Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Malcolm Chisholm' 'Judith Gallucci' 'Khamphee Phomphrai' _publ_contact_author_name 'Prof Malcolm Chisholm' _publ_contact_author_address ; Department of Chemistry The Ohio State University 100 W. 18th Ave. Columbus Ohio 43210 UNITED STATES OF AMERICA ; _publ_contact_author_email 'CHISHOLM@CHEMISTRY.OHIO-STATE.EDU' _publ_requested_journal 'Chemical Communications' _publ_section_title ; Lactide Polymerization by Well-Defined Calcium Coordination Complexes: Comparisons with Related Magnesium and Zinc Chemistry. ; data_Chisholm1047 _database_code_CSD 192309 _audit_creation_method SHELXL-93 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C33 H51 B Ca N6 O' _chemical_formula_weight 598.69 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ca' 'Ca' 0.2262 0.3064 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.1765(1) _cell_length_b 11.7374(1) _cell_length_c 20.8849(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.690(1) _cell_angle_gamma 90.00 _cell_volume 3480.34(5) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description chunk _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.143 _exptl_crystal_density_method ? _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 0.214 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ;The absorption correction is inherent in the scaling and merging of the data. This was done by Scalepack and the scale factor range for the frames is 9.52-10.14. ; _diffrn_ambient_temperature 200(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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60025 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7975 _reflns_number_observed 6389 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ;The methyl group hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5 * Ueq(bonded C atom). For each methyl group, the torsion angle which defines its orientation about the C-C bond was refined. The other hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(bonded atom). Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+1.0612P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7975 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_obs 0.0406 _refine_ls_wR_factor_all 0.1102 _refine_ls_wR_factor_obs 0.1026 _refine_ls_goodness_of_fit_all 1.040 _refine_ls_goodness_of_fit_obs 1.087 _refine_ls_restrained_S_all 1.040 _refine_ls_restrained_S_obs 1.087 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.334 _refine_diff_density_min -0.248 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ca Ca 0.29283(2) 0.10530(2) 0.124037(13) 0.02949(9) Uani 1 d . . O O 0.32007(7) 0.04271(9) 0.22372(5) 0.0373(2) Uani 1 d . . N1 N 0.20635(8) 0.28265(10) 0.08701(6) 0.0326(3) Uani 1 d . . N2 N 0.19051(9) 0.30702(11) 0.01944(6) 0.0351(3) Uani 1 d . . N3 N 0.19389(8) 0.03623(10) 0.01226(6) 0.0326(3) Uani 1 d . . N4 N 0.17897(9) 0.11431(10) -0.03936(6) 0.0338(3) Uani 1 d . . N5 N 0.38442(8) 0.16570(10) 0.05640(6) 0.0327(3) Uani 1 d . . N6 N 0.33280(9) 0.22286(10) -0.00247(6) 0.0329(3) Uani 1 d . . C1 C 0.16624(10) 0.36765(13) 0.11019(8) 0.0359(3) Uani 1 d . . C2 C 0.12422(13) 0.44516(14) 0.05780(10) 0.0485(4) Uani 1 d . . H2 H 0.09067(13) 0.51240(14) 0.06018(10) 0.058 Uiso 1 calc R . C3 C 0.14156(13) 0.40379(14) 0.00215(9) 0.0467(4) Uani 1 d . . H3 H 0.12191(13) 0.43839(14) -0.04178(9) 0.056 Uiso 1 calc R . C4 C 0.15162(10) -0.06016(13) -0.01703(8) 0.0348(3) Uani 1 d . . C5 C 0.10870(12) -0.0441(2) -0.08736(8) 0.0477(4) Uani 1 d . . H5 H 0.07344(12) -0.0982(2) -0.12026(8) 0.057 Uiso 1 calc R . C6 C 0.12808(11) 0.0662(2) -0.09899(8) 0.0429(4) Uani 1 d . . H6 H 0.10856(11) 0.1026(2) -0.14238(8) 0.051 Uiso 1 calc R . C7 C 0.47362(10) 0.16373(12) 0.05810(7) 0.0318(3) Uani 1 d . . C8 C 0.47953(11) 0.21981(14) 0.00087(8) 0.0391(3) Uani 1 d . . H8 H 0.53439(11) 0.23122(14) -0.01028(8) 0.047 Uiso 1 calc R . C9 C 0.38993(11) 0.25496(13) -0.03586(7) 0.0374(3) Uani 1 d . . H9 H 0.37119(11) 0.29535(13) -0.07797(7) 0.045 Uiso 1 calc R . C10 C 0.16527(12) 0.37088(14) 0.18247(9) 0.0419(4) Uani 1 d . . C11 C 0.15906(15) 0.4943(2) 0.20390(11) 0.0586(5) Uani 1 d . . H11A H 0.1581(10) 0.4959(2) 0.2506(3) 0.088 Uiso 1 calc R . H11B H 0.1013(5) 0.5292(4) 0.1725(4) 0.088 Uiso 1 calc R . H11C H 0.2138(5) 0.5369(3) 0.2024(7) 0.088 Uiso 1 calc R . C12 C 0.0776(2) 0.3064(2) 0.18310(12) 0.0668(6) Uani 1 d . . H12A H 0.0732(6) 0.3117(12) 0.2287(2) 0.100 Uiso 1 calc R . H12B H 0.0823(5) 0.2262(3) 0.1717(8) 0.100 Uiso 1 calc R . H12C H 0.0212(2) 0.3402(9) 0.1493(6) 0.100 Uiso 1 calc R . C13 C 0.25304(15) 0.3167(2) 0.23326(9) 0.0621(5) Uani 1 d . . H13A H 0.2541(6) 0.3295(11) 0.27992(10) 0.093 Uiso 1 calc R . H13B H 0.30908(15) 0.3511(9) 0.2282(5) 0.093 Uiso 1 calc R . H13C H 0.2525(5) 0.2347(3) 0.2244(5) 0.093 Uiso 1 calc R . C14 C 0.15392(11) -0.16703(13) 0.02374(8) 0.0401(4) Uani 1 d . . C15 C 0.05727(14) -0.1872(2) 0.02921(12) 0.0625(5) Uani 1 d . . H15A H 0.0594(3) -0.2561(7) 0.0562(7) 0.094 Uiso 1 calc R . H15B H 0.0101(2) -0.1967(13) -0.01672(13) 0.094 Uiso 1 calc R . H15C H 0.0404(5) -0.1217(6) 0.0516(7) 0.094 Uiso 1 calc R . C16 C 0.22778(14) -0.1581(2) 0.09526(9) 0.0557(5) Uani 1 d . . H16A H 0.2314(7) -0.2305(4) 0.1194(3) 0.084 Uiso 1 calc R . H16B H 0.2103(5) -0.0970(8) 0.1205(3) 0.084 Uiso 1 calc R . H16C H 0.2892(2) -0.1409(12) 0.09191(9) 0.084 Uiso 1 calc R . C17 C 0.1796(2) -0.2678(2) -0.01305(12) 0.0643(6) Uani 1 d . . H17A H 0.1822(11) -0.3378(3) 0.0132(4) 0.096 Uiso 1 calc R . H17B H 0.2412(5) -0.2541(6) -0.0170(7) 0.096 Uiso 1 calc R . H17C H 0.1318(6) -0.2761(8) -0.0588(3) 0.096 Uiso 1 calc R . C18 C 0.55104(11) 0.10724(13) 0.11636(8) 0.0374(3) Uani 1 d . . C19 C 0.58214(14) 0.1874(2) 0.17806(9) 0.0559(5) Uani 1 d . . H19A H 0.6300(7) 0.1496(5) 0.2167(2) 0.084 Uiso 1 calc R . H19B H 0.5277(2) 0.2069(10) 0.1908(5) 0.084 Uiso 1 calc R . H19C H 0.6086(9) 0.2570(5) 0.1663(3) 0.084 Uiso 1 calc R . C20 C 0.51549(12) -0.00456(14) 0.13615(9) 0.0460(4) Uani 1 d . . H20A H 0.4669(6) 0.0118(2) 0.1557(6) 0.069 Uiso 1 calc R . H20B H 0.5680(2) -0.0447(5) 0.1701(5) 0.069 Uiso 1 calc R . H20C H 0.4888(8) -0.0524(5) 0.09539(14) 0.069 Uiso 1 calc R . C21 C 0.63449(13) 0.0801(2) 0.09379(11) 0.0641(6) Uani 1 d . . H21A H 0.6835(5) 0.0408(12) 0.1309(3) 0.096 Uiso 1 calc R . H21B H 0.6600(7) 0.1512(2) 0.0828(8) 0.096 Uiso 1 calc R . H21C H 0.6133(3) 0.0311(11) 0.0532(5) 0.096 Uiso 1 calc R . C22 C 0.33216(10) 0.01141(12) 0.28755(7) 0.0307(3) Uani 1 d . . C23 C 0.25513(11) -0.02480(13) 0.30550(7) 0.0361(3) Uani 1 d . . C24 C 0.27044(12) -0.05645(14) 0.37282(8) 0.0411(4) Uani 1 d . . H24 H 0.21836(12) -0.07976(14) 0.38483(8) 0.049 Uiso 1 calc R . C25 C 0.35877(12) -0.05493(14) 0.42238(8) 0.0422(4) Uani 1 d . . H25 H 0.36762(12) -0.07730(14) 0.46795(8) 0.051 Uiso 1 calc R . C26 C 0.43455(11) -0.02047(13) 0.40512(7) 0.0375(3) Uani 1 d . . H26 H 0.49572(11) -0.01990(13) 0.43927(7) 0.045 Uiso 1 calc R . C27 C 0.42328(10) 0.01338(12) 0.33895(7) 0.0314(3) Uani 1 d . . C28 C 0.15649(11) -0.0343(2) 0.25273(8) 0.0473(4) Uani 1 d . . H28 H 0.15714(11) 0.0012(2) 0.20936(8) 0.057 Uiso 1 calc R . C29 C 0.08479(13) 0.0305(2) 0.27500(10) 0.0642(6) Uani 1 d . . H29A H 0.1052(6) 0.1097(4) 0.2852(8) 0.096 Uiso 1 calc R . H29B H 0.0800(8) -0.0054(8) 0.3160(5) 0.096 Uiso 1 calc R . H29C H 0.0232(3) 0.0286(11) 0.2381(3) 0.096 Uiso 1 calc R . C30 C 0.12822(15) -0.1587(2) 0.23770(10) 0.0649(6) Uani 1 d . . H30A H 0.0667(5) -0.1631(2) 0.2007(5) 0.097 Uiso 1 calc R . H30B H 0.1243(11) -0.1948(4) 0.2789(2) 0.097 Uiso 1 calc R . H30C H 0.1754(6) -0.1982(4) 0.2238(8) 0.097 Uiso 1 calc R . C31 C 0.50675(11) 0.05504(14) 0.32167(8) 0.0381(3) Uani 1 d . . H31 H 0.49139(11) 0.04312(14) 0.27148(8) 0.046 Uiso 1 calc R . C32 C 0.5212(2) 0.1811(2) 0.33530(14) 0.0782(7) Uani 1 d . . H32A H 0.5710(9) 0.2083(4) 0.3194(8) 0.117 Uiso 1 calc R . H32B H 0.5396(12) 0.1953(2) 0.3845(2) 0.117 Uiso 1 calc R . H32C H 0.4625(4) 0.2217(2) 0.3109(7) 0.117 Uiso 1 calc R . C33 C 0.5971(2) -0.0092(3) 0.3587(2) 0.1045(11) Uani 1 d . . H33A H 0.6478(4) 0.0207(14) 0.3447(10) 0.157 Uiso 1 calc R . H33B H 0.5879(5) -0.0903(4) 0.3472(10) 0.157 Uiso 1 calc R . H33C H 0.6140(9) 0.0006(17) 0.4082(2) 0.157 Uiso 1 calc R . B B 0.22475(12) 0.23348(15) -0.02879(8) 0.0348(4) Uani 1 d . . H1B H 0.20462(12) 0.27222(15) -0.07435(8) 0.042 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca 0.03143(15) 0.0348(2) 0.02264(14) 0.00428(11) 0.01006(11) 0.00012(12) O 0.0404(6) 0.0481(6) 0.0237(5) 0.0066(4) 0.0116(4) 0.0002(5) N1 0.0336(6) 0.0335(6) 0.0313(6) 0.0009(5) 0.0123(5) -0.0003(5) N2 0.0384(7) 0.0331(6) 0.0333(6) 0.0066(5) 0.0121(5) 0.0028(5) N3 0.0360(6) 0.0333(6) 0.0279(6) 0.0006(5) 0.0106(5) -0.0014(5) N4 0.0359(6) 0.0386(7) 0.0253(6) 0.0032(5) 0.0089(5) 0.0013(5) N5 0.0351(6) 0.0360(7) 0.0283(6) 0.0056(5) 0.0131(5) 0.0012(5) N6 0.0393(7) 0.0343(6) 