# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mo_01123a_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45.50 H69 Mg N3 O2 Si2' _chemical_formula_weight 770.53 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' 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' Mg Mg 0.0486 0.0363 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.031(3) _cell_length_b 12.120(2) _cell_length_c 44.305(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.088(3) _cell_angle_gamma 90.00 _cell_volume 9586(3) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9933 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 27.06 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.068 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3352 _exptl_absorpt_coefficient_mu 0.123 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9878 _exptl_absorpt_correction_T_max 0.9939 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27785 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 0.93 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8417 _reflns_number_gt 6282 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1060P)^2^+13.3176P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8417 _refine_ls_number_parameters 483 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.2076 _refine_ls_wR_factor_gt 0.1881 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 Mg1 Mg 0.39098(5) 0.60694(8) 0.10030(2) 0.0377(3) Uani 1 1 d . . . Si1 Si 0.43951(6) 0.74604(9) 0.04459(2) 0.0606(3) Uani 1 1 d . . . Si2 Si 0.34632(6) 0.86677(8) 0.08300(2) 0.0578(3) Uani 1 1 d . . . O1 O 0.31930(13) 0.51503(19) 0.06454(5) 0.0524(6) Uani 1 1 d . . . O2 O 0.31549(10) 0.59049(17) 0.12676(4) 0.0387(5) Uani 1 1 d . . . N1 N 0.44940(14) 0.4372(2) 0.11004(6) 0.0463(6) Uani 1 1 d . . . N2 N 0.47787(14) 0.6442(2) 0.13993(6) 0.0453(6) Uani 1 1 d . . . N3 N 0.39024(15) 0.7490(2) 0.07467(6) 0.0487(7) Uani 1 1 d . . . C1 C 0.2516(2) 0.5720(3) 0.05247(9) 0.0647(10) Uani 1 1 d . . . H1A H 0.2233 0.5274 0.0371 0.097 Uiso 1 1 calc R . . H1B H 0.2641 0.6408 0.0437 0.097 Uiso 1 1 calc R . . H1C H 0.2224 0.5858 0.0686 0.097 Uiso 1 1 calc R . . C2 C 0.33660(19) 0.4210(3) 0.04895(8) 0.0519(8) Uani 1 1 d . . . C3 C 0.3178(2) 0.4100(4) 0.01787(8) 0.0699(11) Uani 1 1 d . . . H3A H 0.2923 0.4661 0.0064 0.084 Uiso 1 1 calc R . . C4 C 0.3376(3) 0.3139(4) 0.00383(10) 0.0898(15) Uani 1 1 d . . . H4A H 0.3251 0.3057 -0.0171 0.108 Uiso 1 1 calc R . . C5 C 0.3749(3) 0.2321(4) 0.02041(12) 0.0937(16) Uani 1 1 d . . . H5A H 0.3879 0.1682 0.0108 0.112 Uiso 1 1 calc R . . C6 C 0.3938(3) 0.2434(3) 0.05166(11) 0.0774(12) Uani 1 1 d . . . H6A H 0.4192 0.1868 0.0629 0.093 Uiso 1 1 calc R . . C7 C 0.3748(2) 0.3397(3) 0.06645(8) 0.0517(8) Uani 1 1 d . . . C8 C 0.3928(2) 0.3514(3) 0.10035(8) 0.0528(8) Uani 1 1 d . . . H8A H 0.3471 0.3692 0.1086 0.063 Uiso 1 1 calc R . . H8B H 0.4108 0.2812 0.1089 0.063 Uiso 1 1 calc R . . C9 C 0.5214(2) 0.4058(4) 0.09963(10) 0.0706(11) Uani 1 1 d . . . H9A H 0.5347 0.3321 0.1063 0.106 Uiso 1 1 calc R . . H9B H 0.5600 0.4560 0.1081 0.106 Uiso 1 1 calc R . . H9C H 0.5160 0.4091 0.0778 0.106 Uiso 1 1 calc R . . C10 C 0.45982(19) 0.4421(3) 0.14388(7) 0.0519(8) Uani 1 1 d . . . H10A H 0.4843 0.3752 0.1521 0.062 Uiso 1 1 calc R . . H10B H 0.4113 0.4464 0.1508 0.062 Uiso 1 1 calc R . . C11 C 0.50672(19) 0.5415(3) 0.15563(8) 0.0566(9) Uani 1 1 d . . . H11A H 0.5060 0.5492 0.1774 0.068 Uiso 1 1 calc R . . H11B H 0.5582 0.5298 0.1524 0.068 Uiso 1 1 calc R . . C12 C 0.54051(19) 0.7102(3) 0.13111(8) 0.0621(10) Uani 1 1 d . . . H12A H 0.5766 0.7240 0.1488 0.093 Uiso 1 1 calc R . . H12B H 0.5216 0.7791 0.1225 0.093 Uiso 1 1 calc R . . H12C H 0.5640 0.6702 0.1163 0.093 Uiso 1 1 calc R . . C13 C 0.43641(17) 0.7143(3) 0.15912(7) 0.0466(8) Uani 1 1 d . . . H13A H 0.4135 0.7741 0.1466 0.056 Uiso 1 1 calc R . . H13B H 0.4724 0.7469 0.1749 0.056 Uiso 1 1 calc R . . C14 C 0.37626(16) 0.6592(3) 0.17422(7) 0.0413(7) Uani 1 1 d . . . C15 C 0.31643(16) 0.6038(2) 0.15642(6) 0.0362(6) Uani 1 1 d . . . C16 C 0.25781(16) 0.5625(2) 0.17152(6) 0.0366(6) Uani 1 1 d . . . C17 C 0.26389(17) 0.5742(3) 0.20290(7) 0.0425(7) Uani 1 1 d . . . H17A H 0.2260 0.5450 0.2127 0.051 Uiso 1 1 calc R . . C18 C 0.32346(17) 0.6270(3) 0.22056(7) 0.0431(7) Uani 1 1 d . . . C19 C 0.37821(17) 0.6692(3) 0.20546(7) 0.0450(7) Uani 1 1 d . . . H19A H 0.4183 0.7062 0.2166 0.054 Uiso 1 1 calc R . . C20 C 0.32497(19) 0.6366(3) 0.25538(7) 0.0503(8) Uani 1 1 d . . . C21 C 0.3884(3) 0.7114(3) 0.27011(8) 0.0706(11) Uani 1 1 d . . . H21A H 0.4357 0.6810 0.2667 0.106 Uiso 1 1 calc R . . H21B H 0.3866 0.7164 0.2916 0.106 Uiso 1 1 calc R . . H21C H 0.3826 0.7836 0.2612 0.106 Uiso 1 1 calc R . . C22 C 0.2512(3) 0.6889(5) 0.26178(9) 0.0896(15) Uani 1 1 d . . . H22A H 0.2099 0.6442 0.2529 0.134 Uiso 1 1 calc R . . H22B H 0.2465 0.7616 0.2531 0.134 Uiso 1 1 calc R . . H22C H 0.2510 0.6937 0.2834 0.134 Uiso 1 1 calc R . . C23 C 0.33813(18) 0.5224(3) 0.27022(7) 0.0500(8) Uani 1 1 d . . . C24 C 0.3953(2) 0.4576(3) 0.26254(9) 0.0639(10) Uani 1 1 d . . . H24A H 0.4218 0.4813 0.2472 0.077 Uiso 1 1 calc R . . C25 C 0.4146(3) 0.3586(4) 0.27690(11) 0.0888(14) Uani 1 1 d . . . H25A H 0.4541 0.3173 0.2714 0.107 Uiso 1 1 calc R . . C26 C 0.3758(4) 0.3215(4) 0.29908(12) 0.0959(16) Uani 1 1 d . . . H26A H 0.3892 0.2550 0.3089 0.115 Uiso 1 1 calc R . . C27 C 0.3189(3) 0.3797(5) 0.30686(11) 0.0945(16) Uani 1 1 d . . . H27A H 0.2917 0.3530 0.3216 0.113 Uiso 1 1 calc R . . C28 C 0.3001(3) 0.4817(4) 0.29270(9) 0.0819(13) Uani 1 1 d . . . H28A H 0.2611 0.5227 0.2987 0.098 Uiso 1 1 calc R . . C29 C 0.18836(16) 0.5106(2) 0.15283(7) 0.0399(7) Uani 1 1 d . . . C30 C 0.15087(18) 0.5963(3) 0.13038(8) 0.0521(8) Uani 1 1 d . . . H30A H 0.1856 0.6201 0.1172 0.078 Uiso 1 1 calc R . . H30B H 0.1357 0.6586 0.1414 0.078 Uiso 1 1 calc R . . H30C H 0.1077 0.5643 0.1184 0.078 Uiso 1 1 calc R . . C31 C 0.12940(18) 0.4769(3) 0.17329(8) 0.0546(9) Uani 1 1 d . . . H31A H 0.1504 0.4224 0.1877 0.082 Uiso 1 1 calc R . . H31B H 0.0862 0.4469 0.1609 0.082 Uiso 1 1 calc R . . H31C H 0.1150 0.5406 0.1840 0.082 Uiso 1 1 calc R . . C32 C 0.20859(16) 0.4042(3) 0.13723(7) 0.0410(7) Uani 1 1 d . . . C33 C 0.2495(2) 0.3232(3) 0.15430(9) 0.0586(9) Uani 1 1 d . . . H33A H 0.2689 0.3372 0.1745 0.070 Uiso 1 1 calc R . . C34 C 0.2621(3) 0.2206(3) 0.14146(12) 0.0771(13) Uani 1 1 d . . . H34A H 0.2886 0.1664 0.1534 0.093 Uiso 1 1 calc R . . C35 C 0.2361(2) 0.1995(4) 0.11181(12) 0.0766(13) Uani 1 1 d . . . H35A H 0.2445 0.1311 0.1034 0.092 Uiso 1 1 calc R . . C36 C 0.1975(2) 0.2791(4) 0.09437(10) 0.0707(12) Uani 1 1 d . . . H36A H 0.1806 0.2653 0.0739 0.085 Uiso 1 1 calc R . . C37 C 0.18342(18) 0.3805(3) 0.10687(8) 0.0532(8) Uani 1 1 d . . . H37A H 0.1566 0.4335 0.0947 0.064 Uiso 1 1 calc R . . C38 C 0.5010(3) 0.6216(4) 0.04616(11) 0.0871(14) Uani 1 1 d . . . H38A H 0.5326 0.6266 0.0305 0.131 Uiso 1 1 calc R . . H38B H 0.4705 0.5566 0.0430 0.131 Uiso 1 1 calc R . . H38C H 0.5314 0.6178 0.0657 0.131 Uiso 1 1 calc R . . C39 C 0.3811(3) 0.7379(5) 0.00602(9) 0.1010(17) Uani 1 1 d . . . H39A H 0.4029 0.7838 -0.0081 0.151 Uiso 1 1 calc R . . H39B H 0.3312 0.7628 0.0075 0.151 Uiso 1 1 calc R . . H39C H 0.3795 0.6629 -0.0010 0.151 Uiso 1 1 calc R . . C40 C 0.5035(3) 0.8692(4) 0.04289(12) 0.0936(15) Uani 1 1 d . . . H40A H 0.5048 0.8890 0.0220 0.140 Uiso 1 1 calc R . . H40B H 0.5531 0.8507 0.0524 0.140 Uiso 1 1 calc R . . H40C H 0.4849 0.9303 0.0534 0.140 Uiso 1 1 calc R . . C41 C 0.2989(3) 0.9415(4) 0.04794(11) 0.0848(14) Uani 1 1 d . . . H41A H 0.2650 0.8922 0.0360 0.127 Uiso 1 1 calc R . . H41B H 0.3361 0.9666 0.0360 0.127 Uiso 1 1 calc R . . H41C H 0.2716 1.0037 0.0541 0.127 Uiso 1 1 calc R . . C42 C 0.4107(3) 0.9724(3) 0.10408(11) 0.0835(13) Uani 1 1 d . . . H42A H 0.4368 0.9400 0.1223 0.125 Uiso 1 1 calc R . . H42B H 0.3817 1.0342 0.1094 0.125 Uiso 1 1 calc R . . H42C H 0.4462 0.9969 0.0913 0.125 Uiso 1 1 calc R . . C43 C 0.2692(3) 0.8440(4) 0.10653(11) 0.0804(13) Uani 1 1 d . . . H43A H 0.2346 0.7908 0.0967 0.121 Uiso 1 1 calc R . . H43B H 0.2436 0.9124 0.1087 0.121 Uiso 1 1 calc R . . H43C H 0.2900 0.8173 0.1263 0.121 Uiso 1 1 calc R . . C44 C 0.5000 0.0526(18) 0.2500 0.333(18) Uani 1 2 d S . . H44A H 0.4618 0.0996 0.2560 0.400 Uiso 1 1 d R . . C45 C 0.461(2) -0.0091(11) 0.2197(9) 0.54(3) Uani 1 1 d . . . H45A H 0.4969 -0.0550 0.2112 0.648 Uiso 1 1 calc R . . H45B H 0.4198 -0.0550 0.2241 0.648 Uiso 1 1 calc R . . C46 C 0.4343(7) 0.0774(18) 0.1990(4) 