Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 #==================================================================== # 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.' _publ_contact_letter ; The following set of data is for the four compounds included m/s B009082O which was recently submitted to you. ; #======================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Mono- and bidentate trimethylsilyliminophosphines and their reactivity towards titanium and zirconium halides ; loop_ _publ_author_name _publ_author_address 'Mark J. Sarsfield' ; School of Chemical Sciences University of East Anglia Norwich NR4 7TJ UK ; 'Musa Said' ; School of Chemical Sciences University of East Anglia Norwich NR4 7TJ UK ; 'Mark Thornton-Pett' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Lee Gerrard' ; School of Chemical Sciences University of East Anglia Norwich NR4 7TJ UK ; 'Manfred Bochmann' ; School of Chemical Sciences University of East Anglia Norwich NR4 7TJ UK ; #================================================================= data_ms335 _database_code_CSD 154069 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H55 Cl6 N3 P2 Ti2' _chemical_formula_weight 1068.41 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Ti' 'Ti' 0.2776 0.4457 '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 12.0929(2) _cell_length_b 13.4161(4) _cell_length_c 16.3861(4) _cell_angle_alpha 84.4990(14) _cell_angle_beta 80.9110(17) _cell_angle_gamma 81.7870(16) _cell_volume 2590.85(11) _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 prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.716 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6651 _exptl_absorpt_correction_T_max 0.9254 _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 33684 _diffrn_reflns_av_R_equivalents 0.0595 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10152 _reflns_number_gt 8694 _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^)+(0.0587P)^2^+2.8962P] 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 0.0024(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 10152 _refine_ls_number_parameters 579 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0571 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1314 _refine_ls_wR_factor_gt 0.1238 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.045 _refine_ls_shift/su_mean 0.001 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 Ti1 Ti 0.24594(4) 0.12048(3) 0.34153(3) 0.02538(13) Uani 1 1 d . . . Cl1 Cl 0.43056(6) 0.12028(6) 0.35677(5) 0.04448(19) Uani 1 1 d . . . Cl2 Cl 0.18096(6) 0.29038(5) 0.32364(4) 0.03912(18) Uani 1 1 d . . . C1 C 0.2329(2) 0.0313(2) 0.47698(16) 0.0370(6) Uani 1 1 d . . . C2 C 0.2088(3) -0.0303(2) 0.41760(16) 0.0355(6) Uani 1 1 d . . . C3 C 0.1075(2) 0.0143(2) 0.38974(16) 0.0353(6) Uani 1 1 d . . . C4 C 0.0716(2) 0.1045(2) 0.42870(17) 0.0358(6) Uani 1 1 d . . . C5 C 0.1489(2) 0.1157(2) 0.48262(16) 0.0349(6) Uani 1 1 d . . . C6 C 0.3271(3) 0.0050(3) 0.5278(2) 0.0605(10) Uani 1 1 d . . . H6A H 0.3023 -0.0382 0.5771 0.091 Uiso 1 1 calc R . . H6B H 0.3479 0.0669 0.5449 0.091 Uiso 1 1 calc R . . H6C H 0.3926 -0.0311 0.4947 0.091 Uiso 1 1 calc R . . C7 C 0.2770(3) -0.1293(2) 0.3938(2) 0.0537(9) Uani 1 1 d . . . H7A H 0.2574 -0.1830 0.4362 0.081 Uiso 1 1 calc R . . H7B H 0.3577 -0.1236 0.3893 0.081 Uiso 1 1 calc R . . H7C H 0.2603 -0.1454 0.3403 0.081 Uiso 1 1 calc R . . C8 C 0.0441(3) -0.0282(3) 0.3322(2) 0.0566(10) Uani 1 1 d . . . H8A H 0.0971 -0.0722 0.2954 0.085 Uiso 1 1 calc R . . H8B H 0.0062 0.0271 0.2991 0.085 Uiso 1 1 calc R . . H8C H -0.0123 -0.0675 0.3648 0.085 Uiso 1 1 calc R . . C9 C -0.0360(3) 0.1736(3) 0.4195(3) 0.0614(10) Uani 1 1 d . . . H9A H -0.0488 0.1791 0.3615 0.092 Uiso 1 1 calc R . . H9B H -0.0297 0.2407 0.4360 0.092 Uiso 1 1 calc R . . H9C H -0.0995 0.1462 0.4549 0.092 Uiso 1 1 calc R . . C10 C 0.1431(4) 0.2026(3) 0.5350(2) 0.0624(10) Uani 1 1 d . . . H10A H 0.1453 0.2654 0.4994 0.094 Uiso 1 1 calc R . . H10B H 0.2075 0.1920 0.5658 0.094 Uiso 1 1 calc R . . H10C H 0.0726 0.2069 0.5741 0.094 Uiso 1 1 calc R . . N1 N 0.25738(19) 0.08167(17) 0.23844(13) 0.0303(5) Uani 1 1 d . . . P1 P 0.23800(5) 0.09380(5) 0.14484(4) 0.02573(16) Uani 1 1 d . . . C111 C 0.0900(2) 0.1140(2) 0.13439(15) 0.0281(5) Uani 1 1 d . . . C112 C 0.0376(2) 0.0433(2) 0.10213(16) 0.0343(6) Uani 1 1 d . . . H112 H 0.0810 -0.0153 0.0799 0.041 Uiso 1 1 calc R . . C113 C -0.0787(3) 0.0596(3) 0.10283(18) 0.0415(7) Uani 1 1 d . . . H113 H -0.1150 0.0116 0.0815 0.050 Uiso 1 1 calc R . . C114 C -0.1417(2) 0.1449(3) 0.13429(18) 0.0414(7) Uani 1 1 d . . . H114 H -0.2211 0.1553 0.1346 0.050 Uiso 1 1 calc R . . C115 C -0.0896(2) 0.2157(2) 0.16556(18) 0.0390(6) Uani 1 1 d . . . H115 H -0.1332 0.2748 0.1867 0.047 Uiso 1 1 calc R . . C116 C 0.0260(2) 0.1998(2) 0.16585(16) 0.0336(6) Uani 1 1 d . . . H116 H 0.0616 0.2479 0.1877 0.040 Uiso 1 1 calc R . . C121 C 0.3007(2) -0.0141(2) 0.08867(15) 0.0287(5) Uani 1 1 d . . . C122 C 0.3005(3) -0.1087(2) 0.13246(18) 0.0399(7) Uani 1 1 d . . . H122 H 0.2746 -0.1131 0.1904 0.048 Uiso 1 1 calc R . . C123 C 0.3374(3) -0.1960(2) 0.0924(2) 0.0460(7) Uani 1 1 d . . . H123 H 0.3353 -0.2601 0.1223 0.055 Uiso 1 1 calc R . . C124 C 0.3776(3) -0.1895(2) 0.0083(2) 0.0432(7) Uani 1 1 d . . . H124 H 0.4029 -0.2493 -0.0196 0.052 Uiso 1 1 calc R . . C125 C 0.3811(3) -0.0970(3) -0.03492(19) 0.0438(7) Uani 1 1 d . . . H125 H 0.4104 -0.0933 -0.0923 0.053 Uiso 1 1 calc R . . C126 C 0.3421(2) -0.0086(2) 0.00426(17) 0.0368(6) Uani 1 1 d . . . H126 H 0.3438 0.0551 -0.0263 0.044 Uiso 1 1 calc R . . C11 C 0.2912(2) 0.2064(2) 0.09064(14) 0.0260(5) Uani 1 1 d . . . N12 N 0.25935(17) 0.23026(17) 0.01574(12) 0.0272(5) Uani 1 1 d . . . C13 C 0.2923(2) 0.3139(2) -0.02697(15) 0.0271(5) Uani 1 1 d . . . C14 C 0.3560(2) 0.3767(2) 0.00282(16) 0.0300(6) Uani 1 1 d . . . H14 H 0.3780 0.4353 -0.0294 0.036 Uiso 1 1 calc R . . C15 C 0.3868(2) 0.3516(2) 0.08099(16) 0.0307(6) Uani 1 1 d . . . H15 H 0.4292 0.3936 0.1037 0.037 Uiso 1 1 calc R . . C16 C 0.3553(2) 0.2648(2) 0.12538(15) 0.0286(5) Uani 1 1 d . . . H16 H 0.3769 0.2454 0.1785 0.034 Uiso 1 1 calc R . . Ti2 Ti 0.39420(4) 0.50450(4) -0.24386(3) 0.02708(13) Uani 1 1 d . . . Cl3 Cl 0.56737(6) 0.43708(6) -0.20624(4) 0.03992(18) Uani 1 1 d . . . Cl4 Cl 0.36671(6) 0.65200(6) -0.17773(5) 0.04330(19) Uani 1 1 d . . . C21 C 0.3679(3) 0.6141(2) -0.36566(17) 0.0388(7) Uani 1 1 d . . . C22 C 0.2908(3) 0.5444(3) -0.35455(18) 0.0426(7) Uani 1 1 d . . . C23 C 0.3490(3) 0.4492(3) -0.36442(16) 0.0457(8) Uani 1 1 d . . . C24 C 0.4689(3) 0.4573(3) -0.37961(17) 0.0466(8) Uani 1 1 d . . . C25 C 0.4766(2) 0.5625(2) -0.38074(16) 0.0343(6) Uani 1 1 d . . . C26 C 0.3387(3) 0.7276(3) -0.3684(2) 0.0503(8) Uani 1 1 d . . . H26A H 0.3307 0.7541 -0.4253 0.075 Uiso 1 1 calc R . . H26B H 0.3990 0.7572 -0.3497 0.075 Uiso 1 1 calc R . . H26C H 0.2675 0.7450 -0.3319 0.075 Uiso 1 1 calc R . . C27 C 0.1624(3) 0.5680(3) -0.3413(2) 0.0595(10) Uani 1 1 d . . . H27A H 0.1355 0.5811 -0.3952 0.089 Uiso 1 1 calc R . . H27B H 0.1398 0.6278 -0.3096 0.089 Uiso 1 1 calc R . . H27C H 0.1295 0.5103 -0.3107 0.089 Uiso 1 1 calc R . . C28 C 0.2991(4) 0.3521(3) -0.3657(2) 0.0718(13) Uani 1 1 d . . . H28A H 0.2278 0.3541 -0.3276 0.108 Uiso 1 1 calc R . . H28B H 0.3521 0.2946 -0.3484 0.108 Uiso 1 1 calc R . . H28C H 0.2850 0.3447 -0.4220 0.108 Uiso 1 1 calc R . . C29 C 0.5629(4) 0.3751(3) -0.3980(2) 0.0635(10) Uani 1 1 d . . . H29A H 0.5495 0.3155 -0.3602 0.095 Uiso 1 1 calc R . . H29B H 0.6341 0.3974 -0.3906 0.095 Uiso 1 1 calc R . . H29C H 0.5672 0.3580 -0.4553 0.095 Uiso 1 1 calc R . . C30 C 0.5859(3) 0.6073(3) -0.3952(2) 0.0512(8) Uani 1 1 d . . . H30A H 0.5715 0.6792 -0.4130 0.077 Uiso 1 1 calc R . . H30B H 0.6385 0.5723 -0.4384 0.077 Uiso 1 1 calc R . . H30C H 0.6190 0.5995 -0.3437 0.077 Uiso 1 1 calc R . . N2 N 0.2992(2) 0.42880(19) -0.17964(13) 0.0358(5) Uani 1 1 d . . . P2 P 0.24138(6) 0.34052(5) -0.12683(4) 0.02887(17) Uani 1 1 d . . . C211 C 0.2755(2) 0.2217(2) -0.17330(15) 0.0303(6) Uani 1 1 d . . . C212 C 0.1979(2) 0.1766(2) -0.20700(17) 0.0362(6) Uani 1 1 d . . . H212 H 0.1212 0.2063 -0.2029 0.043 Uiso 1 1 calc R . . C213 C 0.2327(3) 0.0883(2) -0.24652(18) 0.0407(7) Uani 1 1 d . . . H213 H 0.1796 0.0577 -0.2694 0.049 Uiso 1 1 calc R . . C214 C 0.3433(3) 0.0444(3) -0.25295(18) 0.0428(7) Uani 1 1 d . . . H214 H 0.3662 -0.0165 -0.2798 0.051 Uiso 1 1 calc R . . C215 C 0.4215(3) 0.0892(3) -0.22017(17) 0.0435(7) Uani 1 1 d . . . H215 H 0.4981 0.0592 -0.2248 0.052 Uiso 1 1 calc R . . C216 C 0.3879(2) 0.1774(2) -0.18076(16) 0.0382(7) Uani 1 1 d . . . H216 H 0.4416 0.2081 -0.1587 0.046 Uiso 1 1 calc R . . C221 C 0.0901(2) 0.3701(2) -0.10267(15) 0.0319(6) Uani 1 1 d . . . C222 C 0.0223(2) 0.3000(2) -0.06050(17) 0.0368(6) Uani 1 1 d . . . H222 H 0.0551 0.2341 -0.0437 0.044 Uiso 1 1 calc R . . C223 C -0.0940(3) 0.3277(3) -0.0434(2) 0.0457(7) Uani 1 1 d . . . H223 H -0.1408 0.2803 -0.0153 0.055 Uiso 1 1 calc R . . C224 C -0.1413(3) 0.4235(3) -0.0671(2) 0.0533(8) Uani 1 1 d . . . H224 H -0.2208 0.4414 -0.0561 0.064 Uiso 1 1 calc R . . C225 C -0.0744(3) 0.4937(3) -0.1065(2) 0.0529(8) Uani 1 1 d . . . H225 H -0.1076 0.5602 -0.1213 0.063 Uiso 1 1 calc R . . C226 C 0.0413(3) 0.4676(2) -0.12459(19) 0.0420(7) Uani 1 1 d . . . H226 H 0.0874 0.5160 -0.1519 0.050 Uiso 1 1 calc R . . C1S C 0.1335(3) 0.5662(3) 0.3151(2) 0.0590(9) Uani 1 1 d . . . H1SA H 0.0925 0.5201 0.2910 0.071 Uiso 1 1 calc R . . H1SB H 0.2154 0.5453 0.2996 0.071 Uiso 1 1 calc R . . Cl1S Cl 0.09976(13) 0.55501(11) 0.42242(7) 0.0975(4) Uani 1 1 d . . . Cl2S Cl 0.09870(12) 0.68989(9) 0.27312(7) 0.0855(4) Uani 1 1 d . . . 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 Ti1 0.0269(2) 0.0300(3) 0.0193(2) -0.00317(17) -0.00229(17) -0.00402(18) Cl1 0.0298(4) 0.0575(5) 0.0492(4) -0.0110(3) -0.0078(3) -0.0090(3) Cl2 0.0459(4) 0.0308(4) 0.0374(4) -0.0018(3) 0.0015(3) -0.0028(3) C1 0.0396(16) 0.0505(18) 0.0200(12) 0.0039(11) -0.0043(11) -0.0078(13) C2 0.0468(16) 0.0334(15) 0.0219(12) 0.0017(11) 0.0043(11) -0.0028(12) C3 0.0404(15) 0.0422(16) 0.0250(13) 0.0034(11) -0.0031(11) -0.0163(13) C4 0.0291(14) 0.0412(16) 0.0323(14) 0.0084(12) 0.0025(11) -0.0036(12) C5 0.0434(16) 0.0380(16) 0.0215(12) -0.0036(11) 0.0058(11) -0.0106(12) C6 0.063(2) 0.083(3) 0.0376(18) 0.0114(17) -0.0232(16) -0.010(2) C7 0.072(2) 0.0386(18) 0.0402(17) 0.0028(14) 0.0075(16) 0.0055(16) C8 0.068(2) 0.077(3) 0.0359(17) 0.0034(16) -0.0120(15) -0.044(2) C9 0.0326(17) 0.070(3) 0.068(2) 0.0205(19) 0.0066(15) 0.0045(16) C10 0.098(3) 0.054(2) 0.0335(17) -0.0139(15) 0.0096(17) -0.019(2) N1 0.0329(12) 0.0358(13) 0.0221(10) -0.0013(9) -0.0042(8) -0.0045(9) P1 0.0275(3) 0.0314(4) 0.0182(3) -0.0031(2) -0.0024(2) -0.0038(3) C111 0.0280(13) 0.0375(15) 0.0192(11) 0.0001(10) -0.0019(9) -0.0081(11) C112 0.0353(15) 0.0405(16) 0.0281(13) -0.0062(11) -0.0032(11) -0.0074(12) C113 0.0362(16) 0.0551(19) 0.0373(15) -0.0053(13) -0.0061(12) -0.0174(14) C114 0.0252(14) 0.061(2) 0.0383(16) -0.0032(14) -0.0023(11) -0.0074(13) C115 0.0312(15) 0.0451(17) 0.0385(15) -0.0058(13) -0.0016(11) -0.0001(12) C116 0.0342(14) 0.0372(15) 0.0300(13) -0.0045(11) -0.0044(11) -0.0060(12) C121 0.0273(13) 0.0350(14) 0.0247(12) -0.0087(10) -0.0049(10) -0.0014(11) C122 0.0492(17) 0.0384(16) 0.0303(14) -0.0038(12) -0.0064(12) 0.0020(13) C123 0.0546(19) 0.0362(17) 0.0475(18) -0.0036(13) -0.0156(14) 0.0031(14) C124 0.0353(16) 0.0446(18) 0.0514(18) -0.0216(14) -0.0096(13) 0.0049(13) C125 0.0394(16) 0.056(2) 0.0342(15) -0.0176(14) 0.0028(12) -0.0007(14) C126 0.0368(15) 0.0422(17) 0.0302(14) -0.0070(12) 0.0019(11) -0.0061(12) C11 0.0225(12) 0.0336(14) 0.0208(12) -0.0031(10) -0.0008(9) -0.0019(10) N12 0.0253(10) 0.0366(12) 0.0197(10) -0.0016(9) -0.0018(8) -0.0059(9) C13 0.0243(12) 0.0359(14) 0.0208(12) -0.0041(10) 0.0000(9) -0.0050(10) C14 0.0265(13) 0.0366(15) 0.0274(13) -0.0021(11) -0.0023(10) -0.0075(11) C15 0.0258(13) 0.0420(16) 0.0262(13) -0.0076(11) -0.0034(10) -0.0085(11) C16 0.0264(13) 0.0400(15) 0.0198(12) -0.0046(10) -0.0039(9) -0.0036(11) Ti2 0.0300(3) 0.0310(3) 0.0219(2) 0.00160(18) -0.00669(17) -0.00844(19) Cl3 0.0362(4) 0.0480(4) 0.0330(3) -0.0002(3) -0.0085(3) 0.0051(3) Cl4 0.0445(4) 0.0382(4) 0.0504(4) -0.0120(3) -0.0184(3) 0.0027(3) C21 0.0437(16) 0.0444(17) 0.0261(13) 0.0063(12) -0.0058(11) -0.0035(13) C22 0.0482(18) 0.054(2) 0.0285(14) 0.0049(13) -0.0153(12) -0.0096(15) C23 0.075(2) 0.054(2) 0.0172(13) 0.0030(12) -0.0111(13) -0.0358(18) C24 0.071(2) 0.0478(19) 0.0178(13) -0.0052(12) -0.0085(13) 0.0075(16) C25 0.0408(15) 0.0395(16) 0.0223(12) 0.0007(11) -0.0003(11) -0.0111(12) C26 0.052(2) 0.0448(19) 0.0502(19) 0.0055(15) -0.0076(15) 0.0011(15) C27 0.048(2) 0.087(3) 0.0475(19) 0.0113(18) -0.0171(15) -0.0195(19) C28 0.127(4) 0.068(3) 0.0363(18) 0.0006(17) -0.024(2) -0.054(3) C29 0.092(3) 0.052(2) 0.0421(19) -0.0135(16) -0.0057(18) 0.010(2) C30 0.0453(18) 0.062(2) 0.0451(18) 0.0030(16) 0.0005(14) -0.0165(16) N2 0.0425(13) 0.0441(14) 0.0231(11) 0.0022(10) -0.0056(9) -0.0159(11) P2 0.0303(4) 0.0379(4) 0.0201(3) 0.0008(3) -0.0044(2) -0.0114(3) C211 0.0335(14) 0.0403(15) 0.0175(11) 0.0005(10) -0.0021(10) -0.0101(11) C212 0.0346(15) 0.0448(17) 0.0308(14) -0.0017(12) -0.0062(11) -0.0100(12) C213 0.0479(18) 0.0451(18) 0.0333(15) -0.0057(13) -0.0099(12) -0.0139(14) C214 0.0500(18) 0.0487(19) 0.0284(14) -0.0089(13) -0.0015(12) -0.0028(14) C215 0.0356(15) 0.065(2) 0.0277(14) -0.0099(13) 0.0001(11) 0.0012(14) C216 0.0322(14) 0.0582(19) 0.0254(13) -0.0094(12) -0.0022(10) -0.0075(13) C221 0.0337(14) 0.0397(16) 0.0231(12) -0.0028(11) -0.0054(10) -0.0059(12) C222 0.0337(15) 0.0447(17) 0.0320(14) 0.0049(12) -0.0081(11) -0.0067(12) C223 0.0337(16) 0.060(2) 0.0425(17) -0.0001(14) -0.0008(12) -0.0106(14) C224 0.0352(17) 0.062(2) 0.058(2) -0.0071(17) -0.0003(14) 0.0052(15) C225 0.0469(19) 0.0423(19) 0.064(2) -0.0060(16) -0.0044(16) 0.0089(15) C226 0.0490(18) 0.0374(16) 0.0388(16) -0.0021(13) -0.0036(13) -0.0064(14) C1S 0.056(2) 0.061(2) 0.056(2) -0.0115(18) 0.0029(16) -0.0017(18) Cl1S 0.1141(10) 0.1014(10) 0.0559(6) -0.0006(6) 0.0207(6) 0.0170(8) Cl2S 0.1136(10) 0.0683(7) 0.0701(7) -0.0078(5) -0.0219(6) 0.0149(7) _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 Ti1 N1 1.794(2) . ? Ti1 Cl1 2.2849(8) . ? Ti1 Cl2 2.3091(8) . ? Ti1 C2 2.334(3) . ? Ti1 C3 2.345(3) . ? Ti1 C4 2.377(3) . ? Ti1 C1 2.412(3) . ? Ti1 C5 2.421(3) . ? C1 C5 1.409(4) . ? C1 C2 1.424(4) . ? C1 C6 1.498(4) . ? C2 C3 1.408(4) . ? C2 C7 1.510(4) . ? C3 C4 1.403(4) . ? C3 C8 1.503(4) . ? C4 C5 1.415(4) . ? C4 C9 1.506(4) . ? C5 C10 1.500(4) . ? N1 P1 1.578(2) . ? P1 C121 1.800(3) . ? P1 C111 1.804(3) . ? P1 C11 1.823(3) . ? C111 C116 1.387(4) . ? C111 C112 1.398(4) . ? C112 C113 1.391(4) . ? C113 C114 1.376(5) . ? C114 C115 1.388(4) . ? C115 C116 1.384(4) . ? C121 C126 1.394(4) . ? C121 C122 1.397(4) . ? C122 C123 1.381(4) . ? C123 C124 1.386(5) . ? C124 C125 1.370(5) . ? C125 C126 1.389(4) . ? C11 N12 1.340(3) . ? C11 C16 1.393(4) . ? N12 C13 1.340(3) . ? C13 C14 1.388(4) . ? C13 P2 1.824(2) . ? C14 C15 1.387(4) . ? C15 C16 1.381(4) . ? Ti2 N2 1.791(2) . ? Ti2 Cl4 2.3044(9) . ? Ti2 Cl3 2.3116(8) . ? Ti2 C22 2.341(3) . ? Ti2 C23 2.343(3) . ? Ti2 C24 2.374(3) . ? Ti2 C21 2.398(3) . ? Ti2 