#------------------------------------------------------------------------------ #$Date: 2010-03-30 13:46:35 +0100 (Tue, 30 Mar 2010) $ #$Revision: 1059 $ #$URL: svn://www.crystallography.net/cod/cif/5/5000320.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_5000320 ## 'minor manual editing of SDT2CIF v. 1.1 BETA output' _chemical_formula_sum 'C42 H88 O14 Ti Zr2' _[local]_cod_chemical_formula_sum_orig 'C42 H88 O14 Ti1 Zr2' _chemical_formula_moiety 'C42 H88 O14 Ti1 Zr2' _chemical_formula_weight 1047.48 _cell_length_a 12.926(3) _cell_length_b 17.727(4) _cell_length_c 23.144(5) _cell_angle_alpha 90 _cell_angle_beta 102.299(11) _cell_angle_gamma 90 _cell_volume 5181.4(19) _cell_formula_units_Z 4 _cell_measurement_reflns_used 52 _cell_measurement_theta_min 9.59 _cell_measurement_theta_max 10.36 _cell_measurement_temperature 109 _exptl_crystal_colour colorless _exptl_crystal_description irregular _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2216 _exptl_absorpt_coefficient_mu 0.6015 _exptl_absorpt_correction_type none _exptl_absorpt_process_details none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _symmetry_cell_setting monoclinic _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_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 109 _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10668 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_theta_min 3.05174 _diffrn_reflns_theta_max 28.1275 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_standards_number 4 _diffrn_standards_decay_% 5.5 _diffrn_standards_interval_count 133 _reflns_number_total 9096 _reflns_number_gt 5996 _reflns_threshold_expression F>3.0\s(F) _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap 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' TI Ti 0.248 0.446 '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 9096 _refine_ls_number_parameters 541 _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_coef 0.00000000(3) _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 0.0553 _refine_ls_wR_factor_ref 0.0521 _refine_ls_goodness_of_fit_ref 1.1078 _refine_ls_shift/su_max 0.5598 _refine_diff_density_max 0.86 _refine_diff_density_min -0.52 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 0.99113(4) 0.13030(3) 0.15003(2) 0.01633(17) Uani 1 0 . ZR2 ZR 1.25466(4) 0.11092(3) 0.23133(2) 0.01473(16) Uani 1 0 . TI3 TI 1.44218(8) 0.12483(6) 0.35921(4) 0.0202(3) Uani 