# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Vadapalli Chandrasekhar' _publ_contact_author_email VC@IITK.AC.IN _publ_section_title ; A phosphorus-supported multisite coordination ligand containing three imidazolyl arms and its metalation behaviour. An unprecedented co-existence of mononuclear and macrocyclic dinuclear Zn(II) complexes in the same unit cell of a crystalline lattice ; loop_ _publ_author_name 'Vadapalli Chandrasekhar' 'Ramachandran Azhakar' 'Ramamoorthy Boomishankar' 'Balasubramanian Murugesa Pandian' 'Alexander Steiner' #===END data_5+6 _database_code_depnum_ccdc_archive 'CCDC 680404' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H84 N56 O24 P4 S4 Zn4' _chemical_formula_weight 2487.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.402(2) _cell_length_b 15.451(3) _cell_length_c 18.222(4) _cell_angle_alpha 65.401(3) _cell_angle_beta 86.569(4) _cell_angle_gamma 74.121(4) _cell_volume 2556.4(9) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3727 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 25.39 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 1.167 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8804 _exptl_absorpt_correction_T_max 0.9145 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17052 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0636 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 28.44 _reflns_number_total 12204 _reflns_number_gt 7513 _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^)+(0.0719P)^2^+1.5667P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12204 _refine_ls_number_parameters 724 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0989 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1751 _refine_ls_wR_factor_gt 0.1334 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 Zn1 Zn -0.00574(5) 0.79189(3) 0.51141(3) 0.04251(14) Uani 1 1 d . . . Zn2 Zn 0.41902(5) 0.22421(4) 0.96603(3) 0.05159(16) Uani 1 1 d . . . P1 P 0.32628(10) 0.63798(8) 0.58810(7) 0.0441(3) Uani 1 1 d . . . P2 P 0.11441(11) 0.27380(9) 1.06707(7) 0.0483(3) Uani 1 1 d . . . S1 S 0.50776(12) 0.56440(11) 0.62779(9) 0.0669(4) Uani 1 1 d . . . S2 S -0.03955(13) 0.28794(10) 1.12910(8) 0.0645(3) Uani 1 1 d . . . N1 N 0.2186(3) 0.6144(3) 0.6601(2) 0.0454(8) Uani 1 1 d . . . N2 N 0.0902(3) 0.6773(2) 0.6391(2) 0.0417(7) Uani 1 1 d . . . N3 N -0.1524(3) 0.8076(2) 0.5875(2) 0.0437(8) Uani 1 1 d . . . N4 N -0.3307(4) 0.8291(3) 0.6533(3) 0.0565(10) Uani 1 1 d . . . N5 N 0.3064(3) 0.7608(3) 0.5444(2) 0.0499(9) Uani 1 1 d . . . N6 N 0.1898(3) 0.8211(3) 0.4973(2) 0.0460(8) Uani 1 1 d . . . N7 N -0.0480(4) 0.9326(3) 0.4199(2) 0.0498(9) Uani 1 1 d . . . N8 N -0.1093(5) 1.0801(3) 0.3222(3) 0.0672(12) Uani 1 1 d . . . N9 N 0.2626(3) 0.6223(2) 0.5138(2) 0.0447(8) Uani 1 1 d . . . N10 N 0.2150(3) 0.5379(2) 0.5431(2) 0.0429(8) Uani 1 1 d . . . N11 N 0.0933(4) 0.3783(3) 0.5945(2) 0.0455(8) Uani 1 1 d . . . N12 N 0.0622(3) 0.2957(2) 0.52726(19) 0.0393(7) Uani 1 1 d . . . N13 N 0.1872(4) 0.3657(3) 1.0433(2) 0.0542(9) Uani 1 1 d . . . N14 N 0.2913(4) 0.3640(3) 0.9928(2) 0.0520(9) Uani 1 1 d . . . N15 N 0.5026(4) 0.3391(3) 0.9048(2) 0.0520(9) Uani 1 1 d . . . N16 N 0.6195(4) 0.4415(3) 0.8350(3) 0.0645(11) Uani 1 1 d . . . N17 N 0.0742(4) 0.2698(3) 0.9817(2) 0.0601(10) Uani 1 1 d . . . N18 N 0.1837(4) 0.2429(3) 0.9406(2) 0.0551(9) Uani 1 1 d . . . N19 N 0.4096(4) 0.1849(3) 0.8737(2) 0.0584(10) Uani 1 1 d . . . N20 N 0.4386(5) 0.1631(4) 0.7621(3) 0.0718(13) Uani 1 1 d . . . N21 N 0.2357(4) 0.1701(3) 1.1178(2) 0.0585(10) Uani 1 1 d . . . N22 N 0.3646(4) 0.1608(3) 1.0887(2) 0.0563(9) Uani 1 1 d . . . N23 N 0.6028(4) 0.1230(3) 1.0302(2) 0.0645(11) Uani 1 1 d . . . N24 N 0.8004(5) 0.0362(4) 1.0938(3) 0.0776(13) Uani 1 1 d D . . N25 N 0.9037(5) 0.4491(3) 0.7336(3) 0.0624(10) Uani 1 1 d . . . N26 N 0.5421(4) 0.9303(3) 0.3753(2) 0.0570(10) Uani 1 1 d . . . N27 N 0.5884(4) 0.2283(3) 0.2222(3) 0.0627(11) Uani 1 1 d . . . N28 N 0.9052(5) 0.1301(4) 0.8090(4) 0.0757(13) Uani 1 1 d . . . O1 O 0.855(3) 0.3837(15) 0.7333(11) 0.092(5) Uani 0.60 1 d P A 1 O1A O 0.842(4) 0.414(3) 0.7066(17) 0.104(10) Uani 0.40 1 d P A 2 O2 O 0.8423(5) 0.5049(3) 0.7639(3) 0.1008(15) Uani 1 1 d . A . O3 O 1.0213(4) 0.4459(3) 0.7160(2) 0.0838(12) Uani 1 1 d . A . O4 O 0.4427(4) 0.9360(4) 0.3365(2) 0.0874(13) Uani 1 1 d . . . O5 O 0.5293(4) 0.9763(2) 0.4176(2) 0.0674(9) Uani 1 1 d . . . O6 O 0.6527(4) 0.8797(3) 0.3693(3) 0.0924(13) Uani 1 1 d . . . O7 O 0.5880(3) 0.1454(3) 0.2764(2) 0.0681(9) Uani 1 1 d . . . O8 O 0.6931(4) 0.2540(3) 0.2125(3) 0.1032(15) Uani 1 1 d . . . O9 O 0.4869(4) 0.2825(3) 0.1775(3) 0.0818(11) Uani 1 1 d . . . O10 O 0.9962(5) 0.1232(4) 0.7653(3) 0.1141(17) Uani 1 1 d . . . O11 O 0.9350(5) 0.0841(4) 0.8835(3) 0.1091(15) Uani 1 1 d . . . O12 O 0.7913(5) 0.1746(4) 0.7865(4) 0.144(2) Uani 1 1 d . . . C1 C 0.2520(5) 0.5388(4) 0.7421(3) 0.0621(13) Uani 1 1 d . . . H1A H 0.2440 0.5697 0.7789 0.093 Uiso 1 1 calc R . . H1B H 0.3423 0.4988 0.7462 0.093 Uiso 1 1 calc R . . H1C H 0.1918 0.4978 0.7556 0.093 Uiso 1 1 calc R . . C2 C 0.0031(4) 0.6698(3) 0.6917(2) 0.0411(9) Uani 1 1 d . . . H2A H 0.0232 0.6218 0.7445 0.049 Uiso 1 1 calc R . . C3 C -0.1270(4) 0.7379(3) 0.6666(2) 0.0424(9) Uani 1 1 d . . . C4 C -0.2771(4) 0.8600(3) 0.5827(3) 0.0486(10) Uani 1 1 d . . . H4A H -0.3217 0.9120 0.5357 0.058 Uiso 1 1 calc R . . C5 C -0.2383(4) 0.7518(4) 0.7080(3) 0.0577(12) Uani 1 1 d . . . H5A H -0.2489 0.7157 0.7624 0.069 Uiso 1 1 calc R . . C6 C 0.4047(6) 0.8041(4) 0.5562(4) 0.0848(18) Uani 1 1 d . . . H6A H 0.4566 0.8212 0.5094 0.127 Uiso 1 1 calc R . . H6B H 0.4628 0.7575 0.6029 0.127 Uiso 1 1 calc R . . H6C H 0.3606 0.8626 0.5641 0.127 Uiso 1 1 calc R . . C7 C 0.1862(5) 0.9092(3) 0.4451(3) 0.0560(11) Uani 1 1 d . . . H7A H 0.2617 0.9325 0.4369 0.067 Uiso 1 1 calc R . . C8 C 0.0611(5) 0.9702(3) 0.4000(3) 0.0532(11) Uani 1 1 d . . . C9 C -0.1478(5) 1.0008(4) 0.3719(3) 0.0631(13) Uani 1 1 d . . . H9N H -0.2345 0.9951 0.3722 0.076 Uiso 1 1 calc R . . C10 C 0.0233(5) 1.0617(4) 0.3392(3) 0.0677(14) Uani 1 1 d . . . H10 H 0.0772 1.1037 0.3141 0.081 Uiso 1 1 calc R . . C11 C 0.3254(5) 0.6507(4) 0.4364(3) 0.0601(12) Uani 1 1 d . . . H11A H 0.4007 0.5972 0.4385 0.090 Uiso 1 1 calc R . . H11B H 0.3552 0.7082 0.4259 0.090 Uiso 1 1 calc R . . H11C H 0.2616 0.6655 0.3940 0.090 Uiso 1 1 calc R . . C12 C 0.2092(4) 0.4972(3) 0.4954(3) 0.0438(9) Uani 1 1 d . . . H12 H 0.2431 0.5197 0.4445 0.053 Uiso 1 1 calc R . . C13 C 0.1494(4) 0.4155(3) 0.5216(2) 0.0417(9) Uani 1 1 d . . . C14 C 0.0417(4) 0.3075(3) 0.5943(2) 0.0458(9) Uani 1 1 d . . . H14 H -0.0031 0.2714 0.6367 0.055 Uiso 1 1 calc R . . C15 C 0.1296(4) 0.3637(3) 0.4813(3) 0.0444(9) Uani 1 1 d . . . H15 H 0.1575 0.3726 0.4299 0.053 Uiso 1 1 calc R . . C16 C 0.1494(5) 0.4418(4) 1.0730(3) 0.0640(13) Uani 1 1 d . . . H16A H 0.2258 0.4411 1.1006 0.096 Uiso 1 1 calc R . . H16B H 0.0797 0.4298 1.1098 0.096 Uiso 1 1 calc R . . H16C H 0.1177 0.5053 1.0284 0.096 Uiso 1 1 calc R . . C17 C 0.3478(5) 0.4345(3) 0.9669(3) 0.0530(11) Uani 1 1 d . . . H17 H 0.3191 0.4888 0.9797 0.064 Uiso 1 1 calc R . . C18 C 0.4581(4) 0.4246(3) 0.9169(3) 0.0511(10) Uani 1 1 d . . . C19 C 0.5989(5) 0.3526(4) 0.8551(3) 0.0618(12) Uani 1 1 d . . . H19 H 0.6469 0.3064 0.8362 0.074 Uiso 1 1 calc R . . C20 C 0.5298(5) 0.4893(4) 0.8728(3) 0.0625(13) Uani 1 1 d . . . H20 H 0.5196 0.5526 0.8694 0.075 Uiso 1 1 calc R . . C21 C -0.0592(5) 0.2909(5) 0.9492(4) 0.0814(17) Uani 1 1 d . . . H21A H -0.0738 0.3458 0.8970 0.122 Uiso 1 1 calc R . . H21B H -0.1232 0.3072 0.9849 0.122 Uiso 1 1 calc R . . H21C H -0.0696 0.2339 0.9439 0.122 Uiso 1 1 calc R . . C22 C 0.1668(5) 0.2351(4) 0.8746(3) 0.0599(12) Uani 1 1 d . . . H22 H 0.0820 0.2480 0.8522 0.072 Uiso 1 1 calc R . . C23 C 0.2855(5) 0.2055(3) 0.8377(3) 0.0556(11) Uani 1 1 d . . . C24 C 0.4984(5) 0.1591(4) 0.8267(3) 0.0655(13) Uani 1 1 d . . . H24 H 0.5907 0.1406 0.8371 0.079 Uiso 1 1 calc R . . C25 C 0.3049(6) 0.1919(4) 0.7678(3) 0.0685(14) Uani 1 1 d . . . H25 H 0.2386 0.2007 0.7313 0.082 Uiso 1 1 calc R . . C26 C 0.1986(7) 0.0777(4) 1.1454(5) 0.118(3) Uani 1 1 d . . . H26A H 0.2140 0.0532 1.1042 0.176 Uiso 1 1 calc R . . H26B H 0.1056 0.0891 1.1565 0.176 Uiso 1 1 calc R . . H26C H 0.2518 0.0299 1.1938 0.176 Uiso 1 1 calc R . . C27 C 0.4600(5) 0.1074(4) 1.1432(3) 0.0605(12) Uani 1 1 d . . . H27 H 0.4455 0.0830 1.1981 0.073 Uiso 1 1 calc R . . C28 C 0.5911(5) 0.0878(4) 1.1136(3) 0.0610(12) Uani 1 1 d . . . C29 C 0.7327(6) 0.0889(4) 1.0234(4) 0.0715(14) Uani 1 1 d . . . H29 H 0.7716 0.1010 0.9741 0.086 Uiso 1 1 calc R . . C30 C 0.7122(6) 0.0343(4) 1.1519(3) 0.0743(15) Uani 1 1 d . . . H30 H 0.7316 0.0022 1.2075 0.089 Uiso 1 1 calc R . . H11N H 0.083(5) 0.403(3) 0.630(3) 0.060(14) Uiso 1 1 d . . . H4N H -0.418(7) 0.858(5) 0.669(4) 0.11(2) Uiso 1 1 d . . . H24N H 0.887(3) -0.002(4) 1.095(4) 0.12(3) Uiso 1 1 d D . . H20N H 0.476(7) 0.142(5) 0.728(4) 0.10(2) Uiso 1 1 d . . . H8N H -0.162(5) 1.131(4) 0.290(3) 0.065(16) Uiso 1 1 d . . . H16N H 0.684(6) 0.463(5) 0.801(4) 0.10(2) Uiso 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 0.0435(3) 0.0422(3) 0.0471(3) -0.0212(2) 0.0078(2) -0.0168(2) Zn2 0.0574(3) 0.0538(3) 0.0494(3) -0.0246(2) 0.0107(2) -0.0209(3) P1 0.0354(5) 0.0482(6) 0.0554(6) -0.0302(5) 0.0047(5) -0.0086(5) P2 0.0479(6) 0.0484(6) 0.0491(6) -0.0217(5) 0.0077(5) -0.0125(5) S1 0.0392(6) 0.0789(9) 0.0800(9) -0.0403(7) -0.0002(6) 0.0003(6) S2 0.0562(7) 0.0741(8) 0.0613(7) -0.0291(6) 0.0197(6) -0.0172(6) N1 0.0404(18) 0.046(2) 0.0463(19) -0.0193(16) 0.0001(15) -0.0054(15) N2 0.0388(18) 0.0396(18) 0.0452(19) -0.0184(15) 0.0023(15) -0.0073(14) N3 0.0412(18) 0.0419(19) 0.050(2) -0.0225(16) 0.0013(15) -0.0085(15) N4 0.038(2) 0.066(3) 0.069(3) -0.037(2) 0.0070(19) -0.0049(18) N5 0.044(2) 0.052(2) 0.067(2) -0.0338(19) 0.0058(17) -0.0196(17) N6 0.046(2) 0.044(2) 0.056(2) -0.0247(17) 0.0080(16) -0.0181(16) N7 0.051(2) 0.0405(19) 0.054(2) -0.0139(16) 0.0056(17) -0.0177(17) N8 0.068(3) 0.046(2) 0.075(3) -0.009(2) -0.009(2) -0.019(2) N9 0.051(2) 0.0432(19) 