# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- JulienJC.cif' #============================================================================== _audit_creation_date 29-05-12 _audit_creation_method SHELXL-97 # 1. Submission Details _publ_contact_author_name 'Jun Okuda' _publ_contact_author_address ; Institute of Inorganic Chemistry RWTH Aachen University Landoltweg 1 D-52056 Aachen Germany ; _publ_contact_author_phone 0049-241-8094645 _publ_contact_author_fax 0049-241-8092644 _publ_contact_author_email jun.okuda@ac.rwth-aachen.de _publ_requested_coeditor_name ? _publ_contact_letter ; This CIF file is part of a manuscript that is submitted for publication in the journal 'Dalton Transactions'. ; # 3. TITLE AND AUTHOR LIST _publ_section_title ; ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_address ; Institute of Inorganic Chemistry RWTH Aachen University Landoltweg 1 D-52056 Aachen Germany ; ; Institute of Inorganic Chemistry RWTH Aachen University Landoltweg 1 D-52056 Aachen Germany ; Thomas ; Institute of Inorganic Chemistry RWTH Aachen University Landoltweg 1 D-52056 Aachen Germany ; ; Institute of Inorganic Chemistry RWTH Aachen University Landoltweg 1 D-52056 Aachen Germany ; #=============================================== _publ_section_abstract ; ; _publ_section_references ; Altomare, A., Cascarano, G.; Giacovazzo, C.; Guagliardi, A. (1993) J. Appl. Crystallogr. 27, 443-350. Brandenburg K. (2004), Diamond, Crystal Impact GbR, Bonn Germany. Bruker (1999). SAINT+. Version 6.02. Program for Reduction of Data Collected on Bruker CCD Area Detector Diffractometer, Bruker AXS Inc., Madison, Wisconson, USA. Bruker (2001). SMART. Version 5.624. Program for Bruker CCD X-ray Diffractometer Control. Bruker AXS Inc., Madison, Wisconson, USA. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837. Sheldrick, G. M. (1996). SADABS. Program for Empirical Absorption Correction of Area Detector Data, University of G\"ottingen, Germany. Sheldrick, G. M. (2008). Acta Crystallogr. Sect. A, 64, 112-122. Spek, A. L. (2009). Acta Crystallogr, Sect. D 65, 148-155. ; _publ_author_name J.Okuda #===================================================== data_(S,S)8 _database_code_depnum_ccdc_archive 'CCDC 884447' #TrackingRef '- JulienJC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_absolute_configuration ad _chemical_formula_moiety 'C24 H60 Ca N2 O4 Si4' _chemical_formula_sum 'C24 H60 Ca N2 O4 Si4' _chemical_formula_weight 593.18 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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 11.5590(13) _cell_length_b 11.5507(13) _cell_length_c 26.697(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3564.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 5189 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 24.78 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 0.338 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9293 _exptl_absorpt_correction_T_max 0.9479 _exptl_absorpt_process_details 'Platon Mulabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'INCOATEC microsource' _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'APEX Area Detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50821 _diffrn_reflns_av_R_equivalents 0.0669 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 0.76 _diffrn_reflns_theta_max 28.83 _reflns_number_total 9351 _reflns_number_gt 8740 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (2001)' _computing_cell_refinement 'Bruker SMART (2001)' _computing_data_reduction 'Bruker SAINT+ (1999)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1999)' _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. The crystal was twinned by lattice merohedry emulating the space group P 43212 (No 96); the twinning matrix 0 1 0 1 0 0 0 0 -1 was used and the refinement resulted in a twin fraction of 0.49. ; _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^)+(0.0260P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack 0.03(3) _refine_ls_abs_structure_details 'Flack H D (1983), 4148 Friedel pairs' _refine_ls_number_reflns 9351 _refine_ls_number_parameters 350 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0648 _refine_ls_wR_factor_gt 0.0635 _refine_ls_goodness_of_fit_ref 0.917 _refine_ls_restrained_S_all 0.917 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.69244(4) 0.05555(4) 0.62437(2) 0.01832(8) Uani 1 1 d . . . Si1 Si 0.90154(7) 0.26774(6) 0.66355(3) 0.02294(15) Uani 1 1 d . A . Si2 Si 0.68380(7) 0.35817(7) 0.62170(3) 0.02744(17) Uani 1 1 d . A . Si3 Si 0.49379(7) -0.15025(7) 0.57728(3) 0.02554(16) Uani 1 1 d . A . Si4 Si 0.38713(6) 0.03548(7) 0.63613(3) 0.02734(17) Uani 1 1 d . A . O1 O 0.71863(18) 0.09668(19) 0.53609(7) 0.0313(5) Uani 1 1 d . A . O2 O 0.87805(16) -0.02701(16) 0.58844(6) 0.0238(4) Uani 1 1 d . A . O3 O 0.75499(19) -0.13773(18) 0.65752(7) 0.0379(5) Uani 1 1 d . A . O4 O 0.6800(2) 0.0377(2) 0.71656(6) 0.0392(5) Uani 1 1 d . A . N1 N 0.7684(2) 0.24536(18) 0.63876(8) 0.0217(5) Uani 1 1 d . A . N2 N 0.50610(19) -0.0252(2) 0.61012(8) 0.0219(5) Uani 1 1 d . A . C1 C 0.6485(3) 0.1039(3) 0.49221(11) 0.0519(10) Uani 1 1 d . . . H1A H 0.6521 0.1827 0.4787 0.078 Uiso 1 1 calc R A . H1B H 0.5683 0.0850 0.5008 0.078 Uiso 1 1 calc R . . H1C H 0.6770 0.0491 0.4671 0.078 Uiso 1 1 calc R . . C2 C 0.8385(3) 0.1162(3) 0.52698(10) 0.0324(7) Uani 1 1 d . A . H2A H 0.8672 0.1792 0.5488 0.039 Uiso 1 1 calc R . . H2B H 0.8505 0.1394 0.4917 0.039 Uiso 1 1 calc R . . C3 C 0.9037(2) 0.0059(3) 0.53776(9) 0.0282(6) Uani 1 1 d . . . H3A H 0.8793 -0.0558 0.5143 0.034 Uiso 1 1 calc R A . H3B H 0.9879 0.0186 0.5337 0.034 Uiso 1 1 calc R . . C4 C 0.9101(2) -0.1440(2) 0.60072(10) 0.0235(6) Uani 1 1 d . . . H4 H 0.8648 -0.1977 0.5788 0.028 Uiso 1 1 calc R A . C5 C 0.8761(3) -0.1659(2) 0.65432(10) 0.0273(6) Uani 1 1 d . A . H5 H 0.9204 -0.1120 0.6764 0.033 Uiso 1 1 calc R . . C6 C 0.9027(3) -0.2897(3) 0.66977(11) 0.0329(6) Uani 1 1 d . . . H6A H 0.8545 -0.3438 0.6499 0.040 Uiso 1 1 calc R A . H6B H 0.8834 -0.3005 0.7056 0.040 Uiso 1 1 calc R . . C7 C 1.0299(3) -0.3171(3) 0.66139(12) 0.0440(8) Uani 1 1 d . A . H7A H 1.0443 -0.3996 0.6692 0.053 Uiso 1 1 calc R . . H7B H 1.0775 -0.2696 0.6844 0.053 Uiso 1 1 calc R . . C8 C 1.0659(3) -0.2928(3) 0.60763(12) 0.0446(8) Uani 1 1 d . . . H8A H 1.0248 -0.3465 0.5849 0.053 Uiso 1 1 calc R A . H8B H 1.1500 -0.3067 0.6040 0.053 Uiso 1 1 calc R . . C9 C 1.0383(2) -0.1682(3) 0.59287(11) 0.0332(7) Uani 1 1 d . A . H9A H 1.0849 -0.1142 0.6135 0.040 Uiso 1 1 calc R . . H9B H 1.0587 -0.1556 0.5573 0.040 Uiso 1 1 calc R . . C10A C 0.6819(5) -0.1647(4) 0.69971(17) 0.0263(12) Uani 0.644(9) 1 d P A 1 H10A H 0.6992 -0.2434 0.7123 0.032 Uiso 0.644(9) 1 calc PR A 1 H10B H 0.5995 -0.1618 0.6897 0.032 Uiso 0.644(9) 1 calc PR A 1 C11A C 0.7058(5) -0.0765(4) 0.73958(16) 0.0277(13) Uani 0.644(9) 1 d P A 1 H11A H 0.6557 -0.0899 0.7691 0.033 Uiso 0.644(9) 1 calc PR A 1 H11B H 0.7877 -0.0803 0.7503 0.033 Uiso 0.644(9) 1 calc PR A 1 C10B C 0.7401(9) -0.1414(8) 0.7162(3) 0.028(2) Uani 0.356(9) 1 d P A 2 H10C H 0.7320 -0.2221 0.7283 0.034 Uiso 0.356(9) 1 calc PR A 2 H10D H 0.8070 -0.1050 0.7332 0.034 Uiso 0.356(9) 1 calc PR A 2 C11B C 0.6379(8) -0.0778(8) 0.7248(3) 0.028(2) Uani 0.356(9) 1 d P A 2 H11C H 0.6090 -0.0883 0.7594 0.033 Uiso 0.356(9) 1 calc PR A 2 H11D H 0.5763 -0.0987 0.7007 0.033 Uiso 0.356(9) 1 calc PR A 2 C12 C 0.6844(3) 0.1231(3) 0.75455(10) 0.0386(7) Uani 1 1 d . . . H12A H 0.6149 0.1176 0.7754 0.058 Uiso 1 1 calc R A . H12B H 0.6882 0.2000 0.7392 0.058 Uiso 1 1 calc R . . H12C H 0.7531 0.1107 0.7754 0.058 Uiso 1 1 calc R . . C13 C 0.9667(2) 0.1325(2) 0.69066(10) 0.0309(6) Uani 1 1 d . . . H13A H 0.9114 0.0964 0.7137 0.046 Uiso 1 1 calc R A . H13B H 1.0376 0.1523 0.7089 0.046 Uiso 1 1 calc R . . H13C H 0.9852 0.0784 0.6636 0.046 Uiso 1 1 calc R . . C14 C 1.0150(2) 0.3172(3) 0.61728(11) 0.0425(8) Uani 1 1 d . . . H14A H 1.0251 0.2581 0.5913 0.064 Uiso 1 1 calc R A . H14B H 1.0886 0.3293 0.6348 0.064 Uiso 1 1 calc R . . H14C H 0.9902 0.3900 0.6017 0.064 Uiso 1 1 calc R . . C15 C 0.9083(3) 0.3796(2) 0.71472(11) 0.0310(7) Uani 1 1 d . . . H15A H 0.8791 0.4536 0.7020 0.047 Uiso 1 1 calc R A . H15B H 0.9887 0.3890 0.7257 0.047 Uiso 1 1 calc R . . H15C H 0.8607 0.3543 0.7431 0.047 Uiso 1 1 calc R . . C16 C 0.5579(3) 0.3119(3) 0.58194(12) 0.0442(8) Uani 1 1 d . . . H16A H 0.5819 0.3085 0.5468 0.066 Uiso 1 1 calc R A . H16B H 0.4947 0.3678 0.5856 0.066 Uiso 1 1 calc R . . H16C H 0.5314 0.2352 0.5927 0.066 Uiso 1 1 calc R . . C17 C 0.7573(3) 0.4689(3) 0.58129(11) 0.0471(8) Uani 1 1 d . . . H17A H 0.8260 0.4984 0.5986 0.071 Uiso 1 1 calc R A . H17B H 0.7039 0.5329 0.5746 0.071 Uiso 1 1 calc R . . H17C H 0.7805 0.4331 0.5495 0.071 Uiso 1 1 calc R . . C18 C 0.6199(3) 0.4392(2) 0.67661(11) 0.0396(7) Uani 1 1 d . . . H18A H 0.5799 0.3846 0.6987 0.059 Uiso 1 1 calc R A . H18B H 0.5647 0.4971 0.6644 0.059 Uiso 1 1 calc R . . H18C H 0.6819 0.4780 0.6952 0.059 Uiso 1 1 calc R . . C19 C 0.4766(4) -0.2844(3) 0.61619(13) 0.0640(11) Uani 1 1 d . . . H19A H 0.5465 -0.2963 0.6364 0.096 Uiso 1 1 calc R A . H19B H 0.4648 -0.3512 0.5942 0.096 Uiso 1 1 calc R . . H19C H 0.4096 -0.2756 0.6384 0.096 Uiso 1 1 calc R . . C20 C 0.6252(3) -0.1824(3) 0.53833(12) 0.0479(9) Uani 1 1 d . . . H20A H 0.6265 -0.1310 0.5091 0.072 Uiso 1 1 calc R A . H20B H 0.6226 -0.2631 0.5271 0.072 Uiso 1 1 calc R . . H20C H 0.6950 -0.1699 0.5584 0.072 Uiso 1 1 calc R . . C21 C 0.3709(3) -0.1547(3) 0.53162(11) 0.0402(8) Uani 1 1 d . . . H21A H 0.2974 -0.1552 0.5499 0.060 Uiso 1 1 calc R A . H21B H 0.3768 -0.2249 0.5112 0.060 Uiso 1 1 calc R . . H21C H 0.3742 -0.0865 0.5099 0.060 Uiso 1 1 calc R . . C22 C 0.2883(2) 0.1083(3) 0.58937(12) 0.0447(8) Uani 1 1 d . . . H22A H 0.3318 0.1670 0.5707 0.067 Uiso 1 1 calc R A . H22B H 0.2240 0.1454 0.6071 0.067 Uiso 1 1 calc R . . H22C H 0.2578 0.0504 0.5660 0.067 Uiso 1 1 calc R . . C23 C 0.4224(3) 0.1491(3) 0.68475(11) 0.0487(9) Uani 1 1 d . . . H23A H 0.4430 0.1111 0.7163 0.073 Uiso 1 1 calc R A . H23B H 0.3548 0.1988 0.6900 0.073 Uiso 1 1 calc R . . H23C H 0.4876 0.1961 0.6731 0.073 Uiso 1 1 calc R . . C24 C 0.2945(2) -0.0698(3) 0.67193(11) 0.0432(8) Uani 1 1 d . . . H24A H 0.2697 -0.1323 0.6496 0.065 Uiso 1 1 calc R A . H24B H 0.2264 -0.0295 0.6851 0.065 Uiso 1 1 calc R . . H24C H 0.3393 -0.1024 0.6997 0.065 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 0.0178(3) 0.0208(3) 0.01638(17) 0.0003(2) 0.0000(2) 0.00112(16) Si1 0.0219(4) 0.0231(4) 0.0238(3) -0.0009(3) 0.0027(3) -0.0019(3) Si2 0.0332(4) 0.0229(4) 0.0262(4) 0.0020(3) -0.0035(3) 0.0037(3) Si3 0.0232(4) 0.0236(4) 0.0299(4) -0.0009(3) -0.0017(3) 0.0008(3) Si4 0.0179(4) 0.0368(4) 0.0274(4) -0.0060(3) 0.0004(3) 0.0025(3) O1 0.0290(11) 0.0468(12) 0.0181(9) 0.0055(8) -0.0018(8) 0.0046(9) O2 0.0256(9) 0.0274(10) 0.0183(8) 0.0048(7) 0.0030(7) 0.0028(8) O3 0.0478(13) 0.0299(12) 0.0361(11) 0.0130(10) 0.0214(10) 0.0137(10) O4 0.0659(15) 0.0303(11) 0.0213(9) -0.0034(9) 0.0118(10) -0.0095(12) N1 0.0247(12) 0.0188(12) 0.0215(11) -0.0002(9) -0.0021(9) 0.0003(9) N2 0.0195(11) 0.0244(12) 0.0218(10) -0.0009(9) 0.0012(9) -0.0004(9) C1 0.051(2) 0.074(3) 0.0313(16) 0.0057(16) -0.0157(15) 0.0060(18) C2 0.0351(17) 0.0388(19) 0.0234(14) 0.0094(13) 0.0056(12) -0.0022(13) C3 0.0266(15) 0.0368(17) 0.0213(12) 0.0022(11) 0.0075(11) 0.0023(13) C4 0.0216(13) 0.0214(13) 0.0274(12) -0.0039(11) -0.0028(10) 0.0034(11) C5 0.0426(17) 0.0183(13) 0.0210(12) -0.0005(10) -0.0053(12) 0.0029(12) C6 0.0402(17) 0.0228(14) 0.0358(14) 0.0026(12) -0.0102(13) 0.0049(13) C7 0.0402(18) 0.0264(16) 0.065(2) 0.0089(15) -0.0219(16) 0.0047(13) C8 0.0280(16) 0.0311(17) 0.075(2) -0.0092(16) -0.0072(15) 0.0073(13) C9 0.0180(13) 0.0362(17) 0.0454(17) 0.0002(14) -0.0015(12) 0.0039(11) C10A 0.026(3) 0.028(2) 0.025(2) 0.0084(18) 0.007(2) -0.002(2) C11A 0.027(3) 0.039(3) 0.017(2) 0.0084(19) 0.0042(19) 0.0045(19) C10B 0.029(5) 0.028(5) 0.027(5) 0.014(4) 0.001(4) -0.006(4) C11B 0.019(5) 0.044(5) 0.020(4) 0.010(3) -0.004(3) -0.002(4) C12 0.0443(17) 0.049(2) 0.0228(14) -0.0093(13) -0.0013(14) 0.0016(16) C13 0.0274(14) 0.0301(15) 0.0353(15) -0.0047(12) -0.0074(11) 0.0014(12) C14 0.0310(16) 0.052(2) 0.0449(17) 0.0022(14) 0.0149(14) -0.0082(14) C15 0.0332(16) 0.0251(15) 0.0347(16) 0.0004(12) -0.0026(13) -0.0027(13) C16 0.0440(19) 0.0382(19) 0.0504(19) 0.0036(15) -0.0185(15) 0.0087(14) C17 0.067(2) 0.0322(17) 0.0418(17) 0.0137(15) 0.0020(16) -0.0016(17) C18 0.0443(18) 0.0330(17) 0.0416(16) -0.0022(13) -0.0021(14) 0.0148(14) C19 0.089(3) 0.038(2) 0.065(2) 0.0133(18) 0.009(2) -0.0001(19) C20 0.0307(16) 0.050(2) 0.063(2) -0.0296(16) 0.0051(16) 0.0018(14) C21 0.0316(17) 0.0445(19) 0.0444(18) -0.0188(16) -0.0098(14) 0.0020(16) C22 0.0319(18) 0.046(2) 0.056(2) 0.0001(16) -0.0068(15) 0.0148(14) C23 0.0418(18) 0.062(2) 0.0427(18) -0.0224(17) 0.0061(15) 0.0014(17) C24 0.0272(16) 0.067(2) 0.0357(15) 0.0025(15) 0.0068(13) -0.0083(14) _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 N2 2.378(2) . ? Ca1 N1 2.393(2) . ? Ca1 O1 2.4234(19) . ? Ca1 O4 2.4738(18) . ? Ca1 O3 2.508(2) . ? Ca1 O2 2.5362(19) . ? Ca1 C11B 3.155(8) . ? Ca1 C2 3.178(3) . ? Ca1 Si2 3.4976(10) . ? Ca1 Si3 3.5361(10) . ? Ca1 Si4 3.5506(10) . ? Ca1 Si1 3.5976(10) . ? Si1 N1 1.695(2) . ? Si1 C13 1.879(3) . ? Si1 C15 1.882(3) . ? Si1 C14 1.890(3) . ? Si2 N1 1.692(2) . ? Si2 C17 1.876(3) . ? Si2 C16 1.879(3) . ? Si2 C18 1.890(3) . ? Si3 N2 1.696(2) . ? Si3 C21 1.872(3) . ? Si3 C19 1.876(3) . ? Si3 C20 1.878(3) . ? Si4 N2 1.692(2) . ? Si4 C24 1.881(3) . ? Si4 C23 1.890(3) . ? Si4 C22 1.890(3) . ? O1 C2 1.425(3) . ? O1 C1 1.427(3) . ? O2 C3 1.436(3) . ? O2 C4 1.439(3) . ? O3 C5 1.440(4) . ? O3 C10A 1.442(4) . ? O3 C10B 1.577(9) . ? O4 C12 1.416(3) . ? O4 C11B 1.437(9) . ? O4 C11A 1.485(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.507(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.505(3) . ? C4 C9 1.523(4) . ? C4 H4 1.0000 . ? C5 C6 1.520(4) . ? C5 H5 1.0000 . ? C6 C7 1.520(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.521(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.526(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10A C11A 1.499(8) . ? C10A H10A 0.9900 . ? C10A H10B 0.9900 . ? C11A H11A 0.9900 . ? C11A H11B 0.9900 . ? C10B C11B 1.410(15) . ? C10B H10C 0.9900 . ? C10B H10D 0.9900 . ? C11B H11C 0.9900 . ? C11B H11D 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ca1 N1 135.84(6) . . ? N2 Ca1 O1 91.97(7) . . ? N1 Ca1 O1 86.02(7) . . ? N2 Ca1 O4 94.24(8) . . ? N1 Ca1 O4 86.44(8) . . ? O1 Ca1 O4 172.38(9) . . ? N2 Ca1 O3 88.20(8) . . ? N1 Ca1 O3 130.79(8) . . ? O1 Ca1 O3 118.80(7) . . ? O4 Ca1 O3 65.90(7) . . ? N2 Ca1 O2 123.94(7) . . ? N1 Ca1 O2 95.44(7) . . ? O1 Ca1 O2 66.43(6) . . ? O4 Ca1 O2 113.21(7) . . ? O3 Ca1 O2 63.57(5) . . ? N2 Ca1 C11B 76.33(19) . . ? N1 Ca1 C11B 112.59(18) . . ? O1 Ca1 C11B 161.27(18) . . ? O4 Ca1 C11B 26.17(18) . . ? O3 Ca1 C11B 47.41(18) . . ? O2 Ca1 C11B 107.87(18) . . ? N2 Ca1 C2 115.89(8) . . ? N1 Ca1 C2 74.60(8) . . ? O1 Ca1 C2 25.15(7) . . ? O4 Ca1 C2 149.67(8) . . ? O3 Ca1 C2 109.37(7) . . ? O2 Ca1 C2 47.47(7) . . ? C11B Ca1 C2 155.33(16) . . ? N2 Ca1 Si2 111.27(6) . . ? N1 Ca1 Si2 25.58(6) . . ? O1 Ca1 Si2 77.74(6) . . ? O4 Ca1 Si2 95.85(6) . . ? O3 Ca1 Si2 154.83(6) . . ? O2 Ca1 Si2 113.09(5) . . ? C11B Ca1 Si2 119.96(17) . . ? C2 Ca1 Si2 77.19(6) . . ? N2 Ca1 Si3 24.66(5) . . ? N1 Ca1 Si3 155.68(6) . . ? O1 Ca1 Si3 82.36(5) . . ? O4 Ca1 Si3 105.07(6) . . ? O3 Ca1 Si3 73.40(6) . . ? O2 Ca1 Si3 99.33(5) . . ? C11B Ca1 Si3 81.04(18) . . ? C2 Ca1 Si3 101.66(6) . . ? Si2 Ca1 Si3 130.24(2) . . ? N2 Ca1 Si4 24.24(5) . . ? N1 Ca1 Si4 114.23(6) . . ? O1 Ca1 Si4 102.88(5) . . ? O4 Ca1 Si4 81.31(6) . . ? O3 Ca1 Si4 101.37(5) . . ? O2 Ca1 Si4 148.18(5) . . ? C11B Ca1 Si4 72.21(18) . . ? C2 Ca1 Si4 127.93(6) . . ? Si2 Ca1 Si4 92.22(2) . . ? Si3 Ca1 Si4 48.86(2) . . ? N2 Ca1 Si1 157.26(6) . . ? N1 Ca1 Si1 23.45(5) . . ? O1 Ca1 Si1 93.74(5) . . ? O4 Ca1 Si1 78.85(6) . . ? O3 Ca1 Si1 108.07(6) . . ? O2 Ca1 Si1 78.33(5) . . ? C11B Ca1 Si1 102.69(18) . . ? C2 Ca1 Si1 74.39(6) . . ? Si2 Ca1 Si1 49.02(2) . . ? Si3 Ca1 Si1 176.03(2) . . ? Si4 Ca1 Si1 133.36(2) . . ? N1 Si1 C13 112.82(12) . . ? N1 Si1 C15 115.22(12) . . ? C13 Si1 C15 105.90(12) . . ? N1 Si1 C14 114.90(13) . . ? C13 Si1 C14 102.99(13) . . ? C15 Si1 C14 103.76(14) . . ? C13 Si1 Ca1 79.35(9) . . ? C15 Si1 Ca1 134.97(10) . . ? C14 Si1 Ca1 118.83(10) . . ? N1 Si2 C17 114.70(14) . . ? N1 Si2 C16 112.38(13) . . ? C17 Si2 C16 102.71(15) . . ? N1 Si2 C18 113.49(12) . . ? C17 Si2 C18 106.59(15) . . ? C16 Si2 C18 106.03(15) . . ? C17 Si2 Ca1 132.83(11) . . ? C16 Si2 Ca1 75.48(10) . . ? C18 Si2 Ca1 119.36(10) . . ? N2 Si3 C21 115.08(13) . . ? N2 Si3 C19 115.22(14) . . ? C21 Si3 C19 104.92(17) . . ? N2 Si3 C20 112.77(13) . . ? C21 Si3 C20 104.33(14) . . ? C19 Si3 C20 103.23(16) . . ? C21 Si3 Ca1 137.96(11) . . ? C19 Si3 Ca1 115.27(13) . . ? C20 Si3 Ca1 78.74(10) . . ? N2 Si4 C24 113.78(14) . . ? N2 Si4 C23 113.20(13) . . ? C24 Si4 C23 102.85(14) . . ? N2 Si4 C22 113.87(13) . . ? C24 Si4 C22 106.22(14) . . ? C23 Si4 C22 105.96(15) . . ? C24 Si4 Ca1 130.75(10) . . ? C23 Si4 Ca1 78.52(10) . . ? C22 Si4 Ca1 120.90(10) . . ? C2 O1 C1 113.8(2) . . ? C2 O1 Ca1 108.56(15) . . ? C1 O1 Ca1 137.65(18) . . ? C3 O2 C4 114.2(2) . . ? C3 O2 Ca1 115.55(15) . . ? C4 O2 Ca1 118.99(14) . . ? C5 O3 C10A 124.5(3) . . ? C5 O3 C10B 99.1(4) . . ? C5 O3 Ca1 117.44(16) . . ? C10A O3 Ca1 107.4(2) . . ? C10B O3 Ca1 110.1(4) . . ? C12 O4 C11B 123.3(4) . . ? C12 O4 C11A 108.4(3) . . ? C12 O4 Ca1 130.75(18) . . ? C11B O4 Ca1 104.4(4) . . ? C11A O4 Ca1 118.3(2) . . ? Si2 N1 Si1 120.83(14) . . ? Si2 N1 Ca1 116.78(12) . . ? Si1 N1 Ca1 122.38(11) . . ? Si4 N2 Si3 119.78(14) . . ? Si4 N2 Ca1 120.53(12) . . ? Si3 N2 Ca1 119.53(11) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 108.7(2) . . ? O1 C2 Ca1 46.29(11) . . ? C3 C2 Ca1 85.60(16) . . ? O1 C2 H2A 110.0 . . ? C3 C2 H2A 110.0 . . ? Ca1 C2 H2A 81.8 . . ? O1 C2 H2B 110.0 . . ? C3 C2 H2B 110.0 . . ? Ca1 C2 H2B 155.9 . . ? H2A C2 H2B 108.3 . . ? O2 C3 C2 107.5(2) . . ? O2 C3 H3A 110.2 . . ? C2 C3 H3A 110.2 . . ? O2 C3 H3B 110.2 . . ? C2 C3 H3B 110.2 . . ? H3A C3 H3B 108.5 . . ? O2 C4 C5 107.9(2) . . ? O2 C4 C9 113.1(2) . . ? C5 C4 C9 110.7(2) . . ? O2 C4 H4 108.3 . . ? C5 C4 H4 108.3 . . ? C9 C4 H4 108.3 . . ? O3 C5 C4 105.8(2) . . ? O3 C5 C6 113.2(2) . . ? C4 C5 C6 111.3(3) . . ? O3 C5 H5 108.8 . . ? C4 C5 H5 108.8 . . ? C6 C5 H5 108.8 . . ? C5 C6 C7 110.6(3) . . ? C5 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C6 C7 C8 111.4(3) . . ? C6 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? C6 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? C7 C8 C9 111.1(3) . . ? C7 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? C7 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C4 C9 C8 109.9(2) . . ? C4 C9 H9A 109.7 . . ? C8 C9 H9A 109.7 . . ? C4 C9 H9B 109.7 . . ? C8 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? O3 C10A C11A 107.5(4) . . ? O3 C10A H10A 110.2 . . ? C11A C10A H10A 110.2 . . ? O3 C10A H10B 110.2 . . ? C11A C10A H10B 110.2 . . ? H10A C10A H10B 108.5 . . ? O4 C11A C10A 105.8(4) . . ? O4 C11A H11A 110.6 . . ? C10A C11A H11A 110.6 . . ? O4 C11A H11B 110.6 . . ? C10A C11A H11B 110.6 . . ? H11A C11A H11B 108.7 . . ? C11B C10B O3 103.8(7) . . ? C11B C10B H10C 111.0 . . ? O3 C10B H10C 111.0 . . ? C11B C10B H10D 111.0 . . ? O3 C10B H10D 111.0 . . ? H10C C10B H10D 109.0 . . ? C10B C11B O4 100.1(7) . . ? C10B C11B Ca1 87.1(5) . . ? O4 C11B Ca1 49.4(3) . . ? C10B C11B H11C 111.8 . . ? O4 C11B H11C 111.8 . . ? Ca1 C11B H11C 156.9 . . ? C10B C11B H11D 111.8 . . ? O4 C11B H11D 