# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email rory.waterman@uvm.edu _publ_contact_author_name 'Rory Waterman' loop_ _publ_author_name 'Annalese Maddox' 'Joseph Tanski' 'Rory Waterman' data_rw1285zr _database_code_depnum_ccdc_archive 'CCDC 840651' #TrackingRef '- RW1285Zr.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H63 N7 Si3 Zr' _chemical_formula_sum 'C26 H63 N7 Si3 Zr' _chemical_formula_weight 649.32 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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3406(5) _cell_length_b 10.3645(5) _cell_length_c 17.2962(8) _cell_angle_alpha 88.5340(10) _cell_angle_beta 87.1460(10) _cell_angle_gamma 77.7520(10) _cell_volume 1809.07(15) _cell_formula_units_Z 2 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9738 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 31.58 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.192 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 0.428 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8822 _exptl_absorpt_correction_T_max 0.9192 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30146 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 31.95 _reflns_number_total 11517 _reflns_number_gt 9995 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0383P)^2^+0.9517P] 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 11517 _refine_ls_number_parameters 353 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0844 _refine_ls_wR_factor_gt 0.0804 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.002 _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 Zr Zr 0.802829(13) 0.816231(13) 0.750832(8) 0.01438(4) Uani 1 1 d . . . Si1 Si 0.74531(4) 1.03501(5) 0.90569(3) 0.02242(9) Uani 1 1 d . . . Si2 Si 0.75035(5) 0.71088(4) 0.56423(2) 0.02251(9) Uani 1 1 d . . . Si3 Si 1.19324(5) 0.42008(4) 0.75521(3) 0.02661(10) Uani 1 1 d . . . N1 N 0.69454(13) 0.93084(13) 0.84325(8) 0.0218(3) Uani 1 1 d . . . N2 N 0.71705(13) 0.72234(14) 0.66406(8) 0.0227(3) Uani 1 1 d . . . N3 N 0.91051(13) 0.65726(14) 0.82447(9) 0.0273(3) Uani 1 1 d . . . N4 N 0.65293(13) 0.68221(13) 0.81720(8) 0.0206(2) Uani 1 1 d . . . N5 N 0.83898(13) 0.97871(12) 0.68581(7) 0.0199(2) Uani 1 1 d D . . H5 H 0.9183(15) 0.983(2) 0.6739(11) 0.024 Uiso 1 1 d D . . N6 N 1.04053(12) 0.75068(12) 0.74750(7) 0.0175(2) Uani 1 1 d . . . N7 N 1.14325(13) 0.55270(12) 0.81869(8) 0.0212(2) Uani 1 1 d . . . C1 C 0.56924(17) 0.89727(18) 0.87314(11) 0.0313(4) Uani 1 1 d . . . H1A H 0.5002 0.9238 0.8348 0.038 Uiso 1 1 calc R . . H1B H 0.5384 0.9453 0.9216 0.038 Uiso 1 1 calc R . . C2 C 0.61449(19) 0.6446(2) 0.68304(10) 0.0324(4) Uani 1 1 d . . . H2A H 0.6555 0.5493 0.6815 0.039 Uiso 1 1 calc R . . H2B H 0.5461 0.6634 0.6439 0.039 Uiso 1 1 calc R . . C3 C 0.86275(18) 0.55376(18) 0.86733(11) 0.0314(4) Uani 1 1 d . . . H3A H 0.8521 0.5739 0.9232 0.038 Uiso 1 1 calc R . . H3B H 0.9259 0.4681 0.8605 0.038 Uiso 1 1 calc R . . C4 C 0.59227(18) 0.75025(18) 0.88838(10) 0.0299(4) Uani 1 1 d . . . H4A H 0.6519 0.7253 0.9318 0.036 Uiso 1 1 calc R . . H4B H 0.5072 0.7245 0.9025 0.036 Uiso 1 1 calc R . . C5 C 0.55071(17) 0.6780(2) 0.76182(10) 0.0302(4) Uani 1 1 d . . . H5B H 0.4885 0.7648 0.7597 0.036 Uiso 1 1 calc R . . H5C H 0.4998 0.6107 0.7789 0.036 Uiso 1 1 calc R . . C6 C 0.72961(17) 0.54799(17) 0.83510(11) 0.0289(3) Uani 1 1 d . . . H6A H 0.7444 0.4949 0.7874 0.035 Uiso 1 1 calc R . . H6B H 0.6783 0.5041 0.8735 0.035 Uiso 1 1 calc R . . C7 C 0.7578(2) 0.9587(2) 1.00606(11) 0.0434(5) Uani 1 1 d . . . H7A H 0.8259 0.8769 1.0052 0.065 Uiso 1 1 calc R . . H7B H 0.6723 0.9390 1.0233 0.065 Uiso 1 1 calc R . . H7C H 0.7819 1.0207 1.0418 0.065 Uiso 1 1 calc R . . C8 C 0.91279(18) 1.0635(2) 0.87794(12) 0.0392(5) Uani 1 1 d . . . H8A H 0.9120 1.1043 0.8262 0.059 Uiso 1 1 calc R . . H8B H 0.9769 0.9790 0.8776 0.059 Uiso 1 1 calc R . . H8C H 0.9380 1.1222 0.9154 0.059 Uiso 1 1 calc R . . C9 C 0.62175(19) 1.19591(18) 0.91371(12) 0.0346(4) Uani 1 1 d . . . H9A H 0.6153 1.2411 0.8631 0.052 Uiso 1 1 calc R . . H9B H 0.6505 1.2516 0.9515 0.052 Uiso 1 1 calc R . . H9C H 0.5349 1.1790 0.9307 0.052 Uiso 1 1 calc R . . C10 C 0.6117(2) 0.8133(2) 0.50946(12) 0.0402(5) Uani 1 1 d . . . H10A H 0.5995 0.9060 0.5240 0.060 Uiso 1 1 calc R . . H10B H 0.5299 0.7823 0.5220 0.060 Uiso 1 1 calc R . . H10C H 0.6333 0.8051 0.4537 0.060 Uiso 1 1 calc R . . C11 C 0.7637(2) 0.53561(19) 0.53289(11) 0.0367(4) Uani 1 1 d . . . H11A H 0.8278 0.4760 0.5642 0.055 Uiso 1 1 calc R . . H11B H 0.7933 0.5276 0.4782 0.055 Uiso 1 1 calc R . . H11C H 0.6769 0.5120 0.5399 0.055 Uiso 1 1 calc R . . C12 C 