# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Hill, Michael' _publ_contact_author_email m.s.hill@bath.ac.uk _publ_section_title ; Synthesis of \^I^2^-diketiminato Calcium Silylamides and their Reactions with Triethyaluminium ; _publ_requested_category FM _publ_author_name M.Hill # Attachment '- bigcif.cif' data_h08msh20 _database_code_depnum_ccdc_archive 'CCDC 762132' #TrackingRef '- bigcif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H69 Ca N3 O Si2' _chemical_formula_weight 692.23 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' Si Si 0.0817 0.0704 '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 P21/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 12.0817(1) _cell_length_b 19.7073(3) _cell_length_c 18.5840(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.699(1) _cell_angle_gamma 90.00 _cell_volume 4191.25(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 40142 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.097 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 0.238 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63608 _diffrn_reflns_av_R_equivalents 0.1114 _diffrn_reflns_av_sigmaI/netI 0.0680 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9575 _reflns_number_gt 6501 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0776P)^2^+1.7412P] 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 SHELXL _refine_ls_extinction_coef 0.0041(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9575 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0889 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1526 _refine_ls_wR_factor_gt 0.1291 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _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 Ca1 Ca 0.31223(4) 0.16951(2) 0.35376(2) 0.02098(13) Uani 1 1 d . . . Si1 Si 0.18426(6) 0.06937(3) 0.20425(4) 0.02871(17) Uani 1 1 d . . . Si2 Si 0.20448(6) 0.00032(3) 0.35061(4) 0.03214(18) Uani 1 1 d . . . O1 O 0.28354(14) 0.16912(8) 0.47486(9) 0.0287(4) Uani 1 1 d . . . N1 N 0.48545(15) 0.21652(9) 0.33941(10) 0.0220(4) Uani 1 1 d . . . N2 N 0.24609(15) 0.28332(9) 0.32435(10) 0.0213(4) Uani 1 1 d . . . N3 N 0.22824(17) 0.06792(9) 0.30063(11) 0.0275(4) Uani 1 1 d . . . C1 C 0.28183(19) 0.31998(11) 0.27590(12) 0.0229(5) Uani 1 1 d . . . C2 C 0.37808(19) 0.30378(11) 0.25201(13) 0.0245(5) Uani 1 1 d . . . H2 H 0.3779 0.3258 0.2065 0.029 Uiso 1 1 calc R . . C3 C 0.47450(19) 0.26073(11) 0.28350(12) 0.0236(5) Uani 1 1 d . . . C4 C 0.2193(2) 0.38557(12) 0.24194(14) 0.0320(5) Uani 1 1 d . . . H4A H 0.1539 0.3935 0.2612 0.048 Uiso 1 1 calc R . . H4B H 0.1898 0.3817 0.1865 0.048 Uiso 1 1 calc R . . H4C H 0.2742 0.4236 0.2563 0.048 Uiso 1 1 calc R . . C5 C 0.5708(2) 0.26745(14) 0.24727(15) 0.0362(6) Uani 1 1 d . . . H5A H 0.6346 0.2361 0.2721 0.054 Uiso 1 1 calc R . . H5B H 0.6005 0.3141 0.2533 0.054 Uiso 1 1 calc R . . H5C H 0.5392 0.2565 0.1931 0.054 Uiso 1 1 calc R . . C6 C 0.16232(19) 0.31310(11) 0.35504(12) 0.0217(4) Uani 1 1 d . . . C7 C 0.04760(19) 0.28636(11) 0.33422(13) 0.0257(5) Uani 1 1 d . . . C8 C -0.0305(2) 0.31419(13) 0.36738(14) 0.0318(5) Uani 1 1 d . . . H8 H -0.1078 0.2969 0.3538 0.038 Uiso 1 1 calc R . . C9 C 0.0023(2) 0.36630(13) 0.41944(14) 0.0339(6) Uani 1 1 d . . . H9 H -0.0524 0.3848 0.4411 0.041 Uiso 1 1 calc R . . C10 C 0.1143(2) 0.39138(12) 0.43988(14) 0.0310(5) Uani 1 1 d . . . H10 H 0.1362 0.4271 0.4760 0.037 Uiso 1 1 calc R . . C11 C 0.1965(2) 0.36568(11) 0.40892(13) 0.0260(5) Uani 1 1 d . . . C12 C 0.00805(19) 0.23098(12) 0.27441(13) 0.0289(5) Uani 1 1 d . . . H12 H 0.0739 0.1979 0.2839 0.035 Uiso 1 1 calc R . . C13 C -0.0152(2) 0.25895(14) 0.19423(14) 0.0391(6) Uani 1 1 d . . . H13A H -0.0402 0.2220 0.1573 0.059 Uiso 1 1 calc R . . H13B H 0.0566 0.2794 0.1901 0.059 Uiso 1 1 calc R . . H13C H -0.0767 0.2935 0.1838 0.059 Uiso 1 1 calc R . . C14 C -0.0989(2) 0.19117(16) 0.27791(18) 0.0488(7) Uani 1 1 d . . . H14A H -0.1191 0.1565 0.2380 0.073 Uiso 1 1 calc R . . H14B H -0.1650 0.2223 0.2704 0.073 Uiso 1 1 calc R . . H14C H -0.0811 0.1692 0.3277 0.073 Uiso 1 1 calc R . . C15 C 0.3202(2) 0.39427(12) 0.43613(14) 0.0305(5) Uani 1 1 d . . . H15 H 0.3630 0.3761 0.4022 0.037 Uiso 1 1 calc R . . C16 C 0.3839(2) 0.37017(15) 0.51683(15) 0.0411(6) Uani 1 1 d . . . H16A H 0.4633 0.3888 0.5338 0.062 Uiso 1 1 calc R . . H16B H 0.3877 0.3205 0.5177 0.062 Uiso 1 1 calc R . . H16C H 0.3417 0.3857 0.5508 0.062 Uiso 1 1 calc R . . C17 C 0.3219(3) 0.47196(14) 0.43211(18) 0.0467(7) Uani 1 1 d . . . H17A H 0.4029 0.4880 0.4497 0.070 Uiso 1 1 calc R . . H17B H 0.2796 0.4909 0.4645 0.070 Uiso 1 1 calc R . . H17C H 0.2842 0.4866 0.3795 0.070 Uiso 1 1 calc R . . C18 C 0.60101(19) 0.19024(12) 0.37791(13) 0.0249(5) Uani 1 1 d . . . C19 C 0.67591(19) 0.22817(12) 0.43923(13) 0.0276(5) Uani 1 1 d . . . C20 C 0.7872(2) 0.20261(13) 0.47658(14) 0.0336(6) Uani 1 1 d . . . H20 H 0.8389 0.2278 0.5171 0.040 Uiso 1 1 calc R . . C21 C 0.8242(2) 0.14135(13) 0.45591(15) 0.0360(6) Uani 1 1 d . . . H21 H 0.9007 0.1251 0.4818 0.043 Uiso 1 1 calc R . . C22 C 0.7499(2) 0.10405(13) 0.39787(14) 0.0325(6) Uani 1 1 d . . . H22 H 0.7757 0.0618 0.3845 0.039 Uiso 1 1 calc R . . C23 C 0.63684(19) 0.12683(12) 0.35798(13) 0.0268(5) Uani 1 1 d . . . C24 C 0.6370(2) 0.29498(13) 0.46449(14) 0.0323(5) Uani 1 1 d . . . H24 H 0.5504 0.2924 0.4527 0.039 Uiso 1 1 calc R . . C25 C 0.6900(3) 0.30711(16) 0.55043(17) 0.0486(7) Uani 1 1 d . . . H25A H 0.6623 0.3507 0.5636 0.073 Uiso 1 1 calc R . . H25B H 0.7755 0.3079 0.5646 0.073 Uiso 1 1 calc R . . H25C H 0.6661 0.2705 0.5779 0.073 Uiso 1 1 calc R . . C26 C 0.6622(3) 0.35621(14) 0.42156(19) 0.0495(7) Uani 1 1 d . . . H26A H 0.6353 0.3977 0.4399 0.074 Uiso 1 1 calc R . . H26B H 0.6209 0.3509 0.3671 0.074 Uiso 1 1 calc R . . H26C H 0.7464 0.3593 0.4302 0.074 Uiso 1 1 calc R . . C27 C 0.5596(2) 0.08231(12) 0.29558(14) 0.0320(5) Uani 1 1 d . . . H27 H 0.4808 0.1041 0.2761 0.038 Uiso 1 1 calc R . . C28 C 0.6076(3) 0.07515(16) 0.22897(17) 0.0501(7) Uani 1 1 d . . . H28A H 0.5551 0.0463 0.1897 0.075 Uiso 1 1 calc R . . H28B H 0.6854 0.0545 0.2469 0.075 Uiso 1 1 calc R . . H28C H 0.6129 0.1201 0.2077 0.075 Uiso 1 1 calc R . . C29 C 0.5442(3) 0.01176(14) 0.32583(17) 0.0428(7) Uani 1 1 d . . . H29A H 0.4937 -0.0159 0.2844 0.064 Uiso 1 1 calc R . . H29B H 0.5084 0.0162 0.3660 0.064 Uiso 1 1 calc R . . H29C H 0.6207 -0.0102 0.3464 0.064 Uiso 1 1 calc R . . C30 C 0.3770(2) 0.16303(13) 0.54570(14) 0.0325(5) Uani 1 1 d . . . H30A H 0.3641 0.1229 0.5741 0.039 Uiso 1 1 calc R . . H30B H 0.3799 0.2039 0.5772 0.039 Uiso 1 1 calc R . . C31 C 0.4896(2) 0.15552(14) 0.52857(16) 0.0409(6) Uani 1 1 d . . . H31A H 0.5544 0.1511 0.5762 0.061 Uiso 1 1 calc R . . H31B H 0.5019 0.1956 0.5009 0.061 Uiso 1 1 calc R . . H31C H 0.4859 0.1149 0.4974 0.061 Uiso 1 1 calc R . . C32 C 0.1679(2) 0.16180(14) 0.48227(15) 0.0368(6) Uani 1 1 d . . . H32A H 0.1623 0.1169 0.5048 0.044 Uiso 1 1 calc R . . H32B H 0.1087 0.1632 0.4311 0.044 Uiso 1 1 calc R . . C33 C 0.1409(2) 0.21613(14) 0.53067(16) 0.0423(6) Uani 1 1 d . . . H33A H 0.0623 0.2090 0.5338 0.064 Uiso 1 1 calc R . . H33B H 0.1446 0.2606 0.5081 0.064 Uiso 1 1 calc R . . H33C H 0.1981 0.2143 0.5818 0.064 Uiso 1 1 calc R . . C34 C 0.2238(2) 0.15395(12) 0.17250(14) 0.0348(6) Uani 1 1 d . . . H34A H 0.3077 0.1621 0.1963 0.052 Uiso 1 1 calc R . . H34B H 0.1796 0.1898 0.1875 0.052 Uiso 1 1 calc R . . H34C H 0.2048 0.1540 0.1171 0.052 Uiso 1 1 calc R . . C35 C 0.2549(3) 0.00569(13) 0.15751(15) 0.0410(6) Uani 1 1 d . . . H35A H 0.3401 0.0091 0.1795 0.062 Uiso 1 1 calc R . . H35B H 0.2317 0.0149 0.1029 0.062 Uiso 1 1 calc R . . H35C H 0.2299 -0.0401 0.1658 0.062 Uiso 1 1 calc R . . C36 C 0.0229(2) 0.05703(15) 0.15687(16) 0.0462(7) Uani 1 1 d . . . H36A H -0.0203 