C25 2.411(3) . ? C21 C25 1.393(4) . ? C21 C22 1.393(4) . ? C21 C26 1.511(5) . ? C22 C23 1.378(5) . ? C22 C27 1.524(5) . ? C23 C24 1.450(5) . ? C23 C28 1.515(4) . ? C24 C25 1.426(4) . ? C24 C29 1.483(5) . ? C25 C30 1.505(4) . ? N2 P2 1.578(2) . ? P2 C211 1.799(3) . ? P2 C221 1.804(3) . ? C211 C212 1.394(4) . ? C211 C216 1.395(4) . ? C212 C213 1.385(4) . ? C213 C214 1.374(5) . ? C214 C215 1.389(4) . ? C215 C216 1.382(4) . ? C221 C226 1.394(4) . ? C221 C222 1.397(4) . ? C222 C223 1.392(4) . ? C223 C224 1.376(5) . ? C224 C225 1.376(5) . ? C225 C226 1.385(5) . ? C1S Cl1S 1.738(4) . ? C1S Cl2S 1.754(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 N1 Ti1 Cl1 102.40(8) . . ? N1 Ti1 Cl2 101.81(8) . . ? Cl1 Ti1 Cl2 102.99(3) . . ? N1 Ti1 C2 99.74(10) . . ? Cl1 Ti1 C2 100.34(8) . . ? Cl2 Ti1 C2 143.78(7) . . ? N1 Ti1 C3 90.99(10) . . ? Cl1 Ti1 C3 135.33(8) . . ? Cl2 Ti1 C3 115.78(8) . . ? C2 Ti1 C3 35.02(10) . . ? N1 Ti1 C4 116.20(10) . . ? Cl1 Ti1 C4 137.47(7) . . ? Cl2 Ti1 C4 86.61(7) . . ? C2 Ti1 C4 57.69(10) . . ? C3 Ti1 C4 34.56(10) . . ? N1 Ti1 C1 133.66(11) . . ? Cl1 Ti1 C1 84.05(7) . . ? Cl2 Ti1 C1 121.63(8) . . ? C2 Ti1 C1 34.88(10) . . ? C3 Ti1 C1 57.50(10) . . ? C4 Ti1 C1 56.78(10) . . ? N1 Ti1 C5 148.15(10) . . ? Cl1 Ti1 C5 103.55(8) . . ? Cl2 Ti1 C5 90.01(7) . . ? C2 Ti1 C5 57.58(10) . . ? C3 Ti1 C5 57.42(9) . . ? C4 Ti1 C5 34.29(10) . . ? C1 Ti1 C5 33.90(10) . . ? C5 C1 C2 108.0(2) . . ? C5 C1 C6 127.2(3) . . ? C2 C1 C6 124.7(3) . . ? C5 C1 Ti1 73.43(15) . . ? C2 C1 Ti1 69.59(15) . . ? C6 C1 Ti1 125.8(2) . . ? C3 C2 C1 107.8(3) . . ? C3 C2 C7 126.8(3) . . ? C1 C2 C7 125.3(3) . . ? C3 C2 Ti1 72.92(16) . . ? C1 C2 Ti1 75.53(16) . . ? C7 C2 Ti1 120.39(19) . . ? C4 C3 C2 107.9(2) . . ? C4 C3 C8 125.1(3) . . ? C2 C3 C8 126.9(3) . . ? C4 C3 Ti1 73.96(16) . . ? C2 C3 Ti1 72.06(16) . . ? C8 C3 Ti1 122.32(19) . . ? C3 C4 C5 108.7(2) . . ? C3 C4 C9 125.5(3) . . ? C5 C4 C9 125.6(3) . . ? C3 C4 Ti1 71.48(15) . . ? C5 C4 Ti1 74.56(15) . . ? C9 C4 Ti1 123.5(2) . . ? C1 C5 C4 107.5(2) . . ? C1 C5 C10 126.4(3) . . ? C4 C5 C10 126.1(3) . . ? C1 C5 Ti1 72.67(15) . . ? C4 C5 Ti1 71.14(15) . . ? C10 C5 Ti1 120.9(2) . . ? P1 N1 Ti1 155.43(16) . . ? N1 P1 C121 113.08(12) . . ? N1 P1 C111 112.14(11) . . ? C121 P1 C111 107.06(12) . . ? N1 P1 C11 111.69(12) . . ? C121 P1 C11 108.87(12) . . ? C111 P1 C11 103.46(12) . . ? C116 C111 C112 119.9(2) . . ? C116 C111 P1 117.5(2) . . ? C112 C111 P1 122.5(2) . . ? C113 C112 C111 119.4(3) . . ? C114 C113 C112 120.4(3) . . ? C113 C114 C115 120.3(3) . . ? C116 C115 C114 119.8(3) . . ? C115 C116 C111 120.3(3) . . ? C126 C121 C122 119.1(3) . . ? C126 C121 P1 123.8(2) . . ? C122 C121 P1 116.9(2) . . ? C123 C122 C121 120.6(3) . . ? C122 C123 C124 119.6(3) . . ? C125 C124 C123 120.3(3) . . ? C124 C125 C126 120.7(3) . . ? C125 C126 C121 119.6(3) . . ? N12 C11 C16 122.9(2) . . ? N12 C11 P1 114.09(18) . . ? C16 C11 P1 122.97(19) . . ? C11 N12 C13 117.7(2) . . ? N12 C13 C14 123.4(2) . . ? N12 C13 P2 113.82(18) . . ? C14 C13 P2 122.7(2) . . ? C15 C14 C13 118.1(2) . . ? C16 C15 C14 119.3(2) . . ? C15 C16 C11 118.6(2) . . ? N2 Ti2 Cl4 102.91(8) . . ? N2 Ti2 Cl3 102.70(8) . . ? Cl4 Ti2 Cl3 99.00(3) . . ? N2 Ti2 C22 97.80(11) . . ? Cl4 Ti2 C22 103.70(9) . . ? Cl3 Ti2 C22 145.00(9) . . ? N2 Ti2 C23 91.50(10) . . ? Cl4 Ti2 C23 137.62(9) . . ? Cl3 Ti2 C23 116.57(10) . . ? C22 Ti2 C23 34.22(12) . . ? N2 Ti2 C24 118.93(12) . . ? Cl4 Ti2 C24 135.38(9) . . ? Cl3 Ti2 C24 86.93(9) . . ? C22 Ti2 C24 58.24(12) . . ? C23 Ti2 C24 35.79(12) . . ? N2 Ti2 C21 130.18(11) . . ? Cl4 Ti2 C21 84.63(8) . . ? Cl3 Ti2 C21 124.97(8) . . ? C22 Ti2 C21 34.16(11) . . ? C23 Ti2 C21 56.76(11) . . ? C24 Ti2 C21 57.31(11) . . ? N2 Ti2 C25 148.98(10) . . ? Cl4 Ti2 C25 100.72(7) . . ? Cl3 Ti2 C25 93.08(7) . . ? C22 Ti2 C25 56.90(10) . . ? C23 Ti2 C25 57.49(10) . . ? C24 Ti2 C25 34.66(11) . . ? C21 Ti2 C25 33.67(10) . . ? C25 C21 C22 108.7(3) . . ? C25 C21 C26 125.2(3) . . ? C22 C21 C26 125.8(3) . . ? C25 C21 Ti2 73.66(16) . . ? C22 C21 Ti2 70.68(16) . . ? C26 C21 Ti2 125.6(2) . . ? C23 C22 C21 108.9(3) . . ? C23 C22 C27 124.3(3) . . ? C21 C22 C27 126.6(3) . . ? C23 C22 Ti2 72.99(16) . . ? C21 C22 Ti2 75.16(16) . . ? C27 C22 Ti2 122.2(2) . . ? C22 C23 C24 108.4(3) . . ? C22 C23 C28 127.0(4) . . ? C24 C23 C28 124.4(4) . . ? C22 C23 Ti2 72.79(16) . . ? C24 C23 Ti2 73.25(15) . . ? C28 C23 Ti2 123.2(2) . . ? C25 C24 C23 105.4(3) . . ? C25 C24 C29 127.2(3) . . ? C23 C24 C29 127.3(3) . . ? C25 C24 Ti2 74.07(16) . . ? C23 C24 Ti2 70.95(16) . . ? C29 C24 Ti2 123.8(2) . . ? C21 C25 C24 108.6(3) . . ? C21 C25 C30 127.1(3) . . ? C24 C25 C30 124.3(3) . . ? C21 C25 Ti2 72.67(15) . . ? C24 C25 Ti2 71.27(15) . . ? C30 C25 Ti2 121.5(2) . . ? P2 N2 Ti2 165.54(18) . . ? N2 P2 C211 113.36(12) . . ? N2 P2 C221 113.05(13) . . ? C211 P2 C221 109.67(13) . . ? N2 P2 C13 110.94(12) . . ? C211 P2 C13 103.67(12) . . ? C221 P2 C13 105.46(11) . . ? C212 C211 C216 119.2(3) . . ? C212 C211 P2 123.5(2) . . ? C216 C211 P2 117.2(2) . . ? C213 C212 C211 119.9(3) . . ? C214 C213 C212 120.7(3) . . ? C213 C214 C215 119.9(3) . . ? C216 C215 C214 120.0(3) . . ? C215 C216 C211 120.3(3) . . ? C226 C221 C222 119.8(3) . . ? C226 C221 P2 118.1(2) . . ? C222 C221 P2 122.1(2) . . ? C223 C222 C221 119.3(3) . . ? C224 C223 C222 120.3(3) . . ? C223 C224 C225 120.6(3) . . ? C224 C225 C226 120.1(3) . . ? C225 C226 C221 120.0(3) . . ? Cl1S C1S Cl2S 112.3(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.870 _refine_diff_density_min -0.792 _refine_diff_density_rms 0.080 #===END data_msp174 _database_code_CSD 154070 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H48 Cl2 N P Ti' _chemical_formula_weight 692.56 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 19.5778(5) _cell_length_b 10.3318(3) _cell_length_c 19.8983(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.136(2) _cell_angle_gamma 90.00 _cell_volume 3728.24(16) _cell_formula_units_Z 4 _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 0.50 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 0.444 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8086 _exptl_absorpt_correction_T_max 0.9739 _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 29110 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7286 _reflns_number_gt 6403 _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^)+(0.0673P)^2^+1.4280P] 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 0.0062(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7286 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1193 _refine_ls_wR_factor_gt 0.1120 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.004 _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 Ti1 Ti 0.461215(17) 0.76403(3) 0.196986(16) 0.02501(12) Uani 1 1 d . . . Cl1 Cl 0.50985(3) 0.92158(5) 0.28432(3) 0.03877(15) Uani 1 1 d . . . Cl2 Cl 0.51865(3) 0.81149(5) 0.11729(2) 0.03426(14) Uani 1 1 d . . . C1 C 0.34827(10) 0.6560(2) 0.16941(11) 0.0348(4) Uani 1 1 d . . . C2 C 0.35133(10) 0.6972(2) 0.10291(10) 0.0315(4) Uani 1 1 d . . . C3 C 0.34776(10) 0.83481(19) 0.10049(10) 0.0308(4) Uani 1 1 d . . . C4 C 0.34447(10) 0.8781(2) 0.16636(11) 0.0350(4) Uani 1 1 d . . . C5 C 0.34620(11) 0.7674(2) 0.20973(11) 0.0364(5) Uani 1 1 d . . . C6 C 0.34482(13) 0.5174(2) 0.19145(15) 0.0537(6) Uani 1 1 d . . . H6A H 0.2932 0.4919 0.1784 0.081 Uiso 1 1 calc R . . H6B H 0.3712 0.5088 0.2440 0.081 Uiso 1 1 calc R . . H6C H 0.3678 0.4613 0.1662 0.081 Uiso 1 1 calc R . . C7 C 0.35168(12) 0.6117(2) 0.04199(12) 0.0460(5) Uani 1 1 d . . . H7A H 0.3802 0.5332 0.0620 0.069 Uiso 1 1 calc R . . H7B H 0.3741 0.6582 0.0126 0.069 Uiso 1 