data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_requested_category FM _publ_contact_author_name 'Martyn P. Coles' _publ_contact_author_email m.p.coles@sussex.ac.uk loop_ _publ_author_name 'Benjamin M. Day' 'Natalie E. Mansfield' 'Martyn P. Coles' 'Peter B. Hitchcock' data_(1b)-feb1806 _database_code_depnum_ccdc_archive 'CCDC 799143' #TrackingRef 'MPC_ChemComm_Nov2010.cif' _audit_creation_date 2006-02-21T11:47:49-00:00 _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 'C22 H40 Cl2 Mg2 N6 O2' _chemical_formula_sum 'C22 H40 Cl2 Mg2 N6 O2' _chemical_formula_weight 540.12 _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 15.4059(19) _cell_length_b 9.8558(14) _cell_length_c 18.998(2) _cell_angle_alpha 90 _cell_angle_beta 109.495(7) _cell_angle_gamma 90 _cell_volume 2719.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 156358 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 22.986 _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 1.319 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_special_details ; The crystal diffraction was weak and limited in extent . ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.316 _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_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.651215E-1 _diffrn_orient_matrix_ub_12 -0.26651E-1 _diffrn_orient_matrix_ub_13 0.75554E-2 _diffrn_orient_matrix_ub_21 0.20327E-1 _diffrn_orient_matrix_ub_22 0.455182E-1 _diffrn_orient_matrix_ub_23 0.499026E-1 _diffrn_orient_matrix_ub_31 -0.93487E-2 _diffrn_orient_matrix_ub_32 -0.866751E-1 _diffrn_orient_matrix_ub_33 0.238836E-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 0.1021 _diffrn_reflns_av_unetI/netI 0.0576 _diffrn_reflns_number 18368 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 22.97 _diffrn_reflns_theta_full 22.97 _diffrn_measured_fraction_theta_full 0.953 _diffrn_measured_fraction_theta_max 0.953 _reflns_number_total 3590 _reflns_number_gt 2911 _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 crystal diffracted weakly at high angle. There is resolved disorder in the ligands and C atoms involved were left isotropic. 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^)+(0.0818P)^2^+6.2126P] 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 3590 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0929 _refine_ls_R_factor_gt 0.0754 _refine_ls_wR_factor_ref 0.2047 _refine_ls_wR_factor_gt 0.1909 _refine_ls_goodness_of_fit_ref 1.09 _refine_ls_restrained_S_all 1.09 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.62 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.065 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Mg1 Mg 0.75345(10) 0.43319(17) 0.25157(8) 0.0370(5) Uani 1 1 d . B . Mg2 Mg 0.74176(10) 0.73542(17) 0.25348(8) 0.0388(5) Uani 1 1 d . C . Cl1 Cl 0.81607(10) 0.86405(15) 0.18905(8) 0.0559(4) Uani 1 1 d . . . Cl2 Cl 0.65920(10) 0.87207(15) 0.30663(8) 0.0587(5) Uani 1 1 d . . . O1 O 0.6611(2) 0.2759(4) 0.20878(19) 0.0485(9) Uani 1 1 d . . . O2 O 0.8571(2) 0.2924(4) 0.2908(2) 0.0509(9) Uani 1 1 d . . . N1 N 0.8330(3) 0.6069(4) 0.3313(2) 0.0397(10) Uani 1 1 d . . . N2 N 0.7302(3) 0.4628(4) 0.3526(2) 0.0418(10) Uani 1 1 d . . . N3 N 0.8405(3) 0.5661(5) 0.4567(2) 0.0517(12) Uani 1 1 d . . . N4 N 0.6611(3) 0.5901(4) 0.1810(2) 0.0394(10) Uani 1 1 d . . . N5 N 0.7728(3) 0.4826(4) 0.1495(2) 0.0416(10) Uani 1 1 d . . . N6 N 0.6484(3) 0.5822(5) 0.0538(2) 0.0531(12) Uani 1 1 d . . . C1 C 0.8004(3) 0.5455(5) 0.3820(3) 0.0417(12) Uani 1 1 d . B . C2 C 0.9266(3) 0.6639(6) 0.3629(3) 0.0496(14) Uani 1 1 d . C . H2A H 0.9403 0.721 0.325 0.06 Uiso 1 1 calc R . . H2B H 0.9723 0.5894 0.3769 0.06 Uiso 1 1 calc R . . C3 C 0.9335(4) 0.7481(6) 0.4308(3) 0.0569(15) Uani 1 1 d . . . H3A H 0.9955 0.7893 0.4508 0.068 Uiso 1 1 calc R C . H3B H 0.8876 0.8223 0.4169 0.068 Uiso 1 1 calc R . . C4 C 0.9163(4) 0.6599(6) 0.4895(3) 0.0590(16) Uani 1 1 d . C . H4A H 0.9728 0.6078 0.5158 0.071 Uiso 1 1 calc R . . H4B H 0.9019 0.7179 0.5266 0.071 Uiso 1 1 calc R . . C5 C 0.8080(4) 0.4890(7) 0.5087(3) 0.0636(16) Uani 1 1 d . C . H5A H 0.8224 0.5388 0.5565 0.076 Uiso 1 1 calc R . . H5B H 0.8393 0.3999 0.5189 0.076 Uiso 1 1 calc R . . C6 C 0.7043(4) 0.4686(7) 0.4745(3) 0.0678(17) Uani 1 1 d . . . H6A H 0.6822 0.4112 0.5078 0.081 Uiso 1 1 calc R C . H6B H 0.6727 0.5573 0.4688 0.081 Uiso 1 1 calc R . . C7 C 0.6824(4) 0.4014(6) 0.3994(3) 0.0495(14) Uani 1 1 d . C . H7A H 0.6995 0.3043 0.4069 0.059 Uiso 1 1 calc R . . H7B H 0.6152 0.4066 0.3729 0.059 Uiso 1 1 calc R . . C8 C 0.6950(3) 0.5524(5) 0.1259(3) 0.0410(12) Uani 1 1 d . B . C9 C 0.5614(3) 0.6131(6) 0.1540(3) 0.0508(14) Uani 1 1 d . B . H9A H 0.5418 0.6466 0.1956 0.061 Uiso 1 1 calc R . . H9B H 0.5291 0.5264 0.1361 0.061 Uiso 1 1 calc R . . C10 C 0.5358(4) 0.7147(7) 0.0919(3) 0.0739(19) Uani 1 1 d . . . H10A H 0.4679 0.7243 0.0719 0.089 Uiso 1 1 calc R B . H10B H 0.5623 0.8041 0.1114 0.089 Uiso 1 1 calc R . . C11 C 0.5700(5) 0.6726(9) 0.0309(4) 0.090(2) Uani 1 1 d . B . H11A H 0.5192 0.6274 -0.0085 0.107 Uiso 1 1 calc R . . H11B H 0.587 0.7549 0.0086 0.107 Uiso 1 1 calc R . . C15 C 0.5841(3) 0.2359(6) 0.2314(3) 0.0499(13) Uani 1 1 d . C . H15A H 0.5504 0.3168 0.2394 0.06 Uiso 1 1 calc R . . H15B H 0.6056 0.183 0.2784 0.06 Uiso 1 1 calc R . . C16 C 0.5234(4) 0.1508(6) 0.1690(3) 0.0596(16) Uani 1 1 d . . . H16A H 0.4734 0.206 0.1346 0.071 Uiso 1 1 calc R A 1 H16B H 0.4959 0.0752 0.1886 0.071 Uiso 1 1 calc R A 1 C19 C 0.9470(4) 0.2947(6) 0.2834(4) 0.0632(16) Uani 1 1 d . C . H19A H 0.9896 0.3522 0.3227 0.076 Uiso 1 1 calc R . . H19B H 0.9438 0.3305 0.2339 0.076 Uiso 1 1 calc R . . C20 C 0.9783(4) 0.1515(6) 0.2918(4) 0.0607(16) Uani 1 1 d . . . H20A H 1.0464 0.1459 0.3112 0.073 Uiso 1 1 calc R C . H20B H 0.9552 0.1026 0.2436 0.073 Uiso 1 1 calc R . . C21 C 0.9370(4) 0.0939(6) 0.3476(3) 0.0563(15) Uani 1 1 d . C . H21A H 0.9218 -0.0035 0.3378 0.068 Uiso 1 1 calc R . . H21B H 0.9799 0.1043 0.3994 0.068 Uiso 1 1 calc R . . C22 C 0.8515(4) 0.1764(7) 0.3355(4) 0.077(2) Uani 1 1 d . C . H22A H 0.7962 0.1217 0.3093 0.093 Uiso 1 1 calc R . . H22B H 0.8473 0.2064 0.384 0.093 Uiso 1 1 calc R . . C12 C 0.6867(5) 0.5471(8) -0.0037(4) 0.083(2) Uiso 0.57(2) 1 d P B 1 H12A H 0.6358 0.5211 -0.0493 0.099 Uiso 0.57(2) 1 calc PR B 1 H12B H 0.7167 0.6285 -0.0156 0.099 Uiso 0.57(2) 1 calc PR B 1 C13 C 0.7473(9) 0.4473(14) 0.0144(6) 0.064(4) Uiso 0.57(2) 1 d P B 1 H13A H 0.7824 0.4492 -0.0208 0.076 Uiso 0.57(2) 1 calc PR B 1 H13B H 0.7129 0.3606 0.0063 0.076 Uiso 0.57(2) 1 calc PR B 1 C14 C 0.8182(4) 0.4465(6) 0.0959(3) 0.0610(16) Uiso 0.57(2) 1 d P B 1 H14A H 0.846 0.3551 0.1078 0.073 Uiso 0.57(2) 1 calc PR B 1 H14B H 0.8682 0.5121 0.0995 0.073 Uiso 0.57(2) 1 calc PR B 1 C17 C 