0.90904(19) 0.7566(2) 0.53144(10) 0.0336(4) Uani 1 1 d . . . H12A H 0.9150 0.8398 0.5552 0.050 Uiso 1 1 calc R . . H12B H 0.9122 0.7671 0.4750 0.050 Uiso 1 1 calc R . . H12C H 0.9834 0.6868 0.5469 0.050 Uiso 1 1 calc R . . C13 C 0.75354(18) 1.09882(16) 0.65431(9) 0.0265(3) Uani 1 1 d . . . C14 C 0.7819(2) 1.1124(2) 0.56677(11) 0.0395(5) Uani 1 1 d . . . H14A H 0.7595 1.0382 0.5402 0.059 Uiso 1 1 calc R . . H14B H 0.8761 1.1122 0.5567 0.059 Uiso 1 1 calc R . . H14C H 0.7284 1.1955 0.5475 0.059 Uiso 1 1 calc R . . C15 C 0.60847(19) 1.09053(19) 0.66968(11) 0.0356(4) Uani 1 1 d . . . H15A H 0.5927 1.0102 0.6465 0.053 Uiso 1 1 calc R . . H15B H 0.5510 1.1680 0.6467 0.053 Uiso 1 1 calc R . . H15C H 0.5888 1.0880 0.7256 0.053 Uiso 1 1 calc R . . C16 C 0.7788(3) 1.22202(18) 0.69323(13) 0.0449(5) Uani 1 1 d . . . H16A H 0.7543 1.2188 0.7486 0.067 Uiso 1 1 calc R . . H16B H 0.7253 1.3012 0.6696 0.067 Uiso 1 1 calc R . . H16C H 0.8728 1.2247 0.6864 0.067 Uiso 1 1 calc R . . C17 C 1.03434(14) 0.65200(14) 0.79691(9) 0.0197(3) Uani 1 1 d . . . C18 C 1.17031(16) 0.53609(19) 0.90261(10) 0.0291(4) Uani 1 1 d . . . H18A H 1.1235 0.4685 0.9261 0.035 Uiso 1 1 calc R . . C19 C 1.1224(2) 0.6687(2) 0.94561(11) 0.0389(4) Uani 1 1 d . . . H19A H 1.0261 0.6970 0.9429 0.058 Uiso 1 1 calc R . . H19B H 1.1652 0.7361 0.9211 0.058 Uiso 1 1 calc R . . H19C H 1.1458 0.6567 0.9999 0.058 Uiso 1 1 calc R . . C20 C 1.31831(18) 0.4916(2) 0.91313(11) 0.0348(4) Uani 1 1 d . . . H20A H 1.3511 0.4068 0.8876 0.052 Uiso 1 1 calc R . . H20B H 1.3349 0.4814 0.9685 0.052 Uiso 1 1 calc R . . H20C H 1.3643 0.5577 0.8901 0.052 Uiso 1 1 calc R . . C21 C 1.2033(3) 0.2597(2) 0.80893(15) 0.0517(6) Uani 1 1 d . . . H21A H 1.2800 0.2439 0.8417 0.078 Uiso 1 1 calc R . . H21B H 1.2130 0.1880 0.7719 0.078 Uiso 1 1 calc R . . H21C H 1.1223 0.2633 0.8414 0.078 Uiso 1 1 calc R . . C22 C 1.0637(2) 0.4353(2) 0.68254(12) 0.0388(4) Uani 1 1 d . . . H22A H 1.0562 0.5197 0.6544 0.058 Uiso 1 1 calc R . . H22B H 0.9785 0.4317 0.7090 0.058 Uiso 1 1 calc R . . H22C H 1.0882 0.3626 0.6459 0.058 Uiso 1 1 calc R . . C23 C 1.35583(19) 0.4205(2) 0.70474(13) 0.0394(4) Uani 1 1 d . . . H23A H 1.3523 0.5054 0.6778 0.059 Uiso 1 1 calc R . . H23B H 1.3761 0.3491 0.6671 0.059 Uiso 1 1 calc R . . H23C H 1.4249 0.4071 0.7427 0.059 Uiso 1 1 calc R . . C24 C 1.16982(14) 0.77904(15) 0.72233(9) 0.0193(3) Uani 1 1 d . . . H24A H 1.2404 0.7075 0.7435 0.023 Uiso 1 1 calc R . . C25 C 1.18996(18) 0.7805(2) 0.63437(10) 0.0306(4) Uani 1 1 d . . . H25A H 1.1804 0.6957 0.6141 0.046 Uiso 1 1 calc R . . H25B H 1.2788 0.7948 0.6202 0.046 Uiso 1 1 calc R . . H25C H 1.1236 0.8519 0.6123 0.046 Uiso 1 1 calc R . . C26 C 1.18692(17) 0.91050(17) 0.75419(11) 0.0288(3) Uani 1 1 d . . . H26A H 1.1820 0.9065 0.8109 0.043 Uiso 1 1 calc R . . H26B H 1.1164 0.9819 0.7360 0.043 Uiso 1 1 calc R . . H26C H 1.2733 0.9273 0.7361 0.043 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 Zr 0.01377(6) 0.01401(6) 0.01508(6) -0.00154(4) -0.00036(4) -0.00222(4) Si1 0.01930(19) 0.0257(2) 0.0213(2) -0.00854(16) -0.00026(15) -0.00156(16) Si2 0.0269(2) 0.0224(2) 0.01754(19) -0.00420(15) -0.00451(16) -0.00232(16) Si3 0.0292(2) 0.0182(2) 0.0324(2) -0.00536(17) -0.00154(18) -0.00414(17) N1 0.0219(6) 0.0229(6) 0.0217(6) -0.0061(5) 0.0050(5) -0.0077(5) N2 0.0243(6) 0.0260(7) 0.0199(6) -0.0041(5) -0.0014(5) -0.0096(5) N3 0.0197(6) 0.0258(7) 0.0358(8) 0.0117(6) 0.0002(5) -0.0051(5) N4 0.0188(6) 0.0216(6) 0.0224(6) -0.0035(5) 0.0024(5) -0.0069(5) N5 0.0206(6) 0.0172(6) 0.0208(6) 0.0019(4) 0.0000(5) -0.0023(5) N6 0.0149(5) 0.0178(5) 0.0195(6) 0.0014(4) 0.0004(4) -0.0032(4) N7 0.0205(6) 0.0168(6) 0.0244(6) 0.0015(5) -0.0025(5) 0.0004(5) C1 0.0249(8) 0.0322(9) 0.0374(9) -0.0125(7) 0.0106(7) -0.0087(7) C2 0.0352(9) 0.0389(10) 0.0287(8) -0.0061(7) -0.0036(7) -0.0198(8) C3 0.0273(8) 0.0299(9) 0.0368(9) 0.0131(7) 0.0000(7) -0.0076(7) C4 0.0293(8) 0.0341(9) 0.0285(8) -0.0068(7) 0.0109(6) -0.0140(7) C5 0.0236(8) 0.0413(10) 0.0301(8) -0.0007(7) -0.0034(6) -0.0159(7) C6 0.0263(8) 0.0237(8) 0.0375(9) 0.0056(7) 0.0029(7) -0.0089(6) C7 0.0372(10) 0.0640(14) 0.0229(8) -0.0062(9) -0.0022(7) 0.0041(10) C8 0.0256(8) 0.0568(13) 0.0384(10) -0.0219(9) 0.0025(7) -0.0139(8) C9 0.0339(9) 0.0256(8) 0.0420(10) -0.0106(7) 0.0065(8) -0.0018(7) C10 0.0436(11) 0.0401(11) 0.0351(10) 0.0002(8) -0.0184(8) -0.0009(9) C11 0.0494(11) 0.0295(9) 0.0311(9) -0.0112(7) -0.0039(8) -0.0064(8) C12 0.0356(9) 0.0403(10) 0.0250(8) -0.0092(7) 0.0039(7) -0.0084(8) C13 0.0380(9) 0.0169(7) 0.0222(7) 0.0032(5) -0.0026(6) -0.0004(6) C14 0.0576(13) 0.0315(9) 0.0249(8) 0.0098(7) -0.0007(8) -0.0011(9) C15 