0.0498(19) -0.0256(16) 0.0107(16) -0.0190(16) N10 0.0422(18) 0.0403(18) 0.0486(19) -0.0210(15) 0.0036(15) -0.0112(15) N11 0.052(2) 0.048(2) 0.044(2) -0.0237(17) 0.0026(16) -0.0176(17) N12 0.0426(18) 0.0376(17) 0.0428(18) -0.0204(14) 0.0047(14) -0.0134(14) N13 0.060(2) 0.052(2) 0.058(2) -0.0302(18) 0.0183(18) -0.0184(18) N14 0.056(2) 0.052(2) 0.053(2) -0.0239(18) 0.0107(17) -0.0204(18) N15 0.049(2) 0.056(2) 0.051(2) -0.0197(18) 0.0096(17) -0.0194(18) N16 0.054(2) 0.071(3) 0.063(3) -0.017(2) 0.009(2) -0.027(2) N17 0.049(2) 0.072(3) 0.067(3) -0.039(2) 0.0039(19) -0.0115(19) N18 0.051(2) 0.061(2) 0.059(2) -0.0329(19) 0.0076(18) -0.0126(18) N19 0.057(2) 0.068(3) 0.064(2) -0.040(2) 0.0093(19) -0.019(2) N20 0.074(3) 0.080(3) 0.070(3) -0.045(3) 0.015(2) -0.014(2) N21 0.055(2) 0.049(2) 0.072(3) -0.0243(19) 0.0130(19) -0.0162(18) N22 0.056(2) 0.057(2) 0.057(2) -0.0259(19) 0.0094(19) -0.0139(19) N23 0.076(3) 0.060(3) 0.052(2) -0.018(2) 0.004(2) -0.019(2) N24 0.066(3) 0.078(3) 0.074(3) -0.026(3) 0.005(3) -0.007(3) N25 0.075(3) 0.065(3) 0.055(2) -0.029(2) 0.022(2) -0.029(2) N26 0.055(2) 0.066(3) 0.049(2) -0.026(2) 0.0130(19) -0.015(2) N27 0.048(2) 0.060(3) 0.073(3) -0.022(2) 0.015(2) -0.017(2) N28 0.061(3) 0.062(3) 0.100(4) -0.028(3) 0.018(3) -0.024(2) O1 0.124(10) 0.104(9) 0.094(12) -0.064(10) 0.048(10) -0.071(8) O1A 0.101(13) 0.18(3) 0.074(15) -0.062(16) 0.032(11) -0.092(17) O2 0.108(3) 0.083(3) 0.143(4) -0.072(3) 0.073(3) -0.049(3) O3 0.071(2) 0.122(3) 0.094(3) -0.073(3) 0.031(2) -0.042(2) O4 0.055(2) 0.147(4) 0.082(3) -0.072(3) 0.0074(19) -0.024(2) O5 0.081(2) 0.061(2) 0.056(2) -0.0307(17) 0.0035(17) -0.0036(18) O6 0.063(2) 0.108(3) 0.128(4) -0.081(3) 0.004(2) -0.006(2) O7 0.059(2) 0.060(2) 0.070(2) -0.0138(18) 0.0174(17) -0.0161(17) O8 0.063(2) 0.084(3) 0.132(4) -0.008(3) 0.012(2) -0.033(2) O9 0.062(2) 0.058(2) 0.103(3) -0.015(2) -0.004(2) -0.0090(18) O10 0.081(3) 0.122(4) 0.096(3) -0.019(3) 0.029(3) -0.010(3) O11 0.107(4) 0.123(4) 0.095(3) -0.049(3) 0.040(3) -0.029(3) O12 0.062(3) 0.103(4) 0.226(7) -0.041(4) 0.004(4) -0.003(3) C1 0.049(3) 0.068(3) 0.055(3) -0.016(2) -0.003(2) -0.008(2) C2 0.038(2) 0.042(2) 0.040(2) -0.0159(17) 0.0044(17) -0.0073(17) C3 0.043(2) 0.041(2) 0.045(2) -0.0216(18) 0.0091(17) -0.0110(17) C4 0.038(2) 0.051(3) 0.058(3) -0.029(2) 0.0005(19) -0.0032(19) C5 0.044(2) 0.068(3) 0.060(3) -0.030(2) 0.011(2) -0.011(2) C6 0.089(4) 0.079(4) 0.093(4) -0.026(3) -0.019(3) -0.043(3) C7 0.054(3) 0.049(3) 0.071(3) -0.023(2) 0.010(2) -0.027(2) C8 0.056(3) 0.044(2) 0.061(3) -0.019(2) 0.007(2) -0.021(2) C9 0.061(3) 0.054(3) 0.070(3) -0.016(2) -0.002(2) -0.023(2) C10 0.071(3) 0.051(3) 0.079(3) -0.017(3) 0.005(3) -0.031(3) C11 0.070(3) 0.064(3) 0.062(3) -0.035(2) 0.018(2) -0.032(3) C12 0.041(2) 0.044(2) 0.051(2) -0.0240(19) 0.0107(18) -0.0139(18) C13 0.039(2) 0.037(2) 0.048(2) -0.0191(18) 0.0043(17) -0.0073(16) C14 0.049(2) 0.043(2) 0.043(2) -0.0148(18) 0.0031(18) -0.0132(19) C15 0.050(2) 0.045(2) 0.046(2) -0.0232(19) 0.0078(18) -0.0192(19) C16 0.072(3) 0.063(3) 0.071(3) -0.040(3) 0.017(3) -0.024(3) C17 0.057(3) 0.045(2) 0.060(3) -0.023(2) 0.004(2) -0.016(2) C18 0.054(3) 0.048(3) 0.052(2) -0.018(2) -0.001(2) -0.018(2) C19 0.056(3) 0.063(3) 0.066(3) -0.028(3) 0.009(2) -0.016(2) C20 0.060(3) 0.058(3) 0.065(3) -0.015(2) -0.001(2) -0.024(2) C21 0.044(3) 0.120(5) 0.095(4) -0.068(4) -0.001(3) -0.008(3) C22 0.059(3) 0.066(3) 0.064(3) -0.038(3) 0.001(2) -0.015(2) C23 0.062(3) 0.057(3) 0.054(3) -0.031(2) -0.003(2) -0.011(2) C24 0.062(3) 0.078(4) 0.069(3) -0.042(3) 0.008(3) -0.022(3) C25 0.068(3) 0.075(4) 0.063(3) -0.036(3) -0.004(3) -0.007(3) C26 0.078(4) 0.052(4) 0.196(8) -0.026(4) 0.032(5) -0.022(3) C27 0.065(3) 0.057(3) 0.049(3) -0.015(2) -0.005(2) -0.011(2) C28 0.065(3) 0.062(3) 0.057(3) -0.027(2) 0.006(2) -0.016(2) C29 0.066(3) 0.079(4) 0.074(4) -0.037(3) 0.023(3) -0.022(3) C30 0.069(4) 0.079(4) 0.062(3) -0.023(3) -0.001(3) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N12 1.988(3) 2_566 ? Zn1 N3 2.033(3) . ? Zn1 N7 2.060(3) . ? Zn1 N6 2.180(3) . ? Zn1 N2 2.329(3) . ? Zn2 N19 2.028(4) . ? Zn2 N15 2.058(4) . ? Zn2 N23 2.139(4) . ? Zn2 N22 2.146(4) . ? Zn2 N14 2.429(4) . ? Zn2 N18 2.435(4) . ? P1 N1 1.660(4) . ? P1 N9 1.672(3) . ? P1 N5 1.680(4) . ? P1 S1 1.9194(16) . ? P2 N17 1.665(4) . ? P2 N13 1.677(4) . ? P2 N21 1.677(4) . ? P2 S2 1.9204(17) . ? N1 N2 1.384(4) . ? N1 C1 1.452(6) . ? N2 C2 1.271(5) . ? N3 C4 1.314(5) . ? N3 C3 1.380(5) . ? N4 C4 1.320(6) . ? N4 C5 1.357(6) . ? N4 H4N 0.98(7) . ? N5 N6 1.384(5) . ? N5 C6 1.436(6) . ? N6 C7 1.287(5) . ? N7 C9 1.302(6) . ? N7 C8 1.377(5) . ? N8 C9 1.335(6) . ? N8 C10 1.358(7) . ? N8 H8N 0.82(5) . ? N9 N10 1.404(4) . ? N9 C11 1.464(5) . ? N10 C12 1.280(5) . ? N11 C14 1.346(5) . ? N11 C13 1.376(5) . ? N11 H11N 0.87(5) . ? N12 C14 1.305(5) . ? N12 C15 1.377(5) . ? N12 Zn1 1.988(3) 2_566 ? N13 N14 1.381(5) . ? N13 C16 1.444(6) . ? N14 C17 1.281(5) . ? N15 C19 1.310(6) . ? N15 C18 1.379(6) . ? N16 C19 1.342(6) . ? N16 C20 1.363(7) . ? N16 H16N 0.92(6) . ? N17 N18 1.389(5) . ? N17 C21 1.440(6) . ? N18 C22 1.284(6) . ? N19 C24 1.317(6) . ? N19 C23 1.379(6) . ? N20 C24 1.335(7) . ? N20 C25 1.351(7) . ? N20 H20N 0.84(7) . ? N21 N22 1.404(5) . ? N21 C26 1.456(7) . ? N22 C27 1.281(6) . ? N23 C29 1.328(6) . ? N23 C28 1.394(6) . ? N24 C29 1.314(7) . ? N24 C30 1.355(7) . ? N24 H24N 0.93(2) . ? N25 O1A 1.19(3) . ? N25 O2 1.229(5) . ? N25 O3 1.239(5) . ? N25 O1 1.25(2) . ? N26 O5 1.228(5) . ? N26 O6 1.229(5) . ? N26 O4 1.251(5) . ? N27 O8 1.237(5) . ? N27 O9 1.238(5) . ? N27 O7 1.251(5) . ? N28 O12 1.193(6) . ? N28 O10 1.211(6) . ? N28 O11 1.254(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.429(5) . ? C2 H2A 0.9300 . ? C3 C5 1.360(6) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.439(6) . ? C7 H7A 0.9300 . ? C8 C10 1.352(6) . ? C9 H9N 0.9300 . ? C10 H10 0.9300 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.449(5) . ? C12 H12 0.9300 . ? C13 C15 1.349(5) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.437(6) . ? C17 H17 0.9300 . ? C18 C20 1.367(6) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.426(7) . ? C22 H22 0.9300 . ? C23 C25 1.369(7) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.437(7) . ? C27 H27 0.9300 . ? C28 C30 1.346(7) . ? C29 H29 0.9300 . ? C30 H30 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 N12 Zn1 N3 100.26(13) 2_566 . ? N12 Zn1 N7 108.73(14) 2_566 . ? N3 Zn1 N7 101.70(14) . . ? N12 Zn1 N6 125.48(13) 2_566 . ? N3 Zn1 N6 132.20(13) . . ? N7 Zn1 N6 78.08(14) . . ? N12 Zn1 N2 100.30(12) 2_566 . ? N3 Zn1 N2 75.79(12) . . ? N7 Zn1 N2 150.77(13) . . ? N6 Zn1 N2 82.46(12) . . ? N19 Zn2 N15 97.20(16) . . ? N19 Zn2 N23 101.74(16) . . ? N15 Zn2 N23 94.39(16) . . ? N19 Zn2 N22 130.49(16) . . ? N15 Zn2 N22 132.28(15) . . ? N23 Zn2 N22 76.42(15) . . ? N19 Zn2 N14 132.78(15) . . ? N15 Zn2 N14 72.80(14) . . ? N23 Zn2 N14 124.59(15) . . ? N22 Zn2 N14 74.81(13) . . ? N19 Zn2 N18 73.44(14) . . ? N15 Zn2 N18 120.69(14) . . ? N23 Zn2 N18 144.83(15) . . ? N22 Zn2 N18 80.92(14) . . ? N14 Zn2 N18 73.24(13) . . ? N1 P1 N9 104.45(17) . . ? N1 P1 N5 108.18(18) . . ? N9 P1 N5 100.53(18) . . ? N1 P1 S1 112.56(13) . . ? N9 P1 S1 117.62(14) . . ? N5 P1 S1 112.42(14) . . ? N17 P2 N13 108.2(2) . . ? N17 P2 N21 107.3(2) . . ? N13 P2 N21 104.8(2) . . ? N17 P2 S2 111.07(15) . . ? N13 P2 S2 112.79(14) . . ? N21 P2 S2 112.29(15) . . ? N2 N1 C1 119.5(3) . . ? N2 N1 P1 115.4(3) . . ? C1 N1 P1 125.0(3) . . ? C2 N2 N1 120.1(3) . . ? C2 N2 Zn1 110.8(3) . . ? N1 N2 Zn1 128.7(2) . . ? C4 N3 C3 105.6(4) . . ? C4 N3 Zn1 138.1(3) . . ? C3 N3 Zn1 115.7(3) . . ? C4 N4 C5 108.8(4) . . ? C4 N4 H4N 129(4) . . ? C5 N4 H4N 122(4) . . ? N6 N5 C6 119.7(4) . . ? N6 N5 P1 118.3(3) . . ? C6 N5 P1 122.0(3) . . ? C7 N6 N5 119.8(4) . . ? C7 N6 Zn1 113.0(3) . . ? N5 N6 Zn1 126.7(2) . . ? C9 N7 C8 106.0(4) . . ? C9 N7 Zn1 140.4(3) . . ? C8 N7 Zn1 113.7(3) . . ? C9 N8 C10 107.8(4) . . ? C9 N8 H8N 122(4) . . ? C10 N8 H8N 130(4) . . ? N10 N9 C11 119.6(3) . . ? N10 N9 P1 112.2(3) . . ? C11 N9 P1 117.9(3) . . ? C12 N10 N9 118.2(3) . . ? C14 N11 C13 107.3(4) . . ? C14 N11 H11N 127(3) . . ? C13 N11 H11N 125(3) . . ? C14 N12 C15 105.4(3) . . ? C14 N12 Zn1 131.1(3) . 2_566 ? C15 N12 Zn1 123.4(3) . 2_566 ? N14 N13 C16 120.2(4) . . ? N14 N13 P2 115.3(3) . . ? C16 N13 P2 124.5(3) . . ? C17 N14 N13 120.1(4) . . ? C17 N14 Zn2 111.6(3) . . ? N13 N14 Zn2 127.1(3) . . ? C19 N15 C18 105.9(4) . . ? C19 N15 Zn2 135.0(4) . . ? C18 N15 Zn2 119.1(3) . . ? C19 N16 C20 108.0(4) . . ? C19 N16 H16N 123(4) . . ? C20 N16 H16N 129(4) . . ? N18 N17 C21 119.7(4) . . ? N18 N17 P2 114.1(3) . . ? C21 N17 P2 126.2(3) . . ? C22 N18 N17 120.5(4) . . ? C22 N18 Zn2 110.2(3) . . ? N17 N18 Zn2 128.9(3) . . ? C24 N19 C23 106.4(4) . . ? C24 N19 Zn2 134.1(3) . . ? C23 N19 Zn2 118.2(3) . . ? C24 N20 C25 107.7(5) . . ? C24 N20 H20N 127(5) . . ? C25 N20 H20N 125(5) . . ? N22 N21 C26 111.5(4) . . ? N22 N21 P2 118.6(3) . . ? C26 N21 P2 116.1(4) . . ? C27 N22 N21 114.7(4) . . ? C27 N22 Zn2 117.2(3) . . ? N21 N22 Zn2 128.1(3) . . ? C29 N23 C28 103.5(4) . . ? C29 N23 Zn2 144.5(4) . . ? C28 N23 Zn2 111.1(3) . . ? C29 N24 C30 107.4(5) . . ? C29 N24 H24N 118(4) . . ? C30 N24 H24N 132(4) . . ? O1A N25 O2 118(2) . . ? O1A N25 O3 119.4(18) . . ? O2 N25 O3 120.7(5) . . ? O1A N25 O1 24(2) . . ? O2 N25 O1 119.1(11) . . ? O3 N25 O1 119.1(12) . . ? O5 N26 O6 120.7(4) . . ? O5 N26 O4 120.2(4) . . ? O6 N26 O4 119.1(4) . . ? O8 N27 O9 120.5(4) . . ? O8 N27 O7 118.9(4) . . ? O9 N27 O7 120.5(4) . . ? O12 N28 O10 125.2(7) . . ? O12 N28 O11 118.7(6) . . ? O10 N28 O11 116.1(5) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 C2 C3 117.5(4) . . ? N2 C2 H2A 121.3 . . ? C3 C2 H2A 121.3 . . ? C5 C3 N3 109.0(4) . . ? C5 C3 C2 131.8(4) . . ? N3 C3 C2 119.2(3) . . ? N3 C4 N4 111.1(4) . . ? N3 C4 H4A 124.5 . . ? N4 C4 H4A 124.5 . . ? N4 C5 C3 105.5(4) . . ? N4 C5 H5A 127.2 . . ? C3 C5 H5A 127.2 . . ? N5 C6 H6A 109.5 . . ? N5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N6 C7 C8 117.5(4) . . ? N6 C7 H7A 121.2 . . ? C8 C7 H7A 121.2 . . ? C10 C8 N7 109.0(4) . . ? C10 