#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100712.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_1100712 _publ_requested_journal 'Inorganic Chemistry' loop_ _publ_author_name 'Leslie W. Pineda' 'Vojtech Jancik' 'Herbert W. Roesky*' 'Regine Herbst-Irmer' _chemical_formula_moiety LGe(m-O)ZrCp2Me _chemical_formula_sum 'C40 H54 Ge N2 O Zr' _chemical_formula_weight 742.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.444(1) _cell_length_b 10.522(1) _cell_length_c 19.750(1) _cell_angle_alpha 88.64(1) _cell_angle_beta 89.60(1) _cell_angle_gamma 67.44(1) _cell_volume 1812(1) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5044 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 58.96 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 3.617 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7137 _exptl_absorpt_correction_T_max 0.8992 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'mirror system' _diffrn_measurement_device_type 'Bruker three circle diffractometer' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean 5.602 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14140 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 58.96 _reflns_number_total 5044 _reflns_number_gt 4879 _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^)+(0.0306P)^2^+2.5234P] 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 SHELXL _refine_ls_extinction_coef 0.00036(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5044 _refine_ls_number_parameters 421 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0297 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0735 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _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 Zr1 Zr -0.14748(3) 0.92344(2) 0.239776(11) 0.02037(10) Uani 1 1 d . . . Ge1 Ge 0.26023(3) 0.78468(3) 0.251684(14) 0.01964(11) Uani 1 1 d . . . N1 N 0.3612(2) 0.6265(2) 0.18811(10) 0.0194(5) Uani 1 1 d . . . O1 O 0.0661(2) 0.79553(19) 0.24598(9) 0.0242(4) Uani 1 1 d . . . C1 C 0.5647(3) 0.4803(3) 0.39116(13) 0.0236(6) Uani 1 1 d . . . H1A H 0.4913 0.4973 0.4285 0.035 Uiso 0.50 1 calc PR . . H1B H 0.6446 0.5139 0.4030 0.035 Uiso 0.50 1 calc PR . . H1C H 0.6117 0.3813 0.3830 0.035 Uiso 0.50 1 calc PR . . H1D H 0.6737 0.4311 0.3812 0.035 Uiso 0.50 1 calc PR . . H1E H 0.5204 0.4144 0.4067 0.035 Uiso 0.50 1 calc PR . . H1F H 0.5533 0.5470 0.4266 0.035 Uiso 0.50 1 calc PR . . N2 N 0.3370(2) 0.6419(2) 0.33005(10) 0.0183(5) Uani 1 1 d . . . C2 C 0.4822(3) 0.5550(3) 0.32784(13) 0.0187(6) Uani 1 1 d . . . C3 C 0.5663(3) 0.5267(3) 0.26735(13) 0.0194(6) Uani 1 1 d . . . H3A H 0.664(4) 0.476(3) 0.2714(15) 0.023 Uiso 1 1 d . . . C4 C 0.5076(3) 0.5491(3) 0.20125(13) 0.0189(6) Uani 1 1 d . . . C5 C 0.6165(3) 0.4840(3) 0.14429(13) 0.0252(6) Uani 1 1 d . . . H5A H 0.5629 0.4545 0.1095 0.038 Uiso 1 1 calc R . . H5B H 0.7032 0.4041 0.1619 0.038 Uiso 1 1 calc R . . H5C H 0.6543 0.5513 0.1244 0.038 Uiso 1 1 calc R . . C6 C 0.2942(3) 0.6236(3) 0.12282(13) 0.0208(6) Uani 1 1 d . . . C7 C 0.2944(3) 0.7176(3) 0.07119(13) 0.0234(6) Uani 1 1 d . . . C8 C 0.2188(3) 0.7160(3) 0.01059(14) 0.0291(7) Uani 1 1 d . . . H8A H 0.2135 0.7811 -0.0244 0.035 Uiso 1 1 calc R . . C9 C 0.1522(3) 0.6227(3) 0.00064(14) 0.0307(7) Uani 1 1 d . . . H9A H 0.1027 0.6231 -0.0411 0.037 Uiso 1 1 calc R . . C10 C 0.1570(3) 0.5280(3) 0.05131(14) 0.0270(6) Uani 1 1 d . . . H10A H 0.1129 0.4622 0.0434 0.032 Uiso 1 1 calc R . . C11 C 0.2256(3) 0.5274(3) 0.11385(13) 0.0228(6) Uani 1 1 d . . . C12 C 0.2260(3) 0.4253(3) 0.16999(14) 0.0255(6) Uani 1 1 d . . . H12A H 0.2120 0.4739 0.2139 0.031 Uiso 1 1 calc R . . C13 C 0.0969(4) 0.3718(3) 0.16389(16) 0.0351(7) Uani 1 1 d . . . H13A H 0.0001 0.4491 0.1539 0.053 Uiso 1 1 calc R . . H13B H 0.0874 0.3265 0.2066 0.053 Uiso 1 1 calc R . . H13C H 0.1206 0.3057 0.1273 0.053 Uiso 1 1 calc R . . C14 C 0.3777(4) 0.2999(3) 0.17425(16) 0.0347(7) Uani 1 1 d . . . H14A H 0.4616 0.3302 0.1833 0.052 Uiso 1 1 calc R . . H14B H 0.3963 0.2515 0.1313 0.052 Uiso 1 1 calc R . . H14C H 0.3721 0.2376 0.2110 0.052 Uiso 1 1 calc R . . C15 C 0.3790(3) 0.8139(3) 0.07656(13) 0.0261(6) Uani 1 1 d . . . H15A H 0.4360 0.7931 0.1206 0.031 Uiso 1 1 calc R . . C16 C 0.4972(4) 0.7878(3) 0.01904(14) 0.0326(7) Uani 1 1 d . . . H16A H 0.5665 0.6906 0.0201 0.049 Uiso 1 1 calc R . . H16B H 0.5565 0.8454 0.0251 0.049 Uiso 1 1 calc R . . H16C H 0.4437 0.8108 -0.0246 0.049 Uiso 1 1 calc R . . C17 C 0.2706(4) 0.9653(3) 0.07593(15) 0.0352(7) Uani 1 1 d . . . H17A H 0.2036 0.9830 0.1157 0.053 Uiso 1 1 calc R . . H17B H 0.2081 0.9867 0.0346 0.053 Uiso 1 1 calc R . . H17C H 0.3306 1.0234 0.0771 0.053 Uiso 1 1 calc R . . C18 C 0.2531(3) 0.6727(3) 0.39271(12) 0.0188(6) Uani 1 1 d . . . C19 C 0.1388(3) 0.6193(3) 0.40480(13) 0.0205(6) Uani 1 1 d . . . C20 C 0.0532(3) 0.6561(3) 0.46422(13) 0.0238(6) Uani 1 1 d . . . H20A H -0.0239 0.6210 0.4735 0.029 Uiso 1 1 calc R . . C21 C 0.0789(3) 0.7429(3) 0.50986(13) 0.0246(6) Uani 1 1 d . . . H21A H 0.0199 0.7663 0.5502 0.029 Uiso 1 1 calc R . . C22 C 0.1896(3) 0.7954(3) 0.49707(13) 0.0229(6) Uani 1 1 d . . . H22A H 0.2060 0.8547 0.5288 0.027 Uiso 1 1 calc R . . C23 C 0.2782(3) 0.7629(3) 0.43816(13) 0.0204(6) Uani 1 1 d . . . C24 C 0.3941(3) 0.8291(3) 0.42555(13) 0.0235(6) Uani 1 1 d . . . H24A H 0.4521 0.7896 0.3834 0.028 Uiso 1 1 calc R . . C25 C 0.5098(4) 0.7984(3) 0.48390(14) 0.0318(7) Uani 1 1 d . . . H25A H 0.5630 0.6986 0.4901 0.048 Uiso 1 1 calc R . . H25B H 0.4555 0.8375 0.5257 0.048 Uiso 1 1 calc R . . H25C H 0.5846 0.8396 0.4732 0.048 Uiso 1 1 calc R . . C26 C 0.3116(4) 0.9850(3) 0.41394(15) 0.0324(7) Uani 1 1 d . . . H26A H 0.2433 1.0029 0.3746 0.049 Uiso 1 1 calc R . . H26B H 0.3875 1.0261 0.4056 0.049 Uiso 1 1 calc R . . H26C H 0.2513 1.0256 0.4541 0.049 Uiso 1 1 calc R . . C27 C 0.1125(3) 0.5234(3) 0.35456(13) 0.0235(6) Uani 1 1 d . . . H27A H 0.1284 0.5554 0.3081 0.028 Uiso 1 1 calc R . . C28 C -0.0500(3) 0.5243(3) 0.35706(15) 0.0295(7) Uani 1 1 d . . . H28A H -0.1248 0.6190 0.3513 0.044 Uiso 1 1 calc R . . H28B H -0.0664 0.4864 0.4009 0.044 Uiso 1 1 calc R . . H28C H -0.0630 0.4681 0.3206 0.044 Uiso 1 1 calc R . . C29 C 0.2294(3) 0.3752(3) 0.36466(15) 0.0306(7) Uani 1 1 d . . . H29A H 0.3332 0.3728 0.3577 0.046 Uiso 1 1 calc R . . H29B H 0.2090 0.3156 0.3320 0.046 Uiso 1 1 calc R . . H29C H 0.2206 0.3425 0.4108 0.046 Uiso 1 1 calc R . . C30 C -0.1172(4) 1.0793(3) 0.16446(16) 0.0363(7) Uani 1 1 d . . . H30A H -0.0738 1.0333 0.1222 0.055 Uiso 1 1 calc R . . H30B H -0.0478 1.1184 0.1837 0.055 Uiso 1 1 calc R . . H30C H -0.2171 1.1532 0.1551 0.055 Uiso 1 1 calc R . . C31 C -0.1727(4) 0.7859(4) 0.14037(16) 0.0402(8) Uani 1 1 d . . . H31A H -0.0889 0.7532 0.1098 0.048 Uiso 1 1 calc R . . C32 C -0.1926(4) 0.7177(3) 0.19842(17) 0.0396(8) Uani 1 1 d . . . H32A H -0.1251 0.6293 0.2141 0.047 Uiso 1 1 calc R . . C33 C -0.3286(4) 0.8008(3) 0.22983(18) 0.0419(8) Uani 1 1 d . . . H33A H -0.3686 0.7797 0.2710 0.050 Uiso 1 1 calc R . . C34 C -0.3957(4) 0.9210(3) 0.18977(18) 0.0399(8) Uani 1 1 d . . . H34A H -0.4901 0.9950 0.1985 0.048 Uiso 1 1 calc R . . C35 C -0.2990(4) 0.9124(4) 0.13487(17) 0.0431(9) Uani 1 1 d . . . H35A H -0.3154 0.9801 0.0999 0.052 Uiso 1 1 calc R . . C36 C -0.3495(4) 1.0635(3) 0.32486(15) 0.0383(8) Uani 1 1 d . . . H36A H -0.4536 1.0763 0.3178 0.046 Uiso 1 1 calc R . . C37 C -0.2798(4) 1.1505(3) 0.30176(15) 0.0360(8) Uani 1 1 d . . . H37A H -0.3274 1.2324 0.2753 0.043 Uiso 1 1 calc R . . C38 C -0.1256(4) 1.0965(3) 0.32432(15) 0.0344(7) Uani 1 1 d . . . H38A H -0.0513 1.1353 0.3156 0.041 Uiso 1 1 calc R . . C39 C -0.1023(4) 0.9754(3) 0.36177(14) 0.0315(7) Uani 1 1 d . . . H39A H -0.0100 0.9187 0.3840 0.038 Uiso 1 1 calc R . . C40 C -0.2389(4) 0.9524(3) 0.36081(14) 0.0352(7) Uani 1 1 d . . . H40A H -0.2544 0.8758 0.3808 0.042 Uiso 1 1 calc R . .