# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Malcolm Chisholm' 'Judith Gallucci' 'Gulsah Yaman' _publ_contact_author_name 'Prof Malcolm Chisholm ' _publ_contact_author_email CHISHOLM@CHEMISTRY.OHIO-STATE.EDU _publ_section_title ; Synthesis and Coordination Chemistry of Tp*MI Complexes where M = Mg, Ca, Sr, Ba and Zn and Tp* = tris[3-(2-methoxy-1,1-dimethyl)pyrazolyl]hydroborate ; _publ_requested_category FM # Attachment 'gulsah_final.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2008-05-28 at 14:49:07 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : shelxl dreduc import struct data_Chisholm1609 _database_code_depnum_ccdc_archive 'CCDC 695433' _audit_creation_date 2008-05-28T14:49:07-00:00 _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_name_common 'Chisholm 1609' _chemical_formula_moiety 'C24 H40 B1 Mg1 N6 O3, C6 H6, I' _chemical_formula_sum 'C30 H46 B I Mg N6 O3' _chemical_formula_weight 700.75 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting cubic _symmetry_space_group_name_H-M P213 _symmetry_space_group_name_Hall 'P 2ac 2ab 3' _symmetry_Int_Tables_number 198 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' 'y, z, x' '-y+1/2, -z, x+1/2' 'y+1/2, -z+1/2, -x' '-y, z+1/2, -x+1/2' 'z, x, y' '-z, x+1/2, -y+1/2' '-z+1/2, -x, y+1/2' 'z+1/2, -x+1/2, -y' _cell_length_a 14.9023(2) _cell_length_b 14.9023(2) _cell_length_c 14.9023(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3309.48(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1109 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description 'triangular chunk' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_special_details ;Examination of the diffraction pattern on a Nonius Kappa CCD diffractometer indicated a cubic crystal system. All work was done at 150K using an Oxford Cryosystems Cryostream Cooler. The data collection strategy was set up to measure a hemisphere of reciprocal space with a redundancy factor of 2.1, which means that 90% of the reflections were measured at least 2.1 times. Phi and omega scans with a frame width of 1.0 degree were used for data collection. Data integration was done with Denzo and scaling and merging of the data was done with Scalepack. The Mg complex contains a crystallographic three-fold axis. Disorder is present in this Mg complex, and it was modeled with two sets of atoms using DFIX and SADI restraints: C(5), C(6), C(7), O(1), C(8) and C(5A), C(6A), C(7A), O(1A), C(8A). Atoms C(5), C(6), C(5A), C(6A), and C(8A) were kept isotropic. There is also a solvent molecule of benzene which sits on a three-fold axis. The two unique carbon atoms of this benzene molecule have large Uiso values. Refinement of their occupancy factors converged to 0.99, so it was assumed that the benzene molecule is fully occupied. It was kept isotropic. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.026 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.856 _exptl_absorpt_correction_T_max 0.884 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor, 1997)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.520958E-1 _diffrn_orient_matrix_ub_12 -0.263055E-1 _diffrn_orient_matrix_ub_13 0.331204E-1 _diffrn_orient_matrix_ub_21 0.191835E-1 _diffrn_orient_matrix_ub_22 -0.615264E-1 _diffrn_orient_matrix_ub_23 -0.186925E-1 _diffrn_orient_matrix_ub_31 0.376953E-1 _diffrn_orient_matrix_ub_32 -0.50435E-2 _diffrn_orient_matrix_ub_33 0.55286E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method "phi and omega scans'" _diffrn_reflns_av_R_equivalents 0.049 _diffrn_reflns_av_unetI/netI ? _diffrn_reflns_number 28583 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 1965 _reflns_number_gt 1907 _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-7 (Sheldrick, 197)' _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 ;For the methyl groups, the hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5 * Ueq(bonded carbon atom). The remaining hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(attached atom). Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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 'w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+4.0481P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 1965 _refine_ls_number_parameters 139 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.056 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1319 _refine_ls_wR_factor_gt 0.1308 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.181 _refine_ls_shift/su_max 0.094 _refine_ls_shift/su_mean 0.014 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(5) _refine_diff_density_max 0.574 _refine_diff_density_min -0.33 _refine_diff_density_rms 0.078 #----------------------------------------------------------------------------# # 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 I I 1.09731(3) 0.90269(3) 