Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Mulvey, Robert' 'Drewette, Katy J.' 'Henderson, Kenneth W.' 'Kennedy, Alan R.' 'O'Hara, Charles T.' 'Rowlings, Rene B.' _publ_contact_author_name 'Prof Robert Mulvey' _publ_contact_author_address ; Pure and Applied Chemistry University of Strathclyde 295 Cathedral St Thomas Graham Building Glasgow Strathclyde G1 1XL UNITED KINGDOM ; _publ_contact_author_email 'R.E.MULVEY@STRATH.AC.UK' _publ_section_title ; Alkoxide encapsulation in inverse crown chemistry: rational synthesis of a series of composite alkali metal-magnesium-alkoxide-diisopropylamides ; _publ_contact_letter ; Dear Sir, Please find herein the cif files for the recently submitted Chem Comm ref. no. b202549c by R E Mulvey and others. If there are any problems with this file please contact me. Yours, Alan Kennedy 0141 548 2016 a.r.kennedy@strath.ac.uk P & A Chemistry University of Strathclyde 295 Cathedral Street Glasgow G1 1XL Scotland ; #---------------------------------------------------------------------- #----- #---------------------------------Compound 1--------------------------- #--- #---------------------------------------------------------------------- #----- data_g39 _database_code_CSD 182083 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H74 Mg2 N4 Na2 O2' _chemical_formula_weight 641.55 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' 'Mg' 'Mg' 0.0486 0.0363 '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' 'Na' 'Na' 0.0362 0.0249 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6321(2) _cell_length_b 10.3272(2) _cell_length_c 11.4653(2) _cell_angle_alpha 100.339(1) _cell_angle_beta 108.296(1) _cell_angle_gamma 108.270(1) _cell_volume 978.18(3) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4400 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description tabular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.089 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 356 _exptl_absorpt_coefficient_mu 0.114 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8633 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 27.44 _reflns_number_total 4460 _reflns_number_gt 3652 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Denzo and Collect' _computing_cell_refinement 'Denzo and Collect' _computing_data_reduction 'Denzo and Collect and scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+0.2207P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4460 _refine_ls_number_parameters 338 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0848 _refine_ls_wR_factor_gt 0.0787 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.40992(4) 0.89610(4) 0.85920(3) 0.01873(10) Uani 1 d . . . Na1 Na 0.58697(6) 0.81023(5) 1.07319(4) 0.02864(13) Uani 1 d . . . N1 N 0.45061(11) 0.71102(10) 0.83460(9) 0.0221(2) Uani 1 d . . . N2 N 0.72032(11) 1.02447(10) 1.26384(9) 0.0228(2) Uani 1 d . . . O1 O 0.38610(9) 0.92864(8) 1.02983(7) 0.02170(17) Uani 1 d . . . C1 C 0.25832(14) 0.87015(13) 1.06652(12) 0.0243(2) Uani 1 d . . . C2 C 0.25297(15) 0.73537(13) 1.10338(13) 0.0259(3) Uani 1 d . . . C3 C 0.12758(16) 0.68194(14) 1.15740(14) 0.0308(3) Uani 1 d . . . C4 C 0.1420(2) 0.56303(17) 1.21481(17) 0.0436(4) Uani 1 d . . . C5 C 0.30116(14) 0.58414(12) 0.79131(12) 0.0247(2) Uani 1 d . . . C6 C 0.21625(17) 0.50674(15) 0.64518(13) 0.0346(3) Uani 1 d . . . C7 C 0.31928(17) 0.47196(14) 0.86029(14) 0.0322(3) Uani 1 d . . . C8 C 0.56529(14) 0.68103(13) 0.78521(12) 0.0260(3) Uani 1 d . . . C9 C 0.56374(19) 0.72461(18) 0.66388(14) 0.0364(3) Uani 1 d . . . C10 C 0.73395(15) 0.75508(15) 0.88915(14) 0.0306(3) Uani 1 d . . . C11 C 0.65572(15) 0.99002(13) 1.36034(11) 0.0263(3) Uani 1 d . . . C12 C 0.66777(19) 0.85507(16) 1.39297(15) 0.0364(3) Uani 1 d . . . C13 C 0.72343(19) 1.11280(16) 1.48697(13) 0.0369(3) Uani 1 d . . . C14 C 0.89512(14) 1.07332(13) 1.31513(12) 0.0262(3) Uani 1 d . . . C15 C 0.94938(18) 0.97981(16) 1.23592(17) 0.0387(3) Uani 1 d . . . C16 C 0.97776(17) 1.22832(15) 1.32234(16) 0.0359(3) Uani 1 d . . . H1 H 0.2635(16) 0.9403(14) 1.1405(13) 0.026(3) Uiso 1 d . . . H2 H 0.1533(18) 0.8477(14) 0.9958(14) 0.030(3) Uiso 1 d . . . H3 H 0.3583(18) 0.7543(15) 1.1695(14) 0.034(4) Uiso 1 d . . . H4 H 0.2337(17) 0.6597(16) 