# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'John Arnold' _publ_contact_author_address ; Department of Chemistry University of California Berkeley CA 94720 UNITED STATES OF AMERICA ; _publ_contact_author_email ARNOLD@BERKELEY.EDU _publ_section_title ; Transition Metal Dinitrogen Complexes Supported by a Versatile Tetradentate Monoanionic Ligand ; loop_ _publ_author_name 'John Arnold' 'Wayne A. Chomitz' # Attachment 'freds.txt' data_freds _database_code_depnum_ccdc_archive 'CCDC 652414' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C52 H124 N6 P4 Si4 Ti2), 1.5(C5 H12)' _chemical_formula_sum 'C59.50 H142 N6 P4 Si4 Ti2' _chemical_formula_weight 1273.83 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' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.224(4) _cell_length_b 18.899(4) _cell_length_c 23.297(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.599(2) _cell_angle_gamma 90.00 _cell_volume 7974(3) _cell_formula_units_Z 4 _cell_measurement_temperature 148(2) _cell_measurement_reflns_used 3235 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 19.4 _exptl_crystal_description 'hexagonal plate' _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.061 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2804 _exptl_absorpt_coefficient_mu 0.376 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 148(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 'SMART 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 35244 _diffrn_reflns_av_R_equivalents 0.0856 _diffrn_reflns_av_sigmaI/netI 0.1331 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 24.72 _reflns_number_total 13477 _reflns_number_gt 6508 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054d' _computing_cell_refinement 'Bruker SAINT v7.07' _computing_data_reduction 'Bruker SAINT v7.07' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. There are two pentane solvent molecules in the unit cell. One molecule is set to fully occupany, and the thermal parameters are large due to wiggling for the solvent molecule up and down. The second molecule lies on an inversion center. The molecule is disordered over two positions where one is shifted over by one carbon but still lies on top of the other. The first carbon in this solvent molecule is set to half occupancy and the other two are set to full occupancy in order to model this disorder. ; _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^)+(0.0600P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13477 _refine_ls_number_parameters 680 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1506 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1431 _refine_ls_wR_factor_gt 0.1176 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.981 _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 0.41317(4) 0.62705(4) 0.19788(3) 0.0308(2) Uani 1 1 d . . . Ti2 Ti 0.15818(4) 0.67385(4) 0.17728(3) 0.0342(2) Uani 1 1 d . . . Si1 Si 0.56680(7) 0.62760(7) 0.27931(6) 0.0403(3) Uani 1 1 d . . . Si2 Si 0.45766(7) 0.74947(7) 0.09192(6) 0.0422(3) Uani 1 1 d . . . Si3 Si 0.06503(7) 0.72288(7) 0.24676(6) 0.0440(4) Uani 1 1 d . . . Si4 Si 0.05868(7) 0.50309(8) 0.13802(7) 0.0559(4) Uani 1 1 d . . . P1 P 0.37564(6) 0.49518(6) 0.18099(5) 0.0356(3) Uani 1 1 d . . . P2 P 0.67017(7) 0.51227(7) 0.12443(6) 0.0448(3) Uani 1 1 d . . . P3 P 0.15759(6) 0.77411(6) 0.09930(5) 0.0400(3) Uani 1 1 d . . . P4 P -0.15634(8) 0.80186(8) 0.05218(6) 0.0611(4) Uani 1 1 d . . . N1 N 0.48510(17) 0.66497(17) 0.27598(14) 0.0340(8) Uani 1 1 d . . . N2 N 0.53146(17) 0.55963(17) 0.22431(14) 0.0333(9) Uani 1 1 d . . . N3 N 0.14991(17) 0.68704(18) 0.26068(15) 0.0373(9) Uani 1 1 d . . . N4 N 0.04946(18) 0.7520(2) 0.17074(15) 0.0426(9) Uani 1 1 d . . . N5 N 0.32091(19) 0.64789(16) 0.19313(14) 0.0319(8) Uani 1 1 d . . . N6 N 0.25235(18) 0.65466(17) 0.18765(14) 0.0318(8) Uani 1 1 d . . . C1 C 0.4766(2) 0.7146(2) 0.32295(19) 0.0398(11) Uani 1 1 d . . . C2 C 0.5464(2) 0.7580(2) 0.3524(2) 0.0578(14) Uani 1 1 d . . . H2A H 0.5581 0.7852 0.3210 0.087 Uiso 1 1 calc R . . H2B H 0.5875 0.7262 0.3728 0.087 Uiso 1 1 calc R . . H2C H 0.5384 0.7905 0.3824 0.087 Uiso 1 1 calc R . . C3 C 0.4593(3) 0.6730(3) 0.3724(2) 0.0622(14) Uani 1 1 d . . . H3A H 0.4144 0.6449 0.3540 0.093 Uiso 1 1 calc R . . H3B H 0.4516 0.7058 0.4023 0.093 Uiso 1 1 calc R . . H3C H 0.5006 0.6414 0.3927 0.093 Uiso 1 1 calc R . . C4 C 0.4138(2) 0.7658(2) 0.2935(2) 0.0513(13) Uani 1 1 d . . . H4A H 0.4247 0.7929 0.2617 0.077 Uiso 1 1 calc R . . H4B H 0.4083 0.7984 0.3245 0.077 Uiso 1 1 calc R . . H4C H 0.3678 0.7393 0.2755 0.077 Uiso 1 1 calc R . . C5 C 0.6255(2) 0.5866(3) 0.3531(2) 0.0583(14) Uani 1 1 d . . . H5A H 0.6765 0.6032 0.3632 0.087 Uiso 1 1 calc R . . H5B H 0.6241 0.5350 0.3490 0.087 Uiso 1 1 calc R . . H5C H 0.6065 0.6004 0.3856 0.087 Uiso 1 1 calc R . . C6 C 0.6305(2) 0.6853(2) 0.2548(2) 0.0581(14) Uani 1 1 d . . . H6A H 0.6804 0.6821 0.2847 0.087 Uiso 1 1 calc R . . H6B H 0.6133 0.7344 0.2519 0.087 Uiso 1 1 calc R . . H6C H 0.6312 0.6696 0.2149 0.087 Uiso 1 1 calc R . . C7 C 0.5211(2) 0.4916(2) 0.25202(18) 0.0372(11) Uani 1 1 d . . . H7A H 0.5077 0.5015 0.2887 0.045 Uiso 1 1 calc R . . H7B H 0.5686 0.4656 0.2653 0.045 Uiso 1 1 calc R . . C8 C 0.4620(2) 0.4446(2) 0.20904(19) 0.0387(11) Uani 1 1 d . . . H8A H 0.4547 0.4018 0.2308 0.046 Uiso 1 1 calc R . . H8B H 0.4774 0.4295 0.1744 0.046 Uiso 1 1 calc R . . C9 C 0.3205(2) 0.4660(2) 0.2278(2) 0.0439(12) Uani 1 1 d . . . H9A H 0.2751 0.4961 0.2162 0.053 Uiso 1 1 calc R . . C10 C 0.2947(3) 0.3891(2) 0.2189(2) 0.0641(15) Uani 1 1 d . . . H10A H 0.2660 0.3786 0.2455 0.096 Uiso 1 1 calc R . . H10B H 0.3378 0.3578 0.2291 0.096 Uiso 1 1 calc R . . H10C H 0.2639 0.3817 0.1763 0.096 Uiso 1 1 calc R . . C11 C 0.3623(3) 0.4803(2) 0.2948(2) 0.0518(13) Uani 1 1 d . . . H11A H 0.3325 0.4647 0.3193 0.078 Uiso 1 1 calc R . . H11B H 0.3722 0.5311 0.3009 0.078 Uiso 1 1 calc R . . H11C H 0.4091 0.4544 0.3073 0.078 Uiso 1 1 calc R . . C12 C 0.3249(2) 0.4641(2) 0.10319(19) 0.0450(12) Uani 1 1 d . . . H12A H 0.3067 0.4151 0.1062 0.054 Uiso 1 1 calc R . . C13 C 0.2578(2) 0.5120(3) 0.0769(2) 0.0608(15) Uani 1 1 d . . . H13A H 0.2296 0.4967 0.0354 0.091 Uiso 1 1 calc R . . H13B H 0.2742 0.5610 0.0760 0.091 Uiso 1 1 calc R . . H13C H 0.2264 0.5092 0.1024 0.091 Uiso 1 1 calc R . . C14 C 0.3713(3) 0.4613(3) 0.0621(2) 0.0577(14) Uani 1 1 d . . . H14A H 0.3410 0.4445 0.0217 0.086 Uiso 1 1 calc R . . H14B H 0.4128 0.4289 0.0795 0.086 Uiso 1 1 calc R . . H14C H 0.3901 0.5088 0.0586 0.086 Uiso 1 1 calc R . . C15 C 0.5619(2) 0.5504(2) 0.17420(19) 0.0402(11) Uani 1 1 d . . . H15A H 0.5676 0.5978 0.1583 0.048 Uiso 1 1 calc R . . H15B H 0.5251 0.5243 0.1408 0.048 Uiso 1 1 calc R . . C16 C 0.6356(2) 0.5118(2) 0.18989(18) 0.0402(11) Uani 1 1 d . . . H16A H 0.6295 0.4623 0.2013 0.048 Uiso 1 1 calc R . . H16B H 0.6723 0.5350 0.2253 0.048 Uiso 1 1 calc R . . C17 C 0.7701(3) 0.5234(3) 0.1624(3) 0.0710(16) Uani 1 1 d . . . H17A H 0.7934 0.5164 0.1303 0.085 Uiso 1 1 calc R . . C18 C 0.8093(3) 0.4741(3) 0.2138(3) 0.0839(19) Uani 1 1 d . . . H18A H 0.8619 0.4861 0.2296 0.126 Uiso 1 1 calc R . . H18B H 0.8033 0.4253 0.1989 0.126 Uiso 1 1 calc R . . H18C H 0.7882 0.4790 0.2465 0.126 Uiso 1 1 calc R . . C19 C 0.7853(3) 0.6008(3) 0.1836(3) 0.102(2) Uani 1 1 d . . . H19A H 0.8385 0.6076 0.2038 0.153 Uiso 1 1 calc R . . H19B H 0.7593 0.6117 0.2123 0.153 Uiso 1 1 calc R . . H19C H 0.7677 0.6323 0.1483 0.153 Uiso 1 1 calc R . . C20 C 0.6624(3) 0.4169(2) 0.1044(2) 0.0542(13) Uani 1 1 d . . . H20A H 0.6814 0.3886 0.1428 0.065 Uiso 1 1 calc R . . C21 C 0.5813(3) 0.3986(3) 0.0727(2) 0.0668(15) Uani 1 1 d . . . H21A H 0.5767 0.3482 0.0619 0.100 Uiso 1 1 calc R . . H21B H 0.5614 0.4271 0.0357 0.100 Uiso 1 1 calc R . . H21C H 0.5535 0.4086 0.1002 0.100 Uiso 1 1 calc R . . C22 C 0.7090(3) 0.3992(3) 0.0641(2) 0.0740(17) Uani 1 1 d . . . H22A H 0.7043 0.3486 0.0540 0.111 Uiso 1 1 calc R . . H22B H 0.7609 0.4104 0.0860 0.111 Uiso 1 1 calc R . . H22C H 0.6916 0.4271 0.0265 0.111 Uiso 1 1 calc R . . C23 C 0.4179(2) 0.6688(2) 0.11270(18) 0.0387(11) Uani 1 1 d . . . H23A H 0.4406 0.6300 0.0965 0.046 Uiso 1 1 calc R . . H23B H 0.3655 0.6702 0.0860 0.046 Uiso 1 1 calc R . . C24 C 0.3949(3) 0.7897(2) 0.0194(2) 0.0567(14) Uani 1 1 d . . . H24A H 0.3467 0.7993 0.0234 0.085 Uiso 1 1 calc R . . H24B H 0.3888 0.7567 -0.0144 0.085 Uiso 1 1 calc R . . H24C H 0.4165 0.8340 0.0114 0.085 Uiso 1 1 calc R . . C25 C 0.4728(3) 0.8199(2) 0.1506(2) 0.0595(14) Uani 1 1 d . . . H25A H 0.5054 0.8020 0.1899 0.089 Uiso 1 1 calc R . . H25B H 0.4253 0.8338 0.1542 0.089 Uiso 1 1 calc R . . H25C H 0.4958 0.8611 0.1386 0.089 Uiso 1 1 calc R . . C26 C 0.5473(3) 0.7335(3) 0.0786(2) 0.0692(16) Uani 1 1 d . . . H26A H 0.5828 0.7124 0.1152 0.104 Uiso 1 1 calc R . . H26B H 0.5668 0.7785 0.0697 0.104 Uiso 1 1 calc R . . H26C H 0.5391 0.7012 0.0441 0.104 Uiso 1 1 calc R . . C27 C 0.2012(2) 0.6703(3) 0.3229(2) 0.0438(12) Uani 1 1 d . . . C28 C 0.2525(2) 0.6102(2) 0.3207(2) 0.0531(13) Uani 1 1 d . . . H28A H 0.2799 0.6231 0.2936 0.080 Uiso 1 1 calc R . . H28B H 0.2235 0.5674 0.3054 0.080 Uiso 1 1 calc R . . H28C H 0.2873 0.6014 0.3617 0.080 Uiso 1 1 calc R . . C29 C 0.2463(3) 0.7363(3) 0.3487(2) 0.0592(14) Uani 1 1 d . . . H29A H 0.2728 0.7514 0.3215 0.089 Uiso 1 1 calc R . . H29B H 0.2819 0.7258 0.3891 0.089 Uiso 1 1 calc R . . H29C H 0.2133 0.7743 0.3522 0.089 Uiso 1 1 calc R . . C30 C 0.1599(3) 0.6476(3) 0.3660(2) 0.0660(16) Uani 1 1 d . . . H30A H 0.1259 0.6853 0.3683 0.099 Uiso 1 1 calc R . . H30B H 0.1956 0.6387 0.4067 0.099 Uiso 1 1 calc R . . H30C H 0.1319 0.6043 0.3505 0.099 Uiso 1 1 calc R . . C31 C -0.0093(3) 0.6598(3) 0.2467(2) 0.0702(16) Uani 1 1 d . . . H31A H -0.0380 0.6795 0.2707 0.105 Uiso 1 1 calc R . . H31B H 0.0128 0.6148 0.2647 0.105 Uiso 1 1 calc R . . H31C H -0.0419 0.6517 0.2048 0.105 Uiso 1 1 calc R . . C32 C 0.0553(3) 0.8002(3) 0.2940(2) 0.0602(15) Uani 1 1 d . . . H32A H 0.0136 0.7920 0.3085 0.090 Uiso 1 1 calc R . . H32B H 0.0464 0.8433 0.2692 0.090 Uiso 1 1 calc R . . H32C H 0.1007 0.8056 0.3290 0.090 Uiso 1 1 calc R . . C33 C 0.0750(2) 0.8244(2) 0.1665(2) 0.0465(12) Uani 1 1 d . . . H33A H 0.1207 0.8329 0.2014 0.056 Uiso 1 1 calc R . . H33B H 0.0371 0.8580 0.1700 0.056 Uiso 1 1 calc R . . C34 C 0.0905(2) 0.8398(2) 0.1071(2) 0.0482(12) Uani 1 1 d . . . H34A H 0.1108 0.8881 0.1083 0.058 Uiso 1 1 calc R . . H34B H 0.0442 0.8366 0.0719 0.058 Uiso 1 1 calc R . . C35 C 0.2450(2) 0.8240(2) 0.1180(2) 0.0485(12) Uani 1 1 d . . . H35A H 0.2842 0.7895 0.1175 0.058 Uiso 1 1 calc R . . C36 C 0.2652(3) 0.8518(3) 0.1830(2) 0.0598(14) Uani 1 1 d . . . H36A H 0.3116 0.8784 0.1935 0.090 Uiso 1 1 calc R . . H36B H 0.2713 0.8119 0.2112 0.090 Uiso 1 1 calc R . . H36C H 0.2258 0.8829 0.1861 0.090 Uiso 1 1 calc R . . C37 C 0.2463(3) 0.8837(3) 0.0747(2) 0.0667(15) Uani 1 1 d . . . H37A H 0.2948 0.9066 0.0886 0.100 Uiso 1 1 calc R . . H37B H 0.2081 0.9185 