# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_srzl1202 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H20 N2 O' _chemical_formula_sum 'C17 H20 N2 O' _chemical_formula_weight 268.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 '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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 6.0329(5) _cell_length_b 7.7817(7) _cell_length_c 9.0003(7) _cell_angle_alpha 115.116(8) _cell_angle_beta 101.212(7) _cell_angle_gamma 99.162(7) _cell_volume 361.11(5) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 2729 _cell_measurement_theta_min 3.5708 _cell_measurement_theta_max 29.3563 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 144 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_T_min 0.97992 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Xcalibur, Eos' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3468 _diffrn_reflns_av_R_equivalents 0.0087 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 29.42 _reflns_number_total 2806 _reflns_number_gt 2720 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _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. ; _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^)+(0.0366P)^2^+0.0746P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(11) _refine_ls_number_reflns 2806 _refine_ls_number_parameters 188 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0761 _refine_ls_wR_factor_gt 0.0750 _refine_ls_goodness_of_fit_ref 1.026 _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 O1 O 0.49270(18) 0.16209(14) 0.69448(12) 0.0219(2) Uani 1 1 d . . . N1 N 0.5647(2) 0.49289(17) 0.79221(15) 0.0194(3) Uani 1 1 d . . . N2 N 0.6871(2) 0.36751(16) 0.97841(14) 0.0181(3) Uani 1 1 d . . . C1 C 0.4290(2) 0.4935(2) 0.63629(17) 0.0173(3) Uani 1 1 d . . . C2 C 0.1704(3) 0.3941(3) 0.5927(2) 0.0292(4) Uani 1 1 d . . . H2A H 0.1111 0.4649 0.6890 0.044 Uiso 1 1 calc R . . H2B H 0.1508 0.2573 0.5710 0.044 Uiso 1 1 calc R . . H2C H 0.0823 0.3959 0.4899 0.044 Uiso 1 1 calc R . . C3 C 0.4633(3) 0.7092(2) 0.6821(2) 0.0273(3) Uani 1 1 d . . . H3A H 0.4043 0.7743 0.7800 0.041 Uiso 1 1 calc R . . H3B H 0.3768 0.7197 0.5835 0.041 Uiso 1 1 calc R . . H3C H 0.6308 0.7730 0.7123 0.041 Uiso 1 1 calc R . . C4 C 0.5251(3) 0.3924(2) 0.4861(2) 0.0279(4) Uani 1 1 d . . . H4A H 0.5140 0.2558 0.4626 0.042 Uiso 1 1 calc R . . H4B H 0.6898 0.4630 0.5151 0.042 Uiso 1 1 calc R . . H4C H 0.4333 0.3936 0.3841 0.042 Uiso 1 1 calc R . . C5 C 0.5725(2) 0.3315(2) 0.81142(17) 0.0176(3) Uani 1 1 d . . . C6 C 0.7062(2) 0.54237(19) 1.13058(16) 0.0152(3) Uani 1 1 d . . . C7 C 0.9158(3) 0.6341(2) 1.26331(17) 0.0173(3) Uani 1 1 d . . . H7A H 1.0471 0.5818 1.2518 0.021 Uiso 1 1 calc R . . C8 C 0.9339(3) 0.8018(2) 1.41252(18) 0.0195(3) Uani 1 1 d . . . H8A H 1.0771 0.8631 1.5030 0.023 Uiso 1 1 calc R . . C9 C 0.7434(3) 0.8801(2) 1.43004(17) 0.0201(3) Uani 1 1 d . . . H9A H 0.7562 0.9951 1.5320 0.024 Uiso 1 1 calc R . . C10 C 0.5355(3) 0.7898(2) 1.29840(19) 0.0203(3) Uani 1 1 d . . . H10A H 0.4058 0.8443 1.3098 0.024 Uiso 1 1 calc R . . C11 C 0.5136(3) 0.6197(2) 1.14901(18) 0.0189(3) Uani 1 1 d . . . H11A H 0.3686 0.5567 1.0603 0.023 Uiso 1 1 calc R . . C12 C 0.8157(2) 0.23262(18) 0.99246(16) 0.0160(3) Uani 1 1 d . . . C13 C 0.7825(3) 0.1501(2) 1.09928(17) 0.0191(3) Uani 1 1 d . . . H13A H 0.6694 0.1784 1.1599 0.023 Uiso 1 1 calc R . . C14 C 0.9157(3) 0.0263(2) 1.11672(18) 0.0227(3) Uani 1 1 d . . . H14A H 0.8950 -0.0288 1.1909 0.027 Uiso 1 1 calc R . . C15 C 1.0792(3) -0.0180(2) 1.02652(19) 0.0235(3) Uani 1 1 d . . . H15A H 1.1686 -0.1040 1.0381 0.028 Uiso 1 1 calc R . . C16 C 1.1114(3) 0.0637(2) 0.91955(19) 0.0219(3) Uani 1 1 d . . . H16A H 1.2227 0.0338 0.8575 0.026 Uiso 1 1 calc R . . C17 C 0.9808(3) 0.1891(2) 0.90370(17) 0.0176(3) Uani 1 1 d . . . H17A H 1.0041 0.2461 0.8313 0.021 Uiso 1 1 calc R . . H1A H 0.639(3) 0.604(3) 0.878(2) 0.022(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0295(6) 0.0147(5) 0.0162(5) 0.0043(4) 0.0024(4) 0.0064(4) N1 0.0261(7) 0.0129(6) 0.0136(6) 0.0043(5) -0.0003(5) 0.0039(5) N2 0.0266(7) 0.0141(6) 0.0135(5) 0.0055(4) 0.0035(5) 0.0104(5) C1 0.0193(7) 0.0190(7) 0.0139(6) 0.0083(5) 0.0028(5) 0.0064(5) C2 0.0209(8) 0.0381(10) 0.0313(9) 0.0218(7) 0.0026(7) 0.0051(7) C3 0.0380(10) 0.0222(8) 0.0249(8) 0.0138(6) 0.0064(7) 0.0121(7) C4 0.0363(9) 0.0332(9) 0.0224(7) 0.0156(7) 0.0132(7) 0.0181(7) C5 0.0185(7) 0.0178(7) 0.0160(6) 0.0070(5) 0.0045(5) 0.0070(6) C6 0.0201(7) 0.0124(6) 0.0132(6) 0.0062(5) 0.0052(5) 0.0040(5) C7 0.0194(7) 0.0171(7) 0.0174(6) 0.0092(5) 0.0055(5) 0.0072(5) C8 0.0216(7) 0.0172(7) 0.0147(6) 0.0061(5) 0.0001(5) 0.0027(5) C9 0.0284(8) 0.0156(7) 0.0155(7) 0.0054(5) 0.0093(6) 0.0059(6) C10 0.0205(7) 0.0191(7) 0.0230(7) 0.0089(6) 0.0102(6) 0.0077(6) C11 0.0179(7) 0.0172(7) 0.0184(7) 0.0066(5) 0.0040(6) 0.0032(5) C12 0.0202(7) 0.0115(6) 0.0132(6) 0.0041(5) 0.0024(5) 0.0045(5) C13 0.0230(7) 0.0187(7) 0.0147(6) 0.0069(5) 0.0065(6) 0.0050(6) C14 0.0312(9) 0.0184(7) 0.0189(7) 0.0105(6) 0.0041(6) 0.0064(6) C15 0.0272(8) 0.0192(7) 0.0232(7) 0.0098(6) 0.0019(6) 0.0114(6) C16 0.0192(7) 0.0223(7) 0.0218(7) 0.0072(6) 0.0065(6) 0.0079(6) C17 0.0210(7) 0.0157(6) 0.0153(6) 0.0075(5) 0.0046(5) 0.0036(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C5 1.2249(17) . ? N1 C5 1.3451(18) . ? N1 C1 1.4832(17) . ? N1 H1A 0.85(2) . ? N2 C5 1.4115(18) . ? N2 C6 1.4309(16) . ? N2 C12 1.4331(18) . ? C1 C3 1.516(2) . ? C1 C2 1.519(2) . ? C1 C4 1.5263(19) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C6 C7 1.3919(19) . ? C6 C11 1.3974(19) . ? C7 C8 1.3886(19) . ? C7 H7A 0.9500 . ? C8 C9 1.388(2) . ? C8 H8A 0.9500 . ? C9 C10 1.381(2) . ? C9 H9A 0.9500 . ? C10 C11 1.394(2) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 C17 1.3896(19) . ? C12 C13 1.3908(18) . ? C13 C14 1.388(2) . ? C13 H13A 0.9500 . ? C14 C15 1.390(2) . ? C14 H14A 0.9500 . ? C15 C16 1.386(2) . ? C15 H15A 0.9500 . ? C16 C17 1.383(2) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? 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 C5 N1 C1 125.53(12) . . ? C5 N1 H1A 117.3(13) . . ? C1 N1 H1A 117.1(13) . . ? C5 N2 C6 123.53(12) . . ? C5 N2 C12 117.19(11) . . ? C6 N2 C12 118.77(11) . . ? N1 C1 C3 105.49(11) . . ? N1 C1 C2 110.14(12) . . ? C3 C1 C2 109.93(13) . . ? N1 C1 C4 110.50(12) . . ? C3 C1 C4 109.65(12) . . ? C2 C1 C4 110.99(13) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O1 C5 N1 124.20(13) . . ? O1 C5 N2 120.18(13) . . ? N1 C5 N2 115.60(12) . . ? C7 C6 C11 119.49(12) . . ? C7 C6 N2 120.05(13) . . ? C11 C6 N2 120.45(12) . . ? C8 C7 C6 120.26(13) . . ? C8 C7 H7A 119.9 . . ? C6 C7 H7A 119.9 . . ? C9 C8 C7 120.28(14) . . ? C9 C8 H8A 119.9 . . ? C7 C8 H8A 119.9 . . ? C10 C9 C8 119.60(13) . . ? C10 C9 H9A 120.2 . . ? C8 C9 H9A 120.2 . . ? C9 C10 C11 120.78(14) . . ? C9 C10 H10A 119.6 . . ? C11 C10 H10A 119.6 . . ? C10 C11 C6 119.58(13) . . ? C10 C11 H11A 120.2 . . ? C6 C11 H11A 120.2 . . ? C17 C12 C13 119.64(13) . . ? C17 C12 N2 119.93(12) . . ? C13 C12 N2 120.39(12) . . ? C14 C13 C12 119.55(13) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? C13 C14 C15 120.52(14) . . ? C13 C14 H14A 119.7 . . ? C15 C14 H14A 119.7 . . ? C16 C15 C14 119.85(14) . . ? C16 C15 H15A 120.1 . . ? C14 C15 H15A 120.1 . . ? C17 C16 C15 119.65(14) . . ? C17 C16 H16A 120.2 . . ? C15 C16 H16A 120.2 . . ? C16 C17 C12 120.77(13) . . ? C16 C17 H17A 119.6 . . ? C12 C17 H17A 119.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 C1 C3 176.17(13) . . . . ? C5 N1 C1 C2 57.59(18) . . . . ? C5 N1 C1 C4 -65.40(18) . . . . ? C1 N1 C5 O1 10.0(2) . . . . ? C1 N1 C5 N2 -171.75(13) . . . . ? C6 N2 C5 O1 -155.53(13) . . . . ? C12 N2 C5 O1 32.7(2) . . . . ? C6 N2 C5 N1 26.1(2) . . . . ? C12 N2 C5 N1 -145.63(12) . . . . ? C5 N2 C6 C7 -138.64(14) . . . . ? C12 N2 C6 C7 32.97(19) . . . . ? C5 N2 C6 C11 42.9(2) . . . . ? C12 N2 C6 C11 -145.51(13) . . . . ? C11 C6 C7 C8 -0.3(2) . . . . ? N2 C6 C7 C8 -178.82(13) . . . . ? C6 C7 C8 C9 -0.5(2) . . . . ? C7 C8 C9 C10 0.3(2) . . . . ? C8 C9 C10 C11 0.8(2) . . . . ? C9 C10 C11 C6 -1.6(2) . . . . ? C7 C6 C11 C10 1.3(2) . . . . ? N2 C6 C11 C10 179.81(13) . . . . ? C5 N2 C12 C17 51.86(18) . . . . ? C6 N2 C12 C17 -120.28(14) . . . . ? C5 N2 C12 C13 -130.42(14) . . . . ? C6 N2 C12 C13 57.44(18) . . . . ? C17 C12 C13 C14 0.4(2) . . . . ? N2 C12 C13 C14 -177.32(13) . . . . ? C12 C13 C14 C15 -0.9(2) . . . . ? C13 C14 C15 C16 0.7(2) . . . . ? C14 C15 C16 C17 0.1(2) . . . . ? C15 C16 C17 C12 -0.6(2) . . . . ? C13 C12 C17 C16 0.4(2) . . . . ? N2 C12 C17 C16 178.11(13) . . . . ? _diffrn_measured_fraction_theta_max 0.873 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.234 _refine_diff_density_min -0.175 _refine_diff_density_rms 0.034 _database_code_depnum_ccdc_archive 'CCDC 940855' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_srzl1108 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H46 Mg N3 Na O2' _chemical_formula_weight 696.14 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' Na Na 0.0362 0.0249 '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 'P 21/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 9.4286(3) _cell_length_b 39.1553(19) _cell_length_c 10.2035(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.029(3) _cell_angle_gamma 90.00 _cell_volume 3738.