Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Vincenzo Passarelli' 'Franco Benetollo' 'Giovanni Carta' 'Gilberto Rossetto' 'Pierino Zanella' _publ_contact_author_name 'Dr Vincenzo Passarelli' _publ_contact_author_address ; CNR - ICIS Corso Stati Uniti 4 Padova 35127 ITALY ; _publ_contact_author_email PASSAREL@SERVER1.DCCI.UNIPI.IT _publ_section_title ; Synthesis and characterisation of novel zirconium(IV) derivatives containing the bis-amido ligand SiMe2(NRR')2 ; #=========================================================================== data_zr-n2 _database_code_CSD 200050 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Zr[(N^i^Pr)~2~SiMe~2~]~2~ _chemical_formula_sum 'C32 H80 N8 Si4 Zr2' _chemical_formula_weight 871.84 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/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 10.033(3) _cell_length_b 46.986(5) _cell_length_c 10.498(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.12(3) _cell_angle_gamma 90.00 _cell_volume 4647(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 0.581 _exptl_absorpt_correction_type '\Y scan' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Philips PW1100' _diffrn_measurement_method \Q/2\Q _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7761 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 55 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 24.98 _reflns_number_total 7168 _reflns_number_gt 6971 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0000P)^2^+37.9809P] 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 7168 _refine_ls_number_parameters 439 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0828 _refine_ls_R_factor_gt 0.0794 _refine_ls_wR_factor_ref 0.1796 _refine_ls_wR_factor_gt 0.1771 _refine_ls_goodness_of_fit_ref 1.268 _refine_ls_restrained_S_all 1.268 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.003 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 0.04712(7) 0.158603(16) 0.56758(7) 0.0332(2) Uani 1 1 d . . . Zr2 Zr 0.12817(8) 0.091902(16) 0.73878(7) 0.0353(2) Uani 1 1 d . . . Si1 Si 0.1475(2) 0.15981(5) 0.8694(2) 0.0420(5) Uani 1 1 d . . . Si2 Si -0.1622(2) 0.09800(5) 0.5279(2) 0.0413(5) Uani 1 1 d . . . Si3 Si 0.0550(3) 0.20715(5) 0.4114(2) 0.0433(5) Uani 1 1 d . . . Si4 Si 0.2844(3) 0.04163(5) 0.8322(3) 0.0488(6) Uani 1 1 d . . . N1 N -0.0054(7) 0.16904(14) 0.7365(6) 0.0397(15) Uani 1 1 d . . . N2 N -0.0113(6) 0.11341(13) 0.5050(6) 0.0330(13) Uani 1 1 d . . . N3 N 0.2181(6) 