Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, p. 435. Coppens, P. (1970). Crystallographic Computing, edited by F.R. Ahmed, S.R.Hall & C.P. Huber, pp. 255-270, Copenhagen, Munksgaard. Hooft, R.W. (1998). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods Enzymol. 276, 307--326. Sheldrick, G. M. (1997). SHELXL97. University of Gottingen, Germany. Spek, A.L. (1999). PLATON. Version 1999. Utrecht University, The Netherlands. ; _publ_contact_author_name 'Petr Hermann' _publ_contact_author_email PETRH@NATUR.CUNI.CZ loop_ _publ_author_name P.Hermann J.Havlickova J.Kotek P.Lubal I.Lukes J.Plutnar I.Svobodova data_mndip _database_code_depnum_ccdc_archive 'CCDC 600826' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C12 H48 Mn2 N4 O16 P2, C12 H28 N4 O6 P2, (H2 O)21' ; _chemical_formula_sum 'C24 H118 Mn2 N8 O43 P4' _chemical_formula_weight 1441.02 _chemical_compound_source 'synthesized by the authors' 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' Mn Mn 0.3368 0.7283 '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 9.7361(3) _cell_length_b 12.2695(4) _cell_length_c 14.0948(4) _cell_angle_alpha 87.8084(17) _cell_angle_beta 77.3777(17) _cell_angle_gamma 88.4157(13) _cell_volume 1641.51(9) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6889 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 0.584 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13728 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 27.51 _reflns_number_total 7504 _reflns_number_gt 5560 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+2.3729P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7504 _refine_ls_number_parameters 406 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0755 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1224 _refine_ls_wR_factor_gt 0.1080 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.007 _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 Mn1 Mn 0.76807(4) -0.00911(3) 0.85614(3) 0.01838(11) Uani 1 1 d . . . O1 O 0.71841(19) -0.02246(15) 1.01938(12) 0.0203(4) Uani 1 1 d . . . H1O1 H 0.7532 -0.0789 1.0488 0.026 Uiso 1 1 d R . . H2O1 H 0.7400 0.0376 1.0425 0.026 Uiso 1 1 d R . . O2 O 0.98566(19) 0.00977(16) 0.85872(14) 0.0251(4) Uani 1 1 d . . . H1O2 H 1.0442 -0.0483 0.8755 0.033 Uiso 1 1 d R . . H2O2 H 1.0411 0.0609 0.8697 0.033 Uiso 1 1 d R . . O3 O 0.8249(3) -0.18065(17) 0.84502(15) 0.0397(6) Uani 1 1 d . . . H1O3 H 0.8225 -0.2239 0.7970 0.052 Uiso 1 1 d R . . H2O3 H 0.8210 -0.2279 0.9049 0.052 Uiso 1 1 d R . . O4A O 0.5438(3) -0.0470(2) 0.87628(19) 0.0238(9) Uiso 0.764(9) 1 d P . . H1O4 H 0.5357 -0.0356 0.8070 0.031 Uiso 1 1 d R . . H2O4 H 0.4605 -0.0005 0.9123 0.031 Uiso 1 1 d R . . O4B O 0.5443(9) 0.0070(9) 0.8675(6) 0.0238(9) Uiso 0.24 1 d P . . O5 O 0.7485(3) 0.16827(18) 0.87267(17) 0.0493(7) Uani 1 1 d . . . H1O5 H 0.8196 0.2013 0.8934 0.064 Uiso 1 1 d R . . H2O5 H 0.7090 0.2114 0.8503 0.064 Uiso 1 1 d R . . P1 P 0.68867(7) -0.02123(5) 0.63274(5) 0.01600(15) Uani 1 1 d . . . O11 O 0.78513(18) -0.00119(15) 0.70331(12) 0.0191(4) Uani 1 1 d . . . O12 O 0.53429(18) -0.02850(15) 0.68677(13) 0.0203(4) Uani 1 1 d . . . O13 O 0.74133(19) -0.11823(15) 0.57017(13) 0.0202(4) Uani 1 1 d . . . C8 C 0.6977(3) 0.1012(2) 0.55393(19) 0.0196(5) Uani 1 1 d . . . H81 H 0.6359 0.0929 0.5093 0.024 Uiso 1 1 calc R . . H82 H 0.6631 0.1631 0.5936 0.024 Uiso 1 1 calc R . . N1 N 0.8419(2) 0.12464(18) 0.49661(15) 0.0197(5) Uani 1 1 d . . . C2 C 0.8483(3) 0.1174(2) 0.39162(19) 0.0251(6) Uani 1 1 d . . . H21 H 0.9374 0.1454 0.3554 0.030 Uiso 1 1 calc R . . H22 H 0.7735 0.1623 0.3742 0.030 Uiso 1 1 calc R . . C3 C 0.8338(3) 0.0010(2) 0.36366(19) 0.0239(6) Uani 1 1 d . . . H31 H 0.7444 -0.0275 0.3988 0.029 Uiso 1 1 calc R . . H32 H 0.8366 -0.0013 0.2945 0.029 Uiso 1 1 calc R . . N4 N 0.9513(2) -0.06612(18) 0.38789(16) 0.0207(5) Uani 1 1 d . . . H41 H 0.9462 -0.0631 0.4523 0.027 Uiso 1 1 calc R . . H42 H 1.0330 -0.0359 0.3573 0.027 Uiso 1 1 calc R . . C5 C 0.9557(3) -0.1827(2) 0.3622(2) 0.0268(6) Uani 1 1 d . . . H51 H 0.9528 -0.1873 0.2941 0.032 Uiso 1 1 calc R . . H52 H 0.8733 -0.2186 0.4005 0.032 Uiso 1 1 calc R . . C6 C 1.0869(3) -0.2413(2) 0.3802(2) 0.0278(6) Uani 1 1 d . . . H61 H 1.1678 -0.2119 0.3345 0.033 Uiso 1 1 calc R . . H62 H 1.0815 -0.3178 0.3665 0.033 Uiso 1 1 calc R . . C7 C 1.1118(3) -0.2333(2) 0.4832(2) 0.0259(6) Uani 1 1 d . . . H71 H 1.0252 -0.2504 0.5296 0.031 Uiso 1 1 calc R . . H72 H 1.1825 -0.2874 0.4926 0.031 Uiso 1 1 calc R . . P2 P 0.89215(8) 0.72571(6) 0.08529(5) 0.02023(16) Uani 1 1 d . . . O21 O 0.83271(19) 0.83319(14) 0.12929(13) 0.0195(4) Uani 1 1 d . . . O22 O 1.0530(2) 0.72657(17) 0.05572(16) 0.0347(5) Uani 1 1 d . . . O23 O 0.8276(3) 0.69443(17) 0.00191(15) 0.0431(6) Uani 1 1 d . . . C18 C 0.8439(3) 0.6213(2) 0.18127(19) 0.0223(6) Uani 1 1 d . . . H181 H 0.8831 0.6391 0.2362 0.027 Uiso 1 1 calc R . . H182 H 0.7422 0.6209 0.2029 0.027 Uiso 1 1 calc R . . N11 N 0.8949(3) 0.51120(19) 0.14864(17) 0.0289(6) Uani 1 1 d . . . C12 C 0.7769(4) 0.4369(2) 0.1552(2) 0.0397(8) Uani 1 1 d D . . H121 H 0.7099 0.4455 0.2166 0.048 Uiso 1 1 calc R A 1 H122 H 0.8114 0.3619 0.1524 0.048 Uiso 1 1 calc R A 1 C13 C 0.7058(9) 0.4630(9) 0.0716(5) 0.034(2) Uani 0.609(8) 1 d P B 1 H131 H 0.6377 0.4075 0.0693 0.041 Uiso 0.609(8) 1 calc PR B 1 H132 H 0.6562 0.5327 0.0813 0.041 Uiso 0.609(8) 1 calc PR B 1 N14 N 0.8117(8) 0.4672(6) -0.0207(4) 0.0206(14) Uani 0.609(8) 1 d P B 1 H141 H 0.8599 0.4033 -0.0272 0.027 Uiso 0.609(8) 1 calc PR B 1 H142 H 0.8731 0.5199 -0.0179 0.027 