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 7930 _cell_measurement_theta_min 2.8883 _cell_measurement_theta_max 29.4150 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.101 _exptl_absorpt_correction_T_min 0.94142 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Xcalibur, Eos' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20985 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 50 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 27.00 _reflns_number_total 8131 _reflns_number_gt 6036 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _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. ; _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^)+(0.0353P)^2^+2.4145P] 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 8131 _refine_ls_number_parameters 476 _refine_ls_number_restraints 91 _refine_ls_R_factor_all 0.0784 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1201 _refine_ls_wR_factor_gt 0.1090 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.033 _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 0.75722(7) 0.109246(17) 0.09403(6) 0.02235(15) Uani 1 1 d . . . Na1 Na 0.92702(9) 0.15848(2) 0.53336(8) 0.0356(2) Uani 1 1 d . . . N1 N 0.80178(17) 0.10410(4) -0.09696(15) 0.0245(4) Uani 1 1 d . . . C1 C 0.7120(2) 0.08234(5) -0.18054(17) 0.0234(4) Uani 1 1 d . . . C2 C 0.5657(2) 0.08989(6) -0.20518(18) 0.0273(4) Uani 1 1 d . . . H2A H 0.5306 0.1101 -0.1691 0.033 Uiso 1 1 calc R . . C3 C 0.4712(2) 0.06859(6) -0.28066(19) 0.0351(5) Uani 1 1 d . . . H3A H 0.3724 0.0742 -0.2947 0.042 Uiso 1 1 calc R . . C4 C 0.5196(3) 0.03919(6) -0.3359(2) 0.0389(6) Uani 1 1 d . . . H4A H 0.4551 0.0247 -0.3888 0.047 Uiso 1 1 calc R . . C5 C 0.6633(3) 0.03124(6) -0.3126(2) 0.0367(5) Uani 1 1 d . . . H5A H 0.6976 0.0112 -0.3507 0.044 Uiso 1 1 calc R . . C6 C 0.7582(2) 0.05201(5) -0.23484(19) 0.0292(5) Uani 1 1 d . . . H6A H 0.8560 0.0456 -0.2180 0.035 Uiso 1 1 calc R . . C7 C 0.9300(2) 0.11452(5) -0.13586(18) 0.0248(4) Uani 1 1 d . . . C8 C 0.9782(2) 0.10814(5) -0.25998(19) 0.0291(5) Uani 1 1 d . . . H8A H 0.9195 0.0953 -0.3244 0.035 Uiso 1 1 calc R . . C9 C 1.1089(2) 0.12021(6) -0.2894(2) 0.0365(5) Uani 1 1 d . . . H9A H 1.1387 0.1149 -0.3727 0.044 Uiso 1 1 calc R . . C10 C 1.1970(2) 0.13977(6) -0.2010(2) 0.0394(6) Uani 1 1 d . . . H10A H 1.2859 0.1481 -0.2227 0.047 Uiso 1 1 calc R . . C11 C 1.1515(2) 0.14689(6) -0.0794(2) 0.0374(5) Uani 1 1 d . . . H11A H 1.2102 0.1604 -0.0170 0.045 Uiso 1 1 calc R . . C12 C 1.0227(2) 0.13472(6) -0.0479(2) 0.0312(5) Uani 1 1 d . . . H12A H 0.9951 0.1401 0.0362 0.037 Uiso 1 1 calc R . . N2 N 0.91756(17) 0.08941(4) 0.22679(15) 0.0252(4) Uani 1 1 d . A . C13 C 0.9068(2) 0.05354(5) 0.23937(19) 0.0259(4) Uani 1 1 d . . . C14 C 0.9073(2) 0.03277(6) 0.1287(2) 0.0299(5) Uani 1 1 d . . . H14A H 0.9220 0.0427 0.0465 0.036 Uiso 1 1 calc R . . C15 C 0.8868(2) -0.00217(6) 0.1368(2) 0.0373(5) Uani 1 1 d . . . H15A H 0.8878 -0.0159 0.0602 0.045 Uiso 1 1 calc R . . C16 C 0.8648(2) -0.01713(6) 0.2550(3) 0.0401(6) Uani 1 1 d . . . H16A H 0.8500 -0.0411 0.2601 0.048 Uiso 1 1 calc R . . C17 C 0.8645(2) 0.00319(6) 0.3664(2) 0.0393(5) Uani 1 1 d . . . H17A H 0.8502 -0.0070 0.4483 0.047 Uiso 1 1 calc R . . C18 C 0.8849(2) 0.03797(6) 0.3592(2) 0.0332(5) Uani 1 1 d . . . H18A H 0.8841 0.0516 0.4363 0.040 Uiso 1 1 calc R . . C19 C 1.0322(2) 0.10531(5) 0.29644(17) 0.0249(4) Uani 1 1 d . . . C20 C 1.1561(2) 0.08810(6) 0.35682(18) 0.0282(4) Uani 1 1 d . A . H20A H 1.1571 0.0638 0.3586 0.034 Uiso 1 1 calc R . . C21 C 1.2752(2) 0.10584(6) 0.41306(18) 0.0314(5) Uani 1 1 d . . . H21A H 1.3568 0.0934 0.4510 0.038 Uiso 1 1 calc R A . C22 C 1.2787(2) 0.14113(6) 0.4155(2) 0.0334(5) Uani 1 1 d . A . H22A H 1.3614 0.1531 0.4535 0.040 Uiso 1 1 calc R . . C23 C 1.1576(2) 0.15860(6) 0.3608(2) 0.0329(5) Uani 1 1 d . A . H23 H 1.1574 0.1829 0.3623 0.039 Uiso 1 1 calc R . . C24 C 1.0368(2) 0.14139(6) 0.30382(19) 0.0287(5) Uani 1 1 d . A . H24 H 0.9550 0.1542 0.2689 0.034 Uiso 1 1 calc R . . N3 N 0.68326(17) 0.15428(4) 0.16550(14) 0.0229(3) Uani 1 1 d . A . C25 C 0.6659(2) 0.15654(5) 0.29893(17) 0.0219(4) Uani 1 1 d . . . C26 C 0.6527(2) 0.18753(5) 0.36742(19) 0.0292(5) Uani 1 1 d . A . H26A H 0.6530 0.2085 0.3209 0.035 Uiso 1 1 calc R . . C27 C 0.6393(2) 0.18785(6) 0.5017(2) 0.0345(5) Uani 1 1 d . A . H27A H 0.6226 0.2101 0.5456 0.041 Uiso 1 1 calc R . . C28 C 0.6418(2) 0.15800(6) 0.57474(19) 0.0330(5) Uani 1 1 d . A . H28A H 0.6145 0.1582 0.6664 0.040 Uiso 1 1 calc R . . C29 C 0.6577(2) 0.12726(5) 0.50992(18) 0.0268(4) Uani 1 1 d . A . H29A H 0.6457 0.1053 0.5575 0.032 Uiso 1 1 calc R . . C30 C 0.6700(2) 0.12652(5) 0.37589(18) 0.0234(4) Uani 1 1 d . A . H30A H 0.6811 0.1040 0.3322 0.028 Uiso 1 1 calc R . . C31 C 0.6224(2) 0.17954(5) 0.07901(18) 0.0252(4) Uani 1 1 d . . . C32 C 0.4919(2) 0.19584(6) 0.0917(2) 0.0357(5) Uani 1 1 d . A . H32A H 0.4438 0.1910 0.1660 0.043 Uiso 1 1 calc R . . C33 C 0.4322(3) 0.21892(7) -0.0026(3) 0.0491(6) Uani 1 1 d . . . H33A H 0.3447 0.2299 0.0092 0.059 Uiso 1 1 calc R A . C34 C 0.4975(3) 0.22623(6) -0.1131(2) 0.0485(7) Uani 1 1 d . A . H34A H 0.4561 0.2421 -0.1772 0.058 Uiso 1 1 calc R . . C35 C 0.6240(3) 0.21005(6) -0.1282(2) 0.0440(6) Uani 1 1 d . . . H35A H 0.6696 0.2147 -0.2043 0.053 Uiso 1 1 calc R A . C36 C 0.6862(3) 0.18712(5) -0.03483(19) 0.0334(5) Uani 1 1 d . A . H36A H 0.7737 0.1764 -0.0481 0.040 Uiso 1 1 calc R . . O1 O 0.57306(14) 0.08195(3) 0.10391(12) 0.0239(3) Uani 1 1 d . . . C37 C 0.4353(2) 0.09992(5) 0.09760(19) 0.0258(4) Uani 1 1 d . . . H37A H 0.4297 0.1184 0.0310 0.031 Uiso 1 1 calc R . . H37B H 0.4227 0.1100 0.1845 0.031 Uiso 1 1 calc R . . C38 C 0.3229(2) 0.07310(5) 0.0590(2) 0.0298(5) Uani 1 1 d . . . H38A H 0.3038 0.0707 -0.0381 0.036 Uiso 1 1 calc R . . H38B H 0.2324 0.0785 0.0947 0.036 Uiso 1 1 calc R . . C39 C 0.3927(2) 0.04119(6) 0.1227(2) 0.0346(5) Uani 1 1 d . . . H39A H 0.3841 0.0404 0.2184 0.042 Uiso 1 1 calc R . . H39B H 0.3498 0.0202 0.0804 0.042 Uiso 1 1 calc R . . C40 C 0.5467(2) 0.04525(5) 0.0980(2) 0.0310(5) Uani 1 1 d . . . H40A H 0.6115 0.0332 0.1665 0.037 Uiso 1 1 calc R . . H40B H 0.5612 0.0360 0.0103 0.037 Uiso 1 1 calc R . . O2 O 0.9941(9) 0.21378(14) 0.5858(5) 0.0532(10) Uani 0.731(3) 1 d PDU A 1 C41 C 0.9126(5) 0.24441(9) 0.5791(5) 0.0739(13) Uani 0.731(3) 1 d PDU A 1 H41A H 0.8338 0.2423 0.6345 0.089 Uiso 0.731(3) 1 calc PR A 1 H41B H 0.8705 0.2487 0.4869 0.089 Uiso 0.731(3) 1 calc PR A 1 C42 C 1.0071(7) 0.27269(15) 0.6266(7) 0.0793(17) Uani 0.731(3) 1 d PDU A 1 H42A H 0.9577 0.2888 0.6804 0.095 Uiso 0.731(3) 1 calc PR A 1 H42B H 1.0406 0.2852 0.5520 0.095 Uiso 0.731(3) 1 calc PR A 1 C43 C 1.1312(5) 0.25518(10) 0.7102(5) 0.0709(12) Uani 0.731(3) 1 d PDU A 1 H43A H 1.2209 0.2683 0.7101 0.085 Uiso 0.731(3) 1 calc PR A 1 H43B H 1.1110 0.2521 0.8024 0.085 Uiso 0.731(3) 1 calc PR A 1 C44 C 1.1397(4) 0.22158(10) 0.6417(5) 0.0737(12) Uani 0.731(3) 1 d PDU A 1 H44A H 1.2030 0.2232 0.5713 0.088 Uiso 0.731(3) 1 calc PR A 1 H44B H 1.1772 0.2037 0.7052 0.088 Uiso 0.731(3) 1 calc PR A 1 O2A O 1.006(3) 0.2092(4) 0.6031(15) 0.0532(10) Uani 0.27 1 d PDU A 2 C41A C 1.0178(14) 0.2401(3) 0.5263(12) 0.0739(13) Uani 0.27 1 d PDU A 2 H41C H 0.9301 0.2437 0.4638 0.089 Uiso 0.269(3) 1 calc PR A 2 H41D H 1.1009 0.2388 0.4756 0.089 Uiso 0.269(3) 1 calc PR A 2 C42A C 1.037(2) 0.2686(4) 0.6271(18) 0.0793(17) Uani 0.27 1 d PDU A 2 H42C H 1.0019 0.2906 0.5879 0.095 Uiso 0.269(3) 1 calc PR A 2 H42D H 1.1393 0.2712 0.6631 0.095 Uiso 0.269(3) 1 calc PR A 2 C44A C 0.9952(12) 0.2197(2) 0.7398(13) 0.0737(12) Uani 0.27 1 d PDU A 2 H44C H 1.0887 0.2172 0.7949 0.088 Uiso 0.269(3) 1 calc PR A 2 H44D H 0.9238 0.2055 0.7783 0.088 Uiso 0.269(3) 1 calc PR A 2 C43A C 0.9487(12) 0.2571(2) 0.7336(12) 0.0709(12) Uani 0.27 1 d PDU A 2 H43C H 0.8448 0.2597 0.7060 0.085 Uiso 0.269(3) 1 calc PR A 2 H43D H 0.9757 0.2692 0.8183 0.085 Uiso 0.269(3) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0222(3) 0.0268(4) 0.0182(3) 0.0018(3) 0.0030(3) 0.0017(3) Na1 0.0393(5) 0.0298(5) 