0.0324(9) 0.0336(9) 0.0336(9) 0.0025(7) -0.0066(7) 0.0101(7) C16 0.0730(16) 0.0169(8) 0.0438(11) -0.0001(7) -0.0055(10) -0.0069(9) C17 0.0183(6) 0.0164(6) 0.0236(7) 0.0011(5) -0.0015(5) -0.0023(5) C18 0.0222(7) 0.0391(9) 0.0254(8) 0.0144(7) -0.0054(6) -0.0061(7) C19 0.0518(12) 0.0349(10) 0.0263(9) -0.0050(7) -0.0103(8) 0.0013(9) C20 0.0291(9) 0.0426(10) 0.0302(9) 0.0055(8) -0.0109(7) -0.0009(7) C21 0.0715(16) 0.0203(9) 0.0635(15) 0.0012(9) -0.0046(12) -0.0098(9) C22 0.0416(11) 0.0429(11) 0.0352(10) -0.0143(8) -0.0042(8) -0.0144(9) C23 0.0322(9) 0.0348(10) 0.0483(11) -0.0176(9) 0.0045(8) -0.0002(8) C24 0.0162(6) 0.0195(7) 0.0220(7) -0.0002(5) 0.0016(5) -0.0040(5) C25 0.0280(8) 0.0414(10) 0.0237(8) -0.0006(7) 0.0058(6) -0.0116(7) C26 0.0222(7) 0.0261(8) 0.0393(9) -0.0061(7) 0.0015(7) -0.0078(6) _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 N5 2.0902(13) . ? Zr N2 2.1353(13) . ? Zr N1 2.1388(13) . ? Zr N3 2.1982(14) . ? Zr N6 2.4054(12) . ? Zr N4 2.5109(13) . ? Zr C17 2.7668(15) . ? Si1 N1 1.7218(14) . ? Si1 C8 1.8557(19) . ? Si1 C9 1.8770(18) . ? Si1 C7 1.888(2) . ? Si2 N2 1.7459(14) . ? Si2 C12 1.8606(19) . ? Si2 C10 1.8755(19) . ? Si2 C11 1.8840(18) . ? Si3 N7 1.7554(14) . ? Si3 C23 1.856(2) . ? Si3 C22 1.862(2) . ? Si3 C21 1.869(2) . ? N1 C1 1.477(2) . ? N2 C2 1.482(2) . ? N3 C17 1.3345(19) . ? N3 C3 1.446(2) . ? N4 C5 1.469(2) . ? N4 C4 1.479(2) . ? N4 C6 1.481(2) . ? N5 C13 1.474(2) . ? N5 H5 0.846(14) . ? N6 C17 1.3260(18) . ? N6 C24 1.4716(18) . ? N7 C17 1.4142(19) . ? N7 C18 1.491(2) . ? C1 C4 1.510(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C5 1.500(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C6 1.524(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5B 0.9900 . ? C5 H5C 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.531(3) . ? C13 C16 1.534(3) . ? C13 C14 1.537(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C18 C20 1.521(2) . ? C18 C19 1.554(3) . ? C18 H18A 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.525(2) . ? C24 C26 1.530(2) . ? C24 H24A 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? 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 N5 Zr N2 98.91(5) . . ? N5 Zr N1 95.06(5) . . ? N2 Zr N1 125.10(5) . . ? N5 Zr N3 138.86(5) . . ? N2 Zr N3 106.38(6) . . ? N1 Zr N3 96.19(6) . . ? N5 Zr N6 83.81(5) . . ? N2 Zr N6 112.51(5) . . ? N1 Zr N6 121.67(5) . . ? N3 Zr N6 56.79(5) . . ? N5 Zr N4 152.99(5) . . ? N2 Zr N4 71.79(5) . . ? N1 Zr N4 72.10(5) . . ? N3 Zr N4 67.52(5) . . ? N6 Zr N4 123.19(4) . . ? N5 Zr C17 112.18(5) . . ? N2 Zr C17 109.85(5) . . ? N1 Zr C17 113.08(5) . . ? N3 Zr C17 28.34(5) . . ? N6 Zr C17 28.63(4) . . ? N4 Zr C17 94.79(4) . . ? N1 Si1 C8 112.34(7) . . ? N1 Si1 C9 110.99(8) . . ? C8 Si1 C9 110.71(10) . . ? N1 Si1 C7 109.96(9) . . ? C8 Si1 C7 105.82(10) . . ? C9 Si1 C7 106.75(9) . . ? N2 Si2 C12 113.81(7) . . ? N2 Si2 C10 111.36(9) . . ? C12 Si2 C10 109.25(10) . . ? N2 Si2 C11 109.98(8) . . ? C12 Si2 C11 106.11(9) . . ? C10 Si2 C11 105.89(9) . . ? N7 Si3 C23 112.53(8) . . ? N7 Si3 C22 107.07(8) . . ? C23 Si3 C22 109.44(10) . . ? N7 Si3 C21 110.28(9) . . ? C23 Si3 C21 108.92(11) . . ? C22 Si3 C21 108.52(11) . . ? C1 N1 Si1 110.35(10) . . ? C1 N1 Zr 118.13(10) . . ? Si1 N1 Zr 129.76(7) . . ? C2 N2 Si2 106.56(10) . . ? C2 N2 Zr 122.28(10) . . ? Si2 N2 Zr 131.10(7) . . ? C17 N3 C3 126.27(14) . . ? C17 N3 Zr 100.24(10) . . ? C3 N3 Zr 129.56(11) . . ? C5 N4 C4 110.27(13) . . ? C5 N4 C6 111.28(13) . . ? C4 N4 C6 111.22(14) . . ? C5 N4 Zr 105.27(10) . . ? C4 N4 Zr 108.94(9) . . ? C6 N4 Zr 109.67(9) . . ? C13 N5 Zr 134.03(11) . . ? C13 N5 H5 107.4(14) . . ? Zr N5 H5 118.6(14) . . ? C17 N6 C24 120.02(12) . . ? C17 N6 Zr 91.00(9) . . ? C24 N6 Zr 148.63(9) . . ? C17 N7 C18 117.81(13) . . ? C17 N7 Si3 116.45(10) . . ? C18 N7 Si3 120.73(11) . . ? N1 C1 C4 108.99(14) . . ? N1 C1 H1A 109.9 . . ? C4 C1 H1A 109.9 . . ? N1 C1 H1B 109.9 . . ? C4 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? N2 C2 C5 110.97(13) . . ? N2 C2 H2A 109.4 . . ? C5 C2 H2A 109.4 . . ? N2 C2 H2B 109.4 . . ? C5 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? N3 C3 C6 106.54(14) . . ? N3 C3 H3A 110.4 . . ? C6 C3 H3A 110.4 . . ? N3 C3 H3B 110.4 . . ? C6 C3 H3B 110.4 . . ? H3A C3 H3B 108.6 . . ? N4 C4 C1 108.22(14) . . ? N4 C4 H4A 110.1 . . ? C1 C4 H4A 110.1 . . ? N4 C4 H4B 110.1 . . ? C1 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? N4 C5 C2 109.75(14) . . ? N4 C5 H5B 109.7 . . ? C2 C5 H5B 109.7 . . ? N4 C5 H5C 109.7 . . ? C2 C5 H5C 109.7 . . ? H5B C5 H5C 108.2 . . ? N4 C6 C3 110.99(14) . . ? N4 C6 H6A 109.4 . . ? C3 C6 H6A 