#------------------------------------------------------------------------------ #$Date: 2023-04-14 13:39:52 +0100 (Fri, 14 Apr 2023) $ #$Revision: 282633 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100824.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_1100824 loop_ _publ_author_name 'Evans, William J.' 'Kozimor, Stosh A.' 'Brady, Jason C.' 'Davis, Benjamin L.' 'Nyce, Gregory W.' 'Seibel, Christopher A.' 'Ziller, Joseph W.' 'Doedens, Robert J.' _publ_section_title ; Metallocene Allyl Reactivity in the Presence of Alkenes Tethered to Cyclopentadienyl Ligands ; _journal_issue 10 _journal_name_full Organometallics _journal_page_first 2269 _journal_page_last 2278 _journal_paper_doi 10.1021/om049286x _journal_volume 24 _journal_year 2005 _chemical_formula_sum 'C64 H116 Al2 Si4 Y2' _chemical_formula_weight 1229.71 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 93.695(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 11.0875(10) _cell_length_b 19.7843(18) _cell_length_c 15.6311(14) _cell_measurement_reflns_used ? _cell_measurement_temperature 171(2) _cell_measurement_theta_max ? _cell_measurement_theta_min ? _cell_volume 3421.7(5) _diffrn_ambient_temperature 171(2) _diffrn_detector_area_resol_mean ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1320 _diffrn_reflns_av_sigmaI/netI 0.1034 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 28964 _diffrn_reflns_theta_max 24.71 _diffrn_reflns_theta_min 1.66 _diffrn_standards_decay_% '< 1.0' _diffrn_standards_interval_count 'initial 50 frames recollected' _diffrn_standards_interval_time ? _diffrn_standards_number '50 frames' _exptl_absorpt_coefficient_mu 1.818 _exptl_absorpt_correction_T_max 0.8833 _exptl_absorpt_correction_T_min 0.5769 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Bruker SADABS' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description Irregular _exptl_crystal_F_000 1320 _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _refine_ls_extinction_coef 0.0032(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXTL _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 350 _refine_ls_number_reflns 5819 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.021 _refine_ls_R_factor_all 0.1233 _refine_ls_R_factor_gt 0.0531 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+2.2823P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1111 _refine_ls_wR_factor_ref 0.1381 _reflns_number_gt 3423 _reflns_number_total 5819 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'none' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas The following automatic conversions were performed: '_atom_sites_solution_hydrogens' value 'difmap & geom' was