0.13667(14) 0.7766(6) 0.0379(15) Uani 1 1 d . . . N4 N -0.0897(7) 0.08768(16) 0.6945(7) 0.0479(17) Uani 1 1 d . . . N5 N -0.0843(7) 0.18699(14) 0.4295(6) 0.0432(16) Uani 1 1 d . . . N6 N 0.1876(7) 0.18460(15) 0.5143(7) 0.0439(16) Uani 1 1 d . . . N7 N 0.2146(7) 0.06739(15) 0.9126(6) 0.0445(16) Uani 1 1 d . . . N8 N 0.2267(7) 0.05912(15) 0.6748(7) 0.0431(16) Uani 1 1 d . . . C1 C 0.2663(11) 0.1907(2) 0.9403(10) 0.068(3) Uani 1 1 d . . . H1A H 0.2913 0.1996 0.8695 0.081 Uiso 1 1 calc R . . H1B H 0.3508 0.1842 1.0101 0.081 Uiso 1 1 calc R . . H1C H 0.2181 0.2041 0.9780 0.081 Uiso 1 1 calc R . . C2 C 0.1170(12) 0.1418(2) 1.0147(9) 0.066(3) Uani 1 1 d . . . H2A H 0.0704 0.1547 1.0567 0.079 Uiso 1 1 calc R . . H2B H 0.2065 0.1361 1.0798 0.079 Uiso 1 1 calc R . . H2C H 0.0585 0.1254 0.9828 0.079 Uiso 1 1 calc R . . C3 C -0.1259(10) 0.1863(2) 0.7455(10) 0.055(2) Uani 1 1 d . . . H3 H -0.1946 0.1879 0.6532 0.066 Uiso 1 1 calc R . . C4 C -0.0814(14) 0.2163(3) 0.7942(13) 0.089(4) Uani 1 1 d . . . H4A H -0.0218 0.2159 0.8879 0.107 Uiso 1 1 calc R . . H4B H -0.1642 0.2276 0.7843 0.107 Uiso 1 1 calc R . . H4C H -0.0301 0.2245 0.7411 0.107 Uiso 1 1 calc R . . C5 C -0.2022(13) 0.1726(3) 0.8305(13) 0.088(4) Uani 1 1 d . . . H5A H -0.2300 0.1536 0.7982 0.106 Uiso 1 1 calc R . . H5B H -0.2851 0.1835 0.8240 0.106 Uiso 1 1 calc R . . H5C H -0.1402 0.1718 0.9233 0.106 Uiso 1 1 calc R . . C6 C 0.0094(9) 0.1052(2) 0.3729(8) 0.049(2) Uani 1 1 d . . . H6 H 0.0057 0.0844 0.3653 0.059 Uiso 1 1 calc R . . C7 C -0.1100(12) 0.1178(2) 0.2484(9) 0.073(3) Uani 1 1 d . . . H7A H -0.1074 0.1382 0.2539 0.088 Uiso 1 1 calc R . . H7B H -0.2006 0.1111 0.2480 0.088 Uiso 1 1 calc R . . H7C H -0.0958 0.1119 0.1665 0.088 Uiso 1 1 calc R . . C8 C 0.1505(10) 0.1151(2) 0.3693(9) 0.055(2) Uani 1 1 d . . . H8A H 0.1544 0.1355 0.3730 0.066 Uiso 1 1 calc R . . H8B H 0.1621 0.1087 0.2869 0.066 Uiso 1 1 calc R . . H8C H 0.2251 0.1074 0.4457 0.066 Uiso 1 1 calc R . . C9 C -0.3125(10) 0.1238(2) 0.4990(11) 0.062(3) Uani 1 1 d . . . H9A H -0.3919 0.1142 0.5111 0.074 Uiso 1 1 calc R . . H9B H -0.3398 0.1312 0.4084 0.074 Uiso 1 1 calc R . . H9C H -0.2827 0.1392 0.5628 0.074 Uiso 1 1 calc R . . C10 C -0.2366(11) 0.0668(2) 0.4129(11) 0.072(3) Uani 1 1 d . . . H10A H -0.1609 0.0541 0.4150 0.086 Uiso 1 1 calc R . . H10B H -0.2830 0.0734 0.3219 0.086 Uiso 1 1 calc R . . H10C H -0.3039 0.0569 0.4433 0.086 Uiso 1 1 calc R . . C11 C 0.3774(8) 0.1385(2) 0.8120(9) 0.050(2) Uani 1 1 d . . . H11 H 0.4010 