#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/5/5000370.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_5000370 ## 'minor manual editing of SDT2CIF v. 1.1 BETA output' _chemical_formula_sum 'C132 H155 N O8 W2' _[local]_cod_chemical_formula_sum_orig 'C132 H155 N1 O8 W2' _chemical_formula_moiety '(C88 H104 O8 W2), (H), (C2 H8 N), 7(C6 H6)' _chemical_formula_weight 2251.36 _cell_length_a 25.421(3) _cell_length_b 34.611(3) _cell_length_c 13.1126(13) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 11537(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 290 _cell_measurement_theta_min 9.54 _cell_measurement_theta_max 11.44 _cell_measurement_temperature 106 _exptl_crystal_colour green _exptl_crystal_description 'trigonal prism' _exptl_crystal_size_max .30 _exptl_crystal_size_mid .30 _exptl_crystal_size_min .25 _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4664 _exptl_absorpt_coefficient_mu 2.0509 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details Tompa _exptl_absorpt_correction_T_min 0.547 _exptl_absorpt_correction_T_max 0.648 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2+z x,1/2-y,z 1/2-x,-y,1/2+z 1/2+x,y,1/2-z -x,1/2+y,-z 1/2+x,1/2-y,1/2-z -x,-y,-z _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature 106 _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16789 _diffrn_reflns_av_R_equivalents 0.063 _diffrn_reflns_theta_min 3.09474 _diffrn_reflns_theta_max 25.0873 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 15 _diffrn_standards_number 4 _diffrn_standards_decay_% -4.9 _diffrn_standards_interval_count 300 _reflns_number_total 10423 _reflns_number_gt 6231 _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' N N 0.004 0.003 '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 10300 _refine_ls_number_parameters 653 _refine_ls_hydrogen_treatment noref _refine_ls_extinction_coef -0.000000015(9) _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 0.0578 _refine_ls_wR_factor_ref 0.0519 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_shift/su_max 0.06 _refine_diff_density_max 2.7 _refine_diff_density_min 1.0 _refine_special_details ; The structure was solved by a combination of direct methods (MULTAN-78) and Fourier techniques. The unique W atom and several atoms from the calix[4]arene ligand were located in the initial E- map. The remaining non-hydrogen atoms were located in iterations of least-squares refinement followed by a difference Fourier calculation. The asymmetric unit was found to contain one half of the W-dimer, one molecule of dimethylamine located in a mirror plane, two full molecules of benzene and three half molecules of benzene solvent, each situated across a mirror plane. The dimer is located on a crystallographic mirror plane, with the mirror at the midpoint of the W-W bond. Disorder was observed in the tert-butyl group on C(22) where atoms C(43) and C(50) refined to 66 and 44% occupancy, respectively. Many hydrogen atoms were evident in a difference