C8 C7 133.5(4) . . ? N7 C8 C7 117.5(4) . . ? N7 C9 N8 111.2(4) . . ? N7 C9 H9N 124.4 . . ? N8 C9 H9N 124.4 . . ? C8 C10 N8 106.1(4) . . ? C8 C10 H10 127.0 . . ? N8 C10 H10 127.0 . . ? N9 C11 H11A 109.5 . . ? N9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N10 C12 C13 119.3(4) . . ? N10 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C15 C13 N11 105.4(4) . . ? C15 C13 C12 129.6(4) . . ? N11 C13 C12 125.0(4) . . ? N12 C14 N11 111.6(4) . . ? N12 C14 H14 124.2 . . ? N11 C14 H14 124.2 . . ? C13 C15 N12 110.4(4) . . ? C13 C15 H15 124.8 . . ? N12 C15 H15 124.8 . . ? N13 C16 H16A 109.5 . . ? N13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N14 C17 C18 116.0(4) . . ? N14 C17 H17 122.0 . . ? C18 C17 H17 122.0 . . ? C20 C18 N15 109.3(4) . . ? C20 C18 C17 131.2(5) . . ? N15 C18 C17 119.4(4) . . ? N15 C19 N16 111.2(5) . . ? N15 C19 H19 124.4 . . ? N16 C19 H19 124.4 . . ? N16 C20 C18 105.6(5) . . ? N16 C20 H20 127.2 . . ? C18 C20 H20 127.2 . . ? N17 C21 H21A 109.5 . . ? N17 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N17 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N18 C22 C23 116.2(4) . . ? N18 C22 H22 121.9 . . ? C23 C22 H22 121.9 . . ? C25 C23 N19 107.8(4) . . ? C25 C23 C22 132.0(5) . . ? N19 C23 C22 120.2(4) . . ? N19 C24 N20 111.0(5) . . ? N19 C24 H24 124.5 . . ? N20 C24 H24 124.5 . . ? N20 C25 C23 107.0(5) . . ? N20 C25 H25 126.5 . . ? C23 C25 H25 126.5 . . ? N21 C26 H26A 109.5 . . ? N21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N22 C27 C28 115.3(4) . . ? N22 C27 H27 122.4 . . ? C28 C27 H27 122.4 . . ? C30 C28 N23 109.5(5) . . ? C30 C28 C27 131.9(5) . . ? N23 C28 C27 118.5(4) . . ? N24 C29 N23 112.9(5) . . ? N24 C29 H29 123.6 . . ? N23 C29 H29 123.6 . . ? C28 C30 N24 106.8(5) . . ? C28 C30 H30 126.6 . . ? N24 C30 H30 126.6 . . ? 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 N9 P1 N1 N2 -62.2(3) . . . . ? N5 P1 N1 N2 44.2(3) . . . . ? S1 P1 N1 N2 169.1(2) . . . . ? N9 P1 N1 C1 121.8(4) . . . . ? N5 P1 N1 C1 -131.8(4) . . . . ? S1 P1 N1 C1 -6.9(4) . . . . ? C1 N1 N2 C2 1.3(6) . . . . ? P1 N1 N2 C2 -175.0(3) . . . . ? C1 N1 N2 Zn1 -171.3(3) . . . . ? P1 N1 N2 Zn1 12.4(4) . . . . ? N12 Zn1 N2 C2 -89.4(3) 2_566 . . . ? N3 Zn1 N2 C2 8.7(3) . . . . ? N7 Zn1 N2 C2 97.4(4) . . . . ? N6 Zn1 N2 C2 145.8(3) . . . . ? N12 Zn1 N2 N1 83.8(3) 2_566 . . . ? N3 Zn1 N2 N1 -178.1(3) . . . . ? N7 Zn1 N2 N1 -89.5(4) . . . . ? N6 Zn1 N2 N1 -41.0(3) . . . . ? N12 Zn1 N3 C4 -80.2(4) 2_566 . . . ? N7 Zn1 N3 C4 31.6(4) . . . . ? N6 Zn1 N3 C4 116.0(4) . . . . ? N2 Zn1 N3 C4 -178.3(4) . . . . ? N12 Zn1 N3 C3 89.7(3) 2_566 . . . ? N7 Zn1 N3 C3 -158.6(3) . . . . ? N6 Zn1 N3 C3 -74.1(3) . . . . ? N2 Zn1 N3 C3 -8.5(3) . . . . ? N1 P1 N5 N6 -69.5(3) . . . . ? N9 P1 N5 N6 39.6(3) . . . . ? S1 P1 N5 N6 165.5(3) . . . . ? N1 P1 N5 C6 108.9(4) . . . . ? N9 P1 N5 C6 -142.0(4) . . . . ? S1 P1 N5 C6 -16.0(5) . . . . ? C6 N5 N6 C7 21.6(6) . . . . ? P1 N5 N6 C7 -160.0(3) . . . . ? C6 N5 N6 Zn1 -149.6(4) . . . . ? P1 N5 N6 Zn1 28.9(4) . . . . ? N12 Zn1 N6 C7 108.3(3) 2_566 . . . ? N3 Zn1 N6 C7 -91.4(3) . . . . ? N7 Zn1 N6 C7 3.7(3) . . . . ? N2 Zn1 N6 C7 -154.4(3) . . . . ? N12 Zn1 N6 N5 -80.0(3) 2_566 . . . ? N3 Zn1 N6 N5 80.3(4) . . . . ? N7 Zn1 N6 N5 175.3(3) . . . . ? N2 Zn1 N6 N5 17.3(3) . . . . ? N12 Zn1 N7 C9 54.3(6) 2_566 . . . ? N3 Zn1 N7 C9 -50.9(6) . . . . ? N6 Zn1 N7 C9 178.0(6) . . . . ? N2 Zn1 N7 C9 -132.6(5) . . . . ? N12 Zn1 N7 C8 -125.0(3) 2_566 . . . ? N3 Zn1 N7 C8 129.8(3) . . . . ? N6 Zn1 N7 C8 -1.3(3) . . . . ? N2 Zn1 N7 C8 48.0(5) . . . . ? N1 P1 N9 N10 -42.9(3) . . . . ? N5 P1 N9 N10 -155.0(3) . . . . ? S1 P1 N9 N10 82.7(3) . . . . ? N1 P1 N9 C11 171.9(3) . . . . ? N5 P1 N9 C11 59.9(4) . . . . ? S1 P1 N9 C11 -62.5(3) . . . . ? C11 N9 N10 C12 -10.7(5) . . . . ? P1 N9 N10 C12 -155.2(3) . . . . ? N17 P2 N13 N14 -51.3(4) . . . . ? N21 P2 N13 N14 62.9(3) . . . . ? S2 P2 N13 N14 -174.6(3) . . . . ? N17 P2 N13 C16 129.9(4) . . . . ? N21 P2 N13 C16 -115.8(4) . . . . ? S2 P2 N13 C16 6.6(4) . . . . ? C16 N13 N14 C17 -5.7(6) . . . . ? P2 N13 N14 C17 175.5(3) . . . . ? C16 N13 N14 Zn2 160.3(3) . . . . ? P2 N13 N14 Zn2 -18.5(5) . . . . ? N19 Zn2 N14 C17 -93.3(3) . . . . ? N15 Zn2 N14 C17 -9.5(3) . . . . ? N23 Zn2 N14 C17 73.9(3) . . . . ? N22 Zn2 N14 C17 135.0(3) . . . . ? N18 Zn2 N14 C17 -140.1(3) . . . . ? N19 Zn2 N14 N13 99.8(4) . . . . ? N15 Zn2 N14 N13 -176.4(4) . . . . ? N23 Zn2 N14 N13 -93.1(4) . . . . ? N22 Zn2 N14 N13 -32.0(3) . . . . ? N18 Zn2 N14 N13 52.9(3) . . . . ? N19 Zn2 N15 C19 -43.5(5) . . . . ? N23 Zn2 N15 C19 58.9(5) . . . . ? N22 Zn2 N15 C19 134.5(4) . . . . ? N14 Zn2 N15 C19 -176.2(5) . . . . ? N18 Zn2 N15 C19 -118.5(4) . . . . ? N19 Zn2 N15 C18 139.7(3) . . . . ? N23 Zn2 N15 C18 -117.9(3) . . . . ? N22 Zn2 N15 C18 -42.2(4) . . . . ? N14 Zn2 N15 C18 7.1(3) . . . . ? N18 Zn2 N15 C18 64.7(4) . . . . ? N13 P2 N17 N18 66.1(4) . . . . ? N21 P2 N17 N18 -46.5(4) . . . . ? S2 P2 N17 N18 -169.6(3) . . . . ? N13 P2 N17 C21 -114.1(5) . . . . ? N21 P2 N17 C21 133.3(5) . . . . ? S2 P2 N17 C21 10.2(5) . . . . ? C21 N17 N18 C22 -1.2(7) . . . . ? P2 N17 N18 C22 178.6(4) . . . . ? C21 N17 N18 Zn2 170.7(4) . . . . ? P2 N17 N18 Zn2 -9.5(5) . . . . ? N19 Zn2 N18 C22 -10.5(3) . . . . ? N15 Zn2 N18 C22 78.1(4) . . . . ? N23 Zn2 N18 C22 -97.5(4) . . . . ? N22 Zn2 N18 C22 -147.7(3) . . . . ? N14 Zn2 N18 C22 135.5(3) . . . . ? N19 Zn2 N18 N17 176.9(4) . . . . ? N15 Zn2 N18 N17 -94.5(4) . . . . ? N23 Zn2 N18 N17 90.0(4) . . . . ? N22 Zn2 N18 N17 39.7(4) . . . . ? N14 Zn2 N18 N17 -37.1(4) . . . . ? N15 Zn2 N19 C24 55.8(5) . . . . ? N23 Zn2 N19 C24 -40.3(5) . . . . ? N22 Zn2 N19 C24 -122.4(5) . . . . ? N14 Zn2 N19 C24 128.9(5) . . . . ? N18 Zn2 N19 C24 175.7(5) . . . . ? N15 Zn2 N19 C23 -108.6(4) . . . . ? N23 Zn2 N19 C23 155.4(4) . . . . ? N22 Zn2 N19 C23 73.3(4) . . . . ? N14 Zn2 N19 C23 -35.4(4) . . . . ? N18 Zn2 N19 C23 11.4(3) . . . . ? N17 P2 N21 N22 72.4(4) . . . . ? N13 P2 N21 N22 -42.5(4) . . . . ? S2 P2 N21 N22 -165.3(3) . . . . ? N17 P2 N21 C26 -64.7(5) . . . . ? N13 P2 N21 C26 -179.6(5) . . . . ? S2 P2 N21 C26 57.6(5) . . . . ? C26 N21 N22 C27 -70.5(6) . . . . ? P2 N21 N22 C27 150.6(4) . . . . ? C26 N21 N22 Zn2 109.3(5) . . . . ? P2 N21 N22 Zn2 -29.6(5) . . . . ? N19 Zn2 N22 C27 103.8(4) . . . . ? N15 Zn2 N22 C27 -73.6(4) . . . . ? N23 Zn2 N22 C27 9.9(4) . . . . ? N14 Zn2 N22 C27 -122.3(4) . . . . ? N18 Zn2 N22 C27 162.8(4) . . . . ? N19 Zn2 N22 N21 -76.0(4) . . . . ? N15 Zn2 N22 N21 106.5(4) . . . . ? N23 Zn2 N22 N21 -170.0(4) . . . . ? N14 Zn2 N22 N21 57.9(3) . . . . ? N18 Zn2 N22 N21 -17.1(3) . . . . ? N19 Zn2 N23 C29 54.1(7) . . . . ? N15 Zn2 N23 C29 -44.2(7) . . . . ? N22 Zn2 N23 C29 -176.7(7) . . . . ? N14 Zn2 N23 C29 -116.3(6) . . . . ? N18 Zn2 N23 C29 132.0(6) . . . . ? N19 Zn2 N23 C28 -139.7(3) . . . . ? N15 Zn2 N23 C28 122.0(3) . . . . ? N22 Zn2 N23 C28 -10.5(3) . . . . ? N14 Zn2 N23 C28 49.9(4) . . . . ? N18 Zn2 N23 C28 -61.9(4) . . . . ? N1 N2 C2 C3 178.9(3) . . . . ? Zn1 N2 C2 C3 -7.3(4) . . . . ? C4 N3 C3 C5 -0.9(5) . . . . ? Zn1 N3 C3 C5 -173.9(3) . . . . ? C4 N3 C3 C2 -178.9(4) . . . . ? Zn1 N3 C3 C2 8.1(5) . . . . ? N2 C2 C3 C5 -177.1(5) . . . . ? N2 C2 C3 N3 0.3(6) . . . . ? C3 N3 C4 N4 0.9(5) . . . . ? Zn1 N3 C4 N4 171.4(3) . . . . ? C5 N4 C4 N3 -0.6(5) . . . . ? C4 N4 C5 C3 0.0(5) . . . . ? N3 C3 C5 N4 0.6(5) . . . . ? C2 C3 C5 N4 178.2(4) . . . . ? N5 N6 C7 C8 -177.7(4) . . . . ? Zn1 N6 C7 C8 -5.4(5) . . . . ? C9 N7 C8 C10 -0.2(6) . . . . ? Zn1 N7 C8 C10 179.4(3) . . . . ? C9 N7 C8 C7 179.4(4) . . . . ? Zn1 N7 C8 C7 -1.0(5) . . . . ? N6 C7 C8 C10 -176.0(5) . . . . ? N6 C7 C8 N7 4.5(7) . . . . ? C8 N7 C9 N8 0.1(6) . . . . ? Zn1 N7 C9 N8 -179.3(4) . . . . ? C10 N8 C9 N7 0.0(6) . . . . ? N7 C8 C10 N8 0.2(6) . . . . ? C7 C8 C10 N8 -179.3(5) . . . . ? C9 N8 C10 C8 -0.1(6) . . . . ? N9 N10 C12 C13 -174.5(3) . . . . ? C14 N11 C13 C15 -0.7(4) . . . . ? C14 N11 C13 C12 176.4(4) . . . . ? N10 C12 C13 C15 178.1(4) . . . . ? N10 C12 C13 N11 1.8(6) . . . . ? C15 N12 C14 N11 -0.7(5) . . . . ? Zn1 N12 C14 N11 -177.4(3) 2_566 . . . ? C13 N11 C14 N12 0.9(5) . . . . ? N11 C13 C15 N12 0.3(5) . . . . ? C12 C13 C15 N12 -176.6(4) . . . . ? C14 N12 C15 C13 0.2(5) . . . . ? Zn1 N12 C15 C13 177.2(3) 2_566 . . . ? N13 N14 C17 C18 178.0(4) . . . . ? Zn2 N14 C17 C18 10.0(5) . . . . ? C19 N15 C18 C20 0.3(5) . . . . ? Zn2 N15 C18 C20 177.9(3) . . . . ? C19 N15 C18 C17 177.7(4) . . . . ? Zn2 N15 C18 C17 -4.7(5) . . . . ? N14 C17 C18 C20 171.9(5) . . . . ? N14 C17 C18 N15 -4.8(6) . . . . ? C18 N15 C19 N16 0.4(5) . . . . ? Zn2 N15 C19 N16 -176.6(3) . . . . ? C20 N16 C19 N15 -1.0(6) . . . . ? C19 N16 C20 C18 1.2(5) . . . . ? N15 C18 C20 N16 -0.9(5) . . . . ? C17 C18 C20 N16 -177.8(5) . . . . ? N17 N18 C22 C23 -179.0(4) . . . . ? Zn2 N18 C22 C23 7.7(5) . . . . ? C24 N19 C23 C25 -0.6(6) . . . . ? Zn2 N19 C23 C25 167.7(3) . . . . ? C24 N19 C23 C22 179.4(5) . . . . ? Zn2 N19 C23 C22 -12.3(6) . . . . ? N18 C22 C23 C25 -178.5(5) . . . . ? N18 C22 C23 N19 1.5(7) . . . . ? C23 N19 C24 N20 0.7(6) . . . . ? Zn2 N19 C24 N20 -164.9(4) . . . . ? C25 N20 C24 N19 -0.6(6) . . . . ? C24 N20 C25 C23 0.2(6) . . . . ? N19 C23 C25 N20 0.2(6) . . . . ? C22 C23 C25 N20 -179.8(5) . . . . ? N21 N22 C27 C28 173.1(4) . . . . ? Zn2 N22 C27 C28 -6.8(6) . . . . ? C29 N23 C28 C30 -0.7(6) . . . . ? Zn2 N23 C28 C30 -172.5(4) . . . . ? C29 N23 C28 C27 -177.0(5) . . . . ? Zn2 N23 C28 C27 11.2(6) . . . . ? N22 C27 C28 C30 -178.6(6) . . . . ? N22 C27 C28 N23 -3.2(7) . . . . ? C30 N24 C29 N23 -0.1(7) . . . . ? C28 N23 C29 N24 0.5(6) . . . . ? Zn2 N23 C29 N24 167.2(5) . . . . ? N23 C28 C30 N24 0.6(7) . . . . ? C27 C28 C30 N24 176.3(5) . . . . ? C29 N24 C30 C28 -0.3(7) . . . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 28.44 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.738 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.089 # Attachment 'vc.