1 0 . O4 O 0.9295(3) 0.1615(2) 0.06539(16) 0.0217(13) Uani 1 0 . C5 C 0.9382(5) 0.2347(3) 0.0418(3) 0.0248(19) Uani 1 0 . C6 C 1.0557(4) 0.2601(3) 0.0645(2) 0.0235(19) Uani 1 0 . O7 O 1.0811(3) 0.2327(2) 0.12525(18) 0.0235(14) Uani 1 0 . C8 C 0.9089(5) 0.2294(3) -0.0259(3) 0.029(2) Uani 1 0 . C9 C 0.8602(5) 0.2864(3) 0.0635(3) 0.031(2) Uani 1 0 . C10 C 1.1310(5) 0.2239(3) 0.0310(3) 0.030(2) Uani 1 0 . C11 C 1.0701(5) 0.3459(3) 0.0660(3) 0.034(2) Uani 1 0 . O12 O 0.9175(3) 0.1975(2) 0.19651(16) 0.0211(13) Uani 1 0 . C13 C 0.9612(4) 0.2290(3) 0.2533(3) 0.0239(19) Uani 1 0 . C14 C 1.0448(5) 0.1711(3) 0.2852(2) 0.0246(19) Uani 1 0 . O15 O 1.1001(3) 0.14378(19) 0.24084(15) 0.0179(12) Uani 1 0 . C16 C 0.8707(5) 0.2418(3) 0.2849(3) 0.032(2) Uani 1 0 . C17 C 1.0109(5) 0.3047(3) 0.2439(3) 0.032(2) Uani 1 0 . C18 C 0.9898(5) 0.1036(4) 0.3058(3) 0.034(2) Uani 1 0 . C19 C 1.1244(5) 0.2052(4) 0.3369(3) 0.033(2) Uani 1 0 . O20 O 1.3239(3) 0.03327(19) 0.19223(15) 0.0169(12) Uani 1 0 . C21 C 1.2846(4) 0.0063(3) 0.1330(3) 0.0217(18) Uani 1 0 . C22 C 1.1634(4) 0.0028(3) 0.1265(2) 0.0178(17) Uani 1 0 . O23 O 1.1369(3) 0.07169(19) 0.15519(15) 0.0164(12) Uani 1 0 . C24 C 1.3182(4) 0.0612(3) 0.0897(3) 0.0252(19) Uani 1 0 . C25 C 1.3334(4) -0.0706(3) 0.1261(3) 0.0252(19) Uani 1 0 . C26 C 1.1010(4) 0.0007(3) 0.0627(2) 0.0201(18) Uani 1 0 . C27 C 1.1297(4) -0.0631(3) 0.1596(2) 0.0222(18) Uani 1 0 . O28 O 1.2723(3) 0.20481(19) 0.18343(16) 0.0186(12) Uani 1 0 . C29 C 1.3519(5) 0.2618(3) 0.2029(3) 0.0252(19) Uani 1 0 . C30 C 1.4448(5) 0.2218(3) 0.2453(3) 0.026(2) Uani 1 0 . O31 O 1.3917(3) 0.1691(2) 0.27818(16) 0.0196(12) Uani 1 0 . C32 C 1.3028(5) 0.3224(3) 0.2351(3) 0.036(2) Uani 1 0 . C33 C 1.3838(5) 0.2950(3) 0.1491(3) 0.035(2) Uani 1 0 . C34 C 1.5151(5) 0.2755(3) 0.2874(3) 0.029(2) Uani 1 0 . C35 C 1.5133(5) 0.1754(3) 0.2125(3) 0.028(2) Uani 1 0 . O36 O 1.4468(3) 0.0465(2) 0.41172(17) 0.0272(14) Uani 1 0 . C37 C 1.3595(4) -0.0026(3) 0.4111(3) 0.027(2) Uani 1 0 . C38 C 1.3089(4) -0.0125(3) 0.3440(3) 0.0229(19) Uani 1 0 . O39 O 1.3076(3) 0.0636(2) 0.31955(16) 0.0204(13) Uani 1 0 . C40 C 1.2867(5) 0.0345(4) 0.4455(3) 0.036(2) Uani 1 0 . C41 C 1.4027(5) -0.0770(4) 0.4410(3) 0.034(2) Uani 1 0 . C42 C 1.1986(5) -0.0447(3) 0.3333(3) 0.032(2) Uani 1 0 . C43 C 1.3775(5) -0.0620(3) 0.3135(3) 0.030(2) Uani 1 0 . O44 O 0.8981(3) 0.0436(2) 0.14153(15) 0.0179(12) Uani 1 0 . C45 C 0.8044(4) -0.0008(3) 