109.4 . . ? N4 C6 H6B 109.4 . . ? C3 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si1 C9 H9A 109.5 . . ? Si1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2 C10 H10A 109.5 . . ? Si2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si2 C11 H11A 109.5 . . ? Si2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N5 C13 C15 108.93(14) . . ? N5 C13 C16 110.41(15) . . ? C15 C13 C16 109.21(16) . . ? N5 C13 C14 110.69(14) . . ? C15 C13 C14 109.48(16) . . ? C16 C13 C14 108.09(16) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N6 C17 N3 111.32(13) . . ? N6 C17 N7 125.41(13) . . ? N3 C17 N7 123.27(13) . . ? N6 C17 Zr 60.37(8) . . ? N3 C17 Zr 51.43(8) . . ? N7 C17 Zr 171.60(10) . . ? N7 C18 C20 110.23(14) . . ? N7 C18 C19 110.91(14) . . ? C20 C18 C19 107.54(16) . . ? N7 C18 H18A 109.4 . . ? C20 C18 H18A 109.4 . . ? C19 C18 H18A 109.4 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si3 C21 H21A 109.5 . . ? Si3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si3 C22 H22A 109.5 . . ? Si3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si3 C23 H23A 109.5 . . ? Si3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N6 C24 C25 112.11(13) . . ? N6 C24 C26 111.25(12) . . ? C25 C24 C26 109.54(14) . . ? N6 C24 H24A 107.9 . . ? C25 C24 H24A 107.9 . . ? C26 C24 H24A 107.9 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8 Si1 N1 C1 172.59(13) . . . . ? C9 Si1 N1 C1 -62.86(14) . . . . ? C7 Si1 N1 C1 55.02(14) . . . . ? C8 Si1 N1 Zr 8.28(14) . . . . ? C9 Si1 N1 Zr 132.83(10) . . . . ? C7 Si1 N1 Zr -109.29(11) . . . . ? N5 Zr N1 C1 134.44(13) . . . . ? N2 Zr N1 C1 29.82(15) . . . . ? N3 Zr N1 C1 -85.20(13) . . . . ? N6 Zr N1 C1 -139.72(12) . . . . ? N4 Zr N1 C1 -21.25(12) . . . . ? C17 Zr N1 C1 -108.83(13) . . . . ? N5 Zr N1 Si1 -62.27(10) . . . . ? N2 Zr N1 Si1 -166.89(8) . . . . ? N3 Zr N1 Si1 78.09(10) . . . . ? N6 Zr N1 Si1 23.57(12) . . . . ? N4 Zr N1 Si1 142.04(11) . . . . ? C17 Zr N1 Si1 54.46(11) . . . . ? C12 Si2 N2 C2 -162.46(12) . . . . ? C10 Si2 N2 C2 73.51(14) . . . . ? C11 Si2 N2 C2 -43.56(14) . . . . ? C12 Si2 N2 Zr 14.72(14) . . . . ? C10 Si2 N2 Zr -109.31(12) . . . . ? C11 Si2 N2 Zr 133.62(11) . . . . ? N5 Zr N2 C2 -148.50(13) . . . . ? N1 Zr N2 C2 -45.83(15) . . . . ? N3 Zr N2 C2 64.29(14) . . . . ? N6 Zr N2 C2 124.54(13) . . . . ? N4 Zr N2 C2 5.37(13) . . . . ? C17 Zr N2 C2 93.92(13) . . . . ? N5 Zr N2 Si2 34.70(11) . . . . ? N1 Zr N2 Si2 137.37(9) . . . . ? N3 Zr N2 Si2 -112.51(10) . . . . ? N6 Zr N2 Si2 -52.25(11) . . . . ? N4 Zr N2 Si2 -171.43(11) . . . . ? C17 Zr N2 Si2 -82.88(10) . . . . ? N5 Zr N3 C17 -24.01(15) . . . . ? N2 Zr N3 C17 101.57(11) . . . . ? N1 Zr N3 C17 -129.03(11) . . . . ? N6 Zr N3 C17 -4.96(9) . . . . ? N4 Zr N3 C17 163.27(12) . . . . ? N5 Zr N3 C3 177.73(14) . . . . ? N2 Zr N3 C3 -56.69(17) . . . . ? N1 Zr N3 C3 72.71(16) . . . . ? N6 Zr N3 C3 -163.22(18) . . . . ? N4 Zr N3 C3 5.01(15) . . . . ? C17 Zr N3 C3 -158.3(2) . . . . ? N5 Zr N4 C5 45.11(16) . . . . ? N2 Zr N4 C5 -28.26(10) . . . . ? N1 Zr N4 C5 109.67(11) . . . . ? N3 Zr N4 C5 -145.48(12) . . . . ? N6 Zr N4 C5 -133.71(10) . . . . ? C17 Zr N4 C5 -137.60(10) . . . . ? N5 Zr N4 C4 -73.15(15) . . . . ? N2 Zr N4 C4 -146.52(12) . . . . ? N1 Zr N4 C4 -8.58(11) . . . . ? N3 Zr N4 C4 96.27(12) . . . . ? N6 Zr N4 C4 108.03(11) . . . . ? C17 Zr N4 C4 104.15(11) . . . . ? N5 Zr N4 C6 164.91(11) . . . . ? N2 Zr N4 C6 91.54(11) . . . . ? N1 Zr N4 C6 -130.52(11) . . . . ? N3 Zr N4 C6 -25.67(11) . . . . ? N6 Zr N4 C6 -13.90(12) . . . . ? C17 Zr N4 C6 -17.79(11) . . . . ? N2 Zr N5 C13 70.86(15) . . . . ? N1 Zr N5 C13 -55.88(15) . . . . ? N3 Zr N5 C13 -161.31(13) . . . . ? N6 Zr N5 C13 -177.25(15) . . . . ? N4 Zr N5 C13 3.7(2) . . . . ? C17 Zr N5 C13 -173.35(13) . . . . ? N5 Zr N6 C17 172.44(9) . . . . ? N2 Zr N6 C17 -90.46(10) . . . . ? N1 Zr N6 C17 80.29(10) . . . . ? N3 Zr N6 C17 4.91(9) . . . . ? N4 Zr N6 C17 -8.10(10) . . . . ? N5 Zr N6 C24 0.65(18) . . . . ? N2 Zr N6 C24 97.76(18) . . . . ? N1 Zr N6 C24 -91.50(19) . . . . ? N3 Zr N6 C24 -166.9(2) . . . . ? N4 Zr N6 C24 -179.89(17) . . . . ? C17 Zr N6 C24 -171.8(2) . . . . ? C23 Si3 N7 C17 110.27(13) . . . . ? C22 Si3 N7 C17 -10.01(14) . . . . ? C21 Si3 N7 C17 -127.89(13) . . . . ? C23 Si3 N7 C18 -95.31(14) . . . . ? C22 Si3 N7 C18 144.41(13) . . . . ? C21 Si3 N7 C18 26.53(16) . . . . ? Si1 N1 C1 C4 -117.71(13) . . . . ? Zr N1 C1 C4 48.66(18) . . . . ? Si2 N2 C2 C5 -163.89(13) . . . . ? Zr N2 C2 C5 18.6(2) . . . . ? C17 N3 C3 C6 -137.19(18) . . . . ? Zr N3 C3 C6 15.9(2) . . . . ? C5 N4 C4 C1 -80.49(17) . . . . ? C6 N4 C4 C1 155.57(14) . . . . ? Zr