Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Chi-Tien Chen' 'Chi-An Huang' 'Bor-Hunn Huang' 'Yi-Ren Tzeng' _publ_contact_author_name 'Dr Chi-Tien Chen' _publ_contact_author_address ; Department of Chemistry National Chung-Hsing University 250 Kuo-Kuang Road Taichung 402 TAIWAN ; _publ_contact_author_phone 886-4-22840412ext416 _publ_contact_author_fax 886-4-22862547 _publ_contact_author_email ctchen@mail.nchu.edu.tw _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_section_title ; Synthesis and Characterisation of Aluminium and Magnesium Complexes Supported by Pendant Oxalic Amidinate Ligands ; data_compound_1 _database_code_CSD 203776 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [C6H5N=C{NH(CH2)2OMe}-C{NH(CH2)2OMe}=NC6H5] _chemical_formula_sum 'C23.50 H26 N4 O2' _chemical_formula_weight 396.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2839(11) _cell_length_b 11.6924(14) _cell_length_c 11.9217(13) _cell_angle_alpha 92.341(3) _cell_angle_beta 112.099(2) _cell_angle_gamma 106.880(2) _cell_volume 1130.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1589 _cell_measurement_theta_min 2.504 _cell_measurement_theta_max 22.747 _exptl_crystal_description parallelpiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.164 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 422 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.238 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6486 _diffrn_reflns_av_R_equivalents 0.0242 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 26.04 _reflns_number_total 4400 _reflns_number_gt 2261 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4400 _refine_ls_number_parameters 265 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1219 _refine_ls_R_factor_gt 0.0663 _refine_ls_wR_factor_ref 0.2073 _refine_ls_wR_factor_gt 0.1748 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O -0.7089(3) 0.0823(2) -0.51513(19) 0.0930(7) Uani 1 1 d . . . O2 O 0.2504(3) 0.1411(2) 0.0777(2) 0.0912(7) Uani 1 1 d . . . N1 N -0.3520(2) 0.12854(19) -0.13982(18) 0.0584(6) Uani 1 1 d . . . N2 N -0.0751(3) 0.20704(19) -0.27697(19) 0.0594(6) Uani 1 1 d . . . N3 N -0.4249(3) 0.0296(2) -0.33218(19) 0.0659(6) Uani 1 1 d . . . H3A H -0.3953 0.0144 -0.3898 0.079 Uiso 1 1 calc R . . N4 N -0.0543(3) 0.0648(2) -0.1521(2) 0.0668(6) Uani 1 1 d . . . H4A H -0.1005 0.0138 -0.1157 0.080 Uiso 1 1 calc R . . C1 C -0.3100(3) 0.0994(2) -0.2254(2) 0.0533(6) Uani 1 1 d . . . C2 C -0.1389(3) 0.1310(2) -0.2203(2) 0.0542(6) Uani 1 1 d . . . C3 C -0.2363(3) 0.2012(2) -0.0253(2) 0.0527(6) Uani 1 1 d . . . C4 C -0.0961(3) 0.2977(2) -0.0059(3) 0.0641(7) Uani 1 1 d . . . H4B H -0.0696 0.3179 -0.0720 0.077 Uiso 1 1 calc R . . C5 C 0.0042(4) 0.3637(3) 0.1091(3) 0.0741(8) Uani 1 1 d . . . H5A H 0.0979 0.4279 0.1197 0.089 Uiso 1 1 calc R . . C6 C -0.0308(4) 0.3370(3) 0.2083(3) 0.0770(9) Uani 1 1 d . . . H6A H 0.0385 0.3817 0.2862 0.092 Uiso 1 1 calc R . . C7 C -0.1697(4) 0.2430(3) 0.1910(3) 0.0752(8) Uani 1 1 d . . . H7A H -0.1950 0.2240 0.2578 0.090 Uiso 1 1 calc R . . C8 C -0.2733(3) 0.1758(2) 0.0750(2) 0.0616(7) Uani 1 1 d . . . H8A H -0.3683 0.1132 0.0647 0.074 Uiso 1 1 calc R . . C9 C -0.1576(3) 0.2790(2) -0.3499(2) 0.0563(7) Uani 1 1 d . . . C10 C -0.1156(4) 0.3131(3) -0.4471(3) 0.0706(8) Uani 1 1 d . . . H10A H -0.0373 0.2868 -0.4607 0.085 Uiso 1 1 calc R . . C11 C -0.1866(5) 0.3847(3) -0.5234(3) 0.0849(10) Uani 1 1 d . . . H11A H -0.1574 0.4046 -0.5884 0.102 Uiso 1 1 calc R . . C12 C -0.3000(5) 0.4267(3) -0.5042(3) 0.0896(10) Uani 1 1 d . . . H12A H -0.3493 0.4742 -0.5562 0.107 Uiso 1 1 calc R . . C13 C -0.3392(4) 0.3975(3) -0.4076(3) 0.0880(10) Uani 1 1 d . . . H13A H -0.4148 0.4267 -0.3932 0.106 Uiso 1 1 calc R . . C14 C -0.2694(4) 0.3259(3) -0.3307(3) 0.0718(8) Uani 1 1 d . . . H14A H -0.2975 0.3085 -0.2647 0.086 Uiso 1 1 calc R . . C15 C -0.5961(4) -0.0208(3) -0.3530(3) 0.0863(10) Uani 1 1 d . . . H15A H -0.6030 -0.0435 -0.2773 0.104 Uiso 1 1 calc R . . H15B H -0.6470 -0.0938 -0.4141 0.104 Uiso 1 1 calc R . . C16 C -0.6906(4) 0.0643(4) -0.3951(3) 0.0959(12) Uani 1 1 d . . . H16A H -0.7983 0.0314 -0.3935 0.115 Uiso 1 1 calc R . . H16B H -0.6331 0.1414 -0.3398 0.115 Uiso 1 1 calc R . . C17 C -0.7968(5) 0.1621(4) -0.5618(4) 0.1290(15) Uani 1 1 d . . . H17A H -0.8056 0.1691 -0.6439 0.194 Uiso 1 1 calc R . . H17B H -0.7397 0.2404 -0.5106 0.194 Uiso 1 1 calc R . . H17C H -0.9050 0.1309 -0.5627 0.194 Uiso 1 1 calc R . . C18 C 0.1111(4) 0.0754(3) -0.1371(3) 0.0850(10) Uani 1 1 d . . . H18A H 0.1217 0.0910 -0.2134 0.102 Uiso 1 1 calc R . . H18B H 0.1281 -0.0016 -0.1219 0.102 Uiso 1 1 calc R . . C19 C 0.2420(4) 0.1720(3) -0.0363(3) 0.0849(10) Uani 1 1 d . . . H19A H 0.3471 0.1834 -0.0410 0.102 Uiso 1 1 calc R . . H19B H 0.2189 0.2477 -0.0448 0.102 Uiso 1 1 calc R . . C20 C 0.3712(4) 0.2323(4) 0.1775(4) 0.1093(12) Uani 1 1 d . . . H20A H 0.3730 0.2067 0.2534 0.164 Uiso 1 1 calc R . . H20B H 0.3453 0.3062 0.1711 0.164 Uiso 1 1 calc R . . H20C H 0.4774 0.2459 0.1757 0.164 Uiso 1 1 calc R . . C31 C 0.5326(9) 0.5233(7) 0.0539(6) 0.093(2) Uiso 0.50 1 d P . . C32 C 0.3877(5) 0.5324(3) -0.0087(5) 0.1042(13) Uani 1 1 d . . . C33 C 0.2956(10) 0.4750(8) -0.1400(9) 0.109(2) Uiso 0.50 1 d P . . C34 C 0.3719(8) 0.4197(4) -0.1900(4) 0.150(2) Uani 1 1 d . . . C35 C 0.5163(12) 0.4113(8) -0.1242(9) 0.109(3) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0981(16) 0.1137(18) 0.0704(14) 0.0006(13) 0.0323(12) 0.0442(15) O2 0.0945(15) 0.0741(14) 0.0909(15) 0.0378(13) 0.0284(13) 0.0168(13) N1 0.0569(12) 0.0574(13) 0.0528(13) 0.0081(10) 0.0195(11) 0.0110(11) N2 0.0653(13) 0.0554(13) 0.0618(13) 0.0147(11) 0.0291(11) 0.0207(11) N3 