0.5872(4) 0.0979(6) 0.1299(3) 0.0629(16) Uiso 0.74(3) 1 d P C 1 H17A H 0.6176 0.013 0.1535 0.075 Uiso 0.74(3) 1 calc PR C 1 H17B H 0.5532 0.0803 0.0765 0.075 Uiso 0.74(3) 1 calc PR C 1 C18 C 0.6539(6) 0.2057(9) 0.1386(6) 0.047(3) Uiso 0.74(3) 1 d P C 1 H18A H 0.6331 0.2694 0.096 0.056 Uiso 0.74(3) 1 calc PR C 1 H18B H 0.7144 0.1679 0.1411 0.056 Uiso 0.74(3) 1 calc PR C 1 C12A C 0.6867(5) 0.5471(8) -0.0037(4) 0.083(2) Uiso 0.43(2) 1 d P B 2 H12C H 0.6779 0.6242 -0.0387 0.099 Uiso 0.43(2) 1 calc PR B 2 H12D H 0.6527 0.4683 -0.0321 0.099 Uiso 0.43(2) 1 calc PR B 2 C13A C 0.7943(12) 0.5106(19) 0.0293(8) 0.066(6) Uiso 0.43(2) 1 d P B 2 H13C H 0.8104 0.452 -0.0069 0.079 Uiso 0.43(2) 1 calc PR B 2 H13D H 0.8306 0.5953 0.035 0.079 Uiso 0.43(2) 1 calc PR B 2 C14A C 0.8182(4) 0.4465(6) 0.0959(3) 0.0610(16) Uiso 0.43(2) 1 d P B 2 H14C H 0.8852 0.4601 0.1208 0.073 Uiso 0.43(2) 1 calc PR B 2 H14D H 0.8086 0.3481 0.0857 0.073 Uiso 0.43(2) 1 calc PR B 2 C17A C 0.5872(4) 0.0979(6) 0.1299(3) 0.0629(16) Uiso 0.26(3) 1 d P C 2 H17C H 0.5641 0.1227 0.0764 0.075 Uiso 0.26(3) 1 calc PR C 2 H17D H 0.5922 -0.0022 0.1341 0.075 Uiso 0.26(3) 1 calc PR C 2 C18A C 0.6831(17) 0.166(3) 0.1701(16) 0.046(8) Uiso 0.26(3) 1 d P C 2 H18C H 0.7257 0.1017 0.2051 0.056 Uiso 0.26(3) 1 calc PR C 2 H18D H 0.7115 0.1978 0.1334 0.056 Uiso 0.26(3) 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0364(9) 0.0377(10) 0.0360(9) -0.0003(7) 0.0109(7) -0.0017(7) Mg2 0.0415(9) 0.0379(10) 0.0327(9) 0.0001(7) 0.0067(7) -0.0010(7) Cl1 0.0593(9) 0.0545(9) 0.0577(9) 0.0110(6) 0.0247(7) 0.0002(7) Cl2 0.0694(10) 0.0561(9) 0.0554(9) -0.0050(6) 0.0270(7) 0.0054(7) O1 0.047(2) 0.047(2) 0.057(2) -0.0129(16) 0.0239(17) -0.0119(17) O2 0.0409(19) 0.046(2) 0.069(2) 0.0158(18) 0.0227(17) 0.0095(17) N1 0.041(2) 0.042(2) 0.033(2) 0.0051(18) 0.0085(18) -0.0031(19) N2 0.042(2) 0.044(3) 0.040(2) 0.0024(19) 0.0131(19) -0.002(2) N3 0.064(3) 0.056(3) 0.031(2) 0.001(2) 0.010(2) -0.007(2) N4 0.039(2) 0.042(2) 0.034(2) -0.0039(18) 0.0084(18) -0.0005(19) N5 0.036(2) 0.052(3) 0.038(2) -0.0040(19) 0.0138(18) -0.002(2) N6 0.053(3) 0.073(3) 0.030(2) -0.002(2) 0.010(2) -0.006(2) C1 0.046(3) 0.038(3) 0.037(3) 0.003(2) 0.008(2) 0.009(3) C2 0.042(3) 0.055(4) 0.044(3) 0.006(3) 0.005(2) -0.006(3) C3 0.055(3) 0.058(4) 0.045(3) -0.002(3) -0.001(3) -0.012(3) C4 0.069(4) 0.055(4) 0.040(3) -0.005(3) 0.001(3) -0.003(3) C5 0.077(4) 0.073(4) 0.040(3) 0.008(3) 0.019(3) -0.002(4) C6 0.077(4) 0.075(5) 0.057(4) 0.007(3) 0.031(3) -0.007(4) C7 0.052(3) 0.055(4) 0.045(3) 0.007(2) 0.019(2) 0.002(3) C8 0.044(3) 0.040(3) 0.035(3) -0.001(2) 0.007(2) -0.013(2) C9 0.036(3) 0.058(4) 0.052(3) -0.006(3) 0.006(2) 0.003(3) C10 0.065(4) 0.070(4) 0.067(4) 0.005(3) -0.005(3) 0.018(3) C11 0.071(4) 0.121(7) 0.071(5) 0.039(4) 0.016(4) 0.029(5) C15 0.044(3) 0.054(3) 0.051(3) -0.003(3) 0.017(2) -0.012(3) C16 0.052(3) 0.073(4) 0.050(3) -0.009(3) 0.012(3) -0.017(3) C19 0.049(3) 0.060(4) 0.085(4) 0.018(3) 0.028(3) 0.010(3) C20 0.047(3) 0.046(3) 0.094(5) 0.008(3) 0.030(3) 0.007(3) C21 0.050(3) 0.044(3) 0.068(4) 0.009(3) 0.011(3) 0.004(3) C22 0.065(4) 0.062(4) 0.117(6) 0.045(4) 0.046(4) 0.013(3) #----------------------------------------------------------------------------# # 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 O2 2.058(4) . ? Mg1 O1 2.078(4) . ? Mg1 N2 2.087(4) . ? Mg1 N5 2.114(4) . ? Mg1 N4 2.222(4) . ? Mg1 N1 2.343(4) . ? Mg2 N4 2.085(4) . ? Mg2 N1 2.093(4) . ? Mg2 Cl2 2.304(2) . ? Mg2 Cl1 2.313(2) . ? O1 C18A 1.42(2) . ? O1 C15 1.444(6) . ? O1 C18 1.472(8) . ? O2 C19 1.438(6) . ? O2 C22 1.444(6) . ? N1 C1 1.367(6) . ? N1 C2 1.475(6) . ? N2 C1 1.320(6) . ? N2 C7 1.462(6) . ? N3 C1 1.361(6) . ? N3 C4 1.457(7) . ? N3 C5 1.461(7) . ? N4 C8 1.369(6) . ? N4 C9 1.466(6) . ? N5 C8 1.323(6) . ? N5 C14 1.459(7) . ? N6 C8 1.350(6) . ? N6 C12 1.445(8) . ? N6 C11 1.446(8) . ? C2 C3 1.508(7) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 C4 1.505(8) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 C6 1.523(8) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 C7 1.505(8) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C9 C10 1.498(8) . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? C10 C11 1.483(9) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C15 C16 1.498(7) . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 C17 1.508(8) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C19 C20 1.483(8) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? C20 C21 1.517(8) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? C21 C22 1.498(8) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? C12 C13 1.320(12) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.570(13) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C17 C18 1.449(9) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C13A H13C 0.99 . ? C13A H13D 0.99 . ? C18A H18C 0.99 . ? C18A H18D 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 O2 Mg1 O1 89.19(16) . . ? O2 Mg1 N2 96.42(16) . . ? O1 Mg1 N2 99.15(16) . . ? O2 Mg1 N5 99.07(16) . . ? O1 Mg1 N5 95.78(15) . . ? N2 Mg1 N5 158.58(19) . . ? O2 Mg1 N4 161.90(16) . . ? O1 Mg1 N4 93.80(15) . . ? N2 Mg1 N4 100.71(16) . . ? N5 Mg1 N4 62.88(16) . . ? O2 Mg1 N1 94.78(15) . . ? O1 Mg1 N1 160.13(15) . . ? N2 Mg1 N1 61.08(15) . . ? N5 Mg1 N1 102.78(16) . . ? N4 Mg1 N1 88.45(15) . . ? N4 Mg2 N1 99.35(17) . . ? N4 Mg2 Cl2 113.37(13) . . ? N1 Mg2 Cl2 112.53(13) . . ? N4 Mg2 Cl1 108.53(13) . . ? N1 Mg2 Cl1 111.78(13) . . ? Cl2 Mg2 Cl1 110.77(9) . . ? C18A O1 C15 108.0(9) . . ? C15 O1 C18 108.7(4) . . ? C18A O1 Mg1 121.6(8) . . ? C15 O1 Mg1 127.6(3) . . ? C18 O1 Mg1 122.6(3) . . ? C19 O2 C22 108.5(4) . . ? C19 O2 Mg1 127.6(3) . . ? C22 O2 Mg1 123.8(3) . . ? C1 N1 C2 114.9(4) . . ? C1 N1 Mg2 116.6(3) . . ? C2 N1 Mg2 113.1(3) . . ? C1 N1 Mg1 84.0(3) . . ? C2 N1 Mg1 140.4(3) . . ? Mg2 N1 Mg1 84.39(14) . . ? C1 N2 C7 120.4(4) . . ? C1 N2 Mg1 96.2(3) . . ? C7 N2 Mg1 141.0(3) . . ? C1 N3 C4 124.1(4) . . ? C1 N3 C5 119.3(4) . . ? C4 N3 C5 116.6(4) . . ? C8 N4 C9 113.4(4) . . ? C8 N4 Mg2 113.4(3) . . ? C9 N4 Mg2 116.6(3) . . ? C8 N4 Mg1 86.7(3) . . ? C9 N4 Mg1 134.7(3) . . ? Mg2 N4 Mg1 87.67(15) . . ? C8 N5 C14 118.7(4) . . ? C8 N5 Mg1 92.4(3) . . ? C14 N5 Mg1 146.2(4) . . ? C8 N6 C12 120.0(5) . . ? C8 N6 C11 123.2(5) . . ? C12 N6 C11 115.6(5) . . ? N2 C1 N3 123.8(5) . . ? N2 C1 N1 114.7(4) . . ? N3 C1 N1 121.5(5) . . ? N1 C2 C3 109.7(4) . . ? N1 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? N1 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C4 C3 C2 109.6(5) . . ? C4 C3 H3A 109.7 . . ? C2 C3 H3A 109.7 . . ? C4 C3 H3B 109.7 . . ? C2 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? N3 C4 C3 111.3(4) . . ? N3 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? N3 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108 . . ? N3 C5 C6 109.1(4) . . ? N3 C5 H5A 109.9 . . ? C6 C5 H5A 109.9 . . ? N3 C5 H5B 109.9 . . ? C6 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? C7 C6 C5 109.5(5) . . ? C7 C6 H6A 109.8 . . ? C5 C6 H6A 109.8 . . ? C7 C6 H6B 109.8 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.2 . . ? N2 C7 C6 113.3(5) . . ? N2 C7 H7A 108.9 . . ? C6 C7 H7A 108.9 . . ? N2 C7 H7B 108.9 . . ? C6 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? N5 C8 N6 125.0(5) . . ? N5 C8 N4 114.5(4) . . ? N6 C8 N4 120.5(5) . . ? N4 C9 C10 110.4(5) . . ? N4 C9 H9A 109.6 . . ? C10 C9 H9A 109.6 . . ? N4 C9 H9B 109.6 . . ? C10 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C11 C10 C9 111.1(5) . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108 . . ? N6 C11 C10 114.6(5) . . ? N6 C11 H11A 108.6 . . ? C10 C11 H11A 108.6 . . ? N6 C11 H11B 108.6 . . ? C10 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? O1 C15 C16 105.9(4) . . ? O1 C15 H15A 110.5 . . ? C16 C15 H15A 110.5 . . ? O1 C15 H15B 110.5 . . ? C16 C15 H15B 110.5 . . ? H15A C15 H15B 108.7 . . ? C15 C16 C17 104.3(5) . . ? C15 C16 H16A 110.9 . . ? C17 C16 H16A 110.9 . . ? C15 C16 H16B 110.9 . . ? C17 C16 H16B 110.9 . . ? H16A C16 H16B 108.9 . . ? O2 C19 C20 105.3(5) . . ? O2 C19 H19A 110.7 . . ? C20 C19 H19A 110.7 . . ? O2 C19 H19B 110.7 . . ? C20 C19 H19B 110.7 . . ? H19A C19 H19B 108.8 . . ? C19 C20 C21 103.5(5) . . ? C19 C20 H20A 111.1 . . ? C21 C20 H20A 111.1 . . ? C19 C20 H20B 111.1 . . ? C21 C20 H20B 111.1 . . ? H20A C20 H20B 109 . . ? C22 C21 C20 104.0(5) . . ? C22 C21 H21A 111 . . ? C20 C21 H21A 111 . . ? C22 C21 H21B 111 . . ? C20 C21 H21B 111 . . ? H21A C21 H21B 109 . . ? O2 C22 C21 107.4(5) . . ? O2 C22 H22A 110.2 . . ? C21 C22 H22A 110.2 . . ? O2 C22 H22B 110.2 . . ? C21 C22 H22B 110.2 . . ? H22A C22 H22B 108.5 . . ? C13 C12 N6 114.5(7) . . ? C13 C12 H12A 108.6 . . ? N6 C12 H12A 108.6 . . ? C13 C12 H12B 108.6 . . ? N6 C12 H12B 108.6 . . ? H12A C12 H12B 107.6 . . ? C12 C13 C14 117.3(9) . . ? C12 C13 H13A 108 . . ? C14 C13 H13A 108 . . ? C12 C13 H13B 108 . . ? C14 C13 H13B 108 . . ? H13A C13 H13B 107.2 . . ? N5 C14 C13 110.4(6) . . ? N5 C14 H14A 109.6 . . ? C13 C14 H14A 109.6 . . ? N5 C14 H14B 109.6 . . ? C13 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? C18 C17 C16 104.1(5) . . ? C18 C17 H17A 110.9 . . ? C16 C17 H17A 110.9 . . ? C18 C17 H17B 110.9 . . ? C16 C17 H17B 110.9 . . ? H17A C17 H17B 109 . . ? C17 C18 O1 106.5(5) . . ? C17 C18 H18A 110.4 . . ? O1 C18 H18A 110.4 . . ? C17 C18 H18B 110.4 . . ? O1 C18 H18B 110.4 . . ? H18A C18 H18B 108.6 . . ? H13C C13A H13D 107.8 . . ? O1 C18A H18C 111.1 . . ? O1 C18A H18D 111.1 . . ? H18C C18A H18D 109.1 . . ? #===END data_(2a)-jan709b _database_code_depnum_ccdc_archive 'CCDC 799144' #TrackingRef 'MPC_ChemComm_Nov2010.cif' _audit_creation_date 2009-02-06T10:50:22-00:00 _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 'C22 H40 Br2 Mg2 N6 O3, C4 H8 O' _chemical_formula_sum 'C26 H48 Br2 Mg2 N6 O4' _chemical_formula_weight 717.12 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a n' _symmetry_space_group_name_Hall '-P 2n 2bc' _symmetry_Int_Tables_number 52 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x, -y+1/2, -z+1/2' '-x+1/2, y, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x, y-1/2, z-1/2' 'x-1/2, -y, z' _cell_length_a 9.41340(10) _cell_length_b 17.0471(2) _cell_length_c 21.1472(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3393.52(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 32311 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.733 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.464 _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 0.5252 _exptl_absorpt_correction_T_max 0.8272 #----------------------------------------------------------------------------# # 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 0.213291E-1 _diffrn_orient_matrix_ub_12 -0.6636E-3 _diffrn_orient_matrix_ub_13 0.463216E-1 _diffrn_orient_matrix_ub_21 -0.103703 _diffrn_orient_matrix_ub_22 -0.50443E-2 _diffrn_orient_matrix_ub_23 0.94148E-2 _diffrn_orient_matrix_ub_31 0.8709E-2 _diffrn_orient_matrix_ub_32 -0.05844 _diffrn_orient_matrix_ub_33 -0.13386E-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 0.0729 _diffrn_reflns_av_unetI/netI 0.0238 _diffrn_reflns_number 55355 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 26.7 _diffrn_reflns_theta_full 26.7 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _reflns_number_total 3552 _reflns_number_gt 2936 _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 ; The C3-N3-C4 unit of the guanidine ligand was disordered over two positions and was refined with SADI restraints on the carbon-nitrogen distances of each component; the disordered atoms were left isotropic It was not possible to differentiate the oxygen and carbon atoms in the THF solvate. It was refined as fully disordered with each position 80% carbon and 20% oxygen 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^)+(0.1271P)^2^+11.1160P] 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 3552 _refine_ls_number_parameters 167 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0766 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.2024 _refine_ls_wR_factor_gt 0.188 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.212 _refine_diff_density_min -0.962 _refine_diff_density_rms 0.117 #----------------------------------------------------------------------------# # 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 Br Br 0.05407(5) 0.37133(4) 0.11527(3) 0.0526(3) Uani 1 1 d . . . Mg Mg 0.24689(14) 0.31556(7) 0.17893(6) 0.0238(3) Uani 1 1 d . . . O1 O 0.4144(3) 0.3615(2) 0.12539(14) 0.0351(7) Uani 1 1 d . . . O2 O 0.0832(4) 0.25 0.25 0.0253(8) Uani 1 2 d S . . N1 N 0.3129(4) 0.37822(19) 0.25553(16) 0.0335(8) Uani 1 1 d . . . N2 N 0.3017(4) 0.2952(2) 0.34723(14) 0.0316(8) Uani 1 1 d . . . C1 C 0.3222(5) 0.3609(2) 0.31715(19) 0.0346(10) Uani 1 1 d . A . C6 C 0.5579(5) 0.3439(4) 0.1456(3) 0.0513(15) Uani 1 1 d . . . H6A H 0.5842 0.2896 0.1336 0.062 Uiso 1 1 calc R . . H6B H 0.5669 0.3494 0.192 0.062 Uiso 1 1 calc R . . C7 C 0.6510(6) 0.4020(4) 0.1123(3) 0.0542(14) Uani 1 1 d . . . H7A H 0.6591 0.4513 0.1368 0.065 Uiso 1 1 calc R . . H7B H 0.7472 0.3803 0.105 0.065 Uiso 1 1 calc R . . C8 C 0.5746(4) 0.4150(3) 0.0513(2) 0.0382(10) Uani 1 1 d . . . H8A H 0.5974 0.3733 0.0204 0.046 Uiso 1 1 calc R . . H8B H 0.5995 0.4666 0.0328 0.046 Uiso 1 1 calc R . . C9 C 0.4199(4) 0.4123(3) 0.06977(19) 0.0344(10) Uani 1 1 d . . . H9A H 0.3845 0.4655 0.0801 0.041 Uiso 1 1 calc R . . H9B H 0.3616 0.3904 0.035 0.041 Uiso 1 1 calc R . . C10 C -0.0092(5) 