changed to 'mixed'. Automatic conversion script Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius ; _cod_original_sg_symbol_H-M P2(1)/n _cod_database_code 1100824 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' 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 Y1 Y 0.60017(5) 0.13404(3) 0.86845(3) 0.02667(18) Uani 1 1 d . . . Si1 Si 0.45240(15) 0.32158(8) 0.91390(11) 0.0402(4) Uani 1 1 d . . . Si2 Si 0.33404(16) 0.10396(9) 0.67591(11) 0.0408(4) Uani 1 1 d . . . Al1 Al 0.76207(15) -0.05838(8) 1.01587(11) 0.0308(4) Uani 1 1 d . . . C1 C 0.5825(5) 0.1535(3) 0.6992(3) 0.0350(14) Uani 1 1 d . . . C2 C 0.7000(5) 0.1290(3) 0.7167(3) 0.0408(15) Uani 1 1 d . . . C3 C 0.6928(5) 0.0609(3) 0.7435(3) 0.0401(15) Uani 1 1 d . . . C4 C 0.5691(5) 0.0429(3) 0.7434(3) 0.0332(14) Uani 1 1 d . . . C5 C 0.4966(5) 0.1012(3) 0.7157(3) 0.0323(13) Uani 1 1 d . . . C6 C 0.5522(6) 0.2193(3) 0.6553(4) 0.0545(18) Uani 1 1 d . . . H6A H 0.5510 0.2131 0.5930 0.082 Uiso 1 1 calc R . . H6B H 0.6132 0.2532 0.6732 0.082 Uiso 1 1 calc R . . H6C H 0.4725 0.2347 0.6710 0.082 Uiso 1 1 calc R . . C7 C 0.8166(6) 0.1640(4) 0.6957(4) 0.0592(19) Uani 1 1 d . . . H7A H 0.8334 0.1545 0.6362 0.089 Uiso 1 1 calc R . . H7B H 0.8834 0.1473 0.7341 0.089 Uiso 1 1 calc R . . H7C H 0.8081 0.2129 0.7035 0.089 Uiso 1 1 calc R . . C8 C 0.8003(5) 0.0145(4) 0.7591(4) 0.0549(18) Uani 1 1 d . . . H8A H 0.8189 -0.0071 0.7050 0.082 Uiso 1 1 calc R . . H8B H 0.7814 -0.0203 0.8008 0.082 Uiso 1 1 calc R . . H8C H 0.8704 0.0407 0.7815 0.082 Uiso 1 1 calc R . . C9 C 0.5250(5) -0.0275(3) 0.7587(4) 0.0422(15) Uani 1 1 d . . . H9A H 0.5200 -0.0526 0.7046 0.063 Uiso 1 1 calc R . . H9B H 0.4448 -0.0255 0.7816 0.063 Uiso 1 1 calc R . . H9C H 0.5814 -0.0504 0.8001 0.063 Uiso 1 1 calc R . . C10 C 0.6907(5) 0.2571(3) 0.8923(3) 0.0331(14) Uani 1 1 d . . . C11 C 0.7716(5) 0.2133(3) 0.9396(4) 0.0347(14) Uani 1 1 d . . . C12 C 0.7110(5) 0.1888(3) 1.0102(4) 0.0368(14) Uani 1 1 d . . . C13 C 0.5938(5) 0.2154(3) 1.0062(3) 0.0326(14) Uani 1 1 d . . . C14 C 0.5769(5) 0.2574(3) 0.9317(4) 0.0325(13) Uani 1 1 d . . . C15 C 0.7301(5) 0.3061(3) 0.8259(4) 0.0480(17) Uani 1 1 d . . . H15A H 0.7601 0.3475 0.8542 0.072 Uiso 1 1 calc R . . H15B H 0.6613 0.3169 0.7857 0.072 Uiso 1 1 calc R . . H15C H 0.7947 0.2857 0.7945 0.072 Uiso 1 1 calc R . . C16 C 0.9034(5) 0.2028(3) 0.9262(4) 0.0511(17) Uani 1 1 d . . . H16A H 0.9513 0.2374 0.9578 0.077 Uiso 1 1 calc R . . H16B H 0.9166 0.2063 0.8650 0.077 Uiso 1 1 calc R . . H16C H 0.9283 0.1579 0.9471 0.077 Uiso 1 1 calc R . . C17 C 0.7734(6) 0.1508(3) 1.0835(4) 0.0530(18) Uani 1 1 d . . . H17A H 0.8059 0.1829 1.1268 0.080 Uiso 1 1 calc R . . H17B H 0.8396 0.1239 1.0624 