data_1100799 _publ_requested_journal 'Organometallics' _publ_section_title ; Crystal structure of compounds 6, 9 and 13 ; loop_ _publ_author_name 'Marta E. G. Mosquera' 'Maria Sudupe' _chemical_formula_sum 'C33 H49 N3 Si2 Zr' _chemical_formula_weight 635.15 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' 'N' 'N' 0.0061 0.0033 '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' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.119(2) _cell_length_b 19.430(4) _cell_length_c 15.805(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.355(11) _cell_angle_gamma 90.00 _cell_volume 3276.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 3.96 _cell_measurement_theta_max 17.209 _exptl_crystal_description prism _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.561 _exptl_crystal_size_mid 0.443 _exptl_crystal_size_min 0.108 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.288 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 0.434 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.794 _exptl_absorpt_correction_T_max 0.954 _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_number 27467 _diffrn_reflns_av_R_equivalents 0.1751 _diffrn_reflns_av_sigmaI/netI 0.1321 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.53 _reflns_number_total 7529 _reflns_number_gt 4388 _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^)+(0.0414P)^2^+5.5411P] 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 7529 _refine_ls_number_parameters 350 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1359 _refine_ls_R_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.1446 _refine_ls_wR_factor_gt 0.1210 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.000 _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 0.16570(4) 0.11245(2) 0.23597(3) 0.01799(12) Uani 1 1 d . . . C1 C 0.2279(5) 0.0594(2) 0.1091(3) 0.0248(11) Uani 1 1 d . . . C2 C 0.1012(5) 0.0810(3) 0.0764(3) 0.0279(11) Uani 1 1 d . . . H2 H 0.0328 0.0519 0.0556 0.034 Uiso 1 1 calc R . . C3 C 0.0951(5) 0.1535(3) 0.0803(3) 0.0240(10) Uani 1 1 d . . . H3 H 0.0223 0.1797 0.0622 0.029 Uiso 1 1 calc R . . C4 C 0.2186(5) 0.1803(2) 0.1164(3) 0.0230(10) Uani 1 1 d . . . C5 C 0.2979(5) 0.1214(3) 0.1314(3) 0.0253(11) Uani 1 1 d . . . H5 H 0.3847 0.1232 0.1532 0.030 Uiso 1 1 calc R . . Si1 Si 0.28551(13) -0.01848(7) 0.17817(9) 0.0267(3) Uani 1 1 d . . . N1 N 0.2559(4) 0.0136(2) 0.2723(2) 