# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Chu-Chieh Lin' _publ_contact_author_email CCHLIN@MAIL.NCHU.EDU.TW _publ_section_title ; Preparation and Characterization of Bisphenolato magnesium Derivatives: An Efficient Catalyst for the Ring-Opening Polymerization of ??Caprolactone and L-Lactide ; loop_ _publ_author_name 'Chu-Chieh Lin.' 'Wen-Chou Hung.' 'Ya-Liu Peng.' 'Min-Yi Shen.' # Attachment '3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 737433' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H94 Mg O4, C4 H10 O' _chemical_formula_sum 'C66 H104 Mg1 O5' _chemical_formula_weight 1001.8 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' 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 26.224(4) _cell_length_b 14.652(2) _cell_length_c 18.448(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.519(3) _cell_angle_gamma 90.00 _cell_volume 6829.5(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2353 _cell_measurement_theta_min 2.617 _cell_measurement_theta_max 20.539 _exptl_crystal_description parallelpiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.974 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 0.067 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.932 _exptl_absorpt_correction_T_max 0.990 _exptl_absorpt_process_details 'SADABS, Sheldrick (1996)' _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 'Bruker SMART 1000 CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19352 _diffrn_reflns_av_R_equivalents 0.1032 _diffrn_reflns_av_sigmaI/netI 0.1216 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 26.13 _reflns_number_total 6754 _reflns_number_gt 2510 _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^)+(0.1110P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6754 _refine_ls_number_parameters 313 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.2000 _refine_ls_R_factor_gt 0.0786 _refine_ls_wR_factor_ref 0.2558 _refine_ls_wR_factor_gt 0.2071 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.026 _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 Mg Mg 0.5000 0.33696(11) 0.2500 0.0472(5) Uani 1 2 d S . . O1 O 0.50000(10) 0.41788(15) 0.15660(13) 0.0499(7) Uani 1 1 d . . . O2 O 0.56644(9) 0.28244(16) 0.26762(13) 0.0515(7) Uani 1 1 d . . . C1 C 0.54428(15) 0.4107(2) 0.12532(19) 0.0465(9) Uani 1 1 d . . . C2 C 0.57502(16) 0.4877(2) 0.1220(2) 0.0537(10) Uani 1 1 d . . . C3 C 0.61556(17) 0.4739(3) 0.0875(2) 0.0601(11) Uani 1 1 d . . . H3A H 0.6364 0.5240 0.0834 0.072 Uiso 1 1 calc R . . C4 C 0.62737(16) 0.3917(3) 0.0589(2) 0.0578(11) Uani 1 1 d . . . C5 C 0.59627(15) 0.3186(3) 0.0666(2) 0.0554(10) Uani 1 1 d . . . H5A H 0.6032 0.2621 0.0483 0.066 Uiso 1 1 calc R . . C6 C 0.55489(15) 0.3252(3) 0.10043(19) 0.0493(10) Uani 1 1 d . . . C7 C 0.52823(15) 0.2359(2) 0.11457(19) 0.0495(10) Uani 1 1 d . . . H7A H 0.5012 0.2513 0.1405 0.059 Uiso 1 1 calc R . . C8 C 0.57105(15) 0.1806(2) 0.1684(2) 0.0490(10) Uani 1 1 d . . . C9 C 0.59507(18) 0.1067(3) 0.1438(2) 0.0673(12) Uani 1 1 d . . . H9A H 0.5809 0.0855 0.0950 0.081 Uiso 1 1 calc R . . C10 C 0.63929(19) 0.0630(3) 0.1890(3) 0.0720(13) Uani 1 1 d D . . C11 C 0.65964(18) 0.1010(3) 0.2598(3) 0.0702(12) Uani 1 1 d . . . H11A H 0.6903 0.0751 0.2902 0.084 Uiso 1 1 calc R . . C12 C 0.63819(16) 0.1741(3) 0.2888(2) 0.0567(11) Uani 1 1 d . . . C13 C 0.59112(15) 0.2136(2) 0.2430(2) 0.0478(9) Uani 1 1 d . . . C14 C 0.56985(19) 0.5802(3) 0.1589(3) 0.0694(13) Uani 1 1 d . . . C15 C 0.5790(2) 0.5655(3) 0.2437(3) 0.0949(17) Uani 1 1 d . . . H15A H 0.6136 0.5401 0.2644 0.142 Uiso 1 1 calc R . . H15B H 0.5527 0.5244 0.2523 0.142 Uiso 1 1 calc R . . H15C H 0.5764 0.6229 0.2675 0.142 Uiso 1 1 calc R . . C16 C 0.5138(2) 0.6218(3) 0.1265(3) 0.0963(17) Uani 1 1 d . . . H16A H 0.5076 0.6313 0.0733 0.144 Uiso 1 1 calc R . . H16B H 0.5116 0.6791 0.1507 0.144 Uiso 1 1 calc R . . H16C H 0.4876 0.5807 0.1354 0.144 Uiso 1 1 calc R . . C17 C 0.6102(2) 0.6508(3) 0.1477(3) 0.112(2) Uani 1 1 d . . . H17A H 0.6453 0.6272 0.1674 0.169 Uiso 1 1 calc R . . H17B H 0.6063 0.7061 0.1736 0.169 Uiso 1 1 calc R . . H17C H 0.6042 0.6632 0.0949 0.169 Uiso 1 1 calc R . . C18 C 0.67353(18) 0.3799(3) 0.0249(3) 0.0743(13) Uani 1 1 d . . . C19 C 0.6951(4) 0.4682(5) 0.0073(7) 0.255(7) Uani 1 1 d . . . H19A H 0.6681 0.5009 -0.0289 0.382 Uiso 1 1 calc R . . H19B H 0.7246 0.4571 -0.0132 0.382 Uiso 1 1 calc R . . H19C H 0.7066 0.5038 0.0524 0.382 Uiso 1 1 calc R . . C20 C 0.6587(3) 0.3262(7) -0.0451(5) 0.204(5) Uani 1 1 d . . . H20A H 0.6458 0.2675 -0.0351 0.307 Uiso 1 1 calc R . . H20B H 0.6891 0.3185 -0.0642 0.307 Uiso 1 1 calc R . . H20C H 0.6314 0.3578 -0.0818 0.307 Uiso 1 1 calc R . . C21 C 0.7157(3) 0.3301(8) 0.0801(5) 0.250(6) Uani 1 1 d . . . H21A H 0.7019 0.2732 0.0926 0.374 Uiso 1 1 calc R . . H21B H 0.7278 0.3662 0.1249 0.374 Uiso 1 1 calc R . . H21C H 0.7447 0.3185 0.0588 0.374 Uiso 1 1 calc R . . C22 C 0.50034(17) 0.1876(3) 0.0400(2) 0.0669(12) Uani 1 1 d . . . H22A H 0.4839 0.1325 0.0507 0.100 Uiso 1 1 calc R . . H22B H 0.5259 0.1730 0.0130 0.100 Uiso 1 1 calc R . . H22C H 0.4739 0.2273 0.0099 0.100 Uiso 1 1 calc R . . C23 C 0.6646(2) -0.0168(3) 0.1598(3) 0.1028(19) Uani 1 1 d D . . C24 C 0.6881(4) -0.0856(5) 0.2187(4) 0.213(5) Uani 1 1 d D . . H24A H 0.7163 -0.0580 0.2566 0.319 Uiso 1 1 calc R . . H24B H 0.7018 -0.1358 0.1963 0.319 Uiso 1 1 calc R . . H24C H 0.6615 -0.1073 0.2414 0.319 Uiso 1 1 calc R . . C25 C 0.6240(4) -0.0774(6) 0.1079(6) 0.270(7) Uani 1 1 d D . . H25A H 0.6417 -0.1267 0.0903 0.405 Uiso 1 1 calc R . . H25B H 0.6042 -0.0423 0.0657 0.405 Uiso 1 1 calc R . . H25C H 