0.0678(14) 0.0628(14) 0.0554(13) 0.0038(11) 0.0255(11) 0.0054(12) N4 0.0766(15) 0.0591(13) 0.0700(15) 0.0218(12) 0.0302(12) 0.0280(12) C1 0.0620(15) 0.0456(13) 0.0477(14) 0.0106(12) 0.0208(13) 0.0130(12) C2 0.0653(16) 0.0432(13) 0.0530(15) 0.0071(12) 0.0254(13) 0.0148(13) C3 0.0564(14) 0.0508(14) 0.0540(14) 0.0087(12) 0.0232(12) 0.0211(13) C4 0.0683(17) 0.0592(16) 0.0608(16) 0.0046(14) 0.0309(14) 0.0098(14) C5 0.0687(18) 0.0619(18) 0.082(2) -0.0046(16) 0.0330(16) 0.0065(15) C6 0.079(2) 0.072(2) 0.0620(18) -0.0048(16) 0.0171(16) 0.0173(17) C7 0.093(2) 0.077(2) 0.0601(18) 0.0104(16) 0.0369(17) 0.0271(19) C8 0.0684(17) 0.0586(16) 0.0605(16) 0.0108(13) 0.0304(14) 0.0193(14) C9 0.0601(15) 0.0469(14) 0.0543(15) 0.0066(12) 0.0214(13) 0.0095(13) C10 0.0832(19) 0.0661(17) 0.0632(17) 0.0126(15) 0.0362(15) 0.0165(16) C11 0.119(3) 0.073(2) 0.0590(18) 0.0209(16) 0.0373(19) 0.024(2) C12 0.107(3) 0.076(2) 0.076(2) 0.0257(18) 0.021(2) 0.034(2) C13 0.088(2) 0.085(2) 0.102(2) 0.035(2) 0.038(2) 0.0423(19) C14 0.0805(19) 0.0680(18) 0.0798(19) 0.0283(16) 0.0417(16) 0.0285(16) C15 0.075(2) 0.086(2) 0.068(2) 0.0052(17) 0.0265(16) -0.0107(19) C16 0.0655(19) 0.131(3) 0.077(2) -0.015(2) 0.0337(17) 0.011(2) C17 0.117(3) 0.142(4) 0.132(4) 0.011(3) 0.036(3) 0.069(3) C18 0.093(2) 0.093(2) 0.097(2) 0.037(2) 0.047(2) 0.058(2) C19 0.0724(19) 0.088(2) 0.103(2) 0.049(2) 0.0377(19) 0.0309(19) C20 0.097(3) 0.090(3) 0.115(3) 0.023(2) 0.026(2) 0.016(2) C32 0.119(3) 0.074(2) 0.169(4) 0.058(3) 0.098(3) 0.047(2) C34 0.207(6) 0.105(3) 0.088(3) 0.017(3) 0.058(4) -0.018(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C16 1.408(4) . ? O1 C17 1.410(4) . ? O2 C19 1.400(4) . ? O2 C20 1.417(4) . ? N1 C1 1.288(3) . ? N1 C3 1.418(3) . ? N2 C2 1.281(3) . ? N2 C9 1.409(3) . ? N3 C1 1.346(3) . ? N3 C15 1.443(4) . ? N4 C2 1.343(3) . ? N4 C18 1.445(4) . ? C1 C2 1.499(4) . ? C3 C8 1.384(3) . ? C3 C4 1.386(4) . ? C4 C5 1.370(4) . ? C5 C6 1.366(4) . ? C6 C7 1.367(4) . ? C7 C8 1.388(4) . ? C9 C14 1.388(4) . ? C9 C10 1.393(4) . ? C10 C11 1.376(4) . ? C11 C12 1.368(5) . ? C12 C13 1.361(5) . ? C13 C14 1.376(4) . ? C15 C16 1.492(5) . ? C18 C19 1.480(4) . ? C31 C31 1.216(13) 2_665 ? C31 C32 1.308(8) . ? C31 C32 1.346(8) 2_665 ? C31 C35 1.389(11) 2_665 ? C31 C34 1.533(7) 2_665 ? C31 C33 1.532(11) 2_665 ? C32 C31 1.346(8) 2_665 ? C32 C33 1.485(10) . ? C32 C35 1.500(10) 2_665 ? C33 C34 1.351(9) . ? C33 C31 1.532(11) 2_665 ? C34 C35 1.310(9) . ? C34 C31 1.533(7) 2_665 ? C35 C31 1.389(11) 2_665 ? C35 C32 1.500(10) 2_665 ? 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 C16 O1 C17 114.1(3) . . ? C19 O2 C20 112.6(3) . . ? C1 N1 C3 122.7(2) . . ? C2 N2 C9 123.2(2) . . ? C1 N3 C15 122.1(2) . . ? C2 N4 C18 122.8(2) . . ? N1 C1 N3 120.2(2) . . ? N1 C1 C2 127.1(2) . . ? N3 C1 C2 112.6(2) . . ? N2 C2 N4 120.6(2) . . ? N2 C2 C1 126.9(2) . . ? N4 C2 C1 112.5(2) . . ? C8 C3 C4 117.6(2) . . ? C8 C3 N1 115.9(2) . . ? C4 C3 N1 126.4(2) . . ? C5 C4 C3 121.1(3) . . ? C6 C5 C4 121.2(3) . . ? C5 C6 C7 118.7(3) . . ? C6 C7 C8 120.9(3) . . ? C3 C8 C7 120.5(3) . . ? C14 C9 C10 116.3(3) . . ? C14 C9 N2 126.7(2) . . ? C10 C9 N2 116.8(2) . . ? C11 C10 C9 121.8(3) . . ? C12 C11 C10 120.5(3) . . ? C13 C12 C11 118.7(3) . . ? C12 C13 C14 121.5(3) . . ? C13 C14 C9 121.1(3) . . ? N3 C15 C16 113.5(3) . . ? O1 C16 C15 110.6(3) . . ? N4 C18 C19 114.3(3) . . ? O2 C19 C18 110.4(3) . . ? C31 C31 C32 64.3(7) 2_665 . ? C31 C31 C32 61.2(7) 2_665 2_665 ? C32 C31 C32 125.5(5) . 2_665 ? C31 C31 C35 131.8(11) 2_665 2_665 ? C32 C31 C35 67.5(6) . 2_665 ? C32 C31 C35 167.0(8) 2_665 2_665 ? C31 C31 C34 175.2(11) 2_665 2_665 ? C32 C31 C34 120.5(7) . 2_665 ? C32 C31 C34 114.1(7) 2_665 2_665 ? C35 C31 C34 53.0(5) 2_665 2_665 ? C31 C31 C33 122.9(10) 2_665 2_665 ? C32 C31 C33 172.6(7) . 2_665 ? C32 C31 C33 61.8(5) 2_665 2_665 ? C35 C31 C33 105.3(7) 2_665 2_665 ? C34 C31 C33 52.3(4) 2_665 2_665 ? C31 C32 C31 54.5(5) . 2_665 ? C31 C32 C33 119.8(6) . . ? C31 C32 C33 65.3(5) 2_665 . ? C31 C32 C35 58.8(5) . 2_665 ? C31 C32 C35 113.3(6) 2_665 2_665 ? C33 C32 C35 178.6(6) . 2_665 ? C34 C33 C32 116.8(7) . . ? C34 C33 C31 63.9(5) . 2_665 ? C32 C33 C31 53.0(4) . 2_665 ? C35 C34 C33 121.6(7) . . ? C35 C34 C31 57.9(5) . 2_665 ? C33 C34 C31 63.8(5) . 2_665 ? C34 C35 C31 69.2(6) . 2_665 ? C34 C35 C32 122.8(7) . 2_665 ? C31 C35 C32 53.7(5) 2_665 2_665 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.332 _refine_diff_density_min -0.197 _refine_diff_density_rms 0.051 #==END data_compound_2 _database_code_CSD 203777 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [C6H5N=C{NH(CH2)2NMe2}-C{NH(CH2)2NMe2}=NC6H5] _chemical_formula_sum 'C44 H64 N12' _chemical_formula_weight 761.07 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) 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' _cell_length_a 9.5940(6) _cell_length_b 17.2591(11) _cell_length_c 27.7148(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4589.