# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_Chisholm1822 _database_code_depnum_ccdc_archive 'CCDC 888666' #TrackingRef '12204_web_deposit_cif_file_0_JudithGallucci_1340739962.archive-1822.cif' _audit_creation_date 2011-02-22T16:09:30-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Chisholm 1822' _chemical_formula_moiety 'C44 H54 Mg1 N2 O1' _chemical_formula_sum 'C44 H54 Mg N2 O' _chemical_formula_weight 651.2 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3070(1) _cell_length_b 11.3957(1) _cell_length_c 19.4004(2) _cell_angle_alpha 87.957(1) _cell_angle_beta 81.710(1) _cell_angle_gamma 71.960(1) _cell_volume 1935.92(3) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 6828 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description 'rectangular block' _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.117 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_special_details ;All work was done at 180 K using an Oxford Cryosystems Cryostream Cooler. The data collection strategy was set up to measure a hemisphere of reciprocal space with a redundancy factor of 3.7, which means that 90% of the reflections were measured at least 3.7 times. Phi and omega scans with a frame width of 1.0 degree were used. Data integration was done with Denzo, and scaling and merging of the data was done with Scalepack. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.08 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.283551E-1 _diffrn_orient_matrix_ub_12 -0.616393E-1 _diffrn_orient_matrix_ub_13 0.376234E-1 _diffrn_orient_matrix_ub_21 0.103351 _diffrn_orient_matrix_ub_22 0.112518E-1 _diffrn_orient_matrix_ub_23 -0.48282E-2 _diffrn_orient_matrix_ub_31 -0.392356E-1 _diffrn_orient_matrix_ub_32 0.677648E-1 _diffrn_orient_matrix_ub_33 0.357036E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_av_unetI/netI ? _diffrn_reflns_number 50524 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.04 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 6839 _reflns_number_gt 4623 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ;A portion of the THF ligand is disordered with atoms C42, C43 and C44 each modeled with two sites. Similarity restraints on the C-C bond lengths (with standard uncertainties of 0.01) and on the 1, 3 distances for C42A to C44A and C42B to C44B (with standard uncertainties of 0.02) were used. Rigid-bond restraints for the anisotropic displacement parameters (standard uncertainty of 0.01) of all of the non-hydrogen atoms in the THF ligand were also applied. For each methyl group bonded to a phenyl ring, it looks as if the hydrogen atoms have two sets of positions related by a 60 degree rotation about the C-C bond. These hydrogen atoms were added at calculated positions with each set having an occupancy factor of 0.5 and with U(H) = 1.5 * Ueq(bonded atom). The methyl hydrogen atoms of the n-butyl ligand were added at calculated positions using a riding model with U(H) = 1.5 * Ueq(bonded carbon atom). The torsion angle, which defines the orientation of this methyl group about the C-C bond, was refined. The rest of the hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(bonded atom). 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^ > 2\s(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 'w=1/[\s^2^(Fo^2^)+(0.0790P)^2^+0.3389P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6839 _refine_ls_number_parameters 462 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0846 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.147 _refine_ls_wR_factor_gt 0.1284 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.339 _refine_diff_density_min -0.214 _refine_diff_density_rms 0.04 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.5997(2) 0.39387(18) 0.37411(10) 0.0367(5) Uani 1 1 d . . . C2 C 0.5994(3) 0.35085(19) 0.44330(10) 0.0455(6) Uani 1 1 d . . . H2 H 0.5625 0.3997 0.4845 0.055 Uiso 1 1 calc R . . C3 C 0.6624(2) 0.22532(18) 0.43954(10) 0.0396(5) Uani 1 1 d . . . H3 H 0.6778 0.1706 0.4778 0.047 Uiso 1 1 calc R . . C4 C 0.7003(2) 0.19199(17) 0.36826(9) 0.0315(4) Uani 1 1 d . . . C5 C 0.7655(2) 0.07182(17) 0.34103(9) 0.0310(4) Uani 1 1 d . . . C6 C 0.7960(2) 0.03510(17) 0.27089(9) 0.0324(4) Uani 1 1 d . . . C7 C 0.8589(2) -0.08814(18) 0.24470(10) 0.0392(5) Uani 1 1 d . . . H7 H 0.8907 -0.1607 0.2714 0.047 Uiso 1 1 calc R . . C8 C 0.8650(3) -0.08246(19) 0.17394(10) 0.0438(5) Uani 1 1 d . . . H8 H 0.9005 -0.1502 0.1422 0.053 Uiso 1 1 calc R . . C9 C 0.8082(2) 0.04379(18) 0.15700(9) 0.0351(5) Uani 1 1 d . . . C10 C 0.5469(2) 0.52153(17) 0.34660(10) 0.0371(5) Uani 1 1 d . . . C11 C 0.3924(2) 0.57975(18) 0.34217(11) 0.0420(5) Uani 1 1 d . . . C12 C 0.3498(3) 0.69139(19) 0.30699(11) 0.0451(5) Uani 1 1 d . . . H12 H 0.245 0.7301 0.3034 0.054 Uiso 1 1 calc R . . C13 C 0.4556(3) 0.74711(19) 0.27735(11) 0.0460(6) Uani 1 1 d . . . C14 C 0.6066(3) 0.69184(19) 0.28574(11) 0.0483(6) Uani 1 1 d . . . H14 H 0.6799 0.7311 0.2673 0.058 Uiso 1 1 calc R . . C15 C 0.6547(2) 0.58047(19) 0.32036(11) 0.0429(5) Uani 1 1 d . . . C16 C 0.2725(3) 0.5226(2) 0.37398(13) 0.0569(6) Uani 1 1 d . . . H16A H 0.3214 0.4451 0.3965 0.085 Uiso 0.5 1 calc PR . . H16B H 0.2186 0.5062 0.3374 0.085 Uiso 0.5 1 calc PR . . H16C H 0.1997 0.5796 0.4087 0.085 Uiso 0.5 1 calc PR . . H16D H 0.1717 0.5755 0.3652 0.085 Uiso 0.5 1 calc PR . . H16E H 0.2745 0.5143 0.4243 0.085 Uiso 0.5 1 calc PR . . H16F H 0.2934 0.441 0.3531 0.085 Uiso 0.5 1 calc PR . . C17 C 0.4102(3) 0.8651(2) 0.23612(13) 0.0640(7) Uani 1 1 d . . . H17A H 0.501 0.8897 0.2193 0.096 Uiso 0.5 1 calc PR . . H17B H 0.3369 0.9306 0.2661 0.096 Uiso 0.5 1 calc PR . . H17C H 0.3633 0.8513 0.1963 0.096 Uiso 0.5 1 calc PR . . H17D H 0.2998 0.8914 0.2351 0.096 Uiso 0.5 1 calc PR . . H17E H 0.4639 0.8505 0.1884 0.096 Uiso 0.5 1 calc PR . . H17F H 0.4376 0.9298 0.2582 0.096 Uiso 0.5 1 calc PR . . C18 C 0.8204(3) 0.5255(2) 0.32923(14) 0.0643(7) Uani 1 1 d . . . H18A H 0.8348 0.4477 0.3546 0.096 Uiso 0.5 1 calc PR . . H18B H 0.8515 0.5833 0.3555 0.096 Uiso 0.5 1 calc PR . . H18C H 0.8829 0.5098 0.2833 0.096 Uiso 0.5 1 calc PR . . H18D H 0.878 0.5794 0.3077 0.096 Uiso 0.5 1 calc PR . . H18E H 0.8613 0.4439 0.3068 0.096 Uiso 0.5 1 calc PR . . H18F H 0.8298 0.5174 0.379 0.096 Uiso 0.5 1 calc PR . . C19 C 0.8104(2) -0.03031(17) 0.39253(9) 0.0310(4) Uani 1 1 d . . . C20 C 0.7059(2) -0.09086(17) 0.42167(9) 0.0343(5) Uani 1 1 d . . . C21 C 0.7544(2) -0.18707(18) 0.46800(10) 0.0408(5) Uani 1 1 d . . . H21 H 0.6849 -0.229 0.488 0.049 Uiso 1 1 calc R . . C22 C 0.9002(3) -0.22301(18) 0.48561(10) 0.0413(5) Uani 1 1 d . . . C23 C 1.0009(2) -0.16198(19) 0.45572(10) 0.0412(5) Uani 1 1 d . . . H23 H 1.1018 -0.1866 0.4672 0.049 Uiso 1 1 calc R . . C24 C 0.9585(2) -0.06580(17) 0.40951(9) 0.0348(5) Uani 1 1 d . . . C25 C 0.5451(2) -0.0532(2) 0.40472(11) 0.0470(6) Uani 1 1 d . . . H25A H 0.5308 0.0153 0.3717 0.071 Uiso 0.5 1 calc PR . . H25B H 0.4732 -0.0268 0.4475 0.071 Uiso 0.5 1 calc PR . . H25C H 0.5267 -0.1234 0.3839 0.071 Uiso 0.5 1 calc PR . . H25D H 0.4897 -0.1052 0.4304 0.071 Uiso 0.5 1 calc PR . . H25E H 0.5473 -0.0631 0.3546 0.071 Uiso 0.5 1 calc PR . . H25F H 0.4937 0.0334 0.4182 0.071 Uiso 0.5 1 calc PR . . C26 C 0.9493(3) -0.3251(2) 0.53742(12) 0.0607(7) Uani 1 1 d . . . H26A H 1.0558 -0.3374 0.5433 0.091 Uiso 0.5 1 calc PR . . H26B H 0.9396 -0.4017 0.5202 0.091 Uiso 0.5 1 calc PR . . H26C H 0.8843 -0.3022 0.5824 0.091 Uiso 0.5 1 calc PR . . H26D H 0.864 -0.3568 0.554 0.091 Uiso 0.5 1 calc PR . . H26E H 0.9802 -0.2925 0.577 0.091 Uiso 0.5 1 calc PR . . H26F H 1.0355 -0.392 0.5149 0.091 Uiso 0.5 1 calc PR . . C27 C 1.0719(2) -0.0009(2) 0.37882(11) 0.0452(5) Uani 1 1 d . . . H27A H 1.0239 0.0643 0.3475 0.068 Uiso 0.5 1 calc PR . . H27B H 1.1609 -0.0605 0.3526 0.068 Uiso 0.5 1 calc PR . . H27C H 1.1044 0.0357 0.4164 0.068 Uiso 0.5 1 calc PR . . H27D H 1.1689 -0.038 0.3969 0.068 Uiso 0.5 1 calc PR . . H27E H 1.0319 0.0868 0.3917 0.068 Uiso 0.5 1 calc PR . . H27F H 1.0884 -0.0094 0.328 0.068 Uiso 0.5 1 calc PR . . C28 C 0.7957(2) 0.10161(18) 0.08734(9) 0.0356(5) Uani 1 1 d . . . C29 C 0.9107(2) 0.14962(19) 0.05611(10) 0.0398(5) Uani 1 1 d . . . C30 C 0.8914(3) 0.2135(2) -0.00577(10) 0.0445(5) Uani 1 1 d . . . H30 H 0.9684 0.2475 -0.0264 0.053 Uiso 1 1 calc R . . C31 C 0.7646(3) 0.2296(2) -0.03843(10) 0.0455(6) Uani 1 1 d . . . C32 C 0.6555(3) 0.1766(2) -0.00823(10) 0.0478(6) Uani 1 1 d . . . H32 H 0.5689 0.1844 -0.0308 0.057 Uiso 1 1 calc R . . C33 C 0.6688(2) 0.1125(2) 0.05385(10) 0.0422(5) Uani 1 1 d . . . C34 C 1.0522(3) 0.1329(2) 0.08915(12) 0.0560(6) Uani 1 1 d . . . H34A H 1.0467 0.086 0.1322 0.084 Uiso 0.5 1 calc PR . . H34B H 1.06 0.214 0.0999 0.084 Uiso 0.5 1 calc PR . . H34C H 1.1421 0.088 0.0569 0.084 Uiso 0.5 1 calc PR . . H34D H 1.1191 0.1727 0.0604 0.084 Uiso 0.5 1 calc PR . . H34E H 1.1059 0.0447 0.0928 0.084 Uiso 0.5 1 calc PR . . H34F H 1.0238 0.1706 0.1358 0.084 Uiso 0.5 1 calc PR . . C35 C 0.7458(3) 0.3024(3) -0.10491(12) 0.0669(7) Uani 1 1 d . . . H35A H 0.6496 0.3038 -0.1205 0.1 Uiso 0.5 1 calc PR . . H35B H 0.8311 0.2635 -0.141 0.1 Uiso 0.5 1 calc PR . . H35C H 0.7443 0.387 -0.0965 0.1 Uiso 0.5 1 calc PR . . H35D H 0.8338 0.3324 -0.1181 0.1 Uiso 0.5 1 calc PR . . H35E H 0.6523 0.3727 -0.0976 0.1 Uiso 0.5 1 calc PR . . H35F H 0.739 0.2492 -0.1421 0.1 Uiso 0.5 1 calc PR . . C36 C 0.5483(3) 0.0550(2) 0.08484(11) 0.0596(7) Uani 1 1 d . . . H36A H 0.5758 0.014 0.1285 0.089 Uiso 0.5 1 calc PR . . H36B H 0.5413 -0.0057 0.052 0.089 Uiso 0.5 1 calc PR . . H36C H 0.4495 0.1194 0.0942 0.089 Uiso 0.5 1 calc PR . . H36D H 0.4686 0.0711 0.0546 0.089 Uiso 0.5 1 calc PR . . H36E H 0.5031 0.0908 0.1311 0.089 Uiso 0.5 1 calc PR . . H36F H 0.5949 -0.0343 0.0889 0.089 Uiso 0.5 1 calc PR . . C37 C 0.6674(3) 0.4471(2) 0.14899(11) 0.0509(6) Uani 1 1 d . A . H37A H 0.644 0.4213 0.1048 0.061 Uiso 1 1 calc R . . H37B H 0.581 0.5204 0.166 0.061 Uiso 1 1 calc R . . C38 C 0.8035(3) 0.4919(2) 0.12988(13) 0.0600(7) Uani 1 1 d . . . H38A H 0.8874 0.4244 0.105 0.072 Uiso 1 1 calc R . . H38B H 0.8375 0.5094 0.1734 0.072 Uiso 1 1 calc R . . C39 C 0.7774(3) 0.6100(3) 0.08346(14) 0.0730(8) Uani 1 1 d . . . H39A H 0.6876 0.6758 0.1059 0.088 Uiso 1 1 calc R . . H39B H 0.8673 0.6397 0.0806 0.088 Uiso 1 1 calc R . . C40 C 0.7525(4) 0.5874(3) 0.01213(14) 0.0868(9) Uani 1 1 d . . . H40A H 0.8433 0.5256 -0.0113 0.13 Uiso 1 1 calc R . . H40B H 0.7333 0.6645 -0.0141 0.13 Uiso 1 1 calc R . . H40C H 0.6642 0.5569 0.0146 0.13 Uiso 1 1 calc R . . C41 C 0.3709(3) 0.2177(2) 0.26763(12) 0.0503(6) Uani 1 1 d DU . . H41A H 0.3496 0.2436 0.3172 0.06 Uiso 0.586(15) 1 calc PR A 1 H41B H 0.4411 0.1322 0.2636 0.06 Uiso 0.586(15) 1 calc PR A 1 H41C H 0.3813 0.2247 0.3173 0.06 Uiso 0.414(15) 1 calc PR A 2 H41D H 0.4211 0.131 0.2521 0.06 Uiso 0.414(15) 1 calc PR A 2 C42A C 0.2251(9) 0.2257(12) 0.2401(7) 0.066(3) Uani 0.586(15) 1 d PDU A 1 H42A H 0.1467 0.2134 0.2774 0.08 Uiso 0.586(15) 1 calc PR A 1 H42B H 0.2425 0.1651 0.202 0.08 Uiso 0.586(15) 1 calc PR A 1 C43A C 0.1815(12) 0.3570(10) 0.2136(7) 0.078(3) Uani 0.586(15) 1 d PDU A 1 H43A H 0.1092 0.3693 0.1792 0.093 Uiso 0.586(15) 1 calc PR A 1 H43B H 0.1357 0.4173 0.2522 0.093 Uiso 0.586(15) 1 calc PR A 1 C44A C 0.3334(18) 0.3673(16) 0.1801(9) 0.076(4) Uani 0.586(15) 1 d PDU A 1 H44A H 0.3612 0.3303 0.1327 0.091 Uiso 0.586(15) 1 calc PR A 1 H44B H 0.3315 0.4546 0.177 0.091 Uiso 0.586(15) 1 calc PR A 1 C42B C 0.2052(11) 0.2590(19) 0.2573(9) 0.076(6) Uani 0.414(15) 1 d PDU A 2 H42C H 0.1424 0.3167 0.2949 0.091 Uiso 0.414(15) 1 calc PR A 2 H42D H 0.1665 0.1873 0.2569 0.091 Uiso 0.414(15) 1 calc PR A 2 C43B C 0.201(2) 0.3230(18) 0.1872(7) 0.077(4) Uani 0.414(15) 1 d PDU A 2 H43C H 0.2307 0.2629 0.1482 0.093 Uiso 0.414(15) 1 calc PR A 2 H43D H 0.0986 0.3818 0.1835 0.093 Uiso 0.414(15) 1 calc PR A 2 C44B C 0.318(3) 0.389(2) 0.1894(11) 0.055(3) Uani 0.414(15) 1 d PDU A 2 H44C H 0.3603 0.4065 0.1418 0.066 Uiso 0.414(15) 1 calc PR A 2 H44D H 0.2727 0.4675 0.216 0.066 Uiso 0.414(15) 1 calc PR A 2 Mg Mg 0.65758(8) 0.30462(6) 0.22129(3) 0.0361(2) Uani 1 1 d . . . N1 N 0.65992(18) 0.29875(14) 0.32863(8) 0.0336(4) Uani 1 1 d . A . N2 N 0.76605(18) 0.11516(14) 0.21458(7) 0.0333(4) Uani 1 1 d . A . O O 0.43737(16) 0.30029(13) 0.22526(7) 0.0477(4) Uani 1 1 d U A . 