Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 ---------- X-Sun-Data-Type: text X-Sun-Content-Length: 37054 X-Sun-Charset: us-ascii X-Sun-Content-Lines: 966 data_global #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Mark Thornton-Pett' _publ_contact_author_address ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; _publ_contact_author_phone '+44 (0)113 2336423' _publ_contact_author_fax '+44 (0)113 2336565' _publ_contact_author_email marktp@chem.leeds.ac.uk _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _journal_coden_Cambridge 186 _publ_contact_letter ; The following data is for two compounds included in m/s B105038A ; #======================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Titanium and zirconium complexes with sterically hindered aryl-substituted iminophosphoranato ligands ; loop_ _publ_author_name _publ_author_address 'Mark Thornton-Pett' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Musa Said' ; Wolfson Materials and Catalysis Centre School of Chemical Sciences University of East Anglia Norwich NR4 7TJ UK ; 'Manfred Bochmann' ; Wolfson Materials and Catalysis Centre School of Chemical Sciences University of East Anglia Norwich NR4 7TJ UK ; #================================================================= data_msp125 _database_code_CSD 165391 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H36 N P' _chemical_formula_weight 465.59 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y-1/2, -z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 20.5350(3) _cell_length_b 10.3459(2) _cell_length_c 24.7566(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5259.62(18) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.49 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.176 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 0.125 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9368 _exptl_absorpt_correction_T_max 0.9460 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 10 degree phi range. ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24484 _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5093 _reflns_number_gt 4379 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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^)+(0.0554P)^2^+2.1413P] 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 SHELXL _refine_ls_extinction_coef 0.002(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5093 _refine_ls_number_parameters 314 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1197 _refine_ls_wR_factor_gt 0.1098 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 P1 P 0.165572(18) 0.01402(4) 0.355015(15) 0.02926(15) Uani 1 1 d . . . N1 N 0.19024(6) 0.14162(12) 0.38183(5) 0.0330(3) Uani 1 1 d . . . C1 C 0.16512(7) 0.20204(14) 0.42841(6) 0.0297(3) Uani 1 1 d . . . C2 C 0.18825(8) 0.16695(15) 0.48007(6) 0.0354(4) Uani 1 1 d . . . C3 C 0.16684(8) 0.23610(18) 0.52512(7) 0.0424(4) Uani 1 1 d . . . H3 H 0.1831 0.2128 0.5597 0.051 Uiso 1 1 calc R . . C4 C 0.12292(9) 0.33710(17) 0.52145(7) 0.0439(4) Uani 1 1 d . . . C5 C 0.09931(8) 0.36773(16) 0.47081(7) 0.0392(4) Uani 1 1 d . . . H5 H 0.0681 0.4351 