# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Cameron Jones' 'Lucia McDyre' 'Damien M Murphy' 'Andreas Stasch' _publ_contact_author_name 'Cameron Jones' _publ_contact_author_email CAMERON.JONES@SCI.MONASH.EDU.AU _publ_section_title ; Magnesium(I) Reduction of Benzophenone and Anthracene: First Structural Characterisation of a Magnesium Ketyl ; # Attachment 'compound1.CIF' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 752049' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H70 Mg N4 O' _chemical_formula_weight 863.49 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' _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 45.398(9) _cell_length_b 15.262(3) _cell_length_c 14.927(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.02(3) _cell_angle_gamma 90.00 _cell_volume 10214(4) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple-blue _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.123 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3728 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.981 _exptl_absorpt_correction_T_max 0.990 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15588 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0700 _diffrn_reflns_limit_h_min -53 _diffrn_reflns_limit_h_max 53 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 24.90 _reflns_number_total 8652 _reflns_number_gt 5264 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. one and a half molecules of benzene of solvation were located in the asymmetric unit and their carbon atoms were refined anisotropically. The relatively high r-factors for the structure arise from weak diffraction data above the theta angle of 22 deg. for the crystal structure. The molecular connectivity of the compound is unambiguous. ; _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^)+(0.1225P)^2^+10.5163P] 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 8652 _refine_ls_number_parameters 589 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.1282 _refine_ls_R_factor_gt 0.0723 _refine_ls_wR_factor_ref 0.2276 _refine_ls_wR_factor_gt 0.1924 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.055 _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 0.09802(2) 0.22990(7) 0.46225(8) 0.0339(3) Uani 1 1 d . . . O1 O 0.12005(5) 0.30008(16) 0.54961(18) 0.0508(7) Uani 1 1 d . . . N1 N 0.07681(5) 0.29109(16) 0.34805(19) 0.0341(7) Uani 1 1 d . . . C1 C 0.04136(7) 0.2943(2) 0.2051(2) 0.0430(9) Uani 1 1 d . . . H1A H 0.0381 0.3571 0.2125 0.064 Uiso 1 1 calc R . . H1B H 0.0224 0.2657 0.1817 0.064 Uiso 1 1 calc R . . H1C H 0.0554 0.2855 0.1623 0.064 Uiso 1 1 calc R . . N2 N 0.06141(5) 0.15551(16) 0.47747(18) 0.0308(6) Uani 1 1 d . . . C2 C 0.05402(7) 0.2550(2) 0.2953(2) 0.0349(8) Uani 1 1 d . . . N3 N 0.13000(5) 0.14637(17) 0.4209(2) 0.0375(7) Uani 1 1 d . . . C3 C 0.03948(7) 0.1788(2) 0.3207(2) 0.0353(8) Uani 1 1 d . . . H3 H 0.0269 0.1506 0.2725 0.042 Uiso 1 1 calc R . . N4 N 0.19282(7) 0.0051(2) 0.3008(3) 0.0622(10) Uani 1 1 d . . . C4 C 0.04072(6) 0.13841(19) 0.4054(2) 0.0317(8) Uani 1 1 d . . . C5 C 0.01613(7) 0.0735(2) 0.4140(2) 0.0384(8) Uani 1 1 d . . . H5A H 0.0249 0.0158 0.4302 0.058 Uiso 1 1 calc R . . H5B H 0.0027 0.0694 0.3560 0.058 Uiso 1 1 calc R . . H5C H 0.0049 0.0931 0.4613 0.058 Uiso 1 1 calc R . . C6 C 0.08694(7) 0.3764(2) 0.3243(2) 0.0387(8) Uani 1 1 d . . . C7 C 0.07675(7) 0.4501(2) 0.3668(3) 0.0413(9) Uani 1 1 d . . . C8 C 0.08748(8) 0.5322(2) 0.3469(3) 0.0525(10) Uani 1 1 d . . . H8 H 0.0809 0.5828 0.3751 0.063 Uiso 1 1 calc R . . C9 C 0.10741(9) 0.5413(2) 0.2872(3) 0.0625(12) Uani 1 1 d . . . H9 H 0.1144 0.5979 0.2742 0.075 Uiso 1 1 calc R . . C10 C 0.11739(8) 0.4688(2) 0.2461(3) 0.0605(12) Uani 1 1 d . . . H10 H 0.1313 0.4761 0.2052 0.073 Uiso 1 1 calc R . . C11 C 0.10751(7) 0.3846(2) 0.2632(3) 0.0480(10) Uani 1 1 d . . . C12 C 0.05383(8) 0.4432(2) 0.4302(3) 0.0455(9) Uani 1 1 d . . . H12 H 0.0515 0.3796 0.4436 0.055 Uiso 1 1 calc R . . C13 C 0.06338(10) 0.4890(3) 0.5202(3) 0.0765(14) Uani 1 1 d . . . H13A H 0.0828 0.4663 0.5486 0.115 Uiso 1 1 calc R . . H13B H 0.0486 0.4783 0.5601 0.115 Uiso 1 1 calc R . . H13C H 0.0650 0.5522 0.5099 0.115 Uiso 1 1 calc R . . C14 C 0.02355(8) 0.4761(3) 0.3842(3) 0.0670(12) Uani 1 1 d . . . H14A H 0.0246 0.5393 0.3736 0.101 Uiso 1 1 calc R . . H14B H 0.0086 0.4644 0.4233 0.101 Uiso 1 1 calc R . . H14C H 0.0180 0.4458 0.3261 0.101 Uiso 1 1 calc R . . C15 C 0.12052(8) 0.3064(2) 0.2204(3) 0.0545(11) Uani 1 1 d . . . H15 H 0.1094 0.2531 0.2349 0.065 Uiso 1 1 calc R . . C16 C 0.11727(10) 0.3137(3) 0.1174(3) 0.0707(13) Uani 1 1 d . . . H16A H 0.0961 0.3187 0.0917 0.106 Uiso 1 1 calc R . . H16B H 0.1257 0.2613 0.0930 0.106 Uiso 1 1 calc R . . H16C H 0.1280 0.3657 0.1012 0.106 Uiso 1 1 calc R . . C17 C 0.15318(9) 0.2941(3) 0.2614(4) 0.0723(14) Uani 1 1 d . . . H17A H 0.1650 0.3421 0.2420 0.108 Uiso 1 1 calc R . . H17B H 0.1604 0.2382 0.2408 0.108 Uiso 1 1 calc R . . H17C H 0.1551 0.2939 0.3277 0.108 Uiso 1 1 calc R . . C18 C 0.05814(6) 0.1150(2) 0.5625(2) 0.0318(7) Uani 1 1 d . . . C19 C 0.04665(7) 0.1651(2) 0.6286(2) 0.0361(8) Uani 1 1 d . . . C20 C 0.04369(7) 0.1252(2) 0.7105(2) 0.0414(9) Uani 1 1 d . . . H20 H 0.0358 0.1579 0.7555 0.050 Uiso 1 1 calc R . . C21 C 0.05193(7) 0.0391(2) 0.7278(2) 0.0429(9) Uani 1 1 d . . . H21 H 0.0493 0.0128 0.7837 0.051 Uiso 1 1 calc R . . C22 C 0.06394(7) -0.0086(2) 0.6641(2) 0.0412(9) Uani 1 1 d . . . H22 H 0.0701 -0.0674 0.6773 0.049 Uiso 1 1 calc R . . C23 C 0.06731(7) 0.0278(2) 0.5806(2) 0.0354(8) Uani 1 1 d . . . C24 C 0.03781(7) 0.2607(2) 0.6112(3) 0.0429(9) Uani 1 1 d . . . H24 H 0.0520 0.2859 0.5730 0.052 Uiso 1 1 calc R . . C25 C 0.00688(9) 0.2694(3) 0.5573(3) 0.0589(11) Uani 1 1 d . . . H25A H -0.0075 0.2401 0.5897 0.088 Uiso 1 1 calc R . . H25B H 0.0064 0.2422 0.4977 0.088 Uiso 1 1 calc R . . H25C H 0.0017 0.3316 0.5497 0.088 Uiso 1 1 calc R . . C26 C 0.04070(8) 0.3159(2) 0.6970(3) 0.0531(10) Uani 1 1 d . . . H26A H 0.0380 0.3779 0.6806 0.080 Uiso 1 1 calc R . . H26B H 0.0605 0.3073 0.7327 0.080 Uiso 1 1 calc R . . H26C H 0.0254 0.2982 0.7330 0.080 Uiso 1 1 calc R . . C27 C 0.08181(7) -0.0264(2) 0.5138(2) 0.0395(8) Uani 1 1 d . . . H27 H 0.0795 0.0065 0.4552 0.047 Uiso 1 1 calc R . . C28 C 0.11509(8) -0.0359(2) 0.5484(3) 0.0510(10) Uani 1 1 d . . . H28A H 0.1240 0.0223 0.5604 0.076 Uiso 1 1 calc R . . H28B H 0.1247 -0.0658 0.5025 0.076 Uiso 1 1 calc R . . H28C H 0.1180 -0.0703 0.6045 0.076 Uiso 1 1 calc R . . C29 C 0.06731(9) -0.1164(2) 0.4946(3) 0.0562(10) Uani 1 1 d . . . H29A H 0.0764 -0.1462 0.4477 0.084 Uiso 1 1 calc R . . H29B H 0.0459 -0.1091 0.4735 0.084 Uiso 1 1 calc R . . H29C H 0.0703 -0.1515 0.5502 0.084 Uiso 1 1 calc R . . C30 C 0.14232(7) 0.3247(2) 0.6121(3) 0.0400(9) Uani 1 1 d . . . C31 C 0.14616(7) 0.2793(2) 0.6972(3) 0.0403(9) Uani 1 1 d . . . C32 C 0.12243(7) 0.2288(2) 0.7206(3) 0.0451(9) Uani 1 1 d . . . H32 H 0.1048 0.2233 0.6775 0.054 Uiso 1 1 calc R . . C33 C 0.12368(9) 0.1875(3) 0.8024(3) 0.0603(11) Uani 1 1 d . . . H33 H 0.1069 0.1556 0.8157 0.072 Uiso 1 1 calc R . . C34 C 0.14905(11) 0.1921(3) 0.8652(3) 0.0779(14) Uani 1 1 d . . . H34 H 0.1498 0.1651 0.9228 0.093 Uiso 1 1 calc R . . C35 C 0.17382(10) 0.2368(3) 0.8439(3) 0.0735(13) Uani 1 1 d . . . H35 H 0.1917 0.2385 0.8866 0.088 Uiso 1 1 calc R . . C36 C 0.17263(8) 0.2784(3) 0.7616(3) 0.0541(10) Uani 1 1 d . . . H36 H 0.1899 0.3071 0.7477 0.065 Uiso 1 1 calc R . . C37 C 0.15959(7) 0.4004(2) 0.5903(3) 0.0420(9) Uani 1 1 d . . . C38 C 0.17957(7) 0.4488(2) 0.6545(3) 0.0496(10) Uani 1 1 d . . . H38 H 0.1826 0.4314 0.7164 0.060 Uiso 1 1 calc R . . C39 C 0.19462(8) 0.5209(2) 0.6287(4) 0.0608(12) Uani 1 1 d . . . H39 H 0.2081 0.5515 0.6731 0.073 Uiso 1 1 calc R . . C40 