map after initial refinement. Hydrogen atoms were introduced in fixed idealized positions with isotropic thermal parameters equal to 1.0 plus the isotropic equivalent of the parent atom. The hydrogen atoms on the dimethylamine were not located. A peak of 0.75e/A3 was located in the mirror plane between O(2) and O(2)' in a position that is plausible for the expected hydrogen atom, H(84). The final cycles of least-squares refinement were carried out with anisotropic thermal parameters on all but three atoms: C(50), the minor component of the disorder (see above), and atoms C(18) and C(31) which did not converge well to the anisotropic form. The final difference map contained a peak of 2.7e/A3 on the mirror plane half-way between the two tungsten atoms. The deepest hole was -1e/A3, in the same section. ; 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 0.322367(14) 0.283283(11) 0.56712(3) 0.02110(11) Uani 1 0 . O2 O 0.2884(2) 0.28378(19) 0.4240(4) 0.0243(19) Uani 1 0 . O3 O 0.2513(2) 0.29264(18) 0.6167(5) 0.022(2) Uani 1 0 . O4 O 0.3534(2) 0.29591(17) 0.7010(5) 0.021(2) Uani 1 0 . O5 O 0.3895(2) 0.29196(19) 0.4975(5) 0.025(2) Uani 1 0 . C6 C 0.2754(4) 0.3158(3) 0.3670(7) 0.024(3) Uani 1 0 . C7 C 0.3123(3) 0.3315(3) 0.3012(7) 0.028(3) Uani 1 0 . C8 C 0.2982(4) 0.3633(3) 0.2426(7) 0.028(3) Uani 1 0 . C9 C 0.2479(4) 0.3795(3) 0.2453(8) 0.031(3) Uani 1 0 . C10 C 0.2124(4) 0.3638(3) 0.3127(7) 0.026(3) Uani 1 0 . C11 C 0.2243(3) 0.3315(3) 0.3741(7) 0.023(3) Uani 1 0 . C12 C 0.1857(3) 0.3167(2) 0.4516(7) 0.021(3) Uani 1 0 . C13 C 0.1888(3) 0.3377(3) 0.5525(7) 0.024(3) Uani 1 0 . C14 C 0.1563(4) 0.3698(3) 0.5725(9) 0.030(3) Uani 1 0 . C15 C 0.1582(4) 0.3904(3) 0.6631(8) 0.030(3) Uani 1 0 . C16 C 0.1950(4) 0.3782(3) 0.7359(8) 0.031(3) Uani 1 0 . C17 C 0.2275(4) 0.3459(3) 0.7209(8) 0.029(3) Uani 1 0 . C18 C 0.2243(4) 0.3257(3) 0.6277(7) 0.023(2) Uiso 1 0 . C19 C 0.2668(4) 0.3345(3) 0.7999(8) 0.028(3) Uani 1 0 . C20 C 0.3194(4) 0.3537(3) 0.7819(7) 0.029(3) Uani 1 0 . C21 C 0.3292(4) 0.3904(3) 0.8159(7) 0.031(3) Uani 1 0 . C22 C 0.3761(4) 0.4103(3) 0.7968(8) 0.030(3) Uani 1 0 . C23 C 0.4137(4) 0.3907(3) 0.7394(8) 0.031(3) Uani 1 0 . C24 C 0.4076(3) 0.3536(3) 0.7052(7) 0.027(3) Uani 1 0 . C25 C 0.3601(4) 0.3345(3) 0.7253(7) 0.022(3) Uani 1 0 . C26 C 0.4504(4) 0.3345(3) 0.6407(8) 0.030(4) Uani 1 0 . C27 C 0.4459(4) 0.3459(3) 0.5271(8) 0.030(4) Uani 1 0 . C28 C 0.4732(4) 0.3771(3) 0.4885(8) 0.033(4) Uani 1 0 . C29 C 0.4685(4) 0.3895(3) 0.3888(9) 0.037(4) Uani 1 0 . C30 C 0.4334(4) 0.3686(4) 0.3269(8) 0.042(4) Uani 1 0 . C31 C 0.4061(4) 0.3365(3) 0.3622(8) 0.029(3) Uiso 1 0 . C32 C 0.4125(4) 0.3247(3) 0.4628(7) 0.028(3) Uani 1 0 . C33 C 0.3676(4) 0.3155(3) 0.2936(8) 0.028(3) Uani 1 0 . C34 C 0.2348(4) 0.4128(3) 0.1742(8) 0.035(4) Uani 1 0 . C35 C 0.2730(5) 0.4458(4) 0.1885(9) 0.054(5) Uani 1 0 . C36 C 0.1783(5) 0.4283(4) 0.1921(11) 0.069(5) Uani 1 0 . C37 C 0.2382(5) 0.3988(3) 0.0628(9) 0.049(4) Uani 1 0 . C38 C 0.1233(4) 0.4256(3) 0.6842(9) 