#------------------------------------------------------------------------------ #$Date: 2008-02-29 13:15:29 +0000 (Fri, 29 Feb 2008) $ #$Revision: 184 $ #$URL: svn://www.crystallography.net/cod/cif/5/5000318.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_5000318 ## 'minor manual editing of SDT2CIF v. 1.1 BETA output' _chemical_formula_sum 'C41 H90 O8 W2' _chemical_formula_moiety 'C41 H90 O8 W2' _chemical_formula_weight 1078.84 _cell_length_a 19.156(2) _cell_length_b 13.8038(14) _cell_length_c 20.759(2) _cell_angle_alpha 90 _cell_angle_beta 112.312(6) _cell_angle_gamma 90 _cell_volume 5078.3(10) _cell_formula_units_Z 4 _cell_measurement_reflns_used 148 _cell_measurement_theta_min 10.37 _cell_measurement_theta_max 17.22 _cell_measurement_temperature 105 _exptl_crystal_colour black _exptl_crystal_description prism _exptl_crystal_size_max .40 _exptl_crystal_size_mid .35 _exptl_crystal_size_min .30 _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 4.5726 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details Tompa _exptl_absorpt_correction_T_min 0.165 _exptl_absorpt_correction_T_max 0.327 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,-z 1/2+x,1/2-y,z -x,-y,-z _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature 105 _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17943 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_theta_min 3.13615 _diffrn_reflns_theta_max 25.0622 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_standards_number 4 _diffrn_standards_decay_% -0.5 _diffrn_standards_interval_count 300 _reflns_number_total 8982 _reflns_number_gt 7142 _reflns_threshold_expression F>3.0\s(F) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source W W -1.421 6.872 '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 8982 _refine_ls_number_parameters 461 _refine_ls_hydrogen_treatment noref _refine_ls_extinction_coef 0.000000147(13) _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 0.0308 _refine_ls_wR_factor_ref 0.0331 _refine_ls_goodness_of_fit_ref 0.8382 _refine_ls_shift/su_max 0.2203 _refine_diff_density_max 1.85 _refine_diff_density_min -1.71 _refine_special_details ; One of the neopentoxide ligands, O40 thru C45, was found to be disordered. Of these atoms, only O40 and the central carbon, C42, of the terminal t-butyl group were ordered. The remaining carbons as well as C52 thru C56 from a difference Fourier map were used to model the disorder. The population