0.40269(3) 0.0554(3) Uani 1 3 d S . . Mg Mg 0.96340(11) 0.96340(11) 0.96340(11) 0.0345(6) Uani 1 3 d S . . N1 N 0.8631(4) 0.7887(3) 0.9245(4) 0.0589(15) Uani 1 1 d . . . N2 N 0.9131(4) 0.8282(3) 0.9911(3) 0.0513(13) Uani 1 1 d . A . C1 C 0.9228(5) 0.7672(4) 1.0567(5) 0.062(2) Uani 1 1 d . . . C2 C 0.8785(6) 0.6884(4) 1.0328(6) 0.075(2) Uani 1 1 d . A . H2 H 0.8739 0.6349 1.0672 0.09 Uiso 1 1 calc R . . C3 C 0.8429(7) 0.7040(5) 0.9497(6) 0.084(3) Uani 1 1 d . A . H3 H 0.8093 0.6621 0.9153 0.1 Uiso 1 1 calc R . . C4 C 0.9701(5) 0.7894(5) 1.1424(5) 0.0676(19) Uani 1 1 d D A . C5A C 0.9078(11) 0.7933(13) 1.2226(10) 0.079(5) Uiso 0.489(13) 1 d PD A 1 H5A H 0.8675 0.7413 1.2216 0.118 Uiso 0.489(13) 1 calc PR A 1 H5B H 0.8722 0.8486 1.2201 0.118 Uiso 0.489(13) 1 calc PR A 1 H5C H 0.9432 0.7925 1.278 0.118 Uiso 0.489(13) 1 calc PR A 1 C6A C 1.0315(10) 0.7065(9) 1.1574(12) 0.083(5) Uiso 0.489(13) 1 d PD A 1 H6A H 0.9942 0.6534 1.1687 0.125 Uiso 0.489(13) 1 calc PR A 1 H6B H 1.0706 0.7172 1.2091 0.125 Uiso 0.489(13) 1 calc PR A 1 H6C H 1.0682 0.6964 1.1038 0.125 Uiso 0.489(13) 1 calc PR A 1 C7A C 1.0301(14) 0.8655(9) 1.1335(14) 0.098(8) Uani 0.489(13) 1 d PD A 1 H7A H 1.0766 0.8494 1.0888 0.117 Uiso 0.489(13) 1 calc PR A 1 H7B H 1.061 0.8737 1.1917 0.117 Uiso 0.489(13) 1 calc PR A 1 O1A O 0.9923(9) 0.9518(7) 1.1074(8) 0.040(3) Uani 0.489(13) 1 d PD A 1 C8A C 0.9946(16) 1.0097(15) 1.1783(15) 0.102(7) Uiso 0.489(13) 1 d P A 1 H8A H 0.9622 1.0648 1.1627 0.154 Uiso 0.489(13) 1 calc PR A 1 H8B H 1.0571 1.0244 1.1926 0.154 Uiso 0.489(13) 1 calc PR A 1 H8C H 0.9662 0.9816 1.2305 0.154 Uiso 0.489(13) 1 calc PR A 1 C5 C 0.9112(14) 0.7501(14) 1.2187(14) 0.115(8) Uiso 0.511(13) 1 d PD A 2 H5D H 0.9392 0.763 1.2768 0.173 Uiso 0.511(13) 1 calc PR A 2 H5E H 0.9059 0.685 1.211 0.173 Uiso 0.511(13) 1 calc PR A 2 H5F H 0.8515 0.7775 1.2166 0.173 Uiso 0.511(13) 1 calc PR A 2 C6 C 1.0649(10) 0.7546(14) 1.152(2) 0.138(10) Uiso 0.511(13) 1 d PD A 2 H6D H 1.0895 0.7737 1.2101 0.207 Uiso 0.511(13) 1 calc PR A 2 H6E H 1.1022 0.7785 1.1035 0.207 Uiso 0.511(13) 1 calc PR A 2 H6F H 1.0646 0.6889 1.1491 0.207 Uiso 0.511(13) 1 calc PR A 2 C7 C 0.9679(6) 0.8919(7) 1.1591(6) 0.035(3) Uani 0.511(13) 1 d PD A 2 H7C H 0.9059 0.9154 1.1541 0.042 Uiso 0.511(13) 1 calc PR A 2 H7D H 0.9918 0.9067 1.2192 0.042 Uiso 0.511(13) 1 calc PR A 2 O1 O 1.0264(9) 0.9296(10) 1.0870(8) 0.057(4) Uani 0.511(13) 1 d PD A 2 C8 C 1.1172(11) 0.9489(17) 1.1135(15) 0.111(8) Uani 0.511(13) 1 d P A 2 H8D H 1.1493 0.9766 1.0632 0.167 Uiso 0.511(13) 1 calc PR A 2 H8E H 1.1473 0.8931 1.1308 0.167 Uiso 0.511(13) 1 calc PR A 2 H8F H 1.1168 0.9903 1.1647 0.167 Uiso 0.511(13) 1 calc PR A 2 B B 0.8385(4) 0.8385(4) 0.8385(4) 0.059(4) Uani 1 3 d S A . H1B1 H 0.7998 0.7998 0.7998 0.071 Uiso 1 3 calc SR . . C1B C 0.6474(12) 0.9294(12) 0.1907(13) 0.156(6) Uiso 1 1 d . . . H1B H 0.6485 0.9829 0.2253 0.187 Uiso 1 1 calc R . . C2B C 0.7063(10) 0.9176(11) 0.1319(11) 0.135(4) Uiso 1 1 d . . . H2B H 0.7595 0.9528 0.1305 0.162 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 I 0.0554(3) 0.0554(3) 0.0554(3) 0.0083(2) -0.0083(2) -0.0083(2) Mg 0.0345(6) 0.0345(6) 0.0345(6) -0.0022(7) -0.0022(7) -0.0022(7) N1 0.069(3) 0.043(3) 0.064(4) -0.012(3) 0.001(3) -0.020(3) N2 0.064(3) 0.041(2) 0.049(3) -0.004(2) 0.000(3) -0.008(2) C1 0.088(6) 0.037(3) 0.061(4) 0.007(3) 0.015(4) -0.004(3) C2 0.104(7) 0.037(3) 0.084(5) 0.006(4) 0.009(5) -0.011(4) C3 0.116(7) 0.044(4) 0.090(6) -0.024(4) 0.023(5) -0.028(4) C4 0.088(5) 0.060(4) 0.055(4) 0.012(3) -0.008(4) 0.004(4) C7A 0.12(2) 0.082(13) 0.089(14) 0.029(11) -0.023(14) -0.023(13) O1A 0.058(8) 0.032(5) 0.032(5) -0.003(4) -0.002(5) 0.006(4) C7 0.026(5) 0.041(6) 0.038(5) -0.004(5) -0.003(4) 0.013(5) O1 0.062(8) 0.056(8) 0.053(8) 0.001(6) -0.017(6) -0.005(6) C8 0.059(10) 0.17(2) 0.108(15) 0.003(14) -0.033(10) -0.025(11) B 0.059(4) 0.059(4) 0.059(4) -0.022(3) -0.022(3) -0.022(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 Mg O1 2.128(13) . ? Mg N2 2.189(5) . ? Mg O1A 2.195(12) . ? N1 C3 1.351(9) . ? N1 N2 1.374(7) . ? N1 B 1.526(7) . ? N2 C1 1.342(8) . ? C1 C2 1.393(10) . ? C1 C4 1.497(10) . ? C2 C3 1.367(13) . ? C2 H2 0.95 . ? C3 H3 0.95 . ? C4 C7A 1.450(19) . ? C4 C6 1.512(10) . ? C4 C5A 1.515(9) . ? C4 C7 1.547(13) . ? C4 C5 1.551(9) . ? C4 C6A 1.553(9) . ? C5A H5A 0.98 . ? C5A H5B 0.98 . ? C5A H5C 0.98 . ? C6A H6A 0.98 . ? C6A H6B 0.98 . ? C6A H6C 0.98 . ? C7A O1A 1.458(13) . ? C7A H7A 0.99 . ? C7A H7B 0.99 . ? O1A C8A 1.37(2) . ? C8A H8A 0.98 . ? C8A H8B 0.98 . ? C8A H8C 0.98 . ? C5 H5D 0.98 . ? C5 H5E 0.98 . ? C5 H5F 0.98 . ? C6 H6D 0.98 . ? C6 H6E 0.98 . ? C6 H6F 0.98 . ? C7 O1 1.492(12) . ? C7 H7C 0.99 . ? C7 H7D 0.99 . ? O1 C8 1.44(2) . ? C8 H8D 0.98 . ? C8 H8E 0.98 . ? C8 H8F 0.98 . ? B H1B1 1 . ? C1B C2B 1.252(19) . ? C1B C2B 1.352(19) 6_664 ? C1B H1B 0.95 . ? C2B H2B 0.95 . ? 