#------------------------------------------------------------------------------ #$Date: 2008-01-26 15:05:32 +0200 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: file:///home/coder/svn-repositories/cod/cif/5/5000429.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_5000429 'minor manual editing of SDT2CIF v. 1.2 BETA output' _chemical_formula_sum 'C60 H126 O21 Zr4' _chemical_formula_moiety ? _chemical_formula_weight 1548.54 _cell_length_a 16.467(5) _cell_length_b 19.970(6) _cell_length_c 23.732(6) _cell_angle_alpha 90 _cell_angle_beta 106.073(14) _cell_angle_gamma 90 _cell_volume 7499(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 52 _cell_measurement_theta_min 8.46 _cell_measurement_theta_max 13.08 _cell_measurement_temperature 95. _exptl_crystal_colour colorless _exptl_crystal_description 'irregular fragment' _exptl_crystal_size_max .30 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .20 _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3256 _exptl_absorpt_coefficient_mu 0.6043 _exptl_absorpt_correction_type none _exptl_absorpt_process_details none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z x,1/2-y,1/2+z -x,-y,-z _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature 95. _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12381 _diffrn_reflns_av_R_equivalents 0.08 _diffrn_reflns_theta_min 3.12104 _diffrn_reflns_theta_max 22.5075 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number 4 _diffrn_standards_decay_% 3 _diffrn_standards_interval_count 300 _reflns_number_total 9777 _reflns_number_gt 6694 _reflns_threshold_expression F^2^>2.33\s(F^2^) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source ZR Zr -2.965 0.56 'International Tables Vol. IV (1974) Table 2.2B' O O 0.008 0.006 'International Tables Vol. IV (1974) Table 2.2B' C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B' H H 0 0 'International Tables Vol. IV (1974) Table 2.2B' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_number_reflns 6694 _refine_ls_number_parameters 767 _refine_ls_hydrogen_treatment ? _refine_ls_extinction_coef 0.00000005(2) _refine_ls_extinction_method Zachariasen _refine_ls_extinction_expression ; Larson, A. C. (1967). Acta Cryst. 23, p. 664. Eq. (3) ; _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? _refine_ls_weighting_scheme calc _refine_ls_weighting_details w^-1^=\s^2^(F)+(.07F)^2^ _refine_ls_R_factor_gt 0.045 _refine_ls_wR_factor_ref 0.0488 _refine_ls_goodness_of_fit_ref 1.0976 _refine_ls_shift/su_max 0.0648 _refine_diff_density_max 0.26 _refine_diff_density_min -0.27 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_disorder_group _atom_site_disorder_assembly ZR1 ZR 0.48031(4) 0.18212(3) 0.07975(3) 0.0176(2) Uani 1 0 . ZR2 ZR 0.63199(4) 0.27678(3) 0.03520(3) 0.0181(2) Uani 1 0 . ZR3 ZR 0.85136(4) 0.34584(3) 0.09840(3) 0.0213(2) Uani 1 0 . ZR4 ZR 0.97423(4) 0.41679(3) 0.23002(3) 0.0203(2) Uani 1 0 . O5 O 0.7385(2) 0.3073(2) 0.09231(17) 0.0195(15) Uani 1 0 . O6 O 0.3791(2) 0.1261(2) 0.03772(18) 0.0218(16) Uani 1 0 . C7 C 0.3050(4) 0.1525(3) -0.0023(3) 0.030(3) Uani 1 0 . C8 C 0.3357(4) 0.2023(3) -0.0432(3) 0.029(3) Uani 1 0 . O9 O 0.4072(2) 0.2374(2) -0.00356(19) 0.0240(16) Uani 1 0 . C10 C 0.2536(4) 0.0953(4) -0.0368(3) 0.034(3) Uani 1 0 . C11 C 0.2527(4) 0.1882(4) 0.0328(3) 0.037(3) Uani 1 0 . C12 C 0.3693(4) 0.1656(4) -0.0884(3) 0.037(3) Uani 1 0 . C13 C 0.2701(4) 0.2536(4) -0.0726(3) 0.042(3) Uani 1 0 . O14 O 0.5826(2) 0.1771(2) 0.03901(17) 0.0188(15) Uani 1 0 . C15 C 0.6329(4) 0.1219(3) 0.0268(3) 0.022(2) Uani 1 0 . C16 C 0.6701(4) 0.1485(3) -0.0224(3) 0.026(3) Uani 1 0 . O17 O 0.6996(3) 0.2154(2) -0.00458(18) 0.0203(16) Uani 1 0 . C18 C 0.5769(4) 0.0610(3) 0.0097(3) 0.025(2) Uani 1 0 . C19 C 0.7020(4) 0.1090(3) 0.0832(3) 0.027(3) Uani 1 0 . C20 C 0.7412(5) 0.1052(4) -0.0290(4) 0.039(3) Uani 1 0 . C21 C 0.6043(5) 0.1527(3) -0.0812(3) 0.031(3) Uani 1 0 . O22 O 0.4323(2) 0.2400(2) 0.12988(18) 0.0219(16) Uani 1 0 . C23 C 0.4558(4) 0.3077(3) 0.1458(3) 0.031(3) Uani 1 0 . C24 C 0.5500(4) 0.3143(3) 0.1445(3) 0.026(3) Uani 1 0 . O25 O 0.5536(2) 0.2782(2) 0.09232(18) 0.0196(15) Uani 1 0 . C26 C 0.4445(5) 0.3197(4) 0.2066(3) 0.036(3) Uani 1 0 . C27 C 0.3978(5) 0.3533(3) 0.1021(3) 0.038(3) Uani 1 0 . C28 C 0.6087(4) 0.2780(4) 0.1959(3) 0.037(3) Uani 1 0 . C29 C 0.5795(5) 0.3854(4) 0.1415(3) 0.042(3) Uani 1 0 . O30 O 0.5271(3) 0.2968(2) -0.03527(18) 0.0243(16) Uani 1 0 . C31 C 0.5127(4) 0.3559(4) -0.0694(3) 0.034(3) Uani 1 0 . C32 C 0.5995(4) 0.3860(3) -0.0668(3) 0.030(3) Uani 1 0 . O33 O 0.6484(3) 0.3753(2) -0.00562(18) 0.0241(16) Uani 1 0 . C34 C 0.4625(5) 0.4061(4) -0.0421(4) 0.045(3) Uani 1 0 . C35 C 0.4609(5) 0.3404(4) -0.1312(4) 0.052(3) Uani 1 0 . C36 C 0.5997(5) 0.4590(4) -0.0834(3) 0.041(3) Uani 1 0 . C37 C 0.6454(5) 0.3464(4) -0.1045(3) 0.045(3) Uani 1 0 . O38 O 0.5211(2) 0.1106(2) 0.13577(17) 0.0182(15) Uani 1 0 . C39 C 0.5228(4) 0.0605(3) 0.1789(3) 0.021(2) Uani 1 0 . C40 C 0.4301(4) 0.0412(3) 0.1758(3) 0.027(3) Uani 1 0 . O41 O 0.3880(3) 0.0202(2) 0.11726(19) 0.0286(17) Uani 1 0 . C42 C 0.5699(4) 0.0887(3) 0.2381(3) 0.031(3) Uani 1 0 . C43 C 0.5694(4) 0.0004(3) 0.1643(3) 0.029(3) Uani 1 0 . C44 C 0.4258(5) -0.0185(4) 0.2147(3) 0.042(3) Uani 1 0 . C45 C 0.3821(4) 0.0994(4) 0.1927(3) 