# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name 'P. Bailey' 'Daniel Lorono-Gonzalez' 'Simon Parsons' _publ_contact_author_name 'Dr P J Bailey' _publ_contact_author_address ; Department of Chemistry University of Edinburgh West Mains Road Edinburgh UNITED KINGDOM ; _publ_contact_author_email PHILIP.BAILEY@ED.AC.UK _publ_section_title ; 6-Aminofulvene-2-aldimine, a novel class of ambidentat cyclopentadienyl/diimine ligand: synthesis and characterisation of magnesium complexes ; data_fulmg22 _database_code_CSD 205884 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [MeMg(Cy)2AFA)] _chemical_formula_sum 'C24 H38 Mg N2 O' _chemical_formula_weight 394.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.3464(9) _cell_length_b 15.2076(13) _cell_length_c 27.249(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4701.9(7) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5808 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 26 _exptl_crystal_description Rod _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.116 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.966 _exptl_absorpt_correction_T_max 0.991 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 28371 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 29.06 _reflns_number_total 5846 _reflns_number_gt 4515 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1995)' _computing_cell_refinement 'SMART (Bruker, 1995)' _computing_data_reduction 'SHELXTL (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0692P)^2^+2.3639P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5846 _refine_ls_number_parameters 271 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_gt 0.0652 _refine_ls_wR_factor_ref 0.1578 _refine_ls_wR_factor_gt 0.1469 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.082 _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 0.28362(5) 0.06023(4) 0.38531(2) 0.02064(16) Uani 1 1 d . . . N1 N 0.18471(13) 0.17524(10) 0.37775(6) 0.0227(3) Uani 1 1 d . A . N2 N 0.42229(13) 0.07681(10) 0.33612(5) 0.0204(3) Uani 1 1 d . A . C1 C 0.15883(16) 0.20906(12) 0.33551(7) 0.0240(4) Uani 1 1 d . . . H1A H 0.0949 0.2494 0.3361 0.029 Uiso 1 1 calc R A . C2 C 0.20996(16) 0.19597(12) 0.28844(7) 0.0230(4) Uani 1 1 d . A . C3 C 0.15545(17) 0.23509(13) 0.24729(7) 0.0287(4) Uani 1 1 d . . . H3A H 0.0842 0.2678 0.2482 0.034 Uiso 1 1 calc R A . C4 C 0.22086(18) 0.21882(14) 0.20565(7) 0.0308(5) Uani 1 1 d . A . H4A H 0.2014 0.2367 0.1732 0.037 Uiso 1 1 calc R . . C5 C 0.32028(18) 0.17160(13) 0.21945(7) 0.0280(4) Uani 1 1 d . . . H5A H 0.3813 0.1533 0.1979 0.034 Uiso 1 1 calc R A . C6 C 0.31666(16) 0.15506(12) 0.27040(6) 0.0216(4) Uani 1 1 d . A . C7 C 0.41231(16) 0.10901(12) 0.29243(6) 0.0217(4) Uani 1 1 d . . . H7A H 0.4790 0.1007 0.2719 0.026 Uiso 1 1 calc R A . C8 C 0.11446(16) 0.20770(13) 0.41971(7) 0.0254(4) Uani 1 1 d . . . H8A H 0.0744 0.2633 0.4094 0.031 Uiso 1 1 calc R A . C9 C 0.01973(18) 0.14143(15) 0.43409(8) 0.0339(5) Uani 1 1 d . A . H9A H 0.0573 0.0848 0.4428 0.041 Uiso 1 1 calc R . . H9B H -0.0334 0.1312 0.4058 0.041 Uiso 1 1 calc R . . C10 C -0.05206(18) 0.17491(17) 0.47778(8) 0.0391(5) Uani 1 1 d . . . H10A H -0.0952 0.2288 0.4682 0.047 Uiso 1 1 calc R A . H10B H -0.1107 0.1299 0.4874 0.047 Uiso 1 1 calc R . . C11 C 0.02722(18) 0.19491(15) 0.52089(7) 0.0332(5) Uani 1 1 d . A . H11A H 0.0644 0.1398 0.5325 0.040 Uiso 1 1 calc R . . H11B H -0.0207 0.2190 0.5481 0.040 Uiso 1 1 calc R . . C12 C 0.12222(19) 0.26027(15) 0.50733(8) 0.0353(5) Uani 1 1 d . . . H12A H 0.1756 0.2689 0.5357 0.042 Uiso 1 1 calc R A . H12B H 0.0855 0.3176 0.4995 0.042 Uiso 1 1 calc R . . C13 C 0.19345(17) 0.22850(14) 0.46326(7) 0.0297(4) Uani 1 1 d . A . H13A H 0.2509 0.2745 0.4538 0.036 Uiso 1 1 calc R . . H13B H 0.2382 0.1751 0.4725 0.036 Uiso 1 1 calc R . . C14 C 0.53561(15) 0.03260(12) 0.34664(6) 0.0220(4) Uani 1 1 d . . . H14A H 0.5897 0.0428 0.3182 0.026 Uiso 1 1 calc R A . C15 C 0.59332(17) 0.07072(14) 0.39254(7) 0.0297(4) Uani 1 1 d . A . H15A H 0.6074 0.1344 0.3879 0.036 Uiso 1 1 calc R . . H15B H 0.5399 0.0633 0.4210 0.036 Uiso 1 1 calc R . . C16 C 0.70980(19) 0.02448(17) 0.40275(9) 0.0408(6) Uani 1 1 d . . . H16A H 0.7657 0.0370 0.3757 0.049 Uiso 1 1 calc R A . H16B H 0.7441 0.0478 0.4335 0.049 Uiso 1 1 calc R . . C17 C 0.6934(2) -0.07408(17) 0.40742(9) 0.0449(6) Uani 1 1 d . A . H17A H 0.6453 -0.0869 0.4369 0.054 Uiso 1 1 calc R . . H17B H 0.7713 -0.1024 0.4118 0.054 Uiso 1 1 calc R . . C18 C 0.63344(19) -0.11248(15) 0.36255(9) 0.0380(5) Uani 1 1 d . . . H18A H 0.6188 -0.1759 0.3679 0.046 Uiso 1 1 calc R A . H18B H 0.6861 -0.1064 0.3338 0.046 Uiso 1 1 calc R . . C19 C 0.51719(17) -0.06625(12) 0.35215(7) 0.0270(4) Uani 1 1 d . A . H19A H 0.4614 -0.0776 0.3794 0.032 Uiso 1 1 calc R . . H19B H 0.4823 -0.0901 0.3216 0.032 Uiso 1 1 calc R . . C20 C 0.3064(2) 0.00049(16) 0.45478(7) 0.0378(5) Uani 1 1 d . A . H20A H 0.2308 -0.0007 0.4722 0.057 Uiso 1 1 calc R . . H20B H 0.3637 0.0343 0.4740 0.057 Uiso 1 1 calc R . . H20C H 0.3353 -0.0597 0.4504 0.057 Uiso 1 1 calc R . . O1A O 0.18042(13) -0.02502(10) 0.34576(5) 0.0348(4) Uani 0.70 1 d PD A 1 C1A C 0.1948(3) -0.0553(3) 0.29531(12) 0.0367(10) Uani 0.70 1 d PD A 1 H1A1 H 0.2667 -0.0917 0.2920 0.044 Uiso 0.70 1 calc PR A 1 H1A2 H 0.2005 -0.0048 0.2725 0.044 Uiso 0.70 1 calc PR A 1 C2A C 0.0855(12) -0.1091(8) 0.28499(18) 0.0480(7) Uani 0.70 1 d PD A 1 H2A1 H 0.1012 -0.1554 0.2603 0.058 Uiso 0.70 1 calc PR A 1 H2A2 H 0.0199 -0.0715 