111.8 . . ? Ca1 C11B H11D 73.2 . . ? H11C C11B H11D 109.5 . . ? O4 C12 H12A 109.5 . . ? O4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si3 C19 H19A 109.5 . . ? Si3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si3 C20 H20A 109.5 . . ? Si3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si3 C21 H21A 109.5 . . ? Si3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si4 C22 H22A 109.5 . . ? Si4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si4 C23 H23A 109.5 . . ? Si4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si4 C24 H24A 109.5 . . ? Si4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 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 Ca1 Si1 N1 -33.18(15) . . . . ? O1 Ca1 Si1 N1 71.00(14) . . . . ? O4 Ca1 Si1 N1 -107.19(15) . . . . ? O3 Ca1 Si1 N1 -167.05(14) . . . . ? O2 Ca1 Si1 N1 136.00(14) . . . . ? C11B Ca1 Si1 N1 -118.1(2) . . . . ? C2 Ca1 Si1 N1 87.23(15) . . . . ? Si2 Ca1 Si1 N1 0.79(13) . . . . ? Si4 Ca1 Si1 N1 -40.65(14) . . . . ? N2 Ca1 Si1 C13 135.19(17) . . . . ? N1 Ca1 Si1 C13 168.37(17) . . . . ? O1 Ca1 Si1 C13 -120.63(10) . . . . ? O4 Ca1 Si1 C13 61.18(11) . . . . ? O3 Ca1 Si1 C13 1.32(10) . . . . ? O2 Ca1 Si1 C13 -55.63(10) . . . . ? C11B Ca1 Si1 C13 50.3(2) . . . . ? C2 Ca1 Si1 C13 -104.41(11) . . . . ? Si2 Ca1 Si1 C13 169.16(9) . . . . ? Si4 Ca1 Si1 C13 127.72(9) . . . . ? N2 Ca1 Si1 C15 33.3(2) . . . . ? N1 Ca1 Si1 C15 66.47(18) . . . . ? O1 Ca1 Si1 C15 137.47(14) . . . . ? O4 Ca1 Si1 C15 -40.73(14) . . . . ? O3 Ca1 Si1 C15 -100.58(14) . . . . ? O2 Ca1 Si1 C15 -157.53(14) . . . . ? C11B Ca1 Si1 C15 -51.6(2) . . . . ? C2 Ca1 Si1 C15 153.69(14) . . . . ? Si2 Ca1 Si1 C15 67.26(13) . . . . ? Si4 Ca1 Si1 C15 25.82(14) . . . . ? N2 Ca1 Si1 C14 -125.75(18) . . . . ? N1 Ca1 Si1 C14 -92.57(17) . . . . ? O1 Ca1 Si1 C14 -21.56(12) . . . . ? O4 Ca1 Si1 C14 160.24(13) . . . . ? O3 Ca1 Si1 C14 100.39(12) . . . . ? O2 Ca1 Si1 C14 43.44(12) . . . . ? C11B Ca1 Si1 C14 149.4(2) . . . . ? C2 Ca1 Si1 C14 -5.34(13) . . . . ? Si2 Ca1 Si1 C14 -91.77(11) . . . . ? Si4 Ca1 Si1 C14 -133.21(11) . . . . ? N2 Ca1 Si2 N1 165.87(15) . . . . ? O1 Ca1 Si2 N1 -106.82(13) . . . . ? O4 Ca1 Si2 N1 69.00(14) . . . . ? O3 Ca1 Si2 N1 27.36(16) . . . . ? O2 Ca1 Si2 N1 -49.32(13) . . . . ? C11B Ca1 Si2 N1 79.8(2) . . . . ? C2 Ca1 Si2 N1 -81.05(13) . . . . ? Si3 Ca1 Si2 N1 -175.59(13) . . . . ? Si4 Ca1 Si2 N1 150.48(12) . . . . ? Si1 Ca1 Si2 N1 -0.73(12) . . . . ? N2 Ca1 Si2 C17 -119.73(16) . . . . ? N1 Ca1 Si2 C17 74.41(19) . . . . ? O1 Ca1 Si2 C17 -32.41(16) . . . . ? O4 Ca1 Si2 C17 143.40(16) . . . . ? O3 Ca1 Si2 C17 101.77(19) . . . . ? O2 Ca1 Si2 C17 25.08(16) . . . . ? C11B Ca1 Si2 C17 154.2(3) . . . . ? C2 Ca1 Si2 C17 -6.65(16) . . . . ? Si3 Ca1 Si2 C17 -101.19(15) . . . . ? Si4 Ca1 Si2 C17 -135.11(15) . . . . ? Si1 Ca1 Si2 C17 73.68(15) . . . . ? N2 Ca1 Si2 C16 -25.71(12) . . . . ? N1 Ca1 Si2 C16 168.42(16) . . . . ? O1 Ca1 Si2 C16 61.60(12) . . . . ? O4 Ca1 Si2 C16 -122.58(12) . . . . ? O3 Ca1 Si2 C16 -164.22(15) . . . . ? O2 Ca1 Si2 C16 119.10(12) . . . . ? C11B Ca1 Si2 C16 -111.8(2) . . . . ? C2 Ca1 Si2 C16 87.36(12) . . . . ? Si3 Ca1 Si2 C16 -7.17(11) . . . . ? Si4 Ca1 Si2 C16 -41.10(11) . . . . ? Si1 Ca1 Si2 C16 167.69(11) . . . . ? N2 Ca1 Si2 C18 74.75(13) . . . . ? N1 Ca1 Si2 C18 -91.11(17) . . . . ? O1 Ca1 Si2 C18 162.07(13) . . . . ? O4 Ca1 Si2 C18 -22.12(13) . . . . ? O3 Ca1 Si2 C18 -63.75(16) . . . . ? O2 Ca1 Si2 C18 -140.44(12) . . . . ? C11B Ca1 Si2 C18 -11.3(2) . . . . ? C2 Ca1 Si2 C18 -172.17(13) . . . . ? Si3 Ca1 Si2 C18 93.29(12) . . . . ? Si4 Ca1 Si2 C18 59.37(12) . . . . ? Si1 Ca1 Si2 C18 -91.84(12) . . . . ? N1 Ca1 Si3 N2 -49.86(15) . . . . ? O1 Ca1 Si3 N2 -112.03(14) . . . . ? O4 Ca1 Si3 N2 66.23(15) . . . . ? O3 Ca1 Si3 N2 124.79(14) . . . . ? O2 Ca1 Si3 N2 -176.51(14) . . . . ? C11B Ca1 Si3 N2 76.7(2) . . . . ? C2 Ca1 Si3 N2 -128.24(14) . . . . ? Si2 Ca1 Si3 N2 -45.24(13) . . . . ? Si4 Ca1 Si3 N2 2.53(13) . . . . ? N2 Ca1 Si3 C21 62.90(19) . . . . ? N1 Ca1 Si3 C21 13.0(2) . . . . ? O1 Ca1 Si3 C21 -49.13(16) . . . . ? O4 Ca1 Si3 C21 129.14(16) . . . . ? O3 Ca1 Si3 C21 -172.30(16) . . . . ? O2 Ca1 Si3 C21 -113.61(15) . . . . ? C11B Ca1 Si3 C21 139.6(2) . . . . ? C2 Ca1 Si3 C21 -65.33(16) . . . . ? Si2 Ca1 Si3 C21 17.66(15) . . . . ? Si4 Ca1 Si3 C21 65.44(15) . . . . ? N2 Ca1 Si3 C19 -98.68(18) . . . . ? N1 Ca1 Si3 C19 -148.54(18) . . . . ? O1 Ca1 Si3 C19 149.29(15) . . . . ? O4 Ca1 Si3 C19 -32.45(15) . . . . ? O3 Ca1 Si3 C19 26.11(14) . . . . ? O2 Ca1 Si3 C19 84.81(14) . . . . ? C11B Ca1 Si3 C19 -22.0(2) . . . . ? C2 Ca1 Si3 C19 133.08(14) . . . . ? Si2 Ca1 Si3 C19 -143.92(14) . . . . ? Si4 Ca1 Si3 C19 -96.15(14) . . . . ? N2 Ca1 Si3 C20 161.88(17) . . . . ? N1 Ca1 Si3 C20 112.02(17) . . . . ? O1 Ca1 Si3 C20 49.85(12) . . . . ? O4 Ca1 Si3 C20 -131.88(12) . . . . ? O3 Ca1 Si3 C20 -73.32(11) . . . . ? O2 Ca1 Si3 C20 -14.63(11) . . . . ? C11B Ca1 Si3 C20 -121.4(2) . . . . ? C2 Ca1 Si3 C20 33.65(12) . . . . ? Si2 Ca1 Si3 C20 116.64(11) . . . . ? Si4 Ca1 Si3 C20 164.42(11) . . . . ? N1 Ca1 Si4 N2 156.46(16) . . . . ? O1 Ca1 Si4 N2 65.04(15) . . . . ? O4 Ca1 Si4 N2 -121.45(14) . . . . ? O3 Ca1 Si4 N2 -58.33(14) . . . . ? O2 Ca1 Si4 N2 -0.79(16) . . . . ? C11B Ca1 Si4 N2 -96.2(2) . . . . ? C2 Ca1 Si4 N2 67.52(15) . . . . ? Si2 Ca1 Si4 N2 142.97(14) . . . . ? Si3 Ca1 Si4 N2 -2.58(13) . . . . ? Si1 Ca1 Si4 N2 172.97(13) . . . . ? N2 Ca1 Si4 C24 72.70(18) . . . . ? N1 Ca1 Si4 C24 -130.84(14) . . . . ? O1 Ca1 Si4 C24 137.74(14) . . . . ? O4 Ca1 Si4 C24 -48.75(14) . . . . ? O3 Ca1 Si4 C24 14.37(14) . . . . ? O2 Ca1 Si4 C24 71.91(15) . . . . ? C11B Ca1 Si4 C24 -23.5(2) . . . . ? C2 Ca1 Si4 C24 140.22(15) . . . . ? Si2 Ca1 Si4 C24 -144.33(13) . . . . ? Si3 Ca1 Si4 C24 70.12(13) . . . . ? Si1 Ca1 Si4 C24 -114.32(13) . . . . ? N2 Ca1 Si4 C23 169.86(18) . . . . ? N1 Ca1 Si4 C23 -33.68(13) . . . . ? O1 Ca1 Si4 C23 -125.10(13) . . . . ? O4 Ca1 Si4 C23 48.41(13) . . . . ? O3 Ca1 Si4 C23 111.53(12) . . . . ? O2 Ca1 Si4 C23 169.07(14) . . . . ? C11B Ca1 Si4 C23 73.7(2) . . . . ? C2 Ca1 Si4 C23 -122.62(14) . . . . ? Si2 Ca1 Si4 C23 -47.17(12) . . . . ? Si3 Ca1 Si4 C23 167.28(12) . . . . ? Si1 Ca1 Si4 C23 -17.17(12) . . . . ? N2 Ca1 Si4 C22 -88.28(18) . . . . ? N1 Ca1 Si4 C22 68.18(13) . . . . ? O1 Ca1 Si4 C22 -23.24(14) . . . . ? O4 Ca1 Si4 C22 150.27(13) . . . . ? O3 Ca1 Si4 C22 -146.62(13) . . . . ? O2 Ca1 Si4 C22 -89.08(15) . . . . ? C11B Ca1 Si4 C22 175.5(2) . . . . ? C2 Ca1 Si4 C22 -20.77(15) . . . . ? Si2 Ca1 Si4 C22 54.69(13) . . . . ? Si3 Ca1 Si4 C22 -90.86(12) . . . . ? Si1 Ca1 Si4 C22 84.69(13) . . . . ? N2 Ca1 O1 C2 -162.74(18) . . . . ? N1 Ca1 O1 C2 61.44(18) . . . . ? O3 Ca1 O1 C2 -73.72(19) . . . . ? O2 Ca1 O1 C2 -36.27(17) . . . . ? C11B Ca1 O1 C2 -112.2(5) . . . . ? Si2 Ca1 O1 C2 85.92(18) . . . . ? Si3 Ca1 O1 C2 -139.97(18) . . . . ? Si4 Ca1 O1 C2 175.40(17) . . . . ? Si1 Ca1 O1 C2 39.28(18) . . . . ? N2 Ca1 O1 C1 15.7(3) . . . . ? N1 Ca1 O1 C1 -120.2(3) . . . . ? O3 Ca1 O1 C1 104.7(3) . . . . ? O2 Ca1 O1 C1 142.1(3) . . . . ? C11B Ca1 O1 C1 66.2(7) . . . . ? C2 Ca1 O1 C1 178.4(4) . . . . ? Si2 Ca1 O1 C1 -95.7(3) . . . . ? Si3 Ca1 O1 C1 38.4(3) . . . . ? Si4 Ca1 O1 C1 -6.2(3) . . . . ? Si1 Ca1 O1 C1 -142.3(3) . . . . ? N2 Ca1 O2 C3 82.26(19) . . . . ? N1 Ca1 O2 C3 -76.60(18) . . . . ? O1 Ca1 O2 C3 6.64(17) . . . . ? O4 Ca1 O2 C3 -165.06(17) . . . . ? O3 Ca1 O2 C3 150.13(18) . . . . ? C11B Ca1 O2 C3 167.5(2) . . . . ? C2 Ca1 O2 C3 -13.30(17) . . . . ? Si2 Ca1 O2 C3 -57.40(18) . . . . ? Si3 Ca1 O2 C3 84.02(17) . . . . ? Si4 Ca1 O2 C3 82.66(19) . . . . ? Si1 Ca1 O2 C3 -92.72(17) . . . . ? N2 Ca1 O2 C4 -59.42(18) . . . . ? N1 Ca1 O2 C4 141.71(16) . . . . ? O1 Ca1 O2 C4 -135.04(18) . . . . ? O4 Ca1 O2 C4 53.26(18) . . . . ? O3 Ca1 O2 C4 8.44(16) . . . . ? C11B Ca1 O2 C4 25.9(2) . . . . ? C2 Ca1 O2 C4 -155.0(2) . . . . ? Si2 Ca1 O2 C4 160.91(15) . . . . ? Si3 Ca1 O2 C4 -57.67(16) . . . . ? Si4 Ca1 O2 C4 -59.03(19) . . . . ? Si1 Ca1 O2 C4 125.59(16) . . . . ? N2 Ca1 O3 C5 153.95(18) . . . . ? N1 Ca1 O3 C5 -49.0(2) . . . . ? O1 Ca1 O3 C5 62.7(2) . . . . ? O4 Ca1 O3 C5 -110.6(2) . . . . ? O2 Ca1 O3 C5 24.20(18) . . . . ? C11B Ca1 O3 C5 -133.0(3) . . . . ? C2 Ca1 O3 C5 37.1(2) . . . . ? Si2 Ca1 O3 C5 -64.2(2) . . . . ? Si3 Ca1 O3 C5 133.90(19) . . . . ? Si4 Ca1 O3 C5 174.41(17) . . . . ? Si1 Ca1 O3 C5 -42.24(19) . . . . ? N2 Ca1 O3 C10A -59.7(3) . . . . ? N1 Ca1 O3 C10A 97.3(3) . . . . ? O1 Ca1 O3 C10A -151.0(3) . . . . ? O4 Ca1 O3 C10A 35.7(3) . . . . ? O2 Ca1 O3 C10A 170.5(3) . . . . ? C11B Ca1 O3 C10A 13.3(4) . . . . ? C2 Ca1 O3 C10A -176.6(3) . . . . ? Si2 Ca1 O3 C10A 82.1(3) . . . . ? Si3 Ca1 O3 C10A -79.8(3) . . . . ? Si4 Ca1 O3 C10A -39.3(3) . . . . ? Si1 Ca1 O3 C10A 104.1(3) . . . . ? N2 Ca1 O3 C10B -93.7(4) . . . . ? N1 Ca1 O3 C10B 63.3(4) . . . . ? O1 Ca1 O3 C10B 175.0(4) . . . . ? O4 Ca1 O3 C10B 1.8(4) . . . . ? O2 Ca1 O3 C10B 136.5(4) . . . . ? C11B Ca1 O3 C10B -20.7(5) . . . . ? C2 Ca1 O3 C10B 149.4(4) . . . . ? Si2 Ca1 O3 C10B 48.1(5) . . . . ? Si3 Ca1 O3 C10B -113.8(4) . . . . ? Si4 Ca1 O3 C10B -73.2(4) . . . . ? Si1 Ca1 O3 C10B 70.1(4) . . . . ? N2 Ca1 O4 C12 -119.5(3) . . . . ? N1 Ca1 O4 C12 16.2(3) . . . . ? O3 Ca1 O4 C12 154.4(3) . . . . ? O2 Ca1 O4 C12 110.6(3) . . . . ? C11B Ca1 O4 C12 -166.0(5) . . . . ? C2 Ca1 O4 C12 67.0(3) . . . . ? Si2 Ca1 O4 C12 -7.6(3) . . . . ? Si3 Ca1 O4 C12 -142.0(3) . . . . ? Si4 Ca1 O4 C12 -98.9(3) . . . . ? Si1 Ca1 O4 C12 38.6(3) . . . . ? N2 Ca1 O4 C11B 46.5(4) . . . . ? N1 Ca1 O4 C11B -177.8(4) . . . . ? O3 Ca1 O4 C11B -39.6(4) . . . . ? O2 Ca1 O4 C11B -83.4(4) . . . . ? C2 Ca1 O4 C11B -127.0(4) . . . . ? Si2 Ca1 O4 C11B 158.4(4) . . . . ? Si3 Ca1 O4 C11B 24.0(4) . . . . ? Si4 Ca1 O4 C11B 67.1(4) . . . . ? Si1 Ca1 O4 C11B -155.4(4) . . . . ? N2 Ca1 O4 C11A 81.1(3) . . . . ? N1 Ca1 O4 C11A -143.1(3) . . . . ? O3 Ca1 O4 C11A -5.0(3) . . . . ? O2 Ca1 O4 C11A -48.7(3) . . . . ? C11B Ca1 O4 C11A 34.6(4) . . . . ? C2 Ca1 O4 C11A -92.4(3) . . . . ? Si2 Ca1 O4 C11A -167.0(3) . . . . ? Si3 Ca1 O4 C11A 58.6(3) . . . . ? Si4 Ca1 O4 C11A 101.7(3) . . . . ? Si1 Ca1 O4 C11A -120.7(3) . . . . ? C17 Si2 N1 Si1 49.7(2) . . . . ? C16 Si2 N1 Si1 166.50(15) . . . . ? C18 Si2 N1 Si1 -73.19(19) . . . . ? Ca1 Si2 N1 Si1 178.6(2) . . . . ? C17 Si2 N1 Ca1 -128.97(14) . . . . ? C16 Si2 N1 Ca1 -12.13(17) . . . . ? C18 Si2 N1 Ca1 108.17(15) . . . . ? C13 Si1 N1 Si2 169.03(14) . . . . ? C15 Si1 N1 Si2 47.25(19) . . . . ? C14 Si1 N1 Si2 -73.32(18) . . . . ? Ca1 Si1 N1 Si2 -178.6(2) . . . . ? C13 Si1 N1 Ca1 -12.41(18) . . . . ? C15 Si1 N1 Ca1 -134.19(13) . . . . ? C14 Si1 N1 Ca1 105.24(15) . . . . ? N2 Ca1 N1 Si2 -19.1(2) . . . . ? O1 Ca1 N1 Si2 69.67(12) . . . . ? O4 Ca1 N1 Si2 -111.49(13) . . . . ? O3 Ca1 N1 Si2 -165.04(9) . . . . ? O2 Ca1 N1 Si2 135.51(11) . . . . ? C11B Ca1 N1 Si2 -112.6(2) . . . . ? C2 Ca1 N1 Si2 92.44(12) . . . . ? Si3 Ca1 N1 Si2 8.2(2) . . . . ? Si4 Ca1 N1 Si2 -32.67(13) . . . . ? Si1 Ca1 N1 Si2 178.6(2) . . . . ? N2 Ca1 N1 Si1 162.32(9) . . . . ? O1 Ca1 N1 Si1 -108.95(14) . . . . ? O4 Ca1 N1 Si1 69.90(14) . . . . ? O3 Ca1 N1 Si1 16.35(18) . . . . ? O2 Ca1 N1 Si1 -43.10(13) . . . . ? C11B Ca1 N1 Si1 68.8(2) . . . . ? C2 Ca1 N1 Si1 -86.17(14) . . . . ? Si2 Ca1 N1 Si1 -178.6(2) . . . . ? Si3 Ca1 N1 Si1 -170.42(6) . . . . ? Si4 Ca1 N1 Si1 148.71(11) . . . . ? C24 Si4 N2 Si3 47.56(19) . . . . ? C23 Si4 N2 Si3 164.52(16) . . . . ? C22 Si4 N2 Si3 -74.37(19) . . . . ? Ca1 Si4 N2 Si3 175.3(2) . . . . ? C24 Si4 N2 Ca1 -127.77(14) . . . . ? C23 Si4 N2 Ca1 -10.82(19) . . . . ? C22 Si4 N2 Ca1 110.30(16) . . . . ? C21 Si3 N2 Si4 45.8(2) . . . . ? C19 Si3 N2 Si4 -76.5(2) . . . . ? C20 Si3 N2 Si4 165.30(15) . . . . ? Ca1 Si3 N2 Si4 -175.4(2) . . . . ? C21 Si3 N2 Ca1 -138.84(14) . . . . ? C19 Si3 N2 Ca1 98.84(18) . . . . ? C20 Si3 N2 Ca1 -19.31(18) . . . . ? N1 Ca1 N2 Si4 -31.5(2) . . . . ? O1 Ca1 N2 Si4 -117.83(13) . . . . ? O4 Ca1 N2 Si4 57.74(14) . . . . ? O3 Ca1 N2 Si4 123.41(13) . . . . ? O2 Ca1 N2 Si4 179.50(10) . . . . ? C11B Ca1 N2 Si4 77.0(2) . . . . ? C2 Ca1 N2 Si4 -125.89(12) . . . . ? Si2 Ca1 N2 Si4 -40.22(14) . . . . ? Si3 Ca1 N2 Si4 175.3(2) . . . . ? Si1 Ca1 N2 Si4 -13.3(2) . . . . ? N1 Ca1 N2 Si3 153.14(9) . . . . ? O1 Ca1 N2 Si3 66.82(13) . . . . ? O4 Ca1 N2 Si3 -117.61(13) . . . . ? O3 Ca1 N2 Si3 -51.94(13) . . . . ? O2 Ca1 N2 Si3 4.15(16) . . . . ? C11B Ca1 N2 Si3 -98.4(2) . . . . ? C2 Ca1 N2 Si3 58.77(15) . . . . ? Si2 Ca1 N2 Si3 144.43(11) . . . . ? Si4 Ca1 N2 Si3 -175.3(2) . . . . ? Si1 Ca1 N2 Si3 171.35(7) . . . . ? C1 O1 C2 C3 -114.6(3) . . . . ? Ca1 O1 C2 C3 64.2(2) . . . . ? C1 O1 C2 Ca1 -178.8(3) . . . . ? N2 Ca1 C2 O1 19.2(2) . . . . ? N1 Ca1 C2 O1 -114.66(19) . . . . ? O4 Ca1 C2 O1 -167.93(16) . . . . ? O3 Ca1 C2 O1 116.92(18) . . . . ? O2 Ca1 C2 O1 132.6(2) . . . . ? C11B Ca1 C2 O1 134.5(5) . . . . ? Si2 Ca1 C2 O1 -88.40(18) . . . . ? Si3 Ca1 C2 O1 40.61(18) . . . . ? Si4 Ca1 C2 O1 -5.7(2) . . . . ? Si1 Ca1 C2 O1 -139.00(18) . . . . ? N2 Ca1 C2 C3 -101.94(17) . . . . ? N1 Ca1 C2 C3 124.15(18) . . . . ? O1 Ca1 C2 C3 -121.2(3) . . . . ? O4 Ca1 C2 C3 70.9(2) . . . . ? O3 Ca1 C2 C3 -4.27(18) . . . . ? O2 Ca1 C2 C3 11.44(14) . . . . ? C11B Ca1 C2 C3 13.4(6) . . . . ? Si2 Ca1 C2 C3 150.41(17) . . . . ? Si3 Ca1 C2 C3 -80.58(16) . . . . ? Si4 Ca1 C2 C3 -126.88(15) . . . . ? Si1 Ca1 C2 C3 99.81(16) . . . . ? C4 O2 C3 C2 165.5(2) . . . . ? Ca1 O2 C3 C2 22.0(3) . . . . ? O1 C2 C3 O2 -56.5(3) . . . . ? Ca1 C2 C3 O2 -15.70(19) . . . . ? C3 O2 C4 C5 -179.0(2) . . . . ? Ca1 O2 C4 C5 -36.8(2) . . . . ? C3 O2 C4 C9 58.2(3) . . . . ? Ca1 O2 C4 C9 -159.66(17) . . . . ? C10A O3 C5 C4 168.8(3) . . . . ? C10B O3 C5 C4 -169.5(4) . . . . ? Ca1 O3 C5 C4 -51.2(2) . . . . ? C10A O3 C5 C6 46.6(4) . . . . ? C10B O3 C5 C6 68.3(4) . . . . ? Ca1 O3 C5 C6 -173.32(16) . . . . ? O2 C4 C5 O3 54.4(2) . . . . ? C9 C4 C5 O3 178.6(2) . . . . ? O2 C4 C5 C6 177.7(2) . . . . ? C9 C4 C5 C6 -58.0(3) . . . . ? O3 C5 C6 C7 175.2(2) . . . . ? C4 C5 C6 C7 56.2(3) . . . . ? C5 C6 C7 C8 -54.8(3) . . . . ? C6 C7 C8 C9 55.5(3) . . . . ? O2 C4 C9 C8 178.9(2) . . . . ? C5 C4 C9 C8 57.6(3) . . . . ? C7 C8 C9 C4 -56.4(3) . . . . ? C5 O3 C10A C11A 78.8(4) . . . . ? C10B O3 C10A C11A 35.7(7) . . . . ? Ca1 O3 C10A C11A -64.5(4) . . . . ? C12 O4 C11A C10A 171.4(3) . . . . ? C11B O4 C11A C10A 49.1(7) . . . . ? Ca1 O4 C11A C10A -24.9(5) . . . . ? O3 C10A C11A O4 58.5(5) . . . . ? C5 O3 C10B C11B 160.6(6) . . . . ? C10A O3 C10B C11B -54.2(8) . . . . ? Ca1 O3 C10B C11B 36.8(8) . . . . ? O3 C10B C11B O4 -74.5(8) . . . . ? O3 C10B C11B Ca1 -26.6(6) . . . . ? C12 O4 C11B C10B -115.4(6) . . . . ? C11A O4 C11B C10B -41.8(7) . . . . ? Ca1 O4 C11B C10B 77.2(7) . . . . ? C12 O4 C11B Ca1 167.3(5) . . . . ? C11A O4 C11B Ca1 -119.1(6) . . . . ? N2 Ca1 C11B C10B 122.2(7) . . . . ? N1 Ca1 C11B C10B -103.5(6) . . . . ? O1 Ca1 C11B C10B 69.5(10) . . . . ? O4 Ca1 C11B C10B -106.0(9) . . . . ? O3 Ca1 C11B C10B 21.8(5) . . . . ? O2 Ca1 C11B C10B 0.5(7) . . . . ? C2 Ca1 C11B C10B -1.0(10) . . . . ? Si2 Ca1 C11B C10B -130.9(6) . . . . ? Si3 Ca1 C11B C10B 97.5(6) . . . . ? Si4 Ca1 C11B C10B 147.0(7) . . . . ? Si1 Ca1 C11B C10B -81.2(6) . . . . ? N2 Ca1 C11B O4 -131.9(4) . . . . ? N1 Ca1 C11B O4 2.4(5) . . . . ? O1 Ca1 C11B O4 175.5(2) . . . . ? O3 Ca1 C11B O4 127.8(5) . . . . ? O2 Ca1 C11B O4 106.4(4) . . . . ? C2 Ca1 C11B O4 105.0(5) . . . . ? Si2 Ca1 C11B O4 -25.0(5) . . . . ? Si3 Ca1 C11B O4 -156.6(4) . . . . ? Si4 Ca1 C11B O4 -107.0(4) . . . . ? Si1 Ca1 C11B O4 24.8(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 14.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.368 _refine_diff_density_min -0.230 _refine_diff_density_rms 0.047 #==END data_rac10 _database_code_depnum_ccdc_archive 'CCDC 884448' #TrackingRef '- JulienJC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H34 Ca O4' _chemical_formula_sum 'C18 H34 Ca O4' _chemical_formula_weight 354.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, 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' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 11.0925(10) _cell_length_b 13.1506(12) _cell_length_c 13.4576(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1963.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 3316 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 21.73 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.200 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 0.336 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9298 _exptl_absorpt_correction_T_max 0.9867 _exptl_absorpt_process_details 'Platon Mulabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'INCOATEC microsource' _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'APEX Area Detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13645 _diffrn_reflns_av_R_equivalents 0.1070 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 28.50 _reflns_number_total 2501 _reflns_number_gt 2191 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (2001)' _computing_cell_refinement 'Bruker SMART (2001)' _computing_data_reduction 'Bruker SAINT+ (1999)' _computing_structure_solution 'SIR-92 (Altomare 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1999)' _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^)+(0.0882P)^2^+0.7363P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.54(8) _refine_ls_number_reflns 2501 _refine_ls_number_parameters 103 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.1731 _refine_ls_wR_factor_gt 0.1663 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.135 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca Ca 0.77196(8) 0.0000 0.5000 0.0378(2) Uani 1 2 d S . . O1 O 0.7373(3) -0.1477(2) 0.3941(2) 0.0747(10) Uani 1 1 d . . . O2 O 0.9626(2) -0.08132(17) 0.43829(19) 0.0514(6) Uani 1 1 d . . . C1 C 0.8225(4) 0.1296(4) 0.3444(3) 0.0653(11) Uani 1 1 d . . . H1A H 0.8266 0.2029 0.3607 0.078 Uiso 1 1 calc R A . H1B H 0.8864 0.1073 0.2979 0.078 Uiso 1 1 calc R . . C2 C 0.7109(4) 0.0911(3) 0.3281(3) 0.0606(11) Uani 1 1 d . . . H2 H 0.7041 0.0446 0.2696 0.073 Uiso 1 1 calc R . . C3 C 0.6081(5) 0.0976(4) 0.3870(4) 0.0704(12) Uani 1 1 d . . . H3A H 0.5382 0.0567 0.3650 0.084 Uiso 1 1 calc R A . H3B H 0.5854 0.1668 0.4093 0.084 Uiso 1 1 calc R . . C4A C 0.6297(7) -0.1669(6) 0.3401(6) 0.0500(17) Uiso 0.597(9) 1 d P A 1 H4A1 H 0.6390 -0.1424 0.2717 0.075 Uiso 0.597(9) 1 calc PR A 1 H4A2 H 0.5623 -0.1315 0.3719 0.075 Uiso 0.597(9) 1 calc PR A 1 H4A3 H 0.6137 -0.2402 0.3393 0.075 Uiso 0.597(9) 1 calc PR A 1 C5A C 0.8306(8) -0.1883(7) 0.3455(7) 0.052(2) Uiso 0.597(9) 1 d P A 1 H5A1 H 0.8434 -0.1516 0.2821 0.063 Uiso 0.597(9) 1 calc PR A 1 H5A2 H 0.8135 -0.2604 0.3299 0.063 Uiso 0.597(9) 1 calc PR A 1 C6A C 0.9363(6) -0.1814(5) 0.4054(5) 0.0519(17) Uiso 0.597(9) 1 d P A 1 H6A1 H 0.9263 -0.2258 0.4642 0.062 Uiso 0.597(9) 1 calc PR A 1 H6A2 H 1.0059 -0.2072 0.3669 0.062 Uiso 0.597(9) 1 calc PR A 1 C7A C 1.0622(5) -0.0572(4) 0.4871(5) 0.0417(13) Uiso 0.597(9) 1 d P . 1 H7A H 1.0621 -0.0959 0.5511 0.050 Uiso 0.597(9) 1 calc PR A 1 C8A C 1.1769(11) -0.0897(10) 0.4275(9) 0.077(4) Uiso 0.597(9) 1 d P . 1 H8A1 H 1.1770 -0.1644 0.4179 0.092 Uiso 0.597(9) 1 calc PR A 1 H8A2 H 1.1764 -0.0570 0.3612 0.092 Uiso 0.597(9) 1 calc PR A 1 C9B C 1.2893(7) -0.0575(6) 0.4849(7) 0.070(2) Uiso 0.597(9) 1 d P . 