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 687000' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H21 Co N14 O6 P S' _chemical_formula_weight 615.42 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.207(3) _cell_length_b 17.697(4) _cell_length_c 30.929(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7229(3) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour light-red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3780 _exptl_absorpt_coefficient_mu 0.931 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.768 _exptl_absorpt_correction_T_max 1.000 _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 Smart Apex' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37027 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0598 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.01 _reflns_number_total 12543 _reflns_number_gt 11689 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+146.8356P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.49(3) _refine_ls_number_reflns 12543 _refine_ls_number_parameters 1026 _refine_ls_number_restraints 1636 _refine_ls_R_factor_all 0.1001 _refine_ls_R_factor_gt 0.0945 _refine_ls_wR_factor_ref 0.2233 _refine_ls_wR_factor_gt 0.2178 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.986 _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 Co1 Co 0.78488(12) 0.71637(8) 0.14766(4) 0.0208(3) Uani 1 1 d . . . S1 S 0.7913(3) 0.52369(17) 0.01437(10) 0.0414(8) Uani 1 1 d . . . P1 P 0.78925(19) 0.59194(13) 0.06225(8) 0.0129(5) Uani 1 1 d . . . C11 C 0.9779(8) 0.5395(6) 0.0818(3) 0.027(2) Uani 1 1 d U . . H11A H 0.9693 0.5175 0.0530 0.040 Uiso 1 1 calc R . . H11B H 0.9712 0.4997 0.1037 0.040 Uiso 1 1 calc R . . H11C H 1.0451 0.5626 0.0840 0.040 Uiso 1 1 calc R . . N12 N 0.9013(6) 0.5964(5) 0.0889(3) 0.0147(15) Uani 1 1 d U . . N13 N 0.8981(6) 0.6330(5) 0.1283(2) 0.0125(14) Uani 1 1 d U . . C14 C 0.9672(8) 0.6172(6) 0.1561(3) 0.0175(18) Uani 1 1 d U . . H14 H 1.0189 0.5812 0.1504 0.021 Uiso 1 1 calc R . . C15 C 0.9618(9) 0.6571(6) 0.1965(3) 0.0273(18) Uani 1 1 d U . . N16 N 0.8868(8) 0.7101(6) 0.2006(3) 0.0317(18) Uani 1 1 d U . . C17 C 0.8955(11) 0.7366(8) 0.2411(4) 0.040(2) Uani 1 1 d U . . H17 H 0.8546 0.7748 0.2538 0.048 Uiso 1 1 calc R . . N18 N 0.9744(9) 0.6988(6) 0.2613(3) 0.045(2) Uani 1 1 d U . . H18 H 0.9948 0.7061 0.2880 0.054 Uiso 1 1 calc R . . C19 C 1.0147(10) 0.6492(7) 0.2333(4) 0.036(2) Uani 1 1 d U . . H19 H 1.0693 0.6155 0.2385 0.043 Uiso 1 1 calc R . . C21 C 0.7606(11) 0.7021(7) 0.0015(4) 0.036(3) Uani 1 1 d U . . H21A H 0.7537 0.6566 -0.0163 0.054 Uiso 1 1 calc R . . H21B H 0.8234 0.7283 -0.0061 0.054 Uiso 1 1 calc R . . H21C H 0.7028 0.7356 -0.0037 0.054 Uiso 1 1 calc R . . N22 N 0.7631(6) 0.6807(5) 0.0470(2) 0.0150(16) Uani 1 1 d U . . N23 N 0.7739(6) 0.7374(4) 0.0777(2) 0.0130(15) Uani 1 1 d U . . C24 C 0.7765(8) 0.8062(5) 0.0664(3) 0.0199(18) Uani 1 1 d U . . H24 H 0.7732 0.8209 0.0369 0.024 Uiso 1 1 calc R . . C25 C 0.7846(10) 0.8601(6) 0.1005(4) 0.0328(19) Uani 1 1 d U . . N26 N 0.8020(9) 0.8338(5) 0.1425(3) 0.0356(19) Uani 1 1 d U . . C27 C 0.8110(11) 0.8941(7) 0.1684(4) 0.039(2) Uani 1 1 d U . . H27 H 0.8207 0.8921 0.1988 0.047 Uiso 1 1 calc R . . N28 N 0.8043(10) 0.9586(6) 0.1447(3) 0.044(2) Uani 1 1 d U . . H28 H 0.8071 1.0051 0.1547 0.053 Uiso 1 1 calc R . . C29 C 0.7922(12) 0.9378(7) 0.1017(4) 0.043(2) Uani 1 1 d U . . H29 H 0.7897 0.9710 0.0776 0.052 Uiso 1 1 calc R . . C31 C 0.6339(9) 0.5032(6) 0.0957(3) 0.027(2) Uani 1 1 d U . . H31A H 0.6548 0.4719 0.0712 0.041 Uiso 1 1 calc R . . H31B H 0.5637 0.5196 0.0916 0.041 Uiso 1 1 calc R . . H31C H 0.6391 0.4738 0.1225 0.041 Uiso 1 1 calc R . . N32 N 0.7003(6) 0.5700(5) 0.0986(3) 0.0182(16) Uani 1 1 d U . . N33 N 0.6818(7) 0.6222(5) 0.1321(3) 0.0212(16) Uani 1 1 d U . . C34 C 0.6058(8) 0.6119(6) 0.1573(3) 0.0244(19) Uani 1 1 d U . . H34 H 0.5594 0.5713 0.1542 0.029 Uiso 1 1 calc R . . C35 C 0.5979(9) 0.6692(7) 0.1913(4) 0.0318(19) Uani 1 1 d U . . N36 N 0.6634(8) 0.7292(5) 0.1905(3) 0.0345(19) Uani 1 1 d U . . C37 C 0.6367(11) 0.7695(7) 0.2246(4) 0.044(2) Uani 1 1 d U . . H37 H 0.6690 0.8153 0.2328 0.052 Uiso 1 1 calc R . . N38 N 0.5574(10) 0.7382(7) 0.2469(4) 0.051(2) Uani 1 1 d U . . H38 H 0.5283 0.7567 0.2702 0.061 Uiso 1 1 calc R . . C39 C 0.5326(11) 0.6735(8) 0.2263(4) 0.043(2) Uani 1 1 d U . . H39 H 0.4813 0.6384 0.2341 0.051 Uiso 1 1 calc R . . Co2 Co 0.26572(12) 0.78282(8) 0.18312(4) 0.0262(4) Uani 1 1 d . . . S2 S 0.1915(2) 0.97296(18) 0.31342(9) 0.0293(6) Uani 1 1 d . . . P2 P 0.2197(2) 0.90484(16) 0.26704(9) 0.0210(6) Uani 1 1 d . . . C41 C 0.3873(13) 0.9909(8) 0.2535(5) 0.057(4) Uani 1 1 d U . . H41A H 0.3594 1.0157 0.2792 0.086 Uiso 1 1 calc R . . H41B H 0.3807 1.0246 0.2286 0.086 Uiso 1 1 calc R . . H41C H 0.4590 0.9794 0.2584 0.086 Uiso 1 1 calc R . . N42 N 0.3316(9) 0.9203(6) 0.2452(3) 0.041(2) Uani 1 1 d U . . N43 N 0.3593(8) 0.8771(5) 0.2094(3) 0.0305(19) Uani 1 1 d U . . C44 C 0.4382(9) 0.8937(6) 0.1873(4) 0.030(2) Uani 1 1 d U . . H44 H 0.4838 0.9324 0.1959 0.036 Uiso 1 1 calc R . . C45 C 0.4533(9) 0.8503(7) 0.1489(4) 0.0294(19) Uani 1 1 d U . . N46 N 0.3828(8) 0.7926(6) 0.1406(3) 0.0361(19) Uani 1 1 d U . . C47 C 0.4241(11) 0.7709(9) 0.1002(4) 0.048(2) Uani 1 1 d U . . H47 H 0.3954 0.7314 0.0834 0.057 Uiso 1 1 calc R . . N48 N 0.4990(9) 0.8059(7) 0.0883(4) 0.046(2) Uani 1 1 d U . . H48 H 0.5320 0.7976 0.0641 0.055 Uiso 1 1 calc R . . C49 C 0.5236(10) 0.8585(8) 0.1175(4) 0.038(2) Uani 1 1 d U . . H49 H 0.5780 0.8936 0.1164 0.046 Uiso 1 1 calc R . . C51 C 0.0556(13) 0.9659(9) 0.2255(5) 0.057(4) Uani 1 1 d U . . H51A H 0.0595 0.9971 0.2516 0.086 Uiso 1 1 calc R . . H51B H -0.0087 0.9384 0.2252 0.086 Uiso 1 1 calc R . . H51C H 0.0598 0.9984 0.1999 0.086 Uiso 1 1 calc R . . N52 N 0.1385(8) 0.9128(6) 0.2251(3) 0.037(2) Uani 1 1 d U . . N53 N 0.1465(7) 0.8625(5) 0.1910(3) 0.0321(19) Uani 1 1 d U . . C54 C 0.0775(9) 0.8647(7) 0.1604(4) 0.032(2) Uani 1 1 d U . . H54 H 0.0224 0.8992 0.1601 0.039 Uiso 1 1 calc R . . C55 C 0.0952(9) 0.8080(6) 0.1266(4) 0.0283(19) Uani 1 1 d U . . N56 N 0.1646(7) 0.7596(6) 0.1322(3) 0.0293(18) Uani 1 1 d U . . C57 C 0.1614(10) 0.7123(8) 0.0976(4) 0.042(2) Uani 1 1 d U . . H57 H 0.2051 0.6704 0.0931 0.051 Uiso 1 1 calc R . . N58 N 0.0881(8) 0.7335(6) 0.0710(3) 0.039(2) Uani 1 1 d U . . H58 H 0.0721 0.7108 0.0466 0.046 Uiso 1 1 calc R . . C59 C 0.0420(9) 0.7950(7) 0.0870(4) 0.033(2) Uani 1 1 d U . . H59 H -0.0125 0.8231 0.0750 0.039 Uiso 1 1 calc R . . C61 C 0.2336(11) 0.7939(8) 0.3262(4) 0.043(3) Uani 1 1 d U . . H61A H 0.2133 0.8367 0.3443 0.065 Uiso 1 1 calc R . . H61B H 0.3052 0.7823 0.3313 0.065 Uiso 1 1 calc R . . H61C H 0.1923 0.7497 0.3335 0.065 Uiso 1 1 calc R . . N62 N 0.2193(8) 0.8124(5) 0.2820(3) 0.0272(18) Uani 1 1 d U . . N63 N 0.2428(6) 0.7605(5) 0.2521(3) 0.0206(16) Uani 1 1 d U . . C64 C 0.2553(9) 0.6907(6) 0.2630(4) 0.028(2) Uani 1 1 d U . . H64 H 0.2493 0.6751 0.2923 0.034 Uiso 1 1 calc R . . C65 C 0.2780(12) 0.6388(8) 0.2302(5) 0.047(2) Uani 1 1 d U . . N66 N 0.2999(11) 0.6670(7) 0.1897(4) 0.055(2) Uani 1 1 d U . . C67 C 0.3422(14) 0.6115(9) 0.1637(6) 0.062(3) Uani 1 1 d U . . H67 H 0.3653 0.6183 0.1349 0.074 Uiso 1 1 calc R . . N68 N 0.3453(11) 0.5456(8) 0.1863(5) 0.066(3) Uani 1 1 d U . . H68 H 0.3713 0.5023 0.1778 0.079 Uiso 1 1 calc R . . C69 C 0.2948(14) 0.5621(9) 0.2291(5) 0.062(3) Uani 1 1 d U . . H69 H 0.2779 0.5265 0.2509 0.074 Uiso 1 1 calc R . . Co3 Co 0.29342(8) 0.21816(7) 0.01550(4) 0.0104(3) Uani 1 1 d . . . S3 S 0.2414(5) 0.0264(2) 0.14734(10) 0.083(2) Uani 1 1 d . . . P3 P 0.2609(3) 0.09621(17) 0.10079(9) 0.0397(9) Uani 1 1 d . . . C71 C 0.4471(11) 0.0273(7) 0.0906(4) 0.036(3) Uani 1 1 d U . . H71A H 0.4294 0.0025 0.1179 0.054 Uiso 1 1 calc R . . H71B H 0.5153 0.0489 0.0928 0.054 Uiso 1 1 calc R . . H71C H 0.4455 -0.0099 0.0671 0.054 Uiso 1 1 calc R . . N72 N 0.3717(8) 0.0895(5) 0.0812(3) 0.0289(19) Uani 1 1 d U . . N73 N 0.3926(7) 0.1281(5) 0.0426(3) 0.0198(16) Uani 1 1 d U . . C74 C 0.4668(8) 0.1095(5) 0.0196(3) 0.0190(17) Uani 1 1 d U . . H74 H 0.5145 0.0724 0.0284 0.023 Uiso 1 1 calc R . . C75 C 0.4747(7) 0.1487(5) -0.0218(3) 0.0145(15) Uani 1 1 d U . . N76 N 0.4030(5) 0.2008(4) -0.0326(2) 0.0095(14) Uani 1 1 d U . . C77 C 0.4218(7) 0.2223(6) -0.0728(3) 0.0167(16) Uani 1 1 d U . . H77 H 0.3830 0.2583 -0.0885 0.020 Uiso 1 1 calc R . . N78 N 0.5036(6) 0.1860(5) -0.0884(3) 0.0217(16) Uani 1 1 d U . . H78 H 0.5296 0.1912 -0.1145 0.026 Uiso 1 1 calc R . . C79 C 0.5392(7) 0.1392(6) -0.0560(3) 0.0183(17) Uani 1 1 d U . . H79 H 0.5967 0.1069 -0.0572 0.022 Uiso 1 1 calc R . . C81 C 0.0974(11) 0.0247(7) 0.0607(4) 0.041(3) Uani 1 1 d U . . H81A H 0.1080 -0.0087 0.0856 0.061 Uiso 1 1 calc R . . H81B H 0.0990 -0.0051 0.0340 0.061 Uiso 1 1 calc R . . H81C H 0.0314 0.0496 0.0634 0.061 Uiso 1 1 calc R . . N82 N 0.1771(8) 0.0816(5) 0.0595(3) 0.0274(19) Uani 1 1 d U . . N83 N 0.1748(7) 0.1332(5) 0.0258(3) 0.0212(16) Uani 1 1 d U . . C84 C 0.1062(8) 0.1309(6) -0.0034(3) 0.0175(17) Uani 1 1 d U . . H84 H 0.0550 0.0931 -0.0031 0.021 Uiso 1 1 calc R . . C85 C 0.1097(7) 0.1877(5) -0.0367(3) 0.0148(16) Uani 1 1 d U . . N86 N 0.1820(6) 0.2444(4) -0.0327(3) 0.0135(15) Uani 1 1 d U . . C87 C 0.1676(6) 0.2889(6) -0.0671(3) 0.0135(16) Uani 1 1 d U . . H87 H 0.2056 0.3333 -0.0731 0.016 Uiso 1 1 calc R . . N88 N 0.0924(6) 0.2626(5) -0.0918(3) 0.0182(16) Uani 1 1 d U . . H88 H 0.0705 0.2831 -0.1159 0.022 Uiso 1 1 calc R . . C89 C 0.0556(7) 0.1983(5) -0.0730(3) 0.0167(17) Uani 1 1 d U . . H89 H 0.0024 0.1673 -0.0836 0.020 Uiso 1 1 calc R . . C91 C 0.2585(10) 0.2087(7) 0.1621(4) 0.038(3) Uani 1 1 d U . . H91A H 0.2440 0.1652 0.1807 0.056 Uiso 1 1 calc R . . H91B H 0.2114 0.2498 0.1689 0.056 Uiso 1 1 calc R . . H91C H 0.3281 0.2258 0.1672 0.056 Uiso 1 1 calc R . . N92 N 0.2466(8) 0.1865(5) 0.1158(3) 0.0290(19) Uani 1 1 d U . . N93 N 0.2660(7) 0.2405(5) 0.0843(3) 0.0204(17) Uani 1 1 d U . . C94 C 0.2805(7) 0.3111(5) 0.0964(3) 0.0139(16) Uani 1 1 d U . . H94 H 0.2748 0.3267 0.1257 0.017 Uiso 1 1 calc R . . C95 C 0.3050(6) 0.3623(5) 0.0626(3) 0.0066(14) Uani 1 1 d U . . N96 N 0.3190(5) 0.3333(4) 0.0216(2) 0.0060(13) Uani 1 1 d U . . C97 C 0.3425(7) 0.3912(5) -0.0030(3) 0.0149(17) Uani 1 