0.2734 0.058 Uiso 0.70 1 calc PR A 1 C3A C 0.0584(3) -0.1491(2) 0.33573(17) 0.0383(10) Uani 0.70 1 d PD A 1 H3A1 H -0.0243 -0.1695 0.3381 0.046 Uiso 0.70 1 calc PR A 1 H3A2 H 0.1123 -0.1983 0.3437 0.046 Uiso 0.70 1 calc PR A 1 C4A C 0.0808(4) -0.0697(3) 0.36801(16) 0.0576(12) Uani 0.70 1 d PD A 1 H4A1 H 0.0108 -0.0308 0.3688 0.069 Uiso 0.70 1 calc PR A 1 H4A2 H 0.0997 -0.0881 0.4020 0.069 Uiso 0.70 1 calc PR A 1 O1B O 0.18042(13) -0.02502(10) 0.34576(5) 0.0348(4) Uani 0.30 1 d PD A 2 C1B C 0.1591(9) -0.0329(7) 0.2940(2) 0.0367(10) Uani 0.30 1 d PD A 2 H1B1 H 0.2344 -0.0392 0.2760 0.044 Uiso 0.30 1 calc PR A 2 H1B2 H 0.1176 0.0198 0.2815 0.044 Uiso 0.30 1 calc PR A 2 C2B C 0.084(3) -0.1139(19) 0.2872(4) 0.0480(7) Uani 0.30 1 d PD A 2 H2B1 H 0.1319 -0.1655 0.2777 0.058 Uiso 0.30 1 calc PR A 2 H2B2 H 0.0218 -0.1043 0.2622 0.058 Uiso 0.30 1 calc PR A 2 C3B C 0.0298(7) -0.1257(7) 0.3388(4) 0.0383(10) Uani 0.30 1 d PD A 2 H3B1 H -0.0350 -0.0835 0.3449 0.046 Uiso 0.30 1 calc PR A 2 H3B2 H 0.0009 -0.1864 0.3441 0.046 Uiso 0.30 1 calc PR A 2 C4B C 0.1380(7) -0.1056(4) 0.3702(3) 0.0324(17) Uani 0.30 1 d PD A 2 H4B1 H 0.1164 -0.0945 0.4049 0.039 Uiso 0.30 1 calc PR A 2 H4B2 H 0.1969 -0.1535 0.3686 0.039 Uiso 0.30 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 0.0236(3) 0.0202(3) 0.0182(3) 0.0016(2) 0.0016(2) 0.0005(2) N1 0.0205(7) 0.0220(8) 0.0256(8) 0.0014(6) 0.0025(6) 0.0004(6) N2 0.0210(7) 0.0201(8) 0.0199(7) 0.0002(6) -0.0002(6) -0.0001(6) C1 0.0184(8) 0.0198(9) 0.0337(10) 0.0026(7) -0.0008(7) 0.0007(7) C2 0.0235(9) 0.0195(9) 0.0259(9) 0.0054(7) -0.0029(7) -0.0027(7) C3 0.0277(10) 0.0260(10) 0.0324(10) 0.0082(8) -0.0071(8) -0.0026(8) C4 0.0349(11) 0.0335(11) 0.0241(9) 0.0095(8) -0.0079(8) -0.0078(9) C5 0.0314(10) 0.0308(11) 0.0218(9) 0.0033(8) -0.0010(7) -0.0066(8) C6 0.0236(9) 0.0198(9) 0.0215(8) 0.0031(7) -0.0005(7) -0.0063(7) C7 0.0219(9) 0.0199(9) 0.0234(9) -0.0017(7) 0.0027(7) -0.0046(7) C8 0.0220(9) 0.0254(10) 0.0289(10) 0.0014(8) 0.0038(7) 0.0043(7) C9 0.0237(10) 0.0465(13) 0.0316(11) -0.0054(9) 0.0005(8) -0.0116(9) C10 0.0235(10) 0.0604(16) 0.0335(11) -0.0024(10) 0.0069(8) -0.0086(10) C11 0.0299(10) 0.0421(13) 0.0276(10) 0.0000(9) 0.0081(8) -0.0017(9) C12 0.0345(11) 0.0371(12) 0.0344(11) -0.0121(9) 0.0092(9) -0.0055(9) C13 0.0217(9) 0.0333(11) 0.0342(11) -0.0081(9) 0.0073(8) -0.0072(8) C14 0.0195(8) 0.0252(10) 0.0213(8) -0.0011(7) -0.0001(7) 0.0015(7) C15 0.0293(10) 0.0316(11) 0.0283(10) -0.0036(8) -0.0046(8) -0.0049(8) C16 0.0281(11) 0.0583(16) 0.0362(11) 0.0031(11) -0.0112(9) -0.0045(10) C17 0.0334(12) 0.0572(16) 0.0442(13) 0.0113(11) -0.0095(10) 0.0123(11) C18 0.0354(12) 0.0355(12) 0.0431(13) 0.0032(10) 0.0028(9) 0.0124(9) C19 0.0270(10) 0.0246(10) 0.0295(10) -0.0029(8) -0.0006(8) 0.0035(8) C20 0.0497(14) 0.0400(13) 0.0238(10) 0.0074(9) 0.0063(9) 0.0116(10) O1A 0.0406(8) 0.0334(8) 0.0305(7) -0.0068(6) 0.0058(6) -0.0169(6) C1A 0.040(3) 0.041(3) 0.0295(12) 0.0005(13) -0.0058(14) -0.0081(17) C2A 0.0549(16) 0.0464(19) 0.0429(14) 0.0029(13) -0.0128(13) -0.0190(13) C3A 0.038(2) 0.031(2) 0.0458(16) -0.0150(17) 0.0104(16) -0.0104(16) C4A 0.055(3) 0.064(3) 0.053(2) -0.024(2) 0.026(2) -0.036(2) O1B 0.0406(8) 0.0334(8) 0.0305(7) -0.0068(6) 0.0058(6) -0.0169(6) C1B 0.040(3) 0.041(3) 0.0295(12) 0.0005(13) -0.0058(14) -0.0081(17) C2B 0.0549(16) 0.0464(19) 0.0429(14) 0.0029(13) -0.0128(13) -0.0190(13) C3B 0.038(2) 0.031(2) 0.0458(16) -0.0150(17) 0.0104(16) -0.0104(16) C4B 0.046(5) 0.024(4) 0.027(4) 0.000(3) 0.010(3) -0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O1A 2.0526(15) . ? Mg1 N2 2.0821(16) . ? Mg1 N1 2.0882(16) . ? Mg1 C20 2.116(2) . ? N1 C1 1.294(2) . ? N1 C8 1.478(2) . ? N2 C7 1.292(2) . ? N2 C14 1.479(2) . ? C1 C2 1.422(3) . ? C1 H1A 0.9500 . ? C2 C3 1.412(3) . ? C2 C6 1.447(3) . ? C3 C4 1.378(3) . ? C3 H3A 0.9500 . ? C4 C5 1.389(3) . ? C4 H4A 0.9500 . ? C5 C6 1.411(3) . ? C5 H5A 0.9500 . ? C6 C7 1.424(3) . ? C7 H7A 0.9500 . ? C8 C13 1.520(3) . ? C8 C9 1.525(3) . ? C8 H8A 1.0000 . ? C9 C10 1.530(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.510(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.512(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.526(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C19 1.525(3) . ? C14 C15 1.526(2) . ? C14 H14A 1.0000 . ? C15 C16 1.523(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.516(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.516(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.521(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? O1A C4A 1.452(3) . ? O1A C1A 1.459(3) . ? C1A C2A 1.512(6) . ? C1A H1A1 0.9900 . ? C1A H1A2 0.9900 . ? C2A C3A 1.542(6) . ? C2A H2A1 0.9900 . ? C2A H2A2 0.9900 . ? C3A C4A 1.515(4) . ? C3A H3A1 0.9900 . ? C3A H3A2 0.9900 . ? C4A H4A1 0.9900 . ? C4A H4A2 0.9900 . ? C1B C2B 1.512(8) . ? C1B H1B1 0.9900 . ? C1B H1B2 0.9900 . ? C2B C3B 1.544(9) . ? C2B H2B1 0.9900 . ? C2B H2B2 0.9900 . ? C3B C4B 1.527(8) . ? C3B H3B1 0.9900 . ? C3B H3B2 0.9900 . ? C4B H4B1 0.9900 . ? C4B H4B2 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 O1A Mg1 N2 99.77(6) . . ? O1A Mg1 N1 99.83(7) . . ? N2 Mg1 N1 103.96(6) . . ? O1A Mg1 C20 105.56(8) . . ? N2 Mg1 C20 122.38(8) . . ? N1 Mg1 C20 120.90(8) . . ? C1 N1 C8 115.63(15) . . ? C1 N1 Mg1 122.84(13) . . ? C8 N1 Mg1 119.55(11) . . ? C7 N2 C14 115.28(15) . . ? C7 N2 Mg1 124.94(13) . . ? C14 N2 Mg1 118.50(11) . . ? N1 C1 C2 130.85(17) . . ? N1 C1 H1A 114.6 . . ? C2 C1 H1A 114.6 . . ? C3 C2 C1 