0.4675 0.047 Uiso 1 1 calc R . . C6 C 0.11963(7) 0.30332(15) 0.42443(6) 0.0329(3) Uani 1 1 d . . . C7 C 0.23402(9) 0.05473(17) 0.48720(8) 0.0453(4) Uani 1 1 d . . . H7A H 0.2599 0.0674 0.5200 0.068 Uiso 1 1 calc R . . H7B H 0.2631 0.0492 0.4559 0.068 Uiso 1 1 calc R . . H7C H 0.2089 -0.0254 0.4903 0.068 Uiso 1 1 calc R . . C8 C 0.10127(12) 0.4117(2) 0.57103(9) 0.0669(6) Uani 1 1 d . . . H8A H 0.1009 0.5044 0.5629 0.100 Uiso 1 1 calc R . . H8B H 0.1315 0.3949 0.6008 0.100 Uiso 1 1 calc R . . H8C H 0.0574 0.3840 0.5814 0.100 Uiso 1 1 calc R . . C9 C 0.09134(8) 0.34091(17) 0.37054(7) 0.0407(4) Uani 1 1 d . . . H9A H 0.0642 0.2702 0.3568 0.061 Uiso 1 1 calc R . . H9B H 0.1267 0.3582 0.3450 0.061 Uiso 1 1 calc R . . H9C H 0.0647 0.4188 0.3748 0.061 Uiso 1 1 calc R . . C10 C 0.12211(7) -0.09464(14) 0.39950(6) 0.0305(3) Uani 1 1 d . . . C11 C 0.14806(8) -0.21263(15) 0.41642(7) 0.0354(4) Uani 1 1 d . . . H11 H 0.1891 -0.2406 0.4031 0.042 Uiso 1 1 calc R . . C12 C 0.11388(8) -0.28896(16) 0.45279(7) 0.0420(4) Uani 1 1 d . . . H12 H 0.1317 -0.3691 0.4643 0.050 Uiso 1 1 calc R . . C13 C 0.05412(8) -0.24907(17) 0.47232(7) 0.0417(4) Uani 1 1 d . . . H13 H 0.0308 -0.3025 0.4968 0.050 Uiso 1 1 calc R . . C14 C 0.02815(8) -0.13151(16) 0.45640(7) 0.0381(4) Uani 1 1 d . . . H14 H -0.0129 -0.1042 0.4699 0.046 Uiso 1 1 calc R . . C15 C 0.06244(7) -0.05377(15) 0.42060(6) 0.0339(3) Uani 1 1 d . . . H15 H 0.0452 0.0278 0.4104 0.041 Uiso 1 1 calc R . . C16 C 0.11127(8) 0.03990(15) 0.29769(6) 0.0341(3) Uani 1 1 d . . . C17 C 0.12523(9) 0.14433(17) 0.26356(7) 0.0421(4) Uani 1 1 d . . . H17 H 0.1628 0.1956 0.2698 0.051 Uiso 1 1 calc R . . C18 C 0.08427(10) 0.17319(19) 0.22055(7) 0.0492(5) Uani 1 1 d . . . H18 H 0.0942 0.2437 0.1974 0.059 Uiso 1 1 calc R . . C19 C 0.02916(9) 0.0996(2) 0.21141(7) 0.0499(5) Uani 1 1 d . . . H19 H 0.0008 0.1206 0.1824 0.060 Uiso 1 1 calc R . . C20 C 0.01533(9) -0.00461(19) 0.24442(7) 0.0461(4) Uani 1 1 d . . . H20 H -0.0223 -0.0556 0.2379 0.055 Uiso 1 1 calc R . . C21 C 0.05643(8) -0.03491(17) 0.28716(6) 0.0372(4) Uani 1 1 d . . . H21 H 0.0470 -0.1074 0.3094 0.045 Uiso 1 1 calc R . . C22 C 0.23337(8) -0.07861(16) 0.32834(7) 0.0371(4) Uani 1 1 d . . . H22A H 0.2653 -0.0928 0.3577 0.044 Uiso 1 1 calc R . . H22B H 0.2171 -0.1644 0.3169 0.044 Uiso 1 1 calc R . . C23 C 0.26810(7) -0.01668(15) 0.28126(6) 0.0335(3) Uani 1 1 d . . . C24 C 0.25312(9) -0.05292(18) 0.22869(7) 0.0447(4) Uani 1 1 d . . . H24 H 0.2210 -0.1174 0.2226 0.054 Uiso 1 1 calc R . . C25 C 0.28421(8) 0.00334(17) 0.18495(7) 0.0421(4) Uani 1 1 d . . . H25 H 0.2727 -0.0230 0.1495 0.051 Uiso 1 1 calc R . . C26 C 0.33198(7) 0.09768(15) 0.19172(6) 0.0317(3) Uani 1 1 d . . . C27 C 0.34715(7) 0.13279(15) 0.24436(6) 0.0323(3) Uani 1 1 d . . . H27 H 0.3796 0.1965 0.2505 0.039 Uiso 1 1 calc R . . C28 C 0.31577(7) 0.07654(15) 0.28848(6) 0.0327(3) Uani 1 1 d . . . H28 H 0.3273 0.1026 0.3240 0.039 Uiso 1 1 calc R . . C29 C 0.36548(7) 0.15540(16) 0.14200(6) 0.0339(4) Uani 1 1 d . . . C30 C 0.31436(9) 0.21626(19) 0.10463(7) 0.0453(4) Uani 1 1 d . . . H30A H 0.2910 0.2844 0.1241 0.068 Uiso 1 1 calc R . . H30B H 0.2835 0.1497 0.0929 0.068 