0.0240(9) Uani 1 1 d . . . C11 C 0.1969(6) -0.0980(3) 0.1282(4) 0.0401(14) Uani 1 1 d . . . H11A H 0.2289 -0.1370 0.1649 0.060 Uiso 1 1 calc R . . H11B H 0.2070 -0.1054 0.0705 0.060 Uiso 1 1 calc R . . H11C H 0.1096 -0.0922 0.1237 0.060 Uiso 1 1 calc R . . C12 C 0.4537(5) -0.0323(3) 0.1829(4) 0.0422(15) Uani 1 1 d . . . H12A H 0.4848 -0.0723 0.2180 0.063 Uiso 1 1 calc R . . H12B H 0.5019 0.0072 0.2088 0.063 Uiso 1 1 calc R . . H12C H 0.4607 -0.0391 0.1243 0.063 Uiso 1 1 calc R . . C13 C 0.2745(5) -0.0289(3) 0.3543(3) 0.0296(12) Uani 1 1 d . . . C14 C 0.1581(5) -0.0720(3) 0.3497(4) 0.0383(13) Uani 1 1 d . . . H14A H 0.1409 -0.1014 0.2989 0.057 Uiso 1 1 calc R . . H14B H 0.0879 -0.0421 0.3453 0.057 Uiso 1 1 calc R . . H14C H 0.1723 -0.0995 0.4020 0.057 Uiso 1 1 calc R . . C15 C 0.3029(6) 0.0182(3) 0.4354(3) 0.0407(14) Uani 1 1 d . . . H15A H 0.3761 0.0452 0.4379 0.061 Uiso 1 1 calc R . . H15B H 0.3176 -0.0093 0.4878 0.061 Uiso 1 1 calc R . . H15C H 0.2329 0.0482 0.4314 0.061 Uiso 1 1 calc R . . C16 C 0.3861(5) -0.0785(3) 0.3674(4) 0.0422(14) Uani 1 1 d . . . H16A H 0.4609 -0.0527 0.3706 0.063 Uiso 1 1 calc R . . H16B H 0.3704 -0.1099 0.3186 0.063 Uiso 1 1 calc R . . H16C H 0.3966 -0.1039 0.4211 0.063 Uiso 1 1 calc R . . Si2 Si 0.26229(13) 0.25520(7) 0.19222(9) 0.0240(3) Uani 1 1 d . . . N2 N 0.2358(4) 0.2134(2) 0.2827(2) 0.0224(9) Uani 1 1 d . . . C21 C 0.1616(5) 0.3317(3) 0.1502(3) 0.0369(13) Uani 1 1 d . . . H21A H 0.1868 0.3692 0.1909 0.055 Uiso 1 1 calc R . . H21B H 0.0756 0.3203 0.1443 0.055 Uiso 1 1 calc R . . H21C H 0.1707 0.3448 0.0937 0.055 Uiso 1 1 calc R . . C22 C 0.4266(5) 0.2800(3) 0.2007(4) 0.0393(14) Uani 1 1 d . . . H22A H 0.4502 0.3186 0.2397 0.059 Uiso 1 1 calc R . . H22B H 0.4334 0.2922 0.1433 0.059 Uiso 1 1 calc R . . H22C H 0.4813 0.2419 0.2233 0.059 Uiso 1 1 calc R . . C23 C 0.2395(5) 0.2498(2) 0.3666(3) 0.0250(11) Uani 1 1 d . . . C24 C 0.1099(5) 0.2803(3) 0.3601(4) 0.0348(13) Uani 1 1 d . . . H24A H 0.0869 0.3118 0.3114 0.052 Uiso 1 1 calc R . . H24B H 0.1126 0.3043 0.4137 0.052 Uiso 1 1 calc R . . H24C H 0.0492 0.2439 0.3511 0.052 Uiso 1 1 calc R . . C25 C 0.3357(5) 0.3094(3) 0.3856(4) 0.0371(13) Uani 1 1 d . . . H25A H 0.3147 0.3416 0.3376 0.056 Uiso 1 1 calc R . . H25B H 0.4181 0.2914 0.3919 0.056 Uiso 1 1 calc R . . H25C H 0.3339 0.3323 0.4391 0.056 Uiso 1 1 calc R . . C26 C 0.2767(6) 0.2002(3) 0.4437(3) 0.0422(15) Uani 1 1 d . . . H26A