Uiso 0.609(8) 1 calc PR B 1 C15 C 0.7516(5) 0.4886(4) -0.1079(3) 0.0277(14) Uani 0.609(8) 1 d P B 1 H151 H 0.7166 0.5634 -0.1083 0.033 Uiso 0.609(8) 1 calc PR B 1 H152 H 0.6730 0.4408 -0.1052 0.033 Uiso 0.609(8) 1 calc PR B 1 C16 C 0.8616(6) 0.4698(5) -0.2004(5) 0.0273(13) Uani 0.609(8) 1 d P B 1 H161 H 0.8225 0.4923 -0.2559 0.033 Uiso 0.609(8) 1 calc PR B 1 H162 H 0.8839 0.3924 -0.2049 0.033 Uiso 0.609(8) 1 calc PR B 1 C13B C 0.6618(13) 0.4677(15) 0.1005(8) 0.052(5) Uani 0.391(8) 1 d PD B 2 H133 H 0.6402 0.5448 0.1087 0.063 Uiso 0.391(8) 1 calc PR B 2 H134 H 0.5778 0.4286 0.1317 0.063 Uiso 0.391(8) 1 calc PR B 2 C14B C 0.6915(8) 0.4460(7) -0.0108(6) 0.031(2) Uani 0.391(8) 1 d P B 2 H143 H 0.6935 0.3683 -0.0214 0.037 Uiso 0.391(8) 1 calc PR B 2 H144 H 0.6186 0.4801 -0.0398 0.037 Uiso 0.391(8) 1 calc PR B 2 N15B N 0.8305(12) 0.4937(8) -0.0548(7) 0.019(2) Uani 0.391(8) 1 d P B 2 H153 H 0.8959 0.4588 -0.0279 0.023 Uiso 0.391(8) 1 calc PR B 2 H154 H 0.8280 0.5639 -0.0381 0.023 Uiso 0.391(8) 1 calc PR B 2 C16B C 0.8776(10) 0.4897(8) -0.1623(7) 0.025(2) Uani 0.391(8) 1 d P B 2 H163 H 0.8817 0.4138 -0.1797 0.030 Uiso 0.391(8) 1 calc PR B 2 H164 H 0.8057 0.5257 -0.1909 0.030 Uiso 0.391(8) 1 calc PR B 2 C17 C 1.0059(4) 0.5355(3) -0.2056(2) 0.0401(8) Uani 1 1 d . . . H171 H 1.0552 0.5415 -0.2732 0.048 Uiso 1 1 calc R B 1 H172 H 0.9803 0.6089 -0.1840 0.048 Uiso 1 1 calc R B 1 O1W O 0.3940(2) 0.16945(16) 0.71255(13) 0.0246(4) Uani 1 1 d . . . H1W1 H 0.3212 0.1653 0.7683 0.032 Uiso 1 1 d R . . H2W1 H 0.4354 0.0997 0.7070 0.032 Uiso 1 1 d R . . O2W O 0.8264(2) 0.14591(16) 0.10010(14) 0.0266(4) Uani 1 1 d . . . H1W2 H 0.7623 0.1822 0.1472 0.035 Uiso 1 1 d R . . H2W2 H 0.8721 0.2008 0.0486 0.035 Uiso 1 1 d R . . O3W O 0.5903(2) 0.37177(19) 0.39563(16) 0.0399(6) Uani 1 1 d . . . H1W3 H 0.6394 0.4138 0.4251 0.052 Uiso 1 1 d R . . H2W3 H 0.5329 0.3410 0.4502 0.052 Uiso 1 1 d R . . O4W O 0.6089(2) 0.21658(18) 0.24677(16) 0.0374(5) Uani 1 1 d . . . H1W4 H 0.5581 0.1583 0.2809 0.049 Uiso 1 1 d R . . H2W4 H 0.6207 0.2665 0.3030 0.049 Uiso 1 1 d R . . O5W O 0.3819(2) 0.26414(17) 0.52810(14) 0.0285(5) Uani 1 1 d . . . H1W5 H 0.3826 0.2362 0.5871 0.037 Uiso 1 1 d R . . H2W5 H 0.3421 0.2065 0.4985 0.037 Uiso 1 1 d R . . O6W O 0.2064(3) 0.29414(18) 0.31434(16) 0.0407(6) Uani 1 1 d . . . H1W6 H 0.2257 0.2365 0.3546 0.053 Uiso 1 1 d R . . H2W6 H 0.2836 0.3482 0.3053 0.053 Uiso 1 1 d R . . O7W O 0.4298(3) 0.6961(2) 0.2133(3) 0.0700(9) Uani 1 1 d . . . H1W7 H 0.4692 0.7578 0.2204 0.091 Uiso 1 1 d R . . H2W7 H 0.4061 0.6665 0.2790 0.091 Uiso 1 1 d R . . O8W O 0.2418(3) 0.4744(2) 0.5427(3) 0.0734(10) Uani 1 1 d . . . H1W8 H 0.2810 0.4031 0.5497 0.095 Uiso 1 1 d R . . H2W8 H 0.1550 0.4903 0.5477 0.095 Uiso 1 1 d R . . O9W O 0.3889(4) 0.4875(4) 0.3192(4) 0.1290(19) Uani 1 1 d . . . H1W9 H 0.4218 0.4593 0.2597 0.168 Uiso 1 1 d R . . H2W9 H 0.4430 0.5376 0.3424 0.168 Uiso 1 1 d R . . O10W O 0.4654(4) 0.2546(3) 0.0069(2) 0.0948(13) Uani 1 1 d . . . H10W H 0.5184 0.2396 0.0572 0.123 Uiso 1 1 d R . . H10V H 0.3804 0.2693 0.0044 0.123 Uiso 1 1 d R . . O11W O 0.0507(5) 0.4718(4) 0.4409(4) 0.0490(13) Uani 0.50 1 d P . . H11W H 0.0977 0.3964 0.4203 0.064 Uiso 0.50 1 d PR . . H11V H 0.1046 0.5225 0.4369 0.064 Uiso 0.50 1 d 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 Mn1 0.0198(2) 0.0192(2) 0.0160(2) -0.00016(15) -0.00357(16) -0.00139(16) O1 0.0253(10) 0.0184(9) 0.0171(9) -0.0002(7) -0.0049(8) 0.0013(8) O2 0.0194(10) 0.0251(11) 0.0320(11) -0.0030(8) -0.0071(8) -0.0036(8) O3 0.0784(18) 0.0187(11) 0.0278(11) -0.0011(9) -0.0241(12) 0.0010(11) O5 0.097(2) 0.0197(12) 0.0409(13) -0.0001(10) -0.0375(14) 0.0038(12) P1 0.0157(3) 0.0175(3) 0.0141(3) -0.0001(2) -0.0019(2) 0.0002(3) O11 0.0173(9) 0.0238(10) 0.0161(9) -0.0001(7) -0.0037(7) -0.0013(7) O12 0.0166(9) 0.0233(10) 0.0199(9) -0.0004(8) -0.0013(7) -0.0022(7) O13 0.0243(10) 0.0188(10) 0.0169(9) -0.0021(7) -0.0031(7) 0.0028(8) C8 0.0159(12) 0.0225(14) 0.0195(13) 0.0007(10) -0.0025(10) 0.0031(10) N1 0.0194(11) 0.0193(12) 0.0186(11) 0.0039(9) -0.0010(9) -0.0006(9) C2 0.0231(14) 0.0311(16) 0.0191(13) 0.0077(12) -0.0018(11) 0.0013(12) C3 0.0201(14) 0.0362(17) 0.0151(12) 0.0001(11) -0.0036(11) 0.0009(12) N4 0.0183(11) 0.0255(13) 0.0179(11) -0.0036(9) -0.0023(9) -0.0019(9) C5 0.0268(15) 0.0257(15) 0.0266(14) -0.0072(12) -0.0010(12) -0.0078(12) C6 0.0279(15) 0.0208(15) 0.0314(15) -0.0055(12) 0.0017(12) -0.0043(12) C7 0.0259(15) 0.0182(14) 0.0307(15) 0.0041(12) -0.0010(12) -0.0003(11) P2 0.0295(4) 0.0136(3) 0.0165(3) 0.0002(3) -0.0027(3) -0.0001(3) O21 0.0229(10) 0.0131(9) 0.0220(9) -0.0015(7) -0.0038(8) -0.0004(7) O22 0.0336(12) 0.0248(11) 0.0365(12) 0.0088(9) 0.0097(10) 0.0088(9) O23 0.0906(19) 0.0217(11) 0.0234(11) 0.0034(9) -0.0251(12) -0.0148(12) C18 0.0297(15) 0.0177(14) 0.0174(12) -0.0008(10) -0.0005(11) -0.0008(11) N11 0.0487(16) 0.0124(12) 0.0209(12) 0.0011(9) 0.0021(11) 0.0002(11) C12 0.072(3) 0.0163(15) 0.0278(16) 0.0000(12) -0.0043(16) -0.0072(15) C13 0.062(4) 0.026(3) 0.012(4) -0.003(4) -0.002(4) -0.015(4) N14 0.021(3) 0.017(3) 0.024(4) -0.004(2) -0.007(3) -0.001(2) C15 0.032(3) 0.025(3) 0.032(3) -0.009(2) -0.017(2) 0.003(2) C16 0.040(3) 0.025(3) 0.022(3) -0.006(2) -0.018(3) 0.006(2) C13B 0.117(14) 0.028(6) 0.003(5) -0.005(5) 0.009(6) -0.025(8) C14B 0.020(4) 0.032(5) 0.037(5) -0.010(3) 0.000(3) 0.001(3) N15B 0.023(4) 0.015(5) 0.021(5) -0.004(3) -0.006(4) 0.000(3) C16B 0.036(5) 0.026(5) 0.019(5) 0.000(4) -0.018(4) 0.006(4) C17 0.052(2) 0.0214(16) 0.0372(18) 0.0092(14) 0.0073(16) 0.0120(15) O1W 