0.0262(6) 0.0055(5) 0.0128(5) 0.0000(5) C1 0.0316(7) 0.0327(8) 0.0449(8) -0.0045(6) 0.0154(6) -0.0043(6) C2 0.0535(10) 0.0343(8) 0.0614(11) 0.0045(8) 0.0246(9) 0.0099(8) C3 0.0527(10) 0.0375(9) 0.0487(10) 0.0124(7) 0.0165(8) 0.0105(8) C4 0.0316(7) 0.0379(8) 0.0362(8) -0.0065(6) 0.0137(6) -0.0023(6) C5 0.0495(10) 0.0532(10) 0.0355(8) -0.0112(7) 0.0088(7) -0.0129(8) C6 0.0415(9) 0.0562(10) 0.0261(7) -0.0010(7) 0.0058(6) -0.0028(8) C7 0.0366(7) 0.0322(7) 0.0296(7) -0.0031(6) 0.0153(6) -0.0037(6) C8 0.0417(9) 0.0457(9) 0.0350(8) 0.0011(7) 0.0197(7) -0.0083(7) C9 0.0481(9) 0.0386(8) 0.0287(7) 0.0035(6) 0.0176(7) -0.0070(7) C10 0.0426(9) 0.0418(9) 0.0467(9) -0.0097(7) 0.0224(7) -0.0054(7) C11 0.0649(12) 0.0513(11) 0.0671(12) -0.0212(9) 0.0324(10) -0.0058(9) C12 0.0728(14) 0.0722(14) 0.0727(14) -0.0185(11) 0.0471(12) -0.0263(11) C13 0.0722(13) 0.0745(14) 0.0391(10) -0.0067(9) 0.0191(9) 0.0147(11) C14 0.0443(9) 0.0338(8) 0.0472(9) -0.0047(7) 0.0223(7) -0.0052(7) C15 0.0558(11) 0.0612(12) 0.0816(14) 0.0034(11) 0.0383(11) -0.0087(10) C16 0.0667(12) 0.0424(10) 0.0515(10) 0.0119(8) 0.0128(9) -0.0055(9) C17 0.089(2) 0.0384(10) 0.0797(14) -0.0077(9) 0.0478(13) -0.0008(10) C18 0.0352(8) 0.0410(8) 0.0370(8) 0.0046(6) 0.0141(6) 0.0025(7) C19 0.0613(12) 0.0521(11) 0.0399(9) 0.0029(8) 0.0002(8) -0.0030(9) C20 0.0489(9) 0.0424(9) 0.0472(9) 0.0090(7) 0.0178(8) 0.0065(8) C21 0.0449(10) 0.088(2) 0.0673(13) 0.0225(11) 0.0296(10) 0.0166(10) C22 0.0377(8) 0.0305(7) 0.0243(6) 0.0029(5) 0.0115(6) 0.0025(6) C23 0.0363(8) 0.0425(8) 0.0286(7) 0.0048(6) 0.0104(6) -0.0006(7) C24 0.0447(9) 0.0489(9) 0.0329(8) 0.0081(7) 0.0177(7) -0.0036(7) C25 0.0524(10) 0.0492(9) 0.0246(7) 0.0085(7) 0.0131(7) -0.0027(8) C26 0.0399(8) 0.0422(8) 0.0259(7) 0.0008(6) 0.0060(6) 0.0002(7) C27 0.0364(7) 0.0314(7) 0.0273(7) -0.0007(6) 0.0126(6) 0.0018(6) C28 0.0374(8) 0.0704(12) 0.0340(8) 0.0090(8) 0.0123(7) -0.0044(8) C29 0.0417(10) 0.096(2) 0.0549(11) 0.0153(11) 0.0167(9) 0.0106(10) C30 0.0552(11) 0.085(2) 0.0513(11) -0.0084(11) 0.0143(9) -0.0230(11) C31 0.0356(8) 0.0515(9) 0.0281(7) -0.0057(7) 0.0125(6) -0.0018(7) C32 0.085(2) 0.0718(14) 0.104(2) -0.0380(13) 0.0662(15) -0.0413(12) C33 0.0558(14) 0.154(3) 0.121(2) 0.055(2) 0.052(2) 0.043(2) B 0.0400(9) 0.0370(9) 0.0265(8) 0.0086(7) 0.0107(7) 0.0034(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 Ca O 2.1064(10) . ? Ca N5 2.4119(12) . ? Ca N3 2.4258(12) . ? Ca N1 2.4365(12) . ? O C22 1.331(2) . ? N1 C1 1.345(2) . ? N1 N2 1.375(2) . ? N2 C3 1.335(2) . ? N2 B 1.549(2) . ? N3 C4 1.337(2) . ? N3 N4 1.372(2) . ? N4 C6 1.337(2) . ? N4 B 1.543(2) . ? N5 C7 1.342(2) . ? N5 N6 1.377(2) . ? N6 C9 1.344(2) . ? N6 B 1.539(2) . ? C1 C2 1.392(2) . ? C1 C10 1.515(2) . ? C2 C3 1.368(2) . ? C2 H2 0.95 . ? C3 H3 0.95 . ? C4 C5 1.393(2) . ? C4 C14 1.509(2) . ? C5 C6 1.368(2) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 C8 1.395(2) . ? C7 C18 1.513(2) . ? C8 C9 1.368(2) . ? C8 H8 0.95 . ? C9 H9 0.95 . ? C10 C13 1.518(3) . ? C10 C11 1.529(2) . ? C10 C12 1.535(2) . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 C16 1.522(2) . ? C14 C15 1.529(2) . ? C14 C17 1.534(2) . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 C19 1.529(2) . ? C18 C20 1.530(2) . ? C18 C21 1.533(2) . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 C23 1.413(2) . ? C22 C27 1.420(2) . ? C23 C24 1.392(2) . ? C23 C28 1.517(2) . ? C24 C25 1.374(2) . ? C24 H24 0.95 . ? C25 C26 1.382(2) . ? C25 H25 0.95 . ? C26 C27 1.389(2) . ? C26 H26 0.95 . ? C27 C31 1.516(2) . ? C28 C30 1.523(3) . ? C28 C29 1.528(3) . ? C28 H28 1.00 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C30 H30A 0.98 . ? C30 H30B 0.98 . ? C30 H30C 0.98 . ? C31 C32 1.508(3) . ? C31 C33 1.515(3) . ? C31 H31 1.00 . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? B H1B 1.00 . ? 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 O Ca N5 136.79(4) . . ? O Ca N3 132.31(4) . . ? N5 Ca N3 79.84(4) . . ? O Ca N1 120.48(4) . . ? N5 Ca N1 85.43(4) . . ? N3 Ca N1 84.22(4) . . ? C22 O Ca 174.43(10) . . ? C1 N1 N2 106.13(12) . . ? C1 N1 Ca 141.37(10) . . ? N2 N1 Ca 112.50(8) . . ? C3 N2 N1 109.47(13) . . ? C3 N2 B 125.49(13) . . ? N1 N2 B 125.04(11) . . ? C4 N3 N4 106.65(11) . . ? C4 N3 Ca 139.18(10) . . ? N4 N3 Ca 114.03(8) . . ? C6 N4 N3 109.29(12) . . ? C6 N4 B 126.82(13) . . ? N3 N4 B 123.54(11) . . ? C7 N5 N6 106.41(11) . . ? C7 N5 Ca 139.84(9) . . ? N6 N5 Ca 113.73(8) . . ? C9 N6 N5 109.39(12) . . ? C9 N6 B 126.37(12) . . ? N5 N6 B 123.83(11) . . ? N1 C1 C2 109.98(14) . . ? N1 C1 C10 122.83(14) . . ? C2 C1 C10 127.13(14) . . ? C3 C2 C1 105.28(14) . . ? C3 C2 H2 127.36(10) . . ? C1 C2 H2 127.36(10) . . ? N2 C3 C2 109.14(15) . . ? N2 C3 H3 125.43(9) . . ? C2 C3 H3 125.43(10) . . ? N3 C4 C5 109.74(14) . . ? N3 C4 C14 122.22(13) . . ? C5 C4 C14 128.03(14) . . ? C6 C5 C4 105.39(14) . . ? C6 C5 H5 127.30(9) . . ? C4 C5 H5 127.30(10) . . ? N4 C6 C5 108.92(14) . . ? N4 C6 H6 125.54(9) . . ? C5 C6 H6 125.54(9) . . ? N5 C7 C8 109.81(13) . . ? N5 C7 C18 121.21(12) . . ? C8 C7 C18 128.98(13) . . ? C9 C8 C7 105.72(13) . . ? C9 C8 H8 127.14(8) . . ? C7 C8 H8 127.14(9) . . ? N6 C9 C8 108.67(13) . . ? N6 C9 H9 125.66(9) . . ? C8 C9 H9 125.66(8) . . ? C1 C10 C13 111.76(14) . . ? C1 C10 C11 109.80(14) . . ? C13 C10 C11 108.8(2) . . ? C1 C10 C12 108.05(14) . . ? C13 C10 C12 109.7(2) . . ? C11 C10 C12 108.74(15) . . ? C10 C11 H11A 109.47(10) . . ? C10 C11 H11B 109.47(11) . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.47(10) . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.47(10) . . ? C10 C12 H12B 109.47(11) . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.47(12) . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.47(9) . . ? C10 C13 H13B 109.47(11) . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.47(10) . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C4 C14 C16 111.00(13) . . ? C4 C14 C15 109.81(14) . . ? C16 C14 C15 109.3(2) . . ? C4 C14 C17 108.53(13) . . ? C16 C14 C17 108.4(2) . . ? C15 C14 C17 109.77(15) . . ? C14 C15 H15A 109.47(10) . . ? C14 C15 H15B 109.47(11) . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.47(10) . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.47(9) . . ? C14 C16 H16B 109.47(10) . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.47(10) . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.47(10) . . ? C14 C17 H17B 109.47(10) . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.47(11) . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C7 C18 C19 109.19(13) . . ? C7 C18 C20 110.20(13) . . ? C19 C18 C20 109.47(14) . . ? C7 C18 C21 109.56(13) . . ? C19 C18 C21 110.1(2) . . ? C20 C18 C21 108.28(15) . . ? C18 C19 H19A 109.47(9) . . ? C18 C19 H19B 109.47(10) . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.47(9) . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.47(9) . . ? C18 C20 H20B 109.47(9) . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.47(9) . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.47(10) . . ? C18 C21 H21B 109.47(11) . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.47(11) . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O C22 C23 120.95(13) . . ? O C22 C27 120.35(12) . . ? C23 C22 C27 118.70(12) . . ? C24 C23 C22 119.32(14) . . ? C24 C23 C28 118.93(14) . . ? C22 C23 C28 121.71(13) . . ? C25 C24 C23 121.84(15) . . ? C25 C24 H24 119.08(9) . . ? C23 C24 H24 119.08(9) . . ? C24 C25 C26 119.20(13) . . ? C24 C25 H25 120.40(9) . . ? C26 C25 H25 120.40(9) . . ? C25 C26 C27 121.46(14) . . ? C25 C26 H26 119.27(9) . . ? C27 C26 H26 119.27(9) . . ? C26 C27 C22 119.48(13) . . ? C26 C27 C31 120.63(13) . . ? C22 C27 C31 119.86(12) . . ? C23 C28 C30 110.7(2) . . ? C23 C28 C29 111.62(15) . . ? C30 C28 C29 111.1(2) . . ? C23 C28 H28 107.73(8) . . ? C30 C28 H28 107.73(10) . . ? C29 C28 H28 107.73(10) . . ? C28 C29 H29A 109.47(11) . . ? C28 C29 H29B 109.47(10) . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.47(10) . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.47(10) . . ? C28 C30 H30B 109.47(10) . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.47(11) . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C33 110.3(2) . . ? C32 C31 C27 110.47(13) . . ? C33 C31 C27 113.5(2) . . ? C32 C31 H31 107.43(12) . . ? C33 C31 H31 107.43(13) . . ? C27 C31 H31 107.43(8) . . ? C31 C32 H32A 109.47(10) . . ? C31 C32 H32B 109.47(12) . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.47(12) . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.47(12) . . ? C31 C33 H33B 109.5(2) . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.47(13) . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N6 B N4 110.29(12) . . ? N6 B N2 111.88(12) . . ? N4 B N2 111.14(12) . . ? N6 B H1B 107.78(7) . . ? N4 B H1B 107.78(7) . . ? N2 B H1B 107.78(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Ca O C22 124.9(10) . . . . ? N3 Ca O C22 -106.8(10) . . . . ? N1 Ca O C22 5.4(10) . . . . ? O Ca N1 C1 2.4(2) . . . . ? N5 Ca N1 C1 -140.9(2) . . . . ? N3 Ca N1 C1 138.9(2) . . . . ? O Ca N1 N2 -176.55(8) . . . . ? N5 Ca N1 N2 40.18(9) . . . . ? N3 Ca N1 N2 -40.04(9) . . . . ? C1 N1 N2 C3 -0.4(2) . . . . ? Ca N1 N2 C3 178.90(11) . . . . ? C1 N1 N2 B 179.34(13) . . . . ? Ca N1 N2 B -1.4(2) . . . . ? O Ca N3 C4 -18.9(2) . . . . ? N5 Ca N3 C4 128.1(2) . . . . ? N1 Ca N3 C4 -145.5(2) . . . . ? O Ca N3 N4 166.27(8) . . . . ? N5 Ca N3 N4 -46.78(9) . . . . ? N1 Ca N3 N4 39.60(9) . . . . ? C4 N3 N4 C6 0.3(2) . . . . ? Ca N3 N4 C6 176.76(10) . . . . ? C4 N3 N4 B -173.41(13) . . . . ? Ca N3 N4 B 3.1(2) . . . . ? O Ca N5 C7 11.2(2) . . . . ? N3 Ca N5 C7 -132.7(2) . . . . ? N1 Ca N5 C7 142.4(2) . . . . ? O Ca N5 N6 -166.92(8) . . . . ? N3 Ca N5 N6 49.17(9) . . . . ? N1 Ca N5 N6 -35.76(9) . . . . ? C7 N5 N6 C9 0.0(2) . . . . ? Ca N5 N6 C9 178.76(9) . . . . ? C7 N5 N6 B 173.05(13) . . . . ? Ca N5 N6 B -8.2(2) . . . . ? N2 N1 C1 C2 0.6(2) . . . . ? Ca N1 C1 C2 -178.36(12) . . . . ? N2 N1 C1 C10 177.98(13) . . . . ? Ca N1 C1 C10 -1.0(2) . . . . ? N1 C1 C2 C3 -0.6(2) . . . . ? C10 C1 C2 C3 -177.8(2) . . . . ? N1 N2 C3 C2 0.0(2) . . . . ? B N2 C3 C2 -179.70(15) . . . . ? C1 C2 C3 N2 0.3(2) . . . . ? N4 N3 C4 C5 -0.6(2) . . . . ? Ca N3 C4 C5 -175.66(12) . . . . ? N4 N3 C4 C14 179.11(13) . . . . ? Ca N3 C4 C14 4.0(2) . . . . ? N3 C4 C5 C6 0.6(2) . . . . ? C14 C4 C5 C6 -179.01(15) . . . . ? N3 N4 C6 C5 0.1(2) . . . . ? B N4 C6 C5 173.55(14) . . . . ? C4 C5 C6 N4 -0.5(2) . . . . ? N6 N5 C7 C8 0.3(2) . . . . ? Ca N5 C7 C8 -177.92(11) . . . . ? N6 N5 C7 C18 179.92(12) . . . . ? Ca N5 C7 C18 1.7(2) . . . . ? N5 C7 C8 C9 -0.5(2) . . . . ? C18 C7 C8 C9 179.93(15) . . . . ? N5 N6 C9 C8 -0.3(2) . . . . ? B N6 C9 C8 -173.16(14) . . . . ? C7 C8 C9 N6 0.5(2) . . . . ? N1 C1 C10 C13 32.7(2) . . . . ? C2 C1 C10 C13 -150.4(2) . . . . ? N1 C1 C10 C11 153.45(15) . . . . ? C2 C1 C10 C11 -29.7(2) . . . . ? N1 C1 C10 C12 -88.1(2) . . . . ? C2 C1 C10 C12 88.8(2) . . . . ? N3 C4 C14 C16 -13.9(2) . . . . ? C5 C4 C14 C16 165.7(2) . . . . ? N3 C4 C14 C15 107.1(2) . . . . ? C5 C4 C14 C15 -73.3(2) . . . . ? N3 C4 C14 C17 -132.9(2) . . . . ? C5 C4 C14 C17 46.7(2) . . . . ? N5 C7 C18 C19 -79.3(2) . . . . ? C8 C7 C18 C19 100.3(2) . . . . ? N5 C7 C18 C20 41.0(2) . . . . ? C8 C7 C18 C20 -139.5(2) . . . . ? N5 C7 C18 C21 160.1(2) . . . . ? C8 C7 C18 C21 -20.4(2) . . . . ? Ca O C22 C23 63.8(10) . . . . ? Ca O C22 C27 -116.5(10) . . . . ? O C22 C23 C24 -179.75(14) . . . . ? C27 C22 C23 C24 0.5(2) . . . . ? O C22 C23 C28 2.5(2) . . . . ? C27 C22 C23 C28 -177.19(15) . . . . ? C22 C23 C24 C25 -0.8(3) . . . . ? C28 C23 C24 C25 176.9(2) . . . . ? C23 C24 C25 C26 0.4(3) . . . . ? C24 C25 C26 C27 0.4(3) . . . . ? C25 C26 C27 C22 -0.7(2) . . . . ? C25 C26 C27 C31 177.73(15) . . . . ? O C22 C27 C26 -179.49(13) . . . . ? C23 C22 C27 C26 0.2(2) . . . . ? O C22 C27 C31 2.0(2) . . . . ? C23 C22 C27 C31 -178.24(13) . . . . ? C24 C23 C28 C30 -69.7(2) . . . . ? C22 C23 C28 C30 108.1(2) . . . . ? C24 C23 C28 C29 54.7(2) . . . . ? C22 C23 C28 C29 -127.6(2) . . . . ? C26 C27 C31 C32 -86.9(2) . . . . ? C22 C27 C31 C32 91.6(2) . . . . ? C26 C27 C31 C33 37.6(2) . . . . ? C22 C27 C31 C33 -143.9(2) . . . . ? C9 N6 B N4 114.6(2) . . . . ? N5 N6 B N4 -57.2(2) . . . . ? C9 N6 B N2 -121.1(2) . . . . ? N5 N6 B N2 67.0(2) . . . . ? C6 N4 B N6 -112.1(2) . . . . ? N3 N4 B N6 60.4(2) . . . . ? C6 N4 B N2 123.2(2) . . . . ? N3 N4 B N2 -64.2(2) . . . . ? C3 N2 B N6 119.3(2) . . . . ? N1 N2 B N6 -60.4(2) . . . . ? C3 N2 B N4 -116.9(2) . . . . ? N1 N2 B N4 63.4(2) . . . . ? #END OF CIF data_Chisholm1052 _database_code_CSD 192310 _audit_creation_method SHELXL-93 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C42 H74 Ca N3 O Si2' _chemical_formula_weight 733.30 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ca' 'Ca' 0.2262 0.3064 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9120(1) _cell_length_b 13.2215(1) _cell_length_c 16.8877(1) _cell_angle_alpha 70.150(1) _cell_angle_beta 80.422(1) _cell_angle_gamma 63.507(1) _cell_volume 2238.64(3) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description chunk _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.088 _exptl_crystal_density_method ? _exptl_crystal_F_000 806 _exptl_absorpt_coefficient_mu 0.226 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ;The absorption correction is inherent in the scaling and merging of the data. This was done by Scalepack and the scale factor range for the frames is 9.57-10.19. The asymmetric unit contains the Ca complex and a half molecule of hexane, which occupies an inversion center. ; _diffrn_ambient_temperature 200(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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47522 _diffrn_reflns_av_R_equivalents 0.028 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10257 _reflns_number_observed 8070 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ;There are two disordered regions in this structure. The THF ligand has one carbon atom, C32, which is disordered over two sites. The hexane molecule has two carbon atoms, C40 and C42, which are each disordered over two sites. The hexane carbon atoms are refined only isotropically. The methyl group hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5 * Ueq(bonded C atom). For each methyl group, the torsion angle which defines its orientation about the Si-C or C-C bond was refined. The other hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(bonded atom). Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0660P)^2^+0.9247P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10257 _refine_ls_number_parameters 456 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_obs 0.0479 _refine_ls_wR_factor_all 0.1362 _refine_ls_wR_factor_obs 0.1261 _refine_ls_goodness_of_fit_all 1.044 _refine_ls_goodness_of_fit_obs 1.095 _refine_ls_restrained_S_all 1.044 _refine_ls_restrained_S_obs 1.095 _refine_ls_shift/esd_max -0.034 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.912 _refine_diff_density_min -0.683 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ca Ca 0.26182(3) -0.16945(3) 0.27374(2) 0.02928(10) Uani 1 d . . Si1 Si 0.23895(5) 0.10911(4) 0.21172(3) 0.03689(13) Uani 1 d . . Si2 Si 0.31878(7) -0.01568(6) 0.38835(4) 0.0526(2) Uani 1 d . . O O 0.24253(13) -0.29106(13) 0.40985(8) 0.0455(3) Uani 1 d . . N1 N 0.38798(12) -0.27563(12) 0.18063(8) 0.0283(3) Uani 1 d . . N2 N 0.10621(12) -0.19548(12) 0.22234(8) 0.0279(3) Uani 1 d . . N3 N 0.28222(14) -0.01500(13) 0.29566(9) 0.0347(3) Uani 1 d . . C1 C 0.3415(2) -0.24174(14) 0.10491(10) 0.0297(3) Uani 1 d . . C2 C 0.2125(2) -0.18695(15) 0.08669(10) 0.0310(3) Uani 1 d . . H2 H 0.1943(2) -0.15075(15) 0.02843(10) 0.037 Uiso 1 calc R . C3 C 0.1056(2) -0.17660(14) 0.14004(10) 0.0287(3) Uani 1 d . . C4 C 0.4286(2) -0.2607(2) 0.02928(12) 0.0436(5) Uani 1 d . . H4A H 0.4353(11) -0.1866(4) -0.0034(5) 0.065 Uiso 1 calc R . H4B H 0.3947(7) -0.2855(13) -0.0061(5) 0.065 Uiso 1 calc R . H4C H 0.5118(4) -0.3223(9) 0.04872(12) 0.065 Uiso 1 calc R . C5 C -0.0135(2) -0.1420(2) 0.09667(12) 0.0396(4) Uani 1 d . . H5A H 0.0078(2) -0.1738(11) 0.0489(5) 0.059 Uiso 1 calc R . H5B H -0.0576(7) -0.0554(2) 0.0764(8) 0.059 Uiso 1 calc R . H5C H -0.0677(6) -0.1743(11) 0.1367(3) 0.059 Uiso 1 calc R . C6 C 0.5185(2) -0.35322(15) 0.19484(10) 0.0317(4) Uani 1 d . . C7 C 0.5557(2) -0.4769(2) 0.21935(12) 0.0420(4) Uani 1 d . . C8 C 0.6823(2) -0.5517(2) 0.23662(14) 0.0531(6) Uani 1 d . . H8 H 0.7086(2) -0.6350(2) 0.25283(14) 0.064 Uiso 1 calc R . C9 C 0.7692(2) -0.5082(2) 0.23080(14) 0.0554(6) Uani 1 d . . H9 H 0.8547(2) -0.5609(2) 0.24248(14) 0.067 Uiso 1 calc R . C10 C 0.7322(2) -0.3883(2) 0.20806(13) 0.0492(5) Uani 1 d . . H10 H 0.7930(2) -0.3589(2) 0.20497(13) 0.059 Uiso 1 calc R . C11 C 0.6078(2) -0.3081(2) 0.18930(11) 0.0371(4) Uani 1 d . . C12 C 0.4629(2) -0.5292(2) 0.2251(2) 0.0608(6) Uani 1 d . . H12 H 0.3765(2) -0.4659(2) 0.2271(2) 0.073 Uiso 1 calc R . C13 C 0.4798(3) -0.6331(2) 0.3051(2) 0.0874(10) Uani 1 d . . H13A H 0.4759(23) -0.6083(7) 0.3543(2) 0.131 Uiso 1 calc R . H13B H 0.5614(10) -0.6989(8) 0.3026(7) 0.131 Uiso 1 calc R . H13C H 0.4129(14) -0.6588(14) 0.3095(8) 0.131 Uiso 1 calc R . C14 C 0.4727(3) -0.5684(3) 0.1483(2) 0.0841(9) Uani 1 d . . H14A H 0.4098(15) -0.5990(19) 0.1532(7) 0.126 Uiso 1 calc R . H14B H 0.5567(8) -0.6307(15) 0.1451(9) 0.126 Uiso 1 calc R . H14C H 0.4579(22) -0.5006(5) 0.0974(3) 0.126 Uiso 1 calc R . C15 C 0.5761(2) -0.1772(2) 0.16294(14) 0.0444(5) Uani 1 d . . H15 H 0.4830(2) -0.1322(2) 0.15726(14) 0.053 Uiso 1 calc R . C16 C 0.6380(3) -0.1391(2) 0.0773(2) 0.0682(7) Uani 1 d . . H16A H 0.6146(15) -0.0538(4) 0.0609(6) 0.102 Uiso 1 calc R . H16B H 0.6094(15) -0.1570(16) 0.0347(3) 0.102 Uiso 1 calc R . H16C H 0.7294(3) -0.1823(13) 0.0818(4) 0.102 Uiso 1 calc R . C17 C 