1.0296(15) 0.036(4) Uiso 1 d . . . H5 H 0.1367(19) 0.7643(17) 1.2266(16) 0.044(4) Uiso 1 d . . . H6 H 0.021(2) 0.6480(17) 1.0890(17) 0.046(4) Uiso 1 d . . . H7 H 0.250(2) 0.5979(18) 1.2835(18) 0.051(5) Uiso 1 d . . . H8 H 0.132(2) 0.481(2) 1.148(2) 0.068(6) Uiso 1 d . . . H9 H 0.062(2) 0.5284(19) 1.2499(17) 0.060(5) Uiso 1 d . . . H10 H 0.2258(15) 0.6176(13) 0.8180(12) 0.022(3) Uiso 1 d . . . H11 H 0.1986(17) 0.5727(16) 0.5984(14) 0.035(4) Uiso 1 d . . . H12 H 0.2793(18) 0.4598(16) 0.6147(15) 0.040(4) Uiso 1 d . . . H13 H 0.111(2) 0.4357(17) 0.6263(15) 0.044(4) Uiso 1 d . . . H14 H 0.3948(19) 0.4348(16) 0.8426(15) 0.041(4) Uiso 1 d . . . H15 H 0.2200(19) 0.3919(17) 0.8279(15) 0.039(4) Uiso 1 d . . . H16 H 0.3578(18) 0.5105(16) 0.9535(16) 0.036(4) Uiso 1 d . . . H17 H 0.5420(15) 0.5768(14) 0.7622(13) 0.025(3) Uiso 1 d . . . H18 H 0.459(2) 0.6771(17) 0.5952(16) 0.044(4) Uiso 1 d . . . H19 H 0.638(2) 0.6987(17) 0.6333(16) 0.050(4) Uiso 1 d . . . H20 H 0.5925(19) 0.8287(18) 0.6830(15) 0.044(4) Uiso 1 d . . . H21 H 0.7449(17) 0.7149(15) 0.9612(15) 0.034(4) Uiso 1 d . . . H22 H 0.7596(18) 0.8602(17) 0.9225(15) 0.040(4) Uiso 1 d . . . H23 H 0.8130(19) 0.7430(16) 0.8567(15) 0.042(4) Uiso 1 d . . . H24 H 0.5366(17) 0.9685(14) 1.3203(13) 0.026(3) Uiso 1 d . . . H25 H 0.781(2) 0.8682(17) 1.4333(16) 0.047(4) Uiso 1 d . . . H26 H 0.6154(19) 0.7719(18) 1.3146(17) 0.044(4) Uiso 1 d . . . H27 H 0.619(2) 0.8329(17) 1.4533(17) 0.049(4) Uiso 1 d . . . H28 H 0.664(2) 1.0876(17) 1.5401(16) 0.047(4) Uiso 1 d . . . H29 H 0.717(2) 1.2033(19) 1.4680(17) 0.054(5) Uiso 1 d . . . H30 H 0.836(2) 1.1325(16) 1.5395(15) 0.043(4) Uiso 1 d . . . H31 H 0.9345(16) 1.0671(14) 1.4038(14) 0.031(4) Uiso 1 d . . . H32 H 1.066(2) 1.0109(17) 1.2733(16) 0.048(4) Uiso 1 d . . . H33 H 0.9122(19) 0.9836(16) 1.1439(17) 0.042(4) Uiso 1 d . . . H34 H 0.905(2) 0.8845(19) 1.2385(16) 0.047(4) Uiso 1 d . . . H35 H 1.092(2) 1.2591(16) 1.3589(15) 0.044(4) Uiso 1 d . . . H36 H 0.9434(19) 1.2382(17) 1.2361(17) 0.044(4) Uiso 1 d . . . H37 H 0.9500(18) 1.2885(17) 1.3742(16) 0.043(4) Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.01934(19) 0.01970(19) 0.01676(19) 0.00658(14) 0.00627(15) 0.00759(14) Na1 0.0320(3) 0.0288(3) 0.0234(3) 0.0067(2) 0.0070(2) 0.0147(2) N1 0.0228(5) 0.0211(5) 0.0236(5) 0.0063(4) 0.0107(4) 0.0089(4) N2 0.0201(5) 0.0291(5) 0.0192(5) 0.0103(4) 0.0059(4) 0.0099(4) O1 0.0188(4) 0.0244(4) 0.0208(4) 0.0074(3) 0.0095(3) 0.0053(3) C1 0.0208(6) 0.0282(6) 0.0264(6) 0.0101(5) 0.0128(5) 0.0085(5) C2 0.0267(6) 0.0246(6) 0.0276(6) 0.0078(5) 0.0143(5) 0.0081(5) C3 0.0319(7) 0.0296(7) 0.0325(7) 0.0109(5) 0.0179(6) 0.0083(5) C4 0.0529(10) 0.0364(8) 0.0507(10) 0.0226(7) 0.0310(9) 0.0137(7) C5 0.0250(6) 0.0226(6) 0.0255(6) 0.0059(5) 0.0102(5) 0.0088(5) C6 0.0329(7) 0.0317(7) 0.0288(7) 0.0020(5) 0.0072(6) 0.0088(6) C7 0.0359(7) 0.0247(6) 0.0372(8) 0.0112(6) 0.0166(6) 0.0102(6) C8 0.0294(6) 0.0258(6) 0.0283(6) 0.0090(5) 0.0149(5) 0.0139(5) C9 0.0362(8) 0.0505(9) 0.0307(7) 0.0154(6) 0.0188(6) 0.0202(7) C10 0.0285(7) 0.0348(7) 0.0358(7) 0.0161(6) 0.0154(6) 0.0161(6) C11 0.0269(6) 0.0322(6) 0.0209(6) 0.0111(5) 0.0091(5) 0.0117(5) C12 0.0417(8) 0.0403(8) 0.0320(7) 0.0205(6) 0.0149(7) 0.0168(6) C13 0.0395(8) 0.0451(8) 0.0230(7) 0.0069(6) 0.0115(6) 0.0160(6) C14 0.0222(6) 0.0334(6) 0.0209(6) 0.0100(5) 0.0046(5) 0.0114(5) C15 0.0270(7) 0.0327(7) 0.0533(10) 0.0071(6) 0.0140(7) 0.0133(6) C16 0.0238(7) 0.0311(7) 0.0448(9) 0.0039(6) 0.0112(6) 0.0076(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 Mg1 O1 2.0216(8) . ? Mg1 O1 2.0320(9) 2_677 ? Mg1 N2 2.0460(10) 2_677 ? Mg1 N1 2.0572(10) . ? Mg1 Na1 2.9692(6) . ? Mg1 Na1 2.9807(6) 2_677 ? Mg1 Mg1 3.1147(7) 2_677 ? Na1 N2 2.4582(11) . ? Na1 N1 2.4803(11) . ? Na1 O1 2.5659(9) . ? Na1 C10 2.9548(14) . ? Na1 Mg1 2.9807(6) 2_677 ? Na1 O1 3.1035(9) 2_677 ? Na1 C15 3.1046(16) . ? Na1 H21 2.578(14) . ? N1 C5 1.4734(15) . ? N1 C8 1.4768(14) . ? N2 C11 1.4740(15) . ? N2 C14 1.4746(15) . ? N2 Mg1 2.0460(10) 2_677 ? O1 C1 1.4167(13) . ? O1 Mg1 2.0320(8) 2_677 ? C1 C2 1.5161(16) . ? C1 H1 0.989(14) . ? C1 H2 1.002(15) . ? C2 C3 1.5236(16) . ? C2 H3 0.991(16) . ? C2 H4 0.967(15) . ? C3 C4 1.517(2) . ? C3 H5 1.014(16) . ? C3 H6 0.978(18) . ? C4 H7 0.988(19) . ? C4 H8 