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 O1 85.8(5) 9 . ? O1 Mg O1 85.8(5) 9 5 ? O1 Mg O1 85.8(5) . 5 ? O1 Mg N2 138.3(4) 9 . ? O1 Mg N2 76.7(4) . . ? O1 Mg N2 129.2(4) 5 . ? O1 Mg N2 129.2(4) 9 5 ? O1 Mg N2 138.3(4) . 5 ? O1 Mg N2 76.7(4) 5 5 ? N2 Mg N2 85.6(2) . 5 ? O1 Mg N2 76.7(4) 9 9 ? O1 Mg N2 129.2(4) . 9 ? O1 Mg N2 138.3(4) 5 9 ? N2 Mg N2 85.6(2) . 9 ? N2 Mg N2 85.6(2) 5 9 ? O1 Mg O1A 71.6(3) 9 5 ? O1 Mg O1A 95.5(3) . 5 ? O1 Mg O1A 17.9(3) 5 5 ? N2 Mg O1A 146.7(3) . 5 ? N2 Mg O1A 79.1(3) 5 5 ? N2 Mg O1A 122.0(4) 9 5 ? O1 Mg O1A 95.5(3) 9 . ? O1 Mg O1A 17.9(3) . . ? O1 Mg O1A 71.6(3) 5 . ? N2 Mg O1A 79.1(3) . . ? N2 Mg O1A 122.0(4) 5 . ? N2 Mg O1A 146.7(3) 9 . ? O1A Mg O1A 84.3(5) 5 . ? O1 Mg O1A 17.9(3) 9 9 ? O1 Mg O1A 71.6(3) . 9 ? O1 Mg O1A 95.5(3) 5 9 ? N2 Mg O1A 122.0(4) . 9 ? N2 Mg O1A 146.7(3) 5 9 ? N2 Mg O1A 79.1(3) 9 9 ? O1A Mg O1A 84.3(5) 5 9 ? O1A Mg O1A 84.3(5) . 9 ? C3 N1 N2 108.7(6) . . ? C3 N1 B 129.4(7) . . ? N2 N1 B 121.9(6) . . ? C1 N2 N1 107.1(5) . . ? C1 N2 Mg 136.4(5) . . ? N1 N2 Mg 116.3(4) . . ? N2 C1 C2 109.6(7) . . ? N2 C1 C4 121.5(6) . . ? C2 C1 C4 128.9(6) . . ? C3 C2 C1 105.8(6) . . ? C3 C2 H2 127.1 . . ? C1 C2 H2 127.1 . . ? N1 C3 C2 108.9(7) . . ? N1 C3 H3 125.6 . . ? C2 C3 H3 125.6 . . ? C7A C4 C1 112.6(9) . . ? C1 C4 C6 116.5(13) . . ? C7A C4 C5A 114.9(10) . . ? C1 C4 C5A 113.1(10) . . ? C1 C4 C7 110.2(6) . . ? C6 C4 C7 110.1(10) . . ? C1 C4 C5 106.0(12) . . ? C6 C4 C5 109.2(10) . . ? C7 C4 C5 104.0(9) . . ? C7A C4 C6A 105.8(9) . . ? C1 C4 C6A 102.9(9) . . ? C5A C4 C6A 106.1(9) . . ? C4 C5A H5A 109.4 . . ? C4 C5A H5B 109.5 . . ? H5A C5A H5B 109.5 . . ? C4 C5A H5C 109.5 . . ? H5A C5A H5C 109.5 . . ? H5B C5A H5C 109.5 . . ? C4 C6A H6A 109.5 . . ? C4 C6A H6B 109.5 . . ? H6A C6A H6B 109.5 . . ? C4 C6A H6C 109.5 . . ? H6A C6A H6C 109.5 . . ? H6B C6A H6C 109.5 . . ? C4 C7A O1A 118.5(15) . . ? C4 C7A H7A 107.7 . . ? O1A C7A H7A 107.8 . . ? C4 C7A H7B 107.6 . . ? O1A C7A H7B 107.6 . . ? H7A C7A H7B 107.1 . . ? C8A O1A C7A 110.0(15) . . ? C8A O1A Mg 135.4(12) . . ? C7A O1A Mg 114.0(11) . . ? O1A C8A H8A 109.5 . . ? O1A C8A H8B 109.5 . . ? H8A C8A H8B 109.5 . . ? O1A C8A H8C 109.5 . . ? H8A C8A H8C 109.5 . . ? H8B C8A H8C 109.5 . . ? C4 C5 H5D 109.5 . . ? C4 C5 H5E 109.4 . . ? H5D C5 H5E 109.5 . . ? C4 C5 H5F 109.5 . . ? H5D C5 H5F 109.5 . . ? H5E C5 H5F 109.5 . . ? C4 C6 H6D 109.5 . . ? C4 C6 H6E 109.4 . . ? H6D C6 H6E 109.5 . . ? C4 C6 H6F 109.5 . . ? H6D C6 H6F 109.5 . . ? H6E C6 H6F 109.5 . . ? O1 C7 C4 104.1(9) . . ? O1 C7 H7C 110.9 . . ? C4 C7 H7C 110.9 . . ? O1 C7 H7D 110.9 . . ? C4 C7 H7D 111 . . ? H7C C7 H7D 109 . . ? C8 O1 C7 115.3(13) . . ? C8 O1 Mg 127.2(12) . . ? C7 O1 Mg 117.0(8) . . ? O1 C8 H8D 109.5 . . ? O1 C8 H8E 109.5 . . ? H8D C8 H8E 109.5 . . ? O1 C8 H8F 109.4 . . ? H8D C8 H8F 109.5 . . ? H8E C8 H8F 109.5 . . ? N1 B N1 108.9(4) . 9 ? N1 B N1 108.9(4) . 5 ? N1 B N1 108.9(4) 9 5 ? N1 B H1B1 110 . . ? N1 B H1B1 110 9 . ? N1 B H1B1 110 5 . ? C2B C1B C2B 122(2) . 6_664 ? C2B C1B H1B 119 . . ? C2B C1B H1B 119 6_664 . ? C1B C2B C1B 117(2) . 12_566 ? C1B C2B H2B 121.6 . . ? C1B C2B H2B 121.6 12_566 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 N1 N2 C1 -0.1(8) . . . . ? B N1 N2 C1 -180.0(5) . . . . ? C3 N1 N2 Mg 175.8(5) . . . . ? B N1 N2 Mg -4.0(7) . . . . ? O1 Mg N2 C1 69.2(10) 9 . . . ? O1 Mg N2 C1 1.4(8) . . . . ? O1 Mg N2 C1 -71.8(9) 5 . . . ? N2 Mg N2 C1 -140.6(8) 5 . . . ? N2 Mg N2 C1 133.5(8) 9 . . . ? O1A Mg N2 C1 -78.2(11) 5 . . . ? O1A Mg N2 C1 -16.8(8) . . . . ? O1A Mg N2 C1 59.3(8) 9 . . . ? O1 Mg N2 N1 -105.2(7) 9 . . . ? O1 Mg N2 N1 -173.0(6) . . . . ? O1 Mg N2 N1 113.8(6) 5 . . . ? N2 Mg N2 N1 45.0(4) 5 . . . ? N2 Mg N2 N1 -40.9(4) 9 . . . ? O1A Mg N2 N1 107.4(8) 5 . . . ? O1A Mg N2 N1 168.8(5) . . . . ? O1A Mg N2 N1 -115.1(5) 9 . . . ? N1 N2 C1 C2 -0.5(8) . . . . ? Mg N2 C1 C2 -175.2(6) . . . . ? N1 N2 C1 C4 -176.8(6) . . . . ? Mg N2 C1 C4 8.5(12) . . . . ? N2 C1 C2 C3 0.9(10) . . . . ? C4 C1 C2 C3 176.9(8) . . . . ? N2 N1 C3 C2 0.7(9) . . . . ? B N1 C3 C2 -179.5(6) . . . . ? C1 C2 C3 N1 -0.9(10) . . . . ? N2 C1 C4 C7A -21.7(12) . . . . ? C2 C1 C4 C7A 162.7(11) . . . . ? N2 C1 C4 C6 -102.8(12) . . . . ? C2 C1 C4 C6 81.6(13) . . . . ? N2 C1 C4 C5A 110.7(11) . . . . ? C2 C1 C4 C5A -64.9(13) . . . . ? N2 C1 C4 C7 23.5(10) . . . . ? C2 C1 C4 C7 -152.1(9) . . . . ? N2 C1 C4 C5 135.5(10) . . . . ? C2 C1 C4 C5 -40.1(13) . . . . ? N2 C1 C4 C6A -135.2(9) . . . . ? C2 C1 C4 C6A 49.2(11) . . . . ? C1 C4 C7A O1A 60.6(18) . . . . ? C6 C4 C7A O1A 173(2) . . . . ? C5A C4 C7A O1A -71(2) . . . . ? C7 C4 C7A O1A -34.8(11) . . . . ? C5 C4 C7A O1A -87(2) . . . . ? C6A C4 C7A O1A 172.3(15) . . . . ? C4 C7A O1A C8A 109.5(18) . . . . ? C4 C7A O1A Mg -78.2(18) . . . . ? O1 Mg O1A C8A 74.6(19) 9 . . . ? O1 Mg O1A C8A 132(3) . . . . ? O1 Mg O1A C8A -9.1(17) 5 . . . ? N2 Mg O1A C8A -147.2(19) . . . . ? N2 