0.334(12) Uani 1 1 d . . . H46A H 0.4048 0.0463 0.1813 0.502 Uiso 1 1 calc R . . H46B H 0.4762 0.1164 0.1929 0.502 Uiso 1 1 calc R . . H46C H 0.4041 0.1274 0.2088 0.502 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 Mg1 0.0382(5) 0.0414(6) 0.0326(5) 0.0056(4) 0.0020(4) -0.0061(4) Si1 0.0667(6) 0.0706(7) 0.0447(5) 0.0141(5) 0.0087(4) -0.0181(5) Si2 0.0691(7) 0.0443(5) 0.0568(6) 0.0134(4) -0.0017(5) -0.0079(5) O1 0.0585(14) 0.0527(14) 0.0422(12) -0.0043(10) -0.0062(10) -0.0003(11) O2 0.0394(11) 0.0483(12) 0.0273(10) 0.0012(9) 0.0011(8) -0.0107(9) N1 0.0452(14) 0.0500(16) 0.0445(15) 0.0053(12) 0.0087(11) -0.0003(12) N2 0.0381(13) 0.0539(16) 0.0418(14) 0.0090(12) -0.0019(11) -0.0116(12) N3 0.0551(16) 0.0497(16) 0.0406(14) 0.0111(12) 0.0040(12) -0.0130(13) C1 0.054(2) 0.075(3) 0.060(2) 0.0015(19) -0.0102(17) 0.0025(19) C2 0.059(2) 0.051(2) 0.0464(18) -0.0076(16) 0.0103(15) -0.0181(16) C3 0.090(3) 0.076(3) 0.043(2) -0.0048(19) 0.0094(19) -0.021(2) C4 0.130(4) 0.094(4) 0.050(2) -0.026(2) 0.028(3) -0.033(3) C5 0.139(5) 0.071(3) 0.082(3) -0.029(3) 0.053(3) -0.018(3) C6 0.099(3) 0.055(2) 0.085(3) -0.009(2) 0.038(2) -0.005(2) C7 0.062(2) 0.0462(19) 0.0493(19) -0.0030(15) 0.0177(16) -0.0116(16) C8 0.060(2) 0.0445(19) 0.055(2) 0.0066(15) 0.0128(16) -0.0044(16) C9 0.052(2) 0.074(3) 0.089(3) 0.009(2) 0.019(2) 0.0093(19) C10 0.0535(19) 0.052(2) 0.0471(19) 0.0145(15) -0.0023(15) 0.0048(16) C11 0.0483(19) 0.069(2) 0.0482(19) 0.0090(17) -0.0087(15) 0.0011(17) C12 0.0478(19) 0.079(3) 0.058(2) 0.0029(19) 0.0028(16) -0.0249(19) C13 0.0476(17) 0.0474(18) 0.0421(17) 0.0020(14) -0.0031(14) -0.0167(15) C14 0.0398(16) 0.0444(17) 0.0374(16) 0.0010(13) -0.0027(12) -0.0108(13) C15 0.0398(15) 0.0370(15) 0.0304(14) 0.0015(12) -0.0006(11) -0.0041(12) C16 0.0383(15) 0.0345(15) 0.0361(15) -0.0007(12) 0.0019(12) -0.0035(12) C17 0.0452(17) 0.0458(17) 0.0369(16) -0.0002(13) 0.0065(13) -0.0034(14) C18 0.0481(17) 0.0469(18) 0.0326(15) -0.0011(13) 0.0002(13) -0.0007(14) C19 0.0465(17) 0.0469(18) 0.0378(16) -0.0031(13) -0.0070(13) -0.0087(14) C20 0.0575(19) 0.060(2) 0.0318(16) -0.0066(14) 0.0008(14) 0.0037(16) C21 0.109(3) 0.061(2) 0.0371(18) -0.0090(16) -0.0034(19) -0.015(2) C22 0.091(3) 0.127(4) 0.050(2) -0.017(2) 0.009(2) 0.043(3) C23 0.0508(19) 0.066(2) 0.0312(15) -0.0029(15) 0.0008(13) -0.0126(17) C24 0.074(3) 0.060(2) 0.058(2) 0.0056(18) 0.0092(18) 0.001(2) C25 0.115(4) 0.066(3) 0.080(3) 0.003(2) -0.003(3) 0.010(3) C26 0.135(5) 0.071(3) 0.073(3) 0.014(3) -0.012(3) -0.026(3) C27 0.113(4) 0.105(4) 0.066(3) 0.026(3) 0.019(3) -0.033(3) C28 0.083(3) 0.110(4) 0.056(2) 0.012(2) 0.017(2) -0.010(3) C29 0.0381(15) 0.0420(17) 0.0398(16) -0.0042(13) 0.0064(12) -0.0082(13) C30 0.0424(17) 0.0512(19) 0.059(2) -0.0033(16) -0.0057(15) -0.0015(15) C31 0.0468(18) 0.059(2) 0.061(2) -0.0122(17) 0.0184(16) -0.0161(16) C32 0.0374(15) 0.0422(17) 0.0454(17) -0.0044(14) 0.0131(13) -0.0131(13) C33 0.069(2) 0.049(2) 0.061(2) 0.0060(17) 0.0184(18) -0.0032(18) C34 0.088(3) 0.042(2) 0.109(4) 0.009(2) 0.038(3) 0.006(2) C35 0.078(3) 0.053(2) 0.107(4) -0.028(2) 0.043(3) -0.017(2) C36 0.068(2) 0.074(3) 0.073(3) -0.033(2) 0.020(2) -0.023(2) C37 0.0489(18) 0.058(2) 0.053(2) -0.0169(16) 0.0089(15) -0.0120(16) C38 0.093(3) 0.089(3) 0.087(3) 0.007(3) 0.038(3) -0.006(3) C39 0.121(4) 0.136(5) 0.044(2) 0.011(3) 0.006(2) -0.015(3) C40 0.101(3) 0.094(3) 0.091(3) 0.014(3) 0.033(3) -0.039(3) C41 0.101(3) 0.063(3) 0.082(3) 0.018(2) -0.019(3) 0.005(2) C42 0.102(3) 0.054(2) 0.089(3) 0.004(2) -0.006(3) -0.016(2) C43 0.086(3) 0.056(2) 0.104(4) 0.014(2) 0.030(3) 0.010(2) C44 0.52(5) 0.109(14) 0.40(4) 0.000 0.16(4) 0.000 C45 0.77(6) 0.116(9) 0.91(7) -0.013(18) 0.72(6) 0.001(18) C46 0.140(9) 0.48(3) 0.38(3) -0.15(2) 0.027(12) 0.093(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O2 1.928(2) . ? Mg1 N3 2.062(3) . ? Mg1 O1 2.201(2) . ? Mg1 N2 2.228(3) . ? Mg1 N1 2.324(3) . ? Si1 N3 1.703(3) . ? Si1 C38 1.867(5) . ? Si1 C39 1.879(4) . ? Si1 C40 1.894(4) . ? Si2 N3 1.698(3) . ? Si2 C43 1.871(4) . ? Si2 C42 1.885(4) . ? Si2 C41 1.895(4) . ? O1 C2 1.391(4) . ? O1 C1 1.438(4) . ? O2 C15 1.322(3) . ? N1 C8 1.478(4) . ? N1 C10 1.486(4) . ? N1 C9 1.487(4) . ? N2 C13 1.477(4) . ? N2 C12 1.481(4) . ? N2 C11 1.484(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C7 1.377(5) . ? C2 C3 1.377(5) . ? C3 C4 1.391(6) . ? C3 H3A 0.9300 . ? C4 C5 1.355(7) . ? C4 H4A 0.9300 . ? C5 C6 1.385(7) . ? C5 H5A 0.9300 . ? C6 C7 1.405(5) . ? C6 H6A 0.9300 . ? C7 C8 1.498(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.521(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.508(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C19 1.385(4) . ? C14 C15 1.413(4) . ? C15 C16 1.419(4) . ? C16 C17 1.387(4) . ? C16 C29 1.536(4) . ? C17 C18 1.393(4) . ? C17 H17A 0.9300 . ? C18 C19 1.368(4) . ? C18 C20 1.544(4) . ? C19 H19A 0.9300 . ? C20 C21 1.531(5) . ? C20 C22 1.536(5) . ? C20 C23 1.536(5) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C28 1.377(5) . ? C23 C24 1.377(5) . ? C24 C25 1.379(6) . ? C24 H24A 0.9300 . ? C25 C26 1.360(7) . ? C25 H25A 0.9300 . ? C26 C27 1.330(7) . ? C26 H26A 0.9300 . ? C27 C28 1.407(7) . ? C27 H27A 0.9300 . ? C28 H28A 0.9300 . ? C29 C30 1.529(4) . ? C29 C32 1.531(4) . ? C29 C31 1.546(4) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C33 1.387(5) . ? C32 C37 1.388(4) . ? C33 C34 1.399(5) . ? C33 H33A 0.9300 . ? C34 C35 1.355(6) . ? C34 H34A 0.9300 . ? C35 C36 1.364(6) . ? C35 H35A 0.9300 . ? C36 C37 1.385(5) . ? C36 H36A 0.9300 . ? C37 H37A 0.9300 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 C45 1.61(4) 2_655 ? C44 C45 1.61(4) . ? C44 H44A 0.9600 . ? C45 C46 1.43(3) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? 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 O2 Mg1 N3 118.09(11) . . ? O2 Mg1 O1 89.54(9) . . ? N3 Mg1 O1 93.93(10) . . ? O2 Mg1 N2 91.16(9) . . ? N3 Mg1 N2 102.36(11) . . ? O1 Mg1 N2 161.09(10) . . ? O2 Mg1 N1 97.81(9) . . ? N3 Mg1 N1 144.03(11) . . ? O1 Mg1 N1 83.71(9) . . ? N2 Mg1 N1 77.48(10) . . ? N3 Si1 C38 111.14(17) . . ? N3 Si1 C39 115.2(2) . . ? C38 Si1 C39 104.2(3) . . ? N3 Si1 C40 113.70(19) . . ? C38 Si1 C40 106.0(2) . . ? C39 Si1 C40 105.7(2) . . ? N3 Si2 C43 113.78(16) . . ? N3 Si2 C42 113.92(19) . . ? C43 Si2 C42 106.1(2) . . ? N3 Si2 C41 113.22(19) . . ? C43 Si2 C41 104.0(2) . . ? C42 Si2 C41 104.9(2) . . ? C2 O1 C1 116.5(3) . . ? C2 O1 Mg1 128.5(2) . . ? C1 O1 Mg1 114.0(2) . . ? C15 O2 Mg1 132.90(17) . . ? C8 N1 C10 107.8(2) . . ? C8 N1 C9 109.2(3) . . ? C10 N1 C9 109.3(3) . . ? C8 N1 Mg1 106.98(19) . . ? C10 N1 Mg1 98.11(19) . . ? C9 N1 Mg1 124.2(2) . . ? C13 N2 C12 107.9(3) . . ? C13 N2 C11 112.6(3) . . ? C12 N2 C11 110.3(3) . . ? C13 N2 Mg1 102.32(18) . . ? C12 N2 Mg1 112.3(2) . . ? C11 N2 Mg1 111.13(19) . . ? Si2 N3 Si1 119.92(15) . . ? Si2 N3 Mg1 123.33(15) . . ? Si1 N3 Mg1 116.71(16) . . ? 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 . . ? C7 C2 C3 121.8(4) . . ? C7 C2 O1 115.9(3) . . ? C3 C2 O1 122.3(3) . . ? C2 C3 C4 119.0(4) . . ? C2 C3 H3A 120.5 . . ? C4 C3 H3A 120.5 . . ? C5 C4 C3 120.7(4) . . ? C5 C4 H4A 119.7 . . ? C3 C4 H4A 119.7 . . ? C4 C5 C6 120.2(4) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? C5 C6 C7 120.4(5) . . ? C5 C6 H6A 119.8 . . ? C7 C6 H6A 119.8 . . ? C2 C7 C6 117.9(4) . . ? C2 C7 C8 121.1(3) . . ? C6 C7 C8 120.9(4) . . ? N1 C8 C7 113.6(3) . . ? N1 C8 H8A 108.8 . . ? C7 C8 H8A 108.8 . . ? N1 C8 H8B 108.8 . . ? C7 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 C11 111.3(3) . . ? N1 C10 H10A 109.4 . . ? C11 C10 H10A 109.4 . . ? N1 C10 H10B 109.4 . . ? C11 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? N2 C11 C10 111.2(2) . . ? N2 C11 H11A 109.4 . . ? C10 C11 H11A 109.4 . . ? N2 C11 H11B 109.4 . . ? C10 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? N2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 C14 117.0(3) . . ? N2 C13 H13A 108.0 . . ? C14 C13 H13A 108.0 . . ? N2 C13 H13B 108.0 . . ? C14 C13 H13B 108.0 . . ? H13A C13 H13B 107.3 . . ? C19 C14 C15 120.6(3) . . ? C19 C14 C13 119.0(3) . . ? C15 C14 C13 120.2(3) . . ? O2 C15 C14 121.0(3) . . ? O2 C15 C16 121.3(2) . . ? C14 C15 C16 117.7(3) . . ? C17 C16 C15 118.5(3) . . ? C17 C16 C29 121.7(3) . . ? C15 C16 C29 119.7(2) . . ? C16 C17 C18 123.8(3) . . ? C16 C17 H17A 118.1 . . ? C18 C17 H17A 118.1 . . ? C19 C18 C17 116.7(3) . . ? C19 C18 C20 123.2(3) . . ? C17 C18 C20 120.0(3) . . ? C18 C19 C14 122.5(3) . . ? C18 C19 H19A 118.7 . . ? C14 C19 H19A 118.7 . . ? C21 C20 C22 107.0(3) . . ? C21 C20 