0.0234(10) 0.0256(11) 0.0225(10) -0.0010(8) -0.0007(8) 0.0034(8) O2W 0.0311(11) 0.0219(10) 0.0246(10) -0.0011(8) -0.0011(8) -0.0005(9) O3W 0.0401(13) 0.0405(14) 0.0353(12) -0.0047(10) 0.0022(10) -0.0123(11) O4W 0.0408(13) 0.0300(12) 0.0373(12) 0.0010(10) 0.0018(10) -0.0115(10) O5W 0.0309(11) 0.0295(11) 0.0259(10) 0.0014(9) -0.0075(9) -0.0075(9) O6W 0.0604(16) 0.0301(12) 0.0374(12) 0.0060(10) -0.0248(12) -0.0005(11) O7W 0.0379(15) 0.0470(17) 0.127(3) -0.0330(18) -0.0177(16) -0.0011(13) O8W 0.0441(16) 0.0439(17) 0.134(3) -0.0318(18) -0.0191(18) 0.0102(13) O9W 0.079(3) 0.114(4) 0.209(5) 0.063(3) -0.074(3) -0.028(2) O10W 0.113(3) 0.095(3) 0.065(2) -0.0183(19) 0.015(2) -0.057(2) O11W 0.049(3) 0.028(3) 0.076(4) -0.006(2) -0.024(3) 0.000(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 Mn1 O11 2.1227(17) . ? Mn1 O2 2.1458(19) . ? Mn1 O4B 2.153(8) . ? Mn1 O3 2.164(2) . ? Mn1 O5 2.196(2) . ? Mn1 O4A 2.200(3) . ? Mn1 O1 2.2459(18) . ? O1 H1O1 0.8906 . ? O1 H2O1 0.8665 . ? O2 H1O2 0.9543 . ? O2 H2O2 0.8781 . ? O3 H1O3 0.8807 . ? O3 H2O3 0.9994 . ? O4A O4B 0.669(10) . ? O4A H1O4 1.0013 . ? O4A H2O4 1.0275 . ? O4B H1O4 1.0381 . ? O4B H2O4 0.9199 . ? O5 H1O5 0.9179 . ? O5 H2O5 0.7462 . ? P1 O13 1.5186(19) . ? P1 O12 1.5326(19) . ? P1 O11 1.5400(18) . ? P1 C8 1.826(3) . ? C8 N1 1.488(3) . ? C8 H81 0.9700 . ? C8 H82 0.9700 . ? N1 C2 1.473(3) . ? N1 C7 1.477(4) 2_756 ? C2 C3 1.513(4) . ? C2 H21 0.9700 . ? C2 H22 0.9700 . ? C3 N4 1.484(3) . ? C3 H31 0.9700 . ? C3 H32 0.9700 . ? N4 C5 1.487(4) . ? N4 H41 0.9000 . ? N4 H42 0.9000 . ? C5 C6 1.513(4) . ? C5 H51 0.9700 . ? C5 H52 0.9700 . ? C6 C7 1.531(4) . ? C6 H61 0.9700 . ? C6 H62 0.9700 . ? C7 N1 1.477(4) 2_756 ? C7 H71 0.9700 . ? C7 H72 0.9700 . ? P2 O23 1.515(2) . ? P2 O21 1.5238(19) . ? P2 O22 1.530(2) . ? P2 C18 1.820(3) . ? C18 N11 1.481(3) . ? C18 H181 0.9700 . ? C18 H182 0.9700 . ? N11 C12 1.472(4) . ? N11 C17 1.476(4) 2_765 ? C12 C13 1.512(8) . ? C12 C13B 1.525(10) . ? C12 H121 0.9700 . ? C12 H122 0.9700 . ? C13 N14 1.473(10) . ? C13 H131 0.9700 . ? C13 H132 0.9700 . ? N14 C15 1.485(8) . ? N14 H141 0.9000 . ? N14 H142 0.9000 . ? C15 C16 1.517(8) . ? C15 H151 0.9700 . ? C15 H152 0.9700 . ? C16 C17 1.625(7) . ? C16 H161 0.9700 . ? C16 H162 0.9700 . ? C13B C14B 1.564(13) . ? C13B H133 0.9700 . ? C13B H134 0.9700 . ? C14B N15B 1.486(13) . ? C14B H143 0.9700 . ? C14B H144 0.9700 . ? N15B C16B 1.487(14) . ? N15B H153 0.9000 . ? N15B H154 0.9000 . ? C16B C17 1.388(10) . ? C16B H163 0.9700 . ? C16B H164 0.9700 . ? C17 N11 1.476(4) 2_765 ? C17 H171 0.9700 . ? C17 H172 0.9700 . ? O1W H1W1 0.9373 . ? O1W H2W1 0.9348 . ? O2W H1W2 0.9246 . ? O2W H2W2 1.0076 . ? O3W H1W3 0.8853 . ? O3W H2W3 0.9210 . ? O4W H1W4 0.9365 . ? O4W H2W4 1.0477 . ? O5W H1W5 0.8888 . ? O5W H2W5 0.9657 . ? O6W H1W6 0.9307 . ? O6W H2W6 0.9997 . ? O7W H1W7 0.8774 . ? O7W H2W7 0.9641 . ? O8W H1W8 0.9549 . ? O8W H2W8 0.8502 . ? O9W H1W9 0.9069 . ? O9W H2W9 0.9340 . ? O10W H10W 0.9735 . ? O10W H10V 0.8499 . ? O11W H11W 1.0440 . ? O11W H11V 0.8173 . ? 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 O11 Mn1 O2 98.99(7) . . ? O11 Mn1 O4B 86.0(2) . . ? O2 Mn1 O4B 167.3(3) . . ? O11 Mn1 O3 88.46(8) . . ? O2 Mn1 O3 83.98(9) . . ? O4B Mn1 O3 108.0(3) . . ? O11 Mn1 O5 94.83(8) . . ? O2 Mn1 O5 85.78(9) . . ? O4B Mn1 O5 82.1(3) . . ? O3 Mn1 O5 169.62(10) . . ? O11 Mn1 O4A 89.38(8) . . ? O2 Mn1 O4A 169.98(9) . . ? O4B Mn1 O4A 17.6(3) . . ? O3 Mn1 O4A 90.80(10) . . ? O5 Mn1 O4A 99.06(11) . . ? O11 Mn1 O1 172.05(7) . . ? O2 Mn1 O1 88.93(7) . . ? O4B Mn1 O1 86.4(2) . . ? O3 Mn1 O1 91.73(7) . . ? O5 Mn1 O1 86.36(8) . . ? O4A Mn1 O1 82.67(8) . . ? Mn1 O1 H1O1 119.2 . . ? Mn1 O1 H2O1 109.6 . . ? H1O1 O1 H2O1 109.2 . . ? Mn1 O2 H1O2 123.4 . . ? Mn1 O2 H2O2 138.5 . . ? H1O2 O2 H2O2 93.8 . . ? Mn1 O3 H1O3 128.2 . . ? Mn1 O3 H2O3 120.5 . . ? H1O3 O3 H2O3 107.4 . . ? O4B O4A Mn1 77.2(8) . . ? O4B O4A H1O4 73.9 . . ? Mn1 O4A H1O4 97.9 . . ? O4B O4A H2O4 61.4 . . ? Mn1 O4A H2O4 126.0 . . ? H1O4 O4A H2O4 101.9 . . ? O4A O4B Mn1 85.1(8) . . ? O4A O4B H1O4 67.9 . . ? Mn1 O4B H1O4 99.5 . . ? O4A O4B H2O4 78.8 . . ? Mn1 O4B H2O4 140.8 . . ? H1O4 O4B H2O4 107.0 . . ? Mn1 O5 H1O5 116.8 . . ? Mn1 O5 H2O5 132.1 . . ? H1O5 O5 H2O5 107.7 . . ? O13 P1 O12 113.95(11) . . ? O13 P1 O11 111.02(10) . . ? O12 P1 O11 111.24(10) . . ? O13 P1 C8 108.63(11) . . ? O12 P1 C8 105.49(11) . . ? O11 P1 C8 106.02(11) . . ? P1 O11 Mn1 136.76(11) . . ? N1 C8 P1 113.80(17) . . ? N1 C8 H81 108.8 . . ? P1 C8 H81 108.8 . . ? N1 C8 H82 108.8 . . ? P1 C8 H82 108.8 . . ? H81 C8 H82 107.7 . . ? C2 N1 C7 109.6(2) . 2_756 ? C2 N1 C8 110.7(2) . . ? C7 N1 C8 111.7(2) 2_756 . ? N1 C2 C3 111.6(2) . . ? N1 C2 H21 109.3 . . ? C3 C2 H21 109.3 . . ? N1 C2 H22 109.3 . . ? C3 C2 H22 109.3 . . ? H21 C2 H22 108.0 . . ? N4 C3 C2 108.8(2) . . ? N4 C3 H31 109.9 . . ? C2 C3 H31 109.9 . . ? N4 C3 H32 109.9 . . ? C2 C3 H32 109.9 . . ? H31 C3 H32 108.3 . . ? C3 N4 C5 115.9(2) . . ? C3 N4 H41 108.3 . . ? C5 N4 H41 108.3 . . ? C3 N4 H42 108.3 . . ? C5 N4 H42 108.3 . . ? H41 N4 H42 107.4 . . ? N4 C5 C6 111.8(2) . . ? N4 C5 H51 109.3 . . ? C6 C5 H51 109.3 . . ? N4 C5 H52 109.3 . . ? C6 C5 H52 109.3 . . ? H51 C5 H52 107.9 . . ? C5 C6 C7 115.2(2) . . ? C5 C6 H61 108.5 . . ? C7 C6 H61 108.5 . . ? C5 C6 H62 108.5 . . ? C7 C6 H62 108.5 . . ? H61 C6 H62 107.5 . . ? N1 C7 C6 113.4(2) 2_756 . ? N1 C7 H71 108.9 2_756 . ? C6 C7 H71 108.9 . . ? N1 C7 H72 108.9 2_756 . ? C6 C7 H72 108.9 . . ? H71 C7 H72 107.7 . . ? O23 P2 O21 112.76(12) . . ? O23 P2 O22 111.63(14) . . ? O21 P2 O22 111.37(11) . . ? O23 P2 C18 106.94(12) . . ? O21 P2 C18 106.15(11) . . ? O22 P2 C18 107.60(12) . . ? N11 C18 P2 112.26(18) . . ? N11 C18 H181 109.2 . . ? P2 C18 H181 109.2 . . ? N11 C18 H182 109.2 . . ? P2 C18 H182 109.2 . . ? H181 C18 H182 107.9 . . ? C12 N11 C17 109.7(2) . 