Uiso 1 1 calc R . . H30C H 0.3360 0.2535 0.0730 0.068 Uiso 1 1 calc R . . C31 C 0.41477(9) 0.2597(2) 0.15711(8) 0.0490(5) Uani 1 1 d . . . H31A H 0.3925 0.3299 0.1762 0.073 Uiso 1 1 calc R . . H31B H 0.4351 0.2937 0.1243 0.073 Uiso 1 1 calc R . . H31C H 0.4483 0.2225 0.1806 0.073 Uiso 1 1 calc R . . C32 C 0.40090(9) 0.04763(19) 0.11137(7) 0.0478(4) Uani 1 1 d . . . H32A H 0.4233 0.0843 0.0799 0.072 Uiso 1 1 calc R . . H32B H 0.3692 -0.0171 0.0993 0.072 Uiso 1 1 calc R . . H32C H 0.4329 0.0067 0.1353 0.072 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 P1 0.0279(2) 0.0297(2) 0.0302(2) 0.00135(15) 0.00279(14) -0.00051(14) N1 0.0323(7) 0.0325(7) 0.0343(7) 0.0006(5) 0.0021(5) -0.0036(5) C1 0.0280(7) 0.0287(7) 0.0322(8) 0.0005(6) 0.0011(6) -0.0065(5) C2 0.0337(8) 0.0354(8) 0.0371(8) 0.0038(6) -0.0038(6) -0.0093(6) C3 0.0483(10) 0.0484(10) 0.0304(8) 0.0026(7) -0.0035(7) -0.0174(8) C4 0.0475(10) 0.0435(9) 0.0407(9) -0.0083(7) 0.0087(7) -0.0152(8) C5 0.0364(8) 0.0321(8) 0.0490(10) -0.0031(7) 0.0086(7) -0.0070(6) C6 0.0296(8) 0.0309(8) 0.0381(8) 0.0023(6) 0.0019(6) -0.0057(6) C7 0.0433(10) 0.0445(10) 0.0480(10) 0.0092(8) -0.0137(7) -0.0030(7) C8 0.0774(15) 0.0711(15) 0.0523(12) -0.0228(11) 0.0162(11) -0.0140(12) C9 0.0362(9) 0.0405(9) 0.0454(9) 0.0054(7) -0.0017(7) 0.0036(7) C10 0.0291(7) 0.0311(8) 0.0314(7) -0.0007(6) 0.0001(6) -0.0032(6) C11 0.0322(8) 0.0333(8) 0.0406(9) 0.0018(7) 0.0028(6) -0.0003(6) C12 0.0390(9) 0.0343(9) 0.0526(10) 0.0105(7) 0.0012(7) -0.0016(7) C13 0.0387(9) 0.0432(9) 0.0432(9) 0.0083(7) 0.0045(7) -0.0083(7) C14 0.0318(8) 0.0441(9) 0.0383(9) 0.0008(7) 0.0054(6) -0.0022(7) C15 0.0315(8) 0.0347(8) 0.0355(8) 0.0006(7) 0.0016(6) 0.0005(6) C16 0.0363(8) 0.0365(8) 0.0296(8) -0.0030(6) 0.0026(6) 0.0033(6) C17 0.0499(10) 0.0428(9) 0.0337(8) 0.0014(7) 0.0016(7) -0.0021(7) C18 0.0639(12) 0.0511(11) 0.0326(9) 0.0036(8) 0.0008(8) 0.0071(9) C19 0.0506(11) 0.0654(12) 0.0337(9) -0.0063(8) -0.0066(8) 0.0150(9) C20 0.0402(10) 0.0593(11) 0.0387(9) -0.0106(8) -0.0025(7) 0.0030(8) C21 0.0371(8) 0.0407(9) 0.0339(8) -0.0044(7) 0.0015(6) 0.0012(7) C22 0.0352(8) 0.0343(8) 0.0418(9) 0.0021(7) 0.0089(7) 0.0021(6) C23 0.0316(8) 0.0316(8) 0.0374(8) 0.0001(6) 0.0073(6) 0.0025(6) C24 0.0417(9) 0.0489(10) 0.0434(9) -0.0083(8) 0.0068(7) -0.0162(8) C25 0.0425(9) 0.0509(10) 0.0330(8) -0.0098(7) 0.0032(7) -0.0124(7) C26 0.0275(7) 0.0326(8) 0.0349(8) -0.0015(6) 0.0024(6) 0.0010(6) C27 0.0308(8) 0.0305(8) 0.0357(8) -0.0001(6) -0.0014(6) -0.0021(6) C28 0.0344(8) 0.0324(8) 0.0313(8) -0.0021(6) -0.0004(6) 0.0023(6) C29 0.0300(8) 0.0384(8) 0.0332(8) 0.0015(6) 0.0019(6) 0.0004(6) C30 0.0456(10) 0.0538(11) 0.0364(9) 0.0027(8) -0.0025(7) 0.0080(8) C31 0.0464(10) 0.0577(11) 0.0428(10) 0.0093(8) 0.0001(8) -0.0178(9) C32 0.0472(10) 0.0543(11) 0.0418(9) 0.0038(8) 0.0144(8) 0.0100(8) _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 P1 N1 1.5620(13) . ? P1 C10 1.8093(15) . ? P1 C22 1.8147(15) . ? P1 C16 1.8247(16) . ? N1 C1 1.409(2) . ? C1 C6 1.407(2) . ? C1 C2 1.412(2) . ? C2 C3 1.396(2) . ? C2 C7 1.504(2) . ? C3 C4 1.383(3) . ? C4 C5 1.381(3) . ? C4 C8 1.516(3) . ? C5 C6 1.392(2) . ? C6 C9 1.506(2) . ? C10 