0.6173(2) -0.1458(2) 0.2285(2) 0.0659(7) Uani 1 d . . H17A H 0.5925(16) -0.0602(3) 0.2110(6) 0.099 Uiso 1 calc R . H17B H 0.7086(3) -0.1878(14) 0.2339(9) 0.099 Uiso 1 calc R . H17C H 0.5772(14) -0.1694(16) 0.2829(3) 0.099 Uiso 1 calc R . C18 C 0.0011(2) -0.20432(15) 0.27484(10) 0.0296(3) Uani 1 d . . C19 C -0.1011(2) -0.1034(2) 0.28827(11) 0.0333(4) Uani 1 d . . C20 C -0.1920(2) -0.1180(2) 0.34893(12) 0.0399(4) Uani 1 d . . H20 H -0.2600(2) -0.0500(2) 0.35909(12) 0.048 Uiso 1 calc R . C21 C -0.1854(2) -0.2288(2) 0.39445(13) 0.0459(5) Uani 1 d . . H21 H -0.2478(2) -0.2372(2) 0.43592(13) 0.055 Uiso 1 calc R . C22 C -0.0872(2) -0.3275(2) 0.37914(12) 0.0435(4) Uani 1 d . . H22 H -0.0842(2) -0.4037(2) 0.40946(12) 0.052 Uiso 1 calc R . C23 C 0.0078(2) -0.3186(2) 0.32048(11) 0.0345(4) Uani 1 d . . C24 C -0.1153(2) 0.0217(2) 0.23907(13) 0.0419(4) Uani 1 d . . H24 H -0.0464(2) 0.0153(2) 0.19560(13) 0.050 Uiso 1 calc R . C25 C -0.1015(2) 0.0838(2) 0.2952(2) 0.0623(6) Uani 1 d . . H25A H -0.0189(7) 0.0382(9) 0.3213(9) 0.093 Uiso 1 calc R . H25B H -0.1671(11) 0.0900(15) 0.3393(7) 0.093 Uiso 1 calc R . H25C H -0.1097(17) 0.1633(6) 0.2614(3) 0.093 Uiso 1 calc R . C26 C -0.2401(2) 0.0959(2) 0.1929(2) 0.0583(6) Uani 1 d . . H26A H -0.2493(8) 0.0532(7) 0.1587(9) 0.087 Uiso 1 calc R . H26B H -0.2415(7) 0.1720(7) 0.1564(9) 0.087 Uiso 1 calc R . H26C H -0.3095(2) 0.1098(13) 0.2341(2) 0.087 Uiso 1 calc R . C27 C 0.1165(2) -0.4286(2) 0.30627(12) 0.0406(4) Uani 1 d . . H27 H 0.1941(2) -0.4148(2) 0.29874(12) 0.049 Uiso 1 calc R . C28 C 0.1016(2) -0.4503(2) 0.2261(2) 0.0568(6) Uani 1 d . . H28A H 0.1753(8) -0.5197(9) 0.2177(6) 0.085 Uiso 1 calc R . H28B H 0.0936(16) -0.3807(6) 0.1777(2) 0.085 Uiso 1 calc R . H28C H 0.0262(9) -0.4644(15) 0.2313(5) 0.085 Uiso 1 calc R . C29 C 0.1385(2) -0.5415(2) 0.3804(2) 0.0644(7) Uani 1 d . . H29A H 0.2176(9) -0.6058(5) 0.3712(6) 0.097 Uiso 1 calc R . H29B H 0.0693(9) -0.5641(10) 0.3846(8) 0.097 Uiso 1 calc R . H29C H 0.1427(18) -0.5268(5) 0.4327(2) 0.097 Uiso 1 calc R . C30 C 0.3279(2) -0.4109(2) 0.4516(2) 0.0625(6) Uani 1 d . . H30A H 0.4147(2) -0.4178(2) 0.4473(2) 0.075 Uiso 1 calc R . H30B H 0.3255(2) -0.4667(2) 0.4257(2) 0.075 Uiso 1 calc R . C31 C 0.2855(3) -0.4379(3) 0.5417(2) 0.0886(10) Uani 1 d . . H31A H 0.3026(3) -0.5227(3) 0.5663(2) 0.106 Uiso 0.568(14) calc PR 1 H31B H 0.3269(3) -0.4168(3) 0.5758(2) 0.106 Uiso 0.568(14) calc PR 1 H31C H 0.3558(3) -0.4660(3) 0.5792(2) 0.106 Uiso 0.432(14) calc PR 2 H31D H 0.2547(3) -0.5003(3) 0.5556(2) 0.106 Uiso 0.432(14) calc PR 2 C32A C 0.1543(5) -0.3646(7) 0.5363(4) 0.068(2) Uani 0.568(14) d P 1 H32A H 0.1207(5) -0.3477(7) 0.5903(4) 0.082 Uiso 0.568(14) calc PR 1 H32B H 0.1094(5) -0.4043(7) 0.5231(4) 0.082 Uiso 0.568(14) calc PR 1 C32B C 0.1764(8) -0.3191(9) 0.5532(4) 0.063(3) Uani 0.432(14) d P 2 H32C H 0.1069(8) -0.3337(9) 0.5887(4) 0.075 Uiso 0.432(14) calc PR 2 H32D H 0.2073(8) -0.2787(9) 0.5782(4) 0.075 Uiso 0.432(14) calc PR 2 C33 C 0.1377(2) -0.2512(2) 0.46663(13) 0.0545(5) Uani 1 d . . H33A H 0.0565(2) -0.2156(2) 0.43839(13) 0.065 Uiso 0.568(14) calc PR 1 H33B H 0.1427(2) -0.1926(2) 0.48844(13) 0.065 Uiso 0.568(14) calc PR 1 H33C H 0.0663(2) -0.2622(2) 0.45419(13) 0.065 Uiso 0.432(14) calc PR 2 H33D H 0.1102(2) -0.1658(2) 0.45859(13) 0.065 Uiso 0.432(14) calc PR 2 C34 C 0.1772(2) 0.0836(2) 0.12783(13) 0.0479(5) Uani 1 d . . H34A H 0.1095(2) 0.0586(2) 0.15171(13) 0.072 Uiso 1 calc R . H34B H 0.2451(2) 0.0217(2) 0.10688(13) 0.072 Uiso 1 calc R . H34C H 0.1449(2) 0.1572(2) 0.08128(13) 0.072 Uiso 1 calc R . C35 C 0.1134(2) 0.2446(2) 0.2367(2) 0.0618(6) Uani 1 d . . H35A H 0.0428(2) 0.2271(2) 0.2656(2) 0.093 Uiso 1 calc R . H35B H 0.0845(2) 0.3096(2) 0.1843(2) 0.093 Uiso 1 calc R . H35C H 0.1475(2) 0.2678(2) 0.2731(2) 0.093 Uiso 1 calc R . C36 C 0.3667(2) 0.1560(2) 0.15701(15) 0.0530(5) Uani 1 d . . H36A H 0.4363(2) 0.0894(2) 0.14183(15) 0.079 Uiso 1 calc R . H36B H 0.3966(2) 0.1806(2) 0.19475(15) 0.079 Uiso 1 calc R . H36C H 0.3336(2) 0.2224(2) 0.10593(15) 0.079 Uiso 1 calc R . C37 C 0.4207(3) -0.1697(3) 0.4530(2) 0.0821(9) Uani 1 d . . H37A H 0.3793(3) -0.2220(3) 0.4607(2) 0.123 Uiso 1 calc R . H37B H 0.4342(3) -0.1680(3) 0.5082(2) 0.123 Uiso 1 calc R . H37C H 0.5017(3) -0.1993(3) 0.4240(2) 0.123 Uiso 1 calc R . C38 C 0.4097(3) 0.0740(3) 0.3791(2) 0.0858(10) Uani 1 d . . H38A H 0.3621(3) 0.1562(3) 0.3458(2) 0.129 Uiso 1 calc R . H38B H 0.4909(3) 0.0405(3) 0.3512(2) 0.129 Uiso 1 calc R . H38C H 0.4234(3) 0.0718(3) 0.4354(2) 0.129 Uiso 1 calc R . C39 C 0.1742(4) 0.0443(3) 0.4542(2) 0.0907(10) Uani 1 d . . H39A H 0.1188(4) 0.1248(3) 0.4222(2) 0.136 Uiso 1 calc R . H39B H 0.1990(4) 0.0461(3) 0.5060(2) 0.136 Uiso 1 calc R . H39C H 0.1298(4) -0.0068(3) 0.4684(2) 0.136 Uiso 1 calc R . C40A C 0.2210(8) 0.5815(7) -0.0184(5) 0.085(2) Uiso 0.485(9) d P 1 H40A H 0.3128(8) 0.5399(7) -0.0171(5) 0.127 Uiso 0.485(9) calc PR 1 H40B H 0.1912(8) 0.6222(7) 0.0249(5) 0.127 Uiso 0.485(9) calc PR 1 H40C H 0.1952(8) 0.6397(7) -0.0739(5) 0.127 Uiso 0.485(9) calc PR 1 C40B C 0.1478(9) 0.6171(7) -0.0318(5) 0.092(2) Uiso 0.515(9) d P 2 H40D H 0.2207(9) 0.6237(7) -0.0183(5) 0.138 Uiso 0.515(9) calc PR 2 H40E H 0.0726(9) 0.6640(7) -0.0045(5) 0.138 Uiso 0.515(9) calc PR 2 H40F H 0.1370(9) 0.6468(7) -0.0929(5) 0.138 Uiso 0.515(9) calc PR 2 C41 C 0.1671(4) 0.4957(4) -0.0020(3) 0.1053(11) Uiso 1 d . . H41A H 0.1966(4) 0.4361(4) 0.0534(3) 0.126 Uiso 0.485(9) calc PR 1 H41B H 0.2005(4) 0.4536(4) -0.0451(3) 0.126 Uiso 0.485(9) calc PR 1 H41C H 0.1809(4) 0.4665(4) 0.0594(3) 0.126 Uiso 0.515(9) calc PR 2 H41D H 0.2450(4) 0.4494(4) -0.0287(3) 0.126 Uiso 0.515(9) calc PR 2 C42A C 0.0265(8) 0.5460(8) -0.0018(5) 0.096(3) Uiso 0.485(9) d P 1 H42A H -0.0045(8) 0.6140(8) -0.0533(5) 0.115 Uiso 0.485(9) calc PR 1 H42B H -0.0072(8) 0.5762(8) 0.0473(5) 0.115 Uiso 0.485(9) calc PR 1 C42B C 0.0646(5) 0.4707(5) -0.0175(3) 0.066(2) Uiso 0.515(9) d P 2 H42C H 0.0911(5) 0.3840(5) 0.0049(3) 0.080 Uiso 0.515(9) calc PR 2 H42D H 0.0576(5) 0.4926(5) -0.0793(3) 0.080 Uiso 0.515(9) calc PR 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 Ca 0.0298(2) 0.0335(2) 0.0319(2) -0.01625(14) 0.00306(13) -0.01617(14) Si1 0.0405(3) 0.0293(2) 0.0451(3) -0.0124(2) 0.0007(2) -0.0179(2) Si2 0.0784(4) 0.0640(4) 0.0390(3) -0.0167(3) -0.0026(3) -0.0488(4) O 0.0469(8) 0.0522(8) 0.0353(7) -0.0106(6) 0.0005(6) -0.0212(7) N1 0.0264(7) 0.0282(7) 0.0309(7) -0.0118(6) 0.0005(5) -0.0103(6) N2 0.0288(7) 0.0287(7) 0.0279(7) -0.0072(5) -0.0003(5) -0.0145(6) N3 0.0418(8) 0.0346(8) 0.0359(8) -0.0146(6) 0.0024(6) -0.0213(7) C1 0.0331(8) 0.0297(8) 0.0300(8) -0.0115(7) 0.0033(7) -0.0157(7) C2 0.0340(9) 0.0320(8) 0.0260(8) -0.0068(7) -0.0020(6) -0.0139(7) C3 0.0311(8) 0.0244(7) 0.0317(8) -0.0067(6) -0.0041(6) -0.0126(7) C4 0.0391(10) 0.0579(12) 0.0331(9) -0.0186(9) 0.0063(8) -0.0186(9) C5 0.0338(9) 0.0502(11) 0.0355(9) -0.0125(8) -0.0062(7) -0.0167(8) C6 0.0283(8) 0.0331(9) 0.0286(8) -0.0124(7) 0.0010(6) -0.0068(7) C7 0.0395(10) 0.0346(9) 0.0432(10) -0.0145(8) 0.0069(8) -0.0087(8) C8 0.0455(12) 0.0368(10) 0.0522(12) -0.0102(9) 0.0029(9) 0.0004(9) C9 0.0335(10) 0.0596(14) 0.0491(12) -0.0147(10) -0.0059(9) 0.0016(10) C10 0.0311(10) 0.0592(13) 0.0523(12) -0.0195(10) -0.0057(9) -0.0110(9) C11 0.0307(9) 0.0443(10) 0.0356(9) -0.0157(8) -0.0022(7) -0.0120(8) C12 0.0470(12) 0.0304(10) 0.096(2) -0.0205(11) 0.0120(12) -0.0117(9) C13 0.097(2) 0.0490(14) 0.105(2) -0.0216(15) 0.038(2) -0.0360(15) C14 0.089(2) 0.066(2) 0.111(2) -0.026(2) -0.018(2) -0.040(2) C15 0.0332(9) 0.0451(11) 0.0598(12) -0.0178(9) -0.0057(9) -0.0177(8) C16 0.076(2) 0.065(2) 0.065(2) -0.0096(12) -0.0031(13) -0.0382(14) C17 0.0558(14) 0.072(2) 0.086(2) -0.0408(14) -0.0079(13) -0.0261(13) C18 0.0299(8) 0.0361(9) 0.0289(8) -0.0102(7) -0.0018(6) -0.0186(7) C19 0.0309(8) 0.0379(9) 0.0356(9) -0.0122(7) -0.0021(7) -0.0169(7) C20 0.0332(9) 0.0499(11) 0.0415(10) -0.0209(9) 0.0031(8) -0.0177(8) C21 0.0419(11) 0.0606(13) 0.0405(10) -0.0141(9) 0.0095(8) -0.0303(10) C22 0.0458(11) 0.0468(11) 0.0411(10) -0.0065(8) 0.0042(8) -0.0287(9) C23 0.0362(9) 0.0368(9) 0.0353(9) -0.0093(7) -0.0009(7) -0.0204(8) C24 0.0354(10) 0.0352(9) 0.0522(11) -0.0143(8) 0.0042(8) -0.0131(8) C25 0.0628(15) 0.0489(13) 0.085(2) -0.0271(12) -0.0034(13) -0.0261(11) C26 0.0480(12) 0.0446(12) 0.0655(14) -0.0066(11) -0.0094(11) -0.0096(10) C27 0.0420(10) 0.0320(9) 0.0479(11) -0.0075(8) 0.0020(8) -0.0197(8) C28 0.0674(15) 0.0437(12) 0.0654(14) -0.0243(11) 0.0003(11) -0.0232(11) C29 0.068(2) 0.0392(11) 0.068(2) -0.0011(11) 0.0056(12) -0.0201(11) C30 0.0631(15) 0.0509(13) 0.0631(15) -0.0119(11) -0.0076(12) -0.0167(11) C31 0.100(2) 0.074(2) 0.060(2) 0.0083(14) -0.012(2) -0.027(2) C32A 0.068(3) 0.087(4) 0.045(3) -0.002(3) 0.005(2) -0.043(3) C32B 0.065(4) 0.084(5) 0.036(3) -0.014(3) 0.004(2) -0.032(4) C33 0.0534(13) 0.0682(15) 0.0415(11) -0.0195(10) 0.0074(9) -0.0258(11) C34 0.0584(13) 0.0483(11) 