H 0.3579 0.1814 0.4477 0.063 Uiso 1 1 calc R . . H26B H 0.2164 0.1636 0.4349 0.063 Uiso 1 1 calc R . . H26C H 0.2792 0.2242 0.4972 0.063 Uiso 1 1 calc R . . N3 N -0.0325(3) 0.1080(2) 0.2283(2) 0.0220(8) Uani 1 1 d . . . C30 C 0.0205(5) 0.0982(2) 0.3108(3) 0.0268(11) Uani 1 1 d . . . C31 C -0.0474(6) 0.0769(4) 0.3775(4) 0.061(2) Uani 1 1 d . . . H31A H -0.0707 0.0289 0.3665 0.073 Uiso 1 1 calc R . . H31B H 0.0125 0.0792 0.4354 0.073 Uiso 1 1 calc R . . C32 C -0.1616(4) 0.1151(3) 0.3818(3) 0.0284(11) Uani 1 1 d D B . C33 C -0.1512(9) 0.1766(4) 0.4271(5) 0.073(3) Uani 1 1 d D . . H33 H -0.0689 0.1923 0.4459 0.088 Uiso 1 1 calc R A 1 C34 C -0.2224(15) 0.2144(7) 0.4479(9) 0.047(4) Uiso 0.511(18) 1 d PD B 1 H34 H -0.1978 0.2521 0.4850 0.057 Uiso 0.511(18) 1 calc PR B 1 C35 C -0.3460(19) 0.1957(10) 0.4106(11) 0.056(5) Uiso 0.511(18) 1 d PD B 1 H35 H -0.4083 0.2242 0.4196 0.068 Uiso 0.511(18) 1 calc PR B 1 C36 C -0.3816(15) 0.1376(11) 0.3613(10) 0.052(4) Uiso 0.511(18) 1 d PD B 1 H36 H -0.4660 0.1276 0.3367 0.063 Uiso 0.511(18) 1 calc PR B 1 C34' C -0.2932(19) 0.2087(8) 0.4202(10) 0.047(4) Uiso 0.489(18) 1 d P B 2 H34' H -0.3044 0.2520 0.4419 0.056 Uiso 0.489(18) 1 calc PR B 2 C35' C -0.3911(14) 0.1671(9) 0.3806(10) 0.043(4) Uiso 0.489(18) 1 d P B 2 H35' H -0.4701 0.1857 0.3746 0.052 Uiso 0.489(18) 1 calc PR B 2 C36' C -0.3905(11) 0.1003(8) 0.3475(8) 0.036(4) Uiso 0.489(18) 1 d P B 2 H36' H -0.4587 0.0708 0.3296 0.044 Uiso 0.489(18) 1 calc PR B 2 C37 C -0.2772(6) 0.0877(4) 0.3466(4) 0.060(2) Uani 1 1 d D . . H37 H -0.2928 0.0454 0.3180 0.072 Uiso 1 1 calc R B 1 C38 C -0.1591(4) 0.1046(3) 0.1727(3) 0.0255(11) Uani 1 1 d . . . C39 C -0.2299(5) 0.1651(3) 0.1521(3) 0.0267(11) Uani 1 1 d . . . C40 C -0.3494(5) 0.1600(3) 0.0939(3) 0.0330(12) Uani 1 1 d . . . H40 H -0.3982 0.1994 0.0796 0.040 Uiso 1 1 calc R . . C41 C -0.3970(5) 0.0986(3) 0.0572(4) 0.0395(14) Uani 1 1 d . . . H41 H -0.4777 0.0963 0.0191 0.047 Uiso 1 1 calc R . . C42 C -0.3240(5) 0.0398(3) 0.0772(4) 0.0375(13) Uani 1 1 d . . . H42 H -0.3555 -0.0016 0.0506 0.045 Uiso 1 1 calc R . . C43 C -0.2057(5) 0.0414(3) 0.1357(4) 0.0291(12) Uani 1 1 d . . . C44 C -0.1299(5) -0.0242(3) 0.1565(4) 0.0394(13) Uani 1 1 d . . . H44A H -0.0504 -0.0146 0.1981 0.059 Uiso 1 1 calc R . . H44B H -0.1168 -0.0424 0.1033 0.059 Uiso 1 1 calc R . . H44C H -0.1745 -0.0573 0.1813 0.059 Uiso 1 1 calc R . . C45 C -0.1787(5) 0.2334(3) 