C11 1.396(2) . ? C10 C15 1.397(2) . ? C11 C12 1.388(2) . ? C12 C13 1.382(2) . ? C13 C14 1.385(2) . ? C14 C15 1.389(2) . ? C16 C21 1.391(2) . ? C16 C17 1.401(2) . ? C17 C18 1.389(3) . ? C18 C19 1.383(3) . ? C19 C20 1.382(3) . ? C20 C21 1.389(2) . ? C22 C23 1.509(2) . ? C23 C28 1.386(2) . ? C23 C24 1.389(2) . ? C24 C25 1.385(2) . ? C25 C26 1.394(2) . ? C26 C27 1.388(2) . ? C26 C29 1.531(2) . ? C27 C28 1.395(2) . ? C29 C31 1.526(2) . ? C29 C32 1.532(2) . ? C29 C30 1.534(2) . ? 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 P1 C10 115.24(7) . . ? N1 P1 C22 110.62(7) . . ? C10 P1 C22 105.77(7) . . ? N1 P1 C16 113.87(7) . . ? C10 P1 C16 105.26(7) . . ? C22 P1 C16 105.27(7) . . ? C1 N1 P1 127.14(10) . . ? C6 C1 N1 121.06(14) . . ? C6 C1 C2 118.56(14) . . ? N1 C1 C2 120.27(14) . . ? C3 C2 C1 119.08(15) . . ? C3 C2 C7 119.91(15) . . ? C1 C2 C7 120.99(15) . . ? C4 C3 C2 122.68(16) . . ? C5 C4 C3 117.51(16) . . ? C5 C4 C8 121.01(19) . . ? C3 C4 C8 121.48(18) . . ? C4 C5 C6 122.27(16) . . ? C5 C6 C1 119.86(15) . . ? C5 C6 C9 119.45(15) . . ? C1 C6 C9 120.68(14) . . ? C11 C10 C15 119.15(14) . . ? C11 C10 P1 122.52(12) . . ? C15 C10 P1 118.17(12) . . ? C12 C11 C10 119.93(15) . . ? C13 C12 C11 120.40(16) . . ? C12 C13 C14 120.29(15) . . ? C13 C14 C15 119.67(15) . . ? C14 C15 C10 120.52(15) . . ? C21 C16 C17 118.79(15) . . ? C21 C16 P1 123.97(12) . . ? C17 C16 P1 117.21(13) . . ? C18 C17 C16 120.27(17) . . ? C19 C18 C17 120.17(18) . . ? C20 C19 C18 120.06(17) . . ? C19 C20 C21 120.10(17) . . ? C20 C21 C16 120.59(16) . . ? C23 C22 P1 114.79(11) . . ? C28 C23 C24 117.71(14) . . ? C28 C23 C22 121.98(15) . . ? C24 C23 C22 120.31(14) . . ? C25 C24 C23 121.13(15) . . ? C24 C25 C26 121.65(15) . . ? C27 C26 C25 116.99(14) . . ? C27 C26 C29 123.49(14) . . ? C25 C26 C29 119.51(14) . . ? C26 C27 C28 121.48(14) . . ? C23 C28 C27 121.03(14) . . ? C31 C29 C26 112.12(13) . . ? C31 C29 C32 108.73(15) . . ? C26 C29 C32 109.11(13) . . ? C31 C29 C30 108.14(14) . . ? C26 C29 C30 109.72(13) . . ? C32 C29 C30 108.97(14) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.276 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.039 #==END data_msp125a _database_code_CSD 165392 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H52 N4 P Zr' _chemical_formula_weight 687.03 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' 'P' 'P' 0.1023 0.0942 '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 10.6664(6) _cell_length_b 13.6098(5) _cell_length_c 14.1992(8) _cell_angle_alpha 92.661(3) _cell_angle_beta 111.753(3) _cell_angle_gamma 104.507(3) _cell_volume 1831.08(16) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 726 _exptl_absorpt_coefficient_mu 0.374 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8928 _exptl_absorpt_correction_T_max 0.9707 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17202 _diffrn_reflns_av_R_equivalents 0.0658 _diffrn_reflns_av_sigmaI/netI 0.0697 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7079 _reflns_number_gt 6024 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'WC (Thornton-Pett, 2000)' _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^)+(0.0835P)^2^+1.1427P] 