2_765 ? C12 N11 C18 111.1(2) . . ? C17 N11 C18 111.5(2) 2_765 . ? N11 C12 C13 109.0(4) . . ? N11 C12 C13B 119.0(7) . . ? C13 C12 C13B 20.0(5) . . ? N11 C12 H121 109.9 . . ? C13 C12 H121 109.9 . . ? C13B C12 H121 89.9 . . ? N11 C12 H122 109.9 . . ? C13 C12 H122 109.9 . . ? C13B C12 H122 117.4 . . ? H121 C12 H122 108.3 . . ? N14 C13 C12 109.9(6) . . ? N14 C13 H131 109.7 . . ? C12 C13 H131 109.7 . . ? N14 C13 H132 109.7 . . ? C12 C13 H132 109.7 . . ? H131 C13 H132 108.2 . . ? C13 N14 C15 114.0(6) . . ? C13 N14 H141 108.7 . . ? C15 N14 H141 108.7 . . ? C13 N14 H142 108.7 . . ? C15 N14 H142 108.7 . . ? H141 N14 H142 107.6 . . ? N14 C15 C16 110.9(5) . . ? N14 C15 H151 109.5 . . ? C16 C15 H151 109.5 . . ? N14 C15 H152 109.5 . . ? C16 C15 H152 109.5 . . ? H151 C15 H152 108.0 . . ? C15 C16 C17 113.2(5) . . ? C15 C16 H161 108.9 . . ? C17 C16 H161 108.9 . . ? C15 C16 H162 108.9 . . ? C17 C16 H162 108.9 . . ? H161 C16 H162 107.7 . . ? C12 C13B C14B 117.9(8) . . ? C12 C13B H133 107.8 . . ? C14B C13B H133 107.8 . . ? C12 C13B H134 107.8 . . ? C14B C13B H134 107.8 . . ? H133 C13B H134 107.2 . . ? N15B C14B C13B 106.8(8) . . ? N15B C14B H143 110.4 . . ? C13B C14B H143 110.4 . . ? N15B C14B H144 110.4 . . ? C13B C14B H144 110.4 . . ? H143 C14B H144 108.6 . . ? C14B N15B C16B 116.7(9) . . ? C14B N15B H153 108.1 . . ? C16B N15B H153 108.1 . . ? C14B N15B H154 108.1 . . ? C16B N15B H154 108.1 . . ? H153 N15B H154 107.3 . . ? C17 C16B N15B 118.0(8) . . ? C17 C16B H163 107.8 . . ? N15B C16B H163 107.8 . . ? C17 C16B H164 107.8 . . ? N15B C16B H164 107.8 . . ? H163 C16B H164 107.1 . . ? C16B C17 N11 104.4(4) . 2_765 ? C16B C17 C16 23.2(3) . . ? N11 C17 C16 117.1(3) 2_765 . ? C16B C17 H171 131.2 . . ? N11 C17 H171 108.0 2_765 . ? C16 C17 H171 108.0 . . ? C16B C17 H172 95.9 . . ? N11 C17 H172 108.0 2_765 . ? C16 C17 H172 108.0 . . ? H171 C17 H172 107.3 . . ? H1W1 O1W H2W1 105.3 . . ? H1W2 O2W H2W2 108.7 . . ? H1W3 O3W H2W3 98.2 . . ? H1W4 O4W H2W4 102.2 . . ? H1W5 O5W H2W5 102.9 . . ? H1W6 O6W H2W6 109.2 . . ? H1W7 O7W H2W7 102.3 . . ? H1W8 O8W H2W8 126.0 . . ? H1W9 O9W H2W9 119.4 . . ? H10W O10W H10V 137.0 . . ? H11W O11W H11V 115.6 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.983 _refine_diff_density_min -0.903 _refine_diff_density_rms 0.081 #===END data_pbdip _database_code_depnum_ccdc_archive 'CCDC 600827' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H32 N4 O8 P2 Pb, (H2 O)6' _chemical_formula_sum 'C12 H44 N4 O14 P2 Pb' _chemical_formula_weight 737.64 _chemical_compound_source 'synthesized by the authors' 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' Pb Pb -3.3944 10.1111 '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 10.029(1) _cell_length_b 10.416(1) _cell_length_c 14.322(1) _cell_angle_alpha 77.055(2) _cell_angle_beta 73.698(2) _cell_angle_gamma 71.776(2) _cell_volume 1348.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prisma _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.817 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 6.444 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.337 _exptl_absorpt_correction_T_max 0.762 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _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 area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23473 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.43 _reflns_number_total 6088 _reflns_number_gt 5864 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+19.8700P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0035(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6088 _refine_ls_number_parameters 303 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1033 _refine_ls_wR_factor_gt 0.1022 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.159 _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 Pb Pb 0.07412(3) 0.57533(2) 0.083053(18) 0.01930(10) Uani 1 1 d . . . O1C O 0.1877(7) 0.6762(7) -0.1283(5) 0.0484(17) Uani 1 1 d . . . H1C1 H 0.2269 0.6990 -0.1790 0.063 Uiso 1 1 d R . . H2C1 H 0.1033 0.6967 -0.1248 0.063 Uiso 1 1 d R . . O2C O 0.3095(6) 0.4378(5) 0.1284(4) 0.0312(12) Uani 1 1 d . . . H1C2 H 0.3530 0.4747 0.1372 0.041 Uiso 1 1 d R . . H2C2 H 0.3551 0.3836 0.0873 0.041 Uiso 1 1 d R . . P1A P -0.0414(2) 0.44783(17) 0.30783(13) 0.0209(4) Uani 1 1 d . . . O11A O -0.0279(6) 0.4297(5) 0.2006(3) 0.0236(10) Uani 1 1 d . . . O12A O -0.1915(6) 0.4482(6) 0.3711(4) 0.0300(12) Uani 1 1 d . . . O13A O 0.0046(6) 0.5714(5) 0.3088(4) 0.0298(12) Uani 1 1 d . . . C8A C 0.0883(8) 0.2974(7) 0.3541(5) 0.0257(15) Uani 1 1 d . . . H8A1 H 0.0578 0.2165 0.3574 0.031 Uiso 1 1 calc R . . H8A2 H 0.1815 0.2888 0.3084 0.031 Uiso 1 1 calc R . . N1A N 0.1032(7) 0.3042(6) 0.4530(4) 0.0242(12) Uani 1 1 d . . . C2A C 0.2513(8) 0.3077(9) 0.4488(6) 0.0343(18) Uani 1 1 d . . . H2A1 H 0.3197 0.2315 0.4180 0.041 Uiso 1 1 calc R . . H2A2 H 0.2632 0.2962 0.5153 0.041 Uiso 1 1 calc R . . C3A C 0.2855(9) 0.4378(9) 0.3929(6) 0.0343(18) Uani 1 1 d . . . H3A1 H 0.3823 0.4358 0.3941 0.041 Uiso 1 1 calc R . . H3A2 H 0.2808 0.4473 0.3249 0.041 Uiso 1 1 calc R . . N4A N 0.1798(7) 0.5554(7) 0.4386(4) 0.0285(13) Uani 1 1 d . . . H4A1 H 0.0905 0.5517 0.4406 0.037 Uiso 1 1 calc R . . H4A2 H 0.1873 0.5452 0.5012 0.037 Uiso 1 1 calc R . . C5A C 0.1943(10) 