data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 # #------------------------------------------------------------------------- # 1. SUBMISSION DETAILS # _publ_contact_author 'Liliane G Hubert-Pfalzgraf' _publ_contact_author_address ; Institut de Recherches sur la Catalyse Universite Claude Bernard -Lyon 1 2, Avenue A. Einstein Lyon Rhone 69626 FRANCE ; _publ_contact_author_email LILIANE.HUBERT@UNIV-LYON1.FR #------------------------------------------------------------------------- # 2. TITLE AND AUTHOR LIST _publ_section_title ; Interplay between lead carboxylate and Ti or Zr isopropoxides in solution routes to perovskites: Synthesis, molecular structures and reactivity of single source non-oxo Pb-Zr and Pb-Ti carboxylatoalkoxides supported by 2-ethylhexanoate ligands ; loop_ _publ_author_name _publ_author_address 'A. Brethon' ; Universite Lyon1, IRC, 2 av. A. Einstein, 69626 Villeurbanne Cedex ; 'L.G. Hubert-Pfalzgraf' ; Universite Lyon1, IRC, 2 av. A. Einstein, 69626 Villeurbanne Cedex ; 'Daran Jean-Claude' ; Laboratoire de Chimie de Coordination UPR-CNRS 8241 205, route de Narbonne 31077 Toulouse cedex, France ; #=========================================================================== _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) SIR97- a program for automatic solution of crystal structures by direct methods. = J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1997) ORTEP-3 for Windows, J. Appl. Cryst. 30, 565. Farrugia, L. J. (1999) WinGX, J. Appl. Cryst. 32, 837-838. Oxford-Diffraction, CRYSALIS-CCD, data collection, version 1.169, 2001, Poland. Oxford-Diffraction, CRYSALIS-RED, data reduction, version 1.169, 2001, Poland. Sheldrick, G.M. (1997) SHELXL97. Program for crystal structure refinement. University of G\"ottingen, Germany. Stoe, IPDS Manual. Version 2.75. Stoe & Cie, Darmstadt,1996, Germany. Stoe, X-RED, Data Reduction for STADI4 and IPDS, Revision 1.08. Stoe & Cie, Darmstadt, 1996, Germany. ; _publ_contact_author_name 'Liliane G Hubert-Pfalzgraf' #=========================================================================== #===================================================================== data_Ab31Re _database_code_depnum_ccdc_archive 'CCDC 230776' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_sum 'C40 H84 O12 Pb Ti2' _chemical_formula_moiety 'C40 H84 O12 Pb Ti2' _chemical_compound_source 'synthesis as described' _chemical_formula_weight 1060.06 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 '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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3722(6) _cell_length_b 12.4435(6) _cell_length_c 19.3035(10) _cell_angle_alpha 91.624(4) _cell_angle_beta 96.393(4) _cell_angle_gamma 109.728(5) _cell_volume 2549.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 7814 _cell_measurement_theta_min 3.7 _cell_measurement_theta_max 30.4 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1050 _exptl_absorpt_coefficient_mu 3.650 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.0564 _exptl_absorpt_correction_T_max 0.1223 _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type ? _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford-Diffraction Xcalibur' _diffrn_measurement_method \w-\f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 9557 _diffrn_reflns_av_R_equivalents 0.0848 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 24.66 _reflns_number_total 6680 _reflns_number_gt 5677 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++) (compiled Jun 6 2003,13:53:32) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++) (compiled Jun 6 2003,13:53:32) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++) (compiled Jun 6 2003,13:53:32) ; _computing_structure_solution 'SIR-97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1084P)^2^+1.0398P] 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 6680 _refine_ls_number_parameters 544 _refine_ls_number_restraints 480 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1586 _refine_ls_wR_factor_gt 0.1484 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.002 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 Pb1 Pb 0.43986(2) 0.48921(2) 0.381043(12) 0.04030(15) Uani 1 1 d U . . Ti1 Ti 0.37071(10) 0.27803(10) 0.23487(7) 0.0322(3) Uani 1 1 d U . . Ti2 Ti 0.27578(10) 0.49894(9) 0.20850(6) 0.0323(3) Uani 1 1 d U . . O11 O 0.2465(4) 0.2293(4) 0.1427(3) 0.0397(10) Uani 1 1 d U . . O12 O 0.4851(4) 0.2346(4) 0.1949(3) 0.0435(11) Uani 1 1 d U . . O14 O 0.4231(4) 0.4382(4) 0.2020(2) 0.0350(9) Uani 1 1 d U . . O21 O 0.1841(4) 0.3798(4) 0.1239(3) 0.0400(10) Uani 1 1 d U . . O22 O 0.1288(4) 0.5180(4) 0.2207(2) 0.0397(10) Uani 1 1 d U . . O23 O 0.3238(4) 0.6055(4) 0.1475(2) 0.0384(10) Uani 1 1 d U . . O24 O 0.2511(4) 0.3621(4) 0.2711(3) 0.0353(9) Uani 1 1 d U . . O31 O 0.4786(4) 0.3390(4) 0.3244(3) 0.0418(10) Uani 1 1 d U . . O32 O 0.3766(4) 0.5949(4) 0.2913(2) 0.0368(10) Uani 1 1 d U . . O33 O 0.6463(5) 0.6164(5) 0.3747(3) 0.0570(14) Uani 1 1 d U . . O34 O 0.6463(6) 0.5786(7) 0.4853(4) 0.0745(19) Uani 1 1 d U . . C20 C 0.3491(8) 0.6619(7) 0.0850(4) 0.0525(17) Uani 1 1 d U . . H20 H 0.4303 0.6603 0.0734 0.063 Uiso 1 1 calc R . . C21 C 0.2495(9) 0.6014(7) 0.0257(5) 0.059(2) Uani 1 1 d U . . H21A H 0.2461 0.5236 0.0193 0.088 Uiso 1 1 calc R . . H21B H 0.2694 0.6394 -0.0163 0.088 Uiso 1 1 calc R . . H21C H 0.1693 0.6026 0.0361 0.088 Uiso 1 1 calc R . . C112 C 0.1868(6) 0.2835(6) 0.1058(4) 0.0422(15) Uani 1 1 d U A . C114 C 0.2106(10) 0.2284(11) -0.0156(6) 0.080(3) Uani 1 1 d U A . H11A H 0.2561 0.3084 -0.0214 0.096 Uiso 1 1 calc R . . H11B H 0.2715 0.1960 0.0052 0.096 Uiso 1 1 calc R . . C115 C 0.1602(9) 0.1708(9) -0.0851(6) 0.070(3) Uani 1 1 d U . . H11C H 0.1120 0.2125 -0.1096 0.084 Uiso 1 1 calc R . . H11D H 0.1022 0.0949 -0.0796 0.084 Uiso 1 1 calc R . . C116 C 0.2557(12) 0.1589(12) -0.1307(7) 0.098(4) Uani 1 1 d U . . H11E H 0.3150 0.2344 -0.1359 0.117 Uiso 1 1 calc R . . H11F H 0.3024 0.1150 -0.1073 0.117 Uiso 1 1 calc R . . C117 C 0.2001(11) 0.1029(12) -0.2008(7) 0.098(4) Uani 1 1 d U . . H11G H 0.1272 0.0371 -0.1968 0.147 Uiso 1 1 calc R . . H11H H 0.2609 0.0793 -0.2218 0.147 Uiso 1 1 calc R . . H11I H 0.1759 0.1557 -0.2294 0.147 Uiso 1 1 calc R . . C113 C 0.1178(7) 0.2235(7) 0.0362(4) 0.0559(19) Uani 1 1 d DU . . C118 C -0.0041(11) 0.2400(12) 0.0141(7) 0.056(3) Uani 0.59 1 d PDU A 1 H11J H -0.0345 0.2082 -0.0336 0.068 Uiso 0.59 1 calc PR A 1 H11K H 0.0095 0.3213 0.0150 0.068 Uiso 0.59 1 calc PR A 1 C11A C -0.0020(14) 0.1392(15) 0.0435(13) 0.073(5) Uani 0.41 1 d PDU A 2 H11L H 0.0111 0.0906 0.0798 0.087 Uiso 0.41 1 calc PR A 2 H11M H -0.0321 0.0914 0.0001 0.087 Uiso 0.41 1 calc PR A 2 C119 C -0.1044(9) 0.1836(10) 0.0609(6) 0.082(3) Uani 1 1 d DU . . H11N H -0.1812 0.1963 0.0444 0.123 Uiso 0.59 1 calc PR A 1 H11O H -0.0758 0.2161 0.1080 0.123 Uiso 0.59 1 calc PR A 1 H11P H -0.1194 0.1028 0.0596 0.123 Uiso 0.59 1 calc PR A 1 H11Q H -0.1186 0.1688 0.1083 0.123 Uiso 0.41 1 d PR A 2 H11R H -0.1812 0.1464 0.0303 0.123 Uiso 0.41 1 d PR A 2 H11S H -0.0774 0.2645 0.0560 0.123 Uiso 0.41 1 d PR A 2 C121 C 0.5215(11) 0.1451(10) 0.1711(6) 0.081(3) Uani 1 1 d U . . H121 H 0.4686 0.0779 0.1922 0.098 Uiso 1 1 calc R . . C122 C 0.4831(13) 0.1189(10) 0.0951(6) 0.094(4) Uani 1 1 d U . . H12A H 0.3946 0.1056 0.0846 0.141 Uiso 1 1 calc R . . H12B H 0.5002 0.0517 0.0807 0.141 Uiso 1 1 calc R . . H12C H 0.5295 0.1823 0.0706 0.141 Uiso 1 1 calc R . . C123 C 0.6480(16) 0.1553(18) 0.1979(10) 0.161(8) Uani 1 1 d U . . H12D H 0.7049 0.1976 0.1672 0.241 Uiso 1 1 calc R . . H12E H 0.6539 0.0804 0.2010 0.241 Uiso 1 1 calc R . . H12F H 0.6697 0.1947 0.2435 0.241 Uiso 1 1 calc R . . O13 O 0.2837(4) 0.1435(4) 0.2662(3) 0.0453(11) Uani 1 1 d DU B . C131 C 0.1944(13) 0.0333(8) 0.2605(8) 0.099(4) Uani 1 1 d DU . . C13A C 0.172(4) -0.031(2) 0.1950(15) 0.107(12) Uani 0.53 1 d PDU B 1 H13A H 0.1451 0.0098 0.1586 0.161 Uiso 0.53 1 calc