# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_rw1271zr _database_code_depnum_ccdc_archive 'CCDC 900053' #TrackingRef '13732_web_deposit_cif_file_0_RoryWaterman_1346784222.RW1271Zr.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H54 N5 P Si3 Zr' _chemical_formula_sum 'C26 H54 N5 P Si3 Zr' _chemical_formula_weight 643.20 _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' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall -P2ybc _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 20.8055(11) _cell_length_b 19.6873(10) _cell_length_c 18.6399(10) _cell_angle_alpha 90.00 _cell_angle_beta 115.8380(10) _cell_angle_gamma 90.00 _cell_volume 6871.7(6) _cell_formula_units_Z 8 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9957 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 30.53 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_absorpt_coefficient_mu 0.494 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8660 _exptl_absorpt_correction_T_max 0.8865 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 110878 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 30.57 _reflns_number_total 21007 _reflns_number_gt 16743 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+2.4581P] 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 21007 _refine_ls_number_parameters 673 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0719 _refine_ls_wR_factor_gt 0.0651 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _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 0.220511(7) 0.271889(7) 0.356593(8) 0.01601(3) Uani 1 1 d . . . Zr2 Zr 0.308772(7) 0.718608(7) 0.212562(8) 0.01564(3) Uani 1 1 d . . . P1 P 0.20291(2) 0.281737(19) 0.49692(2) 0.02101(8) Uani 1 1 d . . . P2 P 0.25509(2) 0.753093(19) 0.04969(2) 0.01877(7) Uani 1 1 d . . . N11 N 0.30267(7) 0.20497(7) 0.36378(8) 0.0235(3) Uani 1 1 d . . . N12 N 0.27704(7) 0.36586(6) 0.38690(7) 0.0224(3) Uani 1 1 d . . . N13 N 0.12144(6) 0.29242(6) 0.26030(7) 0.0181(2) Uani 1 1 d . . . N14 N 0.24219(7) 0.29692(7) 0.24026(7) 0.0248(3) Uani 1 1 d . . . N15 N 0.16825(7) 0.18099(6) 0.39639(7) 0.0201(2) Uani 1 1 d . . . N21 N 0.37942(7) 0.63363(6) 0.24087(8) 0.0217(2) Uani 1 1 d . . . N22 N 0.21031(7) 0.67234(6) 0.19068(8) 0.0218(2) Uani 1 1 d . . . N23 N 0.30954(7) 0.80404(6) 0.27902(7) 0.0210(2) Uani 1 1 d . . . N24 N 0.32692(7) 0.67987(7) 0.34552(8) 0.0261(3) Uani 1 1 d . . . N25 N 0.38082(6) 0.77778(6) 0.16484(7) 0.0189(2) Uani 1 1 d . . . Si11 Si 0.36040(2) 0.15738(2) 0.44525(3) 0.02572(9) Uani 1 1 d . . . Si12 Si 0.34351(2) 0.40288(2) 0.47028(2) 0.02021(8) Uani 1 1 d . . . Si13 Si 0.05585(2) 0.34767(2) 0.26000(2) 0.01993(8) Uani 1 1 d . . . Si21 Si 0.40746(2) 0.58724(2) 0.18015(3) 0.02413(9) Uani 1 1 d . . . Si22 Si 0.14518(2) 0.62704(2) 0.11403(3) 0.02343(9) Uani 1 1 d . . . Si23 Si 0.24931(2) 0.87071(2) 0.25790(3) 0.02460(9) Uani 1 1 d . . . C11 C 0.33393(9) 0.21117(11) 0.30607(10) 0.0365(4) Uani 1 1 d . . . H11A H 0.3516 0.1663 0.2986 0.044 Uiso 1 1 calc R . . H11B H 0.3749 0.2429 0.3272 0.044 Uiso 1 1 calc R . . C12 C 0.26542(9) 0.40336(9) 0.31294(10) 0.0301(4) Uani 1 1 d . . . H12A H 0.2941 0.4456 0.3269 0.036 Uiso 1 1 calc R . . H12B H 0.2144 0.4160 0.2837 0.036 Uiso 1 1 calc R . . C13 C 0.11599(8) 0.27088(8) 0.18169(8) 0.0220(3) Uani 1 1 d . . . H13A H 0.0682 0.2820 0.1390 0.026 Uiso 1 1 calc R . . H13B H 0.1235 0.2213 0.1812 0.026 Uiso 1 1 calc R . . C14 C 0.27846(9) 0.23693(10) 0.22709(10) 0.0346(4) Uani 1 1 d . . . H14A H 0.3016 0.2494 0.1924 0.041 Uiso 1 1 calc R . . H14B H 0.2430 0.2008 0.2001 0.041 Uiso 1 1 calc R . . C15 C 0.28699(9) 0.35922(10) 0.26069(10) 0.0343(4) Uani 1 1 d . . . H15A H 0.2796 0.3840 0.2115 0.041 Uiso 1 1 calc R . . H15B H 0.3381 0.3470 0.2894 0.041 Uiso 1 1 calc R . . C16 C 0.17325(8) 0.30892(9) 0.16899(9) 0.0258(3) Uani 1 1 d . . . H16A H 0.1761 0.2923 0.1203 0.031 Uiso 1 1 calc R . . H16B H 0.1622 0.3581 0.1626 0.031 Uiso 1 1 calc R . . C17 C 0.36464(11) 0.06611(10) 0.41870(14) 0.0453(5) Uani 1 1 d . . . H17A H 0.3809 0.0635 0.3767 0.068 Uiso 1 1 calc R . . H17B H 0.3171 0.0457 0.3996 0.068 Uiso 1 1 calc R . . H17C H 0.3981 0.0415 0.4659 0.068 Uiso 1 1 calc R . . C18 C 0.45425(9) 0.18973(11) 0.48096(12) 0.0411(4) Uani 1 1 d . . . H18A H 0.4713 0.1806 0.4405 0.062 Uiso 1 1 calc R . . H18B H 0.4853 0.1667 0.5307 0.062 Uiso 1 1 calc R . . H18C H 0.4551 0.2388 0.4903 0.062 Uiso 1 1 calc R . . C19 C 0.33889(9) 0.15948(8) 0.53224(10) 0.0301(4) Uani 1 1 d . . . H19A H 0.2936 0.1359 0.5186 0.045 Uiso 1 1 calc R . . H19B H 0.3348 0.2068 0.5462 0.045 Uiso 1 1 calc R . . H19C H 0.3770 0.1369 0.5778 0.045 Uiso 1 1 calc R . . C21 C 0.39082(10) 0.59163(8) 0.31138(10) 0.0309(4) Uani 1 1 d . . . H21A H 0.4370 0.5674 0.3300 0.037 Uiso 1 1 calc R . . H21B H 0.3524 0.5573 0.2966 0.037 Uiso 1 1 calc R . . C22 C 0.19821(9) 0.67539(9) 0.26355(10) 0.0290(3) Uani 1 1 d . . . H22A H 0.1535 0.6512 0.2541 0.035 Uiso 1 1 calc R . . H22B H 0.1933 0.7233 0.2765 0.035 Uiso 1 1 calc R . . C23 C 0.36231(9) 0.79770(9) 0.36327(9) 0.0294(3) Uani 1 1 d . . . H23A H 0.3646 0.8404 0.3924 0.035 Uiso 1 1 calc R . . H23B H 0.4103 0.7881 0.3668 0.035 Uiso 1 1 calc R . . C24 C 0.39093(10) 0.63576(9) 0.37722(10) 0.0316(4) Uani 1 1 d . . . H24A H 0.3908 0.6070 0.4207 0.038 Uiso 1 1 calc R . . H24B H 0.4346 0.6641 0.3992 0.038 Uiso 1 1 calc R . . C25 C 0.26071(10) 0.64268(9) 0.33280(10) 0.0325(4) Uani 1 1 d . . . H25A H 0.2531 0.6448 0.3816 0.039 Uiso 1 1 calc R . . H25B H 0.2649 0.5944 0.3207 0.039 Uiso 1 1 calc R . . C26 C 0.33796(10) 0.73973(9) 0.39853(9) 0.0332(4) Uani 1 1 d . . . H26A H 0.3746 0.7295 0.4531 0.040 Uiso 1 1 calc R . . H26B H 0.2929 0.7517 0.4013 0.040 Uiso 1 1 calc R . . C27 C 0.36521(11) 0.50075(9) 0.16173(13) 0.0433(5) Uani 1 1 d . . . H27A H 0.3857 0.4743 0.2112 0.065 Uiso 1 1 calc R . . H27B H 0.3742 0.4774 0.1206 0.065 Uiso 1 1 calc R . . H27C H 0.3136 0.5054 0.1439 0.065 Uiso 1 1 calc R . . C28 C 0.50637(9) 0.57087(9) 0.22776(12) 0.0352(4) Uani 1 1 d . . . H28A H 0.5320 0.6141 0.2360 0.053 Uiso 1 1 calc R . . H28B H 0.5185 0.5417 0.1929 0.053 Uiso 1 1 calc R . . H28C H 0.5202 0.5483 0.2792 0.053 Uiso 1 1 calc R . . C29 C 0.38534(11) 0.62688(9) 0.08138(10) 0.0357(4) Uani 1 1 d . . . H29A H 0.4074 0.6719 0.0893 0.054 Uiso 1 1 calc R . . H29B H 0.3334 0.6313 0.0516 0.054 Uiso 1 1 calc R . . H29C H 0.4036 0.5983 0.0513 0.054 Uiso 1 1 calc R . . C110 C 0.42477(9) 0.42176(9) 0.45385(11) 0.0337(4) Uani 1 1 d . . . H11C H 0.4465 0.3790 0.4485 0.051 Uiso 1 1 calc R . . H11D H 0.4593 0.4474 0.4994 0.051 Uiso 1 1 calc R . . H11E H 0.4108 0.4486 0.4051 0.051 Uiso 1 1 calc R . . C111 C 0.37735(9) 0.34861(8) 0.56149(10) 0.0305(4) Uani 1 1 d . . . H11F H 0.3401 0.3438 0.5800 0.046 Uiso 1 1 calc R . . H11G H 0.4197 0.3698 0.6034 0.046 Uiso 1 1 calc R . . H11H H 0.3900 0.3037 0.5490 0.046 Uiso 1 1 calc R . . C112 C 0.31388(10) 0.48597(8) 0.49498(11) 0.0336(4) Uani 1 1 d . . . H11I H 0.2753 0.4780 0.5107 0.050 Uiso 1 1 calc R . . H11J H 0.2967 0.5157 0.4481 0.050 Uiso 1 1 calc R . . H11K H 0.3542 0.5077 0.5390 0.050 Uiso 1 1 calc R . . C113 C 0.00576(9) 0.38853(9) 0.15996(10) 0.0316(4) Uani 1 1 d . . . H11L H 0.0396 0.4108 0.1439 0.047 Uiso 1 1 calc R . . H11M H -0.0275 0.4223 0.1631 0.047 Uiso 1 1 calc R . . H11N H -0.0210 0.3538 0.1206 0.047 Uiso 1 1 calc R . . C114 C 0.09648(9) 0.41813(8) 0.33325(10) 0.0281(3) Uani 1 1 d . . . H11O H 0.1368 0.4005 0.3807 0.042 Uiso 1 1 calc R . . H11P H 0.0606 0.4370 0.3485 0.042 Uiso 1 1 calc R . . H11Q H 0.1133 0.4538 0.3089 0.042 Uiso 1 1 calc R . . C115 C -0.01252(9) 0.30436(9) 0.28391(11) 0.0300(3) Uani 1 1 d . . . H11R H 0.0115 0.2766 0.3319 0.045 Uiso 1 1 calc R . . H11S H -0.0426 0.2752 0.2392 0.045 Uiso 1 1 calc R . . H11T H -0.0423 0.3386 0.2931 0.045 Uiso 1 1 calc R . . C116 C 0.14813(8) 0.21281(7) 0.44450(9) 0.0220(3) Uani 1 1 d . . . H11U H 0.1070 0.1999 0.4509 0.026 Uiso 1 1 calc R . . C117 C 0.13531(8) 0.11368(7) 0.36225(9) 0.0227(3) Uani 1 1 d . . . C118 C 0.05519(9) 0.11237(10) 0.33860(12) 0.0382(4) Uani 1 1 d . . . H11W H 0.0323 0.1515 0.3044 0.057 Uiso 1 1 calc R . . H11X H 0.0472 0.1145 0.3866 0.057 Uiso 1 1 calc R . . H11Y H 0.0346 0.0703 0.3096 0.057 Uiso 1 1 calc R . . C119 C 0.14719(11) 0.10053(9) 0.28830(11) 0.0382(4) Uani 1 1 d . . . H11Z H 0.1195 0.1333 0.2466 0.057 Uiso 1 1 calc R . . H12C H 0.1317 0.0543 0.2690 0.057 Uiso 1 1 calc R . . H12D H 0.1980 0.1056 0.3018 0.057 Uiso 1 1 calc R . . C120 C 0.17194(11) 0.05885(8) 0.42423(11) 0.0375(4) Uani 1 1 d . . . H12E H 0.1667 0.0693 0.4729 0.056 Uiso 1 1 calc R . . H12F H 0.2228 0.0572 0.4365 0.056 Uiso 1 1 calc R . . H12G H 0.1499 0.0148 0.4033 0.056 Uiso 1 1 calc R . . C121 C 0.14512(8) 0.33953(7) 0.51839(9) 0.0220(3) Uani 1 1 d . . . C122 C 0.07245(9) 0.32928(9) 0.49632(10) 0.0291(3) Uani 1 1 d . . . H12H H 0.0497 0.2898 0.4670 0.035 Uiso 1 1 calc R . . C123 C 0.03287(10) 0.37588(10) 0.51657(11) 0.0347(4) Uani 1 1 d . . . H12I H -0.0165 0.3680 0.5009 0.042 Uiso 1 1 calc R . . C124 C 0.06492(10) 0.43357(9) 0.55941(11) 0.0358(4) Uani 1 1 d . . . H12J H 0.0377 0.4656 0.5728 0.043 Uiso 1 1 calc R . . C125 C 0.13694(10) 0.44426(9) 0.58268(11) 0.0350(4) Uani 1 1 d . . . H12K H 0.1593 0.4839 0.6121 0.042 Uiso 1 1 calc R . . C126 C 0.17686(9) 0.39752(8) 0.56343(10) 0.0286(3) Uani 1 1 d . . . H12L H 0.2266 0.4050 0.5811 0.034 Uiso 1 1 calc R . . C210 C 0.06187(9) 0.67919(9) 0.06460(10) 0.0309(4) Uani 1 1 d . . . H21C H 0.0714 0.7185 0.0385 0.046 Uiso 1 1 calc R . . H21D H 0.0467 0.6948 0.1047 0.046 Uiso 1 1 calc R . . H21E H 0.0240 0.6515 0.0248 0.046 Uiso 1 1 calc R . . C211 C 0.12156(11) 0.54732(10) 0.15277(14) 0.0462(5) Uani 1 1 d . . . H21F H 0.1028 0.5593 0.1911 0.069 Uiso 1 1 calc R . . H21G H 0.1643 0.5191 0.1791 0.069 Uiso 1 1 calc R . . H21H H 0.0852 0.5220 0.1083 0.069 Uiso 1 1 calc R . . C212 C 0.17283(9) 0.59666(9) 0.03673(11) 0.0320(4) Uani 1 1 d . . . H21I H 0.1749 0.6353 0.0046 0.048 Uiso 1 1 calc R . . H21J H 0.1380 0.5634 0.0022 0.048 Uiso 1 1 calc R . . H21K H 0.2200 0.5753 0.0628 0.048 Uiso 1 1 calc R . . C213 C 0.16570(8) 0.85123(8) 0.16739(9) 0.0261(3) Uani 1 1 d . . . H21L H 0.1768 0.8441 0.1220 0.039 Uiso 1 1 calc R . . H21M H 0.1323 0.8893 0.1559 0.039 Uiso 1 1 calc R . . H21N H 0.1439 0.8101 0.1766 0.039 Uiso 1 1 calc R . . C214 C 0.28832(10) 0.95180(9) 0.24155(12) 0.0380(4) Uani 1 1 d . . . H21O H 0.2928 0.9489 0.1914 0.057 Uiso 1 1 calc R . . H21P H 0.3356 0.9590 0.2858 0.057 Uiso 1 1 calc R . . H21Q H 0.2570 0.9898 0.2389 0.057 Uiso 1 1 calc R . . C215 C 0.22424(11) 0.88574(11) 0.34180(11) 0.0437(5) Uani 1 1 d . . . H21R H 0.2036 0.8442 0.3519 0.066 Uiso 1 1 calc R . . H21S H 0.1891 0.9225 0.3274 0.066 Uiso 1 1 calc R . . H21T H 0.2669 0.8984 0.3899 0.066 Uiso 1 1 calc R . . C216 C 0.33135(8) 0.80384(7) 0.10001(9) 0.0206(3) Uani 1 1 d . . . H21U H 0.3362 0.8475 0.0811 0.025 Uiso 1 1 calc R . . C217 C 0.45215(8) 0.81190(8) 0.20320(10) 0.0237(3) Uani 1 1 d . . . C218 C 0.50324(9) 0.76508(9) 0.26800(11) 0.0335(4) Uani 1 1 d . . . H21W H 0.5072 0.7218 0.2442 0.050 Uiso 1 1 calc R . . H21X H 0.4850 0.7568 0.3077 0.050 Uiso 1 1 calc R . . H21Y H 0.5504 0.7865 0.2939 0.050 Uiso 1 1 calc R . . C219 C 0.44597(9) 0.87975(9) 0.23978(12) 0.0365(4) Uani 1 1 d . . . H21Z H 0.4141 0.9101 0.1976 0.055 Uiso 1 1 calc R . . H22C H 0.4933 0.9006 0.2667 0.055 Uiso 1 1 calc R . . H22D H 0.4265 0.8720 0.2784 0.055 Uiso 1 1 calc R . . C220 C 0.48114(9) 0.82399(11) 0.14173(11) 0.0389(4) Uani 1 1 d . . . H22E H 0.4837 0.7807 0.1172 0.058 Uiso 1 1 calc R . . H22F H 0.5290 0.8439 0.1681 0.058 Uiso 1 1 calc R . . H22G H 0.4494 0.8551 0.1005 0.058 Uiso 1 1 calc R . . C221 C 0.18563(8) 0.81258(7) -0.01091(8) 0.0191(3) Uani 1 1 d . . . C222 C 0.19088(8) 0.88341(8) -0.00422(9) 0.0235(3) Uani 1 1 d . . . H22H H 0.2315 0.9033 0.0377 0.028 Uiso 1 1 calc R . . C223 C 0.13799(9) 0.92513(8) -0.05753(10) 0.0275(3) Uani 1 1 d . . . H22I H 0.1435 0.9731 -0.0530 0.033 Uiso 1 1 calc R . . C224 C 0.07718(9) 0.89724(9) -0.11729(10) 0.0295(3) Uani 1 1 d . . . H22J H 0.0408 0.9259 -0.1536 0.035 Uiso 1 1 calc R . . C225 C 0.06969(9) 0.82740(9) -0.12375(10) 0.0303(3) Uani 1 1 d . . . H22K H 0.0274 0.8080 -0.1637 0.036 Uiso 1 1 calc R . . C226 C 0.12368(8) 0.78546(8) -0.07212(9) 0.0251(3) Uani 1 1 d . . . H22L H 0.1186 0.7376 -0.0784 0.030 Uiso 1 1 calc R . . _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 0.01633(6) 0.01828(6) 0.01293(6) 0.00042(5) 0.00592(5) -0.00172(5) Zr2 0.01810(6) 0.01556(6) 0.01496(6) 0.00053(5) 0.00877(5) 0.00073(5) P1 0.02721(19) 0.02116(18) 0.01657(17) -0.00148(14) 0.01132(15) -0.00328(15) P2 0.02091(18) 0.01954(17) 0.01610(17) 0.00077(13) 0.00829(14) -0.00126(14) N11 0.0202(6) 0.0299(7) 0.0200(6) -0.0003(5) 0.0084(5) 0.0025(5) N12 0.0224(6) 0.0240(6) 0.0175(6) 0.0027(5) 0.0058(5) -0.0055(5) N13 0.0186(6) 0.0202(6) 0.0149(5) -0.0013(4) 0.0068(5) -0.0014(5) N14 0.0214(6) 0.0370(7) 0.0170(6) 0.0019(5) 0.0092(5) -0.0021(5) N15 0.0250(6) 0.0168(6) 0.0180(6) 0.0013(4) 0.0088(5) -0.0017(5) N21 0.0265(6) 0.0182(6) 0.0240(6) 0.0036(5) 0.0144(5) 0.0037(5) N22 0.0221(6) 0.0234(6) 0.0235(6) 0.0018(5) 0.0133(5) -0.0008(5) N23 0.0215(6) 0.0224(6) 0.0174(6) -0.0026(5) 0.0069(5) 0.0023(5) N24 0.0305(7) 0.0312(7) 0.0202(6) 0.0061(5) 0.0142(6) 0.0083(6) N25 0.0190(6) 0.0186(6) 0.0207(6) -0.0013(5) 0.0100(5) -0.0016(5) Si11 0.0218(2) 0.0218(2) 0.0272(2) -0.00094(17) 0.00481(18) 0.00269(16) Si12 0.01899(19) 0.01779(18) 0.0213(2) -0.00202(15) 0.00636(16) -0.00198(15) Si13 0.01920(19) 0.01917(19) 0.01917(19) -0.00075(15) 0.00628(16) 0.00016(15) Si21 0.0275(2) 0.01847(19) 0.0282(2) -0.00212(16) 0.01375(18) 0.00367(16) Si22 0.0203(2) 0.01933(19) 0.0306(2) 0.00260(16) 0.01113(18) -0.00195(16) Si23 0.0267(2) 0.0245(2) 0.0222(2) -0.00389(16) 0.01024(18) 0.00533(17) C11 0.0243(8) 0.0593(12) 0.0292(9) 0.0043(8) 0.0147(7) 0.0101(8) C12 0.0313(9) 0.0309(8) 0.0231(8) 0.0061(6) 0.0072(7) -0.0114(7) C13 0.0219(7) 0.0263(7) 0.0154(6) -0.0024(5) 0.0059(6) -0.0005(6) C14 0.0285(9) 0.0560(12) 0.0244(8) 0.0019(8) 0.0164(7) 0.0090(8) C15 0.0285(8) 0.0512(11) 0.0246(8) 0.0042(7) 0.0128(7) -0.0151(8) C16 0.0270(8) 0.0355(9) 0.0145(7) 0.0009(6) 0.0086(6) -0.0017(6) C17 0.0477(12) 0.0284(9) 0.0578(13) -0.0065(9) 0.0211(10) 0.0072(8) C18 0.0224(8) 0.0478(11) 0.0418(11) 0.0004(9) 0.0035(8) 0.0008(8) C19 0.0341(9) 0.0232(8) 0.0244(8) 0.0050(6) 0.0048(7) 0.0017(7) C21 0.0378(9) 0.0268(8) 0.0338(9) 0.0129(7) 0.0210(8) 0.0113(7) C22 0.0285(8) 0.0362(9) 0.0304(8) 0.0054(7) 0.0204(7) 0.0009(7) C23 0.0295(8) 0.0341(9) 0.0198(7) -0.0064(6) 0.0062(6) 0.0054(7) C24 0.0348(9) 0.0367(9) 0.0248(8) 0.0139(7) 0.0145(7) 0.0146(7) C25 0.0389(10) 0.0381(9) 0.0305(9) 0.0116(7) 0.0245(8) 0.0055(7) C26 0.0380(10) 0.0452(10) 0.0154(7) 0.0020(7) 0.0109(7) 0.0127(8) C27 0.0445(11) 0.0222(8) 0.0592(13) -0.0096(8) 