0.0435(11) -0.0074(9) -0.0063(9) -0.0306(10) C35 0.0604(14) 0.0376(11) 0.087(2) -0.0261(12) 0.0023(12) -0.0158(10) C36 0.0592(13) 0.0485(12) 0.0564(13) -0.0064(10) 0.0003(10) -0.0343(11) C37 0.105(2) 0.093(2) 0.060(2) 0.0124(14) -0.034(2) -0.065(2) C38 0.131(3) 0.102(2) 0.069(2) -0.015(2) -0.023(2) -0.088(2) C39 0.132(3) 0.115(3) 0.059(2) -0.055(2) 0.029(2) -0.071(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 Ca N3 2.3134(14) . ? Ca N1 2.3521(13) . ? Ca O 2.3591(14) . ? Ca N2 2.3698(14) . ? Ca C1 3.176(2) . ? Ca C3 3.204(2) . ? Si1 N3 1.696(2) . ? Si1 C36 1.880(2) . ? Si1 C35 1.881(2) . ? Si1 C34 1.886(2) . ? Si2 N3 1.689(2) . ? Si2 C37 1.881(3) . ? Si2 C38 1.889(3) . ? Si2 C39 1.890(3) . ? O C30 1.444(3) . ? O C33 1.454(3) . ? N1 C1 1.329(2) . ? N1 C6 1.436(2) . ? N2 C3 1.327(2) . ? N2 C18 1.435(2) . ? C1 C2 1.412(2) . ? C1 C4 1.521(2) . ? C2 C3 1.413(2) . ? C2 H2 0.95 . ? C3 C5 1.517(2) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 C11 1.411(3) . ? C6 C7 1.413(3) . ? C7 C8 1.399(3) . ? C7 C12 1.519(3) . ? C8 C9 1.368(4) . ? C8 H8 0.95 . ? C9 C10 1.369(3) . ? C9 H9 0.95 . ? C10 C11 1.395(3) . ? C10 H10 0.95 . ? C11 C15 1.513(3) . ? C12 C14 1.522(4) . ? C12 C13 1.528(4) . ? C12 H12 1.00 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 C17 1.520(3) . ? C15 C16 1.540(3) . ? C15 H15 1.00 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 C19 1.407(2) . ? C18 C23 1.416(2) . ? C19 C20 1.394(3) . ? C19 C24 1.523(3) . ? C20 C21 1.377(3) . ? C20 H20 0.95 . ? C21 C22 1.381(3) . ? C21 H21 0.95 . ? C22 C23 1.393(3) . ? C22 H22 0.95 . ? C23 C27 1.518(3) . ? C24 C25 1.517(3) . ? C24 C26 1.532(3) . ? C24 H24 1.00 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 C28 1.529(3) . ? C27 C29 1.534(3) . ? C27 H27 1.00 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C30 C31 1.494(4) . ? C30 H30A 0.99 . ? C30 H30B 0.99 . ? C31 C32A 1.424(6) . ? C31 C32B 1.580(9) . ? C31 H31A 0.99 . ? C31 H31B 0.99 . ? C31 H31C 0.99 . ? C31 H31D 0.99 . ? C32A C33 1.513(6) . ? C32A H32A 0.99 . ? C32A H32B 0.99 . ? C32B C33 1.456(6) . ? C32B H32C 0.99 . ? C32B H32D 0.99 . ? C33 H33A 0.99 . ? C33 H33B 0.99 . ? C33 H33C 0.99 . ? C33 H33D 0.99 . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? C39 H39A 0.98 . ? C39 H39B 0.98 . ? C39 H39C 0.98 . ? C40A C41 1.468(8) . ? C40A H40A 0.98 . ? C40A H40B 0.98 . ? C40A H40C 0.98 . ? C40B C41 1.429(8) . ? C40B H40D 0.98 . ? C40B H40E 0.98 . ? C40B H40F 0.98 . ? C41 C42B 1.481(7) . ? C41 C42A 1.502(9) . ? C41 H41A 0.99 . ? C41 H41B 0.99 . ? C41 H41C 0.99 . ? C41 H41D 0.99 . ? C42A C42A 1.58(2) 2_565 ? C42A H42A 0.99 . ? C42A H42B 0.99 . ? C42B C42B 1.505(12) 2_565 ? C42B H42C 0.99 . ? C42B H42D 0.99 . ? 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 Ca N1 124.79(5) . . ? N3 Ca O 104.88(5) . . ? N1 Ca O 113.79(5) . . ? N3 Ca N2 136.78(5) . . ? N1 Ca N2 81.14(5) . . ? O Ca N2 91.25(5) . . ? N3 Ca C1 124.58(5) . . ? N1 Ca C1 22.02(4) . . ? O Ca C1 127.25(5) . . ? N2 Ca C1 66.12(4) . . ? N3 Ca C3 132.09(5) . . ? N1 Ca C3 66.23(4) . . ? O Ca C3 111.19(5) . . ? N2 Ca C3 21.57(4) . . ? C1 Ca C3 47.57(4) . . ? N3 Si1 C36 116.46(9) . . ? N3 Si1 C35 113.98(10) . . ? C36 Si1 C35 104.55(11) . . ? N3 Si1 C34 108.99(8) . . ? C36 Si1 C34 104.53(10) . . ? C35 Si1 C34 107.62(11) . . ? N3 Si2 C37 111.53(11) . . ? N3 Si2 C38 114.89(11) . . ? C37 Si2 C38 104.65(14) . . ? N3 Si2 C39 111.95(12) . . ? C37 Si2 C39 107.4(2) . . ? C38 Si2 C39 105.9(2) . . ? C30 O C33 108.9(2) . . ? C30 O Ca 128.27(13) . . ? C33 O Ca 122.81(12) . . ? C1 N1 C6 119.30(13) . . ? C1 N1 Ca 116.44(10) . . ? C6 N1 Ca 122.70(10) . . ? C3 N2 C18 120.76(14) . . ? C3 N2 Ca 117.38(10) . . ? C18 N2 Ca 120.36(10) . . ? Si2 N3 Si1 121.51(9) . . ? Si2 N3 Ca 124.92(8) . . ? Si1 N3 Ca 113.17(7) . . ? N1 C1 C2 124.99(15) . . ? N1 C1 C4 120.5(2) . . ? C2 C1 C4 114.48(15) . . ? N1 C1 Ca 41.54(8) . . ? C2 C1 Ca 87.02(10) . . ? C4 C1 Ca 152.40(12) . . ? C1 C2 C3 131.22(15) . . ? C1 C2 H2 114.39(9) . . ? C3 C2 H2 114.39(9) . . ? N2 C3 C2 123.94(15) . . ? N2 C3 C5 120.90(15) . . ? C2 C3 C5 115.16(15) . . ? N2 C3 Ca 41.05(8) . . ? C2 C3 Ca 85.88(10) . . ? C5 C3 Ca 153.90(12) . . ? C1 C4 H4A 109.47(10) . . ? C1 C4 H4B 109.47(10) . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.47(10) . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.47(10) . . ? C3 C5 H5B 109.47(10) . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.47(10) . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 120.1(2) . . ? C11 C6 N1 121.1(2) . . ? C7 C6 N1 118.7(2) . . ? C8 C7 C6 118.2(2) . . ? C8 C7 C12 120.0(2) . . ? C6 C7 C12 121.8(2) . . ? C9 C8 C7 121.8(2) . . ? C9 C8 H8 119.09(12) . . ? C7 C8 H8 119.09(13) . . ? C8 C9 C10 119.6(2) . . ? C8 C9 H9 120.19(12) . . ? C10 C9 H9 120.19(13) . . ? C9 C10 C11 121.9(2) . . ? C9 C10 H10 119.07(13) . . ? C11 C10 H10 119.07(13) . . ? C10 C11 C6 118.4(2) . . ? C10 C11 C15 118.2(2) . . ? C6 C11 C15 123.4(2) . . ? C7 C12 C14 111.6(2) . . ? C7 C12 C13 112.0(2) . . ? C14 C12 C13 109.6(2) . . ? C7 C12 H12 107.83(10) . . ? C14 C12 H12 107.8(2) . . ? C13 C12 H12 107.83(14) . . ? C12 C13 H13A 109.5(2) . . ? C12 C13 H13B 109.47(14) . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5(2) . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5(2) . . ? C12 C14 H14B 109.5(2) . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.47(15) . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C17 111.2(2) . . ? C11 C15 C16 110.9(2) . . ? C17 C15 C16 109.5(2) . . ? C11 C15 H15 108.40(10) . . ? C17 C15 H15 108.40(12) . . ? C16 C15 H15 108.40(13) . . ? C15 C16 H16A 109.47(13) . . ? C15 C16 H16B 109.47(13) . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.47(13) . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.47(13) . . ? C15 C17 H17B 109.47(12) . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.47(14) . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 119.8(2) . . ? C19 C18 N2 121.46(15) . . ? C23 C18 N2 118.39(15) . . ? C20 C19 C18 119.1(2) . . ? C20 C19 C24 118.7(2) . . ? C18 C19 C24 122.1(2) . . ? C21 C20 C19 121.4(2) . . ? C21 C20 H20 119.28(11) . . ? C19 C20 H20 119.28(11) . . ? C20 C21 C22 119.2(2) . . ? C20 C21 H21 120.38(11) . . ? C22 C21 H21 120.38(11) . . ? C21 C22 C23 121.9(2) . . ? C21 C22 H22 119.05(11) . . ? C23 C22 H22 119.05(11) . . ? C22 C23 C18 118.4(2) . . ? C22 C23 C27 120.9(2) . . ? C18 C23 C27 120.7(2) . . ? C25 C24 C19 111.7(2) . . ? C25 C24 C26 110.4(2) . . ? C19 C24 C26 111.7(2) . . ? C25 C24 H24 107.62(13) . . ? C19 C24 H24 107.62(10) . . ? C26 C24 H24 107.62(12) . . ? C24 C25 H25A 109.47(12) . . ? C24 C25 H25B 109.47(12) . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.47(13) . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.47(12) . . ? C24 C26 H26B 109.47(12) . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.47(12) . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C28 112.0(2) . . ? C23 C27 C29 113.8(2) . . ? C28 C27 C29 108.9(2) . . ? C23 C27 H27 107.26(10) . . ? C28 C27 H27 107.26(12) . . ? C29 C27 H27 107.26(13) . . ? C27 C28 H28A 109.47(11) . . ? C27 C28 H28B 109.47(11) . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.47(12) . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.47(12) . . ? C27 C29 H29B 109.47(13) . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.47(13) . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O C30 C31 106.6(2) . . ? O C30 H30A 110.41(13) . . ? C31 C30 H30A 110.4(2) . . ? O C30 H30B 110.41(12) . . ? C31 C30 H30B 110.4(2) . . ? H30A C30 H30B 108.6 . . ? C32A C31 C30 102.4(3) . . ? C30 C31 C32B 106.9(3) . . ? C32A C31 H31A 111.3(4) . . ? C30 C31 H31A 111.3(2) . . ? C32A C31 H31B 111.3(5) . . ? C30 C31 H31B 111.3(2) . . ? H31A C31 H31B 109.2 . . ? C30 C31 H31C 110.3(2) . . ? C32B C31 H31C 110.3(4) . . ? C30 C31 H31D 110.3(2) . . ? C32B C31 H31D 110.3(5) . . ? H31C C31 H31D 108.6 . . ? C31 C32A C33 106.5(4) . . ? C31 C32A H32A 110.4(4) . . ? C33 C32A H32A 110.4(4) . . ? C31 C32A H32B 110.4(5) . . ? C33 C32A H32B 110.4(4) . . ? H32A C32A H32B 108.6 . . ? C33 C32B C31 101.6(5) . . ? C33 C32B H32C 111.4(4) . . ? C31 C32B H32C 111.4(4) . . ? C33 C32B H32D 111.5(6) . . ? C31 C32B H32D 111.5(5) . . ? H32C C32B H32D 109.3 . . ? O C33 C32B 109.3(3) . . ? O C33 C32A 102.7(3) . . ? O C33 H33A 111.23(11) . . ? C32A C33 H33A 111.2(3) . . ? O C33 H33B 111.23(12) . . ? C32A C33 H33B 111.2(4) . . ? H33A C33 H33B 109.1 . . ? O C33 H33C 109.81(11) . . ? C32B C33 H33C 109.8(5) . . ? O C33 H33D 109.81(11) . . ? C32B C33 H33D 109.8(5) . . ? H33C C33 H33D 108.3 . . ? Si1 C34 H34A 109.47(7) . . ? Si1 C34 H34B 109.47(7) . . ? H34A C34 H34B 109.5 . . ? Si1 C34 H34C 109.47(7) . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si1 C35 H35A 109.47(8) . . ? Si1 C35 H35B 109.47(9) . . ? H35A C35 H35B 109.5 . . ? Si1 C35 H35C 109.47(9) . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si1 C36 H36A 109.47(7) . . ? Si1 C36 H36B 109.47(8) . . ? H36A C36 H36B 109.5 . . ? Si1 C36 H36C 109.47(7) . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si2 C37 H37A 109.47(9) . . ? Si2 C37 H37B 109.47(10) . . ? H37A C37 H37B 109.5 . . ? Si2 C37 H37C 109.47(11) . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si2 C38 H38A 109.47(11) . . ? Si2 C38 H38B 109.47(12) . . ? H38A C38 H38B 109.5 . . ? Si2 C38 H38C 109.47(9) . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si2 C39 H39A 109.47(11) . . ? Si2 C39 H39B 109.47(10) . . ? H39A C39 H39B 109.5 . . ? Si2 C39 H39C 109.47(10) . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40A H40A 109.5(4) . . ? C41 C40A H40B 109.5(3) . . ? H40A C40A H40B 109.5 . . ? C41 C40A H40C 109.5(4) . . ? H40A C40A H40C 109.5 . . ? H40B C40A H40C 109.5 . . ? C41 C40B H40D 109.5(4) . . ? C41 C40B H40E 109.5(4) . . ? H40D C40B H40E 109.5 . . ? C41 C40B H40F 109.5(3) . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? C40B C41 C42B 116.1(5) . . ? C40A C41 C42A 115.9(5) . . ? C40A C41 H41A 108.3(4) . . ? C42A C41 H41A 108.3(3) . . ? C40A C41 H41B 108.3(3) . . ? C42A C41 H41B 108.3(4) . . ? H41A C41 H41B 107.4 . . ? C40B C41 H41C 108.3(4) . . ? C42B C41 H41C 108.3(3) . . ? C40B C41 H41D 108.3(4) . . ? C42B C41 H41D 108.3(3) . . ? H41C C41 H41D 107.4 . . ? C41 C42A C42A 114.0(8) . 2_565 ? C41 C42A H42A 108.8(3) . . ? C42A C42A H42A 108.8(6) 2_565 . ? C41 C42A H42B 108.8(4) . . ? C42A C42A H42B 108.8(6) 2_565 . ? H42A C42A H42B 107.7 . . ? C41 C42B C42B 119.1(6) . 2_565 ? C41 C42B H42C 107.5(3) . . ? C42B C42B H42C 107.5(4) 2_565 . ? C41 C42B H42D 107.5(3) . . ? C42B C42B H42D 107.5(4) 2_565 . ? H42C C42B H42D 107.0 . . ? 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 Ca O C30 -114.7(2) . . . . ? N1 Ca O C30 24.9(2) . . . . ? N2 Ca O C30 105.8(2) . . . . ? C1 Ca O C30 45.3(2) . . . . ? C3 Ca O C30 97.4(2) . . . . ? N3 Ca O C33 63.7(2) . . . . ? N1 Ca O C33 -156.59(15) . . . . ? N2 Ca O C33 -75.7(2) . . . . ? C1 Ca O C33 -136.25(15) . . . . ? C3 Ca O C33 -84.1(2) . . . . ? N3 Ca N1 C1 -97.20(12) . . . . ? O Ca N1 C1 132.41(11) . . . . ? N2 Ca N1 C1 44.97(12) . . . . ? C1 Ca N1 C1 0.0 . . . . ? C3 Ca N1 C1 28.67(11) . . . . ? N3 Ca N1 C6 68.42(14) . . . . ? O Ca N1 C6 -61.97(13) . . . . ? N2 Ca N1 C6 -149.42(13) . . . . ? C1 Ca N1 C6 165.6(2) . . . . ? C3 Ca N1 C6 -165.71(13) . . . . ? N3 Ca N2 C3 88.33(13) . . . . ? N1 Ca N2 C3 -44.31(12) . . . . ? O Ca N2 C3 -158.20(12) . . . . ? C1 Ca N2 C3 -27.47(11) . . . . ? C3 Ca N2 C3 0.0 . . . . ? N3 Ca N2 C18 -77.83(13) . . . . ? N1 Ca N2 C18 149.53(12) . . . . ? O Ca N2 C18 35.63(12) . . . . ? C1 Ca N2 C18 166.37(13) . . . . ? C3 Ca N2 C18 -166.2(2) . . . . ? C37 Si2 N3 Si1 -157.52(13) . . . . ? C38 Si2 N3 Si1 -38.7(2) . . . . ? C39 Si2 N3 Si1 82.2(2) . . . . ? C37 Si2 N3 Ca 30.26(15) . . . . ? C38 Si2 N3 Ca 149.13(15) . . . . ? C39 Si2 N3 Ca -90.05(15) . . . . ? C36 Si1 N3 Si2 72.57(14) . . . . ? C35 Si1 N3 Si2 -49.33(15) . . . . ? C34 Si1 N3 Si2 -169.55(11) . . . . ? C36 Si1 N3 Ca -114.36(10) . . . . ? C35 Si1 N3 Ca 123.74(11) . . . . ? C34 Si1 N3 Ca 3.52(12) . . . . ? N1 Ca N3 Si2 -117.59(9) . . . . ? O Ca N3 Si2 16.27(11) . . . . ? N2 Ca N3 Si2 124.66(9) . . . . ? C1 Ca N3 Si2 -144.44(8) . . . . ? C3 Ca N3 Si2 154.35(8) . . . . ? N1 Ca N3 Si1 69.62(10) . . . . ? O Ca N3 Si1 -156.52(7) . . . . ? N2 Ca N3 Si1 -48.13(12) . . . . ? C1 Ca N3 Si1 42.77(10) . . . . ? C3 Ca N3 Si1 -18.44(11) . . . . ? C6 N1 C1 C2 166.2(2) . . . . ? Ca N1 C1 C2 -27.7(2) . . . . ? C6 N1 C1 C4 -13.8(2) . . . . ? Ca N1 C1 C4 152.34(13) . . . . ? C6 N1 C1 Ca -166.1(2) . . . . ? Ca N1 C1 Ca 0.0 . . . . ? N3 Ca C1 N1 98.28(12) . . . . ? N1 Ca C1 N1 0.0 . . . . ? O Ca C1 N1 -58.08(13) . . . . ? N2 Ca C1 N1 -130.21(13) . . . . ? C3 Ca C1 N1 -143.50(14) . . . . ? N3 Ca C1 C2 -104.12(10) . . . . ? N1 Ca C1 C2 157.6(2) . . . . ? O Ca C1 C2 99.52(10) . . . . ? N2 Ca C1 C2 27.39(9) . . . . ? C3 Ca C1 C2 14.10(9) . . . . ? N3 Ca C1 C4 38.6(3) . . . . ? N1 Ca C1 C4 -59.7(3) . . . . ? O Ca C1 C4 -117.7(3) . . . . ? N2 Ca C1 C4 170.1(3) . . . . ? C3 Ca C1 C4 156.8(3) . . . . ? N1 C1 C2 C3 -14.9(3) . . . . ? C4 C1 C2 C3 165.1(2) . . . . ? Ca C1 C2 C3 -32.8(2) . . . . ? C18 N2 C3 C2 -168.70(15) . . . . ? Ca N2 C3 C2 25.2(2) . . . . ? C18 N2 C3 C5 11.1(2) . . . . ? Ca N2 C3 C5 -155.01(13) . . . . ? C18 N2 C3 Ca 166.1(2) . . . . ? Ca N2 C3 Ca 0.0 . . . . ? C1 C2 C3 N2 16.3(3) . . . . ? C1 C2 C3 C5 -163.5(2) . . . . ? C1 C2 C3 Ca 32.5(2) . . . . ? N3 Ca C3 N2 -112.70(12) . . . . ? N1 Ca C3 N2 131.04(12) . . . . ? O Ca C3 N2 23.46(13) . . . . ? N2 Ca C3 N2 0.0 . . . . ? C1 Ca C3 N2 145.15(13) . . . . ? N3 Ca C3 C2 88.04(11) . . . . ? N1 Ca C3 C2 -28.22(9) . . . . ? O Ca C3 C2 -135.80(9) . . . . ? N2 Ca C3 C2 -159.3(2) . . . . ? C1 Ca C3 C2 -14.12(9) . . . . ? N3 Ca C3 C5 -57.2(3) . . . . ? N1 Ca C3 C5 -173.5(3) . . . . ? O Ca C3 C5 79.0(3) . . . . ? N2 Ca C3 C5 55.5(3) . . . . ? C1 Ca C3 C5 -159.4(3) . . . . ? C1 N1 C6 C11 96.3(2) . . . . ? Ca N1 C6 C11 -68.9(2) . . . . ? C1 N1 C6 C7 -87.3(2) . . . . ? Ca N1 C6 C7 107.5(2) . . . . ? C11 C6 C7 C8 -0.8(3) . . . . ? N1 C6 C7 C8 -177.2(2) . . . . ? C11 C6 C7 C12 -179.3(2) . . . . ? N1 C6 C7 C12 4.3(3) . . . . ? C6 C7 C8 C9 0.4(3) . . . . ? C12 C7 C8 C9 178.9(2) . . . . ? C7 C8 C9 C10 0.4(3) . . . . ? C8 C9 C10 C11 -0.9(3) . . . . ? C9 C10 C11 C6 0.5(3) . . . . ? C9 C10 C11 C15 -178.7(2) . . . . ? C7 C6 C11 C10 0.3(3) . . . . ? N1 C6 C11 C10 176.7(2) . . . . ? C7 C6 C11 C15 179.5(2) . . . . ? N1 C6 C11 C15 -4.1(3) . . . . ? C8 C7 C12 C14 -77.7(3) . . . . ? C6 C7 C12 C14 100.8(2) . . . . ? C8 C7 C12 C13 45.6(3) . . . . ? C6 C7 C12 C13 -135.9(2) . . . . ? C10 C11 C15 C17 -55.5(2) . . . . ? C6 C11 C15 C17 125.3(2) . . . . ? C10 C11 C15 C16 66.5(2) . . . . ? C6 C11 C15 C16 -112.6(2) . . . . ? C3 N2 C18 C19 -87.7(2) . . . . ? Ca N2 C18 C19 78.0(2) . . . . ? C3 N2 C18 C23 98.9(2) . . . . ? Ca N2 C18 C23 -95.4(2) . . . . ? C23 C18 C19 C20 2.4(2) . . . . ? N2 C18 C19 C20 -170.9(2) . . . . ? C23 C18 C19 C24 -178.0(2) . . . . ? N2 C18 C19 C24 8.7(2) . . . . ? C18 C19 C20 C21 -1.6(3) . . . . ? C24 C19 C20 C21 178.9(2) . . . . ? C19 C20 C21 C22 -0.6(3) . . . . ? C20 C21 C22 C23 1.8(3) . . . . ? C21 C22 C23 C18 -1.0(3) . . . . ? C21 C22 C23 C27 178.5(2) . . . . ? C19 C18 C23 C22 -1.2(2) . . . . ? N2 C18 C23 C22 172.3(2) . . . . ? C19 C18 C23 C27 179.3(2) . . . . ? N2 C18 C23 C27 -7.1(2) . . . . ? C20 C19 C24 C25 66.8(2) . . . . ? C18 C19 C24 C25 -112.8(2) . . . . ? C20 C19 C24 C26 -57.4(2) . . . . ? C18 C19 C24 C26 123.0(2) . . . . ? C22 C23 C27 C28 102.2(2) . . . . ? C18 C23 C27 C28 -78.3(2) . . . . ? C22 C23 C27 C29 -21.8(3) . . . . ? C18 C23 C27 C29 157.6(2) . . . . ? C33 O C30 C31 -9.8(3) . . . . ? Ca O C30 C31 168.8(2) . . . . ? O C30 C31 C32A 28.7(6) . . . . ? O C30 C31 C32B -6.3(6) . . . . ? C30 C31 C32A C33 -36.3(7) . . . . ? C32B C31 C32A C33 65.5(6) . . . . ? C32A C31 C32B C33 -67.7(6) . . . . ? C30 C31 C32B C33 19.6(8) . . . . ? C30 O C33 C32B 23.9(6) . . . . ? Ca O C33 C32B -154.8(6) . . . . ? C30 O C33 C32A -11.8(5) . . . . ? Ca O C33 C32A 169.4(4) . . . . ? C31 C32B C33 O -26.0(8) . . . . ? C31 C32B C33 C32A 58.5(7) . . . . ? C31 C32A C33 O 30.7(7) . . . . ? C31 C32A C33 C32B -75.1(7) . . . . ? C40B C41 C42A C42A 162.8(9) . . . 2_565 ? C40A C41 C42A C42A 170.9(7) . . . 2_565 ? C42B C41 C42A C42A 17.7(6) . . . 2_565 ? C40B C41 C42B C42B -58.8(8) . . . 2_565 ? C40A C41 C42B C42B -69.0(11) . . . 2_565 ? C42A C41 C42B C42B -19.5(6) . . . 2_565 ? #END OF CIF data_Chisholm1037 _database_code_CSD 192311 _audit_creation_method SHELXL-93 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C29 H41 Ca0.50 N2' _chemical_formula_weight 437.68 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ca' 'Ca' 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.5130(2) _cell_length_b 12.5265(1) _cell_length_c 22.1472(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.280(1) _cell_angle_gamma 90.00 _cell_volume 5326.53(8) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rectangular plate' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.092 _exptl_crystal_density_method ? _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 0.157 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; The absorption correction is inherent in the scaling and merging of the data. This was done by Scalepack and the scale factor range for the frames is 9.07-10.33. The molecule contains a crystallographic two-fold axis. ; _diffrn_ambient_temperature 200(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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46450 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6114 _reflns_number_observed 4649 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The methyl group hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5 * Ueq(bonded C atom). For each methyl group, the torsion angle which defines its orientation about the C-C bond was refined. The other hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(bonded C atom). Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0680P)^2^+2.2133P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6114 _refine_ls_number_parameters 295 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_obs 0.0448 _refine_ls_wR_factor_all 0.1317 _refine_ls_wR_factor_obs 0.1209 _refine_ls_goodness_of_fit_all 1.055 _refine_ls_goodness_of_fit_obs 1.118 _refine_ls_restrained_S_all 1.055 _refine_ls_restrained_S_obs 1.118 _refine_ls_shift/esd_max -0.008 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.262 _refine_diff_density_min -0.193 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ca Ca 0.0000 0.27795(3) 0.2500 0.02782(12) Uani 1 d S . N1 N 0.04199(6) 0.19172(10) 0.16781(5) 0.0315(3) Uani 1 d . . N2 N 0.10898(6) 0.36757(9) 0.26234(6) 0.0319(3) Uani 1 d . . C1 C 0.10674(7) 0.15450(12) 0.18678(7) 0.0325(3) Uani 1 d . . C2 C 0.15804(8) 0.20375(12) 0.22993(7) 0.0370(3) Uani 1 d . . H2 H 0.19699(8) 0.15942(12) 0.24451(7) 0.044 Uiso 1 calc R . C3 C 0.16285(7) 0.30700(12) 0.25591(7) 0.0352(3) Uani 1 d . . C4 C 0.13030(9) 0.05117(14) 0.16060(8) 0.0476(4) Uani 1 d . . H4A H 0.1356(6) -0.0045(3) 0.1922(2) 0.071 Uiso 1 calc R . H4B H 0.1750(3) 0.0628(3) 0.1473(5) 0.071 Uiso 1 calc R . H4C H 0.0954(3) 0.0287(6) 0.1254(4) 0.071 Uiso 1 calc R . C5 C 0.23684(8) 0.3469(2) 0.27595(10) 0.0534(5) Uani 1 d . . H5A H 0.26765(14) 0.3109(8) 0.2520(4) 0.080 Uiso 1 calc R . H5B H 0.2523(3) 0.3316(10) 0.3196(2) 0.080 Uiso 1 calc R . H5C H 0.2384(2) 0.4241(2) 0.2691(6) 0.080 Uiso 1 calc R . C6 C 0.12341(7) 0.47280(12) 0.28782(7) 0.0336(3) Uani 1 d . . C7 C 0.11368(8) 0.56186(12) 0.24890(8) 0.0385(4) Uani 1 d . . C8 C 0.12748(9) 0.66294(14) 0.27465(9) 0.0476(4) Uani 1 d . . H8 H 0.12055(9) 0.72398(14) 0.24883(9) 0.057 Uiso 1 calc R . C9 C 0.15089(10) 0.67634(14) 0.33655(9) 0.0513(4) Uani 1 d . . H9 H 0.16094(10) 0.74578(14) 0.35301(9) 0.062 Uiso 1 calc R . C10 C 0.15969(9) 0.58837(14) 0.37451(8) 0.0466(4) Uani 1 d . . H10 H 0.17560(9) 0.59798(14) 0.41726(8) 0.056 Uiso 1 calc R . C11 C 0.14570(8) 0.48550(13) 0.35145(8) 0.0393(4) Uani 1 d . . C12 C 0.09295(9) 0.55056(14) 0.17969(8) 0.0451(4) Uani 1 d . . H12 H 0.07535(9) 0.47615(14) 0.17106(8) 0.054 Uiso 1 calc R . C13 C 0.15583(12) 0.5643(3) 0.14936(11) 0.0911(9) Uani 1 d . . H13A H 0.1902(5) 0.5088(10) 0.1640(7) 0.137 Uiso 1 calc R . H13B H 0.1765(6) 0.6347(7) 0.1596(8) 0.137 Uiso 1 calc R . H13C H 0.1416(2) 0.5583(17) 0.10476(12) 0.137 Uiso 1 calc R . C14 C 0.03532(13) 0.6259(2) 0.15229(11) 0.0852(8) Uani 1 d . . H14A H 0.0200(7) 0.6088(10) 0.1088(2) 0.128 Uiso 1 calc R . H14B H 0.0525(3) 0.6995(3) 0.1563(8) 0.128 Uiso 1 calc R . H14C H -0.0040(4) 0.6182(11) 0.1740(6) 0.128 Uiso 1 calc R . C15 C 0.15271(10) 0.39201(14) 0.39598(8) 0.0494(4) Uani 1 d . . H15 H 0.15354(10) 0.32483(14) 0.37173(8) 0.059 Uiso 1 calc R . C16 C 0.08942(12) 0.3880(2) 0.42710(10) 0.0646(6) Uani 1 d . . H16A H 0.0937(4) 0.3272(7) 0.4554(5) 0.097 Uiso 1 calc R . H16B H 0.04723(13) 0.3798(12) 0.39598(11) 0.097 Uiso 1 calc R . H16C H 0.0865(5) 0.4543(5) 0.4500(6) 0.097 Uiso 1 calc R . C17 C 0.21961(13) 0.3960(2) 0.44420(11) 0.0818(7) Uani 1 d . . H17A H 0.2217(5) 0.3332(8) 0.4709(5) 0.123 Uiso 1 calc R . H17B H 0.2198(4) 0.4609(8) 0.4689(5) 0.123 Uiso 1 calc R . H17C H 0.26010(13) 0.3962(14) 0.42363(11) 0.123 Uiso 1 calc R . C18 C 0.00765(8) 0.16144(12) 0.10753(7) 0.0345(3) Uani 1 d . . C19 C -0.05524(8) 0.10344(14) 0.09897(8) 0.0440(4) Uani 1 d . . C20 C -0.09008(10) 0.0843(2) 0.03942(10) 0.0584(5) Uani 1 d . . H20 H -0.13279(10) 0.0460(2) 0.03336(10) 0.070 Uiso 1 calc R . C21 C -0.06409(11) 0.1194(2) -0.01079(9) 0.0608(5) Uani 1 d . . H21 H -0.08906(11) 0.1065(2) -0.05101(9) 0.073 Uiso 1 calc R . C22 C -0.00211(11) 0.1731(2) -0.00254(8) 0.0526(5) Uani 1 d . . H22 H 0.01619(11) 0.1953(2) -0.03749(8) 0.063 Uiso 1 calc R . C23 C 0.03483(9) 0.19605(13) 0.05569(7) 0.0413(4) Uani 1 d . . C24 C -0.08257(10) 0.0554(2) 0.15273(10) 0.0641(6) Uani 1 d . . H24 H -0.06915(10) 0.1044(2) 0.18850(10) 0.077 Uiso 1 calc R . C25 C -0.04786(14) -0.0522(2) 0.17027(13) 0.0945(9) Uani 1 d . . H25A H -0.0663(8) -0.0826(8) 0.2049(6) 0.142 Uiso 1 calc R . H25B H 0.0026(2) -0.0422(3) 0.1820(9) 0.142 Uiso 1 calc R . H25C H -0.0576(9) -0.1009(6) 0.1352(3) 0.142 Uiso 1 calc R . C26 C -0.16188(12) 0.0430(2) 0.14202(13) 0.0886(9) Uani 1 d . . H26A H -0.1766(2) 0.0249(16) 0.1808(2) 0.133 Uiso 1 calc R . H26B H -0.1760(2) -0.0140(11) 0.1121(7) 0.133 Uiso 1 calc R . H26C H -0.18381(12) 0.1102(6) 0.1263(9) 0.133 Uiso 1 calc R . C27 C 0.10157(10) 0.2609(2) 0.06054(8) 0.0536(5) Uani 1 d . . H27 H 0.12123(10) 0.2712(2) 0.10504(8) 0.064 Uiso 1 calc R . C28 C 0.08720(13) 0.3704(2) 0.03140(10) 0.0677(6) Uani 1 d . . H28A H 0.1307(2) 0.4112(5) 0.0362(6) 0.101 Uiso 1 calc R . H28B H 0.0537(6) 0.4086(5) 0.0516(5) 0.101 Uiso 1 calc R . H28C H 0.0679(8) 0.3622(2) -0.0123(2) 0.101 Uiso 1 calc R . C29 C 0.15700(13) 0.2037(2) 0.03033(13) 0.0847(8) Uani 1 d . . H29A H 0.2005(3) 0.2445(8) 0.0381(8) 0.127 Uiso 1 calc R . H29B H 0.1404(4) 0.1985(14) -0.0140(2) 0.127 Uiso 1 calc R . H29C H 0.1652(7) 0.1319(6) 0.0477(6) 0.127 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca 0.0228(2) 0.0291(2) 0.0319(2) 0.000 0.00571(15) 0.000 N1 0.0283(6) 0.0327(6) 0.0331(6) -0.0033(5) 0.0048(5) -0.0007(5) N2 0.0247(6) 0.0344(7) 0.0364(7) -0.0031(5) 0.0053(5) -0.0025(5) C1 0.0324(7) 0.0301(7) 0.0354(8) -0.0002(6) 0.0068(6) 0.0035(6) C2 0.0292(7) 0.0382(8) 0.0417(9) 0.0001(7) 0.0013(6) 0.0068(6) C3 0.0261(7) 0.0398(8) 0.0386(8) -0.0017(6) 0.0023(6) -0.0013(6) C4 0.0467(9) 0.0407(9) 0.0527(10) -0.0096(8) 0.0016(8) 0.0122(7) C5 0.0258(8) 0.0563(11) 0.0760(13) -0.0155(10) 0.0037(8) -0.0020(7) C6 0.0236(7) 0.0344(8) 0.0436(8) -0.0045(6) 0.0080(6) -0.0037(6) C7 0.0294(7) 0.0381(8) 0.0487(9) 0.0001(7) 0.0086(7) -0.0041(6) C8 0.0451(9) 0.0373(9) 0.0614(11) 0.0033(8) 0.0125(8) -0.0060(7) C9 0.0536(10) 0.0376(9) 0.0646(12) -0.0131(9) 0.0157(9) -0.0126(8) C10 0.0459(9) 0.0471(10) 0.0468(10) -0.0114(8) 0.0081(7) -0.0083(8) C11 0.0340(8) 0.0391(9) 0.0443(9) -0.0049(7) 0.0057(7) -0.0035(6) C12 0.0413(9) 0.0459(10) 0.0470(10) 0.0046(8) 0.0045(7) -0.0094(7) C13 0.0610(14) 0.157(3) 0.0600(14) -0.028(2) 0.0249(11) -0.026(2) C14 0.077(2) 0.108(2) 0.0647(15) 0.0180(14) -0.0025(12) 0.0250(14) C15 0.0585(11) 0.0438(10) 0.0426(10) -0.0021(8) -0.0001(8) -0.0040(8) C16 0.085(2) 0.0520(12) 0.0603(12) -0.0003(10) 0.0212(11) -0.0195(11) C17 0.081(2) 0.080(2) 0.071(2) 0.0140(12) -0.0220(12) -0.0042(13) C18 0.0323(7) 0.0329(8) 0.0372(8) -0.0074(6) 0.0032(6) 0.0059(6) C19 0.0361(8) 0.0440(9) 0.0504(10) -0.0179(8) 0.0043(7) -0.0015(7) C20 0.0453(10) 0.0607(12) 0.0643(13) -0.0276(10) -0.0037(9) -0.0035(9) C21 0.0656(13) 0.0634(12) 0.0452(11) -0.0220(9) -0.0121(9) 0.0080(10) C22 0.0655(12) 0.0532(11) 0.0369(9) -0.0067(8) 0.0030(8) 0.0111(9) C23 0.0450(9) 0.0414(9) 0.0360(8) -0.0024(7) 0.0029(7) 0.0062(7) C24 0.0530(11) 0.0797(15) 0.0628(12) -0.0334(11) 0.0189(9) -0.0334(11) C25 0.083(2) 0.115(2) 0.086(2) 0.034(2) 0.0146(14) -0.025(2) C26 0.0577(13) 0.103(2) 0.112(2) -0.043(2) 0.0350(14) -0.0373(13) C27 0.0566(11) 0.0663(12) 0.0383(9) 0.0055(9) 0.0095(8) -0.0085(9) C28 0.086(2) 0.0624(13) 0.0566(12) 0.0056(10) 0.0174(11) -0.0113(11) C29 0.0673(15) 0.096(2) 0.098(2) 0.0141(15) 0.0358(14) 0.0045(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca N2 2.3768(11) 2 ? Ca N2 2.3768(12) . ? Ca N1 2.3841(12) . ? Ca N1 2.3842(12) 2 ? Ca C1 3.1194(14) 2 ? Ca C1 3.1194(14) . ? Ca C3 3.1778(14) . ? Ca C3 3.1778(14) 2 ? N1 C1 1.342(2) . ? N1 C18 1.434(2) . ? N2 C3 1.324(2) . ? N2 C6 1.442(2) . ? C1 C2 1.398(2) . ? C1 C4 1.523(2) . ? C2 C3 1.412(2) . ? C2 H2 0.95 . ? C3 C5 1.518(2) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 C7 1.402(2) . ? C6 C11 1.408(2) . ? C7 C8 1.395(2) . ? C7 C12 1.521(2) . ? C8 C9 1.376(3) . ? C8 H8 0.95 . ? C9 C10 1.378(3) . ? C9 H9 0.95 . ? C10 C11 1.395(2) . ? C10 H10 0.95 . ? C11 C15 1.521(2) . ? C12 C14 1.510(3) . ? C12 C13 1.510(3) . ? C12 H12 1.00 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 C16 1.519(3) . ? C15 C17 1.533(3) . ? C15 H15 1.00 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 C19 1.409(2) . ? C18 C23 1.416(2) . ? C19 C20 1.393(2) . ? C19 C24 1.514(3) . ? C20 C21 1.374(3) . ? C20 H20 0.95 . ? C21 C22 1.367(3) . ? C21 H21 0.95 . ? C22 C23 1.390(2) . ? C22 H22 0.95 . ? C23 C27 1.522(3) . ? C24 C25 1.527(4) . ? C24 C26 1.531(3) . ? C24 H24 1.00 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 C28 1.521(3) . ? C27 C29 1.546(3) . ? C27 H27 1.00 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ca N2 123.63(6) 2 . ? N2 Ca N1 123.26(4) 2 . ? N2 Ca N1 83.08(4) . . ? N2 Ca N1 83.08(4) 2 2 ? N2 Ca N1 123.27(4) . 2 ? N1 Ca N1 126.12(6) . 2 ? N2 Ca C1 68.31(4) 2 2 ? N2 Ca C1 146.91(4) . 