# Electronic Supplementary Material (ESI) for Dalton Transactions # 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_(1)-nov307 _database_code_depnum_ccdc_archive 'CCDC 888956' #TrackingRef 'Dalton_Mg_Comm.cif' _audit_creation_date 2007-11-07T11:22:35-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C31 H48 Mg O3' _chemical_formula_sum 'C31 H48 Mg O3' _chemical_formula_weight 493 _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 9.6951(4) _cell_length_b 12.6917(5) _cell_length_c 13.2396(6) _cell_angle_alpha 105.571(2) _cell_angle_beta 93.391(2) _cell_angle_gamma 111.398(2) _cell_volume 1438.55(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 28119 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.09 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.7107 _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 -0.97473E-1 _diffrn_orient_matrix_ub_12 0.77503E-2 _diffrn_orient_matrix_ub_13 -0.153795E-1 _diffrn_orient_matrix_ub_21 -0.50553E-1 _diffrn_orient_matrix_ub_22 -0.631014E-1 _diffrn_orient_matrix_ub_23 0.330416E-1 _diffrn_orient_matrix_ub_31 0.245835E-1 _diffrn_orient_matrix_ub_32 0.623864E-1 _diffrn_orient_matrix_ub_33 0.708112E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_unetI/netI 0.03 _diffrn_reflns_number 21479 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 26.08 _diffrn_reflns_theta_full 26.08 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _reflns_number_total 5625 _reflns_number_gt 4653 _reflns_threshold_expression >2sigma(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-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+0.7276P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5625 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.122 _refine_ls_wR_factor_gt 0.113 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.472 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.043 #----------------------------------------------------------------------------# # 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' 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 Mg1 Mg 0.71016(6) 0.18350(5) 0.33818(4) 0.02429(14) Uani 1 1 d . . . O1 O 0.59281(12) 0.19215(10) 0.22585(9) 0.0264(3) Uani 1 1 d . . . O2 O 0.93168(12) 0.26586(10) 0.32368(9) 0.0307(3) Uani 1 1 d . . . O3 O 0.69211(14) 0.01104(10) 0.30363(10) 0.0347(3) Uani 1 1 d . . . C1 C 0.70848(18) 0.24914(14) 0.50735(12) 0.0248(3) Uani 1 1 d . . . C2 C 0.61379(18) 0.30637(14) 0.54768(13) 0.0267(3) Uani 1 1 d . . . C3 C 0.62570(19) 0.35965(15) 0.65662(14) 0.0311(4) Uani 1 1 d . . . H3 H 0.5603 0.398 0.6799 0.037 Uiso 1 1 calc R . . C4 C 0.7303(2) 0.35820(15) 0.73193(13) 0.0327(4) Uani 1 1 d . . . C5 C 0.8234(2) 0.30101(15) 0.69456(13) 0.0313(4) Uani 1 1 d . . . H5 H 0.8955 0.2978 0.7442 0.038 Uiso 1 1 calc R . . C6 C 0.81385(18) 0.24805(14) 0.58580(13) 0.0269(3) Uani 1 1 d . . . C7 C 0.49190(19) 0.31021(16) 0.47332(14) 0.0323(4) Uani 1 1 d . . . H7A H 0.3959 0.2452 0.4695 0.048 Uiso 1 1 calc R . . H7B H 0.5185 0.3012 0.4021 0.048 Uiso 1 1 calc R . . H7C H 0.4825 0.3867 0.5003 0.048 Uiso 1 1 calc R . . C8 C 0.7402(3) 0.41470(19) 0.84968(15) 0.0466(5) Uani 1 1 d . . . H8A H 0.6491 0.3694 0.8729 0.07 Uiso 1 1 calc R . . H8B H 0.7494 0.497 0.8631 0.07 Uiso 1 1 calc R . . H8C H 0.8285 0.4143 0.8894 0.07 Uiso 1 1 calc R . . C9 C 0.9224(2) 0.18841(16) 0.55636(14) 0.0339(4) Uani 1 1 d . . . H9A H 1.0247 0.2437 0.5922 0.051 Uiso 1 1 calc R . . H9B H 0.9184 0.1662 0.4791 0.051 Uiso 1 1 calc R . . H9C H 0.894 0.1168 0.5787 0.051 Uiso 1 1 calc R . . C10 C 0.49211(17) 0.20829(14) 0.16645(12) 0.0232(3) Uani 1 1 d . . . C11 C 0.34471(18) 0.11660(14) 0.12538(12) 0.0256(3) Uani 1 1 d . . . C12 C 0.24208(19) 0.13743(16) 0.06342(13) 0.0323(4) Uani 1 1 d . . . H12 H 0.1438 0.0771 0.0365 0.039 Uiso 1 1 calc R . . C13 C 0.2788(2) 0.24310(17) 0.03992(14) 0.0363(4) Uani 1 1 d . . . H13 H 0.2066 0.255 -0.0024 0.044 Uiso 1 1 calc R . . C14 C 0.4215(2) 0.33107(16) 0.07859(13) 0.0323(4) Uani 1 1 d . . . H14 H 0.4463 0.4033 0.0617 0.039 Uiso 1 1 calc R . . C15 C 0.53048(18) 0.31751(14) 0.14161(12) 0.0257(3) Uani 1 1 d . . . C16 C 0.29836(19) -0.00399(15) 0.14709(13) 0.0306(4) Uani 1 1 d . . . C17 C 0.3068(2) 0.01280(16) 0.26696(14) 0.0360(4) Uani 1 1 d . . . H17A H 0.4097 0.0646 0.3042 0.054 Uiso 1 1 calc R . . H17B H 0.2782 -0.0648 0.2787 0.054 Uiso 1 1 calc R . . H17C H 0.2377 0.0494 0.2944 0.054 Uiso 1 1 calc R . . C18 C 0.3986(2) -0.06744(16) 0.09994(15) 0.0371(4) Uani 1 1 d . . . H18A H 0.3792 -0.0886 0.0221 0.056 Uiso 1 1 calc R . . H18B H 0.3761 -0.1399 0.1204 0.056 Uiso 1 1 calc R . . H18C H 0.5046 -0.0143 0.1272 0.056 Uiso 1 1 calc R . . C19 C 0.1349(2) -0.08897(17) 0.09468(17) 0.0431(5) Uani 1 1 d . . . H19A H 0.0663 -0.0523 0.1227 0.065 Uiso 1 1 calc R . . H19B H 0.1108 -0.1641 0.1106 0.065 Uiso 1 1 calc R . . H19C H 0.1238 -0.1045 0.0174 0.065 Uiso 1 1 calc R . . C20 C 0.68896(19) 0.41832(14) 0.18115(13) 0.0278(4) Uani 1 1 d . . . C21 C 0.7048(2) 0.52609(16) 0.14344(16) 0.0394(4) Uani 1 1 d . . . H21A H 0.6849 0.5009 0.0654 0.059 Uiso 1 1 calc R . . H21B H 0.8071 0.5872 0.1698 0.059 Uiso 1 1 calc R . . H21C H 0.6324 0.5588 0.1711 0.059 Uiso 1 1 calc R . . C22 C 0.7238(2) 0.46625(15) 0.30363(13) 0.0334(4) Uani 1 1 d . . . H22A H 0.6491 0.4971 0.3298 0.05 Uiso 1 1 calc R . . H22B H 0.8244 0.5304 0.3269 0.05 Uiso 1 1 calc R . . H22C H 0.72 0.4018 0.3322 0.05 Uiso 1 1 calc R . . C23 C 0.8077(2) 0.37328(16) 0.13812(14) 0.0338(4) Uani 1 1 d . . . H23A H 0.799 0.3027 0.1586 0.051 Uiso 1 1 calc R . . H23B H 0.9083 0.4359 0.168 0.051 Uiso 1 1 calc R . . H23C H 0.7914 0.3524 0.0603 0.051 Uiso 1 1 calc R . . C24 C 1.0264(2) 0.2254(2) 0.25552(17) 0.0489(5) Uani 1 1 d . . . H24A H 0.9947 0.2191 0.1809 0.059 Uiso 1 1 calc R . . H24B H 1.019 0.1462 0.2578 0.059 Uiso 1 1 calc R . . C25 C 1.1837(2) 0.31527(19) 0.29665(16) 0.0452(5) Uani 1 1 d . . . H25A H 1.2121 0.3719 0.2551 0.054 Uiso 1 1 calc R . . H25B H 1.2558 0.2762 0.2938 0.054 Uiso 1 1 calc R . . C26 C 1.18027(19) 0.37820(16) 0.41114(14) 0.0346(4) Uani 1 1 d . . . H26A H 1.1908 0.3326 0.4591 0.041 Uiso 1 1 calc R . . H26B H 1.2603 0.4596 0.4375 0.041 Uiso 1 1 calc R . . C27 C 1.02680(19) 0.38101(15) 0.40091(14) 0.0318(4) Uani 1 1 d . . . H27A H 0.9916 0.3903 0.4702 0.038 Uiso 1 1 calc R . . H27B H 1.0272 0.4472 0.3747 0.038 Uiso 1 1 calc R . . C28 C 0.6381(2) -0.06236(17) 0.37187(17) 0.0389(4) Uani 1 1 d . . . H28A H 0.5317 -0.1179 0.3448 0.047 Uiso 1 1 calc R . . H28B H 0.647 -0.0124 0.4456 0.047 Uiso 1 1 calc R . . C29 C 0.7402(2) -0.13044(18) 0.36776(18) 0.0440(5) Uani 1 1 d . . . H29A H 0.8178 -0.0947 0.4329 0.053 Uiso 1 1 calc R . . H29B H 0.681 -0.215 0.3606 0.053 Uiso 1 1 calc R . . C30 C 0.8118(3) -0.1195(2) 0.2704(2) 0.0616(7) Uani 1 1 d . . . H30A H 0.9211 -0.0701 0.2913 0.074 Uiso 1 1 calc R . . H30B H 0.7966 -0.1989 0.2224 0.074 Uiso 1 1 calc R . . C31 C 0.7351(3) -0.06206(19) 0.21777(17) 0.0479(5) Uani 1 1 d . . . H31A H 0.8038 -0.0125 0.1806 0.058 Uiso 1 1 calc R . . H31B H 0.6455 -0.1224 0.1655 0.058 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0251(3) 0.0272(3) 0.0228(3) 0.0071(2) 0.0017(2) 0.0137(2) O1 0.0252(6) 0.0274(6) 0.0266(6) 0.0094(5) -0.0013(5) 0.0107(5) O2 0.0240(6) 0.0358(6) 0.0285(6) 0.0024(5) 0.0023(5) 0.0134(5) O3 0.0467(7) 0.0302(6) 0.0334(7) 0.0102(5) 0.0079(6) 0.0218(6) C1 0.0261(8) 0.0240(8) 0.0246(8) 0.0082(6) 0.0035(6) 0.0099(7) C2 0.0251(8) 0.0259(8) 0.0296(9) 0.0109(7) 0.0053(7) 0.0091(7) C3 0.0340(9) 0.0285(8) 0.0336(9) 0.0096(7) 0.0112(7) 0.0148(7) C4 0.0412(10) 0.0287(9) 0.0259(9) 0.0079(7) 0.0080(7) 0.0112(8) C5 0.0350(9) 0.0315(9) 0.0267(9) 0.0118(7) -0.0003(7) 0.0113(7) C6 0.0287(8) 0.0269(8) 0.0271(8) 0.0108(7) 0.0048(7) 0.0116(7) C7 0.0279(9) 0.0366(9) 0.0356(9) 0.0103(8) 0.0060(7) 0.0169(8) C8 0.0661(14) 0.0467(11) 0.0277(10) 0.0087(9) 0.0104(9) 0.0249(11) C9 0.0332(9) 0.0401(10) 0.0342(9) 0.0145(8) 0.0018(7) 0.0196(8) C10 0.0256(8) 0.0270(8) 0.0185(7) 0.0053(6) 0.0035(6) 0.0135(7) C11 0.0259(8) 0.0292(8) 0.0213(8) 0.0054(6) 0.0035(6) 0.0123(7) C12 0.0263(8) 0.0382(9) 0.0280(9) 0.0050(7) -0.0011(7) 0.0127(7) C13 0.0347(10) 0.0464(11) 0.0312(9) 0.0111(8) -0.0026(8) 0.0219(9) C14 0.0400(10) 0.0337(9) 0.0294(9) 0.0118(7) 0.0043(7) 0.0205(8) C15 0.0298(8) 0.0284(8) 0.0204(8) 0.0056(6) 0.0044(6) 0.0147(7) C16 0.0270(9) 0.0286(8) 0.0297(9) 0.0066(7) 0.0007(7) 0.0063(7) C17 0.0343(9) 0.0356(9) 0.0344(10) 0.0139(8) 0.0054(8) 0.0079(8) C18 0.0400(10) 0.0264(9) 0.0394(10) 0.0049(8) 0.0043(8) 0.0115(8) C19 0.0321(10) 0.0375(10) 0.0459(11) 0.0104(9) -0.0027(8) 0.0017(8) C20 0.0323(9) 0.0247(8) 0.0249(8) 0.0079(7) 0.0029(7) 0.0098(7) C21 0.0484(11) 0.0294(9) 0.0400(10) 0.0139(8) 0.0049(9) 0.0132(8) C22 0.0375(10) 0.0277(9) 0.0283(9) 0.0043(7) 0.0006(7) 0.0093(8) C23 0.0326(9) 0.0338(9) 0.0341(9) 0.0120(8) 0.0081(7) 0.0110(8) C24 0.0324(10) 0.0600(13) 0.0431(12) -0.0054(10) 0.0082(9) 0.0208(10) C25 0.0317(10) 0.0519(12) 0.0439(11) 0.0050(9) 0.0096(8) 0.0141(9) C26 0.0271(9) 0.0339(9) 0.0358(10) 0.0072(8) 0.0026(7) 0.0073(7) C27 0.0322(9) 0.0266(8) 0.0329(9) 0.0040(7) 0.0032(7) 0.0116(7) C28 0.0364(10) 0.0358(10) 0.0517(12) 0.0214(9) 0.0127(9) 0.0161(8) C29 0.0442(11) 0.0402(10) 0.0607(13) 0.0266(10) 0.0146(10) 0.0228(9) C30 0.0777(17) 0.0665(15) 0.0763(17) 0.0393(13) 0.0356(14) 0.0528(14) C31 0.0663(14) 0.0416(11) 0.0461(12) 0.0108(9) 0.0155(10) 0.0339(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O1 1.8699(11) . ? Mg1 O3 2.0505(12) . ? Mg1 O2 2.0641(12) . ? Mg1 C1 2.1733(17) . ? O1 C10 1.3248(18) . ? O2 C24 1.454(2) . ? O2 C27 1.461(2) . ? O3 C31 1.449(2) . ? O3 C28 1.453(2) . ? C1 C2 1.411(2) . ? C1 C6 1.420(2) . ? C2 C3 1.397(2) . ? C2 C7 1.516(2) . ? C3 C4 1.388(2) . ? C3 H3 0.95 . ? C4 C5 1.388(2) . ? C4 C8 1.512(2) . ? C5 C6 1.397(2) . ? C5 H5 0.95 . ? C6 C9 1.518(2) . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 C11 1.431(2) . ? C10 C15 1.432(2) . ? C11 C12 1.395(2) . ? C11 C16 1.542(2) . ? C12 C13 1.382(3) . ? C12 H12 0.95 . ? C13 C14 1.380(3) . ? C13 H13 0.95 . ? C14 C15 1.396(2) . ? C14 H14 0.95 . ? C15 C20 1.544(2) . ? C16 C18 1.535(2) . ? C16 C17 1.537(2) . ? C16 C19 1.541(2) . ? 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 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 C23 1.536(2) . ? C20 C21 1.538(2) . ? C20 C22 1.539(2) . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 C25 1.491(3) . ? C24 H24A 0.99 . ? C24 H24B 0.99 . ? C25 C26 1.521(3) . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? C26 C27 1.500(2) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? C27 H27A 0.99 . ? C27 H27B 0.99 . ? C28 C29 1.527(3) . ? C28 H28A 0.99 . ? C28 H28B 0.99 . ? C29 C30 1.515(3) . ? C29 H29A 0.99 . ? C29 H29B 0.99 . ? C30 C31 1.475(3) . ? C30 H30A 0.99 . ? C30 H30B 0.99 . ? C31 H31A 0.99 . ? C31 H31B 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 O1 Mg1 O3 107.75(5) . . ? O1 Mg1 O2 106.50(5) . . ? O3 Mg1 O2 99.83(5) . . ? O1 Mg1 C1 127.23(6) . . ? O3 Mg1 C1 107.82(6) . . ? O2 Mg1 C1 104.34(6) . . ? C10 O1 Mg1 165.00(10) . . ? C24 O2 C27 107.93(13) . . ? C24 O2 Mg1 132.12(11) . . ? C27 O2 Mg1 119.48(10) . . ? C31 O3 C28 104.68(13) . . ? C31 O3 Mg1 131.52(11) . . ? C28 O3 Mg1 123.68(11) . . ? C2 C1 C6 114.95(14) . . ? C2 C1 Mg1 122.88(11) . . ? C6 C1 Mg1 121.88(11) . . ? C3 C2 C1 122.11(15) . . ? C3 C2 C7 117.16(14) . . ? C1 C2 C7 120.72(14) . . ? C4 C3 C2 121.96(16) . . ? C4 C3 H3 119 . . ? C2 C3 H3 119 . . ? C5 C4 C3 117.14(15) . . ? C5 C4 C8 121.54(17) . . ? C3 C4 C8 121.31(17) . . ? C4 C5 C6 121.65(15) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 122.18(15) . . ? C5 C6 C9 115.99(14) . . ? C1 C6 C9 121.83(14) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O1 C10 C11 120.53(14) . . ? O1 C10 C15 120.20(14) . . ? C11 C10 C15 119.26(13) . . ? C12 C11 C10 118.65(15) . . ? C12 C11 C16 119.78(15) . . ? C10 C11 C16 121.56(13) . . ? C13 C12 C11 122.10(16) . . ? C13 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C14 C13 C12 119.26(15) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 122.20(16) . . ? C13 C14 H14 118.9 . . ? C15 C14 H14 118.9 . . ? C14 C15 C10 118.52(15) . . ? C14 C15 C20 119.86(14) . . ? C10 C15 C20 121.61(13) . . ? C18 C16 C17 110.97(15) . . ? C18 C16 C19 106.47(14) . . ? C17 C16 C19 106.02(14) . . ? C18 C16 C11 109.75(14) . . ? C17 C16 C11 111.03(14) . . ? C19 C16 C11 112.47(14) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C23 C20 C21 107.02(14) . . ? C23 C20 C22 110.43(14) . . ? C21 C20 C22 105.86(14) . . ? C23 C20 C15 110.09(13) . . ? C21 C20 C15 112.42(14) . . ? C22 C20 C15 110.89(13) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O2 C24 C25 106.91(15) . . ? O2 C24 H24A 110.3 . . ? C25 C24 H24A 110.3 . . ? O2 C24 H24B 110.3 . . ? C25 C24 H24B 110.3 . . ? H24A C24 H24B 108.6 . . ? C24 C25 C26 103.73(15) . . ? C24 C25 H25A 111 . . ? C26 C25 H25A 111 . . ? C24 C25 H25B 111 . . ? C26 C25 H25B 111 . . ? H25A C25 H25B 109 . . ? C27 C26 C25 101.51(14) . . ? C27 C26 H26A 111.5 . . ? C25 C26 H26A 111.5 . . ? C27 C26 H26B 111.5 . . ? C25 C26 H26B 111.5 . . ? H26A C26 H26B 109.3 . . ? O2 C27 C26 104.17(13) . . ? O2 C27 H27A 110.9 . . ? C26 C27 H27A 110.9 . . ? O2 C27 H27B 110.9 . . ? C26 C27 H27B 110.9 . . ? H27A C27 H27B 108.9 . . ? O3 C28 C29 104.37(14) . . ? O3 C28 H28A 110.9 . . ? C29 C28 H28A 110.9 . . ? O3 C28 H28B 110.9 . . ? C29 C28 H28B 110.9 . . ? H28A C28 H28B 108.9 . . ? C30 C29 C28 104.66(16) . . ? C30 C29 H29A 110.8 . . ? C28 C29 H29A 110.8 . . ? C30 C29 H29B 110.8 . . ? C28 C29 H29B 110.8 . . ? H29A C29 H29B 108.9 . . ? C31 C30 C29 105.25(17) . . ? C31 C30 H30A 110.7 . . ? C29 C30 H30A 110.7 . . ? C31 C30 H30B 110.7 . . ? C29 C30 H30B 110.7 . . ? H30A C30 H30B 108.8 . . ? O3 C31 C30 104.64(17) . . ? O3 C31 H31A 110.8 . . ? C30 C31 H31A 110.8 . . ? O3 C31 H31B 110.8 . . ? C30 C31 H31B 110.8 . . ? H31A C31 H31B 108.9 . . ? data_(2)-oct1606 _database_code_depnum_ccdc_archive 'CCDC 888957' #TrackingRef 'Dalton_Mg_Comm.cif' _audit_creation_date 2006-10-25T08:42:31-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C52 H86 Br2 Mg2 N4 O2' _chemical_formula_sum 'C52 H86 Br2 Mg2 N4 O2' _chemical_formula_weight 1007.69 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.5449(4) _cell_length_b 18.3542(5) _cell_length_c 13.3608(4) _cell_angle_alpha 90 _cell_angle_beta 100.793(2) _cell_angle_gamma 90 _cell_volume 2781.04(15) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15765 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.519 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7444 _exptl_absorpt_correction_T_max 0.8283 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(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 0.82107E-2 _diffrn_orient_matrix_ub_12 -0.517415E-1 _diffrn_orient_matrix_ub_13 -0.210564E-1 _diffrn_orient_matrix_ub_21 -0.865561E-1 _diffrn_orient_matrix_ub_22 -0.20309E-2 _diffrn_orient_matrix_ub_23 -0.280201E-1 _diffrn_orient_matrix_ub_31 0.146972E-1 _diffrn_orient_matrix_ub_32 0.169451E-1 _diffrn_orient_matrix_ub_33 -0.676533E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_av_unetI/netI 0.0521 _diffrn_reflns_number 22540 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 26.04 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 5474 _reflns_number_gt 3855 _reflns_threshold_expression >2sigma(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-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+2.2875P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5474 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0793 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0828 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.316 _refine_diff_density_min -0.369 _refine_diff_density_rms 0.055 #----------------------------------------------------------------------------# # 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' Br Br -0.2901 2.4595 '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 Mg Mg 0.50462(8) 0.07985(5) -0.09026(7) 0.0333(2) Uani 1 1 d . . . Br Br 0.51162(3) 0.065639(15) 0.10087(2) 0.04637(12) Uani 1 1 d . . . O O 0.34418(17) 0.09118(11) -0.18347(16) 0.0451(5) Uani 1 1 d . . . N1 N 0.5604(2) 0.19004(12) -0.09026(17) 0.0336(5) Uani 1 1 d . . . N2 N 0.6508(2) 0.09779(11) -0.15349(18) 0.0345(6) Uani 1 1 d . . . C1 C 0.6558(2) 0.16760(14) -0.1241(2) 0.0302(6) Uani 1 1 d . . . C2 C 0.7618(2) 0.21475(13) -0.1258(2) 0.0295(6) Uani 1 1 d . . . C3 C 0.8424(2) 0.22602(14) -0.0353(2) 0.0341(7) Uani 1 1 d . . . C4 C 0.9401(3) 0.26978(17) -0.0381(2) 0.0463(8) Uani 1 1 d . . . H4 H 0.9948 0.2781 0.0233 0.056 Uiso 1 1 calc R . . C5 C 0.9605(3) 0.30172(17) -0.1272(3) 0.0464(8) Uani 1 1 d . . . C6 C 0.8800(3) 0.28880(15) -0.2160(2) 0.0388(7) Uani 1 1 d . . . H6 H 0.8928 0.3099 -0.2779 0.047 Uiso 1 1 calc R . . C7 C 0.7808(2) 0.24565(14) -0.2169(2) 0.0320(6) Uani 1 1 d . . . C8 C 0.8280(3) 0.19204(17) 0.0648(2) 0.0442(8) Uani 1 1 d . . . H8A H 0.8067 0.2299 0.1099 0.066 Uiso 1 1 calc R . . H8B H 0.9023 0.1691 0.097 0.066 Uiso 1 1 calc R . . H8C H 0.7655 0.1552 0.0522 0.066 Uiso 1 1 calc R . . C9 C 1.0674(3) 0.3494(2) -0.1272(3) 0.0789(13) Uani 1 1 d . . . H9A H 1.1139 0.3522 -0.0579 0.118 Uiso 0.5 1 calc PR . . H9B H 1.0418 0.3984 -0.1507 0.118 Uiso 0.5 1 calc PR . . H9C H 1.1158 0.3285 -0.1729 0.118 Uiso 0.5 1 calc PR . . H9D H 1.0671 0.3672 -0.1964 0.118 Uiso 0.5 1 calc PR . . H9E H 1.1392 0.321 -0.1036 0.118 Uiso 0.5 1 calc PR . . H9F H 1.0652 0.3909 -0.0815 0.118 Uiso 0.5 1 calc PR . . C10 C 0.6956(3) 0.23212(15) -0.3152(2) 0.0394(7) Uani 1 1 d . . . H10A H 0.6993 0.1808 -0.3344 0.059 Uiso 1 1 calc R . . H10B H 0.7166 0.2629 -0.369 0.059 Uiso 1 1 calc R . . H10C H 0.6154 0.2439 -0.3061 0.059 Uiso 1 1 calc R . . C11 C 0.5442(2) 0.26536(14) -0.0607(2) 0.0355(7) Uani 1 1 d . . . H11 H 0.6178 0.2936 -0.063 0.043 Uiso 1 1 calc R . . C12 C 0.5175(3) 0.26894(17) 0.0467(2) 0.0472(8) Uani 1 1 d . . . H12A H 0.5852 0.2489 0.0954 0.057 Uiso 1 1 calc R . . H12B H 0.4478 0.2383 0.0501 0.057 Uiso 1 1 calc R . . C13 C 0.4935(3) 0.34704(18) 0.0779(3) 0.0565(9) Uani 1 1 d . . . H13A H 0.4735 0.3467 0.1467 0.068 Uiso 1 1 calc R . . H13B H 0.5656 0.3768 0.0807 0.068 Uiso 1 1 calc R . . C14 C 0.3937(3) 0.38080(18) 0.0036(3) 0.0523(9) Uani 1 1 d . . . H14A H 0.3843 0.4323 0.0226 0.063 Uiso 1 1 calc R . . H14B H 0.3195 0.3549 0.0075 0.063 Uiso 1 1 calc R . . C15 C 0.4156(3) 0.37739(16) -0.1043(2) 0.0502(8) Uani 1 1 d . . . H15A H 0.4831 0.4092 -0.1106 0.06 Uiso 1 1 calc R . . H15B H 0.3453 0.3959 -0.1516 0.06 Uiso 1 1 calc R . . C16 C 0.4417(3) 0.29941(15) -0.1343(2) 0.0409(7) Uani 1 1 d . . . H16A H 0.3704 0.2691 -0.1362 0.049 Uiso 1 1 calc R . . H16B H 0.4605 0.2998 -0.2037 0.049 Uiso 1 1 calc R . . C17 C 0.7497(2) 0.06133(15) -0.1861(2) 0.0378(7) Uani 1 1 d . . . H17 H 0.8033 0.0989 -0.2069 0.045 Uiso 1 1 calc R . . C18 C 0.8185(3) 0.01599(18) -0.0988(3) 0.0500(8) Uani 1 1 d . . . H18A H 0.8531 0.0489 -0.0424 0.06 Uiso 1 1 calc R . . H18B H 0.7635 -0.0174 -0.073 0.06 Uiso 1 1 calc R . . C19 C 0.9167(3) -0.02848(19) -0.1311(3) 0.0585(9) Uani 1 1 d . . . H19A H 0.9764 0.0048 -0.1504 0.07 Uiso 1 1 calc R . . H19B H 0.9559 -0.0588 -0.0733 0.07 Uiso 1 1 calc R . . C20 C 0.8676(3) -0.07689(17) -0.2203(2) 0.0509(9) Uani 1 1 d . . . H20A H 0.9328 -0.1037 -0.2424 0.061 Uiso 1 1 calc R . . H20B H 0.8133 -0.1131 -0.1991 0.061 Uiso 1 1 calc R . . C21 C 0.8023(3) -0.03267(19) -0.3081(3) 0.0607(10) Uani 1 1 d . . . H21A H 0.7682 -0.0658 -0.3644 0.073 Uiso 1 1 calc R . . H21B H 0.8584 0.0003 -0.3333 0.073 Uiso 1 1 calc R . . C22 C 0.7042(3) 0.01218(16) -0.2766(2) 0.0463(8) Uani 1 1 d . . . H22A H 0.6663 0.0425 -0.3349 0.056 Uiso 1 1 calc R . . H22B H 0.6437 -0.0211 -0.2587 0.056 Uiso 1 1 calc R . . C23 C 0.3398(3) 0.12442(18) -0.2822(2) 0.0520(9) Uani 1 1 d . . . H23A H 0.4093 0.1565 -0.2795 0.062 Uiso 1 1 calc R . . H23B H 0.2683 0.1551 -0.2986 0.062 Uiso 1 1 calc R . . C24 C 0.3382(4) 0.0692(2) -0.3647(3) 0.0746(11) Uani 1 1 d . . . H24A H 0.4107 0.0402 -0.3506 0.112 Uiso 1 1 calc R . . H24B H 0.3328 0.0941 -0.4303 0.112 Uiso 1 1 calc R . . H24C H 0.2699 0.037 -0.3674 0.112 Uiso 1 1 calc R . . C25 C 0.2303(3) 0.07062(18) -0.1613(3) 0.0547(9) Uani 1 1 d . . . H25A H 0.2402 0.0288 -0.1136 0.066 Uiso 1 1 calc R . . H25B H 0.1776 0.0553 -0.2249 0.066 Uiso 1 1 calc R . . C26 C 0.1753(3) 0.1331(2) -0.1148(3) 0.0793(12) Uani 1 1 d . . . H26A H 0.2288 0.1495 -0.0532 0.119 Uiso 1 1 calc R . . H26B H 0.1005 0.1172 -0.0971 0.119 Uiso 1 1 calc R . . H26C H 0.1605 0.1733 -0.1638 0.119 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg 0.0349(5) 0.0314(5) 0.0354(6) 0.0030(4) 0.0113(4) -0.0010(4) Br 0.0721(2) 0.03224(16) 0.03814(19) -0.00049(14) 0.01904(16) -0.00595(16) O 0.0360(12) 0.0494(12) 0.0480(14) 0.0132(10) 0.0030(10) -0.0067(10) N1 0.0378(14) 0.0292(12) 0.0359(14) -0.0018(10) 0.0123(11) -0.0016(11) N2 0.0394(14) 0.0263(11) 0.0409(15) -0.0027(10) 0.0159(12) -0.0011(10) C1 0.0332(16) 0.0311(14) 0.0262(15) 0.0040(12) 0.0055(12) 0.0012(12) C2 0.0287(15) 0.0265(14) 0.0343(17) -0.0028(12) 0.0084(13) 0.0016(12) C3 0.0359(17) 0.0322(15) 0.0331(17) 0.0006(12) 0.0032(14) 0.0024(13) C4 0.0386(18) 0.0491(19) 0.045(2) 0.0013(15) -0.0092(15) -0.0018(15) C5 0.0348(18) 0.0461(18) 0.056(2) 0.0095(16) 0.0014(16) -0.0076(15) C6 0.0379(17) 0.0403(17) 0.0391(19) 0.0075(13) 0.0097(15) -0.0005(14) C7 0.0323(16) 0.0312(14) 0.0336(17) 0.0006(12) 0.0087(13) 0.0010(13) C8 0.0491(19) 0.0484(18) 0.0331(18) -0.0011(14) 0.0028(15) 0.0030(16) C9 0.050(2) 0.093(3) 0.086(3) 0.028(2) -0.008(2) -0.030(2) C10 0.0466(18) 0.0397(16) 0.0321(17) -0.0002(13) 0.0080(15) -0.0054(14) C11 0.0319(16) 0.0306(15) 0.0459(18) -0.0058(13) 0.0120(14) 0.0001(13) C12 0.054(2) 0.0493(19) 0.0373(19) -0.0063(15) 0.0051(16) 0.0138(16) C13 0.065(2) 0.056(2) 0.047(2) -0.0165(16) 0.0092(19) 0.0107(18) C14 0.053(2) 0.0480(19) 0.059(2) -0.0082(17) 0.0197(18) 0.0127(16) C15 0.059(2) 0.0368(17) 0.057(2) -0.0001(15) 0.0146(17) 0.0105(16) C16 0.0517(19) 0.0353(16) 0.0376(18) 0.0023(13) 0.0137(15) 0.0050(14) C17 0.0406(17) 0.0297(14) 0.0477(19) -0.0008(13) 0.0203(15) -0.0008(13) C18 0.0444(19) 0.056(2) 0.048(2) -0.0149(16) 0.0037(16) 0.0101(16) C19 0.043(2) 0.056(2) 0.076(3) -0.0079(19) 0.0107(19) 0.0125(17) C20 0.062(2) 0.0413(18) 0.055(2) -0.0009(16) 0.0239(18) 0.0137(16) C21 0.087(3) 0.053(2) 0.049(2) -0.0012(17) 0.029(2) 0.019(2) C22 0.064(2) 0.0414(17) 0.0340(18) -0.0010(14) 0.0119(16) 0.0126(16) C23 0.055(2) 0.0513(19) 0.045(2) 0.0155(16) -0.0023(17) -0.0078(17) C24 0.084(3) 0.082(3) 0.056(3) -0.003(2) 0.007(2) -0.004(2) C25 0.0398(18) 0.058(2) 0.066(2) 0.0085(18) 0.0090(17) -0.0106(17) C26 0.064(3) 0.075(3) 0.106(4) -0.001(2) 0.036(2) -0.001(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg O 2.040(2) . ? Mg N2 2.050(2) . ? Mg N1 2.123(2) . ? Mg Br 2.5532(9) . ? Mg Br 2.6789(9) 3_655 ? Br Mg 2.6789(9) 3_655 ? O C23 1.445(3) . ? O C25 1.451(3) . ? N1 C1 1.331(3) . ? N1 C11 1.459(3) . ? N2 C1 1.338(3) . ? N2 C17 1.459(3) . ? C1 C2 1.503(4) . ? C2 C3 1.396(4) . ? C2 C7 1.396(4) . ? C3 C4 1.390(4) . ? C3 C8 1.513(4) . ? C4 C5 1.385(4) . ? C4 H4 0.95 . ? C5 C6 1.384(4) . ? C5 C9 1.513(4) . ? C6 C7 1.391(4) . ? C6 H6 0.95 . ? C7 C10 1.507(4) . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C9 H9D 0.98 . ? C9 H9E 0.98 . ? C9 H9F 0.98 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 C16 1.524(4) . ? C11 C12 1.524(4) . ? C11 H11 1 . ? C12 C13 1.533(4) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.506(4) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 C15 1.511(4) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 C16 1.532(4) . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 C22 1.521(4) . ? C17 C18 1.528(4) . ? C17 H17 1 . ? C18 C19 1.524(4) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 C20 1.510(5) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? C20 C21 1.507(5) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? C21 C22 1.522(4) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? C23 C24 1.495(5) . ? C23 H23A 0.99 . ? C23 H23B 0.99 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 C26 1.500(5) . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O Mg N2 117.09(10) . . ? O Mg N1 98.28(9) . . ? N2 Mg N1 64.76(8) . . ? O Mg Br 118.43(7) . . ? N2 Mg Br 123.66(8) . . ? N1 Mg Br 98.32(7) . . ? O Mg Br 91.30(7) . 3_655 ? N2 Mg Br 101.13(7) . 3_655 ? N1 Mg Br 165.47(7) . 3_655 ? Br Mg Br 86.55(3) . 3_655 ? Mg Br Mg 93.45(3) . 3_655 ? C23 O C25 114.7(2) . . ? C23 O Mg 118.20(18) . . ? C25 O Mg 127.06(19) . . ? C1 N1 C11 122.8(2) . . ? C1 N1 Mg 88.61(16) . . ? C11 N1 Mg 148.02(17) . . ? C1 N2 C17 122.2(2) . . ? C1 N2 Mg 91.52(16) . . ? C17 N2 Mg 143.14(17) . . ? N1 C1 N2 113.7(2) . . ? N1 C1 C2 123.7(2) . . ? N2 C1 C2 122.5(2) . . ? C3 C2 C7 120.5(2) . . ? C3 C2 C1 119.0(2) . . ? C7 C2 C1 120.5(2) . . ? C4 C3 C2 118.3(3) . . ? C4 C3 C8 119.1(3) . . ? C2 C3 C8 122.6(2) . . ? C5 C4 C3 122.5(3) . . ? C5 C4 H4 118.8 . . ? C3 C4 H4 118.8 . . ? C6 C5 C4 118.0(3) . . ? C6 C5 C9 121.0(3) . . ? C4 C5 C9 121.0(3) . . ? C5 C6 C7 121.6(3) . . ? C5 C6 H6 119.2 . . ? C7 C6 H6 119.2 . . ? C6 C7 C2 119.2(3) . . ? C6 C7 C10 120.2(2) . . ? C2 C7 C10 120.6(2) . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C9 H9D 109.5 . . ? H9A C9 H9D 141.1 . . ? H9B C9 H9D 56.3 . . ? H9C C9 H9D 56.3 . . ? C5 C9 H9E 109.5 . . ? H9A C9 H9E 56.3 . . ? H9B C9 H9E 141.1 . . ? H9C C9 H9E 56.3 . . ? H9D C9 H9E 109.5 . . ? C5 C9 H9F 109.5 . . ? H9A C9 H9F 56.3 . . ? H9B C9 H9F 56.3 . . ? H9C C9 H9F 141.1 . . ? H9D C9 H9F 109.5 . . ? H9E C9 H9F 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C16 109.7(2) . . ? N1 C11 C12 110.8(2) . . ? C16 C11 C12 108.7(2) . . ? N1 C11 H11 109.2 . . ? C16 C11 H11 109.2 . . ? C12 C11 H11 109.2 . . ? C11 C12 C13 112.0(3) . . ? C11 C12 H12A 109.2 . . ? C13 C12 H12A 109.2 . . ? C11 C12 H12B 109.2 . . ? C13 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C14 C13 C12 111.1(3) . . ? C14 C13 H13A 109.4 . . ? C12 C13 H13A 109.4 . . ? C14 C13 H13B 109.4 . . ? C12 C13 H13B 109.4 . . ? H13A C13 H13B 108 . . ? C13 C14 C15 111.6(3) . . ? C13 C14 H14A 109.3 . . ? C15 C14 H14A 109.3 . . ? C13 C14 H14B 109.3 . . ? C15 C14 H14B 109.3 . . ? H14A C14 H14B 108 . . ? C14 C15 C16 111.4(3) . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 108 . . ? C11 C16 C15 112.4(3) . . ? C11 C16 H16A 109.1 . . ? C15 C16 H16A 109.1 . . ? C11 C16 H16B 109.1 . . ? C15 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? N2 C17 C22 109.7(2) . . ? N2 C17 C18 110.3(2) . . ? C22 C17 C18 109.6(2) . . ? N2 C17 H17 109.1 . . ? C22 C17 H17 109.1 . . ? C18 C17 H17 109.1 . . ? C19 C18 C17 112.6(3) . . ? C19 C18 H18A 109.1 . . ? C17 C18 H18A 109.1 . . ? C19 C18 H18B 109.1 . . ? C17 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? C20 C19 C18 110.4(3) . . ? C20 C19 H19A 109.6 . . ? C18 C19 H19A 109.6 . . ? C20 C19 H19B 109.6 . . ? C18 C19 H19B 109.6 . . ? H19A C19 H19B 108.1 . . ? C21 C20 C19 110.9(3) . . ? C21 C20 H20A 109.5 . . ? C19 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 108.1 . . ? C20 C21 C22 111.4(3) . . ? C20 C21 H21A 109.3 . . ? C22 C21 H21A 109.3 . . ? C20 C21 H21B 109.3 . . ? C22 C21 H21B 109.3 . . ? H21A C21 H21B 108 . . ? C17 C22 C21 112.1(3) . . ? C17 C22 H22A 109.2 . . ? C21 C22 H22A 109.2 . . ? C17 C22 H22B 109.2 . . ? C21 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? O C23 C24 112.3(3) . . ? O C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? O C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.9 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O C25 C26 110.9(3) . . ? O C25 H25A 109.5 . . ? C26 C25 H25A 109.5 . . ? O C25 H25B 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? data_(3)-aug1211 _database_code_depnum_ccdc_archive 'CCDC 888958' #TrackingRef 'Dalton_Mg_Comm.cif' _audit_creation_date 2011-09-09T09:10:33-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C40 H62 Mg N2 O2, C6 H14' _chemical_formula_sum 'C46 H76 Mg N2 O2' _chemical_formula_weight 713.42 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 14.9601(6) _cell_length_b 19.0704(5) _cell_length_c 19.3281(6) _cell_angle_alpha 90 _cell_angle_beta 117.177(2) _cell_angle_gamma 90 _cell_volume 4905.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 66022 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 0.849 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.063 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(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_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.54517E-2 _diffrn_orient_matrix_ub_12 0.439943E-1 _diffrn_orient_matrix_ub_13 0.310103E-1 _diffrn_orient_matrix_ub_21 -0.20744E-1 _diffrn_orient_matrix_ub_22 0.280805E-1 _diffrn_orient_matrix_ub_23 -0.49114E-1 _diffrn_orient_matrix_ub_31 -0.676493E-1 _diffrn_orient_matrix_ub_32 -0.50652E-2 _diffrn_orient_matrix_ub_33 -0.29348E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0839 _diffrn_reflns_av_unetI/netI 0.0725 _diffrn_reflns_number 53413 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 26.04 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 9631 _reflns_number_gt 5923 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 -0.032 0.871 1480 135 ' ' _platon_squeeze_details The unit cell contains poorly defined hexane solvate molecules which have been treated as diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1451P)^2^+0.7731P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 9631 _refine_ls_number_parameters 408 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1337 _refine_ls_R_factor_gt 0.082 _refine_ls_wR_factor_ref 0.2539 _refine_ls_wR_factor_gt 0.2264 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.248 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.062 #----------------------------------------------------------------------------# # 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 Mg Mg 1.01371(7) 0.83579(4) 0.17517(5) 0.0331(3) Uani 1 1 d . . . O1 O 0.96956(14) 0.77852(9) 0.08902(10) 0.0401(5) Uani 1 1 d . . . O2 O 0.94202(16) 0.79767(10) 0.23293(11) 0.0477(6) Uani 1 1 d . . . N1 N 1.15286(17) 0.86903(11) 0.25868(13) 0.0368(6) Uani 1 1 d . . . N2 N 1.02860(16) 0.94281(11) 0.18612(12) 0.0320(5) Uani 1 1 d . . . C1 C 1.1229(2) 0.93507(13) 0.24085(15) 0.0313(6) Uani 1 1 d . . . C2 C 1.1914(2) 0.99640(13) 0.27948(16) 0.0358(6) Uani 1 1 d . . . C3 C 1.2590(2) 1.01862(14) 0.25214(17) 0.0424(7) Uani 1 1 d . . . C4 C 1.3202(2) 1.07652(16) 0.2880(2) 0.0575(10) Uani 1 1 d . . . H4 H 1.3656 1.0922 0.2694 0.069 Uiso 1 1 calc R . . C5 C 1.3172(3) 1.11166(16) 0.3489(2) 0.0618(11) Uani 1 1 d . . . C6 C 1.2516(3) 1.08822(16) 0.37519(19) 0.0572(10) Uani 1 1 d . . . H6 H 1.2495 1.1117 0.4178 0.069 Uiso 1 1 calc R . . C7 C 1.1875(2) 1.03100(14) 0.34170(16) 0.0426(7) Uani 1 1 d . . . C8 C 1.2688(3) 0.98133(18) 0.1879(2) 0.0573(9) Uani 1 1 d . . . H8A H 1.3154 0.9419 0.2094 0.086 Uiso 1 1 calc R . . H8B H 1.2945 1.0139 0.162 0.086 Uiso 1 1 calc R . . H8C H 1.2028 0.9638 0.1502 0.086 Uiso 1 1 calc R . . C9 C 1.3837(3) 1.17452(17) 0.3855(3) 0.1005(18) Uani 1 1 d . . . H9A H 1.4254 1.1834 0.3594 0.151 Uiso 0.5 1 calc PR . . H9B H 1.4271 1.1652 0.4408 0.151 Uiso 0.5 1 calc PR . . H9C H 1.3418 1.2157 0.3802 0.151 Uiso 0.5 1 calc PR . . H9D H 1.3708 1.1928 0.4275 0.151 Uiso 0.5 1 calc PR . . H9E H 1.3691 1.211 0.3461 0.151 Uiso 0.5 1 calc PR . . H9F H 1.4544 1.1605 0.4068 0.151 Uiso 0.5 1 calc PR . . C10 C 1.1164(3) 1.00698(17) 0.37229(19) 0.0575(9) Uani 1 1 d . . . H10A H 1.0505 0.9972 0.3286 0.086 Uiso 1 1 calc R . . H10B H 1.1097 1.0438 0.405 0.086 Uiso 1 1 calc R . . H10C H 1.1427 0.9643 0.4032 0.086 Uiso 1 1 calc R . . C11 C 1.2494(2) 0.84950(14) 0.32194(18) 0.0429(7) Uani 1 1 d . . . H11 H 1.2892 0.8931 0.345 0.052 Uiso 1 1 calc R . . C12 C 1.2354(3) 0.81066(19) 0.38450(19) 0.0577(9) Uani 1 1 d . . . H12A H 1.1907 0.7699 0.3607 0.069 Uiso 1 1 calc R . . H12B H 1.2016 0.8421 0.4061 0.069 Uiso 1 1 calc R . . C13 C 1.3336(3) 0.7849(2) 0.4507(2) 0.0788(12) Uani 1 1 d . . . H13A H 1.3755 0.8256 0.4787 0.095 Uiso 1 1 calc R . . H13B H 1.3191 0.7575 0.488 0.095 Uiso 1 1 calc R . . C14 C 1.3904(3) 0.73969(18) 0.4202(3) 0.0791(13) Uani 1 1 d . . . H14A H 1.4564 0.7269 0.4636 0.095 Uiso 1 1 calc R . . H14B H 1.3524 0.6959 0.3984 0.095 Uiso 1 1 calc R . . C15 C 1.4061(3) 0.7771(2) 0.3587(3) 0.0787(12) Uani 1 1 d . . . H15A H 1.439 0.7449 0.3372 0.094 Uiso 1 1 calc R . . H15B H 1.4515 0.8174 0.3824 0.094 Uiso 1 1 calc R . . C16 C 1.3077(2) 0.80321(19) 0.2929(2) 0.0613(9) Uani 1 1 d . . . H16A H 1.3223 0.83 0.2554 0.074 Uiso 1 1 calc R . . H16B H 1.2656 0.7624 0.2652 0.074 Uiso 1 1 calc R . . C17 C 0.9837(2) 1.01121(13) 0.15725(15) 0.0337(6) Uani 1 1 d . . . H17 H 1.0254 1.048 0.195 0.04 Uiso 1 1 calc R . . C18 C 0.8785(2) 1.01320(17) 0.15026(19) 0.0519(8) Uani 1 1 d . . . H18A H 0.8827 1.0081 0.2026 0.062 Uiso 1 1 calc R . . H18B H 0.8395 0.973 0.1183 0.062 Uiso 1 1 calc R . . C19 C 0.8228(3) 1.08147(18) 0.1133(2) 0.0641(10) Uani 1 1 d . . . H19A H 0.7537 1.0792 0.1077 0.077 Uiso 1 1 calc R . . H19B H 0.8576 1.1214 0.148 0.077 Uiso 1 1 calc R . . C20 C 0.8183(3) 1.09359(18) 0.0350(2) 0.0612(10) Uani 1 1 d . . . H20A H 0.7855 1.1392 0.0141 0.073 Uiso 1 1 calc R . . H20B H 0.7772 1.0564 -0.0014 0.073 Uiso 1 1 calc R . . C21 C 0.9229(3) 1.09336(16) 0.04055(19) 0.0527(8) Uani 1 1 d . . . H21A H 0.961 1.1343 0.0714 0.063 Uiso 1 1 calc R . . H21B H 0.9175 1.0977 -0.0122 0.063 Uiso 1 1 calc R . . C22 C 0.9794(2) 1.02640(14) 0.07846(16) 0.0396(7) Uani 1 1 d . . . H22A H 0.9465 0.9864 0.0432 0.047 Uiso 1 1 calc R . . H22B H 1.0488 1.03 0.085 0.047 Uiso 1 1 calc R . . C23 C 0.9259(2) 0.72703(14) 0.03788(15) 0.0388(7) Uani 1 1 d . . . C24 C 0.8232(2) 0.73447(16) -0.02003(17) 0.0456(8) Uani 1 1 d . . . C25 C 0.7784(3) 0.67723(18) -0.06805(19) 0.0593(9) Uani 1 1 d . . . H25 H 0.7094 0.6801 -0.1047 0.071 Uiso 1 1 calc R . . C26 C 0.8306(3) 0.61618(18) -0.0644(2) 0.0680(11) Uani 1 1 d . . . H26 H 0.7977 0.5778 -0.0976 0.082 Uiso 1 1 calc R . . C27 C 0.9303(3) 0.61205(15) -0.01224(18) 0.0554(9) Uani 1 1 d . . . H27 H 0.9665 0.5708 -0.0114 0.066 Uiso 1 1 calc R . . C28 C 0.9808(3) 0.66581(14) 0.03956(17) 0.0444(8) Uani 1 1 d . . . C29 C 0.7657(2) 0.80483(18) -0.03152(18) 0.0522(8) Uani 1 1 d . . . C30 C 0.7466(3) 0.8216(2) 0.0381(2) 0.0743(11) Uani 1 1 d . . . H30A H 0.7088 0.7831 0.0459 0.112 Uiso 1 1 calc R . . H30B H 0.7079 0.8651 0.028 0.112 Uiso 1 1 calc R . . H30C H 0.811 0.8272 0.0848 0.112 Uiso 1 1 calc R . . C31 C 0.8236(2) 0.86417(16) -0.04502(19) 0.0512(8) Uani 1 1 d . . . H31A H 0.8348 0.8531 -0.09 0.077 Uiso 1 1 calc R . . H31B H 0.8885 0.87 0.0012 0.077 Uiso 1 1 calc R . . H31C H 0.7849 0.9077 -0.055 0.077 Uiso 1 1 calc R . . C32 C 0.6630(3) 0.8026(2) -0.1040(3) 0.0831(12) Uani 1 1 d . . . H32A H 0.6724 0.7921 -0.1498 0.125 Uiso 1 1 calc R . . H32B H 0.6298 0.8482 -0.1108 0.125 Uiso 1 1 calc R . . H32C H 0.6213 0.7661 -0.0975 0.125 Uiso 1 1 calc R . . C33 C 1.0925(3) 0.65865(15) 0.09416(19) 0.0526(8) Uani 1 1 d . . . C34 C 1.1388(4) 0.5905(2) 0.0816(3) 0.0924(15) Uani 1 1 d . . . H34A H 1.1277 0.5883 0.0276 0.139 Uiso 1 1 calc R . . H34B H 1.1069 0.5499 0.0925 0.139 Uiso 1 1 calc R . . H34C H 1.2111 0.5899 0.1167 0.139 Uiso 1 1 calc R . . C35 C 1.1125(3) 0.65663(16) 0.17933(19) 0.0610(10) Uani 1 1 d . . . H35A H 1.0863 0.6995 0.1915 0.092 Uiso 1 1 calc R . . H35B H 1.185 0.6534 0.2132 0.092 Uiso 1 1 calc R . . H35C H 