0.0738 0.100 Uiso 1 1 calc R . . H37C H 0.2367 0.8645 0.0337 0.100 Uiso 1 1 calc R . . C38 C 0.1319(2) 0.7560(3) 0.01707(19) 0.0493(13) Uani 1 1 d . . . H38A H 0.1323 0.8019 -0.0042 0.059 Uiso 1 1 calc R . . C39 C 0.0551(3) 0.7236(3) -0.0102(2) 0.0653(15) Uani 1 1 d . . . H39A H 0.0446 0.7149 -0.0537 0.098 Uiso 1 1 calc R . . H39B H 0.0183 0.7562 -0.0046 0.098 Uiso 1 1 calc R . . H39C H 0.0532 0.6787 0.0104 0.098 Uiso 1 1 calc R . . C40 C 0.1893(3) 0.7073(3) 0.0056(2) 0.0633(15) Uani 1 1 d . . . H40A H 0.1754 0.6977 -0.0381 0.095 Uiso 1 1 calc R . . H40B H 0.1915 0.6627 0.0277 0.095 Uiso 1 1 calc R . . H40C H 0.2378 0.7303 0.0200 0.095 Uiso 1 1 calc R . . C41 C -0.0229(2) 0.7376(3) 0.1236(2) 0.0561(14) Uani 1 1 d . . . H41A H -0.0354 0.6873 0.1269 0.067 Uiso 1 1 calc R . . H41B H -0.0176 0.7442 0.0832 0.067 Uiso 1 1 calc R . . C42 C -0.0875(2) 0.7828(3) 0.1262(2) 0.0723(17) Uani 1 1 d . . . H42A H -0.0680 0.8281 0.1465 0.087 Uiso 1 1 calc R . . H42B H -0.1121 0.7581 0.1517 0.087 Uiso 1 1 calc R . . C43 C -0.2175(3) 0.7260(3) 0.0399(3) 0.094(2) Uani 1 1 d . . . H43A H -0.2303 0.7183 0.0777 0.112 Uiso 1 1 calc R . . C44 C -0.2892(4) 0.7398(4) -0.0132(3) 0.153(4) Uani 1 1 d . . . H44A H -0.3215 0.6983 -0.0192 0.229 Uiso 1 1 calc R . . H44B H -0.2776 0.7486 -0.0505 0.229 Uiso 1 1 calc R . . H44C H -0.3144 0.7811 -0.0040 0.229 Uiso 1 1 calc R . . C45 C -0.1802(4) 0.6601(4) 0.0281(4) 0.194(5) Uani 1 1 d . . . H45A H -0.2144 0.6200 0.0215 0.292 Uiso 1 1 calc R . . H45B H -0.1360 0.6504 0.0632 0.292 Uiso 1 1 calc R . . H45C H -0.1661 0.6670 -0.0082 0.292 Uiso 1 1 calc R . . C46 C -0.2115(3) 0.8715(3) 0.0722(3) 0.102(2) Uani 1 1 d . . . H46A H -0.2570 0.8783 0.0358 0.122 Uiso 1 1 calc R . . C47 C -0.2366(4) 0.8561(6) 0.1250(4) 0.199(5) Uani 1 1 d . . . H47A H -0.2652 0.8963 0.1317 0.298 Uiso 1 1 calc R . . H47B H -0.1934 0.8484 0.1616 0.298 Uiso 1 1 calc R . . H47C H -0.2675 0.8136 0.1164 0.298 Uiso 1 1 calc R . . C48 C -0.1691(5) 0.9405(4) 0.0820(6) 0.235(6) Uani 1 1 d . . . H48A H -0.1980 0.9777 0.0927 0.353 Uiso 1 1 calc R . . H48B H -0.1599 0.9537 0.0445 0.353 Uiso 1 1 calc R . . H48C H -0.1219 0.9347 0.1151 0.353 Uiso 1 1 calc R . . C49 C 0.0926(2) 0.5899(2) 0.1222(2) 0.0454(12) Uani 1 1 d . . . H49A H 0.0471 0.6144 0.0971 0.055 Uiso 1 1 calc R . . H49B H 0.1193 0.5782 0.0938 0.055 Uiso 1 1 calc R . . C50 C 0.0821(3) 0.4300(3) 0.0929(3) 0.095(2) Uani 1 1 d . . . H50A H 0.1357 0.4278 0.1026 0.142 Uiso 1 1 calc R . . H50B H 0.0584 0.4392 0.0493 0.142 Uiso 1 1 calc R . . H50C H 0.0643 0.3848 0.1033 0.142 Uiso 1 1 calc R . . C51 C 0.0969(3) 0.4771(3) 0.2199(2) 0.0824(18) Uani 1 1 d . . . H51A H 0.0857 0.5141 0.2450 0.124 Uiso 1 1 calc R . . H51B H 0.1505 0.4712 0.2317 0.124 Uiso 1 1 calc R . . H51C H 0.0745 0.4324 0.2260 0.124 Uiso 1 1 calc R . . C52 C -0.0443(3) 0.5022(3) 0.1163(3) 0.0822(18) Uani 1 1 d . . . H52A H -0.0599 0.5396 0.1385 0.123 Uiso 1 1 calc R . . H52B H -0.0604 0.4562 0.1266 0.123 Uiso 1 1 calc R . . H52C H -0.0666 0.5104 0.0724 0.123 Uiso 1 1 calc R . . C53 C -0.1541(6) 0.7633(7) -0.1575(8) 0.269(8) Uani 1 1 d . . . C54 C -0.1561(9) 0.8459(12) -0.1324(6) 0.251(9) Uani 1 1 d . . . C55 C -0.0811(12) 0.8731(13) -0.1071(10) 0.265(8) Uani 1 1 d . . . C56 C -0.0787(13) 0.9450(12) -0.0928(11) 0.306(11) Uani 1 1 d . . . C57 C 0.0020(11) 0.9627(9) -0.0806(10) 0.298(9) Uani 1 1 d . . . C58 C -0.3570(11) 1.0101(10) 0.0042(9) 0.134(7) Uiso 0.50 1 d P . . C59 C -0.3979(7) 0.9689(9) 0.0184(5) 0.228(7) Uani 1 1 d . . . C60 C -0.4783(10) 0.9897(7) 0.0265(5) 0.259(7) 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 0.0292(5) 0.0289(5) 0.0340(5) -0.0001(4) 0.0100(4) 0.0009(4) Ti2 0.0283(5) 0.0356(5) 0.0380(5) -0.0047(4) 0.0103(4) -0.0015(4) Si1 0.0297(7) 0.0431(8) 0.0446(8) -0.0051(7) 0.0079(6) 0.0018(6) Si2 0.0460(8) 0.0413(8) 0.0406(8) -0.0021(6) 0.0165(6) -0.0078(6) Si3 0.0360(8) 0.0511(9) 0.0491(9) -0.0064(7) 0.0198(6) -0.0014(6) Si4 0.0444(9) 0.0461(9) 0.0745(10) -0.0101(8) 0.0165(8) -0.0101(7) P1 0.0353(7) 0.0301(7) 0.0421(7) 0.0002(6) 0.0139(6) 0.0004(6) P2 0.0461(8) 0.0432(8) 0.0525(8) 0.0071(6) 0.0263(6) 0.0079(6) P3 0.0383(7) 0.0417(8) 0.0407(7) 0.0016(6) 0.0141(6) 0.0077(6) P4 0.0553(9) 0.0618(10) 0.0642(10) -0.0039(8) 0.0176(8) 0.0094(7) N1 0.034(2) 0.034(2) 0.033(2) -0.0048(17) 0.0102(16) 0.0028(17) N2 0.033(2) 0.035(2) 0.035(2) 0.0007(17) 0.0155(17) 0.0008(16) N3 0.032(2) 0.044(2) 0.036(2) -0.0061(18) 0.0110(17) -0.0026(17) N4 0.029(2) 0.048(3) 0.048(2) -0.010(2) 0.0084(18) -0.0015(18) N5 0.034(2) 0.030(2) 0.030(2) -0.0018(16) 0.0080(16) -0.0057(16) N6 0.030(2) 0.032(2) 0.034(2) -0.0033(16) 0.0110(16) -0.0040(16) C1 0.039(3) 0.041(3) 0.039(3) -0.008(2) 0.013(2) 0.000(2) C2 0.051(3) 0.053(3) 0.060(3) -0.019(3) 0.006(3) -0.001(3) C3 0.080(4) 0.067(4) 0.046(3) -0.011(3) 0.029(3) -0.003(3) C4 0.046(3) 0.053(3) 0.051(3) -0.013(3) 0.012(2) 0.009(3) C5 0.050(3) 0.057(4) 0.055(3) -0.008(3) 0.001(3) 0.010(3) C6 0.038(3) 0.053(3) 0.081(4) -0.015(3) 0.017(3) -0.006(2) C7 0.032(3) 0.042(3) 0.040(3) 0.004(2) 0.016(2) 0.010(2) C8 0.046(3) 0.028(3) 0.047(3) 0.002(2) 0.023(2) 0.001(2) C9 0.040(3) 0.039(3) 0.057(3) 0.002(2) 0.022(2) 0.003(2) C10 0.066(4) 0.054(4) 0.084(4) 0.003(3) 0.040(3) -0.013(3) C11 0.059(3) 0.050(3) 0.057(3) 0.012(3) 0.034(3) 0.009(3) C12 0.044(3) 0.037(3) 0.050(3) -0.002(2) 0.010(2) -0.003(2) C13 0.047(3) 0.076(4) 0.051(3) -0.008(3) 0.005(3) 0.001(3) C14 0.060(4) 0.063(4) 0.045(3) -0.007(3) 0.011(3) 0.008(3) C15 0.038(3) 0.034(3) 0.050(3) 0.004(2) 0.017(2) 0.001(2) C16 0.038(3) 0.039(3) 0.042(3) 0.002(2) 0.012(2) 0.007(2) C17 0.057(4) 0.083(5) 0.083(4) -0.008(4) 0.036(3) -0.006(3) C18 0.046(4) 0.115(5) 0.084(4) 0.006(4) 0.013(3) 0.016(3) C19 0.071(4) 0.106(6) 0.135(6) -0.023(5) 0.042(4) -0.036(4) C20 0.072(4) 0.048(3) 0.051(3) 0.004(3) 0.031(3) 0.013(3) C21 0.068(4) 0.063(4) 0.069(4) -0.013(3) 0.023(3) -0.002(3) C22 0.102(5) 0.066(4) 0.074(4) 0.007(3) 0.056(4) 0.024(3) C23 0.032(3) 0.040(3) 0.040(3) -0.001(2) 0.007(2) 0.003(2) C24 0.077(4) 0.042(3) 0.048(3) 0.003(2) 0.016(3) -0.001(3) C25 0.079(4) 0.045(3) 0.052(3) -0.006(3) 0.017(3) -0.016(3) C26 0.061(4) 0.077(4) 0.076(4) 0.005(3) 0.030(3) -0.013(3) C27 0.041(3) 0.049(3) 0.043(3) -0.007(3) 0.016(2) -0.003(3) C28 0.053(3) 0.060(4) 0.045(3) 0.008(3) 0.014(2) 0.011(3) C29 0.060(3) 0.064(4) 0.043(3) -0.007(3) 0.004(3) 0.003(3) C30 0.065(4) 0.083(4) 0.055(3) 0.012(3) 0.028(3) 0.013(3) C31 0.043(3) 0.083(4) 0.091(4) -0.001(3) 0.030(3) -0.007(3) C32 0.062(4) 0.065(4) 0.058(3) -0.004(3) 0.027(3) 0.011(3) C33 0.042(3) 0.049(3) 0.048(3) -0.004(3) 0.015(2) 0.008(3) C34 0.044(3) 0.048(3) 0.052(3) 0.003(2) 0.015(2) 0.013(2) C35 0.047(3) 0.041(3) 0.059(3) 0.002(3) 0.021(3) 0.002(2) C36 0.049(3) 0.055(4) 0.068(4) 0.004(3) 0.010(3) -0.008(3) C37 0.076(4) 0.053(4) 0.080(4) 0.010(3) 0.038(3) -0.004(3) C38 0.051(3) 0.057(3) 0.038(3) 0.002(2) 0.013(2) 0.011(3) C39 0.062(4) 0.087(4) 0.040(3) -0.008(3) 0.008(3) 0.003(3) C40 0.072(4) 0.068(4) 0.055(3) -0.009(3) 0.029(3) 0.010(3) C41 0.033(3) 0.077(4) 0.056(3) -0.022(3) 0.012(2) -0.003(3) C42 0.030(3) 0.109(5) 0.068(4) -0.031(3) 0.005(3) 0.013(3) C43 0.072(4) 0.069(5) 0.108(5) -0.008(4) -0.012(4) 0.002(3) C44 0.096(6) 0.110(6) 0.169(7) -0.036(6) -0.067(5) 0.013(5) C45 0.116(6) 0.079(6) 0.269(11) -0.074(6) -0.093(7) 0.029(5) C46 0.068(5) 0.079(5) 0.134(6) -0.034(4) 0.002(4) 0.026(4) C47 0.125(7) 0.349(16) 0.115(7) -0.075(8) 0.033(6) 0.118(9) C48 0.157(9) 0.068(6) 0.423(18) -0.094(8) 0.021(10) 0.012(6) C49 0.037(3) 0.049(3) 0.053(3) -0.011(2) 0.020(2) -0.006(2) C50 0.094(5) 0.061(4) 0.134(6) -0.031(4) 0.044(4) -0.014(3) C51 0.081(4) 0.062(4) 0.095(5) 0.015(3) 0.018(4) -0.018(3) C52 0.049(4) 0.076(4) 0.116(5) 0.001(4) 0.021(3) -0.017(3) C53 0.172(12) 0.120(9) 0.45(2) 0.053(12) 0.013(12) 0.032(8) C54 0.171(13) 0.36(3) 0.187(12) 0.027(13) 0.015(10) -0.014(16) C55 0.28(2) 0.25(2) 0.32(2) 0.091(18) 0.172(19) 0.056(19) C56 0.35(3) 0.178(16) 0.43(3) 0.034(18) 0.18(2) 0.057(19) C57 0.29(2) 0.26(2) 0.41(2) -0.003(15) 0.21(2) 0.032(16) C59 0.168(12) 0.33(2) 0.161(10) -0.019(11) 0.027(9) 0.090(12) C60 0.37(2) 0.182(12) 0.153(13) -0.007(11) 0.000(15) 0.088(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 Ti1 N5 1.784(4) . ? Ti1 N1 2.012(3) . ? Ti1 C23 2.166(4) . ? Ti1 N2 2.497(3) . ? Ti1 P1 2.5876(14) . ? Ti1 Si1 2.9261(15) . ? Ti2 N6 1.782(3) . ? Ti2 N3 2.017(3) . ? Ti2 C49 2.160(4) . ? Ti2 N4 2.522(3) . ? Ti2 P3 2.6225(15) . ? Ti2 Si3 2.9375(15) . ? Si1 N1 1.700(3) . ? Si1 N2 1.780(3) . ? Si1 C6 1.866(5) . ? Si1 C5 1.878(4) . ? Si2 C23 1.841(4) . ? Si2 C25 1.861(4) . ? Si2 C26 1.875(5) . ? Si2 C24 1.875(4) . ? Si3 N3 1.694(3) . ? Si3 N4 1.781(4) . ? Si3 C31 1.862(5) . ? Si3 C32 1.876(5) . ? Si4 C49 1.847(4) . ? Si4 C51 1.866(5) . ? Si4 C52 1.872(5) . ? Si4 C50 1.880(5) . ? P1 C8 1.835(4) . ? P1 C12 1.843(4) . ? P1 C9 1.843(4) . ? P2 C17 1.838(5) . ? P2 C20 1.856(5) . ? P2 C16 1.857(4) . ? P3 C34 1.843(4) . ? P3 C38 1.843(4) . ? P3 C35 1.846(4) . ? P4 C43 1.815(6) . ? P4 C42 1.824(5) . ? P4 C46 1.846(6) . ? N1 C1 1.492(5) . ? N2 C15 1.481(5) . ? N2 C7 1.482(5) . ? N3 C27 1.488(5) . ? N4 C33 1.467(5) . ? N4 C41 1.479(5) . ? N5 N6 1.287(4) . ? C1 C4 1.519(6) . ? C1 C3 1.521(6) . ? C1 C2 1.525(6) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.523(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C11 1.519(6) . ? C9 C10 1.527(6) . ? C9 H9A 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C14 1.511(6) . ? C12 C13 1.526(6) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.525(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.505(7) . ? C17 C19 1.540(7) . ? C17 H17A 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.525(6) . ? C20 C22 1.537(6) . ? C20 H20A 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.517(6) . ? C27 C29 1.524(6) . ? C27 C30 1.534(6) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.538(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C37 1.520(6) . ? C35 C36 1.525(6) . ? C35 H35A 1.0000 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.525(6) . ? C38 C40 1.527(6) . ? C38 H38A 1.0000 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.525(6) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C45 1.508(8) . ? C43 C44 1.536(7) . ? C43 H43A 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.493(10) . ? C46 C48 1.514(10) . ? C46 H46A 1.0000 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.672(19) . ? C54 C55 1.46(2) . ? C55 C56 1.40(2) . ? C56 C57 1.52(2) . ? C58 C59 1.23(2) . ? C59 C60 1.66(2) . ? C60 C60 1.296(19) 3_475 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Ti1 N1 110.17(14) . . ? N5 Ti1 C23 102.07(15) . . ? N1 Ti1 C23 118.13(14) . . ? N5 Ti1 N2 158.81(13) . . ? N1 Ti1 N2 70.49(12) . . ? C23 Ti1 N2 95.59(13) . . ? N5 Ti1 P1 89.00(11) . . ? N1 Ti1 P1 123.54(10) . . ? C23 Ti1 P1 107.88(12) . . ? N2 Ti1 P1 74.36(8) . . ? N5 Ti1 Si1 143.68(11) . . ? N1 Ti1 Si1 34.36(9) . . ? C23 Ti1 Si1 104.45(11) . . ? N2 