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 7079 _refine_ls_number_parameters 409 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1502 _refine_ls_wR_factor_gt 0.1392 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 Zr1 Zr 0.74174(3) 0.81720(2) 0.70715(2) 0.03421(13) Uani 1 1 d . . . N1 N 0.8964(3) 0.72309(19) 0.7437(2) 0.0339(5) Uani 1 1 d . . . C11 C 0.8753(3) 0.6170(2) 0.7569(2) 0.0345(6) Uani 1 1 d . . . C12 C 0.8661(3) 0.5882(2) 0.8487(2) 0.0382(7) Uani 1 1 d . . . C13 C 0.8338(4) 0.4849(3) 0.8585(3) 0.0437(8) Uani 1 1 d . . . H13 H 0.8297 0.4661 0.9211 0.052 Uiso 1 1 calc R . . C14 C 0.8074(4) 0.4080(2) 0.7800(3) 0.0430(8) Uani 1 1 d . . . C15 C 0.8195(4) 0.4381(2) 0.6908(3) 0.0407(7) Uani 1 1 d . . . H15 H 0.8039 0.3867 0.6368 0.049 Uiso 1 1 calc R . . C16 C 0.8538(3) 0.5408(2) 0.6776(3) 0.0370(7) Uani 1 1 d . . . C17 C 0.8900(5) 0.6682(3) 0.9354(3) 0.0496(9) Uani 1 1 d . . . H17A H 0.8071 0.6934 0.9187 0.074 Uiso 1 1 calc R . . H17B H 0.9729 0.7256 0.9456 0.074 Uiso 1 1 calc R . . H17C H 0.9057 0.6377 0.9985 0.074 Uiso 1 1 calc R . . C18 C 0.7658(4) 0.2957(3) 0.7914(3) 0.0505(9) Uani 1 1 d . . . H18A H 0.8146 0.2876 0.8628 0.076 Uiso 1 1 calc R . . H18B H 0.7921 0.2554 0.7466 0.076 Uiso 1 1 calc R . . H18C H 0.6636 0.2713 0.7719 0.076 Uiso 1 1 calc R . . C19 C 0.8654(4) 0.5673(3) 0.5783(3) 0.0448(8) Uani 1 1 d . . . H19A H 0.9650 0.5936 0.5897 0.067 Uiso 1 1 calc R . . H19B H 0.8178 0.6200 0.5548 0.067 Uiso 1 1 calc R . . H19C H 0.8208 0.5057 0.5261 0.067 Uiso 1 1 calc R . . P1 P 1.04643(8) 0.80735(6) 0.76482(6) 0.03201(19) Uani 1 1 d . . . C111 C 1.1943(3) 0.7872(2) 0.8700(2) 0.0347(6) Uani 1 1 d . . . C112 C 1.2158(4) 0.6908(2) 0.8837(3) 0.0417(7) Uani 1 1 d . . . H112 H 1.1488 0.6308 0.8391 0.050 Uiso 1 1 calc R . . C113 C 1.3363(4) 0.6835(3) 0.9633(3) 0.0486(8) Uani 1 1 d . . . H113 H 1.3506 0.6181 0.9741 0.058 Uiso 1 1 calc R . . C114 C 1.4358(4) 0.7714(3) 1.0271(3) 0.0505(9) Uani 1 1 d . . . H114 H 1.5195 0.7662 1.0797 0.061 Uiso 1 1 calc R . . C115 C 1.4134(4) 0.8662(3) 1.0143(3) 0.0453(8) Uani 1 1 d . . . H115 H 1.4807 0.9260 1.0590 0.054 Uiso 1 1 calc R . . C116 C 1.2933(3) 0.8742(2) 0.9366(3) 0.0383(7) Uani 1 1 d . . . H116 H 1.2780 0.9397 0.9284 0.046 Uiso 1 1 calc R . . C121 C 1.1013(3) 0.8072(2) 0.6584(2) 0.0355(6) Uani 1 1 d . . . C122 C 1.2238(4) 0.7837(3) 0.6655(3) 0.0418(7) Uani 1 1 d . . . H122 H 1.2829 0.7689 0.7286 0.050 Uiso 1 1 calc R . . C123 C 1.2610(4) 0.7815(3) 0.5819(3) 0.0465(8) Uani 1 1 d . . . H123 H 1.3439 0.7640 0.5873 0.056 Uiso 1 1 calc R . . C124 C 1.1769(4) 0.8050(3) 0.4907(3) 0.0467(8) Uani 1 1 d . . . H124 H 1.2018 0.8035 0.4331 0.056 Uiso 1 1 calc R . . C125 C 1.0554(4) 0.8308(3) 0.4831(3) 0.0446(8) Uani 1 1 d . . . H125 H 0.9988 0.8484 0.4206 0.054 Uiso 1 1 calc R . . C126 C 1.0169(4) 0.8311(2) 0.5656(3) 0.0411(7) Uani 1 1 d . . . H126 H 0.9330 0.8475 0.5595 0.049 Uiso 1 1 calc R . . C1 C 1.0032(3) 0.9189(2) 0.7854(2) 0.0345(6) Uani 1 1 d . . . C131 C 1.0749(3) 1.0255(2) 0.7786(2) 0.0335(6) Uani 1 1 d . . . C132 C 1.0317(4) 1.1060(2) 0.8099(3) 0.0391(7) Uani 1 1 d . . . H132 H 0.9574 1.0900 0.8334 