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 C1 0.0432(12) 0.0287(11) 0.0369(11) 0.0001(9) -0.0050(9) -0.0093(9) C2 0.0662(15) 0.0316(12) 0.0331(11) -0.0050(9) -0.0015(10) -0.0087(11) C3 0.0552(13) 0.0315(12) 0.0294(11) 0.0034(9) -0.0054(9) -0.0102(10) C4 0.0376(11) 0.0255(11) 0.0304(10) 0.0032(8) -0.0050(8) -0.0084(9) C5 0.0330(11) 0.0296(11) 0.0296(10) 0.0033(8) -0.0049(8) -0.0086(9) C6 0.0381(11) 0.0284(11) 0.0291(10) 0.0039(8) -0.0050(8) -0.0083(9) C7 0.0521(13) 0.0285(11) 0.0332(11) 0.0039(9) -0.0043(9) -0.0081(10) C8 0.0632(15) 0.0310(12) 0.0330(11) -0.0044(9) -0.0013(10) -0.0103(11) C9 0.0417(12) 0.0339(12) 0.0290(10) 0.0009(9) -0.0027(8) -0.0114(9) C10 0.0495(13) 0.0251(11) 0.0348(11) -0.0021(9) -0.0031(9) -0.0095(10) C11 0.0507(14) 0.0273(11) 0.0453(12) -0.0031(9) -0.0038(10) -0.0091(10) C12 0.0479(13) 0.0311(12) 0.0502(13) -0.0005(10) -0.0055(10) -0.0037(10) C13 0.0638(16) 0.0278(12) 0.0427(12) 0.0001(9) -0.0055(11) -0.0096(11) C14 0.0616(16) 0.0330(13) 0.0527(13) 0.0025(10) -0.0006(11) -0.0217(12) C15 0.0489(14) 0.0325(12) 0.0473(12) 0.0007(10) -0.0073(10) -0.0123(10) C16 0.0515(15) 0.0448(14) 0.0718(16) 0.0045(12) -0.0004(12) -0.0154(12) C17 0.0847(19) 0.0371(14) 0.0652(16) 0.0145(12) -0.0107(14) -0.0128(13) C18 0.0554(16) 0.0570(16) 0.0832(18) 0.0126(14) -0.0144(13) -0.0205(13) C19 0.0404(12) 0.0245(10) 0.0248(9) -0.0004(8) -0.0019(8) -0.0063(9) C20 0.0430(12) 0.0298(11) 0.0284(10) 0.0000(8) -0.0014(9) -0.0102(9) C21 0.0534(14) 0.0334(12) 0.0353(11) 0.0046(9) 0.0030(10) -0.0174(10) C22 0.0557(14) 0.0291(11) 0.0347(11) 0.0066(9) -0.0050(10) -0.0079(10) C23 0.0457(13) 0.0366(12) 0.0375(11) 0.0060(10) -0.0092(10) -0.0065(10) C24 0.0431(13) 0.0283(11) 0.0307(10) 0.0014(8) -0.0039(9) -0.0084(9) C25 0.0506(14) 0.0505(14) 0.0426(12) 0.0040(10) -0.0050(10) -0.0205(11) C26 0.0791(18) 0.0452(14) 0.0535(14) 0.0223(12) -0.0109(13) -0.0145(13) C27 0.0436(13) 0.0432(13) 0.0489(13) 0.0088(10) -0.0068(10) -0.0141(11) C28 0.0461(13) 0.0313(11) 0.0271(10) 0.0008(8) -0.0037(9) -0.0091(10) C29 0.0451(13) 0.0403(12) 0.0318(11) 0.0006(9) -0.0044(9) -0.0103(10) C30 0.0531(14) 0.0463(14) 0.0346(11) 0.0037(10) -0.0006(10) -0.0188(11) C31 0.0579(15) 0.0444(13) 0.0325(11) 0.0047(10) -0.0073(10) -0.0131(11) C32 0.0547(14) 0.0530(14) 0.0364(12) 0.0043(10) -0.0131(10) -0.0151(12) C33 0.0491(13) 0.0458(13) 0.0325(11) -0.0013(10) -0.0042(10) -0.0162(11) C34 0.0501(14) 0.0709(17) 0.0500(14) 0.0101(12) -0.0089(11) -0.0232(13) C35 0.0844(19) 0.0703(18) 0.0473(14) 0.0267(13) -0.0201(13) -0.0238(15) C36 0.0636(16) 0.0811(19) 0.0452(13) 0.0080(12) -0.0101(11) -0.0380(15) C37 0.0663(16) 0.0404(13) 0.0465(13) 0.0049(10) -0.0043(11) -0.0192(12) C38 0.0544(15) 0.0642(17) 0.0600(15) 0.0067(13) -0.0094(12) -0.0164(13) C39 0.0757(19) 0.0717(19) 0.0775(19) 0.0117(15) 0.0032(15) -0.0385(16) C40 0.100(2) 0.084(2) 0.072(2) 0.0247(17) -0.0056(17) -0.0273(19) C41 0.0598(15) 0.0440(14) 0.0514(13) 0.0093(11) -0.0066(11) -0.0236(12) C42A 0.058(4) 0.075(5) 0.074(7) 0.012(5) -0.016(4) -0.030(3) C43A 0.048(4) 0.083(5) 0.104(8) 0.008(5) -0.032(5) -0.015(4) C44A 0.055(5) 0.069(8) 0.105(9) 0.043(6) -0.037(5) -0.016(6) C42B 0.063(5) 0.116(14) 0.062(7) 0.013(8) -0.009(5) -0.048(7) C43B 0.069(7) 0.095(11) 0.085(8) 0.017(7) -0.031(7) -0.043(7) C44B 0.056(8) 0.057(6) 0.052(5) 0.023(4) -0.026(4) -0.010(5) Mg 0.0455(4) 0.0297(4) 0.0321(4) 0.0067(3) -0.0065(3) -0.0104(3) N1 0.0420(10) 0.0248(9) 0.0324(9) 0.0013(7) -0.0054(7) -0.0081(8) N2 0.0412(10) 0.0312(9) 0.0261(8) 0.0028(7) -0.0039(7) -0.0098(8) O 0.0475(9) 0.0444(9) 0.0535(9) 0.0187(7) -0.0169(7) -0.0150(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.348(2) . ? C1 C2 1.412(3) . ? C1 C10 1.490(3) . ? C2 C3 1.368(3) . ? C2 H2 0.95 . ? C3 C4 1.412(3) . ? C3 H3 0.95 . ? C4 N1 1.395(2) . ? C4 C5 1.402(3) . ? C5 C6 1.401(2) . ? C5 C19 1.505(2) . ? C6 N2 1.401(2) . ? C6 C7 1.424(3) . ? C7 C8 1.366(3) . ? C7 H7 0.95 . ? C8 C9 1.415(3) . ? C8 H8 0.95 . ? C9 N2 1.343(2) . ? C9 C28 1.486(3) . ? C10 C11 1.398(3) . ? C10 C15 1.401(3) . ? C11 C12 1.395(3) . ? C11 C16 1.507(3) . ? C12 C13 1.378(3) . ? C12 H12 0.95 . ? C13 C14 1.381(3) . ? C13 C17 1.515(3) . ? C14 C15 1.391(3) . ? C14 H14 0.95 . ? C15 C18 1.508(3) . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C16 H16D 0.98 . ? C16 H16E 0.98 . ? C16 H16F 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C17 H17D 0.98 . ? C17 H17E 0.98 . ? C17 H17F 0.98 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C18 H18D 0.98 . ? C18 H18E 0.98 . ? C18 H18F 0.98 . ? C19 C24 1.396(3) . ? C19 C20 1.403(3) . ? C20 C21 1.398(3) . ? C20 C25 1.506(3) . ? C21 C22 1.380(3) . ? C21 H21 0.95 . ? C22 C23 1.384(3) . ? C22 C26 1.514(3) . ? C23 C24 1.387(3) . ? C23 H23 0.95 . ? C24 C27 1.512(3) . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C25 H25D 0.98 . ? C25 H25E 0.98 . ? C25 H25F 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C26 H26D 0.98 . ? C26 H26E 0.98 . ? C26 H26F 0.98 . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C27 H27D 0.98 . ? C27 H27E 0.98 . ? C27 H27F 0.98 . ? C28 C33 1.399(3) . ? C28 C29 1.401(3) . ? C29 C30 1.387(3) . ? C29 C34 1.504(3) . ? C30 C31 1.378(3) . ? C30 H30 0.95 . ? C31 C32 1.388(3) . ? C31 C35 1.510(3) . ? C32 C33 1.387(3) . ? C32 H32 0.95 . ? C33 C36 1.511(3) . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C34 H34D 0.98 . ? C34 H34E 0.98 . ? C34 H34F 0.98 . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C35 H35D 0.98 . ? C35 H35E 0.98 . ? C35 H35F 0.98 . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C36 H36D 0.98 . ? C36 H36E 0.98 . ? C36 H36F 0.98 . ? C37 C38 1.502(3) . ? C37 Mg 2.122(2) . ? C37 H37A 0.99 . ? C37 H37B 0.99 . ? C38 C39 1.566(3) . ? C38 H38A 0.99 . ? C38 H38B 0.99 . ? C39 C40 1.480(4) . ? C39 H39A 0.99 . ? C39 H39B 0.99 . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? C41 O 1.450(2) . ? C41 C42A 1.505(6) . ? C41 C42B 1.508(7) . ? C41 H41A 0.99 . ? C41 H41B 0.99 . ? C41 H41C 0.99 . ? C41 H41D 0.99 . ? C42A C43A 1.515(9) . ? C42A H42A 0.99 . ? C42A H42B 0.99 . ? C43A C44A 1.505(8) . ? C43A H43A 0.99 . ? C43A H43B 0.99 . ? C44A O 1.424(19) . ? C44A H44A 0.99 . ? C44A H44B 0.99 . ? C42B C43B 1.520(10) . ? C42B H42C 0.99 . ? C42B H42D 0.99 . ? C43B C44B 1.508(8) . ? C43B H43C 0.99 . ? C43B H43D 0.99 . ? C44B O 1.49(3) . ? C44B H44C 0.99 . ? C44B H44D 0.99 . ? Mg O 2.0557(15) . ? Mg N2 2.0808(16) . ? Mg N1 2.0841(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 110.49(17) . . ? N1 C1 C10 118.86(16) . . ? C2 C1 C10 130.65(18) . . ? C3 C2 C1 106.85(17) . . ? C3 C2 H2 126.6 . . ? C1 C2 H2 126.6 . . ? C2 C3 C4 107.37(17) . . ? C2 C3 H3 126.3 . . ? C4 C3 H3 126.3 . . ? N1 C4 C5 125.07(16) . . ? N1 C4 C3 108.71(16) . . ? C5 C4 C3 126.22(17) . . ? C6 C5 C4 127.60(17) . . ? C6 C5 C19 115.57(16) . . ? C4 C5 C19 116.83(15) . . ? C5 C6 N2 124.93(17) . . ? C5 C6 C7 126.47(17) . . ? N2 C6 C7 108.59(15) . . ? C8 C7 C6 107.18(17) . . ? C8 C7 H7 126.4 . . ? C6 C7 H7 126.4 . . ? C7 C8 C9 106.84(17) . . ? C7 C8 H8 126.6 . . ? C9 C8 H8 126.6 . . ? N2 C9 C8 111.08(16) . . ? N2 C9 C28 119.82(17) . . ? C8 C9 C28 129.07(17) . . ? C11 C10 C15 119.57(18) . . ? C11 C10 C1 120.87(18) . . ? C15 C10 C1 119.40(18) . . ? C12 C11 C10 119.19(19) . . ? C12 C11 C16 119.9(2) . . ? C10 C11 C16 120.90(19) . . ? C13 C12 C11 121.8(2) . . ? C13 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? C12 C13 C14 118.1(2) . . ? C12 C13 C17 121.8(2) . . ? C14 C13 C17 120.1(2) . . ? C13 C14 C15 122.1(2) . . ? C13 C14 H14 118.9 . . ? C15 C14 H14 118.9 . . ? C14 C15 C10 118.9(2) . . ? C14 C15 C18 119.9(2) . . ? C10 C15 C18 121.17(19) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C11 C16 H16D 109.5 . . ? H16A C16 H16D 141.1 . . ? H16B C16 H16D 56.3 . . ? H16C C16 H16D 56.3 . . ? C11 C16 H16E 109.5 . . ? H16A C16 H16E 56.3 . . ? H16B C16 H16E 141.1 . . ? H16C C16 H16E 56.3 . . ? H16D C16 H16E 109.5 . . ? C11 C16 H16F 109.5 . . ? H16A C16 H16F 56.3 . . ? H16B C16 H16F 56.3 . . ? H16C C16 H16F 141.1 . . ? H16D C16 H16F 109.5 . . ? H16E C16 H16F 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C17 H17D 109.5 . . ? H17A C17 H17D 141.1 . . ? H17B C17 H17D 56.3 . . ? H17C C17 H17D 56.3 . . ? C13 C17 H17E 109.5 . . ? H17A C17 H17E 56.3 . . ? H17B C17 H17E 141.1 . . ? H17C C17 H17E 56.3 . . ? H17D C17 H17E 109.5 . . ? C13 C17 H17F 109.5 . . ? H17A C17 H17F 56.3 . . ? H17B C17 H17F 56.3 . . ? H17C C17 H17F 141.1 . . ? H17D C17 H17F 109.5 . . ? H17E C17 H17F 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C15 C18 H18D 109.5 . . ? H18A C18 H18D 141.1 . . ? H18B C18 H18D 56.3 . . ? H18C C18 H18D 56.3 . . ? C15 C18 H18E 109.5 . . ? H18A C18 H18E 56.3 . . ? H18B C18 H18E 141.1 . . ? H18C C18 H18E 56.3 . . ? H18D C18 H18E 109.5 . . ? C15 C18 H18F 109.5 . . ? H18A C18 H18F 56.3 . . ? H18B C18 H18F 56.3 . . ? H18C C18 H18F 141.1 . . ? H18D C18 H18F 109.5 . . ? H18E C18 H18F 109.5 . . ? C24 C19 C20 120.61(17) . . ? C24 C19 C5 118.96(16) . . ? C20 C19 C5 120.41(17) . . ? C21 C20 C19 118.19(18) . . ? C21 C20 C25 120.32(18) . . ? C19 C20 C25 121.49(17) . . ? C22 C21 C20 121.97(19) . . ? C22 C21 H21 119 . . ? C20 C21 H21 119 . . ? C21 C22 C23 118.49(18) . . ? C21 C22 C26 121.2(2) . . ? C23 C22 C26 120.3(2) . . ? C22 C23 C24 121.8(2) . . ? C22 C23 H23 119.1 . . ? C24 C23 H23 119.1 . . ? C23 C24 C19 118.88(18) . . ? C23 C24 C27 119.95(19) . . ? C19 C24 C27 121.16(17) . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C20 C25 H25D 109.5 . . ? H25A C25 H25D 141.1 . . ? H25B C25 H25D 56.3 . . ? H25C C25 H25D 56.3 . . ? C20 C25 H25E 109.5 . . ? H25A C25 H25E 56.3 . . ? H25B C25 H25E 141.1 . . ? H25C C25 H25E 56.3 . . ? H25D C25 H25E 109.5 . . ? C20 C25 H25F 109.5 . . ? H25A C25 H25F 56.3 . . ? H25B C25 H25F 56.3 . . ? H25C C25 H25F 141.1 . . ? H25D C25 H25F 109.5 . . ? H25E C25 H25F 109.5 . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C26 H26D 109.5 . . ? H26A C26 H26D 141.1 . . ? H26B C26 H26D 56.3 . . ? H26C C26 H26D 56.3 . . ? C22 C26 H26E 109.5 . . ? H26A C26 H26E 56.3 . . ? H26B C26 H26E 141.1 . . ? H26C C26 H26E 56.3 . . ? H26D C26 H26E 109.5 . . ? C22 C26 H26F 109.5 . . ? H26A C26 H26F 56.3 . . ? H26B C26 H26F 56.3 . . ? H26C C26 H26F 141.1 . . ? H26D C26 H26F 109.5 . . ? H26E C26 H26F 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C27 H27D 109.5 . . ? H27A C27 H27D 141.1 . . ? H27B C27 H27D 56.3 . . ? H27C C27 H27D 56.3 . . ? C24 C27 H27E 109.5 . . ? H27A C27 H27E 56.3 . . ? H27B C27 H27E 141.1 . . ? H27C C27 H27E 56.3 . . ? H27D C27 H27E 109.5 . . ? C24 C27 H27F 109.5 . . ? H27A C27 H27F 56.3 . . ? H27B C27 H27F 56.3 . . ? H27C C27 H27F 141.1 . . ? H27D C27 H27F 109.5 . . ? H27E C27 H27F 109.5 . . ? C33 C28 C29 119.79(18) . . ? C33 C28 C9 121.00(18) . . ? C29 C28 C9 119.17(18) . . ? C30 C29 C28 118.79(19) . . ? C30 C29 C34 120.46(19) . . ? C28 C29 C34 120.76(18) . . ? C31 C30 C29 122.5(2) . . ? C31 C30 H30 118.8 . . ? C29 C30 H30 118.8 . . ? C30 C31 C32 117.75(19) . . ? C30 C31 C35 121.0(2) . . ? C32 C31 C35 121.3(2) . . ? C33 C32 C31 122.0(2) . . ? C33 C32 H32 119 . . ? C31 C32 H32 119 . . ? C32 C33 C28 119.05(19) . . ? C32 C33 C36 120.5(2) . . ? C28 C33 C36 120.43(18) . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C29 C34 H34D 109.5 . . ? H34A C34 H34D 141.1 . . ? H34B C34 H34D 56.3 . . ? H34C C34 H34D 56.3 . . ? C29 C34 H34E 109.5 . . ? H34A C34 H34E 56.3 . . ? H34B C34 H34E 141.1 . . ? H34C C34 H34E 56.3 . . ? H34D C34 H34E 109.5 . . ? C29 C34 H34F 109.5 . . ? H34A C34 H34F 56.3 . . ? H34B C34 H34F 56.3 . . ? H34C C34 H34F 141.1 . . ? H34D C34 H34F 109.5 . . ? H34E C34 H34F 109.5 . . ? C31 C35 H35A 109.5 . . ? C31 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C31 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C31 C35 H35D 109.5 . . ? H35A C35 H35D 141.1 . . ? H35B C35 H35D 56.3 . . ? H35C C35 H35D 56.3 . . ? C31 C35 H35E 109.5 . . ? H35A C35 H35E 56.3 . . ? H35B C35 H35E 141.1 . . ? H35C C35 H35E 56.3 . . ? H35D C35 H35E 109.5 . . ? C31 C35 H35F 109.5 . . ? H35A C35 H35F 56.3 . . ? H35B C35 H35F 56.3 . . ? H35C C35 H35F 141.1 . . ? H35D C35 H35F 109.5 . . ? H35E C35 H35F 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C33 C36 H36D 109.5 . . ? H36A C36 H36D 141.1 . . ? H36B C36 H36D 56.3 . . ? H36C C36 H36D 56.3 . . ? C33 C36 H36E 109.5 . . ? H36A C36 H36E 56.3 . . ? H36B C36 H36E 141.1 . . ? H36C C36 H36E 56.3 . . ? H36D C36 H36E 109.5 . . ? C33 C36 H36F 109.5 . . ? H36A C36 H36F 56.3 . . ? H36B C36 H36F 56.3 . . ? H36C C36 H36F 141.1 . . ? H36D C36 H36F 109.5 . . ? H36E C36 H36F 109.5 . . ? C38 C37 Mg 124.56(17) . . ? C38 C37 H37A 106.2 . . ? Mg C37 H37A 106.2 . . ? C38 C37 H37B 106.2 . . ? Mg C37 H37B 106.2 . . ? H37A C37 H37B 106.4 . . ? C37 C38 C39 115.6(2) . . ? C37 C38 H38A 108.4 . . ? C39 C38 H38A 108.4 . . ? C37 C38 H38B 108.4 . . ? C39 C38 H38B 108.4 . . ? H38A C38 H38B 107.4 . . ? C40 C39 C38 112.8(2) . . ? C40 C39 H39A 109 . . ? C38 C39 H39A 109 . . ? C40 C39 H39B 109 . . ? C38 C39 H39B 109 . . ? H39A C39 H39B 107.8 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O C41 C42A 105.9(4) . . ? O C41 C42B 104.9(6) . . ? O C41 H41A 110.5 . . ? C42A C41 H41A 110.5 . . ? O C41 H41B 110.5 . . ? C42A C41 H41B 110.5 . . ? H41A C41 H41B 108.7 . . ? O C41 H41C 110.8 . . ? C42B C41 H41C 110.8 . . ? O C41 H41D 110.8 . . ? C42B C41 H41D 110.8 . . ? H41C C41 H41D 108.8 . . ? C41 C42A C43A 100.7(7) . . ? C41 C42A H42A 111.6 . . ? C43A C42A H42A 111.6 . . ? C41 C42A H42B 111.6 . . ? C43A C42A H42B 111.6 . . ? H42A C42A H42B 109.4 . . ? C44A C43A C42A 101.9(7) . . ? C44A C43A H43A 111.4 . . ? C42A C43A H43A 111.4 . . ? C44A C43A H43B 111.4 . . ? C42A C43A H43B 111.4 . . ? H43A C43A H43B 109.2 . . ? O C44A C43A 104.0(9) . . ? O C44A H44A 111 . . ? C43A C44A H44A 110.9 . . ? O C44A H44B 110.9 . . ? C43A C44A H44B 110.9 . . ? H44A C44A H44B 109 . . ? C41 C42B C43B 105.2(11) . . ? C41 C42B H42C 110.7 . . ? C43B C42B H42C 110.7 . . ? C41 C42B H42D 110.7 . . ? C43B C42B H42D 110.7 . . ? H42C C42B H42D 108.8 . . ? C44B C43B C42B 100.9(9) . . ? C44B C43B H43C 111.6 . . ? C42B C43B H43C 111.6 . . ? C44B C43B H43D 111.6 . . ? C42B C43B H43D 111.6 . . ? H43C C43B H43D 109.4 . . ? O C44B C43B 103.8(13) . . ? O C44B H44C 111 . . ? C43B C44B H44C 111 . . ? O C44B H44D 111 . . ? C43B C44B H44D 111 . . ? H44C C44B H44D 109 . . ? O Mg N2 97.70(6) . . ? O Mg N1 96.13(6) . . ? N2 Mg N1 89.97(6) . . ? O Mg C37 103.04(8) . . ? N2 Mg C37 130.87(8) . . ? N1 Mg C37 130.49(8) . . ? C1 N1 C4 106.58(15) . . ? C1 N1 Mg 126.85(13) . . ? C4 N1 Mg 125.73(12) . . ? C9 N2 C6 106.31(15) . . ? C9 N2 Mg 127.49(13) . . ? C6 N2 Mg 125.95(12) . . ? C44A O C41 109.5(5) . . ? C41 O C44B 109.5(6) . . ? C44A O Mg 124.6(5) . . ? C41 O Mg 125.49(12) . . ? C44B O Mg 124.9(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 0.3(2) . . . . ? C10 C1 C2 C3 -179.3(2) . . . . ? C1 C2 C3 C4 -0.3(2) . . . . ? C2 C3 C4 N1 0.1(2) . . . . ? C2 C3 C4 C5 -178.95(19) . . . . ? N1 C4 C5 C6 -3.0(3) . . . . ? C3 C4 C5 C6 175.90(19) . . . . ? N1 C4 C5 C19 176.03(17) . . . . ? C3 C4 C5 C19 -5.0(3) . . . . ? C4 C5 C6 N2 0.3(3) . . . . ? C19 C5 C6 N2 -178.80(17) . . . . ? C4 C5 C6 C7 -178.30(19) . . . . ? C19 C5 C6 C7 2.6(3) . . . . ? C5 C6 C7 C8 178.09(19) . . . . ? N2 C6 C7 C8 -0.7(2) . . . . ? C6 C7 C8 C9 0.8(2) . . . . ? C7 C8 C9 N2 -0.8(2) . . . . ? C7 C8 C9 C28 177.3(2) . . . . ? N1 C1 C10 C11 99.2(2) . . . . ? C2 C1 C10 C11 -81.2(3) . . . . ? N1 C1 C10 C15 -76.3(2) . . . . ? C2 C1 C10 C15 103.3(3) . . . . ? C15 C10 C11 C12 4.8(3) . . . . ? C1 C10 C11 C12 -170.74(18) . . . . ? C15 C10 C11 C16 -176.02(19) . . . . ? C1 C10 C11 C16 8.5(3) . . . . ? C10 C11 C12 C13 -1.0(3) . . . . ? C16 C11 C12 C13 179.75(19) . . . . ? C11 C12 C13 C14 -2.6(3) . . . . ? C11 C12 C13 C17 176.9(2) . . . . ? C12 C13 C14 C15 2.7(3) . . . . ? C17 C13 C14 C15 -176.9(2) . . . . ? C13 C14 C15 C10 1.0(3) . . . . ? C13 C14 C15 C18 -178.8(2) . . . . ? C11 C10 C15 C14 -4.8(3) . . . . ? C1 C10 C15 C14 170.82(18) . . . . ? C11 C10 C15 C18 175.08(19) . . . . ? C1 C10 C15 C18 -9.3(3) . . . . ? C6 C5 C19 C24 87.6(2) . . . . ? C4 C5 C19 C24 -91.6(2) . . . . ? C6 C5 C19 C20 -90.9(2) . . . . ? C4 C5 C19 C20 89.9(2) . . . . ? C24 C19 C20 C21 0.1(3) . . . . ? C5 C19 C20 C21 178.51(16) . . . . ? C24 C19 C20 C25 179.30(17) . . . . ? C5 C19 C20 C25 -2.3(3) . . . . ? C19 C20 C21 C22 0.2(3) . . . . ? C25 C20 C21 C22 -179.02(18) . . . . ? C20 C21 C22 C23 -0.6(3) . . . . ? C20 C21 C22 C26 178.27(19) . . . . ? C21 C22 C23 C24 0.6(3) . . . . ? C26 C22 C23 C24 -178.21(19) . . . . ? C22 C23 C24 C19 -0.3(3) . . . . ? C22 C23 C24 C27 179.28(18) . . . . ? C20 C19 C24 C23 0.0(3) . . . . ? C5 C19 C24 C23 -178.46(17) . . . . ? C20 C19 C24 C27 -179.64(17) . . . . ? C5 C19 C24 C27 1.9(3) . . . . ? N2 C9 C28 C33 -96.6(2) . . . . ? C8 C9 C28 C33 85.5(3) . . . . ? N2 C9 C28 C29 81.2(2) . . . . ? C8 C9 C28 C29 -96.7(3) . . . . ? C33 C28 C29 C30 3.7(3) . . . . ? C9 C28 C29 C30 -174.06(18) . . . . ? C33 C28 C29 C34 -176.61(19) . . . . ? C9 C28 C29 C34 5.6(3) . . . . ? C28 C29 C30 C31 -1.3(3) . . . . ? C34 C29 C30 C31 179.1(2) . . . . ? C29 C30 C31 C32 -1.6(3) . . . . ? C29 C30 C31 C35 178.6(2) . . . . ? C30 C31 C32 C33 2.0(3) . . . . ? C35 C31 C32 C33 -178.1(2) . . . . ? C31 C32 C33 C28 0.4(3) . . . . ? C31 C32 C33 C36 -179.5(2) . . . . ? C29 C28 C33 C32 -3.3(3) . . . . ? C9 C28 C33 C32 174.43(18) . . . . ? C29 C28 C33 C36 176.55(19) . . . . ? C9 C28 C33 C36 -5.7(3) . . . . ? Mg C37 C38 C39 -171.79(18) . . . . ? C37 C38 C39 C40 -68.2(3) . . . . ? O C41 C42A C43A -29.8(10) . . . . ? C42B C41 C42A C43A 60(3) . . . . ? C41 C42A C43A C44A 41.0(15) . . . . ? C42A C43A C44A O -38.1(15) . . . . ? O C41 C42B C43B 24.4(17) . . . . ? C42A C41 C42B C43B -71(3) . . . . ? C41 C42B C43B C44B -38(2) . . . . ? C42B C43B C44B O 37(2) . . . . ? C38 C37 Mg O 176.88(19) . . . . ? C38 C37 Mg N2 -70.6(2) . . . . ? C38 C37 Mg N1 66.9(2) . . . . ? C2 C1 N1 C4 -0.2(2) . . . . ? C10 C1 N1 C4 179.43(17) . . . . ? C2 C1 N1 Mg 169.63(14) . . . . ? C10 C1 N1 Mg -10.7(3) . . . . ? C5 C4 N1 C1 179.16(18) . . . . ? C3 C4 N1 C1 0.1(2) . . . . ? C5 C4 N1 Mg 9.1(3) . . . . ? C3 C4 N1 Mg -169.94(13) . . . . ? O Mg N1 C1 -79.67(16) . . . . ? N2 Mg N1 C1 -177.41(16) . . . . ? C37 Mg N1 C1 33.3(2) . . . . ? O Mg N1 C4 88.34(15) . . . . ? N2 Mg N1 C4 -9.40(15) . . . . ? C37 Mg N1 C4 -158.70(15) . . . . ? C8 C9 N2 C6 0.3(2) . . . . ? C28 C9 N2 C6 -177.93(17) . . . . ? C8 C9 N2 Mg -174.06(14) . . . . ? C28 C9 N2 Mg 7.7(3) . . . . ? C5 C6 N2 C9 -178.58(18) . . . . ? C7 C6 N2 C9 0.2(2) . . . . ? C5 C6 N2 Mg -4.1(3) . . . . ? C7 C6 N2 Mg 174.71(13) . . . . ? O Mg N2 C9 84.20(16) . . . . ? N1 Mg N2 C9 -179.62(16) . . . . ? C37 Mg N2 C9 -30.5(2) . . . . ? O Mg N2 C6 -89.15(15) . . . . ? N1 Mg N2 C6 7.04(15) . . . . ? C37 Mg N2 C6 156.14(15) . . . . ? C43A C44A O C41 19.7(12) . . . . ? C43A C44A O C44B -72(5) . . . . ? C43A C44A O Mg -167.6(6) . . . . ? C42A C41 O C44A 6.7(9) . . . . ? C42B C41 O C44A -12.6(12) . . . . ? C42A C41 O C44B 18.8(12) . . . . ? C42B C41 O C44B -0.5(12) . . . . ? C42A C41 O Mg -165.9(6) . . . . ? C42B C41 O Mg 174.8(9) . . . . ? C43B C44B O C44A 69(5) . . . . ? C43B C44B O C41 -23.7(17) . . . . ? C43B C44B O Mg 161.0(9) . . . . ? N2 Mg O C44A -126.7(9) . . . . ? N1 Mg O C44A 142.5(9) . . . . ? C37 Mg O C44A 8.4(9) . . . . ? N2 Mg O C41 44.83(16) . . . . ? N1 Mg O C41 -45.97(16) . . . . ? C37 Mg O C41 179.99(16) . . . . ? N2 Mg O C44B -140.6(11) . . . . ? N1 Mg O C44B 128.6(11) . . . . ? C37 Mg O C44B -5.5(11) . . . . ? data_Chisholm1825 _database_code_depnum_ccdc_archive 'CCDC 888667' #TrackingRef '12205_web_deposit_cif_file_1_JudithGallucci_1340739962.archive-1825.cif' _audit_creation_date 2011-03-03T13:40:38-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Chisholm 1825' _chemical_formula_moiety 'C37 H58 Mg1 N2 O1' _chemical_formula_sum 'C37 H58 Mg N2 O' _chemical_formula_weight 571.16 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2133(1) _cell_length_b 12.1983(1) _cell_length_c 15.8164(2) _cell_angle_alpha 85.663(1) _cell_angle_beta 78.098(1) _cell_angle_gamma 87.241(1) _cell_volume 1733.39(3) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 6072 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.094 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 628 _exptl_special_details ;All work was done at 180 K using an Oxford Cryosystems Cryostream Cooler. The data collection strategy was set up to measure a hemisphere of reciprocal space with a redundancy factor of 3.8, which means that 90% of the reflections were measured at least 3.8 times. Phi and omega scans with a frame width of 1.0 degree were used. Data integration was done with Denzo, and scaling and merging of the data was done with Scalepack. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.435725E-1 _diffrn_orient_matrix_ub_12 0.556093E-1 _diffrn_orient_matrix_ub_13 -0.469603E-1 _diffrn_orient_matrix_ub_21 -0.966184E-1 _diffrn_orient_matrix_ub_22 0.428426E-1 _diffrn_orient_matrix_ub_23 0.88493E-2 _diffrn_orient_matrix_ub_31 0.329248E-1 _diffrn_orient_matrix_ub_32 0.428811E-1 _diffrn_orient_matrix_ub_33 0.437084E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_av_unetI/netI 0.0351 _diffrn_reflns_number 47895 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 6082 _reflns_number_gt 4585 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ;For the methyl carbon atoms C4 and C5, it looks as if the hydrogen atoms have two sets of positions related by a 60 degree rotation about the C-C bond. These hydrogen atoms were added at calculated positions with each set having an occupancy factor of 0.5 and with U(H) = 1.5 * Ueq(bonded atom). The other methyl hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5 * Ueq(bonded carbon atom). The torsion angle, which defines the orientation of each methyl group about the C-C bond, was refined. The rest of the hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(bonded atom). 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^ > 2\s(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 'w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+0.3969P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6082 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.118 _refine_ls_wR_factor_gt 0.1078 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.239 _refine_diff_density_min -0.221 _refine_diff_density_rms 0.041 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.56789(16) 0.04585(13) 0.83211(10) 0.0263(4) Uani 1 1 d . . . C2 C 0.59834(16) 0.12783(13) 0.88329(10) 0.0279(4) Uani 1 1 d . . . H2 H 0.6648 0.1053 0.9204 0.033 Uiso 1 1 calc R . . C3 C 0.54591(16) 0.23816(13) 0.88823(10) 0.0262(4) Uani 1 1 d . . . C4 C 0.6135(2) -0.07049(14) 0.85967(12) 0.0368(4) Uani 1 1 d . . . H4A H 0.5383 -0.1214 0.8527 0.055 Uiso 0.5 1 calc PR . . H4B H 0.6223 -0.0741 0.9205 0.055 Uiso 0.5 1 calc PR . . H4C H 0.7093 -0.0911 0.8236 0.055 Uiso 0.5 1 calc PR . . H4D H 0.7083 -0.0697 0.8785 0.055 Uiso 0.5 1 calc PR . . H4E H 0.6243 -0.1169 0.8107 0.055 Uiso 0.5 1 calc PR . . H4F H 0.5373 -0.1 0.9076 0.055 Uiso 0.5 1 calc PR . . C5 C 0.57351(19) 0.29602(14) 0.96446(11) 0.0340(4) Uani 1 1 d . . . H5A H 0.6466 0.3528 0.9438 0.051 Uiso 0.5 1 calc PR . . H5B H 0.6114 0.2425 1.0047 0.051 Uiso 0.5 1 calc PR . . H5C H 0.4804 0.3302 0.9942 0.051 Uiso 0.5 1 calc PR . . H5D H 0.5123 0.2642 1.018 0.051 Uiso 0.5 1 calc PR . . H5E H 0.5475 0.3745 0.9571 0.051 Uiso 0.5 1 calc PR . . H5F H 0.6786 0.2868 0.9676 0.051 Uiso 0.5 1 calc PR . . C6 C 0.45593(17) -0.02754(12) 0.72622(10) 0.0276(4) Uani 1 1 d . . . C7 C 0.55383(18) -0.08258(14) 0.66155(11) 0.0329(4) Uani 1 1 d . . . C8 C 0.5036(2) -0.17333(14) 0.62820(12) 0.0397(4) Uani 1 1 d . . . H8 H 0.5694 -0.2118 0.5851 0.048 Uiso 1 1 calc R . . C9 C 0.3611(2) -0.20797(15) 0.65656(12) 0.0405(4) Uani 1 1 d . . . H9 H 0.3301 -0.2716 0.6349 0.049 Uiso 1 1 calc R . . C10 C 0.2631(2) -0.14998(14) 0.71666(12) 0.0378(4) Uani 1 1 d . . . H10 H 0.1637 -0.1728 0.7344 0.045 Uiso 1 1 calc R . . C11 C 0.30694(18) -0.05897(13) 0.75170(11) 0.0299(4) Uani 1 1 d . . . C12 C 0.7101(2) -0.04500(15) 0.62397(12) 0.0442(5) Uani 1 1 d . . . H12 H 0.7292 0.0181 0.6566 0.053 Uiso 1 1 calc R . . C13 C 0.8284(2) -0.1358(2) 0.63251(19) 0.0726(7) Uani 1 1 d . . . H13A H 0.8177 -0.1624 0.6934 0.109 Uiso 1 1 calc R . . H13B H 0.9273 -0.1062 0.6115 0.109 Uiso 1 1 calc R . . H13C H 0.8155 -0.1968 0.598 0.109 Uiso 1 1 calc R . . C14 C 0.7225(3) -0.0043(2) 0.52902(14) 0.0699(7) Uani 1 1 d . . . H14A H 0.7069 -0.0654 0.4955 0.105 Uiso 1 1 calc R . . H14B H 0.8215 0.0245 0.5062 0.105 Uiso 1 1 calc R . . H14C H 0.6472 0.0542 0.5245 0.105 Uiso 1 1 calc R . . C15 C 0.19680(18) 0.00410(15) 0.81734(12) 0.0377(4) Uani 1 1 d . . . H15 H 0.2285 0.0821 0.8111 0.045 Uiso 