0.1585 0.8047 0.060 Uiso 1 1 calc R . . C12 C 0.4290(9) 0.1217(2) 0.7140(10) 0.059(2) Uani 1 1 d . . . H12A H 0.4033 0.1020 0.7154 0.071 Uiso 1 1 calc R . . H12B H 0.5303 0.1233 0.7408 0.071 Uiso 1 1 calc R . . H12C H 0.3858 0.1291 0.6239 0.071 Uiso 1 1 calc R . . C13 C 0.4603(10) 0.1288(3) 0.9569(10) 0.073(3) Uani 1 1 d . . . H13A H 0.4217 0.1378 1.0186 0.088 Uiso 1 1 calc R . . H13B H 0.5582 0.1341 0.9799 0.088 Uiso 1 1 calc R . . H13C H 0.4531 0.1086 0.9630 0.088 Uiso 1 1 calc R . . C14 C -0.1853(12) 0.0726(2) 0.7552(11) 0.066(3) Uani 1 1 d . . . H14 H -0.2813 0.0767 0.6926 0.079 Uiso 1 1 calc R . . C15 C -0.1813(13) 0.0854(3) 0.8852(12) 0.082(4) Uani 1 1 d . . . H15A H -0.0894 0.0824 0.9525 0.098 Uiso 1 1 calc R . . H15B H -0.2525 0.0767 0.9143 0.098 Uiso 1 1 calc R . . H15C H -0.1996 0.1055 0.8732 0.098 Uiso 1 1 calc R . . C16 C -0.1735(12) 0.0412(2) 0.7526(13) 0.076(3) Uani 1 1 d . . . H16A H -0.1953 0.0349 0.6607 0.091 Uiso 1 1 calc R . . H16B H -0.2391 0.0328 0.7901 0.091 Uiso 1 1 calc R . . H16C H -0.0786 0.0355 0.8054 0.091 Uiso 1 1 calc R . . C17 C 0.0439(14) 0.2099(3) 0.2298(10) 0.086(4) Uani 1 1 d . . . H17A H 0.0478 0.1912 0.1945 0.103 Uiso 1 1 calc R . . H17B H 0.1221 0.2210 0.2244 0.103 Uiso 1 1 calc R . . H17C H -0.0438 0.2189 0.1775 0.103 Uiso 1 1 calc R . . C18 C 0.0689(11) 0.2447(2) 0.4759(11) 0.066(3) Uani 1 1 d . . . H18A H -0.0134 0.2553 0.4228 0.079 Uiso 1 1 calc R . . H18B H 0.1525 0.2535 0.4688 0.079 Uiso 1 1 calc R . . H18C H 0.0747 0.2446 0.5691 0.079 Uiso 1 1 calc R . . C19 C -0.3004(14) 0.1870(3) 0.2206(13) 0.112(5) Uani 1 1 d . . . H19A H -0.2488 0.1971 0.1731 0.134 Uiso 1 1 calc R . . H19B H -0.3982 0.1928 0.1867 0.134 Uiso 1 1 calc R . . H19C H -0.2940 0.1669 0.2069 0.134 Uiso 1 1 calc R . . C20 C -0.2376(9) 0.1937(2) 0.3710(11) 0.064(3) Uani 1 1 d . . . H20 H -0.2863 0.1816 0.4172 0.077 Uiso 1 1 calc R . . C21 C -0.2734(11) 0.2243(2) 0.3923(13) 0.079(3) Uani 1 1 d . . . H21A H -0.2320 0.2291 0.4866 0.095 Uiso 1 1 calc R . . H21B H -0.3746 0.2265 0.3637 0.095 Uiso 1 1 calc R . . H21C H -0.2363 0.2367 0.3399 0.095 Uiso 1 1 calc R . . C22 C 0.3411(10) 0.1882(2) 0.5384(11) 0.066(3) Uani 1 1 d . . . H22 H 0.3893 0.1733 0.6030 0.079 Uiso 1 1 calc R . . C23 C 0.4019(13) 0.2156(3) 0.6040(16) 0.107(5) Uani 1 1 d . . . H23A H 0.3729 0.2307 0.5386 0.128 Uiso 1 1 calc R . . H23B H 0.5036 0.2143 0.6380 0.128 Uiso 1 1 calc R . . H23C H 0.3685 0.2194 0.6776 0.128 Uiso 1 1 calc R . . C24 C 0.3792(14) 0.1828(4) 