1 d U . . H97 H 0.3564 0.3883 -0.0331 0.018 Uiso 1 1 calc R . . N98 N 0.3439(6) 0.4552(5) 0.0203(3) 0.0191(15) Uani 1 1 d U . . H98 H 0.3592 0.5004 0.0104 0.023 Uiso 1 1 calc R . . C99 C 0.3178(7) 0.4388(5) 0.0620(3) 0.0123(16) Uani 1 1 d U . . H99 H 0.3102 0.4730 0.0855 0.015 Uiso 1 1 calc R . . N1 N 0.0787(7) 0.6242(5) 0.3537(3) 0.030(2) Uani 1 1 d DU . . O11 O 0.1098(6) 0.6043(4) 0.3900(2) 0.0293(17) Uani 1 1 d DU . . O12 O 0.0294(7) 0.6832(5) 0.3486(3) 0.040(2) Uani 1 1 d DU . . O13 O 0.1029(7) 0.5861(5) 0.3211(2) 0.0365(19) Uani 1 1 d DU . . N2 N 0.0939(7) 0.3996(5) -0.1676(3) 0.032(2) Uani 1 1 d DU . . O21 O 0.0744(8) 0.4578(5) -0.1894(3) 0.052(2) Uani 1 1 d DU . . O22 O 0.1724(6) 0.3971(4) -0.1451(2) 0.0330(19) Uani 1 1 d DU . . O23 O 0.0332(7) 0.3452(5) -0.1677(3) 0.046(2) Uani 1 1 d DU . . N3 N 0.4485(7) 0.6306(4) 0.0193(2) 0.0244(18) Uani 1 1 d DU . . O31 O 0.4292(6) 0.5910(3) -0.0132(2) 0.0230(15) Uani 1 1 d DU . . O32 O 0.4863(7) 0.6952(4) 0.0142(3) 0.0346(19) Uani 1 1 d DU . . O33 O 0.4285(7) 0.6067(4) 0.0565(2) 0.0347(19) Uani 1 1 d DU . . N4 N 0.6265(8) 0.9054(5) -0.0010(3) 0.040(2) Uani 1 1 d DU . . O41 O 0.6201(8) 0.9592(5) 0.0250(3) 0.053(2) Uani 1 1 d DU . . O42 O 0.5663(7) 0.8511(5) 0.0045(3) 0.046(2) Uani 1 1 d DU . . O43 O 0.6943(6) 0.9027(5) -0.0288(3) 0.043(2) Uani 1 1 d DU . . N5 N 0.8827(9) 0.8926(5) 0.3188(3) 0.046(2) Uani 1 1 d DU . . O51 O 0.9232(7) 0.8315(4) 0.3266(3) 0.042(2) Uani 1 1 d DU . . O52 O 0.8735(7) 0.9404(5) 0.3482(3) 0.042(2) Uani 1 1 d DU . . O53 O 0.8533(10) 0.9050(6) 0.2807(3) 0.069(3) Uani 1 1 d DU . . N6 N 0.5606(15) 0.8794(9) 0.3252(7) 0.042(3) Uiso 0.50 1 d PDU A 1 O61 O 0.5480(7) 0.9294(5) 0.3516(3) 0.0419(19) Uani 1 1 d DU . . O62 O 0.5065(7) 0.8209(5) 0.3242(3) 0.0440(19) Uani 1 1 d DU . . O63 O 0.6410(10) 0.8874(9) 0.3042(5) 0.032(3) Uiso 0.50 1 d PDU A 1 N6' N 0.5458(19) 0.8842(9) 0.3200(5) 0.042(3) Uiso 0.50 1 d PDU A 2 O63' O 0.5564(14) 0.9017(10) 0.2808(4) 0.044(4) Uiso 0.50 1 d PDU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0444(8) 0.0114(6) 0.0068(6) -0.0009(5) 0.0077(6) 0.0020(7) S1 0.078(2) 0.0250(14) 0.0210(14) -0.0185(12) -0.0066(16) 0.0041(16) P1 0.0122(11) 0.0130(11) 0.0134(11) -0.0044(9) 0.0020(10) 0.0008(10) C11 0.024(4) 0.034(5) 0.022(4) 0.006(4) 0.003(4) 0.010(4) N12 0.011(3) 0.018(3) 0.015(3) -0.001(3) -0.005(3) 0.000(3) N13 0.009(3) 0.018(3) 0.011(3) -0.001(3) -0.006(3) -0.003(3) C14 0.015(3) 0.022(3) 0.015(3) 0.003(3) -0.003(3) -0.009(3) C15 0.033(3) 0.031(3) 0.018(3) 0.003(3) -0.007(3) -0.007(3) N16 0.040(4) 0.035(4) 0.019(3) 0.001(3) -0.003(3) -0.010(3) C17 0.049(4) 0.044(4) 0.027(4) -0.004(3) -0.004(4) -0.007(4) N18 0.054(4) 0.051(4) 0.030(4) 0.004(3) -0.013(3) -0.003(4) C19 0.042(4) 0.043(4) 0.023(4) 0.005(3) -0.009(3) -0.007(4) C21 0.057(5) 0.030(5) 0.022(4) 0.002(4) -0.004(4) 0.002(4) N22 0.021(3) 0.016(3) 0.008(3) -0.006(3) -0.005(3) -0.001(3) N23 0.011(3) 0.014(3) 0.013(3) -0.001(2) -0.002(2) 0.003(2) C24 0.025(4) 0.015(3) 0.019(3) 0.004(3) 0.002(3) -0.007(3) C25 0.049(4) 0.024(3) 0.026(3) 0.002(3) -0.001(3) 0.001(3) N26 0.057(4) 0.023(3) 0.026(3) -0.004(3) -0.006(3) -0.004(3) C27 0.062(4) 0.027(4) 0.029(4) -0.003(3) 0.002(4) -0.005(4) N28 0.071(4) 0.027(3) 0.034(4) -0.006(3) 0.001(4) 0.002(4) C29 0.064(4) 0.031(4) 0.034(4) 0.001(3) 0.003(4) 0.006(4) C31 0.032(5) 0.031(5) 0.019(4) 0.006(4) -0.009(4) -0.015(4) N32 0.022(3) 0.016(3) 0.017(3) 0.000(3) 0.006(3) -0.002(3) N33 0.026(3) 0.021(3) 0.017(3) 0.005(3) 0.007(3) 0.004(3) C34 0.025(4) 0.027(4) 0.021(3) 0.013(3) 0.008(3) 0.008(3) C35 0.038(4) 0.033(3) 0.025(3) 0.012(3) 0.017(3) 0.017(3) N36 0.049(4) 0.028(3) 0.026(3) 0.009(3) 0.015(3) 0.017(3) C37 0.064(4) 0.035(4) 0.032(4) 0.012(3) 0.020(4) 0.015(4) N38 0.066(4) 0.046(4) 0.039(4) 0.014(3) 0.027(4) 0.021(4) C39 0.047(4) 0.044(4) 0.037(4) 0.014(4) 0.020(4) 0.018(4) Co2 0.0523(10) 0.0117(7) 0.0147(6) 0.0009(5) -0.0140(6) -0.0030(7) S2 0.0217(14) 0.0401(16) 0.0260(14) -0.0170(12) 0.0034(11) -0.0069(12) P2 0.0216(13) 0.0225(13) 0.0189(12) -0.0048(11) -0.0071(11) -0.0063(12) C41 0.069(6) 0.058(6) 0.044(5) -0.021(5) 0.020(5) -0.021(5) N42 0.055(4) 0.042(4) 0.026(4) -0.013(3) 0.010(4) -0.021(4) N43 0.043(4) 0.028(3) 0.021(3) -0.003(3) 0.004(3) -0.016(3) C44 0.041(4) 0.026(4) 0.024(4) 0.000(3) 0.006(3) -0.009(3) C45 0.036(4) 0.030(3) 0.021(3) 0.002(3) 0.004(3) 0.011(3) N46 0.037(4) 0.040(4) 0.031(3) -0.015(3) -0.010(3) 0.014(3) C47 0.049(4) 0.054(4) 0.040(4) -0.017(4) -0.015(4) 0.010(4) N48 0.043(4) 0.057(4) 0.039(4) -0.006(3) -0.009(3) 0.024(4) C49 0.043(4) 0.041(4) 0.031(4) 0.004(3) 0.003(4) 0.020(4) C51 0.063(6) 0.050(6) 0.059(6) -0.015(5) -0.011(5) 0.013(5) N52 0.040(4) 0.032(4) 0.038(4) -0.009(3) -0.023(3) 0.010(3) N53 0.036(4) 0.026(3) 0.034(4) -0.004(3) -0.022(3) -0.003(3) C54 0.033(4) 0.027(4) 0.037(4) 0.004(3) -0.011(3) -0.003(3) C55 0.031(3) 0.029(3) 0.024(3) 0.002(3) -0.005(3) -0.011(3) N56 0.025(3) 0.038(4) 0.024(3) -0.002(3) 0.000(3) -0.019(3) C57 0.043(4) 0.049(4) 0.035(4) 0.000(4) -0.002(4) -0.009(4) N58 0.034(4) 0.050(4) 0.032(4) -0.001(3) 0.001(3) -0.005(3) C59 0.025(4) 0.039(4) 0.033(4) 0.004(3) -0.013(3) -0.011(3) C61 0.063(6) 0.035(5) 0.032(5) 0.002(4) 0.007(4) 0.000(5) N62 0.036(4) 0.026(4) 0.020(3) 0.005(3) 0.007(3) -0.003(3) N63 0.022(3) 0.017(3) 0.023(3) 0.005(3) 0.003(3) -0.007(3) C64 0.028(4) 0.026(4) 0.032(4) 0.011(3) -0.002(3) -0.002(3) C65 0.060(4) 0.035(4) 0.046(4) 0.007(3) -0.013(4) 0.004(4) N66 0.075(4) 0.041(4) 0.049(4) -0.004(3) -0.014(4) 0.008(4) C67 0.076(5) 0.052(4) 0.058(4) 0.000(4) -0.013(4) 0.004(4) N68 0.080(5) 0.052(4) 0.067(4) -0.003(4) -0.012(4) 0.001(4) C69 0.076(5) 0.046(4) 0.063(4) 0.005(4) -0.013(4) 0.001(4) Co3 0.0078(5) 0.0115(6) 0.0118(6) 0.0000(5) 0.0060(5) -0.0011(5) S3 0.204(6) 0.0254(17) 0.0187(15) 0.0063(13) 0.029(3) -0.026(3) P3 0.092(3) 0.0153(14) 0.0118(13) 0.0011(11) 0.0205(15) -0.0084(16) C71 0.058(6) 0.026(5) 0.024(4) 0.008(4) 0.001(4) 0.010(4) N72 0.047(4) 0.022(3) 0.018(3) 0.001(3) -0.002(3) 0.002(3) N73 0.029(3) 0.015(3) 0.015(3) 0.001(3) -0.009(3) 0.004(3) C74 0.021(3) 0.015(3) 0.020(3) 0.004(3) -0.009(3) 0.002(3) C75 0.011(3) 0.012(3) 0.020(3) -0.002(3) -0.003(3) 0.001(3) N76 0.0092(16) 0.0094(16) 0.0098(16) -0.0003(10) 0.0003(10) 0.0011(10) C77 0.014(3) 0.020(3) 0.016(3) 0.000(3) 0.003(3) 0.001(3) N78 0.020(3) 0.024(3) 0.021(3) -0.001(3) 0.006(3) 0.001(3) C79 0.007(3) 0.020(3) 0.028(4) -0.002(3) 0.001(3) 0.002(3) C81 0.055(6) 0.028(5) 0.038(5) 0.004(4) 0.018(5) -0.017(4) N82 0.046(4) 0.018(3) 0.019(3) 0.002(3) 0.010(3) -0.011(3) N83 0.032(3) 0.014(3) 0.017(3) 0.001(3) 0.013(3) -0.008(3) C84 0.018(3) 0.019(3) 0.015(3) -0.002(3) 0.010(3) -0.008(3) C85 0.011(3) 0.016(3) 0.017(3) -0.009(3) 0.000(3) -0.004(3) N86 0.011(3) 0.014(3) 0.016(3) -0.003(3) -0.005(2) -0.009(2) C87 0.008(3) 0.019(3) 0.014(3) -0.006(3) -0.003(3) 0.005(3) N88 0.016(3) 0.025(3) 0.014(3) -0.009(3) -0.006(3) 0.001(3) C89 0.010(3) 0.021(3) 0.019(3) -0.005(3) -0.001(3) -0.001(3) C91 0.060(6) 0.031(5) 0.021(4) 0.000(4) 0.009(4) 0.003(4) N92 0.045(4) 0.022(4) 0.020(3) -0.001(3) 0.010(3) -0.003(3) N93 0.027(3) 0.022(3) 0.012(3) 0.001(3) 0.006(3) -0.006(3) C94 0.012(3) 0.018(3) 0.012(3) -0.002(3) 0.001(3) -0.004(3) C95 0.002(3) 0.009(3) 0.008(3) -0.004(2) 0.002(2) 0.000(2) N96 0.0057(15) 0.0062(15) 0.0061(15) 0.0002(10) -0.0012(10) 0.0011(10) C97 0.019(3) 0.014(3) 0.012(3) 0.000(3) -0.008(3) -0.006(3) N98 0.027(3) 0.014(3) 0.016(3) 0.000(3) -0.007(3) -0.003(3) C99 0.013(3) 0.013(3) 0.011(3) -0.002(3) -0.003(3) 0.002(3) N1 0.034(4) 0.037(4) 0.020(4) 0.001(3) -0.006(3) -0.010(4) O11 0.042(4) 0.035(4) 0.011(3) 0.006(3) -0.003(3) -0.011(3) O12 0.050(4) 0.043(4) 0.029(4) -0.003(3) -0.016(3) 0.011(4) O13 0.052(4) 0.033(4) 0.024(3) -0.004(3) -0.007(3) 0.002(3) N2 0.042(4) 0.030(4) 0.025(4) -0.001(3) -0.007(4) 0.026(4) O21 0.069(5) 0.045(4) 0.042(4) 0.016(4) -0.011(4) 0.034(4) O22 0.046(4) 0.029(4) 0.024(3) 0.004(3) -0.023(3) 0.010(3) O23 0.051(5) 0.050(4) 0.038(4) -0.003(4) -0.016(4) 0.003(4) N3 0.044(4) 0.010(3) 0.019(4) 0.000(3) 0.000(3) -0.012(3) O31 0.047(4) 0.008(3) 0.014(3) -0.004(3) 0.001(3) -0.010(3) O32 0.059(4) 0.016(3) 0.029(4) -0.012(3) 0.013(3) -0.029(3) O33 0.063(5) 0.019(3) 0.022(3) -0.001(3) -0.003(3) -0.014(3) N4 0.045(4) 0.042(4) 0.033(4) 0.008(4) -0.015(4) -0.013(4) O41 0.056(5) 0.049(4) 0.055(5) -0.013(4) -0.007(4) -0.014(4) O42 0.060(5) 0.044(4) 0.033(4) 0.004(3) -0.008(4) -0.029(4) O43 0.039(4) 0.043(4) 0.047(4) 0.007(4) -0.008(4) -0.016(4) N5 0.057(5) 0.040(4) 0.042(4) 0.003(4) -0.022(4) 0.000(4) O51 0.062(5) 0.032(4) 0.032(4) 0.000(3) -0.026(4) 0.004(4) O52 0.037(4) 0.051(4) 0.037(4) -0.009(4) -0.007(3) 0.001(4) O53 0.091(6) 0.059(5) 0.057(5) -0.002(4) -0.028(5) 0.013(5) O61 0.041(3) 0.049(3) 0.036(3) 0.012(3) 0.007(3) 0.006(3) O62 0.044(3) 0.050(4) 0.038(3) 0.013(3) 0.017(3) 0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N36 2.093(9) . ? Co1 N26 2.097(10) . ? Co1 N16 2.122(9) . ? Co1 N13 2.184(8) . ? Co1 N23 2.199(8) . ? Co1 N33 2.205(9) . ? S1 P1 1.911(4) . ? P1 N32 1.672(8) . ? P1 N22 1.676(8) . ? P1 N12 1.696(8) . ? C11 N12 1.443(13) . ? N12 N13 1.382(11) . ? N13 C14 1.286(12) . ? C14 C15 1.436(14) . ? C15 C19 1.344(16) . ? C15 N16 1.369(16) . ? N16 C17 1.343(15) . ? C17 N18 1.388(17) . ? N18 C19 1.342(17) . ? C21 N22 1.459(13) . ? N22 N23 1.388(11) . ? N23 C24 1.268(13) . ? C24 C25 1.427(15) . ? C25 C29 1.379(17) . ? C25 N26 1.398(15) . ? N26 C27 1.340(15) . ? C27 N28 1.359(16) . ? N28 C29 1.387(16) . ? C31 N32 1.474(13) . ? N32 N33 1.408(12) . ? N33 C34 1.283(13) . ? C34 C35 1.466(16) . ? C35 N36 1.370(16) . ? C35 C39 1.384(16) . ? N36 C37 1.321(15) . ? C37 N38 1.371(17) . ? N38 C39 1.352(19) . ? Co2 N46 2.038(11) . ? Co2 N56 2.104(9) . ? Co2 N66 2.108(12) . ? Co2 N53 2.128(10) . ? Co2 N63 2.191(9) . ? Co2 N43 2.229(9) . ? S2 P2 1.910(4) . ? P2 N42 1.647(11) . ? P2 N52 1.690(9) . ? P2 N62 1.699(9) . ? C41 N42 1.474(17) . ? N42 N43 1.394(13) . ? N43 C44 1.280(15) . ? C44 C45 1.428(16) . ? C45 C49 1.352(17) . ? C45 N46 1.406(16) . ? N46 C47 1.414(17) . ? C47 N48 1.224(19) . ? N48 