0.6930(9) 0.3895(6) 0.040(2) Uani 1 1 d . . . H5A1 H 0.1727 0.7109 0.3251 0.048 Uiso 1 1 calc R . . H5A2 H 0.2931 0.6957 0.3801 0.048 Uiso 1 1 calc R . . C6A C 0.0934(11) 0.8036(9) 0.4497(6) 0.041(2) Uani 1 1 d . . . H6A1 H 0.1228 0.7896 0.5110 0.049 Uiso 1 1 calc R . . H6A2 H 0.1058 0.8915 0.4140 0.049 Uiso 1 1 calc R . . C7A C -0.0653(10) 0.8102(7) 0.4737(6) 0.0349(19) Uani 1 1 d . . . H7A1 H -0.1206 0.8954 0.4982 0.042 Uiso 1 1 calc R . . H7A2 H -0.0924 0.8107 0.4137 0.042 Uiso 1 1 calc R . . P1B P 0.24819(19) 0.26206(16) -0.01579(12) 0.0175(3) Uani 1 1 d . . . O11B O 0.1280(5) 0.3979(4) -0.0058(3) 0.0204(10) Uani 1 1 d . . . O12B O 0.3909(5) 0.2720(5) -0.0064(4) 0.0223(10) Uani 1 1 d . . . O13B O 0.2602(6) 0.2126(5) -0.1110(4) 0.0245(10) Uani 1 1 d . . . C8B C 0.1844(7) 0.1421(7) 0.0880(5) 0.0225(14) Uani 1 1 d . . . H8B1 H 0.1642 0.1794 0.1483 0.027 Uiso 1 1 calc R . . H8B2 H 0.0950 0.1312 0.0814 0.027 Uiso 1 1 calc R . . N1B N 0.2913(6) 0.0053(5) 0.0951(4) 0.0221(12) Uani 1 1 d . . . C2B C 0.3368(8) -0.0266(7) 0.1889(5) 0.0265(15) Uani 1 1 d . . . H2B1 H 0.3917 -0.1216 0.1978 0.032 Uiso 1 1 calc R . . H2B2 H 0.2521 -0.0144 0.2427 0.032 Uiso 1 1 calc R . . C3B C 0.4273(8) 0.0626(7) 0.1926(5) 0.0269(15) Uani 1 1 d . . . H3B1 H 0.4590 0.0359 0.2538 0.032 Uiso 1 1 calc R . . H3B2 H 0.3707 0.1573 0.1893 0.032 Uiso 1 1 calc R . . N4B N 0.5563(6) 0.0472(6) 0.1066(5) 0.0242(13) Uani 1 1 d . . . H4B1 H 0.6061 -0.0415 0.1106 0.031 Uiso 1 1 calc R . . H4B2 H 0.5243 0.0696 0.0508 0.031 Uiso 1 1 calc R . . C5B C 0.6563(8) 0.1292(7) 0.0984(6) 0.0284(16) Uani 1 1 d . . . H5B1 H 0.6829 0.1147 0.1608 0.034 Uiso 1 1 calc R . . H5B2 H 0.6086 0.2254 0.0835 0.034 Uiso 1 1 calc R . . C6B C 0.7907(9) 0.0901(7) 0.0186(6) 0.0290(16) Uani 1 1 d . . . H6B1 H 0.8417 -0.0038 0.0380 0.035 Uiso 1 1 calc R . . H6B2 H 0.8527 0.1470 0.0152 0.035 Uiso 1 1 calc R . . C7B C 0.7670(9) 0.1029(7) -0.0850(6) 0.0299(16) Uani 1 1 d . . . H7B1 H 0.7010 0.1911 -0.1001 0.036 Uiso 1 1 calc R . . H7B2 H 0.8581 0.0995 -0.1325 0.036 Uiso 1 1 calc R . . O1W O 0.1008(8) 0.1706(6) 0.7749(5) 0.054(2) Uani 1 1 d . . . H1W1 H 0.1518 0.1712 0.8118 0.070 Uiso 1 1 d R . . H2W1 H 0.0770 0.2571 0.7409 0.070 Uiso 1 1 d R . . O2W O 0.5989(8) 0.6511(10) 0.2928(6) 0.080(3) Uani 1 1 d . . . H1W2 H 0.6631 0.5890 0.3174 0.105 Uiso 1 1 d R . . H2W2 H 0.6483 0.7085 0.2292 0.105 Uiso 1 1 d R . . O3W O 0.5324(12) 0.1320(11) 0.5904(6) 0.095(3) Uani 1 1 d . . . H1W3 H 0.4944 0.1959 0.6254 0.124 Uiso 1 1 d R . . H2W3 H 0.4900 0.0664 0.6101 0.124 Uiso 1 1 d R . . O4W O 0.5096(8) 0.5410(8) 0.1557(5) 0.055(2) Uani 1 1 d . . . H1W4 H 0.5423 0.5513 0.1988 0.071 Uiso 1 1 d R . . H2W4 H 0.5478 0.6069 0.1014 0.071 Uiso 1 1 d R . . O5WA O 0.6348(13) 0.2609(12) 0.4005(9) 0.021(2) Uiso 0.40 1 d P . . O5WB O 0.381(2) 0.903(2) 0.6023(17) 0.047(5) Uiso 0.30 1 d P . . O5WC O 0.624(2) 0.372(2) 0.3035(16) 0.047(5) Uiso 0.30 1 d P . . O6WA O 0.8853(13) 0.0666(12) 0.2817(9) 0.039(3) Uiso 0.50 1 d P . . O6WB O 0.6642(19) 0.0135(17) 0.3453(13) 0.068(4) Uiso 0.50 1 d P . . 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 Pb 0.02718(15) 0.01330(13) 0.02051(14) -0.00433(8) -0.01163(10) -0.00294(9) O1C 0.055(4) 0.054(4) 0.051(4) -0.025(3) 0.003(3) -0.037(3) O2C 0.031(3) 0.033(3) 0.036(3) -0.015(2) -0.015(2) -0.003(2) P1A 0.0308(9) 0.0179(8) 0.0173(8) -0.0030(6) -0.0145(7) -0.0028(7) O11A 0.033(3) 0.025(2) 0.015(2) -0.0027(18) -0.012(2) -0.006(2) O12A 0.031(3) 0.036(3) 0.022(3) -0.007(2) -0.010(2) -0.002(2) O13A 0.041(3) 0.020(2) 0.035(3) -0.004(2) -0.022(2) -0.005(2) C8A 0.036(4) 0.023(3) 0.019(3) -0.007(3) -0.013(3) 0.001(3) N1A 0.036(3) 0.021(3) 0.018(3) -0.003(2) -0.015(2) -0.002(2) C2A 0.028(4) 0.043(5) 0.032(4) -0.011(3) -0.018(3) 0.005(3) C3A 0.027(4) 0.050(5) 0.029(4) -0.015(4) -0.006(3) -0.008(4) N4A 0.030(3) 0.041(4) 0.021(3) -0.008(3) -0.008(3) -0.015(3) C5A 0.054(5) 0.054(5) 0.026(4) -0.006(4) -0.007(4) -0.037(5) C6A 0.077(7) 0.033(4) 0.025(4) 0.002(3) -0.016(4) -0.032(4) C7A 0.065(6) 0.020(3) 0.023(4) 0.001(3) -0.023(4) -0.007(4) P1B 0.0223(8) 0.0107(7) 0.0199(8) -0.0042(6) -0.0106(6) 0.0014(6) O11B 0.027(2) 0.011(2) 0.025(2) -0.0051(17) -0.013(2) 0.0004(18) O12B 0.024(2) 0.020(2) 0.025(2) -0.0022(19) -0.014(2) -0.0008(19) O13B 0.035(3) 0.015(2) 0.024(2) -0.0065(19) -0.013(2) 0.001(2) C8B 0.022(3) 0.018(3) 0.026(3) -0.005(3) -0.008(3) 0.001(3) N1B 0.027(3) 0.013(2) 0.023(3) -0.002(2) -0.009(2) 0.002(2) C2B 0.031(4) 0.022(3) 0.021(3) 0.002(3) -0.009(3) 0.000(3) C3B 0.030(4) 0.023(3) 0.023(3) -0.006(3) -0.010(3) 0.004(3) N4B 0.027(3) 0.020(3) 0.030(3) -0.010(2) -0.016(3) 0.001(2) C5B 0.033(4) 0.019(3) 0.039(4) -0.009(3) -0.019(3) -0.001(3) C6B 0.037(4) 0.014(3) 0.038(4) -0.004(3) -0.014(3) -0.006(3) C7B 0.033(4) 0.016(3) 0.036(4) -0.003(3) -0.006(3) -0.003(3) O1W 0.085(5) 0.028(3) 0.066(5) 0.007(3) -0.057(4) -0.014(3) O2W 0.035(4) 0.107(7) 0.061(5) 0.031(5) -0.012(4) 0.003(4) O3W 0.107(8) 0.114(8) 0.043(5) 0.008(5) -0.030(5) -0.004(6) O4W 0.082(5) 0.075(5) 0.033(3) 0.007(3) -0.022(3) -0.058(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 Pb O11A 2.245(5) . ? Pb O11B 2.318(4) . ? Pb O11B 2.485(5) 2_565 ? Pb O2C 2.525(5) . ? O1C H1C1 0.7484 . ? O1C H2C1 0.7955 . ? O2C H1C2 0.7145 . ? O2C H2C2 0.8426 . ? P1A O13A 1.501(5) . ? P1A O12A 1.523(6) . ? P1A O11A 1.552(5) . ? P1A C8A 1.825(7) . ? C8A N1A 1.484(8) . ? C8A H8A1 0.9700 . ? C8A H8A2 0.9700 . ? N1A C7A 1.472(10) 2_566 ? N1A C2A 1.482(10) . ? C2A C3A 1.498(12) . ? C2A H2A1 0.9700 . ? C2A H2A2 0.9700 . ? C3A N4A 