1 H9B1 H 1.3613 -0.0714 0.4437 0.084 Uiso 0.597(9) 1 calc PR A 1 H9B2 H 1.2957 -0.0994 0.5458 0.084 Uiso 0.597(9) 1 calc PR A 1 C4B C 0.6135(9) -0.1889(9) 0.3663(8) 0.049(2) Uiso 0.403(9) 1 d P A 2 H4B1 H 0.5902 -0.1627 0.3009 0.073 Uiso 0.403(9) 1 calc PR A 2 H4B2 H 0.5542 -0.1671 0.4160 0.073 Uiso 0.403(9) 1 calc PR A 2 H4B3 H 0.6163 -0.2633 0.3642 0.073 Uiso 0.403(9) 1 calc PR A 2 C5B C 0.8466(12) -0.2036(10) 0.3623(11) 0.055(4) Uiso 0.403(9) 1 d P A 2 H5B1 H 0.8304 -0.2352 0.2969 0.066 Uiso 0.403(9) 1 calc PR A 2 H5B2 H 0.8617 -0.2592 0.4103 0.066 Uiso 0.403(9) 1 calc PR A 2 C6B C 0.9601(7) -0.1399(6) 0.3539(6) 0.042(2) Uiso 0.403(9) 1 d P A 2 H6B1 H 1.0324 -0.1839 0.3503 0.050 Uiso 0.403(9) 1 calc PR A 2 H6B2 H 0.9573 -0.0965 0.2938 0.050 Uiso 0.403(9) 1 calc PR A 2 C7B C 1.0831(7) -0.0284(6) 0.4506(7) 0.039(2) Uiso 0.403(9) 1 d P . 2 H7B H 1.0887 0.0240 0.3970 0.047 Uiso 0.403(9) 1 calc PR A 2 C8B C 1.1924(10) -0.0889(9) 0.4458(9) 0.040(3) Uiso 0.403(9) 1 d P . 2 H8B1 H 1.1921 -0.1278 0.3828 0.048 Uiso 0.403(9) 1 calc PR A 2 H8B2 H 1.1913 -0.1387 0.5010 0.048 Uiso 0.403(9) 1 calc PR A 2 C9A C 1.3116(9) -0.0272(8) 0.4518(8) 0.051(2) Uiso 0.403(9) 1 d P . 2 H9A1 H 1.3819 -0.0734 0.4475 0.061 Uiso 0.403(9) 1 calc PR A 2 H9A2 H 1.3162 0.0220 0.3962 0.061 Uiso 0.403(9) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca 0.0570(5) 0.0276(3) 0.0289(3) -0.0028(4) 0.000 0.000 O1 0.0694(18) 0.0664(16) 0.088(2) -0.0497(15) -0.0423(16) 0.0279(15) O2 0.0599(15) 0.0417(12) 0.0525(14) -0.0077(11) 0.0108(11) -0.0018(11) C1 0.076(3) 0.060(2) 0.060(2) 0.025(2) 0.009(2) 0.015(2) C2 0.077(3) 0.065(2) 0.0403(17) 0.0135(16) -0.0033(18) 0.026(2) C3 0.078(3) 0.063(2) 0.070(3) 0.011(2) 0.002(2) 0.026(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 O1 2.439(2) . ? Ca O1 2.439(2) 3_556 ? Ca O2 2.511(3) 3_556 ? Ca O2 2.511(3) . ? Ca C2 2.691(3) . ? Ca C2 2.691(3) 3_556 ? Ca C3 2.695(4) . ? Ca C3 2.695(4) 3_556 ? Ca C1 2.757(4) . ? Ca C1 2.757(4) 3_556 ? O1 C5A 1.335(9) . ? O1 C4A 1.421(7) . ? O1 C5B 1.481(14) . ? O1 C4B 1.524(11) . ? O2 C7A 1.325(6) . ? O2 C6B 1.372(8) . ? O2 C6A 1.418(7) . ? O2 C7B 1.516(9) . ? C1 C2 1.355(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.391(7) . ? C2 H2 1.0000 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4A H4A1 0.9800 . ? C4A H4A2 0.9800 . ? C4A H4A3 0.9800 . ? C5A C6A 1.427(11) . ? C5A H5A1 0.9900 . ? C5A H5A2 0.9900 . ? C6A H6A1 0.9900 . ? C6A H6A2 0.9900 . ? C7A C7A 1.543(10) 3_556 ? C7A C8A 1.564(13) . ? C7A H7A 1.0000 . ? C8A C9B 1.527(14) . ? C8A H8A1 0.9900 . ? C8A H8A2 0.9900 . ? C9B C9B 1.566(16) 3_556 ? C9B H9B1 0.9900 . ? C9B H9B2 0.9900 . ? C4B H4B1 0.9800 . ? C4B H4B2 0.9800 . ? C4B H4B3 0.9800 . ? C5B C6B 1.517(15) . ? C5B H5B1 0.9900 . ? C5B H5B2 0.9900 . ? C6B H6B1 0.9900 . ? C6B H6B2 0.9900 . ? C7B C8B 1.453(13) . ? C7B C7B 1.524(16) 3_556 ? C7B H7B 1.0000 . ? C8B C9A 1.554(15) . ? C8B H8B1 0.9900 . ? C8B H8B2 0.9900 . ? C9A C9A 1.482(19) 3_556 ? C9A H9A1 0.9900 . ? C9A H9A2 0.9900 . ? 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 O1 Ca O1 161.89(15) . 3_556 ? O1 Ca O2 131.67(10) . 3_556 ? O1 Ca O2 66.44(9) 3_556 3_556 ? O1 Ca O2 66.44(9) . . ? O1 Ca O2 131.67(10) 3_556 . ? O2 Ca O2 65.26(11) 3_556 . ? O1 Ca C2 79.19(13) . . ? O1 Ca C2 96.21(13) 3_556 . ? O2 Ca C2 107.86(12) 3_556 . ? O2 Ca C2 96.73(11) . . ? O1 Ca C2 96.21(13) . 3_556 ? O1 Ca C2 79.19(13) 3_556 3_556 ? O2 Ca C2 96.73(11) 3_556 3_556 ? O2 Ca C2 107.86(12) . 3_556 ? C2 Ca C2 150.8(2) . 3_556 ? O1 Ca C3 86.75(13) . . ? O1 Ca C3 81.05(14) 3_556 . ? O2 Ca C3 123.48(14) 3_556 . ? O2 Ca C3 125.74(12) . . ? C2 Ca C3 29.92(14) . . ? C2 Ca C3 121.82(15) 3_556 . ? O1 Ca C3 81.05(14) . 3_556 ? O1 Ca C3 86.75(13) 3_556 3_556 ? O2 Ca C3 125.74(12) 3_556 3_556 ? O2 Ca C3 123.48(14) . 3_556 ? C2 Ca C3 121.82(15) . 3_556 ? C2 Ca C3 29.92(14) 3_556 3_556 ? C3 Ca C3 95.2(2) . 3_556 ? O1 Ca C1 94.59(14) . . ? O1 Ca C1 89.07(13) 3_556 . ? O2 Ca C1 79.45(12) 3_556 . ? O2 Ca C1 80.84(11) . . ? C2 Ca C1 28.76(14) . . ? C2 Ca C1 168.21(14) 3_556 . ? C3 Ca C1 54.12(14) . . ? C3 Ca C1 149.31(15) 3_556 . ? O1 Ca C1 89.07(13) . 3_556 ? O1 Ca C1 94.59(14) 3_556 3_556 ? O2 Ca C1 80.84(11) 3_556 3_556 ? O2 Ca C1 79.45(12) . 3_556 ? C2 Ca C1 168.21(14) . 3_556 ? C2 Ca C1 28.76(14) 3_556 3_556 ? C3 Ca C1 149.31(15) . 3_556 ? C3 Ca C1 54.12(14) 3_556 3_556 ? C1 Ca C1 156.56(19) . 3_556 ? C5A O1 C4A 109.2(5) . . ? C5A O1 C5B 13.1(7) . . ? C4A O1 C5B 116.8(6) . . ? C5A O1 C4B 115.8(6) . . ? C4A O1 C4B 18.7(5) . . ? C5B O1 C4B 119.4(6) . . ? C5A O1 Ca 118.9(4) . . ? C4A O1 Ca 125.0(3) . . ? C5B O1 Ca 115.8(5) . . ? C4B O1 Ca 124.7(4) . . ? C7A O2 C6B 124.2(4) . . ? C7A O2 C6A 123.3(4) . . ? C6B O2 C6A 38.5(4) . . ? C7A O2 C7B 25.8(3) . . ? C6B O2 C7B 111.5(5) . . ? C6A O2 C7B 129.9(4) . . ? C7A O2 Ca 115.9(3) . . ? C6B O2 Ca 119.7(4) . . ? C6A O2 Ca 109.0(3) . . ? C7B O2 Ca 120.7(3) . . ? C2 C1 Ca 72.9(2) . . ? C2 C1 H1A 116.3 . . ? Ca C1 H1A 116.3 . . ? C2 C1 H1B 116.3 . . ? Ca C1 H1B 116.3 . . ? H1A C1 H1B 113.3 . . ? C1 C2 C3 129.3(4) . . ? C1 C2 Ca 78.3(2) . . ? C3 C2 Ca 75.2(2) . . ? C1 C2 H2 115.1 . . ? C3 C2 H2 115.1 . . ? Ca C2 H2 115.1 . . ? C2 C3 Ca 74.9(2) . . ? C2 C3 H3A 116.0 . . ? Ca C3 H3A 116.0 . . ? C2 C3 H3B 116.0 . . ? Ca C3 H3B 116.0 . . ? H3A C3 H3B 113.0 . . ? O1 C4A H4A1 109.5 . . ? O1 C4A H4A2 109.5 . . ? O1 C4A H4A3 109.5 . . ? O1 C5A C6A 109.5(7) . . ? O1 C5A H5A1 109.8 . . ? C6A C5A H5A1 109.8 . . ? O1 C5A H5A2 109.8 . . ? C6A C5A H5A2 109.8 . . ? H5A1 C5A H5A2 108.2 . . ? O2 C6A C5A 113.9(6) . . ? O2 C6A H6A1 108.8 . . ? C5A C6A H6A1 108.8 . . ? O2 C6A H6A2 108.8 . . ? C5A C6A H6A2 108.8 . . ? H6A1 C6A H6A2 107.7 . . ? O2 C7A C7A 110.2(4) . 3_556 ? O2 C7A C8A 111.0(6) . . ? C7A C7A C8A 112.5(6) 3_556 . ? O2 C7A H7A 107.7 . . ? C7A C7A H7A 107.7 3_556 . ? C8A C7A H7A 107.7 . . ? C9B C8A C7A 109.1(8) . . ? C9B C8A H8A1 109.9 . . ? C7A C8A H8A1 109.9 . . ? C9B C8A H8A2 109.9 . . ? C7A C8A H8A2 109.9 . . ? H8A1 C8A H8A2 108.3 . . ? C8A C9B C9B 113.5(7) . 3_556 ? C8A C9B H9B1 108.9 . . ? C9B C9B H9B1 108.9 3_556 . ? C8A C9B H9B2 108.9 . . ? C9B C9B H9B2 108.9 3_556 . ? H9B1 C9B H9B2 107.7 . . ? O1 C4B H4B1 109.5 . . ? O1 C4B H4B2 109.5 . . ? H4B1 C4B H4B2 109.5 . . ? O1 C4B H4B3 109.5 . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? O1 C5B C6B 115.3(9) . . ? O1 C5B H5B1 108.5 . . ? C6B C5B H5B1 108.5 . . ? O1 C5B H5B2 108.5 . . ? C6B C5B H5B2 108.5 . . ? H5B1 C5B H5B2 107.5 . . ? O2 C6B C5B 105.4(7) . . ? O2 C6B H6B1 110.7 . . ? C5B C6B H6B1 110.7 . . ? O2 C6B H6B2 110.7 . . ? C5B C6B H6B2 110.7 . . ? H6B1 C6B H6B2 108.8 . . ? C8B C7B O2 118.6(7) . . ? C8B C7B C7B 107.9(7) . 3_556 ? O2 C7B C7B 108.7(5) . 3_556 ? C8B C7B H7B 107.0 . . ? O2 C7B H7B 107.0 . . ? C7B C7B H7B 107.0 3_556 . ? C7B C8B C9A 114.9(9) . . ? C7B C8B H8B1 108.5 . . ? C9A C8B H8B1 108.5 . . ? C7B C8B H8B2 108.5 . . ? C9A C8B H8B2 108.5 . . ? H8B1 C8B H8B2 107.5 . . ? C9A C9A C8B 107.3(7) 3_556 . ? C9A C9A H9A1 110.3 3_556 . ? C8B C9A H9A1 110.3 . . ? C9A C9A H9A2 110.3 3_556 . ? C8B C9A H9A2 110.3 . . ? H9A1 C9A H9A2 108.5 . . ? 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 O1 Ca O1 C5A 169.6(6) 3_556 . . . ? O2 Ca O1 C5A -11.6(6) 3_556 . . . ? O2 Ca O1 C5A -9.5(5) . . . . ? C2 Ca O1 C5A 92.8(6) . . . . ? C2 Ca O1 C5A -116.3(6) 3_556 . . . ? C3 Ca O1 C5A 122.0(6) . . . . ? C3 Ca O1 C5A -142.2(6) 3_556 . . . ? C1 Ca O1 C5A 68.4(6) . . . . ? C1 Ca O1 C5A -88.4(6) 3_556 . . . ? O1 Ca O1 C4A 22.0(5) 3_556 . . . ? O2 Ca O1 C4A -159.1(5) 3_556 . . . ? O2 Ca O1 C4A -157.1(5) . . . . ? C2 Ca O1 C4A -54.8(5) . . . . ? C2 Ca O1 C4A 96.1(5) 3_556 . . . ? C3 Ca O1 C4A -25.6(5) . . . . ? C3 Ca O1 C4A 70.2(5) 3_556 . . . ? C1 Ca O1 C4A -79.2(5) . . . . ? C1 Ca O1 C4A 124.0(5) 3_556 . . . ? O1 Ca O1 C5B -176.1(7) 3_556 . . . ? O2 Ca O1 C5B 2.8(7) 3_556 . . . ? O2 Ca O1 C5B 4.8(7) . . . . ? C2 Ca O1 C5B 107.1(7) . . . . ? C2 Ca O1 C5B -102.0(7) 3_556 . . . ? C3 Ca O1 C5B 136.3(7) . . . . ? C3 Ca O1 C5B -127.9(7) 3_556 . . . ? C1 Ca O1 C5B 82.7(7) . . . . ? C1 Ca O1 C5B -74.1(7) 3_556 . . . ? O1 Ca O1 C4B -0.9(6) 3_556 . . . ? O2 Ca O1 C4B 178.0(6) 3_556 . . . ? O2 Ca O1 C4B -180.0(6) . . . . ? C2 Ca O1 C4B -77.6(6) . . . . ? C2 Ca O1 C4B 73.2(6) 3_556 . . . ? C3 Ca O1 C4B -48.4(6) . . . . ? C3 Ca O1 C4B 47.4(6) 3_556 . . . ? C1 Ca O1 C4B -102.0(6) . . . . ? C1 Ca O1 C4B 101.1(6) 3_556 . . . ? O1 Ca O2 C7A -162.5(4) . . . . ? O1 Ca O2 C7A 17.9(4) 3_556 . . . ? O2 Ca O2 C7A 15.8(3) 3_556 . . . ? C2 Ca O2 C7A 122.4(4) . . . . ? C2 Ca O2 C7A -73.5(4) 3_556 . . . ? C3 Ca O2 C7A 130.4(4) . . . . ? C3 Ca O2 C7A -102.0(4) 3_556 . . . ? C1 Ca O2 C7A 98.3(4) . . . . ? C1 Ca O2 C7A -68.9(4) 3_556 . . . ? O1 Ca O2 C6B 22.5(4) . . . . ? O1 Ca O2 C6B -157.1(4) 3_556 . . . ? O2 Ca O2 C6B -159.1(5) 3_556 . . . ? C2 Ca O2 C6B -52.5(4) . . . . ? C2 Ca O2 C6B 111.6(4) 3_556 . . . ? C3 Ca O2 C6B -44.5(5) . . . . ? C3 Ca O2 C6B 83.1(5) 3_556 . . . ? C1 Ca O2 C6B -76.6(4) . . . . ? C1 Ca O2 C6B 116.2(4) 3_556 . . . ? O1 Ca O2 C6A -18.3(3) . . . . ? O1 Ca O2 C6A 162.1(3) 3_556 . . . ? O2 Ca O2 C6A 160.0(4) 3_556 . . . ? C2 Ca O2 C6A -93.4(3) . . . . ? C2 Ca O2 C6A 70.8(3) 3_556 . . . ? C3 Ca O2 C6A -85.3(4) . . . . ? C3 Ca O2 C6A 42.3(4) 3_556 . . . ? C1 Ca O2 C6A -117.4(4) . . . . ? C1 Ca O2 C6A 75.3(3) 3_556 . . . ? O1 Ca O2 C7B 168.5(5) . . . . ? O1 Ca O2 C7B -11.1(5) 3_556 . . . ? O2 Ca O2 C7B -13.1(4) 3_556 . . . ? C2 Ca O2 C7B 93.5(5) . . . . ? C2 Ca O2 C7B -102.4(5) 3_556 . . . ? C3 Ca O2 C7B 101.5(5) . . . . ? C3 Ca O2 C7B -130.9(5) 3_556 . . . ? C1 Ca O2 C7B 69.4(5) . . . . ? C1 Ca O2 C7B -97.8(5) 3_556 . . . ? O1 Ca C1 C2 57.5(3) . . . . ? O1 Ca C1 C2 -104.7(3) 3_556 . . . ? O2 Ca C1 C2 -170.9(3) 3_556 . . . ? O2 Ca C1 C2 122.7(3) . . . . ? C2 Ca C1 C2 -98.9(8) 3_556 . . . ? C3 Ca C1 C2 -25.1(3) . . . . ? C3 Ca C1 C2 -22.7(4) 3_556 . . . ? C1 Ca C1 C2 155.8(3) 3_556 . . . ? Ca C1 C2 C3 59.5(4) . . . . ? O1 Ca C2 C1 -121.1(3) . . . . ? O1 Ca C2 C1 76.6(3) 3_556 . . . ? O2 Ca C2 C1 9.4(3) 3_556 . . . ? O2 Ca C2 C1 -56.8(3) . . . . ? C2 Ca C2 C1 155.5(3) 3_556 . . . ? C3 Ca C2 C1 136.4(4) . . . . ? C3 Ca C2 C1 166.6(3) 3_556 . . . ? C1 Ca C2 C1 -127.1(7) 3_556 . . . ? O1 Ca C2 C3 102.5(3) . . . . ? O1 Ca C2 C3 -59.8(3) 3_556 . . . ? O2 Ca C2 C3 -127.0(3) 3_556 . . . ? O2 Ca C2 C3 166.9(3) . . . . ? C2 Ca C2 C3 19.1(3) 3_556 . . . ? C3 Ca C2 C3 30.2(4) 3_556 . . . ? C1 Ca C2 C3 -136.4(4) . . . . ? C1 Ca C2 C3 96.5(7) 3_556 . . . ? C1 C2 C3 Ca -60.8(4) . . . . ? O1 Ca C3 C2 -73.9(3) . . . . ? O1 Ca C3 C2 119.6(3) 3_556 . . . ? O2 Ca C3 C2 65.7(3) 3_556 . . . ? O2 Ca C3 C2 -16.2(3) . . . . ? C2 Ca C3 C2 -169.17(18) 3_556 . . . ? C3 Ca C3 C2 -154.6(4) 3_556 . . . ? C1 Ca C3 C2 24.2(3) . . . . ? C1 Ca C3 C2 -156.6(3) 3_556 . . . ? C4A O1 C5A C6A -172.2(7) . . . . ? C5B O1 C5A C6A -44(3) . . . . ? C4B O1 C5A C6A -153.2(7) . . . . ? Ca O1 C5A C6A 35.5(9) . . . . ? C7A O2 C6A C5A -173.8(6) . . . . ? C6B O2 C6A C5A -69.0(8) . . . . ? C7B O2 C6A C5A -142.5(7) . . . . ? Ca O2 C6A C5A 45.2(7) . . . . ? O1 C5A C6A O2 -54.6(9) . . . . ? C6B O2 C7A C7A 133.9(6) . . . 3_556 ? C6A O2 C7A C7A -179.4(5) . . . 3_556 ? C7B O2 C7A C7A 66.7(9) . . . 3_556 ? Ca O2 C7A C7A -40.7(8) . . . 3_556 ? C6B O2 C7A C8A 8.7(9) . . . . ? C6A O2 C7A C8A 55.4(9) . . . . ? C7B O2 C7A C8A -58.5(10) . . . . ? Ca O2 C7A C8A -166.0(6) . . . . ? O2 C7A C8A C9B 178.3(7) . . . . ? C7A C7A C8A C9B 54.3(12) 3_556 . . . ? C7A C8A C9B C9B -52.4(14) . . . 3_556 ? C5A O1 C5B C6B 78(3) . . . . ? C4A O1 C5B C6B 134.5(9) . . . . ? C4B O1 C5B C6B 155.6(9) . . . . ? Ca O1 C5B C6B -28.9(13) . . . . ? C7A O2 C6B C5B 143.3(7) . . . . ? C6A O2 C6B C5B 41.1(8) . . . . ? C7B O2 C6B C5B 168.9(8) . . . . ? Ca O2 C6B C5B -42.2(9) . . . . ? O1 C5B C6B O2 45.2(12) . . . . ? C7A O2 C7B C8B 73.0(11) . . . . ? C6B O2 C7B C8B -51.9(10) . . . . ? C6A O2 C7B C8B -12.1(12) . . . . ? Ca O2 C7B C8B 159.5(7) . . . . ? C7A O2 C7B C7B -50.6(9) . . . 3_556 ? C6B O2 C7B C7B -175.6(7) . . . 3_556 ? C6A O2 C7B C7B -135.7(7) . . . 3_556 ? Ca O2 C7B C7B 35.8(10) . . . 3_556 ? O2 C7B C8B C9A 175.9(8) . . . . ? C7B C7B C8B C9A -60.1(13) 3_556 . . . ? C7B C8B C9A C9A 60.3(14) . . . 3_556 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.574 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.069 #==END data_[Ca{N(SiMe3)2}2(thf)2] _database_code_depnum_ccdc_archive 'CCDC 884449' #TrackingRef '- JulienJC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H72 Ca2 N4 O2 Si8' _chemical_formula_sum 'C24 H72 Ca2 N4 O2 Si8' _chemical_formula_weight 753.74 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _space_group_name_Hall '-P 2yn' 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 18.1714(18) _cell_length_b 23.153(2) _cell_length_c 21.826(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.8750(15) _cell_angle_gamma 90.00 _cell_volume 9095.8(16) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6991 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 26.74 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.101 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3296 _exptl_absorpt_coefficient_mu 0.486 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8760 _exptl_absorpt_correction_T_max 0.9485 _exptl_absorpt_process_details 'Platon Mulabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 123697 _diffrn_reflns_av_R_equivalents 0.0811 _diffrn_reflns_av_sigmaI/netI 0.0775 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 28.39 _reflns_number_total 22744 _reflns_number_gt 14770 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (2001)' _computing_cell_refinement 'Bruker SMART (2001)' _computing_data_reduction 'Bruker SAINT+ (1999)' _computing_structure_solution 'SIR 92 (Altomare et al, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0275P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22744 _refine_ls_number_parameters 801 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0661 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0803 _refine_ls_wR_factor_gt 0.0733 _refine_ls_goodness_of_fit_ref 0.850 _refine_ls_restrained_S_all 0.850 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.34418(3) 0.66732(2) 0.19180(3) 0.02323(13) Uani 1 1 d . . . H1 H 0.2712(10) 0.6817(8) 0.1580(8) 0.028 Uiso 1 1 d . . . Si2 Si 0.41144(3) 0.55088(2) 0.21455(3) 0.02125(13) Uani 1 1 d . . . H2 H 0.3926(10) 0.5024(8) 0.2525(8) 0.026 Uiso 1 1 d . . . Si3 Si 0.16873(3) 0.65148(2) 0.30095(3) 0.02160(13) Uani 1 1 d . . . H3 H 0.2437(10) 0.6510(8) 0.3375(8) 0.026 Uiso 1 1 d . . . Si4 Si 0.08702(3) 0.55546(2) 0.23082(3) 0.02097(13) Uani 1 1 d . . . H4 H 0.0951(10) 0.5321(8) 0.1707(8) 0.025 Uiso 1 1 d . . . Si5 Si 0.22299(3) 0.44625(3) 0.14485(3) 0.02561(14) Uani 1 1 d . . . H5 H 0.2345(10) 0.4749(8) 0.2071(8) 0.031 Uiso 1 1 d . . . Si6 Si 0.21542(3) 0.50480(3) 0.01705(3) 0.02635(14) Uani 1 1 d . . . H6 H 0.2156(10) 0.5655(8) 0.0005(9) 0.032 Uiso 1 1 d . . . Si7 Si 0.24197(3) 0.49238(3) 0.42316(3) 0.02488(14) Uani 1 1 d . . . H7 H 0.2179(10) 0.5503(8) 0.4084(8) 0.030 Uiso 1 1 d . . . Si8 Si 0.31117(3) 0.40444(2) 0.34382(3) 0.02256(13) Uani 1 1 d . . . H8 H 0.3345(10) 0.4072(8) 0.2844(8) 0.027 Uiso 1 1 d . . . O1 O 0.12332(7) 0.63934(6) 0.08998(6) 0.0253(3) Uani 1 1 d . . . O2 O 0.39121(7) 0.58513(6) 0.37534(6) 0.0241(3) Uani 1 1 d . . . N1 N 0.33737(8) 0.59675(7) 0.21164(7) 0.0194(4) Uani 1 1 d . . . N2 N 0.16718(8) 0.59236(6) 0.25409(7) 0.0178(3) Uani 1 1 d . . . N3 N 0.22110(9) 0.50114(7) 0.09439(7) 0.0239(4) Uani 1 1 d . . . N4 N 0.28327(9) 0.47054(7) 0.36301(7) 0.0200(4) Uani 1 1 d . . . Ca1 Ca 0.21328(2) 0.583173(17) 0.152756(18) 0.01897(9) Uani 1 1 d . . . Ca2 Ca 0.28748(2) 0.553031(17) 0.303453(18) 0.01801(9) Uani 1 1 d . . . C1 C 0.36098(11) 0.72034(9) 0.25660(10) 0.0294(5) Uani 1 1 d . . . H1A H 0.4123 0.7167 0.2770 0.044 Uiso 1 1 calc R . . H1B H 0.3267 0.7126 0.2866 0.044 Uiso 1 1 calc R . . H1C H 0.3528 0.7596 0.2403 0.044 Uiso 1 1 calc R . . C2 C 0.41071(12) 0.68353(10) 0.13576(10) 0.0380(6) Uani 1 1 d . . . H2A H 0.3994 0.6589 0.0992 0.057 Uiso 1 1 calc R . . H2B H 0.4616 0.6760 0.1554 0.057 Uiso 1 1 calc R . . H2C H 0.4060 0.7242 0.1233 0.057 Uiso 1 1 calc R . . C3 C 0.42828(12) 0.51986(10) 0.13881(10) 0.0354(6) Uani 1 1 d . . . H3A H 0.4508 0.5493 0.1150 0.053 Uiso 1 1 calc R . . H3B H 0.3810 0.5072 0.1156 0.053 Uiso 1 1 calc R . . H3C H 0.4619 0.4867 0.1460 0.053 Uiso 1 1 calc R . . C4 C 0.50161(10) 0.58068(9) 0.25310(9) 0.0250(5) Uani 1 1 d . . . H4A H 0.4928 0.6038 0.2890 0.037 Uiso 1 1 calc R . . H4B H 0.5238 0.6051 0.2238 0.037 Uiso 1 1 calc R . . H4C H 0.5355 0.5488 0.2666 0.037 Uiso 1 1 calc R . . C5 C 0.10300(12) 0.65159(10) 0.35946(10) 0.0343(6) Uani 1 1 d . . . H5A H 0.1036 0.6136 0.3794 0.051 Uiso 1 1 calc R . . H5B H 0.0527 0.6600 0.3390 0.051 Uiso 1 1 calc R . . H5C H 0.1181 0.6812 0.3907 0.051 Uiso 1 1 calc R . . C6 C 0.15871(12) 0.72239(9) 0.26025(10) 0.0332(5) Uani 1 1 d . . . H6A H 0.1077 0.7266 0.2393 0.050 Uiso 1 1 calc R . . H6B H 0.1934 0.7242 0.2296 0.050 Uiso 1 1 calc R . . H6C H 0.1698 0.7537 0.2904 0.050 Uiso 1 1 calc R . . C7 C 0.00033(11) 0.59955(9) 0.21553(10) 0.0322(5) Uani 1 1 d . . . H7A H 0.0102 0.6345 0.1927 0.048 Uiso 1 1 calc R . . H7B H -0.0160 0.6104 0.2549 0.048 Uiso 1 1 calc R . . H7C H -0.0386 0.5769 0.1910 0.048 Uiso 1 1 calc R . . C8 C 0.07033(12) 0.49264(9) 0.27985(10) 0.0357(6) Uani 1 1 d . . . H8A H 0.0564 0.5063 0.3192 0.054 Uiso 1 1 calc R . . H8B H 0.1157 0.4694 0.2879 0.054 Uiso 1 1 calc R . . H8C H 0.0301 0.4690 0.2584 0.054 Uiso 1 1 calc R . . C9 C 0.30027(13) 0.39277(9) 0.14506(10) 0.0368(6) Uani 1 1 d . . . H9A H 0.3481 0.4125 0.1553 0.055 Uiso 1 1 calc R . . H9B H 0.2977 0.3750 0.1040 0.055 Uiso 1 1 calc R . . H9C H 0.2955 0.3628 0.1759 0.055 Uiso 1 1 calc R . . C10 C 0.13602(13) 0.40266(9) 0.14282(10) 0.0378(6) Uani 1 1 d . . . H10A H 0.1296 0.3784 0.1057 0.057 Uiso 1 1 calc R . . H10B H 0.0933 0.4286 0.1421 0.057 Uiso 1 1 calc R . . H10C H 0.1396 0.3781 0.1797 0.057 Uiso 1 1 calc R . . C11 C 0.12812(12) 0.47247(9) -0.02504(10) 0.0336(5) Uani 1 1 d . . . H11A H 0.0849 0.4911 -0.0111 0.050 Uiso 1 1 calc R . . H11B H 0.1271 0.4310 -0.0163 0.050 Uiso 1 1 calc R . . H11C H 0.1268 0.4785 -0.0696 0.050 Uiso 1 1 calc R . . C12 C 0.29481(13) 0.47172(11) -0.01685(10) 0.0432(6) Uani 1 1 d . . . H12A H 0.2972 0.4303 -0.0076 0.065 Uiso 1 1 calc R . . H12B H 0.3414 0.4902 0.0011 0.065 Uiso 1 1 calc R . . H12C H 0.2874 0.4774 -0.0618 0.065 Uiso 1 1 calc R . . C13 C 0.30218(12) 0.49965(9) 0.49968(9) 0.0329(5) Uani 1 1 d . . . H13A H 0.3411 0.5283 0.4963 0.049 Uiso 1 1 calc R . . H13B H 0.3251 0.4623 0.5116 0.049 Uiso 1 1 calc R . . H13C H 0.2718 0.5121 0.5311 0.049 Uiso 1 1 calc R . . C14 C 0.16009(12) 0.44966(11) 0.44032(11) 0.0434(6) Uani 1 1 d . . . H14A H 0.1772 0.4141 0.4620 0.065 Uiso 1 1 calc R . . H14B H 0.1287 0.4399 0.4015 0.065 Uiso 1 1 calc R . . H14C H 0.1313 0.4726 0.4664 0.065 Uiso 1 1 calc R . . C15 C 0.39243(12) 0.37504(9) 0.39702(10) 0.0337(5) Uani 1 1 d . . . H15A H 0.3793 0.3719 0.4390 0.051 Uiso 1 1 calc R . . H15B H 0.4350 0.4011 0.3973 0.051 Uiso 1 1 calc R . . H15C H 0.4055 0.3368 0.3826 0.051 Uiso 1 1 calc R . . C16 C 0.23710(13) 0.34801(10) 0.33819(12) 0.0451(7) Uani 1 1 d . . . H16A H 0.1943 0.3607 0.3090 0.068 Uiso 1 1 calc R . . H16B H 0.2217 0.3420 0.3790 0.068 Uiso 1 1 calc R . . H16C H 0.2564 0.3118 0.3236 0.068 Uiso 1 1 calc R . . C17 C 0.12281(15) 0.69977(11) 0.07564(14) 0.0621(9) Uani 1 1 d . . . H17A H 0.1685 0.7103 0.0582 0.074 Uiso 1 1 calc R . . H17B H 0.1209 0.7228 0.1136 0.074 Uiso 1 1 calc R . . C18 C 0.05534(12) 0.71191(9) 0.02922(10) 0.0313(5) Uani 1 1 d . . . H18A H 0.0688 0.7154 -0.0131 0.038 Uiso 1 1 calc R . . H18B H 0.0302 0.7478 0.0397 0.038 Uiso 1 1 calc R . . C19 C 0.00648(12) 0.65955(9) 0.03465(10) 0.0344(6) Uani 1 1 d . . . H19A H -0.0257 0.6652 0.0673 0.041 Uiso 1 1 calc R . . H19B H -0.0251 0.6513 -0.0051 0.041 Uiso 1 1 calc R . . C20 C 0.06173(11) 0.61213(9) 0.05152(10) 0.0294(5) Uani 1 1 d . . . H20A H 0.0399 0.5811 0.0745 0.035 Uiso 1 1 calc R . . H20B H 0.0782 0.5953 0.0140 0.035 Uiso 1 1 calc R . . C21 C 0.41327(12) 0.64075(9) 0.40147(10) 0.0300(5) Uani 1 1 d . . . H21A H 0.3694 0.6631 0.4100 0.036 Uiso 1 1 calc R . . H21B H 0.4401 0.6632 0.3729 0.036 Uiso 1 1 calc R . . C22 C 0.46332(13) 0.62761(10) 0.46038(10) 0.0394(6) Uani 1 1 d . . . H22A H 0.4344 0.6194 0.4946 0.047 Uiso 1 1 calc R . . H22B H 0.4980 0.6599 0.4724 0.047 Uiso 1 1 calc R . . C23 C 0.50445(13) 0.57427(10) 0.44310(12) 0.0431(6) Uani 1 1 d . . . H23A H 0.5473 0.5848 0.4218 0.052 Uiso 1 1 calc R . . H23B H 0.5223 0.5508 0.4801 0.052 Uiso 1 1 calc R . . C24 C 0.44621(11) 0.54228(9) 0.40026(9) 0.0265(5) Uani 1 1 d . . . H24A H 0.4687 0.5237 0.3664 0.032 Uiso 1 1 calc R . . H24B H 0.4228 0.5120 0.4231 0.032 Uiso 1 1 calc R . . Si9 Si 0.07591(3) 0.19167(2) 0.77013(3) 0.02153(13) Uani 1 1 d . . . H9 H 0.0825(10) 0.2386(8) 0.7292(8) 0.026 Uiso 1 1 d . . . Si10 Si 0.15758(3) 0.08072(2) 0.78749(3) 0.02047(12) Uani 1 1 d . . . H10 H 0.2329(10) 0.0700(8) 0.8177(8) 0.025 Uiso 1 1 d . . . Si11 Si 0.40326(3) 0.20502(2) 0.75704(3) 0.02337(13) Uani 1 1 d . . . H11 H 0.3922(10) 0.2233(8) 0.8205(8) 0.028 Uiso 1 1 d . . . Si12 Si 0.32847(3) 0.11158(2) 0.67931(3) 0.02156(13) Uani 1 1 d . . . H12 H 0.2564(10) 0.1126(8) 0.6432(8) 0.026 Uiso 1 1 d . . . Si13 Si 0.26168(3) 0.23483(3) 0.97689(3) 0.02461(14) Uani 1 1 d . . . H13 H 0.3283(10) 0.2452(8) 1.0168(8) 0.030 Uiso 1 1 d . . . Si14 Si 0.27006(3) 0.30477(2) 0.85745(3) 0.02102(13) Uani 1 1 d . . . H14 H 0.2592(10) 0.2803(8) 0.7919(8) 0.025 Uiso 1 1 d . . . Si15 Si 0.18032(3) 0.35291(3) 0.66538(3) 0.02817(14) Uani 1 1 d . . . H15 H 0.1440(10) 0.3436(8) 0.7215(9) 0.034 Uiso 1 1 d . . . Si16 Si 0.23994(4) 0.27596(3) 0.56977(3) 0.03473(16) Uani 1 1 d . . . H16 H 0.2660(11) 0.2144(9) 0.5763(9) 0.042 Uiso 1 1 d . . . O3 O 0.37166(8) 0.11757(6) 0.89058(7) 0.0339(4) Uani 1 1 d . . . O4 O 0.10006(8) 0.17027(6) 0.60604(6) 0.0323(4) Uani 1 1 d . . . N5 N 0.15603(8) 0.15285(7) 0.77258(7) 0.0187(4) Uani 1 1 d . . . N6 N 0.32505(8) 0.16631(7) 0.73122(7) 0.0199(4) Uani 1 1 d . . . N7 N 0.26791(9) 0.24575(7) 0.90177(7) 0.0212(4) Uani 1 1 d . . . N8 N 0.20537(9) 0.29025(7) 0.63566(7) 0.0242(4) Uani 1 1 d . . . Ca3 Ca 0.27760(2) 0.171675(17) 0.832209(18) 0.01946(9) Uani 1 1 d . . . Ca4 Ca 0.20071(2) 0.200902(18) 0.681849(18) 0.02178(9) Uani 1 1 d . . . C25 C 0.05902(12) 0.22283(9) 0.84576(10) 0.0311(5) Uani 1 1 d . . . H25A H 0.0445 0.1920 0.8724 0.047 Uiso 1 1 calc R . . H25B H 0.0192 0.2516 0.8388 0.047 Uiso 1 1 calc R . . H25C H 0.1045 0.2413 0.8658 0.047 Uiso 1 1 calc R . . C26 C -0.00990(11) 0.15256(9) 0.73525(10) 0.0309(5) Uani 1 1 d . . . H26A H 0.0000 0.1322 0.6979 0.046 Uiso 1 1 calc R . . H26B H -0.0502 0.1804 0.7245 0.046 Uiso 1 1 calc R . . H26C H -0.0244 0.1246 0.7652 0.046 Uiso 1 1 calc R . . C27 C 0.09763(12) 0.05565(9) 0.84539(9) 0.0300(5) Uani 1 1 d . . . H27A H 0.1043 0.0814 0.8814 0.045 Uiso 1 1 calc R . . H27B H 0.1117 0.0162 0.8585 0.045 Uiso 1 1 calc R . . H27C H 0.0455 0.0562 0.8266 0.045 Uiso 1 1 calc R . . C28 C 0.14176(11) 0.03256(8) 0.71834(9) 0.0248(5) Uani 1 1 d . . . H28A H 0.0905 0.0371 0.6980 0.037 Uiso 1 1 calc R . . H28B H 0.1502 -0.0077 0.7313 0.037 Uiso 1 1 calc R . . H28C H 0.1762 0.0430 0.6893 0.037 Uiso 1 1 calc R . . C29 C 0.41710(12) 0.27019(9) 0.71032(11) 0.0362(6) Uani 1 1 d . . . H29A H 0.4319 0.2584 0.6706 0.054 Uiso 1 1 calc R . . H29B H 0.4561 0.2944 0.7327 0.054 Uiso 1 1 calc R . . H29C H 0.3706 0.2921 0.7029 0.054 Uiso 1 1 calc R . . C30 C 0.49191(11) 0.16343(9) 0.77136(10) 0.0312(5) Uani 1 1 d . . . H30A H 0.4837 0.1275 0.7932 0.047 Uiso 1 1 calc R . . H30B H 0.5297 0.1867 0.7966 0.047 Uiso 1 1 calc R . . H30C H 0.5089 0.1543 0.7318 0.047 Uiso 1 1 calc R . . C31 C 0.34326(12) 0.03731(9) 0.71146(10) 0.0302(5) Uani 1 1 d . . . H31A H 0.3945 0.0335 0.7319 0.045 Uiso 1 1 calc R . . H31B H 0.3342 0.0091 0.6778 0.045 Uiso 1 1 calc R . . H31C H 0.3089 0.0303 0.7415 0.045 Uiso 1 1 calc R . . C32 C 0.39430(12) 0.12183(10) 0.62173(10) 0.0345(6) Uani 1 1 d . . . H32A H 0.3878 0.1606 0.6038 0.052 Uiso 1 1 calc R . . H32B H 0.3843 0.0929 0.5889 0.052 Uiso 1 1 calc R . . H32C H 0.4454 0.1174 0.6423 0.052 Uiso 1 1 calc R . . C33 C 0.18982(13) 0.27882(10) 1.00999(10) 0.0413(6) Uani 1 1 d . . . H33A H 0.2006 0.3200 1.0058 0.062 Uiso 1 1 calc R . . H33B H 0.1907 0.2693 1.0538 0.062 Uiso 1 1 calc R . . H33C H 0.1406 0.2702 0.9876 0.062 Uiso 1 1 calc R . . C34 C 0.23958(13) 0.15688(9) 0.98877(10) 0.0376(6) Uani 1 1 d . . . H34A H 0.1911 0.1476 0.9653 0.056 Uiso 1 1 calc R . . H34B H 0.2381 0.1497 1.0328 0.056 Uiso 1 1 calc R . . H34C H 0.2779 0.1326 0.9744 0.056 Uiso 1 1 calc R . . C35 C 0.35853(11) 0.34724(9) 0.86853(10) 0.0317(5) Uani 1 1 d . . . H35A H 0.3637 0.3668 0.9087 0.048 Uiso 1 1 calc R . . H35B H 0.3575 0.3760 0.8355 0.048 Uiso 1 1 calc R . . H35C H 0.4007 0.3211 0.8672 0.048 Uiso 1 1 calc R . . C36 C 0.19314(11) 0.35797(9) 0.85857(9) 0.0293(5) Uani 1 1 d . . . H36A H 0.1454 0.3387 0.8465 0.044 Uiso 1 1 calc R . . H36B H 0.1989 0.3893 0.8295 0.044 Uiso 1 1 calc R . . H36C H 0.1947 0.3738 0.9004 0.044 Uiso 1 1 calc R . . C37 C 0.25831(13) 0.40543(10) 0.68556(12) 0.0468(7) Uani 1 1 d . . . H37A H 0.2983 0.3868 0.7133 0.070 Uiso 1 1 calc R . . H37B H 0.2402 0.4391 0.7062 0.070 Uiso 1 1 calc R . . H37C H 0.2773 0.4178 0.6477 0.070 Uiso 1 1 calc R . . C38 C 0.10629(13) 0.39337(10) 0.61492(10) 0.0400(6) Uani 1 1 d . . . H38A H 0.1260 0.4071 0.5779 0.060 Uiso 1 1 calc R . . H38B H 0.0902 0.4264 0.6377 0.060 Uiso 1 1 calc R . . H38C H 0.0639 0.3678 0.6026 0.060 Uiso 1 1 calc R . . C39 C 0.32053(14) 0.32046(11) 0.55363(12) 0.0518(7) Uani 1 1 d . . . H39A H 0.3041 0.3602 0.5443 0.078 Uiso 1 1 calc R . . H39B H 0.3412 0.3043 0.5182 0.078 Uiso 1 1 calc R . . H39C H 0.3587 0.3203 0.5900 0.078 Uiso 1 1 calc R . . C40 C 0.17281(16) 0.27720(11) 0.49760(10) 0.0592(8) Uani 1 1 d . . . H40A H 0.1350 0.2474 0.4997 0.089 Uiso 1 1 calc R . . H40B H 0.1991 0.2697 0.4621 0.089 Uiso 1 1 calc R . . H40C H 0.1489 0.3152 0.4929 0.089 Uiso 1 1 calc R . . C41 C 0.38192(14) 0.05558(10) 0.89266(11) 0.0444(7) Uani 1 1 d . . . H41A H 0.3840 0.0403 0.8506 0.053 Uiso 1 1 calc R . . H41B H 0.3402 0.0367 0.9097 0.053 Uiso 1 1 calc R . . C42 C 0.45269(14) 0.04426(12) 0.93288(13) 0.0561(8) Uani 1 1 d . . . H42A H 0.4496 0.0085 0.9573 0.067 Uiso 1 1 calc R . . H42B H 0.4943 0.0407 0.9083 0.067 Uiso 1 1 calc R . . C43 C 0.46187(17) 0.09542(13) 0.97330(12) 0.0714(10) Uani 1 1 d . . . H43A H 0.5151 0.1024 0.9882 0.086 Uiso 1 1 calc R . . H43B H 0.4351 0.0903 1.0095 0.086 Uiso 1 1 calc R . . C44 C 0.42966(13) 0.14457(11) 0.93390(11) 0.0468(7) Uani 1 1 d . . . H44A H 0.4086 0.1742 0.9592 0.056 Uiso 1 1 calc R . . H44B H 0.4678 0.1627 0.9118 0.056 Uiso 1 1 calc R . . C45 C 0.03683(13) 0.20821(11) 0.58735(10) 0.0430(6) Uani 1 1 d . . . H45A H 0.0539 0.2479 0.5801 0.052 Uiso 1 1 calc R . . H45B H 0.0036 0.2095 0.6197 0.052 Uiso 1 1 calc R . . C46 C -0.00326(14) 0.18242(13) 0.52795(12) 0.0557(8) Uani 1 1 d . . . H46A H -0.0576 0.1882 0.5250 0.067 Uiso 1 1 calc R . . H46B H 0.0145 0.1998 0.4912 0.067 Uiso 1 1 calc R . . C47 C 0.01638(14) 0.11957(12) 0.53355(12) 0.0536(8) Uani 1 1 d . . . H47A H 0.0127 0.1010 0.4924 0.064 Uiso 1 1 calc R . . H47B H -0.0161 0.0989 0.5591 0.064 Uiso 1 1 calc R . . C48 C 0.09570(14) 0.12096(10) 0.56487(11) 0.0431(6) Uani 1 1 d . . . H48A H 0.1081 0.0849 0.5884 0.052 Uiso 1 1 calc R . . H48B H 0.1305 0.1255 0.5340 0.052 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 Si1 0.0170(3) 0.0258(3) 0.0264(3) 0.0081(2) 0.0012(2) -0.0009(2) Si2 0.0172(3) 0.0246(3) 0.0224(3) 0.0005(2) 0.0039(2) 0.0021(2) Si3 0.0178(3) 0.0225(3) 0.0245(3) -0.0033(2) 0.0031(2) 0.0016(2) Si4 0.0159(3) 0.0227(3) 0.0240(3) 0.0015(2) 0.0014(2) -0.0004(2) Si5 0.0298(3) 0.0245(3) 0.0215(3) -0.0034(2) -0.0002(3) 0.0044(3) Si6 0.0289(3) 0.0293(3) 0.0204(3) -0.0030(3) 0.0017(3) 0.0013(3) Si7 0.0289(3) 0.0265(3) 0.0199(3) 0.0036(2) 0.0060(3) 0.0059(3) Si8 0.0265(3) 0.0221(3) 0.0193(3) 0.0005(2) 0.0041(2) 0.0017(3) O1 0.0247(8) 0.0236(8) 0.0258(8) 0.0025(6) -0.0033(6) 0.0014(6) O2 0.0218(8) 0.0239(8) 0.0247(8) -0.0007(6) -0.0036(6) 0.0010(6) N1 0.0159(8) 0.0235(9) 0.0189(9) 0.0029(7) 0.0031(7) 0.0019(7) N2 0.0150(8) 0.0196(9) 0.0188(9) 0.0003(7) 0.0030(7) 0.0000(7) N3 0.0248(9) 0.0272(10) 0.0189(9) -0.0019(7) 0.0002(7) 0.0040(8) N4 0.0223(9) 0.0220(9) 0.0159(9) 0.0016(7) 0.0031(7) -0.0011(7) Ca1 0.0177(2) 0.0220(2) 0.0170(2) 0.00045(16) 0.00149(16) 0.00169(17) Ca2 0.0158(2) 0.0204(2) 0.0178(2) 0.00328(16) 0.00206(16) 0.00087(17) C1 0.0225(12) 0.0243(12) 0.0401(14) 0.0066(10) -0.0001(10) -0.0045(9) C2 0.0296(13) 0.0482(16) 0.0369(14) 0.0186(11) 0.0074(11) -0.0021(11) C3 0.0264(12) 0.0499(16) 0.0301(13) -0.0090(11) 0.0045(10) 0.0063(11) C4 0.0198(11) 0.0286(12) 0.0265(12) 0.0014(9) 0.0034(9) 0.0024(9) C5 0.0297(13) 0.0440(15) 0.0306(13) -0.0092(11) 0.0093(10) 0.0021(11) C6 0.0271(12) 0.0248(12) 0.0464(15) -0.0029(10) 0.0000(11) 0.0036(10) C7 0.0221(12) 0.0361(14) 0.0371(14) -0.0023(10) -0.0008(10) 0.0020(10) C8 0.0267(13) 0.0363(14) 0.0436(14) 0.0105(11) 0.0029(11) -0.0085(11) C9 0.0462(15) 0.0328(13) 0.0296(13) -0.0036(10) -0.0018(11) 0.0123(12) C10 0.0451(15) 0.0303(13) 0.0378(14) -0.0039(11) 0.0048(12) -0.0026(11) C11 0.0385(14) 0.0355(13) 0.0254(12) -0.0059(10) -0.0005(10) 0.0001(11) C12 0.0393(15) 0.0633(18) 0.0278(13) -0.0108(12) 0.0080(11) 0.0008(13) C13 0.0414(14) 0.0373(14) 0.0208(12) 0.0022(10) 0.0067(10) 0.0045(11) C14 0.0332(14) 0.0642(18) 0.0351(14) 0.0064(12) 0.0129(11) -0.0012(13) C15 0.0376(14) 0.0303(13) 0.0330(13) 0.0042(10) 0.0039(11) 0.0073(11) C16 0.0390(15) 0.0281(13) 0.0674(19) -0.0127(12) 0.0045(13) -0.0063(11) C17 0.0488(17) 0.0340(16) 0.092(2) 0.0267(15) -0.0298(16) -0.0065(13) C18 0.0353(13) 0.0273(12) 0.0295(13) 0.0050(10) -0.0015(10) 0.0078(10) C19 0.0303(13) 0.0378(14) 0.0325(13) 0.0009(10) -0.0057(10) 0.0065(11) C20 0.0326(13) 0.0272(12) 0.0258(12) -0.0009(9) -0.0050(10) -0.0012(10) C21 0.0300(13) 0.0276(13) 0.0310(13) -0.0046(10) -0.0006(10) -0.0002(10) C22 0.0390(14) 0.0427(15) 0.0329(14) -0.0054(11) -0.0080(11) -0.0036(12) C23 0.0329(14) 0.0360(14) 0.0542(17) 0.0000(12) -0.0163(12) -0.0004(11) C24 0.0228(11) 0.0289(12) 0.0266(12) 0.0040(9) -0.0009(9) 0.0055(9) Si9 0.0167(3) 0.0243(3) 0.0237(3) -0.0008(2) 0.0034(2) -0.0001(2) Si10 0.0187(3) 0.0215(3) 0.0210(3) 0.0016(2) 0.0019(2) -0.0026(2) Si11 0.0164(3) 0.0217(3) 0.0325(3) -0.0047(3) 0.0051(3) -0.0018(2) Si12 0.0199(3) 0.0232(3) 0.0223(3) -0.0040(2) 0.0057(2) -0.0026(2) Si13 0.0269(3) 0.0283(3) 0.0183(3) -0.0004(2) 0.0020(3) -0.0007(3) Si14 0.0216(3) 0.0220(3) 0.0196(3) -0.0009(2) 0.0033(2) 0.0027(2) Si15 0.0306(4) 0.0279(3) 0.0250(3) -0.0017(3) 0.0000(3) 0.0023(3) Si16 0.0561(5) 0.0236(3) 0.0277(4) 0.0028(3) 0.0171(3) -0.0004(3) O3 0.0276(9) 0.0370(10) 0.0334(9) -0.0021(7) -0.0088(7) 0.0079(7) O4 0.0312(9) 0.0389(9) 0.0251(8) -0.0004(7) -0.0027(7) 0.0039(7) N5 0.0153(8) 0.0219(9) 0.0191(9) -0.0008(7) 0.0024(7) -0.0007(7) N6 0.0149(8) 0.0201(9) 0.0257(9) -0.0037(7) 0.0058(7) -0.0017(7) N7 0.0214(9) 0.0224(9) 0.0197(9) -0.0013(7) 0.0026(7) 0.0012(7) N8 0.0286(10) 0.0239(10) 0.0204(9) 0.0022(7) 0.0041(8) 0.0008(8) Ca3 0.0162(2) 0.0226(2) 0.0191(2) -0.00249(17) 0.00067(16) -0.00015(17) Ca4 0.0206(2) 0.0250(2) 0.0201(2) 0.00416(17) 0.00432(17) 0.00085(18) C25 0.0251(12) 0.0357(13) 0.0342(13) -0.0068(10) 0.0097(10) 0.0023(10) C26 0.0186(11) 0.0365(13) 0.0367(13) -0.0036(10) 0.0010(10) 0.0008(10) C27 0.0333(13) 0.0320(13) 0.0252(12) 0.0031(10) 0.0058(10) -0.0078(10) C28 0.0224(11) 0.0246(11) 0.0276(12) -0.0012(9) 0.0043(9) -0.0036(9) C29 0.0249(12) 0.0279(13) 0.0565(16) 0.0034(11) 0.0082(11) -0.0051(10) C30 0.0213(12) 0.0299(13) 0.0429(14) -0.0045(10) 0.0059(10) 0.0001(10) C31 0.0290(12) 0.0269(12) 0.0351(13) -0.0053(10) 0.0054(10) 0.0022(10) C32 0.0355(14) 0.0392(14) 0.0313(13) -0.0086(10) 0.0141(11) -0.0059(11) C33 0.0537(16) 0.0454(15) 0.0272(13) -0.0013(11) 0.0137(12) 0.0081(13) C34 0.0441(15) 0.0366(14) 0.0335(14) 0.0073(11) 0.0111(12) 0.0006(12) C35 0.0305(13) 0.0278(12) 0.0385(14) -0.0039(10) 0.0112(11) -0.0010(10) C36 0.0327(13) 0.0297(13) 0.0257(12) -0.0016(9) 0.0048(10) 0.0070(10) C37 0.0422(16) 0.0332(14) 0.0623(18) -0.0161(12) -0.0017(13) 0.0004(12) C38 0.0398(15) 0.0397(15) 0.0398(15) 0.0059(11) 0.0028(12) 0.0038(12) C39 0.0607(19) 0.0490(17) 0.0511(17) 0.0154(13) 0.0275(15) 0.0008(14) C40 0.100(2) 0.0549(18) 0.0239(14) -0.0008(12) 0.0137(15) -0.0280(17) C41 0.0488(16) 0.0429(16) 0.0391(15) 0.0068(12) -0.0022(12) 0.0184(13) C42 0.0436(17) 0.062(2) 0.0595(19) 0.0076(15) -0.0061(14) 0.0098(15) C43 0.065(2) 0.103(3) 0.0390(17) -0.0145(17) -0.0198(15) 0.0389(19) C44 0.0329(14) 0.0597(18) 0.0428(16) -0.0119(13) -0.0135(12) 0.0043(13) C45 0.0359(14) 0.0630(18) 0.0282(13) -0.0001(12) -0.0028(11) 0.0155(13) C46 0.0372(16) 0.087(2) 0.0387(16) -0.0036(15) -0.0083(13) 0.0088(15) C47 0.0515(18) 0.068(2) 0.0371(16) -0.0013(14) -0.0080(13) -0.0170(15) C48 0.0517(17) 0.0399(15) 0.0341(14) -0.0041(11) -0.0069(12) -0.0012(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 Si1 N1 1.6991(16) . ? Si1 C1 1.866(2) . ? Si1 C2 1.872(2) . ? Si1 Ca1 3.1022(7) . ? Si1 H1 1.465(18) . ? Si2 N1 1.7088(16) . ? Si2 C3 1.866(2) . ? Si2 C4 1.868(2) . ? Si2 Ca2 3.1685(7) . ? Si2 H2 1.463(18) . ? Si3 N2 1.7067(16) . ? Si3 C6 1.863(2) . ? Si3 C5 1.864(2) . ? Si3 Ca2 3.1341(7) . ? Si3 H3 1.481(18) . ? Si4 N2 1.7049(16) . ? Si4 C8 1.855(2) . ? Si4 C7 1.868(2) . ? Si4 Ca1 3.1064(7) . ? Si4 H4 1.445(18) . ? Si5 N3 1.6790(17) . ? Si5 C10 1.871(2) . ? Si5 C9 1.872(2) . ? Si5 Ca1 3.1811(8) . ? Si5 H5 1.501(18) . ? Si6 N3 1.6791(17) . ? Si6 C12 1.873(2) . ? Si6 C11 1.876(2) . ? Si6 Ca1 3.4784(7) . ? Si6 H6 1.452(18) . ? Si7 N4 1.6770(16) . ? Si7 C14 1.867(2) . ? Si7 C13 1.874(2) . ? Si7 Ca2 3.1739(7) . ? Si7 H7 1.434(18) . ? Si8 N4 1.6830(17) . ? Si8 C16 1.868(2) . ? Si8 C15 1.877(2) . ? Si8 Ca2 3.5629(8) . ? Si8 H8 1.419(18) . ? O1 C17 1.434(3) . ? O1 C20 1.448(2) . ? O1 Ca1 2.3720(13) . ? O2 C21 1.443(2) . ? O2 C24 1.459(2) . ? O2 Ca2 2.3993(13) . ? N1 Ca1 2.4578(16) . ? N1 Ca2 2.5220(16) . ? N2 Ca2 2.4744(15) . ? N2 Ca1 2.4791(15) . ? N3 Ca1 2.3022(16) . ? N4 Ca2 2.3175(16) . ? Ca1 Ca2 3.4507(6) . ? Ca1 H1 2.507(18) . ? Ca1 H4 2.529(18) . ? Ca1 H5 2.777(18) . ? Ca2 H2 2.617(18) . ? Ca2 H3 2.548(18) . ? Ca2 H7 2.764(18) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.506(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.517(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.499(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.501(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.518(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.507(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? Si9 N5 1.7055(16) . ? Si9 C25 1.865(2) . ? Si9 C26 1.872(2) . ? Si9 Ca4 3.1778(7) . ? Si9 H9 1.421(18) . ? Si10 N5 1.7009(16) . ? Si10 C28 1.867(2) . ? Si10 C27 1.870(2) . ? Si10 Ca3 3.0919(7) . ? Si10 H10 1.458(18) . ? Si11 N6 1.7090(16) . ? Si11 C29 1.857(2) . ? Si11 C30 1.866(2) . ? Si11 Ca3 3.0868(7) . ? Si11 H11 1.488(18) . ? Si12 N6 1.7068(16) . ? Si12 C31 1.863(2) . ? Si12 C32 1.865(2) . ? Si12 Ca4 3.1153(7) . ? Si12 H12 1.434(18) . ? Si13 N7 1.6781(16) . ? Si13 C34 1.874(2) . ? Si13 C33 1.877(2) . ? Si13 Ca3 3.5275(7) . ? Si13 H13 1.411(18) . ? Si14 N7 1.6777(17) . ? Si14 C36 1.866(2) . ? Si14 C35 1.872(2) . ? Si14 Ca3 3.1366(7) . ? Si14 H14 1.526(18) . ? Si15 N8 1.6775(17) . ? Si15 C38 1.869(2) . ? Si15 C37 1.873(2) . ? Si15 Ca4 3.5519(8) . ? Si15 H15 1.483(19) . ? Si16 N8 1.6792(17) . ? Si16 C40 1.856(3) . ? Si16 C39 1.863(2) . ? Si16 Ca4 3.1607(7) . ? Si16 H16 1.50(2) . ? O3 C41 1.447(3) . ? O3 C44 1.457(3) . ? O3 Ca3 2.3488(14) . ? O4 C48 1.448(3) . ? O4 C45 1.459(2) . ? O4 Ca4 2.3992(15) . ? N5 Ca3 2.4445(16) . ? N5 Ca4 2.5018(16) . ? N6 Ca3 2.4774(16) . ? N6 Ca4 2.4981(16) . ? N7 Ca3 2.3131(16) . ? N8 Ca4 2.3078(16) . ? Ca3 Ca4 3.4530(6) . ? Ca3 H10 2.496(18) . ? Ca3 H11 2.444(18) . ? Ca3 H14 2.671(18) . ? Ca4 H9 2.655(18) . ? Ca4 H12 2.479(18) . ? Ca4 H16 2.75(2) . ? 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 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 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 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.478(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.473(4) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.496(3) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.520(3) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.499(3) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.509(3) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? 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 Si1 C1 116.71(9) . . ? N1 Si1 C2 115.81(9) . . ? C1 Si1 C2 108.07(10) . . ? N1 Si1 Ca1 52.14(5) . . ? C1 Si1 Ca1 131.38(7) . . ? C2 Si1 Ca1 119.07(8) . . ? N1 Si1 H1 104.7(7) . . ? C1 Si1 H1 106.0(7) . . ? C2 Si1 H1 104.3(7) . . ? Ca1 Si1 H1 52.9(7) . . ? N1 Si2 C3 115.49(9) . . ? N1 Si2 C4 115.14(9) . . ? C3 Si2 C4 107.52(9) . . ? N1 Si2 Ca2 52.45(5) . . ? C3 Si2 Ca2 139.94(7) . . ? C4 Si2 Ca2 111.81(7) . . ? N1 Si2 H2 104.7(7) . . ? C3 Si2 H2 106.5(7) . . ? C4 Si2 H2 106.7(7) . . ? Ca2 Si2 H2 54.9(7) . . ? N2 Si3 C6 115.37(9) . . ? N2 Si3 C5 116.88(9) . . ? C6 Si3 C5 107.19(10) . . ? N2 Si3 Ca2 51.82(5) . . ? C6 Si3 Ca2 132.15(7) . . ? C5 Si3 Ca2 119.55(7) . . ? N2 Si3 H3 104.8(7) . . ? C6 Si3 H3 106.6(7) . . ? C5 Si3 H3 105.0(7) . . ? Ca2 Si3 H3 53.5(7) . . ? N2 Si4 C8 114.93(9) . . ? N2 Si4 C7 116.39(9) . . ? C8 Si4 C7 109.32(10) . . ? N2 Si4 Ca1 52.76(5) . . ? C8 Si4 Ca1 132.04(8) . . ? C7 Si4 Ca1 117.21(7) . . ? N2 Si4 H4 105.6(7) . . ? C8 Si4 H4 106.0(7) . . ? C7 Si4 H4 103.3(7) . . ? Ca1 Si4 H4 53.5(7) . . ? N3 Si5 C10 116.84(10) . . ? N3 Si5 C9 116.76(10) . . ? C10 Si5 C9 105.92(11) . . ? C10 Si5 Ca1 119.08(7) . . ? C9 Si5 Ca1 134.94(8) . . ? N3 Si5 H5 104.3(7) . . ? C10 Si5 H5 105.8(7) . . ? C9 Si5 H5 106.2(7) . . ? Ca1 Si5 H5 60.8(7) . . ? N3 Si6 C12 115.59(10) . . ? N3 Si6 C11 113.79(9) . . ? C12 Si6 C11 106.78(10) . . ? C12 Si6 Ca1 130.45(7) . . ? C11 Si6 Ca1 121.17(7) . . ? N3 Si6 H6 107.2(7) . . ? C12 Si6 H6 105.7(7) . . ? C11 Si6 H6 107.2(7) . . ? Ca1 Si6 H6 72.9(7) . . ? N4 Si7 C14 116.85(10) . . ? N4 Si7 C13 117.09(9) . . ? C14 Si7 C13 104.64(10) . . ? N4 Si7 Ca2 45.09(6) . . ? C14 Si7 Ca2 134.77(8) . . ? C13 Si7 Ca2 120.51(7) . . ? N4 Si7 H7 105.2(7) . . ? C14 Si7 H7 108.3(7) . . ? C13 Si7 H7 103.8(7) . . ? Ca2 Si7 H7 60.4(7) . . ? N4 Si8 C16 114.43(10) . . ? N4 Si8 C15 114.46(9) . . ? C16 Si8 C15 106.61(11) . . ? C16 Si8 Ca2 126.70(8) . . ? C15 Si8 Ca2 124.15(7) . . ? N4 Si8 H8 108.9(7) . . ? C16 Si8 H8 105.9(7) . . ? C15 Si8 H8 105.9(7) . . ? Ca2 Si8 H8 76.8(7) . . ? C17 O1 C20 108.46(15) . . ? C17 O1 Ca1 130.13(13) . . ? C20 O1 Ca1 120.87(11) . . ? C21 O2 C24 108.69(15) . . ? C21 O2 Ca2 133.29(11) . . ? C24 O2 Ca2 118.02(11) . . ? Si1 N1 Si2 121.51(9) . . ? Si1 N1 Ca1 94.78(7) . . ? Si2 N1 Ca1 126.97(8) . . ? Si1 N1 Ca2 129.43(8) . . ? Si2 N1 Ca2 95.05(7) . . ? Ca1 N1 Ca2 87.72(5) . . ? Si4 N2 Si3 121.57(9) . . ? Si4 N2 Ca2 127.81(8) . . ? Si3 N2 Ca2 95.35(7) . . ? Si4 N2 Ca1 94.05(7) . . ? Si3 N2 Ca1 128.58(8) . . ? Ca2 N2 Ca1 88.31(5) . . ? Si5 N3 Si6 133.67(10) . . ? Si5 N3 Ca1 104.99(8) . . ? Si6 N3 Ca1 120.98(9) . . ? Si7 N4 Si8 130.64(10) . . ? Si7 N4 Ca2 104.08(8) . . ? Si8 N4 Ca2 125.15(8) . . ? N3 Ca1 O1 102.86(5) . . ? N3 Ca1 N1 105.85(6) . . ? O1 Ca1 N1 137.92(5) . . ? N3 Ca1 N2 128.20(6) . . ? O1 Ca1 N2 100.25(5) . . ? N1 Ca1 N2 85.44(5) . . ? N3 Ca1 Si1 124.54(5) . . ? O1 Ca1 Si1 104.84(4) . . ? N1 Ca1 Si1 33.08(4) . . ? N2 Ca1 Si1 92.36(4) . . ? N3 Ca1 Si4 103.85(4) . . ? O1 Ca1 Si4 85.85(4) . . ? N1 Ca1 Si4 115.67(4) . . ? N2 