0.1937(3) 0.2171(2) 0.0336(9) Uani 1 1 d . . . H10A H 0.0012 0.1991 0.1707 0.04 Uiso 1 1 calc R . . H10B H 0.0159 0.1393 0.2291 0.04 Uiso 1 1 calc R . . C11 C -0.1556(5) 0.2117(4) 0.2364(4) 0.0678(18) Uani 1 1 d . . . H11A H -0.2197 0.2101 0.1993 0.081 Uiso 1 1 calc R . . H11B H -0.1892 0.1728 0.2678 0.081 Uiso 1 1 calc R . . N3 N 0.3305(13) 0.4295(5) 0.3560(4) 0.027(2) Uiso 0.461(19) 1 d P A 1 C2 C 0.3449(8) 0.4637(3) 0.2518(2) 0.0602(17) Uani 0.461(19) 1 d P A 1 H2A H 0.4248 0.4733 0.2223 0.072 Uiso 0.461(19) 1 calc PR A 1 H2B H 0.2608 0.493 0.2365 0.072 Uiso 0.461(19) 1 calc PR A 1 C3 C 0.3832(17) 0.4894(6) 0.3169(5) 0.038(3) Uiso 0.461(19) 1 d P A 1 H3A H 0.4875 0.4945 0.3215 0.045 Uiso 0.461(19) 1 calc PR A 1 H3B H 0.3383 0.5403 0.3271 0.045 Uiso 0.461(19) 1 calc PR A 1 C4 C 0.3704(18) 0.4001(7) 0.4152(6) 0.045(3) Uiso 0.461(19) 1 d P A 1 H4A H 0.3243 0.4301 0.4496 0.055 Uiso 0.461(19) 1 calc PR A 1 H4B H 0.4747 0.403 0.4207 0.055 Uiso 0.461(19) 1 calc PR A 1 C5 C 0.3200(8) 0.3146(3) 0.4152(2) 0.0585(16) Uani 0.461(19) 1 d P A 1 H5A H 0.3916 0.28 0.4351 0.07 Uiso 0.461(19) 1 calc PR A 1 H5B H 0.229 0.3093 0.4383 0.07 Uiso 0.461(19) 1 calc PR A 1 N3A N 0.3838(13) 0.4186(5) 0.3539(4) 0.037(2) Uiso 0.539(19) 1 d P A 2 C2A C 0.3449(8) 0.4637(3) 0.2518(2) 0.0602(17) Uani 0.539(19) 1 d P A 2 H2A1 H 0.2811 0.4901 0.2212 0.072 Uiso 0.539(19) 1 calc PR A 2 H2A2 H 0.4446 0.4726 0.2387 0.072 Uiso 0.539(19) 1 calc PR A 2 C3A C 0.3192(17) 0.4942(6) 0.3189(5) 0.048(3) Uiso 0.539(19) 1 d P A 2 H3A1 H 0.2172 0.5021 0.3282 0.057 Uiso 0.539(19) 1 calc PR A 2 H3A2 H 0.3732 0.5427 0.3281 0.057 Uiso 0.539(19) 1 calc PR A 2 C4A C 0.2982(15) 0.4048(6) 0.4172(5) 0.047(3) Uiso 0.539(19) 1 d P A 2 H4A1 H 0.3431 0.4298 0.4544 0.056 Uiso 0.539(19) 1 calc PR A 2 H4A2 H 0.1971 0.4204 0.414 0.056 Uiso 0.539(19) 1 calc PR A 2 C5A C 0.3200(8) 0.3146(3) 0.4152(2) 0.0585(16) Uani 0.539(19) 1 d P A 2 H5A1 H 0.4161 0.3002 0.4302 0.07 Uiso 0.539(19) 1 calc PR A 2 H5A2 H 0.2483 0.2874 0.4415 0.07 Uiso 0.539(19) 1 calc PR A 2 C1S C 0.25 0.590(2) 0.5 0.296(5) Uiso 0.8 2 d SP . 1 H1S1 H 0.1947 0.555 0.4717 0.355 Uiso 0.4 1 calc PR . 1 H1S2 H 0.3053 0.555 0.5283 0.355 Uiso 0.4 1 calc PR . 1 C2S C 0.350(2) 0.6288(10) 0.4612(10) 0.203(7) Uiso 0.8 1 d P B 1 H2S1 H 0.4481 0.6248 0.4777 0.243 Uiso 0.8 1 calc PR B 1 H2S2 H 0.3464 0.611 0.4167 0.243 Uiso 0.8 1 calc PR B 1 C3S C 0.2942(19) 0.6998(11) 0.4691(7) 0.201(7) Uiso 0.8 1 d P . 1 H3S1 H 0.2327 0.7131 0.4327 0.242 Uiso 0.8 1 calc PR . 1 H3S2 H 0.3708 0.7394 0.4719 0.242 Uiso 0.8 1 calc PR . 1 O1S O 0.25 0.590(2) 0.5 0.296(5) Uiso 0.2 2 d SP . 2 O2S O 0.350(2) 0.6288(10) 0.4612(10) 0.203(7) Uiso 0.2 1 d P C 2 O3S O 0.2942(19) 0.6998(11) 0.4691(7) 0.201(7) Uiso 0.2 1 d P . 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 Br 0.0316(3) 0.0712(4) 0.0549(4) 0.0327(3) -0.0046(2) 0.0029(2) Mg 0.0249(7) 0.0276(7) 0.0189(6) 0.0049(5) -0.0017(5) 0.0004(5) O1 0.0198(14) 0.0542(19) 0.0313(15) 0.0248(13) -0.0017(12) 0.0017(13) O2 0.0212(18) 0.0244(18) 0.0302(19) -0.0047(15) 0 0 N1 0.048(2) 0.0291(18) 0.0233(16) 0.0059(13) -0.0017(15) -0.0148(16) N2 0.046(2) 0.0323(18) 0.0169(15) 0.0025(13) -0.0071(14) -0.0059(15) C1 0.048(3) 0.030(2) 0.026(2) -0.0018(16) -0.0034(18) -0.0114(19) C6 0.020(2) 0.086(4) 0.048(3) 0.034(3) -0.0066(19) 0.006(2) C7 0.029(3) 0.080(4) 0.053(3) 0.014(3) -0.002(2) -0.003(3) C8 0.025(2) 0.055(3) 0.034(2) 0.011(2) 0.0067(17) -0.0005(19) C9 0.026(2) 0.052(3) 0.0253(19) 0.0197(18) 0.0016(15) 0.0001(18) C10 0.028(2) 0.033(2) 0.039(2) -0.0022(18) -0.0072(18) -0.0086(17) C11 0.026(2) 0.083(4) 0.095(5) -0.025(4) 0.000(3) -0.010(3) C2 0.105(5) 0.037(3) 0.039(3) 0.007(2) -0.007(3) -0.032(3) C5 0.102(5) 0.052(3) 0.021(2) 0.000(2) -0.009(3) -0.021(3) C2A 0.105(5) 0.037(3) 0.039(3) 0.007(2) -0.007(3) -0.032(3) C5A 0.102(5) 0.052(3) 0.021(2) 0.000(2) -0.009(3) -0.021(3) #----------------------------------------------------------------------------# # 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 Br Mg 2.4516(13) . ? Mg N2 2.034(4) 3 ? Mg N1 2.037(4) . ? Mg O1 2.093(3) . ? Mg O2 2.426(3) . ? O1 C6 1.448(5) . ? O1 C9 1.461(4) . ? O2 C10 1.471(5) . ? O2 C10 1.471(5) 3 ? O2 Mg 2.426(3) 3 ? N1 C1 1.339(5) . ? N1 C2 1.491(6) . ? N2 C1 1.303(5) . ? N2 C5 1.486(5) . ? N2 Mg 2.034(4) 3 ? C1 N3A 1.381(9) . ? C1 N3 1.431(9) . ? C6 C7 1.498(8) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 C8 1.495(7) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 C9 1.508(6) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? C10 C11 1.470(7) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C11 C11 1.425(13) 3 ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? N3 C4 1.401(15) . ? N3 C3 1.404(14) . ? C2 C3 1.489(11) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 C5 1.532(13) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? N3A C4A 1.580(15) . ? N3A C3A 1.605(16) . ? C3A H3A1 0.99 . ? C3A H3A2 0.99 . ? C4A H4A1 0.99 . ? C4A H4A2 0.99 . ? C1S C2S 1.41(2) 4_556 ? C1S C2S 1.41(2) . ? C1S C3S 2.03(4) . ? C1S C3S 2.03(4) 4_556 ? C1S H1S1 0.99 . ? C1S H1S2 0.99 . ? C2S C3S 1.329(19) . ? C2S H2S1 0.99 . ? C2S H2S2 0.99 . ? C3S C3S 1.55(3) 4_556 ? C3S H3S1 0.99 . ? C3S H3S2 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 N2 Mg N1 128.71(16) 3 . ? N2 Mg O1 90.52(15) 3 . ? N1 Mg O1 90.22(15) . . ? N2 Mg O2 84.38(11) 3 . ? N1 Mg O2 86.73(11) . . ? O1 Mg O2 170.47(12) . . ? N2 Mg Br 113.48(12) 3 . ? N1 Mg Br 117.33(12) . . ? O1 Mg Br 96.64(9) . . ? O2 Mg Br 92.78(8) . . ? C6 O1 C9 109.1(3) . . ? C6 O1 Mg 117.7(2) . . ? C9 O1 Mg 133.1(2) . . ? C10 O2 C10 107.5(4) . 3 ? C10 O2 Mg 112.54(18) . . ? C10 O2 Mg 111.60(18) 3 . ? C10 O2 Mg 111.60(18) . 3 ? C10 O2 Mg 112.54(18) 3 3 ? Mg O2 Mg 101.10(15) . 3 ? C1 N1 C2 104.7(3) . . ? C1 N1 Mg 132.7(3) . . ? C2 N1 Mg 122.1(3) . . ? C1 N2 C5 105.3(4) . . ? C1 N2 Mg 134.7(3) . 3 ? C5 N2 Mg 120.0(3) . 