0.0191(10) -0.0008(8) C28 0.0328(9) 0.0309(9) 0.0449(10) -0.0036(8) 0.0196(8) 0.0083(7) C29 0.0476(11) 0.0346(9) 0.0300(9) -0.0011(7) 0.0216(8) 0.0129(8) C110 0.0235(8) 0.0394(10) 0.0368(10) -0.0048(8) 0.0118(7) -0.0068(7) C111 0.0290(8) 0.0274(8) 0.0231(8) 0.0008(6) 0.0002(7) -0.0035(7) C112 0.0404(10) 0.0231(8) 0.0397(10) -0.0018(7) 0.0198(8) 0.0029(7) C113 0.0302(9) 0.0292(8) 0.0266(8) 0.0029(7) 0.0042(7) 0.0040(7) C114 0.0322(9) 0.0220(7) 0.0276(8) -0.0041(6) 0.0107(7) -0.0005(6) C115 0.0264(8) 0.0330(9) 0.0353(9) -0.0064(7) 0.0178(7) -0.0024(7) C116 0.0283(8) 0.0203(7) 0.0195(7) 0.0019(5) 0.0124(6) -0.0028(6) C117 0.0281(8) 0.0157(6) 0.0237(7) -0.0020(5) 0.0109(6) -0.0034(6) C118 0.0294(9) 0.0349(9) 0.0465(11) -0.0153(8) 0.0129(8) -0.0076(7) C119 0.0575(12) 0.0286(9) 0.0370(10) -0.0140(7) 0.0286(9) -0.0150(8) C120 0.0472(11) 0.0192(8) 0.0361(10) 0.0030(7) 0.0087(8) -0.0044(7) C121 0.0302(8) 0.0218(7) 0.0167(7) 0.0007(5) 0.0128(6) -0.0018(6) C122 0.0319(9) 0.0315(8) 0.0243(8) -0.0055(6) 0.0126(7) -0.0040(7) C123 0.0310(9) 0.0447(10) 0.0301(9) -0.0022(8) 0.0151(7) 0.0029(8) C124 0.0451(11) 0.0349(9) 0.0318(9) -0.0004(7) 0.0208(8) 0.0093(8) C125 0.0477(11) 0.0254(8) 0.0359(9) -0.0073(7) 0.0220(9) -0.0024(7) C126 0.0337(9) 0.0267(8) 0.0277(8) -0.0043(6) 0.0156(7) -0.0050(7) C210 0.0240(8) 0.0380(9) 0.0314(9) 0.0019(7) 0.0126(7) 0.0035(7) C211 0.0436(11) 0.0317(10) 0.0584(13) 0.0129(9) 0.0177(10) -0.0105(8) C212 0.0278(8) 0.0249(8) 0.0405(10) -0.0105(7) 0.0123(7) -0.0023(6) C213 0.0227(7) 0.0315(8) 0.0263(8) 0.0012(6) 0.0127(6) 0.0039(6) C214 0.0339(9) 0.0237(8) 0.0487(11) -0.0049(8) 0.0109(9) 0.0027(7) C215 0.0523(12) 0.0502(12) 0.0321(10) -0.0043(8) 0.0217(9) 0.0213(10) C216 0.0225(7) 0.0199(7) 0.0227(7) 0.0023(5) 0.0129(6) -0.0002(5) C217 0.0178(7) 0.0232(7) 0.0287(8) -0.0002(6) 0.0089(6) -0.0033(6) C218 0.0237(8) 0.0316(9) 0.0352(9) 0.0018(7) 0.0036(7) -0.0006(7) C219 0.0280(9) 0.0246(8) 0.0526(11) -0.0100(8) 0.0136(8) -0.0071(7) C220 0.0241(8) 0.0560(12) 0.0400(10) 0.0032(9) 0.0170(8) -0.0070(8) C221 0.0216(7) 0.0217(7) 0.0157(6) 0.0015(5) 0.0098(6) -0.0016(5) C222 0.0255(8) 0.0223(7) 0.0203(7) 0.0006(6) 0.0077(6) -0.0029(6) C223 0.0333(9) 0.0215(7) 0.0280(8) 0.0030(6) 0.0135(7) 0.0010(6) C224 0.0280(8) 0.0307(8) 0.0259(8) 0.0058(6) 0.0082(7) 0.0057(7) C225 0.0252(8) 0.0315(8) 0.0263(8) -0.0001(7) 0.0039(7) -0.0014(7) C226 0.0259(8) 0.0214(7) 0.0253(8) -0.0002(6) 0.0086(6) -0.0026(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; _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 N13 2.0997(12) . ? Zr1 N11 2.1156(13) . ? Zr1 N12 2.1320(12) . ? Zr1 N15 2.3745(12) . ? Zr1 N14 2.4498(12) . ? Zr1 P1 2.8014(4) . ? Zr2 N23 2.0848(12) . ? Zr2 N22 2.1128(12) . ? Zr2 N21 2.1358(12) . ? Zr2 N25 2.3575(12) . ? Zr2 N24 2.4598(13) . ? Zr2 P2 2.8230(4) . ? P1 C116 1.7677(15) . ? P1 C121 1.8221(16) . ? P2 C216 1.7601(15) . ? P2 C221 1.8202(15) . ? N11 C11 1.485(2) . ? N11 Si11 1.7426(14) . ? N12 C12 1.4880(19) . ? N12 Si12 1.7279(13) . ? N13 C13 1.4816(18) . ? N13 Si13 1.7432(13) . ? N14 C14 1.478(2) . ? N14 C15 1.486(2) . ? N14 C16 1.489(2) . ? N15 C116 1.3035(19) . ? N15 C117 1.5002(18) . ? N21 C21 1.4818(19) . ? N21 Si21 1.7411(13) . ? N22 C22 1.4867(19) . ? N22 Si22 1.7279(14) . ? N23 C23 1.4779(19) . ? N23 Si23 1.7372(13) . ? N24 C24 1.480(2) . ? N24 C25 1.485(2) . ? N24 C26 1.490(2) . ? N25 C216 1.3034(19) . ? N25 C217 1.4965(19) . ? Si11 C19 1.8610(18) . ? Si11 C17 1.8760(19) . ? Si11 C18 1.8784(18) . ? Si12 C111 1.8667(16) . ? Si12 C112 1.8748(17) . ? Si12 C110 1.8820(17) . ? Si13 C114 1.8699(16) . ? Si13 C115 1.8712(17) . ? Si13 C113 1.8753(17) . ? Si21 C29 1.8632(18) . ? Si21 C27 1.8779(18) . ? Si21 C28 1.8799(18) . ? Si22 C212 1.8674(18) . ? Si22 C210 1.8750(17) . ? Si22 C211 1.8802(18) . ? Si23 C213 1.8604(16) . ? Si23 C214 1.8749(19) . ? Si23 C215 1.8753(18) . ? C11 C14 1.509(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C15 1.512(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C16 1.511(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 C24 1.503(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C25 1.519(2) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C26 1.511(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C110 H11C 0.9800 . ? C110 H11D 0.9800 . ? C110 H11E 0.9800 . ? C111 H11F 0.9800 . ? C111 H11G 0.9800 . ? C111 H11H 0.9800 . ? C112 H11I 0.9800 . ? C112 H11J 0.9800 . ? C112 H11K 0.9800 . ? C113 H11L 0.9800 . ? C113 H11M 0.9800 . ? C113 H11N 0.9800 . ? C114 H11O 0.9800 . ? C114 H11P 0.9800 . ? C114 H11Q 0.9800 . ? C115 H11R 0.9800 . ? C115 H11S 0.9800 . ? C115 H11T 0.9800 . ? C116 H11U 0.9500 . ? C117 C120 1.521(2) . ? C117 C119 1.525(2) . ? C117 C118 1.528(2) . ? C118 H11W 0.9800 . ? C118 H11X 0.9800 . ? C118 H11Y 0.9800 . ? C119 H11Z 0.9800 . ? C119 H12C 0.9800 . ? C119 H12D 0.9800 . ? C120 H12E 0.9800 . ? C120 H12F 0.9800 . ? C120 H12G 0.9800 . ? C121 C122 1.398(2) . ? C121 C126 1.400(2) . ? C122 C123 1.390(2) . ? C122 H12H 0.9500 . ? C123 C124 1.381(3) . ? C123 H12I 0.9500 . ? C124 C125 1.382(3) . ? C124 H12J 0.9500 . ? C125 C126 1.387(2) . ? C125 H12K 0.9500 . ? C126 H12L 0.9500 . ? C210 H21C 0.9800 . ? C210 H21D 0.9800 . ? C210 H21E 0.9800 . ? C211 H21F 0.9800 . ? C211 H21G 0.9800 . ? C211 H21H 0.9800 . ? C212 H21I 0.9800 . ? C212 H21J 0.9800 . ? C212 H21K 0.9800 . ? C213 H21L 0.9800 . ? C213 H21M 0.9800 . ? C213 H21N 0.9800 . ? C214 H21O 0.9800 . ? C214 H21P 0.9800 . ? C214 H21Q 0.9800 . ? C215 H21R 0.9800 . ? C215 H21S 0.9800 . ? C215 H21T 0.9800 . ? C216 H21U 0.9500 . ? C217 C218 1.523(2) . ? C217 C220 1.528(2) . ? C217 C219 1.531(2) . ? C218 H21W 0.9800 . ? C218 H21X 0.9800 . ? C218 H21Y 0.9800 . ? C219 H21Z 0.9800 . ? C219 H22C 0.9800 . ? C219 H22D 0.9800 . ? C220 H22E 0.9800 . ? C220 H22F 0.9800 . ? C220 H22G 0.9800 . ? C221 C222 1.400(2) . ? C221 C226 1.402(2) . ? C222 C223 1.386(2) . ? C222 H22H 0.9500 . ? C223 C224 1.384(2) . ? C223 H22I 0.9500 . ? C224 C225 1.383(2) . ? C224 H22J 0.9500 . ? C225 C226 1.388(2) . ? C225 H22K 0.9500 . ? C226 H22L 0.9500 . ? _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 N13 Zr1 N11 129.73(5) . . ? N13 Zr1 N12 106.38(5) . . ? N11 Zr1 N12 100.75(5) . . ? N13 Zr1 N15 89.97(4) . . ? N11 Zr1 N15 88.75(5) . . ? N12 Zr1 N15 147.78(4) . . ? N13 Zr1 N14 72.27(4) . . ? N11 Zr1 N14 74.09(5) . . ? N12 Zr1 N14 76.52(5) . . ? N15 Zr1 N14 135.58(4) . . ? N13 Zr1 P1 107.80(3) . . ? N11 Zr1 P1 114.50(4) . . ? N12 Zr1 P1 88.51(4) . . ? N15 Zr1 P1 59.77(3) . . ? N14 Zr1 P1 164.15(3) . . ? N23 Zr2 N22 102.60(5) . . ? N23 Zr2 N21 131.22(5) . . ? N22 Zr2 N21 102.41(5) . . ? N23 Zr2 N25 89.09(5) . . ? N22 Zr2 N25 149.61(5) . . ? N21 Zr2 N25 89.89(4) . . ? N23 Zr2 N24 72.15(5) . . ? N22 Zr2 N24 76.76(5) . . ? N21 Zr2 N24 73.82(4) . . ? N25 Zr2 N24 133.61(5) . . ? N23 Zr2 P2 109.99(4) . . ? N22 Zr2 P2 90.01(4) . . ? N21 Zr2 P2 111.17(3) . . ? N25 Zr2 P2 59.60(3) . . ? N24 Zr2 P2 166.69(3) . . ? C116 P1 C121 105.81(7) . . ? C116 P1 Zr1 75.29(5) . . ? C121 P1 Zr1 127.99(5) . . ? C216 P2 C221 104.66(7) . . ? C216 P2 Zr2 73.81(5) . . ? C221 P2 Zr2 131.08(5) . . ? C11 N11 Si11 108.80(10) . . ? C11 N11 Zr1 119.99(10) . . ? Si11 N11 Zr1 128.39(7) . . ? C12 N12 Si12 111.54(10) . . ? C12 N12 Zr1 109.69(9) . . ? Si12 N12 Zr1 137.49(7) . . ? C13 N13 Si13 116.94(9) . . ? C13 N13 Zr1 114.44(9) . . ? Si13 N13 Zr1 126.75(6) . . ? C14 N14 C15 113.16(14) . . ? C14 N14 C16 109.97(13) . . ? C15 N14 C16 110.51(13) . . ? C14 N14 Zr1 106.89(10) . . ? C15 N14 Zr1 106.02(9) . . ? C16 N14 Zr1 110.13(9) . . ? C116 N15 C117 119.48(12) . . ? C116 N15 Zr1 100.42(9) . . ? C117 N15 Zr1 136.04(9) . . ? C21 N21 Si21 108.33(10) . . ? C21 N21 Zr2 118.89(9) . . ? Si21 N21 Zr2 129.78(7) . . ? C22 N22 Si22 113.09(10) . . ? C22 N22 Zr2 110.02(10) . . ? Si22 N22 Zr2 136.65(7) . . ? C23 N23 Si23 115.66(10) . . ? C23 N23 Zr2 111.90(9) . . ? Si23 N23 Zr2 131.07(7) . . ? C24 N24 C25 112.65(13) . . ? C24 N24 C26 110.34(13) . . ? C25 N24 C26 111.09(13) . . ? C24 N24 Zr2 107.49(9) . . ? C25 N24 Zr2 105.52(9) . . ? C26 N24 Zr2 109.55(9) . . ? C216 N25 C217 118.96(12) . . ? C216 N25 Zr2 99.75(9) . . ? C217 N25 Zr2 134.64(9) . . ? N11 Si11 C19 114.28(7) . . ? N11 Si11 C17 112.26(8) . . ? C19 Si11 C17 107.94(9) . . ? N11 Si11 C18 109.98(8) . . ? C19 Si11 C18 106.93(9) . . ? C17 Si11 C18 104.90(10) . . ? N12 Si12 C111 114.46(7) . . ? N12 Si12 C112 111.65(8) . . ? C111 Si12 C112 108.04(8) . . ? N12 Si12 C110 111.13(7) . . ? C111 Si12 C110 104.61(8) . . ? C112 Si12 C110 106.41(8) . . ? N13 Si13 C114 110.87(7) . . ? N13 Si13 C115 112.96(7) . . ? C114 Si13 C115 108.24(8) . . ? N13 Si13 C113 111.46(7) . . ? C114 Si13 C113 106.64(8) . . ? C115 Si13 C113 106.36(8) . . ? N21 Si21 C29 114.46(7) . . ? N21 Si21 C27 109.37(8) . . ? C29 Si21 C27 107.74(10) . . ? N21 Si21 C28 113.02(7) . . ? C29 Si21 C28 106.65(9) . . ? C27 Si21 C28 105.06(9) . . ? N22 Si22 C212 114.14(7) . . ? N22 Si22 C210 110.34(7) . . ? C212 Si22 C210 109.02(8) . . ? N22 Si22 C211 110.81(8) . . ? C212 Si22 C211 104.42(9) . . ? C210 Si22 C211 107.79(9) . . ? N23 Si23 C213 110.29(7) . . ? N23 Si23 C214 111.08(8) . . ? C213 Si23 C214 109.15(8) . . ? N23 Si23 C215 111.44(8) . . ? C213 Si23 C215 107.38(9) . . ? C214 Si23 C215 107.38(10) . . ? N11 C11 C14 110.14(13) . . ? N11 C11 H11A 109.6 . . ? C14 C11 H11A 109.6 . . ? N11 C11 H11B 109.6 . . ? C14 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? N12 C12 C15 109.74(14) . . ? N12 C12 H12A 109.7 . . ? C15 C12 H12A 109.7 . . ? N12 C12 H12B 109.7 . . ? C15 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? N13 C13 C16 106.71(12) . . ? N13 C13 H13A 110.4 . . ? C16 C13 H13A 110.4 . . ? N13 C13 H13B 110.4 . . ? C16 C13 H13B 110.4 . . ? H13A C13 H13B 108.6 . . ? N14 C14 C11 109.59(14) . . ? N14 C14 H14A 109.8 . . ? C11 C14 H14A 109.8 . . ? N14 C14 H14B 109.8 . . ? C11 C14 H14B 109.8 . . ? H14A C14 H14B 108.2 . . ? N14 C15 C12 108.08(13) . . ? N14 C15 H15A 110.1 . . ? C12 C15 H15A 110.1 . . ? N14 C15 H15B 110.1 . . ? C12 C15 H15B 110.1 . . ? H15A C15 H15B 108.4 . . ? N14 C16 C13 107.48(12) . . ? N14 C16 H16A 110.2 . . ? C13 C16 H16A 110.2 . . ? N14 C16 H16B 110.2 . . ? C13 C16 H16B 110.2 . . ? H16A C16 H16B 108.5 . . ? Si11 C17 H17A 109.5 . . ? Si11 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si11 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si11 C18 H18A 109.5 . . ? Si11 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si11 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si11 C19 H19A 109.5 . . ? Si11 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si11 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N21 C21 C24 110.15(13) . . ? N21 C21 H21A 109.6 . . ? C24 C21 H21A 109.6 . . ? N21 C21 H21B 109.6 . . ? C24 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? N22 C22 C25 109.63(13) . . ? N22 C22 H22A 109.7 . . ? C25 C22 H22A 109.7 . . ? N22 C22 H22B 109.7 . . ? C25 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? N23 C23 C26 106.95(14) . . ? N23 C23 H23A 110.3 . . ? C26 C23 H23A 110.3 . . ? N23 C23 H23B 110.3 . . ? C26 C23 H23B 110.3 . . ? H23A C23 H23B 108.6 . . ? N24 C24 C21 109.41(14) . . ? N24 C24 H24A 109.8 . . ? C21 C24 H24A 109.8 . . ? N24 C24 H24B 109.8 . . ? C21 C24 H24B 109.8 . . ? H24A C24 H24B 108.2 . . ? N24 C25 C22 108.53(13) . . ? N24 C25 H25A 110.0 . . ? C22 C25 H25A 110.0 . . ? N24 C25 H25B 110.0 . . ? C22 C25 H25B 110.0 . . ? H25A C25 H25B 108.4 . . ? N24 C26 C23 107.03(13) . . ? N24 C26 H26A 110.3 . . ? C23 C26 H26A 110.3 . . ? N24 C26 H26B 110.3 . . ? C23 C26 H26B 110.3 . . ? H26A C26 H26B 108.6 . . ? Si21 C27 H27A 109.5 . . ? Si21 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si21 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si21 C28 H28A 109.5 . . ? Si21 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si21 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si21 C29 H29A 109.5 . . ? Si21 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si21 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si12 C110 H11C 109.5 . . ? Si12 C110 H11D 109.5 . . ? H11C C110 H11D 109.5 . . ? Si12 C110 H11E 109.5 . . ? H11C C110 H11E 109.5 . . ? H11D C110 H11E 109.5 . . ? Si12 C111 H11F 109.5 . . ? Si12 C111 H11G 109.5 . . ? H11F C111 H11G 109.5 . . ? Si12 C111 H11H 109.5 . . ? H11F C111 H11H 109.5 . . ? H11G C111 H11H 109.5 . . ? Si12 C112 H11I 109.5 . . ? Si12 C112 H11J 109.5 . . ? H11I C112 H11J 109.5 . . ? Si12 C112 H11K 109.5 . . ? H11I C112 H11K 109.5 . . ? H11J C112 H11K 109.5 . . ? Si13 C113 H11L 109.5 . . ? Si13 C113 H11M 109.5 . . ? H11L C113 H11M 109.5 . . ? Si13 C113 H11N 109.5 . . ? H11L C113 H11N 109.5 . . ? H11M C113 H11N 109.5 . . ? Si13 C114 H11O 109.5 . . ? Si13 C114 H11P 109.5 . . ? H11O C114 H11P 109.5 . . ? Si13 C114 H11Q 109.5 . . ? H11O C114 H11Q 109.5 . . ? H11P C114 H11Q 109.5 . . ? Si13 C115 H11R 109.5 . . ? Si13 C115 H11S 109.5 . . ? H11R C115 H11S 109.5 . . ? Si13 C115 H11T 109.5 . . ? H11R C115 H11T 109.5 . . ? H11S C115 H11T 109.5 . . ? N15 C116 P1 115.22(11) . . ? N15 C116 H11U 122.4 . . ? P1 C116 H11U 122.4 . . ? N15 C117 C120 108.64(12) . . ? N15 C117 C119 108.03(12) . . ? C120 C117 C119 109.95(14) . . ? N15 C117 C118 112.13(13) . . ? C120 C117 C118 109.25(15) . . ? C119 C117 C118 108.82(14) . . ? C117 C118 H11W 109.5 . . ? C117 C118 H11X 109.5 . . ? H11W C118 H11X 109.5 . . ? C117 C118 H11Y 109.5 . . ? H11W C118 H11Y 109.5 . . ? H11X C118 H11Y 109.5 . . ? C117 C119 H11Z 109.5 . . ? C117 C119 H12C 109.5 . . ? H11Z C119 H12C 109.5 . . ? C117 C119 H12D 109.5 . . ? H11Z C119 H12D 109.5 . . ? H12C C119 H12D 109.5 . . ? C117 C120 H12E 109.5 . . ? C117 C120 H12F 109.5 . . ? H12E C120 H12F 109.5 . . ? C117 C120 H12G 109.5 . . ? H12E C120 H12G 109.5 . . ? H12F C120 H12G 109.5 . . ? C122 C121 C126 117.46(15) . . ? C122 C121 P1 125.30(12) . . ? C126 C121 P1 117.19(12) . . ? C123 C122 C121 121.17(16) . . ? C123 C122 H12H 119.4 . . ? C121 C122 H12H 119.4 . . ? C124 C123 C122 120.37(17) . . ? C124 C123 H12I 119.8 . . ? C122 C123 H12I 119.8 . . ? C123 C124 C125 119.39(16) . . ? C123 C124 H12J 120.3 . . ? C125 C124 H12J 120.3 . . ? C124 C125 C126 120.47(16) . . ? C124 C125 H12K 119.8 . . ? C126 C125 H12K 119.8 . . ? C125 C126 C121 121.11(16) . . ? C125 C126 H12L 119.4 . . ? C121 C126 H12L 119.4 . . ? Si22 C210 H21C 109.5 . . ? Si22 C210 H21D 109.5 . . ? H21C C210 H21D 109.5 . . ? Si22 C210 H21E 109.5 . . ? H21C C210 H21E 109.5 . . ? H21D C210 H21E 109.5 . . ? Si22 C211 H21F 109.5 . . ? Si22 C211 H21G 109.5 . . ? H21F C211 H21G 109.5 . . ? Si22 C211 H21H 109.5 . . ? H21F C211 H21H 109.5 . . ? H21G C211 H21H 109.5 . . ? Si22 C212 H21I 109.5 . . ? Si22 C212 H21J 109.5 . . ? H21I C212 H21J 109.5 . . ? Si22 C212 H21K 109.5 . . ? H21I C212 H21K 109.5 . . ? H21J C212 H21K 109.5 . . ? Si23 C213 H21L 109.5 . . ? Si23 C213 H21M 109.5 . . ? H21L C213 H21M 109.5 . . ? Si23 C213 H21N 109.5 . . ? H21L C213 H21N 109.5 . . ? H21M C213 H21N 109.5 . . ? Si23 C214 H21O 109.5 . . ? Si23 C214 H21P 109.5 . . ? H21O C214 H21P 109.5 . . ? Si23 C214 H21Q 109.5 . . ? H21O C214 H21Q 109.5 . . ? H21P C214 H21Q 109.5 . . ? Si23 C215 H21R 109.5 . . ? Si23 C215 H21S 109.5 . . ? H21R C215 H21S 109.5 . . ? Si23 C215 H21T 109.5 . . ? H21R C215 H21T 109.5 . . ? H21S C215 H21T 109.5 . . ? N25 C216 P2 115.78(11) . . ? N25 C216 H21U 122.1 . . ? P2 C216 H21U 122.1 . . ? N25 C217 C218 108.13(12) . . ? N25 C217 C220 110.18(13) . . ? C218 C217 C220 108.78(14) . . ? N25 C217 C219 110.26(12) . . ? C218 C217 C219 109.88(14) . . ? C220 C217 C219 109.59(14) . . ? C217 C218 H21W 109.5 . . ? C217 C218 H21X 109.5 . . ? H21W C218 H21X 109.5 . . ? C217 C218 H21Y 109.5 . . ? H21W C218 H21Y 109.5 . . ? H21X C218 H21Y 109.5 . . ? C217 C219 H21Z 109.5 . . ? C217 C219 H22C 109.5 . . ? H21Z C219 H22C 109.5 . . ? C217 C219 H22D 109.5 . . ? H21Z C219 H22D 109.5 . . ? H22C C219 H22D 109.5 . . ? C217 C220 H22E 109.5 . . ? C217 C220 H22F 109.5 . . ? H22E C220 H22F 109.5 . . ? C217 C220 H22G 109.5 . . ? H22E C220 H22G 109.5 . . ? H22F C220 H22G 109.5 . . ? C222 C221 C226 117.40(14) . . ? C222 C221 P2 125.13(11) . . ? C226 C221 P2 117.36(11) . . ? C223 C222 C221 121.32(14) . . ? C223 C222 H22H 119.3 . . ? C221 C222 H22H 119.3 . . ? C224 C223 C222 120.25(15) . . ? C224 C223 H22I 119.9 . . ? C222 C223 H22I 119.9 . . ? C225 C224 C223 119.56(15) . . ? C225 C224 H22J 120.2 . . ? C223 C224 H22J 120.2 . . ? C224 C225 C226 120.30(15) . . ? C224 C225 H22K 119.9 . . ? C226 C225 H22K 119.9 . . ? C225 C226 C221 121.11(14) . . ? C225 C226 H22L 119.4 . . ? C221 C226 H22L 119.4 . . ? _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 N13 Zr1 P1 C116 64.03(6) . . . . ? N11 Zr1 P1 C116 -88.10(7) . . . . ? N12 Zr1 P1 C116 170.76(6) . . . . ? N15 Zr1 P1 C116 -15.16(6) . . . . ? N14 Zr1 P1 C116 151.73(13) . . . . ? N13 Zr1 P1 C121 -34.74(7) . . . . ? N11 Zr1 P1 C121 173.13(7) . . . . ? N12 Zr1 P1 C121 72.00(7) . . . . ? N15 Zr1 P1 C121 -113.92(7) . . . . ? N14 Zr1 P1 C121 52.97(14) . . . . ? N23 Zr2 P2 C216 60.03(6) . . . . ? N22 Zr2 P2 C216 163.46(6) . . . . ? N21 Zr2 P2 C216 -93.21(6) . . . . ? N25 Zr2 P2 C216 -16.49(6) . . . . ? N24 Zr2 P2 C216 156.97(15) . . . . ? N23 Zr2 P2 C221 -35.51(7) . . . . ? N22 Zr2 P2 C221 67.92(7) . . . . ? N21 Zr2 P2 C221 171.25(7) . . . . ? N25 Zr2 P2 C221 -112.03(7) . . . . ? N24 Zr2 P2 C221 61.44(16) . . . . ? N13 Zr1 N11 C11 55.45(14) . . . . ? N12 Zr1 N11 C11 -66.62(13) . . . . ? N15 Zr1 N11 C11 144.38(12) . . . . ? N14 Zr1 N11 C11 5.88(12) . . . . ? P1 Zr1 N11 C11 -159.91(11) . . . . ? N13 Zr1 N11 Si11 -145.79(8) . . . . ? N12 Zr1 N11 Si11 92.14(9) . . . . ? N15 Zr1 N11 Si11 -56.86(9) . . . . ? N14 Zr1 N11 Si11 164.64(10) . . . . ? P1 Zr1 N11 Si11 -1.15(10) . . . . ? N13 Zr1 N12 C12 -40.67(11) . . . . ? N11 Zr1 N12 C12 96.54(11) . . . . ? N15 Zr1 N12 C12 -158.42(10) . . . . ? N14 Zr1 N12 C12 25.95(10) . . . . ? P1 Zr1 N12 C12 -148.80(10) . . . . ? N13 Zr1 N12 Si12 153.95(10) . . . . ? N11 Zr1 N12 Si12 -68.84(11) . . . . ? N15 Zr1 N12 Si12 36.20(17) . . . . ? N14 Zr1 N12 Si12 -139.43(12) . . . . ? P1 Zr1 N12 Si12 45.82(11) . . . . ? N11 Zr1 N13 C13 -17.27(12) . . . . ? N12 Zr1 N13 C13 102.53(10) . . . . ? N15 Zr1 N13 C13 -105.63(10) . . . . ? N14 Zr1 N13 C13 32.95(9) . . . . ? P1 Zr1 N13 C13 -163.69(9) . . . . ? N11 Zr1 N13 Si13 178.86(7) . . . . ? N12 Zr1 N13 Si13 -61.33(9) . . . . ? N15 Zr1 N13 Si13 90.51(8) . . . . ? N14 Zr1 N13 Si13 -130.91(9) . . . . ? P1 Zr1 N13 Si13 32.45(8) . . . . ? N13 Zr1 N14 C14 -121.95(11) . . . . ? N11 Zr1 N14 C14 20.13(10) . . . . ? N12 Zr1 N14 C14 125.65(11) . . . . ? N15 Zr1 N14 C14 -51.02(12) . . . . ? P1 Zr1 N14 C14 145.24(11) . . . . ? N13 Zr1 N14 C15 117.07(11) . . . . ? N11 Zr1 N14 C15 -100.86(11) . . . . ? N12 Zr1 N14 C15 4.66(10) . . . . ? N15 Zr1 N14 C15 -172.01(10) . . . . ? P1 Zr1 N14 C15 24.25(19) . . . . ? N13 Zr1 N14 C16 -2.51(10) . . . . ? N11 Zr1 N14 C16 139.56(11) . . . . ? N12 Zr1 N14 C16 -114.91(11) . . . . ? N15 Zr1 N14 C16 68.41(12) . . . . ? P1 Zr1 N14 C16 -95.33(14) . . . . ? N13 Zr1 N15 C116 -90.33(10) . . . . ? N11 Zr1 N15 C116 139.93(10) . . . . ? N12 Zr1 N15 C116 31.56(14) . . . . ? N14 Zr1 N15 C116 -154.51(9) . . . . ? P1 Zr1 N15 C116 20.41(8) . . . . ? N13 Zr1 N15 C117 65.40(14) . . . . ? N11 Zr1 N15 C117 -64.34(14) . . . . ? N12 Zr1 N15 C117 -172.72(12) . . . . ? N14 Zr1 N15 C117 1.21(16) . . . . ? P1 Zr1 N15 C117 176.13(15) . . . . ? N23 Zr2 N21 C21 57.69(14) . . . . ? N22 Zr2 N21 C21 -61.63(12) . . . . ? N25 Zr2 N21 C21 146.38(12) . . . . ? N24 Zr2 N21 C21 10.43(11) . . . . ? P2 Zr2 N21 C21 -156.54(11) . . . . ? N23 Zr2 N21 Si21 -144.38(8) . . . . ? N22 Zr2 N21 Si21 96.29(9) . . . . ? N25 Zr2 N21 Si21 -55.69(9) . . . . ? N24 Zr2 N21 Si21 168.36(10) . . . . ? P2 Zr2 N21 Si21 1.39(10) . . . . ? N23 Zr2 N22 C22 -41.23(11) . . . . ? N21 Zr2 N22 C22 96.55(10) . . . . ? N25 Zr2 N22 C22 -151.66(10) . . . . ? N24 Zr2 N22 C22 26.73(10) . . . . ? P2 Zr2 N22 C22 -151.74(10) . . . . ? N23 Zr2 N22 Si22 145.07(10) . . . . ? N21 Zr2 N22 Si22 -77.16(11) . . . . ? N25 Zr2 N22 Si22 34.63(16) . . . . ? N24 Zr2 N22 Si22 -146.98(11) . . . . ? P2 Zr2 N22 Si22 34.55(10) . . . . ? N22 Zr2 N23 C23 109.08(11) . . . . ? N21 Zr2 N23 C23 -10.17(13) . . . . ? N25 Zr2 N23 C23 -99.21(11) . . . . ? N24 Zr2 N23 C23 37.66(10) . . . . ? P2 Zr2 N23 C23 -156.24(10) . . . . ? N22 Zr2 N23 Si23 -56.68(10) . . . . ? N21 Zr2 N23 Si23 -175.93(7) . . . . ? N25 Zr2 N23 Si23 95.03(9) . . . . ? N24 Zr2 N23 Si23 -128.10(10) . . . . ? P2 Zr2 N23 Si23 38.00(10) . . . . ? N23 Zr2 N24 C24 -127.74(12) . . . . ? N22 Zr2 N24 C24 124.12(11) . . . . ? N21 Zr2 N24 C24 16.78(11) . . . . ? N25 Zr2 N24 C24 -57.00(13) . . . . ? P2 Zr2 N24 C24 130.79(13) . . . . ? N23 Zr2 N24 C25 111.83(10) . . . . ? N22 Zr2 N24 C25 3.69(10) . . . . ? N21 Zr2 N24 C25 -103.66(10) . . . . ? N25 Zr2 N24 C25 -177.44(9) . . . . ? P2 Zr2 N24 C25 10.4(2) . . . . ? N23 Zr2 N24 C26 -7.84(10) . . . . ? N22 Zr2 N24 C26 -115.98(11) . . . . ? N21 Zr2 N24 C26 136.68(11) . . . . ? N25 Zr2 N24 C26 62.90(12) . . . . ? P2 Zr2 N24 C26 -109.31(16) . . . . ? N23 Zr2 N25 C216 -92.01(9) . . . . ? N22 Zr2 N25 C216 21.84(14) . . . . ? N21 Zr2 N25 C216 136.76(9) . . . . ? N24 Zr2 N25 C216 -155.99(9) . . . . ? P2 Zr2 N25 C216 21.93(8) . . . . ? N23 Zr2 N25 C217 57.33(13) . . . . ? N22 Zr2 N25 C217 171.18(12) . . . . ? N21 Zr2 N25 C217 -73.89(13) . . . . ? N24 Zr2 N25 C217 -6.65(15) . . . . ? P2 Zr2 N25 C217 171.28(14) . . . . ? C11 N11 Si11 C19 168.10(12) . . . . ? Zr1 N11 Si11 C19 7.46(12) . . . . ? C11 N11 Si11 C17 -68.55(14) . . . . ? Zr1 N11 Si11 C17 130.81(10) . . . . ? C11 N11 Si11 C18 47.84(14) . . . . ? Zr1 N11 Si11 C18 -112.80(11) . . . . ? C12 N12 Si12 C111 -165.68(12) . . . . ? Zr1 N12 Si12 C111 -0.48(14) . . . . ? C12 N12 Si12 C112 71.18(13) . . . . ? Zr1 N12 Si12 C112 -123.62(11) . . . . ? C12 N12 Si12 C110 -47.46(13) . . . . ? Zr1 N12 Si12 C110 117.74(11) . . . . ? C13 N13 Si13 C114 -134.94(11) . . . . ? Zr1 N13 Si13 C114 28.56(10) . . . . ? C13 N13 Si13 C115 103.37(11) . . . . ? Zr1 N13 Si13 C115 -93.12(9) . . . . ? C13 N13 Si13 C113 -16.31(13) . . . . ? Zr1 N13 Si13 C113 147.20(8) . . . . ? C21 N21 Si21 C29 171.72(12) . . . . ? Zr2 N21 Si21 C29 12.00(13) . . . . ? C21 N21 Si21 C27 50.73(13) . . . . ? Zr2 N21 Si21 C27 -108.99(10) . . . . ? C21 N21 Si21 C28 -65.92(13) . . . . ? Zr2 N21 Si21 C28 134.36(10) . . . . ? C22 N22 Si22 C212 -160.10(11) . . . . ? Zr2 N22 Si22 C212 13.47(13) . . . . ? C22 N22 Si22 C210 76.74(12) . . . . ? Zr2 N22 Si22 C210 -109.69(11) . . . . ? C22 N22 Si22 C211 -42.57(14) . . . . ? Zr2 N22 Si22 C211 131.01(11) . . . . ? C23 N23 Si23 C213 -154.63(11) . . . . ? Zr2 N23 Si23 C213 10.70(12) . . . . ? C23 N23 Si23 C214 84.21(13) . . . . ? Zr2 N23 Si23 C214 -110.45(11) . . . . ? C23 N23 Si23 C215 -35.47(15) . . . . ? Zr2 N23 Si23 C215 129.86(11) . . . . ? Si11 N11 C11 C14 166.41(13) . . . . ? Zr1 N11 C11 C14 -31.0(2) . . . . ? Si12 N12 C12 C15 113.70(12) . . . . ? Zr1 N12 C12 C15 -55.74(14) . . . . ? Si13 N13 C13 C16 105.60(12) . . . . ? Zr1 N13 C13 C16 -59.93(13) . . . . ? C15 N14 C14 C11 74.46(18) . . . . ? C16 N14 C14 C11 -161.42(14) . . . . ? Zr1 N14 C14 C11 -41.88(16) . . . . ? N11 C11 C14 N14 48.5(2) . . . . ? C14 N14 C15 C12 -150.44(14) . . . . ? C16 N14 C15 C12 85.74(15) . . . . ? Zr1 N14 C15 C12 -33.59(15) . . . . ? N12 C12 C15 N14 60.07(17) . . . . ? C14 N14 C16 C13 91.40(15) . . . . ? C15 N14 C16 C13 -142.96(13) . . . . ? Zr1 N14 C16 C13 -26.14(14) . . . . ? N13 C13 C16 N14 52.83(16) . . . . ? Si21 N21 C21 C24 161.30(12) . . . . ? Zr2 N21 C21 C24 -36.41(18) . . . . ? Si22 N22 C22 C25 119.33(13) . . . . ? Zr2 N22 C22 C25 -55.98(15) . . . . ? Si23 N23 C23 C26 103.25(13) . . . . ? Zr2 N23 C23 C26 -64.87(14) . . . . ? C25 N24 C24 C21 75.73(17) . . . . ? C26 N24 C24 C21 -159.48(14) . . . . ? Zr2 N24 C24 C21 -40.08(16) . . . . ? N21 C21 C24 N24 50.41(19) . . . . ? C24 N24 C25 C22 -149.43(14) . . . . ? C26 N24 C25 C22 86.20(16) . . . . ? Zr2 N24 C25 C22 -32.44(15) . . . . ? N22 C22 C25 N24 59.32(18) . . . . ? C24 N24 C26 C23 96.48(15) . . . . ? C25 N24 C26 C23 -137.85(14) . . . . ? Zr2 N24 C26 C23 -21.66(15) . . . . ? N23 C23 C26 N24 52.91(16) . . . . ? C117 N15 C116 P1 167.28(10) . . . . ? Zr1 N15 C116 P1 -31.85(11) . . . . ? C121 P1 C116 N15 153.01(11) . . . . ? Zr1 P1 C116 N15 27.06(10) . . . . ? C116 N15 C117 C120 -80.65(18) . . . . ? Zr1 N15 C117 C120 127.03(14) . . . . ? C116 N15 C117 C119 160.11(15) . . . . ? Zr1 N15 C117 C119 7.8(2) . . . . ? C116 N15 C117 C118 40.20(19) . . . . ? Zr1 N15 C117 C118 -112.13(15) . . . . ? C116 P1 C121 C122 -0.23(15) . . . . ? Zr1 P1 C121 C122 83.24(14) . . . . ? C116 P1 C121 C126 177.04(12) . . . . ? Zr1 P1 C121 C126 -99.49(12) . . . . ? C126 C121 C122 C123 1.7(2) . . . . ? P1 C121 C122 C123 178.94(13) . . . . ? C121 C122 C123 C124 -0.2(3) . . . . ? C122 C123 C124 C125 -0.6(3) . . . . ? C123 C124 C125 C126 -0.1(3) . . . . ? C124 C125 C126 C121 1.7(3) . . . . ? C122 C121 C126 C125 -2.4(2) . . . . ? P1 C121 C126 C125 -179.92(13) . . . . ? C217 N25 C216 P2 169.48(10) . . . . ? Zr2 N25 C216 P2 -35.02(11) . . . . ? C221 P2 C216 N25 158.61(11) . . . . ? Zr2 P2 C216 N25 29.46(10) . . . . ? C216 N25 C217 C218 -170.08(14) . . . . ? Zr2 N25 C217 C218 44.98(18) . . . . ? C216 N25 C217 C220 -51.32(18) . . . . ? Zr2 N25 C217 C220 163.74(11) . . . . ? C216 N25 C217 C219 69.77(18) . . . . ? Zr2 N25 C217 C219 -75.18(17) . . . . ? C216 P2 C221 C222 -11.38(14) . . . . ? Zr2 P2 C221 C222 69.75(14) . . . . ? C216 P2 C221 C226 164.71(12) . . . . ? Zr2 P2 C221 C226 -114.16(11) . . . . ? C226 C221 C222 C223 -2.0(2) . . . . ? P2 C221 C222 C223 174.08(12) . . . . ? C221 C222 C223 C224 2.3(2) . . . . ? C222 C223 C224 C225 -0.4(3) . . . . ? C223 C224 C225 C226 -1.9(3) . . . . ? C224 C225 C226 C221 2.2(3) . . . . ? C222 C221 C226 C225 -0.2(2) . . . . ? P2 C221 C226 C225 -176.62(13) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.57 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.463 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.062 data_rw02 _database_code_depnum_ccdc_archive 'CCDC 900054' #TrackingRef '14694_web_deposit_cif_file_0_RoryWaterman_1350308768.RW02.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H56 N5 P Si3 Zr' _chemical_formula_weight 669.24 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' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.1609(10) _cell_length_b 20.3994(19) _cell_length_c 16.9631(16) _cell_angle_alpha 90.00 _cell_angle_beta 91.791(2) _cell_angle_gamma 90.00 _cell_volume 3514.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9712 _cell_measurement_theta_min 1.56 _cell_measurement_theta_max 32.20 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.265 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 0.485 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8862 _exptl_absorpt_correction_T_max 0.9440 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 65436 _diffrn_reflns_av_R_equivalents 0.0595 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 32.20 _reflns_number_total 12205 _reflns_number_gt 9712 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. In order to address high disorder, several sections of the molecule were modeled. ; _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^)+(0.0419P)^2^+10.9053P] 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 12205 _refine_ls_number_parameters 433 _refine_ls_number_restraints 509 _refine_ls_R_factor_all 0.0810 _refine_ls_R_factor_gt 0.0626 _refine_ls_wR_factor_ref 0.1474 _refine_ls_wR_factor_gt 0.1380 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.138 _refine_ls_shift/su_mean 0.006 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 0.423299(7) 0.216418(4) 0.988526(4) 0.01595(2) Uani 1 1 d DU . . P1 P 0.09015(2) 0.147572(12) 1.140415(13) 0.02186(5) Uani 1 1 d U . . C1 C 0.16003(9) 0.07579(4) 1.19020(5) 0.02258(19) Uani 1 1 d U A . C2 C 0.29028(10) 0.06962(5) 1.21772(6) 0.0298(2) Uani 1 1 d U . . H2 H 0.3512 0.1036 1.2070 0.040(3) Uiso 1 1 calc R A . C3 C 0.33298(11) 0.01545(5) 1.26007(6) 0.0325(2) Uani 1 1 d U A . H3 H 0.4227 0.0120 1.2770 0.043(4) Uiso 1 1 calc R . . C4 C 0.24533(11) -0.03374(5) 1.27788(6) 0.0313(2) Uani 1 1 d U . . H4 H 0.2741 -0.0708 1.3077 0.042(4) Uiso 1 1 calc R A . C5 C 0.11586(11) -0.02867(5) 1.25196(6) 0.0321(2) Uani 1 1 d U A . H5 H 0.0552 -0.0625 1.2637 0.053(4) Uiso 1 1 calc R . . C6 C 0.07348(10) 0.02575(5) 1.20863(5) 0.0277(2) Uani 1 1 d U . . H6 H -0.0162 0.0287 1.1914 0.059(4) Uiso 1 1 calc R A . C7 C 0.22347(8) 0.17465(4) 1.08915(5) 0.01888(18) Uani 1 1 d U A . H7 H 0.2985 0.1548 1.0863 0.018(3) Uiso 1 1 d R . . N1 N 0.23371(7) 0.22808(3) 1.04281(4) 0.01807(15) Uani 1 1 d U A . C8 C 0.11788(8) 0.27124(4) 1.03625(5) 0.02042(19) Uani 1 1 d U . . H8A H 0.0375 0.2430 1.0316 0.022(3) Uiso 1 1 calc R A . C9 C 0.10628(9) 0.31407(5) 1.10918(6) 0.0263(2) Uani 1 1 d U A . H9A H 0.1892 0.3389 1.1181 0.024(3) Uiso 1 1 calc R . . H9B H 0.0934 0.2858 1.1558 0.044(4) Uiso 1 1 calc R . . C10 C -0.00931(9) 0.36242(5) 1.10049(7) 0.0324(2) Uani 1 1 d U . . H10A H -0.0931 0.3376 1.0983 0.047(4) Uiso 1 1 calc R A . H10B H -0.0099 0.3914 1.1473 0.026(3) Uiso 1 1 calc R . . C11 C -0.00018(10) 0.40361(5) 1.02743(8) 0.0379(3) Uani 1 1 d U A . H11A H 0.0793 0.4316 1.0316 0.038(3) Uiso 1 1 calc R . . H11B H -0.0781 0.4326 1.0225 0.030(3) Uiso 1 1 calc R . . C12 C 0.00681(10) 0.36029(5) 0.95442(7) 0.0334(3) Uani 1 1 d U . . H12A H 0.0167 0.3881 0.9071 0.037(3) Uiso 1 1 calc R A . H12B H -0.0760 0.3350 0.9476 0.056(4) Uiso 1 1 calc R . . C13 C 0.12360(9) 0.31292(5) 0.96248(6) 0.0254(2) Uani 1 1 d U A . H13A H 