Mg O1A C8A -69.5(19) 5 . . . ? N2 Mg O1A C8A 148.6(16) 9 . . . ? O1A Mg O1A C8A 3.8(19) 5 . . . ? O1A Mg O1A C8A 88.6(17) 9 . . . ? O1 Mg O1A C7A -95.0(13) 9 . . . ? O1 Mg O1A C7A -37.3(16) . . . . ? O1 Mg O1A C7A -178.7(16) 5 . . . ? N2 Mg O1A C7A 43.2(12) . . . . ? N2 Mg O1A C7A 120.9(11) 5 . . . ? N2 Mg O1A C7A -20.9(16) 9 . . . ? O1A Mg O1A C7A -165.8(12) 5 . . . ? O1A Mg O1A C7A -81.0(15) 9 . . . ? C7A C4 C7 O1 33.7(13) . . . . ? C1 C4 C7 O1 -68.1(9) . . . . ? C6 C4 C7 O1 61.7(15) . . . . ? C5A C4 C7 O1 -179.2(11) . . . . ? C5 C4 C7 O1 178.6(12) . . . . ? C6A C4 C7 O1 77.8(15) . . . . ? C4 C7 O1 C8 -97.7(15) . . . . ? C4 C7 O1 Mg 89.6(10) . . . . ? O1 Mg O1 C8 -1.9(16) 9 . . . ? O1 Mg O1 C8 -88.0(14) 5 . . . ? N2 Mg O1 C8 140.0(17) . . . . ? N2 Mg O1 C8 -152.6(14) 5 . . . ? N2 Mg O1 C8 67.2(17) 9 . . . ? O1A Mg O1 C8 -72.9(16) 5 . . . ? O1A Mg O1 C8 -124(3) . . . . ? O1A Mg O1 C8 9.2(14) 9 . . . ? O1 Mg O1 C7 169.9(11) 9 . . . ? O1 Mg O1 C7 83.8(14) 5 . . . ? N2 Mg O1 C7 -48.2(9) . . . . ? N2 Mg O1 C7 19.2(14) 5 . . . ? N2 Mg O1 C7 -121.0(9) 9 . . . ? O1A Mg O1 C7 98.9(11) 5 . . . ? O1A Mg O1 C7 47.4(15) . . . . ? O1A Mg O1 C7 -179.0(14) 9 . . . ? C3 N1 B N1 -117.9(9) . . . 9 ? N2 N1 B N1 61.9(7) . . . 9 ? C3 N1 B N1 123.5(9) . . . 5 ? N2 N1 B N1 -56.7(7) . . . 5 ? C2B C1B C2B C1B 15(3) 6_664 . . 12_566 ? # SQUEEZE RESULTS #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 #1 -0.137 0.137 0.637 132.4 27.0 #2 0.137 0.637 0.863 132.3 27.4 #3 0.363 0.363 0.363 132.4 27.1 #4 0.637 0.863 0.137 132.3 27.1 #_platon_squeeze_details #; #; #END OF CIF #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2008-05-29 at 15:34:31 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : shelxl dreduc import struct data_Chisholm1463 _database_code_depnum_ccdc_archive 'CCDC 695434' _audit_creation_date 2008-05-29T15:34:31-00:00 _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_name_common 'Chisholm 1463' _chemical_formula_moiety 'C28 H48 B1 I1 N6 O4 Sr1' _chemical_formula_sum 'C28 H48 B I N6 O4 Sr' _chemical_formula_weight 758.05 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 11.6346(10) _cell_length_b 18.6487(10) _cell_length_c 15.6835(10) _cell_angle_alpha 90 _cell_angle_beta 93.152(3) _cell_angle_gamma 90 _cell_volume 3397.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8040 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description 'rectangular tablet' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_special_details ;Examination of the diffraction pattern on a Nonius Kappa CCD diffractometer indicated a monoclinic crystal system. All work was done at 150K using an Oxford Cryosystems Cryostream Cooler. The data collection strategy was set up to measure a quadrant of reciprocal space with a redundancy factor of 4.8, which means that 90% of the reflections were measured at least 4.8 times. Omega scans with a frame width of 1.0 degree were used for data collection. Data integration was done with Denzo and scaling and merging of the data was done with Scalepack. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.535 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.615 _exptl_absorpt_correction_T_max 0.684 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor, 1997)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.447137E-1 _diffrn_orient_matrix_ub_12 -0.331767E-1 _diffrn_orient_matrix_ub_13 -0.357566E-1 _diffrn_orient_matrix_ub_21 0.343732E-1 _diffrn_orient_matrix_ub_22 0.42124E-1 _diffrn_orient_matrix_ub_23 -0.287377E-1 _diffrn_orient_matrix_ub_31 0.650313E-1 _diffrn_orient_matrix_ub_32 0.5462E-3 _diffrn_orient_matrix_ub_33 0.444234E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'omega scans' _diffrn_reflns_av_R_equivalents 0.051 _diffrn_reflns_av_unetI/netI ? _diffrn_reflns_number 80681 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 7792 _reflns_number_gt 6292 _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 ;There is a disordered THF ligand coordinated to the Sr atom. The disorder consists of one carbon atom of this THF occupying two positions: C(27A) and C(27B). DFIX restraints were used in the refinements for the bond lengths involving this disordered carbon atom. The occupancy factors for these two atoms refined to 0.63(1) and 0.37(1) for C(27A) and C(27B), respectively. For the methyl groups, the hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5 *Ueq(bonded carbon atom). The torsion angle, which defines the orientation of the methyl group about the C-C or O-C bond, was refined. The remaining hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(attached atom). Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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 'w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+0.6984P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7792 _refine_ls_number_parameters 389 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0572 _refine_ls_wR_factor_gt 0.0538 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.462 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.073 #----------------------------------------------------------------------------# # 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' Sr Sr -1.5307 3.2498 '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 I I 0.810940(11) 0.395276(7) 0.370947(9) 0.02451(5) Uani 1 1 d . . . Sr Sr 1.058326(15) 0.309821(10) 0.327007(11) 0.01523(5) Uani 1 1 d . . . O1 O 1.01054(12) 0.38994(7) 0.19087(9) 0.0228(3) Uani 1 1 d . . . O2 O 1.05627(13) 0.29524(7) 0.49333(9) 0.0252(3) Uani 1 1 d . . . O3 O 1.15306(12) 0.43150(7) 0.36333(9) 0.0254(3) Uani 1 1 d . . . N1 N 1.18872(14) 0.19187(8) 0.18678(10) 0.0167(4) Uani 1 1 d . . . N2 N 1.10754(13) 0.24550(9) 0.18426(10) 0.0174(4) Uani 1 1 d . . . N3 N 1.20254(14) 0.14315(8) 0.34182(10) 0.0182(4) Uani 1 1 d . . . N4 N 1.12687(14) 0.18225(9) 0.38714(10) 0.0180(4) Uani 1 1 d . . . N5 N 1.33828(13) 0.23947(8) 0.29485(10) 0.0164(4) Uani 1 1 d . . . N6 N 1.29175(14) 0.30441(8) 0.31603(10) 0.0173(4) Uani 1 1 d . . . C1 C 1.07192(16) 0.25226(10) 0.10207(12) 0.0187(4) Uani 1 1 d . . . C2 C 1.12994(18) 0.20381(11) 0.05118(13) 0.0242(5) Uani 1 1 d . . . H2 H 1.1209 0.1978 -0.009 0.029 Uiso 1 1 calc R . . C3 C 1.20231(17) 0.16729(11) 0.10718(13) 0.0216(5) Uani 1 1 d . . . H3 H 1.254 0.1304 0.0924 0.026 Uiso 1 1 calc R . . C4 C 0.98123(18) 0.30566(11) 0.07018(13) 0.0216(5) Uani 1 1 d . . . C5 C 0.88178(18) 0.26464(12) 0.02272(14) 0.0294(5) Uani 1 1 d . . . H5A H 0.8471 0.2313 0.0622 0.044 Uiso 1 1 calc R . . H5B H 0.9117 0.2377 -0.0249 0.044 Uiso 1 1 calc R . . H5C H 0.8235 0.2988 0.0007 0.044 Uiso 1 1 calc R . . C6 C 1.0347(2) 0.35856(12) 0.00864(14) 0.0328(6) Uani 1 1 d . . . H6A H 0.9752 0.3914 -0.0147 0.049 Uiso 1 1 calc R . . H6B H 1.0676 0.332 -0.0381 0.049 Uiso 1 1 calc R . . H6C H 1.0955 0.3861 0.0395 0.049 Uiso 1 1 calc R . . C7 C 0.92819(17) 0.34611(11) 0.14234(13) 0.0218(5) Uani 1 1 d . . . H7A H 0.8654 0.3771 0.1182 0.026 Uiso 1 1 calc R . . H7B H 0.8939 0.3112 0.1812 0.026 Uiso 1 1 calc R . . C8 C 0.9844(2) 0.46504(11) 0.18548(14) 0.0300(5) Uani 1 1 d . . . H8A H 0.9828 0.4803 0.1256 0.045 Uiso 1 1 calc R . . H8B H 1.0435 0.4922 0.2186 0.045 Uiso 1 1 calc R . . H8C H 0.9091 0.4739 0.2085 0.045 Uiso 1 1 calc R . . C9 C 1.10308(18) 0.14232(11) 0.45499(13) 0.0213(5) Uani 1 1 d . . . C10 C 1.1643(2) 0.07714(12) 0.45371(14) 0.0295(5) Uani 1 1 d . . . H10 H 1.1635 0.0392 0.4941 0.035 Uiso 1 1 calc R . . C11 C 1.22504(19) 0.08028(11) 0.38191(14) 0.0255(5) Uani 1 1 d . . . H11 H 1.2752 0.044 0.3631 0.031 Uiso 1 1 calc R . . C12 C 1.02551(18) 0.16695(12) 0.52319(13) 0.0255(5) Uani 1 1 d . . . C13 C 0.9248(2) 0.11424(14) 0.53023(19) 0.0488(7) Uani 1 1 d . . . H13A H 0.8806 0.1117 0.4753 0.073 Uiso 1 1 calc R . . H13B H 0.8747 0.1309 0.5744 0.073 Uiso 1 1 calc R . . H13C H 0.9549 0.0666 0.5455 0.073 Uiso 1 1 calc R . . C14 C 1.0946(2) 0.16969(14) 0.60935(14) 0.0391(6) Uani 1 1 d . . . H14A H 1.125 0.1219 0.6235 0.059 Uiso 1 1 calc R . . H14B H 1.0444 0.1854 0.6539 0.059 Uiso 1 1 calc R . . H14C H 1.1586 0.2035 0.6057 0.059 Uiso 1 1 calc R . . C15 C 0.97169(19) 0.23960(12) 0.50214(14) 0.0285(5) Uani 1 1 d . . . H15A H 0.9237 0.2357 0.4482 0.034 Uiso 1 1 calc R . . H15B H 0.9206 0.2531 0.5479 0.034 Uiso 1 1 calc R . . C16 C 1.0577(2) 0.34778(13) 0.55879(15) 0.0442(7) Uani 1 1 d . . . H16A H 0.9848 0.3742 0.5556 0.066 Uiso 1 1 calc R . . H16B H 1.1214 0.3812 0.5514 0.066 Uiso 1 1 calc R . . H16C H 1.068 0.3243 0.6146 0.066 Uiso 1 1 calc R . . C17 C 1.38189(17) 0.34817(10) 0.33218(12) 0.0182(4) Uani 1 1 d . . . C18 C 1.48545(17) 0.31218(11) 0.32246(13) 0.0208(5) Uani 1 1 d . . . H18 H 1.5612 0.3309 0.3305 0.025 Uiso 1 1 calc R . . C19 C 1.45407(17) 0.24419(11) 0.29885(12) 0.0210(5) Uani 1 1 d . . . H19 H 1.5055 0.2063 0.2871 0.025 Uiso 1 1 calc R . . C20 C 1.36608(18) 0.42630(11) 0.35681(14) 0.0241(5) Uani 1 1 d . . . C21 C 1.4606(2) 0.47162(14) 0.3175(2) 0.0560(8) Uani 1 1 d . . . H21A H 1.5364 0.4538 0.3378 0.084 Uiso 1 1 calc R . . H21B H 1.4525 0.5218 0.3346 0.084 Uiso 1 1 calc R . . H21C H 1.4528 0.468 0.2551 0.084 Uiso 1 1 calc R . . C22 C 1.3753(2) 0.43407(13) 0.45372(16) 0.0427(7) Uani 1 1 d . . . H22A H 1.3152 0.4053 0.4787 0.064 Uiso 1 1 calc R . . H22B H 1.3655 0.4846 0.4691 0.064 Uiso 1 1 calc R . . H22C H 1.4511 0.4174 0.4757 0.064 Uiso 1 1 calc R . . C23 C 1.25233(18) 0.45520(12) 0.31857(14) 0.0275(5) Uani 1 1 d . . . H23A H 1.255 0.5083 0.3193 0.033 Uiso 1 1 calc R . . H23B H 1.2428 0.4397 0.2582 0.033 Uiso 1 1 calc R . . C24 C 1.1022(2) 0.48864(12) 0.40852(15) 0.0324(6) Uani 1 1 d . . . H24A H 1.1556 0.5046 0.4552 0.049 Uiso 1 1 calc R . . H24B H 1.0306 0.4719 0.432 0.049 Uiso 1 