0.0370(5) 0.0018(4) 0.0023(4) -0.0038(4) N1 0.0211(8) 0.0330(10) 0.0197(7) 0.0020(7) 0.0039(6) 0.0016(7) C1 0.0234(10) 0.0317(11) 0.0157(8) 0.0062(7) 0.0045(8) 0.0017(9) C2 0.0256(10) 0.0392(12) 0.0175(9) 0.0066(8) 0.0044(8) 0.0031(9) C3 0.0254(11) 0.0559(15) 0.0238(10) 0.0083(10) 0.0021(9) -0.0050(11) C4 0.0393(13) 0.0505(15) 0.0265(11) 0.0000(10) 0.0021(10) -0.0138(12) C5 0.0497(14) 0.0328(12) 0.0292(11) 0.0001(9) 0.0114(10) -0.0040(11) C6 0.0302(11) 0.0326(12) 0.0256(10) 0.0052(8) 0.0068(9) 0.0054(9) C7 0.0214(10) 0.0292(11) 0.0242(9) 0.0077(8) 0.0040(8) 0.0063(9) C8 0.0295(11) 0.0338(12) 0.0251(10) 0.0071(8) 0.0079(9) 0.0067(10) C9 0.0329(12) 0.0438(14) 0.0358(12) 0.0141(10) 0.0159(10) 0.0143(11) C10 0.0227(11) 0.0461(14) 0.0519(14) 0.0194(11) 0.0140(11) 0.0040(10) C11 0.0262(11) 0.0410(14) 0.0438(13) 0.0081(10) -0.0007(10) -0.0020(10) C12 0.0272(11) 0.0379(13) 0.0289(10) 0.0044(9) 0.0047(9) 0.0016(10) N2 0.0243(9) 0.0290(9) 0.0217(8) 0.0006(7) -0.0001(7) 0.0033(7) C13 0.0200(10) 0.0301(11) 0.0269(10) 0.0025(8) 0.0004(8) 0.0057(9) C14 0.0230(10) 0.0370(12) 0.0299(10) -0.0016(9) 0.0041(9) 0.0067(9) C15 0.0265(11) 0.0360(13) 0.0493(13) -0.0092(10) 0.0043(10) 0.0058(10) C16 0.0250(11) 0.0294(12) 0.0658(16) 0.0022(11) 0.0052(11) 0.0014(10) C17 0.0349(12) 0.0397(14) 0.0430(13) 0.0137(10) 0.0034(10) -0.0007(11) C18 0.0336(12) 0.0377(13) 0.0277(10) 0.0022(9) 0.0007(9) 0.0007(10) C19 0.0230(10) 0.0357(12) 0.0166(8) 0.0014(8) 0.0055(8) 0.0015(9) C20 0.0264(10) 0.0366(12) 0.0221(9) 0.0040(8) 0.0049(8) 0.0046(9) C21 0.0228(10) 0.0492(14) 0.0225(10) 0.0054(9) 0.0037(8) 0.0038(10) C22 0.0213(10) 0.0519(15) 0.0271(10) 0.0013(10) 0.0030(9) -0.0058(10) C23 0.0314(11) 0.0351(12) 0.0326(11) -0.0001(9) 0.0052(9) -0.0036(10) C24 0.0229(10) 0.0352(12) 0.0276(10) 0.0025(9) 0.0014(8) 0.0042(9) N3 0.0251(8) 0.0245(9) 0.0190(7) 0.0027(6) 0.0025(7) 0.0011(7) C25 0.0194(9) 0.0251(10) 0.0206(9) 0.0007(7) 0.0001(7) 0.0001(8) C26 0.0356(12) 0.0244(11) 0.0271(10) 0.0008(8) 0.0019(9) 0.0017(9) C27 0.0429(13) 0.0320(12) 0.0281(10) -0.0075(9) 0.0026(10) 0.0036(10) C28 0.0375(12) 0.0412(13) 0.0206(9) -0.0026(9) 0.0044(9) 0.0010(11) C29 0.0247(10) 0.0330(11) 0.0221(9) 0.0027(8) 0.0005(8) -0.0013(9) C30 0.0233(10) 0.0251(10) 0.0216(9) 0.0011(8) 0.0022(8) 0.0020(8) C31 0.0310(11) 0.0215(10) 0.0218(9) 0.0011(8) -0.0025(8) -0.0038(9) C32 0.0307(12) 0.0363(13) 0.0386(12) 0.0090(10) -0.0022(10) 0.0013(10) C33 0.0390(14) 0.0418(15) 0.0620(16) 0.0147(12) -0.0119(12) 0.0064(12) C34 0.0612(17) 0.0364(14) 0.0413(13) 0.0159(11) -0.0211(12) -0.0052(13) C35 0.0753(19) 0.0306(13) 0.0244(11) 0.0051(9) -0.0008(11) -0.0098(13) C36 0.0479(14) 0.0267(11) 0.0254(10) 0.0027(8) 0.0042(9) -0.0016(10) O1 0.0232(7) 0.0244(7) 0.0244(7) 0.0000(5) 0.0039(6) 0.0008(6) C37 0.0221(10) 0.0291(11) 0.0268(10) 0.0002(8) 0.0052(8) 0.0042(9) C38 0.0271(11) 0.0320(12) 0.0305(10) -0.0005(9) 0.0040(9) -0.0012(9) C39 0.0318(12) 0.0318(12) 0.0405(12) 0.0027(9) 0.0055(10) -0.0034(10) C40 0.0321(12) 0.0242(11) 0.0369(11) 0.0009(9) 0.0057(9) 0.0002(9) O2 0.0513(19) 0.0249(19) 0.0783(19) -0.0043(13) -0.0124(17) 0.0001(15) C41 0.058(2) 0.036(2) 0.119(3) -0.015(2) -0.020(2) 0.0046(19) C42 0.074(4) 0.035(2) 0.120(3) -0.0106(19) -0.022(3) 0.004(2) C43 0.063(2) 0.052(2) 0.090(3) -0.013(2) -0.019(2) -0.0035(19) C44 0.058(2) 0.036(2) 0.118(3) -0.011(2) -0.024(2) -0.0029(18) O2A 0.0513(19) 0.0249(19) 0.0783(19) -0.0043(13) -0.0124(17) 0.0001(15) C41A 0.058(2) 0.036(2) 0.119(3) -0.015(2) -0.020(2) 0.0046(19) C42A 0.074(4) 0.035(2) 0.120(3) -0.0106(19) -0.022(3) 0.004(2) C44A 0.058(2) 0.036(2) 0.118(3) -0.011(2) -0.024(2) -0.0029(18) C43A 0.063(2) 0.052(2) 0.090(3) -0.013(2) -0.019(2) -0.0035(19) _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 2.0510(14) . ? Mg1 N1 2.0527(16) . ? Mg1 N2 2.0542(17) . ? Mg1 N3 2.0612(17) . ? Na1 O2A 2.207(19) . ? Na1 O2 2.300(6) . ? Na1 C24 2.756(2) . ? Na1 C28 2.772(2) . ? Na1 C9 2.774(2) 1_556 ? Na1 C29 2.801(2) . ? Na1 C8 2.883(2) 1_556 ? Na1 C27 2.927(2) . ? Na1 C23 2.959(2) . ? Na1 C30 3.010(2) . ? Na1 C26 3.126(2) . ? N1 C7 1.379(2) . ? N1 C1 1.412(2) . ? C1 C6 1.402(3) . ? C1 C2 1.402(3) . ? C2 C3 1.383(3) . ? C2 H2A 0.9500 . ? C3 C4 1.383(3) . ? C3 H3A 0.9500 . ? C4 C5 1.382(3) . ? C4 H4A 0.9500 . ? C5 C6 1.384(3) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C12 1.415(3) . ? C7 C8 1.419(3) . ? C8 C9 1.386(3) . ? C8 Na1 2.883(2) 1_554 ? C8 H8A 0.9500 . ? C9 C10 1.380(3) . ? C9 Na1 2.774(2) 1_554 ? C9 H9A 0.9500 . ? C10 C11 1.389(3) . ? C10 H10A 0.9500 . ? C11 C12 1.378(3) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? N2 C19 1.369(2) . ? N2 C13 1.415(3) . ? C13 C14 1.392(3) . ? C13 C18 1.404(3) . ? C14 C15 1.385(3) . ? C14 H14A 0.9500 . ? C15 C16 1.379(3) . ? C15 H15A 0.9500 . ? C16 C17 1.387(3) . ? C16 H16A 0.9500 . ? C17 C18 1.378(3) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C24 1.415(3) . ? C19 C20 1.421(3) . ? C20 C21 1.384(3) . ? C20 H20A 0.9500 . ? C21 C22 1.382(3) . ? C21 H21A 0.9500 . ? C22 C23 1.387(3) . ? C22 H22A 0.9500 . ? C23 C24 1.388(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? N3 C25 1.394(2) . ? N3 C31 1.401(2) . ? C25 C30 1.411(3) . ? C25 C26 1.413(3) . ? C26 C27 1.392(3) . ? C26 H26A 0.9500 . ? C27 C28 1.384(3) . ? C27 H27A 1.0000 . ? C28 C29 1.390(3) . ? C28 H28A 1.0000 . ? C29 C30 1.387(2) . ? C29 H29A 1.0000 . ? C30 H30A 1.0000 . ? C31 C36 1.404(3) . ? C31 C32 1.405(3) . ? C32 C33 1.388(3) . ? C32 H32A 0.9500 . ? C33 C34 1.378(4) . ? C33 H33A 0.9500 . ? C34 C35 1.375(4) . ? C34 H34A 0.9500 . ? C35 C36 1.386(3) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? O1 C40 1.458(2) . ? O1 C37 1.471(2) . ? C37 C38 1.509(3) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.520(3) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.512(3) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? O2 C41 1.421(6) . ? O2 C44 1.452(8) . ? C41 C42 1.465(6) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.524(7) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.496(5) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? O2A C41A 1.454(10) . ? O2A C44A 1.469(10) . ? C41A C42A 1.513(10) . ? C41A H41C 0.9900 . ? C41A H41D 0.9900 . ? C42A C43A 1.518(10) . ? C42A H42C 0.9900 . ? C42A H42D 0.9900 . ? C44A C43A 1.529(8) . ? C44A H44C 0.9900 . ? C44A H44D 0.9900 . ? C43A H43C 0.9900 . ? C43A H43D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mg1 N1 105.55(6) . . ? O1 Mg1 N2 109.22(7) . . ? N1 Mg1 N2 111.68(7) . . ? O1 Mg1 N3 95.93(6) . . ? N1 Mg1 N3 122.48(7) . . ? N2 Mg1 N3 110.08(7) . . ? O2A Na1 O2 6.4(6) . . ? O2A Na1 C24 110.2(5) . . ? O2 Na1 C24 107.77(17) . . ? O2A Na1 C28 104.7(6) . . ? O2 Na1 C28 102.4(2) . . ? C24 Na1 C28 126.84(7) . . ? O2A Na1 C9 96.8(5) . 1_556 ? O2 Na1 C9 103.07(17) . 1_556 ? C24 Na1 C9 99.01(7) . 1_556 ? C28 Na1 C9 115.50(7) . 1_556 ? O2A Na1 C29 133.4(6) . . ? O2 Na1 C29 130.6(2) . . ? C24 Na1 C29 104.59(6) . . ? C28 Na1 C29 28.88(6) . . ? C9 Na1 C29 107.54(7) 1_556 . ? O2A Na1 C8 111.0(4) . 1_556 ? O2 Na1 C8 117.15(14) . 1_556 ? C24 Na1 C8 114.14(7) . 1_556 ? C28 Na1 C8 87.85(6) . 1_556 ? C9 Na1 C8 28.29(6) 1_556 1_556 ? C29 Na1 C8 80.38(6) . 1_556 ? O2A Na1 C27 87.4(6) . . ? O2 Na1 C27 83.1(2) . . ? C24 Na1 C27 116.15(6) . . ? C28 Na1 C27 27.95(6) . . ? C9 Na1 C27 140.75(7) 1_556 . ? C29 Na1 C27 49.02(6) . . ? C8 Na1 C27 114.77(6) 1_556 . ? O2A Na1 C23 86.9(5) . . ? O2 Na1 C23 86.32(19) . . ? C24 Na1 C23 27.82(6) . . ? C28 Na1 C23 152.51(7) . . ? C9 Na1 C23 87.04(6) 1_556 . ? C29 Na1 C23 132.35(6) . . ? C8 Na1 C23 111.52(6) 1_556 . ? C27 Na1 C23 132.20(7) . . ? O2A Na1 C30 139.8(6) . . ? O2 Na1 C30 134.09(18) . . ? C24 Na1 C30 78.85(6) . . ? C28 Na1 C30 49.19(6) . . ? C9 Na1 C30 121.08(7) 1_556 . ? C29 Na1 C30 27.31(5) . . ? C8 Na1 C30 99.09(6) 1_556 . ? C27 Na1 C30 55.27(6) . . ? C23 Na1 C30 106.53(6) . . ? O2A Na1 C26 94.1(6) . . ? O2 Na1 C26 88.24(18) . . ? C24 Na1 C26 89.97(6) . . ? C28 Na1 C26 48.07(6) . . ? C9 Na1 C26 162.50(7) 1_556 . ? C29 Na1 C26 55.37(6) . . ? C8 Na1 C26 134.26(6) 1_556 . ? C27 Na1 C26 26.32(5) . . ? C23 Na1 C26 107.22(6) . . ? C30 Na1 C26 45.89(5) . . ? C7 N1 C1 119.11(15) . . ? C7 N1 Mg1 122.17(13) . . ? C1 N1 Mg1 117.10(11) . . ? C6 C1 C2 116.99(19) . . ? C6 C1 N1 123.88(18) . . ? C2 C1 N1 119.00(18) . . ? C3 C2 C1 121.6(2) . . ? C3 C2 H2A 119.2 . . ? C1 C2 H2A 119.2 . . ? C4 C3 C2 120.4(2) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C5 C4 C3 118.8(2) . . ? C5 C4 H4A 120.6 . . ? C3 C4 H4A 120.6 . . ? C4 C5 C6 121.1(2) . . ? C4 C5 H5A 119.4 . . ? C6 C5 H5A 119.4 . . ? C5 C6 C1 120.9(2) . . ? C5 C6 H6A 119.5 . . ? C1 C6 H6A 119.5 . . ? N1 C7 C12 118.54(17) . . ? N1 C7 C8 126.31(19) . . ? C12 C7 C8 115.10(18) . . ? C9 C8 C7 121.6(2) . . ? C9 C8 Na1 71.47(12) . 