.021(2) 0.041(3) -0.002(2) 0.004(2) 0.005(2) N6 0.034(3) 0.036(3) 0.027(3) 0.000(2) -0.002(2) 0.004(2) N7 0.023(3) 0.059(4) 0.030(3) 0.001(2) 0.000(2) 0.010(2) N8 0.022(2) 0.033(3) 0.037(3) 0.001(2) 0.005(2) -0.0019(19) N9 0.052(4) 0.072(5) 0.044(4) 0.015(3) -0.003(3) 0.009(4) N10 0.079(6) 0.109(7) 0.053(5) -0.015(5) 0.004(4) 0.016(6) O1 0.031(2) 0.024(2) 0.026(2) -0.0026(16) -0.0042(16) 0.0037(16) O2 0.031(2) 0.032(2) 0.024(2) 0.0011(16) 0.0027(16) 0.0046(17) O3 0.0241(19) 0.026(2) 0.033(2) -0.0045(16) -0.0012(16) -0.0005(15) O4 0.0203(19) 0.024(2) 0.041(2) -0.0021(17) 0.0002(17) -0.0009(15) O5 0.027(2) 0.0207(18) 0.028(2) 0.0006(15) 0.0007(16) -0.0058(15) O6 0.028(2) 0.037(2) 0.022(2) -0.0006(17) -0.0020(16) -0.0007(17) O7 0.029(3) 0.034(3) 0.071(5) 0.000 -0.002(3) 0.000 O8 0.032(2) 0.043(3) 0.041(3) 0.003(2) 0.0055(19) 0.0003(19) O9 0.025(2) 0.034(2) 0.051(3) 0.003(2) 0.0037(19) 0.0080(18) O10 0.030(2) 0.040(3) 0.044(3) -0.003(2) 0.0088(19) 0.0027(18) O11 0.050(3) 0.053(3) 0.076(4) -0.001(3) -0.008(3) 0.012(3) O12 0.051(3) 0.063(3) 0.037(3) 0.015(2) 0.012(2) 0.014(3) O13 0.063(4) 0.094(5) 0.110(6) 0.048(5) 0.025(4) -0.002(4) O14 0.055(3) 0.075(4) 0.052(3) 0.012(3) -0.004(3) 0.022(3) O15 0.067(5) 0.091(6) 0.087(5) -0.027(4) -0.010(4) 0.028(4) O16 0.044(3) 0.099(5) 0.041(3) -0.006(3) 0.017(2) 0.001(3) O17 0.082(5) 0.104(6) 0.092(5) -0.014(5) -0.001(4) 0.047(5) O18 0.104(7) 0.178(9) 0.172(9) 0.052(8) 0.080(7) 0.047(7) P1 0.0262(7) 0.0257(7) 0.0228(7) -0.0001(6) 0.0005(5) 0.0012(5) P2 0.0212(7) 0.0223(7) 0.0263(7) -0.0011(5) -0.0014(5) 0.0002(5) P3 0.0250(7) 0.0246(7) 0.0209(7) 0.0011(5) -0.0015(5) -0.0015(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.362(9) . ? C1 C6 1.413(9) . ? C1 O1 1.414(7) . ? C2 H2 0.9500 . ? C2 C3 1.408(9) . ? C3 H3 0.9500 . ? C3 C4 1.367(11) . ? C4 H4 0.9500 . ? C4 C5 1.398(11) . ? C5 H5 0.9500 . ? C5 C6 1.384(9) . ? C6 C7 1.459(9) . ? C7 C8 1.413(9) . ? C7 C12 1.396(9) . ? C8 H8 0.9500 . ? C8 C9 1.395(11) . ? C9 H9 0.9500 . ? C9 C10 1.380(12) . ? C10 H10 0.9500 . ? C10 C11 1.385(10) . ? C11 H11 0.9500 . ? C11 C12 1.371(9) . ? C12 O2 1.414(7) . ? C13 C14 1.391(9) . ? C13 C17 1.364(8) . ? C13 O3 1.380(7) . ? C14 H14 0.9500 . ? C14 N4 1.317(8) . ? C15 H15 0.9500 . ? C15 C16 1.370(13) . ? C15 N4 1.372(12) . ? C16 H16 0.9500 . ? C16 C17 1.386(10) . ? C17 H17 0.9500 . ? C18 C19 1.363(8) . ? C18 C22 1.398(9) . ? C18 O4 1.388(7) . ? C19 H19 0.9500 . ? C19 N5 1.344(7) . ? C20 H20 0.9500 . ? C20 C21 1.361(10) . ? C20 N5 1.355(9) . ? C21 H21 0.9500 . ? C21 C22 1.374(10) . ? C22 H22 0.9500 . ? C23 C24 1.371(8) 7_565 ? C23 C27 1.376(8) 7_565 ? C23 O5 1.410(7) . ? C24 C23 1.371(8) 7_565 ? C24 H24 0.9500 . ? C24 N6 1.329(8) . ? C25 H25 0.9500 . ? C25 C26 1.390(9) . ? C25 N6 1.345(8) . ? C26 H26 0.9500 . ? C26 C27 1.381(8) . ? C27 C23 1.376(8) 7_565 ? C27 H27 0.9500 . ? C28 C29 1.393(8) . ? C28 C32 1.385(8) . ? C28 O6 1.382(7) . ? C29 H29 0.9500 . ? C29 N7 1.355(8) . ? C30 H30 0.9500 . ? C30 C31 1.368(10) . ? C30 N7 1.332(8) . ? C31 H31 0.9500 . ? C31 C32 1.386(10) . ? C32 H32 0.9500 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C35 O11 1.352(13) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C36 O15 1.421(14) . ? Cd1 N5 2.280(5) . ? Cd1 N5 2.280(5) 2_655 ? Cd1 O7 2.288(6) . ? Cd1 O9 2.432(5) 2_655 ? Cd1 O9 2.432(5) . ? Cd1 O10 2.444(5) . ? Cd1 O10 2.444(5) 2_655 ? Cd2 N6 2.256(5) . ? Cd2 N7 2.261(5) . ? Cd2 O11 2.342(6) . ? Cd2 O12 2.596(5) . ? Cd2 O14 2.405(6) . ? Cd2 O15 2.349(7) . ? Cd2 O16 2.450(6) . ? N1 P1 1.575(5) . ? N1 P2 1.590(5) . ? N2 P2 1.582(5) . ? N2 P3 1.578(5) . ? N3 P1 1.584(5) . ? N3 P3 1.571(5) . ? N8 O8 1.224(7) . ? N8 O9 1.269(6) . ? N8 O10 1.263(6) . ? N9 O12 1.275(9) . ? N9 O13 1.202(9) . ? N9 O14 1.264(8) . ? N10 O16 1.272(10) . ? N10 O17 1.247(12) . ? N10 O18 1.276(13) . ? O1 P1 1.579(4) . ? O2 P1 1.581(4) . ? O3 P2 1.583(4) . ? O4 P2 1.585(4) . ? O5 P3 1.586(4) . ? O6 P3 1.588(4) . ? O7 H7 0.8400 . ? O11 H11A 0.83(2) . ? O15 H15A 0.847(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 123.8(6) . . ? C2 C1 O1 117.3(6) . . ? C6 C1 O1 118.8(5) . . ? C1 C2 H2 121.1 . . ? C1 C2 C3 117.9(7) . . ? C3 C2 H2 121.1 . . ? C2 C3 H3 119.9 . . ? C4 C3 C2 120.3(7) . . ? C4 C3 H3 119.9 . . ? C3 C4 H4 119.8 . . ? C3 C4 C5 120.5(7) . . ? C5 C4 H4 119.8 . . ? C4 C5 H5 119.4 . . ? C6 C5 C4 121.2(7) . . ? C6 C5 H5 119.4 . . ? C1 C6 C7 121.4(5) . . ? C5 C6 C1 116.3(6) . . ? C5 C6 C7 122.3(6) . . ? C8 C7 C6 121.5(6) . . ? C12 C7 C6 123.5(6) . . ? C12 C7 C8 114.9(6) . . ? C7 C8 H8 118.6 . . ? C9 C8 C7 122.8(7) . . ? C9 C8 H8 118.6 . . ? C8 C9 H9 120.4 . . ? C10 C9 C8 119.1(7) . . ? C10 C9 H9 120.4 . . ? C9 C10 H10 120.1 . . ? C9 C10 C11 119.8(7) . . ? C11 C10 H10 120.1 . . ? C10 C11 H11 120.0 . . ? C12 C11 C10 120.1(7) . . ? C12 C11 H11 120.0 . . ? C7 C12 O2 118.9(6) . . ? C11 C12 C7 123.3(6) . . ? C11 C12 O2 117.6(6) . . ? C17 C13 C14 119.9(6) . . ? C17 C13 O3 120.6(6) . . ? O3 C13 C14 119.2(5) . . ? C13 C14 H14 118.4 . . ? N4 C14 C13 123.3(6) . . ? N4 C14 H14 118.4 . . ? C16 C15 H15 118.1 . . ? C16 C15 N4 123.9(7) . . ? N4 C15 H15 118.1 . . ? C15 C16 H16 120.8 . . ? C15 C16 C17 118.4(7) . . ? C17 C16 H16 120.8 . . ? C13 C17 C16 118.3(7) . . ? C13 C17 H17 120.9 . . ? C16 C17 H17 120.9 . . ? C19 C18 C22 120.3(5) . . ? C19 C18 O4 120.2(5) . . ? O4 C18 C22 119.4(5) . . ? C18 C19 H19 118.4 . . ? N5 C19 C18 123.2(6) . . ? N5 C19 H19 118.4 . . ? C21 C20 H20 118.0 . . ? N5 C20 H20 118.0 . . ? N5 C20 C21 124.0(6) . . ? C20 C21 H21 120.0 . . ? C20 C21 C22 120.0(6) . . ? C22 C21 H21 120.0 . . ? C18 C22 H22 121.7 . . ? C21 C22 C18 116.7(6) . . ? C21 C22 H22 121.7 . . ? C24 C23 C27 121.3(6) 7_565 7_565 ? C24 C23 O5 117.8(5) 7_565 . ? C27 C23 O5 120.8(5) 7_565 . ? C23 C24 H24 119.5 7_565 . ? N6 C24 C23 121.1(6) . 7_565 ? N6 C24 H24 119.5 . . ? C26 C25 H25 118.9 . . ? N6 C25 H25 118.9 . . ? N6 C25 C26 122.2(6) . . ? C25 C26 H26 120.6 . . ? C27 C26 C25 118.8(6) . . ? C27 C26 H26 120.6 . . ? C23 C27 C26 117.6(5) 7_565 . ? C23 C27 H27 121.2 7_565 . ? C26 C27 H27 121.2 . . ? C32 C28 C29 120.4(6) . . ? O6 C28 C29 122.4(5) . . ? O6 C28 C32 117.2(5) . . ? C28 C29 H29 119.7 . . ? N7 C29 C28 120.7(5) . . ? N7 C29 H29 119.7 . . ? C31 C30 H30 118.4 . . ? N7 C30 H30 118.4 . . ? N7 C30 C31 123.2(6) . . ? C30 C31 H31 120.2 . . ? C30 C31 C32 119.6(6) . . ? C32 C31 H31 120.2 . . ? C28 C32 C31 117.5(5) . . ? C28 C32 H32 121.2 . . ? C31 C32 H32 121.2 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O11 C35 H35A 109.5 . . ? O11 C35 H35B 109.5 . . ? O11 C35 H35C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O15 C36 H36A 109.5 . . ? O15 C36 H36B 109.5 . . ? O15 C36 H36C 109.5 . . ? N5 Cd1 N5 176.1(2) . 2_655 ? N5 Cd1 O7 88.05(12) . . ? N5 Cd1 O7 88.04(12) 2_655 . ? N5 Cd1 O9 89.99(17) . 2_655 ? N5 Cd1 O9 89.92(17) 2_655 2_655 ? N5 Cd1 O9 89.92(17) . . ? N5 Cd1 O9 89.99(17) 2_655 . ? N5 Cd1 O10 98.11(16) 2_655 . ? N5 Cd1 O10 84.93(17) 2_655 2_655 ? N5 Cd1 O10 84.93(17) . . ? N5 Cd1 O10 98.11(16) . 2_655 ? O7 Cd1 O9 88.64(10) . 2_655 ? O7 Cd1 O9 88.64(10) . . ? O7 Cd1 O10 140.63(10) . 2_655 ? O7 Cd1 O10 140.63(10) . . ? O9 Cd1 O9 177.3(2) 2_655 . ? O9 Cd1 O10 129.95(15) 2_655 . ? O9 Cd1 O10 52.74(14) . . ? O9 Cd1 O10 52.74(14) 2_655 2_655 ? O9 Cd1 O10 129.95(15) . 2_655 ? O10 Cd1 O10 78.7(2) . 2_655 ? N6 Cd2 N7 173.2(2) . . ? N6 Cd2 O11 87.2(2) . . ? N6 Cd2 O12 86.10(18) . . ? N6 Cd2 O14 95.63(19) . . ? N6 Cd2 O15 93.0(2) . . ? N6 Cd2 O16 89.00(19) . . ? N7 Cd2 O11 88.4(2) . . ? N7 Cd2 O12 97.55(18) . . ? N7 Cd2 O14 91.1(2) . . ? N7 Cd2 O15 89.1(2) . . ? N7 Cd2 O16 85.25(19) . . ? O11 Cd2 O12 73.3(2) . . ? O11 Cd2 O14 123.9(2) . . ? O11 Cd2 O15 157.3(3) . . ? O11 Cd2 O16 81.1(2) . . ? O14 Cd2 O12 51.18(18) . . ? O14 Cd2 O16 154.7(2) . . ? O15 Cd2 O12 129.4(3) . . ? O15 Cd2 O14 78.7(3) . . ? O15 Cd2 O16 76.2(3) . . ? O16 Cd2 O12 154.16(19) . . ? P1 N1 P2 123.3(3) . . ? P3 N2 P2 122.3(3) . . ? P3 N3 P1 120.5(3) . . ? C14 N4 C15 116.1(7) . . ? C19 N5 C20 115.8(5) . . ? C19 N5 Cd1 121.1(4) . . ? C20 N5 Cd1 123.1(4) . . ? C24 N6 C25 119.0(5) . . ? C24 N6 Cd2 123.6(4) . . ? C25 N6 Cd2 117.4(4) . . ? C29 N7 Cd2 118.0(4) . . ? C30 N7 C29 118.6(5) . . ? C30 N7 Cd2 123.4(4) . . ? O8 N8 O9 120.6(5) . . ? O8 N8 O10 121.8(5) . . ? O10 N8 O9 117.5(5) . . ? O13 N9 O12 120.9(7) . . ? O13 N9 O14 121.9(8) . . ? O14 N9 O12 117.1(7) . . ? O16 N10 O18 115.9(10) . . ? O17 N10 O16 126.8(11) . . ? O17 N10 O18 117.3(10) . . ? C1 O1 P1 120.7(3) . . ? C12 O2 P1 120.7(4) . . ? C13 O3 P2 122.2(4) . . ? C18 O4 P2 123.6(4) . . ? C23 O5 P3 120.6(3) . . ? C28 O6 P3 126.2(4) . . ? Cd1 O7 H7 109.5 . . ? N8 O9 Cd1 94.4(3) . . ? N8 O10 Cd1 94.0(3) . . ? C35 O11 Cd2 126.9(6) . . ? C35 O11 H11A 98(5) . . ? Cd2 O11 H11A 129(5) . . ? N9 O12 Cd2 91.1(4) . . ? N9 O14 Cd2 100.5(5) . . ? C36 O15 Cd2 135.9(7) . . ? C36 O15 H15A 128(5) . . ? Cd2 O15 H15A 93(5) . . ? N10 O16 Cd2 134.4(7) . . ? N1 P1 N3 117.9(3) . . ? N1 P1 O1 105.0(2) . . ? N1 P1 O2 112.4(3) . . ? O1 P1 N3 111.6(2) . . ? O1 P1 O2 104.4(2) . . ? O2 P1 N3 104.9(2) . . ? N2 P2 N1 115.9(3) . . ? N2 P2 O3 111.7(2) . . ? N2 P2 O4 110.7(2) . . ? O3 P2 N1 110.7(2) . . ? O3 P2 O4 94.7(2) . . ? O4 P2 N1 111.1(2) . . ? N2 P3 O5 108.9(2) . . ? N2 P3 O6 111.8(2) . . ? N3 P3 N2 118.4(3) . . ? N3 P3 O5 110.6(2) . . ? N3 P3 O6 106.2(2) . . ? O5 P3 O6 99.2(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 C3 C4 -0.8(9) . . . . ? C1 C6 C7 C8 141.1(6) . . . . ? C1 C6 C7 C12 -43.0(9) . . . . ? C1 O1 P1 N1 -162.7(4) . . . . ? C1 O1 P1 N3 68.5(5) . . . . ? C1 O1 P1 O2 -44.3(5) . . . . ? C2 C1 C6 C5 -0.4(9) . . . . ? C2 C1 C6 C7 179.0(6) . . . . ? C2 C1 O1 P1 -110.2(5) . . . . ? C2 C3 C4 C5 -0.9(11) . . . . ? C3 C4 C5 C6 2.0(10) . . . . ? C4 C5 C6 C1 -1.3(9) . . . . ? C4 C5 C6 C7 179.2(6) . . . . ? C5 C6 C7 C8 -39.5(9) . . . . ? C5 C6 C7 C12 136.5(6) . . . . ? C6 C1 C2 C3 1.5(9) . . . . ? C6 C1 O1 P1 73.8(6) . . . . ? C6 C7 C8 C9 177.5(6) . . . . ? C6 C7 C12 C11 -176.5(6) . . . . ? C6 C7 C12 O2 -1.4(9) . . . . ? C7 C8 C9 C10 -1.4(11) . . . . ? C7 C12 O2 P1 71.5(6) . . . . ? C8 C7 C12 C11 -0.4(9) . . . . ? C8 C7 C12 O2 174.8(5) . . . . ? C8 C9 C10 C11 0.6(10) . . . . ? C9 C10 C11 C12 0.3(10) . . . . ? C10 C11 C12 C7 -0.4(9) . . . . ? C10 C11 C12 O2 -175.6(6) . . . . ? C11 C12 O2 P1 -113.1(5) . . . . ? C12 C7 C8 C9 1.3(9) . . . . ? C12 O2 P1 N1 68.4(5) . . . . ? C12 O2 P1 N3 -162.3(4) . . . . ? C12 O2 P1 O1 -44.8(5) . . . . ? C13 C14 N4 C15 0.9(10) . . . . ? C13 O3 P2 N1 55.6(5) . . . . ? C13 O3 P2 N2 -75.3(5) . . . . ? C13 O3 P2 O4 170.3(4) . . . . ? C14 C13 C17 C16 0.4(9) . . . . ? C14 C13 O3 P2 -88.9(6) . . . . ? C15 C16 C17 C13 1.9(10) . . . . ? C16 C15 N4 C14 1.6(11) . . . . ? C17 C13 C14 N4 -1.8(10) . . . . ? C17 C13 O3 P2 96.2(6) . . . . ? C18 C19 N5 C20 0.7(8) . . . . ? C18 C19 N5 Cd1 179.3(4) . . . . ? C18 O4 P2 N1 -97.9(5) . . . . ? C18 O4 P2 N2 32.5(5) . . . . ? C18 O4 P2 O3 147.8(4) . . . . ? C19 C18 C22 C21 2.3(9) . . . . ? C19 C18 O4 P2 86.4(6) . . . . ? C20 C21 C22 C18 -2.1(10) . . . . ? C21 C20 N5 C19 -0.5(9) . . . . ? C21 C20 N5 Cd1 -179.1(5) . . . . ? C22 C18 C19 N5 -1.7(9) . . . . ? C22 C18 O4 P2 -96.7(6) . . . . ? C23 C24 N6 C25 1.8(9) 7_565 . . . ? C23 C24 N6 Cd2 179.5(4) 7_565 . . . ? C23 O5 P3 N2 62.3(5) . . . . ? C23 O5 P3 N3 -69.5(4) . . . . ? C23 O5 P3 O6 179.3(4) . . . . ? C24 C23 O5 P3 -118.2(5) 7_565 . . . ? C25 C26 C27 C23 1.6(9) . . . 