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7348 _cell_measurement_theta_min 2.470 _cell_measurement_theta_max 22.381 _exptl_crystal_description parallelpiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.72 _exptl_crystal_size_min 0.61 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.102 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.527 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25891 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 26.03 _reflns_number_total 9046 _reflns_number_gt 5606 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -1(3) _refine_ls_number_reflns 9046 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1078 _refine_ls_R_factor_gt 0.0688 _refine_ls_wR_factor_ref 0.2078 _refine_ls_wR_factor_gt 0.1885 _refine_ls_goodness_of_fit_ref 1.254 _refine_ls_restrained_S_all 1.254 _refine_ls_shift/su_max 0.832 _refine_ls_shift/su_mean 0.078 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 N1 N 0.0034(3) 0.33016(15) 0.12215(10) 0.0588(7) Uani 1 1 d . . . N2 N 0.1557(3) 0.41785(15) 0.08929(10) 0.0593(7) Uani 1 1 d . . . H2A H 0.2403 0.4328 0.0849 0.071 Uiso 1 1 calc R . . N3 N 0.0193(4) 0.5629(3) 0.12718(16) 0.1043(12) Uani 1 1 d . . . N4 N 0.2788(3) 0.31171(17) 0.18635(10) 0.0591(7) Uani 1 1 d . . . N5 N 0.3567(3) 0.30066(18) 0.10914(10) 0.0662(7) Uani 1 1 d . . . H5A H 0.3384 0.3047 0.0789 0.079 Uiso 1 1 calc R . . N6 N 0.5748(3) 0.29646(19) 0.04080(11) 0.0715(8) Uani 1 1 d . . . C1 C 0.1295(3) 0.35591(18) 0.11776(11) 0.0521(7) Uani 1 1 d . . . C2 C -0.0317(3) 0.26449(19) 0.14913(11) 0.0553(8) Uani 1 1 d . . . C3 C 0.0304(4) 0.1924(2) 0.14411(13) 0.0684(9) Uani 1 1 d . . . H3A H 0.1057 0.1862 0.1233 0.082 Uiso 1 1 calc R . . C4 C -0.0194(5) 0.1301(2) 0.16991(16) 0.0847(12) Uani 1 1 d . . . H4B H 0.0233 0.0821 0.1662 0.102 Uiso 1 1 calc R . . C5 C -0.1301(5) 0.1369(3) 0.20079(16) 0.0884(12) Uani 1 1 d . . . H5B H -0.1624 0.0942 0.2179 0.106 Uiso 1 1 calc R . . C6 C -0.1921(4) 0.2076(3) 0.20590(17) 0.0871(12) Uani 1 1 d . . . H6A H -0.2668 0.2132 0.2270 0.104 Uiso 1 1 calc R . . C7 C -0.1452(3) 0.2712(2) 0.18004(14) 0.0679(9) Uani 1 1 d . . . H7A H -0.1899 0.3187 0.1834 0.081 Uiso 1 1 calc R . . C8 C 0.0429(4) 0.4595(2) 0.06601(15) 0.0740(10) Uani 1 1 d . . . H8A H -0.0132 0.4226 0.0481 0.089 Uiso 1 1 calc R . . H8B H 0.0826 0.4955 0.0430 0.089 Uiso 1 1 calc R . . C9 C -0.0532(5) 0.5048(3) 0.10047(19) 0.0905(13) Uani 1 1 d . . . H9A H -0.1269 0.5291 0.0819 0.109 Uiso 1 1 calc R . . H9B H -0.0964 0.4688 0.1228 0.109 Uiso 1 1 calc R . . C10 C 0.0381(9) 0.6330(4) 0.0934(3) 0.171(3) Uani 1 1 d . . . H10A H 0.0852 0.6738 0.1104 0.257 Uiso 1 1 calc R . . H10B H -0.0516 0.6510 0.0829 0.257 Uiso 1 1 calc R . . H10C H 0.0924 0.6179 0.0659 0.257 Uiso 1 1 calc R . . C11 C -0.0589(10) 0.5924(4) 0.1667(2) 0.162(3) Uani 1 1 d . . . H11A H -0.0739 0.5519 0.1899 0.243 Uiso 1 1 calc R . . H11B H -0.1472 0.6112 0.1554 0.243 Uiso 1 1 calc R . . H11C H -0.0084 0.6341 0.1816 0.243 Uiso 1 1 calc R . . C12 C 0.2585(3) 0.32269(18) 0.14110(12) 0.0540(8) Uani 1 1 d . . . C13 C 0.1800(3) 0.3378(2) 0.22144(11) 0.0586(8) Uani 1 1 d . . . C14 C 0.1462(4) 0.2871(2) 0.25841(13) 0.0714(10) Uani 1 1 d . . . H14A H 0.1826 0.2372 0.2585 0.086 Uiso 1 1 calc R . . C15 C 0.0591(4) 0.3105(3) 0.29487(14) 0.0856(12) Uani 1 1 d . . . H15A H 0.0351 0.2757 0.3191 0.103 Uiso 1 1 calc R . . C16 C 0.0062(5) 0.3851(3) 0.29607(16) 0.0945(14) Uani 1 1 d . . . H16A H -0.0507 0.4014 0.3213 0.113 Uiso 1 1 calc R . . C17 C 0.0403(5) 0.4348(2) 0.25885(15) 0.0837(12) Uani 1 1 d . . . H17A H 0.0036 0.4847 0.2586 0.100 Uiso 1 1 calc R . . C18 C 0.1266(4) 0.4122(2) 0.22240(14) 0.0682(9) Uani 1 1 d . . . H18A H 0.1496 0.4469 0.1980 0.082 Uiso 1 1 calc R . . C19 C 0.4927(4) 0.2703(3) 0.12342(15) 0.0826(11) Uani 1 1 d . . . H19A H 0.4802 0.2288 0.1466 0.099 Uiso 1 1 calc R . . H19B H 0.5465 0.3110 0.1388 0.099 Uiso 1 1 calc R . . C20 C 0.5693(5) 0.2407(3) 0.08089(18) 0.0924(13) Uani 1 1 d . . . H20A H 0.6637 0.2278 0.0905 0.111 Uiso 1 1 calc R . . H20B H 0.5248 0.1935 0.0697 0.111 Uiso 1 1 calc R . . C21 C 0.6663(5) 0.3600(3) 0.0525(2) 0.1210(18) Uani 1 1 d . . . H21A H 0.6681 0.3960 0.0261 0.182 Uiso 1 1 calc R . . H21B H 0.7586 0.3406 0.0581 0.182 Uiso 1 1 calc R . . H21C H 0.6331 0.3857 0.0809 0.182 Uiso 1 1 calc R . . C22 C 0.6223(7) 0.2594(5) -0.0025(2) 0.152(3) Uani 1 1 d . . . H22A H 0.6257 0.2966 -0.0282 0.228 Uiso 1 1 calc R . . H22B H 0.5592 0.2184 -0.0110 0.228 Uiso 1 1 calc R . . H22C H 0.7137 0.2383 0.0027 0.228 Uiso 1 1 calc R . . N7 N 0.4058(3) 0.52185(16) 0.06380(10) 0.0622(7) Uani 1 1 d . . . N8 N 0.5253(3) 0.55583(16) 0.13164(10) 0.0663(8) Uani 1 1 d . . . H8C H 0.6005 0.5758 0.1431 0.080 Uiso 1 1 calc R . . N9 N 0.5826(4) 0.5573(2) 0.23028(12) 0.0784(9) Uani 1 1 d . . . N10 N 0.6057(3) 0.69411(16) 0.07222(10) 0.0609(7) Uani 1 1 d . . . N11 N 0.6652(3) 0.59379(17) 0.02244(10) 0.0655(7) Uani 1 1 d . . . H11D H 0.6632 0.5445 0.0181 0.079 Uiso 1 1 calc R . . N12 N 0.7833(3) 0.5190(2) -0.05587(11) 0.0771(9) Uani 1 1 d . . . C31 C 0.4986(3) 0.56393(17) 0.08436(12) 0.0564(8) Uani 1 1 d . . . C32 C 0.3688(3) 0.5317(2) 0.01476(13) 0.0664(9) Uani 1 1 d . . . C33 C 0.3626(4) 0.4651(2) -0.01360(14) 0.0768(10) Uani 1 1 d . . . H33A H 0.3861 0.4169 -0.0010 0.092 Uiso 1 1 calc R . . C34 C 0.3190(5) 0.4734(4) -0.06233(19) 0.0999(14) Uani 1 1 d . . . H34A H 0.3166 0.4300 -0.0822 0.120 Uiso 1 1 calc R . . C35 C 0.2808(5) 0.5435(5) -0.08055(19) 0.1130(18) Uani 1 1 d . . . H35A H 0.2489 0.5473 -0.1121 0.136 Uiso 1 1 calc R . . C36 C 0.2894(6) 0.6066(4) -0.05295(19) 0.1097(16) Uani 1 1 d . . . H36A H 0.2666 0.6545 -0.0662 0.132 Uiso 1 1 calc R . . C37 C 0.3315(4) 0.6028(3) -0.00464(15) 0.0857(12) Uani 1 1 d . . . H37A H 0.3345 0.6474 0.0142 0.103 Uiso 1 1 calc R . . C38 C 0.4324(6) 0.5148(3) 0.16421(13) 0.0947(15) Uani 1 1 d . . . H38A H 0.4629 0.4616 0.1680 0.114 Uiso 1 1 calc R . . H38B H 0.3383 0.5145 0.1513 0.114 Uiso 1 1 calc R . . C39 C 0.4356(8) 0.5582(5) 0.2149(3) 0.157(3) Uani 1 1 d . . . H39A H 0.4024 0.6110 0.2116 0.188 Uiso 1 1 calc R . . H39B H 0.3774 0.5315 0.2382 0.188 Uiso 1 1 calc R . . C40 C 0.6108(16) 0.4874(6) 0.2366(5) 0.401(14) Uani 1 1 d . . . H40A H 0.6067 0.4607 0.2063 0.601 Uiso 1 1 calc R . . H40B H 0.5445 0.4651 0.2585 0.601 Uiso 1 1 calc R . . H40C H 0.7028 0.4829 0.2499 0.601 Uiso 1 1 calc R . . C41 C 0.5903(18) 0.6043(7) 