1 calc R . . H7C H 0.3009 0.5879 0.0116 0.069 Uiso 1 1 calc R . . C8 C 0.34432(13) 0.9168(2) 0.03692(12) 0.0459(5) Uani 1 1 d . . . H8A H 0.2973 0.9018 -0.0036 0.069 Uiso 1 1 calc R . . H8B H 0.3851 0.8937 0.0221 0.069 Uiso 1 1 calc R . . H8C H 0.3483 1.0083 0.0508 0.069 Uiso 1 1 calc R . . C9 C 0.33627(14) 1.0154(2) 0.18684(14) 0.0545(6) Uani 1 1 d . . . H9A H 0.3499 1.0745 0.1555 0.082 Uiso 1 1 calc R . . H9B H 0.3686 1.0302 0.2375 0.082 Uiso 1 1 calc R . . H9C H 0.2849 1.0311 0.1809 0.082 Uiso 1 1 calc R . . C10 C 0.34111(14) 0.7716(3) 0.28337(12) 0.0570(7) Uani 1 1 d . . . H10A H 0.3815 0.8242 0.3163 0.085 Uiso 1 1 calc R . . H10B H 0.3447 0.6835 0.3027 0.085 Uiso 1 1 calc R . . H10C H 0.2938 0.8098 0.2791 0.085 Uiso 1 1 calc R . . N1 N 0.50788(9) 0.62028(15) 0.23809(8) 0.0305(3) Uani 1 1 d . . . P1 P 0.56055(2) 0.49827(4) 0.26209(2) 0.02557(13) Uani 1 1 d . . . C11 C 0.65583(10) 0.54492(19) 0.28891(9) 0.0295(4) Uani 1 1 d . . . C12 C 0.70988(11) 0.4513(2) 0.29928(11) 0.0379(4) Uani 1 1 d . . . H12 H 0.6966 0.3628 0.2900 0.045 Uiso 1 1 calc R . . C13 C 0.78358(12) 0.4881(3) 0.32334(12) 0.0475(6) Uani 1 1 d . . . H13 H 0.8208 0.4248 0.3305 0.057 Uiso 1 1 calc R . . C14 C 0.80247(12) 0.6175(3) 0.33684(12) 0.0489(6) Uani 1 1 d . . . H14 H 0.8528 0.6426 0.3529 0.059 Uiso 1 1 calc R . . C15 C 0.74887(12) 0.7104(2) 0.32724(12) 0.0452(5) Uani 1 1 d . . . H15 H 0.7625 0.7987 0.3372 0.054 Uiso 1 1 calc R . . C16 C 0.67515(11) 0.6749(2) 0.30307(11) 0.0353(4) Uani 1 1 d . . . H16 H 0.6381 0.7386 0.2962 0.042 Uiso 1 1 calc R . . C21 C 0.53932(10) 0.38011(18) 0.19016(9) 0.0276(4) Uani 1 1 d . . . C22 C 0.52300(11) 0.25183(18) 0.19856(11) 0.0330(4) Uani 1 1 d . . . H22 H 0.5259 0.2214 0.2446 0.040 Uiso 1 1 calc R . . C23 C 0.50239(11) 0.1679(2) 0.13971(11) 0.0369(4) Uani 1 1 d . . . H23 H 0.4909 0.0803 0.1456 0.044 Uiso 1 1 calc R . . C24 C 0.49852(11) 0.2112(2) 0.07283(11) 0.0363(4) Uani 1 1 d . . . H24 H 0.4841 0.1536 0.0327 0.044 Uiso 1 1 calc R . . C25 C 0.51565(12) 0.3387(2) 0.06420(10) 0.0376(4) Uani 1 1 d . . . H25 H 0.5135 0.3681 0.0182 0.045 Uiso 1 1 calc R . . C26 C 0.53588(11) 0.4234(2) 0.12230(10) 0.0341(4) Uani 1 1 d . . . H26 H 0.5474 0.5108 0.1161 0.041 Uiso 1 1 calc R . . C31 C 0.55403(11) 0.41509(18) 0.33991(10) 0.0308(4) Uani 1 1 d . . . H31A H 0.5049 0.3740 0.3258 0.037 Uiso 1 1 calc R . . H31B H 0.5918 0.3460 0.3560 0.037 Uiso 1 1 calc R . . C32 C 0.56538(11) 0.50841(18) 0.40169(10) 0.0301(4) Uani 1 1 d . . . C33 C 0.63519(11) 0.5349(2) 0.45225(10) 0.0366(4) Uani 1 1 d . . . H33 H 0.6768 0.4919 0.4492 0.044 Uiso 1 1 calc R . . C34 C 0.64474(11) 0.6239(2) 0.50730(11) 0.0381(5) Uani 1 1 d . . . H34 H 0.6931 0.6407 0.5414 0.046 Uiso 1 1 calc R . . C35 C 0.58523(10) 0.68919(19) 0.51386(10) 0.0305(4) Uani 1 1 d . . . C36 C 0.51582(11) 0.6615(2) 0.46293(11) 0.0357(4) Uani 1 1 d . . . H36 H 0.4740 0.7042 0.4658 0.043 Uiso 1 1 calc R . . C37 C 0.50599(11) 0.5726(2) 0.40781(11) 0.0361(4) Uani 1 1 d . . . H37 H 0.4577 0.5555 0.3737 0.043 Uiso 1 1 calc R . . C38 C 0.59860(11) 0.7885(2) 0.57466(10) 0.0333(4) Uani 1 1 d . . . C39 C 0.64446(14) 0.9009(2) 0.56332(14) 0.0486(5) Uani 1 1 d . . . H39A H 0.6929 0.8687 0.5673 0.073 Uiso 1 1 calc R . . H39B H 0.6508 0.9672 0.6004 0.073 Uiso 1 1 calc R . . H39C H 0.6190 0.9385 0.5151 0.073 Uiso 1 1 calc R . . C40 C 0.64100(13) 0.7244(2) 0.64841(11) 0.0435(5) Uani 1 1 d . . . H40A H 0.6118 0.6528 0.6558 0.065 Uiso 1 1 calc R . . H40B H 0.6500 0.7884 0.6872 0.065 Uiso 1 1 calc R . . H40C H 0.6882 0.6913 0.6492 0.065 Uiso 1 1 calc R . . C41 C 0.52652(12) 0.8442(2) 0.57547(12) 0.0400(5) Uani 1 1 d . . . H41A H 0.5007 0.8908 0.5301 0.060 Uiso 1 1 calc R . . H41B H 0.5374 0.9038 0.6165 0.060 Uiso 1 1 calc R . . H41C H 0.4953 0.7735 0.5804 0.060 Uiso 1 1 calc R . . C1S C 0.72247(12) 0.18776(19) 0.47734(12) 0.0384(5) Uani 1 1 d . . . C2S C 0.79301(13) 0.2175(2) 0.48034(12) 0.0424(5) Uani 1 1 d . . . H2S H 0.8259 0.2640 0.5208 0.051 Uiso 1 1 calc R . . C3S C 0.81589(12) 0.1805(2) 0.42533(13) 0.0457(5) Uani 1 1 d . . . H3S H 0.8641 0.2018 0.4282 0.055 Uiso 1 1 calc R . . C4S C 0.76891(13) 0.1130(2) 0.36646(12) 0.0457(5) Uani 1 1 d . . . H4S H 0.7846 0.0879 0.3287 0.055 Uiso 1 1 calc R . . C5S C 0.69855(13) 0.0816(2) 0.36237(12) 0.0446(5) Uani 1 1 d . . . H5S H 0.6660 0.0346 0.3219 0.054 Uiso 1 1 calc R . . C6S C 0.67602(12) 0.1189(2) 0.41743(12) 0.0414(5) Uani 1 1 d . . . H6S H 0.6278 0.0971 0.4143 0.050 Uiso 1 1 calc R . . C7S C 0.69839(15) 0.2275(2) 0.53770(14) 0.0509(6) Uani 1 1 d . . . H7S1 H 0.6450 0.2150 0.5224 0.076 Uiso 1 1 calc R . . H7S2 H 0.7104 0.3190 0.5494 0.076 Uiso 1 1 calc R . . H7S3 H 0.7240 0.1746 0.5807 0.076 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 Ti1 0.02471(19) 0.02578(19) 0.02368(18) -0.00146(11) 0.00813(14) 0.00074(12) Cl1 0.0398(3) 0.0372(3) 0.0364(3) -0.01212(19) 0.0110(2) -0.0028(2) Cl2 0.0350(3) 0.0378(3) 0.0334(2) 0.00041(18) 0.0168(2) -0.00044(19) C1 0.0240(9) 0.0407(11) 0.0364(10) 0.0049(8) 0.0077(8) -0.0028(8) C2 0.0233(9) 0.0382(11) 0.0299(9) -0.0042(8) 0.0064(7) -0.0023(8) C3 0.0224(9) 0.0362(10) 0.0295(9) 0.0010(7) 0.0048(7) 0.0014(7) C4 0.0254(9) 0.0403(11) 0.0356(10) -0.0047(8) 0.0071(8) 0.0070(8) C5 0.0255(9) 0.0544(13) 0.0295(10) 0.0026(8) 0.0107(8) 0.0046(8) C6 0.0392(12) 0.0476(14) 0.0656(15) 0.0176(12) 0.0099(11) -0.0091(10) C7 0.0385(11) 0.0510(13) 0.0445(12) -0.0189(10) 0.0111(9) -0.0059(10) C8 0.0393(11) 0.0526(14) 0.0402(11) 0.0132(10) 0.0087(9) 0.0010(10) C9 0.0472(13) 0.0474(14) 0.0601(14) -0.0142(11) 0.0105(11) 0.0165(11) C10 0.0409(12) 0.100(2) 0.0339(12) 0.0031(12) 0.0185(10) 0.0083(13) N1 0.0302(8) 0.0313(8) 0.0288(8) 0.0006(6) 0.0099(6) 0.0004(6) P1 0.0268(2) 0.0252(2) 0.0245(2) 0.00108(16) 0.00950(18) -0.00027(17) C11 0.0289(9) 0.0350(10) 0.0244(8) 0.0008(7) 0.0097(7) -0.0018(8) C12 0.0330(10) 0.0408(11) 0.0393(11) 0.0035(9) 0.0129(8) 0.0048(9) C13 0.0304(11) 0.0640(15) 0.0456(12) 0.0083(11) 0.0114(9) 0.0104(10) C14 0.0294(11) 0.0726(17) 0.0409(12) 0.0026(11) 0.0089(9) -0.0099(11) C15 0.0384(12) 0.0524(13) 0.0417(12) -0.0043(10) 0.0118(9) -0.0145(10) C16 0.0333(10) 0.0357(11) 0.0356(10) -0.0010(8) 0.0117(8) -0.0035(8) C21 0.0256(9) 0.0299(9) 0.0265(9) -0.0011(7) 0.0089(7) -0.0003(7) C22 0.0386(11) 0.0305(10) 0.0297(10) 0.0022(7) 0.0128(8) -0.0005(8) C23 0.0394(11) 0.0297(10) 0.0412(11) -0.0050(8) 0.0148(9) -0.0040(8) C24 0.0326(10) 0.0413(11) 0.0321(10) -0.0086(8) 0.0088(8) 0.0010(8) C25 0.0421(11) 0.0429(12) 0.0277(9) -0.0007(8) 0.0130(8) 0.0018(9) C26 0.0401(11) 0.0328(10) 0.0307(9) 0.0014(7) 0.0149(8) -0.0004(8) C31 0.0363(10) 0.0297(10) 0.0274(9) 0.0015(7) 0.0130(8) -0.0013(8) C32 0.0355(10) 0.0312(10) 0.0247(8) 0.0028(7) 0.0126(7) -0.0010(7) C33 0.0301(10) 0.0471(12) 0.0315(10) -0.0024(8) 0.0103(8) 0.0066(9) C34 0.0278(10) 0.0517(13) 0.0316(10) -0.0059(9) 0.0077(8) 0.0004(9) C35 0.0330(10) 0.0325(10) 0.0277(9) 0.0013(7) 0.0134(8) -0.0012(8) C36 0.0303(10) 0.0424(11) 0.0348(10) -0.0020(8) 0.0127(8) 0.0043(8) C37 0.0296(10) 0.0451(12) 0.0314(10) -0.0040(8) 0.0089(8) -0.0015(8) C38 0.0341(10) 0.0361(10) 0.0314(9) -0.0038(8) 0.0140(8) -0.0041(8) C39 0.0507(13) 0.0431(13) 0.0577(14) -0.0089(10) 0.0269(11) -0.0125(10) C40 0.0454(12) 0.0528(13) 0.0299(10) -0.0067(9) 0.0113(9) 0.0029(10) C41 0.0434(12) 0.0399(11) 0.0402(11) -0.0048(9) 0.0196(9) 0.0028(9) C1S 0.0421(11) 0.0295(10) 0.0440(11) 0.0060(8) 0.0166(9) 0.0043(8) C2S 0.0414(12) 0.0349(11) 0.0453(12) 0.0005(9) 0.0101(9) -0.0049(9) C3S 0.0353(11) 0.0477(13) 0.0553(13) 0.0103(10) 0.0183(10) -0.0015(9) C4S 0.0455(12) 0.0511(13) 0.0430(12) 0.0058(10) 0.0196(10) 0.0049(10) C5S 0.0429(12) 