0.047 Uiso 1 1 calc R . . C133 C 1.0932(4) 1.2075(2) 0.8078(3) 0.0391(7) Uani 1 1 d . . . H133 H 1.0609 1.2591 0.8308 0.047 Uiso 1 1 calc R . . C134 C 1.2019(3) 1.2368(2) 0.7729(2) 0.0361(7) Uani 1 1 d . . . C135 C 1.2442(3) 1.1570(2) 0.7411(2) 0.0368(7) Uani 1 1 d . . . H135 H 1.3170 1.1730 0.7162 0.044 Uiso 1 1 calc R . . C136 C 1.1841(3) 1.0549(2) 0.7445(2) 0.0361(6) Uani 1 1 d . . . H136 H 1.2180 1.0035 0.7230 0.043 Uiso 1 1 calc R . . C137 C 1.2667(4) 1.3503(2) 0.7710(3) 0.0424(7) Uani 1 1 d . . . C138 C 1.3378(5) 1.4096(3) 0.8801(3) 0.0588(10) Uani 1 1 d . . . H13A H 1.2665 1.4083 0.9084 0.088 Uiso 1 1 calc R . . H13B H 1.3852 1.4810 0.8789 0.088 Uiso 1 1 calc R . . H13C H 1.4072 1.3777 0.9230 0.088 Uiso 1 1 calc R . . C139 C 1.3753(6) 1.3637(3) 0.7234(5) 0.0781(16) Uani 1 1 d . . . H13D H 1.4103 1.4365 0.7193 0.117 Uiso 1 1 calc R . . H13E H 1.3315 1.3237 0.6543 0.117 Uiso 1 1 calc R . . H13F H 1.4541 1.3395 0.7659 0.117 Uiso 1 1 calc R . . C140 C 1.1515(5) 1.3978(3) 0.7084(4) 0.0688(13) Uani 1 1 d . . . H14A H 1.0795 1.3886 0.7372 0.103 Uiso 1 1 calc R . . H14B H 1.1080 1.3638 0.6369 0.103 Uiso 1 1 calc R . . H14C H 1.1934 1.4712 0.7113 0.103 Uiso 1 1 calc R . . N2 N 0.6627(3) 0.8507(2) 0.5613(2) 0.0420(6) Uani 1 1 d . . . C21 C 0.5382(4) 0.7992(3) 0.4695(3) 0.0525(9) Uani 1 1 d . . . H21A H 0.4702 0.8390 0.4553 0.079 Uiso 1 1 calc R . . H21B H 0.4952 0.7304 0.4803 0.079 Uiso 1 1 calc R . . H21C H 0.5653 0.7934 0.4111 0.079 Uiso 1 1 calc R . . C22 C 0.7279(4) 0.9529(3) 0.5461(3) 0.0548(9) Uani 1 1 d . . . H22A H 0.7589 0.9471 0.4896 0.082 Uiso 1 1 calc R . . H22B H 0.8094 0.9880 0.6091 0.082 Uiso 1 1 calc R . . H22C H 0.6593 0.9924 0.5292 0.082 Uiso 1 1 calc R . . N3 N 0.7074(3) 0.9156(2) 0.8024(2) 0.0459(7) Uani 1 1 d . . . C31 C 0.7693(5) 0.9274(3) 0.9142(3) 0.0584(10) Uani 1 1 d . . . H31A H 0.8209 0.9997 0.9425 0.088 Uiso 1 1 calc R . . H31B H 0.8342 0.8853 0.9358 0.088 Uiso 1 1 calc R . . H31C H 0.6943 0.9052 0.9394 0.088 Uiso 1 1 calc R . . C32 C 0.6154(5) 0.9805(3) 0.7674(4) 0.0638(11) Uani 1 1 d . . . H32A H 0.5387 0.9613 0.7914 0.096 Uiso 1 1 calc R . . H32B H 0.5759 0.9715 0.6923 0.096 Uiso 1 1 calc R . . H32C H 0.6695 1.0525 0.7951 0.096 Uiso 1 1 calc R . . N4 N 0.5855(3) 0.6881(2) 0.6996(2) 0.0425(6) Uani 1 1 d . . . C41 C 0.5502(4) 0.5968(3) 0.6265(3) 0.0514(9) Uani 1 1 d . . . H41A H 0.5762 0.5413 0.6637 0.077 Uiso 1 1 calc R . . H41B H 0.6018 0.6123 0.5820 0.077 Uiso 1 1 calc R . . H41C H 0.4486 0.5754 0.5846 0.077 Uiso 1 1 calc R . . C42 C 0.5151(4) 0.6669(3) 0.7697(4) 0.0544(10) Uani 1 1 d . . . H42A H 0.4132 0.6393 0.7303 0.082 Uiso 1 1 calc R . . H42B H 0.5348 0.7305 0.8146 0.082 Uiso 1 1 calc R . . H42C H 0.5498 0.6164 0.8113 0.082 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 0.03220(19) 0.03055(18) 0.0377(2) 0.00355(12) 0.01314(14) 0.00667(12) N1 0.0337(13) 0.0311(12) 0.0328(13) 0.0020(10) 0.0116(11) 0.0054(10) C11 0.0339(16) 0.0313(14) 0.0344(16) 0.0037(12) 0.0110(13) 0.0071(12) C12 0.0388(17) 0.0386(16) 0.0329(16) 0.0021(13) 0.0123(14) 0.0076(13) C13 0.049(2) 0.0409(17) 0.0404(18) 0.0113(14) 0.0181(16) 0.0104(14) C14 0.0405(18) 0.0342(16) 