Ca1 Si4 33.19(4) . . ? Si1 Ca1 Si4 125.11(2) . . ? N3 Ca1 Si5 30.65(4) . . ? O1 Ca1 Si5 123.64(4) . . ? N1 Ca1 Si5 95.86(4) . . ? N2 Ca1 Si5 99.32(4) . . ? Si1 Ca1 Si5 126.49(2) . . ? Si4 Ca1 Si5 82.794(18) . . ? N3 Ca1 Ca2 108.36(4) . . ? O1 Ca1 Ca2 144.07(4) . . ? N1 Ca1 Ca2 46.91(4) . . ? N2 Ca1 Ca2 45.79(4) . . ? Si1 Ca1 Ca2 71.365(15) . . ? Si4 Ca1 Ca2 69.935(16) . . ? Si5 Ca1 Ca2 80.376(15) . . ? N3 Ca1 Si6 24.45(4) . . ? O1 Ca1 Si6 83.19(4) . . ? N1 Ca1 Si6 113.30(4) . . ? N2 Ca1 Si6 148.10(4) . . ? Si1 Ca1 Si6 117.641(19) . . ? Si4 Ca1 Si6 117.038(19) . . ? Si5 Ca1 Si6 55.023(16) . . ? Ca2 Ca1 Si6 131.121(17) . . ? N3 Ca1 H1 135.9(4) . . ? O1 Ca1 H1 77.3(4) . . ? N1 Ca1 H1 60.7(4) . . ? N2 Ca1 H1 94.1(4) . . ? Si1 Ca1 H1 27.8(4) . . ? Si4 Ca1 H1 120.0(4) . . ? Si5 Ca1 H1 152.0(4) . . ? Ca2 Ca1 H1 91.9(4) . . ? Si6 Ca1 H1 117.4(4) . . ? N3 Ca1 H4 79.5(4) . . ? O1 Ca1 H4 79.2(4) . . ? N1 Ca1 H4 135.8(4) . . ? N2 Ca1 H4 60.3(4) . . ? Si1 Ca1 H4 152.4(4) . . ? Si4 Ca1 H4 27.3(4) . . ? Si5 Ca1 H4 66.2(4) . . ? Ca2 Ca1 H4 89.3(4) . . ? Si6 Ca1 H4 89.8(4) . . ? H1 Ca1 H4 141.1(6) . . ? N3 Ca1 H5 58.4(4) . . ? O1 Ca1 H5 141.8(4) . . ? N1 Ca1 H5 80.1(4) . . ? N2 Ca1 H5 75.0(4) . . ? Si1 Ca1 H5 113.1(4) . . ? Si4 Ca1 H5 69.5(4) . . ? Si5 Ca1 H5 28.1(4) . . ? Ca2 Ca1 H5 52.9(4) . . ? Si6 Ca1 H5 82.9(4) . . ? H1 Ca1 H5 140.2(6) . . ? H4 Ca1 H5 65.4(5) . . ? N4 Ca2 O2 88.38(5) . . ? N4 Ca2 N2 116.90(5) . . ? O2 Ca2 N2 137.63(5) . . ? N4 Ca2 N1 145.04(5) . . ? O2 Ca2 N1 93.41(5) . . ? N2 Ca2 N1 84.18(5) . . ? N4 Ca2 Si3 122.25(4) . . ? O2 Ca2 Si3 105.28(4) . . ? N2 Ca2 Si3 32.83(4) . . ? N1 Ca2 Si3 90.91(4) . . ? N4 Ca2 Si2 114.29(4) . . ? O2 Ca2 Si2 81.06(4) . . ? N2 Ca2 Si2 113.51(4) . . ? N1 Ca2 Si2 32.50(4) . . ? Si3 Ca2 Si2 123.113(19) . . ? N4 Ca2 Si7 30.83(4) . . ? O2 Ca2 Si7 82.45(4) . . ? N2 Ca2 Si7 101.95(4) . . ? N1 Ca2 Si7 173.85(4) . . ? Si3 Ca2 Si7 94.573(18) . . ? Si2 Ca2 Si7 141.67(2) . . ? N4 Ca2 Ca1 131.50(4) . . ? O2 Ca2 Ca1 136.89(4) . . ? N2 Ca2 Ca1 45.90(4) . . ? N1 Ca2 Ca1 45.37(4) . . ? Si3 Ca2 Ca1 70.009(15) . . ? Si2 Ca2 Ca1 68.727(16) . . ? Si7 Ca2 Ca1 139.664(18) . . ? N4 Ca2 Si8 22.72(4) . . ? O2 Ca2 Si8 94.58(3) . . ? N2 Ca2 Si8 122.18(4) . . ? N1 Ca2 Si8 122.66(4) . . ? Si3 Ca2 Si8 140.011(19) . . ? Si2 Ca2 Si8 93.689(17) . . ? Si7 Ca2 Si8 53.522(15) . . ? Ca1 Ca2 Si8 116.691(16) . . ? N4 Ca2 H2 87.2(4) . . ? O2 Ca2 H2 82.1(4) . . ? N2 Ca2 H2 129.2(4) . . ? N1 Ca2 H2 58.6(4) . . ? Si3 Ca2 H2 149.3(4) . . ? Si2 Ca2 H2 27.2(4) . . ? Si7 Ca2 H2 116.1(4) . . ? Ca1 Ca2 H2 84.1(4) . . ? Si8 Ca2 H2 66.5(4) . . ? N4 Ca2 H3 122.3(4) . . ? O2 Ca2 H3 77.4(4) . . ? N2 Ca2 H3 60.4(4) . . ? N1 Ca2 H3 92.0(4) . . ? Si3 Ca2 H3 27.8(4) . . ? Si2 Ca2 H3 118.0(4) . . ? Si7 Ca2 H3 91.5(4) . . ? Ca1 Ca2 H3 90.1(4) . . ? Si8 Ca2 H3 145.0(4) . . ? H2 Ca2 H3 143.0(6) . . ? N4 Ca2 H7 57.5(4) . . ? O2 Ca2 H7 82.7(4) . . ? N2 Ca2 H7 83.8(4) . . ? N1 Ca2 H7 157.3(4) . . ? Si3 Ca2 H7 68.8(4) . . ? Si2 Ca2 H7 162.0(4) . . ? Si7 Ca2 H7 26.8(4) . . ? Ca1 Ca2 H7 129.1(4) . . ? Si8 Ca2 H7 80.0(4) . . ? H2 Ca2 H7 141.8(5) . . ? H3 Ca2 H7 65.3(5) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si2 C3 H3A 109.5 . . ? Si2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si3 C5 H5A 109.5 . . ? Si3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si3 C6 H6A 109.5 . . ? Si3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si4 C7 H7A 109.5 . . ? Si4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si4 C8 H8A 109.5 . . ? Si4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si5 C9 H9A 109.5 . . ? Si5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si5 C10 H10A 109.5 . . ? Si5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si6 C11 H11A 109.5 . . ? Si6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si6 C12 H12A 109.5 . . ? Si6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si7 C13 H13A 109.5 . . ? Si7 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si7 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si7 C14 H14A 109.5 . . ? Si7 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si7 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si8 C15 H15A 109.5 . . ? Si8 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si8 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si8 C16 H16A 109.5 . . ? Si8 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si8 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O1 C17 C18 108.02(19) . . ? O1 C17 H17A 110.1 . . ? C18 C17 H17A 110.1 . . ? O1 C17 H17B 110.1 . . ? C18 C17 H17B 110.1 . . ? H17A C17 H17B 108.4 . . ? C17 C18 C19 103.27(17) . . ? C17 C18 H18A 111.1 . . ? C19 C18 H18A 111.1 . . ? C17 C18 H18B 111.1 . . ? C19 C18 H18B 111.1 . . ? H18A C18 H18B 109.1 . . ? C20 C19 C18 103.00(17) . . ? C20 C19 H19A 111.2 . . ? C18 C19 H19A 111.2 . . ? C20 C19 H19B 111.2 . . ? C18 C19 H19B 111.2 . . ? H19A C19 H19B 109.1 . . ? O1 C20 C19 105.19(16) . . ? O1 C20 H20A 110.7 . . ? C19 C20 H20A 110.7 . . ? O1 C20 H20B 110.7 . . ? C19 C20 H20B 110.7 . . ? H20A C20 H20B 108.8 . . ? O2 C21 C22 105.11(17) . . ? O2 C21 H21A 110.7 . . ? C22 C21 H21A 110.7 . . ? O2 C21 H21B 110.7 . . ? C22 C21 H21B 110.7 . . ? H21A C21 H21B 108.8 . . ? C21 C22 C23 102.33(18) . . ? C21 C22 H22A 111.3 . . ? C23 C22 H22A 111.3 . . ? C21 C22 H22B 111.3 . . ? C23 C22 H22B 111.3 . . ? H22A C22 H22B 109.2 . . ? C24 C23 C22 103.07(18) . . ? C24 C23 H23A 111.1 . . ? C22 C23 H23A 111.1 . . ? C24 C23 H23B 111.1 . . ? C22 C23 H23B 111.1 . . ? H23A C23 H23B 109.1 . . ? O2 C24 C23 106.50(16) . . ? O2 C24 H24A 110.4 . . ? C23 C24 H24A 110.4 . . ? O2 C24 H24B 110.4 . . ? C23 C24 H24B 110.4 . . ? H24A C24 H24B 108.6 . . ? N5 Si9 C25 114.80(9) . . ? N5 Si9 C26 114.68(9) . . ? C25 Si9 C26 108.54(10) . . ? N5 Si9 Ca4 51.50(5) . . ? C25 Si9 Ca4 136.75(7) . . ? C26 Si9 Ca4 114.19(7) . . ? N5 Si9 H9 106.1(7) . . ? C25 Si9 H9 107.4(7) . . ? C26 Si9 H9 104.6(7) . . ? Ca4 Si9 H9 55.9(7) . . ? N5 Si10 C28 115.79(9) . . ? N5 Si10 C27 115.98(9) . . ? C28 Si10 C27 108.75(9) . . ? N5 Si10 Ca3 51.99(5) . . ? C28 Si10 Ca3 133.31(7) . . ? C27 Si10 Ca3 116.68(7) . . ? N5 Si10 H10 104.1(7) . . ? C28 Si10 H10 107.2(7) . . ? C27 Si10 H10 103.9(7) . . ? Ca3 Si10 H10 52.8(7) . . ? N6 Si11 C29 114.46(9) . . ? N6 Si11 C30 116.39(9) . . ? C29 Si11 C30 109.41(10) . . ? N6 Si11 Ca3 53.26(5) . . ? C29 Si11 Ca3 131.35(7) . . ? C30 Si11 Ca3 117.80(7) . . ? N6 Si11 H11 104.1(7) . . ? C29 Si11 H11 109.0(7) . . ? C30 Si11 H11 102.4(7) . . ? Ca3 Si11 H11 51.1(7) . . ? N6 Si12 C31 116.86(9) . . ? N6 Si12 C32 115.96(9) . . ? C31 Si12 C32 107.37(10) . . ? N6 Si12 Ca4 53.15(5) . . ? C31 Si12 Ca4 132.50(7) . . ? C32 Si12 Ca4 118.41(8) . . ? N6 Si12 H12 103.8(7) . . ? C31 Si12 H12 107.2(7) . . ? C32 Si12 H12 104.5(7) . . ? Ca4 Si12 H12 51.1(7) . . ? N7 Si13 C34 108.94(9) . . ? N7 Si13 C33 115.97(9) . . ? C34 Si13 C33 107.20(11) . . ? C34 Si13 Ca3 76.71(7) . . ? C33 Si13 Ca3 135.74(8) . . ? N7 Si13 H13 114.2(7) . . ? C34 Si13 H13 105.1(7) . . ? C33 Si13 H13 104.7(7) . . ? Ca3 Si13 H13 117.0(7) . . ? N7 Si14 C36 116.97(9) . . ? N7 Si14 C35 116.16(9) . . ? C36 Si14 C35 106.45(10) . . ? N7 Si14 Ca3 46.06(6) . . ? C36 Si14 Ca3 134.57(7) . . ? C35 Si14 Ca3 118.78(7) . . ? N7 Si14 H14 103.2(7) . . ? C36 Si14 H14 104.8(7) . . ? C35 Si14 H14 108.3(7) . . ? Ca3 Si14 H14 58.3(7) . . ? N8 Si15 C38 114.65(10) . . ? N8 Si15 C37 114.56(10) . . ? C38 Si15 C37 105.87(11) . . ? C38 Si15 Ca4 127.79(8) . . ? C37 Si15 Ca4 123.66(8) . . ? N8 Si15 H15 111.6(7) . . ? C38 Si15 H15 101.2(7) . . ? C37 Si15 H15 107.9(7) . . ? Ca4 Si15 H15 79.9(7) . . ? N8 Si16 C40 116.39(11) . . ? N8 Si16 C39 116.67(11) . . ? C40 Si16 C39 105.86(12) . . ? N8 Si16 Ca4 45.17(6) . . ? C40 Si16 Ca4 118.28(8) . . ? C39 Si16 Ca4 135.79(9) . . ? N8 Si16 H16 104.8(8) . . ? C40 Si16 H16 104.9(7) . . ? C39 Si16 H16 107.3(8) . . ? Ca4 Si16 H16 60.4(8) . . ? C41 O3 C44 109.06(16) . . ? C41 O3 Ca3 128.82(13) . . ? C44 O3 Ca3 122.09(13) . . ? C48 O4 C45 109.09(16) . . ? C48 O4 Ca4 129.24(13) . . ? C45 O4 Ca4 120.76(13) . . ? Si10 N5 Si9 121.01(9) . . ? Si10 N5 Ca3 94.77(7) . . ? Si9 N5 Ca3 128.90(8) . . ? Si10 N5 Ca4 126.11(8) . . ? Si9 N5 Ca4 96.26(7) . . ? Ca3 N5 Ca4 88.54(5) . . ? Si12 N6 Si11 120.26(9) . . ? Si12 N6 Ca3 132.58(8) . . ? Si11 N6 Ca3 93.18(7) . . ? Si12 N6 Ca4 93.71(7) . . ? Si11 N6 Ca4 129.51(8) . . ? Ca3 N6 Ca4 87.89(5) . . ? Si14 N7 Si13 134.11(10) . . ? Si14 N7 Ca3 102.45(8) . . ? Si13 N7 Ca3 123.44(8) . . ? Si15 N8 Si16 130.90(10) . . ? Si15 N8 Ca4 125.32(9) . . ? Si16 N8 Ca4 103.77(8) . . ? N7 Ca3 O3 98.89(6) . . ? N7 Ca3 N5 109.70(6) . . ? O3 Ca3 N5 136.97(5) . . ? N7 Ca3 N6 133.48(6) . . ? O3 Ca3 N6 98.03(5) . . ? N5 Ca3 N6 85.22(5) . . ? N7 Ca3 Si11 106.97(4) . . ? O3 Ca3 Si11 83.42(4) . . ? N5 Ca3 Si11 116.23(4) . . ? N6 Ca3 Si11 33.56(4) . . ? N7 Ca3 Si10 126.75(4) . . ? O3 Ca3 Si10 103.73(4) . . ? N5 Ca3 Si10 33.24(4) . . ? N6 Ca3 Si10 90.08(4) . . ? Si11 Ca3 Si10 122.94(2) . . ? N7 Ca3 Si14 31.49(4) . . ? O3 Ca3 Si14 118.34(4) . . ? N5 Ca3 Si14 102.16(4) . . ? N6 Ca3 Si14 103.56(4) . . ? Si11 Ca3 Si14 84.317(18) . . ? Si10 Ca3 Si14 132.74(2) . . ? N7 Ca3 Ca4 114.91(4) . . ? O3 Ca3 Ca4 142.15(4) . . ? N5 Ca3 Ca4 46.41(4) . . ? N6 Ca3 Ca4 46.30(4) . . ? Si11 Ca3 Ca4 71.235(16) . . ? Si10 Ca3 Ca4 69.967(15) . . ? Si14 Ca3 Ca4 87.289(16) . . ? N7 Ca3 Si13 23.39(4) . . ? O3 Ca3 Si13 83.01(4) . . ? N5 Ca3 Si13 111.81(4) . . ? N6 Ca3 Si13 153.95(4) . . ? Si11 Ca3 Si13 121.971(19) . . ? Si10 Ca3 Si13 115.093(18) . . ? Si14 Ca3 Si13 54.875(15) . . ? Ca4 Ca3 Si13 134.221(17) . . ? N7 Ca3 H10 136.9(4) . . ? O3 Ca3 H10 76.4(4) . . ? N5 Ca3 H10 60.7(4) . . ? N6 Ca3 H10 89.2(4) . . ? Si11 Ca3 H10 114.8(4) . . ? Si10 Ca3 H10 27.7(4) . . ? Si14 Ca3 H10 158.1(4) . . ? Ca4 Ca3 H10 89.0(4) . . ? Si13 Ca3 H10 116.1(4) . . ? N7 Ca3 H11 81.3(4) . . ? O3 Ca3 H11 75.5(4) . . ? N5 Ca3 H11 138.8(4) . . ? N6 Ca3 H11 61.7(4) . . ? Si11 Ca3 H11 28.3(4) . . ? Si10 Ca3 H11 150.9(4) . . ? Si14 Ca3 H11 66.2(4) . . ? Ca4 Ca3 H11 92.5(4) . . ? Si13 Ca3 H11 93.8(4) . . ? H10 Ca3 H11 135.6(6) . . ? N7 Ca3 H14 60.0(4) . . ? O3 Ca3 H14 136.9(4) . . ? N5 Ca3 H14 85.9(4) . . ? N6 Ca3 H14 78.3(4) . . ? Si11 Ca3 H14 70.0(4) . . ? Si10 Ca3 H14 119.1(4) . . ? Si14 Ca3 H14 29.1(4) . . ? Ca4 Ca3 H14 59.1(4) . . ? Si13 Ca3 H14 83.3(4) . . ? H10 Ca3 H14 145.4(6) . . ? H11 Ca3 H14 64.9(6) . . ? N8 Ca4 O4 91.94(6) . . ? N8 Ca4 N6 112.99(6) . . ? O4 Ca4 N6 139.62(5) . . ? N8 Ca4 N5 141.23(6) . . ? O4 Ca4 N5 96.61(5) . . ? N6 Ca4 N5 83.59(5) . . ? N8 Ca4 Si12 121.01(5) . . ? O4 Ca4 Si12 106.92(4) . . ? N6 Ca4 Si12 33.14(4) . . ? N5 Ca4 Si12 92.43(4) . . ? N8 Ca4 Si16 31.06(4) . . ? O4 Ca4 Si16 81.97(4) . . ? N6 Ca4 Si16 102.92(4) . . ? N5 Ca4 Si16 171.57(4) . . ? Si12 Ca4 Si16 95.95(2) . . ? N8 Ca4 Si9 113.40(4) . . ? O4 Ca4 Si9 81.86(4) . . ? N6 Ca4 Si9 113.28(4) . . ? N5 Ca4 Si9 32.24(4) . . ? Si12 Ca4 Si9 124.17(2) . . ? Si16 Ca4 Si9 139.61(2) . . ? N8 Ca4 Ca3 123.82(4) . . ? O4 Ca4 Ca3 140.21(4) . . ? N6 Ca4 Ca3 45.81(4) . . ? N5 Ca4 Ca3 45.05(4) . . ? Si12 Ca4 Ca3 71.418(15) . . ? Si16 Ca4 Ca3 137.61(2) . . ? Si9 Ca4 Ca3 68.899(16) . . ? N8 Ca4 Si15 22.67(4) . . ? O4 Ca4 Si15 99.44(4) . . ? N6 Ca4 Si15 115.91(4) . . ? N5 Ca4 Si15 118.69(4) . . ? Si12 Ca4 Si15 136.36(2) . . ? Si16 Ca4 Si15 53.727(17) . . ? Si9 Ca4 Si15 93.139(18) . . ? Ca3 Ca4 Si15 108.262(16) . . ? N8 Ca4 H9 87.5(4) . . ? O4 Ca4 H9 77.6(4) . . ? N6 Ca4 H9 132.0(4) . . ? N5 Ca4 H9 58.0(4) . . ? Si12 Ca4 H9 150.4(4) . . ? Si16 Ca4 H9 113.6(4) . . ? Si9 Ca4 H9 26.3(4) . . ? Ca3 Ca4 H9 86.4(4) . . ? Si15 Ca4 H9 68.6(4) . . ? N8 Ca4 H12 123.3(4) . . ? O4 Ca4 H12 80.2(4) . . ? N6 Ca4 H12 59.7(4) . . ? N5 Ca4 H12 95.4(4) . . ? Si12 Ca4 H12 26.7(4) . . ? Si16 Ca4 H12 92.6(4) . . ? Si9 Ca4 H12 120.6(4) . . ? Ca3 Ca4 H12 91.8(4) . . ? Si15 Ca4 H12 145.5(4) . . ? H9 Ca4 H12 142.4(6) . . ? N8 Ca4 H16 59.1(4) . . ? O4 Ca4 H16 80.3(4) . . ? N6 Ca4 H16 85.9(4) . . ? N5 Ca4 H16 159.7(4) . . ? Si12 Ca4 H16 69.6(4) . . ? Si16 Ca4 H16 28.4(4) . . ? Si9 Ca4 H16 160.3(4) . . ? Ca3 Ca4 H16 130.8(4) . . ? Si15 Ca4 H16 81.6(4) . . ? H9 Ca4 H16 138.9(6) . . ? H12 Ca4 H16 64.3(6) . . ? Si9 C25 H25A 109.5 . . ? Si9 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si9 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si9 C26 H26A 109.5 . . ? Si9 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si9 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si10 C27 H27A 109.5 . . ? Si10 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si10 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si10 C28 H28A 109.5 . . ? Si10 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si10 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si11 C29 H29A 109.5 . . ? Si11 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si11 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si11 C30 H30A 109.5 . . ? Si11 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si11 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si12 C31 H31A 109.5 . . ? Si12 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si12 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si12 C32 H32A 109.5 . . ? Si12 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si12 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si13 C33 H33A 109.5 . . ? Si13 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si13 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si13 C34 H34A 109.5 . . ? Si13 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si13 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si14 C35 H35A 109.5 . . ? Si14 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si14 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si14 C36 H36A 109.5 . . ? Si14 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si14 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si15 C37 H37A 109.5 . . ? Si15 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si15 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si15 C38 H38A 109.5 . . ? Si15 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si15 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si16 C39 H39A 109.5 . . ? Si16 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si16 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si16 C40 H40A 109.5 . . ? Si16 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Si16 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O3 C41 C42 107.0(2) . . ? O3 C41 H41A 110.3 . . ? C42 C41 H41A 110.3 . . ? O3 C41 H41B 110.3 . . ? C42 C41 H41B 110.3 . . ? H41A C41 H41B 108.6 . . ? C43 C42 C41 103.4(2) . . ? C43 C42 H42A 111.1 . . ? C41 C42 H42A 111.1 . . ? C43 C42 H42B 111.1 . . ? C41 C42 H42B 111.1 . . ? H42A C42 H42B 109.1 . . ? C42 C43 C44 105.3(2) . . ? C42 C43 H43A 110.7 . . ? C44 C43 H43A 110.7 . . ? C42 C43 H43B 110.7 . . ? C44 C43 H43B 110.7 . . ? H43A C43 H43B 108.8 . . ? O3 C44 C43 103.8(2) . . ? O3 C44 H44A 111.0 . . ? C43 C44 H44A 111.0 . . ? O3 C44 H44B 111.0 . . ? C43 C44 H44B 111.0 . . ? H44A C44 H44B 109.0 . . ? O4 C45 C46 105.60(19) . . ? O4 C45 H45A 110.6 . . ? C46 C45 H45A 110.6 . . ? O4 C45 H45B 110.6 . . ? C46 C45 H45B 110.6 . . ? H45A C45 H45B 108.8 . . ? C47 C46 C45 103.3(2) . . ? C47 C46 H46A 111.1 . . ? C45 C46 H46A 111.1 . . ? C47 C46 H46B 111.1 . . ? C45 C46 H46B 111.1 . . ? H46A C46 H46B 109.1 . . ? C46 C47 C48 102.6(2) . . ? C46 C47 H47A 111.2 . . ? C48 C47 H47A 111.2 . . ? C46 C47 H47B 111.2 . . ? C48 C47 H47B 111.2 . . ? H47A C47 H47B 109.2 . . ? O4 C48 C47 105.4(2) . . ? O4 C48 H48A 110.7 . . ? C47 C48 H48A 110.7 . . ? O4 C48 H48B 110.7 . . ? C47 C48 H48B 110.7 . . ? H48A C48 H48B 108.8 . . ? 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 C1 Si1 N1 Si2 -97.50(12) . . . . ? C2 Si1 N1 Si2 31.47(15) . . . . ? Ca1 Si1 N1 Si2 139.40(13) . . . . ? C1 Si1 N1 Ca1 123.10(8) . . . . ? C2 Si1 N1 Ca1 -107.93(9) . . . . ? C1 Si1 N1 Ca2 32.13(14) . . . . ? C2 Si1 N1 Ca2 161.10(10) . . . . ? Ca1 Si1 N1 Ca2 -90.98(10) . . . . ? C3 Si2 N1 Si1 -82.01(13) . . . . ? C4 Si2 N1 Si1 44.29(14) . . . . ? Ca2 Si2 N1 Si1 143.33(13) . . . . ? C3 Si2 N1 Ca1 43.72(14) . . . . ? C4 Si2 N1 Ca1 170.02(9) . . . . ? Ca2 Si2 N1 Ca1 -90.95(9) . . . . ? C3 Si2 N1 Ca2 134.66(9) . . . . ? C4 Si2 N1 Ca2 -99.03(9) . . . . ? C8 Si4 N2 Si3 -93.94(13) . . . . ? C7 Si4 N2 Si3 35.71(14) . . . . ? Ca1 Si4 N2 Si3 141.01(12) . . . . ? C8 Si4 N2 Ca2 34.04(14) . . . . ? C7 Si4 N2 Ca2 163.69(10) . . . . ? Ca1 Si4 N2 Ca2 -91.01(9) . . . . ? C8 Si4 N2 Ca1 125.05(9) . . . . ? C7 Si4 N2 Ca1 -105.30(9) . . . . ? C6 Si3 N2 Si4 -93.83(12) . . . . ? C5 Si3 N2 Si4 33.54(14) . . . . ? Ca2 Si3 N2 Si4 141.28(13) . . . . ? C6 Si3 N2 Ca2 124.88(8) . . . . ? C5 Si3 N2 Ca2 -107.75(9) . . . . ? C6 Si3 N2 Ca1 32.77(13) . . . . ? C5 Si3 N2 Ca1 160.14(10) . . . . ? Ca2 Si3 N2 Ca1 -92.11(10) . . . . ? C10 Si5 N3 Si6 -67.80(17) . . . . ? C9 Si5 N3 Si6 59.02(17) . . . . ? Ca1 Si5 N3 Si6 -172.97(19) . . . . ? C10 Si5 N3 Ca1 105.16(10) . . . . ? C9 Si5 N3 Ca1 -128.01(9) . . . . ? C12 Si6 N3 Si5 -62.99(18) . . . . ? C11 Si6 N3 Si5 61.14(17) . . . . ? Ca1 Si6 N3 Si5 172.1(2) . . . . ? C12 Si6 N3 Ca1 124.95(11) . . . . ? C11 Si6 N3 Ca1 -110.93(11) . . . . ? C14 Si7 N4 Si8 -48.27(17) . . . . ? C13 Si7 N4 Si8 76.97(15) . . . . ? Ca2 Si7 N4 Si8 -175.85(17) . . . . ? C14 Si7 N4 Ca2 127.58(10) . . . . ? C13 Si7 N4 Ca2 -107.17(10) . . . . ? C16 Si8 N4 Si7 54.35(16) . . . . ? C15 Si8 N4 Si7 -69.12(15) . . . . ? Ca2 Si8 N4 Si7 175.1(2) . . . . ? C16 Si8 N4 Ca2 -120.72(12) . . . . ? C15 Si8 N4 Ca2 115.80(11) . . . . ? Si5 N3 Ca1 O1 -136.83(7) . . . . ? Si6 N3 Ca1 O1 37.24(11) . . . . ? Si5 N3 Ca1 N1 74.28(8) . . . . ? Si6 N3 Ca1 N1 -111.65(10) . . . . ? Si5 N3 Ca1 N2 -22.51(11) . . . . ? Si6 N3 Ca1 N2 151.56(8) . . . . ? Si5 N3 Ca1 Si1 104.74(7) . . . . ? Si6 N3 Ca1 Si1 -81.19(10) . . . . ? Si5 N3 Ca1 Si4 -47.98(8) . . . . ? Si6 N3 Ca1 Si4 126.09(9) . . . . ? Si6 N3 Ca1 Si5 174.07(16) . . . . ? Si5 N3 Ca1 Ca2 25.13(8) . . . . ? Si6 N3 Ca1 Ca2 -160.80(8) . . . . ? Si5 N3 Ca1 Si6 -174.07(16) . . . . ? C17 O1 Ca1 N3 -136.4(2) . . . . ? C20 O1 Ca1 N3 34.14(14) . . . . ? C17 O1 Ca1 N1 -4.3(2) . . . . ? C20 O1 Ca1 N1 166.27(13) . . . . ? C17 O1 Ca1 N2 90.3(2) . . . . ? C20 O1 Ca1 N2 -99.17(14) . . . . ? C17 O1 Ca1 Si1 -5.0(2) . . . . ? C20 O1 Ca1 Si1 165.61(13) . . . . ? C17 O1 Ca1 Si4 120.3(2) . . . . ? C20 O1 Ca1 Si4 -69.13(13) . . . . ? C17 O1 Ca1 Si5 -161.20(19) . . . . ? C20 O1 Ca1 Si5 9.37(15) . . . . ? C17 O1 Ca1 Ca2 73.6(2) . . . . ? C20 O1 Ca1 Ca2 -115.79(13) . . . . ? C17 O1 Ca1 Si6 -121.8(2) . . . . ? C20 O1 Ca1 Si6 48.75(13) . . . . ? Si1 N1 Ca1 N3 130.09(7) . . . . ? Si2 N1 Ca1 N3 -5.92(11) . . . . ? Ca2 N1 Ca1 N3 -100.53(6) . . . . ? Si1 N1 Ca1 O1 -1.18(11) . . . . ? Si2 N1 Ca1 O1 -137.19(9) . . . . ? Ca2 N1 Ca1 O1 128.21(6) . . . . ? Si1 N1 Ca1 N2 -101.42(7) . . . . ? Si2 N1 Ca1 N2 122.56(10) . . . . ? Ca2 N1 Ca1 N2 27.96(5) . . . . ? Si2 N1 Ca1 Si1 -136.01(14) . . . . ? Ca2 N1 Ca1 Si1 129.38(8) . . . . ? Si1 N1 Ca1 Si4 -115.54(6) . . . . ? Si2 N1 Ca1 Si4 108.44(9) . . . . ? Ca2 N1 Ca1 Si4 13.84(5) . . . . ? Si1 N1 Ca1 Si5 159.65(6) . . . . ? Si2 N1 Ca1 Si5 23.64(10) . . . . ? Ca2 N1 Ca1 Si5 -70.96(4) . . . . ? Si1 N1 Ca1 Ca2 -129.38(8) . . . . ? Si2 N1 Ca1 Ca2 94.60(10) . . . . ? Si1 N1 Ca1 Si6 105.33(6) . . . . ? Si2 N1 Ca1 Si6 -30.68(11) . . . . ? Ca2 N1 Ca1 Si6 -125.29(3) . . . . ? Si4 N2 Ca1 N3 -49.71(9) . . . . ? Si3 N2 Ca1 N3 173.58(9) . . . . ? Ca2 N2 Ca1 N3 78.08(7) . . . . ? Si4 N2 Ca1 O1 65.76(7) . . . . ? Si3 N2 Ca1 O1 -70.95(10) . . . . ? Ca2 N2 Ca1 O1 -166.45(5) . . . . ? Si4 N2 Ca1 N1 -156.32(7) . . . . ? Si3 N2 Ca1 N1 66.97(10) . . . . ? Ca2 N2 Ca1 N1 -28.53(5) . . . . ? Si4 N2 Ca1 Si1 