1.079 0.6157 0.1877 0.092 Uiso 1 1 calc R . . C36 C 1.1526(3) 0.72016(18) 0.0821(2) 0.0618(9) Uani 1 1 d . . . H36A H 1.1395 0.7214 0.0276 0.093 Uiso 1 1 calc R . . H36B H 1.2246 0.7131 0.1156 0.093 Uiso 1 1 calc R . . H36C H 1.1315 0.7646 0.0956 0.093 Uiso 1 1 calc R . . C37 C 0.9473(3) 0.82795(15) 0.30308(17) 0.0472(8) Uani 1 1 d . . . H37A H 0.8884 0.8583 0.2914 0.057 Uiso 1 1 calc R . . H37B H 1.0094 0.8558 0.3309 0.057 Uiso 1 1 calc R . . C38 C 0.9473(3) 0.76510(16) 0.34993(18) 0.0575(9) Uani 1 1 d . . . H38A H 0.9225 0.7773 0.3879 0.069 Uiso 1 1 calc R . . H38B H 1.0153 0.7445 0.3779 0.069 Uiso 1 1 calc R . . C39 C 0.8753(3) 0.71526(17) 0.28762(18) 0.0546(9) Uani 1 1 d . . . H39A H 0.8876 0.666 0.3057 0.066 Uiso 1 1 calc R . . H39B H 0.8044 0.7274 0.2724 0.066 Uiso 1 1 calc R . . C40 C 0.9000(3) 0.72687(18) 0.2228(2) 0.0670(11) Uani 1 1 d . . . H40A H 0.9496 0.6918 0.2243 0.08 Uiso 1 1 calc R . . H40B H 0.8389 0.7229 0.1722 0.08 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg 0.0426(6) 0.0281(5) 0.0282(5) -0.0047(4) 0.0158(4) -0.0053(4) O1 0.0486(12) 0.0385(11) 0.0298(10) -0.0107(8) 0.0149(9) -0.0076(9) O2 0.0731(15) 0.0429(12) 0.0359(11) -0.0115(9) 0.0324(11) -0.0229(10) N1 0.0387(14) 0.0279(12) 0.0356(13) -0.0021(10) 0.0099(11) 0.0019(10) N2 0.0333(13) 0.0291(12) 0.0318(12) -0.0023(9) 0.0133(11) 0.0008(9) C1 0.0402(17) 0.0274(14) 0.0307(14) -0.0028(11) 0.0199(13) -0.0009(11) C2 0.0377(16) 0.0277(14) 0.0337(15) 0.0005(11) 0.0092(13) 0.0043(11) C3 0.0388(17) 0.0323(15) 0.0480(18) 0.0101(13) 0.0128(14) 0.0041(12) C4 0.0362(18) 0.0351(17) 0.082(3) 0.0156(17) 0.0103(17) 0.0007(13) C5 0.044(2) 0.0272(16) 0.073(3) -0.0003(17) -0.0088(18) -0.0008(14) C6 0.056(2) 0.0335(17) 0.0448(19) -0.0113(14) -0.0089(17) 0.0128(15) C7 0.0469(18) 0.0353(15) 0.0338(16) -0.0025(13) 0.0082(14) 0.0077(13) C8 0.057(2) 0.062(2) 0.063(2) 0.0107(17) 0.0369(18) 0.0016(16) C9 0.061(3) 0.0352(19) 0.139(4) -0.012(2) -0.011(3) -0.0066(17) C10 0.081(3) 0.0513(19) 0.0416(18) -0.0078(15) 0.0296(18) 0.0092(17) C11 0.0371(17) 0.0287(14) 0.0489(18) -0.0058(13) 0.0074(14) -0.0029(12) C12 0.054(2) 0.062(2) 0.0456(19) 0.0156(16) 0.0123(16) 0.0129(16) C13 0.067(3) 0.077(3) 0.062(2) 0.027(2) 0.003(2) 0.012(2) C14 0.053(2) 0.042(2) 0.094(3) 0.018(2) -0.007(2) 0.0062(17) C15 0.048(2) 0.068(2) 0.100(3) 0.006(2) 0.017(2) 0.0168(18) C16 0.046(2) 0.062(2) 0.072(2) 0.0050(18) 0.0231(18) 0.0159(16) C17 0.0342(15) 0.0278(14) 0.0320(15) -0.0044(11) 0.0090(12) 0.0014(11) C18 0.052(2) 0.056(2) 0.0517(19) 0.0087(15) 0.0271(16) 0.0136(15) C19 0.056(2) 0.063(2) 0.077(3) 0.0159(19) 0.033(2) 0.0265(17) C20 0.058(2) 0.052(2) 0.055(2) 0.0092(16) 0.0101(18) 0.0167(16) C21 0.061(2) 0.0430(17) 0.0414(18) 0.0090(14) 0.0119(16) 0.0069(15) C22 0.0463(18) 0.0330(15) 0.0380(16) 0.0023(12) 0.0181(14) 0.0010(12) C23 0.059(2) 0.0360(16) 0.0268(14) -0.0061(12) 0.0247(14) -0.0170(13) C24 0.053(2) 0.0477(18) 0.0388(17) -0.0059(14) 0.0233(15) -0.0178(15) C25 0.062(2) 0.061(2) 0.0422(19) -0.0072(16) 0.0131(17) -0.0296(18) C26 0.101(3) 0.041(2) 0.050(2) -0.0114(16) 0.024(2) -0.031(2) C27 0.091(3) 0.0310(16) 0.0407(18) -0.0018(14) 0.0275(19) -0.0079(16) C28 0.074(2) 0.0310(15) 0.0346(16) -0.0013(12) 0.0300(16) -0.0086(14) C29 0.0410(19) 0.066(2) 0.0458(19) -0.0039(16) 0.0164(15) -0.0099(15) C30 0.061(2) 0.100(3) 0.074(3) -0.004(2) 0.042(2) 0.001(2) C31 0.051(2) 0.0489(18) 0.0494(19) -0.0003(15) 0.0196(16) 0.0045(15) C32 0.046(2) 0.090(3) 0.086(3) -0.009(2) 0.007(2) -0.007(2) C33 0.075(2) 0.0329(16) 0.0453(19) -0.0018(13) 0.0238(17) 0.0082(15) C34 0.106(4) 0.066(3) 0.089(3) -0.015(2) 0.030(3) 0.028(2) C35 0.084(3) 0.0389(18) 0.0441(19) 0.0028(14) 0.0150(18) -0.0027(16) C36 0.064(2) 0.063(2) 0.062(2) -0.0012(17) 0.033(2) 0.0052(17) C37 0.065(2) 0.0423(17) 0.0421(17) -0.0088(13) 0.0307(16) -0.0027(15) C38 0.092(3) 0.0480(19) 0.0412(18) -0.0016(15) 0.0379(19) -0.0068(17) C39 0.070(2) 0.0520(19) 0.0467(19) -0.0008(15) 0.0308(18) -0.0112(16) C40 0.102(3) 0.057(2) 0.058(2) -0.0203(17) 0.051(2) -0.043(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg O1 1.8431(19) . ? Mg O2 2.005(2) . ? Mg N2 2.054(2) . ? Mg N1 2.067(2) . ? Mg C1 2.443(3) . ? O1 C23 1.333(3) . ? O2 C37 1.443(3) . ? O2 C40 1.464(3) . ? N1 C1 1.328(3) . ? N1 C11 1.451(4) . ? N2 C1 1.329(3) . ? N2 C17 1.457(3) . ? C1 C2 1.509(4) . ? C2 C7 1.396(4) . ? C2 C3 1.404(4) . ? C3 C4 1.399(4) . ? C3 C8 1.495(4) . ? C4 C5 1.373(5) . ? C4 H4 0.95 . ? C5 C6 1.370(5) . ? C5 C9 1.511(4) . ? C6 C7 1.401(4) . ? C6 H6 0.95 . ? C7 C10 1.505(5) . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C9 H9D 0.98 . ? C9 H9E 0.98 . ? C9 H9F 0.98 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 C12 1.512(4) . ? C11 C16 1.517(4) . ? C11 H11 1 . ? C12 C13 1.524(5) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.506(6) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 C15 1.494(6) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 C16 1.524(5) . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 C22 1.522(4) . ? C17 C18 1.518(4) . ? C17 H17 1 . ? C18 C19 1.535(4) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 C20 1.502(5) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? C20 C21 1.519(5) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? C21 C22 1.522(4) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? C23 C28 1.419(4) . ? C23 C24 1.437(4) . ? C24 C25 1.391(4) . ? C24 C29 1.554(5) . ? C25 C26 1.386(5) . ? C25 H25 0.95 . ? C26 C27 1.369(5) . ? C26 H26 0.95 . ? C27 C28 1.390(4) . ? C27 H27 0.95 . ? C28 C33 1.521(5) . ? C29 C31 1.518(4) . ? C29 C30 1.531(5) . ? C29 C32 1.536(5) . ? C30 H30A 0.98 . ? C30 H30B 0.98 . ? C30 H30C 0.98 . ? C31 H31A 0.98 . ? C31 H31B 0.98 . ? C31 H31C 0.98 . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? C33 C35 1.533(5) . ? C33 C34 1.544(5) . ? C33 C36 1.559(5) . ? 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 C38 1.502(4) . ? C37 H37A 0.99 . ? C37 H37B 0.99 . ? C38 C39 1.526(5) . ? C38 H38A 0.99 . ? C38 H38B 0.99 . ? C39 C40 1.476(4) . ? C39 H39A 0.99 . ? C39 H39B 0.99 . ? C40 H40A 0.99 . ? C40 H40B 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 O1 Mg O2 103.07(9) . . ? O1 Mg N2 131.25(9) . . ? O2 Mg N2 111.31(9) . . ? O1 Mg N1 134.82(10) . . ? O2 Mg N1 106.29(9) . . ? N2 Mg N1 65.89(9) . . ? O1 Mg C1 143.83(9) . . ? O2 Mg C1 113.10(9) . . ? N2 Mg C1 32.96(8) . . ? N1 Mg C1 32.93(8) . . ? C23 O1 Mg 163.38(18) . . ? C37 O2 C40 109.3(2) . . ? C37 O2 Mg 124.41(17) . . ? C40 O2 Mg 124.46(18) . . ? C1 N1 C11 123.4(2) . . ? C1 N1 Mg 89.31(16) . . ? C11 N1 Mg 147.03(17) . . ? C1 N2 C17 122.7(2) . . ? C1 N2 Mg 89.84(15) . . ? C17 N2 Mg 147.26(17) . . ? N1 C1 N2 114.9(2) . . ? N1 C1 C2 122.3(2) . . ? N2 C1 C2 122.8(2) . . ? N1 C1 Mg 57.76(13) . . ? N2 C1 Mg 57.19(13) . . ? C2 C1 Mg 178.23(19) . . ? C7 C2 C3 120.1(3) . . ? C7 C2 C1 120.5(3) . . ? C3 C2 C1 119.4(2) . . ? C4 C3 C2 118.2(3) . . ? C4 C3 C8 119.8(3) . . ? C2 C3 C8 122.0(3) . . ? C5 C4 C3 122.7(3) . . ? C5 C4 H4 118.7 . . ? C3 C4 H4 118.7 . . ? C6 C5 C4 117.9(3) . . ? C6 C5 C9 121.0(4) . . ? C4 C5 C9 121.1(4) . . ? C5 C6 C7 122.6(3) . . ? C5 C6 H6 118.7 . . ? C7 C6 H6 118.7 . . ? C2 C7 C6 118.5(3) . . ? C2 C7 C10 120.6(3) . . ? C6 C7 C10 120.9(3) . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C9 H9D 109.5 . . ? H9A C9 H9D 141.1 . . ? H9B C9 H9D 56.3 . . ? H9C C9 H9D 56.3 . . ? C5 C9 H9E 109.5 . . ? H9A C9 H9E 56.3 . . ? H9B C9 H9E 141.1 . . ? H9C C9 H9E 56.3 . . ? H9D C9 H9E 109.5 . . ? C5 C9 H9F 109.5 . . ? H9A C9 H9F 56.3 . . ? H9B C9 H9F 56.3 . . ? H9C C9 H9F 141.1 . . ? H9D C9 H9F 109.5 . . ? H9E C9 H9F 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 110.6(2) . . ? N1 C11 C16 110.9(2) . . ? C12 C11 C16 108.9(3) . . ? N1 C11 H11 108.8 . . ? C12 C11 H11 108.8 . . ? C16 C11 H11 108.8 . . ? C11 C12 C13 113.4(3) . . ? C11 C12 H12A 108.9 . . ? C13 C12 H12A 108.9 . . ? C11 C12 H12B 108.9 . . ? C13 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? C14 C13 C12 110.9(3) . . ? C14 C13 H13A 109.5 . . ? C12 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C15 C14 C13 111.1(3) . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14B 109.4 . . ? C13 C14 H14B 109.4 . . ? H14A C14 H14B 108 . . ? C14 C15 C16 112.2(3) . . ? C14 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? C14 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C11 C16 C15 112.4(3) . . ? C11 C16 H16A 109.1 . . ? C15 C16 H16A 109.1 . . ? C11 C16 H16B 109.1 . . ? C15 C16 H16B 109.1 . . ? H16A C16 H16B 107.9 . . ? N2 C17 C22 110.8(2) . . ? N2 C17 C18 109.6(2) . . ? C22 C17 C18 109.7(2) . . ? N2 C17 H17 108.9 . . ? C22 C17 H17 108.9 . . ? C18 C17 H17 108.9 . . ? C17 C18 C19 112.5(3) . . ? C17 C18 H18A 109.1 . . ? C19 C18 H18A 109.1 . . ? C17 C18 H18B 109.1 . . ? C19 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? C20 C19 C18 111.4(3) . . ? C20 C19 H19A 109.4 . . ? C18 C19 H19A 109.4 . . ? C20 C19 H19B 109.4 . . ? C18 C19 H19B 109.4 . . ? H19A C19 H19B 108 . . ? C19 C20 C21 110.9(3) . . ? C19 C20 H20A 109.5 . . ? C21 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 108 . . ? C20 C21 C22 111.4(3) . . ? C20 C21 H21A 109.4 . . ? C22 C21 H21A 109.4 . . ? C20 C21 H21B 109.4 . . ? C22 C21 H21B 109.4 . . ? H21A C21 H21B 108 . . ? C17 C22 C21 113.7(2) . . ? C17 C22 H22A 108.8 . . ? C21 C22 H22A 108.8 . . ? C17 C22 H22B 108.8 . . ? C21 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? O1 C23 C28 120.5(3) . . ? O1 C23 C24 119.5(3) . . ? C28 C23 C24 120.1(2) . . ? C25 C24 C23 117.4(3) . . ? C25 C24 C29 121.0(3) . . ? C23 C24 C29 121.5(2) . . ? C26 C25 C24 122.5(3) . . ? C26 C25 H25 118.8 . . ? C24 C25 H25 118.8 . . ? C27 C26 C25 119.0(3) . . ? C27 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? C26 C27 C28 122.6(3) . . ? C26 C27 H27 118.7 . . ? C28 C27 H27 118.7 . . ? C27 C28 C23 118.2(3) . . ? C27 C28 C33 119.8(3) . . ? C23 C28 C33 122.0(2) . . ? C31 C29 C30 110.2(3) . . ? C31 C29 C32 106.0(3) . . ? C30 C29 C32 107.2(3) . . ? C31 C29 C24 110.3(3) . . ? C30 C29 C24 111.6(3) . . ? C32 C29 C24 111.4(3) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C28 C33 C35 111.2(3) . . ? C28 C33 C34 113.3(3) . . ? C35 C33 C34 105.4(3) . . ? C28 C33 C36 110.8(2) . . ? C35 C33 C36 109.6(3) . . ? C34 C33 C36 106.2(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 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 . . ? O2 C37 C38 103.4(2) . . ? O2 C37 H37A 111.1 . . ? C38 C37 H37A 111.1 . . ? O2 C37 H37B 111.1 . . ? C38 C37 H37B 111.1 . . ? H37A C37 H37B 109 . . ? C37 C38 C39 102.4(3) . . ? C37 C38 H38A 111.3 . . ? C39 C38 H38A 111.3 . . ? C37 C38 H38B 111.3 . . ? C39 C38 H38B 111.3 . . ? H38A C38 H38B 109.2 . . ? C40 C39 C38 102.5(3) . . ? C40 C39 H39A 111.3 . . ? C38 C39 H39A 111.3 . . ? C40 C39 H39B 111.3 . . ? C38 C39 H39B 111.3 . . ? H39A C39 H39B 109.2 . . ? O2 C40 C39 106.4(2) . . ? O2 C40 H40A 110.4 . . ? C39 C40 H40A 110.4 . . ? O2 C40 H40B 110.4 . . ? C39 C40 H40B 110.4 . . ? H40A C40 H40B 108.6 . . ? data_(4)-oct709 _database_code_depnum_ccdc_archive 'CCDC 888959' #TrackingRef 'Dalton_Mg_Comm.cif' _audit_creation_date 2009-10-21T08:17:41-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C32 H59 Mg N3 O Si2' _chemical_formula_sum 'C32 H59 Mg N3 O Si2' _chemical_formula_weight 582.31 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 11.7025(3) _cell_length_b 15.7522(2) _cell_length_c 19.5807(5) _cell_angle_alpha 90 _cell_angle_beta 93.645(1) _cell_angle_gamma 90 _cell_volume 3602.21(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 29041 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.103 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.074 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.142 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.352141E-1 _diffrn_orient_matrix_ub_12 0.57825E-1 _diffrn_orient_matrix_ub_13 0.30916E-2 _diffrn_orient_matrix_ub_21 0.36683E-1 _diffrn_orient_matrix_ub_22 -0.143729E-1 _diffrn_orient_matrix_ub_23 0.460684E-1 _diffrn_orient_matrix_ub_31 0.688911E-1 _diffrn_orient_matrix_ub_32 -0.219044E-1 _diffrn_orient_matrix_ub_33 -0.220669E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0978 _diffrn_reflns_av_unetI/netI 0.0587 _diffrn_reflns_number 56481 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 27.11 _diffrn_reflns_theta_full 27.11 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 7937 _reflns_number_gt 5634 _reflns_threshold_expression >2sigma(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, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+3.5919P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7937 _refine_ls_number_parameters 354 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.095 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1425 _refine_ls_wR_factor_gt 0.1264 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.494 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.056 #----------------------------------------------------------------------------# # 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' Si Si 0.0817 0.0704 '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 Si1 Si 0.40432(6) 0.89333(4) 0.24848(3) 0.02523(16) Uani 1 1 d . . . Si2 Si 0.49191(6) 0.83275(5) 0.11408(4) 0.03044(18) Uani 1 1 d . . . Mg Mg 0.66857(6) 0.87439(5) 0.23775(4) 0.01991(18) Uani 1 1 d . . . O O 0.73915(15) 0.97921(11) 0.19841(10) 0.0352(4) Uani 1 1 d . . . N1 N 0.79723(16) 0.78524(12) 0.25740(9) 0.0213(4) Uani 1 1 d . . . N2 N 0.73014(16) 0.86783(12) 0.33968(9) 0.0218(4) Uani 1 1 d . . . N3 N 0.50890(16) 0.86931(12) 0.19543(10) 0.0227(4) Uani 1 1 d . . . C1 C 0.79913(18) 0.80438(13) 0.32393(11) 0.0184(5) Uani 1 1 d . . . C2 C 0.86821(19) 0.75490(14) 0.37803(11) 0.0206(5) Uani 1 1 d . . . C3 C 0.9794(2) 0.77967(15) 0.39978(12) 0.0241(5) Uani 1 1 d . . . C4 C 1.0378(2) 0.73335(16) 0.45185(12) 0.0309(6) Uani 1 1 d . . . H4 H 1.113 0.7502 0.4672 0.037 Uiso 1 1 calc R . . C5 C 0.9889(2) 0.66340(17) 0.48174(13) 0.0335(6) Uani 1 1 d . . . C6 C 0.8788(2) 0.64038(15) 0.45934(12) 0.0311(6) Uani 1 1 d . . . H6 H 0.8444 0.5929 0.4798 0.037 Uiso 1 1 calc R . . C7 C 0.8165(2) 0.68491(14) 0.40750(12) 0.0244(5) Uani 1 1 d . . . C8 C 1.0356(2) 0.85506(17) 0.36883(14) 0.0350(6) Uani 1 1 d . . . H8A H 1.022 0.8534 0.3189 0.052 Uiso 1 1 calc R . . H8B H 1.1181 0.8535 0.3808 0.052 Uiso 1 1 calc R . . H8C H 1.0032 0.9074 0.3865 0.052 Uiso 1 1 calc R . . C9 C 1.0551(3) 0.6133(2) 0.53723(15) 0.0498(8) Uani 1 1 d . . . H9A H 1.1311 0.6386 0.5462 0.075 Uiso 0.5 1 calc PR . . H9B H 1.0634 0.5544 0.5222 0.075 Uiso 0.5 1 calc PR . . H9C H 1.0137 0.6145 0.5792 0.075 Uiso 0.5 1 calc PR . . H9D H 1.0077 0.5664 0.5522 0.075 Uiso 0.5 1 calc PR . . H9E H 1.0754 0.6506 0.5762 0.075 Uiso 0.5 1 calc PR . . H9F H 1.1251 0.5905 0.5192 0.075 Uiso 0.5 1 calc PR . . C10 C 0.6966(2) 0.65671(16) 0.38529(14) 0.0333(6) Uani 1 1 d . . . H10A H 0.6942 0.6379 0.3375 0.05 Uiso 1 1 calc R . . H10B H 0.6435 0.7042 0.3896 0.05 Uiso 1 1 calc R . . H10C H 0.6742 0.6096 0.4143 0.05 Uiso 1 1 calc R . . C11 C 0.87099(19) 0.71930(14) 0.23158(11) 0.0213(5) Uani 1 1 d . . . H11 H 0.921 0.6969 0.2708 0.026 Uiso 1 1 calc R . . C12 C 0.8005(2) 0.64586(15) 0.20030(13) 0.0258(5) Uani 1 1 d . . . H12A H 0.7429 0.6685 0.1658 0.031 Uiso 1 1 calc R . . H12B H 0.7591 0.6178 0.2366 0.031 Uiso 1 1 calc R . . C13 C 0.8748(2) 0.58017(15) 0.16626(13) 0.0297(6) Uani 1 1 d . . . H13A H 0.9253 0.5518 0.2017 0.036 Uiso 1 1 calc R . . H13B H 0.8248 0.5364 0.1437 0.036 Uiso 1 1 calc R . . C14 C 0.9475(2) 0.62072(16) 0.11361(13) 0.0308(6) Uani 1 1 d . . . H14A H 0.9967 0.577 0.0941 0.037 Uiso 1 1 calc R . . H14B H 0.8972 0.6447 0.0759 0.037 Uiso 1 1 calc R . . C15 C 1.0217(2) 0.69057(16) 0.14616(14) 0.0313(6) Uani 1 1 d . . . H15A H 1.0665 0.7177 0.1109 0.038 Uiso 1 1 calc R . . H15B H 1.0762 0.6659 0.1815 0.038 Uiso 1 1 calc R . . C16 C 0.9477(2) 0.75740(15) 0.17893(13) 0.0268(5) Uani 1 1 d . . . H16A H 0.8991 0.786 0.1426 0.032 Uiso 1 1 calc R . . H16B H 0.9981 0.8009 0.2016 0.032 Uiso 1 1 calc R . . C17 C 0.73890(19) 0.90569(14) 0.40831(11) 0.0211(5) Uani 1 1 d . . . H17 H 0.8038 0.8777 0.4353 0.025 Uiso 1 1 calc R . . C18 C 0.6310(2) 0.89432(15) 0.44717(12) 0.0247(5) Uani 1 1 d . . . H18A H 0.614 0.8331 0.4517 0.03 Uiso 1 1 calc R . . H18B H 0.5652 0.9213 0.4213 0.03 Uiso 1 1 calc R . . C19 C 0.6474(2) 0.93469(16) 0.51850(12) 0.0280(5) Uani 1 1 d . . . H19A H 0.5756 0.9292 0.5423 0.034 Uiso 1 1 calc R . . H19B H 0.7083 0.9038 0.5457 0.034 Uiso 1 1 calc R . . C20 C 0.6797(2) 1.02784(16) 0.51437(13) 0.0313(6) Uani 1 1 d . . . H20A H 0.6957 1.0503 0.5612 0.038 Uiso 1 1 calc R . . H20B H 0.6143 1.06 0.4928 0.038 Uiso 1 1 calc R . . C21 C 0.7843(2) 1.04106(16) 0.47328(12) 0.0293(6) Uani 1 1 d . . . H21A H 0.8523 1.0157 0.4981 0.035 Uiso 1 1 calc R . . H21B H 0.7984 1.1026 0.4681 0.035 Uiso 1 1 calc R . . C22 C 0.7666(2) 1.00027(15) 0.40270(12) 0.0255(5) Uani 1 1 d . . . H22A H 0.8368 1.0074 0.3776 0.031 Uiso 1 1 calc R . . H22B H 0.703 1.0293 0.3763 0.031 Uiso 1 1 calc R . . C23 C 0.3909(3) 0.80853(19) 0.31480(15) 0.0447(7) Uani 1 1 d . . . H23A H 0.3714 0.7545 0.2922 0.067 Uiso 1 1 calc R . . H23B H 0.3304 0.8241 0.3449 0.067 Uiso 1 1 calc R . . H23C H 0.4637 0.8027 0.3419 0.067 Uiso 1 1 calc R . . C24 C 0.4415(2) 0.99560(16) 0.29318(13) 0.0318(6) Uani 1 1 d . . . H24A H 0.4488 1.0406 0.2592 0.048 Uiso 1 1 calc R . . H24B H 0.5143 0.9892 0.3203 0.048 Uiso 1 1 calc R . . H24C H 0.381 1.0105 0.3234 0.048 Uiso 1 1 calc R . . C25 C 0.2569(2) 0.9073(2) 0.20572(16) 0.0462(8) Uani 1 1 d . . . H25A H 0.2339 0.855 0.1815 0.069 Uiso 1 1 calc R . . H25B H 0.2577 0.9543 0.173 0.069 Uiso 1 1 calc R . . H25C H 0.2025 0.9198 0.2404 0.069 Uiso 1 1 calc R . . C26 C 0.6366(3) 0.8210(2) 0.07839(14) 0.0454(7) Uani 1 1 d . . . H26A H 0.6773 0.8754 0.0818 0.068 Uiso 1 1 calc R . . H26B H 0.627 0.8038 0.0303 0.068 Uiso 1 1 calc R . . H26C H 0.6809 0.7778 0.1045 0.068 Uiso 1 1 calc R . . C27 C 0.4107(3) 0.9069(3) 0.05338(16) 0.0597(10) Uani 1 1 d . . . H27A H 0.4467 0.9631 0.0556 0.09 Uiso 1 1 calc R . . H27B H 0.3313 0.9116 0.0662 0.09 Uiso 1 1 calc R . . H27C H 0.4117 0.8848 0.0067 0.09 Uiso 1 1 calc R . . C28 C 0.4183(4) 0.7276(2) 0.1066(2) 0.0742(12) Uani 1 1 d . . . H28A H 0.3425 0.7319 0.1249 0.111 Uiso 1 1 calc R . . H28B H 0.464 0.685 0.1326 0.111 Uiso 1 1 calc R . . H28C H 0.4099 0.7108 0.0583 0.111 Uiso 1 1 calc R . . C29 C 0.8601(2) 0.9976(2) 0.20449(18) 0.0499(8) Uani 1 1 d . . . H29A H 0.9045 0.9493 0.1876 0.06 Uiso 1 1 calc R . . H29B H 0.8857 1.0086 0.2528 0.06 Uiso 1 1 calc R . . C30 C 0.8764(3) 1.0735(3) 0.1626(2) 0.0887(16) Uani 1 1 d . . . H30A H 0.9044 1.1213 0.1919 0.106 Uiso 1 1 calc R . . H30B H 0.9337 1.062 0.1286 0.106 Uiso 1 1 calc R . . C31 C 0.7675(3) 1.0950(3) 0.1280(3) 0.0874(15) Uani 1 1 d . . . H31A H 0.7662 1.0783 0.0792 0.105 Uiso 1 1 calc R . . H31B H 0.7538 1.1569 0.1306 0.105 Uiso 1 1 calc R . . C32 C 0.6797(3) 1.0485(2) 0.1629(2) 0.0569(9) Uani 1 1 d . . . H32A H 0.6428 1.0858 0.1957 0.068 Uiso 1 1 calc R . . H32B H 0.62 1.0264 0.1293 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0201(3) 0.0329(4) 0.0226(3) -0.0030(3) 0.0010(3) -0.0001(3) Si2 0.0304(4) 0.0390(4) 0.0211(4) -0.0090(3) -0.0040(3) 0.0024(3) Mg 0.0198(4) 0.0221(4) 0.0176(4) 0.0002(3) -0.0005(3) 0.0003(3) O 0.0302(10) 0.0304(10) 0.0444(11) 0.0130(8) -0.0034(8) -0.0059(8) N1 0.0221(10) 0.0236(10) 0.0183(10) -0.0035(8) 0.0014(8) 0.0022(8) N2 0.0249(10) 0.0239(10) 0.0162(9) -0.0035(7) -0.0018(8) 0.0033(8) N3 0.0220(10) 0.0275(10) 0.0181(10) -0.0034(8) -0.0017(8) 0.0001(8) C1 0.0160(11) 0.0195(11) 0.0196(11) -0.0007(8) 0.0001(9) -0.0036(8) C2 0.0251(12) 0.0205(11) 0.0162(11) -0.0033(9) 0.0007(9) 0.0033(9) C3 0.0253(12) 0.0267(12) 0.0200(12) -0.0058(9) -0.0002(10) 0.0040(10) C4 0.0311(14) 0.0371(15) 0.0236(13) -0.0101(11) -0.0061(11) 0.0131(11) C5 0.0452(16) 0.0344(14) 0.0206(13) -0.0025(10) 0.0008(11) 0.0200(12) C6 0.0465(16) 0.0252(13) 0.0224(13) 0.0045(10) 0.0092(12) 0.0094(11) C7 0.0329(13) 0.0201(12) 0.0204(12) -0.0025(9) 0.0044(10) 0.0035(10) C8 0.0267(13) 0.0415(16) 0.0361(15) -0.0004(12) -0.0040(11) -0.0064(11) C9 0.067(2) 0.0539(19) 0.0277(15) 0.0043(13) -0.0061(14) 0.0308(16) C10 0.0395(15) 0.0280(13) 0.0327(15) 0.0035(11) 0.0055(12) -0.0072(11) C11 0.0212(11) 0.0248(12) 0.0177(11) -0.0037(9) -0.0008(9) 0.0046(9) C12 0.0250(12) 0.0245(12) 0.0284(13) -0.0041(10) 0.0054(10) -0.0031(10) C13 0.0314(14) 0.0238(12) 0.0337(14) -0.0071(10) -0.0003(11) 0.0039(10) C14 0.0290(13) 0.0356(14) 0.0282(13) -0.0099(11) 0.0051(11) 0.0084(11) C15 0.0235(13) 0.0394(15) 0.0316(14) -0.0037(11) 0.0072(11) 0.0033(11) C16 0.0238(12) 0.0266(13) 0.0304(14) -0.0059(10) 0.0052(11) -0.0033(10) C17 0.0222(12) 0.0252(12) 0.0156(11) -0.0034(9) -0.0014(9) 0.0035(9) C18 0.0277(13) 0.0273(12) 0.0189(12) -0.0001(9) 0.0005(10) -0.0030(10) C19 0.0282(13) 0.0385(14) 0.0175(12) -0.0005(10) 0.0033(10) 0.0003(11) C20 0.0363(14) 0.0344(14) 0.0232(13) -0.0098(10) 0.0005(11) 0.0078(11) C21 0.0357(14) 0.0274(13) 0.0244(13) -0.0091(10) -0.0018(11) -0.0042(11) C22 0.0293(13) 0.0263(12) 0.0212(12) -0.0041(9) 0.0034(10) -0.0046(10) C23 0.0505(18) 0.0449(17) 0.0401(17) 0.0034(13) 0.0142(14) -0.0084(14) C24 0.0320(14) 0.0377(15) 0.0258(13) -0.0075(11) 0.0017(11) 0.0075(11) C25 0.0245(14) 0.068(2) 0.0462(18) -0.0122(15) 0.0011(13) 0.0031(13) C26 0.0476(18) 0.065(2) 0.0241(14) -0.0064(13) 0.0047(13) 0.0154(15) C27 0.051(2) 0.099(3) 0.0268(16) 0.0054(16) -0.0101(14) 0.0223(19) C28 0.083(3) 0.064(2) 0.076(3) -0.041(2) 0.011(2) -0.025(2) C29 0.0340(16) 0.0554(19) 0.060(2) 0.0163(16) -0.0035(15) -0.0172(14) C30 0.070(3) 0.116(4) 0.076(3) 0.063(3) -0.025(2) -0.053(2) C31 0.066(3) 0.079(3) 0.120(4) 0.065(3) 0.025(3) 0.007(2) C32 0.0477(19) 0.0378(17) 0.085(3) 0.0301(17) 0.0026(18) 0.0029(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N3 1.697(2) . ? Si1 C24 1.871(3) . ? Si1 C23 1.877(3) . ? Si1 C25 1.882(3) . ? Si1 Mg 3.1270(10) . ? Si2 N3 1.6937(19) . ? Si2 C28 1.868(3) . ? Si2 C27 1.881(3) . ? Si2 C26 1.882(3) . ? Si2 Mg 3.1515(10) . ? Mg N3 1.997(2) . ? Mg O 2.0205(18) . ? Mg N1 2.077(2) . ? Mg N2 2.081(2) . ? O C29 1.443(3) . ? O C32 1.448(3) . ? N1 C1 1.336(3) . ? N1 C11 1.461(3) . ? N2 C1 1.333(3) . ? N2 C17 1.468(3) . ? C1 C2 1.508(3) . ? C2 C3 1.399(3) . ? C2 C7 1.399(3) . ? C3 C4 1.396(3) . ? C3 C8 1.503(3) . ? C4 C5 1.388(4) . ? C4 H4 0.95 . ? C5 C6 1.382(4) . ? C5 C9 1.516(4) . ? C6 C7 1.400(3) . ? C6 H6 0.95 . ? C7 C10 1.510(3) . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C9 H9D 0.98 . ? C9 H9E 0.98 . ? C9 H9F 0.98 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 C12 1.526(3) . ? C11 C16 1.532(3) . ? C11 H11 1 . ? C12 C13 1.531(3) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.519(4) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 C15 1.517(4) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 C16 1.530(3) . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 C18 1.526(3) . ? C17 C22 1.530(3) . ? C17 H17 1 . ? C18 C19 1.536(3) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 C20 1.519(4) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? C20 C21 1.521(3) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? C21 C22 1.526(3) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? 