0.0888 0.1785 0.069 Uiso 1 1 calc R . . H36B H 0.0016 0.0104 0.1651 0.069 Uiso 1 1 calc R . . H36C H 0.0033 0.0655 0.1022 0.069 Uiso 1 1 calc R . . C37 C 0.3106(2) -0.00161(13) 0.44970(14) 0.0361(6) Uani 1 1 d . . . H37A H 0.3906 -0.0012 0.4476 0.054 Uiso 1 1 calc R . . H37B H 0.2982 -0.0429 0.4755 0.054 Uiso 1 1 calc R . . H37C H 0.2983 0.0383 0.4777 0.054 Uiso 1 1 calc R . . C38 C 0.2232(3) -0.08521(13) 0.30992(16) 0.0494(7) Uani 1 1 d . . . H38A H 0.1705 -0.0885 0.2575 0.074 Uiso 1 1 calc R . . H38B H 0.2046 -0.1212 0.3406 0.074 Uiso 1 1 calc R . . H38C H 0.3042 -0.0903 0.3105 0.074 Uiso 1 1 calc R . . C39 C 0.0539(3) -0.00058(17) 0.35985(19) 0.0535(8) Uani 1 1 d . . . H39A H -0.0047 0.0004 0.3092 0.080 Uiso 1 1 calc R . . H39B H 0.0440 0.0393 0.3887 0.080 Uiso 1 1 calc R . . H39C H 0.0439 -0.0419 0.3865 0.080 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 Ca1 0.0219(2) 0.0205(2) 0.0216(2) -0.00009(17) 0.00849(17) -0.00133(17) Si1 0.0353(4) 0.0254(3) 0.0230(3) -0.0038(3) 0.0060(3) -0.0010(3) Si2 0.0389(4) 0.0261(4) 0.0301(4) -0.0006(3) 0.0093(3) -0.0097(3) O1 0.0310(9) 0.0346(9) 0.0220(8) 0.0027(7) 0.0105(7) 0.0005(7) N1 0.0186(9) 0.0250(10) 0.0225(10) 0.0025(7) 0.0067(7) 0.0013(7) N2 0.0204(9) 0.0230(9) 0.0208(9) 0.0014(7) 0.0071(7) 0.0008(7) N3 0.0318(11) 0.0235(10) 0.0268(10) -0.0029(8) 0.0090(8) -0.0033(8) C1 0.0241(11) 0.0250(11) 0.0185(11) 0.0000(9) 0.0051(9) -0.0010(9) C2 0.0282(12) 0.0264(12) 0.0210(11) 0.0046(9) 0.0107(9) 0.0008(9) C3 0.0250(11) 0.0257(11) 0.0216(11) 0.0003(9) 0.0095(9) -0.0028(9) C4 0.0353(13) 0.0301(13) 0.0311(13) 0.0089(10) 0.0112(11) 0.0077(10) C5 0.0323(13) 0.0446(15) 0.0386(15) 0.0140(12) 0.0211(11) 0.0072(11) C6 0.0228(11) 0.0219(11) 0.0211(11) 0.0033(8) 0.0080(9) 0.0046(8) C7 0.0227(11) 0.0305(12) 0.0238(12) 0.0024(9) 0.0074(9) 0.0028(9) C8 0.0212(12) 0.0427(14) 0.0322(13) 0.0010(11) 0.0094(10) 0.0034(10) C9 0.0295(13) 0.0397(14) 0.0353(14) -0.0014(11) 0.0143(11) 0.0089(11) C10 0.0364(14) 0.0287(13) 0.0300(13) -0.0027(10) 0.0135(11) 0.0040(10) C11 0.0275(12) 0.0246(12) 0.0260(12) 0.0031(9) 0.0088(9) 0.0024(9) C12 0.0196(11) 0.0359(13) 0.0314(13) -0.0028(10) 0.0086(9) -0.0009(10) C13 0.0337(14) 0.0480(16) 0.0291(13) -0.0060(12) 0.0012(11) 0.0068(12) C14 0.0331(15) 0.0625(19) 0.0545(19) -0.0168(15) 0.0190(14) -0.0148(13) C15 0.0306(13) 0.0319(13) 0.0308(13) -0.0076(10) 0.0125(10) -0.0050(10) C16 0.0306(14) 0.0527(17) 0.0383(15) -0.0039(13) 0.0086(11) -0.0021(12) C17 0.0552(18) 0.0339(15) 0.0543(18) -0.0084(13) 0.0222(15) -0.0141(13) C18 0.0199(11) 0.0334(12) 0.0242(12) 0.0078(9) 0.0107(9) 0.0017(9) C19 0.0219(11) 0.0346(13) 0.0267(12) 0.0051(10) 0.0083(9) -0.0013(10) C20 0.0230(12) 0.0434(15) 0.0329(14) 0.0024(11) 0.0069(10) -0.0015(11) C21 0.0235(12) 0.0442(15) 0.0397(15) 0.0123(12) 0.0093(11) 0.0069(11) C22 0.0301(13) 0.0357(14) 0.0357(14) 0.0099(11) 0.0160(11) 0.0076(10) C23 0.0263(12) 0.0316(12) 0.0255(12) 0.0057(10) 0.0125(10) 0.0029(9) C24 0.0235(12) 0.0353(14) 0.0360(14) -0.0051(11) 0.0064(10) -0.0028(10) C25 0.0380(16) 0.0573(18) 0.0435(17) -0.0165(14) 0.0032(13) 0.0014(13) C26 0.0519(18) 0.0348(15) 0.062(2) 0.0008(14) 0.0189(15) -0.0092(13) C27 0.0326(13) 0.0319(13) 0.0317(13) 0.0003(10) 0.0106(11) 0.0078(10) C28 0.070(2) 0.0492(17) 0.0371(16) -0.0017(13) 0.0250(15) 0.0021(15) C29 0.0473(16) 0.0379(15) 0.0443(16) -0.0011(12) 0.0162(13) -0.0026(12) C30 0.0373(14) 0.0363(14) 0.0231(12) 0.0026(10) 0.0086(10) -0.0017(11) C31 0.0352(15) 0.0471(16) 0.0396(16) 0.0043(12) 0.0109(12) 0.0024(12) C32 0.0350(14) 0.0426(15) 0.0343(14) -0.0023(11) 0.0133(11) -0.0028(11) C33 0.0381(15) 0.0475(16) 0.0438(16) -0.0065(13) 0.0165(13) 0.0008(12) C34 0.0451(15) 0.0329(14) 0.0259(13) 0.0002(10) 0.0108(11) 0.0024(11) C35 0.0566(18) 0.0342(14) 0.0317(14) -0.0057(11) 0.0134(12) 0.0029(12) C36 0.0452(16) 0.0476(17) 0.0385(16) -0.0121(13) 0.0032(13) -0.0044(13) C37 0.0456(15) 0.0299(13) 0.0325(14) 0.0033(11) 0.0122(12) -0.0042(11) C38 0.075(2) 0.0274(14) 0.0394(16) -0.0011(12) 0.0090(15) -0.0113(14) C39 0.0460(18) 0.062(2) 0.0525(19) 0.0053(15) 0.0154(15) -0.0200(15) _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 Ca1 N3 2.3174(19) . ? Ca1 N1 2.3806(17) . ? Ca1 O1 2.3843(15) . ? Ca1 N2 2.3850(18) . ? Si1 N3 1.697(2) . ? Si1 C36 1.880(3) . ? Si1 C34 1.880(3) . ? Si1 C35 1.880(3) . ? Si2 N3 1.7003(19) . ? Si2 C37 1.877(3) . ? Si2 C39 1.882(3) . ? Si2 C38 1.890(3) . ? O1 C30 1.438(3) . ? O1 C32 1.455(3) . ? N1 C3 1.330(3) . ? N1 C18 1.445(3) . ? N2 C1 1.330(3) . ? N2 C6 1.437(3) . ? C1 C2 1.408(3) . ? C1 C4 1.528(3) . ? C2 C3 1.408(3) . ? C2 H2 0.9500 . ? C3 C5 1.526(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C11 1.408(3) . ? C6 C7 1.416(3) . ? C7 C8 1.394(3) . ? C7 C12 1.521(3) . ? C8 C9 1.379(4) . ? C8 H8 0.9500 . ? C9 C10 1.375(3) . ? C9 H9 0.9500 . ? C10 C11 1.393(3) . ? C10 H10 0.9500 . ? C11 C15 1.524(3) . ? C12 C13 1.528(4) . ? C12 C14 1.531(3) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.525(4) . ? C15 C17 1.533(4) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.410(3) . ? C18 C19 1.420(3) . ? C19 C20 1.395(3) . ? C19 C24 1.522(3) . ? C20 C21 1.384(4) . ? C20 H20 0.9500 . ? C21 C22 1.374(4) . ? C21 H21 0.9500 . ? C22 C23 1.402(3) . ? C22 H22 0.9500 . ? C23 C27 1.514(3) . ? C24 C26 1.530(4) . ? C24 C25 1.537(4) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.533(4) . ? C27 C29 1.533(4) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.500(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.500(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ca1 N1 124.68(6) . . ? N3 Ca1 O1 102.90(6) . . ? N1 Ca1 O1 120.40(6) . . ? N3 Ca1 N2 130.24(7) . . ? N1 Ca1 N2 81.39(6) . . ? O1 Ca1 N2 94.58(6) . . ? N3 Si1 C36 114.76(12) . . ? N3 Si1 C34 108.73(10) . . ? C36 Si1 C34 107.31(13) . . ? N3 Si1 C35 116.19(11) . . ? C36 Si1 C35 104.69(13) . . ? C34 Si1 C35 104.36(12) . . ? N3 Si2 C37 111.72(10) . . ? N3 Si2 C39 113.25(12) . . ? C37 Si2 C39 106.65(13) . . ? N3 Si2 C38 114.66(12) . . ? C37 Si2 C38 104.05(13) . . ? C39 Si2 C38 105.73(15) . . ? C30 O1 C32 113.64(18) . . ? C30 O1 Ca1 123.73(13) . . ? C32 O1 Ca1 121.63(14) . . ? C3 N1 C18 117.38(17) . . ? C3 N1 Ca1 118.15(14) . . ? C18 N1 Ca1 123.33(13) . . ? C1 N2 C6 118.03(18) . . ? C1 N2 Ca1 120.56(14) . . ? C6 N2 Ca1 121.33(13) . . ? Si1 N3 Si2 122.63(11) . . ? Si1 N3 Ca1 112.41(9) . . ? Si2 N3 Ca1 124.86(10) . . ? N2 C1 C2 124.8(2) . . ? N2 C1 C4 120.97(19) . . ? C2 C1 C4 114.22(19) . . ? C1 C2 C3 131.5(2) . . ? C1 C2 H2 114.3 . . ? C3 C2 H2 114.3 . . ? N1 C3 C2 125.55(19) . . ? N1 C3 C5 120.19(19) . . ? C2 C3 C5 114.26(19) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 120.43(19) . . ? C11 C6 N2 119.98(19) . . ? C7 C6 N2 119.48(19) . . ? C8 C7 C6 118.3(2) . . ? C8 C7 C12 120.5(2) . . ? C6 C7 C12 121.14(18) . . ? C9 C8 C7 121.4(2) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C10 C9 C8 119.8(2) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 121.6(2) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C10 C11 C6 118.4(2) . . ? C10 C11 C15 118.8(2) . . ? C6 C11 C15 122.74(19) . . ? C7 C12 C13 111.7(2) . . ? C7 C12 C14 114.10(19) . . ? C13 C12 C14 109.4(2) . . ? C7 C12 H12 107.1 . . ? C13 C12 H12 107.1 . . ? C14 C12 H12 107.1 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 110.06(19) . . ? C11 C15 C17 112.3(2) . . ? C16 C15 C17 110.4(2) . . ? C11 C15 H15 108.0 . . ? C16 C15 H15 108.0 . . ? C17 C15 H15 108.0 . . ? 