171.30(6) . . . . ? Si3 N2 Ca1 Si1 34.59(10) . . . . ? Ca2 N2 Ca1 Si1 -60.91(4) . . . . ? Si3 N2 Ca1 Si4 -136.71(14) . . . . ? Ca2 N2 Ca1 Si4 127.79(8) . . . . ? Si4 N2 Ca1 Si5 -61.12(6) . . . . ? Si3 N2 Ca1 Si5 162.17(9) . . . . ? Ca2 N2 Ca1 Si5 66.67(4) . . . . ? Si4 N2 Ca1 Ca2 -127.79(8) . . . . ? Si3 N2 Ca1 Ca2 95.50(10) . . . . ? Si4 N2 Ca1 Si6 -27.81(11) . . . . ? Si3 N2 Ca1 Si6 -164.52(5) . . . . ? Ca2 N2 Ca1 Si6 99.98(7) . . . . ? N1 Si1 Ca1 N3 -63.30(8) . . . . ? C1 Si1 Ca1 N3 -157.54(10) . . . . ? C2 Si1 Ca1 N3 38.16(10) . . . . ? N1 Si1 Ca1 O1 179.18(8) . . . . ? C1 Si1 Ca1 O1 84.95(10) . . . . ? C2 Si1 Ca1 O1 -79.35(9) . . . . ? C1 Si1 Ca1 N1 -94.24(11) . . . . ? C2 Si1 Ca1 N1 101.46(11) . . . . ? N1 Si1 Ca1 N2 77.94(8) . . . . ? C1 Si1 Ca1 N2 -16.30(10) . . . . ? C2 Si1 Ca1 N2 179.40(9) . . . . ? N1 Si1 Ca1 Si4 83.74(7) . . . . ? C1 Si1 Ca1 Si4 -10.49(9) . . . . ? C2 Si1 Ca1 Si4 -174.79(8) . . . . ? N1 Si1 Ca1 Si5 -25.48(7) . . . . ? C1 Si1 Ca1 Si5 -119.72(9) . . . . ? C2 Si1 Ca1 Si5 75.98(9) . . . . ? N1 Si1 Ca1 Ca2 36.56(7) . . . . ? C1 Si1 Ca1 Ca2 -57.68(9) . . . . ? C2 Si1 Ca1 Ca2 138.02(8) . . . . ? N1 Si1 Ca1 Si6 -90.80(7) . . . . ? C1 Si1 Ca1 Si6 174.96(9) . . . . ? C2 Si1 Ca1 Si6 10.66(9) . . . . ? N2 Si4 Ca1 N3 141.88(8) . . . . ? C8 Si4 Ca1 N3 50.30(11) . . . . ? C7 Si4 Ca1 N3 -114.41(9) . . . . ? N2 Si4 Ca1 O1 -115.89(7) . . . . ? C8 Si4 Ca1 O1 152.53(10) . . . . ? C7 Si4 Ca1 O1 -12.18(8) . . . . ? N2 Si4 Ca1 N1 26.37(8) . . . . ? C8 Si4 Ca1 N1 -65.21(11) . . . . ? C7 Si4 Ca1 N1 130.08(9) . . . . ? C8 Si4 Ca1 N2 -91.58(12) . . . . ? C7 Si4 Ca1 N2 103.71(10) . . . . ? N2 Si4 Ca1 Si1 -10.64(7) . . . . ? C8 Si4 Ca1 Si1 -102.22(10) . . . . ? C7 Si4 Ca1 Si1 93.07(8) . . . . ? N2 Si4 Ca1 Si5 119.43(7) . . . . ? C8 Si4 Ca1 Si5 27.85(10) . . . . ? C7 Si4 Ca1 Si5 -136.86(8) . . . . ? N2 Si4 Ca1 Ca2 37.09(6) . . . . ? C8 Si4 Ca1 Ca2 -54.49(10) . . . . ? C7 Si4 Ca1 Ca2 140.80(8) . . . . ? N2 Si4 Ca1 Si6 163.93(7) . . . . ? C8 Si4 Ca1 Si6 72.35(10) . . . . ? C7 Si4 Ca1 Si6 -92.36(8) . . . . ? C10 Si5 Ca1 N3 -99.80(12) . . . . ? C9 Si5 Ca1 N3 83.64(13) . . . . ? N3 Si5 Ca1 O1 53.24(9) . . . . ? C10 Si5 Ca1 O1 -46.56(10) . . . . ? C9 Si5 Ca1 O1 136.88(11) . . . . ? N3 Si5 Ca1 N1 -111.43(9) . . . . ? C10 Si5 Ca1 N1 148.77(9) . . . . ? C9 Si5 Ca1 N1 -27.79(11) . . . . ? N3 Si5 Ca1 N2 162.25(9) . . . . ? C10 Si5 Ca1 N2 62.45(9) . . . . ? C9 Si5 Ca1 N2 -114.11(11) . . . . ? N3 Si5 Ca1 Si1 -97.78(8) . . . . ? C10 Si5 Ca1 Si1 162.42(8) . . . . ? C9 Si5 Ca1 Si1 -14.14(11) . . . . ? N3 Si5 Ca1 Si4 133.36(8) . . . . ? C10 Si5 Ca1 Si4 33.55(9) . . . . ? C9 Si5 Ca1 Si4 -143.01(10) . . . . ? N3 Si5 Ca1 Ca2 -155.87(8) . . . . ? C10 Si5 Ca1 Ca2 104.33(9) . . . . ? C9 Si5 Ca1 Ca2 -72.23(10) . . . . ? N3 Si5 Ca1 Si6 2.99(8) . . . . ? C10 Si5 Ca1 Si6 -96.81(9) . . . . ? C9 Si5 Ca1 Si6 86.63(10) . . . . ? C12 Si6 Ca1 N3 -76.30(15) . . . . ? C11 Si6 Ca1 N3 87.30(13) . . . . ? N3 Si6 Ca1 O1 -143.54(11) . . . . ? C12 Si6 Ca1 O1 140.16(11) . . . . ? C11 Si6 Ca1 O1 -56.24(9) . . . . ? N3 Si6 Ca1 N1 76.78(11) . . . . ? C12 Si6 Ca1 N1 0.49(12) . . . . ? C11 Si6 Ca1 N1 164.09(9) . . . . ? N3 Si6 Ca1 N2 -45.09(12) . . . . ? C12 Si6 Ca1 N2 -121.38(13) . . . . ? C11 Si6 Ca1 N2 42.22(11) . . . . ? N3 Si6 Ca1 Si1 113.24(10) . . . . ? C12 Si6 Ca1 Si1 36.94(11) . . . . ? C11 Si6 Ca1 Si1 -159.46(8) . . . . ? N3 Si6 Ca1 Si4 -61.75(10) . . . . ? C12 Si6 Ca1 Si4 -138.05(11) . . . . ? C11 Si6 Ca1 Si4 25.55(9) . . . . ? N3 Si6 Ca1 Si5 -3.69(10) . . . . ? C12 Si6 Ca1 Si5 -79.98(11) . . . . ? C11 Si6 Ca1 Si5 83.62(8) . . . . ? N3 Si6 Ca1 Ca2 24.48(10) . . . . ? C12 Si6 Ca1 Ca2 -51.82(11) . . . . ? C11 Si6 Ca1 Ca2 111.78(8) . . . . ? Si7 N4 Ca2 O2 77.93(8) . . . . ? Si8 N4 Ca2 O2 -105.92(10) . . . . ? Si7 N4 Ca2 N2 -66.60(9) . . . . ? Si8 N4 Ca2 N2 109.55(10) . . . . ? Si7 N4 Ca2 N1 171.58(7) . . . . ? Si8 N4 Ca2 N1 -12.27(16) . . . . ? Si7 N4 Ca2 Si3 -29.16(9) . . . . ? Si8 N4 Ca2 Si3 146.99(8) . . . . ? Si7 N4 Ca2 Si2 157.37(6) . . . . ? Si8 N4 Ca2 Si2 -26.48(11) . . . . ? Si8 N4 Ca2 Si7 176.15(16) . . . . ? Si7 N4 Ca2 Ca1 -120.23(6) . . . . ? Si8 N4 Ca2 Ca1 55.93(12) . . . . ? Si7 N4 Ca2 Si8 -176.15(16) . . . . ? C21 O2 Ca2 N4 -140.57(17) . . . . ? C24 O2 Ca2 N4 39.34(13) . . . . ? C21 O2 Ca2 N2 -10.7(2) . . . . ? C24 O2 Ca2 N2 169.18(12) . . . . ? C21 O2 Ca2 N1 74.38(17) . . . . ? C24 O2 Ca2 N1 -105.71(13) . . . . ? C21 O2 Ca2 Si3 -17.49(17) . . . . ? C24 O2 Ca2 Si3 162.41(12) . . . . ? C21 O2 Ca2 Si2 104.53(16) . . . . ? C24 O2 Ca2 Si2 -75.56(12) . . . . ? C21 O2 Ca2 Si7 -110.20(16) . . . . ? C24 O2 Ca2 Si7 69.71(12) . . . . ? C21 O2 Ca2 Ca1 59.40(18) . . . . ? C24 O2 Ca2 Ca1 -120.69(12) . . . . ? C21 O2 Ca2 Si8 -162.44(16) . . . . ? C24 O2 Ca2 Si8 17.46(12) . . . . ? Si4 N2 Ca2 N4 -29.08(12) . . . . ? Si3 N2 Ca2 N4 108.51(7) . . . . ? Ca1 N2 Ca2 N4 -122.90(5) . . . . ? Si4 N2 Ca2 O2 -149.69(8) . . . . ? Si3 N2 Ca2 O2 -12.11(11) . . . . ? Ca1 N2 Ca2 O2 116.49(7) . . . . ? Si4 N2 Ca2 N1 121.62(10) . . . . ? Si3 N2 Ca2 N1 -100.79(7) . . . . ? Ca1 N2 Ca2 N1 27.80(5) . . . . ? Si4 N2 Ca2 Si3 -137.59(14) . . . . ? Ca1 N2 Ca2 Si3 128.60(8) . . . . ? Si4 N2 Ca2 Si2 107.29(9) . . . . ? Si3 N2 Ca2 Si2 -115.13(6) . . . . ? Ca1 N2 Ca2 Si2 13.47(5) . . . . ? Si4 N2 Ca2 Si7 -57.82(10) . . . . ? Si3 N2 Ca2 Si7 79.77(6) . . . . ? Ca1 N2 Ca2 Si7 -151.63(3) . . . . ? Si4 N2 Ca2 Ca1 93.82(10) . . . . ? Si3 N2 Ca2 Ca1 -128.60(8) . . . . ? Si4 N2 Ca2 Si8 -3.61(12) . . . . ? Si3 N2 Ca2 Si8 133.98(5) . . . . ? Ca1 N2 Ca2 Si8 -97.42(4) . . . . ? Si1 N1 Ca2 N4 -163.37(9) . . . . ? Si2 N1 Ca2 N4 -24.61(13) . . . . ? Ca1 N1 Ca2 N4 102.31(9) . . . . ? Si1 N1 Ca2 O2 -71.31(10) . . . . ? Si2 N1 Ca2 O2 67.45(7) . . . . ? Ca1 N1 Ca2 O2 -165.63(5) . . . . ? Si1 N1 Ca2 N2 66.24(10) . . . . ? Si2 N1 Ca2 N2 -155.00(7) . . . . ? Ca1 N1 Ca2 N2 -28.08(5) . . . . ? Si1 N1 Ca2 Si3 34.05(10) . . . . ? Si2 N1 Ca2 Si3 172.81(6) . . . . ? Ca1 N1 Ca2 Si3 -60.26(4) . . . . ? Si1 N1 Ca2 Si2 -138.76(14) . . . . ? Ca1 N1 Ca2 Si2 126.92(8) . . . . ? Si1 N1 Ca2 Ca1 94.31(11) . . . . ? Si2 N1 Ca2 Ca1 -126.92(8) . . . . ? Si1 N1 Ca2 Si8 -168.97(8) . . . . ? Si2 N1 Ca2 Si8 -30.21(8) . . . . ? Ca1 N1 Ca2 Si8 96.71(4) . . . . ? N2 Si3 Ca2 N4 -90.51(8) . . . . ? C6 Si3 Ca2 N4 178.16(10) . . . . ? C5 Si3 Ca2 N4 11.93(10) . . . . ? N2 Si3 Ca2 O2 171.57(7) . . . . ? C6 Si3 Ca2 O2 80.24(10) . . . . ? C5 Si3 Ca2 O2 -85.99(9) . . . . ? C6 Si3 Ca2 N2 -91.34(12) . . . . ? C5 Si3 Ca2 N2 102.43(11) . . . . ? N2 Si3 Ca2 N1 77.79(8) . . . . ? C6 Si3 Ca2 N1 -13.55(10) . . . . ? C5 Si3 Ca2 N1 -179.78(9) . . . . ? N2 Si3 Ca2 Si2 82.39(7) . . . . ? C6 Si3 Ca2 Si2 -8.95(10) . . . . ? C5 Si3 Ca2 Si2 -175.18(8) . . . . ? N2 Si3 Ca2 Si7 -105.01(7) . . . . ? C6 Si3 Ca2 Si7 163.65(10) . . . . ? C5 Si3 Ca2 Si7 -2.58(8) . . . . ? N2 Si3 Ca2 Ca1 36.67(7) . . . . ? C6 Si3 Ca2 Ca1 -54.67(10) . . . . ? C5 Si3 Ca2 Ca1 139.11(8) . . . . ? N2 Si3 Ca2 Si8 -71.39(7) . . . . ? C6 Si3 Ca2 Si8 -162.73(9) . . . . ? C5 Si3 Ca2 Si8 31.04(9) . . . . ? N1 Si2 Ca2 N4 164.82(8) . . . . ? C3 Si2 Ca2 N4 78.88(12) . . . . ? C4 Si2 Ca2 N4 -89.54(8) . . . . ? N1 Si2 Ca2 O2 -111.05(8) . . . . ? C3 Si2 Ca2 O2 163.00(12) . . . . ? C4 Si2 Ca2 O2 -5.41(8) . . . . ? N1 Si2 Ca2 N2 27.29(8) . . . . ? C3 Si2 Ca2 N2 -58.66(12) . . . . ? C4 Si2 Ca2 N2 132.93(8) . . . . ? C3 Si2 Ca2 N1 -85.94(13) . . . . ? C4 Si2 Ca2 N1 105.64(10) . . . . ? N1 Si2 Ca2 Si3 -8.59(7) . . . . ? C3 Si2 Ca2 Si3 -94.53(12) . . . . ? C4 Si2 Ca2 Si3 97.05(7) . . . . ? N1 Si2 Ca2 Si7 -176.64(7) . . . . ? C3 Si2 Ca2 Si7 97.42(12) . . . . ? C4 Si2 Ca2 Si7 -71.00(8) . . . . ? N1 Si2 Ca2 Ca1 37.63(7) . . . . ? C3 Si2 Ca2 Ca1 -48.32(12) . . . . ? C4 Si2 Ca2 Ca1 143.27(7) . . . . ? N1 Si2 Ca2 Si8 154.88(7) . . . . ? C3 Si2 Ca2 Si8 68.94(12) . . . . ? C4 Si2 Ca2 Si8 -99.48(7) . . . . ? C14 Si7 Ca2 N4 -84.81(14) . . . . ? C13 Si7 Ca2 N4 99.15(11) . . . . ? N4 Si7 Ca2 O2 -99.58(8) . . . . ? C14 Si7 Ca2 O2 175.61(12) . . . . ? C13 Si7 Ca2 O2 -0.43(9) . . . . ? N4 Si7 Ca2 N2 123.22(9) . . . . ? C14 Si7 Ca2 N2 38.41(12) . . . . ? C13 Si7 Ca2 N2 -137.63(9) . . . . ? N4 Si7 Ca2 Si3 155.58(8) . . . . ? C14 Si7 Ca2 Si3 70.77(12) . . . . ? C13 Si7 Ca2 Si3 -105.27(8) . . . . ? N4 Si7 Ca2 Si2 -34.44(8) . . . . ? C14 Si7 Ca2 Si2 -119.25(12) . . . . ? C13 Si7 Ca2 Si2 64.71(9) . . . . ? N4 Si7 Ca2 Ca1 91.41(8) . . . . ? C14 Si7 Ca2 Ca1 6.60(12) . . . . ? C13 Si7 Ca2 Ca1 -169.44(8) . . . . ? N4 Si7 Ca2 Si8 1.85(8) . . . . ? C14 Si7 Ca2 Si8 -82.96(11) . . . . ? C13 Si7 Ca2 Si8 101.00(8) . . . . ? N3 Ca1 Ca2 N4 -36.82(7) . . . . ? O1 Ca1 Ca2 N4 112.21(8) . . . . ? N1 Ca1 Ca2 N4 -131.62(7) . . . . ? N2 Ca1 Ca2 N4 89.07(7) . . . . ? Si1 Ca1 Ca2 N4 -158.06(6) . . . . ? Si4 Ca1 Ca2 N4 61.64(6) . . . . ? Si5 Ca1 Ca2 N4 -24.14(6) . . . . ? Si6 Ca1 Ca2 N4 -47.23(6) . . . . ? N3 Ca1 Ca2 O2 116.06(7) . . . . ? O1 Ca1 Ca2 O2 -94.91(8) . . . . ? N1 Ca1 Ca2 O2 21.26(7) . . . . ? N2 Ca1 Ca2 O2 -118.05(7) . . . . ? Si1 Ca1 Ca2 O2 -5.18(5) . . . . ? Si4 Ca1 Ca2 O2 -145.47(5) . . . . ? Si5 Ca1 Ca2 O2 128.74(5) . . . . ? Si6 Ca1 Ca2 O2 105.65(5) . . . . ? N3 Ca1 Ca2 N2 -125.90(7) . . . . ? O1 Ca1 Ca2 N2 23.14(8) . . . . ? N1 Ca1 Ca2 N2 139.31(7) . . . . ? Si1 Ca1 Ca2 N2 112.87(5) . . . . ? Si4 Ca1 Ca2 N2 -27.43(5) . . . . ? Si5 Ca1 Ca2 N2 -113.21(5) . . . . ? Si6 Ca1 Ca2 N2 -136.30(5) . . . . ? N3 Ca1 Ca2 N1 94.80(7) . . . . ? O1 Ca1 Ca2 N1 -116.17(8) . . . . ? N2 Ca1 Ca2 N1 -139.31(7) . . . . ? Si1 Ca1 Ca2 N1 -26.44(5) . . . . ? Si4 Ca1 Ca2 N1 -166.73(5) . . . . ? Si5 Ca1 Ca2 N1 107.48(5) . . . . ? Si6 Ca1 Ca2 N1 84.39(5) . . . . ? N3 Ca1 Ca2 Si3 -152.70(5) . . . . ? O1 Ca1 Ca2 Si3 -3.67(6) . . . . ? N1 Ca1 Ca2 Si3 112.50(5) . . . . ? N2 Ca1 Ca2 Si3 -26.80(5) . . . . ? Si1 Ca1 Ca2 Si3 86.07(2) . . . . ? Si4 Ca1 Ca2 Si3 -54.227(17) . . . . ? Si5 Ca1 Ca2 Si3 -140.011(19) . . . . ? Si6 Ca1 Ca2 Si3 -163.11(2) . . . . ? N3 Ca1 Ca2 Si2 67.36(5) . . . . ? O1 Ca1 Ca2 Si2 -143.61(6) . . . . ? N1 Ca1 Ca2 Si2 -27.44(5) . . . . ? N2 Ca1 Ca2 Si2 -166.75(5) . . . . ? Si1 Ca1 Ca2 Si2 -53.880(18) . . . . ? Si4 Ca1 Ca2 Si2 165.825(19) . . . . ? Si5 Ca1 Ca2 Si2 80.041(18) . . . . ? Si6 Ca1 Ca2 Si2 56.95(2) . . . . ? N3 Ca1 Ca2 Si7 -79.99(5) . . . . ? O1 Ca1 Ca2 Si7 69.04(7) . . . . ? N1 Ca1 Ca2 Si7 -174.79(6) . . . . ? N2 Ca1 Ca2 Si7 45.90(5) . . . . ? Si1 Ca1 Ca2 Si7 158.77(3) . . . . ? Si4 Ca1 Ca2 Si7 18.48(3) . . . . ? Si5 Ca1 Ca2 Si7 -67.31(3) . . . . ? Si6 Ca1 Ca2 Si7 -90.40(3) . . . . ? N3 Ca1 Ca2 Si8 -15.84(5) . . . . ? O1 Ca1 Ca2 Si8 133.19(6) . . . . ? N1 Ca1 Ca2 Si8 -110.64(5) . . . . ? N2 Ca1 Ca2 Si8 110.05(5) . . . . ? Si1 Ca1 Ca2 Si8 -137.08(2) . . . . ? Si4 Ca1 Ca2 Si8 82.629(19) . . . . ? Si5 Ca1 Ca2 Si8 -3.16(2) . . . . ? Si6 Ca1 Ca2 Si8 -26.25(3) . . . . ? C16 Si8 Ca2 N4 77.47(14) . . . . ? C15 Si8 Ca2 N4 -82.00(13) . . . . ? N4 Si8 Ca2 O2 74.66(11) . . . . ? C16 Si8 Ca2 O2 152.13(11) . . . . ? C15 Si8 Ca2 O2 -7.34(9) . . . . ? N4 Si8 Ca2 N2 -83.18(11) . . . . ? C16 Si8 Ca2 N2 -5.71(11) . . . . ? C15 Si8 Ca2 N2 -165.18(9) . . . . ? N4 Si8 Ca2 N1 171.68(11) . . . . ? C16 Si8 Ca2 N1 -110.85(11) . . . . ? C15 Si8 Ca2 N1 89.68(10) . . . . ? N4 Si8 Ca2 Si3 -45.80(11) . . . . ? C16 Si8 Ca2 Si3 31.67(11) . . . . ? C15 Si8 Ca2 Si3 -127.80(9) . . . . ? N4 Si8 Ca2 Si2 155.97(10) . . . . ? C16 Si8 Ca2 Si2 -126.56(10) . . . . ? C15 Si8 Ca2 Si2 73.97(9) . . . . ? N4 Si8 Ca2 Si7 -2.45(10) . . . . ? C16 Si8 Ca2 Si7 75.02(10) . . . . ? C15 Si8 Ca2 Si7 -84.45(9) . . . . ? N4 Si8 Ca2 Ca1 -136.03(10) . . . . ? C16 Si8 Ca2 Ca1 -58.56(10) . . . . ? C15 Si8 Ca2 Ca1 141.97(9) . . . . ? C20 O1 C17 C18 3.7(3) . . . . ? Ca1 O1 C17 C18 175.21(13) . . . . ? O1 C17 C18 C19 17.7(3) . . . . ? C17 C18 C19 C20 -31.4(2) . . . . ? C17 O1 C20 C19 -24.1(2) . . . . ? Ca1 O1 C20 C19 163.48(13) . . . . ? C18 C19 C20 O1 34.4(2) . . . . ? C24 O2 C21 C22 -22.6(2) . . . . ? Ca2 O2 C21 C22 157.31(14) . . . . ? O2 C21 C22 C23 36.3(2) . . . . ? C21 C22 C23 C24 -35.8(2) . . . . ? C21 O2 C24 C23 -0.5(2) . . . . ? Ca2 O2 C24 C23 179.57(14) . . . . ? C22 C23 C24 O2 22.9(2) . . . . ? C28 Si10 N5 Si9 92.15(12) . . . . ? C27 Si10 N5 Si9 -37.08(14) . . . . ? Ca3 Si10 N5 Si9 -141.75(13) . . . . ? C28 Si10 N5 Ca3 -126.10(8) . . . . ? C27 Si10 N5 Ca3 104.66(9) . . . . ? C28 Si10 N5 Ca4 -34.43(13) . . . . ? C27 Si10 N5 Ca4 -163.67(9) . . . . ? Ca3 Si10 N5 Ca4 91.67(9) . . . . ? C25 Si9 N5 Si10 89.61(12) . . . . ? C26 Si9 N5 Si10 -37.10(14) . . . . ? Ca4 Si9 N5 Si10 -139.26(13) . . . . ? C25 Si9 N5 Ca3 -37.94(14) . . . . ? C26 Si9 N5 Ca3 -164.66(10) . . . . ? Ca4 Si9 N5 Ca3 93.18(10) . . . . ? C25 Si9 N5 Ca4 -131.12(8) . . . . ? C26 Si9 N5 Ca4 102.16(9) . . . . ? C31 Si12 N6 Si11 94.59(12) . . . . ? C32 Si12 N6 Si11 -33.65(15) . . . . ? Ca4 Si12 N6 Si11 -140.89(13) . . . . ? C31 Si12 N6 Ca3 -33.98(15) . . . . ? C32 Si12 N6 Ca3 -162.21(11) . . . . ? Ca4 Si12 N6 Ca3 90.54(10) . . . . ? C31 Si12 N6 Ca4 -124.52(8) . . . . ? C32 Si12 N6 Ca4 107.24(9) . . . . ? C29 Si11 N6 Si12 90.74(13) . . . . ? C30 Si11 N6 Si12 -38.56(15) . . . . ? Ca3 Si11 N6 Si12 -144.78(13) . . . . ? C29 Si11 N6 Ca3 -124.48(9) . . . . ? C30 Si11 N6 Ca3 106.22(9) . . . . ? C29 Si11 N6 Ca4 -34.59(14) . . . . ? C30 Si11 N6 Ca4 -163.88(10) . . . . ? Ca3 Si11 N6 Ca4 89.89(10) . . . . ? C36 Si14 N7 Si13 -53.58(17) . . . . ? C35 Si14 N7 Si13 73.58(16) . . . . ? Ca3 Si14 N7 Si13 179.33(18) . . . . ? C36 Si14 N7 Ca3 127.09(9) . . . . ? C35 Si14 N7 Ca3 -105.75(9) . . . . ? C34 Si13 N7 Si14 166.48(13) . . . . ? C33 Si13 N7 Si14 45.49(18) . . . . ? Ca3 Si13 N7 Si14 -179.2(2) . . . . ? C34 Si13 N7 Ca3 -14.30(13) . . . . ? C33 Si13 N7 Ca3 -135.29(11) . . . . ? C38 Si15 N8 Si16 58.83(17) . . . . ? C37 Si15 N8 Si16 -63.88(17) . . . . ? Ca4 Si15 N8 Si16 -178.6(2) . . . . ? C38 Si15 N8 Ca4 -122.54(11) . . . . ? C37 Si15 N8 Ca4 114.75(13) . . . . ? C40 Si16 N8 Si15 -76.52(17) . . . . ? C39 Si16 N8 Si15 49.68(18) . . . . ? Ca4 Si16 N8 Si15 178.85(18) . . . . ? C40 Si16 N8 Ca4 104.63(11) . . . . ? C39 Si16 N8 Ca4 -129.17(10) . . . . ? Si14 N7 Ca3 O3 131.64(7) . . . . ? Si13 N7 Ca3 O3 -47.78(11) . . . . ? Si14 N7 Ca3 N5 -81.01(8) . . . . ? Si13 N7 Ca3 N5 99.56(10) . . . . ? Si14 N7 Ca3 N6 21.57(11) . . . . ? Si13 N7 Ca3 N6 -157.86(8) . . . . ? Si14 N7 Ca3 Si11 45.87(8) . . . . ? Si13 N7 Ca3 Si11 -133.56(9) . . . . ? Si14 N7 Ca3 Si10 -113.73(6) . . . . ? Si13 N7 Ca3 Si10 66.84(11) . . . . ? Si13 N7 Ca3 Si14 -179.43(16) . . . . ? Si14 N7 Ca3 Ca4 -30.89(8) . . . . ? Si13 N7 Ca3 Ca4 149.69(8) . . . . ? Si14 N7 Ca3 Si13 179.43(16) . . . . ? C41 O3 Ca3 N7 146.11(17) . . . . ? C44 O3 Ca3 N7 -31.62(17) . . . . ? C41 O3 Ca3 N5 14.2(2) . . . . ? C44 O3 Ca3 N5 -163.50(15) . . . . ? C41 O3 Ca3 N6 -77.38(18) . . . . ? C44 O3 Ca3 N6 104.89(16) . . . . ? C41 O3 Ca3 Si11 -107.68(17) . . . . ? C44 O3 Ca3 Si11 74.60(16) . . . . ? C41 O3 Ca3 Si10 14.68(18) . . . . ? C44 O3 Ca3 Si10 -163.04(15) . . . . ? C41 O3 Ca3 Si14 172.43(16) . . . . ? C44 O3 Ca3 Si14 -5.29(17) . . . . ? C41 O3 Ca3 Ca4 -60.2(2) . . . . ? C44 O3 Ca3 Ca4 122.05(15) . . . . ? C41 O3 Ca3 Si13 128.88(17) . . . . ? C44 O3 Ca3 Si13 -48.85(16) . . . . ? Si10 N5 Ca3 N7 -127.81(7) . . . . ? Si9 N5 Ca3 N7 9.21(12) . . . . ? Ca4 N5 Ca3 N7 106.07(6) . . . . ? Si10 N5 Ca3 O3 0.82(11) . . . . ? Si9 N5 Ca3 O3 137.83(10) . . . . ? Ca4 N5 Ca3 O3 -125.30(7) . . . . ? Si10 N5 Ca3 N6 97.48(7) . . . . ? Si9 N5 Ca3 N6 -125.51(11) . . . . ? Ca4 N5 Ca3 N6 -28.64(5) . . . . ? Si10 N5 Ca3 Si11 110.73(6) . . . . ? Si9 N5 Ca3 Si11 -112.26(9) . . . . ? Ca4 N5 Ca3 Si11 -15.39(6) . . . . ? Si9 N5 Ca3 Si10 137.02(14) . . . . ? Ca4 N5 Ca3 Si10 -126.12(8) . . . . ? Si10 N5 Ca3 Si14 -159.66(5) . . . . ? Si9 N5 Ca3 Si14 -22.64(11) . . . . ? Ca4 N5 Ca3 Si14 74.22(4) . . . . ? Si10 N5 Ca3 Ca4 126.12(8) . . . . ? Si9 N5 Ca3 Ca4 -96.86(11) . . . . ? Si10 N5 Ca3 Si13 -102.87(6) . . . . ? Si9 N5 Ca3 Si13 34.15(11) . . . . ? Ca4 N5 Ca3 Si13 131.01(3) . . . . ? Si12 N6 Ca3 N7 -177.17(9) . . . . ? Si11 N6 Ca3 N7 45.40(10) . . . . ? Ca4 N6 Ca3 N7 -84.07(8) . . . . ? Si12 N6 Ca3 O3 72.41(12) . . . . ? Si11 N6 Ca3 O3 -65.03(7) . . . . ? Ca4 N6 Ca3 O3 165.51(5) . . . . ? Si12 N6 Ca3 N5 -64.40(11) . . . . ? Si11 N6 Ca3 N5 158.16(7) . . . . ? Ca4 N6 Ca3 N5 28.70(5) . . . . ? Si12 N6 Ca3 Si11 137.44(15) . . . . ? Ca4 N6 Ca3 Si11 -129.46(8) . . . . ? Si12 N6 Ca3 Si10 -31.47(11) . . . . ? Si11 N6 Ca3 Si10 -168.91(6) . . . . ? Ca4 N6 Ca3 Si10 61.63(4) . . . . ? Si12 N6 Ca3 Si14 -165.78(10) . . . . ? Si11 N6 Ca3 Si14 56.79(6) . . . . ? Ca4 N6 Ca3 Si14 -72.68(4) . . . . ? Si12 N6 Ca3 Ca4 -93.10(11) . . . . ? Si11 N6 Ca3 Ca4 129.46(8) . . . . ? Si12 N6 Ca3 Si13 162.92(6) . . . . ? Si11 N6 Ca3 Si13 25.48(13) . . . . ? Ca4 N6 Ca3 Si13 -103.99(8) . . . . ? N6 Si11 Ca3 N7 -147.31(8) . . . . ? C29 Si11 Ca3 N7 -55.51(11) . . . . ? C30 Si11 Ca3 N7 109.19(9) . . . . ? N6 Si11 Ca3 O3 115.37(8) . . . . ? C29 Si11 Ca3 O3 -152.84(11) . . . . ? C30 Si11 Ca3 O3 11.87(9) . . . . ? N6 Si11 Ca3 N5 -24.41(8) . . . . ? C29 Si11 Ca3 N5 67.39(11) . . . . ? C30 Si11 Ca3 N5 -127.91(9) . . . . ? C29 Si11 Ca3 N6 91.80(12) . . . . ? C30 Si11 Ca3 N6 -103.50(10) . . . . ? N6 Si11 Ca3 Si10 13.25(7) . . . . ? C29 Si11 Ca3 Si10 105.05(10) . . . . ? C30 Si11 Ca3 Si10 -90.25(8) . . . . ? N6 Si11 Ca3 Si14 -125.18(7) . . . . ? C29 Si11 Ca3 Si14 -33.38(10) . . . . ? C30 Si11 Ca3 Si14 131.32(8) . . . . ? N6 Si11 Ca3 Ca4 -36.12(7) . . . . ? C29 Si11 Ca3 Ca4 55.68(10) . . . . ? C30 Si11 Ca3 Ca4 -139.62(8) . . . . ? N6 Si11 Ca3 Si13 -167.13(7) . . . . ? C29 Si11 Ca3 Si13 -75.34(10) . . . . ? C30 Si11 Ca3 Si13 89.37(8) . . . . ? N5 Si10 Ca3 N7 68.18(8) . . . . ? C28 Si10 Ca3 N7 159.45(10) . . . . ? C27 Si10 Ca3 N7 -35.08(10) . . . . ? N5 Si10 Ca3 O3 -179.42(8) . . . . ? C28 Si10 Ca3 O3 -88.15(10) . . . . ? C27 Si10 Ca3 O3 77.32(9) . . . . ? C28 Si10 Ca3 N5 91.27(11) . . . . ? C27 Si10 Ca3 N5 -103.26(10) . . . . ? N5 Si10 Ca3 N6 -81.13(8) . . . . ? C28 Si10 Ca3 N6 10.14(10) . . . . ? C27 Si10 Ca3 N6 175.61(9) . . . . ? N5 Si10 Ca3 Si11 -88.41(7) . . . . ? C28 Si10 Ca3 Si11 2.86(10) . . . . ? C27 Si10 Ca3 Si11 168.33(8) . . . . ? N5 Si10 Ca3 Si14 27.56(7) . . . . ? C28 Si10 Ca3 Si14 118.83(9) . . . . ? C27 Si10 Ca3 Si14 -75.70(8) . . . . ? N5 Si10 Ca3 Ca4 -38.52(7) . . . . ? C28 Si10 Ca3 Ca4 52.75(9) . . . . ? C27 Si10 Ca3 Ca4 -141.78(8) . . . . ? N5 Si10 Ca3 Si13 91.94(7) . . . . ? C28 Si10 Ca3 Si13 -176.78(9) . . . . ? C27 Si10 Ca3 Si13 -11.31(8) . . . . ? C36 Si14 Ca3 N7 -86.27(12) . . . . ? C35 Si14 Ca3 N7 99.75(11) . . . . ? N7 Si14 Ca3 O3 -57.02(9) . . . . ? C36 Si14 Ca3 O3 -143.29(10) . . . . ? C35 Si14 Ca3 O3 42.73(9) . . . . ? N7 Si14 Ca3 N5 107.97(9) . . . . ? C36 Si14 Ca3 N5 21.70(10) . . . . ? C35 Si14 Ca3 N5 -152.29(9) . . . . ? N7 Si14 Ca3 N6 -164.08(9) . . . . ? C36 Si14 Ca3 N6 109.65(10) . . . . ? C35 Si14 Ca3 N6 -64.33(9) . . . . ? N7 Si14 Ca3 Si11 -136.38(8) . . . . ? C36 Si14 Ca3 Si11 137.35(10) . . . . ? C35 Si14 Ca3 Si11 -36.64(8) . . . . ? N7 Si14 Ca3 Si10 92.93(8) . . . . ? C36 Si14 Ca3 Si10 6.66(10) . . . . ? C35 Si14 Ca3 Si10 -167.33(8) . . . . ? N7 Si14 Ca3 Ca4 152.22(8) . . . . ? C36 Si14 Ca3 Ca4 65.95(10) . . . . ? C35 Si14 Ca3 Ca4 -108.04(8) . . . . ? N7 Si14 Ca3 Si13 -0.28(8) . . . . ? C36 Si14 Ca3 Si13 -86.55(10) . . . . ? C35 Si14 Ca3 Si13 99.47(8) . . . . ? C34 Si13 Ca3 N7 166.11(13) . . . . ? C33 Si13 Ca3 N7 64.98(15) . . . . ? N7 Si13 Ca3 O3 132.51(11) . . . . ? C34 Si13 Ca3 O3 -61.38(8) . . . . ? C33 Si13 Ca3 O3 -162.51(12) . . . . ? N7 Si13 Ca3 N5 -89.40(11) . . . . ? C34 Si13 Ca3 N5 76.71(9) . . . . ? C33 Si13 Ca3 N5 -24.42(12) . . . . ? N7 Si13 Ca3 N6 38.51(14) . . . . ? C34 Si13 Ca3 N6 -155.38(12) . . . . ? C33 Si13 Ca3 N6 103.49(14) . . . . ? N7 Si13 Ca3 Si11 54.79(10) . . . . ? C34 Si13 Ca3 Si11 -139.10(8) . . . . ? C33 Si13 