0.1241 0.2839 0.9157 0.056(4) Uiso 1 1 calc R . . H13B H 0.2066 0.3384 0.9639 0.038(3) Uiso 1 1 calc R . . Si1 Si 0.24277(2) 0.084931(11) 0.900084(14) 0.01910(5) Uani 1 1 d DU . . C14 C 0.26584(10) 0.05780(5) 0.79544(5) 0.0274(2) Uani 1 1 d DU A . H14A H 0.3090 0.0928 0.7663 0.036(3) Uiso 1 1 calc R . . H14B H 0.1798 0.0482 0.7703 0.051(4) Uiso 1 1 calc R . . H14C H 0.3207 0.0183 0.7952 0.085(6) Uiso 1 1 calc R . . C15 C 0.21431(11) 0.01026(5) 0.96110(6) 0.0339(3) Uani 1 1 d DU A . H15A H 0.2043 0.0231 1.0163 0.039(3) Uiso 1 1 calc R . . H15B H 0.2895 -0.0195 0.9573 0.074(5) Uiso 1 1 calc R . . H15C H 0.1341 -0.0120 0.9418 0.045(4) Uiso 1 1 calc R . . C16 C 0.09179(8) 0.13586(5) 0.90251(5) 0.0237(2) Uani 1 1 d DU A . H16A H 0.0733 0.1469 0.9573 0.030(3) Uiso 1 1 calc R . . H16B H 0.0174 0.1114 0.8791 0.039(3) Uiso 1 1 calc R . . H16C H 0.1049 0.1762 0.8724 0.042(4) Uiso 1 1 calc R . . N2 N 0.38393(7) 0.12646(4) 0.93295(5) 0.02270(17) Uani 1 1 d U A . C17 C 0.50248(10) 0.08716(5) 0.91621(7) 0.0368(3) Uani 1 1 d U . . H17A H 0.4768 0.0470 0.8869 0.043(4) Uiso 1 1 calc R A . H17B H 0.5478 0.0740 0.9663 0.035(3) Uiso 1 1 calc R . . C18 C 0.59312(10) 0.12793(6) 0.86790(6) 0.0392(3) Uani 1 1 d U A . H18A H 0.6764 0.1041 0.8596 0.036(3) Uiso 1 1 calc R . . H18B H 0.5513 0.1378 0.8157 0.031(3) Uiso 1 1 calc R . . N3 N 0.61918(7) 0.18918(4) 0.91208(5) 0.02780(19) Uani 1 1 d DU A . C19 C 0.64261(10) 0.24493(6) 0.85824(5) 0.0336(2) Uani 1 1 d U . . H19A H 0.6793 0.2288 0.8085 0.033(3) Uiso 1 1 calc R A . H19B H 0.7067 0.2758 0.8831 0.035(3) Uiso 1 1 calc R . . C20 C 0.51273(10) 0.27954(6) 0.84123(5) 0.0347(3) Uani 1 1 d U A . H20A H 0.5271 0.3196 0.8098 0.038(3) Uiso 1 1 calc R . . H20B H 0.4519 0.2504 0.8109 0.047(4) Uiso 1 1 calc R . . N4 N 0.45614(7) 0.29677(4) 0.91777(4) 0.02366(18) Uani 1 1 d U A . Si2 Si 0.47680(2) 0.378196(13) 0.945733(16) 0.02591(6) Uani 1 1 d DU . . C21 C 0.64743(9) 0.40792(5) 0.92904(7) 0.0346(3) Uani 1 1 d DU A . H21A H 0.7102 0.3825 0.9617 0.046(4) Uiso 1 1 calc R . . H21B H 0.6540 0.4544 0.9433 0.063(5) Uiso 1 1 calc R . . H21C H 0.6677 0.4025 0.8733 0.047(4) Uiso 1 1 calc R . . C22 C 0.36323(11) 0.43459(6) 0.88972(8) 0.0441(3) Uani 1 1 d DU A . H22A H 0.2726 0.4269 0.9055 0.056(4) Uiso 1 1 calc R . . H22B H 0.3697 0.4263 0.8331 0.061(5) Uiso 1 1 calc R . . H22C H 0.3878 0.4801 0.9012 0.070(5) Uiso 1 1 calc R . . C23 C 0.44986(10) 0.38429(5) 1.05360(6) 0.0319(2) Uani 1 1 d DU A . H23A H 0.5280 0.3681 1.0829 0.064(5) Uiso 1 1 calc R . . H23B H 0.3732 0.3578 1.0670 0.047(4) Uiso 1 1 calc R . . H23C H 0.4342 0.4302 1.0677 0.061(5) Uiso 1 1 calc R . . C24 C 0.73044(13) 0.18134(8) 0.96937(9) 0.0290(2) Uani 0.6510(9) 1 d PDU A 1 H24A H 0.8143 0.1922 0.9442 0.037(5) Uiso 0.6510(9) 1 calc PR A 1 H24B H 0.7352 0.1354 0.9882 0.033(5) Uiso 0.6510(9) 1 calc PR A 1 C25 C 0.70811(12) 0.22739(7) 1.03813(8) 0.0237(2) Uani 0.6510(9) 1 d PDU A 1 H25A H 0.7769 0.2193 1.0796 0.034(5) Uiso 0.6510(9) 1 calc PR A 1 H25B H 0.7178 0.2732 1.0199 0.035(5) Uiso 0.6510(9) 1 calc PR A 1 N5 N 0.58018(9) 0.21986(5) 1.07191(6) 0.01374(15) Uani 0.6510(9) 1 d PDU A 1 Si3 Si 0.59250(3) 0.21753(2) 1.17384(2) 0.01974(6) Uani 0.6510(9) 1 d PDU A 1 C26 C 0.71504(15) 0.28073(9) 1.20792(9) 0.0388(4) Uani 0.6510(9) 1 d PDU A 1 H26A H 0.8032 0.2676 1.1922 0.041(5) Uiso 0.6510(9) 1 calc PR A 1 H26B H 0.7138 0.2846 1.2655 0.042(6) Uiso 0.6510(9) 1 calc PR A 1 H26C H 0.6923 0.3231 1.1839 0.030(5) Uiso 0.6510(9) 1 calc PR A 1 C27 C 0.64757(17) 0.13667(8) 1.21471(11) 0.0443(4) Uani 0.6510(9) 1 d PDU A 1 H27A H 0.5822 0.1030 1.2004 0.019(4) Uiso 0.6510(9) 1 calc PR A 1 H27B H 0.6568 0.1397 1.2723 0.071(8) Uiso 0.6510(9) 1 calc PR A 1 H27C H 0.7326 0.1249 1.1929 0.060(7) Uiso 0.6510(9) 1 calc PR A 1 C28 C 0.43630(12) 0.24401(7) 1.21904(7) 0.0217(2) Uani 0.6510(9) 1 d PDU A 1 H28A H 0.3650 0.2143 1.2024 0.093(10) Uiso 0.6510(9) 1 calc PR A 1 H28B H 0.4147 0.2887 1.2019 0.046(6) Uiso 0.6510(9) 1 calc PR A 1 H28C H 0.4471 0.2430 1.2766 0.023(4) Uiso 0.6510(9) 1 calc PR A 1 C24' C 0.7244(2) 0.17560(15) 0.97215(15) 0.0290(2) Uani 0.3490(9) 1 d PDU A 2 H24C H 0.8111 0.1827 0.9486 0.035 Uiso 0.3490(9) 1 calc PR A 2 H24D H 0.7192 0.1291 0.9884 0.035 Uiso 0.3490(9) 1 calc PR A 2 C25' C 0.7137(2) 0.21908(14) 1.04461(15) 0.0237(2) Uani 0.3490(9) 1 d PDU A 2 H25C H 0.7274 0.2656 1.0303 0.028 Uiso 0.3490(9) 1 calc PR A 2 H25D H 0.7811 0.2066 1.0853 0.028 Uiso 0.3490(9) 1 calc PR A 2 N5' N 0.57332(17) 0.20922(9) 1.07646(10) 0.01374(15) Uani 0.3490(9) 1 d PDU A 2 Si3' Si 0.58395(7) 0.20937(4) 1.17804(4) 0.01974(6) Uani 0.3490(9) 1 d PDU A 2 C26' C 0.7268(3) 0.25595(16) 1.21963(17) 0.0388(4) Uani 0.3490(9) 1 d PDU A 2 H26D H 0.8083 0.2384 1.1985 0.058 Uiso 0.3490(9) 1 calc PR A 2 H26E H 0.7297 0.2518 1.2772 0.058 Uiso 0.3490(9) 1 calc PR A 2 H26F H 0.7179 0.3023 1.2051 0.058 Uiso 0.3490(9) 1 calc PR A 2 C27' C 0.6162(3) 0.12049(13) 1.1954(2) 0.0443(4) Uani 0.3490(9) 1 d PDU A 2 H27D H 0.7017 0.1088 1.1742 0.066 Uiso 0.3490(9) 1 calc PR A 2 H27E H 0.5468 0.0945 1.1688 0.066 Uiso 0.3490(9) 1 calc PR A 2 H27F H 0.6170 0.1115 1.2521 0.066 Uiso 0.3490(9) 1 calc PR A 2 C28' C 0.4364(2) 0.23782(13) 1.23013(13) 0.0217(2) Uani 0.3490(9) 1 d PDU A 2 H28D H 0.4339 0.2858 1.2302 0.033 Uiso 0.3490(9) 1 calc PR A 2 H28E H 0.4405 0.2218 1.2846 0.033 Uiso 0.3490(9) 1 calc PR A 2 H28F H 0.3568 0.2208 1.2031 0.033 Uiso 0.3490(9) 1 calc PR A 2 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 0.01189(3) 0.02192(3) 0.01408(3) -0.00146(3) 0.00083(2) -0.00268(3) P1 0.01751(8) 0.02809(10) 0.02003(9) 0.00462(8) 0.00149(7) -0.00350(8) C1 0.0254(4) 0.0253(4) 0.0172(3) 0.0017(3) 0.0032(3) -0.0037(3) C2 0.0258(4) 0.0322(4) 0.0313(4) 0.0106(4) -0.0015(4) -0.0050(3) C3 0.0310(4) 0.0348(5) 0.0319(4) 0.0091(4) 0.0025(4) 0.0045(4) C4 0.0427(5) 0.0272(4) 0.0242(4) 0.0042(3) 0.0066(4) 0.0032(4) C5 0.0421(5) 0.0290(4) 0.0250(4) 0.0040(3) 0.0017(4) -0.0100(4) C6 0.0284(4) 0.0345(4) 0.0201(4) 0.0027(3) -0.0003(3) -0.0099(3) C7 0.0182(3) 0.0215(3) 0.0169(3) -0.0006(3) 0.0002(3) -0.0031(3) N1 0.0157(3) 0.0206(3) 0.0179(3) 0.0005(2) 0.0001(2) -0.0013(2) C8 0.0144(3) 0.0216(3) 0.0254(4) 0.0002(3) 0.0030(3) -0.0007(3) C9 0.0227(4) 0.0268(4) 0.0297(4) -0.0058(3) 0.0056(3) -0.0006(3) C10 0.0205(4) 0.0314(4) 0.0456(5) -0.0102(4) 0.0080(4) 0.0006(3) C11 0.0229(4) 0.0269(4) 0.0640(7) -0.0006(5) 0.0013(5) 0.0045(3) C12 0.0215(4) 0.0312(4) 0.0474(5) 0.0062(4) -0.0023(4) 0.0040(3) C13 0.0183(3) 0.0269(4) 0.0311(4) 0.0061(3) 0.0018(3) 0.0018(3) Si1 0.01737(9) 0.02065(9) 0.01913(9) -0.00018(8) -0.00178(8) -0.00394(8) C14 0.0326(4) 0.0245(4) 0.0252(4) -0.0039(3) 0.0024(3) 0.0009(3) C15 0.0353(5) 0.0322(4) 0.0337(5) 0.0093(4) -0.0062(4) -0.0077(4) C16 0.0214(3) 0.0308(4) 0.0186(3) -0.0018(3) -0.0055(3) -0.0002(3) N2 0.0146(3) 0.0263(3) 0.0271(3) -0.0058(3) 0.0004(3) -0.0015(2) C17 0.0201(4) 0.0338(4) 0.0568(6) -0.0191(4) 0.0038(4) -0.0004(3) C18 0.0201(4) 0.0545(5) 0.0436(5) -0.0316(4) 0.0095(4) -0.0066(4) N3 0.0167(3) 0.0423(4) 0.0247(3) -0.0151(3) 0.0061(3) -0.0088(3) C19 0.0258(4) 0.0575(6) 0.0180(3) -0.0091(4) 0.0098(3) -0.0117(4) C20 0.0307(4) 0.0608(6) 0.0127(3) 0.0019(4) 0.0018(3) -0.0118(4) N4 0.0182(3) 0.0364(4) 0.0163(3) 0.0044(3) -0.0013(2) -0.0051(3) Si2 0.01812(10) 0.02831(11) 0.03117(12) 0.01210(10) -0.00153(9) -0.00344(9) C21 0.0235(4) 0.0328(4) 0.0477(6) 0.0121(4) 0.0028(4) -0.0065(3) C22 0.0300(5) 0.0427(5) 0.0591(6) 0.0270(5) -0.0087(5) -0.0054(4) C23 0.0321(4) 0.0290(4) 0.0347(5) -0.0012(4) 0.0040(4) -0.0039(4) C24 0.0137(3) 0.0413(5) 0.0326(4) -0.0111(4) 0.0071(3) -0.0045(3) C25 0.0133(3) 0.0354(5) 0.0225(4) -0.0054(3) 0.0013(3) -0.0044(3) N5 0.0121(3) 0.0137(3) 0.0155(3) 0.0035(2) 0.0013(2) -0.0072(2) Si3 0.01378(9) 0.03123(12) 0.01426(9) 0.00559(9) 0.00115(8) -0.00347(9) C26 0.0306(5) 0.0662(9) 0.0195(5) -0.0084(6) 0.0001(4) -0.0190(6) C27 0.0342(6) 0.0541(6) 0.0452(6) 0.0279(5) 0.0116(5) 0.0150(5) C28 0.0236(4) 0.0317(4) 0.0101(3) 0.0001(3) 0.0037(3) -0.0031(3) C24' 0.0137(3) 0.0413(5) 0.0326(4) -0.0111(4) 0.0071(3) -0.0045(3) C25' 0.0133(3) 0.0354(5) 0.0225(4) -0.0054(3) 0.0013(3) -0.0044(3) N5' 0.0121(3) 0.0137(3) 0.0155(3) 0.0035(2) 0.0013(2) -0.0072(2) Si3' 0.01378(9) 0.03123(12) 0.01426(9) 0.00559(9) 0.00115(8) -0.00347(9) C26' 0.0306(5) 0.0662(9) 0.0195(5) -0.0084(6) 0.0001(4) -0.0190(6) C27' 0.0342(6) 0.0541(6) 0.0452(6) 0.0279(5) 0.0116(5) 0.0150(5) C28' 0.0236(4) 0.0317(4) 0.0101(3) 0.0001(3) 0.0037(3) -0.0031(3) _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 N4 2.0649(8) . ? Zr1 N2 2.0959(8) . ? Zr1 N5 2.0990(9) . ? Zr1 N5' 2.1043(17) . ? Zr1 N1 2.1740(7) . ? Zr1 N3 2.4725(8) . ? Zr1 C7 2.8247(9) . ? P1 C7 1.7234(9) . ? P1 C1 1.8231(9) . ? C1 C6 1.3895(13) . ? C1 C2 1.3952(13) . ? C2 C3 1.3807(14) . ? C2 H2 0.9500 . ? C3 C4 1.3813(15) . ? C3 H3 0.9500 . ? C4 C5 1.3778(16) . ? C4 H4 0.9500 . ? C5 C6 1.3922(14) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 N1 1.3497(11) . ? C7 H7 0.8660 . ? N1 C8 1.4713(11) . ? C8 C13 1.5154(13) . ? C8 C9 1.5222(13) . ? C8 H8A 1.0000 . ? C9 C10 1.5373(14) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.5028(17) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.5249(17) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.5332(14) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? Si1 N2 1.7424(8) . ? Si1 C16 1.8543(9) . ? Si1 C15 1.8691(11) . ? Si1 C14 1.8809(10) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? N2 C17 1.4818(13) . ? C17 C18 1.5029(16) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 N3 1.4766(14) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? N3 C24 1.4763(16) . ? N3 C24' 1.480(3) . ? N3 C19 1.4824(14) . ? C19 C20 1.5164(15) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 N4 1.4786(12) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? N4 Si2 1.7384(9) . ? Si2 C23 1.8628(11) . ? Si2 C21 1.8667(10) . ? Si2 C22 1.8680(12) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.520(2) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 N5 1.4450(16) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? N5 Si3 1.7302(10) . ? Si3 C28 1.8641(13) . ? Si3 C27 1.8682(18) . ? Si3 C26 1.8713(17) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C24' C25' 1.522(4) . ? C24' H24C 0.9900 . ? C24' H24D 0.9900 . ? C25' N5' 1.554(3) . ? C25' H25C 0.9900 . ? C25' H25D 0.9900 . ? N5' Si3' 1.7231(18) . ? Si3' C26' 1.856(3) . ? Si3' C28' 1.857(2) . ? Si3' C27' 1.864(3) . ? C26' H26D 0.9800 . ? C26' H26E 0.9800 . ? C26' H26F 0.9800 . ? C27' H27D 0.9800 . ? C27' H27E 0.9800 . ? C27' H27F 0.9800 . ? C28' H28D 0.9800 . ? C28' H28E 0.9800 . ? C28' H28F 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 N4 Zr1 N2 117.75(3) . . ? N4 Zr1 N5 103.42(3) . . ? N2 Zr1 N5 117.56(3) . . ? N4 Zr1 N5' 109.92(5) . . ? N2 Zr1 N5' 112.43(5) . . ? N5 Zr1 N5' 6.58(6) . . ? N4 Zr1 N1 108.71(3) . . ? N2 Zr1 N1 97.30(3) . . ? N5 Zr1 N1 112.04(3) . . ? N5' Zr1 N1 109.83(5) . . ? N4 Zr1 N3 74.11(3) . . ? N2 Zr1 N3 73.31(3) . . ? N5 Zr1 N3 75.77(3) . . ? N5' Zr1 N3 77.23(5) . . ? N1 Zr1 N3 170.14(3) . . ? N4 Zr1 C7 136.30(3) . . ? N2 Zr1 C7 82.93(3) . . ? N5 Zr1 C7 98.51(3) . . ? N5' Zr1 C7 93.96(5) . . ? N1 Zr1 C7 27.61(2) . . ? N3 Zr1 C7 148.73(3) . . ? C7 P1 C1 100.96(4) . . ? C6 C1 C2 117.31(8) . . ? C6 C1 P1 117.02(7) . . ? C2 C1 P1 125.39(7) . . ? C3 C2 C1 121.72(9) . . ? C3 C2 H2 119.1 . . ? C1 C2 H2 119.1 . . ? C2 C3 C4 120.06(10) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 119.43(9) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 120.32(10) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C1 C6 C5 121.14(9) . . ? C1 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? N1 C7 P1 128.96(6) . . ? N1 C7 Zr1 48.28(4) . . ? P1 C7 Zr1 173.12(4) . . ? N1 C7 H7 105.1 . . ? P1 C7 H7 125.9 . . ? Zr1 C7 H7 57.0 . . ? C7 N1 C8 116.82(7) . . ? C7 N1 Zr1 104.11(5) . . ? C8 N1 Zr1 138.66(5) . . ? N1 C8 C13 110.30(7) . . ? N1 C8 C9 111.35(7) . . ? C13 C8 C9 110.79(7) . . ? N1 C8 H8A 108.1 . . ? C13 C8 H8A 108.1 . . ? C9 C8 H8A 108.1 . . ? C8 C9 C10 111.64(8) . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C11 C10 C9 111.79(9) . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10B 109.3 . . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? C10 C11 C12 110.57(9) . . ? C10 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C11 C12 C13 110.39(9) . . ? C11 C12 H12A 109.6 . . ? C13 C12 H12A 109.6 . . ? C11 C12 H12B 109.6 . . ? C13 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? C8 C13 C12 112.19(8) . . ? C8 C13 H13A 109.2 . . ? C12 C13 H13A 109.2 . . ? C8 C13 H13B 109.2 . . ? C12 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? N2 Si1 C16 113.19(4) . . ? N2 Si1 C15 111.04(4) . . ? C16 Si1 C15 107.57(5) . . ? N2 Si1 C14 108.63(4) . . ? C16 Si1 C14 108.26(4) . . ? C15 Si1 C14 107.99(5) . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C17 N2 Si1 109.98(6) . . ? C17 N2 Zr1 114.52(6) . . ? Si1 N2 Zr1 135.50(4) . . ? N2 C17 C18 108.72(8) . . ? N2 C17 H17A 109.9 . . ? C18 C17 H17A 109.9 . . ? N2 C17 H17B 109.9 . . ? C18 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? N3 C18 C17 107.14(9) . . ? N3 C18 H18A 110.3 . . ? C17 C18 H18A 110.3 . . ? N3 C18 H18B 110.3 . . ? C17 C18 H18B 110.3 . . ? H18A C18 H18B 108.5 . . ? C24 N3 C18 111.34(9) . . ? C24 N3 C24' 5.48(13) . . ? C18 N3 C24' 107.78(13) . . ? C24 N3 C19 110.74(9) . . ? C18 N3 C19 111.48(8) . . ? C24' N3 C19 116.20(13) . . ? C24 N3 Zr1 106.95(7) . . ? C18 N3 Zr1 108.77(6) . . ? C24' N3 Zr1 104.88(10) . . ? C19 N3 Zr1 107.34(6) . . ? N3 C19 C20 108.59(8) . . ? N3 C19 H19A 110.0 . . ? C20 C19 H19A 110.0 . . ? N3 C19 H19B 110.0 . . ? C20 C19 H19B 110.0 . . ? H19A C19 H19B 108.4 . . ? N4 C20 C19 107.67(7) . . ? N4 C20 H20A 110.2 . . ? C19 C20 H20A 110.2 . . ? N4 C20 H20B 110.2 . . ? C19 C20 H20B 110.2 . . ? H20A C20 H20B 108.5 . . ? C20 N4 Si2 114.82(7) . . ? C20 N4 Zr1 113.33(7) . . ? Si2 N4 Zr1 128.33(4) . . ? N4 Si2 C23 108.16(4) . . ? N4 Si2 C21 111.95(4) . . ? C23 Si2 C21 107.04(5) . . ? N4 Si2 C22 112.47(5) . . ? C23 Si2 C22 110.56(5) . . ? C21 Si2 C22 106.54(5) . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N3 C24 C25 107.97(11) . . ? N3 C24 H24A 110.1 . . ? C25 C24 H24A 110.1 . . ? N3 C24 H24B 110.1 . . ? C25 C24 H24B 110.1 . . ? H24A C24 H24B 108.4 . . ? N5 C25 C24 113.35(11) . . ? N5 C25 H25A 108.9 . . ? C24 C25 H25A 108.9 . . ? N5 C25 H25B 108.9 . . ? C24 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? C25 N5 Si3 111.18(8) . . ? C25 N5 Zr1 114.20(8) . . ? Si3 N5 Zr1 134.60(5) . . ? N5 Si3 C28 111.54(5) . . ? N5 Si3 C27 114.00(7) . . ? C28 Si3 C27 110.62(7) . . ? N5 Si3 C26 108.44(6) . . ? C28 Si3 C26 103.89(7) . . ? C27 Si3 C26 107.76(8) . . ? N3 C24' C25' 112.3(2) . . ? N3 C24' H24C 109.2 . . ? C25' C24' H24C 109.2 . . ? N3 C24' H24D 109.2 . . ? C25' C24' H24D 109.2 . . ? H24C C24' H24D 107.9 . . ? C24' C25' N5' 107.14(19) . . ? C24' C25' H25C 110.3 . . ? N5' C25' H25C 110.3 . . ? C24' C25' H25D 110.3 . . ? N5' C25' H25D 110.3 . . ? H25C C25' H25D 108.5 . . ? C25' N5' Si3' 108.54(13) . . ? C25' N5' Zr1 113.39(13) . . ? Si3' N5' Zr1 136.90(10) . . ? N5' Si3' C26' 113.89(11) . . ? N5' Si3' C28' 116.74(10) . . ? C26' Si3' C28' 107.02(12) . . ? N5' Si3' C27' 99.27(13) . . ? C26' Si3' C27' 107.85(15) . . ? C28' Si3' C27' 111.69(14) . . ? Si3' C26' H26D 109.5 . . ? Si3' C26' H26E 109.5 . . ? H26D C26' H26E 109.5 . . ? Si3' C26' H26F 109.5 . . ? H26D C26' H26F 109.5 . . ? H26E C26' H26F 109.5 . . ? Si3' C27' H27D 109.5 . . ? Si3' C27' H27E 109.5 . . ? H27D C27' H27E 109.5 . . ? Si3' C27' H27F 109.5 . . ? H27D C27' H27F 109.5 . . ? H27E C27' H27F 109.5 . . ? Si3' C28' H28D 109.5 . . ? Si3' C28' H28E 109.5 . . ? H28D C28' H28E 109.5 . . ? Si3' C28' H28F 109.5 . . ? H28D C28' H28F 109.5 . . ? H28E C28' H28F 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 C7 P1 C1 C6 -152.48(7) . . . . ? C7 P1 C1 C2 33.85(9) . . . . ? C6 C1 C2 C3 1.43(14) . . . . ? P1 C1 C2 C3 175.09(8) . . . . ? C1 C2 C3 C4 -1.56(16) . . . . ? C2 C3 C4 C5 1.02(16) . . . . ? C3 C4 C5 C6 -0.40(15) . . . . ? C2 C1 C6 C5 -0.80(14) . . . . ? P1 C1 C6 C5 -175.00(8) . . . . ? C4 C5 C6 C1 0.31(15) . . . . ? C1 P1 C7 N1 -177.59(8) . . . . ? C1 P1 C7 Zr1 118.7(4) . . . . ? N4 Zr1 C7 N1 2.44(7) . . . . ? N2 Zr1 C7 N1 -120.89(5) . . . . ? N5 Zr1 C7 N1 122.18(6) . . . . ? N5' Zr1 C7 N1 126.97(7) . . . . ? N3 Zr1 C7 N1 -161.26(5) . . . . ? N4 Zr1 C7 P1 71.5(4) . . . . ? N2 Zr1 C7 P1 -51.8(4) . . . . ? N5 Zr1 C7 P1 -168.7(4) . . . . ? N5' Zr1 C7 P1 -163.9(4) . . . . ? N1 Zr1 C7 P1 69.1(4) . . . . ? N3 Zr1 C7 P1 -92.2(4) . . . . ? P1 C7 N1 C8 2.30(11) . . . . ? Zr1 C7 N1 C8 174.03(8) . . . . ? P1 C7 N1 Zr1 -171.73(5) . . . . ? N4 Zr1 N1 C7 -178.22(5) . . . . ? N2 Zr1 N1 C7 59.16(5) . . . . ? N5 Zr1 N1 C7 -64.56(6) . . . . ? N5' Zr1 N1 C7 -57.92(7) . . . . ? N3 Zr1 N1 C7 76.69(17) . . . . ? N4 Zr1 N1 C8 9.85(9) . . . . ? N2 Zr1 N1 C8 -112.77(8) . . . . ? N5 Zr1 N1 C8 123.52(8) . . . . ? N5' Zr1 N1 C8 130.16(9) . . . . ? N3 Zr1 N1 C8 -95.23(17) . . . . ? C7 Zr1 N1 C8 -171.92(11) . . . . ? C7 N1 C8 C13 -159.32(7) . . . . ? Zr1 N1 C8 C13 11.90(11) . . . . ? C7 N1 C8 C9 77.25(9) . . . . ? Zr1 N1 C8 C9 -111.53(8) . . . . ? N1 C8 C9 C10 176.31(7) . . . . ? C13 C8 C9 C10 53.16(10) . . . . ? C8 C9 C10 C11 -55.05(11) . . . . ? C9 C10 C11 C12 56.55(11) . . . . ? C10 C11 C12 C13 -56.77(11) . . . . ? N1 C8 C13 C12 -178.25(7) . . . . ? C9 C8 C13 C12 -54.50(10) . . . . ? C11 C12 C13 C8 56.35(11) . . . . ? C16 Si1 N2 C17 -170.05(7) . . . . ? C15 Si1 N2 C17 68.84(8) . . . . ? C14 Si1 N2 C17 -49.77(8) . . . . ? C16 Si1 N2 Zr1 9.68(8) . . . . ? C15 Si1 N2 Zr1 -111.43(7) . . . . ? C14 Si1 N2 Zr1 129.96(6) . . . . ? N4 Zr1 N2 C17 88.41(7) . . . . ? N5 Zr1 N2 C17 -36.36(8) . . . . ? N5' Zr1 N2 C17 -40.92(9) . . . . ? N1 Zr1 N2 C17 -155.94(7) . . . . ? N3 Zr1 N2 C17 27.15(7) . . . . ? C7 Zr1 N2 C17 -132.30(7) . . . . ? N4 Zr1 N2 Si1 -91.31(7) . . . . ? N5 Zr1 N2 Si1 143.92(6) . . . . ? N5' Zr1 N2 Si1 139.36(7) . . . . ? N1 Zr1 N2 Si1 24.34(6) . . . . ? N3 Zr1 N2 Si1 -152.57(7) . . . . ? C7 Zr1 N2 Si1 47.98(6) . . . . ? Si1 N2 C17 C18 123.97(8) . . . . ? Zr1 N2 C17 C18 -55.83(10) . . . . ? N2 C17 C18 N3 55.27(10) . . . . ? C17 C18 N3 C24 86.37(10) . . . . ? C17 C18 N3 C24' 81.95(13) . . . . ? C17 C18 N3 C19 -149.41(8) . . . . ? C17 C18 N3 Zr1 -31.24(9) . . . . ? N4 Zr1 N3 C24 116.75(8) . . . . ? N2 Zr1 N3 C24 -117.04(8) . . . . ? N5 Zr1 N3 C24 8.02(8) . . . . ? N5' Zr1 N3 C24 1.42(9) . . . . ? N1 Zr1 N3 C24 -135.22(15) . . . . ? C7 Zr1 N3 C24 -74.89(9) . . . . ? N4 Zr1 N3 C18 -122.89(7) . . . . ? N2 Zr1 N3 C18 3.32(6) . . . . ? N5 Zr1 N3 C18 128.38(7) . . . . ? N5' Zr1 N3 C18 121.78(8) . . . . ? N1 Zr1 N3 C18 -14.85(19) . . . . ? C7 Zr1 N3 C18 45.48(8) . . . . ? N4 Zr1 N3 C24' 122.02(13) . . . . ? N2 Zr1 N3 C24' -111.76(13) . . . . ? N5 Zr1 N3 C24' 13.30(13) . . . . ? N5' Zr1 N3 C24' 6.69(13) . . . . ? N1 Zr1 N3 C24' -129.94(18) . . . . ? C7 Zr1 N3 C24' -69.61(14) . . . . ? N4 Zr1 N3 C19 -2.14(6) . . . . ? N2 Zr1 N3 C19 124.08(6) . . . . ? N5 Zr1 N3 C19 -110.87(6) . . . . ? N5' Zr1 N3 C19 -117.47(8) . . . . ? N1 Zr1 N3 C19 105.90(16) . . . . ? C7 Zr1 N3 C19 166.23(5) . . . . ? C24 N3 C19 C20 -142.87(9) . . . . ? C18 N3 C19 C20 92.57(9) . . . . ? C24' N3 C19 C20 -143.43(13) . . . . ? Zr1 N3 C19 C20 -26.46(9) . . . . ? N3 C19 C20 N4 54.09(11) . . . . ? C19 C20 N4 Si2 101.24(9) . . . . ? C19 C20 N4 Zr1 -59.43(9) . . . . ? N2 Zr1 N4 C20 -28.60(7) . . . . ? N5 Zr1 N4 C20 102.93(6) . . . . ? N5' Zr1 N4 C20 101.89(8) . . . . ? N1 Zr1 N4 C20 -137.86(6) . . . . ? N3 Zr1 N4 C20 32.24(6) . . . . ? C7 Zr1 N4 C20 -139.05(6) . . . . ? N2 Zr1 N4 Si2 173.91(4) . . . . ? N5 Zr1 N4 Si2 -54.56(6) . . . . ? N5' Zr1 N4 Si2 -55.59(7) . . . . ? N1 Zr1 N4 Si2 64.65(6) . . . . ? N3 Zr1 N4 Si2 -125.25(6) . . . . ? C7 Zr1 N4 Si2 63.46(7) . . . . ? C20 N4 Si2 C23 -162.09(7) . . . . ? Zr1 N4 Si2 C23 -4.89(7) . . . . ? C20 N4 Si2 C21 -44.41(8) . . . . ? Zr1 N4 Si2 C21 112.80(6) . . . . ? C20 N4 Si2 C22 75.52(8) . . . . ? Zr1 N4 Si2 C22 -127.27(6) . . . . ? C18 N3 C24 C25 -150.52(10) . . . . ? C24' N3 C24 C25 -100.4(13) . . . . ? C19 N3 C24 C25 84.84(12) . . . . ? Zr1 N3 C24 C25 -31.81(12) . . . . ? N3 C24 C25 N5 52.67(15) . . . . ? C24 C25 N5 Si3 134.37(10) . . . . ? C24 C25 N5 Zr1 -46.94(13) . . . . ? N4 Zr1 N5 C25 -49.71(9) . . . . ? N2 Zr1 N5 C25 81.93(9) . . . . ? N5' Zr1 N5 C25 121.8(5) . . . . ? N1 Zr1 N5 C25 -166.61(8) . . . . ? N3 Zr1 N5 C25 19.74(8) . . . . ? C7 Zr1 N5 C25 168.36(8) . . . . ? N4 Zr1 N5 Si3 128.58(7) . . . . ? N2 Zr1 N5 Si3 -99.78(8) . . . . ? N5' Zr1 N5 Si3 -59.9(5) . . . . ? N1 Zr1 N5 Si3 11.68(8) . . . . ? N3 Zr1 N5 Si3 -161.97(8) . . . . ? C7 Zr1 N5 Si3 -13.35(8) . . . . ? C25 N5 Si3 C28 155.25(9) . . . . ? Zr1 N5 Si3 C28 -23.07(10) . . . . ? C25 N5 Si3 C27 -78.58(11) . . . . ? Zr1 N5 Si3 C27 103.09(9) . . . . ? C25 N5 Si3 C26 41.44(11) . . . . ? Zr1 N5 Si3 C26 -136.89(8) . . . . ? C24 N3 C24' C25' 77.6(13) . . . . ? C18 N3 C24' C25' -151.02(18) . . . . ? C19 N3 C24' C25' 83.1(2) . . . . ? Zr1 N3 C24' C25' -35.2(2) . . . . ? N3 C24' C25' N5' 55.7(3) . . . . ? C24' C25' N5' Si3' 141.68(17) . . . . ? C24' C25' N5' Zr1 -48.6(2) . . . . ? N4 Zr1 N5' C25' -45.31(16) . . . . ? N2 Zr1 N5' C25' 87.96(15) . . . . ? N5 Zr1 N5' C25' -54.1(5) . . . . ? N1 Zr1 N5' C25' -164.88(14) . . . . ? N3 Zr1 N5' C25' 22.31(14) . . . . ? C7 Zr1 N5' C25' 171.95(14) . . . . ? N4 Zr1 N5' Si3' 120.38(14) . . . . ? N2 Zr1 N5' Si3' -106.35(14) . . . . ? N5 Zr1 N5' Si3' 111.6(6) . . . . ? N1 Zr1 N5' Si3' 0.81(16) . . . . ? N3 Zr1 N5' Si3' -172.01(16) . . . . ? C7 Zr1 N5' Si3' -22.37(15) . . . . ? C25' N5' Si3' C26' 26.1(2) . . . . ? Zr1 N5' Si3' C26' -140.03(16) . . . . ? C25' N5' Si3' C28' 151.69(16) . . . . ? Zr1 N5' Si3' C28' -14.5(2) . . . . ? C25' N5' Si3' C27' -88.21(18) . . . . ? Zr1 N5' Si3' C27' 105.64(17) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 32.20 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 5.358 _refine_diff_density_min -1.010 _refine_diff_density_rms 0.125 data_rw1149zr _database_code_depnum_ccdc_archive 'CCDC 900055' #TrackingRef '13734_web_deposit_cif_file_2_RoryWaterman_1346784222.RW1149Zr.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H57 Cl N5 P Si3 Zr' _chemical_formula_sum 'C29 H57 Cl N5 P Si3 Zr' _chemical_formula_weight 717.71 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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6702(4) _cell_length_b 11.2128(4) _cell_length_c 16.7109(6) _cell_angle_alpha 83.7040(10) _cell_angle_beta 72.3920(10) _cell_angle_gamma 78.7610(10) _cell_volume 1866.37(12) _cell_formula_units_Z 2 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9995 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 31.50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.531 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8278 _exptl_absorpt_correction_T_max 0.9439 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30223 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 30.51 _reflns_number_total 11282 _reflns_number_gt 9476 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+0.4013P] 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 11282 _refine_ls_number_parameters 391 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0743 _refine_ls_wR_factor_gt 0.0700 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 Zr Zr 0.874564(13) 0.229750(12) 0.266444(8) 0.01415(4) Uani 1 1 d . . . P P 0.80972(4) 0.65642(4) 0.19973(3) 0.02487(9) Uani 1 1 d . . . Si1 Si 1.17721(4) 0.12904(4) 0.30947(3) 0.02424(9) Uani 1 1 d . . . Si2 Si 0.79506(4) 0.27084(4) 0.07305(2) 0.01822(8) Uani 1 1 d . . . Si3 Si 0.59088(4) 0.26275(4) 0.43315(3) 0.01977(8) Uani 1 1 d . . . N1 N 1.06528(12) 0.13315(11) 0.25193(8) 0.0191(2) Uani 1 1 d . . . N2 N 0.78306(12) 0.21231(10) 0.17538(7) 0.0168(2) Uani 1 1 d . . . N3 N 0.75006(12) 0.18765(11) 0.38356(7) 0.0186(2) Uani 1 1 d . . . N4 N 0.86202(12) 0.00562(11) 0.27001(8) 0.0189(2) Uani 1 1 d . . . N5 N 0.89501(12) 0.42246(11) 0.25897(8) 0.0179(2) Uani 1 1 d . . . C1 C 1.09160(15) 0.02693(14) 0.19918(9) 0.0226(3) Uani 1 1 d . . . H1A H 1.1863 -0.0126 0.1873 0.027 Uiso 1 1 calc R . . H1B H 1.0725 0.0540 0.1450 0.027 Uiso 1 1 calc R . . C2 C 0.70171(15) 0.11311(13) 0.19920(10) 0.0205(3) Uani 1 1 d . . . H2A H 0.6572 0.1090 0.1557 0.025 Uiso 1 1 calc R . . H2B H 0.6321 0.1292 0.2534 0.025 Uiso 1 1 calc R . . C3 C 0.78820(16) 0.06216(13) 0.41668(9) 0.0217(3) Uani 1 1 d . . . H3A H 0.7264 0.0476 0.4730 0.026 Uiso 1 1 calc R . . H3B H 0.8797 0.0509 0.4221 0.026 Uiso 1 1 calc R . . C4 C 1.00106(15) -0.06195(14) 0.24786(10) 0.0237(3) Uani 1 1 d . . . H4A H 1.0097 -0.1307 0.2130 0.028 Uiso 1 1 calc R . . H4B H 1.0258 -0.0950 0.2995 0.028 Uiso 1 1 calc R . . C5 C 0.79369(16) -0.00623(13) 0.20707(10) 0.0221(3) Uani 1 1 d . . . H5A H 0.7415 -0.0734 0.2252 0.027 Uiso 1 1 calc R . . H5B H 0.8601 -0.0247 0.1521 0.027 Uiso 1 1 calc R . . C6 C 0.78196(16) -0.02757(13) 0.35622(9) 0.0232(3) Uani 1 1 d . . . H6A H 0.8178 -0.1114 0.3735 0.028 Uiso 1 1 calc R . . H6B H 0.6882 -0.0248 0.3573 0.028 Uiso 1 1 calc R . . C7 C 1.33578(17) 0.1782(2) 0.24282(12) 0.0411(5) Uani 1 1 d . . . H7A H 1.3761 0.1256 0.1953 0.062 Uiso 1 1 calc R . . H7B H 1.3978 0.1721 0.2766 0.062 Uiso 1 1 calc R . . H7C H 1.3165 0.2627 0.2216 0.062 Uiso 1 1 calc R . . C8 C 1.2268(2) -0.02938(17) 0.35179(12) 0.0391(5) Uani 1 1 d . . . H8A H 1.2597 -0.0848 0.3057 0.059 Uiso 1 1 calc R . . H8B H 1.1493 -0.0558 0.3936 0.059 Uiso 1 1 calc R . . H8C H 1.2974 -0.0303 0.3782 0.059 Uiso 1 1 calc R . . C9 C 1.09770(18) 0.22688(16) 0.40131(11) 0.0305(4) Uani 1 1 d . . . H9A H 1.1111 0.3110 0.3841 0.046 Uiso 1 1 calc R . . H9B H 1.1384 0.1967 0.4466 0.046 Uiso 1 1 calc R . . H9C H 1.0019 0.2242 0.4214 0.046 Uiso 1 1 calc R . . C10 C 0.84905(18) 0.14533(16) -0.00228(10) 0.0301(4) Uani 1 1 d . . . H10A H 0.7880 0.0863 0.0164 0.045 Uiso 1 1 calc R . . H10B H 0.9397 0.1045 -0.0040 0.045 Uiso 1 1 calc R . . H10C H 0.8476 0.1797 -0.0586 0.045 Uiso 1 1 calc R . . C11 C 0.62915(17) 0.35707(16) 0.06643(11) 0.0295(3) Uani 1 1 d . . . H11A H 0.5638 0.3019 0.0816 0.044 Uiso 1 1 calc R . . H11B H 0.6374 0.3914 0.0089 0.044 Uiso 1 1 calc R . . H11C H 0.5995 0.4231 0.1053 0.044 Uiso 1 1 calc R . . C12 C 0.92497(17) 0.36935(16) 0.03847(10) 0.0278(3) Uani 1 1 d . . . H12A H 0.8871 0.4507 0.0595 0.042 Uiso 1 1 calc R . . H12B H 0.9564 0.3754 -0.0231 0.042 Uiso 1 1 calc R . . H12C H 1.0000 0.3339 0.0607 0.042 Uiso 1 1 calc R . . C13 C 0.58092(18) 0.31262(17) 0.53832(10) 0.0324(4) Uani 1 1 d . . . H13A H 0.6362 0.3756 0.5309 0.049 Uiso 1 1 calc R . . H13B H 0.6133 0.2428 0.5718 0.049 Uiso 1 1 calc R . . H13C H 0.4881 0.3457 0.5674 0.049 Uiso 1 1 calc R . . C14 C 0.46115(17) 0.16257(16) 0.45458(12) 0.0314(4) Uani 1 1 d . . . H14A H 0.4710 0.1221 0.4034 0.047 Uiso 1 1 calc R . . H14B H 0.3721 0.2122 0.4722 0.047 Uiso 1 1 calc R . . H14C H 0.4726 0.1011 0.4994 0.047 Uiso 1 1 calc R . . C15 C 0.54421(16) 0.39159(14) 0.36136(10) 0.0258(3) Uani 1 1 d . . . H15A H 0.6008 0.4531 0.3553 0.039 Uiso 1 1 calc R . . H15B H 0.4505 0.4281 0.3849 0.039 Uiso 1 1 calc R . . H15C H 0.5568 0.3613 0.3062 0.039 Uiso 1 1 calc R . . C16 C 0.98761(15) 0.47710(13) 0.28373(9) 0.0205(3) Uani 1 1 d . A . C17 C 1.11682(16) 0.47975(15) 0.23088(10) 0.0258(3) Uani 1 1 d . . . C19 C 1.20711(19) 0.52990(18) 0.25641(12) 0.0368(4) Uani 1 1 d . A . H19A H 1.2954 0.5290 0.2206 0.044 Uiso 1 1 calc R . . C20 C 1.1690(2) 0.58095(18) 0.33353(13) 0.0394(4) Uani 1 1 d . . . H20A H 1.2309 0.6154 0.3505 0.047 Uiso 1 1 calc R A . C21 C 1.04107(19) 0.58193(16) 0.38584(12) 0.0339(4) Uani 1 1 d . A . H21A H 1.0146 0.6179 0.4386 0.041 Uiso 1 1 calc R . . C22 C 0.95075(16) 0.53046(14) 0.36164(10) 0.0249(3) Uani 1 1 d . . . C23 C 0.81391(14) 0.50336(13) 0.22075(9) 0.0181(3) Uani 1 1 d . . . H23A H 0.7516 0.4697 0.2037 0.022 Uiso 1 1 calc R . . C24 C 0.68068(16) 0.68802(13) 0.14105(10) 0.0234(3) Uani 1 1 d . . . H24A H 0.6869 0.6129 0.1119 0.028 Uiso 1 1 calc R . . C25 C 0.71225(17) 0.79072(16) 0.07341(11) 0.0295(3) Uani 1 1 d . . . H25A H 0.7120 0.8649 0.1006 0.035 Uiso 1 1 calc R . . H25B H 0.8027 0.7668 0.0348 0.035 Uiso 1 1 calc R . . C26 C 0.61134(19) 0.81933(17) 0.02273(11) 0.0338(4) Uani 1 1 d . . . H26A H 0.6325 0.8887 -0.0181 0.041 Uiso 1 1 calc R . . H26B H 0.6179 0.7479 -0.0092 0.041 Uiso 1 1 calc R . . C27 C 0.47004(19) 0.85084(16) 0.08012(12) 0.0349(4) Uani 1 1 d . . . H27A H 0.4062 0.8644 0.0463 0.042 Uiso 1 1 calc R . . H27B H 0.4609 0.9271 0.1077 0.042 Uiso 1 1 calc R . . C28 C 0.43688(18) 0.74872(18) 0.14698(13) 0.0372(4) Uani 1 1 d . . . H28A H 0.4366 0.6749 0.1196 0.045 Uiso 1 1 calc R . . H28B H 0.3464 0.7732 0.1854 0.045 Uiso 1 1 calc R . . C29 C 0.53799(18) 0.71900(17) 0.19792(11) 0.0336(4) Uani 1 1 d . . . H29A H 0.5308 0.7898 0.2306 0.040 Uiso 1 1 calc R . . H29B H 0.5166 0.6491 0.2382 0.040 Uiso 1 1 calc R . . Cl Cl 1.1652(5) 0.4231(5) 0.1318(4) 0.0353(6) Uani 0.459(2) 1 d P A 1 C18 C 0.8125(18) 0.528(2) 0.4225(13) 0.037(4) Uani 0.459(2) 1 d P A 1 H18A H 0.7453 0.5779 0.3983 0.056 Uiso 0.459(2) 1 calc PR A 1 H18B H 0.8072 0.5606 0.4757 0.056 Uiso 0.459(2) 1 calc PR A 1 H18C H 0.7959 0.4439 0.4328 0.056 Uiso 0.459(2) 1 calc PR A 1 C18' C 1.1616(15) 0.4261(16) 0.1452(10) 0.037(3) Uani 0.541(2) 1 d P A 2 H18D H 1.1078 0.4717 0.1100 0.056 Uiso 0.541(2) 1 calc PR A 2 H18E H 1.1500 0.3406 0.1518 0.056 Uiso 0.541(2) 1 calc PR A 2 H18F H 1.2559 0.4312 0.1183 0.056 Uiso 0.541(2) 1 calc PR A 2 Cl' Cl 0.7906(5) 0.5315(5) 0.4287(3) 0.0351(5) Uani 