1.487(10) . ? C3A H3A1 0.9700 . ? C3A H3A2 0.9700 . ? N4A C5A 1.481(10) . ? N4A H4A1 0.9000 . ? N4A H4A2 0.9000 . ? C5A C6A 1.523(13) . ? C5A H5A1 0.9700 . ? C5A H5A2 0.9700 . ? C6A C7A 1.513(13) . ? C6A H6A1 0.9700 . ? C6A H6A2 0.9700 . ? C7A N1A 1.472(10) 2_566 ? C7A H7A1 0.9700 . ? C7A H7A2 0.9700 . ? P1B O12B 1.511(5) . ? P1B O13B 1.523(5) . ? P1B O11B 1.550(5) . ? P1B C8B 1.821(7) . ? O11B Pb 2.485(5) 2_565 ? C8B N1B 1.493(8) . ? C8B H8B1 0.9700 . ? C8B H8B2 0.9700 . ? N1B C7B 1.472(9) 2_655 ? N1B C2B 1.474(9) . ? C2B C3B 1.504(11) . ? C2B H2B1 0.9700 . ? C2B H2B2 0.9700 . ? C3B N4B 1.511(10) . ? C3B H3B1 0.9700 . ? C3B H3B2 0.9700 . ? N4B C5B 1.475(9) . ? N4B H4B1 0.9000 . ? N4B H4B2 0.9000 . ? C5B C6B 1.513(11) . ? C5B H5B1 0.9700 . ? C5B H5B2 0.9700 . ? C6B C7B 1.538(11) . ? C6B H6B1 0.9700 . ? C6B H6B2 0.9700 . ? C7B N1B 1.472(9) 2_655 ? C7B H7B1 0.9700 . ? C7B H7B2 0.9700 . ? O1W H1W1 0.8345 . ? O1W H2W1 0.9163 . ? O2W H1W2 0.8500 . ? O2W H2W2 1.0580 . ? O3W H1W3 0.8504 . ? O3W H2W3 0.8687 . ? O4W H1W4 0.8149 . ? O4W H2W4 0.9900 . ? O5WA O5WC 1.60(2) . ? O5WA O5WB 1.77(3) 2_666 ? O5WB O6WB 1.18(3) 2_666 ? O5WB O5WA 1.77(3) 2_666 ? O6WB O5WB 1.18(3) 2_666 ? 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 O11A Pb O11B 81.18(17) . . ? O11A Pb O11B 84.84(16) . 2_565 ? O11B Pb O11B 70.20(17) . 2_565 ? O11A Pb O2C 86.40(18) . . ? O11B Pb O2C 81.32(16) . . ? O11B Pb O2C 151.15(15) 2_565 . ? H1C1 O1C H2C1 110.6 . . ? Pb O2C H1C2 117.3 . . ? Pb O2C H2C2 108.7 . . ? H1C2 O2C H2C2 113.2 . . ? O13A P1A O12A 113.4(3) . . ? O13A P1A O11A 110.5(3) . . ? O12A P1A O11A 111.5(3) . . ? O13A P1A C8A 107.7(3) . . ? O12A P1A C8A 108.7(3) . . ? O11A P1A C8A 104.6(3) . . ? P1A O11A Pb 115.3(3) . . ? N1A C8A P1A 112.5(5) . . ? N1A C8A H8A1 109.1 . . ? P1A C8A H8A1 109.1 . . ? N1A C8A H8A2 109.1 . . ? P1A C8A H8A2 109.1 . . ? H8A1 C8A H8A2 107.8 . . ? C7A N1A C2A 110.4(6) 2_566 . ? C7A N1A C8A 111.8(6) 2_566 . ? C2A N1A C8A 110.6(6) . . ? N1A C2A C3A 113.2(6) . . ? N1A C2A H2A1 108.9 . . ? C3A C2A H2A1 108.9 . . ? N1A C2A H2A2 108.9 . . ? C3A C2A H2A2 108.9 . . ? H2A1 C2A H2A2 107.7 . . ? N4A C3A C2A 109.3(7) . . ? N4A C3A H3A1 109.8 . . ? C2A C3A H3A1 109.8 . . ? N4A C3A H3A2 109.8 . . ? C2A C3A H3A2 109.8 . . ? H3A1 C3A H3A2 108.3 . . ? C5A N4A C3A 116.3(7) . . ? C5A N4A H4A1 108.2 . . ? C3A N4A H4A1 108.2 . . ? C5A N4A H4A2 108.2 . . ? C3A N4A H4A2 108.2 . . ? H4A1 N4A H4A2 107.4 . . ? N4A C5A C6A 111.5(7) . . ? N4A C5A H5A1 109.3 . . ? C6A C5A H5A1 109.3 . . ? N4A C5A H5A2 109.3 . . ? C6A C5A H5A2 109.3 . . ? H5A1 C5A H5A2 108.0 . . ? C7A C6A C5A 116.0(7) . . ? C7A C6A H6A1 108.3 . . ? C5A C6A H6A1 108.3 . . ? C7A C6A H6A2 108.3 . . ? C5A C6A H6A2 108.3 . . ? H6A1 C6A H6A2 107.4 . . ? N1A C7A C6A 113.5(6) 2_566 . ? N1A C7A H7A1 108.9 2_566 . ? C6A C7A H7A1 108.9 . . ? N1A C7A H7A2 108.9 2_566 . ? C6A C7A H7A2 108.9 . . ? H7A1 C7A H7A2 107.7 . . ? O12B P1B O13B 112.5(3) . . ? O12B P1B O11B 112.8(3) . . ? O13B P1B O11B 109.9(3) . . ? O12B P1B C8B 108.1(3) . . ? O13B P1B C8B 108.9(3) . . ? O11B P1B C8B 104.2(3) . . ? P1B O11B Pb 134.6(3) . . ? P1B O11B Pb 115.0(2) . 2_565 ? Pb O11B Pb 109.80(17) . 2_565 ? N1B C8B P1B 112.4(5) . . ? N1B C8B H8B1 109.1 . . ? P1B C8B H8B1 109.1 . . ? N1B C8B H8B2 109.1 . . ? P1B C8B H8B2 109.1 . . ? H8B1 C8B H8B2 107.8 . . ? C7B N1B C2B 110.4(6) 2_655 . ? C7B N1B C8B 111.5(6) 2_655 . ? C2B N1B C8B 110.4(5) . . ? N1B C2B C3B 112.2(6) . . ? N1B C2B H2B1 109.2 . . ? C3B C2B H2B1 109.2 . . ? N1B C2B H2B2 109.2 . . ? C3B C2B H2B2 109.2 . . ? H2B1 C2B H2B2 107.9 . . ? C2B C3B N4B 108.9(6) . . ? C2B C3B H3B1 109.9 . . ? N4B C3B H3B1 109.9 . . ? C2B C3B H3B2 109.9 . . ? N4B C3B H3B2 109.9 . . ? H3B1 C3B H3B2 108.3 . . ? C5B N4B C3B 116.1(6) . . ? C5B N4B H4B1 108.3 . . ? C3B N4B H4B1 108.3 . . ? C5B N4B H4B2 108.3 . . ? C3B N4B H4B2 108.3 . . ? H4B1 N4B H4B2 107.4 . . ? N4B C5B C6B 110.9(6) . . ? N4B C5B H5B1 109.5 . . ? C6B C5B H5B1 109.5 . . ? N4B C5B H5B2 109.5 . . ? C6B C5B H5B2 109.5 . . ? H5B1 C5B H5B2 108.1 . . ? C5B C6B C7B 116.1(6) . . ? C5B C6B H6B1 108.3 . . ? C7B C6B H6B1 108.3 . . ? C5B C6B H6B2 108.3 . . ? C7B C6B H6B2 108.3 . . ? H6B1 C6B H6B2 107.4 . . ? N1B C7B C6B 113.1(6) 2_655 . ? N1B C7B H7B1 109.0 2_655 . ? C6B C7B H7B1 109.0 . . ? N1B C7B H7B2 109.0 2_655 . ? C6B C7B H7B2 109.0 . . ? H7B1 C7B H7B2 107.8 . . ? H1W1 O1W H2W1 107.5 . . ? H1W2 O2W H2W2 109.8 . . ? H1W3 O3W H2W3 112.5 . . ? H1W4 O4W H2W4 99.0 . . ? O5WC O5WA O5WB 117.7(13) . 2_666 ? O6WB O5WB O5WA 139(2) 2_666 2_666 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 6.576 _refine_diff_density_min -3.228 _refine_diff_density_rms 0.191 #===END data_zndip _database_code_depnum_ccdc_archive 'CCDC 600828' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H28 N4 O6 P2 Zn' _chemical_formula_sum 'C12 H28 N4 O6 P2 Zn' _chemical_formula_weight 451.69 _chemical_compound_source 'synthesized by the authors' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4638(7) _cell_length_b 9.5509(6) _cell_length_c 11.1074(8) _cell_angle_alpha 89.068(4) _cell_angle_beta 88.094(3) _cell_angle_gamma 60.882(3) _cell_volume 876.61(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3540 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.711 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 1.622 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6406 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0526 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.53 _reflns_number_total 3913 _reflns_number_gt 2973 