PR B 1 H13B H 0.1073 -0.1041 0.1969 0.161 Uiso 0.53 1 calc PR B 1 H13C H 0.2480 -0.0426 0.1853 0.161 Uiso 0.53 1 calc PR B 1 C13C C 0.238(3) -0.0198(19) 0.3214(16) 0.137(12) Uani 0.53 1 d PDU B 1 H13D H 0.2533 0.0303 0.3627 0.205 Uiso 0.53 1 calc PR B 1 H13E H 0.3141 -0.0326 0.3136 0.205 Uiso 0.53 1 calc PR B 1 H13F H 0.1741 -0.0915 0.3274 0.205 Uiso 0.53 1 calc PR B 1 C13B C 0.203(5) -0.046(3) 0.2074(16) 0.089(12) Uani 0.47 1 d PDU B 2 H13G H 0.2299 -0.0065 0.1670 0.134 Uiso 0.47 1 calc PR B 2 H13H H 0.1216 -0.1043 0.1948 0.134 Uiso 0.47 1 calc PR B 2 H13I H 0.2623 -0.0814 0.2250 0.134 Uiso 0.47 1 calc PR B 2 C13D C 0.151(4) -0.014(2) 0.3242(16) 0.118(12) Uani 0.47 1 d PDU B 2 H13J H 0.1435 0.0449 0.3545 0.177 Uiso 0.47 1 calc PR B 2 H13K H 0.2107 -0.0452 0.3470 0.177 Uiso 0.47 1 calc PR B 2 H13L H 0.0707 -0.0738 0.3134 0.177 Uiso 0.47 1 calc PR B 2 C141 C 0.5301(6) 0.5018(7) 0.1700(4) 0.0488(17) Uani 1 1 d U . . H141 H 0.5288 0.5801 0.1688 0.059 Uiso 1 1 calc R . . C142 C 0.6508(7) 0.5101(9) 0.2114(6) 0.070(3) Uani 1 1 d U . . H14A H 0.6560 0.5454 0.2570 0.104 Uiso 1 1 calc R . . H14B H 0.7195 0.5555 0.1883 0.104 Uiso 1 1 calc R . . H14C H 0.6551 0.4349 0.2157 0.104 Uiso 1 1 calc R . . C143 C 0.5141(7) 0.4566(7) 0.0941(4) 0.0490(17) Uani 1 1 d U . . H14D H 0.5053 0.3770 0.0923 0.073 Uiso 1 1 calc R . . H14E H 0.5867 0.4988 0.0728 0.073 Uiso 1 1 calc R . . H14F H 0.4403 0.4655 0.0694 0.073 Uiso 1 1 calc R . . C221 C 0.0532(8) 0.5795(8) 0.1921(5) 0.057(2) Uani 1 1 d U . . H221 H 0.1077 0.6419 0.1682 0.068 Uiso 1 1 calc R . . C222 C 0.0052(8) 0.6336(8) 0.2468(6) 0.066(3) Uani 1 1 d U . . H22A H -0.0379 0.5766 0.2763 0.099 Uiso 1 1 calc R . . H22B H -0.0520 0.6681 0.2250 0.099 Uiso 1 1 calc R . . H22C H 0.0746 0.6913 0.2743 0.099 Uiso 1 1 calc R . . C223 C -0.0476(8) 0.5055(9) 0.1375(5) 0.066(2) Uani 1 1 d U . . H22D H -0.0103 0.4722 0.1045 0.099 Uiso 1 1 calc R . . H22E H -0.0906 0.5509 0.1138 0.099 Uiso 1 1 calc R . . H22F H -0.1066 0.4457 0.1593 0.099 Uiso 1 1 calc R . . C241 C 0.1426(6) 0.3018(7) 0.3057(4) 0.0434(16) Uani 1 1 d U . . H241 H 0.1642 0.2447 0.3334 0.052 Uiso 1 1 calc R . . C242 C 0.0309(7) 0.2393(7) 0.2534(5) 0.0519(18) Uani 1 1 d U . . H24A H 0.0148 0.2918 0.2213 0.078 Uiso 1 1 calc R . . H24B H -0.0415 0.2066 0.2771 0.078 Uiso 1 1 calc R . . H24C H 0.0476 0.1796 0.2282 0.078 Uiso 1 1 calc R . . C243 C 0.1107(7) 0.3820(7) 0.3556(4) 0.0524(18) Uani 1 1 d U . . H24D H 0.1825 0.4190 0.3897 0.079 Uiso 1 1 calc R . . H24E H 0.0410 0.3388 0.3787 0.079 Uiso 1 1 calc R . . H24F H 0.0887 0.4387 0.3297 0.079 Uiso 1 1 calc R . . C311 C 0.5433(9) 0.2722(8) 0.3622(5) 0.066(2) Uani 1 1 d U . . H311 H 0.5287 0.2014 0.3337 0.079 Uiso 1 1 calc R . . C321 C 0.3863(8) 0.7142(6) 0.3033(5) 0.0502(18) Uani 1 1 d U . . H321 H 0.3192 0.7282 0.2724 0.060 Uiso 1 1 calc R . . C322 C 0.5110(8) 0.7887(7) 0.2849(5) 0.060(2) Uani 1 1 d U . . H32A H 0.5773 0.7742 0.3141 0.090 Uiso 1 1 calc R . . H32B H 0.5189 0.8676 0.2921 0.090 Uiso 1 1 calc R . . H32C H 0.5167 0.7719 0.2368 0.090 Uiso 1 1 calc R . . C323 C 0.3678(11) 0.7339(9) 0.3786(6) 0.072(3) Uani 1 1 d U . . H32D H 0.2879 0.6814 0.3874 0.109 Uiso 1 1 calc R . . H32E H 0.3697 0.8110 0.3867 0.109 Uiso 1 1 calc R . . H32F H 0.4340 0.7219 0.4092 0.109 Uiso 1 1 calc R . . C331 C 0.6979(7) 0.6287(7) 0.4375(5) 0.0483(17) Uani 1 1 d U . . C332 C 0.8385(8) 0.7066(9) 0.4509(6) 0.070(2) Uani 1 1 d U . . H332 H 0.8524 0.7253 0.5015 0.084 Uiso 1 1 calc R . . C333 C 0.8619(12) 0.8152(11) 0.4229(9) 0.103(3) Uani 1 1 d U . . H33A H 0.8416 0.8028 0.3725 0.123 Uiso 1 1 calc R . . H33B H 0.9515 0.8578 0.4328 0.123 Uiso 1 1 calc R . . C334 C 0.7923(13) 0.8888(10) 0.4483(8) 0.104(4) Uani 1 1 d U . . H33C H 0.8188 0.9105 0.4977 0.125 Uiso 1 1 calc R . . H33D H 0.7025 0.8464 0.4418 0.125 Uiso 1 1 calc R . . C335 C 0.820(2) 0.9944(14) 0.4077(12) 0.162(8) Uani 1 1 d U . . H33E H 0.9079 1.0410 0.4191 0.194 Uiso 1 1 calc R . . H33F H 0.8046 0.9719 0.3581 0.194 Uiso 1 1 calc R . . C336 C 0.745(3) 1.0598(17) 0.4225(18) 0.249(15) Uani 1 1 d U . . H33G H 0.7521 1.1170 0.3894 0.374 Uiso 1 1 calc R . . H33H H 0.7722 1.0962 0.4688 0.374 Uiso 1 1 calc R . . H33I H 0.6582 1.0106 0.4195 0.374 Uiso 1 1 calc R . . C337 C 0.9178(8) 0.6278(11) 0.4414(6) 0.085(3) Uani 1 1 d U . . H33J H 0.8879 0.5630 0.4695 0.102 Uiso 1 1 calc R . . H33K H 0.9006 0.5982 0.3929 0.102 Uiso 1 1 calc R . . C338 C 1.0541(10) 0.6785(13) 0.4594(8) 0.104(4) Uani 1 1 d U . . H33L H 1.0861 0.7424 0.4317 0.157 Uiso 1 1 calc R . . H33M H 1.0923 0.6224 0.4502 0.157 Uiso 1 1 calc R . . H33N H 1.0736 0.7042 0.5080 0.157 Uiso 1 1 calc R . . C312 C 0.6816(12) 0.3381(11) 0.3722(12) 0.159(7) Uani 1 1 d U . . H31A H 0.7071 0.3680 0.3289 0.239 Uiso 1 1 calc R . . H31B H 0.7268 0.2884 0.3872 0.239 Uiso 1 1 calc R . . H31C H 0.6998 0.4001 0.4070 0.239 Uiso 1 1 calc R . . C313 C 0.491(2) 0.2405(17) 0.4307(7) 0.152(7) Uani 1 1 d U . . H31D H 0.5171 0.3075 0.4624 0.228 Uiso 1 1 calc R . . H31E H 0.5228 0.1843 0.4507 0.228 Uiso 1 1 calc R . . H31F H 0.4009 0.2097 0.4223 0.228 Uiso 1 1 calc R . . C22 C 0.3590(10) 0.7863(7) 0.0972(5) 0.067(2) Uani 1 1 d U . . H22G H 0.2809 0.7893 0.1099 0.100 Uiso 1 1 calc R . . H22H H 0.3768 0.8248 0.0552 0.100 Uiso 1 1 calc R . . H22I H 0.4257 0.8231 0.1342 0.100 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 Pb1 0.0418(2) 0.0428(2) 0.0366(2) 0.00265(13) 0.00387(12) 0.01518(13) Ti1 0.0295(6) 0.0286(6) 0.0395(7) 0.0026(5) 0.0061(5) 0.0109(5) Ti2 0.0342(6) 0.0295(6) 0.0346(6) 0.0033(5) 0.0051(4) 0.0124(5) O11 0.044(2) 0.030(2) 0.043(3) -0.0016(19) 0.0015(19) 0.0124(19) O12 0.041(2) 0.041(3) 0.055(3) 0.005(2) 0.012(2) 0.019(2) O14 0.030(2) 0.031(2) 0.044(3) 0.0068(18) 0.0123(17) 0.0085(17) O21 0.049(3) 0.035(2) 0.037(3) 0.0000(19) 0.0025(19) 0.019(2) O22 0.040(2) 0.042(3) 0.042(3) 0.004(2) 0.0075(18) 0.0178(19) O23 0.045(2) 0.035(2) 0.037(2) 0.0050(18) 0.0058(18) 0.0154(19) O24 0.032(2) 0.035(2) 0.040(3) 0.0064(18) 0.0104(17) 0.0101(17) O31 0.043(2) 0.043(3) 0.042(3) 0.007(2) 0.0008(19) 0.019(2) O32 0.045(2) 0.031(2) 0.038(2) -0.0005(19) 0.0035(18) 0.0177(19) O33 0.047(3) 0.057(3) 0.060(3) 0.005(3) 0.002(2) 0.009(2) O34 0.052(3) 0.112(6) 0.050(4) 0.008(4) 0.002(3) 0.017(3) C20 0.059(4) 0.052(4) 0.050(4) 0.012(3) 0.011(3) 0.022(4) C21 0.088(6) 0.046(4) 0.042(4) 0.013(3) 0.005(4) 0.022(4) C112 0.038(3) 0.037(3) 0.046(4) -0.003(3) 0.001(3) 0.007(3) C114 0.074(6) 0.096(7) 0.058(5) -0.010(5) 0.004(4) 0.015(5) C115 0.065(5) 0.075(6) 0.063(5) -0.019(5) 0.004(4) 0.018(5) C116 0.089(7) 0.113(9) 0.081(7) -0.012(7) 0.040(6) 0.015(7) C117 0.083(7) 0.106(9) 0.090(8) -0.029(7) 0.024(6) 0.011(7) C113 0.062(4) 0.054(4) 0.044(4) -0.013(4) -0.011(3) 0.017(4) C118 0.069(6) 0.053(7) 0.048(8) -0.003(6) -0.004(5) 0.025(6) C11A 0.065(8) 0.052(10) 0.080(13) 0.004(9) -0.018(7) 0.001(6) C119 0.079(5) 0.090(7) 0.071(7) 0.019(6) 0.010(5) 0.021(5) C121 0.097(7) 0.080(7) 0.088(7) -0.009(6) 0.023(5) 0.055(6) C122 0.141(10) 0.075(7) 0.086(7) -0.013(6) 0.037(6) 0.059(7) C123 0.146(12) 0.25(2) 0.159(14) -0.024(14) 0.007(9) 0.168(15) O13 0.045(3) 0.034(2) 0.057(3) 0.011(2) 0.011(2) 0.0127(19) C131 0.130(9) 0.034(4) 0.125(9) 0.020(5) 0.051(8) 0.006(5) C13A 0.11(2) 0.036(11) 0.134(15) -0.005(11) -0.025(16) -0.013(14) C13C 0.22(3) 0.046(11) 0.117(17) 0.032(11) 0.037(19) 0.001(18) C13B 0.12(3) 0.051(12) 0.087(16) 0.006(11) 0.015(17) 0.009(13) C13D 0.16(3) 0.050(13) 0.15(2) 0.024(13) 0.10(2) 0.008(16) C141 0.035(3) 0.055(4) 0.048(4) 0.011(3) 0.018(3) -0.001(3) C142 0.040(4) 0.080(6) 0.083(7) 0.001(5) 0.011(4) 0.013(4) C143 0.056(4) 0.051(4) 0.046(4) 0.006(3) 0.023(3) 0.020(4) C221 0.063(5) 0.056(5) 0.061(5) 0.006(4) 0.001(4) 0.037(4) C222 0.052(5) 0.062(5) 0.084(7) -0.020(5) 0.003(4) 0.023(4) C223 0.065(5) 0.084(6) 0.060(5) -0.010(4) -0.003(4) 0.047(5) C241 0.034(3) 0.053(4) 0.047(4) 0.014(3) 0.018(3) 0.015(3) C242 0.040(4) 0.047(4) 0.065(5) 0.014(4) 0.018(3) 0.006(3) C243 0.053(4) 0.067(5) 0.047(4) 0.017(4) 