1_554 ? C7 C8 Na1 119.29(13) . 1_554 ? C9 C8 H8A 119.2 . . ? C7 C8 H8A 119.2 . . ? Na1 C8 H8A 79.9 1_554 . ? C10 C9 C8 121.8(2) . . ? C10 C9 Na1 113.60(15) . 1_554 ? C8 C9 Na1 80.24(13) . 1_554 ? C10 C9 H9A 119.1 . . ? C8 C9 H9A 119.1 . . ? Na1 C9 H9A 76.3 1_554 . ? C9 C10 C11 117.9(2) . . ? C9 C10 H10A 121.0 . . ? C11 C10 H10A 121.0 . . ? C12 C11 C10 121.0(2) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C11 C12 C7 122.58(19) . . ? C11 C12 H12A 118.7 . . ? C7 C12 H12A 118.7 . . ? C19 N2 C13 117.72(16) . . ? C19 N2 Mg1 129.86(14) . . ? C13 N2 Mg1 112.33(12) . . ? C14 C13 C18 117.9(2) . . ? C14 C13 N2 119.92(18) . . ? C18 C13 N2 121.99(18) . . ? C15 C14 C13 120.9(2) . . ? C15 C14 H14A 119.5 . . ? C13 C14 H14A 119.5 . . ? C16 C15 C14 120.5(2) . . ? C16 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? C15 C16 C17 119.2(2) . . ? C15 C16 H16A 120.4 . . ? C17 C16 H16A 120.4 . . ? C18 C17 C16 120.6(2) . . ? C18 C17 H17A 119.7 . . ? C16 C17 H17A 119.7 . . ? C17 C18 C13 120.7(2) . . ? C17 C18 H18A 119.6 . . ? C13 C18 H18A 119.6 . . ? N2 C19 C24 119.90(18) . . ? N2 C19 C20 124.33(19) . . ? C24 C19 C20 115.63(19) . . ? C21 C20 C19 121.6(2) . . ? C21 C20 H20A 119.2 . . ? C19 C20 H20A 119.2 . . ? C22 C21 C20 121.7(2) . . ? C22 C21 H21A 119.2 . . ? C20 C21 H21A 119.2 . . ? C21 C22 C23 118.0(2) . . ? C21 C22 H22A 121.0 . . ? C23 C22 H22A 121.0 . . ? C22 C23 C24 121.4(2) . . ? C22 C23 Na1 112.79(13) . . ? C24 C23 Na1 67.90(11) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? Na1 C23 H23 89.4 . . ? C23 C24 C19 121.6(2) . . ? C23 C24 Na1 84.28(12) . . ? C19 C24 Na1 106.00(12) . . ? C23 C24 H24 119.2 . . ? C19 C24 H24 119.2 . . ? Na1 C24 H24 79.6 . . ? C25 N3 C31 118.84(16) . . ? C25 N3 Mg1 119.02(12) . . ? C31 N3 Mg1 120.74(12) . . ? N3 C25 C30 119.48(17) . . ? N3 C25 C26 124.44(17) . . ? C30 C25 C26 115.96(16) . . ? C27 C26 C25 121.25(19) . . ? C27 C26 Na1 68.82(12) . . ? C25 C26 Na1 80.70(12) . . ? C27 C26 H26A 119.4 . . ? C25 C26 H26A 119.4 . . ? Na1 C26 H26A 122.2 . . ? C28 C27 C26 121.64(19) . . ? C28 C27 Na1 69.80(13) . . ? C26 C27 Na1 84.86(13) . . ? C28 C27 H27A 119.1 . . ? C26 C27 H27A 119.1 . . ? Na1 C27 H27A 119.1 . . ? C27 C28 C29 118.07(18) . . ? C27 C28 Na1 82.25(13) . . ? C29 C28 Na1 76.72(12) . . ? C27 C28 H28A 120.5 . . ? C29 C28 H28A 120.5 . . ? Na1 C28 H28A 120.5 . . ? C30 C29 C28 120.94(19) . . ? C30 C29 Na1 84.76(12) . . ? C28 C29 Na1 74.40(12) . . ? C30 C29 H29A 119.2 . . ? C28 C29 H29A 119.2 . . ? Na1 C29 H29A 119.2 . . ? C29 C30 C25 122.10(18) . . ? C29 C30 Na1 67.93(11) . . ? C25 C30 Na1 85.22(12) . . ? C29 C30 H30A 118.9 . . ? C25 C30 H30A 118.9 . . ? Na1 C30 H30A 118.9 . . ? N3 C31 C36 119.09(18) . . ? N3 C31 C32 123.95(17) . . ? C36 C31 C32 116.66(19) . . ? C33 C32 C31 121.1(2) . . ? C33 C32 H32A 119.4 . . ? C31 C32 H32A 119.4 . . ? C34 C33 C32 121.2(2) . . ? C34 C33 H33A 119.4 . . ? C32 C33 H33A 119.4 . . ? C35 C34 C33 118.4(2) . . ? C35 C34 H34A 120.8 . . ? C33 C34 H34A 120.8 . . ? C34 C35 C36 121.4(2) . . ? C34 C35 H35A 119.3 . . ? C36 C35 H35A 119.3 . . ? C35 C36 C31 121.2(2) . . ? C35 C36 H36A 119.4 . . ? C31 C36 H36A 119.4 . . ? C40 O1 C37 108.92(14) . . ? C40 O1 Mg1 130.73(12) . . ? C37 O1 Mg1 119.75(11) . . ? O1 C37 C38 105.45(16) . . ? O1 C37 H37A 110.7 . . ? C38 C37 H37A 110.7 . . ? O1 C37 H37B 110.7 . . ? C38 C37 H37B 110.7 . . ? H37A C37 H37B 108.8 . . ? C37 C38 C39 101.96(17) . . ? C37 C38 H38A 111.4 . . ? C39 C38 H38A 111.4 . . ? C37 C38 H38B 111.4 . . ? C39 C38 H38B 111.4 . . ? H38A C38 H38B 109.2 . . ? C40 C39 C38 102.47(17) . . ? C40 C39 H39A 111.3 . . ? C38 C39 H39A 111.3 . . ? C40 C39 H39B 111.3 . . ? C38 C39 H39B 111.3 . . ? H39A C39 H39B 109.2 . . ? O1 C40 C39 105.03(16) . . ? O1 C40 H40A 110.7 . . ? C39 C40 H40A 110.7 . . ? O1 C40 H40B 110.7 . . ? C39 C40 H40B 110.7 . . ? H40A C40 H40B 108.8 . . ? C41 O2 C44 108.7(5) . . ? C41 O2 Na1 130.6(5) . . ? C44 O2 Na1 120.6(4) . . ? O2 C41 C42 108.6(5) . . ? O2 C41 H41A 110.0 . . ? C42 C41 H41A 110.0 . . ? O2 C41 H41B 110.0 . . ? C42 C41 H41B 110.0 . . ? H41A C41 H41B 108.4 . . ? C41 C42 C43 103.8(4) . . ? C41 C42 H42A 111.0 . . ? C43 C42 H42A 111.0 . . ? C41 C42 H42B 111.0 . . ? C43 C42 H42B 111.0 . . ? H42A C42 H42B 109.0 . . ? C44 C43 C42 102.4(4) . . ? C44 C43 H43A 111.3 . . ? C42 C43 H43A 111.3 . . ? C44 C43 H43B 111.3 . . ? C42 C43 H43B 111.3 . . ? H43A C43 H43B 109.2 . . ? O2 C44 C43 105.5(4) . . ? O2 C44 H44A 110.6 . . ? C43 C44 H44A 110.6 . . ? O2 C44 H44B 110.6 . . ? C43 C44 H44B 110.6 . . ? H44A C44 H44B 108.8 . . ? C41A O2A C44A 107.3(13) . . ? C41A O2A Na1 128.3(11) . . ? C44A O2A Na1 119.8(11) . . ? O2A C41A C42A 104.9(12) . . ? O2A C41A H41C 110.8 . . ? C42A C41A H41C 110.8 . . ? O2A C41A H41D 110.8 . . ? C42A C41A H41D 110.8 . . ? H41C C41A H41D 108.8 . . ? C41A C42A C43A 103.7(10) . . ? C41A C42A H42C 111.0 . . ? C43A C42A H42C 111.0 . . ? C41A C42A H42D 111.0 . . ? C43A C42A H42D 111.0 . . ? H42C C42A H42D 109.0 . . ? O2A C44A C43A 106.4(11) . . ? O2A C44A H44C 110.4 . . ? C43A C44A H44C 110.4 . . ? O2A C44A H44D 110.4 . . ? C43A C44A H44D 110.4 . . ? H44C C44A H44D 108.6 . . ? C42A C43A C44A 97.6(11) . . ? C42A C43A H43C 112.2 . . ? C44A C43A H43C 112.2 . . ? C42A C43A H43D 112.2 . . ? C44A C43A H43D 112.2 . . ? H43C C43A H43D 109.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Mg1 N1 C7 -169.61(14) . . . . ? N2 Mg1 N1 C7 -51.03(17) . . . . ? N3 Mg1 N1 C7 82.68(16) . . . . ? O1 Mg1 N1 C1 -4.29(15) . . . . ? N2 Mg1 N1 C1 114.29(14) . . . . ? N3 Mg1 N1 C1 -112.01(14) . . . . ? C7 N1 C1 C6 50.7(3) . . . . ? Mg1 N1 C1 C6 -115.12(17) . . . . ? C7 N1 C1 C2 -133.60(18) . . . . ? Mg1 N1 C1 C2 60.6(2) . . . . ? C6 C1 C2 C3 -0.6(3) . . . . ? N1 C1 C2 C3 -176.62(17) . . . . ? C1 C2 C3 C4 -0.9(3) . . . . ? C2 C3 C4 C5 1.0(3) . . . . ? C3 C4 C5 C6 0.5(3) . . . . ? C4 C5 C6 C1 -2.0(3) . . . . ? C2 C1 C6 C5 2.0(3) . . . . ? N1 C1 C6 C5 177.84(17) . . . . ? C1 N1 C7 C12 -176.43(17) . . . . ? Mg1 N1 C7 C12 -11.4(2) . . . . ? C1 N1 C7 C8 6.2(3) . . . . ? Mg1 N1 C7 C8 171.27(15) . . . . ? N1 C7 C8 C9 179.24(19) . . . . ? C12 C7 C8 C9 1.8(3) . . . . ? N1 C7 C8 Na1 94.0(2) . . . 1_554 ? C12 C7 C8 Na1 -83.4(2) . . . 1_554 ? C7 C8 C9 C10 -1.8(3) . . . . ? Na1 C8 C9 C10 111.8(2) 1_554 . . . ? C7 C8 C9 Na1 -113.56(19) . . . 1_554 ? C8 C9 C10 C11 0.7(3) . . . . ? Na1 C9 C10 C11 93.7(2) 1_554 . . . ? C9 C10 C11 C12 0.2(3) . . . . ? C10 C11 C12 C7 0.0(3) . . . . ? N1 C7 C12 C11 -178.6(2) . . . . ? C8 C7 C12 C11 -1.0(3) . . . . ? O1 Mg1 N2 C19 -148.77(15) . . . . ? N1 Mg1 N2 C19 94.87(16) . . . . ? N3 Mg1 N2 C19 -44.64(17) . . . . ? O1 Mg1 N2 C13 34.82(14) . . . . ? N1 Mg1 N2 C13 -81.55(14) . . . . ? N3 Mg1 N2 C13 138.94(12) . . . . ? C19 N2 C13 C14 -119.2(2) . . . . ? Mg1 N2 C13 C14 57.7(2) . . . . ? C19 N2 C13 C18 65.6(2) . . . . ? Mg1 N2 C13 C18 -117.51(18) . . . . ? C18 C13 C14 C15 0.0(3) . . . . ? N2 C13 C14 C15 -175.38(18) . . . . ? C13 C14 C15 C16 0.2(3) . . . . ? C14 C15 C16 C17 -0.5(3) . . . . ? C15 C16 C17 C18 0.5(3) . . . . ? C16 C17 C18 C13 -0.2(3) . . . . ? C14 C13 C18 C17 0.0(3) . . . . ? N2 C13 C18 C17 175.28(19) . . . . ? C13 N2 C19 C24 -170.18(17) . . . . ? Mg1 N2 C19 C24 13.6(3) . . . . ? C13 N2 C19 C20 14.4(3) . . . . ? Mg1 N2 C19 C20 -161.86(14) . . . . ? N2 C19 C20 C21 172.55(17) . . . . ? C24 C19 C20 C21 -3.1(3) . . . . ? C19 C20 C21 C22 1.3(3) . . . . ? C20 C21 C22 C23 0.7(3) . . . . ? C21 C22 C23 C24 -0.7(3) . . . . ? C21 C22 C23 Na1 76.5(2) . . . . ? O2A Na1 C23 C22 96.6(5) . . . . ? O2 Na1 C23 C22 102.9(2) . . . . ? C24 Na1 C23 C22 -116.1(2) . . . . ? C28 Na1 C23 C22 -146.97(17) . . . . ? C9 Na1 C23 C22 -0.38(17) 1_556 . . . ? C29 Na1 C23 C22 -111.56(17) . . . . ? C8 Na1 C23 C22 -14.87(18) 1_556 . . . ? C27 Na1 C23 C22 -179.76(15) . . . . ? C30 Na1 C23 C22 -121.98(16) . . . . ? C26 Na1 C23 C22 -170.06(16) . . . . ? O2A Na1 C23 C24 -147.4(5) . . . . ? O2 Na1 C23 C24 -141.0(2) . . . . ? C28 Na1 C23 C24 -30.9(2) . . . . ? C9 Na1 C23 C24 115.71(14) 1_556 . . . ? C29 Na1 C23 C24 4.54(17) . . . . ? C8 Na1 C23 C24 101.23(14) 1_556 . . . ? C27 Na1 C23 C24 -63.67(16) . . . . ? C30 Na1 C23 C24 -5.88(14) . . . . ? C26 Na1 C23 C24 -53.96(14) . . . . ? C22 C23 C24 C19 -1.3(3) . . . . ? Na1 C23 C24 C19 -105.28(18) . . . . ? C22 C23 C24 Na1 103.99(18) . . . . ? N2 C19 C24 C23 -172.74(17) . . . . ? C20 C19 C24 C23 3.1(3) . . . . ? N2 C19 C24 Na1 94.11(16) . . . . ? C20 C19 C24 Na1 -90.07(16) . . . . ? O2A Na1 C24 C23 35.0(6) . . . . ? O2 Na1 C24 C23 41.3(2) . . . . ? C28 Na1 C24 C23 162.78(13) . . . . ? C9 Na1 C24 C23 -65.65(14) 1_556 . . . ? C29 Na1 C24 C23 -176.54(13) . . . . ? C8 Na1 C24 C23 -90.69(14) 1_556 . . . ? C27 Na1 C24 C23 132.30(13) . . . . ? C30 Na1 C24 C23 174.25(14) . . . . ? C26 Na1 C24 C23 129.43(13) . . . . ? O2A Na1 C24 C19 156.3(6) . . . . ? O2 Na1 C24 C19 162.6(2) . . . . ? C28 Na1 C24 C19 -75.91(16) . . . . ? C9 Na1 C24 C19 55.66(14) 1_556 . . . ? C29 Na1 C24 C19 -55.23(14) . . . . ? C8 Na1 C24 C19 30.62(15) 1_556 . . . ? C27 Na1 C24 C19 -106.39(14) . . . . ? C23 Na1 C24 C19 121.3(2) . . . . ? C30 Na1 C24 C19 -64.44(13) . . . . ? C26 Na1 C24 C19 -109.26(14) . . . . ? O1 Mg1 N3 C25 72.19(14) . . . . ? N1 Mg1 N3 C25 -175.13(13) . . . . ? N2 Mg1 N3 C25 -40.79(15) . . . . ? O1 Mg1 N3 C31 -94.15(14) . . . . ? N1 Mg1 N3 C31 18.53(17) . . . . ? N2 Mg1 N3 C31 152.86(14) . . . . ? C31 N3 C25 C30 153.48(18) . . . . ? Mg1 N3 C25 C30 -13.1(2) . . . . ? C31 N3 C25 C26 -30.6(3) . . . . ? Mg1 N3 C25 C26 162.76(16) . . . . ? N3 C25 C26 C27 -178.34(19) . . . . ? C30 C25 C26 C27 -2.3(3) . . . . ? N3 C25 C26 Na1 -120.18(18) . . . . ? C30 C25 C26 Na1 55.83(16) . . . . ? O2A Na1 C26 C27 -75.6(5) . . . . ? O2 Na1 C26 C27 -78.0(2) . . . . ? C24 Na1 C26 C27 174.19(14) . . . . ? C28 Na1 C26 C27 30.45(13) . . . . ? C9 Na1 C26 C27 52.9(3) 1_556 . . . ? C29 Na1 C26 C27 66.34(13) . . . . ? C8 Na1 C26 C27 49.39(16) 1_556 . . . ? C23 Na1 C26 C27 -163.64(13) . . . . ? C30 Na1 C26 C27 99.79(14) . . . . ? O2A Na1 C26 C25 155.6(5) . . . . ? O2 Na1 C26 C25 153.12(19) . . . . ? C24 Na1 C26 C25 45.34(12) . . . . ? C28 Na1 C26 C25 -98.40(13) . . . . ? C9 Na1 C26 C25 -75.9(3) 1_556 . . . ? C29 Na1 C26 C25 -62.50(11) . . . . ? C8 Na1 C26 C25 -79.46(14) 1_556 . . . ? C27 Na1 C26 C25 -128.84(19) . . . . ? C23 Na1 C26 C25 67.52(12) . . . . ? C30 Na1 C26 C25 -29.06(10) . . . . ? C25 C26 C27 C28 1.6(3) . . . . ? Na1 C26 C27 C28 -62.4(2) . . . . ? C25 C26 C27 Na1 64.04(19) . . . . ? O2A Na1 C27 C28 -128.8(4) . . . . ? O2 Na1 C27 C28 -133.55(18) . . . . ? C24 Na1 C27 C28 119.99(13) . . . . ? C9 Na1 C27 C28 -31.26(18) 1_556 . . . ? C29 Na1 C27 C28 33.12(11) . . . . ? C8 Na1 C27 C28 -16.76(14) 1_556 . . . ? C23 Na1 C27 C28 147.76(13) . . . . ? C30 Na1 C27 C28 67.04(12) . . . . ? C26 Na1 C27 C28 126.46(19) . . . . ? O2A Na1 C27 C26 104.8(4) . . . . ? O2 Na1 C27 C26 99.99(18) . . . . ? C24 Na1 C27 C26 -6.48(15) . . . . ? C28 Na1 C27 C26 -126.46(19) . . . . ? C9 Na1 C27 C26 -157.72(14) 1_556 . . . ? C29 Na1 C27 C26 -93.34(14) . . . . ? C8 Na1 C27 C26 -143.22(13) 1_556 . . . ? C23 Na1 C27 C26 21.30(17) . . . . ? C30 Na1 C27 C26 -59.43(12) . . . . ? C26 C27 C28 C29 -0.2(3) . . . . ? Na1 C27 C28 C29 -70.41(18) . . . . ? C26 C27 C28 Na1 70.2(2) . . . . ? O2A Na1 C28 C27 53.6(4) . . . . ? O2 Na1 C28 C27 47.47(18) . . . . ? C24 Na1 C28 C27 -76.28(15) . . . . ? C9 Na1 C28 C27 158.67(12) 1_556 . . . ? C29 Na1 C28 C27 -121.33(18) . . . . ? C8 Na1 C28 C27 164.81(13) 1_556 . . . ? C23 Na1 C28 C27 -58.9(2) . . . . ? C30 Na1 C28 C27 -91.22(13) . . . . ? C26 Na1 C28 C27 -28.64(11) . . . . ? O2A Na1 C28 C29 175.0(4) . . . . ? O2 Na1 C28 C29 168.79(17) . . . . ? C24 Na1 C28 C29 45.05(15) . . . . ? C9 Na1 C28 C29 -80.00(13) 1_556 . . . ? C8 Na1 C28 C29 -73.86(12) 1_556 . . . ? C27 Na1 C28 C29 121.33(18) . . . . ? C23 Na1 C28 C29 62.5(2) . . . . ? C30 Na1 C28 C29 30.11(11) . . . . ? C26 Na1 C28 C29 92.69(13) . . . . ? C27 C28 C29 C30 -0.3(3) . . . . ? Na1 C28 C29 C30 -73.87(18) . . . . ? C27 C28 C29 Na1 73.57(19) . . . . ? O2A Na1 C29 C30 117.5(5) . . . . ? O2 Na1 C29 C30 109.7(2) . . . . ? C24 Na1 C29 C30 -20.01(13) . . . . ? C28 Na1 C29 C30 124.17(18) . . . . ? C9 Na1 C29 C30 -124.61(12) 1_556 . . . ? C8 Na1 C29 C30 -132.63(13) 1_556 . . . ? C27 Na1 C29 C30 92.14(13) . . . . ? C23 Na1 C29 C30 -22.20(16) . . . . ? C26 Na1 C29 C30 59.60(12) . . . . ? O2A Na1 C29 C28 -6.7(5) . . . . ? O2 Na1 C29 C28 -14.5(2) . . . . ? C24 Na1 C29 C28 -144.18(12) . . . . ? C9 Na1 C29 C28 111.23(13) 1_556 . . . ? C8 Na1 C29 C28 103.20(12) 1_556 . . . ? C27 Na1 C29 C28 -32.03(11) . . . . ? C23 Na1 C29 C28 -146.37(12) . . . . ? C30 Na1 C29 C28 -124.17(18) . . . . ? C26 Na1 C29 C28 -64.57(12) . . . . ? C28 C29 C30 C25 -0.6(3) . . . . ? Na1 C29 C30 C25 -68.86(18) . . . . ? C28 C29 C30 Na1 68.30(18) . . . . ? N3 C25 C30 C29 178.06(17) . . . . ? C26 C25 C30 C29 1.8(3) . . . . ? N3 C25 C30 Na1 117.90(16) . . . . ? C26 C25 C30 Na1 -58.32(16) . . . . ? O2A Na1 C30 C29 -91.6(7) . . . . ? O2 Na1 C30 C29 -95.7(2) . . . . ? C24 Na1 C30 C29 160.27(13) . . . . ? C28 Na1 C30 C29 -31.87(12) . . . . ? C9 Na1 C30 C29 66.40(14) 1_556 . . . ? C8 Na1 C30 C29 47.28(13) 1_556 . . . ? C27 Na1 C30 C29 -66.63(12) . . . . ? C23 Na1 C30 C29 163.07(12) . . . . ? C26 Na1 C30 C29 -98.75(13) . . . . ? O2A Na1 C30 C25 36.0(7) . . . . ? O2 Na1 C30 C25 31.8(3) . . . . ? C24 Na1 C30 C25 -72.18(11) . . . . ? C28 Na1 C30 C25 95.68(13) . . . . ? C9 Na1 C30 C25 -166.05(11) 1_556 . . . ? C29 Na1 C30 C25 127.55(18) . . . . ? C8 Na1 C30 C25 174.82(11) 1_556 . . . ? C27 Na1 C30 C25 60.91(11) . . . . ? C23 Na1 C30 C25 -69.39(12) . . . . ? C26 Na1 C30 C25 28.80(10) . . . . ? C25 N3 C31 C36 151.65(18) . . . . ? Mg1 N3 C31 C36 -42.0(2) . . . . ? C25 N3 C31 C32 -34.8(3) . . . . ? Mg1 N3 C31 C32 131.55(18) . . . . ? N3 C31 C32 C33 -175.3(2) . . . . ? C36 C31 C32 C33 -1.7(3) . . . . ? C31 C32 C33 C34 1.1(4) . . . . ? C32 C33 C34 C35 0.1(4) . . . . ? C33 C34 C35 C36 -0.6(4) . . . . ? C34 C35 C36 C31 0.0(3) . . . . ? N3 C31 C36 C35 175.10(19) . . . . ? C32 C31 C36 C35 1.1(3) . . . . ? N1 Mg1 O1 C40 69.39(16) . . . . ? N2 Mg1 O1 C40 -50.82(16) . . . . ? N3 Mg1 O1 C40 -164.50(15) . . . . ? N1 Mg1 O1 C37 -100.63(13) . . . . ? N2 Mg1 O1 C37 139.17(12) . . . . ? N3 Mg1 O1 C37 25.48(13) . . . . ? C40 O1 C37 C38 -11.55(19) . . . . ? Mg1 O1 C37 C38 160.47(11) . . . . ? O1 C37 C38 C39 31.96(19) . . . . ? C37 C38 C39 C40 -39.9(2) . . . . ? C37 O1 C40 C39 -13.9(2) . . . . ? Mg1 O1 C40 C39 175.21(12) . . . . ? C38 C39 C40 O1 33.6(2) . . . . ? O2A Na1 O2 C41 -139(7) . . . . ? C24 Na1 O2 C41 107.9(5) . . . . ? C28 Na1 O2 C41 -27.8(5) . . . . ? C9 Na1 O2 C41 -148.0(5) 1_556 . . . ? C29 Na1 O2 C41 -20.7(6) . . . . ? C8 Na1 O2 C41 -121.8(5) 1_556 . . . ? C27 Na1 O2 C41 -7.4(5) . . . . ? C23 Na1 O2 C41 125.9(5) . . . . ? C30 Na1 O2 C41 16.3(6) . . . . ? C26 Na1 O2 C41 18.5(5) . . . . ? O2A Na1 O2 C44 38(6) . . . . ? C24 Na1 O2 C44 -75.5(4) . . . . ? C28 Na1 O2 C44 148.8(4) . . . . ? C9 Na1 O2 C44 28.6(5) 1_556 . . . ? C29 Na1 O2 C44 155.9(4) . . . . ? C8 Na1 O2 C44 54.8(5) 1_556 . . . ? C27 Na1 O2 C44 169.2(4) . . . . ? C23 Na1 O2 C44 -57.5(4) . . . . ? C30 Na1 O2 C44 -167.1(3) . . . . ? C26 Na1 O2 C44 -164.9(4) . . . . ? C44 O2 C41 C42 2.0(7) . . . . ? Na1 O2 C41 C42 179.0(4) . . . . ? O2 C41 C42 C43 -21.5(6) . . . . ? C41 C42 C43 C44 31.9(6) . . . . ? C41 O2 C44 C43 18.8(6) . . . . ? Na1 O2 C44 C43 -158.5(3) . . . . ? C42 C43 C44 O2 -31.0(5) . . . . ? O2 Na1 O2A C41A -25(5) . . . . ? C24 Na1 O2A C41A 44(2) . . . . ? C28 Na1 O2A C41A -95.2(18) . . . . ? C9 Na1 O2A C41A 146.1(18) 1_556 . . . ? C29 Na1 O2A C41A -91.9(18) . . . . ? C8 Na1 O2A C41A 171.4(16) 1_556 . . . ? C27 Na1 O2A C41A -73.0(18) . . . . ? C23 Na1 O2A C41A 59.5(18) . . . . ? C30 Na1 O2A C41A -53(2) . . . . ? C26 Na1 O2A C41A -47.6(19) . . . . ? O2 Na1 O2A C44A 128(8) . . . . ? C24 Na1 O2A C44A -163.4(13) . . . . ? C28 Na1 O2A C44A 57.5(15) . . . . ? C9 Na1 O2A C44A -61.1(15) 1_556 . . . ? C29 Na1 O2A C44A 60.8(17) . . . . ? C8 Na1 O2A C44A -35.9(17) 1_556 . . . ? C27 Na1 O2A C44A 79.7(15) . . . . ? C23 Na1 O2A C44A -147.8(15) . . . . ? C30 Na1 O2A C44A 100.0(13) . . . . ? C26 Na1 O2A C44A 105.1(15) . . . . ? C44A O2A C41A C42A 9(2) . . . . ? Na1 O2A C41A C42A 164.3(16) . . . . ? O2A C41A C42A C43A -34(2) . . . . ? C41A O2A C44A C43A 19(2) . . . . ? Na1 O2A C44A C43A -138.6(12) . . . . ? C41A C42A C43A C44A 43.4(16) . . . . ? O2A C44A C43A C42A -38.6(16) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.420 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.045 _database_code_depnum_ccdc_archive 'CCDC 940856' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_srzl1010 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C63 H81 Mg N6 Na O6' _chemical_formula_sum 'C63 H81 Mg N6 Na O6' _chemical_formula_weight 1065.