0.051(2) 0.0091(14) 0.0143(16) 0.0101(13) C15 0.0397(18) 0.0343(16) 0.0403(18) -0.0011(13) 0.0103(14) 0.0075(13) C16 0.0326(16) 0.0372(16) 0.0368(17) 0.0039(12) 0.0108(13) 0.0077(12) C17 0.064(2) 0.0431(18) 0.0391(19) 0.0024(14) 0.0223(18) 0.0081(16) C18 0.051(2) 0.0371(18) 0.058(2) 0.0117(15) 0.0161(18) 0.0112(15) C19 0.054(2) 0.0398(17) 0.0366(18) -0.0013(13) 0.0194(16) 0.0055(15) P1 0.0313(4) 0.0301(4) 0.0303(4) 0.0023(3) 0.0093(3) 0.0064(3) C111 0.0334(16) 0.0371(15) 0.0308(15) 0.0018(12) 0.0111(13) 0.0084(12) C112 0.0394(18) 0.0358(16) 0.0442(19) 0.0019(13) 0.0127(15) 0.0080(13) C113 0.047(2) 0.0394(18) 0.050(2) 0.0070(15) 0.0073(17) 0.0142(15) C114 0.046(2) 0.052(2) 0.042(2) 0.0072(16) 0.0034(16) 0.0175(16) C115 0.0424(19) 0.0433(18) 0.0362(18) -0.0020(14) 0.0049(15) 0.0066(14) C116 0.0386(17) 0.0350(16) 0.0362(17) 0.0016(12) 0.0107(14) 0.0088(13) C121 0.0372(16) 0.0319(15) 0.0338(16) 0.0033(12) 0.0124(13) 0.0069(12) C122 0.0414(18) 0.0478(18) 0.0369(17) 0.0085(14) 0.0142(15) 0.0158(14) C123 0.050(2) 0.051(2) 0.050(2) 0.0099(16) 0.0279(17) 0.0189(16) C124 0.053(2) 0.0475(19) 0.0395(19) 0.0033(14) 0.0223(17) 0.0081(16) C125 0.048(2) 0.0460(18) 0.0309(17) 0.0036(13) 0.0109(15) 0.0068(15) C126 0.0413(18) 0.0408(17) 0.0372(17) 0.0038(13) 0.0128(14) 0.0096(14) C1 0.0347(16) 0.0311(15) 0.0328(15) 0.0022(11) 0.0093(13) 0.0077(12) C131 0.0324(15) 0.0318(14) 0.0299(15) 0.0014(11) 0.0075(12) 0.0066(12) C132 0.0370(17) 0.0378(16) 0.0409(18) 0.0019(13) 0.0160(14) 0.0079(13) C133 0.0385(17) 0.0333(15) 0.0428(18) -0.0001(13) 0.0145(14) 0.0091(13) C134 0.0373(16) 0.0326(15) 0.0317(16) 0.0030(12) 0.0085(13) 0.0067(12) C135 0.0360(16) 0.0364(15) 0.0353(16) 0.0052(12) 0.0130(13) 0.0078(13) C136 0.0352(16) 0.0343(15) 0.0357(16) 0.0035(12) 0.0102(13) 0.0110(12) C137 0.0437(18) 0.0314(15) 0.049(2) 0.0054(13) 0.0166(16) 0.0081(13) C138 0.060(2) 0.0344(18) 0.062(3) -0.0029(16) 0.010(2) 0.0021(16) C139 0.099(4) 0.038(2) 0.130(5) 0.018(2) 0.084(4) 0.014(2) C140 0.063(3) 0.040(2) 0.081(3) 0.021(2) 0.006(2) 0.0117(18) N2 0.0383(15) 0.0424(15) 0.0416(15) 0.0070(12) 0.0133(13) 0.0093(12) C21 0.048(2) 0.063(2) 0.041(2) 0.0044(16) 0.0142(17) 0.0128(17) C22 0.048(2) 0.049(2) 0.057(2) 0.0159(17) 0.0115(18) 0.0100(16) N3 0.0435(16) 0.0426(15) 0.0553(18) 0.0026(13) 0.0253(15) 0.0106(12) C31 0.065(3) 0.061(2) 0.054(2) -0.0021(18) 0.033(2) 0.0145(19) C32 0.061(3) 0.062(2) 0.072(3) 0.002(2) 0.026(2) 0.026(2) N4 0.0345(14) 0.0366(14) 0.0560(18) 0.0065(12) 0.0203(13) 0.0062(11) C41 0.0419(19) 0.0376(17) 0.066(2) -0.0006(16) 0.0168(18) 0.0054(14) C42 0.049(2) 0.0444(19) 0.080(3) 0.0162(18) 0.037(2) 0.0121(16) _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 N2 2.048(3) . ? Zr1 N3 2.049(3) . ? Zr1 N4 2.064(3) . ? Zr1 N1 2.262(3) . ? Zr1 C1 2.560(3) . ? Zr1 P1 3.0832(9) . ? N1 C11 1.436(4) . ? N1 P1 1.631(3) . ? C11 C16 1.406(5) . ? C11 C12 1.409(4) . ? C12 C13 1.389(5) . ? C12 C17 1.507(5) . ? C13 C14 1.388(5) . ? C14 C15 1.390(5) . ? C14 C18 1.515(5) . ? C15 C16 1.393(4) . ? C16 C19 1.513(5) . ? P1 C1 1.735(3) . ? P1 C121 1.811(3) . ? P1 C111 1.817(3) . ? C111 C116 1.394(4) . ? C111 C112 1.397(4) . ? C112 C113 