# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jose Goicoechea' _publ_contact_author_email JOSE.GOICOECHEA@CHEM.OX.AC.UK _publ_section_title ; Reactivity studies of group 15 Zintl ions towards homoleptic post-transition metal organometallics: a 'bottom-up' approach to bimetallic molecular alloys ; _publ_contact_author ; Dr. J. M. Goicoechea Chemistry Research Laboratory University of Oxford Mansfield Road Oxford OX1 3TA UK ; _publ_contact_author_phone '+44 1865 275961' loop_ _publ_author_name 'Jose Goicoechea' 'Mark S Denning' 'Caroline Knapp' 'Nick Rees' 'Binbin Zhou' # Attachment 'combined_revised.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 736076' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K(2,2,2-crypt)]4[Cu2(As7)2]*2en ; _contact_author_fax '+44 1865 272690' _chemical_name_common (K(2,2,2-crypt))4(Cu2(As7)2)*2en _chemical_melting_point ? _chemical_formula_moiety '4(C18 H36 N2 O6), Cu2 As14, 2(C2 H8 N2)' _chemical_formula_sum 'C76 H160 As14 Cu2 K4 N12 O24' _chemical_formula_weight 2958.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.1540(2) _cell_length_b 15.1810(2) _cell_length_c 15.7640(2) _cell_angle_alpha 111.460(1) _cell_angle_beta 90.070(1) _cell_angle_gamma 118.900(1) _cell_volume 2883.41(7) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 142390 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.704 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 4.565 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2501 _exptl_absorpt_correction_T_max 0.3613 _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _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 19140 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 5.14 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10050 _reflns_number_gt 8511 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; KappaCCD software "Collect" (Nonius, 2000) ; _computing_cell_refinement ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_data_reduction ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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^)+(0.0703P)^2^+13.1803P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10050 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1372 _refine_ls_wR_factor_gt 0.1318 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 As4 As 0.11582(5) -0.08727(5) 0.68251(4) 0.03342(16) Uani 1 1 d . . . As7 As 0.15828(5) 0.09748(5) 0.76889(5) 0.03795(17) Uani 1 1 d . . . As1 As 0.06146(4) -0.15253(4) 0.79891(4) 0.02740(15) Uani 1 1 d . . . As6 As 0.23337(4) 0.14949(5) 0.93009(4) 0.03093(15) Uani 1 1 d . . . As5 As 0.03397(5) 0.09409(5) 0.87016(5) 0.04020(18) Uani 1 1 d . . . As2 As -0.06400(4) -0.09662(5) 0.84555(4) 0.03285(16) Uani 1 1 d . . . As3 As 0.19966(5) -0.01768(5) 0.93633(4) 0.03058(15) Uani 1 1 d . . . Cu1 Cu 0.08904(6) 0.05989(7) 0.99710(5) 0.0411(2) Uani 1 1 d . . . K1 K 0.26557(9) 0.69613(9) 0.21794(8) 0.0254(2) Uani 1 1 d . . . N11 N 0.0392(4) 0.5876(4) 0.2238(3) 0.0312(10) Uani 1 1 d . . . N12 N 0.4928(4) 0.8063(4) 0.2144(4) 0.0339(11) Uani 1 1 d . . . O11 O 0.1389(3) 0.7514(3) 0.1464(3) 0.0315(9) Uani 1 1 d . . . O12 O 0.3460(3) 0.8370(3) 0.1229(3) 0.0319(9) Uani 1 1 d . . . O13 O 0.1338(4) 0.4630(3) 0.1213(3) 0.0391(10) Uani 1 1 d . . . O14 O 0.3490(4) 0.5576(4) 0.1348(3) 0.0397(10) Uani 1 1 d . . . O15 O 0.2067(3) 0.7265(3) 0.3934(3) 0.0318(9) Uani 1 1 d . . . O16 O 0.4181(3) 0.8481(3) 0.3877(3) 0.0335(9) Uani 1 1 d . . . C101 C -0.0059(5) 0.6438(5) 0.1981(5) 0.0372(14) Uani 1 1 d . . . H10A H 0.0109 0.7118 0.2536 0.045 Uiso 1 1 calc R . . H10B H -0.0820 0.5946 0.1803 0.045 Uiso 1 1 calc R . . C102 C 0.0307(5) 0.6750(5) 0.1197(4) 0.0357(13) Uani 1 1 d . . . H10C H 0.0147 0.6079 0.0635 0.043 Uiso 1 1 calc R . . H10D H -0.0052 0.7088 0.1042 0.043 Uiso 1 1 calc R . . C103 C 0.1753(5) 0.7969(5) 0.0801(5) 0.0369(14) Uani 1 1 d . . . H10E H 0.1346 0.8278 0.0684 0.044 Uiso 1 1 calc R . . H10F H 0.1675 0.7382 0.0203 0.044 Uiso 1 1 calc R . . C104 C 0.2866(5) 0.8861(5) 0.1183(5) 0.0374(14) Uani 1 1 d . . . H10G H 0.3108 0.9257 0.0775 0.045 Uiso 1 1 calc R . . H10H H 0.2953 0.9403 0.1815 0.045 Uiso 1 1 calc R . . C105 C 0.4535(5) 0.9175(5) 0.1557(5) 0.0371(14) Uani 1 1 d . . . H10I H 0.4669 0.9697 0.2212 0.045 Uiso 1 1 calc R . . H10J H 0.4762 0.9604 0.1174 0.045 Uiso 1 1 calc R . . C106 C 0.5134(5) 0.8612(6) 0.1501(5) 0.0406(15) Uani 1 1 d . . . H10K H 0.4954 0.8053 0.0853 0.049 Uiso 1 1 calc R . . H10L H 0.5881 0.9168 0.1650 0.049 Uiso 1 1 calc R . . C107 C -0.0155(5) 0.4699(5) 0.1558(5) 0.0405(15) Uani 1 1 d . . . H10M H -0.0300 0.4656 0.0927 0.049 Uiso 1 1 calc R . . H10N H -0.0826 0.4294 0.1714 0.049 Uiso 1 1 calc R . . C108 C 0.0431(5) 0.4132(5) 0.1533(5) 0.0434(16) Uani 1 1 d . . . H10O H 0.0613 0.4198 0.2166 0.052 Uiso 1 1 calc R . . H10P H -0.0002 0.3335 0.1110 0.052 Uiso 1 1 calc R . . C109 C 0.1827(6) 0.3992(5) 0.1019(5) 0.0480(17) Uani 1 1 d . . . H10Q H 0.1339 0.3223 0.0559 0.058 Uiso 1 1 calc R . . H10R H 0.2044 0.3967 0.1599 0.058 Uiso 1 1 calc R . . C110 C 0.2741(6) 0.4527(6) 0.0639(5) 0.0491(18) Uani 1 1 d . . . H11A H 0.3041 0.4052 0.0420 0.059 Uiso 1 1 calc R . . H11B H 0.2531 0.4624 0.0101 0.059 Uiso 1 1 calc R . . C111 C 0.4366(6) 0.6146(6) 0.1018(5) 0.0456(16) Uani 1 1 d . . . H11C H 0.4161 0.6327 0.0537 0.055 Uiso 1 1 calc R . . H11D H 0.4644 0.5663 0.0725 0.055 Uiso 1 1 calc R . . C112 C 0.5187(5) 0.7191(6) 0.1798(5) 0.0462(16) Uani 1 1 d . . . H11E H 0.5304 0.7020 0.2322 0.055 Uiso 1 1 calc R . . H11F H 0.5840 0.7477 0.1580 0.055 Uiso 1 1 calc R . . C113 C 0.0300(5) 0.5952(5) 0.3183(4) 0.0383(14) Uani 1 1 d . . . H11G H 0.0407 0.5393 0.3267 0.046 Uiso 1 1 calc R . . H11H H -0.0410 0.5770 0.3251 0.046 Uiso 1 1 calc R . . C114 C 0.1053(5) 0.7072(5) 0.3935(4) 0.0369(14) Uani 1 1 d . . . H11I H 0.1005 0.7650 0.3824 0.044 Uiso 1 1 calc R . . H11J H 0.0890 0.7107 0.4550 0.044 Uiso 1 1 calc R . . C115 C 0.2815(5) 0.8306(5) 0.4674(4) 0.0381(14) Uani 1 1 d . . . H11K H 0.2610 0.8353 0.5277 0.046 Uiso 1 1 calc R . . H11L H 0.2861 0.8924 0.4559 0.046 Uiso 1 1 calc R . . C116 C 0.3838(5) 0.8383(5) 0.4705(4) 0.0392(14) Uani 1 1 d . . . H11M H 0.4346 0.9037 0.5267 0.047 Uiso 1 1 calc R . . H11N H 0.3770 0.7712 0.4733 0.047 Uiso 1 1 calc R . . C117 C 0.5142(5) 0.8534(6) 0.3843(5) 0.0426(15) Uani 1 1 d . . . H11O H 0.5046 0.7800 0.3710 0.051 Uiso 1 1 calc R . . H11P H 0.5635 0.9075 0.4450 0.051 Uiso 1 1 calc R . . C118 C 0.5553(5) 0.8887(6) 0.3081(5) 0.0449(16) Uani 1 1 d . . . H11Q H 0.5583 0.9588 0.3195 0.054 Uiso 1 1 calc R . . H11R H 0.6266 0.9033 0.3109 0.054 Uiso 1 1 calc R . . K2 K 0.63560(8) 0.41520(9) 0.35467(7) 0.0214(2) Uani 1 1 d . . . N21 N 0.7873(3) 0.5513(4) 0.5395(3) 0.0290(10) Uani 1 1 d . . . N22 N 0.4813(4) 0.2823(4) 0.1727(3) 0.0315(11) Uani 1 1 d . . . O21 O 0.7996(3) 0.3842(3) 0.3770(3) 0.0353(9) Uani 1 1 d . . . O22 O 0.6332(3) 0.2310(3) 0.2173(3) 0.0340(9) Uani 1 1 d . . . O23 O 0.5716(3) 0.3943(3) 0.5219(3) 0.0305(9) Uani 1 1 d . . . O24 O 0.4247(3) 0.2987(3) 0.3542(3) 0.0286(8) Uani 1 1 d . . . O25 O 0.7585(3) 0.6485(3) 0.4154(3) 0.0293(8) Uani 1 1 d . . . O26 O 0.6396(3) 0.5161(3) 0.2338(3) 0.0338(9) Uani 1 1 d . . . C201 C 0.8772(4) 0.5388(5) 0.5266(5) 0.0366(14) Uani 1 1 d . . . H20A H 0.9197 0.5670 0.5886 0.044 Uiso 1 1 calc R . . H20B H 0.9199 0.5846 0.4945 0.044 Uiso 1 1 calc R . . C202 C 0.8480(5) 0.4213(6) 0.4710(5) 0.0389(14) Uani 1 1 d . . . H20C H 0.9105 0.4159 0.4716 0.047 Uiso 1 1 calc R . . H20D H 0.8001 0.3736 0.4993 0.047 Uiso 1 1 calc R . . C203 C 0.7736(6) 0.2721(6) 0.3231(6) 0.0514(18) Uani 1 1 d . . . H20E H 0.7220 0.2224 0.3479 0.062 Uiso 1 1 calc R . . H20F H 0.8360 0.2670 0.3276 0.062 Uiso 1 1 calc R . . C204 C 0.7309(5) 0.2376(6) 0.2242(5) 0.0480(17) Uani 1 1 d . . . H20G H 0.7793 0.2920 0.2015 0.058 Uiso 1 1 calc R . . H20H H 0.7216 0.1645 0.1851 0.058 Uiso 1 1 calc R . . C205 C 0.5861(5) 0.1943(5) 0.1242(4) 0.0378(14) Uani 1 1 d . . . H20I H 0.5812 0.1236 0.0846 0.045 Uiso 1 1 calc R . . H20J H 0.6281 0.2498 0.0999 0.045 Uiso 1 1 calc R . . C206 C 0.4794(5) 0.1780(5) 0.1213(4) 0.0390(15) Uani 1 1 d . . . H20K H 0.4437 0.1450 0.0553 0.047 Uiso 1 1 calc R . . H20L H 0.4393 0.1250 0.1485 0.047 Uiso 1 1 calc R . . C207 C 0.7446(5) 0.5172(6) 0.6128(4) 0.0393(15) Uani 1 1 d . . . H20M H 0.7871 0.5783 0.6744 0.047 Uiso 1 1 calc R . . H20N H 0.7492 0.4525 0.6071 0.047 Uiso 1 1 calc R . . C208 C 0.6332(5) 0.4872(6) 0.6090(4) 0.0395(15) Uani 1 1 d . . . H20O H 0.6091 0.4679 0.6616 0.047 Uiso 1 1 calc R . . H20P H 0.6270 0.5508 0.6141 0.047 Uiso 1 1 calc R . . C209 C 0.4637(4) 0.3540(6) 0.5181(4) 0.0383(15) Uani 1 1 d . . . H20Q H 0.4500 0.4139 0.5269 0.046 Uiso 1 1 calc R . . H20R H 0.4428 0.3294 0.5687 0.046 Uiso 1 1 calc R . . C210 C 0.4031(4) 0.2594(6) 0.4256(5) 0.0395(15) Uani 1 1 d . . . H21A H 0.4219 0.2026 0.4142 0.047 Uiso 1 1 calc R . . H21B H 0.3284 0.2248 0.4251 0.047 Uiso 1 1 calc R . . C211 C 0.3544(4) 0.2161(5) 0.2679(4) 0.0397(15) Uani 1 1 d . . . H21C H 0.2830 0.1961 0.2748 0.048 Uiso 1 1 calc R . . H21D H 0.3586 0.1488 0.2500 0.048 Uiso 1 1 calc R . . C212 C 0.3791(5) 0.2577(6) 0.1927(4) 0.0402(15) Uani 1 1 d . . . H21E H 0.3257 0.2013 0.1346 0.048 Uiso 1 1 calc R . . H21F H 0.3760 0.3258 0.2119 0.048 Uiso 1 1 calc R . . C213 C 0.8175(5) 0.6675(5) 0.5655(4) 0.0406(15) Uani 1 1 d . . . H21G H 0.8770 0.7159 0.6197 0.049 Uiso 1 1 calc R . . H21H H 0.7595 0.6766 0.5857 0.049 Uiso 1 1 calc R . . C214 C 0.8463(5) 0.7064(5) 0.4893(5) 0.0403(15) Uani 1 1 d . . . H21I H 0.8735 0.7869 0.5145 0.048 Uiso 1 1 calc R . . H21J H 0.9012 0.6932 0.4654 0.048 Uiso 1 1 calc R . . C215 C 0.7852(5) 0.6817(5) 0.3416(5) 0.0388(14) Uani 1 1 d . . . H21K H 0.8306 0.6560 0.3111 0.047 Uiso 1 1 calc R . . H21L H 0.8234 0.7636 0.3666 0.047 Uiso 1 1 calc R . . C216 C 0.6905(5) 0.6340(5) 0.2727(5) 0.0391(14) Uani 1 1 d . . . H21M H 0.6442 0.6581 0.3034 0.047 Uiso 1 1 calc R . . H21N H 0.7085 0.6601 0.2226 0.047 Uiso 1 1 calc R . . C217 C 0.5462(6) 0.4659(6) 0.1683(5) 0.0422(15) Uani 1 1 d . . . H21O H 0.5588 0.5022 0.1250 0.051 Uiso 1 1 calc R . . H21P H 0.4936 0.4748 0.2015 0.051 Uiso 1 1 calc R . . C218 C 0.5080(5) 0.3449(5) 0.1144(4) 0.0398(15) Uani 1 1 d . . . H21Q H 0.4462 0.3114 0.0656 0.048 Uiso 1 1 calc R . . H21R H 0.5619 0.3376 0.0826 0.048 Uiso 1 1 calc R . . N1E N 0.7652(5) 0.9333(7) 0.4819(6) 0.070(2) Uani 1 1 d . . . H1E4 H 0.7552 0.9125 0.4190 0.106 Uiso 0.67 1 calc PR . . H1E5 H 0.7307 0.9684 0.5064 0.106 Uiso 0.67 1 calc PR . . H1E3 H 0.7411 0.8722 0.4937 0.106 Uiso 0.67 1 calc PR . . C1E C 0.8728(8) 1.0065(8) 0.5232(7) 0.072(2) Uani 1 1 d . . . H1E1 H 0.8995 1.0728 0.5100 0.087 Uiso 1 1 calc R . . H1E2 H 0.9108 0.9689 0.4960 0.087 Uiso 1 1 calc R . . C2E C 0.8898(8) 1.0410(7) 0.6277(7) 0.069(2) Uani 1 1 d . . . H2E1 H 0.9619 1.1024 0.6582 0.083 Uiso 1 1 calc R . . H2E2 H 0.8429 1.0670 0.6536 0.083 Uiso 1 1 calc R . . N2E N 0.8692(7) 0.9468(6) 0.6446(6) 0.090(3) Uani 1 1 d . . . H2E3 H 0.8791 0.9661 0.7072 0.135 Uiso 0.67 1 calc PR . . H2E4 H 0.9127 0.9237 0.6207 0.135 Uiso 0.67 1 calc PR . . H2E5 H 0.8026 0.8911 0.6167 0.135 Uiso 0.67 1 calc PR . . 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 As4 0.0376(3) 0.0332(3) 0.0239(3) 0.0108(2) 0.0081(2) 0.0153(3) As7 0.0432(4) 0.0273(3) 0.0400(4) 0.0207(3) 0.0030(3) 0.0113(3) As1 0.0306(3) 0.0185(3) 0.0314(3) 0.0100(2) 0.0101(2) 0.0118(2) As6 0.0240(3) 0.0212(3) 0.0327(3) 0.0065(2) -0.0012(2) 0.0047(2) As5 0.0438(4) 0.0302(3) 0.0491(4) 0.0094(3) 0.0030(3) 0.0262(3) As2 0.0204(3) 0.0296(3) 0.0352(3) 0.0053(3) 0.0046(2) 0.0096(2) As3 0.0377(3) 0.0351(3) 0.0262(3) 0.0135(3) 0.0060(2) 0.0236(3) Cu1 0.0263(4) 0.0396(4) 0.0381(4) 0.0050(3) 0.0087(3) 0.0117(3) K1 0.0293(6) 0.0225(6) 0.0271(6) 0.0118(5) 0.0087(5) 0.0144(5) N11 0.034(3) 0.024(2) 0.030(3) 0.011(2) 0.010(2) 0.011(2) N12 0.029(2) 0.040(3) 0.040(3) 0.020(2) 0.012(2) 0.020(2) O11 0.028(2) 0.029(2) 0.037(2) 0.0177(18) 0.0038(17) 0.0121(17) O12 0.034(2) 0.0226(19) 0.042(2) 0.0174(18) 0.0071(18) 0.0136(17) O13 0.052(3) 0.020(2) 0.041(2) 0.0104(18) 0.010(2) 0.017(2) O14 0.059(3) 0.036(2) 0.035(2) 0.0151(19) 0.017(2) 0.033(2) O15 0.033(2) 0.028(2) 0.026(2) 0.0079(17) 0.0103(16) 0.0128(18) O16 0.028(2) 0.040(2) 0.031(2) 0.0166(18) 0.0054(16) 0.0147(18) C101 0.026(3) 0.041(3) 0.041(3) 0.016(3) 0.009(3) 0.016(3) C102 0.032(3) 0.035(3) 0.042(3) 0.015(3) 0.003(3) 0.019(3) C103 0.037(3) 0.037(3) 0.046(4) 0.026(3) 0.005(3) 0.020(3) C104 0.039(3) 0.028(3) 0.051(4) 0.023(3) 0.007(3) 0.017(3) C105 0.033(3) 0.029(3) 0.048(4) 0.022(3) 0.013(3) 0.011(3) C106 0.039(3) 0.047(4) 0.048(4) 0.029(3) 0.023(3) 0.025(3) C107 0.037(3) 0.026(3) 0.041(4) 0.012(3) 0.004(3) 0.006(3) C108 0.054(4) 0.021(3) 0.037(3) 0.011(3) 0.004(3) 0.008(3) C109 0.072(5) 0.025(3) 0.044(4) 0.008(3) 0.010(3) 0.028(3) C110 0.073(5) 0.037(4) 0.042(4) 0.005(3) 0.011(3) 0.040(4) C111 0.060(4) 0.057(4) 0.051(4) 0.030(4) 0.031(3) 0.048(4) C112 0.041(4) 0.058(4) 0.059(4) 0.029(4) 0.021(3) 0.037(4) C113 0.035(3) 0.038(3) 0.039(3) 0.020(3) 0.017(3) 0.014(3) C114 0.040(3) 0.040(3) 0.030(3) 0.015(3) 0.017(3) 0.020(3) C115 0.047(4) 0.030(3) 0.022(3) 0.003(2) 0.008(3) 0.015(3) C116 0.042(3) 0.035(3) 0.025(3) 0.010(3) 0.003(3) 0.012(3) C117 0.031(3) 0.051(4) 0.044(4) 0.020(3) 0.002(3) 0.020(3) C118 0.024(3) 0.052(4) 0.052(4) 0.021(3) 0.005(3) 0.016(3) K2 0.0199(5) 0.0195(5) 0.0236(5) 0.0077(4) 0.0046(4) 0.0103(4) N21 0.023(2) 0.035(3) 0.025(2) 0.010(2) 0.0012(18) 0.015(2) N22 0.032(3) 0.022(2) 0.029(2) 0.005(2) 0.001(2) 0.010(2) O21 0.034(2) 0.037(2) 0.044(2) 0.0154(19) 0.0114(18) 0.025(2) O22 0.039(2) 0.032(2) 0.034(2) 0.0104(18) 0.0151(18) 0.0228(19) O23 0.0215(19) 0.045(2) 0.029(2) 0.0151(18) 0.0096(15) 0.0206(18) O24 0.0218(18) 0.028(2) 0.029(2) 0.0151(17) 0.0021(15) 0.0061(16) O25 0.0235(19) 0.0222(19) 0.033(2) 0.0110(17) 0.0033(16) 0.0061(16) O26 0.040(2) 0.026(2) 0.036(2) 0.0160(18) 0.0039(18) 0.0161(18) C201 0.023(3) 0.045(4) 0.043(3) 0.020(3) 0.003(2) 0.017(3) C202 0.024(3) 0.049(4) 0.054(4) 0.025(3) 0.010(3) 0.023(3) C203 0.047(4) 0.044(4) 0.070(5) 0.012(4) 0.008(3) 0.037(3) C204 0.049(4) 0.047(4) 0.052(4) 0.010(3) 0.023(3) 0.034(3) C205 0.056(4) 0.026(3) 0.029(3) 0.009(2) 0.019(3) 0.021(3) C206 0.044(4) 0.023(3) 0.026(3) 0.000(2) 0.003(3) 0.007(3) C207 0.029(3) 0.059(4) 0.028(3) 0.017(3) 0.002(2) 0.023(3) C208 0.037(3) 0.060(4) 0.021(3) 0.013(3) 0.008(2) 0.028(3) C209 0.026(3) 0.064(4) 0.043(4) 0.036(3) 0.019(3) 0.026(3) C210 0.021(3) 0.048(4) 0.058(4) 0.039(3) 0.012(3) 0.013(3) C211 0.021(3) 0.034(3) 0.041(4) 0.010(3) 0.002(2) 0.002(3) C212 0.029(3) 0.048(4) 0.026(3) 0.006(3) -0.006(2) 0.015(3) C213 0.039(3) 0.028(3) 0.033(3) -0.003(3) -0.008(3) 0.014(3) C214 0.028(3) 0.019(3) 0.055(4) 0.007(3) -0.007(3) 0.005(2) C215 0.039(3) 0.022(3) 0.048(4) 0.015(3) 0.016(3) 0.010(3) C216 0.052(4) 0.026(3) 0.046(4) 0.023(3) 0.018(3) 0.021(3) C217 0.056(4) 0.043(4) 0.035(3) 0.020(3) 0.004(3) 0.027(3) C218 0.048(4) 0.041(4) 0.023(3) 0.011(3) -0.001(3) 0.020(3) N1E 0.031(3) 0.100(6) 0.089(5) 0.063(5) 0.005(3) 0.024(4) C1E 0.083(6) 0.081(6) 0.071(6) 0.043(5) 0.035(5) 0.047(5) C2E 0.091(7) 0.061(5) 0.076(6) 0.036(5) 0.017(5) 0.049(5) N2E 0.092(6) 0.055(4) 0.082(6) 0.021(4) -0.035(5) 0.014(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As4 As1 2.3605(8) . ? As4 As7 2.3650(9) . ? As7 As6 2.4561(9) . ? As7 As5 2.4645(10) . ? As1 As3 2.4228(8) . ? As1 As2 2.4458(8) . ? As6 As3 2.3750(8) . ? As6 Cu1 2.4353(10) . ? As6 As5 2.7722(9) . ? As5 As2 2.3997(9) . ? As5 Cu1 2.4788(11) . ? As2 Cu1 2.4089(10) 2_557 ? As2 Cu1 2.6903(9) . ? As3 Cu1 2.4902(9) . ? Cu1 As2 2.4089(10) 2_557 ? Cu1 Cu1 2.4447(15) 2_557 ? K1 O11 2.811(4) . ? K1 O13 2.837(4) . ? K1 O15 2.851(4) . ? K1 O12 2.852(4) . ? K1 O16 2.853(4) . ? K1 O14 2.881(4) . ? K1 N11 