0.1903(4) 0.0386(13) Uani 1 1 d . . . H45A H -0.0956 0.2273 0.2289 0.058 Uiso 1 1 calc R . . H45B H -0.2317 0.2524 0.2230 0.058 Uiso 1 1 calc R . . H45C H -0.1758 0.2643 0.1435 0.058 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 Zr1 0.0230(2) 0.0147(2) 0.0170(2) -0.0002(2) 0.00688(15) -0.0007(2) C1 0.037(3) 0.017(2) 0.024(3) -0.003(2) 0.014(2) 0.001(2) C2 0.037(3) 0.029(3) 0.017(2) -0.004(2) 0.006(2) -0.005(2) C3 0.033(3) 0.022(3) 0.016(2) -0.003(2) 0.006(2) 0.002(2) C4 0.036(3) 0.021(3) 0.015(2) -0.0004(19) 0.011(2) 0.001(2) C5 0.031(3) 0.029(3) 0.019(2) -0.005(2) 0.0122(19) -0.005(2) Si1 0.0339(8) 0.0172(7) 0.0321(8) -0.0007(6) 0.0144(6) 0.0027(6) N1 0.032(2) 0.019(2) 0.022(2) 0.0010(17) 0.0084(17) 0.0031(17) C11 0.059(4) 0.022(3) 0.045(3) -0.005(2) 0.023(3) -0.004(3) C12 0.047(4) 0.040(4) 0.049(4) 0.005(3) 0.027(3) 0.009(3) C13 0.039(3) 0.026(3) 0.025(3) 0.009(2) 0.013(2) 0.008(2) C14 0.045(3) 0.035(3) 0.038(3) 0.008(3) 0.017(3) 0.002(3) C15 0.053(4) 0.037(3) 0.030(3) 0.009(3) 0.008(3) 0.007(3) C16 0.053(4) 0.027(3) 0.046(3) 0.009(3) 0.013(3) 0.014(3) Si2 0.0358(8) 0.0152(7) 0.0237(7) -0.0005(5) 0.0127(6) -0.0026(6) N2 0.028(2) 0.022(2) 0.0194(19) -0.0049(17) 0.0111(17) -0.0034(17) C21 0.057(4) 0.023(3) 0.034(3) 0.004(2) 0.018(3) 0.005(3) C22 0.044(3) 0.036(3) 0.043(3) -0.005(3) 0.020(3) -0.016(3) C23 0.036(3) 0.022(3) 0.017(2) -0.009(2) 0.009(2) -0.004(2) C24 0.041(3) 0.033(3) 0.036(3) -0.016(3) 0.020(2) -0.004(2) C25 0.043(3) 0.031(3) 0.036(3) -0.016(3) 0.009(3) -0.005(2) C26 0.070(4) 0.036(3) 0.021(3) -0.001(2) 0.013(3) 0.004(3) N3 0.028(2) 0.017(2) 0.0227(19) 0.0012(18) 0.0103(16) -0.0007(17) C30 0.031(3) 0.022(3) 0.029(3) 0.006(2) 0.011(2) 0.004(2) C31 0.051(4) 0.095(6) 0.050(4) 0.039(4) 0.034(3) 0.028(4) C32 0.028(3) 0.037(3) 0.023(2) 0.008(3) 0.0119(19) 0.004(2) C33 0.138(7) 0.043(4) 0.069(5) -0.009(4) 0.078(5) -0.024(5) C37 0.057(4) 0.095(6) 0.034(3) -0.004(4) 0.021(3) -0.023(4) C38 0.026(2) 0.027(3) 0.026(2) 0.008(2) 0.0109(19) 0.000(2) C39 0.031(3) 0.026(3) 0.025(3) 0.001(2) 0.012(2) 0.002(2) C40 0.030(3) 0.037(3) 0.034(3) 0.003(3) 0.012(2) 0.010(2) C41 0.024(3) 0.048(4) 0.042(3) 0.002(3) 0.001(2) -0.007(2) C42 0.033(3) 0.037(3) 0.038(3) -0.003(3) 0.004(2) -0.011(2) C43 0.027(3) 0.022(3) 0.041(3) 0.005(2) 0.013(2) -0.006(2) C44 0.040(3) 0.026(3) 0.053(4) 0.002(3) 0.012(3) -0.002(2) C45 0.048(3) 0.027(3) 0.038(3) 0.000(2) 0.007(3) 0.012(3)