Ti1 Si1 37.28(8) . . ? P1 Ti1 Si1 105.74(4) . . ? N6 Ti2 N3 107.42(14) . . ? N6 Ti2 C49 107.15(16) . . ? N3 Ti2 C49 116.34(15) . . ? N6 Ti2 N4 155.69(13) . . ? N3 Ti2 N4 69.78(12) . . ? C49 Ti2 N4 95.03(15) . . ? N6 Ti2 P3 90.52(11) . . ? N3 Ti2 P3 126.48(10) . . ? C49 Ti2 P3 104.68(13) . . ? N4 Ti2 P3 73.98(9) . . ? N6 Ti2 Si3 140.27(10) . . ? N3 Ti2 Si3 33.99(10) . . ? C49 Ti2 Si3 102.51(12) . . ? N4 Ti2 Si3 37.11(8) . . ? P3 Ti2 Si3 106.98(5) . . ? N1 Si1 N2 98.24(16) . . ? N1 Si1 C6 115.7(2) . . ? N2 Si1 C6 109.39(19) . . ? N1 Si1 C5 118.39(19) . . ? N2 Si1 C5 109.19(19) . . ? C6 Si1 C5 105.5(2) . . ? N1 Si1 Ti1 41.91(11) . . ? N2 Si1 Ti1 58.15(11) . . ? C6 Si1 Ti1 115.25(16) . . ? C5 Si1 Ti1 139.29(17) . . ? C23 Si2 C25 112.1(2) . . ? C23 Si2 C26 113.3(2) . . ? C25 Si2 C26 108.1(2) . . ? C23 Si2 C24 111.9(2) . . ? C25 Si2 C24 105.5(2) . . ? C26 Si2 C24 105.4(2) . . ? N3 Si3 N4 98.27(16) . . ? N3 Si3 C31 115.7(2) . . ? N4 Si3 C31 109.0(2) . . ? N3 Si3 C32 118.56(19) . . ? N4 Si3 C32 109.1(2) . . ? C31 Si3 C32 105.7(2) . . ? N3 Si3 Ti2 41.72(11) . . ? N4 Si3 Ti2 58.66(11) . . ? C31 Si3 Ti2 114.06(17) . . ? C32 Si3 Ti2 140.20(16) . . ? C49 Si4 C51 113.1(2) . . ? C49 Si4 C52 111.5(2) . . ? C51 Si4 C52 107.0(3) . . ? C49 Si4 C50 112.0(2) . . ? C51 Si4 C50 107.0(3) . . ? C52 Si4 C50 105.8(3) . . ? C8 P1 C12 107.5(2) . . ? C8 P1 C9 105.3(2) . . ? C12 P1 C9 105.5(2) . . ? C8 P1 Ti1 105.95(14) . . ? C12 P1 Ti1 119.04(15) . . ? C9 P1 Ti1 112.61(15) . . ? C17 P2 C20 102.4(3) . . ? C17 P2 C16 102.1(2) . . ? C20 P2 C16 100.5(2) . . ? C34 P3 C38 106.0(2) . . ? C34 P3 C35 104.1(2) . . ? C38 P3 C35 104.2(2) . . ? C34 P3 Ti2 105.01(15) . . ? C38 P3 Ti2 121.54(16) . . ? C35 P3 Ti2 114.38(15) . . ? C43 P4 C42 102.6(3) . . ? C43 P4 C46 101.9(3) . . ? C42 P4 C46 101.5(3) . . ? C1 N1 Si1 123.7(3) . . ? C1 N1 Ti1 132.5(3) . . ? Si1 N1 Ti1 103.73(16) . . ? C15 N2 C7 112.8(3) . . ? C15 N2 Si1 119.7(3) . . ? C7 N2 Si1 112.8(2) . . ? C15 N2 Ti1 115.7(2) . . ? C7 N2 Ti1 107.8(2) . . ? Si1 N2 Ti1 84.57(13) . . ? C27 N3 Si3 123.5(3) . . ? C27 N3 Ti2 132.2(3) . . ? Si3 N3 Ti2 104.29(17) . . ? C33 N4 C41 112.0(4) . . ? C33 N4 Si3 114.0(3) . . ? C41 N4 Si3 118.9(3) . . ? C33 N4 Ti2 105.1(2) . . ? C41 N4 Ti2 119.4(3) . . ? Si3 N4 Ti2 84.23(14) . . ? N6 N5 Ti1 172.7(3) . . ? N5 N6 Ti2 173.6(3) . . ? N1 C1 C4 109.6(3) . . ? N1 C1 C3 109.6(3) . . ? C4 C1 C3 109.2(4) . . ? N1 C1 C2 111.8(3) . . ? C4 C1 C2 107.9(4) . . ? C3 C1 C2 108.7(4) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 113.5(3) . . ? N2 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? N2 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C7 C8 P1 108.5(3) . . ? C7 C8 H8A 110.0 . . ? P1 C8 H8A 110.0 . . ? C7 C8 H8B 110.0 . . ? P1 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? C11 C9 C10 110.2(4) . . ? C11 C9 P1 110.1(3) . . ? C10 C9 P1 115.4(3) . . ? C11 C9 H9A 106.9 . . ? C10 C9 H9A 106.9 . . ? P1 C9 H9A 106.9 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C14 C12 C13 111.4(4) . . ? C14 C12 P1 113.8(3) . . ? C13 C12 P1 107.6(3) . . ? C14 C12 H12A 107.9 . . ? C13 C12 H12A 107.9 . . ? P1 C12 H12A 107.9 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 C16 116.6(3) . . ? N2 C15 H15A 108.1 . . ? C16 C15 H15A 108.1 . . ? N2 C15 H15B 108.1 . . ? C16 C15 H15B 108.1 . . ? H15A C15 H15B 107.3 . . ? C15 C16 P2 111.1(3) . . ? C15 C16 H16A 109.4 . . ? P2 C16 H16A 109.4 . . ? C15 C16 H16B 109.4 . . ? P2 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C18 C17 C19 110.0(5) . . ? C18 C17 P2 118.4(4) . . ? C19 C17 P2 108.6(4) . . ? C18 C17 H17A 106.4 . . ? C19 C17 H17A 106.4 . . ? P2 C17 H17A 106.4 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C22 111.5(4) . . ? C21 C20 P2 109.0(3) . . ? C22 C20 P2 110.6(3) . . ? C21 C20 H20A 108.6 . . ? C22 C20 H20A 108.6 . . ? P2 C20 H20A 108.6 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 Ti1 133.7(2) . . ? Si2 C23 H23A 103.8 . . ? Ti1 C23 H23A 103.8 . . ? Si2 C23 H23B 103.8 . . ? Ti1 C23 H23B 103.8 . . ? H23A C23 H23B 105.4 . . ? Si2 C24 H24A 109.5 . . ? Si2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si2 C25 H25A 109.5 . . ? Si2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C27 C28 110.6(3) . . ? N3 C27 C29 108.3(4) . . ? C28 C27 C29 109.6(4) . . ? N3 C27 C30 112.2(4) . . ? C28 C27 C30 107.3(4) . . ? C29 C27 C30 108.8(4) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si3 C31 H31A 109.5 . . ? Si3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si3 C32 H32A 109.5 . . ? Si3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N4 C33 C34 114.0(4) . . ? N4 C33 H33A 108.7 . . ? C34 C33 H33A 108.7 . . ? N4 C33 H33B 108.7 . . ? C34 C33 H33B 108.7 . . ? H33A C33 H33B 107.6 . . ? C33 C34 P3 108.3(3) . . ? C33 C34 H34A 110.0 . . ? P3 C34 H34A 110.0 . . ? C33 C34 H34B 110.0 . . ? P3 C34 H34B 110.0 . . ? H34A C34 H34B 108.4 . . ? C37 C35 C36 110.4(4) . . ? C37 C35 P3 116.0(3) . . ? C36 C35 P3 108.6(3) . . ? C37 C35 H35A 107.1 . . ? C36 C35 H35A 107.1 . . ? P3 C35 H35A 107.1 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C40 109.9(4) . . ? C39 C38 P3 113.1(3) . . ? C40 C38 P3 109.6(3) . . ? C39 C38 H38A 108.0 . . ? C40 C38 H38A 108.0 . . ? P3 C38 H38A 108.0 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N4 C41 C42 116.3(4) . . ? N4 C41 H41A 108.2 . . ? C42 C41 H41A 108.2 . . ? N4 C41 H41B 108.2 . . ? C42 C41 H41B 108.2 . . ? H41A C41 H41B 107.4 . . ? C41 C42 P4 114.6(3) . . ? C41 C42 H42A 108.6 . . ? P4 C42 H42A 108.6 . . ? C41 C42 H42B 108.6 . . ? P4 C42 H42B 108.6 . . ? H42A C42 H42B 107.6 . . ? C45 C43 C44 110.2(5) . . ? C45 C43 P4 111.1(5) . . ? C44 C43 P4 110.6(5) . . ? C45 C43 H43A 108.3 . . ? C44 C43 H43A 108.3 . . ? P4 C43 H43A 108.3 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C47 C46 C48 110.5(7) . . ? C47 C46 P4 116.1(6) . . ? C48 C46 P4 109.0(5) . . ? C47 C46 H46A 106.9 . . ? C48 C46 H46A 106.9 . . ? P4 C46 H46A 106.9 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? Si4 C49 Ti2 135.1(2) . . ? Si4 C49 H49A 103.4 . . ? Ti2 C49 H49A 103.4 . . ? Si4 C49 H49B 103.4 . . ? Ti2 C49 H49B 103.4 . . ? H49A C49 H49B 105.2 . . ? Si4 C50 H50A 109.5 . . ? Si4 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? Si4 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? Si4 C51 H51A 109.5 . . ? Si4 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? Si4 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? Si4 C52 H52A 109.5 . . ? Si4 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? Si4 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C55 C54 C53 109.5(17) . . ? C56 C55 C54 113(2) . . ? C55 C56 C57 102.1(19) . . ? C58 C59 C60 125.7(18) . . ? C60 C60 C59 107(2) 3_475 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Ti1 Si1 N1 -16.6(2) . . . . ? C23 Ti1 Si1 N1 119.1(2) . . . . ? N2 Ti1 Si1 N1 -160.9(2) . . . . ? P1 Ti1 Si1 N1 -127.23(17) . . . . ? N5 Ti1 Si1 N2 144.3(2) . . . . ? N1 Ti1 Si1 N2 160.9(2) . . . . ? C23 Ti1 Si1 N2 -80.07(17) . . . . ? P1 Ti1 Si1 N2 33.63(13) . . . . ? N5 Ti1 Si1 C6 -117.7(2) . . . . ? N1 Ti1 Si1 C6 -101.1(2) . . . . ? C23 Ti1 Si1 C6 17.9(2) . . . . ? N2 Ti1 Si1 C6 98.0(2) . . . . ? P1 Ti1 Si1 C6 131.63(17) . . . . ? N5 Ti1 Si1 C5 61.7(3) . . . . ? N1 Ti1 Si1 C5 78.3(3) . . . . ? C23 Ti1 Si1 C5 -162.7(3) . . . . ? N2 Ti1 Si1 C5 -82.6(3) . . . . ? P1 Ti1 Si1 C5 -49.0(2) . . . . ? N6 Ti2 Si3 N3 -18.8(2) . . . . ? C49 Ti2 Si3 N3 118.9(2) . . . . ? N4 Ti2 Si3 N3 -159.4(2) . . . . ? P3 Ti2 Si3 N3 -131.23(18) . . . . ? N6 Ti2 Si3 N4 140.6(2) . . . . ? N3 Ti2 Si3 N4 159.4(2) . . . . ? C49 Ti2 Si3 N4 -81.69(19) . . . . ? P3 Ti2 Si3 N4 28.14(14) . . . . ? N6 Ti2 Si3 C31 -121.1(2) . . . . ? N3 Ti2 Si3 C31 -102.3(3) . . . . ? C49 Ti2 Si3 C31 16.6(2) . . . . ? N4 Ti2 Si3 C31 98.3(2) . . . . ? P3 Ti2 Si3 C31 126.46(19) . . . . ? N6 Ti2 Si3 C32 58.3(3) . . . . ? N3 Ti2 Si3 C32 77.1(3) . . . . ? C49 Ti2 Si3 C32 -164.0(3) . . . . ? N4 Ti2 Si3 C32 -82.3(3) . . . . ? P3 Ti2 Si3 C32 -54.2(3) . . . . ? N5 Ti1 P1 C8 -160.04(17) . . . . ? N1 Ti1 P1 C8 -46.32(18) . . . . ? C23 Ti1 P1 C8 97.60(18) . . . . ? N2 Ti1 P1 C8 6.69(16) . . . . ? Si1 Ti1 P1 C8 -13.70(15) . . . . ? N5 Ti1 P1 C12 78.83(19) . . . . ? N1 Ti1 P1 C12 -167.5(2) . . . . ? C23 Ti1 P1 C12 -23.5(2) . . . . ? N2 Ti1 P1 C12 -114.45(18) . . . . ? Si1 Ti1 P1 C12 -134.83(17) . . . . ? N5 Ti1 P1 C9 -45.39(19) . . . . ? N1 Ti1 P1 C9 68.3(2) . . . . ? C23 Ti1 P1 C9 -147.7(2) . . . . ? N2 Ti1 P1 C9 121.34(18) . . . . ? Si1 Ti1 P1 C9 100.95(16) . . . . ? N6 Ti2 P3 C34 -149.78(18) . . . . ? N3 Ti2 P3 C34 -37.5(2) . . . . ? C49 Ti2 P3 C34 102.3(2) . . . . ? N4 Ti2 P3 C34 11.23(18) . . . . ? Si3 Ti2 P3 C34 -5.99(16) . . . . ? N6 Ti2 P3 C38 90.3(2) . . . . ? N3 Ti2 P3 C38 -157.4(2) . . . . ? C49 Ti2 P3 C38 -17.6(2) . . . . ? N4 Ti2 P3 C38 -108.69(19) . . . . ? Si3 Ti2 P3 C38 -125.91(17) . . . . ? N6 Ti2 P3 C35 -36.24(19) . . . . ? N3 Ti2 P3 C35 76.0(2) . . . . ? C49 Ti2 P3 C35 -144.1(2) . . . . ? N4 Ti2 P3 C35 124.77(19) . . . . ? Si3 Ti2 P3 C35 107.55(17) . . . . ? N2 Si1 N1 C1 164.4(3) . . . . ? C6 Si1 N1 C1 -79.3(4) . . . . ? C5 Si1 N1 C1 47.3(4) . . . . ? Ti1 Si1 N1 C1 -179.2(4) . . . . ? N2 Si1 N1 Ti1 -16.35(18) . . . . ? C6 Si1 N1 Ti1 99.9(2) . . . . ? C5 Si1 N1 Ti1 -133.5(2) . . . . ? N5 Ti1 N1 C1 -11.3(4) . . . . ? C23 Ti1 N1 C1 105.4(4) . . . . ? N2 Ti1 N1 C1 -168.7(4) . . . . ? P1 Ti1 N1 C1 -114.0(3) . . . . ? Si1 Ti1 N1 C1 179.1(5) . . . . ? N5 Ti1 N1 Si1 169.63(16) . . . . ? C23 Ti1 N1 Si1 -73.7(2) . . . . ? N2 Ti1 N1 Si1 12.16(14) . . . . ? P1 Ti1 N1 Si1 66.85(18) . . . . ? N1 Si1 N2 C15 129.4(3) . . . . ? C6 Si1 N2 C15 8.3(3) . . . . ? C5 Si1 N2 C15 -106.7(3) . . . . ? Ti1 Si1 N2 C15 116.6(3) . . . . ? N1 Si1 N2 C7 -94.3(3) . . . . ? C6 Si1 N2 C7 144.6(3) . . . . ? C5 Si1 N2 C7 29.7(3) . . . . ? Ti1 Si1 N2 C7 -107.1(3) . . . . ? N1 Si1 N2 Ti1 12.79(14) . . . . ? C6 Si1 N2 Ti1 -108.29(18) . . . . ? C5 Si1 N2 Ti1 136.78(17) . . . . ? N5 Ti1 N2 C15 132.6(4) . . . . ? N1 Ti1 N2 C15 -131.8(3) . . . . ? C23 Ti1 N2 C15 -13.9(3) . . . . ? P1 Ti1 N2 C15 93.1(3) . . . . ? Si1 Ti1 N2 C15 -120.5(3) . . . . ? N5 Ti1 N2 C7 5.2(5) . . . . ? N1 Ti1 N2 C7 100.9(2) . . . . ? C23 Ti1 N2 C7 -141.2(2) . . . . ? P1 Ti1 N2 C7 -34.2(2) . . . . ? Si1 Ti1 N2 C7 112.2(3) . . . . ? N5 Ti1 N2 Si1 -107.0(3) . . . . ? N1 Ti1 N2 Si1 -11.32(13) . . . . ? C23 Ti1 N2 Si1 106.58(15) . . . . ? P1 Ti1 N2 Si1 -146.39(12) . . . . ? N4 Si3 N3 C27 163.3(3) . . . . ? C31 Si3 N3 C27 -81.0(4) . . . . ? C32 Si3 N3 C27 46.3(4) . . . . ? Ti2 Si3 N3 C27 -179.0(4) . . . . ? N4 Si3 N3 Ti2 -17.70(19) . . . . ? C31 Si3 N3 Ti2 98.0(2) . . . . ? C32 Si3 N3 Ti2 -134.7(2) . . . . ? N6 Ti2 N3 C27 -13.6(4) . . . . ? C49 Ti2 N3 C27 106.4(4) . . . . ? N4 Ti2 N3 C27 -168.0(4) . . . . ? P3 Ti2 N3 C27 -117.7(3) . . . . ? Si3 Ti2 N3 C27 178.9(5) . . . . ? N6 Ti2 N3 Si3 167.56(16) . . . . ? C49 Ti2 N3 Si3 -72.4(2) . . . . ? N4 Ti2 N3 Si3 13.09(15) . . . . ? P3 Ti2 N3 Si3 63.45(19) . . . . ? N3 Si3 