0.1280(3) 0.0245(19) Uani 1 0 . C46 C 0.7155(5) 0.0472(4) 0.0876(3) 0.031(2) Uani 1 0 . O47 O 0.7495(3) 0.0693(3) 0.03609(18) 0.0318(15) Uani 1 0 . C48 C 0.8270(5) -0.0709(4) 0.0961(3) 0.037(2) Uani 1 0 . C49 C 0.7766(5) -0.0226(4) 0.1858(3) 0.042(2) Uani 1 0 . C50 C 0.6144(5) 0.0011(4) 0.0646(3) 0.041(2) Uani 1 0 . C51 C 0.6869(5) 0.1160(4) 0.1203(3) 0.039(2) Uani 1 0 . O52 O 1.5783(3) 0.1140(2) 0.35537(17) 0.0266(13) Uani 1 0 . C53 C 1.6614(5) 0.0600(4) 0.3762(3) 0.031(2) Uani 1 0 . C54 C 1.6947(5) 0.0267(4) 0.3237(3) 0.045(3) Uani 1 0 . C55 C 1.7504(5) 0.0995(4) 0.4171(3) 0.044(3) Uani 1 0 . O56 O 1.4220(3) 0.2064(2) 0.40046(17) 0.0274(14) Uani 1 0 . C57 C 1.4540(6) 0.2693(4) 0.4380(3) 0.041(3) Uani 1 0 . C58 C 1.5708(6) 0.2689(4) 0.4609(3) 0.043(3) Uani 1 0 . C59 C 1.3940(6) 0.2690(4) 0.4856(3) 0.052(3) Uani 1 0 . H1 H 1.139(4) 0.238(3) 0.136(2) 0.009(15) Uiso 1 0 . H2 H 0.8363 0.2416 -0.0396 0.0423 Uiso 1 0 . H3 H 0.9511 0.2638 -0.0426 0.0423 Uiso 1 0 . H4 H 0.9216 0.1796 -0.038 0.0423 Uiso 1 0 . H5 H 0.8811 0.2927 0.1051 0.0429 Uiso 1 0 . H6 H 0.8586 0.3343 0.0448 0.0429 Uiso 1 0 . H7 H 0.7912 0.2647 0.0541 0.0429 Uiso 1 0 . H8 H 1.1218 0.1708 0.0304 0.0423 Uiso 1 0 . H9 H 1.1169 0.2425 -0.0086 0.0423 Uiso 1 0 . H10 H 1.202 0.2359 0.0496 0.0423 Uiso 1 0 . H11 H 1.14 0.3589 0.0623 0.045 Uiso 1 0 . H12 H 1.0206 0.3689 0.0342 0.045 Uiso 1 0 . H13 H 1.0584 0.3661 0.1024 0.045 Uiso 1 0 . H14 H 0.8974 0.2413 0.3265 0.0439 Uiso 1 0 . H15 H 0.838 0.2887 0.2733 0.0439 Uiso 1 0 . H16 H 0.8199 0.2023 0.2747 0.0439 Uiso 1 0 . H17 H 1.0304 0.3303 0.2808 0.0431 Uiso 1 0 . H18 H 1.0719 0.2966 0.2282 0.0431 Uiso 1 0 . H19 H 0.9612 0.3344 0.2173 0.0431 Uiso 1 0 . H20 H 0.9612 0.1176 0.3387 0.046 Uiso 1 0 . H21 H 0.9338 0.0871 0.2744 0.046 Uiso 1 0 . H22 H 1.039 0.0637 0.3165 0.046 Uiso 1 0 . H23 H 1.1732 0.1676 0.3547 0.0462 Uiso 1 0 . H24 H 1.1614 0.2453 0.3231 0.0462 Uiso 1 0 . H25 H 1.0877 0.2242 0.3654 0.0462 Uiso 1 0 . H26 H 1.3934 0.0639 0.0972 0.0374 Uiso 1 0 . H27 H 1.2919 0.0446 0.0504 0.0374 Uiso 1 0 . H28 H 1.2905 0.1101 0.0947 0.0374 Uiso 1 0 . H29 H 1.3267 -0.1021 0.1586 0.038 Uiso 1 0 . H30 H 1.2978 -0.0935 0.0904 0.038 Uiso 1 0 . H31 H 1.4063 -0.0648 0.1258 0.038 Uiso 1 0 . H32 H 1.1007 0.0496 0.0456 0.0322 Uiso 1 0 . H33 H 1.1335 -0.0339 0.0405 0.0322 Uiso 1 0 . H34 H 1.0304 -0.0147 0.0616 0.0322 Uiso 1 0 . H35 H 1.0549 -0.0619 0.1563 0.0339 Uiso 1 0 . H36 H 1.1482 -0.1092 0.1432 0.0339 Uiso 1 0 . H37 H 1.1639 -0.0607 0.2002 0.0339 Uiso 1 0 . H38 H 1.3452 0.3666 0.2389 0.0468 Uiso 1 0 . H39 H 1.2337 0.3335 0.2133 0.0468 Uiso 1 0 . H40 H 1.299 0.3045 0.2733 0.0468 Uiso 1 0 . H41 H 1.4457 0.3249 0.161 0.0465 Uiso 1 0 . H42 H 1.3975 0.2555 0.1241 0.0465 Uiso 1 0 . H43 H 1.3278 0.3257 0.128 0.0465 Uiso 1 0 . H44 H 1.5659 0.2476 0.3147 0.042 Uiso 1 0 . H45 H 1.5492 0.3089 0.2657 0.042 Uiso 1 0 . H46 H 1.4721 0.3038 0.3086 0.042 Uiso 1 0 . H47 H 1.5589 0.1432 0.2396 0.0396 Uiso 1 0 . H48 H 1.4694 0.1453 0.1831 0.0396 Uiso 1 0 . H49 H 1.5549 0.2081 0.1942 0.0396 Uiso 1 0 . H50 H 1.3268 0.0523 0.4823 0.0495 Uiso 1 0 . H51 H 1.2516 0.0758 0.4235 0.0495 Uiso 1 0 . H52 H 1.2357 -0.001 0.4526 0.0495 Uiso 1 0 . H53 H 1.3464 -0.1117 0.4395 0.0459 Uiso 1 0 . H54 H 1.4534 -0.0976 0.4211 0.0459 Uiso 1 0 . H55 H 1.4358 -0.0675 0.4812 0.0459 Uiso 1 0 . H56 H 1.1569 -0.0171 0.3553 0.0431 Uiso 1 0 . H57 H 1.1668 -0.0419 0.2924 0.0431 Uiso 1 0 . H58 H 1.2018 -0.0961 0.3455 0.0431 Uiso 1 0 . H59 H 1.3718 -0.1133 0.3248 0.0427 Uiso 1 0 . H60 H 1.3542 -0.0579 0.2717 0.0427 Uiso 1 0 . H61 H 1.4492 -0.0465 0.3246 0.0427 Uiso 1 0 . H62 H 0.811(4) 0.100(3) 0.040(2) 0.022(16) Uiso 1 0 . H63 H 0.7649 -0.1014 0.0873 0.0492 Uiso 1 0 . H64 H 0.8475 -0.0577 0.0605 0.0492 Uiso 1 0 . H65 H 0.8824 -0.0986 0.1208 0.0492 Uiso 1 0 . H66 H 0.7686 0.0215 0.2073 0.0531 Uiso 1 0 . H67 H 0.7124 -0.0504 0.1778 0.0531 Uiso 1 0 . H68 H 0.8318 -0.0529 0.2076 0.0531 Uiso 1 0 . H69 H 0.5648 0.0308 0.0378 0.0527 Uiso 1 0 . H70 H 0.6314 -0.0427 0.0446 0.0527 Uiso 1 0 . H71 H 0.5842 -0.0139 0.0967 0.0527 Uiso 1 0 . H72 H 0.7483 0.1455 0.134 0.0506 Uiso 1 0 . H73 H 0.6353 0.1451 0.0943 0.0506 Uiso 1 0 . H74 H 0.6587 0.0999 0.153 0.0506 Uiso 1 0 . H75 H 1.6346 0.0211 0.3971 0.0438 Uiso 1 0 . H76 H 1.6367 0.0012 0.2998 0.0569 Uiso 1 0 . H77 H 1.7179 0.0661 0.3016 0.0569 Uiso 1 0 . H78 H 1.7511 -0.0075 0.3369 0.0569 Uiso 1 0 . H79 H 1.8069 0.0651 0.4292 0.0557 Uiso 1 0 . H80 H 1.7738 0.1405 0.3965 0.0557 Uiso 1 0 . H81 H 1.7264 0.1178 0.4502 0.0557 Uiso 1 0 . H82 H 1.4367 0.3142 0.4152 0.0528 Uiso 1 0 . H83 H 1.5895 0.225 0.4845 0.0549 Uiso 1 0 . H84 H 1.6056 0.2687 0.429 0.0549 Uiso 1 0 . H85 H 1.5904 0.3125 0.4846 0.0549 Uiso 1 0 . H86 H 1.423 0.3056 0.5146 0.0632 Uiso 1 0 . H87 H 1.3221 0.2805 0.4695 0.0632 Uiso 1 0 . H88 H 1.3991 0.2204 0.5034 0.0632 Uiso 1 0 . _cod_database_code 5000320