0.99(2) . ? C4 H9 0.978(19) . ? C5 C6 1.5375(18) . ? C5 C7 1.5385(17) . ? C5 H10 1.000(13) . ? C6 H11 0.962(15) . ? C6 H12 0.991(16) . ? C6 H13 0.977(17) . ? C7 H14 0.978(16) . ? C7 H15 0.952(16) . ? C7 H16 0.971(16) . ? C8 C10 1.5240(18) . ? C8 C9 1.5342(18) . ? C8 H17 0.994(13) . ? C9 H18 0.967(18) . ? C9 H19 0.975(17) . ? C9 H20 0.985(17) . ? C10 H21 0.981(15) . ? C10 H22 1.005(16) . ? C10 H23 0.977(16) . ? C11 C12 1.5353(18) . ? C11 C13 1.5386(18) . ? C11 H24 1.024(14) . ? C12 H25 0.991(18) . ? C12 H26 0.983(17) . ? C12 H27 0.969(17) . ? C13 H28 0.975(17) . ? C13 H29 1.012(18) . ? C13 H30 0.990(17) . ? C14 C16 1.5215(18) . ? C14 C15 1.5265(18) . ? C14 H31 0.989(15) . ? C15 H32 0.986(18) . ? C15 H33 1.015(17) . ? C15 H34 0.953(17) . ? C16 H35 0.966(17) . ? C16 H36 0.975(17) . ? C16 H37 0.940(16) . ? 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 O1 79.58(3) . 2_677 ? O1 Mg1 N2 111.84(4) . 2_677 ? O1 Mg1 N2 102.87(4) 2_677 2_677 ? O1 Mg1 N1 104.42(4) . . ? O1 Mg1 N1 111.73(4) 2_677 . ? N2 Mg1 N1 133.44(4) 2_677 . ? O1 Mg1 Na1 58.24(3) . . ? O1 Mg1 Na1 74.06(3) 2_677 . ? N2 Mg1 Na1 169.82(3) 2_677 . ? N1 Mg1 Na1 55.63(3) . . ? O1 Mg1 Na1 73.91(3) . 2_677 ? O1 Mg1 Na1 57.94(3) 2_677 2_677 ? N2 Mg1 Na1 54.82(3) 2_677 2_677 ? N1 Mg1 Na1 169.63(3) . 2_677 ? Na1 Mg1 Na1 116.867(15) . 2_677 ? O1 Mg1 Mg1 39.92(2) . 2_677 ? O1 Mg1 Mg1 39.67(2) 2_677 2_677 ? N2 Mg1 Mg1 112.76(3) 2_677 2_677 ? N1 Mg1 Mg1 113.78(3) . 2_677 ? Na1 Mg1 Mg1 58.614(15) . 2_677 ? Na1 Mg1 Mg1 58.253(14) 2_677 2_677 ? N2 Na1 N1 147.07(4) . . ? N2 Na1 O1 78.76(3) . . ? N1 Na1 O1 79.38(3) . . ? N2 Na1 C10 122.16(4) . . ? N1 Na1 C10 53.16(3) . . ? O1 Na1 C10 121.16(3) . . ? N2 Na1 Mg1 105.74(3) . . ? N1 Na1 Mg1 43.20(2) . . ? O1 Na1 Mg1 42.059(19) . . ? C10 Na1 Mg1 79.46(3) . . ? N2 Na1 Mg1 42.86(2) . 2_677 ? N1 Na1 Mg1 105.95(3) . 2_677 ? O1 Na1 Mg1 42.16(2) . 2_677 ? C10 Na1 Mg1 115.26(3) . 2_677 ? Mg1 Na1 Mg1 63.133(15) . 2_677 ? N2 Na1 O1 73.54(3) . 2_677 ? N1 Na1 O1 73.68(3) . 2_677 ? O1 Na1 O1 53.45(3) . 2_677 ? C10 Na1 O1 78.87(3) . 2_677 ? Mg1 Na1 O1 39.020(17) . 2_677 ? Mg1 Na1 O1 38.748(16) 2_677 2_677 ? N2 Na1 C15 51.65(4) . . ? N1 Na1 C15 127.34(4) . . ? O1 Na1 C15 123.45(4) . . ? C10 Na1 C15 76.18(4) . . ? Mg1 Na1 C15 121.75(4) . . ? Mg1 Na1 C15 81.30(3) 2_677 . ? O1 Na1 C15 84.39(4) 2_677 . ? N2 Na1 H21 121.6(3) . . ? N1 Na1 H21 65.4(3) . . ? O1 Na1 H21 139.6(3) . . ? C10 Na1 H21 18.9(3) . . ? Mg1 Na1 H21 97.6(3) . . ? Mg1 Na1 H21 129.6(3) 2_677 . ? O1 Na1 H21 96.2(3) 2_677 . ? C15 Na1 H21 70.4(3) . . ? C5 N1 C8 112.53(9) . . ? C5 N1 Mg1 110.79(7) . . ? C8 N1 Mg1 127.32(7) . . ? C5 N1 Na1 112.76(7) . . ? C8 N1 Na1 107.50(7) . . ? Mg1 N1 Na1 81.16(3) . . ? C11 N2 C14 112.25(9) . . ? C11 N2 Mg1 112.31(7) . 2_677 ? C14 N2 Mg1 125.32(7) . 2_677 ? C11 N2 Na1 107.47(7) . . ? C14 N2 Na1 112.19(7) . . ? Mg1 N2 Na1 82.32(4) 2_677 . ? C1 O1 Mg1 133.23(7) . . ? C1 O1 Mg1 125.52(7) . 2_677 ? Mg1 O1 Mg1 100.42(3) . 2_677 ? C1 O1 Na1 113.62(6) . . ? Mg1 O1 Na1 79.70(3) . . ? Mg1 O1 Na1 79.90(3) 2_677 . ? O1 C1 C2 113.49(9) . . ? O1 C1 H1 111.2(8) . . ? C2 C1 H1 107.7(8) . . ? O1 C1 H2 111.2(8) . . ? C2 C1 H2 108.3(8) . . ? H1 C1 H2 104.6(11) . . ? C1 C2 C3 113.55(10) . . ? C1 C2 H3 109.2(8) . . ? C3 C2 H3 108.1(8) . . ? C1 C2 H4 110.2(9) . . ? C3 C2 H4 109.0(9) . . ? H3 C2 H4 106.5(12) . . ? C4 C3 C2 112.95(12) . . ? C4 C3 H5 108.7(9) . . ? C2 C3 H5 109.7(9) . . ? C4 C3 H6 109.4(9) . . ? C2 C3 H6 109.4(9) . . ? H5 C3 H6 106.6(13) . . ? C3 C4 H7 108.9(10) . . ? C3 C4 H8 109.4(11) . . ? H7 C4 H8 106.6(15) . . ? C3 C4 H9 113.4(10) . . ? H7 C4 H9 109.5(14) . . ? H8 C4 H9 108.9(16) . . ? N1 C5 C6 116.48(10) . . ? N1 C5 C7 113.13(10) . . ? C6 C5 C7 108.11(10) . . ? N1 C5 H10 106.8(7) . . ? C6 C5 H10 106.8(8) . . ? C7 C5 H10 104.7(7) . . ? C5 C6 H11 110.8(9) . . ? C5 C6 H12 110.6(9) . . ? H11 C6 H12 109.7(12) . . ? C5 C6 H13 109.3(9) . . ? H11 C6 H13 106.1(13) . . ? H12 C6 H13 110.2(13) . . ? C5 C7 H14 110.9(9) . . ? C5 C7 H15 109.7(9) . . ? H14 C7 H15 106.3(13) . . ? C5 C7 H16 112.7(9) . . ? H14 C7 H16 107.0(13) . . ? H15 C7 H16 110.0(12) . . ? N1 C8 C10 110.69(10) . . ? N1 C8 C9 114.03(10) . . ? C10 C8 C9 108.81(11) . . ? N1 C8 H17 110.5(7) . . ? C10 C8 H17 105.9(8) . . ? C9 C8 H17 