0.023(3) 0.028(4) C311 0.085(5) 0.054(5) 0.066(5) -0.007(4) -0.020(4) 0.045(4) C321 0.070(5) 0.027(3) 0.054(5) -0.007(3) -0.003(4) 0.022(3) C322 0.059(5) 0.038(4) 0.070(6) 0.005(4) -0.010(4) 0.004(3) C323 0.100(7) 0.064(6) 0.061(6) -0.017(5) 0.006(5) 0.041(5) C331 0.042(3) 0.050(4) 0.060(5) 0.002(3) 0.007(3) 0.024(3) C332 0.040(4) 0.074(5) 0.088(7) -0.004(5) 0.002(4) 0.011(4) C333 0.083(7) 0.088(6) 0.110(10) 0.012(7) 0.013(6) -0.007(5) C334 0.107(8) 0.059(6) 0.127(11) 0.007(6) -0.029(7) 0.016(5) C335 0.193(17) 0.086(9) 0.161(17) 0.026(9) -0.040(14) 0.007(9) C336 0.30(3) 0.098(13) 0.34(4) 0.017(18) -0.10(2) 0.093(16) C337 0.050(4) 0.112(7) 0.082(7) -0.020(6) 0.018(4) 0.014(5) C338 0.064(5) 0.142(12) 0.116(11) -0.003(9) 0.013(6) 0.047(7) C312 0.085(6) 0.074(8) 0.30(2) 0.000(10) -0.097(9) 0.036(6) C313 0.289(17) 0.211(17) 0.049(7) 0.030(8) 0.034(9) 0.203(15) C22 0.093(7) 0.035(4) 0.062(6) 0.015(4) 0.006(5) 0.009(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 Pb1 O31 2.331(5) . ? Pb1 O33 2.366(5) . ? Pb1 O32 2.395(5) . ? Pb1 O34 2.803(6) . ? Pb1 O34 2.909(7) 2_666 ? Ti1 O13 1.795(5) . ? Ti1 O12 1.804(5) . ? Ti1 O31 1.973(5) . ? Ti1 O14 2.021(5) . ? Ti1 O11 2.081(5) . ? Ti1 O24 2.137(5) . ? Ti1 Ti2 3.3077(15) . ? Ti2 O23 1.785(5) . ? Ti2 O22 1.806(5) . ? Ti2 O32 1.963(5) . ? Ti2 O14 2.072(4) . ? Ti2 O24 2.075(5) . ? Ti2 O21 2.096(5) . ? O11 C112 1.285(9) . ? O12 C121 1.396(10) . ? O14 C141 1.425(8) . ? O21 C112 1.250(8) . ? O22 C221 1.411(9) . ? O23 C20 1.422(10) . ? O24 C241 1.456(8) . ? O31 C311 1.446(9) . ? O32 C321 1.461(8) . ? O33 C331 1.267(10) . ? O34 C331 1.222(11) . ? C20 C21 1.499(12) . ? C20 C22 1.523(12) . ? C112 C113 1.515(10) . ? C114 C115 1.463(14) . ? C114 C113 1.520(14) . ? C115 C116 1.513(14) . ? C116 C117 1.474(17) . ? C113 C11A 1.436(15) . ? C113 C118 1.486(12) . ? C118 C119 1.529(14) . ? C11A C119 1.512(16) . ? C121 C123 1.435(17) . ? C121 C122 1.479(16) . ? O13 C131 1.397(11) . ? C131 C13A 1.43(2) . ? C131 C13B 1.44(2) . ? C131 C13D 1.44(3) . ? C131 C13C 1.48(3) . ? C141 C142 1.479(11) . ? C141 C143 1.523(11) . ? C221 C222 1.482(12) . ? C221 C223 1.495(12) . ? C241 C242 1.498(11) . ? C241 C243 1.523(11) . ? C311 C312 1.495(16) . ? C311 C313 1.517(19) . ? C321 C322 1.496(13) . ? C321 C323 1.516(14) . ? C331 C332 1.553(11) . ? C332 C333 1.421(17) . ? C332 C337 1.560(14) . ? C333 C334 1.50(2) . ? C334 C335 1.51(2) . ? C335 C336 1.41(3) . ? C337 C338 1.459(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O31 Pb1 O33 92.15(19) . . ? O31 Pb1 O32 106.48(16) . . ? O33 Pb1 O32 85.22(18) . . ? O31 Pb1 O34 104.18(19) . . ? O33 Pb1 O34 49.5(2) . . ? O32 Pb1 O34 125.4(2) . . ? O31 Pb1 O34 109.9(2) . 2_666 ? O33 Pb1 O34 121.23(19) . 2_666 ? O32 Pb1 O34 133.15(18) . 2_666 ? O34 Pb1 O34 72.1(2) . 2_666 ? O13 Ti1 O12 98.8(2) . . ? O13 Ti1 O31 95.1(2) . . ? O12 Ti1 O31 95.7(2) . . ? O13 Ti1 O14 163.8(2) . . ? O12 Ti1 O14 96.4(2) . . ? O31 Ti1 O14 89.2(2) . . ? O13 Ti1 O11 87.6(2) . . ? O12 Ti1 O11 90.5(2) . . ? O31 Ti1 O11 172.76(19) . . ? O14 Ti1 O11 86.49(19) . . ? O13 Ti1 O24 93.3(2) . . ? O12 Ti1 O24 167.8(2) . . ? O31 Ti1 O24 85.24(19) . . ? O14 Ti1 O24 71.46(18) . . ? O11 Ti1 O24 87.88(19) . . ? O13 Ti1 Ti2 127.19(16) . . ? O12 Ti1 Ti2 130.44(18) . . ? O31 Ti1 Ti2 97.29(14) . . ? O14 Ti1 Ti2 36.60(12) . . ? O11 Ti1 Ti2 75.81(13) . . ? O24 Ti1 Ti2 37.60(14) . . ? O23 Ti2 O22 97.2(2) . . ? O23 Ti2 O32 96.1(2) . . ? O22 Ti2 O32 96.9(2) . . ? O23 Ti2 O14 95.3(2) . . ? O22 Ti2 O14 166.2(2) . . ? O32 Ti2 O14 87.29(18) . . ? O23 Ti2 O24 166.9(2) . . ? O22 Ti2 O24 95.4(2) . . ? O32 Ti2 O24 86.0(2) . . ? O14 Ti2 O24 71.75(18) . . ? O23 Ti2 O21 88.4(2) . . ? O22 Ti2 O21 90.1(2) . . ? O32 Ti2 O21 171.14(19) . . ? O14 Ti2 O21 84.70(18) . . ? O24 Ti2 O21 87.88(19) . . ? O23 Ti2 Ti1 127.98(15) . . ? O22 Ti2 Ti1 130.70(16) . . ? O32 Ti2 Ti1 96.65(13) . . ? O14 Ti2 Ti1 35.56(12) . . ? O24 Ti2 Ti1 38.93(13) . . ? O21 Ti2 Ti1 74.60(13) . . ? C112 O11 Ti1 131.6(4) . . ? C121 O12 Ti1 147.8(6) . . ? C141 O14 Ti1 131.1(4) . . ? C141 O14 Ti2 120.6(4) . . ? Ti1 O14 Ti2 107.84(19) . . ? C112 O21 Ti2 133.5(4) . . ? C221 O22 Ti2 138.5(5) . . ? C20 O23 Ti2 163.3(5) . . ? C241 O24 Ti2 128.9(4) . . ? C241 O24 Ti1 121.9(4) . . ? Ti2 O24 Ti1 103.5(2) . . ? C311 O31 Ti1 121.1(5) . . ? C311 O31 Pb1 120.9(5) . . ? Ti1 O31 Pb1 114.8(2) . . ? C321 O32 Ti2 122.1(4) . . ? C321 O32 Pb1 122.7(4) . . ? Ti2 O32 Pb1 113.8(2) . . ? C331 O33 Pb1 103.0(5) . . ? C331 O34 Pb1 83.3(5) . . ? O23 C20 C21 110.6(7) . . ? O23 C20 C22 109.2(7) . . ? C21 C20 C22 111.7(7) . . ? O21 C112 O11 124.3(6) . . ? O21 C112 C113 120.1(7) . . ? O11 C112 C113 115.6(6) . . ? C115 C114 C113 117.7(8) . . ? C114 C115 C116 116.4(9) . . ? C117 C116 C115 114.1(10) . . ? C11A C113 C118 57.1(10) . . ? C11A C113 C112 111.9(11) . . ? C118 C113 C112 115.4(8) . . ? C11A C113 C114 131.3(11) . . ? C118 C113 C114 121.1(9) . . ? C112 C113 C114 110.4(7) . . ? C113 C118 C119 112.7(10) . . ? C113 C11A C119 116.6(13) . . ? C11A C119 C118 54.7(10) . . ? O12 C121 C123 113.7(10) . . ? O12 C121 C122 110.8(9) . . ? C123 C121 C122 117.6(11) . . ? C131 O13 Ti1 155.2(8) . . ? O13 C131 C13A 117.0(17) . . ? O13 C131 C13B 117.4(18) . . ? C13A C131 C13B 20(3) . . ? O13 C131 C13D 117.0(17) . . ? C13A C131 C13D 125(2) . . ? C13B C131 C13D 116.3(18) . . ? O13 C131 C13C 102.9(14) . . ? C13A C131 C13C 115(2) . . ? C13B C131 C13C 97(3) . . ? C13D C131 C13C 40.5(19) . . ? O14 C141 C142 112.8(7) . . ? O14 C141 C143 109.6(6) . . ? C142 C141 C143 115.0(7) . . ? O22 C221 C222 112.3(8) . . ? O22 C221 C223 110.2(7) . . ? C222 C221 C223 113.9(7) . . ? O24 C241 C242 111.0(6) . . ? O24 C241 C243 111.8(6) . . ? C242 C241 C243 110.8(6) . . ? O31 C311 C312 108.9(9) . . ? O31 C311 C313 110.5(9) . . ? C312 C311 C313 112.6(13) . . ? O32 C321 C322 108.2(7) . . ? O32 C321 C323 108.4(7) . . ? C322 C321 C323 113.6(7) . . ? O34 C331 O33 124.1(7) . . ? O34 C331 C332 119.8(8) . . ? O33 C331 C332 115.9(8) . . ? C333 C332 C331 113.3(9) . . ? C333 C332 C337 124.5(10) . . ? C331 C332 C337 106.7(8) . . ? C332 C333 C334 117.1(12) . . ? C333 C334 C335 109.1(17) . . ? C336 C335 C334 112(2) . . ? C338 C337 C332 117.3(10) . . ? _diffrn_measured_fraction_theta_max 0.769 _diffrn_reflns_theta_full 24.66 _diffrn_measured_fraction_theta_full 0.769 _refine_diff_density_max 1.189 _refine_diff_density_min -1.070 _refine_diff_density_rms 0.112 #========END #=========================================================================== #===================================================================== data_ab42r3 _database_code_depnum_ccdc_archive 'CCDC 230777' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H48 O8 Pb Ti1.50' _chemical_formula_sum 'C23 H48 O8 Pb Ti1.50' _chemical_compound_source 'synthesis as described' _chemical_formula_weight 731.65 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 '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 monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.6632(17) _cell_length_b 14.2307(14) _cell_length_c 22.7373(17) _cell_angle_alpha 90.00 _cell_angle_beta 116.342(8) _cell_angle_gamma 90.00 _cell_volume 6281.7(9) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description box _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.42 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2920 _exptl_absorpt_coefficient_mu 5.762 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.0375 _exptl_absorpt_correction_T_max 0.0693 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method \f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 200 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 3 _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 19801 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 24.09 _reflns_number_total 4824 _reflns_number_gt 3850 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS X-red' _computing_structure_solution 'SIR-97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0660P)^2^+26.4607P] 