Electronic Supplementary Material for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_author_name R.Waterman _publ_contact_author_name 'Rory Waterman' _publ_contact_author_email RORY.WATERMAN@UVM.EDU data_rw537as_0t _database_code_depnum_ccdc_archive 'CCDC 668519' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H52 As4' _chemical_formula_weight 868.53 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2517(18) _cell_length_b 12.4234(19) _cell_length_c 14.266(2) _cell_angle_alpha 90.180(2) _cell_angle_beta 96.133(2) _cell_angle_gamma 116.656(2) _cell_volume 1926.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 2059 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 29.65 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 3.469 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5586 _exptl_absorpt_correction_T_max 0.7230 _exptl_absorpt_process_details twinabs _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 23292 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0792 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 30.08 _reflns_number_total 10292 _reflns_number_gt 8531 _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. Using CELL_NOW, the crystal that was determined to contain two domains. Both domains were integrated with SAINT using the two-component orientation matrix produced by CELL_NOW. The data was scaled and absorption corrected with TWINABS. The initial solution was refined with single component data for the stronger domain before final refinement with HKLF 5 format data of both twin domains as produced by TWINABS. R(sigma) 0.0908; calculated by XPREP for the HKLF 4 data BASF 0.0583(3) From Cell_Now: Rotated froim first domain by 179.9 degrees about reciprocal axis 0 1 0 and real axis 0.459 1.000 0.045 SHELXL TWIN matrix -1.000 0.000 0.001 0.919 1.000 0.090 -0.001 0.001 -1.000 ; _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^)+(0.0617P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14569 _refine_ls_number_parameters 436 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0858 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.1068 _refine_ls_wR_factor_gt 0.0934 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 As1 As -0.05710(4) 0.92483(4) 0.36118(3) 0.01791(10) Uani 1 1 d . . . As2 As 0.06088(4) 0.85162(4) 0.27071(3) 0.01701(10) Uani 1 1 d . . . As3 As -0.00857(4) 0.93183(4) 0.12968(3) 0.01659(10) Uani 1 1 d . . . As4 As -0.19646(4) 0.84109(4) 0.21113(3) 0.01666(10) Uani 1 1 d . . . C11 C -0.1393(4) 0.7880(4) 0.4411(3) 0.0196(9) Uani 1 1 d . . . C12 C -0.0736(4) 0.7366(4) 0.4955(3) 0.0213(9) Uani 1 1 d . . . C13 C 0.0650(4) 0.7867(5) 0.5001(3) 0.0328(11) Uani 1 1 d . . . H13A H 0.0975 0.7671 0.5599 0.049 Uiso 1 1 calc R . . H13B H 0.1020 0.8745 0.4962 0.049 Uiso 1 1 calc R . . H13C H 0.0849 0.7510 0.4473 0.049 Uiso 1 1 calc R . . C14 C -0.1356(4) 0.6399(4) 0.5487(3) 0.0264(10) Uani 1 1 d . . . H14A H -0.0907 0.6046 0.5836 0.032 Uiso 1 1 calc R . . C15 C -0.2613(4) 0.5924(4) 0.5531(3) 0.0238(9) Uani 1 1 d . . . C16 C -0.3277(5) 0.4852(5) 0.6101(4) 0.0412(13) Uani 1 1 d . . . H16A H -0.4053 0.4830 0.6238 0.062 Uiso 1 1 calc R . . H16B H -0.2761 0.4920 0.6694 0.062 Uiso 1 1 calc R . . H16C H -0.3447 0.4110 0.5740 0.062 Uiso 1 1 calc R . . C17 C -0.3232(4) 0.6494(4) 0.5055(3) 0.0227(9) Uani 1 1 d . . . H17A H -0.4083 0.6210 0.5104 0.027 Uiso 1 1 calc R . . C18 C -0.2650(4) 0.7473(4) 0.4505(3) 0.0202(9) Uani 1 1 d . . . C19 C -0.3388(4) 0.8083(4) 0.4072(3) 0.0293(10) Uani 1 1 d . . . H19A H -0.2852 0.8950 0.4058 0.044 Uiso 1 1 calc R . . H19B H -0.4055 0.7953 0.4450 0.044 Uiso 1 1 calc R . . H19C H -0.3737 0.7742 0.3427 0.044 Uiso 1 1 calc R . . C21 C 0.2364(4) 0.9660(4) 0.3103(3) 0.0177(8) Uani 1 1 d . . . C22 C 0.2865(4) 1.0926(4) 0.3186(3) 0.0198(9) Uani 1 1 d . . . C23 C 0.2120(4) 1.1605(4) 0.2942(3) 0.0242(9) Uani 1 1 d . . . H23A H 0.1638 1.1303 0.2322 0.036 Uiso 1 1 calc R . . H23B H 0.2676 1.2467 0.2927 0.036 Uiso 1 1 calc R . . H23C H 0.1564 1.1485 0.3420 0.036 Uiso 1 1 calc R . . C24 C 0.4109(4) 1.1605(4) 0.3509(3) 0.0231(9) Uani 1 1 d . . . H24A H 0.4436 1.2458 0.3570 0.028 Uiso 1 1 calc R . . C25 C 0.4890(4) 1.1088(4) 0.3747(3) 0.0241(9) Uani 1 1 d . . . C26 C 0.6239(4) 1.1840(5) 0.4076(3) 0.0355(12) Uani 1 1 d . . . H26A H 0.6535 1.1378 0.4494 0.053 Uiso 1 1 calc R . . H26B H 0.6359 1.2577 0.4419 0.053 Uiso 1 1 calc R . . H26C H 0.6699 1.2055 0.3528 0.053 Uiso 1 1 calc R . . C27 C 0.4388(4) 0.9841(4) 0.3640(3) 0.0243(9) Uani 1 1 d . . . H27A H 0.4909 0.9469 0.3787 0.029 Uiso 1 1 calc R . . C28 C 0.3145(4) 0.9109(4) 0.3324(3) 0.0219(9) Uani 1 1 d . . . C29 C 0.2730(4) 0.7769(4) 0.3215(3) 0.0281(10) Uani 1 1 d . . . H29A H 0.2122 0.7429 0.2655 0.042 Uiso 1 1 calc R . . H29B H 0.2359 0.7385 0.3776 0.042 Uiso 1 1 calc R . . H29C H 0.3440 0.7623 0.3144 0.042 Uiso 1 1 calc R . . C31 C -0.0442(4) 0.7982(4) 0.0359(3) 0.0176(8) Uani 1 1 d . . . C32 C 0.0460(4) 0.7602(4) 0.0243(3) 0.0190(8) Uani 1 1 d . . . C33 C 0.1775(4) 0.8275(4) 0.0699(3) 0.0242(9) Uani 1 1 d . . . H33A H 0.1912 0.9054 0.0978 0.036 Uiso 1 1 calc R . . H33B H 0.2334 0.8409 0.0221 0.036 Uiso 1 1 calc R . . H33C H 0.1931 0.7799 0.1193 0.036 Uiso 1 1 calc R . . C34 C 0.0163(4) 0.6608(4) -0.0371(3) 0.0214(9) Uani 1 1 d . . . H34A H 0.0758 0.6324 -0.0419 0.026 Uiso 1 1 calc R . . C35 C -0.0970(4) 0.6023(4) -0.0912(3) 0.0209(9) Uani 1 1 d . . . C36 C -0.1276(4) 0.4946(4) -0.1570(3) 0.0311(11) Uani 1 1 d . . . H36A H -0.0801 0.4525 -0.1330 0.047 Uiso 1 1 calc R . . H36B H -0.1070 0.5217 -0.2200 0.047 Uiso 1 1 calc R . . H36C H -0.2157 0.4395 -0.1607 0.047 Uiso 1 1 calc R . . C37 C -0.1795(4) 0.6505(4) -0.0870(3) 0.0207(9) Uani 1 1 d . . . H37A H -0.2548 0.6161 -0.1278 0.025 Uiso 1 1 calc R . . C38 C -0.1555(4) 0.7473(4) -0.0249(3) 0.0182(8) Uani 1 1 d . . . C39 C -0.2506(4) 0.7935(4) -0.0254(3) 0.0236(9) Uani 1 1 d . . . H39A H -0.2983 0.7763 -0.0880 0.035 Uiso 1 1 calc R . . H39B H -0.2093 0.8807 -0.0104 0.035 Uiso 1 1 calc R . . H39C H -0.3059 0.7533 0.0220 0.035 Uiso 1 1 calc R . . C41 C -0.2796(4) 0.9454(4) 0.1855(3) 0.0179(8) Uani 1 1 d . . . C42 C -0.2226(4) 1.0726(4) 0.1926(3) 0.0184(8) Uani 1 1 d . . . C43 C -0.0867(4) 1.1490(4) 0.2236(3) 0.0225(9) Uani 1 1 d . . . H43A H -0.0692 1.2339 0.2309 0.034 Uiso 1 1 calc R . . H43B H -0.0391 1.1398 0.1760 0.034 Uiso 1 1 calc R . . H43C H -0.0638 1.1229 0.2841 0.034 Uiso 1 1 calc R . . C44 C -0.2934(4) 1.1338(4) 0.1711(3) 0.0213(9) Uani 1 1 d . . . H44A H -0.2542 1.2195 0.1758 0.026 Uiso 1 1 calc R . . C45 C -0.4195(4) 1.0728(4) 0.1428(3) 0.0239(9) Uani 1 1 d . . . C46 C -0.4948(4) 1.1401(4) 0.1206(3) 0.0317(11) Uani 1 1 d . . . H46A H -0.5687 1.1047 0.1530 0.048 Uiso 1 1 calc R . . H46B H -0.5188 1.1340 0.0523 0.048 Uiso 1 1 calc R . . H46C H -0.4457 1.2251 0.1421 0.048 Uiso 1 1 calc R . . C47 C -0.4741(4) 0.9478(4) 0.1369(3) 0.0227(9) Uani 1 1 d . . . H47A H -0.5602 0.9048 0.1182 0.027 Uiso 1 1 calc R . . C48 C -0.4073(4) 0.8826(4) 0.1573(3) 0.0199(9) Uani 1 1 d . . . C49 C -0.4798(4) 0.7462(4) 0.1480(3) 0.0271(10) Uani 1 1 d . . . H49A H -0.4231 0.7103 0.1585 0.041 Uiso 1 1 calc R . . H49B H -0.5248 0.7212 0.0844 0.041 Uiso 1 1 calc R . . H49C H -0.5381 0.7191 0.1949 0.041 Uiso 1 1 calc R . . C1S C 0.8776(5) 0.4962(5) 0.3121(4) 0.0449(14) Uani 1 1 d . . . H1SA H 0.8678 0.5071 0.3782 0.067 Uiso 1 1 calc R . . H1SB H 0.9518 0.5650 0.2957 0.067 Uiso 1 1 calc R . . H1SC H 0.8853 0.4217 0.3032 0.067 Uiso 1 1 calc R . . C2S C 0.7667(4) 0.4881(4) 0.2492(3) 0.0310(11) Uani 1 1 d . . . C3S C 0.6619(5) 0.4762(4) 0.2854(4) 0.0392(13) Uani 1 1 d . . . H3SA H 0.6599 0.4749 0.3518 0.047 Uiso 1 1 calc R . . C4S C 0.5602(5) 0.4661(5) 0.2268(4) 0.0449(14) Uani 1 1 d . . . H4SA H 0.4888 0.4573 0.2531 0.054 Uiso 1 1 calc R . . C5S C 0.5614(5) 0.4688(4) 0.1310(4) 0.0393(12) Uani 1 1 d . . . H5SA H 0.4910 0.4616 0.0910 0.047 Uiso 1 1 calc R . . C6S C 0.6651(5) 0.4821(4) 0.0931(4) 0.0398(13) Uani 1 1 d . . . H6SA H 0.6667 0.4846 0.0267 0.048 Uiso 1 1 calc R . . C7S C 0.7665(5) 0.4917(4) 0.1513(4) 0.0376(12) Uani 1 1 d . . . H7SA H 0.8377 0.5009 0.1244 0.045 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 As1 0.0189(2) 0.0229(2) 0.0141(2) 0.00124(16) 0.00203(16) 0.01133(18) As2 0.0175(2) 0.0206(2) 0.0143(2) 0.00039(16) 0.00091(16) 0.01008(18) As3 0.0167(2) 0.0202(2) 0.0139(2) 0.00093(16) 0.00170(16) 0.00925(17) As4 0.0167(2) 0.0200(2) 0.0150(2) 0.00167(16) 0.00204(16) 0.00974(17) C11 0.022(2) 0.023(2) 0.015(2) 0.0002(16) 0.0030(16) 0.0116(18) C12 0.023(2) 0.032(2) 0.014(2) -0.0011(17) 0.0014(17) 0.018(2) C13 0.032(3) 0.054(3) 0.021(2) 0.009(2) 0.003(2) 0.027(2) C14 0.039(3) 0.036(3) 0.015(2) 0.0031(18) 0.0007(19) 0.027(2) C15 0.034(3) 0.024(2) 0.015(2) 0.0019(17) 0.0031(18) 0.015(2) C16 0.046(3) 0.038(3) 0.041(3) 0.017(2) 0.009(3) 0.020(3) C17 0.024(2) 0.027(2) 0.017(2) 0.0006(17) 0.0016(17) 0.0110(19) C18 0.025(2) 0.026(2) 0.0111(19) 0.0005(16) 0.0002(16) 0.0131(19) C19 0.025(2) 0.044(3) 0.028(2) 0.016(2) 0.0081(19) 0.023(2) C21 0.020(2) 0.026(2) 0.0105(19) -0.0006(16) 0.0006(15) 0.0138(18) C22 0.022(2) 0.028(2) 0.0116(19) 0.0007(16) 0.0026(16) 0.0126(19) C23 0.020(2) 0.024(2) 0.027(2) -0.0016(18) -0.0012(18) 0.0097(19) C24 0.023(2) 0.026(2) 0.016(2) -0.0020(17) 0.0029(17) 0.0067(19) C25 0.018(2) 0.038(3) 0.014(2) 0.0021(18) 0.0023(17) 0.011(2) C26 0.022(2) 0.051(3) 0.030(3) 0.001(2) -0.001(2) 0.014(2) C27 0.022(2) 0.038(3) 0.019(2) 0.0024(19) 0.0021(17) 0.019(2) C28 0.024(2) 0.033(2) 0.0115(19) -0.0005(17) 0.0008(17) 0.016(2) C29 0.029(3) 0.035(3) 0.027(2) 0.001(2) 0.000(2) 0.021(2) C31 0.021(2) 0.021(2) 0.0127(19) 0.0024(16) 0.0025(16) 0.0112(18) C32 0.018(2) 0.024(2) 0.016(2) 0.0023(16) 0.0026(16) 0.0105(18) C33 0.018(2) 0.037(3) 0.020(2) -0.0051(19) -0.0036(17) 0.016(2) C34 0.026(2) 0.027(2) 0.017(2) 0.0024(17) 0.0025(17) 0.018(2) C35 0.025(2) 0.023(2) 0.014(2) 0.0023(16) 0.0027(17) 0.0098(19) C36 0.034(3) 0.032(3) 0.028(2) -0.005(2) -0.001(2) 0.016(2) C37 0.017(2) 0.026(2) 0.014(2) 0.0020(17) -0.0016(16) 0.0055(18) C38 0.020(2) 0.024(2) 0.0138(19) 0.0044(16) 0.0038(16) 0.0117(18) C39 0.022(2) 0.035(3) 0.018(2) 0.0005(18) -0.0009(17) 0.017(2) C41 0.020(2) 0.027(2) 0.0124(19) 0.0038(16) 0.0026(16) 0.0150(18) C42 0.021(2) 0.025(2) 0.0114(18) 0.0016(16) 0.0029(16) 0.0125(18) C43 0.022(2) 0.016(2) 0.029(2) 0.0020(17) -0.0007(18) 0.0096(18) C44 0.030(2) 0.023(2) 0.016(2) 0.0034(17) 0.0042(17) 0.0161(19) C45 0.027(2) 0.037(3) 0.017(2) 0.0042(19) 0.0082(18) 0.021(2) C46 0.036(3) 0.043(3) 0.029(3) 0.003(2) 0.003(2) 0.030(2) C47 0.018(2) 0.035(3) 0.019(2) 0.0006(18) 0.0012(17) 0.016(2) C48 0.021(2) 0.029(2) 0.0131(19) 0.0015(17) 0.0049(16) 0.0142(19) C49 0.019(2) 0.028(2) 0.031(2) 0.000(2) 0.0014(19) 0.0087(19) C1S 0.043(3) 0.040(3) 0.046(3) -0.005(3) 0.000(3) 0.015(3) C2S 0.036(3) 0.025(2) 0.033(3) -0.002(2) 0.007(2) 0.013(2) C3S 0.054(3) 0.039(3) 0.031(3) 0.003(2) 0.020(3) 0.024(3) C4S 0.045(3) 0.043(3) 0.060(4) 0.011(3) 0.026(3) 0.027(3) C5S 0.037(3) 0.032(3) 0.051(3) 0.013(2) 0.008(3) 0.017(2) C6S 0.044(3) 0.033(3) 0.033(3) 0.007(2) 0.012(2) 0.008(2) C7S 0.036(3) 0.033(3) 0.042(3) 0.001(2) 0.018(2) 0.011(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 C11 1.981(4) . ? As1 As2 2.4805(6) . ? As1 As4 2.4881(6) . ? As2 C21 1.989(4) . ? As2 As3 2.4844(6) . ? As3 C31 1.986(4) . ? As3 As4 2.4842(6) . ? As4 C41 1.990(4) . ? C11 C12 1.410(5) . ? C11 C18 1.411(6) . ? C12 C14 1.381(6) . ? C12 C13 1.516(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.389(6) . ? C14 H14A 0.9500 . ? C15 C17 1.384(6) . ? C15 C16 1.507(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.396(6) . ? C17 H17A 0.9500 . ? C18 C19 1.508(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 C22 1.408(6) . ? C21 C28 1.416(5) . ? C22 C24 1.393(6) . ? C22 C23 1.514(5) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.389(6) . ? C24 H24A 0.9500 . ? C25 C27 1.387(6) . ? C25 C26 1.506(6) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.399(6) . ? C27 H27A 0.9500 . ? C28 C29 1.509(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C31 C32 1.407(5) . ? C31 C38 1.408(5) . ? C32 C34 1.394(5) . ? C32 C33 1.511(5) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.383(6) . ? C34 H34A 0.9500 . ? C35 C37 1.392(6) . ? C35 C36 1.510(6) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.392(6) . ? C37 H37A 0.9500 . ? C38 C39 1.512(5) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C41 C42 1.410(6) . ? C41 C48 1.410(5) . ? C42 C44 1.401(5) . ? C42 C43 1.514(5) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.392(6) . ? C44 H44A 0.9500 . ? C45 C47 1.386(6) . ? C45 C46 1.510(5) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.399(5) . ? C47 H47A 0.9500 . ? C48 C49 1.516(6) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C1S C2S 1.509(7) . ? C1S H1SA 0.9800 . ? C1S H1SB 0.9800 . ? C1S H1SC 0.9800 . ? C2S C3S 1.382(6) . ? C2S C7S 1.397(7) . ? C3S C4S 1.381(7) . ? C3S H3SA 0.9500 . ? C4S C5S 1.368(7) . ? C4S H4SA 0.9500 . ? C5S C6S 1.377(7) . ? C5S H5SA 0.9500 . ? C6S C7S 1.376(7) . ? C6S H6SA 0.9500 . ? C7S H7SA 0.9500 . ? 