N4 C33 -90.3(3) . . . . ? C31 Si3 N4 C33 148.8(3) . . . . ? C32 Si3 N4 C33 33.8(3) . . . . ? Ti2 Si3 N4 C33 -104.0(3) . . . . ? N3 Si3 N4 C41 134.2(3) . . . . ? C31 Si3 N4 C41 13.3(4) . . . . ? C32 Si3 N4 C41 -101.6(3) . . . . ? Ti2 Si3 N4 C41 120.5(3) . . . . ? N3 Si3 N4 Ti2 13.71(15) . . . . ? C31 Si3 N4 Ti2 -107.19(19) . . . . ? C32 Si3 N4 Ti2 137.85(17) . . . . ? N6 Ti2 N4 C33 13.5(5) . . . . ? N3 Ti2 N4 C33 101.2(3) . . . . ? C49 Ti2 N4 C33 -142.6(3) . . . . ? P3 Ti2 N4 C33 -38.7(2) . . . . ? Si3 Ti2 N4 C33 113.3(3) . . . . ? N6 Ti2 N4 C41 140.1(4) . . . . ? N3 Ti2 N4 C41 -132.2(3) . . . . ? C49 Ti2 N4 C41 -15.9(3) . . . . ? P3 Ti2 N4 C41 87.9(3) . . . . ? Si3 Ti2 N4 C41 -120.1(4) . . . . ? N6 Ti2 N4 Si3 -99.8(3) . . . . ? N3 Ti2 N4 Si3 -12.12(13) . . . . ? C49 Ti2 N4 Si3 104.14(16) . . . . ? P3 Ti2 N4 Si3 -152.01(14) . . . . ? N1 Ti1 N5 N6 -134(2) . . . . ? C23 Ti1 N5 N6 100(2) . . . . ? N2 Ti1 N5 N6 -46(2) . . . . ? P1 Ti1 N5 N6 -8(2) . . . . ? Si1 Ti1 N5 N6 -124(2) . . . . ? Ti1 N5 N6 Ti2 -146.0(18) . . . . ? N3 Ti2 N6 N5 -105(2) . . . . ? C49 Ti2 N6 N5 129(2) . . . . ? N4 Ti2 N6 N5 -26(3) . . . . ? P3 Ti2 N6 N5 23(2) . . . . ? Si3 Ti2 N6 N5 -94(2) . . . . ? Si1 N1 C1 C4 150.3(3) . . . . ? Ti1 N1 C1 C4 -28.6(5) . . . . ? Si1 N1 C1 C3 -89.8(4) . . . . ? Ti1 N1 C1 C3 91.2(4) . . . . ? Si1 N1 C1 C2 30.8(5) . . . . ? Ti1 N1 C1 C2 -148.2(3) . . . . ? C15 N2 C7 C8 -66.6(4) . . . . ? Si1 N2 C7 C8 154.0(3) . . . . ? Ti1 N2 C7 C8 62.4(3) . . . . ? N2 C7 C8 P1 -55.2(4) . . . . ? C12 P1 C8 C7 148.3(3) . . . . ? C9 P1 C8 C7 -99.6(3) . . . . ? Ti1 P1 C8 C7 20.0(3) . . . . ? C8 P1 C9 C11 58.9(3) . . . . ? C12 P1 C9 C11 172.5(3) . . . . ? Ti1 P1 C9 C11 -56.1(3) . . . . ? C8 P1 C9 C10 -66.5(4) . . . . ? C12 P1 C9 C10 47.1(4) . . . . ? Ti1 P1 C9 C10 178.5(3) . . . . ? C8 P1 C12 C14 -49.3(4) . . . . ? C9 P1 C12 C14 -161.4(3) . . . . ? Ti1 P1 C12 C14 71.0(4) . . . . ? C8 P1 C12 C13 -173.3(3) . . . . ? C9 P1 C12 C13 74.7(3) . . . . ? Ti1 P1 C12 C13 -52.9(4) . . . . ? C7 N2 C15 C16 -57.4(5) . . . . ? Si1 N2 C15 C16 78.9(4) . . . . ? Ti1 N2 C15 C16 177.8(3) . . . . ? N2 C15 C16 P2 -174.6(3) . . . . ? C17 P2 C16 C15 142.4(3) . . . . ? C20 P2 C16 C15 -112.4(3) . . . . ? C20 P2 C17 C18 -52.2(5) . . . . ? C16 P2 C17 C18 51.6(5) . . . . ? C20 P2 C17 C19 -178.4(4) . . . . ? C16 P2 C17 C19 -74.7(4) . . . . ? C17 P2 C20 C21 179.2(3) . . . . ? C16 P2 C20 C21 74.2(3) . . . . ? C17 P2 C20 C22 -57.9(4) . . . . ? C16 P2 C20 C22 -162.9(3) . . . . ? C25 Si2 C23 Ti1 -20.3(4) . . . . ? C26 Si2 C23 Ti1 102.4(3) . . . . ? C24 Si2 C23 Ti1 -138.6(3) . . . . ? N5 Ti1 C23 Si2 102.1(3) . . . . ? N1 Ti1 C23 Si2 -18.8(4) . . . . ? N2 Ti1 C23 Si2 -89.7(3) . . . . ? P1 Ti1 C23 Si2 -165.0(3) . . . . ? Si1 Ti1 C23 Si2 -52.8(3) . . . . ? Si3 N3 C27 C28 152.8(3) . . . . ? Ti2 N3 C27 C28 -25.8(5) . . . . ? Si3 N3 C27 C29 -87.1(4) . . . . ? Ti2 N3 C27 C29 94.2(4) . . . . ? Si3 N3 C27 C30 33.0(5) . . . . ? Ti2 N3 C27 C30 -145.7(3) . . . . ? C41 N4 C33 C34 -64.3(5) . . . . ? Si3 N4 C33 C34 157.1(3) . . . . ? Ti2 N4 C33 C34 66.8(4) . . . . ? N4 C33 C34 P3 -55.7(4) . . . . ? C38 P3 C34 C33 145.1(3) . . . . ? C35 P3 C34 C33 -105.3(3) . . . . ? Ti2 P3 C34 C33 15.3(3) . . . . ? C34 P3 C35 C37 -64.6(4) . . . . ? C38 P3 C35 C37 46.3(4) . . . . ? Ti2 P3 C35 C37 -178.7(3) . . . . ? C34 P3 C35 C36 60.4(4) . . . . ? C38 P3 C35 C36 171.3(3) . . . . ? Ti2 P3 C35 C36 -53.7(3) . . . . ? C34 P3 C38 C39 -62.5(4) . . . . ? C35 P3 C38 C39 -172.1(3) . . . . ? Ti2 P3 C38 C39 56.9(4) . . . . ? C34 P3 C38 C40 174.5(3) . . . . ? C35 P3 C38 C40 64.9(4) . . . . ? Ti2 P3 C38 C40 -66.1(4) . . . . ? C33 N4 C41 C42 -62.1(5) . . . . ? Si3 N4 C41 C42 74.2(5) . . . . ? Ti2 N4 C41 C42 174.6(3) . . . . ? N4 C41 C42 P4 147.1(4) . . . . ? C43 P4 C42 C41 87.0(5) . . . . ? C46 P4 C42 C41 -167.8(4) . . . . ? C42 P4 C43 C45 -70.3(6) . . . . ? C46 P4 C43 C45 -175.1(6) . . . . ? C42 P4 C43 C44 167.0(5) . . . . ? C46 P4 C43 C44 62.2(6) . . . . ? C43 P4 C46 C47 56.4(6) . . . . ? C42 P4 C46 C47 -49.3(6) . . . . ? C43 P4 C46 C48 -178.1(6) . . . . ? C42 P4 C46 C48 76.2(7) . . . . ? C51 Si4 C49 Ti2 -7.2(4) . . . . ? C52 Si4 C49 Ti2 113.4(3) . . . . ? C50 Si4 C49 Ti2 -128.3(3) . . . . ? N6 Ti2 C49 Si4 89.5(3) . . . . ? N3 Ti2 C49 Si4 -30.7(4) . . . . ? N4 Ti2 C49 Si4 -100.6(3) . . . . ? P3 Ti2 C49 Si4 -175.3(3) . . . . ? Si3 Ti2 C49 Si4 -63.8(3) . . . . ? C53 C54 C55 C56 171.8(16) . . . . ? C54 C55 C56 C57 -168.6(16) . . . . ? C58 C59 C60 C60 63(3) . . . 3_475 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 24.72 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.388 _refine_diff_density_min -0.301 _refine_diff_density_rms 0.062 # Attachment 'wac3158xs.txt' data_wac3158xs _database_code_depnum_ccdc_archive 'CCDC 652415' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H51 Fe N3 P2 Si' _chemical_formula_sum 'C22 H51 Fe N3 P2 Si' _chemical_formula_weight 503.54 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' Fe Fe 0.3463 0.8444 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.6476(11) _cell_length_b 18.0559(18) _cell_length_c 13.3821(13) _cell_angle_alpha 90.00 _cell_angle_beta 102.0550(10) _cell_angle_gamma 90.00 _cell_volume 2752.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 154(2) _cell_measurement_reflns_used 5424 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 26.2 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 0.721 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 154(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 'SMART 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13059 _diffrn_reflns_av_R_equivalents 0.0162 _diffrn_reflns_av_sigmaI/netI 0.0218 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 26.34 _reflns_number_total 5248 _reflns_number_gt 4422 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054d' _computing_cell_refinement 'Bruker SAINT v7.07' _computing_data_reduction 'Bruker SAINT v7.07' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5248 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0936 _refine_ls_wR_factor_gt 0.0909 _refine_ls_goodness_of_fit_ref 1.576 _refine_ls_restrained_S_all 1.576 _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 Fe1 Fe 0.35635(2) 0.015856(15) 0.341221(19) 0.01902(10) Uani 1 1 d . . . Si4 Si 0.15061(5) -0.05016(3) 0.17809(4) 0.02549(14) Uani 1 1 d . . . P1 P 0.48541(4) 0.03333(3) 0.22529(4) 0.02158(13) Uani 1 1 d . . . P2 P 0.24419(4) 0.13130(3) 0.32780(4) 0.02220(13) Uani 1 1 d . . . N1 N 0.22817(14) -0.05866(9) 0.30024(12) 0.0241(4) Uani 1 1 d . . . N2 N 0.20305(15) 0.02908(9) 0.12651(12) 0.0250(4) Uani 1 1 d . . . N3 N 0.46541(14) 0.00638(9) 0.46280(12) 0.0217(3) Uani 1 1 d . . . C1 C 0.21480(19) -0.11943(12) 0.37158(15) 0.0297(5) Uani 1 1 d . . . C2 C 0.2118(2) -0.08768(14) 0.47615(16) 0.0430(6) Uani 1 1 d . . . H2A H 0.2835 -0.0591 0.5013 0.064 Uiso 1 1 calc R . . H2B H 0.2067 -0.1282 0.5238 0.064 Uiso 1 1 calc R . . H2C H 0.1433 -0.0553 0.4708 0.064 Uiso 1 1 calc R . . C3 C 0.0998(2) -0.16315(16) 0.33804(19) 0.0579(8) Uani 1 1 d . . . H3C H 0.0971 -0.1850 0.2705 0.087 Uiso 1 1 calc R . . H3D H 0.0328 -0.1297 0.3347 0.087 Uiso 1 1 calc R . . H3E H 0.0962 -0.2026 0.3876 0.087 Uiso 1 1 calc R . . C4 C 0.3170(3) -0.17203(15) 0.3822(2) 0.0665(9) Uani 1 1 d . . . H4A H 0.3905 -0.1445 0.4036 0.100 Uiso 1 1 calc R . . H4B H 0.3159 -0.1961 0.3164 0.100 Uiso 1 1 calc R . . H4C H 0.3109 -0.2097 0.4336 0.100 Uiso 1 1 calc R . . C5 C 0.1604(2) -0.13046(13) 0.08985(16) 0.0373(5) Uani 1 1 d . . . H5A H 0.2430 -0.1423 0.0923 0.056 Uiso 1 1 calc R . . H5B H 0.1221 -0.1170 0.0198 0.056 Uiso 1 1 calc R . . H5C H 0.1210 -0.1737 0.1116 0.056 Uiso 1 1 calc R . . C6 C -0.01330(19) -0.03671(14) 0.16193(18) 0.0380(5) Uani 1 1 d . . . H6A H -0.0286 0.0044 0.2052 0.057 Uiso 1 1 calc R . . H6B H -0.0487 -0.0821 0.1820 0.057 Uiso 1 1 calc R . . H6C H -0.0475 -0.0254 0.0903 0.057 Uiso 1 1 calc R . . C7 C 0.28693(18) 0.02374(12) 0.05958(15) 0.0265(5) Uani 1 1 d . . . H7A H 0.2502 0.0454 -0.0074 0.032 Uiso 1 1 calc R . . H7B H 0.3009 -0.0294 0.0482 0.032 Uiso 1 1 calc R . . C8 C 0.40647(17) 0.06136(11) 0.09705(14) 0.0240(4) Uani 1 1 d . . . H8A H 0.3943 0.1156 0.0970 0.029 Uiso 1 1 calc R . . H8B H 0.4568 0.0505 0.0477 0.029 Uiso 1 1 calc R . . C9 C 0.60615(17) 0.10288(12) 0.25337(15) 0.0267(4) Uani 1 1 d . . . H9A H 0.6649 0.0828 0.3125 0.032 Uiso 1 1 calc R . . C10 C 0.6727(2) 0.11515(14) 0.16700(17) 0.0397(6) Uani 1 1 d . . . H10A H 0.7341 0.1524 0.1883 0.060 Uiso 1 1 calc R . . H10B H 0.6178 0.1325 0.1057 0.060 Uiso 1 1 calc R . . H10C H 0.7084 0.0684 0.1520 0.060 Uiso 1 1 calc R . . C11 C 0.5645(2) 0.17605(12) 0.28880(17) 0.0366(5) Uani 1 1 d . . . H11A H 0.6302 0.2111 0.3027 0.055 Uiso 1 1 calc R . . H11B H 0.5347 0.1682 0.3512 0.055 Uiso 1 1 calc R . . H11C H 0.5018 0.1962 0.2353 0.055 Uiso 1 1 calc R . . C12 C 0.56889(18) -0.05003(12) 0.19947(15) 0.0282(5) Uani 1 1 d . . . H12A H 0.6120 -0.0373 0.1445 0.034 Uiso 1 1 calc R . . C13 C 0.4889(2) -0.11513(12) 0.16341(18) 0.0392(6) Uani 1 1 d . . . H13A H 0.5361 -0.1577 0.1507 0.059 Uiso 1 1 calc R . . H13B H 0.4337 -0.1018 0.1001 0.059 Uiso 1 1 calc R . . H13C H 0.4450 -0.1280 0.2160 0.059 Uiso 1 1 calc R . . C14 C 0.6598(2) -0.07065(15) 0.29644(17) 0.0449(6) Uani 1 1 d . . . H14A H 0.7037 -0.1145 0.2829 0.067 Uiso 1 1 calc R . . H14B H 0.6194 -0.0814 0.3521 0.067 Uiso 1 1 calc R . . H14C H 0.7142 -0.0292 0.3161 0.067 Uiso 1 1 calc R . . C15 C 0.14155(18) 0.09961(11) 0.12107(15) 0.0280(5) Uani 1 1 d . . . H15A H 0.0625 0.0904 0.1349 0.034 Uiso 1 1 calc R . . H15B H 0.1305 0.1183 0.0502 0.034 Uiso 1 1 calc R . . C16 C 0.19985(18) 0.16089(11) 0.19331(15) 0.0270(4) Uani 1 1 d . . . H16A H 0.1446 0.2030 0.1892 0.032 Uiso 1 1 calc R . . H16B H 0.2701 0.1788 0.1698 0.032 Uiso 1 1 calc R . . C17 C 0.30379(18) 0.22061(11) 0.38652(16) 0.0295(5) Uani 1 1 d . . . H17A H 0.3607 0.2374 0.3446 0.035 Uiso 1 1 calc R . . C18 C 0.3777(2) 0.21057(13) 0.49461(17) 0.0415(6) Uani 1 1 d . . . H18A H 0.4070 0.2589 0.5222 0.062 Uiso 1 1 calc R . . H18B H 0.4443 0.1779 0.4923 0.062 Uiso 1 1 calc R . . H18C H 0.3293 0.1886 0.5385 0.062 Uiso 1 1 calc R . . C19 C 0.2179(2) 0.28494(12) 0.38274(19) 0.0419(6) Uani 1 1 d . . . H19A H 0.2597 0.3284 0.4160 0.063 Uiso 1 1 calc R . . H19B H 0.1557 0.2710 0.4185 0.063 Uiso 1 1 calc R . . H19C H 0.1830 0.2968 0.3114 0.063 Uiso 1 1 calc R . . C20 C 0.10273(17) 0.11231(12) 0.36655(15) 0.0287(5) Uani 1 1 d . . . H20A H 0.0816 0.0605 0.3434 0.034 Uiso 1 1 calc R . . C21 C 0.1212(2) 0.10978(15) 0.48268(16) 0.0399(6) Uani 1 1 d . . . H21A H 0.0461 0.0997 0.5022 0.060 Uiso 1 1 calc R . . H21B H 0.1520 0.1575 0.5112 0.060 Uiso 1 1 calc R . . H21C H 0.1772 0.0705 0.5093 0.060 Uiso 1 1 calc R . . C22 C -0.00542(19) 0.15893(15) 0.32097(19) 0.0427(6) Uani 1 1 d . . . H22A H -0.0724 0.1422 0.3488 0.064 Uiso 1 1 calc R . . H22B H -0.0237 0.1532 0.2465 0.064 Uiso 1 1 calc R . . H22C H 0.0107 0.2111 0.3384 