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Na Na 0.0362 0.0249 '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' O O 0.0106 0.0060 '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' 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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 20.8559(6) _cell_length_b 20.8559(6) _cell_length_c 11.8574(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4466.6(2) _cell_formula_units_Z 3 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 12971 _cell_measurement_theta_min 2.8294 _cell_measurement_theta_max 30.2960 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1716 _exptl_absorpt_coefficient_mu 0.092 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.94259 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Oxford Diffraction Gemini S' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23200 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 30.37 _reflns_number_total 5471 _reflns_number_gt 4944 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _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. ; _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^)+(0.0554P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(17) _refine_ls_number_reflns 5471 _refine_ls_number_parameters 232 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0870 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.092 _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 Na1 Na 0.3333 0.6667 0.93223(7) 0.02060(18) Uani 1 3 d S . . Mg1 Mg 0.3333 0.6667 1.19355(6) 0.01326(14) Uani 1 3 d S . . O1 O 0.43884(6) 0.70564(6) 0.81482(9) 0.0325(2) Uani 1 1 d D . . O2 O 0.42193(4) 0.73352(4) 1.07943(7) 0.01616(17) Uani 1 1 d . . . N1 N 0.49463(5) 0.86078(5) 1.10360(9) 0.0167(2) Uani 1 1 d . . . N2 N 0.41736(5) 0.77587(5) 1.24922(9) 0.01523(19) Uani 1 1 d . . . C1 C 0.46399(7) 0.90609(6) 1.07692(10) 0.0187(2) Uani 1 1 d . . . C2 C 0.50545(7) 0.98270(7) 1.09215(12) 0.0233(3) Uani 1 1 d . . . H2A H 0.5554 1.0051 1.1166 0.028 Uiso 1 1 calc R B . C3 C 0.47354(9) 1.02607(8) 1.07147(14) 0.0324(3) Uani 1 1 d . . . H3A H 0.5021 1.0782 1.0812 0.039 Uiso 1 1 calc R . . C4 C 0.40065(9) 0.99427(8) 1.03685(15) 0.0367(4) Uani 1 1 d . . . H4A H 0.3791 1.0243 1.0227 0.044 Uiso 1 1 calc R B . C5 C 0.35933(8) 0.91822(8) 1.02304(15) 0.0332(3) Uani 1 1 d . . . H5A H 0.3090 0.8960 1.0003 0.040 Uiso 1 1 calc R . . C6 C 0.39059(7) 0.87406(7) 1.04200(12) 0.0237(3) Uani 1 1 d . . . H6A H 0.3620 0.8220 1.0312 0.028 Uiso 1 1 calc R B . C7 C 0.56610(6) 0.87667(6) 1.07341(10) 0.0172(2) Uani 1 1 d . . . C8 C 0.59593(7) 0.83682(7) 1.12293(11) 0.0203(2) Uani 1 1 d . . . H8A H 0.5674 0.7990 1.1759 0.024 Uiso 1 1 calc R B . C9 C 0.66663(8) 0.85173(8) 1.09581(13) 0.0282(3) Uani 1 1 d . . . H9A H 0.6861 0.8239 1.1301 0.034 Uiso 1 1 calc R . . C10 C 0.70905(8) 0.90673(9) 1.01928(14) 0.0343(3) Uani 1 1 d . . . H10A H 0.7578 0.9173 1.0013 0.041 Uiso 1 1 calc R B . C11 C 0.67959(8) 0.94630(8) 0.96907(13) 0.0319(3) Uani 1 1 d . . . H11A H 0.7086 0.9842 0.9165 0.038 Uiso 1 1 calc R . . C12 C 0.60869(7) 0.93157(7) 0.99410(12) 0.0237(3) Uani 1 1 d . . . H12A H 0.5890 0.9585 0.9577 0.028 Uiso 1 1 calc R B . C13 C 0.44365(6) 0.78797(6) 1.14748(10) 0.0143(2) Uani 1 1 d . . . C14 C 0.43895(6) 0.82994(6) 1.34230(10) 0.0181(2) Uani 1 1 d . . . C15 C 0.51961(7) 0.89290(7) 1.34233(12) 0.0245(3) Uani 1 1 d . . . H15A H 0.5524 0.8725 1.3297 0.037 Uiso 1 1 calc R B . H15B H 0.5312 0.9184 1.4152 0.037 Uiso 1 1 calc R . . H15C H 0.5268 0.9281 1.2821 0.037 Uiso 1 1 calc R . . C16 C 0.38679(8) 0.86146(9) 1.34412(13) 0.0315(3) Uani 1 1 d . . . H16A H 0.3955 0.8923 1.2772 0.047 Uiso 1 1 calc R B . H16B H 0.3960 0.8916 1.4121 0.047 Uiso 1 1 calc R . . H16C H 0.3354 0.8207 1.3442 0.047 Uiso 1 1 calc R . . C17 C 0.42754(9) 0.78489(8) 1.44949(12) 0.0285(3) Uani 1 1 d . . . H17A H 0.3761 0.7443 1.4530 0.043 Uiso 1 1 calc R B . H17B H 0.4383 0.8169 1.5155 0.043 Uiso 1 1 calc R . . H17C H 0.4609 0.7645 1.4487 0.043 Uiso 1 1 calc R . . C20 C 0.50936(8) 0.77113(8) 0.83207(13) 0.0331(3) Uani 1 1 d D B . H20A H 0.5276 0.7715 0.9092 0.040 Uiso 1 1 calc R A 1 H20B H 0.5049 0.8159 0.8223 0.040 Uiso 1 1 calc R A 1 C21 C 0.5627(3) 0.7700(3) 0.7446(4) 0.0542(13) Uiso 0.50 1 d PD B 1 H21A H 0.6070 0.7735 0.7813 0.065 Uiso 0.50 1 calc PR B 1 H21B H 0.5787 0.8113 0.6902 0.065 Uiso 0.50 1 calc PR B 1 C22 C 0.5165(2) 0.6951(2) 0.6865(4) 0.0430(10) Uiso 0.50 1 d PD B 1 H22A H 0.5240 0.7004 0.6038 0.052 Uiso 0.50 1 calc PR B 1 H22B H 0.5308 0.6592 0.7140 0.052 Uiso 0.50 1 calc PR B 1 C23 C 0.43973(17) 0.67029(18) 0.7144(3) 0.0323(7) Uiso 0.50 1 d PD B 1 H23C H 0.4161 0.6831 0.6528 0.039 Uiso 0.50 1 calc PR B 1 H23D H 0.4120 0.6159 0.7247 0.039 Uiso 0.50 1 calc PR B 1 C21A C 0.5514(2) 0.77878(18) 0.7243(3) 0.0289(8) Uiso 0.50 1 d PD B 2 H21C H 0.6052 0.8130 0.7330 0.035 Uiso 0.50 1 calc PR B 2 H21D H 0.5324 0.7948 0.6601 0.035 Uiso 0.50 1 calc PR B 2 C22A C 0.5320(2) 0.6957(2) 0.7125(4) 0.0375(9) Uiso 0.50 1 d PD B 2 H22C H 0.5386 0.6839 0.6340 0.045 Uiso 0.50 1 calc PR B 2 H22D H 0.5625 0.6843 0.7637 0.045 Uiso 0.50 1 calc PR B 2 C23A C 0.45144(17) 0.65487(17) 0.7469(3) 0.0320(6) Uiso 0.50 1 d PD B 2 H23A H 0.4193 0.6393 0.6793 0.038 Uiso 0.50 1 calc PR B 2 H23B H 0.4402 0.6102 0.7911 0.038 Uiso 0.50 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0236(3) 0.0236(3) 0.0147(4) 0.000 0.000 0.01179(13) Mg1 0.01288(19) 0.01288(19) 0.0140(3) 0.000 0.000 0.00644(9) O1 0.0286(5) 0.0323(5) 0.0287(5) -0.0121(4) 0.0025(4) 0.0094(4) O2 0.0155(4) 0.0152(4) 0.0165(4) -0.0008(3) 0.0002(3) 0.0067(3) N1 0.0125(4) 0.0113(4) 0.0243(5) 0.0025(4) 0.0017(4) 0.0045(4) N2 0.0140(4) 0.0147(4) 0.0167(5) -0.0015(4) -0.0003(4) 0.0069(4) C1 0.0199(6) 0.0157(5) 0.0209(6) 0.0027(4) 0.0010(5) 0.0093(5) C2 0.0218(6) 0.0163(6) 0.0298(7) 0.0023(5) 0.0013(5) 0.0081(5) C3 0.0356(8) 0.0169(6) 0.0454(9) 0.0040(6) 0.0020(6) 0.0137(6) C4 0.0381(8) 0.0274(7) 0.0549(11) 0.0079(7) 0.0009(7) 0.0241(7) C5 0.0237(7) 0.0278(7) 0.0503(10) 0.0057(6) -0.0041(6) 0.0147(6) C6 0.0205(6) 0.0174(6) 0.0321(7) 0.0013(5) -0.0037(5) 0.0086(5) C7 0.0149(5) 0.0151(5) 0.0182(6) -0.0023(4) 0.0012(4) 0.0051(4) C8 0.0178(6) 0.0211(6) 0.0206(6) 0.0000(5) 0.0018(5) 0.0086(5) C9 0.0219(6) 0.0336(7) 0.0324(8) -0.0027(6) -0.0001(5) 0.0165(6) C10 0.0190(6) 0.0392(8) 0.0417(9) -0.0020(6) 0.0088(6) 0.0124(6) C11 0.0274(7) 0.0277(7) 0.0328(8) 0.0044(6) 0.0150(6) 0.0079(6) C12 0.0238(6) 0.0200(6) 0.0247(7) 0.0024(5) 0.0054(5) 0.0090(5) C13 0.0102(5) 0.0128(5) 0.0193(6) 0.0009(4) -0.0008(4) 0.0053(4) C14 0.0187(6) 0.0182(5) 0.0173(6) -0.0048(4) -0.0006(4) 0.0093(5) C15 0.0218(6) 0.0222(6) 0.0233(7) -0.0071(5) -0.0038(5) 0.0063(5) C16 0.0305(7) 0.0377(8) 0.0354(8) -0.0115(6) 0.0000(6) 0.0240(6) C17 0.0350(8) 0.0287(7) 0.0174(6) -0.0036(5) 0.0007(5) 0.0126(6) C20 0.0318(7) 0.0289(7) 0.0304(8) -0.0062(6) -0.0032(6) 0.0090(6) _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 Na1 O1 2.3775(11) 2_665 ? Na1 O1 2.3775(12) 3_565 ? Na1 O1 2.3775(12) . ? Na1 O2 2.4142(10) 2_665 ? Na1 O2 2.4142(10) . ? Na1 O2 2.4142(10) 3_565 ? Na1 Mg1 3.0986(11) . ? Mg1 O2 2.1477(9) 2_665 ? Mg1 O2 2.1477(9) . ? Mg1 O2 2.1477(9) 3_565 ? Mg1 N2 2.1686(10) 2_665 ? Mg1 N2 2.1686(10) . ? Mg1 N2 2.1686(10) 3_565 ? Mg1 C13 2.4842(11) 2_665 ? Mg1 C13 2.4842(11) . ? Mg1 C13 2.4842(11) 3_565 ? O1 C23 1.405(3) . ? O1 C20 1.4358(18) . ? O1 C23A 1.455(3) . ? O2 C13 1.2772(14) . ? N1 C7 1.4020(15) . ? N1 C1 1.4161(15) . ? N1 C13 1.4466(14) . ? N2 C13 1.2966(15) . ? N2 C14 1.4782(15) . ? C1 C6 1.3923(17) . ? C1 C2 1.3970(17) . ? C2 C3 1.3866(19) . ? C2 H2A 0.9500 . ? C3 C4 1.383(2) . ? C3 H3A 0.9500 . ? C4 C5 1.385(2) . ? C4 H4A 0.9500 . ? C5 C6 1.3872(19) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.3926(17) . ? C7 C12 1.4027(18) . ? C8 C9 1.3842(18) . ? C8 H8A 0.9500 . ? C9 C10 1.381(2) . ? C9 H9A 0.9500 . ? C10 C11 1.386(2) . ? C10 H10A 0.9500 . ? C11 C12 1.384(2) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C14 C16 1.5268(18) . ? C14 C17 1.5269(19) . ? C14 C15 1.5315(17) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C20 C21A 1.512(3) . ? C20 C21 1.529(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.530(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.453(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23C 0.9900 . ? C23 H23D 0.9900 . ? C21A C22A 1.576(5) . ? C21A H21C 0.9900 . ? C21A H21D 0.9900 . ? C22A C23A 1.511(5) . ? C22A H22C 0.9900 . ? C22A H22D 0.9900 . ? C23A H23A 0.9900 . ? C23A H23B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Na1 O1 89.18(5) 2_665 3_565 ? O1 Na1 O1 89.18(5) 2_665 . ? O1 Na1 O1 89.18(5) 3_565 . ? O1 Na1 O2 85.16(3) 2_665 2_665 ? O1 Na1 O2 118.20(4) 3_565 2_665 ? O1 Na1 O2 151.87(3) . 2_665 ? O1 Na1 O2 118.20(4) 2_665 . ? O1 Na1 O2 151.87(3) 3_565 . ? O1 Na1 O2 85.16(3) . . ? O2 Na1 O2 73.50(4) 2_665 . ? O1 Na1 O2 151.87(3) 2_665 3_565 ? O1 Na1 O2 85.16(3) 3_565 3_565 ? O1 Na1 O2 118.20(4) . 3_565 ? O2 Na1 O2 73.50(4) 2_665 3_565 ? O2 Na1 O2 73.50(4) . 