3 ? N2 C1 N1 130.9(4) . . ? N2 C1 N3A 113.6(5) . . ? N1 C1 N3A 114.7(5) . . ? N2 C1 N3 115.5(4) . . ? N1 C1 N3 112.4(5) . . ? O1 C6 C7 105.7(4) . . ? O1 C6 H6A 110.6 . . ? C7 C6 H6A 110.6 . . ? O1 C6 H6B 110.6 . . ? C7 C6 H6B 110.6 . . ? H6A C6 H6B 108.7 . . ? C8 C7 C6 102.8(4) . . ? C8 C7 H7A 111.2 . . ? C6 C7 H7A 111.2 . . ? C8 C7 H7B 111.2 . . ? C6 C7 H7B 111.2 . . ? H7A C7 H7B 109.1 . . ? C7 C8 C9 103.7(4) . . ? C7 C8 H8A 111 . . ? C9 C8 H8A 111 . . ? C7 C8 H8B 111 . . ? C9 C8 H8B 111 . . ? H8A C8 H8B 109 . . ? O1 C9 C8 105.1(3) . . ? O1 C9 H9A 110.7 . . ? C8 C9 H9A 110.7 . . ? O1 C9 H9B 110.7 . . ? C8 C9 H9B 110.7 . . ? H9A C9 H9B 108.8 . . ? C11 C10 O2 106.6(4) . . ? C11 C10 H10A 110.4 . . ? O2 C10 H10A 110.4 . . ? C11 C10 H10B 110.4 . . ? O2 C10 H10B 110.4 . . ? H10A C10 H10B 108.6 . . ? C11 C11 C10 107.7(3) 3 . ? C11 C11 H11A 110.2 3 . ? C10 C11 H11A 110.2 . . ? C11 C11 H11B 110.2 3 . ? C10 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? C4 N3 C3 133.8(12) . . ? C4 N3 C1 103.6(8) . . ? C3 N3 C1 106.0(7) . . ? C3 C2 N1 106.7(5) . . ? C3 C2 H2A 110.4 . . ? N1 C2 H2A 110.4 . . ? C3 C2 H2B 110.4 . . ? N1 C2 H2B 110.4 . . ? H2A C2 H2B 108.6 . . ? N3 C3 C2 104.2(8) . . ? N3 C3 H3A 110.9 . . ? C2 C3 H3A 110.9 . . ? N3 C3 H3B 110.9 . . ? C2 C3 H3B 110.9 . . ? H3A C3 H3B 108.9 . . ? N3 C4 C5 104.9(9) . . ? N3 C4 H4A 110.8 . . ? C5 C4 H4A 110.8 . . ? N3 C4 H4B 110.8 . . ? C5 C4 H4B 110.8 . . ? H4A C4 H4B 108.8 . . ? N2 C5 C4 104.3(5) . . ? N2 C5 H5A 110.9 . . ? C4 C5 H5A 110.9 . . ? N2 C5 H5B 110.9 . . ? C4 C5 H5B 110.9 . . ? H5A C5 H5B 108.9 . . ? C1 N3A C4A 99.0(7) . . ? C1 N3A C3A 98.8(8) . . ? C4A N3A C3A 108.5(12) . . ? N3A C3A H3A1 112.6 . . ? N3A C3A H3A2 112.6 . . ? H3A1 C3A H3A2 110.1 . . ? N3A C4A H4A1 113 . . ? N3A C4A H4A2 113 . . ? H4A1 C4A H4A2 110.4 . . ? C2S C1S C2S 124(3) 4_556 . ? C2S C1S C3S 84(2) 4_556 . ? C2S C1S C3S 84(2) . 4_556 ? C2S C1S H1S1 106.3 4_556 . ? C2S C1S H1S1 106.3 . . ? C3S C1S H1S1 117.8 . . ? C3S C1S H1S1 129.8 4_556 . ? C2S C1S H1S2 106.3 4_556 . ? C2S C1S H1S2 106.3 . . ? C3S C1S H1S2 129.8 . . ? C3S C1S H1S2 117.8 4_556 . ? H1S1 C1S H1S2 106.4 . . ? C3S C2S C1S 95(2) . . ? C3S C2S H2S1 112.7 . . ? C1S C2S H2S1 112.7 . . ? C3S C2S H2S2 112.7 . . ? C1S C2S H2S2 112.7 . . ? H2S1 C2S H2S2 110.2 . . ? C2S C3S C3S 108.5(12) . 4_556 ? C3S C3S C1S 67.6(7) 4_556 . ? C2S C3S H3S1 110 . . ? C3S C3S H3S1 110 4_556 . ? C1S C3S H3S1 110 . . ? C2S C3S H3S2 110 . . ? C3S C3S H3S2 110 4_556 . ? C1S C3S H3S2 139.6 . . ? H3S1 C3S H3S2 108.4 . . ? #===END data_(3)-jun1506 _database_code_depnum_ccdc_archive 'CCDC 799145' #TrackingRef 'MPC_ChemComm_Nov2010.cif' _audit_creation_date 2006-06-19T13:40:55-00:00 _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 'C26 H60 Mg2 N8 Si4' _chemical_formula_sum 'C26 H60 Mg2 N8 Si4' _chemical_formula_weight 645.8 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 12.3450(2) _cell_length_b 16.7408(3) _cell_length_c 18.0363(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3727.48(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 16889 _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 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.151 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.221 _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_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.765528E-1 _diffrn_orient_matrix_ub_12 0.84448E-2 _diffrn_orient_matrix_ub_13 -0.163446E-1 _diffrn_orient_matrix_ub_21 0.214967E-1 _diffrn_orient_matrix_ub_22 0.116458E-1 _diffrn_orient_matrix_ub_23 0.523515E-1 _diffrn_orient_matrix_ub_31 0.154687E-1 _diffrn_orient_matrix_ub_32 -0.579763E-1 _diffrn_orient_matrix_ub_33 0.81352E-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 0.0622 _diffrn_reflns_av_unetI/netI 0.028 _diffrn_reflns_number 30490 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 26.01 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 3652 _reflns_number_gt 3095 _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 ; Atom C6 is disordered , with the lower occupancy site left isotropic. 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^)+(0.0341P)^2^+2.0133P] 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 3652 _refine_ls_number_parameters 186 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.043 _refine_ls_R_factor_gt 0.033 _refine_ls_wR_factor_ref 0.0868 _refine_ls_wR_factor_gt 0.0818 _refine_ls_goodness_of_fit_ref 1.08 _refine_ls_restrained_S_all 1.08 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.256 _refine_diff_density_min -0.216 _refine_diff_density_rms 0.046 #----------------------------------------------------------------------------# # 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' 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 0.46241(4) 0.59657(2) 0.70769(3) 0.02293(12) Uani 1 1 d . A . Si2 Si 0.39155(4) 0.42687(3) 0.73467(3) 0.02539(13) Uani 1 1 d . A . Mg Mg 0.48267(4) 0.47428(3) 0.57668(3) 0.02145(14) Uani 1 1 d . . . N1 N 0.62645(10) 0.49202(8) 0.50894(8) 0.0224(3) Uani 1 1 d . . . N2 N 0.55754(11) 0.37120(8) 0.53874(8) 0.0278(3) Uani 1 1 d . . . N3 N 0.74357(11) 0.37833(9) 0.50816(8) 0.0307(3) Uani 1 1 d . . . N4 N 0.44220(11) 0.50058(7) 0.68006(7) 0.0217(3) Uani 1 1 d . . . C1 C 0.64486(13) 0.41144(10) 0.51821(9) 0.0240(4) Uani 1 1 d . A . C2 C 0.72415(13) 0.54239(11) 0.50607(10) 0.0306(4) Uani 1 1 d . A . H2A H 0.7545 0.5484 0.5566 0.037 Uiso 1 1 calc R . . H2B H 0.7049 0.5962 0.4874 0.037 Uiso 1 1 calc R . . C3 C 0.80840(15) 0.50495(12) 0.45543(11) 0.0387(5) Uani 1 1 d . . . H3A H 0.7786 0.4991 0.4048 0.046 Uiso 1 1 calc R A . H3B H 0.8733 0.5396 0.4528 0.046 Uiso 1 1 calc R . . C4 C 0.83907(15) 0.42386(13) 0.48595(12) 0.0419(5) Uani 1 1 d . A . H4A H 0.8795 0.3936 0.4477 0.05 Uiso 1 1 calc R . . H4B H 0.8873 0.4309 0.5293 0.05 Uiso 1 1 calc R . . C8 C 0.33753(16) 0.65968(11) 0.69973(13) 0.0424(5) Uani 1 1 d . . . H8A H 0.2798 0.6366 0.7303 0.064 Uiso 1 1 calc R A . H8B H 0.314 0.6614 0.6478 0.064 Uiso 1 1 calc R . . H8C H 0.3535 0.714 0.7169 0.064 Uiso 1 1 calc R . . C9 C 0.51113(17) 0.60657(11) 0.80586(11) 0.0378(4) Uani 1 1 d . . . H9A H 0.4583 0.5822 0.8395 0.057 Uiso 1 1 calc R A . H9B H 0.5195 0.6633 0.8181 0.057 Uiso 1 1 calc R . . H9C H 0.5811 0.5795 0.8112 0.057 Uiso 1 1 calc R . . C10 C 0.56848(15) 0.64470(10) 0.64798(11) 0.0345(4) Uani 1 1 d . . . H10A H 0.6356 0.6135 0.6506 0.052 Uiso 1 1 calc R A . H10B H 0.5822 0.6991 0.6656 0.052 Uiso 1 1 calc R . . H10C H 0.543 0.6466 0.5965 0.052 Uiso 1 1 calc R . . C11 C 0.49529(18) 0.38383(13) 0.79913(14) 0.0512(6) Uani 1 1 d . . . H11A H 0.5245 0.4263 0.8307 0.077 Uiso 1 1 calc R A . H11B H 0.5541 0.3599 0.7702 0.077 Uiso 1 1 calc R . . H11C H 0.4615 0.3428 0.8302 0.077 Uiso 1 1 calc R . . C12 C 0.27452(17) 0.45993(13) 0.79345(12) 0.0439(5) Uani 1 1 d . . . H12A H 0.2974 0.5043 0.8253 0.066 Uiso 1 1 calc R A . H12B H 0.25 0.4153 0.8243 0.066 Uiso 1 1 calc R . . H12C H 0.215 0.4776 0.7614 0.066 Uiso 1 1 calc R . . C13 C 0.33991(18) 0.34230(11) 0.67658(12) 0.0451(5) Uani 1 1 d . . . H13A H 0.2851 0.3623 0.642 0.068 Uiso 1 1 calc R A . H13B H 0.3076 0.3016 0.7087 0.068 Uiso 1 1 calc R . . H13C H 0.4001 0.3188 0.6486 0.068 Uiso 1 1 calc R . . C5 C 0.76366(16) 0.29433(12) 0.52629(12) 0.0438(5) Uani 0.829(6) 1 d P A 1 H5A H 0.8329 0.2899 0.5537 0.053 Uiso 0.829(6) 1 calc PR A 1 H5B H 0.7707 0.2633 0.4798 0.053 Uiso 0.829(6) 1 calc PR A 1 C6 C 0.6737(2) 0.25930(14) 0.57264(15) 0.0433(8) Uani 0.829(6) 1 d P A 1 H6A H 0.6791 0.2003 0.5725 0.052 Uiso 0.829(6) 1 calc PR A 1 H6B H 0.6807 