106.5(8) . . ? C8 C9 H18 110.8(9) . . ? C8 C9 H19 110.7(10) . . ? H18 C9 H19 108.2(14) . . ? C8 C9 H20 109.8(9) . . ? H18 C9 H20 107.6(13) . . ? H19 C9 H20 109.8(13) . . ? C8 C10 Na1 86.71(7) . . ? C8 C10 H21 111.1(9) . . ? Na1 C10 H21 58.3(8) . . ? C8 C10 H22 109.2(9) . . ? Na1 C10 H22 68.9(8) . . ? H21 C10 H22 109.1(12) . . ? C8 C10 H23 112.2(9) . . ? Na1 C10 H23 159.9(9) . . ? H21 C10 H23 106.2(12) . . ? H22 C10 H23 109.0(12) . . ? N2 C11 C12 113.77(10) . . ? N2 C11 C13 115.25(11) . . ? C12 C11 C13 108.80(11) . . ? N2 C11 H24 106.8(7) . . ? C12 C11 H24 106.1(7) . . ? C13 C11 H24 105.3(7) . . ? C11 C12 H25 110.9(9) . . ? C11 C12 H26 110.9(9) . . ? H25 C12 H26 107.5(13) . . ? C11 C12 H27 111.5(10) . . ? H25 C12 H27 107.3(13) . . ? H26 C12 H27 108.6(14) . . ? C11 C13 H28 110.6(10) . . ? C11 C13 H29 110.3(10) . . ? H28 C13 H29 108.8(13) . . ? C11 C13 H30 111.6(9) . . ? H28 C13 H30 106.4(13) . . ? H29 C13 H30 109.0(14) . . ? N2 C14 C16 112.50(10) . . ? N2 C14 C15 112.28(11) . . ? C16 C14 C15 108.52(11) . . ? N2 C14 H31 109.5(8) . . ? C16 C14 H31 107.3(8) . . ? C15 C14 H31 106.5(8) . . ? C14 C15 Na1 83.87(7) . . ? C14 C15 H32 111.5(10) . . ? Na1 C15 H32 164.3(9) . . ? C14 C15 H33 109.3(9) . . ? Na1 C15 H33 65.4(9) . . ? H32 C15 H33 110.0(13) . . ? C14 C15 H34 107.9(10) . . ? Na1 C15 H34 63.6(10) . . ? H32 C15 H34 107.0(13) . . ? H33 C15 H34 111.0(14) . . ? C14 C16 H35 111.1(9) . . ? C14 C16 H36 109.6(10) . . ? H35 C16 H36 109.5(13) . . ? C14 C16 H37 110.0(10) . . ? H35 C16 H37 108.4(14) . . ? H36 C16 H37 108.2(14) . . ? 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 Na1 N2 -52.08(4) . . . . ? O1 Mg1 Na1 N2 35.38(4) 2_677 . . . ? N2 Mg1 Na1 N2 -38.4(2) 2_677 . . . ? N1 Mg1 Na1 N2 166.82(4) . . . . ? Na1 Mg1 Na1 N2 -4.85(3) 2_677 . . . ? Mg1 Mg1 Na1 N2 -4.85(3) 2_677 . . . ? O1 Mg1 Na1 N1 141.10(4) . . . . ? O1 Mg1 Na1 N1 -131.44(4) 2_677 . . . ? N2 Mg1 Na1 N1 154.78(19) 2_677 . . . ? Na1 Mg1 Na1 N1 -171.67(4) 2_677 . . . ? Mg1 Mg1 Na1 N1 -171.67(4) 2_677 . . . ? O1 Mg1 Na1 O1 87.46(4) 2_677 . . . ? N2 Mg1 Na1 O1 13.68(18) 2_677 . . . ? N1 Mg1 Na1 O1 -141.10(4) . . . . ? Na1 Mg1 Na1 O1 47.23(3) 2_677 . . . ? Mg1 Mg1 Na1 O1 47.23(3) 2_677 . . . ? O1 Mg1 Na1 C10 -172.75(4) . . . . ? O1 Mg1 Na1 C10 -85.29(4) 2_677 . . . ? N2 Mg1 Na1 C10 -159.06(18) 2_677 . . . ? N1 Mg1 Na1 C10 46.15(4) . . . . ? Na1 Mg1 Na1 C10 -125.51(3) 2_677 . . . ? Mg1 Mg1 Na1 C10 -125.51(3) 2_677 . . . ? O1 Mg1 Na1 Mg1 -47.23(3) . . . 2_677 ? O1 Mg1 Na1 Mg1 40.23(2) 2_677 . . 2_677 ? N2 Mg1 Na1 Mg1 -33.55(18) 2_677 . . 2_677 ? N1 Mg1 Na1 Mg1 171.67(4) . . . 2_677 ? Na1 Mg1 Na1 Mg1 0.0 2_677 . . 2_677 ? O1 Mg1 Na1 O1 -87.46(4) . . . 2_677 ? N2 Mg1 Na1 O1 -73.78(18) 2_677 . . 2_677 ? N1 Mg1 Na1 O1 131.44(4) . . . 2_677 ? Na1 Mg1 Na1 O1 -40.23(2) 2_677 . . 2_677 ? Mg1 Mg1 Na1 O1 -40.23(2) 2_677 . . 2_677 ? O1 Mg1 Na1 C15 -106.37(4) . . . . ? O1 Mg1 Na1 C15 -18.91(4) 2_677 . . . ? N2 Mg1 Na1 C15 -92.69(19) 2_677 . . . ? N1 Mg1 Na1 C15 112.53(5) . . . . ? Na1 Mg1 Na1 C15 -59.14(4) 2_677 . . . ? Mg1 Mg1 Na1 C15 -59.14(4) 2_677 . . . ? O1 Mg1 N1 C5 77.63(8) . . . . ? O1 Mg1 N1 C5 161.98(7) 2_677 . . . ? N2 Mg1 N1 C5 -62.96(9) 2_677 . . . ? Na1 Mg1 N1 C5 111.08(8) . . . . ? Na1 Mg1 N1 C5 157.00(15) 2_677 . . . ? Mg1 Mg1 N1 C5 118.85(7) 2_677 . . . ? O1 Mg1 N1 C8 -138.78(9) . . . . ? O1 Mg1 N1 C8 -54.43(10) 2_677 . . . ? N2 Mg1 N1 C8 80.63(11) 2_677 . . . ? Na1 Mg1 N1 C8 -105.32(10) . . . . ? Na1 Mg1 N1 C8 -59.4(2) 2_677 . . . ? Mg1 Mg1 N1 C8 -97.55(9) 2_677 . . . ? O1 Mg1 N1 Na1 -33.46(4) . . . . ? O1 Mg1 N1 Na1 50.89(4) 2_677 . . . ? N2 Mg1 N1 Na1 -174.05(5) 2_677 . . . ? Na1 Mg1 N1 Na1 45.92(18) 2_677 . . . ? Mg1 Mg1 N1 Na1 7.77(4) 2_677 . . . ? N2 Na1 N1 C5 -132.73(8) . . . . ? O1 Na1 N1 C5 -83.58(7) . . . . ? C10 Na1 N1 C5 133.45(8) . . . . ? Mg1 Na1 N1 C5 -108.92(8) . . . . ? Mg1 Na1 N1 C5 -116.65(7) 2_677 . . . ? O1 Na1 N1 C5 -138.38(7) 2_677 . . . ? C15 Na1 N1 C5 152.20(7) . . . . ? N2 Na1 N1 C8 102.66(9) . . . . ? O1 Na1 N1 C8 151.81(7) . . . . ? C10 Na1 N1 C8 8.84(7) . . . . ? Mg1 Na1 N1 C8 126.47(8) . . . . ? Mg1 Na1 N1 C8 118.74(7) 2_677 . . . ? O1 Na1 N1 C8 97.01(7) 2_677 . . . ? C15 Na1 N1 C8 27.59(9) . . . . ? N2 Na1 N1 Mg1 -23.80(8) . . . . ? O1 Na1 N1 Mg1 25.34(3) . . . . ? C10 