7_565 ? C26 C25 N6 C24 -1.0(9) . . . . ? C26 C25 N6 Cd2 -178.8(5) . . . . ? C27 C23 O5 P3 63.7(7) 7_565 . . . ? C28 C29 N7 C30 -0.7(10) . . . . ? C28 C29 N7 Cd2 175.5(4) . . . . ? C28 O6 P3 N2 38.6(5) . . . . ? C28 O6 P3 N3 169.2(4) . . . . ? C28 O6 P3 O5 -76.1(5) . . . . ? C29 C28 C32 C31 -1.6(9) . . . . ? C29 C28 O6 P3 22.0(8) . . . . ? C30 C31 C32 C28 2.0(11) . . . . ? C31 C30 N7 C29 1.1(12) . . . . ? C31 C30 N7 Cd2 -174.9(6) . . . . ? C32 C28 C29 N7 1.0(9) . . . . ? C32 C28 O6 P3 -159.7(4) . . . . ? N4 C15 C16 C17 -3.0(11) . . . . ? N5 C20 C21 C22 1.3(11) . . . . ? N5 Cd1 N5 C19 99.5(4) 2_655 . . . ? N5 Cd1 N5 C20 -81.9(5) 2_655 . . . ? N5 Cd1 O9 N8 -106.8(3) 2_655 . . . ? N5 Cd1 O9 N8 77.1(3) . . . . ? N5 Cd1 O10 N8 90.4(3) 2_655 . . . ? N5 Cd1 O10 N8 -87.2(3) . . . . ? N6 C25 C26 C27 -0.7(9) . . . . ? N6 Cd2 N7 C29 108.4(16) . . . . ? N6 Cd2 N7 C30 -75.6(18) . . . . ? N6 Cd2 O11 C35 -137.7(9) . . . . ? N6 Cd2 O12 N9 99.6(4) . . . . ? N6 Cd2 O14 N9 -79.5(5) . . . . ? N6 Cd2 O15 C36 -64.8(12) . . . . ? N6 Cd2 O16 N10 -99.1(7) . . . . ? N7 C30 C31 C32 -1.8(13) . . . . ? N7 Cd2 N6 C24 -102.7(16) . . . . ? N7 Cd2 N6 C25 75.0(17) . . . . ? N7 Cd2 O11 C35 37.1(9) . . . . ? N7 Cd2 O12 N9 -86.1(4) . . . . ? N7 Cd2 O14 N9 99.7(5) . . . . ? N7 Cd2 O15 C36 121.6(12) . . . . ? N7 Cd2 O16 N10 84.4(7) . . . . ? O1 C1 C2 C3 -174.3(5) . . . . ? O1 C1 C6 C5 175.3(5) . . . . ? O1 C1 C6 C7 -5.2(8) . . . . ? O3 C13 C14 N4 -176.8(6) . . . . ? O3 C13 C17 C16 175.3(6) . . . . ? O4 C18 C19 N5 175.2(5) . . . . ? O4 C18 C22 C21 -174.6(6) . . . . ? O6 C28 C29 N7 179.3(6) . . . . ? O6 C28 C32 C31 -180.0(6) . . . . ? O7 Cd1 N5 C19 99.5(4) . . . . ? O7 Cd1 N5 C20 -81.9(5) . . . . ? O7 Cd1 O9 N8 165.2(3) . . . . ? O7 Cd1 O10 N8 -6.5(4) . . . . ? O8 N8 O9 Cd1 -167.1(5) . . . . ? O8 N8 O10 Cd1 167.1(5) . . . . ? O9 Cd1 N5 C19 -171.8(4) . . . . ? O9 Cd1 N5 C19 10.9(4) 2_655 . . . ? O9 Cd1 N5 C20 6.7(5) . . . . ? O9 Cd1 N5 C20 -170.6(5) 2_655 . . . ? O9 Cd1 O9 N8 165.2(3) 2_655 . . . ? O9 Cd1 O10 N8 -172.9(3) 2_655 . . . ? O9 Cd1 O10 N8 6.6(3) . . . . ? O9 N8 O10 Cd1 -11.4(5) . . . . ? O10 Cd1 N5 C19 -41.4(4) 2_655 . . . ? O10 Cd1 N5 C19 -119.2(4) . . . . ? O10 Cd1 N5 C20 137.1(5) 2_655 . . . ? O10 Cd1 N5 C20 59.3(5) . . . . ? O10 Cd1 O9 N8 -6.6(3) . . . . ? O10 Cd1 O9 N8 -23.4(4) 2_655 . . . ? O10 Cd1 O10 N8 173.5(4) 2_655 . . . ? O10 N8 O9 Cd1 11.5(5) . . . . ? O11 Cd2 N6 C24 -53.3(5) . . . . ? O11 Cd2 N6 C25 124.4(5) . . . . ? O11 Cd2 N7 C29 59.1(5) . . . . ? O11 Cd2 N7 C30 -124.9(6) . . . . ? O11 Cd2 O12 N9 -172.2(4) . . . . ? O11 Cd2 O14 N9 10.9(5) . . . . ? O11 Cd2 O15 C36 -154.7(11) . . . . ? O11 Cd2 O16 N10 173.6(7) . . . . ? O12 Cd2 N6 C24 20.2(5) . . . . ? O12 Cd2 N6 C25 -162.1(5) . . . . ? O12 Cd2 N7 C29 -13.9(5) . . . . ? O12 Cd2 N7 C30 162.2(6) . . . . ? O12 Cd2 O11 C35 135.5(9) . . . . ? O12 Cd2 O14 N9 0.9(4) . . . . ? O12 Cd2 O15 C36 22.6(13) . . . . ? O12 Cd2 O16 N10 -178.1(6) . . . . ? O12 N9 O14 Cd2 -1.6(7) . . . . ? O13 N9 O12 Cd2 -179.0(7) . . . . ? O13 N9 O14 Cd2 178.9(7) . . . . ? O14 Cd2 N6 C24 70.5(5) . . . . ? O14 Cd2 N6 C25 -111.8(5) . . . . ? O14 Cd2 N7 C29 -64.8(5) . . . . ? O14 Cd2 N7 C30 111.2(6) . . . . ? O14 Cd2 O11 C35 127.4(8) . . . . ? O14 Cd2 O12 N9 -0.9(4) . . . . ? O14 Cd2 O15 C36 30.3(12) . . . . ? O14 Cd2 O16 N10 2.0(10) . . . . ? O14 N9 O12 Cd2 1.4(6) . . . . ? O15 Cd2 N6 C24 149.4(5) . . . . ? O15 Cd2 N6 C25 -32.9(5) . . . . ? O15 Cd2 N7 C29 -143.5(5) . . . . ? O15 Cd2 N7 C30 32.6(6) . . . . ? O15 Cd2 O11 C35 -46.6(11) . . . . ? O15 Cd2 O12 N9 8.9(5) . . . . ? O15 Cd2 O14 N9 -171.5(5) . . . . ? O15 Cd2 O16 N10 -5.8(7) . . . . ? O16 Cd2 N6 C24 -134.4(5) . . . . ? O16 Cd2 N6 C25 43.3(5) . . . . ? O16 Cd2 N7 C29 140.3(5) . . . . ? O16 Cd2 N7 C30 -43.7(6) . . . . ? O16 Cd2 O11 C35 -48.3(9) . . . . ? O16 Cd2 O12 N9 179.2(4) . . . . ? O16 Cd2 O14 N9 -179.1(4) . . . . ? O16 Cd2 O15 C36 -153.0(12) . . . . ? O17 N10 O16 Cd2 -6.7(14) . . . . ? O18 N10 O16 Cd2 172.9(8) . . . . ? P1 N1 P2 N2 1.7(5) . . . . ? P1 N1 P2 O3 -127.0(3) . . . . ? P1 N1 P2 O4 129.2(3) . . . . ? P1 N3 P3 N2 15.8(5) . . . . ? P1 N3 P3 O5 142.4(3) . . . . ? P1 N3 P3 O6 -110.9(3) . . . . ? P2 N1 P1 N3 0.5(5) . . . . ? P2 N1 P1 O1 -124.5(3) . . . . ? P2 N1 P1 O2 122.7(3) . . . . ? P2 N2 P3 N3 -13.8(5) . . . . ? P2 N2 P3 O5 -141.2(3) . . . . ? P2 N2 P3 O6 110.1(3) . . . . ? P3 N2 P2 N1 5.1(5) . . . . ? P3 N2 P2 O3 133.3(3) . . . . ? P3 N2 P2 O4 -122.6(3) . . . . ? P3 N3 P1 N1 -9.4(5) . . . . ? P3 N3 P1 O1 112.2(3) . . . . ? P3 N3 P1 O2 -135.3(3) . . . . ? data_908594 _database_code_depnum_ccdc_archive 'CCDC 908594' #TrackingRef '17694_web_deposit_cif_file_5_RSuriyaNarayanan_1360734625.908594.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H48 Cl2 Co N10 O12 P6, 4(C H Cl3)' _chemical_formula_sum 'C72 H52 Cl14 Co N10 O12 P6' _chemical_formula_weight 1990.29 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' Co Co 0.3494 0.9721 '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 9.708(5) _cell_length_b 25.369(5) _cell_length_c 17.721(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 105.577(5) _cell_angle_gamma 90.000(5) _cell_volume 4204(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3548 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 21.50 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2010 _exptl_absorpt_coefficient_mu 0.828 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.914 _exptl_absorpt_correction_T_max 0.952 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 4033 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25123 _diffrn_reflns_av_R_equivalents 0.0642 _diffrn_reflns_av_unetI/netI 0.0783 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 27.00 _reflns_number_total 9133 _reflns_number_gt 5567 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0961P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9133 _refine_ls_number_parameters 520 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1120 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1926 _refine_ls_wR_factor_gt 0.1603 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 Co1 Co 1.0000 0.0000 1.0000 0.0394(2) Uani 1 2 d S . . Cl1 Cl 1.15830(11) 0.05327(4) 1.09944(6) 0.0510(3) Uani 1 1 d . . . Cl2 Cl -0.1430(2) 0.29107(8) 0.77359(12) 0.1225(7) Uani 1 1 d . . . Cl3 Cl 0.0416(2) 0.32698(9) 0.91727(13) 0.1355(7) Uani 1 1 d . . . Cl4 Cl 0.0734(2) 0.36572(7) 0.76834(13) 0.1195(7) Uani 1 1 d . . . Cl5 Cl 0.7584(4) 0.43069(11) 0.83320(17) 0.1979(14) Uani 1 1 d . . . Cl6 Cl 0.8359(2) 0.52872(11) 0.91423(13) 0.1507(9) Uani 1 1 d . . . Cl7 Cl 0.5504(2) 0.51007(8) 0.82349(12) 0.1189(6) Uani 1 1 d . . . P1 P 0.44340(10) 0.10509(4) 0.85638(6) 0.0378(2) Uani 1 1 d . . . P2 P 0.35612(10) 0.19591(4) 0.91277(6) 0.0387(3) Uani 1 1 d . . . P3 P 0.19375(10) 0.15161(4) 0.77518(5) 0.0378(2) Uani 1 1 d . . . O1 O 0.4801(3) 0.04838(10) 0.89337(16) 0.0475(7) Uani 1 1 d . . . O2 O 0.5696(3) 0.11306(10) 0.81594(14) 0.0431(6) Uani 1 1 d . . . O3 O 0.2820(3) 0.20224(10) 0.98153(14) 0.0414(6) Uani 1 1 d . . . O4 O 0.4603(3) 0.24483(10) 0.92480(15) 0.0472(7) Uani 1 1 d . . . O5 O 0.1755(3) 0.17033(11) 0.68823(14) 0.0453(7) Uani 1 1 d . . . O6 O 0.0381(3) 0.13317(10) 0.77445(14) 0.0442(6) Uani 1 1 d . . . N1 N 0.4557(3) 0.14562(13) 0.92486(18) 0.0459(8) Uani 1 1 d . . . N2 N 0.2313(3) 0.19930(12) 0.83518(17) 0.0438(8) Uani 1 1 d . . . N3 N 0.3004(3) 0.10374(12) 0.78859(18) 0.0423(8) Uani 1 1 d . . . N4 N 0.8240(3) 0.01462(12) 1.05818(19) 0.0444(8) Uani 1 1 d . . . N5 N 0.9204(3) 0.07279(12) 0.93324(18) 0.0407(7) Uani 1 1 d . . . C1 C 0.6182(4) -0.01056(15) 1.0980(2) 0.0416(9) Uani 1 1 d . . . C2 C 0.7286(4) -0.02190(15) 1.0657(2) 0.0429(9) Uani 1 1 d . . . H2 H 0.7376 -0.0560 1.0486 0.051 Uiso 1 1 calc R . . C3 C 0.8067(5) 0.06318(16) 1.0827(3) 0.0571(11) Uani 1 1 d . . . H3 H 0.8741 0.0886 1.0798 0.069 Uiso 1 1 calc R . . C4 C 0.6950(6) 0.07774(18) 1.1119(3) 0.0705(14) Uani 1 1 d . . . H4 H 0.6860 0.1125 1.1268 0.085 Uiso 1 1 calc R . . C5 C 0.5960(5) 0.04022(17) 1.1190(3) 0.0577(11) Uani 1 1 d . . . H5 H 0.5176 0.0490 1.1373 0.069 Uiso 1 1 calc R . . C6 C 0.7120(4) 0.11684(14) 0.8599(2) 0.0371(8) Uani 1 1 d . . . C7 C 0.7841(4) 0.07192(15) 0.8907(2) 0.0409(9) Uani 1 1 d . . . H7 H 0.7365 0.0398 0.8816 0.049 Uiso 1 1 calc R . . C8 C 0.9871(4) 0.11989(15) 0.9427(2) 0.0438(9) Uani 1 1 d . . . H8 H 1.0824 0.1213 0.9716 0.053 Uiso 1 1 calc R . . C9 C 0.9218(4) 0.16569(15) 0.9119(2) 0.0466(10) Uani 1 1 d . . . H9 H 0.9726 0.1972 0.9192 0.056 Uiso 1 1 calc R . . C10 C 0.7801(4) 0.16497(15) 0.8700(2) 0.0460(10) Uani 1 1 d . . . H10 H 0.7324 0.1957 0.8494 0.055 Uiso 1 1 calc R . . C11 C 0.3676(4) 0.20907(15) 1.0595(2) 0.0392(9) Uani 1 1 d . . . C12 C 0.3762(5) 0.16818(17) 1.1104(2) 0.0506(10) Uani 1 1 d . . . H12 H 0.3347 0.1359 1.0926 0.061 Uiso 1 1 calc R . . C13 C 0.4466(6) 0.1750(2) 1.1881(3) 0.0626(12) Uani 1 1 d . . . H13 H 0.4543 0.1472 1.2233 0.075 Uiso 1 1 calc R . . C14 C 0.5057(5) 0.2234(2) 1.2132(3) 0.0661(13) Uani 1 1 d . . . H14 H 0.5524 0.2284 1.2659 0.079 Uiso 1 1 calc R . . C15 C 0.4968(5) 0.26451(19) 1.1617(2) 0.0584(12) Uani 1 1 d . . . H15 H 0.5377 0.2968 1.1798 0.070 Uiso 1 1 calc R . . C16 C 0.4269(4) 0.25828(15) 1.0822(2) 0.0452(9) Uani 1 1 d . . . C17 C 0.4183(4) 0.30232(16) 1.0263(2) 0.0481(10) Uani 1 1 d . . . C18 C 0.4025(5) 0.35448(18) 1.0481(3) 0.0648(13) Uani 1 1 d . . . H18 H 0.3904 0.3611 1.0976 0.078 Uiso 1 1 calc R . . C19 C 0.4040(7) 0.3957(2) 0.9998(3) 0.0810(16) Uani 1 1 d . . . H19 H 0.3957 0.4299 1.0169 0.097 Uiso 1 1 calc R . . C20 C 0.4179(7) 0.3872(2) 0.9257(4) 0.0825(16) Uani 1 1 d . . . H20 H 0.4196 0.4155 0.8926 0.099 Uiso 1 1 calc R . . C21 C 0.4291(6) 0.33642(18) 0.9009(3) 0.0644(13) Uani 1 1 d . . . H21 H 0.4357 0.3302 0.8503 0.077 Uiso 1 1 calc R . . C22 C 0.4306(4) 0.29510(15) 0.9505(2) 0.0458(10) Uani 1 1 d . . . C23 C 0.0556(4) 0.20108(18) 0.6492(2) 0.0487(10) Uani 1 1 d . . . C24 C 0.0780(6) 0.25278(19) 0.6355(3) 0.0643(13) Uani 1 1 d . . . H24 H 0.1679 0.2678 0.6551 0.077 Uiso 1 1 calc R . . C25 C -0.0329(8) 0.2823(2) 0.5926(3) 0.0853(17) Uani 1 1 d . . . H25 H -0.0182 0.3175 0.5824 0.102 Uiso 1 1 calc R . . C26 C -0.1665(7) 0.2603(3) 0.5643(3) 0.094(2) Uani 1 1 d . . . H26 H -0.2421 0.2806 0.5353 0.113 Uiso 1 1 calc R . . C27 C -0.1877(6) 0.2079(3) 0.5792(3) 0.0812(16) Uani 1 1 d . . . H27 H -0.2778 0.1930 0.5595 0.097 Uiso 1 1 calc R . . C28 C -0.0763(5) 0.17702(19) 0.6231(2) 0.0559(11) Uani 1 1 d . . . C29 C -0.1024(5) 0.1213(2) 0.6413(3) 0.0591(12) Uani 1 1 d . . . C30 C -0.1917(6) 0.0878(3) 0.5859(3) 0.0876(18) Uani 1 1 d . . . H30 H -0.2350 0.1002 0.5358 0.105 Uiso 1 1 calc R . . C31 C -0.2151(7) 0.0366(3) 0.6057(4) 0.102(2) Uani 1 1 d . . . H31 H -0.2730 0.0147 0.5684 0.122 Uiso 1 1 calc R . . C32 C -0.1543(7) 0.0176(2) 0.6797(4) 0.0926(19) Uani 1 1 d . . . H32 H -0.1742 -0.0166 0.6926 0.111 Uiso 1 1 calc R . . C33 C -0.0650(5) 0.04855(18) 0.7343(3) 0.0634(12) Uani 1 1 d . . . H33 H -0.0203 0.0353 0.7838 0.076 Uiso 1 1 calc R . . C34 C -0.0417(4) 0.09990(16) 0.7153(2) 0.0462(10) Uani 1 1 d . . . C35 