# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1351 data_DHL-3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[{Zr(NMe2)2(m-Me3SiNC6H4NSiMe3)}2]' _chemical_formula_analytical ? _chemical_formula_sum 'C32 H68 N8 Si4 Zr2' _chemical_formula_weight 859.74 _chemical_melting_point ? _chemical_compound_source ? 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 14.234(2) _cell_length_b 17.771(4) _cell_length_c 18.860(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.55(2) _cell_angle_gamma 90.00 _cell_volume 4495.6(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_method ? _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 0.600 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ' Enraf-Nonius CAD4' _diffrn_measurement_method \w--2\q _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4123 _diffrn_reflns_av_R_equivalents 0.0167 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 24.97 _reflns_number_total 3963 _reflns_number_observed 3288 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+3.0789P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3963 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_obs 0.0306 _refine_ls_wR_factor_all 0.0774 _refine_ls_wR_factor_obs 0.0718 _refine_ls_goodness_of_fit_all 1.066 _refine_ls_goodness_of_fit_obs 1.091 _refine_ls_restrained_S_all 1.066 _refine_ls_restrained_S_obs 1.091 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zr Zr 0.19643(2) -0.096068(15) 0.185268(14) 0.02089(9) Uani 1 d . . Si1 Si 0.33930(5) -0.04669(4) 0.36003(4) 0.0243(2) Uani 1 d . . Si2 Si 0.00257(6) -0.20490(4) 0.43317(4) 0.0240(2) Uani 1 d . . N1 N 0.2211(2) -0.05047(12) 0.29217(12) 0.0208(5) Uani 1 d . . N2 N -0.0512(2) -0.12588(13) 0.38133(12) 0.0234(5) Uani 1 d . . N3 N 0.2599(2) -0.02971(14) 0.12663(13) 0.0291(5) Uani 1 d . . N4 N 0.2695(2) -0.19621(13) 0.19708(13) 0.0286(5) Uani 1 d . . C1 C 0.1420(2) -0.03018(15) 0.31918(14) 0.0203(6) Uani 1 d . . C2 C 0.0857(2) -0.08545(14) 0.33757(14) 0.0207(6) Uani 1 d . . H2 H 0.0998(2) -0.13668(14) 0.33076(14) 0.025 Uiso 1 calc R . C3 C 0.0087(2) -0.06889(14) 0.36582(14) 0.0196(5) Uani 1 d . . C4 C -0.0106(2) 0.0066(2) 0.3755(2) 0.0264(6) Uani 1 d . . H4 H -0.0609(2) 0.0198(2) 0.3961(2) 0.032 Uiso 1 calc R . C5 C 0.0435(2) 0.0625(2) 0.3553(2) 0.0315(7) Uani 1 d . . H5 H 0.0285(2) 0.1138(2) 0.3610(2) 0.038 Uiso 1 calc R . C6 C 0.1190(2) 0.0453(2) 0.3270(2) 