3.024(5) . ? K1 N12 3.027(5) . ? N11 C113 1.464(8) . ? N11 C101 1.475(8) . ? N11 C107 1.481(8) . ? N12 C118 1.464(9) . ? N12 C112 1.475(8) . ? N12 C106 1.480(8) . ? O11 C102 1.419(7) . ? O11 C103 1.426(7) . ? O12 C105 1.424(7) . ? O12 C104 1.434(7) . ? O13 C108 1.412(8) . ? O13 C109 1.435(8) . ? O14 C111 1.416(8) . ? O14 C110 1.421(8) . ? O15 C114 1.418(7) . ? O15 C115 1.435(7) . ? O16 C117 1.421(7) . ? O16 C116 1.436(7) . ? C101 C102 1.495(9) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.495(9) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C105 C106 1.501(9) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 C108 1.498(10) . ? C107 H10M 0.9900 . ? C107 H10N 0.9900 . ? C108 H10O 0.9900 . ? C108 H10P 0.9900 . ? C109 C110 1.487(11) . ? C109 H10Q 0.9900 . ? C109 H10R 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.496(11) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 C114 1.499(9) . ? C113 H11G 0.9900 . ? C113 H11H 0.9900 . ? C114 H11I 0.9900 . ? C114 H11J 0.9900 . ? C115 C116 1.496(9) . ? C115 H11K 0.9900 . ? C115 H11L 0.9900 . ? C116 H11M 0.9900 . ? C116 H11N 0.9900 . ? C117 C118 1.505(10) . ? C117 H11O 0.9900 . ? C117 H11P 0.9900 . ? C118 H11Q 0.9900 . ? C118 H11R 0.9900 . ? K2 O21 2.789(4) . ? K2 O24 2.804(4) . ? K2 O22 2.825(4) . ? K2 O26 2.833(4) . ? K2 O25 2.840(4) . ? K2 O23 2.883(4) . ? K2 N22 2.993(5) . ? K2 N21 3.005(5) . ? N21 C207 1.461(8) . ? N21 C201 1.468(7) . ? N21 C213 1.476(8) . ? N22 C212 1.472(8) . ? N22 C218 1.475(8) . ? N22 C206 1.477(8) . ? O21 C202 1.427(8) . ? O21 C203 1.437(8) . ? O22 C205 1.409(8) . ? O22 C204 1.437(8) . ? O23 C208 1.433(7) . ? O23 C209 1.434(7) . ? O24 C211 1.420(7) . ? O24 C210 1.427(7) . ? O25 C215 1.416(7) . ? O25 C214 1.421(7) . ? O26 C217 1.424(8) . ? O26 C216 1.426(7) . ? C201 C202 1.496(9) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C203 C204 1.481(11) . ? C203 H20E 0.9900 . ? C203 H20F 0.9900 . ? C204 H20G 0.9900 . ? C204 H20H 0.9900 . ? C205 C206 1.510(9) . ? C205 H20I 0.9900 . ? C205 H20J 0.9900 . ? C206 H20K 0.9900 . ? C206 H20L 0.9900 . ? C207 C208 1.516(8) . ? C207 H20M 0.9900 . ? C207 H20N 0.9900 . ? C208 H20O 0.9900 . ? C208 H20P 0.9900 . ? C209 C210 1.490(10) . ? C209 H20Q 0.9900 . ? C209 H20R 0.9900 . ? C210 H21A 0.9900 . ? C210 H21B 0.9900 . ? C211 C212 1.506(9) . ? C211 H21C 0.9900 . ? C211 H21D 0.9900 . ? C212 H21E 0.9900 . ? C212 H21F 0.9900 . ? C213 C214 1.501(10) . ? C213 H21G 0.9900 . ? C213 H21H 0.9900 . ? C214 H21I 0.9900 . ? C214 H21J 0.9900 . ? C215 C216 1.477(9) . ? C215 H21K 0.9900 . ? C215 H21L 0.9900 . ? C216 H21M 0.9900 . ? C216 H21N 0.9900 . ? C217 C218 1.504(9) . ? C217 H21O 0.9900 . ? C217 H21P 0.9900 . ? C218 H21Q 0.9900 . ? C218 H21R 0.9900 . ? N1E C1E 1.427(12) . ? N1E H1E4 0.9100 . ? N1E H1E5 0.9100 . ? N1E H1E3 0.9100 . ? C1E C2E 1.514(13) . ? C1E H1E1 0.9900 . ? C1E H1E2 0.9900 . ? C2E N2E 1.436(11) . ? C2E H2E1 0.9900 . ? C2E H2E2 0.9900 . ? N2E H2E3 0.9100 . ? N2E H2E4 0.9100 . ? N2E H2E5 0.9100 . ? 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 As1 As4 As7 97.98(3) . . ? As4 As7 As6 106.13(3) . . ? As4 As7 As5 107.74(3) . . ? As6 As7 As5 68.58(3) . . ? As4 As1 As3 104.66(3) . . ? As4 As1 As2 102.03(3) . . ? As3 As1 As2 98.24(3) . . ? As3 As6 Cu1 62.34(3) . . ? As3 As6 As7 105.80(3) . . ? Cu1 As6 As7 106.20(3) . . ? As3 As6 As5 100.29(3) . . ? Cu1 As6 As5 56.40(3) . . ? As7 As6 As5 55.85(3) . . ? As2 As5 As7 103.09(3) . . ? As2 As5 Cu1 66.91(3) . . ? As7 As5 Cu1 104.62(3) . . ? As2 As5 As6 101.56(3) . . ? As7 As5 As6 55.57(2) . . ? Cu1 As5 As6 54.92(2) . . ? As5 As2 Cu1 95.62(3) . 2_557 ? As5 As2 As1 100.52(3) . . ? Cu1 As2 As1 118.07(4) 2_557 . ? As5 As2 Cu1 57.95(3) . . ? Cu1 As2 Cu1 56.97(3) 2_557 . ? As1 As2 Cu1 83.18(3) . . ? As6 As3 As1 100.41(3) . . ? As6 As3 Cu1 60.02(3) . . ? As1 As3 Cu1 88.03(3) . . ? As2 Cu1 As6 133.76(4) 2_557 . ? As2 Cu1 Cu1 67.32(4) 2_557 2_557 ? As6 Cu1 Cu1 158.21(6) . 2_557 ? As2 Cu1 As5 133.35(4) 2_557 . ? As6 Cu1 As5 68.68(3) . . ? Cu1 Cu1 As5 92.71(5) 2_557 . ? As2 Cu1 As3 120.87(4) 2_557 . ? As6 Cu1 As3 57.64(3) . . ? Cu1 Cu1 As3 120.98(5) 2_557 . ? As5 Cu1 As3 105.66(3) . . ? As2 Cu1 As2 123.03(3) 2_557 . ? As6 Cu1 As2 102.97(3) . . ? Cu1 Cu1 As2 55.71(3) 2_557 . ? As5 Cu1 As2 55.14(3) . . ? As3 Cu1 As2 90.48(3) . . ? O11 K1 O13 96.42(13) . . ? O11 K1 O15 96.33(12) . . ? O13 K1 O15 99.25(12) . . ? O11 K1 O12 60.27(11) . . ? O13 K1 O12 122.27(13) . . ? O15 K1 O12 132.68(12) . . ? O11 K1 O16 121.37(12) . . ? O13 K1 O16 136.95(13) . . ? O15 K1 O16 59.79(11) . . ? O12 K1 O16 95.91(12) . . ? O11 K1 O14 134.21(13) . . ? O13 K1 O14 59.25(13) . . ? O15 K1 O14 123.77(13) . . ? O12 K1 O14 98.32(12) . . ? O16 K1 O14 99.32(13) . . ? O11 K1 N11 60.02(12) . . ? O13 K1 N11 60.08(13) . . ? O15 K1 N11 60.28(12) . . ? O12 K1 N11 119.97(13) . . ? O16 K1 N11 119.68(12) . . ? O14 K1 N11 118.81(14) . . ? O11 K1 N12 120.17(13) . . ? O13 K1 N12 120.35(14) . . ? O15 K1 N12 119.10(13) . . ? O12 K1 N12 60.29(13) . . ? O16 K1 N12 59.69(13) . . ? O14 K1 N12 61.55(14) . . ? N11 K1 N12 179.37(15) . . ? C113 N11 C101 110.6(5) . . ? C113 N11 C107 110.0(5) . . ? C101 N11 C107 108.8(5) . . ? C113 N11 K1 108.5(3) . . ? C101 N11 K1 109.6(3) . . ? C107 N11 K1 109.2(4) . . ? C118 N12 C112 110.5(5) . . ? C118 N12 C106 109.3(5) . . ? C112 N12 C106 109.1(5) . . ? C118 N12 K1 110.3(3) . . ? C112 N12 K1 107.8(4) . . ? C106 N12 K1 109.9(3) . . ? C102 O11 C103 111.7(4) . . ? C102 O11 K1 118.2(3) . . ? C103 O11 K1 115.4(3) . . ? C105 O12 C104 111.8(4) . . ? C105 O12 K1 114.5(3) . . ? C104 O12 K1 112.4(3) . . ? C108 O13 C109 110.8(5) . . ? C108 O13 K1 116.7(3) . . ? C109 O13 K1 116.4(4) . . ? C111 O14 C110 112.0(5) . . ? C111 O14 K1 109.7(3) . . ? C110 O14 K1 112.6(4) . . ? C114 O15 C115 111.4(4) . . ? C114 O15 K1 115.8(3) . . ? C115 O15 K1 112.6(3) . . ? C117 O16 C116 111.8(5) . . ? C117 O16 K1 114.1(4) . . ? C116 O16 K1 115.1(3) . . ? N11 C101 C102 114.3(5) . . ? N11 C101 H10A 108.7 . . ? C102 C101 H10A 108.7 . . ? N11 C101 H10B 108.7 . . ? C102 C101 H10B 108.7 . . ? H10A C101 H10B 107.6 . . ? O11 C102 C101 109.4(5) . . ? O11 C102 H10C 109.8 . . ? C101 C102 H10C 109.8 . . ? O11 C102 H10D 109.8 . . ? C101 C102 H10D 109.8 . . ? H10C C102 H10D 108.2 . . ? O11 C103 C104 108.6(5) . . ? O11 C103 H10E 110.0 . . ? C104 C103 H10E 110.0 . . ? O11 C103 H10F 110.0 . . ? C104 C103 H10F 110.0 . . ? H10E C103 H10F 108.4 . . ? O12 C104 C103 109.0(5) . . ? O12 C104 H10G 109.9 . . ? C103 C104 H10G 109.9 . . ? O12 C104 H10H 109.9 . . ? C103 C104 H10H 109.9 . . ? H10G C104 H10H 108.3 . . ? O12 C105 C106 109.9(5) . . ? O12 C105 H10I 109.7 . . ? C106 C105 H10I 109.7 . . ? O12 C105 H10J 109.7 . . ? C106 C105 H10J 109.7 . . ? H10I C105 H10J 108.2 . . ? N12 C106 C105 112.9(5) . . ? N12 C106 H10K 109.0 . . ? C105 C106 H10K 109.0 . . ? N12 C106 H10L 109.0 . . ? C105 C106 H10L 109.0 . . ? H10K C106 H10L 107.8 . . ? N11 C107 C108 114.1(5) . . ? N11 C107 H10M 108.7 . . ? C108 C107 H10M 108.7 . . ? N11 C107 H10N 108.7 . . ? C108 C107 H10N 108.7 . . ? H10M C107 H10N 107.6 . . ? O13 C108 C107 109.0(5) . . ? O13 C108 H10O 109.9 . . ? C107 C108 H10O 109.9 . . ? O13 C108 H10P 109.9 . . ? C107 C108 H10P 109.9 . . ? H10O C108 H10P 108.3 . . ? O13 C109 C110 108.0(5) . . ? O13 C109 H10Q 110.1 . . ? C110 C109 H10Q 110.1 . . ? O13 C109 H10R 110.1 . . ? C110 C109 H10R 110.1 . . ? H10Q C109 H10R 108.4 . . ? O14 C110 C109 109.3(5) . . ? O14 C110 H11A 109.8 . . ? C109 C110 H11A 109.8 . . ? O14 C110 H11B 109.8 . . ? C109 C110 H11B 109.8 . . ? H11A C110 H11B 108.3 . . ? O14 C111 C112 111.0(5) . . ? O14 C111 H11C 109.4 . . ? C112 C111 H11C 109.4 . . ? O14 C111 H11D 109.4 . . ? C112 C111 H11D 109.4 . . ? H11C C111 H11D 108.0 . . ? N12 C112 C111 113.3(5) . . ? N12 C112 H11E 108.9 . . ? C111 C112 H11E 108.9 . . ? N12 C112 H11F 108.9 . . ? C111 C112 H11F 108.9 . . ? H11E C112 H11F 107.7 . . ? N11 C113 C114 113.6(5) . . ? N11 C113 H11G 108.9 . . ? C114 C113 H11G 108.9 . . ? N11 C113 H11H 108.9 . . ? C114 C113 H11H 108.9 . . ? H11G C113 H11H 107.7 . . ? O15 C114 C113 109.1(5) . . ? O15 C114 H11I 109.9 . . ? C113 C114 H11I 109.9 . . ? O15 C114 H11J 109.9 . . ? C113 C114 H11J 109.9 . . ? H11I C114 H11J 108.3 . . ? O15 C115 C116 108.2(5) . . ? O15 C115 H11K 110.1 . . ? C116 C115 H11K 110.1 . . ? O15 C115 H11L 110.1 . . ? C116 C115 H11L 110.1 . . ? H11K C115 H11L 108.4 . . ? O16 C116 C115 108.3(5) . . ? O16 C116 H11M 110.0 . . ? C115 C116 H11M 110.0 . . ? O16 C116 H11N 110.0 . . ? C115 C116 H11N 110.0 . . ? H11M C116 H11N 108.4 . . ? O16 C117 C118 108.1(5) . . ? O16 C117 H11O 110.1 . . ? C118 C117 H11O 110.1 . . ? O16 C117 H11P 110.1 . . ? C118 C117 H11P 110.1 . . ? H11O C117 H11P 108.4 . . ? N12 C118 C117 113.4(5) . . ? N12 C118 H11Q 108.9 . . ? C117 C118 H11Q 108.9 . . ? N12 C118 H11R 108.9 . . ? C117 C118 H11R 108.9 . . ? H11Q C118 H11R 107.7 . . ? O21 K2 O24 134.58(13) . . ? O21 K2 O22 61.10(12) . . ? O24 K2 O22 94.99(12) . . ? O21 K2 O26 117.01(13) . . ? O24 K2 O26 102.39(12) . . ? O22 K2 O26 95.63(12) . . ? O21 K2 O25 96.00(12) . . ? O24 K2 O25 124.62(12) . . ? O22 K2 O25 135.02(12) . . ? O26 K2 O25 58.80(11) . . ? O21 K2 O23 94.91(12) . . ? O24 K2 O23 60.05(11) . . ? O22 K2 O23 116.73(12) . . ? O26 K2 O23 143.19(12) . . ? O25 K2 O23 102.47(12) . . ? O21 K2 N22 120.25(13) . . ? O24 K2 N22 60.97(12) . . ? O22 K2 N22 60.16(13) . . ? O26 K2 N22 60.15(13) . . ? O25 K2 N22 118.03(13) . . ? O23 K2 N22 120.22(13) . . ? O21 K2 N21 61.23(13) . . ? O24 K2 N21 118.05(12) . . ? O22 K2 N21 121.27(13) . . ? O26 K2 N21 119.53(13) . . ? O25 K2 N21 61.40(12) . . ? O23 K2 N21 59.03(12) . . ? N22 K2 N21 178.52(13) . . ? C207 N21 C201 109.0(5) . . ? C207 N21 C213 110.0(5) . . ? C201 N21 C213 110.4(5) . . ? C207 N21 K2 112.9(3) . . ? C201 N21 K2 107.8(3) . . ? C213 N21 K2 106.8(3) . . ? C212 N22 C218 109.4(5) . . ? C212 N22 C206 109.9(5) . . ? C218 N22 C206 108.7(5) . . ? C212 N22 K2 108.2(3) . . ? C218 N22 K2 110.7(3) . . ? C206 N22 K2 109.9(4) . . ? C202 O21 C203 109.9(5) . . ? C202 O21 K2 116.0(3) . . ? C203 O21 K2 112.8(3) . . ? C205 O22 C204 112.1(5) . . ? C205 O22 K2 117.6(3) . . ? C204 O22 K2 113.6(3) . . ? C208 O23 C209 111.1(4) . . ? C208 O23 K2 117.0(3) . . ? C209 O23 K2 113.9(3) . . ? C211 O24 C210 110.8(4) . . ? C211 O24 K2 118.5(3) . . ? C210 O24 K2 113.9(3) . . ? C215 O25 C214 110.7(5) . . ? C215 O25 K2 113.6(3) . . ? C214 O25 K2 116.7(3) . . ? C217 O26 C216 111.1(5) . . ? C217 O26 K2 117.0(3) . . ? C216 O26 K2 118.1(3) . . ? N21 C201 C202 113.0(5) . . ? N21 C201 H20A 109.0 . . ? C202 C201 H20A 109.0 . . ? N21 C201 H20B 109.0 . . ? C202 C201 H20B 109.0 . . ? H20A C201 H20B 107.8 . . ? O21 C202 C201 109.9(5) . . ? O21 C202 H20C 109.7 . . ? C201 C202 H20C 109.7 . . ? O21 C202 H20D 109.7 . . ? C201 C202 H20D 109.7 . . ? H20C C202 H20D 108.2 . . ? O21 C203 C204 109.3(6) . . ? O21 C203 H20E 109.8 . . ? C204 C203 H20E 109.8 . . ? O21 C203 H20F 109.8 . . ? C204 C203 H20F 109.8 . . ? H20E C203 H20F 108.3 . . ? O22 C204 C203 109.1(5) . . ? O22 C204 H20G 109.9 . . ? C203 C204 H20G 109.9 . . ? O22 C204 H20H 109.9 . . ? C203 C204 H20H 109.9 . . ? H20G C204 H20H 108.3 . . ? O22 C205 C206 109.0(5) . . ? O22 C205 H20I 109.9 . . ? C206 C205 H20I 109.9 . . ? O22 C205 H20J 109.9 . . ? C206 C205 H20J 109.9 . . ? H20I C205 H20J 108.3 . . ? N22 C206 C205 112.8(5) . . ? N22 C206 H20K 109.0 . . ? C205 C206 H20K 109.0 . . ? N22 C206 H20L 109.0 . . ? C205 C206 H20L 109.0 . . ? H20K C206 H20L 107.8 . . ? N21 C207 C208 113.4(5) . . ? N21 C207 H20M 108.9 . . ? C208 C207 H20M 108.9 . . ? N21 C207 H20N 108.9 . . ? C208 C207 H20N 108.9 . . ? H20M C207 H20N 107.7 . . ? O23 C208 C207 108.3(5) . . ? O23 C208 H20O 110.0 . . ? C207 C208 H20O 110.0 . . ? O23 C208 H20P 110.0 . . ? C207 C208 H20P 110.0 . . ? H20O C208 H20P 108.4 . . ? O23 C209 C210 109.1(5) . . ? O23 C209 H20Q 109.9 . . ? C210 C209 H20Q 109.9 . . ? O23 C209 H20R 109.9 . . ? C210 C209 H20R 109.9 . . ? H20Q C209 H20R 108.3 . . ? O24 C210 C209 109.2(5) . . ? O24 C210 H21A 109.8 . . ? C209 C210 H21A 109.8 . . ? O24 C210 H21B 109.8 . . ? C209 C210 H21B 109.8 . . ? H21A C210 H21B 108.3 . . ? O24 C211 C212 110.4(5) . . ? O24 C211 H21C 109.6 . . ? C212 C211 H21C 109.6 . . ? O24 C211 H21D 109.6 . . ? C212 C211 H21D 109.6 . . ? H21C C211 H21D 108.1 . . ? N22 C212 C211 113.6(5) . . ? N22 C212 H21E 108.9 . . ? C211 C212 H21E 108.9 . . ? N22 C212 H21F 108.9 . . ? C211 C212 H21F 108.9 . . ? H21E C212 H21F 107.7 . . ? N21 C213 C214 114.9(5) . . ? N21 C213 H21G 108.5 . . ? C214 C213 H21G 108.5 . . ? N21 C213 H21H 108.5 . . ? C214 C213 H21H 108.5 . . ? H21G C213 H21H 107.5 . . ? O25 C214 C213 110.0(5) . . ? O25 C214 H21I 109.7 . . ? C213 C214 H21I 109.7 . . ? O25 C214 H21J 109.7 . . ? C213 C214 H21J 109.7 . . ? H21I C214 H21J 108.2 . . ? O25 C215 C216 109.6(5) . . ? O25 C215 H21K 109.8 . . ? C216 C215 H21K 109.8 . . ? O25 C215 H21L 109.8 . . ? C216 C215 H21L 109.8 . . ? H21K C215 H21L 108.2 . . ? O26 C216 C215 108.9(5) . . ? O26 C216 H21M 109.9 . . ? C215 C216 H21M 109.9 . . ? O26 C216 H21N 109.9 . . ? C215 C216 H21N 109.9 . . ? H21M C216 H21N 108.3 . . ? O26 C217 C218 108.9(5) . . ? O26 C217 H21O 109.9 . . ? C218 C217 H21O 109.9 . . ? O26 C217 H21P 109.9 . . ? C218 C217 H21P 109.9 . . ? H21O C217 H21P 108.3 . . ? N22 C218 C217 113.8(5) . . ? N22 C218 H21Q 108.8 . . ? C217 C218 H21Q 108.8 . . ? N22 C218 H21R 108.8 . . ? C217 C218 H21R 108.8 . . ? H21Q C218 H21R 107.7 . . ? C1E N1E H1E4 109.5 . . ? C1E N1E H1E5 109.5 . . ? H1E4 N1E H1E5 109.5 . . ? C1E N1E H1E3 109.5 . . ? H1E4 N1E H1E3 109.5 . . ? H1E5 N1E H1E3 109.5 . . ? N1E C1E C2E 109.6(8) . . ? N1E C1E H1E1 109.7 . . ? C2E C1E H1E1 109.7 . . ? N1E C1E H1E2 109.7 . . ? C2E C1E H1E2 109.7 . . ? H1E1 C1E H1E2 108.2 . . ? N2E C2E C1E 108.2(8) . . ? N2E C2E H2E1 110.1 . . ? C1E C2E H2E1 110.1 . . ? N2E C2E H2E2 110.1 . . ? C1E C2E H2E2 110.1 . . ? H2E1 C2E H2E2 108.4 . . ? C2E N2E H2E3 109.5 . . ? C2E N2E H2E4 109.5 . . ? H2E3 N2E H2E4 109.5 . . ? C2E N2E H2E5 109.5 . . ? H2E3 N2E H2E5 109.5 . . ? H2E4 N2E H2E5 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.656 _refine_diff_density_min -1.221 _refine_diff_density_rms 0.133 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 736077' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K(2,2,2-crypt)]4[Zn(P7)2]*6py ; _contact_author_fax '+44 1865 272690' _chemical_name_common (K(2,2,2-crypt))4(Zn(P7)2)*6py _chemical_melting_point ? _chemical_formula_moiety '4(C18 H36 K N2 O6), P14 Zn, 6(C5 H5 N)' _chemical_formula_sum 'C102 H174 K4 N14 O24 P14 Zn' _chemical_formula_weight 2635.90 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' K K 0.2009 0.2494 '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 Orthorhombic _symmetry_space_group_name_H-M Fdd2 _symmetry_space_group_name_Hall 'F 2 -2d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 23.6766(2) _cell_length_b 74.2498(6) _cell_length_c 15.1492(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 26632.0(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8034 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _exptl_crystal_description needles _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11136 _exptl_absorpt_coefficient_mu 0.545 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8624 _exptl_absorpt_correction_T_max 0.9083 _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _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 14850 _diffrn_reflns_av_R_equivalents 0.0840 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -95 _diffrn_reflns_limit_k_max 96 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 5.12 _diffrn_reflns_theta_max 27.51 _reflns_number_total 14850 _reflns_number_gt 11990 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; KappaCCD software "Collect" (Nonius, 2000) ; _computing_cell_refinement ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_data_reduction ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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^)+(0.0558P)^2^+49.7941P] 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 0.467(11) _refine_ls_number_reflns 14850 _refine_ls_number_parameters 718 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1173 _refine_ls_wR_factor_gt 0.1060 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.002 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.2500 0.2500 0.22617(4) 0.03668(13) Uani 1 2 d S . . P1 P 0.18302(4) 0.216266(13) 0.28082(6) 0.0384(2) Uani 1 1 d . . . P2 P 0.17920(3) 0.230509(12) 0.15334(6) 0.03487(18) Uani 1 1 d . . . P3 P 0.27313(4) 0.221679(12) 0.30756(6) 0.0390(2) Uani 1 1 d . . . P4 P 0.18141(4) 0.188077(13) 0.24489(7) 0.0434(2) Uani 1 1 d . . . P5 P 0.24512(4) 0.215930(12) 0.08435(6) 0.03414(18) Uani 1 1 d . . . P6 P 0.30912(4) 0.209968(12) 0.18932(6) 0.0371(2) Uani 1 1 d . . . P7 P 0.24745(4) 0.188464(12) 0.14860(6) 0.0390(2) Uani 1 1 d . . . K1 K 0.09709(3) 0.245480(10) 0.70573(5) 0.03721(16) Uani 1 1 d . . . K2 K 0.01071(3) 0.156090(9) 0.90946(5) 0.03554(16) Uani 1 1 d . . . N11 N 0.14982(14) 0.21723(4) 0.5913(2) 0.0478(8) Uani 1 1 d . . . N12 N 0.04473(15) 0.27358(4) 0.8222(2) 0.0518(8) Uani 1 1 d . . . N21 N -0.04602(13) 0.12277(4) 0.8364(2) 0.0452(7) Uani 1 1 d . . . N22 N 0.06897(11) 0.18900(4) 0.9808(2) 0.0359(6) Uani 1 1 d . . . O11 O 0.02746(12) 0.22076(4) 0.60984(19) 0.0540(7) Uani 1 1 d . . . O12 O -0.01662(10) 0.24238(4) 0.74815(18) 0.0477(6) Uani 1 1 d . . . O13 O 0.17773(10) 0.22041(4) 0.77986(18) 0.0481(6) Uani 1 1 d . . . O14 O 0.14550(12) 0.25237(4) 0.87063(18) 0.0515(7) Uani 1 1 d . . . O15 O 0.15882(10) 0.25657(4) 0.55797(16) 0.0443(6) Uani 1 1 d . . . O16 O 0.08731(11) 0.28194(3) 0.64740(17) 0.0466(6) Uani 1 1 d . . . O21 O 0.06868(11) 0.13322(3) 0.78474(18) 0.0468(6) Uani 1 1 d . . . O22 O 0.12798(10) 0.16060(3) 0.87479(17) 0.0426(6) Uani 1 1 d . . . O23 O -0.03134(11) 0.13000(3) 1.02753(18) 0.0466(6) Uani 1 1 d . . . O24 O 0.00360(11) 0.16437(3) 1.09270(16) 0.0443(6) Uani 1 1 d . . . O25 O -0.09029(10) 0.15892(3) 0.81485(18) 0.0445(6) Uani 1 1 d . . . O26 O -0.02636(9) 0.19044(3) 0.85530(16) 0.0394(5) Uani 1 1 d . . . C101 C 0.1067(2) 0.20845(6) 0.5351(3) 0.0626(11) Uani 1 1 d . . . H10A H 0.1224 0.1970 0.5118 0.075 Uiso 1 1 calc R . . H10B H 0.0985 0.2164 0.4841 0.075 Uiso 1 1 calc R . . C102 C 0.0528(2) 0.20447(7) 0.5820(4) 0.0694(13) Uani 1 1 d . . . H10C H 0.0268 0.1979 0.5420 0.083 Uiso 1 1 calc R . . H10D H 0.0604 0.1967 0.6338 0.083 Uiso 1 1 calc R . . C103 C -0.02636(18) 0.21769(6) 0.6514(3) 0.0605(11) Uani 1 1 d . . . H10E H -0.0215 0.2097 0.7033 0.073 Uiso 1 1 calc R . . H10F H -0.0523 0.2117 0.6094 0.073 Uiso 1 1 calc R . . C104 C -0.05040(16) 0.23520(7) 0.6795(3) 0.0581(11) Uani 1 1 d . . . H10G H -0.0512 0.2436 0.6289 0.070 Uiso 1 1 calc R . . H10H H -0.0896 0.2335 0.7006 0.070 Uiso 1 1 calc R . . C105 C -0.04456(17) 0.25755(6) 0.7893(3) 0.0601(11) Uani 1 1 d . . . H10I H -0.0803 0.2535 0.8170 0.072 Uiso 1 1 calc R . . H10J H -0.0539 0.2667 0.7441 0.072 Uiso 1 1 calc R . . C106 C -0.0074(2) 0.26561(7) 0.8572(3) 0.0651(12) Uani 1 1 d . . . H10K H -0.0287 0.2750 0.8891 0.078 Uiso 1 1 calc R . . H10L H 0.0028 0.2562 0.9006 0.078 Uiso 1 1 calc R . . C107 C 0.1754(2) 0.20339(6) 0.6476(3) 0.0617(12) Uani 1 1 d . . . H10M H 0.1985 0.1953 0.6102 0.074 Uiso 1 1 calc R . . H10N H 0.1450 0.1961 0.6743 0.074 Uiso 1 1 calc R . . C108 C 0.21134(19) 0.21059(7) 0.7187(3) 0.0630(12) Uani 1 1 d . . . H10O H 0.2306 0.2006 0.7494 0.076 Uiso 1 1 calc R . . H10P H 0.2406 0.2186 0.6933 0.076 Uiso 1 1 calc R . . C109 C 0.21200(18) 0.22847(6) 0.8459(3) 0.0581(11) Uani 1 1 d . . . H10Q H 0.2391 0.2369 0.8178 0.070 Uiso 1 1 calc R . . H10R H 0.2340 0.2190 0.8766 0.070 Uiso 1 1 calc R . . C110 C 0.17695(17) 0.23853(6) 0.9119(3) 0.0518(10) Uani 1 1 d . . . H11A H 0.1508 0.2301 0.9416 0.062 Uiso 1 1 calc R . . H11B H 0.2019 0.2438 0.9575 0.062 Uiso 1 1 calc R . . C111 C 0.1127(2) 0.26169(7) 0.9359(3) 0.0665(12) Uani 1 1 d . . . H11C H 0.1376 0.2657 0.9847 0.080 Uiso 1 1 calc R . . H11D H 0.0839 0.2535 0.9607 0.080 Uiso 1 1 calc R . . C112 C 0.0842(2) 0.27778(6) 0.8947(3) 0.0647(12) Uani 1 1 d . . . H11E H 0.0633 0.2843 0.9414 0.078 Uiso 1 1 calc R . . H11F H 0.1137 0.2860 0.8719 0.078 Uiso 1 1 calc R . . C113 C 0.19251(17) 0.22644(6) 0.5353(2) 0.0514(10) Uani 1 1 d . . . H11G H 0.2056 0.2180 0.4890 0.062 Uiso 1 1 calc R . . H11H H 0.2255 0.2296 0.5722 0.062 Uiso 1 1 calc R . . C114 C 0.17018(17) 0.24317(6) 0.4920(2) 0.0487(9) Uani 1 1 d . . . H11I H 0.1983 0.2478 0.4493 0.058 Uiso 1 1 calc R . . H11J H 0.1351 0.2403 0.4593 0.058 Uiso 1 1 calc R . . C115 C 0.13567(18) 0.27232(5) 0.5178(3) 0.0511(10) Uani 1 1 d . . . H11K H 0.0981 0.2695 0.4925 0.061 Uiso 1 1 calc R . . H11L H 0.1607 0.2765 0.4695 0.061 Uiso 1 1 calc R . . C116 C 0.13024(17) 0.28670(6) 0.5858(3) 0.0511(9) Uani 1 1 d . . . H11M H 0.1667 0.2882 0.6169 0.061 Uiso 1 1 calc R . . H11N H 0.1205 0.2983 0.5570 0.061 Uiso 1 1 calc R . . C117 C 0.0792(2) 0.29575(6) 0.7119(3) 0.0566(10) Uani 1 1 d . . . H11O H 0.0694 0.3073 0.6826 0.068 Uiso 1 1 calc R . . H11P H 0.1143 0.2976 0.7463 0.068 Uiso 1 1 calc R . . C118 C 0.0317(2) 0.29003(6) 0.7727(3) 0.0585(11) Uani 1 1 d . . . H11Q H 0.0237 0.2999 0.8149 0.070 Uiso 1 1 calc R . . H11R H -0.0029 0.2880 0.7372 0.070 Uiso 1 1 calc R . . C201 C -0.01398(18) 0.11538(6) 0.7626(3) 0.0568(11) Uani 1 1 d . . . H20A H -0.0226 0.1225 0.7091 0.068 Uiso 1 1 calc R . . H20B H -0.0270 0.1029 0.7517 0.068 Uiso 1 1 calc R . . C202 C 0.04926(18) 0.11514(5) 0.7758(3) 0.0547(10) Uani 1 1 d . . . H20C H 0.0588 0.1082 0.8295 0.066 Uiso 1 1 calc R . . H20D H 0.0678 0.1093 0.7246 0.066 Uiso 1 1 calc R . . C203 C 0.12893(16) 0.13394(6) 0.7875(3) 0.0527(10) Uani 1 1 d . . . H20E H 0.1448 0.1285 0.7333 0.063 Uiso 1 1 calc R . . H20F H 0.1430 0.1271 0.8390 0.063 Uiso 1 1 calc R . . C204 C 0.14711(17) 0.15322(6) 0.7942(3) 0.0544(10) Uani 1 1 d . . . H20G H 0.1888 0.1540 0.7912 0.065 Uiso 1 1 calc R . . H20H H 0.1313 0.1602 0.7442 0.065 Uiso 1 1 calc R . . C205 C 0.14999(15) 0.17841(5) 0.8880(3) 0.0482(9) Uani 1 1 d . . . H20I H 0.1371 0.1864 0.8396 0.058 Uiso 1 1 calc R . . H20J H 0.1918 0.1780 0.8867 0.058 Uiso 1 1 calc R . . C206 C 0.13044(14) 0.18589(5) 0.9751(3) 0.0448(9) Uani 1 1 d . . . H20K H 0.1416 0.1774 1.0225 0.054 Uiso 1 1 calc R . . H20L H 0.1502 0.1974 0.9859 0.054 Uiso 1 1 calc R . . C207 C -0.04799(18) 0.10930(5) 0.9084(3) 0.0517(10) Uani 1 1 d . . . H20M H -0.0095 0.1044 0.9174 0.062 Uiso 1 1 calc R . . H20N H -0.0726 0.0992 0.8899 0.062 Uiso 1 1 calc R . . C208 C -0.06942(17) 0.11665(5) 0.9950(3) 0.0522(10) Uani 1 1 d . . . H20O H -0.1073 0.1220 0.9866 0.063 Uiso 1 1 calc R . . H20P H -0.0728 0.1068 1.0385 0.063 Uiso 1 1 calc R . . C209 C -0.05213(19) 0.13777(6) 1.1077(3) 0.0560(10) Uani 1 1 d . . . H20Q H -0.0631 0.1281 1.1495 0.067 Uiso 1 1 calc R . . H20R H -0.0859 0.1452 1.0952 0.067 Uiso 1 1 calc R . . C210 C -0.00631(18) 0.14928(6) 1.1477(3) 0.0516(10) Uani 1 1 d . . . H21A H -0.0180 0.1534 1.2072 0.062 Uiso 1 1 calc R . . H21B H 0.0288 0.1422 1.1539 0.062 Uiso 1 1 calc R . . C211 C 0.04849(16) 0.17513(5) 1.1272(2) 0.0447(9) Uani 1 1 d . . . H21C H 0.0844 0.1683 1.1249 0.054 Uiso 1 1 calc R . . H21D H 0.0407 0.1782 1.1897 0.054 Uiso 1 1 calc R . . C212 C 0.05380(16) 0.19217(5) 1.0735(2) 0.0431(8) Uani 1 1 d . . . H21E H 0.0174 0.1987 1.0756 0.052 Uiso 1 1 calc R . . H21F H 0.0829 0.2000 1.1008 0.052 Uiso 1 1 calc R . . C213 C -0.10349(17) 0.12717(5) 0.8069(3) 0.0532(10) Uani 1 1 d . . . H21G H -0.1286 0.1279 0.8590 0.064 Uiso 1 1 calc R . . H21H H -0.1175 0.1173 0.7686 0.064 Uiso 1 1 calc R . . C214 C -0.10687(18) 0.14477(5) 0.7566(3) 0.0522(10) Uani 1 1 d . . . H21I H -0.0815 0.1444 0.7047 0.063 Uiso 1 1 calc R . . H21J H -0.1459 0.1468 0.7356 0.063 Uiso 1 1 calc R . . C215 C -0.10114(16) 0.17624(5) 0.7756(3) 0.0460(9) Uani 1 1 d . . . H21K H -0.1415 0.1772 0.7594 0.055 Uiso 1 1 calc R . . H21L H -0.0783 0.1777 0.7213 0.055 Uiso 1 1 calc R . . C216 C -0.08609(14) 0.19051(5) 0.8405(3) 0.0432(8) Uani 1 1 d . . . H21M H -0.0979 0.2024 0.8177 0.052 Uiso 1 1 calc R . . H21N H -0.1061 0.1883 0.8969 0.052 Uiso 1 1 calc R . . C217 C -0.00999(14) 0.20539(4) 0.9090(3) 0.0387(7) Uani 1 1 d . . . H21O H -0.0314 0.2052 0.9651 0.046 Uiso 1 1 calc R . . H21P H -0.0190 0.2168 0.8780 0.046 Uiso 1 1 calc R . . C218 C 0.05231(15) 0.20453(4) 0.9279(3) 0.0413(8) Uani 1 1 d . . . H21Q H 0.0731 0.2042 0.8712 0.050 Uiso 1 1 calc R . . H21R H 0.0637 0.2156 0.9593 0.050 Uiso 1 1 calc R . . N1Q N 0.1405(3) 0.33723(8) 0.8176(4) 0.1112(19) Uani 1 1 d . . . C1Q C 0.1855(2) 0.32681(7) 0.8432(4) 0.0672(12) Uani 1 1 d . . . H1Q H 0.2175 0.3253 0.8059 0.081 Uiso 1 1 calc R . . C2Q C 0.1828(2) 0.31900(6) 0.9215(4) 0.0670(13) Uani 1 1 d . . . H2Q H 0.2140 0.3119 0.9402 0.080 Uiso 1 1 calc R . . C3Q C 0.1376(2) 0.32057(6) 0.9768(4) 0.0678(13) Uani 1 1 d . . . H3Q H 0.1370 0.3147 1.0326 0.081 Uiso 1 1 calc R . . C4Q C 0.0927(2) 0.33105(7) 0.9486(4) 0.0772(15) Uani 1 1 d . . . H4Q H 0.0604 0.3323 0.9854 0.093 Uiso 1 1 calc R . . C5Q C 0.0940(2) 0.33946(8) 0.8700(4) 0.0733(14) Uani 1 1 d . . . H5Q H 0.0633 0.3468 0.8512 0.088 Uiso 1 1 calc R . . N1S N 0.0796(5) 0.14030(13) 0.5479(6) 0.181(4) Uani 1 1 d . . . C1S C 0.1251(3) 0.15266(10) 0.5226(5) 0.106(2) Uani 1 1 d . . . H1S H 0.1565 0.1549 0.5598 0.127 Uiso 1 1 calc R . . C2S C 0.1194(3) 0.16080(8) 0.4419(4) 0.0853(17) Uani 1 1 d . . . H2S H 0.1461 0.1695 0.4230 0.102 Uiso 1 1 calc R . . C3S C 0.0762(4) 0.15633(12) 0.3905(6) 0.108(2) Uani 1 1 d . . . H3S H 0.0726 0.1621 0.3349 0.130 Uiso 1 1 calc R . . C4S C 0.0399(4) 0.14482(15) 0.4118(8) 0.133(3) Uani 1 1 d . . . H4S H 0.0111 0.1418 0.3706 0.159 Uiso 1 1 calc R . . C5S C 0.0401(4) 0.13675(13) 0.4891(9) 0.137(3) Uani 1 1 d . . . H5S H 0.0114 0.1282 0.5028 0.164 Uiso 1 1 calc R . . N1P N 0.2108(3) 0.34703(9) 0.5856(5) 0.122(2) Uani 1 1 d . . . C1P C 0.2161(3) 0.35758(8) 0.5086(6) 0.099(2) Uani 1 1 d . . . H1P H 0.2152 0.3704 0.5116 0.118 Uiso 1 1 calc R . . C2P C 0.2224(2) 0.34904(10) 0.4303(5) 0.097(2) Uani 1 1 d . . . H2P H 0.2258 0.3560 0.3778 0.116 Uiso 1 1 calc R . . C3P C 0.2241(2) 0.33082(8) 0.4253(4) 0.0789(15) Uani 1 1 d . . . H3P H 0.2300 0.3252 0.3699 0.095 Uiso 1 1 calc R . . C4P C 0.2174(2) 0.32081(8) 0.4971(5) 0.0804(16) Uani 1 1 d . . . H4P H 0.2176 0.3080 0.4931 0.096 Uiso 1 1 calc R . . C5P C 0.2102(2) 0.32932(8) 0.5786(4) 0.0853(16) Uani 1 1 d . . . H5P H 0.2048 0.3222 0.6300 0.102 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0461(3) 0.0275(3) 0.0364(3) 0.000 0.000 0.0002(2) P1 0.0427(5) 0.0406(5) 0.0320(4) 0.0022(4) 0.0000(4) 0.0003(4) P2 0.0355(4) 0.0368(5) 0.0324(4) 0.0024(4) -0.0049(4) 0.0058(4) P3 0.0495(5) 0.0327(5) 0.0349(5) 0.0010(4) -0.0145(4) -0.0033(4) P4 0.0480(5) 0.0366(5) 0.0455(5) 0.0064(4) -0.0064(4) -0.0104(4) P5 0.0379(4) 0.0347(4) 0.0298(4) 0.0008(3) -0.0029(3) 0.0028(3) P6 0.0322(4) 0.0331(4) 0.0460(5) 0.0024(4) -0.0086(4) 0.0019(3) P7 0.0450(5) 0.0286(4) 0.0432(5) -0.0029(4) -0.0079(4) 0.0001(4) K1 0.0361(4) 0.0440(4) 0.0316(4) 0.0024(3) 0.0005(3) 0.0013(3) K2 0.0381(4) 0.0299(4) 0.0387(4) 0.0020(3) -0.0056(3) -0.0007(3) N11 0.0598(19) 0.0523(19) 0.0313(15) 0.0060(13) 0.0064(14) 0.0171(15) N12 0.070(2) 0.0472(19) 0.0379(18) -0.0022(14) 0.0008(16) 0.0080(16) N21 0.0511(17) 0.0312(16) 0.0532(19) 0.0001(14) -0.0120(15) -0.0005(13) N22 0.0340(14) 0.0324(14) 0.0415(16) 0.0003(12) -0.0085(12) -0.0031(11) O11 0.0572(16) 0.0526(17) 0.0523(17) -0.0049(13) 0.0036(13) -0.0124(13) O12 0.0376(12) 0.0564(16) 0.0490(15) 0.0030(12) 0.0016(11) 0.0036(11) O13 0.0425(13) 0.0604(17) 0.0416(14) 0.0076(13) -0.0034(11) 0.0038(12) O14 0.0658(17) 0.0526(16) 0.0361(14) 0.0068(12) -0.0091(13) -0.0013(13) O15 0.0469(14) 0.0528(15) 0.0331(13) 0.0105(11) 0.0067(11) 0.0104(11) O16 0.0576(15) 0.0427(14) 0.0396(14) -0.0005(11) 0.0067(12) -0.0003(11) O21 0.0507(14) 0.0410(14) 0.0486(15) -0.0067(11) -0.0044(12) 0.0057(11) O22 0.0428(13) 0.0417(14) 0.0433(14) -0.0023(11) 0.0051(11) -0.0035(11) O23 0.0534(15) 0.0390(14) 0.0475(15) 0.0065(11) -0.0012(12) -0.0112(11) O24 0.0510(14) 0.0440(14) 0.0379(14) 0.0030(11) -0.0054(11) -0.0077(11) O25 0.0494(14) 0.0333(13) 0.0508(15) 0.0018(11) -0.0229(12) 0.0012(10) O26 0.0368(12) 0.0332(12) 0.0483(14) 0.0003(10) -0.0080(11) 0.0027(10) C101 0.081(3) 0.057(3) 0.050(3) -0.012(2) 0.003(2) 0.001(2) C102 0.083(3) 0.056(3) 0.069(3) -0.008(2) 0.002(3) -0.011(2) C103 0.051(2) 0.077(3) 0.054(2) 0.002(2) -0.001(2) -0.029(2) C104 0.037(2) 0.078(3) 0.060(3) 0.013(2) -0.0072(18) -0.0119(19) C105 0.042(2) 0.068(3) 0.070(3) 0.002(2) 0.017(2) 0.0112(19) C106 0.076(3) 0.069(3) 0.050(3) 0.003(2) 0.024(2) 0.009(2) C107 0.080(3) 0.057(3) 0.049(2) 0.012(2) 0.014(2) 0.029(2) C108 0.059(2) 0.080(3) 0.050(3) 0.014(2) 0.005(2) 0.024(2) C109 0.050(2) 0.070(3) 0.055(3) 0.015(2) -0.018(2) -0.012(2) C110 0.056(2) 0.061(3) 0.039(2) 0.0146(18) -0.0151(18) -0.0163(19) C111 0.093(3) 0.071(3) 0.035(2) 0.000(2) -0.005(2) -0.001(3) C112 0.100(4) 0.053(3) 0.041(2) -0.0119(19) -0.007(2) 0.006(2) C113 0.055(2) 0.067(3) 0.0316(19) 0.0069(18) 0.0094(17) 0.024(2) C114 0.052(2) 0.064(3) 0.0301(18) 0.0043(17) 0.0091(16) 0.0133(18) C115 0.054(2) 0.058(2) 0.042(2) 0.0148(19) 0.0073(17) 0.0103(19) C116 0.051(2) 0.051(2) 0.052(2) 0.0142(18) 0.0037(19) -0.0016(18) C117 0.079(3) 0.042(2) 0.049(2) 0.0000(18) -0.006(2) 0.0028(19) C118 0.080(3) 0.053(2) 0.042(2) -0.0027(19) 0.006(2) 0.019(2) C201 0.063(2) 0.049(2) 0.058(3) -0.018(2) -0.017(2) 0.0014(19) C202 0.067(3) 0.036(2) 0.061(3) -0.0158(19) -0.006(2) 0.0083(18) C203 0.049(2) 0.056(2) 0.054(2) -0.0096(19) 0.0048(19) 0.0072(18) C204 0.051(2) 0.062(3) 0.050(2) -0.0038(19) 0.0141(19) 0.0016(19) C205 0.0357(18) 0.039(2) 0.070(3) 0.0083(18) 0.0034(18) -0.0046(15) C206 0.0337(17) 0.0389(19) 0.062(2) -0.0037(17) -0.0122(17) -0.0013(14) C207 0.060(2) 0.0298(19) 0.066(3) 0.0055(18) -0.021(2) -0.0053(16) C208 0.053(2) 0.042(2) 0.062(3) 0.0131(19) -0.0061(19) -0.0164(17) C209 0.061(2) 0.061(3) 0.046(2) 0.0064(19) 0.007(2) -0.014(2) C210 0.063(2) 0.057(2) 0.035(2) 0.0019(17) 0.0041(18) -0.0039(19) C211 0.051(2) 0.046(2) 0.037(2) 0.0002(16) -0.0131(16) -0.0011(16) C212 0.0488(19) 0.0378(19) 0.043(2) -0.0078(15) -0.0081(16) 0.0007(15) C213 0.053(2) 0.039(2) 0.068(3) -0.0009(19) -0.022(2) -0.0092(17) C214 0.058(2) 0.038(2) 0.061(3) -0.0045(18) -0.0256(19) -0.0006(17) C215 0.047(2) 0.0354(19) 0.055(2) 0.0076(17) -0.0220(18) 0.0009(15) C216 0.0348(17) 0.0360(19) 0.059(2) 0.0034(16) -0.0129(16) 0.0022(14) C217 0.0437(18) 0.0270(16) 0.045(2) 0.0011(15) -0.0106(16) 0.0030(14) C218 0.0438(19) 0.0292(17) 0.051(2) 0.0029(15) -0.0102(16) -0.0061(14) N1Q 0.144(5) 0.100(4) 0.090(4) -0.009(3) -0.021(4) -0.003(4) C1Q 0.067(3) 0.068(3) 0.067(3) -0.003(2) 0.000(2) 0.010(2) C2Q 0.059(3) 0.055(3) 0.087(4) -0.001(3) -0.012(3) 0.005(2) C3Q 0.067(3) 0.055(3) 0.081(3) 0.008(2) -0.013(3) -0.014(2) C4Q 0.061(3) 0.077(3) 0.094(4) 0.000(3) -0.015(3) -0.007(2) C5Q 0.071(3) 0.079(4) 0.069(3) 0.001(3) -0.018(3) 0.008(3) N1S 0.244(11) 0.164(8) 0.134(7) 0.050(6) -0.004(7) -0.053(7) C1S 0.102(5) 0.129(6) 0.085(5) -0.018(4) -0.009(4) -0.015(4) C2S 0.108(5) 0.067(3) 0.081(4) -0.008(3) 0.040(4) 0.002(3) C3S 0.115(6) 0.111(6) 0.099(5) -0.004(4) -0.027(5) 0.030(5) C4S 0.113(6) 0.147(8) 0.138(8) -0.003(7) -0.067(6) -0.010(6) C5S 0.110(6) 0.131(7) 0.169(10) 0.004(7) -0.018(6) -0.050(5) N1P 0.118(5) 0.102(5) 0.145(6) -0.020(4) 0.039(4) -0.001(4) C1P 0.096(4) 0.058(3) 0.141(6) 0.004(4) 0.051(4) 0.009(3) C2P 0.076(4) 0.101(5) 0.113(5) 0.034(4) 0.028(4) 0.012(3) C3P 0.055(3) 0.085(4) 0.097(4) 