0.278 0.6245 0.052 Uiso 0.829(6) 1 calc PR A 1 C7 C 0.56650(17) 0.28411(10) 0.54220(13) 0.0432(5) Uani 0.829(6) 1 d P A 1 H7A H 0.5574 0.2615 0.4918 0.052 Uiso 0.829(6) 1 calc PR A 1 H7B H 0.508 0.2626 0.574 0.052 Uiso 0.829(6) 1 calc PR A 1 C5A C 0.76366(16) 0.29433(12) 0.52629(12) 0.0438(5) Uani 0.171(6) 1 d P A 2 H5A1 H 0.7852 0.2887 0.5789 0.053 Uiso 0.171(6) 1 calc PR A 2 H5A2 H 0.8221 0.2724 0.4947 0.053 Uiso 0.171(6) 1 calc PR A 2 C6A C 0.6524(9) 0.2487(7) 0.5110(7) 0.040(4) Uiso 0.171(6) 1 d P A 2 H6A1 H 0.6407 0.2454 0.4568 0.048 Uiso 0.171(6) 1 calc PR A 2 H6A2 H 0.6583 0.1935 0.5303 0.048 Uiso 0.171(6) 1 calc PR A 2 C7A C 0.56650(17) 0.28411(10) 0.54220(13) 0.0432(5) Uani 0.171(6) 1 d P A 2 H7A1 H 0.5651 0.2685 0.5951 0.052 Uiso 0.171(6) 1 calc PR A 2 H7A2 H 0.5007 0.2614 0.519 0.052 Uiso 0.171(6) 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 Si1 0.0251(2) 0.0185(2) 0.0253(2) -0.00212(17) 0.00086(19) 0.00158(17) Si2 0.0276(3) 0.0229(2) 0.0256(3) 0.00372(18) 0.0034(2) -0.00250(18) Mg 0.0228(3) 0.0207(3) 0.0209(3) 0.0006(2) 0.0033(2) 0.0028(2) N1 0.0215(7) 0.0228(6) 0.0231(7) 0.0009(5) 0.0024(6) 0.0012(5) N2 0.0283(7) 0.0191(7) 0.0360(8) 0.0013(6) 0.0033(6) 0.0042(6) N3 0.0258(7) 0.0347(8) 0.0316(8) 0.0046(6) 0.0040(6) 0.0120(6) N4 0.0252(7) 0.0195(6) 0.0205(7) -0.0002(5) 0.0032(6) -0.0007(5) C1 0.0256(8) 0.0285(8) 0.0178(8) -0.0008(6) 0.0001(7) 0.0078(7) C2 0.0253(9) 0.0360(9) 0.0307(10) 0.0036(8) 0.0017(7) -0.0040(7) C3 0.0267(9) 0.0527(12) 0.0366(11) 0.0088(9) 0.0091(8) 0.0007(9) C4 0.0261(10) 0.0604(13) 0.0392(12) 0.0101(10) 0.0086(9) 0.0118(9) C8 0.0379(11) 0.0294(10) 0.0600(14) -0.0020(9) -0.0010(10) 0.0100(8) C9 0.0467(11) 0.0359(10) 0.0309(10) -0.0094(8) -0.0025(9) -0.0031(9) C10 0.0391(10) 0.0236(8) 0.0410(11) 0.0003(8) 0.0048(9) -0.0046(8) C11 0.0487(12) 0.0424(11) 0.0624(15) 0.0266(11) -0.0095(11) -0.0030(10) C12 0.0432(12) 0.0492(12) 0.0394(11) 0.0016(9) 0.0146(10) -0.0054(10) C13 0.0566(13) 0.0299(10) 0.0489(13) -0.0038(9) 0.0133(11) -0.0176(9) C5 0.0418(11) 0.0390(11) 0.0506(12) 0.0064(9) 0.0042(10) 0.0227(9) C6 0.0513(15) 0.0280(12) 0.0508(18) 0.0084(10) 0.0030(13) 0.0146(11) C7 0.0447(11) 0.0210(8) 0.0639(14) 0.0031(9) 0.0031(10) 0.0064(8) C5A 0.0418(11) 0.0390(11) 0.0506(12) 0.0064(9) 0.0042(10) 0.0227(9) C7A 0.0447(11) 0.0210(8) 0.0639(14) 0.0031(9) 0.0031(10) 0.0064(8) #----------------------------------------------------------------------------# # 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 N4 1.7009(13) . ? Si1 C8 1.8745(19) . ? Si1 C10 1.8770(18) . ? Si1 C9 1.8774(19) . ? Si2 N4 1.6983(13) . ? Si2 C13 1.873(2) . ? Si2 C11 1.874(2) . ? Si2 C12 1.876(2) . ? Mg N4 1.9798(14) . ? Mg N2 2.0738(14) . ? Mg N1 2.1255(14) 5_666 ? Mg N1 2.1752(14) . ? N1 C1 1.378(2) . ? N1 C2 1.473(2) . ? N1 Mg 2.1255(14) 5_666 ? N2 C1 1.324(2) . ? N2 C7 1.464(2) . ? N3 C1 1.351(2) . ? N3 C4 1.460(2) . ? N3 C5 1.465(2) . ? C2 C3 1.520(2) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 C4 1.513(3) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? 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 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C5 C6 1.508(3) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 C7 1.492(3) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C6A H6A1 0.99 . ? C6A H6A2 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 N4 Si1 C8 112.91(8) . . ? N4 Si1 C10 109.87(7) . . ? C8 Si1 C10 106.73(9) . . ? N4 Si1 C9 114.05(8) . . ? C8 Si1 C9 106.58(10) . . ? C10 Si1 C9 106.22(9) . . ? N4 Si2 C13 110.49(8) . . ? N4 Si2 C11 112.81(8) . . ? C13 Si2 C11 106.80(11) . . ? N4 Si2 C12 113.39(8) . . ? C13 Si2 C12 106.09(10) . . ? C11 Si2 C12 106.81(11) . . ? N4 Mg N2 127.47(6) . . ? N4 Mg N1 117.73(6) . 5_666 ? N2 Mg N1 105.28(6) . 5_666 ? N4 Mg N1 134.79(6) . . ? N2 Mg N1 64.19(5) . . ? N1 Mg N1 94.17(5) 5_666 . ? C1 N1 C2 115.45(13) . . ? C1 N1 Mg 116.90(10) . 5_666 ? C2 N1 Mg 109.97(10) . 5_666 ? C1 N1 Mg 86.15(9) . . ? C2 N1 Mg 140.02(11) . . ? Mg N1 Mg 85.83(5) 5_666 . ? C1 N2 C7 117.21(14) . . ? C1 N2 Mg 91.82(10) . . ? C7 N2 Mg 148.06(13) . . ? C1 N3 C4 123.44(15) . . ? C1 N3 C5 121.11(15) . . ? C4 N3 C5 115.19(14) . . ? Si2 N4 Si1 124.79(8) . . ? Si2 N4 Mg 118.52(7) . . ? Si1 N4 Mg 116.68(7) . . ? N2 C1 N3 124.27(15) . . ? N2 C1 N1 113.43(14) . . ? N3 C1 N1 122.29(15) . . ? N1 C2 C3 110.22(15) . . ? N1 C2 H2A 109.6 . . ? C3 C2 H2A 109.6 . . ? N1 C2 H2B 109.6 . . ? C3 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? C4 C3 C2 108.83(15) . . ? C4 C3 H3A 109.9 . . ? C2 C3 H3A 109.9 . . ? C4 C3 H3B 109.9 . . ? C2 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? N3 C4 C3 111.48(15) . . ? N3 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? N3 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 108 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si1 C9 H9A 109.5 . . ? Si1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si2 C11 H11A 109.5 . . ? Si2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si2 C13 H13A 109.5 . . ? Si2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C5 C6 111.86(16) . . ? N3 C5 H5A 109.2 . . ? C6 C5 H5A 109.2 . . ? N3 C5 H5B 109.2 . . ? C6 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C7 C6 C5 109.93(19) . . ? C7 C6 H6A 109.7 . . ? C5 C6 H6A 109.7 . . ? C7 C6 H6B 109.7 . . ? C5 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? N2 C7 C6 111.10(17) . . ? N2 C7 H7A 109.4 . . ? C6 C7 H7A 109.4 . . ? N2 C7 H7B 109.4 . . ? C6 C7 H7B 109.4 . . ? H7A C7 H7B 108 . . ? H6A1 C6A H6A2 107.7 . . ? #===END data_(4)-apr609 _database_code_depnum_ccdc_archive 'CCDC 799146' #TrackingRef 'MPC_ChemComm_Nov2010.cif' _audit_creation_date 2009-05-15T08:42:25-00:00 _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 'C30 H68 Mg2 N8 O2 Si4' _chemical_formula_sum 'C30 H68 Mg2 N8 O2 Si4' _chemical_formula_weight 733.90 _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 11.6231(3) _cell_length_b 11.1599(2) _cell_length_c 17.1244(4) _cell_angle_alpha 90 _cell_angle_beta 103.218(1) _cell_angle_gamma 90 _cell_volume 2162.40(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 54529 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.127 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.202 _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 Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.127685E-1 _diffrn_orient_matrix_ub_12 0.805418E-1 _diffrn_orient_matrix_ub_13 0.26145E-1 _diffrn_orient_matrix_ub_21 -0.407251E-1 _diffrn_orient_matrix_ub_22 0.386361E-1 _diffrn_orient_matrix_ub_23 -0.516195E-1 _diffrn_orient_matrix_ub_31 -0.77388E-1 _diffrn_orient_matrix_ub_32 -0.70432E-2 _diffrn_orient_matrix_ub_33 0.158149E-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 0.0488 _diffrn_reflns_av_unetI/netI 0.0222 _diffrn_reflns_number 33110 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.85 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 4909 _reflns_number_gt 4352 _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 ; One of the SiMe3 groups of the amide ligand is disordered over two positions and was refined with SADI restraints; the carbon atoms of the lower occupancy site were left isotropic. The THF was also disordered over two positions and was refined with SADI restraints; the carbon atoms of both orientations were left isotropic. 