0.0277(6) Uani 1 d . . H6 H 0.1549(2) 0.0844(2) 0.3131(2) 0.033 Uiso 1 calc R . C7 C 0.3756(2) 0.0513(2) 0.3922(2) 0.0409(8) Uani 1 d . . H7A H 0.3742(2) 0.0825(2) 0.3490(2) 0.061 Uiso 1 calc R . H7B H 0.4431(2) 0.0514(2) 0.4292(2) 0.061 Uiso 1 calc R . H7C H 0.3288(2) 0.0715(2) 0.4153(2) 0.061 Uiso 1 calc R . C8 C 0.4332(2) -0.0844(2) 0.3206(2) 0.0433(8) Uani 1 d . . H8A H 0.4324(2) -0.0544(2) 0.2768(2) 0.065 Uiso 1 calc R . H8B H 0.4171(2) -0.1369(2) 0.3052(2) 0.065 Uiso 1 calc R . H8C H 0.4996(2) -0.0820(2) 0.3589(2) 0.065 Uiso 1 calc R . C9 C 0.3425(2) -0.1047(2) 0.4424(2) 0.0365(7) Uani 1 d . . H9A H 0.3235(2) -0.1565(2) 0.4262(2) 0.055 Uiso 1 calc R . H9B H 0.2957(2) -0.0840(2) 0.4654(2) 0.055 Uiso 1 calc R . H9C H 0.4101(2) -0.1042(2) 0.4793(2) 0.055 Uiso 1 calc R . C10 C -0.0877(2) -0.2473(2) 0.4735(2) 0.0364(7) Uani 1 d . . H10A H -0.1071(2) -0.2097(2) 0.5040(2) 0.055 Uiso 1 calc R . H10B H -0.0566(2) -0.2904(2) 0.5051(2) 0.055 Uiso 1 calc R . H10C H -0.1469(2) -0.2642(2) 0.4326(2) 0.055 Uiso 1 calc R . C11 C 0.1153(2) -0.1748(2) 0.5123(2) 0.0396(8) Uani 1 d . . H11A H 0.1638(2) -0.1523(2) 0.4920(2) 0.059 Uiso 1 calc R . H11B H 0.1453(2) -0.2187(2) 0.5431(2) 0.059 Uiso 1 calc R . H11C H 0.0961(2) -0.1377(2) 0.5434(2) 0.059 Uiso 1 calc R . C12 C 0.0386(2) -0.2772(2) 0.3754(2) 0.0369(7) Uani 1 d . . H12A H 0.0862(2) -0.2554(2) 0.3538(2) 0.055 Uiso 1 calc R . H12B H -0.0209(2) -0.2941(2) 0.3347(2) 0.055 Uiso 1 calc R . H12C H 0.0693(2) -0.3202(2) 0.4072(2) 0.055 Uiso 1 calc R . C13 C 0.3163(2) 0.0396(2) 0.1480(2) 0.0388(8) Uani 1 d . . H13A H 0.3283(2) 0.0499(2) 0.2013(2) 0.058 Uiso 1 calc R . H13B H 0.2783(2) 0.0812(2) 0.1176(2) 0.058 Uiso 1 calc R . H13C H 0.3802(2) 0.0345(2) 0.1394(2) 0.058 Uiso 1 calc R . C14 C 0.2399(3) -0.0475(2) 0.0477(2) 0.0441(8) Uani 1 d . . H14A H 0.2018(3) -0.0945(2) 0.0352(2) 0.066 Uiso 1 calc R . H14B H 0.3032(3) -0.0535(2) 0.0382(2) 0.066 Uiso 1 calc R . H14C H 0.2014(3) -0.0066(2) 0.0164(2) 0.066 Uiso 1 calc R . C15 C 0.3432(2) -0.2227(2) 0.1655(2) 0.0434(8) Uani 1 d . . H15A H 0.3532(2) -0.1846(2) 0.1311(2) 0.065 Uiso 1 calc R . H15B H 0.3200(2) -0.2696(2) 0.1378(2) 0.065 Uiso 1 calc R . H15C H 0.4064(2) -0.2318(2) 0.2061(2) 0.065 Uiso 1 calc R . C16 C 0.2526(3) -0.2511(2) 0.2484(2) 0.0459(8) Uani 1 d . . H16A H 0.2025(3) -0.2318(2) 0.2689(2) 0.069 Uiso 1 calc R . H16B H 0.3151(3) -0.2604(2) 0.2897(2) 