# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 #data_c:\windows\desktop\lf0503\ibam data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Richard Layfield' _publ_contact_author_address ; Department of Chemistry University of Cambridge Lensfield Road Cambridge CB2 1EW UNITED KINGDOM ; _publ_contact_author_email ral34@cam.ac.uk _publ_section_title ; The cationic cluster Grignard [{MgCl(thf)2}3(mu3-C3H5)2]+ ; loop_ _publ_author_name 'Richard A. Layfield' 'Thomas H. Bullock' 'Felipe Garcia' 'Simon M. Humphrey' 'Peter Schuler' data_c:\windows\desktop\lf0503\ibam _database_code_depnum_ccdc_archive 'CCDC 298100' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C30 H58 Cl3 Mg3 O6), C12 H20 Mg1' _chemical_formula_sum 'C72 H136 Cl6 Mg7 O12' _chemical_formula_weight 1576.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'I b a m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1, y+1, -z+1/2' 'x+1, -y+1, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'x, -y, z+1/2' '-x, y, z+1/2' _cell_length_a 22.2467(4) _cell_length_b 24.4885(5) _cell_length_c 19.6433(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10701.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 230(2) _cell_measurement_reflns_used 23882 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.979 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3400 _exptl_absorpt_coefficient_mu 0.244 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.836 _exptl_absorpt_correction_T_max 0.949 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 230(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 27938 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.60 _diffrn_reflns_theta_max 24.00 _reflns_number_total 4290 _reflns_number_gt 3116 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4290 _refine_ls_number_parameters 251 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1257 _refine_ls_R_factor_gt 0.1067 _refine_ls_wR_factor_ref 0.3278 _refine_ls_wR_factor_gt 0.3094 _refine_ls_goodness_of_fit_ref 1.321 _refine_ls_restrained_S_all 1.324 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.27013(7) 0.19731(6) 0.42552(7) 0.0602(6) Uani 1 1 d . . . Mg2 Mg 0.22291(10) 0.29213(8) 0.5000 0.0600(7) Uani 1 2 d S . . Cl1 Cl 0.22660(6) 0.28198(5) 0.37276(6) 0.0693(5) Uani 1 1 d . . . Cl2 Cl 0.30905(9) 0.12265(6) 0.5000 0.0751(6) Uani 1 2 d S . . C1 C 0.2047(2) 0.20862(16) 0.5000 0.0318(10) Uani 1 2 d S . . H1A H 0.2237 0.1950 0.4577 0.038 Uiso 1 1 calc R A 1 C2 C 0.1467(4) 0.1842(3) 0.5000 0.083(2) Uani 0.42(2) 2 d SP B 1 H2 H 0.1125 0.2067 0.5000 0.099 Uiso 0.42(2) 2 calc SPR B 1 C3 C 0.1395(10) 0.1285(7) 0.5000 0.082(7) Uani 0.42(2) 2 d SP B 1 H3A H 0.1734 0.1056 0.5000 0.098 Uiso 0.42(2) 2 calc SPR B 1 H3B H 0.1007 0.1133 0.5000 0.098 Uiso 0.42(2) 2 calc SPR B 1 C2' C 0.1467(4) 0.1842(3) 0.5000 0.083(2) Uani 0.58(2) 2 d SP B -2 H2' H 0.1350 0.1621 0.5368 0.099 Uiso 0.289(11) 1 calc PR B -2 C3' C 0.1093(13) 0.1921(10) 0.4495(17) 0.141(12) Uani 0.289(11) 1 d P B -2 H3'A H 0.1207 0.2141 0.4125 0.212 Uiso 0.289(11) 1 calc PR B -2 H3'B H 0.0711 0.1757 0.4502 0.212 Uiso 0.289(11) 1 calc PR B -2 C4 C 0.3042(2) 0.24969(16) 0.5000 0.0301(10) Uani 1 2 d S . . H4A H 0.3002 0.2302 0.4567 0.036 Uiso 0.50 1 calc PR C -1 H4B H 0.2764 0.2806 0.4978 0.036 Uiso 1 2 calc SR C -1 C5 C 0.3597(5) 0.2713(4) 0.5000 0.109(3) Uani 1 2 d S . . H5 H 0.3863 0.2614 0.5350 0.131 Uiso 0.50 1 calc PR D -1 C6 C 0.3783(7) 0.3060(5) 0.4530(7) 0.101(4) Uani 0.50 1 d P E -1 H6A H 0.3524 0.3165 0.4176 0.151 Uiso 0.50 1 calc PR E -1 H6B H 0.4176 0.3201 0.4550 0.151 