C23 106.8(3) . . ? C22 C20 C23 112.2(3) . . ? C21 C20 C18 112.2(3) . . ? C22 C20 C18 108.8(3) . . ? C23 C20 C18 109.8(3) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C28 C23 C24 116.1(4) . . ? C28 C23 C20 124.7(4) . . ? C24 C23 C20 119.0(3) . . ? C23 C24 C25 122.1(4) . . ? C23 C24 H24A 119.0 . . ? C25 C24 H24A 119.0 . . ? C26 C25 C24 119.9(5) . . ? C26 C25 H25A 120.0 . . ? C24 C25 H25A 120.0 . . ? C27 C26 C25 120.4(5) . . ? C27 C26 H26A 119.8 . . ? C25 C26 H26A 119.8 . . ? C26 C27 C28 119.8(5) . . ? C26 C27 H27A 120.1 . . ? C28 C27 H27A 120.1 . . ? C23 C28 C27 121.6(5) . . ? C23 C28 H28A 119.2 . . ? C27 C28 H28A 119.2 . . ? C30 C29 C32 113.0(3) . . ? C30 C29 C16 108.9(2) . . ? C32 C29 C16 111.1(2) . . ? C30 C29 C31 106.4(3) . . ? C32 C29 C31 105.6(2) . . ? C16 C29 C31 111.6(2) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C37 117.3(3) . . ? C33 C32 C29 119.5(3) . . ? C37 C32 C29 123.1(3) . . ? C32 C33 C34 120.8(4) . . ? C32 C33 H33A 119.6 . . ? C34 C33 H33A 119.6 . . ? C35 C34 C33 120.5(4) . . ? C35 C34 H34A 119.8 . . ? C33 C34 H34A 119.8 . . ? C34 C35 C36 119.7(4) . . ? C34 C35 H35A 120.1 . . ? C36 C35 H35A 120.1 . . ? C35 C36 C37 120.6(4) . . ? C35 C36 H36A 119.7 . . ? C37 C36 H36A 119.7 . . ? C36 C37 C32 121.2(4) . . ? C36 C37 H37A 119.4 . . ? C32 C37 H37A 119.4 . . ? Si1 C38 H38A 109.5 . . ? Si1 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si1 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si1 C39 H39A 109.5 . . ? Si1 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si1 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si1 C40 H40A 109.5 . . ? Si1 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Si1 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Si2 C41 H41A 109.5 . . ? Si2 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si2 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si2 C42 H42A 109.5 . . ? Si2 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si2 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Si2 C43 H43A 109.5 . . ? Si2 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si2 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C45 125(3) 2_655 . ? C45 C44 H44A 106.9 2_655 . ? C45 C44 H44A 105.0 . . ? C46 C45 C44 105.2(13) . . ? C46 C45 H45A 110.7 . . ? C44 C45 H45A 110.7 . . ? C46 C45 H45B 110.7 . . ? C44 C45 H45B 110.7 . . ? H45A C45 H45B 108.8 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.329 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.058 _database_code_depnum_ccdc_archive 'CCDC 937977' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cd211292 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H55 Mg N3 O2 Si2' _chemical_formula_weight 582.27 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' Mg Mg 0.0486 0.0363 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.9422(11) _cell_length_b 17.3627(13) _cell_length_c 14.9983(12) _cell_angle_alpha 90.00 _cell_angle_beta 114.3660(10) _cell_angle_gamma 90.00 _cell_volume 3544.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2803 _cell_measurement_theta_min 4.692 _cell_measurement_theta_max 41.610 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.268 _exptl_crystal_size_mid 0.213 _exptl_crystal_size_min 0.169 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.091 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 0.147 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.47141 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19159 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_sigmaI/netI 0.0598 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6957 _reflns_number_gt 3880 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0770P)^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 6957 _refine_ls_number_parameters 403 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1084 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1510 _refine_ls_wR_factor_gt 0.1254 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.22845(6) 0.63281(5) 0.31439(6) 0.0436(2) Uani 1 1 d . . . Si1 Si 0.13647(7) 0.60168(5) 0.46267(7) 0.0653(3) Uani 1 1 d . . . Si2 Si 0.16492(7) 0.46572(5) 0.35450(7) 0.0658(3) Uani 1 1 d . . . N1 N 0.26420(15) 0.75895(11) 0.33637(15) 0.0487(5) Uani 1 1 d . . . N2 N 0.38943(15) 0.63011(12) 0.40837(15) 0.0511(5) Uani 1 1 d . . . N3 N 0.17194(14) 0.55970(12) 0.38169(15) 0.0495(5) Uani 1 1 d . . . O1 O 0.07905(12) 0.67650(10) 0.21085(13) 0.0568(5) Uani 1 1 d . . . O2 O 0.24835(12) 0.59962(10) 0.20219(12) 0.0507(4) Uani 1 1 d . . . C1 C 0.0356(2) 0.74252(16) 0.22627(19) 0.0552(7) Uani 1 1 d . . . C2 C -0.0582(2) 0.7443(2) 0.2210(2) 0.0723(9) Uani 1 1 d . . . H2 H -0.0974 0.7004 0.2039 0.087 Uiso 1 1 calc R . . C3 C -0.0933(3) 0.8120(3) 0.2413(3) 0.0940(12) Uani 1 1 d . . . H3 H -0.1563 0.8136 0.2394 0.113 Uiso 1 1 calc R . . C4 C -0.0380(3) 0.8763(3) 0.2641(2) 0.0950(13) Uani 1 1 d . . . H4 H -0.0632 0.9219 0.2768 0.114 Uiso 1 1 calc R . . C5 C 0.0557(3) 0.87454(18) 0.2685(2) 0.0779(10) Uani 1 1 d . . . H5 H 0.0937 0.9191 0.2848 0.093 Uiso 1 1 calc R . . C6 C 0.0943(2) 0.80735(16) 0.24896(19) 0.0560(7) Uani 1 1 d . . . C7 C 0.1950(2) 0.80412(15) 0.2519(2) 0.0598(8) Uani 1 1 d . . . H7A H 0.2199 0.8561 0.2556 0.072 Uiso 1 1 calc R . . H7B H 0.1918 0.7812 0.1917 0.072 Uiso 1 1 calc R . . C8 C 0.3606(2) 0.75795(16) 0.3314(2) 0.0621(8) Uani 1 1 d . . . H8A H 0.3865 0.8100 0.3395 0.075 Uiso 1 1 calc R . . H8B H 0.3527 0.7397 0.2675 0.075 Uiso 1 1 calc R . . C9 C 0.4330(2) 0.70669(17) 0.4096(2) 0.0645(8) Uani 1 1 d . . . H9A H 0.4920 0.7010 0.3983 0.077 Uiso 1 1 calc R . . H9B H 0.4511 0.7303 0.4733 0.077 Uiso 1 1 calc R . . C10 C 0.42779(18) 0.57150(16) 0.35985(19) 0.0545(7) Uani 1 1 d . . . H10A H 0.4962 0.5617 0.4019 0.065 Uiso 1 1 calc R . . H10B H 0.3921 0.5238 0.3542 0.065 Uiso 1 1 calc R . . C11 C 0.42041(18) 0.59308(14) 0.26095(18) 0.0485(6) Uani 1 1 d . . . C12 C 0.5050(2) 0.60264(15) 0.2456(2) 0.0572(7) Uani 1 1 d . . . H12 H 0.5656 0.5980 0.2987 0.069 Uiso 1 1 calc R . . C13 C 0.5029(2) 0.61866(15) 0.1555(2) 0.0572(7) Uani 1 1 d . A . C14 C 0.4103(2) 0.62120(15) 0.0783(2) 0.0585(7) Uani 1 1 d . . . H14 H 0.4068 0.6296 0.0157 0.070 Uiso 1 1 calc R . . C15 C 0.32290(19) 0.61205(14) 0.08847(19) 0.0480(6) Uani 1 1 d . . . C16 C 0.32752(18) 0.60132(14) 0.18319(18) 0.0451(6) Uani 1 1 d . . . C17 C 0.0159(2) 0.61501(17) 0.1567(2) 0.0716(9) Uani 1 1 d . . . H17A H -0.0137 0.5914 0.1958 0.107 Uiso 1 1 calc R . . H17B H 0.0537 0.5774 0.1403 0.107 Uiso 1 1 calc R . . H17C H -0.0346 0.6351 0.0978 0.107 Uiso 1 1 calc R . . C18 C 0.2729(2) 0.79685(16) 0.4279(2) 0.0634(8) Uani 1 1 d . . . H18A H 0.3152 0.7669 0.4830 0.095 Uiso 1 1 calc R . . H18B H 0.2091 0.8007 0.4286 0.095 Uiso 1 1 calc R . . H18C H 0.3001 0.8475 0.4315 0.095 Uiso 1 1 calc R . . C19 C 0.4129(2) 0.60316(19) 0.50849(19) 0.0682(8) Uani 1 1 d . . . H19A H 0.4829 0.6007 0.5444 0.102 Uiso 1 1 calc R . . H19B H 0.3852 0.5529 0.5061 0.102 Uiso 1 1 calc R . . H19C H 0.3859 0.6383 0.5403 0.102 Uiso 1 1 calc R . . C20 C 0.2241(2) 0.61114(16) -0.00077(19) 0.0560(7) Uani 1 1 d . . . C21 C 0.1734(2) 0.53433(17) -0.0048(2) 0.0764(9) Uani 1 1 d . . . H21A H 0.1670 0.5262 0.0556 0.115 Uiso 1 1 calc R . . H21B H 0.2118 0.4935 -0.0145 0.115 Uiso 1 1 calc R . . H21C H 0.1094 0.5349 -0.0580 0.115 Uiso 1 1 calc R . . C22 C 0.1584(2) 0.67676(17) 0.0040(2) 0.0726(9) Uani 1 1 d . . . H22A H 0.1490 0.6728 0.0634 0.109 Uiso 1 1 calc R . . H22B H 0.0960 0.6737 -0.0512 0.109 Uiso 1 1 calc R . . H22C H 0.1890 0.7252 0.0028 0.109 Uiso 1 1 calc R . . C23 C 0.2360(2) 0.6208(2) -0.0972(2) 0.0876(11) Uani 1 1 d . . . H23A H 0.1729 0.6172 -0.1513 0.131 Uiso 1 1 calc R . . H23B H 0.2782 0.5810 -0.1024 0.131 Uiso 1 1 calc R . . H23C H 0.2644 0.6702 -0.0980 0.131 Uiso 1 1 calc R . . C24 C 0.5954(2) 0.6344(2) 0.1397(2) 0.0740(9) Uani 1 1 d D . . C25 C 0.5928(8) 0.7145(5) 0.1037(10) 0.123(4) Uani 0.55 1 d PDU A 1 H25A H 0.6546 0.7265 0.1015 0.185 Uiso 0.55 1 calc PR A 1 H25B H 0.5809 0.7497 0.1470 0.185 Uiso 0.55 1 calc PR A 1 H25C H 0.5411 0.7191 0.0392 0.185 Uiso 0.55 1 calc PR A 1 C26 C 0.5971(7) 0.5797(6) 0.0592(9) 0.124(4) Uani 0.55 1 d PDU A 1 H26A H 0.5459 0.5940 -0.0027 0.186 Uiso 0.55 1 calc PR A 1 H26B H 0.5868 0.5277 0.0747 0.186 Uiso 0.55 1 calc PR A 1 H26C H 0.6596 0.5835 0.0555 0.186 Uiso 0.55 1 calc PR A 1 C27 C 0.6890(7) 0.6199(8) 0.2297(8) 0.129(5) Uani 0.55 1 d PDU A 1 H27A H 0.6890 0.5680 0.2519 0.194 Uiso 0.55 1 calc PR A 1 H27B H 0.6930 0.6552 0.2805 0.194 Uiso 0.55 