0.069 Uiso 1 calc R . H16C H 0.2287(3) -0.2982(2) 0.2214(2) 0.069 Uiso 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 Zr 0.01986(14) 0.02408(15) 0.02025(14) -0.00215(11) 0.00873(10) -0.00299(11) Si1 0.0196(4) 0.0289(4) 0.0233(4) -0.0013(3) 0.0058(3) -0.0031(3) Si2 0.0244(4) 0.0231(4) 0.0245(4) 0.0038(3) 0.0084(3) 0.0007(3) N1 0.0194(11) 0.0242(12) 0.0191(11) -0.0005(9) 0.0070(9) -0.0016(9) N2 0.0226(12) 0.0242(12) 0.0254(12) 0.0045(10) 0.0105(10) -0.0003(10) N3 0.0259(13) 0.0364(14) 0.0268(13) 0.0016(11) 0.0112(10) -0.0057(11) N4 0.0254(12) 0.0308(13) 0.0305(13) -0.0003(10) 0.0105(11) 0.0026(10) C1 0.0183(13) 0.0262(15) 0.0135(12) -0.0018(10) 0.0016(10) -0.0001(11) C2 0.0217(14) 0.0188(14) 0.0203(13) -0.0015(10) 0.0051(11) 0.0003(11) C3 0.0180(13) 0.0224(14) 0.0155(12) 0.0020(10) 0.0017(10) 0.0013(11) C4 0.0239(14) 0.0275(15) 0.0282(15) -0.0046(12) 0.0094(12) 0.0015(12) C5 0.033(2) 0.0198(14) 0.043(2) -0.0041(13) 0.0157(14) 0.0004(12) C6 0.030(2) 0.0218(15) 0.032(2) 0.0020(12) 0.0102(13) -0.0048(12) C7 0.035(2) 0.038(2) 0.040(2) -0.0038(15) -0.0006(14) -0.0125(15) C8 0.024(2) 0.065(2) 0.042(2) -0.008(2) 0.0115(14) -0.001(2) C9 0.035(2) 0.040(2) 0.030(2) 0.0084(14) 0.0035(13) 0.0035(14) C10 0.038(2) 0.034(2) 0.041(2) 0.0117(14) 0.0186(15) -0.0005(14) C11 0.035(2) 0.036(2) 0.039(2) 0.0074(14) 0.0005(14) -0.0019(14) C12 0.048(2) 0.026(2) 0.041(2) 0.0068(14) 0.020(2) 0.0064(14) C13 0.035(2) 0.039(2) 0.041(2) 0.0078(15) 0.0106(15) -0.0077(14) C14 0.053(2) 0.054(2) 0.032(2) 0.001(2) 0.023(2) -0.011(2) C15 0.032(2) 0.045(2) 0.055(2) -0.008(2) 0.018(2) 0.0062(15) C16 0.053(2) 0.036(2) 0.050(2) 0.003(2) 0.017(2) 0.001(2) _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 Zr N3 2.025(2) . ? Zr N4 2.036(2) . ? Zr N1 2.091(2) . ? Zr N2 2.097(2) 6_556 ? Zr C3 2.794(3) 6_556 ? Si1 N1 1.741(2) . ? Si1 C9 1.852(3) . ? Si1 C7 1.859(3) . ? Si1 C8 1.859(3) . ? Si2 N2 1.736(2) . ? Si2 C10 1.857(3) . ? Si2 C12 1.865(3) . ? Si2 C11 1.868(3) . ? N1 C1 1.429(3) . ? N2 C3 1.416(3) . ? N2 Zr 2.097(2) 6_556 ? N3 C13 1.452(4) . ? N3 C14 1.455(4) . ? N4 C15 1.448(4) . ? N4 C16 1.451(4) . ? C1 C2 1.383(4) . ? C1 C6 1.401(4) . ? C2 C3 1.401(4) . ? C3 C4 1.394(4) . ? C3 Zr 2.794(3) 6_556 ? C4 C5 1.387(4) . ? C5 C6 1.383(4) . ? 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 N3 Zr N4 105.29(10) . . ? N3 Zr N1 109.83(9) . . ? N4 Zr N1 108.56(9) . . ? N3 Zr N2 110.54(9) . 