0.4120(16) 0.125(6) Uani 1 1 d . . . H24A H 0.3412 0.1648 0.3732 0.150 Uiso 1 1 calc R . . H24B H 0.4806 0.1827 0.4360 0.150 Uiso 1 1 calc R . . H24C H 0.3398 0.1977 0.3471 0.150 Uiso 1 1 calc R . . C25 C 0.2125(11) 0.0049(2) 0.8275(11) 0.068(3) Uani 1 1 d . . . H25A H 0.2450 -0.0029 0.9174 0.081 Uiso 1 1 calc R . . H25B H 0.2448 -0.0067 0.7690 0.081 Uiso 1 1 calc R . . H25C H 0.1106 0.0056 0.7938 0.081 Uiso 1 1 calc R . . C26 C 0.4817(10) 0.0383(3) 0.9112(12) 0.085(4) Uani 1 1 d . . . H26A H 0.5247 0.0566 0.9116 0.102 Uiso 1 1 calc R . . H26B H 0.5160 0.0251 0.8598 0.102 Uiso 1 1 calc R . . H26C H 0.5057 0.0316 1.0027 0.102 Uiso 1 1 calc R . . C27 C 0.2220(11) 0.0661(2) 1.0583(9) 0.063(3) Uani 1 1 d . . . H27 H 0.1604 0.0813 1.0703 0.075 Uiso 1 1 calc R . . C28 C 0.3684(12) 0.0719(3) 1.1577(10) 0.100(5) Uani 1 1 d . . . H28A H 0.4303 0.0565 1.1561 0.119 Uiso 1 1 calc R . . H28B H 0.3641 0.0737 1.2473 0.119 Uiso 1 1 calc R . . H28C H 0.4040 0.0893 1.1332 0.119 Uiso 1 1 calc R . . C29 C 0.1671(16) 0.0387(3) 1.0954(12) 0.110(5) Uani 1 1 d . . . H29A H 0.0695 0.0362 1.0395 0.132 Uiso 1 1 calc R . . H29B H 0.1745 0.0393 1.1890 0.132 Uiso 1 1 calc R . . H29C H 0.2222 0.0231 1.0814 0.132 Uiso 1 1 calc R . . C30 C 0.2426(10) 0.0481(2) 0.5476(10) 0.057(2) Uani 1 1 d . . . H30 H 0.2144 0.0636 0.4810 0.068 Uiso 1 1 calc R . . C31 C 0.1442(14) 0.0235(3) 0.4889(12) 0.091(4) Uani 1 1 d . . . H31A H 0.1719 0.0075 0.5488 0.109 Uiso 1 1 calc R . . H31B H 0.1494 0.0186 0.4020 0.109 Uiso 1 1 calc R . . H31C H 0.0487 0.0289 0.4785 0.109 Uiso 1 1 calc R . . C32 C 0.3933(14) 0.0407(3) 0.5647(15) 0.110(5) Uani 1 1 d . . . H32A H 0.4550 0.0558 0.6120 0.132 Uiso 1 1 calc R . . H32B H 0.4019 0.0381 0.4771 0.132 Uiso 1 1 calc R . . H32C H 0.4195 0.0234 0.6158 0.132 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 0.0321(4) 0.0354(4) 0.0326(4) 0.0014(3) 0.0117(3) -0.0004(3) Zr2 0.0342(4) 0.0366(4) 0.0342(4) 0.0029(3) 0.0105(3) -0.0009(3) Si1 0.0497(13) 0.0410(13) 0.0348(11) -0.0057(9) 0.0139(10) -0.0051(10) Si2 0.0336(11) 0.0425(13) 0.0459(12) -0.0043(10) 0.0113(9) -0.0016(9) Si3 0.0547(14) 0.0371(13) 0.0415(12) 0.0045(10) 0.0210(10) 0.0036(10) Si4 0.0432(13) 0.0421(14) 0.0585(15) 0.0128(11) 0.0143(11) 0.0068(10) N1 0.036(3) 0.046(4) 0.043(4) 0.007(3) 0.021(3) 0.005(3) N2 0.038(3) 0.028(3) 0.034(3) -0.007(3) 0.014(3) 0.000(3) N3 0.028(3) 0.047(4) 0.037(3) 0.000(3) 0.010(3) -0.007(3) N4 0.040(4) 0.062(5) 0.045(4) 0.008(3) 0.018(3) -0.006(3) N5 0.045(4) 