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 C11 As1 As2 101.82(12) . . ? C11 As1 As4 98.81(12) . . ? As2 As1 As4 77.81(2) . . ? C21 As2 As1 104.79(11) . . ? C21 As2 As3 107.06(11) . . ? As1 As2 As3 86.82(2) . . ? C31 As3 As4 100.36(12) . . ? C31 As3 As2 98.72(11) . . ? As4 As3 As2 77.81(2) . . ? C41 As4 As3 105.38(12) . . ? C41 As4 As1 106.42(11) . . ? As3 As4 As1 86.66(2) . . ? C12 C11 C18 118.6(4) . . ? C12 C11 As1 121.9(3) . . ? C18 C11 As1 119.2(3) . . ? C14 C12 C11 119.6(4) . . ? C14 C12 C13 118.4(4) . . ? C11 C12 C13 122.0(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 C15 122.4(4) . . ? C12 C14 H14A 118.8 . . ? C15 C14 H14A 118.8 . . ? C17 C15 C14 117.5(4) . . ? C17 C15 C16 120.9(4) . . ? C14 C15 C16 121.6(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 C18 122.3(4) . . ? C15 C17 H17A 118.9 . . ? C18 C17 H17A 118.9 . . ? C17 C18 C11 119.1(4) . . ? C17 C18 C19 117.9(4) . . ? C11 C18 C19 122.9(4) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C21 C28 119.2(4) . . ? C22 C21 As2 126.0(3) . . ? C28 C21 As2 114.9(3) . . ? C24 C22 C21 119.2(4) . . ? C24 C22 C23 117.4(4) . . ? C21 C22 C23 123.4(4) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C22 122.8(4) . . ? C25 C24 H24A 118.6 . . ? C22 C24 H24A 118.6 . . ? C27 C25 C24 117.2(4) . . ? C27 C25 C26 120.8(4) . . ? C24 C25 C26 121.9(4) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 C28 122.6(4) . . ? C25 C27 H27A 118.7 . . ? C28 C27 H27A 118.7 . . ? C27 C28 C21 118.9(4) . . ? C27 C28 C29 117.0(4) . . ? C21 C28 C29 124.0(4) . . ? 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 . . ? C32 C31 C38 119.1(4) . . ? C32 C31 As3 120.1(3) . . ? C38 C31 As3 120.6(3) . . ? C34 C32 C31 119.2(4) . . ? C34 C32 C33 117.7(4) . . ? C31 C32 C33 123.0(4) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C32 122.2(4) . . ? C35 C34 H34A 118.9 . . ? C32 C34 H34A 118.9 . . ? C34 C35 C37 117.6(4) . . ? C34 C35 C36 121.4(4) . . ? C37 C35 C36 120.9(4) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C35 122.2(4) . . ? C38 C37 H37A 118.9 . . ? C35 C37 H37A 118.9 . . ? C37 C38 C31 119.0(4) . . ? C37 C38 C39 118.5(4) . . ? C31 C38 C39 122.5(4) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C42 C41 C48 119.0(4) . . ? C42 C41 As4 126.2(3) . . ? C48 C41 As4 114.8(3) . . ? C44 C42 C41 119.6(4) . . ? C44 C42 C43 116.9(4) . . ? C41 C42 C43 123.4(3) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C42 121.9(4) . . ? C45 C44 H44A 119.0 . . ? C42 C44 H44A 119.0 . . ? C47 C45 C44 117.6(4) . . ? C47 C45 C46 121.0(4) . . ? C44 C45 C46 121.3(4) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 C48 122.6(4) . . ? C45 C47 H47A 118.7 . . ? C48 C47 H47A 118.7 . . ? C47 C48 C41 119.2(4) . . ? C47 C48 C49 116.6(4) . . ? C41 C48 C49 124.2(4) . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C2S C1S H1SA 109.5 . . ? C2S C1S H1SB 109.5 . . ? H1SA C1S H1SB 109.5 . . ? C2S C1S H1SC 109.5 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? C3S C2S C7S 117.5(5) . . ? C3S C2S C1S 121.8(5) . . ? C7S C2S C1S 120.7(5) . . ? C4S C3S C2S 121.1(5) . . ? C4S C3S H3SA 119.4 . . ? C2S C3S H3SA 119.4 . . ? C5S C4S C3S 120.5(5) . . ? C5S C4S H4SA 119.7 . . ? C3S C4S H4SA 119.7 . . ? C4S C5S C6S 119.6(5) . . ? C4S C5S H5SA 120.2 . . ? C6S C5S H5SA 120.2 . . ? C7S C6S C5S 120.0(5) . . ? C7S C6S H6SA 120.0 . . ? C5S C6S H6SA 120.0 . . ? C6S C7S C2S 121.2(5) . . ? C6S C7S H7SA 119.4 . . ? C2S C7S H7SA 119.4 . . ? 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 C11 As1 As2 C21 -116.27(17) . . . . ? As4 As1 As2 C21 147.14(12) . . . . ? C11 As1 As2 As3 136.91(12) . . . . ? As4 As1 As2 As3 40.320(18) . . . . ? C21 As2 As3 C31 116.31(16) . . . . ? As1 As2 As3 C31 -139.19(12) . . . . ? C21 As2 As3 As4 -144.90(11) . . . . ? As1 As2 As3 As4 -40.396(18) . . . . ? C31 As3 As4 C41 -116.84(16) . . . . ? As2 As3 As4 C41 146.37(12) . . . . ? C31 As3 As4 As1 137.04(11) . . . . ? As2 As3 As4 As1 40.254(18) . . . . ? C11 As1 As4 C41 114.32(17) . . . . ? As2 As1 As4 C41 -145.39(12) . . . . ? C11 As1 As4 As3 -140.62(12) . . . . ? As2 As1 As4 As3 -40.330(18) . . . . ? As2 As1 C11 C12 50.3(3) . . . . ? As4 As1 C11 C12 129.6(3) . . . . ? As2 As1 C11 C18 -135.3(3) . . . . ? As4 As1 C11 C18 -56.0(3) . . . . ? C18 C11 C12 C14 6.7(6) . . . . ? As1 C11 C12 C14 -178.9(3) . . . . ? C18 C11 C12 C13 -171.3(4) . . . . ? As1 C11 C12 C13 3.1(6) . . . . ? C11 C12 C14 C15 -1.8(6) . . . . ? C13 C12 C14 C15 176.3(4) . . . . ? C12 C14 C15 C17 -3.2(6) . . . . ? C12 C14 C15 C16 178.7(4) . . . . ? C14 C15 C17 C18 3.3(6) . . . . ? C16 C15 C17 C18 -178.6(4) . . . . ? C15 C17 C18 C11 1.6(6) . . . . ? C15 C17 C18 C19 -175.8(4) . . . . ? C12 C11 C18 C17 -6.6(6) . . . . ? As1 C11 C18 C17 178.9(3) . . . . ? C12 C11 C18 C19 170.6(4) . . . . ? As1 C11 C18 C19 -3.9(5) . . . . ? As1 As2 C21 C22 -45.5(3) . . . . ? As3 As2 C21 C22 45.7(3) . . . . ? As1 As2 C21 C28 133.9(3) . . . . ? As3 As2 C21 C28 -134.9(3) . . . . ? C28 C21 C22 C24 -1.9(6) . . . . ? As2 C21 C22 C24 177.5(3) . . . . ? C28 C21 C22 C23 178.3(4) . . . . ? As2 C21 C22 C23 -2.4(6) . . . . ? C21 C22 C24 C25 0.7(6) . . . . ? C23 C22 C24 C25 -179.4(4) . . . . ? C22 C24 C25 C27 0.7(6) . . . . ? C22 C24 C25 C26 178.7(4) . . . . ? C24 C25 C27 C28 -1.1(6) . . . . ? C26 C25 C27 C28 -179.1(4) . . . . ? C25 C27 C28 C21 0.0(6) . . . . ? C25 C27 C28 C29 178.4(4) . . . . ? C22 C21 C28 C27 1.5(6) . . . . ? As2 C21 C28 C27 -177.9(3) . . . . ? C22 C21 C28 C29 -176.7(4) . . . . ? As2 C21 C28 C29 3.9(5) . . . . ? As4 As3 C31 C32 -132.1(3) . . . . ? As2 As3 C31 C32 -53.1(3) . . . . ? As4 As3 C31 C38 53.1(3) . . . . ? As2 As3 C31 C38 132.2(3) . . . . ? C38 C31 C32 C34 -9.7(6) . . . . ? As3 C31 C32 