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 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 C30 1.469(4) . ? C29 H29A 0.99 . ? C29 H29B 0.99 . ? C30 C31 1.445(5) . ? C30 H30A 0.99 . ? C30 H30B 0.99 . ? C31 C32 1.466(4) . ? C31 H31A 0.99 . ? C31 H31B 0.99 . ? C32 H32A 0.99 . ? C32 H32B 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 N3 Si1 C24 108.83(11) . . ? N3 Si1 C23 111.12(12) . . ? C24 Si1 C23 108.44(13) . . ? N3 Si1 C25 115.46(12) . . ? C24 Si1 C25 106.68(13) . . ? C23 Si1 C25 106.03(15) . . ? C24 Si1 Mg 84.94(8) . . ? C23 Si1 Mg 96.06(10) . . ? C25 Si1 Mg 149.73(10) . . ? N3 Si2 C28 113.66(15) . . ? N3 Si2 C27 114.05(13) . . ? C28 Si2 C27 106.81(19) . . ? N3 Si2 C26 109.15(12) . . ? C28 Si2 C26 107.76(16) . . ? C27 Si2 C26 104.88(15) . . ? C28 Si2 Mg 121.43(15) . . ? C27 Si2 Mg 129.55(13) . . ? C26 Si2 Mg 75.16(9) . . ? N3 Mg O 105.60(8) . . ? N3 Mg N1 134.26(8) . . ? O Mg N1 108.30(8) . . ? N3 Mg N2 130.83(8) . . ? O Mg N2 106.34(8) . . ? N1 Mg N2 65.54(7) . . ? N3 Mg Si1 29.36(6) . . ? O Mg Si1 112.19(6) . . ? N1 Mg Si1 139.50(6) . . ? N2 Mg Si1 102.94(6) . . ? C1 Mg Si1 124.72(6) . . ? N3 Mg Si2 28.60(6) . . ? O Mg Si2 98.12(6) . . ? N1 Mg Si2 115.72(6) . . ? N2 Mg Si2 153.75(6) . . ? C1 Mg Si2 141.36(6) . . ? Si1 Mg Si2 57.88(2) . . ? C29 O C32 109.1(2) . . ? C29 O Mg 123.76(16) . . ? C32 O Mg 127.08(16) . . ? C1 N1 C11 121.62(19) . . ? C1 N1 Mg 89.71(13) . . ? C11 N1 Mg 148.63(15) . . ? C1 N2 C17 120.55(19) . . ? C1 N2 Mg 89.62(13) . . ? C17 N2 Mg 149.05(15) . . ? Si2 N3 Si1 127.24(12) . . ? Si2 N3 Mg 117.05(10) . . ? Si1 N3 Mg 115.41(10) . . ? N2 C1 N1 115.0(2) . . ? N2 C1 C2 122.04(19) . . ? N1 C1 C2 122.90(19) . . ? N2 C1 Mg 57.62(11) . . ? N1 C1 Mg 57.45(11) . . ? C2 C1 Mg 173.63(15) . . ? C3 C2 C7 120.8(2) . . ? C3 C2 C1 121.1(2) . . ? C7 C2 C1 118.1(2) . . ? C4 C3 C2 118.6(2) . . ? C4 C3 C8 120.1(2) . . ? C2 C3 C8 121.3(2) . . ? C5 C4 C3 121.8(2) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C6 C5 C4 118.4(2) . . ? C6 C5 C9 121.0(3) . . ? C4 C5 C9 120.7(3) . . ? C5 C6 C7 122.0(2) . . ? C5 C6 H6 119 . . ? C7 C6 H6 119 . . ? C2 C7 C6 118.4(2) . . ? C2 C7 C10 122.1(2) . . ? C6 C7 C10 119.5(2) . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C9 H9D 109.5 . . ? H9A C9 H9D 141.1 . . ? H9B C9 H9D 56.3 . . ? H9C C9 H9D 56.3 . . ? C5 C9 H9E 109.5 . . ? H9A C9 H9E 56.3 . . ? H9B C9 H9E 141.1 . . ? H9C C9 H9E 56.3 . . ? H9D C9 H9E 109.5 . . ? C5 C9 H9F 109.5 . . ? H9A C9 H9F 56.3 . . ? H9B C9 H9F 56.3 . . ? H9C C9 H9F 141.1 . . ? H9D C9 H9F 109.5 . . ? H9E C9 H9F 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 111.21(18) . . ? N1 C11 C16 109.79(18) . . ? C12 C11 C16 110.59(19) . . ? N1 C11 H11 108.4 . . ? C12 C11 H11 108.4 . . ? C16 C11 H11 108.4 . . ? C11 C12 C13 112.34(19) . . ? C11 C12 H12A 109.1 . . ? C13 C12 H12A 109.1 . . ? C11 C12 H12B 109.1 . . ? C13 C12 H12B 109.1 . . ? H12A C12 H12B 107.9 . . ? C14 C13 C12 111.7(2) . . ? C14 C13 H13A 109.3 . . ? C12 C13 H13A 109.3 . . ? C14 C13 H13B 109.3 . . ? C12 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? C15 C14 C13 110.5(2) . . ? C15 C14 H14A 109.5 . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C14 C15 C16 110.5(2) . . ? C14 C15 H15A 109.5 . . ? C16 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C15 C16 C11 112.6(2) . . ? C15 C16 H16A 109.1 . . ? C11 C16 H16A 109.1 . . ? C15 C16 H16B 109.1 . . ? C11 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? N2 C17 C18 113.38(18) . . ? N2 C17 C22 109.43(18) . . ? C18 C17 C22 109.61(18) . . ? N2 C17 H17 108.1 . . ? C18 C17 H17 108.1 . . ? C22 C17 H17 108.1 . . ? C17 C18 C19 110.18(19) . . ? C17 C18 H18A 109.6 . . ? C19 C18 H18A 109.6 . . ? C17 C18 H18B 109.6 . . ? C19 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? C20 C19 C18 111.7(2) . . ? C20 C19 H19A 109.3 . . ? C18 C19 H19A 109.3 . . ? C20 C19 H19B 109.3 . . ? C18 C19 H19B 109.3 . . ? H19A C19 H19B 108 . . ? C19 C20 C21 111.8(2) . . ? C19 C20 H20A 109.3 . . ? C21 C20 H20A 109.3 . . ? C19 C20 H20B 109.3 . . ? C21 C20 H20B 109.3 . . ? H20A C20 H20B 107.9 . . ? C20 C21 C22 110.7(2) . . ? C20 C21 H21A 109.5 . . ? C22 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C21 C22 C17 111.23(19) . . ? C21 C22 H22A 109.4 . . ? C17 C22 H22A 109.4 . . ? C21 C22 H22B 109.4 . . ? C17 C22 H22B 109.4 . . ? H22A C22 H22B 108 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si1 C25 H25A 109.5 . . ? Si1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si2 C27 H27A 109.5 . . ? Si2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si2 C28 H28A 109.5 . . ? Si2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O C29 C30 106.2(3) . . ? O C29 H29A 110.5 . . ? C30 C29 H29A 110.5 . . ? O C29 H29B 110.5 . . ? C30 C29 H29B 110.5 . . ? H29A C29 H29B 108.7 . . ? C31 C30 C29 108.1(3) . . ? C31 C30 H30A 110.1 . . ? C29 C30 H30A 110.1 . . ? C31 C30 H30B 110.1 . . ? C29 C30 H30B 110.1 . . ? H30A C30 H30B 108.4 . . ? C30 C31 C32 106.8(3) . . ? C30 C31 H31A 110.4 . . ? C32 C31 H31A 110.4 . . ? C30 C31 H31B 110.4 . . ? C32 C31 H31B 110.4 . . ? H31A C31 H31B 108.6 . . ? O C32 C31 105.7(3) . . ? O C32 H32A 110.6 . . ? C31 C32 H32A 110.6 . . ? O C32 H32B 110.6 . . ? C31 C32 H32B 110.6 . . ? H32A C32 H32B 108.7 . . ? data_(5)-feb1308 _database_code_depnum_ccdc_archive 'CCDC 888960' #TrackingRef 'Dalton_Mg_Comm.cif' _audit_creation_date 2008-02-14T15:52:13-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C56 H78 Mg1 N2 O3, C5 H12' _chemical_formula_sum 'C61 H90 Mg N2 O3' _chemical_formula_weight 923.66 _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 13.4403(2) _cell_length_b 15.2099(3) _cell_length_c 15.6483(3) _cell_angle_alpha 89.8510(10) _cell_angle_beta 89.8010(10) _cell_angle_gamma 65.2270(10) _cell_volume 2904.51(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 23585 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.056 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.7107 _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 0.150977E-1 _diffrn_orient_matrix_ub_12 0.5489E-2 _diffrn_orient_matrix_ub_13 -0.619396E-1 _diffrn_orient_matrix_ub_21 -0.803057E-1 _diffrn_orient_matrix_ub_22 0.268542E-1 _diffrn_orient_matrix_ub_23 -0.122318E-1 _diffrn_orient_matrix_ub_31 -0.61563E-2 _diffrn_orient_matrix_ub_32 0.670221E-1 _diffrn_orient_matrix_ub_33 0.9886E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.04 _diffrn_reflns_av_unetI/netI 0.0349 _diffrn_reflns_number 43604 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 26.01 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 11356 _reflns_number_gt 8751 _reflns_threshold_expression >2sigma(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-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The disordered pentane solvate was refined isotropically, with the C1, C3 and C5 positions constrained as the same in each orientation with the EADP EXYZ commands. The hydrogen atoms on the coordinated aldehydes were located and refined; all other hydrogen atoms were placed in calculated positions. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1216P)^2^+2.1744P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 11356 _refine_ls_number_parameters 608 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0736 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1709 _refine_ls_wR_factor_gt 0.149 _refine_ls_goodness_of_fit_ref 0.791 _refine_ls_restrained_S_all 0.791 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.377 _refine_diff_density_min -0.36 _refine_diff_density_rms 0.038 #----------------------------------------------------------------------------# # 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 Mg Mg 0.96234(4) 0.76536(4) 0.20821(3) 0.02743(15) Uani 1 1 d . . . O1 O 1.10884(9) 0.72132(9) 0.17120(8) 0.0321(3) Uani 1 1 d . . . O2 O 0.90076(10) 0.66081(9) 0.20591(8) 0.0357(3) Uani 1 1 d . . . O3 O 0.90055(10) 0.79534(10) 0.07939(8) 0.0355(3) Uani 1 1 d . . . N1 N 0.83358(11) 0.88851(10) 0.25819(9) 0.0305(3) Uani 1 1 d . . . N2 N 0.95415(12) 0.77584(11) 0.34324(9) 0.0310(3) Uani 1 1 d . . . C1 C 0.86313(13) 0.85652(12) 0.33781(11) 0.0284(4) Uani 1 1 d . . . C2 C 0.79494(14) 0.90763(13) 0.41395(11) 0.0328(4) Uani 1 1 d . . . C3 C 0.80452(15) 0.98829(14) 0.44894(12) 0.0390(4) Uani 1 1 d . . . C4 C 0.73799(18) 1.03481(16) 0.51888(13) 0.0487(5) Uani 1 1 d . . . H4 H 0.7454 1.0885 0.5441 0.058 Uiso 1 1 calc R . . C5 C 0.66203(17) 1.00493(17) 0.55218(13) 0.0497(6) Uani 1 1 d . . . C6 C 0.65217(16) 0.92661(17) 0.51509(12) 0.0459(5) Uani 1 1 d . . . H6 H 0.5984 0.9069 0.5364 0.055 Uiso 1 1 calc R . . C7 C 0.71903(15) 0.87551(14) 0.44711(11) 0.0369(4) Uani 1 1 d . . . C8 C 0.88188(19) 1.02657(16) 0.41156(15) 0.0503(5) Uani 1 1 d . . . H8C H 0.9449 0.9731 0.386 0.075 Uiso 1 1 calc R . . H8B H 0.9072 1.0566 0.4568 0.075 Uiso 1 1 calc R . . H8A H 0.8439 1.0749 0.3675 0.075 Uiso 1 1 calc R . . C9 C 0.5934(2) 1.0541(2) 0.62956(16) 0.0742(9) Uani 1 1 d . . . H9F H 0.5466 1.0214 0.6451 0.111 Uiso 0.5 1 calc PR . . H9E H 0.5475 1.1221 0.6161 0.111 Uiso 0.5 1 calc PR . . H9D H 0.6416 1.0504 0.6775 0.111 Uiso 0.5 1 calc PR . . H9C H 0.6105 1.1079 0.6474 0.111 Uiso 0.5 1 calc PR . . H9B H 0.6096 1.0072 0.6764 0.111 Uiso 0.5 1 calc PR . . H9A H 0.5155 1.0789 0.615 0.111 Uiso 0.5 1 calc PR . . C10 C 0.71065(18) 0.78673(16) 0.41235(14) 0.0464(5) Uani 1 1 d . . . H10C H 0.7103 0.789 0.3498 0.07 Uiso 1 1 calc R . . H10B H 0.6427 0.7846 0.4328 0.07 Uiso 1 1 calc R . . H10A H 0.7735 0.7288 0.4319 0.07 Uiso 1 1 calc R . . C11 C 0.73680(14) 0.97816(13) 0.24115(11) 0.0317(4) Uani 1 1 d . . . H11 H 0.7127 1.0147 0.296 0.038 Uiso 1 1 calc R . . C12 C 0.76417(15) 1.04084(14) 0.17789(13) 0.0389(4) Uani 1 1 d . . . H12B H 0.7911 1.0045 0.124 0.047 Uiso 1 1 calc R . . H12A H 0.8235 1.0558 0.2015 0.047 Uiso 1 1 calc R . . C13 C 0.66472(17) 1.13532(15) 0.15877(16) 0.0479(5) Uani 1 1 d . . . H13B H 0.6412 1.1743 0.2117 0.057 Uiso 1 1 calc R . . H13A H 0.685 1.1732 0.1161 0.057 Uiso 1 1 calc R . . C14 C 0.57059(18) 1.11535(17) 0.12459(18) 0.0569(6) Uani 1 1 d . . . H14B H 0.5057 1.1774 0.1162 0.068 Uiso 1 1 calc R . . H14A H 0.5913 1.0829 0.0684 0.068 Uiso 1 1 calc R . . C15 C 0.54154(17) 1.05169(17) 0.18544(18) 0.0541(6) Uani 1 1 d . . . H15B H 0.4844 1.0355 0.1592 0.065 Uiso 1 1 calc R . . H15A H 0.5112 1.0877 0.2389 0.065 Uiso 1 1 calc R . . C16 C 0.64199(15) 0.95809(14) 0.20633(14) 0.0395(4) Uani 1 1 d . . . H16B H 0.6214 0.9206 0.2492 0.047 Uiso 1 1 calc R . . H16A H 0.6664 0.9182 0.154 0.047 Uiso 1 1 calc R . . C17 C 0.99835(15) 0.72966(14) 0.42497(11) 0.0342(4) Uani 1 1 d . . . H17 H 0.9395 0.7556 0.4693 0.041 Uiso 1 1 calc R . . C18 C 1.0345(2) 0.62113(15) 0.41786(14) 0.0489(5) Uani 1 1 d . . . H18B H 1.0872 0.596 0.37 0.059 Uiso 1 1 calc R . . H18A H 0.97 0.608 0.4046 0.059 Uiso 1 1 calc R . . C19 C 1.0880(2) 0.56759(19) 0.49992(16) 0.0626(7) Uani 1 1 d . . . H19B H 1.0328 0.5866 0.5463 0.075 Uiso 1 1 calc R . . H19A H 1.1146 0.497 0.4908 0.075 Uiso 1 1 calc R . . C20 C 1.1835(2) 0.5903(2) 0.52657(15) 0.0637(7) Uani 1 1 d . . . H20B H 1.2131 0.5584 0.5818 0.076 Uiso 1 1 calc R . . H20A H 1.2427 0.5646 0.4833 0.076 Uiso 1 1 calc R . . C21 C 1.1469(2) 0.6983(2) 0.53525(16) 0.0634(7) Uani 1 1 d . . . H21B H 1.2108 0.7119 0.5496 0.076 Uiso 1 1 calc R . . H21A H 1.0932 0.7229 0.5825 0.076 Uiso 1 1 calc R . . C22 C 1.09477(19) 0.75105(17) 0.45233(15) 0.0519(5) Uani 1 1 d . . . H22B H 1.0692 0.8217 0.4607 0.062 Uiso 1 1 calc R . . H22A H 1.1507 0.7308 0.4064 0.062 Uiso 1 1 calc R . . C23 C 1.19840(13) 0.70384(13) 0.12595(11) 0.0298(4) Uani 1 1 d . . . C24 C 1.23594(14) 0.77781(13) 0.11313(11) 0.0317(4) Uani 1 1 d . . . C25 C 1.32455(15) 0.75902(15) 0.05841(12) 0.0390(4) Uani 1 1 d . . . H25 H 1.3483 0.8087 0.0479 0.047 Uiso 1 1 calc R . . C26 C 1.37899(16) 0.67023(16) 0.01886(13) 0.0449(5) Uani 1 1 d . . . H26 H 1.438 0.6599 -0.0193 0.054 Uiso 1 1 calc R . . C27 C 1.34697(16) 0.59741(15) 0.03528(13) 0.0424(5) Uani 1 1 d . . . H27 H 1.3865 0.536 0.0095 0.051 Uiso 1 1 calc R . . C28 C 1.25822(14) 0.60999(13) 0.08863(12) 0.0347(4) Uani 1 1 d . . . C29 C 1.18235(15) 0.87666(13) 0.15868(12) 0.0358(4) Uani 1 1 d . . . C30 C 