0.041(4) 0.039(4) -0.001(3) 0.007(3) 0.004(3) N6 0.035(3) 0.047(4) 0.054(4) 0.008(3) 0.021(3) 0.002(3) N7 0.049(4) 0.043(4) 0.036(3) 0.008(3) 0.007(3) 0.001(3) N8 0.040(4) 0.041(4) 0.049(4) 0.003(3) 0.017(3) 0.005(3) C1 0.071(7) 0.053(6) 0.067(6) -0.017(5) 0.008(5) -0.012(5) C2 0.091(8) 0.075(7) 0.041(5) -0.009(5) 0.035(5) -0.001(6) C3 0.055(5) 0.058(6) 0.058(5) 0.004(4) 0.027(4) 0.010(4) C4 0.103(9) 0.073(8) 0.100(9) -0.023(7) 0.045(8) 0.018(7) C5 0.076(8) 0.095(10) 0.112(10) 0.008(8) 0.057(7) 0.009(7) C6 0.056(5) 0.060(6) 0.031(4) -0.007(4) 0.015(4) 0.004(4) C7 0.098(8) 0.069(7) 0.045(5) -0.004(5) 0.013(5) 0.015(6) C8 0.076(6) 0.048(6) 0.055(5) 0.000(4) 0.040(5) -0.002(5) C9 0.048(5) 0.062(7) 0.079(7) 0.004(5) 0.027(5) 0.009(5) C10 0.061(6) 0.079(8) 0.071(7) -0.019(6) 0.015(5) -0.018(5) C11 0.031(4) 0.064(6) 0.051(5) 0.003(4) 0.009(4) -0.009(4) C12 0.042(5) 0.064(7) 0.077(7) -0.004(5) 0.027(5) -0.007(4) C13 0.048(6) 0.083(8) 0.067(7) 0.013(6) -0.006(5) -0.002(5) C14 0.073(7) 0.059(6) 0.088(7) 0.003(5) 0.057(6) -0.013(5) C15 0.089(8) 0.093(9) 0.092(8) -0.001(7) 0.067(7) -0.015(7) C16 0.072(7) 0.054(7) 0.109(9) 0.016(6) 0.040(7) -0.008(5) C17 0.119(10) 0.092(9) 0.058(6) 0.025(6) 0.045(7) 0.021(8) C18 0.072(7) 0.048(6) 0.076(7) -0.008(5) 0.024(5) -0.001(5) C19 0.088(9) 0.091(10) 0.102(10) -0.006(8) -0.039(8) 0.019(7) C20 0.035(5) 0.066(7) 0.076(7) 0.020(5) -0.001(4) 0.007(4) C21 0.055(6) 0.072(8) 0.110(9) 0.014(7) 0.029(6) 0.017(5) C22 0.044(5) 0.073(7) 0.084(7) 0.019(6) 0.028(5) -0.008(5) C23 0.065(8) 0.093(10) 0.154(13) -0.017(9) 0.029(8) -0.034(7) C24 0.085(10) 0.173(17) 0.158(14) -0.002(12) 0.092(10) -0.012(10) C25 0.068(6) 0.057(7) 0.076(7) 0.010(5) 0.022(5) -0.003(5) C26 0.047(6) 0.110(10) 0.096(9) 0.038(8) 0.021(6) 0.016(6) C27 0.071(6) 0.077(7) 0.037(5) 0.016(5) 0.016(4) 0.005(5) C28 0.072(8) 0.164(15) 0.044(6) 0.012(7) -0.003(5) -0.019(8) C29 0.130(12) 0.136(13) 0.066(8) 0.034(8) 0.036(8) -0.041(10) C30 0.063(6) 0.055(6) 0.058(6) -0.004(4) 0.028(5) 0.003(5) C31 0.116(10) 0.084(9) 0.075(8) -0.021(7) 0.036(7) -0.026(8) C32 0.095(10) 0.137(14) 0.117(11) -0.031(10) 0.060(9) 0.023(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 N1 2.075(6) . ? Zr1 N5 2.075(7) . ? Zr1 N6 2.082(6) . ? Zr1 N2 2.240(6) . ? Zr1 N3 2.496(6) . ? Zr1 Si3 2.826(2) . ? Zr1 Si1 2.977(2) . ? Zr1 Zr2 3.5648(11) . ? Zr2 N8 2.064(7) . ? Zr2 N7 2.078(6) . ? Zr2 N4 2.082(7) . ? Zr2 N3 2.269(6) . ? Zr2 N2 2.577(6) . ? Zr2 Si4 2.818(3) . ? Zr2 Si2 3.006(3) . ? Si1 