N4 C4 C1 34.57(16) . . . . ? N1 C1 C4 N4 -52.98(19) . . . . ? C4 N4 C5 C2 164.15(15) . . . . ? C6 N4 C5 C2 -71.95(18) . . . . ? Zr N4 C5 C2 46.79(16) . . . . ? N2 C2 C5 N4 -45.2(2) . . . . ? C5 N4 C6 C3 159.41(14) . . . . ? C4 N4 C6 C3 -77.22(17) . . . . ? Zr N4 C6 C3 43.35(16) . . . . ? N3 C3 C6 N4 -38.5(2) . . . . ? Zr N5 C13 C15 -5.4(2) . . . . ? Zr N5 C13 C16 114.55(17) . . . . ? Zr N5 C13 C14 -125.79(15) . . . . ? C24 N6 C17 N3 167.80(13) . . . . ? Zr N6 C17 N3 -7.28(13) . . . . ? C24 N6 C17 N7 -12.2(2) . . . . ? Zr N6 C17 N7 172.76(14) . . . . ? C24 N6 C17 Zr 175.07(14) . . . . ? C3 N3 C17 N6 167.35(16) . . . . ? Zr N3 C17 N6 8.10(15) . . . . ? C3 N3 C17 N7 -12.7(3) . . . . ? Zr N3 C17 N7 -171.94(12) . . . . ? C3 N3 C17 Zr 159.3(2) . . . . ? C18 N7 C17 N6 122.78(17) . . . . ? Si3 N7 C17 N6 -82.03(17) . . . . ? C18 N7 C17 N3 -57.2(2) . . . . ? Si3 N7 C17 N3 98.01(17) . . . . ? C18 N7 C17 Zr -105.8(7) . . . . ? Si3 N7 C17 Zr 49.4(8) . . . . ? N5 Zr C17 N6 -8.13(10) . . . . ? N2 Zr C17 N6 100.84(9) . . . . ? N1 Zr C17 N6 -114.23(9) . . . . ? N3 Zr C17 N6 -171.32(16) . . . . ? N4 Zr C17 N6 173.20(9) . . . . ? N5 Zr C17 N3 163.19(11) . . . . ? N2 Zr C17 N3 -87.84(11) . . . . ? N1 Zr C17 N3 57.09(12) . . . . ? N6 Zr C17 N3 171.32(16) . . . . ? N4 Zr C17 N3 -15.48(11) . . . . ? N5 Zr C17 N7 -143.4(7) . . . . ? N2 Zr C17 N7 -34.5(7) . . . . ? N1 Zr C17 N7 110.5(7) . . . . ? N3 Zr C17 N7 53.4(7) . . . . ? N6 Zr C17 N7 -135.3(8) . . . . ? N4 Zr C17 N7 37.9(7) . . . . ? C17 N7 C18 C20 -147.51(15) . . . . ? Si3 N7 C18 C20 58.40(18) . . . . ? C17 N7 C18 C19 -28.5(2) . . . . ? Si3 N7 C18 C19 177.38(13) . . . . ? C17 N6 C24 C25 125.39(15) . . . . ? Zr N6 C24 C25 -64.1(2) . . . . ? C17 N6 C24 C26 -111.57(16) . . . . ? Zr N6 C24 C26 58.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 30.25 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.013 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.067 # Attachment '- ar05191_0l.cif' data_ar05191_0l _database_code_depnum_ccdc_archive 'CCDC 840652' #TrackingRef '- ar05191_0l.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H53 Cl N6 Si3 Zr' _chemical_formula_weight 612.64 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' Cl Cl 0.1484 0.1585 '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 9.517(3) _cell_length_b 10.057(4) _cell_length_c 19.313(6) _cell_angle_alpha 76.739(5) _cell_angle_beta 80.800(3) _cell_angle_gamma 62.440(3) _cell_volume 1592.0(10) _cell_formula_units_Z 2 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9281 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 29.26 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 0.563 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9079 _exptl_absorpt_correction_T_max 0.9458 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7558 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 27.88 _reflns_number_total 7558 _reflns_number_gt 6665 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0287P)^2^+0.7899P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7558 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0643 _refine_ls_wR_factor_gt 0.0616 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.002 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 Zr Zr 0.146295(17) 0.803418(17) 0.205184(8) 0.01456(5) Uani 1 1 d . . . Cl Cl -0.08396(5) 0.74445(5) 0.24952(2) 0.02285(9) Uani 1 1 d . . . Si1 Si -0.19908(5) 1.14249(5) 0.19244(2) 0.01948(10) Uani 1 1 d . . . Si2 Si 0.15224(6) 0.52341(5) 0.12607(2) 0.01888(10) Uani 1 1 d . . . Si5 Si 0.33279(6) 0.90916(6) 0.41355(3) 0.02514(11) Uani 1 1 d . . . N2 N 0.23241(16) 0.64473(15) 0.13553(7) 0.0183(3) Uani 1 1 d . . . N4 N 0.29886(15) 0.88985(15) 0.11218(7) 0.0167(3) Uani 1 1 d . . . N5 N 0.19990(17) 0.73033(16) 0.32559(7) 0.0201(3) Uani 1 1 d . . . N3 N 0.34777(16) 0.80381(16) 0.24331(7) 0.0199(3) Uani 1 1 d . . . N6 N 0.41372(17) 0.75672(17) 0.36589(7) 0.0208(3) Uani 1 1 d . . . N1 N -0.00411(16) 1.03103(15) 0.16247(7) 0.0181(3) Uani 1 1 d . . . C16 C 0.32267(19) 0.76279(18) 0.31347(8) 0.0182(3) Uani 1 1 d . . . C5 C 0.42334(19) 0.75188(19) 0.08662(9) 0.0206(3) Uani 1 1 d . . . H5A H 0.5056 0.6942 0.1218 0.025 Uiso 1 1 calc R . . H5B H 0.4747 0.7814 0.0410 0.025 Uiso 1 1 calc R . . C1 C 0.0384(2) 1.10663(19) 0.09288(9) 0.0210(3) Uani 1 1 d . . . H1A H 0.0589 1.1903 0.1001 0.025 Uiso 1 1 calc R . . H1B H -0.0513 1.1512 0.0617 0.025 Uiso 1 1 calc R . . C4 C 0.18564(19) 0.99259(19) 0.05722(8) 0.0202(3) Uani 1 1 d . . . H4A H 0.1559 0.9326 0.0335 0.024 Uiso 1 1 calc R . . H4B H 0.2354 1.0472 0.0207 0.024 Uiso 1 1 calc R . . C6 