3_565 ? O1 Na1 Mg1 125.84(3) 2_665 . ? O1 Na1 Mg1 125.84(3) 3_565 . ? O1 Na1 Mg1 125.84(3) . . ? O2 Na1 Mg1 43.70(2) 2_665 . ? O2 Na1 Mg1 43.70(2) . . ? O2 Na1 Mg1 43.70(2) 3_565 . ? O2 Mg1 O2 84.53(4) 2_665 . ? O2 Mg1 O2 84.53(4) 2_665 3_565 ? O2 Mg1 O2 84.53(4) . 3_565 ? O2 Mg1 N2 61.89(3) 2_665 2_665 ? O2 Mg1 N2 143.84(4) . 2_665 ? O2 Mg1 N2 103.83(3) 3_565 2_665 ? O2 Mg1 N2 103.83(3) 2_665 . ? O2 Mg1 N2 61.89(3) . . ? O2 Mg1 N2 143.84(4) 3_565 . ? N2 Mg1 N2 111.16(3) 2_665 . ? O2 Mg1 N2 143.84(4) 2_665 3_565 ? O2 Mg1 N2 103.83(3) . 3_565 ? O2 Mg1 N2 61.89(3) 3_565 3_565 ? N2 Mg1 N2 111.16(3) 2_665 3_565 ? N2 Mg1 N2 111.16(3) . 3_565 ? O2 Mg1 C13 30.94(4) 2_665 2_665 ? O2 Mg1 C13 115.29(4) . 2_665 ? O2 Mg1 C13 90.86(4) 3_565 2_665 ? N2 Mg1 C13 31.44(4) 2_665 2_665 ? N2 Mg1 C13 114.50(3) . 2_665 ? N2 Mg1 C13 129.74(4) 3_565 2_665 ? O2 Mg1 C13 90.86(4) 2_665 . ? O2 Mg1 C13 30.94(4) . . ? O2 Mg1 C13 115.29(4) 3_565 . ? N2 Mg1 C13 129.74(4) 2_665 . ? N2 Mg1 C13 31.44(4) . . ? N2 Mg1 C13 114.50(4) 3_565 . ? C13 Mg1 C13 115.31(2) 2_665 . ? O2 Mg1 C13 115.29(4) 2_665 3_565 ? O2 Mg1 C13 90.86(4) . 3_565 ? O2 Mg1 C13 30.94(3) 3_565 3_565 ? N2 Mg1 C13 114.50(4) 2_665 3_565 ? N2 Mg1 C13 129.74(4) . 3_565 ? N2 Mg1 C13 31.44(4) 3_565 3_565 ? C13 Mg1 C13 115.31(2) 2_665 3_565 ? C13 Mg1 C13 115.31(2) . 3_565 ? O2 Mg1 Na1 50.95(3) 2_665 . ? O2 Mg1 Na1 50.95(3) . . ? O2 Mg1 Na1 50.95(3) 3_565 . ? N2 Mg1 Na1 107.72(3) 2_665 . ? N2 Mg1 Na1 107.72(3) . . ? N2 Mg1 Na1 107.72(3) 3_565 . ? C13 Mg1 Na1 77.30(3) 2_665 . ? C13 Mg1 Na1 77.30(3) . . ? C13 Mg1 Na1 77.30(3) 3_565 . ? C23 O1 C20 110.11(16) . . ? C20 O1 C23A 107.42(15) . . ? C23 O1 Na1 124.71(14) . . ? C20 O1 Na1 125.07(9) . . ? C23A O1 Na1 123.26(13) . . ? C13 O2 Mg1 89.24(7) . . ? C13 O2 Na1 143.04(7) . . ? Mg1 O2 Na1 85.35(3) . . ? C7 N1 C1 124.50(10) . . ? C7 N1 C13 118.45(9) . . ? C1 N1 C13 116.16(9) . . ? C13 N2 C14 127.47(10) . . ? C13 N2 Mg1 87.84(7) . . ? C14 N2 Mg1 143.75(8) . . ? C6 C1 C2 119.38(11) . . ? C6 C1 N1 120.06(10) . . ? C2 C1 N1 120.43(11) . . ? C3 C2 C1 119.91(13) . . ? C3 C2 H2A 120.0 . . ? C1 C2 H2A 120.0 . . ? C4 C3 C2 120.73(13) . . ? C4 C3 H3A 119.6 . . ? C2 C3 H3A 119.6 . . ? C3 C4 C5 119.32(13) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? C4 C5 C6 120.75(13) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? C5 C6 C1 119.90(12) . . ? C5 C6 H6A 120.0 . . ? C1 C6 H6A 120.0 . . ? C8 C7 N1 119.38(10) . . ? C8 C7 C12 118.71(11) . . ? N1 C7 C12 121.91(11) . . ? C9 C8 C7 120.77(12) . . ? C9 C8 H8A 119.6 . . ? C7 C8 H8A 119.6 . . ? C10 C9 C8 120.48(13) . . ? C10 C9 H9A 119.8 . . ? C8 C9 H9A 119.8 . . ? C9 C10 C11 119.11(12) . . ? C9 C10 H10A 120.4 . . ? C11 C10 H10A 120.4 . . ? C12 C11 C10 121.23(13) . . ? C12 C11 H11A 119.4 . . ? C10 C11 H11A 119.4 . . ? C11 C12 C7 119.69(13) . . ? C11 C12 H12A 120.2 . . ? C7 C12 H12A 120.2 . . ? O2 C13 N2 119.16(10) . . ? O2 C13 N1 117.00(10) . . ? N2 C13 N1 123.80(10) . . ? O2 C13 Mg1 59.82(6) . . ? N2 C13 Mg1 60.73(6) . . ? N1 C13 Mg1 165.57(8) . . ? N2 C14 C16 109.16(10) . . ? N2 C14 C17 104.94(10) . . ? C16 C14 C17 109.14(11) . . ? N2 C14 C15 116.06(10) . . ? C16 C14 C15 110.15(11) . . ? C17 C14 C15 107.09(11) . . ? 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 . . ? O1 C20 C21A 104.12(16) . . ? O1 C20 C21 107.2(2) . . ? O1 C20 H20A 110.3 . . ? C21A C20 H20A 125.4 . . ? C21 C20 H20A 110.3 . . ? O1 C20 H20B 110.3 . . ? C21A C20 H20B 97.1 . . ? C21 C20 H20B 110.3 . . ? H20A C20 H20B 108.5 . . ? C20 C21 C22 103.3(3) . . ? C20 C21 H21A 111.1 . . ? C22 C21 H21A 111.1 . . ? C20 C21 H21B 111.1 . . ? C22 C21 H21B 111.1 . . ? H21A C21 H21B 109.1 . . ? C23 C22 C21 106.3(3) . . ? C23 C22 H22A 110.5 . . ? C21 C22 H22A 110.5 . . ? C23 C22 H22B 110.5 . . ? C21 C22 H22B 110.5 . . ? H22A C22 H22B 108.7 . . ? O1 C23 C22 107.9(3) . . ? O1 C23 H23C 110.1 . . ? C22 C23 H23C 110.1 . . ? O1 C23 H23D 110.1 . . ? C22 C23 H23D 110.1 . . ? H23C C23 H23D 108.4 . . ? C20 C21A C22A 98.2(2) . . ? C20 C21A H21C 112.1 . . ? C22A C21A H21C 112.1 . . ? C20 C21A H21D 112.1 . . ? C22A C21A H21D 112.1 . . ? H21C C21A H21D 109.8 . . ? C23A C22A C21A 101.4(3) . . ? C23A C22A H22C 111.5 . . ? C21A C22A H22C 111.5 . . ? C23A C22A H22D 111.5 . . ? C21A C22A H22D 111.5 . . ? H22C C22A H22D 109.3 . . ? O1 C23A C22A 107.1(2) . . ? O1 C23A H23A 110.3 . . ? C22A C23A H23A 110.3 . . ? O1 C23A H23B 110.3 . . ? C22A C23A H23B 110.3 . . ? H23A C23A H23B 108.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Na1 Mg1 O2 24.96(4) 2_665 . . 2_665 ? O1 Na1 Mg1 O2 -95.04(4) 3_565 . . 2_665 ? O1 Na1 Mg1 O2 144.96(4) . . . 2_665 ? O2 Na1 Mg1 O2 120.00(5) . . . 2_665 ? O2 Na1 Mg1 O2 -120.00(5) 3_565 . . 2_665 ? O1 Na1 Mg1 O2 -95.04(4) 2_665 . . . ? O1 Na1 Mg1 O2 144.96(4) 3_565 . . . ? O1 Na1 Mg1 O2 24.96(4) . . . . ? O2 Na1 Mg1 O2 -120.00(5) 2_665 . . . ? O2 Na1 Mg1 O2 120.00(5) 3_565 . . . ? O1 Na1 Mg1 O2 144.96(4) 2_665 . . 3_565 ? O1 Na1 Mg1 O2 24.96(4) 3_565 . . 3_565 ? O1 Na1 Mg1 O2 -95.04(4) . . . 3_565 ? O2 Na1 Mg1 O2 120.00(5) 2_665 . . 3_565 ? O2 Na1 Mg1 O2 -120.00(5) . . . 3_565 ? O1 Na1 Mg1 N2 51.29(4) 2_665 . . 2_665 ? O1 Na1 Mg1 N2 -68.71(4) 3_565 . . 2_665 ? O1 Na1 Mg1 N2 171.29(4) . . . 2_665 ? O2 Na1 Mg1 N2 26.33(4) 2_665 . . 2_665 ? O2 Na1 Mg1 N2 146.33(4) . . . 2_665 ? O2 Na1 Mg1 N2 -93.67(4) 3_565 . . 2_665 ? O1 Na1 Mg1 N2 -68.71(4) 2_665 . . . ? O1 Na1 Mg1 N2 171.29(4) 3_565 . . . ? O1 Na1 Mg1 N2 51.29(4) . . . . ? O2 Na1 Mg1 N2 -93.67(4) 2_665 . . . ? O2 Na1 Mg1 N2 26.33(4) . . . . ? O2 Na1 Mg1 N2 146.33(4) 3_565 . . . ? O1 Na1 Mg1 N2 171.29(4) 2_665 . . 3_565 ? O1 Na1 Mg1 N2 51.29(4) 3_565 . . 3_565 ? O1 Na1 Mg1 N2 -68.71(4) . . . 3_565 ? O2 Na1 Mg1 N2 146.33(4) 2_665 . . 3_565 ? O2 Na1 Mg1 N2 -93.67(4) . . . 3_565 ? O2 Na1 Mg1 N2 26.33(4) 3_565 . . 3_565 ? O1 Na1 Mg1 C13 43.27(4) 2_665 . . 2_665 ? O1 Na1 Mg1 C13 -76.73(4) 3_565 . . 2_665 ? O1 Na1 Mg1 C13 163.27(4) . . . 2_665 ? O2 Na1 Mg1 C13 18.31(4) 2_665 . . 2_665 ? O2 Na1 Mg1 C13 138.31(4) . . . 2_665 ? O2 Na1 Mg1 C13 -101.69(4) 3_565 . . 2_665 ? O1 Na1 Mg1 C13 -76.73(4) 2_665 . . . ? O1 Na1 Mg1 C13 163.27(4) 3_565 . . . ? O1 Na1 Mg1 C13 43.27(4) . . . . ? O2 Na1 Mg1 C13 -101.69(4) 2_665 . . . ? O2 Na1 Mg1 C13 18.31(4) . . . . ? O2 Na1 Mg1 C13 138.31(4) 3_565 . . . ? O1 Na1 Mg1 C13 163.27(4) 2_665 . . 3_565 ? O1 Na1 Mg1 C13 43.27(4) 3_565 . . 3_565 ? O1 Na1 Mg1 C13 -76.73(4) . . . 3_565 ? O2 Na1 Mg1 C13 138.31(4) 2_665 . . 3_565 ? O2 Na1 Mg1 C13 -101.69(4) . . . 3_565 ? O2 Na1 Mg1 C13 18.31(4) 3_565 . . 3_565 ? O1 Na1 O1 C23 -84.2(2) 2_665 . . . ? O1 Na1 O1 C23 5.0(2) 3_565 . . . ? O2 Na1 O1 C23 -162.3(2) 2_665 . . . ? O2 Na1 O1 C23 157.4(2) . . . . ? O2 Na1 O1 C23 89.1(2) 3_565 . . . ? Mg1 Na1 O1 C23 140.4(2) . . . . ? O1 Na1 O1 C20 91.61(14) 2_665 . . . ? O1 Na1 O1 C20 -179.20(12) 3_565 . . . ? O2 Na1 O1 C20 13.49(18) 2_665 . . . ? O2 Na1 O1 C20 -26.78(12) . . . . ? O2 Na1 O1 C20 -95.13(12) 3_565 . . . ? Mg1 Na1 O1 C20 -43.79(13) . . . . ? O1 Na1 O1 C23A -114.54(19) 2_665 . . . ? O1 Na1 O1 C23A -25.3(2) 3_565 . . . ? O2 Na1 O1 C23A 167.3(2) 2_665 . . . ? O2 Na1 O1 C23A 127.1(2) . . . . ? O2 Na1 O1 C23A 58.7(2) 3_565 . . . ? Mg1 Na1 O1 C23A 110.1(2) . . . . ? O2 Mg1 O2 C13 100.90(8) 2_665 . . . ? O2 Mg1 O2 C13 -174.10(7) 3_565 . . . ? N2 Mg1 O2 C13 79.88(9) 2_665 . . . ? N2 Mg1 O2 C13 -7.97(6) . . . . ? N2 Mg1 O2 C13 -114.83(7) 3_565 . . . ? C13 Mg1 O2 C13 97.55(4) 2_665 . . . ? C13 Mg1 O2 C13 -143.77(6) 3_565 . . . ? Na1 Mg1 O2 C13 143.40(7) . . . . ? O2 Mg1 O2 Na1 -42.502(16) 2_665 . . . ? O2 Mg1 O2 Na1 42.502(16) 3_565 . . . ? N2 Mg1 O2 Na1 -63.52(7) 2_665 . . . ? N2 Mg1 O2 Na1 -151.38(4) . . . . ? N2 Mg1 O2 Na1 101.77(4) 3_565 . . . ? C13 Mg1 O2 Na1 -45.86(4) 2_665 . . . ? C13 Mg1 O2 Na1 -143.40(7) . . . . ? C13 Mg1 O2 Na1 72.82(3) 3_565 . . . ? O1 Na1 O2 C13 31.09(14) 2_665 . . . ? O1 Na1 O2 C13 -163.34(12) 3_565 . . . ? O1 Na1 O2 C13 117.55(12) . . . . ? O2 Na1 O2 C13 -43.92(13) 2_665 . . . ? O2 Na1 O2 C13 -121.14(12) 3_565 . . . ? Mg1 Na1 O2 C13 -82.53(12) . . . . ? O1 Na1 O2 Mg1 113.62(4) 2_665 . . . ? O1 Na1 O2 Mg1 -80.81(9) 3_565 . . . ? O1 Na1 O2 Mg1 -159.92(4) . . . . ? O2 Na1 O2 Mg1 38.609(11) 2_665 . . . ? O2 Na1 O2 Mg1 -38.609(11) 3_565 . . . ? O2 Mg1 N2 C13 -68.08(7) 2_665 . . . ? O2 Mg1 N2 C13 7.86(6) . . . . ? O2 Mg1 N2 C13 31.73(10) 3_565 . . . ? N2 Mg1 N2 C13 -132.93(7) 2_665 . . . ? N2 Mg1 N2 C13 102.67(8) 3_565 . . . ? C13 Mg1 N2 C13 -98.93(7) 2_665 . . . ? C13 Mg1 N2 C13 72.89(8) 3_565 . . . ? Na1 Mg1 N2 C13 -15.13(7) . . . . ? O2 Mg1 N2 C14 99.90(13) 2_665 . . . ? O2 Mg1 N2 C14 175.85(14) . . . . ? O2 Mg1 N2 C14 -160.28(12) 3_565 . . . ? N2 Mg1 N2 C14 35.06(14) 2_665 . . . ? N2 Mg1 N2 C14 -89.34(11) 3_565 . . . ? C13 Mg1 N2 C14 69.06(14) 2_665 . . . ? C13 Mg1 N2 C14 167.99(17) . . . . ? C13 Mg1 N2 C14 -119.12(13) 