data_1100798 _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_moiety 'C18 H36 N2 Si2 Zr1' _chemical_formula_sum 'C18 H36 N2 Si2 Zr' _chemical_formula_weight 427.89 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 11.3691(15) _cell_length_b 13.9028(9) _cell_length_c 15.137(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.131(12) _cell_angle_gamma 90.00 _cell_volume 2273.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 87 _cell_measurement_theta_min 3.315 _cell_measurement_theta_max 20.963 _exptl_crystal_description blocK _exptl_crystal_colour yellow _exptl_crystal_size_max 0.71 _exptl_crystal_size_mid 0.479 _exptl_crystal_size_min 0.433 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 0.591 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.826 _exptl_absorpt_correction_T_max 1.258 _exptl_absorpt_process_details ? _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 18635 _diffrn_reflns_av_R_equivalents 0.0799 _diffrn_reflns_av_sigmaI/netI 0.0622 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5211 _reflns_number_gt 3843 _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^)+(0.0355P)^2^+1.8463P] 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 5211 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1001 _refine_ls_wR_factor_gt 0.0886 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 C9 C 0.4473(4) 0.4577(3) 0.3492(3) 0.0549(10) Uani 1 1 d . . . H9A H 0.4490 0.4426 0.4129 0.082 Uiso 1 1 calc R . . H9B H 0.3612 0.4612 0.3089 0.082 Uiso 1 1 calc R . . H9C H 0.4880 0.5197 0.3486 0.082 Uiso 1 1 calc R . . Zr1 Zr 0.75090(2) 0.418728(19) 0.242124(17) 0.02164(9) Uani 1 1 d . . . Si1 Si 0.79033(9) 0.34443(6) 0.06332(6) 0.0327(2) Uani 1 1 d . . . Si2 Si 0.53047(8) 0.36155(7) 0.30600(6) 0.0335(2) Uani 1 1 d . . . N1 N 0.8785(2) 0.36275(18) 0.17851(16) 0.0274(5) Uani 1 1 d . . . N2 N 0.6906(2) 0.36530(18) 0.35132(16) 0.0269(5) Uani 1 1 d . . . C10 C 0.8101(3) 0.5766(2) 0.28131(19) 0.0279(6) Uani 1 1 d . . . H10A H 0.8392 0.6053 0.2328 0.042 Uiso 1 1 calc R . . H10B H 0.8768 0.5779 0.3407 0.042 Uiso 1 1 calc R . . H10C H 0.7391 0.6132 0.2870 0.042 Uiso 1 1 calc R . . C1 C 0.6402(3) 0.3816(2) 0.07908(19) 0.0316(7) Uani 1 1 d . . . C5 C 0.5855(3) 0.3281(2) 0.13688(19) 0.0291(7) Uani 1 1 d . . . H5 H 0.5881 0.2601 0.1427 0.035 Uiso 1 1 calc R . . C2 C 0.6116(3) 0.4795(2) 0.0906(2) 0.0344(7) Uani 1 1 d . . . H2 H 0.6353 0.5329 0.0607 0.041 Uiso 1 1 calc R . . C3 C 0.5431(3) 0.4848(2) 0.1531(2) 0.0343(7) Uani 1 1 d . . . H3 H 0.5124 0.5424 0.1716 0.041 Uiso 1 1 calc R . . C13 C 1.0736(3) 0.4178(3) 0.2901(3) 0.0508(10) Uani 1 1 d . . . H13A H 1.0350 0.4165 0.3396 0.076 Uiso 1 1 calc R . . H13B H 1.0623 0.4816 0.2610 0.076 Uiso 1 1 calc R . . H13C H 1.1622 0.4041 0.3164 0.076 Uiso 1 1 calc R . . C21 C 0.7648(3) 0.3408(2) 0.4479(2) 0.0349(7) Uani 1 1 d . . . C7 C 0.8225(4) 0.4275(3) -0.0239(2) 0.0526(10) Uani 1 1 d . . . H7A H 0.8259 0.4939 -0.0016 0.079 Uiso 1 1 calc R . . H7B H 0.7565 0.4215 -0.0834 0.079 Uiso 1 1 calc R . . H7C H 0.9020 0.4105 -0.0323 0.079 Uiso 1 1 calc R . . C6 C 0.7842(4) 0.2175(3) 0.0211(2) 0.0498(9) Uani 1 1 d . . . H6A H 0.8640 0.2003 0.0134 0.075 Uiso 1 