0.064 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01916(16) 0.01984(16) 0.01726(15) 0.00018(11) 0.00196(11) -0.00051(11) Si4 0.0253(3) 0.0264(3) 0.0228(3) -0.0001(2) 0.0006(2) -0.0062(2) P1 0.0228(3) 0.0245(3) 0.0174(3) 0.0007(2) 0.0041(2) 0.0015(2) P2 0.0227(3) 0.0210(3) 0.0229(3) -0.0004(2) 0.0047(2) 0.0024(2) N1 0.0257(9) 0.0242(9) 0.0216(8) 0.0018(7) 0.0033(7) -0.0051(7) N2 0.0270(9) 0.0267(9) 0.0207(8) 0.0019(7) 0.0035(7) -0.0009(7) N3 0.0229(9) 0.0223(8) 0.0207(8) -0.0012(7) 0.0064(6) -0.0014(7) C1 0.0331(12) 0.0287(11) 0.0266(11) 0.0028(9) 0.0046(9) -0.0072(9) C2 0.0541(15) 0.0493(15) 0.0276(12) 0.0022(11) 0.0131(10) -0.0198(13) C3 0.075(2) 0.0564(17) 0.0383(14) 0.0099(12) 0.0021(13) -0.0421(15) C4 0.081(2) 0.0441(16) 0.087(2) 0.0387(16) 0.0477(18) 0.0226(16) C5 0.0481(14) 0.0331(12) 0.0285(12) -0.0047(10) 0.0032(10) -0.0127(11) C6 0.0268(12) 0.0460(14) 0.0379(13) 0.0037(11) -0.0007(10) -0.0104(10) C7 0.0302(11) 0.0301(11) 0.0187(10) 0.0006(8) 0.0040(8) -0.0002(9) C8 0.0272(11) 0.0267(11) 0.0181(9) 0.0023(8) 0.0050(8) 0.0006(9) C9 0.0223(10) 0.0329(11) 0.0242(10) -0.0001(9) 0.0032(8) -0.0032(9) C10 0.0347(13) 0.0472(15) 0.0412(13) -0.0051(11) 0.0169(10) -0.0092(11) C11 0.0383(13) 0.0341(13) 0.0383(12) -0.0063(10) 0.0102(10) -0.0087(10) C12 0.0317(12) 0.0309(12) 0.0243(10) 0.0024(9) 0.0113(9) 0.0080(9) C13 0.0446(14) 0.0265(12) 0.0491(14) -0.0018(11) 0.0156(11) 0.0057(10) C14 0.0494(15) 0.0483(15) 0.0346(13) 0.0031(11) 0.0035(11) 0.0251(13) C15 0.0277(11) 0.0305(11) 0.0236(10) 0.0027(9) 0.0005(8) 0.0027(9) C16 0.0299(11) 0.0247(11) 0.0262(10) 0.0051(9) 0.0056(8) 0.0036(9) C17 0.0330(12) 0.0227(11) 0.0337(11) -0.0046(9) 0.0092(9) -0.0002(9) C18 0.0498(15) 0.0335(13) 0.0378(13) -0.0096(10) 0.0015(10) -0.0038(11) C19 0.0514(15) 0.0243(12) 0.0513(15) -0.0064(11) 0.0135(12) 0.0061(11) C20 0.0235(11) 0.0319(12) 0.0309(11) 0.0010(9) 0.0059(8) 0.0038(9) C21 0.0356(13) 0.0523(15) 0.0343(13) 0.0039(11) 0.0130(10) 0.0014(11) C22 0.0272(12) 0.0536(16) 0.0476(14) 0.0062(12) 0.0085(10) 0.0123(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 Fe1 N3 1.8511(16) . ? Fe1 N1 1.9994(16) . ? Fe1 P1 2.3959(6) . ? Fe1 P2 2.4466(6) . ? Si4 N1 1.7014(16) . ? Si4 N2 1.7530(17) . ? Si4 C5 1.888(2) . ? Si4 C6 1.892(2) . ? P1 C8 1.8406(18) . ? P1 C12 1.863(2) . ? P1 C9 1.864(2) . ? P2 C16 1.845(2) . ? P2 C20 1.860(2) . ? P2 C17 1.863(2) . ? N1 C1 1.484(2) . ? N2 C15 1.455(3) . ? N2 C7 1.460(2) . ? N3 N3 1.166(3) 3_656 ? C1 C4 1.506(3) . ? C1 C2 1.519(3) . ? C1 C3 1.539(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3C 0.9800 . ? C3 H3D 0.9800 . ? C3 H3E 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.536(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C11 1.517(3) . ? C9 C10 1.536(3) . ? C9 H9A 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.515(3) . ? C12 C14 1.539(3) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.532(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C19 1.527(3) . ? C17 C18 1.532(3) . ? C17 H17A 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.524(3) . ? C20 C22 1.532(3) . ? C20 H20A 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Fe1 N1 120.99(7) . . ? N3 Fe1 P1 99.96(5) . . ? N1 Fe1 P1 116.39(5) . . ? N3 Fe1 P2 113.65(5) . . ? N1 Fe1 P2 101.33(5) . . ? P1 Fe1 P2 103.76(2) . . ? N1 Si4 N2 107.04(8) . . ? N1 Si4 C5 116.26(10) . . ? N2 Si4 C5 108.00(9) . . ? N1 Si4 C6 116.24(9) . . ? N2 Si4 C6 106.05(10) . . ? C5 Si4 C6 102.60(11) . . ? C8 P1 C12 103.16(9) . . ? C8 P1 C9 102.21(9) . . ? C12 P1 C9 100.41(9) . . ? C8 P1 Fe1 112.40(6) . . ? C12 P1 Fe1 115.86(7) . . ? C9 P1 Fe1 120.47(6) . . ? C16 P2 C20 103.98(9) . . ? C16 P2 C17 99.47(9) . . ? C20 P2 C17 108.40(10) . . ? C16 P2 Fe1 110.78(7) . . ? C20 P2 Fe1 108.24(7) . . ? C17 P2 Fe1 124.07(7) . . ? C1 N1 Si4 125.36(13) . . ? C1 N1 Fe1 119.59(12) . . ? Si4 N1 Fe1 114.78(8) . . ? C15 N2 C7 114.36(16) . . ? C15 N2 Si4 121.70(13) . . ? C7 N2 Si4 121.36(13) . . ? N3 N3 Fe1 173.8(2) 3_656 . ? N1 C1 C4 109.90(17) . . ? N1 C1 C2 109.83(17) . . ? C4 C1 C2 108.7(2) . . ? N1 C1 C3 113.18(17) . . ? C4 C1 C3 109.1(2) . . ? C2 C1 C3 106.04(18) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3C 109.5 . . ? C1 C3 H3D 109.5 . . ? H3C C3 H3D 109.5 . . ? C1 C3 H3E 109.5 . . ? H3C C3 H3E 109.5 . . ? H3D C3 H3E 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si4 C5 H5A 109.5 . . ? Si4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si4 C6 H6A 109.5 . . ? Si4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 116.59(16) . . ? N2 C7 H7A 108.1 . . ? C8 C7 H7A 108.1 . . ? N2 C7 H7B 108.1 . . ? C8 C7 H7B 108.1 . . ? H7A C7 H7B 107.3 . . ? C7 C8 P1 115.15(13) . . ? C7 C8 H8A 108.5 . . ? P1 C8 H8A 108.5 . . ? C7 C8 H8B 108.5 . . ? P1 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? C11 C9 C10 110.72(18) . . ? C11 C9 P1 111.89(14) . . ? C10 C9 P1 115.05(14) . . ? C11 C9 H9A 106.2 . . ? C10 C9 H9A 106.2 . . ? P1 C9 H9A 106.2 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C14 110.48(19) . . ? C13 C12 P1 112.06(14) . . ? C14 C12 P1 109.44(14) . . ? C13 C12 H12A 108.3 . . ? C14 C12 H12A 108.3 . . ? P1 C12 H12A 108.3 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 C16 116.86(16) . . ? N2 C15 H15A 108.1 . . ? C16 C15 H15A 108.1 . . ? N2 C15 H15B 108.1 . . ? C16 C15 H15B 108.1 . . ? H15A C15 H15B 107.3 . . ? C15 C16 P2 113.80(14) . . ? C15 C16 H16A 108.8 . . ? P2 C16 H16A 108.8 . . ? C15 C16 H16B 108.8 . . ? P2 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? C19 C17 C18 110.89(18) . . ? C19 C17 P2 117.42(15) . . ? C18 C17 P2 112.48(15) . . ? C19 C17 H17A 104.9 . . ? C18 C17 H17A 104.9 . . ? P2 C17 H17A 104.9 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C22 110.57(18) . . ? C21 C20 P2 110.22(14) . . ? C22 C20 P2 119.37(15) . . ? C21 C20 H20A 105.2 . . ? C22 C20 H20A 105.2 . . ? P2 C20 H20A 105.2 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Fe1 P1 C8 -169.89(9) . . . . ? N1 Fe1 P1 C8 57.98(9) . . . . ? P2 Fe1 P1 C8 -52.35(7) . . . . ? N3 Fe1 P1 C12 71.86(9) . . . . ? N1 Fe1 P1 C12 -60.28(9) . . . . ? P2 Fe1 P1 C12 -170.61(7) . . . . ? N3 Fe1 P1 C9 -49.35(10) . . . . ? N1 Fe1 P1 C9 178.52(9) . . . . ? P2 Fe1 P1 C9 68.19(8) . . . . ? N3 Fe1 P2 C16 150.15(9) . . . . ? N1 Fe1 P2 C16 -78.46(9) . . . . ? P1 Fe1 P2 C16 42.59(7) . . . . ? N3 Fe1 P2 C20 -96.44(9) . . . . ? N1 Fe1 P2 C20 34.94(8) . . . . ? P1 Fe1 P2 C20 155.99(7) . . . . ? N3 Fe1 P2 C17 32.17(10) . . . . ? N1 Fe1 P2 C17 163.56(9) . . . . ? P1 Fe1 P2 C17 -75.39(8) . . . . ? N2 Si4 N1 C1 -178.24(16) . . . . ? C5 Si4 N1 C1 -57.46(19) . . . . ? C6 Si4 N1 C1 63.50(19) . . . . ? N2 Si4 N1 Fe1 -4.24(12) . . . . ? C5 Si4 N1 Fe1 116.54(11) . . . . ? C6 Si4 N1 Fe1 -122.50(11) . . . . ? N3 Fe1 N1 C1 4.52(17) . . . . ? P1 Fe1 N1 C1 126.09(13) . . . . ? P2 Fe1 N1 C1 -122.18(14) . . . . ? N3 Fe1 N1 Si4 -169.85(8) . . . . ? P1 Fe1 N1 Si4 -48.28(10) . . . . ? P2 Fe1 N1 Si4 63.45(9) . . . . ? N1 Si4 N2 C15 -99.19(16) . . . . ? C5 Si4 N2 C15 134.92(16) . . . . ? C6 Si4 N2 C15 25.51(17) . . . . ? N1 Si4 N2 C7 100.01(16) . . . . ? C5 Si4 N2 C7 -25.88(17) . . . . ? C6 Si4 N2 C7 -135.29(16) . . . . ? N1 Fe1 N3 N3 43.6(19) . . . 3_656 ? P1 Fe1 N3 N3 -85.6(19) . . . 3_656 ? P2 Fe1 N3 N3 164.5(18) . . . 3_656 ? Si4 N1 C1 C4 105.2(2) . . . . ? Fe1 N1 C1 C4 -68.5(2) . . . . ? Si4 N1 C1 C2 -135.25(17) . . . . ? Fe1 N1 C1 C2 51.0(2) . . . . ? Si4 N1 C1 C3 -17.0(3) . . . . ? Fe1 N1 C1 C3 169.30(17) . . . . ? C15 N2 C7 C8 79.2(2) . . . . ? Si4 N2 C7 C8 -118.65(17) . . . . ? N2 C7 C8 P1 54.0(2) . . . . ? C12 P1 C8 C7 87.27(16) . . . . ? C9 P1 C8 C7 -168.82(14) . . . . ? Fe1 P1 C8 C7 -38.24(16) . . . . ? C8 P1 C9 C11 80.03(16) . . . . ? C12 P1 C9 C11 -173.91(15) . . . . ? Fe1 P1 C9 C11 -45.41(17) . . . . ? C8 P1 C9 C10 -47.46(18) . . . . ? C12 P1 C9 C10 58.59(17) . . . . ? Fe1 P1 C9 C10 -172.90(13) . . . . ? C8 P1 C12 C13 -69.00(16) . . . . ? C9 P1 C12 C13 -174.30(15) . . . . ? Fe1 P1 C12 C13 54.25(16) . . . . ? C8 P1 C12 C14 168.09(15) . . . . ? C9 P1 C12 C14 62.79(17) . . . . ? Fe1 P1 C12 C14 -68.66(16) . . . . ? C7 N2 C15 C16 -88.8(2) . . . . ? Si4 N2 C15 C16 109.13(18) . . . . ? N2 C15 C16 P2 -50.5(2) . . . . ? C20 P2 C16 C15 -66.33(17) . . . . ? C17 P2 C16 C15 -178.13(15) . . . . ? Fe1 P2 C16 C15 49.75(16) . . . . ? C16 P2 C17 C19 64.54(18) . . . . ? C20 P2 C17 C19 -43.74(19) . . . . ? Fe1 P2 C17 C19 -172.30(13) . . . . ? C16 P2 C17 C18 -164.96(16) . . . . ? C20 P2 C17 C18 86.75(17) . . . . ? Fe1 P2 C17 C18 -41.80(18) . . . . ? C16 P2 C20 C21 -163.01(16) . . . . ? C17 P2 C20 C21 -57.85(18) . . . . ? Fe1 P2 C20 C21 79.14(16) . . . . ? C16 P2 C20 C22 -33.5(2) . . . . ? C17 P2 C20 C22 71.71(19) . . . . ? Fe1 P2 C20 C22 -151.30(16) . . . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 26.34 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 0.564 _refine_diff_density_min -0.256 _refine_diff_density_rms 0.057 # Attachment 'wac4019xs.txt' data_wac4019xs _database_code_depnum_ccdc_archive 'CCDC 652416' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H51 Cl N3 P2 Si Zr' _chemical_formula_sum 'C22 H51 Cl N3 P2 Si Zr' _chemical_formula_weight 574.36 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.956(2) _cell_length_b 12.070(3) _cell_length_c 12.438(2) _cell_angle_alpha 111.752(4) _cell_angle_beta 110.138(3) _cell_angle_gamma 100.111(3) _cell_volume 1467.