1 calc R . . H24C H 1.0853 0.5287 0.3694 0.049 Uiso 1 1 calc R . . B B 1.2673(2) 0.17343(13) 0.26635(15) 0.0197(5) Uani 1 1 d . . . H1B H 1.3226 0.1357 0.2491 0.024 Uiso 1 1 calc R . . O4 O 0.88411(12) 0.20280(7) 0.28922(10) 0.0267(4) Uani 1 1 d . A . C25 C 0.76124(19) 0.20213(12) 0.29668(17) 0.0335(6) Uani 1 1 d . A . H25A H 0.7225 0.2297 0.2494 0.04 Uiso 1 1 calc R . . H25B H 0.7413 0.2239 0.3515 0.04 Uiso 1 1 calc R . . C26 C 0.7238(2) 0.12436(13) 0.29276(19) 0.0412(7) Uani 1 1 d D . . H26A H 0.6664 0.1166 0.2447 0.049 Uiso 0.630(11) 1 calc PR A 1 H26B H 0.6892 0.1102 0.3465 0.049 Uiso 0.630(11) 1 calc PR A 1 H26C H 0.6423 0.1194 0.272 0.049 Uiso 0.370(11) 1 calc PR A 2 H26D H 0.7357 0.1003 0.3488 0.049 Uiso 0.370(11) 1 calc PR A 2 C27A C 0.8325(4) 0.0810(2) 0.2798(5) 0.0369(15) Uani 0.630(11) 1 d PD A 1 H27A H 0.8621 0.0587 0.3339 0.044 Uiso 0.630(11) 1 calc PR A 1 H27B H 0.818 0.043 0.2364 0.044 Uiso 0.630(11) 1 calc PR A 1 C27B C 0.8073(6) 0.0954(5) 0.2268(8) 0.044(3) Uani 0.370(11) 1 d PD A 2 H27C H 0.8194 0.0431 0.2334 0.053 Uiso 0.370(11) 1 calc PR A 2 H27D H 0.7783 0.1058 0.1676 0.053 Uiso 0.370(11) 1 calc PR A 2 C28 C 0.9146(2) 0.13607(12) 0.24956(16) 0.0343(6) Uani 1 1 d D . . H28A H 0.9949 0.1227 0.2668 0.041 Uiso 0.630(11) 1 calc PR A 1 H28B H 0.9073 0.1404 0.1866 0.041 Uiso 0.630(11) 1 calc PR A 1 H28C H 0.9653 0.1076 0.2895 0.041 Uiso 0.370(11) 1 calc PR A 2 H28D H 0.9566 0.1458 0.1976 0.041 Uiso 0.370(11) 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 I 0.01640(8) 0.02501(8) 0.03256(9) -0.00352(6) 0.00532(6) 0.00084(6) Sr 0.01291(10) 0.01617(10) 0.01676(10) -0.00267(8) 0.00203(7) 0.00108(8) O1 0.0239(8) 0.0197(8) 0.0245(8) -0.0024(6) -0.0029(6) 0.0040(6) O2 0.0300(9) 0.0240(8) 0.0222(8) -0.0046(6) 0.0076(7) -0.0006(7) O3 0.0175(8) 0.0204(8) 0.0389(9) -0.0098(7) 0.0074(7) -0.0033(6) N1 0.0148(9) 0.0179(9) 0.0176(9) -0.0045(7) 0.0018(7) 0.0025(7) N2 0.0134(8) 0.0209(9) 0.0178(9) -0.0034(7) 0.0000(7) 0.0033(7) N3 0.0191(9) 0.0155(9) 0.0198(9) -0.0021(7) 0.0004(7) 0.0017(7) N4 0.0160(9) 0.0199(9) 0.0183(9) -0.0024(7) 0.0023(7) -0.0001(7) N5 0.0139(8) 0.0182(9) 0.0171(9) -0.0008(7) 0.0018(7) 0.0035(7) N6 0.0146(9) 0.0154(9) 0.0220(9) -0.0015(7) 0.0020(7) 0.0004(7) C1 0.0154(10) 0.0217(11) 0.0190(11) -0.0017(9) 0.0014(8) -0.0026(9) C2 0.0245(12) 0.0318(13) 0.0163(11) -0.0067(9) 0.0014(9) 0.0034(10) C3 0.0187(11) 0.0237(11) 0.0227(11) -0.0074(9) 0.0036(9) 0.0032(9) C4 0.0206(11) 0.0260(12) 0.0178(11) -0.0023(9) -0.0019(9) 0.0043(9) C5 0.0228(12) 0.0391(14) 0.0254(12) -0.0072(10) -0.0053(10) 0.0061(10) C6 0.0354(14) 0.0389(14) 0.0244(12) 0.0046(10) 0.0039(10) 0.0070(12) C7 0.0178(11) 0.0243(12) 0.0231(11) -0.0029(9) -0.0012(9) 0.0038(9) C8 0.0356(14) 0.0213(12) 0.0329(13) 0.0039(10) -0.0012(10) 0.0029(10) C9 0.0214(11) 0.0207(11) 0.0215(11) -0.0005(9) 0.0004(9) -0.0051(9) C10 0.0415(14) 0.0188(11) 0.0280(13) 0.0047(10) 0.0015(11) -0.0009(11) C11 0.0321(13) 0.0171(11) 0.0272(12) -0.0024(9) 0.0024(10) 0.0025(10) C12 0.0242(12) 0.0285(12) 0.0242(12) 0.0019(10) 0.0061(9) -0.0055(10) C13 0.0395(16) 0.0510(17) 0.0576(19) 0.0043(14) 0.0168(14) -0.0179(13) C14 0.0463(16) 0.0490(16) 0.0227(13) 0.0038(11) 0.0089(11) 0.0069(13) C15 0.0239(12) 0.0355(13) 0.0268(12) -0.0002(10) 0.0083(10) -0.0005(10) C16 0.069(2) 0.0343(15) 0.0307(14) -0.0123(11) 0.0115(13) -0.0060(14) C17 0.0158(10) 0.0212(11) 0.0174(10) 0.0039(9) 0.0003(8) -0.0025(9) C18 0.0128(10) 0.0295(12) 0.0201(11) 0.0012(9) -0.0004(8) -0.0035(9) C19 0.0131(10) 0.0294(12) 0.0205(11) -0.0014(9) 0.0023(8) 0.0034(9) C20 0.0168(11) 0.0197(11) 0.0357(13) 0.0007(10) -0.0002(9) -0.0041(9) C21 0.0298(15) 0.0322(15) 0.107(3) 0.0111(16) 0.0164(15) -0.0083(12) C22 0.0439(16) 0.0354(15) 0.0466(16) -0.0154(12) -0.0176(13) 0.0065(12) C23 0.0271(12) 0.0219(11) 0.0339(13) 0.0024(10) 0.0055(10) -0.0019(10) C24 0.0279(13) 0.0270(12) 0.0433(15) -0.0155(11) 0.0108(11) -0.0022(10) B 0.0182(12) 0.0201(12) 0.0211(12) -0.0038(10) 0.0033(10) 0.0050(10) O4 0.0167(8) 0.0239(8) 0.0399(9) -0.0088(7) 0.0042(7) -0.0011(6) C25 0.0172(12) 0.0303(13) 0.0530(16) -0.0037(11) 0.0011(11) 0.0003(10) C26 0.0222(13) 0.0311(14) 0.071(2) -0.0086(13) 0.0092(12) -0.0035(11) C27A 0.026(2) 0.028(2) 0.057(4) -0.008(2) 0.003(2) -0.0002(18) C27B 0.020(4) 0.028(5) 0.084(8) -0.021(5) 0.000(4) 0.001(3) C28 0.0286(13) 0.0272(13) 0.0481(16) -0.0147(11) 0.0099(11) -0.0038(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 I Sr 3.3937(3) . ? Sr O3 2.5729(13) . ? Sr O2 2.6242(14) . ? Sr N2 2.6305(16) . ? Sr O1 2.6400(14) . ? Sr N4 2.6651(16) . ? Sr N6 2.7326(16) . ? Sr O4 2.8829(14) . ? Sr C15 3.253(2) . ? Sr C7 3.264(2) . ? O1 C8 1.435(2) . ? O1 C7 1.444(2) . ? O2 C16 1.419(3) . ? O2 C15 1.442(3) . ? O3 C24 1.426(2) . ? O3 C23 1.453(3) . ? N1 C3 1.347(2) . ? N1 N2 1.375(2) . ? N1 B 1.545(3) . ? N2 C1 1.338(2) . ? N3 C11 1.349(3) . ? N3 N4 1.371(2) . ? N3 B 1.545(3) . ? N4 C9 1.340(3) . ? N5 C19 1.348(2) . ? N5 N6 1.375(2) . ? N5 B 1.535(3) . ? N6 C17 1.342(2) . ? C1 C2 1.403(3) . ? C1 C4 1.516(3) . ? C2 C3 1.365(3) . ? C2 H2 0.95 . ? C3 H3 0.95 . ? C4 C7 1.519(3) . ? C4 C6 1.536(3) . ? C4 C5 1.544(3) . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 C10 1.410(3) . ? C9 C12 1.509(3) . ? C10 C11 1.363(3) . ? C10 H10 0.95 . ? C11 H11 0.95 . ? C12 C15 1.521(3) . ? C12 C14 1.535(3) . ? C12 C13 1.538(3) . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 C18 1.395(3) . ? C17 C20 1.521(3) . ? C18 C19 1.365(3) . ? C18 H18 0.95 . ? C19 H19 0.95 . ? C20 C23 1.521(3) . ? C20 C22 1.525(3) . ? C20 C21 1.542(3) . ? 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 0.99 . ? C23 H23B 0.99 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? B H1B 1 . ? O4 C25 1.441(3) . ? O4 C28 1.444(2) . ? C25 C26 1.515(3) . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? C26 C27A 1.524(4) . ? C26 C27B 1.554(6) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? C26 H26C 0.99 . ? C26 H26D 0.99 . ? C27A C28 1.498(4) . ? C27A H27A 0.99 . ? C27A H27B 0.99 . ? C27B C28 1.487(6) . ? C27B H27C 0.99 . ? C27B H27D 0.99 . ? C28 H28A 0.99 . ? C28 H28B 0.99 . ? C28 H28C 0.99 . ? C28 H28D 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 O3 Sr O2 84.18(5) . . ? O3 Sr N2 118.68(5) . . ? O2 Sr N2 144.40(5) . . ? O3 Sr O1 75.43(4) . . ? O2 Sr O1 148.17(4) . . ? N2 Sr O1 67.40(5) . . ? O3 Sr N4 126.35(5) . . ? O2 Sr N4 64.83(5) . . ? N2 Sr N4 79.59(5) . . ? O1 Sr N4 146.83(5) . . ? O3 Sr N6 68.37(4) . . ? O2 Sr N6 97.02(5) . . ? N2 Sr N6 70.48(5) . . ? O1 Sr N6 97.80(5) . . ? N4 Sr N6 73.15(5) . . ? O3 Sr O4 160.72(4) . . ? O2 Sr O4 95.04(4) . . ? N2 Sr O4 72.11(5) . . ? O1 Sr O4 96.38(4) . . ? N4 Sr O4 69.40(4) . . ? N6 Sr O4 130.65(4) . . ? O3 Sr C15 108.48(5) . . ? O2 Sr C15 25.66(5) . . ? N2 Sr C15 128.84(5) . . ? O1 Sr C15 148.16(5) . . ? N4 Sr C15 56.11(5) . . ? N6 Sr C15 113.18(5) . . ? O4 Sr C15 69.38(5) . . ? O3 Sr C7 100.71(5) . . ? O2 Sr C7 150.96(5) . . ? N2 Sr C7 56.73(5) . . ? O1 Sr C7 25.63(5) . . ? N4 Sr C7 127.89(5) . . ? N6 Sr C7 111.46(5) . . ? O4 Sr C7 71.01(5) . . ? C15 Sr C7 133.04(5) . . ? O3 Sr I 84.18(3) . . ? O2 Sr I 78.03(3) . . ? N2 Sr I 127.85(3) . . ? O1 Sr I 75.83(3) . . ? N4 Sr I 126.01(4) . . ? N6 Sr I 152.51(3) . . ? O4 Sr I 76.84(3) . . ? C15 Sr I 73.26(4) . . ? C7 Sr I 74.08(4) . . ? C8 O1 C7 112.92(15) . . ? C8 O1 Sr 129.39(12) . . ? C7 O1 Sr 102.12(11) . . ? C16 O2 C15 114.14(17) . . ? C16 O2 Sr 130.34(13) . . ? C15 O2 Sr 102.32(11) . . ? C24 O3 C23 112.07(16) . . ? C24 O3 Sr 125.76(12) . . ? C23 O3 Sr 120.23(12) . . ? C3 N1 N2 109.65(15) . . ? C3 N1 B 125.33(17) . . ? N2 N1 B 124.09(15) . . ? C1 N2 N1 105.79(15) . . ? C1 N2 Sr 134.96(13) . . ? N1 N2 Sr 119.25(11) . . ? C11 N3 N4 109.52(16) . . ? C11 N3 B 125.75(17) . . ? N4 N3 B 123.85(16) . . ? C9 N4 N3 106.42(16) . . ? C9 N4 Sr 134.92(13) . . ? N3 N4 Sr 118.64(11) . . ? C19 N5 N6 109.69(16) . . ? C19 N5 B 125.86(17) . . ? N6 N5 B 124.36(15) . . ? C17 N6 N5 105.51(15) . . ? C17 N6 Sr 137.28(13) . . ? N5 N6 Sr 116.98(11) . . ? N2 C1 C2 110.74(18) . . ? N2 C1 C4 123.56(17) . . ? C2 C1 C4 125.70(18) . . ? C3 C2 C1 104.74(18) . . ? C3 C2 H2 127.6 . . ? C1 C2 H2 127.6 . . ? N1 C3 C2 109.08(18) . . ? N1 C3 H3 125.5 . . ? C2 C3 H3 125.5 . . ? C1 C4 C7 112.60(16) . . ? C1 C4 C6 109.31(17) . . ? C7 C4 C6 110.16(17) . . ? C1 C4 C5 108.85(17) . . ? C7 C4 C5 106.31(17) . . ? C6 C4 C5 109.53(17) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O1 C7 C4 112.88(16) . . ? O1 C7 Sr 52.25(9) . . ? C4 C7 Sr 111.75(12) . . ? O1 C7 H7A 109 . . ? C4 C7 H7A 109 . . ? Sr C7 H7A 139.2 . . ? O1 C7 H7B 109 . . ? C4 C7 H7B 109 . . ? Sr C7 H7B 60 . . ? H7A C7 H7B 107.8 . . ? O1 C8 H8A 109.5 . . ? O1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N4 C9 C10 109.95(19) . . ? N4 C9 C12 123.47(18) . . ? C10 C9 C12 126.53(19) . . ? C11 C10 C9 105.08(19) . . ? C11 C10 H10 127.5 . . ? C9 C10 H10 127.5 . . ? N3 C11 C10 109.03(19) . . ? N3 C11 H11 125.5 . . ? C10 C11 H11 125.5 . . ? C9 C12 C15 111.87(17) . . ? C9 C12 C14 109.23(18) . . ? C15 C12 C14 110.54(18) . . ? C9 C12 C13 110.13(19) . . ? C15 C12 C13 106.18(19) . . ? C14 C12 C13 108.8(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 C15 C12 112.75(17) . . ? O2 C15 Sr 52.02(9) . . ? C12 C15 Sr 113.51(13) . . ? O2 C15 H15A 109 . . ? C12 C15 H15A 109 . . ? Sr C15 H15A 59.6 . . ? O2 C15 H15B 109 . . ? C12 C15 H15B 109 . . ? Sr C15 H15B 137.4 . . ? H15A C15 H15B 107.8 . . ? O2 C16 H16A 109.5 . . ? O2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N6 C17 C18 110.95(17) . . ? N6 C17 C20 121.76(17) . . ? C18 C17 C20 127.30(18) . . ? C19 C18 C17 104.88(18) . . ? C19 C18 H18 127.6 . . ? C17 C18 H18 127.6 . . ? N5 C19 C18 108.97(18) . . ? N5 C19 H19 125.5 . . ? C18 C19 H19 125.5 . . ? C17 C20 C23 110.73(17) . . ? C17 C20 C22 109.96(18) . . ? C23 C20 C22 111.79(19) . . ? C17 C20 C21 108.95(19) . . ? C23 C20 C21 105.79(18) . . ? C22 C20 C21 109.5(2) . . ? 