N1 1.737(7) . ? Si1 N3 1.763(7) . ? Si1 C2 1.859(9) . ? Si1 C1 1.862(9) . ? Si2 N4 1.717(7) . ? Si2 N2 1.768(6) . ? Si2 C9 1.876(9) . ? Si2 C10 1.884(10) . ? Si3 N5 1.751(7) . ? Si3 N6 1.752(7) . ? Si3 C17 1.876(10) . ? Si3 C18 1.880(10) . ? Si4 N7 1.753(8) . ? Si4 N8 1.756(7) . ? Si4 C25 1.863(10) . ? Si4 C26 1.872(10) . ? N1 C3 1.485(10) . ? N2 C6 1.521(9) . ? N3 C11 1.514(9) . ? N4 C14 1.498(10) . ? N5 C20 1.481(10) . ? N6 C22 1.482(11) . ? N7 C27 1.508(10) . ? N8 C30 1.490(11) . ? C3 C5 1.506(13) . ? C3 C4 1.515(15) . ? C6 C8 1.502(12) . ? C6 C7 1.556(12) . ? C11 C12 1.522(12) . ? C11 C13 1.530(12) . ? C14 C15 1.479(14) . ? C14 C16 1.483(14) . ? C19 C20 1.518(16) . ? C20 C21 1.517(14) . ? C22 C23 1.487(16) . ? C22 C24 1.523(16) . ? C27 C29 1.502(15) . ? C27 C28 1.505(14) . ? C30 C32 1.502(14) . ? C30 C31 1.507(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zr1 N5 99.1(3) . . ? N1 Zr1 N6 119.0(3) . . ? N5 Zr1 N6 76.2(3) . . ? N1 Zr1 N2 110.9(2) . . ? N5 Zr1 N2 111.4(2) . . ? N6 Zr1 N2 127.6(2) . . ? N1 Zr1 N3 69.3(2) . . ? N5 Zr1 N3 163.6(2) . . ? N6 Zr1 N3 98.9(2) . . ? N2 Zr1 N3 84.1(2) . . ? N1 Zr1 Si3 111.77(19) . . ? N5 Zr1 Si3 38.1(2) . . ? N6 Zr1 Si3 38.17(19) . . ? N2 Zr1 Si3 130.67(16) . . ? N3 Zr1 Si3 134.07(15) . . ? N1 Zr1 Si1 34.74(18) . . ? N5 Zr1 Si1 129.24(19) . . ? N6 Zr1 Si1 105.2(2) . . ? N2 Zr1 Si1 106.78(16) . . ? N3 Zr1 Si1 36.24(16) . . ? Si3 Zr1 Si1 122.36(7) . . ? N1 Zr1 Zr2 81.83(18) . . ? N5 Zr1 Zr2 153.83(19) . . ? N6 Zr1 Zr2 126.40(18) . . ? N2 Zr1 Zr2 46.03(15) . . ? N3 Zr1 Zr2 39.21(15) . . ? Si3 Zr1 Zr2 162.77(6) . . ? Si1 Zr1 Zr2 62.95(5) . . ? N8 Zr2 N7 76.7(3) . . ? N8 Zr2 N4 116.1(3) . . ? N7 Zr2 N4 103.4(3) . . ? N8 Zr2 N3 122.9(2) . . ? N7 Zr2 N3 109.8(2) . . ? N4 Zr2 N3 116.8(3) . . ? N8 Zr2 N2 98.4(2) . . ? N7 Zr2 N2 168.4(2) . . ? N4 Zr2 N2 68.9(2) . . ? N3 Zr2 N2 81.7(2) . . ? N8 Zr2 Si4 38.39(19) . . ? N7 Zr2 Si4 38.3(2) . . ? N4 Zr2 Si4 114.4(2) . . ? N3 Zr2 Si4 125.18(17) . . ? N2 Zr2 Si4 135.64(14) . . ? N8 Zr2 Si2 106.44(19) . . ? N7 Zr2 Si2 134.9(2) . . ? N4 Zr2 Si2 33.63(19) . . ? N3 Zr2 Si2 105.47(16) . . ? N2 Zr2 Si2 35.91(14) . . ? Si4 Zr2 Si2 128.20(8) . . ? N8 Zr2 Zr1 122.94(19) . . ? N7 Zr2 Zr1 152.1(2) . . ? N4 Zr2 Zr1 86.1(2) . . ? N3 Zr2 Zr1 44.06(15) . . ? N2 Zr2 Zr1 38.74(13) . . ? Si4 Zr2 Zr1 156.28(6) . . ? Si2 Zr2 Zr1 63.23(5) . . ? N1 Si1 N3 97.0(3) . . ? N1 Si1 C2 115.1(4) . . ? N3 Si1 C2 112.6(4) . . ? N1 Si1 C1 113.2(4) . . ? N3 Si1 C1 112.2(4) . . ? C2 Si1 