6_556 ? N4 Zr N2 102.14(9) . 6_556 ? N1 Zr N2 119.32(8) . 6_556 ? N3 Zr C3 108.48(9) . 6_556 ? N4 Zr C3 128.74(8) . 6_556 ? N1 Zr C3 94.86(8) . 6_556 ? N2 Zr C3 29.49(8) 6_556 6_556 ? N1 Si1 C9 110.00(13) . . ? N1 Si1 C7 111.78(13) . . ? C9 Si1 C7 108.7(2) . . ? N1 Si1 C8 109.80(13) . . ? C9 Si1 C8 108.4(2) . . ? C7 Si1 C8 108.0(2) . . ? N2 Si2 C10 108.91(12) . . ? N2 Si2 C12 112.58(13) . . ? C10 Si2 C12 108.82(14) . . ? N2 Si2 C11 108.52(13) . . ? C10 Si2 C11 108.43(15) . . ? C12 Si2 C11 109.5(2) . . ? C1 N1 Si1 114.3(2) . . ? C1 N1 Zr 122.9(2) . . ? Si1 N1 Zr 122.23(11) . . ? C3 N2 Si2 120.9(2) . . ? C3 N2 Zr 103.7(2) . 6_556 ? Si2 N2 Zr 134.60(12) . 6_556 ? C13 N3 C14 111.7(2) . . ? C13 N3 Zr 130.5(2) . . ? C14 N3 Zr 117.5(2) . . ? C15 N4 C16 111.2(3) . . ? C15 N4 Zr 130.8(2) . . ? C16 N4 Zr 117.9(2) . . ? C2 C1 C6 118.5(2) . . ? C2 C1 N1 120.1(2) . . ? C6 C1 N1 121.3(2) . . ? C1 C2 C3 122.6(2) . . ? C4 C3 C2 117.8(2) . . ? C4 C3 N2 120.1(2) . . ? C2 C3 N2 122.0(2) . . ? C4 C3 Zr 89.0(2) . 6_556 ? C2 C3 Zr 133.9(2) . 6_556 ? N2 C3 Zr 46.81(12) . 6_556 ? C5 C4 C3 120.0(3) . . ? C6 C5 C4 121.5(3) . . ? C5 C6 C1 119.5(3) . . ? _refine_diff_density_max 0.357 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.065 #===END data_DHL-4 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[{Zr(NMe2)2(p-Me3SiNC6H4NSiMe3)}2]' _chemical_formula_analytical ? _chemical_formula_sum 'C32 H68 N8 Si4 Zr2' _chemical_formula_weight 859.74 _chemical_melting_point ? _chemical_compound_source ? 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.005(4) _cell_length_b 10.128(8) _cell_length_c 13.168(9) _cell_angle_alpha 69.17(6) _cell_angle_beta 80.33(4) _cell_angle_gamma 78.63(5) _cell_volume 1094.1(12) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method ? _exptl_crystal_F_000 452 _exptl_absorpt_coefficient_mu 0.617 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ' Enraf-Nonius CAD4' _diffrn_measurement_method \w--2\q _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6379 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 30.00 _reflns_number_total 6379 _reflns_number_observed 5617 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+0.4093P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6378 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_obs 0.0312 _refine_ls_wR_factor_all 0.0820 _refine_ls_wR_factor_obs 0.0769 _refine_ls_goodness_of_fit_all 1.061 _refine_ls_goodness_of_fit_obs 1.072 _refine_ls_restrained_S_all 1.070 _refine_ls_restrained_S_obs 1.072 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zr Zr -0.25331(2) -0.12459(2) 0.257168(13) 0.01738(5) Uani 1 d . . Si1 Si 0.04638(6) 0.45699(5) -0.26416(4) 0.02229(10) Uani 1 d . . Si2 Si -0.51658(6) 0.18553(6) 0.14896(5) 0.02707(12) Uani 1 d . . N1 N -0.3554(2) 0.0606(2) 0.14528(13) 0.0219(3) Uani 1 d . . N2 N 0.0934(2) 0.2732(2) -0.20526(12) 0.0200(3) Uani 1 d . . N3 N -0.4236(2) -0.2247(2) 0.35696(13) 0.0261(3) Uani 1 d . . N4 N -0.1538(2) -0.0712(2) 0.36135(13) 0.0270(3) Uani 1 d . . C1 C -0.2411(2) 0.1104(2) 0.05707(14) 0.0198(3) Uani 1 d . . C2 C -0.1183(2) 0.1621(2) 0.0732(2) 0.0260(4) Uani 1 d . . H2 H -0.1103(2) 0.1634(2) 0.1438(2) 0.031 Uiso 1 calc R . C3 C -0.0070(2) 0.2117(2) -0.0115(2) 0.0265(4) Uani 1 d . . H3 H 0.0766(2) 0.2447(2) 0.0026(2) 0.032 Uiso 1 calc R . C4 C -0.0156(2) 0.2139(2) -0.11619(14) 0.0192(3) Uani 1 d . . C5 C -0.1371(2) 0.1591(2) -0.1320(2) 0.0258(4) Uani 1 d . . H5 H -0.1446(2) 0.1569(2) -0.2025(2) 0.031 Uiso 1 calc R . C6 C -0.2469(2) 0.1079(2) -0.0472(2) 0.0260(4) Uani 1 d . . H6 H -0.3277(2) 0.0704(2) -0.0603(2) 0.031 Uiso 1 calc R . C7 C -0.4690(3) 0.3413(3) 0.1743(3) 0.0473(6) Uani 1 d . . H7A H -0.3925(3) 0.3856(3) 0.1163(3) 0.071 Uiso 1 calc R . H7B H -0.4283(3) 0.3089(3) 0.2451(3) 0.071 Uiso 1 calc R . H7C H -0.5611(3) 0.4113(3) 0.1749(3) 0.071 Uiso 1 calc R . C8 C -0.5999(3) 0.2586(3) 0.0161(2) 0.0409(5) Uani 1 d . . H8A H -0.5239(3) 0.3035(3) -0.0421(2) 0.061 Uiso 1 calc R . H8B H -0.6895(3) 0.3299(3) 0.0205(2) 0.061 Uiso 1 calc R . H8C H -0.6299(3) 0.1809(3) 0.0000(2) 0.061 Uiso 1 calc R . C9 C -0.6613(3) 0.1008(3) 0.2586(2) 0.0522(7) Uani 1 d . . H9A H -0.6181(3) 0.0622(3) 0.3287(2) 0.078 Uiso 1 calc R . H9B H -0.6912(3) 0.0232(3) 0.2422(2) 0.078 Uiso 1 calc R . H9C H -0.7509(3) 0.1722(3) 0.2627(2) 0.078 Uiso 1 calc R . C10 C -0.1385(3) 0.5000(3) -0.3230(2) 0.0449(6) Uani 1 d . . H10A H -0.2181(3) 0.4609(3) -0.2655(2) 0.067 Uiso 1 calc R . H10B H -0.1290(3) 0.4578(3) -0.3807(2) 0.067 Uiso 1 calc R . H10C H -0.1658(3) 0.6039(3) -0.3539(2) 0.067 Uiso 1 calc R . C11 C 0.1964(3) 0.5311(3) -0.3733(2) 0.0444(6) Uani 1 d . . H11A H 0.2110(3) 0.4837(3) -0.4283(2) 0.067 Uiso 1 calc R . H11B H 0.2921(3) 0.5147(3) -0.3416(2) 0.067 Uiso 1 calc R . H11C H 0.1655(3) 