Uiso 0.50 1 calc PR E -1 O1 O 0.34414(16) 0.19553(14) 0.36076(16) 0.0766(10) Uani 1 1 d . . . C7 C 0.3494(4) 0.2225(4) 0.2977(3) 0.141(3) Uani 1 1 d . . . H7A H 0.3487 0.2621 0.3050 0.169 Uiso 1 1 calc R . . H7B H 0.3153 0.2128 0.2687 0.169 Uiso 1 1 calc R . . C8 C 0.4036(4) 0.2077(4) 0.2649(4) 0.136(3) Uani 1 1 d . . . H8A H 0.4237 0.2401 0.2466 0.163 Uiso 1 1 calc R . . H8B H 0.3956 0.1823 0.2275 0.163 Uiso 1 1 calc R . . C9 C 0.4406(4) 0.1819(4) 0.3167(4) 0.133(3) Uani 1 1 d . . . H9A H 0.4687 0.2082 0.3366 0.159 Uiso 1 1 calc R . . H9B H 0.4634 0.1514 0.2974 0.159 Uiso 1 1 calc R . . C10 C 0.3982(4) 0.1625(3) 0.3677(4) 0.128(3) Uani 1 1 d . . . H10A H 0.4152 0.1666 0.4135 0.154 Uiso 1 1 calc R . . H10B H 0.3889 0.1238 0.3602 0.154 Uiso 1 1 calc R . . O2 O 0.22661(18) 0.14442(14) 0.35937(18) 0.0824(11) Uani 1 1 d . . . C11 C 0.2355(9) 0.0895(3) 0.3522(7) 0.270(10) Uani 1 1 d . . . H11A H 0.2088 0.0691 0.3826 0.324 Uiso 1 1 calc R . . H11B H 0.2772 0.0799 0.3629 0.324 Uiso 1 1 calc R . . C12 C 0.2216(8) 0.0771(6) 0.2795(9) 0.249(9) Uani 1 1 d . . . H12A H 0.2587 0.0749 0.2528 0.299 Uiso 1 1 calc R . . H12B H 0.2003 0.0422 0.2758 0.299 Uiso 1 1 calc R . . C13 C 0.1859(6) 0.1191(5) 0.2558(5) 0.170(5) Uani 1 1 d . . . H13A H 0.2038 0.1365 0.2157 0.204 Uiso 1 1 calc R . . H13B H 0.1456 0.1060 0.2441 0.204 Uiso 1 1 calc R . . C14 C 0.1840(6) 0.1535(4) 0.3083(5) 0.177(5) Uani 1 1 d . . . H14A H 0.1439 0.1515 0.3288 0.212 Uiso 1 1 calc R . . H14B H 0.1893 0.1907 0.2910 0.212 Uiso 1 1 calc R . . O3 O 0.1350(2) 0.3227(2) 0.5000 0.0802(14) Uani 1 2 d S . . C15 C 0.1002(4) 0.3382(5) 0.4433(4) 0.174(5) Uani 1 1 d . B . H15A H 0.1197 0.3685 0.4192 0.209 Uiso 1 1 calc R . . H15B H 0.0963 0.3075 0.4117 0.209 Uiso 1 1 calc R . . C16 C 0.0442(5) 0.3541(7) 0.4662(5) 0.232(7) Uani 1 1 d . . . H16A H 0.0348 0.3908 0.4493 0.278 Uiso 1 1 calc R B . H16B H 0.0135 0.3289 0.4493 0.278 Uiso 1 1 calc R . . O4 O 0.2545(3) 0.37207(19) 0.5000 0.0926(17) Uani 1 2 d S . . C17 C 0.2669(9) 0.4036(4) 0.4413(5) 0.222(8) Uani 1 1 d . B . H17A H 0.2336 0.4017 0.4087 0.266 Uiso 1 1 calc R . . H17B H 0.3039 0.3912 0.4190 0.266 Uiso 1 1 calc R . . C18 C 0.2741(7) 0.4612(4) 0.4693(7) 0.253(10) Uani 1 1 d . . . H18A H 0.3120 0.4768 0.4527 0.303 Uiso 1 1 calc R B . H18B H 0.2412 0.4842 0.4527 0.303 Uiso 1 1 calc R . . Mg3 Mg 0.5000 0.0000 0.7500 0.0938(12) Uani 1 4 d S . . C19 C 0.5525(5) -0.0471(3) 0.8079(5) 0.156(4) Uani 1 1 d . . . H19A H 0.5268 -0.0695 0.8373 0.188 Uiso 1 1 calc R . . H19B H 0.5751 -0.0719 0.7782 0.188 Uiso 1 1 calc R . . C20 C 0.5973(8) -0.0157(4) 0.8529(8) 0.230(7) Uani 1 1 d . . . H20 H 0.6348 -0.0157 0.8308 0.276 Uiso 1 1 calc RD . . C21 C 0.6023(10) 0.0069(6) 0.9017(8) 0.325(15) Uani 1 1 d D . . H21A H 0.5690 0.0110 0.9309 0.390 Uiso 1 1 calc R . . H21B H 0.6397 0.0219 0.9138 0.390 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0831(12) 0.0629(10) 0.0346(8) -0.0019(6) 0.0016(6) 0.0165(7) Mg2 0.0846(15) 0.0566(11) 0.0388(12) 0.000 0.000 0.0171(9) Cl1 0.0995(10) 0.0703(8) 0.0382(7) 0.0036(5) 0.0005(5) 0.0189(5) Cl2 0.1133(15) 0.0677(10) 0.0442(9) 0.000 0.000 0.0308(9) C1 0.047(3) 0.033(2) 0.015(2) 0.000 0.000 0.0089(19) C2 0.095(6) 0.086(5) 0.068(5) 0.000 0.000 0.007(4) C3 0.112(15) 0.087(13) 0.046(10) 0.000 0.000 0.007(10) C2' 0.095(6) 0.086(5) 0.068(5) 0.000 0.000 0.007(4) C3' 0.12(2) 0.105(16) 0.19(3) -0.047(17) -0.07(2) 0.026(14) C4 0.036(3) 0.034(2) 0.021(2) 0.000 0.000 0.0056(18) C5 0.124(8) 0.105(6) 0.098(7) 0.000 0.000 0.015(6) C6 0.114(10) 0.106(8) 0.082(8) 0.021(7) 0.013(7) -0.011(7) O1 0.084(2) 0.096(2) 