C1 106.8(5) . . ? N1 Si1 Zr1 42.9(2) . . ? N3 Si1 Zr1 56.8(2) . . ? C2 Si1 Zr1 140.7(3) . . ? C1 Si1 Zr1 112.1(4) . . ? N4 Si2 N2 99.9(3) . . ? N4 Si2 C9 112.5(4) . . ? N2 Si2 C9 113.1(4) . . ? N4 Si2 C10 111.6(5) . . ? N2 Si2 C10 113.6(4) . . ? C9 Si2 C10 106.3(5) . . ? N4 Si2 Zr2 42.2(2) . . ? N2 Si2 Zr2 58.7(2) . . ? C9 Si2 Zr2 134.6(3) . . ? C10 Si2 Zr2 117.9(4) . . ? N5 Si3 N6 94.1(3) . . ? N5 Si3 C17 112.1(5) . . ? N6 Si3 C17 115.8(5) . . ? N5 Si3 C18 115.6(4) . . ? N6 Si3 C18 113.6(4) . . ? C17 Si3 C18 105.8(5) . . ? N5 Si3 Zr1 47.0(2) . . ? N6 Si3 Zr1 47.3(2) . . ? C17 Si3 Zr1 129.9(4) . . ? C18 Si3 Zr1 124.3(3) . . ? N7 Si4 N8 94.2(3) . . ? N7 Si4 C25 115.9(4) . . ? N8 Si4 C25 114.1(4) . . ? N7 Si4 C26 112.4(5) . . ? N8 Si4 C26 114.3(4) . . ? C25 Si4 C26 106.0(5) . . ? N7 Si4 Zr2 47.3(2) . . ? N8 Si4 Zr2 46.9(2) . . ? C25 Si4 Zr2 127.1(3) . . ? C26 Si4 Zr2 126.9(4) . . ? C3 N1 Si1 126.8(6) . . ? C3 N1 Zr1 129.4(5) . . ? Si1 N1 Zr1 102.3(3) . . ? C6 N2 Si2 114.3(5) . . ? C6 N2 Zr1 113.8(5) . . ? Si2 N2 Zr1 119.9(3) . . ? C6 N2 Zr2 124.7(5) . . ? Si2 N2 Zr2 85.4(2) . . ? Zr1 N2 Zr2 95.2(2) . . ? C11 N3 Si1 114.9(5) . . ? C11 N3 Zr2 114.7(5) . . ? Si1 N3 Zr2 117.2(3) . . ? C11 N3 Zr1 122.7(5) . . ? Si1 N3 Zr1 86.9(3) . . ? Zr2 N3 Zr1 96.7(2) . . ? C14 N4 Si2 117.2(6) . . ? C14 N4 Zr2 136.6(6) . . ? Si2 N4 Zr2 104.2(3) . . ? C20 N5 Si3 126.5(6) . . ? C20 N5 Zr1 138.2(6) . . ? Si3 N5 Zr1 94.9(3) . . ? C22 N6 Si3 124.1(6) . . ? C22 N6 Zr1 141.3(6) . . ? Si3 N6 Zr1 94.6(3) . . ? C27 N7 Si4 124.9(6) . . ? C27 N7 Zr2 140.7(6) . . ? Si4 N7 Zr2 94.3(3) . . ? C30 N8 Si4 125.3(6) . . ? C30 N8 Zr2 139.6(6) . . ? Si4 N8 Zr2 94.7(3) . . ? N1 C3 C5 113.2(8) . . ? N1 C3 C4 112.2(8) . . ? C5 C3 C4 110.5(9) . . ? C8 C6 N2 111.7(7) . . ? C8 C6 C7 108.7(8) . . ? N2 C6 C7 111.2(7) . . ? N3 C11 C12 112.4(7) . . ? N3 C11 C13 113.2(7) . . ? C12 C11 C13 108.8(8) . . ? C15 C14 C16 116.4(10) . . ? C15 C14 N4 112.5(8) . . ? C16 C14 N4 113.3(8) . . ? N5 C20 C21 113.9(8) . . ? N5 C20 C19 112.8(9) . . ? C21 C20 C19 108.3(9) . . ? N6 C22 C23 114.5(9) . . ? N6 C22 C24 112.9(9) . . ? C23 C22 C24 111.1(10) . . ? C29 C27 N7 113.8(9) . . ? C29 C27 C28 109.5(10) . . ? N7 C27 C28 113.1(8) . . ? N8 C30 C32 112.8(9) . . ? N8 C30 C31 112.1(8) . . ? C32 C30 C31 111.2(10) . . ? _diffrn_measured_fraction_theta_max 0.879 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.879 _refine_diff_density_max 0.674 _refine_diff_density_min -0.756 _refine_diff_density_rms 0.117