C 0.3701(2) 0.97109(19) 0.13898(9) 0.0203(3) Uani 1 1 d . . . H6A H 0.2868 1.0728 0.1468 0.024 Uiso 1 1 calc R . . H6B H 0.4513 0.9854 0.1033 0.024 Uiso 1 1 calc R . . C10 C 0.2777(2) 0.4026(2) 0.05765(9) 0.0263(4) Uani 1 1 d . . . H10A H 0.3864 0.3416 0.0728 0.039 Uiso 1 1 calc R . . H10B H 0.2786 0.4685 0.0117 0.039 Uiso 1 1 calc R . . H10C H 0.2334 0.3347 0.0528 0.039 Uiso 1 1 calc R . . C11 C -0.0500(2) 0.6322(2) 0.08965(10) 0.0294(4) Uani 1 1 d . . . H11A H -0.1234 0.6986 0.1226 0.044 Uiso 1 1 calc R . . H11B H -0.0887 0.5605 0.0842 0.044 Uiso 1 1 calc R . . H11C H -0.0435 0.6943 0.0432 0.044 Uiso 1 1 calc R . . C12 C 0.1516(2) 0.3849(2) 0.20951(9) 0.0262(4) Uani 1 1 d . . . H12A H 0.0876 0.4409 0.2476 0.039 Uiso 1 1 calc R . . H12B H 0.2606 0.3204 0.2238 0.039 Uiso 1 1 calc R . . H12C H 0.1061 0.3209 0.2007 0.039 Uiso 1 1 calc R . . C3 C 0.4465(2) 0.8780(2) 0.20902(9) 0.0226(3) Uani 1 1 d . . . H3A H 0.5569 0.8017 0.1999 0.027 Uiso 1 1 calc R . . H3B H 0.4477 0.9451 0.2390 0.027 Uiso 1 1 calc R . . C51 C 0.1727(2) 0.6434(2) 0.39451(9) 0.0239(4) Uani 1 1 d . . . H51A H 0.2511 0.6297 0.4276 0.029 Uiso 1 1 calc R . . C511 C 0.2028(3) 0.4859(2) 0.38489(10) 0.0317(4) Uani 1 1 d . . . H51B H 0.3104 0.4341 0.3635 0.048 Uiso 1 1 calc R . . H51C H 0.1254 0.4964 0.3536 0.048 Uiso 1 1 calc R . . H51D H 0.1918 0.4260 0.4314 0.048 Uiso 1 1 calc R . . C61 C 0.5908(2) 0.6632(2) 0.35672(10) 0.0279(4) Uani 1 1 d . . . H61A H 0.6385 0.7287 0.3263 0.033 Uiso 1 1 calc R . . C8 C -0.2537(2) 1.3508(2) 0.16138(10) 0.0294(4) Uani 1 1 d . . . H8A H -0.1824 1.3768 0.1808 0.044 Uiso 1 1 calc R . . H8B H -0.3635 1.4115 0.1780 0.044 Uiso 1 1 calc R . . H8C H -0.2436 1.3726 0.1092 0.044 Uiso 1 1 calc R . . C7 C -0.2261(2) 1.1138(2) 0.29155(9) 0.0284(4) Uani 1 1 d . . . H7A H -0.1989 1.0063 0.3106 0.043 Uiso 1 1 calc R . . H7B H -0.3369 1.1770 0.3059 0.043 Uiso 1 1 calc R . . H7C H -0.1565 1.1429 0.3103 0.043 Uiso 1 1 calc R . . C2 C 0.3503(2) 0.65200(19) 0.07597(9) 0.0218(3) Uani 1 1 d . . . H2A H 0.2975 0.6939 0.0304 0.026 Uiso 1 1 calc R . . H2B H 0.4351 0.5479 0.0733 0.026 Uiso 1 1 calc R . . C13 C 0.1414(2) 1.0558(2) 0.37566(12) 0.0366(5) Uani 1 1 d . . . H13A H 0.0665 1.0117 0.3818 0.055 Uiso 1 1 calc R . . H13B H 0.1601 1.0899 0.3248 0.055 Uiso 1 1 calc R . . H13C H 0.0970 1.1428 0.4005 0.055 Uiso 1 1 calc R . . C9 C -0.3408(2) 1.1042(2) 0.15266(11) 0.0318(4) Uani 1 1 d . . . H9A H -0.3172 0.9965 0.1673 0.048 Uiso 1 1 calc R . . H9B H -0.3295 1.1286 0.1006 0.048 Uiso 1 1 calc R . . H9C H -0.4497 1.1677 0.1692 0.048 Uiso 1 1 calc R . . C611 C 0.6606(2) 0.6050(3) 0.42969(11) 0.0366(5) Uani 1 1 d . . . H61B H 0.6349 0.6917 0.4526 0.055 Uiso 1 1 calc R . . H61C H 0.7761 0.5466 0.4239 0.055 Uiso 1 1 calc R . . H61D H 0.6155 0.5393 0.4595 0.055 Uiso 1 1 calc R . . C15 C 0.2977(3) 0.8442(3) 0.51033(10) 0.0374(5) Uani 1 1 d . . . H15A H 0.2265 0.7959 0.5164 0.056 Uiso 1 1 calc R . . H15B H 0.2489 0.9320 0.5348 0.056 Uiso 1 1 calc R . . H15C H 0.3991 0.7705 0.5307 0.056 Uiso 1 1 calc R . . C612 C 0.6326(2) 0.5276(3) 0.32241(12) 0.0411(5) Uani 1 1 d . . . H61E H 0.5886 0.5631 0.2754 0.062 Uiso 1 1 calc R . . H61F H 0.5879 0.4619 0.3525 0.062 Uiso 1 1 calc R . . H61G H 0.7483 0.4699 0.3170 0.062 Uiso 1 1 calc R . . C512 C 0.0064(2) 0.7277(2) 0.42808(10) 0.0337(4) Uani 1 1 d . . . H51E H -0.0096 0.8282 0.4338 0.051 Uiso 1 1 calc R . . H51F H -0.0053 0.6690 0.4748 0.051 Uiso 1 1 calc R . . H51G H -0.0726 0.7400 0.3972 0.051 Uiso 1 1 calc R . . C14 C 0.4681(3) 1.0025(3) 0.39973(12) 0.0427(5) Uani 1 1 d . . . H14A H 0.5707 0.9292 0.4190 0.064 Uiso 1 1 calc R . . H14B H 0.4205 1.0901 0.4243 0.064 Uiso 1 1 calc R . . H14C H 0.4838 1.0371 0.3486 0.064 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 Zr 0.01486(8) 0.01557(8) 0.01327(8) -0.00210(5) -0.00021(5) -0.00718(6) Cl 0.01970(19) 0.0248(2) 0.0257(2) -0.00375(16) 0.00241(16) -0.01282(16) Si1 0.0162(2) 0.0189(2) 0.0193(2) -0.00203(17) -0.00051(17) -0.00520(18) Si2 0.0231(2) 0.0177(2) 0.0172(2) -0.00165(17) -0.00379(17) -0.01001(19) Si5 0.0296(3) 0.0287(3) 0.0222(2) -0.0068(2) -0.0011(2) -0.0163(2) N2 0.0177(6) 0.0192(7) 0.0187(7) -0.0045(5) 0.0008(5) -0.0089(6) N4 0.0167(6) 0.0182(6) 0.0156(6) -0.0032(5) -0.0010(5) -0.0081(5) N5 0.0226(7) 0.0241(7) 0.0153(6) -0.0010(5) -0.0001(5) -0.0132(6) N3 0.0210(7) 0.0279(7) 0.0150(6) -0.0010(6) -0.0018(5) -0.0154(6) N6 0.0203(7) 0.0268(7) 0.0168(7) -0.0028(6) -0.0031(5) -0.0117(6) N1 0.0178(6) 0.0171(6) 0.0172(6) -0.0016(5) 0.0006(5) -0.0071(5) C16 0.0196(8) 0.0174(7) 0.0169(7) -0.0023(6) -0.0022(6) -0.0076(6) C5 0.0179(8) 0.0220(8) 