0.6003 -0.1017 0.1347 0.405 Uiso 1 1 calc R . . C26 C 0.7021(5) 0.0162(5) 0.1194(9) 0.380(12) Uani 1 1 d D . . H26A H 0.7282 0.0541 0.1522 0.570 Uiso 1 1 calc R . . H26B H 0.6834 0.0510 0.0764 0.570 Uiso 1 1 calc R . . H26C H 0.7191 -0.0348 0.1032 0.570 Uiso 1 1 calc R . . C27 C 0.66505(17) 0.2135(3) 0.3667(3) 0.0735(13) Uani 1 1 d . . . C28 C 0.7173(2) 0.1617(4) 0.4051(3) 0.136(3) Uani 1 1 d . . . H28A H 0.7094 0.0988 0.4116 0.204 Uiso 1 1 calc R . . H28B H 0.7333 0.1886 0.4533 0.204 Uiso 1 1 calc R . . H28C H 0.7413 0.1659 0.3740 0.204 Uiso 1 1 calc R . . C29 C 0.6296(2) 0.2048(3) 0.4190(2) 0.0932(16) Uani 1 1 d . . . H29A H 0.6218 0.1416 0.4245 0.140 Uiso 1 1 calc R . . H29B H 0.5972 0.2375 0.3984 0.140 Uiso 1 1 calc R . . H29C H 0.6472 0.2298 0.4673 0.140 Uiso 1 1 calc R . . C30 C 0.67906(19) 0.3151(3) 0.3572(3) 0.1001(17) Uani 1 1 d . . . H30A H 0.6473 0.3484 0.3341 0.150 Uiso 1 1 calc R . . H30B H 0.7030 0.3188 0.3259 0.150 Uiso 1 1 calc R . . H30C H 0.6955 0.3410 0.4056 0.150 Uiso 1 1 calc R . . C31 C 0.45014(16) 0.4227(3) 0.0976(2) 0.0675(12) Uani 1 1 d . . . H31A H 0.4545 0.4614 0.0577 0.101 Uiso 1 1 calc R . . H31B H 0.4231 0.4473 0.1181 0.101 Uiso 1 1 calc R . . H31C H 0.4401 0.3626 0.0783 0.101 Uiso 1 1 calc R . . O3 O 0.5000 0.0916(18) -0.2500 0.530(15) Uiso 1 2 d S . . C33 C 0.5345(6) 0.0445(13) -0.1857(10) 0.370(9) Uiso 1 1 d D . . H33A H 0.5486 -0.0077 -0.2063 0.444 Uiso 1 1 calc R . . H33B H 0.5114 0.0200 -0.1572 0.444 Uiso 1 1 calc R . . C34 C 0.5810(6) 0.0863(10) -0.1283(9) 0.331(7) Uiso 1 1 d D . . H34A H 0.5976 0.0407 -0.0923 0.497 Uiso 1 1 calc R . . H34B H 0.5688 0.1354 -0.1028 0.497 Uiso 1 1 calc R . . H34C H 0.6061 0.1094 -0.1533 0.497 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 Mg 0.0571(12) 0.0494(10) 0.0361(10) 0.000 0.0141(9) 0.000 O1 0.0566(17) 0.0543(15) 0.0398(15) 0.0019(12) 0.0145(14) 0.0039(12) O2 0.0566(16) 0.0545(15) 0.0416(15) -0.0035(12) 0.0101(13) 0.0072(13) C1 0.058(3) 0.052(2) 0.031(2) 0.0076(17) 0.0137(19) 0.0025(19) C2 0.070(3) 0.050(2) 0.044(2) 0.0077(18) 0.020(2) 0.000(2) C3 0.073(3) 0.061(3) 0.049(3) 0.006(2) 0.021(2) -0.010(2) C4 0.058(3) 0.068(3) 0.049(3) 0.007(2) 0.017(2) 0.000(2) C5 0.064(3) 0.058(3) 0.045(2) -0.0007(19) 0.015(2) 0.005(2) C6 0.057(3) 0.055(2) 0.034(2) 0.0002(18) 0.0082(19) 0.000(2) C7 0.065(3) 0.047(2) 0.036(2) -0.0031(17) 0.012(2) -0.0030(19) C8 0.061(3) 0.046(2) 0.041(2) -0.0007(18) 0.015(2) 0.0001(19) C9 0.093(4) 0.057(3) 0.052(3) -0.006(2) 0.020(3) 0.006(2) C10 0.092(4) 0.063(3) 0.059(3) -0.005(2) 0.017(3) 0.024(3) C11 0.075(3) 0.072(3) 0.061(3) -0.001(2) 0.013(3) 0.020(2) C12 0.057(3) 0.065(3) 0.047(2) -0.004(2) 0.010(2) 0.006(2) C13 0.057(3) 0.047(2) 0.039(2) -0.0015(18) 0.013(2) 0.0036(19) C14 0.100(4) 0.052(3) 0.065(3) 0.000(2) 0.038(3) -0.006(3) C15 0.149(5) 0.079(3) 0.061(3) -0.015(3) 0.037(3) -0.020(3) C16 0.132(5) 0.059(3) 0.106(4) 0.008(3) 0.046(4) 0.023(3) C17 0.164(6) 0.069(3) 0.128(5) -0.022(3) 0.080(5) -0.041(3) C18 0.066(3) 0.085(3) 0.080(4) 0.001(3) 0.032(3) -0.001(3) C19 0.267(10) 0.121(6) 0.502(19) 0.000(8) 0.322(13) -0.025(6) C20 0.163(7) 0.341(12) 0.153(7) -0.130(8) 0.119(6) -0.083(7) C21 0.099(6) 0.500(19) 0.159(8) 0.098(10) 0.049(5) 0.138(8) C22 0.078(3) 0.071(3) 0.045(2) -0.008(2) 0.005(2) -0.010(2) C23 0.147(5) 0.086(4) 0.079(4) -0.009(3) 0.035(4) 0.049(4) C24 0.322(12) 0.161(7) 0.146(7) 0.003(6) 0.047(7) 0.171(8) C25 0.351(14) 0.196(9) 0.203(10) -0.121(8) -0.028(10) 0.149(10) C26 0.55(2) 0.100(6) 0.73(3) 0.044(10) 0.58(2) 0.080(9) C27 0.060(3) 0.085(3) 0.061(3) -0.017(3) -0.007(2) 0.015(2) C28 0.093(4) 0.173(6) 0.101(4) -0.041(4) -0.046(3) 0.055(4) C29 0.121(4) 0.106(4) 0.047(3) 0.000(3) 0.014(3) 0.020(3) C30 0.078(4) 0.105(4) 0.105(4) -0.034(3) 0.005(3) -0.018(3) C31 0.064(3) 0.084(3) 0.051(3) 0.010(2) 0.009(2) 0.013(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 Mg O2 1.865(2) . ? Mg O2 1.865(2) 2_655 ? Mg O1 2.091(2) 2_655 ? Mg O1 2.091(2) . ? O1 C1 1.432(4) . ? O1 C31 1.462(4) . ? O2 C13 1.341(4) . ? C1 C6 1.389(5) . ? C1 C2 1.397(5) . ? C2 C3 1.392(5) . ? C2 C14 1.539(5) . ? C3 C4 1.383(5) . ? C4 C5 1.377(5) . ? C4 C18 1.514(6) . ? C5 C6 1.392(5) . ? C6 C7 1.537(5) . ? C7 C8 1.519(5) . ? C7 C22 1.546(5) . ? C8 C9 1.389(5) . ? C8 C13 1.420(5) . ? C9 C10 1.389(6) . ? C10 C11 1.389(6) . ? C10 C23 1.512(4) . ? C11 C12 1.382(5) . ? C12 C13 1.419(5) . ? C12 C27 1.534(6) . ? C14 C17 1.532(6) . ? C14 C15 1.534(6) . ? C14 C16 1.555(6) . ? C18 C20 1.474(8) . ? C18 C21 1.480(8) . ? C18 C19 1.483(7) . ? C23 C26 1.465(5) . ? C23 C24 1.491(5) . ? C23 C25 1.515(5) . ? C27 C29 1.515(6) . ? C27 C30 1.554(6) . ? C27 C28 1.560(6) . ? O3 C33 1.460(19) 2_654 ? O3 C33 1.460(19) . ? C33 C34 1.514(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 O2 Mg O2 129.27(17) . 2_655 ? O2 Mg O1 107.77(10) . 