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 4824 _refine_ls_number_parameters 219 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1216 _refine_ls_wR_factor_gt 0.1156 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.001 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 O4 O 0.5781(3) 0.4434(4) 0.2404(3) 0.0703(16) Uani 1 1 d . A . C41 C 0.5317(5) 0.4685(6) 0.1855(5) 0.061(2) Uiso 1 1 d . . . C42 C 0.5534(6) 0.5335(7) 0.1455(5) 0.083(3) Uiso 1 1 d D . . C43A C 0.6086(9) 0.4957(11) 0.1313(9) 0.093(5) Uiso 0.65 1 d PD A 1 H43A H 0.6498 0.4877 0.1723 0.112 Uiso 0.65 1 calc PR A 1 H43B H 0.6189 0.5411 0.1051 0.112 Uiso 0.65 1 calc PR A 1 C43B C 0.5525(18) 0.4910(18) 0.0855(12) 0.103(10) Uiso 0.35 1 d PD A 2 H43C H 0.5716 0.5362 0.0661 0.123 Uiso 0.35 1 calc PR A 2 H43D H 0.5049 0.4806 0.0542 0.123 Uiso 0.35 1 calc PR A 2 C44 C 0.5904(7) 0.4011(9) 0.0946(7) 0.111(4) Uiso 1 1 d D . . H44E H 0.5832 0.3552 0.1225 0.133 Uiso 0.65 1 calc PR A 1 H44F H 0.5470 0.4084 0.0557 0.133 Uiso 0.65 1 calc PR A 1 H44G H 0.5741 0.3567 0.1170 0.133 Uiso 0.35 1 d PR A 2 H44H H 0.6388 0.4125 0.1227 0.133 Uiso 0.35 1 d PR A 2 C45A C 0.6418(13) 0.3625(17) 0.0744(15) 0.152(9) Uiso 0.65 1 d PD A 1 H45A H 0.6853 0.3542 0.1131 0.182 Uiso 0.65 1 calc PR A 1 H45B H 0.6490 0.4076 0.0461 0.182 Uiso 0.65 1 calc PR A 1 C45B C 0.584(2) 0.362(2) 0.0314(13) 0.125(13) Uiso 0.35 1 d PD A 2 H45C H 0.5360 0.3533 0.0016 0.150 Uiso 0.35 1 calc PR A 2 H45D H 0.6032 0.4065 0.0116 0.150 Uiso 0.35 1 calc PR A 2 C46 C 0.6204(10) 0.2699(12) 0.0388(9) 0.157(6) Uiso 1 1 d D . . H46A H 0.6554 0.2488 0.0269 0.236 Uiso 0.65 1 calc PR A 1 H46B H 0.5778 0.2778 0.0000 0.236 Uiso 0.65 1 calc PR A 1 H46C H 0.6145 0.2243 0.0670 0.236 Uiso 0.65 1 calc PR A 1 H46D H 0.6526 0.2747 0.0206 0.236 Uiso 0.35 1 d PR A 2 H46E H 0.5874 0.2216 0.0164 0.236 Uiso 0.35 1 d PR A 2 H46F H 0.6446 0.2547 0.0846 0.236 Uiso 0.35 1 d PR A 2 C47 C 0.5522(9) 0.6319(10) 0.1631(8) 0.133(5) Uiso 1 1 d D A . H47E H 0.5959 0.6432 0.2010 0.159 Uiso 0.65 1 calc PR B 1 H47F H 0.5533 0.6682 0.1274 0.159 Uiso 0.65 1 calc PR B 1 H47G H 0.5059 0.6522 0.1337 0.159 Uiso 0.35 1 d PR B 2 H47H H 0.5819 0.6629 0.1473 0.159 Uiso 0.35 1 d PR B 2 C48A C 0.5001(14) 0.6764(18) 0.1780(15) 0.154(10) Uiso 0.65 1 d PD A 1 H48A H 0.5113 0.7415 0.1881 0.231 Uiso 0.65 1 calc PR A 1 H48B H 0.4989 0.6457 0.2151 0.231 Uiso 0.65 1 calc PR A 1 H48C H 0.4559 0.6711 0.1408 0.231 Uiso 0.65 1 calc PR A 1 C48B C 0.569(3) 0.680(3) 0.2256(15) 0.136(16) Uiso 0.35 1 d PD A 2 H48D H 0.5650 0.7467 0.2186 0.205 Uiso 0.35 1 calc PR A 2 H48E H 0.6153 0.6647 0.2566 0.205 Uiso 0.35 1 calc PR A 2 H48F H 0.5376 0.6599 0.2425 0.205 Uiso 0.35 1 calc PR A 2 C51 C 0.3706(6) 0.2562(7) 0.0561(5) 0.080(3) Uiso 1 1 d . . . H51 H 0.3299 0.2941 0.0481 0.096 Uiso 1 1 calc R . . C52 C 0.3472(10) 0.1566(12) 0.0380(9) 0.147(6) Uiso 1 1 d . . . H52A H 0.3860 0.1178 0.0449 0.221 Uiso 1 1 calc R . . H52B H 0.3142 0.1538 -0.0074 0.221 Uiso 1 1 calc R . . H52C H 0.3263 0.1345 0.0648 0.221 Uiso 1 1 calc R . . C53 C 0.4039(9) 0.2984(12) 0.0170(9) 0.143(6) Uiso 1 1 d . . . H53D H 0.3716 0.3389 -0.0161 0.214 Uiso 1 1 calc R . . H53E H 0.4178 0.2492 -0.0034 0.214 Uiso 1 1 calc R . . H53F H 0.4435 0.3341 0.0456 0.214 Uiso 1 1 calc R . . C81 C 0.5429(7) -0.0644(9) 0.1422(6) 0.101(4) Uiso 1 1 d D . . C82A C 0.6185(10) -0.083(3) 0.1731(17) 0.159(13) Uiso 0.50 1 d PD C 1 H82A H 0.6293 -0.0528 0.2144 0.239 Uiso 0.50 1 calc PR C 1 H82B H 0.6582 -0.1162 0.1760 0.239 Uiso 0.50 1 calc PR C 1 H82C H 0.5810 -0.1256 0.1628 0.239 Uiso 0.50 1 calc PR C 1 C82B C 0.6029(13) -0.0257(18) 0.1322(13) 0.101(7) Uiso 0.50 1 d P C 1 H82D H 0.6036 0.0352 0.1507 0.151 Uiso 0.50 1 calc PR C 1 H82E H 0.5574 -0.0387 0.0986 0.151 Uiso 0.50 1 calc PR C 1 H82F H 0.6349 -0.0266 0.1135 0.151 Uiso 0.50 1 calc PR C 1 C83A C 0.5002(17) -0.037(3) 0.0694(11) 0.154(13) Uiso 0.50 1 d PD C 2 H83A H 0.4941 0.0141 0.0942 0.231 Uiso 0.50 1 calc PR C 2 H83B H 0.4739 -0.0242 0.0233 0.231 Uiso 0.50 1 calc PR C 2 H83C H 0.5480 -0.0420 0.0796 0.231 Uiso 0.50 1 calc PR C 2 C83B C 0.4840(14) -0.097(2) 0.0808(13) 0.143(12) Uiso 0.50 1 d PD C 2 H83D H 0.4661 -0.0840 0.1118 0.215 Uiso 0.50 1 calc PR C 2 H83E H 0.5218 -0.1397 0.0997 0.215 Uiso 0.50 1 calc PR C 2 H83F H 0.4484 -0.1237 0.0418 0.215 Uiso 0.50 1 calc PR C 2 C31 C 0.3638(10) -0.0984(13) 0.1477(9) 0.144(6) Uiso 1 1 d . . . H31 H 0.3707 -0.0719 0.1113 0.173 Uiso 1 1 calc R . . C32 C 0.3150(14) -0.0370(19) 0.1582(13) 0.244(12) Uiso 1 1 d . . . H32A H 0.3071 -0.0609 0.1937 0.366 Uiso 1 1 calc R . . H32B H 0.2722 -0.0351 0.1189 0.366 Uiso 1 1 calc R . . H32C H 0.3337 0.0253 0.1686 0.366 Uiso 1 1 calc R . . C33 C 0.3375(11) -0.1942(14) 0.1289(11) 0.180(8) Uiso 1 1 d . . . H33D H 0.3703 -0.2306 0.1208 0.270 Uiso 1 1 calc R . . H33E H 0.2946 -0.1922 0.0899 0.270 Uiso 1 1 calc R . . H33F H 0.3305 -0.2226 0.1638 0.270 Uiso 1 1 calc R . . C61 C 0.6810(6) 0.5098(8) 0.3809(6) 0.093(3) Uiso 1 1 d . . . H61 H 0.6427 0.5484 0.3504 0.111 Uiso 1 1 calc R . . C62 C 0.7409(8) 0.5306(11) 0.3705(8) 0.128(5) Uiso 1 1 d . . . H62A H 0.7783 0.4906 0.3979 0.192 Uiso 1 1 calc R . . H62B H 0.7538 0.5952 0.3815 0.192 Uiso 1 1 calc R . . H62C H 0.7301 0.5200 0.3253 0.192 Uiso 1 1 calc R . . C63 C 0.6925(8) 0.5333(10) 0.4479(7) 0.121(4) Uiso 1 1 d . . . H63D H 0.6517 0.5195 0.4528 0.182 Uiso 1 1 calc R . . H63E H 0.7032 0.5990 0.4558 0.182 Uiso 1 1 calc R . . H63F H 0.7302 0.4968 0.4788 0.182 Uiso 1 1 calc R . . C71 C 0.7008(7) 0.2661(10) 0.2845(7) 0.106(4) Uiso 1 1 d . . . H71 H 0.7114 0.3312 0.2784 0.127 Uiso 1 1 calc R . . C72 C 0.7465(10) 0.2365(14) 0.3462(10) 0.169(7) Uiso 1 1 d . . . H72A H 0.7431 0.2766 0.3785 0.253 Uiso 1 1 calc R . . H72B H 0.7925 0.2392 0.3502 0.253 Uiso 1 1 calc R . . H72C H 0.7359 0.1731 0.3528 0.253 Uiso 1 1 calc R . . C73 C 0.7063(9) 0.2046(11) 0.2321(9) 0.141(6) Uiso 1 1 d . . . H73D H 0.7532 0.2037 0.2385 0.211 Uiso 1 1 calc R . . H73E H 0.6773 0.2296 0.1894 0.211 Uiso 1 1 calc R . . H73F H 0.6919 0.1418 0.2353 0.211 Uiso 1 1 calc R . . O5 O 0.4160(3) 0.2614(4) 0.1244(3) 0.0667(15) Uani 1 1 d . . . O8 O 0.5261(4) 0.0036(4) 0.1798(3) 0.084(2) Uani 1 1 d . C . O1 O 0.5000 0.1063(5) 0.2500 0.062(2) Uani 1 2 d S . . O3 O 0.4294(4) -0.1017(4) 0.2034(4) 0.0808(19) Uani 1 1 d . C . O6 O 0.6618(3) 0.4138(4) 0.3670(3) 0.0706(16) Uani 1 1 d . C . O9 O 0.5294(3) 0.4431(4) 0.3379(3) 0.0697(16) Uani 1 1 d . . . O2 O 0.5000 0.2950(5) 0.2500 0.0473(16) Uani 1 2 d S . . O7 O 0.6321(3) 0.2621(4) 0.2791(3) 0.0674(16) Uani 1 1 d . C . Ti1 Ti 0.5000 -0.02529(13) 0.2500 0.0572(5) Uani 1 2 d S . . Ti2 Ti 0.58783(8) 0.34603(10) 0.31303(8) 0.0555(4) Uani 1 1 d . . . Pb1 Pb 0.530538(17) 0.18249(2) 0.184938(15) 0.05585(15) 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 O4 0.073(4) 0.057(3) 0.087(5) 0.003(3) 0.041(4) -0.012(3) O5 0.072(4) 0.063(4) 0.047(3) -0.002(3) 0.011(3) 0.003(3) O8 0.148(7) 0.040(3) 0.105(5) -0.013(3) 0.094(5) -0.006(3) O1 0.087(6) 0.043(4) 0.073(5) 0.000 0.052(5) 0.000 O3 0.085(5) 0.060(4) 0.091(5) -0.008(3) 0.033(4) -0.011(3) O6 0.068(4) 0.047(3) 0.084(4) -0.013(3) 0.022(4) -0.006(3) O9 0.078(4) 0.060(3) 0.072(4) -0.014(3) 0.035(4) 0.003(3) O2 0.053(4) 0.039(4) 0.053(4) 0.000 0.027(4) 0.000 O7 0.055(4) 0.059(3) 0.094(5) -0.010(3) 0.038(4) -0.003(3) Ti1 0.0741(14) 0.0363(10) 0.0697(14) 0.000 0.0397(13) 0.000 Ti2 0.0616(9) 0.0419(7) 0.0636(9) -0.0051(6) 0.0282(8) -0.0020(6) Pb1 0.0737(3) 0.04438(19) 0.0626(2) -0.00266(13) 0.04216(19) -0.00308(14) _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 O4 C41 1.258(10) . ? O4 Ti2 2.093(6) . ? C41 O9 1.242(10) 2_655 ? C41 C42 1.512(13) . ? C42 C47 1.461(14) . ? C42 C43A 1.470(14) . ? C42 C43B 1.484(18) . ? C43A C44 1.540(15) . ? C43B C44 1.484(18) . ? C44 C45A 1.486(17) . ? C44 C45B 1.495(18) . ? C45A C46 1.506(17) . ? C45B C46 1.490(19) . ? C47 C48A 1.460(17) . ? C47 C48B 1.472(19) . ? C51 O5 1.425(12) . ? C51 C53 1.495(19) . ? C51 C52 1.500(19) . ? C81 O8 1.440(13) . ? C81 C83B 1.486(18) . ? C81 C82A 1.492(14) . ? C81 C82B 1.52(3) . ? C81 C83A 1.549(18) . ? C82A C82B 1.17(4) . ? C83A C83B 1.00(4) . ? C31 O3 1.424(18) . ? C31 C33 1.47(2) . ? C31 C32 1.47(3) . ? C61 O6 1.423(13) . ? C61 C62 1.448(17) . ? C61 C63 1.468(16) . ? C71 C72 1.37(2) . ? C71 O7 1.439(14) . ? C71 C73 1.526(19) . ? O5 Ti2 1.894(6) 2_655 ? O5 Pb1 2.506(6) . ? O8 Ti1 1.959(6) . ? O8 Pb1 2.548(6) . ? O1 Ti1 1.873(7) . ? O1 Pb1 2.161(4) 2_655 ? O1 Pb1 2.161(4) . ? O3 Ti1 1.791(7) . ? O6 Ti2 1.805(6) . ? O9 C41 1.242(10) 2_655 ? O9 Ti2 2.112(6) . ? O2 Ti2 1.944(3) 2_655 ? O2 Ti2 1.944(3) . ? O2 Pb1 2.462(4) 2_655 ? O2 Pb1 2.462(4) . ? O7 Ti2 1.896(6) . ? O7 Pb1 2.555(6) . ? Ti1 O3 1.791(7) 2_655 ? Ti1 O8 1.959(6) 2_655 ? Ti1 Pb1 3.4982(16) 2_655 ? Ti1 Pb1 3.4982(16) . ? Ti2 O5 1.894(6) 2_655 ? Ti2 Pb1 3.4783(15) 2_655 ? Ti2 Pb1 3.4973(15) . ? Pb1 Ti2 3.4783(15) 2_655 ? 