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 151(2) _cell_measurement_reflns_used 750 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 17.81 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.300 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 610 _exptl_absorpt_coefficient_mu 0.630 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 151(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9536 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.1337 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 26.38 _reflns_number_total 5812 _reflns_number_gt 3736 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.631' _computing_cell_refinement 'Bruker SAINT v7.07' _computing_data_reduction 'Bruker SAINT v7.07' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5812 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1144 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1487 _refine_ls_wR_factor_gt 0.1336 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.001 _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 0.11305(5) 0.93320(5) 0.44766(5) 0.02294(17) Uani 1 1 d . . . Cl1 Cl 0.33037(14) 1.09054(14) 0.59557(14) 0.0396(4) Uani 1 1 d . . . Si1 Si -0.02041(15) 0.65141(14) 0.30326(15) 0.0269(4) Uani 1 1 d . . . P1 P 0.14546(13) 0.98755(13) 0.25809(13) 0.0228(3) Uani 1 1 d . . . P2 P -0.33978(14) 0.69089(14) -0.05815(14) 0.0281(4) Uani 1 1 d . . . N1 N 0.1277(4) 0.7488(4) 0.4234(4) 0.0281(11) Uani 1 1 d . . . N2 N -0.0501(4) 0.7595(4) 0.2372(4) 0.0237(10) Uani 1 1 d . . . N3 N -0.0062(5) 1.0392(4) 0.4610(5) 0.0367(13) Uani 1 1 d . . . C1 C 0.2171(6) 0.7140(6) 0.5121(5) 0.0348(15) Uani 1 1 d . . . C2 C 0.2053(7) 0.7557(8) 0.6362(6) 0.063(2) Uani 1 1 d . . . H2A H 0.2240 0.8478 0.6769 0.094 Uiso 1 1 calc R . . H2B H 0.2655 0.7344 0.6950 0.094 Uiso 1 1 calc R . . H2C H 0.1185 0.7120 0.6178 0.094 Uiso 1 1 calc R . . C3 C 0.3531(6) 0.7728(6) 0.5374(7) 0.0525(19) Uani 1 1 d . . . H3C H 0.3772 0.8656 0.5768 0.079 Uiso 1 1 calc R . . H3D H 0.3591 0.7410 0.4555 0.079 Uiso 1 1 calc R . . H3E H 0.4105 0.7496 0.5964 0.079 Uiso 1 1 calc R . . C4 C 0.1887(7) 0.5698(6) 0.4515(6) 0.0516(19) Uani 1 1 d . . . H4A H 0.1019 0.5263 0.4330 0.077 Uiso 1 1 calc R . . H4B H 0.2490 0.5501 0.5119 0.077 Uiso 1 1 calc R . . H4C H 0.1971 0.5410 0.3708 0.077 Uiso 1 1 calc R . . C5 C -0.1441(6) 0.6145(6) 0.3553(6) 0.0396(16) Uani 1 1 d . . . H5A H -0.1899 0.5225 0.3094 0.059 Uiso 1 1 calc R . . H5B H -0.2040 0.6582 0.3351 0.059 Uiso 1 1 calc R . . H5C H -0.1039 0.6433 0.4488 0.059 Uiso 1 1 calc R . . C6 C -0.0385(6) 0.4973(5) 0.1730(6) 0.0447(17) Uani 1 1 d . . . H6A H -0.1022 0.4272 0.1648 0.067 Uiso 1 1 calc R . . H6B H 0.0431 0.4836 0.1955 0.067 Uiso 1 1 calc R . . H6C H -0.0660 0.5003 0.0906 0.067 Uiso 1 1 calc R . . C7 C -0.0139(5) 0.7358(5) 0.1293(5) 0.0267(13) Uani 1 1 d . . . H7A H -0.0857 0.6667 0.0481 0.032 Uiso 1 1 calc R . . H7B H 0.0593 0.7060 0.1469 0.032 Uiso 1 1 calc R . . C8 C 0.0212(5) 0.8519(5) 0.1089(5) 0.0280(13) Uani 1 1 d . . . H8A H -0.0551 0.8747 0.0785 0.034 Uiso 1 1 calc R . . H8B H 0.0510 0.8307 0.0412 0.034 Uiso 1 1 calc R . . C9 C 0.1284(6) 1.1290(5) 0.2386(6) 0.0322(14) Uani 1 1 d . . . H9A H 0.1297 1.1183 0.1554 0.039 Uiso 1 1 calc R . . C10 C 0.0015(6) 1.1422(6) 0.2332(7) 0.0457(17) Uani 1 1 d . . . H10A H -0.0065 1.2173 0.2224 0.069 Uiso 1 1 calc R . . H10B H -0.0014 1.1516 0.3138 0.069 Uiso 1 1 calc R . . H10C H -0.0686 1.0661 0.1599 0.069 Uiso 1 1 calc R . . C11 C 0.2396(6) 1.2466(5) 0.3494(7) 0.0506(18) Uani 1 1 d . . . H11A H 0.2310 1.3216 0.3388 0.076 Uiso 1 1 calc R . . H11B H 0.3193 1.2368 0.3493 0.076 Uiso 1 1 calc R . . H11C H 0.2404 1.2573 0.4318 0.076 Uiso 1 1 calc R . . C12 C 0.2977(5) 0.9829(5) 0.2531(5) 0.0299(13) Uani 1 1 d . . . H12A H 0.3669 1.0537 0.3370 0.036 Uiso 1 1 calc R . . C13 C 0.3149(6) 1.0046(6) 0.1463(6) 0.0419(16) Uani 1 1 d . . . H13A H 0.3978 1.0016 0.1511 0.063 Uiso 1 1 calc R . . H13B H 0.3106 1.0881 0.1569 0.063 Uiso 1 1 calc R . . H13C H 0.2475 0.9382 0.0620 0.063 Uiso 1 1 calc R . . C14 C 0.3164(6) 0.8592(6) 0.2475(6) 0.0425(16) Uani 1 1 d . . . H14A H 0.3976 0.8585 0.2457 0.064 Uiso 1 1 calc R . . H14B H 0.2470 0.7867 0.1691 0.064 Uiso 1 1 calc R . . H14C H 0.3167 0.8531 0.3239 0.064 Uiso 1 1 calc R . . C15 C -0.1736(5) 0.7796(5) 0.2076(5) 0.0264(13) Uani 1 1 d . . . H15A H -0.1664 0.8558 0.1940 0.032 Uiso 1 1 calc R . . H15B H -0.1895 0.7985 0.2844 0.032 Uiso 1 1 calc R . . C16 C -0.2887(5) 0.6699(5) 0.0905(5) 0.0338(14) Uani 1 1 d . . . H16A H -0.3605 0.6595 0.1127 0.041 Uiso 1 1 calc R . . H16B H -0.2687 0.5906 0.0713 0.041 Uiso 1 1 calc R . . C17 C -0.4437(6) 0.5258(5) -0.1840(5) 0.0369(15) Uani 1 1 d . . . H17A H -0.5050 0.4925 -0.1557 0.044 Uiso 1 1 calc R . . C18 C -0.3656(7) 0.4405(6) -0.2023(6) 0.0531(19) Uani 1 1 d . . . H18A H -0.4220 0.3538 -0.2687 0.080 Uiso 1 1 calc R . . H18B H -0.3194 0.4400 -0.1204 0.080 Uiso 1 1 calc R . . H18C H -0.3049 0.4725 -0.2296 0.080 Uiso 1 1 calc R . . C19 C -0.5177(7) 0.5246(6) -0.3108(6) 0.0539(19) Uani 1 1 d . . . H19A H -0.5727 0.4372 -0.3766 0.081 Uiso 1 1 calc R . . H19B H -0.4585 0.5578 -0.3390 0.081 Uiso 1 1 calc R . . H19C H -0.5699 0.5780 -0.2991 0.081 Uiso 1 1 calc R . . C20 C -0.4562(5) 0.7726(6) -0.0428(6) 0.0329(14) Uani 1 1 d . . . H20A H -0.4911 0.7837 -0.1221 0.040 Uiso 1 1 calc R . . C21 C -0.3878(6) 0.9061(5) 0.0727(6) 0.0395(16) Uani 1 1 d . . . H21A H -0.4496 0.9485 0.0799 0.059 Uiso 1 1 calc R . . H21B H -0.3238 0.9555 0.0599 0.059 Uiso 1 1 calc R . . H21C H -0.3463 0.8998 0.1522 0.059 Uiso 1 1 calc R . . C22 C -0.5688(6) 0.7042(7) -0.0339(7) 0.0556(19) Uani 1 1 d . . . H22A H -0.6233 0.7557 -0.0267 0.083 Uiso 1 1 calc R . . H22B H -0.5387 0.6908 0.0427 0.083 Uiso 1 1 calc R . . H22C H -0.6174 0.6218 -0.1117 0.083 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 0.0241(3) 0.0230(3) 0.0186(3) 0.0102(2) 0.0075(2) 0.0045(2) Cl1 0.0282(8) 0.0399(9) 0.0357(9) 0.0089(7) 0.0133(7) 0.0004(7) Si1 0.0278(9) 0.0244(8) 0.0279(9) 0.0146(7) 0.0097(7) 0.0081(7) P1 0.0231(8) 0.0234(8) 0.0250(8) 0.0124(7) 0.0126(7) 0.0088(7) P2 0.0224(8) 0.0332(9) 0.0295(8) 0.0168(7) 0.0110(7) 0.0079(7) N1 0.026(3) 0.030(3) 0.025(3) 0.016(2) 0.006(2) 0.008(2) N2 0.025(2) 0.026(2) 0.025(2) 0.014(2) 0.013(2) 0.010(2) N3 0.044(3) 0.033(3) 0.061(4) 0.032(3) 0.039(3) 0.022(3) C1 0.036(4) 0.043(4) 0.032(3) 0.027(3) 0.009(3) 0.016(3) C2 0.069(5) 0.109(6) 0.042(4) 0.047(5) 0.028(4) 0.067(5) C3 0.041(4) 0.069(5) 0.065(5) 0.046(4) 0.020(4) 0.033(4) C4 0.052(4) 0.060(5) 0.053(4) 0.033(4) 0.018(4) 0.036(4) C5 0.035(4) 0.042(4) 0.040(4) 0.024(3) 0.015(3) 0.000(3) C6 0.050(4) 0.023(3) 0.043(4) 0.010(3) 0.010(3) 0.009(3) C7 0.025(3) 0.024(3) 0.029(3) 0.010(3) 0.014(3) 0.005(3) C8 0.021(3) 0.043(4) 0.025(3) 0.021(3) 0.008(3) 0.012(3) C9 0.046(4) 0.029(3) 0.037(3) 0.023(3) 0.024(3) 0.018(3) C10 0.055(4) 0.052(4) 0.065(5) 0.041(4) 0.041(4) 0.036(4) C11 0.058(5) 0.021(3) 0.067(5) 0.015(3) 0.030(4) 0.008(3) C12 0.025(3) 0.034(3) 0.030(3) 0.017(3) 0.012(3) 0.005(3) C13 0.054(4) 0.046(4) 0.054(4) 0.031(4) 0.041(4) 0.027(4) C14 0.030(3) 0.059(4) 0.064(4) 0.042(4) 0.028(3) 0.026(3) C15 0.023(3) 0.029(3) 0.030(3) 0.015(3) 0.012(3) 0.012(3) C16 0.027(3) 0.044(4) 0.039(4) 0.028(3) 0.015(3) 0.013(3) C17 0.033(4) 0.035(4) 0.035(4) 0.013(3) 0.015(3) 0.003(3) C18 0.062(5) 0.043(4) 0.044(4) 0.011(4) 0.022(4) 0.020(4) C19 0.050(4) 0.051(4) 0.036(4) 0.015(4) 0.006(3) 0.003(4) C20 0.024(3) 0.046(4) 0.040(4) 0.028(3) 0.016(3) 0.017(3) C21 0.046(4) 0.043(4) 0.041(4) 0.023(3) 0.022(3) 0.027(3) C22 0.034(4) 0.057(5) 0.074(5) 0.027(4) 0.028(4) 0.012(4) _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 N3 1.975(5) 2_576 ? Zr1 N3 2.084(5) . ? Zr1 N1 2.179(4) . ? Zr1 N2 2.456(4) . ? Zr1 Cl1 2.4757(16) . ? Zr1 P1 2.7976(15) . ? Zr1 Si1 2.9889(17) . ? Si1 N1 1.702(5) . ? Si1 N2 1.805(4) . ? Si1 C5 1.857(6) . ? Si1 C6 1.875(6) . ? P1 C8 1.824(5) . ? P1 C9 1.847(5) . ? P1 C12 1.853(6) . ? P2 C17 1.856(6) . ? P2 C20 1.863(6) . ? P2 C16 1.865(5) . ? N1 C1 1.492(6) . ? N2 C15 1.481(6) . ? N2 C7 1.494(6) . ? N3 N3 1.576(9) 2_576 ? N3 Zr1 1.975(5) 2_576 ? C1 C2 1.502(8) . ? C1 C3 1.524(8) . ? C1 C4 1.535(8) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3C 0.9800 . ? C3 H3D 0.9800 . ? C3 H3E 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.527(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C11 1.519(8) . ? C9 C10 1.534(8) . ? C9 H9A 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.517(7) . ? C12 C14 1.528(8) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.523(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C19 1.513(8) . ? C17 C18 1.514(8) . ? C17 H17A 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C22 1.512(8) . ? C20 C21 1.531(8) . ? C20 H20A 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Zr1 N3 45.6(2) 2_576 . ? N3 Zr1 N1 104.06(18) 2_576 . ? N3 Zr1 N1 142.87(18) . . ? N3 Zr1 N2 98.53(19) 2_576 . ? N3 Zr1 N2 92.54(17) . . ? N1 Zr1 N2 68.30(15) . . ? N3 Zr1 Cl1 108.56(16) 2_576 . ? N3 Zr1 Cl1 104.74(15) . . ? N1 Zr1 Cl1 105.93(12) . . ? N2 Zr1 Cl1 152.83(11) . . ? N3 Zr1 P1 136.42(14) 2_576 . ? N3 Zr1 P1 91.29(13) . . ? N1 Zr1 P1 111.53(12) . . ? N2 Zr1 P1 73.27(10) . . ? Cl1 Zr1 P1 85.34(5) . . ? N3 Zr1 Si1 93.08(14) 2_576 . ? N3 Zr1 Si1 114.63(14) . . ? N1 Zr1 Si1 34.11(12) . . ? N2 Zr1 Si1 37.12(10) . . ? Cl1 Zr1 Si1 139.49(5) . . ? P1 Zr1 Si1 102.37(5) . . ? N1 Si1 N2 96.3(2) . . ? N1 Si1 C5 116.3(3) . . ? N2 Si1 C5 108.5(2) . . ? N1 Si1 C6 118.7(3) . . ? N2 Si1 C6 109.5(2) . . ? C5 Si1 C6 106.6(3) . . ? N1 Si1 Zr1 45.89(15) . . ? N2 Si1 Zr1 55.19(14) . . ? C5 Si1 Zr1 107.5(2) . . ? C6 Si1 Zr1 145.7(2) . . ? C8 P1 C9 105.2(3) . . ? C8 P1 C12 106.0(3) . . ? C9 P1 C12 103.8(3) . . ? C8 P1 Zr1 102.10(17) . . ? C9 P1 Zr1 124.66(19) . . ? C12 P1 Zr1 113.45(17) . . ? C17 P2 C20 102.7(3) . . ? C17 P2 C16 100.8(3) . . ? C20 P2 C16 102.1(3) . . ? C1 N1 Si1 125.8(4) . . ? C1 N1 Zr1 130.9(3) . . ? Si1 N1 Zr1 100.0(2) . . ? C15 N2 C7 112.7(4) . . ? C15 N2 Si1 118.7(3) . . ? C7 N2 Si1 111.3(3) . . ? C15 N2 Zr1 110.0(3) . . ? C7 N2 Zr1 114.1(3) . . ? Si1 N2 Zr1 87.69(17) . . ? N3 N3 Zr1 70.9(3) 2_576 2_576 ? N3 N3 Zr1 63.5(3) 2_576 . ? Zr1 N3 Zr1 134.4(2) 2_576 . ? N1 C1 C2 109.7(5) . . ? N1 C1 C3 110.6(5) . . ? C2 C1 C3 111.2(5) . . ? N1 C1 C4 111.5(5) . . ? C2 C1 C4 108.3(5) . . ? C3 C1 C4 105.5(5) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3C 109.5 . . ? C1 C3 H3D 109.5 . . ? H3C C3 H3D 109.5 . . ? C1 C3 H3E 109.5 . . ? H3C C3 H3E 109.5 . . ? H3D C3 H3E 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 114.3(4) . . ? N2 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? N2 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C7 C8 P1 111.3(4) . . ? C7 C8 H8A 109.4 . . ? P1 C8 H8A 109.4 . . ? C7 C8 H8B 109.4 . . ? P1 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C11 C9 C10 111.1(5) . . ? C11 C9 P1 109.4(4) . . ? C10 C9 P1 110.3(4) . . ? C11 C9 H9A 108.7 . . ? C10 C9 H9A 108.7 . . ? P1 C9 H9A 108.7 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C14 111.0(5) . . ? C13 C12 P1 114.7(4) . . ? C14 C12 P1 110.4(4) . . ? C13 C12 H12A 106.7 . . ? C14 C12 H12A 106.7 . . ? P1 C12 H12A 106.