0.080 Uiso 1 1 calc R . . H17C H 0.7154 0.1207 1.1091 0.080 Uiso 1 1 calc R . . C18 C 0.5088(5) 0.2060(3) 1.0774(4) 0.0447(16) Uani 1 1 d . . . H18A H 0.5233 0.2417 1.1204 0.067 Uiso 1 1 calc R . . H18B H 0.5231 0.1618 1.1044 0.067 Uiso 1 1 calc R . . H18C H 0.4250 0.2086 1.0535 0.067 Uiso 1 1 calc R . . C19 C 0.4372(7) 0.3569(4) 0.8050(4) 0.069(2) Uani 1 1 d . . . H19A H 0.5143 0.3768 0.7908 0.103 Uiso 1 1 calc R . . H19B H 0.3744 0.3918 0.8021 0.103 Uiso 1 1 calc R . . H19C H 0.4147 0.3209 0.7640 0.103 Uiso 1 1 calc R . . C20 C 0.4806(6) 0.3939(3) 0.9875(4) 0.0554(18) Uani 1 1 d . . . H20A H 0.5577 0.4152 0.9760 0.083 Uiso 1 1 calc R . . H20B H 0.4839 0.3779 1.0469 0.083 Uiso 1 1 calc R . . H20C H 0.4151 0.4269 0.9785 0.083 Uiso 1 1 calc R . . C21 C 0.3020(6) 0.2847(3) 0.9383(5) 0.062(2) Uani 1 1 d . . . H21A H 0.2872 0.2439 0.9027 0.075 Uiso 1 1 calc R . . H21B H 0.3061 0.2704 0.9991 0.075 Uiso 1 1 calc R . . C22 C 0.1977(7) 0.3315(4) 0.9230(7) 0.095(3) Uani 1 1 d . . . H22A H 0.1976 0.3695 0.9602 0.114 Uiso 1 1 calc R . . C23 C 0.1153(9) 0.3286(6) 0.8717(8) 0.144(5) Uani 1 1 d . . . H23A H 0.1092 0.2920 0.8322 0.172 Uiso 1 1 calc R . . H23B H 0.0550 0.3627 0.8698 0.172 Uiso 1 1 calc R . . C24 C 0.2538(5) 0.0236(3) 0.6899(4) 0.0533(18) Uani 1 1 d . . . H24A H 0.2573 0.0117 0.7508 0.080 Uiso 1 1 calc R . . H24B H 0.2921 -0.0121 0.6578 0.080 Uiso 1 1 calc R . . H24C H 0.1692 0.0285 0.6685 0.080 Uiso 1 1 calc R . . C25 C 0.2465(6) 0.1719(3) 0.7274(4) 0.0549(18) Uani 1 1 d . . . H25A H 0.2489 0.1643 0.7894 0.082 Uiso 1 1 calc R . . H25B H 0.1624 0.1710 0.7039 0.082 Uiso 1 1 calc R . . H25C H 0.2823 0.2160 0.7158 0.082 Uiso 1 1 calc R . . C26 C 0.3243(6) 0.1225(3) 0.5579(4) 0.0574(19) Uani 1 1 d . . . H26A H 0.2381 0.1261 0.5377 0.069 Uiso 1 1 calc R . . H26B H 0.3627 0.1668 0.5484 0.069 Uiso 1 1 calc R . . C27 C 0.3820(7) 0.0714(4) 0.5064(4) 0.070(2) Uani 1 1 d . . . H27A H 0.4675 0.0730 0.5050 0.084 Uiso 1 1 calc R . . C28 C 0.3239(8) 0.0232(4) 0.4616(5) 0.078(2) Uani 1 1 d . . . H28A H 0.2384 0.0201 0.4614 0.094 Uiso 1 1 calc R . . H28B H 0.3677 -0.0081 0.4297 0.094 Uiso 1 1 calc R . . C29 C 0.6946(6) 0.0265(3) 0.9557(4) 0.0306(14) Uani 1 1 d . . . C30 C 0.6112(5) -0.0925(3) 1.0722(4) 0.0308(14) Uani 1 1 d . . . C31 C 0.8113(5) -0.1249(3) 0.9294(4) 0.0414(15) Uani 1 1 d . . . H31A H 0.8832 -0.1083 0.9027 0.062 Uiso 1 1 calc R . . H31B H 0.7453 -0.1309 0.8853 0.062 Uiso 1 1 calc R . . H31C H 0.8296 -0.1683 0.9575 0.062 Uiso 1 1 calc R . . C32 C 0.8973(5) -0.0363(3) 1.1009(3) 0.0401(15) Uani 1 1 d . . . H32A H 0.9668 -0.0203 1.0708 0.060 Uiso 1 1 calc R . . H32B H 0.9203 -0.0768 1.1341 0.060 Uiso 1 1 calc R . . H32C H 0.8716 -0.0009 1.1396 0.060 Uiso 1 1 calc R . . H29A H 0.759(5) 0.051(3) 0.935(3) 0.044(17) Uiso 1 1 d . . . H29B H 0.653(4) 0.050(3) 0.997(3) 0.032(15) Uiso 1 1 d . . . H29C H 0.645(4) 0.009(3) 0.916(3) 0.028(16) Uiso 1 1 d . . . H30A H 0.619(4) -0.135(3) 1.096(3) 0.037(16) Uiso 1 1 d . . . H30B H 0.602(4) -0.063(3) 1.114(3) 0.037(16) Uiso 1 1 d . . . H30C H 0.548(5) -0.097(3) 1.022(4) 0.047(17) Uiso 1 1 d . . . 