0.0465(13) 0.0400(11) 0.0013(9) 0.0105(9) -0.0005(10) C6S 0.0332(10) 0.0400(11) 0.0489(12) 0.0077(9) 0.0133(9) 0.0011(9) C7S 0.0624(16) 0.0435(13) 0.0537(14) 0.0004(10) 0.0297(12) 0.0012(11) _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 Ti1 N1 1.7737(16) . ? Ti1 Cl1 2.3085(5) . ? Ti1 Cl2 2.3158(5) . ? Ti1 C1 2.3496(19) . ? Ti1 C5 2.359(2) . ? Ti1 C2 2.3610(18) . ? Ti1 C4 2.4363(19) . ? Ti1 C3 2.4375(18) . ? C1 C5 1.412(3) . ? C1 C2 1.412(3) . ? C1 C6 1.507(3) . ? C2 C3 1.424(3) . ? C2 C7 1.502(3) . ? C3 C4 1.409(3) . ? C3 C8 1.503(3) . ? C4 C5 1.425(3) . ? C4 C9 1.501(3) . ? C5 C10 1.506(3) . ? N1 P1 1.5841(16) . ? P1 C11 1.8018(19) . ? P1 C21 1.8066(18) . ? P1 C31 1.8170(18) . ? C11 C12 1.390(3) . ? C11 C16 1.395(3) . ? C12 C13 1.391(3) . ? C13 C14 1.386(4) . ? C14 C15 1.381(4) . ? C15 C16 1.388(3) . ? C21 C22 1.388(3) . ? C21 C26 1.400(3) . ? C22 C23 1.389(3) . ? C23 C24 1.379(3) . ? C24 C25 1.386(3) . ? C25 C26 1.384(3) . ? C31 C32 1.511(3) . ? C32 C37 1.383(3) . ? C32 C33 1.385(3) . ? C33 C34 1.388(3) . ? C34 C35 1.394(3) . ? C35 C36 1.385(3) . ? C35 C38 1.532(3) . ? C36 C37 1.387(3) . ? C38 C41 1.530(3) . ? C38 C39 1.535(3) . ? C38 C40 1.537(3) . ? C1S C6S 1.392(3) . ? C1S C2S 1.394(3) . ? C1S C7S 1.504(3) . ? C2S C3S 1.384(3) . ? C3S C4S 1.376(3) . ? C4S C5S 1.387(3) . ? C5S C6S 1.381(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 Ti1 Cl1 104.39(5) . . ? N1 Ti1 Cl2 101.21(5) . . ? Cl1 Ti1 Cl2 101.38(2) . . ? N1 Ti1 C1 89.20(7) . . ? Cl1 Ti1 C1 126.55(6) . . ? Cl2 Ti1 C1 126.70(5) . . ? N1 Ti1 C5 108.02(7) . . ? Cl1 Ti1 C5 92.77(5) . . ? Cl2 Ti1 C5 143.11(5) . . ? C1 Ti1 C5 34.90(7) . . ? N1 Ti1 C2 106.13(7) . . ? Cl1 Ti1 C2 142.86(5) . . ? Cl2 Ti1 C2 92.95(5) . . ? C1 Ti1 C2 34.89(7) . . ? C5 Ti1 C2 57.87(7) . . ? N1 Ti1 C4 142.38(7) . . ? Cl1 Ti1 C4 85.93(5) . . ? Cl2 Ti1 C4 112.22(5) . . ? C1 Ti1 C4 57.29(7) . . ? C5 Ti1 C4 34.54(7) . . ? C2 Ti1 C4 56.94(7) . . ? N1 Ti1 C3 140.59(7) . . ? Cl1 Ti1 C3 112.11(5) . . ? Cl2 Ti1 C3 86.02(5) . . ? C1 Ti1 C3 57.34(7) . . ? C5 Ti1 C3 57.10(6) . . ? C2 Ti1 C3 34.47(7) . . ? C4 Ti1 C3 33.61(6) . . ? C5 C1 C2 107.91(18) . . ? C5 C1 C6 126.5(2) . . ? C2 C1 C6 125.5(2) . . ? C5 C1 Ti1 72.92(11) . . ? C2 C1 Ti1 72.99(11) . . ? C6 C1 Ti1 121.65(14) . . ? C1 C2 C3 108.27(17) . . ? C1 C2 C7 126.4(2) . . ? C3 C2 C7 125.11(18) . . ? C1 C2 Ti1 72.12(11) . . ? C3 C2 Ti1 75.71(10) . . ? C7 C2 Ti1 122.14(13) . . ? C4 C3 C2 107.73(17) . . ? C4 C3 C8 126.93(19) . . ? C2 C3 C8 125.28(18) . . ? C4 C3 Ti1 73.14(10) . . ? C2 C3 Ti1 69.82(10) . . ? C8 C3 Ti1 124.80(13) . . ? C3 C4 C5 108.02(17) . . ? C3 C4 C9 126.8(2) . . ? C5 C4 C9 125.1(2) . . ? C3 C4 Ti1 73.24(11) . . ? C5 C4 Ti1 69.77(11) . . ? C9 C4 Ti1 125.13(15) . . ? C1 C5 C4 108.01(17) . . ? C1 C5 C10 127.1(2) . . ? C4 C5 C10 124.8(2) . . ? C1 C5 Ti1 72.18(11) . . ? C4 C5 Ti1 75.69(11) . . ? C10 C5 Ti1 121.38(14) . . ? P1 N1 Ti1 165.69(11) . . ? N1 P1 C11 111.10(9) . . ? N1 P1 C21 111.69(8) . . ? C11 P1 C21 108.59(8) . . ? N1 P1 C31 112.74(9) . . ? C11 P1 C31 105.75(9) . . ? C21 P1 C31 106.65(8) . . ? C12 C11 C16 120.41(18) . . ? C12 C11 P1 120.21(15) . . ? C16 C11 P1 119.28(15) . . ? C11 C12 C13 119.6(2) . . ? C14 C13 C12 119.8(2) . . ? C15 C14 C13 120.7(2) . . ? C14 C15 C16 120.1(2) . . ? C15 C16 C11 119.5(2) . . ? C22 C21 C26 119.45(17) . . ? C22 C21 P1 122.99(14) . . ? C26 C21 P1 117.48(14) . . ? C21 C22 C23 120.11(18) . . ? C24 C23 C22 120.24(19) . . ? C23 C24 C25 120.00(18) . . ? C26 C25 C24 120.29(18) . . ? C25 C26 C21 119.89(18) . . ? C32 C31 P1 110.81(13) . . ? C37 C32 C33 118.26(18) . . ? C37 C32 C31 120.43(17) . . ? C33 C32 C31 121.29(17) . . ? C32 C33 C34 120.45(18) . . ? C33 C34 C35 121.72(18) . . ? C36 C35 C34 117.08(18) . . ? C36 C35 C38 123.03(17) . . ? C34 C35 C38 119.87(17) . . ? C35 C36 C37 121.41(18) . . ? C32 C37 C36 121.07(18) . . ? C41 C38 C35 112.12(16) . . ? C41 C38 C39 108.08(18) . . ? C35 C38 C39 109.02(16) . . ? C41 C38 C40 108.67(17) . . ? C35 C38 C40 109.61(17) . . ? C39 C38 C40 109.30(18) . . ? C6S C1S C2S 117.8(2) . . ? C6S C1S C7S 121.6(2) . . ? C2S C1S C7S 120.6(2) . . ? C3S C2S C1S 121.1(2) . . ? C4S C3S C2S 120.1(2) . . ? C3S C4S C5S 119.9(2) . . ? C6S C5S C4S 119.7(2) . . ? C5S C6S C1S 121.4(2) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.861 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.087 #===END data_musa1 _database_code_CSD 154071 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'Zr2 Si2 C52 H66 Cl10 N2 P2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C52 H66 Cl10 N2 P2 Si2 Zr2' _chemical_formula_weight 1374.13 _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' 'P' 'P' 0.1023 0.0942 '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 Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.729(3) _cell_length_b 11.509(2) _cell_length_c 17.448(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.13(3) _cell_angle_gamma 90.00 _cell_volume 3325.5(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method ? _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 0.832 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku R-axis IIc' _diffrn_measurement_method 'image plate oscillation photographs' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9122 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.55 _reflns_number_total 5572 _reflns_number_observed 3623 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'MSC Raxis II control software' _computing_cell_refinement ; DENZO AND SCALEPACK (Otwinowski and Minor, 1985) ; _computing_data_reduction 'SHELX97-SHELXPRO (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL+XP' _computing_publication_material 'SHELXTL+XCIF' _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^)+(0.1393P)^2^+0.0000P] 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 5572 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0954 _refine_ls_R_factor_obs 0.0544 _refine_ls_wR_factor_all 0.2193 _refine_ls_wR_factor_obs 0.1653 _refine_ls_goodness_of_fit_all 1.053 _refine_ls_goodness_of_fit_obs 0.994 _refine_ls_restrained_S_all 1.053 _refine_ls_restrained_S_obs 0.994 _refine_ls_shift/esd_max 0.000 _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 Zr1 Zr 0.41258(4) 0.45114(4) 0.06524(3) 0.0689(3) Uani 1 d . . Cl1 Cl 0.33226(11) 0.3957(2) -0.05643(9) 0.0874(5) Uani 1 d . . Cl2 Cl 0.38363(14) 0.26706(14) 0.11815(10) 0.0947(6) Uani 1 d . . Cl3 Cl 0.46168(10) 0.63118(11) -0.00679(9) 0.0732(4) Uani 1 d . . Cl4 Cl 0.50577(14) 0.5008(2) 0.17852(10) 0.1009(6) Uani 1 d . . Cl5 Cl 0.30660(14) 0.5649(2) 0.10288(12) 0.1018(6) Uani 1 d . . P1 P 0.26517(9) 0.97301(14) -0.03510(8) 0.0653(4) Uani 1 d . . Si1 Si 0.13549(13) 1.1639(2) -0.07587(13) 0.0976(7) Uani 1 d . . N1 N 0.2334(3) 1.1019(5) -0.0647(3) 0.0738(13) Uani 1 d . . H1 H 0.2704(3) 1.1472(5) -0.0770(3) 0.089 Uiso 1 calc R . C1 C 0.3745(4) 0.9732(6) -0.0080(3) 0.0699(14) Uani 1 d . . C2 C 0.4181(3) 1.0084(5) -0.0764(3) 0.0624(12) Uani 1 d . . C3 C 0.4379(4) 0.9276(5) -0.1278(3) 0.0674(14) Uani 1 d . . H3 H 0.4237(4) 0.8503(5) -0.1221(3) 0.081 Uiso 1 calc R . C4 C 0.4790(4) 0.9589(5) -0.1884(4) 0.0703(15) Uani 1 d . . H4 H 0.4931(4) 0.9012(5) -0.2213(4) 0.084 Uiso 1 calc R . C5 C 0.4993(4) 1.0713(5) -0.2015(3) 0.0672(14) Uani 1 d . . C6 C 0.4769(4) 1.1569(5) -0.1502(4) 0.0714(15) Uani 1 d . . H6 H 0.4898(4) 1.2345(5) -0.1572(4) 0.086 Uiso 1 calc R . C7 C 0.4361(4) 1.1255(5) -0.0900(3) 0.0708(15) Uani 1 d . . H7 H 0.4201(4) 1.1828(5) -0.0578(3) 0.085 Uiso 1 calc R . C8 C 0.5431(5) 1.1061(7) -0.2703(4) 0.091(2) Uani 1 d . . C9 C 0.4866(9) 1.1664(27) -0.3301(9) 0.437(22) Uani 1 d . . H9A H 0.5144(9) 