1 1 calc R . . C16 C 0.1994(2) -0.0391(2) 0.90953(13) 0.0582(6) Uani 1 1 d . . . H16A H 0.1754 -0.1171 0.9169 0.087 Uiso 1 1 calc R . . H16B H 0.1261 0.0026 0.9499 0.087 Uiso 1 1 calc R . . H16C H 0.2985 -0.0307 0.9213 0.087 Uiso 1 1 calc R . . C17 C 0.0387(2) 0.0057(2) 0.80141(17) 0.0665(7) Uani 1 1 d . . . H17A H -0.0004 -0.0684 0.8137 0.1 Uiso 1 1 calc R . . H17B H 0.0393 0.03 0.7409 0.1 Uiso 1 1 calc R . . H17C H -0.0242 0.0566 0.8395 0.1 Uiso 1 1 calc R . . C18 C 0.40168(17) 0.39589(13) 0.84888(10) 0.0270(4) Uani 1 1 d . . . C19 C 0.47951(17) 0.49380(13) 0.82582(10) 0.0293(4) Uani 1 1 d . . . C20 C 0.40067(19) 0.59392(14) 0.83723(11) 0.0356(4) Uani 1 1 d . . . H20 H 0.4516 0.6606 0.8212 0.043 Uiso 1 1 calc R . . C21 C 0.2506(2) 0.59807(15) 0.87128(12) 0.0379(4) Uani 1 1 d . . . H21 H 0.1989 0.667 0.879 0.046 Uiso 1 1 calc R . . C22 C 0.17573(19) 0.50181(15) 0.89414(12) 0.0374(4) Uani 1 1 d . . . H22 H 0.0723 0.5054 0.9179 0.045 Uiso 1 1 calc R . . C23 C 0.24775(17) 0.39934(13) 0.88330(10) 0.0306(4) Uani 1 1 d . . . C24 C 0.64549(18) 0.49470(14) 0.78737(12) 0.0364(4) Uani 1 1 d . . . H24 H 0.6848 0.4169 0.7887 0.044 Uiso 1 1 calc R . . C25 C 0.7300(2) 0.55972(17) 0.83996(15) 0.0518(5) Uani 1 1 d . . . H25A H 0.8369 0.5515 0.817 0.078 Uiso 1 1 calc R . . H25B H 0.7076 0.5316 0.9008 0.078 Uiso 1 1 calc R . . H25C H 0.6995 0.6377 0.8357 0.078 Uiso 1 1 calc R . . C26 C 0.6747(2) 0.54006(17) 0.69333(13) 0.0507(5) Uani 1 1 d . . . H26A H 0.6193 0.4985 0.6605 0.076 Uiso 1 1 calc R . . H26B H 0.7811 0.5331 0.6685 0.076 Uiso 1 1 calc R . . H26C H 0.6425 0.6178 0.6904 0.076 Uiso 1 1 calc R . . C27 C 0.16251(18) 0.29454(15) 0.90966(12) 0.0395(4) Uani 1 1 d . . . H27 H 0.2174 0.2349 0.8748 0.047 Uiso 1 1 calc R . . C28 C 0.1564(2) 0.26006(18) 1.00507(15) 0.0591(6) Uani 1 1 d . . . H28A H 0.2575 0.2483 1.0152 0.089 Uiso 1 1 calc R . . H28B H 0.1025 0.1917 1.0205 0.089 Uiso 1 1 calc R . . H28C H 0.1052 0.3181 1.0408 0.089 Uiso 1 1 calc R . . C29 C 0.0050(2) 0.3032(2) 0.89302(15) 0.0582(6) Uani 1 1 d . . . H29A H -0.0539 0.3568 0.9302 0.087 Uiso 1 1 calc R . . H29B H -0.0403 0.2312 0.9061 0.087 Uiso 1 1 calc R . . H29C H 0.0079 0.327 0.8321 0.087 Uiso 1 1 calc R . . C30 C 0.3169(2) 0.25992(16) 0.63482(13) 0.0432(5) Uani 1 1 d . . . H30A H 0.3216 0.1964 0.5988 0.052 Uiso 1 1 calc R . . H30B H 0.2181 0.2596 0.674 0.052 Uiso 1 1 calc R . . C31 C 0.3181(2) 0.36227(18) 0.57400(13) 0.0502(5) Uani 1 1 d . . . H31A H 0.4145 0.364 0.5325 0.06 Uiso 1 1 calc R . . H31B H 0.2394 0.3572 0.5404 0.06 Uiso 1 1 calc R . . C32 C 0.2945(2) 0.46834(18) 0.61834(15) 0.0590(6) Uani 1 1 d . . . H32A H 0.3274 0.5296 0.575 0.071 Uiso 1 1 calc R . . H32B H 0.3577 0.466 0.6621 0.071 Uiso 1 1 calc R . . C33 C 0.1361(3) 0.4917(2) 0.66217(17) 0.0748(7) Uani 1 1 d . . . H33A H 0.0731 0.4972 0.619 0.112 Uiso 1 1 calc R . . H33B H 0.1293 0.5612 0.6903 0.112 Uiso 1 1 calc R . . H33C H 0.1027 0.4319 0.7058 0.112 Uiso 1 1 calc R . . C34 C 0.7166(2) 0.29852(17) 0.55655(11) 0.0425(5) Uani 1 1 d . . . H34A H 0.6743 0.3739 0.5489 0.051 Uiso 1 1 calc R . . H34B H 0.6732 0.2495 0.5219 0.051 Uiso 1 1 calc R . . C35 C 0.8829(2) 0.2975(2) 0.52835(14) 0.0574(6) Uani 1 1 d . . . H35A H 0.9213 0.3719 0.5287 0.069 Uiso 1 1 calc R . . H35B H 0.9146 0.2711 0.4695 0.069 Uiso 1 1 calc R . . C36 C 0.93683(19) 0.21847(18) 0.59515(13) 0.0475(5) Uani 1 1 d . . . H36A H 0.9357 0.1412 0.5802 0.057 Uiso 1 1 calc R . . H36B H 1.0383 0.2352 0.6009 0.057 Uiso 1 1 calc R . . C37 C 0.82506(18) 0.23987(16) 0.67627(12) 0.0392(4) Uani 1 1 d . . . H37A H 0.8191 0.1754 0.7187 0.047 Uiso 1 1 calc R . . H37B H 0.8511 0.3048 0.7033 0.047 Uiso 1 1 calc R . . Mg Mg 0.47501(5) 0.22470(4) 0.71479(3) 0.02538(15) Uani 1 1 d . . . N1 N 0.50223(13) 0.06487(10) 0.76466(8) 0.0257(3) Uani 1 1 d . . . N2 N 0.47422(13) 0.29017(10) 0.83142(8) 0.0254(3) Uani 1 1 d . . . O O 0.68527(12) 0.25986(10) 0.64728(7) 0.0348(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0220(8) 0.0277(9) 0.0275(9) -0.0006(7) -0.0019(7) 0.0020(6) C2 0.0250(8) 0.0321(9) 0.0283(9) -0.0017(7) -0.0102(7) 0.0023(7) C3 0.0229(8) 0.0315(9) 0.0247(9) -0.0045(7) -0.0043(6) -0.0025(7) C4 0.0396(10) 0.0308(10) 0.0407(11) -0.0012(8) -0.0118(8) 0.0047(8) C5 0.0371(10) 0.0367(10) 0.0306(9) -0.0075(8) -0.0109(7) -0.0008(8) C6 0.0345(9) 0.0217(8) 0.0277(9) -0.0008(7) -0.0097(7) 0.0012(7) C7 0.0377(10) 0.0285(9) 0.0326(10) -0.0049(7) -0.0061(7) -0.0010(7) C8 0.0520(11) 0.0329(10) 0.0341(10) -0.0095(8) -0.0060(8) -0.0006(8) C9 0.0575(12) 0.0292(10) 0.0389(11) -0.0061(8) -0.0162(9) -0.0083(9) C10 0.0397(10) 0.0343(10) 0.0417(11) 0.0012(8) -0.0135(8) -0.0083(8) C11 0.0324(9) 0.0264(9) 0.0321(9) 0.0018(7) -0.0103(7) -0.0019(7) C12 0.0419(11) 0.0406(11) 0.0469(12) -0.0195(9) 0.0052(9) -0.0053(8) C13 0.0403(12) 0.0703(16) 0.102(2) -0.0276(14) 0.0041(12) 0.0060(11) C14 0.0815(17) 0.0738(17) 0.0492(14) -0.0158(12) 0.0101(12) -0.0340(13) C15 0.0285(9) 0.0334(10) 0.0503(12) -0.0065(8) -0.0039(8) -0.0037(7) C16 0.0478(12) 0.0793(16) 0.0424(12) -0.0094(11) 0.0035(9) 0.0027(11) C17 0.0391(12) 0.0745(16) 0.0880(18) -0.0177(14) -0.0168(11) 0.0117(11) C18 0.0299(9) 0.0281(9) 0.0244(9) -0.0068(7) -0.0074(7) 0.0022(7) C19 0.0321(9) 0.0291(9) 0.0275(9) -0.0054(7) -0.0066(7) -0.0003(7) C20 0.0418(10) 0.0273(9) 0.0380(10) -0.0059(8) -0.0077(8) -0.0009(8) C21 0.0426(11) 0.0298(10) 0.0411(11) -0.0095(8) -0.0076(8) 0.0090(8) C22 0.0300(9) 0.0399(11) 0.0415(11) -0.0110(8) -0.0038(8) 0.0052(8) C23 0.0309(9) 0.0322(9) 0.0289(9) -0.0081(7) -0.0050(7) 0.0019(7) C24 0.0329(9) 0.0289(9) 0.0466(11) -0.0067(8) -0.0044(8) -0.0024(7) C25 0.0389(11) 0.0481(12) 0.0715(15) -0.0126(11) -0.0139(10) -0.0076(9) C26 0.0454(11) 0.0485(12) 0.0515(13) 0.0005(10) 0.0046(9) -0.0037(9) C27 0.0298(9) 0.0343(10) 0.0513(12) -0.0144(9) 0.0028(8) -0.0013(8) C28 0.0517(13) 0.0513(13) 0.0748(16) 0.0221(12) -0.0204(11) -0.0149(10) C29 0.0454(12) 0.0692(15) 0.0627(15) 0.0016(12) -0.0148(10) -0.0201(11) C30 0.0447(11) 0.0427(11) 0.0493(12) -0.0066(9) -0.0255(9) 0.0027(9) C31 0.0418(11) 0.0681(14) 0.0431(12) 0.0045(10) -0.0185(9) 0.0051(10) C32 0.0614(14) 0.0542(14) 0.0653(15) 0.0136(11) -0.0264(12) -0.0084(11) C33 0.0763(17) 0.0727(17) 0.0723(17) -0.0110(14) -0.0081(13) 0.0070(13) C34 0.0416(10) 0.0555(12) 0.0276(10) 0.0041(9) -0.0038(8) -0.0004(9) C35 0.0396(11) 0.0842(16) 0.0426(12) 0.0016(11) 0.0035(9) -0.0062(11) C36 0.0276(9) 0.0650(14) 0.0505(12) -0.0139(10) -0.0056(8) -0.0016(9) C37 0.0286(9) 0.0498(11) 0.0417(11) -0.0053(9) -0.0122(8) 0.0006(8) Mg 0.0258(3) 0.0255(3) 0.0259(3) -0.0034(2) -0.0077(2) 0.0011(2) N1 0.0255(7) 0.0261(7) 0.0257(7) -0.0047(6) -0.0050(5) -0.0002(5) N2 0.0252(7) 0.0244(7) 0.0267(7) -0.0044(6) -0.0049(6) 0.0007(5) O 0.0276(6) 0.0479(7) 0.0286(6) 0.0012(5) -0.0060(5) -0.0009(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.332(2) . ? C1 C2 1.406(2) . ? C1 C4 1.518(2) . ? C2 C3 1.410(2) . ? C2 H2 0.95 . ? C3 N2 1.328(2) . ? C3 C5 1.513(2) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C4 H4D 0.98 . ? C4 H4E 0.98 . ? C4 H4F 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C5 H5D 0.98 . ? C5 H5E 0.98 . ? C5 H5F 0.98 . ? C6 C7 1.406(2) . ? C6 C11 1.412(2) . ? C6 N1 1.442(2) . ? C7 C8 1.399(2) . ? C7 C12 1.519(2) . ? C8 C9 1.373(3) . ? C8 H8 0.95 . ? C9 C10 1.380(3) . ? C9 H9 0.95 . ? C10 C11 1.390(2) . ? C10 H10 0.95 . ? C11 C15 1.520(2) . ? C12 C14 1.529(3) . ? C12 C13 1.534(3) . ? C12 H12 1 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 C16 1.517(3) . ? C15 C17 1.528(3) . ? C15 H15 1 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 C19 1.408(2) . ? C18 C23 1.410(2) . ? C18 N2 1.442(2) . ? C19 C20 1.395(2) . ? C19 C24 1.525(2) . ? C20 C21 1.376(2) . ? C20 H20 0.95 . ? C21 C22 1.377(3) . ? C21 H21 0.95 . ? C22 C23 1.392(2) . ? C22 H22 0.95 . ? C23 C27 1.519(2) . ? C24 C26 1.522(3) . ? C24 C25 1.534(3) . ? C24 H24 1 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 C29 1.525(3) . ? C27 C28 1.526(3) . ? C27 H27 1 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C30 C31 1.517(3) . ? C30 Mg 2.1269(17) . ? C30 H30A 0.99 . ? C30 H30B 0.99 . ? C31 C32 1.504(3) . ? C31 H31A 0.99 . ? C31 H31B 0.99 . ? C32 C33 1.505(3) . ? C32 H32A 0.99 . ? C32 H32B 0.99 . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? C34 O 1.451(2) . ? C34 C35 1.505(3) . ? C34 H34A 0.99 . ? C34 H34B 0.99 . ? C35 C36 1.519(3) . ? C35 H35A 0.99 . ? C35 H35B 0.99 . ? C36 C37 1.502(3) . ? C36 H36A 0.99 . ? C36 H36B 0.99 . ? C37 O 1.4578(19) . ? C37 H37A 0.99 . ? C37 H37B 0.99 . ? Mg O 2.0577(12) . ? Mg N2 2.0634(14) . ? Mg N1 2.0708(14) . ? 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 C1 C2 124.35(14) . . ? N1 C1 C4 120.53(14) . . ? C2 C1 C4 115.11(14) . . ? C1 C2 C3 130.23(14) . . ? C1 C2 H2 114.9 . . ? C3 C2 H2 114.9 . . ? N2 C3 C2 123.59(14) . . ? N2 C3 C5 120.49(14) . . ? C2 C3 C5 115.91(14) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C1 C4 H4D 109.5 . . ? H4A C4 H4D 141.1 . . ? H4B C4 H4D 56.3 . . ? H4C C4 H4D 56.3 . . ? C1 C4 H4E 109.5 . . ? H4A C4 H4E 56.3 . . ? H4B C4 H4E 141.1 . . ? H4C C4 H4E 56.3 . . ? H4D C4 H4E 109.5 . . ? C1 C4 H4F 109.5 . . ? H4A C4 H4F 56.3 . . ? H4B C4 H4F 56.3 . . ? H4C C4 H4F 141.1 . . ? H4D C4 H4F 109.5 . . ? H4E C4 H4F 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C5 H5D 109.5 . . ? H5A C5 H5D 141.1 . . ? H5B C5 H5D 56.3 . . ? H5C C5 H5D 56.3 . . ? C3 C5 H5E 109.5 . . ? H5A C5 H5E 56.3 . . ? H5B C5 H5E 141.1 . . ? H5C C5 H5E 56.3 . . ? H5D C5 H5E 109.5 . . ? C3 C5 H5F 109.5 . . ? H5A C5 H5F 56.3 . . ? H5B C5 H5F 56.3 . . ? H5C C5 H5F 141.1 . . ? H5D C5 H5F 109.5 . . ? H5E C5 H5F 109.5 . . ? C7 C6 C11 119.98(15) . . ? C7 C6 N1 121.33(14) . . ? C11 C6 N1 118.61(14) . . ? C8 C7 C6 118.70(16) . . ? C8 C7 C12 118.57(15) . . ? C6 C7 C12 122.69(15) . . ? C9 C8 C7 121.29(17) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 119.70(16) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C9 C10 C11 121.38(17) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C10 C11 C6 118.72(15) . . ? C10 C11 C15 120.45(15) . . ? C6 C11 C15 120.82(14) . . ? C7 C12 C14 109.82(17) . . ? C7 C12 C13 112.42(17) . . ? C14 C12 C13 110.25(18) . . ? C7 C12 H12 108.1 . . ? C14 C12 H12 108.1 . . ? C13 C12 H12 108.1 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C11 111.73(15) . . ? C16 C15 C17 110.28(17) . . ? C11 C15 C17 112.94(16) . . ? C16 C15 H15 107.2 . . ? C11 C15 H15 107.2 . . ? C17 C15 H15 107.2 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 120.58(14) . . ? C19 C18 N2 121.03(14) . . ? C23 C18 N2 118.20(14) . . ? C20 C19 C18 118.47(15) . . ? C20 C19 C24 118.83(15) . . ? C18 C19 C24 122.69(14) . . ? C21 C20 C19 121.34(16) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C20 C21 C22 119.71(16) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C21 C22 C23 121.69(16) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C22 C23 C18 118.20(15) . . ? C22 C23 C27 120.53(15) . . ? C18 C23 C27 121.26(14) . . ? C26 C24 C19 111.04(15) . . ? C26 C24 C25 110.17(16) . . ? C19 C24 C25 112.12(15) . . ? C26 C24 H24 107.8 . . ? C19 C24 H24 107.8 . . ? C25 C24 H24 107.8 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 113.61(16) . . ? C23 C27 C28 110.78(15) . . ? C29 C27 C28 109.03(16) . . ? C23 C27 H27 107.7 . . ? C29 C27 H27 107.7 . . ? C28 C27 H27 107.7 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 Mg 123.62(13) . . ? C31 C30 H30A 106.4 . . ? Mg C30 H30A 106.4 . . ? C31 C30 H30B 106.4 . . ? Mg C30 H30B 106.4 . . ? H30A C30 H30B 106.5 . . ? C32 C31 C30 114.42(17) . . ? C32 C31 H31A 108.7 . . ? C30 C31 H31A 108.7 . . ? C32 C31 H31B 108.7 . . ? C30 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? C31 C32 C33 113.95(19) . . ? C31 C32 H32A 108.8 . . ? C33 C32 H32A 108.8 . . ? C31 C32 H32B 108.8 . . ? C33 C32 H32B 108.8 . . ? H32A C32 H32B 107.7 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O C34 C35 106.41(14) . . ? O C34 H34A 110.4 . . ? C35 C34 H34A 110.4 . . ? O C34 H34B 110.4 . . ? C35 C34 H34B 110.4 . . ? H34A C34 H34B 108.6 . . ? C34 C35 C36 103.91(16) . . ? C34 C35 H35A 111 . . ? C36 C35 H35A 111 . . ? C34 C35 H35B 111 . . ? C36 C35 H35B 111 . . ? H35A C35 H35B 109 . . ? C37 C36 C35 102.17(15) . . ? C37 C36 H36A 111.3 . . ? C35 C36 H36A 111.3 . . ? C37 C36 H36B 111.3 . . ? C35 C36 H36B 111.3 . . ? H36A C36 H36B 109.2 . . ? O C37 C36 104.40(14) . . ? O