2_655 ? O2 Mg O1 100.40(10) 2_655 2_655 ? O2 Mg O1 100.40(10) . . ? O2 Mg O1 107.77(10) 2_655 . ? O1 Mg O1 110.94(14) 2_655 . ? C1 O1 C31 111.3(3) . . ? C1 O1 Mg 118.0(2) . . ? C31 O1 Mg 116.3(2) . . ? C13 O2 Mg 140.9(2) . . ? C6 C1 C2 123.0(3) . . ? C6 C1 O1 117.1(3) . . ? C2 C1 O1 119.9(3) . . ? C3 C2 C1 115.0(4) . . ? C3 C2 C14 119.9(4) . . ? C1 C2 C14 124.9(3) . . ? C4 C3 C2 125.3(4) . . ? C5 C4 C3 116.0(4) . . ? C5 C4 C18 121.0(4) . . ? C3 C4 C18 122.9(4) . . ? C4 C5 C6 123.2(4) . . ? C1 C6 C5 117.4(3) . . ? C1 C6 C7 124.8(3) . . ? C5 C6 C7 117.5(3) . . ? C8 C7 C6 105.9(3) . . ? C8 C7 C22 115.4(3) . . ? C6 C7 C22 111.5(3) . . ? C9 C8 C13 119.9(4) . . ? C9 C8 C7 121.5(4) . . ? C13 C8 C7 118.0(3) . . ? C10 C9 C8 122.8(4) . . ? C11 C10 C9 115.4(4) . . ? C11 C10 C23 123.4(4) . . ? C9 C10 C23 121.2(4) . . ? C12 C11 C10 125.5(4) . . ? C11 C12 C13 117.7(4) . . ? C11 C12 C27 121.5(4) . . ? C13 C12 C27 120.8(3) . . ? O2 C13 C12 121.8(3) . . ? O2 C13 C8 119.7(3) . . ? C12 C13 C8 118.4(3) . . ? C17 C14 C15 107.9(4) . . ? C17 C14 C2 112.9(4) . . ? C15 C14 C2 108.6(3) . . ? C17 C14 C16 107.4(4) . . ? C15 C14 C16 108.7(4) . . ? C2 C14 C16 111.2(4) . . ? C20 C18 C21 108.3(7) . . ? C20 C18 C19 107.4(6) . . ? C21 C18 C19 108.8(7) . . ? C20 C18 C4 111.7(4) . . ? C21 C18 C4 107.7(4) . . ? C19 C18 C4 112.7(4) . . ? C26 C23 C24 113.0(7) . . ? C26 C23 C10 110.1(5) . . ? C24 C23 C10 113.5(4) . . ? C26 C23 C25 109.0(8) . . ? C24 C23 C25 98.5(6) . . ? C10 C23 C25 112.2(5) . . ? C29 C27 C12 111.0(4) . . ? C29 C27 C30 110.9(4) . . ? C12 C27 C30 108.6(4) . . ? C29 C27 C28 106.5(4) . . ? C12 C27 C28 111.7(4) . . ? C30 C27 C28 108.2(4) . . ? C33 O3 C33 123(3) 2_654 . ? O3 C33 C34 125.8(18) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.13 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.377 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.056 # Attachment '4.cif' data_mys1m _database_code_depnum_ccdc_archive 'CCDC 737434' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C76 H108 Mg2 O6, 2(C7 H8)' _chemical_formula_sum 'C90 H124 Mg2 O6' _chemical_formula_weight 1350.51 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' 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 18.354(3) _cell_length_b 14.909(3) _cell_length_c 30.879(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.342(4) _cell_angle_gamma 90.00 _cell_volume 8313(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5860 _cell_measurement_theta_min 2.256 _cell_measurement_theta_max 25.907 _exptl_crystal_description parallelpiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.079 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.933 _exptl_absorpt_correction_T_max 0.987 _exptl_absorpt_process_details 'SADABS, Sheldrick (1996)' _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 21853 _diffrn_reflns_av_R_equivalents 0.0683 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 26.01 _reflns_number_total 8057 _reflns_number_gt 4816 _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^)+(0.1000P)^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 8057 _refine_ls_number_parameters 430 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1250 _refine_ls_R_factor_gt 0.0755 _refine_ls_wR_factor_ref 0.2081 _refine_ls_wR_factor_gt 0.1839 _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_restrained_S_all 1.153 _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 0.00970(5) 0.43297(6) 0.20456(3) 0.0362(2) Uani 1 1 d . . . O1 O 0.02591(11) 0.34069(12) 0.16728(5) 0.0431(5) Uani 1 1 d . . . O2 O 0.01589(10) 0.55709(11) 0.17472(5) 0.0379(4) Uani 1 1 d . . . O3 O 0.07188(10) 0.43672(12) 0.26314(5) 0.0414(5) Uani 1 1 d . . . C1 C 0.02040(15) 0.30312(17) 0.12806(8) 0.0367(6) Uani 1 1 d . . . C2 C 0.02820(16) 0.20818(18) 0.12268(9) 0.0418(7) Uani 1 1 d . . . C3 C 0.02488(18) 0.17569(18) 0.08059(9) 0.0484(7) Uani 1 1 d . . . H3A H 0.0308 0.1143 0.0773 0.058 Uiso 1 1 calc R . . C4 C 0.01342(18) 0.22774(19) 0.04295(9) 0.0481(7) Uani 1 1 d . . . C5 C 0.00373(16) 0.31863(18) 0.04868(9) 0.0421(7) Uani 1 1 d . . . H5A H -0.0047 0.3557 0.0241 0.050 Uiso 1 1 calc R . . C6 C 0.00620(15) 0.35585(16) 0.08975(8) 0.0356(6) Uani 1 1 d . . . C7 C -0.00985(15) 0.45538(16) 0.09544(8) 0.0342(6) Uani 1 1 d . . . H7A H -0.0388 0.4595 0.1191 0.041 Uiso 1 1 calc R . . C8 C 0.06017(15) 0.51053(16) 0.10993(8) 0.0331(6) Uani 1 1 d . . . C9 C 0.11401(15) 0.51191(17) 0.08387(8) 0.0368(6) Uani 1 1 d . . . H9A H 0.1086 0.4746 0.0594 0.044 Uiso 1 1 calc R . . C10 C 0.17598(16) 0.56719(18) 0.09304(8) 0.0407(6) Uani 1 1 d . . . C11 C 0.18094(16) 0.62236(19) 0.12936(9) 0.0449(7) Uani 1 1 d . . . H11A H 0.2206 0.6620 0.1350 0.054 Uiso 1 1 calc R . . C12 C 0.13008(16) 0.62260(18) 0.15827(8) 0.0420(7) Uani 1 1 d . . . C13 C 0.06958(15) 0.56477(16) 0.14738(8) 0.0347(6) Uani 1 1 d . . . C14 C 0.03740(18) 0.14557(19) 0.16312(9) 0.0502(8) Uani 1 1 d . . . C15 C 0.0404(2) 0.0471(2) 0.14972(12) 0.0748(11) Uani 1 1 d . . . H15A H -0.0044 0.0318 0.1299 0.112 Uiso 1 1 calc R . . H15B H 0.0452 0.0099 0.1755 0.112 Uiso 1 1 calc R . . H15C H 0.0821 0.0378 0.1354 0.112 Uiso 1 1 calc R . . C16 C -0.0277(2) 0.1555(2) 0.18727(10) 0.0622(9) Uani 1 1 d . . . H16A H -0.0312 0.2167 0.1963 0.093 Uiso 1 1 calc R . . H16B H -0.0202 0.1173 0.2127 0.093 Uiso 1 1 calc R . . H16C H -0.0726 0.1387 0.1680 0.093 Uiso 1 1 calc R . . C17 C 0.1098(2) 0.1676(2) 0.19477(11) 0.0697(10) Uani 1 1 d . . . H17A H 0.1091 0.2293 0.2037 0.105 Uiso 1 1 calc R . . H17B H 0.1511 0.1578 0.1802 0.105 Uiso 1 1 calc R . . H17C H 0.1144 0.1296 0.2202 0.105 Uiso 1 1 calc R . . C18 C 0.0107(2) 0.1849(2) -0.00283(10) 0.0625(9) Uani 1 1 d . . . C19 C -0.0573(3) 0.1241(3) -0.01278(12) 0.0974(15) Uani 1 1 d . . . H19A H -0.0544 0.0789 0.0096 0.146 Uiso 1 1 calc R . . H19B H -0.0590 0.0959 -0.0409 0.146 Uiso 1 1 calc R . . H19C H -0.1013 0.1592 -0.0133 0.146 Uiso 1 1 calc R . . C20 C 0.0025(3) 0.2537(3) -0.03948(11) 0.0924(15) Uani 1 1 d . . . H20A H 0.0441 0.2938 -0.0345 0.139 Uiso 1 1 calc R . . H20B H -0.0423 0.2872 -0.0400 0.139 Uiso 1 1 calc R . . H20C H 0.0006 0.2237 -0.0672 0.139 Uiso 1 1 calc R . . C21 C 0.0807(3) 0.1290(3) -0.00289(13) 0.0951(15) Uani 1 1 d . . . H21A H 0.0857 0.0855 0.0204 0.143 Uiso 1 1 calc R . . H21B H 0.1232 0.1677 0.0016 0.143 Uiso 1 1 calc R . . H21C H 0.0771 0.0988 -0.0307 0.143 Uiso 1 1 calc R . . C22 C -0.05638(17) 