0.009(3) 0.011(3) 0.007(3) C4P 0.062(3) 0.072(3) 0.107(5) 0.008(3) 0.005(3) 0.002(3) C5P 0.089(4) 0.074(4) 0.092(4) 0.013(3) 0.021(3) -0.001(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 P2 2.4742(9) . ? Zn1 P2 2.4742(9) 14 ? Zn1 P3 2.4984(9) . ? Zn1 P3 2.4984(9) 14 ? P1 P4 2.1630(14) . ? P1 P2 2.2037(12) . ? P1 P3 2.2084(13) . ? P2 P5 2.1679(12) . ? P3 P6 2.1658(14) . ? P4 P7 2.1387(14) . ? P5 P6 2.2407(12) . ? P5 P7 2.2604(12) . ? P6 P7 2.2498(12) . ? K1 O12 2.777(3) . ? K1 O14 2.796(3) . ? K1 O15 2.797(2) . ? K1 O16 2.857(3) . ? K1 O11 2.863(3) . ? K1 O13 2.893(3) . ? K1 N11 2.994(3) . ? K1 N12 3.001(3) . ? K2 O25 2.796(2) . ? K2 O23 2.818(3) . ? K2 O26 2.819(2) . ? K2 O22 2.845(3) . ? K2 O24 2.848(3) . ? K2 O21 2.888(3) . ? K2 N22 3.007(3) . ? K2 N21 3.025(3) . ? N11 C107 1.466(5) . ? N11 C101 1.481(6) . ? N11 C113 1.487(5) . ? N12 C118 1.467(5) . ? N12 C106 1.467(6) . ? N12 C112 1.476(6) . ? N21 C201 1.458(6) . ? N21 C213 1.469(5) . ? N21 C207 1.481(5) . ? N22 C218 1.458(4) . ? N22 C212 1.469(5) . ? N22 C206 1.476(4) . ? O11 C102 1.415(6) . ? O11 C103 1.439(5) . ? O12 C104 1.416(5) . ? O12 C105 1.448(5) . ? O13 C109 1.421(5) . ? O13 C108 1.423(5) . ? O14 C110 1.415(5) . ? O14 C111 1.435(5) . ? O15 C115 1.427(4) . ? O15 C114 1.436(5) . ? O16 C116 1.425(5) . ? O16 C117 1.430(5) . ? O21 C202 1.425(5) . ? O21 C203 1.428(5) . ? O22 C204 1.413(5) . ? O22 C205 1.436(4) . ? O23 C208 1.427(4) . ? O23 C209 1.432(5) . ? O24 C210 1.416(5) . ? O24 C211 1.429(4) . ? O25 C214 1.427(4) . ? O25 C215 1.440(4) . ? O26 C217 1.429(4) . ? O26 C216 1.432(4) . ? C101 C102 1.489(7) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.481(7) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C105 C106 1.480(7) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 C108 1.473(7) . ? C107 H10M 0.9900 . ? C107 H10N 0.9900 . ? C108 H10O 0.9900 . ? C108 H10P 0.9900 . ? C109 C110 1.499(7) . ? C109 H10Q 0.9900 . ? C109 H10R 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.508(6) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 C114 1.501(5) . ? C113 H11G 0.9900 . ? C113 H11H 0.9900 . ? C114 H11I 0.9900 . ? C114 H11J 0.9900 . ? C115 C116 1.488(6) . ? C115 H11K 0.9900 . ? C115 H11L 0.9900 . ? C116 H11M 0.9900 . ? C116 H11N 0.9900 . ? C117 C118 1.514(6) . ? C117 H11O 0.9900 . ? C117 H11P 0.9900 . ? C118 H11Q 0.9900 . ? C118 H11R 0.9900 . ? C201 C202 1.511(6) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C203 C204 1.498(6) . ? C203 H20E 0.9900 . ? C203 H20F 0.9900 . ? C204 H20G 0.9900 . ? C204 H20H 0.9900 . ? C205 C206 1.504(6) . ? C205 H20I 0.9900 . ? C205 H20J 0.9900 . ? C206 H20K 0.9900 . ? C206 H20L 0.9900 . ? C207 C208 1.510(6) . ? C207 H20M 0.9900 . ? C207 H20N 0.9900 . ? C208 H20O 0.9900 . ? C208 H20P 0.9900 . ? C209 C210 1.508(6) . ? C209 H20Q 0.9900 . ? C209 H20R 0.9900 . ? C210 H21A 0.9900 . ? C210 H21B 0.9900 . ? C211 C212 1.510(5) . ? C211 H21C 0.9900 . ? C211 H21D 0.9900 . ? C212 H21E 0.9900 . ? C212 H21F 0.9900 . ? C213 C214 1.515(5) . ? C213 H21G 0.9900 . ? C213 H21H 0.9900 . ? C214 H21I 0.9900 . ? C214 H21J 0.9900 . ? C215 C216 1.489(5) . ? C215 H21K 0.9900 . ? C215 H21L 0.9900 . ? C216 H21M 0.9900 . ? C216 H21N 0.9900 . ? C217 C218 1.504(5) . ? C217 H21O 0.9900 . ? C217 H21P 0.9900 . ? C218 H21Q 0.9900 . ? C218 H21R 0.9900 . ? N1Q C5Q 1.367(8) . ? N1Q C1Q 1.372(8) . ? C1Q C2Q 1.322(7) . ? C1Q H1Q 0.9500 . ? C2Q C3Q 1.364(7) . ? C2Q H2Q 0.9500 . ? C3Q C4Q 1.386(7) . ? C3Q H3Q 0.9500 . ? C4Q C5Q 1.346(8) . ? C4Q H4Q 0.9500 . ? C5Q H5Q 0.9500 . ? N1S C5S 1.317(12) . ? N1S C1S 1.466(11) . ? C1S C2S 1.369(10) . ? C1S H1S 0.9500 . ? C2S C3S 1.328(10) . ? C2S H2S 0.9500 . ? C3S C4S 1.255(11) . ? C3S H3S 0.9500 . ? C4S C5S 1.316(13) . ? C4S H4S 0.9500 . ? C5S H5S 0.9500 . ? N1P C5P 1.320(8) . ? N1P C1P 1.411(9) . ? C1P C2P 1.353(10) . ? C1P H1P 0.9500 . ? C2P C3P 1.356(8) . ? C2P H2P 0.9500 . ? C3P C4P 1.325(8) . ? C3P H3P 0.9500 . ? C4P C5P 1.398(9) . ? C4P H4P 0.9500 . ? C5P H5P 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Zn1 P2 127.03(5) . 14 ? P2 Zn1 P3 82.89(3) . . ? P2 Zn1 P3 124.33(3) 14 . ? P2 Zn1 P3 124.33(3) . 14 ? P2 Zn1 P3 82.89(3) 14 14 ? P3 Zn1 P3 120.86(5) . 14 ? P4 P1 P2 104.07(5) . . ? P4 P1 P3 103.85(5) . . ? P2 P1 P3 96.49(5) . . ? P5 P2 P1 98.82(5) . . ? P5 P2 Zn1 91.11(4) . . ? P1 P2 Zn1 82.07(4) . . ? P6 P3 P1 98.94(5) . . ? P6 P3 Zn1 90.92(4) . . ? P1 P3 Zn1 81.43(4) . . ? P7 P4 P1 98.38(5) . . ? P2 P5 P6 104.08(5) . . ? P2 P5 P7 105.10(5) . . ? P6 P5 P7 59.98(4) . . ? P3 P6 P5 103.98(5) . . ? P3 P6 P7 104.85(5) . . ? P5 P6 P7 60.45(4) . . ? P4 P7 P6 107.28(5) . . ? P4 P7 P5 106.74(5) . . ? P6 P7 P5 59.58(4) . . ? O12 K1 O14 101.88(9) . . ? O12 K1 O15 135.73(8) . . ? O14 K1 O15 116.55(8) . . ? O12 K1 O16 94.10(8) . . ? O14 K1 O16 97.83(8) . . ? O15 K1 O16 61.04(8) . . ? O12 K1 O11 60.40(8) . . ? O14 K1 O11 143.78(9) . . ? O15 K1 O11 94.80(8) . . ? O16 K1 O11 113.81(9) . . ? O12 K1 O13 119.77(8) . . ? O14 K1 O13 60.02(8) . . ? O15 K1 O13 98.93(8) . . ? O16 K1 O13 141.55(8) . . ? O11 K1 O13 99.47(8) . . ? O12 K1 N11 118.69(9) . . ? O14 K1 N11 118.33(9) . . ? O15 K1 N11 61.65(8) . . ? O16 K1 N11 121.24(8) . . ? O11 K1 N11 59.82(9) . . ? O13 K1 N11 59.92(8) . . ? O12 K1 N12 61.39(9) . . ? O14 K1 N12 61.09(9) . . ? O15 K1 N12 118.80(9) . . ? O16 K1 N12 59.31(8) . . ? O11 K1 N12 120.41(9) . . ? O13 K1 N12 119.45(9) . . ? N11 K1 N12 179.35(10) . . ? O25 K2 O23 94.29(8) . . ? O25 K2 O26 61.09(7) . . ? O23 K2 O26 134.15(8) . . ? O25 K2 O22 136.98(8) . . ? O23 K2 O22 122.86(8) . . ? O26 K2 O22 98.26(7) . . ? O25 K2 O24 115.65(8) . . ? O23 K2 O24 60.59(8) . . ? O26 K2 O24 94.01(8) . . ? O22 K2 O24 102.25(7) . . ? O25 K2 O21 96.62(8) . . ? O23 K2 O21 100.31(8) . . ? O26 K2 O21 119.32(8) . . ? O22 K2 O21 58.98(7) . . ? O24 K2 O21 142.45(8) . . ? O25 K2 N22 121.03(7) . . ? O23 K2 N22 119.51(8) . . ? O26 K2 N22 60.80(7) . . ? O22 K2 N22 61.51(8) . . ? O24 K2 N22 60.10(8) . . ? O21 K2 N22 119.66(8) . . ? O25 K2 N21 59.60(8) . . ? O23 K2 N21 60.88(9) . . ? O26 K2 N21 119.67(8) . . ? O22 K2 N21 117.51(8) . . ? O24 K2 N21 120.47(9) . . ? O21 K2 N21 59.38(8) . . ? N22 K2 N21 179.02(9) . . ? C107 N11 C101 108.1(4) . . ? C107 N11 C113 111.9(3) . . ? C101 N11 C113 110.1(3) . . ? C107 N11 K1 109.1(2) . . ? C101 N11 K1 110.7(2) . . ? C113 N11 K1 107.0(2) . . ? C118 N12 C106 110.1(4) . . ? C118 N12 C112 109.8(3) . . ? C106 N12 C112 110.4(4) . . ? C118 N12 K1 111.4(2) . . ? C106 N12 K1 106.2(2) . . ? C112 N12 K1 108.8(2) . . ? C201 N21 C213 109.4(3) . . ? C201 N21 C207 109.1(3) . . ? C213 N21 C207 110.2(3) . . ? C201 N21 K2 110.9(2) . . ? C213 N21 K2 109.9(2) . . ? C207 N21 K2 107.3(2) . . ? C218 N22 C212 109.4(3) . . ? C218 N22 C206 111.0(3) . . ? C212 N22 C206 108.8(3) . . ? C218 N22 K2 108.73(19) . . ? C212 N22 K2 111.2(2) . . ? C206 N22 K2 107.71(19) . . ? C102 O11 C103 111.8(3) . . ? C102 O11 K1 117.1(3) . . ? C103 O11 K1 112.9(2) . . ? C104 O12 C105 110.6(3) . . ? C104 O12 K1 114.1(2) . . ? C105 O12 K1 118.6(2) . . ? C109 O13 C108 110.8(3) . . ? C109 O13 K1 112.3(2) . . ? C108 O13 K1 116.5(2) . . ? C110 O14 C111 109.3(3) . . ? C110 O14 K1 118.6(2) . . ? C111 O14 K1 118.9(2) . . ? C115 O15 C114 110.1(3) . . ? C115 O15 K1 112.4(2) . . ? C114 O15 K1 116.8(2) . . ? C116 O16 C117 111.5(3) . . ? C116 O16 K1 112.3(2) . . ? C117 O16 K1 118.6(2) . . ? C202 O21 C203 111.1(3) . . ? C202 O21 K2 117.6(2) . . ? C203 O21 K2 115.7(2) . . ? C204 O22 C205 111.2(3) . . ? C204 O22 K2 115.3(2) . . ? C205 O22 K2 115.9(2) . . ? C208 O23 C209 110.8(3) . . ? C208 O23 K2 118.8(2) . . ? C209 O23 K2 112.5(2) . . ? C210 O24 C211 110.5(3) . . ? C210 O24 K2 114.4(2) . . ? C211 O24 K2 115.7(2) . . ? C214 O25 C215 110.7(3) . . ? C214 O25 K2 119.8(2) . . ? C215 O25 K2 115.57(19) . . ? C217 O26 C216 110.7(3) . . ? C217 O26 K2 116.92(18) . . ? C216 O26 K2 110.89(19) . . ? N11 C101 C102 113.8(4) . . ? N11 C101 H10A 108.8 . . ? C102 C101 H10A 108.8 . . ? N11 C101 H10B 108.8 . . ? C102 C101 H10B 108.8 . . ? H10A C101 H10B 107.7 . . ? O11 C102 C101 109.7(4) . . ? O11 C102 H10C 109.7 . . ? C101 C102 H10C 109.7 . . ? O11 C102 H10D 109.7 . . ? C101 C102 H10D 109.7 . . ? H10C C102 H10D 108.2 . . ? O11 C103 C104 109.1(3) . . ? O11 C103 H10E 109.9 . . ? C104 C103 H10E 109.9 . . ? O11 C103 H10F 109.9 . . ? C104 C103 H10F 109.9 . . ? H10E C103 H10F 108.3 . . ? O12 C104 C103 108.9(3) . . ? O12 C104 H10G 109.9 . . ? C103 C104 H10G 109.9 . . ? O12 C104 H10H 109.9 . . ? C103 C104 H10H 109.9 . . ? H10G C104 H10H 108.3 . . ? O12 C105 C106 110.0(3) . . ? O12 C105 H10I 109.7 . . ? C106 C105 H10I 109.7 . . ? O12 C105 H10J 109.7 . . ? C106 C105 H10J 109.7 . . ? H10I C105 H10J 108.2 . . ? N12 C106 C105 114.3(4) . . ? N12 C106 H10K 108.7 . . ? C105 C106 H10K 108.7 . . ? N12 C106 H10L 108.7 . . ? C105 C106 H10L 108.7 . . ? H10K C106 H10L 107.6 . . ? N11 C107 C108 114.2(4) . . ? N11 C107 H10M 108.7 . . ? C108 C107 H10M 108.7 . . ? N11 C107 H10N 108.7 . . ? C108 C107 H10N 108.7 . . ? H10M C107 H10N 107.6 . . ? O13 C108 C107 109.9(3) . . ? O13 C108 H10O 109.7 . . ? C107 C108 H10O 109.7 . . ? O13 C108 H10P 109.7 . . ? C107 C108 H10P 109.7 . . ? H10O C108 H10P 108.2 . . ? O13 C109 C110 111.3(3) . . ? O13 C109 H10Q 109.4 . . ? C110 C109 H10Q 109.4 . . ? O13 C109 H10R 109.4 . . ? C110 C109 H10R 109.4 . . ? H10Q C109 H10R 108.0 . . ? O14 C110 C109 111.0(3) . . ? O14 C110 H11A 109.4 . . ? C109 C110 H11A 109.4 . . ? O14 C110 H11B 109.4 . . ? C109 C110 H11B 109.4 . . ? H11A C110 H11B 108.0 . . ? O14 C111 C112 109.8(3) . . ? O14 C111 H11C 109.7 . . ? C112 C111 H11C 109.7 . . ? O14 C111 H11D 109.7 . . ? C112 C111 H11D 109.7 . . ? H11C C111 H11D 108.2 . . ? N12 C112 C111 115.1(4) . . ? N12 C112 H11E 108.5 . . ? C111 C112 H11E 108.5 . . ? N12 C112 H11F 108.5 . . ? C111 C112 H11F 108.5 . . ? H11E C112 H11F 107.5 . . ? N11 C113 C114 113.0(3) . . ? N11 C113 H11G 109.0 . . ? C114 C113 H11G 109.0 . . ? N11 C113 H11H 109.0 . . ? C114 C113 H11H 109.0 . . ? H11G C113 H11H 107.8 . . ? O15 C114 C113 109.6(3) . . ? O15 C114 H11I 109.8 . . ? C113 C114 H11I 109.8 . . ? O15 C114 H11J 109.8 . . ? C113 C114 H11J 109.8 . . ? H11I C114 H11J 108.2 . . ? O15 C115 C116 109.0(3) . . ? O15 C115 H11K 109.9 . . ? C116 C115 H11K 109.9 . . ? O15 C115 H11L 109.9 . . ? C116 C115 H11L 109.9 . . ? H11K C115 H11L 108.3 . . ? O16 C116 C115 109.7(3) . . ? O16 C116 H11M 109.7 . . ? C115 C116 H11M 109.7 . . ? O16 C116 H11N 109.7 . . ? C115 C116 H11N 109.7 . . ? H11M C116 H11N 108.2 . . ? O16 C117 C118 108.3(3) . . ? O16 C117 H11O 110.0 . . ? C118 C117 H11O 110.0 . . ? O16 C117 H11P 110.0 . . ? C118 C117 H11P 110.0 . . ? H11O C117 H11P 108.4 . . ? N12 C118 C117 112.9(3) . . ? N12 C118 H11Q 109.0 . . ? C117 C118 H11Q 109.0 . . ? N12 C118 H11R 109.0 . . ? C117 C118 H11R 109.0 . . ? H11Q C118 H11R 107.8 . . ? N21 C201 C202 114.7(3) . . ? N21 C201 H20A 108.6 . . ? C202 C201 H20A 108.6 . . ? N21 C201 H20B 108.6 . . ? C202 C201 H20B 108.6 . . ? H20A C201 H20B 107.6 . . ? O21 C202 C201 108.7(3) . . ? O21 C202 H20C 109.9 . . ? C201 C202 H20C 109.9 . . ? O21 C202 H20D 109.9 . . ? C201 C202 H20D 109.9 . . ? H20C C202 H20D 108.3 . . ? O21 C203 C204 109.0(3) . . ? O21 C203 H20E 109.9 . . ? C204 C203 H20E 109.9 . . ? O21 C203 H20F 109.9 . . ? C204 C203 H20F 109.9 . . ? H20E C203 H20F 108.3 . . ? O22 C204 C203 109.7(3) . . ? O22 C204 H20G 109.7 . . ? C203 C204 H20G 109.7 . . ? O22 C204 H20H 109.7 . . ? C203 C204 H20H 109.7 . . ? H20G C204 H20H 108.2 . . ? O22 C205 C206 110.5(3) . . ? O22 C205 H20I 109.5 . . ? C206 C205 H20I 109.5 . . ? O22 C205 H20J 109.5 . . ? C206 C205 H20J 109.5 . . ? H20I C205 H20J 108.1 . . ? N22 C206 C205 114.4(3) . . ? N22 C206 H20K 108.7 . . ? C205 C206 H20K 108.7 . . ? N22 C206 H20L 108.7 . . ? C205 C206 H20L 108.7 . . ? H20K C206 H20L 107.6 . . ? N21 C207 C208 114.0(3) . . ? N21 C207 H20M 108.7 . . ? C208 C207 H20M 108.7 . . ? N21 C207 H20N 108.7 . . ? C208 C207 H20N 108.7 . . ? H20M C207 H20N 107.6 . . ? O23 C208 C207 109.8(3) . . ? O23 C208 H20O 109.7 . . ? C207 C208 H20O 109.7 . . ? O23 C208 H20P 109.7 . . ? C207 C208 H20P 109.7 . . ? H20O C208 H20P 108.2 . . ? O23 C209 C210 108.8(3) . . ? O23 C209 H20Q 109.9 . . ? C210 C209 H20Q 109.9 . . ? O23 C209 H20R 109.9 . . ? C210 C209 H20R 109.9 . . ? H20Q C209 H20R 108.3 . . ? O24 C210 C209 109.3(3) . . ? O24 C210 H21A 109.8 . . ? C209 C210 H21A 109.8 . . ? O24 C210 H21B 109.8 . . ? C209 C210 H21B 109.8 . . ? H21A C210 H21B 108.3 . . ? O24 C211 C212 109.5(3) . . ? O24 C211 H21C 109.8 . . ? C212 C211 H21C 109.8 . . ? O24 C211 H21D 109.8 . . ? C212 C211 H21D 109.8 . . ? H21C C211 H21D 108.2 . . ? N22 C212 C211 113.7(3) . . ? N22 C212 H21E 108.8 . . ? C211 C212 H21E 108.8 . . ? N22 C212 H21F 108.8 . . ? C211 C212 H21F 108.8 . . ? H21E C212 H21F 107.7 . . ? N21 C213 C214 113.2(3) . . ? N21 C213 H21G 108.9 . . ? C214 C213 H21G 108.9 . . ? N21 C213 H21H 108.9 . . ? C214 C213 H21H 108.9 . . ? H21G C213 H21H 107.8 . . ? O25 C214 C213 108.1(3) . . ? O25 C214 H21I 110.1 . . ? C213 C214 H21I 110.1 . . ? O25 C214 H21J 110.1 . . ? C213 C214 H21J 110.1 . . ? H21I C214 H21J 108.4 . . ? O25 C215 C216 108.7(3) . . ? O25 C215 H21K 110.0 . . ? C216 C215 H21K 110.0 . . ? O25 C215 H21L 110.0 . . ? C216 C215 H21L 110.0 . . ? H21K C215 H21L 108.3 . . ? O26 C216 C215 109.7(3) . . ? O26 C216 H21M 109.7 . . ? C215 C216 H21M 109.7 . . ? O26 C216 H21N 109.7 . . ? C215 C216 H21N 109.7 . . ? H21M C216 H21N 108.2 . . ? O26 C217 C218 109.9(3) . . ? O26 C217 H21O 109.7 . . ? C218 C217 H21O 109.7 . . ? O26 C217 H21P 109.7 . . ? C218 C217 H21P 109.7 . . ? H21O C217 H21P 108.2 . . ? N22 C218 C217 113.8(3) . . ? N22 C218 H21Q 108.8 . . ? C217 C218 H21Q 108.8 . . ? N22 C218 H21R 108.8 . . ? C217 C218 H21R 108.8 . . ? H21Q C218 H21R 107.7 . . ? C5Q N1Q C1Q 122.0(6) . . ? C2Q C1Q N1Q 117.5(5) . . ? C2Q C1Q H1Q 121.2 . . ? N1Q C1Q H1Q 121.2 . . ? C1Q C2Q C3Q 123.5(5) . . ? C1Q C2Q H2Q 118.2 . . ? C3Q C2Q H2Q 118.2 . . ? C2Q C3Q C4Q 117.4(5) . . ? C2Q C3Q H3Q 121.3 . . ? C4Q C3Q H3Q 121.3 . . ? C5Q C4Q C3Q 121.1(6) . . ? C5Q C4Q H4Q 119.5 . . ? C3Q C4Q H4Q 119.5 . . ? C4Q C5Q N1Q 118.4(5) . . ? C4Q C5Q H5Q 120.8 . . ? N1Q C5Q H5Q 120.8 . . ? C5S N1S C1S 118.0(8) . . ? C2S C1S N1S 115.9(7) . . ? C2S C1S H1S 122.0 . . ? N1S C1S H1S 122.0 . . ? C3S C2S C1S 119.3(7) . . ? C3S C2S H2S 120.4 . . ? C1S C2S H2S 120.4 . . ? C4S C3S C2S 123.2(8) . . ? C4S C3S H3S 118.4 . . ? C2S C3S H3S 118.4 . . ? C3S C4S C5S 122.4(8) . . ? C3S C4S H4S 118.8 . . ? C5S C4S H4S 118.8 . . ? N1S C5S C4S 120.9(8) . . ? N1S C5S H5S 119.6 . . ? C4S C5S H5S 119.6 . . ? C5P N1P C1P 119.2(6) . . ? C2P C1P N1P 118.3(6) . . ? C2P C1P H1P 120.8 . . ? N1P C1P H1P 120.8 . . ? C1P C2P C3P 121.3(6) . . ? C1P C2P H2P 119.4 . . ? C3P C2P H2P 119.4 . . ? C4P C3P C2P 120.7(6) . . ? C4P C3P H3P 119.7 . . ? C2P C3P H3P 119.7 . . ? C3P C4P C5P 119.1(6) . . ? C3P C4P H4P 120.5 . . ? C5P C4P H4P 120.5 . . ? N1P C5P C4P 121.3(6) . . ? N1P C5P H5P 119.3 . . ? C4P C5P H5P 119.3 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.410 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.055 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 736078' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K(2,2,2-crypt)]4[Cd(P7)2]*6py ; _contact_author_fax '+44 1865 272690' _chemical_name_common (K(2,2,2-crypt))4(Cd(P7)2)*6py _chemical_melting_point ? _chemical_formula_moiety '6(C18 H36 K N2 O6), 6(C5 H5 N), Cd P14' _chemical_formula_sum 'C102 H174 Cd K4 N14 O24 P14' _chemical_formula_weight 2682.