0.541(2) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.01457(6) 0.01355(6) 0.01450(6) -0.00091(4) -0.00525(5) -0.00105(4) P 0.0328(2) 0.01481(17) 0.0338(2) 0.00143(15) -0.02055(18) -0.00414(15) Si1 0.0191(2) 0.0312(2) 0.0224(2) -0.00403(17) -0.01005(17) 0.00370(17) Si2 0.02037(19) 0.01928(19) 0.01646(18) -0.00080(15) -0.00785(15) -0.00285(15) Si3 0.01826(19) 0.01960(19) 0.01867(19) -0.00251(15) -0.00187(15) -0.00133(15) N1 0.0187(6) 0.0207(6) 0.0178(6) -0.0026(5) -0.0070(5) 0.0009(5) N2 0.0181(6) 0.0152(5) 0.0184(6) -0.0002(4) -0.0069(5) -0.0038(4) N3 0.0201(6) 0.0165(6) 0.0168(6) -0.0009(4) -0.0034(5) -0.0002(5) N4 0.0212(6) 0.0154(5) 0.0184(6) -0.0012(4) -0.0048(5) -0.0006(5) N5 0.0184(6) 0.0166(6) 0.0205(6) -0.0001(5) -0.0084(5) -0.0028(4) C1 0.0216(7) 0.0239(7) 0.0195(7) -0.0040(6) -0.0052(6) 0.0034(6) C2 0.0202(7) 0.0208(7) 0.0227(7) -0.0012(6) -0.0078(6) -0.0063(5) C3 0.0259(7) 0.0192(7) 0.0172(7) 0.0016(5) -0.0048(6) -0.0008(6) C4 0.0257(8) 0.0183(7) 0.0232(7) -0.0041(6) -0.0061(6) 0.0055(6) C5 0.0274(8) 0.0180(7) 0.0228(7) -0.0035(6) -0.0081(6) -0.0055(6) C6 0.0281(8) 0.0164(7) 0.0213(7) 0.0028(5) -0.0029(6) -0.0039(6) C7 0.0194(8) 0.0679(14) 0.0368(10) -0.0024(9) -0.0118(7) -0.0034(8) C8 0.0455(11) 0.0386(10) 0.0343(10) -0.0061(8) -0.0250(9) 0.0141(8) C9 0.0321(9) 0.0342(9) 0.0275(8) -0.0053(7) -0.0145(7) 0.0000(7) C10 0.0364(9) 0.0320(9) 0.0221(8) -0.0071(6) -0.0092(7) -0.0023(7) C11 0.0301(8) 0.0281(8) 0.0336(9) 0.0006(7) -0.0173(7) -0.0013(7) C12 0.0310(8) 0.0337(9) 0.0193(7) 0.0010(6) -0.0045(6) -0.0123(7) C13 0.0337(9) 0.0356(9) 0.0231(8) -0.0101(7) -0.0024(7) 0.0011(7) C14 0.0252(8) 0.0298(9) 0.0355(9) 0.0007(7) -0.0025(7) -0.0074(7) C15 0.0220(7) 0.0230(7) 0.0294(8) -0.0014(6) -0.0057(6) 0.0005(6) C16 0.0237(7) 0.0170(6) 0.0244(7) 0.0028(5) -0.0127(6) -0.0048(5) C17 0.0262(8) 0.0285(8) 0.0257(8) 0.0046(6) -0.0114(6) -0.0091(6) C19 0.0297(9) 0.0457(11) 0.0421(10) 0.0038(8) -0.0157(8) -0.0177(8) C20 0.0411(11) 0.0413(10) 0.0498(11) -0.0012(9) -0.0268(9) -0.0187(9) C21 0.0422(10) 0.0298(9) 0.0390(10) -0.0064(7) -0.0232(8) -0.0071(8) C22 0.0266(8) 0.0229(7) 0.0285(8) -0.0032(6) -0.0131(6) -0.0030(6) C23 0.0195(7) 0.0168(6) 0.0187(7) -0.0013(5) -0.0067(5) -0.0026(5) C24 0.0289(8) 0.0164(7) 0.0292(8) -0.0011(6) -0.0165(7) -0.0008(6) C25 0.0292(8) 0.0319(9) 0.0286(8) 0.0039(7) -0.0127(7) -0.0041(7) C26 0.0406(10) 0.0339(9) 0.0313(9) 0.0040(7) -0.0207(8) -0.0037(8) C27 0.0382(10) 0.0284(9) 0.0439(10) -0.0008(8) -0.0265(9) 0.0037(7) C28 0.0272(9) 0.0415(10) 0.0448(11) 0.0027(8) -0.0166(8) -0.0032(8) C29 0.0304(9) 0.0383(10) 0.0328(9) 0.0077(7) -0.0132(7) -0.0063(7) Cl 0.0282(9) 0.0541(13) 0.0235(9) 0.0003(7) -0.0066(6) -0.0098(8) C18 0.046(9) 0.040(5) 0.036(7) -0.012(5) -0.027(6) -0.001(5) C18' 0.025(4) 0.057(5) 0.035(7) 0.006(4) -0.009(3) -0.023(3) Cl' 0.0292(8) 0.0456(10) 0.0307(8) -0.0163(7) -0.0065(6) -0.0019(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr N1 2.0671(12) . ? Zr N3 2.0704(12) . ? Zr N2 2.0847(12) . ? Zr N5 2.2001(12) . ? Zr N4 2.5358(12) . ? P C23 1.7083(15) . ? P C24 1.8797(15) . ? Si1 N1 1.7369(13) . ? Si1 C7 1.8698(19) . ? Si1 C9 1.8702(17) . ? Si1 C8 1.8763(19) . ? Si2 N2 1.7394(12) . ? Si2 C12 1.8568(16) . ? Si2 C11 1.8732(17) . ? Si2 C10 1.8790(16) . ? Si3 N3 1.7392(13) . ? Si3 C15 1.8642(16) . ? Si3 C13 1.8688(17) . ? Si3 C14 1.8772(17) . ? N1 C1 1.4915(19) . ? N2 C2 1.4898(18) . ? N3 C3 1.4813(18) . ? N4 C5 1.4792(19) . ? N4 C4 1.4843(19) . ? N4 C6 1.4850(19) . ? N5 C23 1.3715(18) . ? N5 C16 1.4359(18) . ? C1 C4 1.520(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C5 1.516(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C6 1.526(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.398(2) . ? C16 C22 1.406(2) . ? C17 C19 1.392(2) . ? C17 C18' 1.518(15) . ? C17 Cl 1.731(6) . ? C19 C20 1.381(3) . ? C19 H19A 0.9500 . ? C20 C21 1.379(3) . ? C20 H20A 0.9500 . ? C21 C22 1.389(2) . ? C21 H21A 0.9500 . ? C22 C18 1.521(18) . ? C22 Cl' 1.735(5) . ? C23 H23A 0.9500 . ? C24 C29 1.527(2) . ? C24 C25 1.534(2) . ? C24 H24A 1.0000 . ? C25 C26 1.529(2) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.520(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.524(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.534(2) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C18' H18D 0.9800 . ? C18' H18E 0.9800 . ? C18' H18F 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 N1 Zr N3 110.39(5) . . ? N1 Zr N2 117.00(5) . . ? N3 Zr N2 108.62(5) . . ? N1 Zr N5 105.18(5) . . ? N3 Zr N5 109.02(5) . . ? N2 Zr N5 106.29(4) . . ? N1 Zr N4 72.54(4) . . ? N3 Zr N4 73.42(4) . . ? N2 Zr N4 73.78(4) . . ? N5 Zr N4 177.25(4) . . ? C23 P C24 99.17(7) . . ? N1 Si1 C7 111.52(7) . . ? N1 Si1 C9 109.62(7) . . ? C7 Si1 C9 110.76(9) . . ? N1 Si1 C8 111.51(8) . . ? C7 Si1 C8 105.82(10) . . ? C9 Si1 C8 107.50(8) . . ? N2 Si2 C12 110.05(7) . . ? N2 Si2 C11 110.05(7) . . ? C12 Si2 C11 111.13(8) . . ? N2 Si2 C10 110.94(7) . . ? C12 Si2 C10 106.26(8) . . ? C11 Si2 C10 108.36(8) . . ? N3 Si3 C15 108.34(7) . . ? N3 Si3 C13 111.45(7) . . ? C15 Si3 C13 112.85(8) . . ? N3 Si3 C14 112.45(7) . . ? C15 Si3 C14 106.45(8) . . ? C13 Si3 C14 105.22(8) . . ? C1 N1 Si1 115.01(9) . . ? C1 N1 Zr 111.24(9) . . ? Si1 N1 Zr 131.27(7) . . ? C2 N2 Si2 111.72(9) . . ? C2 N2 Zr 111.99(9) . . ? Si2 N2 Zr 135.64(7) . . ? C3 N3 Si3 116.36(9) . . ? C3 N3 Zr 113.47(9) . . ? Si3 N3 Zr 128.03(7) . . ? C5 N4 C4 111.93(11) . . ? C5 N4 C6 111.14(12) . . ? C4 N4 C6 113.04(11) . . ? C5 N4 Zr 106.22(8) . . ? C4 N4 Zr 107.24(9) . . ? C6 N4 Zr 106.83(8) . . ? C23 N5 C16 113.75(11) . . ? C23 N5 Zr 116.62(9) . . ? C16 N5 Zr 129.51(9) . . ? N1 C1 C4 107.59(12) . . ? N1 C1 H1A 110.2 . . ? C4 C1 H1A 110.2 . . ? N1 C1 H1B 110.2 . . ? C4 C1 H1B 110.2 . . ? H1A C1 H1B 108.5 . . ? N2 C2 C5 108.36(12) . . ? N2 C2 H2A 110.0 . . ? C5 C2 H2A 110.0 . . ? N2 C2 H2B 110.0 . . ? C5 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? N3 C3 C6 108.77(12) . . ? N3 C3 H3A 109.9 . . ? C6 C3 H3A 109.9 . . ? N3 C3 H3B 109.9 . . ? C6 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? N4 C4 C1 107.51(12) . . ? N4 C4 H4A 110.2 . . ? C1 C4 H4A 110.2 . . ? N4 C4 H4B 110.2 . . ? C1 C4 H4B 110.2 . . ? H4A C4 H4B 108.5 . . ? N4 C5 C2 108.19(11) . . ? N4 C5 H5A 110.1 . . ? C2 C5 H5A 110.1 . . ? N4 C5 H5B 110.1 . . ? C2 C5 H5B 110.1 . . ? H5A C5 H5B 108.4 . . ? N4 C6 C3 109.00(12) . . ? N4 C6 H6A 109.9 . . ? C3 C6 H6A 109.9 . . ? N4 C6 H6B 109.9 . . ? C3 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si1 C9 H9A 109.5 . . ? Si1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2 C10 H10A 109.5 . . ? Si2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si2 C11 H11A 109.5 . . ? Si2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si3 C13 H13A 109.5 . . ? Si3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si3 C14 H14A 109.5 . . ? Si3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si3 C15 H15A 109.5 . . ? Si3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C22 117.94(14) . . ? C17 C16 N5 121.07(13) . . ? C22 C16 N5 120.99(14) . . ? C19 C17 C16 120.64(16) . . ? C19 C17 C18' 118.9(6) . . ? C16 C17 C18' 120.4(6) . . ? C19 C17 Cl 119.2(2) . . ? C16 C17 Cl 120.1(2) . . ? C18' C17 Cl 2.0(8) . . ? C20 C19 C17 120.37(17) . . ? C20 C19 H19A 119.8 . . ? C17 C19 H19A 119.8 . . ? C21 C20 C19 119.96(16) . . ? C21 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C20 C21 C22 120.20(17) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C21 C22 C16 120.84(16) . . ? C21 C22 C18 118.8(8) . . ? C16 C22 C18 120.3(8) . . ? C21 C22 Cl' 119.5(2) . . ? C16 C22 Cl' 119.6(2) . . ? C18 C22 Cl' 2.1(11) . . ? N5 C23 P 128.80(11) . . ? N5 C23 H23A 115.6 . . ? P C23 H23A 115.6 . . ? C29 C24 C25 110.27(13) . . ? C29 C24 P 113.49(11) . . ? C25 C24 P 109.66(11) . . ? C29 C24 H24A 107.7 . . ? C25 C24 H24A 107.7 . . ? P C24 H24A 107.7 . . ? C26 C25 C24 112.01(14) . . ? C26 C25 H25A 109.2 . . ? C24 C25 H25A 109.2 . . ? C26 C25 H25B 109.2 . . ? C24 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? C27 C26 C25 110.95(15) . . ? C27 C26 H26A 109.4 . . ? C25 C26 H26A 109.4 . . ? C27 C26 H26B 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C26 C27 C28 110.82(15) . . ? C26 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C27 C28 C29 111.56(15) . . ? C27 C28 H28A 109.3 . . ? C29 C28 H28A 109.3 . . ? C27 C28 H28B 109.3 . . ? C29 C28 H28B 109.3 . . ? H28A C28 H28B 108.0 . . ? C24 C29 C28 111.57(15) . . ? C24 C29 H29A 109.3 . . ? C28 C29 H29A 109.3 . . ? C24 C29 H29B 109.3 . . ? C28 C29 H29B 109.3 . . ? H29A C29 H29B 108.0 . . ? C22 C18 H18A 109.5 . . ? C22 C18 H18B 109.5 . . ? C22 C18 H18C 109.5 . . ? C17 C18' H18D 109.5 . . ? C17 C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? C17 C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 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 C7 Si1 N1 C1 79.80(13) . . . . ? C9 Si1 N1 C1 -157.18(11) . . . . ? C8 Si1 N1 C1 -38.26(13) . . . . ? C7 Si1 N1 Zr -119.98(11) . . . . ? C9 Si1 N1 Zr 3.05(12) . . . . ? C8 Si1 N1 Zr 121.96(10) . . . . ? N3 Zr N1 C1 101.83(10) . . . . ? N2 Zr N1 C1 -23.04(11) . . . . ? N5 Zr N1 C1 -140.71(9) . . . . ? N4 Zr N1 C1 37.69(9) . . . . ? N3 Zr N1 Si1 -58.96(10) . . . . ? N2 Zr N1 Si1 176.17(8) . . . . ? N5 Zr N1 Si1 58.49(10) . . . . ? N4 Zr N1 Si1 -123.11(10) . . . . ? C12 Si2 N2 C2 -167.96(10) . . . . ? C11 Si2 N2 C2 69.25(11) . . . . ? C10 Si2 N2 C2 -50.66(12) . . . . ? C12 Si2 N2 Zr 1.74(12) . . . . ? C11 Si2 N2 Zr -121.05(10) . . . . ? C10 Si2 N2 Zr 119.04(10) . . . . ? N1 Zr N2 C2 92.28(10) . . . . ? N3 Zr N2 C2 -33.47(10) . . . . ? N5 Zr N2 C2 -150.64(9) . . . . ? N4 Zr N2 C2 32.22(9) . . . . ? N1 Zr N2 Si2 -77.40(10) . . . . ? N3 Zr N2 Si2 156.84(9) . . . . ? N5 Zr N2 Si2 39.67(10) . . . . ? N4 Zr N2 Si2 -137.47(10) . . . . ? C15 Si3 N3 C3 -161.02(11) . . . . ? C13 Si3 N3 C3 74.24(12) . . . . ? C14 Si3 N3 C3 -43.64(13) . . . . ? C15 Si3 N3 Zr 1.14(11) . . . . ? C13 Si3 N3 Zr -123.60(9) . . . . ? C14 Si3 N3 Zr 118.52(9) . . . . ? N1 Zr N3 C3 -29.93(11) . . . . ? N2 Zr N3 C3 99.60(10) . . . . ? N5 Zr N3 C3 -144.99(9) . . . . ? N4 Zr N3 C3 33.67(9) . . . . ? N1 Zr N3 Si3 167.49(8) . . . . ? N2 Zr N3 Si3 -62.99(9) . . . . ? N5 Zr N3 Si3 52.43(9) . . . . ? N4 Zr N3 Si3 -128.92(9) . . . . ? N1 Zr N4 C5 -127.51(10) . . . . ? N3 Zr N4 C5 114.15(10) . . . . ? N2 Zr N4 C5 -1.55(9) . . . . ? N5 Zr N4 C5 -93.4(9) . . . . ? N1 Zr N4 C4 -7.68(9) . . . . ? N3 Zr N4 C4 -126.02(10) . . . . ? N2 Zr N4 C4 118.29(10) . . . . ? N5 Zr N4 C4 26.5(9) . . . . ? N1 Zr N4 C6 113.78(10) . . . . ? N3 Zr N4 C6 -4.56(9) . . . . ? N2 Zr N4 C6 -120.25(10) . . . . ? N5 Zr N4 C6 147.9(8) . . . . ? N1 Zr N5 C23 144.51(10) . . . . ? N3 Zr N5 C23 -97.11(11) . . . . ? N2 Zr N5 C23 19.80(11) . . . . ? N4 Zr N5 C23 110.8(9) . . . . ? N1 Zr N5 C16 -31.11(13) . . . . ? N3 Zr N5 C16 87.27(13) . . . . ? N2 Zr N5 C16 -155.82(12) . . . . ? N4 Zr N5 C16 -64.8(9) . . . . ? Si1 N1 C1 C4 97.76(12) . . . . ? Zr N1 C1 C4 -66.41(13) . . . . ? Si2 N2 C2 C5 110.65(11) . . . . ? Zr N2 C2 C5 -61.61(13) . . . . ? Si3 N3 C3 C6 104.21(12) . . . . ? Zr N3 C3 C6 -60.54(14) . . . . ? C5 N4 C4 C1 93.64(14) . . . . ? C6 N4 C4 C1 -139.96(12) . . . . ? Zr N4 C4 C1 -22.48(13) . . . . ? N1 C1 C4 N4 54.97(15) . . . . ? C4 N4 C5 C2 -144.75(12) . . . . ? C6 N4 C5 C2 87.82(14) . . . . ? Zr N4 C5 C2 -28.02(13) . . . . ? N2 C2 C5 N4 57.41(15) . . . . ? C5 N4 C6 C3 -138.90(12) . . . . ? C4 N4 C6 C3 94.27(14) . . . . ? Zr N4 C6 C3 -23.44(13) . . . . ? N3 C3 C6 N4 52.53(16) . . . . ? C23 N5 C16 C17 -93.44(17) . . . . ? Zr N5 C16 C17 82.28(17) . . . . ? C23 N5 C16 C22 86.07(17) . . . . ? Zr N5 C16 C22 -98.21(15) . . . . ? C22 C16 C17 C19 2.3(2) . . . . ? N5 C16 C17 C19 -178.19(15) . . . . ? C22 C16 C17 C18' -178.7(8) . . . . ? N5 C16 C17 C18' 0.8(8) . . . . ? C22 C16 C17 Cl -176.4(2) . . . . ? N5 C16 C17 Cl 3.1(3) . . . . ? C16 C17 C19 C20 -1.8(3) . . . . ? C18' C17 C19 C20 179.1(8) . . . . ? Cl C17 C19 C20 176.9(2) . . . . ? C17 C19 C20 C21 0.3(3) . . . . ? C19 C20 C21 C22 0.7(3) . . . . ? C20 C21 C22 C16 -0.2(3) . . . . ? C20 C21 C22 C18 177.3(11) . . . . ? C20 C21 C22 Cl' 179.5(3) . . . . ? C17 C16 C22 C21 -1.3(2) . . . . ? N5 C16 C22 C21 179.21(14) . . . . ? C17 C16 C22 C18 -178.7(11) . . . . ? N5 C16 C22 C18 1.8(11) . . . . ? C17 C16 C22 Cl' 179.0(2) . . . . ? N5 C16 C22 Cl' -0.5(3) . . . . ? C16 N5 C23 P -0.04(19) . . . . ? Zr N5 C23 P -176.34(8) . . . . ? C24 P C23 N5 176.07(14) . . . . ? C23 P C24 C29 89.19(12) . . . . ? C23 P C24 C25 -147.00(11) . . . . ? C29 C24 C25 C26 -55.08(19) . . . . ? P C24 C25 C26 179.25(12) . . . . ? C24 C25 C26 C27 56.2(2) . . . . ? C25 C26 C27 C28 -56.0(2) . . . . ? C26 C27 C28 C29 55.9(2) . . . . ? C25 C24 C29 C28 54.38(19) . . . . ? P C24 C29 C28 177.85(12) . . . . ? C27 C28 C29 C24 -55.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.439 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.063 data_slg001_0m _database_code_depnum_ccdc_archive 'CCDC 900056' #TrackingRef '13735_web_deposit_cif_file_3_RoryWaterman_1346784222.SLG001_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H56 N5 P Si3 Zr' _chemical_formula_weight 753.31 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' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.2901(9) _cell_length_b 19.5468(16) _cell_length_c 18.9804(16) _cell_angle_alpha 90.00 _cell_angle_beta 105.4240(10) _cell_angle_gamma 90.00 _cell_volume 4037.