0.0490(19) 0.0062(16) 0.0091(16) 0.0250(17) C7 0.142(6) 0.214(8) 0.065(4) 0.049(5) 0.029(4) 0.081(6) C8 0.119(6) 0.209(8) 0.080(5) 0.047(5) 0.037(4) 0.054(5) C9 0.109(5) 0.173(6) 0.116(6) 0.047(5) 0.040(5) 0.047(5) C10 0.126(6) 0.132(5) 0.126(6) 0.043(5) 0.052(5) 0.054(5) O2 0.121(3) 0.072(2) 0.054(2) -0.0059(16) -0.0100(18) 0.0113(17) C11 0.50(3) 0.063(5) 0.248(14) -0.027(6) -0.238(17) 0.005(8) C12 0.279(17) 0.185(11) 0.283(18) -0.169(13) -0.121(14) 0.089(11) C13 0.249(13) 0.178(9) 0.082(6) -0.016(6) -0.016(7) -0.078(9) C14 0.285(14) 0.129(6) 0.115(7) -0.020(5) -0.110(8) 0.020(7) O3 0.091(3) 0.098(3) 0.052(3) 0.000 0.000 0.035(3) C15 0.145(7) 0.311(14) 0.066(4) 0.043(6) 0.007(4) 0.128(8) C16 0.124(7) 0.45(2) 0.119(8) 0.038(10) -0.004(5) 0.119(10) O4 0.150(5) 0.057(3) 0.070(3) 0.000 0.000 0.004(3) C17 0.44(2) 0.098(6) 0.124(8) 0.054(5) -0.052(10) -0.084(9) C18 0.377(18) 0.108(7) 0.27(2) 0.065(9) -0.099(16) -0.067(8) Mg3 0.135(3) 0.0677(18) 0.079(2) 0.000 0.000 0.000 C19 0.234(10) 0.095(4) 0.141(7) 0.006(4) -0.082(7) -0.023(5) C20 0.41(2) 0.096(6) 0.186(13) 0.012(7) -0.111(14) 0.006(9) C21 0.59(4) 0.146(11) 0.235(17) 0.052(11) -0.22(2) -0.084(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O2 2.074(4) . ? Mg1 O1 2.081(4) . ? Mg1 Cl2 2.4965(18) . ? Mg1 Cl1 2.5122(18) . ? Mg1 Mg1 2.926(3) 10_556 ? Mg1 Mg2 2.939(2) . ? Mg2 O4 2.080(5) . ? Mg2 C1 2.085(4) . ? Mg2 O3 2.094(5) . ? Mg2 Cl1 2.5131(11) . ? Mg2 Cl1 2.5131(11) 10_556 ? Mg2 Mg1 2.939(2) 10_556 ? Cl2 Mg1 2.4965(18) 10_556 ? C1 C2 1.423(10) . ? C1 Mg1 2.082(4) 10_556 ? C1 H1A 0.9900 . ? C2 C3 1.374(19) . ? C2 H2 0.9400 . ? C3 H3A 0.9400 . ? C3 H3B 0.9400 . ? C3' H3'A 0.9400 . ? C3' H3'B 0.9400 . ? C4 C5 1.342(12) . ? C4 Mg1 2.089(3) 10_556 ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 C6 1.320(13) 10_556 ? C5 C6 1.320(13) . ? C5 H5 0.9400 . ? C6 H6A 0.9400 . ? C6 H6B 0.9400 . ? O1 C7 1.408(7) . ? O1 C10 1.456(8) . ? C7 C8 1.412(10) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.454(10) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.455(10) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? O2 C11 1.366(9) . ? O2 C14 1.398(9) . ? C11 C12 1.494(17) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 C13 1.380(14) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 C14 1.333(12) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? O3 C15 1.409(7) . ? O3 C15 1.409(7) 10_556 ? C15 C16 1.381(12) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 C16 1.326(19) 10_556 ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? O4 C17 1.414(9) 10_556 ? O4 C17 1.414(9) . ? C17 C18 1.524(14) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 C18 1.21(3) 10_556 ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? Mg3 C19 1.996(8) 7_546 ? Mg3 C19 1.996(8) . ? Mg3 C19 1.996(8) 2_655 ? Mg3 C19 1.996(8) 8_446 ? C19 C20 1.538(17) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C20 C21 1.113(12) . ? C20 H20 0.9400 . ? C21 H21A 0.9400 . ? C21 H21B 0.9400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mg1 O1 88.47(16) . . ? O2 Mg1 Cl2 94.12(12) . . ? O1 Mg1 Cl2 93.93(11) . . ? O2 Mg1 Cl1 94.41(11) . . ? O1 Mg1 Cl1 94.02(11) . . ? Cl2 Mg1 Cl1 168.49(7) . . ? O2 Mg1 Mg1 128.79(11) . 10_556 ? O1 Mg1 Mg1 127.68(11) . 10_556 ? Cl2 Mg1 Mg1 54.12(4) . 10_556 ? Cl1 Mg1 Mg1 114.36(4) . 10_556 ? O2 Mg1 Mg2 129.67(13) . . ? O1 Mg1 Mg2 127.14(12) . . ? Cl2 Mg1 Mg2 114.26(6) . . ? Cl1 Mg1 Mg2 54.23(4) . . ? Mg1 Mg1 Mg2 60.14(3) 10_556 . ? O4 Mg2 C1 171.4(2) . . ? O4 Mg2 O3 88.8(2) . . ? C1 Mg2 O3 99.8(2) . . ? O4 Mg2 Cl1 94.71(6) . . ? C1 Mg2 Cl1 84.80(5) . . ? O3 Mg2 Cl1 93.78(6) . . ? O4 Mg2 Cl1 94.71(6) . 