#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/4/4060164.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_4060164 _journal_name_full 'Organometallics' _journal_year 2005 _chemical_name_common '(5b) [Al(CH3)(DBP)(OTHF)]' _chemical_formula_moiety 'C40 H66 Al2 O6' _chemical_formula_sum 'C40 H66 Al2 O6' _chemical_formula_weight 696.89 _symmetry_cell_setting Monoclinic _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M 'P 2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.6840(16) _cell_length_b 12.117(2) _cell_length_c 17.288(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.609(3) _cell_angle_gamma 90.00 _cell_volume 2026.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.114 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _diffrn_ambient_temperature 203(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14409 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0488 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 26.49 _reflns_number_total 4161 _reflns_number_gt 3325 _reflns_threshold_expression >2sigma(I) _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^)+(0.0783P)^2^+1.3624P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4161 _refine_ls_number_parameters 224 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0782 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1713 _refine_ls_wR_factor_gt 0.1585 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 Al1 Al 0.90890(7) 0.06002(6) 0.05296(4) 0.0280(2) Uani 1 1 d . . . O1 O 0.8428(2) 0.21301(15) 0.01431(10) 0.0459(5) Uani 1 1 d . . . O2 O 0.98686(16) 0.11342(13) 0.13778(8) 0.0326(4) Uani 1 1 d . . . O3 O 1.02562(16) -0.06439(13) 0.04634(8) 0.0306(4) Uani 1 1 d . . . C1 C 0.7873(4) 0.3116(3) 0.04413(19) 0.0693(10) Uani 1 1 d . . . H1A H 0.8561 0.3491 0.0781 0.083 Uiso 1 1 calc R . . H1B H 0.7058 0.2955 0.0738 0.083 Uiso 1 1 calc R . . C2 C 0.7500(10) 0.3796(4) -0.0224(3) 0.186(4) Uani 1 1 d . . . H2A H 0.7973 0.4510 -0.0173 0.223 Uiso 1 1 calc R . . H2B H 0.6502 0.3933 -0.0242 0.223 Uiso 1 1 calc R . . C3 C 0.7875(4) 0.3268(3) -0.09364(18) 0.0616(9) Uani 1 1 d . . . H3A H 0.8707 0.3603 -0.1137 0.074 Uiso 1 1 calc R . . H3B H 0.7120 0.3317 -0.1333 0.074 Uiso 1 1 calc R . . C4 C 0.8139(3) 0.2073(3) -0.06942(16) 0.0537(7) Uani 1 1 d . . . H4 H 0.7293 0.1630 -0.0804 0.064 Uiso 1 1 calc R . . C6 C 1.0645(3) -0.1486(2) 0.09961(14) 0.0390(6) Uani 1 1 d . . . H6A H 0.9878 -0.2002 0.1052 0.047 Uiso 1 1 calc R . . H6B H 1.0886 -0.1165 0.1505 0.047 Uiso 1 1 calc R . . C7 C 0.6758(3) 0.1413(3) 0.2239(2) 0.0573(8) Uani 1 1 d . . . H7A H 0.6440 0.2138 0.2391 0.086 Uiso 1 1 calc R . . H7B H 0.6038 0.0873 0.2318 0.086 Uiso 1 1 calc R . . H7C H 0.6973 0.1425 0.1697 0.086 Uiso 1 1 calc R . . C8 C 0.8495(3) -0.0091(2) 0.25774(16) 0.0441(6) Uani 1 1 d . . . H8A H 0.8683 -0.0174 0.2034 0.066 Uiso 1 1 calc R . . H8B H 0.7753 -0.0587 0.2707 0.066 Uiso 1 1 calc R . . H8C H 0.9320 -0.0269 0.2892 0.066 Uiso 1 1 calc R . . C9 C 0.7652(5) 0.1123(3) 0.35811(19) 0.0782(11) Uani 1 1 d . . . H9A H 0.8451 0.0954 0.3918 0.117 Uiso 1 1 calc R . . H9B H 0.6935 0.0579 0.3655 0.117 Uiso 1 1 calc R . . H9C H 0.7307 0.1851 0.3705 0.117 Uiso 1 1 calc R . . C10 C 0.8066(3) 0.1102(2) 0.27345(14) 0.0381(6) Uani 1 1 d . . . C11 