C37 H37A 110.9 . . ? C36 C37 H37A 110.9 . . ? O C37 H37B 110.9 . . ? C36 C37 H37B 110.9 . . ? H37A C37 H37B 108.9 . . ? O Mg N2 101.31(5) . . ? O Mg N1 102.55(5) . . ? N2 Mg N1 93.00(5) . . ? O Mg C30 110.57(7) . . ? N2 Mg C30 126.40(7) . . ? N1 Mg C30 119.20(7) . . ? C1 N1 C6 118.74(13) . . ? C1 N1 Mg 119.76(10) . . ? C6 N1 Mg 121.47(10) . . ? C3 N2 C18 120.14(13) . . ? C3 N2 Mg 120.41(10) . . ? C18 N2 Mg 119.37(10) . . ? C34 O C37 108.94(12) . . ? C34 O Mg 122.91(10) . . ? C37 O Mg 127.81(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 13.6(3) . . . . ? C4 C1 C2 C3 -165.44(16) . . . . ? C1 C2 C3 N2 -12.3(3) . . . . ? C1 C2 C3 C5 166.62(16) . . . . ? C11 C6 C7 C8 -4.7(2) . . . . ? N1 C6 C7 C8 178.47(15) . . . . ? C11 C6 C7 C12 172.96(16) . . . . ? N1 C6 C7 C12 -3.9(2) . . . . ? C6 C7 C8 C9 0.9(3) . . . . ? C12 C7 C8 C9 -176.83(17) . . . . ? C7 C8 C9 C10 2.6(3) . . . . ? C8 C9 C10 C11 -2.3(3) . . . . ? C9 C10 C11 C6 -1.5(3) . . . . ? C9 C10 C11 C15 179.58(16) . . . . ? C7 C6 C11 C10 4.9(2) . . . . ? N1 C6 C11 C10 -178.13(14) . . . . ? C7 C6 C11 C15 -176.09(15) . . . . ? N1 C6 C11 C15 0.8(2) . . . . ? C8 C7 C12 C14 64.7(2) . . . . ? C6 C7 C12 C14 -112.99(19) . . . . ? C8 C7 C12 C13 -58.5(2) . . . . ? C6 C7 C12 C13 123.9(2) . . . . ? C10 C11 C15 C16 91.8(2) . . . . ? C6 C11 C15 C16 -87.2(2) . . . . ? C10 C11 C15 C17 -33.2(2) . . . . ? C6 C11 C15 C17 147.83(18) . . . . ? C23 C18 C19 C20 -0.5(2) . . . . ? N2 C18 C19 C20 174.38(14) . . . . ? C23 C18 C19 C24 -179.26(15) . . . . ? N2 C18 C19 C24 -4.4(2) . . . . ? C18 C19 C20 C21 0.9(3) . . . . ? C24 C19 C20 C21 179.72(16) . . . . ? C19 C20 C21 C22 -0.5(3) . . . . ? C20 C21 C22 C23 -0.4(3) . . . . ? C21 C22 C23 C18 0.8(3) . . . . ? C21 C22 C23 C27 179.59(17) . . . . ? C19 C18 C23 C22 -0.3(2) . . . . ? N2 C18 C23 C22 -175.32(14) . . . . ? C19 C18 C23 C27 -179.14(15) . . . . ? N2 C18 C23 C27 5.9(2) . . . . ? C20 C19 C24 C26 -67.0(2) . . . . ? C18 C19 C24 C26 111.81(18) . . . . ? C20 C19 C24 C25 56.8(2) . . . . ? C18 C19 C24 C25 -124.46(18) . . . . ? C22 C23 C27 C29 36.2(2) . . . . ? C18 C23 C27 C29 -145.00(17) . . . . ? C22 C23 C27 C28 -86.9(2) . . . . ? C18 C23 C27 C28 91.87(19) . . . . ? Mg C30 C31 C32 -63.1(2) . . . . ? C30 C31 C32 C33 -75.9(2) . . . . ? O C34 C35 C36 20.6(2) . . . . ? C34 C35 C36 C37 -34.9(2) . . . . ? C35 C36 C37 O 36.58(19) . . . . ? C31 C30 Mg O -42.70(18) . . . . ? C31 C30 Mg N2 79.78(18) . . . . ? C31 C30 Mg N1 -161.11(14) . . . . ? C2 C1 N1 C6 -170.16(14) . . . . ? C4 C1 N1 C6 8.9(2) . . . . ? C2 C1 N1 Mg 11.9(2) . . . . ? C4 C1 N1 Mg -169.13(11) . . . . ? C7 C6 N1 C1 -86.59(19) . . . . ? C11 C6 N1 C1 96.52(17) . . . . ? C7 C6 N1 Mg 91.35(16) . . . . ? C11 C6 N1 Mg -85.53(16) . . . . ? O Mg N1 C1 75.89(12) . . . . ? N2 Mg N1 C1 -26.41(12) . . . . ? C30 Mg N1 C1 -161.65(12) . . . . ? O Mg N1 C6 -102.04(11) . . . . ? N2 Mg N1 C6 155.67(11) . . . . ? C30 Mg N1 C6 20.42(14) . . . . ? C2 C3 N2 C18 169.14(14) . . . . ? C5 C3 N2 C18 -9.8(2) . . . . ? C2 C3 N2 Mg -14.1(2) . . . . ? C5 C3 N2 Mg 166.94(11) . . . . ? C19 C18 N2 C3 87.10(19) . . . . ? C23 C18 N2 C3 -97.93(18) . . . . ? C19 C18 N2 Mg -89.65(16) . . . . ? C23 C18 N2 Mg 85.32(16) . . . . ? O Mg N2 C3 -75.78(12) . . . . ? N1 Mg N2 C3 27.66(12) . . . . ? C30 Mg N2 C3 157.88(12) . . . . ? O Mg N2 C18 100.96(11) . . . . ? N1 Mg N2 C18 -155.60(11) . . . . ? C30 Mg N2 C18 -25.38(14) . . . . ? C35 C34 O C37 2.4(2) . . . . ? C35 C34 O Mg -171.42(13) . . . . ? C36 C37 O C34 -24.76(19) . . . . ? C36 C37 O Mg 148.63(13) . . . . ? N2 Mg O C34 -138.70(13) . . . . ? N1 Mg O C34 125.60(13) . . . . ? C30 Mg O C34 -2.53(15) . . . . ? N2 Mg O C37 48.75(14) . . . . ? N1 Mg O C37 -46.94(14) . . . . ? C30 Mg O C37 -175.07(13) . . . . ? data_Chisholm1828 _database_code_depnum_ccdc_archive 'CCDC 888668' #TrackingRef '12206_web_deposit_cif_file_2_JudithGallucci_1340739962.archive-1828.cif' _audit_creation_date 2011-04-05T14:28:30-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Chisholm 1828' _chemical_formula_moiety 'C44 H54 Mg N2 O2, 2(C4 H8 O)' _chemical_formula_sum 'C52 H70 Mg N2 O4' _chemical_formula_weight 811.41 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 18.1220(2) _cell_length_b 14.9771(2) _cell_length_c 18.2681(2) _cell_angle_alpha 90 _cell_angle_beta 103.969(1) _cell_angle_gamma 90 _cell_volume 4811.60(10) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8794 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.12 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_special_details ;All work was done at 180 K using an Oxford Cryosystems Cryostream Cooler. The data collection strategy was set up to measure a quadrant of reciprocal space with a redundancy factor of 3.8, which means that 90% of these reflections were measured at least 3.8 times. Omega scans with a frame width of 1.0 degree were used. Data integration was done with Denzo, and scaling and merging of the data was done with Scalepack. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.00842 _diffrn_orient_matrix_ub_12 -0.244262E-1 _diffrn_orient_matrix_ub_13 0.482803E-1 _diffrn_orient_matrix_ub_21 0.293736E-1 _diffrn_orient_matrix_ub_22 -0.548083E-1 _diffrn_orient_matrix_ub_23 -0.62998E-2 _diffrn_orient_matrix_ub_31 0.479555E-1 _diffrn_orient_matrix_ub_32 0.292823E-1 _diffrn_orient_matrix_ub_33 0.284823E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'omega scans' _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_av_unetI/netI ? _diffrn_reflns_number 77883 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 8489 _reflns_number_gt 5173 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ;One of the solvent molecules of THF (containing atoms O3, C45, C46 C47 and C48) is disordered. This was modeled with two sites each for C46 and C47. Similarity restraints on 1-2 and 1-3 distances were used in the refinement of this molecule along with rigid bond restraints for the anisotropic displacement parameters. The occupancy factor for C46A and C47A refined to 0.53(1). Since the sum of the occupancy factors was constrained to one for each disordered pair of atoms, the occupancy factor for C46B and C47B is 0.47(1). The other solvent molecule of THF appears to be ordered, but it was also subject to restraints: a similarity restraint was used for the bonds O4-C49 and O4-C52. For each methyl group, the hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5*Ueq(bonded carbon atom). The torsion angle, which defines the orientation of the methyl group about the C-C bond, was refined. The rest of the hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2*Ueq(bonded atom). 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^ > 2\s(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 'w=1/[\s^2^(Fo^2^)+(0.0952P)^2^+1.6780P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 8489 _refine_ls_number_parameters 563 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.1069 _refine_ls_R_factor_gt 0.0602 _refine_ls_wR_factor_ref 0.1876 _refine_ls_wR_factor_gt 0.1608 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.03 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.508 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.044 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.29483(13) 0.93788(14) 0.43845(12) 0.0354(5) Uani 1 1 d . . . C2 C 0.36522(14) 0.98297(16) 0.44906(14) 0.0451(6) Uani 1 1 d . . . H2 H 0.373 1.0457 0.4515 0.054 Uiso 1 1 calc R . . C3 C 0.41998(13) 0.91825(15) 0.45518(13) 0.0396(6) Uani 1 1 d . . . H3 H 0.4731 0.9278 0.4624 0.048 Uiso 1 1 calc R . . C4 C 0.38262(12) 0.83442(14) 0.44877(12) 0.0322(5) Uani 1 1 d . . . C5 C 0.41778(12) 0.75039(14) 0.45360(12) 0.0305(5) Uani 1 1 d . . . C6 C 0.38400(12) 0.66598(14) 0.45104(12) 0.0314(5) Uani 1 1 d . . . C7 C 0.42287(13) 0.58300(15) 0.46015(13) 0.0394(6) Uani 1 1 d . . . H7 H 0.476 0.5745 0.4665 0.047 Uiso 1 1 calc R . . C8 C 0.36997(13) 0.51757(16) 0.45809(14) 0.0434(6) Uani 1 1 d . . . H8 H 0.3792 0.4552 0.4631 0.052 Uiso 1 1 calc R . . C9 C 0.29867(12) 0.56100(15) 0.44704(12) 0.0341(5) Uani 1 1 d . . . C10 C 0.21808(12) 0.97939(14) 0.42626(13) 0.0354(5) Uani 1 1 d . . . C11 C 0.19232(14) 1.01228(15) 0.48769(13) 0.0402(6) Uani 1 1 d . . . C12 C 0.12007(14) 1.05035(16) 0.47416(14) 0.0451(6) Uani 1 1 d . . . H12 H 0.1019 1.0711 0.5157 0.054 Uiso 1 1 calc R . . C13 C 0.07391(14) 1.05884(16) 0.40187(15) 0.0461(6) Uani 1 1 d . . . C14 C 0.10148(14) 1.02773(17) 0.34228(15) 0.0476(7) Uani 1 1 d . . . H14 H 0.0709 1.034 0.2924 0.057 Uiso 1 1 calc R . . C15 C 0.17246(14) 0.98759(16) 0.35316(13) 0.0417(6) Uani 1 1 d . . . C16 C 0.24152(16) 1.00775(19) 0.56700(14) 0.0580(7) Uani 1 1 d . . . H16A H 0.2818 1.0528 0.5733 0.087 Uiso 1 1 calc R . . H16B H 0.2644 0.9483 0.5762 0.087 Uiso 1 1 calc R . . H16C H 0.2103 1.0192 0.603 0.087 Uiso 1 1 calc R . . C17 C -0.00462(16) 1.0983(2) 0.38935(18) 0.0677(9) Uani 1 1 d . . . H17A H -0.031 1.0715 0.4249 0.102 Uiso 1 1 calc R . . H17B H -0.0332 1.0859 0.3376 0.102 Uiso 1 1 calc R . . H17C H -0.0007 1.163 0.3974 0.102 Uiso 1 1 calc R . . C18 C 0.19874(16) 0.9513(2) 0.28682(14) 0.0568(7) Uani 1 1 d . . . H18A H 0.251 0.9708 0.29 0.085 Uiso 1 1 calc R . . H18B H 0.1654 0.9735 0.2399 0.085 Uiso 1 1 calc R . . H18C H 0.1969 0.8859 0.2874 0.085 Uiso 1 1 calc R . . C19 C 0.50307(12) 0.75115(14) 0.46488(13) 0.0325(5) Uani 1 1 d . . . C20 C 0.54942(13) 0.74571(14) 0.53803(13) 0.0378(6) Uani 1 1 d . . . C21 C 0.62768(13) 0.74617(15) 0.54781(15) 0.0426(6) Uani 1 1 d . . . H21 H 0.6592 0.743 0.5975 0.051 Uiso 1 1 calc R . . C22 C 0.66132(14) 0.75105(15) 0.48772(16) 0.0462(6) Uani 1 1 d . . . C23 C 0.61451(14) 0.75582(16) 0.41565(16) 0.0487(7) Uani 1 1 d . . . H23 H 0.6368 0.759 0.3737 0.058 Uiso 1 1 calc R . . C24 C 0.53536(13) 0.75600(15) 0.40303(14) 0.0400(6) Uani 1 1 d . . . C25 C 0.51552(16) 0.73881(19) 0.60590(15) 0.0573(8) Uani 1 1 d . . . H25A H 0.4817 0.7897 0.6064 0.086 Uiso 1 1 calc R . . H25B H 0.5564 0.739 0.6521 0.086 Uiso 1 1 calc R . . H25C H 0.4865 0.6832 0.603 0.086 Uiso 1 1 calc R . . C26 C 0.74683(15) 0.75092(18) 0.5008(2) 0.0677(9) Uani 1 1 d . . . H26A H 0.7606 0.7495 0.4522 0.101 Uiso 1 1 calc R . . H26B H 0.7677 0.6982 0.5304 0.101 Uiso 1 1 calc R . . H26C H 0.7676 0.805 0.5284 0.101 Uiso 1 1 calc R . . C27 C 0.48607(16) 0.76066(19) 0.32372(15) 0.0590(8) Uani 1 1 d . . . H27A H 0.4569 0.7052 0.312 0.089 Uiso 1 1 calc R . . H27B H 0.5183 0.7686 0.2881 0.089 Uiso 1 1 calc R . . H27C H 0.451 0.8112 0.3195 0.089 Uiso 1 1 calc R . . C28 C 0.22383(12) 0.51689(14) 0.44041(13) 0.0353(5) Uani 1 1 d . . . C29 C 0.17511(13) 0.50296(15) 0.36944(13) 0.0398(6) Uani 1 1 d . . . C30 C 0.10715(14) 0.45773(17) 0.36443(15) 0.0489(7) Uani 1 1 d . . . H30 H 0.0752 0.4459 0.316 0.059 Uiso 1 1 calc R . . C31 C 0.08438(15) 0.42933(17) 0.42788(16) 0.0513(7) Uani 1 1 d . . . C32 C 0.13267(15) 0.44493(17) 0.49740(16) 0.0509(7) Uani 1 1 d . . . H32 H 0.1176 0.4266 0.5414 0.061 Uiso 1 1 calc R . . C33 C 0.20309(14) 0.48687(15) 0.50545(14) 0.0421(6) Uani 1 1 d . . . C34 C 0.19441(15) 0.53928(19) 0.29949(14) 0.0549(7) Uani 1 1 d . . . H34A H 0.1855 0.6039 0.2966 0.082 Uiso 1 1 calc R . . H34B H 0.1623 0.5104 0.2549 0.082 Uiso 1 1 calc R . . H34C H 0.248 0.5272 0.3014 0.082 Uiso 1 1 calc R . . C35 C 0.00856(17) 0.3843(2) 0.4212(2) 0.0785(10) Uani 1 1 d . . . H35A H 0.0166 0.3208 0.4335 0.118 Uiso 1 1 calc R . . H35B H -0.0224 0.3907 0.3695 0.118 Uiso 1 1 calc R . . H35C H -0.0177 0.4123 0.4564 0.118 Uiso 1 1 calc R . . C36 C 0.25581(17) 0.4978(2) 0.58260(15) 0.0642(8) Uani 1 1 d . . . H36A H 0.2956 0.452 0.5901 0.096 Uiso 1 1 calc R . . H36B H 0.2269 0.4912 0.6212 0.096 Uiso 1 1 calc R . . H36C H 0.2792 0.5571 0.5866 0.096 Uiso 1 1 calc R . . C37 C 0.05196(13) 0.75138(16) 0.36015(14) 0.0430(6) Uani 1 1 d . . . C38 C 0.03150(16) 0.7879(2) 0.27994(16) 0.0651(8) Uani 1 1 d . . . H38A H 0.0513 0.8487 0.2797 0.098 Uiso 1 1 calc R . . H38B H -0.0239 0.7886 0.2611 0.098 Uiso 1 1 calc R . . H38C H 0.0539 0.7498 0.2474 0.098 Uiso 1 1 calc R . . C39 C 0.01853(16) 0.6586(2) 0.36090(18) 0.0696(9) Uani 1 1 d . . . H39A H 0.0356 0.6206 0.3245 0.104 Uiso 1 1 calc R . . H39B H -0.0371 0.6624 0.3472 0.104 Uiso 1 1 calc R . . H39C H 0.0355 0.6329 0.4115 0.104 Uiso 1 1 calc R . . C40 C 0.01973(17) 0.8134(2) 0.41043(17) 0.0672(8) Uani 1 1 d . . . H40A H 0.0291 0.7881 0.4613 0.101 Uiso 1 1 