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 C41 O4 Ti2 136.6(6) . . ? O9 C41 O4 124.9(8) 2_655 . ? O9 C41 C42 118.6(9) 2_655 . ? O4 C41 C42 116.5(8) . . ? C47 C42 C43A 121.7(11) . . ? C47 C42 C43B 130.3(15) . . ? C43A C42 C43B 48.0(14) . . ? C47 C42 C41 112.0(10) . . ? C43A C42 C41 114.2(11) . . ? C43B C42 C41 115.1(15) . . ? C42 C43A C44 113.6(12) . . ? C42 C43B C44 116.1(17) . . ? C43B C44 C45A 136(2) . . ? C43B C44 C45B 112.5(15) . . ? C45A C44 C45B 47.2(17) . . ? C43B C44 C43A 46.8(14) . . ? C45A C44 C43A 116.4(13) . . ? C45B C44 C43A 138(2) . . ? C44 C45A C46 113.3(16) . . ? C46 C45B C44 113.7(19) . . ? C45B C46 C45A 46.9(17) . . ? C48A C47 C42 126.1(17) . . ? C48A C47 C48B 57(2) . . ? C42 C47 C48B 133(2) . . ? O5 C51 C53 110.2(10) . . ? O5 C51 C52 109.5(10) . . ? C53 C51 C52 114.2(12) . . ? O8 C81 C83B 115.3(16) . . ? O8 C81 C82A 110.6(17) . . ? C83B C81 C82A 134(2) . . ? O8 C81 C82B 107.7(13) . . ? C83B C81 C82B 113.9(19) . . ? C82A C81 C82B 45.5(15) . . ? O8 C81 C83A 105.9(17) . . ? C83B C81 C83A 38.5(16) . . ? C82A C81 C83A 124(2) . . ? C82B C81 C83A 83.7(17) . . ? C82B C82A C81 68.6(17) . . ? C82A C82B C81 65.9(15) . . ? C83B C83A C81 67.4(15) . . ? C83A C83B C81 74.2(17) . . ? O3 C31 C33 109.5(15) . . ? O3 C31 C32 112.4(17) . . ? C33 C31 C32 112.7(19) . . ? O6 C61 C62 110.8(11) . . ? O6 C61 C63 110.4(10) . . ? C62 C61 C63 111.8(12) . . ? C72 C71 O7 109.0(13) . . ? C72 C71 C73 110.5(14) . . ? O7 C71 C73 110.3(12) . . ? C51 O5 Ti2 127.8(6) . 2_655 ? C51 O5 Pb1 127.7(6) . . ? Ti2 O5 Pb1 103.6(2) 2_655 . ? C81 O8 Ti1 125.6(6) . . ? C81 O8 Pb1 133.2(6) . . ? Ti1 O8 Pb1 101.0(2) . . ? Ti1 O1 Pb1 120.10(16) . 2_655 ? Ti1 O1 Pb1 120.10(16) . . ? Pb1 O1 Pb1 119.8(3) 2_655 . ? C31 O3 Ti1 139.5(9) . . ? C61 O6 Ti2 138.5(7) . . ? C41 O9 Ti2 136.7(6) 2_655 . ? Ti2 O2 Ti2 136.2(4) 2_655 . ? Ti2 O2 Pb1 104.46(9) 2_655 2_655 ? Ti2 O2 Pb1 103.64(9) . 2_655 ? Ti2 O2 Pb1 103.64(9) 2_655 . ? Ti2 O2 Pb1 104.46(9) . . ? Pb1 O2 Pb1 98.8(2) 2_655 . ? C71 O7 Ti2 129.1(7) . . ? C71 O7 Pb1 124.2(7) . . ? Ti2 O7 Pb1 102.6(2) . . ? O3 Ti1 O3 105.3(4) . 2_655 ? O3 Ti1 O1 127.4(2) . . ? O3 Ti1 O1 127.4(2) 2_655 . ? O3 Ti1 O8 97.5(3) . 2_655 ? O3 Ti1 O8 97.1(3) 2_655 2_655 ? O1 Ti1 O8 77.89(17) . 2_655 ? O3 Ti1 O8 97.1(3) . . ? O3 Ti1 O8 97.5(3) 2_655 . ? O1 Ti1 O8 77.89(17) . . ? O8 Ti1 O8 155.8(3) 2_655 . ? O3 Ti1 Pb1 119.4(2) . 2_655 ? O3 Ti1 Pb1 122.3(2) 2_655 2_655 ? O1 Ti1 Pb1 32.302(17) . 2_655 ? O8 Ti1 Pb1 45.65(17) 2_655 2_655 ? O8 Ti1 Pb1 110.14(18) . 2_655 ? O3 Ti1 Pb1 122.3(2) . . ? O3 Ti1 Pb1 119.4(2) 2_655 . ? O1 Ti1 Pb1 32.302(17) . . ? O8 Ti1 Pb1 110.14(18) 2_655 . ? O8 Ti1 Pb1 45.65(17) . . ? Pb1 Ti1 Pb1 64.60(3) 2_655 . ? O6 Ti2 O5 98.7(3) . 2_655 ? O6 Ti2 O7 99.0(3) . . ? O5 Ti2 O7 95.9(3) 2_655 . ? O6 Ti2 O2 169.6(3) . . ? O5 Ti2 O2 87.8(2) 2_655 . ? O7 Ti2 O2 88.3(2) . . ? O6 Ti2 O4 86.0(3) . . ? O5 Ti2 O4 172.2(3) 2_655 . ? O7 Ti2 O4 89.4(3) . . ? O2 Ti2 O4 86.7(2) . . ? O6 Ti2 O9 85.7(3) . . ? O5 Ti2 O9 89.1(3) 2_655 . ? O7 Ti2 O9 172.5(3) . . ? O2 Ti2 O9 86.3(2) . . ? O4 Ti2 O9 85.1(3) . . ? O6 Ti2 Pb1 141.8(2) . 2_655 ? O5 Ti2 Pb1 44.43(19) 2_655 2_655 ? O7 Ti2 Pb1 95.29(18) . 2_655 ? O2 Ti2 Pb1 43.45(11) . 2_655 ? O4 Ti2 Pb1 129.52(19) . 2_655 ? O9 Ti2 Pb1 84.34(17) . 2_655 ? O6 Ti2 Pb1 143.3(2) . . ? O5 Ti2 Pb1 94.84(18) 2_655 . ? O7 Ti2 Pb1 45.48(19) . . ? O2 Ti2 Pb1 42.97(11) . . ? O4 Ti2 Pb1 84.81(18) . . ? O9 Ti2 Pb1 128.64(18) . . ? Pb1 Ti2 Pb1 64.82(3) 2_655 . ? O1 Pb1 O2 70.7(2) . . ? O1 Pb1 O5 94.09(16) . . ? O2 Pb1 O5 64.78(13) . . ? O1 Pb1 O8 60.9(2) . . ? O2 Pb1 O8 131.51(17) . . ? O5 Pb1 O8 114.5(2) . . ? O1 Pb1 O7 93.42(16) . . ? O2 Pb1 O7 64.46(12) . . ? O5 Pb1 O7 122.42(18) . . ? O8 Pb1 O7 118.8(2) . . ? O1 Pb1 Ti2 82.82(14) . 2_655 ? O2 Pb1 Ti2 32.90(4) . 2_655 ? O5 Pb1 Ti2 31.95(13) . 2_655 ? O8 Pb1 Ti2 130.98(16) . 2_655 ? O7 Pb1 Ti2 93.32(13) . 2_655 ? O1 Pb1 Ti2 82.35(14) . . ? O2 Pb1 Ti2 32.57(4) . . ? O5 Pb1 Ti2 93.34(13) . . ? O8 Pb1 Ti2 134.05(15) . . ? O7 Pb1 Ti2 31.95(12) . . ? Ti2 Pb1 Ti2 62.29(5) 2_655 . ? O1 Pb1 Ti1 27.60(16) . . ? O2 Pb1 Ti1 98.29(12) . . ? O5 Pb1 Ti1 106.50(14) . . ? O8 Pb1 Ti1 33.34(12) . . ? O7 Pb1 Ti1 105.91(14) . . ? Ti2 Pb1 Ti1 106.32(3) 2_655 . ? Ti2 Pb1 Ti1 105.91(3) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 24.09 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.956 _refine_diff_density_min -0.929 _refine_diff_density_rms 0.181 #========END #=========================================================================== #=============================================================== data_AB43 _database_code_depnum_ccdc_archive 'CCDC 230778' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H112 O17 Pb2 Zr2' _chemical_formula_sum 'C54 H112 O17 Pb2 Zr2' _chemical_compound_source 'synthesis as described' _chemical_formula_weight 1630.26 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' O O 0.0106 0.0060 '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' Zr Zr -2.9673 0.5597 '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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3776(10) _cell_length_b 13.1183(12) _cell_length_c 26.190(3) _cell_angle_alpha 85.559(8) _cell_angle_beta 83.667(7) _cell_angle_gamma 76.410(8) _cell_volume 3771.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 6226 _cell_measurement_theta_min 3.31 _cell_measurement_theta_max 23.21 _exptl_crystal_description 'flat box' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 4.772 _exptl_absorpt_correction_T_min 0.30423 _exptl_absorpt_correction_T_max 0.48701 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++) (compiled Jun 6 2003,13:53:32) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type ? _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford-Diffraction XCALIBUR' _diffrn_measurement_method \w-\f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 20240 _diffrn_reflns_av_R_equivalents 0.0674 _diffrn_reflns_av_sigmaI/netI 0.0996 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 23.21 _diffrn_orient_matrix_UB_11 0.0588890499 _diffrn_orient_matrix_UB_12 -0.0325913467 _diffrn_orient_matrix_UB_13 -0.0049040321 _diffrn_orient_matrix_UB_21 0.0217084697 _diffrn_orient_matrix_UB_22 0.0257243571 _diffrn_orient_matrix_UB_23 0.0185913572 _diffrn_orient_matrix_UB_31 -0.0145593022 _diffrn_orient_matrix_UB_32 -0.0371382891 _diffrn_orient_matrix_UB_33 0.0193635544 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -54.00 60.75 0.7500 20.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 26.0000 -79.0000 0.0000 0.0000 0.0000 153 #__ type_ start__ end____ width___ exp.time_ 2 omega -54.00 60.75 0.7500 20.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 26.0000 -79.0000 90.0000 0.0000 0.0000 153 #__ type_ start__ end____ width___ exp.time_ 3 omega -54.00 60.75 0.7500 20.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 26.0000 -79.0000 180.0000 0.0000 0.0000 153 #__ type_ start__ end____ width___ exp.time_ 4 omega -54.00 60.75 0.7500 20.