Na1 N1 Mg1 -117.63(5) . . . . ? Mg1 Na1 N1 Mg1 -7.73(3) 2_677 . . . ? O1 Na1 N1 Mg1 -29.46(2) 2_677 . . . ? C15 Na1 N1 Mg1 -98.88(5) . . . . ? N1 Na1 N2 C11 134.09(8) . . . . ? O1 Na1 N2 C11 84.80(7) . . . . ? C10 Na1 N2 C11 -155.31(7) . . . . ? Mg1 Na1 N2 C11 117.40(7) . . . . ? Mg1 Na1 N2 C11 111.05(8) 2_677 . . . ? O1 Na1 N2 C11 139.75(7) 2_677 . . . ? C15 Na1 N2 C11 -124.30(9) . . . . ? N1 Na1 N2 C14 -102.06(9) . . . . ? O1 Na1 N2 C14 -151.34(7) . . . . ? C10 Na1 N2 C14 -31.45(9) . . . . ? Mg1 Na1 N2 C14 -118.74(7) . . . . ? Mg1 Na1 N2 C14 -125.10(8) 2_677 . . . ? O1 Na1 N2 C14 -96.40(7) 2_677 . . . ? C15 Na1 N2 C14 -0.44(7) . . . . ? N1 Na1 N2 Mg1 23.04(8) . . . 2_677 ? O1 Na1 N2 Mg1 -26.24(3) . . . 2_677 ? C10 Na1 N2 Mg1 93.65(4) . . . 2_677 ? Mg1 Na1 N2 Mg1 6.36(4) . . . 2_677 ? O1 Na1 N2 Mg1 28.70(3) 2_677 . . 2_677 ? C15 Na1 N2 Mg1 124.66(6) . . . 2_677 ? O1 Mg1 O1 C1 169.56(11) 2_677 . . . ? N2 Mg1 O1 C1 69.75(10) 2_677 . . . ? N1 Mg1 O1 C1 -80.47(10) . . . . ? Na1 Mg1 O1 C1 -112.83(10) . . . . ? Na1 Mg1 O1 C1 110.14(10) 2_677 . . . ? Mg1 Mg1 O1 C1 169.56(11) 2_677 . . . ? N2 Mg1 O1 Mg1 -99.81(4) 2_677 . . 2_677 ? N1 Mg1 O1 Mg1 109.97(4) . . . 2_677 ? Na1 Mg1 O1 Mg1 77.61(3) . . . 2_677 ? Na1 Mg1 O1 Mg1 -59.43(3) 2_677 . . 2_677 ? O1 Mg1 O1 Na1 -77.61(3) 2_677 . . . ? N2 Mg1 O1 Na1 -177.42(4) 2_677 . . . ? N1 Mg1 O1 Na1 32.36(4) . . . . ? Na1 Mg1 O1 Na1 -137.03(2) 2_677 . . . ? Mg1 Mg1 O1 Na1 -77.61(3) 2_677 . . . ? N2 Na1 O1 C1 -97.86(7) . . . . ? N1 Na1 O1 C1 106.93(7) . . . . ? C10 Na1 O1 C1 141.21(7) . . . . ? Mg1 Na1 O1 C1 132.87(8) . . . . ? Mg1 Na1 O1 C1 -124.48(8) 2_677 . . . ? O1 Na1 O1 C1 -175.60(9) 2_677 . . . ? C15 Na1 O1 C1 -125.06(8) . . . . ? N2 Na1 O1 Mg1 129.27(3) . . . . ? N1 Na1 O1 Mg1 -25.94(3) . . . . ? C10 Na1 O1 Mg1 8.34(5) . . . . ? Mg1 Na1 O1 Mg1 102.65(3) 2_677 . . . ? O1 Na1 O1 Mg1 51.53(3) 2_677 . . . ? C15 Na1 O1 Mg1 102.07(5) . . . . ? N2 Na1 O1 Mg1 26.62(3) . . . 2_677 ? N1 Na1 O1 Mg1 -128.59(3) . . . 2_677 ? C10 Na1 O1 Mg1 -94.31(4) . . . 2_677 ? Mg1 Na1 O1 Mg1 -102.65(3) . . . 2_677 ? O1 Na1 O1 Mg1 -51.12(3) 2_677 . . 2_677 ? C15 Na1 O1 Mg1 -0.58(5) . . . 2_677 ? Mg1 O1 C1 C2 89.00(12) . . . . ? Mg1 O1 C1 C2 -103.64(10) 2_677 . . . ? Na1 O1 C1 C2 -9.23(12) . . . . ? O1 C1 C2 C3 173.42(10) . . . . ? C1 C2 C3 C4 -170.19(12) . . . . ? C8 N1 C5 C6 -52.64(14) . . . . ? Mg1 N1 C5 C6 96.64(11) . . . . ? Na1 N1 C5 C6 -174.45(9) . . . . ? C8 N1 C5 C7 73.54(12) . . . . ? Mg1 N1 C5 C7 -137.18(9) . . . . ? Na1 N1 C5 C7 -48.27(11) . . . . ? C5 N1 C8 C10 -139.51(10) . . . . ? Mg1 N1 C8 C10 77.41(12) . . . . ? Na1 N1 C8 C10 -14.76(11) . . . . ? C5 N1 C8 C9 97.42(13) . . . . ? Mg1 N1 C8 C9 -45.67(14) . . . . ? Na1 N1 C8 C9 -137.84(10) . . . . ? N1 C8 C10 Na1 11.79(9) . . . . ? C9 C8 C10 Na1 137.84(9) . . . . ? N2 Na1 C10 C8 -148.33(7) . . . . ? N1 Na1 C10 C8 -8.18(6) . . . . ? O1 Na1 C10 C8 -51.94(8) . . . . ? Mg1 Na1 C10 C8 -46.27(7) . . . . ? Mg1 Na1 C10 C8 -99.68(7) 2_677 . . . ? O1 Na1 C10 C8 -86.02(7) 2_677 . . . ? C15 Na1 C10 C8 -172.92(8) . . . . ? C14 N2 C11 C12 -69.58(13) . . . . ? Mg1 N2 C11 C12 142.97(9) 2_677 . . . ? Na1 N2 C11 C12 54.24(12) . . . . ? C14 N2 C11 C13 57.07(14) . . . . ? Mg1 N2 C11 C13 -90.38(11) 2_677 . . . ? Na1 N2 C11 C13 -179.10(9) . . . . ? C11 N2 C14 C16 -115.33(12) . . . . ? Mg1 N2 C14 C16 27.09(14) 2_677 . . . ? Na1 N2 C14 C16 123.52(10) . . . . ? C11 N2 C14 C15 121.91(12) . . . . ? Mg1 N2 C14 C15 -95.68(12) 2_677 . . . ? Na1 N2 C14 C15 0.76(12) . . . . ? N2 C14 C15 Na1 -0.56(9) . . . . ? C16 C14 C15 Na1 -125.54(9) . . . . ? N2 Na1 C15 C14 0.40(7) . . . . ? N1 Na1 C15 C14 138.34(7) . . . . ? O1 Na1 C15 C14 35.27(10) . . . . ? C10 Na1 C15 C14 153.71(9) . . . . ? Mg1 Na1 C15 C14 85.65(8) . . . . ? Mg1 Na1 C15 C14 34.88(7) 2_677 . . . ? O1 Na1 C15 C14 73.82(8) 2_677 . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.225 _refine_diff_density_min -0.159 _refine_diff_density_rms 0.034 #===END #---------------------------------------------------------------------- #----- #-------------------------------Compound 2----------------------------- #------ #---------------------------------------------------------------------- #---- data_import _database_code_CSD 182084 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H90 Mg2 N4 Na2 O2' _chemical_formula_weight 753.76 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 monoclinic _symmetry_space_group_name_H-M P21/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 10.7260(4) _cell_length_b 13.8181(4) _cell_length_c 16.5769(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.680(1) _cell_angle_gamma 90.00 _cell_volume 2428.77(14) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 'all' _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 25.00 _exptl_crystal_description 'cut prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.031 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 0.101 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18646 _diffrn_reflns_av_R_equivalents 0.150 _diffrn_reflns_av_sigmaI/netI 0.0863 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4218 _reflns_number_gt 3614 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Denzo and Collect' _computing_cell_refinement 'Denzo and Collect' _computing_data_reduction 'Denzo and Denzox' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; The C and H atoms of one NPr2 ligand are modeled as disordered over 2 sites each. An overall occupancy factor was refined for each grouping so as to total 100 percent occupancy. 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 w=1/[\s^2^(Fo^2^)+(0.0780P)^2^+1.1041P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4218 _refine_ls_number_parameters 260 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0724 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1814 _refine_ls_wR_factor_gt 0.1719 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na 0.49531(9) 1.12569(6) 0.11171(5) 0.0424(3) Uani 1 d . . . Mg1 Mg 0.41253(6) 0.93214(5) 0.04065(4) 0.0316(2) Uani 1 d . . . O1 O 0.59514(13) 0.94185(10) 0.02251(9) 0.0339(4) Uani 1 d . . . N1 N 0.34210(17) 0.81783(12) -0.03106(11) 0.0372(5) Uani 1 d . . . N2 N 0.39276(19) 0.97779(14) 0.15514(12) 0.0418(5) Uani 1 d . . . C1 C 0.7069(2) 0.89663(15) 0.06030(15) 0.0394(5) Uani 1 d . . . H1A H 0.7125 0.9038 0.1202 0.047 Uiso 1 calc R . . H1B H 0.7800 0.9309 0.0436 0.047 Uiso 1 calc R . . C2 C 0.7168(2) 0.79145(17) 0.04076(16) 0.0470(6) Uani 1 d . . . H2A H 0.7157 0.7842 -0.0188 0.056 Uiso 1 calc R . . H2B H 0.6421 0.7573 0.0552 0.056 Uiso 1 calc R . . C3 C 0.8350(2) 0.74383(17) 0.08517(16) 0.0445(6) Uani 1 d . . . H3A H 0.9091 0.7732 0.0656 0.053 Uiso 1 calc R . . H3B H 0.8412 0.7586 0.1441 0.053 Uiso 1 calc R . . C4 C 0.8415(2) 0.63535(17) 0.07499(18) 0.0508(6) Uani 1 d . . . H4A H 0.7662 0.6054 0.0926 0.061 Uiso 1 calc R . . H4B H 0.8401 0.6200 0.0165 0.061 Uiso 1 calc R . . C5 C 0.9587(2) 0.59206(17) 0.12372(18) 0.0488(6) Uani 1 d . . . H5A H 1.0333 0.6203 0.1038 0.059 Uiso 1 calc R . . H5B H 0.9621 0.6118 0.1814 0.059 Uiso 1 calc R . . C6 C 0.9691(3) 0.48327(18) 0.12069(19) 0.0549(7) Uani 1 d . . . H6A H 0.9653 0.4626 0.0632 0.066 Uiso 1 calc R . . H6B H 0.8962 0.4542 0.1419 0.066 Uiso 1 calc R . . C7 C 1.0908(3) 0.44543(19) 0.1702(2) 0.0611(8) Uani 1 d . . . H7A H 1.1633 0.4735 0.1478 0.073 Uiso 1 calc R . . H7B H 1.0955 0.4684 0.2272 0.073 Uiso 1 calc R . . C8 C 1.1029(3) 0.3379(2) 0.1709(2) 0.0714(9) Uani 1 d . . . H8A H 1.0340 0.3094 0.1956 0.107 Uiso 1 calc R . . H8B H 1.1839 0.3194 0.2028 0.107 Uiso 1 calc R . . H8C H 1.0988 0.3143 0.1148 0.107 Uiso 1 calc R . . C9 C 0.1103(2) 0.8576(2) -0.0568(2) 0.0621(8) Uani 1 d . . . H9A H 0.0960 0.8256 -0.0063 0.093 Uiso 1 calc R . . H9B H 0.0350 0.8507 -0.0980 0.093 Uiso 1 calc R . . H9C H 0.1276 0.9264 -0.0462 0.093 Uiso 1 calc R . . C10 C 0.2228(2) 0.81095(18) -0.08804(16) 0.0487(6) Uani 1 d . . . H10 H 0.2031 0.7406 -0.0967 0.058 Uiso 1 calc R . . C11 C 0.2359(3) 0.8540(2) -0.17011(18) 0.0649(8) Uani 1 d . . . H11A H 0.2625 0.9217 -0.1631 0.097 Uiso 1 calc R . . H11B H 0.1546 0.8506 -0.2060 0.097 Uiso 1 calc R . . H11C H 0.2991 0.8174 -0.1945 0.097 Uiso 1 calc R . . C12 C 0.2705(3) 0.68472(19) 0.05899(18) 0.0557(7) Uani 1 d . . . H12A H 0.2473 0.7336 0.0969 0.084 Uiso 1 calc R . . H12B H 0.3028 0.6270 0.0896 0.084 Uiso 1 calc R . . H12C H 0.1961 0.6674 0.0198 0.084 Uiso 1 calc R . . C13 C 0.3724(2) 0.72550(16) 0.01330(15) 0.0431(6) Uani 1 d . . . H13 H 