0.0207(8) -0.0063(6) 0.0029(6) -0.0081(7) C1 0.0199(8) 0.0201(8) 0.0193(8) -0.0003(6) -0.0008(6) -0.0074(7) C4 0.0209(8) 0.0235(8) 0.0139(7) -0.0001(6) -0.0013(6) -0.0093(7) C6 0.0240(8) 0.0239(8) 0.0180(8) -0.0029(6) -0.0003(6) -0.0156(7) C10 0.0352(10) 0.0242(9) 0.0223(8) -0.0058(7) -0.0030(7) -0.0145(8) C11 0.0287(9) 0.0330(10) 0.0294(10) 0.0004(8) -0.0093(8) -0.0164(8) C12 0.0368(10) 0.0212(8) 0.0216(8) -0.0011(7) -0.0031(7) -0.0144(8) C3 0.0237(8) 0.0323(9) 0.0174(8) -0.0019(7) -0.0005(6) -0.0184(8) C51 0.0310(9) 0.0297(9) 0.0153(8) 0.0002(7) -0.0012(7) -0.0190(8) C511 0.0442(11) 0.0282(10) 0.0248(9) 0.0028(8) -0.0049(8) -0.0202(9) C61 0.0206(8) 0.0358(10) 0.0252(9) -0.0002(8) -0.0053(7) -0.0120(8) C8 0.0290(9) 0.0206(9) 0.0301(10) -0.0028(7) 0.0002(8) -0.0053(8) C7 0.0290(9) 0.0270(9) 0.0220(9) -0.0040(7) 0.0024(7) -0.0080(8) C2 0.0210(8) 0.0231(8) 0.0214(8) -0.0079(7) 0.0032(7) -0.0097(7) C13 0.0351(11) 0.0302(10) 0.0411(12) -0.0098(9) -0.0044(9) -0.0095(9) C9 0.0219(9) 0.0368(11) 0.0351(10) -0.0033(8) -0.0049(8) -0.0121(8) C611 0.0283(10) 0.0445(12) 0.0327(11) -0.0024(9) -0.0115(8) -0.0115(9) C15 0.0479(12) 0.0476(12) 0.0232(9) -0.0129(9) 0.0036(9) -0.0255(11) C612 0.0290(10) 0.0421(12) 0.0389(12) -0.0146(10) -0.0071(9) 0.0003(9) C512 0.0372(11) 0.0406(11) 0.0230(9) -0.0039(8) 0.0080(8) -0.0208(9) C14 0.0543(14) 0.0489(13) 0.0430(12) -0.0122(10) -0.0021(10) -0.0365(12) _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 N1 2.1092(15) . ? Zr N2 2.1095(15) . ? Zr N3 2.1631(15) . ? Zr N5 2.3358(15) . ? Zr N4 2.3891(14) . ? Zr Cl 2.5014(8) . ? Zr C16 2.7302(17) . ? Si1 N1 1.7505(15) . ? Si1 C7 1.8630(19) . ? Si1 C9 1.872(2) . ? Si1 C8 1.880(2) . ? Si2 N2 1.7642(15) . ? Si2 C12 1.8741(18) . ? Si2 C11 1.8783(19) . ? Si2 C10 1.8810(19) . ? Si5 N6 1.7660(16) . ? Si5 C15 1.864(2) . ? Si5 C13 1.864(2) . ? Si5 C14 1.872(2) . ? N2 C2 1.487(2) . ? N4 C5 1.476(2) . ? N4 C4 1.479(2) . ? N4 C6 1.488(2) . ? N5 C16 1.326(2) . ? N5 C51 1.472(2) . ? N3 C16 1.340(2) . ? N3 C3 1.450(2) . ? N6 C16 1.408(2) . ? N6 C61 1.507(2) . ? N1 C1 1.480(2) . ? C5 C2 1.524(2) . ? C1 C4 1.523(2) . ? C6 C3 1.529(2) . ? C51 C511 1.524(3) . ? C51 C512 1.525(3) . ? C61 C612 1.512(3) . ? C61 C611 1.527(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 N1 Zr N2 116.66(6) . . ? N1 Zr N3 107.22(6) . . ? N2 Zr N3 108.22(5) . . ? N1 Zr N5 121.08(5) . . ? N2 Zr N5 122.14(6) . . ? N3 Zr N5 57.87(5) . . ? N1 Zr N4 73.08(5) . . ? N2 Zr N4 74.84(5) . . ? N3 Zr N4 67.18(5) . . ? N5 Zr N4 125.04(5) . . ? N1 Zr Cl 92.17(5) . . ? N2 Zr Cl 91.68(4) . . ? N3 Zr Cl 140.90(4) . . ? N5 Zr Cl 83.03(4) . . ? N4 Zr Cl 151.91(3) . . ? N1 Zr C16 116.17(5) . . ? N2 Zr C16 120.31(5) . . ? N3 Zr C16 28.92(5) . . ? N5 Zr C16 29.02(5) . . ? N4 Zr C16 96.03(5) . . ? Cl Zr C16 112.01(4) . . ? N1 Si1 C7 112.30(8) . . ? N1 Si1 C9 109.83(8) . . ? C7 Si1 C9 111.65(9) . . ? N1 Si1 C8 110.48(8) . . ? C7 Si1 C8 106.14(9) . . ? C9 Si1 C8 106.21(9) . . ? N2 Si2 C12 113.46(8) . . ? N2 Si2 C11 112.27(8) . . ? C12 Si2 C11 111.21(9) . . ? N2 Si2 C10 109.64(8) . . ? C12 Si2 C10 105.26(9) . . ? C11 Si2 C10 104.34(9) . . ? N6 Si5 C15 111.60(9) . . ? N6 Si5 C13 108.58(8) . . ? C15 Si5 C13 109.56(10) . . ? N6 Si5 C14 109.57(9) . . ? C15 Si5 C14 110.75(10) . . ? C13 Si5 C14 106.64(11) . . ? C2 N2 Si2 111.64(10) . . ? C2 N2 Zr 119.74(10) . . ? Si2 N2 Zr 127.24(7) . . ? C5 N4 C4 112.16(13) . . ? C5 N4 C6 110.98(13) . . ? C4 N4 C6 111.30(13) . . ? C5 N4 Zr 105.85(10) . . ? C4 N4 Zr 105.20(10) . . ? C6 N4 Zr 111.08(9) . . ? C16 N5 C51 121.01(14) . . ? C16 N5 Zr 92.23(10) . . ? C51 N5 Zr 144.77(11) . . ? C16 N3 C3 126.98(14) . . ? C16 N3 Zr 99.74(10) . . ? C3 N3 Zr 129.96(11) . . ? C16 N6 C61 116.48(14) . . ? C16 N6 Si5 117.63(11) . . ? C61 N6 Si5 120.83(11) . . ? C1 N1 Si1 110.98(10) . . ? C1 N1 Zr 120.83(10) . . ? Si1 N1 Zr 127.38(7) . . ? N5 C16 N3 109.90(14) . . ? N5 C16 N6 125.71(15) . . ? N3 C16 N6 124.40(14) . . ? N5 C16 Zr 58.75(8) . . ? N3 C16 Zr 51.34(8) . . ? N6 C16 Zr 173.92(11) . . ? N4 C5 C2 109.82(13) . . ? N1 C1 C4 110.43(13) . . ? N4 C4 C1 108.78(13) . . ? N4 C6 C3 109.47(13) . . ? N3 C3 C6 104.81(13) . . ? N5 C51 C511 109.77(14) . . ? N5 C51 C512 111.83(15) . . ? C511 C51 C512 111.13(15) . . ? N6 C61 C612 111.71(15) . . ? N6 C61 C611 109.18(15) . . ? C612 C61 C611 108.46(17) . . ? N2 C2 C5 110.92(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 Si2 N2 C2 132.06(12) . . . . ? C11 Si2 N2 C2 -100.79(13) . . . . ? C10 Si2 N2 C2 14.70(13) . . . . ? C12 Si2 N2 Zr -61.60(12) . . . . ? C11 Si2 N2 Zr 65.55(11) . . . . ? C10 Si2 N2 Zr -178.96(9) . . . . ? N1 Zr N2 C2 