calc R . . H40B H -0.0351 0.8202 0.3898 0.101 Uiso 1 1 calc R . . H40C H 0.0444 0.8719 0.4126 0.101 Uiso 1 1 calc R . . C41 C 0.30492(14) 0.75635(17) 0.61271(14) 0.0481(7) Uani 1 1 d . . . H41A H 0.3323 0.812 0.6065 0.058 Uiso 1 1 calc R . . H41B H 0.3379 0.7047 0.6089 0.058 Uiso 1 1 calc R . . C42 C 0.2837(2) 0.7560(3) 0.68706(18) 0.0891(13) Uani 1 1 d . . . H42A H 0.2964 0.6978 0.7127 0.107 Uiso 1 1 calc R . . H42B H 0.3111 0.8037 0.7202 0.107 Uiso 1 1 calc R . . C43 C 0.2021(2) 0.7715(3) 0.66968(18) 0.0917(12) Uani 1 1 d . . . H43A H 0.1784 0.736 0.7037 0.11 Uiso 1 1 calc R . . H43B H 0.1913 0.8355 0.6761 0.11 Uiso 1 1 calc R . . C44 C 0.17259(16) 0.7450(3) 0.59328(17) 0.0798(11) Uani 1 1 d . . . H44A H 0.1304 0.7849 0.5685 0.096 Uiso 1 1 calc R . . H44B H 0.153 0.6831 0.5912 0.096 Uiso 1 1 calc R . . C45 C 0.27290(18) 0.3291(2) 0.24852(19) 0.0803(10) Uani 1 1 d DU . . H45A H 0.2845 0.3746 0.2136 0.096 Uiso 0.534(13) 1 calc PR A 1 H45B H 0.2799 0.3562 0.2991 0.096 Uiso 0.534(13) 1 calc PR A 1 H45C H 0.2695 0.3625 0.2011 0.096 Uiso 0.466(13) 1 calc PR A 2 H45D H 0.2931 0.3696 0.2915 0.096 Uiso 0.466(13) 1 calc PR A 2 C46A C 0.1936(3) 0.2961(5) 0.2209(11) 0.100(5) Uani 0.534(13) 1 d PDU A 1 H46A H 0.1792 0.29 0.1653 0.121 Uiso 0.534(13) 1 calc PR A 1 H46B H 0.1565 0.335 0.2373 0.121 Uiso 0.534(13) 1 calc PR A 1 C47A C 0.2012(4) 0.2046(5) 0.2606(7) 0.102(4) Uani 0.534(13) 1 d PDU A 1 H47A H 0.2003 0.2101 0.3143 0.123 Uiso 0.534(13) 1 calc PR A 1 H47B H 0.161 0.1626 0.235 0.123 Uiso 0.534(13) 1 calc PR A 1 C46B C 0.1964(4) 0.2954(5) 0.2518(14) 0.119(8) Uani 0.466(13) 1 d PDU A 2 H46C H 0.1553 0.3327 0.2211 0.143 Uiso 0.466(13) 1 calc PR A 2 H46D H 0.1908 0.2928 0.3044 0.143 Uiso 0.466(13) 1 calc PR A 2 C47B C 0.1973(3) 0.2012(5) 0.2179(6) 0.080(3) Uani 0.466(13) 1 d PDU A 2 H47C H 0.1615 0.1603 0.2344 0.096 Uiso 0.466(13) 1 calc PR A 2 H47D H 0.1857 0.2027 0.1621 0.096 Uiso 0.466(13) 1 calc PR A 2 C48 C 0.2785(2) 0.1764(3) 0.2516(2) 0.0942(12) Uani 1 1 d DU . . H48A H 0.3037 0.1369 0.2937 0.113 Uiso 0.534(13) 1 calc PR A 1 H48B H 0.2736 0.1437 0.2036 0.113 Uiso 0.534(13) 1 calc PR A 1 H48C H 0.2846 0.1538 0.3036 0.113 Uiso 0.466(13) 1 calc PR A 2 H48D H 0.2954 0.1295 0.2211 0.113 Uiso 0.466(13) 1 calc PR A 2 C49 C 0.5379(3) 1.0196(3) 0.3312(2) 0.1115(14) Uani 1 1 d D . . H49A H 0.5409 1.0586 0.3756 0.134 Uiso 1 1 calc R . . H49B H 0.5467 0.9571 0.3489 0.134 Uiso 1 1 calc R . . C50 C 0.4621(2) 1.0281(3) 0.2778(2) 0.1003(13) Uani 1 1 d D . . H50A H 0.442 1.0895 0.2776 0.12 Uiso 1 1 calc R . . H50B H 0.4251 0.9856 0.2902 0.12 Uiso 1 1 calc R . . C51 C 0.4797(2) 1.0052(3) 0.2022(2) 0.1048(13) Uani 1 1 d D . . H51A H 0.4571 0.9472 0.1826 0.126 Uiso 1 1 calc R . . H51B H 0.4612 1.0523 0.1642 0.126 Uiso 1 1 calc R . . C52 C 0.5639(3) 1.0009(4) 0.2231(2) 0.136(2) Uani 1 1 d D . . H52A H 0.5807 0.9378 0.2272 0.163 Uiso 1 1 calc R . . H52B H 0.5846 1.0301 0.1837 0.163 Uiso 1 1 calc R . . Mg Mg 0.22689(4) 0.74899(5) 0.44245(4) 0.0320(2) Uani 1 1 d . . . N1 N 0.30448(9) 0.84899(11) 0.43855(10) 0.0320(4) Uani 1 1 d . . . N2 N 0.30622(9) 0.64986(11) 0.44275(10) 0.0310(4) Uani 1 1 d . . . O1 O 0.13079(9) 0.74723(11) 0.38495(12) 0.0581(5) Uani 1 1 d . . . O2 O 0.23341(9) 0.75056(11) 0.55572(9) 0.0433(4) Uani 1 1 d . . . O3 O 0.32108(12) 0.25457(17) 0.25181(12) 0.0773(7) Uani 1 1 d DU A . O4 O 0.59122(19) 1.0447(3) 0.2930(2) 0.1504(14) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0377(13) 0.0241(13) 0.0456(14) 0.0001(10) 0.0125(11) 0.0022(10) C2 0.0420(15) 0.0237(12) 0.0699(17) -0.0010(12) 0.0141(12) -0.0025(11) C3 0.0315(13) 0.0304(13) 0.0569(15) -0.0001(11) 0.0105(11) -0.0047(11) C4 0.0272(12) 0.0293(13) 0.0402(12) 0.0003(10) 0.0086(9) -0.0009(10) C5 0.0264(11) 0.0314(12) 0.0335(12) 0.0001(10) 0.0069(9) -0.0015(10) C6 0.0276(12) 0.0269(13) 0.0398(12) 0.0003(10) 0.0087(9) 0.0013(10) C7 0.0300(12) 0.0294(13) 0.0580(15) 0.0004(11) 0.0089(11) 0.0039(11) C8 0.0372(14) 0.0253(13) 0.0668(17) 0.0035(11) 0.0105(12) 0.0037(11) C9 0.0341(13) 0.0272(13) 0.0408(13) 0.0003(10) 0.0087(10) -0.0015(10) C10 0.0351(13) 0.0222(12) 0.0492(14) 0.0030(10) 0.0107(11) 0.0026(10) C11 0.0448(15) 0.0282(13) 0.0472(14) -0.0022(11) 0.0107(11) 0.0036(11) C12 0.0486(15) 0.0340(14) 0.0575(16) -0.0040(12) 0.0218(13) 0.0077(12) C13 0.0406(14) 0.0342(14) 0.0646(17) 0.0052(12) 0.0152(13) 0.0107(11) C14 0.0429(15) 0.0448(16) 0.0524(15) 0.0095(12) 0.0062(12) 0.0098(12) C15 0.0426(14) 0.0346(14) 0.0496(15) 0.0027(11) 0.0145(12) 0.0056(11) C16 0.0665(19) 0.0551(18) 0.0504(16) -0.0058(13) 0.0105(14) 0.0142(15) C17 0.0530(18) 0.064(2) 0.087(2) 0.0055(17) 0.0192(16) 0.0229(15) C18 0.0559(17) 0.0656(19) 0.0505(16) 0.0028(14) 0.0159(13) 0.0125(14) C19 0.0275(12) 0.0234(11) 0.0469(13) 0.0006(10) 0.0094(10) 0.0013(10) C20 0.0315(12) 0.0313(13) 0.0497(14) -0.0005(11) 0.0079(11) 0.0002(10) C21 0.0313(13) 0.0336(14) 0.0587(16) 0.0010(12) 0.0028(11) -0.0004(11) C22 0.0308(13) 0.0296(13) 0.0776(19) -0.0009(13) 0.0122(13) -0.0004(11) C23 0.0400(15) 0.0459(16) 0.0672(18) 0.0001(13) 0.0266(14) -0.0005(12) C24 0.0357(13) 0.0356(14) 0.0503(14) 0.0004(11) 0.0137(11) -0.0011(11) C25 0.0434(16) 0.082(2) 0.0437(15) 0.0023(14) 0.0050(12) -0.0022(14) C26 0.0305(14) 0.0605(19) 0.113(3) 0.0012(17) 0.0193(16) 0.0020(13) C27 0.0513(17) 0.080(2) 0.0500(16) 0.0028(14) 0.0194(13) 0.0004(15) C28 0.0343(13) 0.0241(12) 0.0484(14) -0.0010(10) 0.0116(11) 0.0000(10) C29 0.0378(14) 0.0313(13) 0.0513(15) -0.0038(11) 0.0127(11) -0.0042(11) C30 0.0417(15) 0.0433(15) 0.0607(17) -0.0129(13) 0.0109(13) -0.0103(12) C31 0.0462(15) 0.0379(15) 0.0747(19) -0.0095(13) 0.0243(14) -0.0120(12) C32 0.0577(17) 0.0379(15) 0.0667(18) 0.0010(13) 0.0334(15) -0.0095(13) C33 0.0476(15) 0.0294(13) 0.0508(15) 0.0007(11) 0.0146(12) -0.0024(11) C34 0.0547(17) 0.0595(18) 0.0483(15) -0.0003(13) 0.0083(13) -0.0092(14) C35 0.060(2) 0.073(2) 0.110(3) -0.0155(19) 0.0377(19) -0.0317(17) C36 0.074(2) 0.064(2) 0.0555(17) 0.0056(14) 0.0173(15) -0.0158(16) C37 0.0269(12) 0.0436(15) 0.0540(15) -0.0041(12) 0.0009(11) -0.0001(11) C38 0.0489(17) 0.082(2) 0.0618(18) 0.0017(16) 0.0079(14) 0.0039(16) C39 0.0550(19) 0.057(2) 0.090(2) 0.0009(16) 0.0049(16) -0.0046(15) C40 0.0613(19) 0.067(2) 0.070(2) -0.0133(16) 0.0104(15) 0.0087(16) C41 0.0293(13) 0.0586(17) 0.0520(15) 0.0008(13) 0.0011(11) -0.0023(12) C42 0.062(2) 0.152(4) 0.0479(18) 0.0040(19) 0.0033(15) -0.018(2) C43 0.082(3) 0.143(4) 0.057(2) 0.001(2) 0.0304(18) 0.008(2) C44 0.0365(16) 0.152(4) 0.0566(19) -0.0096(19) 0.0231(14) -0.0037(18) C45 0.062(2) 0.086(2) 0.084(2) 0.0214(19) 0.0001(17) -0.0045(18) C46A 0.055(4) 0.070(7) 0.169(14) -0.019(5) 0.012(5) -0.005(4) C47A 0.070(5) 0.101(7) 0.123(9) 0.020(6) -0.001(5) -0.027(4) C46B 0.048(5) 0.108(11) 0.20(2) -0.040(9) 0.017(6) 0.009(5) C47B 0.053(4) 0.097(7) 0.082(7) 0.004(5) 0.003(4) -0.009(4) C48 0.074(2) 0.085(3) 0.106(3) -0.035(2) -0.012(2) 0.002(2) C49 0.126(4) 0.109(3) 0.102(3) -0.002(3) 0.031(3) -0.021(3) C50 0.093(3) 0.099(3) 0.116(3) 0.017(2) 0.038(3) 0.020(2) C51 0.103(3) 0.110(3) 0.094(3) -0.001(2) 0.009(2) 0.022(3) C52 0.113(4) 0.222(6) 0.070(3) 0.018(3) 0.017(3) 0.073(4) Mg 0.0250(4) 0.0284(4) 0.0422(4) -0.0011(3) 0.0073(3) 0.0005(3) N1 0.0284(10) 0.0265(10) 0.0414(11) 0.0006(8) 0.0093(8) 0.0022(8) N2 0.0270(10) 0.0260(10) 0.0403(10) 0.0005(8) 0.0088(8) -0.0020(8) O1 0.0282(9) 0.0592(12) 0.0781(13) -0.0029(9) -0.0043(9) 0.0003(8) O2 0.0274(8) 0.0615(11) 0.0420(9) -0.0048(8) 0.0100(7) -0.0032(8) O3 0.0462(12) 0.115(2) 0.0673(14) -0.0045(12) 0.0069(10) 0.0031(13) O4 0.114(2) 0.188(4) 0.128(3) 0.061(3) -0.013(2) -0.049(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.343(3) . ? C1 C2 1.415(3) . ? C1 C10 1.490(3) . ? C2 C3 1.372(3) . ? C2 H2 0.95 . ? C3 C4 1.418(3) . ? C3 H3 0.95 . ? C4 N1 1.400(3) . ? C4 C5 1.404(3) . ? C5 C6 1.401(3) . ? C5 C19 1.509(3) . ? C6 N2 1.402(3) . ? C6 C7 1.418(3) . ? C7 C8 1.365(3) . ? C7 H7 0.95 . ? C8 C9 1.417(3) . ? C8 H8 0.95 . ? C9 N2 1.342(3) . ? C9 C28 1.487(3) . ? C10 C15 1.396(3) . ? C10 C11 1.405(3) . ? C11 C12 1.394(3) . ? C11 C16 1.508(3) . ? C12 C13 1.388(4) . ? C12 H12 0.95 . ? C13 C14 1.383(3) . ? C13 C17 1.506(3) . ? C14 C15 1.390(3) . ? C14 H14 0.95 . ? C15 C18 1.507(3) . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 C24 1.394(3) . ? C19 C20 1.399(3) . ? C20 C21 1.386(3) . ? C20 C25 1.514(4) . ? C21 C22 1.380(4) . ? C21 H21 0.95 . ? C22 C23 1.385(4) . ? C22 C26 1.510(3) . ? C23 C24 1.397(3) . ? C23 H23 0.95 . ? C24 C27 1.509(4) . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C28 C29 1.397(3) . ? C28 C33 1.404(3) . ? C29 C30 1.389(3) . ? C29 C34 1.506(3) . ? C30 C31 1.387(4) . ? C30 H30 0.95 . ? C31 C32 1.377(4) . ? C31 C35 1.509(4) . ? C32 C33 1.398(3) . ? C32 H32 0.95 . ? C33 C36 1.508(3) . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 O1 1.392(3) . ? C37 C39 1.517(4) . ? C37 C40 1.519(4) . ? C37 C38 1.524(4) . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? C39 H39A 0.98 . ? C39 H39B 0.98 . ? C39 H39C 0.98 . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? C41 O2 1.456(3) . ? C41 C42 1.498(4) . ? C41 H41A 0.99 . ? C41 H41B 0.99 . ? C42 C43 1.455(5) . ? C42 H42A 0.99 . ? C42 H42B 0.99 . ? C43 C44 1.425(4) . ? C43 H43A 0.99 . ? C43 H43B 0.99 . ? C44 O2 1.434(3) . ? C44 H44A 0.99 . ? C44 H44B 0.99 . ? C45 O3 1.409(4) . ? C45 C46A 1.488(7) . ? C45 C46B 1.489(7) . ? C45 H45A 0.99 . ? C45 H45B 0.99 . ? C45 H45C 0.99 . ? C45 H45D 0.99 . ? C46A C47A 1.541(10) . ? C46A H46A 0.99 . ? C46A H46B 0.99 . ? C47A C48 1.509(7) . ? C47A H47A 0.99 . ? C47A H47B 0.99 . ? C46B C47B 1.543(10) . ? C46B H46C 0.99 . ? C46B H46D 0.99 . ? C47B C48 1.498(6) . ? C47B H47C 0.99 . ? C47B H47D 0.99 . ? C48 O3 1.401(4) . ? C48 H48A 0.99 . ? C48 H48B 0.99 . ? C48 H48C 0.99 . ? C48 H48D 0.99 . ? C49 O4 1.374(4) . ? C49 C50 1.486(5) . ? C49 H49A 0.99 . ? C49 H49B 0.99 . ? C50 C51 1.528(5) . ? C50 H50A 0.99 . ? C50 H50B 0.99 . ? C51 C52 1.483(5) . ? C51 H51A 0.99 . ? C51 H51B 0.99 . ? C52 O4 1.415(5) . ? C52 H52A 0.99 . ? C52 H52B 0.99 . ? Mg O1 1.8039(18) . ? Mg O2 2.0441(17) . ? Mg N2 2.0659(18) . ? Mg N1 2.0672(18) . ? 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 C1 C2 111.11(19) . . ? N1 C1 C10 122.03(19) . . ? C2 C1 C10 126.8(2) . . ? C3 C2 C1 106.5(2) . . ? C3 C2 H2 126.7 . . ? C1 C2 H2 126.7 . . ? C2 C3 C4 107.3(2) . . ? C2 C3 H3 126.4 . . ? C4 C3 H3 126.4 . . ? N1 C4 C5 125.25(19) . . ? N1 C4 C3 108.69(18) . . ? C5 C4 C3 126.0(2) . . ? C6 C5 C4 128.3(2) . . ? C6 C5 C19 115.87(18) . . ? C4 C5 C19 115.86(18) . . ? C5 C6 N2 125.39(19) . . ? C5 C6 C7 125.9(2) . . ? N2 C6 C7 108.65(18) . . ? C8 C7 C6 107.5(2) . . ? C8 C7 H7 126.3 . . ? C6 C7 H7 126.3 . . ? C7 C8 C9 106.5(2) . . ? C7 C8 H8 126.7 . . ? C9 C8 H8 126.7 . . ? N2 C9 C8 111.17(19) . . ? N2 C9 C28 122.66(19) . . ? C8 C9 C28 126.2(2) . . ? C15 C10 C11 119.9(2) . . ? C15 C10 C1 119.7(2) . . ? C11 C10 C1 120.3(2) . . ? C12 C11 C10 118.7(2) . . ? C12 C11 C16 120.0(2) . . ? C10 C11 C16 121.2(2) . . ? C13 C12 C11 122.0(2) . . ? C13 C12 H12 119 . . ? C11 C12 H12 119 . . ? C14 C13 C12 117.9(2) . . ? C14 C13 C17 121.3(2) . . ? C12 C13 C17 120.7(2) . . ? C13 C14 C15 122.0(2) . . ? C13 C14 H14 119 . . ? C15 C14 H14 119 . . ? C14 C15 C10 119.3(2) . . ? C14 C15 C18 120.2(2) . . ? C10 C15 C18 120.6(2) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 120.3(2) . . ? C24 C19 C5 120.4(2) . . ? C20 C19 C5 119.3(2) . . ? C21 C20 C19 118.9(2) . . ? C21 C20 C25 120.0(2) . . ? C19 C20 C25 121.2(2) . . ? C22 C21 C20 122.2(2) . . ? C22 C21 H21 118.9 . . ? C20 C21 H21 118.9 . . ? C21 C22 C23 118.2(2) . . ? C21 C22 C26 120.5(3) . . ? C23 C22 C26 121.4(3) . . ? C22 C23 C24 121.7(2) . . ? C22 C23 H23 119.1 . . ? C24 C23 H23 119.1 . . ? C19 C24 C23 118.8(2) . . ? C19 C24 C27 120.9(2) . . ? C23 C24 C27 120.3(2) . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C33 120.0(2) . . ? C29 C28 C9 120.1(2) . . ? C33 C28 C9 119.9(2) . . ? C30 C29 C28 119.0(2) . . ? C30 C29 C34 120.3(2) . . ? C28 C29 C34 120.6(2) . . ? C31 C30 C29 122.2(2) . . ? C31 C30 H30 118.9 . . ? C29 C30 H30 118.9 . . ? C32 C31 C30 117.9(2) . . ? C32 C31 C35 120.9(3) . . ? C30 C31 C35 121.2(3) . . ? C31 C32 C33 122.3(2) . . ? C31 C32 H32 118.9 . . ? C33 C32 H32 118.9 . . ? C32 C33 C28 118.6(2) . . ? C32 C33 C36 120.2(2) . . ? C28 C33 C36 121.2(2) . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C35 H35A 109.5 . . ? C31 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C31 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O1 C37 C39 109.7(2) . . ? O1 C37 C40 110.2(2) . . ? C39 C37 C40 110.0(2) . . ? O1 C37 C38 108.8(2) . . ? C39 C37 C38 109.4(2) . . ? C40 C37 C38 108.8(2) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O2 C41 C42 105.6(2) . . ? O2 C41 H41A 110.6 . . ? C42 C41 H41A 110.6 . . ? O2 C41 H41B 110.6 . . ? C42 C41 H41B 110.6 . . ? H41A C41 H41B 108.7 . . ? C43 C42 C41 105.7(3) . . ? C43 C42 H42A 110.6 . . ? C41 C42 H42A 110.6 . . ? C43 C42 H42B 110.6 . . ? C41 C42 H42B 110.6 . . ? H42A C42 H42B 108.7 . . ? C44 C43 C42 106.8(3) . . ? C44 C43 H43A 110.4 . . ? C42 C43 H43A 110.4 . . ? C44 C43 H43B 110.4 . . ? C42 C43 H43B 110.4 . . ? H43A C43 H43B 108.6 . . ? C43 C44 O2 107.6(3) . . ? C43 C44 H44A 110.2 . . ? O2 C44 H44A 110.2 . . ? C43 C44 H44B 110.2 . . ? O2 C44 H44B 110.2 . . ? H44A C44 H44B 108.5 . . ? O3 C45 C46A 106.8(4) . . ? O3 C45 C46B 107.7(4) . . ? O3 C45 H45A 110.4 . . ? C46A C45 H45A 110.4 . . ? O3 C45 H45B 110.4 . . ? C46A C45 H45B 110.4 . . ? H45A C45 H45B 108.6 . . ? O3 C45 H45C 110.2 . . ? C46B C45 H45C 110.2 . . ? O3 C45 H45D 110.2 . . ? C46B C45 H45D 110.2 . . ? H45C C45 H45D 108.5 . . ? C45 C46A C47A 99.6(7) . . ? C45 C46A H46A 111.9 . . ? C47A C46A H46A 111.9 . . ? C45 C46A H46B 111.9 . . ? C47A C46A H46B 111.9 . . ? H46A C46A H46B 109.6 . . ? C48 C47A C46A 100.2(5) . . ? C48 C47A H47A 111.7 . . ? C46A C47A H47A 111.7 . . ? C48 C47A H47B 111.7 . . ? C46A C47A H47B 111.7 . . ? H47A C47A H47B 109.5 . . ? C45 C46B C47B 101.1(7) . . ? C45 C46B H46C 111.5 . . ? C47B C46B H46C 111.5 . . ? C45 C46B H46D 111.5 . . ? C47B C46B H46D 111.5 . . ? H46C C46B H46D 109.4 . . ? C48 C47B C46B 99.5(5) . . ? C48 C47B H47C 111.9 . . ? C46B C47B H47C 111.9 . . ? C48 C47B H47D 111.9 . . ? C46B C47B H47D 111.9 . . ? H47C C47B H47D 109.6 . . ? O3 C48 C47B 106.3(4) . . ? O3 C48 C47A 106.9(4) . . ? O3 C48 H48A 110.3 . . ? C47A C48 H48A 110.3 . . ? O3 C48 H48B 110.3 . . ? C47A C48 H48B 110.3 . . ? H48A C48 H48B 108.6 . . ? O3 C48 H48C 110.5 . . ? C47B C48 H48C 110.5 . . ? O3 C48 H48D 110.5 . . ? C47B C48 H48D 110.5 . . ? H48C C48 H48D 108.7 . . ? O4 C49 C50 107.1(3) . . ? O4 C49 H49A 110.3 . . ? C50 C49 H49A 110.3 . . ? O4 C49 H49B 110.3 . . ? C50 C49 H49B 110.3 . . ? H49A C49 H49B 108.5 . . ? C49 C50 C51 102.3(3) . . ? C49 C50 H50A 111.3 . . ? C51 C50 H50A 111.3 . . ? C49 C50 H50B 111.3 . . ? C51 C50 H50B 111.3 . . ? H50A C50 H50B 109.2 . . ? C52 C51 C50 101.7(3) . . ? C52 C51 H51A 111.4 . . ? C50 C51 H51A 111.4 . . ? C52 C51 H51B 111.4 . . ? C50 C51 H51B 111.4 . . ? H51A C51 H51B 109.3 . . ? O4 C52 C51 109.0(3) . . ? O4 C52 H52A 109.9 . . ? C51 C52 H52A 109.9 . . ? O4 C52 H52B 109.9 . . ? C51 C52 H52B 109.9 . . ? H52A C52 H52B 108.3 . . ? O1 Mg O2 113.67(9) . . ? O1 Mg N2 124.36(8) . . ? O2 Mg N2 97.78(7) . . ? O1 Mg N1 124.03(8) . . ? O2 Mg N1 98.80(7) . . ? N2 Mg N1 92.41(7) . . ? C1 N1 C4 106.38(17) . . ? C1 N1 Mg 128.97(15) . . ? C4 N1 Mg 123.85(14) . . ? C9 N2 C6 106.18(17) . . ? C9 N2 Mg 129.21(14) . . ? C6 N2 Mg 123.88(14) . . ? C37 O1 Mg 163.66(19) . . ? C44 O2 C41 108.39(19) . . ? C44 O2 Mg 128.33(16) . . ? C41 O2 Mg 123.27(14) . . ? C48 O3 C45 109.0(3) . . ? C49 O4 C52 101.3(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 0.6(3) . . . . ? C10 C1 C2 C3 -177.8(2) . . . . ? C1 C2 C3 C4 -0.4(3) . . . . ? C2 C3 C4 N1 0.1(3) . . . . ? C2 C3 C4 C5 -178.5(2) . . . . ? N1 C4 C5 C6 -1.5(4) . . . . ? C3 C4 C5 C6 176.9(2) . . . . ? N1 C4 C5 C19 -179.87(19) . . . . ? C3 C4 C5 C19 -1.5(3) . . . . ? C4 C5 C6 N2 0.2(4) . . . . ? C19 C5 C6 N2 178.51(19) . . . . ? C4 C5 C6 C7 -176.5(2) . . . . ? C19 C5 C6 C7 1.9(3) . . . . ? C5 C6 C7 C8 176.6(2) . . . . ? N2 C6 C7 C8 -0.5(3) . . . . ? C6 C7 C8 C9 0.5(3) . . . . ? C7 C8 C9 N2 -0.3(3) . . . . ? C7 C8 C9 C28 179.4(2) . . . . ? N1 C1 C10 C15 -80.0(3) . . . . ? C2 C1 C10 C15 98.1(3) . . . . ? N1 C1 C10 C11 101.6(3) . . . . ? C2 C1 C10 C11 -80.2(3) . . . . ? C15 C10 C11 C12 1.9(3) . . . . ? C1 C10 C11 C12 -179.7(2) . . . . ? C15 C10 C11 C16 -177.5(2) . . . . ? C1 C10 C11 C16 0.8(3) . . . . ? C10 C11 C12 C13 -1.8(4) . . . . ? C16 C11 C12 C13 177.7(2) . . . . ? C11 C12 C13 C14 0.3(4) . . . . ? C11 C12 C13 C17 178.5(2) . . . . ? C12 C13 C14 C15 1.1(4) . . . . ? C17 C13 C14 C15 -177.1(3) . . . . ? C13 C14 C15 C10 -1.0(4) . . . . ? C13 C14 C15 C18 177.5(2) . . . . ? C11 C10 C15 C14 -0.6(4) . . . . ? C1 C10 C15 C14 -178.9(2) . . . . ? C11 C10 C15 C18 -179.0(2) . . . . ? C1 C10 C15 C18 2.7(3) . . . . ? C6 C5 C19 C24 94.8(2) . . . . ? C4 C5 C19 C24 -86.6(3) . . . . ? C6 C5 C19 C20 -84.3(3) . . . . ? C4 C5 C19 C20 94.2(2) . . . . ? C24 C19 C20 C21 0.7(3) . . . . ? C5 C19 C20 C21 179.80(19) . . . . ? C24 C19 C20 C25 -179.0(2) . . . . ? C5 C19 C20 C25 0.2(3) . . . . ? C19 C20 C21 C22 -0.6(3) . . . . ? C25 C20 C21 C22 179.0(2) . . . . ? C20 C21 C22 C23 0.2(3) . . . . ? C20 C21 C22 C26 -179.7(2) . . . . ? C21 C22 C23 C24 0.2(4) . . . . ? C26 C22 C23 C24 -180.0(2) . . . . ? C20 C19 C24 C23 -0.4(3) . . . . ? C5 C19 C24 C23 -179.5(2) . . . . ? C20 C19 C24 C27 179.2(2) . . . . ? C5 C19 C24 C27 0.1(3) . . . . ? C22 C23 C24 C19 -0.1(3) . . . . ? C22 C23 C24 C27 -179.6(2) . . . . ? N2 C9 C28 C29 80.0(3) . . . . ? C8 C9 C28 C29 -99.7(3) . . . . ? N2 C9 C28 C33 -101.9(3) . . . . ? C8 C9 C28 C33 78.4(3) . . . . ? C33 C28 C29 C30 -1.3(3) . . . . ? C9 C28 C29 C30 176.9(2) . . . . ? C33 C28 C29 C34 176.5(2) . . . . ? C9 C28 C29 C34 -5.4(3) . . . . ? C28 C29 C30 C31 2.9(4) . . . . ? C34 C29 C30 C31 -174.8(2) . . . . ? C29 C30 C31 C32 -1.9(4) . . . . ? C29 C30 C31 C35 176.9(3) . . . . ? C30 C31 C32 C33 -0.8(4) . . . . ? C35 C31 C32 C33 -179.7(3) . . . . ? C31 C32 C33 C28 2.4(4) . . . . ? C31 C32 C33 C36 -176.5(3) . . . . ? C29 C28 C33 C32 -1.3(3) . . . . ? C9 C28 C33 C32 -179.4(2) . . . . ? C29 C28 C33 C36 177.6(2) . . . . ? C9 C28 C33 C36 -0.5(3) . . . . ? O2 C41 C42 C43 -13.3(4) . . . . ? C41 C42 C43 C44 23.0(4) . . . . ? C42 C43 C44 O2 -24.1(4) . . . . ? O3 C45 C46A C47A 36.7(13) . . . . ? C46B C45 C46A C47A -58.9(12) . . . . ? C45 C46A C47A C48 -39.8(13) . . . . ? O3 C45 C46B C47B -27.1(15) . . . . ? C46A C45 C46B C47B 64.0(13) . . . . ? C45 C46B C47B C48 38.0(15) . . . . ? C46B C47B C48 O3 -37.4(11) . . . . ? C46B C47B C48 C47A 58.4(10) . . . . ? C46A C47A C48 O3 31.1(11) . . . . ? C46A C47A C48 C47B -62.2(9) . . . . ? O4 C49 C50 C51 32.8(5) . . . . ? C49 C50 C51 C52 -8.2(4) . . . . ? C50 C51 C52 O4 -17.7(5) . . . . ? C2 C1 N1 C4 -0.5(3) . . . . ? C10 C1 N1 C4 177.92(19) . . . . ? C2 C1 N1 Mg 169.37(16) . . . . ? C10 C1 N1 Mg -12.2(3) . . . . ? C5 C4 N1 C1 178.8(2) . . . . ? C3 C4 N1 C1 0.2(2) . . . . ? C5 C4 N1 Mg 8.3(3) . . . . ? C3 C4 N1 Mg -170.28(14) . . . . ? O1 Mg N1 C1 46.3(2) . . . . ? O2 Mg N1 C1 -80.21(19) . . . . ? N2 Mg N1 C1 -178.47(18) . . . . ? O1 Mg N1 C4 -145.46(16) . . . . ? O2 Mg N1 C4 88.05(16) . . . . ? N2 Mg N1 C4 -10.21(17) . . . . ? C8 C9 N2 C6 0.0(2) . . . . ? C28 C9 N2 C6 -179.74(19) . . . . ? C8 C9 N2 Mg -170.27(15) . . . . ? C28 C9 N2 Mg 10.0(3) . . . . ? C5 C6 N2 C9 -176.8(2) . . . . ? C7 C6 N2 C9 0.3(2) . . . . ? C5 C6 N2 Mg -5.9(3) . . . . ? C7 C6 N2 Mg 171.23(14) . . . . ? O1 Mg N2 C9 -47.1(2) . . . . ? O2 Mg N2 C9 78.61(19) . . . . ? N1 Mg N2 C9 177.84(18) . . . . ? O1 Mg N2 C6 144.09(16) . . . . ? O2 Mg N2 C6 -90.15(16) . . . . ? N1 Mg N2 C6 9.07(17) . . . . ? C39 C37 O1 Mg -93.6(6) . . . . ? C40 C37 O1 Mg 27.7(7) . . . . ? C38 C37 O1 Mg 146.8(5) . . . . ? O2 Mg O1 C37 11.7(6) . . . . ? N2 Mg O1 C37 130.3(6) . . . . ? N1 Mg O1 C37 -108.1(6) . . . . ? C43 C44 O2 C41 15.6(4) . . . . ? C43 C44 O2 Mg -165.3(2) . . . . ? C42 C41 O2 C44 -1.2(3) . . . . ? C42 C41 O2 Mg 179.73(19) . . . . ? O1 Mg O2 C44 4.1(2) . . . . ? N2 Mg O2 C44 -128.9(2) . . . . ? N1 Mg O2 C44 137.5(2) . . . . ? O1 Mg O2 C41 -176.98(16) . . . . ? N2 Mg O2 C41 50.03(18) . . . . ? N1 Mg O2 C41 -43.65(18) . . . . ? C47B C48 O3 C45 21.9(6) . . . . ? C47A C48 O3 C45 -8.9(6) . . . . ? C46A C45 O3 C48 -18.4(9) . . . . ? C46B C45 O3 C48 4.1(10) . . . . ? C50 C49 O4 C52 -43.7(5) . . . . ? C51 C52 O4 C49 38.3(5) . . . . ? data_Chisholm1855 _database_code_depnum_ccdc_archive 'CCDC 888669' #TrackingRef '12207_web_deposit_cif_file_3_JudithGallucci_1340739962.archive-1855.cif' _audit_creation_date 2012-03-06T11:43:03-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Chisholm 1855' _chemical_formula_moiety 'C66 H100 Mg2 N4 O2, C6 H14' _chemical_formula_sum 'C72 H114 Mg2 N4 O2' _chemical_formula_weight 1116.29 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m _symmetry_space_group_name_Hall '-C 2y' _symmetry_Int_Tables_number 12 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 18.4898(3) _cell_length_b 18.3357(3) _cell_length_c 12.0991(2) _cell_angle_alpha 90 _cell_angle_beta 123.001(1) _cell_angle_gamma 90 _cell_volume 3440.08(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4057 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.078 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1228 _exptl_special_details ;All work was done at 150 K using an Oxford Cryosystems Cryostream Cooler. The data collection strategy was set up to measure a quadrant of reciprocal space with a redundancy factor of 4.3, which means that 90% of these reflections were measured at least 4.3 times. Phi and omega scans with a frame width of 1.0 degree were used. Data integration was done with Denzo, and scaling and merging of the data was done with Scalepack. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.08 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.837 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor, 1997)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.292668E-1 _diffrn_orient_matrix_ub_12 -0.458553E-1 _diffrn_orient_matrix_ub_13 -0.487542E-1 _diffrn_orient_matrix_ub_21 -0.573128E-1 _diffrn_orient_matrix_ub_22 0.21979E-1 _diffrn_orient_matrix_ub_23 -0.296432E-1 _diffrn_orient_matrix_ub_31 -0.41776E-2 _diffrn_orient_matrix_ub_32 0.197144E-1 _diffrn_orient_matrix_ub_33 -0.80353E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_av_unetI/netI ? _diffrn_reflns_number 34280 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 4063 _reflns_number_gt 2965 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ;The Mg dimer contains 2/m crystallographic symmetry so that the asymmetric unit consists of one fourth of the dimer, with the Mg, O and C(2) atoms lying on the mirror plane. The n-butyl chain appears to be disordered about this plane, with atoms C(16) and C(17) lying in the plane and atoms C(18) and C(19) disordered about the plane. Distance restraints were used in refining the n-butyl chain. There is also a molecule of n-hexane present and it also contains 2/m symmetry, with the two-fold rotation axis bisecting the molecule and all of the carbon atoms lying in a mirror plane. Thus there is one half of a molecule of hexane in the asymmetric unit. For the four methyl groups belonging to isopropyl groups, the hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5*Ueq(bonded atom). The torsion angle, which defines the orientation of the methyl group about the C-C bond, was allowed to refine. The methyl group of atom C(3) contains two different sets of hydrogen atoms related to each other by rotation of 60 degrees about the C(3)-C(1) bond. Each set has an occupancy factor of 0.5. The torsion angles for the C(19) methyl group of the n-butyl ligand and for the methyl group of the n-hexane molecule were not allowed to refine. The rest of the hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2*Ueq(bonded atom). 