0.6339(3) -0.4079(2) 0.067 Uiso 1 calc R . C12 C 0.0229(3) 0.5497(3) -0.1622(2) 0.0436(6) Uani 1 d . . H12A H -0.0561(3) 0.5123(3) -0.1035(2) 0.065 Uiso 1 calc R . H12B H -0.0071(3) 0.6525(3) -0.1978(2) 0.065 Uiso 1 calc R . H12C H 0.1195(3) 0.5333(3) -0.1315(2) 0.065 Uiso 1 calc R . C13 C -0.5247(3) -0.2722(3) 0.3073(2) 0.0426(6) Uani 1 d . . H13A H -0.4937(3) -0.2467(3) 0.2285(2) 0.064 Uiso 1 calc R . H13B H -0.6293(3) -0.2262(3) 0.3198(2) 0.064 Uiso 1 calc R . H13C H -0.5198(3) -0.3761(3) 0.3398(2) 0.064 Uiso 1 calc R . C14 C -0.4649(3) -0.2601(3) 0.4735(2) 0.0457(6) Uani 1 d . . H14A H -0.3943(3) -0.2264(3) 0.5046(2) 0.069 Uiso 1 calc R . H14B H -0.4594(3) -0.3639(3) 0.5075(2) 0.069 Uiso 1 calc R . H14C H -0.5689(3) -0.2139(3) 0.4874(2) 0.069 Uiso 1 calc R . C15 C -0.1987(5) 0.0583(4) 0.3859(3) 0.0857(15) Uani 1 d . . H15A H -0.2843(5) 0.1157(4) 0.3452(3) 0.129 Uiso 1 calc R . H15B H -0.1128(5) 0.1123(4) 0.3648(3) 0.129 Uiso 1 calc R . H15C H -0.2297(5) 0.0359(4) 0.4644(3) 0.129 Uiso 1 calc R . C16 C -0.0284(3) -0.1541(3) 0.4214(2) 0.0500(7) Uani 1 d . . H16A H 0.0031(3) -0.2434(3) 0.4052(2) 0.075 Uiso 1 calc R . H16B H -0.0598(3) -0.1758(3) 0.4999(2) 0.075 Uiso 1 calc R . H16C H 0.0571(3) -0.0997(3) 0.4003(2) 0.075 Uiso 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 Zr 0.01586(8) 0.01830(8) 0.01701(8) -0.00611(6) 0.00172(5) -0.00288(5) Si1 0.0210(2) 0.0208(2) 0.0245(2) -0.0089(2) 0.0002(2) -0.0018(2) Si2 0.0198(2) 0.0209(2) 0.0343(3) -0.0052(2) 0.0037(2) -0.0021(2) N1 0.0187(7) 0.0201(7) 0.0230(7) -0.0039(6) 0.0023(5) -0.0037(5) N2 0.0170(6) 0.0206(7) 0.0219(7) -0.0081(6) 0.0023(5) -0.0034(5) N3 0.0212(7) 0.0251(8) 0.0265(8) -0.0039(6) 0.0050(6) -0.0058(6) N4 0.0304(8) 0.0294(8) 0.0237(7) -0.0129(7) -0.0025(6) -0.0031(7) C1 0.0160(7) 0.0174(7) 0.0226(8) -0.0048(6) 0.0004(6) -0.0008(6) C2 0.0242(9) 0.0350(10) 0.0198(8) -0.0081(7) -0.0019(7) -0.0092(8) C3 0.0211(8) 0.0371(10) 0.0234(8) -0.0095(8) -0.0016(7) -0.0108(7) C4 0.0152(7) 0.0193(8) 0.0217(8) -0.0073(6) 0.0008(6) -0.0006(6) C5 0.0261(9) 0.0325(10) 0.0240(8) -0.0142(8) 0.0021(7) -0.0110(7) C6 0.0245(9) 0.0296(9) 0.0276(9) -0.0118(8) 0.0007(7) -0.0111(7) C7 0.0437(13) 0.0303(11) 0.070(2) -0.0242(12) -0.0037(12) 0.0010(10) C8 0.0282(11) 0.0351(12) 0.0534(14) -0.0065(10) -0.0132(10) 0.0011(9) C9 0.0344(12) 0.0358(13) 0.063(2) -0.0043(12) 0.0249(12) 0.0007(10) C10 0.0370(12) 