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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 Orthorhombic _symmetry_space_group_name_H-M Fdd2 _symmetry_space_group_name_Hall 'F 2 -2d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 23.5977(2) _cell_length_b 75.1887(8) _cell_length_c 15.1082(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 26806.2(4) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 47010 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 25.028 _exptl_crystal_description plates _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11280 _exptl_absorpt_coefficient_mu 0.521 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8346 _exptl_absorpt_correction_T_max 0.9744 _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _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 10425 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0600 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -89 _diffrn_reflns_limit_k_max 89 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10425 _reflns_number_gt 8533 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; KappaCCD software "Collect" (Nonius, 2000) ; _computing_cell_refinement ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_data_reduction ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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^)+(0.0435P)^2^+162.0573P] 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 0.56(3) _refine_ls_number_reflns 10425 _refine_ls_number_parameters 726 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1161 _refine_ls_wR_factor_gt 0.1086 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 0.5000 0.0000 0.51889(4) 0.03866(16) Uani 1 2 d S . . P1 P 0.56580(7) 0.03641(2) 0.46252(10) 0.0393(4) Uani 1 1 d . . . P2 P 0.47542(7) 0.03058(2) 0.43698(10) 0.0422(4) Uani 1 1 d . . . P3 P 0.57345(6) 0.02260(2) 0.59058(10) 0.0350(3) Uani 1 1 d . . . P4 P 0.56407(7) 0.06411(2) 0.50063(11) 0.0442(4) Uani 1 1 d . . . P5 P 0.43965(6) 0.04090(2) 0.55858(11) 0.0383(4) Uani 1 1 d . . . P6 P 0.50534(6) 0.035616(19) 0.66132(9) 0.0330(3) Uani 1 1 d . . . P7 P 0.49889(6) 0.062881(19) 0.59861(11) 0.0388(4) Uani 1 1 d . . . K1 K 0.48805(5) 0.156023(15) 0.58755(8) 0.0308(3) Uani 1 1 d . . . K2 K 0.65136(5) 0.002495(17) 1.03512(7) 0.0372(3) Uani 1 1 d . . . N11 N 0.5436(2) 0.12365(6) 0.6671(3) 0.0432(12) Uani 1 1 d . . . N12 N 0.43223(17) 0.18798(6) 0.5095(3) 0.0346(11) Uani 1 1 d . . . N21 N 0.7025(2) -0.02588(8) 0.9201(3) 0.0553(15) Uani 1 1 d . . . N22 N 0.5968(2) 0.03076(7) 1.1482(3) 0.0468(13) Uani 1 1 d . . . O11 O 0.52519(17) 0.12866(5) 0.4740(3) 0.0458(10) Uani 1 1 d . . . O12 O 0.49390(16) 0.16181(6) 0.4013(3) 0.0464(10) Uani 1 1 d . . . O13 O 0.58862(16) 0.15963(5) 0.6843(3) 0.0419(10) Uani 1 1 d . . . O14 O 0.52519(14) 0.19032(5) 0.6375(2) 0.0352(9) Uani 1 1 d . . . O15 O 0.42987(16) 0.13501(5) 0.7181(3) 0.0437(10) Uani 1 1 d . . . O16 O 0.37119(15) 0.16130(5) 0.6205(3) 0.0408(10) Uani 1 1 d . . . O21 O 0.6058(2) -0.00352(6) 0.8674(3) 0.0562(12) Uani 1 1 d . . . O22 O 0.57157(19) 0.02796(7) 0.9607(3) 0.0641(13) Uani 1 1 d . . . O23 O 0.76608(16) 0.00515(6) 0.9904(3) 0.0491(11) Uani 1 1 d . . . O24 O 0.72083(17) 0.02725(6) 1.1263(3) 0.0523(11) Uani 1 1 d . . . O25 O 0.65881(18) -0.03367(6) 1.0954(3) 0.0492(10) Uani 1 1 d . . . O26 O 0.58970(15) -0.00795(6) 1.1854(2) 0.0423(10) Uani 1 1 d . . . C101 C 0.5446(3) 0.10955(8) 0.5972(4) 0.0509(16) Uani 1 1 d . . . H10A H 0.5060 0.1045 0.5913 0.061 Uiso 1 1 calc R . . H10B H 0.5700 0.0998 0.6170 0.061 Uiso 1 1 calc R . . C102 C 0.5640(3) 0.11588(8) 0.5083(5) 0.0581(18) Uani 1 1 d . . . H10C H 0.6021 0.1213 0.5136 0.070 Uiso 1 1 calc R . . H10D H 0.5667 0.1057 0.4672 0.070 Uiso 1 1 calc R . . C103 C 0.5423(3) 0.13443(11) 0.3887(5) 0.069(2) Uani 1 1 d . . . H10E H 0.5484 0.1240 0.3498 0.083 Uiso 1 1 calc R . . H10F H 0.5785 0.1410 0.3931 0.083 Uiso 1 1 calc R . . C104 C 0.4981(3) 0.14605(10) 0.3506(4) 0.0623(19) Uani 1 1 d . . . H10G H 0.5078 0.1490 0.2886 0.075 Uiso 1 1 calc R . . H10H H 0.4612 0.1398 0.3506 0.075 Uiso 1 1 calc R . . C105 C 0.4512(3) 0.17326(9) 0.3649(4) 0.0527(17) Uani 1 1 d . . . H10I H 0.4139 0.1673 0.3672 0.063 Uiso 1 1 calc R . . H10J H 0.4601 0.1759 0.3022 0.063 Uiso 1 1 calc R . . C106 C 0.4489(3) 0.19021(8) 0.4167(4) 0.0426(15) Uani 1 1 d . . . H10K H 0.4868 0.1959 0.4147 0.051 Uiso 1 1 calc R . . H10L H 0.4218 0.1984 0.3877 0.051 Uiso 1 1 calc R . . C107 C 0.6016(3) 0.12828(8) 0.6932(5) 0.0540(18) Uani 1 1 d . . . H10M H 0.6255 0.1288 0.6394 0.065 Uiso 1 1 calc R . . H10N H 0.6168 0.1187 0.7313 0.065 Uiso 1 1 calc R . . C108 C 0.6067(3) 0.14556(8) 0.7416(4) 0.0478(16) Uani 1 1 d . . . H10O H 0.5828 0.1453 0.7954 0.057 Uiso 1 1 calc R . . H10P H 0.6465 0.1475 0.7598 0.057 Uiso 1 1 calc R . . C109 C 0.5977(2) 0.17655(7) 0.7230(4) 0.0416(15) Uani 1 1 d . . . H10Q H 0.6377 0.1776 0.7423 0.050 Uiso 1 1 calc R . . H10R H 0.5731 0.1780 0.7754 0.050 Uiso 1 1 calc R . . C110 C 0.5845(2) 0.19055(7) 0.6561(4) 0.0416(15) Uani 1 1 d . . . H11A H 0.5956 0.2024 0.6792 0.050 Uiso 1 1 calc R . . H11B H 0.6062 0.1883 0.6011 0.050 Uiso 1 1 calc R . . C111 C 0.5103(2) 0.20460(7) 0.5808(4) 0.0375(13) Uani 1 1 d . . . H11C H 0.5325 0.2039 0.5254 0.045 Uiso 1 1 calc R . . H11D H 0.5191 0.2161 0.6100 0.045 Uiso 1 1 calc R . . C112 C 0.4481(2) 0.20362(7) 0.5602(4) 0.0417(15) Uani 1 1 d . . . H11E H 0.4266 0.2037 0.6164 0.050 Uiso 1 1 calc R . . H11F H 0.4371 0.2144 0.5265 0.050 Uiso 1 1 calc R . . C113 C 0.5118(3) 0.11723(9) 0.7443(5) 0.0525(17) Uani 1 1 d . . . H11G H 0.5210 0.1248 0.7959 0.063 Uiso 1 1 calc R . . H11H H 0.5242 0.1050 0.7582 0.063 Uiso 1 1 calc R . . C114 C 0.4490(3) 0.11725(8) 0.7311(5) 0.0534(17) Uani 1 1 d . . . H11I H 0.4392 0.1099 0.6789 0.064 Uiso 1 1 calc R . . H11J H 0.4301 0.1120 0.7836 0.064 Uiso 1 1 calc R . . C115 C 0.3696(2) 0.13624(9) 0.7156(5) 0.0520(17) Uani 1 1 d . . . H11K H 0.3534 0.1314 0.7711 0.062 Uiso 1 1 calc R . . H11L H 0.3547 0.1291 0.6656 0.062 Uiso 1 1 calc R . . C116 C 0.3527(3) 0.15495(9) 0.7049(5) 0.0558(18) Uani 1 1 d . . . H11M H 0.3110 0.1560 0.7094 0.067 Uiso 1 1 calc R . . H11N H 0.3699 0.1622 0.7525 0.067 Uiso 1 1 calc R . . C117 C 0.3500(2) 0.17878(8) 0.6022(5) 0.0494(17) Uani 1 1 d . . . H11O H 0.3629 0.1871 0.6489 0.059 Uiso 1 1 calc R . . H11P H 0.3080 0.1786 0.6029 0.059 Uiso 1 1 calc R . . C118 C 0.3700(2) 0.18509(8) 0.5150(5) 0.0489(17) Uani 1 1 d . . . H11Q H 0.3506 0.1964 0.5008 0.059 Uiso 1 1 calc R . . H11R H 0.3590 0.1763 0.4695 0.059 Uiso 1 1 calc R . . C201 C 0.6627(4) -0.02923(10) 0.8458(5) 0.073(2) Uani 1 1 d . . . H20A H 0.6831 -0.0361 0.8000 0.088 Uiso 1 1 calc R . . H20B H 0.6315 -0.0368 0.8681 0.088 Uiso 1 1 calc R . . C202 C 0.6375(3) -0.01337(11) 0.8030(4) 0.069(2) Uani 1 1 d . . . H20C H 0.6678 -0.0058 0.7780 0.082 Uiso 1 1 calc R . . H20D H 0.6122 -0.0171 0.7541 0.082 Uiso 1 1 calc R . . C203 C 0.5755(3) 0.01080(10) 0.8258(4) 0.0546(19) Uani 1 1 d . . . H20E H 0.5506 0.0059 0.7789 0.066 Uiso 1 1 calc R . . H20F H 0.6029 0.0190 0.7976 0.066 Uiso 1 1 calc R . . C204 C 0.5411(4) 0.02064(11) 0.8897(5) 0.079(2) Uani 1 1 d . . . H20G H 0.5214 0.0304 0.8581 0.094 Uiso 1 1 calc R . . H20H H 0.5118 0.0126 0.9136 0.094 Uiso 1 1 calc R . . C205 C 0.5348(3) 0.03647(11) 1.0216(5) 0.075(2) Uani 1 1 d . . . H20I H 0.5075 0.0278 1.0459 0.090 Uiso 1 1 calc R . . H20J H 0.5133 0.0460 0.9914 0.090 Uiso 1 1 calc R . . C206 C 0.5690(4) 0.04411(11) 1.0939(5) 0.075(2) Uani 1 1 d . . . H20K H 0.5981 0.0520 1.0681 0.090 Uiso 1 1 calc R . . H20L H 0.5441 0.0514 1.1320 0.090 Uiso 1 1 calc R . . C207 C 0.7570(3) -0.01848(12) 0.8862(5) 0.076(2) Uani 1 1 d . . . H20M H 0.7484 -0.0094 0.8404 0.091 Uiso 1 1 calc R . . H20N H 0.7785 -0.0282 0.8572 0.091 Uiso 1 1 calc R . . C208 C 0.7939(3) -0.01012(11) 0.9558(5) 0.069(2) Uani 1 1 d . . . H20O H 0.8011 -0.0188 1.0039 0.082 Uiso 1 1 calc R . . H20P H 0.8307 -0.0067 0.9296 0.082 Uiso 1 1 calc R . . C209 C 0.7993(3) 0.01319(10) 1.0591(5) 0.0553(18) Uani 1 1 d . . . H20Q H 0.8385 0.0152 1.0378 0.066 Uiso 1 1 calc R . . H20R H 0.8010 0.0052 1.1110 0.066 Uiso 1 1 calc R . . C210 C 0.7737(3) 0.03015(10) 1.0845(5) 0.0569(18) Uani 1 1 d . . . H21A H 0.7993 0.0366 1.1253 0.068 Uiso 1 1 calc R . . H21B H 0.7682 0.0376 1.0311 0.068 Uiso 1 1 calc R . . C211 C 0.6947(3) 0.04351(10) 1.1512(6) 0.070(2) Uani 1 1 d . . . H21C H 0.6864 0.0506 1.0977 0.084 Uiso 1 1 calc R . . H21D H 0.7208 0.0504 1.1892 0.084 Uiso 1 1 calc R . . C212 C 0.6403(3) 0.03980(10) 1.2009(5) 0.066(2) Uani 1 1 d . . . H21E H 0.6492 0.0324 1.2532 0.079 Uiso 1 1 calc R . . H21F H 0.6247 0.0512 1.2226 0.079 Uiso 1 1 calc R . . C213 C 0.7125(4) -0.04216(10) 0.9699(5) 0.069(2) Uani 1 1 d . . . H21G H 0.7474 -0.0407 1.0056 0.083 Uiso 1 1 calc R . . H21H H 0.7191 -0.0520 0.9277 0.083 Uiso 1 1 calc R . . C214 C 0.6653(4) -0.04705(9) 1.0293(5) 0.068(2) Uani 1 1 d . . . H21I H 0.6299 -0.0482 0.9947 0.081 Uiso 1 1 calc R . . H21J H 0.6734 -0.0587 1.0576 0.081 Uiso 1 1 calc R . . C215 C 0.6158(3) -0.03784(9) 1.1580(5) 0.0588(19) Uani 1 1 d . . . H21K H 0.6250 -0.0492 1.1876 0.071 Uiso 1 1 calc R . . H21L H 0.5791 -0.0393 1.1271 0.071 Uiso 1 1 calc R . . C216 C 0.6111(3) -0.02357(9) 1.2249(4) 0.0525(18) Uani 1 1 d . . . H21M H 0.5855 -0.0274 1.2731 0.063 Uiso 1 1 calc R . . H21N H 0.6489 -0.0212 1.2508 0.063 Uiso 1 1 calc R . . C217 C 0.5799(3) 0.00553(9) 1.2510(4) 0.0491(17) Uani 1 1 d . . . H21O H 0.6160 0.0085 1.2809 0.059 Uiso 1 1 calc R . . H21P H 0.5531 0.0010 1.2962 0.059 Uiso 1 1 calc R . . C218 C 0.5559(3) 0.02180(9) 1.2076(4) 0.0468(16) Uani 1 1 d . . . H21Q H 0.5220 0.0184 1.1731 0.056 Uiso 1 1 calc R . . H21R H 0.5438 0.0303 1.2541 0.056 Uiso 1 1 calc R . . N1 N 0.4303(2) 0.07093(7) 0.8239(4) 0.101(3) Uani 1 1 d G . . C1 C 0.4300(3) 0.07916(9) 0.9062(4) 0.081(3) Uani 1 1 d G . . H1 H 0.4615 0.0778 0.9449 0.097 Uiso 1 1 calc R . . C2 C 0.3837(4) 0.08934(8) 0.9320(5) 0.110(4) Uani 1 1 d G . . H2 H 0.3835 0.0950 0.9883 0.132 Uiso 1 1 calc R . . C3 C 0.3377(3) 0.09129(8) 0.8755(7) 0.102(4) Uani 1 1 d G . . H3 H 0.3060 0.0982 0.8931 0.123 Uiso 1 1 calc R . . C4 C 0.3380(2) 0.08306(10) 0.7931(6) 0.138(6) Uani 1 1 d G . . H4 H 0.3065 0.0844 0.7544 0.166 Uiso 1 1 calc R . . C5 C 0.3843(3) 0.07288(8) 0.7673(4) 0.103(3) Uani 1 1 d G . . H5 H 0.3845 0.0673 0.7110 0.123 Uiso 1 1 calc R . . C3S C 0.6985(4) 0.10141(15) 0.1939(5) 0.168(7) Uani 1 1 d G . . H3S H 0.7074 0.1033 0.1333 0.201 Uiso 1 1 calc R . . C2S C 0.7015(3) 0.11483(11) 0.2508(7) 0.115(4) Uani 1 1 d G . . H2S H 0.7125 0.1263 0.2309 0.138 Uiso 1 1 calc R . . C1S C 0.6891(3) 0.11222(10) 0.3354(7) 0.153(5) Uani 1 1 d G . . H1S H 0.6912 0.1218 0.3762 0.184 Uiso 1 1 calc R . . N1S N 0.6737(3) 0.09619(12) 0.3632(4) 0.116(3) Uani 1 1 d G . . C5S C 0.6707(4) 0.08277(10) 0.3064(5) 0.162(6) Uani 1 1 d G . . H5S H 0.6597 0.0713 0.3263 0.194 Uiso 1 1 calc R . . C4S C 0.6832(4) 0.08538(13) 0.2217(5) 0.137(5) Uani 1 1 d G . . H4S H 0.6810 0.0758 0.1810 0.165 Uiso 1 1 calc R . . N1R N 0.6724(3) 0.16163(17) 0.4929(9) 0.164(8) Uani 0.707(9) 1 d PG A 1 C1R C 0.7143(4) 0.16766(14) 0.5502(6) 0.080(5) Uani 0.707(9) 1 d PG A 1 H1R H 0.7043 0.1720 0.6072 0.096 Uiso 0.707(9) 1 calc PR A 1 C2R C 0.7707(4) 0.16734(12) 0.5242(5) 0.078(4) Uani 0.707(9) 1 d PG A 1 H2R H 0.7994 0.1715 0.5633 0.093 Uiso 0.707(9) 1 calc PR A 1 C3R C 0.7853(3) 0.16100(13) 0.4408(6) 0.094(5) Uani 0.707(9) 1 d PG A 1 H3R H 0.8239 0.1608 0.4230 0.113 Uiso 0.707(9) 1 calc PR A 1 C4R C 0.7434(4) 0.15497(18) 0.3835(6) 0.202(14) Uani 0.707(9) 1 d PG A 1 H4R H 0.7534 0.1506 0.3265 0.243 Uiso 0.707(9) 1 calc PR A 1 C5R C 0.6870(4) 0.1553(2) 0.4096(9) 0.26(2) Uani 0.707(9) 1 d PG A 1 H5R H 0.6583 0.1512 0.3704 0.310 Uiso 0.707(9) 1 calc PR A 1 N1Q N 0.7123(8) 0.1432(2) 0.4788(14) 0.072(7) Uani 0.293(9) 1 d PGU A 2 C1Q C 0.7208(9) 0.1507(3) 0.5618(12) 0.093(10) Uani 0.293(9) 1 d PGU A 2 H1Q H 0.7227 0.1433 0.6128 0.111 Uiso 0.293(9) 1 calc PR A 2 C2Q C 0.7265(10) 0.1690(3) 0.5702(12) 0.081(13) Uani 0.293(9) 1 d PGU A 2 H2Q H 0.7323 0.1742 0.6269 0.097 Uiso 0.293(9) 1 calc PR A 2 C3Q C 0.7237(9) 0.1798(2) 0.4956(17) 0.085(9) Uani 0.293(9) 1 d PGU A 2 H3Q H 0.7276 0.1923 0.5014 0.101 Uiso 0.293(9) 1 calc PR A 2 C4Q C 0.7152(10) 0.1723(3) 0.4127(13) 0.104(11) Uani 0.293(9) 1 d PGU A 2 H4Q H 0.7133 0.1797 0.3617 0.124 Uiso 0.293(9) 1 calc PR A 2 C5Q C 0.7095(10) 0.1540(3) 0.4042(11) 0.105(13) Uani 0.293(9) 1 d PGU A 2 H5Q H 0.7037 0.1488 0.3475 0.126 Uiso 0.293(9) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0543(4) 0.0231(3) 0.0385(3) 0.000 0.000 -0.0014(3) P1 0.0486(9) 0.0388(9) 0.0304(8) 0.0027(7) -0.0007(7) -0.0004(7) P2 0.0559(10) 0.0350(9) 0.0356(9) 0.0020(7) -0.0229(8) -0.0066(7) P3 0.0342(8) 0.0411(9) 0.0296(7) 0.0010(7) -0.0059(7) 0.0080(6) P4 0.0534(10) 0.0332(9) 0.0459(10) 0.0040(7) -0.0067(8) -0.0123(7) P5 0.0310(8) 0.0326(8) 0.0512(10) 0.0040(7) -0.0119(7) 0.0027(6) P6 0.0343(8) 0.0364(8) 0.0283(7) -0.0001(6) -0.0043(6) 0.0034(6) P7 0.0435(9) 0.0276(8) 0.0454(9) -0.0040(7) -0.0078(7) -0.0025(7) K1 0.0323(6) 0.0272(6) 0.0330(6) -0.0011(5) -0.0050(5) 0.0000(5) K2 0.0331(6) 0.0545(8) 0.0240(7) 0.0032(6) -0.0016(5) -0.0014(6) N11 0.044(3) 0.033(3) 0.053(3) 0.004(2) -0.009(3) 0.001(2) N12 0.028(2) 0.035(3) 0.040(3) 0.009(2) -0.007(2) 0.0009(19) N21 0.074(4) 0.063(4) 0.029(3) -0.003(3) 0.001(3) 0.005(3) N22 0.056(3) 0.056(3) 0.028(3) 0.011(3) 0.009(3) 0.016(3) O11 0.052(2) 0.042(2) 0.044(2) -0.0093(19) -0.001(2) 0.011(2) O12 0.050(2) 0.053(3) 0.036(2) 0.002(2) -0.007(2) 0.010(2) O13 0.045(2) 0.033(2) 0.047(2) -0.0008(19) -0.0204(19) 0.0026(18) O14 0.028(2) 0.032(2) 0.046(2) 0.0017(18) -0.0108(17) -0.0014(16) O15 0.045(2) 0.040(2) 0.046(2) 0.011(2) -0.002(2) -0.0042(18) O16 0.033(2) 0.039(2) 0.051(3) 0.0072(19) -0.0012(18) 0.0011(17) O21 0.083(3) 0.056(3) 0.030(2) 0.008(2) -0.014(2) -0.016(2) O22 0.056(3) 0.089(4) 0.047(3) 0.015(3) -0.009(2) 0.001(3) O23 0.035(2) 0.068(3) 0.044(3) 0.003(2) 0.0025(19) 0.005(2) O24 0.042(3) 0.060(3) 0.054(3) 0.000(2) 0.011(2) -0.014(2) O25 0.058(3) 0.049(3) 0.040(2) 0.006(2) 0.003(2) 0.002(2) O26 0.035(2) 0.062(3) 0.030(2) 0.014(2) 0.0048(18) 0.0087(19) C101 0.072(4) 0.021(3) 0.060(4) -0.004(3) -0.008(4) 0.008(3) C102 0.066(4) 0.037(4) 0.071(5) -0.017(4) -0.007(4) 0.012(3) C103 0.082(5) 0.081(6) 0.044(4) -0.009(4) 0.007(4) 0.023(4) C104 0.069(5) 0.080(5) 0.038(4) -0.005(4) -0.003(4) 0.018(4) C105 0.056(4) 0.058(5) 0.044(4) 0.013(3) -0.015(3) -0.008(3) C106 0.044(3) 0.042(4) 0.042(4) 0.011(3) -0.017(3) -0.001(3) C107 0.045(4) 0.047(4) 0.070(5) 0.011(3) -0.017(3) 0.013(3) C108 0.052(4) 0.037(4) 0.055(4) 0.000(3) -0.024(3) 0.002(3) C109 0.044(3) 0.028(3) 0.053(4) -0.009(3) -0.023(3) -0.004(3) C110 0.034(3) 0.032(3) 0.059(4) -0.008(3) -0.014(3) -0.003(2) C111 0.039(3) 0.022(3) 0.051(4) 0.000(3) -0.007(3) -0.001(2) C112 0.038(3) 0.032(3) 0.055(4) 0.006(3) -0.006(3) 0.005(3) C113 0.056(4) 0.045(4) 0.056(4) 0.014(3) -0.013(3) 0.010(3) C114 0.059(4) 0.042(4) 0.059(4) 0.026(3) -0.007(3) -0.005(3) C115 0.041(4) 0.066(5) 0.049(4) 0.020(3) 0.009(3) 0.000(3) C116 0.048(4) 0.064(5) 0.056(4) 0.005(4) 0.017(3) 0.001(3) C117 0.030(3) 0.041(4) 0.077(5) 0.002(3) 0.000(3) 0.005(3) C118 0.030(3) 0.042(4) 0.075(5) 0.014(3) -0.023(3) 0.004(3) C201 0.113(6) 0.067(5) 0.040(4) -0.014(4) -0.003(4) 0.005(5) C202 0.092(6) 0.083(6) 0.031(4) -0.004(4) -0.003(4) -0.013(5) C203 0.066(4) 0.069(5) 0.029(3) 0.017(3) -0.021(3) -0.021(4) C204 0.095(6) 0.084(6) 0.057(5) 0.007(4) -0.023(5) -0.012(5) C205 0.062(5) 0.110(7) 0.052(4) 0.027(5) 0.012(4) 0.043(4) C206 0.090(6) 0.081(6) 0.054(5) 0.016(4) 0.022(5) 0.030(5) C207 0.077(5) 0.096(6) 0.053(5) -0.011(4) 0.026(4) 0.015(5) C208 0.048(4) 0.098(6) 0.060(5) -0.010(5) 0.018(4) 0.011(4) C209 0.033(3) 0.074(5) 0.059(4) 0.007(4) -0.006(3) -0.006(3) C210 0.053(4) 0.069(5) 0.049(4) 0.006(4) -0.001(3) -0.021(4) C211 0.073(5) 0.052(5) 0.085(6) -0.010(4) 0.022(4) -0.014(4) C212 0.070(5) 0.069(5) 0.058(5) -0.018(4) 0.013(4) -0.007(4) C213 0.102(6) 0.062(5) 0.043(4) -0.011(4) 0.011(4) 0.030(4) C214 0.107(6) 0.045(4) 0.050(4) 