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 26.0000 -79.0000 270.0000 0.0000 0.0000 153 ; _reflns_number_total 10765 _reflns_number_gt 6832 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++) (compiled Jun 6 2003,13:53:32) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++) (compiled Jun 6 2003,13:53:32) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++) (compiled Jun 6 2003,13:53:32) ; _computing_structure_solution 'SIR-97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0809P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10765 _refine_ls_number_parameters 692 _refine_ls_number_restraints 772 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1225 _refine_ls_wR_factor_gt 0.1165 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.110 _refine_ls_shift/su_mean 0.003 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 C11 C 0.8493(14) 0.2444(11) 0.0813(6) 0.079(4) Uani 1 1 d U . . C41 C 0.3293(13) 0.5284(10) 0.3026(5) 0.061(3) Uani 1 1 d U . . C43 C 0.4919(15) 0.2696(10) 0.4179(5) 0.075(4) Uani 1 1 d U . . C45 C 0.6837(14) 0.4775(14) 0.4286(5) 0.089(4) Uani 1 1 d U . . C111 C 0.9292(19) 0.2009(14) 0.0353(6) 0.123(5) Uani 1 1 d DU . . H111 H 0.8961 0.1419 0.0275 0.147 Uiso 1 1 calc R . . C112 C 1.0557(19) 0.1474(19) 0.0518(8) 0.170(8) Uani 1 1 d DU . . H11A H 1.0876 0.1995 0.0668 0.204 Uiso 1 1 calc R . . H11B H 1.0461 0.0941 0.0787 0.204 Uiso 1 1 calc R . . C113 C 1.148(2) 0.097(2) 0.0109(10) 0.216(12) Uani 1 1 d DU . . H11C H 1.2073 0.0425 0.0262 0.324 Uiso 1 1 calc R . . H11D H 1.1871 0.1492 -0.0067 0.324 Uiso 1 1 calc R . . H11E H 1.1087 0.0683 -0.0132 0.324 Uiso 1 1 calc R . . C114 C 0.912(2) 0.273(2) -0.0117(8) 0.181(8) Uani 1 1 d DU . . H11F H 0.9782 0.2549 -0.0384 0.217 Uiso 1 1 calc R . . H11G H 0.9011 0.3462 -0.0039 0.217 Uiso 1 1 calc R . . C115 C 0.794(3) 0.250(3) -0.0259(13) 0.251(11) Uani 1 1 d DU . . H11H H 0.7702 0.2020 0.0013 0.301 Uiso 1 1 calc R . . H11I H 0.7328 0.3149 -0.0234 0.301 Uiso 1 1 calc R . . C116 C 0.781(4) 0.205(4) -0.0754(15) 0.260(14) Uani 1 1 d DU . . H11J H 0.8145 0.2465 -0.1032 0.312 Uiso 1 1 calc R . . H11K H 0.8311 0.1347 -0.0760 0.312 Uiso 1 1 calc R . . C117 C 0.686(4) 0.202(4) -0.0848(18) 0.31(2) Uani 1 1 d U . . H11L H 0.6701 0.1348 -0.0725 0.461 Uiso 1 1 calc R . . H11M H 0.6822 0.2099 -0.1213 0.461 Uiso 1 1 calc R . . H11N H 0.6263 0.2567 -0.0684 0.461 Uiso 1 1 calc R . . C121 C 1.0199(12) 0.4837(12) 0.1641(6) 0.080(4) Uani 1 1 d U . . H121 H 1.0577 0.4549 0.1956 0.097 Uiso 1 1 calc R . . C122 C 1.0051(17) 0.6007(13) 0.1610(8) 0.130(7) Uani 1 1 d U . . H12A H 1.0832 0.6169 0.1609 0.196 Uiso 1 1 calc R . . H12B H 0.9531 0.6301 0.1902 0.196 Uiso 1 1 calc R . . H12C H 0.9697 0.6299 0.1300 0.196 Uiso 1 1 calc R . . C123 C 1.0981(15) 0.4335(14) 0.1195(7) 0.111(6) Uani 1 1 d U . . H12D H 1.0889 0.3629 0.1183 0.166 Uiso 1 1 calc R . . H12E H 1.1814 0.4325 0.1232 0.166 Uiso 1 1 calc R . . H12F H 1.0745 0.4727 0.0884 0.166 Uiso 1 1 calc R . . C131 C 0.6853(17) 0.6285(11) 0.0632(5) 0.090(4) Uani 1 1 d U . . H131 H 0.6077 0.6271 0.0506 0.108 Uiso 1 1 calc R . . C132 C 0.674(3) 0.7330(12) 0.0789(8) 0.174(11) Uani 1 1 d U . . H13A H 0.5952 0.7580 0.0963 0.261 Uiso 1 1 calc R . . H13B H 0.6857 0.7785 0.0491 0.261 Uiso 1 1 calc R . . H13C H 0.7351 0.7325 0.1017 0.261 Uiso 1 1 calc R . . C133 C 0.7840(17) 0.5930(14) 0.0196(6) 0.114(6) Uani 1 1 d U . . H13D H 0.8623 0.5886 0.0312 0.170 Uiso 1 1 calc R . . H13E H 0.7723 0.6428 -0.0092 0.170 Uiso 1 1 calc R . . H13F H 0.7795 0.5253 0.0096 0.170 Uiso 1 1 calc R . . C141 C 0.4888(13) 0.4016(11) 0.1221(5) 0.073(3) Uani 1 1 d U . . H141 H 0.4354 0.3535 0.1328 0.087 Uiso 1 1 calc R . . C142 C 0.5202(14) 0.3998(12) 0.0637(5) 0.087(4) Uani 1 1 d U . . H14A H 0.5816 0.4386 0.0536 0.131 Uiso 1 1 calc R . . H14B H 0.4488 0.4312 0.0467 0.131 Uiso 1 1 calc R . . H14C H 0.5499 0.3285 0.0541 0.131 Uiso 1 1 calc R . . C143 C 0.4246(12) 0.5109(10) 0.1372(5) 0.071(3) Uani 1 1 d U . . H14D H 0.4747 0.5590 0.1253 0.107 Uiso 1 1 calc R . . H14E H 0.4092 0.5115 0.1740 0.107 Uiso 1 1 calc R . . H14F H 0.3490 0.5316 0.1220 0.107 Uiso 1 1 calc R . . C221 C 0.476(2) 0.1092(16) 0.1008(8) 0.150(6) Uani 1 1 d DU . . H221 H 0.4083 0.1583 0.0857 0.180 Uiso 1 1 calc R . . C222 C 0.445(4) 0.015(2) 0.1302(12) 0.150(6) Uani 0.50 1 d PDU . . H22A H 0.3827 0.0371 0.1574 0.225 Uiso 0.50 1 calc PR . . H22B H 0.5162 -0.0269 0.1446 0.225 Uiso 0.50 1 calc PR . . H22C H 0.4170 -0.0262 0.1074 0.225 Uiso 0.50 1 calc PR . . C223 C 0.578(3) 0.057(3) 0.0630(14) 0.150(6) Uani 0.50 1 d PDU . . H22D H 0.6066 0.1103 0.0411 0.225 Uiso 0.50 1 calc PR . . H22E H 0.5488 0.0127 0.0425 0.225 Uiso 0.50 1 calc PR . . H22F H 0.6430 0.0164 0.0814 0.225 Uiso 0.50 1 calc PR . . C231 C 0.8241(19) -0.0293(12) 0.2076(8) 0.116(6) Uani 1 1 d U . . H231 H 0.8986 -0.0156 0.2182 0.140 Uiso 1 1 calc R . . C232 C 0.856(3) -0.0768(14) 0.1598(9) 0.177(10) Uani 1 1 d U . . H23A H 0.7883 -0.1001 0.1501 0.266 Uiso 1 1 calc R . . H23B H 0.9238 -0.1358 0.1628 0.266 Uiso 1 1 calc R . . H23C H 0.8782 -0.0267 0.1340 0.266 Uiso 1 1 calc R . . C233 C 0.776(2) -0.0912(15) 0.2493(11) 0.202(12) Uani 1 1 d U . . H23D H 0.7474 -0.0487 0.2783 0.303 Uiso 1 1 calc R . . H23E H 0.8392 -0.1502 0.2587 0.303 Uiso 1 1 calc R . . H23F H 0.7104 -0.1158 0.2384 0.303 Uiso 1 1 calc R . . C241 C 0.8644(12) 0.2431(10) 0.2357(5) 0.065(3) Uani 1 1 d U . . H241 H 0.8392 0.1856 0.2569 0.078 Uiso 1 1 calc R . . C242 C 0.8971(13) 0.3140(11) 0.2721(5) 0.079(4) Uani 1 1 d U . . H24A H 0.9222 0.3717 0.2527 0.118 Uiso 1 1 calc R . . H24B H 0.9622 0.2749 0.2910 0.118 Uiso 1 1 calc R . . H24C H 0.8276 0.3404 0.2956 0.118 Uiso 1 1 calc R . . C243 C 0.9746(13) 0.1948(12) 0.2015(6) 0.088(4) Uani 1 1 d U . . H24D H 0.9571 0.1403 0.1831 0.131 Uiso 1 1 calc R . . H24E H 1.0406 0.1654 0.2220 0.131 Uiso 1 1 calc R . . H24F H 0.9967 0.2476 0.1773 0.131 Uiso 1 1 calc R . . C311 C 0.6509(16) 0.6147(10) 0.2311(6) 0.089(4) Uani 1 1 d U . . H311 H 0.7052 0.6337 0.2021 0.106 Uiso 1 1 calc R . . C312 C 0.7256(17) 0.6096(11) 0.2746(5) 0.090(4) Uani 1 1 d U . . H31A H 0.8053 0.5668 0.2662 0.135 Uiso 1 1 calc R . . H31B H 0.6879 0.5796 0.3049 0.135 Uiso 1 1 calc R . . H31C H 0.7318 0.6792 0.2810 0.135 Uiso 1 1 calc R . . C313 C 0.543(2) 0.6898(13) 0.2238(9) 0.142(8) Uani 1 1 d U . . H31D H 0.5270 0.6938 0.1883 0.214 Uiso 1 1 calc R . . H31E H 0.5503 0.7571 0.2331 0.214 Uiso 1 1 calc R . . H31F H 0.4765 0.6696 0.2449 0.214 Uiso 1 1 calc R . . C321 C 0.4226(12) 0.2162(11) 0.2610(5) 0.070(3) Uani 1 1 d U . . H321 H 0.4002 0.2463 0.2947 0.084 Uiso 1 1 calc R . . C322 C 0.3190(13) 0.2552(12) 0.2296(5) 0.084(4) Uani 1 1 d U . . H32A H 0.3131 0.3281 0.2199 0.126 Uiso 1 1 calc R . . H32B H 0.2453 0.2467 0.2494 0.126 Uiso 1 1 calc R . . H32C H 0.3315 0.2159 0.1993 0.126 Uiso 1 1 calc R . . C323 C 0.4569(15) 0.0960(10) 0.2695(5) 0.088(4) Uani 1 1 d U . . H32D H 0.4755 0.0645 0.2368 0.132 Uiso 1 1 calc R . . H32E H 0.3900 0.0724 0.2883 0.132 Uiso 1 1 calc R . . H32F H 0.5266 0.0760 0.2887 0.132 Uiso 1 1 calc R . . C411 C 0.1952(14) 0.5717(14) 0.3067(8) 0.109(5) Uani 1 1 d DU . . H411 H 0.1878 0.6037 0.3399 0.130 Uiso 1 1 calc R . . C412 C 0.1189(17) 0.4960(17) 0.3226(10) 0.165(8) Uani 1 1 d DU . . H41A H 0.0410 0.5362 0.3369 0.198 Uiso 1 1 calc R . . H41B H 0.1044 0.4674 0.2914 0.198 Uiso 1 1 calc R . . C413 C 0.1565(17) 0.4063(16) 0.3592(8) 0.147(8) Uani 1 1 d DU . . H41C H 0.0939 0.3677 0.3654 0.220 Uiso 1 1 calc R . . H41D H 0.1699 0.4314 0.3911 0.220 Uiso 1 1 calc R . . H41E H 0.2302 0.3612 0.3452 0.220 Uiso 1 1 calc R . . C414 C 0.1538(18) 0.6565(19) 0.2796(11) 0.178(8) Uani 1 1 d DU . . H414A H 0.0714 0.6828 0.2946 0.214 Uiso 1 1 calc R . . H414B H 0.1465 0.6332 0.2461 0.214 Uiso 1 1 calc R . . C415 C 0.205(2) 0.7496(16) 0.2690(11) 0.175(8) Uani 1 1 d DU . . H415C H 0.2214 0.7660 0.3026 0.210 Uiso 1 1 calc R . . H415D H 0.2841 0.7227 0.2509 0.210 Uiso 1 1 calc R . . C416 C 0.164(3) 0.849(2) 0.2440(15) 0.237(12) Uani 1 1 d DU . . H416E H 0.0918 0.8832 0.2651 0.285 Uiso 1 1 calc R . . H416F H 0.1357 0.8352 0.2122 0.285 Uiso 1 1 calc R . . C417 C 0.234(3) 0.930(2) 0.2302(15) 0.247(15) Uani 1 1 d DU . . H41G H 0.2312 0.9709 0.2594 0.370 Uiso 1 1 calc R . . H41H H 0.1991 0.9758 0.2025 0.370 Uiso 1 1 calc R . . H41I H 0.3166 0.8974 0.2195 0.370 Uiso 1 1 calc R . . C431 C 0.507(2) 0.1535(12) 0.4175(7) 0.126(6) Uani 1 1 d U . . H431 H 0.4889 0.1429 0.3828 0.152 Uiso 1 1 calc R . . C432 C 0.633(3) 0.1018(16) 0.4183(11) 0.175(9) Uani 1 1 d U . . H43A H 0.6570 0.1158 0.4509 0.210 Uiso 1 1 calc R . . H43B H 0.6367 0.0270 0.4192 0.210 Uiso 1 1 calc R . . C433 C 0.722(3) 0.121(3) 0.3806(11) 0.249(16) Uani 1 1 d U . . H43C H 0.8005 0.0825 0.3899 0.373 Uiso 1 1 calc R . . H43D H 0.7206 0.1948 0.3778 0.373 Uiso 1 1 calc R . . H43E H 0.7079 0.0991 0.3482 0.373 Uiso 1 1 calc R . . C434 C 0.423(3) 0.1085(19) 0.4500(12) 0.173(9) Uani 1 1 d U . . H43F H 0.4413 0.0340 0.4442 0.207 Uiso 1 1 calc R . . H43G H 0.4373 0.1153 0.4853 0.207 Uiso 1 1 calc R . . C435 C 0.310(3) 0.146(2) 0.4452(13) 0.200(12) Uani 1 1 d U . . H43H H 0.2619 0.1142 0.4714 0.300 Uiso 1 1 calc R . . H43I H 0.2914 0.1318 0.4119 0.300 Uiso 1 1 calc R . . H43J H 0.2907 0.2208 0.4487 0.300 Uiso 1 1 calc R . . C451 C 0.8154(16) 0.4728(17) 0.4286(7) 0.131(5) Uani 1 1 d DU . . H451 H 0.8554 0.4532 0.3946 0.157 Uiso 1 1 calc R . . C452 C 0.843(2) 0.575(2) 0.4401(11) 0.191(9) Uani 1 1 d DU . . H45A H 0.9308 0.5630 0.4385 0.230 Uiso 1 1 calc R . . H45B H 0.8122 0.5879 0.4756 0.230 Uiso 1 1 calc R . . C453 C 0.798(4) 0.675(2) 0.4081(13) 0.275(17) Uani 1 1 d DU . . H45C H 0.8210 0.7327 0.4220 0.412 Uiso 1 1 calc R . . H45D H 0.7110 0.6897 0.4089 0.412 Uiso 1 1 calc R . . H45E H 0.8331 0.6675 0.3732 0.412 Uiso 1 1 calc R . . C454 C 0.8777(19) 0.395(2) 0.4683(9) 0.169(8) Uani 1 1 d DU . . H45F H 0.9624 0.3978 0.4674 0.203 Uiso 1 1 calc R . . H45G H 0.8386 0.4107 0.5025 0.203 Uiso 1 1 calc R . . C455 C 0.867(3) 0.289(2) 0.4544(13) 0.238(14) Uani 1 1 d DU . . H45H H 0.9075 0.2357 0.4779 0.357 Uiso 1 1 calc R . . H45I H 0.9035 0.2755 0.4200 0.357 Uiso 1 1 calc R . . H45J H 0.7827 0.2867 0.4563 0.357 Uiso 1 1 calc R . . C471 C 0.420(2) 0.7967(15) 0.4169(7) 0.144(8) Uani 1 1 d U . . H471 H 0.4439 0.8480 0.4363 0.173 Uiso 1 1 calc R . . C472 C 0.280(3) 0.824(3) 0.4159(14) 0.287(19) Uani 1 1 d U . . H47A H 0.2598 0.7949 0.3864 0.431 Uiso 1 1 calc R . . H47B H 0.2509 0.8986 0.4141 0.431 Uiso 1 1 calc R . . H47C H 0.2439 0.7943 0.4466 0.431 Uiso 1 1 calc R . . C473 C 0.469(3) 0.8010(19) 0.3657(9) 0.226(14) Uani 1 1 d U . . H47D H 0.4518 0.8725 0.3521 0.339 Uiso 1 1 calc R . . H47E H 0.4343 0.7593 0.3458 0.339 Uiso 1 1 calc R . . H47F H 0.5555 0.7742 0.3641 0.339 Uiso 1 1 calc R . . O11 O 0.8468(8) 0.3341(6) 0.0951(3) 0.065(2) Uani 1 1 d U . . O12 O 0.9043(7) 0.4637(6) 0.1677(3) 0.062(2) Uani 1 1 d U . . O13 O 0.7033(8) 0.5520(6) 0.1047(3) 0.062(2) Uani 1 1 d U . . O14 O 0.6003(7) 0.3650(5) 0.1452(3) 0.0476(16) Uani 1 1 d U . . O21 O 0.7849(8) 0.1866(6) 0.1060(3) 0.066(2) Uani 1 1 d U . . O22 O 0.5391(8) 0.1536(6) 0.1353(3) 0.067(2) Uani 1 1 d U . . O23 O 0.7414(8) 0.0701(6) 0.2020(3) 0.074(2) Uani 1 1 d U . . O24 O 0.7651(7) 0.2928(5) 0.2063(3) 0.0487(16) Uani 1 1 d U . . O31 O 0.6480(7) 0.5084(5) 0.2193(3) 0.0503(17) Uani 1 1 d U . . O32 O 0.5293(7) 0.2508(5) 0.2376(3) 0.0516(17) Uani 1 1 d U . . O41 O 0.3927(8) 0.5536(6) 0.3322(3) 0.066(2) Uani 1 1 d U . . O42 O 0.3687(8) 0.4684(6) 0.2672(3) 0.0600(19) Uani 1 1 d U . . O43 O 0.4631(8) 0.3254(6) 0.3779(3) 0.067(2) Uani 1 1 d U . . O44 O 0.5000(10) 0.3110(6) 0.4589(3) 0.079(3) Uani 1 1 d U . . O45 O 0.6379(8) 0.4731(7) 0.3881(3) 0.070(2) Uani 1 1 d U . . O46 O 0.6164(8) 0.4913(6) 0.4704(3) 0.065(2) Uani 1 1 d U . . O47 O 0.4510(13) 0.6989(7) 0.4403(4) 0.116(4) Uani 1 1 d U . . Pb3 Pb 0.57065(4) 0.38985(3) 0.281130(16) 0.04984(16) Uani 1 1 d U . . Pb4 Pb 0.43329(5) 0.49537(4) 0.427624(17) 0.05615(17) Uani 1 1 d U . . Zr1 Zr 0.74960(11) 0.43884(8) 0.15482(4) 0.0472(3) Uani 1 1 d U . . Zr2 Zr 0.65009(11) 0.20236(8) 0.17390(4) 0.0498(3) Uani 1 1 d U . . 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 C11 0.085(9) 0.074(8) 0.082(8) -0.019(6) 0.012(6) -0.030(7) C41 0.062(6) 0.057(7) 0.066(7) -0.006(5) -0.013(6) -0.010(5) C43 0.110(11) 0.058(5) 0.058(7) -0.001(5) -0.004(8) -0.024(7) C45 0.074(5) 0.159(12) 0.047(6) -0.015(7) 0.002(5) -0.055(7) C111 0.154(11) 0.118(11) 0.100(10) -0.039(7) 0.059(8) -0.060(10) C112 0.139(13) 0.196(19) 0.153(15) -0.066(13) 0.076(11) -0.017(13) C113 0.183(18) 0.24(3) 0.21(2) -0.10(2) 0.098(19) -0.031(18) C114 0.204(18) 0.225(18) 0.122(11) 0.006(11) 0.057(12) -0.105(15) C115 0.23(2) 0.33(3) 0.21(2) -0.029(18) -0.029(17) -0.09(2) C116 0.29(3) 0.26(3) 0.25(3) -0.04(2) -0.04(2) -0.09(3) C117 0.35(4) 0.28(4) 0.32(4) 0.02(3) -0.19(4) -0.05(4) C121 0.054(7) 0.099(9) 0.101(10) -0.011(8) -0.008(7) -0.039(8) C122 0.111(15) 0.108(10) 0.197(19) -0.056(12) 0.022(13) -0.077(11) C123 0.074(10) 0.126(12) 0.140(15) -0.036(10) 0.024(9) -0.046(10) C131 0.129(13) 0.078(8) 0.064(8) 0.019(6) -0.004(7) -0.036(9) C132 0.31(3) 0.061(7) 0.130(16) 0.028(8) 0.033(17) -0.034(14) C133 0.127(15) 0.130(13) 0.083(10) 0.022(9) 0.021(9) -0.052(12) C141 0.074(8) 0.076(7) 0.073(7) 0.002(6) -0.054(7) -0.007(6) C142 0.107(12) 0.103(11) 0.070(7) 0.006(7) -0.059(8) -0.040(9) C143 0.059(8) 0.078(8) 0.085(9) 0.009(6) -0.037(7) -0.022(6) C221 0.204(15) 0.156(12) 0.141(12) -0.081(9) -0.021(10) -0.116(11) C222 0.204(15) 0.156(12) 0.141(12) -0.081(9) -0.021(10) -0.116(11) C223 0.204(15) 0.156(12) 0.141(12) -0.081(9) -0.021(10) -0.116(11) C231 0.119(14) 0.053(8) 0.160(14) 0.003(7) 0.002(12) 0.004(7) C232 0.24(3) 0.075(12) 0.194(16) -0.051(11) -0.063(17) 0.047(13) C233 0.20(2) 0.079(13) 0.28(2) 0.093(13) 0.02(2) 0.017(15) C241 0.059(7) 0.061(7) 0.077(9) 0.004(5) -0.029(5) -0.011(6) C242 0.068(9) 0.104(10) 0.081(9) 0.005(7) -0.025(7) -0.047(8) C243 0.067(8) 0.086(10) 0.101(11) 0.011(7) -0.020(7) -0.001(7) C311 0.121(12) 0.046(6) 0.109(10) -0.014(6) -0.025(8) -0.029(7) C312 0.160(14) 0.078(9) 0.051(8) -0.015(6) 0.001(7) -0.063(9) C313 0.156(18) 0.070(9) 0.20(2) -0.051(12) -0.049(15) 0.003(9) C321 0.067(8) 0.087(7) 0.069(8) -0.008(6) 0.006(5) -0.049(7) C322 0.063(8) 0.118(11) 0.082(10) -0.018(8) 0.007(7) -0.047(8) C323 0.124(12) 0.083(7) 0.080(10) 0.000(7) 0.003(9) -0.076(8) C411 0.058(6) 0.111(10) 0.149(14) -0.012(9) -0.015(8) 0.001(7) C412 0.061(10) 0.189(17) 0.24(2) 0.029(14) 0.006(13) -0.030(11) C413 0.088(14) 0.168(17) 0.19(2) 0.009(12) 0.022(13) -0.053(14) C414 0.070(12) 0.179(15) 0.27(2) 0.064(15) -0.052(14) -0.007(10) C415 0.124(16) 0.131(14) 0.26(2) 0.021(15) -0.056(16) -0.005(11) C416 0.15(2) 0.183(18) 0.35(3) 0.08(2) -0.06(2) -0.009(15) C417 0.22(3) 0.127(18) 0.39(4) 0.04(2) -0.07(3) -0.017(17) C431 0.211(16) 0.053(6) 0.097(11) -0.006(6) 0.015(12) -0.008(9) C432 0.217(17) 0.082(12) 0.21(2) -0.055(15) -0.008(16) 0.012(11) C433 0.23(2) 0.29(3) 0.17(2) -0.10(2) 0.046(19) 0.06(2) C434 0.26(2) 0.092(15) 0.19(2) 0.028(14) -0.02(2) -0.094(17) C435 0.244(19) 0.16(3) 0.20(3) 0.02(2) 0.02(3) -0.09(3) C451 0.075(7) 0.244(16) 0.089(11) -0.029(11) 0.007(7) -0.068(11) C452 0.113(16) 0.291(19) 0.21(2) -0.048(17) 0.034(15) -0.138(16) C453 0.33(4) 0.24(2) 0.24(4) -0.07(2) 0.04(3) -0.07(3) C454 0.077(11) 0.31(2) 0.119(15) -0.024(15) -0.020(11) -0.031(16) C455 0.18(3) 0.250(18) 0.27(4) 0.01(2) -0.06(3) 0.01(3) C471 0.22(2) 0.099(11) 0.079(10) 0.038(10) -0.028(13) 0.020(15) C472 0.22(2) 0.31(4) 0.25(3) 0.07(3) -0.01(2) 0.09(2) C473 0.33(3) 0.154(19) 0.120(15) 0.062(14) 0.05(2) 0.04(2) O11 0.067(5) 0.067(5) 0.064(5) -0.006(4) 0.006(4) -0.027(4) O12 0.049(4) 0.067(5) 0.079(6) -0.007(4) -0.004(4) -0.028(4) O13 0.077(6) 0.063(4) 0.056(4) 0.013(3) -0.010(4) -0.038(4) O14 0.047(4) 0.053(4) 0.048(4) 0.000(3) -0.009(3) -0.021(3) O21 0.079(6) 0.058(4) 0.063(5) -0.015(4) 0.006(4) -0.022(4) O22 0.087(6) 0.061(5) 0.062(5) -0.016(4) -0.009(4) -0.035(4) O23 