10_556 ? C1 Mg2 Cl1 84.80(5) . 10_556 ? O3 Mg2 Cl1 93.78(6) . 10_556 ? Cl1 Mg2 Cl1 168.04(10) . 10_556 ? O4 Mg2 Mg1 128.53(16) . 10_556 ? C1 Mg2 Mg1 45.11(10) . 10_556 ? O3 Mg2 Mg1 128.04(14) . 10_556 ? Cl1 Mg2 Mg1 113.91(7) . 10_556 ? Cl1 Mg2 Mg1 54.20(4) 10_556 10_556 ? O4 Mg2 Mg1 128.53(16) . . ? C1 Mg2 Mg1 45.11(10) . . ? O3 Mg2 Mg1 128.04(14) . . ? Cl1 Mg2 Mg1 54.20(4) . . ? Cl1 Mg2 Mg1 113.91(7) 10_556 . ? Mg1 Mg2 Mg1 59.72(6) 10_556 . ? Mg1 Cl1 Mg2 71.58(6) . . ? Mg1 Cl2 Mg1 71.75(7) . 10_556 ? C2 C1 Mg1 125.3(2) . 10_556 ? C2 C1 Mg2 126.0(4) . . ? Mg1 C1 Mg2 89.71(16) 10_556 . ? C2 C1 H1A 104.3 . . ? Mg1 C1 H1A 104.3 10_556 . ? Mg2 C1 H1A 104.3 . . ? C3 C2 C1 121.5(11) . . ? C3 C2 H2 119.2 . . ? C1 C2 H2 119.2 . . ? C2 C3 H3A 120.0 . . ? C2 C3 H3B 120.0 . . ? H3A C3 H3B 120.0 . . ? H3'A C3' H3'B 120.0 . . ? C5 C4 Mg1 125.2(3) . 10_556 ? C5 C4 H4A 106.0 . . ? Mg1 C4 H4A 106.0 10_556 . ? C5 C4 H4B 106.0 . . ? Mg1 C4 H4B 106.0 10_556 . ? H4A C4 H4B 106.3 . . ? C6 C5 C6 88.6(14) 10_556 . ? C6 C5 C4 122.9(9) 10_556 . ? C6 C5 C4 122.9(9) . . ? C6 C5 H5 57.2 10_556 . ? C6 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? C5 C6 H6A 120.0 . . ? C5 C6 H6B 120.0 . . ? H6A C6 H6B 120.0 . . ? C7 O1 C10 105.9(5) . . ? C7 O1 Mg1 126.4(4) . . ? C10 O1 Mg1 127.4(3) . . ? O1 C7 C8 110.7(6) . . ? O1 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? O1 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C7 C8 C9 105.9(6) . . ? C7 C8 H8A 110.5 . . ? C9 C8 H8A 110.5 . . ? C7 C8 H8B 110.5 . . ? C9 C8 H8B 110.5 . . ? H8A C8 H8B 108.7 . . ? C8 C9 C10 104.9(7) . . ? C8 C9 H9A 110.8 . . ? C10 C9 H9A 110.8 . . ? C8 C9 H9B 110.8 . . ? C10 C9 H9B 110.8 . . ? H9A C9 H9B 108.8 . . ? C9 C10 O1 106.8(5) . . ? C9 C10 H10A 110.4 . . ? O1 C10 H10A 110.4 . . ? C9 C10 H10B 110.4 . . ? O1 C10 H10B 110.4 . . ? H10A C10 H10B 108.6 . . ? C11 O2 C14 100.5(6) . . ? C11 O2 Mg1 127.6(5) . . ? C14 O2 Mg1 131.8(4) . . ? O2 C11 C12 105.5(8) . . ? O2 C11 H11A 110.6 . . ? C12 C11 H11A 110.6 . . ? O2 C11 H11B 110.6 . . ? C12 C11 H11B 110.6 . . ? H11A C11 H11B 108.8 . . ? C13 C12 C11 106.9(9) . . ? C13 C12 H12A 110.3 . . ? C11 C12 H12A 110.3 . . ? C13 C12 H12B 110.3 . . ? C11 C12 H12B 110.3 . . ? H12A C12 H12B 108.6 . . ? C14 C13 C12 103.2(9) . . ? C14 C13 H13A 111.1 . . ? C12 C13 H13A 111.1 . . ? C14 C13 H13B 111.1 . . ? C12 C13 H13B 111.1 . . ? H13A C13 H13B 109.1 . . ? C13 C14 O2 115.6(9) . . ? C13 C14 H14A 108.4 . . ? O2 C14 H14A 108.4 . . ? C13 C14 H14B 108.4 . . ? O2 C14 H14B 108.4 . . ? H14A C14 H14B 107.4 . . ? C15 O3 C15 104.5(7) . 10_556 ? C15 O3 Mg2 127.6(3) . . ? C15 O3 Mg2 127.6(3) 10_556 . ? C16 C15 O3 108.3(6) . . ? C16 C15 H15A 110.0 . . ? O3 C15 H15A 110.0 . . ? C16 C15 H15B 110.0 . . ? O3 C15 H15B 110.0 . . ? H15A C15 H15B 108.4 . . ? C16 C16 C15 109.1(5) 10_556 . ? C16 C16 H16A 109.9 10_556 . ? C15 C16 H16A 109.9 . . ? C16 C16 H16B 109.9 10_556 . ? C15 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? C17 O4 C17 109.2(9) 10_556 . ? C17 O4 Mg2 125.4(4) 10_556 . ? C17 O4 Mg2 125.4(4) . . ? O4 C17 C18 103.4(9) . . ? O4 C17 H17A 111.1 . . ? C18 C17 H17A 111.1 . . ? O4 C17 H17B 111.1 . . ? C18 C17 H17B 111.1 . . ? H17A C17 H17B 109.1 . . ? C18 C18 C17 111.2(6) 10_556 . ? C18 C18 H18A 109.4 10_556 . ? C17 C18 H18A 109.4 . . ? C18 C18 H18B 109.4 10_556 . ? C17 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C19 Mg3 C19 109.5(4) 7_546 . ? C19 Mg3 C19 108.4(6) 7_546 2_655 ? C19 Mg3 C19 110.5(6) . 2_655 ? C19 Mg3 C19 110.5(6) 7_546 8_446 ? C19 Mg3 C19 108.4(6) . 