0.2686(3) 0.317(9) Uani 1 1 d . . . H41A H 0.6844 0.6054 0.2803 0.476 Uiso 1 1 calc R . . H41B H 0.5295 0.5857 0.2935 0.476 Uiso 1 1 calc R . . H41C H 0.5625 0.6557 0.2593 0.476 Uiso 1 1 calc R . . C42 C 0.5917(3) 0.62307(19) 0.05971(12) 0.0569(8) Uani 1 1 d . . . C43 C 0.5284(4) 0.72758(18) 0.11033(13) 0.0628(9) Uani 1 1 d . . . C44 C 0.5990(4) 0.7697(2) 0.14448(14) 0.0753(10) Uani 1 1 d . . . H44A H 0.6955 0.7739 0.1423 0.090 Uiso 1 1 calc R . . C45 C 0.5315(5) 0.8057(3) 0.18153(17) 0.0924(12) Uani 1 1 d . . . H45A H 0.5821 0.8322 0.2049 0.111 Uiso 1 1 calc R . . C46 C 0.3874(5) 0.8028(3) 0.18425(18) 0.0928(13) Uani 1 1 d . . . H46A H 0.3398 0.8271 0.2092 0.111 Uiso 1 1 calc R . . C47 C 0.3178(5) 0.7636(3) 0.1497(2) 0.1051(16) Uani 1 1 d . . . H47A H 0.2209 0.7619 0.1509 0.126 Uiso 1 1 calc R . . C48 C 0.3852(4) 0.7262(2) 0.11287(18) 0.0892(13) Uani 1 1 d . . . H48A H 0.3341 0.6999 0.0895 0.107 Uiso 1 1 calc R . . C49 C 0.7470(5) 0.6399(2) -0.01069(15) 0.0820(11) Uani 1 1 d . . . H49A H 0.7978 0.6794 0.0069 0.098 Uiso 1 1 calc R . . H49B H 0.6862 0.6653 -0.0338 0.098 Uiso 1 1 calc R . . C50 C 0.8530(6) 0.5848(3) -0.03809(18) 0.1071(15) Uani 1 1 d . . . H50A H 0.8955 0.6127 -0.0646 0.128 Uiso 1 1 calc R . . H50B H 0.9264 0.5688 -0.0162 0.128 Uiso 1 1 calc R . . C51 C 0.6921(7) 0.5338(5) -0.0951(2) 0.158(3) Uani 1 1 d . . . H51A H 0.6249 0.5723 -0.0858 0.237 Uiso 1 1 calc R . . H51B H 0.6447 0.4869 -0.1038 0.237 Uiso 1 1 calc R . . H51C H 0.7448 0.5524 -0.1221 0.237 Uiso 1 1 calc R . . C52 C 0.8846(8) 0.4607(5) -0.0723(3) 0.163(3) Uani 1 1 d . . . H52A H 0.9476 0.4487 -0.0464 0.245 Uiso 1 1 calc R . . H52B H 0.9361 0.4808 -0.0992 0.245 Uiso 1 1 calc R . . H52C H 0.8361 0.4146 -0.0819 0.245 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 N1 0.0520(15) 0.0650(15) 0.0593(16) 0.0053(13) -0.0034(14) -0.0042(12) N2 0.0501(14) 0.0630(16) 0.0649(16) 0.0133(14) -0.0058(13) -0.0034(12) N3 0.074(2) 0.123(3) 0.116(3) -0.029(3) -0.006(2) 0.010(2) N4 0.0485(14) 0.0800(18) 0.0487(15) 0.0047(14) 0.0035(13) 0.0053(13) N5 0.0547(15) 0.094(2) 0.0502(15) 0.0048(14) 0.0032(13) 0.0152(15) N6 0.0635(17) 0.089(2) 0.0622(18) -0.0054(16) 0.0081(15) -0.0033(16) C1 0.0489(17) 0.0619(18) 0.0455(16) 0.0003(14) -0.0034(15) -0.0039(14) C2 0.0468(17) 0.0647(18) 0.0543(18) 0.0030(15) -0.0057(15) -0.0068(15) C3 0.071(2) 0.066(2) 0.068(2) 0.0007(17) 0.0143(19) -0.0005(18) C4 0.101(3) 0.062(2) 0.091(3) 0.002(2) 0.020(3) 0.005(2) C5 0.092(3) 0.076(3) 0.097(3) 0.013(2) 0.024(3) -0.007(2) C6 0.070(2) 0.099(3) 0.092(3) 0.009(2) 0.023(2) -0.010(2) C7 0.0536(19) 0.072(2) 0.078(2) 0.0001(19) 0.0058(19) -0.0039(17) C8 0.067(2) 0.075(2) 0.080(2) 0.0138(19) -0.018(2) 0.0003(18) C9 0.073(2) 0.087(3) 0.111(3) 0.016(3) 0.003(3) 0.007(2) C10 0.167(6) 0.137(5) 0.209(7) -0.043(6) 0.054(6) -0.069(5) C11 0.220(7) 0.136(5) 0.131(5) -0.011(4) 0.018(6) 0.055(6) C12 0.0475(17) 0.0597(18) 0.0547(19) 0.0008(15) 0.0041(15) -0.0001(14) C13 0.0494(17) 0.084(2) 0.0430(17) -0.0025(16) -0.0029(14) -0.0064(16) C14 0.067(2) 0.091(3) 0.056(2) 0.0092(19) 0.0031(19) 0.0098(19) C15 0.080(2) 0.117(4) 0.060(2) 0.014(2) 0.017(2) -0.005(3) C16 0.087(3) 0.126(4) 0.070(3) -0.022(3) 0.020(2) -0.006(3) C17 0.093(3) 0.082(3) 0.076(3) -0.020(2) 0.009(2) -0.004(2) C18 0.068(2) 0.069(2) 0.068(2) -0.0066(18) 0.0058(19) -0.0062(18) C19 0.059(2) 0.118(3) 0.071(2) 0.016(2) 0.009(2) 0.027(2) C20 0.075(3) 0.092(3) 0.110(4) -0.001(3) 0.009(3) 0.015(2) C21 0.091(3) 0.114(3) 0.158(5) -0.008(4) 0.007(3) -0.022(3) C22 0.151(5) 0.221(7) 0.084(3) -0.033(4) 0.035(4) 0.030(5) N7 0.0654(17) 0.0652(16) 0.0560(16) 0.0007(14) -0.0007(15) -0.0056(14) N8 0.0755(18) 0.0731(17) 0.0504(16) 0.0029(13) 0.0014(14) -0.0250(15) N9 0.078(2) 0.089(2) 0.068(2) 0.0148(18) -0.0045(17) 0.0032(17) N10 0.0627(16) 0.0566(15) 0.0633(17) 0.0046(14) 0.0039(14) -0.0082(13) N11 0.0751(18) 0.0639(16) 0.0575(16) 0.0051(14) 0.0132(15) -0.0018(14) N12 0.076(2) 0.097(2) 0.0581(18) -0.0110(17) -0.0008(17) -0.0002(18) C31 0.0600(19) 0.0503(16) 0.0587(19) 0.0050(14) 0.0049(16) -0.0052(15) C32 0.0519(18) 0.086(2) 0.061(2) 0.0106(19) -0.0045(17) -0.0143(18) C33 0.083(2) 0.083(2) 0.064(2) -0.008(2) 0.007(2) -0.019(2) C34 0.088(3) 0.130(4) 0.082(3) -0.020(3) -0.006(3) -0.026(3) C35 0.086(3) 0.178(6) 0.075(3) 0.026(4) -0.023(3) -0.019(4) C36 0.112(4) 0.135(4) 0.082(3) 0.035(3) -0.035(3) -0.004(3) C37 0.087(3) 0.092(3) 0.078(3) 0.018(2) -0.009(2) 0.004(2) C38 0.131(4) 0.105(3) 0.048(2) 0.010(2) -0.004(2) -0.054(3) C39 0.121(5) 0.200(7) 0.148(6) 0.061(5) 0.041(5) -0.007(5) C40 0.52(2) 0.182(9) 0.50(2) 0.170(13) 0.39(2) 0.128(13) C41 0.54(2) 0.295(12) 0.112(5) -0.042(7) 0.125(10) -0.234(15) C42 0.0524(17) 0.062(2) 0.0562(18) 0.0087(16) -0.0010(16) -0.0031(15) C43 0.064(2) 0.0515(17) 0.073(2) 0.0062(17) 0.0054(19) -0.0055(16) C44 0.065(2) 0.089(2) 0.072(2) -0.012(2) -0.003(2) -0.005(2) C45 0.090(3) 0.104(3) 0.083(3) -0.019(3) -0.013(3) 0.006(3) C46 0.103(3) 0.076(3) 0.099(3) -0.016(2) 0.016(3) 0.008(3) C47 0.074(3) 0.092(3) 0.150(5) -0.037(3) 0.018(3) -0.001(2) C48 0.074(3) 0.081(2) 0.113(3) -0.028(3) 0.006(3) -0.006(2) C49 0.091(3) 0.086(3) 0.069(2) 0.012(2) 0.021(2) -0.010(2) C50 0.099(3) 0.144(4) 0.078(3) 0.021(3) 0.006(3) -0.002(3) C51 0.110(4) 0.254(9) 0.109(4) 0.006(5) -0.030(4) 0.008(5) C52 0.158(6) 0.200(7) 0.132(5) -0.013(5) 0.011(5) 0.072(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.294(4) . ? N1 C2 1.399(4) . ? N2 C1 1.352(4) . ? N2 C8 1.450(4) . ? N3 C9 1.428(6) . ? N3 C11 1.423(8) . ? N3 C10 1.540(9) . ? N4 C12 1.283(4) . ? N4 C13 1.431(4) . ? N5 C12 1.348(4) . ? N5 C19 1.461(4) . ? N6 C21 1.441(6) . ? N6 C22 1.434(6) . ? N6 C20 1.470(5) . ? C1 