Ca3 Si11 119.77(11) . . . . ? N7 Si13 Ca3 Si10 -125.57(10) . . . . ? C34 Si13 Ca3 Si10 40.54(8) . . . . ? C33 Si13 Ca3 Si10 -60.58(11) . . . . ? N7 Si13 Ca3 Si14 0.37(10) . . . . ? C34 Si13 Ca3 Si14 166.47(8) . . . . ? C33 Si13 Ca3 Si14 65.35(11) . . . . ? N7 Si13 Ca3 Ca4 -39.70(10) . . . . ? C34 Si13 Ca3 Ca4 126.41(8) . . . . ? C33 Si13 Ca3 Ca4 25.28(12) . . . . ? Si15 N8 Ca4 O4 110.17(11) . . . . ? Si16 N8 Ca4 O4 -70.90(8) . . . . ? Si15 N8 Ca4 N6 -102.45(11) . . . . ? Si16 N8 Ca4 N6 76.48(9) . . . . ? Si15 N8 Ca4 N5 7.11(17) . . . . ? Si16 N8 Ca4 N5 -173.96(7) . . . . ? Si15 N8 Ca4 Si12 -138.73(9) . . . . ? Si16 N8 Ca4 Si12 40.21(9) . . . . ? Si15 N8 Ca4 Si16 -178.93(17) . . . . ? Si15 N8 Ca4 Si9 28.20(12) . . . . ? Si16 N8 Ca4 Si9 -152.87(6) . . . . ? Si15 N8 Ca4 Ca3 -51.30(12) . . . . ? Si16 N8 Ca4 Ca3 127.64(6) . . . . ? Si16 N8 Ca4 Si15 178.93(17) . . . . ? C48 O4 Ca4 N8 122.54(18) . . . . ? C45 O4 Ca4 N8 -45.28(15) . . . . ? C48 O4 Ca4 N6 -7.5(2) . . . . ? C45 O4 Ca4 N6 -175.30(14) . . . . ? C48 O4 Ca4 N5 -95.35(18) . . . . ? C45 O4 Ca4 N5 96.84(15) . . . . ? C48 O4 Ca4 Si12 -0.77(18) . . . . ? C45 O4 Ca4 Si12 -168.59(14) . . . . ? C48 O4 Ca4 Si16 93.04(17) . . . . ? C45 O4 Ca4 Si16 -74.78(15) . . . . ? C48 O4 Ca4 Si9 -124.10(17) . . . . ? C45 O4 Ca4 Si9 68.08(15) . . . . ? C48 O4 Ca4 Ca3 -81.84(18) . . . . ? C45 O4 Ca4 Ca3 110.34(15) . . . . ? C48 O4 Ca4 Si15 144.05(17) . . . . ? C45 O4 Ca4 Si15 -23.77(15) . . . . ? Si12 N6 Ca4 N8 -111.95(7) . . . . ? Si11 N6 Ca4 N8 23.12(12) . . . . ? Ca3 N6 Ca4 N8 115.51(6) . . . . ? Si12 N6 Ca4 O4 11.80(11) . . . . ? Si11 N6 Ca4 O4 146.87(9) . . . . ? Ca3 N6 Ca4 O4 -120.74(7) . . . . ? Si12 N6 Ca4 N5 104.47(7) . . . . ? Si11 N6 Ca4 N5 -120.46(11) . . . . ? Ca3 N6 Ca4 N5 -28.07(5) . . . . ? Si11 N6 Ca4 Si12 135.07(14) . . . . ? Ca3 N6 Ca4 Si12 -132.54(8) . . . . ? Si12 N6 Ca4 Si16 -80.97(6) . . . . ? Si11 N6 Ca4 Si16 54.10(11) . . . . ? Ca3 N6 Ca4 Si16 146.49(3) . . . . ? Si12 N6 Ca4 Si9 117.34(6) . . . . ? Si11 N6 Ca4 Si9 -107.59(10) . . . . ? Ca3 N6 Ca4 Si9 -15.20(5) . . . . ? Si12 N6 Ca4 Ca3 132.54(8) . . . . ? Si11 N6 Ca4 Ca3 -92.39(11) . . . . ? Si12 N6 Ca4 Si15 -136.68(5) . . . . ? Si11 N6 Ca4 Si15 -1.61(12) . . . . ? Ca3 N6 Ca4 Si15 90.78(4) . . . . ? Si10 N5 Ca4 N8 174.43(9) . . . . ? Si9 N5 Ca4 N8 38.25(12) . . . . ? Ca3 N5 Ca4 N8 -90.74(9) . . . . ? Si10 N5 Ca4 O4 72.98(10) . . . . ? Si9 N5 Ca4 O4 -63.21(7) . . . . ? Ca3 N5 Ca4 O4 167.81(5) . . . . ? Si10 N5 Ca4 N6 -66.37(10) . . . . ? Si9 N5 Ca4 N6 157.45(7) . . . . ? Ca3 N5 Ca4 N6 28.47(5) . . . . ? Si10 N5 Ca4 Si12 -34.37(9) . . . . ? Si9 N5 Ca4 Si12 -170.55(6) . . . . ? Ca3 N5 Ca4 Si12 60.47(4) . . . . ? Si10 N5 Ca4 Si9 136.18(14) . . . . ? Ca3 N5 Ca4 Si9 -128.98(8) . . . . ? Si10 N5 Ca4 Ca3 -94.84(10) . . . . ? Si9 N5 Ca4 Ca3 128.98(8) . . . . ? Si10 N5 Ca4 Si15 177.54(7) . . . . ? Si9 N5 Ca4 Si15 41.36(7) . . . . ? Ca3 N5 Ca4 Si15 -87.62(4) . . . . ? N6 Si12 Ca4 N8 85.01(8) . . . . ? C31 Si12 Ca4 N8 179.55(10) . . . . ? C32 Si12 Ca4 N8 -17.50(10) . . . . ? N6 Si12 Ca4 O4 -172.04(8) . . . . ? C31 Si12 Ca4 O4 -77.50(10) . . . . ? C32 Si12 Ca4 O4 85.45(9) . . . . ? C31 Si12 Ca4 N6 94.54(12) . . . . ? C32 Si12 Ca4 N6 -102.51(11) . . . . ? N6 Si12 Ca4 N5 -74.39(8) . . . . ? C31 Si12 Ca4 N5 20.15(10) . . . . ? C32 Si12 Ca4 N5 -176.90(9) . . . . ? N6 Si12 Ca4 Si16 104.57(7) . . . . ? C31 Si12 Ca4 Si16 -160.89(9) . . . . ? C32 Si12 Ca4 Si16 2.06(8) . . . . ? N6 Si12 Ca4 Si9 -80.46(7) . . . . ? C31 Si12 Ca4 Si9 14.08(10) . . . . ? C32 Si12 Ca4 Si9 177.03(8) . . . . ? N6 Si12 Ca4 Ca3 -33.87(7) . . . . ? C31 Si12 Ca4 Ca3 60.67(9) . . . . ? C32 Si12 Ca4 Ca3 -136.38(8) . . . . ? N6 Si12 Ca4 Si15 63.40(7) . . . . ? C31 Si12 Ca4 Si15 157.93(9) . . . . ? C32 Si12 Ca4 Si15 -39.11(9) . . . . ? C40 Si16 Ca4 N8 -100.18(14) . . . . ? C39 Si16 Ca4 N8 83.45(14) . . . . ? N8 Si16 Ca4 O4 107.49(9) . . . . ? C40 Si16 Ca4 O4 7.31(11) . . . . ? C39 Si16 Ca4 O4 -169.07(13) . . . . ? N8 Si16 Ca4 N6 -113.32(9) . . . . ? C40 Si16 Ca4 N6 146.49(11) . . . . ? C39 Si16 Ca4 N6 -29.88(13) . . . . ? N8 Si16 Ca4 Si12 -146.20(8) . . . . ? C40 Si16 Ca4 Si12 113.61(11) . . . . ? C39 Si16 Ca4 Si12 -62.76(12) . . . . ? N8 Si16 Ca4 Si9 40.23(9) . . . . ? C40 Si16 Ca4 Si9 -59.95(11) . . . . ? C39 Si16 Ca4 Si9 123.68(12) . . . . ? N8 Si16 Ca4 Ca3 -77.37(9) . . . . ? C40 Si16 Ca4 Ca3 -177.55(10) . . . . ? C39 Si16 Ca4 Ca3 6.07(13) . . . . ? N8 Si16 Ca4 Si15 -0.51(8) . . . . ? C40 Si16 Ca4 Si15 -100.69(11) . . . . ? C39 Si16 Ca4 Si15 82.94(12) . . . . ? N5 Si9 Ca4 N8 -155.02(8) . . . . ? C25 Si9 Ca4 N8 -68.65(12) . . . . ? C26 Si9 Ca4 N8 101.83(9) . . . . ? N5 Si9 Ca4 O4 116.40(8) . . . . ? C25 Si9 Ca4 O4 -157.23(11) . . . . ? C26 Si9 Ca4 O4 13.24(8) . . . . ? N5 Si9 Ca4 N6 -24.51(8) . . . . ? C25 Si9 Ca4 N6 61.86(11) . . . . ? C26 Si9 Ca4 N6 -127.67(9) . . . . ? C25 Si9 Ca4 N5 86.37(12) . . . . ? C26 Si9 Ca4 N5 -103.16(10) . . . . ? N5 Si9 Ca4 Si12 11.43(7) . . . . ? C25 Si9 Ca4 Si12 97.80(11) . . . . ? C26 Si9 Ca4 Si12 -91.72(8) . . . . ? N5 Si9 Ca4 Si16 -176.31(7) . . . . ? C25 Si9 Ca4 Si16 -89.94(11) . . . . ? C26 Si9 Ca4 Si16 80.53(8) . . . . ? N5 Si9 Ca4 Ca3 -36.13(7) . . . . ? C25 Si9 Ca4 Ca3 50.23(10) . . . . ? C26 Si9 Ca4 Ca3 -139.29(8) . . . . ? N5 Si9 Ca4 Si15 -144.51(7) . . . . ? C25 Si9 Ca4 Si15 -58.14(11) . . . . ? C26 Si9 Ca4 Si15 112.33(8) . . . . ? N7 Ca3 Ca4 N8 37.02(7) . . . . ? O3 Ca3 Ca4 N8 -114.08(8) . . . . ? N5 Ca3 Ca4 N8 131.10(7) . . . . ? N6 Ca3 Ca4 N8 -90.26(7) . . . . ? Si11 Ca3 Ca4 N8 -63.47(5) . . . . ? Si10 Ca3 Ca4 N8 159.22(5) . . . . ? Si14 Ca3 Ca4 N8 21.45(5) . . . . ? Si13 Ca3 Ca4 N8 53.26(6) . . . . ? N7 Ca3 Ca4 O4 -113.21(7) . . . . ? O3 Ca3 Ca4 O4 95.70(9) . . . . ? N5 Ca3 Ca4 O4 -19.13(8) . . . . ? N6 Ca3 Ca4 O4 119.52(8) . . . . ? Si11 Ca3 Ca4 O4 146.31(6) . . . . ? Si10 Ca3 Ca4 O4 8.99(6) . . . . ? Si14 Ca3 Ca4 O4 -128.78(6) . . . . ? Si13 Ca3 Ca4 O4 -96.97(6) . . . . ? N7 Ca3 Ca4 N6 127.28(7) . . . . ? O3 Ca3 Ca4 N6 -23.82(8) . . . . ? N5 Ca3 Ca4 N6 -138.65(7) . . . . ? Si11 Ca3 Ca4 N6 26.79(5) . . . . ? Si10 Ca3 Ca4 N6 -110.52(5) . . . . ? Si14 Ca3 Ca4 N6 111.71(5) . . . . ? Si13 Ca3 Ca4 N6 143.51(5) . . . . ? N7 Ca3 Ca4 N5 -94.08(7) . . . . ? O3 Ca3 Ca4 N5 114.82(8) . . . . ? N6 Ca3 Ca4 N5 138.65(7) . . . . ? Si11 Ca3 Ca4 N5 165.44(5) . . . . ? Si10 Ca3 Ca4 N5 28.12(5) . . . . ? Si14 Ca3 Ca4 N5 -109.65(5) . . . . ? Si13 Ca3 Ca4 N5 -77.84(5) . . . . ? N7 Ca3 Ca4 Si12 152.43(5) . . . . ? O3 Ca3 Ca4 Si12 1.33(7) . . . . ? N5 Ca3 Ca4 Si12 -113.50(5) . . . . ? N6 Ca3 Ca4 Si12 25.15(5) . . . . ? Si11 Ca3 Ca4 Si12 51.941(17) . . . . ? Si10 Ca3 Ca4 Si12 -85.373(19) . . . . ? Si14 Ca3 Ca4 Si12 136.857(18) . . . . ? Si13 Ca3 Ca4 Si12 168.66(2) . . . . ? N7 Ca3 Ca4 Si16 74.33(5) . . . . ? O3 Ca3 Ca4 Si16 -76.77(7) . . . . ? N5 Ca3 Ca4 Si16 168.40(6) . . . . ? N6 Ca3 Ca4 Si16 -52.95(6) . . . . ? Si11 Ca3 Ca4 Si16 -26.16(3) . . . . ? Si10 Ca3 Ca4 Si16 -163.48(3) . . . . ? Si14 Ca3 Ca4 Si16 58.75(3) . . . . ? Si13 Ca3 Ca4 Si16 90.56(3) . . . . ? N7 Ca3 Ca4 Si9 -67.68(5) . . . . ? O3 Ca3 Ca4 Si9 141.22(7) . . . . ? N5 Ca3 Ca4 Si9 26.39(5) . . . . ? N6 Ca3 Ca4 Si9 165.04(5) . . . . ? Si11 Ca3 Ca4 Si9 -168.170(19) . . . . ? Si10 Ca3 Ca4 Si9 54.516(17) . . . . ? Si14 Ca3 Ca4 Si9 -83.254(17) . . . . ? Si13 Ca3 Ca4 Si9 -51.45(2) . . . . ? N7 Ca3 Ca4 Si15 18.56(5) . . . . ? O3 Ca3 Ca4 Si15 -132.54(7) . . . . ? N5 Ca3 Ca4 Si15 112.64(5) . . . . ? N6 Ca3 Ca4 Si15 -108.72(5) . . . . ? Si11 Ca3 Ca4 Si15 -81.928(19) . . . . ? Si10 Ca3 Ca4 Si15 140.76(2) . . . . ? Si14 Ca3 Ca4 Si15 2.988(19) . . . . ? Si13 Ca3 Ca4 Si15 34.79(3) . . . . ? C38 Si15 Ca4 N8 75.84(14) . . . . ? C37 Si15 Ca4 N8 -82.93(15) . . . . ? N8 Si15 Ca4 O4 -72.00(12) . . . . ? C38 Si15 Ca4 O4 3.84(10) . . . . ? C37 Si15 Ca4 O4 -154.92(11) . . . . ? N8 Si15 Ca4 N6 87.92(12) . . . . ? C38 Si15 Ca4 N6 163.76(10) . . . . ? C37 Si15 Ca4 N6 5.00(11) . . . . ? N8 Si15 Ca4 N5 -174.93(12) . . . . ? C38 Si15 Ca4 N5 -99.10(10) . . . . ? C37 Si15 Ca4 N5 102.14(11) . . . . ? N8 Si15 Ca4 Si12 55.00(11) . . . . ? C38 Si15 Ca4 Si12 130.84(10) . . . . ? C37 Si15 Ca4 Si12 -27.92(11) . . . . ? N8 Si15 Ca4 Si16 0.68(11) . . . . ? C38 Si15 Ca4 Si16 76.52(10) . . . . ? C37 Si15 Ca4 Si16 -82.24(10) . . . . ? N8 Si15 Ca4 Si9 -154.26(11) . . . . ? C38 Si15 Ca4 Si9 -78.42(10) . . . . ? C37 Si15 Ca4 Si9 122.82(10) . . . . ? N8 Si15 Ca4 Ca3 136.94(11) . . . . ? C38 Si15 Ca4 Ca3 -147.22(10) . . . . ? C37 Si15 Ca4 Ca3 54.02(10) . . . . ? C44 O3 C41 C42 -6.4(3) . . . . ? Ca3 O3 C41 C42 175.63(15) . . . . ? O3 C41 C42 C43 25.0(3) . . . . ? C41 C42 C43 C44 -34.1(3) . . . . ? C41 O3 C44 C43 -14.6(3) . . . . ? Ca3 O3 C44 C43 163.53(16) . . . . ? C42 C43 C44 O3 30.3(3) . . . . ? C48 O4 C45 C46 -5.4(3) . . . . ? Ca4 O4 C45 C46 164.60(15) . . . . ? O4 C45 C46 C47 26.5(3) . . . . ? C45 C46 C47 C48 -36.7(3) . . . . ? C45 O4 C48 C47 -17.8(2) . . . . ? Ca4 O4 C48 C47 173.26(14) . . . . ? C46 C47 C48 O4 34.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.990 _refine_diff_density_min -0.497 _refine_diff_density_rms 0.065 #==END data_rac9 _database_code_depnum_ccdc_archive 'CCDC 884450' #TrackingRef '- JulienJC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H52 Ca N2 O4 Si4' _chemical_formula_sum 'C20 H52 Ca N2 O4 Si4' _chemical_formula_weight 537.08 _chemical_absolute_configuration ad 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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.321(2) _cell_length_b 16.216(4) _cell_length_c 21.088(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3187.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 6733 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 24.83 _exptl_crystal_description plate _exptl_crystal_colour ? _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.119 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.372 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9533 _exptl_absorpt_correction_T_max 0.9926 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40012 _diffrn_reflns_av_R_equivalents 0.1201 _diffrn_reflns_av_sigmaI/netI 0.1477 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 28.49 _reflns_number_total 7992 _reflns_number_gt 5690 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (2001)' _computing_cell_refinement 'Bruker SMART (2001)' _computing_data_reduction 'Bruker SAINT+ (1999)' _computing_structure_solution 'SIR 92 (Altomare et al, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(8) _refine_ls_number_reflns 7992 _refine_ls_number_parameters 331 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1149 _refine_ls_R_factor_gt 0.0907 _refine_ls_wR_factor_ref 0.2200 _refine_ls_wR_factor_gt 0.2087 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.83016(13) 0.97666(6) 0.34331(5) 0.0222(2) Uani 1 1 d . . . Si1 Si 0.8327(2) 0.93946(11) 0.17391(9) 0.0376(4) Uani 1 1 d . A . H1 H 0.815(7) 0.998(4) 0.120(3) 0.045 Uiso 1 1 d . . . Si2 Si 0.56610(18) 0.99386(10) 0.23645(8) 0.0258(4) Uani 1 1 d . A . H2 H 0.511(7) 0.992(4) 0.301(3) 0.031 Uiso 1 1 d . . . Si3 Si 1.1104(2) 0.95060(11) 0.45804(9) 0.0329(4) Uani 1 1 d . A . H3 H 1.265(7) 0.971(4) 0.432(3) 0.039 Uiso 1 1 d . . . Si4 Si 1.0496(2) 0.82199(11) 0.36037(9) 0.0364(5) Uani 1 1 d . A . H4 H 0.953(8) 0.812(4) 0.305(3) 0.044 Uiso 1 1 d . . . O1 O 1.0050(5) 1.0783(3) 0.3094(2) 0.0356(11) Uani 1 1 d . A . O2 O 0.7437(5) 1.1222(2) 0.35685(18) 0.0261(9) Uani 1 1 d . A . O3 O 0.6861(6) 1.0032(2) 0.4395(2) 0.0431(13) Uani 1 1 d . A . O4 O 0.6787(6) 0.8601(2) 0.3702(2) 0.0409(12) Uani 1 1 d . A . N2 N 1.0154(5) 0.9114(3) 0.3972(2) 0.0233(10) Uani 1 1 d . A . N1 N 0.7401(5) 0.9695(3) 0.2391(3) 0.0292(11) Uani 1 1 d . A . C1 C 1.1543(8) 1.0822(5) 0.3079(4) 0.051(2) Uani 1 1 d . . . H1A H 1.1875 1.1260 0.3363 0.077 Uiso 1 1 calc R A . H1B H 1.1861 1.0940 0.2646 0.077 Uiso 1 1 calc R . . H1C H 1.1942 1.0293 0.3217 0.077 Uiso 1 1 calc R . . C2 C 0.9284(8) 1.1475(4) 0.2829(3) 0.0370(16) Uani 1 1 d . A . H2A H 0.8646 1.1288 0.2482 0.044 Uiso 1 1 calc R . . H2B H 0.9968 1.1883 0.2654 0.044 Uiso 1 1 calc R . . C3 C 0.8429(7) 1.1851(3) 0.3343(3) 0.0314(14) Uani 1 1 d . . . H3A H 0.9064 1.2034 0.3692 0.038 Uiso 1 1 calc R A . H3B H 0.7894 1.2335 0.3182 0.038 Uiso 1 1 calc R . . C4 C 0.6681(7) 1.1438(3) 0.4134(3) 0.0265(12) Uani 1 1 d . . . H4A H 0.7391 1.1574 0.4474 0.032 Uiso 1 1 calc R A . C5 C 0.5815(7) 1.0691(3) 0.4336(3) 0.0250(13) Uani 1 1 d . A . H5 H 0.5111 1.0549 0.3995 0.030 Uiso 1 1 calc R . . C6 C 0.5016(8) 1.0847(4) 0.4953(3) 0.0327(14) Uani 1 1 d . . . H6A H 0.5712 1.0944 0.5300 0.039 Uiso 1 1 calc R A . H6B H 0.4435 1.0356 0.5064 0.039 Uiso 1 1 calc R . . C7 C 0.4038(8) 1.1597(4) 0.4881(3) 0.0420(18) Uani 1 1 d . A . H7A H 0.3579 1.1723 0.5293 0.050 Uiso 1 1 calc R . . H7B H 0.3270 1.1472 0.4571 0.050 Uiso 1 1 calc R . . C8 C 0.4892(9) 1.2352(4) 0.4654(3) 0.0455(19) Uani 1 1 d . . . H8A H 0.4229 1.2822 0.4590 0.055 Uiso 1 1 calc R A . H8B H 0.5596 1.2510 0.4984 0.055 Uiso 1 1 calc R . . C9 C 0.5671(8) 1.2172(4) 0.4042(3) 0.0371(16) Uani 1 1 d . A . H9A H 0.6228 1.2663 0.3910 0.045 Uiso 1 1 calc R . . H9B H 0.4967 1.2046 0.3704 0.045 Uiso 1 1 calc R . . C10A C 0.6583(13) 0.9290(5) 0.4735(5) 0.032(2) Uani 0.693(16) 1 d PU A 1 H10A H 0.5961 0.9400 0.5106 0.038 Uiso 0.693(16) 1 calc PR A 1 H10B H 0.7490 0.9039 0.4885 0.038 Uiso 0.693(16) 1 calc PR A 1 C11A C 0.5824(12) 0.8717(5) 0.4261(4) 0.029(3) Uani 0.693(16) 1 d P A 1 H11A H 0.5620 0.8179 0.4463 0.035 Uiso 0.693(16) 1 calc PR A 1 H11B H 0.4904 0.8965 0.4125 0.035 Uiso 0.693(16) 1 calc PR A 1 C10B C 0.582(2) 0.9222(11) 0.4486(10) 0.025(5) Uani 0.307(16) 1 d P A 2 H10C H 0.5553 0.9149 0.4937 0.029 Uiso 0.307(16) 1 calc PR A 2 H10D H 0.4928 0.9281 0.4233 0.029 Uiso 0.307(16) 1 calc PR A 2 C11B C 0.666(3) 0.8531(12) 0.4263(9) 0.025(5) Uani 0.307(16) 1 d PU A 2 H11C H 0.7619 0.8534 0.4468 0.030 Uiso 0.307(16) 1 calc PR A 2 H11D H 0.6178 0.8005 0.4367 0.030 Uiso 0.307(16) 1 calc PR A 2 C12 C 0.6346(9) 0.7948(4) 0.3305(4) 0.0473(19) Uani 1 1 d . . . H12A H 0.5486 0.7689 0.3483 0.071 Uiso 1 1 calc R A . H12B H 0.7117 0.7539 0.3275 0.071 Uiso 1 1 calc R . . H12C H 0.6130 0.8163 0.2882 0.071 Uiso 1 1 calc R . . C13 C 0.8074(8) 0.8281(4) 0.1535(4) 0.0457(18) Uani 1 1 d . . . H13A H 0.7069 0.8183 0.1421 0.069 Uiso 1 1 calc R A . H13B H 0.8330 0.7940 0.1901 0.069 Uiso 1 1 calc R . . H13C H 0.8691 0.8138 0.1175 0.069 Uiso 1 1 calc R . . C14 C 1.0292(10) 0.9587(6) 0.1733(4) 0.068(3) Uani 1 1 d . . . H14A H 1.0685 0.9482 0.2157 0.102 Uiso 1 1 calc R A . H14B H 1.0475 1.0162 0.1615 0.102 Uiso 1 1 calc R . . H14C H 1.0752 0.9219 0.1426 0.102 Uiso 1 1 calc R . . C15 C 0.4502(7) 0.9248(5) 0.1874(3) 0.0413(16) Uani 1 1 d . . . H15A H 0.4658 0.8673 0.2000 0.062 Uiso 1 1 calc R A . H15B H 0.4748 0.9315 0.1425 0.062 Uiso 1 1 calc R . . H15C H 0.3492 0.9393 0.1939 0.062 Uiso 1 1 calc R . . C16 C 0.5268(8) 1.1017(4) 0.2092(4) 0.0440(18) Uani 1 1 d . . . H16A H 0.5583 1.1083 0.1652 0.066 Uiso 1 1 calc R A . H16B H 0.5781 1.1410 0.2362 0.066 Uiso 1 1 calc R . . H16C H 0.4234 1.1121 0.2120 0.066 Uiso 1 1 calc R . . C17A C 1.1474(16) 0.8806(7) 0.5249(5) 0.047(3) Uani 0.693(16) 1 d PU A 1 H17A H 1.0577 0.8548 0.5388 0.070 Uiso 0.693(16) 1 calc PR A 1 H17B H 1.1891 0.9119 0.5600 0.070 Uiso 0.693(16) 1 calc PR A 1 H17C H 1.2149 0.8378 0.5113 0.070 Uiso 0.693(16) 1 calc PR A 1 C17B C 1.070(3) 0.8831(13) 0.5365(11) 0.037(6) Uani 0.307(16) 1 d PU A 2 H17D H 0.9672 0.8829 0.5451 0.055 Uiso 0.307(16) 1 calc PR A 2 H17E H 1.1214 0.9071 0.5727 0.055 Uiso 0.307(16) 1 calc PR A 2 H17F H 1.1035 0.8264 0.5299 0.055 Uiso 0.307(16) 1 calc PR A 2 C18 C 1.0340(9) 1.0489(4) 0.4865(3) 0.0435(18) Uani 1 1 d . . . H18A H 0.9487 1.0378 0.5123 0.065 Uiso 1 1 calc R A . H18B H 1.0074 1.0832 0.4501 0.065 Uiso 1 1 calc R . . H18C H 1.1055 1.0780 0.5123 0.065 Uiso 1 1 calc R . . C19 C 0.9961(13) 0.7273(4) 0.4050(5) 0.080(3) Uani 1 1 d . . . H19A H 0.8989 0.7344 0.4219 0.120 Uiso 1 1 calc R A . H19B H 1.0632 0.7183 0.4401 0.120 Uiso 1 1 calc R . . H19C H 0.9982 0.6796 0.3765 0.120 Uiso 1 1 calc R . . C20 C 1.2356(10) 0.8072(6) 0.3325(5) 0.072(3) Uani 1 1 d . . . H20A H 1.3005 0.8054 0.3690 0.108 Uiso 1 1 calc R A . H20B H 1.2626 0.8531 0.3047 0.108 Uiso 1 1 calc R . . H20C H 1.2423 0.7553 0.3089 0.108 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 0.0238(6) 0.0166(5) 0.0261(6) 0.0009(4) -0.0035(5) -0.0002(4) Si1 0.0352(10) 0.0299(9) 0.0478(11) 0.0043(8) 0.0100(9) 0.0048(8) Si2 0.0276(9) 0.0247(8) 0.0251(8) 0.0026(6) -0.0075(7) 0.0009(7) Si3 0.0398(11) 0.0270(8) 0.0319(10) -0.0056(7) -0.0113(8) 0.0071(7) Si4 0.0491(12) 0.0267(8) 0.0333(10) -0.0075(7) -0.0159(9) 0.0123(8) O1 0.027(2) 0.030(2) 0.050(3) 0.014(2) -0.006(2) -0.0038(19) O2 0.041(3) 0.0177(18) 0.020(2) -0.0017(15) 0.0006(19) -0.0047(17) O3 0.062(3) 0.0169(19) 0.051(3) 0.0147(18) 0.027(3) 0.013(2) O4 0.055(3) 0.024(2) 0.044(3) 0.0030(19) -0.005(3) -0.019(2) N2 0.024(3) 0.020(2) 0.026(3) -0.0017(19) -0.004(2) 0.0068(19) N1 0.026(3) 0.021(2) 0.041(3) 0.000(2) -0.003(2) 0.001(2) C1 0.037(4) 0.053(4) 0.065(5) 0.015(4) 0.009(4) -0.003(4) C2 0.046(4) 0.027(3) 0.039(4) 0.008(3) 0.002(3) -0.007(3) C3 0.038(4) 0.022(3) 0.034(3) 0.003(2) -0.004(3) -0.005(3) C4 0.030(3) 0.021(3) 0.029(3) -0.005(2) 0.001(3) 0.003(3) C5 0.034(4) 0.016(3) 0.025(3) -0.009(2) -0.004(3) -0.001(2) C6 0.044(4) 0.027(3) 0.028(3) -0.013(3) 0.007(3) 0.000(3) C7 0.050(5) 0.042(4) 0.034(4) -0.019(3) 0.001(3) 0.010(3) C8 0.060(5) 0.033(3) 0.043(4) -0.015(3) -0.009(4) 0.020(3) C9 0.043(4) 0.024(3) 0.044(4) -0.002(3) -0.005(3) 0.013(3) C10A 0.032(3) 0.032(3) 0.032(3) 0.0003(10) -0.0002(10) -0.0002(10) C11A 0.030(6) 0.021(5) 0.036(5) 0.004(4) -0.005(4) -0.008(4) C10B 0.026(12) 0.020(9) 0.028(11) -0.020(8) 0.009(9) -0.006(8) C11B 0.025(5) 0.025(5) 0.025(5) -0.0001(10) -0.0002(10) -0.0001(10) C12 0.055(5) 0.042(4) 0.045(4) -0.005(3) -0.005(4) -0.015(3) C13 0.044(5) 0.047(4) 0.046(4) -0.021(3) -0.001(4) 0.012(3) C14 0.076(7) 0.073(6) 0.056(5) -0.010(4) -0.007(5) 0.010(5) C15 0.023(3) 0.060(4) 0.041(4) 0.002(3) -0.006(3) -0.005(3) C16 0.039(4) 0.046(4) 0.047(4) 0.013(3) -0.005(3) 0.006(3) C17A 0.047(3) 0.047(3) 0.046(3) 0.0001(10) -0.0010(10) 0.0005(10) C17B 0.037(6) 0.037(6) 0.037(6) 0.0000(10) -0.0001(10) -0.0001(10) C18 0.054(5) 0.038(4) 0.038(4) -0.012(3) -0.007(3) -0.001(3) C19 0.129(10) 0.026(4) 0.085(7) 0.000(4) -0.045(7) 0.001(5) C20 0.058(6) 0.080(6) 0.078(7) -0.028(5) -0.002(5) 0.034(5) _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 N2 2.323(5) . ? Ca1 N1 2.356(5) . ? Ca1 O1 2.426(4) . ? Ca1 O4 2.427(4) . ? Ca1 O3 2.471(5) . ? Ca1 O2 2.510(4) . ? Ca1 C11B 3.07(2) . ? Ca1 C2 3.184(6) . ? Ca1 Si4 3.256(2) . ? Ca1 Si2 3.349(2) . ? Ca1 Si3 3.585(2) . ? Ca1 Si1 3.623(2) . ? Si1 N1 1.694(6) . ? Si1 C14 1.858(10) . ? Si1 C13 1.871(7) . ? Si1 H1 1.49(6) . ? Si2 N1 1.670(5) . ? Si2 C15 1.869(7) . ? Si2 C16 1.877(7) . ? Si2 H2 1.45(6) . ? Si3 N2 1.683(5) . ? Si3 C17A 1.842(11) . ? Si3 C18 1.847(7) . ? Si3 C17B 2.02(2) . ? Si3 H3 1.58(7) . ? Si4 N2 1.675(5) . ? Si4 C20 1.847(9) . ? Si4 C19 1.869(9) . ? Si4 H4 1.48(7) . ? O1 C1 1.394(9) . ? O1 C2 1.443(8) . ? O2 C4 1.429(7) . ? O2 C3 1.457(7) . ? O3 C10A 1.425(9) . ? O3 C5 1.452(7) . ? O3 C10B 1.646(18) . ? O4 C11B 1.194(19) . ? O4 C12 1.409(8) . ? O4 C11A 1.494(11) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.476(9) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.516(8) . ? C4 C9 1.530(8) . ? C4 H4A 1.0000 . ? C5 C6 1.521(8) . ? C5 H5 1.0000 . ? C6 C7 1.529(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.536(10) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.510(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10A C11A 1.537(14) . ? C10A