0.49774(19) 0.05487(9) 0.0453(7) Uani 1 1 d . . . H22A H -0.0647 0.5598 0.0606 0.068 Uiso 1 1 calc R . . H22B H -0.1031 0.4672 0.0479 0.068 Uiso 1 1 calc R . . H22C H -0.0307 0.4929 0.0305 0.068 Uiso 1 1 calc R . . C23 C 0.23490(16) 0.5715(2) 0.06355(9) 0.0471(7) Uani 1 1 d . . . C24 C 0.2361(2) 0.4863(2) 0.03600(11) 0.0625(9) Uani 1 1 d . . . H24A H 0.1883 0.4774 0.0180 0.094 Uiso 1 1 calc R . . H24B H 0.2481 0.4357 0.0552 0.094 Uiso 1 1 calc R . . H24C H 0.2726 0.4924 0.0175 0.094 Uiso 1 1 calc R . . C25 C 0.2174(2) 0.6520(2) 0.03281(11) 0.0652(9) Uani 1 1 d . . . H25A H 0.2169 0.7056 0.0500 0.098 Uiso 1 1 calc R . . H25B H 0.1697 0.6437 0.0145 0.098 Uiso 1 1 calc R . . H25C H 0.2545 0.6571 0.0147 0.098 Uiso 1 1 calc R . . C26 C 0.31215(19) 0.5827(3) 0.09129(11) 0.0780(12) Uani 1 1 d . . . H26A H 0.3133 0.6356 0.1091 0.117 Uiso 1 1 calc R . . H26B H 0.3479 0.5883 0.0722 0.117 Uiso 1 1 calc R . . H26C H 0.3238 0.5312 0.1099 0.117 Uiso 1 1 calc R . . C27 C 0.1457(2) 0.6898(2) 0.19764(10) 0.0556(8) Uani 1 1 d . . . C28 C 0.1292(3) 0.7838(2) 0.17837(14) 0.1022(17) Uani 1 1 d . . . H28A H 0.1382 0.8274 0.2016 0.153 Uiso 1 1 calc R . . H28B H 0.0784 0.7871 0.1640 0.153 Uiso 1 1 calc R . . H28C H 0.1608 0.7959 0.1574 0.153 Uiso 1 1 calc R . . C29 C 0.2287(2) 0.6844(3) 0.21856(13) 0.0999(15) Uani 1 1 d . . . H29A H 0.2396 0.6257 0.2308 0.150 Uiso 1 1 calc R . . H29B H 0.2397 0.7285 0.2415 0.150 Uiso 1 1 calc R . . H29C H 0.2582 0.6956 0.1964 0.150 Uiso 1 1 calc R . . C30 C 0.1035(3) 0.6737(3) 0.23388(12) 0.0952(16) Uani 1 1 d . . . H30A H 0.1150 0.6151 0.2461 0.143 Uiso 1 1 calc R . . H30B H 0.0513 0.6776 0.2225 0.143 Uiso 1 1 calc R . . H30C H 0.1169 0.7180 0.2564 0.143 Uiso 1 1 calc R . . C31 C -0.04817(18) 0.6136(2) 0.16135(10) 0.0515(8) Uani 1 1 d . . . H31A H -0.0335 0.6675 0.1482 0.077 Uiso 1 1 calc R . . H31B H -0.0694 0.6287 0.1866 0.077 Uiso 1 1 calc R . . H31C H -0.0841 0.5822 0.1403 0.077 Uiso 1 1 calc R . . C32 C 0.14714(18) 0.4131(3) 0.27301(10) 0.0714(11) Uani 1 1 d . . . H32A H 0.1745 0.4503 0.2557 0.086 Uiso 1 1 calc R . . H32B H 0.1525 0.3512 0.2644 0.086 Uiso 1 1 calc R . . C33 C 0.18045(17) 0.4233(2) 0.32066(10) 0.0524(8) Uani 1 1 d . . . C34 C 0.2286(2) 0.4920(3) 0.33517(13) 0.0766(11) Uani 1 1 d . . . H34A H 0.2407 0.5332 0.3150 0.092 Uiso 1 1 calc R . . C35 C 0.2590(3) 0.5011(4) 0.37876(17) 0.1006(15) Uani 1 1 d . . . H35A H 0.2922 0.5474 0.3879 0.121 Uiso 1 1 calc R . . C36 C 0.2411(3) 0.4435(5) 0.40817(14) 0.1051(18) Uani 1 1 d . . . H36A H 0.2610 0.4510 0.4378 0.126 Uiso 1 1 calc R . . C37 C 0.1936(3) 0.3731(4) 0.39531(14) 0.0907(15) Uani 1 1 d . . . H37A H 0.1822 0.3324 0.4159 0.109 Uiso 1 1 calc R . . C38 C 0.16321(19) 0.3639(2) 0.35157(12) 0.0634(9) Uani 1 1 d . . . H38A H 0.1306 0.3170 0.3426 0.076 Uiso 1 1 calc R . . C41 C -0.2127(6) 0.7900(4) 0.1171(2) 0.258(7) Uani 1 1 d GD . . C42 C -0.2707(3) 0.8210(7) 0.1364(4) 0.282(11) Uani 1 1 d G . . H42A H -0.3191 0.8035 0.1252 0.338 Uiso 1 1 calc R . . C43 C -0.2564(7) 0.8782(7) 0.1725(4) 0.349(15) Uani 1 1 d G . . H43A H -0.2952 0.8989 0.1855 0.419 Uiso 1 1 calc R . . C44 C -0.1842(9) 0.9043(5) 0.1892(2) 0.258(7) Uani 1 1 d G . . H44A H -0.1746 0.9426 0.2134 0.310 Uiso 1 1 calc R . . C45 C -0.1262(5) 0.8734(6) 0.1699(4) 0.346(14) Uani 1 1 d G . . H45A H -0.0779 0.8909 0.1811 0.415 Uiso 1 1 calc R . . C46 C -0.1405(4) 0.8162(6) 0.1338(4) 0.208(6) Uani 1 1 d G . . H46A H -0.1017 0.7955 0.1208 0.250 Uiso 1 1 calc R . . C47 C -0.2395(14) 0.7310(10) 0.0784(4) 0.54(2) Uani 1 1 d D . . H47A H -0.2922 0.7235 0.0751 0.814 Uiso 1 1 calc R . . H47B H -0.2158 0.6735 0.0830 0.814 Uiso 1 1 calc R . . H47C H -0.2278 0.7580 0.0523 0.814 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 0.0359(5) 0.0385(5) 0.0348(4) -0.0006(4) 0.0081(4) -0.0028(4) O1 0.0472(12) 0.0404(10) 0.0414(10) -0.0041(8) 0.0070(9) 0.0015(9) O2 0.0396(11) 0.0359(9) 0.0416(10) -0.0022(7) 0.0163(8) -0.0040(8) O3 0.0313(10) 0.0521(11) 0.0403(9) -0.0021(8) 0.0048(8) 0.0044(9) C1 0.0329(15) 0.0350(14) 0.0429(15) -0.0051(11) 0.0090(12) -0.0031(12) C2 0.0397(17) 0.0349(14) 0.0507(16) 0.0016(12) 0.0081(13) -0.0011(13) C3 0.055(2) 0.0314(14) 0.0610(18) -0.0042(13) 0.0164(15) -0.0001(14) C4 0.058(2) 0.0389(15) 0.0513(16) -0.0074(13) 0.0195(14) -0.0074(14) C5 0.0494(18) 0.0357(14) 0.0428(15) -0.0018(12) 0.0130(13) -0.0050(13) C6 0.0331(15) 0.0284(13) 0.0463(15) -0.0057(11) 0.0095(12) -0.0068(11) C7 0.0323(15) 0.0333(13) 0.0378(13) -0.0021(10) 0.0088(11) -0.0029(11) C8 0.0335(15) 0.0293(12) 0.0368(13) 0.0019(10) 0.0072(11) -0.0024(11) C9 0.0367(16) 0.0394(14) 0.0362(13) -0.0023(11) 0.0114(11) 0.0005(12) C10 0.0387(16) 0.0443(15) 0.0399(14) 0.0036(12) 0.0097(12) -0.0050(13) C11 0.0374(17) 0.0512(17) 0.0470(15) -0.0022(13) 0.0101(13) -0.0184(14) C12 0.0437(17) 0.0419(15) 0.0415(14) -0.0039(12) 0.0111(12) -0.0110(13) C13 0.0374(15) 0.0327(13) 0.0361(13) 0.0023(11) 0.0127(11) -0.0041(12) C14 0.052(2) 0.0423(16) 0.0554(17) 0.0059(13) 0.0065(15) 0.0047(14) C15 0.099(3) 0.0406(18) 0.084(2) 0.0154(16) 0.014(2) 0.0071(19) C16 0.069(2) 0.061(2) 0.0578(19) 0.0136(15) 0.0134(17) -0.0063(18) C17 0.060(2) 0.065(2) 0.080(2) 0.0162(18) -0.0019(19) 0.0104(18) C18 0.094(3) 0.0430(17) 0.0558(18) -0.0094(14) 0.0293(18) -0.0037(18) C19 0.135(4) 0.085(3) 0.074(2) -0.033(2) 0.022(3) -0.040(3) C20 0.164(5) 0.067(2) 0.053(2) -0.0100(18) 0.038(2) 0.004(3) C21 0.127(4) 0.080(3) 0.089(3) -0.017(2) 0.049(3) 0.022(3) C22 0.0459(18) 0.0402(15) 0.0489(15) 0.0007(12) 0.0061(13) -0.0021(14) C23 0.0378(16) 0.0592(18) 0.0467(15) 0.0038(13) 0.0141(13) -0.0045(14) C24 0.054(2) 0.074(2) 