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 C16 116.3(4) . . ? N2 C15 H15A 108.2 . . ? C16 C15 H15A 108.2 . . ? N2 C15 H15B 108.2 . . ? C16 C15 H15B 108.2 . . ? H15A C15 H15B 107.4 . . ? C15 C16 P2 114.2(4) . . ? C15 C16 H16A 108.7 . . ? P2 C16 H16A 108.7 . . ? C15 C16 H16B 108.7 . . ? P2 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? C19 C17 C18 109.8(5) . . ? C19 C17 P2 110.0(4) . . ? C18 C17 P2 110.7(4) . . ? C19 C17 H17A 108.8 . . ? C18 C17 H17A 108.8 . . ? P2 C17 H17A 108.8 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C20 C21 109.3(5) . . ? C22 C20 P2 116.8(4) . . ? C21 C20 P2 110.0(4) . . ? C22 C20 H20A 106.7 . . ? C21 C20 H20A 106.7 . . ? P2 C20 H20A 106.7 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Zr1 Si1 N1 -110.8(3) 2_576 . . . ? N3 Zr1 Si1 N1 -152.5(3) . . . . ? N2 Zr1 Si1 N1 149.2(3) . . . . ? Cl1 Zr1 Si1 N1 12.9(2) . . . . ? P1 Zr1 Si1 N1 110.3(2) . . . . ? N3 Zr1 Si1 N2 100.1(2) 2_576 . . . ? N3 Zr1 Si1 N2 58.3(2) . . . . ? N1 Zr1 Si1 N2 -149.2(3) . . . . ? Cl1 Zr1 Si1 N2 -136.29(19) . . . . ? P1 Zr1 Si1 N2 -38.91(18) . . . . ? N3 Zr1 Si1 C5 -0.7(2) 2_576 . . . ? N3 Zr1 Si1 C5 -42.5(3) . . . . ? N1 Zr1 Si1 C5 110.0(3) . . . . ? N2 Zr1 Si1 C5 -100.8(3) . . . . ? Cl1 Zr1 Si1 C5 122.9(2) . . . . ? P1 Zr1 Si1 C5 -139.7(2) . . . . ? N3 Zr1 Si1 C6 172.7(4) 2_576 . . . ? N3 Zr1 Si1 C6 131.0(4) . . . . ? N1 Zr1 Si1 C6 -76.5(4) . . . . ? N2 Zr1 Si1 C6 72.6(4) . . . . ? Cl1 Zr1 Si1 C6 -63.7(4) . . . . ? P1 Zr1 Si1 C6 33.7(4) . . . . ? N3 Zr1 P1 C8 -85.4(3) 2_576 . . . ? N3 Zr1 P1 C8 -92.9(2) . . . . ? N1 Zr1 P1 C8 57.1(2) . . . . ? N2 Zr1 P1 C8 -0.7(2) . . . . ? Cl1 Zr1 P1 C8 162.39(19) . . . . ? Si1 Zr1 P1 C8 22.65(19) . . . . ? N3 Zr1 P1 C9 32.9(3) 2_576 . . . ? N3 Zr1 P1 C9 25.4(3) . . . . ? N1 Zr1 P1 C9 175.4(3) . . . . ? N2 Zr1 P1 C9 117.7(3) . . . . ? Cl1 Zr1 P1 C9 -79.3(2) . . . . ? Si1 Zr1 P1 C9 141.0(2) . . . . ? N3 Zr1 P1 C12 161.0(3) 2_576 . . . ? N3 Zr1 P1 C12 153.5(2) . . . . ? N1 Zr1 P1 C12 -56.5(2) . . . . ? N2 Zr1 P1 C12 -114.3(2) . . . . ? Cl1 Zr1 P1 C12 48.8(2) . . . . ? Si1 Zr1 P1 C12 -91.0(2) . . . . ? N2 Si1 N1 C1 -173.7(5) . . . . ? C5 Si1 N1 C1 72.1(5) . . . . ? C6 Si1 N1 C1 -57.4(5) . . . . ? Zr1 Si1 N1 C1 161.3(6) . . . . ? N2 Si1 N1 Zr1 25.0(2) . . . . ? C5 Si1 N1 Zr1 -89.2(3) . . . . ? C6 Si1 N1 Zr1 141.3(3) . . . . ? N3 Zr1 N1 C1 -85.6(5) 2_576 . . . ? N3 Zr1 N1 C1 -115.8(5) . . . . ? N2 Zr1 N1 C1 -179.3(5) . . . . ? Cl1 Zr1 N1 C1 28.8(5) . . . . ? P1 Zr1 N1 C1 120.0(5) . . . . ? Si1 Zr1 N1 C1 -159.9(6) . . . . ? N3 Zr1 N1 Si1 74.3(2) 2_576 . . . ? N3 Zr1 N1 Si1 44.0(4) . . . . ? N2 Zr1 N1 Si1 -19.44(18) . . . . ? Cl1 Zr1 N1 Si1 -171.34(16) . . . . ? P1 Zr1 N1 Si1 -80.1(2) . . . . ? N1 Si1 N2 C15 -133.4(4) . . . . ? C5 Si1 N2 C15 -12.9(4) . . . . ? C6 Si1 N2 C15 103.2(4) . . . . ? Zr1 Si1 N2 C15 -111.7(4) . . . . ? N1 Si1 N2 C7 93.3(4) . . . . ? C5 Si1 N2 C7 -146.2(4) . . . . ? C6 Si1 N2 C7 -30.1(4) . . . . ? Zr1 Si1 N2 C7 115.1(4) . . . . ? N1 Si1 N2 Zr1 -21.7(2) . . . . ? C5 Si1 N2 Zr1 98.8(2) . . . . ? C6 Si1 N2 Zr1 -145.2(2) . . . . ? N3 Zr1 N2 C15 36.0(3) 2_576 . . . ? N3 Zr1 N2 C15 -9.4(3) . . . . ? N1 Zr1 N2 C15 137.8(4) . . . . ? Cl1 Zr1 N2 C15 -139.5(3) . . . . ? P1 Zr1 N2 C15 -100.0(3) . . . . ? Si1 Zr1 N2 C15 119.8(4) . . . . ? N3 Zr1 N2 C7 163.8(3) 2_576 . . . ? N3 Zr1 N2 C7 118.4(3) . . . . ? N1 Zr1 N2 C7 -94.4(3) . . . . ? Cl1 Zr1 N2 C7 -11.7(5) . . . . ? P1 Zr1 N2 C7 27.8(3) . . . . ? Si1 Zr1 N2 C7 -112.4(4) . . . . ? N3 Zr1 N2 Si1 -83.80(19) 2_576 . . . ? N3 Zr1 N2 Si1 -129.26(19) . . . . ? N1 Zr1 N2 Si1 18.02(17) . . . . ? Cl1 Zr1 N2 Si1 100.6(2) . . . . ? P1 Zr1 N2 Si1 140.16(17) . . . . ? N1 Zr1 N3 N3 43.1(5) . . . 2_576 ? N2 Zr1 N3 N3 99.5(4) . . . 2_576 ? Cl1 Zr1 N3 N3 -101.7(3) . . . 2_576 ? P1 Zr1 N3 N3 172.8(3) . . . 2_576 ? Si1 Zr1 N3 N3 68.5(4) . . . 2_576 ? N3 Zr1 N3 Zr1 0.000(1) 2_576 . . 2_576 ? N1 Zr1 N3 Zr1 43.1(5) . . . 2_576 ? N2 Zr1 N3 Zr1 99.5(4) . . . 2_576 ? Cl1 Zr1 N3 Zr1 -101.7(3) . . . 2_576 ? P1 Zr1 N3 Zr1 172.8(3) . . . 2_576 ? Si1 Zr1 N3 Zr1 68.5(4) . . . 2_576 ? Si1 N1 C1 C2 -95.7(6) . . . . ? Zr1 N1 C1 C2 59.6(7) . . . . ? Si1 N1 C1 C3 141.3(5) . . . . ? Zr1 N1 C1 C3 -63.4(7) . . . . ? Si1 N1 C1 C4 24.2(7) . . . . ? Zr1 N1 C1 C4 179.5(4) . . . . ? C15 N2 C7 C8 69.9(6) . . . . ? Si1 N2 C7 C8 -153.9(4) . . . . ? Zr1 N2 C7 C8 -56.6(5) . . . . ? N2 C7 C8 P1 54.2(5) . . . . ? C9 P1 C8 C7 -156.6(4) . . . . ? C12 P1 C8 C7 93.8(4) . . . . ? Zr1 P1 C8 C7 -25.2(4) . . . . ? C8 P1 C9 C11 -171.8(4) . . . . ? C12 P1 C9 C11 -60.6(5) . . . . ? Zr1 P1 C9 C11 71.3(5) . . . . ? C8 P1 C9 C10 65.7(5) . . . . ? C12 P1 C9 C10 176.9(4) . . . . ? Zr1 P1 C9 C10 -51.2(5) . . . . ? C8 P1 C12 C13 65.5(5) . . . . ? C9 P1 C12 C13 -45.1(5) . . . . ? Zr1 P1 C12 C13 176.7(4) . . . . ? C8 P1 C12 C14 -60.8(5) . . . . ? C9 P1 C12 C14 -171.4(4) . . . . ? Zr1 P1 C12 C14 50.4(4) . . . . ? C7 N2 C15 C16 60.5(6) . . . . ? Si1 N2 C15 C16 -72.2(5) . . . . ? Zr1 N2 C15 C16 -170.9(4) . . . . ? N2 C15 C16 P2 -100.7(5) . . . . ? C17 P2 C16 C15 163.8(4) . . . . ? C20 P2 C16 C15 -90.5(4) . . . . ? C20 P2 C17 C19 63.4(5) . . . . ? C16 P2 C17 C19 168.5(5) . . . . ? C20 P2 C17 C18 -175.2(4) . . . . ? C16 P2 C17 C18 -70.0(5) . . . . ? C17 P2 C20 C22 46.0(5) . . . . ? C16 P2 C20 C22 -58.2(5) . . . . ? C17 P2 C20 C21 171.3(4) . . . . ? C16 P2 C20 C21 67.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.166 _refine_diff_density_min -0.639 _refine_diff_density_rms 0.123 # Attachment 'wac5080xs.txt' data_wac5080xs _database_code_depnum_ccdc_archive 'CCDC 652417' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H51 Mn N3 P2 Si' _chemical_formula_sum 'C22 H51 Mn N3 P2 Si' _chemical_formula_weight 502.63 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' Mn Mn 0.3368 0.7283 '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, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.381(2) _cell_length_b 15.4611(17) _cell_length_c 19.772(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5619.0(11) _cell_formula_units_Z 8 _cell_measurement_temperature 151(2) _cell_measurement_reflns_used 1333 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 18.6 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.188 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 0.640 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 151(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 26856 _diffrn_reflns_av_R_equivalents 0.1055 _diffrn_reflns_av_sigmaI/netI 0.0887 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 24.71 _reflns_number_total 4787 _reflns_number_gt 3249 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.631' _computing_cell_refinement 'Bruker SAINT v7.07' _computing_data_reduction 'Bruker SAINT v7.07' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4787 _refine_ls_number_parameters 260 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0907 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1382 _refine_ls_wR_factor_gt 0.1263 _refine_ls_goodness_of_fit_ref 1.190 _refine_ls_restrained_S_all 1.190 _refine_ls_shift/su_max 0.006 _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 Mn1 Mn 0.02079(3) 0.13223(4) 0.43336(3) 0.01939(19) Uani 1 1 d . . . Si1 Si 0.05661(6) 0.33101(7) 0.41019(6) 0.0246(3) Uani 1 1 d . . . P1 P 0.12807(6) 0.09643(7) 0.35641(6) 0.0283(3) Uani 1 1 d . . . P2 P -0.08523(6) 0.15125(6) 0.35117(5) 0.0222(3) Uani 1 1 d . . . N1 N 0.04894(17) 0.25301(19) 0.46959(15) 0.0205(8) Uani 1 1 d . . . N2 N 0.05055(17) 0.2828(2) 0.33020(16) 0.0225(8) Uani 1 1 d . . . N3 N 0.00361(16) 0.03155(19) 0.48231(16) 0.0227(8) Uani 1 1 d . . . C1 C 0.0497(2) 0.2706(3) 0.5437(2) 0.0265(10) Uani 1 1 d . . . C2 C -0.0271(2) 0.2904(3) 0.5692(2) 0.0447(13) Uani 1 1 d . . . H2A H -0.0595 0.2422 0.5577 0.067 Uiso 1 1 calc R . . H2B H -0.0449 0.3435 0.5479 0.067 Uiso 1 1 calc R . . H2C H -0.0260 0.2980 0.6184 0.067 Uiso 1 1 calc R . . C3 C 0.0988(2) 0.3469(3) 0.5629(2) 0.0352(11) Uani 1 1 d . . . H3C H 0.1486 0.3354 0.5476 0.053 Uiso 1 1 calc R . . H3D H 0.0985 0.3544 0.6121 0.053 Uiso 1 1 calc R . . H3E H 0.0807 0.3997 0.5413 0.053 Uiso 1 1 calc R . . C4 C 0.0791(3) 0.1921(3) 0.5806(2) 0.0381(12) Uani 1 1 d . . . H4A H 0.0491 0.1415 0.5698 0.057 Uiso 1 1 calc R . . H4B H 0.0778 0.2026 0.6295 0.057 Uiso 1 1 calc R . . H4C H 0.1294 0.1814 0.5664 0.057 Uiso 1 1 calc R . . C5 C -0.0139(3) 0.4196(3) 0.4140(2) 0.0401(12) Uani 1 1 d . . . H5A H -0.0626 0.3938 0.4147 0.060 Uiso 1 1 calc R . . H5B H -0.0091 0.4569 0.3742 0.060 Uiso 1 1 calc R . . H5C H -0.0066 0.4540 0.4550 0.060 Uiso 1 1 calc R . . C6 C 0.1449(3) 0.3936(3) 0.4096(2) 0.0424(13) Uani 1 1 d . . . H6A H 0.1859 0.3530 0.4080 0.064 Uiso 1 1 calc R . . H6B H 0.1482 0.4288 0.4506 0.064 Uiso 1 1 calc R . . H6C H 0.1464 0.4312 0.3697 0.064 Uiso 1 1 calc R . . C7 C 0.1163(2) 0.2590(3) 0.2929(2) 0.0309(10) Uani 1 1 d . . . H7A H 0.1589 0.2810 0.3183 0.037 Uiso 1 1 calc R . . H7B H 0.1154 0.2895 0.2488 0.037 Uiso 1 1 calc R . . C8 C 0.1282(2) 0.1631(3) 0.2793(2) 0.0308(10) Uani 1 1 d . . . H8A H 0.1754 0.1555 0.2558 0.037 Uiso 1 1 calc R . . H8B H 0.0895 0.1421 0.2486 0.037 Uiso 1 1 calc R . . C9 C 0.2096(3) 0.1330(4) 0.4027(3) 0.0541(15) Uani 1 1 d . . . H9A H 0.1948 0.1898 0.4225 0.065 Uiso 1 1 calc R . . C10 C 0.2226(3) 0.0755(3) 0.4640(2) 0.0488(14) Uani 1 1 d . . . H10A H 0.2657 0.0958 0.4884 0.073 Uiso 1 1 calc R . . H10B H 0.2302 0.0158 0.4491 0.073 Uiso 1 1 calc R . . H10C H 0.1801 0.0781 0.4940 0.073 Uiso 1 1 calc R . . C11 C 0.2775(3) 0.1532(4) 0.3645(3) 0.0549(15) Uani 1 1 d . . . H11A H 0.3153 0.1720 0.3962 0.082 Uiso 1 1 calc R . . H11B H 0.2677 0.1995 0.3319 0.082 Uiso 1 1 calc R . . H11C H 0.2939 0.1014 0.3404 0.082 Uiso 1 1 calc R . . C12 C 0.1272(6) -0.0182(6) 0.3141(5) 0.039(2) Uiso 0.50 1 d P . . C12A C 0.1642(5) -0.0084(5) 0.3301(4) 0.023(2) Uiso 0.50 1 d P . . C13 C 0.1256(3) -0.0839(3) 0.3719(3) 0.0517(14) Uani 1 1 d . . . C14 C 0.1874(7) -0.0348(7) 0.2659(6) 0.063(3) Uiso 0.50 1 d P . . C14A C 0.1451(5) -0.0294(6) 0.2516(5) 0.036(2) Uiso 0.50 1 d P . . C15 C -0.0142(2) 0.2921(3) 0.2876(2) 0.0280(10) Uani 1 1 d . . . H15A H 0.0010 0.3166 0.2435 0.034 Uiso 1 1 calc R . . H15B H -0.0472 0.3345 0.3092 0.034 Uiso 1 1 calc R . . C16 C -0.0576(2) 0.2085(2) 0.2741(2) 0.0265(10) Uani 1 1 d . . . H16A H -0.0275 0.1692 0.2462 0.032 Uiso 1 1 calc R . . H16B H -0.1017 0.2232 0.2477 0.032 Uiso 1 1 calc R . . C17 C -0.1562(2) 0.2237(3) 0.3862(2) 0.0296(10) Uani 1 1 d . . . H17A H -0.1328 0.2818 0.3910 0.036 Uiso 1 1 calc R . . C18 C -0.1786(2) 0.1963(3) 0.4581(2) 0.0460(13) Uani 1 1 d . . . H18A H -0.2158 0.2361 0.4753 0.069 Uiso 1 1 calc R . . H18B H -0.1360 0.1979 0.4879 0.069 Uiso 1 1 calc R . . H18C H -0.1984 0.1374 0.4569 0.069 Uiso 1 1 calc R . . C19 C -0.2231(3) 0.2374(3) 0.3416(3) 0.0466(13) Uani 1 1 d . . . H19A H -0.2571 0.2767 0.3644 0.070 Uiso 1 1 calc R . . H19B H -0.2470 0.1817 0.3335 0.070 Uiso 1 1 calc R . . H19C H -0.2082 0.2626 0.2983 0.070 Uiso 1 1 calc R . . C20 C -0.1335(2) 0.0575(3) 0.3142(2) 0.0320(11) Uani 1 1 d . . . H20A H -0.1694 0.0792 0.2802 0.038 Uiso 1 1 calc R . . C21 C -0.1743(3) 0.0064(3) 0.3683(3) 0.0457(13) Uani 1 1 d . . . H21A H -0.1996 -0.0424 0.3472 0.069 Uiso 1 1 calc R . . H21B H -0.2099 0.0442 0.3905 0.069 Uiso 1 1 calc R . . H21C H -0.1397 -0.0152 0.4020 0.069 Uiso 1 1 calc R . . C22 C -0.0790(3) -0.0011(3) 0.2783(3) 0.0502(14) Uani 1 1 d . . . H22A H -0.1047 -0.0506 0.2585 0.075 Uiso 1 1 calc R . . H22B H -0.0428 -0.0218 0.3109 0.075 Uiso 1 1 calc R . . H22C H -0.0545 0.0314 0.2423 0.075 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 Mn1 0.0231(4) 0.0183(3) 0.0167(3) 0.0012(3) 0.0011(3) -0.0013(2) Si1 0.0305(7) 0.0196(6) 0.0235(7) 0.0008(5) -0.0036(5) -0.0045(5) P1 0.0316(6) 0.0264(6) 0.0269(7) 0.0042(5) 0.0090(5) 0.0043(5) P2 0.0249(6) 0.0234(6) 0.0182(6) 0.0002(4) -0.0018(5) -0.0034(4) N1 0.027(2) 0.0190(17) 0.0154(18) 0.0006(14) 0.0005(14) -0.0009(14) N2 0.026(2) 0.0232(19) 0.0184(19) 0.0009(14) 0.0013(15) -0.0021(14) N3 0.0257(19) 0.0230(19) 0.020(2) 0.0000(14) -0.0005(15) -0.0036(15) C1 0.031(3) 0.028(2) 0.020(2) -0.0070(18) -0.0041(19) -0.0002(19) C2 0.035(3) 0.075(4) 0.025(3) -0.016(3) 0.004(2) 0.001(2) C3 0.043(3) 0.035(3) 0.029(3) -0.007(2) -0.009(2) -0.002(2) C4 0.064(3) 0.033(3) 