C34 175.5(3) . . . . ? C38 C31 C32 C33 165.8(4) . . . . ? As3 C31 C32 C33 -9.0(5) . . . . ? C31 C32 C34 C35 3.8(6) . . . . ? C33 C32 C34 C35 -171.9(4) . . . . ? C32 C34 C35 C37 3.8(6) . . . . ? C32 C34 C35 C36 -179.8(4) . . . . ? C34 C35 C37 C38 -5.7(6) . . . . ? C36 C35 C37 C38 178.0(4) . . . . ? C35 C37 C38 C31 -0.2(6) . . . . ? C35 C37 C38 C39 -180.0(4) . . . . ? C32 C31 C38 C37 7.9(6) . . . . ? As3 C31 C38 C37 -177.3(3) . . . . ? C32 C31 C38 C39 -172.3(4) . . . . ? As3 C31 C38 C39 2.5(5) . . . . ? As3 As4 C41 C42 -45.8(4) . . . . ? As1 As4 C41 C42 45.2(4) . . . . ? As3 As4 C41 C48 133.9(3) . . . . ? As1 As4 C41 C48 -135.1(3) . . . . ? C48 C41 C42 C44 -0.5(6) . . . . ? As4 C41 C42 C44 179.2(3) . . . . ? C48 C41 C42 C43 179.0(4) . . . . ? As4 C41 C42 C43 -1.3(6) . . . . ? C41 C42 C44 C45 0.2(6) . . . . ? C43 C42 C44 C45 -179.3(4) . . . . ? C42 C44 C45 C47 0.2(6) . . . . ? C42 C44 C45 C46 179.4(4) . . . . ? C44 C45 C47 C48 -0.5(6) . . . . ? C46 C45 C47 C48 -179.7(4) . . . . ? C45 C47 C48 C41 0.3(6) . . . . ? C45 C47 C48 C49 179.8(4) . . . . ? C42 C41 C48 C47 0.2(6) . . . . ? As4 C41 C48 C47 -179.5(3) . . . . ? C42 C41 C48 C49 -179.3(4) . . . . ? As4 C41 C48 C49 1.0(5) . . . . ? C7S C2S C3S C4S 1.1(7) . . . . ? C1S C2S C3S C4S -178.5(5) . . . . ? C2S C3S C4S C5S -0.6(8) . . . . ? C3S C4S C5S C6S -0.2(8) . . . . ? C4S C5S C6S C7S 0.5(8) . . . . ? C5S C6S C7S C2S 0.1(7) . . . . ? C3S C2S C7S C6S -0.9(7) . . . . ? C1S C2S C7S C6S 178.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 30.08 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 1.389 _refine_diff_density_min -1.538 _refine_diff_density_rms 0.226 # Attachment '_N3N_ZrAsHMes.cif' data_rw535zr _database_code_depnum_ccdc_archive 'CCDC 668520' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H51 As N4 Si3 Zr' _chemical_formula_weight 646.10 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' As As 0.0499 2.0058 '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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 19.0720(15) _cell_length_b 18.0788(15) _cell_length_c 19.3656(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6677.2(9) _cell_formula_units_Z 8 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9965 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 28.29 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2704 _exptl_absorpt_coefficient_mu 1.438 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8131 _exptl_absorpt_correction_T_max 0.9581 _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 84248 _diffrn_reflns_av_R_equivalents 0.0719 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 28.30 _reflns_number_total 8297 _reflns_number_gt 5747 _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. EXTI refined to zero. ; _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^)+(0.0261P)^2^+4.6549P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8297 _refine_ls_number_parameters 314 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0736 _refine_ls_wR_factor_gt 0.0629 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 0.188707(11) 0.752877(12) 0.139224(10) 0.01641(6) Uani 1 1 d . . . As As 0.192242(14) 0.744205(14) -0.006628(11) 0.02406(7) Uani 1 1 d . . . N1 N 0.12594(10) 0.67308(11) 0.18258(10) 0.0218(4) Uani 1 1 d . . . N2 N 0.28972(10) 0.74358(10) 0.17657(9) 0.0214(4) Uani 1 1 d . . . N3 N 0.14860(11) 0.85915(10) 0.14521(10) 0.0238(4) Uani 1 1 d . . . N4 N 0.18036(11) 0.78291(11) 0.26509(10) 0.0254(5) Uani 1 1 d . . . Si1 Si 0.13795(4) 0.57767(4) 0.17892(3) 0.02596(15) Uani 1 1 d . . . Si2 Si 0.37032(3) 0.77105(4) 0.14390(3) 0.02311(15) Uani 1 1 d . . . Si3 Si 0.07787(4) 0.89778(4) 0.10162(4) 0.03041(17) Uani 1 1 d . . . C1 C 0.08166(13) 0.70159(15) 0.23952(12) 0.0293(6) Uani 1 1 d . . . H1A H 0.0513 0.6616 0.2576 0.035 Uiso 1 1 calc R . . H1B H 0.0513 0.7421 0.2225 0.035 Uiso 1 1 calc R . . C2 C 0.29074(13) 0.71752(15) 0.24924(12) 0.0283(6) Uani 1 1 d . . . H2A H 0.3398 0.7127 0.2655 0.034 Uiso 1 1 calc R . . H2B H 0.2680 0.6684 0.2526 0.034 Uiso 1 1 calc R . . C3 C 0.17795(14) 0.90068(14) 0.20463(13) 0.0304(6) Uani 1 1 d . . . H3A H 0.1599 0.9520 0.2048 0.036 Uiso 1 1 calc R . . H3B H 0.2297 0.9024 0.2015 0.036 Uiso 1 1 calc R . . C4 C 0.12979(14) 0.73000(14) 0.29633(12) 0.0301(6) Uani 1 1 d . . . H4A H 0.1019 0.7550 0.3326 0.036 Uiso 1 1 calc R . . H4B H 0.1553 0.6882 0.3178 0.036 Uiso 1 1 calc R . . C5 C 0.25170(14) 0.77317(15) 0.29356(12) 0.0306(6) Uani 1 1 d . . . H5A H 0.2489 0.7551 0.3418 0.037 Uiso 1 1 calc R . . H5B H 0.2769 0.8211 0.2935 0.037 Uiso 1 1 calc R . . C6 C 0.15557(16) 0.86076(14) 0.27014(13) 0.0341(6) Uani 1 1 d . . . H6A H 0.1764 0.8851 0.3111 0.041 Uiso 1 1 calc R . . H6B H 0.1039 0.8620 0.2748 0.041 Uiso 1 1 calc R . . C7 C 0.05900(16) 0.53165(16) 0.14165(16) 0.0449(8) Uani 1 1 d . . . H7A H 0.0530 0.5473 0.0936 0.067 Uiso 1 1 calc R . . H7B H 0.0175 0.5456 0.1684 0.067 Uiso 1 1 calc R . . H7C H 0.0651 0.4779 0.1434 0.067 Uiso 1 1 calc R . . C8 C 0.21671(15) 0.55897(15) 0.12507(13) 0.0363(7) Uani 1 1 d . . . H8A H 0.2577 0.5830 0.1458 0.054 Uiso 1 1 calc R . . H8B H 0.2092 0.5786 0.0785 0.054 Uiso 1 1 calc R . . H8C H 0.2247 0.5055 0.1226 0.054 Uiso 1 1 calc R . . C9 C 0.15335(15) 0.53826(15) 0.26724(13) 0.0347(6) Uani 1 1 d . . . H9A H 0.1970 0.5583 0.2862 0.052 Uiso 1 1 calc R . . H9B H 0.1569 0.4843 0.2642 0.052 Uiso 1 1 calc R . . H9C H 0.1142 0.5516 0.2975 0.052 Uiso 1 1 calc R . . C10 C 0.42672(14) 0.68903(15) 0.12571(14) 0.0363(7) Uani 1 1 d . . . H10A H 0.4037 0.6574 0.0914 0.054 Uiso 1 1 calc R . . H10B H 0.4340 0.6610 0.1684 0.054 Uiso 1 1 calc R . . H10C H 0.4721 0.7056 0.1078 0.054 Uiso 1 1 calc R . . C11 C 0.41905(14) 0.82829(14) 0.20851(14) 0.0340(6) Uani 1 1 d . . . H11A H 0.3914 0.8723 0.2199 0.051 Uiso 1 1 calc R . . H11B H 0.4642 0.8434 0.1890 0.051 Uiso 1 1 calc R . . H11C H 0.4270 0.7991 0.2504 0.051 Uiso 1 1 calc R . . C12 C 0.35615(14) 0.82730(16) 0.06467(14) 0.0377(7) Uani 1 1 d . . . H12A H 0.3393 0.7953 0.0273 0.057 Uiso 1 1 calc R . . H12B H 0.4004 0.8504 0.0509 0.057 Uiso 1 1 calc R . . H12C H 0.3212 0.8658 0.0741 0.057 Uiso 1 1 calc R . . C13 C 0.10704(17) 0.94473(18) 0.02099(15) 0.0509(9) Uani 1 1 d . . . H13A H 0.1391 0.9852 0.0327 0.076 Uiso 