C 0.19055(9) 0.5493(3) 0.5408(4) 0.0709(14) Uani 1 1 d . . . H40 H 0.2013 0.5984 0.5240 0.085 Uiso 1 1 calc R . . C41 C 0.17064(10) 0.5057(3) 0.4769(4) 0.0738(13) Uani 1 1 d . . . H41 H 0.1672 0.5259 0.4160 0.089 Uiso 1 1 calc R . . C42 C 0.15558(8) 0.4329(3) 0.5009(3) 0.0563(11) Uani 1 1 d . . . H42 H 0.1421 0.4037 0.4556 0.068 Uiso 1 1 calc R . . C43 C 0.12250(7) 0.0929(2) 0.3495(2) 0.0398(8) Uani 1 1 d . . . H43 H 0.1019 0.0885 0.3253 0.048 Uiso 1 1 calc R . . C44 C 0.14202(7) 0.0439(2) 0.3087(3) 0.0442(9) Uani 1 1 d . . . H44 H 0.1349 0.0066 0.2589 0.053 Uiso 1 1 calc R . . C45 C 0.17266(8) 0.0499(2) 0.3416(3) 0.0491(10) Uani 1 1 d . . . C46 C 0.18059(8) 0.1039(2) 0.4168(3) 0.0545(11) Uani 1 1 d . . . H46 H 0.2010 0.1092 0.4431 0.065 Uiso 1 1 calc R . . C47 C 0.15942(7) 0.1494(2) 0.4531(3) 0.0480(9) Uani 1 1 d . . . H47 H 0.1658 0.1855 0.5042 0.058 Uiso 1 1 calc R . . C48 C 0.22443(10) 0.0177(4) 0.3283(4) 0.106(2) Uani 1 1 d . . . H48A H 0.2286 0.0803 0.3380 0.159 Uiso 1 1 calc R . . H48B H 0.2352 -0.0043 0.2808 0.159 Uiso 1 1 calc R . . H48C H 0.2310 -0.0143 0.3848 0.159 Uiso 1 1 calc R . . C49 C 0.18335(10) -0.0461(3) 0.2184(4) 0.0761(14) Uani 1 1 d . . . H49A H 0.1680 -0.0882 0.2294 0.114 Uiso 1 1 calc R . . H49B H 0.2005 -0.0776 0.2019 0.114 Uiso 1 1 calc R . . H49C H 0.1752 -0.0067 0.1689 0.114 Uiso 1 1 calc R . . C50 C 0.21707(11) 0.2212(4) 0.1457(4) 0.0905(17) Uani 1 1 d . . . H50 H 0.2099 0.2716 0.1729 0.109 Uiso 1 1 calc R . . C51 C 0.19870(12) 0.1692(4) 0.0923(4) 0.0974(18) Uani 1 1 d . . . H51 H 0.1779 0.1816 0.0842 0.117 Uiso 1 1 calc R . . C52 C 0.20815(12) 0.0988(4) 0.0486(4) 0.0996(19) Uani 1 1 d . . . H52 H 0.1946 0.0672 0.0054 0.120 Uiso 1 1 calc R . . C53 C 0.23769(13) 0.0739(4) 0.0677(4) 0.0958(17) Uani 1 1 d U . . H53 H 0.2442 0.0217 0.0421 0.115 Uiso 1 1 calc R . . C54 C 0.25688(12) 0.1230(4) 0.1217(4) 0.108(2) Uani 1 1 d DU . . H54 H 0.2774 0.1073 0.1348 0.129 Uiso 1 1 calc R . . C55 C 0.24603(15) 0.2003(5) 0.1599(5) 0.138(3) Uani 1 1 d DU . . H55 H 0.2597 0.2377 0.1963 0.166 Uiso 1 1 calc R . . C56 C 0.25340(17) 0.2017(5) 0.5784(5) 0.124(2) Uani 1 1 d U . . H56 H 0.2558 0.1691 0.6332 0.149 Uiso 1 1 calc R . . C57 C 0.27097(12) 0.1855(4) 0.5134(6) 0.1012(19) Uani 1 1 d U . . H57 H 0.2854 0.1401 0.5220 0.121 Uiso 1 1 calc R . . C58 C 0.26761(15) 0.2339(5) 0.4378(5) 0.110(2) Uani 1 1 d U . . H58 H 0.2803 0.2231 0.3940 0.132 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 0.0283(6) 0.0327(6) 0.0410(7) 0.0042(5) 0.0065(5) -0.0029(4) O1 0.0374(14) 0.0546(15) 0.0584(18) -0.0103(13) 0.0011(12) -0.0082(11) N1 0.0282(14) 0.0313(14) 0.0442(18) 0.0037(13) 0.0105(12) -0.0009(11) C1 0.042(2) 0.047(2) 0.040(2) 0.0077(17) 0.0081(16) 0.0026(15) N2 0.0289(14) 0.0307(13) 0.0331(17) 0.0000(12) 0.0061(12) -0.0030(11) C2 0.0331(18) 0.0360(17) 0.037(2) -0.0004(15) 0.0087(15) 0.0032(14) N3 0.0302(15) 0.0345(14) 0.0474(19) 0.0029(14) 0.0050(13) -0.0024(11) C3 0.0322(17) 0.0374(17) 0.036(2) -0.0038(16) 0.0051(14) -0.0029(13) N4 0.0378(18) 0.068(2) 0.083(3) -0.012(2) 0.0172(17) 0.0093(15) C4 0.0277(16) 0.0308(16) 0.037(2) -0.0012(15) 0.0078(14) 0.0004(12) C5 0.0328(17) 0.0443(19) 0.038(2) -0.0020(16) 0.0046(15) -0.0072(14) C6 0.0287(17) 0.0370(18) 0.051(2) 0.0136(17) 0.0077(15) -0.0004(13) C7 0.0351(18) 0.0366(18) 0.052(2) 0.0081(17) 0.0052(16) 0.0018(14) C8 0.047(2) 0.0366(19) 0.073(3) 0.0117(19) 0.007(2) 0.0044(16) C9 0.051(2) 0.039(2) 0.099(4) 0.025(2) 0.018(2) -0.0018(17) C10 0.046(2) 0.050(2) 0.090(4) 0.030(2) 0.025(2) 0.0046(18) C11 0.0347(19) 0.0419(19) 0.070(3) 0.0169(19) 0.0153(18) 0.0058(15) C12 0.049(2) 0.0338(18) 0.055(3) 0.0036(18) 0.0139(18) 0.0029(15) C13 0.074(3) 0.094(3) 0.061(3) -0.014(3) 0.009(2) -0.001(3) C14 0.044(2) 0.093(3) 0.066(3) -0.008(3) 0.013(2) 0.008(2) C15 0.051(2) 0.049(2) 0.072(3) 0.017(2) 0.034(2) 0.0080(17) C16 0.076(3) 0.068(3) 0.078(4) 0.018(3) 0.043(3) 0.009(2) C17 0.055(3) 0.065(3) 0.105(4) 0.029(3) 0.039(2) 0.021(2) C18 0.0293(16) 0.0353(17) 0.031(2) -0.0001(15) 0.0066(14) -0.0071(13) C19 0.0311(17) 0.0404(18) 0.038(2) -0.0056(16) 0.0083(15) -0.0091(14) C20 0.0411(19) 0.049(2) 0.036(2) -0.0050(17) 0.0113(16) -0.0101(15) C21 0.046(2) 0.053(2) 0.031(2) 0.0019(18) 0.0084(16) -0.0121(16) C22 0.043(2) 0.0400(19) 0.041(2) 0.0061(17) 0.0077(16) -0.0072(15) C23 0.0322(18) 0.0370(18) 0.037(2) -0.0003(16) 0.0061(14) -0.0056(13) C24 0.043(2) 0.0395(19) 0.049(2) -0.0008(17) 0.0175(17) -0.0016(15) C25 0.066(3) 0.050(2) 0.057(3) -0.008(2) -0.002(2) 0.0105(19) C26 0.047(2) 0.053(2) 0.062(3) -0.014(2) 0.0160(19) -0.0030(17) C27 0.047(2) 0.0355(18) 0.037(2) 0.0050(16) 0.0107(16) -0.0001(14) C28 0.051(2) 0.052(2) 0.051(3) 0.0071(19) 0.0131(18) 0.0108(17) C29 0.077(3) 0.041(2) 0.054(3) -0.0051(19) 0.021(2) -0.0060(18) C30 0.0299(18) 0.0427(19) 0.047(2) -0.0126(18) 0.0056(16) 0.0002(14) C31 0.0312(18) 0.0369(18) 0.053(3) -0.0101(18) 0.0076(16) -0.0035(14) C32 0.0320(18) 0.045(2) 0.059(3) -0.010(2) 0.0094(17) -0.0020(15) C33 0.050(2) 0.061(3) 0.072(3) -0.002(2) 0.015(2) -0.0120(19) C34 0.085(3) 0.085(3) 0.064(3) 0.016(3) 0.014(3) -0.024(3) C35 0.058(3) 0.094(3) 0.064(3) 0.012(3) -0.005(2) -0.020(2) C36 0.041(2) 0.062(2) 0.058(3) -0.002(2) 0.0055(18) -0.0129(18) C37 0.0268(17) 0.0427(19) 0.058(3) -0.0042(18) 0.0124(16) 0.0043(14) C38 0.036(2) 0.041(2) 0.072(3) -0.0086(19) 0.0106(18) -0.0022(15) C39 0.038(2) 0.046(2) 0.101(4) -0.012(2) 0.017(2) -0.0027(17) C40 0.047(2) 0.056(3) 0.114(5) 0.014(3) 0.026(3) -0.006(2) C41 0.058(3) 0.078(3) 0.088(4) 0.026(3) 0.021(3) -0.003(2) C42 0.040(2) 0.061(2) 0.068(3) 0.004(2) 0.0103(19) -0.0016(18) C43 0.0334(18) 0.0409(19) 0.045(2) 0.0060(18) 0.0070(16) -0.0035(14) C44 0.039(2) 0.0416(19) 0.053(3) 0.0012(18) 0.0111(17) -0.0018(15) C45 0.039(2) 0.046(2) 0.063(3) 0.003(2) 0.0130(18) 0.0068(16) C46 0.0288(19) 0.060(2) 0.073(3) -0.002(2) 0.0031(18) 0.0041(17) C47 0.034(2) 0.045(2) 0.064(3) -0.0048(19) 0.0039(17) -0.0007(15) C48 0.043(3) 0.140(5) 0.137(5) -0.040(4) 0.018(3) 0.025(3) C49 0.066(3) 0.076(3) 0.092(4) -0.017(3) 0.031(3) 0.010(2) C50 0.054(3) 0.096(4) 0.124(5) -0.033(4) 0.021(3) 0.003(3) C51 0.061(3) 0.117(5) 0.114(5) -0.027(4) 0.014(3) 0.007(3) C52 0.071(3) 0.118(5) 0.105(5) -0.035(4) -0.004(3) 0.006(3) C53 0.092(4) 0.091(3) 0.101(4) -0.012(3) 0.005(3) 0.014(3) C54 0.062(3) 0.129(4) 0.125(4) -0.045(4) -0.009(3) 0.017(3) C55 0.100(4) 0.155(5) 0.157(5) -0.063(4) 0.013(4) -0.006(4) C56 0.116(4) 0.129(5) 0.123(5) -0.015(4) 0.005(4) -0.017(4) C57 0.062(3) 0.092(4) 0.145(5) -0.034(4) 0.005(3) 0.008(3) C58 0.094(4) 0.120(4) 0.123(5) -0.048(4) 0.035(4) -0.007(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 1.854(3) . ? Mg1 N1 2.047(3) . ? Mg1 N2 2.055(3) . ? Mg1 N3 2.096(3) . ? O1 C30 1.319(4) . ? N1 C2 1.318(4) . ? N1 C6 1.443(4) . ? C1 C2 1.503(5) . ? N2 C4 1.338(4) . ? N2 C18 1.440(4) . ? C2 C3 1.418(4) . ? N3 C43 1.343(4) . ? N3 C47 1.347(4) . ? C3 C4 1.399(5) . ? N4 C45 1.360(5) . ? N4 C48 1.442(5) . ? N4 C49 1.463(5) . ? C4 C5 1.513(4) . ? C6 C7 1.406(5) . ? C6 C11 1.409(5) . ? C7 C8 1.394(5) . ? C7 C12 1.516(5) . ? C8 C9 1.373(6) . ? C9 C10 1.376(6) . ? C10 C11 1.398(5) . ? C11 C15 1.516(5) . ? C12 C13 1.516(6) . ? C12 C14 1.523(5) . ? C15 C17 1.524(5) . ? C15 C16 1.525(6) . ? C18 C23 1.409(4) . ? C18 C19 1.411(5) . ? C19 C20 1.391(5) . ? C19 C24 1.525(5) . ? C20 C21 1.379(5) . ? C21 C22 1.376(5) . ? C22 C23 1.395(5) . ? C23 C27 1.522(5) . ? C24 C25 1.510(5) . ? C24 C26 1.521(5) . ? C27 C28 1.525(5) . ? C27 C29 1.530(5) . ? C30 C31 1.434(5) . ? C30 C37 1.461(5) . ? C31 C32 1.412(5) . ? C31 C36 1.416(5) . ? C32 C33 1.368(5) . ? C33 C34 1.367(6) . ? C34 C35 1.393(6) . ? C35 C36 1.376(6) . ? C37 C42 1.408(5) . ? C37 C38 1.420(5) . ? C38 C39 1.381(5) . ? C39 C40 1.367(6) . ? C40 C41 1.378(7) . ? C41 C42 1.382(6) . ? C43 C44 1.373(5) . ? C44 C45 1.404(5) . ? C45 C46 1.394(5) . ? C46 C47 1.364(5) . ? C50 C51 1.323(7) . ? C50 C55 1.337(7) . ? C51 C52 1.361(7) . ? C52 C53 1.380(7) . ? C53 C54 1.323(7) . ? C54 C55 1.432(6) . ? C56 C58 1.364(9) 7_556 ? C56 C57 1.372(9) . ? C57 C58 1.337(9) . ? C58 C56 1.364(9) 7_556 ? 