0.002(4) -0.008(4) 0.003(4) C215 0.053(4) 0.060(5) 0.063(5) 0.031(4) -0.005(4) -0.004(3) C216 0.053(4) 0.062(5) 0.042(4) 0.028(4) 0.016(3) 0.019(3) C217 0.043(4) 0.075(5) 0.029(3) 0.009(3) 0.010(3) 0.006(3) C218 0.045(4) 0.064(4) 0.031(3) 0.011(3) 0.006(3) 0.016(3) N1 0.084(5) 0.087(6) 0.133(7) 0.025(5) -0.013(5) -0.019(4) C1 0.100(7) 0.081(6) 0.061(5) -0.003(5) 0.017(5) -0.030(5) C2 0.148(10) 0.083(7) 0.099(8) 0.003(6) 0.074(9) -0.021(7) C3 0.093(8) 0.086(7) 0.128(10) 0.012(7) 0.068(7) 0.013(6) C4 0.067(7) 0.108(9) 0.241(18) 0.081(11) 0.037(8) -0.003(6) C5 0.084(6) 0.078(6) 0.146(9) 0.032(7) 0.001(7) -0.027(5) C3S 0.202(14) 0.212(17) 0.089(9) 0.041(11) 0.005(9) -0.098(14) C2S 0.123(9) 0.082(8) 0.141(11) 0.041(8) 0.040(8) -0.001(6) C1S 0.230(15) 0.067(8) 0.163(13) -0.002(8) 0.055(12) -0.019(8) N1S 0.119(7) 0.133(8) 0.097(7) -0.005(6) -0.016(5) 0.032(6) C5S 0.306(19) 0.102(9) 0.077(8) -0.005(7) -0.007(10) -0.086(10) C4S 0.200(13) 0.148(11) 0.064(7) -0.015(7) 0.000(7) -0.087(10) N1R 0.128(12) 0.145(14) 0.218(19) -0.082(13) 0.056(13) -0.044(10) C1R 0.063(10) 0.110(14) 0.066(9) -0.011(9) 0.003(7) 0.019(8) C2R 0.072(8) 0.094(9) 0.067(8) 0.011(7) 0.000(7) 0.002(6) C3R 0.090(9) 0.087(9) 0.105(11) -0.008(8) 0.047(8) -0.023(7) C4R 0.061(9) 0.31(3) 0.24(2) -0.24(2) 0.049(11) -0.068(12) C5R 0.071(14) 0.43(5) 0.28(3) -0.29(3) 0.037(15) -0.027(17) N1Q 0.083(14) 0.058(12) 0.074(13) -0.018(10) 0.003(11) -0.030(10) C1Q 0.076(15) 0.090(17) 0.111(18) 0.010(15) -0.003(14) -0.002(14) C2Q 0.036(15) 0.09(2) 0.12(2) 0.006(16) 0.001(14) 0.004(13) C3Q 0.073(15) 0.087(16) 0.094(17) 0.010(14) -0.011(13) -0.003(13) C4Q 0.109(18) 0.117(18) 0.085(16) 0.040(15) -0.037(14) -0.003(15) C5Q 0.067(19) 0.13(2) 0.12(2) -0.067(17) -0.018(15) 0.002(15) _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 P3 2.6579(15) . ? Cd1 P3 2.6579(15) 2_655 ? Cd1 P2 2.6751(15) . ? Cd1 P2 2.6751(15) 2_655 ? P1 P4 2.161(2) . ? P1 P3 2.203(2) . ? P1 P2 2.211(2) . ? P2 P5 2.165(2) . ? P3 P6 2.164(2) . ? P4 P7 2.137(2) . ? P5 P6 2.229(2) . ? P5 P7 2.247(2) . ? P6 P7 2.263(2) . ? K1 O13 2.801(4) . ? K1 O11 2.819(4) . ? K1 O14 2.826(4) . ? K1 O16 2.830(4) . ? K1 O12 2.851(4) . ? K1 O15 2.876(4) . ? K1 N12 2.983(4) . ? K1 N11 3.015(5) . ? K2 O21 2.789(4) . ? K2 O23 2.797(4) . ? K2 O26 2.809(4) . ? K2 O24 2.837(4) . ? K2 O25 2.873(4) . ? K2 O22 2.911(5) . ? K2 N21 3.004(5) . ? K2 N22 3.016(5) . ? N11 C107 1.466(7) . ? N11 C113 1.469(8) . ? N11 C101 1.497(8) . ? N12 C112 1.452(7) . ? N12 C106 1.466(7) . ? N12 C118 1.486(7) . ? N21 C213 1.456(9) . ? N21 C201 1.485(9) . ? N21 C207 1.491(9) . ? N22 C206 1.454(8) . ? N22 C212 1.466(8) . ? N22 C218 1.480(7) . ? O11 C103 1.418(8) . ? O11 C102 1.425(7) . ? O12 C104 1.414(8) . ? O12 C105 1.434(7) . ? O13 C109 1.417(6) . ? O13 C108 1.431(7) . ? O14 C111 1.418(6) . ? O14 C110 1.428(6) . ? O15 C114 1.423(7) . ? O15 C115 1.427(7) . ? O16 C116 1.429(7) . ? O16 C117 1.434(7) . ? O21 C202 1.434(8) . ? O21 C203 1.437(8) . ? O22 C204 1.404(8) . ? O22 C205 1.417(8) . ? O23 C208 1.422(8) . ? O23 C209 1.434(7) . ? O24 C210 1.415(7) . ? O24 C211 1.420(8) . ? O25 C215 1.421(8) . ? O25 C214 1.427(8) . ? O26 C216 1.411(7) . ? O26 C217 1.436(8) . ? C101 C102 1.497(9) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.479(9) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C105 C106 1.496(9) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 C108 1.496(9) . ? C107 H10M 0.9900 . ? C107 H10N 0.9900 . ? C108 H10O 0.9900 . ? C108 H10P 0.9900 . ? C109 C110 1.492(8) . ? C109 H10Q 0.9900 . ? C109 H10R 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.502(8) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 C114 1.495(8) . ? C113 H11G 0.9900 . ? C113 H11H 0.9900 . ? C114 H11I 0.9900 . ? C114 H11J 0.9900 . ? C115 C116 1.471(9) . ? C115 H11K 0.9900 . ? C115 H11L 0.9900 . ? C116 H11M 0.9900 . ? C116 H11N 0.9900 . ? C117 C118 1.479(9) . ? C117 H11O 0.9900 . ? C117 H11P 0.9900 . ? C118 H11Q 0.9900 . ? C118 H11R 0.9900 . ? C201 C202 1.481(10) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C203 C204 1.461(10) . ? C203 H20E 0.9900 . ? C203 H20F 0.9900 . ? C204 H20G 0.9900 . ? C204 H20H 0.9900 . ? C205 C206 1.473(11) . ? C205 H20I 0.9900 . ? C205 H20J 0.9900 . ? C206 H20K 0.9900 . ? C206 H20L 0.9900 . ? C207 C208 1.503(10) . ? C207 H20M 0.9900 . ? C207 H20N 0.9900 . ? C208 H20O 0.9900 . ? C208 H20P 0.9900 . ? C209 C210 1.463(9) . ? C209 H20Q 0.9900 . ? C209 H20R 0.9900 . ? C210 H21A 0.9900 . ? C210 H21B 0.9900 . ? C211 C212 1.513(9) . ? C211 H21C 0.9900 . ? C211 H21D 0.9900 . ? C212 H21E 0.9900 . ? C212 H21F 0.9900 . ? C213 C214 1.476(10) . ? C213 H21G 0.9900 . ? C213 H21H 0.9900 . ? C214 H21I 0.9900 . ? C214 H21J 0.9900 . ? C215 C216 1.479(10) . ? C215 H21K 0.9900 . ? C215 H21L 0.9900 . ? C216 H21M 0.9900 . ? C216 H21N 0.9900 . ? C217 C218 1.499(9) . ? C217 H21O 0.9900 . ? C217 H21P 0.9900 . ? C218 H21Q 0.9900 . ? C218 H21R 0.9900 . ? N1 C1 1.3900 . ? N1 C5 1.3900 . ? C1 C2 1.3900 . ? C1 H1 0.9500 . ? C2 C3 1.3900 . ? C2 H2 0.9500 . ? C3 C4 1.3900 . ? C3 H3 0.9500 . ? C4 C5 1.3900 . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C3S C2S 1.327(4) . ? C3S C4S 1.327(4) . ? C3S H3S 0.9500 . ? C2S C1S 1.327(4) . ? C2S H2S 0.9500 . ? C1S N1S 1.327(4) . ? C1S H1S 0.9500 . ? N1S C5S 1.327(4) . ? C5S C4S 1.327(4) . ? C5S H5S 0.9500 . ? C4S H4S 0.9500 . ? N1R C1R 1.3900 . ? N1R C5R 1.3900 . ? C1R C2R 1.3900 . ? C1R H1R 0.9500 . ? C2R C3R 1.3900 . ? C2R H2R 0.9500 . ? C3R C4R 1.3900 . ? C3R H3R 0.9500 . ? C4R C5R 1.3900 . ? C4R H4R 0.9500 . ? C5R H5R 0.9500 . ? N1Q C1Q 1.3900 . ? N1Q C5Q 1.3900 . ? C1Q C2Q 1.3900 . ? C1Q H1Q 0.9500 . ? C2Q C3Q 1.3900 . ? C2Q H2Q 0.9500 . ? C3Q C4Q 1.3900 . ? C3Q H3Q 0.9500 . ? C4Q C5Q 1.3900 . ? C4Q H4Q 0.9500 . ? C5Q H5Q 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P3 Cd1 P3 131.90(7) . 2_655 ? P3 Cd1 P2 77.31(4) . . ? P3 Cd1 P2 126.63(5) 2_655 . ? P3 Cd1 P2 126.63(5) . 2_655 ? P3 Cd1 P2 77.31(4) 2_655 2_655 ? P2 Cd1 P2 124.89(7) . 2_655 ? P4 P1 P3 102.82(9) . . ? P4 P1 P2 102.67(9) . . ? P3 P1 P2 97.98(8) . . ? P5 P2 P1 99.02(8) . . ? P5 P2 Cd1 90.00(7) . . ? P1 P2 Cd1 83.14(6) . . ? P6 P3 P1 99.18(8) . . ? P6 P3 Cd1 90.35(6) . . ? P1 P3 Cd1 83.69(6) . . ? P7 P4 P1 99.00(8) . . ? P2 P5 P6 104.82(8) . . ? P2 P5 P7 104.43(9) . . ? P6 P5 P7 60.74(7) . . ? P3 P6 P5 104.67(8) . . ? P3 P6 P7 104.65(8) . . ? P5 P6 P7 60.02(6) . . ? P4 P7 P5 107.05(9) . . ? P4 P7 P6 106.31(8) . . ? P5 P7 P6 59.24(6) . . ? O13 K1 O11 97.18(12) . . ? O13 K1 O14 60.63(10) . . ? O11 K1 O14 137.07(12) . . ? O13 K1 O16 136.06(13) . . ? O11 K1 O16 120.83(12) . . ? O14 K1 O16 97.30(11) . . ? O13 K1 O12 117.36(12) . . ? O11 K1 O12 59.70(12) . . ? O14 K1 O12 96.29(12) . . ? O16 K1 O12 101.51(11) . . ? O13 K1 O15 95.72(12) . . ? O11 K1 O15 99.49(12) . . ? O14 K1 O15 117.78(12) . . ? O16 K1 O15 59.42(11) . . ? O12 K1 O15 141.61(12) . . ? O13 K1 N12 120.17(12) . . ? O11 K1 N12 118.99(13) . . ? O14 K1 N12 60.50(11) . . ? O16 K1 N12 61.74(11) . . ? O12 K1 N12 60.55(12) . . ? O15 K1 N12 120.19(12) . . ? O13 K1 N11 60.09(12) . . ? O11 K1 N11 61.19(13) . . ? O14 K1 N11 119.69(12) . . ? O16 K1 N11 117.83(12) . . ? O12 K1 N11 119.71(13) . . ? O15 K1 N11 59.38(12) . . ? N12 K1 N11 179.57(14) . . ? O21 K2 O23 99.54(13) . . ? O21 K2 O26 119.28(13) . . ? O23 K2 O26 135.76(12) . . ? O21 K2 O24 140.38(13) . . ? O23 K2 O24 60.73(13) . . ? O26 K2 O24 95.17(12) . . ? O21 K2 O25 99.10(13) . . ? O23 K2 O25 94.87(13) . . ? O26 K2 O25 60.71(12) . . ? O24 K2 O25 115.57(13) . . ? O21 K2 O22 60.43(14) . . ? O23 K2 O22 119.06(14) . . ? O26 K2 O22 99.26(13) . . ? O24 K2 O22 97.45(14) . . ? O25 K2 O22 141.68(14) . . ? O21 K2 N21 60.96(15) . . ? O23 K2 N21 61.47(15) . . ? O26 K2 N21 118.50(15) . . ? O24 K2 N21 120.97(14) . . ? O25 K2 N21 59.12(14) . . ? O22 K2 N21 120.24(15) . . ? O21 K2 N22 117.66(14) . . ? O23 K2 N22 119.97(14) . . ? O26 K2 N22 61.17(13) . . ? O24 K2 N22 60.60(14) . . ? O25 K2 N22 120.89(13) . . ? O22 K2 N22 58.60(14) . . ? N21 K2 N22 178.38(15) . . ? C107 N11 C113 110.0(5) . . ? C107 N11 C101 110.1(5) . . ? C113 N11 C101 109.6(5) . . ? C107 N11 K1 108.8(3) . . ? C113 N11 K1 111.1(3) . . ? C101 N11 K1 107.3(3) . . ? C112 N12 C106 110.0(4) . . ? C112 N12 C118 110.2(4) . . ? C106 N12 C118 109.6(5) . . ? C112 N12 K1 109.2(3) . . ? C106 N12 K1 110.6(3) . . ? C118 N12 K1 107.2(3) . . ? C213 N21 C201 110.5(6) . . ? C213 N21 C207 110.6(6) . . ? C201 N21 C207 110.3(6) . . ? C213 N21 K2 111.3(4) . . ? C201 N21 K2 107.7(4) . . ? C207 N21 K2 106.3(4) . . ? C206 N22 C212 107.6(6) . . ? C206 N22 C218 111.2(5) . . ? C212 N22 C218 109.8(5) . . ? C206 N22 K2 111.1(4) . . ? C212 N22 K2 109.6(4) . . ? C218 N22 K2 107.5(4) . . ? C103 O11 C102 110.7(5) . . ? C103 O11 K1 114.7(4) . . ? C102 O11 K1 118.1(3) . . ? C104 O12 C105 110.1(5) . . ? C104 O12 K1 114.2(4) . . ? C105 O12 K1 115.8(3) . . ? C109 O13 C108 111.7(4) . . ? C109 O13 K1 115.5(3) . . ? C108 O13 K1 119.7(3) . . ? C111 O14 C110 110.6(4) . . ? C111 O14 K1 116.9(3) . . ? C110 O14 K1 111.5(3) . . ? C114 O15 C115 112.4(4) . . ? C114 O15 K1 117.3(3) . . ? C115 O15 K1 115.0(3) . . ? C116 O16 C117 111.9(5) . . ? C116 O16 K1 114.0(3) . . ? C117 O16 K1 115.8(3) . . ? C202 O21 C203 110.4(5) . . ? C202 O21 K2 119.9(4) . . ? C203 O21 K2 117.9(4) . . ? C204 O22 C205 111.1(6) . . ? C204 O22 K2 111.6(4) . . ? C205 O22 K2 116.2(4) . . ? C208 O23 C209 110.7(5) . . ? C208 O23 K2 118.5(4) . . ? C209 O23 K2 112.7(3) . . ? C210 O24 C211 111.6(5) . . ? C210 O24 K2 113.1(4) . . ? C211 O24 K2 116.3(4) . . ? C215 O25 C214 112.8(5) . . ? C215 O25 K2 112.1(4) . . ? C214 O25 K2 116.9(4) . . ? C216 O26 C217 110.7(4) . . ? C216 O26 K2 112.9(3) . . ? C217 O26 K2 116.3(3) . . ? N11 C101 C102 114.3(5) . . ? N11 C101 H10A 108.7 . . ? C102 C101 H10A 108.7 . . ? N11 C101 H10B 108.7 . . ? C102 C101 H10B 108.7 . . ? H10A C101 H10B 107.6 . . ? O11 C102 C101 110.2(5) . . ? O11 C102 H10C 109.6 . . ? C101 C102 H10C 109.6 . . ? O11 C102 H10D 109.6 . . ? C101 C102 H10D 109.6 . . ? H10C C102 H10D 108.1 . . ? O11 C103 C104 109.5(6) . . ? O11 C103 H10E 109.8 . . ? C104 C103 H10E 109.8 . . ? O11 C103 H10F 109.8 . . ? C104 C103 H10F 109.8 . . ? H10E C103 H10F 108.2 . . ? O12 C104 C103 109.5(6) . . ? O12 C104 H10G 109.8 . . ? C103 C104 H10G 109.8 . . ? O12 C104 H10H 109.8 . . ? C103 C104 H10H 109.8 . . ? H10G C104 H10H 108.2 . . ? O12 C105 C106 109.7(5) . . ? O12 C105 H10I 109.7 . . ? C106 C105 H10I 109.7 . . ? O12 C105 H10J 109.7 . . ? C106 C105 H10J 109.7 . . ? H10I C105 H10J 108.2 . . ? N12 C106 C105 114.3(5) . . ? N12 C106 H10K 108.7 . . ? C105 C106 H10K 108.7 . . ? N12 C106 H10L 108.7 . . ? C105 C106 H10L 108.7 . . ? H10K C106 H10L 107.6 . . ? N11 C107 C108 114.3(5) . . ? N11 C107 H10M 108.7 . . ? C108 C107 H10M 108.7 . . ? N11 C107 H10N 108.7 . . ? C108 C107 H10N 108.7 . . ? H10M C107 H10N 107.6 . . ? O13 C108 C107 108.8(5) . . ? O13 C108 H10O 109.9 . . ? C107 C108 H10O 109.9 . . ? O13 C108 H10P 109.9 . . ? C107 C108 H10P 109.9 . . ? H10O C108 H10P 108.3 . . ? O13 C109 C110 108.8(5) . . ? O13 C109 H10Q 109.9 . . ? C110 C109 H10Q 109.9 . . ? O13 C109 H10R 109.9 . . ? C110 C109 H10R 109.9 . . ? H10Q C109 H10R 108.3 . . ? O14 C110 C109 109.3(5) . . ? O14 C110 H11A 109.8 . . ? C109 C110 H11A 109.8 . . ? O14 C110 H11B 109.8 . . ? C109 C110 H11B 109.8 . . ? H11A C110 H11B 108.3 . . ? O14 C111 C112 109.3(4) . . ? O14 C111 H11C 109.8 . . ? C112 C111 H11C 109.8 . . ? O14 C111 H11D 109.8 . . ? C112 C111 H11D 109.8 . . ? H11C C111 H11D 108.3 . . ? N12 C112 C111 113.7(4) . . ? N12 C112 H11E 108.8 . . ? C111 C112 H11E 108.8 . . ? N12 C112 H11F 108.8 . . ? C111 C112 H11F 108.8 . . ? H11E C112 H11F 107.7 . . ? N11 C113 C114 113.6(5) . . ? N11 C113 H11G 108.8 . . ? C114 C113 H11G 108.8 . . ? N11 C113 H11H 108.8 . . ? C114 C113 H11H 108.8 . . ? H11G C113 H11H 107.7 . . ? O15 C114 C113 109.5(5) . . ? O15 C114 H11I 109.8 . . ? C113 C114 H11I 109.8 . . ? O15 C114 H11J 109.8 . . ? C113 C114 H11J 109.8 . . ? H11I C114 H11J 108.2 . . ? O15 C115 C116 109.5(5) . . ? O15 C115 H11K 109.8 . . ? C116 C115 H11K 109.8 . . ? O15 C115 H11L 109.8 . . ? C116 C115 H11L 109.8 . . ? H11K C115 H11L 108.2 . . ? O16 C116 C115 109.6(5) . . ? O16 C116 H11M 109.7 . . ? C115 C116 H11M 109.7 . . ? O16 C116 H11N 109.7 . . ? C115 C116 H11N 109.7 . . ? H11M C116 H11N 108.2 . . ? O16 C117 C118 110.7(5) . . ? O16 C117 H11O 109.5 . . ? C118 C117 H11O 109.5 . . ? O16 C117 H11P 109.5 . . ? C118 C117 H11P 109.5 . . ? H11O C117 H11P 108.1 . . ? C117 C118 N12 114.4(5) . . ? C117 C118 H11Q 108.7 . . ? N12 C118 H11Q 108.7 . . ? C117 C118 H11R 108.7 . . ? N12 C118 H11R 108.7 . . ? H11Q C118 H11R 107.6 . . ? C202 C201 N21 116.6(6) . . ? C202 C201 H20A 108.1 . . ? N21 C201 H20A 108.1 . . ? C202 C201 H20B 108.1 . . ? N21 C201 H20B 108.1 . . ? H20A C201 H20B 107.3 . . ? O21 C202 C201 109.2(5) . . ? O21 C202 H20C 109.8 . . ? C201 C202 H20C 109.8 . . ? O21 C202 H20D 109.8 . . ? C201 C202 H20D 109.8 . . ? H20C C202 H20D 108.3 . . ? O21 C203 C204 111.5(5) . . ? O21 C203 H20E 109.3 . . ? C204 C203 H20E 109.3 . . ? O21 C203 H20F 109.3 . . ? C204 C203 H20F 109.3 . . ? H20E C203 H20F 108.0 . . ? O22 C204 C203 114.8(7) . . ? O22 C204 H20G 108.6 . . ? C203 C204 H20G 108.6 . . ? O22 C204 H20H 108.6 . . ? C203 C204 H20H 108.6 . . ? H20G C204 H20H 107.5 . . ? O22 C205 C206 108.8(6) . . ? O22 C205 H20I 109.9 . . ? C206 C205 H20I 109.9 . . ? O22 C205 H20J 109.9 . . ? C206 C205 H20J 109.9 . . ? H20I C205 H20J 108.3 . . ? N22 C206 C205 113.4(7) . . ? N22 C206 H20K 108.9 . . ? C205 C206 H20K 108.9 . . ? N22 C206 H20L 108.9 . . ? C205 C206 H20L 108.9 . . ? H20K C206 H20L 107.7 . . ? N21 C207 C208 114.5(6) . . ? N21 C207 H20M 108.6 . . ? C208 C207 H20M 108.6 . . ? N21 C207 H20N 108.6 . . ? C208 C207 H20N 108.6 . . ? H20M C207 H20N 107.6 . . ? O23 C208 C207 109.2(6) . . ? O23 C208 H20O 109.8 . . ? C207 C208 H20O 109.8 . . ? O23 C208 H20P 109.8 . . ? C207 C208 H20P 109.8 . . ? H20O C208 H20P 108.3 . . ? O23 C209 C210 109.3(5) . . ? O23 C209 H20Q 109.8 . . ? C210 C209 H20Q 109.8 . . ? O23 C209 H20R 109.8 . . ? C210 C209 H20R 109.8 . . ? H20Q C209 H20R 108.3 . . ? O24 C210 C209 110.3(5) . . ? O24 C210 H21A 109.6 . . ? C209 C210 H21A 109.6 . . ? O24 C210 H21B 109.6 . . ? C209 C210 H21B 109.6 . . ? H21A C210 H21B 108.1 . . ? O24 C211 C212 109.9(6) . . ? O24 C211 H21C 109.7 . . ? C212 C211 H21C 109.7 . . ? O24 C211 H21D 109.7 . . ? C212 C211 H21D 109.7 . . ? H21C C211 H21D 108.2 . . ? N22 C212 C211 114.2(6) . . ? N22 C212 H21E 108.7 . . ? C211 C212 H21E 108.7 . . ? N22 C212 H21F 108.7 . . ? C211 C212 H21F 108.7 . . ? H21E C212 H21F 107.6 . . ? N21 C213 C214 113.6(6) . . ? N21 C213 H21G 108.8 . . ? C214 C213 H21G 108.8 . . ? N21 C213 H21H 108.8 . . ? C214 C213 H21H 108.8 . . ? H21G C213 H21H 107.7 . . ? O25 C214 C213 109.4(6) . . ? O25 C214 H21I 109.8 . . ? C213 C214 H21I 109.8 . . ? O25 C214 H21J 109.8 . . ? C213 C214 H21J 109.8 . . ? H21I C214 H21J 108.2 . . ? O25 C215 C216 110.4(5) . . ? O25 C215 H21K 109.6 . . ? C216 C215 H21K 109.6 . . ? O25 C215 H21L 109.6 . . ? C216 C215 H21L 109.6 . . ? H21K C215 H21L 108.1 . . ? O26 C216 C215 110.0(5) . . ? O26 C216 H21M 109.7 . . ? C215 C216 H21M 109.7 . . ? O26 C216 H21N 109.7 . . ? C215 C216 H21N 109.7 . . ? H21M C216 H21N 108.2 . . ? O26 C217 C218 109.6(5) . . ? O26 C217 H21O 109.8 . . ? C218 C217 H21O 109.8 . . ? O26 C217 H21P 109.8 . . ? C218 C217 H21P 109.8 . . ? H21O C217 H21P 108.2 . . ? N22 C218 C217 113.0(5) . . ? N22 C218 H21Q 109.0 . . ? C217 C218 H21Q 109.0 . . ? N22 C218 H21R 109.0 . . ? C217 C218 H21R 109.0 . . ? H21Q C218 H21R 107.8 . . ? C1 N1 C5 120.0 . . ? C2 C1 N1 120.0 . . ? C2 C1 H1 120.0 . . ? N1 C1 H1 120.0 . . ? C3 C2 C1 120.0 . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 N1 120.0 . . ? C4 C5 H5 120.0 . . ? N1 C5 H5 120.0 . . ? C2S C3S C4S 120.0 . . ? C2S C3S H3S 120.0 . . ? C4S C3S H3S 120.0 . . ? C3S C2S C1S 120.0 . . ? C3S C2S H2S 120.0 . . ? C1S C2S H2S 120.0 . . ? C2S C1S N1S 120.0 . . ? C2S C1S H1S 120.0 . . ? N1S C1S H1S 120.0 . . ? C1S N1S C5S 120.0 . . ? C4S C5S N1S 120.0 . . ? C4S C5S H5S 120.0 . . ? N1S C5S H5S 120.0 . . ? C5S C4S C3S 120.0 . . ? C5S C4S H4S 120.0 . . ? C3S C4S H4S 120.0 . . ? C1R N1R C5R 120.0 . . ? N1R C1R C2R 120.0 . . ? N1R C1R H1R 120.0 . . ? C2R C1R H1R 120.0 . . ? C3R C2R C1R 120.0 . . ? C3R C2R H2R 120.0 . . ? C1R C2R H2R 120.0 . . ? C4R C3R C2R 120.0 . . ? C4R C3R H3R 120.0 . . ? C2R C3R H3R 120.0 . . ? C5R C4R C3R 120.0 . . ? C5R C4R H4R 120.0 . . ? C3R C4R H4R 120.0 . . ? C4R C5R N1R 120.0 . . ? C4R C5R H5R 120.0 . . ? N1R C5R H5R 120.0 . . ? C1Q N1Q C5Q 120.0 . . ? C2Q C1Q N1Q 120.0 . . ? C2Q C1Q H1Q 120.0 . . ? N1Q C1Q H1Q 120.0 . . ? C3Q C2Q C1Q 120.0 . . ? C3Q C2Q H2Q 120.0 . . ? C1Q C2Q H2Q 120.0 . . ? C2Q C3Q C4Q 120.0 . . ? C2Q C3Q H3Q 120.0 . . ? C4Q C3Q H3Q 120.0 . . ? C3Q C4Q C5Q 120.0 . . ? C3Q C4Q H4Q 120.0 . . ? C5Q C4Q H4Q 120.0 . . ? C4Q C5Q N1Q 120.0 . . ? C4Q C5Q H5Q 120.0 . . ? N1Q C5Q H5Q 120.0 . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.745 _refine_diff_density_min -0.452 _refine_diff_density_rms 0.067 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 736079' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K(2,2,2-crypt)]2[P7In(C6H5)2] ; _contact_author_fax '+44 1865 272690' _chemical_name_common (K(2,2,2-crypt))2(P7In(C6H5)2) _chemical_melting_point ? _chemical_formula_moiety '2(C18 H36 N2 O6), C12 H10 In P7' _chemical_formula_sum 'C48 H82 In K2 N4 O12 P7' _chemical_formula_weight 1316.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 '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)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.4911(1) _cell_length_b 24.2435(2) _cell_length_c 22.4105(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.211(1) _cell_angle_gamma 90.00 _cell_volume 6238.57(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 142390 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2744 _exptl_absorpt_coefficient_mu 0.748 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8408 _exptl_absorpt_correction_T_max 0.9156 _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _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 21140 _diffrn_reflns_av_R_equivalents 0.0620 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 5.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10893 _reflns_number_gt 8995 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; KappaCCD software "Collect" (Nonius, 2000) ; _computing_cell_refinement ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_data_reduction ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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^)+(0.1071P)^2^+28.3581P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10893 _refine_ls_number_parameters 667 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0716 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1906 _refine_ls_wR_factor_gt 0.1835 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 P1 P 0.24842(11) 0.35183(6) 0.29788(6) 0.0261(3) Uani 1 1 d . . . P2 P 0.37951(11) 0.31421(6) 0.24138(6) 0.0240(3) Uani 1 1 d . . . P3 P 0.36954(12) 0.38400(6) 0.36880(6) 0.0276(3) Uani 1 1 d . . . P4 P 0.17117(12) 0.28062(6) 0.33829(6) 0.0296(3) Uani 1 1 d . . . P5 P 0.46859(12) 0.26063(6) 0.30683(6) 0.0257(3) Uani 1 1 d . . . P6 P 0.45856(12) 0.30808(6) 0.39332(6) 0.0273(3) Uani 1 1 d . . . P7 P 0.32822(12) 0.24141(6) 0.37067(6) 0.0276(3) Uani 1 1 d . . . In1 In 0.49506(4) 0.400625(18) 0.279111(19) 0.03591(16) Uani 1 1 d . . . C1 C 0.4509(5) 0.4779(3) 0.2286(2) 0.0345(13) Uani 1 1 d . . . C2 C 0.3503(5) 0.4806(2) 0.1935(3) 0.0317(12) Uani 1 1 d . . . H2 H 0.2982 0.4502 0.1942 0.038 Uiso 1 1 calc R . . C3 C 0.3204(5) 0.5248(3) 0.1574(3) 0.0369(13) Uani 1 1 d . . . H3 H 0.2503 0.5244 0.1334 0.044 Uiso 1 1 calc R . . C4 C 0.3942(7) 0.5698(3) 0.1567(3) 0.0501(18) Uani 1 1 d . . . H4 H 0.3757 0.6007 0.1321 0.060 Uiso 1 1 calc R . . C5 C 0.4951(6) 0.5693(3) 0.1919(4) 0.055(2) Uani 1 1 d . . . H5 H 0.5454 0.6004 0.1920 0.066 Uiso 1 1 calc R . . C6 C 0.5242(5) 0.5244(3) 0.2272(3) 0.0434(15) Uani 1 1 d . . . H6 H 0.5946 0.5249 0.2510 0.052 Uiso 1 1 calc R . . C7 C 0.6842(4) 0.3881(2) 0.2865(2) 0.0266(11) Uani 1 1 d . . . C8 C 0.7405(5) 0.3507(2) 0.3257(2) 0.0320(12) Uani 1 1 d . . . H8 H 0.6952 0.3299 0.3523 0.038 Uiso 1 1 calc R . . C9 C 0.8590(5) 0.3433(3) 0.3270(3) 0.0401(14) Uani 1 1 d . . . H9 H 0.8948 0.3172 0.3535 0.048 Uiso 1 1 calc R . . C10 C 0.9237(5) 0.3732(3) 0.2903(4) 0.053(2) Uani 1 1 d . . . H10 H 1.0057 0.3681 0.2916 0.064 Uiso 1 1 calc R . . C11 C 0.8752(6) 0.4109(3) 0.2509(3) 0.0527(19) Uani 1 1 d . . . H11 H 0.9228 0.4319 0.2256 0.063 Uiso 1 1 calc R . . C12 C 0.7529(5) 0.4178(3) 0.2487(3) 0.0357(13) Uani 1 1 d . . . H12 H 0.7177 0.4431 0.2211 0.043 Uiso 1 1 calc R . . K1 K -0.08829(10) 0.59316(4) 0.38717(5) 0.0249(3) Uani 1 1 d . . . K2 K 0.83113(9) 0.35566(4) 0.06545(5) 0.0212(2) Uani 1 1 d . . . N11 N -0.3338(4) 0.62478(19) 0.4181(2) 0.0323(10) Uani 1 1 d . . . N12 N 0.1583(4) 0.56078(18) 0.35586(19) 0.0298(10) Uani 1 1 d . . . N21 N 0.5744(4) 0.34239(19) 0.0579(2) 0.0286(10) Uani 1 1 d . . . N22 N 1.0882(4) 0.37064(18) 0.06873(19) 0.0246(9) Uani 1 1 d . . . O11 O -0.2376(3) 0.51536(14) 0.44508(17) 0.0292(8) Uani 1 1 d . . . O12 O -0.0185(3) 0.48540(15) 0.39624(17) 0.0319(9) Uani 1 1 d . . . O13 O -0.1168(3) 0.68347(14) 0.46460(15) 0.0270(8) Uani 1 1 d . . . O14 O 0.1095(3) 0.63769(14) 0.45019(16) 0.0273(8) Uani 1 1 d . . . O15 O -0.2535(4) 0.62360(17) 0.29594(17) 0.0401(10) Uani 1 1 d . . . O16 O -0.0075(4) 0.61407(18) 0.27150(17) 0.0400(10) Uani 1 1 d . . . O21 O 0.6850(3) 0.44691(15) 0.09030(17) 0.0283(8) Uani 1 1 d . . . O22 O 0.9235(3) 0.46469(15) 0.07293(17) 0.0288(8) Uani 1 1 d . . . O23 O 0.7203(3) 0.33188(15) -0.04836(15) 0.0261(8) Uani 1 1 d . . . O24 O 0.9614(3) 0.32462(15) -0.03585(15) 0.0245(7) Uani 1 1 d . . . O25 O 0.7332(3) 0.27052(14) 0.13572(15) 0.0254(8) Uani 1 1 d . . . O26 O 0.9668(3) 0.30095(14) 0.15105(15) 0.0255(8) Uani 1 1 d . . . C101 C -0.3826(5) 0.5843(2) 0.4582(3) 0.0361(13) Uani 1 1 d . . . H10A H -0.4677 0.5902 0.4595 0.043 Uiso 1 1 calc R . . H10B H -0.3488 0.5902 0.4990 0.043 Uiso 1 1 calc R . . C102 C -0.3597(5) 0.5252(3) 0.4394(3) 0.0412(14) Uani 1 1 d . . . H10C H -0.4017 0.4993 0.4651 0.049 Uiso 1 1 calc R . . H10D H -0.3875 0.5194 0.3975 0.049 Uiso 1 1 calc R . . C103 C -0.2099(5) 0.4610(2) 0.4242(3) 0.0344(13) Uani 1 1 d . . . H10E H -0.2315 0.4580 0.3811 0.041 Uiso 1 1 calc R . . H10F H -0.2552 0.4333 0.4459 0.041 Uiso 1 1 calc R . . C104 C -0.0833(5) 0.4501(2) 0.4339(3) 0.0343(13) Uani 1 1 d . . . H10G H -0.0600 0.4568 0.4763 0.041 Uiso 1 1 calc R . . H10H H -0.0665 0.4110 0.4246 0.041 Uiso 1 1 calc R . . C105 C 0.1002(5) 0.4688(2) 0.3956(3) 0.0339(13) Uani 1 1 d . . . H10I H 0.1051 0.4287 0.3877 0.041 Uiso 1 1 calc R . . H10J H 0.1392 0.4764 0.4349 0.041 Uiso 1 1 calc R . . C106 C 0.1597(5) 0.5005(2) 0.3474(3) 0.0361(13) Uani 1 1 d . . . H10K H 0.2416 0.4880 0.3461 0.043 Uiso 1 1 calc R . . H10L H 0.1209 0.4916 0.3084 0.043 Uiso 1 1 calc R . . C107 C -0.3251(5) 0.6791(2) 0.4484(3) 0.0369(13) Uani 1 1 d . . . H10M H -0.3989 0.6864 0.4684 0.044 Uiso 1 1 calc R . . H10N H -0.3158 0.7081 0.4178 0.044 Uiso 1 1 calc R . . C108 C -0.2269(5) 0.6832(2) 0.4934(3) 0.0326(12) Uani 1 1 d . . . H10O H -0.2348 0.7174 0.5169 0.039 Uiso 1 1 calc R . . H10P H -0.2295 0.6515 0.5211 0.039 Uiso 1 1 calc R . . C109 C -0.0249(5) 0.6884(2) 0.5084(2) 0.0289(12) Uani 1 1 d . . . H10Q H -0.0272 0.6569 0.5364 0.035 Uiso 1 1 calc R . . H10R H -0.0345 0.7228 0.5315 0.035 Uiso 1 1 calc R . . C110 C 0.0910(5) 0.6893(2) 0.4785(3) 0.0311(12) Uani 1 1 d . . . H11A H 0.0914 0.7193 0.4485 0.037 Uiso 1 1 calc R . . H11B H 0.1544 0.6964 0.5087 0.037 Uiso 1 1 calc R . . C111 C 0.2240(5) 0.6338(2) 0.4281(3) 0.0353(13) Uani 1 1 d . . . H11C H 0.2825 0.6418 0.4606 0.042 Uiso 1 1 calc R . . H11D H 0.2337 0.6610 0.3958 0.042 Uiso 1 1 calc R . . C112 C 0.2413(5) 0.5758(2) 0.4045(3) 0.0347(13) Uani 1 1 d . . . H11E H 0.3214 0.5725 0.3901 0.042 Uiso 1 1 calc R . . H11F H 0.2336 0.5492 0.4377 0.042 Uiso 1 1 calc R . . C113 C -0.4080(6) 0.6295(3) 0.3631(3) 0.0456(16) Uani 1 1 d . . . H11G H -0.4786 0.6510 0.3720 0.055 Uiso 1 1 calc R . . H11H H -0.4333 0.5922 0.3503 0.055 Uiso 1 1 calc R . . C114 C -0.3481(7) 0.6567(3) 0.3129(3) 0.0500(17) Uani 1 1 d . . . H11I H -0.4036 0.6617 0.2784 0.060 Uiso 1 1 calc R . . H11J H -0.3194 0.6936 0.3256 0.060 Uiso 1 1 calc R . . C115 C -0.1997(6) 0.6471(3) 0.2456(3) 0.0549(19) Uani 1 1 d . . . H11K H -0.1695 0.6843 0.2559 0.066 Uiso 1 1 calc R . . H11L H -0.2578 0.6509 0.2121 0.066 Uiso 1 1 calc R . . C116 C -0.1048(7) 0.6119(4) 0.2279(3) 0.059(2) Uani 1 1 d . . . H11M H -0.0782 0.6239 0.1885 0.070 Uiso 1 1 calc R . . H11N H -0.1329 0.5734 0.2240 0.070 Uiso 1 1 calc R . . C117 C 0.0941(7) 0.5863(3) 0.2525(3) 0.0503(17) Uani 1 1 d . . . H11O H 0.1215 0.6038 0.2157 0.060 Uiso 1 1 calc R . . H11P H 0.0749 0.5473 0.2433 0.060 Uiso 1 1 calc R . . C118 C 0.1875(6) 0.5886(3) 0.2998(3) 0.0423(15) Uani 1 1 d . . . H11Q H 0.2585 0.5714 0.2844 0.051 Uiso 1 1 calc R . . H11R H 0.2057 0.6277 0.3086 0.051 Uiso 1 1 calc R . . C201 C 0.5182(5) 0.3882(2) 0.0891(3) 0.0350(13) Uani 1 1 d . . . H20A H 0.5298 0.3827 0.1327 0.042 Uiso 1 1 calc R . . H20B H 0.4334 0.3870 0.0796 0.042 Uiso 1 1 calc R . . C202 C 0.5631(5) 0.4438(3) 0.0733(3) 0.0359(13) Uani 1 1 d . . . H20C H 0.5519 0.4501 0.0298 0.043 Uiso 1 1 calc R . . H20D H 0.5197 0.4727 0.0945 0.043 Uiso 1 1 calc R . . C203 C 0.7305(5) 0.5001(2) 0.0802(3) 0.0361(13) Uani 1 1 d . . . H20E H 0.6828 0.5283 0.1000 0.043 Uiso 1 1 calc R . . H20F H 0.7291 0.5081 0.0369 0.043 Uiso 1 1 calc R . . C204 C 0.8532(5) 0.5019(2) 0.1053(3) 0.0326(12) Uani 1 1 d . . . H20G H 0.8844 0.5398 0.1022 0.039 Uiso 1 1 calc R . . H20H H 0.8549 0.4914 0.1480 0.039 Uiso 1 1 calc R . . C205 C 1.0436(5) 0.4690(2) 0.0926(3) 0.0335(12) Uani 1 1 d . . . H20I H 1.0516 0.4607 0.1358 0.040 Uiso 1 1 calc R . . H20J H 1.0716 0.5070 0.0862 0.040 Uiso 1 1 calc R . . C206 C 1.1151(5) 0.4293(2) 0.0584(3) 0.0307(12) Uani 1 1 d . . . H20K H 1.1034 0.4372 0.0153 0.037 Uiso 1 1 calc R . . H20L H 1.1983 0.4357 0.0692 0.037 Uiso 1 1 calc R . . C207 C 0.5331(5) 0.3413(3) -0.0052(3) 0.0389(14) Uani 1 1 d . . . H20M H 0.5302 0.3796 -0.0204 0.047 Uiso 1 1 calc R . . H20N H 0.4528 0.3266 -0.0074 0.047 Uiso 1 1 calc R . . C208 C 0.6072(5) 0.3074(3) -0.0453(3) 0.0374(14) Uani 1 1 d . . . H20O H 0.6146 0.2693 -0.0294 0.045 Uiso 1 1 calc R . . H20P H 0.5698 0.3054 -0.0858 0.045 Uiso 1 1 calc R . . C209 C 0.7862(5) 0.3034(2) -0.0908(2) 0.0289(11) Uani 1 1 d . . . H20Q H 0.7461 0.3055 -0.1307 0.035 Uiso 1 1 calc R . . H20R H 0.7934 0.2641 -0.0795 0.035 Uiso 1 1 calc R . . C210 C 0.9044(5) 0.3288(2) -0.0932(2) 0.0304(12) Uani 1 1 d . . . H21A H 0.9504 0.3094 -0.1232 0.036 Uiso 1 1 calc R . . H21B H 0.8973 0.3680 -0.1050 0.036 Uiso 1 1 calc R . . C211 C 1.0807(5) 0.3411(2) -0.0385(2) 0.0306(12) Uani 1 1 d . . . H21C H 1.0852 0.3798 -0.0521 0.037 Uiso 1 1 calc R . . H21D H 1.1210 0.3175 -0.0673 0.037 Uiso 1 1 calc R . . C212 C 1.1388(4) 0.3354(2) 0.0229(2) 0.0305(12) Uani 1 1 d . . . H21E H 1.1335 0.2965 0.0357 0.037 Uiso 1 1 calc R . . H21F H 1.2224 0.3447 0.0203 0.037 Uiso 1 1 calc R . . C213 C 0.5474(5) 0.2896(2) 0.0868(3) 0.0345(13) Uani 1 1 d . . . H21G H 0.5656 0.2593 0.0591 0.041 Uiso 1 1 calc R . . H21H H 0.4628 0.2884 0.0933 0.041 Uiso 1 1 calc R . . C214 C 0.6119(5) 0.2794(2) 0.1457(3) 0.0334(12) Uani 1 1 d . . . H21I H 0.6028 0.3116 0.1723 0.040 Uiso 1 1 calc R . . H21J H 0.5790 0.2467 0.1653 0.040 Uiso 1 1 calc R . . C215 C 0.7962(5) 0.2651(2) 0.1920(2) 0.0313(12) Uani 1 1 d . . . H21K H 0.7638 0.2341 0.2148 0.038 Uiso 1 1 calc R . . H21L H 0.7874 0.2992 0.2157 0.038 Uiso 1 1 calc R . . C216 C 0.9223(5) 0.2549(2) 0.1826(2) 0.0297(12) Uani 1 1 d . . . H21M H 0.9651 0.2506 0.2215 0.036 Uiso 1 1 calc R . . H21N H 0.9320 0.2207 0.1592 0.036 Uiso 1 1 calc R . . C217 C 1.0916(4) 0.2982(2) 0.1492(2) 0.0290(11) Uani 1 1 d . . . H21O H 1.1149 0.2689 0.1213 0.035 Uiso 1 1 calc R . . H21P H 1.1259 0.2896 0.1894 0.035 Uiso 1 1 calc R . . C218 C 1.1342(5) 0.3538(2) 0.1284(2) 0.0303(12) Uani 1 1 d . . . H21Q H 1.1122 0.3821 0.1578 0.036 Uiso 1 1 calc R . . H21R H 1.2203 0.3530 0.1279 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0229(6) 0.0307(7) 0.0245(7) 0.0007(5) 0.0000(5) 0.0117(5) P2 0.0221(6) 0.0302(7) 0.0197(6) -0.0006(5) 0.0014(5) 0.0052(5) P3 0.0295(7) 0.0283(7) 0.0249(7) -0.0056(5) -0.0003(5) 0.0097(6) P4 0.0259(7) 0.0339(8) 0.0290(7) 0.0002(6) 0.0006(5) 0.0036(6) P5 0.0255(7) 0.0258(7) 0.0259(7) -0.0023(5) 0.0008(5) 0.0089(5) P6 0.0264(7) 0.0328(7) 0.0224(6) -0.0024(5) -0.0039(5) 0.0096(6) P7 0.0299(7) 0.0274(7) 0.0254(7) 0.0036(5) 0.0011(5) 0.0057(6) In1 0.0309(2) 0.0382(3) 0.0387(3) 0.00036(17) 0.00176(18) 0.00274(17) C1 0.028(3) 0.048(3) 0.028(3) 0.001(2) 0.004(2) -0.001(3) C2 0.024(3) 0.031(3) 0.040(3) 0.002(2) 0.000(2) -0.003(2) C3 0.032(3) 0.040(3) 0.038(3) 0.002(3) -0.002(2) 0.009(3) C4 0.066(5) 0.030(3) 0.057(4) 0.016(3) 0.026(4) 0.021(3) C5 0.053(4) 0.033(4) 0.081(5) -0.018(4) 0.027(4) -0.020(3) C6 0.035(3) 0.056(4) 0.040(3) -0.013(3) 0.002(3) -0.012(3) C7 0.018(2) 0.032(3) 0.029(3) -0.008(2) 0.000(2) 0.002(2) C8 0.039(3) 0.030(3) 0.027(3) -0.006(2) -0.005(2) 0.003(2) C9 0.032(3) 0.041(3) 0.046(4) -0.011(3) -0.015(3) 0.007(3) C10 0.022(3) 0.060(4) 0.076(5) -0.028(4) -0.013(3) 0.015(3) C11 0.032(3) 0.064(5) 0.064(5) -0.010(4) 0.026(3) -0.015(3) C12 0.029(3) 0.039(3) 0.039(3) 0.006(3) 0.005(2) 0.006(2) K1 0.0350(6) 0.0192(5) 0.0204(5) -0.0005(4) 0.0017(4) 0.0061(4) K2 0.0189(5) 0.0216(5) 0.0231(5) -0.0009(4) 0.0017(4) -0.0020(4) N11 0.032(2) 0.028(2) 0.036(3) -0.006(2) -0.006(2) 0.0086(19) N12 0.040(3) 0.025(2) 0.025(2) 0.0032(18) 0.0114(19) 0.0085(19) N21 0.020(2) 0.036(3) 0.029(2) -0.0025(19) 0.0023(18) -0.0048(18) N22 0.021(2) 0.026(2) 0.027(2) 0.0014(18) 0.0019(17) -0.0047(17) O11 0.0286(19) 0.0225(18) 0.036(2) -0.0076(15) 0.0004(16) 0.0004(15) O12 0.043(2) 0.0210(18) 0.033(2) 0.0060(15) 0.0107(17) 0.0110(16) O13 0.033(2) 0.0268(19) 0.0214(17) -0.0052(14) 0.0019(15) 0.0059(15) O14 0.0276(19) 0.0219(18) 0.033(2) -0.0058(15) 0.0079(15) 0.0002(15) O15 0.052(3) 0.039(2) 0.028(2) 0.0116(17) -0.0083(18) -0.006(2) O16 0.055(3) 0.041(2) 0.024(2) 0.0034(17) 0.0040(18) 0.001(2) O21 0.0246(18) 0.0244(19) 0.036(2) 0.0043(15) 0.0054(15) 0.0013(14) O22 0.0251(18) 0.0257(19) 0.036(2) -0.0046(15) 0.0011(15) -0.0037(15) O23 0.0243(18) 0.0282(19) 0.0256(18) -0.0070(15) -0.0022(14) -0.0013(15) O24 0.0242(18) 0.0315(19) 0.0179(17) 0.0038(14) 0.0040(14) 0.0040(15) O25 0.0222(17) 0.0284(19) 0.0261(18) -0.0036(15) 0.0071(14) -0.0025(14) O26 0.0217(17) 0.0279(19) 0.0268(18) 0.0066(15) 0.0015(14) -0.0008(14) C101 0.028(3) 0.035(3) 0.045(3) -0.006(3) 0.004(2) 0.004(2) C102 0.034(3) 0.036(3) 0.053(4) 0.001(3) 0.000(3) -0.004(3) C103 0.052(4) 0.016(2) 0.035(3) -0.004(2) 0.003(3) -0.003(2) C104 0.050(3) 0.019(3) 0.034(3) 0.005(2) 0.006(3) 0.005(2) C105 0.042(3) 0.023(3) 0.037(3) 0.001(2) 0.006(3) 0.012(2) C106 0.044(3) 0.031(3) 0.034(3) -0.007(2) 0.012(3) 0.012(3) C107 0.038(3) 0.028(3) 0.044(3) -0.011(2) 0.002(3) 0.011(2) C108 0.036(3) 0.031(3) 0.031(3) -0.012(2) 0.009(2) 0.003(2) C109 0.036(3) 0.024(3) 0.027(3) -0.006(2) 0.000(2) 0.007(2) C110 0.041(3) 0.022(3) 0.031(3) -0.010(2) 0.002(2) -0.002(2) C111 0.032(3) 0.030(3) 0.044(3) -0.003(2) 0.006(3) -0.001(2) C112 0.033(3) 0.032(3) 0.040(3) -0.001(2) 0.010(2) 0.009(2) C113 0.040(3) 0.047(4) 