1 calc PR A 1 H27C H 0.7445 0.6272 0.2140 0.194 Uiso 0.55 1 calc PR A 1 C25' C 0.6361(10) 0.7135(8) 0.1884(12) 0.144(5) Uani 0.45 1 d PDU A 2 H25D H 0.6803 0.7337 0.1624 0.216 Uiso 0.45 1 calc PR A 2 H25E H 0.6706 0.7068 0.2579 0.216 Uiso 0.45 1 calc PR A 2 H25F H 0.5826 0.7487 0.1748 0.216 Uiso 0.45 1 calc PR A 2 C26' C 0.5796(10) 0.6393(12) 0.0350(9) 0.149(5) Uani 0.45 1 d PDU A 2 H26D H 0.5388 0.6829 0.0050 0.224 Uiso 0.45 1 calc PR A 2 H26E H 0.5479 0.5932 0.0016 0.224 Uiso 0.45 1 calc PR A 2 H26F H 0.6418 0.6449 0.0311 0.224 Uiso 0.45 1 calc PR A 2 C27' C 0.6713(10) 0.5731(8) 0.1861(12) 0.133(6) Uani 0.45 1 d PDU A 2 H27D H 0.6430 0.5235 0.1630 0.200 Uiso 0.45 1 calc PR A 2 H27E H 0.6937 0.5754 0.2560 0.200 Uiso 0.45 1 calc PR A 2 H27F H 0.7259 0.5814 0.1691 0.200 Uiso 0.45 1 calc PR A 2 C28 C 0.0028(3) 0.6045(2) 0.4270(3) 0.1005(12) Uani 1 1 d . . . H28A H -0.0294 0.6247 0.3618 0.151 Uiso 1 1 calc R . . H28B H -0.0111 0.6369 0.4716 0.151 Uiso 1 1 calc R . . H28C H -0.0207 0.5534 0.4290 0.151 Uiso 1 1 calc R . . C29 C 0.1926(3) 0.5613(2) 0.5884(2) 0.1018(12) Uani 1 1 d . . . H29A H 0.1695 0.5096 0.5878 0.153 Uiso 1 1 calc R . . H29B H 0.1744 0.5924 0.6312 0.153 Uiso 1 1 calc R . . H29C H 0.2628 0.5610 0.6113 0.153 Uiso 1 1 calc R . . C30 C 0.0425(3) 0.4215(2) 0.3152(3) 0.1129(14) Uani 1 1 d . . . H30A H 0.0236 0.4207 0.3691 0.169 Uiso 1 1 calc R . . H30B H 0.0444 0.3697 0.2935 0.169 Uiso 1 1 calc R . . H30C H -0.0045 0.4509 0.2624 0.169 Uiso 1 1 calc R . . C31 C 0.2484(3) 0.4026(2) 0.4515(4) 0.143(2) Uani 1 1 d . . . H31A H 0.3152 0.4155 0.4647 0.214 Uiso 1 1 calc R . . H31B H 0.2361 0.3499 0.4306 0.214 Uiso 1 1 calc R . . H31C H 0.2376 0.4094 0.5098 0.214 Uiso 1 1 calc R . . H1 H 0.1675(18) 0.6789(15) 0.4741(19) 0.080(8) Uiso 1 1 d . . . H2A H 0.1899(18) 0.4566(15) 0.2703(19) 0.080(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0410(5) 0.0441(5) 0.0461(5) -0.0012(4) 0.0183(4) -0.0025(4) Si1 0.0843(6) 0.0543(5) 0.0778(6) -0.0072(4) 0.0541(5) -0.0145(4) Si2 0.0805(6) 0.0480(5) 0.0814(6) -0.0007(4) 0.0461(5) -0.0031(4) N1 0.0530(13) 0.0473(12) 0.0476(13) -0.0029(10) 0.0226(10) -0.0093(10) N2 0.0440(13) 0.0620(14) 0.0449(13) -0.0013(11) 0.0160(10) -0.0053(10) N3 0.0504(13) 0.0483(12) 0.0551(13) 0.0014(10) 0.0272(10) -0.0033(10) O1 0.0473(11) 0.0475(11) 0.0691(13) -0.0003(9) 0.0176(9) 0.0019(8) O2 0.0403(10) 0.0656(11) 0.0470(10) -0.0047(8) 0.0188(8) -0.0019(8) C1 0.0564(19) 0.0569(17) 0.0521(17) 0.0124(13) 0.0220(13) 0.0155(14) C2 0.059(2) 0.084(2) 0.074(2) 0.0200(17) 0.0266(16) 0.0176(17) C3 0.081(3) 0.124(4) 0.080(3) 0.019(2) 0.037(2) 0.047(3) C4 0.108(3) 0.105(3) 0.062(2) 0.004(2) 0.025(2) 0.058(3) C5 0.104(3) 0.062(2) 0.056(2) 0.0062(15) 0.0205(18) 0.0239(19) C6 0.067(2) 0.0519(17) 0.0450(16) 0.0102(13) 0.0190(14) 0.0121(14) C7 0.080(2) 0.0443(15) 0.0560(18) 0.0046(13) 0.0286(16) -0.0077(14) C8 0.068(2) 0.0523(17) 0.074(2) -0.0085(15) 0.0369(16) -0.0221(14) C9 0.0471(18) 0.076(2) 0.068(2) -0.0162(16) 0.0208(15) -0.0174(15) C10 0.0412(16) 0.0643(17) 0.0548(17) 0.0076(14) 0.0164(13) 0.0047(13) C11 0.0438(16) 0.0556(16) 0.0484(16) 0.0058(12) 0.0214(13) 0.0054(12) C12 0.0456(17) 0.0661(18) 0.0570(18) 0.0055(14) 0.0183(14) 0.0042(13) C13 0.0545(19) 0.0597(18) 0.065(2) 0.0076(14) 0.0326(16) 0.0021(13) C14 0.069(2) 0.0625(18) 0.0505(17) 0.0080(13) 0.0313(15) 0.0062(14) C15 0.0495(17) 0.0458(15) 0.0490(16) 0.0008(12) 0.0207(13) 0.0057(12) C16 0.0454(16) 0.0425(14) 0.0486(16) -0.0012(11) 0.0204(13) 0.0018(11) C17 0.0510(19) 0.0672(19) 0.077(2) -0.0075(16) 0.0071(15) -0.0065(14) C18 0.071(2) 0.0557(17) 0.0613(19) -0.0107(14) 0.0255(15) -0.0091(14) C19 0.0561(19) 0.099(2) 0.0430(17) 0.0015(16) 0.0138(13) -0.0003(16) C20 0.0563(18) 0.0613(17) 0.0449(16) -0.0009(13) 0.0155(13) 0.0065(13) C21 0.073(2) 0.069(2) 0.073(2) -0.0164(17) 0.0162(17) -0.0076(16) C22 0.070(2) 0.072(2) 0.064(2) 0.0030(16) 0.0163(16) 0.0212(16) C23 0.084(3) 0.123(3) 0.0477(19) 0.0023(18) 0.0198(17) 0.015(2) C24 0.062(2) 0.088(2) 0.084(2) 0.0195(19) 0.0422(19) 0.0002(17) C25 0.115(7) 0.102(6) 0.189(10) 0.049(7) 0.099(7) -0.002(5) C26 0.100(6) 0.153(8) 0.166(9) -0.009(7) 0.102(7) 0.013(6) C27 0.056(5) 0.215(12) 0.119(7) 0.065(8) 0.039(5) -0.002(7) C25' 0.126(10) 0.128(9) 0.223(13) -0.054(10) 0.116(10) -0.067(8) C26' 0.114(9) 0.244(14) 0.127(9) -0.002(10) 0.087(7) -0.057(10) C27' 0.094(9) 0.152(10) 0.198(15) 0.042(9) 0.104(10) 0.033(8) C28 0.097(3) 0.123(3) 0.109(3) 0.032(2) 0.070(2) 0.032(2) C29 0.090(3) 0.155(4) 0.066(2) -0.010(2) 0.0380(19) -0.037(2) C30 0.114(3) 0.079(3) 0.132(4) -0.016(2) 0.036(3) -0.038(2) C31 0.141(4) 0.073(3) 0.168(5) 0.021(3) 0.017(3) 0.032(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 Mg1 O2 1.9145(19) . ? Mg1 N3 2.012(2) . ? Mg1 N2 2.231(2) . ? Mg1 N1 2.246(2) . ? Mg1 O1 2.2605(18) . ? Mg1 Si1 3.1063(12) . ? Mg1 Si2 3.1860(11) . ? Si1 N3 1.679(2) . ? Si1 C28 1.843(4) . ? Si1 C29 1.857(3) . ? Si1 H1 1.41(3) . ? Si2 N3 1.675(2) . ? Si2 C31 1.837(4) . ? Si2 C30 1.843(4) . ? Si2 H2A 1.47(3) . ? N1 C8 1.473(3) . ? N1 C18 1.479(3) . ? N1 C7 1.486(3) . ? N2 C19 1.470(3) . ? N2 C9 1.477(3) . ? N2 C10 1.496(3) . ? O1 C1 1.383(3) . ? O1 C17 1.434(3) . ? O2 C16 1.327(3) . ? C1 C2 1.371(4) . ? C1 C6 1.381(4) . ? C2 C3 1.372(5) . ? C2 H2 0.9300 . ? C3 C4 1.346(5) . ? C3 H3 0.9300 . ? C4 C5 1.375(5) . ? C4 H4 0.9300 . ? C5 C6 1.385(4) . ? C5 H5 0.9300 . ? C6 C7 1.487(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.513(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.489(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.385(3) . ? C11 C16 1.404(3) . ? C12 C13 1.367(4) . ? C12 H12 0.9300 . ? C13 C14 1.391(4) . ? C13 C24 1.521(4) . ? C14 C15 1.384(4) . ? C14 H14 0.9300 . ? C15 C16 1.406(3) . ? C15 C20 1.530(4) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.523(4) . ? C20 C22 1.525(4) . ? C20 C23 1.537(4) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.487(8) . ? C24 C26' 1.491(11) . ? C24 C27' 1.500(11) . ? C24 C27 1.511(9) . ? C24 C26 1.545(9) . ? C24 C25' 1.556(10) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C25' H25D 0.9600 . ? C25' H25E 0.9600 . ? C25' H25F 0.9600 . ? C26' H26D 0.9600 . ? C26' H26E 0.9600 . ? C26' H26F 0.9600 . ? C27' H27D 0.9600 . ? C27' H27E 0.9600 . ? C27' H27F 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? 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 O2 Mg1 N3 120.04(9) . . ? O2 Mg1 N2 91.78(8) . . ? N3 Mg1 N2 103.65(9) . . ? O2 Mg1 N1 107.99(8) . . ? N3 Mg1 N1 131.70(9) . . ? N2 Mg1 N1 78.38(8) . . ? O2 Mg1 O1 87.98(7) . . ? N3 Mg1 O1 93.24(8) . . ? N2 Mg1 O1 160.53(8) . . ? N1 Mg1 O1 83.18(7) . . ? O2 Mg1 Si1 148.43(6) . . ? N3 Mg1 Si1 29.50(6) . . ? N2 Mg1 Si1 102.95(6) . . ? N1 Mg1 Si1 102.31(6) . . ? O1 Mg1 Si1 86.96(6) . . ? O2 Mg1 Si2 93.34(6) . . ? N3 Mg1 Si2 27.28(6) . . ? N2 Mg1 Si2 100.90(6) . . ? N1 Mg1 Si2 158.67(7) . . ? O1 Mg1 Si2 98.55(5) . . ? Si1 Mg1 Si2 56.78(3) . . ? N3 Si1 C28 115.43(14) . . ? N3 Si1 C29 115.22(16) . . ? C28 Si1 C29 106.61(16) . . ? N3 Si1 Mg1 36.16(7) . . ? C28 Si1 Mg1 122.29(12) . . ? C29 Si1 Mg1 130.20(12) . . ? N3 Si1 H1 108.4(11) . . ? C28 Si1 H1 105.9(10) . . ? C29 Si1 H1 104.4(11) . . ? Mg1 Si1 H1 72.5(11) . . ? N3 Si2 C31 115.75(17) . . ? N3 Si2 C30 116.00(15) . . ? C31 Si2 C30 105.4(2) . . ? N3 Si2 Mg1 33.40(7) . . ? C31 Si2 Mg1 122.32(15) . . ? C30 Si2 Mg1 130.77(13) . . ? N3 Si2 H2A 107.6(10) . . ? C31 Si2 H2A 106.7(10) . . ? C30 Si2 H2A 104.5(10) . . ? Mg1 Si2 H2A 74.6(10) . . ? C8 N1 C18 109.8(2) . . ? C8 N1 C7 108.3(2) . . ? C18 N1 C7 108.7(2) . . ? C8 N1 Mg1 99.17(15) . . ? C18 N1 Mg1 119.64(16) . . ? C7 N1 Mg1 110.47(15) . . ? C19 N2 C9 110.8(2) . . ? C19 N2 C10 107.6(2) . . ? C9 N2 C10 111.3(2) . . ? C19 N2 Mg1 113.12(16) . . ? C9 N2 Mg1 110.09(16) . . ? C10 N2 Mg1 103.68(15) . . ? Si2 N3 Si1 126.34(12) . . ? Si2 N3 Mg1 119.32(11) . . ? Si1 N3 Mg1 114.34(11) . . ? C1 O1 C17 117.8(2) . . ? C1 O1 Mg1 124.19(16) . . ? C17 O1 Mg1 111.82(15) . . ? C16 O2 Mg1 131.13(15) . . ? C2 C1 C6 121.8(3) . . ? C2 C1 O1 123.2(3) . . ? C6 C1 O1 115.0(2) . . ? C1 C2 C3 118.8(3) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C4 C3 C2 121.1(4) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 120.0(4) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 120.9(3) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C1 C6 C5 117.5(3) . . ? C1 C6 C7 120.6(2) . . ? C5 C6 C7 122.0(3) . . ? C6 C7 N1 112.7(2) . . ? C6 C7 H7A 109.1 . . ? N1 C7 H7A 109.1 . . ? C6 C7 H7B 109.1 . . ? N1 