8_446 ? C19 Mg3 C19 109.5(4) 2_655 8_446 ? C20 C19 Mg3 114.7(5) . . ? C20 C19 H19A 108.6 . . ? Mg3 C19 H19A 108.6 . . ? C20 C19 H19B 108.6 . . ? Mg3 C19 H19B 108.6 . . ? H19A C19 H19B 107.6 . . ? C21 C20 C19 143.9(17) . . ? C21 C20 H20 108.0 . . ? C19 C20 H20 108.0 . . ? C20 C21 H21A 120.0 . . ? C20 C21 H21B 120.0 . . ? H21A C21 H21B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.141 _refine_diff_density_min -0.758 _refine_diff_density_rms 0.098 # Attachment '3.cif' data_lf0507 _database_code_depnum_ccdc_archive 'CCDC 298101' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H20 Cl2 Mg N4' _chemical_formula_sum 'C20 H20 Cl2 Mg N4' _chemical_formula_weight 411.61 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' Cl Cl 0.1484 0.1585 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1636(2) _cell_length_b 9.2462(2) _cell_length_c 13.4528(3) _cell_angle_alpha 74.8540(10) _cell_angle_beta 78.9020(10) _cell_angle_gamma 77.6580(10) _cell_volume 1063.47(4) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9388 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 428 _exptl_absorpt_coefficient_mu 0.346 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.828 _exptl_absorpt_correction_T_max 0.870 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 12285 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.66 _diffrn_reflns_theta_max 27.53 _reflns_number_total 4817 _reflns_number_gt 4211 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+0.7737P] 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 4817 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1313 _refine_ls_wR_factor_gt 0.1262 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _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 Cl1_1 Cl 0.23082(6) -0.19475(6) -0.01657(5) 0.04716(16) Uani 1 1 d . . . Mg1_1 Mg 0.0000 0.0000 0.0000 0.0378(2) Uani 1 2 d S . . N1_1 N -0.1425(2) -0.1805(2) 0.02318(16) 0.0445(4) Uani 1 1 d . . . N2_1 N 0.0091(2) -0.0401(2) 0.17346(15) 0.0448(4) Uani 1 1 d . . . C1_1 C -0.2748(3) -0.1468(3) -0.0120(2) 0.0603(7) Uani 1 1 d . . . H1_1 H -0.3083 -0.0448 -0.0466 0.072 Uiso 1 1 calc R . . C2_1 C -0.3661(3) -0.2536(4) -0.0003(3) 0.0720(8) Uani 1 1 d . . . H2_1 H -0.4603 -0.2249 -0.0259 0.086 Uiso 1 1 calc R . . C3_1 C -0.3183(3) -0.4013(4) 0.0486(2) 0.0664(8) Uani 1 1 d . . . H3_1 H -0.3784 -0.4769 0.0571 0.080 Uiso 1 1 calc R . . C4_1 C -0.1837(4) -0.4377(3) 0.0847(3) 0.0697(8) Uani 1 1 d . . . H4_1 H -0.1481 -0.5392 0.1191 0.084 Uiso 1 1 calc R . . C5_1 C -0.0991(3) -0.3250(3) 0.0705(2) 0.0579(6) Uani 1 1 d . . . H5_1 H -0.0049 -0.3520 0.0960 0.070 Uiso 1 1 calc R . . C6_1 C 0.0879(5) -0.1636(3) 0.2264(2) 0.0871(12) Uani 1 1 d . . . H6_1 H 0.1406 -0.2397 0.1906 0.105 Uiso 1 1 calc R . . C7_1 C 0.0975(7) -0.1875(4) 0.3301(3) 0.142(2) Uani 1 1 d . . . H7_1 H 0.1560 -0.2780 0.3645 0.171 Uiso 1 1 calc R . . C8_1 C 0.0224(6) -0.0806(4) 0.3833(3) 0.1166(18) Uani 1 1 d . . . H8_1 H 0.0256 -0.0958 0.4556 0.140 Uiso 1 1 calc R . . C9_1 C -0.0576(4) 0.0490(3) 0.3302(2) 0.0727(8) Uani 1 1 d . . . H9_1 H -0.1097 0.1270 0.3644 0.087 Uiso 1 1 calc R . . C10_1 C -0.0613(3) 0.0645(3) 0.2268(2) 0.0541(6) Uani 1 1 d . . . H10_1 H -0.1173 0.1552 0.1907 0.065 Uiso 1 1 calc R . . Mg1_2 Mg -0.5000 -0.5000 0.5000 0.0376(2) Uani 1 2 d S . . Cl1_2 Cl -0.27019(6) -0.59365(7) 0.39009(5) 0.05283(17) Uani 1 1 d . . . N1_2 N -0.3579(2) -0.4489(2) 0.60177(16) 0.0456(4) Uani 1 1 d . . . N2_2 N -0.4945(2) -0.2589(2) 0.39937(16) 0.0471(4) Uani 1 1 d . . . C1_2 C -0.3975(3) -0.4694(3) 0.7044(2) 0.0580(6) Uani 1 1 d . . . H1_2 