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^)+(0.0564P)^2^+1.8806P] 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 4909 _refine_ls_number_parameters 221 _refine_ls_number_restraints 64 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.13 _refine_ls_wR_factor_gt 0.1239 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.603 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.051 #----------------------------------------------------------------------------# # 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 0.79240(5) 0.14533(4) 0.03920(3) 0.03107(14) Uani 1 1 d . A . Mg Mg 0.85376(5) 0.39604(5) -0.02142(3) 0.02202(15) Uani 1 1 d . . . O O 0.79010(12) 0.54486(11) -0.08843(7) 0.0310(3) Uani 1 1 d D A . N1 N 0.88997(12) 0.48155(13) 0.08720(8) 0.0254(3) Uani 1 1 d . A . N2 N 1.02186(13) 0.64842(13) 0.08424(9) 0.0276(3) Uani 1 1 d . . . N3 N 0.91703(15) 0.62993(15) 0.18151(10) 0.0352(4) Uani 1 1 d . A . N4 N 0.73838(13) 0.26003(13) -0.02344(9) 0.0280(3) Uani 1 1 d D A . C1 C 0.94555(14) 0.58264(16) 0.11253(10) 0.0252(3) Uani 1 1 d . . . C2 C 0.81469(17) 0.45603(17) 0.14470(11) 0.0324(4) Uani 1 1 d . . . H2A H 0.8509 0.3933 0.1835 0.039 Uiso 1 1 calc R A . H2B H 0.7351 0.429 0.1161 0.039 Uiso 1 1 calc R . . C3 C 0.8076(2) 0.5749(2) 0.18729(14) 0.0437(5) Uani 1 1 d . A . H3A H 0.7387 0.6229 0.1595 0.052 Uiso 1 1 calc R . . H3B H 0.8036 0.5626 0.2439 0.052 Uiso 1 1 calc R . . C4 C 0.9455(2) 0.7546(2) 0.18232(14) 0.0435(5) Uani 1 1 d . . . H4A H 0.9739 0.7847 0.2378 0.052 Uiso 1 1 calc R A . H4B H 0.8768 0.8029 0.1546 0.052 Uiso 1 1 calc R . . C5 C 1.04341(19) 0.75613(19) 0.13680(13) 0.0394(5) Uani 1 1 d . A . H5A H 1.0396 0.8301 0.1044 0.047 Uiso 1 1 calc R . . H5B H 1.1219 0.7516 0.1743 0.047 Uiso 1 1 calc R . . C6 C 0.7830(3) -0.0048(2) -0.01139(19) 0.0601(7) Uani 1 1 d . . . H6A H 0.8199 -0.0002 -0.0573 0.09 Uiso 1 1 calc R A . H6B H 0.6999 -0.0279 -0.03 0.09 Uiso 1 1 calc R . . H6C H 0.8243 -0.0647 0.0267 0.09 Uiso 1 1 calc R . . C7 C 0.95375(19) 0.1702(2) 0.08565(14) 0.0429(5) Uani 1 1 d . . . H7A H 0.964 0.2478 0.1131 0.064 Uiso 1 1 calc R A . H7B H 0.9985 0.1694 0.0436 0.064 Uiso 1 1 calc R . . H7C H 0.9827 0.1062 0.1244 0.064 Uiso 1 1 calc R . . C8 C 0.7196(2) 0.1250(2) 0.12553(14) 0.0549(6) Uani 1 1 d . . . H8A H 0.7215 0.2009 0.1546 0.082 Uiso 1 1 calc R A . H8B H 0.7619 0.0634 0.1618 0.082 Uiso 1 1 calc R . . H8C H 0.6373 0.1 0.1052 0.082 Uiso 1 1 calc R . . Si2 Si 0.60882(10) 0.23825(14) -0.09423(8) 0.0337(3) Uani 0.651(4) 1 d PD A 1 C9 C 0.4904(4) 0.1726(5) -0.0513(4) 0.084(4) Uani 0.651(4) 1 d PD A 1 H9A H 0.5182 0.0971 -0.0242 0.126 Uiso 0.651(4) 1 calc PR A 1 H9B H 0.4205 0.1573 -0.0944 0.126 Uiso 0.651(4) 1 calc PR A 1 H9C H 0.47 0.2287 -0.0125 0.126 Uiso 0.651(4) 1 calc PR A 1 C11 C 0.5505(4) 0.3777(5) -0.1458(4) 0.109(3) Uani 0.651(4) 1 d PD A 1 H11A H 0.6111 0.4147 -0.1694 0.163 Uiso 0.651(4) 1 calc PR A 1 H11B H 0.5286 0.433 -0.1072 0.163 Uiso 0.651(4) 1 calc PR A 1 H11C H 0.4806 0.3595 -0.1884 0.163 Uiso 0.651(4) 1 calc PR A 1 C10 C 0.6218(5) 0.1358(6) -0.1800(3) 0.099(2) Uani 0.651(4) 1 d PD A 1 H10A H 0.6532 0.058 -0.1586 0.148 Uiso 0.651(4) 1 calc PR A 1 H10B H 0.6752 0.1718 -0.2101 0.148 Uiso 0.651(4) 1 calc PR A 1 H10C H 0.5436 0.1246 -0.2156 0.148 Uiso 0.651(4) 1 calc PR A 1 C12 C 0.7959(5) 0.5769(5) -0.1679(3) 0.0367(14) Uiso 0.521(7) 1 d PD A 1 H12A H 0.7576 0.5143 -0.206 0.044 Uiso 0.521(7) 1 calc PR A 1 H12B H 0.8795 0.5838 -0.1714 0.044 Uiso 0.521(7) 1 calc PR A 1 C13 C 0.7348(4) 0.6932(5) -0.1889(3) 0.0462(12) Uiso 0.521(7) 1 d PD A 1 H13A H 0.6879 0.6927 -0.245 0.055 Uiso 0.521(7) 1 calc PR A 1 H13B H 0.7923 0.76 -0.1821 0.055 Uiso 0.521(7) 1 calc PR A 1 C14 C 0.6558(4) 0.7046(3) -0.1310(2) 0.0317(10) Uiso 0.521(7) 1 d PD A 1 H14A H 0.5786 0.6652 -0.1522 0.038 Uiso 0.521(7) 1 calc PR A 1 H14B H 0.6421 0.7898 -0.1197 0.038 Uiso 0.521(7) 1 calc PR A 1 C15 C 0.72404(18) 0.6417(2) -0.05715(14) 0.0382(11) Uiso 0.521(7) 1 d PD A 1 H15A H 0.7792 0.6976 -0.0224 0.046 Uiso 0.521(7) 1 calc PR A 1 H15B H 0.6699 0.6074 -0.026 0.046 Uiso 0.521(7) 1 calc PR A 1 Si2A Si 0.59637(18) 0.2838(2) -0.07376(14) 0.0364(6) Uani 0.349(4) 1 d PRD A 2 C9A C 0.48362(18) 0.1734(2) -0.05532(14) 0.044(3) Uiso 0.349(4) 1 d PRD A 2 H9A1 H 0.5121 0.0917 -0.0603 0.065 Uiso 0.349(4) 1 calc PR A 2 H9A2 H 0.409 0.1857 -0.0948 0.065 Uiso 0.349(4) 1 calc PR A 2 H9A3 H 0.4709 0.1851 -0.0012 0.065 Uiso 0.349(4) 1 calc PR A 2 C10A C 0.5930(10) 0.2650(10) -0.1833(5) 0.086(3) Uiso 0.349(4) 1 d PD A 2 H10D H 0.6267 0.187 -0.192 0.129 Uiso 0.349(4) 1 calc PR A 2 H10E H 0.6394 0.3289 -0.2006 0.129 Uiso 0.349(4) 1 calc PR A 2 H10F H 0.5111 0.2693 -0.2144 0.129 Uiso 0.349(4) 1 calc PR A 2 C11A C 0.5325(9) 0.4300(7) -0.0612(6) 0.080(3) Uiso 0.349(4) 1 d PD A 2 H11D H 0.5324 0.4421 -0.0045 0.121 Uiso 0.349(4) 1 calc PR A 2 H11E H 0.4512 0.4333 -0.0934 0.121 Uiso 0.349(4) 1 calc PR A 2 H11F H 0.5796 0.4929 -0.0788 0.121 Uiso 0.349(4) 1 calc PR A 2 C12A C 0.7973(5) 0.5491(6) -0.1743(3) 0.0351(14) Uiso 0.479(7) 1 d PD A 2 H12C H 0.7772 0.4705 -0.2007 0.042 Uiso 0.479(7) 1 calc PR A 2 H12D H 0.8772 0.5732 -0.1795 0.042 Uiso 0.479(7) 1 calc PR A 2 C13A C 0.7069(4) 0.6423(5) -0.2093(3) 0.0384(12) Uiso 0.479(7) 1 d PD A 2 H13C H 0.7305 0.6856 -0.2536 0.046 Uiso 0.479(7) 1 calc PR A 2 H13D H 0.6287 0.6048 -0.2302 0.046 Uiso 0.479(7) 1 calc PR A 2 C14A C 0.7027(6) 0.7247(5) -0.1425(3) 0.0577(16) Uiso 0.479(7) 1 d PD A 2 H14C H 0.6201 0.7488 -0.1445 0.069 Uiso 0.479(7) 1 calc PR A 2 H14D H 0.7495 0.7978 -0.1464 0.069 Uiso 0.479(7) 1 calc PR A 2 C15A C 0.7540(4) 0.6587(4) -0.0649(2) 0.0311(10) Uiso 0.479(7) 1 d PD A 2 H15C H 0.8223 0.703 -0.0326 0.037 Uiso 0.479(7) 1 calc PR A 2 H15D H 0.6937 0.6492 -0.0328 0.037 Uiso 0.479(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 Si1 0.0357(3) 0.0251(3) 0.0325(3) 0.00343(19) 0.0079(2) -0.00490(19) Mg 0.0227(3) 0.0221(3) 0.0228(3) -0.0006(2) 0.0083(2) -0.0025(2) O 0.0389(7) 0.0273(6) 0.0264(6) 0.0026(5) 0.0069(5) 0.0018(5) N1 0.0259(7) 0.0278(7) 0.0248(7) -0.0027(5) 0.0107(5) -0.0032(5) N2 0.0286(7) 0.0268(7) 0.0302(7) -0.0076(6) 