0.035(3) Uani 1 0 . O46 O 0.8501(3) 0.2642(2) 0.03407(19) 0.0315(18) Uani 1 0 . C47 C 0.9130(5) 0.2663(4) 0.0008(3) 0.037(3) Uani 1 0 . C48 C 0.9925(5) 0.2920(5) 0.0441(3) 0.048(3) Uani 1 0 . O49 O 0.9665(3) 0.3413(2) 0.0795(2) 0.0334(18) Uani 1 0 . C50 C 0.9214(5) 0.1997(5) -0.0265(4) 0.062(4) Uani 1 0 . C51 C 0.8798(6) 0.3160(5) -0.0497(4) 0.060(4) Uani 1 0 . C52 C 1.0564(5) 0.3217(4) 0.0165(4) 0.053(4) Uani 1 0 . C53 C 1.0387(5) 0.2350(5) 0.0843(4) 0.056(4) Uani 1 0 . O54 O 0.9116(3) 0.3233(2) 0.18696(18) 0.0233(16) Uani 1 0 . C55 C 0.9107(4) 0.2702(3) 0.2290(3) 0.024(2) Uani 1 0 . C56 C 0.9990(4) 0.2729(3) 0.2749(3) 0.028(3) Uani 1 0 . O57 O 1.0170(2) 0.3426(2) 0.28671(18) 0.0249(17) Uani 1 0 . C58 C 0.8910(5) 0.2040(4) 0.1967(3) 0.038(3) Uani 1 0 . C59 C 0.8408(4) 0.2885(4) 0.2573(3) 0.035(3) Uani 1 0 . C60 C 1.0684(5) 0.2435(4) 0.2522(4) 0.046(3) Uani 1 0 . C61 C 0.9991(4) 0.2391(4) 0.3322(3) 0.038(3) Uani 1 0 . O62 O 0.7965(3) 0.4217(2) 0.04152(19) 0.0335(18) Uani 1 0 . C63 C 0.8274(5) 0.4896(4) 0.0531(3) 0.042(3) Uani 1 0 . C64 C 0.8431(4) 0.4990(3) 0.1197(3) 0.029(3) Uani 1 0 . O65 O 0.8883(3) 0.4391(2) 0.14548(18) 0.0219(16) Uani 1 0 . C66 C 0.9071(6) 0.4957(4) 0.0332(3) 0.059(4) Uani 1 0 . C67 C 0.7624(6) 0.5386(4) 0.0180(4) 0.061(4) Uani 1 0 . C68 C 0.8967(5) 0.5600(4) 0.1450(3) 0.042(3) Uani 1 0 . C69 C 0.7623(4) 0.5008(4) 0.1387(3) 0.039(3) Uani 1 0 . O70 O 1.0700(3) 0.4827(2) 0.24660(19) 0.0248(17) Uani 1 0 . C71 C 1.1518(4) 0.4685(4) 0.2394(3) 0.029(3) Uani 1 0 . C72 C 1.1390(4) 0.4319(4) 0.1809(3) 0.034(3) Uani 1 0 . O73 O 1.0674(3) 0.3877(2) 0.17760(18) 0.0257(17) Uani 1 0 . C74 C 1.1975(4) 0.5356(4) 0.2407(3) 0.037(3) Uani 1 0 . C75 C 1.1991(4) 0.4276(4) 0.2929(3) 0.038(3) Uani 1 0 . C76 C 1.1184(5) 0.4780(4) 0.1288(3) 0.045(3) Uani 1 0 . C77 C 1.2148(4) 0.3876(4) 0.1791(4) 0.051(3) Uani 1 0 . O78 O 0.9135(3) 0.4646(2) 0.27626(19) 0.0251(17) Uani 1 0 . C79 C 0.8892(4) 0.4961(4) 0.3231(3) 0.034(3) Uani 1 0 . C80 C 0.9652(9) 0.4958(9) 0.3756(5) 0.138(8) Uani 1 0 . C81 C 0.8620(7) 0.5662(5) 0.3043(5) 0.082(5) Uani 1 0 . C82 C 0.8166(8) 0.4597(5) 0.3323(6) 0.126(8) Uani 1 0 . C83 C 0.9390(14) 0.5249(16) 0.4272(7) 0.40(2) Uani 1 0 . O84 O 1.0353(6) 0.5292(9) 0.3648(8) 0.343(14) Uani 1 0 . C85 C 0.9806(11) 0.4184(7) 0.3882(4) 0.150(9) Uani 1 0 . HT1 H 0.7107 0.4045 0.007 0.038 Uiso 1 0 . HT2 H 0.384 0.0507 0.0853 0.038 Uiso 1 0 . HT3 H 0.7982 0.2431 0.0038 0.038 Uiso 1 0 . HT4 H 1.0455 0.3781 0.1374 0.038 Uiso 1 0 . H1 H 0.2038 0.1127 -0.063 0.0463 Uiso 1 0 . H2 H 0.2865 0.0732 -0.0586 0.0463 Uiso 1 0 . H3 H 0.2397 0.0646 -0.0106 0.0463 Uiso 1 0 . H4 H 0.285 0.2237 