1.1875(27) -0.3725(9) 0.656 Uiso 1 calc R . H9B H 0.4664(9) 1.2351(27) -0.3083(9) 0.656 Uiso 1 calc R . H9C H 0.4424(9) 1.1156(27) -0.3483(9) 0.656 Uiso 1 calc R . C10 C 0.5852(7) 0.9971(10) -0.3014(7) 0.164(5) Uani 1 d . . H10A H 0.6208(7) 0.9623(10) -0.2598(7) 0.246 Uiso 1 calc R . H10B H 0.6155(7) 1.0208(10) -0.3415(7) 0.246 Uiso 1 calc R . H10C H 0.5449(7) 0.9417(10) -0.3219(7) 0.246 Uiso 1 calc R . C11 C 0.6158(9) 1.1939(12) -0.2395(8) 0.215(9) Uani 1 d . . H11A H 0.6531(9) 1.1559(12) -0.2006(8) 0.323 Uiso 1 calc R . H11B H 0.5943(9) 1.2617(12) -0.2178(8) 0.323 Uiso 1 calc R . H11C H 0.6434(9) 1.2163(12) -0.2819(8) 0.323 Uiso 1 calc R . C12 C 0.2416(3) 0.8655(5) -0.1091(3) 0.0646(13) Uani 1 d . . C13 C 0.2033(4) 0.8960(6) -0.1812(4) 0.079(2) Uani 1 d . . H13 H 0.1876(4) 0.9725(6) -0.1920(4) 0.095 Uiso 1 calc R . C14 C 0.1884(4) 0.8093(8) -0.2385(4) 0.095(2) Uani 1 d . . H14 H 0.1623(4) 0.8288(8) -0.2875(4) 0.114 Uiso 1 calc R . C15 C 0.2123(5) 0.6944(7) -0.2226(5) 0.094(2) Uani 1 d . . H15 H 0.2008(5) 0.6371(7) -0.2602(5) 0.113 Uiso 1 calc R . C16 C 0.2515(4) 0.6680(6) -0.1537(4) 0.084(2) Uani 1 d . . H16 H 0.2695(4) 0.5922(6) -0.1440(4) 0.101 Uiso 1 calc R . C17 C 0.2663(4) 0.7501(6) -0.0953(4) 0.077(2) Uani 1 d . . H17 H 0.2928(4) 0.7286(6) -0.0469(4) 0.092 Uiso 1 calc R . C18 C 0.2202(4) 0.9353(6) 0.0487(4) 0.073(2) Uani 1 d . . C19 C 0.2278(5) 1.0184(8) 0.1102(4) 0.097(2) Uani 1 d . . H19 H 0.2553(5) 1.0878(8) 0.1058(4) 0.117 Uiso 1 calc R . C20 C 0.1939(6) 0.9947(12) 0.1765(5) 0.129(3) Uani 1 d . . H20 H 0.1956(6) 1.0502(12) 0.2155(5) 0.154 Uiso 1 calc R . C21 C 0.1584(6) 0.8911(12) 0.1845(5) 0.124(3) Uani 1 d . . H21 H 0.1392(6) 0.8752(12) 0.2309(5) 0.148 Uiso 1 calc R . C22 C 0.1486(6) 0.8039(10) 0.1251(6) 0.124(3) Uani 1 d . . H22 H 0.1222(6) 0.7341(10) 0.1310(6) 0.149 Uiso 1 calc R . C23 C 0.1819(5) 0.8310(7) 0.0567(5) 0.102(2) Uani 1 d . . H23 H 0.1778(5) 0.7772(7) 0.0165(5) 0.122 Uiso 1 calc R . C24 C 0.0616(5) 1.0461(10) -0.0770(7) 0.161(6) Uani 1 d . . H24A H 0.0705(5) 1.0051(10) -0.0287(7) 0.242 Uiso 1 calc R . H24B H 0.0675(5) 0.9934(10) -0.1186(7) 0.242 Uiso 1 calc R . H24C H 0.0080(5) 1.0780(10) -0.0845(7) 0.242 Uiso 1 calc R . C25 C 0.1213(6) 1.2453(8) -0.1670(5) 0.117(3) Uani 1 d . . H25A H 0.1607(6) 1.3062(8) -0.1648(5) 0.175 Uiso 1 calc R . H25B H 0.0681(6) 1.2784(8) -0.1750(5) 0.175 Uiso 1 calc R . H25C H 0.1276(6) 1.1938(8) -0.2091(5) 0.175 Uiso 1 calc R . C26 C 0.1291(9) 1.2617(12) 0.0067(7) 0.206(7) Uani 1 d . . H26A H 0.1367(9) 1.2177(12) 0.0539(7) 0.310 Uiso 1 calc R . H26B H 0.0770(9) 1.2982(12) 0.0006(7) 0.310 Uiso 1 calc R . H26C H 0.1703(9) 1.3201(12) 0.0086(7) 0.310 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 Zr1 0.0890(5) 0.0622(4) 0.0558(3) -0.0017(2) 0.0106(3) 0.0104(3) Cl1 0.1020(12) 0.0864(10) 0.0690(9) -0.0061(7) -0.0040(8) 0.0045(9) Cl2 0.133(2) 0.0730(9) 0.0812(10) 0.0083(8) 0.0250(11) 0.0018(9) Cl3 0.0897(10) 0.0584(7) 0.0726(8) 0.0028(6) 0.0146(8) 0.0141(7) Cl4 0.132(2) 0.1057(13) 0.0608(9) -0.0053(9) -0.0002(9) -0.0062(12) Cl5 0.1162(15) 0.0975(12) 0.0970(13) -0.0048(9) 0.0335(11) 0.0300(10) P1 0.0591(8) 0.0837(9) 0.0546(8) 0.0132(7) 0.0128(6) 0.0094(7) Si1 0.0898(13) 0.121(2) 0.0877(13) 0.0268(12) 0.0336(11) 0.0453(12) N1 0.067(3) 0.082(3) 0.075(3) 0.019(3) 0.021(2) 0.019(3) C1 0.064(3) 0.092(4) 0.055(3) 0.005(3) 0.010(3) 0.006(3) C2 0.056(3) 0.074(3) 0.058(3) 0.001(3) 0.008(2) 0.005(3) C3 0.071(3) 0.060(3) 0.073(3) 0.001(3) 0.017(3) 0.001(3) C4 0.080(4) 0.064(3) 0.069(3) -0.011(3) 0.019(3) 0.000(3) C5 0.071(3) 0.073(3) 0.058(3) -0.002(2) 0.012(3) -0.003(3) C6 0.082(4) 0.061(3) 0.074(3) -0.001(3) 0.023(3) 0.002(3) C7 0.079(4) 0.076(3) 0.060(3) -0.006(3) 0.017(3) 0.011(3) C8 0.101(5) 0.103(5) 0.076(4) -0.009(4) 0.040(4) -0.018(4) C9 0.142(12) 1.029(62) 0.159(12) 0.321(25) 0.084(10) 0.108(22) C10 0.196(12) 0.150(9) 0.178(11) -0.013(8) 0.134(10) -0.007(8) C11 0.265(16) 0.198(12) 0.221(14) -0.092(11) 0.168(14) -0.149(12) C12 0.054(3) 0.082(4) 0.059(3) 0.014(3) 0.012(2) 0.007(3) C13 0.072(4) 0.099(4) 0.069(4) 0.020(3) 0.018(3) 0.012(3) C14 0.085(5) 0.136(7) 0.062(4) -0.007(4) 0.006(3) -0.010(4) C15 0.094(5) 0.099(5) 0.088(5) -0.014(4) 0.009(4) 0.000(4) C16 0.077(4) 0.081(4) 0.092(5) 0.004(4) 0.003(4) 0.011(3) C17 0.072(4) 0.084(4) 0.074(4) 0.015(3) 0.007(3) 0.015(3) C18 0.059(3) 0.091(4) 0.069(3) 0.020(3) 0.011(3) 0.008(3) C19 0.100(5) 0.129(6) 0.067(4) 0.004(4) 0.026(4) 0.002(5) C20 0.133(8) 0.190(10) 0.072(5) 0.020(6) 0.046(5) 0.030(8) C21 0.107(7) 0.181(10) 0.092(6) 0.044(7) 0.044(5) 0.029(6) C22 0.110(7) 0.148(8) 0.125(7) 0.052(7) 0.055(6) 0.006(6) C23 0.099(5) 0.116(6) 0.098(5) 0.036(4) 0.042(5) 0.028(4) C24 0.074(5) 0.222(13) 0.199(11) 0.117(9) 0.060(6) 0.058(6) C25 0.110(6) 0.122(6) 0.118(6) 0.046(5) 0.018(5) 0.044(5) C26 0.238(15) 0.255(16) 0.145(10) -0.011(10) 0.092(11) 0.133(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 Zr1 Cl5 2.371(2) . ? Zr1 Cl2 2.388(2) . ? Zr1 Cl4 2.407(2) . ? Zr1 Cl1 2.431(2) . ? Zr1 Cl3 2.615(2) . ? Zr1 Cl3 2.640(2) 3_665 ? Cl3 Zr1 2.640(2) 3_665 ? P1 N1 1.635(5) . ? P1 C18 1.790(6) . ? P1 C12 1.792(6) . ? P1 C1 1.823(6) . ? Si1 N1 1.772(5) . ? Si1 C25 1.832(8) . ? Si1 C24 1.833(12) . ? Si1 C26 1.843(11) . ? C1 C2 1.539(7) . ? C2 C3 1.365(8) . ? C2 C7 1.408(8) . ? C3 C4 1.387(8) . ? C4 C5 1.366(8) . ? C5 C6 1.416(8) . ? C5 C8 1.545(8) . ? C6 C7 1.380(8) . ? C8 C9 1.48(2) . ? C8 C10 1.572(13) . ? C8 C11 1.614(14) . ? C12 C13 1.374(8) . ? C12 C17 1.401(8) . ? C13 C14 1.411(10) . ? C14 C15 1.398(11) . ? C15 C16 1.322(10) . ? C16 C17 1.385(10) . ? C18 C23 1.377(10) . ? C18 C19 1.429(10) . ? C19 C20 1.386(10) . ? C20 C21 1.35(2) . ? C21 C22 1.43(2) . ? C22 C23 1.422(10) . ? 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 Cl5 Zr1 Cl2 100.51(7) . . ? Cl5 Zr1 Cl4 93.68(8) . . ? Cl2 Zr1 Cl4 92.09(7) . . ? Cl5 Zr1 Cl1 92.54(8) . . ? Cl2 Zr1 Cl1 89.28(7) . . ? Cl4 Zr1 Cl1 173.28(7) . . ? Cl5 Zr1 Cl3 89.62(6) . . ? Cl2 Zr1 Cl3 169.56(6) . . ? Cl4 Zr1 Cl3 89.74(6) . . ? Cl1 Zr1 Cl3 87.75(6) . . ? Cl5 Zr1 Cl3 166.74(6) . 3_665 ? Cl2 Zr1 Cl3 92.71(6) . 3_665 ? Cl4 Zr1 Cl3 86.76(7) . 3_665 ? Cl1 Zr1 Cl3 86.60(6) . 3_665 ? Cl3 Zr1 Cl3 77.12(5) . 3_665 ? Zr1 Cl3 Zr1 102.88(5) . 3_665 ? N1 P1 C18 108.8(3) . . ? N1 P1 C12 111.7(3) . . ? C18 P1 C12 110.3(3) . . ? N1 P1 C1 110.5(3) . . ? C18 P1 C1 108.1(3) . . ? C12 P1 C1 107.3(3) . . ? N1 Si1 C25 107.8(3) . . ? N1 Si1 C24 108.4(3) . . ? C25 Si1 C24 111.3(5) . . ? N1 Si1 C26 108.4(5) . . ? C25 Si1 C26 110.6(5) . . ? C24 Si1 C26 110.3(6) . . ? P1 N1 Si1 130.8(3) . . ? C2 C1 P1 111.6(4) . . ? C3 C2 C7 117.7(5) . . ? C3 C2 C1 121.1(5) . . ? C7 C2 C1 121.2(5) . . ? C2 C3 C4 121.1(5) . . ? C5 C4 C3 122.4(5) . . ? C4 C5 C6 117.3(5) . . ? C4 C5 C8 122.1(5) . . ? C6 C5 C8 120.5(5) . . ? C7 C6 C5 120.2(5) . . ? C6 C7 C2 121.3(5) . . ? C9 C8 C5 110.2(7) . . ? C9 C8 C10 113.8(12) . . ? C5 C8 C10 110.2(6) . . ? C9 C8 C11 108.5(14) . . ? C5 C8 C11 108.7(6) . . ? C10 C8 C11 105.1(8) . . ? C13 C12 C17 119.2(6) . . ? C13 C12 P1 120.6(5) . . ? C17 C12 P1 120.1(5) . . ? C12 C13 C14 118.8(7) . . ? C15 C14 C13 120.8(7) . . ? C16 C15 C14 119.3(7) . . ? C15 C16 C17 121.8(7) . . ? C16 C17 C12 120.2(6) . . ? C23 C18 C19 120.1(6) . . ? C23 C18 P1 123.3(6) . . ? C19 C18 P1 116.6(5) . . ? C20 C19 C18 119.4(9) . . ? C21 C20 C19 119.9(10) . . ? C20 C21 C22 123.4(8) . . ? C23 C22 C21 115.8(9) . . ? C18 C23 C22 121.2(9) . . ? _refine_diff_density_max 0.658 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.167 #===END data_ms340 _database_code_CSD 154072 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H45 Cl7 N2 P2 Si2 