H10A 0.9900 . ? C10A H10B 0.9900 . ? C11A H11A 0.9900 . ? C11A H11B 0.9900 . ? C10B C11B 1.45(3) . ? C10B H10C 0.9900 . ? C10B H10D 0.9900 . ? C11B H11C 0.9900 . ? C11B H11D 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17A H17A 0.9800 . ? C17A H17B 0.9800 . ? C17A H17C 0.9800 . ? C17B H17D 0.9800 . ? C17B H17E 0.9800 . ? C17B H17F 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 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 N2 Ca1 N1 134.36(17) . . ? N2 Ca1 O1 87.39(16) . . ? N1 Ca1 O1 89.91(17) . . ? N2 Ca1 O4 87.89(17) . . ? N1 Ca1 O4 88.38(17) . . ? O1 Ca1 O4 171.55(18) . . ? N2 Ca1 O3 94.69(17) . . ? N1 Ca1 O3 125.52(19) . . ? O1 Ca1 O3 119.23(16) . . ? O4 Ca1 O3 68.17(16) . . ? N2 Ca1 O2 127.70(15) . . ? N1 Ca1 O2 92.19(15) . . ? O1 Ca1 O2 67.05(14) . . ? O4 Ca1 O2 121.28(17) . . ? O3 Ca1 O2 64.41(13) . . ? N2 Ca1 C11B 78.1(5) . . ? N1 Ca1 C11B 108.8(4) . . ? O1 Ca1 C11B 161.2(5) . . ? O4 Ca1 C11B 21.3(4) . . ? O3 Ca1 C11B 51.3(4) . . ? O2 Ca1 C11B 112.9(4) . . ? N2 Ca1 C2 112.25(19) . . ? N1 Ca1 C2 76.84(17) . . ? O1 Ca1 C2 25.51(17) . . ? O4 Ca1 C2 159.82(19) . . ? O3 Ca1 C2 109.45(16) . . ? O2 Ca1 C2 47.13(16) . . ? C11B Ca1 C2 160.0(4) . . ? N2 Ca1 Si4 29.31(12) . . ? N1 Ca1 Si4 106.78(13) . . ? O1 Ca1 Si4 97.72(12) . . ? O4 Ca1 Si4 74.89(14) . . ? O3 Ca1 Si4 112.65(11) . . ? O2 Ca1 Si4 155.97(11) . . ? C11B Ca1 Si4 75.3(5) . . ? C2 Ca1 Si4 122.27(15) . . ? N2 Ca1 Si2 156.04(12) . . ? N1 Ca1 Si2 27.67(13) . . ? O1 Ca1 Si2 103.83(11) . . ? O4 Ca1 Si2 78.13(13) . . ? O3 Ca1 Si2 97.96(14) . . ? O2 Ca1 Si2 76.24(10) . . ? C11B Ca1 Si2 94.1(5) . . ? C2 Ca1 Si2 82.51(14) . . ? Si4 Ca1 Si2 126.88(5) . . ? N2 Ca1 Si3 22.23(11) . . ? N1 Ca1 Si3 152.06(13) . . ? O1 Ca1 Si3 77.85(11) . . ? O4 Ca1 Si3 100.05(13) . . ? O3 Ca1 Si3 82.10(13) . . ? O2 Ca1 Si3 105.54(10) . . ? C11B Ca1 Si3 84.3(5) . . ? C2 Ca1 Si3 99.39(14) . . ? Si4 Ca1 Si3 51.47(5) . . ? Si2 Ca1 Si3 177.98(5) . . ? N2 Ca1 Si1 113.70(13) . . ? N1 Ca1 Si1 22.20(13) . . ? O1 Ca1 Si1 79.54(12) . . ? O4 Ca1 Si1 95.98(12) . . ? O3 Ca1 Si1 147.37(14) . . ? O2 Ca1 Si1 105.71(10) . . ? C11B Ca1 Si1 117.2(4) . . ? C2 Ca1 Si1 75.43(13) . . ? Si4 Ca1 Si1 88.66(5) . . ? Si2 Ca1 Si1 49.85(5) . . ? Si3 Ca1 Si1 129.87(6) . . ? N1 Si1 C14 117.4(3) . . ? N1 Si1 C13 113.6(3) . . ? C14 Si1 C13 106.6(4) . . ? C14 Si1 Ca1 89.1(3) . . ? C13 Si1 Ca1 112.8(3) . . ? N1 Si1 H1 112(3) . . ? C14 Si1 H1 90(3) . . ? C13 Si1 H1 115(3) . . ? Ca1 Si1 H1 130(2) . . ? N1 Si2 C15 116.0(3) . . ? N1 Si2 C16 114.9(3) . . ? C15 Si2 C16 106.0(3) . . ? C15 Si2 Ca1 138.4(2) . . ? C16 Si2 Ca1 115.3(2) . . ? N1 Si2 H2 108(2) . . ? C15 Si2 H2 108(2) . . ? C16 Si2 H2 104(2) . . ? Ca1 Si2 H2 68(2) . . ? N2 Si3 C17A 116.6(4) . . ? N2 Si3 C18 111.8(3) . . ? C17A Si3 C18 110.8(4) . . ? N2 Si3 C17B 108.8(7) . . ? C18 Si3 C17B 97.5(8) . . ? C17A Si3 Ca1 136.5(4) . . ? C18 Si3 Ca1 80.6(2) . . ? C17B Si3 Ca1 118.9(8) . . ? N2 Si3 H3 107(2) . . ? C17A Si3 H3 103(2) . . ? C18 Si3 H3 106(2) . . ? C17B Si3 H3 125(2) . . ? Ca1 Si3 H3 114(2) . . ? N2 Si4 C20 116.0(4) . . ? N2 Si4 C19 115.2(4) . . ? C20 Si4 C19 107.7(5) . . ? C20 Si4 Ca1 130.9(3) . . ? C19 Si4 Ca1 121.4(4) . . ? N2 Si4 H4 110(3) . . ? C20 Si4 H4 108(3) . . ? C19 Si4 H4 98(3) . . ? Ca1 Si4 H4 67(3) . . ? C1 O1 C2 116.8(5) . . ? C1 O1 Ca1 135.1(4) . . ? C2 O1 Ca1 108.1(4) . . ? C4 O2 C3 114.5(4) . . ? C4 O2 Ca1 118.9(3) . . ? C3 O2 Ca1 114.6(3) . . ? C10A O3 C5 122.9(6) . . ? C5 O3 C10B 101.6(8) . . ? C10A O3 Ca1 111.4(4) . . ? C5 O3 Ca1 115.0(3) . . ? C10B O3 Ca1 106.1(6) . . ? C11B O4 C12 119.3(10) . . ? C12 O4 C11A 112.9(6) . . ? C11B O4 Ca1 111.1(11) . . ? C12 O4 Ca1 128.0(4) . . ? C11A O4 Ca1 115.8(4) . . ? Si4 N2 Si3 125.5(3) . . ? Si4 N2 Ca1 107.9(2) . . ? Si3 N2 Ca1 126.3(2) . . ? Si2 N1 Si1 122.4(3) . . ? Si2 N1 Ca1 111.4(3) . . ? Si1 N1 Ca1 126.1(3) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 107.6(5) . . ? C3 C2 Ca1 84.9(3) . . ? O1 C2 H2A 110.2 . . ? C3 C2 H2A 110.2 . . ? Ca1 C2 H2A 81.7 . . ? O1 C2 H2B 110.2 . . ? C3 C2 H2B 110.2 . . ? Ca1 C2 H2B 156.3 . . ? H2A C2 H2B 108.5 . . ? O2 C3 C2 107.1(5) . . ? O2 C3 H3A 110.3 . . ? C2 C3 H3A 110.3 . . ? O2 C3 H3B 110.3 . . ? C2 C3 H3B 110.3 . . ? H3A C3 H3B 108.6 . . ? O2 C4 C5 107.5(4) . . ? O2 C4 C9 112.9(5) . . ? C5 C4 C9 109.2(6) . . ? O2 C4 H4A 109.1 . . ? C5 C4 H4A 109.1 . . ? C9 C4 H4A 109.1 . . ? O3 C5 C4 104.8(5) . . ? O3 C5 C6 112.1(5) . . ? C4 C5 C6 111.6(4) . . ? O3 C5 H5 109.4 . . ? C4 C5 H5 109.4 . . ? C6 C5 H5 109.4 . . ? C5 C6 C7 109.8(5) . . ? C5 C6 H6A 109.7 . . ? C7 C6 H6A 109.7 . . ? C5 C6 H6B 109.7 . . ? C7 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? C6 C7 C8 110.9(6) . . ? C6 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C9 C8 C7 111.2(5) . . ? C9 C8 H8A 109.4 . . ? C7 C8 H8A 109.4 . . ? C9 C8 H8B 109.4 . . ? C7 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C8 C9 C4 109.7(5) . . ? C8 C9 H9A 109.7 . . ? C4 C9 H9A 109.7 . . ? C8 C9 H9B 109.7 . . ? C4 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? O3 C10A C11A 105.5(7) . . ? O3 C10A H10A 110.6 . . ? C11A C10A H10A 110.6 . . ? O3 C10A H10B 110.6 . . ? C11A C10A H10B 110.6 . . ? H10A C10A H10B 108.8 . . ? O4 C11A C10A 108.3(8) . . ? O4 C11A H11A 110.0 . . ? C10A C11A H11A 110.0 . . ? O4 C11A H11B 110.0 . . ? C10A C11A H11B 110.0 . . ? H11A C11A H11B 108.4 . . ? C11B C10B O3 104.9(15) . . ? C11B C10B H10C 110.8 . . ? O3 C10B H10C 110.8 . . ? C11B C10B H10D 110.8 . . ? O3 C10B H10D 110.8 . . ? H10C C10B H10D 108.8 . . ? O4 C11B C10B 107.6(19) . . ? O4 C11B Ca1 47.6(8) . . ? C10B C11B Ca1 87.2(11) . . ? O4 C11B H11C 110.2 . . ? C10B C11B H11C 110.2 . . ? Ca1 C11B H11C 78.4 . . ? O4 C11B H11D 110.2 . . ? C10B C11B H11D 110.2 . . ? Ca1 C11B H11D 156.5 . . ? H11C C11B H11D 108.5 . . ? O4 C12 H12A 109.5 . . ? O4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si2 C15 H15A 109.5 . . ? Si2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si3 C17A H17A 109.5 . . ? Si3 C17A H17B 109.5 . . ? Si3 C17A H17C 109.5 . . ? Si3 C17B H17D 109.5 . . ? Si3 C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? Si3 C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? Si3 C18 H18A 109.5 . . ? Si3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si4 C19 H19A 109.5 . . ? Si4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si4 C20 H20A 109.5 . . ? Si4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 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 Ca1 Si1 N1 160.9(3) . . . . ? O1 Ca1 Si1 N1 -116.6(3) . . . . ? O4 Ca1 Si1 N1 70.6(3) . . . . ? O3 Ca1 Si1 N1 12.6(4) . . . . ? O2 Ca1 Si1 N1 -54.3(3) . . . . ? C11B Ca1 Si1 N1 72.6(6) . . . . ? C2 Ca1 Si1 N1 -90.8(3) . . . . ? Si4 Ca1 Si1 N1 145.3(3) . . . . ? Si2 Ca1 Si1 N1 1.7(3) . . . . ? Si3 Ca1 Si1 N1 179.0(3) . . . . ? N2 Ca1 Si1 C14 -45.0(3) . . . . ? N1 Ca1 Si1 C14 154.0(4) . . . . ? O1 Ca1 Si1 C14 37.4(3) . . . . ? O4 Ca1 Si1 C14 -135.4(3) . . . . ? O3 Ca1 Si1 C14 166.6(3) . . . . ? O2 Ca1 Si1 C14 99.8(3) . . . . ? C11B Ca1 Si1 C14 -133.4(6) . . . . ? C2 Ca1 Si1 C14 63.2(3) . . . . ? Si4 Ca1 Si1 C14 -60.7(3) . . . . ? Si2 Ca1 Si1 C14 155.7(3) . . . . ? Si3 Ca1 Si1 C14 -26.9(3) . . . . ? N2 Ca1 Si1 C13 62.6(3) . . . . ? N1 Ca1 Si1 C13 -98.4(4) . . . . ? O1 Ca1 Si1 C13 145.0(3) . . . . ? O4 Ca1 Si1 C13 -27.7(3) . . . . ? O3 Ca1 Si1 C13 -85.7(3) . . . . ? O2 Ca1 Si1 C13 -152.6(3) . . . . ? C11B Ca1 Si1 C13 -25.8(6) . . . . ? C2 Ca1 Si1 C13 170.8(3) . . . . ? Si4 Ca1 Si1 C13 46.9(3) . . . . ? Si2 Ca1 Si1 C13 -96.7(3) . . . . ? Si3 Ca1 Si1 C13 80.7(3) . . . . ? N2 Ca1 Si2 N1 -54.2(4) . . . . ? O1 Ca1 Si2 N1 61.8(3) . . . . ? O4 Ca1 Si2 N1 -109.8(3) . . . . ? O3 Ca1 Si2 N1 -175.4(3) . . . . ? O2 Ca1 Si2 N1 123.5(3) . . . . ? C11B Ca1 Si2 N1 -123.9(5) . . . . ? C2 Ca1 Si2 N1 75.9(3) . . . . ? Si4 Ca1 Si2 N1 -49.2(3) . . . . ? Si1 Ca1 Si2 N1 -1.3(2) . . . . ? N2 Ca1 Si2 C15 18.7(5) . . . . ? N1 Ca1 Si2 C15 73.0(4) . . . . ? O1 Ca1 Si2 C15 134.7(4) . . . . ? O4 Ca1 Si2 C15 -36.8(4) . . . . ? O3 Ca1 Si2 C15 -102.4(4) . . . . ? O2 Ca1 Si2 C15 -163.5(4) . . . . ? C11B Ca1 Si2 C15 -50.9(5) . . . . ? C2 Ca1 Si2 C15 148.9(4) . . . . ? Si4 Ca1 Si2 C15 23.8(4) . . . . ? Si1 Ca1 Si2 C15 71.6(3) . . . . ? N2 Ca1 Si2 C16 -153.7(4) . . . . ? N1 Ca1 Si2 C16 -99.5(4) . . . . ? O1 Ca1 Si2 C16 -37.7(3) . . . . ? O4 Ca1 Si2 C16 150.7(3) . . . . ? O3 Ca1 Si2 C16 85.1(3) . . . . ? O2 Ca1 Si2 C16 24.0(3) . . . . ? C11B Ca1 Si2 C16 136.6(5) . . . . ? C2 Ca1 Si2 C16 -23.6(3) . . . . ? Si4 Ca1 Si2 C16 -148.7(3) . . . . ? Si1 Ca1 Si2 C16 -100.9(3) . . . . ? N1 Ca1 Si3 N2 -48.0(4) . . . . ? O1 Ca1 Si3 N2 -113.8(4) . . . . ? O4 Ca1 Si3 N2 57.8(4) . . . . ? O3 Ca1 Si3 N2 123.9(3) . . . . ? O2 Ca1 Si3 N2 -175.5(4) . . . . ? C11B Ca1 Si3 N2 72.2(5) . . . . ? C2 Ca1 Si3 N2 -127.6(4) . . . . ? Si4 Ca1 Si3 N2 -3.5(3) . . . . ? Si1 Ca1 Si3 N2 -48.8(3) . . . . ? N2 Ca1 Si3 C17A -61.8(7) . . . . ? N1 Ca1 Si3 C17A -109.8(6) . . . . ? O1 Ca1 Si3 C17A -175.6(6) . . . . ? O4 Ca1 Si3 C17A -3.9(6) . . . . ? O3 Ca1 Si3 C17A 62.1(6) . . . . ? O2 Ca1 Si3 C17A 122.7(6) . . . . ? C11B Ca1 Si3 C17A 10.5(7) . . . . ? C2 Ca1 Si3 C17A 170.6(6) . . . . ? Si4 Ca1 Si3 C17A -65.3(6) . . . . ? Si1 Ca1 Si3 C17A -110.5(6) . . . . ? N2 Ca1 Si3 C18 -172.2(4) . . . . ? N1 Ca1 Si3 C18 139.8(4) . . . . ? O1 Ca1 Si3 C18 73.9(3) . . . . ? O4 Ca1 Si3 C18 -114.4(3) . . . . ? O3 Ca1 Si3 C18 -48.4(3) . . . . ? O2 Ca1 Si3 C18 12.2(3) . . . . ? C11B Ca1 Si3 C18 -100.0(5) . . . . ? C2 Ca1 Si3 C18 60.2(3) . . . . ? Si4 Ca1 Si3 C18 -175.8(3) . . . . ? Si1 Ca1 Si3 C18 139.0(3) . . . . ? N2 Ca1 Si3 C17B -78.8(8) . . . . ? N1 Ca1 Si3 C17B -126.8(8) . . . . ? O1 Ca1 Si3 C17B 167.4(8) . . . . ? O4 Ca1 Si3 C17B -20.9(8) . . . . ? O3 Ca1 Si3 C17B 45.1(8) . . . . ? O2 Ca1 Si3 C17B 105.7(8) . . . . ? C11B Ca1 Si3 C17B -6.5(9) . . . . ? C2 Ca1 Si3 C17B 153.6(8) . . . . ? Si4 Ca1 Si3 C17B -82.3(8) . . . . ? Si1 Ca1 Si3 C17B -127.5(8) . . . . ? N1 Ca1 Si4 N2 162.7(3) . . . . ? O1 Ca1 Si4 N2 70.4(3) . . . . ? O4 Ca1 Si4 N2 -113.8(3) . . . . ? O3 Ca1 Si4 N2 -55.8(3) . . . . ? O2 Ca1 Si4 N2 21.9(4) . . . . ? C11B Ca1 Si4 N2 -91.7(5) . . . . ? C2 Ca1 Si4 N2 77.9(3) . . . . ? Si2 Ca1 Si4 N2 -175.8(3) . . . . ? Si3 Ca1 Si4 N2 2.7(3) . . . . ? Si1 Ca1 Si4 N2 149.7(3) . . . . ? N2 Ca1 Si4 C20 -85.3(5) . . . . ? N1 Ca1 Si4 C20 77.4(4) . . . . ? O1 Ca1 Si4 C20 -14.9(4) . . . . ? O4 Ca1 Si4 C20 160.9(4) . . . . ? O3 Ca1 Si4 C20 -141.1(4) . . . . ? O2 Ca1 Si4 C20 -63.4(5) . . . . ? C11B Ca1 Si4 C20 -177.0(6) . . . . ? C2 Ca1 Si4 C20 -7.4(4) . . . . ? Si2 Ca1 Si4 C20 98.9(4) . . . . ? Si3 Ca1 Si4 C20 -82.6(4) . . . . ? Si1 Ca1 Si4 C20 64.4(4) . . . . ? N2 Ca1 Si4 C19 94.3(4) . . . . ? N1 Ca1 Si4 C19 -103.0(4) . . . . ? O1 Ca1 Si4 C19 164.7(3) . . . . ? O4 Ca1 Si4 C19 -19.5(4) . . . . ? O3 Ca1 Si4 C19 38.5(4) . . . . ? O2 Ca1 Si4 C19 116.2(4) . . . . ? C11B Ca1 Si4 C19 2.6(5) . . . . ? C2 Ca1 Si4 C19 172.2(4) . . . . ? Si2 Ca1 Si4 C19 -81.5(3) . . . . ? Si3 Ca1 Si4 C19 97.0(3) . . . . ? Si1 Ca1 Si4 C19 -116.0(3) . . . . ? N2 Ca1 O1 C1 15.9(7) . . . . ? N1 Ca1 O1 C1 -118.6(7) . . . . ? O3 Ca1 O1 C1 109.8(7) . . . . ? O2 Ca1 O1 C1 149.0(7) . . . . ? C11B Ca1 O1 C1 55.1(16) . . . . ? C2 Ca1 O1 C1 -176.9(9) . . . . ? Si4 Ca1 O1 C1 -11.6(7) . . . . ? Si2 Ca1 O1 C1 -142.7(7) . . . . ? Si3 Ca1 O1 C1 36.1(7) . . . . ? Si1 Ca1 O1 C1 -98.8(7) . . . . ? N2 Ca1 O1 C2 -167.3(4) . . . . ? N1 Ca1 O1 C2 58.3(4) . . . . ? O3 Ca1 O1 C2 -73.4(4) . . . . ? O2 Ca1 O1 C2 -34.1(4) . . . . ? C11B Ca1 O1 C2 -128.0(14) . . . . ? Si4 Ca1 O1 C2 165.2(4) . . . . ? Si2 Ca1 O1 C2 34.2(4) . . . . ? Si3 Ca1 O1 C2 -147.0(4) . . . . ? Si1 Ca1 O1 C2 78.1(4) . . . . ? N2 Ca1 O2 C4 -70.9(5) . . . . ? N1 Ca1 O2 C4 133.0(4) . . . . ? O1 Ca1 O2 C4 -138.0(4) . . . . ? O4 Ca1 O2 C4 43.6(4) . . . . ? O3 Ca1 O2 C4 4.3(4) . . . . ? C11B Ca1 O2 C4 21.5(7) . . . . ? C2 Ca1 O2 C4 -157.2(5) . . . . ? Si4 Ca1 O2 C4 -84.3(5) . . . . ? Si2 Ca1 O2 C4 110.2(4) . . . . ? Si3 Ca1 O2 C4 -68.8(4) . . . . ? Si1 Ca1 O2 C4 150.9(4) . . . . ? N2 Ca1 O2 C3 69.8(4) . . . . ? N1 Ca1 O2 C3 -86.2(4) . . . . ? O1 Ca1 O2 C3 2.7(3) . . . . ? O4 Ca1 O2 C3 -175.7(3) . . . . ? O3 Ca1 O2 C3 145.0(4) . . . . ? C11B Ca1 O2 C3 162.3(6) . . . . ? C2 Ca1 O2 C3 -16.5(4) . . . . ? Si4 Ca1 O2 C3 56.5(5) . . . . ? Si2 Ca1 O2 C3 -109.0(4) . . . . ? Si3 Ca1 O2 C3 71.9(4) . . . . ? Si1 Ca1 O2 C3 -68.4(4) . . . . ? N2 Ca1 O3 C10A -55.5(6) . . . . ? N1 Ca1 O3 C10A 101.5(6) . . . . ? O1 Ca1 O3 C10A -145.1(6) . . . . ? O4 Ca1 O3 C10A 30.4(6) . . . . ? O2 Ca1 O3 C10A 174.7(6) . . . . ? C11B Ca1 O3 C10A 15.2(9) . . . . ? C2 Ca1 O3 C10A -171.1(6) . . . . ? Si4 Ca1 O3 C10A -31.5(6) . . . . ? Si2 Ca1 O3 C10A 104.1(6) . . . . ? Si3 Ca1 O3 C10A -73.8(6) . . . . ? Si1 Ca1 O3 C10A 95.7(6) . . . . ? N2 Ca1 O3 C5 158.8(4) . . . . ? N1 Ca1 O3 C5 -44.2(4) . . . . ? O1 Ca1 O3 C5 69.2(4) . . . . ? O4 Ca1 O3 C5 -115.4(4) . . . . ? O2 Ca1 O3 C5 28.9(3) . . . . ? C11B Ca1 O3 C5 -130.5(8) . . . . ? C2 Ca1 O3 C5 43.2(4) . . . . ? Si4 Ca1 O3 C5 -177.2(3) . . . . ? Si2 Ca1 O3 C5 -41.6(4) . . . . ? Si3 Ca1 O3 C5 140.4(4) . . . . ? Si1 Ca1 O3 C5 -50.0(5) . . . . ? N2 Ca1 O3 C10B -89.8(9) . . . . ? N1 Ca1 O3 C10B 67.2(9) . . . . ? O1 Ca1 O3 C10B -179.4(9) . . . . ? O4 Ca1 O3 C10B -3.9(9) . . . . ? O2 Ca1 O3 C10B 140.4(9) . . . . ? C11B Ca1 O3 C10B -19.1(11) . . . . ? C2 Ca1 O3 C10B 154.6(9) . . . . ? Si4 Ca1 O3 C10B -65.8(9) . . . . ? Si2 Ca1 O3 C10B 69.8(9) . . . . ? Si3 Ca1 O3 C10B -108.1(9) . . . . ? Si1 Ca1 O3 C10B 61.4(9) . . . . ? N2 Ca1 O4 C11B 61.6(14) . . . . ? N1 Ca1 O4 C11B -163.9(14) . . . . ? O3 Ca1 O4 C11B -34.3(14) . . . . ? O2 Ca1 O4 C11B -72.3(14) . . . . ? C2 Ca1 O4 C11B -121.4(14) . . . . ? Si4 Ca1 O4 C11B 88.3(14) . . . . ? Si2 Ca1 O4 C11B -138.0(14) . . . . ? Si3 Ca1 O4 C11B 42.9(14) . . . . ? Si1 Ca1 O4 C11B 175.2(14) . . . . ? N2 Ca1 O4 C12 -103.8(6) . . . . ? N1 Ca1 O4 C12 30.7(6) . . . . ? O3 Ca1 O4 C12 160.3(6) . . . . ? O2 Ca1 O4 C12 122.3(6) . . . . ? C11B Ca1 O4 C12 -165.4(16) . . . . ? C2 Ca1 O4 C12 73.2(8) . . . . ? Si4 Ca1 O4 C12 -77.1(6) . . . . ? Si2 Ca1 O4 C12 56.6(6) . . . . ? Si3 Ca1 O4 C12 -122.5(6) . . . . ? Si1 Ca1 O4 C12 9.8(6) . . . . ? N2 Ca1 O4 C11A 98.5(5) . . . . ? N1 Ca1 O4 C11A -127.0(5) . . . . ? O3 Ca1 O4 C11A 2.6(5) . . . . ? O2 Ca1 O4 C11A -35.4(6) . . . . ? C11B Ca1 O4 C11A 36.9(12) . . . . ? C2 Ca1 O4 C11A -84.5(7) . . . . ? Si4 Ca1 O4 C11A 125.2(5) . . . . ? Si2 Ca1 O4 C11A -101.1(5) . . . . ? Si3 Ca1 O4 C11A 79.8(5) . . . . ? Si1 Ca1 O4 C11A -147.9(5) . . . . ? C20 Si4 N2 Si3 -51.4(6) . . . . ? C19 Si4 N2 Si3 75.8(5) . . . . ? Ca1 Si4 N2 Si3 -174.4(5) . . . . ? C20 Si4 N2 Ca1 123.0(4) . . . . ? C19 Si4 N2 Ca1 -109.8(4) . . . . ? C17A Si3 N2 Si4 -49.3(7) . . . . ? C18 Si3 N2 Si4 -178.3(4) . . . . ? C17B Si3 N2 Si4 -71.7(9) . . . . ? Ca1 Si3 N2 Si4 173.4(6) . . . . ? C17A Si3 N2 Ca1 137.3(6) . . . . ? C18 Si3 N2 Ca1 8.2(5) . . . . ? C17B Si3 N2 Ca1 114.8(9) . . . . ? N1 Ca1 N2 Si4 -23.5(4) . . . . ? O1 Ca1 N2 Si4 -110.8(3) . . . . ? O4 Ca1 N2 Si4 62.1(3) . . . . ? O3 Ca1 N2 Si4 130.0(3) . . . . ? O2 Ca1 N2 Si4 -168.9(2) . . . . ? C11B Ca1 N2 Si4 81.2(4) . . . . ? C2 Ca1 N2 Si4 -116.7(3) . . . . ? Si2 Ca1 N2 Si4 8.3(5) . . . . ? Si3 Ca1 N2 Si4 -174.4(5) . . . . ? Si1 Ca1 N2 Si4 -33.5(3) . . . . ? N1 Ca1 N2 Si3 150.9(3) . . . . ? O1 Ca1 N2 Si3 63.5(3) . . . . ? O4 Ca1 N2 Si3 -123.5(3) . . . . ? O3 Ca1 N2 Si3 -55.6(3) . . . . ? O2 Ca1 N2 Si3 5.4(4) . . . . ? C11B Ca1 N2 Si3 -104.4(5) . . . . ? C2 Ca1 N2 Si3 57.7(4) . . . . ? Si4 Ca1 N2 Si3 174.4(5) . . . . ? Si2 Ca1 N2 Si3 -177.34(15) . . . . ? Si1 Ca1 N2 Si3 140.9(3) . . . . ? C15 Si2 N1 Si1 42.3(5) . . . . ? C16 Si2 N1 Si1 -82.0(4) . . . . ? Ca1 Si2 N1 Si1 177.4(5) . . . . ? C15 Si2 N1 Ca1 -135.1(3) . . . . ? C16 Si2 N1 Ca1 100.6(3) . . . . ? C14 Si1 N1 Si2 153.5(4) . . . . ? C13 Si1 N1 Si2 -81.4(4) . . . . ? Ca1 Si1 N1 Si2 -177.0(6) . . . . ? C14 Si1 N1 Ca1 -29.5(5) . . . . ? C13 Si1 N1 Ca1 95.6(4) . . . . ? N2 Ca1 N1 Si2 152.6(2) . . . . ? O1 Ca1 N1 Si2 -121.2(3) . . . . ? O4 Ca1 N1 Si2 67.1(3) . . . . ? O3 Ca1 N1 Si2 5.6(3) . . . . ? O2 Ca1 N1 Si2 -54.2(2) . . . . ? C11B Ca1 N1 Si2 61.0(5) . . . . ? C2 Ca1 N1 Si2 -99.1(3) . . . . ? Si4 Ca1 N1 Si2 140.8(2) . . . . ? Si3 Ca1 N1 Si2 175.71(12) . . . . ? Si1 Ca1 N1 Si2 177.3(5) . . . . ? N2 Ca1 N1 Si1 -24.7(4) . . . . ? O1 Ca1 N1 Si1 61.5(3) . . . . ? O4 Ca1 N1 Si1 -110.2(3) . . . . ? O3 Ca1 N1 Si1 -171.7(2) . . . . ? O2 Ca1 N1 Si1 128.6(3) . . . . ? C11B Ca1 N1 Si1 -116.3(5) . . . . ? C2 Ca1 N1 Si1 83.6(3) . . . . ? Si4 Ca1 N1 Si1 -36.5(3) . . . . ? Si2 Ca1 N1 Si1 -177.3(5) . . . . ? Si3 Ca1 N1 Si1 -1.6(5) . . . . ? C1 O1 C2 C3 -118.1(7) . . . . ? Ca1 O1 C2 C3 64.4(5) . . . . ? C1 O1 C2 Ca1 177.5(7) . . . . ? N2 Ca1 C2 O1 13.8(4) . . . . ? N1 Ca1 C2 O1 -119.1(4) . . . . ? O4 Ca1 C2 O1 -163.0(5) . . . . ? O3 Ca1 C2 O1 117.5(4) . . . . ? O2 Ca1 C2 O1 135.2(5) . . . . ? C11B Ca1 C2 O1 131.9(14) . . . . ? Si4 Ca1 C2 O1 -17.4(4) . . . . ? Si2 Ca1 C2 O1 -146.6(4) . . . . ? Si3 Ca1 C2 O1 32.7(4) . . . . ? Si1 Ca1 C2 O1 -96.3(4) . . . . ? N2 Ca1 C2 C3 -106.6(4) . . . . ? N1 Ca1 C2 C3 120.5(4) . . . . ? O1 Ca1 C2 C3 -120.4(6) . . . . ? O4 Ca1 C2 C3 76.7(6) . . . . ? O3 Ca1 C2 C3 -2.8(4) . . . . ? O2 Ca1 C2 C3 14.8(3) . . . . ? C11B Ca1 C2 C3 11.5(15) . . . . ? Si4 Ca1 C2 C3 -137.8(3) . . . . ? Si2 Ca1 C2 C3 93.0(4) . . . . ? Si3 Ca1 C2 C3 -87.7(4) . . . . ? Si1 Ca1 C2 C3 143.4(4) . . . . ? C4 O2 C3 C2 170.5(5) . . . . ? Ca1 O2 C3 C2 28.0(6) . . . . ? O1 C2 C3 O2 -60.7(6) . . . . ? Ca1 C2 C3 O2 -19.8(4) . . . . ? C3 O2 C4 C5 -174.6(5) . . . . ? Ca1 O2 C4 C5 -33.8(6) . . . . ? C3 O2 C4 C9 64.9(7) . . . . ? Ca1 O2 C4 C9 -154.3(4) . . . . ? C10A O3 C5 C4 162.5(7) . . . . ? C10B O3 C5 C4 -170.3(8) . . . . ? Ca1 O3 C5 C4 -56.2(5) . . . . ? C10A O3 C5 C6 41.2(9) . . . . ? C10B O3 C5 C6 68.5(9) . . . . ? Ca1 O3 C5 C6 -177.4(4) . . . . ? O2 C4 C5 O3 56.0(6) . . . . ? C9 C4 C5 O3 178.7(5) . . . . ? O2 C4 C5 C6 177.5(5) . . . . ? C9 C4 C5 C6 -59.7(7) . . . . ? O3 C5 C6 C7 174.6(5) . . . . ? C4 C5 C6 C7 57.4(7) . . . . ? C5 C6 C7 C8 -54.7(7) . . . . ? C6 C7 C8 C9 56.3(8) . . . . ? C7 C8 C9 C4 -58.2(8) . . . . ? O2 C4 C9 C8 178.9(5) . . . . ? C5 C4 C9 C8 59.4(7) . . . . ? C5 O3 C10A C11A 85.4(8) . . . . ? C10B O3 C10A C11A 29.6(12) . . . . ? Ca1 O3 C10A C11A -57.2(9) . . . . ? C11B O4 C11A C10A 57.8(18) . . . . ? C12 O4 C11A C10A 166.7(7) . . . . ? Ca1 O4 C11A C10A -32.2(8) . . . . ? O3 C10A C11A O4 58.1(9) . . . . ? C10A O3 C10B C11B -70.5(18) . . . . ? C5 O3 C10B C11B 154.6(14) . . . . ? Ca1 O3 C10B C11B 34.0(17) . . . . ? C12 O4 C11B C10B -124.1(14) . . . . ? C11A O4 C11B C10B -36.1(15) . . . . ? Ca1 O4 C11B C10B 69(2) . . . . ? C12 O4 C11B Ca1 166.8(15) . . . . ? C11A O4 C11B Ca1 -105.1(17) . . . . ? O3 C10B C11B O4 -69(2) . . . . ? O3 C10B C11B Ca1 -25.7(12) . . . . ? N2 Ca1 C11B O4 -116.0(13) . . . . ? N1 Ca1 C11B O4 17.1(15) . . . . ? O1 Ca1 C11B O4 -156.2(7) . . . . ? O3 Ca1 C11B O4 138.0(17) . . . . ? O2 Ca1 C11B O4 117.9(12) . . . . ? C2 Ca1 C11B O4 120.5(11) . . . . ? Si4 Ca1 C11B O4 -86.0(13) . . . . ? Si2 Ca1 C11B O4 41.1(13) . . . . ? Si3 Ca1 C11B O4 -137.6(13) . . . . ? Si1 Ca1 C11B O4 -5.3(16) . . . . ? N2 Ca1 C11B C10B 127.0(14) . . . . ? N1 Ca1 C11B C10B -99.9(13) . . . . ? O1 Ca1 C11B C10B 87(2) . . . . ? O4 Ca1 C11B C10B -117(2) . . . . ? O3 Ca1 C11B C10B 21.0(11) . . . . ? O2 Ca1 C11B C10B 0.9(15) . . . . ? C2 Ca1 C11B C10B 4(2) . . . . ? Si4 Ca1 C11B C10B 157.0(14) . . . . ? Si2 Ca1 C11B C10B -75.9(13) . . . . ? Si3 Ca1 C11B C10B 105.4(13) . . . . ? Si1 Ca1 C11B C10B -122.3(12) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.49 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.814 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.106 #==END