C12 1.509(4) . ? C2 C7 1.390(5) . ? C2 C3 1.386(5) . ? C3 C4 1.378(5) . ? C4 C5 1.369(6) . ? C5 C6 1.365(6) . ? C6 C7 1.386(6) . ? C8 C9 1.541(6) . ? C13 C14 1.386(5) . ? C13 C18 1.382(5) . ? C14 C15 1.372(5) . ? C15 C16 1.385(7) . ? C16 C17 1.381(6) . ? C17 C18 1.363(5) . ? C19 C20 1.480(6) . ? N7 C31 1.283(4) . ? N7 C32 1.415(5) . ? N8 C31 1.342(4) . ? N8 C38 1.453(5) . ? N9 C40 1.247(9) . ? N9 C41 1.338(9) . ? N9 C39 1.473(8) . ? N10 C42 1.281(4) . ? N10 C43 1.414(4) . ? N11 C42 1.349(4) . ? N11 C49 1.446(4) . ? N12 C50 1.407(6) . ? N12 C51 1.418(6) . ? N12 C52 1.470(7) . ? C31 C42 1.518(4) . ? C32 C37 1.387(6) . ? C32 C33 1.394(5) . ? C33 C34 1.421(7) . ? C34 C35 1.361(8) . ? C35 C36 1.334(8) . ? C36 C37 1.400(7) . ? C38 C39 1.592(9) . ? C43 C44 1.373(5) . ? C43 C48 1.376(5) . ? C44 C45 1.364(6) . ? C45 C46 1.386(6) . ? C46 C47 1.350(7) . ? C47 C48 1.369(6) . ? C49 C50 1.586(7) . ? 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 C1 N1 C2 123.6(3) . . ? C1 N2 C8 120.8(3) . . ? C9 N3 C11 113.2(5) . . ? C9 N3 C10 107.1(4) . . ? C11 N3 C10 104.4(5) . . ? C12 N4 C13 121.1(3) . . ? C12 N5 C19 123.2(3) . . ? C21 N6 C22 109.5(5) . . ? C21 N6 C20 110.5(4) . . ? C22 N6 C20 110.6(4) . . ? N1 C1 N2 120.0(3) . . ? N1 C1 C12 126.5(3) . . ? N2 C1 C12 113.4(2) . . ? C7 C2 C3 118.2(3) . . ? C7 C2 N1 116.8(3) . . ? C3 C2 N1 124.7(3) . . ? C4 C3 C2 120.0(3) . . ? C5 C4 C3 121.8(4) . . ? C4 C5 C6 118.7(4) . . ? C5 C6 C7 120.8(4) . . ? C6 C7 C2 120.5(4) . . ? N2 C8 C9 115.0(3) . . ? N3 C9 C8 112.7(4) . . ? N4 C12 N5 119.6(3) . . ? N4 C12 C1 126.8(3) . . ? N5 C12 C1 113.5(3) . . ? C14 C13 C18 119.0(3) . . ? C14 C13 N4 117.3(3) . . ? C18 C13 N4 123.4(3) . . ? C15 C14 C13 120.1(4) . . ? C14 C15 C16 120.9(4) . . ? C17 C16 C15 118.2(4) . . ? C18 C17 C16 121.3(4) . . ? C17 C18 C13 120.4(4) . . ? N5 C19 C20 110.6(3) . . ? N6 C20 C19 113.2(3) . . ? C31 N7 C32 122.1(3) . . ? C31 N8 C38 122.7(3) . . ? C40 N9 C41 117.6(10) . . ? C40 N9 C39 105.0(9) . . ? C41 N9 C39 106.0(9) . . ? C42 N10 C43 122.5(3) . . ? C42 N11 C49 124.3(3) . . ? C50 N12 C51 114.5(5) . . ? C50 N12 C52 110.3(5) . . ? C51 N12 C52 107.1(5) . . ? N7 C31 N8 120.5(3) . . ? N7 C31 C42 126.1(3) . . ? N8 C31 C42 113.4(3) . . ? C37 C32 C33 120.0(4) . . ? C37 C32 N7 122.9(4) . . ? C33 C32 N7 116.9(3) . . ? C32 C33 C34 117.7(4) . . ? C35 C34 C33 121.4(5) . . ? C36 C35 C34 119.8(5) . . ? C35 C36 C37 121.9(5) . . ? C32 C37 C36 119.1(5) . . ? N8 C38 C39 107.9(4) . . ? N9 C39 C38 105.6(5) . . ? N10 C42 N11 120.7(3) . . ? N10 C42 C31 125.7(3) . . ? N11 C42 C31 113.6(3) . . ? C44 C43 C48 117.8(4) . . ? C44 C43 N10 118.2(3) . . ? C48 C43 N10 123.7(4) . . ? C45 C44 C43 121.7(4) . . ? C44 C45 C46 119.9(4) . . ? C47 C46 C45 118.3(4) . . ? C46 C47 C48 122.1(4) . . ? C47 C48 C43 120.1(4) . . ? N11 C49 C50 108.8(3) . . ? N12 C50 C49 110.3(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.503 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.047 #==END data_compound_3 _database_code_CSD 203778 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Al(Me2)(C6H5N)C{N(CH2)2OMe}-]2 _chemical_formula_sum 'C12 H18 Al N2 O' _chemical_formula_weight 233.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 10.3225(10) _cell_length_b 9.2411(8) _cell_length_c 14.5906(13) _cell_angle_alpha 90.00 _cell_angle_beta 108.326(2) _cell_angle_gamma 90.00 _cell_volume 1321.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3111 _cell_measurement_theta_min 2.648 _cell_measurement_theta_max 25.922 _exptl_crystal_description parallelpiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.173 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 500 _exptl_absorpt_coefficient_mu 0.136 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.746 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7182 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 26.03 _reflns_number_total 2595 _reflns_number_gt 2014 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2595 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0571 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1556 _refine_ls_wR_factor_gt 0.1449 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _refine_ls_shift/su_max 0.126 _refine_ls_shift/su_mean 0.016 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 Al Al 0.24409(6) 1.05614(6) -0.11801(4) 0.0335(2) Uani 1 1 d . . . O O 0.14742(15) 1.26093(18) -0.09259(10) 0.0456(4) Uani 1 1 d . . . N1 N 0.37836(16) 1.13817(17) -0.00567(11) 0.0329(4) Uani 1 1 d . . . N2 N 0.60826(16) 1.09227(18) 0.10009(11) 0.0336(4) Uani 1 1 d . . . C1 C 0.49590(18) 1.06860(19) 0.02788(12) 0.0291(4) Uani 1 1 d . . . C2 C 0.3506(2) 1.2750(2) 0.03700(16) 0.0447(5) Uani 1 1 d . . . H2B H 0.3925 1.3553 0.0141 0.054 Uiso 1 1 calc R . . H2C H 0.3882 1.2710 0.1068 0.054 Uiso 1 1 calc R . . C3 C 0.1987(2) 1.2953(3) 0.00741(16) 0.0486(6) Uani 1 1 d . . . H3A H 0.1591 1.2318 0.0444 0.058 Uiso 1 1 calc R . . H3B H 0.1767 1.3945 0.0183 0.058 Uiso 1 1 calc R . . C4 C 0.0045(2) 1.2915(4) -0.1335(2) 0.0710(8) Uani 1 1 d . . . H4A H -0.0146 1.3856 -0.1130 0.107 Uiso 1 1 calc R . . H4B H -0.0472 1.2200 -0.1122 0.107 Uiso 1 1 calc R . . H4C H -0.0204 1.2892 -0.2026 0.107 Uiso 1 1 calc R . . C5 C 0.2276(3) 1.1283(3) -0.24810(15) 0.0481(5) Uani 1 1 d . . . H5A H 0.2642 1.0579 -0.2816 0.072 Uiso 1 1 calc R . . H5B H 0.2774 1.2173 -0.2430 0.072 Uiso 1 1 calc R . . H5C H 0.1332 1.1449 -0.2831 0.072 Uiso 1 1 calc R . . C6 C 0.0993(2) 0.9375(3) -0.09344(18) 0.0512(6) Uani 1 1 d . . . H6A H 0.1177 0.8369 -0.1002 0.077 Uiso 1 1 calc R . . H6B H 0.0127 0.9626 -0.1391 0.077 Uiso 1 1 calc R . . H6C H 0.0971 0.9554 -0.0291 0.077 Uiso 1 1 calc R . . C7 C 