0.081(6) 0.042(4) 0.097(6) 0.004(4) -0.005(5) -0.017(4) O24 0.049(4) 0.048(4) 0.052(4) 0.003(3) -0.012(3) -0.014(3) O31 0.061(5) 0.046(4) 0.052(4) -0.003(3) -0.004(3) -0.028(4) O32 0.063(4) 0.053(4) 0.047(4) -0.003(3) -0.006(3) -0.028(3) O41 0.078(6) 0.063(5) 0.057(5) -0.003(4) -0.009(4) -0.017(5) O42 0.062(5) 0.067(5) 0.057(5) -0.010(4) -0.012(4) -0.020(4) O43 0.089(7) 0.065(5) 0.049(4) -0.001(3) -0.004(4) -0.024(5) O44 0.116(8) 0.060(5) 0.063(5) 0.001(4) -0.019(5) -0.021(5) O45 0.073(5) 0.102(6) 0.036(4) 0.000(4) -0.003(3) -0.025(5) O46 0.063(5) 0.083(6) 0.050(4) -0.002(4) -0.001(3) -0.021(5) O47 0.216(13) 0.053(5) 0.081(7) 0.013(5) -0.051(8) -0.024(7) Pb3 0.0547(3) 0.0570(3) 0.0433(3) -0.0044(2) -0.0048(2) -0.0229(2) Pb4 0.0650(4) 0.0583(3) 0.0448(3) -0.0043(2) 0.0001(2) -0.0153(3) Zr1 0.0523(7) 0.0502(7) 0.0456(6) 0.0006(5) -0.0067(5) -0.0246(6) Zr2 0.0604(8) 0.0459(6) 0.0492(7) -0.0045(5) -0.0067(6) -0.0229(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic= ) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C11 O11 1.251(14) . ? C11 O21 1.269(15) . ? C11 C111 1.49(2) . ? C41 O41 1.226(14) . ? C41 O42 1.238(14) . ? C41 C411 1.49(2) . ? C43 O43 1.259(15) . ? C43 O44 1.263(15) . ? C43 C431 1.492(19) . ? C45 O45 1.245(15) . ? C45 O46 1.264(15) . ? C45 C451 1.49(2) . ? C45 Pb4 2.807(15) . ? C111 C114 1.497(16) . ? C111 C112 1.539(17) . ? C112 C113 1.489(16) . ? C114 C115 1.535(18) . ? C115 C116 1.497(19) . ? C116 C117 1.15(5) . ? C121 O12 1.392(14) . ? C121 C123 1.48(2) . ? C121 C122 1.50(2) . ? C131 O13 1.420(14) . ? C131 C132 1.43(2) . ? C131 C133 1.53(2) . ? C141 O14 1.429(14) . ? C141 C143 1.508(18) . ? C141 C142 1.534(18) . ? C221 O22 1.447(17) . ? C221 C222 1.499(14) . ? C221 C223 1.503(14) . ? C231 C232 1.41(3) . ? C231 O23 1.425(17) . ? C231 C233 1.44(2) . ? C241 O24 1.435(14) . ? C241 C243 1.497(18) . ? C241 C242 1.513(16) . ? C311 C313 1.41(2) . ? C311 O31 1.459(13) . ? C311 C312 1.48(2) . ? C321 O32 1.452(13) . ? C321 C322 1.479(19) . ? C321 C323 1.537(18) . ? C411 C414 1.29(2) . ? C411 C412 1.474(15) . ? C412 C413 1.473(13) . ? C414 C415 1.467(16) . ? C415 C416 1.416(17) . ? C416 C417 1.476(18) . ? C431 C434 1.41(3) . ? C431 C432 1.43(3) . ? C432 C433 1.39(3) . ? C434 C435 1.29(4) . ? C451 C452 1.500(17) . ? C451 C454 1.509(17) . ? C452 C453 1.524(18) . ? C454 C455 1.509(17) . ? C471 O47 1.364(18) . ? C471 C473 1.40(3) . ? C471 C472 1.54(4) . ? O11 Zr1 2.190(8) . ? O12 Zr1 1.934(8) . ? O13 Zr1 1.920(7) . ? O14 Zr2 2.171(7) . ? O14 Zr1 2.190(7) . ? O21 Zr2 2.206(8) . ? O22 Zr2 1.946(8) . ? O23 Zr2 1.938(8) . ? O24 Zr2 2.230(7) . ? O24 Zr1 2.239(7) . ? O24 Pb3 2.909(7) . ? O31 Zr1 2.082(7) . ? O31 Pb3 2.399(6) . ? O32 Zr2 2.079(7) . ? O32 Pb3 2.386(7) . ? O41 Pb4 2.615(8) . ? O41 Pb3 2.882(8) . ? O42 Pb3 2.343(8) . ? O43 Pb4 2.604(8) . ? O44 Pb4 2.463(8) . ? O45 Pb4 2.402(8) . ? O46 Pb4 2.460(8) . ? O46 Pb4 2.679(8) 2_666 ? Pb4 O46 2.679(8) 2_666 ? Zr1 Zr2 3.5272(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 C11 O21 121.5(12) . . ? O11 C11 C111 121.1(13) . . ? O21 C11 C111 117.4(13) . . ? O41 C41 O42 124.5(13) . . ? O41 C41 C411 120.7(13) . . ? O42 C41 C411 114.8(14) . . ? O43 C43 O44 120.9(12) . . ? O43 C43 C431 119.0(14) . . ? O44 C43 C431 120.0(13) . . ? O45 C45 O46 119.6(13) . . ? O45 C45 C451 121.4(13) . . ? O46 C45 C451 118.9(14) . . ? O45 C45 Pb4 58.5(7) . . ? O46 C45 Pb4 61.1(7) . . ? C451 C45 Pb4 177.6(14) . . ? C11 C111 C114 112.6(17) . . ? C11 C111 C112 109.0(14) . . ? C114 C111 C112 122.4(18) . . ? C113 C112 C111 117(2) . . ? C111 C114 C115 98.4(19) . . ? C116 C115 C114 124(3) . . ? C117 C116 C115 119(5) . . ? O12 C121 C123 111.6(12) . . ? O12 C121 C122 107.5(13) . . ? C123 C121 C122 112.2(13) . . ? O13 C131 C132 112.5(13) . . ? O13 C131 C133 108.1(13) . . ? C132 C131 C133 115.4(14) . . ? O14 C141 C143 112.0(10) . . ? O14 C141 C142 107.1(11) . . ? C143 C141 C142 110.5(11) . . ? O22 C221 C222 104.9(18) . . ? O22 C221 C223 102.5(18) . . ? C222 C221 C223 100(3) . . ? C232 C231 O23 110.8(17) . . ? C232 C231 C233 116.3(19) . . ? O23 C231 C233 109.2(16) . . ? O24 C241 C243 111.3(11) . . ? O24 C241 C242 114.4(10) . . ? C243 C241 C242 109.9(11) . . ? C313 C311 O31 114.1(14) . . ? C313 C311 C312 125.1(15) . . ? O31 C311 C312 109.4(11) . . ? O32 C321 C322 110.7(10) . . ? O32 C321 C323 108.3(11) . . ? C322 C321 C323 113.9(12) . . ? C414 C411 C412 120.7(17) . . ? C414 C411 C41 118.0(17) . . ? C412 C411 C41 116.3(15) . . ? C413 C412 C411 122.1(17) . . ? C411 C414 C415 128(2) . . ? C416 C415 C414 134(2) . . ? C415 C416 C417 127(2) . . ? C434 C431 C432 117(2) . . ? C434 C431 C43 117.1(19) . . ? C432 C431 C43 110(2) . . ? C433 C432 C431 123(3) . . ? C435 C434 C431 117(3) . . ? C45 C451 C452 114.0(17) . . ? C45 C451 C454 114.3(16) . . ? C452 C451 C454 103.7(19) . . ? C451 C452 C453 121(3) . . ? C451 C454 C455 106(2) . . ? O47 C471 C473 112.8(18) . . ? O47 C471 C472 107(2) . . ? C473 C471 C472 107(2) . . ? C11 O11 Zr1 137.8(8) . . ? C121 O12 Zr1 166.1(9) . . ? C131 O13 Zr1 171.3(9) . . ? C141 O14 Zr2 119.2(7) . . ? C141 O14 Zr1 132.7(7) . . ? Zr2 O14 Zr1 108.0(3) . . ? C11 O21 Zr2 135.8(8) . . ? C221 O22 Zr2 169.7(11) . . ? C231 O23 Zr2 163.3(10) . . ? C241 O24 Zr2 122.5(6) . . ? C241 O24 Zr1 127.4(7) . . ? Zr2 O24 Zr1 104.2(3) . . ? C241 O24 Pb3 105.4(7) . . ? Zr2 O24 Pb3 93.5(2) . . ? Zr1 O24 Pb3 93.6(2) . . ? C311 O31 Zr1 120.7(8) . . ? C311 O31 Pb3 122.6(8) . . ? Zr1 O31 Pb3 114.9(3) . . ? C321 O32 Zr2 132.0(7) . . ? C321 O32 Pb3 112.9(7) . . ? Zr2 O32 Pb3 115.1(3) . . ? C41 O41 Pb4 132.8(8) . . ? C41 O41 Pb3 80.4(7) . . ? Pb4 O41 Pb3 99.2(3) . . ? C41 O42 Pb3 106.1(8) . . ? C43 O43 Pb4 90.6(8) . . ? C43 O44 Pb4 97.2(8) . . ? C45 O45 Pb4 95.3(8) . . ? C45 O46 Pb4 92.1(8) . . ? C45 O46 Pb4 155.8(9) . 2_666 ? Pb4 O46 Pb4 111.8(3) . 2_666 ? O42 Pb3 O32 82.2(3) . . ? O42 Pb3 O31 92.6(3) . . ? O32 Pb3 O31 109.3(2) . . ? O42 Pb3 O41 48.0(3) . . ? O32 Pb3 O41 126.1(3) . . ? O31 Pb3 O41 94.3(2) . . ? O42 Pb3 O24 127.7(2) . . ? O32 Pb3 O24 65.1(2) . . ? O31 Pb3 O24 64.3(2) . . ? O41 Pb3 O24 158.6(2) . . ? O45 Pb4 O46 53.0(3) . . ? O45 Pb4 O44 84.7(3) . . ? O46 Pb4 O44 75.6(3) . . ? O45 Pb4 O43 77.2(3) . . ? O46 Pb4 O43 109.8(3) . . ? O44 Pb4 O43 51.2(3) . . ? O45 Pb4 O41 79.5(3) . . ? O46 Pb4 O41 128.2(3) . . ? O44 Pb4 O41 123.8(3) . . ? O43 Pb4 O41 72.7(3) . . ? O45 Pb4 O46 121.1(3) . 2_666 ? O46 Pb4 O46 68.2(3) . 2_666 ? O44 Pb4 O46 78.0(3) . 2_666 ? O43 Pb4 O46 125.5(2) . 2_666 ? O41 Pb4 O46 153.3(3) . 2_666 ? O45 Pb4 C45 26.2(3) . . ? O46 Pb4 C45 26.7(3) . . ? O44 Pb4 C45 78.9(4) . . ? O43 Pb4 C45 93.5(4) . . ? O41 Pb4 C45 103.9(4) . . ? O46 Pb4 C45 94.9(4) 2_666 . ? O13 Zr1 O12 99.0(3) . . ? O13 Zr1 O31 98.6(3) . . ? O12 Zr1 O31 97.5(3) . . ? O13 Zr1 O14 94.9(3) . . ? O12 Zr1 O14 163.9(3) . . ? O31 Zr1 O14 88.4(3) . . ? O13 Zr1 O11 91.7(3) . . ? O12 Zr1 O11 88.0(3) . . ? O31 Zr1 O11 167.4(3) . . ? O14 Zr1 O11 83.4(3) . . ? O13 Zr1 O24 165.5(3) . . ? O12 Zr1 O24 95.1(3) . . ? O31 Zr1 O24 82.7(3) . . ? O14 Zr1 O24 70.7(3) . . ? O11 Zr1 O24 85.5(3) . . ? O13 Zr1 Zr2 128.0(2) . . ? O12 Zr1 Zr2 128.2(2) . . ? O31 Zr1 Zr2 95.66(18) . . ? O14 Zr1 Zr2 35.84(19) . . ? O11 Zr1 Zr2 72.2(2) . . ? O24 Zr1 Zr2 37.79(18) . . ? O23 Zr2 O22 100.8(4) . . ? O23 Zr2 O32 99.9(3) . . ? O22 Zr2 O32 97.8(3) . . ? O23 Zr2 O14 162.0(3) . . ? O22 Zr2 O14 95.4(3) . . ? O32 Zr2 O14 85.5(3) . . ? O23 Zr2 O21 88.5(3) . . ? O22 Zr2 O21 89.9(3) . . ? O32 Zr2 O21 167.2(3) . . ? O14 Zr2 O21 83.7(3) . . ? O23 Zr2 O24 92.1(3) . . ? O22 Zr2 O24 166.4(3) . . ? O32 Zr2 O24 83.9(3) . . ? O14 Zr2 O24 71.2(3) . . ? O21 Zr2 O24 86.2(3) . . ? O23 Zr2 Zr1 125.8(3) . . ? O22 Zr2 Zr1 128.5(2) . . ? O32 Zr2 Zr1 94.63(18) . . ? O14 Zr2 Zr1 36.19(18) . . ? O21 Zr2 Zr1 72.6(2) . . ? O24 Zr2 Zr1 37.99(18) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 23.21 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.868 _refine_diff_density_min -1.206 _refine_diff_density_rms 0.147 #========END