2 ? N1 Ca C1 117.78(4) . 2 ? N1 Ca C1 23.75(4) 2 2 ? N2 Ca C1 146.91(4) 2 . ? N2 Ca C1 68.31(4) . . ? N1 Ca C1 23.75(4) . . ? N1 Ca C1 117.78(4) 2 . ? C1 Ca C1 120.56(6) 2 . ? N2 Ca C3 144.90(4) 2 . ? N2 Ca C3 22.13(4) . . ? N1 Ca C3 66.79(4) . . ? N1 Ca C3 119.86(4) 2 . ? C1 Ca C3 141.36(4) 2 . ? C1 Ca C3 48.12(4) . . ? N2 Ca C3 22.13(4) 2 2 ? N2 Ca C3 144.90(4) . 2 ? N1 Ca C3 119.85(4) . 2 ? N1 Ca C3 66.79(4) 2 2 ? C1 Ca C3 48.12(4) 2 2 ? C1 Ca C3 141.36(4) . 2 ? C3 Ca C3 166.85(6) . 2 ? C1 N1 C18 117.20(12) . . ? C1 N1 Ca 110.55(9) . . ? C18 N1 Ca 131.57(9) . . ? C3 N2 C6 117.54(12) . . ? C3 N2 Ca 115.34(9) . . ? C6 N2 Ca 125.81(9) . . ? N1 C1 C2 125.45(13) . . ? N1 C1 C4 120.50(13) . . ? C2 C1 C4 114.04(13) . . ? N1 C1 Ca 45.70(7) . . ? C2 C1 Ca 85.90(9) . . ? C4 C1 Ca 149.72(11) . . ? C1 C2 C3 132.08(14) . . ? C1 C2 H2 113.96(8) . . ? C3 C2 H2 113.96(8) . . ? N2 C3 C2 124.91(13) . . ? N2 C3 C5 120.78(14) . . ? C2 C3 C5 114.30(13) . . ? N2 C3 Ca 42.53(7) . . ? C2 C3 Ca 83.40(8) . . ? C5 C3 Ca 160.39(11) . . ? C1 C4 H4A 109.47(9) . . ? C1 C4 H4B 109.47(9) . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.47(9) . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.47(9) . . ? C3 C5 H5B 109.47(10) . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.47(10) . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 120.61(14) . . ? C7 C6 N2 119.44(13) . . ? C11 C6 N2 119.94(14) . . ? C8 C7 C6 118.4(2) . . ? C8 C7 C12 119.59(15) . . ? C6 C7 C12 121.88(14) . . ? C9 C8 C7 121.6(2) . . ? C9 C8 H8 119.21(10) . . ? C7 C8 H8 119.21(10) . . ? C8 C9 C10 119.6(2) . . ? C8 C9 H9 120.22(10) . . ? C10 C9 H9 120.22(10) . . ? C9 C10 C11 121.4(2) . . ? C9 C10 H10 119.32(10) . . ? C11 C10 H10 119.32(10) . . ? C10 C11 C6 118.4(2) . . ? C10 C11 C15 119.0(2) . . ? C6 C11 C15 122.54(14) . . ? C14 C12 C13 110.9(2) . . ? C14 C12 C7 113.1(2) . . ? C13 C12 C7 110.29(15) . . ? C14 C12 H12 107.45(13) . . ? C13 C12 H12 107.45(14) . . ? C7 C12 H12 107.45(9) . . ? C12 C13 H13A 109.47(14) . . ? C12 C13 H13B 109.47(13) . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.47(11) . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.47(12) . . ? C12 C14 H14B 109.47(13) . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.47(12) . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C11 109.5(2) . . ? C16 C15 C17 110.2(2) . . ? C11 C15 C17 113.2(2) . . ? C16 C15 H15 107.93(10) . . ? C11 C15 H15 107.93(9) . . ? C17 C15 H15 107.93(13) . . ? C15 C16 H16A 109.47(11) . . ? C15 C16 H16B 109.47(11) . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.47(10) . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.47(12) . . ? C15 C17 H17B 109.47(13) . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.47(13) . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 119.46(14) . . ? C19 C18 N1 120.84(14) . . ? C23 C18 N1 119.57(13) . . ? C20 C19 C18 118.8(2) . . ? C20 C19 C24 119.7(2) . . ? C18 C19 C24 121.32(15) . . ? C21 C20 C19 121.5(2) . . ? C21 C20 H20 119.24(11) . . ? C19 C20 H20 119.24(11) . . ? C22 C21 C20 119.7(2) . . ? C22 C21 H21 120.17(11) . . ? C20 C21 H21 120.17(11) . . ? C21 C22 C23 121.7(2) . . ? C21 C22 H22 119.16(11) . . ? C23 C22 H22 119.16(11) . . ? C22 C23 C18 118.8(2) . . ? C22 C23 C27 118.1(2) . . ? C18 C23 C27 123.07(14) . . ? C19 C24 C25 110.4(2) . . ? C19 C24 C26 114.0(2) . . ? C25 C24 C26 109.9(2) . . ? C19 C24 H24 107.42(9) . . ? C25 C24 H24 107.42(14) . . ? C26 C24 H24 107.42(12) . . ? C24 C25 H25A 109.47(13) . . ? C24 C25 H25B 109.47(12) . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.47(14) . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.47(13) . . ? C24 C26 H26B 109.47(12) . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.47(15) . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C23 111.2(2) . . ? C28 C27 C29 108.9(2) . . ? C23 C27 C29 112.2(2) . . ? C28 C27 H27 108.13(11) . . ? C23 C27 H27 108.13(9) . . ? C29 C27 H27 108.13(13) . . ? C27 C28 H28A 109.47(12) . . ? C27 C28 H28B 109.47(11) . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.47(11) . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.47(13) . . ? C27 C29 H29B 109.47(13) . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.47(12) . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 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 N2 Ca N1 C1 175.57(9) 2 . . . ? N2 Ca N1 C1 49.59(10) . . . . ? N1 Ca N1 C1 -76.96(9) 2 . . . ? C1 Ca N1 C1 -103.29(11) 2 . . . ? C1 Ca N1 C1 0.0 . . . . ? C3 Ca N1 C1 34.00(9) . . . . ? C3 Ca N1 C1 -158.70(9) 2 . . . ? N2 Ca N1 C18 -14.37(14) 2 . . . ? N2 Ca N1 C18 -140.36(13) . . . . ? N1 Ca N1 C18 93.10(12) 2 . . . ? C1 Ca N1 C18 66.77(13) 2 . . . ? C1 Ca N1 C18 170.1(2) . . . . ? C3 Ca N1 C18 -155.94(14) . . . . ? C3 Ca N1 C18 11.36(14) 2 . . . ? N2 Ca N2 C3 -166.61(12) 2 . . . ? N1 Ca N2 C3 -40.96(11) . . . . ? N1 Ca N2 C3 88.13(11) 2 . . . ? C1 Ca N2 C3 91.39(12) 2 . . . ? C1 Ca N2 C3 -21.69(10) . . . . ? C3 Ca N2 C3 0.0 . . . . ? C3 Ca N2 C3 -175.33(5) 2 . . . ? N2 Ca N2 C6 26.81(10) 2 . . . ? N1 Ca N2 C6 152.46(12) . . . . ? N1 Ca N2 C6 -78.45(12) 2 . . . ? C1 Ca N2 C6 -75.19(14) 2 . . . ? C1 Ca N2 C6 171.73(12) . . . . ? C3 Ca N2 C6 -166.6(2) . . . . ? C3 Ca N2 C6 18.1(2) 2 . . . ? C18 N1 C1 C2 153.20(15) . . . . ? Ca N1 C1 C2 -35.1(2) . . . . ? C18 N1 C1 C4 -26.0(2) . . . . ? Ca N1 C1 C4 145.65(12) . . . . ? C18 N1 C1 Ca -171.6(2) . . . . ? Ca N1 C1 Ca 0.0 . . . . ? N2 Ca C1 N1 -6.79(14) 2 . . . ? N2 Ca C1 N1 -125.57(10) . . . . ? N1 Ca C1 N1 0.0 . . . . ? N1 Ca C1 N1 117.19(10) 2 . . . ? C1 Ca C1 N1 90.11(10) 2 . . . ? C3 Ca C1 N1 -136.35(11) . . . . ? C3 Ca C1 N1 30.30(13) 2 . . . ? N2 Ca C1 C2 145.17(9) 2 . . . ? N2 Ca C1 C2 26.39(9) . . . . ? N1 Ca C1 C2 152.0(2) . . . . ? N1 Ca C1 C2 -90.85(9) 2 . . . ? C1 Ca C1 C2 -117.94(9) 2 . . . ? C3 Ca C1 C2 15.61(8) . . . . ? C3 Ca C1 C2 -177.74(8) 2 . . . ? N2 Ca C1 C4 -81.4(2) 2 . . . ? N2 Ca C1 C4 159.8(2) . . . . ? N1 Ca C1 C4 -74.6(2) . . . . ? N1 Ca C1 C4 42.6(2) 2 . . . ? C1 Ca C1 C4 15.5(2) 2 . . . ? C3 Ca C1 C4 149.0(2) . . . . ? C3 Ca C1 C4 -44.3(2) 2 . . . ? N1 C1 C2 C3 -13.0(3) . . . . ? C4 C1 C2 C3 166.2(2) . . . . ? Ca C1 C2 C3 -37.4(2) . . . . ? C6 N2 C3 C2 -177.74(14) . . . . ? Ca N2 C3 C2 14.5(2) . . . . ? C6 N2 C3 C5 1.2(2) . . . . ? Ca N2 C3 C5 -166.57(13) . . . . ? C6 N2 C3 Ca 167.7(2) . . . . ? Ca N2 C3 Ca 0.0 . . . . ? C1 C2 C3 N2 27.0(3) . . . . ? C1 C2 C3 C5 -152.0(2) . . . . ? C1 C2 C3 Ca 36.8(2) . . . . ? N2 Ca C3 N2 19.6(2) 2 . . . ? N2 Ca C3 N2 0.0 . . . . ? N1 Ca C3 N2 134.93(12) . . . . ? N1 Ca C3 N2 -105.51(11) 2 . . . ? C1 Ca C3 N2 -119.07(11) 2 . . . ? C1 Ca C3 N2 152.54(13) . . . . ? C3 Ca C3 N2 11.86(10) 2 . . . ? N2 Ca C3 C2 -148.46(9) 2 . . . ? N2 Ca C3 C2 -168.1(2) . . . . ? N1 Ca C3 C2 -33.13(9) . . . . ? N1 Ca C3 C2 86.43(10) 2 . . . ? C1 Ca C3 C2 72.88(11) 2 . . . ? C1 Ca C3 C2 -15.52(8) . . . . ? C3 Ca C3 C2 -156.19(9) 2 . . . ? N2 Ca C3 C5 56.1(4) 2 . . . ? N2 Ca C3 C5 36.5(3) . . . . ? N1 Ca C3 C5 171.4(4) . . . . ? N1 Ca C3 C5 -69.0(4) 2 . . . ? C1 Ca C3 C5 -82.6(4) 2 . . . ? C1 Ca C3 C5 -171.0(4) . . . . ? C3 Ca C3 C5 48.3(4) 2 . . . ? C3 N2 C6 C7 103.9(2) . . . . ? Ca N2 C6 C7 -89.78(15) . . . . ? C3 N2 C6 C11 -77.4(2) . . . . ? Ca N2 C6 C11 88.92(15) . . . . ? C11 C6 C7 C8 0.8(2) . . . . ? N2 C6 C7 C8 179.53(13) . . . . ? C11 C6 C7 C12 177.07(14) . . . . ? N2 C6 C7 C12 -4.2(2) . . . . ? C6 C7 C8 C9 0.8(2) . . . . ? C12 C7 C8 C9 -175.6(2) . . . . ? C7 C8 C9 C10 -1.4(3) . . . . ? C8 C9 C10 C11 0.4(3) . . . . ? C9 C10 C11 C6 1.2(2) . . . . ? C9 C10 C11 C15 -176.8(2) . . . . ? C7 C6 C11 C10 -1.8(2) . . . . ? N2 C6 C11 C10 179.55(13) . . . . ? C7 C6 C11 C15 176.14(14) . . . . ? N2 C6 C11 C15 -2.5(2) . . . . ? C8 C7 C12 C14 -49.4(2) . . . . ? C6 C7 C12 C14 134.4(2) . . . . ? C8 C7 C12 C13 75.4(2) . . . . ? C6 C7 C12 C13 -100.8(2) . . . . ? C10 C11 C15 C16 77.7(2) . . . . ? C6 C11 C15 C16 -100.2(2) . . . . ? C10 C11 C15 C17 -45.6(2) . . . . ? C6 C11 C15 C17 136.5(2) . . . . ? C1 N1 C18 C19 119.6(2) . . . . ? Ca N1 C18 C19 -49.9(2) . . . . ? C1 N1 C18 C23 -64.5(2) . . . . ? Ca N1 C18 C23 125.99(13) . . . . ? C23 C18 C19 C20 -1.8(2) . . . . ? N1 C18 C19 C20 174.15(15) . . . . ? C23 C18 C19 C24 173.8(2) . . . . ? N1 C18 C19 C24 -10.2(2) . . . . ? C18 C19 C20 C21 0.8(3) . . . . ? C24 C19 C20 C21 -174.9(2) . . . . ? C19 C20 C21 C22 1.0(3) . . . . ? C20 C21 C22 C23 -1.8(3) . . . . ? C21 C22 C23 C18 0.8(3) . . . . ? C21 C22 C23 C27 -177.0(2) . . . . ? C19 C18 C23 C22 1.0(2) . . . . ? N1 C18 C23 C22 -174.98(14) . . . . ? C19 C18 C23 C27 178.8(2) . . . . ? N1 C18 C23 C27 2.8(2) . . . . ? C20 C19 C24 C25 92.5(2) . . . . ? C18 C19 C24 C25 -83.1(2) . . . . ? C20 C19 C24 C26 -31.8(3) . . . . ? C18 C19 C24 C26 152.7(2) . . . . ? C22 C23 C27 C28 60.7(2) . . . . ? C18 C23 C27 C28 -117.1(2) . . . . ? C22 C23 C27 C29 -61.6(2) . . . . ? C18 C23 C27 C29 120.6(2) . . . . ? #END OF CIF