parameters for the disordered atoms were refined, the result- ing occupancies were normalized to give the correct total occupancy, and the final population parameters were then fixed. Calculated hydrogens were included on the ordered carbons with thermal parameters fixed at one plus the iso- tropic parameter of the parent carbon atoms. In the final cycles of refinement, the disordered carbons were varied with isotropic thermal parameters and the ordered non-hydrogen atoms were varied with anisotropic thermal parameters. ; 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 W1 W 0.368693(12) 0.012691(15) 0.734344(11) 0.01610(8) Uani 1 0 . W2 W 0.402357(13) 0.194704(14) 0.774014(11) 0.01905(9) Uani 1 0 . C3 C 0.3335(3) 0.0974(4) 0.8009(3) 0.0212(18) Uani 1 0 . O4 O 0.4109(2) 0.1229(2) 0.69030(17) 0.0210(13) Uani 1 0 . C5 C 0.4681(3) 0.1217(4) 0.6605(3) 0.0226(19) Uani 1 0 . C6 C 0.4373(3) 0.1530(4) 0.5848(3) 0.028(2) Uani 1 0 . C7 C 0.3739(4) 0.0844(5) 0.5413(3) 0.043(3) Uani 1 0 . C8 C 0.4084(4) 0.2563(5) 0.5780(4) 0.049(3) Uani 1 0 . C9 C 0.5009(4) 0.1481(5) 0.5579(3) 0.043(3) Uani 1 0 . O10 O 0.46224(19) 0.0636(3) 0.81756(17) 0.0198(13) Uani 1 0 . C11 C 0.5401(3) 0.0402(4) 0.8337(3) 0.025(2) Uani 1 0 . C12 C 0.5760(3) 0.0014(4) 0.9078(3) 0.033(2) Uani 1 0 . C13 C 0.5362(4) -0.0915(5) 0.9140(3) 0.049(3) Uani 1 0 . C14 C 0.5697(4) 0.0757(5) 0.9597(3) 0.050(3) Uani 1 0 . C15 C 0.6592(4) -0.0192(6) 0.9211(4) 0.059(3) Uani 1 0 . O16 O 0.3431(2) -0.1020(3) 0.77336(18) 0.0244(14) Uani 1 0 . C17 C 0.3035(4) -0.1117(5) 0.8186(3) 0.039(3) Uani 1 0 . C18 C 0.2782(4) -0.2156(4) 0.8224(3) 0.034(2) Uani 1 0 . C19 C 0.3444(5) -0.2797(7) 0.8491(6) 0.089(5) Uani 1 0 . C20 C 0.2244(5) -0.2477(6) 0.7530(4) 0.062(4) Uani 1 0 . C21 C 0.2361(6) -0.2151(6) 0.8720(5) 0.071(4) Uani 1 0 . O22 O 0.4365(2) -0.0725(2) 0.71095(18) 0.0206(13) Uani 1 0 . C23 C 0.4593(3) -0.1700(4) 0.7279(3) 0.028(2) Uani 1 0 . C24 C 0.4446(3) -0.2302(4) 0.6623(3) 0.030(2) Uani 1 0 . C25 C 0.4896(5) -0.1898(5) 0.6212(4) 0.046(3) Uani 1 0 . C26 C 0.4713(4) -0.3333(5) 0.6857(4) 0.044(3) Uani 1 0 . C27 C 0.3599(4) -0.2292(5) 0.6179(4) 0.048(3) Uani 1 0 . O28 O 0.2780(2) 0.0268(3) 0.66099(19) 0.0243(14) Uani 1 0 . C29 C 0.2153(3) 0.0869(4) 0.6254(3) 0.026(2) Uani 1 0 . C30 C 0.1528(3) 0.0297(4) 0.5699(3) 0.027(2) Uani 1 0 . C31 C 0.1778(4) -0.0028(4) 0.5124(3) 0.036(2) Uani 1 0 . C32 C 0.0868(4) 0.0989(5) 0.5406(4) 0.048(3) Uani 1 0 . C33 C 0.1313(4) -0.0580(5) 0.6034(3) 