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 N1 116.97(12) . . ? O1 Mg1 N2 126.71(12) . . ? N1 Mg1 N2 93.50(11) . . ? O1 Mg1 N3 103.67(11) . . ? N1 Mg1 N3 106.81(12) . . ? N2 Mg1 N3 107.83(11) . . ? C30 O1 Mg1 158.7(2) . . ? C2 N1 C6 118.7(3) . . ? C2 N1 Mg1 122.0(2) . . ? C6 N1 Mg1 119.3(2) . . ? C4 N2 C18 118.0(2) . . ? C4 N2 Mg1 119.8(2) . . ? C18 N2 Mg1 122.11(19) . . ? N1 C2 C3 122.5(3) . . ? N1 C2 C1 121.5(3) . . ? C3 C2 C1 116.0(3) . . ? C43 N3 C47 114.7(3) . . ? C43 N3 Mg1 120.1(2) . . ? C47 N3 Mg1 124.6(2) . . ? C4 C3 C2 130.4(3) . . ? C45 N4 C48 121.0(4) . . ? C45 N4 C49 121.0(3) . . ? C48 N4 C49 117.3(3) . . ? N2 C4 C3 124.3(3) . . ? N2 C4 C5 119.6(3) . . ? C3 C4 C5 116.1(3) . . ? C7 C6 C11 121.3(3) . . ? C7 C6 N1 118.1(3) . . ? C11 C6 N1 120.6(3) . . ? C8 C7 C6 118.2(3) . . ? C8 C7 C12 119.5(3) . . ? C6 C7 C12 122.2(3) . . ? C9 C8 C7 121.1(4) . . ? C8 C9 C10 120.3(3) . . ? C9 C10 C11 121.4(4) . . ? C10 C11 C6 117.6(3) . . ? C10 C11 C15 119.2(3) . . ? C6 C11 C15 123.0(3) . . ? C13 C12 C7 113.1(3) . . ? C13 C12 C14 111.1(3) . . ? C7 C12 C14 110.8(3) . . ? C11 C15 C17 110.3(4) . . ? C11 C15 C16 112.7(3) . . ? C17 C15 C16 110.4(3) . . ? C23 C18 C19 120.6(3) . . ? C23 C18 N2 120.4(3) . . ? C19 C18 N2 119.0(3) . . ? C20 C19 C18 118.4(3) . . ? C20 C19 C24 120.6(3) . . ? C18 C19 C24 121.0(3) . . ? C21 C20 C19 121.4(3) . . ? C22 C21 C20 120.0(3) . . ? C21 C22 C23 121.2(3) . . ? C22 C23 C18 118.5(3) . . ? C22 C23 C27 119.2(3) . . ? C18 C23 C27 122.2(3) . . ? C25 C24 C26 110.5(3) . . ? C25 C24 C19 111.9(3) . . ? C26 C24 C19 113.6(3) . . ? C23 C27 C28 109.7(3) . . ? C23 C27 C29 113.2(3) . . ? C28 C27 C29 110.6(3) . . ? O1 C30 C31 117.5(3) . . ? O1 C30 C37 116.5(3) . . ? C31 C30 C37 125.8(3) . . ? C32 C31 C36 115.2(4) . . ? C32 C31 C30 119.4(3) . . ? C36 C31 C30 125.3(3) . . ? C33 C32 C31 123.1(3) . . ? C34 C33 C32 120.0(4) . . ? C33 C34 C35 119.5(4) . . ? C36 C35 C34 120.6(4) . . ? C35 C36 C31 121.4(4) . . ? C42 C37 C38 115.5(3) . . ? C42 C37 C30 119.7(3) . . ? C38 C37 C30 124.7(4) . . ? C39 C38 C37 121.2(4) . . ? C40 C39 C38 121.4(4) . . ? C39 C40 C41 119.2(4) . . ? C40 C41 C42 120.4(5) . . ? C41 C42 C37 122.2(4) . . ? N3 C43 C44 125.6(3) . . ? C43 C44 C45 118.8(3) . . ? N4 C45 C46 123.4(3) . . ? N4 C45 C44 120.6(4) . . ? C46 C45 C44 115.9(3) . . ? C47 C46 C45 120.7(3) . . ? N3 C47 C46 124.2(4) . . ? C51 C50 C55 117.6(5) . . ? C50 C51 C52 123.1(5) . . ? C51 C52 C53 119.2(5) . . ? C54 C53 C52 119.7(5) . . ? C53 C54 C55 118.3(5) . . ? C50 C55 C54 121.7(6) . . ? C58 C56 C57 118.2(7) 7_556 . ? C58 C57 C56 119.6(6) . . ? C57 C58 C56 122.1(7) . 7_556 ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 24.90 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.691 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.058 # Attachment 'compound2.CIF' data_compound2 _database_code_depnum_ccdc_archive 'CCDC 752050' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63.50 H72 Mg2 N4' _chemical_formula_weight 939.87 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' Mg Mg 0.0486 0.0363 '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 14.933(3) _cell_length_b 21.081(4) _cell_length_c 34.381(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.97(3) _cell_angle_gamma 90.00 _cell_volume 10783(4) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'deep red' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.158 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4040 _exptl_absorpt_coefficient_mu 0.088 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9784 _exptl_absorpt_correction_T_max 0.9913 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36366 _diffrn_reflns_av_R_equivalents 0.2127 _diffrn_reflns_av_sigmaI/netI 0.2918 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.00 _reflns_number_total 18904 _reflns_number_gt 6116 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Two molecules were located in the asymmetric unit and successfully refined. There are no significant geometric differences between them. Two molecules of toluene were also located in the asymmetric unit. Their atomic sites were refined isotropically with 50% occupancy of the sites. The isotropic displacement parameters for the carbon atoms of these molecules were high, which is reflected in the relatively high r-factors for the structure. Moreover, the diffraction data for the crystal structure above the theta angle of 22 deg. are weak, which is also reflected in the relatively high r-factors for the structure. The gross molecular framework for the compound 2 is, however, unambiguous. Attempts to solve and refine the crystal structure in higher symmetry space groups were not successful. ; _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^)+(0.1189P)^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 18904 _refine_ls_number_parameters 1270 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.2920 _refine_ls_R_factor_gt 0.0931 _refine_ls_wR_factor_ref 0.2782 _refine_ls_wR_factor_gt 0.1935 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_restrained_S_all 1.026 _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 -0.13219(14) 0.19359(11) 0.85840(6) 0.0383(6) Uani 1 1 d . . . Mg2 Mg 0.14403(14) 0.33860(11) 0.88397(6) 0.0373(6) Uani 1 1 d . . . Mg3 Mg 0.34744(14) 0.65679(12) 0.36429(6) 0.0385(6) Uani 1 1 d . . . Mg4 Mg 0.62477(14) 0.80553(11) 0.38762(6) 0.0388(6) Uani 1 1 d . . . N1 N -0.2658(3) 0.2045(3) 0.86113(15) 0.0351(14) Uani 1 1 d . . . N2 N -0.1474(3) 0.1457(3) 0.80749(14) 0.0360(15) Uani 1 1 d . . . N3 N 0.1868(3) 0.4234(2) 0.90564(14) 0.0305(14) Uani 1 1 d . . . N4 N 0.2529(4) 0.2928(3) 0.91105(15) 0.0386(15) Uani 1 1 d . . . N5 N 0.2145(3) 0.6714(3) 0.36755(15) 0.0371(15) Uani 1 1 d . . . N6 N 0.3288(3) 0.6126(3) 0.31175(14) 0.0349(15) Uani 1 1 d . . . N7 N 0.6772(4) 0.8909(3) 0.40560(15) 0.0362(15) Uani 1 1 d . . . N8 N 0.7390(4) 0.7582(3) 0.40754(15) 0.0377(15) Uani 1 1 d . . . C1 C -0.4266(4) 0.1943(3) 0.83968(19) 0.047(2) Uani 1 1 d . . . H1A H -0.4425 0.1779 0.8649 0.071 Uiso 1 1 calc R . . H1B H -0.4637 0.1734 0.8185 0.071 Uiso 1 1 calc R . . H1C H -0.4371 0.2401 0.8385 0.071 Uiso 1 1 calc R . . C2 C -0.3285(4) 0.1809(3) 0.8353(2) 0.0385(19) Uani 1 1 d . . . C3 C -0.3096(4) 0.1436(3) 0.80292(18) 0.0358(18) Uani 1 1 d . . . H3 H -0.3603 0.1258 0.7883 0.043 Uiso 1 1 calc R . . C4 C -0.2262(5) 0.1295(3) 0.78954(19) 0.0367(18) Uani 1 1 d . . . C5 C -0.2280(4) 0.0941(3) 0.75108(18) 0.048(2) Uani 1 1 d . . . H5A H -0.2064 0.1220 0.7311 0.071 Uiso 1 1 calc R . . H5B H -0.2897 0.0807 0.7430 0.071 Uiso 1 1 calc R . . H5C H -0.1891 0.0567 0.7543 0.071 Uiso 1 1 calc R . . C6 C -0.2931(4) 0.2456(4) 0.89159(19) 0.0385(19) Uani 1 1 d . . . C7 C -0.2948(4) 0.3115(4) 0.8857(2) 0.043(2) Uani 1 1 d . . . C8 C -0.3170(4) 0.3503(4) 0.9158(2) 0.046(2) Uani 1 1 d . . . H8 H -0.3180 0.3949 0.9119 0.056 Uiso 1 1 calc R . . C9 C -0.3377(5) 0.3264(4) 0.9514(2) 0.048(2) Uani 1 1 d . . . C10 C -0.3328(4) 0.2614(4) 0.9569(2) 0.047(2) Uani 1 1 d . . . H10 H -0.3453 0.2442 0.9814 0.057 Uiso 1 1 calc R . . C11 C -0.3103(4) 0.2204(4) 0.9276(2) 0.044(2) Uani 1 1 d . . . C12 C -0.2710(4) 0.3388(3) 0.84745(17) 0.047(2) Uani 1 1 d . . . H12A H -0.2107 0.3248 0.8423 0.070 Uiso 1 1 calc R . . H12B H -0.2724 0.3853 0.8488 0.070 Uiso 1 1 calc R . . H12C H -0.3146 0.3242 0.8264 0.070 Uiso 1 1 calc R . . C13 C -0.3654(5) 