0.63032(19) 1.2148(2) 0.16359(13) 0.0358(5) Uani 1 1 d . . . C8 C 0.6819(3) 1.3425(2) 0.13974(18) 0.0510(6) Uani 1 1 d . . . H8A H 0.6980 1.3502 0.0807 0.061 Uiso 1 1 calc R . . C9 C 0.7099(3) 1.4589(3) 0.2027(2) 0.0663(8) Uani 1 1 d . . . H9A H 0.7432 1.5449 0.1856 0.080 Uiso 1 1 calc R . . C10 C 0.6881(3) 1.4468(3) 0.2910(2) 0.0645(8) Uani 1 1 d . . . H10A H 0.7065 1.5247 0.3335 0.077 Uiso 1 1 calc R . . C11 C 0.6395(3) 1.3207(3) 0.31567(18) 0.0606(7) Uani 1 1 d . . . H11A H 0.6255 1.3128 0.3754 0.073 Uiso 1 1 calc R . . C12 C 0.6104(2) 1.2030(3) 0.25245(16) 0.0460(5) Uani 1 1 d . . . H12A H 0.5777 1.1171 0.2701 0.055 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 Al 0.0316(3) 0.0380(4) 0.0275(3) -0.0010(2) 0.0046(2) -0.0016(2) O 0.0375(8) 0.0565(10) 0.0378(8) -0.0018(7) 0.0046(6) 0.0084(7) N1 0.0339(8) 0.0316(9) 0.0300(8) -0.0049(6) 0.0057(6) 0.0022(7) N2 0.0334(8) 0.0331(9) 0.0299(8) -0.0064(7) 0.0037(6) -0.0011(7) C1 0.0320(9) 0.0311(10) 0.0247(9) -0.0006(7) 0.0095(7) -0.0026(7) C2 0.0440(12) 0.0407(12) 0.0424(12) -0.0124(9) 0.0037(9) 0.0102(9) C3 0.0483(12) 0.0558(14) 0.0378(11) -0.0077(10) 0.0080(9) 0.0139(11) C4 0.0416(13) 0.095(2) 0.0640(17) -0.0017(15) -0.0019(11) 0.0195(14) C5 0.0579(13) 0.0495(13) 0.0356(11) 0.0025(10) 0.0130(10) 0.0068(11) C6 0.0436(12) 0.0537(15) 0.0584(14) 0.0003(11) 0.0191(11) -0.0052(10) C7 0.0315(9) 0.0365(11) 0.0336(10) -0.0082(8) 0.0020(8) 0.0018(8) C8 0.0572(14) 0.0413(13) 0.0538(14) -0.0072(10) 0.0166(11) -0.0058(11) C9 0.0662(17) 0.0411(14) 0.087(2) -0.0181(13) 0.0178(15) -0.0096(12) C10 0.0552(15) 0.0564(17) 0.0694(18) -0.0342(13) 0.0017(13) 0.0016(12) C11 0.0608(15) 0.0753(19) 0.0419(13) -0.0188(12) 0.0107(11) 0.0153(14) C12 0.0455(12) 0.0494(13) 0.0419(12) -0.0073(10) 0.0119(9) 0.0009(10) _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 Al N1 1.9374(16) . ? Al C5 1.968(2) . ? Al C6 1.975(2) . ? Al N2 2.0054(17) 3_675 ? Al O 2.2243(17) . ? O C3 1.423(3) . ? O C4 1.435(3) . ? N1 C1 1.323(2) . ? N1 C2 1.477(2) . ? N2 C1 1.317(2) . ? N2 C7 1.435(2) . ? N2 Al 2.0054(17) 3_675 ? C1 C1 1.523(3) 3_675 ? C2 C3 1.502(3) . ? C7 C8 1.383(3) . ? C7 C12 1.379(3) . ? C8 C9 1.386(3) . ? C9 C10 1.379(4) . ? C10 C11 1.362(4) . ? C11 C12 1.396(3) . ? 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 Al C5 120.35(9) . . ? N1 Al C6 116.39(9) . . ? C5 Al C6 121.47(11) . . ? N1 Al N2 81.09(7) . 3_675 ? C5 Al N2 100.91(9) . 3_675 ? C6 Al N2 100.62(9) . 3_675 ? N1 Al O 76.42(6) . . ? C5 Al O 88.01(8) . . ? C6 Al O 92.13(8) . . ? N2 Al O 157.30(6) 3_675 . ? C3 O C4 112.64(18) . . ? C3 O Al 108.61(12) . . ? C4 O Al 123.68(16) . . ? C1 N1 C2 122.46(16) . . ? C1 N1 Al 116.85(12) . . ? C2 N1 Al 120.65(13) . . ? C1 N2 C7 124.64(16) . . ? C1 N2 Al 115.64(12) . 3_675 ? C7 N2 Al 119.71(12) . 3_675 ? N2 C1 N1 133.59(17) . . ? N2 C1 C1 112.5(2) . 3_675 ? N1 C1 C1 113.91(19) . 3_675 ? N1 C2 C3 108.02(17) . . ? O C3 C2 106.57(17) . . ? C8 C7 C12 119.15(19) . . ? C8 C7 N2 120.40(18) . . ? C12 C7 N2 120.26(19) . . ? C7 C8 C9 120.8(2) . . ? C10 C9 C8 119.7(3) . . ? C9 C10 C11 119.9(2) . . ? C10 C11 C12 120.8(2) . . ? C11 C12 C7 119.6(2) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.291 _refine_diff_density_min -0.255 _refine_diff_density_rms 0.048 #==END data_compound_5 _database_code_CSD 203779 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Mg(Br)(THF)(C6H5N)C{N(CH2)2OMe}-]2 _chemical_formula_sum 'C14 H20 Br Mg N2 O2' _chemical_formula_weight 352.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.7976(8) _cell_length_b 11.4638(10) _cell_length_c 15.2253(13) _cell_angle_alpha 90.00 _cell_angle_beta 104.651(2) _cell_angle_gamma 90.00 _cell_volume 1654.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3678 _cell_measurement_theta_min 2.764 _cell_measurement_theta_max 25.356 _exptl_crystal_description parallelpiped _exptl_crystal_colour yellow _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 2.525 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.562 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9070 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 26.02 _reflns_number_total 3247 _reflns_number_gt 2421 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3247 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1249 _refine_ls_wR_factor_gt 0.1154 _refine_ls_goodness_of_fit_ref 0.864 _refine_ls_restrained_S_all 0.864 _refine_ls_shift/su_max 0.257 _refine_ls_shift/su_mean 0.047 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg Mg 0.97587(9) 0.83929(7) 0.13529(6) 0.0430(2) Uani 1 1 d . . . Br Br 0.87928(4) 0.63842(3) 0.11011(3) 0.07263(18) Uani 1 1 d . . . O1 O 0.8428(2) 0.89573(18) 0.22022(13) 0.0614(5) Uani 1 1 d . . . O2 O 1.1410(2) 0.82420(18) 0.24850(14) 0.0645(6) Uani 1 1 d . . . N1 N 0.9002(2) 1.12797(17) -0.04324(14) 0.0405(5) Uani 1 1 d . . . N2 N 0.8995(2) 0.99651(17) 0.08097(13) 0.0421(5) Uani 1 1 d . . . C1 C 0.9398(2) 1.0360(2) 0.01034(14) 0.0354(5) Uani 1 1 d . . . C2 C 0.7745(3) 1.1909(2) -0.04578(16) 0.0420(6) Uani 1 1 d . . . C3 C 0.6431(3) 1.1374(3) -0.0686(2) 0.0600(8) Uani 1 1 d . . . H3A H 0.6367 1.0575 -0.0794 0.072 Uiso 1 1 calc R . . C4 C 0.5208(3) 1.2024(4) -0.0755(2) 0.0756(10) Uani 1 1 d . . . H4A H 0.4333 1.1657 -0.0901 0.091 Uiso 1 1 calc R . . C5 C 0.5293(4) 1.3215(3) -0.0608(2) 0.0704(9) Uani 1 1 d . . . H5A H 0.4479 1.3652 -0.0653 0.085 Uiso 1 1 calc R . . C6 C 0.6574(4) 1.3737(3) -0.0398(2) 0.0633(8) Uani 1 1 d . . . H6A H 0.6635 1.4537 -0.0295 0.076 Uiso 1 1 calc R . . C7 C 0.7788(3) 1.3100(2) -0.03344(18) 0.0495(6) Uani 1 1 d . . . H7A H 0.8653 1.3482 -0.0206 0.059 Uiso 1 1 calc R . . C8 C 0.8031(3) 1.0602(3) 0.12302(18) 0.0559(7) Uani 