C49 1.337(17) . ? C51 N52 1.443(17) . ? N52 N53 1.385(14) . ? N53 C54 1.314(14) . ? C54 C55 1.467(17) . ? C55 N56 1.266(15) . ? C55 C59 1.431(15) . ? N56 C57 1.361(16) . ? C57 N58 1.324(17) . ? N58 C59 1.342(16) . ? C61 N62 1.419(15) . ? N62 N63 1.340(13) . ? N63 C64 1.291(14) . ? C64 C65 1.403(18) . ? C65 C69 1.37(2) . ? C65 N66 1.377(19) . ? N66 C67 1.39(2) . ? C67 N68 1.36(2) . ? N68 C69 1.51(2) . ? Co3 N96 2.074(7) . ? Co3 N76 2.098(7) . ? Co3 N86 2.147(8) . ? Co3 N93 2.193(8) . ? Co3 N83 2.194(8) . ? Co3 N73 2.226(8) . ? S3 P3 1.915(4) . ? P3 N72 1.588(11) . ? P3 N92 1.674(10) . ? P3 N82 1.711(10) . ? C71 N72 1.513(15) . ? N72 N73 1.404(12) . ? N73 C74 1.256(14) . ? C74 C75 1.458(14) . ? C75 N76 1.363(12) . ? C75 C79 1.369(14) . ? N76 C77 1.325(12) . ? C77 N78 1.347(13) . ? N78 C79 1.385(13) . ? C81 N82 1.457(14) . ? N82 N83 1.386(12) . ? N83 C84 1.280(13) . ? C84 C85 1.441(14) . ? C85 C89 1.344(13) . ? C85 N86 1.391(11) . ? N86 C87 1.335(12) . ? C87 N88 1.336(12) . ? N88 C89 1.366(13) . ? C91 N92 1.495(14) . ? N92 N93 1.389(12) . ? N93 C94 1.318(13) . ? C94 C95 1.421(13) . ? C95 C99 1.364(12) . ? C95 N96 1.380(11) . ? N96 C97 1.313(12) . ? C97 N98 1.342(12) . ? N98 C99 1.367(12) . ? N1 O12 1.240(9) . ? N1 O11 1.246(9) . ? N1 O13 1.254(9) . ? N2 O22 1.249(9) . ? N2 O23 1.253(10) . ? N2 O21 1.257(9) . ? N3 O31 1.252(8) . ? N3 O33 1.254(9) . ? N3 O32 1.258(8) . ? N4 O43 1.243(10) . ? N4 O41 1.248(10) . ? N4 O42 1.258(10) . ? N5 O51 1.231(10) . ? N5 O52 1.250(10) . ? N5 O53 1.258(10) . ? N6 O61 1.216(12) . ? N6 O63 1.253(13) . ? N6 O62 1.257(12) . ? O61 N6' 1.263(12) . ? O62 N6' 1.240(13) . ? N6' O63' 1.259(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N36 Co1 N26 91.3(4) . . ? N36 Co1 N16 90.2(4) . . ? N26 Co1 N16 92.5(4) . . ? N36 Co1 N13 140.5(3) . . ? N26 Co1 N13 125.1(4) . . ? N16 Co1 N13 75.0(3) . . ? N36 Co1 N23 123.6(3) . . ? N26 Co1 N23 76.4(3) . . ? N16 Co1 N23 144.0(3) . . ? N13 Co1 N23 83.7(3) . . ? N36 Co1 N33 75.4(4) . . ? N26 Co1 N33 143.0(4) . . ? N16 Co1 N33 121.4(4) . . ? N13 Co1 N33 81.5(3) . . ? N23 Co1 N33 82.6(3) . . ? N32 P1 N22 105.1(4) . . ? N32 P1 N12 107.3(4) . . ? N22 P1 N12 105.8(4) . . ? N32 P1 S1 112.6(3) . . ? N22 P1 S1 112.2(3) . . ? N12 P1 S1 113.2(3) . . ? N13 N12 C11 118.9(8) . . ? N13 N12 P1 115.0(6) . . ? C11 N12 P1 120.4(7) . . ? C14 N13 N12 117.8(8) . . ? C14 N13 Co1 116.7(7) . . ? N12 N13 Co1 125.5(6) . . ? N13 C14 C15 116.1(10) . . ? C19 C15 N16 111.7(11) . . ? C19 C15 C14 131.3(12) . . ? N16 C15 C14 116.9(9) . . ? C17 N16 C15 105.3(10) . . ? C17 N16 Co1 139.0(9) . . ? C15 N16 Co1 115.1(7) . . ? N16 C17 N18 108.3(12) . . ? C19 N18 C17 108.9(10) . . ? N18 C19 C15 105.8(12) . . ? N23 N22 C21 118.5(8) . . ? N23 N22 P1 117.6(6) . . ? C21 N22 P1 121.2(7) . . ? C24 N23 N22 120.4(8) . . ? C24 N23 Co1 115.7(7) . . ? N22 N23 Co1 123.9(6) . . ? N23 C24 C25 116.1(9) . . ? C29 C25 N26 107.1(10) . . ? C29 C25 C24 133.9(11) . . ? N26 C25 C24 118.4(10) . . ? C27 N26 C25 107.7(10) . . ? C27 N26 Co1 138.9(9) . . ? C25 N26 Co1 112.6(7) . . ? N26 C27 N28 109.9(11) . . ? C27 N28 C29 107.5(10) . . ? C25 C29 N28 107.5(11) . . ? N33 N32 C31 117.8(8) . . ? N33 N32 P1 117.7(6) . . ? C31 N32 P1 124.3(7) . . ? C34 N33 N32 119.3(9) . . ? C34 N33 Co1 117.2(8) . . ? N32 N33 Co1 123.3(6) . . ? N33 C34 C35 113.2(10) . . ? N36 C35 C39 111.5(11) . . ? N36 C35 C34 118.5(9) . . ? C39 C35 C34 130.0(12) . . ? C37 N36 C35 103.6(10) . . ? C37 N36 Co1 140.2(10) . . ? C35 N36 Co1 114.3(7) . . ? N36 C37 N38 112.8(13) . . ? C39 N38 C37 106.8(11) . . ? N38 C39 C35 105.3(12) . . ? N46 Co2 N56 90.9(4) . . ? N46 Co2 N66 89.0(5) . . ? N56 Co2 N66 91.1(4) . . ? N46 Co2 N53 125.4(4) . . ? N56 Co2 N53 75.2(4) . . ? N66 Co2 N53 142.3(5) . . ? N46 Co2 N63 138.5(4) . . ? N56 Co2 N63 127.2(3) . . ? N66 Co2 N63 76.1(4) . . ? N53 Co2 N63 84.6(4) . . ? N46 Co2 N43 75.6(4) . . ? N56 Co2 N43 140.4(4) . . ? N66 Co2 N43 125.0(5) . . ? N53 Co2 N43 82.7(4) . . ? N63 Co2 N43 81.7(3) . . ? N42 P2 N52 103.9(6) . . ? N42 P2 N62 105.9(6) . . ? N52 P2 N62 106.6(5) . . ? N42 P2 S2 112.2(4) . . ? N52 P2 S2 113.6(4) . . ? N62 P2 S2 113.7(3) . . ? N43 N42 C41 118.3(10) . . ? N43 N42 P2 118.1(8) . . ? C41 N42 P2 121.1(9) . . ? C44 N43 N42 120.8(10) . . ? C44 N43 Co2 115.4(8) . . ? N42 N43 Co2 123.7(7) . . ? N43 C44 C45 115.7(11) . . ? C49 C45 N46 113.6(11) . . ? C49 C45 C44 129.4(12) . . ? N46 C45 C44 116.8(10) . . ? C45 N46 C47 96.0(11) . . ? C45 N46 Co2 116.4(7) . . ? C47 N46 Co2 147.1(9) . . ? N48 C47 N46 116.1(13) . . ? C47 N48 C49 110.2(13) . . ? N48 C49 C45 104.1(13) . . ? N53 N52 C51 118.9(10) . . ? N53 N52 P2 118.9(7) . . ? C51 N52 P2 122.0(9) . . ? C54 N53 N52 118.5(10) . . ? C54 N53 Co2 116.8(8) . . ? N52 N53 Co2 124.7(7) . . ? N53 C54 C55 112.4(11) . . ? N56 C55 C59 111.4(11) . . ? N56 C55 C54 118.7(10) . . ? C59 C55 C54 129.8(11) . . ? C55 N56 C57 106.6(10) . . ? C55 N56 Co2 115.5(8) . . ? C57 N56 Co2 136.8(9) . . ? N58 C57 N56 109.8(13) . . ? C57 N58 C59 109.4(11) . . ? N58 C59 C55 102.9(10) . . ? N63 N62 C61 118.3(9) . . ? N63 N62 P2 118.1(7) . . ? C61 N62 P2 119.0(8) . . ? C64 N63 N62 120.3(9) . . ? C64 N63 Co2 114.2(8) . . ? N62 N63 Co2 125.4(6) . . ? N63 C64 C65 117.7(11) . . ? C69 C65 N66 107.6(14) . . ? C69 C65 C64 134.3(14) . . ? N66 C65 C64 117.7(12) . . ? C65 N66 C67 110.7(13) . . ? C65 N66 Co2 113.4(9) . . ? C67 N66 Co2 135.9(11) . . ? N68 C67 N66 108.7(15) . . ? C67 N68 C69 105.7(13) . . ? C65 C69 N68 106.5(14) . . ? N96 Co3 N76 95.5(3) . . ? N96 Co3 N86 87.8(3) . . ? N76 Co3 N86 90.7(3) . . ? N96 Co3 N93 76.3(3) . . ? N76 Co3 N93 145.8(3) . . ? N86 Co3 N93 121.5(3) . . ? N96 Co3 N83 140.9(3) . . ? N76 Co3 N83 119.7(3) . . ? N86 Co3 N83 76.1(3) . . ? N93 Co3 N83 82.2(3) . . ? N96 Co3 N73 125.0(3) . . ? N76 Co3 N73 75.9(3) . . ? N86 Co3 N73 145.1(3) . . ? N93 Co3 N73 82.0(3) . . ? N83 Co3 N73 82.8(3) . . ? N72 P3 N92 106.3(5) . . ? N72 P3 N82 107.5(5) . . ? N92 P3 N82 106.2(5) . . ? N72 P3 S3 111.2(4) . . ? N92 P3 S3 113.1(4) . . ? N82 P3 S3 112.2(4) . . ? N73 N72 C71 112.8(9) . . ? N73 N72 P3 118.0(7) . . ? C71 N72 P3 126.0(8) . . ? C74 N73 N72 120.6(9) . . ? C74 N73 Co3 115.7(7) . . ? N72 N73 Co3 123.6(7) . . ? N73 C74 C75 115.4(9) . . ? N76 C75 C79 109.0(9) . . ? N76 C75 C74 119.2(8) . . ? C79 C75 C74 131.5(9) . . ? C77 N76 C75 107.2(8) . . ? C77 N76 Co3 138.9(6) . . ? C75 N76 Co3 113.8(6) . . ? N76 C77 N78 110.5(9) . . ? C77 N78 C79 107.4(8) . . ? C75 C79 N78 106.0(8) . . ? N83 N82 C81 117.4(10) . . ? N83 N82 P3 118.4(7) . . ? C81 N82 P3 123.5(8) . . ? C84 N83 N82 121.6(8) . . ? C84 N83 Co3 115.2(6) . . ? N82 N83 Co3 123.1(7) . . ? N83 C84 C85 117.3(9) . . ? C89 C85 N86 109.7(9) . . ? C89 C85 C84 132.7(9) . . ? N86 C85 C84 117.6(8) . . ? C87 N86 C85 104.9(7) . . ? C87 N86 Co3 141.1(6) . . ? C85 N86 Co3 112.1(6) . . ? N86 C87 N88 110.8(9) . . ? C87 N88 C89 108.2(8) . . ? C85 C89 N88 106.4(8) . . ? N93 N92 C91 118.1(9) . . ? N93 N92 P3 116.2(7) . . ? C91 N92 P3 120.3(8) . . ? C94 N93 N92 118.7(8) . . ? C94 N93 Co3 114.9(6) . . ? N92 N93 Co3 125.9(6) . . ? N93 C94 C95 115.4(8) . . ? C99 C95 N96 110.0(8) . . ? C99 C95 C94 132.0(8) . . ? N96 C95 C94 118.0(7) . . ? C97 N96 C95 105.8(7) . . ? C97 N96 Co3 138.9(6) . . ? C95 N96 Co3 115.2(5) . . ? N96 C97 N98 110.5(8) . . ? C97 N98 C99 108.9(8) . . ? C95 C99 N98 104.7(8) . . ? O12 N1 O11 121.7(8) . . ? O12 N1 O13 118.9(8) . . ? O11 N1 O13 119.2(8) . . ? O22 N2 O23 120.3(8) . . ? O22 N2 O21 120.0(9) . . ? O23 N2 O21 119.7(9) . . ? O31 N3 O33 120.4(7) . . ? O31 N3 O32 119.2(7) . . ? O33 N3 O32 120.4(7) . . ? O43 N4 O41 121.5(9) . . ? O43 N4 O42 121.3(10) . . ? O41 N4 O42 116.9(10) . . ? O51 N5 O52 119.6(9) . . ? O51 N5 O53 118.2(10) . . ? O52 N5 O53 122.2(10) . . ? O61 N6 O63 112.4(13) . . ? O61 N6 O62 122.5(13) . . ? O63 N6 O62 124.2(13) . . ? N6 O61 N6' 12(2) . . ? N6' O62 N6 12(2) . . ? O62 N6' O63' 111.7(13) . . ? O62 N6' O61 120.0(13) . . ? O63' N6' O61 125.8(14) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.513 _refine_diff_density_min -1.716 _refine_diff_density_rms 0.169 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 687001' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H21 Cl2 N12 Ni O8 P S' _chemical_formula_weight 690.08 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 10.6094(10) _cell_length_b 17.2830(16) _cell_length_c 14.7831(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2710.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour Violet _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 1.114 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8079 _exptl_absorpt_correction_T_max 0.8507 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14839 _diffrn_reflns_av_R_equivalents 0.0734 _diffrn_reflns_av_sigmaI/netI 0.0772 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4240 _reflns_number_gt 3078 _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^)+(0.0544P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(2) _refine_ls_number_reflns 4240 _refine_ls_number_parameters 364 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0874 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1247 _refine_ls_wR_factor_gt 0.1127 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 Ni1 Ni 0.01489(6) 0.03789(4) 0.21568(7) 0.0374(2) Uani 1 1 d . . . P1 P 0.27574(14) 0.14519(9) 0.21898(16) 0.0425(4) Uani 1 1 d . . . S1 S 0.42660(16) 0.20567(11) 0.2183(2) 0.0677(6) Uani 1 1 d . . . N1 N 0.2078(5) 0.1388(3) 0.1156(4) 0.0468(15) Uani 1 1 d . . . N2 N 0.0864(5) 0.1092(3) 0.1139(4) 0.0357(13) Uani 1 1 d . . . N3 N -0.1490(5) 0.0657(3) 0.1448(5) 0.0476(15) Uani 1 1 d . . . N4 N -0.3178(7) 0.0728(4) 0.0590(6) 0.073(2) Uani 1 1 d . . . N5 N 0.1629(5) 0.1816(3) 0.2864(4) 0.0430(14) Uani 1 1 d . . . N6 N 0.0647(5) 0.1303(3) 0.3059(4) 0.0385(14) Uani 1 1 d . . . N7 N -0.0882(6) 0.0109(4) 0.3292(5) 0.0546(17) Uani 1 1 d . . . N8 N -0.2403(7) -0.0086(5) 0.4269(6) 0.078(2) Uani 1 1 d . . . N9 N 0.2974(5) 0.0539(3) 0.2543(4) 0.0453(15) Uani 1 1 d . . . N10 N 0.2026(5) 0.0031(3) 0.2334(4) 0.0358(13) Uani 1 1 d . . . N11 N 