0.066(2) 0.0026(17) 0.0276(17) 0.0099(18) C25 0.067(2) 0.068(2) 0.066(2) 0.0142(17) 0.0273(18) -0.0026(19) C26 0.0357(19) 0.129(4) 0.071(2) 0.007(2) 0.0159(17) -0.009(2) C27 0.063(2) 0.0528(18) 0.0527(17) -0.0128(14) 0.0165(16) -0.0265(16) C28 0.165(5) 0.046(2) 0.099(3) -0.017(2) 0.034(3) -0.016(3) C29 0.078(3) 0.140(4) 0.078(3) -0.043(3) 0.003(2) -0.040(3) C30 0.128(4) 0.106(3) 0.061(2) -0.043(2) 0.043(2) -0.064(3) C31 0.0480(19) 0.0487(17) 0.0608(18) 0.0022(14) 0.0177(15) 0.0118(15) C32 0.0339(17) 0.125(3) 0.0547(19) -0.0135(19) 0.0053(14) 0.019(2) C33 0.0332(16) 0.073(2) 0.0505(17) -0.0042(15) 0.0055(13) 0.0131(16) C34 0.061(3) 0.085(3) 0.084(3) -0.003(2) 0.012(2) -0.015(2) C35 0.069(3) 0.136(4) 0.093(3) -0.040(3) 0.003(3) -0.018(3) C36 0.066(3) 0.183(6) 0.060(3) -0.022(3) -0.005(2) 0.023(4) C37 0.071(3) 0.130(4) 0.076(3) 0.036(3) 0.026(2) 0.050(3) C38 0.044(2) 0.072(2) 0.075(2) 0.0016(18) 0.0131(17) 0.0135(17) C41 0.227(14) 0.197(11) 0.334(17) 0.200(12) 0.013(14) -0.002(11) C42 0.117(6) 0.312(16) 0.45(2) 0.312(18) 0.156(10) 0.107(8) C43 0.45(3) 0.34(2) 0.34(2) 0.218(18) 0.29(2) 0.25(2) C44 0.35(2) 0.195(10) 0.251(10) 0.160(9) 0.103(15) 0.088(14) C45 0.234(14) 0.241(18) 0.60(4) 0.31(2) 0.172(17) 0.123(11) C46 0.139(8) 0.157(9) 0.360(15) 0.166(10) 0.133(9) 0.094(6) C47 0.55(4) 0.36(3) 0.61(4) 0.29(3) -0.19(3) -0.19(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 1.8520(19) . ? Mg1 O3 1.943(2) 2 ? Mg1 O3 1.9587(19) . ? Mg1 O2 2.0795(19) . ? Mg1 Mg1 2.8914(16) 2 ? O1 C1 1.322(3) . ? O2 C13 1.413(3) . ? O2 C31 1.445(3) . ? O3 C32 1.405(4) . ? O3 Mg1 1.943(2) 2 ? C1 C6 1.405(4) . ? C1 C2 1.435(4) . ? C2 C3 1.378(4) . ? C2 C14 1.544(4) . ? C3 C4 1.382(4) . ? C3 H3A 0.9300 . ? C4 C5 1.382(4) . ? C4 C18 1.544(4) . ? C5 C6 1.378(4) . ? C5 H5A 0.9300 . ? C6 C7 1.529(3) . ? C7 C22 1.521(4) . ? C7 C8 1.524(4) . ? C7 H7A 0.9800 . ? C8 C9 1.382(4) . ? C8 C13 1.396(3) . ? C9 C10 1.392(4) . ? C9 H9A 0.9300 . ? C10 C11 1.381(4) . ? C10 C23 1.535(4) . ? C11 C12 1.403(4) . ? C11 H11A 0.9300 . ? C12 C13 1.398(4) . ? C12 C27 1.562(4) . ? C14 C16 1.525(4) . ? C14 C15 1.529(4) . ? C14 C17 1.537(5) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C20 1.515(5) . ? C18 C19 1.528(6) . ? C18 C21 1.533(6) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? 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 C25 1.528(4) . ? C23 C26 1.528(4) . ? C23 C24 1.530(4) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? 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 C30 1.491(5) . ? C27 C28 1.531(5) . ? C27 C29 1.546(5) . ? 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 . ? C32 C33 1.496(4) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.375(5) . ? C33 C38 1.379(5) . ? C34 C35 1.368(6) . ? C34 H34A 0.9300 . ? C35 C36 1.334(7) . ? C35 H35A 0.9300 . ? C36 C37 1.377(7) . ? C36 H36A 0.9300 . ? C37 C38 1.372(5) . ? C37 H37A 0.9300 . ? C38 H38A 0.9300 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C41 C47 1.494(6) . ? C42 C43 1.3900 . ? C42 H42A 0.9300 . ? C43 C44 1.3900 . ? C43 H43A 0.9300 . ? C44 C45 1.3900 . ? C44 H44A 0.9300 . ? C45 C46 1.3900 . ? C45 H45A 0.9300 . ? C46 H46A 0.9300 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 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 O1 Mg1 O3 124.40(9) . 2 ? O1 Mg1 O3 117.59(9) . . ? O3 Mg1 O3 84.27(9) 2 . ? O1 Mg1 O2 110.97(8) . . ? O3 Mg1 O2 108.08(8) 2 . ? O3 Mg1 O2 108.35(8) . . ? O1 Mg1 Mg1 131.67(6) . 2 ? O3 Mg1 Mg1 42.39(5) 2 2 ? O3 Mg1 Mg1 41.98(6) . 2 ? O2 Mg1 Mg1 117.14(5) . 2 ? C1 O1 Mg1 152.88(17) . . ? C13 O2 C31 113.64(19) . . ? C13 O2 Mg1 115.88(14) . . ? C31 O2 Mg1 122.62(17) . . ? C32 O3 Mg1 134.40(19) . 2 ? C32 O3 Mg1 125.48(17) . . ? Mg1 O3 Mg1 95.64(9) 2 . ? O1 C1 C6 120.4(2) . . ? O1 C1 C2 122.1(2) . . ? C6 C1 C2 117.5(2) . . ? C3 C2 C1 117.9(2) . . ? C3 C2 C14 122.0(2) . . ? C1 C2 C14 120.1(2) . . ? C2 C3 C4 124.8(3) . . ? C2 C3 H3A 117.6 . . ? C4 C3 H3A 117.6 . . ? C3 C4 C5 116.5(3) . . ? C3 C4 C18 120.9(3) . . ? C5 C4 C18 122.6(3) . . ? C6 C5 C4 121.9(2) . . ? C6 C5 H5A 119.0 . . ? C4 C5 H5A 119.0 . . ? C5 C6 C1 121.3(2) . . ? C5 C6 C7 121.4(2) . . ? C1 C6 C7 117.2(2) . . ? C22 C7 C8 109.7(2) . . ? C22 C7 C6 113.6(2) . . ? C8 C7 C6 112.8(2) . . ? C22 C7 H7A 106.8 . . ? C8 C7 H7A 106.8 . . ? C6 C7 H7A 106.8 . . ? C9 C8 C13 118.6(2) . . ? C9 C8 C7 119.4(2) . . ? C13 C8 C7 121.9(2) . . ? C8 C9 C10 122.3(2) . . ? C8 C9 H9A 118.9 . . ? C10 C9 H9A 118.9 . . ? C11 C10 C9 116.8(2) . . ? C11 C10 C23 120.4(3) . . ? C9 C10 C23 122.8(2) . . ? C10 C11 C12 124.3(3) . . ? C10 C11 H11A 117.8 . . ? C12 C11 H11A 117.8 . . ? C13 C12 C11 115.8(2) . . ? C13 C12 C27 127.6(2) . . ? C11 C12 C27 116.6(2) . . ? C8 C13 C12 122.1(2) . . ? C8 C13 O2 116.9(2) . . ? C12 C13 O2 121.0(2) . . ? C16 C14 C15 107.1(3) . . ? C16 C14 C17 109.4(3) . . ? C15 C14 C17 108.0(3) . . ? C16 C14 C2 110.8(2) . . ? C15 C14 C2 111.4(2) . . ? C17 C14 C2 110.0(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C20 C18 C19 106.5(3) . . ? C20 C18 C21 109.7(3) . . ? C19 C18 C21 109.4(3) . . ? C20 C18 C4 112.7(3) . . ? C19 C18 C4 108.7(3) . . ? C21 C18 C4 109.7(3) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C7 C22 H22A 109.5 . . ? C7 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C7 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C25 C23 C26 109.5(3) . . ? C25 C23 C24 109.2(2) . . ? C26 C23 C24 107.3(3) . . ? C25 C23 C10 108.0(2) . . ? C26 C23 C10 110.7(2) . . ? C24 C23 C10 112.2(2) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C30 C27 C28 110.3(3) . . ? C30 C27 C29 106.5(3) . . ? C28 C27 C29 108.7(3) . . ? C30 