Zr' _chemical_formula_weight 939.21 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 22.6760(10) _cell_length_b 9.5021(5) _cell_length_c 21.3807(7) _cell_angle_alpha 90.00 _cell_angle_beta 113.031(3) _cell_angle_gamma 90.00 _cell_volume 4239.7(3) _cell_formula_units_Z 4 _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 0.26 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.860 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8073 _exptl_absorpt_correction_T_max 0.9113 _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 29078 _diffrn_reflns_av_R_equivalents 0.0677 _diffrn_reflns_av_sigmaI/netI 0.0689 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8215 _reflns_number_gt 4228 _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^)+(0.0000P)^2^+56.0512P] 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 0.0014(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8215 _refine_ls_number_parameters 459 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.1608 _refine_ls_R_factor_gt 0.1024 _refine_ls_wR_factor_ref 0.2288 _refine_ls_wR_factor_gt 0.2000 _refine_ls_goodness_of_fit_ref 1.198 _refine_ls_restrained_S_all 1.196 _refine_ls_shift/su_max 0.157 _refine_ls_shift/su_mean 0.036 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 0.99990(7) 0.88057(8) 0.75009(7) 0.0239(2) Uani 1 1 d . . . Cl1 Cl 1.0005(3) 0.6199(2) 0.7498(3) 0.0492(6) Uani 1 1 d . A . Cl2 Cl 0.94395(17) 0.8737(5) 0.82787(16) 0.0503(10) Uani 1 1 d . A . Cl3 Cl 1.05584(16) 0.8746(5) 0.67207(16) 0.0511(10) Uani 1 1 d . A . N1 N 1.0882(5) 0.9483(12) 0.8331(5) 0.036(3) Uani 1 1 d . A . Si1 Si 1.14780(19) 0.8368(4) 0.88682(18) 0.0383(9) Uani 1 1 d . . . C11 C 1.2144(7) 0.9330(13) 0.9532(6) 0.039(3) Uani 1 1 d . A . H11A H 1.2392 0.9845 0.9319 0.058 Uiso 1 1 calc R . . H11B H 1.2424 0.8657 0.9863 0.058 Uiso 1 1 calc R . . H11C H 1.1968 0.9996 0.9764 0.058 Uiso 1 1 calc R . . C12 C 1.1829(7) 0.7326(11) 0.8358(7) 0.037(3) Uani 1 1 d . A . H12A H 1.1498 0.6714 0.8042 0.056 Uiso 1 1 calc R . . H12B H 1.2183 0.6749 0.8663 0.056 Uiso 1 1 calc R . . H12C H 1.1989 0.7968 0.8102 0.056 Uiso 1 1 calc R . . C13 C 1.1110(7) 0.7152(14) 0.9289(7) 0.043(3) Uani 1 1 d . A . H13A H 1.0969 0.7685 0.9597 0.065 Uiso 1 1 calc R . . H13B H 1.1426 0.6445 0.9548 0.065 Uiso 1 1 calc R . . H13C H 1.0741 0.6683 0.8944 0.065 Uiso 1 1 calc R . . P1 P 1.08997(16) 1.1198(4) 0.83416(15) 0.0310(7) Uani 1 1 d D A . C111 C 1.1671(5) 1.1839(11) 0.8395(6) 0.033(3) Uani 1 1 d D . . C112 C 1.2054(7) 1.2832(13) 0.8855(7) 0.041(3) Uani 1 1 d D A . H112 H 1.1913 1.3262 0.9173 0.049 Uiso 1 1 calc R . . C113 C 1.2659(7) 1.3196(12) 0.8845(7) 0.046(4) Uani 1 1 d D . . H113 H 1.2938 1.3836 0.9168 0.055 Uiso 1 1 calc R A . C114 C 1.2832(7) 1.2576(15) 0.8341(7) 0.044(3) Uani 1 1 d D A . H114 H 1.3219 1.2865 0.8304 0.052 Uiso 1 1 calc R . . C115 C 1.2460(7) 1.1566(14) 0.7900(7) 0.040(3) Uani 1 1 d D . . H115 H 1.2604 1.1102 0.7592 0.048 Uiso 1 1 calc R A . C116 C 1.1883(6) 1.1254(15) 0.7918(6) 0.037(3) Uani 1 1 d D A . H116 H 1.1611 1.0610 0.7593 0.044 Uiso 1 1 calc R . . C121 C 1.0736(4) 1.1944(17) 0.9047(5) 0.043(4) Uani 1 1 d D . . C122 C 1.0670(6) 1.3422(13) 0.9104(8) 0.047(4) Uani 1 1 d D A . H122 H 1.0707 1.4080 0.8786 0.056 Uiso 1 1 calc R . . C123 C 1.0547(7) 1.3811(15) 0.9667(8) 0.051(4) Uani 1 1 d D . . H123 H 1.0481 1.4788 0.9708 0.061 Uiso 1 1 calc R A . C124 C 1.0509(7) 1.2991(14) 1.0162(7) 0.038(3) Uani 1 1 d D A . H124 H 1.0453 1.3371 1.0546 0.046 Uiso 1 1 calc R . . C125 C 1.0556(6) 1.1539(16) 1.0074(7) 0.044(4) Uani 1 1 d D . . H125 H 1.0510 1.0917 1.0400 0.052 Uiso 1 1 calc R A . C126 C 1.0671(6) 1.0952(12) 0.9512(6) 0.028(3) Uani 1 1 d D A . H126 H 1.0702 0.9967 0.9456 0.033 Uiso 1 1 calc R . . C1A C 1.0265(12) 1.127(2) 0.7530(12) 0.025(5) Uani 0.50 1 d PDU A 1 H1A H 1.0443 1.1458 0.7178 0.030 Uiso 0.50 1 calc PR A 1 C2A C 0.9675(10) 1.219(3) 0.7391(11) 0.026(5) Uani 0.50 1 d PDU A 1 H2AA H 0.9741 1.3160 0.7265 0.031 Uiso 0.50 1 calc PR A 1 H2AB H 0.9545 1.2209 0.7782 0.031 Uiso 0.50 1 calc PR A 1 C1B C 1.0355(9) 1.205(3) 0.7598(11) 0.022(5) Uani 0.50 1 d PDU A 2 H1BA H 1.0316 1.3065 0.7680 0.026 Uiso 0.50 1 calc PR A 2 H1BB H 1.0488 1.1939 0.7212 0.026 Uiso 0.50 1 calc PR A 2 C2B C 0.9728(10) 1.127(3) 0.7471(10) 0.019(4) Uani 0.50 1 d PDU A 2 H2B H 0.9563 1.1495 0.7829 0.023 Uiso 0.50 1 calc PR A 2 N2 N 0.9105(5) 0.9499(12) 0.6664(5) 0.037(3) Uani 1 1 d . A . Si2 Si 0.85177(19) 0.8344(4) 0.61327(19) 0.0360(8) Uani 1 1 d . . . C21 C 0.7858(8) 0.9355(17) 0.5473(8) 0.057(4) Uani 1 1 d . A . H21A H 0.7552 0.9674 0.5663 0.085 Uiso 1 1 calc R . . H21B H 0.7639 0.8749 0.5079 0.085 Uiso 1 1 calc R . . H21C H 0.8039 1.0172 0.5331 0.085 Uiso 1 1 calc R . . C22 C 0.8192(9) 0.733(3) 0.6660(10) 0.106(9) Uani 1 1 d . A . H22A H 0.8507 0.6622 0.6924 0.159 Uiso 1 1 calc R . . H22B H 0.7797 0.6851 0.6366 0.159 Uiso 1 1 calc R . . H22C H 0.8099 0.7963 0.6970 0.159 Uiso 1 1 calc R . . C23 C 0.8880(8) 0.7109(16) 0.5695(9) 0.055(4) Uani 1 1 d . A . H23A H 0.8946 0.7607 0.5327 0.082 Uiso 1 1 calc R . . H23B H 0.8590 0.6312 0.5508 0.082 Uiso 1 1 calc R . . H23C H 0.9292 0.6764 0.6023 0.082 Uiso 1 1 calc R . . P2 P 0.90935(15) 1.1193(4) 0.66566(16) 0.0330(8) Uani 1 1 d D A . C211 C 0.9258(3) 1.1879(10) 0.5959(5) 0.020(2) Uani 1 1 d D . . C212 C 0.9322(6) 1.3257(15) 0.5886(7) 0.045(4) Uani 1 1 d D A . H212 H 0.9288 1.3866 0.6223 0.053 Uiso 1 1 calc R . . C213 C 0.9436(7) 1.3869(14) 0.5349(8) 0.046(4) Uani 1 1 d D . . H213 H 0.9469 1.4857 0.5306 0.056 Uiso 1 1 calc R A . C214 C 0.9496(6) 1.2911(14) 0.4879(7) 0.037(3) Uani 1 1 d D A . H214 H 0.9573 1.3261 0.4501 0.044 Uiso 1 1 calc R . . C215 C 0.9449(6) 1.1496(11) 0.4945(6) 0.027(3) Uani 1 1 d D . . H215 H 0.9498 1.0860 0.4626 0.033 Uiso 1 1 calc R A . C216 C 0.9329(6) 1.1027(14) 0.5480(5) 0.033(3) Uani 1 1 d D A . H216 H 0.9292 1.0040 0.5526 0.040 Uiso 1 1 calc R . . C221 C 0.8329(6) 1.1826(12) 0.6613(5) 0.031(3) Uani 1 1 d D . . C222 C 0.7964(7) 1.2833(14) 0.6154(7) 0.047(4) Uani 1 1 d D A . H222 H 0.8115 1.3234 0.5837 0.057 Uiso 1 1 calc R . . C223 C 0.7379(7) 1.325(2) 0.6156(9) 0.081(6) Uani 1 1 d D . . H223 H 0.7142 1.3957 0.5842 0.097 Uiso 1 1 calc R A . C224 C 0.7134(8) 1.2705(18) 0.6586(8) 0.060(5) Uani 1 1 d D A . H224 H 0.6726 1.2986 0.6568 0.072 Uiso 1 1 calc R . . C225 C 0.7506(6) 1.1699(15) 0.7063(6) 0.038(3) Uani 1 1 d D . . H225 H 0.7350 1.1312 0.7379 0.045 Uiso 1 1 calc R A . C226 C 0.8105(7) 1.1261(15) 0.7079(6) 0.040(3) Uani 1 1 d D A . H226 H 0.8353 1.0587 0.7404 0.048 Uiso 1 1 calc R . . C1S C 1.1445(10) 1.3718(13) 0.6359(12) 0.089(7) Uani 1 1 d D . . H1SA H 1.1906 1.3724 0.6660 0.106 Uiso 1 1 calc R . . H1SB H 1.1395 1.4240 0.5940 0.106 Uiso 1 1 calc R . . Cl1S Cl 1.1199(2) 1.1973(4) 0.6142(2) 0.0642(12) Uani 1 1 d D . . Cl2S Cl 1.1018(2) 1.4590(5) 0.6766(2) 0.0654(12) Uani 1 1 d D . . C2S C 0.8537(8) 1.3688(13) 0.8620(10) 0.066(5) Uani 1 1 d D . . H2SA H 0.8083 1.3644 0.8300 0.079 Uiso 1 1 calc R . . H2SB H 0.8558 1.4229 0.9024 0.079 Uiso 1 1 calc R . . Cl3S Cl 0.8816(3) 1.1978(6) 0.8871(2) 0.0806(15) Uani 1 1 d D . . Cl4S Cl 0.8977(2) 1.4574(5) 0.8230(2) 0.0669(12) Uani 1 1 d D . . 