0.0364(12) 0.064(2) -0.0181(12) -0.0229(12) 0.0071(10) C11 0.0386(12) 0.0282(11) 0.0454(13) 0.0031(10) 0.0108(10) 0.0007(9) C12 0.066(2) 0.0301(11) 0.0402(12) -0.0198(10) -0.0097(11) -0.0015(11) C13 0.0295(11) 0.0349(12) 0.061(2) -0.0082(11) -0.0094(10) -0.0094(9) C14 0.0445(13) 0.0468(14) 0.0325(11) -0.0067(10) 0.0181(10) -0.0078(11) C15 0.151(4) 0.059(2) 0.059(2) -0.045(2) -0.059(2) 0.046(2) C16 0.055(2) 0.060(2) 0.0413(13) -0.0294(13) -0.0225(12) 0.0140(13) _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 Zr N3 2.024(2) . ? Zr N4 2.027(2) . ? Zr N1 2.085(2) . ? Zr N2 2.086(2) 2 ? Zr C1 2.858(3) . ? Si1 N2 1.738(2) . ? Si1 C11 1.853(3) . ? Si1 C12 1.858(3) . ? Si1 C10 1.863(3) . ? Si2 N1 1.733(2) . ? Si2 C9 1.856(3) . ? Si2 C8 1.863(3) . ? Si2 C7 1.864(3) . ? N1 C1 1.432(2) . ? N2 C4 1.430(2) . ? N2 Zr 2.086(2) 2 ? N3 C13 1.444(3) . ? N3 C14 1.446(3) . ? N4 C15 1.427(3) . ? N4 C16 1.435(3) . ? C1 C2 1.388(3) . ? C1 C6 1.392(3) . ? C2 C3 1.387(3) . ? C3 C4 1.386(3) . ? C4 C5 1.395(3) . ? C5 C6 1.383(3) . ? 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 N3 Zr N4 102.11(9) . . ? N3 Zr N1 106.90(9) . . ? N4 Zr N1 109.34(9) . . ? N3 Zr N2 109.03(8) . 2 ? N4 Zr N2 106.63(8) . 2 ? N1 Zr N2 121.21(8) . 2 ? N3 Zr C1 134.04(7) . . ? N4 Zr C1 105.14(8) . . ? N1 Zr C1 28.58(6) . . ? N2 Zr C1 97.70(8) 2 . ? N2 Si1 C11 110.73(11) . . ? N2 Si1 C12 111.86(11) . . ? C11 Si1 C12 107.90(14) . . ? N2 Si1 C10 110.03(11) . . ? C11 Si1 C10 109.32(14) . . ? C12 Si1 C10 106.89(13) . . ? N1 Si2 C9 109.38(11) . . ? N1 Si2 C8 111.56(11) . . ? C9 Si2 C8 109.09(14) . . ? N1 Si2 C7 110.76(11) . . ? C9 Si2 C7 109.77(15) . . ? C8 Si2 C7 106.22(14) . . ? C1 N1 Si2 114.31(13) . . ? C1 N1 Zr 107.27(12) . . ? Si2 N1 Zr 135.83(10) . . ? C4 N2 Si1 112.13(13) . . ? C4 N2 Zr 115.31(12) . 2 ? Si1 N2 Zr 131.54(9) . 2 ? C13 N3 C14 111.5(2) . . ? C13 N3 Zr 117.1(2) . . ? C14 N3 Zr 131.4(2) . . ? C15 N4 C16 108.9(2) . . ? C15 N4 Zr 124.4(2) . . ? C16 N4 Zr 126.7(2) . . ? C2 C1 C6 117.3(2) . . ? C2 C1 N1 120.7(2) . . ? C6 C1 N1 122.0(2) . . ? C2 C1 Zr 97.84(13) . . ? C6 C1 Zr 126.86(14) . . ? N1 C1 Zr 44.15(9) . . ? C3 C2 C1 121.5(2) . . ? C4 C3 C2 121.1(2) . . ? C3 C4 C5 117.4(2) . . ? C3 C4 N2 121.4(2) . . ? C5 C4 N2 121.1(2) . . ? C6 C5 C4 121.3(2) . . ? C5 C6 C1 121.2(2) . . ? _refine_diff_density_max 0.619 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.076 #===END