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0686P)^2^+1.3136P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3913 _refine_ls_number_parameters 269 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0748 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1424 _refine_ls_wR_factor_gt 0.1284 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 Zn1A Zn 0.0000 0.5000 0.5000 0.03081(18) Uani 1 2 d S . . N1A N 0.2526(4) 0.3537(4) 0.5325(3) 0.0370(8) Uani 1 1 d . . . C2A C 0.2550(6) 0.2215(6) 0.6066(4) 0.0483(11) Uani 1 1 d . . . H2A1 H 0.2161 0.2599 0.6878 0.055(15) Uiso 1 1 calc R . . H2A2 H 0.3654 0.1346 0.6110 0.049(14) Uiso 1 1 calc R . . C3A C 0.1492(7) 0.1586(6) 0.5531(5) 0.0527(12) Uani 1 1 d . . . H3A1 H 0.1928 0.1120 0.4745 0.045(13) Uiso 1 1 calc R . . H3A2 H 0.1491 0.0758 0.6048 0.071(18) Uiso 1 1 calc R . . N4A N -0.0204(5) 0.2935(5) 0.5416(4) 0.0441(9) Uani 1 1 d . . . H4A1 H -0.071(6) 0.307(6) 0.616(5) 0.042(13) Uiso 1 1 d . . . C5A C -0.1168(7) 0.2603(6) 0.4585(5) 0.0530(12) Uani 1 1 d . . . H5A1 H -0.1209 0.1649 0.4846 0.08(2) Uiso 1 1 calc R . . H5A2 H -0.0660 0.2401 0.3787 0.09(2) Uiso 1 1 calc R . . C6A C -0.2856(7) 0.3984(7) 0.4530(5) 0.0557(13) Uani 1 1 d . . . H6A1 H -0.3300 0.4222 0.5347 0.08(2) Uiso 1 1 calc R . . H6A2 H -0.3496 0.3627 0.4096 0.075(19) Uiso 1 1 calc R . . C7A C -0.3110(6) 0.5547(6) 0.3956(4) 0.0457(11) Uani 1 1 d . . . H7A1 H -0.2558 0.5307 0.3174 0.053(15) Uiso 1 1 calc R . . H7A2 H -0.4256 0.6225 0.3826 0.060(16) Uiso 1 1 calc R . . C8A C 0.3486(5) 0.2927(6) 0.4175(4) 0.0436(10) Uani 1 1 d . . . H8A1 H 0.4281 0.1809 0.4284 0.075(19) Uiso 1 1 calc R . . H8A2 H 0.4071 0.3512 0.4014 0.066(17) Uiso 1 1 calc R . . P1A P 0.23059(14) 0.30912(13) 0.28509(10) 0.0365(3) Uani 1 1 d . . . O11A O 0.0600(4) 0.4319(4) 0.3150(3) 0.0473(8) Uani 1 1 d . . . O12A O 0.3070(4) 0.3676(4) 0.1822(3) 0.0450(8) Uani 1 1 d . . . H12A H 0.301(8) 0.464(9) 0.194(6) 0.08(2) Uiso 1 1 d . . . O13A O 0.2574(5) 0.1485(4) 0.2473(3) 0.0587(10) Uani 1 1 d . . . Zn1B Zn 0.0000 1.0000 0.0000 0.03258(19) Uani 1 2 d S . . N1B N 0.2527(4) 0.8608(5) -0.0493(3) 0.0391(8) Uani 1 1 d . . . C2B C 0.2523(6) 0.7344(6) -0.1257(5) 0.0498(11) Uani 1 1 d . . . H2B1 H 0.3626 0.6493 -0.1395 0.060(16) Uiso 1 1 calc R . . H2B2 H 0.2078 0.7797 -0.2033 0.043(13) Uiso 1 1 calc R . . C3B C 0.1526(6) 0.6650(6) -0.0661(5) 0.0501(11) Uani 1 1 d . . . H3B1 H 0.1532 0.5838 -0.1177 0.078(19) Uiso 1 1 calc R . . H3B2 H 0.1997 0.6150 0.0097 0.050(14) Uiso 1 1 calc R . . N4B N -0.0146(5) 0.7936(4) -0.0445(4) 0.0404(8) Uani 1 1 d . . . H4B1 H -0.066(7) 0.813(7) -0.115(5) 0.053(15) Uiso 1 1 d . . . C5B C -0.1077(6) 0.7517(6) 0.0444(5) 0.0482(11) Uani 1 1 d . . . H5B1 H -0.0546 0.7277 0.1211 0.046(14) Uiso 1 1 calc R . . H5B2 H -0.1093 0.6563 0.0177 0.055(15) Uiso 1 1 calc R . . C6B C -0.2802(6) 0.8868(7) 0.0613(5) 0.0503(12) Uani 1 1 d . . . H6B1 H -0.3405 0.8457 0.1082 0.057(15) Uiso 1 1 calc R . . H6B2 H -0.3280 0.9156 -0.0174 0.042(13) Uiso 1 1 calc R . . C7B C -0.3050(6) 1.0400(6) 0.1223(4) 0.0461(11) Uani 1 1 d . . . H7B1 H -0.4189 1.1051 0.1436 0.063(16) Uiso 1 1 calc R . . H7B2 H -0.2461 1.0106 0.1966 0.051(14) Uiso 1 1 calc R . . C8B C 0.3553(6) 0.7913(7) 0.0576(5) 0.0514(12) Uani 1 1 d . . . H8B1 H 0.4155 0.8479 0.0692 0.09(2) Uiso 1 1 calc R . . H8B2 H 0.4332 0.6803 0.0402 0.09(2) Uiso 1 1 calc R . . P1B P 0.24664(15) 0.79827(13) 0.19868(11) 0.0402(3) Uani 1 1 d . . . O11B O 0.0717(4) 0.9136(4) 0.1803(3) 0.0469(8) Uani 1 1 d . . . O12B O 0.3193(5) 0.8622(4) 0.2953(4) 0.0529(10) Uani 1 1 d . . . H12B H 0.337(10) 0.917(10) 0.272(7) 0.09(3) Uiso 1 1 d . . . O13B O 0.2897(6) 0.6331(4) 0.2390(3) 0.0639(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1A 0.0288(3) 0.0275(3) 0.0367(4) -0.0008(2) 0.0004(3) -0.0143(3) N1A 0.0306(18) 0.0399(19) 0.0376(19) -0.0009(15) 0.0004(14) -0.0148(15) C2A 0.050(3) 0.043(3) 0.047(3) 0.011(2) -0.010(2) -0.018(2) C3A 0.071(4) 0.032(2) 0.054(3) 0.005(2) 0.001(2) -0.024(2) N4A 0.044(2) 0.036(2) 0.056(2) -0.0057(17) 0.0114(18) -0.0231(18) C5A 0.060(3) 0.049(3) 0.063(3) -0.013(2) 0.004(3) -0.036(3) C6A 0.052(3) 0.063(3) 0.064(3) -0.018(3) 0.014(2) -0.037(3) C7A 0.033(2) 0.058(3) 0.047(3) -0.005(2) -0.0030(19) -0.023(2) C8A 0.032(2) 0.048(3) 0.046(3) -0.011(2) 0.0060(19) -0.017(2) P1A 0.0421(6) 0.0351(6) 0.0374(6) -0.0063(4) 0.0060(4) -0.0231(5) O11A 0.0393(17) 0.063(2) 0.0384(16) -0.0074(14) 0.0030(13) -0.0239(16) O12A 0.054(2) 0.0331(16) 0.0489(18) -0.0037(13) 0.0140(15) -0.0228(15) O13A 0.098(3) 0.046(2) 0.050(2) -0.0050(15) 0.0015(19) -0.049(2) Zn1B 0.0325(4) 0.0298(3) 0.0373(4) 0.0029(3) -0.0044(3) -0.0166(3) N1B 0.0355(19) 0.041(2) 0.0391(19) 0.0026(15) -0.0031(15) -0.0167(16) C2B 0.046(3) 0.041(3) 0.053(3) -0.009(2) 0.006(2) -0.014(2) C3B 0.054(3) 0.036(2) 0.057(3) -0.005(2) -0.003(2) -0.019(2) N4B 0.044(2) 0.0355(19) 0.046(2) 0.0030(16) -0.0085(17) -0.0222(17) C5B 0.058(3) 0.043(2) 0.057(3) 0.012(2) -0.011(2) -0.034(2) C6B 0.050(3) 0.063(3) 0.053(3) 0.013(2) -0.007(2) -0.039(3) C7B 0.038(2) 0.055(3) 0.047(3) 0.008(2) 0.000(2) -0.024(2) C8B 0.035(2) 0.053(3) 0.060(3) 0.020(2) -0.013(2) -0.017(2) P1B 0.0510(7) 0.0330(6) 0.0449(6) 0.0110(5) -0.0169(5) -0.0263(5) O11B 0.0464(19) 0.060(2) 0.0398(17) 0.0098(14) -0.0081(14) -0.0304(17) O12B 0.061(2) 0.0376(18) 0.064(2) 0.0074(16) -0.0264(18) -0.0260(18) O13B 0.108(3) 0.0419(19) 0.059(2) 0.0149(16) -0.022(2) -0.049(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 Zn1A N4A 2.116(4) 2_566 ? Zn1A N4A 2.116(4) . ? Zn1A O11A 2.138(3) . ? Zn1A O11A 