0.0087(5) -0.0756(3) 0.1694(4) 0.0463(14) Uani 1 1 d . . . N12 N -0.0192(6) -0.1990(4) 0.1411(6) 0.072(2) Uani 1 1 d . . . C1 C 0.2338(8) 0.1997(5) 0.0489(6) 0.068(2) Uani 1 1 d . . . H1A H 0.2167 0.1805 -0.0108 0.102 Uiso 1 1 calc R . . H1B H 0.3207 0.2148 0.0529 0.102 Uiso 1 1 calc R . . H1C H 0.1811 0.2437 0.0608 0.102 Uiso 1 1 calc R . . C2 C 0.0087(7) 0.1284(4) 0.0540(6) 0.0415(18) Uani 1 1 d . . . H2 H 0.0327 0.1593 0.0054 0.050 Uiso 1 1 calc R . . C3 C -0.1171(7) 0.1013(4) 0.0629(6) 0.049(2) Uani 1 1 d . . . C4 C -0.2205(9) 0.1058(5) 0.0107(6) 0.069(3) Uani 1 1 d . . . H4 H -0.2254 0.1270 -0.0470 0.083 Uiso 1 1 calc R . . C5 C -0.2678(8) 0.0492(5) 0.1378(8) 0.075(3) Uani 1 1 d . . . H5 H -0.3135 0.0237 0.1825 0.090 Uiso 1 1 calc R . . C6 C 0.1930(9) 0.2408(5) 0.3557(7) 0.073(3) Uani 1 1 d . . . H6A H 0.1178 0.2686 0.3714 0.109 Uiso 1 1 calc R . . H6B H 0.2545 0.2762 0.3320 0.109 Uiso 1 1 calc R . . H6C H 0.2263 0.2159 0.4086 0.109 Uiso 1 1 calc R . . C7 C -0.0020(8) 0.1337(5) 0.3791(6) 0.057(2) Uani 1 1 d . . . H7 H 0.0073 0.1732 0.4214 0.069 Uiso 1 1 calc R . . C8 C -0.0920(7) 0.0715(5) 0.3904(5) 0.054(2) Uani 1 1 d . . . C9 C -0.1873(8) 0.0587(7) 0.4491(7) 0.075(3) Uani 1 1 d . . . H9 H -0.2115 0.0909 0.4963 0.090 Uiso 1 1 calc R . . C10 C -0.1771(8) -0.0348(5) 0.3547(6) 0.070(3) Uani 1 1 d . . . H10 H -0.1957 -0.0812 0.3259 0.084 Uiso 1 1 calc R . . C11 C 0.4211(7) 0.0228(5) 0.2764(7) 0.071(3) Uani 1 1 d . . . H11A H 0.4132 -0.0142 0.3245 0.106 Uiso 1 1 calc R . . H11B H 0.4757 0.0641 0.2952 0.106 Uiso 1 1 calc R . . H11C H 0.4561 -0.0021 0.2240 0.106 Uiso 1 1 calc R . . C12 C 0.2225(6) -0.0699(4) 0.2226(6) 0.0484(16) Uani 1 1 d . . . H12 H 0.3004 -0.0925 0.2345 0.058 Uiso 1 1 calc R . . C13 C 0.1174(7) -0.1137(4) 0.1914(5) 0.0479(19) Uani 1 1 d . . . C14 C 0.0973(9) -0.1911(4) 0.1745(6) 0.066(2) Uani 1 1 d . . . H14 H 0.1547 -0.2309 0.1845 0.079 Uiso 1 1 calc R . . C15 C -0.0704(8) -0.1271(4) 0.1390(6) 0.065(2) Uani 1 1 d . . . H15 H -0.1512 -0.1160 0.1185 0.078 Uiso 1 1 calc R . . Cl1 Cl 0.0090(2) 0.61307(11) 0.03733(15) 0.0573(5) Uani 1 1 d . . . Cl2 Cl 0.47675(19) 0.17972(11) 0.86925(15) 0.0570(5) Uani 1 1 d . . . O1 O -0.0954(6) 0.6594(3) 0.0663(5) 0.093(2) Uani 1 1 d . . . O2 O 0.1090(6) 0.6226(4) 0.0948(6) 0.109(3) Uani 1 1 d . . . O3 O 0.0418(13) 0.6336(9) -0.0482(8) 0.206(6) Uani 1 1 d . . . O4 O -0.0297(6) 0.5348(3) 0.0378(7) 0.106(3) Uani 1 1 d . . . O5 O 0.4411(8) 0.2518(4) 0.8971(5) 0.115(3) Uani 1 1 d . . . O6 O 0.5945(9) 0.1849(5) 0.8324(8) 0.154(4) Uani 1 1 d . . . O7 O 0.3973(11) 0.1538(5) 0.8038(6) 0.154(4) Uani 1 1 d . . . O8 O 0.4728(7) 0.1247(5) 0.9409(6) 0.105(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 Ni1 0.0335(4) 0.0318(4) 0.0468(5) 0.0000(5) 0.0064(5) -0.0029(3) P1 0.0339(8) 0.0385(8) 0.0552(11) 0.0009(12) -0.0049(11) -0.0065(7) S1 0.0465(10) 0.0698(12) 0.0868(15) 0.0008(15) -0.0047(16) -0.0259(9) N1 0.042(4) 0.042(3) 0.056(4) 0.005(3) 0.000(3) -0.015(3) N2 0.032(3) 0.030(3) 0.045(4) -0.005(3) -0.001(3) -0.002(2) N3 0.025(3) 0.040(3) 0.077(5) 0.002(3) -0.005(3) -0.001(2) N4 0.051(4) 0.064(5) 0.104(7) -0.018(5) -0.017(4) 0.001(4) N5 0.045(3) 0.032(3) 0.052(4) -0.013(3) -0.010(3) -0.004(3) N6 0.034(3) 0.033(3) 0.048(4) -0.001(3) -0.009(3) 0.004(3) N7 0.051(4) 0.054(4) 0.059(4) 0.012(3) 0.021(3) -0.003(3) N8 0.060(5) 0.087(6) 0.088(6) 0.028(5) 0.023(4) 0.001(4) N9 0.036(3) 0.039(3) 0.061(4) -0.003(3) -0.005(3) -0.001(3) N10 0.039(3) 0.033(3) 0.035(4) 0.000(2) 0.000(2) 0.002(2) N11 0.050(4) 0.033(3) 0.056(4) -0.001(3) 0.007(3) -0.009(3) N12 0.063(5) 0.042(4) 0.112(7) -0.007(4) 0.012(5) -0.012(3) C1 0.073(6) 0.071(6) 0.060(6) 0.018(5) 0.012(5) -0.027(5) C2 0.048(5) 0.037(4) 0.040(5) 0.004(3) 0.005(4) 0.001(3) C3 0.048(5) 0.035(4) 0.065(6) -0.003(4) -0.013(4) -0.004(3) C4 0.068(6) 0.051(5) 0.090(8) -0.005(5) -0.036(5) 0.000(4) C5 0.045(5) 0.058(5) 0.123(9) -0.002(5) -0.001(5) -0.002(4) C6 0.074(6) 0.062(5) 0.082(7) -0.035(5) -0.022(5) -0.005(5) C7 0.060(6) 0.071(6) 0.041(5) -0.012(4) 0.001(4) 0.029(4) C8 0.051(5) 0.056(5) 0.055(6) 0.008(4) 0.008(4) 0.010(4) C9 0.066(6) 0.095(7) 0.065(6) 0.015(5) 0.028(5) 0.019(6) C10 0.054(5) 0.071(6) 0.083(7) 0.021(5) 0.030(5) -0.002(5) C11 0.052(5) 0.060(5) 0.100(7) -0.009(5) -0.028(5) 0.009(4) C12 0.050(4) 0.042(4) 0.053(4) 0.005(5) 0.000(5) 0.006(3) C13 0.066(5) 0.033(4) 0.045(5) -0.003(3) 0.007(3) 0.002(3) C14 0.089(7) 0.034(4) 0.074(6) 0.002(4) 0.011(5) 0.003(4) C15 0.056(5) 0.051(5) 0.089(7) -0.008(5) 0.013(5) -0.018(4) Cl1 0.0662(14) 0.0520(12) 0.0536(13) -0.0072(10) -0.0105(11) 0.0039(10) Cl2 0.0605(12) 0.0534(12) 0.0569(12) -0.0110(10) 0.0000(11) 0.0080(9) O1 0.060(4) 0.057(4) 0.161(7) -0.034(4) -0.021(4) 0.004(3) O2 0.065(4) 0.110(6) 0.151(8) -0.034(5) -0.048(4) 0.006(4) O3 0.266(14) 0.258(15) 0.093(8) 0.053(8) 0.047(9) 0.039(12) O4 0.077(4) 0.057(4) 0.184(8) -0.021(4) -0.059(5) 0.014(3) O5 0.180(8) 0.072(4) 0.095(6) -0.015(4) 0.040(5) 0.021(5) O6 0.114(7) 0.136(7) 0.213(11) 0.022(6) 0.095(7) 0.024(6) O7 0.233(11) 0.114(6) 0.114(7) 0.029(5) -0.080(8) -0.067(7) O8 0.106(6) 0.121(6) 0.089(6) 0.048(5) -0.009(4) 0.035(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 Ni1 N7 2.057(6) . ? Ni1 N11 2.078(5) . ? Ni1 N3 2.086(5) . ? Ni1 N2 2.087(6) . ? Ni1 N10 2.096(5) . ? Ni1 N6 2.147(6) . ? P1 N9 1.677(5) . ? P1 N5 1.680(6) . ? P1 N1 1.693(6) . ? P1 S1 1.912(2) . ? N1 N2 1.386(7) . ? N1 C1 1.470(9) . ? N2 C2 1.254(9) . ? N3 C5 1.297(9) . ? N3 C3 1.400(10) . ? N4 C5 1.343(12) . ? N4 C4 1.378(11) . ? N5 N6 1.398(8) . ? N5 C6 1.483(8) . ? N6 C7 1.294(10) . ? N7 C10 1.287(9) . ? N7 C8 1.384(10) . ? N8 C9 1.332(12) . ? N8 C10 1.340(11) . ? N9 N10 1.371(7) . ? N9 C11 1.456(9) . ? N10 C12 1.290(7) . ? N11 C15 1.303(9) . ? N11 C13 1.368(9) . ? N12 C14 1.338(10) . ? N12 C15 1.357(10) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.421(10) . ? C2 H2 0.9300 . ? C3 C4 1.343(10) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.447(11) . ? C7 H7 0.9300 . ? C8 C9 1.351(11) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.425(9) . ? C12 H12 0.9300 . ? C13 C14 1.378(9) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? Cl1 O3 1.358(11) . ? Cl1 O2 1.369(6) . ? Cl1 O4 1.413(6) . ? Cl1 O1 1.433(6) . ? Cl2 O7 1.358(8) . ? Cl2 O5 1.365(6) . ? Cl2 O6 1.365(8) . ? Cl2 O8 1.424(7) . ? 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 N7 Ni1 N11 92.2(2) . . ? N7 Ni1 N3 91.1(3) . . ? N11 Ni1 N3 91.5(2) . . ? N7 Ni1 N2 156.2(2) . . ? N11 Ni1 N2 109.4(2) . . ? N3 Ni1 N2 78.7(2) . . ? N7 Ni1 N10 109.8(2) . . ? N11 Ni1 N10 78.5(2) . . ? N3 Ni1 N10 157.0(2) . . ? N2 Ni1 N10 85.1(2) . . ? N7 Ni1 N6 78.0(2) . . ? N11 Ni1 N6 156.1(2) . . ? N3 Ni1 N6 110.2(2) . . ? N2 Ni1 N6 85.4(2) . . ? N10 Ni1 N6 84.4(2) . . ? N9 P1 N5 105.4(3) . . ? N9 P1 N1 106.2(3) . . ? N5 P1 N1 104.8(3) . . ? N9 P1 S1 113.6(2) . . ? N5 P1 S1 113.2(2) . . ? N1 P1 S1 112.8(2) . . ? N2 N1 C1 115.3(6) . . ? N2 N1 P1 115.9(5) . . ? C1 N1 P1 118.7(5) . . ? C2 N2 N1 121.7(6) . . ? C2 N2 Ni1 115.3(5) . . ? N1 N2 Ni1 122.8(4) . . ? C5 N3 C3 105.2(8) . . ? C5 N3 Ni1 143.1(7) . . ? C3 N3 Ni1 109.5(4) . . ? C5 N4 C4 106.2(7) . . ? N6 N5 C6 117.1(6) . . ? N6 N5 P1 114.6(4) . . ? C6 N5 P1 121.0(5) . . ? C7 N6 N5 123.4(7) . . ? C7 N6 Ni1 114.8(5) . . ? N5 N6 Ni1 121.8(4) . . ? C10 N7 C8 104.6(7) . . ? C10 N7 Ni1 140.1(6) . . ? C8 N7 Ni1 112.2(5) . . ? C9 N8 C10 106.2(7) . . ? N10 N9 C11 118.4(5) . . ? N10 N9 P1 115.5(4) . . ? C11 N9 P1 122.8(5) . . ? C12 N10 N9 122.3(5) . . ? C12 N10 Ni1 114.9(4) . . ? N9 N10 Ni1 122.8(4) . . ? C15 N11 C13 107.2(6) . . ? C15 N11 Ni1 141.2(6) . . ? C13 N11 Ni1 110.5(4) . . ? C14 N12 C15 106.5(6) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 C2 C3 117.6(7) . . ? N2 C2 H2 121.2 . . ? C3 C2 H2 121.2 . . ? C4 C3 N3 108.9(7) . . ? C4 C3 C2 134.0(8) . . ? N3 C3 C2 116.9(7) . . ? C3 C4 N4 106.9(8) . . ? C3 C4 H4 126.6 . . ? N4 C4 H4 126.6 . . ? N3 C5 N4 112.7(9) . . ? N3 C5 H5 123.7 . . ? N4 C5 H5 123.7 . . ? N5 C6 H6A 109.5 . . ? N5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N6 C7 C8 115.0(8) . . ? N6 C7 H7 122.5 . . ? C8 C7 H7 122.5 . . ? C9 C8 N7 108.5(8) . . ? C9 C8 C7 133.6(9) . . ? N7 C8 C7 117.9(7) . . ? N8 C9 C8 107.5(9) . . ? N8 C9 H9 126.2 . . ? C8 C9 H9 126.2 . . ? N7 C10 N8 113.1(9) . . ? N7 C10 H10 123.4 . . ? N8 C10 H10 123.4 . . ? N9 C11 H11A 109.5 . . ? N9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N10 C12 C13 115.5(6) . . ? N10 C12 H12 122.2 . . ? C13 C12 H12 122.2 . . ? N11 C13 C14 107.1(7) . . ? N11 C13 C12 118.8(6) . . ? C14 C13 C12 134.1(7) . . ? N12 C14 C13 108.0(7) . . ? N12 C14 H14 126.0 . . ? C13 C14 H14 126.0 . . ? N11 C15 N12 111.1(8) . . ? N11 C15 H15 124.4 . . ? N12 C15 H15 124.4 . . ? O3 Cl1 O2 110.3(7) . . ? O3 Cl1 O4 109.2(8) . . ? O2 Cl1 O4 109.7(4) . . ? O3 Cl1 O1 109.3(7) . . ? O2 Cl1 O1 110.2(4) . . ? O4 Cl1 O1 108.0(4) . . ? O7 Cl2 O5 110.1(6) . . ? O7 Cl2 O6 107.8(8) . . ? O5 Cl2 O6 108.3(5) . . ? O7 Cl2 O8 106.9(5) . . ? O5 Cl2 O8 112.2(5) . . ? O6 Cl2 O8 111.5(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.407 _refine_diff_density_min -0.269 _refine_diff_density_rms 0.075 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 687002' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H23 Cd N14 O7 P S' _chemical_formula_weight 686.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.8866(18) _cell_length_b 10.6431(12) _cell_length_c 20.684(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.991(19) _cell_angle_gamma 90.00 _cell_volume 2610.