C27 C12 115.7(3) . . ? C28 C27 C12 106.8(3) . . ? C29 C27 C12 108.7(3) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O2 C31 H31A 109.5 . . ? O2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O3 C32 C33 113.6(2) . . ? O3 C32 H32A 108.8 . . ? C33 C32 H32A 108.8 . . ? O3 C32 H32B 108.8 . . ? C33 C32 H32B 108.8 . . ? H32A C32 H32B 107.7 . . ? C34 C33 C38 117.8(3) . . ? C34 C33 C32 121.4(3) . . ? C38 C33 C32 120.7(3) . . ? C35 C34 C33 121.3(4) . . ? C35 C34 H34A 119.3 . . ? C33 C34 H34A 119.3 . . ? C36 C35 C34 119.9(5) . . ? C36 C35 H35A 120.0 . . ? C34 C35 H35A 120.0 . . ? C35 C36 C37 121.1(4) . . ? C35 C36 H36A 119.5 . . ? C37 C36 H36A 119.5 . . ? C38 C37 C36 119.0(4) . . ? C38 C37 H37A 120.5 . . ? C36 C37 H37A 120.5 . . ? C37 C38 C33 120.9(4) . . ? C37 C38 H38A 119.5 . . ? C33 C38 H38A 119.5 . . ? C42 C41 C46 120.0 . . ? C42 C41 C47 111.8(13) . . ? C46 C41 C47 128.2(13) . . ? C41 C42 C43 120.0 . . ? C41 C42 H42A 120.0 . . ? C43 C42 H42A 120.0 . . ? C42 C43 C44 120.0 . . ? C42 C43 H43A 120.0 . . ? C44 C43 H43A 120.0 . . ? C45 C44 C43 120.0 . . ? C45 C44 H44A 120.0 . . ? C43 C44 H44A 120.0 . . ? C46 C45 C44 120.0 . . ? C46 C45 H45A 120.0 . . ? C44 C45 H45A 120.0 . . ? C45 C46 C41 120.0 . . ? C45 C46 H46A 120.0 . . ? C41 C46 H46A 120.0 . . ? C41 C47 H47A 109.5 . . ? C41 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C41 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.338 _refine_diff_density_min -0.272 _refine_diff_density_rms 0.058 # Attachment '5.cif' data_green2m _database_code_depnum_ccdc_archive 'CCDC 737435' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C70 H116 N4 O4 Mg2 2(C H2 Cl2)' _chemical_formula_sum 'C72 H120 Cl4 Mg2 N4 O4' _chemical_formula_weight 1296.4 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.566(2) _cell_length_b 10.567(2) _cell_length_c 18.362(4) _cell_angle_alpha 84.166(5) _cell_angle_beta 80.160(4) _cell_angle_gamma 77.437(5) _cell_volume 1967.3(8) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2414 _cell_measurement_theta_min 2.257 _cell_measurement_theta_max 22.614 _exptl_crystal_description parallelpiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.094 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 0.211 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.926 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_process_details 'SADABS, Sheldrick (1996)' _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 10833 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0653 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 26.01 _reflns_number_total 7631 _reflns_number_gt 3722 _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^)+(0.1293P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7631 _refine_ls_number_parameters 388 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1421 _refine_ls_R_factor_gt 0.0766 _refine_ls_wR_factor_ref 0.2556 _refine_ls_wR_factor_gt 0.2174 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 0.04658(11) 0.86587(10) 0.47922(6) 0.0504(3) Uani 1 1 d . . . Cl1 Cl 0.5690(2) 0.1061(3) 0.41606(19) 0.2154(13) Uani 1 1 d . . . Cl2 Cl 0.4732(2) 0.1328(2) 0.27896(12) 0.1750(9) Uani 1 1 d . . . O1 O -0.0165(3) 1.0275(2) 0.23128(14) 0.0670(7) Uani 1 1 d . . . O2 O 0.1123(2) 0.7557(2) 0.40444(12) 0.0589(6) Uani 1 1 d . . . N1 N -0.1373(3) 0.9840(3) 0.50501(17) 0.0594(8) Uani 1 1 d . . . H1A H -0.1698 1.0555 0.4808 0.071 Uiso 1 1 d R . . N2 N -0.0002(3) 0.7613(3) 0.58474(17) 0.0643(8) Uani 1 1 d . . . C1 C 0.1437(3) 0.6870(3) 0.34485(17) 0.0485(8) Uani 1 1 d . . . C2 C 0.2661(3) 0.6010(3) 0.32864(18) 0.0500(8) Uani 1 1 d . . . C3 C 0.3706(4) 0.5835(4) 0.3801(2) 0.0632(10) Uani 1 1 d . . . C4 C 0.4052(4) 0.7133(5) 0.3894(3) 0.0890(14) Uani 1 1 d . . . H4A H 0.3276 0.7725 0.4098 0.133 Uiso 1 1 calc R . . H4B H 0.4407 0.7490 0.3421 0.133 Uiso 1 1 calc R . . H4C H 0.4691 0.7001 0.4223 0.133 Uiso 1 1 calc R . . C5 C 0.3191(4) 0.5218(5) 0.4554(2) 0.0904(14) Uani 1 1 d . . . H5A H 0.2978 0.4404 0.4486 0.136 Uiso 1 1 calc R . . H5B H 0.2419 0.5790 0.4778 0.136 Uiso 1 1 calc R . . H5C H 0.3853 0.5074 0.4869 0.136 Uiso 1 1 calc R . . C6 C 0.4995(4) 0.4929(5) 0.3494(3) 0.0883(14) Uani 1 1 d . . . H6A H 0.4821 0.4100 0.3421 0.132 Uiso 1 1 calc R . . H6B H 0.5603 0.4817 0.3840 0.132 Uiso 1 1 calc R . . H6C H 0.5364 0.5305 0.3030 0.132 Uiso 1 1 calc R . . C7 C 0.2888(4) 0.5324(3) 0.26559(19) 0.0552(9) Uani 1 1 d . . . H7A H 0.3690 0.4751 0.2553 0.066 Uiso 1 1 calc R . . C8 C 0.1986(4) 0.5441(3) 0.21672(18) 0.0527(9) Uani 1 1 d . . . C9 C 0.2317(4) 0.4658(3) 0.1477(2) 0.0614(10) Uani 1 1 d . . . C10 C 0.3573(5) 0.4883(6) 0.1023(3) 0.1157(19) Uani 1 1 d . . . H10A H 0.4264 0.4653 0.1320 0.174 Uiso 1 1 calc R . . H10B H 0.3477 0.5783 0.0853 0.174 Uiso 1 1 calc R . . H10C H 0.3784 0.4357 0.0605 0.174 Uiso 1 1 calc R . . C11 C 0.2378(7) 0.3236(4) 0.1696(3) 0.122(2) Uani 1 1 d . . . H11A H 0.3046 0.2928 0.2003 0.183 Uiso 1 1 calc R . . H11B H 0.2581 0.2757 0.1259 0.183 Uiso 1 1 calc R . . H11C H 0.1545 0.3117 0.1965 0.183 Uiso 1 1 calc R . . C12 C 0.1240(5) 0.5037(5) 0.0977(3) 0.1055(17) Uani 1 1 d . . . H12A H 0.1486 0.4533 0.0550 0.158 Uiso 1 1 calc R . . H12B H 0.1138 0.5944 0.0822 0.158 Uiso 1 1 calc R . . H12C H 0.0426 0.4871 0.1249 0.158 Uiso 1 1 calc R . . C13 C 0.0824(4) 0.6293(3) 0.23351(18) 0.0531(9) Uani 1 1 d . . . H13A H 0.0204 0.6395 0.2018 0.064 Uiso 1 1 calc R . . C14 C 0.0519(3) 0.7013(3) 0.29540(18) 0.0492(8) Uani 1 1 d . . . C15 C -0.0785(3) 0.7956(3) 0.31122(18) 0.0558(9) Uani 1 1 d . . . H15A H -0.0620 0.8676 0.3355 0.067 Uiso 1 1 calc R . . C16 