1.392(5) . ? C113 C114 1.389(5) . ? C114 C115 1.378(5) . ? C115 C116 1.380(5) . ? C121 C122 1.390(5) . ? C121 C126 1.401(5) . ? C122 C123 1.385(5) . ? C123 C124 1.380(5) . ? C124 C125 1.394(5) . ? C125 C126 1.378(5) . ? C1 C131 1.487(4) . ? C131 C136 1.397(5) . ? C131 C132 1.403(4) . ? C132 C133 1.380(4) . ? C133 C134 1.400(5) . ? C134 C135 1.391(5) . ? C134 C137 1.533(4) . ? C135 C136 1.388(4) . ? C137 C139 1.523(5) . ? C137 C138 1.528(5) . ? C137 C140 1.535(5) . ? N2 C21 1.456(5) . ? N2 C22 1.457(5) . ? N3 C32 1.450(5) . ? N3 C31 1.459(5) . ? N4 C42 1.453(5) . ? N4 C41 1.455(5) . ? 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 N2 Zr1 N3 108.27(12) . . ? N2 Zr1 N4 101.37(12) . . ? N3 Zr1 N4 97.53(12) . . ? N2 Zr1 N1 118.54(11) . . ? N3 Zr1 N1 130.27(11) . . ? N4 Zr1 N1 89.26(10) . . ? N2 Zr1 C1 106.05(11) . . ? N3 Zr1 C1 88.67(11) . . ? N4 Zr1 C1 148.37(11) . . ? N1 Zr1 C1 63.93(9) . . ? N2 Zr1 P1 110.15(8) . . ? N3 Zr1 P1 117.58(9) . . ? N4 Zr1 P1 120.11(8) . . ? N1 Zr1 P1 30.94(6) . . ? C1 Zr1 P1 34.24(7) . . ? C11 N1 P1 126.5(2) . . ? C11 N1 Zr1 129.7(2) . . ? P1 N1 Zr1 103.56(12) . . ? C16 C11 C12 119.4(3) . . ? C16 C11 N1 121.4(3) . . ? C12 C11 N1 119.0(3) . . ? C13 C12 C11 119.3(3) . . ? C13 C12 C17 120.0(3) . . ? C11 C12 C17 120.7(3) . . ? C14 C13 C12 122.3(3) . . ? C13 C14 C15 117.5(3) . . ? C13 C14 C18 121.0(3) . . ? C15 C14 C18 121.5(3) . . ? C14 C15 C16 122.4(3) . . ? C15 C16 C11 119.0(3) . . ? C15 C16 C19 119.3(3) . . ? C11 C16 C19 121.7(3) . . ? N1 P1 C1 99.27(14) . . ? N1 P1 C121 114.52(14) . . ? C1 P1 C121 111.52(15) . . ? N1 P1 C111 113.39(14) . . ? C1 P1 C111 115.48(15) . . ? C121 P1 C111 103.19(15) . . ? N1 P1 Zr1 45.50(9) . . ? C1 P1 Zr1 56.13(11) . . ? C121 P1 Zr1 114.56(11) . . ? C111 P1 Zr1 141.81(10) . . ? C116 C111 C112 119.5(3) . . ? C116 C111 P1 117.0(2) . . ? C112 C111 P1 123.5(2) . . ? C113 C112 C111 119.4(3) . . ? C114 C113 C112 120.3(3) . . ? C115 C114 C113 120.2(3) . . ? C114 C115 C116 120.0(3) . . ? C115 C116 C111 120.6(3) . . ? C122 C121 C126 118.9(3) . . ? C122 C121 P1 122.4(2) . . ? C126 C121 P1 118.7(3) . . ? C123 C122 C121 121.0(3) . . ? C124 C123 C122 119.6(3) . . ? C123 C124 C125 120.1(3) . . ? C126 C125 C124 120.3(3) . . ? C125 C126 C121 120.0(3) . . ? C131 C1 P1 127.9(2) . . ? C131 C1 Zr1 130.5(2) . . ? P1 C1 Zr1 89.63(12) . . ? C136 C131 C132 115.6(3) . . ? C136 C131 C1 126.3(3) . . ? C132 C131 C1 118.1(3) . . ? C133 C132 C131 122.4(3) . . ? C132 C133 C134 122.0(3) . . ? C135 C134 C133 115.7(3) . . ? C135 C134 C137 123.9(3) . . ? C133 C134 C137 120.4(3) . . ? C136 C135 C134 122.5(3) . . ? C135 C136 C131 121.8(3) . . ? C139 C137 C138 108.9(4) . . ? C139 C137 C134 111.5(3) . . ? C138 C137 C134 109.9(3) . . ? C139 C137 C140 108.4(4) . . ? C138 C137 C140 107.8(3) . . ? C134 C137 C140 110.3(3) . . ? C21 N2 C22 110.0(3) . . ? C21 N2 Zr1 133.1(2) . . ? C22 N2 Zr1 116.1(2) . . ? C32 N3 C31 111.1(3) . . ? C32 N3 Zr1 124.5(3) . . ? C31 N3 Zr1 124.4(3) . . ? C42 N4 C41 111.0(3) . . ? C42 N4 Zr1 128.5(2) . . ? C41 N4 Zr1 119.8(2) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.121 _refine_diff_density_min -1.086 _refine_diff_density_rms 0.092