0.0122(6) -0.0053(6) N3 0.0386(9) 0.0391(9) 0.0339(8) -0.0133(7) 0.0204(7) -0.0088(7) N4 0.0236(7) 0.0287(7) 0.0313(7) 0.0044(6) 0.0052(6) -0.0062(6) C1 0.0240(8) 0.0296(8) 0.0234(7) -0.0032(6) 0.0082(6) 0.0005(6) C2 0.0343(9) 0.0365(10) 0.0307(9) -0.0030(7) 0.0167(7) -0.0058(8) C3 0.0473(12) 0.0472(12) 0.0455(11) -0.0135(9) 0.0291(10) -0.0121(10) C4 0.0529(13) 0.0406(11) 0.0441(11) -0.0178(9) 0.0254(10) -0.0121(9) C5 0.0421(11) 0.0366(10) 0.0446(11) -0.0182(9) 0.0209(9) -0.0122(8) C6 0.0678(17) 0.0309(11) 0.0841(19) -0.0114(12) 0.0224(14) -0.0085(11) C7 0.0378(11) 0.0418(11) 0.0443(11) 0.0091(9) -0.0008(9) 0.0037(9) C8 0.0677(16) 0.0602(15) 0.0398(12) 0.0115(10) 0.0185(11) -0.0178(12) Si2 0.0231(4) 0.0345(7) 0.0405(6) 0.0039(5) 0.0012(4) -0.0070(4) C9 0.029(2) 0.103(5) 0.114(6) 0.038(4) 0.002(2) -0.036(3) C11 0.047(2) 0.084(4) 0.159(6) 0.078(4) -0.051(3) -0.033(2) C10 0.060(3) 0.168(7) 0.057(3) -0.047(3) -0.011(2) -0.001(3) Si2A 0.0235(9) 0.0394(14) 0.0436(12) 0.0037(9) 0.0021(7) -0.0124(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 Si1 N4 1.6956(15) . ? Si1 C8 1.878(2) . ? Si1 C6 1.878(2) . ? Si1 C7 1.883(2) . ? Si1 Mg 3.1229(7) . ? Mg N4 2.0205(15) . ? Mg N1 2.0468(15) . ? Mg N2 2.0507(15) 3_765 ? Mg O 2.0578(14) . ? Mg Si2A 3.177(2) . ? O C12 1.423(5) . ? O C15A 1.425(4) . ? O C12A 1.493(5) . ? O C15 1.494(3) . ? N1 C1 1.323(2) . ? N1 C2 1.487(2) . ? N2 C1 1.325(2) . ? N2 C5 1.488(2) . ? N2 Mg 2.0507(15) 3_765 ? N3 C1 1.401(2) . ? N3 C4 1.430(3) . ? N3 C3 1.436(3) . ? N4 Si2A 1.699(2) . ? N4 Si2 1.7209(19) . ? C2 C3 1.525(3) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 C5 1.519(3) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? Si2 C11 1.840(4) . ? Si2 C9 1.853(4) . ? Si2 C10 1.894(5) . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C12 C13 1.484(6) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.503(5) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 C15 1.505(4) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? Si2A C11A 1.825(8) . ? Si2A C9A 1.8772 . ? Si2A C10A 1.879(8) . ? C9A H9A1 0.98 . ? C9A H9A2 0.98 . ? C9A H9A3 0.98 . ? C10A H10D 0.98 . ? C10A H10E 0.98 . ? C10A H10F 0.98 . ? C11A H11D 0.98 . ? C11A H11E 0.98 . ? C11A H11F 0.98 . ? C12A C13A 1.502(6) . ? C12A H12C 0.99 . ? C12A H12D 0.99 . ? C13A C14A 1.478(7) . ? C13A H13C 0.99 . ? C13A H13D 0.99 . ? C14A C15A 1.517(6) . ? C14A H14C 0.99 . ? C14A H14D 0.99 . ? C15A H15C 0.99 . ? C15A H15D 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 N4 Si1 C8 114.90(11) . . ? N4 Si1 C6 114.06(11) . . ? C8 Si1 C6 105.44(13) . . ? N4 Si1 C7 110.19(9) . . ? C8 Si1 C7 105.65(11) . . ? C6 Si1 C7 105.87(12) . . ? C8 Si1 Mg 123.25(9) . . ? C6 Si1 Mg 129.77(10) . . ? C7 Si1 Mg 74.18(7) . . ? N4 Mg N1 111.32(6) . . ? N4 Mg N2 110.73(6) . 3_765 ? N1 Mg N2 124.50(6) . 3_765 ? N4 Mg O 116.37(6) . . ? N1 Mg O 95.94(6) . . ? N2 Mg O 96.28(6) 3_765 . ? N4 Mg Si1 29.72(4) . . ? N1 Mg Si1 97.52(5) . . ? N2 Mg Si1 101.51(5) 3_765 . ? O Mg Si1 145.91(4) . . ? N1 Mg Si2A 115.14(7) . . ? N2 Mg Si2A 119.20(7) 3_765 . ? O Mg Si2A 88.03(6) . . ? Si1 Mg Si2A 57.91(4) . . ? C12 O C15A 97.3(3) . . ? C15A O C12A 109.6(3) . . ? C12 O C15 107.6(2) . . ? C12A O C15 118.6(2) . . ? C12 O Mg 130.3(2) . . ? C15A O Mg 130.84(18) . . ? C12A O Mg 118.8(2) . . ? C15 O Mg 122.17(11) . . ? C1 N1 C2 105.28(13) . . ? C1 N1 Mg 132.77(11) . . ? C2 N1 Mg 118.86(11) . . ? C1 N2 C5 105.10(14) . . ? C1 N2 Mg 131.96(12) . 3_765 ? C5 N2 Mg 118.12(11) . 3_765 ? C1 N3 C4 106.01(15) . . ? C1 N3 C3 106.32(15) . . ? C4 N3 C3 128.51(18) . . ? Si1 N4 Si2A 127.94(11) . . ? Si1 N4 Si2 118.48(9) . . ? Si1 N4 Mg 114.07(8) . . ? Si2A N4 Mg 117.10(11) . . ? Si2 N4 Mg 126.06(9) . . ? N1 C1 N2 132.07(15) . . ? N1 C1 N3 113.93(15) . . ? N2 C1 N3 113.99(15) . . ? N1 C2 C3 104.74(14) . . ? N1 C2 H2A 110.8 . . ? C3 C2 H2A 110.8 . . ? N1 C2 H2B 110.8 . . ? C3 C2 H2B 110.8 . . ? H2A C2 H2B 108.9 . . ? N3 C3 C2 101.16(15) . . ? N3 C3 H3A 111.5 . . ? C2 C3 H3A 111.5 . . ? N3 C3 H3B 111.5 . . ? C2 C3 H3B 111.5 . . ? H3A C3 H3B 109.4 . . ? N3 C4 C5 101.82(16) . . ? N3 C4 H4A 111.4 . . ? C5 C4 H4A 111.4 . . ? N3 C4 H4B 111.4 . . ? C5 C4 H4B 111.4 . . ? H4A C4 H4B 109.3 . . ? N2 C5 C4 105.03(15) . . ? N2 C5 H5A 110.7 . . ? C4 C5 H5A 110.7 . . ? N2 C5 H5B 110.7 . . ? C4 C5 H5B 110.7 . . ? H5A C5 H5B 108.8 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N4 Si2 C11 112.70(17) . . ? N4 Si2 C9 112.7(2) . . ? C11 Si2 C9 107.4(3) . . ? N4 Si2 C10 114.80(18) . . ? C11 Si2 C10 102.9(3) . . ? C9 Si2 C10 105.5(3) . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2 C11 H11A 109.5 . . ? Si2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si2 C10 H10A 109.5 . . ? Si2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O C12 C13 109.1(4) . . ? O C12 H12A 109.9 . . ? C13 C12 H12A 109.9 . . ? O C12 H12B 109.9 . . ? C13 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? C12 C13 C14 104.2(3) . . ? C12 C13 H13A 110.9 . . ? C14 C13 H13A 110.9 . . ? C12 C13 H13B 110.9 . . ? C14 C13 H13B 110.9 . . ? H13A C13 H13B 108.9 . . ? C13 C14 C15 103.3(3) . . ? C13 C14 H14A 111.1 . . ? C15 C14 H14A 111.1 . . ? C13 C14 H14B 111.1 . . ? C15 C14 H14B 111.1 . . ? H14A C14 H14B 109.1 . . ? O C15 C14 104.6(2) . . ? O C15 H15A 110.8 . . ? C14 C15 H15A 110.8 . . ? O C15 H15B 110.8 . . ? C14 C15 H15B 110.8 . . ? H15A C15 H15B 108.9 . . ? N4 Si2A C11A 117.0(4) . . ? N4 Si2A C9A 116.55(9) . . ? C11A Si2A C9A 104.4(3) . . ? N4 Si2A C10A 106.6(4) . . ? C11A Si2A C10A 107.5(4) . . ? C9A Si2A C10A 103.8(3) . . ? C11A Si2A Mg 89.8(3) . . ? C9A Si2A Mg 149.3 . . ? C10A Si2A Mg 97.4(3) . . ? Si2A C9A H9A1 109.5 . . ? Si2A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? Si2A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? Si2A C10A H10D 109.5 . . ? Si2A C10A H10E 109.5 . . ? H10D C10A H10E 109.5 . . ? Si2A C10A H10F 109.5 . . ? H10D C10A H10F 109.5 . . ? H10E C10A H10F 109.5 . . ? Si2A C11A H11D 109.5 . . ? Si2A C11A H11E 109.5 . . ? H11D C11A H11E 109.5 . . ? Si2A C11A H11F 109.5 . . ? H11D C11A H11F 109.5 . . ? H11E C11A H11F 109.5 . . ? O C12A C13A 102.9(4) . . ? O C12A H12C 111.2 . . ? C13A C12A H12C 111.2 . . ? O C12A H12D 111.2 . . ? C13A C12A H12D 111.2 . . ? H12C C12A H12D 109.1 . . ? C14A C13A C12A 105.4(4) . . ? C14A C13A H13C 110.7 . . ? C12A C13A H13C 110.7 . . ? C14A C13A H13D 110.7 . . ? C12A C13A H13D 110.7 . . ? H13C C13A H13D 108.8 . . ? C13A C14A C15A 107.4(4) . . ? C13A C14A H14C 110.2 . . ? C15A C14A H14C 110.2 . . ? C13A C14A H14D 110.2 . . ? C15A C14A H14D 110.2 . . ? H14C C14A H14D 108.5 . . ? O C15A C14A 105.5(3) . . ? O C15A H15C 110.6 . . ? C14A C15A H15C 110.6 . . ? O C15A H15D 110.6 . . ? C14A C15A H15D 110.6 . . ? H15C C15A H15D 108.8 . . ? #===END