0.3704(4) 0.9836(2) 0.066(3) Uani 1 1 d . . . H13A H -0.4274 0.3847 0.9771 0.099 Uiso 1 1 calc R . . H13B H -0.3252 0.4072 0.9858 0.099 Uiso 1 1 calc R . . H13C H -0.3615 0.3475 1.0085 0.099 Uiso 1 1 calc R . . C14 C -0.3043(5) 0.1502(4) 0.93488(19) 0.060(2) Uani 1 1 d . . . H14A H -0.3145 0.1415 0.9621 0.090 Uiso 1 1 calc R . . H14B H -0.2445 0.1350 0.9297 0.090 Uiso 1 1 calc R . . H14C H -0.3500 0.1283 0.9176 0.090 Uiso 1 1 calc R . . C15 C -0.0662(4) 0.1375(4) 0.78808(18) 0.0386(19) Uani 1 1 d . . . C16 C -0.0110(4) 0.0845(4) 0.79703(18) 0.0387(19) Uani 1 1 d . . . C17 C 0.0727(4) 0.0825(3) 0.78217(19) 0.043(2) Uani 1 1 d . . . H17 H 0.1112 0.0474 0.7885 0.052 Uiso 1 1 calc R . . C18 C 0.1019(5) 0.1305(4) 0.7583(2) 0.045(2) Uani 1 1 d . . . C19 C 0.0438(4) 0.1806(4) 0.74901(18) 0.042(2) Uani 1 1 d . . . H19 H 0.0624 0.2128 0.7322 0.050 Uiso 1 1 calc R . . C20 C -0.0403(4) 0.1860(3) 0.76312(18) 0.0364(18) Uani 1 1 d . . . C21 C -0.0395(5) 0.0317(3) 0.82304(19) 0.055(2) Uani 1 1 d . . . H21A H -0.0915 0.0095 0.8100 0.082 Uiso 1 1 calc R . . H21B H -0.0559 0.0496 0.8478 0.082 Uiso 1 1 calc R . . H21C H 0.0103 0.0017 0.8282 0.082 Uiso 1 1 calc R . . C22 C 0.1958(5) 0.1292(4) 0.7448(2) 0.065(3) Uani 1 1 d . . . H22A H 0.1926 0.1171 0.7172 0.097 Uiso 1 1 calc R . . H22B H 0.2324 0.0982 0.7603 0.097 Uiso 1 1 calc R . . H22C H 0.2230 0.1714 0.7481 0.097 Uiso 1 1 calc R . . C23 C -0.0978(4) 0.2428(3) 0.75529(18) 0.045(2) Uani 1 1 d . . . H23A H -0.1590 0.2295 0.7463 0.068 Uiso 1 1 calc R . . H23B H -0.0733 0.2688 0.7351 0.068 Uiso 1 1 calc R . . H23C H -0.0991 0.2678 0.7793 0.068 Uiso 1 1 calc R . . C24 C 0.2796(4) 0.4989(3) 0.94559(18) 0.0401(19) Uani 1 1 d . . . H24A H 0.2901 0.5263 0.9234 0.060 Uiso 1 1 calc R . . H24B H 0.3335 0.4983 0.9640 0.060 Uiso 1 1 calc R . . H24C H 0.2287 0.5153 0.9587 0.060 Uiso 1 1 calc R . . C25 C 0.2587(5) 0.4319(3) 0.93104(19) 0.0362(18) Uani 1 1 d . . . C26 C 0.3188(4) 0.3840(4) 0.94449(18) 0.0356(18) Uani 1 1 d . . . H26 H 0.3674 0.3972 0.9623 0.043 Uiso 1 1 calc R . . C27 C 0.3165(5) 0.3198(4) 0.93517(19) 0.0393(19) Uani 1 1 d . . . C28 C 0.3923(4) 0.2792(3) 0.95326(19) 0.050(2) Uani 1 1 d . . . H28A H 0.3676 0.2449 0.9684 0.075 Uiso 1 1 calc R . . H28B H 0.4329 0.3053 0.9706 0.075 Uiso 1 1 calc R . . H28C H 0.4256 0.2610 0.9326 0.075 Uiso 1 1 calc R . . C29 C 0.1320(4) 0.4774(3) 0.89394(18) 0.0351(18) Uani 1 1 d . . . C30 C 0.1457(4) 0.5088(3) 0.85951(18) 0.0345(18) Uani 1 1 d . . . C31 C 0.0879(4) 0.5582(3) 0.84713(19) 0.0380(19) Uani 1 1 d . . . H31 H 0.0970 0.5796 0.8235 0.046 Uiso 1 1 calc R . . C32 C 0.0181(4) 0.5769(3) 0.86807(19) 0.0388(19) Uani 1 1 d . . . C33 C 0.0054(4) 0.5445(3) 0.90279(17) 0.0359(19) Uani 1 1 d . . . H33 H -0.0425 0.5569 0.9176 0.043 Uiso 1 1 calc R . . C34 C 0.0608(4) 0.4949(3) 0.91600(17) 0.0326(18) Uani 1 1 d . . . C35 C 0.2214(4) 0.4886(3) 0.83530(17) 0.044(2) Uani 1 1 d . . . H35A H 0.2066 0.4475 0.8230 0.066 Uiso 1 1 calc R . . H35B H 0.2773 0.4848 0.8523 0.066 Uiso 1 1 calc R . . H35C H 0.2289 0.5204 0.8151 0.066 Uiso 1 1 calc R . . C36 C -0.0411(4) 0.6325(3) 0.85484(19) 0.051(2) Uani 1 1 d . . . H36A H -0.0120 0.6722 0.8640 0.077 Uiso 1 1 calc R . . H36B H -0.0993 0.6286 0.8657 0.077 Uiso 1 1 calc R . . H36C H -0.0502 0.6329 0.8263 0.077 Uiso 1 1 calc R . . C37 C 0.0425(4) 0.4587(3) 0.95267(17) 0.047(2) Uani 1 1 d . . . H37A H 0.0444 0.4131 0.9475 0.070 Uiso 1 1 calc R . . H37B H -0.0171 0.4702 0.9604 0.070 Uiso 1 1 calc R . . H37C H 0.0882 0.4696 0.9738 0.070 Uiso 1 1 calc R . . C38 C 0.2546(4) 0.2249(4) 0.90580(19) 0.0346(18) Uani 1 1 d . . . C39 C 0.2920(4) 0.1986(4) 0.8733(2) 0.0383(18) Uani 1 1 d . . . C40 C 0.2871(4) 0.1341(4) 0.8678(2) 0.048(2) Uani 1 1 d . . . H40 H 0.3121 0.1163 0.8457 0.058 Uiso 1 1 calc R . . C41 C 0.2468(5) 0.0934(4) 0.8934(2) 0.054(2) Uani 1 1 d . . . C42 C 0.2102(5) 0.1210(4) 0.9254(2) 0.049(2) Uani 1 1 d . . . H42 H 0.1833 0.0947 0.9435 0.059 Uiso 1 1 calc R . . C43 C 0.2123(4) 0.1856(4) 0.93116(19) 0.0415(19) Uani 1 1 d . . . C44 C 0.3361(4) 0.2392(3) 0.84467(19) 0.049(2) Uani 1 1 d . . . H44A H 0.3904 0.2586 0.8576 0.073 Uiso 1 1 calc R . . H44B H 0.2944 0.2725 0.8348 0.073 Uiso 1 1 calc R . . H44C H 0.3525 0.2130 0.8228 0.073 Uiso 1 1 calc R . . C45 C 0.2423(5) 0.0232(4) 0.8864(2) 0.077(3) Uani 1 1 d . . . H45A H 0.2383 0.0149 0.8583 0.115 Uiso 1 1 calc R . . H45B H 0.1891 0.0058 0.8974 0.115 Uiso 1 1 calc R . . H45C H 0.2964 0.0030 0.8989 0.115 Uiso 1 1 calc R . . C46 C 0.1641(4) 0.2143(3) 0.96405(18) 0.049(2) Uani 1 1 d . . . H46A H 0.2056 0.2419 0.9799 0.074 Uiso 1 1 calc R . . H46B H 0.1430 0.1803 0.9805 0.074 Uiso 1 1 calc R . . H46C H 0.1126 0.2392 0.9531 0.074 Uiso 1 1 calc R . . C47 C -0.0762(4) 0.2662(4) 0.90942(18) 0.0391(19) Uani 1 1 d . . . H47 H -0.1191 0.2941 0.9191 0.047 Uiso 1 1 calc R . . C48 C -0.0700(4) 0.2050(4) 0.9242(2) 0.046(2) Uani 1 1 d . . . H48 H -0.1017 0.1935 0.9460 0.055 Uiso 1 1 calc R . . C49 C -0.0172(5) 0.1603(4) 0.90699(19) 0.048(2) Uani 1 1 d . . . H49 H -0.0115 0.1184 0.9170 0.058 Uiso 1 1 calc R . . C50 C 0.0281(4) 0.1792(3) 0.87394(18) 0.0362(18) Uani 1 1 d . . . H50 H 0.0556 0.1477 0.8592 0.043 Uiso 1 1 calc R . . C51 C 0.0330(4) 0.2436(4) 0.86259(18) 0.0365(18) Uani 1 1 d . . . C52 C 0.0919(4) 0.2667(3) 0.83515(18) 0.0395(19) Uani 1 1 d . . . H52 H 0.1457 0.2444 0.8312 0.047 Uiso 1 1 calc R . . C53 C 0.0694(4) 0.3245(4) 0.8132(2) 0.0403(19) Uani 1 1 d . . . C54 C 0.1013(5) 0.3388(4) 0.7773(2) 0.048(2) Uani 1 1 d . . . H54 H 0.1381 0.3092 0.7652 0.058 Uiso 1 1 calc R . . C55 C 0.0793(5) 0.3958(4) 0.7592(2) 0.060(2) Uani 1 1 d . . . H55 H 0.1044 0.4060 0.7355 0.072 Uiso 1 1 calc R . . C56 C 0.0228(6) 0.4378(4) 0.7745(2) 0.060(2) Uani 1 1 d . . . H56 H 0.0071 0.4761 0.7611 0.072 Uiso 1 1 calc R . . C57 C -0.0124(5) 0.4242(4) 0.8104(2) 0.054(2) Uani 1 1 d . . . H57 H -0.0530 0.4528 0.8210 0.065 Uiso 1 1 calc R . . C58 C 0.0128(4) 0.3686(4) 0.8303(2) 0.0416(19) Uani 1 1 d . . . C59 C -0.0130(4) 0.3529(4) 0.86992(19) 0.042(2) Uani 1 1 d . . . H59 H -0.0235 0.3857 0.8879 0.050 Uiso 1 1 calc R . . C60 C -0.0218(4) 0.2895(4) 0.88054(18) 0.0342(18) Uani 1 1 d . . . C61 C 0.0533(4) 0.6640(3) 0.34690(19) 0.049(2) Uani 1 1 d . . . H61A H 0.0379 0.6504 0.3728 0.073 Uiso 1 1 calc R . . H61B H 0.0146 0.6419 0.3268 0.073 Uiso 1 1 calc R . . H61C H 0.0442 0.7098 0.3442 0.073 Uiso 1 1 calc R . . C62 C 0.1511(5) 0.6480(3) 0.3423(2) 0.0396(19) Uani 1 1 d . . . C63 C 0.1677(4) 0.6113(3) 0.30959(18) 0.0390(19) Uani 1 1 d . . . H63 H 0.1159 0.5933 0.2958 0.047 Uiso 1 1 calc R . . C64 C 0.2493(5) 0.5974(3) 0.29453(18) 0.0381(19) Uani 1 1 d . . . C65 C 0.2436(4) 0.5651(3) 0.25497(17) 0.0424(19) Uani 1 1 d . . . H65A H 0.2643 0.5944 0.2355 0.064 Uiso 1 1 calc R . . H65B H 0.1812 0.5529 0.2474 0.064 Uiso 1 1 calc R . . H65C H 0.2817 0.5272 0.2564 0.064 Uiso 1 1 calc R . . C66 C 0.1892(4) 0.7150(4) 0.3972(2) 0.0388(19) Uani 1 1 d . . . C67 C 0.1924(4) 0.7802(4) 0.38996(19) 0.0350(18) Uani 1 1 d . . . C68 C 0.1701(4) 0.8213(3) 0.41924(19) 0.0396(19) Uani 1 1 d . . . H68 H 0.1713 0.8657 0.4144 0.048 Uiso 1 1 calc R . . C69 C 0.1462(4) 0.8004(4) 0.45507(18) 0.0379(19) Uani 1 1 d . . . C70 C 0.1468(4) 0.7356(4) 0.4618(2) 0.047(2) Uani 1 1 d . . . H70 H 0.1324 0.7204 0.4865 0.057 Uiso 1 1 calc R . . C71 C 0.1675(4) 0.6921(4) 0.43359(19) 0.043(2) Uani 1 1 d . . . C72 C 0.2194(4) 0.8047(3) 0.35164(16) 0.042(2) Uani 1 1 d . . . H72A H 0.1734 0.7931 0.3308 0.063 Uiso 1 1 calc R . . H72B H 0.2771 0.7858 0.3463 0.063 Uiso 1 1 calc R . . H72C H 0.2253 0.8509 0.3529 0.063 Uiso 1 1 calc R . . C73 C 0.1185(5) 0.8458(4) 0.48586(19) 0.059(2) Uani 1 1 d . . . H73A H 0.1118 0.8885 0.4747 0.088 Uiso 1 1 calc R . . H73B H 0.1646 0.8463 0.5080 