H -0.4923 -0.4991 0.7344 0.070 Uiso 1 1 calc R . . C2_2 C -0.3075(4) -0.4496(4) 0.7694(3) 0.0768(9) Uani 1 1 d . . . H2_2 H -0.3390 -0.4679 0.8424 0.092 Uiso 1 1 calc R . . C3_2 C -0.1721(4) -0.4033(4) 0.7271(3) 0.0799(10) Uani 1 1 d . . . H3_2 H -0.1087 -0.3872 0.7699 0.096 Uiso 1 1 calc R . . C4_2 C -0.1303(3) -0.3806(4) 0.6218(3) 0.0739(9) Uani 1 1 d . . . H4_2 H -0.0368 -0.3488 0.5904 0.089 Uiso 1 1 calc R . . C5_2 C -0.2247(3) -0.4041(3) 0.5618(3) 0.0589(6) Uani 1 1 d . . . H5_2 H -0.1942 -0.3879 0.4887 0.071 Uiso 1 1 calc R . . C6_2 C -0.5715(5) -0.1397(4) 0.4337(4) 0.123(2) Uani 1 1 d . . . H6_2 H -0.6321 -0.1568 0.5000 0.148 Uiso 1 1 calc R . . C7_2 C -0.5689(7) 0.0094(4) 0.3785(5) 0.164(3) Uani 1 1 d . . . H7_2 H -0.6260 0.0914 0.4072 0.196 Uiso 1 1 calc R . . C8_2 C -0.4848(5) 0.0370(4) 0.2840(3) 0.1033(14) Uani 1 1 d . . . H8_2 H -0.4865 0.1377 0.2426 0.124 Uiso 1 1 calc R . . C9_2 C -0.4000(4) -0.0803(4) 0.2508(3) 0.0793(9) Uani 1 1 d . . . H9_2 H -0.3340 -0.0647 0.1867 0.095 Uiso 1 1 calc R . . C10_2 C -0.4076(4) -0.2248(3) 0.3093(2) 0.0672(8) Uani 1 1 d . . . H10_2 H -0.3454 -0.3068 0.2829 0.081 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 Cl1_1 0.0379(3) 0.0373(3) 0.0650(4) -0.0107(2) -0.0144(2) 0.0010(2) Mg1_1 0.0363(5) 0.0298(5) 0.0480(6) -0.0079(4) -0.0125(4) -0.0026(4) N1_1 0.0413(9) 0.0378(9) 0.0567(11) -0.0131(8) -0.0102(8) -0.0063(7) N2_1 0.0532(11) 0.0326(9) 0.0492(10) -0.0096(7) -0.0151(8) -0.0018(8) C1_1 0.0512(14) 0.0524(14) 0.0853(19) -0.0201(13) -0.0251(13) -0.0071(11) C2_1 0.0534(15) 0.083(2) 0.095(2) -0.0360(18) -0.0186(15) -0.0201(14) C3_1 0.0691(18) 0.0692(18) 0.0740(18) -0.0304(15) 0.0050(14) -0.0368(15) C4_1 0.0762(19) 0.0464(14) 0.086(2) -0.0054(13) -0.0090(16) -0.0255(13) C5_1 0.0542(14) 0.0425(12) 0.0747(17) -0.0031(12) -0.0143(12) -0.0115(11) C6_1 0.149(3) 0.0444(14) 0.0629(17) -0.0206(13) -0.046(2) 0.0321(17) C7_1 0.275(7) 0.065(2) 0.073(2) -0.0299(18) -0.087(3) 0.073(3) C8_1 0.220(5) 0.065(2) 0.0597(19) -0.0250(16) -0.060(3) 0.033(3) C9_1 0.100(2) 0.0573(16) 0.0630(17) -0.0282(14) -0.0225(16) 0.0095(15) C10_1 0.0597(14) 0.0427(12) 0.0579(14) -0.0144(10) -0.0161(12) 0.0058(11) Mg1_2 0.0303(5) 0.0344(5) 0.0466(5) -0.0120(4) -0.0052(4) 0.0006(4) Cl1_2 0.0375(3) 0.0514(3) 0.0640(4) -0.0197(3) 0.0021(2) 0.0038(2) N1_2 0.0399(9) 0.0393(9) 0.0585(11) -0.0146(8) -0.0122(8) -0.0002(7) N2_2 0.0431(10) 0.0374(9) 0.0557(11) -0.0090(8) -0.0049(8) -0.0003(8) C1_2 0.0619(15) 0.0578(15) 0.0579(15) -0.0156(12) -0.0150(12) -0.0093(12) C2_2 0.099(2) 0.073(2) 0.0701(19) -0.0194(15) -0.0377(18) -0.0133(18) C3_2 0.083(2) 0.0607(17) 0.112(3) -0.0198(17) -0.062(2) -0.0037(16) C4_2 0.0490(15) 0.0661(18) 0.115(3) -0.0219(18) -0.0326(16) -0.0072(13) C5_2 0.0419(12) 0.0567(15) 0.0817(19) -0.0210(13) -0.0148(12) -0.0045(11) C6_2 0.136(3) 0.0447(16) 0.128(3) -0.0022(18) 0.068(3) 0.0159(19) C7_2 0.183(5) 0.0430(18) 0.183(5) -0.002(2) 0.088(4) 0.024(2) C8_2 0.113(3) 0.0456(17) 0.114(3) 0.0111(18) 0.018(2) -0.0013(18) C9_2 0.097(2) 0.0577(17) 0.071(2) -0.0029(14) 0.0099(17) -0.0217(16) C10_2 0.0803(19) 0.0472(14) 0.0658(17) -0.0117(12) 0.0102(14) -0.0133(13) _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 Cl1_1 Mg1_1 2.4832(5) . ? Mg1_1 N1_1 2.2561(18) . ? Mg1_1 N1_1 2.2561(18) 2 ? Mg1_1 N2_1 2.2803(19) 2 ? Mg1_1 N2_1 2.2803(19) . ? Mg1_1 Cl1_1 2.4832(5) 2 ? N1_1 C1_1 1.332(3) . ? N1_1 C5_1 1.333(3) . ? N2_1 C6_1 1.324(3) . ? N2_1 C10_1 1.335(3) . ? C1_1 C2_1 1.386(4) . ? C1_1 H1_1 0.9500 . ? C2_1 C3_1 1.369(5) . ? C2_1 H2_1 0.9500 . ? C3_1 C4_1 1.355(4) . ? C3_1 H3_1 0.9500 . ? C4_1 C5_1 1.381(4) . ? C4_1 H4_1 0.9500 . ? C5_1 H5_1 0.9500 . ? C6_1 C7_1 1.371(4) . ? C6_1 H6_1 0.9500 . ? C7_1 C8_1 1.362(5) . ? C7_1 H7_1 0.9500 . ? C8_1 C9_1 1.365(4) . ? C8_1 H8_1 0.9500 . ? C9_1 C10_1 1.367(4) . ? C9_1 H9_1 0.9500 . ? C10_1 H10_1 0.9500 . ? Mg1_2 N1_2 2.2539(19) 2_446 ? Mg1_2 N1_2 2.2539(19) . ? Mg1_2 N2_2 2.2908(19) 2_446 ? Mg1_2 N2_2 2.2908(19) . ? Mg1_2 Cl1_2 2.4620(5) 2_446 ? Mg1_2 Cl1_2 2.4620(5) . ? N1_2 C1_2 1.332(3) . ? N1_2 C5_2 1.341(3) . ? N2_2 C6_2 1.317(4) . ? N2_2 C10_2 1.318(3) . ? C1_2 C2_2 1.379(4) . ? C1_2 H1_2 0.9500 . ? C2_2 C3_2 1.370(5) . ? C2_2 H2_2 0.9500 . ? C3_2 C4_2 1.365(5) . ? C3_2 H3_2 0.9500 . ? C4_2 C5_2 1.374(4) . ? C4_2 H4_2 0.9500 . ? C5_2 H5_2 0.9500 . ? C6_2 C7_2 1.388(5) . ? C6_2 H6_2 0.9500 . ? C7_2 C8_2 1.346(6) . ? C7_2 H7_2 0.9500 . ? C8_2 C9_2 1.319(5) . ? C8_2 H8_2 0.9500 . ? C9_2 C10_2 1.371(4) . ? C9_2 H9_2 0.9500 . ? C10_2 H10_2 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 N1_1 Mg1_1 N1_1 180.00(11) . 2 ? N1_1 Mg1_1 N2_1 86.45(7) . 2 ? N1_1 Mg1_1 N2_1 93.55(7) 2 2 ? N1_1 Mg1_1 N2_1 93.55(7) . . ? N1_1 Mg1_1 N2_1 86.45(7) 2 . ? N2_1 Mg1_1 N2_1 180.0 2 . ? N1_1 Mg1_1 Cl1_1 89.44(5) . . ? N1_1 Mg1_1 Cl1_1 90.56(5) 2 . ? N2_1 Mg1_1 Cl1_1 89.94(5) 2 . ? N2_1 Mg1_1 Cl1_1 90.06(5) . . ? N1_1 Mg1_1 Cl1_1 90.56(5) . 2 ? N1_1 Mg1_1 Cl1_1 89.44(5) 2 2 ? N2_1 Mg1_1 Cl1_1 90.06(5) 2 2 ? N2_1 Mg1_1 Cl1_1 89.94(5) . 2 ? Cl1_1 Mg1_1 Cl1_1 180.00(4) . 2 ? C1_1 N1_1 C5_1 116.6(2) . . ? C1_1 N1_1 Mg1_1 120.84(16) . . ? C5_1 N1_1 Mg1_1 122.55(16) . . ? C6_1 N2_1 C10_1 116.0(2) . . ? C6_1 N2_1 Mg1_1 122.86(17) . . ? C10_1 N2_1 Mg1_1 121.10(15) . . ? N1_1 C1_1 C2_1 123.1(3) . . ? N1_1 C1_1 H1_1 118.5 . . ? C2_1 C1_1 H1_1 118.5 . . ? C3_1 C2_1 C1_1 119.0(3) . . ? C3_1 C2_1 H2_1 120.5 . . ? C1_1 C2_1 H2_1 120.5 . . ? C4_1 C3_1 C2_1 118.8(2) . . ? C4_1 C3_1 H3_1 120.6 . . ? C2_1 C3_1 H3_1 120.6 . . ? C3_1 C4_1 C5_1 119.0(3) . . ? C3_1 C4_1 H4_1 120.5 . . ? C5_1 C4_1 H4_1 120.5 . . ? N1_1 C5_1 C4_1 123.6(3) . . ? N1_1 C5_1 H5_1 118.2 . . ? C4_1 C5_1 H5_1 118.2 . . ? N2_1 C6_1 C7_1 123.5(3) . . ? N2_1 C6_1 H6_1 118.2 . . ? C7_1 C6_1 H6_1 118.2 . . ? C8_1 C7_1 C6_1 119.4(3) . . ? C8_1 C7_1 H7_1 120.3 . . ? C6_1 C7_1 H7_1 120.3 . . ? C7_1 C8_1 C9_1 118.2(3) . . ? C7_1 C8_1 H8_1 120.9 . . ? C9_1 C8_1 H8_1 120.9 . . ? C8_1 C9_1 C10_1 118.8(3) . . ? C8_1 C9_1 H9_1 120.6 . . ? C10_1 C9_1 H9_1 120.6 . . ? N2_1 C10_1 C9_1 124.0(2) . . ? N2_1 C10_1 H10_1 118.0 . . ? C9_1 C10_1 H10_1 118.0 . . ? N1_2 Mg1_2 N1_2 180.00(7) 2_446 . ? N1_2 Mg1_2 N2_2 87.84(7) 2_446 2_446 ? N1_2 Mg1_2 N2_2 92.16(7) . 2_446 ? N1_2 Mg1_2 N2_2 92.16(7) 2_446 . ? N1_2 Mg1_2 N2_2 87.84(7) . . ? N2_2 Mg1_2 N2_2 180.0 2_446 . ? N1_2 Mg1_2 Cl1_2 90.29(5) 2_446 2_446 ? N1_2 Mg1_2 Cl1_2 89.71(5) . 2_446 ? N2_2 Mg1_2 Cl1_2 89.46(5) 2_446 2_446 ? N2_2 Mg1_2 Cl1_2 90.54(5) . 2_446 ? N1_2 Mg1_2 Cl1_2 89.71(5) 2_446 . ? N1_2 Mg1_2 Cl1_2 90.29(5) . . ? N2_2 Mg1_2 Cl1_2 90.54(5) 2_446 . ? N2_2 Mg1_2 Cl1_2 89.46(5) . . ? Cl1_2 Mg1_2 Cl1_2 180.0 2_446 . ? C1_2 N1_2 C5_2 116.8(2) . . ? C1_2 N1_2 Mg1_2 122.05(17) . . ? C5_2 N1_2 Mg1_2 121.01(18) . . ? C6_2 N2_2 C10_2 114.1(2) . . ? C6_2 N2_2 Mg1_2 120.7(2) . . ? C10_2 N2_2 Mg1_2 124.93(17) . . ? N1_2 C1_2 C2_2 123.2(3) . . ? N1_2 C1_2 H1_2 118.4 . . ? C2_2 C1_2 H1_2 118.4 . . ? C3_2 C2_2 C1_2 119.0(3) . . ? C3_2 C2_2 H2_2 120.5 . . ? C1_2 C2_2 H2_2 120.5 . . ? C4_2 C3_2 C2_2 118.5(3) . . ? C4_2 C3_2 H3_2 120.8 . . ? C2_2 C3_2 H3_2 120.8 . . ? C3_2 C4_2 C5_2 119.4(3) . . ? C3_2 C4_2 H4_2 120.3 . . ? C5_2 C4_2 H4_2 120.3 . . ? N1_2 C5_2 C4_2 123.0(3) . . ? N1_2 C5_2 H5_2 118.5 . . ? C4_2 C5_2 H5_2 118.5 . . ? N2_2 C6_2 C7_2 123.7(3) . . ? N2_2 C6_2 H6_2 118.2 . . ? C7_2 C6_2 H6_2 118.2 . . ? C8_2 C7_2 C6_2 119.5(4) . . ? C8_2 C7_2 H7_2 120.3 . . ? C6_2 C7_2 H7_2 120.3 . . ? C9_2 C8_2 C7_2 117.8(3) . . ? C9_2 C8_2 H8_2 121.1 . . ? C7_2 C8_2 H8_2 121.1 . . ? C8_2 C9_2 C10_2 119.7(3) . . ? C8_2 C9_2 H9_2 120.2 . . ? C10_2 C9_2 H9_2 120.2 . . ? N2_2 C10_2 C9_2 125.0(3) . . ? N2_2 C10_2 H10_2 117.5 . . ? C9_2 C10_2 H10_2 117.5 . . ? 