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 0.0328(4) 0.0191(4) 0.0205(4) 0.0004(5) 0.0112(3) 0.0005(6) Cl1 0.0600(15) 0.0233(10) 0.0737(17) 0.0017(19) 0.0363(13) 0.0005(19) Cl2 0.035(2) 0.092(3) 0.0281(16) -0.0018(17) 0.0168(15) 0.0051(19) Cl3 0.0281(18) 0.099(3) 0.0297(17) 0.0201(18) 0.0153(15) -0.0049(19) N1 0.026(6) 0.058(7) 0.023(5) -0.009(5) 0.010(5) -0.015(5) Si1 0.033(2) 0.052(2) 0.0333(19) -0.0086(17) 0.0174(17) -0.0042(17) C11 0.037(8) 0.033(7) 0.030(7) -0.001(5) -0.004(6) -0.004(6) C12 0.053(9) 0.019(5) 0.052(8) -0.008(5) 0.033(7) 0.009(5) C13 0.050(9) 0.036(7) 0.043(8) -0.003(6) 0.018(7) -0.012(7) P1 0.0279(18) 0.0451(19) 0.0232(16) 0.0076(14) 0.0136(14) 0.0062(15) C111 0.022(6) 0.035(6) 0.039(7) 0.007(6) 0.010(5) 0.000(5) C112 0.036(8) 0.040(7) 0.043(8) -0.002(6) 0.013(6) -0.002(6) C113 0.071(10) 0.022(6) 0.053(8) -0.019(6) 0.033(8) -0.031(6) C114 0.037(8) 0.050(8) 0.057(8) 0.012(7) 0.033(7) -0.004(6) C115 0.046(8) 0.040(7) 0.037(7) 0.006(6) 0.020(6) 0.006(6) C116 0.023(7) 0.053(8) 0.037(7) 0.004(6) 0.015(6) -0.004(6) C121 0.021(7) 0.086(10) 0.017(5) 0.010(6) 0.003(5) -0.002(7) C122 0.057(10) 0.019(6) 0.080(11) 0.017(6) 0.044(9) 0.022(6) C123 0.053(10) 0.040(8) 0.071(10) 0.009(8) 0.036(9) 0.015(7) C124 0.047(9) 0.042(7) 0.031(6) -0.012(6) 0.021(6) -0.014(6) C125 0.042(8) 0.061(9) 0.034(7) -0.026(6) 0.022(6) -0.014(7) C126 0.035(7) 0.019(5) 0.032(7) -0.006(5) 0.016(6) 0.000(5) C1A 0.039(16) 0.008(11) 0.027(13) 0.003(10) 0.013(11) 0.000(11) C2A 0.039(15) 0.023(12) 0.024(12) 0.002(9) 0.023(11) -0.001(10) C1B 0.012(12) 0.027(13) 0.026(12) -0.001(11) 0.008(9) -0.004(9) C2B 0.015(12) 0.028(14) 0.017(11) 0.006(9) 0.008(8) -0.003(10) N2 0.038(7) 0.054(7) 0.026(5) 0.001(5) 0.020(5) 0.003(5) Si2 0.037(2) 0.0368(19) 0.037(2) 0.0100(16) 0.0176(17) 0.0098(16) C21 0.055(11) 0.055(9) 0.052(10) -0.001(8) 0.012(8) 0.005(8) C22 0.039(10) 0.22(3) 0.059(11) 0.046(14) 0.021(9) 0.035(13) C23 0.050(10) 0.050(9) 0.079(11) -0.006(8) 0.041(9) -0.001(8) P2 0.0183(17) 0.057(2) 0.0236(16) -0.0055(15) 0.0082(13) -0.0042(15) C211 0.022(6) 0.010(4) 0.033(6) 0.002(4) 0.016(5) -0.007(4) C212 0.049(9) 0.053(9) 0.048(8) -0.022(7) 0.037(7) -0.008(7) C213 0.067(11) 0.029(6) 0.068(10) -0.013(7) 0.052(9) -0.011(7) C214 0.031(7) 0.035(7) 0.053(8) 0.004(6) 0.026(6) -0.007(5) C215 0.035(7) 0.021(5) 0.031(6) -0.021(5) 0.017(5) -0.008(5) C216 0.034(8) 0.044(7) 0.020(6) 0.002(5) 0.009(5) 0.007(6) C221 0.032(7) 0.042(7) 0.028(6) -0.014(5) 0.020(5) -0.015(6) C222 0.050(10) 0.045(8) 0.058(9) 0.006(7) 0.033(8) 0.007(7) C223 0.020(7) 0.144(18) 0.081(13) 0.022(12) 0.021(8) 0.008(9) C224 0.032(8) 0.078(11) 0.067(10) 0.029(9) 0.015(7) 0.017(8) C225 0.014(6) 0.066(9) 0.037(7) 0.003(6) 0.015(5) 0.007(6) C226 0.039(8) 0.056(8) 0.027(6) -0.002(6) 0.016(6) -0.007(7) C1S 0.092(16) 0.048(10) 0.139(19) 0.023(11) 0.060(15) 0.016(11) Cl1S 0.086(3) 0.048(2) 0.055(2) -0.0124(18) 0.023(2) -0.006(2) Cl2S 0.066(3) 0.067(3) 0.062(3) -0.004(2) 0.024(2) -0.003(2) C2S 0.059(11) 0.061(10) 0.095(13) 0.020(10) 0.049(10) 0.011(9) Cl3S 0.083(4) 0.095(4) 0.048(2) -0.003(2) 0.009(2) 0.005(3) Cl4S 0.062(3) 0.070(3) 0.068(3) -0.007(2) 0.026(2) -0.010(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 Zr1 N1 2.189(10) . ? Zr1 N2 2.216(11) . ? Zr1 C1A 2.41(3) . ? Zr1 C2B 2.41(3) . ? Zr1 Cl2 2.456(3) . ? Zr1 Cl3 2.460(3) . ? Zr1 Cl1 2.477(2) . ? Zr1 P1 3.114(4) . ? Zr1 P2 3.118(4) . ? N1 P1 1.630(12) . ? N1 Si1 1.748(12) . ? Si1 C13 1.851(14) . ? Si1 C11 1.858(13) . ? Si1 C12 1.866(11) . ? P1 C1A 1.77(2) . ? P1 C1B 1.78(2) . ? P1 C111 1.813(13) . ? P1 C121 1.831(13) . ? C111 C112 1.394(18) . ? C111 C116 1.402(18) . ? C112 C113 1.423(19) . ? C113 C114 1.413(18) . ? C114 C115 1.38(2) . ? C115 C116 1.357(18) . ? C121 C126 1.418(17) . ? C121 C122 1.42(2) . ? C122 C123 1.39(2) . ? C123 C124 1.34(2) . ? C124 C125 1.40(2) . ? C125 C126 1.439(16) . ? C1A C2A 1.526(17) . ? C2A P2 1.87(2) . ? C1B C2B 1.532(16) . ? C2B P2 1.77(2) . ? N2 P2 1.610(12) . ? N2 Si2 1.755(12) . ? Si2 C22 1.85(2) . ? Si2 C21 1.870(16) . ? Si2 C23 1.878(15) . ? P2 C211 1.796(10) . ? P2 C221 1.803(13) . ? C211 C212 1.333(18) . ? C211 C216 1.363(16) . ? C212 C213 1.398(19) . ? C213 C214 1.403(18) . ? C214 C215 1.360(17) . ? C215 C216 1.351(16) . ? C221 C226 1.391(17) . ? C221 C222 1.389(19) . ? C222 C223 1.39(2) . ? C223 C224 1.35(2) . ? C224 C225 1.41(2) . ? C225 C226 1.408(18) . ? C1S Cl2S 1.746(12) . ? C1S Cl1S 1.753(12) . ? C2S Cl4S 1.745(10) . ? C2S Cl3S 1.750(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zr1 N2 145.6(3) . . ? N1 Zr1 C1A 63.5(6) . . ? N2 Zr1 C1A 82.7(6) . . ? N1 Zr1 C2B 83.1(6) . . ? N2 Zr1 C2B 63.1(6) . . ? C1A Zr1 C2B 28.2(5) . . ? N1 Zr1 Cl2 90.6(3) . . ? N2 Zr1 Cl2 90.2(3) . . ? C1A Zr1 Cl2 101.5(6) . . ? C2B Zr1 Cl2 81.4(5) . . ? N1 Zr1 Cl3 90.3(3) . . ? N2 Zr1 Cl3 90.6(3) . . ? C1A Zr1 Cl3 81.3(6) . . ? C2B Zr1 Cl3 101.4(5) . . ? Cl2 Zr1 Cl3 177.15(11) . . ? N1 Zr1 Cl1 107.0(3) . . ? N2 Zr1 Cl1 107.4(3) . . ? C1A Zr1 Cl1 165.7(6) . . ? C2B Zr1 Cl1 166.1(5) . . ? Cl2 Zr1 Cl1 88.85(16) . . ? Cl3 Zr1 Cl1 88.31(16) . . ? N1 Zr1 P1 29.8(3) . . ? N2 Zr1 P1 115.8(3) . . ? C1A Zr1 P1 34.5(6) . . ? C2B Zr1 P1 53.9(5) . . ? Cl2 Zr1 P1 91.41(12) . . ? Cl3 Zr1 P1 90.71(12) . . ? Cl1 Zr1 P1 136.77(15) . . ? N1 Zr1 P2 116.2(3) . . ? N2 Zr1 P2 29.4(3) . . ? C1A Zr1 P2 53.9(6) . . ? C2B Zr1 P2 34.5(5) . . ? Cl2 Zr1 P2 90.79(12) . . ? Cl3 Zr1 P2 91.24(11) . . ? Cl1 Zr1 P2 136.79(15) . . ? P1 Zr1 P2 86.43(6) . . ? P1 N1 Si1 126.0(6) . . ? P1 N1 Zr1 108.4(6) . . ? Si1 N1 Zr1 125.5(6) . . ? N1 Si1 C13 108.6(6) . . ? N1 Si1 C11 113.1(6) . . ? C13 Si1 C11 108.8(6) . . ? N1 Si1 C12 109.5(6) . . ? C13 Si1 C12 109.2(6) . . ? C11 Si1 C12 107.6(7) . . ? N1 P1 C1A 90.9(9) . . ? N1 P1 C1B 115.9(9) . . ? C1A P1 C1B 25.1(9) . . ? N1 P1 C111 110.8(5) . . ? C1A P1 C111 116.4(9) . . ? C1B P1 C111 102.7(7) . . ? N1 P1 C121 112.8(6) . . ? C1A P1 C121 116.4(8) . . ? C1B P1 C121 105.4(9) . . ? C111 P1 C121 108.6(5) . . ? N1 P1 Zr1 41.8(4) . . ? C1A P1 Zr1 50.4(8) . . ? C1B P1 Zr1 75.4(8) . . ? C111 P1 Zr1 132.9(4) . . ? C121 P1 Zr1 117.3(4) . . ? C112 C111 C116 119.0(12) . . ? C112 C111 P1 126.3(10) . . ? C116 C111 P1 114.7(10) . . ? C111 C112 C113 119.6(12) . . ? C114 C113 C112 117.8(12) . . ? C115 C114 C113 122.3(12) . . ? C116 C115 C114 118.2(13) . . ? C115 C116 C111 122.9(13) . . ? C126 C121 C122 123.5(12) . . ? C126 C121 P1 115.5(11) . . ? C122 C121 P1 121.0(10) . . ? C123 C122 C121 113.6(12) . . ? C124 C123 C122 128.7(14) . . ? C123 C124 C125 115.7(13) . . ? C124 C125 C126 122.8(13) . . ? C121 C126 C125 115.5(12) . . ? C2A C1A P1 121.7(17) . . ? C2A C1A Zr1 111.2(19) . . ? P1 C1A Zr1 95.1(9) . . ? C1A C2A P2 98.6(17) . . ? C2B C1B P1 102.1(17) . . ? C1B C2B P2 122.3(16) . . ? C1B C2B Zr1 104.9(18) . . ? P2 C2B Zr1 95.1(9) . . ? P2 N2 Si2 127.8(7) . . ? P2 N2 Zr1 108.1(6) . . ? Si2 N2 Zr1 124.0(6) . . ? N2 Si2 C22 108.4(8) . . ? N2 Si2 C21 110.3(6) . . ? C22 Si2 C21 109.7(8) . . ? N2 Si2 C23 110.1(6) . . ? C22 Si2 C23 109.5(10) . . ? C21 Si2 C23 108.8(8) . . ? N2 P2 C2B 91.5(9) . . ? N2 P2 C211 111.3(5) . . ? C2B P2 C211 116.7(7) . . ? N2 P2 C221 110.2(5) . . ? C2B P2 C221 115.6(8) . . ? C211 P2 C221 110.1(5) . . ? N2 P2 C2A 119.7(8) . . ? C2B P2 C2A 28.2(9) . . ? C211 P2 C2A 101.9(8) . . ? C221 P2 C2A 102.9(7) . . ? N2 P2 Zr1 42.5(4) . . ? C2B P2 Zr1 50.4(8) . . ? C211 P2 Zr1 116.2(3) . . ? C221 P2 Zr1 132.4(4) . . ? C2A P2 Zr1 78.0(7) . . ? C212 C211 C216 116.5(11) . . ? C212 C211 P2 121.4(9) . . ? C216 C211 P2 122.1(8) . . ? C211 C212 C213 124.6(12) . . ? C212 C213 C214 114.9(12) . . ? C215 C214 C213 122.1(12) . . ? C214 C215 C216 117.7(11) . . ? C215 C216 C211 124.2(12) . . ? C226 C221 C222 119.2(12) . . ? C226 C221 P2 116.6(11) . . ? C222 C221 P2 124.2(9) . . ? C223 C222 C221 120.2(14) . . ? C224 C223 C222 122.6(17) . . ? C223 C224 C225 117.7(15) . . ? C226 C225 C224 121.0(12) . . ? C221 C226 C225 119.2(13) . . ? Cl2S C1S Cl1S 113.4(9) . . ? Cl4S C2S Cl3S 112.9(7) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.872 _refine_diff_density_min -0.621 _refine_diff_density_rms 0.121