0.088 Uiso 1 1 calc R . . H73C H 0.0611 0.8320 0.4949 0.088 Uiso 1 1 calc R . . C74 C 0.1702(5) 0.6221(4) 0.4422(2) 0.058(2) Uani 1 1 d . . . H74A H 0.1214 0.6009 0.4263 0.087 Uiso 1 1 calc R . . H74B H 0.1630 0.6152 0.4699 0.087 Uiso 1 1 calc R . . H74C H 0.2280 0.6047 0.4358 0.087 Uiso 1 1 calc R . . C75 C 0.4085(4) 0.6055(4) 0.29066(18) 0.0380(19) Uani 1 1 d . . . C76 C 0.4629(5) 0.5524(4) 0.29692(19) 0.044(2) Uani 1 1 d . . . C77 C 0.5442(5) 0.5508(4) 0.2793(2) 0.048(2) Uani 1 1 d . . . H77 H 0.5823 0.5149 0.2837 0.057 Uiso 1 1 calc R . . C78 C 0.5713(5) 0.5993(4) 0.2559(2) 0.048(2) Uani 1 1 d . . . C79 C 0.5135(4) 0.6506(4) 0.24913(18) 0.0417(19) Uani 1 1 d . . . H79 H 0.5294 0.6836 0.2322 0.050 Uiso 1 1 calc R . . C80 C 0.4317(4) 0.6551(4) 0.26677(18) 0.0376(19) Uani 1 1 d . . . C81 C 0.4353(5) 0.4982(3) 0.3221(2) 0.056(2) Uani 1 1 d . . . H81A H 0.3796 0.4792 0.3103 0.084 Uiso 1 1 calc R . . H81B H 0.4256 0.5142 0.3482 0.084 Uiso 1 1 calc R . . H81C H 0.4830 0.4661 0.3243 0.084 Uiso 1 1 calc R . . C82 C 0.6609(5) 0.5966(4) 0.2390(2) 0.077(3) Uani 1 1 d . . . H82A H 0.6615 0.5609 0.2207 0.116 Uiso 1 1 calc R . . H82B H 0.7087 0.5908 0.2601 0.116 Uiso 1 1 calc R . . H82C H 0.6710 0.6363 0.2251 0.116 Uiso 1 1 calc R . . C83 C 0.3738(4) 0.7129(3) 0.26075(18) 0.045(2) Uani 1 1 d . . . H83A H 0.3130 0.7003 0.2506 0.067 Uiso 1 1 calc R . . H83B H 0.3994 0.7412 0.2420 0.067 Uiso 1 1 calc R . . H83C H 0.3711 0.7351 0.2857 0.067 Uiso 1 1 calc R . . C84 C 0.7775(4) 0.9639(3) 0.44377(19) 0.045(2) Uani 1 1 d . . . H84A H 0.7900 0.9908 0.4216 0.067 Uiso 1 1 calc R . . H84B H 0.8312 0.9615 0.4622 0.067 Uiso 1 1 calc R . . H84C H 0.7277 0.9821 0.4569 0.067 Uiso 1 1 calc R . . C85 C 0.7520(4) 0.8972(3) 0.42908(19) 0.0329(17) Uani 1 1 d . . . C86 C 0.8112(4) 0.8493(3) 0.43900(17) 0.0307(17) Uani 1 1 d . . . H86 H 0.8618 0.8613 0.4561 0.037 Uiso 1 1 calc R . . C87 C 0.8092(4) 0.7855(4) 0.42800(19) 0.0360(18) Uani 1 1 d . . . C88 C 0.8920(4) 0.7458(3) 0.43930(18) 0.046(2) Uani 1 1 d . . . H88A H 0.8741 0.7063 0.4516 0.069 Uiso 1 1 calc R . . H88B H 0.9330 0.7695 0.4577 0.069 Uiso 1 1 calc R . . H88C H 0.9223 0.7358 0.4159 0.069 Uiso 1 1 calc R . . C89 C 0.6243(4) 0.9463(3) 0.39532(18) 0.0335(18) Uani 1 1 d . . . C90 C 0.5577(4) 0.9671(3) 0.41851(18) 0.0335(18) Uani 1 1 d . . . C91 C 0.5075(4) 1.0199(4) 0.40675(19) 0.0405(19) Uani 1 1 d . . . H91 H 0.4639 1.0352 0.4230 0.049 Uiso 1 1 calc R . . C92 C 0.5186(4) 1.0516(3) 0.3719(2) 0.0366(18) Uani 1 1 d . . . C93 C 0.5825(4) 1.0284(3) 0.34836(18) 0.0395(19) Uani 1 1 d . . . H93 H 0.5896 1.0483 0.3240 0.047 Uiso 1 1 calc R . . C94 C 0.6357(4) 0.9772(3) 0.35980(18) 0.0327(17) Uani 1 1 d . . . C95 C 0.5428(4) 0.9349(3) 0.45630(17) 0.0393(19) Uani 1 1 d . . . H95A H 0.5960 0.9405 0.4748 0.059 Uiso 1 1 calc R . . H95B H 0.5324 0.8895 0.4516 0.059 Uiso 1 1 calc R . . H95C H 0.4903 0.9535 0.4672 0.059 Uiso 1 1 calc R . . C96 C 0.4653(5) 1.1107(3) 0.36092(19) 0.052(2) Uani 1 1 d . . . H96A H 0.4038 1.1057 0.3683 0.077 Uiso 1 1 calc R . . H96B H 0.4640 1.1175 0.3327 0.077 Uiso 1 1 calc R . . H96C H 0.4935 1.1472 0.3747 0.077 Uiso 1 1 calc R . . C97 C 0.7053(4) 0.9539(3) 0.33380(18) 0.0431(19) Uani 1 1 d . . . H97A H 0.7067 0.9823 0.3113 0.065 Uiso 1 1 calc R . . H97B H 0.6897 0.9109 0.3247 0.065 Uiso 1 1 calc R . . H97C H 0.7644 0.9535 0.3485 0.065 Uiso 1 1 calc R . . C98 C 0.7425(4) 0.6917(3) 0.39825(19) 0.0328(17) Uani 1 1 d . . . C99 C 0.7055(4) 0.6484(4) 0.42217(19) 0.0352(18) Uani 1 1 d . . . C100 C 0.7047(4) 0.5845(4) 0.4113(2) 0.045(2) Uani 1 1 d . . . H100 H 0.6802 0.5542 0.4280 0.054 Uiso 1 1 calc R . . C101 C 0.7381(4) 0.5637(4) 0.3773(2) 0.0437(19) Uani 1 1 d . . . C102 C 0.7730(4) 0.6080(4) 0.3540(2) 0.044(2) Uani 1 1 d . . . H102 H 0.7954 0.5944 0.3303 0.053 Uiso 1 1 calc R . . C103 C 0.7773(4) 0.6725(4) 0.36309(19) 0.0394(19) Uani 1 1 d . . . C104 C 0.6642(4) 0.6684(3) 0.45859(18) 0.046(2) Uani 1 1 d . . . H10A H 0.7084 0.6925 0.4754 0.070 Uiso 1 1 calc R . . H10B H 0.6459 0.6307 0.4726 0.070 Uiso 1 1 calc R . . H10C H 0.6115 0.6950 0.4515 0.070 Uiso 1 1 calc R . . C105 C 0.7307(5) 0.4937(3) 0.3653(2) 0.064(2) Uani 1 1 d . . . H10D H 0.7789 0.4695 0.3797 0.096 Uiso 1 1 calc R . . H10E H 0.7362 0.4899 0.3372 0.096 Uiso 1 1 calc R . . H10F H 0.6723 0.4770 0.3714 0.096 Uiso 1 1 calc R . . C106 C 0.8125(4) 0.7199(3) 0.33569(19) 0.048(2) Uani 1 1 d . . . H10G H 0.8331 0.6977 0.3130 0.072 Uiso 1 1 calc R . . H10H H 0.8629 0.7431 0.3492 0.072 Uiso 1 1 calc R . . H10I H 0.7646 0.7497 0.3269 0.072 Uiso 1 1 calc R . . C107 C 0.4071(4) 0.7249(4) 0.41865(19) 0.048(2) Uani 1 1 d . . . H107 H 0.3660 0.7515 0.4305 0.057 Uiso 1 1 calc R . . C108 C 0.4152(5) 0.6613(4) 0.4308(2) 0.051(2) Uani 1 1 d . . . H108 H 0.3868 0.6467 0.4528 0.061 Uiso 1 1 calc R . . C109 C 0.4649(4) 0.6206(4) 0.4100(2) 0.044(2) Uani 1 1 d . . . H109 H 0.4713 0.5774 0.4178 0.053 Uiso 1 1 calc R . . C110 C 0.5066(4) 0.6426(3) 0.37721(18) 0.0376(19) Uani 1 1 d . . . H110 H 0.5333 0.6127 0.3611 0.045 Uiso 1 1 calc R . . C112 C 0.5100(4) 0.7071(4) 0.36773(18) 0.0356(18) Uani 1 1 d . . . C113 C 0.5631(4) 0.7346(3) 0.33978(18) 0.0389(19) Uani 1 1 d . . . H113 H 0.6164 0.7139 0.3335 0.047 Uiso 1 1 calc R . . C114 C 0.5365(5) 0.7939(4) 0.3208(2) 0.048(2) Uani 1 1 d . . . C115 C 0.5622(6) 0.8130(5) 0.2840(2) 0.066(3) Uani 1 1 d . . . H115 H 0.5975 0.7854 0.2697 0.080 Uiso 1 1 calc R . . C116 C 0.5365(7) 0.8713(6) 0.2688(3) 0.091(4) Uani 1 1 d . . . H116 H 0.5554 0.8844 0.2444 0.110 Uiso 1 1 calc R . . C117 C 0.4835(7) 0.9104(5) 0.2890(4) 0.093(4) Uani 1 1 d . . . H117 H 0.4649 0.9501 0.2780 0.112 Uiso 1 1 calc R . . C118 C 0.4566(6) 0.8932(4) 0.3251(3) 0.074(3) Uani 1 1 d . . . H118 H 0.4191 0.9207 0.3384 0.089 Uiso 1 1 calc R . . C119 C 0.4841(5) 0.8364(4) 0.3415(2) 0.050(2) Uani 1 1 d . . . C120 C 0.4664(4) 0.8165(3) 0.3812(2) 0.042(2) Uani 1 1 d . . . H120 H 0.4610 0.8472 0.4010 0.051 Uiso 1 1 calc R . . C121 C 0.4576(4) 0.7513(3) 0.38947(18) 0.0346(18) Uani 1 1 d . . . C122 C -0.5297(14) 0.1052(9) 0.9470(5) 0.127(8) Uiso 0.50 1 d PD A -1 H12D H -0.5100 0.1410 0.9638 0.191 Uiso 0.50 1 calc PR A -1 H12E H -0.5920 0.1119 0.9364 0.191 Uiso 0.50 1 calc PR A -1 H12F H -0.4910 0.1020 0.9254 0.191 Uiso 0.50 1 calc PR A -1 C123 C -0.5234(12) 0.0448(10) 0.9704(7) 0.091(9) Uiso 0.50 1 d PD A -1 C124 C -0.4425(14) 0.0248(11) 0.9882(7) 0.076(8) Uiso 0.50 1 d PD A -1 H124 H -0.3907 0.0457 0.9803 0.091 Uiso 0.50 1 calc PR A -1 C125 C -0.4267(16) -0.0219(11) 1.0162(7) 0.111(10) Uiso 0.50 1 d PD A -1 H125 H -0.3692 -0.0312 1.0290 0.133 Uiso 0.50 1 calc PR A -1 C126 C -0.5050(13) -0.0533(9) 1.0234(6) 0.065(7) Uiso 0.50 1 d PD A -1 H126 H -0.5015 -0.0922 1.0374 0.077 Uiso 0.50 1 calc PR A -1 C127 C -0.5886(14) -0.0287(10) 1.0103(7) 0.082(9) Uiso 0.50 1 d PD A -1 H127 H -0.6406 -0.0481 1.0191 0.099 Uiso 0.50 1 calc PR A -1 C128 C -0.6003(9) 0.0226(7) 0.9851(4) 0.088(10) Uiso 0.50 1 d PD A -1 H128 H -0.6575 0.0411 0.9784 0.106 Uiso 0.50 1 calc PR A -1 C129 C 1.0743(9) 0.4525(7) 0.5345(4) 0.186(15) Uiso 0.50 1 d PRDU A -1 H12G H 1.1370 0.4667 0.5366 0.279 Uiso 0.50 1 calc PR A -1 H12H H 1.0709 0.4088 0.5247 0.279 Uiso 0.50 1 calc PR A -1 H12I H 1.0512 0.4541 0.5603 0.279 Uiso 0.50 1 calc PR A -1 C135 C 1.0358(9) 0.5464(7) 0.5105(4) 0.092(7) Uiso 0.50 1 d PRDU A -1 H135 H 1.0823 0.5637 0.5279 0.111 Uiso 0.50 1 calc PR A -1 C130 C 1.0263(9) 0.4893(7) 0.5106(4) 0.167(9) Uiso 0.50 1 d PRDU A -1 C131 C 0.970(2) 0.4560(7) 0.4804(8) 0.243(14) Uiso 0.50 1 d PDU A -1 H131 H 0.9693 0.4110 0.4786 0.292 Uiso 0.50 1 calc PR A -1 C132 C 0.9163(14) 0.4953(8) 0.4536(5) 0.170(10) Uiso 0.50 1 d PDU A -1 H132 H 0.8770 0.4763 0.4338 0.204 Uiso 0.50 1 calc PR A -1 C133 C 0.9213(11) 0.5622(8) 