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9632 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 27.45 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas not _exptl_crystal_density_diffrn 1.239 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 0.430 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9075 _exptl_absorpt_correction_T_max 0.9502 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 46730 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9248 _reflns_number_gt 7866 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+2.2336P] 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 9248 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0724 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr Zr 0.689552(13) 0.158489(8) 0.705344(8) 0.01895(5) Uani 1 1 d . . . P2 P 0.81745(4) 0.09406(2) 0.91379(2) 0.02064(9) Uani 1 1 d . . . Si3 Si 0.95494(4) 0.26215(2) 0.77510(2) 0.02272(10) Uani 1 1 d . . . Si1 Si 0.41033(4) 0.10563(3) 0.73411(3) 0.03204(12) Uani 1 1 d . . . Si2 Si 0.76998(5) 0.07589(3) 0.56125(3) 0.03309(12) Uani 1 1 d . . . C4 C 0.45215(18) 0.25781(11) 0.63777(11) 0.0373(4) Uani 1 1 d . . . H4A H 0.3905 0.2300 0.6048 0.045 Uiso 1 1 calc R . . H4B H 0.4273 0.3054 0.6308 0.045 Uiso 1 1 calc R . . N1 N 0.51624(13) 0.16629(7) 0.72498(8) 0.0266(3) Uani 1 1 d . . . N2 N 0.66862(13) 0.11922(8) 0.59854(7) 0.0258(3) Uani 1 1 d . . . N4 N 0.57382(14) 0.24797(8) 0.62299(8) 0.0287(3) Uani 1 1 d . . . C25 C 0.72824(15) 0.16200(8) 0.94216(9) 0.0223(3) Uani 1 1 d . . . N3 N 0.81400(13) 0.24191(7) 0.71606(7) 0.0234(3) Uani 1 1 d . . . C18 C 0.77176(14) 0.10541(8) 0.81525(8) 0.0196(3) Uani 1 1 d . . . C31 C 0.74575(15) 0.01627(8) 0.93825(8) 0.0223(3) Uani 1 1 d . . . C30 C 0.69447(17) 0.15560(9) 1.00728(9) 0.0295(4) Uani 1 1 d . . . H30A H 0.7114 0.1151 1.0338 0.035 Uiso 1 1 calc R . . C33 C 0.7716(2) -0.09316(9) 1.00017(10) 0.0359(4) Uani 1 1 d . . . H33A H 0.8233 -0.1268 1.0263 0.043 Uiso 1 1 calc R . . C2 C 0.55585(16) 0.14636(10) 0.54672(10) 0.0325(4) Uani 1 1 d . . . H2A H 0.4839 0.1311 0.5611 0.039 Uiso 1 1 calc R . . H2B H 0.5500 0.1293 0.4979 0.039 Uiso 1 1 calc R . . C32 C 0.82152(17) -0.03492(9) 0.97686(9) 0.0280(4) Uani 1 1 d . . . H32A H 0.9064 -0.0302 0.9872 0.034 Uiso 1 1 calc R . . C12 C 0.92791(17) 0.08408(11) 0.62336(11) 0.0357(4) Uani 1 1 d . . . H12A H 0.9483 0.1316 0.6316 0.054 Uiso 1 1 calc R . . H12B H 0.9857 0.0626 0.6014 0.054 Uiso 1 1 calc R . . H12C H 0.9311 0.0623 0.6691 0.054 Uiso 1 1 calc R . . N5 N 0.77160(12) 0.06325(7) 0.76295(7) 0.0208(3) Uani 1 1 d . . . C19 C 0.92902(16) -0.03000(8) 0.77392(9) 0.0260(3) Uani 1 1 d . . . C17 C 0.79666(16) -0.01128(8) 0.76856(10) 0.0254(3) Uani 1 1 d . . . H17A H 0.7441 -0.0337 0.7260 0.030 Uiso 1 1 calc R . . H17B H 0.7751 -0.0288 0.8113 0.030 Uiso 1 1 calc R . . C14 C 0.9381(2) 0.33841(10) 0.83153(11) 0.0415(5) Uani 1 1 d . . . H14A H 0.8801 0.3283 0.8590 0.062 Uiso 1 1 calc R . . H14B H 0.9094 0.3767 0.8000 0.062 Uiso 1 1 calc R . . H14C H 1.0162 0.3493 0.8645 0.062 Uiso 1 1 calc R . . C34 C 0.6463(2) -0.10113(10) 0.98464(11) 0.0372(5) Uani 1 1 d . . . H34A H 0.6132 -0.1400 1.0004 0.045 Uiso 1 1 calc R . . C13 C 1.06952(19) 0.28581(11) 0.72324(12) 0.0425(5) Uani 1 1 d . . . H13A H 1.0807 0.2479 0.6935 0.064 Uiso 1 1 calc R . . H13B H 1.1466 0.2971 0.7571 0.064 Uiso 1 1 calc R . . H13C H 1.0398 0.3246 0.6926 0.064 Uiso 1 1 calc R . . C20 C 0.95706(19) -0.07191(9) 0.72130(11) 0.0361(4) Uani 1 1 d . . . H20A H 0.8944 -0.0875 0.6822 0.043 Uiso 1 1 calc R . . C22 C 1.1722(2) -0.06822(10) 0.78477(12) 0.0414(5) Uani 1 1 d . . . H22A H 1.2530 -0.0811 0.7885 0.050 Uiso 1 1 calc R . . C36 C 0.61900(17) 0.00750(10) 0.92317(11) 0.0337(4) Uani 1 1 d . . . H36A H 0.5667 0.0413 0.8979 0.040 Uiso 1 1 calc R . . C26 C 0.7051(2) 0.22398(9) 0.90505(10) 0.0361(4) Uani 1 1 d . . . H26A H 0.7290 0.2301 0.8622 0.043 Uiso 1 1 calc R . . C6 C 0.64680(18) 0.31150(9) 0.64017(11) 0.0343(4) Uani 1 1 d . . . H6A H 0.6293 0.3340 0.6818 0.041 Uiso 1 1 calc R . . H6B H 0.6248 0.3425 0.5988 0.041 Uiso 1 1 calc R . . C29 C 0.63619(18) 0.20845(10) 1.03314(10) 0.0362(4) Uani 1 1 d . . . H29A H 0.6139 0.2029 1.0766 0.043 Uiso 1 1 calc R . . C3 C 0.78181(17) 0.29444(9) 0.65725(10) 0.0315(4) Uani 1 1 d . . . H3A H 0.8011 0.2773 0.6136 0.038 Uiso 1 1 calc R . . H3B H 0.8300 0.3354 0.6728 0.038 Uiso 1 1 calc R . . C35 C 0.57005(19) -0.05128(10) 0.94561(12) 0.0405(5) Uani 1 1 d . . . H35A H 0.4853 -0.0570 0.9342 0.049 Uiso 1 1 calc R . . C24 C 1.02438(17) -0.00754(9) 0.83199(10) 0.0293(4) Uani 1 1 d . . . H24A H 1.0070 0.0204 0.8677 0.035 Uiso 1 1 calc R . . C8 C 0.47439(18) 0.01796(10) 0.72923(13) 0.0419(5) Uani 1 1 d . . . H8A H 0.4956 0.0128 0.6838 0.063 Uiso 1 1 calc R . . H8B H 0.4140 -0.0156 0.7323 0.063 Uiso 1 1 calc R . . H8C H 0.5465 0.0118 0.7691 0.063 Uiso 1 1 calc R . . C9 C 0.3652(2) 0.12092(13) 0.82116(13) 0.0488(6) Uani 1 1 d . . . H9A H 0.3329 0.1664 0.8208 0.073 Uiso 1 1 calc R . . H9B H 0.4359 0.1159 0.8621 0.073 Uiso 1 1 calc R . . H9C H 0.3036 0.0883 0.8250 0.073 Uiso 1 1 calc R . . C21 C 1.0780(2) -0.09071(11) 0.72675(12) 0.0443(5) Uani 1 1 d . . . H21A H 1.0956 -0.1186 0.6911 0.053 Uiso 1 1 calc R . . C1 C 0.46531(18) 0.23660(10) 0.71619(11) 0.0355(4) Uani 1 1 d . . . H1A H 0.5201 0.2677 0.7494 0.043 Uiso 1 1 calc R . . H1B H 0.3860 0.2375 0.7269 0.043 Uiso 1 1 calc R . . C5 C 0.56070(18) 0.22396(11) 0.54693(10) 0.0350(4) Uani 1 1 d . . . H5A H 0.6299 0.2395 0.5299 0.042 Uiso 1 1 calc R . . H5B H 0.4860 0.2423 0.5146 0.042 Uiso 1 1 calc R . . C28 C 0.61092(19) 0.26905(11) 0.99538(11) 0.0400(5) Uani 1 1 d . . . H28A H 0.5705 0.3042 1.0125 0.048 Uiso 1 1 calc R . . C11 C 0.7249(2) -0.01647(13) 0.54331(15) 0.0605(7) Uani 1 1 d . . . H11A H 0.6437 -0.0191 0.5110 0.091 Uiso 1 1 calc R . . H11B H 0.7263 -0.0387 0.5886 0.091 Uiso 1 1 calc R . . H11C H 0.7819 -0.0387 0.5212 0.091 Uiso 1 1 calc R . . C10 C 0.7784(2) 0.11306(18) 0.47132(12) 0.0700(9) Uani 1 1 d . . . H10A H 0.8002 0.1606 0.4777 0.105 Uiso 1 1 calc R . . H10B H 0.6998 0.1086 0.4363 0.105 Uiso 1 1 calc R . . H10C H 0.8393 0.0890 0.4541 0.105 Uiso 1 1 calc R . . C23 C 1.14525(18) -0.02626(10) 0.83740(11) 0.0361(4) Uani 1 1 d . . . H23A H 1.2081 -0.0106 0.8764 0.043 Uiso 1 1 calc R . . C27 C 0.6468(2) 0.27688(11) 0.93140(11) 0.0465(5) Uani 1 1 d . . . H27A H 0.6316 0.3180 0.9059 0.056 Uiso 1 1 calc R . . C7 C 0.26600(19) 0.11058(14) 0.65780(14) 0.0542(6) Uani 1 1 d . . . H7A H 0.2851 0.1033 0.6120 0.081 Uiso 1 1 calc R . . H7B H 0.2293 0.1549 0.6578 0.081 Uiso 1 1 calc R . . H7C H 0.2095 0.0760 0.6645 0.081 Uiso 1 1 calc R . . C15 C 1.02782(17) 0.19218(11) 0.83764(12) 0.0396(5) Uani 1 1 d . . . H15A H 0.9734 0.1778 0.8660 0.059 Uiso 1 1 calc R . . H15B H 1.1034 0.2083 0.8698 0.059 Uiso 1 1 calc R . . H15C H 1.0445 0.1543 0.8096 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.01902(8) 0.01957(8) 0.01781(8) 0.00115(6) 0.00413(5) -0.00007(6) P2 0.0222(2) 0.02087(19) 0.01968(19) 0.00304(15) 0.00696(15) -0.00142(15) Si3 0.0234(2) 0.0236(2) 0.0214(2) 0.00377(17) 0.00629(17) -0.00300(17) Si1 0.0205(2) 0.0389(3) 0.0384(3) 0.0024(2) 0.0108(2) 0.0010(2) Si2 0.0272(2) 0.0489(3) 0.0231(2) -0.0072(2) 0.00653(19) 0.0005(2) C4 0.0301(10) 0.0374(10) 0.0427(11) 0.0093(8) 0.0066(8) 0.0118(8) N1 0.0230(7) 0.0288(8) 0.0287(7) 0.0023(6) 0.0082(6) 0.0051(6) N2 0.0227(7) 0.0316(8) 0.0208(7) -0.0013(6) 0.0018(5) -0.0011(6) N4 0.0284(7) 0.0296(8) 0.0261(7) 0.0059(6) 0.0036(6) 0.0047(6) C25 0.0237(8) 0.0230(8) 0.0201(7) -0.0016(6) 0.0059(6) -0.0031(6) N3 0.0287(7) 0.0207(7) 0.0194(7) 0.0040(5) 0.0039(5) -0.0029(5) C18 0.0176(7) 0.0213(8) 0.0208(7) 0.0017(6) 0.0065(6) -0.0018(6) C31 0.0273(8) 0.0211(8) 0.0202(7) 0.0012(6) 0.0094(6) -0.0024(6) C30 0.0372(10) 0.0301(9) 0.0229(8) 0.0004(7) 0.0109(7) -0.0051(7) C33 0.0554(12) 0.0239(9) 0.0271(9) 0.0062(7) 0.0084(8) -0.0006(8) C2 0.0257(9) 0.0436(11) 0.0232(8) -0.0029(7) -0.0021(7) -0.0006(8) C32 0.0318(9) 0.0260(9) 0.0251(8) 0.0038(7) 0.0056(7) 0.0003(7) C12 0.0274(9) 0.0443(11) 0.0357(10) 0.0006(8) 0.0090(8) -0.0003(8) N5 0.0203(6) 0.0194(7) 0.0231(7) 0.0001(5) 0.0065(5) -0.0015(5) C19 0.0346(9) 0.0165(7) 0.0300(9) 0.0034(6) 0.0139(7) 0.0015(7) C17 0.0306(9) 0.0175(8) 0.0289(8) -0.0007(6) 0.0094(7) -0.0024(6) C14 0.0455(12) 0.0393(11) 0.0367(11) -0.0116(9) 0.0058(9) -0.0062(9) C34 0.0578(13) 0.0261(9) 0.0356(10) -0.0030(7) 0.0265(9) -0.0134(9) C13 0.0402(11) 0.0465(12) 0.0464(12) 0.0097(9) 0.0212(9) -0.0086(9) C20 0.0469(11) 0.0266(9) 0.0373(10) -0.0040(8) 0.0158(9) 0.0034(8) C22 0.0397(11) 0.0337(10) 0.0590(13) 0.0090(9) 0.0272(10) 0.0107(9) C36 0.0282(9) 0.0299(9) 0.0438(11) 0.0032(8) 0.0111(8) -0.0004(7) C26 0.0573(12) 0.0281(9) 0.0266(9) 0.0017(7) 0.0178(9) 0.0055(9) C6 0.0429(11) 0.0242(9) 0.0327(10) 0.0098(7) 0.0049(8) 0.0036(8) C29 0.0416(11) 0.0432(11) 0.0296(9) -0.0106(8) 0.0195(8) -0.0085(9) C3 0.0388(10) 0.0279(9) 0.0248(9) 0.0082(7) 0.0029(7) -0.0059(7) C35 0.0354(10) 0.0356(11) 0.0567(13) -0.0027(9) 0.0231(9) -0.0099(8) C24 0.0337(9) 0.0247(8) 0.0320(9) 0.0021(7) 0.0131(7) 0.0044(7) C8 0.0305(10) 0.0360(11) 0.0614(14) -0.0037(9) 0.0160(9) -0.0080(8) C9 0.0438(12) 0.0569(14) 0.0571(14) 0.0151(11) 0.0332(11) 0.0126(10) C21 0.0576(14) 0.0329(10) 0.0519(13) -0.0036(9) 0.0313(11) 0.0110(10) C1 0.0320(10) 0.0346(10) 0.0425(11) 0.0042(8) 0.0146(8) 0.0100(8) C5 0.0315(9) 0.0465(11) 0.0220(8) 0.0083(8) -0.0017(7) 0.0039(8) C28 0.0420(11) 0.0407(11) 0.0381(11) -0.0130(9) 0.0123(9) 0.0070(9) C11 0.0513(14) 0.0593(15) 0.0633(16) -0.0348(13) 0.0022(12) 0.0003(12) C10 0.0484(14) 0.135(3) 0.0301(12) 0.0144(14) 0.0170(10) 0.0167(16) C23 0.0328(10) 0.0323(10) 0.0448(11) 0.0053(8) 0.0127(8) 0.0046(8) C27 0.0740(16) 0.0309(10) 0.0348(11) 0.0017(8) 0.0151(10) 0.0166(10) C7 0.0242(10) 0.0703(16) 0.0629(15) 0.0013(12) 0.0024(10) -0.0030(10) C15 0.0221(9) 0.0418(11) 0.0511(12) 0.0209(9) 0.0034(8) -0.0031(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr N1 2.0925(14) . ? Zr N2 2.1213(14) . ? Zr N3 2.1265(14) . ? Zr N5 2.2317(13) . ? Zr C18 2.2934(15) . ? Zr N4 2.4745(14) . ? P2 C18 1.8166(16) . ? P2 C25 1.8320(17) . ? P2 C31 1.8392(16) . ? Si3 N3 1.7309(14) . ? Si3 C15 1.8539(19) . ? Si3 C14 1.874(2) . ? Si3 C13 1.8798(19) . ? Si1 N1 1.7250(15) . ? Si1 C8 1.872(2) . ? Si1 C7 1.873(2) . ? Si1 C9 1.878(2) . ? Si2 N2 1.7200(15) . ? Si2 C12 1.8646(19) . ? Si2 C10 1.880(2) . ? Si2 C11 1.882(2) . ? C4 N4 1.486(2) . ? C4 C1 1.514(3) . ? N1 C1 1.482(2) . ? N2 C2 1.485(2) . ? N4 C6 1.478(2) . ? N4 C5 1.487(2) . ? C25 C26 1.391(2) . ? C25 C30 1.393(2) . ? N3 C3 1.489(2) . ? C18 N5 1.290(2) . ? C31 C32 1.392(2) . ? C31 C36 1.393(2) . ? C30 C29 1.383(3) . ? C33 C34 1.375(3) . ? C33 C32 1.394(2) . ? C2 C5 1.518(3) . ? N5 C17 1.482(2) . ? C19 C24 1.391(3) . ? C19 C20 1.392(2) . ? C19 C17 1.515(2) . ? C34 C35 1.379(3) . ? C20 C21 1.391(3) . ? C22 C21 1.384(3) . ? C22 C23 1.388(3) . ? C36 C35 1.390(3) . ? C26 C27 1.389(3) . ? C6 C3 1.509(3) . ? C29 C28 1.374(3) . ? C24 C23 1.390(3) . ? C28 C27 1.387(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zr N2 108.95(6) . . ? N1 Zr N3 123.53(6) . . ? N2 Zr N3 105.77(5) . . ? N1 Zr N5 105.04(5) . . ? N2 Zr N5 95.31(5) . . ? N3 Zr N5 114.53(5) . . ? N1 Zr C18 92.43(5) . . ? N2 Zr C18 128.38(6) . . ? N3 Zr C18 99.36(5) . . ? N5 Zr C18 33.09(5) . . ? N1 Zr N4 72.50(5) . . ? N2 Zr N4 75.30(5) . . ? N3 Zr N4 75.10(5) . . ? N5 Zr N4 168.44(5) . . ? C18 Zr N4 155.82(5) . . ? C18 P2 C25 100.74(7) . . ? C18 P2 C31 109.71(7) . . ? C25 P2 C31 102.22(7) . . ? N3 Si3 C15 114.89(8) . . ? N3 Si3 C14 109.64(9) . . ? C15 Si3 C14 108.43(10) . . ? N3 Si3 C13 111.06(9) . . ? C15 Si3 C13 105.47(10) . . ? C14 Si3 C13 106.98(10) . . ? N1 Si1 C8 109.69(8) . . ? N1 Si1 C7 111.75(10) . . ? C8 Si1 C7 106.10(11) . . ? N1 Si1 C9 109.68(10) . . ? C8 Si1 C9 112.83(10) . . ? C7 Si1 C9 106.75(11) . . ? N2 Si2 C12 109.06(8) . . ? N2 Si2 C10 112.51(10) . . ? C12 Si2 C10 105.68(11) . . ? N2 Si2 C11 111.68(10) . . ? C12 Si2 C11 111.33(11) . . ? C10 Si2 C11 106.43(14) . . ? N4 C4 C1 107.23(15) . . ? C1 N1 Si1 112.96(12) . . ? C1 N1 Zr 113.62(11) . . ? Si1 N1 Zr 132.36(8) . . ? C2 N2 Si2 116.78(11) . . ? C2 N2 Zr 111.21(11) . . ? Si2 N2 Zr 130.86(8) . . ? C6 N4 C4 109.79(15) . . ? C6 N4 C5 112.65(15) . . ? C4 N4 C5 111.45(15) . . ? C6 N4 Zr 106.55(10) . . ? C4 N4 Zr 109.37(10) . . ? C5 N4 Zr 106.83(11) . . ? C26 C25 C30 117.96(16) . . ? C26 C25 P2 121.76(13) . . ? C30 C25 P2 119.83(13) . . ? C3 N3 Si3 109.07(11) . . ? C3 N3 Zr 115.71(10) . . ? Si3 N3 Zr 135.03(7) . . ? N5 C18 P2 131.01(12) . . ? N5 C18 Zr 70.83(9) . . ? P2 C18 Zr 157.99(9) . . ? C32 C31 C36 118.26(16) . . ? C32 C31 P2 118.50(13) . . ? C36 C31 P2 123.16(13) . . ? C29 C30 C25 121.08(17) . . ? C34 C33 C32 120.29(18) . . ? N2 C2 C5 109.36(14) . . ? C31 C32 C33 120.71(17) . . ? C18 N5 C17 127.69(14) . . ? C18 N5 Zr 76.08(9) . . ? C17 N5 Zr 154.34(11) . . ? C24 C19 C20 118.58(17) . . ? C24 C19 C17 121.24(15) . . ? C20 C19 C17 120.15(17) . . ? N5 C17 C19 114.07(13) . . ? C33 C34 C35 119.68(17) . . ? C21 C20 C19 120.55(19) . . ? C21 C22 C23 119.41(19) . . ? C35 C36 C31 120.61(18) . . ? C27 C26 C25 120.62(17) . . ? N4 C6 C3 109.49(15) . . ? C28 C29 C30 120.73(17) . . ? N3 C3 C6 110.16(14) . . ? C34 C35 C36 120.43(19) . . ? C23 C24 C19 120.88(17) . . ? C22 C21 C20 120.47(18) . . ? N1 C1 C4 107.36(15) . . ? N4 C5 C2 108.19(14) . . ? C29 C28 C27 118.90(18) . . ? C22 C23 C24 120.11(19) . . ? C28 C27 C26 120.67(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8 Si1 N1 C1 170.66(13) . . . . ? C7 Si1 N1 C1 53.28(16) . . . . ? C9 Si1 N1 C1 -64.89(15) . . . . ? C8 Si1 N1 Zr 3.40(15) . . . . ? C7 Si1 N1 Zr -113.97(13) . . . . ? C9 Si1 N1 Zr 127.85(12) . . . . ? N2 Zr N1 C1 -100.41(13) . . . . ? N3 Zr N1 C1 24.49(14) . . . . ? N5 Zr N1 C1 158.43(12) . . . . ? C18 Zr N1 C1 127.40(12) . . . . ? N4 Zr N1 C1 -33.34(12) . . . . ? N2 Zr N1 Si1 66.78(12) . . . . ? N3 Zr N1 Si1 -168.32(9) . . . . ? N5 Zr N1 Si1 -34.38(12) . . . . ? C18 Zr N1 Si1 -65.41(11) . . . . ? N4 Zr N1 Si1 133.85(12) . . . . ? C12 Si2 N2 C2 152.51(13) . . . . ? C10 Si2 N2 C2 35.59(17) . . . . ? C11 Si2 N2 C2 -84.02(16) . . . . ? C12 Si2 N2 Zr -13.98(14) . . . . ? C10 Si2 N2 Zr -130.90(14) . . . . ? C11 Si2 N2 Zr 109.49(13) . . . . ? N1 Zr N2 C2 37.09(13) . . . . ? N3 Zr N2 C2 -97.65(12) . . . . ? N5 Zr N2 C2 145.00(12) . . . . ? C18 Zr N2 C2 146.30(11) . . . . ? N4 Zr N2 C2 -28.15(11) . . . . ? N1 Zr N2 Si2 -155.84(10) . . . . ? N3 Zr N2 Si2 69.42(11) . . . . ? N5 Zr N2 Si2 -47.93(11) . . . . ? C18 Zr N2 Si2 -46.63(13) . . . . ? N4 Zr N2 Si2 138.92(12) . . . . ? C1 C4 N4 C6 -90.62(18) . . . . ? C1 C4 N4 C5 143.85(16) . . . . ? C1 C4 N4 Zr 25.95(18) . . . . ? N1 Zr N4 C6 121.52(12) . . . . ? N2 Zr N4 C6 -122.71(12) . . . . ? N3 Zr N4 C6 -11.58(11) . . . . ? N5 Zr N4 C6 -159.1(2) . . . . ? C18 Zr N4 C6 67.95(18) . . . . ? N1 Zr N4 C4 2.91(12) . . . . ? N2 Zr N4 C4 118.68(13) . . . . ? N3 Zr N4 C4 -130.19(13) . . . . ? N5 Zr N4 C4 82.3(3) . . . . ? C18 Zr N4 C4 -50.66(19) . . . . ? N1 Zr N4 C5 -117.85(12) . . . . ? N2 Zr N4 C5 -2.08(11) . . . . ? N3 Zr N4 C5 109.05(12) . . . . ? N5 Zr N4 C5 -38.4(3) . . . . ? C18 Zr N4 C5 -171.42(12) . . . . ? C18 P2 C25 C26 -34.37(16) . . . . ? C31 P2 C25 C26 -147.47(15) . . . . ? C18 P2 C25 C30 153.42(14) . . . . ? C31 P2 C25 C30 40.32(15) . . . . ? C15 Si3 N3 C3 -165.38(13) . . . . ? C14 Si3 N3 C3 72.23(14) . . . . ? C13 Si3 N3 C3 -45.78(14) . . . . ? C15 Si3 N3 Zr 9.23(15) . . . . ? C14 Si3 N3 Zr -113.16(12) . . . . ? C13 Si3 N3 Zr 128.83(12) . . . . ? N1 Zr N3 C3 -73.79(13) . . . . ? N2 Zr N3 C3 52.51(13) . . . . ? N5 Zr N3 C3 156.08(11) . . . . ? C18 Zr N3 C3 -173.03(12) . . . . ? N4 Zr N3 C3 -17.12(12) . . . . ? N1 Zr N3 Si3 111.87(11) . . . . ? N2 Zr N3 Si3 -121.83(11) . . . . ? N5 Zr N3 Si3 -18.27(13) . . . . ? C18 Zr N3 Si3 12.62(12) . . . . ? N4 Zr N3 Si3 168.53(12) . . . . ? C25 P2 C18 N5 -156.29(15) . . . . ? C31 P2 C18 N5 -49.02(17) . . . . ? C25 P2 C18 Zr 15.7(2) . . . . ? C31 P2 C18 Zr 123.0(2) . . . . ? N1 Zr C18 N5 114.25(9) . . . . ? N2 Zr C18 N5 -2.38(12) . . . . ? N3 Zr C18 N5 -121.18(9) . . . . ? N4 Zr C18 N5 164.43(11) . . . . ? N1 Zr C18 P2 -59.4(2) . . . . ? N2 Zr C18 P2 -176.0(2) . . . . ? N3 Zr C18 P2 65.2(2) . . . . ? N5 Zr C18 P2 -173.6(3) . . . . ? N4 Zr C18 P2 -9.2(3) . . . . ? C18 P2 C31 C32 121.76(13) . . . . ? C25 P2 C31 C32 -131.97(13) . . . . ? C18 P2 C31 C36 -61.52(16) . . . . ? C25 P2 C31 C36 44.75(16) . . . . ? C26 C25 C30 C29 2.0(3) . . . . ? P2 C25 C30 C29 174.51(14) . . . . ? Si2 N2 C2 C5 -112.06(15) . . . . ? Zr N2 C2 C5 57.01(17) . . . . ? C36 C31 C32 C33 -0.4(3) . . . . ? P2 C31 C32 C33 176.46(14) . . . . ? C34 C33 C32 C31 0.6(3) . . . . ? P2 C18 N5 C17 7.7(2) . . . . ? Zr C18 N5 C17 -169.13(16) . . . . ? P2 C18 N5 Zr 176.84(14) . . . . ? N1 Zr N5 C18 -70.61(10) . . . . ? N2 Zr N5 C18 178.13(9) . . . . ? N3 Zr N5 C18 68.11(10) . . . . ? N4 Zr N5 C18 -146.7(2) . . . . ? N1 Zr N5 C17 89.2(2) . . . . ? N2 Zr N5 C17 -22.0(2) . . . . ? N3 Zr N5 C17 -132.0(2) . . . . ? C18 Zr N5 C17 159.8(3) . . . . ? N4 Zr N5 C17 13.1(4) . . . . ? C18 N5 C17 C19 -94.26(19) . . . . ? Zr N5 C17 C19 110.7(2) . . . . ? C24 C19 C17 N5 61.5(2) . . . . ? C20 C19 C17 N5 -120.22(17) . . . . ? C32 C33 C34 C35 0.2(3) . . . . ? C24 C19 C20 C21 -0.1(3) . . . . ? C17 C19 C20 C21 -178.43(17) . . . . ? C32 C31 C36 C35 -0.6(3) . . . . ? P2 C31 C36 C35 -177.36(15) . . . . ? C30 C25 C26 C27 -1.9(3) . . . . ? P2 C25 C26 C27 -174.24(17) . . . . ? C4 N4 C6 C3 155.46(15) . . . . ? C5 N4 C6 C3 -79.70(18) . . . . ? Zr N4 C6 C3 37.13(16) . . . . ? C25 C30 C29 C28 -0.5(3) . . . . ? Si3 N3 C3 C6 -139.85(13) . . . . ? Zr N3 C3 C6 44.37(18) . . . . ? N4 C6 C3 N3 -54.13(19) . . . . ? C33 C34 C35 C36 -1.3(3) . . . . ? C31 C36 C35 C34 1.5(3) . . . . ? C20 C19 C24 C23 0.2(3) . . . . ? C17 C19 C24 C23 178.48(16) . . . . ? C23 C22 C21 C20 -0.4(3) . . . . ? C19 C20 C21 C22 0.3(3) . . . . ? Si1 N1 C1 C4 -108.66(15) . . . . ? Zr N1 C1 C4 61.09(17) . . . . ? N4 C4 C1 N1 -53.8(2) . . . . ? C6 N4 C5 C2 147.28(15) . . . . ? C4 N4 C5 C2 -88.79(17) . . . . ? Zr N4 C5 C2 30.63(16) . . . . ? N2 C2 C5 N4 -57.61(19) . . . . ? C30 C29 C28 C27 -1.1(3) . . . . ? C21 C22 C23 C24 0.5(3) . . . . ? C19 C24 C23 C22 -0.4(3) . . . . ? C29 C28 C27 C26 1.2(3) . . . . ? C25 C26 C27 C28 0.