C -0.1733(4) 0.7304(4) 0.3670(2) 0.0759(12) Uani 1 1 d . . . H16A H -0.2553 0.7906 0.3776 0.114 Uiso 1 1 calc R . . H16B H -0.1366 0.7043 0.4119 0.114 Uiso 1 1 calc R . . H16C H -0.1874 0.6555 0.3467 0.114 Uiso 1 1 calc R . . C17 C -0.1362(3) 0.8547(3) 0.24169(18) 0.0499(8) Uani 1 1 d . . . C18 C -0.1062(3) 0.9704(3) 0.20524(19) 0.0524(9) Uani 1 1 d . . . C19 C -0.1714(4) 1.0357(3) 0.1477(2) 0.0605(9) Uani 1 1 d . . . C20 C -0.1555(5) 1.1711(4) 0.1131(3) 0.0835(14) Uani 1 1 d . . . C21 C -0.0161(6) 1.1673(5) 0.0712(3) 0.120(2) Uani 1 1 d . . . H21A H -0.0083 1.2528 0.0504 0.180 Uiso 1 1 calc R . . H21B H 0.0010 1.1091 0.0321 0.180 Uiso 1 1 calc R . . H21C H 0.0462 1.1374 0.1048 0.180 Uiso 1 1 calc R . . C22 C -0.1827(7) 1.2658(4) 0.1743(3) 0.127(2) Uani 1 1 d . . . H22A H -0.2698 1.2686 0.2007 0.191 Uiso 1 1 calc R . . H22B H -0.1750 1.3509 0.1528 0.191 Uiso 1 1 calc R . . H22C H -0.1203 1.2371 0.2080 0.191 Uiso 1 1 calc R . . C23 C -0.2533(7) 1.2241(5) 0.0595(4) 0.143(3) Uani 1 1 d . . . H23A H -0.3410 1.2287 0.0854 0.214 Uiso 1 1 calc R . . H23B H -0.2379 1.1674 0.0198 0.214 Uiso 1 1 calc R . . H23C H -0.2424 1.3093 0.0397 0.214 Uiso 1 1 calc R . . C24 C -0.2544(4) 0.9711(4) 0.1219(2) 0.0637(10) Uani 1 1 d . . . H24A H -0.2955 1.0105 0.0821 0.076 Uiso 1 1 calc R . . C25 C -0.2803(3) 0.8519(3) 0.15153(19) 0.0539(9) Uani 1 1 d . . . C26 C -0.3723(4) 0.7860(4) 0.1201(2) 0.0699(11) Uani 1 1 d . . . C27 C -0.5065(6) 0.8181(10) 0.1632(5) 0.221(5) Uani 1 1 d . . . H27A H -0.5032 0.7909 0.2144 0.331 Uiso 1 1 calc R . . H27B H -0.5634 0.7739 0.1446 0.331 Uiso 1 1 calc R . . H27C H -0.5393 0.9102 0.1583 0.331 Uiso 1 1 calc R . . C28 C -0.3212(8) 0.6400(5) 0.1217(5) 0.177(4) Uani 1 1 d . . . H28A H -0.3163 0.6062 0.1719 0.265 Uiso 1 1 calc R . . H28B H -0.2354 0.6215 0.0927 0.265 Uiso 1 1 calc R . . H28C H -0.3795 0.5999 0.1015 0.265 Uiso 1 1 calc R . . C29 C -0.3815(8) 0.8293(7) 0.0401(3) 0.154(3) Uani 1 1 d . . . H29A H -0.4114 0.9219 0.0355 0.231 Uiso 1 1 calc R . . H29B H -0.4423 0.7878 0.0232 0.231 Uiso 1 1 calc R . . H29C H -0.2966 0.8059 0.0108 0.231 Uiso 1 1 calc R . . C30 C -0.2233(3) 0.7984(3) 0.21329(19) 0.0548(9) Uani 1 1 d . . . H30A H -0.2442 0.7217 0.2367 0.066 Uiso 1 1 calc R . . C31 C 0.1173(4) 0.9693(4) 0.2107(3) 0.0774(12) Uani 1 1 d . . . H31A H 0.1712 1.0142 0.2315 0.116 Uiso 1 1 calc R . . H31B H 0.1391 0.9746 0.1577 0.116 Uiso 1 1 calc R . . H31C H 0.1324 0.8798 0.2291 0.116 Uiso 1 1 calc R . . C32 C -0.2047(4) 0.9238(4) 0.5716(3) 0.0856(13) Uani 1 1 d . . . H32A H -0.2489 0.8607 0.5575 0.103 Uiso 1 1 calc R . . H32B H -0.2705 0.9898 0.5976 0.103 Uiso 1 1 calc R . . C33 C -0.1087(5) 0.8582(4) 0.6216(2) 0.0857(14) Uani 1 1 d . . . H33A H -0.0723 0.9235 0.6397 0.103 Uiso 1 1 calc R . . H33B H -0.1547 0.8154 0.6640 0.103 Uiso 1 1 calc R . . C34 C -0.0456(5) 0.6425(4) 0.5752(3) 0.0864(13) Uani 1 1 d . . . H34A H -0.0653 0.5982 0.6227 0.130 Uiso 1 1 calc R . . H34B H 0.0220 0.5866 0.5446 0.130 Uiso 1 1 calc R . . H34C H -0.1230 0.6654 0.5520 0.130 Uiso 1 1 calc R . . C35 C 0.1064(5) 0.7263(5) 0.6307(3) 0.1032(16) Uani 1 1 d . . . H35A H 0.0764 0.6808 0.6761 0.155 Uiso 1 1 calc R . . H35B H 0.1308 0.8039 0.6416 0.155 Uiso 1 1 calc R . . H35C H 0.1810 0.6715 0.6042 0.155 Uiso 1 1 calc R . . C36 C 0.5774(9) 0.0560(9) 0.3289(5) 0.235(6) Uani 1 1 d . . . H36A H 0.6641 0.0595 0.3021 0.282 Uiso 1 1 calc R . . H36B H 0.5698 -0.0344 0.3342 0.282 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 0.0599(7) 0.0490(7) 0.0438(6) -0.0115(5) -0.0066(5) -0.0117(5) Cl1 0.1370(17) 0.277(3) 0.227(3) 0.049(2) -0.0836(18) -0.0177(18) Cl2 0.1572(17) 0.200(2) 0.1488(17) -0.0077(15) -0.0020(14) -0.0132(16) O1 0.0715(17) 0.0661(16) 0.0724(17) -0.0165(13) -0.0208(14) -0.0206(14) O2 0.0682(15) 0.0610(15) 0.0482(14) -0.0164(11) -0.0167(12) -0.0028(12) N1 0.0628(18) 0.0510(17) 0.066(2) -0.0094(14) -0.0094(15) -0.0122(14) N2 0.080(2) 0.0606(19) 0.0539(18) -0.0064(14) -0.0074(16) -0.0199(17) C1 0.065(2) 0.0418(18) 0.0390(18) -0.0073(14) -0.0107(16) -0.0084(16) C2 0.061(2) 0.0432(19) 0.0444(19) -0.0041(14) -0.0121(16) -0.0033(16) C3 0.065(2) 0.073(3) 0.053(2) -0.0112(18) -0.0191(18) -0.005(2) C4 0.079(3) 0.103(4) 0.097(3) -0.026(3) -0.024(3) -0.028(3) C5 0.086(3) 0.124(4) 0.064(3) 0.015(3) -0.035(2) -0.019(3) C6 0.073(3) 0.105(4) 0.081(3) -0.025(3) -0.031(2) 0.016(3) C7 0.063(2) 0.050(2) 0.048(2) -0.0103(15) -0.0089(17) 0.0017(17) C8 0.072(2) 0.0448(19) 0.0435(19) -0.0090(15) -0.0093(17) -0.0126(18) C9 0.084(3) 0.055(2) 0.048(2) -0.0131(16) -0.0090(19) -0.0153(19) C10 0.113(4) 0.167(5) 0.080(3) -0.066(3) 0.018(3) -0.057(4) C11 0.220(7) 0.066(3) 0.086(4) -0.028(3) -0.029(4) -0.028(4) C12 0.125(4) 0.128(4) 0.066(3) -0.042(3) -0.027(3) -0.007(3) C13 0.072(2) 0.050(2) 0.0425(19) -0.0066(15) -0.0217(17) -0.0119(18) C14 0.065(2) 0.0419(18) 0.0430(19) -0.0053(14) -0.0155(16) -0.0091(16) C15 0.069(2) 0.051(2) 0.047(2) -0.0067(15) -0.0185(17) -0.0003(18) C16 0.070(3) 0.093(3) 0.055(2) 0.010(2) -0.013(2) -0.001(2) C17 0.056(2) 0.0459(19) 0.0479(19) -0.0063(15) -0.0139(16) -0.0041(16) C18 0.060(2) 0.050(2) 0.053(2) -0.0094(16) -0.0165(17) -0.0145(17) C19 0.078(2) 0.053(2) 0.055(2) 0.0041(17) -0.0206(19) -0.0180(19) C20 0.124(4) 0.058(3) 0.083(3) 0.019(2) -0.043(3) -0.038(3) C21 0.164(6) 0.110(4) 0.098(4) 0.026(3) -0.015(4) -0.073(4) C22 0.200(6) 0.055(3) 0.130(5) 0.003(3) -0.043(5) -0.023(3) C23 0.198(7) 0.088(4) 0.165(6) 0.075(4) -0.105(5) -0.056(4) C24 0.078(3) 0.063(2) 0.055(2) 0.0067(18) -0.028(2) -0.017(2) C25 0.060(2) 0.053(2) 0.051(2) -0.0039(16) -0.0163(17) -0.0122(17) C26 0.078(3) 