0.4565(5) 0.102(8) Uiso 0.50 1 d PDU A -1 H133 H 0.8844 0.5880 0.4390 0.122 Uiso 0.50 1 calc PR A -1 C134 C 0.9823(13) 0.5907(7) 0.4858(5) 0.151(8) Uiso 0.50 1 d PDU A -1 H134 H 0.9874 0.6354 0.4890 0.181 Uiso 0.50 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0346(14) 0.0495(18) 0.0313(13) -0.0059(12) 0.0056(11) 0.0014(12) Mg2 0.0354(14) 0.0399(16) 0.0369(14) -0.0012(12) 0.0043(11) 0.0007(12) Mg3 0.0331(13) 0.0452(17) 0.0375(14) -0.0045(12) 0.0050(11) -0.0008(12) Mg4 0.0358(14) 0.0392(16) 0.0410(14) -0.0008(12) 0.0015(11) -0.0009(12) N1 0.033(3) 0.040(4) 0.033(3) -0.005(3) 0.004(3) -0.003(3) N2 0.028(3) 0.047(4) 0.033(3) -0.002(3) 0.004(3) -0.004(3) N3 0.028(3) 0.034(4) 0.030(3) -0.003(3) 0.005(3) 0.002(3) N4 0.036(4) 0.037(4) 0.044(4) 0.002(3) 0.006(3) 0.004(3) N5 0.031(3) 0.045(4) 0.036(4) -0.007(3) 0.009(3) -0.009(3) N6 0.030(3) 0.042(4) 0.034(3) -0.001(3) 0.011(3) -0.002(3) N7 0.034(4) 0.042(4) 0.034(3) -0.001(3) 0.010(3) 0.003(3) N8 0.033(4) 0.038(4) 0.040(4) -0.002(3) -0.002(3) 0.001(3) C1 0.029(4) 0.058(6) 0.054(5) -0.015(4) 0.003(4) -0.007(4) C2 0.032(4) 0.045(5) 0.039(5) 0.004(4) 0.007(4) 0.000(4) C3 0.031(4) 0.043(5) 0.033(4) -0.009(4) 0.002(3) -0.004(4) C4 0.037(5) 0.037(5) 0.037(4) -0.006(4) 0.011(4) -0.001(4) C5 0.046(5) 0.052(6) 0.045(5) -0.010(4) 0.012(4) 0.000(4) C6 0.034(4) 0.046(6) 0.036(5) -0.014(4) 0.008(3) -0.008(4) C7 0.035(4) 0.053(6) 0.042(5) -0.011(4) 0.007(4) 0.007(4) C8 0.044(5) 0.049(6) 0.047(5) -0.005(4) 0.002(4) 0.009(4) C9 0.037(5) 0.070(7) 0.036(5) -0.019(5) 0.000(4) 0.000(4) C10 0.038(5) 0.071(7) 0.034(5) -0.005(5) 0.010(4) -0.002(5) C11 0.043(5) 0.051(6) 0.041(5) -0.008(4) 0.023(4) -0.011(4) C12 0.050(5) 0.057(6) 0.034(4) -0.001(4) 0.006(4) 0.014(4) C13 0.060(5) 0.086(7) 0.051(5) -0.032(5) 0.006(4) 0.002(5) C14 0.079(6) 0.062(7) 0.043(5) 0.004(4) 0.030(4) -0.021(5) C15 0.039(4) 0.049(6) 0.029(4) -0.003(4) 0.011(4) 0.000(4) C16 0.038(5) 0.049(6) 0.030(4) -0.008(4) 0.009(4) -0.001(4) C17 0.041(5) 0.037(5) 0.053(5) -0.009(4) 0.006(4) 0.009(4) C18 0.045(5) 0.056(6) 0.037(5) -0.015(4) 0.016(4) -0.004(4) C19 0.041(5) 0.049(6) 0.036(4) -0.009(4) 0.013(4) -0.007(4) C20 0.044(5) 0.043(5) 0.023(4) -0.009(4) 0.007(3) -0.001(4) C21 0.061(5) 0.058(6) 0.049(5) -0.001(4) 0.017(4) 0.006(5) C22 0.056(5) 0.081(7) 0.062(5) 0.001(5) 0.031(4) 0.007(5) C23 0.051(5) 0.048(5) 0.037(4) -0.007(4) 0.007(4) 0.000(4) C24 0.042(4) 0.043(5) 0.036(4) -0.004(4) 0.004(3) -0.001(4) C25 0.037(5) 0.040(5) 0.035(4) -0.002(4) 0.020(4) -0.008(4) C26 0.034(4) 0.041(5) 0.032(4) -0.002(4) 0.002(3) 0.003(4) C27 0.028(4) 0.057(6) 0.033(4) 0.002(4) 0.005(4) -0.003(4) C28 0.041(5) 0.059(6) 0.049(5) 0.005(4) 0.003(4) -0.004(4) C29 0.035(4) 0.040(5) 0.029(4) -0.010(4) -0.001(4) 0.002(4) C30 0.039(4) 0.044(5) 0.021(4) -0.001(4) 0.009(3) 0.003(4) C31 0.039(4) 0.036(5) 0.040(4) 0.007(4) 0.009(4) 0.002(4) C32 0.036(4) 0.047(5) 0.034(4) -0.009(4) 0.006(4) 0.005(4) C33 0.030(4) 0.057(6) 0.021(4) -0.006(4) 0.006(3) 0.000(4) C34 0.032(4) 0.040(5) 0.026(4) 0.000(4) 0.001(3) -0.008(4) C35 0.040(4) 0.057(6) 0.036(4) 0.007(4) 0.009(4) 0.003(4) C36 0.050(5) 0.058(6) 0.047(5) 0.008(4) 0.012(4) 0.007(4) C37 0.047(5) 0.063(6) 0.033(4) 0.000(4) 0.015(4) 0.005(4) C38 0.033(4) 0.037(5) 0.033(4) 0.001(4) -0.003(3) 0.001(4) C39 0.033(4) 0.037(5) 0.045(5) -0.006(4) 0.005(4) -0.002(4) C40 0.044(5) 0.037(5) 0.067(6) -0.001(4) 0.019(4) -0.003(4) C41 0.057(5) 0.029(5) 0.076(6) -0.003(5) 0.005(5) 0.002(4) C42 0.050(5) 0.050(6) 0.049(5) 0.018(5) 0.007(4) 0.005(4) C43 0.040(5) 0.047(6) 0.037(5) 0.002(4) -0.001(4) 0.002(4) C44 0.037(4) 0.046(5) 0.064(5) -0.010(4) 0.013(4) 0.002(4) C45 0.083(7) 0.045(6) 0.105(7) -0.007(5) 0.023(5) 0.003(5) C46 0.040(5) 0.072(6) 0.036(4) 0.005(4) 0.003(4) -0.003(4) C47 0.038(4) 0.045(6) 0.036(4) -0.007(4) 0.010(4) 0.003(4) C48 0.043(5) 0.057(6) 0.038(5) -0.007(4) 0.005(4) 0.004(4) C49 0.048(5) 0.055(6) 0.039(5) 0.009(4) -0.008(4) 0.000(4) C50 0.034(4) 0.045(5) 0.027(4) -0.008(4) -0.006(3) 0.003(4) C51 0.036(4) 0.045(5) 0.028(4) -0.011(4) -0.003(3) -0.001(4) C52 0.031(4) 0.047(5) 0.040(4) 0.001(4) 0.000(4) 0.006(4) C53 0.037(4) 0.046(5) 0.037(5) -0.003(4) -0.007(4) -0.007(4) C54 0.050(5) 0.055(6) 0.039(5) -0.003(4) 0.002(4) -0.018(4) C55 0.069(6) 0.062(7) 0.048(5) 0.002(5) 0.000(5) -0.017(5) C56 0.074(6) 0.048(6) 0.054(6) 0.014(5) -0.017(5) -0.004(5) C57 0.051(5) 0.048(6) 0.061(6) -0.008(5) -0.013(5) 0.002(4) C58 0.034(4) 0.043(5) 0.046(5) -0.005(4) -0.006(4) -0.002(4) C59 0.042(5) 0.043(5) 0.041(5) -0.021(4) 0.006(4) -0.002(4) C60 0.025(4) 0.043(5) 0.034(4) -0.008(4) -0.002(3) 0.007(4) C61 0.040(5) 0.060(6) 0.046(5) -0.015(4) 0.002(4) -0.007(4) C62 0.036(5) 0.040(5) 0.042(5) 0.000(4) 0.004(4) -0.004(4) C63 0.035(4) 0.051(5) 0.031(4) -0.002(4) 0.001(3) -0.006(4) C64 0.036(5) 0.050(5) 0.028(4) -0.003(4) 0.001(4) -0.009(4) C65 0.045(5) 0.048(5) 0.034(4) -0.006(4) 0.000(4) -0.002(4) C66 0.026(4) 0.051(6) 0.038(5) -0.002(4) 0.002(3) 0.000(4) C67 0.023(4) 0.045(5) 0.037(4) 0.000(4) 0.004(3) 0.004(4) C68 0.035(4) 0.046(5) 0.038(5) -0.004(4) 0.004(4) 0.008(4) C69 0.034(4) 0.055(6) 0.025(4) -0.010(4) 0.005(3) 0.004(4) C70 0.048(5) 0.066(7) 0.027(4) -0.009(4) 0.006(4) -0.002(4) C71 0.042(5) 0.057(6) 0.030(4) -0.002(4) 0.012(4) -0.002(4) C72 0.048(5) 0.057(6) 0.022(4) 0.004(4) 0.005(3) 0.006(4) C73 0.062(5) 0.079(7) 0.036(4) -0.012(4) 0.011(4) 0.003(5) C74 0.069(6) 0.050(6) 0.060(5) 0.006(5) 0.028(4) -0.001(5) C75 0.037(4) 0.052(6) 0.024(4) -0.008(4) 0.000(3) 0.004(4) C76 0.048(5) 0.046(6) 0.038(5) 0.004(4) 0.004(4) 0.003(4) C77 0.036(5) 0.058(6) 0.047(5) -0.015(4) -0.004(4) 0.013(4) C78 0.040(5) 0.066(6) 0.039(5) -0.006(4) 0.010(4) -0.003(5) C79 0.043(5) 0.056(6) 0.028(4) -0.005(4) 0.015(4) -0.005(4) C80 0.040(4) 0.049(6) 0.024(4) -0.006(4) 0.009(3) -0.002(4) C81 0.064(5) 0.055(6) 0.051(5) -0.004(4) 0.011(4) 0.014(5) C82 0.049(5) 0.123(9) 0.062(6) -0.001(5) 0.026(4) 0.019(5) C83 0.044(5) 0.059(6) 0.031(4) 0.002(4) 0.005(4) -0.003(4) C84 0.038(4) 0.051(6) 0.045(5) -0.006(4) 0.005(4) -0.001(4) C85 0.028(4) 0.039(5) 0.033(4) 0.000(4) 0.006(4) 0.003(4) C86 0.020(4) 0.044(5) 0.028(4) -0.005(4) -0.001(3) -0.003(4) C87 0.030(4) 0.043(5) 0.036(4) -0.001(4) 0.012(4) 0.004(4) C88 0.039(5) 0.053(5) 0.045(5) -0.002(4) 0.000(4) -0.004(4) C89 0.025(4) 0.045(5) 0.030(4) -0.005(4) 0.003(3) -0.004(4) C90 0.025(4) 0.044(5) 0.032(4) 0.001(4) 0.006(3) -0.001(4) C91 0.036(4) 0.056(6) 0.031(4) 0.004(4) 0.013(3) 0.004(4) C92 0.031(4) 0.035(5) 0.042(5) -0.004(4) -0.004(4) -0.005(4) C93 0.045(5) 0.047(6) 0.027(4) 0.002(4) 0.009(4) -0.001(4) C94 0.034(4) 0.037(5) 0.027(4) -0.004(4) 0.006(3) -0.002(4) C95 0.044(4) 0.041(5) 0.033(4) 0.004(4) 0.009(3) 0.002(4) C96 0.054(5) 0.053(6) 0.048(5) 0.005(4) 0.009(4) 0.008(4) C97 0.045(4) 0.041(5) 0.045(4) -0.007(4) 0.016(4) 0.001(4) C98 0.026(4) 0.034(5) 0.038(4) 0.002(4) -0.001(3) 0.002(3) C99 0.024(4) 0.041(5) 0.039(4) 0.005(4) -0.006(3) 0.000(4) C100 0.040(5) 0.046(6) 0.049(5) 0.011(4) 0.005(4) -0.008(4) C101 0.035(4) 0.038(5) 0.057(5) 0.004(5) 0.001(4) 0.004(4) C102 0.045(5) 0.038(5) 0.051(5) -0.003(4) 0.013(4) 0.002(4) C103 0.028(4) 0.052(6) 0.037(5) 0.000(4) 0.001(3) -0.004(4) C104 0.040(4) 0.056(6) 0.044(5) 0.000(4) 0.009(4) -0.003(4) C105 0.072(6) 0.050(6) 0.072(6) -0.005(5) 0.023(5) 0.007(5) C106 0.046(5) 0.049(5) 0.051(5) -0.002(4) 0.015(4) 0.003(4) C107 0.029(4) 0.076(7) 0.038(5) -0.011(5) 0.001(4) -0.001(4) C108 0.045(5) 0.069(7) 0.040(5) -0.006(5) 0.005(4) -0.007(5) C109 0.045(5) 0.041(5) 0.044(5) 0.008(4) -0.008(4) -0.001(4) C110 0.037(4) 0.040(5) 0.035(4) -0.010(4) -0.001(4) 0.001(4) C112 0.029(4) 0.043(5) 0.034(4) -0.006(4) -0.004(3) 0.003(4) C113 0.028(4) 0.051(6) 0.039(4) -0.005(4) 0.006(3) -0.004(4) C114 0.051(5) 0.060(6) 