118.60(17) . . ? C3 C2 C6 106.14(16) . . ? C1 C2 C6 135.06(17) . . ? C4 C3 C2 110.01(18) . . ? C4 C3 H3A 125.0 . . ? C2 C3 H3A 125.0 . . ? C3 C4 C5 107.89(17) . . ? C3 C4 H4A 126.1 . . ? C5 C4 H4A 126.1 . . ? C4 C5 C6 109.56(18) . . ? C4 C5 H5A 125.2 . . ? C6 C5 H5A 125.2 . . ? C5 C6 C7 118.68(17) . . ? C5 C6 C2 106.37(16) . . ? C7 C6 C2 134.89(17) . . ? N2 C7 C6 129.89(17) . . ? N2 C7 H7A 115.1 . . ? C6 C7 H7A 115.1 . . ? N1 C8 C13 110.80(15) . . ? N1 C8 C9 110.99(16) . . ? C13 C8 C9 110.63(16) . . ? N1 C8 H8A 108.1 . . ? C13 C8 H8A 108.1 . . ? C9 C8 H8A 108.1 . . ? C8 C9 C10 110.83(18) . . ? C8 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C11 C10 C9 110.80(17) . . ? C11 C10 H10A 109.5 . . ? C9 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? C10 C11 C12 111.52(17) . . ? C10 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? C10 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? C11 C12 C13 111.20(17) . . ? C11 C12 H12A 109.4 . . ? C13 C12 H12A 109.4 . . ? C11 C12 H12B 109.4 . . ? C13 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C8 C13 C12 111.59(16) . . ? C8 C13 H13A 109.3 . . ? C12 C13 H13A 109.3 . . ? C8 C13 H13B 109.3 . . ? C12 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? N2 C14 C19 110.36(15) . . ? N2 C14 C15 111.04(15) . . ? C19 C14 C15 110.65(15) . . ? N2 C14 H14A 108.2 . . ? C19 C14 H14A 108.2 . . ? C15 C14 H14A 108.2 . . ? C16 C15 C14 110.29(17) . . ? C16 C15 H15A 109.6 . . ? C14 C15 H15A 109.6 . . ? C16 C15 H15B 109.6 . . ? C14 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? C17 C16 C15 111.44(18) . . ? C17 C16 H16A 109.3 . . ? C15 C16 H16A 109.3 . . ? C17 C16 H16B 109.3 . . ? C15 C16 H16B 109.3 . . ? H16A C16 H16B 108.0 . . ? C16 C17 C18 111.61(19) . . ? C16 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? C16 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? C17 C18 C19 111.18(18) . . ? C17 C18 H18A 109.4 . . ? C19 C18 H18A 109.4 . . ? C17 C18 H18B 109.4 . . ? C19 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C18 C19 C14 110.79(17) . . ? C18 C19 H19A 109.5 . . ? C14 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? Mg1 C20 H20A 109.5 . . ? Mg1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Mg1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C4A O1A C1A 109.5(2) . . ? C4A O1A Mg1 121.38(17) . . ? C1A O1A Mg1 129.04(18) . . ? O1A C1A C2A 104.7(3) . . ? O1A C1A H1A1 110.8 . . ? C2A C1A H1A1 110.8 . . ? O1A C1A H1A2 110.8 . . ? C2A C1A H1A2 110.8 . . ? H1A1 C1A H1A2 108.9 . . ? C1A C2A C3A 102.2(4) . . ? C1A C2A H2A1 111.3 . . ? C3A C2A H2A1 111.3 . . ? C1A C2A H2A2 111.3 . . ? C3A C2A H2A2 111.3 . . ? H2A1 C2A H2A2 109.2 . . ? C4A C3A C2A 99.9(4) . . ? C4A C3A H3A1 111.8 . . ? C2A C3A H3A1 111.8 . . ? C4A C3A H3A2 111.8 . . ? C2A C3A H3A2 111.8 . . ? H3A1 C3A H3A2 109.5 . . ? O1A C4A C3A 105.1(3) . . ? O1A C4A H4A1 110.7 . . ? C3A C4A H4A1 110.7 . . ? O1A C4A H4A2 110.7 . . ? C3A C4A H4A2 110.7 . . ? H4A1 C4A H4A2 108.8 . . ? C2B C1B H1B1 110.4 . . ? C2B C1B H1B2 110.4 . . ? H1B1 C1B H1B2 108.6 . . ? C1B C2B C3B 102.0(8) . . ? C1B C2B H2B1 111.4 . . ? C3B C2B H2B1 111.4 . . ? C1B C2B H2B2 111.4 . . ? C3B C2B H2B2 111.4 . . ? H2B1 C2B H2B2 109.2 . . ? C4B C3B C2B 99.7(9) . . ? C4B C3B H3B1 111.8 . . ? C2B C3B H3B1 111.8 . . ? C4B C3B H3B2 111.8 . . ? C2B C3B H3B2 111.8 . . ? H3B1 C3B H3B2 109.5 . . ? C3B C4B H4B1 111.8 . . ? C3B C4B H4B2 111.8 . . ? H4B1 C4B H4B2 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 O1A Mg1 N1 C1 -58.07(15) . . . . ? N2 Mg1 N1 C1 44.67(16) . . . . ? C20 Mg1 N1 C1 -172.97(15) . . . . ? O1A Mg1 N1 C8 105.22(13) . . . . ? N2 Mg1 N1 C8 -152.04(13) . . . . ? C20 Mg1 N1 C8 -9.67(17) . . . . ? O1A Mg1 N2 C7 61.01(16) . . . . ? N1 Mg1 N2 C7 -41.77(16) . . . . ? C20 Mg1 N2 C7 176.58(15) . . . . ? O1A Mg1 N2 C14 -105.37(13) . . . . ? N1 Mg1 N2 C14 151.85(12) . . . . ? C20 Mg1 N2 C14 10.20(16) . . . . ? C8 N1 C1 C2 177.49(18) . . . . ? Mg1 N1 C1 C2 -18.6(3) . . . . ? N1 C1 C2 C3 173.43(19) . . . . ? N1 C1 C2 C6 -12.5(4) . . . . ? C1 C2 C3 C4 176.92(17) . . . . ? C6 C2 C3 C4 1.3(2) . . . . ? C2 C3 C4 C5 -1.9(2) . . . . ? C3 C4 C5 C6 1.8(2) . . . . ? C4 C5 C6 C7 -178.52(17) . . . . ? C4 C5 C6 C2 -1.0(2) . . . . ? C3 C2 C6 C5 -0.2(2) . . . . ? C1 C2 C6 C5 -174.7(2) . . . . ? C3 C2 C6 C7 176.7(2) . . . . ? C1 C2 C6 C7 2.2(4) . . . . ? C14 N2 C7 C6 -179.98(18) . . . . ? Mg1 N2 C7 C6 13.3(3) . . . . ? C5 C6 C7 N2 -170.21(18) . . . . ? C2 C6 C7 N2 13.2(3) . . . . ? C1 N1 C8 C13 -134.57(18) . . . . ? Mg1 N1 C8 C13 60.96(18) . . . . ? C1 N1 C8 C9 102.10(19) . . . . ? Mg1 N1 C8 C9 -62.36(18) . . . . ? N1 C8 C9 C10 179.51(16) . . . . ? C13 C8 C9 C10 56.1(2) . . . . ? C8 C9 C10 C11 -56.7(3) . . . . ? C9 C10 C11 C12 56.4(3) . . . . ? C10 C11 C12 C13 -55.4(3) . . . . ? N1 C8 C13 C12 -178.79(17) . . . . ? C9 C8 C13 C12 -55.3(2) . . . . ? C11 C12 C13 C8 54.8(2) . . . . ? C7 N2 C14 C19 -110.97(18) . . . . ? Mg1 N2 C14 C19 56.70(17) . . . . ? C7 N2 C14 C15 125.94(17) . . . . ? Mg1 N2 C14 C15 -66.39(17) . . . . ? N2 C14 C15 C16 -179.96(16) . . . . ? C19 C14 C15 C16 57.1(2) . . . . ? C14 C15 C16 C17 -56.1(2) . . . . ? C15 C16 C17 C18 55.2(3) . . . . ? C16 C17 C18 C19 -54.8(3) . . . . ? C17 C18 C19 C14 55.8(2) . . . . ? N2 C14 C19 C18 179.51(15) . . . . ? C15 C14 C19 C18 -57.2(2) . . . . ? N2 Mg1 O1A C4A 168.9(3) . . . . ? N1 Mg1 O1A C4A -84.9(3) . . . . ? C20 Mg1 O1A C4A 41.2(3) . . . . ? N2 Mg1 O1A C1A -6.8(2) . . . . ? N1 Mg1 O1A C1A 99.3(2) . . . . ? C20 Mg1 O1A C1A -134.6(2) . . . . ? C4A O1A C1A C2A 9.7(7) . . . . ? Mg1 O1A C1A C2A -174.2(6) . . . . ? O1A C1A C2A C3A -32.6(10) . . . . ? C1A C2A C3A C4A 42.2(10) . . . . ? C1A O1A C4A C3A 17.8(5) . . . . ? Mg1 O1A C4A C3A -158.7(3) . . . . ? C2A C3A C4A O1A -36.9(8) . . . . ? C1B C2B C3B C4B -42(2) . . . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 29.06 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.540 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.056 data_fulmg23 _database_code_CSD 205885 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H54 Br2 Mg2 N4' _chemical_formula_sum 'C38 H54 Br2 Mg2 N4' _chemical_formula_weight 775.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' _symmetry_space_group_name_Hall '-P 2ybc' 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 11.354(5) _cell_length_b 26.306(5) _cell_length_c 12.779(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.925(5) _cell_angle_gamma 90.00 _cell_volume 3748(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9169 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 26 _exptl_crystal_description Plate _exptl_crystal_colour Colouress _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 2.229 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.518 _exptl_absorpt_correction_T_max 0.800 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 33990 _diffrn_reflns_av_R_equivalents 0.0604 _diffrn_reflns_av_sigmaI/netI 0.0667 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 29.03 _reflns_number_total 9169 _reflns_number_gt 6814 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER, 1995)' _computing_cell_refinement 'SMART (BRUKER, 1995)' _computing_data_reduction 'SHELXTL (Sheldrick, 1997)' _computing_structure_solution 'SHELXTL (Sheldrick, 1997)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0519P)^2^+0.1595P] 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_number_reflns 9169 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0746 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1094 _refine_ls_wR_factor_gt 0.1010 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Br1 Br 0.58395(3) 0.317394(11) 0.79781(2) 0.02116(9) Uani 1 1 d . . . Br2 Br 0.91340(3) 0.247320(12) 0.91978(2) 0.02860(9) Uani 1 1 d . . . Mg1 Mg 0.78242(8) 0.28025(4) 0.76304(7) 0.0195(2) Uani 1 1 d . . . N1 N 0.7218(2) 0.23433(8) 0.63339(18) 0.0180(5) Uani 1 1 d . . . N2 N 0.8491(2) 0.34430(9) 0.70108(18) 0.0202(5) Uani 1 1 d . . . C1 C 0.6520(3) 0.25286(11) 0.5516(2) 0.0193(6) Uani 1 1 d . . . H1 H 0.6134 0.2284 0.5020 0.023 Uiso 1 1 calc R . . C2 C 0.6228(2) 0.30502(10) 0.5232(2) 0.0181(6) Uani 1 1 d . . . C3 C 0.5211(3) 0.31480(11) 0.4436(2) 0.0216(6) Uani 1 1 d . . . H3 H 0.4680 0.2897 0.4081 0.026 Uiso 1 1 calc R . . C4 C 0.5102(3) 0.36709(11) 0.4247(2) 0.0234(7) Uani 1 1 d . . . H4 H 0.4474 0.3837 0.3773 0.028 Uiso 1 1 calc R . . C5 C 0.6086(3) 0.39029(11) 0.4884(2) 0.0222(6) Uani 1 1 d . . . H5 H 0.6255 0.4257 0.4890 0.027 Uiso 1 1 calc R . . C6 C 0.6799(3) 0.35367(11) 0.5521(2) 0.0194(6) Uani 1 1 d . . . C7 C 0.7880(3) 0.36912(11) 0.6231(2) 0.0211(6) Uani 1 1 d . . . H7 H 0.8177 0.4019 0.6105 0.025 Uiso 1 1 calc R . . C8 C 0.7306(3) 0.17836(10) 0.6359(2) 0.0191(6) Uani 1 1 d . . . H8 H 0.6951 0.1652 0.5634 0.023 Uiso 1 1 calc R . . C9 C 0.8604(3) 0.16125(11) 0.6629(3) 0.0252(7) Uani 1 1 d . . . H9A H 0.8986 0.1751 0.7332 0.030 Uiso 1 1 calc R . . H9B H 0.9045 0.1745 0.6089 0.030 Uiso 1 1 calc R . . C10 C 0.8676(3) 0.10308(11) 0.6656(3) 0.0277(7) Uani 1 1 d . . . H10A H 0.8378 0.0895 0.5931 0.033 Uiso 1 1 calc R . . H10B H 0.9523 0.0925 0.6879 0.033 Uiso 1 1 calc R . . C11 C 0.7937(3) 0.08090(11) 0.7421(3) 0.0285(7) Uani 1 1 d . . . H11A H 0.7960 0.0433 0.7388 0.034 Uiso 1 1 calc R . . H11B H 0.8289 0.0914 0.8159 0.034 Uiso 1 1 calc R . . C12 C 0.6651(3) 0.09884(11) 0.7144(3) 0.0265(7) Uani 1 1 d . . . H12A H 0.6195 0.0852 0.7669 0.032 Uiso 1 1 calc R . . H12B H 0.6278 0.0858 0.6431 0.032 Uiso 1 1 calc R . . C13 C 0.6592(3) 0.15661(11) 0.7144(2) 0.0239(7) Uani 1 1 d . . . H13A H 0.5746 0.1677 0.6947 0.029 Uiso 1 1 calc R . . H13B H 0.6919 0.1696 0.7868 0.029 Uiso 1 1 calc R . . C14 C 0.9550(2) 0.36970(11) 0.7673(2) 0.0225(6) Uani 1 1 d . . . H14 H 1.0086 0.3423 0.8040 0.027 Uiso 1 1 calc R . . C15 C 1.0293(3) 0.40185(16) 0.7059(3) 0.0453(10) Uani 1 1 d . . . H15A H 0.9787 0.4290 0.6670 0.054 Uiso 1 1 calc R . . H15B H 1.0598 0.3805 0.6530 0.054 Uiso 1 1 calc R . . C16 C 1.1350(3) 0.42558(16) 0.7830(3) 0.0479(10) Uani 1 1 d . . . H16A H 1.1878 0.3983 0.8188 0.058 Uiso 1 1 calc R . . H16B H 1.1826 0.4469 0.7426 0.058 Uiso 1 1 calc R . . C17 C 1.0917(3) 0.45750(14) 0.8654(3) 0.0404(9) Uani 1 1 d . . . H17A H 1.0434 0.4862 0.8301 0.048 Uiso 1 1 calc R . . H17B H 1.1614 0.4718 0.9151 0.048 Uiso 1 1 calc R . . C18 C 1.0168(3) 0.42647(13) 0.9270(3) 0.0368(8) Uani 1 1 d . . . H18A H 0.9849 0.4488 0.9774 0.044 Uiso 1 1 calc R . . H18B H 1.0677 0.4003 0.9690 0.044 Uiso 1 1 calc R . . C19 C 0.9129(3) 0.40078(12) 0.8532(2) 0.0279(7) Uani 1 1 d . . . H19A H 0.8701 0.3783 0.8956 0.033 Uiso 1 1 calc R . . H19B H 0.8557 0.4270 0.8192 0.033 Uiso 1 1 calc R . . Mg2 Mg 0.47950(8) 0.35358(3) 0.61511(7) 0.0174(2) Uani 1 1 d . . . N3 N 0.4489(2) 0.42723(8) 0.65156(18) 0.0166(5) Uani 1 1 d . . . N4 N 0.3167(2) 0.31863(9) 0.58794(19) 0.0213(5) Uani 1 1 d . . . C20 C 0.3561(2) 0.45338(11) 0.6069(2) 0.0193(6) Uani 1 1 d . . . H20 H 0.3588 0.4884 0.6254 0.023 Uiso 1 1 calc R . . C21 C 0.2515(2) 0.43819(10) 0.5352(2) 0.0184(6) Uani 1 1 d . . . C22 C 0.1702(3) 0.47528(11) 0.4873(2) 0.0237(7) Uani 1 1 d . . . H22 H 0.1798 0.5108 0.4994 0.028 Uiso 1 1 calc R . . C23 C 0.0739(3) 0.45312(12) 0.4201(2) 0.0285(7) Uani 1 1 d . . . H23 H 0.0084 0.4704 0.3774 0.034 Uiso 1 1 calc R . . C24 C 0.0913(3) 0.40097(11) 0.4268(2) 0.0247(7) Uani 1 1 d . . . H24 H 0.0376 0.3765 0.3895 0.030 Uiso 1 1 calc R . . C25 C 0.1993(2) 0.38931(11) 0.4962(2) 0.0204(6) Uani 1 1 d . . . C26 C 0.2232(2) 0.33825(11) 0.5274(2) 0.0201(6) Uani 1 1 d . . . H26 H 0.1615 0.3148 0.4998 0.024 Uiso 1 1 calc R . . C27 C 0.5465(2) 0.45406(10) 0.7236(2) 0.0183(6) Uani 1 1 d . . . H27 H 0.6175 0.4308 0.7347 0.022 Uiso 1 1 calc R . . C28 C 0.5864(3) 0.50364(11) 0.6782(2) 0.0236(7) Uani 1 1 d . . . H28A H 0.6081 0.4969 0.6080 0.028 Uiso 1 1 calc R . . H28B H 0.5192 0.5282 0.6674 0.028 Uiso 1 1 calc R . . C29 C 0.6936(3) 0.52663(12) 0.7527(3) 0.0300(7) Uani 1 1 d . . . H29A H 0.7633 0.5035 0.7582 0.036 Uiso 1 1 calc R . . H29B H 0.7152 0.5594 0.7231 0.036 Uiso 1 1 calc R . . C30 C 0.6652(3) 0.53527(12) 0.8625(3) 0.0344(8) Uani 1 1 d . . . H30A H 0.6021 0.5616 0.8580 0.041 Uiso 1 1 calc R . . H30B H 0.7378 0.5480 0.9108 0.041 Uiso 1 1 calc R . . C31 C 0.6226(3) 0.48671(13) 0.9088(2) 0.0321(8) Uani 1 1 d . . . H31A H 0.5993 0.4945 0.9779 0.039 Uiso 1 1 calc R . . H31B H 0.6893 0.4619 0.9220 0.039 Uiso 1 1 calc R . . C32 C 0.5156(3) 0.46324(12) 0.8333(2) 0.0247(7) Uani 1 1 d . . . H32A H 0.4936 0.4306 0.8631 0.030 Uiso 1 1 calc R . . H32B H 0.4458 0.4864 0.8264 0.030 Uiso 1 1 calc R . . C33 C 0.3071(3) 0.26455(11) 0.6203(3) 0.0295(8) Uani 1 1 d . . . H33 H 0.3869 0.2549 0.6636 0.035 Uiso 1 1 calc R . . C34 C 0.2809(3) 0.22739(12) 0.5280(3) 0.0336(8) Uani 1 1 d . . . H34A H 0.3433 0.2304 0.4837 0.040 Uiso 1 1 calc R . . H34B H 0.2024 0.2356 0.4827 0.040 Uiso 1 1 calc R . . C35 C 0.2787(3) 0.17300(12) 0.5697(3) 0.0396(9) Uani 1 1 d . . . H35A H 0.2600 0.1492 0.5089 0.048 Uiso 1 1 calc R . . H35B H 0.3587 0.1641 0.6114 0.048 Uiso 1 1 calc R . . C36 C 0.1860(3) 0.16770(12) 0.6391(3) 0.0374(9) Uani 1 1 d . . . H36A H 0.1875 0.1325 0.6667 0.045 Uiso 1 1 calc R . . H36B H 0.1054 0.1740 0.5957 0.045 Uiso 1 1 calc R . . C37 C 0.2084(4) 0.20453(13) 0.7319(3) 0.0469(10) Uani 1 1 d . . . H37A H 0.2843 0.1955 0.7804 0.056 Uiso 1 1 calc R . . H37B H 0.1425 0.2018 0.7725 0.056 Uiso 1 1 calc R . . C38 C 0.2160(3) 0.25922(12) 0.6929(3) 0.0364(9) Uani 1 1 d . . . H38A H 0.1361 0.2699 0.6538 0.044 Uiso 1 1 calc R . . H38B H 0.2388 0.2820 0.7551 0.044 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 Br1 0.02232(16) 0.02322(16) 0.01803(15) 0.00402(12) 0.00404(11) 0.00401(12) Br2 0.02739(18) 0.03274(19) 0.02251(17) 0.00188(13) -0.00332(13) 0.00636(14) Mg1 0.0216(5) 0.0184(5) 0.0174(5) -0.0002(4) 0.0007(4) 0.0002(4) N1 0.0226(13) 0.0158(12) 0.0155(12) -0.0002(9) 0.0034(10) 0.0031(10) N2 0.0188(13) 0.0217(13) 0.0196(13) -0.0037(10) 0.0027(10) -0.0023(10) C1 0.0231(16) 0.0176(15) 0.0176(15) -0.0039(11) 0.0048(12) -0.0003(12) C2 0.0207(15) 0.0189(15) 0.0153(14) 0.0018(11) 0.0046(11) 0.0028(11) C3 0.0239(16) 0.0230(15) 0.0176(15) -0.0009(12) 0.0034(12) 0.0003(12) C4 0.0249(16) 0.0251(16) 0.0193(15) 0.0034(12) 0.0021(12) 0.0030(13) C5 0.0291(17) 0.0167(15) 0.0235(16) 0.0045(12) 0.0114(13) 0.0029(12) C6 0.0210(15) 0.0192(15) 0.0192(15) 0.0029(11) 0.0067(12) 0.0013(12) C7 0.0208(15) 0.0179(15) 0.0253(16) -0.0005(12) 0.0061(12) -0.0008(12) C8 0.0241(16) 0.0152(14) 0.0174(14) -0.0002(11) 0.0023(12) 0.0006(12) C9 0.0248(16) 0.0220(16) 0.0306(17) 0.0039(13) 0.0104(13) 0.0041(13) C10 0.0264(17) 0.0235(17) 0.0335(18) -0.0005(13) 0.0061(14) 0.0066(13) C11 0.0361(19) 0.0162(15) 0.0337(18) 0.0007(13) 0.0077(15) 0.0018(13) C12 0.0290(17) 0.0201(16) 0.0318(18) 0.0028(13) 0.0089(14) -0.0036(13) C13 0.0183(15) 0.0205(16) 0.0332(18) 0.0001(13) 0.0054(13) 0.0028(12) C14 0.0156(15) 0.0233(16) 0.0271(16) -0.0019(12) 0.0003(12) -0.0025(12) C15 0.038(2) 0.069(3) 0.033(2) -0.0106(19) 0.0167(17) -0.0269(19) C16 0.031(2) 0.072(3) 0.043(2) -0.004(2) 0.0122(17) -0.0231(19) C17 0.046(2) 0.043(2) 0.0287(19) 0.0009(16) -0.0025(16) -0.0184(17) C18 0.040(2) 0.040(2) 0.0277(18) -0.0042(15) 0.0012(15) -0.0123(16) C19 0.0285(17) 0.0333(18) 0.0217(16) -0.0026(13) 0.0044(13) -0.0045(14) Mg2 0.0176(5) 0.0146(5) 0.0195(5) -0.0002(4) 0.0022(4) 0.0003(4) N3 0.0171(12) 0.0153(12) 0.0173(12) -0.0002(9) 0.0028(9) -0.0002(9) N4 0.0204(13) 0.0151(12) 0.0284(14) 0.0018(10) 0.0045(11) -0.0001(10) C20 0.0221(15) 0.0154(14) 0.0216(15) 0.0014(11) 0.0075(12) -0.0015(12) C21 0.0168(14) 0.0181(15) 0.0208(15) 0.0025(11) 0.0049(12) 0.0017(11) C22 0.0193(15) 0.0183(15) 0.0329(18) 0.0042(13) 0.0035(13) 0.0004(12) C23 0.0224(17) 0.0283(17) 0.0312(18) 0.0097(14) -0.0041(14) 0.0061(13) C24 0.0223(16) 0.0239(16) 0.0259(16) -0.0031(13) -0.0007(13) 0.0008(13) C25 0.0175(15) 0.0258(16) 0.0187(15) -0.0001(12) 0.0053(11) -0.0012(12) C26 0.0150(14) 0.0211(15) 0.0244(16) -0.0033(12) 0.0043(12) -0.0011(12) C27 0.0180(15) 0.0148(14) 0.0218(15) -0.0012(11) 0.0030(12) 0.0002(11) C28 0.0268(17) 0.0162(15) 0.0271(17) 0.0003(12) 0.0030(13) -0.0015(12) C29 0.0269(18) 0.0182(16) 0.042(2) 0.0037(14) -0.0012(15) -0.0021(13) C30 0.0289(18) 0.0270(18) 0.042(2) -0.0123(15) -0.0058(15) -0.0035(14) C31 0.0310(18) 0.039(2) 0.0239(17) -0.0093(14) -0.0020(14) 0.0010(15) C32 0.0247(16) 0.0256(16) 0.0234(16) -0.0034(13) 0.0036(13) -0.0009(13) C33 0.0217(17) 0.0181(16) 0.044(2) 