1 1 calc R . . H13B H 0.0662 0.9646 -0.0034 0.076 Uiso 1 1 calc R . . H13C H 0.1312 0.9090 -0.0088 0.076 Uiso 1 1 calc R . . C14 C 0.01190(15) 0.82443(17) 0.08143(16) 0.0434(7) Uani 1 1 d . . . H14A H 0.0361 0.7796 0.0660 0.065 Uiso 1 1 calc R . . H14B H -0.0194 0.8419 0.0448 0.065 Uiso 1 1 calc R . . H14C H -0.0156 0.8134 0.1229 0.065 Uiso 1 1 calc R . . C15 C 0.03130(17) 0.96777(17) 0.15625(16) 0.0503(8) Uani 1 1 d . . . H15A H 0.0622 1.0102 0.1643 0.075 Uiso 1 1 calc R . . H15B H 0.0185 0.9454 0.2006 0.075 Uiso 1 1 calc R . . H15C H -0.0112 0.9844 0.1324 0.075 Uiso 1 1 calc R . . C16 C 0.18260(12) 0.64089(12) -0.03660(11) 0.0202(5) Uani 1 1 d . . . C17 C 0.11761(12) 0.60446(13) -0.04270(11) 0.0233(5) Uani 1 1 d . . . C18 C 0.11583(14) 0.53157(14) -0.06571(12) 0.0272(6) Uani 1 1 d . . . H18A H 0.0718 0.5073 -0.0691 0.033 Uiso 1 1 calc R . . C19 C 0.17595(14) 0.49302(13) -0.08391(12) 0.0271(6) Uani 1 1 d . . . C20 C 0.23955(13) 0.52951(14) -0.07752(12) 0.0268(6) Uani 1 1 d . . . H20A H 0.2814 0.5040 -0.0895 0.032 Uiso 1 1 calc R . . C21 C 0.24437(13) 0.60214(13) -0.05426(11) 0.0228(5) Uani 1 1 d . . . C22 C 0.04954(13) 0.64099(15) -0.02395(15) 0.0322(6) Uani 1 1 d . . . H22A H 0.0111 0.6054 -0.0289 0.048 Uiso 1 1 calc R . . H22B H 0.0414 0.6832 -0.0547 0.048 Uiso 1 1 calc R . . H22C H 0.0517 0.6583 0.0240 0.048 Uiso 1 1 calc R . . C23 C 0.17179(17) 0.41458(15) -0.11053(14) 0.0427(7) Uani 1 1 d . . . H23A H 0.2128 0.3867 -0.0947 0.064 Uiso 1 1 calc R . . H23B H 0.1708 0.4151 -0.1611 0.064 Uiso 1 1 calc R . . H23C H 0.1290 0.3910 -0.0930 0.064 Uiso 1 1 calc R . . C24 C 0.31555(13) 0.63630(15) -0.04579(13) 0.0312(6) Uani 1 1 d . . . H24A H 0.3172 0.6835 -0.0707 0.047 Uiso 1 1 calc R . . H24B H 0.3512 0.6028 -0.0645 0.047 Uiso 1 1 calc R . . H24C H 0.3247 0.6449 0.0033 0.047 Uiso 1 1 calc R . . H1 H 0.1346(17) 0.7595(16) -0.0117(16) 0.058(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.01754(10) 0.01961(10) 0.01207(10) 0.00009(8) -0.00012(8) -0.00144(9) As 0.03332(14) 0.02578(13) 0.01308(11) -0.00076(10) -0.00054(10) -0.00023(12) N1 0.0200(10) 0.0267(10) 0.0189(10) 0.0012(8) 0.0011(8) -0.0037(8) N2 0.0229(10) 0.0253(10) 0.0159(9) 0.0054(8) -0.0034(7) -0.0027(8) N3 0.0294(11) 0.0220(10) 0.0201(10) -0.0009(8) 0.0028(9) 0.0001(8) N4 0.0320(12) 0.0271(10) 0.0170(10) -0.0006(8) 0.0008(9) -0.0047(9) Si1 0.0320(4) 0.0234(3) 0.0225(3) 0.0045(3) -0.0063(3) -0.0070(3) Si2 0.0185(3) 0.0267(3) 0.0241(3) 0.0030(3) -0.0043(3) -0.0030(3) Si3 0.0324(4) 0.0312(4) 0.0277(4) 0.0050(3) 0.0062(3) 0.0114(3) C1 0.0265(14) 0.0349(14) 0.0263(14) 0.0017(11) 0.0076(11) -0.0047(11) C2 0.0289(14) 0.0353(14) 0.0207(12) 0.0084(11) -0.0090(10) -0.0079(11) C3 0.0419(16) 0.0225(12) 0.0268(13) -0.0044(10) 0.0011(12) -0.0003(11) C4 0.0357(15) 0.0366(15) 0.0181(12) 0.0001(10) 0.0072(11) -0.0031(12) C5 0.0391(15) 0.0374(15) 0.0153(11) 0.0004(10) -0.0051(11) -0.0096(12) C6 0.0481(17) 0.0336(15) 0.0205(13) -0.0087(11) 0.0048(12) -0.0002(13) C7 0.053(2) 0.0349(16) 0.0466(18) 0.0092(14) -0.0196(15) -0.0191(14) C8 0.0511(18) 0.0308(14) 0.0269(14) 0.0025(11) -0.0026(13) 0.0091(13) C9 0.0417(16) 0.0325(14) 0.0300(14) 0.0082(12) -0.0064(13) -0.0113(12) C10 0.0286(14) 0.0414(16) 0.0390(16) -0.0086(13) -0.0052(13) 0.0038(12) C11 0.0295(15) 0.0313(14) 0.0412(16) -0.0010(12) -0.0100(13) -0.0045(12) C12 0.0278(15) 0.0519(18) 0.0334(15) 0.0173(13) -0.0058(12) -0.0150(13) C13 0.055(2) 0.055(2) 0.0428(18) 0.0223(16) 0.0084(16) 0.0188(16) C14 0.0292(16) 0.0564(19) 0.0447(18) -0.0043(15) -0.0039(14) 0.0123(14) C15 0.057(2) 0.0420(17) 0.052(2) -0.0006(15) 0.0127(17) 0.0221(16) C16 0.0248(13) 0.0250(12) 0.0109(11) 0.0013(9) -0.0024(9) 0.0010(10) C17 0.0232(13) 0.0310(13) 0.0158(11) 0.0001(10) -0.0044(10) 0.0018(10) C18 0.0302(14) 0.0306(13) 0.0209(12) 0.0006(10) -0.0052(11) -0.0067(11) C19 0.0394(16) 0.0271(13) 0.0149(12) -0.0016(10) -0.0008(11) 0.0016(11) C20 0.0291(14) 0.0344(14) 0.0168(12) -0.0005(10) 0.0013(10) 0.0105(11) C21 0.0233(13) 0.0317(13) 0.0133(11) 0.0002(10) -0.0018(10) 0.0022(10) C22 0.0215(13) 0.0346(15) 0.0405(16) 0.0013(12) -0.0011(12) 0.0017(11) C23 0.062(2) 0.0318(15) 0.0340(16) -0.0070(12) 0.0024(14) -0.0011(14) C24 0.0232(14) 0.0403(15) 0.0300(14) 0.0011(12) -0.0015(11) 0.0017(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr N1 2.0540(19) . ? Zr N2 2.0646(19) . ? Zr N3 2.0712(19) . ? Zr N4 2.5023(19) . ? Zr As 2.8297(4) . ? As C16 1.965(2) . ? As H1 1.14(3) . ? N1 C1 1.482(3) . ? N1 Si1 1.742(2) . ? N2 C2 1.484(3) . ? N2 Si2 1.735(2) . ? N3 C3 1.484(3) . ? N3 Si3 1.738(2) . ? N4 C5 1.479(3) . ? N4 C4 1.487(3) . ? N4 C6 1.488(3) . ? Si1 C8 1.860(3) . ? Si1 C7 1.866(3) . ? Si1 C9 1.876(3) . ? Si2 C12 1.860(3) . ? Si2 C10 1.865(3) . ? Si2 C11 1.871(3) . ? Si3 C13 1.862(3) . ? Si3 C14 1.869(3) . ? Si3 C15 1.873(3) . ? C1 C4 1.522(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C5 1.518(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C6 1.521(3) . ? 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 1.409(3) . ? C16 C21 1.413(3) . ? C17 C18 1.391(3) . ? C17 C22 1.501(3) . ? C18 C19 1.387(3) . ? C18 H18A 0.9500 . ? C19 C20 1.386(4) . ? C19 C23 1.511(3) . ? C20 C21 1.391(3) . ? C20 H20A 0.9500 . ? C21 C24 1.500(3) . ? 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 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 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 N2 110.09(7) . . ? N1 Zr N3 114.41(8) . . ? N2 Zr N3 113.61(8) . . ? N1 Zr N4 73.57(7) . . ? N2 Zr N4 74.68(7) . . ? N3 Zr N4 73.78(7) . . ? N1 Zr As 112.52(5) . . ? N2 Zr As 108.84(5) . . ? N3 Zr As 96.67(5) . . ? N4 Zr As 170.36(5) . . ? C16 As Zr 110.21(6) . . ? C16 As H1 96.6(14) . . ? Zr As H1 92.8(15) . . ? C1 N1 Si1 116.73(15) . . ? C1 N1 Zr 113.09(15) . . ? Si1 N1 Zr 127.04(11) . . ? C2 N2 Si2 115.15(15) . . ? C2 N2 Zr 111.73(14) . . ? Si2 N2 Zr 132.51(10) . . ? C3 N3 Si3 117.79(16) . . ? C3 N3 Zr 111.93(15) . . ? Si3 N3 Zr 129.22(11) . . ? C5 N4 C4 111.63(19) . . ? C5 N4 C6 112.4(2) . . ? C4 N4 C6 112.1(2) . . ? C5 N4 Zr 106.19(14) . . ? C4 N4 Zr 107.34(14) . . ? C6 N4 Zr 106.82(14) . . ? N1 Si1 C8 108.00(11) . . ? N1 Si1 C7 110.56(12) . . ? C8 Si1 C7 110.72(14) . . ? N1 Si1 C9 111.08(11) . . ? C8 Si1 C9 108.41(13) . . ? C7 Si1 C9 