1 calc R . . H6B H 0.7187 0.2114 -0.0386 0.075 Uiso 1 1 calc R . . H6C H 0.7666 0.1742 0.0666 0.075 Uiso 1 1 calc R . . C11 C 1.0133(3) 0.3420(2) 0.2170(2) 0.0369(8) Uani 1 1 d . . . C4 C 0.5263(3) 0.3909(2) 0.1847(2) 0.0320(7) Uani 1 1 d . . . C8 C 0.4550(3) 0.2436(3) 0.3109(3) 0.0537(10) Uani 1 1 d . . . H8A H 0.4583 0.2300 0.3752 0.081 Uiso 1 1 calc R . . H8B H 0.4985 0.1928 0.2887 0.081 Uiso 1 1 calc R . . H8C H 0.3685 0.2460 0.2714 0.081 Uiso 1 1 calc R . . C14 C 1.0311(3) 0.2420(3) 0.2614(3) 0.0513(10) Uani 1 1 d . . . H14A H 0.9914 0.2396 0.3102 0.077 Uiso 1 1 calc R . . H14B H 1.1198 0.2288 0.2885 0.077 Uiso 1 1 calc R . . H14C H 0.9937 0.1936 0.2139 0.077 Uiso 1 1 calc R . . C24 C 0.8968(4) 0.3753(4) 0.4632(3) 0.0714(14) Uani 1 1 d . . . H24A H 0.8967 0.4451 0.4537 0.107 Uiso 1 1 calc R . . H24B H 0.9309 0.3432 0.4189 0.107 Uiso 1 1 calc R . . H24C H 0.9478 0.3599 0.5267 0.107 Uiso 1 1 calc R . . C12 C 1.0766(4) 0.3457(4) 0.1419(3) 0.0649(12) Uani 1 1 d . . . H12A H 1.0397 0.2974 0.0941 0.097 Uiso 1 1 calc R . . H12B H 1.1651 0.3323 0.1697 0.097 Uiso 1 1 calc R . . H12C H 1.0658 0.4098 0.1135 0.097 Uiso 1 1 calc R . . C23 C 0.7672(4) 0.2336(3) 0.4634(3) 0.0649(13) Uani 1 1 d . . . H23A H 0.7995 0.2015 0.4181 0.097 Uiso 1 1 calc R . . H23B H 0.6831 0.2106 0.4557 0.097 Uiso 1 1 calc R . . H23C H 0.8206 0.2188 0.5264 0.097 Uiso 1 1 calc R . . C22 C 0.7150(5) 0.3915(4) 0.5185(3) 0.0805(16) Uani 1 1 d . . . H22A H 0.7134 0.4611 0.5080 0.121 Uiso 1 1 calc R . . H22B H 0.7687 0.3772 0.5816 0.121 Uiso 1 1 calc R . . H22C H 0.6309 0.3686 0.5113 0.121 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 C9 0.045(2) 0.057(3) 0.072(3) -0.005(2) 0.032(2) 0.0099(19) Zr1 0.01990(14) 0.02195(15) 0.01984(14) -0.00172(11) 0.00149(10) -0.00176(12) Si1 0.0417(5) 0.0336(5) 0.0224(4) -0.0015(3) 0.0091(4) -0.0005(4) Si2 0.0252(4) 0.0356(5) 0.0417(5) -0.0008(4) 0.0133(4) 0.0004(4) N1 0.0230(12) 0.0325(14) 0.0265(12) 0.0002(10) 0.0075(10) 0.0000(11) N2 0.0279(13) 0.0293(13) 0.0231(12) 0.0014(10) 0.0071(10) 0.0012(11) C10 0.0309(16) 0.0188(15) 0.0313(14) -0.0011(12) 0.0057(12) -0.0025(12) C1 0.0325(16) 0.0333(17) 0.0202(13) -0.0038(12) -0.0046(12) -0.0025(13) C5 0.0217(14) 0.0296(16) 0.0276(14) -0.0043(12) -0.0044(12) -0.0075(12) C2 0.0339(16) 0.0331(17) 0.0268(14) 0.0056(13) -0.0042(13) 0.0010(14) C3 0.0264(15) 0.0320(17) 0.0355(16) 0.0009(13) -0.0032(13) 0.0086(13) C13 0.0270(17) 0.055(2) 0.059(2) 0.0034(19) -0.0020(16) -0.0072(17) C21 0.0450(19) 0.0384(19) 0.0207(14) 0.0009(12) 0.0093(13) 0.0043(15) C7 0.068(3) 0.057(2) 0.0372(18) 0.0098(17) 0.0230(18) 0.001(2) C6 0.071(3) 0.043(2) 0.0369(18) -0.0088(16) 0.0189(18) -0.0030(19) C11 0.0296(16) 0.042(2) 0.0403(17) 0.0065(14) 0.0123(14) 0.0043(14) C4 0.0179(14) 0.0360(17) 0.0346(16) -0.0030(13) -0.0027(12) 0.0009(12) C8 0.039(2) 0.050(2) 0.074(3) -0.001(2) 0.0199(19) -0.0094(18) C14 0.041(2) 0.040(2) 0.065(2) 0.0063(18) 0.0052(18) 0.0084(17) C24 0.048(2) 0.101(4) 0.049(2) 0.027(2) -0.0082(19) -0.019(2) C12 0.038(2) 0.096(4) 0.069(3) 0.015(2) 0.028(2) 0.012(2) C23 0.081(3) 0.046(2) 0.049(2) 0.0138(18) -0.006(2) 0.003(2) C22 0.101(4) 0.105(4) 0.034(2) -0.006(2) 0.020(2) 0.035(3)