3_565 . . . ? Na1 Mg1 N2 C14 152.86(12) . . . . ? C7 N1 C1 C6 138.91(13) . . . . ? C13 N1 C1 C6 -30.07(16) . . . . ? C7 N1 C1 C2 -45.15(18) . . . . ? C13 N1 C1 C2 145.87(12) . . . . ? C6 C1 C2 C3 -0.6(2) . . . . ? N1 C1 C2 C3 -176.55(13) . . . . ? C1 C2 C3 C4 0.6(2) . . . . ? C2 C3 C4 C5 0.1(3) . . . . ? C3 C4 C5 C6 -0.9(3) . . . . ? C4 C5 C6 C1 1.0(2) . . . . ? C2 C1 C6 C5 -0.2(2) . . . . ? N1 C1 C6 C5 175.79(13) . . . . ? C1 N1 C7 C8 167.03(11) . . . . ? C13 N1 C7 C8 -24.22(16) . . . . ? C1 N1 C7 C12 -13.22(18) . . . . ? C13 N1 C7 C12 155.53(12) . . . . ? N1 C7 C8 C9 -179.30(12) . . . . ? C12 C7 C8 C9 0.94(19) . . . . ? C7 C8 C9 C10 0.3(2) . . . . ? C8 C9 C10 C11 -0.7(2) . . . . ? C9 C10 C11 C12 -0.1(2) . . . . ? C10 C11 C12 C7 1.3(2) . . . . ? C8 C7 C12 C11 -1.71(19) . . . . ? N1 C7 C12 C11 178.54(12) . . . . ? Mg1 O2 C13 N2 13.55(10) . . . . ? Na1 O2 C13 N2 94.79(14) . . . . ? Mg1 O2 C13 N1 -163.95(8) . . . . ? Na1 O2 C13 N1 -82.71(14) . . . . ? Na1 O2 C13 Mg1 81.24(11) . . . . ? C14 N2 C13 O2 175.49(10) . . . . ? Mg1 N2 C13 O2 -13.43(10) . . . . ? C14 N2 C13 N1 -7.18(17) . . . . ? Mg1 N2 C13 N1 163.90(10) . . . . ? C14 N2 C13 Mg1 -171.08(12) . . . . ? C7 N1 C13 O2 -67.10(14) . . . . ? C1 N1 C13 O2 102.58(12) . . . . ? C7 N1 C13 N2 115.52(13) . . . . ? C1 N1 C13 N2 -74.80(14) . . . . ? C7 N1 C13 Mg1 -140.6(3) . . . . ? C1 N1 C13 Mg1 29.1(4) . . . . ? O2 Mg1 C13 O2 -77.85(8) 2_665 . . . ? O2 Mg1 C13 O2 6.50(7) 3_565 . . . ? N2 Mg1 C13 O2 -130.95(7) 2_665 . . . ? N2 Mg1 C13 O2 166.43(10) . . . . ? N2 Mg1 C13 O2 75.56(7) 3_565 . . . ? C13 Mg1 C13 O2 -97.49(6) 2_665 . . . ? C13 Mg1 C13 O2 40.82(8) 3_565 . . . ? Na1 Mg1 C13 O2 -28.33(6) . . . . ? O2 Mg1 C13 N2 115.72(7) 2_665 . . . ? O2 Mg1 C13 N2 -166.43(10) . . . . ? O2 Mg1 C13 N2 -159.93(6) 3_565 . . . ? N2 Mg1 C13 N2 62.62(8) 2_665 . . . ? N2 Mg1 C13 N2 -90.87(8) 3_565 . . . ? C13 Mg1 C13 N2 96.08(8) 2_665 . . . ? C13 Mg1 C13 N2 -125.61(8) 3_565 . . . ? Na1 Mg1 C13 N2 165.24(7) . . . . ? O2 Mg1 C13 N1 3.4(3) 2_665 . . . ? O2 Mg1 C13 N1 81.2(3) . . . . ? O2 Mg1 C13 N1 87.7(3) 3_565 . . . ? N2 Mg1 C13 N1 -49.7(4) 2_665 . . . ? N2 Mg1 C13 N1 -112.4(4) . . . . ? N2 Mg1 C13 N1 156.8(3) 3_565 . . . ? C13 Mg1 C13 N1 -16.3(4) 2_665 . . . ? C13 Mg1 C13 N1 122.0(3) 3_565 . . . ? Na1 Mg1 C13 N1 52.9(3) . . . . ? C13 N2 C14 C16 94.03(14) . . . . ? Mg1 N2 C14 C16 -70.78(16) . . . . ? C13 N2 C14 C17 -149.10(12) . . . . ? Mg1 N2 C14 C17 46.09(16) . . . . ? C13 N2 C14 C15 -31.14(17) . . . . ? Mg1 N2 C14 C15 164.06(10) . . . . ? C23 O1 C20 C21A 7.3(3) . . . . ? C23A O1 C20 C21A 33.7(3) . . . . ? Na1 O1 C20 C21A -169.05(17) . . . . ? C23 O1 C20 C21 -9.6(3) . . . . ? C23A O1 C20 C21 16.9(3) . . . . ? Na1 O1 C20 C21 174.1(2) . . . . ? O1 C20 C21 C22 -4.9(4) . . . . ? C21A C20 C21 C22 -86.4(9) . . . . ? C20 C21 C22 C23 17.0(5) . . . . ? C20 O1 C23 C22 21.0(3) . . . . ? C23A O1 C23 C22 -67.3(5) . . . . ? Na1 O1 C23 C22 -162.7(2) . . . . ? C21 C22 C23 O1 -23.6(4) . . . . ? O1 C20 C21A C22A -45.7(3) . . . . ? C21 C20 C21A C22A 57.4(8) . . . . ? C20 C21A C22A C23A 40.5(3) . . . . ? C23 O1 C23A C22A 94.3(5) . . . . ? C20 O1 C23A C22A -6.1(3) . . . . ? Na1 O1 C23A C22A -163.8(2) . . . . ? C21A C22A C23A O1 -22.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.241 _refine_diff_density_min -0.267 _refine_diff_density_rms 0.037 _database_code_depnum_ccdc_archive 'CCDC 940857' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_srzl1104 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H21 N3 O3' _chemical_formula_sum 'C24 H21 N3 O3' _chemical_formula_weight 399.44 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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' _cell_length_a 12.6655(19) _cell_length_b 12.6655(19) _cell_length_c 26.761(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3717.7(11) _cell_formula_units_Z 6 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 1191 _cell_measurement_theta_min 3.2104 _cell_measurement_theta_max 29.3393 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.070 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1260 _exptl_absorpt_coefficient_mu 0.072 _exptl_absorpt_correction_T_min 0.89393 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; the equivalent of approx 152 electrons were removed from approx 910 A^3^ of void space per cell - this is probably either THF or hexane but could not be modelled adequately ; _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 'OD Xcalibur, Eos' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2894 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 29.40 _reflns_number_total 1477 _reflns_number_gt 1225 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _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. ; _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^)+(0.0906P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -1(2) _refine_ls_number_reflns 1477 _refine_ls_number_parameters 92 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1443 _refine_ls_wR_factor_gt 0.1362 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 O1 O 0.77822(16) -0.19026(16) 0.00998(7) 0.0436(5) Uani 1 1 d . . . C1 C 0.8803(2) -0.1027(2) 0.00911(10) 0.0332(5) Uani 1 1 d . . . N1 N 0.90199(17) 0.01615(18) 0.00925(9) 0.0338(5) Uani 1 1 d . . . C2 C 0.7971(2) 0.0336(2) 0.01378(10) 0.0339(6) Uani 1 1 d . . . C3 C 0.7418(2) 0.0168(3) 0.05959(10) 0.0392(6) Uani 1 1 d . . . H3A H 0.7702 -0.0083 0.0875 0.047 Uiso 1 1 calc R . . C4 C 0.6440(2) 0.0368(3) 0.06474(10) 0.0399(6) Uani 1 1 d . . . H4A H 0.6058 0.0253 0.0964 0.048 Uiso 1 1 calc R . . C5 C 0.6014(2) 0.0732(3) 0.02460(11) 0.0391(6) Uani 1 1 d . . . C6 C 0.6583(3) 0.0888(3) -0.02099(11) 0.0446(7) Uani 1 1 d . . . H6A H 0.6297 0.1135 -0.0490 0.054 Uiso 1 1 calc R . . C7 C 0.7561(3) 0.0694(3) -0.02711(11) 0.0415(6) Uani 1 1 d . . . H7A H 0.7941 0.0804 -0.0588 0.050 Uiso 1 1 calc R . . C8 C 0.4966(3) 0.0974(4) 0.03137(14) 0.0630(9) Uani 1 1 d . . . H8A H 0.5179 0.1761 0.0163 0.094 Uiso 1 1 calc R . . H8B H 0.4806 0.0993 0.0671 0.094 Uiso 1 1 calc R . . H8C H 0.4235 0.0326 0.0151 0.094 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 O1 0.0291(10) 0.0324(10) 0.0666(13) -0.0022(9) -0.0038(8) 0.0133(8) C1 0.0303(12) 0.0305(12) 0.0387(13) -0.0001(10) -0.0042(10) 0.0151(11) N1 0.0277(11) 0.0294(11) 0.0459(12) 0.0018(10) -0.0004(10) 0.0155(8) C2 0.0244(12) 0.0313(12) 0.0466(15) -0.0008(11) -0.0026(11) 0.0144(10) C3 0.0390(14) 0.0398(14) 0.0394(14) 0.0044(12) -0.0009(12) 0.0202(12) C4 0.0350(14) 0.0463(15) 0.0401(14) 0.0016(12) 0.0035(12) 0.0214(12) C5 0.0304(13) 0.0414(14) 0.0469(15) -0.0004(12) -0.0003(11) 0.0189(12) C6 0.0417(15) 0.0575(17) 0.0441(16) 0.0049(13) -0.0032(13) 0.0319(14) C7 0.0417(15) 0.0466(16) 0.0400(14) 0.0037(12) 0.0013(12) 0.0248(13) C8 0.0528(19) 0.088(3) 0.066(2) 0.0099(18) 0.0082(16) 0.048(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 O1 C1 1.212(3) . ? C1 N1 1.388(3) . ? C1 N1 1.391(3) 2_645 ? N1 C1 1.391(3) 3_765 ? N1 C2 1.456(3) . ? C2 C3 1.375(4) . ? C2 C7 1.381(4) . ? C3 C4 1.390(4) . ? C3 H3A 0.9500 . ? C4 C5 1.380(4) . ? C4 H4A 0.9500 . ? C5 C6 1.380(4) . ? C5 C8 1.516(4) . ? C6 C7 1.388(4) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 N1 122.4(2) . . ? O1 C1 N1 122.3(2) . 2_645 ? N1 C1 N1 115.3(2) . 2_645 ? C1 N1 C1 124.7(2) . 3_765 ? C1 N1 C2 117.6(2) . . ? C1 N1 C2 117.6(2) 3_765 . ? C3 C2 C7 120.7(2) . . ? C3 C2 N1 118.9(2) . . ? C7 C2 N1 120.3(2) . . ? C2 C3 C4 119.5(2) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C5 C4 C3 121.0(2) . . ? C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? C4 C5 C6 118.3(2) . . ? C4 C5 C8 120.1(3) . . ? C6 C5 C8 121.6(3) . . ? C5 C6 C7 121.8(3) . . ? C5 C6 H6A 119.1 . . ? C7 C6 H6A 119.1 . . ? C2 C7 C6 118.7(3) . . ? C2 C7 H7A 120.7 . . ? C6 C7 H7A 120.7 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 N1 C1 178.90(16) . . . 3_765 ? N1 C1 N1 C1 0.5(4) 2_645 . . 3_765 ? O1 C1 N1 C2 3.9(3) . . . . ? N1 C1 N1 C2 -174.45(18) 2_645 . . . ? C1 N1 C2 C3 75.2(3) . . . . ? C1 N1 C2 C3 -100.2(3) 3_765 . . . ? C1 N1 C2 C7 -106.4(3) . . . . ? C1 N1 C2 C7 78.2(3) 3_765 . . . ? C7 C2 C3 C4 -0.4(4) . . . . ? N1 C2 C3 C4 178.0(2) . . . . ? C2 C3 C4 C5 0.1(4) . . . . ? C3 C4 C5 C6 0.2(4) . . . . ? C3 C4 C5 C8 -178.5(3) . . . . ? C4 C5 C6 C7 -0.2(4) . . . . ? C8 C5 C6 C7 178.5(3) . . . . ? C3 C2 C7 C6 0.4(4) . . . . ? N1 C2 C7 C6 -178.0(2) . . . . ? C5 C6 C7 C2 -0.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.896 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.192 _refine_diff_density_min -0.306 _refine_diff_density_rms 0.055 #===END _database_code_depnum_ccdc_archive 'CCDC 940858'