0.037(4) Uani 1 0 . C39 C 0.0854(5) 0.4155(4) 0.7745(10) 0.059(5) Uani 1 0 . C40 C 0.0900(5) 0.4370(3) 0.5943(10) 0.053(5) Uani 1 0 . C41 C 0.1565(5) 0.4601(4) 0.7149(10) 0.057(5) Uani 1 0 . C42 C 0.3852(4) 0.4509(3) 0.8412(10) 0.046(4) Uani 1 0 . C43 C 0.3379(8) 0.4771(5) 0.8020(19) 0.063(8) Uani 0.66 0 . C44 C 0.4318(6) 0.4701(4) 0.7993(15) 0.101(8) Uani 1 0 . C45 C 0.3900(11) 0.4479(5) 0.9551(13) 0.148(12) Uani 1 0 . C46 C 0.5004(4) 0.4224(4) 0.3408(9) 0.047(4) Uani 1 0 . C47 C 0.4619(6) 0.4526(4) 0.2918(11) 0.072(6) Uani 1 0 . C48 C 0.5356(5) 0.4063(4) 0.2597(10) 0.066(5) Uani 1 0 . C49 C 0.5333(5) 0.4430(4) 0.4190(11) 0.071(6) Uani 1 0 . C50 C 0.3396(17) 0.4711(13) 0.881(3) 0.059(12) Uiso 0.34 0 . N51 N 0.3878(6) 0.25 0.8600(10) 0.052(6) Uani 1 0 . C52 C 0.4431(8) 0.25 0.8623(19) 0.090(10) Uani 1 0 . C53 C 0.3537(10) 0.25 0.9463(14) 0.108(13) Uani 1 0 . C54 C 0.2799(6) 0.4225(4) 0.5165(10) 0.061(5) Uani 1 0 . C55 C 0.3324(5) 0.4196(4) 0.5305(11) 0.063(5) Uani 1 0 . C56 C 0.3637(5) 0.4509(5) 0.5114(11) 0.072(7) Uani 1 0 . C57 C 0.3424(6) 0.4855(5) 0.4796(11) 0.067(6) Uani 1 0 . C58 C 0.2897(6) 0.4883(4) 0.4669(9) 0.052(5) Uani 1 0 . C59 C 0.2586(5) 0.4566(5) 0.4858(10) 0.052(5) Uani 1 0 . C60 C 0.0073(11) 0.3356(8) 0.5852(13) 0.129(13) Uani 1 0 . C61 C 0.0409(7) 0.3127(7) 0.5286(14) 0.118(10) Uani 1 0 . C62 C 0.0255(6) 0.3003(5) 0.4299(11) 0.079(6) Uani 1 0 . C63 C -0.0203(5) 0.3118(6) 0.3936(11) 0.082(7) Uani 1 0 . C64 C -0.0502(10) 0.3367(7) 0.4517(13) 0.155(12) Uani 1 0 . C65 C -0.0388(13) 0.3471(7) 0.5464(13) 0.166(15) Uani 1 0 . C66 C 0.1329(6) 0.25 0.7208(11) 0.040(6) Uani 1 0 . C67 C 0.1140(4) 0.2840(4) 0.7580(9) 0.049(4) Uani 1 0 . C68 C 0.0755(4) 0.2847(3) 0.8345(10) 0.049(4) Uani 1 0 . C69 C 0.0570(6) 0.25 0.8699(12) 0.044(6) Uani 1 0 . C70 C 0.5102(6) 0.25 0.3645(12) 0.050(7) Uani 1 0 . C71 C 0.5337(5) 0.2846(4) 0.3498(9) 0.056(5) Uani 1 0 . C72 C 0.5856(5) 0.2836(4) 0.3179(10) 0.063(5) Uani 1 0 . C73 C 0.6119(6) 0.25 0.3017(13) 0.054(7) Uani 1 0 . C74 C 0.2581(6) 0.25 0.1411(12) 0.039(6) Uani 1 0 . C75 C 0.2425(4) 0.2847(3) 0.1016(8) 0.039(4) Uani 1 0 . C76 C 0.2087(5) 0.2844(4) 0.0189(9) 0.045(4) Uani 1 0 . C77 C 0.1923(5) 0.25 -0.0223(11) 0.033(5) Uani 1 0 . H1 H 0.3239 0.3741 0.1986 0.04 Uiso 1 0 . H2 H 0.1786 0.3751 0.3183 0.039 Uiso 1 0 . H3 H 0.1512 0.3197 0.4252 0.0337 Uiso 1 0 . H4 H 0.1926 0.2901 0.4631 0.0337 Uiso 1 0 . H5 H 0.1317 0.3775 0.5217 0.0429 Uiso 1 0 . H6 H 0.198 0.3921 0.7981 0.044 Uiso 1 0 . H7 H 0.2541 0.342 0.8652 0.0415 Uiso 1 0 . H8 H 0.2714 0.3073 0.7986 0.0415 Uiso 1 0 . H9 H 0.3024 0.4031 0.8543 0.0442 Uiso 1 0 . H10 H 0.4454 0.4038 0.7225 0.0438 Uiso 1 0 . H11 H 0.4838 0.3424 0.6658 0.0421 Uiso 1 0 . H12 H 0.4472 0.3073 0.6466 0.0421 Uiso 1 0 . H13 H 0.4969 0.3903 0.5323 0.0457 Uiso 1 0 . H14 H 0.4286 0.3767 0.2583 0.0546 Uiso 1 0 . H15 H 0.3669 0.289 0.3123 0.0399 Uiso 1 0 . H16 H 0.3791 0.3179 0.2249 0.0399 Uiso 1 0 . H17 H 0.3076 0.4367 0.1762 0.0662 Uiso 1 0 . H18 H 0.2647 0.4658 