C 0.9201(2) 0.19464(19) 0.25763(13) 0.0324(5) Uani 1 1 d . . . C12 C 1.0069(2) 0.19033(18) 0.19363(12) 0.0289(5) Uani 1 1 d . . . C13 C 1.1202(2) 0.26480(18) 0.18964(13) 0.0326(5) Uani 1 1 d . . . C14 C 1.1270(3) 0.3527(2) 0.24197(16) 0.0425(6) Uani 1 1 d . . . H14 H 1.1968 0.4060 0.2378 0.051 Uiso 1 1 calc R . . C15 C 1.0342(3) 0.3634(2) 0.29953(18) 0.0529(8) Uani 1 1 d . . . H15 H 1.0379 0.4252 0.3324 0.063 Uiso 1 1 calc R . . C16 C 0.9366(3) 0.2837(2) 0.30842(16) 0.0455(7) Uani 1 1 d . . . H16 H 0.8784 0.2889 0.3503 0.055 Uiso 1 1 calc R . . C17 C 1.2375(3) 0.2482(2) 0.13375(14) 0.0374(6) Uani 1 1 d . . . C18 C 1.1887(3) 0.2681(3) 0.04919(16) 0.0531(8) Uani 1 1 d . . . H18A H 1.1197 0.2135 0.0337 0.080 Uiso 1 1 calc R . . H18B H 1.2668 0.2622 0.0162 0.080 Uiso 1 1 calc R . . H18C H 1.1488 0.3413 0.0442 0.080 Uiso 1 1 calc R . . C19 C 1.3582(3) 0.3279(3) 0.15071(18) 0.0540(8) Uani 1 1 d . . . H19A H 1.3268 0.4032 0.1425 0.081 Uiso 1 1 calc R . . H19B H 1.4321 0.3119 0.1163 0.081 Uiso 1 1 calc R . . H19C H 1.3921 0.3191 0.2040 0.081 Uiso 1 1 calc R . . C20 C 1.2959(3) 0.1313(2) 0.14432(16) 0.0440(6) Uani 1 1 d . . . H20A H 1.3269 0.1207 0.1980 0.066 Uiso 1 1 calc R . . H20B H 1.3733 0.1216 0.1113 0.066 Uiso 1 1 calc R . . H20C H 1.2245 0.0778 0.1304 0.066 Uiso 1 1 calc R . . C22 C 0.7231(3) -0.0046(3) 0.05348(16) 0.0493(7) Uani 1 1 d . . . H22A H 0.7122 -0.0434 0.1019 0.074 Uiso 1 1 calc R . . H22B H 0.7108 -0.0560 0.0107 0.074 Uiso 1 1 calc R . . H22C H 0.6545 0.0535 0.0481 0.074 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 Al1 0.0311(4) 0.0285(4) 0.0242(3) -0.0034(3) -0.0013(3) -0.0037(3) O1 0.0675(12) 0.0393(10) 0.0305(9) -0.0014(8) -0.0020(8) 0.0174(9) O2 0.0422(9) 0.0301(8) 0.0252(8) -0.0048(7) -0.0025(7) -0.0078(7) O3 0.0388(9) 0.0284(8) 0.0245(8) 0.0006(6) 0.0007(6) 0.0000(7) C1 0.111(3) 0.0431(17) 0.0539(19) -0.0036(15) 0.0042(18) 0.0287(18) C2 0.428(13) 0.069(3) 0.058(3) 0.010(2) -0.007(4) 0.100(5) C3 0.087(2) 0.0464(17) 0.0511(18) 0.0110(14) -0.0039(16) 0.0223(16) C4 0.072(2) 0.0517(17) 0.0367(14) 0.0027(13) -0.0068(13) 0.0119(15) C6 0.0539(15) 0.0338(13) 0.0289(12) 0.0057(10) -0.0021(10) 0.0028(11) C7 0.0359(14) 0.0452(17) 0.090(2) -0.0038(16) -0.0083(15) 0.0050(12) C8 0.0470(15) 0.0369(14) 0.0487(15) 0.0076(12) 0.0073(12) 0.0050(12) C9 0.109(3) 0.079(3) 0.0495(19) -0.0109(18) 0.0323(19) -0.012(2) C10 0.0410(13) 0.0393(14) 0.0343(13) -0.0041(11) 0.0040(10) 0.0047(11) C11 0.0329(12) 0.0303(12) 0.0332(12) -0.0036(10) -0.0084(9) 0.0100(10) C12 0.0347(12) 0.0242(11) 0.0265(11) -0.0021(9) -0.0110(9) 0.0039(9) C13 0.0380(12) 0.0250(11) 0.0335(12) 0.0003(9) -0.0130(10) 0.0010(10) C14 0.0433(14) 0.0288(13) 0.0538(16) -0.0086(12) -0.0162(12) -0.0013(11) C15 0.0569(17) 0.0397(15) 0.0609(18) -0.0259(14) -0.0109(14) 0.0069(13) C16 0.0448(15) 0.0465(16) 0.0446(15) -0.0163(12) -0.0027(12) 0.0103(12) C17 0.0422(14) 0.0337(13) 0.0353(13) 0.0010(10) -0.0076(10) -0.0104(11) C18 0.0611(18) 0.0564(18) 0.0408(15) 0.0081(13) -0.0078(13) -0.0223(15) C19 0.0506(16) 0.0532(18) 0.0575(18) -0.0037(14) -0.0064(13) -0.0204(14) C20 0.0410(14) 0.0427(15) 0.0484(15) -0.0045(12) 0.0030(11) -0.0017(12) C22 0.0393(14) 0.069(2) 0.0399(14) -0.0141(14) 0.0021(11) -0.0136(14) _cod_database_code 4060164