0.4463 0.7399 0.0561 0.052 Uiso 1 calc R . . C14 C 0.4169(3) 0.64606(17) -0.04047(17) 0.0512(6) Uani 1 d . . . H14A H 0.3494 0.6312 -0.0855 0.077 Uiso 1 calc R . . H14B H 0.4383 0.5877 -0.0077 0.077 Uiso 1 calc R . . H14C H 0.4916 0.6686 -0.0626 0.077 Uiso 1 calc R . . C15 C 0.2544(9) 1.1025(6) 0.2105(6) 0.0606(18) Uani 0.720(8) d P A 1 H15A H 0.1676 1.1263 0.2070 0.091 Uiso 0.720(8) calc PR A 1 H15B H 0.3083 1.1542 0.1946 0.091 Uiso 0.720(8) calc PR A 1 H15C H 0.2852 1.0824 0.2667 0.091 Uiso 0.720(8) calc PR A 1 C16 C 0.2574(4) 1.0159(3) 0.1531(3) 0.0458(11) Uani 0.720(8) d P A 1 H16 H 0.2294 1.0405 0.0965 0.055 Uiso 0.720(8) calc PR A 1 C17 C 0.1618(5) 0.9391(4) 0.1691(4) 0.0562(13) Uani 0.720(8) d P A 1 H17A H 0.1670 0.8838 0.1328 0.084 Uiso 0.720(8) calc PR A 1 H17B H 0.0767 0.9666 0.1589 0.084 Uiso 0.720(8) calc PR A 1 H17C H 0.1805 0.9177 0.2260 0.084 Uiso 0.720(8) calc PR A 1 C18 C 0.4907(6) 0.8358(4) 0.2275(4) 0.0548(13) Uani 0.720(8) d P A 1 H18A H 0.4206 0.7921 0.2082 0.082 Uiso 0.720(8) calc PR A 1 H18B H 0.5320 0.8147 0.2814 0.082 Uiso 0.720(8) calc PR A 1 H18C H 0.5517 0.8349 0.1891 0.082 Uiso 0.720(8) calc PR A 1 C19 C 0.4401(5) 0.9387(2) 0.2336(2) 0.0442(11) Uani 0.720(8) d P A 1 H19 H 0.3688 0.9360 0.2660 0.053 Uiso 0.720(8) calc PR A 1 C20 C 0.5470(10) 0.9971(7) 0.2826(7) 0.0576(19) Uani 0.720(8) d P A 1 H20A H 0.6165 1.0039 0.2508 0.086 Uiso 0.720(8) calc PR A 1 H20B H 0.5772 0.9635 0.3339 0.086 Uiso 0.720(8) calc PR A 1 H20C H 0.5157 1.0614 0.2945 0.086 Uiso 0.720(8) calc PR A 1 C15A C 0.261(3) 1.111(2) 0.1917(16) 0.062(7) Uiso 0.280(8) d P A 2 H15D H 0.3315 1.1478 0.2212 0.093 Uiso 0.280(8) calc PR A 2 H15E H 0.1854 1.1214 0.2174 0.093 Uiso 0.280(8) calc PR A 2 H15F H 0.2444 1.1328 0.1349 0.093 Uiso 0.280(8) calc PR A 2 C16A C 0.2947(9) 1.0003(7) 0.1943(8) 0.040(2) Uiso 0.280(8) d P A 2 H16A H 0.3084 0.9754 0.2516 0.048 Uiso 0.280(8) calc PR A 2 C17A C 0.1722(16) 0.9572(12) 0.1446(10) 0.059(5) Uiso 0.280(8) d P A 2 H17D H 0.1801 0.8866 0.1419 0.089 Uiso 0.280(8) calc PR A 2 H17E H 0.1600 0.9840 0.0893 0.089 Uiso 0.280(8) calc PR A 2 H17F H 0.0997 0.9737 0.1715 0.089 Uiso 0.280(8) calc PR A 2 C18A C 0.4607(16) 0.8278(12) 0.2441(10) 0.051(4) Uiso 0.280(8) d P A 2 H18D H 0.4521 0.7848 0.1966 0.077 Uiso 0.280(8) calc PR A 2 H18E H 0.3790 0.8339 0.2634 0.077 Uiso 0.280(8) calc PR A 2 H18F H 0.5227 0.8008 0.2878 0.077 Uiso 0.280(8) calc PR A 2 C19A C 0.5047(13) 0.9277(7) 0.2201(7) 0.046(3) Uiso 0.280(8) d P A 2 H19A H 0.5813 0.9196 0.1931 0.055 Uiso 0.280(8) calc PR A 2 C20A C 0.535(4) 1.002(3) 0.293(3) 0.107(15) Uiso 0.280(8) d P A 2 H20D H 0.5663 1.0626 0.2719 0.160 Uiso 0.280(8) calc PR A 2 H20E H 0.6000 0.9749 0.3345 0.160 Uiso 0.280(8) calc PR A 2 H20F H 0.4586 1.0151 0.3162 0.160 Uiso 0.280(8) 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 Na1 0.0489(6) 0.0409(5) 0.0382(5) -0.0037(4) 0.0092(4) -0.0081(4) Mg1 0.0310(4) 0.0319(4) 0.0315(4) -0.0001(3) 0.0036(3) -0.0016(3) O1 0.0305(7) 0.0333(8) 0.0373(9) 0.0031(6) 0.0037(6) 0.0018(6) N1 0.0369(10) 0.0332(9) 0.0396(11) 0.0017(8) -0.0006(8) -0.0044(7) N2 0.0484(11) 0.0420(11) 0.0366(11) -0.0013(8) 0.0118(9) -0.0018(9) C1 0.0332(11) 0.0371(12) 0.0459(14) 0.0043(10) -0.0001(10) 0.0033(9) C2 0.0379(13) 0.0436(13) 0.0562(16) -0.0032(11) -0.0031(11) 0.0074(10) C3 0.0338(12) 0.0419(13) 0.0570(15) -0.0016(11) 0.0040(11) 0.0039(10) C4 0.0459(14) 0.0434(13) 0.0603(17) -0.0033(11) -0.0015(12) 0.0078(11) C5 0.0368(12) 0.0431(13) 0.0658(17) -0.0016(12) 0.0050(12) 0.0056(10) C6 0.0529(15) 0.0412(13) 0.0675(18) -0.0024(12) -0.0007(13) 0.0053(11) C7 0.0492(15) 0.0465(15) 0.084(2) -0.0041(14) -0.0009(14) 0.0055(12) C8 0.072(2) 0.0529(16) 0.084(2) 0.0056(15) -0.0040(17) 0.0126(14) C9 0.0360(13) 0.0586(17) 0.086(2) -0.0060(15) -0.0080(13) -0.0027(11) C10 0.0463(14) 0.0455(13) 0.0499(15) -0.0007(11) -0.0073(11) -0.0060(11) C11 0.0664(18) 0.0626(18) 0.0580(18) 0.0121(14) -0.0155(14) -0.0069(14) C12 0.0587(16) 0.0502(15) 0.0577(17) 0.0094(12) 0.0067(13) -0.0080(12) C13 0.0452(13) 0.0385(12) 0.0451(14) 0.0032(10) 0.0051(11) -0.0038(10) C14 0.0571(16) 0.0364(12) 0.0590(17) -0.0019(11) 0.0051(13) 0.0014(11) C15 0.076(4) 0.048(3) 0.062(4) 0.000(3) 0.020(4) 0.013(2) C16 0.040(2) 0.053(2) 0.046(3) -0.0024(17) 