C 0.0287(7) 0.3123(2) 0.8200(4) 0.0942(19) Uani 1 1 d . . . H35 H 0.0951 0.2833 0.8187 0.113 Uiso 1 1 calc R . . C36 C 0.7269(7) 0.4976(3) 0.8317(4) 0.100(2) Uani 1 1 d . . . H36 H 0.7498 0.5122 0.7854 0.120 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 Co1 0.0321(4) 0.0338(4) 0.0519(4) 0.0032(3) 0.0106(3) -0.0002(3) Cl1 0.0479(6) 0.0405(5) 0.0603(6) -0.0011(4) 0.0072(5) -0.0037(4) Cl2 0.1011(14) 0.1270(15) 0.1305(15) 0.0119(12) 0.0158(11) -0.0371(11) Cl3 0.1180(16) 0.1512(18) 0.1230(15) -0.0019(13) 0.0076(13) 0.0170(13) Cl4 0.1082(14) 0.0792(11) 0.1604(17) 0.0155(11) 0.0177(12) -0.0146(9) Cl5 0.269(4) 0.136(2) 0.199(3) 0.0198(18) 0.081(3) 0.099(2) Cl6 0.1112(16) 0.214(3) 0.1322(17) 0.0009(17) 0.0417(14) -0.0006(16) Cl7 0.1027(14) 0.1144(14) 0.1464(16) 0.0318(12) 0.0451(12) 0.0030(10) P1 0.0331(5) 0.0357(5) 0.0428(5) 0.0015(4) 0.0067(4) 0.0043(4) P2 0.0346(5) 0.0395(5) 0.0392(5) -0.0043(4) 0.0053(4) 0.0011(4) P3 0.0308(5) 0.0427(6) 0.0374(5) -0.0016(4) 0.0047(4) 0.0034(4) O1 0.0331(15) 0.0417(15) 0.0678(18) 0.0135(13) 0.0140(13) 0.0057(11) O2 0.0359(15) 0.0479(15) 0.0442(14) 0.0061(12) 0.0084(12) 0.0017(12) O3 0.0365(15) 0.0429(15) 0.0426(14) -0.0076(12) 0.0066(12) -0.0036(11) O4 0.0430(16) 0.0513(17) 0.0495(15) -0.0083(13) 0.0160(13) -0.0064(13) O5 0.0357(15) 0.0583(17) 0.0405(14) 0.0015(12) 0.0079(12) 0.0008(12) O6 0.0337(15) 0.0560(17) 0.0423(14) -0.0012(12) 0.0090(12) 0.0005(12) N1 0.0376(19) 0.051(2) 0.0429(18) -0.0058(15) -0.0002(15) 0.0086(15) N2 0.0415(19) 0.0383(18) 0.0463(18) -0.0028(14) 0.0023(15) 0.0076(14) N3 0.0380(18) 0.0395(18) 0.0452(18) -0.0051(14) 0.0039(15) 0.0052(14) N4 0.0387(19) 0.0379(18) 0.057(2) 0.0012(15) 0.0125(16) -0.0027(14) N5 0.0315(17) 0.0392(18) 0.0512(19) 0.0012(14) 0.0109(15) 0.0008(14) C1 0.036(2) 0.039(2) 0.049(2) 0.0070(17) 0.0097(18) 0.0035(17) C2 0.036(2) 0.037(2) 0.054(2) 0.0004(18) 0.0091(18) 0.0042(17) C3 0.061(3) 0.036(2) 0.079(3) -0.006(2) 0.028(3) -0.010(2) C4 0.086(4) 0.039(2) 0.105(4) -0.011(2) 0.057(3) -0.004(2) C5 0.061(3) 0.045(2) 0.077(3) -0.002(2) 0.035(3) 0.008(2) C6 0.031(2) 0.040(2) 0.040(2) 0.0022(16) 0.0102(16) 0.0014(16) C7 0.036(2) 0.036(2) 0.049(2) 0.0006(17) 0.0089(18) -0.0039(16) C8 0.034(2) 0.047(2) 0.052(2) -0.0014(19) 0.0136(18) -0.0054(18) C9 0.043(2) 0.037(2) 0.061(3) 0.0021(19) 0.016(2) -0.0062(18) C10 0.050(3) 0.035(2) 0.055(2) 0.0075(18) 0.016(2) 0.0024(18) C11 0.031(2) 0.049(2) 0.037(2) -0.0032(17) 0.0088(16) 0.0003(17) C12 0.056(3) 0.046(2) 0.051(2) -0.0027(19) 0.016(2) 0.000(2) C13 0.075(3) 0.063(3) 0.053(3) 0.009(2) 0.022(2) 0.009(3) C14 0.067(3) 0.083(4) 0.042(2) -0.001(2) 0.005(2) -0.004(3) C15 0.062(3) 0.066(3) 0.045(2) -0.012(2) 0.009(2) -0.019(2) C16 0.045(2) 0.046(2) 0.045(2) -0.0056(18) 0.0132(19) -0.0077(18) C17 0.045(2) 0.047(2) 0.051(2) -0.0077(19) 0.0102(19) -0.0091(19) C18 0.079(4) 0.048(3) 0.069(3) -0.011(2) 0.024(3) -0.008(2) C19 0.108(5) 0.047(3) 0.093(4) -0.007(3) 0.036(4) -0.008(3) C20 0.108(5) 0.046(3) 0.097(4) 0.018(3) 0.034(4) -0.003(3) C21 0.083(4) 0.055(3) 0.058(3) 0.007(2) 0.024(3) -0.004(2) C22 0.047(2) 0.042(2) 0.047(2) -0.0045(18) 0.0118(19) -0.0062(18) C23 0.042(2) 0.063(3) 0.039(2) 0.010(2) 0.0063(18) 0.005(2) C24 0.068(3) 0.064(3) 0.060(3) 0.017(2) 0.016(3) 0.001(2) C25 0.102(5) 0.076(4) 0.079(4) 0.037(3) 0.027(4) 0.020(3) C26 0.079(5) 0.122(6) 0.075(4) 0.039(4) 0.008(3) 0.033(4) C27 0.052(3) 0.118(5) 0.062(3) 0.022(3) -0.005(2) 0.008(3) C28 0.044(3) 0.074(3) 0.042(2) 0.004(2) -0.0013(19) 0.000(2) C29 0.042(2) 0.078(3) 0.052(3) -0.007(2) 0.004(2) -0.011(2) C30 0.065(4) 0.120(5) 0.067(3) -0.020(3) -0.002(3) -0.030(3) C31 0.086(5) 0.104(5) 0.110(5) -0.041(4) 0.018(4) -0.047(4) C32 0.091(5) 0.069(4) 0.121(5) -0.021(4) 0.035(4) -0.030(3) C33 0.056(3) 0.059(3) 0.081(3) -0.002(3) 0.027(3) -0.009(2) C34 0.033(2) 0.055(3) 0.051(2) -0.009(2) 0.0134(18) -0.0075(18) C35 0.076(4) 0.079(4) 0.123(5) 0.013(4) 0.018(4) 0.017(3) C36 0.114(6) 0.109(5) 0.085(4) 0.024(4) 0.041(4) 0.022(4) _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 Co1 N5 2.217(3) 3_757 ? Co1 N5 2.217(3) . ? Co1 N4 2.251(3) 3_757 ? Co1 N4 2.251(3) . ? Co1 Cl1 2.4164(11) 3_757 ? Co1 Cl1 2.4164(11) . ? Cl2 C35 1.734(7) . ? Cl3 C35 1.735(7) . ? Cl4 C35 1.755(6) . ? Cl5 C36 1.724(7) . ? Cl6 C36 1.747(7) . ? Cl7 C36 1.710(7) . ? P1 N1 1.570(3) . ? P1 N3 1.573(3) . ? P1 O1 1.581(3) . ? P1 O2 1.589(3) . ? P2 N2 1.572(3) . ? P2 O4 1.579(3) . ? P2 N1 1.580(3) . ? P2 O3 1.581(3) . ? P3 N3 1.572(3) . ? P3 O5 1.576(3) . ? P3 O6 1.579(3) . ? P3 N2 1.587(3) . ? O1 C1 1.390(4) 3_657 ? O2 C6 1.396(4) . ? O3 C11 1.420(4) . ? O4 C22 1.410(5) . ? O5 C23 1.418(5) . ? O6 C34 1.406(5) . ? N4 C3 1.332(5) . ? N4 C2 1.342(5) . ? N5 C7 1.335(5) . ? N5 C8 1.348(5) . ? C1 C2 1.374(5) . ? C1 C5 1.374(5) . ? C1 O1 1.390(4) 3_657 ? C3 C4 1.372(6) . ? C4 C5 1.383(6) . ? C6 C7 1.372(5) . ? C6 C10 1.377(5) . ? C8 C9 1.365(5) . ? C9 C10 1.376(6) . ? C11 C12 1.362(5) . ? C11 C16 1.388(5) . ? C12 C13 1.374(6) . ? C13 C14 1.379(7) . ? C14 C15 1.374(6) . ? C15 C16 1.399(6) . ? C16 C17 1.480(6) . ? C17 C22 1.393(6) . ? C17 C18 1.399(6) . ? C18 C19 1.354(7) . ? C19 C20 1.372(7) . ? C20 C21 1.375(7) . ? C21 C22 1.365(6) . ? C23 C24 1.362(6) . ? C23 C28 1.381(6) . ? C24 C25 1.362(7) . ? C25 C26 1.377(8) . ? C26 C27 1.382(8) . ? C27 C28 1.391(6) . ? C28 C29 1.486(7) . ? C29 C34 1.394(6) . ? C29 C30 1.407(6) . ? C30 C31 1.380(9) . ? C31 C32 1.373(9) . ? C32 C33 1.362(7) . ? C33 C34 1.380(6) . ? 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 N5 Co1 N5 179.999(1) 3_757 . ? N5 Co1 N4 84.74(11) 3_757 3_757 ? N5 Co1 N4 95.26(11) . 3_757 ? N5 Co1 N4 95.26(11) 3_757 . ? N5 Co1 N4 84.74(11) . . ? N4 Co1 N4 179.998(1) 3_757 . ? N5 Co1 Cl1 89.18(9) 3_757 3_757 ? N5 Co1 Cl1 90.82(9) . 3_757 ? N4 Co1 Cl1 89.21(9) 3_757 3_757 ? N4 Co1 Cl1 90.79(9) . 3_757 ? N5 Co1 Cl1 90.82(9) 3_757 . ? N5 Co1 Cl1 89.18(9) . . ? N4 Co1 Cl1 90.80(9) 3_757 . ? N4 Co1 Cl1 89.20(9) . . ? Cl1 Co1 Cl1 179.998(1) 3_757 . ? N1 P1 N3 118.22(17) . . ? N1 P1 O1 108.27(17) . . ? N3 P1 O1 110.56(16) . . ? N1 P1 O2 110.92(17) . . ? N3 P1 O2 106.69(16) . . ? O1 P1 O2 100.80(14) . . ? N2 P2 O4 112.97(16) . . ? N2 P2 N1 117.55(16) . . ? O4 P2 N1 105.64(17) . . ? N2 P2 O3 105.39(16) . . ? O4 P2 O3 102.93(14) . . ? N1 P2 O3 111.49(16) . . ? N3 P3 O5 106.08(16) . . ? N3 P3 O6 111.27(16) . . ? O5 P3 O6 103.01(14) . . ? N3 P3 N2 117.64(17) . . ? O5 P3 N2 111.75(16) . . ? O6 P3 N2 106.19(16) . . ? C1 O1 P1 126.1(2) 3_657 . ? C6 O2 P1 121.7(2) . . ? C11 O3 P2 119.6(2) . . ? C22 O4 P2 125.1(2) . . ? C23 O5 P3 120.3(2) . . ? C34 O6 P3 121.2(2) . . ? P1 N1 P2 120.5(2) . . ? P2 N2 P3 121.92(19) . . ? P3 N3 P1 120.59(19) . . ? C3 N4 C2 117.1(4) . . ? C3 N4 Co1 118.6(3) . . ? C2 N4 Co1 124.1(3) . . ? C7 N5 C8 117.1(3) . . ? C7 N5 Co1 116.0(2) . . ? C8 N5 Co1 125.8(3) . . ? C2 C1 C5 120.4(4) . . ? C2 C1 O1 122.5(3) . 3_657 ? C5 C1 O1 117.0(4) . 3_657 ? N4 C2 C1 122.2(4) . . ? N4 C3 C4 123.6(4) . . ? C3 C4 C5 119.3(4) . . ? C1 C5 C4 117.2(4) . . ? C7 C6 C10 120.6(4) . . ? C7 C6 O2 119.2(3) . . ? C10 C6 O2 120.2(3) . . ? N5 C7 C6 122.2(3) . . ? N5 C8 C9 123.3(4) . . ? C8 C9 C10 119.6(4) . . ? C9 C10 C6 117.2(4) . . ? C12 C11 C16 123.2(4) . . ? C12 C11 O3 117.9(3) . . ? C16 C11 O3 118.7(3) . . ? C11 C12 C13 119.6(4) . . ? C12 C13 C14 119.2(4) . . ? C15 C14 C13 121.0(4) . . ? C14 C15 C16 120.7(4) . . ? C11 C16 C15 116.3(4) . . ? C11 C16 C17 122.8(3) . . ? C15 C16 C17 120.9(4) . . ? C22 C17 C18 115.8(4) . . ? C22 C17 C16 122.8(4) . . ? C18 C17 C16 121.4(4) . . ? C19 C18 C17 122.3(5) . . ? C18 C19 C20 120.3(5) . . ? C19 C20 C21 119.3(5) . . ? C22 C21 C20 120.1(5) . . ? C21 C22 C17 122.1(4) . . ? C21 C22 O4 117.0(4) . . ? C17 C22 O4 120.5(3) . . ? C24 C23 C28 123.0(4) . . ? C24 C23 O5 117.9(4) . . ? C28 C23 O5 119.1(4) . . ? C23 C24 C25 119.2(5) . . ? C24 C25 C26 120.4(6) . . ? C25 C26 C27 119.6(5) . . ? C26 C27 C28 121.0(5) . . ? C23 C28 C27 116.7(5) . . ? C23 C28 C29 123.0(4) . . ? C27 C28 C29 120.3(4) . . ? C34 C29 C30 116.5(5) . . ? C34 C29 C28 121.4(4) . . ? C30 C29 C28 122.1(4) . . ? C31 C30 C29 120.2(6) . . ? C32 C31 C30 121.1(5) . . ? C33 C32 C31 120.3(6) . . ? C32 C33 C34 119.0(5) . . ? C33 C34 C29 122.9(4) . . ? C33 C34 O6 118.5(4) . . ? C29 C34 O6 118.4(4) . . ? Cl2 C35 Cl3 110.0(4) . . ? Cl2 C35 Cl4 109.5(3) . . ? Cl3 C35 Cl4 112.9(4) . . ? Cl7 C36 Cl5 110.7(4) . . ? Cl7 C36 Cl6 110.9(4) . . ? Cl5 C36 Cl6 111.5(4) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.896 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.111 data_908595 _database_code_depnum_ccdc_archive 'CCDC 908595' #TrackingRef '17695_web_deposit_cif_file_6_RSuriyaNarayanan_1360734625.908595.cif' _audit_creation_date 2013-02-11 _audit_creation_method ; Olex2 1.2 (compiled Dec 5 2012 16:20:19, GUI svn.r4385) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C34 H24 Cl2 Cu N5 O6 P3' _chemical_formula_sum 'C34 H24 Cl2 Cu N5 O6 P3' _chemical_formula_weight 825.93 _chemical_melting_point ? 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' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z+1/2' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x, -y, z-1/2' 7 '-x+1/2, -y+1/2, -z' 8 'x+1/2, -y+1/2, z-1/2' _cell_length_a 35.470(7) _cell_length_b 11.331(2) _cell_length_c 24.468(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.74(3) _cell_angle_gamma 90.00 _cell_volume 9510.1(3) _cell_formula_units_Z 8 _cell_measurement_reflns_used 2943 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 21.132 _cell_measurement_theta_min 2.327 _exptl_absorpt_coefficient_mu 0.712 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.398261 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS v.2.10 (Bruker,2003) was used for absorption correction. R(int) was 0.0963 before and 0.0360 after correction. The Ratio of minimum to maximum transmission is 0.3983. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour 'light blue' _exptl_crystal_density_diffrn 1.154 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 3352 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_unetI/netI 0.0998 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 24874 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.50 _diffrn_reflns_theta_min 2.02 _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4710 _reflns_number_total 8820 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'SAINT v6.45A (Bruker, 2003)' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'SAINT v6.45A (Bruker, 2003)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.394 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.088 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.906 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 460 _refine_ls_number_reflns 8820 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1028 _refine_ls_R_factor_gt 0.0624 _refine_ls_restrained_S_all 0.906 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0950P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1633 _refine_ls_wR_factor_ref 0.1837 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: H10 of C10, H15 of C15, H11 of C11, H16 of C16, H17 of C17, H14 of C14, H20 of C20, H22 of C22, H8 of C8, H21 of C21, H9 of C9, H23 of C23, H26 of C26, H27 of C27, H28 of C28, H31 of C31, H29 of C29, H32 of C32, H33 of C33, H34 of C34, H3 of C3, H2 of C2, H4 of C4, H5 of C5 2.a Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33), C34(H34) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.63558(15) 1.3321(5) 0.7612(2) 0.0612(14) Uani 1 1 d . . . C2 C 0.61908(18) 1.3793(5) 0.8042(3) 0.0822(18) Uani 1 1 d . . . H2 H 0.6163 1.3331 0.8344 0.099 Uiso 1 1 calc R . . C3 C 0.6075(2) 1.4953(6) 0.7992(3) 0.093(2) Uani 1 1 d . . . H3 H 0.5976 1.5311 0.8268 0.111 Uiso 1 1 calc R . . C4 C 0.61103(19) 1.5585(6) 0.7514(4) 0.103(2) Uani 1 1 d . . . H4 H 0.6023 1.6362 0.7468 0.124 Uiso 1 1 calc R . . C5 C 0.62659(19) 1.5099(5) 0.7126(3) 0.0861(19) Uani 1 1 d . . . H5 H 0.6288 1.5550 0.6818 0.103 Uiso 1 1 calc R . . C6 C 0.63953(15) 1.3950(5) 0.7167(3) 0.0679(15) Uani 1 1 d . . . C7 C 0.65721(16) 1.3417(5) 0.6726(2) 0.0637(14) Uani 1 1 d . . . C8 C 0.6849(2) 1.4032(6) 0.6540(3) 0.0883(19) Uani 1 1 d . . . H8 H 0.6926 1.4783 0.6678 0.106 Uiso 1 1 calc R . . C9 C 0.7014(2) 1.3493(8) 0.6132(4) 0.111(3) Uani 1 1 d . . . H9 H 0.7191 1.3926 0.5991 0.133 Uiso 1 1 calc R . . C10 C 0.6926(2) 1.2375(7) 0.5934(3) 0.098(2) Uani 1 1 d . . . H10 H 0.7041 1.2037 0.5669 0.118 Uiso 1 1 calc R . . C11 C 0.66465(18) 1.1751(6) 0.6157(2) 0.0817(18) Uani 1 1 d . . . H11 H 0.6580 1.0977 0.6046 0.098 Uiso 1 1 calc R . . C12 C 0.64802(15) 1.2283(5) 0.6528(2) 0.0631(14) Uani 1 1 d . . . C13 C 0.69094(13) 0.7521(4) 0.7077(2) 0.0523(12) Uani 1 1 d . . . C14 C 0.69550(16) 0.7708(5) 0.6549(2) 0.0681(15) Uani 1 1 d . . . H14 H 0.6765 0.8126 0.6289 0.082 Uiso 1 1 calc R . . C15 C 0.72711(17) 0.7298(6) 0.6397(3) 0.0792(18) Uani 1 1 d . . . H15 H 0.7300 0.7431 0.6034 0.095 Uiso 1 1 calc R . . C16 C 0.75455(19) 0.6690(7) 0.6780(3) 0.100(2) Uani 1 1 d . . . H16 H 0.7764 0.6402 0.6679 0.120 Uiso 1 1 calc R . . C17 C 0.75033(15) 0.6497(6) 0.7310(3) 0.0786(17) Uani 1 1 d . . . H17 H 0.7694 0.6082 0.7570 0.094 Uiso 1 1 calc R . . C18 C 0.71765(14) 0.6916(4) 0.7469(2) 0.0576(13) Uani 1 1 d . . . C19 C 0.71114(15) 0.6631(5) 0.8027(2) 0.0674(15) Uani 1 1 d . . . C20 C 0.71949(17) 0.5479(6) 0.8290(3) 0.090(2) Uani 1 1 d . . . H20 H 0.7297 0.4898 0.8100 0.108 Uiso 1 1 calc R . . C21 C 0.7134(2) 0.5215(8) 0.8785(3) 0.111(3) Uani 1 1 d . . . H21 H 0.7174 0.4449 0.8924 0.133 Uiso 1 1 calc R . . C22 C 0.7010(2) 0.6081(9) 0.9094(4) 0.121(3) Uani 1 1 d . . . H22 H 0.6986 0.5914 0.9455 0.145 Uiso 1 1 calc R . . C23 C 0.69219(18) 0.7208(7) 0.8868(3) 0.091(2) Uani 1 1 d . . . H23 H 0.6830 0.7784 0.9072 0.109 Uiso 1 1 calc R . . C24 C 0.69707(15) 0.7455(6) 0.8354(2) 0.0674(15) Uani 1 1 d . . . C25 C 0.53627(13) 0.8612(5) 0.69026(18) 0.0499(12) Uani 1 1 d . . . C26 C 0.52673(17) 0.7455(5) 0.6829(2) 0.0743(16) Uani 1 1 d . . . H26 H 0.5245 0.6997 0.7134 0.089 Uiso 1 1 calc R . . C27 C 0.53875(13) 1.0731(4) 1.14444(17) 0.0480(11) Uani 1 1 d . . . H27 H 0.5442 0.9929 1.1493 0.058 Uiso 1 1 calc R . . C28 C 0.52457(18) 1.2344(5) 1.0854(2) 0.0739(16) Uani 1 1 d . . . H28 H 0.5211 1.2674 1.0496 0.089 Uiso 1 1 calc R . . C29 C 0.52030(19) 0.6956(6) 0.6292(2) 0.0873(19) Uani 1 1 d . . . H29 H 0.5133 0.6166 0.6233 0.105 Uiso 1 1 calc R . . C30 C 0.57432(14) 0.9254(4) 0.87899(18) 0.0504(12) Uani 1 1 d . . . C31 C 0.56327(14) 0.9852(4) 0.92144(19) 0.0509(12) Uani 1 1 d . . . H31 H 0.5556 1.0637 0.9158 0.061 Uiso 1 1 calc R . . C32 C 0.57584(18) 0.8225(5) 0.9792(2) 0.0758(17) Uani 1 1 d . . . H32 H 0.5771 0.7853 1.0135 0.091 Uiso 1 1 calc R . . C33 C 0.5871(2) 0.7622(6) 0.9368(3) 0.096(2) Uani 1 1 d . . . H33 H 0.5955 0.6845 0.9431 0.116 Uiso 1 1 calc R . . C34 C 0.58615(18) 0.8130(5) 0.8864(2) 0.0754(17) Uani 1 1 d . . . H34 H 0.5935 0.7714 0.8580 0.090 Uiso 1 1 calc R . . Cl1 Cl 0.60332(4) 1.13055(15) 1.04423(7) 0.0829(5) Uani 1 1 d . . . Cl2 Cl 0.50928(4) 0.87139(11) 1.04659(5) 0.0552(3) Uani 1 1 d . . . Cu1 Cu 0.547705(18) 1.02539(6) 1.03123(2) 0.0547(2) Uani 1 1 d . . . N1 N 0.66109(11) 1.0125(3) 0.74257(18) 0.0546(10) Uani 1 1 d . . . N2 N 0.61483(10) 0.8656(3) 0.78035(15) 0.0491(9) Uani 1 1 d . . . N3 N 0.58926(11) 1.0836(3) 0.74492(16) 0.0526(10) Uani 1 1 d . . . N4 N 0.53364(12) 1.1198(4) 1.09277(16) 0.0550(10) Uani 1 1 d . . . N5 N 0.56333(12) 0.9324(4) 0.97127(16) 0.0581(11) Uani 1 1 d . . . O1 O 0.65073(10) 1.2173(3) 0.77060(14) 0.0605(9) Uani 1 1 d . . . O2 O 0.61948(9) 1.1649(3) 0.67168(12) 0.0583(9) Uani 1 1 d . . . O3 O 0.65536(8) 0.7877(3) 0.71946(12) 0.0505(8) Uani 1 1 d . . . O4 O 0.69069(9) 0.8608(3) 0.81396(13) 0.0583(9) Uani 1 1 d . . . O5 O 0.54139(8) 0.9092(3) 0.74320(12) 0.0540(8) Uani 1 1 d . . . O6 O 0.57304(10) 0.9966(3) 0.83200(13) 0.0632(10) Uani 1 1 d . . . P1 P 0.62977(4) 1.11305(11) 0.73353(5) 0.0502(3) Uani 1 1 d . . . P2 P 0.65421(4) 0.88677(11) 0.76352(5) 0.0487(3) Uani 1 1 d . . . P3 P 0.58259(4) 0.96348(12) 0.77412(5) 0.0486(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.066(3) 0.047(3) 0.068(3) -0.005(3) 0.012(3) -0.001(3) C2 0.101(5) 0.063(4) 0.084(4) -0.011(3) 0.025(4) -0.005(4) C3 0.104(5) 0.076(5) 0.110(6) -0.013(4) 0.050(4) 0.012(4) C4 0.080(5) 0.055(4) 0.175(8) -0.009(5) 0.033(5) 0.001(4) C5 0.081(4) 0.060(4) 0.124(6) 0.010(4) 0.039(4) -0.002(3) C6 0.060(3) 0.043(3) 0.099(5) 0.007(3) 0.019(3) 0.003(3) C7 0.069(4) 0.053(3) 0.073(4) 0.012(3) 0.023(3) 0.000(3) C8 0.095(5) 0.076(4) 0.104(5) 0.013(4) 0.044(4) -0.007(4) C9 0.096(5) 0.111(6) 0.138(7) 0.035(6) 0.054(5) -0.012(5) C10 0.106(5) 0.096(6) 0.112(6) 0.003(4) 0.062(5) -0.003(5) C11 0.088(4) 0.092(5) 0.073(4) -0.007(3) 0.035(3) -0.002(4) C12 0.061(3) 0.072(4) 0.063(3) 0.007(3) 0.027(3) -0.001(3) C13 0.045(3) 0.052(3) 0.060(3) -0.003(2) 0.013(2) 0.006(2) C14 0.058(3) 0.089(4) 0.056(3) 0.003(3) 0.013(3) -0.003(3) C15 0.063(4) 0.116(5) 0.068(4) 0.008(4) 0.034(3) 0.011(4) C16 0.057(4) 0.149(7) 0.105(6) -0.027(5) 0.041(4) -0.001(4) C17 0.045(3) 0.099(5) 0.089(5) -0.008(4) 0.013(3) 0.022(3) C18 0.053(3) 0.057(3) 0.065(3) -0.002(3) 0.017(3) 0.008(3) C19 0.050(3) 0.074(4) 0.076(4) 0.001(3) 0.012(3) 0.010(3) C20 0.079(4) 0.074(4) 0.105(5) 0.022(4) 0.000(4) 0.026(4) C21 0.139(7) 0.107(6) 0.086(5) 0.053(5) 0.025(5) 0.035(5) C22 0.119(6) 0.144(8) 0.095(6) 0.067(6) 0.019(5) 0.023(6) C23 0.082(4) 0.116(6) 0.072(4) 0.009(4) 0.017(3) 0.015(4) C24 0.054(3) 0.092(4) 0.052(3) 0.007(3) 0.007(3) 0.013(3) C25 0.055(3) 0.064(3) 0.031(2) 0.007(2) 0.012(2) -0.008(3) C26 0.094(4) 0.080(4) 0.049(3) 0.020(3) 0.018(3) -0.012(4) C27 0.056(3) 0.055(3) 0.035(2) 0.002(2) 0.014(2) -0.004(2) C28 0.110(5) 0.069(4) 0.043(3) -0.003(3) 0.018(3) 0.003(4) C29 0.128(5) 0.072(4) 0.060(4) 0.005(3) 0.021(4) -0.017(4) C30 0.056(3) 0.061(3) 0.039(3) 0.000(2) 0.020(2) 0.006(3) C31 0.059(3) 0.055(3) 0.040(3) -0.003(2) 0.015(2) 0.003(2) C32 0.108(5) 0.069(4) 0.063(4) 0.025(3) 0.043(3) 0.026(4) C33 0.151(6) 0.066(4) 0.095(5) 0.029(4) 0.074(5) 0.043(4) C34 0.112(5) 0.054(3) 0.075(4) 0.006(3) 0.051(4) 0.018(3) Cl1 0.0758(10) 0.0914(11) 0.0827(10) -0.0126(8) 0.0224(8) -0.0182(9) Cl2 0.0739(8) 0.0551(7) 0.0402(6) 0.0038(5) 0.0208(6) 0.0000(6) Cu1 0.0684(4) 0.0621(4) 0.0367(3) -0.0021(3) 0.0190(3) -0.0042(3) N1 0.048(2) 0.045(2) 0.074(3) -0.004(2) 0.022(2) 0.0014(19) N2 0.053(2) 0.048(2) 0.049(2) 0.0020(18) 0.0182(18) 0.0012(19) N3 0.047(2) 0.059(3) 0.053(2) 0.0090(19) 0.0151(18) 0.009(2) N4 0.071(3) 0.052(3) 0.043(2) -0.0039(19) 0.0160(19) -0.005(2) N5 0.069(3) 0.069(3) 0.042(2) 0.001(2) 0.024(2) -0.004(2) O1 0.068(2) 0.053(2) 0.057(2) -0.0035(16) 0.0099(17) -0.0019(18) O2 0.066(2) 0.065(2) 0.0452(18) 0.0055(16) 0.0173(16) -0.0121(18) O3 0.0422(17) 0.053(2) 0.0538(19) -0.0001(15) 0.0078(14) 0.0145(15) O4 0.0517(19) 0.060(2) 0.060(2) 0.0008(17) 0.0096(16) 0.0081(17) O5 0.0453(18) 0.084(2) 0.0357(17) 0.0045(16) 0.0163(14) -0.0032(17) O6 0.084(2) 0.072(2) 0.0379(18) 0.0045(16) 0.0229(17) 0.0217(19) P1 0.0541(8) 0.0493(8) 0.0469(7) 0.0004(6) 0.0126(6) 0.0013(6) P2 0.0450(7) 0.0543(8) 0.0470(7) 0.0003(6) 0.0120(5) 0.0051(6) P3 0.0507(7) 0.0622(8) 0.0348(6) 0.0027(6) 0.0145(5) 0.0087(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.431(8) . ? C1 C6 1.338(7) . ? C1 O1 1.404(6) . ? C2 H2 0.9300 . ? C2 C3 1.374(8) . ? C3 H3 0.9300 . ? C3 C4 1.403(10) . ? C4 H4 0.9300 . ? C4 C5 1.334(9) . ? C5 H5 0.9300 . ? C5 C6 1.376(8) . ? C6 C7 1.504(8) . ? C7 C8 1.373(8) . ? C7 C12 1.384(7) . ? C8 H8 0.9300 . ? C8 C9 1.418(10) . ? C9 H9 0.9300 . ? C9 C10 1.363(10) . ? C10 H10 0.9300 . ? C10 C11 1.436(8) . ? C11 H11 0.9300 . ? C11 C12 1.344(7) . ? C12 O2 1.412(6) . ? C13 C14 1.358(7) . ? C13 C18 1.350(6) . ? C13 O3 1.422(5) . ? C14 H14 0.9300 . ? C14 C15 1.351(7) . ? C15 H15 0.9300 . ? C15 C16 1.355(9) . ? C16 H16 0.9300 . ? C16 C17 1.361(8) . ? C17 H17 0.9300 . ? C17 C18 1.396(7) . ? C18 C19 1.478(7) . ? C19 C20 1.453(8) . ? C19 C24 1.401(7) . ? C20 H20 0.9300 . ? C20 C21 1.316(9) . ? C21 H21 0.9300 . ? C21 C22 1.377(11) . ? C22 H22 0.9300 . ? C22 C23 1.395(10) . ? C23 H23 0.9300 . ? C23 C24 1.342(8) . ? C24 O4 1.405(7) . ? C25 C26 1.354(7) . ? C25 C27 1.367(6) 6_575 ? C25 O5 1.374(5) . ? C26 H26 0.9300 . ? C26 C29 1.394(8) . ? C27 C25 1.367(6) 6_576 ? C27 H27 0.9300 . ? C27 N4 1.340(5) . ? C28 H28 0.9300 . ? C28 C29 1.374(7) 6_576 ? C28 N4 1.338(6) . ? C29 C28 1.374(7) 6_575 ? C29 H29 0.9300 . ? C30 C31 1.378(6) . ? C30 C34 1.339(7) . ? C30 O6 1.396(5) . ? C31 H31 0.9300 . ? C31 N5 1.357(6) . ? C32 H32 0.9300 . ? C32 C33 1.382(8) . ? C32 N5 1.320(6) . ? C33 H33 0.9300 . ? C33 C34 1.353(7) . ? C34 H34 0.9300 . ? Cl1 Cu1 2.2569(16) . ? Cl2 Cu1 2.6683(13) 5_677 ? Cl2 Cu1 2.3031(14) . ? Cu1 Cl2 2.6683(13) 5_677 ? Cu1 N4 2.011(4) . ? Cu1 N5 1.996(4) . ? N1 P1 1.567(4) . ? N1 P2 1.555(4) . ? N2 P2 1.572(4) . ? N2 P3 1.572(4) . ? N3 P1 1.568(4) . ? N3 P3 1.583(4) . ? O1 P1 1.558(3) . ? O2 P1 1.577(3) . ? O3 P2 1.564(3) . ? O4 P2 1.572(3) . ? O5 P3 1.589(3) . ? O6 P3 1.583(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 123.1(5) . . ? C6 C1 O1 120.8(5) . . ? O1 C1 C2 115.9(5) . . ? C1 C2 H2 121.3 . . ? C3 C2 C1 117.4(6) . . ? C3 C2 H2 121.3 . . ? C2 C3 H3 120.8 . . ? C2 C3 C4 118.4(6) . . ? C4 C3 H3 120.8 . . ? C3 C4 H4 119.2 . . ? C5 C4 C3 121.6(7) . . ? C5 C4 H4 119.2 . . ? C4 C5 H5 119.0 . . ? C4 C5 C6 122.0(7) . . ? C6 C5 H5 119.0 . . ? C1 C6 C5 117.5(6) . . ? C1 C6 C7 121.2(5) . . ? C5 C6 C7 121.3(6) . . ? C8 C7 C6 119.9(5) . . ? C8 C7 C12 118.7(6) . . ? C12 C7 C6 121.3(5) . . ? C7 C8 H8 120.9 . . ? C7 C8 C9 118.2(6) . . ? C9 C8 H8 120.9 . . ? C8 C9 H9 118.1 . . ? C10 C9 C8 123.7(6) . . ? C10 C9 H9 118.1 . . ? C9 C10 H10 122.0 . . ? C9 C10 C11 116.0(7) . . ? C11 C10 H10 122.0 . . ? C10 C11 H11 120.0 . . ? C12 C11 C10 120.1(6) . . ? C12 C11 H11 120.0 . . ? C7 C12 O2 118.8(5) . . ? C11 C12 C7 123.3(5) . . ? C11 C12 O2 117.8(5) . . ? C14 C13 O3 118.3(4) . . ? C18 C13 C14 121.5(5) . . ? C18 C13 O3 119.9(4) . . ? C13 C14 H14 119.4 . . ? C15 C14 C13 121.1(5) . . ? C15 C14 H14 119.4 . . ? C14 C15 H15 120.5 . . ? C14 C15 C16 118.9(6) . . ? C16 C15 H15 120.5 . . ? C15 C16 H16 119.8 . . ? C15 C16 C17 120.5(6) . . ? C17 C16 H16 119.8 . . ? C16 C17 H17 119.6 . . ? C16 C17 C18 120.7(6) . . ? C18 C17 H17 119.6 . . ? C13 C18 C17 117.3(5) . . ? C13 C18 C19 121.4(5) . . ? C17 C18 C19 121.2(5) . . ? C20 C19 C18 123.0(5) . . ? C24 C19 C18 122.9(5) . . ? C24 C19 C20 114.0(6) . . ? C19 C20 H20 118.3 . . ? C21 C20 C19 123.3(7) . . ? C21 C20 H20 118.3 . . ? C20 C21 H21 120.2 . . ? C20 C21 C22 119.5(7) . . ? C22 C21 H21 120.2 . . ? C21 C22 H22 119.8 . . ? C21 C22 C23 120.3(7) . . ? C23 C22 H22 119.8 . . ? C22 C23 H23 120.2 . . ? C24 C23 C22 119.5(7) . . ? C24 C23 H23 120.2 . . ? C19 C24 O4 117.0(5) . . ? C23 C24 C19 123.1(6) . . ? C23 C24 O4 119.8(6) . . ? C26 C25 C27 118.9(4) . 