0.032(5) 0.002(5) -0.013(4) -0.015(5) C115 0.079(7) 0.079(8) 0.039(5) 0.001(5) -0.004(5) -0.034(6) C116 0.087(9) 0.104(11) 0.076(8) 0.037(8) -0.037(7) -0.051(7) C117 0.087(9) 0.076(9) 0.105(10) 0.027(8) -0.056(7) -0.026(7) C118 0.071(6) 0.054(7) 0.090(8) 0.010(6) -0.028(6) -0.010(5) C119 0.039(5) 0.040(6) 0.068(6) -0.003(5) -0.007(4) -0.017(4) C120 0.039(4) 0.030(5) 0.058(5) -0.016(4) 0.000(4) -0.005(4) C121 0.030(4) 0.036(5) 0.036(4) -0.008(4) -0.003(3) 0.003(4) _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 N2 2.017(5) . ? Mg1 N1 2.019(5) . ? Mg1 C48 2.382(7) . ? Mg1 C49 2.394(7) . ? Mg1 C47 2.422(7) . ? Mg1 C50 2.426(6) . ? Mg1 C51 2.675(7) . ? Mg1 C60 2.677(7) . ? Mg2 N3 2.019(6) . ? Mg2 N4 2.044(6) . ? Mg2 C52 2.344(7) . ? Mg2 C59 2.372(7) . ? Mg2 C53 2.604(7) . ? Mg2 C58 2.650(7) . ? Mg2 C51 2.663(7) . ? Mg2 C60 2.677(7) . ? Mg3 N5 2.021(5) . ? Mg3 N6 2.030(5) . ? Mg3 C109 2.378(7) . ? Mg3 C110 2.399(7) . ? Mg3 C108 2.420(7) . ? Mg3 C107 2.462(7) . ? Mg3 C112 2.643(7) . ? Mg3 C121 2.679(7) . ? Mg4 N7 2.038(6) . ? Mg4 N8 2.042(6) . ? Mg4 C113 2.352(7) . ? Mg4 C120 2.367(7) . ? Mg4 C114 2.559(7) . ? Mg4 C119 2.602(8) . ? Mg4 C112 2.740(7) . ? Mg4 C121 2.751(7) . ? N1 C2 1.329(8) . ? N1 C6 1.444(8) . ? N2 C4 1.325(7) . ? N2 C15 1.444(7) . ? N3 C25 1.336(8) . ? N3 C29 1.440(8) . ? N4 C27 1.333(8) . ? N4 C38 1.443(8) . ? N5 C62 1.325(8) . ? N5 C66 1.448(8) . ? N6 C64 1.319(7) . ? N6 C75 1.455(7) . ? N7 C85 1.327(7) . ? N7 C89 1.438(8) . ? N8 C87 1.340(8) . ? N8 C98 1.440(8) . ? C1 C2 1.513(8) . ? C2 C3 1.411(8) . ? C3 C4 1.396(8) . ? C4 C5 1.517(8) . ? C6 C11 1.390(9) . ? C6 C7 1.405(9) . ? C7 C8 1.382(9) . ? C7 C12 1.506(9) . ? C8 C9 1.384(9) . ? C9 C10 1.385(10) . ? C9 C13 1.527(9) . ? C10 C11 1.391(9) . ? C11 C14 1.502(9) . ? C15 C16 1.406(9) . ? C15 C20 1.410(9) . ? C16 C17 1.392(8) . ? C16 C21 1.513(9) . ? C17 C18 1.397(9) . ? C18 C19 1.386(9) . ? C18 C22 1.515(9) . ? C19 C20 1.389(8) . ? C20 C23 1.486(9) . ? C24 C25 1.522(8) . ? C25 C26 1.402(9) . ? C26 C27 1.391(9) . ? C27 C28 1.510(9) . ? C29 C30 1.386(8) . ? C29 C34 1.408(8) . ? C30 C31 1.396(8) . ? C30 C35 1.521(8) . ? C31 C32 1.374(8) . ? C32 C33 1.403(8) . ? C32 C36 1.514(8) . ? C33 C34 1.385(8) . ? C34 C37 1.518(8) . ? C38 C43 1.394(9) . ? C38 C39 1.408(8) . ? C39 C40 1.375(9) . ? C39 C44 1.498(9) . ? C40 C41 1.403(9) . ? C41 C42 1.397(9) . ? C41 C45 1.499(10) . ? C42 C43 1.375(9) . ? C43 C46 1.518(9) . ? C47 C48 1.388(9) . ? C47 C60 1.424(8) . ? C48 C49 1.392(9) . ? C49 C50 1.428(8) . ? C50 C51 1.417(9) . ? C51 C52 1.430(8) . ? C51 C60 1.440(8) . ? C52 C53 1.457(9) . ? C53 C54 1.396(8) . ? C53 C58 1.417(9) . ? C54 C55 1.379(10) . ? C55 C56 1.359(10) . ? C56 C57 1.414(9) . ? C57 C58 1.391(9) . ? C58 C59 1.487(9) . ? C59 C60 1.394(9) . ? C61 C62 1.520(8) . ? C62 C63 1.404(8) . ? C63 C64 1.397(8) . ? C64 C65 1.516(8) . ? C66 C67 1.398(9) . ? C66 C71 1.404(9) . ? C67 C68 1.390(8) . ? C67 C72 1.502(8) . ? C68 C69 1.384(8) . ? C69 C70 1.384(9) . ? C69 C73 1.512(8) . ? C70 C71 1.389(9) . ? C71 C74 1.504(9) . ? C75 C76 1.389(9) . ? C75 C80 1.391(9) . ? C76 C77 1.403(9) . ? C76 C81 1.513(9) . ? C77 C78 1.383(9) . ? C78 C79 1.391(9) . ? C78 C82 1.506(9) . ? C79 C80 1.413(8) . ? C80 C83 1.499(9) . ? C84 C85 1.531(8) . ? C85 C86 1.366(8) . ? C86 C87 1.398(9) . ? C87 C88 1.515(8) . ? C89 C90 1.397(8) . ? C89 C94 1.407(8) . ? C90 C91 1.384(9) . ? C90 C95 1.499(8) . ? C91 C92 1.395(8) . ? C92 C93 1.391(8) . ? C92 C96 1.509(9) . ? C93 C94 1.378(8) . ? C94 C97 1.510(8) . ? C98 C99 1.378(8) . ? C98 C103 1.415(8) . ? C99 C100 1.397(9) . ? C99 C104 1.503(8) . ? C100 C101 1.384(9) . ? C101 C102 1.364(9) . ? C101 C105 1.533(9) . ? C102 C103 1.396(9) . ? C103 C106 1.498(9) . ? C107 C108 1.407(10) . ? C107 C121 1.420(9) . ? C108 C109 1.374(9) . ? C109 C110 1.415(8) . ? C110 C112 1.399(9) . ? C112 C113 1.420(8) . ? C112 C121 1.463(8) . ? C113 C114 1.450(9) . ? C114 C115 1.411(10) . ? C114 C119 1.421(10) . ? C115 C116 1.379(12) . ? C116 C117 1.371(13) . ? C117 C118 1.385(12) . ? C118 C119 1.373(10) . ? C119 C120 1.472(9) . ? C120 C121 1.413(9) . ? C122 C123 1.505(7) . ? C123 C124 1.373(10) . ? C123 C128 1.376(10) . ? C124 C125 1.383(10) . ? C125 C126 1.384(11) . ? C126 C127 1.390(10) . ? C127 C128 1.387(10) . ? C129 C130 1.3007 . ? C135 C130 1.2124 . ? C135 C134 1.452(6) . ? C130 C131 1.458(6) . ? C131 C132 1.433(6) . ? C132 C133 1.415(6) . ? C133 C134 1.432(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 N2 Mg1 N1 93.4(2) . . ? N2 Mg1 C48 151.7(3) . . ? N1 Mg1 C48 104.5(2) . . ? N2 Mg1 C49 118.6(3) . . ? N1 Mg1 C49 130.8(2) . . ? C48 Mg1 C49 33.9(2) . . ? N2 Mg1 C47 162.0(2) . . ? N1 Mg1 C47 100.1(2) . . ? C48 Mg1 C47 33.6(2) . . ? C49 Mg1 C47 59.9(3) . . ? N2 Mg1 C50 99.4(2) . . ? N1 Mg1 C50 164.7(2) . . ? C48 Mg1 C50 60.5(2) . . ? C49 Mg1 C50 34.5(2) . . ? C47 Mg1 C50 69.4(2) . . ? N2 Mg1 C51 106.2(2) . . ? N1 Mg1 C51 149.7(3) . . ? C48 Mg1 C51 68.1(2) . . ? C49 Mg1 C51 58.4(2) . . ? C47 Mg1 C51 56.8(2) . . ? C50 Mg1 C51 31.8(2) . . ? N2 Mg1 C60 130.2(2) . . ? N1 Mg1 C60 119.2(2) . . ? C48 Mg1 C60 58.3(2) . . ? C49 Mg1 C60 68.7(2) . . ? C47 Mg1 C60 31.94(19) . . ? C50 Mg1 C60 57.4(2) . . ? C51 Mg1 C60 31.21(18) . . ? N3 Mg2 N4 92.1(2) . . ? N3 Mg2 C52 155.7(2) . . ? N4 Mg2 C52 102.8(3) . . ? N3 Mg2 C59 103.8(2) . . ? N4 Mg2 C59 152.3(3) . . ? C52 Mg2 C59 71.1(2) . . ? N3 Mg2 C53 122.8(2) . . ? N4 Mg2 C53 129.1(2) . . ? C52 Mg2 C53 33.7(2) . . ? C59 Mg2 C53 59.2(2) . . ? N3 Mg2 C58 103.7(2) . . ? N4 Mg2 C58 160.2(3) . . ? C52 Mg2 C58 58.4(2) . . ? C59 Mg2 C58 33.9(2) . . ? C53 Mg2 C58 31.3(2) . . ? N3 Mg2 C51 159.6(2) . . ? N4 Mg2 C51 102.8(2) . . ? C52 Mg2 C51 32.41(19) . . ? C59 Mg2 C51 57.2(2) . . ? C53 Mg2 C51 56.6(2) . . ? C58 Mg2 C51 65.3(2) . . ? N3 Mg2 C60 128.4(2) . . ? N4 Mg2 C60 122.2(2) . . ? C52 Mg2 C60 58.0(2) . . ? C59 Mg2 C60 31.3(2) . . ? C53 Mg2 C60 66.1(2) . . ? C58 Mg2 C60 55.7(2) . . ? C51 Mg2 C60 31.29(19) . . ? N5 Mg3 N6 93.4(2) . . ? N5 Mg3 C109 133.1(2) . . ? N6 Mg3 C109 118.5(3) . . ? N5 Mg3 C110 166.1(2) . . ? N6 Mg3 C110 99.5(2) . . ? C109 Mg3 C110 34.4(2) . . ? N5 Mg3 C108 105.9(2) . . ? N6 Mg3 C108 150.7(3) . . ? C109 Mg3 C108 33.3(2) . . ? C110 Mg3 C108 60.2(2) . . ? N5 Mg3 C107 99.3(2) . . ? N6 Mg3 C107 162.9(2) . . ? C109 Mg3 C107 59.2(3) . . ? C110 Mg3 C107 69.2(2) . . ? C108 Mg3 C107 33.5(2) . . ? N5 Mg3 C112 147.1(2) . . ? N6 Mg3 C112 106.2(2) . . ? C109 Mg3 C112 58.5(2) . . ? C110 Mg3 C112 31.8(2) . . ? C108 Mg3 C112 68.6(2) . . ? C107 Mg3 C112 57.4(2) . . ? N5 Mg3 C121 116.6(2) . . ? N6 Mg3 C121 131.4(2) . . ? C109 Mg3 C121 68.1(2) . . ? C110 Mg3 C121 57.4(2) . . ? C108 Mg3 C121 58.1(2) . . ? C107 Mg3 C121 31.7(2) . . ? C112 Mg3 C121 31.89(18) . . ? N7 Mg4 N8 92.4(2) . . ? N7 Mg4 C113 153.0(3) . . ? N8 Mg4 C113 100.9(3) . . ? N7 Mg4 C120 107.3(2) . . ? N8 Mg4 C120 151.4(3) . . ? C113 Mg4 C120 70.7(2) . . ? N7 Mg4 C114 120.8(3) . . ? N8 Mg4 C114 127.2(3) . . ? C113 Mg4 C114 34.0(2) . . ? C120 Mg4 C114 59.5(2) . . ? N7 Mg4 C119 103.5(3) . . ? N8 Mg4 C119 158.9(3) . . ? C113 Mg4 C119 59.1(2) . . ? C120 Mg4 C119 34.1(2) . . ? C114 Mg4 C119 31.9(2) . . ? N7 Mg4 C112 163.8(2) . . ? N8 Mg4 C112 101.5(2) . . ? C113 Mg4 C112 31.22(19) . . ? C120 Mg4 C112 56.8(2) . . ? C114 Mg4 C112 56.0(2) . . ? C119 Mg4 C112 65.4(2) . . ? N7 Mg4 C121 133.3(2) . . ? N8 Mg4 C121 121.5(2) . . ? C113 Mg4 C121 56.7(2) . . ? C120 Mg4 C121 30.9(2) . . ? C114 Mg4 C121 65.4(2) . . ? C119 Mg4 C121 55.4(2) . . ? C112 Mg4 C121 30.89(18) . . ? C2 N1 C6 118.8(5) . . ? C2 N1 Mg1 124.6(4) . . ? C6 N1 Mg1 116.4(4) . . ? C4 N2 C15 120.1(5) . . ? C4 N2 Mg1 124.2(4) . . ? C15 N2 Mg1 115.2(4) . . ? C25 N3 C29 118.7(6) . . ? C25 N3 Mg2 124.8(5) . . ? C29 N3 Mg2 116.3(4) . . ? C27 N4 C38 118.8(6) . . ? C27 