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 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 120.5(2) . . ? C23 C18 N1 121.1(2) . . ? C19 C18 N1 118.3(2) . . ? C20 C19 C18 118.3(2) . . ? C20 C19 C24 120.2(2) . . ? C18 C19 C24 121.5(2) . . ? C21 C20 C19 121.5(2) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C22 C21 C20 119.8(2) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C23 121.6(2) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C22 C23 C18 118.3(2) . . ? C22 C23 C27 118.4(2) . . ? C18 C23 C27 123.3(2) . . ? C19 C24 C26 112.9(2) . . ? C19 C24 C25 112.8(2) . . ? C26 C24 C25 109.4(2) . . ? C19 C24 H24 107.1 . . ? C26 C24 H24 107.1 . . ? C25 C24 H24 107.1 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C28 111.8(2) . . ? C23 C27 C29 111.2(2) . . ? C28 C27 C29 109.5(2) . . ? C23 C27 H27 108.0 . . ? C28 C27 H27 108.0 . . ? C29 C27 H27 108.0 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O1 C30 C31 108.23(19) . . ? O1 C30 H30A 110.1 . . ? C31 C30 H30A 110.1 . . ? O1 C30 H30B 110.1 . . ? C31 C30 H30B 110.1 . . ? H30A C30 H30B 108.4 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O1 C32 C33 112.7(2) . . ? O1 C32 H32A 109.1 . . ? C33 C32 H32A 109.1 . . ? O1 C32 H32B 109.1 . . ? C33 C32 H32B 109.1 . . ? H32A C32 H32B 107.8 . . ? 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 . . ? Si1 C34 H34A 109.5 . . ? Si1 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si1 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si1 C35 H35A 109.5 . . ? Si1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si1 C36 H36A 109.5 . . ? Si1 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si1 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si2 C37 H37A 109.5 . . ? Si2 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si2 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si2 C38 H38A 109.5 . . ? Si2 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si2 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si2 C39 H39A 109.5 . . ? Si2 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si2 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Ca1 O1 C30 111.87(16) . . . . ? N1 Ca1 O1 C30 -32.34(18) . . . . ? N2 Ca1 O1 C30 -115.04(16) . . . . ? N3 Ca1 O1 C32 -55.92(17) . . . . ? N1 Ca1 O1 C32 159.88(15) . . . . ? N2 Ca1 O1 C32 77.18(16) . . . . ? N3 Ca1 N1 C3 93.51(17) . . . . ? O1 Ca1 N1 C3 -130.38(15) . . . . ? N2 Ca1 N1 C3 -40.11(16) . . . . ? N3 Ca1 N1 C18 -73.97(18) . . . . ? O1 Ca1 N1 C18 62.14(17) . . . . ? N2 Ca1 N1 C18 152.42(17) . . . . ? N3 Ca1 N2 C1 -93.95(17) . . . . ? N1 Ca1 N2 C1 34.80(16) . . . . ? O1 Ca1 N2 C1 154.88(16) . . . . ? N3 Ca1 N2 C6 82.78(17) . . . . ? N1 Ca1 N2 C6 -148.47(16) . . . . ? O1 Ca1 N2 C6 -28.39(16) . . . . ? C36 Si1 N3 Si2 58.23(17) . . . . ? C34 Si1 N3 Si2 178.38(13) . . . . ? C35 Si1 N3 Si2 -64.33(17) . . . . ? C36 Si1 N3 Ca1 -118.32(13) . . . . ? C34 Si1 N3 Ca1 1.83(14) . . . . ? C35 Si1 N3 Ca1 119.12(12) . . . . ? C37 Si2 N3 Si1 157.06(13) . . . . ? C39 Si2 N3 Si1 -82.48(17) . . . . ? C38 Si2 N3 Si1 38.99(19) . . . . ? C37 Si2 N3 Ca1 -26.83(16) . . . . ? C39 Si2 N3 Ca1 93.63(16) . . . . ? C38 Si2 N3 Ca1 -144.90(14) . . . . ? N1 Ca1 N3 Si1 -62.36(12) . . . . ? O1 Ca1 N3 Si1 155.48(9) . . . . ? N2 Ca1 N3 Si1 47.95(13) . . . . ? N1 Ca1 N3 Si2 121.19(11) . . . . ? O1 Ca1 N3 Si2 -20.97(13) . . . . ? N2 Ca1 N3 Si2 -128.50(11) . . . . ? C6 N2 C1 C2 167.5(2) . . . . ? Ca1 N2 C1 C2 -15.6(3) . . . . ? C6 N2 C1 C4 -11.7(3) . . . . ? Ca1 N2 C1 C4 165.16(16) . . . . ? N2 C1 C2 C3 -18.9(4) . . . . ? C4 C1 C2 C3 160.3(2) . . . . ? C18 N1 C3 C2 -163.7(2) . . . . ? Ca1 N1 C3 C2 28.0(3) . . . . ? C18 N1 C3 C5 17.0(3) . . . . ? Ca1 N1 C3 C5 -151.27(17) . . . . ? C1 C2 C3 N1 11.2(4) . . . . ? C1 C2 C3 C5 -169.4(2) . . . . ? C1 N2 C6 C11 -71.9(3) . . . . ? Ca1 N2 C6 C11 111.33(19) . . . . ? C1 N2 C6 C7 112.0(2) . . . . ? Ca1 N2 C6 C7 -64.8(2) . . . . ? C11 C6 C7 C8 1.1(3) . . . . ? N2 C6 C7 C8 177.2(2) . . . . ? C11 C6 C7 C12 178.2(2) . . . . ? N2 C6 C7 C12 -5.7(3) . . . . ? C6 C7 C8 C9 -0.2(4) . . . . ? C12 C7 C8 C9 -177.4(2) . . . . ? C7 C8 C9 C10 -0.5(4) . . . . ? C8 C9 C10 C11 0.4(4) . . . . ? C9 C10 C11 C6 0.5(3) . . . . ? C9 C10 C11 C15 -178.0(2) . . . . ? C7 C6 C11 C10 -1.2(3) . . . . ? N2 C6 C11 C10 -177.3(2) . . . . ? C7 C6 C11 C15 177.2(2) . . . . ? N2 C6 C11 C15 1.1(3) . . . . ? C8 C7 C12 C13 101.7(2) . . . . ? C6 C7 C12 C13 -75.3(3) . . . . ? C8 C7 C12 C14 -23.1(3) . . . . ? C6 C7 C12 C14 159.9(2) . . . . ? C10 C11 C15 C16 71.8(3) . . . . ? C6 C11 C15 C16 -106.5(2) . . . . ? C10 C11 C15 C17 -51.6(3) . . . . ? C6 C11 C15 C17 130.0(2) . . . . ? C3 N1 C18 C23 -97.5(2) . . . . ? Ca1 N1 C18 C23 70.0(2) . . . . ? C3 N1 C18 C19 85.7(2) . . . . ? Ca1 N1 C18 C19 -106.7(2) . . . . ? C23 C18 C19 C20 3.0(3) . . . . ? N1 C18 C19 C20 179.71(19) . . . . ? C23 C18 C19 C24 -176.8(2) . . . . ? N1 C18 C19 C24 -0.1(3) . . . . ? C18 C19 C20 C21 -1.1(3) . . . . ? C24 C19 C20 C21 178.7(2) . . . . ? C19 C20 C21 C22 -0.7(4) . . . . ? C20 C21 C22 C23 0.7(4) . . . . ? C21 C22 C23 C18 1.1(3) . . . . ? C21 C22 C23 C27 -179.1(2) . . . . ? C19 C18 C23 C22 -3.0(3) . . . . ? N1 C18 C23 C22 -179.61(19) . . . . ? C19 C18 C23 C27 177.2(2) . . . . ? N1 C18 C23 C27 0.6(3) . . . . ? C20 C19 C24 C26 92.0(3) . . . . ? C18 C19 C24 C26 -88.2(3) . . . . ? C20 C19 C24 C25 -32.8(3) . . . . ? C18 C19 C24 C25 147.0(2) . . . . ? C22 C23 C27 C28 -65.7(3) . . . . ? C18 C23 C27 C28 114.1(2) . . . . ? C22 C23 C27 C29 57.1(3) . . . . ? C18 C23 C27 C29 -123.1(2) . . . . ? C32 O1 C30 C31 167.2(2) . . . . ? Ca1 O1 C30 C31 -1.4(3) . . . . ? C30 O1 C32 C33 62.8(3) . . . . ? Ca1 O1 C32 C33 -128.28(19) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.446 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.078 data_aug1906 _database_code_depnum_ccdc_archive 'CCDC 762133' #TrackingRef '- bigcif.cif' _audit_creation_date 2006-08-24T11:21:18-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C35 H59 Ca N3 Si2, 0.5(C5 H12)' _chemical_formula_sum 'C37.5 H65 Ca N3 Si2' _chemical_formula_weight 654.19 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/n' _symmetry_space_group_name_Hall '-P 4bc' _symmetry_Int_Tables_number 86 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' _cell_length_a 26.9889(11) _cell_length_b 26.9889(11) _cell_length_c 11.5798(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8434.7(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 19623 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.03 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2872 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.231 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8862 _exptl_absorpt_correction_T_max 0.9328 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.315383E-1 _diffrn_orient_matrix_ub_12 0.58376E-2 _diffrn_orient_matrix_ub_13 0.43236E-1 _diffrn_orient_matrix_ub_21 0.181677E-1 _diffrn_orient_matrix_ub_22 0.37659E-2 _diffrn_orient_matrix_ub_23 -0.747502E-1 _diffrn_orient_matrix_ub_31 -0.69385E-2 _diffrn_orient_matrix_ub_32 0.363952E-1 _diffrn_orient_matrix_ub_33 0.7997E-3 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0931 _diffrn_reflns_av_unetI/netI 0.1244 _diffrn_reflns_number 26227 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 26.01 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 8203 _reflns_number_gt 4367 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; There is a poorly defined molecule of pentane solvate lying on a 2-fold axis which was incleded with isotropic C atoms and SADI restraints. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0806P)^2^+10.1501P] 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_number_reflns 8203 _refine_ls_number_parameters 382 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1658 _refine_ls_R_factor_gt 0.0807 _refine_ls_wR_factor_ref 0.2088 _refine_ls_wR_factor_gt 0.1715 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.59 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.066 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Ca Ca 0.44262(3) 0.17638(3) 0.21587(6) 0.0267(2) Uani 1 1 d . . . Si1 Si 0.49748(5) 0.27832(5) 0.27423(13) 0.0503(4) Uani 1 1 d . . . Si2 Si 0.39240(5) 0.28282(4) 0.36061(10) 0.0337(3) Uani 1 1 d . . . N1 N 0.48683(12) 0.10371(13) 0.2466(3) 0.0277(8) Uani 1 1 d . . . N2 N 0.46167(12) 0.15895(12) 0.0238(3) 0.0272(8) Uani 1 1 d . . . N3 N 0.43987(13) 0.25504(12) 0.2917(3) 0.0315(8) Uani 1 1 d . . . C1 C 0.47085(15) 0.06632(16) 0.1830(3) 0.0300(10) Uani 1 1 d . . . C2 C 0.45091(15) 0.07185(15) 0.0710(3) 0.0279(10) Uani 1 1 d . . . H2 H 0.4341 0.0434 0.0426 0.033 Uiso 1 1 calc R . . C3 C 0.45173(16) 0.11258(16) -0.0060(3) 0.0296(10) Uani 1 1 d . . . C4 C 0.47131(18) 0.01416(16) 0.2305(4) 0.0396(11) Uani 1 1 d . . . H4A H 0.5016 0.009 0.2757 0.059 Uiso 1 1 calc R . . H4B H 0.4703 -0.0096 0.1665 0.059 Uiso 1 1 calc R . . H4C H 0.4423 0.0092 0.2801 0.059 Uiso 1 1 calc R . . C5 C 0.43802(17) 0.10025(17) -0.1306(3) 0.0369(11) Uani 1 1 d . . . H5A H 0.4066 0.1163 -0.1503 0.055 Uiso 1 1 calc R . . H5B H 0.4346 0.0643 -0.1391 0.055 Uiso 1 1 calc R . . H5C H 0.4641 0.1122 -0.1825 0.055 Uiso 1 1 calc R . . C6 C 0.51559(16) 0.09455(15) 0.3490(3) 0.0308(10) Uani 1 1 d . . . C7 C 0.56732(16) 0.09101(16) 0.3398(4) 0.0356(11) Uani 1 1 d . . . C8 C 0.59537(18) 0.08534(18) 0.4404(4) 0.0456(13) Uani 1 1 d . . . H8 H 0.6304 0.0823 0.4349 0.055 Uiso 1 1 calc R . . C9 C 0.57310(19) 0.08413(19) 0.5473(4) 0.0478(13) Uani 1 1 d . . . H9 H 0.5926 0.0801 0.615 0.057 Uiso 1 1 calc R . . C10 C 0.52264(18) 0.08877(18) 0.5559(4) 0.0435(12) Uani 1 1 d . . . H10 H 0.5077 0.0886 0.6301 0.052 Uiso 1 1 calc R . . C11 C 0.49268(17) 0.09375(16) 0.4587(3) 0.0337(11) Uani 1 1 d . . . C12 C 0.59305(17) 0.09283(19) 0.2217(4) 0.0461(13) Uani 1 1 d . . . H12 H 0.571 0.1119 0.1683 0.055 Uiso 1 1 calc R . . C13 C 0.6427(2) 0.1196(2) 0.2255(5) 0.0713(18) Uani 1 1 d . . . H13A H 0.6574 0.1199 0.1481 0.107 Uiso 1 1 calc R . . H13B H 0.665 0.1024 0.279 0.107 Uiso 1 1 calc R . . H13C H 0.6377 0.1537 0.2519 0.107 Uiso 1 1 calc R . . C14 C 0.5995(2) 0.0413(2) 0.1705(5) 0.0678(17) Uani 1 1 d . . . H14A H 0.5673 0.0247 0.1669 0.102 Uiso 1 1 calc R . . H14B H 0.6221 0.022 0.2191 0.102 Uiso 1 1 calc R . . H14C H 0.6133 0.0441 0.0925 0.102 Uiso 1 1 calc R . . C15 C 0.43734(17) 0.09877(18) 0.4736(4) 0.0402(12) Uani 1 1 d . . . H15 H 0.4218 0.0962 0.3955 0.048 Uiso 1 1 calc R . . C16 C 0.4240(2) 0.1496(2) 0.5236(5) 0.0556(15) Uani 1 1 d . . . H16A H 0.388 0.152 0.5325 0.083 Uiso 1 1 calc R . . H16B H 0.4355 0.1756 0.4711 0.083 Uiso 1 1 calc R . . H16C H 0.4399 0.1536 0.599 0.083 Uiso 1 1 calc R . . C17 C 0.4157(2) 0.0577(2) 0.5490(4) 0.0538(14) Uani 1 1 d . . . H17A H 0.3798 0.0623 0.556 0.081 Uiso 1 1 calc R . . H17B H 0.4309 0.0589 0.6258 0.081 Uiso 1 1 calc R . . H17C H 0.4225 0.0254 0.5134 0.081 Uiso 1 1 calc R . . C18 C 0.47035(17) 0.19521(15) -0.0658(3) 0.0308(10) Uani 1 1 d . . . C19 C 0.51927(17) 0.20300(17) -0.1033(4) 0.0363(11) Uani 1 1 d . . . C20 C 0.5279(2) 0.2386(2) -0.1878(4) 0.0534(14) Uani 1 1 d . . . H20 H 0.5606 0.2433 -0.2162 0.064 Uiso 1 1 calc R . . C21 C 0.4900(2) 0.2673(2) -0.2308(4) 0.0611(16) Uani 1 1 d . . . H21 H 0.4966 0.2916 -0.288 0.073 Uiso 1 1 calc R . . C22 C 0.4424(2) 0.26047(18) -0.1906(4) 0.0475(13) Uani 1 1 d . . . H22 H 0.4165 0.281 -0.2191 0.057 Uiso 1 1 calc R . . C23 C 0.43125(17) 0.22421(16) -0.1093(3) 0.0335(11) Uani 1 1 d . . . C24 C 0.56240(17) 0.17285(19) -0.0569(4) 0.0460(13) Uani 1 1 d . . . H24 H 0.552 0.1595 0.0199 0.055 Uiso 1 1 calc R . . C25 C 0.6086(2) 0.2048(3) -0.0362(5) 0.079(2) Uani 1 1 d . . . H25A H 0.6354 0.1841 -0.0057 0.118 Uiso 1 1 calc R . . H25B H 0.6008 0.231 0.0195 0.118 Uiso 1 1 calc R . . H25C H 0.6192 0.2198 -0.1093 0.118 Uiso 1 1 calc R . . C26 C 0.5743(2) 0.1287(2) -0.1327(6) 0.0794(19) Uani 1 1 d . . . H26A H 0.6018 0.11 -0.0987 0.119 Uiso 1 1 calc R . . H26B H 0.5837 0.1402 -0.2099 0.119 Uiso 1 1 calc R . . H26C H 0.5451 0.1073 -0.1385 0.119 Uiso 1 1 calc R . . C27 C 0.37840(17) 0.21772(17) -0.0698(4) 0.0380(11) Uani 1 1 d . . . H27 H 0.3766 0.1863 -0.0243 0.046 Uiso 1 1 calc R . . C28 C 0.3631(2) 0.2601(2) 0.0094(5) 0.0583(15) Uani 1 1 d . . . H28A H 0.3288 0.255 0.0349 0.087 Uiso 1 1 calc R . . H28B H 0.3655 0.2915 -0.0325 0.087 Uiso 1 1 calc R . . H28C H 0.385 0.2609 0.0768 0.087 Uiso 1 1 calc R . . C29 C 0.3419(2) 0.2133(2) -0.1715(4) 0.0567(15) Uani 1 1 d . . . H29A H 0.3082 0.2085 -0.1417 0.085 Uiso 1 1 calc R . . H29B H 0.3511 0.185 -0.2198 0.085 Uiso 1 1 calc R . . H29C H 0.343 0.2437 -0.2178 0.085 Uiso 1 1 calc R . . C30 C 0.5029(3) 0.3165(3) 0.1364(6) 0.096(2) Uani 1 1 d . . . H30A H 0.4907 0.2969 0.0709 0.144 Uiso 1 1 calc R . . H30B H 0.5376 0.3254 0.1235 0.144 Uiso 1 1 calc R . . H30C H 0.483 0.3467 0.144 0.144 Uiso 1 1 calc R . . C31 C 0.54070(19) 0.2265(2) 0.2499(6) 0.0671(17) Uani 1 1 d . . . H31A H 0.5283 0.2056 0.1871 0.101 Uiso 1 1 calc R . . H31B H 0.5434 0.2067 0.3206 0.101 Uiso 1 1 calc R . . H31C H 0.5734 0.2396 0.2292 0.101 Uiso 1 1 calc R . . C32 C 0.5210(3) 0.3177(3) 0.3897(7) 0.108(3) Uani 1 1 d . . . H32A H 0.4981 0.3454 0.4022 0.162 Uiso 1 1 calc R . . H32B H 0.5537 0.3306 0.368 0.162 Uiso 1 1 calc R . . H32C H 0.5239 0.2983 0.4609 0.162 Uiso 1 1 calc R . . C33 C 0.33489(18) 0.24457(17) 0.3575(4) 0.0477(13) Uani 1 1 d . . . H33A H 0.3266 0.2363 0.2773 0.072 Uiso 1 1 calc R . . H33B H 0.3075 0.2633 0.3921 0.072 Uiso 1 1 calc R . . H33C H 0.3402 0.214 0.4014 0.072 Uiso 1 1 calc R . . C34 C 0.4051(2) 0.2971(2) 0.5168(4) 0.0535(15) Uani 1 1 d . . . H34A H 0.4351 0.3174 0.5228 0.08 Uiso 1 1 calc R . . H34B H 0.4099 0.266 0.5594 0.08 Uiso 1 1 calc R . . H34C H 0.377 0.3152 0.5496 0.08 Uiso 1 1 calc R . . C35 C 0.37235(17) 0.34436(15) 0.2965(4) 0.0355(11) Uani 1 1 d . . . H35A H 0.4006 0.3671 0.2949 0.053 Uiso 1 1 calc R . . H35B H 0.3459 0.3586 0.3439 0.053 Uiso 1 1 calc R . . H35C H 0.3602 0.3391 0.2178 0.053 Uiso 1 1 calc R . . C1S C 0.75 0.25 0.077(3) 0.360(17) Uiso 1 2 d SD . 1 H1S1 H 0.7736 0.2673 0.0258 0.432 Uiso 0.5 1 calc PR . 1 H1S2 H 0.7264 0.2327 0.0258 0.432 Uiso 0.5 1 calc PR . 1 C2S C 0.7832(11) 0.2047(8) 0.141(2) 0.472(18) Uiso 1 1 d D A 1 H2S1 H 0.8168 0.2171 0.1598 0.567 Uiso 1 1 calc R A 1 H2S2 H 0.7669 0.1945 0.2139 0.567 Uiso 1 1 calc R A 1 C3S C 0.7872(8) 0.1569(8) 0.0525(18) 0.343(11) Uiso 1 1 d D A 1 H3S1 H 0.8067 0.1306 0.089 0.514 Uiso 1 1 calc R A 1 H3S2 H 0.8033 0.1672 -0.0194 0.514 Uiso 1 1 calc R A 1 H3S3 H 0.7538 0.1444 0.0355 0.514 Uiso 1 1 calc R A 1 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 0.0305(5) 0.0245(5) 0.0249(4) -0.0019(4) -0.0004(4) 0.0030(4) Si1 0.0467(9) 0.0322(8) 0.0720(10) -0.0124(7) 0.0092(8) -0.0091(7) Si2 0.0418(8) 0.0274(7) 0.0318(6) -0.0017(5) 0.0011(6) 0.0050(6) N1 0.031(2) 0.030(2) 0.0220(17) 0.0020(15) 0.0010(15) 0.0024(17) N2 0.031(2) 0.027(2) 0.0229(17) 0.0024(15) -0.0025(15) 0.0003(16) N3 0.037(2) 0.0233(19) 0.0340(19) -0.0022(16) 0.0032(17) -0.0003(17) C1 0.029(2) 0.029(2) 0.032(2) -0.0007(19) 0.0038(19) 0.008(2) C2 0.031(2) 0.024(2) 0.029(2) -0.0031(18) -0.0027(19) -0.0018(19) C3 0.030(2) 0.033(3) 0.026(2) -0.0050(19) 0.0005(18) 0.003(2) C4 0.050(3) 0.028(3) 0.040(3) 0.006(2) -0.003(2) 0.005(2) C5 0.050(3) 0.034(3) 0.027(2) -0.002(2) -0.002(2) 0.003(2) C6 0.036(3) 0.024(2) 0.031(2) 0.0009(19) -0.008(2) 0.009(2) C7 0.032(3) 0.033(3) 0.042(2) 0.008(2) -0.004(2) 0.010(2) C8 0.033(3) 0.049(3) 0.055(3) 0.004(3) -0.008(2) 0.008(2) C9 0.049(3) 0.057(3) 0.038(3) 0.001(2) -0.015(2) 0.013(3) C10 0.052(3) 0.051(3) 0.028(2) 0.002(2) -0.005(2) 0.012(3) C11 0.038(3) 0.034(3) 0.030(2) 0.0028(19) -0.003(2) 0.005(2) C12 0.031(3) 0.061(3) 0.047(3) 0.013(3) 0.006(2) 0.011(2) C13 0.042(3) 0.093(5) 0.079(4) 0.015(4) 0.006(3) -0.007(3) C14 0.058(4) 0.079(4) 0.067(4) -0.016(3) 0.025(3) 0.006(3) C15 0.041(3) 0.055(3) 