6_575 ? C26 C25 O5 118.5(4) . . ? C27 C25 O5 122.5(4) 6_575 . ? C25 C26 H26 120.2 . . ? C25 C26 C29 119.6(5) . . ? C29 C26 H26 120.2 . . ? C25 C27 H27 118.8 6_576 . ? N4 C27 C25 122.5(5) . 6_576 ? N4 C27 H27 118.8 . . ? C29 C28 H28 119.1 6_576 . ? N4 C28 H28 119.1 . . ? N4 C28 C29 121.7(5) . 6_576 ? C26 C29 H29 120.8 . . ? C28 C29 C26 118.4(6) 6_575 . ? C28 C29 H29 120.8 6_575 . ? C31 C30 O6 112.4(4) . . ? C34 C30 C31 120.3(5) . . ? C34 C30 O6 127.2(4) . . ? C30 C31 H31 119.2 . . ? N5 C31 C30 121.6(5) . . ? N5 C31 H31 119.2 . . ? C33 C32 H32 119.8 . . ? N5 C32 H32 119.8 . . ? N5 C32 C33 120.4(5) . . ? C32 C33 H33 119.0 . . ? C34 C33 C32 121.9(5) . . ? C34 C33 H33 119.0 . . ? C30 C34 C33 117.6(5) . . ? C30 C34 H34 121.2 . . ? C33 C34 H34 121.2 . . ? Cu1 Cl2 Cu1 85.63(4) . 5_677 ? Cl1 Cu1 Cl2 155.42(6) . . ? Cl1 Cu1 Cl2 110.21(6) . 5_677 ? Cl2 Cu1 Cl2 94.37(4) . 5_677 ? N4 Cu1 Cl1 89.32(12) . . ? N4 Cu1 Cl2 90.79(12) . 5_677 ? N4 Cu1 Cl2 90.63(12) . . ? N5 Cu1 Cl1 89.20(13) . . ? N5 Cu1 Cl2 90.49(13) . 5_677 ? N5 Cu1 Cl2 90.38(13) . . ? N5 Cu1 N4 178.31(17) . . ? P2 N1 P1 123.2(3) . . ? P2 N2 P3 122.7(2) . . ? P1 N3 P3 120.8(2) . . ? C27 N4 Cu1 119.8(3) . . ? C28 N4 C27 118.7(4) . . ? C28 N4 Cu1 120.8(3) . . ? C31 N5 Cu1 119.4(3) . . ? C32 N5 C31 118.1(4) . . ? C32 N5 Cu1 122.4(3) . . ? C1 O1 P1 120.1(3) . . ? C12 O2 P1 119.6(3) . . ? C13 O3 P2 121.6(3) . . ? C24 O4 P2 119.3(3) . . ? C25 O5 P3 119.2(3) . . ? C30 O6 P3 129.1(3) . . ? N1 P1 N3 118.0(2) . . ? N1 P1 O2 112.9(2) . . ? N3 P1 O2 104.54(19) . . ? O1 P1 N1 104.6(2) . . ? O1 P1 N3 112.4(2) . . ? O1 P1 O2 103.65(19) . . ? N1 P2 N2 116.8(2) . . ? N1 P2 O3 113.4(2) . . ? N1 P2 O4 105.3(2) . . ? N2 P2 O4 111.99(19) . . ? O3 P2 N2 104.60(19) . . ? O3 P2 O4 104.25(17) . . ? N2 P3 N3 117.5(2) . . ? N2 P3 O5 109.3(2) . . ? N2 P3 O6 113.36(19) . . ? N3 P3 O5 110.08(19) . . ? N3 P3 O6 106.9(2) . . ? O6 P3 O5 97.90(18) . . ? 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 C1 C2 C3 C4 2.6(10) . . . . ? C1 C6 C7 C8 -133.9(6) . . . . ? C1 C6 C7 C12 42.0(8) . . . . ? C1 O1 P1 N1 162.4(4) . . . . ? C1 O1 P1 N3 -68.4(4) . . . . ? C1 O1 P1 O2 43.9(4) . . . . ? C2 C1 C6 C5 -0.6(9) . . . . ? C2 C1 C6 C7 179.7(5) . . . . ? C2 C1 O1 P1 110.2(5) . . . . ? C2 C3 C4 C5 -2.6(11) . . . . ? C3 C4 C5 C6 0.9(11) . . . . ? C4 C5 C6 C1 0.7(9) . . . . ? C4 C5 C6 C7 -179.6(6) . . . . ? C5 C6 C7 C8 46.5(8) . . . . ? C5 C6 C7 C12 -137.6(6) . . . . ? C6 C1 C2 C3 -1.1(9) . . . . ? C6 C1 O1 P1 -74.9(6) . . . . ? C6 C7 C8 C9 178.9(6) . . . . ? C6 C7 C12 C11 -176.4(5) . . . . ? C6 C7 C12 O2 4.3(8) . . . . ? C7 C8 C9 C10 -3.3(11) . . . . ? C7 C12 O2 P1 -74.3(6) . . . . ? C8 C7 C12 C11 -0.4(9) . . . . ? C8 C7 C12 O2 -179.8(5) . . . . ? C8 C9 C10 C11 0.9(12) . . . . ? C9 C10 C11 C12 1.7(10) . . . . ? C10 C11 C12 C7 -2.0(9) . . . . ? C10 C11 C12 O2 177.4(5) . . . . ? C11 C12 O2 P1 106.3(5) . . . . ? C12 C7 C8 C9 3.0(9) . . . . ? C12 O2 P1 N1 -66.7(4) . . . . ? C12 O2 P1 N3 163.9(4) . . . . ? C12 O2 P1 O1 46.0(4) . . . . ? C13 C14 C15 C16 0.0(10) . . . . ? C13 C18 C19 C20 135.9(6) . . . . ? C13 C18 C19 C24 -45.3(8) . . . . ? C13 O3 P2 N1 72.5(4) . . . . ? C13 O3 P2 N2 -159.2(3) . . . . ? C13 O3 P2 O4 -41.5(4) . . . . ? C14 C13 C18 C17 0.4(8) . . . . ? C14 C13 C18 C19 -175.0(5) . . . . ? C14 C13 O3 P2 -115.7(4) . . . . ? C14 C15 C16 C17 -0.1(11) . . . . ? C15 C16 C17 C18 0.3(11) . . . . ? C16 C17 C18 C13 -0.5(9) . . . . ? C16 C17 C18 C19 175.0(6) . . . . ? C17 C18 C19 C20 -39.3(8) . . . . ? C17 C18 C19 C24 139.4(6) . . . . ? C18 C13 C14 C15 -0.2(9) . . . . ? C18 C13 O3 P2 70.2(5) . . . . ? C18 C19 C20 C21 -179.2(7) . . . . ? C18 C19 C24 C23 -178.0(5) . . . . ? C18 C19 C24 O4 -2.7(8) . . . . ? C19 C20 C21 C22 -4.7(12) . . . . ? C19 C24 O4 P2 74.8(5) . . . . ? C20 C19 C24 C23 0.8(8) . . . . ? C20 C19 C24 O4 176.2(5) . . . . ? C20 C21 C22 C23 4.9(13) . . . . ? C21 C22 C23 C24 -2.2(12) . . . . ? C22 C23 C24 C19 -0.6(10) . . . . ? C22 C23 C24 O4 -175.8(6) . . . . ? C23 C24 O4 P2 -109.7(5) . . . . ? C24 C19 C20 C21 1.9(9) . . . . ? C24 O4 P2 N1 -168.0(4) . . . . ? C24 O4 P2 N2 64.1(4) . . . . ? C24 O4 P2 O3 -48.4(4) . . . . ? C25 C26 C29 C28 1.1(9) . . . 6_575 ? C25 C27 N4 C28 -2.1(7) 6_576 . . . ? C25 C27 N4 Cu1 168.4(4) 6_576 . . . ? C25 O5 P3 N2 -58.5(4) . . . . ? C25 O5 P3 N3 72.0(4) . . . . ? C25 O5 P3 O6 -176.7(3) . . . . ? C26 C25 O5 P3 119.2(5) . . . . ? C27 C25 C26 C29 1.1(8) 6_575 . . . ? C27 C25 O5 P3 -63.8(6) 6_575 . . . ? C29 C28 N4 C27 -0.2(8) 6_576 . . . ? C29 C28 N4 Cu1 -170.6(5) 6_576 . . . ? C30 C31 N5 C32 2.7(7) . . . . ? C30 C31 N5 Cu1 179.1(4) . . . . ? C30 O6 P3 N2 -31.4(5) . . . . ? C30 O6 P3 N3 -162.5(4) . . . . ? C30 O6 P3 O5 83.7(4) . . . . ? C31 C30 C34 C33 -0.6(9) . . . . ? C31 C30 O6 P3 -178.9(3) . . . . ? C32 C33 C34 C30 0.8(11) . . . . ? C33 C32 N5 C31 -2.4(9) . . . . ? C33 C32 N5 Cu1 -178.7(5) . . . . ? C34 C30 C31 N5 -1.1(8) . . . . ? C34 C30 O6 P3 3.9(8) . . . . ? Cl1 Cu1 N4 C27 -101.8(3) . . . . ? Cl1 Cu1 N4 C28 68.4(4) . . . . ? Cl1 Cu1 N5 C31 -70.0(4) . . . . ? Cl1 Cu1 N5 C32 106.2(4) . . . . ? Cl2 Cu1 N4 C27 148.0(3) 5_677 . . . ? Cl2 Cu1 N4 C27 53.6(3) . . . . ? Cl2 Cu1 N4 C28 -41.8(4) 5_677 . . . ? Cl2 Cu1 N4 C28 -136.1(4) . . . . ? Cl2 Cu1 N5 C31 40.2(4) 5_677 . . . ? Cl2 Cu1 N5 C31 134.6(4) . . . . ? Cl2 Cu1 N5 C32 -49.2(4) . . . . ? Cl2 Cu1 N5 C32 -143.6(4) 5_677 . . . ? Cu1 Cl2 Cu1 Cl1 -179.41(13) 5_677 . . . ? Cu1 Cl2 Cu1 Cl2 0.0 5_677 . . 5_677 ? Cu1 Cl2 Cu1 N4 90.84(12) 5_677 . . . ? Cu1 Cl2 Cu1 N5 -90.52(13) 5_677 . . . ? N4 Cu1 N5 C31 -99(6) . . . . ? N4 Cu1 N5 C32 77(6) . . . . ? N5 C32 C33 C34 0.7(11) . . . . ? N5 Cu1 N4 C27 -73(6) . . . . ? N5 Cu1 N4 C28 97(6) . . . . ? O1 C1 C2 C3 173.7(5) . . . . ? O1 C1 C6 C5 -175.2(5) . . . . ? O1 C1 C6 C7 5.2(8) . . . . ? O3 C13 C14 C15 -174.2(5) . . . . ? O3 C13 C18 C17 174.3(5) . . . . ? O3 C13 C18 C19 -1.1(7) . . . . ? O5 C25 C26 C29 178.2(5) . . . . ? O6 C30 C31 N5 -178.6(4) . . . . ? O6 C30 C34 C33 176.4(6) . . . . ? P1 N1 P2 N2 -4.7(4) . . . . ? P1 N1 P2 O3 117.0(3) . . . . ? P1 N1 P2 O4 -129.7(3) . . . . ? P1 N3 P3 N2 -11.6(4) . . . . ? P1 N3 P3 O5 -137.6(3) . . . . ? P1 N3 P3 O6 117.1(3) . . . . ? P2 N1 P1 N3 -1.5(4) . . . . ? P2 N1 P1 O1 124.3(3) . . . . ? P2 N1 P1 O2 -123.7(3) . . . . ? P2 N2 P3 N3 5.2(4) . . . . ? P2 N2 P3 O5 131.5(3) . . . . ? P2 N2 P3 O6 -120.4(3) . . . . ? P3 N2 P2 N1 2.7(4) . . . . ? P3 N2 P2 O3 -123.5(3) . . . . ? P3 N2 P2 O4 124.2(3) . . . . ? P3 N3 P1 N1 9.9(4) . . . . ? P3 N3 P1 O1 -112.1(3) . . . . ? P3 N3 P1 O2 136.2(3) . . . . ? _platon_squeeze_details ; ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.186 0.308 0.402 3238 1091 ' ' 2 0.250 0.250 0.000 4 0 ' ' 3 0.750 0.250 0.500 4 0 ' ' 4 0.250 0.750 0.500 4 0 ' ' 5 0.750 0.750 0.000 4 0 ' ' data_908596 _database_code_depnum_ccdc_archive 'CCDC 908596' #TrackingRef '17696_web_deposit_cif_file_7_RSuriyaNarayanan_1360734625.908596.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H48 Cl2 Cu N10 O12 P6, 2(C3 H7 N O)' _chemical_formula_sum 'C74 H62 Cl2 Cu N12 O14 P6' _chemical_formula_weight 1663.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 11.299(4) _cell_length_b 21.076(8) _cell_length_c 15.289(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.992(7) _cell_angle_gamma 90.00 _cell_volume 3636(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2036 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 25.76 _exptl_crystal_description block _exptl_crystal_colour violet _exptl_crystal_size_max 0.069 _exptl_crystal_size_mid 0.047 _exptl_crystal_size_min 0.025 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1710 _exptl_absorpt_coefficient_mu 0.582 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.968 _exptl_absorpt_correction_T_max 0.986 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19021 _diffrn_reflns_av_R_equivalents 0.0976 _diffrn_reflns_av_unetI/netI 0.1204 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6756 _reflns_number_gt 3939 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0894P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6756 _refine_ls_number_parameters 495 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1171 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.1764 _refine_ls_wR_factor_gt 0.1461 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8806(4) 0.2056(2) 0.4038(3) 0.0215(11) Uani 1 1 d . . . C2 C 0.9274(4) 0.1965(2) 0.4873(3) 0.0267(12) Uani 1 1 d . . . H2 H 0.9361 0.2308 0.5275 0.032 Uiso 1 1 calc R . . C3 C 0.9611(4) 0.1362(2) 0.5108(3) 0.0247(11) Uani 1 1 d . . . H3 H 0.9969 0.1301 0.5678 0.030 Uiso 1 1 calc R . . C4 C 0.9006(4) 0.0962(2) 0.3790(4) 0.0265(12) Uani 1 1 d . . . H4 H 0.8899 0.0609 0.3408 0.032 Uiso 1 1 calc R . . C5 C 0.8671(4) 0.1549(2) 0.3481(3) 0.0236(11) Uani 1 1 d . . . H5 H 0.8355 0.1603 0.2897 0.028 Uiso 1 1 calc R . . C6 C 0.8348(4) 0.4026(2) 0.2877(3) 0.0227(11) Uani 1 1 d . . . C7 C 0.7615(4) 0.4265(2) 0.2205(3) 0.0254(12) Uani 1 1 d . . . H7 H 0.6782 0.4203 0.2203 0.030 Uiso 1 1 calc R . . C8 C 0.8105(4) 0.4589(2) 0.1549(3) 0.0280(12) Uani 1 1 d . . . H8 H 0.7592 0.4752 0.1091 0.034 Uiso 1 1 calc R . . C9 C 0.9973(4) 0.4459(2) 0.2168(3) 0.0250(12) Uani 1 1 d . . . H9 H 1.0803 0.4528 0.2156 0.030 Uiso 1 1 calc R . . C10 C 0.9562(4) 0.4125(2) 0.2862(3) 0.0260(12) Uani 1 1 d . . . H10 H 1.0089 0.3967 0.3316 0.031 Uiso 1 1 calc R . . C11 C 1.1403(4) 0.4429(2) 0.5949(3) 0.0215(11) Uani 1 1 d . . . C12 C 1.1762(4) 0.4836(2) 0.5317(3) 0.0263(12) Uani 1 1 d . . . H12 H 1.1211 0.4989 0.4875 0.032 Uiso 1 1 calc R . . C13 C 1.2942(4) 0.5023(2) 0.5330(4) 0.0288(12) Uani 1 1 d . . . H13 H 1.3209 0.5299 0.4891 0.035 Uiso 1 1 calc R . . C14 C 1.3725(4) 0.4803(2) 0.5987(4) 0.0296(13) Uani 1 1 d . . . H14 H 1.4528 0.4938 0.6007 0.036 Uiso 1 1 calc R . . C15 C 1.3352(4) 0.4394(2) 0.6607(4) 0.0265(12) Uani 1 1 d . . . H15 H 1.3902 0.4248 0.7053 0.032 Uiso 1 1 calc R . . C16 C 1.2159(4) 0.4183(2) 0.6598(3) 0.0241(11) Uani 1 1 d . . . C17 C 1.1813(4) 0.3703(2) 0.7228(3) 0.0238(11) Uani 1 1 d . . . C18 C 1.2181(4) 0.3711(2) 0.8103(3) 0.0247(12) Uani 1 1 d . . . H18 H 1.2617 0.4065 0.8331 0.030 Uiso 1 1 calc R . . C19 C 1.1933(4) 0.3219(2) 0.8653(3) 0.0294(12) Uani 1 1 d . . . H19 H 1.2195 0.3238 0.9253 0.035 Uiso 1 1 calc R . . C20 C 1.1301(4) 0.2696(2) 0.8336(3) 0.0270(12) Uani 1 1 d . . . H20 H 1.1142 0.2353 0.8716 0.032 Uiso 1 1 calc R . . C21 C 1.0906(4) 0.2676(2) 0.7472(3) 0.0268(12) Uani 1 1 d . . . H21 H 1.0469 0.2321 0.7251 0.032 Uiso 1 1 calc R . . C22 C 1.1149(4) 0.3176(2) 0.6929(3) 0.0219(11) Uani 1 1 d . . . C23 C 0.6086(4) 0.3771(2) 0.7008(3) 0.0241(11) Uani 1 1 d . . . C24 C 0.6371(4) 0.4350(3) 0.7383(4) 0.0289(12) Uani 1 1 d . . . H24 H 0.6759 0.4667 0.7062 0.035 Uiso 1 1 calc R . . C25 C 0.6082(4) 0.4458(3) 0.8227(4) 0.0349(14) Uani 1 1 d . . . H25 H 0.6262 0.4854 0.8499 0.042 Uiso 1 1 calc R . . C26 C 0.5525(4) 0.3987(3) 0.8685(4) 0.0370(14) Uani 1 1 d . . . H26 H 0.5328 0.4062 0.9272 0.044 Uiso 1 1 calc R . . C27 C 0.5255(4) 0.3412(3) 0.8300(3) 0.0315(13) Uani 1 1 d . . . H27 H 0.4875 0.3094 0.8627 0.038 Uiso 1 1 calc R . . C28 C 0.5527(4) 0.3287(2) 0.7440(3) 0.0244(11) Uani 1 1 d . . . C29 C 0.5197(4) 0.2692(2) 0.6997(3) 0.0264(12) Uani 1 1 d . . . C30 C 0.4075(4) 0.2416(3) 0.7067(4) 0.0304(13) Uani 1 1 d . . . H30 H 0.3517 0.2615 0.7423 0.036 Uiso 1 1 calc R . . C31 C 0.3768(5) 0.1865(3) 0.6632(4) 0.0384(14) Uani 1 1 d . . . H31 H 0.3010 0.1683 0.6702 0.046 Uiso 1 1 calc R . . C32 C 0.4540(5) 0.1577(3) 0.6100(4) 0.0378(14) Uani 1 1 d . . . H32 H 0.4309 0.1202 0.5791 0.045 Uiso 1 1 calc R . . C33 C 0.5666(4) 0.1831(2) 0.6008(3) 0.0299(12) Uani 1 1 d . . . H33 H 0.6215 0.1633 0.5646 0.036 Uiso 1 1 calc R . . C34 C 0.5952(4) 0.2375(2) 0.6457(3) 0.0244(12) Uani 1 1 d . . . C35 C 0.4750(4) 0.1314(3) 0.8777(4) 0.0390(15) Uani 1 1 d . . . H35A H 0.4636 0.1025 0.8277 0.058 Uiso 1 1 calc R . . H35B H 0.5265 0.1111 0.9232 0.058 Uiso 1 1 calc R . . H35C H 0.5120 0.1707 0.8586 0.058 Uiso 1 1 calc R . . C36 C 0.3604(5) 0.1873(3) 0.9869(4) 0.0396(14) Uani 1 1 d . . . H36A H 0.2792 0.1918 1.0056 0.059 Uiso 1 1 calc R . . H36B H 0.3909 0.2290 0.9708 0.059 Uiso 1 1 calc R . . H36C H 0.4107 0.1696 1.0350 0.059 Uiso 1 1 calc R . . C37 C 0.2615(4) 0.1160(3) 0.8815(4) 0.0309(13) Uani 1 1 d . . . H37 H 0.1901 0.1259 0.9087 0.037 Uiso 1 1 calc R . . Cl1 Cl 1.18746(11) 0.04269(6) 0.53909(9) 0.0332(3) Uani 1 1 d . . . Cu1 Cu 1.0000 0.0000 0.5000 0.0304(3) Uani 1 2 d S . . N1 N 0.9518(3) 0.34915(18) 0.4710(3) 0.0206(9) Uani 1 1 d . . . N2 N 0.8592(3) 0.35045(19) 0.6289(3) 0.0221(9) Uani 1 1 d . . . N3 N 0.7247(3) 0.31274(18) 0.4883(3) 0.0216(9) Uani 1 1 d . . . N4 N 0.9472(3) 0.08576(18) 0.4597(3) 0.0259(10) Uani 1 1 d . . . N5 N 0.9285(4) 0.46947(19) 0.1509(3) 0.0275(10) Uani 1 1 d . . . N6 N 0.3611(4) 0.1457(2) 0.9127(3) 0.0297(10) Uani 1 1 d . . . O1 O 0.8510(3) 0.26493(15) 0.3693(2) 0.0235(8) Uani 1 1 d . . . O2 O 0.7801(3) 0.37148(15) 0.3536(2) 0.0219(8) Uani 1 1 d . . . O3 O 1.0184(3) 0.42830(15) 0.5959(2) 0.0233(8) Uani 1 1 d . . . O4 O 1.0757(2) 0.31465(14) 0.6047(2) 0.0177(7) Uani 1 1 d . . . O5 O 0.6307(2) 0.36860(15) 0.6119(2) 0.0232(8) Uani 1 1 d . . . O6 O 0.7124(3) 0.26134(15) 0.6417(2) 0.0240(8) Uani 1 1 d . . . O7 O 0.2551(3) 0.07819(18) 0.8225(3) 0.0406(10) Uani 1 1 d . . . P1 P 0.82998(10) 0.32563(6) 0.42727(9) 0.0209(3) Uani 1 1 d . . . P2 P 0.96940(10) 0.35987(6) 0.57272(9) 0.0211(3) Uani 1 1 d . . . P3 P 0.73708(10) 0.32368(6) 0.58899(9) 0.0224(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.010(2) 0.025(3) 0.029(3) 0.004(2) 0.000(2) 0.0025(19) C2 0.021(3) 0.029(3) 0.031(3) -0.002(2) -0.003(2) 0.002(2) C3 0.024(3) 0.028(3) 0.021(3) -0.003(2) -0.005(2) 0.003(2) C4 0.014(3) 0.032(3) 0.033(3) -0.007(2) 0.001(2) 0.000(2) C5 0.012(2) 0.034(3) 0.025(3) -0.003(2) -0.002(2) -0.001(2) C6 0.020(3) 0.024(3) 0.024(3) -0.001(2) 0.004(2) -0.002(2) C7 0.014(2) 0.032(3) 0.030(3) 0.002(2) -0.003(2) 0.001(2) C8 0.021(3) 0.032(3) 0.030(3) 0.008(2) -0.006(2) 0.003(2) C9 0.019(3) 0.027(3) 0.029(3) 0.004(2) -0.001(2) -0.003(2) C10 0.016(3) 0.032(3) 0.030(3) 0.006(2) -0.003(2) 0.000(2) C11 0.013(2) 0.024(3) 0.027(3) 0.002(2) -0.001(2) -0.001(2) C12 0.021(3) 0.027(3) 0.030(3) 0.006(2) -0.004(2) 0.004(2) C13 0.020(3) 0.028(3) 0.039(3) 0.008(2) 0.004(2) -0.003(2) C14 0.012(2) 0.026(3) 0.051(4) 0.000(3) -0.002(2) -0.003(2) C15 0.015(3) 0.030(3) 0.034(3) 0.002(2) -0.004(2) 0.001(2) C16 0.017(3) 0.025(3) 0.030(3) 0.002(2) -0.004(2) -0.001(2) C17 0.010(2) 0.025(3) 0.036(3) 0.002(2) 0.000(2) 0.004(2) C18 0.011(2) 0.036(3) 0.027(3) -0.001(2) -0.008(2) 0.003(2) C19 0.018(3) 0.043(3) 0.026(3) 0.005(3) -0.005(2) 0.005(2) C20 0.014(3) 0.037(3) 0.029(3) 0.008(2) 0.001(2) 0.006(2) C21 0.012(2) 0.031(3) 0.037(3) 0.006(2) 0.001(2) 0.002(2) C22 0.008(2) 0.032(3) 0.024(3) 0.002(2) -0.005(2) 0.004(2) C23 0.009(2) 0.039(3) 0.024(3) 0.001(2) -0.002(2) 0.007(2) C24 0.011(2) 0.038(3) 0.038(3) 0.003(3) -0.002(2) 0.005(2) C25 0.018(3) 0.045(3) 0.040(4) -0.005(3) -0.005(3) 0.002(2) C26 0.021(3) 0.056(4) 0.033(3) -0.006(3) 0.000(3) 0.004(3) C27 0.016(3) 0.051(4) 0.027(3) 0.006(3) -0.002(2) 0.002(2) C28 0.007(2) 0.037(3) 0.029(3) 0.002(2) 0.000(2) 0.003(2) C29 0.018(3) 0.037(3) 0.025(3) 0.005(2) 0.001(2) 0.000(2) C30 0.014(3) 0.037(3) 0.041(3) 0.007(3) 0.004(2) 0.002(2) C31 0.021(3) 0.048(4) 0.047(4) 0.014(3) 0.005(3) -0.009(3) C32 0.033(3) 0.039(3) 0.042(4) 0.002(3) 0.000(3) -0.007(3) C33 0.027(3) 0.031(3) 0.032(3) 0.007(2) 0.001(2) -0.003(2) C34 0.011(2) 0.031(3) 0.031(3) 0.010(2) 0.004(2) -0.001(2) C35 0.016(3) 0.042(3) 0.059(4) -0.005(3) -0.003(3) 0.002(2) C36 0.039(3) 0.040(3) 0.038(4) -0.003(3) -0.005(3) -0.006(3) C37 0.019(3) 0.035(3) 0.037(3) 0.007(3) -0.008(2) 0.000(2) Cl1 0.0246(7) 0.0371(8) 0.0372(8) -0.0046(6) -0.0065(6) 0.0014(5) Cu1 0.0226(5) 0.0272(5) 0.0400(6) -0.0041(4) -0.0119(4) 0.0046(4) N1 0.0061(19) 0.030(2) 0.026(2) -0.0031(18) -0.0021(17) -0.0010(16) N2 0.010(2) 0.034(2) 0.022(2) -0.0007(18) -0.0017(17) -0.0028(17) N3 0.0105(19) 0.027(2) 0.027(2) 0.0022(18) -0.0022(18) -0.0057(16) N4 0.017(2) 0.026(2) 0.034(3) -0.002(2) -0.004(2) 0.0042(17) N5 0.024(2) 0.031(2) 0.027(3) 0.005(2) -0.002(2) 0.0007(19) N6 0.020(2) 0.032(2) 0.036(3) 0.001(2) -0.005(2) -0.0007(19) O1 0.0190(17) 0.0278(19) 0.023(2) 0.0007(15) -0.0013(15) -0.0010(14) O2 0.0131(16) 0.0296(19) 0.0230(19) 0.0070(15) 0.0000(14) 0.0006(14) O3 0.0070(16) 0.0285(18) 0.034(2) -0.0023(15) -0.0044(15) 0.0007(13) O4 0.0092(15) 0.0253(18) 0.0181(18) -0.0004(14) -0.0024(13) 0.0018(13) O5 0.0098(16) 0.0312(19) 0.028(2) 0.0019(15) 0.0001(15) 0.0028(13) O6 0.0111(16) 0.0339(19) 0.027(2) 0.0070(15) 0.0012(15) 0.0014(14) O7 0.029(2) 0.047(2) 0.045(3) -0.007(2) -0.0094(19) -0.0033(18) P1 0.0122(6) 0.0265(7) 0.0238(7) 0.0032(6) -0.0006(5) -0.0005(5) P2 0.0100(6) 0.0270(7) 0.0259(8) 0.0006(6) -0.0015(5) 0.0009(5) P3 0.0101(6) 0.0317(7) 0.0253(8) 0.0021(6) -0.0002(5) 0.0011(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.369(7) . ? C1 C5 1.371(7) . ? C1 O1 1.391(5) . ? C2 C3 1.369(7) . ? C3 N4 1.324(6) . ? C4 N4 1.334(6) . ? C4 C5 1.370(7) . ? C6 O2 1.376(6) . ? C6 C7 1.381(7) . ? C6 C10 1.389(7) . ? C7 C8 1.356(7) . ? C8 N5 1.356(6) . ? C9 N5 1.335(6) . ? C9 C10 1.375(7) . ? C11 C12 1.370(7) . ? C11 C16 1.376(7) . ? C11 O3 1.411(5) . ? C12 C13 1.390(6) . ? C13 C14 1.383(7) . ? C14 C15 1.364(7) . ? C15 C16 1.419(6) . ? C16 C17 1.464(7) . ? C17 C18 1.381(7) . ? C17 C22 1.403(7) . ? C18 C19 1.372(7) . ? C19 C20 1.388(7) . ? C20 C21 1.373(7) . ? C21 C22 1.378(7) . ? C22 O4 1.398(6) . ? C23 C24 1.380(7) . ? C23 C28 1.385(7) . ? C23 O5 1.405(6) . ? C24 C25 1.366(7) . ? C25 C26 1.385(8) . ? C26 C27 1.374(7) . ? C27 C28 1.391(7) . ? C28 C29 1.464(7) . ? C29 C34 1.389(7) . ? C29 C30 1.404(6) . ? C30 C31 1.374(8) . ? C31 C32 1.367(8) . ? C32 C33 1.394(7) . ? C33 C34 1.366(7) . ? C34 O6 1.420(5) . ? C35 N6 1.452(6) . ? C36 N6 1.434(7) . ? C37 O7 1.204(6) . ? C37 N6 1.352(6) . ? Cl1 Cu1 2.3497(14) . ? Cu1 N4 1.991(4) . ? Cu1 N4 1.991(4) 3_756 ? Cu1 Cl1 2.3497(14) 3_756 ? N1 P2 1.574(4) . ? N1 P1 1.578(4) . ? N2 P2 1.562(4) . ? N2 P3 1.583(4) . ? N3 P3 1.556(4) . ? N3 P1 1.573(4) . ? O1 P1 1.581(3) . ? O2 P1 1.566(3) . ? O3 P2 1.578(3) . ? O4 P2 1.591(3) . ? O5 P3 1.584(3) . ? O6 P3 1.574(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 119.7(5) . . ? C2 C1 O1 123.6(4) . . ? C5 C1 O1 116.6(4) . . ? C1 C2 C3 117.6(5) . . ? N4 C3 C2 124.5(5) . . ? N4 C4 C5 123.8(5) . . ? C4 C5 C1 118.0(5) . . ? O2 C6 C7 116.3(4) . . ? O2 C6 C10 124.4(5) . . ? C7 C6 C10 119.2(5) . . ? C8 C7 C6 118.8(4) . . ? N5 C8 C7 123.8(5) . . ? N5 C9 C10 124.5(5) . . ? C9 C10 C6 117.6(5) . . ? C12 C11 C16 123.2(4) . . ? C12 C11 O3 117.9(4) . . ? C16 C11 O3 118.7(4) . . ? C11 C12 C13 119.1(5) . . ? C14 C13 C12 119.5(5) . . ? C15 C14 C13 120.5(5) . . ? C14 C15 C16 121.3(5) . . ? C11 C16 C15 116.3(4) . . ? C11 C16 C17 123.8(4) . . ? C15 C16 C17 119.8(4) . . ? C18 C17 C22 117.0(5) . . ? C18 C17 C16 123.5(5) . . ? C22 C17 C16 119.3(5) . . ? C19 C18 C17 121.6(5) . . ? C18 C19 C20 120.3(5) . . ? C21 C20 C19 119.7(5) . . ? C20 C21 C22 119.5(5) . . ? C21 C22 O4 119.0(4) . . ? C21 C22 C17 121.9(5) . . ? O4 C22 C17 119.1(4) . . ? C24 C23 C28 123.7(5) . . ? C24 C23 O5 117.7(4) . . ? C28 C23 O5 118.4(4) . . ? C25 C24 C23 118.5(5) . . ? C24 C25 C26 119.7(5) . . ? C27 C26 C25 120.9(5) . . ? C26 C27 C28 121.0(5) . . ? C23 C28 C27 116.2(5) . . ? C23 C28 C29 121.4(5) . . ? C27 C28 C29 122.4(5) . . ? C34 C29 C30 115.6(5) . . ? C34 C29 C28 122.5(4) . . ? C30 C29 C28 121.9(4) . . ? C31 C30 C29 121.3(5) . . ? C32 C31 C30 120.8(5) . . ? C31 C32 C33 120.1(5) . . ? C34 C33 C32 117.8(5) . . ? C33 C34 C29 124.4(4) . . ? C33 C34 O6 118.2(4) . . ? C29 C34 O6 117.3(4) . . ? O7 C37 N6 126.0(5) . . ? N4 Cu1 N4 180.00(9) . 3_756 ? N4 Cu1 Cl1 89.02(12) . . ? N4 Cu1 Cl1 90.99(12) 3_756 . ? N4 Cu1 Cl1 90.99(12) . 3_756 ? N4 Cu1 Cl1 89.01(12) 3_756 3_756 ? Cl1 Cu1 Cl1 180.0 . 3_756 ? P2 N1 P1 121.8(2) . . ? P2 N2 P3 122.5(3) . . ? P3 N3 P1 122.0(2) . . ? C3 N4 C4 116.3(4) . . ? C3 N4 Cu1 121.4(4) . . ? C4 N4 Cu1 122.2(3) . . ? C9 N5 C8 116.1(4) . . ? C37 N6 C36 121.6(5) . . ? C37 N6 C35 120.7(5) . . ? C36 N6 C35 117.4(4) . . ? C1 O1 P1 123.7(3) . . ? C6 O2 P1 131.4(3) . . ? C11 O3 P2 121.8(3) . . ? C22 O4 P2 117.8(3) . . ? C23 O5 P3 117.7(3) . . ? C34 O6 P3 120.5(3) . . ? O2 P1 N3 106.13(19) . . ? O2 P1 N1 112.6(2) . . ? N3 P1 N1 118.2(2) . . ? O2 P1 O1 98.92(18) . . ? N3 P1 O1 109.45(19) . . ? N1 P1 O1 109.79(19) . . ? N2 P2 N1 117.5(2) . . ? N2 P2 O3 105.9(2) . . ? N1 P2 O3 112.2(2) . . ? N2 P2 O4 111.47(19) . . ? N1 P2 O4 105.82(18) . . ? O3 P2 O4 103.17(17) . . ? N3 P3 O6 112.0(2) . . ? N3 P3 N2 117.8(2) . . ? O6 P3 N2 105.92(19) . . ? N3 P3 O5 106.1(2) . . ? O6 P3 O5 103.21(17) . . ? N2 P3 O5 111.0(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.076 _refine_diff_density_min -0.834 _refine_diff_density_rms 0.113 data_908597 _database_code_depnum_ccdc_archive 'CCDC 908597' #TrackingRef '17697_web_deposit_cif_file_8_RSuriyaNarayanan_1360734625.908597.cif' _audit_creation_date 2012-06-22 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '0.5(C136 H96 Cd2 N24 O36 P12), C H2 Cl2' _chemical_formula_sum 'C69 H50 Cd Cl2 N12 O18 P6' _chemical_formula_weight 1704.33 _chemical_melting_point ? 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' Cd Cd -0.8075 1.2024 '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' _space_group_crystal_system orthorhombic _space_group_IT_number 56 _space_group_name_H-M_alt 'P c c n' _space_group_name_Hall '-P 2ab 2ac' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, -y+1/2, z' 3 'x+1/2, -y, -z+1/2' 4 '-x, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x-1/2, y-1/2, -z' 7 '-x-1/2, y, z-1/2' 8 'x, -y-1/2, z-1/2' _cell_length_a 31.874(5) _cell_length_b 11.337(5) _cell_length_c 21.874(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7904.3 _cell_formula_units_Z 4 _cell_measurement_reflns_used 5780 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 24.953 _cell_measurement_theta_min 2.257 _exptl_absorpt_coefficient_mu 0.538 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.492931 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS v.2.10 (Bruker,2003) was used for absorption correction. R(int) was 0.0686 before and 0.0382 after correction. The Ratio of minimum to maximum transmission is 0.4929. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 3456 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_unetI/netI 0.0510 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 7347 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.50 _diffrn_reflns_theta_min 2.12 _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'MO K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_current 25.0 _diffrn_source_power 1.125 _diffrn_source_voltage 45.0 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 5390 _reflns_number_total 7347 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'SAINT v6.45A (Bruker, 2003)' _computing_data_collection 'Bruker Smart' _computing_data_reduction 'SAINT v6.45A (Bruker, 2003)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 1.363 _refine_diff_density_min -1.209 _refine_diff_density_rms 0.140 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 488 _refine_ls_number_reflns 7347 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0911 _refine_ls_R_factor_gt 0.0741 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1255P)^2^+19.9690P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2090 _refine_ls_wR_factor_ref 0.2224 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Cd1 Cd 0.2500 1.2500 0.07348(3) 0.0367(2) Uani 1 2 d S . . N6 N 0.3453(2) 1.2169(7) 0.0738(3) 0.0618(17) Uani 1 1 d . . . O7 O 0.3276(2) 1.2879(6) 0.1115(3) 0.0840(19) Uani 1 1 d . . . O8 O 0.38208(17) 1.1877(7) 0.0804(3) 0.0801(18) Uani 1 1 d . . . O9 O 0.32257(19) 1.1765(5) 0.0331(3) 0.0795(18) Uani 1 1 d . . . P1 P 0.31398(4) 0.82498(10) 0.32884(6) 0.0242(3) Uani 1 1 d . . . P2 P 0.39442(4) 0.89693(11) 0.30203(7) 0.0273(3) Uani 1 1 d . . . P3 P 0.36957(4) 0.66836(11) 0.27794(7) 0.0280(3) Uani 1 1 d . . . N1 N 0.34943(14) 0.9215(3) 0.3294(2) 0.0304(10) Uani 1 1 d . . . N2 N 0.40391(14) 0.7678(4) 0.2781(2) 0.0349(11) Uani 1 1 d . . . N3 N 0.32446(13) 0.6989(4) 0.3036(2) 0.0287(10) Uani 1 1 d . . . O1 O 0.27272(10) 0.8777(3) 0.29775(16) 0.0261(8) Uani 1 1 d . . . O2 O 0.29592(11) 0.8061(3) 0.39607(17) 0.0311(8) Uani 1 1 d . . . O3 O 0.43095(11) 0.9275(3) 0.34873(18) 0.0335(9) Uani 1 1 d . . . O4 O 0.39956(10) 0.9928(3) 0.24966(17) 0.0281(8) Uani 1 1 d . . . O6 O 0.38980(11) 0.5609(3) 0.31441(18) 0.0309(8) Uani 1 1 d . . . O5 O 0.36287(11) 0.6156(3) 0.21147(18) 0.0311(8) Uani 1 1 d . . . C11 C 0.43614(16) 1.0438(5) 0.3692(3) 0.0323(12) Uani 1 1 d . . . C12 C 0.42712(18) 1.0702(6) 0.4281(3) 0.0415(14) Uani 1 1 d . . . H12 H 0.4160 1.0125 0.4536 0.050 Uiso 1 1 calc R . . C13 C 0.4344(2) 1.1828(6) 0.4507(3) 0.0513(17) Uani 1 1 d . . . H13 H 0.4284 1.2014 0.4912 0.062 Uiso 1 1 calc R . . C14 C 0.4508(2) 1.2671(6) 0.4113(3) 0.0498(17) Uani 1 1 d . . . H14 H 0.4550 1.3436 0.4253 0.060 Uiso 1 1 calc R . . C15 C 0.46071(18) 1.2398(5) 0.3522(3) 0.0396(14) Uani 1 1 d . . . H15 H 0.4723 1.2979 0.3274 0.048 Uiso 1 1 calc R . . C16 C 0.45404(16) 1.1273(5) 0.3278(3) 0.0338(13) Uani 1 1 d . . . C17 C 0.46441(16) 1.0988(4) 0.2655(3) 0.0305(12) Uani 1 1 d . . . C18 C 0.50113(17) 1.1414(5) 0.2377(3) 0.0383(14) Uani 1 1 d . . . H18 H 0.5200 1.1846 0.2611 0.046 Uiso 1 1 calc R . . C19 C 0.51014(17) 1.1212(6) 0.1767(3) 0.0401(14) Uani 1 1 d . . . H19 H 0.5343 1.1525 0.1594 0.048 Uiso 1 1 calc R . . C20 C 0.48257(19) 1.0531(5) 0.1410(3) 0.0411(14) Uani 1 1 d . . . H20 H 0.4884 1.0391 0.1000 0.049 Uiso 1 1 calc R . . C21 C 0.44697(17) 1.0076(5) 0.1673(3) 0.0345(13) Uani 1 1 d . . . H21 H 0.4287 0.9618 0.1442 0.041 Uiso 1 1 calc R . . C22 C 0.43851(15) 1.0300(4) 0.2274(3) 0.0269(11) Uani 1 1 d . . . C23 C 0.37399(15) 0.4472(4) 0.3083(3) 0.0297(12) Uani 1 1 d . . . C24 C 0.35370(17) 0.3985(5) 0.3596(3) 0.0400(14) Uani 1 1 d . . . H24 H 0.3493 0.4424 0.3950 0.048 Uiso 1 1 calc R . . C25 C 0.34041(17) 0.2811(5) 0.3551(4) 0.0458(17) Uani 1 1 d . . . H25 H 0.3276 0.2457 0.3886 0.055 Uiso 1 1 calc R . . C26 C 0.34585(18) 0.2171(5) 0.3024(3) 0.0398(14) Uani 1 1 d . . . H26 H 0.3361 0.1400 0.3001 0.048 Uiso 1 1 calc R . . C27 C 0.36611(17) 0.2680(4) 0.2526(3) 0.0378(14) Uani 1 1 d . . . H27 H 0.3703 0.2233 0.2174 0.045 Uiso 1 1 calc R . . C28 C 0.38027(16) 0.3844(4) 0.2540(3) 0.0327(12) Uani 1 1 d . . . C29 C 0.40316(17) 0.4381(4) 0.2019(3) 0.0330(12) Uani 1 1 d . . . C30 C 0.43389(18) 0.3766(5) 0.1699(3) 0.0395(14) Uani 1 1 d . . . H30 H 0.4396 0.2991 0.1811 0.047 Uiso 1 1 calc R . . C31 C 0.45610(19) 0.4258(5) 0.1223(3) 0.0460(16) Uani 1 1 d . . . H31 H 0.4770 0.3833 0.1025 0.055 Uiso 1 1 calc R . . C32 C 0.4463(2) 0.5434(5) 0.1040(3) 0.0446(15) Uani 1 1 d . . . H32 H 0.4600 0.5778 0.0710 0.053 Uiso 1 1 calc R . . C33 C 0.41632(19) 0.6053(5) 0.1358(3) 0.0399(14) Uani 1 1 d . . . H33 H 0.4104 0.6829 0.1252 0.048 Uiso 1 1 calc R . . C34 C 0.39526(16) 0.5532(5) 0.1830(3) 0.0307(12) Uani 1 1 d . . . C1 C 0.27044(16) 0.9537(4) 0.2491(2) 0.0278(11) Uani 1 1 d . . . C5 C 0.29878(19) 0.9526(5) 0.2014(3) 0.0406(14) Uani 1 1 d . . . H5 H 0.3215 0.9012 0.2011 0.049 Uiso 1 1 calc R . . C4 C 0.2919(2) 1.0321(5) 0.1535(3) 0.0430(15) Uani 1 1 d . . . H4 H 0.3106 1.0320 0.1209 0.052 Uiso 1 1 calc R . . C3 C 0.23323(18) 1.1069(5) 0.2004(3) 0.0330(12) Uani 1 1 d . . . H3 H 0.2110 1.1600 0.2007 0.040 Uiso 1 1 calc R . . C2 C 0.23726(17) 1.0319(4) 0.2484(3) 0.0325(12) Uani 1 1 d . . . H2 H 0.2180 1.0332 0.2804 0.039 Uiso 1 1 calc R . . N4 N 0.25964(15) 1.1087(4) 0.1523(2) 0.0353(11) Uani 1 1 d . . . C6 C 0.28551(17) 0.9054(5) 0.4310(2) 0.0319(12) Uani 1 1 d . . . C7 C 0.2495(2) 0.9679(6) 0.4220(3) 0.0466(16) Uani 1 1 d . . . H7 H 0.2310 0.9476 0.3909 0.056 Uiso 1 1 calc R . . C8 C 0.1974(2) 1.0341(6) 0.0127(3) 0.0450(15) Uani 1 1 d . . . H8 H 0.1793 1.0563 0.0441 0.054 Uiso 1 1 calc R . . C9 C 0.2589(2) 1.0621(7) -0.0398(3) 0.0558(19) Uani 1 1 d . . . H9 H 0.2837 1.1042 -0.0456 0.067 Uiso 1 1 calc R . . C10 C 0.31353(18) 0.9404(6) 0.4763(3) 0.0411(14) Uani 1 1 d . . . H10 H 0.3389 0.9013 0.4818 0.049 Uiso 1 1 calc R . . N5 N 0.23334(17) 1.0952(5) 0.0046(2) 0.0417(12) Uani 1 1 d . . . C35 C 0.2500 0.7500 0.0855(6) 0.097(5) Uani 1 2 d S . . H35A H 0.2635 0.8080 0.0595 0.116 Uiso 0.50 1 calc PR . . H35B H 0.2365 0.6920 0.0595 0.116 Uiso 0.50 1 calc PR . . Cl1 Cl 0.28793(8) 0.6803(2) 0.13204(12) 0.0870(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0520(4) 0.0334(3) 0.0248(3) 0.000 0.000 0.0056(3) N6 0.053(4) 0.086(5) 0.046(4) 0.018(3) -0.010(3) -0.019(4) O7 0.085(4) 0.106(5) 0.061(4) 0.037(3) 0.023(3) 0.025(4) O8 0.040(3) 0.124(5) 0.076(4) -0.013(4) -0.009(3) -0.002(3) O9 0.076(4) 0.090(4) 0.072(4) 0.016(3) -0.028(3) -0.026(3) P1 0.0156(6) 0.0165(6) 0.0405(8) 0.0008(5) 0.0020(5) -0.0006(4) P2 0.0178(7) 0.0172(6) 0.0469(8) 0.0023(6) 0.0023(6) -0.0010(5) P3 0.0197(7) 0.0163(6) 0.0481(8) 0.0034(5) 0.0040(6) 0.0013(5) N1 0.028(2) 0.0140(19) 0.049(3) 0.0016(18) 0.001(2) -0.0035(17) N2 0.023(2) 0.023(2) 0.059(3) 0.003(2) 0.010(2) 0.0031(17) N3 0.021(2) 0.019(2) 0.046(3) -0.0012(19) 0.000(2) -0.0031(17) O1 0.0144(17) 0.0223(17) 0.042(2) 0.0043(15) 0.0028(15) 0.0019(13) O2 0.030(2) 0.0261(18) 0.037(2) 0.0018(16) 0.0032(16) -0.0015(15) O3 0.0248(19) 0.0257(18) 0.050(2) 0.0083(17) -0.0042(17) -0.0020(15) O4 0.0189(18) 0.0202(17) 0.045(2) 0.0038(15) -0.0023(16) 0.0009(13) O6 0.0211(18) 0.0223(18) 0.049(2) 0.0052(16) 0.0032(16) 0.0006(14) O5 0.0205(18) 0.0194(17) 0.054(2) 0.0036(16) 0.0014(17) 0.0026(14) C11 0.021(3) 0.027(3) 0.048(3) 0.003(2) -0.007(2) -0.005(2) C12 0.024(3) 0.048(3) 0.053(4) 0.004(3) -0.006(3) -0.006(3) C13 0.041(4) 0.056(4) 0.056(4) -0.015(3) -0.008(3) 0.000(3) C14 0.039(4) 0.048(4) 0.063(4) -0.021(3) -0.009(3) -0.015(3) C15 0.027(3) 0.031(3) 0.061(4) 0.001(3) -0.007(3) -0.011(2) C16 0.014(2) 0.033(3) 0.055(4) 0.006(3) -0.007(2) -0.001(2) C17 0.019(3) 0.024(3) 0.048(3) 0.010(2) -0.001(2) 0.001(2) C18 0.022(3) 0.037(3) 0.056(4) 0.006(3) -0.002(3) -0.004(2) C19 0.017(3) 0.047(3) 0.056(4) 0.005(3) 0.004(3) -0.005(2) C20 0.038(3) 0.041(3) 0.045(3) 0.004(3) 0.011(3) 0.009(3) C21 0.028(3) 0.028(3) 0.047(4) 0.005(2) 0.004(2) -0.001(2) C22 0.016(2) 0.017(2) 0.048(3) 0.005(2) 0.005(2) 0.0010(18) C23 0.014(2) 0.014(2) 0.061(4) 0.006(2) 0.001(2) 0.0018(18) C24 0.028(3) 0.025(3) 0.067(4) 0.008(3) 0.006(3) 0.002(2) C25 0.020(3) 0.027(3) 0.090(5) 0.021(3) 0.010(3) 0.003(2) C26 0.032(3) 0.020(3) 0.067(4) 0.005(3) 0.007(3) -0.002(2) C27 0.026(3) 0.024(3) 0.063(4) 0.000(3) 0.001(3) 0.003(2) C28 0.015(2) 0.024(3) 0.059(4) 0.001(2) 0.000(2) 0.008(2) C29 0.026(3) 0.019(2) 0.054(3) -0.010(2) 0.004(2) -0.004(2) C30 0.038(3) 0.021(3) 0.059(4) -0.002(3) 0.005(3) 0.005(2) C31 0.035(3) 0.041(3) 0.063(4) -0.019(3) 0.009(3) 0.001(3) C32 0.042(4) 0.038(3) 0.054(4) -0.007(3) 0.017(3) -0.008(3) C33 0.043(3) 0.024(3) 0.053(4) -0.002(2) 0.007(3) -0.003(2) C34 0.025(3) 0.027(3) 0.040(3) -0.007(2) 0.007(2) 0.001(2) C1 0.026(3) 0.020(2) 0.037(3) -0.003(2) 0.005(2) -0.003(2) C5 0.038(3) 0.034(3) 0.049(4) -0.006(3) 0.001(3) 0.018(2) C4 0.046(4) 0.044(3) 0.039(3) 0.001(3) 0.015(3) 0.011(3) C3 0.031(3) 0.026(3) 0.042(3) 0.000(2) 0.003(2) 0.008(2) C2 0.032(3) 0.027(3) 0.039(3) 0.005(2) 0.011(2) -0.001(2) N4 0.043(3) 0.030(2) 0.033(2) 0.000(2) 0.005(2) 0.009(2) C6 0.034(3) 0.032(3) 0.030(3) 0.000(2) 0.002(2) 0.005(2) C7 0.041(4) 0.053(4) 0.046(4) -0.012(3) -0.017(3) 0.010(3) C8 0.042(4) 0.064(4) 0.029(3) 0.001(3) 0.012(3) -0.001(3) C9 0.058(4) 0.065(4) 0.044(4) -0.020(3) 0.020(3) -0.030(4) C10 0.027(3) 0.051(4) 0.045(3) 0.000(3) -0.004(3) 0.009(3) N5 0.048(3) 0.047(3) 0.030(3) -0.007(2) 0.004(2) -0.003(2) C35 0.112(12) 0.132(14) 0.047(7) 0.000 0.000 -0.045(10) Cl1 0.0791(15) 0.0815(15) 0.1003(18) -0.0220(13) 0.0144(13) -0.0094(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O7 2.644(7) . ? Cd1 O7 2.644(7) 2_575 ? Cd1 O9 2.613(7) 2_575 ? Cd1 O9 2.613(7) . ? Cd1 N4 2.374(5) . ? Cd1 N4 2.374(5) 2_575 ? Cd1 N5 2.374(5) . ? Cd1 N5 2.374(5) 2_575 ? N6 O7 1.284(9) . ? N6 O8 1.225(9) . ? N6 O9 1.236(8) . ? P1 N1 1.573(4) . ? P1 N3 1.568(4) . ? P1 O1 1.597(3) . ? P1 O2 1.594(4) . ? P2 N1 1.579(5) . ? P2 N2 1.584(4) . ? P2 O3 1.587(4) . ? P2 O4 1.587(4) . ? P3 N2 1.571(5) . ? P3 N3 1.582(4) . ? P3 O6 1.592(4) . ? P3 O5 1.587(4) . ? O1 C1 1.371(6) . ? O2 C6 1.400(6) . ? O3 C11 1.403(6) . ? O4 C22 1.399(6) . ? O6 C23 1.391(6) . ? O5 C34 1.398(6) . ? C11 C12 1.352(8) . ? C11 C16 1.429(8) . ? C12 H12 0.9300 . ? C12 C13 1.389(9) . ? C13 H13 0.9300 . ? C13 C14 1.389(10) . ? C14 H14 0.9300 . ? C14 C15 1.365(10) . ? C15 H15 0.9300 . ? C15 C16 1.399(8) . ? C16 C17 1.439(8) . ? C17 C18 1.405(8) . ? C17 C22 1.409(8) . ? C18 H18 0.9300 . ? C18 C19 1.385(9) . ? C19 H19 0.9300 . ? C19 C20 1.406(9) . ? C20 H20 0.9300 . ? C20 C21 1.373(8) . ? C21 H21 0.9300 . ? C21 C22 1.367(8) . ? C23 C24 1.409(8) . ? C23 C28 1.399(8) . ? C24 H24 0.9300 . ? C24 C25 1.400(8) . ? C25 H25 0.9300 . ? C25 C26 1.372(10) . ? C26 H26 0.9300 . ? C26 C27 1.393(9) . ? C27 H27 0.9300 . ? C27 C28 1.395(7) . ? C28 C29 1.483(8) . ? C29 C30 1.392(8) . ? C29 C34 1.392(8) . ? C30 H30 0.9300 . ? C30 C31 1.377(9) . ? C31 H31 0.9300 . ? C31 C32 1.427(9) . ? C32 H32 0.9300 . ? C32 C33 1.374(8) . ? C33 H33 0.9300 . ? C33 C34 1.364(8) . ? C1 C5 1.381(8) . ? C1 C2 1.380(8) . ? C5 H5 0.9300 . ? C5 C4 1.398(9) . ? C4 H4 0.9300 . ? C4 N4 1.346(7) . ? C3 H3 0.9300 . ? C3 C2 1.357(8) . ? C3 N4 1.348(7) . ? C2 H2 0.9300 . ? C6 C7 1.364(8) . ? C6 C10 1.393(8) . ? C7 H7 0.9300 . ? C7 C9 1.382(9) 7_656 ? C8 H8 0.9300 . ? C8 C10 1.371(9) 7_655 ? C8 N5 1.351(8) . ? C9 C7 1.382(9) 7_655 ? C9 H9 0.9300 . ? C9 N5 1.322(8) . ? C10 C8 1.371(9) 7_656 ? C10 H10 0.9300 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 Cl1 1.767(8) 2_565 ? C35 Cl1 1.767(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Cd1 O7 143.4(2) 2_575 . ? O9 Cd1 O7 152.0(2) 2_575 . ? O9 Cd1 O7 47.93(19) . . ? O9 Cd1 O7 47.9(2) 2_575 2_575 ? O9 Cd1 O7 152.0(2) . 