2.138(3) 2_566 ? Zn1A N1A 2.142(4) 2_566 ? Zn1A N1A 2.142(4) . ? N1A C2A 1.487(6) . ? N1A C8A 1.493(6) . ? N1A C7A 1.494(6) 2_566 ? C2A C3A 1.535(7) . ? C2A H2A1 0.9700 . ? C2A H2A2 0.9700 . ? C3A N4A 1.499(7) . ? C3A H3A1 0.9700 . ? C3A H3A2 0.9700 . ? N4A C5A 1.461(6) . ? N4A H4A1 0.93(5) . ? C5A C6A 1.499(8) . ? C5A H5A1 0.9700 . ? C5A H5A2 0.9700 . ? C6A C7A 1.523(7) . ? C6A H6A1 0.9700 . ? C6A H6A2 0.9700 . ? C7A N1A 1.494(6) 2_566 ? C7A H7A1 0.9700 . ? C7A H7A2 0.9700 . ? C8A P1A 1.835(5) . ? C8A H8A1 0.9700 . ? C8A H8A2 0.9700 . ? P1A O11A 1.492(3) . ? P1A O13A 1.493(3) . ? P1A O12A 1.568(3) . ? O12A H12A 0.91(7) . ? Zn1B N4B 2.110(4) . ? Zn1B N4B 2.110(4) 2_575 ? Zn1B N1B 2.152(4) . ? Zn1B N1B 2.152(4) 2_575 ? Zn1B O11B 2.155(3) 2_575 ? Zn1B O11B 2.155(3) . ? N1B C7B 1.485(6) 2_575 ? N1B C8B 1.489(6) . ? N1B C2B 1.489(6) . ? C2B C3B 1.523(7) . ? C2B H2B1 0.9700 . ? C2B H2B2 0.9700 . ? C3B N4B 1.471(6) . ? C3B H3B1 0.9700 . ? C3B H3B2 0.9700 . ? N4B C5B 1.478(6) . ? N4B H4B1 0.91(6) . ? C5B C6B 1.517(7) . ? C5B H5B1 0.9700 . ? C5B H5B2 0.9700 . ? C6B C7B 1.531(7) . ? C6B H6B1 0.9700 . ? C6B H6B2 0.9700 . ? C7B N1B 1.485(6) 2_575 ? C7B H7B1 0.9700 . ? C7B H7B2 0.9700 . ? C8B P1B 1.830(5) . ? C8B H8B1 0.9700 . ? C8B H8B2 0.9700 . ? P1B O13B 1.490(3) . ? P1B O11B 1.495(4) . ? P1B O12B 1.573(3) . ? O12B H12B 0.67(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4A Zn1A N4A 180.0 2_566 . ? N4A Zn1A O11A 87.77(15) 2_566 . ? N4A Zn1A O11A 92.23(15) . . ? N4A Zn1A O11A 92.23(15) 2_566 2_566 ? N4A Zn1A O11A 87.77(15) . 2_566 ? O11A Zn1A O11A 180.0 . 2_566 ? N4A Zn1A N1A 86.05(15) 2_566 2_566 ? N4A Zn1A N1A 93.95(15) . 2_566 ? O11A Zn1A N1A 93.34(13) . 2_566 ? O11A Zn1A N1A 86.66(13) 2_566 2_566 ? N4A Zn1A N1A 93.95(15) 2_566 . ? N4A Zn1A N1A 86.05(15) . . ? O11A Zn1A N1A 86.66(13) . . ? O11A Zn1A N1A 93.34(13) 2_566 . ? N1A Zn1A N1A 180.00(18) 2_566 . ? C2A N1A C8A 111.6(4) . . ? C2A N1A C7A 109.9(4) . 2_566 ? C8A N1A C7A 111.6(3) . 2_566 ? C2A N1A Zn1A 102.2(3) . . ? C8A N1A Zn1A 111.3(3) . . ? C7A N1A Zn1A 109.8(3) 2_566 . ? N1A C2A C3A 111.4(4) . . ? N1A C2A H2A1 109.3 . . ? C3A C2A H2A1 109.4 . . ? N1A C2A H2A2 109.3 . . ? C3A C2A H2A2 109.3 . . ? H2A1 C2A H2A2 108.0 . . ? N4A C3A C2A 109.7(4) . . ? N4A C3A H3A1 109.7 . . ? C2A C3A H3A1 109.7 . . ? N4A C3A H3A2 109.7 . . ? C2A C3A H3A2 109.7 . . ? H3A1 C3A H3A2 108.2 . . ? C5A N4A C3A 113.8(4) . . ? C5A N4A Zn1A 114.9(3) . . ? C3A N4A Zn1A 106.2(3) . . ? C5A N4A H4A1 106(3) . . ? C3A N4A H4A1 107(3) . . ? Zn1A N4A H4A1 109(3) . . ? N4A C5A C6A 111.1(4) . . ? N4A C5A H5A1 109.4 . . ? C6A C5A H5A1 109.4 . . ? N4A C5A H5A2 109.4 . . ? C6A C5A H5A2 109.4 . . ? H5A1 C5A H5A2 108.0 . . ? C5A C6A C7A 118.7(4) . . ? C5A C6A H6A1 107.6 . . ? C7A C6A H6A1 107.6 . . ? C5A C6A H6A2 107.6 . . ? C7A C6A H6A2 107.6 . . ? H6A1 C6A H6A2 107.1 . . ? N1A C7A C6A 114.9(4) 2_566 . ? N1A C7A H7A1 108.6 2_566 . ? C6A C7A H7A1 108.6 . . ? N1A C7A H7A2 108.6 2_566 . ? C6A C7A H7A2 108.6 . . ? H7A1 C7A H7A2 107.5 . . ? N1A C8A P1A 115.3(3) . . ? N1A C8A H8A1 108.4 . . ? P1A C8A H8A1 108.4 . . ? N1A C8A H8A2 108.4 . . ? P1A C8A H8A2 108.4 . . ? H8A1 C8A H8A2 107.5 . . ? O11A P1A O13A 116.3(2) . . ? O11A P1A O12A 111.80(19) . . ? O13A P1A O12A 106.4(2) . . ? O11A P1A C8A 106.49(19) . . ? O13A P1A C8A 111.1(2) . . ? O12A P1A C8A 104.1(2) . . ? P1A O11A Zn1A 117.10(18) . . ? P1A O12A H12A 116(4) . . ? N4B Zn1B N4B 180.0 . 2_575 ? N4B Zn1B N1B 85.61(15) . . ? N4B Zn1B N1B 94.39(15) 2_575 . ? N4B Zn1B N1B 94.39(15) . 2_575 ? N4B Zn1B N1B 85.61(15) 2_575 2_575 ? N1B Zn1B N1B 180.00(13) . 2_575 ? N4B Zn1B O11B 88.35(14) . 2_575 ? N4B Zn1B O11B 91.65(14) 2_575 2_575 ? N1B Zn1B O11B 94.14(13) . 2_575 ? N1B Zn1B O11B 85.86(13) 2_575 2_575 ? N4B Zn1B O11B 91.65(14) . . ? N4B Zn1B O11B 88.35(14) 2_575 . ? N1B Zn1B O11B 85.86(13) . . ? N1B Zn1B O11B 94.14(13) 2_575 . ? O11B Zn1B O11B 180.0(2) 2_575 . ? C7B N1B C8B 111.3(4) 2_575 . ? C7B N1B C2B 110.2(4) 2_575 . ? C8B N1B C2B 111.7(4) . . ? C7B N1B Zn1B 109.9(3) 2_575 . ? C8B N1B Zn1B 112.2(3) . . ? C2B N1B Zn1B 101.2(3) . . ? N1B C2B C3B 111.2(4) . . ? N1B C2B H2B1 109.4 . . ? C3B C2B H2B1 109.4 . . ? N1B C2B H2B2 109.4 . . ? C3B C2B H2B2 109.4 . . ? H2B1 C2B H2B2 108.0 . . ? N4B C3B C2B 109.7(4) . . ? N4B C3B H3B1 109.7 . . ? C2B C3B H3B1 109.7 . . ? N4B C3B H3B2 109.7 . . ? C2B C3B H3B2 109.7 . . ? H3B1 C3B H3B2 108.2 . . ? C3B N4B C5B 113.9(4) . . ? C3B N4B Zn1B 106.4(3) . . ? C5B N4B Zn1B 114.1(3) . . ? C3B N4B H4B1 108(4) . . ? C5B N4B H4B1 107(3) . . ? Zn1B N4B H4B1 108(3) . . ? N4B C5B C6B 111.8(4) . . ? N4B C5B H5B1 109.3 . . ? C6B C5B H5B1 109.3 . . ? N4B C5B H5B2 109.3 . . ? C6B C5B H5B2 109.3 . . ? H5B1 C5B H5B2 107.9 . . ? C5B C6B C7B 117.4(4) . . ? C5B C6B H6B1 108.0 . . ? C7B C6B H6B1 108.0 . . ? C5B C6B H6B2 108.0 . . ? C7B C6B H6B2 108.0 . . ? H6B1 C6B H6B2 107.2 . . ? N1B C7B C6B 115.4(4) 2_575 . ? N1B C7B H7B1 108.4 2_575 . ? C6B C7B H7B1 108.4 . . ? N1B C7B H7B2 108.4 2_575 . ? C6B C7B H7B2 108.4 . . ? H7B1 C7B H7B2 107.5 . . ? N1B C8B P1B 115.6(3) . . ? N1B C8B H8B1 108.4 . . ? P1B C8B H8B1 108.4 . . ? N1B C8B H8B2 108.4 . . ? P1B C8B H8B2 108.4 . . ? H8B1 C8B H8B2 107.4 . . ? O13B P1B O11B 117.5(2) . . ? O13B P1B O12B 105.0(2) . . ? O11B P1B O12B 111.3(2) . . ? O13B P1B C8B 110.3(3) . . ? O11B P1B C8B 106.98(19) . . ? O12B P1B C8B 105.1(2) . . ? P1B O11B Zn1B 117.52(19) . . ? P1B O12B H12B 112(7) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.187 _refine_diff_density_min -0.831 _refine_diff_density_rms 0.107