0.025(2) 0.011(2) 0.000(2) 0.005(3) C16 0.054(3) 0.056(4) 0.057(3) 0.013(3) 0.012(3) 0.019(3) C17 0.056(3) 0.061(4) 0.044(3) 0.009(3) 0.006(3) -0.010(3) C18 0.047(3) 0.027(2) 0.018(2) -0.0017(18) 0.000(2) -0.007(2) C19 0.042(3) 0.038(3) 0.029(2) 0.001(2) 0.003(2) -0.008(2) C20 0.052(3) 0.060(4) 0.048(3) 0.007(3) 0.008(3) -0.012(3) C21 0.078(4) 0.057(4) 0.049(3) 0.029(3) -0.002(3) -0.015(3) C22 0.058(4) 0.045(3) 0.039(3) 0.016(2) -0.010(3) -0.006(3) C23 0.045(3) 0.030(3) 0.026(2) 0.0018(19) -0.001(2) -0.003(2) C24 0.035(3) 0.058(3) 0.044(3) 0.001(3) 0.006(2) -0.002(3) C25 0.047(4) 0.109(6) 0.080(4) 0.018(4) -0.007(3) -0.022(4) C26 0.066(4) 0.086(5) 0.087(4) -0.012(4) 0.000(4) 0.026(4) C27 0.044(3) 0.036(3) 0.034(2) 0.007(2) -0.005(2) 0.005(2) C28 0.061(4) 0.053(3) 0.061(3) 0.000(3) 0.011(3) 0.009(3) C29 0.053(3) 0.069(4) 0.049(3) 0.015(3) -0.015(3) 0.003(3) C30 0.102(6) 0.079(5) 0.108(5) 0.030(4) 0.018(5) -0.021(4) C31 0.040(3) 0.062(4) 0.100(4) -0.025(3) 0.012(3) -0.013(3) C32 0.073(5) 0.102(6) 0.149(7) -0.069(5) 0.011(5) -0.031(4) C33 0.048(3) 0.032(3) 0.063(3) 0.001(2) 0.016(3) 0.003(2) C34 0.067(4) 0.062(4) 0.032(2) -0.001(2) 0.002(2) 0.028(3) C35 0.043(3) 0.026(2) 0.038(2) 0.001(2) -0.004(2) 0.002(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 2.299(3) . ? Ca N1 2.323(3) . ? Ca N2 2.331(3) . ? Si1 N3 1.689(4) . ? Si1 C32 1.822(6) . ? Si1 C31 1.843(6) . ? Si1 C30 1.904(6) . ? Si2 N3 1.685(4) . ? Si2 C33 1.865(5) . ? Si2 C34 1.881(4) . ? Si2 C35 1.898(4) . ? N1 C1 1.322(5) . ? N1 C6 1.439(5) . ? N2 C3 1.326(5) . ? N2 C18 1.445(5) . ? C1 C2 1.412(6) . ? C1 C4 1.511(6) . ? C2 C3 1.416(6) . ? C2 H2 0.95 . ? C3 C5 1.526(5) . ? 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 1.403(6) . ? C6 C11 1.413(6) . ? C7 C8 1.398(6) . ? C7 C12 1.535(6) . ? C8 C9 1.377(7) . ? C8 H8 0.95 . ? C9 C10 1.371(7) . ? C9 H9 0.95 . ? C10 C11 1.392(6) . ? C10 H10 0.95 . ? C11 C15 1.510(6) . ? C12 C14 1.521(7) . ? C12 C13 1.524(7) . ? C12 H12 1 . ? 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 1.528(6) . ? C15 C16 1.531(7) . ? C15 H15 1 . ? 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 1.406(6) . ? C18 C23 1.407(6) . ? C19 C20 1.391(6) . ? C19 C24 1.519(6) . ? C20 C21 1.375(7) . ? C20 H20 0.95 . ? C21 C22 1.380(7) . ? C21 H21 0.95 . ? C22 C23 1.391(6) . ? C22 H22 0.95 . ? C23 C27 1.508(6) . ? C24 C26 1.514(7) . ? C24 C25 1.535(7) . ? C24 H24 1 . ? 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 1.522(6) . ? C27 C29 1.541(6) . ? C27 H27 1 . ? 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 H30A 0.98 . ? C30 H30B 0.98 . ? C30 H30C 0.98 . ? C31 H31A 0.98 . ? C31 H31B 0.98 . ? C31 H31C 0.98 . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C1S C2S 1.69(2) 2_655 ? C1S C2S 1.69(2) . ? C1S H1S1 0.99 . ? C1S H1S2 0.99 . ? C2S C3S 1.65(2) . ? C2S H2S1 0.99 . ? C2S H2S2 0.99 . ? C3S H3S1 0.98 . ? C3S H3S2 0.98 . ? C3S H3S3 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 N3 Ca N1 137.53(12) . . ? N3 Ca N2 123.92(12) . . ? N1 Ca N2 82.11(11) . . ? N3 Si1 C32 116.7(3) . . ? N3 Si1 C31 108.6(2) . . ? C32 Si1 C31 109.5(3) . . ? N3 Si1 C30 111.8(3) . . ? C32 Si1 C30 105.8(4) . . ? C31 Si1 C30 103.5(3) . . ? N3 Si2 C33 112.2(2) . . ? N3 Si2 C34 114.0(2) . . ? C33 Si2 C34 106.5(2) . . ? N3 Si2 C35 114.91(19) . . ? C33 Si2 C35 103.9(2) . . ? C34 Si2 C35 104.4(2) . . ? C1 N1 C6 120.3(3) . . ? C1 N1 Ca 113.0(3) . . ? C6 N1 Ca 123.3(2) . . ? C3 N2 C18 119.1(3) . . ? C3 N2 Ca 113.2(3) . . ? C18 N2 Ca 125.7(2) . . ? Si2 N3 Si1 126.2(2) . . ? Si2 N3 Ca 128.05(19) . . ? Si1 N3 Ca 105.55(17) . . ? N1 C1 C2 123.7(4) . . ? N1 C1 C4 120.4(4) . . ? C2 C1 C4 115.8(4) . . ? C1 C2 C3 130.9(4) . . ? C1 C2 H2 114.5 . . ? C3 C2 H2 114.5 . . ? N2 C3 C2 124.9(4) . . ? N2 C3 C5 120.0(4) . . ? C2 C3 C5 115.0(4) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 120.2(4) . . ? C7 C6 N1 119.0(4) . . ? C11 C6 N1 120.5(4) . . ? C8 C7 C6 118.8(4) . . ? C8 C7 C12 120.1(4) . . ? C6 C7 C12 121.1(4) . . ? C9 C8 C7 121.1(4) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C10 C9 C8 119.7(4) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 121.9(4) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? C10 C11 C6 118.3(4) . . ? C10 C11 C15 119.4(4) . . ? C6 C11 C15 122.3(4) . . ? C14 C12 C13 110.1(4) . . ? C14 C12 C7 111.7(4) . . ? C13 C12 C7 112.8(4) . . ? C14 C12 H12 107.3 . . ? C13 C12 H12 107.3 . . ? C7 C12 H12 107.3 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C17 112.3(4) . . ? C11 C15 C16 110.9(4) . . ? C17 C15 C16 110.1(4) . . ? C11 C15 H15 107.8 . . ? C17 C15 H15 107.8 . . ? C16 C15 H15 107.8 . . ? 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 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 120.7(4) . . ? C19 C18 N2 118.4(4) . . ? C23 C18 N2 120.8(4) . . ? C20 C19 C18 118.5(4) . . ? C20 C19 C24 119.4(4) . . ? C18 C19 C24 122.0(4) . . ? C21 C20 C19 121.3(5) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C20 C21 C22 119.7(5) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C21 C22 C23 121.5(5) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C22 C23 C18 118.2(4) . . ? C22 C23 C27 119.4(4) . . ? C18 C23 C27 122.4(4) . . ? C26 C24 C19 112.3(4) . . ? C26 C24 C25 111.1(5) . . ? C19 C24 C25 112.1(4) . . ? C26 C24 H24 107 . . ? C19 C24 H24 107 . . ? C25 C24 H24 107 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C28 110.6(4) . . ? C23 C27 C29 112.5(4) . . ? C28 C27 C29 110.2(4) . . ? C23 C27 H27 107.8 . . ? C28 C27 H27 107.8 . . ? C29 C27 H27 107.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si1 C30 H30A 109.5 . . ? Si1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si1 C31 H31A 109.5 . . ? Si1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si1 C32 H32A 109.5 . . ? Si1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si2 C33 H33A 109.5 . . ? Si2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si2 C34 H34A 109.5 . . ? Si2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si2 C35 H35A 109.5 . . ? Si2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C2S C1S C2S 128(3) 2_655 . ? C2S C1S H1S1 105.3 2_655 . ? C2S C1S H1S1 105.3 . . ? C2S C1S H1S2 105.3 2_655 . ? C2S C1S H1S2 105.3 . . ? H1S1 C1S H1S2 106 . . ? C3S C2S C1S 109(2) . . ? C3S C2S H2S1 109.8 . . ? C1S C2S H2S1 109.8 . . ? C3S C2S H2S2 109.8 . . ? C1S C2S H2S2 109.8 . . ? H2S1 C2S H2S2 108.3 . . ? C2S C3S H3S1 109.5 . . ? C2S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? C2S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? #===END data_apr507 _database_code_depnum_ccdc_archive 'CCDC 762134' #TrackingRef '- bigcif.cif' _audit_creation_date 2007-04-18T15:29:21-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C43 H76 Al2 Ca N2' _chemical_formula_sum 'C43 H76 Al2 Ca N2' _chemical_formula_weight 715.1 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.1238(2) _cell_length_b 20.7676(4) _cell_length_c 19.6414(3) _cell_angle_alpha 90 _cell_angle_beta 98.304(1) _cell_angle_gamma 90 _cell_volume 4489.88(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 30011 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.058 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.207 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.892 _exptl_absorpt_correction_T_max 0.9635 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.66057E-2 _diffrn_orient_matrix_ub_12 -0.334156E-1 _diffrn_orient_matrix_ub_13 0.359302E-1 _diffrn_orient_matrix_ub_21 -0.35229E-1 _diffrn_orient_matrix_ub_22 0.328104E-1 _diffrn_orient_matrix_ub_23 0.287228E-1 _diffrn_orient_matrix_ub_31 -0.834804E-1 _diffrn_orient_matrix_ub_32 -0.11202E-1 _diffrn_orient_matrix_ub_33 -0.230513E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_unetI/netI 0.0359 _diffrn_reflns_number 40326 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 26.03 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 8781 _reflns_number_gt 6713 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The AlEt4 moiety is disordered over two overlapping orientations corresponding to two different coordination modes. Because of the incomplete resolution the two sets of positions were restrained to have similar bonds and angles using the SAME instruction. An alternative refinement using instead a set of SADI restraints on the 1,2and 1,3 distances gave a similar result. There is also disorder of the C42C43 ethyl group. The disordered atoms were left isotropic. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1088P)^2^+9.8219P] 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_number_reflns 8781 _refine_ls_number_parameters 446 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.1256 _refine_ls_R_factor_gt 0.1004 _refine_ls_wR_factor_ref 0.2742 _refine_ls_wR_factor_gt 0.2539 _refine_ls_goodness_of_fit_ref 1.06 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.867 _refine_diff_density_min -0.885 _refine_diff_density_rms 0.066 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Al Al 0.0645 0.0514 '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' 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 Ca Ca 0.94461(7) 0.12763(4) 0.75994(4) 0.0440(3) Uani 1 1 d . . . Al2 Al 1.15095(15) 0.12395(6) 0.60920(6) 0.0562(4) Uani 1 1 d . . . N1 N 1.1154(3) 0.05710(14) 0.77403(15) 0.0393(7) Uani 1 1 d . A . N2 N 1.1049(3) 0.20535(13) 0.76688(14) 0.0362(7) Uani 1 1 d . A . C1 C 1.2137(4) 0.06958(17) 0.74773(18) 0.0406(8) Uani 1 1 d . . . C2 C 1.2383(4) 0.13117(17) 0.7168(2) 0.0422(8) Uani 1 1 d . A . H2 H 1.3279 0.1326 0.7157 0.051 Uiso 1 1 calc R . . C3 C 1.2048(3) 0.19417(17) 0.74140(17) 0.0379(8) Uani 1 1 d . . . C4 C 1.3114(4) 0.0192(2) 0.7465(2) 0.0554(11) Uani 1 1 d . A . H4A H 1.3714 0.0232 0.7881 0.083 Uiso 1 1 calc R . . H4B H 1.3515 0.0255 0.7058 0.083 Uiso 1 1 calc R . . H4C H 1.2746 -0.0238 0.745 0.083 Uiso 1 1 calc R . . C5 C 1.2962(4) 0.24669(19) 0.7344(2) 0.0516(10) Uani 1 1 d . A . H5A H 1.3047 0.2522 0.6858 0.077 Uiso 1 1 calc R . . H5B H 1.375 0.2348 0.7605 0.077 Uiso 1 1 calc R . . H5C H 1.2683 0.2871 0.7525 0.077 Uiso 1 1 calc R . . C6 C 1.1033(4) -0.00499(17) 0.8059(2) 0.0441(9) Uani 1 1 d . . . C7 C 1.0472(4) -0.05627(18) 0.7662(2) 0.0518(10) Uani 1 1 d . A . C8 C 1.0249(5) -0.1133(2) 0.7998(3) 0.0601(12) Uani 1 1 d . . . H8 H 0.9857 -0.148 0.7741 0.072 Uiso 1 1 calc R A . C9 C 1.0587(5) -0.1201(2) 0.8696(3) 0.0621(12) Uani 1 1 d . A . H9 H 1.043 -0.1593 0.8916 0.074 Uiso 1 1 calc R . . C10 C 1.1150(4) -0.0704(2) 0.9072(2) 0.0563(11) Uani 1 1 d . . . H10 H 1.1378 -0.0757 0.9554 0.068 Uiso 1 1 calc R A . C11 C 1.1399(4) -0.01210(18) 0.8769(2) 0.0460(9) Uani 1 1 d . A . C12 C 1.0114(5) -0.0521(2) 0.6888(2) 0.0656(13) Uani 1 1 d . . . H12 H 1.0453 -0.011 0.6731 0.079 Uiso 1 1 calc R A . C13 C 0.8730(6) -0.0497(3) 0.6688(3) 0.095(2) Uani 1 1 d . A . H13A H 0.8362 -0.0867 0.6887 0.142 Uiso 1 1 calc R . . H13B H 0.8528 -0.0509 0.6186 0.142 Uiso 1 1 calc R . . H13C H 0.8416 -0.0098 0.6862 0.142 Uiso 1 1 calc R . . C14 C 1.0662(7) -0.1075(2) 0.6523(3) 0.091(2) Uani 1 1 d . A . H14A H 1.155 -0.1061 0.6632 0.136 Uiso 1 1 calc R . . H14B H 1.0424 -0.1034 0.6025 0.136 Uiso 1 1 calc R . . H14C H 1.0365 -0.1486 0.6679 0.136 Uiso 1 1 calc R . . C15 C 1.2049(4) 0.0413(2) 0.9215(2) 0.0510(10) Uani 1 1 d . . . H15 H 1.2116 0.0796 0.8914 0.061 Uiso 1 1 calc R A . C16 C 1.3322(5) 0.0211(3) 0.9519(3) 0.0779(15) Uani 1 1 d . A . H16A H 1.3279 -0.0158 0.9825 0.117 Uiso 1 1 calc R . . H16B H 1.3731 0.057 0.978 0.117 Uiso 1 1 calc R . . H16C H 1.3779 0.009 0.9147 0.117 Uiso 1 1 calc R . . C17 C 1.1311(6) 0.0612(3) 0.9780(3) 0.0777(16) Uani 1 1 d . A . H17A H 1.1199 0.0238 1.0069 0.117 Uiso 1 1 calc R . . H17B H 1.0516 0.0774 0.9569 0.117 Uiso 1 1 calc R . . H17C H 1.1746 0.0951 1.0063 0.117 Uiso 1 1 calc R . . C18 C 1.0817(4) 0.26952(17) 0.7906(2) 0.0429(8) Uani 1 1 d . . . C19 C 1.0970(5) 0.2811(2) 0.8616(2) 0.0599(12) Uani 1 1 d . A . C20 C 1.0691(7) 0.3418(3) 0.8847(3) 0.088(2) Uani 1 1 d . . . H20 H 1.0808 0.3507 0.9327 0.106 Uiso 1 1 calc R A . C21 C 1.0246(7) 0.3891(3) 0.8390(3) 0.0848(18) Uani 1 1 d . A . H21 H 1.0057 0.4303 0.8556 0.102 Uiso 1 1 calc R . . C22 C 1.0072(5) 0.3774(2) 0.7697(3) 0.0664(13) Uani 1 1 d . . . H22 H 0.9751 0.4104 0.7388 0.08 Uiso 1 1 calc R A . C23 C 1.0361(4) 0.31772(18) 0.7437(2) 0.0480(9) Uani 1 1 d . A . C24 C 1.1438(5) 0.2288(2) 0.9136(2) 0.0670(14) Uani 1 1 d . . . H24 H 1.109 0.187 0.8948 0.08 Uiso 1 1 calc R A . C25 C 1.2809(6) 0.2225(3) 0.9216(3) 0.0813(17) Uani 1 1 d . A . H25A H 1.3183 0.2642 0.9347 0.122 Uiso 1 1 calc R . . H25B H 1.3051 0.2084 0.8779 0.122 Uiso 1 1 calc R . . H25C H 1.308 0.1907 0.9574 0.122 Uiso 1 1 calc R . . C26 C 1.1030(8) 0.2381(3) 0.9837(3) 0.106(3) Uani 1 1 d . A . H26A H 1.1328 0.2022 1.0139 0.159 Uiso 1 1 calc R . . H26B H 1.0141 0.2393 0.9783 0.159 Uiso 1 1 calc R . . H26C H 1.1359 0.2787 1.0039 0.159 Uiso 1 1 calc R . . C27 C 1.0149(5) 0.30801(19) 0.6671(2) 0.0565(11) Uani 1 1 d . . . H27 H 1.052 0.2659 0.6569 0.068 Uiso 1 1 calc R A . C28 C 0.8781(6) 0.3048(3) 0.6398(3) 0.091(2) Uani 1 1 d . A . H28A H 0.8409 0.2697 0.6628 0.136 Uiso 1 1 calc R . . H28B H 0.8666 0.297 0.5901 0.136 Uiso 1 1 calc R . . H28C H 0.8396 0.3457 0.6492 0.136 Uiso 1 1 calc R . . C29 C 1.0753(7) 0.3609(2) 0.6296(3) 0.0823(18) Uani 1 1 d . A . H29A H 1.034 0.402 0.6345 0.123 Uiso 1 1 calc R . . H29B H 1.0696 0.35 0.5807 0.123 Uiso 1 1 calc R . . H29C H 1.1609 0.3647 0.6496 0.123 Uiso 1 1 calc R . . C38 C 0.9726(5) 0.12416(18) 0.6189(2) 0.0546(11) Uani 1 1 d . A . H38A H 0.9551 0.0866 0.6469 0.066 Uiso 1 1 calc R . . H38B H 0.9542 0.1635 0.6438 0.066 Uiso 1 1 calc R . . C39 C 0.8894(7) 0.1217(3) 0.5495(3) 0.091(2) Uani 1 1 d . . . H39A H 0.9036 0.1598 0.5223 0.137 Uiso 1 1 calc R A . H39B H 0.8044 0.121 0.5573 0.137 Uiso 1 1 calc R . . H39C H 0.9071 0.0828 0.5246 0.137 Uiso 1 1 calc R . . C40 C 1.1999(6) 0.0420(2) 0.5694(3) 0.0814(17) Uani 1 1 d . A . H40A H 1.1962 0.008 0.6044 0.098 Uiso 1 1 calc R . . H40B H 1.1372 0.0314 0.5299 0.098 Uiso 1 1 calc R . . C41 C 1.3196(10) 0.0365(4) 0.5452(4) 0.136(4) Uani 1 1 d . . . H41A H 1.3228 0.0662 0.5068 0.205 Uiso 1 1 calc R A . H41B H 1.3311 -0.0077 0.53 0.205 Uiso 1 1 calc R . . H41C H 1.384 0.0473 0.583 0.205 Uiso 1 1 calc R . . Al1 Al 0.7102(2) 0.13408(13) 0.81230(16) 0.0407(8) Uiso 0.543(8) 1 d PD A 1 C30 C 0.8230(9) 0.2094(4) 0.8466(6) 0.069(3) Uiso 0.543(8) 1 d PD A 1 H30A H 0.8543 0.2025 0.8958 0.083 Uiso 0.543(8) 1 calc PR A 1 H30B H 0.8934 0.2092 0.821 0.083 Uiso 0.543(8) 1 calc PR A 1 C31 C 0.7631(12) 0.2749(6) 0.8387(7) 0.097(4) Uiso 0.543(8) 1 d PD A 1 H31A H 0.7698 0.2921 0.7929 0.145 Uiso 0.543(8) 1 calc PR A 1 H31B H 0.8035 0.3041 0.8739 0.145 Uiso 0.543(8) 1 calc PR A 1 H31C H 0.6772 0.2708 0.8439 0.145 Uiso 0.543(8) 1 calc PR A 1 C32 C 0.8087(6) 0.0558(3) 0.8512(5) 0.0408(18) Uiso 0.543(8) 1 d PD A 1 H32A H 0.8828 0.0505 0.8292 0.049 Uiso 0.543(8) 1 calc PR A 1 H32B H 0.8325 0.0597 0.9016 0.049 Uiso 0.543(8) 1 calc PR A 1 C33 C 0.7169(12) -0.0028(6) 0.8326(7) 0.080(3) Uiso 0.543(8) 1 d PD A 1 H33A H 0.6366 0.0089 0.8435 0.121 Uiso 0.543(8) 1 calc PR A 1 H33B H 0.7469 -0.0408 0.8594 0.121 Uiso 0.543(8) 1 calc PR A 1 H33C H 0.711 -0.0126 0.7834 0.121 Uiso 0.543(8) 1 calc PR A 1 C34 C 0.6851(14) 0.1287(7) 0.7104(7) 0.106(4) Uiso 0.543(8) 1 d PD A 1 H34A H 0.7659 0.1338 0.6956 0.127 Uiso 0.543(8) 1 calc PR A 1 H34B H 0.6581 0.0842 0.6983 0.127 Uiso 0.543(8) 1 calc PR A 1 C35 C 0.6080(16) 0.1688(9) 0.6706(9) 0.131(6) Uiso 0.543(8) 1 d PD A 1 H35A H 0.5254 0.1631 0.6815 0.196 Uiso 