2_575 ? O9 Cd1 O9 140.5(2) . 2_575 ? N4 Cd1 O7 77.48(19) 2_575 . ? N4 Cd1 O7 76.13(17) . . ? N4 Cd1 O7 77.48(19) . 2_575 ? N4 Cd1 O7 76.13(17) 2_575 2_575 ? N4 Cd1 O9 85.17(17) 2_575 2_575 ? N4 Cd1 O9 85.17(17) . . ? N4 Cd1 O9 125.13(17) . 2_575 ? N4 Cd1 O9 125.14(17) 2_575 . ? N4 Cd1 N4 86.8(2) 2_575 . ? N4 Cd1 N5 158.65(18) . 2_575 ? N4 Cd1 N5 89.50(17) . . ? N4 Cd1 N5 89.50(17) 2_575 2_575 ? N4 Cd1 N5 158.65(18) 2_575 . ? N5 Cd1 O7 82.54(18) . 2_575 ? N5 Cd1 O7 121.9(2) 2_575 2_575 ? N5 Cd1 O7 121.9(2) . . ? N5 Cd1 O7 82.54(18) 2_575 . ? N5 Cd1 O9 75.38(18) 2_575 2_575 ? N5 Cd1 O9 79.80(18) . 2_575 ? N5 Cd1 O9 79.80(18) 2_575 . ? N5 Cd1 O9 75.38(18) . . ? N5 Cd1 N5 101.2(2) . 2_575 ? O8 N6 O7 121.0(7) . . ? O8 N6 O9 123.1(8) . . ? O9 N6 O7 115.8(7) . . ? N6 O7 Cd1 96.2(5) . . ? N6 O9 Cd1 99.1(5) . . ? N1 P1 O1 109.5(2) . . ? N1 P1 O2 110.2(2) . . ? N3 P1 N1 118.9(2) . . ? N3 P1 O1 111.5(2) . . ? N3 P1 O2 106.2(2) . . ? O2 P1 O1 98.39(19) . . ? N1 P2 N2 117.5(2) . . ? N1 P2 O3 112.5(2) . . ? N1 P2 O4 104.3(2) . . ? N2 P2 O3 105.9(2) . . ? N2 P2 O4 112.0(2) . . ? O3 P2 O4 103.85(19) . . ? N2 P3 N3 118.4(2) . . ? N2 P3 O6 105.4(2) . . ? N2 P3 O5 111.5(2) . . ? N3 P3 O6 111.0(2) . . ? N3 P3 O5 106.6(2) . . ? O5 P3 O6 103.0(2) . . ? P1 N1 P2 121.8(3) . . ? P3 N2 P2 122.0(3) . . ? P1 N3 P3 121.2(3) . . ? C1 O1 P1 127.6(3) . . ? C6 O2 P1 118.7(3) . . ? C11 O3 P2 119.8(3) . . ? C22 O4 P2 123.3(3) . . ? C23 O6 P3 120.9(3) . . ? C34 O5 P3 120.0(3) . . ? O3 C11 C16 117.9(5) . . ? C12 C11 O3 119.2(5) . . ? C12 C11 C16 122.8(5) . . ? C11 C12 H12 119.7 . . ? C11 C12 C13 120.5(6) . . ? C13 C12 H12 119.7 . . ? C12 C13 H13 120.9 . . ? C12 C13 C14 118.2(7) . . ? C14 C13 H13 120.9 . . ? C13 C14 H14 119.4 . . ? C15 C14 C13 121.3(6) . . ? C15 C14 H14 119.4 . . ? C14 C15 H15 118.9 . . ? C14 C15 C16 122.2(6) . . ? C16 C15 H15 118.9 . . ? C11 C16 C17 122.9(5) . . ? C15 C16 C11 115.0(5) . . ? C15 C16 C17 122.1(5) . . ? C18 C17 C16 121.6(5) . . ? C18 C17 C22 115.0(5) . . ? C22 C17 C16 123.4(5) . . ? C17 C18 H18 118.9 . . ? C19 C18 C17 122.2(5) . . ? C19 C18 H18 118.9 . . ? C18 C19 H19 120.1 . . ? C18 C19 C20 119.8(5) . . ? C20 C19 H19 120.1 . . ? C19 C20 H20 120.3 . . ? C21 C20 C19 119.4(6) . . ? C21 C20 H20 120.3 . . ? C20 C21 H21 120.1 . . ? C22 C21 C20 119.7(5) . . ? C22 C21 H21 120.1 . . ? O4 C22 C17 118.8(5) . . ? C21 C22 O4 117.0(5) . . ? C21 C22 C17 123.8(5) . . ? O6 C23 C24 116.9(5) . . ? O6 C23 C28 120.1(5) . . ? C28 C23 C24 122.9(5) . . ? C23 C24 H24 121.5 . . ? C25 C24 C23 117.0(6) . . ? C25 C24 H24 121.5 . . ? C24 C25 H25 119.2 . . ? C26 C25 C24 121.6(6) . . ? C26 C25 H25 119.2 . . ? C25 C26 H26 120.1 . . ? C25 C26 C27 119.8(5) . . ? C27 C26 H26 120.1 . . ? C26 C27 H27 119.2 . . ? C26 C27 C28 121.7(6) . . ? C28 C27 H27 119.2 . . ? C23 C28 C29 120.9(5) . . ? C27 C28 C23 117.0(5) . . ? C27 C28 C29 122.1(5) . . ? C30 C29 C28 121.8(5) . . ? C34 C29 C28 121.7(5) . . ? C34 C29 C30 116.6(5) . . ? C29 C30 H30 118.7 . . ? C31 C30 C29 122.6(5) . . ? C31 C30 H30 118.7 . . ? C30 C31 H31 120.7 . . ? C30 C31 C32 118.5(5) . . ? C32 C31 H31 120.7 . . ? C31 C32 H32 120.4 . . ? C33 C32 C31 119.2(6) . . ? C33 C32 H32 120.4 . . ? C32 C33 H33 119.9 . . ? C34 C33 C32 120.3(5) . . ? C34 C33 H33 119.9 . . ? C29 C34 O5 118.3(5) . . ? C33 C34 O5 118.8(5) . . ? C33 C34 C29 122.8(5) . . ? O1 C1 C5 123.1(5) . . ? O1 C1 C2 116.9(4) . . ? C2 C1 C5 119.9(5) . . ? C1 C5 H5 121.4 . . ? C1 C5 C4 117.2(5) . . ? C4 C5 H5 121.4 . . ? C5 C4 H4 118.3 . . ? N4 C4 C5 123.4(5) . . ? N4 C4 H4 118.3 . . ? C2 C3 H3 118.2 . . ? N4 C3 H3 118.2 . . ? N4 C3 C2 123.7(5) . . ? C1 C2 H2 120.6 . . ? C3 C2 C1 118.9(5) . . ? C3 C2 H2 120.6 . . ? C4 N4 Cd1 123.3(4) . . ? C4 N4 C3 116.8(5) . . ? C3 N4 Cd1 119.8(3) . . ? C7 C6 O2 122.6(5) . . ? C7 C6 C10 119.6(5) . . ? C10 C6 O2 117.8(5) . . ? C6 C7 H7 120.7 . . ? C6 C7 C9 118.6(6) . 7_656 ? C9 C7 H7 120.7 7_656 . ? C10 C8 H8 118.8 7_655 . ? N5 C8 H8 118.8 . . ? N5 C8 C10 122.4(5) . 7_655 ? C7 C9 H9 118.6 7_655 . ? N5 C9 C7 122.9(6) . 7_655 ? N5 C9 H9 118.6 . . ? C6 C10 H10 120.9 . . ? C8 C10 C6 118.1(5) 7_656 . ? C8 C10 H10 120.9 7_656 . ? C8 N5 Cd1 119.0(4) . . ? C9 N5 Cd1 122.5(4) . . ? C9 N5 C8 118.3(5) . . ? H35A C35 H35B 108.2 . . ? Cl1 C35 H35A 109.7 2_565 . ? Cl1 C35 H35A 109.7 . . ? Cl1 C35 H35B 109.7 2_565 . ? Cl1 C35 H35B 109.7 . . ? Cl1 C35 Cl1 109.7(7) 2_565 . ? 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 O7 Cd1 O7 N6 135.8(4) 2_575 . . . ? O7 Cd1 O9 N6 -121.6(5) 2_575 . . . ? O7 Cd1 O9 N6 5.6(4) . . . . ? O7 Cd1 N4 C4 -53.4(5) . . . . ? O7 Cd1 N4 C4 152.3(5) 2_575 . . . ? O7 Cd1 N4 C3 -31.2(4) 2_575 . . . ? O7 Cd1 N4 C3 123.1(5) . . . . ? O7 Cd1 N5 C8 141.3(4) . . . . ? O7 Cd1 N5 C8 -9.4(5) 2_575 . . . ? O7 Cd1 N5 C9 -35.2(6) . . . . ? O7 Cd1 N5 C9 174.1(6) 2_575 . . . ? O7 N6 O9 Cd1 -9.6(7) . . . . ? O8 N6 O7 Cd1 -167.2(6) . . . . ? O8 N6 O9 Cd1 166.9(6) . . . . ? O9 Cd1 O7 N6 -5.4(4) . . . . ? O9 Cd1 O7 N6 -126.4(5) 2_575 . . . ? O9 Cd1 O9 N6 146.3(5) 2_575 . . . ? O9 Cd1 N4 C4 146.9(5) 2_575 . . . ? O9 Cd1 N4 C4 -5.6(5) . . . . ? O9 Cd1 N4 C3 170.9(4) . . . . ? O9 Cd1 N4 C3 -36.6(5) 2_575 . . . ? O9 Cd1 N5 C8 153.1(5) . . . . ? O9 Cd1 N5 C8 -57.9(5) 2_575 . . . ? O9 Cd1 N5 C9 -23.3(6) . . . . ? O9 Cd1 N5 C9 125.6(6) 2_575 . . . ? O9 N6 O7 Cd1 9.4(6) . . . . ? P1 O1 C1 C5 33.5(7) . . . . ? P1 O1 C1 C2 -148.1(4) . . . . ? P1 O2 C6 C7 77.7(7) . . . . ? P1 O2 C6 C10 -102.2(5) . . . . ? P2 O3 C11 C12 110.3(5) . . . . ? P2 O3 C11 C16 -74.7(5) . . . . ? P2 O4 C22 C17 -69.9(5) . . . . ? P2 O4 C22 C21 117.1(5) . . . . ? P3 O6 C23 C24 -111.5(5) . . . . ? P3 O6 C23 C28 71.4(5) . . . . ? P3 O5 C34 C29 76.2(6) . . . . ? P3 O5 C34 C33 -107.1(5) . . . . ? N1 P1 N3 P3 -1.0(5) . . . . ? N1 P1 O1 C1 37.0(5) . . . . ? N1 P1 O2 C6 47.1(4) . . . . ? N1 P2 N2 P3 3.2(5) . . . . ? N1 P2 O3 C11 -62.4(4) . . . . ? N1 P2 O4 C22 157.7(4) . . . . ? N2 P2 N1 P1 -4.4(5) . . . . ? N2 P2 O3 C11 167.9(4) . . . . ? N2 P2 O4 C22 -74.2(4) . . . . ? N2 P3 N3 P1 -0.2(5) . . . . ? N2 P3 O6 C23 -160.8(4) . . . . ? N2 P3 O5 C34 65.6(4) . . . . ? N3 P1 N1 P2 3.4(5) . . . . ? N3 P1 O1 C1 -96.8(4) . . . . ? N3 P1 O2 C6 177.2(4) . . . . ? N3 P3 N2 P2 -0.9(5) . . . . ? N3 P3 O6 C23 69.8(4) . . . . ? N3 P3 O5 C34 -163.9(4) . . . . ? O1 P1 N1 P2 -126.5(3) . . . . ? O1 P1 N3 P3 128.0(3) . . . . ? O1 P1 O2 C6 -67.4(4) . . . . ? O1 C1 C5 C4 177.7(5) . . . . ? O1 C1 C2 C3 -178.5(5) . . . . ? O2 P1 N1 P2 126.3(3) . . . . ? O2 P1 N3 P3 -125.9(3) . . . . ? O2 P1 O1 C1 152.0(4) . . . . ? O2 C6 C7 C9 177.6(6) . . . 7_656 ? O2 C6 C10 C8 -176.9(5) . . . 7_656 ? O3 P2 N1 P1 -127.9(3) . . . . ? O3 P2 N2 P3 129.9(3) . . . . ? O3 P2 O4 C22 39.7(4) . . . . ? O3 C11 C12 C13 176.1(5) . . . . ? O3 C11 C16 C15 -176.3(5) . . . . ? O3 C11 C16 C17 3.9(7) . . . . ? O4 P2 N1 P1 120.2(3) . . . . ? O4 P2 N2 P3 -117.5(3) . . . . ? O4 P2 O3 C11 49.8(4) . . . . ? O6 P3 N2 P2 -125.8(3) . . . . ? O6 P3 N3 P1 121.8(3) . . . . ? O6 P3 O5 C34 -47.0(4) . . . . ? O6 C23 C24 C25 -175.6(5) . . . . ? O6 C23 C28 C27 175.7(4) . . . . ? O6 C23 C28 C29 -0.9(7) . . . . ? O5 P3 N2 P2 123.2(3) . . . . ? O5 P3 N3 P1 -126.7(3) . . . . ? O5 P3 O6 C23 -43.9(4) . . . . ? C11 C12 C13 C14 0.4(9) . . . . ? C11 C16 C17 C18 -140.3(5) . . . . ? C11 C16 C17 C22 41.6(8) . . . . ? C12 C11 C16 C15 -1.4(8) . . . . ? C12 C11 C16 C17 178.8(5) . . . . ? C12 C13 C14 C15 -1.9(10) . . . . ? C13 C14 C15 C16 1.7(10) . . . . ? C14 C15 C16 C11 -0.1(8) . . . . ? C14 C15 C16 C17 179.8(6) . . . . ? C15 C16 C17 C18 39.9(8) . . . . ? C15 C16 C17 C22 -138.2(5) . . . . ? C16 C11 C12 C13 1.2(9) . . . . ? C16 C17 C18 C19 -175.6(5) . . . . ? C16 C17 C22 O4 3.8(7) . . . . ? C16 C17 C22 C21 176.4(5) . . . . ? C17 C18 C19 C20 -1.8(9) . . . . ? C18 C17 C22 O4 -174.4(4) . . . . ? C18 C17 C22 C21 -1.8(7) . . . . ? C18 C19 C20 C21 0.1(9) . . . . ? C19 C20 C21 C22 0.7(8) . . . . ? C20 C21 C22 O4 172.9(5) . . . . ? C20 C21 C22 C17 0.2(8) . . . . ? C22 C17 C18 C19 2.6(8) . . . . ? C23 C24 C25 C26 -1.7(8) . . . . ? C23 C28 C29 C30 134.7(6) . . . . ? C23 C28 C29 C34 -44.8(8) . . . . ? C24 C23 C28 C27 -1.2(8) . . . . ? C24 C23 C28 C29 -177.8(5) . . . . ? C24 C25 C26 C27 1.8(9) . . . . ? C25 C26 C27 C28 -1.6(9) . . . . ? C26 C27 C28 C23 1.3(8) . . . . ? C26 C27 C28 C29 177.8(5) . . . . ? C27 C28 C29 C30 -41.8(8) . . . . ? C27 C28 C29 C34 138.8(6) . . . . ? C28 C23 C24 C25 1.4(8) . . . . ? C28 C29 C30 C31 -178.6(6) . . . . ? C28 C29 C34 O5 -4.4(8) . . . . ? C28 C29 C34 C33 179.0(5) . . . . ? C29 C30 C31 C32 -1.9(9) . . . . ? C30 C29 C34 O5 176.1(5) . . . . ? C30 C29 C34 C33 -0.4(8) . . . . ? C30 C31 C32 C33 2.6(9) . . . . ? C31 C32 C33 C34 -2.2(9) . . . . ? C32 C33 C34 O5 -175.4(5) . . . . ? C32 C33 C34 C29 1.2(9) . . . . ? C34 C29 C30 C31 0.9(9) . . . . ? C1 C5 C4 N4 0.5(10) . . . . ? C5 C1 C2 C3 -0.1(8) . . . . ? C5 C4 N4 Cd1 176.8(5) . . . . ? C5 C4 N4 C3 0.2(9) . . . . ? C2 C1 C5 C4 -0.6(8) . . . . ? C2 C3 N4 Cd1 -177.7(4) . . . . ? C2 C3 N4 C4 -1.0(9) . . . . ? N4 Cd1 O7 N6 90.7(4) . . . . ? N4 Cd1 O7 N6 -179.5(4) 2_575 . . . ? N4 Cd1 O9 N6 -70.0(4) . . . . ? N4 Cd1 O9 N6 12.6(5) 2_575 . . . ? N4 Cd1 N4 C4 -131.3(5) 2_575 . . . ? N4 Cd1 N4 C3 45.2(4) 2_575 . . . ? N4 Cd1 N5 C8 68.0(5) . . . . ? N4 Cd1 N5 C8 -11.9(8) 2_575 . . . ? N4 Cd1 N5 C9 -108.5(6) . . . . ? N4 Cd1 N5 C9 171.6(5) 2_575 . . . ? N4 C3 C2 C1 0.9(9) . . . . ? C7 C6 C10 C8 3.3(9) . . . 7_656 ? C7 C9 N5 Cd1 176.3(6) 7_655 . . . ? C7 C9 N5 C8 -0.2(11) 7_655 . . . ? C10 C6 C7 C9 -2.6(10) . . . 7_656 ? C10 C8 N5 Cd1 -177.2(5) 7_655 . . . ? C10 C8 N5 C9 -0.6(10) 7_655 . . . ? N5 Cd1 O7 N6 -88.3(4) 2_575 . . . ? N5 Cd1 O7 N6 10.2(5) . . . . ? N5 Cd1 O9 N6 -160.8(5) . . . . ? N5 Cd1 O9 N6 94.7(4) 2_575 . . . ? N5 Cd1 N4 C4 -50.8(7) 2_575 . . . ? N5 Cd1 N4 C4 69.8(5) . . . . ? N5 Cd1 N4 C3 -113.7(4) . . . . ? N5 Cd1 N4 C3 125.7(5) 2_575 . . . ? N5 Cd1 N5 C8 -130.6(5) 2_575 . . . ? N5 Cd1 N5 C9 52.9(5) 2_575 . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.098 0.151 -0.001 151 52 ' ' 2 0.402 0.151 0.499 150 52 ' ' 3 0.599 -0.152 0.501 149 55 ' ' 4 0.901 -0.152 0.001 148 55 ' ' 5 0.098 0.349 0.499 150 55 ' ' 6 0.402 0.349 0.999 150 55 ' ' 7 0.750 0.250 0.158 13 3 ' ' 8 0.750 0.250 0.658 13 3 ' ' 9 0.599 0.652 1.001 150 53 ' ' 10 0.901 0.652 0.501 149 53 ' ' 11 0.250 0.750 0.342 13 2 ' ' 12 0.250 0.750 0.842 13 2 ' ' _platon_squeeze_details ; ;