0.0116(18) 0.0002(16) C17 0.043(2) 0.068(3) 0.058(3) 0.001(3) 0.010(2) -0.0019(19) C18 0.059(3) 0.053(3) 0.053(3) 0.010(2) 0.010(2) 0.010(2) C19 0.051(3) 0.047(2) 0.0349(18) 0.0012(14) 0.0065(16) 0.0002(16) C20 0.052(3) 0.060(3) 0.055(3) -0.005(2) -0.008(3) -0.015(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 Na1 O1 2.4722(17) 3_675 ? Na1 N1 2.478(2) 3_675 ? Na1 N2 2.479(2) . ? Na1 C11 2.913(3) 3_675 ? Na1 Mg1 2.9578(11) 3_675 ? Na1 Mg1 3.0021(11) . ? Na1 O1 3.2037(16) . ? Mg1 O1 2.0270(15) 3_675 ? Mg1 O1 2.0304(15) . ? Mg1 N2 2.041(2) . ? Mg1 N1 2.0513(19) . ? Mg1 Na1 2.9578(11) 3_675 ? Mg1 Mg1 3.1012(13) 3_675 ? O1 C1 1.412(2) . ? O1 Mg1 2.0270(15) 3_675 ? O1 Na1 2.4721(17) 3_675 ? N1 C10 1.475(3) . ? N1 C13 1.484(3) . ? N1 Na1 2.478(2) 3_675 ? N2 C16A 1.354(9) . ? N2 C19 1.429(4) . ? N2 C16 1.540(4) . ? N2 C19A 1.640(11) . ? C1 C2 1.496(3) . ? C2 C3 1.517(3) . ? C3 C4 1.511(3) . ? C4 C5 1.511(3) . ? C5 C6 1.509(3) . ? C6 C7 1.526(4) . ? C7 C8 1.491(4) . ? C9 C10 1.526(4) . ? C10 C11 1.510(4) . ? C12 C13 1.528(3) . ? C13 C14 1.535(3) . ? C15 C16 1.534(9) . ? C16 C17 1.525(7) . ? C18 C19 1.530(7) . ? C19 C20 1.531(8) . ? C15A C16A 1.57(3) . ? C16A C17A 1.56(2) . ? C18A C19A 1.531(18) . ? C19A C20A 1.58(4) . ? 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 N1 81.13(6) 3_675 3_675 ? O1 Na1 N2 79.58(6) 3_675 . ? N1 Na1 N2 142.71(7) 3_675 . ? O1 Na1 C11 124.74(8) 3_675 3_675 ? N1 Na1 C11 53.64(7) 3_675 3_675 ? N2 Na1 C11 116.32(8) . 3_675 ? O1 Na1 Mg1 42.76(4) 3_675 3_675 ? N1 Na1 Mg1 43.23(5) 3_675 3_675 ? N2 Na1 Mg1 104.21(5) . 3_675 ? C11 Na1 Mg1 82.43(7) 3_675 3_675 ? O1 Na1 Mg1 42.09(4) 3_675 . ? N1 Na1 Mg1 105.04(5) 3_675 . ? N2 Na1 Mg1 42.40(5) . . ? C11 Na1 Mg1 115.83(7) 3_675 . ? Mg1 Na1 Mg1 62.71(3) 3_675 . ? O1 Na1 O1 53.01(5) 3_675 . ? N1 Na1 O1 71.90(5) 3_675 . ? N2 Na1 O1 70.98(5) . . ? C11 Na1 O1 81.20(7) 3_675 . ? Mg1 Na1 O1 38.15(3) 3_675 . ? Mg1 Na1 O1 38.02(3) . . ? O1 Mg1 O1 80.30(6) 3_675 . ? O1 Mg1 N2 102.30(7) 3_675 . ? O1 Mg1 N2 110.81(8) . . ? O1 Mg1 N1 112.29(7) 3_675 . ? O1 Mg1 N1 104.13(7) . . ? N2 Mg1 N1 134.10(8) . . ? O1 Mg1 Na1 77.51(5) 3_675 3_675 ? O1 Mg1 Na1 55.75(5) . 3_675 ? N2 Mg1 Na1 166.53(7) . 3_675 ? N1 Mg1 Na1 55.83(6) . 3_675 ? O1 Mg1 Na1 54.83(5) 3_675 . ? O1 Mg1 Na1 76.38(5) . . ? N2 Mg1 Na1 54.97(6) . . ? N1 Mg1 Na1 167.06(6) . . ? Na1 Mg1 Na1 117.29(3) 3_675 . ? O1 Mg1 Mg1 40.19(4) 3_675 3_675 ? O1 Mg1 Mg1 40.11(4) . 3_675 ? N2 Mg1 Mg1 111.83(6) . 3_675 ? N1 Mg1 Mg1 114.07(6) . 3_675 ? Na1 Mg1 Mg1 59.35(3) 3_675 3_675 ? Na1 Mg1 Mg1 57.95(3) . 3_675 ? C1 O1 Mg1 125.09(13) . 3_675 ? C1 O1 Mg1 132.73(14) . . ? Mg1 O1 Mg1 99.70(6) 3_675 . ? C1 O1 Na1 115.08(13) . 3_675 ? Mg1 O1 Na1 83.08(6) 3_675 3_675 ? Mg1 O1 Na1 81.49(5) . 3_675 ? C1 O1 Na1 117.82(12) . . ? Mg1 O1 Na1 64.34(4) 3_675 . ? Mg1 O1 Na1 65.60(4) . . ? Na1 O1 Na1 126.99(5) 3_675 . ? C10 N1 C13 111.47(17) . . ? C10 N1 Mg1 128.98(15) . . ? C13 N1 Mg1 109.93(14) . . ? C10 N1 Na1 106.74(15) . 3_675 ? C13 N1 Na1 114.75(14) . 3_675 ? Mg1 N1 Na1 80.94(6) . 3_675 ? C16A N2 C19 81.1(5) . . ? C16A N2 C16 30.0(5) . . ? C19 N2 C16 110.7(3) . . ? C16A N2 C19A 109.1(6) . . ? C19 N2 C19A 28.2(4) . . ? C16 N2 C19A 138.9(5) . . ? C16A N2 Mg1 135.6(5) . . ? C19 N2 Mg1 131.1(2) . . ? C16 N2 Mg1 108.3(2) . . ? C19A N2 Mg1 108.2(5) . . ? C16A N2 Na1 111.2(4) . . ? C19 N2 Na1 117.62(19) . . ? C16 N2 Na1 99.80(17) . . ? C19A N2 Na1 103.0(4) . . ? Mg1 N2 Na1 82.63(7) . . ? O1 C1 C2 114.65(18) . . ? C1 C2 C3 113.44(19) . . ? C4 C3 C2 115.2(2) . . ? C5 C4 C3 112.5(2) . . ? C6 C5 C4 115.9(2) . . ? C5 C6 C7 112.6(2) . . ? C8 C7 C6 114.3(2) . . ? N1 C10 C11 111.2(2) . . ? N1 C10 C9 114.2(2) . . ? C11 C10 C9 109.0(2) . . ? N1 C13 C12 116.3(2) . . ? N1 C13 C14 113.03(19) . . ? C12 C13 C14 109.4(2) . . ? C17 C16 C15 110.9(5) . . ? C17 C16 N2 114.5(3) . . ? C15 C16 N2 111.1(4) . . ? N2 C19 C18 111.9(4) . . ? N2 C19 C20 114.8(5) . . ? C18 C19 C20 106.3(6) . . ? N2 C16A C17A 108.2(10) . . ? N2 C16A C15A 113.8(11) . . ? C17A C16A C15A 100.7(14) . . ? C18A C19A C20A 115.2(18) . . ? C18A C19A N2 109.1(10) . . ? C20A C19A N2 105.8(16) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.418 _refine_diff_density_min -0.235 _refine_diff_density_rms 0.049 #===END