0.055 0.05 Uiso 1 0 . H5 H 0.2028 0.206 0.0068 0.05 Uiso 1 0 . H6 H 0.2378 0.1573 0.0588 0.05 Uiso 1 0 . H7 H 0.3237 0.1439 -0.1158 0.0494 Uiso 1 0 . H8 H 0.3951 0.1966 -0.1082 0.0494 Uiso 1 0 . H9 H 0.4095 0.1331 -0.0691 0.0494 Uiso 1 0 . H10 H 0.2502 0.2761 -0.0437 0.0543 Uiso 1 0 . H11 H 0.2949 0.2854 -0.0927 0.0543 Uiso 1 0 . H12 H 0.2244 0.232 -0.0997 0.0543 Uiso 1 0 . H13 H 0.5516 0.0509 0.0402 0.0372 Uiso 1 0 . H14 H 0.5339 0.0701 -0.0254 0.0372 Uiso 1 0 . H15 H 0.6098 0.0241 0.0038 0.0372 Uiso 1 0 . H16 H 0.6766 0.0986 0.1135 0.0402 Uiso 1 0 . H17 H 0.7354 0.0723 0.0774 0.0402 Uiso 1 0 . H18 H 0.7359 0.1477 0.0932 0.0402 Uiso 1 0 . H19 H 0.7204 0.062 -0.0418 0.0523 Uiso 1 0 . H20 H 0.7653 0.1248 -0.0573 0.0523 Uiso 1 0 . H21 H 0.7832 0.102 0.0074 0.0523 Uiso 1 0 . H22 H 0.5582 0.1792 -0.0779 0.0439 Uiso 1 0 . H23 H 0.6289 0.1721 -0.1091 0.0439 Uiso 1 0 . H24 H 0.5848 0.1088 -0.0938 0.0439 Uiso 1 0 . H25 H 0.4808 0.291 0.2341 0.0494 Uiso 1 0 . H26 H 0.4578 0.3651 0.2176 0.0494 Uiso 1 0 . H27 H 0.3874 0.3112 0.2059 0.0494 Uiso 1 0 . H28 H 0.4109 0.3985 0.113 0.0504 Uiso 1 0 . H29 H 0.4046 0.3455 0.0642 0.0504 Uiso 1 0 . H30 H 0.3407 0.3442 0.1015 0.0504 Uiso 1 0 . H31 H 0.5893 0.2333 0.1976 0.0495 Uiso 1 0 . H32 H 0.6643 0.2768 0.1913 0.0495 Uiso 1 0 . H33 H 0.6097 0.3005 0.2313 0.0495 Uiso 1 0 . H34 H 0.6356 0.3848 0.1371 0.0544 Uiso 1 0 . H35 H 0.5431 0.4075 0.1092 0.0544 Uiso 1 0 . H36 H 0.5804 0.408 0.1768 0.0544 Uiso 1 0 . H37 H 0.4948 0.4174 -0.0038 0.0585 Uiso 1 0 . H38 H 0.4514 0.4454 -0.0658 0.0585 Uiso 1 0 . H39 H 0.4107 0.3863 -0.0411 0.0585 Uiso 1 0 . H40 H 0.4505 0.3805 -0.1537 0.0654 Uiso 1 0 . H41 H 0.4899 0.3094 -0.1488 0.0654 Uiso 1 0 . H42 H 0.4079 0.3215 -0.1302 0.0654 Uiso 1 0 . H43 H 0.6569 0.474 -0.076 0.0531 Uiso 1 0 . H44 H 0.572 0.4641 -0.1239 0.0531 Uiso 1 0 . H45 H 0.5721 0.4845 -0.0608 0.0531 Uiso 1 0 . H46 H 0.6459 0.3003 -0.0948 0.0577 Uiso 1 0 . H47 H 0.6172 0.3528 -0.1446 0.0577 Uiso 1 0 . H48 H 0.7021 0.3622 -0.0966 0.0577 Uiso 1 0 . H49 H 0.5728 0.0558 0.2678 0.0437 Uiso 1 0 . H50 H 0.6255 0.101 0.238 0.0437 Uiso 1 0 . H51 H 0.541 0.1271 0.2466 0.0437 Uiso 1 0 . H52 H 0.5723 -0.0338 0.1925 0.0417 Uiso 1 0 . H53 H 0.5404 -0.0159 0.1264 0.0417 Uiso 1 0 . H54 H 0.6252 0.0133 0.1644 0.0417 Uiso 1 0 . H55 H 0.3683 -0.0309 0.2092 0.0547 Uiso 1 0 . H56 H 0.4556 -0.0551 0.2043 0.0547 Uiso 1 0 . H57 H 0.4504 -0.0069 0.2544 0.0547 Uiso 1 0 . H58 H 0.4066 0.1105 0.2328 0.0477 Uiso 1 0 . H59 H 0.3847 0.1371 0.1689 0.0477 Uiso 1 0 . H60 H 0.3245 0.0871 0.1872 0.0477 Uiso 1 0 . H61 H 0.8677 0.1864 -0.0504 0.0748 Uiso 1 0 . H62 H 0.9597 0.2042 -0.0497 