0.048(4) -0.007(3) -0.016(3) 0.012(3) C114 0.066(5) 0.036(3) 0.045(4) 0.005(3) -0.026(3) 0.008(3) C115 0.050(4) 0.070(5) 0.043(4) 0.026(3) -0.016(3) -0.019(4) C116 0.071(5) 0.087(6) 0.017(3) 0.008(3) -0.004(3) -0.029(4) C117 0.081(5) 0.047(4) 0.023(3) 0.008(3) 0.013(3) 0.008(4) C118 0.056(4) 0.040(3) 0.033(3) 0.006(3) 0.021(3) 0.008(3) C201 0.021(3) 0.040(3) 0.044(3) -0.003(3) 0.008(2) 0.002(2) C202 0.024(3) 0.043(3) 0.041(3) 0.000(3) 0.003(2) 0.007(2) C203 0.037(3) 0.024(3) 0.048(3) 0.006(2) 0.009(3) 0.004(2) C204 0.040(3) 0.018(3) 0.040(3) -0.003(2) 0.011(3) -0.004(2) C205 0.029(3) 0.029(3) 0.042(3) -0.003(2) -0.003(2) -0.010(2) C206 0.023(3) 0.031(3) 0.038(3) 0.005(2) 0.002(2) -0.010(2) C207 0.021(3) 0.056(4) 0.039(3) -0.005(3) -0.005(2) -0.005(3) C208 0.030(3) 0.048(4) 0.034(3) -0.009(3) -0.006(2) -0.016(3) C209 0.039(3) 0.030(3) 0.018(2) -0.006(2) -0.003(2) 0.005(2) C210 0.037(3) 0.037(3) 0.017(2) 0.003(2) 0.003(2) 0.009(2) C211 0.029(3) 0.035(3) 0.029(3) 0.001(2) 0.011(2) -0.002(2) C212 0.020(3) 0.038(3) 0.033(3) -0.004(2) 0.007(2) 0.001(2) C213 0.024(3) 0.036(3) 0.044(3) -0.006(3) 0.006(2) -0.009(2) C214 0.023(3) 0.036(3) 0.042(3) -0.002(2) 0.013(2) -0.003(2) C215 0.038(3) 0.030(3) 0.026(3) 0.003(2) 0.011(2) -0.004(2) C216 0.032(3) 0.027(3) 0.030(3) 0.008(2) 0.002(2) -0.001(2) C217 0.020(3) 0.035(3) 0.031(3) 0.002(2) -0.003(2) 0.004(2) C218 0.022(3) 0.037(3) 0.031(3) 0.005(2) -0.006(2) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 P4 2.157(2) . ? P1 P2 2.2026(18) . ? P1 P3 2.214(2) . ? P2 P5 2.1841(19) . ? P2 In1 2.6040(14) . ? P3 P6 2.1662(19) . ? P3 In1 2.5509(15) . ? P4 P7 2.142(2) . ? P5 P7 2.2459(19) . ? P5 P6 2.2608(19) . ? P6 P7 2.248(2) . ? In1 C7 2.195(5) . ? In1 C1 2.238(6) . ? C1 C2 1.375(8) . ? C1 C6 1.409(9) . ? C2 C3 1.378(8) . ? C2 H2 0.9500 . ? C3 C4 1.382(10) . ? C3 H3 0.9500 . ? C4 C5 1.378(11) . ? C4 H4 0.9500 . ? C5 C6 1.378(11) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.383(8) . ? C7 C8 1.402(8) . ? C8 C9 1.373(8) . ? C8 H8 0.9500 . ? C9 C10 1.343(11) . ? C9 H9 0.9500 . ? C10 C11 1.373(11) . ? C10 H10 0.9500 . ? C11 C12 1.414(9) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? K1 O12 2.738(4) . ? K1 O13 2.821(4) . ? K1 O16 2.833(4) . ? K1 O15 2.833(4) . ? K1 O14 2.842(4) . ? K1 O11 2.891(4) . ? K1 N11 3.030(5) . ? K1 N12 3.049(5) . ? K2 O26 2.764(4) . ? K2 O21 2.846(4) . ? K2 O22 2.851(4) . ? K2 O25 2.854(4) . ? K2 O23 2.865(4) . ? K2 O24 2.867(3) . ? K2 N21 2.966(4) . ? K2 N22 2.974(4) . ? N11 C101 1.456(8) . ? N11 C113 1.476(8) . ? N11 C107 1.483(7) . ? N12 C112 1.466(8) . ? N12 C106 1.474(7) . ? N12 C118 1.476(7) . ? N21 C213 1.471(7) . ? N21 C201 1.474(7) . ? N21 C207 1.475(7) . ? N22 C212 1.472(7) . ? N22 C206 1.475(7) . ? N22 C218 1.476(7) . ? O11 C102 1.423(7) . ? O11 C103 1.437(6) . ? O12 C105 1.422(7) . ? O12 C104 1.433(7) . ? O13 C109 1.418(6) . ? O13 C108 1.442(6) . ? O14 C110 1.422(6) . ? O14 C111 1.426(7) . ? O15 C114 1.415(8) . ? O15 C115 1.425(8) . ? O16 C117 1.426(8) . ? O16 C116 1.458(8) . ? O21 C203 1.414(7) . ? O21 C202 1.439(6) . ? O22 C204 1.427(6) . ? O22 C205 1.435(6) . ? O23 C209 1.418(6) . ? O23 C208 1.433(6) . ? O24 C210 1.423(6) . ? O24 C211 1.431(6) . ? O25 C214 1.436(6) . ? O25 C215 1.437(7) . ? O26 C216 1.426(6) . ? O26 C217 1.438(6) . ? C101 C102 1.520(8) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.487(8) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C105 C106 1.511(8) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 C108 1.488(8) . ? C107 H10M 0.9900 . ? C107 H10N 0.9900 . ? C108 H10O 0.9900 . ? C108 H10P 0.9900 . ? C109 C110 1.513(8) . ? C109 H10Q 0.9900 . ? C109 H10R 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.519(8) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 C114 1.496(10) . ? C113 H11G 0.9900 . ? C113 H11H 0.9900 . ? C114 H11I 0.9900 . ? C114 H11J 0.9900 . ? C115 C116 1.453(12) . ? C115 H11K 0.9900 . ? C115 H11L 0.9900 . ? C116 H11M 0.9900 . ? C116 H11N 0.9900 . ? C117 C118 1.479(10) . ? C117 H11O 0.9900 . ? C117 H11P 0.9900 . ? C118 H11Q 0.9900 . ? C118 H11R 0.9900 . ? C201 C202 1.492(8) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C203 C204 1.498(8) . ? C203 H20E 0.9900 . ? C203 H20F 0.9900 . ? C204 H20G 0.9900 . ? C204 H20H 0.9900 . ? C205 C206 1.495(8) . ? C205 H20I 0.9900 . ? C205 H20J 0.9900 . ? C206 H20K 0.9900 . ? C206 H20L 0.9900 . ? C207 C208 1.506(9) . ? C207 H20M 0.9900 . ? C207 H20N 0.9900 . ? C208 H20O 0.9900 . ? C208 H20P 0.9900 . ? C209 C210 1.494(8) . ? C209 H20Q 0.9900 . ? C209 H20R 0.9900 . ? C210 H21A 0.9900 . ? C210 H21B 0.9900 . ? C211 C212 1.513(8) . ? C211 H21C 0.9900 . ? C211 H21D 0.9900 . ? C212 H21E 0.9900 . ? C212 H21F 0.9900 . ? C213 C214 1.509(8) . ? C213 H21G 0.9900 . ? C213 H21H 0.9900 . ? C214 H21I 0.9900 . ? C214 H21J 0.9900 . ? C215 C216 1.493(8) . ? C215 H21K 0.9900 . ? C215 H21L 0.9900 . ? C216 H21M 0.9900 . ? C216 H21N 0.9900 . ? C217 C218 1.514(8) . ? C217 H21O 0.9900 . ? C217 H21P 0.9900 . ? C218 H21Q 0.9900 . ? C218 H21R 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P4 P1 P2 102.22(7) . . ? P4 P1 P3 103.77(8) . . ? P2 P1 P3 97.68(7) . . ? P5 P2 P1 99.99(7) . . ? P5 P2 In1 92.32(6) . . ? P1 P2 In1 80.31(6) . . ? P6 P3 P1 99.24(7) . . ? P6 P3 In1 93.34(6) . . ? P1 P3 In1 81.31(6) . . ? P7 P4 P1 98.19(8) . . ? P2 P5 P7 102.81(7) . . ? P2 P5 P6 103.60(7) . . ? P7 P5 P6 59.85(6) . . ? P3 P6 P7 104.45(7) . . ? P3 P6 P5 104.72(7) . . ? P7 P6 P5 59.74(6) . . ? P4 P7 P5 107.97(8) . . ? P4 P7 P6 107.62(8) . . ? P5 P7 P6 60.40(6) . . ? C7 In1 C1 111.0(2) . . ? C7 In1 P3 120.46(15) . . ? C1 In1 P3 114.02(14) . . ? C7 In1 P2 113.85(14) . . ? C1 In1 P2 114.00(15) . . ? P3 In1 P2 80.33(4) . . ? C2 C1 C6 116.1(6) . . ? C2 C1 In1 119.9(4) . . ? C6 C1 In1 123.9(4) . . ? C1 C2 C3 123.9(5) . . ? C1 C2 H2 118.0 . . ? C3 C2 H2 118.0 . . ? C2 C3 C4 118.7(6) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 119.4(6) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C6 C5 C4 121.1(6) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C1 120.8(6) . . ? C5 C6 H6 119.6 . . ? C1 C6 H6 119.6 . . ? C12 C7 C8 117.4(5) . . ? C12 C7 In1 117.9(4) . . ? C8 C7 In1 124.6(4) . . ? C9 C8 C7 122.1(6) . . ? C9 C8 H8 119.0 . . ? C7 C8 H8 119.0 . . ? C10 C9 C8 119.2(6) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C9 C10 C11 122.2(6) . . ? C9 C10 H10 118.9 . . ? C11 C10 H10 118.9 . . ? C10 C11 C12 118.6(6) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? C7 C12 C11 120.5(6) . . ? C7 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? O12 K1 O13 137.36(12) . . ? O12 K1 O16 97.66(12) . . ? O13 K1 O16 118.29(12) . . ? O12 K1 O15 119.23(13) . . ? O13 K1 O15 98.70(12) . . ? O16 K1 O15 61.79(13) . . ? O12 K1 O14 95.69(12) . . ? O13 K1 O14 60.60(10) . . ? O16 K1 O14 95.88(12) . . ? O15 K1 O14 139.48(12) . . ? O12 K1 O11 61.42(11) . . ? O13 K1 O11 98.35(11) . . ? O16 K1 O11 138.49(12) . . ? O15 K1 O11 95.80(12) . . ? O14 K1 O11 120.13(11) . . ? O12 K1 N11 119.82(13) . . ? O13 K1 N11 62.07(12) . . ? O16 K1 N11 120.35(13) . . ? O15 K1 N11 59.70(13) . . ? O14 K1 N11 121.61(11) . . ? O11 K1 N11 59.21(12) . . ? O12 K1 N12 59.94(12) . . ? O13 K1 N12 118.19(12) . . ? O16 K1 N12 59.67(12) . . ? O15 K1 N12 120.26(13) . . ? O14 K1 N12 58.63(11) . . ? O11 K1 N12 120.57(11) . . ? N11 K1 N12 179.72(14) . . ? O26 K2 O21 123.96(11) . . ? O26 K2 O22 101.85(11) . . ? O21 K2 O22 59.27(10) . . ? O26 K2 O25 59.59(10) . . ? O21 K2 O25 101.89(10) . . ? O22 K2 O25 142.37(11) . . ? O26 K2 O23 137.80(11) . . ? O21 K2 O23 94.88(11) . . ? O22 K2 O23 112.99(11) . . ? O25 K2 O23 100.05(10) . . ? O26 K2 O24 97.23(10) . . ? O21 K2 O24 133.55(11) . . ? O22 K2 O24 94.89(11) . . ? O25 K2 O24 118.43(10) . . ? O23 K2 O24 58.00(10) . . ? O26 K2 N21 121.38(12) . . ? O21 K2 N21 60.14(12) . . ? O22 K2 N21 118.12(12) . . ? O25 K2 N21 62.64(12) . . ? O23 K2 N21 61.34(11) . . ? O24 K2 N21 118.35(12) . . ? O26 K2 N22 60.55(11) . . ? O21 K2 N22 119.56(11) . . ? O22 K2 N22 61.18(11) . . ? O25 K2 N22 119.16(11) . . ? O23 K2 N22 116.97(11) . . ? O24 K2 N22 60.23(11) . . ? N21 K2 N22 177.99(13) . . ? C101 N11 C113 110.1(5) . . ? C101 N11 C107 109.7(5) . . ? C113 N11 C107 109.8(5) . . ? C101 N11 K1 110.8(3) . . ? C113 N11 K1 110.0(4) . . ? C107 N11 K1 106.4(3) . . ? C112 N12 C106 109.4(4) . . ? C112 N12 C118 111.0(5) . . ? C106 N12 C118 109.8(4) . . ? C112 N12 K1 110.4(3) . . ? C106 N12 K1 107.4(3) . . ? C118 N12 K1 108.8(3) . . ? C213 N21 C201 110.0(4) . . ? C213 N21 C207 109.9(4) . . ? C201 N21 C207 109.7(5) . . ? C213 N21 K2 107.2(3) . . ? C201 N21 K2 110.1(3) . . ? C207 N21 K2 109.8(3) . . ? C212 N22 C206 111.0(4) . . ? C212 N22 C218 109.5(4) . . ? C206 N22 C218 109.8(4) . . ? C212 N22 K2 109.3(3) . . ? C206 N22 K2 109.1(3) . . ? C218 N22 K2 108.0(3) . . ? C102 O11 C103 110.7(4) . . ? C102 O11 K1 116.8(3) . . ? C103 O11 K1 108.0(3) . . ? C105 O12 C104 110.9(4) . . ? C105 O12 K1 123.2(3) . . ? C104 O12 K1 117.2(3) . . ? C109 O13 C108 109.5(4) . . ? C109 O13 K1 112.9(3) . . ? C108 O13 K1 113.3(3) . . ? C110 O14 C111 111.6(4) . . ? C110 O14 K1 115.1(3) . . ? C111 O14 K1 122.2(3) . . ? C114 O15 C115 110.2(5) . . ? C114 O15 K1 117.0(3) . . ? C115 O15 K1 112.1(4) . . ? C117 O16 C116 113.5(5) . . ? C117 O16 K1 119.3(3) . . ? C116 O16 K1 109.7(3) . . ? C203 O21 C202 111.6(4) . . ? C203 O21 K2 116.9(3) . . ? C202 O21 K2 118.9(3) . . ? C204 O22 C205 110.8(4) . . ? C204 O22 K2 113.5(3) . . ? C205 O22 K2 115.9(3) . . ? C209 O23 C208 109.8(4) . . ? C209 O23 K2 117.7(3) . . ? C208 O23 K2 114.4(3) . . ? C210 O24 C211 110.5(4) . . ? C210 O24 K2 117.4(3) . . ? C211 O24 K2 119.3(3) . . ? C214 O25 C215 109.7(4) . . ? C214 O25 K2 112.5(3) . . ? C215 O25 K2 110.8(3) . . ? C216 O26 C217 110.8(4) . . ? C216 O26 K2 121.1(3) . . ? C217 O26 K2 122.6(3) . . ? N11 C101 C102 112.9(5) . . ? N11 C101 H10A 109.0 . . ? C102 C101 H10A 109.0 . . ? N11 C101 H10B 109.0 . . ? C102 C101 H10B 109.0 . . ? H10A C101 H10B 107.8 . . ? O11 C102 C101 108.3(5) . . ? O11 C102 H10C 110.0 . . ? C101 C102 H10C 110.0 . . ? O11 C102 H10D 110.0 . . ? C101 C102 H10D 110.0 . . ? H10C C102 H10D 108.4 . . ? O11 C103 C104 110.1(5) . . ? O11 C103 H10E 109.6 . . ? C104 C103 H10E 109.6 . . ? O11 C103 H10F 109.6 . . ? C104 C103 H10F 109.6 . . ? H10E C103 H10F 108.1 . . ? O12 C104 C103 109.5(4) . . ? O12 C104 H10G 109.8 . . ? C103 C104 H10G 109.8 . . ? O12 C104 H10H 109.8 . . ? C103 C104 H10H 109.8 . . ? H10G C104 H10H 108.2 . . ? O12 C105 C106 108.9(4) . . ? O12 C105 H10I 109.9 . . ? C106 C105 H10I 109.9 . . ? O12 C105 H10J 109.9 . . ? C106 C105 H10J 109.9 . . ? H10I C105 H10J 108.3 . . ? N12 C106 C105 113.9(4) . . ? N12 C106 H10K 108.8 . . ? C105 C106 H10K 108.8 . . ? N12 C106 H10L 108.8 . . ? C105 C106 H10L 108.8 . . ? H10K C106 H10L 107.7 . . ? N11 C107 C108 113.9(5) . . ? N11 C107 H10M 108.8 . . ? C108 C107 H10M 108.8 . . ? N11 C107 H10N 108.8 . . ? C108 C107 H10N 108.8 . . ? H10M C107 H10N 107.7 . . ? O13 C108 C107 110.7(4) . . ? O13 C108 H10O 109.5 . . ? C107 C108 H10O 109.5 . . ? O13 C108 H10P 109.5 . . ? C107 C108 H10P 109.5 . . ? H10O C108 H10P 108.1 . . ? O13 C109 C110 109.9(4) . . ? O13 C109 H10Q 109.7 . . ? C110 C109 H10Q 109.7 . . ? O13 C109 H10R 109.7 . . ? C110 C109 H10R 109.7 . . ? H10Q C109 H10R 108.2 . . ? O14 C110 C109 109.5(4) . . ? O14 C110 H11A 109.8 . . ? C109 C110 H11A 109.8 . . ? O14 C110 H11B 109.8 . . ? C109 C110 H11B 109.8 . . ? H11A C110 H11B 108.2 . . ? O14 C111 C112 108.5(4) . . ? O14 C111 H11C 110.0 . . ? C112 C111 H11C 110.0 . . ? O14 C111 H11D 110.0 . . ? C112 C111 H11D 110.0 . . ? H11C C111 H11D 108.4 . . ? N12 C112 C111 113.5(5) . . ? N12 C112 H11E 108.9 . . ? C111 C112 H11E 108.9 . . ? N12 C112 H11F 108.9 . . ? C111 C112 H11F 108.9 . . ? H11E C112 H11F 107.7 . . ? N11 C113 C114 113.3(5) . . ? N11 C113 H11G 108.9 . . ? C114 C113 H11G 108.9 . . ? N11 C113 H11H 108.9 . . ? C114 C113 H11H 108.9 . . ? H11G C113 H11H 107.7 . . ? O15 C114 C113 109.4(5) . . ? O15 C114 H11I 109.8 . . ? C113 C114 H11I 109.8 . . ? O15 C114 H11J 109.8 . . ? C113 C114 H11J 109.8 . . ? H11I C114 H11J 108.2 . . ? O15 C115 C116 109.5(6) . . ? O15 C115 H11K 109.8 . . ? C116 C115 H11K 109.8 . . ? O15 C115 H11L 109.8 . . ? C116 C115 H11L 109.8 . . ? H11K C115 H11L 108.2 . . ? C115 C116 O16 111.1(6) . . ? C115 C116 H11M 109.4 . . ? O16 C116 H11M 109.4 . . ? C115 C116 H11N 109.4 . . ? O16 C116 H11N 109.4 . . ? H11M C116 H11N 108.0 . . ? O16 C117 C118 110.4(5) . . ? O16 C117 H11O 109.6 . . ? C118 C117 H11O 109.6 . . ? O16 C117 H11P 109.6 . . ? C118 C117 H11P 109.6 . . ? H11O C117 H11P 108.1 . . ? N12 C118 C117 114.2(6) . . ? N12 C118 H11Q 108.7 . . ? C117 C118 H11Q 108.7 . . ? N12 C118 H11R 108.7 . . ? C117 C118 H11R 108.7 . . ? H11Q C118 H11R 107.6 . . ? N21 C201 C202 114.0(5) . . ? N21 C201 H20A 108.7 . . ? C202 C201 H20A 108.7 . . ? N21 C201 H20B 108.7 . . ? C202 C201 H20B 108.7 . . ? H20A C201 H20B 107.6 . . ? O21 C202 C201 109.0(5) . . ? O21 C202 H20C 109.9 . . ? C201 C202 H20C 109.9 . . ? O21 C202 H20D 109.9 . . ? C201 C202 H20D 109.9 . . ? H20C C202 H20D 108.3 . . ? O21 C203 C204 108.4(4) . . ? O21 C203 H20E 110.0 . . ? C204 C203 H20E 110.0 . . ? O21 C203 H20F 110.0 . . ? C204 C203 H20F 110.0 . . ? H20E C203 H20F 108.4 . . ? O22 C204 C203 109.6(5) . . ? O22 C204 H20G 109.8 . . ? C203 C204 H20G 109.8 . . ? O22 C204 H20H 109.8 . . ? C203 C204 H20H 109.8 . . ? H20G C204 H20H 108.2 . . ? O22 C205 C206 109.7(4) . . ? O22 C205 H20I 109.7 . . ? C206 C205 H20I 109.7 . . ? O22 C205 H20J 109.7 . . ? C206 C205 H20J 109.7 . . ? H20I C205 H20J 108.2 . . ? N22 C206 C205 114.7(4) . . ? N22 C206 H20K 108.6 . . ? C205 C206 H20K 108.6 . . ? N22 C206 H20L 108.6 . . ? C205 C206 H20L 108.6 . . ? H20K C206 H20L 107.6 . . ? N21 C207 C208 114.4(5) . . ? N21 C207 H20M 108.7 . . ? C208 C207 H20M 108.7 . . ? N21 C207 H20N 108.7 . . ? C208 C207 H20N 108.7 . . ? H20M C207 H20N 107.6 . . ? O23 C208 C207 109.6(5) . . ? O23 C208 H20O 109.7 . . ? C207 C208 H20O 109.7 . . ? O23 C208 H20P 109.7 . . ? C207 C208 H20P 109.7 . . ? H20O C208 H20P 108.2 . . ? O23 C209 C210 109.5(4) . . ? O23 C209 H20Q 109.8 . . ? C210 C209 H20Q 109.8 . . ? O23 C209 H20R 109.8 . . ? C210 C209 H20R 109.8 . . ? H20Q C209 H20R 108.2 . . ? O24 C210 C209 109.0(4) . . ? O24 C210 H21A 109.9 . . ? C209 C210 H21A 109.9 . . ? O24 C210 H21B 109.9 . . ? C209 C210 H21B 109.9 . . ? H21A C210 H21B 108.3 . . ? O24 C211 C212 109.1(4) . . ? O24 C211 H21C 109.9 . . ? C212 C211 H21C 109.9 . . ? O24 C211 H21D 109.9 . . ? C212 C211 H21D 109.9 . . ? H21C C211 H21D 108.3 . . ? N22 C212 C211 114.2(4) . . ? N22 C212 H21E 108.7 . . ? C211 C212 H21E 108.7 . . ? N22 C212 H21F 108.7 . . ? C211 C212 H21F 108.7 . . ? H21E C212 H21F 107.6 . . ? N21 C213 C214 115.0(4) . . ? N21 C213 H21G 108.5 . . ? C214 C213 H21G 108.5 . . ? N21 C213 H21H 108.5 . . ? C214 C213 H21H 108.5 . . ? H21G C213 H21H 107.5 . . ? O25 C214 C213 109.6(4) . . ? O25 C214 H21I 109.7 . . ? C213 C214 H21I 109.7 . . ? O25 C214 H21J 109.7 . . ? C213 C214 H21J 109.7 . . ? H21I C214 H21J 108.2 . . ? O25 C215 C216 110.5(4) . . ? O25 C215 H21K 109.6 . . ? C216 C215 H21K 109.6 . . ? O25 C215 H21L 109.6 . . ? C216 C215 H21L 109.6 . . ? H21K C215 H21L 108.1 . . ? O26 C216 C215 108.0(4) . . ? O26 C216 H21M 110.1 . . ? C215 C216 H21M 110.1 . . ? O26 C216 H21N 110.1 . . ? C215 C216 H21N 110.1 . . ? H21M C216 H21N 108.4 . . ? O26 C217 C218 107.6(4) . . ? O26 C217 H21O 110.2 . . ? C218 C217 H21O 110.2 . . ? O26 C217 H21P 110.2 . . ? C218 C217 H21P 110.2 . . ? H21O C217 H21P 108.5 . . ? N22 C218 C217 114.6(4) . . ? N22 C218 H21Q 108.6 . . ? C217 C218 H21Q 108.6 . . ? N22 C218 H21R 108.6 . . ? C217 C218 H21R 108.6 . . ? H21Q C218 H21R 107.6 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.970 _refine_diff_density_min -2.436 _refine_diff_density_rms 0.129