69.67(13) . . . . ? N3 Zr N2 C2 -51.26(13) . . . . ? N5 Zr N2 C2 -114.22(12) . . . . ? N4 Zr N2 C2 7.93(11) . . . . ? Cl Zr N2 C2 162.95(11) . . . . ? C16 Zr N2 C2 -80.21(13) . . . . ? N1 Zr N2 Si2 -95.69(10) . . . . ? N3 Zr N2 Si2 143.39(9) . . . . ? N5 Zr N2 Si2 80.42(10) . . . . ? N4 Zr N2 Si2 -157.42(10) . . . . ? Cl Zr N2 Si2 -2.41(9) . . . . ? C16 Zr N2 Si2 114.43(9) . . . . ? N1 Zr N4 C5 -154.17(11) . . . . ? N2 Zr N4 C5 -29.53(10) . . . . ? N3 Zr N4 C5 88.20(10) . . . . ? N5 Zr N4 C5 89.36(10) . . . . ? Cl Zr N4 C5 -93.24(11) . . . . ? C16 Zr N4 C5 90.28(10) . . . . ? N1 Zr N4 C4 -35.26(10) . . . . ? N2 Zr N4 C4 89.38(10) . . . . ? N3 Zr N4 C4 -152.89(11) . . . . ? N5 Zr N4 C4 -151.73(9) . . . . ? Cl Zr N4 C4 25.67(14) . . . . ? C16 Zr N4 C4 -150.82(10) . . . . ? N1 Zr N4 C6 85.28(11) . . . . ? N2 Zr N4 C6 -150.08(11) . . . . ? N3 Zr N4 C6 -32.35(10) . . . . ? N5 Zr N4 C6 -31.19(12) . . . . ? Cl Zr N4 C6 146.21(8) . . . . ? C16 Zr N4 C6 -30.28(10) . . . . ? N1 Zr N5 C16 -88.56(11) . . . . ? N2 Zr N5 C16 95.50(11) . . . . ? N3 Zr N5 C16 3.13(9) . . . . ? N4 Zr N5 C16 1.87(12) . . . . ? Cl Zr N5 C16 -176.90(10) . . . . ? N1 Zr N5 C51 109.83(19) . . . . ? N2 Zr N5 C51 -66.1(2) . . . . ? N3 Zr N5 C51 -158.5(2) . . . . ? N4 Zr N5 C51 -159.74(18) . . . . ? Cl Zr N5 C51 21.49(19) . . . . ? C16 Zr N5 C51 -161.6(3) . . . . ? N1 Zr N3 C16 113.19(10) . . . . ? N2 Zr N3 C16 -120.19(10) . . . . ? N5 Zr N3 C16 -3.14(9) . . . . ? N4 Zr N3 C16 175.73(11) . . . . ? Cl Zr N3 C16 -3.19(14) . . . . ? N1 Zr N3 C3 -46.90(15) . . . . ? N2 Zr N3 C3 79.72(15) . . . . ? N5 Zr N3 C3 -163.23(17) . . . . ? N4 Zr N3 C3 15.65(14) . . . . ? Cl Zr N3 C3 -163.27(12) . . . . ? C16 Zr N3 C3 -160.1(2) . . . . ? C15 Si5 N6 C16 116.61(14) . . . . ? C13 Si5 N6 C16 -4.24(15) . . . . ? C14 Si5 N6 C16 -120.35(14) . . . . ? C15 Si5 N6 C61 -89.43(15) . . . . ? C13 Si5 N6 C61 149.72(13) . . . . ? C14 Si5 N6 C61 33.61(16) . . . . ? C7 Si1 N1 C1 -150.06(12) . . . . ? C9 Si1 N1 C1 85.07(13) . . . . ? C8 Si1 N1 C1 -31.77(13) . . . . ? C7 Si1 N1 Zr 40.32(12) . . . . ? C9 Si1 N1 Zr -84.55(11) . . . . ? C8 Si1 N1 Zr 158.61(9) . . . . ? N2 Zr N1 C1 -47.21(13) . . . . ? N3 Zr N1 C1 74.25(13) . . . . ? N5 Zr N1 C1 136.64(11) . . . . ? N4 Zr N1 C1 15.49(11) . . . . ? Cl Zr N1 C1 -140.18(12) . . . . ? C16 Zr N1 C1 103.93(12) . . . . ? N2 Zr N1 Si1 121.50(9) . . . . ? N3 Zr N1 Si1 -117.05(9) . . . . ? N5 Zr N1 Si1 -54.65(11) . . . . ? N4 Zr N1 Si1 -175.80(10) . . . . ? Cl Zr N1 Si1 28.52(9) . . . . ? C16 Zr N1 Si1 -87.36(10) . . . . ? C51 N5 C16 N3 163.18(14) . . . . ? Zr N5 C16 N3 -4.56(13) . . . . ? C51 N5 C16 N6 -17.2(2) . . . . ? Zr N5 C16 N6 175.03(15) . . . . ? C51 N5 C16 Zr 167.74(17) . . . . ? C3 N3 C16 N5 165.92(16) . . . . ? Zr N3 C16 N5 4.99(15) . . . . ? C3 N3 C16 N6 -13.7(3) . . . . ? Zr N3 C16 N6 -174.60(13) . . . . ? C3 N3 C16 Zr 160.9(2) . . . . ? C61 N6 C16 N5 126.85(18) . . . . ? Si5 N6 C16 N5 -78.06(19) . . . . ? C61 N6 C16 N3 -53.6(2) . . . . ? Si5 N6 C16 N3 101.47(17) . . . . ? C61 N6 C16 Zr -97.5(11) . . . . ? Si5 N6 C16 Zr 57.6(11) . . . . ? N1 Zr C16 N5 107.46(10) . . . . ? N2 Zr C16 N5 -102.52(11) . . . . ? N3 Zr C16 N5 -174.51(16) . . . . ? N4 Zr C16 N5 -178.46(10) . . . . ? Cl Zr C16 N5 3.32(10) . . . . ? N1 Zr C16 N3 -78.03(11) . . . . ? N2 Zr C16 N3 71.99(12) . . . . ? N5 Zr C16 N3 174.51(16) . . . . ? N4 Zr C16 N3 -3.95(11) . . . . ? Cl Zr C16 N3 177.83(9) . . . . ? N1 Zr C16 N6 -30.9(11) . . . . ? N2 Zr C16 N6 119.1(11) . . . . ? N3 Zr C16 N6 47.1(11) . . . . ? N5 Zr C16 N6 -138.4(11) . . . . ? N4 Zr C16 N6 43.2(11) . . . . ? Cl Zr C16 N6 -135.1(11) . . . . ? C4 N4 C5 C2 -68.00(17) . . . . ? C6 N4 C5 C2 166.82(13) . . . . ? Zr N4 C5 C2 46.20(14) . . . . ? Si1 N1 C1 C4 -163.36(11) . . . . ? Zr N1 C1 C4 7.04(18) . . . . ? C5 N4 C4 C1 164.35(13) . . . . ? C6 N4 C4 C1 -70.65(16) . . . . ? Zr N4 C4 C1 49.75(14) . . . . ? N1 C1 C4 N4 -39.63(18) . . . . ? C5 N4 C6 C3 -70.69(16) . . . . ? C4 N4 C6 C3 163.65(13) . . . . ? Zr N4 C6 C3 46.78(15) . . . . ? C16 N3 C3 C6 -150.85(16) . . . . ? Zr N3 C3 C6 4.3(2) . . . . ? N4 C6 C3 N3 -33.08(18) . . . . ? C16 N5 C51 C511 -110.65(18) . . . . ? Zr N5 C51 C511 47.8(3) . . . . ? C16 N5 C51 C512 125.52(17) . . . . ? Zr N5 C51 C512 -76.1(2) . . . . ? C16 N6 C61 C612 -32.9(2) . . . . ? Si5 N6 C61 C612 172.89(13) . . . . ? C16 N6 C61 C611 -152.82(16) . . . . ? Si5 N6 C61 C611 52.94(19) . . . . ? Si2 N2 C2 C5 -177.61(11) . . . . ? Zr N2 C2 C5 14.89(18) . . . . ? N4 C5 C2 N2 -42.05(18) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.815 _refine_diff_density_min -0.293 _refine_diff_density_rms 0.057