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^ > 2\s(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 'w=1/[\s^2^(Fo^2^)+(0.0895P)^2^+3.2471P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4063 _refine_ls_number_parameters 210 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0837 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1745 _refine_ls_wR_factor_gt 0.1595 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.651 _refine_diff_density_min -0.727 _refine_diff_density_rms 0.053 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.30661(11) 0.06944(10) 0.10078(17) 0.0272(4) Uani 1 1 d . . . C2 C 0.29542(17) 0 0.0447(2) 0.0295(6) Uani 1 2 d S . . H2 H 0.2775 0 -0.0453 0.035 Uiso 1 2 calc SR . . C3 C 0.26549(13) 0.13072(12) 0.00126(19) 0.0373(5) Uani 1 1 d . . . H3A H 0.2756 0.1772 0.0476 0.056 Uiso 0.5 1 calc PR . . H3B H 0.2033 0.1221 -0.0566 0.056 Uiso 0.5 1 calc PR . . H3C H 0.2909 0.1326 -0.0516 0.056 Uiso 0.5 1 calc PR . . H3D H 0.2376 0.1107 -0.088 0.056 Uiso 0.5 1 calc PR . . H3E H 0.3099 0.1658 0.0162 0.056 Uiso 0.5 1 calc PR . . H3F H 0.2223 0.1553 0.0112 0.056 Uiso 0.5 1 calc PR . . C4 C 0.34058(11) 0.15544(9) 0.26733(17) 0.0267(4) Uani 1 1 d . . . C5 C 0.27758(12) 0.17003(10) 0.29582(18) 0.0304(4) Uani 1 1 d . . . C6 C 0.26914(14) 0.24154(11) 0.3275(2) 0.0385(5) Uani 1 1 d . . . H6 H 0.226 0.2524 0.3448 0.046 Uiso 1 1 calc R . . C7 C 0.32210(15) 0.29647(11) 0.3340(2) 0.0415(5) Uani 1 1 d . . . H7 H 0.3156 0.3447 0.3561 0.05 Uiso 1 1 calc R . . C8 C 0.38475(14) 0.28123(11) 0.3083(2) 0.0382(5) Uani 1 1 d . . . H8 H 0.4217 0.3192 0.3145 0.046 Uiso 1 1 calc R . . C9 C 0.39486(12) 0.21128(10) 0.27336(18) 0.0312(4) Uani 1 1 d . . . C10 C 0.21705(13) 0.11070(11) 0.2860(2) 0.0358(5) Uani 1 1 d . . . H10 H 0.2474 0.063 0.3019 0.043 Uiso 1 1 calc R . . C11 C 0.19406(15) 0.11867(14) 0.3896(2) 0.0478(6) Uani 1 1 d . . . H11A H 0.2471 0.1239 0.4771 0.072 Uiso 1 1 calc R . . H11B H 0.1627 0.0752 0.3882 0.072 Uiso 1 1 calc R . . H11C H 0.1578 0.1619 0.3697 0.072 Uiso 1 1 calc R . . C12 C 0.13475(15) 0.10772(15) 0.1486(2) 0.0517(6) Uani 1 1 d . . . H12A H 0.1048 0.1547 0.1284 0.078 Uiso 1 1 calc R . . H12B H 0.0971 0.069 0.1456 0.078 Uiso 1 1 calc R . . H12C H 0.1494 0.0975 0.0836 0.078 Uiso 1 1 calc R . . C13 C 0.46276(13) 0.19726(11) 0.2417(2) 0.0351(5) Uani 1 1 d . . . H13 H 0.4521 0.1475 0.2018 0.042 Uiso 1 1 calc R . . C14 C 0.45882(17) 0.25188(14) 0.1423(3) 0.0541(6) Uani 1 1 d . . . H14A H 0.4004 0.2526 0.0629 0.081 Uiso 1 1 calc R . . H14B H 0.4998 0.2372 0.1188 0.081 Uiso 1 1 calc R . . H14C H 0.4738 0.3007 0.1818 0.081 Uiso 1 1 calc R . . C15 C 0.55230(14) 0.19732(16) 0.3669(2) 0.0554(7) Uani 1 1 d . . . H15A H 0.5642 0.2454 0.4089 0.083 Uiso 1 1 calc R . . H15B H 0.5951 0.1865 0.3453 0.083 Uiso 1 1 calc R . . H15C H 0.5554 0.1601 0.4275 0.083 Uiso 1 1 calc R . . C16 C 0.6022(3) 0 0.4090(5) 0.0849(14) Uani 1 2 d SD B . H16A H 0.6398 -0.0436 0.4433 0.102 Uiso 0.5 1 calc PR . . H16B H 0.6398 0.0436 0.4433 0.102 Uiso 0.5 1 calc PR . . C17 C 0.5559(3) 0 0.2664(4) 0.0790(13) Uani 1 2 d SD . . H17A H 0.5352 0.0501 0.2344 0.095 Uiso 0.25 1 calc PR A 1 H17B H 0.5046 -0.0317 0.2313 0.095 Uiso 0.25 1 calc PR A 1 H17C H 0.5181 0.0435 0.2336 0.095 Uiso 0.25 1 calc PR A 2 H17D H 0.5181 -0.0435 0.2336 0.095 Uiso 0.25 1 calc PR A 2 C18 C 0.6076(7) -0.0255(12) 0.2108(17) 0.190(19) Uani 0.25 1 d PD B 1 H18A H 0.609 -0.0795 0.2143 0.228 Uiso 0.25 1 calc PR B 1 H18B H 0.5751 -0.0116 0.1166 0.228 Uiso 0.25 1 calc PR B 1 C19 C 0.6970(7) 0 0.2708(12) 0.148(7) Uani 0.5 2 d SPD B 1 H19A H 0.7197 -0.0181 0.2192 0.223 Uiso 0.25 1 calc PR B 1 H19B H 0.7328 -0.0184 0.3613 0.223 Uiso 0.25 1 calc PR B 1 H19C H 0.6981 0.0534 0.2719 0.223 Uiso 0.25 1 calc PR B 1 C18A C 0.6081(14) 0 0.206(2) 0.202(18) Uiso 0.5 2 d SPD B 2 H18C H 0.5828 0.0359 0.1326 0.242 Uiso 0.25 1 calc PR B 2 H18D H 0.6673 0.0166 0.2724 0.242 Uiso 0.25 1 calc PR B 2 C19A C 0.614(2) -0.0714(10) 0.154(3) 0.238(16) Uiso 0.25 1 d PD B 2 H19D H 0.6498 -0.0669 0.1177 0.357 Uiso 0.25 1 calc PR B 2 H19E H 0.5556 -0.0873 0.0838 0.357 Uiso 0.25 1 calc PR B 2 H19F H 0.639 -0.1075 0.225 0.357 Uiso 0.25 1 calc PR B 2 Mg Mg 0.42281(5) 0 0.36320(8) 0.0233(2) Uani 1 2 d S . . N N 0.34752(9) 0.08224(8) 0.23021(14) 0.0248(3) Uani 1 1 d . . . O O 0.55257(15) 0 0.4519(2) 0.0478(6) Uani 1 2 d S . . C1A C 0.4487(3) 0.5 0.2023(4) 0.0659(11) Uani 1 2 d S . . H1A1 H 0.3946 0.5 0.1154 0.099 Uiso 1 2 calc SR . . H1A2 H 0.4822 0.4564 0.2114 0.099 Uiso 0.5 1 calc PR . . H1A3 H 0.4822 0.5436 0.2114 0.099 Uiso 0.5 1 calc PR . . C2A C 0.4292(2) 0.5 0.3078(3) 0.0485(8) Uani 1 2 d S . . H2A1 H 0.3942 0.4564 0.2965 0.058 Uiso 0.5 1 calc PR . . H2A2 H 0.3942 0.5436 0.2965 0.058 Uiso 0.5 1 calc PR . . C3A C 0.5094(2) 0.5 0.4463(4) 0.0558(9) Uani 1 2 d S . . H3A1 H 0.5443 0.4564 0.4573 0.067 Uiso 0.5 1 calc PR . . H3A2 H 0.5443 0.5436 0.4573 0.067 Uiso 0.5 1 calc PR . . 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 C1 0.0250(8) 0.0295(9) 0.0261(9) 0.0038(7) 0.0132(7) 0.0004(7) C2 0.0311(13) 0.0339(14) 0.0230(12) 0 0.0144(11) 0 C3 0.0393(11) 0.0354(11) 0.0289(9) 0.0073(8) 0.0133(9) 0.0035(9) C4 0.0293(9) 0.0220(9) 0.0245(8) 0.0040(7) 0.0120(7) 0.0035(7) C5 0.0321(9) 0.0273(10) 0.0297(9) 0.0054(8) 0.0155(8) 0.0063(8) C6 0.0448(12) 0.0317(11) 0.0416(11) 0.0035(9) 0.0253(10) 0.0103(9) C7 0.0576(13) 0.0242(10) 0.0427(11) 0.0026(9) 0.0274(11) 0.0075(9) C8 0.0496(12) 0.0245(10) 0.0374(10) 0.0025(8) 0.0217(10) -0.0032(9) C9 0.0358(10) 0.0267(9) 0.0271(9) 0.0053(7) 0.0145(8) 0.0016(8) C10 0.0356(10) 0.0330(10) 0.0460(11) 0.0021(9) 0.0268(9) 0.0044(8) C11 0.0504(13) 0.0513(14) 0.0541(13) 0.0023(11) 0.0365(12) -0.0005(11) C12 0.0421(12) 0.0619(16) 0.0516(13) -0.0066(12) 0.0259(11) -0.0112(11) C13 0.0362(10) 0.0307(10) 0.0383(11) 0.0026(8) 0.0203(9) -0.0050(8) C14 0.0644(15) 0.0526(15) 0.0577(14) 0.0136(12) 0.0413(13) -0.0004(12) C15 0.0370(12) 0.0736(18) 0.0498(13) -0.0005(13) 0.0199(11) -0.0079(12) C16 0.065(3) 0.111(4) 0.078(3) 0 0.038(3) 0 C17 0.056(2) 0.070(3) 0.080(3) 0 0.018(2) 0 C18 0.082(11) 0.083(13) 0.44(6) -0.085(18) 0.16(2) -0.029(9) C19 0.088(8) 0.28(2) 0.087(8) 0 0.055(7) 0 Mg 0.0232(4) 0.0210(4) 0.0232(4) 0 0.0111(3) 0 N 0.0244(7) 0.0235(8) 0.0254(7) 0.0012(6) 0.0127(6) 0.0010(6) O 0.0495(13) 0.0406(12) 0.0304(10) 0 0.0070(10) 0 C1A 0.051(2) 0.084(3) 0.059(2) 0 0.0281(19) 0 C2A 0.0459(18) 0.0393(17) 0.0507(19) 0 0.0200(16) 0 C3A 0.0473(19) 0.061(2) 0.053(2) 0 0.0234(17) 0 #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N 1.338(2) . ? C1 C2 1.404(2) . ? C1 C3 1.514(3) . ? C2 C1 1.404(2) 6 ? C2 H2 0.95 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C3 H3D 0.98 . ? C3 H3E 0.98 . ? C3 H3F 0.98 . ? C4 C9 1.408(3) . ? C4 C5 1.409(3) . ? C4 N 1.443(2) . ? C5 C6 1.398(3) . ? C5 C10 1.518(3) . ? C6 C7 1.377(3) . ? C6 H6 0.95 . ? C7 C8 1.382(3) . ? C7 H7 0.95 . ? C8 C9 1.394(3) . ? C8 H8 0.95 . ? C9 C13 1.521(3) . ? C10 C12 1.525(3) . ? C10 C11 1.535(3) . ? C10 H10 1 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 C15 1.518(3) . ? C13 C14 1.536(3) . ? C13 H13 1 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 O 1.277(5) . ? C16 C17 1.449(6) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 C18A 1.500(9) . ? C17 C18 1.511(8) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? C17 H17C 0.99 . ? C17 H17D 0.99 . ? C18 C19 1.474(9) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C18A C19A 1.480(10) . ? C18A H18C 0.99 . ? C18A H18D 0.99 . ? C19A H19D 0.98 . ? C19A H19E 0.98 . ? C19A H19F 0.98 . ? Mg O 2.026(2) . ? Mg O 2.026(2) 5_656 ? Mg N 2.0883(15) 6 ? Mg N 2.0883(15) . ? Mg Mg 2.9688(16) 5_656 ? O Mg 2.026(2) 5_656 ? C1A C2A 1.504(5) . ? C1A H1A1 0.98 . ? C1A H1A2 0.98 . ? C1A H1A3 0.98 . ? C2A C3A 1.517(5) . ? C2A H2A1 0.99 . ? C2A H2A2 0.99 . ? C3A C3A 1.516(7) 5_666 ? C3A H3A1 0.99 . ? C3A H3A2 0.99 . ? 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 N C1 C2 124.43(17) . . ? N C1 C3 121.30(17) . . ? C2 C1 C3 114.25(17) . . ? C1 C2 C1 130.1(2) . 6 ? C1 C2 H2 114.9 . . ? C1 C2 H2 114.9 6 . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C3 H3D 109.5 . . ? H3A C3 H3D 141.1 . . ? H3B C3 H3D 56.3 . . ? H3C C3 H3D 56.3 . . ? C1 C3 H3E 109.5 . . ? H3A C3 H3E 56.3 . . ? H3B C3 H3E 141.1 . . ? H3C C3 H3E 56.3 . . ? H3D C3 H3E 109.5 . . ? C1 C3 H3F 109.5 . . ? H3A C3 H3F 56.3 . . ? H3B C3 H3F 56.3 . . ? H3C C3 H3F 141.1 . . ? H3D C3 H3F 109.5 . . ? H3E C3 H3F 109.5 . . ? C9 C4 C5 120.70(17) . . ? C9 C4 N 120.72(16) . . ? C5 C4 N 118.58(15) . . ? C6 C5 C4 118.39(18) . . ? C6 C5 C10 120.40(17) . . ? C4 C5 C10 121.14(16) . . ? C7 C6 C5 121.31(19) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C6 C7 C8 119.77(19) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C7 C8 C9 121.42(19) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C8 C9 C4 118.38(18) . . ? C8 C9 C13 119.80(17) . . ? C4 C9 C13 121.81(17) . . ? C5 C10 C12 111.52(17) . . ? C5 C10 C11 112.83(17) . . ? C12 C10 C11 109.74(17) . . ? C5 C10 H10 107.5 . . ? C12 C10 H10 107.5 . . ? C11 C10 H10 107.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C9 110.46(17) . . ? C15 C13 C14 110.00(18) . . ? C9 C13 C14 113.17(17) . . ? C15 C13 H13 107.7 . . ? C9 C13 H13 107.7 . . ? C14 C13 H13 107.7 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O C16 C17 113.3(4) . . ? O C16 H16A 108.9 . . ? C17 C16 H16A 108.9 . . ? O C16 H16B 108.9 . . ? C17 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? C16 C17 C18A 117.6(10) . . ? C16 C17 C18 115.0(7) . . ? C16 C17 H17A 108.5 . . ? C18 C17 H17A 108.5 . . ? C16 C17 H17B 108.5 . . ? C18 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? C16 C17 H17C 107.9 . . ? C18A C17 H17C 107.9 . . ? C16 C17 H17D 107.9 . . ? C18A C17 H17D 107.9 . . ? H17C C17 H17D 107.2 . . ? C19 C18 C17 119.6(10) . . ? C19 C18 H18A 107.4 . . ? C17 C18 H18A 107.4 . . ? C19 C18 H18B 107.4 . . ? C17 C18 H18B 107.4 . . ? H18A C18 H18B 106.9 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C19A C18A C17 114.8(11) . . ? C19A C18A H18C 108.6 . . ? C17 C18A H18C 108.6 . . ? C19A C18A H18D 108.6 . . ? C17 C18A H18D 108.6 . . ? H18C C18A H18D 107.5 . . ? C18A C19A H19D 109.5 . . ? C18A C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? C18A C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? O Mg O 85.77(11) . 5_656 ? O Mg N 120.55(6) . 6 ? O Mg N 120.37(6) 5_656 6 ? O Mg N 120.55(6) . . ? O Mg N 120.37(6) 5_656 . ? N Mg N 92.46(9) 6 . ? O Mg Mg 42.89(7) . 5_656 ? O Mg Mg 42.88(7) 5_656 5_656 ? N Mg Mg 133.77(4) 6 5_656 ? N Mg Mg 133.77(4) . 5_656 ? C1 N C4 115.99(14) . . ? C1 N Mg 119.33(12) . . ? C4 N Mg 124.53(11) . . ? C16 O Mg 133.7(3) . . ? C16 O Mg 132.1(3) . 5_656 ? Mg O Mg 94.23(11) . 5_656 ? C2A C1A H1A1 109.5 . . ? C2A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? C2A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? C1A C2A C3A 113.3(3) . . ? C1A C2A H2A1 108.9 . . ? C3A C2A H2A1 108.9 . . ? C1A C2A H2A2 108.9 . . ? C3A C2A H2A2 108.9 . . ? H2A1 C2A H2A2 107.7 . . ? C3A C3A C2A 113.9(4) 5_666 . ? C3A C3A H3A1 108.8 5_666 . ? C2A C3A H3A1 108.8 . . ? C3A C3A H3A2 108.8 5_666 . ? C2A C3A H3A2 108.8 . . ? H3A1 C3A H3A2 107.7 . . ? 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 N C1 C2 C1 14.1(4) . . . 6 ? C3 C1 C2 C1 -164.1(2) . . . 6 ? C9 C4 C5 C6 1.3(3) . . . . ? N C4 C5 C6 -177.90(16) . . . . ? C9 C4 C5 C10 178.29(17) . . . . ? N C4 C5 C10 -0.9(3) . . . . ? C4 C5 C6 C7 -1.5(3) . . . . ? C10 C5 C6 C7 -178.50(19) . . . . ? C5 C6 C7 C8 0.3(3) . . . . ? C6 C7 C8 C9 1.1(3) . . . . ? C7 C8 C9 C4 -1.3(3) . . . . ? C7 C8 C9 C13 178.10(18) . . . . ? C5 C4 C9 C8 0.0(3) . . . . ? N C4 C9 C8 179.25(16) . . . . ? C5 C4 C9 C13 -179.34(16) . . . . ? N C4 C9 C13 -0.1(3) . . . . ? C6 C5 C10 C12 86.6(2) . . . . ? C4 C5 C10 C12 -90.3(2) . . . . ? C6 C5 C10 C11 -37.4(3) . . . . ? C4 C5 C10 C11 145.65(18) . . . . ? C8 C9 C13 C15 74.0(2) . . . . ? C4 C9 C13 C15 -106.6(2) . . . . ? C8 C9 C13 C14 -49.8(3) . . . . ? C4 C9 C13 C14 129.6(2) . . . . ? O C16 C17 C18A 180.000(2) . . . . ? O C16 C17 C18 -160.0(9) . . . . ? C16 C17 C18 C19 -43(2) . . . . ? C18A C17 C18 C19 59(4) . . . . ? C16 C17 C18A C19A 103(2) . . . . ? C18 C17 C18A C19A 17(3) . . . . ? C2 C1 N C4 -170.57(19) . . . . ? C3 C1 N C4 7.5(2) . . . . ? C2 C1 N Mg 13.7(3) . . . . ? C3 C1 N Mg -168.24(13) . . . . ? C9 C4 N C1 -82.4(2) . . . . ? C5 C4 N C1 96.87(19) . . . . ? C9 C4 N Mg 93.12(18) . . . . ? C5 C4 N Mg -87.66(18) . . . . ? O Mg N C1 99.39(14) . . . . ? O Mg N C1 -156.34(13) 5_656 . . . ? N Mg N C1 -28.64(16) 6 . . . ? Mg Mg N C1 151.59(12) 5_656 . . . ? O Mg N C4 -75.94(15) . . . . ? O Mg N C4 28.33(16) 5_656 . . . ? N Mg N C4 156.03(11) 6 . . . ? Mg Mg N C4 -23.74(17) 5_656 . . . ? C17 C16 O Mg 0 . . . . ? C17 C16 O Mg 180 . . . 5_656 ? O Mg O C16 180.0000(10) 5_656 . . . ? N Mg O C16 56.98(7) 6 . . . ? N Mg O C16 -56.98(7) . . . . ? Mg Mg O C16 180.0000(10) 5_656 . . . ? O Mg O Mg 0 5_656 . . 5_656 ? N Mg O Mg -123.02(6) 6 . . 5_656 ? N Mg O Mg 123.02(7) . . . 5_656 ? C1A C2A C3A C3A 180 . . . 5_666 ? # END of CIF