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? N1 C8 C9 111.6(2) . . ? N1 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? N1 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? N2 C9 C8 110.5(2) . . ? N2 C9 H9A 109.6 . . ? C8 C9 H9A 109.6 . . ? N2 C9 H9B 109.6 . . ? C8 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C11 C10 N2 115.3(2) . . ? C11 C10 H10A 108.4 . . ? N2 C10 H10A 108.4 . . ? C11 C10 H10B 108.4 . . ? N2 C10 H10B 108.4 . . ? H10A C10 H10B 107.5 . . ? C12 C11 C16 120.5(2) . . ? C12 C11 C10 119.9(2) . . ? C16 C11 C10 119.6(2) . . ? C13 C12 C11 122.6(3) . . ? C13 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? C12 C13 C14 116.0(3) . . ? C12 C13 C24 122.6(3) . . ? C14 C13 C24 121.4(3) . . ? C15 C14 C13 124.3(3) . . ? C15 C14 H14 117.8 . . ? C13 C14 H14 117.8 . . ? C14 C15 C16 118.1(2) . . ? C14 C15 C20 121.2(2) . . ? C16 C15 C20 120.7(2) . . ? O2 C16 C11 118.9(2) . . ? O2 C16 C15 122.9(2) . . ? C11 C16 C15 118.2(2) . . ? O1 C17 H17A 109.5 . . ? O1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N1 C18 H18A 109.5 . . ? N1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 C19 H19A 109.5 . . ? N2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C22 109.7(2) . . ? C21 C20 C15 109.2(2) . . ? C22 C20 C15 111.0(2) . . ? C21 C20 C23 107.9(2) . . ? C22 C20 C23 106.8(2) . . ? C15 C20 C23 112.2(2) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C26' 66.1(7) . . ? C25 C24 C27' 137.2(7) . . ? C26' C24 C27' 106.9(9) . . ? C25 C24 C27 110.9(7) . . ? C26' C24 C27 129.5(7) . . ? C27' C24 C27 39.0(6) . . ? C25 C24 C13 109.6(4) . . ? C26' C24 C13 114.5(5) . . ? C27' C24 C13 111.2(6) . . ? C27 C24 C13 113.4(5) . . ? C25 C24 C26 107.3(7) . . ? C26' C24 C26 42.1(7) . . ? C27' C24 C26 71.0(7) . . ? C27 C24 C26 106.8(7) . . ? C13 C24 C26 108.7(4) . . ? C25 C24 C25' 44.9(6) . . ? C26' C24 C25' 107.8(8) . . ? C27' C24 C25' 109.5(9) . . ? C27 C24 C25' 71.9(8) . . ? C13 C24 C25' 106.9(5) . . ? C26 C24 C25' 141.2(6) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? C24 C25' H25D 109.5 . . ? C24 C25' H25E 109.5 . . ? H25D C25' H25E 109.5 . . ? C24 C25' H25F 109.5 . . ? H25D C25' H25F 109.5 . . ? H25E C25' H25F 109.5 . . ? C24 C26' H26D 109.5 . . ? C24 C26' H26E 109.5 . . ? H26D C26' H26E 109.5 . . ? C24 C26' H26F 109.5 . . ? H26D C26' H26F 109.5 . . ? H26E C26' H26F 109.5 . . ? C24 C27' H27D 109.5 . . ? C24 C27' H27E 109.5 . . ? H27D C27' H27E 109.5 . . ? C24 C27' H27F 109.5 . . ? H27D C27' H27F 109.5 . . ? H27E C27' H27F 109.5 . . ? Si1 C28 H28A 109.5 . . ? Si1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si1 C29 H29A 109.5 . . ? Si1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si2 C30 H30A 109.5 . . ? Si2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si2 C31 H31A 109.5 . . ? Si2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 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 O2 Mg1 Si1 N3 20.90(17) . . . . ? N2 Mg1 Si1 N3 -94.89(14) . . . . ? N1 Mg1 Si1 N3 -175.61(14) . . . . ? O1 Mg1 Si1 N3 102.05(13) . . . . ? Si2 Mg1 Si1 N3 -0.23(12) . . . . ? O2 Mg1 Si1 C28 -68.9(2) . . . . ? N3 Mg1 Si1 C28 -89.77(19) . . . . ? N2 Mg1 Si1 C28 175.33(16) . . . . ? N1 Mg1 Si1 C28 94.62(16) . . . . ? O1 Mg1 Si1 C28 12.28(16) . . . . ? Si2 Mg1 Si1 C28 -90.00(15) . . . . ? O2 Mg1 Si1 C29 98.7(2) . . . . ? N3 Mg1 Si1 C29 77.8(2) . . . . ? N2 Mg1 Si1 C29 -17.06(18) . . . . ? N1 Mg1 Si1 C29 -97.77(18) . . . . ? O1 Mg1 Si1 C29 179.88(18) . . . . ? Si2 Mg1 Si1 C29 77.61(17) . . . . ? O2 Mg1 Si2 N3 -168.86(14) . . . . ? N2 Mg1 Si2 N3 98.68(14) . . . . ? N1 Mg1 Si2 N3 12.7(2) . . . . ? O1 Mg1 Si2 N3 -80.41(14) . . . . ? Si1 Mg1 Si2 N3 0.24(13) . . . . ? O2 Mg1 Si2 C31 102.6(2) . . . . ? N3 Mg1 Si2 C31 -88.5(2) . . . . ? N2 Mg1 Si2 C31 10.1(2) . . . . ? N1 Mg1 Si2 C31 -75.8(3) . . . . ? O1 Mg1 Si2 C31 -168.9(2) . . . . ? Si1 Mg1 Si2 C31 -88.3(2) . . . . ? O2 Mg1 Si2 C30 -93.71(19) . . . . ? N3 Mg1 Si2 C30 75.1(2) . . . . ? N2 Mg1 Si2 C30 173.8(2) . . . . ? N1 Mg1 Si2 C30 87.9(3) . . . . ? O1 Mg1 Si2 C30 -5.3(2) . . . . ? Si1 Mg1 Si2 C30 75.39(19) . . . . ? O2 Mg1 N1 C8 -49.73(17) . . . . ? N3 Mg1 N1 C8 136.38(16) . . . . ? N2 Mg1 N1 C8 38.36(16) . . . . ? O1 Mg1 N1 C8 -135.36(16) . . . . ? Si1 Mg1 N1 C8 139.27(15) . . . . ? Si2 Mg1 N1 C8 128.60(19) . . . . ? O2 Mg1 N1 C18 -168.85(18) . . . . ? N3 Mg1 N1 C18 17.3(2) . . . . ? N2 Mg1 N1 C18 -80.77(19) . . . . ? O1 Mg1 N1 C18 105.52(19) . . . . ? Si1 Mg1 N1 C18 20.15(19) . . . . ? Si2 Mg1 N1 C18 9.5(3) . . . . ? O2 Mg1 N1 C7 63.88(18) . . . . ? N3 Mg1 N1 C7 -110.01(18) . . . . ? N2 Mg1 N1 C7 151.97(18) . . . . ? O1 Mg1 N1 C7 -21.75(17) . . . . ? Si1 Mg1 N1 C7 -107.12(16) . . . . ? Si2 Mg1 N1 C7 -117.8(2) . . . . ? O2 Mg1 N2 C19 -142.73(19) . . . . ? N3 Mg1 N2 C19 -21.2(2) . . . . ? N1 Mg1 N2 C19 109.27(19) . . . . ? O1 Mg1 N2 C19 128.3(3) . . . . ? Si1 Mg1 N2 C19 9.13(19) . . . . ? Si2 Mg1 N2 C19 -48.98(19) . . . . ? O2 Mg1 N2 C9 92.67(17) . . . . ? N3 Mg1 N2 C9 -145.80(17) . . . . ? N1 Mg1 N2 C9 -15.33(17) . . . . ? O1 Mg1 N2 C9 3.7(3) . . . . ? Si1 Mg1 N2 C9 -115.47(16) . . . . ? Si2 Mg1 N2 C9 -173.58(16) . . . . ? O2 Mg1 N2 C10 -26.47(16) . . . . ? N3 Mg1 N2 C10 95.07(16) . . . . ? N1 Mg1 N2 C10 -134.47(16) . . . . ? O1 Mg1 N2 C10 -115.4(3) . . . . ? Si1 Mg1 N2 C10 125.39(14) . . . . ? Si2 Mg1 N2 C10 67.28(15) . . . . ? C31 Si2 N3 Si1 -69.2(3) . . . . ? C30 Si2 N3 Si1 55.0(2) . . . . ? Mg1 Si2 N3 Si1 -179.5(2) . . . . ? C31 Si2 N3 Mg1 110.3(2) . . . . ? C30 Si2 N3 Mg1 -125.47(18) . . . . ? C28 Si1 N3 Si2 -69.8(2) . . . . ? C29 Si1 N3 Si2 55.2(2) . . . . ? Mg1 Si1 N3 Si2 179.5(2) . . . . ? C28 Si1 N3 Mg1 110.61(16) . . . . ? C29 Si1 N3 Mg1 -124.38(15) . . . . ? O2 Mg1 N3 Si2 12.88(17) . . . . ? N2 Mg1 N3 Si2 -87.34(13) . . . . ? N1 Mg1 N3 Si2 -173.83(11) . . . . ? O1 Mg1 N3 Si2 102.41(13) . . . . ? Si1 Mg1 N3 Si2 -179.6(2) . . . . ? O2 Mg1 N3 Si1 -167.54(10) . . . . ? N2 Mg1 N3 Si1 92.24(12) . . . . ? N1 Mg1 N3 Si1 5.75(18) . . . . ? O1 Mg1 N3 Si1 -78.00(12) . . . . ? Si2 Mg1 N3 Si1 179.6(2) . . . . ? O2 Mg1 O1 C1 -144.17(19) . . . . ? N3 Mg1 O1 C1 95.8(2) . . . . ? N2 Mg1 O1 C1 -54.6(3) . . . . ? N1 Mg1 O1 C1 -35.8(2) . . . . ? Si1 Mg1 O1 C1 67.01(19) . . . . ? Si2 Mg1 O1 C1 122.75(18) . . . . ? O2 Mg1 O1 C17 64.19(19) . . . . ? N3 Mg1 O1 C17 -55.80(19) . . . . ? N2 Mg1 O1 C17 153.8(3) . . . . ? N1 Mg1 O1 C17 172.57(19) . . . . ? Si1 Mg1 O1 C17 -84.64(18) . . . . ? Si2 Mg1 O1 C17 -28.89(19) . . . . ? N3 Mg1 O2 C16 -126.6(2) . . . . ? N2 Mg1 O2 C16 -19.7(2) . . . . ? N1 Mg1 O2 C16 58.7(2) . . . . ? O1 Mg1 O2 C16 140.8(2) . . . . ? Si1 Mg1 O2 C16 -138.30(18) . . . . ? Si2 Mg1 O2 C16 -120.7(2) . . . . ? C17 O1 C1 C2 21.1(4) . . . . ? Mg1 O1 C1 C2 -129.0(2) . . . . ? C17 O1 C1 C6 -159.7(2) . . . . ? Mg1 O1 C1 C6 50.2(3) . . . . ? C6 C1 C2 C3 -1.7(4) . . . . ? O1 C1 C2 C3 177.4(3) . . . . ? C1 C2 C3 C4 1.4(5) . . . . ? C2 C3 C4 C5 -0.8(6) . . . . ? C3 C4 C5 C6 0.5(5) . . . . ? C2 C1 C6 C5 1.4(4) . . . . ? O1 C1 C6 C5 -177.8(2) . . . . ? C2 C1 C6 C7 -178.6(3) . . . . ? O1 C1 C6 C7 2.2(3) . . . . ? C4 C5 C6 C1 -0.8(4) . . . . ? C4 C5 C6 C7 179.2(3) . . . . ? C1 C6 C7 N1 -70.3(3) . . . . ? C5 C6 C7 N1 109.8(3) . . . . ? C8 N1 C7 C6 178.8(2) . . . . ? C18 N1 C7 C6 -61.9(3) . . . . ? Mg1 N1 C7 C6 71.2(2) . . . . ? C18 N1 C8 C9 66.9(3) . . . . ? C7 N1 C8 C9 -174.6(2) . . . . ? Mg1 N1 C8 C9 -59.3(2) . . . . ? C19 N2 C9 C8 -137.7(2) . . . . ? C10 N2 C9 C8 102.6(3) . . . . ? Mg1 N2 C9 C8 -11.8(3) . . . . ? N1 C8 C9 N2 50.6(3) . . . . ? C19 N2 C10 C11 -173.6(2) . . . . ? C9 N2 C10 C11 -52.0(3) . . . . ? Mg1 N2 C10 C11 66.3(2) . . . . ? N2 C10 C11 C12 116.1(3) . . . . ? N2 C10 C11 C16 -65.8(3) . . . . ? C16 C11 C12 C13 -1.4(4) . . . . ? C10 C11 C12 C13 176.7(3) . . . . ? C11 C12 C13 C14 -3.0(4) . . . . ? C11 C12 C13 C24 175.8(3) . . . . ? C12 C13 C14 C15 2.9(4) . . . . ? C24 C13 C14 C15 -176.0(3) . . . . ? C13 C14 C15 C16 1.6(4) . . . . ? C13 C14 C15 C20 -176.6(2) . . . . ? Mg1 O2 C16 C11 32.2(3) . . . . ? Mg1 O2 C16 C15 -147.0(2) . . . . ? C12 C11 C16 O2 -173.2(2) . . . . ? C10 C11 C16 O2 8.8(3) . . . . ? C12 C11 C16 C15 6.0(4) . . . . ? C10 C11 C16 C15 -172.1(2) . . . . ? C14 C15 C16 O2 173.1(2) . . . . ? C20 C15 C16 O2 -8.7(4) . . . . ? C14 C15 C16 C11 -6.0(3) . . . . ? C20 C15 C16 C11 172.2(2) . . . . ? C14 C15 C20 C21 119.9(3) . . . . ? C16 C15 C20 C21 -58.3(3) . . . . ? C14 C15 C20 C22 -119.1(3) . . . . ? C16 C15 C20 C22 62.8(3) . . . . ? C14 C15 C20 C23 0.3(3) . . . . ? C16 C15 C20 C23 -177.8(2) . . . . ? C12 C13 C24 C25 -116.6(7) . . . . ? C14 C13 C24 C25 62.2(7) . . . . ? C12 C13 C24 C26' 171.5(9) . . . . ? C14 C13 C24 C26' -9.7(10) . . . . ? C12 C13 C24 C27' 50.2(8) . . . . ? C14 C13 C24 C27' -131.0(8) . . . . ? C12 C13 C24 C27 7.9(7) . . . . ? C14 C13 C24 C27 -173.3(6) . . . . ? C12 C13 C24 C26 126.4(6) . . . . ? C14 C13 C24 C26 -54.7(6) . . . . ? C12 C13 C24 C25' -69.3(8) . . . . ? C14 C13 C24 C25' 109.6(8) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.342 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.042 _database_code_depnum_ccdc_archive 'CCDC 937978' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a00120a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H59 Mg N3 O2 Si2' _chemical_formula_weight 610.32 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' Mg Mg 0.0486 0.0363 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.423(4) _cell_length_b 27.293(10) _cell_length_c 15.241(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.172(5) _cell_angle_gamma 90.00 _cell_volume 3846(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 914 _cell_measurement_theta_min 2.620 _cell_measurement_theta_max 21.428 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.054 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 0.138 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9469 _exptl_absorpt_correction_T_max 0.9756 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 6.08 _diffrn_reflns_number 15806 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6765 _reflns_number_gt 3957 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1065P)^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 SHELXL _refine_ls_extinction_coef 0.0004(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6765 _refine_ls_number_parameters 386 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1022 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.1929 _refine_ls_wR_factor_gt 0.1683 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _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 Mg1 Mg 0.64525(10) 0.16713(3) 0.85300(6) 0.0577(3) Uani 1 1 d . . . Si1 Si 0.53609(11) 0.05959(3) 0.79062(8) 0.0862(4) Uani 1 1 d . . . Si2 Si 0.46568(12) 0.13645(4) 0.65446(8) 0.0953(4) Uani 1 1 d . . . O1 O 0.70050(19) 0.23020(6) 0.81552(12) 0.0568(5) Uani 1 1 d . . . O2 O 0.8648(2) 0.14034(8) 0.84904(13) 0.0694(6) Uani 1 1 d . . . N1 N 0.4617(3) 0.20034(10) 0.9047(2) 0.0839(9) Uani 1 1 d . . . N2 N 0.7403(3) 0.17377(9) 1.00566(16) 0.0765(8) Uani 1 1 d . . . N3 N 0.5449(3) 0.11881(8) 0.75971(17) 0.0707(7) Uani 1 1 d . . . C1 C 0.5117(5) 0.22007(15) 0.9956(3) 0.1042(14) Uani 1 1 d . . . H1A H 0.4745 0.1998 1.0384 0.125 Uiso 1 1 calc R . . H1B H 0.4738 0.2529 0.9989 0.125 Uiso 1 1 calc R . . C2 C 0.6739(5) 0.22141(13) 1.0198(2) 0.0945(12) Uani 1 1 d . . . H2A H 0.7097 0.2462 0.9839 0.113 Uiso 1 1 calc R . . H2B H 0.7030 0.2307 1.0821 0.113 Uiso 1 1 calc R . . C3 C 0.4123(3) 0.23964(12) 0.8384(3) 0.0863(11) Uani 1 1 d . . . H3A H 0.3201 0.2518 0.8486 0.104 Uiso 1 1 calc R . . H3B H 0.3954 0.2251 0.7792 0.104 Uiso 1 1 calc R . . C4 C 0.5114(3) 0.28230(11) 0.8388(2) 0.0673(8) Uani 1 1 d . . . C5 C 0.6514(3) 0.27553(10) 0.82155(18) 0.0552(7) Uani 1 1 d . . . C6 C 0.7343(3) 0.31752(10) 0.81190(18) 0.0554(7) Uani 1 1 d . . . C7 C 0.6782(3) 0.36280(10) 0.8274(2) 0.0642(8) Uani 1 1 d . . . H7 H 0.7351 0.3902 0.8230 0.077 Uiso 1 1 calc R . . C8 C 0.5437(3) 0.37049(11) 0.8491(2) 0.0680(8) Uani 1 1 d . . . C9 C 0.4623(3) 0.32911(11) 0.8532(2) 0.0734(9) Uani 1 1 d . . . H9 H 0.3703 0.3325 0.8662 0.088 Uiso 1 1 calc R . . C10 C 0.8986(4) 0.18043(13) 1.0172(2) 0.0854(10) Uani 1 1 d . . . H10A H 0.9361 0.1913 1.0779 0.102 Uiso 1 1 calc R . . H10B H 0.9182 0.2060 0.9770 0.102 Uiso 1 1 calc R . . C11 C 0.9764(4) 0.13490(13) 0.9996(2) 0.0800(10) Uani 1 1 d . . . C12 C 0.9590(3) 0.11548(12) 0.9152(2) 0.0709(8) Uani 1 1 d . . . C13 C 1.0303(4) 0.07379(13) 0.8973(3) 0.0950(12) Uani 1 1 d . . . H13 H 1.0172 0.0614 0.8395 0.114 Uiso 1 1 calc R . . C14 C 1.1220(5) 0.05067(17) 0.9669(4) 0.1296(18) Uani 1 1 d . . . H14 H 1.1712 0.0225 0.9558 0.156 Uiso 1 1 calc R . . C15 C 1.1405(6) 0.0686(2) 1.0506(4) 0.137(2) Uani 1 1 d . . . H15 H 1.2016 0.0526 1.0969 0.164 Uiso 1 1 calc R . . C16 C 1.0702(5) 0.11019(18) 1.0679(3) 0.1148(15) Uani 1 1 d . . . H16 H 1.0849 0.1223 1.1260 0.138 Uiso 1 1 calc R . . C17 C 0.3380(4) 0.16584(14) 0.9022(4) 0.1258(17) Uani 1 1 d . . . H17A H 0.3682 0.1388 0.9417 0.189 Uiso 1 1 calc R . . H17B H 0.3066 0.1539 0.8424 0.189 Uiso 1 1 calc R . . H17C H 0.2595 0.1827 0.9210 0.189 Uiso 1 1 calc R . . C18 C 0.7114(5) 0.13907(14) 1.0755(2) 0.1041(13) Uani 1 1 d . . . H18A H 0.7394 0.1539 1.1334 0.156 Uiso 1 1 calc R . . H18B H 0.7660 0.1096 1.0732 0.156 Uiso 1 1 calc R . . H18C H 0.6101 0.1314 1.0650 0.156 Uiso 1 1 calc R . . C19 C 0.8978(4) 0.14019(14) 0.7609(2) 0.0905(11) Uani 1 1 d . . . H19A H 1.0004 0.1431 0.7652 0.136 Uiso 1 1 calc R . . H19B H 0.8501 0.1673 0.7272 0.136 Uiso 1 1 calc R . . H19C H 0.8648 0.1101 0.7312 0.136 Uiso 1 1 calc R . . C20 C 0.8822(3) 0.31308(11) 0.7850(2) 0.0653(8) Uani 1 1 d . . . C21 C 0.9508(4) 0.36283(13) 0.7734(3) 0.1006(12) Uani 1 1 d . . . H21A H 0.9623 0.3808 0.8284 0.151 Uiso 1 1 calc R . . H21B H 0.8894 0.3809 0.7268 0.151 Uiso 1 1 calc R . . H21C H 1.0436 0.3580 0.7577 0.151 Uiso 1 1 calc R . . C22 C 0.8633(4) 0.28606(14) 0.6957(2) 0.0964(12) Uani 1 1 d . . . H22A H 0.9564 0.2801 0.6812 0.145 Uiso 1 1 calc R . . H22B H 0.8063 0.3057 0.6497 0.145 Uiso 1 1 calc R . . H22C H 0.8151 0.2554 0.7002 0.145 Uiso 1 1 calc R . . C23 C 0.9865(3) 0.28423(14) 0.8553(2) 0.0922(11) Uani 1 1 d . . . H23A H 0.9496 0.2517 0.8597 0.138 Uiso 1 1 calc R . . H23B H 0.9960 0.3003 0.9122 0.138 Uiso 1 1 calc R . . H23C H 1.0793 0.2825 0.8385 0.138 Uiso 1 1 calc R . . C24 C 0.4926(4) 0.42166(12) 0.8653(3) 0.0825(10) Uani 1 1 d . . . C25 C 0.3521(6) 0.42230(16) 0.8964(5) 0.182(3) Uani 1 1 d . . . H25A H 0.2773 0.4096 0.8501 0.274 Uiso 1 1 calc R . . H25B H 0.3288 0.4553 0.9100 0.274 Uiso 1 1 calc R . . H25C H 0.3595 0.4024 0.9490 0.274 Uiso 1 1 calc R . . C26 C 0.6066(5) 0.45004(14) 0.9294(3) 0.1264(17) Uani 1 1 d . . . H26A H 0.5809 0.4841 0.9277 0.190 Uiso 1 1 calc R . . H26B H 0.6987 0.4463 0.9120 0.190 Uiso 1 1 calc R . . H26C H 0.6126 0.4377 0.9889 0.190 Uiso 1 1 calc R . . C27 C 0.4729(6) 0.45203(16) 0.7773(3) 0.1342(17) Uani 1 1 d . . . H27A H 0.3962 0.4381 0.7338 0.201 Uiso 1 1 calc R . . H27B H 0.5611 0.4515 0.7547 0.201 Uiso 1 1 calc R . . H27C H 0.4491 0.4853 0.7892 0.201 Uiso 1 1 calc R . . C28 C 0.6547(5) 0.01726(15) 0.7420(3) 0.1243(16) Uani 1 1 d . . . H28A H 0.6331 0.0199 0.6780 0.186 Uiso 1 1 calc R . . H28B H 0.6381 -0.0158 0.7591 0.186 Uiso 1 1 calc R . . H28C H 0.7541 0.0258 0.7638 0.186 Uiso 1 1 calc R . . C29 C 0.3484(5) 0.03321(18) 0.7626(4) 0.156(2) Uani 1 1 d . . . H29A H 0.2835 0.0533 0.7882 0.235 Uiso 1 1 calc R . . H29B H 0.3489 0.0006 0.7863 0.235 Uiso 1 1 calc R . . H29C H 0.3170 0.0322 0.6988 0.235 Uiso 1 1 calc R . . C30 C 0.5961(5) 0.05241(13) 0.9134(3) 0.1088(13) Uani 1 1 d . . . H30A H 0.6956 0.0621 0.9304 0.163 Uiso 1 1 calc R . . H30B H 0.5860 0.0188 0.9296 0.163 Uiso 1 1 calc R . . H30C H 0.5376 0.0727 0.9437 0.163 Uiso 1 1 calc R . . C31 C 0.5397(5) 0.19526(15) 0.6204(3) 0.1213(15) Uani 1 1 d . . . H31A H 0.5343 0.2199 0.6646 0.182 Uiso 1 1 calc R . . H31B H 0.4841 0.2055 0.5638 0.182 Uiso 1 1 calc R . . H31C H 0.6387 0.1907 0.6151 0.182 Uiso 1 1 calc R . . C32 C 0.2645(4) 0.14682(18) 0.6383(4) 0.145(2) Uani 1 1 d . . . H32A H 0.2187 0.1178 0.6550 0.217 Uiso 1 1 calc R . . H32B H 0.2266 0.1543 0.5766 0.217 Uiso 1 1 calc R . . H32C H 0.2456 0.1737 0.6750 0.217 Uiso 1 1 calc R . . C33 C 0.4907(5) 0.09130(18) 0.5642(3) 0.1314(17) Uani 1 1 d . . . H33A H 0.5919 0.0879 0.5636 0.197 Uiso 1 1 calc R . . H33B H 0.4410 0.1031 0.5071 0.197 Uiso 1 1 calc R . . H33C H 0.4518 0.0600 0.5763 0.197 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 Mg1 0.0566(6) 0.0585(6) 0.0601(6) -0.0040(4) 0.0161(4) -0.0011(4) Si1 0.0811(7) 0.0623(6) 0.1082(8) -0.0113(5) 0.0012(6) -0.0088(5) Si2 0.0925(8) 0.0881(7) 0.0891(8) -0.0129(6) -0.0226(6) 0.0098(6) O1 0.0565(11) 0.0538(10) 0.0663(12) -0.0026(9) 0.0270(9) 0.0067(9) O2 0.0601(12) 0.0863(14) 0.0591(12) 0.0028(11) 0.0048(10) 0.0144(10) N1 0.0763(18) 0.0759(18) 0.115(2) -0.0103(18) 0.0574(17) -0.0119(15) N2 0.104(2) 0.0737(18) 0.0556(15) -0.0011(13) 0.0249(14) -0.0210(15) N3 0.0658(15) 0.0600(15) 0.0799(18) -0.0079(13) -0.0014(13) 0.0011(12) C1 