108.04(12) . . ? N2 Si2 C12 109.18(11) . . ? N2 Si2 C10 110.63(11) . . ? C12 Si2 C10 111.26(14) . . ? N2 Si2 C11 110.77(11) . . ? C12 Si2 C11 108.74(13) . . ? C10 Si2 C11 106.23(12) . . ? N3 Si3 C13 111.02(12) . . ? N3 Si3 C14 109.81(12) . . ? C13 Si3 C14 110.42(15) . . ? N3 Si3 C15 111.42(13) . . ? C13 Si3 C15 107.90(14) . . ? C14 Si3 C15 106.16(14) . . ? N1 C1 C4 108.2(2) . . ? N1 C1 H1A 110.1 . . ? C4 C1 H1A 110.1 . . ? N1 C1 H1B 110.1 . . ? C4 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? N2 C2 C5 108.6(2) . . ? N2 C2 H2A 110.0 . . ? C5 C2 H2A 110.0 . . ? N2 C2 H2B 110.0 . . ? C5 C2 H2B 110.0 . . ? H2A C2 H2B 108.3 . . ? N3 C3 C6 107.5(2) . . ? N3 C3 H3A 110.2 . . ? C6 C3 H3A 110.2 . . ? N3 C3 H3B 110.2 . . ? C6 C3 H3B 110.2 . . ? H3A C3 H3B 108.5 . . ? N4 C4 C1 108.31(19) . . ? N4 C4 H4A 110.0 . . ? C1 C4 H4A 110.0 . . ? N4 C4 H4B 110.0 . . ? C1 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? N4 C5 C2 108.63(19) . . ? N4 C5 H5A 110.0 . . ? C2 C5 H5A 110.0 . . ? N4 C5 H5B 110.0 . . ? C2 C5 H5B 110.0 . . ? H5A C5 H5B 108.3 . . ? N4 C6 C3 107.8(2) . . ? N4 C6 H6A 110.2 . . ? C3 C6 H6A 110.2 . . ? N4 C6 H6B 110.2 . . ? C3 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? 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 C21 118.8(2) . . ? C17 C16 As 123.48(17) . . ? C21 C16 As 117.71(17) . . ? C18 C17 C16 119.4(2) . . ? C18 C17 C22 118.2(2) . . ? C16 C17 C22 122.4(2) . . ? C19 C18 C17 122.5(2) . . ? C19 C18 H18A 118.8 . . ? C17 C18 H18A 118.8 . . ? C20 C19 C18 117.5(2) . . ? C20 C19 C23 121.5(2) . . ? C18 C19 C23 121.0(2) . . ? C19 C20 C21 122.4(2) . . ? C19 C20 H20A 118.8 . . ? C21 C20 H20A 118.8 . . ? C20 C21 C16 119.4(2) . . ? C20 C21 C24 118.9(2) . . ? C16 C21 C24 121.6(2) . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.599 _refine_diff_density_min -0.562 _refine_diff_density_rms 0.074 # Attachment '_N3N_ZrAsPh2.cif' data_rw429zr _database_code_depnum_ccdc_archive 'CCDC 668521' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H49 As N4 Si3 Zr' _chemical_formula_weight 680.11 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' As As 0.0499 2.0058 '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 10.815(3) _cell_length_b 16.799(4) _cell_length_c 19.280(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.249(4) _cell_angle_gamma 90.00 _cell_volume 3423.3(15) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 414 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 25.08 _exptl_crystal_description Bulk _exptl_crystal_colour Orange _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 1.407 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6858 _exptl_absorpt_correction_T_max 0.9330 _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 46122 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 28.86 _reflns_number_total 8956 _reflns_number_gt 7442 _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. EXTI refined to 0 ; _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^)+(0.0289P)^2^+1.3668P] 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 8956 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0618 _refine_ls_wR_factor_gt 0.0574 _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 0.878415(15) 0.740479(9) 0.242668(8) 0.01540(4) Uani 1 1 d . . . As As 0.720018(16) 0.618524(10) 0.172840(9) 0.01679(5) Uani 1 1 d . . . N1 N 0.98694(14) 0.67384(9) 0.32311(8) 0.0223(3) Uani 1 1 d . . . N2 N 0.98306(13) 0.79662(9) 0.17822(8) 0.0201(3) Uani 1 1 d . . . N3 N 0.76330(13) 0.81589(8) 0.28269(7) 0.0183(3) Uani 1 1 d . . . N4 N 1.02315(14) 0.83734(9) 0.32002(8) 0.0215(3) Uani 1 1 d . . . Si1 Si 1.04621(5) 0.57823(3) 0.32211(3) 0.02537(11) Uani 1 1 d . . . Si2 Si 0.92156(5) 0.84827(3) 0.10052(3) 0.02235(11) Uani 1 1 d . . . Si3 Si 0.63992(5) 0.79113(3) 0.32364(3) 0.02131(10) Uani 1 1 d . . . C1 C 1.02343(19) 0.71765(11) 0.39127(10) 0.0288(4) Uani 1 1 d . . . H1A H 1.0747 0.6830 0.4279 0.035 Uiso 1 1 calc R . . H1B H 0.9468 0.7343 0.4079 0.035 Uiso 1 1 calc R . . C2 C 1.11290(16) 0.81902(11) 0.21529(10) 0.0253(4) Uani 1 1 d . . . H2A H 1.1576 0.8455 0.1818 0.030 Uiso 1 1 calc R . . H2B H 1.1613 0.7709 0.2344 0.030 Uiso 1 1 calc R . . C3 C 0.81292(17) 0.89827(10) 0.29272(10) 0.0220(4) Uani 1 1 d . . . H3A H 0.7527 0.9326 0.3110 0.026 Uiso 1 1 calc R . . H3B H 0.8243 0.9204 0.2469 0.026 Uiso 1 1 calc R . . C4 C 1.09984(18) 0.79033(12) 0.37900(10) 0.0287(4) Uani 1 1 d . . . H4A H 1.1201 0.8230 0.4227 0.034 Uiso 1 1 calc R . . H4B H 1.1802 0.7736 0.3666 0.034 Uiso 1 1 calc R . . C5 C 1.10244(17) 0.87554(11) 0.27569(10) 0.0254(4) Uani 1 1 d . . . H5A H 1.1876 0.8870 0.3047 0.030 Uiso 1 1 calc R . . H5B H 1.0636 0.9264 0.2562 0.030 Uiso 1 1 calc R . . C6 C 0.93966(17) 0.89563(11) 0.34569(10) 0.0232(4) Uani 1 1 d . . . H6A H 0.9793 0.9490 0.3500 0.028 Uiso 1 1 calc R . . H6B H 0.9267 0.8795 0.3930 0.028 Uiso 1 1 calc R . . C7 C 1.2172(2) 0.57476(18) 0.36756(13) 0.0538(7) Uani 1 1 d . . . H7A H 1.2256 0.5868 0.4181 0.081 Uiso 1 1 calc R . . H7B H 1.2645 0.6142 0.3461 0.081 Uiso 1 1 calc R . . H7C H 1.2510 0.5215 0.3623 0.081 Uiso 1 1 calc R . . C8 C 0.9573(3) 0.50687(14) 0.36699(15) 0.0556(7) Uani 1 1 d . . . H8A H 0.8677 0.5074 0.3432 0.083 Uiso 1 1 calc R . . H8B H 0.9657 0.5225 0.4168 0.083 Uiso 1 1 calc R . . H8C H 0.9917 0.4532 0.3647 0.083 Uiso 1 1 calc R . . C9 C 1.03563(17) 0.54678(11) 0.22817(10) 0.0273(4) Uani 1 1 d . . . H9A H 0.9493 0.5290 0.2077 0.041 Uiso 1 1 calc R . . H9B H 1.0950 0.5030 0.2268 0.041 Uiso 1 1 calc R . . H9C H 1.0571 0.5919 0.2007 0.041 Uiso 1 1 calc R . . C10 C 0.74864(17) 0.82672(12) 0.07671(10) 0.0276(4) Uani 1 1 d . . . H10A H 0.7123 0.8329 0.1188 0.041 Uiso 1 1 calc R . . H10B H 0.7353 0.7720 0.0590 0.041 Uiso 1 1 calc R . . H10C H 0.7074 0.8639 0.0398 0.041 Uiso 1 1 calc R . . C11 C 0.9988(2) 0.81840(14) 0.02655(11) 0.0392(5) Uani 1 1 d . . . H11A H 0.9831 0.7618 0.0160 0.059 Uiso 1 1 calc R . . H11B H 1.0901 0.8278 0.0406 0.059 Uiso 1 1 calc R . . H11C H 0.9636 0.8500 -0.0158 0.059 Uiso 1 1 calc R . . C12 C 0.9427(2) 0.95881(12) 0.11088(12) 0.0348(5) Uani 1 1 d . . . H12A H 0.8953 0.9783 0.1455 0.052 Uiso 1 1 calc R . . H12B H 0.9111 0.9848 0.0650 0.052 Uiso 1 1 calc R . . H12C H 1.0327 0.9711 0.1275 0.052 Uiso 1 1 calc R . . C13 