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.359 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.051 data_rw1163p _database_code_depnum_ccdc_archive 'CCDC 900057' #TrackingRef '13736_web_deposit_cif_file_4_RoryWaterman_1346784222.RW1163P.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H32 N P' _chemical_formula_sum 'C35 H32 N P' _chemical_formula_weight 497.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall -P2ybc 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 9.3521(9) _cell_length_b 9.9508(9) _cell_length_c 29.528(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.9060(10) _cell_angle_gamma 90.00 _cell_volume 2737.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9927 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 30.54 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 0.124 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9636 _exptl_absorpt_correction_T_max 0.9816 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 42804 _diffrn_reflns_av_R_equivalents 0.0703 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 30.57 _reflns_number_total 8388 _reflns_number_gt 5690 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0767P)^2^+0.3064P] 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 8388 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0897 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1486 _refine_ls_wR_factor_gt 0.1294 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 P P 0.25209(4) 0.48759(4) 0.166758(13) 0.02055(11) Uani 1 1 d . . . N N 0.13034(15) 0.25600(14) 0.13503(5) 0.0261(3) Uani 1 1 d . . . C1 C 0.16885(16) 0.66217(15) 0.15358(5) 0.0192(3) Uani 1 1 d . . . C2 C 0.03169(16) 0.67505(16) 0.17916(5) 0.0207(3) Uani 1 1 d . . . C3 C -0.05353(17) 0.78965(17) 0.17197(6) 0.0268(3) Uani 1 1 d . . . H3A H -0.0309 0.8539 0.1499 0.032 Uiso 1 1 calc R . . C4 C -0.17162(18) 0.81044(19) 0.19693(6) 0.0311(4) Uani 1 1 d . . . H4A H -0.2291 0.8884 0.1915 0.037 Uiso 1 1 calc R . . C5 C -0.20593(18) 0.71837(19) 0.22956(6) 0.0322(4) Uani 1 1 d . . . H5A H -0.2861 0.7333 0.2466 0.039 Uiso 1 1 calc R . . C6 C -0.12259(18) 0.60502(19) 0.23704(6) 0.0295(4) Uani 1 1 d . . . H6A H -0.1457 0.5413 0.2592 0.035 Uiso 1 1 calc R . . C7 C -0.00457(17) 0.58346(17) 0.21218(5) 0.0251(3) Uani 1 1 d . . . H7A H 0.0523 0.5051 0.2178 0.030 Uiso 1 1 calc R . . C8 C 0.27221(15) 0.76943(16) 0.17576(5) 0.0214(3) Uani 1 1 d . . . C9 C 0.28940(18) 0.89426(17) 0.15567(6) 0.0276(3) Uani 1 1 d . . . H9A H 0.2413 0.9128 0.1267 0.033 Uiso 1 1 calc R . . C10 C 0.37653(19) 0.99260(18) 0.17761(7) 0.0336(4) Uani 1 1 d . . . H10A H 0.3879 1.0772 0.1634 0.040 Uiso 1 1 calc R . . C11 C 0.44646(19) 0.96701(19) 0.22003(6) 0.0334(4) Uani 1 1 d . . . H11A H 0.5085 1.0326 0.2345 0.040 Uiso 1 1 calc R . . C12 C 0.42533(18) 0.84535(19) 0.24117(6) 0.0307(4) Uani 1 1 d . . . H12A H 0.4705 0.8284 0.2707 0.037 Uiso 1 1 calc R . . C13 C 0.33822(17) 0.74809(17) 0.21933(5) 0.0252(3) Uani 1 1 d . . . H13A H 0.3233 0.6655 0.2343 0.030 Uiso 1 1 calc R . . C14 C 0.14107(16) 0.67677(15) 0.10195(5) 0.0207(3) Uani 1 1 d . . . C15 C 0.25309(18) 0.70964(17) 0.07493(5) 0.0250(3) Uani 1 1 d . . . H15A H 0.3461 0.7281 0.0891 0.030 Uiso 1 1 calc R . . C16 C 0.2295(2) 0.71538(18) 0.02784(6) 0.0314(4) Uani 1 1 d . . . H16A H 0.3058 0.7404 0.0103 0.038 Uiso 1 1 calc R . . C17 C 0.0964(2) 0.68509(18) 0.00620(6) 0.0335(4) Uani 1 1 d . . . H17A H 0.0814 0.6877 -0.0260 0.040 Uiso 1 1 calc R . . C18 C -0.0148(2) 0.65087(17) 0.03203(6) 0.0304(4) Uani 1 1 d . . . H18A H -0.1064 0.6291 0.0175 0.037 Uiso 1 1 calc R . . C19 C 0.00737(18) 0.64830(16) 0.07940(5) 0.0247(3) Uani 1 1 d . . . H19A H -0.0706 0.6266 0.0967 0.030 Uiso 1 1 calc R . . C20 C 0.39722(17) 0.47798(16) 0.12934(5) 0.0228(3) Uani 1 1 d . . . C21 C 0.38622(19) 0.41956(18) 0.08614(6) 0.0303(4) Uani 1 1 d . . . H21A H 0.2978 0.3813 0.0743 0.036 Uiso 1 1 calc R . . C22 C 0.5043(2) 0.4172(2) 0.06044(7) 0.0389(5) Uani 1 1 d . . . H22A H 0.4964 0.3763 0.0313 0.047 Uiso 1 1 calc R . . C23 C 0.6331(2) 0.4741(2) 0.07722(7) 0.0425(5) Uani 1 1 d . . . H23A H 0.7131 0.4731 0.0594 0.051 Uiso 1 1 calc R . . C24 C 0.64525(19) 0.5324(2) 0.11988(7) 0.0368(4) Uani 1 1 d . . . H24A H 0.7335 0.5720 0.1313 0.044 Uiso 1 1 calc R . . C25 C 0.52867(17) 0.53314(18) 0.14610(6) 0.0287(4) Uani 1 1 d . . . H25A H 0.5384 0.5715 0.1757 0.034 Uiso 1 1 calc R . . C26 C 0.11154(17) 0.38128(16) 0.13844(5) 0.0224(3) Uani 1 1 d . . . H26A H 0.0240 0.4206 0.1263 0.027 Uiso 1 1 calc R . . C27 C 0.01381(18) 0.17432(16) 0.11672(5) 0.0242(3) Uani 1 1 d . . . C28 C -0.11909(18) 0.17111(17) 0.13582(6) 0.0269(3) Uani 1 1 d . . . C29 C -0.1488(2) 0.24989(19) 0.17789(6) 0.0333(4) Uani 1 1 d . . . H29A H -0.2236 0.2044 0.1934 0.050 Uiso 1 1 calc R . . H29B H -0.1811 0.3406 0.1691 0.050 Uiso 1 1 calc R . . H29C H -0.0609 0.2557 0.1984 0.050 Uiso 1 1 calc R . . C30 C -0.22561(19) 0.08622(18) 0.11609(6) 0.0311(4) Uani 1 1 d . . . H30A H -0.3166 0.0853 0.1282 0.037 Uiso 1 1 calc R . . C31 C -0.2042(2) 0.00291(19) 0.07950(6) 0.0329(4) Uani 1 1 d . . . C32 C -0.3224(2) -0.0902(2) 0.06016(8) 0.0477(5) Uani 1 1 d . . . H32A H -0.3967 -0.0970 0.0816 0.071 Uiso 1 1 calc R . . H32B H -0.2823 -0.1795 0.0553 0.071 Uiso 1 1 calc R . . H32C H -0.3647 -0.0543 0.0311 0.071 Uiso 1 1 calc R . . C33 C -0.0705(2) 0.00591(17) 0.06222(6) 0.0304(4) Uani 1 1 d . . . H33A H -0.0535 -0.0512 0.0375 0.036 Uiso 1 1 calc R . . C34 C 0.03922(18) 0.09002(16) 0.08011(6) 0.0255(3) Uani 1 1 d . . . C35 C 0.18071(19) 0.09532(18) 0.05917(6) 0.0304(4) Uani 1 1 d . . . H35A H 0.1969 0.0098 0.0439 0.046 Uiso 1 1 calc R . . H35B H 0.2584 0.1110 0.0830 0.046 Uiso 1 1 calc R . . H35C H 0.1787 0.1686 0.0369 0.046 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 P 0.01998(19) 0.0241(2) 0.01841(19) 0.00018(15) 0.00631(14) 0.00147(15) N 0.0295(7) 0.0259(7) 0.0234(7) -0.0012(5) 0.0047(6) 0.0000(6) C1 0.0182(7) 0.0233(7) 0.0165(7) -0.0004(5) 0.0043(5) 0.0005(6) C2 0.0183(7) 0.0266(8) 0.0180(7) -0.0032(6) 0.0059(5) -0.0015(6) C3 0.0249(8) 0.0305(9) 0.0263(8) -0.0013(7) 0.0094(6) 0.0018(7) C4 0.0263(8) 0.0338(9) 0.0342(9) -0.0034(7) 0.0093(7) 0.0068(7) C5 0.0238(8) 0.0435(10) 0.0313(9) -0.0069(8) 0.0136(7) -0.0004(7) C6 0.0263(8) 0.0381(10) 0.0260(8) 0.0002(7) 0.0126(7) -0.0037(7) C7 0.0233(7) 0.0297(9) 0.0232(8) -0.0007(6) 0.0076(6) 0.0021(6) C8 0.0168(7) 0.0265(8) 0.0217(7) -0.0037(6) 0.0068(6) 0.0007(6) C9 0.0286(8) 0.0290(9) 0.0255(8) -0.0002(7) 0.0049(7) -0.0032(7) C10 0.0345(9) 0.0288(9) 0.0387(10) -0.0039(8) 0.0089(8) -0.0080(7) C11 0.0247(8) 0.0369(10) 0.0390(10) -0.0155(8) 0.0045(7) -0.0052(7) C12 0.0247(8) 0.0399(10) 0.0273(8) -0.0106(7) 0.0005(7) 0.0053(7) C13 0.0240(8) 0.0294(9) 0.0223(8) -0.0036(6) 0.0038(6) 0.0044(6) C14 0.0241(7) 0.0202(7) 0.0184(7) 0.0004(6) 0.0063(6) 0.0019(6) C15 0.0279(8) 0.0268(8) 0.0216(7) 0.0018(6) 0.0093(6) 0.0035(6) C16 0.0435(10) 0.0295(9) 0.0235(8) 0.0020(7) 0.0168(7) 0.0071(8) C17 0.0526(12) 0.0314(9) 0.0170(7) -0.0016(7) 0.0060(7) 0.0111(8) C18 0.0395(10) 0.0276(9) 0.0233(8) -0.0024(7) -0.0024(7) 0.0037(7) C19 0.0291(8) 0.0239(8) 0.0215(7) -0.0006(6) 0.0043(6) -0.0002(6) C20 0.0233(7) 0.0231(8) 0.0232(7) 0.0010(6) 0.0084(6) 0.0033(6) C21 0.0312(9) 0.0325(9) 0.0288(9) -0.0068(7) 0.0124(7) -0.0024(7) C22 0.0418(11) 0.0421(11) 0.0362(10) -0.0132(8) 0.0223(8) -0.0026(9) C23 0.0340(10) 0.0512(12) 0.0461(11) -0.0058(9) 0.0260(9) 0.0010(9) C24 0.0228(8) 0.0499(12) 0.0393(10) -0.0026(9) 0.0115(7) -0.0025(8) C25 0.0235(8) 0.0362(10) 0.0273(8) -0.0013(7) 0.0077(6) 0.0019(7) C26 0.0219(7) 0.0264(8) 0.0198(7) 0.0031(6) 0.0063(6) 0.0013(6) C27 0.0290(8) 0.0212(8) 0.0227(7) 0.0027(6) 0.0037(6) 0.0006(6) C28 0.0309(9) 0.0239(8) 0.0266(8) 0.0042(6) 0.0070(7) 0.0023(7) C29 0.0341(9) 0.0367(10) 0.0311(9) -0.0021(8) 0.0141(7) -0.0022(8) C30 0.0307(9) 0.0309(9) 0.0328(9) 0.0049(7) 0.0090(7) -0.0008(7) C31 0.0366(10) 0.0298(9) 0.0322(9) 0.0021(7) 0.0028(7) -0.0060(7) C32 0.0457(12) 0.0479(13) 0.0497(13) -0.0087(10) 0.0059(10) -0.0158(10) C33 0.0407(10) 0.0255(8) 0.0252(8) -0.0007(7) 0.0041(7) -0.0033(7) C34 0.0309(8) 0.0218(8) 0.0245(8) 0.0027(6) 0.0063(6) 0.0018(6) C35 0.0362(9) 0.0274(9) 0.0288(9) -0.0012(7) 0.0102(7) 0.0005(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P C20 1.8245(16) . ? P C26 1.8324(17) . ? P C1 1.9297(16) . ? N C26 1.264(2) . ? N C27 1.428(2) . ? C1 C14 1.531(2) . ? C1 C8 1.547(2) . ? C1 C2 1.549(2) . ? C2 C3 1.397(2) . ? C2 C7 1.398(2) . ? C3 C4 1.395(2) . ? C3 H3A 0.9500 . ? C4 C5 1.387(3) . ? C4 H4A 0.9500 . ? C5 C6 1.378(3) . ? C5 H5A 0.9500 . ? C6 C7 1.393(2) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.392(2) . ? C8 C13 1.395(2) . ? C9 C10 1.397(2) . ? C9 H9A 0.9500 . ? C10 C11 1.386(3) . ? C10 H10A 0.9500 . ? C11 C12 1.384(3) . ? C11 H11A 0.9500 . ? C12 C13 1.388(2) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C19 1.394(2) . ? C14 C15 1.409(2) . ? C15 C16 1.390(2) . ? C15 H15A 0.9500 . ? C16 C17 1.383(3) . ? C16 H16A 0.9500 . ? C17 C18 1.383(3) . ? C17 H17A 0.9500 . ? C18 C19 1.397(2) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C21 1.397(2) . ? C20 C25 1.398(2) . ? C21 C22 1.393(2) . ? C21 H21A 0.9500 . ? C22 C23 1.384(3) . ? C22 H22A 0.9500 . ? C23 C24 1.383(3) . ? C23 H23A 0.9500 . ? C24 C25 1.390(2) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C34 1.405(2) . ? C27 C28 1.408(2) . ? C28 C30 1.395(2) . ? C28 C29 1.514(2) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.390(3) . ? C30 H30A 0.9500 . ? C31 C33 1.390(3) . ? C31 C32 1.517(3) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.393(2) . ? C33 H33A 0.9500 . ? C34 C35 1.509(2) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 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 C20 P C26 103.60(7) . . ? C20 P C1 103.48(7) . . ? C26 P C1 99.58(7) . . ? C26 N C27 118.99(14) . . ? C14 C1 C8 113.74(12) . . ? C14 C1 C2 113.62(12) . . ? C8 C1 C2 104.47(11) . . ? C14 C1 P 108.51(10) . . ? C8 C1 P 108.00(10) . . ? C2 C1 P 108.23(10) . . ? C3 C2 C7 117.97(14) . . ? C3 C2 C1 118.62(13) . . ? C7 C2 C1 123.15(14) . . ? C4 C3 C2 120.53(16) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? C5 C4 C3 120.66(16) . . ? C5 C4 H4A 119.7 . . ? C3 C4 H4A 119.7 . . ? C6 C5 C4 119.38(15) . . ? C6 C5 H5A 120.3 . . ? C4 C5 H5A 120.3 . . ? C5 C6 C7 120.29(16) . . ? C5 C6 H6A 119.9 . . ? C7 C6 H6A 119.9 . . ? C6 C7 C2 121.17(15) . . ? C6 C7 H7A 119.4 . . ? C2 C7 H7A 119.4 . . ? C9 C8 C13 118.09(15) . . ? C9 C8 C1 121.73(14) . . ? C13 C8 C1 119.78(14) . . ? C8 C9 C10 120.77(16) . . ? C8 C9 H9A 119.6 . . ? C10 C9 H9A 119.6 . . ? C11 C10 C9 120.13(17) . . ? C11 C10 H10A 119.9 . . ? C9 C10 H10A 119.9 . . ? C12 C11 C10 119.58(16) . . ? C12 C11 H11A 120.2 . . ? C10 C11 H11A 120.2 . . ? C11 C12 C13 120.08(16) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C12 C13 C8 121.22(16) . . ? C12 C13 H13A 119.4 . . ? C8 C13 H13A 119.4 . . ? C19 C14 C15 117.18(14) . . ? C19 C14 C1 121.66(13) . . ? C15 C14 C1 120.98(14) . . ? C16 C15 C14 120.93(16) . . ? C16 C15 H15A 119.5 . . ? C14 C15 H15A 119.5 . . ? C17 C16 C15 120.83(16) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C16 C17 C18 119.22(15) . . ? C16 C17 H17A 120.4 . . ? C18 C17 H17A 120.4 . . ? C17 C18 C19 120.17(17) . . ? C17 C18 H18A 119.9 . . ? C19 C18 H18A 119.9 . . ? C14 C19 C18 121.64(16) . . ? C14 C19 H19A 119.2 . . ? C18 C19 H19A 119.2 . . ? C21 C20 C25 118.71(15) . . ? C21 C20 P 125.03(13) . . ? C25 C20 P 116.26(12) . . ? C22 C21 C20 120.30(17) . . ? C22 C21 H21A 119.9 . . ? C20 C21 H21A 119.9 . . ? C23 C22 C21 120.29(17) . . ? C23 C22 H22A 119.9 . . ? C21 C22 H22A 119.9 . . ? C24 C23 C22 119.93(16) . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C23 C24 C25 120.17(17) . . ? C23 C24 H24A 119.9 . . ? C25 C24 H24A 119.9 . . ? C24 C25 C20 120.58(16) . . ? C24 C25 H25A 119.7 . . ? C20 C25 H25A 119.7 . . ? N C26 P 120.43(13) . . ? N C26 H26A 119.8 . . ? P C26 H26A 119.8 . . ? C34 C27 C28 120.52(15) . . ? C34 C27 N 117.22(14) . . ? C28 C27 N 122.15(14) . . ? C30 C28 C27 118.01(15) . . ? C30 C28 C29 118.78(15) . . ? C27 C28 C29 123.15(15) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C28 122.71(16) . . ? C31 C30 H30A 118.6 . . ? C28 C30 H30A 118.6 . . ? C30 C31 C33 117.80(16) . . ? C30 C31 C32 120.54(17) . . ? C33 C31 C32 121.64(17) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 C34 122.03(16) . . ? C31 C33 H33A 119.0 . . ? C34 C33 H33A 119.0 . . ? C33 C34 C27 118.88(15) . . ? C33 C34 C35 120.62(15) . . ? C27 C34 C35 120.44(15) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.57 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.710 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.065