0.1419 0.0662 Uiso 1 0 . H19 H 0.2704 0.4551 0.2563 0.0662 Uiso 1 0 . H20 H 0.1752 0.4369 0.2605 0.0812 Uiso 1 0 . H21 H 0.172 0.4493 0.147 0.0812 Uiso 1 0 . H22 H 0.1538 0.4083 0.1793 0.0812 Uiso 1 0 . H23 H 0.2139 0.3785 0.0523 0.0609 Uiso 1 0 . H24 H 0.2305 0.4197 0.0182 0.0609 Uiso 1 0 . H25 H 0.2729 0.3897 0.0497 0.0609 Uiso 1 0 . H26 H 0.0637 0.4372 0.7891 0.0733 Uiso 1 0 . H27 H 0.0641 0.3941 0.7565 0.0733 Uiso 1 0 . H28 H 0.1056 0.4092 0.8333 0.0733 Uiso 1 0 . H29 H 0.068 0.4581 0.6131 0.0659 Uiso 1 0 . H30 H 0.1121 0.4445 0.5396 0.0659 Uiso 1 0 . H31 H 0.0688 0.4158 0.5741 0.0659 Uiso 1 0 . H32 H 0.1764 0.4539 0.7738 0.0697 Uiso 1 0 . H33 H 0.1795 0.4666 0.6605 0.0697 Uiso 1 0 . H34 H 0.1342 0.4814 0.7292 0.0697 Uiso 1 0 . H35 H 0.3422 0.5031 0.8246 0.0742 Uiso 1 0 . H36 H 0.337 0.4771 0.7288 0.0742 Uiso 1 0 . H37 H 0.3052 0.4674 0.8265 0.0742 Uiso 1 0 . H38 H 0.4618 0.4552 0.8133 0.1173 Uiso 1 0 . H39 H 0.4274 0.4733 0.7281 0.1173 Uiso 1 0 . H40 H 0.4351 0.495 0.8305 0.1173 Uiso 1 0 . H41 H 0.3584 0.437 0.9816 0.1678 Uiso 1 0 . H42 H 0.4187 0.4317 0.9714 0.1678 Uiso 1 0 . H43 H 0.3952 0.4728 0.9829 0.1678 Uiso 1 0 . H44 H 0.482 0.4728 0.2617 0.0841 Uiso 1 0 . H45 H 0.4413 0.4403 0.2411 0.0841 Uiso 1 0 . H46 H 0.4398 0.4629 0.3432 0.0841 Uiso 1 0 . H47 H 0.5595 0.3885 0.2892 0.0785 Uiso 1 0 . H48 H 0.5148 0.3934 0.2098 0.0785 Uiso 1 0 . H49 H 0.5543 0.4268 0.2285 0.0785 Uiso 1 0 . H50 H 0.5574 0.4253 0.4485 0.0831 Uiso 1 0 . H51 H 0.5515 0.4635 0.3874 0.0831 Uiso 1 0 . H52 H 0.5107 0.4529 0.4709 0.0831 Uiso 1 0 . H53 H 0.3793 0.2724 0.8244 0.0702 Uiso 1 0 . H54 H 0.4562 0.2276 0.897 0.1023 Uiso 1 0 . H55 H 0.4565 0.25 0.7945 0.1023 Uiso 1 0 . H56 H 0.4562 0.2724 0.897 0.1023 Uiso 1 0 . H57 H 0.3581 0.2724 0.9871 0.1329 Uiso 1 0 . H58 H 0.3174 0.25 0.9218 0.1329 Uiso 1 0 . H59 H 0.3581 0.2276 0.9871 0.1329 Uiso 1 0 . H60 H 0.258 0.4005 0.5281 0.0733 Uiso 1 0 . H61 H 0.3473 0.396 0.5536 0.076 Uiso 1 0 . H62 H 0.4008 0.4487 0.5197 0.0844 Uiso 1 0 . H63 H 0.3646 0.507 0.4669 0.0797 Uiso 1 0 . H64 H 0.2746 0.5119 0.4453 0.0641 Uiso 1 0 . H65 H 0.2215 0.4583 0.4772 0.0635 Uiso 1 0 . H66 H 0.0153 0.3429 0.6533 0.1376 Uiso 1 0 . H67 H 0.0742 0.3063 0.5555 0.1286 Uiso 1 0 . H68 H 0.0474 0.2834 0.3911 0.0947 Uiso 1 0 . H69 H -0.0326 0.3028 0.3293 0.0966 Uiso 1 0 . H70 H -0.0796 0.348 0.4204 0.1626 Uiso 1 0 . H71 H -0.0633 0.3619 0.5846 0.1748 Uiso 1 0 . H72 H 0.159 0.25 0.669 0.0524 Uiso 1 0 . H73 H 0.1269 0.3077 0.7314 0.0625 Uiso 1 0 . H74 H 0.063 0.3085 0.8614 0.0612 Uiso 1 0 . H75 H 0.0301 0.25 0.9202 0.0584 Uiso 1 0 . H76 H 0.4745 0.25 0.3869 0.0618 Uiso 1 0 . H77 H 0.5154 0.3084 0.3602 0.0689 Uiso 1 0 . H78 H 0.6037 0.3073 0.3082 0.0748 Uiso 1 0 . H79 H 0.6473 0.25 0.279 0.0687 Uiso 1 0 . H80 H 0.2805 0.25 0.199 0.051 Uiso 1 0 . H81 H 0.255 0.3084 0.1298 0.0505 Uiso 1 0 . H82 H 0.1969 0.3084 -0.0094 0.0583 Uiso 1 0 . H83 H 0.1695 0.25 -0.0797 0.0441 Uiso 1 0 . H84 H 0.272 0.25 0.4069 0.0367 Uiso 1 0 . _cod_database_code 5000370