C 0.48261(18) 0.81166(12) 0.26514(12) 0.0328(5) Uani 1 1 d . . . H13A H 0.4751 0.8687 0.2543 0.049 Uiso 1 1 calc R . . H13B H 0.4156 0.7956 0.2894 0.049 Uiso 1 1 calc R . . H13C H 0.4744 0.7815 0.2209 0.049 Uiso 1 1 calc R . . C14 C 0.6492(2) 0.85050(12) 0.40654(11) 0.0338(5) Uani 1 1 d . . . H14A H 0.6248 0.9057 0.3941 0.051 Uiso 1 1 calc R . . H14B H 0.7360 0.8492 0.4347 0.051 Uiso 1 1 calc R . . H14C H 0.5917 0.8278 0.4343 0.051 Uiso 1 1 calc R . . C15 C 0.65651(19) 0.68369(11) 0.34972(10) 0.0285(4) Uani 1 1 d . . . H15A H 0.6741 0.6523 0.3101 0.043 Uiso 1 1 calc R . . H15B H 0.5778 0.6650 0.3617 0.043 Uiso 1 1 calc R . . H15C H 0.7264 0.6775 0.3910 0.043 Uiso 1 1 calc R . . C21 C 0.53976(16) 0.64476(10) 0.14893(9) 0.0189(3) Uani 1 1 d . . . C22 C 0.48355(17) 0.69323(11) 0.09211(10) 0.0244(4) Uani 1 1 d . . . H22A H 0.5339 0.7153 0.0621 0.029 Uiso 1 1 calc R . . C23 C 0.35472(18) 0.70939(12) 0.07903(11) 0.0312(4) Uani 1 1 d . . . H23A H 0.3180 0.7427 0.0403 0.037 Uiso 1 1 calc R . . C24 C 0.27939(18) 0.67765(13) 0.12158(12) 0.0337(5) Uani 1 1 d . . . H24A H 0.1913 0.6889 0.1123 0.040 Uiso 1 1 calc R . . C25 C 0.33350(19) 0.62931(12) 0.17795(11) 0.0318(5) Uani 1 1 d . . . H25A H 0.2825 0.6075 0.2077 0.038 Uiso 1 1 calc R . . C26 C 0.46222(17) 0.61261(11) 0.19120(10) 0.0244(4) Uani 1 1 d . . . H26A H 0.4981 0.5787 0.2297 0.029 Uiso 1 1 calc R . . C31 C 0.74969(15) 0.59242(10) 0.07934(9) 0.0169(3) Uani 1 1 d . . . C32 C 0.86289(17) 0.61244(11) 0.05982(10) 0.0226(4) Uani 1 1 d . . . H32A H 0.9201 0.6480 0.0886 0.027 Uiso 1 1 calc R . . C33 C 0.89285(18) 0.58092(12) -0.00117(10) 0.0281(4) Uani 1 1 d . . . H33A H 0.9709 0.5945 -0.0132 0.034 Uiso 1 1 calc R . . C34 C 0.81012(18) 0.52983(11) -0.04465(10) 0.0259(4) Uani 1 1 d . . . H34A H 0.8314 0.5081 -0.0861 0.031 Uiso 1 1 calc R . . C35 C 0.69602(17) 0.51080(10) -0.02688(9) 0.0214(4) Uani 1 1 d . . . H35A H 0.6379 0.4767 -0.0568 0.026 Uiso 1 1 calc R . . C36 C 0.66646(16) 0.54147(10) 0.03443(9) 0.0181(3) Uani 1 1 d . . . H36A H 0.5882 0.5277 0.0462 0.022 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 0.01508(8) 0.01383(8) 0.01633(8) -0.00323(6) 0.00118(6) 0.00022(6) As 0.01639(9) 0.01668(9) 0.01707(9) -0.00365(6) 0.00306(6) -0.00143(6) N1 0.0238(8) 0.0189(7) 0.0210(8) -0.0026(6) -0.0025(6) 0.0017(6) N2 0.0167(7) 0.0211(7) 0.0219(8) -0.0043(6) 0.0030(6) -0.0023(6) N3 0.0196(7) 0.0154(7) 0.0199(7) -0.0035(5) 0.0044(6) -0.0008(5) N4 0.0190(7) 0.0203(7) 0.0234(8) -0.0047(6) 0.0005(6) -0.0007(6) Si1 0.0257(3) 0.0210(3) 0.0281(3) 0.0025(2) 0.0027(2) 0.0074(2) Si2 0.0232(2) 0.0222(2) 0.0230(3) -0.00043(19) 0.0077(2) -0.00266(19) Si3 0.0229(2) 0.0194(2) 0.0234(3) -0.00508(19) 0.0089(2) -0.00110(19) C1 0.0332(10) 0.0258(10) 0.0225(9) -0.0028(7) -0.0048(8) 0.0027(8) C2 0.0174(8) 0.0285(10) 0.0299(10) -0.0079(8) 0.0047(7) -0.0037(7) C3 0.0235(9) 0.0161(8) 0.0272(9) -0.0032(7) 0.0070(7) 0.0001(7) C4 0.0267(10) 0.0275(10) 0.0261(10) -0.0073(8) -0.0072(8) -0.0003(8) C5 0.0178(8) 0.0258(10) 0.0318(10) -0.0095(8) 0.0032(7) -0.0061(7) C6 0.0252(9) 0.0191(9) 0.0251(9) -0.0081(7) 0.0048(7) -0.0020(7) C7 0.0375(13) 0.0707(18) 0.0446(14) -0.0111(13) -0.0104(11) 0.0267(12) C8 0.085(2) 0.0294(12) 0.0614(17) 0.0124(11) 0.0367(15) 0.0054(13) C9 0.0214(9) 0.0244(9) 0.0359(11) -0.0043(8) 0.0052(8) 0.0021(7) C10 0.0262(10) 0.0277(10) 0.0263(10) 0.0017(8) 0.0000(8) -0.0033(8) C11 0.0476(13) 0.0429(13) 0.0328(11) 0.0042(10) 0.0219(10) 0.0044(10) C12 0.0348(11) 0.0256(10) 0.0445(12) 0.0045(9) 0.0092(9) -0.0069(8) C13 0.0232(10) 0.0266(10) 0.0486(13) -0.0090(9) 0.0074(9) 0.0016(8) C14 0.0456(12) 0.0297(11) 0.0318(11) -0.0102(8) 0.0212(9) -0.0060(9) C15 0.0360(11) 0.0240(10) 0.0275(10) -0.0009(8) 0.0114(8) -0.0035(8) C21 0.0176(8) 0.0183(8) 0.0206(8) -0.0077(6) 0.0037(6) -0.0023(6) C22 0.0214(9) 0.0262(10) 0.0250(9) -0.0034(7) 0.0034(7) -0.0008(7) C23 0.0247(10) 0.0299(10) 0.0351(11) -0.0059(8) -0.0021(8) 0.0050(8) C24 0.0162(9) 0.0380(12) 0.0456(12) -0.0182(10) 0.0039(8) 0.0008(8) C25 0.0242(10) 0.0360(11) 0.0389(12) -0.0152(9) 0.0152(9) -0.0095(8) C26 0.0260(9) 0.0236(9) 0.0249(9) -0.0080(7) 0.0081(7) -0.0058(7) C31 0.0193(8) 0.0145(8) 0.0172(8) 0.0001(6) 0.0045(6) 0.0020(6) C32 0.0195(9) 0.0217(9) 0.0271(9) -0.0026(7) 0.0058(7) -0.0022(7) C33 0.0255(10) 0.0293(10) 0.0331(11) -0.0005(8) 0.0145(8) -0.0004(8) C34 0.0323(10) 0.0266(10) 0.0209(9) -0.0009(7) 0.0101(8) 0.0078(8) C35 0.0257(9) 0.0172(8) 0.0192(8) -0.0003(7) 0.0001(7) 0.0033(7) C36 0.0174(8) 0.0157(8) 0.0208(8) 0.0005(6) 0.0030(6) 0.0001(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 N3 2.0392(14) . ? Zr N1 2.0650(15) . ? Zr N2 2.0763(15) . ? Zr N4 2.5163(15) . ? Zr As 2.8224(5) . ? As C31 1.9469(17) . ? As C21 1.9561(17) . ? N1 C1 1.485(2) . ? N1 Si1 1.7310(16) . ? N2 C2 1.483(2) . ? N2 Si2 1.7369(16) . ? N3 C3 1.482(2) . ? N3 Si3 1.7389(15) . ? N4 C5 1.479(2) . ? N4 C4 1.485(2) . ? N4 C6 1.486(2) . ? Si1 C8 1.861(2) . ? Si1 C9 1.867(2) . ? Si1 C7 1.872(2) . ? Si2 C10 1.8642(19) . ? Si2 C11 1.868(2) . ? Si2 C12 1.877(2) . ? Si3 C13 1.863(2) . ? Si3 C14 1.869(2) . ? Si3 C15 1.872(2) . ? C1 C4 1.521(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C5 1.525(3) . ? 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 . ? C21 C26 1.396(2) . ? C21 C22 1.396(3) . ? C22 C23 1.389(3) . ? C22 H22A 0.9500 . ? C23 C24 1.380(3) . ? C23 H23A 0.9500 . ? C24 C25 1.383(3) . ? C24 H24A 0.9500 . ? C25 C26 1.390(3) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C31 C32 1.396(2) . ? C31 C36 1.401(2) . ? C32 C33 1.389(3) . ? C32 H32A 0.9500 . ? C33 C34 1.386(3) . ? C33 H33A 0.9500 . ? C34 C35 1.386(3) . ? C34 H34A 0.9500 . ? C35 C36 1.388(2) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Zr N1 110.36(6) . . ? N3 Zr N2 113.48(6) . . ? N1 Zr N2 113.62(6) . . ? N3 Zr N4 74.16(5) . . ? N1 Zr N4 73.89(6) . . ? N2 Zr N4 73.23(6) . . ? N3 Zr As 105.90(4) . . ? N1 Zr As 98.94(4) . . ? N2 Zr As 113.39(4) . . ? N4 Zr As 172.07(4) . . ? C31 As C21 100.63(7) . . ? C31 As Zr 113.74(5) . . ? C21 As Zr 115.00(5) . . ? C1 N1 Si1 116.13(12) . . ? C1 N1 Zr 113.45(11) . . ? Si1 N1 Zr 130.35(8) . . ? C2 N2 Si2 116.05(12) . . ? C2 N2 Zr 114.06(11) . . ? Si2 N2 Zr 125.83(8) . . ? C3 N3 Si3 117.10(11) . . ? C3 N3 Zr 113.34(11) . . ? Si3 N3 Zr 