0.074(3) 0.069(3) -0.006(2) -0.028(2) -0.027(2) C27 0.100(5) 0.370(13) 0.241(10) -0.204(10) 0.033(5) -0.115(6) C28 0.238(8) 0.079(4) 0.266(10) -0.024(5) -0.173(8) -0.036(5) C29 0.235(8) 0.186(6) 0.097(4) 0.011(4) -0.090(5) -0.123(6) C30 0.064(2) 0.047(2) 0.055(2) 0.0006(16) -0.0149(18) -0.0133(17) C31 0.067(3) 0.082(3) 0.090(3) -0.004(2) -0.019(2) -0.028(2) C32 0.068(3) 0.075(3) 0.105(4) -0.008(3) 0.020(3) -0.021(2) C33 0.110(4) 0.080(3) 0.063(3) -0.013(2) 0.022(3) -0.032(3) C34 0.120(4) 0.066(3) 0.079(3) -0.003(2) -0.008(3) -0.040(3) C35 0.121(4) 0.132(4) 0.066(3) 0.002(3) -0.034(3) -0.034(3) C36 0.194(8) 0.213(9) 0.182(9) 0.052(7) 0.043(7) 0.125(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O2 1.836(2) . ? Mg1 N1 2.076(3) . ? Mg1 N1 2.090(3) 2_576 ? Mg1 N2 2.167(3) . ? Mg1 Mg1 2.925(2) 2_576 ? Cl1 C36 1.718(11) . ? Cl2 C36 1.587(9) . ? O1 C18 1.397(4) . ? O1 C31 1.417(5) . ? O2 C1 1.330(4) . ? N1 C32 1.466(5) . ? N1 Mg1 2.090(3) 2_576 ? N1 H1A 0.8700 . ? N2 C34 1.473(5) . ? N2 C33 1.478(5) . ? N2 C35 1.483(5) . ? C1 C2 1.414(5) . ? C1 C14 1.414(4) . ? C2 C7 1.387(4) . ? C2 C3 1.543(5) . ? C3 C4 1.528(6) . ? C3 C5 1.531(6) . ? C3 C6 1.539(6) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.396(5) . ? C7 H7A 0.9300 . ? C8 C13 1.364(5) . ? C8 C9 1.533(5) . ? C9 C10 1.493(6) . ? C9 C11 1.506(6) . ? C9 C12 1.543(6) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.385(4) . ? C13 H13A 0.9300 . ? C14 C15 1.516(5) . ? C15 C17 1.527(4) . ? C15 C16 1.527(5) . ? C15 H15A 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C30 1.393(5) . ? C17 C18 1.405(5) . ? C18 C19 1.401(5) . ? C19 C24 1.388(5) . ? C19 C20 1.537(5) . ? C20 C23 1.527(6) . ? C20 C22 1.530(7) . ? C20 C21 1.535(7) . ? 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 1.384(5) . ? C24 H24A 0.9300 . ? C25 C30 1.387(5) . ? C25 C26 1.527(5) . ? C26 C27 1.488(7) . ? C26 C29 1.505(6) . ? C26 C28 1.519(7) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 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 0.9300 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C33 1.495(6) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? 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 N1 130.81(12) . . ? O2 Mg1 N1 121.90(12) . 2_576 ? N1 Mg1 N1 90.81(12) . 2_576 ? O2 Mg1 N2 111.97(12) . . ? N1 Mg1 N2 85.65(13) . . ? N1 Mg1 N2 109.26(12) 2_576 . ? O2 Mg1 Mg1 147.29(10) . 2_576 ? N1 Mg1 Mg1 45.60(8) . 2_576 ? N1 Mg1 Mg1 45.21(8) 2_576 2_576 ? N2 Mg1 Mg1 100.48(10) . 2_576 ? C18 O1 C31 115.4(3) . . ? C1 O2 Mg1 170.6(2) . . ? C32 N1 Mg1 107.3(2) . . ? C32 N1 Mg1 116.6(3) . 2_576 ? Mg1 N1 Mg1 89.19(12) . 2_576 ? C32 N1 H1A 125.7 . . ? Mg1 N1 H1A 127.0 . . ? Mg1 N1 H1A 69.5 2_576 . ? C34 N2 C33 110.8(3) . . ? C34 N2 C35 108.6(3) . . ? C33 N2 C35 109.4(4) . . ? C34 N2 Mg1 111.4(2) . . ? C33 N2 Mg1 100.8(2) . . ? C35 N2 Mg1 115.6(3) . . ? O2 C1 C2 122.5(3) . . ? O2 C1 C14 118.8(3) . . ? C2 C1 C14 118.7(3) . . ? C7 C2 C1 118.1(3) . . ? C7 C2 C3 121.1(3) . . ? C1 C2 C3 120.7(3) . . ? C4 C3 C5 110.5(4) . . ? C4 C3 C6 106.6(3) . . ? C5 C3 C6 107.3(3) . . ? C4 C3 C2 111.1(3) . . ? C5 C3 C2 109.2(3) . . ? C6 C3 C2 112.1(3) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 C8 123.9(3) . . ? C2 C7 H7A 118.0 . . ? C8 C7 H7A 118.0 . . ? C13 C8 C7 116.4(3) . . ? C13 C8 C9 122.8(3) . . ? C7 C8 C9 120.8(3) . . ? C10 C9 C11 111.4(4) . . ? C10 C9 C8 110.6(3) . . ? C11 C9 C8 110.3(3) . . ? C10 C9 C12 107.6(4) . . ? C11 C9 C12 104.9(4) . . ? C8 C9 C12 112.0(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C8 C13 C14 123.3(3) . . ? C8 C13 H13A 118.4 . . ? C14 C13 H13A 118.4 . . ? C13 C14 C1 119.6(3) . . ? C13 C14 C15 121.2(3) . . ? C1 C14 C15 119.2(3) . . ? C14 C15 C17 113.7(3) . . ? C14 C15 C16 109.5(3) . . ? C17 C15 C16 112.9(3) . . ? C14 C15 H15A 106.8 . . ? C17 C15 H15A 106.8 . . ? C16 C15 H15A 106.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C30 C17 C18 117.5(3) . . ? C30 C17 C15 121.4(3) . . ? C18 C17 C15 121.0(3) . . ? O1 C18 C19 119.0(3) . . ? O1 C18 C17 118.9(3) . . ? C19 C18 C17 121.9(3) . . ? C24 C19 C18 116.2(3) . . ? C24 C19 C20 120.0(3) . . ? C18 C19 C20 123.8(3) . . ? C23 C20 C22 107.3(5) . . ? C23 C20 C21 108.7(4) . . ? C22 C20 C21 109.1(4) . . ? C23 C20 C19 111.3(4) . . ? C22 C20 C19 109.3(4) . . ? C21 C20 C19 110.9(4) . . ? 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 C19 124.4(3) . . ? C25 C24 H24A 117.8 . . ? C19 C24 H24A 117.8 . . ? C24 C25 C30 116.6(3) . . ? C24 C25 C26 121.6(3) . . ? C30 C25 C26 121.7(3) . . ? C27 C26 C29 107.9(6) . . ? C27 C26 C28 110.9(6) . . ? C29 C26 C28 105.7(5) . . ? C27 C26 C25 109.6(4) . . ? C29 C26 C25 112.3(4) . . ? C28 C26 C25 110.4(4) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 C17 122.7(3) . . ? C25 C30 H30A 118.6 . . ? C17 C30 H30A 118.6 . . ? O1 C31 H31A 109.5 . . ? O1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N1 C32 C33 110.4(3) . . ? N1 C32 H32A 109.6 . . ? C33 C32 H32A 109.6 . . ? N1 C32 H32B 109.6 . . ? C33 C32 H32B 109.6 . . ? H32A C32 H32B 108.1 . . ? N2 C33 C32 113.1(4) . . ? N2 C33 H33A 108.9 . . ? C32 C33 H33A 108.9 . . ? N2 C33 H33B 108.9 . . ? C32 C33 H33B 108.9 . . ? H33A C33 H33B 107.8 . . ? N2 C34 H34A 109.5 . . ? N2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N2 C35 H35A 109.5 . . ? N2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Cl2 C36 Cl1 118.2(5) . . ? Cl2 C36 H36A 107.8 . . ? Cl1 C36 H36A 107.8 . . ? Cl2 C36 H36B 107.8 . . ? Cl1 C36 H36B 107.8 . . ? H36A C36 H36B 107.1 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.394 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.051