1.06444(16) 0.93521(14) 0.12695(15) 0.0445(5) Uani 1 1 d . . . H30C H 1.0324 0.9976 0.1567 0.067 Uiso 1 1 calc R . . H30B H 1.0204 0.899 0.1387 0.067 Uiso 1 1 calc R . . H30A H 1.0655 0.9463 0.0653 0.067 Uiso 1 1 calc R . . C31 C 1.1816(2) 0.86235(17) 0.25559(13) 0.0502(5) Uani 1 1 d . . . H31C H 1.2571 0.8286 0.2761 0.075 Uiso 1 1 calc R . . H31B H 1.1408 0.8237 0.2691 0.075 Uiso 1 1 calc R . . H31A H 1.1465 0.9256 0.2836 0.075 Uiso 1 1 calc R . . C32 C 1.24361(18) 0.94044(16) 0.14165(16) 0.0501(5) Uani 1 1 d . . . H32C H 1.3198 0.9065 0.1606 0.075 Uiso 1 1 calc R . . H32B H 1.208 1.0014 0.1732 0.075 Uiso 1 1 calc R . . H32A H 1.2421 0.9542 0.0803 0.075 Uiso 1 1 calc R . . C33 C 1.22587(16) 0.52576(14) 0.10476(14) 0.0428(5) Uani 1 1 d . . . C34 C 1.3122(2) 0.42921(17) 0.0698(2) 0.0656(7) Uani 1 1 d . . . H34C H 1.3838 0.4163 0.0947 0.098 Uiso 1 1 calc R . . H34B H 1.3163 0.4332 0.0075 0.098 Uiso 1 1 calc R . . H34A H 1.2913 0.3767 0.0851 0.098 Uiso 1 1 calc R . . C35 C 1.2162(2) 0.51017(16) 0.20063(15) 0.0528(6) Uani 1 1 d . . . H35C H 1.1597 0.569 0.2257 0.079 Uiso 1 1 calc R . . H35B H 1.2866 0.4957 0.2283 0.079 Uiso 1 1 calc R . . H35A H 1.196 0.4559 0.2092 0.079 Uiso 1 1 calc R . . C36 C 1.11759(18) 0.54464(17) 0.05926(16) 0.0530(6) Uani 1 1 d . . . H36C H 1.1 0.4888 0.0673 0.079 Uiso 1 1 calc R . . H36B H 1.1251 0.5545 -0.0019 0.079 Uiso 1 1 calc R . . H36A H 1.0587 0.6026 0.0834 0.079 Uiso 1 1 calc R . . C37 C 0.80397(16) 0.67771(14) 0.19508(12) 0.0351(4) Uani 1 1 d . . . H2 H 0.7524(18) 0.7430(17) 0.1818(14) 0.043(6) Uiso 1 1 d . . . C38 C 0.75618(15) 0.60853(13) 0.20115(11) 0.0341(4) Uani 1 1 d . . . C39 C 0.64250(16) 0.64168(15) 0.18523(13) 0.0420(5) Uani 1 1 d . . . C40 C 0.59497(18) 0.57671(17) 0.18981(15) 0.0490(5) Uani 1 1 d . . . H40 H 0.5191 0.5986 0.1776 0.059 Uiso 1 1 calc R . . C41 C 0.65521(19) 0.48070(17) 0.21167(14) 0.0494(5) Uani 1 1 d . . . C42 C 0.76640(19) 0.44942(16) 0.22743(14) 0.0480(5) Uani 1 1 d . . . H42 H 0.8081 0.3834 0.242 0.058 Uiso 1 1 calc R . . C43 C 0.81893(17) 0.50998(14) 0.22289(13) 0.0402(4) Uani 1 1 d . . . C44 C 0.56967(19) 0.74620(18) 0.1642(2) 0.0657(7) Uani 1 1 d . . . H44C H 0.4935 0.7545 0.1596 0.099 Uiso 1 1 calc R . . H44B H 0.593 0.7637 0.1098 0.099 Uiso 1 1 calc R . . H44A H 0.5753 0.7881 0.2096 0.099 Uiso 1 1 calc R . . C45 C 0.6015(2) 0.4111(2) 0.2178(2) 0.0710(8) Uani 1 1 d . . . H45F H 0.6563 0.3469 0.2343 0.107 Uiso 0.5 1 calc PR . . H45E H 0.5704 0.407 0.1622 0.107 Uiso 0.5 1 calc PR . . H45D H 0.5431 0.4344 0.2608 0.107 Uiso 0.5 1 calc PR . . H45C H 0.5235 0.4453 0.2039 0.107 Uiso 0.5 1 calc PR . . H45B H 0.6095 0.3852 0.276 0.107 Uiso 0.5 1 calc PR . . H45A H 0.6368 0.3578 0.1774 0.107 Uiso 0.5 1 calc PR . . C46 C 0.94018(19) 0.46974(16) 0.2407(2) 0.0629(7) Uani 1 1 d . . . H46C H 0.9671 0.4013 0.2566 0.094 Uiso 1 1 calc R . . H46B H 0.9535 0.5059 0.2877 0.094 Uiso 1 1 calc R . . H46A H 0.9788 0.4759 0.1894 0.094 Uiso 1 1 calc R . . C47 C 0.95758(15) 0.78970(13) 0.01613(11) 0.0324(4) Uani 1 1 d . . . H1 H 1.0309(17) 0.7816(14) 0.0242(12) 0.032(5) Uiso 1 1 d . . . C48 C 0.92364(14) 0.79432(12) -0.07255(11) 0.0309(4) Uani 1 1 d . . . C49 C 0.81990(15) 0.79926(13) -0.09597(12) 0.0347(4) Uani 1 1 d . . . C50 C 0.79680(16) 0.79877(14) -0.18220(12) 0.0416(5) Uani 1 1 d . . . H50 H 0.7282 0.8 -0.1986 0.05 Uiso 1 1 calc R . . C51 C 0.87052(18) 0.79654(15) -0.24528(12) 0.0455(5) Uani 1 1 d . . . C52 C 0.96997(17) 0.79487(14) -0.22108(12) 0.0419(5) Uani 1 1 d . . . H52 H 1.0196 0.7956 -0.2642 0.05 Uiso 1 1 calc R . . C53 C 0.99999(15) 0.79217(13) -0.13585(11) 0.0345(4) Uani 1 1 d . . . C54 C 0.73399(17) 0.80533(18) -0.03155(14) 0.0488(5) Uani 1 1 d . . . H54C H 0.6686 0.8084 -0.0613 0.073 Uiso 1 1 calc R . . H54B H 0.7147 0.8636 0.0033 0.073 Uiso 1 1 calc R . . H54A H 0.7626 0.748 0.0053 0.073 Uiso 1 1 calc R . . C55 C 0.8430(2) 0.7944(2) -0.33844(15) 0.0717(8) Uani 1 1 d . . . H55F H 0.77 0.7952 -0.3435 0.108 Uiso 0.5 1 calc PR . . H55E H 0.8973 0.7355 -0.3649 0.108 Uiso 0.5 1 calc PR . . H55D H 0.8439 0.8513 -0.3674 0.108 Uiso 0.5 1 calc PR . . H55C H 0.9042 0.7928 -0.3738 0.108 Uiso 0.5 1 calc PR . . H55B H 0.7769 0.8525 -0.3523 0.108 Uiso 0.5 1 calc PR . . H55A H 0.8303 0.7367 -0.3498 0.108 Uiso 0.5 1 calc PR . . C56 C 1.11182(16) 0.78658(16) -0.11468(13) 0.0425(5) Uani 1 1 d . . . H56C H 1.1502 0.7881 -0.1676 0.064 Uiso 1 1 calc R . . H56B H 1.154 0.7262 -0.0839 0.064 Uiso 1 1 calc R . . H56A H 1.104 0.8418 -0.0787 0.064 Uiso 1 1 calc R . . C1A C 0.4291(5) 0.6318(5) 0.3857(4) 0.157(2) Uiso 0.515(7) 1 d P A 1 H1A1 H 0.4572 0.5882 0.3368 0.236 Uiso 0.515(7) 1 calc PR A 1 H1A2 H 0.3956 0.699 0.3656 0.236 Uiso 0.515(7) 1 calc PR A 1 H1A3 H 0.3739 0.617 0.416 0.236 Uiso 0.515(7) 1 calc PR A 1 C2A C 0.5233(7) 0.6182(6) 0.4464(5) 0.103(3) Uiso 0.515(7) 1 d P A 1 H2A1 H 0.5576 0.549 0.4629 0.123 Uiso 0.515(7) 1 calc PR A 1 H2A2 H 0.5787 0.6309 0.4131 0.123 Uiso 0.515(7) 1 calc PR A 1 C3A C 0.5041(4) 0.6722(4) 0.5215(4) 0.1322(16) Uiso 0.515(7) 1 d P A 1 H3A1 H 0.4426 0.6657 0.5516 0.159 Uiso 0.515(7) 1 calc PR A 1 H3A2 H 0.4781 0.741 0.5047 0.159 Uiso 0.515(7) 1 calc PR A 1 C4A C 0.5960(6) 0.6510(5) 0.5868(4) 0.085(2) Uiso 0.515(7) 1 d P A 1 H4A1 H 0.6153 0.5851 0.6098 0.102 Uiso 0.515(7) 1 calc PR A 1 H4A2 H 0.661 0.649 0.5556 0.102 Uiso 0.515(7) 1 calc PR A 1 C5A C 0.5789(5) 0.7114(4) 0.6545(4) 0.1442(18) Uiso 0.515(7) 1 d P A 1 H5A1 H 0.645 0.6886 0.6899 0.216 Uiso 0.515(7) 1 calc PR A 1 H5A2 H 0.5172 0.7122 0.6886 0.216 Uiso 0.515(7) 1 calc PR A 1 H5A3 H 0.5623 0.7769 0.6338 0.216 Uiso 0.515(7) 1 calc PR A 1 C1B C 0.4291(5) 0.6318(5) 0.3857(4) 0.157(2) Uiso 0.485(7) 1 d P A 2 H1B1 H 0.359 0.6643 0.3559 0.236 Uiso 0.485(7) 1 calc PR A 2 H1B2 H 0.4399 0.566 0.4014 0.236 Uiso 0.485(7) 1 calc PR A 2 H1B3 H 0.4888 0.6289 0.3482 0.236 Uiso 0.485(7) 1 calc PR A 2 C2B C 0.4283(13) 0.6765(12) 0.4495(10) 0.178(6) Uiso 0.485(7) 1 d P A 2 H2B1 H 0.363 0.6784 0.4803 0.214 Uiso 0.485(7) 1 calc PR A 2 H2B2 H 0.4063 0.743 0.4273 0.214 Uiso 0.485(7) 1 calc PR A 2 C3B C 0.5041(4) 0.6722(4) 0.5215(4) 0.1322(16) Uiso 0.485(7) 1 d P A 2 H3B1 H 0.5225 0.6084 0.5487 0.159 Uiso 0.485(7) 1 calc PR A 2 H3B2 H 0.5721 0.6669 0.4928 0.159 Uiso 0.485(7) 1 calc PR A 2 C4B C 0.4922(11) 0.7276(10) 0.5816(8) 0.157(5) Uiso 0.485(7) 1 d P A 2 H4B1 H 0.4237 0.735 0.6108 0.189 Uiso 0.485(7) 1 calc PR A 2 H4B2 H 0.4776 0.7913 0.5559 0.189 Uiso 0.485(7) 1 calc PR A 2 C5B C 0.5789(5) 0.7114(4) 0.6545(4) 0.1442(18) Uiso 0.485(7) 1 d P A 2 H5B1 H 0.5505 0.7656 0.6947 0.216 Uiso 0.485(7) 1 calc PR A 2 H5B2 H 0.6475 0.7075 0.6292 0.216 Uiso 0.485(7) 1 calc PR A 2 H5B3 H 0.5927 0.6509 0.6848 0.216 Uiso 0.485(7) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg 0.0246(3) 0.0308(3) 0.0254(3) -0.0014(2) 0.0009(2) -0.0101(2) O1 0.0252(6) 0.0350(7) 0.0334(7) -0.0039(5) 0.0039(5) -0.0098(5) O2 0.0334(7) 0.0355(7) 0.0387(7) -0.0012(5) -0.0019(5) -0.0149(6) O3 0.0330(7) 0.0444(7) 0.0278(6) -0.0011(5) -0.0009(5) -0.0148(6) N1 0.0280(7) 0.0311(8) 0.0277(7) 0.0013(6) 0.0014(6) -0.0077(6) N2 0.0294(7) 0.0333(8) 0.0257(7) 0.0001(6) -0.0004(6) -0.0086(6) C1 0.0268(8) 0.0311(9) 0.0283(9) -0.0010(7) 0.0010(6) -0.0130(7) C2 0.0290(9) 0.0352(9) 0.0274(9) -0.0012(7) -0.0003(7) -0.0069(8) C3 0.0356(10) 0.0386(10) 0.0343(10) -0.0049(8) -0.0047(8) -0.0072(8) C4 0.0458(12) 0.0489(12) 0.0363(11) -0.0135(9) -0.0060(9) -0.0047(10) C5 0.0362(11) 0.0614(14) 0.0306(10) -0.0089(9) -0.0014(8) 0.0000(10) C6 0.0312(10) 0.0660(14) 0.0292(10) 0.0039(9) 0.0030(8) -0.0091(9) C7 0.0297(9) 0.0463(11) 0.0284(9) 0.0028(8) -0.0007(7) -0.0099(8) C8 0.0536(13) 0.0450(12) 0.0542(13) -0.0089(10) -0.0054(10) -0.0225(10) C9 0.0550(15) 0.097(2) 0.0413(13) -0.0216(13) 0.0085(11) -0.0028(14) C10 0.0436(11) 0.0543(13) 0.0449(12) 0.0029(9) 0.0053(9) -0.0242(10) C11 0.0284(9) 0.0307(9) 0.0314(9) 0.0007(7) 0.0008(7) -0.0079(7) C12 0.0300(9) 0.0392(10) 0.0464(11) 0.0098(8) -0.0042(8) -0.0134(8) C13 0.0391(11) 0.0395(11) 0.0636(14) 0.0179(10) -0.0090(10) -0.0150(9) C14 0.0373(11) 0.0487(13) 0.0797(17) 0.0226(11) -0.0186(11) -0.0131(10) C15 0.0300(10) 0.0481(13) 0.0831(17) 0.0133(11) -0.0100(10) -0.0152(9) C16 0.0312(9) 0.0349(10) 0.0521(12) 0.0046(8) -0.0009(8) -0.0135(8) C17 0.0319(9) 0.0412(10) 0.0234(8) 0.0012(7) -0.0006(7) -0.0093(8) C18 0.0603(13) 0.0419(11) 0.0406(11) 0.0076(9) -0.0089(10) -0.0176(10) C19 0.0711(16) 0.0534(14) 0.0515(14) 0.0195(11) -0.0093(12) -0.0145(12) C20 0.0489(13) 0.0739(17) 0.0431(12) 0.0194(11) -0.0070(10) -0.0010(12) C21 0.0546(14) 0.0809(18) 0.0483(13) 0.0078(12) -0.0230(11) -0.0220(13) C22 0.0508(13) 0.0536(13) 0.0520(13) 0.0087(10) -0.0197(10) -0.0224(11) C23 0.0235(8) 0.0348(9) 0.0264(8) -0.0012(7) -0.0007(6) -0.0076(7) C24 0.0254(8) 0.0348(9) 0.0311(9) 0.0021(7) -0.0035(7) -0.0088(7) C25 0.0310(9) 0.0454(11) 0.0402(10) 0.0048(8) 0.0008(8) -0.0156(8) C26 0.0327(10) 0.0530(12) 0.0445(11) -0.0038(9) 0.0124(8) -0.0135(9) C27 0.0328(10) 0.0419(11) 0.0445(11) -0.0094(8) 0.0103(8) -0.0077(9) C28 0.0275(9) 0.0355(10) 0.0363(10) -0.0033(7) 0.0018(7) -0.0083(8) C29 0.0309(9) 0.0346(10) 0.0410(10) -0.0013(8) -0.0014(7) -0.0129(8) C30 0.0321(10) 0.0338(10) 0.0623(13) -0.0019(9) -0.0025(9) -0.0085(8) C31 0.0609(14) 0.0512(13) 0.0411(11) -0.0092(9) -0.0037(10) -0.0258(11) C32 0.0399(11) 0.0393(11) 0.0725(15) -0.0040(10) 0.0021(10) -0.0180(9) C33 0.0353(10) 0.0336(10) 0.0544(12) -0.0094(9) 0.0105(9) -0.0096(8) C34 0.0565(14) 0.0395(12) 0.097(2) -0.0186(12) 0.0256(14) -0.0159(11) C35 0.0527(13) 0.0396(11) 0.0615(14) 0.0070(10) 0.0079(10) -0.0149(10) C36 0.0477(12) 0.0503(13) 0.0643(15) -0.0151(11) 0.0068(10) -0.0239(11) C37 0.0351(10) 0.0336(10) 0.0358(10) 0.0005(7) -0.0032(7) -0.0135(8) C38 0.0362(10) 0.0347(10) 0.0329(9) -0.0006(7) -0.0015(7) -0.0164(8) C39 0.0396(11) 0.0439(11) 0.0460(11) -0.0001(9) -0.0035(8) -0.0209(9) C40 0.0436(11) 0.0585(14) 0.0536(13) -0.0054(10) 0.0014(9) -0.0301(11) C41 0.0596(13) 0.0523(13) 0.0500(12) -0.0078(10) 0.0056(10) -0.0370(11) C42 0.0588(13) 0.0373(11) 0.0519(13) -0.0004(9) -0.0023(10) -0.0239(10) C43 0.0442(11) 0.0353(10) 0.0424(11) -0.0025(8) -0.0026(8) -0.0179(9) C44 0.0373(12) 0.0498(14) 0.111(2) 0.0121(14) -0.0210(13) -0.0186(11) C45 0.0809(19) 0.0711(17) 0.085(2) -0.0063(14) 0.0071(15) -0.0553(16) C46 0.0509(13) 0.0330(11) 0.102(2) 0.0064(12) -0.0203(13) -0.0144(10) C47 0.0315(9) 0.0370(10) 0.0295(9) -0.0011(7) -0.0021(7) -0.0152(8) C48 0.0335(9) 0.0293(9) 0.0278(9) -0.0009(7) -0.0025(7) -0.0111(7) C49 0.0353(9) 0.0321(9) 0.0338(9) -0.0023(7) -0.0046(7) -0.0114(8) C50 0.0385(10) 0.0400(11) 0.0381(11) -0.0043(8) -0.0125(8) -0.0082(9) C51 0.0479(12) 0.0426(11) 0.0282(10) -0.0015(8) -0.0094(8) -0.0014(9) C52 0.0452(11) 0.0390(11) 0.0283(9) 0.0007(8) 0.0030(8) -0.0048(9) C53 0.0374(10) 0.0305(9) 0.0305(9) 0.0003(7) -0.0005(7) -0.0091(8) C54 0.0389(11) 0.0694(15) 0.0444(12) -0.0026(10) -0.0042(9) -0.0288(11) C55 0.0617(15) 0.094(2) 0.0338(12) -0.0063(12) -0.0137(11) -0.0071(14) C56 0.0401(11) 0.0495(12) 0.0379(10) -0.0011(9) 0.0048(8) -0.0188(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg O1 1.8842(13) . ? Mg O2 2.0780(14) . ? Mg N1 2.0967(15) . ? Mg N2 2.1184(15) . ? Mg O3 2.1566(13) . ? Mg C1 2.5019(17) . ? O1 C23 1.322(2) . ? O2 C37 1.228(2) . ? O3 C47 1.231(2) . ? N1 C1 1.336(2) . ? N1 C11 1.462(2) . ? N2 C1 1.324(2) . ? N2 C17 1.460(2) . ? C1 C2 1.505(2) . ? C2 C3 1.399(3) . ? C2 C7 1.401(3) . ? C3 C4 1.402(3) . ? C3 C8 1.505(3) . ? C4 C5 1.380(4) . ? C4 H4 0.95 . ? C5 C6 1.382(3) . ? C5 C9 1.515(3) . ? C6 C7 1.398(3) . ? C6 H6 0.95 . ? C7 C10 1.505(3) . ? C8 H8C 0.98 . ? C8 H8B 0.98 . ? C8 H8A 0.98 . ? C9 H9F 0.98 . ? C9 H9E 0.98 . ? C9 H9D 0.98 . ? C9 H9C 0.98 . ? C9 H9B 0.98 . ? C9 H9A 0.98 . ? C10 H10C 0.98 . ? C10 H10B 0.98 . ? C10 H10A 0.98 . ? C11 C12 1.520(3) . ? C11 C16 1.531(3) . ? C11 