0.0057(14) -0.0069(15) -0.0010(12) C34 0.0303(19) 0.0208(17) 0.052(2) -0.0071(15) 0.0135(16) -0.0022(14) C35 0.0218(18) 0.0166(17) 0.078(3) -0.0016(17) 0.0032(17) -0.0015(13) C36 0.031(2) 0.0213(17) 0.055(2) 0.0088(16) -0.0041(17) -0.0072(14) C37 0.062(3) 0.037(2) 0.036(2) 0.0126(17) -0.0070(19) -0.0189(19) C38 0.055(2) 0.0255(18) 0.0258(18) 0.0024(14) 0.0011(16) -0.0107(16) _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 Br1 Mg1 2.5710(14) . ? Br1 Mg2 2.5912(12) . ? Br2 Mg1 2.4177(12) . ? Mg1 N1 2.061(2) . ? Mg1 N2 2.066(3) . ? N1 C1 1.282(3) . ? N1 C8 1.475(3) . ? N2 C7 1.280(3) . ? N2 C14 1.491(3) . ? C1 C2 1.442(4) . ? C1 H1 0.9500 . ? C2 C3 1.410(4) . ? C2 C6 1.451(4) . ? C2 Mg2 2.526(3) . ? C3 C4 1.398(4) . ? C3 Mg2 2.542(3) . ? C3 H3 0.9500 . ? C4 C5 1.393(4) . ? C4 Mg2 2.548(3) . ? C4 H4 0.9500 . ? C5 C6 1.413(4) . ? C5 Mg2 2.570(3) . ? C5 H5 0.9500 . ? C6 C7 1.439(4) . ? C6 Mg2 2.553(3) . ? C7 H7 0.9500 . ? C8 C13 1.516(4) . ? C8 C9 1.517(4) . ? C8 H8 1.0000 . ? C9 C10 1.532(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.520(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.511(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.521(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.514(4) . ? C14 C19 1.517(4) . ? C14 H14 1.0000 . ? C15 C16 1.534(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.501(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.504(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.522(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? Mg2 N4 2.035(3) . ? Mg2 N3 2.038(2) . ? N3 C20 1.297(3) . ? N3 C27 1.478(3) . ? N4 C26 1.296(4) . ? N4 C33 1.491(4) . ? C20 C21 1.413(4) . ? C20 H20 0.9500 . ? C21 C22 1.402(4) . ? C21 C25 1.463(4) . ? C22 C23 1.385(4) . ? C22 H22 0.9500 . ? C23 C24 1.386(4) . ? C23 H23 0.9500 . ? C24 C25 1.404(4) . ? C24 H24 0.9500 . ? C25 C26 1.412(4) . ? C26 H26 0.9500 . ? C27 C32 1.526(4) . ? C27 C28 1.531(4) . ? C27 H27 1.0000 . ? C28 C29 1.521(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.516(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.524(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.531(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.518(4) . ? C33 C38 1.521(5) . ? C33 H33 1.0000 . ? C34 C35 1.529(4) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.505(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.516(5) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.531(4) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 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 Mg1 Br1 Mg2 104.50(4) . . ? N1 Mg1 N2 105.12(10) . . ? N1 Mg1 Br2 121.02(8) . . ? N2 Mg1 Br2 113.40(8) . . ? N1 Mg1 Br1 101.05(8) . . ? N2 Mg1 Br1 98.82(8) . . ? Br2 Mg1 Br1 114.50(4) . . ? C1 N1 C8 115.2(2) . . ? C1 N1 Mg1 119.53(19) . . ? C8 N1 Mg1 123.80(18) . . ? C7 N2 C14 118.3(2) . . ? C7 N2 Mg1 122.0(2) . . ? C14 N2 Mg1 117.57(18) . . ? N1 C1 C2 130.1(3) . . ? N1 C1 H1 114.9 . . ? C2 C1 H1 114.9 . . ? C3 C2 C1 118.2(3) . . ? C3 C2 C6 106.8(2) . . ? C1 C2 C6 134.8(3) . . ? C3 C2 Mg2 74.45(16) . . ? C1 C2 Mg2 120.11(19) . . ? C6 C2 Mg2 74.44(16) . . ? C4 C3 C2 109.7(3) . . ? C4 C3 Mg2 74.29(17) . . ? C2 C3 Mg2 73.23(16) . . ? C4 C3 H3 125.1 . . ? C2 C3 H3 125.1 . . ? Mg2 C3 H3 119.1 . . ? C5 C4 C3 107.2(3) . . ? C5 C4 Mg2 75.08(17) . . ? C3 C4 Mg2 73.83(16) . . ? C5 C4 H4 126.4 . . ? C3 C4 H4 126.4 . . ? Mg2 C4 H4 116.8 . . ? C4 C5 C6 110.3(3) . . ? C4 C5 Mg2 73.33(17) . . ? C6 C5 Mg2 73.36(16) . . ? C4 C5 H5 124.9 . . ? C6 C5 H5 124.9 . . ? Mg2 C5 H5 120.1 . . ? C5 C6 C7 119.8(3) . . ? C5 C6 C2 106.0(2) . . ? C7 C6 C2 134.1(3) . . ? C5 C6 Mg2 74.62(16) . . ? C7 C6 Mg2 120.38(19) . . ? C2 C6 Mg2 72.38(16) . . ? N2 C7 C6 128.2(3) . . ? N2 C7 H7 115.9 . . ? C6 C7 H7 115.9 . . ? N1 C8 C13 110.4(2) . . ? N1 C8 C9 111.1(2) . . ? C13 C8 C9 110.9(2) . . ? N1 C8 H8 108.1 . . ? C13 C8 H8 108.1 . . ? C9 C8 H8 108.1 . . ? C8 C9 C10 110.3(2) . . ? C8 C9 H9A 109.6 . . ? C10 C9 H9A 109.6 . . ? C8 C9 H9B 109.6 . . ? C10 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C11 C10 C9 111.4(2) . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C12 C11 C10 110.8(3) . . ? C12 C11 H11A 109.5 . . ? C10 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C11 C12 C13 110.7(2) . . ? C11 C12 H12A 109.5 . . ? C13 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? C8 C13 C12 110.3(2) . . ? C8 C13 H13A 109.6 . . ? C12 C13 H13A 109.6 . . ? C8 C13 H13B 109.6 . . ? C12 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? N2 C14 C15 115.1(2) . . ? N2 C14 C19 108.8(2) . . ? C15 C14 C19 110.9(3) . . ? N2 C14 H14 107.2 . . ? C15 C14 H14 107.2 . . ? C19 C14 H14 107.2 . . ? C14 C15 C16 109.8(3) . . ? C14 C15 H15A 109.7 . . ? C16 C15 H15A 109.7 . . ? C14 C15 H15B 109.7 . . ? C16 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? C17 C16 C15 111.0(3) . . ? C17 C16 H16A 109.4 . . ? C15 C16 H16A 109.4 . . ? C17 C16 H16B 109.4 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C16 C17 C18 110.9(3) . . ? C16 C17 H17A 109.5 . . ? C18 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 108.0 . . ? C17 C18 C19 111.4(3) . . ? C17 C18 H18A 109.3 . . ? C19 C18 H18A 109.3 . . ? C17 C18 H18B 109.3 . . ? C19 C18 H18B 109.3 . . ? H18A C18 H18B 108.0 . . ? C14 C19 C18 112.0(3) . . ? C14 C19 H19A 109.2 . . ? C18 C19 H19A 109.2 . . ? C14 C19 H19B 109.2 . . ? C18 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? N4 Mg2 N3 106.26(10) . . ? N4 Mg2 C2 109.67(10) . . ? N3 Mg2 C2 