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 N1_1 Mg1_1 N1_1 C1_1 -179(100) 2 . . . ? N2_1 Mg1_1 N1_1 C1_1 -56.4(2) 2 . . . ? N2_1 Mg1_1 N1_1 C1_1 123.6(2) . . . . ? Cl1_1 Mg1_1 N1_1 C1_1 -146.4(2) . . . . ? Cl1_1 Mg1_1 N1_1 C1_1 33.6(2) 2 . . . ? N1_1 Mg1_1 N1_1 C5_1 0(100) 2 . . . ? N2_1 Mg1_1 N1_1 C5_1 122.5(2) 2 . . . ? N2_1 Mg1_1 N1_1 C5_1 -57.5(2) . . . . ? Cl1_1 Mg1_1 N1_1 C5_1 32.5(2) . . . . ? Cl1_1 Mg1_1 N1_1 C5_1 -147.5(2) 2 . . . ? N1_1 Mg1_1 N2_1 C6_1 71.2(3) . . . . ? N1_1 Mg1_1 N2_1 C6_1 -108.8(3) 2 . . . ? N2_1 Mg1_1 N2_1 C6_1 -161(48) 2 . . . ? Cl1_1 Mg1_1 N2_1 C6_1 -18.3(3) . . . . ? Cl1_1 Mg1_1 N2_1 C6_1 161.7(3) 2 . . . ? N1_1 Mg1_1 N2_1 C10_1 -111.50(19) . . . . ? N1_1 Mg1_1 N2_1 C10_1 68.50(19) 2 . . . ? N2_1 Mg1_1 N2_1 C10_1 16(48) 2 . . . ? Cl1_1 Mg1_1 N2_1 C10_1 159.05(19) . . . . ? Cl1_1 Mg1_1 N2_1 C10_1 -20.95(19) 2 . . . ? C5_1 N1_1 C1_1 C2_1 0.6(4) . . . . ? Mg1_1 N1_1 C1_1 C2_1 179.6(2) . . . . ? N1_1 C1_1 C2_1 C3_1 -0.7(5) . . . . ? C1_1 C2_1 C3_1 C4_1 0.5(5) . . . . ? C2_1 C3_1 C4_1 C5_1 -0.2(5) . . . . ? C1_1 N1_1 C5_1 C4_1 -0.3(4) . . . . ? Mg1_1 N1_1 C5_1 C4_1 -179.3(2) . . . . ? C3_1 C4_1 C5_1 N1_1 0.2(5) . . . . ? C10_1 N2_1 C6_1 C7_1 0.9(6) . . . . ? Mg1_1 N2_1 C6_1 C7_1 178.3(4) . . . . ? N2_1 C6_1 C7_1 C8_1 0.3(9) . . . . ? C6_1 C7_1 C8_1 C9_1 -1.4(9) . . . . ? C7_1 C8_1 C9_1 C10_1 1.3(7) . . . . ? C6_1 N2_1 C10_1 C9_1 -1.0(4) . . . . ? Mg1_1 N2_1 C10_1 C9_1 -178.5(2) . . . . ? C8_1 C9_1 C10_1 N2_1 0.0(6) . . . . ? N1_2 Mg1_2 N1_2 C1_2 139(100) 2_446 . . . ? N2_2 Mg1_2 N1_2 C1_2 -52.70(19) 2_446 . . . ? N2_2 Mg1_2 N1_2 C1_2 127.30(19) . . . . ? Cl1_2 Mg1_2 N1_2 C1_2 36.75(18) 2_446 . . . ? Cl1_2 Mg1_2 N1_2 C1_2 -143.25(18) . . . . ? N1_2 Mg1_2 N1_2 C5_2 -45(100) 2_446 . . . ? N2_2 Mg1_2 N1_2 C5_2 123.60(18) 2_446 . . . ? N2_2 Mg1_2 N1_2 C5_2 -56.40(18) . . . . ? Cl1_2 Mg1_2 N1_2 C5_2 -146.96(18) 2_446 . . . ? Cl1_2 Mg1_2 N1_2 C5_2 33.04(18) . . . . ? N1_2 Mg1_2 N2_2 C6_2 108.2(3) 2_446 . . . ? N1_2 Mg1_2 N2_2 C6_2 -71.8(3) . . . . ? N2_2 Mg1_2 N2_2 C6_2 -52(100) 2_446 . . . ? Cl1_2 Mg1_2 N2_2 C6_2 17.9(3) 2_446 . . . ? Cl1_2 Mg1_2 N2_2 C6_2 -162.1(3) . . . . ? N1_2 Mg1_2 N2_2 C10_2 -78.2(2) 2_446 . . . ? N1_2 Mg1_2 N2_2 C10_2 101.8(2) . . . . ? N2_2 Mg1_2 N2_2 C10_2 122(100) 2_446 . . . ? Cl1_2 Mg1_2 N2_2 C10_2 -168.5(2) 2_446 . . . ? Cl1_2 Mg1_2 N2_2 C10_2 11.5(2) . . . . ? C5_2 N1_2 C1_2 C2_2 -1.3(4) . . . . ? Mg1_2 N1_2 C1_2 C2_2 175.2(2) . . . . ? N1_2 C1_2 C2_2 C3_2 1.6(5) . . . . ? C1_2 C2_2 C3_2 C4_2 -1.0(5) . . . . ? C2_2 C3_2 C4_2 C5_2 0.3(5) . . . . ? C1_2 N1_2 C5_2 C4_2 0.5(4) . . . . ? Mg1_2 N1_2 C5_2 C4_2 -176.0(2) . . . . ? C3_2 C4_2 C5_2 N1_2 0.0(4) . . . . ? C10_2 N2_2 C6_2 C7_2 3.3(8) . . . . ? Mg1_2 N2_2 C6_2 C7_2 177.6(5) . . . . ? N2_2 C6_2 C7_2 C8_2 0.5(11) . . . . ? C6_2 C7_2 C8_2 C9_2 -4.4(10) . . . . ? C7_2 C8_2 C9_2 C10_2 4.3(8) . . . . ? C6_2 N2_2 C10_2 C9_2 -3.4(6) . . . . ? Mg1_2 N2_2 C10_2 C9_2 -177.4(3) . . . . ? C8_2 C9_2 C10_2 N2_2 -0.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.408 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.048