0.0748 Uiso 1 0 . H63 H 0.9422 0.1678 0.0035 0.0748 Uiso 1 0 . H64 H 0.8745 0.3589 -0.0338 0.0735 Uiso 1 0 . H65 H 0.9187 0.3183 -0.0726 0.0735 Uiso 1 0 . H66 H 0.8266 0.3013 -0.0731 0.0735 Uiso 1 0 . H67 H 1.1031 0.338 0.046 0.0654 Uiso 1 0 . H68 H 1.0746 0.2881 -0.0059 0.0654 Uiso 1 0 . H69 H 1.0309 0.3574 -0.009 0.0654 Uiso 1 0 . H70 H 1.0016 0.2158 0.1041 0.0687 Uiso 1 0 . H71 H 1.0564 0.2022 0.0616 0.0687 Uiso 1 0 . H72 H 1.0867 0.2532 0.1125 0.0687 Uiso 1 0 . H73 H 0.8394 0.2075 0.1672 0.051 Uiso 1 0 . H74 H 0.9354 0.1933 0.1795 0.051 Uiso 1 0 . H75 H 0.8874 0.1697 0.2237 0.051 Uiso 1 0 . H76 H 0.8538 0.3296 0.2775 0.0485 Uiso 1 0 . H77 H 0.7886 0.2918 0.228 0.0485 Uiso 1 0 . H78 H 0.8366 0.2541 0.2846 0.0485 Uiso 1 0 . H79 H 1.059 0.1967 0.2462 0.0581 Uiso 1 0 . H80 H 1.0678 0.2643 0.2162 0.0581 Uiso 1 0 . H81 H 1.1213 0.2508 0.28 0.0581 Uiso 1 0 . H82 H 0.9558 0.2575 0.3466 0.0512 Uiso 1 0 . H83 H 0.9899 0.1923 0.3258 0.0512 Uiso 1 0 . H84 H 1.0525 0.2459 0.3601 0.0512 Uiso 1 0 . H85 H 0.9487 0.4652 0.0549 0.0721 Uiso 1 0 . H86 H 0.8948 0.4854 -0.0074 0.0721 Uiso 1 0 . H87 H 0.9286 0.5401 0.0397 0.0721 Uiso 1 0 . H88 H 0.7833 0.583 0.0246 0.0718 Uiso 1 0 . H89 H 0.75 0.5284 -0.0227 0.0718 Uiso 1 0 . H90 H 0.7114 0.5352 0.0297 0.0718 Uiso 1 0 . H91 H 0.9101 0.5593 0.1863 0.0551 Uiso 1 0 . H92 H 0.9471 0.5594 0.1329 0.0551 Uiso 1 0 . H93 H 0.8657 0.5998 0.1305 0.0551 Uiso 1 0 . H94 H 0.7316 0.5406 0.1246 0.0508 Uiso 1 0 . H95 H 0.7282 0.4629 0.123 0.0508 Uiso 1 0 . H96 H 0.7756 0.4997 0.1802 0.0508 Uiso 1 0 . H97 H 1.2538 0.5278 0.2396 0.0511 Uiso 1 0 . H98 H 1.1688 0.5618 0.2076 0.0511 Uiso 1 0 . H99 H 1.1978 0.5592 0.2756 0.0511 Uiso 1 0 . H100 H 1.1718 0.3856 0.2926 0.05 Uiso 1 0 . H101 H 1.2556 0.4206 0.2916 0.05 Uiso 1 0 . H102 H 1.1992 0.4512 0.3277 0.05 Uiso 1 0 . H103 H 1.1657 0.5055 0.1302 0.0579 Uiso 1 0 . H104 H 1.1045 0.4522 0.0939 0.0579 Uiso 1 0 . H105 H 1.0715 0.5052 0.1301 0.0579 Uiso 1 0 . H106 H 1.228 0.3588 0.2126 0.0624 Uiso 1 0 . H107 H 1.2006 0.3615 0.1446 0.0624 Uiso 1 0 . H108 H 1.262 0.4151 0.1801 0.0624 Uiso 1 0 . H109 H 0.9078 0.5921 0.298 0.1703 Uiso 1 0 . H110 H 0.8176 0.566 0.2674 0.1703 Uiso 1 0 . H111 H 0.8403 0.5889 0.3324 0.1703 Uiso 1 0 . H112 H 0.7705 0.4581 0.2958 0.1294 Uiso 1 0 . H113 H 0.8298 0.4142 0.3439 0.1294 Uiso 1 0 . H114 H 0.794 0.4807 0.3608 0.1294 Uiso 1 0 . H115 H 0.9341 0.5744 0.4227 0.3462 Uiso 1 0 . H116 H 0.887 0.5077 0.4257 0.3462 Uiso 1 0 . H117 H 0.9798 0.517 0.4633 0.3462 Uiso 1 0 . H118 H 0.926 0.3989 0.3875 0.1526 Uiso 1 0 . H119 H 0.9994 0.3957 0.3584 0.1526 Uiso 1 0 . H120 H 1.0187 0.4081 0.4253 0.1526 Uiso 1 0 .