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.748 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 1.044 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Stoe IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16202 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 24.21 _reflns_number_total 4135 _reflns_number_gt 3274 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0412P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4135 _refine_ls_number_parameters 361 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0654 _refine_ls_wR_factor_gt 0.0616 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _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 Cd1 Cd 0.727056(17) 0.41731(2) 0.930323(10) 0.02382(8) Uani 1 1 d . . . S1 S 0.73220(8) 0.91529(8) 0.84179(5) 0.0424(2) Uani 1 1 d . . . P1 P 0.73011(7) 0.74327(8) 0.86917(4) 0.02746(19) Uani 1 1 d . . . N1 N 0.8604(2) 0.6862(2) 0.88653(14) 0.0322(6) Uani 1 1 d . . . N2 N 0.8724(2) 0.5567(2) 0.89183(13) 0.0285(6) Uani 1 1 d . . . N3 N 0.8854(2) 0.3046(3) 0.92051(13) 0.0284(6) Uani 1 1 d . . . N4 N 1.0287(2) 0.1777(3) 0.91731(14) 0.0346(7) Uani 1 1 d . . . H4A H 1.0681 0.1087 0.9195 0.042 Uiso 1 1 calc R . . N5 N 0.6669(2) 0.6493(3) 0.81273(13) 0.0304(6) Uani 1 1 d . . . N6 N 0.6377(2) 0.5307(2) 0.83367(12) 0.0272(6) Uani 1 1 d . . . N7 N 0.6002(2) 0.2903(2) 0.87861(12) 0.0266(6) Uani 1 1 d . . . N8 N 0.4905(2) 0.1442(3) 0.83524(14) 0.0363(7) Uani 1 1 d . . . H8 H 0.4541 0.0736 0.8303 0.044 Uiso 1 1 calc R . . N9 N 0.6601(2) 0.7249(2) 0.93585(12) 0.0280(6) Uani 1 1 d . . . N10 N 0.6850(2) 0.6212(2) 0.97448(12) 0.0259(6) Uani 1 1 d . . . N11 N 0.7128(2) 0.3977(2) 1.03863(12) 0.0256(6) Uani 1 1 d . . . N12 N 0.7050(2) 0.3585(3) 1.14179(13) 0.0313(6) Uani 1 1 d . . . H12A H 0.7107 0.3181 1.1784 0.038 Uiso 1 1 calc R . . C1 C 0.9572(3) 0.7655(4) 0.9036(2) 0.0519(10) Uani 1 1 d . . . H1A H 0.9936 0.7378 0.9445 0.078 Uiso 1 1 calc R . . H1B H 0.9326 0.8519 0.9075 0.078 Uiso 1 1 calc R . . H1C H 1.0101 0.7599 0.8701 0.078 Uiso 1 1 calc R . . C2 C 0.9706(3) 0.5067(3) 0.89434(17) 0.0326(8) Uani 1 1 d . . . H2 H 1.0353 0.5557 0.8897 0.039 Uiso 1 1 calc R . . C3 C 0.9787(3) 0.3723(3) 0.90463(16) 0.0295(7) Uani 1 1 d . . . C4 C 1.0675(3) 0.2929(3) 0.90267(18) 0.0374(8) Uani 1 1 d . . . H4 H 1.1413 0.3138 0.8931 0.045 Uiso 1 1 calc R . . C5 C 0.9192(3) 0.1881(3) 0.92788(16) 0.0305(7) Uani 1 1 d . . . H5 H 0.8729 0.1210 0.9390 0.037 Uiso 1 1 calc R . . C6 C 0.6458(4) 0.6846(4) 0.74484(18) 0.0518(11) Uani 1 1 d . . . H6A H 0.6837 0.6258 0.7178 0.078 Uiso 1 1 calc R . . H6B H 0.6744 0.7687 0.7383 0.078 Uiso 1 1 calc R . . H6C H 0.5654 0.6827 0.7332 0.078 Uiso 1 1 calc R . . C7 C 0.5820(3) 0.4556(3) 0.79556(16) 0.0302(7) Uani 1 1 d . . . H7 H 0.5587 0.4800 0.7530 0.036 Uiso 1 1 calc R . . C8 C 0.5555(3) 0.3324(3) 0.81926(15) 0.0288(7) Uani 1 1 d . . . C9 C 0.4870(3) 0.2409(4) 0.79240(17) 0.0396(8) Uani 1 1 d . . . H9 H 0.4454 0.2442 0.7521 0.047 Uiso 1 1 calc R . . C10 C 0.5594(3) 0.1761(3) 0.88611(16) 0.0301(7) Uani 1 1 d . . . H10 H 0.5767 0.1245 0.9223 0.036 Uiso 1 1 calc R . . C11 C 0.5533(3) 0.7915(3) 0.94264(17) 0.0335(8) Uani 1 1 d . . . H11A H 0.4949 0.7313 0.9513 0.050 Uiso 1 1 calc R . . H11B H 0.5319 0.8363 0.9028 0.050 Uiso 1 1 calc R . . H11C H 0.5625 0.8508 0.9782 0.050 Uiso 1 1 calc R . . C12 C 0.6497(3) 0.6162(3) 1.03153(15) 0.0280(7) Uani 1 1 d . . . H12 H 0.6096 0.6834 1.0485 0.034 Uiso 1 1 calc R . . C13 C 0.6737(2) 0.5034(3) 1.06888(15) 0.0258(7) Uani 1 1 d . . . C14 C 0.6689(3) 0.4785(3) 1.13322(16) 0.0315(8) Uani 1 1 d . . . H14 H 0.6453 0.5335 1.1652 0.038 Uiso 1 1 calc R . . C15 C 0.7303(3) 0.3126(3) 1.08429(16) 0.0292(7) Uani 1 1 d . . . H15 H 0.7570 0.2308 1.0775 0.035 Uiso 1 1 calc R . . N13 N 0.3528(2) -0.1071(3) 0.76370(14) 0.0351(7) Uani 1 1 d . . . O1 O 0.3670(2) -0.0872(2) 0.82320(11) 0.0486(7) Uani 1 1 d . . . O2 O 0.3855(3) -0.0300(3) 0.72470(13) 0.0581(8) Uani 1 1 d . . . O3 O 0.3011(2) -0.2049(2) 0.74426(13) 0.0516(7) Uani 1 1 d . . . N14 N 1.2616(3) 0.0099(3) 0.95123(14) 0.0366(7) Uani 1 1 d . . . O4 O 1.1630(2) -0.0352(3) 0.94249(16) 0.0546(8) Uani 1 1 d . . . O5 O 1.2815(2) 0.1126(2) 0.92685(13) 0.0465(7) Uani 1 1 d . . . O6 O 1.3346(3) -0.0512(3) 0.98235(15) 0.0677(9) Uani 1 1 d . . . O7 O 0.1338(3) 0.0424(3) 0.79245(15) 0.0660(9) Uani 1 1 d D . . H7A H 0.174(4) 0.007(5) 0.836(2) 0.099 Uiso 1 1 d D . . H7B H 0.148(5) 0.142(4) 0.792(3) 0.099 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 Cd1 0.02302(12) 0.02135(13) 0.02745(13) -0.00268(10) 0.00425(8) 0.00070(10) S1 0.0540(5) 0.0206(4) 0.0543(6) 0.0081(4) 0.0153(4) 0.0011(4) P1 0.0316(4) 0.0186(4) 0.0332(5) 0.0019(3) 0.0093(3) 0.0011(4) N1 0.0269(14) 0.0205(15) 0.0501(18) -0.0012(13) 0.0099(12) -0.0019(12) N2 0.0273(14) 0.0222(15) 0.0369(15) -0.0011(11) 0.0093(11) 0.0000(11) N3 0.0265(13) 0.0280(16) 0.0312(15) -0.0018(12) 0.0063(11) 0.0032(12) N4 0.0313(15) 0.0307(17) 0.0423(17) -0.0009(13) 0.0058(12) 0.0114(13) N5 0.0382(15) 0.0244(15) 0.0290(15) 0.0040(12) 0.0039(12) -0.0012(13) N6 0.0289(14) 0.0232(14) 0.0301(15) 0.0024(12) 0.0062(12) 0.0008(12) N7 0.0261(13) 0.0235(15) 0.0301(15) -0.0014(11) 0.0009(11) 0.0004(12) N8 0.0383(16) 0.0268(16) 0.0432(18) -0.0033(13) -0.0011(13) -0.0095(13) N9 0.0318(14) 0.0234(15) 0.0296(14) 0.0028(11) 0.0081(11) 0.0065(12) N10 0.0265(13) 0.0214(14) 0.0303(14) -0.0012(11) 0.0051(11) 0.0014(11) N11 0.0272(13) 0.0214(14) 0.0285(14) -0.0016(11) 0.0035(11) -0.0021(11) N12 0.0377(15) 0.0270(15) 0.0290(15) 0.0042(12) 0.0012(12) -0.0018(13) C1 0.044(2) 0.035(2) 0.075(3) -0.007(2) -0.0056(19) -0.0064(19) C2 0.0221(16) 0.032(2) 0.045(2) -0.0024(16) 0.0095(14) -0.0034(15) C3 0.0246(16) 0.0276(18) 0.0369(19) -0.0017(14) 0.0062(14) 0.0036(14) C4 0.0272(17) 0.036(2) 0.049(2) -0.0005(17) 0.0068(15) 0.0030(16) C5 0.0315(17) 0.0270(19) 0.0335(18) -0.0019(14) 0.0063(14) 0.0024(15) C6 0.086(3) 0.034(2) 0.034(2) 0.0072(17) 0.003(2) 0.000(2) C7 0.0327(17) 0.0296(19) 0.0282(17) 0.0018(14) 0.0004(14) 0.0041(14) C8 0.0266(16) 0.0277(18) 0.0316(18) -0.0037(14) -0.0002(13) 0.0018(14) C9 0.045(2) 0.035(2) 0.037(2) -0.0009(16) -0.0085(16) -0.0051(17) C10 0.0302(17) 0.0268(19) 0.0334(18) -0.0009(14) 0.0027(14) 0.0007(14) C11 0.0246(16) 0.037(2) 0.0389(19) 0.0043(16) 0.0056(14) 0.0075(15) C12 0.0297(16) 0.0221(17) 0.0330(18) -0.0050(13) 0.0080(14) 0.0034(13) C13 0.0257(16) 0.0212(17) 0.0313(17) -0.0017(13) 0.0089(13) 0.0004(14) C14 0.0344(17) 0.0292(19) 0.0320(18) -0.0037(15) 0.0092(14) 0.0007(15) C15 0.0278(16) 0.0232(18) 0.0364(19) 0.0008(15) 0.0006(14) -0.0015(14) N13 0.0396(16) 0.0308(17) 0.0346(17) 0.0008(13) -0.0001(13) -0.0036(14) O1 0.0741(18) 0.0416(15) 0.0291(13) -0.0011(12) -0.0033(12) -0.0169(15) O2 0.081(2) 0.0518(18) 0.0419(16) 0.0084(14) 0.0089(14) -0.0252(16) O3 0.0748(18) 0.0359(15) 0.0429(15) -0.0050(12) -0.0039(13) -0.0180(14) N14 0.0420(17) 0.0290(18) 0.0383(17) -0.0062(14) -0.0014(13) 0.0114(15) O4 0.0387(15) 0.0316(15) 0.094(2) 0.0107(14) 0.0118(14) 0.0042(12) O5 0.0466(15) 0.0332(16) 0.0598(17) 0.0052(12) 0.0038(12) -0.0037(12) O6 0.082(2) 0.0474(18) 0.068(2) -0.0123(15) -0.0390(17) 0.0268(16) O7 0.068(2) 0.078(2) 0.0507(18) -0.0081(17) -0.0029(15) 0.0097(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N7 2.241(3) . ? Cd1 N3 2.253(3) . ? Cd1 N11 2.268(3) . ? Cd1 N10 2.419(3) . ? Cd1 N2 2.451(3) . ? Cd1 N6 2.507(3) . ? S1 P1 1.9170(12) . ? P1 N9 1.671(3) . ? P1 N5 1.675(3) . ? P1 N1 1.679(3) . ? N1 N2 1.390(4) . ? N1 C1 1.450(5) . ? N2 C2 1.280(4) . ? N3 C5 1.309(4) . ? N3 C3 1.380(4) . ? N4 C5 1.340(4) . ? N4 C4 1.351(5) . ? N5 N6 1.386(4) . ? N5 C6 1.458(4) . ? N6 C7 1.275(4) . ? N7 C10 1.322(4) . ? N7 C8 1.378(4) . ? N8 C10 1.331(4) . ? N8 C9 1.357(5) . ? N9 N10 1.383(4) . ? N9 C11 1.469(4) . ? N10 C12 1.281(4) . ? N11 C15 1.315(4) . ? N11 C13 1.384(4) . ? N12 C15 1.340(4) . ? N12 C14 1.355(4) . ? C2 C3 1.449(5) . ? C3 C4 1.355(5) . ? C7 C8 1.443(5) . ? C8 C9 1.362(5) . ? C12 C13 1.445(4) . ? C13 C14 1.362(5) . ? N13 O2 1.232(4) . ? N13 O1 1.249(4) . ? N13 O3 1.260(4) . ? N14 O6 1.230(4) . ? N14 O5 1.234(4) . ? N14 O4 1.268(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 N7 Cd1 N3 100.05(9) . . ? N7 Cd1 N11 108.79(9) . . ? N3 Cd1 N11 99.22(9) . . ? N7 Cd1 N10 124.85(9) . . ? N3 Cd1 N10 134.99(9) . . ? N11 Cd1 N10 71.22(9) . . ? N7 Cd1 N2 132.54(9) . . ? N3 Cd1 N2 71.38(9) . . ? N11 Cd1 N2 118.62(9) . . ? N10 Cd1 N2 75.45(9) . . ? N7 Cd1 N6 71.11(9) . . ? N3 Cd1 N6 119.64(9) . . ? N11 Cd1 N6 140.84(9) . . ? N10 Cd1 N6 77.42(9) . . ? N2 Cd1 N6 73.66(9) . . ? N9 P1 N5 106.27(14) . . ? N9 P1 N1 106.63(14) . . ? N5 P1 N1 107.18(14) . . ? N9 P1 S1 111.91(10) . . ? N5 P1 S1 112.27(11) . . ? N1 P1 S1 112.19(10) . . ? N2 N1 C1 118.9(3) . . ? N2 N1 P1 117.6(2) . . ? C1 N1 P1 123.1(2) . . ? C2 N2 N1 120.2(3) . . ? C2 N2 Cd1 113.4(2) . . ? N1 N2 Cd1 123.72(18) . . ? C5 N3 C3 106.1(3) . . ? C5 N3 Cd1 138.2(2) . . ? C3 N3 Cd1 115.7(2) . . ? C5 N4 C4 108.2(3) . . ? N6 N5 C6 120.4(3) . . ? N6 N5 P1 115.8(2) . . ? C6 N5 P1 123.8(2) . . ? C7 N6 N5 120.5(3) . . ? C7 N6 Cd1 111.4(2) . . ? N5 N6 Cd1 125.89(19) . . ? C10 N7 C8 106.4(3) . . ? C10 N7 Cd1 137.6(2) . . ? C8 N7 Cd1 115.7(2) . . ? C10 N8 C9 108.2(3) . . ? N10 N9 C11 118.8(2) . . ? N10 N9 P1 118.11(19) . . ? C11 N9 P1 120.4(2) . . ? C12 N10 N9 119.6(3) . . ? C12 N10 Cd1 113.6(2) . . ? N9 N10 Cd1 122.64(18) . . ? C15 N11 C13 106.1(3) . . ? C15 N11 Cd1 138.9(2) . . ? C13 N11 Cd1 115.00(19) . . ? C15 N12 C14 108.5(3) . . ? N2 C2 C3 117.8(3) . . ? C4 C3 N3 108.8(3) . . ? C4 C3 C2 130.9(3) . . ? N3 C3 C2 120.3(3) . . ? N4 C4 C3 106.3(3) . . ? N3 C5 N4 110.6(3) . . ? N6 C7 C8 118.4(3) . . ? C9 C8 N7 108.3(3) . . ? C9 C8 C7 130.5(3) . . ? N7 C8 C7 121.2(3) . . ? N8 C9 C8 106.6(3) . . ? N7 C10 N8 110.6(3) . . ? N10 C12 C13 117.5(3) . . ? C14 C13 N11 108.8(3) . . ? C14 C13 C12 131.6(3) . . ? N11 C13 C12 119.6(3) . . ? N12 C14 C13 106.1(3) . . ? N11 C15 N12 110.6(3) . . ? O2 N13 O1 120.4(3) . . ? O2 N13 O3 120.7(3) . . ? O1 N13 O3 118.9(3) . . ? O6 N14 O5 122.3(3) . . ? O6 N14 O4 119.1(3) . . ? O5 N14 O4 118.6(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4A O4 0.87 1.94 2.799(4) 168.4 . N8 H8 O1 0.87 2.00 2.870(4) 177.1 . N12 H12A O3 0.87 2.02 2.874(4) 168.9 3_657 O7 H7A O4 1.06(4) 2.26(5) 3.207(5) 148(4) 1_455 O7 H7A O5 1.06(4) 2.46(5) 3.269(4) 132(4) 1_455 O7 H7A O1 1.06(4) 2.53(5) 3.121(4) 114(4) . O7 H7B O3 1.07(4) 1.91(4) 2.914(5) 155(5) 2_556 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 24.21 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.536 _refine_diff_density_min -0.978 _refine_diff_density_rms 0.082