0.135(4) 0.096(3) 0.105(3) -0.012(2) 0.082(3) -0.007(2) C2 0.147(4) 0.085(2) 0.062(2) -0.0171(18) 0.047(2) -0.019(2) C3 0.0503(18) 0.079(2) 0.136(3) -0.015(2) 0.035(2) 0.0013(16) C4 0.0503(17) 0.0669(19) 0.090(2) -0.0119(16) 0.0264(15) -0.0003(14) C5 0.0508(16) 0.0597(17) 0.0588(17) -0.0032(13) 0.0197(13) 0.0063(13) C6 0.0520(16) 0.0601(17) 0.0571(16) 0.0006(13) 0.0179(13) 0.0057(13) C7 0.0601(18) 0.0582(17) 0.075(2) -0.0048(15) 0.0145(15) 0.0037(14) C8 0.0613(19) 0.0632(18) 0.081(2) -0.0112(16) 0.0161(16) 0.0112(15) C9 0.0525(17) 0.075(2) 0.098(2) -0.0136(18) 0.0274(16) 0.0118(15) C10 0.110(3) 0.085(2) 0.0559(19) -0.0036(17) 0.0035(18) -0.035(2) C11 0.077(2) 0.079(2) 0.076(2) 0.0205(19) -0.0056(18) -0.0187(18) C12 0.0554(18) 0.071(2) 0.081(2) 0.0077(18) -0.0019(16) -0.0023(15) C13 0.072(2) 0.081(2) 0.125(3) 0.011(2) 0.002(2) 0.0052(19) C14 0.107(3) 0.100(3) 0.172(5) 0.044(4) 0.003(4) 0.025(3) C15 0.116(4) 0.138(5) 0.136(5) 0.057(4) -0.024(4) 0.010(3) C16 0.115(3) 0.126(4) 0.087(3) 0.033(3) -0.022(2) -0.020(3) C17 0.090(3) 0.100(3) 0.212(5) -0.013(3) 0.089(3) -0.025(2) C18 0.152(4) 0.094(3) 0.076(2) 0.010(2) 0.043(2) -0.030(2) C19 0.086(2) 0.115(3) 0.076(2) 0.007(2) 0.0314(19) 0.028(2) C20 0.0563(17) 0.0690(18) 0.078(2) 0.0124(16) 0.0318(15) 0.0037(14) C21 0.077(2) 0.094(3) 0.144(4) 0.018(2) 0.055(2) -0.0041(19) C22 0.106(3) 0.115(3) 0.085(2) 0.006(2) 0.060(2) 0.013(2) C23 0.0542(19) 0.127(3) 0.102(3) 0.025(2) 0.0319(19) 0.0179(19) C24 0.075(2) 0.073(2) 0.099(3) -0.014(2) 0.0135(19) 0.0212(17) C25 0.139(4) 0.087(3) 0.363(9) -0.048(4) 0.149(5) 0.012(3) C26 0.125(4) 0.091(3) 0.157(4) -0.043(3) 0.011(3) 0.019(3) C27 0.151(4) 0.103(3) 0.145(4) 0.001(3) 0.020(3) 0.057(3) C28 0.152(4) 0.080(3) 0.134(4) -0.015(3) 0.012(3) 0.032(3) C29 0.115(4) 0.108(3) 0.231(7) -0.008(4) -0.005(4) -0.053(3) C30 0.134(4) 0.073(2) 0.120(3) 0.015(2) 0.025(3) -0.014(2) C31 0.164(4) 0.102(3) 0.080(3) 0.016(2) -0.021(3) 0.012(3) C32 0.101(3) 0.136(4) 0.167(5) -0.022(4) -0.047(3) 0.022(3) C33 0.151(4) 0.140(4) 0.088(3) -0.031(3) -0.015(3) 0.017(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O1 1.917(2) . ? Mg1 N3 2.033(3) . ? Mg1 O2 2.206(2) . ? Mg1 N1 2.227(3) . ? Mg1 N2 2.333(3) . ? Mg1 Si1 3.1934(16) . ? Si1 N3 1.690(3) . ? Si1 C30 1.858(4) . ? Si1 C28 1.858(4) . ? Si1 C29 1.880(4) . ? Si2 N3 1.702(3) . ? Si2 C31 1.864(4) . ? Si2 C32 1.885(4) . ? Si2 C33 1.895(4) . ? O1 C5 1.331(3) . ? O2 C12 1.385(4) . ? O2 C19 1.437(4) . ? N1 C1 1.477(5) . ? N1 C3 1.485(5) . ? N1 C17 1.494(4) . ? N2 C2 1.477(4) . ? N2 C10 1.479(4) . ? N2 C18 1.489(4) . ? C1 C2 1.502(5) . ? C3 C4 1.492(4) . ? C4 C9 1.391(4) . ? C4 C5 1.406(4) . ? C5 C6 1.411(4) . ? C6 C7 1.383(4) . ? C6 C20 1.532(4) . ? C7 C8 1.386(4) . ? C8 C9 1.374(4) . ? C8 C24 1.514(4) . ? C10 C11 1.493(5) . ? C11 C12 1.372(5) . ? C11 C16 1.401(5) . ? C12 C13 1.375(5) . ? C13 C14 1.383(6) . ? C14 C15 1.345(7) . ? C15 C16 1.365(7) . ? C20 C23 1.526(4) . ? C20 C22 1.527(4) . ? C20 C21 1.528(4) . ? C24 C25 1.490(5) . ? C24 C26 1.517(5) . ? C24 C27 1.557(6) . ? 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 Mg1 N3 119.36(11) . . ? O1 Mg1 O2 88.80(8) . . ? N3 Mg1 O2 94.45(9) . . ? O1 Mg1 N1 90.82(9) . . ? N3 Mg1 N1 102.91(11) . . ? O2 Mg1 N1 160.24(11) . . ? O1 Mg1 N2 98.82(9) . . ? N3 Mg1 N2 141.69(10) . . ? O2 Mg1 N2 82.65(9) . . ? N1 Mg1 N2 77.89(12) . . ? O1 Mg1 Si1 145.78(7) . . ? N3 Mg1 Si1 27.91(7) . . ? O2 Mg1 Si1 86.39(7) . . ? N1 Mg1 Si1 104.59(8) . . ? N2 Mg1 Si1 114.06(7) . . ? N3 Si1 C30 111.10(15) . . ? N3 Si1 C28 114.70(19) . . ? C30 Si1 C28 104.3(2) . . ? N3 Si1 C29 113.41(18) . . ? C30 Si1 C29 106.1(2) . . ? C28 Si1 C29 106.4(2) . . ? N3 Si1 Mg1 34.28(9) . . ? C30 Si1 Mg1 77.25(11) . . ? C28 Si1 Mg1 120.41(16) . . ? C29 Si1 Mg1 130.85(17) . . ? N3 Si2 C31 112.77(15) . . ? N3 Si2 C32 114.3(2) . . ? C31 Si2 C32 104.8(2) . . ? N3 Si2 C33 113.99(17) . . ? C31 Si2 C33 104.6(2) . . ? C32 Si2 C33 105.4(2) . . ? C5 O1 Mg1 134.12(16) . . ? C12 O2 C19 117.1(2) . . ? C12 O2 Mg1 127.92(19) . . ? C19 O2 Mg1 113.60(18) . . ? C1 N1 C3 112.1(3) . . ? C1 N1 C17 111.0(3) . . ? C3 N1 C17 107.3(3) . . ? C1 N1 Mg1 110.6(2) . . ? C3 N1 Mg1 102.49(18) . . ? C17 N1 Mg1 113.0(2) . . ? C2 N2 C10 108.7(3) . . ? C2 N2 C18 108.3(3) . . ? C10 N2 C18 108.2(3) . . ? C2 N2 Mg1 97.0(2) . . ? C10 N2 Mg1 108.20(18) . . ? C18 N2 Mg1 125.1(2) . . ? Si1 N3 Si2 119.80(14) . . ? Si1 N3 Mg1 117.81(14) . . ? Si2 N3 Mg1 122.35(14) . . ? N1 C1 C2 111.3(3) . . ? N2 C2 C1 112.5(3) . . ? N1 C3 C4 116.6(3) . . ? C9 C4 C5 120.2(3) . . ? C9 C4 C3 119.4(3) . . ? C5 C4 C3 120.4(3) . . ? O1 C5 C4 119.1(2) . . ? O1 C5 C6 122.7(2) . . ? C4 C5 C6 118.1(2) . . ? C7 C6 C5 118.1(2) . . ? C7 C6 C20 120.9(3) . . ? C5 C6 C20 121.0(2) . . ? C6 C7 C8 125.0(3) . . ? C9 C8 C7 115.5(3) . . ? C9 C8 C24 123.5(3) . . ? C7 C8 C24 120.9(3) . . ? C8 C9 C4 122.8(3) . . ? N2 C10 C11 113.3(3) . . ? C12 C11 C16 117.0(4) . . ? C12 C11 C10 121.1(3) . . ? C16 C11 C10 121.9(4) . . ? C11 C12 C13 122.1(3) . . ? C11 C12 O2 115.9(3) . . ? C13 C12 O2 122.0(3) . . ? C12 C13 C14 118.8(4) . . ? C15 C14 C13 120.5(5) . . ? C14 C15 C16 120.5(5) . . ? C15 C16 C11 121.1(5) . . ? C23 C20 C22 109.0(3) . . ? C23 C20 C21 108.1(3) . . ? C22 C20 C21 107.8(3) . . ? C23 C20 C6 110.3(2) . . ? C22 C20 C6 108.7(3) . . ? C21 C20 C6 112.8(2) . . ? C25 C24 C8 113.2(3) . . ? C25 C24 C26 110.6(4) . . ? C8 C24 C26 111.6(3) . . ? C25 C24 C27 107.6(4) . . ? C8 C24 C27 109.8(3) . . ? C26 C24 C27 103.5(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.373 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.042 _database_code_depnum_ccdc_archive 'CCDC 937979' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a00408a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H41 Cl2 Mg N3 O2 Si2' _chemical_formula_weight 567.00 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' Mg Mg 0.0486 0.0363 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.650(5) _cell_length_b 14.321(6) _cell_length_c 18.739(7) _cell_angle_alpha 90.00 _cell_angle_beta 97.448(5) _cell_angle_gamma 90.00 _cell_volume 3100(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 936 _cell_measurement_theta_min 2.265 _cell_measurement_theta_max 22.742 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.333 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9365 _exptl_absorpt_correction_T_max 0.9549 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.82 _diffrn_reflns_number 13710 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_sigmaI/netI 0.0630 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 26.01 _reflns_number_total 6095 _reflns_number_gt 3439 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6095 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0974 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1344 _refine_ls_wR_factor_gt 0.1125 _refine_ls_goodness_of_fit_ref 0.929 _refine_ls_restrained_S_all 0.929 _refine_ls_shift/su_max 0.003 _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 Mg1 Mg 0.26813(7) 0.86005(6) 0.18101(5) 0.0462(2) Uani 1 1 d . . . N1 N 0.20919(19) 0.89981(18) 0.28644(12) 0.0569(6) Uani 1 1 d . . . N2 N 0.29004(18) 1.02019(15) 0.18076(11) 0.0487(5) Uani 1 1 d . . . N3 N 0.16310(16) 0.75065(15) 0.14756(12) 0.0505(6) Uani 1 1 d . . . O1 O 0.41902(15) 0.82753(14) 0.22951(10) 0.0562(5) Uani 1 1 d . . . O2 O 0.34412(18) 0.86912(13) 0.08127(10) 0.0622(5) Uani 1 1 d . . . Si1 Si 0.04320(7) 0.77630(6) 0.08909(5) 0.0618(3) Uani 1 1 d . . . Si2 Si 0.18661(7) 0.63964(6) 0.17781(6) 0.0707(3) Uani 1 1 d . . . Cl1 Cl 0.67381(6) 0.82199(6) 0.24511(5) 0.0754(3) Uani 1 1 d . . . Cl2 Cl 0.64027(10) 0.88693(9) 0.52408(5) 0.1132(4) Uani 1 1 d . . . C1 C 0.4674(2) 0.83686(19) 0.29554(15) 0.0508(7) Uani 1 1 d . . . C2 C 0.5889(2) 0.83787(19) 0.31330(16) 0.0556(7) Uani 1 1 d . . . C3 C 0.6420(3) 0.8521(2) 0.38282(19) 0.0667(9) Uani 1 1 d . . . H3 H 0.7223 0.8516 0.3930 0.080 Uiso 1 1 calc R . . C4 C 0.5751(3) 0.8668(2) 0.43613(18) 0.0702(9) Uani 1 1 d . . . C5 C 0.4569(3) 0.8655(2) 0.42280(16) 0.0649(8) Uani 1 1 d . . . H5 H 0.4129 0.8755 0.4601 0.078 Uiso 1 1 calc R . . C6 C 0.4024(2) 0.8491(2) 0.35317(15) 0.0549(7) Uani 1 1 d . . . C7 C 0.2738(2) 0.8372(2) 0.34110(15) 0.0630(8) Uani 1 1 d . . . H7A H 0.2569 0.7731 0.3267 0.076 Uiso 1 1 calc R . . H7B H 0.2443 0.8470 0.3866 0.076 Uiso 1 1 calc R . . C8 C 0.2361(3) 0.9985(2) 0.30323(15) 0.0705(9) Uani 1 1 d . . . H8A H 0.2652 1.0044 0.3539 0.085 Uiso 1 1 calc R . . H8B H 0.1659 1.0353 0.2939 0.085 Uiso 1 1 calc R . . C9 C 0.3255(3) 1.0361(2) 0.25865(14) 0.0616(8) Uani 1 1 d . . . H9A H 0.3357 1.1025 0.2675 0.074 Uiso 1 1 calc R . . H9B H 0.3992 1.0056 0.2732 0.074 Uiso 1 1 calc R . . C10 C 0.3906(2) 1.0415(2) 0.14228(15) 0.0576(8) Uani 1 1 d . . . H10A H 0.4542 1.0004 0.1599 0.069 Uiso 1 1 calc R . . H10B H 0.4154 1.1052 0.1529 0.069 Uiso 1 1 calc R . . C11 C 0.3635(2) 1.0300(2) 0.06271(15) 0.0524(7) Uani 1 1 d . . . C12 C 0.3414(2) 0.9428(2) 0.03312(15) 0.0549(7) Uani 1 1 d . . . C13 C 0.3171(3) 0.9307(3) -0.04048(17) 0.0794(10) Uani 1 1 d . . . H13 H 0.3019 0.8715 -0.0598 0.095 Uiso 1 1 calc R . . C14 C 0.3158(3) 1.0077(4) -0.08475(19) 0.0879(12) Uani 1 1 d . . . H14 H 0.3000 1.0004 -0.1344 0.105 Uiso 1 1 calc R . . C15 C 0.3377(3) 1.0950(3) -0.0560(2) 0.0902(12) Uani 1 1 d . . . H15 H 0.3372 1.1469 -0.0859 0.108 Uiso 1 1 calc R . . C16 C 0.3602(3) 1.1052(3) 0.0165(2) 0.0758(10) Uani 1 1 d . . . H16 H 0.3737 1.1647 0.0357 0.091 Uiso 1 1 calc R . . C17 C 0.0851(3) 0.8811(3) 0.28865(18) 0.0781(10) Uani 1 1 d . . . H17A H 0.0656 0.8963 0.3355 0.117 Uiso 1 1 calc R . . H17B H 0.0694 0.8162 0.2788 0.117 Uiso 1 1 calc R . . H17C H 0.0396 0.9185 0.2531 0.117 Uiso 1 1 calc R . . C18 C 0.1948(2) 1.0856(2) 0.15542(16) 0.0620(8) Uani 1 1 d . . . H18A H 0.2194 1.1485 0.1666 0.093 Uiso 1 1 calc R . . H18B H 0.1285 1.0714 0.1789 0.093 Uiso 1 1 calc R . . H18C H 0.1750 1.0793 0.1043 0.093 Uiso 1 1 calc R . . C19 C 0.3901(3) 0.7816(3) 0.0604(2) 0.0866(11) Uani 1 1 d . . . H19A H 0.3286 0.7440 0.0365 0.130 Uiso 1 1 calc R . . H19B H 0.4260 0.7494 0.1024 0.130 Uiso 1 1 calc R . . H19C H 0.4466 0.7929 0.0284 0.130 Uiso 1 1 calc R . . C20 C 0.0247(3) 0.9052(2) 0.07895(19) 0.0829(10) Uani 1 1 d . . . H20A H 0.0148 0.9322 0.1247 0.124 Uiso 1 1 calc R . . H20B H -0.0423 0.9182 0.0449 0.124 Uiso 1 1 calc R . . H20C H 0.0920 0.9315 0.0621 0.124 Uiso 1 1 calc R . . C21 C -0.0943(3) 0.7310(3) 0.1184(2) 0.1003(13) Uani 1 1 d . . . H21A H -0.0902 0.6643 0.1227 0.150 Uiso 1 1 calc R . . H21B H -0.1586 0.7479 0.0835 0.150 Uiso 1 1 calc R . . H21C H -0.1045 0.7578 0.1642 0.150 Uiso 1 1 calc R . . C22 C 0.0458(4) 0.7345(3) -0.0055(2) 0.1169(15) Uani 1 1 d . . . H22A H 0.1112 0.7611 -0.0244 0.175 Uiso 1 1 calc R . . H22B H -0.0242 0.7535 -0.0347 0.175 Uiso 1 1 calc R . . H22C H 0.0515 0.6677 -0.0058 0.175 Uiso 1 1 calc R . . C23 C 0.1069(3) 0.6107(3) 0.2562(2) 0.0979(13) Uani 1 1 d . . . H23A H 0.1381 0.6469 0.2973 0.147 Uiso 1 1 calc R . . H23B H 0.1156 0.5455 0.2673 0.147 Uiso 1 1 calc R . . H23C H 0.0262 0.6251 0.2440 0.147 Uiso 1 1 calc R . . C24 C 0.1371(3) 0.5474(3) 0.1092(2) 0.1125(15) Uani 1 1 d . . . H24A H 0.0575 0.5582 0.0905 0.169 Uiso 1 1 calc R . . H24B H 0.1446 0.4870 0.1315 0.169 Uiso 1 1 calc R . . H24C H 0.1838 0.5500 0.0707 0.169 Uiso 1 1 calc R . . C25 C 0.3417(3) 0.6120(3) 0.2092(3) 0.1059(15) Uani 1 1 d . . . H25A H 0.3858 0.6169 0.1695 0.159 Uiso 1 1 calc R . . H25B H 0.3477 0.5495 0.2280 0.159 Uiso 1 1 calc R . . H25C H 0.3714 0.6552 0.2462 0.159 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 Mg1 0.0438(5) 0.0489(6) 0.0459(5) 0.0004(4) 0.0051(4) 0.0029(4) N1 0.0526(14) 0.0669(17) 0.0516(14) 0.0025(12) 0.0092(11) 0.0099(12) N2 0.0499(13) 0.0488(13) 0.0467(13) -0.0045(11) 0.0033(10) 0.0028(10) N3 0.0367(11) 0.0515(14) 0.0621(14) 0.0016(11) 0.0021(10) -0.0010(10) O1 0.0477(10) 0.0698(14) 0.0494(11) -0.0023(10) 0.0001(9) 0.0066(9) O2 0.0852(15) 0.0494(13) 0.0564(12) -0.0074(10) 0.0261(10) -0.0056(10) Si1 0.0478(4) 0.0652(6) 0.0686(6) 0.0013(5) -0.0063(4) -0.0033(4) Si2 0.0482(5) 0.0541(5) 0.1074(8) 0.0111(5) 0.0008(5) -0.0019(4) Cl1 0.0547(4) 0.0833(6) 0.0890(6) 0.0159(5) 0.0122(4) 0.0063(4) Cl2 0.1315(9) 0.1180(9) 0.0753(7) -0.0085(6) -0.0429(6) 0.0003(7) C1 0.0507(16) 0.0458(17) 0.0545(18) 0.0073(13) 0.0019(13) 0.0039(12) C2 0.0515(16) 0.0468(17) 0.067(2) 0.0132(14) 0.0002(14) -0.0005(13) C3 0.0590(18) 0.057(2) 0.078(2) 0.0099(17) -0.0151(17) -0.0030(15) C4 0.086(2) 0.056(2) 0.060(2) 0.0065(16) -0.0203(18) -0.0021(17) C5 0.082(2) 0.060(2) 0.0501(19) 0.0100(15) 0.0006(16) 0.0049(16) C6 0.0549(17) 0.0582(19) 0.0503(17) 0.0086(14) 0.0016(14) 0.0001(13) C7 0.0602(18) 0.079(2) 0.0509(18) 0.0094(16) 0.0113(14) 0.0038(16) C8 0.088(2) 0.075(2) 0.0483(18) -0.0111(16) 0.0080(16) 0.0197(19) C9 0.075(2) 0.0507(18) 0.0555(18) -0.0112(15) -0.0045(16) 0.0048(15) C10 0.0500(16) 0.0508(18) 0.072(2) -0.0038(15) 0.0065(14) -0.0093(13) C11 0.0446(15) 0.059(2) 0.0546(18) 0.0051(15) 0.0103(13) -0.0045(13) C12 0.0463(16) 0.069(2) 0.0507(17) 0.0025(16) 0.0131(13) -0.0063(14) C13 0.071(2) 0.113(3) 0.055(2) -0.012(2) 0.0121(16) -0.021(2) C14 0.064(2) 0.147(4) 0.052(2) 0.020(3) 0.0067(16) -0.004(2) C15 0.074(2) 0.116(4) 0.083(3) 0.043(3) 0.019(2) 0.010(2) C16 0.072(2) 0.075(2) 0.083(3) 0.019(2) 0.0241(18) 0.0030(18) C17 0.0567(19) 0.111(3) 0.070(2) 0.004(2) 0.0185(16) 0.0158(19) C18 0.0573(17) 0.0563(19) 0.071(2) -0.0013(16) 0.0019(15) 0.0080(14) C19 0.105(3) 0.067(2) 0.099(3) -0.017(2) 0.054(2) -0.002(2) C20 0.071(2) 0.078(3) 0.092(3) 0.016(2) -0.0152(18) 0.0033(18) C21 0.0447(18) 0.104(3) 0.147(4) 0.025(3) -0.007(2) -0.0095(18) C22 0.137(4) 0.123(4) 0.082(3) -0.021(3) -0.019(3) -0.004(3) C23 0.077(2) 0.089(3) 0.125(3) 0.037(2) 0.003(2) -0.021(2) C24 0.106(3) 0.062(3) 0.168(4) -0.017(3) 0.011(3) 0.002(2) C25 0.057(2) 0.068(2) 0.188(4) 0.044(3) 0.000(2) 0.0114(18) _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 Mg1 O1 1.929(2) . ? Mg1 N3 2.036(2) . ? Mg1 O2 2.173(2) . ? Mg1 N1 2.247(2) . ? Mg1 N2 2.308(3) . ? Mg1 Si1 3.1783(14) . ? N1 C8 1.473(4) . ? N1 C17 1.476(4) . ? N1 C7 1.489(4) . ? N2 C18 1.482(3) . ? N2 C9 1.482(3) . ? N2 C10 1.485(3) . ? N3 Si2 1.698(2) . ? N3 Si1 1.700(2) . ? O1 C1 1.298(3) . ? O2 C12 1.386(3) . ? O2 C19 1.437(4) . ? Si1 C20 1.865(4) . ? Si1 C22 1.874(4) . ? Si1 C21 1.876(3) . ? Si2 C25 1.869(3) . ? Si2 C24 1.881(4) . ? Si2 C23 1.883(4) . ? Cl1 C2 1.729(3) . ? Cl2 C4 1.747(3) . ? C1 C6 1.408(4) . ? C1 C2 1.412(4) . ? C2 C3 1.383(4) . ? C3 C4 1.361(5) . ? C4 C5 1.368(4) . ? C5 C6 1.395(4) . ? C6 C7 1.496(4) . ? C8 C9 1.516(4) . ? C10 C11 1.493(4) . ? C11 C12 1.377(4) . ? C11 C16 1.379(4) . ? C12 C13 1.382(4) . ? C13 C14 1.379(5) . ? C14 C15 1.373(5) . ? C15 C16 1.358(5) . ? 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 Mg1 N3 115.72(9) . . ? O1 Mg1 O2 88.38(9) . . ? N3 Mg1 O2 94.41(9) . . ? O1 Mg1 N1 90.61(9) . . ? N3 Mg1 N1 103.04(10) . . ? O2 Mg1 N1 161.06(10) . . ? O1 Mg1 N2 98.43(8) . . ? N3 Mg1 N2 145.72(9) . . ? O2 Mg1 N2 83.18(8) . . ? N1 Mg1 N2 78.25(9) . . ? O1 Mg1 Si1 143.27(7) . . ? N3 Mg1 Si1 28.65(6) . . ? O2 Mg1 Si1 87.46(7) . . ? N1 Mg1 Si1 104.34(7) . . ? N2 Mg1 Si1 117.23(6) . . ? C8 N1 C17 110.5(2) . . ? C8 N1 C7 110.8(2) . . ? C17 N1 C7 106.3(2) . . ? C8 N1 Mg1 110.48(17) . . ? C17 N1 Mg1 112.99(18) . . ? C7 N1 Mg1 105.51(17) . . ? C18 N2 C9 108.7(2) . . ? C18 N2 C10 108.6(2) . . ? C9 N2 C10 108.0(2) . . ? C18 N2 Mg1 123.40(17) . . ? C9 N2 Mg1 99.65(16) . . ? C10 N2 Mg1 107.42(16) . . ? Si2 N3 Si1 120.07(12) . . ? Si2 N3 Mg1 123.58(12) . . ? Si1 N3 Mg1 116.29(12) . . ? C1 O1 Mg1 132.92(18) . . ? C12 O2 C19 117.7(2) . . ? C12 O2 Mg1 128.91(17) . . ? C19 O2 Mg1 112.93(18) . . ? N3 Si1 C20 110.74(13) . . ? N3 Si1 C22 115.34(16) . . ? C20 Si1 C22 103.60(19) . . ? N3 Si1 C21 113.46(15) . . ? C20 Si1 C21 106.26(18) . . ? C22 Si1 C21 106.6(2) . . ? N3 Si1 Mg1 35.05(8) . . ? C20 Si1 Mg1 76.01(10) . . ? C22 Si1 Mg1 121.32(14) . . ? C21 Si1 Mg1 130.32(13) . . ? N3 Si2 C25 114.27(14) . . ? N3 Si2 C24 114.03(16) . . ? C25 Si2 C24 105.35(19) . . ? N3 Si2 C23 113.05(16) . . ? C25 Si2 C23 105.24(18) . . ? C24 Si2 C23 103.89(19) . . ? O1 C1 C6 122.2(2) . . ? O1 C1 C2 121.6(3) . . ? C6 C1 C2 116.2(2) . . ? C3 C2 C1 122.4(3) . . ? C3 C2 Cl1 119.1(2) . . ? C1 C2 Cl1 118.5(2) . . ? C4 C3 C2 119.1(3) . . ? C3 C4 C5 121.5(3) . . ? C3 C4 Cl2 119.9(3) . . ? C5 C4 Cl2 118.6(3) . . ? C4 C5 C6 119.9(3) . . ? C5 C6 C1 120.9(3) . . ? C5 C6 C7 119.1(3) . . ? C1 C6 C7 119.9(2) . . ? N1 C7 C6 116.3(2) . . ? N1 C8 C9 111.5(2) . . ? N2 C9 C8 111.4(2) . . ? N2 C10 C11 112.6(2) . . ? C12 C11 C16 117.9(3) . . ? C12 C11 C10 120.4(3) . . ? C16 C11 C10 121.7(3) . . ? C11 C12 C13 121.2(3) . . ? C11 C12 O2 116.2(2) . . ? C13 C12 O2 122.6(3) . . ? C14 C13 C12 119.0(4) . . ? C15 C14 C13 120.3(3) . . ? C16 C15 C14 119.5(4) . . ? C15 C16 C11 122.0(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.270 _refine_diff_density_min -0.199 _refine_diff_density_rms 0.048 _database_code_depnum_ccdc_archive 'CCDC 937980'