N4 Mg2 125.2(5) . . ? C38 N4 Mg2 115.7(4) . . ? C62 N5 C66 118.9(5) . . ? C62 N5 Mg3 123.9(5) . . ? C66 N5 Mg3 117.0(4) . . ? C64 N6 C75 119.6(5) . . ? C64 N6 Mg3 124.1(4) . . ? C75 N6 Mg3 115.8(4) . . ? C85 N7 C89 119.0(6) . . ? C85 N7 Mg4 123.7(5) . . ? C89 N7 Mg4 117.0(4) . . ? C87 N8 C98 119.4(6) . . ? C87 N8 Mg4 124.0(5) . . ? C98 N8 Mg4 116.5(4) . . ? N1 C2 C3 123.9(6) . . ? N1 C2 C1 119.8(6) . . ? C3 C2 C1 116.3(6) . . ? C4 C3 C2 128.6(6) . . ? N2 C4 C3 125.0(6) . . ? N2 C4 C5 118.7(6) . . ? C3 C4 C5 116.3(6) . . ? C11 C6 C7 120.2(7) . . ? C11 C6 N1 120.1(7) . . ? C7 C6 N1 119.4(6) . . ? C8 C7 C6 118.7(7) . . ? C8 C7 C12 121.2(7) . . ? C6 C7 C12 120.1(6) . . ? C7 C8 C9 122.2(7) . . ? C8 C9 C10 117.8(7) . . ? C8 C9 C13 121.0(8) . . ? C10 C9 C13 121.2(7) . . ? C9 C10 C11 122.1(7) . . ? C6 C11 C10 118.8(7) . . ? C6 C11 C14 120.8(6) . . ? C10 C11 C14 120.4(7) . . ? C16 C15 C20 121.4(6) . . ? C16 C15 N2 119.6(6) . . ? C20 C15 N2 118.7(6) . . ? C17 C16 C15 118.3(7) . . ? C17 C16 C21 120.1(7) . . ? C15 C16 C21 121.6(6) . . ? C16 C17 C18 121.9(7) . . ? C19 C18 C17 117.8(6) . . ? C19 C18 C22 121.4(7) . . ? C17 C18 C22 120.7(7) . . ? C18 C19 C20 123.3(7) . . ? C19 C20 C15 117.2(7) . . ? C19 C20 C23 121.9(7) . . ? C15 C20 C23 120.7(6) . . ? N3 C25 C26 125.0(7) . . ? N3 C25 C24 118.1(6) . . ? C26 C25 C24 116.9(7) . . ? C27 C26 C25 128.5(7) . . ? N4 C27 C26 124.1(7) . . ? N4 C27 C28 118.8(7) . . ? C26 C27 C28 117.0(7) . . ? C30 C29 C34 120.6(6) . . ? C30 C29 N3 119.6(6) . . ? C34 C29 N3 119.6(6) . . ? C29 C30 C31 118.9(6) . . ? C29 C30 C35 120.3(6) . . ? C31 C30 C35 120.8(6) . . ? C32 C31 C30 122.1(6) . . ? C31 C32 C33 118.1(7) . . ? C31 C32 C36 120.9(6) . . ? C33 C32 C36 121.0(6) . . ? C34 C33 C32 121.7(6) . . ? C33 C34 C29 118.6(6) . . ? C33 C34 C37 120.4(6) . . ? C29 C34 C37 121.0(6) . . ? C43 C38 C39 119.7(7) . . ? C43 C38 N4 119.9(6) . . ? C39 C38 N4 120.2(6) . . ? C40 C39 C38 118.6(7) . . ? C40 C39 C44 119.8(6) . . ? C38 C39 C44 121.6(7) . . ? C39 C40 C41 122.7(7) . . ? C42 C41 C40 117.2(7) . . ? C42 C41 C45 121.6(8) . . ? C40 C41 C45 121.2(7) . . ? C43 C42 C41 121.4(7) . . ? C42 C43 C38 120.3(7) . . ? C42 C43 C46 119.7(7) . . ? C38 C43 C46 119.9(7) . . ? C48 C47 C60 123.5(7) . . ? C48 C47 Mg1 71.6(4) . . ? C60 C47 Mg1 84.0(4) . . ? C47 C48 C49 119.7(7) . . ? C47 C48 Mg1 74.8(4) . . ? C49 C48 Mg1 73.5(4) . . ? C48 C49 C50 118.4(7) . . ? C48 C49 Mg1 72.6(4) . . ? C50 C49 Mg1 74.0(4) . . ? C51 C50 C49 121.7(7) . . ? C51 C50 Mg1 83.8(4) . . ? C49 C50 Mg1 71.6(4) . . ? C50 C51 C52 123.9(6) . . ? C50 C51 C60 118.8(6) . . ? C52 C51 C60 117.3(7) . . ? C50 C51 Mg2 133.7(5) . . ? C52 C51 Mg2 61.4(4) . . ? C60 C51 Mg2 74.9(4) . . ? C50 C51 Mg1 64.4(4) . . ? C52 C51 Mg1 135.7(4) . . ? C60 C51 Mg1 74.5(4) . . ? Mg2 C51 Mg1 149.4(3) . . ? C51 C52 C53 119.8(6) . . ? C51 C52 Mg2 86.1(4) . . ? C53 C52 Mg2 83.0(4) . . ? C54 C53 C58 119.1(7) . . ? C54 C53 C52 123.9(7) . . ? C58 C53 C52 117.0(6) . . ? C54 C53 Mg2 130.6(5) . . ? C58 C53 Mg2 76.1(4) . . ? C52 C53 Mg2 63.3(3) . . ? C55 C54 C53 120.0(8) . . ? C56 C55 C54 121.7(8) . . ? C55 C56 C57 119.7(8) . . ? C58 C57 C56 119.6(7) . . ? C57 C58 C53 119.7(7) . . ? C57 C58 C59 123.8(7) . . ? C53 C58 C59 116.4(7) . . ? C57 C58 Mg2 134.0(5) . . ? C53 C58 Mg2 72.6(4) . . ? C59 C58 Mg2 62.8(3) . . ? C60 C59 C58 119.5(6) . . ? C60 C59 Mg2 86.5(4) . . ? C58 C59 Mg2 83.4(4) . . ? C59 C60 C47 125.8(6) . . ? C59 C60 C51 117.5(6) . . ? C47 C60 C51 116.5(7) . . ? C59 C60 Mg2 62.2(4) . . ? C47 C60 Mg2 133.2(4) . . ? C51 C60 Mg2 73.8(4) . . ? C59 C60 Mg1 135.9(5) . . ? C47 C60 Mg1 64.1(4) . . ? C51 C60 Mg1 74.3(4) . . ? Mg2 C60 Mg1 148.1(3) . . ? N5 C62 C63 124.4(6) . . ? N5 C62 C61 119.2(6) . . ? C63 C62 C61 116.3(6) . . ? C64 C63 C62 129.3(6) . . ? N6 C64 C63 124.2(6) . . ? N6 C64 C65 119.3(6) . . ? C63 C64 C65 116.4(6) . . ? C67 C66 C71 120.7(7) . . ? C67 C66 N5 118.9(6) . . ? C71 C66 N5 120.2(7) . . ? C68 C67 C66 118.0(6) . . ? C68 C67 C72 121.4(7) . . ? C66 C67 C72 120.6(6) . . ? C69 C68 C67 122.8(7) . . ? C68 C69 C70 117.7(6) . . ? C68 C69 C73 121.9(7) . . ? C70 C69 C73 120.4(6) . . ? C69 C70 C71 122.2(7) . . ? C70 C71 C66 118.5(7) . . ? C70 C71 C74 121.0(6) . . ? C66 C71 C74 120.5(7) . . ? C76 C75 C80 121.6(6) . . ? C76 C75 N6 119.9(7) . . ? C80 C75 N6 118.3(6) . . ? C75 C76 C77 118.0(7) . . ? C75 C76 C81 120.8(6) . . ? C77 C76 C81 121.2(7) . . ? C78 C77 C76 122.7(7) . . ? C77 C78 C79 117.6(6) . . ? C77 C78 C82 120.7(8) . . ? C79 C78 C82 121.6(7) . . ? C78 C79 C80 121.8(7) . . ? C75 C80 C79 118.2(7) . . ? C75 C80 C83 121.5(6) . . ? C79 C80 C83 120.3(7) . . ? N7 C85 C86 124.8(7) . . ? N7 C85 C84 117.7(6) . . ? C86 C85 C84 117.3(6) . . ? C85 C86 C87 130.2(7) . . ? N8 C87 C86 123.5(6) . . ? N8 C87 C88 118.8(6) . . ? C86 C87 C88 117.7(6) . . ? C90 C89 C94 119.8(6) . . ? C90 C89 N7 121.1(6) . . ? C94 C89 N7 118.9(6) . . ? C91 C90 C89 118.7(6) . . ? C91 C90 C95 120.0(6) . . ? C89 C90 C95 121.3(6) . . ? C90 C91 C92 122.3(6) . . ? C93 C92 C91 118.1(7) . . ? C93 C92 C96 121.2(6) . . ? C91 C92 C96 120.7(6) . . ? C94 C93 C92 121.1(6) . . ? C93 C94 C89 120.0(6) . . ? C93 C94 C97 119.6(6) . . ? C89 C94 C97 120.4(6) . . ? C99 C98 C103 121.1(7) . . ? C99 C98 N8 119.3(6) . . ? C103 C98 N8 119.4(6) . . ? C98 C99 C100 118.4(7) . . ? C98 C99 C104 121.7(7) . . ? C100 C99 C104 119.9(6) . . ? C101 C100 C99 122.4(7) . . ? C102 C101 C100 117.7(7) . . ? C102 C101 C105 121.7(7) . . ? C100 C101 C105 120.6(7) . . ? C101 C102 C103 123.3(7) . . ? C102 C103 C98 117.2(7) . . ? C102 C103 C106 121.3(6) . . ? C98 C103 C106 121.4(7) . . ? C108 C107 C121 123.1(7) . . ? C108 C107 Mg3 71.6(4) . . ? C121 C107 Mg3 82.6(4) . . ? C109 C108 C107 118.5(7) . . ? C109 C108 Mg3 71.7(4) . . ? C107 C108 Mg3 74.9(4) . . ? C108 C109 C110 120.3(7) . . ? C108 C109 Mg3 75.0(4) . . ? C110 C109 Mg3 73.6(4) . . ? C112 C110 C109 122.2(6) . . ? C112 C110 Mg3 83.8(4) . . ? C109 C110 Mg3 72.0(4) . . ? C110 C112 C113 125.9(7) . . ? C110 C112 C121 117.9(6) . . ? C113 C112 C121 116.1(7) . . ? C110 C112 Mg3 64.5(4) . . ? C113 C112 Mg3 134.2(4) . . ? C121 C112 Mg3 75.4(4) . . ? C110 C112 Mg4 135.4(4) . . ? C113 C112 Mg4 59.1(4) . . ? C121 C112 Mg4 75.0(4) . . ? Mg3 C112 Mg4 150.1(3) . . ? C112 C113 C114 120.6(6) . . ? C112 C113 Mg4 89.7(4) . . ? C114 C113 Mg4 80.9(4) . . ? C115 C114 C119 118.3(8) . . ? C115 C114 C113 124.3(8) . . ? C119 C114 C113 117.4(7) . . ? C115 C114 Mg4 128.1(5) . . ? C119 C114 Mg4 75.7(4) . . ? C113 C114 Mg4 65.1(4) . . ? C116 C115 C114 120.4(10) . . ? C117 C116 C115 119.8(11) . . ? C116 C117 C118 121.4(11) . . ? C119 C118 C117 119.8(10) . . ? C118 C119 C114 120.1(8) . . ? C118 C119 C120 124.0(8) . . ? C114 C119 C120 115.8(7) . . ? C118 C119 Mg4 131.8(5) . . ? C114 C119 Mg4 72.4(4) . . ? C120 C119 Mg4 64.2(4) . . ? C121 C120 C119 119.4(7) . . ? C121 C120 Mg4 89.8(4) . . ? C119 C120 Mg4 81.7(4) . . ? C120 C121 C107 126.0(7) . . ? C120 C121 C112 117.0(6) . . ? C107 C121 C112 116.9(7) . . ? C120 C121 Mg3 136.4(5) . . ? C107 C121 Mg3 65.7(4) . . ? C112 C121 Mg3 72.7(4) . . ? C120 C121 Mg4 59.3(4) . . ? C107 C121 Mg4 135.9(4) . . ? C112 C121 Mg4 74.1(4) . . ? Mg3 C121 Mg4 146.6(3) . . ? C124 C123 C128 117.5(17) . . ? C124 C123 C122 120.7(16) . . ? C128 C123 C122 118.0(16) . . ? C123 C124 C125 128(2) . . ? C124 C125 C126 112(2) . . ? C125 C126 C127 121(2) . . ? C128 C127 C126 123.5(18) . . ? C123 C128 C127 115.5(15) . . ? C130 C135 C134 125.6(6) . . ? C135 C130 C129 122.6 . . ? C135 C130 C131 122.4(6) . . ? C129 C130 C131 114.4(6) . . ? C132 C131 C130 115.8(6) . . ? C133 C132 C131 120.5(7) . . ? C132 C133 C134 119.6(6) . . ? C133 C134 C135 115.1(6) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.853 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.070