H11 1 . ? C12 C13 1.527(3) . ? C12 H12B 0.99 . ? C12 H12A 0.99 . ? C13 C14 1.519(3) . ? C13 H13B 0.99 . ? C13 H13A 0.99 . ? C14 C15 1.519(3) . ? C14 H14B 0.99 . ? C14 H14A 0.99 . ? C15 C16 1.532(3) . ? C15 H15B 0.99 . ? C15 H15A 0.99 . ? C16 H16B 0.99 . ? C16 H16A 0.99 . ? C17 C18 1.517(3) . ? C17 C22 1.525(3) . ? C17 H17 1 . ? C18 C19 1.530(3) . ? C18 H18B 0.99 . ? C18 H18A 0.99 . ? C19 C20 1.522(4) . ? C19 H19B 0.99 . ? C19 H19A 0.99 . ? C20 C21 1.510(4) . ? C20 H20B 0.99 . ? C20 H20A 0.99 . ? C21 C22 1.532(3) . ? C21 H21B 0.99 . ? C21 H21A 0.99 . ? C22 H22B 0.99 . ? C22 H22A 0.99 . ? C23 C24 1.426(3) . ? C23 C28 1.437(2) . ? C24 C25 1.394(3) . ? C24 C29 1.543(3) . ? C25 C26 1.384(3) . ? C25 H25 0.95 . ? C26 C27 1.369(3) . ? C26 H26 0.95 . ? C27 C28 1.400(3) . ? C27 H27 0.95 . ? C28 C33 1.536(3) . ? C29 C31 1.532(3) . ? C29 C32 1.535(3) . ? C29 C30 1.540(3) . ? C30 H30C 0.98 . ? C30 H30B 0.98 . ? C30 H30A 0.98 . ? C31 H31C 0.98 . ? C31 H31B 0.98 . ? C31 H31A 0.98 . ? C32 H32C 0.98 . ? C32 H32B 0.98 . ? C32 H32A 0.98 . ? C33 C35 1.532(3) . ? C33 C36 1.537(3) . ? C33 C34 1.541(3) . ? C34 H34C 0.98 . ? C34 H34B 0.98 . ? C34 H34A 0.98 . ? C35 H35C 0.98 . ? C35 H35B 0.98 . ? C35 H35A 0.98 . ? C36 H36C 0.98 . ? C36 H36B 0.98 . ? C36 H36A 0.98 . ? C37 C38 1.447(3) . ? C37 H2 0.97(2) . ? C38 C39 1.417(3) . ? C38 C43 1.419(3) . ? C39 C40 1.385(3) . ? C39 C44 1.513(3) . ? C40 C41 1.383(3) . ? C40 H40 0.95 . ? C41 C42 1.388(3) . ? C41 C45 1.513(3) . ? C42 C43 1.377(3) . ? C42 H42 0.95 . ? C43 C46 1.508(3) . ? C44 H44C 0.98 . ? C44 H44B 0.98 . ? C44 H44A 0.98 . ? C45 H45F 0.98 . ? C45 H45E 0.98 . ? C45 H45D 0.98 . ? C45 H45C 0.98 . ? C45 H45B 0.98 . ? C45 H45A 0.98 . ? C46 H46C 0.98 . ? C46 H46B 0.98 . ? C46 H46A 0.98 . ? C47 C48 1.455(2) . ? C47 H1 0.95(2) . ? C48 C49 1.414(3) . ? C48 C53 1.414(3) . ? C49 C50 1.386(3) . ? C49 C54 1.504(3) . ? C50 C51 1.387(3) . ? C50 H50 0.95 . ? C51 C52 1.380(3) . ? C51 C55 1.509(3) . ? C52 C53 1.390(3) . ? C52 H52 0.95 . ? C53 C56 1.507(3) . ? C54 H54C 0.98 . ? C54 H54B 0.98 . ? C54 H54A 0.98 . ? C55 H55F 0.98 . ? C55 H55E 0.98 . ? C55 H55D 0.98 . ? C55 H55C 0.98 . ? C55 H55B 0.98 . ? C55 H55A 0.98 . ? C56 H56C 0.98 . ? C56 H56B 0.98 . ? C56 H56A 0.98 . ? C1A C2A 1.528(10) . ? C1A H1A1 0.98 . ? C1A H1A2 0.98 . ? C1A H1A3 0.98 . ? C2A C3A 1.395(9) . ? C2A H2A1 0.99 . ? C2A H2A2 0.99 . ? C3A C4A 1.532(8) . ? C3A H3A1 0.99 . ? C3A H3A2 0.99 . ? C4A C5A 1.358(8) . ? C4A H4A1 0.99 . ? C4A H4A2 0.99 . ? C5A H5A1 0.98 . ? C5A H5A2 0.98 . ? C5A H5A3 0.98 . ? C2B H2B1 0.99 . ? C2B H2B2 0.99 . ? C4B H4B1 0.99 . ? C4B H4B2 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 O1 Mg O2 114.43(6) . . ? O1 Mg N1 141.21(6) . . ? O2 Mg N1 104.30(6) . . ? O1 Mg N2 110.13(6) . . ? O2 Mg N2 93.07(6) . . ? N1 Mg N2 64.14(6) . . ? O1 Mg O3 92.44(5) . . ? O2 Mg O3 84.31(5) . . ? N1 Mg O3 93.38(6) . . ? N2 Mg O3 156.06(6) . . ? O1 Mg C1 132.74(6) . . ? O2 Mg C1 98.64(6) . . ? N1 Mg C1 32.27(6) . . ? N2 Mg C1 31.94(6) . . ? O3 Mg C1 124.90(6) . . ? C23 O1 Mg 164.09(12) . . ? C37 O2 Mg 124.71(12) . . ? C47 O3 Mg 124.23(12) . . ? C1 N1 C11 121.53(14) . . ? C1 N1 Mg 90.80(10) . . ? C11 N1 Mg 147.55(12) . . ? C1 N2 C17 122.32(14) . . ? C1 N2 Mg 90.20(10) . . ? C17 N2 Mg 147.10(12) . . ? N2 C1 N1 114.61(15) . . ? N2 C1 C2 123.63(15) . . ? N1 C1 C2 121.73(15) . . ? N2 C1 Mg 57.86(9) . . ? N1 C1 Mg 56.93(9) . . ? C2 C1 Mg 174.28(13) . . ? C3 C2 C7 120.62(17) . . ? C3 C2 C1 120.31(17) . . ? C7 C2 C1 119.03(17) . . ? C2 C3 C4 118.4(2) . . ? C2 C3 C8 121.33(17) . . ? C4 C3 C8 120.22(19) . . ? C5 C4 C3 121.9(2) . . ? C5 C4 H4 119 . . ? C3 C4 H4 119 . . ? C4 C5 C6 118.50(18) . . ? C4 C5 C9 121.2(2) . . ? C6 C5 C9 120.3(2) . . ? C5 C6 C7 121.9(2) . . ? C5 C6 H6 119 . . ? C7 C6 H6 119 . . ? C6 C7 C2 118.52(19) . . ? C6 C7 C10 120.21(18) . . ? C2 C7 C10 121.25(17) . . ? C3 C8 H8C 109.5 . . ? C3 C8 H8B 109.5 . . ? H8C C8 H8B 109.5 . . ? C3 C8 H8A 109.5 . . ? H8C C8 H8A 109.5 . . ? H8B C8 H8A 109.5 . . ? C5 C9 H9F 109.5 . . ? C5 C9 H9E 109.5 . . ? H9F C9 H9E 109.5 . . ? C5 C9 H9D 109.5 . . ? H9F C9 H9D 109.5 . . ? H9E C9 H9D 109.5 . . ? C5 C9 H9C 109.5 . . ? H9F C9 H9C 141.1 . . ? H9E C9 H9C 56.3 . . ? H9D C9 H9C 56.3 . . ? C5 C9 H9B 109.5 . . ? H9F C9 H9B 56.3 . . ? H9E C9 H9B 141.1 . . ? H9D C9 H9B 56.3 . . ? H9C C9 H9B 109.5 . . ? C5 C9 H9A 109.5 . . ? H9F C9 H9A 56.3 . . ? H9E C9 H9A 56.3 . . ? H9D C9 H9A 141.1 . . ? H9C C9 H9A 109.5 . . ? H9B C9 H9A 109.5 . . ? C7 C10 H10C 109.5 . . ? C7 C10 H10B 109.5 . . ? H10C C10 H10B 109.5 . . ? C7 C10 H10A 109.5 . . ? H10C C10 H10A 109.5 . . ? H10B C10 H10A 109.5 . . ? N1 C11 C12 110.44(14) . . ? N1 C11 C16 111.67(15) . . ? C12 C11 C16 109.40(15) . . ? N1 C11 H11 108.4 . . ? C12 C11 H11 108.4 . . ? C16 C11 H11 108.4 . . ? C11 C12 C13 111.79(16) . . ? C11 C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? C11 C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? H12B C12 H12A 107.9 . . ? C14 C13 C12 110.84(18) . . ? C14 C13 H13B 109.5 . . ? C12 C13 H13B 109.5 . . ? C14 C13 H13A 109.5 . . ? C12 C13 H13A 109.5 . . ? H13B C13 H13A 108.1 . . ? C15 C14 C13 111.32(19) . . ? C15 C14 H14B 109.4 . . ? C13 C14 H14B 109.4 . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14A 109.4 . . ? H14B C14 H14A 108 . . ? C14 C15 C16 111.37(18) . . ? C14 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? H15B C15 H15A 108 . . ? C11 C16 C15 112.00(16) . . ? C11 C16 H16B 109.2 . . ? C15 C16 H16B 109.2 . . ? C11 C16 H16A 109.2 . . ? C15 C16 H16A 109.2 . . ? H16B C16 H16A 107.9 . . ? N2 C17 C18 109.74(15) . . ? N2 C17 C22 110.92(16) . . ? C18 C17 C22 109.90(17) . . ? N2 C17 H17 108.7 . . ? C18 C17 H17 108.7 . . ? C22 C17 H17 108.7 . . ? C17 C18 C19 112.38(19) . . ? C17 C18 H18B 109.1 . . ? C19 C18 H18B 109.1 . . ? C17 C18 H18A 109.1 . . ? C19 C18 H18A 109.1 . . ? H18B C18 H18A 107.9 . . ? C20 C19 C18 111.4(2) . . ? C20 C19 H19B 109.3 . . ? C18 C19 H19B 109.3 . . ? C20 C19 H19A 109.3 . . ? C18 C19 H19A 109.3 . . ? H19B C19 H19A 108 . . ? C21 C20 C19 110.6(2) . . ? C21 C20 H20B 109.5 . . ? C19 C20 H20B 109.5 . . ? C21 C20 H20A 109.5 . . ? C19 C20 H20A 109.5 . . ? H20B C20 H20A 108.1 . . ? C20 C21 C22 111.1(2) . . ? C20 C21 H21B 109.4 . . ? C22 C21 H21B 109.4 . . ? C20 C21 H21A 109.4 . . ? C22 C21 H21A 109.4 . . ? H21B C21 H21A 108 . . ? C17 C22 C21 111.9(2) . . ? C17 C22 H22B 109.2 . . ? C21 C22 H22B 109.2 . . ? C17 C22 H22A 109.2 . . ? C21 C22 H22A 109.2 . . ? H22B C22 H22A 107.9 . . ? O1 C23 C24 120.51(15) . . ? O1 C23 C28 120.01(16) . . ? C24 C23 C28 119.48(15) . . ? C25 C24 C23 118.46(17) . . ? C25 C24 C29 119.53(17) . . ? C23 C24 C29 122.00(15) . . ? C26 C25 C24 122.09(19) . . ? C26 C25 H25 119 . . ? C24 C25 H25 119 . . ? C27 C26 C25 119.33(18) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C26 C27 C28 122.52(18) . . ? C26 C27 H27 118.7 . . ? C28 C27 H27 118.7 . . ? C27 C28 C23 117.88(18) . . ? C27 C28 C33 120.32(17) . . ? C23 C28 C33 121.80(16) . . ? C31 C29 C32 107.17(17) . . ? C31 C29 C30 109.69(17) . . ? C32 C29 C30 105.89(16) . . ? C31 C29 C24 110.35(16) . . ? C32 C29 C24 112.45(16) . . ? C30 C29 C24 111.12(15) . . ? C29 C30 H30C 109.5 . . ? C29 C30 H30B 109.5 . . ? H30C C30 H30B 109.5 . . ? C29 C30 H30A 109.5 . . ? H30C C30 H30A 109.5 . . ? H30B C30 H30A 109.5 . . ? C29 C31 H31C 109.5 . . ? C29 C31 H31B 109.5 . . ? H31C C31 H31B 109.5 . . ? C29 C31 H31A 109.5 . . ? H31C C31 H31A 109.5 . . ? H31B C31 H31A 109.5 . . ? C29 C32 H32C 109.5 . . ? C29 C32 H32B 109.5 . . ? H32C C32 H32B 109.5 . . ? C29 C32 H32A 109.5 . . ? H32C C32 H32A 109.5 . . ? H32B C32 H32A 109.5 . . ? C35 C33 C28 111.05(17) . . ? C35 C33 C36 110.46(18) . . ? C28 C33 C36 110.24(17) . . ? C35 C33 C34 106.17(19) . . ? C28 C33 C34 112.01(17) . . ? C36 C33 C34 106.76(19) . . ? C33 C34 H34C 109.5 . . ? C33 C34 H34B 109.5 . . ? H34C C34 H34B 109.5 . . ? C33 C34 H34A 109.5 . . ? H34C C34 H34A 109.5 . . ? H34B C34 H34A 109.5 . . ? C33 C35 H35C 109.5 . . ? C33 C35 H35B 109.5 . . ? H35C C35 H35B 109.5 . . ? C33 C35 H35A 109.5 . . ? H35C C35 H35A 109.5 . . ? H35B C35 H35A 109.5 . . ? C33 C36 H36C 109.5 . . ? C33 C36 H36B 109.5 . . ? H36C C36 H36B 109.5 . . ? C33 C36 H36A 109.5 . . ? H36C C36 H36A 109.5 . . ? H36B C36 H36A 109.5 . . ? O2 C37 C38 126.37(18) . . ? O2 C37 H2 119.1(13) . . ? C38 C37 H2 114.5(13) . . ? C39 C38 C43 119.59(17) . . ? C39 C38 C37 118.11(17) . . ? C43 C38 C37 122.30(17) . . ? C40 C39 C38 119.24(19) . . ? C40 C39 C44 118.13(19) . . ? C38 C39 C44 122.63(18) . . ? C41 C40 C39 121.6(2) . . ? C41 C40 H40 119.2 . . ? C39 C40 H40 119.2 . . ? C40 C41 C42 118.44(19) . . ? C40 C41 C45 120.9(2) . . ? C42 C41 C45 120.7(2) . . ? C43 C42 C41 122.8(2) . . ? C43 C42 H42 118.6 . . ? C41 C42 H42 118.6 . . ? C42 C43 C38 118.27(19) . . ? C42 C43 C46 119.28(19) . . ? C38 C43 C46 122.44(18) . . ? C39 C44 H44C 109.5 . . ? C39 C44 H44B 109.5 . . ? H44C C44 H44B 109.5 . . ? C39 C44 H44A 109.5 . . ? H44C C44 H44A 109.5 . . ? H44B C44 H44A 109.5 . . ? C41 C45 H45F 109.5 . . ? C41 C45 H45E 109.5 . . ? H45F C45 H45E 109.5 . . ? C41 C45 H45D 109.5 . . ? H45F C45 H45D 109.5 . . ? H45E C45 H45D 109.5 . . ? C41 C45 H45C 109.5 . . ? H45F C45 H45C 141.1 . . ? H45E C45 H45C 56.3 . . ? H45D C45 H45C 56.3 . . ? C41 C45 H45B 109.5 . . ? H45F C45 H45B 56.3 . . ? H45E C45 H45B 141.1 . . ? H45D C45 H45B 56.3 . . ? H45C C45 H45B 109.5 . . ? C41 C45 H45A 109.5 . . ? H45F C45 H45A 56.3 . . ? H45E C45 H45A 56.3 . . ? H45D C45 H45A 141.1 . . ? H45C C45 H45A 109.5 . . ? H45B C45 H45A 109.5 . . ? C43 C46 H46C 109.5 . . ? C43 C46 H46B 109.5 . . ? H46C C46 H46B 109.5 . . ? C43 C46 H46A 109.5 . . ? H46C C46 H46A 109.5 . . ? H46B C46 H46A 109.5 . . ? O3 C47 C48 126.11(17) . . ? O3 C47 H1 118.8(12) . . ? C48 C47 H1 115.1(12) . . ? C49 C48 C53 120.51(16) . . ? C49 C48 C47 122.37(16) . . ? C53 C48 C47 117.11(16) . . ? C50 C49 C48 118.25(17) . . ? C50 C49 C54 118.88(17) . . ? C48 C49 C54 122.86(16) . . ? C49 C50 C51 122.13(18) . . ? C49 C50 H50 118.9 . . ? C51 C50 H50 118.9 . . ? C52 C51 C50 118.68(17) . . ? C52 C51 C55 120.8(2) . . ? C50 C51 C55 120.5(2) . . ? C51 C52 C53 122.28(19) . . ? C51 C52 H52 118.9 . . ? C53 C52 H52 118.9 . . ? C52 C53 C48 118.08(18) . . ? C52 C53 C56 119.09(17) . . ? C48 C53 C56 122.83(16) . . ? C49 C54 H54C 109.5 . . ? C49 C54 H54B 109.5 . . ? H54C C54 H54B 109.5 . . ? C49 C54 H54A 109.5 . . ? H54C C54 H54A 109.5 . . ? H54B C54 H54A 109.5 . . ? C51 C55 H55F 109.5 . . ? C51 C55 H55E 109.5 . . ? H55F C55 H55E 109.5 . . ? C51 C55 H55D 109.5 . . ? H55F C55 H55D 109.5 . . ? H55E C55 H55D 109.5 . . ? C51 C55 H55C 109.5 . . ? H55F C55 H55C 141.1 . . ? H55E C55 H55C 56.3 . . ? H55D C55 H55C 56.3 . . ? C51 C55 H55B 109.5 . . ? H55F C55 H55B 56.3 . . ? H55E C55 H55B 141.1 . . ? H55D C55 H55B 56.3 . . ? H55C C55 H55B 109.5 . . ? C51 C55 H55A 109.5 . . ? H55F C55 H55A 56.3 . . ? H55E C55 H55A 56.3 . . ? H55D C55 H55A 141.1 . . ? H55C C55 H55A 109.5 . . ? H55B C55 H55A 109.5 . . ? C53 C56 H56C 109.5 . . ? C53 C56 H56B 109.5 . . ? H56C C56 H56B 109.5 . . ? C53 C56 H56A 109.5 . . ? H56C C56 H56A 109.5 . . ? H56B C56 H56A 109.5 . . ? 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 . . ? C3A C2A C1A 120.5(7) . . ? C3A C2A H2A1 107.2 . . ? C1A C2A H2A1 107.2 . . ? C3A C2A H2A2 107.2 . . ? C1A C2A H2A2 107.2 . . ? H2A1 C2A H2A2 106.8 . . ? C2A C3A C4A 120.5(6) . . ? C2A C3A H3A1 107.2 . . ? C4A C3A H3A1 107.2 . . ? C2A C3A H3A2 107.2 . . ? C4A C3A H3A2 107.2 . . ? H3A1 C3A H3A2 106.8 . . ? C5A C4A C3A 119.2(6) . . ? C5A C4A H4A1 107.5 . . ? C3A C4A H4A1 107.5 . . ? C5A C4A H4A2 107.5 . . ? C3A C4A H4A2 107.5 . . ? H4A1 C4A H4A2 107 . . ? C4A C5A H5A1 109.5 . . ? C4A C5A H5A2 109.5 . . ? H5A1 C5A H5A2 109.5 . . ? C4A C5A H5A3 109.5 . . ? H5A1 C5A H5A3 109.5 . . ? H5A2 C5A H5A3 109.5 . . ? H2B1 C2B H2B2 104.9 . . ? H4B1 C4B H4B2 106.3 . . ? #===END