137.70(10) . . ? N4 Mg2 C3 89.02(10) . . ? N3 Mg2 C3 130.26(10) . . ? C2 Mg2 C3 32.32(9) . . ? N4 Mg2 C4 100.62(10) . . ? N3 Mg2 C4 98.39(10) . . ? C2 Mg2 C4 53.83(9) . . ? C3 Mg2 C4 31.88(9) . . ? N4 Mg2 C6 141.43(10) . . ? N3 Mg2 C6 105.77(10) . . ? C2 Mg2 C6 33.18(9) . . ? C3 Mg2 C6 53.58(9) . . ? C4 Mg2 C6 53.67(9) . . ? N4 Mg2 C5 132.13(11) . . ? N3 Mg2 C5 85.93(10) . . ? C2 Mg2 C5 53.31(9) . . ? C3 Mg2 C5 52.12(10) . . ? C4 Mg2 C5 31.59(9) . . ? C6 Mg2 C5 32.02(9) . . ? N4 Mg2 Br1 103.51(8) . . ? N3 Mg2 Br1 102.24(7) . . ? C2 Mg2 Br1 90.46(7) . . ? C3 Mg2 Br1 120.10(8) . . ? C4 Mg2 Br1 142.17(8) . . ? C6 Mg2 Br1 90.07(7) . . ? C5 Mg2 Br1 119.17(8) . . ? C20 N3 C27 118.1(2) . . ? C20 N3 Mg2 124.28(19) . . ? C27 N3 Mg2 117.16(17) . . ? C26 N4 C33 116.8(2) . . ? C26 N4 Mg2 122.4(2) . . ? C33 N4 Mg2 119.67(18) . . ? N3 C20 C21 130.4(3) . . ? N3 C20 H20 114.8 . . ? C21 C20 H20 114.8 . . ? C22 C21 C20 119.3(3) . . ? C22 C21 C25 105.8(2) . . ? C20 C21 C25 134.9(3) . . ? C23 C22 C21 110.8(3) . . ? C23 C22 H22 124.6 . . ? C21 C22 H22 124.6 . . ? C22 C23 C24 107.0(3) . . ? C22 C23 H23 126.5 . . ? C24 C23 H23 126.5 . . ? C23 C24 C25 110.6(3) . . ? C23 C24 H24 124.7 . . ? C25 C24 H24 124.7 . . ? C24 C25 C26 118.9(3) . . ? C24 C25 C21 105.8(2) . . ? C26 C25 C21 134.1(3) . . ? N4 C26 C25 129.7(3) . . ? N4 C26 H26 115.2 . . ? C25 C26 H26 115.2 . . ? N3 C27 C32 111.8(2) . . ? N3 C27 C28 114.3(2) . . ? C32 C27 C28 110.4(2) . . ? N3 C27 H27 106.6 . . ? C32 C27 H27 106.6 . . ? C28 C27 H27 106.6 . . ? C29 C28 C27 111.2(2) . . ? C29 C28 H28A 109.4 . . ? C27 C28 H28A 109.4 . . ? C29 C28 H28B 109.4 . . ? C27 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C30 C29 C28 110.7(3) . . ? C30 C29 H29A 109.5 . . ? C28 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? C29 C30 C31 111.9(3) . . ? C29 C30 H30A 109.2 . . ? C31 C30 H30A 109.2 . . ? C29 C30 H30B 109.2 . . ? C31 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? C30 C31 C32 111.4(3) . . ? C30 C31 H31A 109.3 . . ? C32 C31 H31A 109.3 . . ? C30 C31 H31B 109.3 . . ? C32 C31 H31B 109.3 . . ? H31A C31 H31B 108.0 . . ? C27 C32 C31 110.5(3) . . ? C27 C32 H32A 109.6 . . ? C31 C32 H32A 109.6 . . ? C27 C32 H32B 109.6 . . ? C31 C32 H32B 109.6 . . ? H32A C32 H32B 108.1 . . ? N4 C33 C34 114.3(3) . . ? N4 C33 C38 110.5(3) . . ? C34 C33 C38 111.0(3) . . ? N4 C33 H33 106.8 . . ? C34 C33 H33 106.8 . . ? C38 C33 H33 106.8 . . ? C33 C34 C35 110.2(3) . . ? C33 C34 H34A 109.6 . . ? C35 C34 H34A 109.6 . . ? C33 C34 H34B 109.6 . . ? C35 C34 H34B 109.6 . . ? H34A C34 H34B 108.1 . . ? C36 C35 C34 110.6(3) . . ? C36 C35 H35A 109.5 . . ? C34 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? C35 C36 C37 111.7(3) . . ? C35 C36 H36A 109.3 . . ? C37 C36 H36A 109.3 . . ? C35 C36 H36B 109.3 . . ? C37 C36 H36B 109.3 . . ? H36A C36 H36B 107.9 . . ? C36 C37 C38 110.9(3) . . ? C36 C37 H37A 109.5 . . ? C38 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? C38 C37 H37B 109.5 . . ? H37A C37 H37B 108.0 . . ? C33 C38 C37 111.9(3) . . ? C33 C38 H38A 109.2 . . ? C37 C38 H38A 109.2 . . ? C33 C38 H38B 109.2 . . ? C37 C38 H38B 109.2 . . ? H38A C38 H38B 107.9 . . ? 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 Mg2 Br1 Mg1 N1 -52.14(8) . . . . ? Mg2 Br1 Mg1 N2 55.27(8) . . . . ? Mg2 Br1 Mg1 Br2 176.10(4) . . . . ? N2 Mg1 N1 C1 -50.3(2) . . . . ? Br2 Mg1 N1 C1 179.67(19) . . . . ? Br1 Mg1 N1 C1 52.0(2) . . . . ? N2 Mg1 N1 C8 144.0(2) . . . . ? Br2 Mg1 N1 C8 14.0(2) . . . . ? Br1 Mg1 N1 C8 -113.6(2) . . . . ? N1 Mg1 N2 C7 51.1(2) . . . . ? Br2 Mg1 N2 C7 -174.6(2) . . . . ? Br1 Mg1 N2 C7 -53.0(2) . . . . ? N1 Mg1 N2 C14 -145.94(19) . . . . ? Br2 Mg1 N2 C14 -11.6(2) . . . . ? Br1 Mg1 N2 C14 110.00(19) . . . . ? C8 N1 C1 C2 -179.7(3) . . . . ? Mg1 N1 C1 C2 13.4(4) . . . . ? N1 C1 C2 C3 -164.0(3) . . . . ? N1 C1 C2 C6 21.7(5) . . . . ? N1 C1 C2 Mg2 -76.3(4) . . . . ? C1 C2 C3 C4 -177.9(2) . . . . ? C6 C2 C3 C4 -2.1(3) . . . . ? Mg2 C2 C3 C4 65.9(2) . . . . ? C1 C2 C3 Mg2 116.2(2) . . . . ? C6 C2 C3 Mg2 -68.01(19) . . . . ? C2 C3 C4 C5 3.1(3) . . . . ? Mg2 C3 C4 C5 68.3(2) . . . . ? C2 C3 C4 Mg2 -65.2(2) . . . . ? C3 C4 C5 C6 -2.9(3) . . . . ? Mg2 C4 C5 C6 64.6(2) . . . . ? C3 C4 C5 Mg2 -67.4(2) . . . . ? C4 C5 C6 C7 178.9(3) . . . . ? Mg2 C5 C6 C7 -116.5(3) . . . . ? C4 C5 C6 C2 1.5(3) . . . . ? Mg2 C5 C6 C2 66.09(19) . . . . ? C4 C5 C6 Mg2 -64.6(2) . . . . ? C3 C2 C6 C5 0.4(3) . . . . ? C1 C2 C6 C5 175.1(3) . . . . ? Mg2 C2 C6 C5 -67.65(19) . . . . ? C3 C2 C6 C7 -176.4(3) . . . . ? C1 C2 C6 C7 -1.7(6) . . . . ? Mg2 C2 C6 C7 115.5(3) . . . . ? C3 C2 C6 Mg2 68.0(2) . . . . ? C1 C2 C6 Mg2 -117.2(3) . . . . ? C14 N2 C7 C6 -176.6(3) . . . . ? Mg1 N2 C7 C6 -13.8(4) . . . . ? C5 C6 C7 N2 164.1(3) . . . . ? C2 C6 C7 N2 -19.5(5) . . . . ? Mg2 C6 C7 N2 75.1(4) . . . . ? C1 N1 C8 C13 -104.2(3) . . . . ? Mg1 N1 C8 C13 62.0(3) . . . . ? C1 N1 C8 C9 132.4(3) . . . . ? Mg1 N1 C8 C9 -61.4(3) . . . . ? N1 C8 C9 C10 179.8(2) . . . . ? C13 C8 C9 C10 56.6(3) . . . . ? C8 C9 C10 C11 -55.3(3) . . . . ? C9 C10 C11 C12 55.6(3) . . . . ? C10 C11 C12 C13 -56.8(3) . . . . ? N1 C8 C13 C12 178.2(2) . . . . ? C9 C8 C13 C12 -58.2(3) . . . . ? C11 C12 C13 C8 58.1(3) . . . . ? C7 N2 C14 C15 -39.4(4) . . . . ? Mg1 N2 C14 C15 156.9(2) . . . . ? C7 N2 C14 C19 85.7(3) . . . . ? Mg1 N2 C14 C19 -77.9(3) . . . . ? N2 C14 C15 C16 -179.9(3) . . . . ? C19 C14 C15 C16 56.1(4) . . . . ? C14 C15 C16 C17 -58.3(4) . . . . ? C15 C16 C17 C18 57.9(4) . . . . ? C16 C17 C18 C19 -55.3(4) . . . . ? N2 C14 C19 C18 177.9(2) . . . . ? C15 C14 C19 C18 -54.5(4) . . . . ? C17 C18 C19 C14 53.8(4) . . . . ? C3 C2 Mg2 N4 53.20(19) . . . . ? C1 C2 Mg2 N4 -60.8(2) . . . . ? C6 C2 Mg2 N4 166.04(16) . . . . ? C3 C2 Mg2 N3 -93.4(2) . . . . ? C1 C2 Mg2 N3 152.7(2) . . . . ? C6 C2 Mg2 N3 19.5(2) . . . . ? C1 C2 Mg2 C3 -114.0(3) . . . . ? C6 C2 Mg2 C3 112.8(2) . . . . ? C3 C2 Mg2 C4 -35.72(16) . . . . ? C1 C2 Mg2 C4 -149.7(3) . . . . ? C6 C2 Mg2 C4 77.12(17) . . . . ? C3 C2 Mg2 C6 -112.8(2) . . . . ? C1 C2 Mg2 C6 133.2(3) . . . . ? C3 C2 Mg2 C5 -75.27(18) . . . . ? C1 C2 Mg2 C5 170.8(3) . . . . ? C6 C2 Mg2 C5 37.57(15) . . . . ? C3 C2 Mg2 Br1 157.73(16) . . . . ? C1 C2 Mg2 Br1 43.8(2) . . . . ? C6 C2 Mg2 Br1 -89.43(15) . . . . ? C4 C3 Mg2 N4 112.12(18) . . . . ? C2 C3 Mg2 N4 -131.05(18) . . . . ? C4 C3 Mg2 N3 1.5(2) . . . . ? C2 C3 Mg2 N3 118.31(18) . . . . ? C4 C3 Mg2 C2 -116.8(3) . . . . ? C2 C3 Mg2 C4 116.8(3) . . . . ? C4 C3 Mg2 C6 -78.01(19) . . . . ? C2 C3 Mg2 C6 38.82(16) . . . . ? C4 C3 Mg2 C5 -37.57(17) . . . . ? C2 C3 Mg2 C5 79.26(18) . . . . ? C4 C3 Mg2 Br1 -142.81(16) . . . . ? C2 C3 Mg2 Br1 -25.98(19) . . . . ? C5 C4 Mg2 N4 176.27(17) . . . . ? C3 C4 Mg2 N4 -70.46(18) . . . . ? C5 C4 Mg2 N3 67.87(18) . . . . ? C3 C4 Mg2 N3 -178.85(18) . . . . ? C5 C4 Mg2 C2 -77.05(18) . . . . ? C3 C4 Mg2 C2 36.22(17) . . . . ? C5 C4 Mg2 C3 -113.3(3) . . . . ? C5 C4 Mg2 C6 -35.58(16) . . . . ? C3 C4 Mg2 C6 77.69(19) . . . . ? C3 C4 Mg2 C5 113.3(3) . . . . ? C5 C4 Mg2 Br1 -54.8(2) . . . . ? C3 C4 Mg2 Br1 58.5(2) . . . . ? C5 C6 Mg2 N4 91.4(2) . . . . ? C7 C6 Mg2 N4 -152.7(2) . . . . ? C2 C6 Mg2 N4 -21.4(2) . . . . ? C5 C6 Mg2 N3 -53.78(18) . . . . ? C7 C6 Mg2 N3 62.1(2) . . . . ? C2 C6 Mg2 N3 -166.53(16) . . . . ? C5 C6 Mg2 C2 112.7(2) . . . . ? C7 C6 Mg2 C2 -131.4(3) . . . . ? C5 C6 Mg2 C3 74.99(18) . . . . ? C7 C6 Mg2 C3 -169.1(3) . . . . ? C2 C6 Mg2 C3 -37.76(15) . . . . ? C5 C6 Mg2 C4 35.09(16) . . . . ? C7 C6 Mg2 C4 151.0(3) . . . . ? C2 C6 Mg2 C4 -77.65(17) . . . . ? C7 C6 Mg2 C5 115.9(3) . . . . ? C2 C6 Mg2 C5 -112.7(2) . . . . ? C5 C6 Mg2 Br1 -156.53(16) . . . . ? C7 C6 Mg2 Br1 -40.6(2) . . . . ? C2 C6 Mg2 Br1 90.73(15) . . . . ? C4 C5 Mg2 N4 -4.9(2) . . . . ? C6 C5 Mg2 N4 -122.81(18) . . . . ? C4 C5 Mg2 N3 -113.25(18) . . . . ? C6 C5 Mg2 N3 128.89(18) . . . . ? C4 C5 Mg2 C2 78.85(18) . . . . ? C6 C5 Mg2 C2 -39.01(16) . . . . ? C4 C5 Mg2 C3 37.93(17) . . . . ? C6 C5 Mg2 C3 -79.93(18) . . . . ? C6 C5 Mg2 C4 -117.9(3) . . . . ? C4 C5 Mg2 C6 117.9(3) . . . . ? C4 C5 Mg2 Br1 145.00(15) . . . . ? C6 C5 Mg2 Br1 27.13(18) . . . . ? Mg1 Br1 Mg2 N4 124.86(8) . . . . ? Mg1 Br1 Mg2 N3 -124.85(8) . . . . ? Mg1 Br1 Mg2 C2 14.49(7) . . . . ? Mg1 Br1 Mg2 C3 28.04(9) . . . . ? Mg1 Br1 Mg2 C4 -3.34(13) . . . . ? Mg1 Br1 Mg2 C6 -18.69(7) . . . . ? Mg1 Br1 Mg2 C5 -32.68(9) . . . . ? N4 Mg2 N3 C20 -37.5(3) . . . . ? C2 Mg2 N3 C20 109.8(2) . . . . ? C3 Mg2 N3 C20 65.4(3) . . . . ? C4 Mg2 N3 C20 66.2(2) . . . . ? C6 Mg2 N3 C20 120.7(2) . . . . ? C5 Mg2 N3 C20 95.3(2) . . . . ? Br1 Mg2 N3 C20 -145.7(2) . . . . ? N4 Mg2 N3 C27 150.47(18) . . . . ? C2 Mg2 N3 C27 -62.2(2) . . . . ? C3 Mg2 N3 C27 -106.6(2) . . . . ? C4 Mg2 N3 C27 -105.82(19) . . . . ? C6 Mg2 N3 C27 -51.3(2) . . . . ? C5 Mg2 N3 C27 -76.70(19) . . . . ? Br1 Mg2 N3 C27 42.28(19) . . . . ? N3 Mg2 N4 C26 47.4(3) . . . . ? C2 Mg2 N4 C26 -109.8(2) . . . . ? C3 Mg2 N4 C26 -84.5(2) . . . . ? C4 Mg2 N4 C26 -54.6(2) . . . . ? C6 Mg2 N4 C26 -97.6(3) . . . . ? C5 Mg2 N4 C26 -52.0(3) . . . . ? Br1 Mg2 N4 C26 154.7(2) . . . . ? N3 Mg2 N4 C33 -144.7(2) . . . . ? C2 Mg2 N4 C33 58.1(2) . . . . ? C3 Mg2 N4 C33 83.4(2) . . . . ? C4 Mg2 N4 C33 113.3(2) . . . . ? C6 Mg2 N4 C33 70.3(3) . . . . ? C5 Mg2 N4 C33 115.9(2) . . . . ? Br1 Mg2 N4 C33 -37.4(2) . . . . ? C27 N3 C20 C21 179.6(3) . . . . ? Mg2 N3 C20 C21 7.6(4) . . . . ? N3 C20 C21 C22 -171.9(3) . . . . ? N3 C20 C21 C25 10.3(5) . . . . ? C20 C21 C22 C23 -180.0(3) . . . . ? C25 C21 C22 C23 -1.6(3) . . . . ? C21 C22 C23 C24 1.7(4) . . . . ? C22 C23 C24 C25 -1.2(4) . . . . ? C23 C24 C25 C26 169.5(3) . . . . ? C23 C24 C25 C21 0.2(3) . . . . ? C22 C21 C25 C24 0.8(3) . . . . ? C20 C21 C25 C24 178.8(3) . . . . ? C22 C21 C25 C26 -166.1(3) . . . . ? C20 C21 C25 C26 11.9(6) . . . . ? C33 N4 C26 C25 170.3(3) . . . . ? Mg2 N4 C26 C25 -21.4(4) . . . . ? C24 C25 C26 N4 178.3(3) . . . . ? C21 C25 C26 N4 -16.1(5) . . . . ? C20 N3 C27 C32 78.4(3) . . . . ? Mg2 N3 C27 C32 -109.0(2) . . . . ? C20 N3 C27 C28 -48.0(3) . . . . ? Mg2 N3 C27 C28 124.5(2) . . . . ? N3 C27 C28 C29 -175.2(2) . . . . ? C32 C27 C28 C29 57.6(3) . . . . ? C27 C28 C29 C30 -56.5(3) . . . . ? C28 C29 C30 C31 55.1(4) . . . . ? C29 C30 C31 C32 -54.8(4) . . . . ? N3 C27 C32 C31 174.9(2) . . . . ? C28 C27 C32 C31 -56.6(3) . . . . ? C30 C31 C32 C27 55.3(3) . . . . ? C26 N4 C33 C34 59.6(4) . . . . ? Mg2 N4 C33 C34 -109.0(3) . . . . ? C26 N4 C33 C38 -66.6(3) . . . . ? Mg2 N4 C33 C38 124.9(2) . . . . ? N4 C33 C34 C35 177.4(3) . . . . ? C38 C33 C34 C35 -56.7(3) . . . . ? C33 C34 C35 C36 58.1(4) . . . . ? C34 C35 C36 C37 -57.5(4) . . . . ? C35 C36 C37 C38 54.8(4) . . . . ? N4 C33 C38 C37 -177.3(3) . . . . ? C34 C33 C38 C37 54.7(4) . . . . ? C36 C37 C38 C33 -53.2(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C1 H1 Br1 0.95 2.84 3.686(3) 149.4 4_565 _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 29.03 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 0.674 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.094