0.017(2) 0.001(2) -0.011(2) -0.003(2) C5 0.061(3) 0.023(2) 0.036(3) -0.005(2) -0.010(2) 0.005(2) C6 0.051(3) 0.041(3) 0.035(3) 0.005(2) -0.005(2) -0.022(2) C7 0.032(3) 0.035(3) 0.025(2) 0.008(2) 0.006(2) -0.002(2) C8 0.033(3) 0.034(3) 0.026(2) 0.001(2) 0.007(2) 0.001(2) C9 0.037(3) 0.086(4) 0.039(3) 0.023(3) 0.005(2) 0.007(3) C10 0.047(3) 0.061(4) 0.038(3) 0.014(3) 0.006(2) 0.022(3) C11 0.043(3) 0.074(4) 0.047(3) 0.014(3) 0.003(3) -0.010(3) C13 0.072(4) 0.026(3) 0.057(4) 0.010(2) 0.015(3) 0.003(2) C15 0.030(3) 0.030(2) 0.023(2) 0.0040(19) 0.003(2) -0.0021(19) C16 0.032(3) 0.029(2) 0.018(2) 0.0021(18) -0.0036(19) 0.0013(19) C17 0.026(2) 0.032(3) 0.031(3) -0.009(2) 0.004(2) -0.0007(19) C18 0.034(3) 0.078(4) 0.026(3) -0.008(3) -0.003(2) 0.004(3) C19 0.044(3) 0.049(3) 0.047(3) 0.009(3) -0.001(3) 0.015(2) C20 0.037(3) 0.027(2) 0.032(3) 0.001(2) -0.012(2) -0.0059(19) C21 0.052(3) 0.026(2) 0.059(4) 0.006(2) -0.006(3) -0.014(2) C22 0.063(4) 0.035(3) 0.053(3) -0.013(3) 0.002(3) -0.003(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 Mn1 N3 1.860(3) . ? Mn1 N1 2.066(3) . ? Mn1 P1 2.5514(12) . ? Mn1 P2 2.5543(12) . ? Si1 N1 1.689(3) . ? Si1 N2 1.752(3) . ? Si1 C5 1.887(4) . ? Si1 C6 1.889(4) . ? P1 C12A 1.827(8) . ? P1 C8 1.840(4) . ? P1 C9 1.844(5) . ? P1 C12 1.960(9) . ? P2 C16 1.834(4) . ? P2 C20 1.850(4) . ? P2 C17 1.854(4) . ? N1 C1 1.489(5) . ? N2 C7 1.464(5) . ? N2 C15 1.465(5) . ? N3 N3 1.208(6) 5_556 ? C1 C4 1.516(6) . ? C1 C2 1.530(6) . ? C1 C3 1.533(5) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3C 0.9800 . ? C3 H3D 0.9800 . ? C3 H3E 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.524(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C11 1.491(6) . ? C9 C10 1.522(6) . ? C9 H9A 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C12A 0.764(10) . ? C12 C14A 1.291(13) . ? C12 C14 1.483(15) . ? C12 C13 1.528(10) . ? C12A C14 1.400(14) . ? C12A C13 1.595(9) . ? C12A C14A 1.624(13) . ? C14 C14A 0.832(13) . ? C15 C16 1.541(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C19 1.529(6) . ? C17 C18 1.539(6) . ? C17 H17A 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C22 1.525(6) . ? C20 C21 1.527(6) . ? C20 H20A 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Mn1 N1 128.21(13) . . ? N3 Mn1 P1 105.07(10) . . ? N1 Mn1 P1 102.08(9) . . ? N3 Mn1 P2 107.33(10) . . ? N1 Mn1 P2 107.91(9) . . ? P1 Mn1 P2 103.61(4) . . ? N1 Si1 N2 108.56(15) . . ? N1 Si1 C5 115.67(19) . . ? N2 Si1 C5 107.51(18) . . ? N1 Si1 C6 116.22(19) . . ? N2 Si1 C6 105.46(19) . . ? C5 Si1 C6 102.6(2) . . ? C12A P1 C8 105.1(3) . . ? C12A P1 C9 96.8(3) . . ? C8 P1 C9 103.8(2) . . ? C12A P1 C12 22.9(3) . . ? C8 P1 C12 98.8(3) . . ? C9 P1 C12 119.7(4) . . ? C12A P1 Mn1 130.0(3) . . ? C8 P1 Mn1 111.95(14) . . ? C9 P1 Mn1 105.42(17) . . ? C12 P1 Mn1 116.4(3) . . ? C16 P2 C20 100.51(19) . . ? C16 P2 C17 102.3(2) . . ? C20 P2 C17 106.51(19) . . ? C16 P2 Mn1 111.89(14) . . ? C20 P2 Mn1 121.80(14) . . ? C17 P2 Mn1 111.63(14) . . ? C1 N1 Si1 123.5(3) . . ? C1 N1 Mn1 120.6(2) . . ? Si1 N1 Mn1 115.16(16) . . ? C7 N2 C15 113.9(3) . . ? C7 N2 Si1 120.6(3) . . ? C15 N2 Si1 121.9(3) . . ? N3 N3 Mn1 174.9(4) 5_556 . ? N1 C1 C4 109.3(3) . . ? N1 C1 C2 110.6(3) . . ? C4 C1 C2 109.2(4) . . ? N1 C1 C3 113.0(3) . . ? C4 C1 C3 106.7(3) . . ? C2 C1 C3 107.9(4) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3C 109.5 . . ? C1 C3 H3D 109.5 . . ? H3C C3 H3D 109.5 . . ? C1 C3 H3E 109.5 . . ? H3C C3 H3E 109.5 . . ? H3D C3 H3E 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 116.8(3) . . ? N2 C7 H7A 108.1 . . ? C8 C7 H7A 108.1 . . ? N2 C7 H7B 108.1 . . ? C8 C7 H7B 108.1 . . ? H7A C7 H7B 107.3 . . ? C7 C8 P1 113.5(3) . . ? C7 C8 H8A 108.9 . . ? P1 C8 H8A 108.9 . . ? C7 C8 H8B 108.9 . . ? P1 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C11 C9 C10 113.2(4) . . ? C11 C9 P1 119.6(4) . . ? C10 C9 P1 110.1(4) . . ? C11 C9 H9A 104.0 . . ? C10 C9 H9A 104.0 . . ? P1 C9 H9A 104.0 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C12A C12 C14A 101.3(13) . . ? C12A C12 C14 68.7(11) . . ? C14A C12 C14 34.0(6) . . ? C12A C12 C13 80.8(11) . . ? C14A C12 C13 129.2(8) . . ? C14 C12 C13 112.3(8) . . ? C12A C12 P1 68.7(10) . . ? C14A C12 P1 121.8(8) . . ? C14 C12 P1 115.1(7) . . ? C13 C12 P1 106.4(6) . . ? C12 C12A C14 80.8(12) . . ? C12 C12A C13 71.0(10) . . ? C14 C12A C13 113.1(7) . . ? C12 C12A C14A 51.3(10) . . ? C14 C12A C14A 30.8(5) . . ? C13 C12A C14A 104.7(6) . . ? C12 C12A P1 88.3(11) . . ? C14 C12A P1 128.8(7) . . ? C13 C12A P1 109.9(5) . . ? C14A C12A P1 111.8(6) . . ? C12 C13 C12A 28.2(4) . . ? C14A C14 C12A 89.7(13) . . ? C14A C14 C12 60.3(11) . . ? C12A C14 C12 30.6(5) . . ? C14 C14A C12 85.7(13) . . ? C14 C14A C12A 59.5(11) . . ? C12 C14A C12A 27.5(5) . . ? N2 C15 C16 115.9(3) . . ? N2 C15 H15A 108.3 . . ? C16 C15 H15A 108.3 . . ? N2 C15 H15B 108.3 . . ? C16 C15 H15B 108.3 . . ? H15A C15 H15B 107.4 . . ? C15 C16 P2 113.8(3) . . ? C15 C16 H16A 108.8 . . ? P2 C16 H16A 108.8 . . ? C15 C16 H16B 108.8 . . ? P2 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? C19 C17 C18 110.8(4) . . ? C19 C17 P2 115.8(3) . . ? C18 C17 P2 111.5(3) . . ? C19 C17 H17A 106.0 . . ? C18 C17 H17A 106.0 . . ? P2 C17 H17A 106.0 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C20 C21 110.0(4) . . ? C22 C20 P2 109.6(3) . . ? C21 C20 P2 111.3(3) . . ? C22 C20 H20A 108.6 . . ? C21 C20 H20A 108.6 . . ? P2 C20 H20A 108.6 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Mn1 P1 C12A 18.9(4) . . . . ? N1 Mn1 P1 C12A 154.4(4) . . . . ? P2 Mn1 P1 C12A -93.6(4) . . . . ? N3 Mn1 P1 C8 153.68(18) . . . . ? N1 Mn1 P1 C8 -70.86(18) . . . . ? P2 Mn1 P1 C8 41.19(16) . . . . ? N3 Mn1 P1 C9 -94.1(2) . . . . ? N1 Mn1 P1 C9 41.3(2) . . . . ? P2 Mn1 P1 C9 153.36(18) . . . . ? N3 Mn1 P1 C12 41.1(4) . . . . ? N1 Mn1 P1 C12 176.6(3) . . . . ? P2 Mn1 P1 C12 -71.4(3) . . . . ? N3 Mn1 P2 C16 -150.69(17) . . . . ? N1 Mn1 P2 C16 67.89(17) . . . . ? P1 Mn1 P2 C16 -39.85(15) . . . . ? N3 Mn1 P2 C20 -32.0(2) . . . . ? N1 Mn1 P2 C20 -173.40(19) . . . . ? P1 Mn1 P2 C20 78.87(17) . . . . ? N3 Mn1 P2 C17 95.29(18) . . . . ? N1 Mn1 P2 C17 -46.13(18) . . . . ? P1 Mn1 P2 C17 -153.86(15) . . . . ? N2 Si1 N1 C1 -178.4(3) . . . . ? C5 Si1 N1 C1 -57.5(4) . . . . ? C6 Si1 N1 C1 63.0(4) . . . . ? N2 Si1 N1 Mn1 -8.3(2) . . . . ? C5 Si1 N1 Mn1 112.6(2) . . . . ? C6 Si1 N1 Mn1 -126.9(2) . . . . ? N3 Mn1 N1 C1 -7.0(3) . . . . ? P1 Mn1 N1 C1 -127.5(3) . . . . ? P2 Mn1 N1 C1 123.8(3) . . . . ? N3 Mn1 N1 Si1 -177.37(16) . . . . ? P1 Mn1 N1 Si1 62.17(17) . . . . ? P2 Mn1 N1 Si1 -46.62(18) . . . . ? N1 Si1 N2 C7 -95.5(3) . . . . ? C5 Si1 N2 C7 138.7(3) . . . . ? C6 Si1 N2 C7 29.7(3) . . . . ? N1 Si1 N2 C15 106.9(3) . . . . ? C5 Si1 N2 C15 -18.9(3) . . . . ? C6 Si1 N2 C15 -127.9(3) . . . . ? N1 Mn1 N3 N3 -32(5) . . . 5_556 ? P1 Mn1 N3 N3 87(5) . . . 5_556 ? P2 Mn1 N3 N3 -163(5) . . . 5_556 ? Si1 N1 C1 C4 -151.9(3) . . . . ? Mn1 N1 C1 C4 38.6(4) . . . . ? Si1 N1 C1 C2 87.8(4) . . . . ? Mn1 N1 C1 C2 -81.8(4) . . . . ? Si1 N1 C1 C3 -33.3(5) . . . . ? Mn1 N1 C1 C3 157.1(3) . . . . ? C15 N2 C7 C8 -84.9(4) . . . . ? Si1 N2 C7 C8 115.8(4) . . . . ? N2 C7 C8 P1 -55.9(5) . . . . ? C12A P1 C8 C7 -166.9(4) . . . . ? C9 P1 C8 C7 -65.9(4) . . . . ? C12 P1 C8 C7 170.5(4) . . . . ? Mn1 P1 C8 C7 47.3(3) . . . . ? C12A P1 C9 C11 68.2(5) . . . . ? C8 P1 C9 C11 -39.2(5) . . . . ? C12 P1 C9 C11 69.6(6) . . . . ? Mn1 P1 C9 C11 -157.0(4) . . . . ? C12A P1 C9 C10 -65.4(4) . . . . ? C8 P1 C9 C10 -172.8(3) . . . . ? C12 P1 C9 C10 -64.1(5) . . . . ? Mn1 P1 C9 C10 69.4(4) . . . . ? C8 P1 C12 C12A 108.0(11) . . . . ? C9 P1 C12 C12A -3.4(12) . . . . ? Mn1 P1 C12 C12A -132.1(10) . . . . ? C12A P1 C12 C14A -90.3(14) . . . . ? C8 P1 C12 C14A 17.7(10) . . . . ? C9 P1 C12 C14A -93.7(10) . . . . ? Mn1 P1 C12 C14A 137.7(8) . . . . ? C12A P1 C12 C14 -52.2(11) . . . . ? C8 P1 C12 C14 55.9(9) . . . . ? C9 P1 C12 C14 -55.6(9) . . . . ? Mn1 P1 C12 C14 175.8(7) . . . . ? C12A P1 C12 C13 72.9(11) . . . . ? C8 P1 C12 C13 -179.0(5) . . . . ? C9 P1 C12 C13 69.5(6) . . . . ? Mn1 P1 C12 C13 -59.1(6) . . . . ? C14A C12 C12A C14 -9.9(10) . . . . ? C13 C12 C12A C14 118.4(6) . . . . ? P1 C12 C12A C14 -129.8(6) . . . . ? C14A C12 C12A C13 -128.3(9) . . . . ? C14 C12 C12A C13 -118.4(6) . . . . ? P1 C12 C12A C13 111.7(4) . . . . ? C14 C12 C12A C14A 9.9(10) . . . . ? C13 C12 C12A C14A 128.3(9) . . . . ? P1 C12 C12A C14A -120.0(8) . . . . ? C14A C12 C12A P1 120.0(8) . . . . ? C14 C12 C12A P1 129.8(6) . . . . ? C13 C12 C12A P1 -111.7(4) . . . . ? C8 P1 C12A C12 -76.7(11) . . . . ? C9 P1 C12A C12 177.0(10) . . . . ? Mn1 P1 C12A C12 60.3(12) . . . . ? C8 P1 C12A C14 0.0(11) . . . . ? C9 P1 C12A C14 -106.3(10) . . . . ? C12 P1 C12A C14 76.7(13) . . . . ? Mn1 P1 C12A C14 137.0(9) . . . . ? C8 P1 C12A C13 -145.8(5) . . . . ? C9 P1 C12A C13 108.0(5) . . . . ? C12 P1 C12A C13 -69.0(11) . . . . ? Mn1 P1 C12A C13 -8.8(7) . . . . ? C8 P1 C12A C14A -30.0(7) . . . . ? C9 P1 C12A C14A -136.3(6) . . . . ? C12 P1 C12A C14A 46.7(10) . . . . ? Mn1 P1 C12A C14A 107.0(6) . . . . ? C14A C12 C13 C12A 97.1(16) . . . . ? C14 C12 C13 C12A 62.3(11) . . . . ? P1 C12 C13 C12A -64.5(10) . . . . ? C14 C12A C13 C12 -70.6(12) . . . . ? C14A C12A C13 C12 -39.2(10) . . . . ? P1 C12A C13 C12 80.9(11) . . . . ? C12 C12A C14 C14A 15.1(15) . . . . ? C13 C12A C14 C14A 79.8(13) . . . . ? P1 C12A C14 C14A -65.1(15) . . . . ? C13 C12A C14 C12 64.6(10) . . . . ? C14A C12A C14 C12 -15.1(15) . . . . ? P1 C12A C14 C12 -80.3(12) . . . . ? C12A C12 C14 C14A -162.5(17) . . . . ? C13 C12 C14 C14A 127.7(13) . . . . ? P1 C12 C14 C14A -110.3(13) . . . . ? C14A C12 C14 C12A 162.5(17) . . . . ? C13 C12 C14 C12A -69.8(11) . . . . ? P1 C12 C14 C12A 52.2(10) . . . . ? C12A C14 C14A C12 -8.8(9) . . . . ? C12 C14 C14A C12A 8.8(9) . . . . ? C12A C12 C14A C14 16.6(16) . . . . ? C13 C12 C14A C14 -70.7(16) . . . . ? P1 C12 C14A C14 88.4(14) . . . . ? C14 C12 C14A C12A -16.6(16) . . . . ? C13 C12 C14A C12A -87.2(15) . . . . ? P1 C12 C14A C12A 71.8(12) . . . . ? C12 C12A C14A C14 -160.7(19) . . . . ? C13 C12A C14A C14 -110.7(13) . . . . ? P1 C12A C14A C14 130.4(13) . . . . ? C14 C12A C14A C12 160.7(19) . . . . ? C13 C12A C14A C12 50.1(11) . . . . ? P1 C12A C14A C12 -68.8(12) . . . . ? C7 N2 C15 C16 86.7(4) . . . . ? Si1 N2 C15 C16 -114.3(3) . . . . ? N2 C15 C16 P2 54.6(4) . . . . ? C20 P2 C16 C15 -179.5(3) . . . . ? C17 P2 C16 C15 70.8(3) . . . . ? Mn1 P2 C16 C15 -48.8(3) . . . . ? C16 P2 C17 C19 61.8(4) . . . . ? C20 P2 C17 C19 -43.3(4) . . . . ? Mn1 P2 C17 C19 -178.4(3) . . . . ? C16 P2 C17 C18 -170.3(3) . . . . ? C20 P2 C17 C18 84.6(3) . . . . ? Mn1 P2 C17 C18 -50.5(3) . . . . ? C16 P2 C20 C22 68.3(3) . . . . ? C17 P2 C20 C22 174.6(3) . . . . ? Mn1 P2 C20 C22 -55.8(4) . . . . ? C16 P2 C20 C21 -169.8(3) . . . . ? C17 P2 C20 C21 -63.5(3) . . . . ? Mn1 P2 C20 C21 66.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.568 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.080