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 Y1 0.0354(3) 0.0201(3) 0.0242(3) 0.0005(3) -0.0006(2) -0.0020(3) Si1 0.0446(10) 0.0261(9) 0.0490(11) -0.0024(8) -0.0038(8) 0.0032(8) Si2 0.0475(11) 0.0387(10) 0.0350(10) 0.0002(8) -0.0074(8) -0.0010(8) Al1 0.0347(10) 0.0244(9) 0.0333(10) 0.0020(7) 0.0021(8) 0.0037(7) C1 0.052(4) 0.030(3) 0.022(3) 0.005(2) 0.001(3) -0.005(3) C2 0.050(4) 0.049(4) 0.025(3) -0.001(3) 0.010(3) -0.015(3) C3 0.052(4) 0.050(4) 0.019(3) -0.006(3) 0.001(3) 0.010(3) C4 0.052(4) 0.027(3) 0.020(3) -0.002(2) -0.004(3) -0.003(3) C5 0.042(3) 0.032(3) 0.023(3) -0.005(3) -0.003(3) 0.004(3) C6 0.092(5) 0.042(4) 0.028(4) 0.007(3) -0.010(3) -0.015(4) C7 0.055(4) 0.079(5) 0.045(4) -0.013(4) 0.014(3) -0.020(4) C8 0.055(4) 0.074(5) 0.035(4) -0.015(3) 0.006(3) 0.014(4) C9 0.058(4) 0.033(4) 0.034(3) -0.005(3) -0.011(3) 0.004(3) C10 0.047(4) 0.020(3) 0.032(3) -0.007(3) 0.001(3) -0.009(3) C11 0.040(4) 0.025(3) 0.038(4) -0.014(3) -0.006(3) -0.002(3) C12 0.048(4) 0.025(3) 0.036(4) -0.010(3) -0.009(3) -0.001(3) C13 0.050(4) 0.020(3) 0.027(3) -0.003(2) -0.001(3) -0.007(3) C14 0.038(3) 0.020(3) 0.039(3) -0.004(3) 0.001(3) -0.005(2) C15 0.051(4) 0.040(4) 0.053(4) 0.003(3) 0.001(3) -0.016(3) C16 0.040(4) 0.050(4) 0.062(5) -0.017(3) -0.004(3) -0.002(3) C17 0.074(5) 0.034(4) 0.048(4) -0.008(3) -0.022(4) 0.003(3) C18 0.058(4) 0.042(4) 0.035(4) -0.006(3) 0.004(3) -0.003(3) C19 0.085(5) 0.065(5) 0.056(5) 0.010(4) -0.002(4) 0.031(4) C20 0.060(4) 0.035(4) 0.071(5) -0.006(3) -0.002(4) 0.011(3) C21 0.051(4) 0.042(4) 0.093(6) 0.006(4) -0.008(4) 0.008(3) C22 0.051(5) 0.036(4) 0.198(11) -0.004(6) -0.006(6) -0.002(4) C23 0.071(7) 0.111(9) 0.245(15) 0.106(9) -0.010(8) -0.006(6) C24 0.049(4) 0.058(4) 0.052(4) -0.011(3) -0.003(3) -0.008(3) C25 0.051(4) 0.051(4) 0.061(5) 0.002(4) -0.006(3) 0.008(3) C26 0.066(5) 0.057(5) 0.048(4) 0.008(4) -0.011(4) 0.000(4) C27 0.073(5) 0.094(7) 0.041(4) 0.004(4) -0.003(4) 0.003(5) C28 0.108(7) 0.081(6) 0.045(5) 0.000(4) 0.008(4) 0.016(5) C29 0.034(4) 0.027(3) 0.032(4) -0.005(3) 0.006(3) -0.005(3) C30 0.042(4) 0.023(4) 0.027(3) 0.000(3) -0.002(3) 0.000(3) C31 0.051(4) 0.029(3) 0.046(4) 0.003(3) 0.008(3) 0.009(3) C32 0.045(4) 0.043(4) 0.032(3) 0.010(3) -0.002(3) -0.002(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'