127.74(8) . . ? C5 N4 C4 112.03(15) . . ? C5 N4 C6 111.97(14) . . ? C4 N4 C6 112.06(15) . . ? C5 N4 Zr 107.58(10) . . ? C4 N4 Zr 106.62(10) . . ? C6 N4 Zr 106.14(10) . . ? N1 Si1 C8 111.31(10) . . ? N1 Si1 C9 109.08(8) . . ? C8 Si1 C9 109.73(11) . . ? N1 Si1 C7 110.80(10) . . ? C8 Si1 C7 108.60(14) . . ? C9 Si1 C7 107.25(10) . . ? N2 Si2 C10 107.22(8) . . ? N2 Si2 C11 111.89(9) . . ? C10 Si2 C11 110.33(10) . . ? N2 Si2 C12 112.76(9) . . ? C10 Si2 C12 108.16(9) . . ? C11 Si2 C12 106.44(10) . . ? N3 Si3 C13 111.77(9) . . ? N3 Si3 C14 110.70(8) . . ? C13 Si3 C14 107.19(10) . . ? N3 Si3 C15 108.27(8) . . ? C13 Si3 C15 111.36(9) . . ? C14 Si3 C15 107.47(9) . . ? N1 C1 C4 108.15(16) . . ? N1 C1 H1A 110.1 . . ? C4 C1 H1A 110.1 . . ? N1 C1 H1B 110.1 . . ? C4 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? N2 C2 C5 108.05(14) . . ? N2 C2 H2A 110.1 . . ? C5 C2 H2A 110.1 . . ? N2 C2 H2B 110.1 . . ? C5 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? N3 C3 C6 108.01(14) . . ? N3 C3 H3A 110.1 . . ? C6 C3 H3A 110.1 . . ? N3 C3 H3B 110.1 . . ? C6 C3 H3B 110.1 . . ? H3A C3 H3B 108.4 . . ? N4 C4 C1 108.21(15) . . ? N4 C4 H4A 110.1 . . ? C1 C4 H4A 110.1 . . ? N4 C4 H4B 110.1 . . ? C1 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? N4 C5 C2 108.49(14) . . ? N4 C5 H5A 110.0 . . ? C2 C5 H5A 110.0 . . ? N4 C5 H5B 110.0 . . ? C2 C5 H5B 110.0 . . ? H5A C5 H5B 108.4 . . ? N4 C6 C3 108.61(14) . . ? N4 C6 H6A 110.0 . . ? C3 C6 H6A 110.0 . . ? N4 C6 H6B 110.0 . . ? C3 C6 H6B 110.0 . . ? 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 . . ? C26 C21 C22 117.91(16) . . ? C26 C21 As 117.86(13) . . ? C22 C21 As 124.23(13) . . ? C23 C22 C21 120.63(18) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C24 C23 C22 120.82(19) . . ? C24 C23 H23A 119.6 . . ? C22 C23 H23A 119.6 . . ? C23 C24 C25 119.29(18) . . ? C23 C24 H24A 120.4 . . ? C25 C24 H24A 120.4 . . ? C24 C25 C26 120.22(19) . . ? C24 C25 H25A 119.9 . . ? C26 C25 H25A 119.9 . . ? C25 C26 C21 121.13(19) . . ? C25 C26 H26A 119.4 . . ? C21 C26 H26A 119.4 . . ? C32 C31 C36 117.77(15) . . ? C32 C31 As 121.43(13) . . ? C36 C31 As 119.97(12) . . ? C33 C32 C31 120.77(17) . . ? C33 C32 H32A 119.6 . . ? C31 C32 H32A 119.6 . . ? C34 C33 C32 120.75(17) . . ? C34 C33 H33A 119.6 . . ? C32 C33 H33A 119.6 . . ? C33 C34 C35 119.18(17) . . ? C33 C34 H34A 120.4 . . ? C35 C34 H34A 120.4 . . ? C34 C35 C36 120.19(16) . . ? C34 C35 H35A 119.9 . . ? C36 C35 H35A 119.9 . . ? C35 C36 C31 121.30(16) . . ? C35 C36 H36A 119.3 . . ? C31 C36 H36A 119.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Zr As C31 134.21(7) . . . . ? N1 Zr As C31 -111.51(7) . . . . ? N2 Zr As C31 9.14(7) . . . . ? N4 Zr As C31 -136.5(3) . . . . ? N3 Zr As C21 18.91(7) . . . . ? N1 Zr As C21 133.19(7) . . . . ? N2 Zr As C21 -106.15(7) . . . . ? N4 Zr As C21 108.2(3) . . . . ? N3 Zr N1 C1 -34.07(14) . . . . ? N2 Zr N1 C1 94.69(13) . . . . ? N4 Zr N1 C1 31.70(12) . . . . ? As Zr N1 C1 -144.81(12) . . . . ? N3 Zr N1 Si1 149.04(10) . . . . ? N2 Zr N1 Si1 -82.20(12) . . . . ? N4 Zr N1 Si1 -145.19(12) . . . . ? As Zr N1 Si1 38.29(11) . . . . ? N3 Zr N2 C2 96.13(12) . . . . ? N1 Zr N2 C2 -31.03(13) . . . . ? N4 Zr N2 C2 32.35(11) . . . . ? As Zr N2 C2 -142.99(10) . . . . ? N3 Zr N2 Si2 -60.15(11) . . . . ? N1 Zr N2 Si2 172.69(8) . . . . ? N4 Zr N2 Si2 -123.93(10) . . . . ? As Zr N2 Si2 60.73(10) . . . . ? N1 Zr N3 C3 99.22(12) . . . . ? N2 Zr N3 C3 -29.61(13) . . . . ? N4 Zr N3 C3 33.62(11) . . . . ? As Zr N3 C3 -154.63(10) . . . . ? N1 Zr N3 Si3 -64.85(11) . . . . ? N2 Zr N3 Si3 166.32(9) . . . . ? N4 Zr N3 Si3 -130.45(10) . . . . ? As Zr N3 Si3 41.30(10) . . . . ? N3 Zr N4 C5 -123.55(12) . . . . ? N1 Zr N4 C5 119.15(12) . . . . ? N2 Zr N4 C5 -2.35(11) . . . . ? As Zr N4 C5 144.9(2) . . . . ? N3 Zr N4 C4 116.10(12) . . . . ? N1 Zr N4 C4 -1.19(11) . . . . ? N2 Zr N4 C4 -122.70(12) . . . . ? As Zr N4 C4 24.6(3) . . . . ? N3 Zr N4 C6 -3.54(11) . . . . ? N1 Zr N4 C6 -120.83(12) . . . . ? N2 Zr N4 C6 117.67(12) . . . . ? As Zr N4 C6 -95.1(3) . . . . ? C1 N1 Si1 C8 77.17(17) . . . . ? Zr N1 Si1 C8 -106.00(14) . . . . ? C1 N1 Si1 C9 -161.62(14) . . . . ? Zr N1 Si1 C9 15.21(14) . . . . ? C1 N1 Si1 C7 -43.78(17) . . . . ? Zr N1 Si1 C7 133.05(13) . . . . ? C2 N2 Si2 C10 -166.97(12) . . . . ? Zr N2 Si2 C10 -11.11(12) . . . . ? C2 N2 Si2 C11 71.92(15) . . . . ? Zr N2 Si2 C11 -132.21(11) . . . . ? C2 N2 Si2 C12 -48.04(15) . . . . ? Zr N2 Si2 C12 107.83(11) . . . . ? C3 N3 Si3 C13 89.72(14) . . . . ? Zr N3 Si3 C13 -106.72(11) . . . . ? C3 N3 Si3 C14 -29.69(15) . . . . ? Zr N3 Si3 C14 133.87(11) . . . . ? C3 N3 Si3 C15 -147.26(13) . . . . ? Zr N3 Si3 C15 16.30(12) . . . . ? Si1 N1 C1 C4 117.30(15) . . . . ? Zr N1 C1 C4 -60.06(17) . . . . ? Si2 N2 C2 C5 99.07(16) . . . . ? Zr N2 C2 C5 -59.65(17) . . . . ? Si3 N3 C3 C6 104.72(14) . . . . ? Zr N3 C3 C6 -61.17(16) . . . . ? C5 N4 C4 C1 -145.04(16) . . . . ? C6 N4 C4 C1 88.12(18) . . . . ? Zr N4 C4 C1 -27.60(17) . . . . ? N1 C1 C4 N4 55.5(2) . . . . ? C4 N4 C5 C2 90.97(17) . . . . ? C6 N4 C5 C2 -142.15(15) . . . . ? Zr N4 C5 C2 -25.90(16) . . . . ? N2 C2 C5 N4 53.55(19) . . . . ? C5 N4 C6 C3 91.94(17) . . . . ? C4 N4 C6 C3 -141.19(15) . . . . ? Zr N4 C6 C3 -25.17(16) . . . . ? N3 C3 C6 N4 54.09(19) . . . . ? C31 As C21 C26 134.09(13) . . . . ? Zr As C21 C26 -103.27(13) . . . . ? C31 As C21 C22 -45.57(16) . . . . ? Zr As C21 C22 77.08(15) . . . . ? C26 C21 C22 C23 0.8(3) . . . . ? As C21 C22 C23 -179.56(14) . . . . ? C21 C22 C23 C24 -0.3(3) . . . . ? C22 C23 C24 C25 0.1(3) . . . . ? C23 C24 C25 C26 -0.4(3) . . . . ? C24 C25 C26 C21 0.9(3) . . . . ? C22 C21 C26 C25 -1.1(3) . . . . ? As C21 C26 C25 179.27(14) . . . . ? C21 As C31 C32 143.39(14) . . . . ? Zr As C31 C32 19.87(15) . . . . ? C21 As C31 C36 -47.26(14) . . . . ? Zr As C31 C36 -170.78(11) . . . . ? C36 C31 C32 C33 -1.7(3) . . . . ? As C31 C32 C33 167.85(14) . . . . ? C31 C32 C33 C34 1.0(3) . . . . ? C32 C33 C34 C35 0.5(3) . . . . ? C33 C34 C35 C36 -1.2(3) . . . . ? C34 C35 C36 C31 0.5(3) . . . . ? C32 C31 C36 C35 1.0(2) . . . . ? As C31 C36 C35 -168.73(13) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.86 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.525 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.066