0.543(8) 1 calc PR A 1 H35B H 0.6093 0.1588 0.622 0.196 Uiso 0.543(8) 1 calc PR A 1 H35C H 0.6336 0.2135 0.6797 0.196 Uiso 0.543(8) 1 calc PR A 1 C36 C 0.5618(7) 0.1469(5) 0.8541(4) 0.059(2) Uiso 0.543(8) 1 d PD A 1 H36A H 0.5215 0.1869 0.8352 0.071 Uiso 0.543(8) 1 calc PR A 1 H36B H 0.5056 0.1107 0.8405 0.071 Uiso 0.543(8) 1 calc PR A 1 C37 C 0.5825(9) 0.1515(6) 0.9308(5) 0.061(3) Uiso 0.543(8) 1 d PD A 1 H37A H 0.6448 0.1203 0.9494 0.092 Uiso 0.543(8) 1 calc PR A 1 H37B H 0.5066 0.142 0.9486 0.092 Uiso 0.543(8) 1 calc PR A 1 H37C H 0.6096 0.1951 0.9445 0.092 Uiso 0.543(8) 1 calc PR A 1 C42 C 1.1764(9) 0.2005(4) 0.5548(4) 0.053(2) Uiso 0.578(12) 1 d PD A 1 H42A H 1.1247 0.1971 0.5095 0.063 Uiso 0.578(12) 1 calc PR A 1 H42B H 1.1494 0.2389 0.5784 0.063 Uiso 0.578(12) 1 calc PR A 1 C43 C 1.3089(9) 0.2107(5) 0.5431(6) 0.084(3) Uiso 0.578(12) 1 d PD A 1 H43A H 1.362 0.2098 0.5875 0.126 Uiso 0.578(12) 1 calc PR A 1 H43B H 1.3164 0.2524 0.5209 0.126 Uiso 0.578(12) 1 calc PR A 1 H43C H 1.3326 0.1763 0.5136 0.126 Uiso 0.578(12) 1 calc PR A 1 Al1A Al 0.6962(4) 0.1180(2) 0.7888(3) 0.0714(13) Uiso 0.457(8) 1 d PD A 2 C30A C 0.7860(11) 0.2057(5) 0.8007(8) 0.081(4) Uiso 0.457(8) 1 d PD A 2 H30C H 0.837 0.207 0.8463 0.098 Uiso 0.457(8) 1 calc PR A 2 H30D H 0.8402 0.2099 0.7651 0.098 Uiso 0.457(8) 1 calc PR A 2 C31A C 0.6971(15) 0.2621(7) 0.7945(9) 0.099(5) Uiso 0.457(8) 1 d PD A 2 H31D H 0.6554 0.2649 0.7471 0.148 Uiso 0.457(8) 1 calc PR A 2 H31E H 0.7417 0.3022 0.8066 0.148 Uiso 0.457(8) 1 calc PR A 2 H31F H 0.6372 0.2554 0.8259 0.148 Uiso 0.457(8) 1 calc PR A 2 C32A C 0.8156(13) 0.0507(7) 0.8256(10) 0.110(6) Uiso 0.457(8) 1 d PD A 2 H32C H 0.872 0.0435 0.7918 0.131 Uiso 0.457(8) 1 calc PR A 2 H32D H 0.864 0.0673 0.8683 0.131 Uiso 0.457(8) 1 calc PR A 2 C33A C 0.7611(14) -0.0140(6) 0.8417(7) 0.072(4) Uiso 0.457(8) 1 d PD A 2 H33D H 0.6922 -0.0069 0.8668 0.108 Uiso 0.457(8) 1 calc PR A 2 H33E H 0.8229 -0.0399 0.87 0.108 Uiso 0.457(8) 1 calc PR A 2 H33F H 0.7332 -0.0369 0.7987 0.108 Uiso 0.457(8) 1 calc PR A 2 C34A C 0.6499(18) 0.0928(9) 0.6927(7) 0.120(6) Uiso 0.457(8) 1 d PD A 2 H34C H 0.7264 0.0818 0.6752 0.144 Uiso 0.457(8) 1 calc PR A 2 H34D H 0.6038 0.0522 0.6935 0.144 Uiso 0.457(8) 1 calc PR A 2 C35A C 0.5898(19) 0.1278(10) 0.6469(10) 0.130(7) Uiso 0.457(8) 1 d PD A 2 H35D H 0.5028 0.123 0.6491 0.195 Uiso 0.457(8) 1 calc PR A 2 H35E H 0.6067 0.1144 0.6014 0.195 Uiso 0.457(8) 1 calc PR A 2 H35F H 0.6134 0.1729 0.6548 0.195 Uiso 0.457(8) 1 calc PR A 2 C36A C 0.5633(9) 0.1193(6) 0.8473(5) 0.059(3) Uiso 0.457(8) 1 d PD A 2 H36C H 0.5062 0.1538 0.829 0.071 Uiso 0.457(8) 1 calc PR A 2 H36D H 0.5188 0.0781 0.8392 0.071 Uiso 0.457(8) 1 calc PR A 2 C37A C 0.5888(16) 0.1285(9) 0.9224(7) 0.096(6) Uiso 0.457(8) 1 d PD A 2 H37D H 0.6636 0.1536 0.9339 0.145 Uiso 0.457(8) 1 calc PR A 2 H37E H 0.5987 0.0864 0.9451 0.145 Uiso 0.457(8) 1 calc PR A 2 H37F H 0.521 0.1515 0.9381 0.145 Uiso 0.457(8) 1 calc PR A 2 C42A C 1.2319(12) 0.1984(5) 0.5626(5) 0.047(3) Uiso 0.422(12) 1 d PD A 2 H42C H 1.2004 0.24 0.5771 0.057 Uiso 0.422(12) 1 calc PR A 2 H42D H 1.3207 0.1975 0.5779 0.057 Uiso 0.422(12) 1 calc PR A 2 C43A C 1.2070(14) 0.1935(8) 0.4830(7) 0.087(5) Uiso 0.422(12) 1 d PD A 2 H43D H 1.225 0.1497 0.4688 0.13 Uiso 0.422(12) 1 calc PR A 2 H43E H 1.2588 0.2242 0.4628 0.13 Uiso 0.422(12) 1 calc PR A 2 H43F H 1.1215 0.2034 0.4669 0.13 Uiso 0.422(12) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca 0.0386(4) 0.0414(4) 0.0495(5) 0.0065(3) -0.0016(3) -0.0011(3) Al2 0.0962(11) 0.0346(6) 0.0388(7) 0.0024(5) 0.0136(6) -0.0002(6) N1 0.0495(18) 0.0292(14) 0.0387(16) 0.0048(12) 0.0045(13) -0.0003(13) N2 0.0429(17) 0.0298(14) 0.0336(15) 0.0001(12) -0.0016(12) 0.0003(12) C1 0.053(2) 0.0333(18) 0.0356(18) 0.0033(15) 0.0084(16) 0.0047(16) C2 0.052(2) 0.0360(19) 0.0398(19) 0.0043(15) 0.0120(16) -0.0013(16) C3 0.048(2) 0.0326(17) 0.0316(17) 0.0031(14) 0.0006(15) -0.0033(15) C4 0.064(3) 0.044(2) 0.062(3) 0.0119(19) 0.020(2) 0.0119(19) C5 0.056(2) 0.040(2) 0.059(3) 0.0011(18) 0.0095(19) -0.0093(18) C6 0.052(2) 0.0313(18) 0.051(2) 0.0061(16) 0.0123(17) 0.0009(16) C7 0.064(3) 0.0314(19) 0.059(3) 0.0043(17) 0.006(2) -0.0003(18) C8 0.079(3) 0.036(2) 0.067(3) 0.005(2) 0.013(2) -0.008(2) C9 0.082(3) 0.040(2) 0.069(3) 0.016(2) 0.024(3) -0.003(2) C10 0.074(3) 0.045(2) 0.052(2) 0.0153(19) 0.019(2) 0.002(2) C11 0.054(2) 0.039(2) 0.048(2) 0.0072(16) 0.0143(18) 0.0032(17) C12 0.100(4) 0.034(2) 0.057(3) 0.0039(19) -0.007(2) -0.011(2) C13 0.113(5) 0.069(4) 0.089(4) 0.011(3) -0.029(4) -0.020(3) C14 0.172(7) 0.037(2) 0.062(3) -0.003(2) 0.014(4) -0.004(3) C15 0.067(3) 0.044(2) 0.042(2) 0.0079(17) 0.0078(18) 0.0002(19) C16 0.080(4) 0.067(3) 0.080(4) 0.011(3) -0.011(3) -0.003(3) C17 0.107(4) 0.072(3) 0.058(3) -0.011(3) 0.024(3) -0.017(3) C18 0.051(2) 0.0325(18) 0.044(2) -0.0017(15) 0.0031(16) 0.0007(16) C19 0.092(3) 0.044(2) 0.043(2) -0.0047(18) 0.008(2) 0.016(2) C20 0.154(6) 0.052(3) 0.058(3) -0.010(2) 0.014(3) 0.032(3) C21 0.136(5) 0.047(3) 0.071(3) -0.010(2) 0.015(3) 0.029(3) C22 0.090(4) 0.036(2) 0.071(3) 0.005(2) 0.004(3) 0.014(2) C23 0.058(2) 0.0330(19) 0.051(2) 0.0035(16) 0.0013(18) -0.0004(17) C24 0.110(4) 0.054(3) 0.036(2) -0.0039(19) 0.006(2) 0.023(3) C25 0.102(4) 0.078(4) 0.055(3) -0.007(3) -0.019(3) 0.017(3) C26 0.186(7) 0.087(4) 0.048(3) 0.009(3) 0.032(4) 0.054(5) C27 0.082(3) 0.034(2) 0.049(2) 0.0048(17) -0.008(2) 0.000(2) C28 0.092(4) 0.065(3) 0.100(4) -0.003(3) -0.038(3) 0.007(3) C29 0.144(6) 0.043(3) 0.061(3) 0.013(2) 0.020(3) -0.002(3) C38 0.087(3) 0.0328(19) 0.039(2) 0.0025(16) -0.008(2) -0.0023(19) C39 0.118(5) 0.091(4) 0.053(3) -0.001(3) -0.025(3) 0.005(4) C40 0.138(5) 0.050(3) 0.063(3) -0.003(2) 0.034(3) 0.016(3) C41 0.232(11) 0.083(5) 0.113(6) 0.012(4) 0.090(7) 0.042(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N1 2.383(3) . ? Ca N2 2.394(3) . ? Ca C30A 2.606(12) . ? Ca C32A 2.611(16) . ? Ca C38 2.832(4) . ? Ca C30 2.878(10) . ? Ca C34 2.910(15) . ? Ca C32 2.916(8) . ? Al2 C42 1.959(8) . ? Al2 C40 1.982(5) . ? Al2 C38 2.020(6) . ? Al2 C42A 2.069(11) . ? Al2 C2 2.201(4) . ? N1 C1 1.302(5) . ? N1 C6 1.448(4) . ? N2 C3 1.304(5) . ? N2 C18 1.447(5) . ? C1 C2 1.458(5) . ? C1 C4 1.511(5) . ? C2 C3 1.461(5) . ? C2 H2 1 . ? C3 C5 1.511(5) . ? 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 1.402(6) . ? C6 C7 1.412(6) . ? C7 C8 1.396(6) . ? C7 C12 1.516(6) . ? C8 C9 1.374(7) . ? C8 H8 0.95 . ? C9 C10 1.369(7) . ? C9 H9 0.95 . ? C10 C11 1.393(5) . ? C10 H10 0.95 . ? C11 C15 1.528(6) . ? C12 C14 1.529(7) . ? C12 C13 1.533(8) . ? C12 H12 1 . ? 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 1.514(7) . ? C15 C17 1.529(7) . ? C15 H15 1 . ? 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 1.401(6) . ? C18 C23 1.404(5) . ? C19 C20 1.392(6) . ? C19 C24 1.529(6) . ? C20 C21 1.374(8) . ? C20 H20 0.95 . ? C21 C22 1.369(8) . ? C21 H21 0.95 . ? C22 C23 1.395(6) . ? C22 H22 0.95 . ? C23 C27 1.503(6) . ? C24 C25 1.516(8) . ? C24 C26 1.524(7) . ? C24 H24 1 . ? 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 C29 1.531(7) . ? C27 C28 1.541(7) . ? C27 H27 1 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C38 C39 1.534(6) . ? C38 H38A 0.99 . ? C38 H38B 0.99 . ? C39 H39A 0.98 . ? C39 H39B 0.98 . ? C39 H39C 0.98 . ? C40 C41 1.480(10) . ? C40 H40A 0.99 . ? C40 H40B 0.99 . ? C41 H41A 0.98 . ? C41 H41B 0.98 . ? C41 H41C 0.98 . ? Al1 C36 1.965(8) . ? Al1 C34 1.983(13) . ? Al1 C32 2.046(7) . ? Al1 C30 2.057(9) . ? C30 C31 1.511(13) . ? C30 H30A 0.99 . ? C30 H30B 0.99 . ? C31 H31A 0.98 . ? C31 H31B 0.98 . ? C31 H31C 0.98 . ? C32 C33 1.597(11) . ? C32 H32A 0.99 . ? C32 H32B 0.99 . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? C34 C35 1.360(15) . ? C34 H34A 0.99 . ? C34 H34B 0.99 . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C36 C37 1.493(11) . ? C36 H36A 0.99 . ? C36 H36B 0.99 . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C42 C43 1.538(12) . ? C42 H42A 0.99 . ? C42 H42B 0.99 . ? C43 H43A 0.98 . ? C43 H43B 0.98 . ? C43 H43C 0.98 . ? Al1A C34A 1.954(15) . ? Al1A C32A 1.991(12) . ? Al1A C36A 1.999(10) . ? Al1A C30A 2.074(11) . ? C30A C31A 1.526(14) . ? C30A H30C 0.99 . ? C30A H30D 0.99 . ? C31A H31D 0.98 . ? C31A H31E 0.98 . ? C31A H31F 0.98 . ? C32A C33A 1.526(14) . ? C32A H32C 0.99 . ? C32A H32D 0.99 . ? C33A H33D 0.98 . ? C33A H33E 0.98 . ? C33A H33F 0.98 . ? C34A C35A 1.269(16) . ? C34A H34C 0.99 . ? C34A H34D 0.99 . ? C35A H35D 0.98 . ? C35A H35E 0.98 . ? C35A H35F 0.98 . ? C36A C37A 1.474(14) . ? C36A H36C 0.99 . ? C36A H36D 0.99 . ? C37A H37D 0.98 . ? C37A H37E 0.98 . ? C37A H37F 0.98 . ? C42A C43A 1.551(14) . ? C42A H42C 0.99 . ? C42A H42D 0.99 . ? C43A H43D 0.98 . ? C43A H43E 0.98 . ? C43A H43F 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 N1 Ca N2 80.39(10) . . ? N1 Ca C30A 155.6(3) . . ? N2 Ca C30A 95.4(3) . . ? N1 Ca C32A 93.0(3) . . ? N2 Ca C32A 147.4(4) . . ? C30A Ca C32A 77.5(4) . . ? N1 Ca C38 84.23(12) . . ? N2 Ca C38 83.49(12) . . ? C30A Ca C38 119.4(3) . . ? C32A Ca C38 127.9(4) . . ? N1 Ca C30 136.8(2) . . ? N2 Ca C30 88.76(19) . . ? C38 Ca C30 136.1(2) . . ? N1 Ca C34 141.2(3) . . ? N2 Ca C34 135.1(3) . . ? C38 Ca C34 85.3(3) . . ? C30 Ca C34 70.4(3) . . ? N1 Ca C32 95.13(15) . . ? N2 Ca C32 139.25(18) . . ? C38 Ca C32 136.72(18) . . ? C30 Ca C32 67.0(2) . . ? C34 Ca C32 68.4(3) . . ? C42 Al2 C40 114.4(3) . . ? C42 Al2 C38 105.7(3) . . ? C40 Al2 C38 111.6(2) . . ? C40 Al2 C42A 107.8(4) . . ? C38 Al2 C42A 122.4(4) . . ? C42 Al2 C2 113.0(3) . . ? C40 Al2 C2 109.2(2) . . ? C38 Al2 C2 102.27(17) . . ? C42A Al2 C2 102.4(3) . . ? C1 N1 C6 119.0(3) . . ? C1 N1 Ca 122.2(2) . . ? C6 N1 Ca 118.4(2) . . ? C3 N2 C18 119.3(3) . . ? C3 N2 Ca 121.8(2) . . ? C18 N2 Ca 118.2(2) . . ? N1 C1 C2 124.0(3) . . ? N1 C1 C4 121.0(3) . . ? C2 C1 C4 115.0(3) . . ? C1 C2 C3 125.1(3) . . ? C1 C2 Al2 104.9(3) . . ? C3 C2 Al2 106.3(2) . . ? C1 C2 H2 106.4 . . ? C3 C2 H2 106.4 . . ? Al2 C2 H2 106.4 . . ? N2 C3 C2 123.9(3) . . ? N2 C3 C5 121.9(3) . . ? C2 C3 C5 114.2(3) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 120.8(3) . . ? C11 C6 N1 119.5(3) . . ? C7 C6 N1 119.5(3) . . ? C8 C7 C6 118.2(4) . . ? C8 C7 C12 119.0(4) . . ? C6 C7 C12 122.9(4) . . ? C9 C8 C7 121.2(4) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C10 C9 C8 119.9(4) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 121.9(4) . . ? C9 C10 H10 119 . . ? C11 C10 H10 119 . . ? C10 C11 C6 117.9(4) . . ? C10 C11 C15 119.5(4) . . ? C6 C11 C15 122.6(3) . . ? C7 C12 C14 111.2(4) . . ? C7 C12 C13 111.6(5) . . ? C14 C12 C13 111.0(5) . . ? C7 C12 H12 107.6 . . ? C14 C12 H12 107.6 . . ? C13 C12 H12 107.6 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C11 111.3(4) . . ? C16 C15 C17 111.0(4) . . ? C11 C15 C17 110.7(4) . . ? C16 C15 H15 107.9 . . ? C11 C15 H15 107.9 . . ? C17 C15 H15 107.9 . . ? 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 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 120.7(4) . . ? C19 C18 N2 118.4(3) . . ? C23 C18 N2 120.7(3) . . ? C20 C19 C18 118.6(4) . . ? C20 C19 C24 119.7(4) . . ? C18 C19 C24 121.6(4) . . ? C21 C20 C19 120.7(5) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C22 C21 C20 120.6(5) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 121.0(4) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C22 C23 C18 118.3(4) . . ? C22 C23 C27 118.3(4) . . ? C18 C23 C27 123.4(4) . . ? C25 C24 C26 110.1(5) . . ? C25 C24 C19 111.8(5) . . ? C26 C24 C19 113.4(4) . . ? C25 C24 H24 107.1 . . ? C26 C24 H24 107.1 . . ? C19 C24 H24 107.1 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 111.6(4) . . ? C23 C27 C28 111.0(5) . . ? C29 C27 C28 110.1(4) . . ? C23 C27 H27 108 . . ? C29 C27 H27 108 . . ? C28 C27 H27 108 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C39 C38 Al2 113.0(4) . . ? C39 C38 Ca 137.1(4) . . ? Al2 C38 Ca 109.92(17) . . ? C39 C38 H38A 109 . . ? Al2 C38 H38A 109 . . ? Ca C38 H38A 54.5 . . ? C39 C38 H38B 109 . . ? Al2 C38 H38B 109 . . ? Ca C38 H38B 55.6 . . ? H38A C38 H38B 107.8 . . ? 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 . . ? C41 C40 Al2 120.2(5) . . ? C41 C40 H40A 107.3 . . ? Al2 C40 H40A 107.3 . . ? C41 C40 H40B 107.3 . . ? Al2 C40 H40B 107.3 . . ? H40A C40 H40B 106.9 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C36 Al1 C34 115.1(5) . . ? C36 Al1 C32 112.9(4) . . ? C34 Al1 C32 108.8(5) . . ? C36 Al1 C30 105.6(4) . . ? C34 Al1 C30 111.3(5) . . ? C32 Al1 C30 102.3(3) . . ? C31 C30 Al1 114.3(7) . . ? C31 C30 Ca 135.0(8) . . ? Al1 C30 Ca 71.0(3) . . ? C31 C30 H30A 108.7 . . ? Al1 C30 H30A 108.7 . . ? Ca C30 H30A 111.2 . . ? C31 C30 H30B 108.7 . . ? Al1 C30 H30B 108.7 . . ? Ca C30 H30B 39 . . ? H30A C30 H30B 107.6 . . ? C33 C32 Al1 103.3(6) . . ? C33 C32 Ca 128.3(7) . . ? Al1 C32 Ca 70.2(2) . . ? C33 C32 H32A 111.1 . . ? Al1 C32 H32A 111.1 . . ? Ca C32 H32A 41.5 . . ? C33 C32 H32B 111.1 . . ? Al1 C32 H32B 111.1 . . ? Ca C32 H32B 119.1 . . ? H32A C32 H32B 109.1 . . ? C35 C34 Al1 122.1(13) . . ? C35 C34 Ca 135.2(12) . . ? Al1 C34 Ca 71.0(4) . . ? C35 C34 H34A 106.8 . . ? Al1 C34 H34A 106.8 . . ? Ca C34 H34A 36.9 . . ? C35 C34 H34B 106.8 . . ? Al1 C34 H34B 106.8 . . ? Ca C34 H34B 109 . . ? H34A C34 H34B 106.7 . . ? C37 C36 Al1 114.4(6) . . ? C37 C36 H36A 108.7 . . ? Al1 C36 H36A 108.7 . . ? C37 C36 H36B 108.7 . . ? Al1 C36 H36B 108.7 . . ? H36A C36 H36B 107.6 . . ? C43 C42 Al2 114.2(7) . . ? C43 C42 H42A 108.7 . . ? Al2 C42 H42A 108.7 . . ? C43 C42 H42B 108.7 . . ? Al2 C42 H42B 108.7 . . ? H42A C42 H42B 107.6 . . ? C34A Al1A C32A 103.4(8) . . ? C34A Al1A C36A 116.4(7) . . ? C32A Al1A C36A 108.1(6) . . ? C34A Al1A C30A 113.5(7) . . ? C32A Al1A C30A 106.9(6) . . ? C36A Al1A C30A 107.9(5) . . ? C31A C30A Al1A 111.7(9) . . ? C31A C30A Ca 155.9(10) . . ? Al1A C30A Ca 75.8(4) . . ? C31A C30A H30C 109.3 . . ? Al1A C30A H30C 109.3 . . ? Ca C30A H30C 88.3 . . ? C31A C30A H30D 109.3 . . ? Al1A C30A H30D 109.3 . . ? Ca C30A H30D 47.9 . . ? H30C C30A H30D 107.9 . . ? C30A C31A H31D 109.5 . . ? C30A C31A H31E 109.5 . . ? H31D C31A H31E 109.5 . . ? C30A C31A H31F 109.5 . . ? H31D C31A H31F 109.5 . . ? H31E C31A H31F 109.5 . . ? C33A C32A Al1A 115.5(10) . . ? C33A C32A Ca 154.8(12) . . ? Al1A C32A Ca 77.0(5) . . ? C33A C32A H32C 108.4 . . ? Al1A C32A H32C 108.4 . . ? Ca C32A H32C 46.6 . . ? C33A C32A H32D 108.4 . . ? Al1A C32A H32D 108.4 . . ? Ca C32A H32D 86.2 . . ? H32C C32A H32D 107.5 . . ? C32A C33A H33D 109.5 . . ? C32A C33A H33E 109.5 . . ? H33D C33A H33E 109.5 . . ? C32A C33A H33F 109.5 . . ? H33D C33A H33F 109.5 . . ? H33E C33A H33F 109.5 . . ? C35A C34A Al1A 124.8(16) . . ? C35A C34A H34C 106.1 . . ? Al1A C34A H34C 106.1 . . ? C35A C34A H34D 106.1 . . ? Al1A C34A H34D 106.1 . . ? H34C C34A H34D 106.3 . . ? C34A C35A H35D 109.5 . . ? C34A C35A H35E 109.5 . . ? H35D C35A H35E 109.5 . . ? C34A C35A H35F 109.5 . . ? H35D C35A H35F 109.5 . . ? H35E C35A H35F 109.5 . . ? C37A C36A Al1A 121.7(9) . . ? C37A C36A H36C 106.9 . . ? Al1A C36A H36C 106.9 . . ? C37A C36A H36D 106.9 . . ? Al1A C36A H36D 106.9 . . ? H36C C36A H36D 106.7 . . ? C36A C37A H37D 109.5 . . ? C36A C37A H37E 109.5 . . ? H37D C37A H37E 109.5 . . ? C36A C37A H37F 109.5 . . ? H37D C37A H37F 109.5 . . ? H37E C37A H37F 109.5 . . ? C43A C42A Al2 111.8(8) . . ? C43A C42A H42C 109.3 . . ? Al2 C42A H42C 109.3 . . ? C43A C42A H42D 109.3 . . ? Al2 C42A H42D 109.3 . . ? H42C C42A H42D 107.9 . . ? C42A C43A H43D 109.5 . . ? C42A C43A H43E 109.5 . . ? H43D C43A H43E 109.5 . . ? C42A C43A H43F 109.5 . . ? H43D C43A H43F 109.5 . . ? H43E C43A H43F 109.5 . . ? #===END