0.042(3) Uani 1 0 . O34 O 0.3244(2) 0.2665(3) 0.71253(19) 0.0291(15) Uani 1 0 . C35 C 0.2688(3) 0.3306(4) 0.7197(3) 0.031(2) Uani 1 0 . C36 C 0.2499(3) 0.4137(4) 0.6684(3) 0.029(2) Uani 1 0 . C37 C 0.2163(3) 0.3757(5) 0.5937(3) 0.037(2) Uani 1 0 . C38 C 0.3200(4) 0.4733(5) 0.6799(4) 0.051(3) Uani 1 0 . C39 C 0.1915(4) 0.4746(5) 0.6839(4) 0.047(3) Uani 1 0 . O40 O 0.5005(2) 0.2484(3) 0.7885(2) 0.0292(15) Uani 1 0 . C41 C 0.5652(6) 0.2863(7) 0.8512(5) 0.029(2) Uiso 0.6214 0 . C42 C 0.5971(4) 0.3731(5) 0.8274(4) 0.047(3) Uani 1 0 . C43 C 0.6640(6) 0.4106(7) 0.8951(5) 0.038(2) Uiso 0.752 0 . C44 C 0.5325(8) 0.4617(10) 0.8186(7) 0.043(3) Uiso 0.5104 0 . C45 C 0.5850(15) 0.4033(19) 0.7541(12) 0.039(5) Uiso 0.33 0 . O46 O 0.4099(2) 0.2699(3) 0.85415(18) 0.0257(14) Uani 1 0 . C47 C 0.3739(3) 0.2600(4) 0.9024(3) 0.027(2) Uani 1 0 . C48 C 0.3887(4) 0.3493(4) 0.9516(3) 0.029(2) Uani 1 0 . C49 C 0.3437(4) 0.3310(5) 0.9977(3) 0.039(3) Uani 1 0 . C50 C 0.3617(4) 0.4419(4) 0.9093(3) 0.036(2) Uani 1 0 . C51 C 0.4722(4) 0.3567(5) 0.9959(3) 0.039(3) Uani 1 0 . C52 C 0.5351(9) 0.3192(11) 0.8396(8) 0.027(3) Uiso 0.3786 0 . C53 C 0.6528(10) 0.2776(12) 0.8188(9) 0.046(4) Uiso 0.4172 0 . C54 C 0.6175(10) 0.3666(12) 0.7701(8) 0.033(4) Uiso 0.403 0 . C55 C 0.566(2) 0.432(3) 0.7633(18) 0.063(10) Uiso 0.2744 0 . C56 C 0.6426(16) 0.441(2) 0.8776(14) 0.053(7) Uiso 0.3129 0 . H1 H 0.2814 0.1123 0.7851 0.0341 Uiso 1 0 . H2 H 0.3511 0.0776 0.8484 0.0341 Uiso 1 0 . H3 H 0.5076 0.1647 0.6864 0.0348 Uiso 1 0 . H4 H 0.4874 0.058 0.6635 0.0348 Uiso 1 0 . H5 H 0.3333 0.0886 0.5568 0.0558 Uiso 1 0 . H6 H 0.3565 0.1034 0.4935 0.0558 Uiso 1 0 . H7 H 0.3924 0.0204 0.5461 0.0558 Uiso 1 0 . H8 H 0.4481 0.2979 0.6045 0.0609 Uiso 1 0 . H9 H 0.3899 0.2749 0.5304 0.0609 Uiso 1 0 . H10 H 0.3686 0.2595 0.5947 0.0609 Uiso 1 0 . H11 H 0.5191 0.0834 0.562 0.0563 Uiso 1 0 . H12 H 0.4826 0.1675 0.5106 0.0563 Uiso 1 0 . H13 H 0.5406 0.1899 0.5848 0.0563 Uiso 1 0 . H14 H 0.5433 -0.0078 0.8022 0.0388 Uiso 1 0 . H15 H 0.5663 0.0966 0.8297 0.0388 Uiso 1 0 . H16 H 0.4844 -0.0777 0.9045 0.0606 Uiso 1 0 . H17 H 0.5395 -0.1376 0.8815 0.0606 Uiso 1 0 . H18 H 0.5591 -0.1164 0.9599 0.0606 Uiso 1 0 . H19 H 0.5936 0.0517 1.0057 0.0629 Uiso 1 0 . H20 H 0.5923 0.1345 0.9548 0.0629 Uiso 1 0 . H21 H 0.5174 0.0869 0.9507 0.0629 Uiso 1 0 . H22 H 0.6833 -0.046 0.9669 0.0705 Uiso 1 0 . H23 H 0.6622 -0.0645 0.888 0.0705 Uiso 1 0 . H24 H 0.6836 0.039 0.9181 0.0705 Uiso 1 0 . H25 H 0.3355 -0.0918 0.864 0.0512 Uiso 1 0 . H26 H 0.26 -0.0714 0.8022 0.0512 Uiso 1 0 . H27 H 0.3286 -0.3442 0.8535 0.1006 Uiso 1 0 . H28 H 0.3694 -0.2807 0.8168 0.1006 Uiso 1 0 . H29 H 0.3784 -0.2577 0.8927 0.1006 Uiso 1 0 . H30 H 0.1833 -0.2046 0.7363 0.0742 Uiso 1 0 . H31 H 0.2499 -0.249 0.7211 0.0742 Uiso 1 0 . H32 H 0.2071 -0.3113 0.7565 0.0742 Uiso 1 0 . H33 H 0.2684 -0.1933 0.9167 0.0805 Uiso 1 0 . H34 H 0.1934 -0.1733 0.8544 0.0805 Uiso 1 0 . H35 H 0.219 -0.2791 0.8759 0.0805 Uiso 1 0 . H36 H 0.5118 -0.1712 0.7559 0.0405 Uiso 1 0 . H37 H 0.432 -0.1969 0.7534 0.0405 Uiso 1 0 . H38 H 0.5416 -0.1894 0.6502 0.06 Uiso 1 0 . H39 H 0.4814 -0.2292 0.5817 0.06 Uiso 1 0 . H40 H 0.4733 -0.1255 0.6068 0.06 Uiso 1 0 . H41 H 0.445 -0.3578 0.7127 0.0572 Uiso 1 0 . H42 H 0.4619 -0.373 0.6459 0.0572 Uiso 1 0 . H43 H 0.524 -0.3323 0.7128 0.0572 Uiso 1 0 . H44 H 0.3443 -0.1644 0.604 0.0609 Uiso 1 0 . H45 H 0.3504 -0.268 0.5775 0.0609 Uiso 1 0 . H46 H 0.333 -0.254 0.6441 0.0609 Uiso 1 0 . H47 H 0.1959 0.1128 0.6579 0.0393 Uiso 1 0 . H48 H 0.2307 0.1388 0.6037 0.0393 Uiso 1 0 . H49 H 0.1372 -0.0345 0.4771 0.0486 Uiso 1 0 . H50 H 0.1931 0.0519 0.4934 0.0486 Uiso 1 0 . H51 H 0.2191 -0.0465 0.531 0.0486 Uiso 1 0 . H52 H 0.0731 0.1213 0.5773 0.0599 Uiso 1 0 . H53 H 0.1019 0.1524 0.5199 0.0599 Uiso 1 0 . H54 H 0.0458 0.0666 0.5068 0.0599 Uiso 1 0 . H55 H 0.1158 -0.0369 0.639 0.0547 Uiso 1 0 . H56 H 0.0912 -0.0918 0.5687 0.0547 Uiso 1 0 . H57 H 0.1738 -0.0995 0.6219 0.0547 Uiso 1 0 . H58 H 0.2238 0.2943 0.7118 0.0443 Uiso 1 0 . H59 H 0.2871 0.3558 0.7655 0.0443 Uiso 1 0 . H60 H 0.1719 0.3394 0.5875 0.0505 Uiso 1 0 . H61 H 0.2037 0.4287 0.5623 0.0505 Uiso 1 0 . H62 H 0.2519 0.3354 0.5852 0.0505 Uiso 1 0 . H63 H 0.3565 0.4345 0.6711 0.063 Uiso 1 0 . H64 H 0.3077 0.5277 0.6502 0.063 Uiso 1 0 . H65 H 0.3409 0.4946 0.7274 0.063 Uiso 1 0 . H66 H 0.2133 0.4982 0.7303 0.0596 Uiso 1 0 . H67 H 0.1776 0.5284 0.6526 0.0596 Uiso 1 0 . H68 H 0.1488 0.4367 0.6781 0.0596 Uiso 1 0 . H69 H 0.3211 0.2537 0.8775 0.0397 Uiso 1 0 . H70 H 0.3927 0.2036 0.9298 0.0397 Uiso 1 0 . H71 H 0.3509 0.3837 1.0292 0.0518 Uiso 1 0 . H72 H 0.2916 0.3255 0.9693 0.0518 Uiso 1 0 . H73 H 0.3605 0.2728 1.0234 0.0518 Uiso 1 0 . H74 H 0.3701 0.4957 0.94 0.0492 Uiso 1 0 . H75 H 0.3895 0.4514 0.8801 0.0492 Uiso 1 0 . H76 H 0.3097 0.437 0.8815 0.0492 Uiso 1 0 . H77 H 0.4891 0.298 1.0206 0.0523 Uiso 1 0 . H78 H 0.4993 0.3682 0.9665 0.0523 Uiso 1 0 . H79 H 0.4805 0.4087 1.0277 0.0523 Uiso 1 0 .