1 1 d . . . H8A H 0.7060 1.0436 0.0915 0.067 Uiso 1 1 calc R . . H8B H 0.8187 1.1435 0.1203 0.067 Uiso 1 1 calc R . . C9 C 0.8326(4) 1.0206(3) 0.2204(2) 0.0684(9) Uani 1 1 d . . . H9A H 0.9201 1.0543 0.2556 0.082 Uiso 1 1 calc R . . H9B H 0.7569 1.0447 0.2469 0.082 Uiso 1 1 calc R . . C10 C 0.8360(6) 0.8457(3) 0.3042(3) 0.1064(17) Uani 1 1 d . . . H10A H 0.7681 0.8873 0.3279 0.160 Uiso 1 1 calc R . . H10B H 0.9270 0.8506 0.3465 0.160 Uiso 1 1 calc R . . H10C H 0.8084 0.7654 0.2951 0.160 Uiso 1 1 calc R . . C11 C 1.1947(6) 0.7202(4) 0.2958(4) 0.142(2) Uani 1 1 d . . . H11A H 1.1826 0.6549 0.2541 0.171 Uiso 1 1 calc R . . H11B H 1.1450 0.7031 0.3419 0.171 Uiso 1 1 calc R . . C12 C 1.3380(7) 0.7390(6) 0.3359(5) 0.194(4) Uani 1 1 d . . . H12A H 1.3945 0.6952 0.3035 0.233 Uiso 1 1 calc R . . H12B H 1.3610 0.7121 0.3983 0.233 Uiso 1 1 calc R . . C13 C 1.3693(7) 0.8596(6) 0.3335(5) 0.150(3) Uani 1 1 d . . . H13A H 1.4485 0.8717 0.3072 0.180 Uiso 1 1 calc R . . H13B H 1.3924 0.8922 0.3943 0.180 Uiso 1 1 calc R . . C14 C 1.2426(4) 0.9140(3) 0.2777(3) 0.0899(12) Uani 1 1 d . . . H14A H 1.2070 0.9720 0.3126 0.108 Uiso 1 1 calc R . . H14B H 1.2634 0.9521 0.2257 0.108 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg 0.0443(5) 0.0450(5) 0.0416(5) 0.0064(4) 0.0145(4) 0.0017(4) Br 0.0739(3) 0.0577(2) 0.0976(3) -0.00849(16) 0.0424(2) -0.01891(15) O1 0.0824(14) 0.0614(11) 0.0515(11) 0.0134(9) 0.0377(10) 0.0120(11) O2 0.0670(14) 0.0633(12) 0.0545(12) 0.0156(10) -0.0005(10) 0.0054(11) N1 0.0363(11) 0.0439(11) 0.0422(11) 0.0061(9) 0.0116(9) 0.0059(9) N2 0.0456(11) 0.0467(12) 0.0383(11) 0.0030(9) 0.0187(9) 0.0080(9) C1 0.0343(12) 0.0388(12) 0.0328(11) -0.0044(9) 0.0080(9) -0.0017(10) C2 0.0385(13) 0.0511(14) 0.0370(12) 0.0071(11) 0.0106(10) 0.0057(11) C3 0.0455(17) 0.0650(19) 0.0678(19) -0.0020(15) 0.0112(14) 0.0004(13) C4 0.0354(16) 0.105(3) 0.082(2) 0.006(2) 0.0069(15) 0.0049(17) C5 0.057(2) 0.090(2) 0.067(2) 0.0151(18) 0.0202(16) 0.0315(19) C6 0.072(2) 0.0616(18) 0.0616(18) 0.0104(14) 0.0269(16) 0.0206(16) C7 0.0512(16) 0.0503(15) 0.0492(15) 0.0046(12) 0.0167(12) 0.0057(12) C8 0.0683(19) 0.0544(15) 0.0558(16) 0.0080(13) 0.0353(14) 0.0188(14) C9 0.096(2) 0.0660(19) 0.0572(18) 0.0038(15) 0.0445(17) 0.0157(18) C10 0.162(5) 0.098(3) 0.088(3) 0.037(2) 0.084(3) 0.021(3) C11 0.134(4) 0.101(3) 0.150(5) 0.070(3) -0.042(4) -0.002(3) C12 0.156(6) 0.123(5) 0.223(8) 0.004(5) -0.102(5) 0.046(5) C13 0.101(4) 0.147(6) 0.159(6) 0.033(4) -0.044(4) -0.019(4) C14 0.106(3) 0.075(2) 0.072(2) -0.0104(19) -0.006(2) -0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg N2 2.044(2) . ? Mg O2 2.051(2) . ? Mg N1 2.107(2) 3_775 ? Mg O1 2.155(2) . ? Mg Br 2.4823(9) . ? O1 C10 1.418(4) . ? O1 C9 1.435(4) . ? O2 C11 1.423(4) . ? O2 C14 1.423(4) . ? N1 C1 1.329(3) . ? N1 C2 1.419(3) . ? N1 Mg 2.107(2) 3_775 ? N2 C1 1.316(3) . ? N2 C8 1.463(3) . ? C1 C1 1.536(4) 3_775 ? C2 C3 1.388(4) . ? C2 C7 1.378(4) . ? C3 C4 1.393(4) . ? C4 C5 1.382(5) . ? C5 C6 1.353(5) . ? C6 C7 1.378(4) . ? C8 C9 1.507(4) . ? C11 C12 1.399(7) . ? C12 C13 1.418(7) . ? C13 C14 1.455(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Mg O2 123.00(9) . . ? N2 Mg N1 77.74(8) . 3_775 ? O2 Mg N1 96.27(9) . 3_775 ? N2 Mg O1 76.28(8) . . ? O2 Mg O1 89.38(10) . . ? N1 Mg O1 152.07(9) 3_775 . ? N2 Mg Br 131.99(7) . . ? O2 Mg Br 103.91(7) . . ? N1 Mg Br 108.89(6) 3_775 . ? O1 Mg Br 96.11(6) . . ? C10 O1 C9 112.5(2) . . ? C10 O1 Mg 126.4(2) . . ? C9 O1 Mg 110.72(16) . . ? C11 O2 C14 107.9(3) . . ? C11 O2 Mg 127.4(2) . . ? C14 O2 Mg 122.83(19) . . ? C1 N1 C2 122.4(2) . . ? C1 N1 Mg 114.91(16) . 3_775 ? C2 N1 Mg 122.24(15) . 3_775 ? C1 N2 C8 123.1(2) . . ? C1 N2 Mg 118.61(16) . . ? C8 N2 Mg 118.28(16) . . ? N2 C1 N1 132.3(2) . . ? N2 C1 C1 112.8(2) . 3_775 ? N1 C1 C1 114.9(2) . 3_775 ? C3 C2 C7 117.8(3) . . ? C3 C2 N1 121.7(2) . . ? C7 C2 N1 120.2(2) . . ? C2 C3 C4 120.5(3) . . ? C5 C4 C3 120.1(3) . . ? C6 C5 C4 119.3(3) . . ? C5 C6 C7 121.0(3) . . ? C6 C7 C2 121.3(3) . . ? N2 C8 C9 107.2(2) . . ? O1 C9 C8 107.2(2) . . ? O2 C11 C12 107.1(5) . . ? C11 C12 C13 109.8(5) . . ? C12 C13 C14 106.0(4) . . ? O2 C14 C13 107.3(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.603 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.060 #==END data_compound_6 _database_code_CSD 203780 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Mg(Br)(THF)(C6H5N)C{N(CH2)2NMe2}-]2 _chemical_formula_sum 'C15 H23 Br Mg N3 O' _chemical_formula_weight 365.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.3022(7) _cell_length_b 12.2215(8) _cell_length_c 14.8699(9) _cell_angle_alpha 90.00 _cell_angle_beta 108.0400(10) _cell_angle_gamma 90.00 _cell_volume 1780.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4078 _cell_measurement_theta_min 2.199 _cell_measurement_theta_max 25.809 _exptl_crystal_description parallelpiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 2.347 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.511 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9764 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 26.05 _reflns_number_total 3505 _reflns_number_gt 2706 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3505 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.1152 _refine_ls_wR_factor_gt 0.1066 _refine_ls_goodness_of_fit_ref 0.813 _refine_ls_restrained_S_all 0.813 _refine_ls_shift/su_max 0.293 _refine_ls_shift/su_mean 0.043 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg Mg 1.08477(8) 0.35556(6) -0.11952(6) 0.0379(2) Uani 1 1 d . . . Br Br 1.25477(3) 0.20531(3) -0.05732(2) 0.06040(15) Uani 1 1 d . . . O O 0.9383(2) 0.28706(18) -0.23166(15) 0.0676(6) Uani 1 1 d . . . N1 N 1.04083(19) 0.64038(15) 0.03048(14) 0.0369(4) Uani 1 1 d . . . N2 N 1.0879(2) 0.51836(16) -0.08377(13) 0.0383(4) Uani 1 1 d . . . N3 N 1.1952(3) 0.4327(2) -0.21513(19) 0.0670(7) Uani 1 1 d . . . C1 C 1.0394(2) 0.54663(18) -0.01520(15) 0.0321(5) Uani 1 1 d . . . C2 C 1.1357(3) 0.72500(19) 0.03049(17) 0.0380(5) Uani 1 1 d . . . C3 C 1.0915(3) 0.8323(2) 0.0156(2) 0.0514(7) Uani 1 1 d . . . H3A H 0.9991 0.8479 0.0018 0.062 Uiso 1 1 calc R . . C4 C 1.1834(4) 0.9171(2) 0.0210(2) 0.0634(8) Uani 1 1 d . . . H4A H 1.1517 0.9886 0.0096 0.076 Uiso 1 1 calc R . . C5 C 1.3201(3) 0.8964(3) 0.0429(2) 0.0650(8) Uani 1 1 d . . . H5A H 1.3813 0.9533 0.0462 0.078 Uiso 1 1 calc R . . C6 C 1.3659(3) 0.7906(3) 0.0598(2) 0.0636(8) Uani 1 1 d . . . H6A H 1.4588 0.7761 0.0754 0.076 Uiso 1 1 calc R . . C7 C 1.2751(3) 0.7053(2) 0.0540(2) 0.0520(7) Uani 1 1 d . . . H7A H 1.3078 0.6341 0.0660 0.062 Uiso 1 1 calc R . . C8 C 1.1422(3) 0.5970(2) -0.13748(19) 0.0491(6) Uani 1 1 d . . . H8A H 1.2360 0.6154 -0.1029 0.059 Uiso 1 1 calc R . . H8B H 1.0884 0.6637 -0.1485 0.059 Uiso 1 1 calc R . . C9 C 1.1343(4) 0.5428(2) -0.2301(2) 0.0608(8) Uani 1 1 d . . . H9A H 1.0396 0.5375 -0.2688 0.073 Uiso 1 1 calc R . . H9B H 1.1821 0.5874 -0.2637 0.073 Uiso 1 1 calc R . . C10 C 1.3425(4) 0.4398(4) -0.1664(4) 0.1155(19) Uani 1 1 d . . . H10A H 1.3869 0.4722 -0.2079 0.173 Uiso 1 1 calc R . . H10B H 1.3784 0.3677 -0.1488 0.173 Uiso 1 1 calc R . . H10C H 1.3584 0.4841 -0.1108 0.173 Uiso 1 1 calc R . . C11 C 1.1727(8) 0.3791(4) -0.3076(4) 0.147(3) Uani 1 1 d . . . H11A H 1.2234 0.4170 -0.3424 0.221 Uiso 1 1 calc R . . H11B H 1.0772 0.3809 -0.3426 0.221 Uiso 1 1 calc R . . H11C H 1.2029 0.3045 -0.2980 0.221 Uiso 1 1 calc R . . C12 C 0.9365(7) 0.1789(4) -0.2691(4) 0.130(2) Uani 1 1 d . . . H12A H 0.9752 0.1796 -0.3208 0.156 Uiso 1 1 calc R . . H12B H 0.9907 0.1302 -0.2203 0.156 Uiso 1 1 calc R . . C13 C 0.8020(12) 0.1421(7) -0.3012(6) 0.228(6) Uani 1 1 d . . . H13A H 0.7879 0.0847 -0.2601 0.274 Uiso 1 1 calc R . . H13B H 0.7817 0.1129 -0.3647 0.274 Uiso 1 1 calc R . . C14 C 0.7138(6) 0.2344(8) -0.3008(4) 0.158(3) Uani 1 1 d . . . H14A H 0.6651 0.2231 -0.2553 0.189 Uiso 1 1 calc R . . H14B H 0.6478 0.2446 -0.3629 0.189 Uiso 1 1 calc R . . C15 C 0.8042(4) 0.3296(4) -0.2746(3) 0.0945(13) Uani 1 1 d . . . H15A H 0.8009 0.3725 -0.3301 0.113 Uiso 1 1 calc R . . H15B H 0.7771 0.3759 -0.2304 0.113 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg 0.0418(4) 0.0345(4) 0.0417(4) -0.0017(3) 0.0194(3) 0.0013(3) Br 0.0549(2) 0.0554(2) 0.0817(3) 0.02046(14) 0.03695(17) 0.01719(13) O 0.0694(14) 0.0697(15) 0.0558(12) -0.0189(10) 0.0077(11) -0.0013(11) N1 0.0360(10) 0.0311(10) 0.0484(11) -0.0034(8) 0.0200(9) -0.0039(8) N2 0.0461(11) 0.0330(10) 0.0425(11) 0.0018(8) 0.0236(9) -0.0034(9) N3 0.099(2) 0.0503(14) 0.0772(17) 0.0068(12) 0.0655(16) 0.0119(14) C1 0.0298(10) 0.0297(11) 0.0393(12) 0.0012(9) 0.0144(9) -0.0014(9) C2 0.0432(13) 0.0324(12) 0.0434(13) -0.0042(10) 0.0207(11) -0.0049(10) C3 0.0521(16) 0.0359(13) 0.0716(18) -0.0029(13) 0.0272(14) -0.0031(12) C4 0.077(2) 0.0361(15) 0.085(2) -0.0048(14) 0.0381(18) -0.0126(14) C5 0.071(2) 0.0597(19) 0.0697(19) -0.0098(15) 0.0287(16) -0.0330(17) C6 0.0456(16) 0.072(2) 0.073(2) -0.0014(16) 0.0183(15) -0.0171(15) C7 0.0413(14) 0.0498(17) 0.0653(18) 0.0030(12) 0.0168(13) -0.0030(12) C8 0.0601(16) 0.0416(14) 0.0566(15) 0.0086(12) 0.0341(13) 0.0011(12) C9 0.088(2) 0.0538(17) 0.0542(16) 0.0132(13) 0.0418(16) 0.0021(16) C10 0.086(3) 0.084(3) 0.212(5) 0.061(3) 0.098(3) 0.022(2) C11 0.301(8) 0.086(3) 0.118(4) -0.024(3) 0.157(5) -0.018(4) C12 0.167(6) 0.084(3) 0.111(4) -0.054(3) 0.001(4) -0.003(3) C13 0.284(12) 0.139(6) 0.164(7) 0.016(5) -0.074(8) -0.126(7) C14 0.104(4) 0.291(10) 0.066(3) -0.034(5) 0.009(3) -0.094(6) C15 0.072(2) 0.138(4) 0.060(2) 0.016(2) 0.0016(19) 0.014(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 Mg O 2.050(2) . ? Mg N2 2.057(2) . ? Mg N1 2.119(2) 3_765 ? Mg N3 2.282(3) . ? Mg Br 2.5082(8) . ? O C15 1.428(5) . ? O C12 1.432(5) . ? N1 C1 1.330(3) . ? N1 C2 1.423(3) . ? N1 Mg 2.119(2) 3_765 ? N2 C1 1.313(3) . ? N2 C8 1.467(3) . ? N3 C10 1.467(6) . ? N3 C9 1.472(4) . ? N3 C11 1.475(5) . ? C1 C1 1.546(4) 3_765 ? C2 C3 1.384(4) . ? C2 C7 1.390(4) . ? C3 C4 1.389(4) . ? C4 C5 1.366(5) . ? C5 C6 1.372(5) . ? C6 C7 1.385(4) . ? C8 C9 1.508(4) . ? C12 C13 1.393(11) . ? C13 C14 1.449(12) . ? C14 C15 1.465(9) . ? 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 O Mg N2 123.64(9) . . ? O Mg N1 94.56(9) . 3_765 ? N2 Mg N1 77.28(8) . 3_765 ? O Mg N3 92.60(11) . . ? N2 Mg N3 77.90(9) . . ? N1 Mg N3 153.95(9) 3_765 . ? O Mg Br 104.78(7) . . ? N2 Mg Br 131.26(7) . . ? N1 Mg Br 106.17(6) 3_765 . ? N3 Mg Br 96.10(7) . . ? C15 O C12 105.6(4) . . ? C15 O Mg 125.5(2) . . ? C12 O Mg 127.6(3) . . ? C1 N1 C2 121.68(19) . . ? C1 N1 Mg 115.28(14) . 3_765 ? C2 N1 Mg 122.36(15) . 3_765 ? C1 N2 C8 123.4(2) . . ? C1 N2 Mg 118.41(15) . . ? C8 N2 Mg 118.13(15) . . ? C10 N3 C9 110.3(3) . . ? C10 N3 C11 109.0(4) . . ? C9 N3 C11 109.2(3) . . ? C10 N3 Mg 110.8(2) . . ? C9 N3 Mg 101.58(16) . . ? C11 N3 Mg 115.7(3) . . ? N2 C1 N1 132.6(2) . . ? N2 C1 C1 113.2(2) . 3_765 ? N1 C1 C1 114.2(2) . 3_765 ? C3 C2 C7 117.9(2) . . ? C3 C2 N1 119.8(2) . . ? C7 C2 N1 122.0(2) . . ? C4 C3 C2 120.9(3) . . ? C3 C4 C5 120.6(3) . . ? C6 C5 C4 119.2(3) . . ? C5 C6 C7 120.7(3) . . ? C6 C7 C2 120.6(3) . . ? N2 C8 C9 106.7(2) . . ? N3 C9 C8 111.3(2) . . ? C13 C12 O 108.8(7) . . ? C12 C13 C14 107.8(6) . . ? C13 C14 C15 105.8(6) . . ? O C15 C14 106.0(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.554 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.056 #==END