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 . . ? O3 C23 C20 113.53(17) . . ? O3 C23 H23A 108.9 . . ? C20 C23 H23A 108.9 . . ? O3 C23 H23B 108.9 . . ? C20 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? O3 C24 H24A 109.5 . . ? O3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N5 B N3 110.33(16) . . ? N5 B N1 109.97(16) . . ? N3 B N1 114.08(17) . . ? N5 B H1B 107.4 . . ? N3 B H1B 107.4 . . ? N1 B H1B 107.4 . . ? C25 O4 C28 107.22(16) . . ? C25 O4 Sr 132.75(12) . . ? C28 O4 Sr 119.89(12) . . ? O4 C25 C26 106.84(18) . . ? O4 C25 H25A 110.4 . . ? C26 C25 H25A 110.4 . . ? O4 C25 H25B 110.4 . . ? C26 C25 H25B 110.4 . . ? H25A C25 H25B 108.6 . . ? C25 C26 C27A 105.9(2) . . ? C25 C26 C27B 99.8(4) . . ? C25 C26 H26A 110.6 . . ? C27A C26 H26A 110.6 . . ? C25 C26 H26B 110.6 . . ? C27A C26 H26B 110.6 . . ? H26A C26 H26B 108.7 . . ? C25 C26 H26C 111.8 . . ? C27B C26 H26C 111.8 . . ? C25 C26 H26D 111.8 . . ? C27B C26 H26D 111.8 . . ? H26C C26 H26D 109.5 . . ? C28 C27A C26 103.1(3) . . ? C28 C27A H27A 111.1 . . ? C26 C27A H27A 111.1 . . ? C28 C27A H27B 111.1 . . ? C26 C27A H27B 111.1 . . ? H27A C27A H27B 109.1 . . ? C28 C27B C26 102.2(4) . . ? C28 C27B H27C 111.3 . . ? C26 C27B H27C 111.3 . . ? C28 C27B H27D 111.3 . . ? C26 C27B H27D 111.3 . . ? H27C C27B H27D 109.2 . . ? O4 C28 C27B 108.6(3) . . ? O4 C28 C27A 106.2(2) . . ? O4 C28 H28A 110.5 . . ? C27A C28 H28A 110.5 . . ? O4 C28 H28B 110.5 . . ? C27A C28 H28B 110.5 . . ? H28A C28 H28B 108.7 . . ? O4 C28 H28C 110 . . ? C27B C28 H28C 110 . . ? O4 C28 H28D 110 . . ? C27B C28 H28D 110 . . ? H28C C28 H28D 108.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Sr O1 C8 -36.45(16) . . . . ? O2 Sr O1 C8 15.4(2) . . . . ? N2 Sr O1 C8 -166.64(17) . . . . ? N4 Sr O1 C8 -172.66(15) . . . . ? N6 Sr O1 C8 -101.62(16) . . . . ? O4 Sr O1 C8 125.78(16) . . . . ? C15 Sr O1 C8 65.23(19) . . . . ? C7 Sr O1 C8 133.8(2) . . . . ? I Sr O1 C8 51.12(16) . . . . ? O3 Sr O1 C7 -170.22(11) . . . . ? O2 Sr O1 C7 -118.34(12) . . . . ? N2 Sr O1 C7 59.59(11) . . . . ? N4 Sr O1 C7 53.58(15) . . . . ? N6 Sr O1 C7 124.62(11) . . . . ? O4 Sr O1 C7 -7.99(11) . . . . ? C15 Sr O1 C7 -68.54(14) . . . . ? I Sr O1 C7 -82.65(11) . . . . ? O3 Sr O2 C16 24.18(19) . . . . ? N2 Sr O2 C16 157.51(18) . . . . ? O1 Sr O2 C16 -25.8(2) . . . . ? N4 Sr O2 C16 159.1(2) . . . . ? N6 Sr O2 C16 91.48(19) . . . . ? O4 Sr O2 C16 -136.47(19) . . . . ? C15 Sr O2 C16 -137.3(2) . . . . ? C7 Sr O2 C16 -77.4(2) . . . . ? I Sr O2 C16 -61.09(18) . . . . ? O3 Sr O2 C15 161.45(12) . . . . ? N2 Sr O2 C15 -65.21(14) . . . . ? O1 Sr O2 C15 111.51(13) . . . . ? N4 Sr O2 C15 -63.61(11) . . . . ? N6 Sr O2 C15 -131.24(11) . . . . ? O4 Sr O2 C15 0.81(12) . . . . ? C7 Sr O2 C15 59.86(16) . . . . ? I Sr O2 C15 76.19(11) . . . . ? O2 Sr O3 C24 -61.60(16) . . . . ? N2 Sr O3 C24 147.26(15) . . . . ? O1 Sr O3 C24 93.75(16) . . . . ? N4 Sr O3 C24 -114.30(16) . . . . ? N6 Sr O3 C24 -161.54(17) . . . . ? O4 Sr O3 C24 27.0(2) . . . . ? C15 Sr O3 C24 -53.25(17) . . . . ? C7 Sr O3 C24 89.46(16) . . . . ? I Sr O3 C24 16.91(15) . . . . ? O2 Sr O3 C23 135.57(14) . . . . ? N2 Sr O3 C23 -15.57(15) . . . . ? O1 Sr O3 C23 -69.08(13) . . . . ? N4 Sr O3 C23 82.87(14) . . . . ? N6 Sr O3 C23 35.63(13) . . . . ? O4 Sr O3 C23 -135.80(15) . . . . ? C15 Sr O3 C23 143.92(13) . . . . ? C7 Sr O3 C23 -73.37(14) . . . . ? I Sr O3 C23 -145.92(13) . . . . ? C3 N1 N2 C1 0.5(2) . . . . ? B N1 N2 C1 170.03(17) . . . . ? C3 N1 N2 Sr -178.84(12) . . . . ? B N1 N2 Sr -9.4(2) . . . . ? O3 Sr N2 C1 -80.48(19) . . . . ? O2 Sr N2 C1 155.08(16) . . . . ? O1 Sr N2 C1 -23.04(17) . . . . ? N4 Sr N2 C1 153.61(19) . . . . ? N6 Sr N2 C1 -130.71(19) . . . . ? O4 Sr N2 C1 82.07(18) . . . . ? C15 Sr N2 C1 124.77(18) . . . . ? C7 Sr N2 C1 3.45(17) . . . . ? I Sr N2 C1 25.7(2) . . . . ? O3 Sr N2 N1 98.68(13) . . . . ? O2 Sr N2 N1 -25.76(17) . . . . ? O1 Sr N2 N1 156.12(14) . . . . ? N4 Sr N2 N1 -27.23(13) . . . . ? N6 Sr N2 N1 48.45(12) . . . . ? O4 Sr N2 N1 -98.76(13) . . . . ? C15 Sr N2 N1 -56.07(15) . . . . ? C7 Sr N2 N1 -177.39(15) . . . . ? I Sr N2 N1 -155.13(11) . . . . ? C11 N3 N4 C9 -0.3(2) . . . . ? B N3 N4 C9 -170.16(17) . . . . ? C11 N3 N4 Sr -179.10(12) . . . . ? B N3 N4 Sr 11.1(2) . . . . ? O3 Sr N4 C9 90.03(18) . . . . ? O2 Sr N4 C9 29.06(17) . . . . ? N2 Sr N4 C9 -151.89(18) . . . . ? O1 Sr N4 C9 -146.24(16) . . . . ? N6 Sr N4 C9 135.52(18) . . . . ? O4 Sr N4 C9 -77.23(18) . . . . ? C15 Sr N4 C9 1.19(17) . . . . ? C7 Sr N4 C9 -120.08(17) . . . . ? I Sr N4 C9 -22.27(19) . . . . ? O3 Sr N4 N3 -91.63(13) . . . . ? O2 Sr N4 N3 -152.61(14) . . . . ? N2 Sr N4 N3 26.44(12) . . . . ? O1 Sr N4 N3 32.09(17) . . . . ? N6 Sr N4 N3 -46.15(12) . . . . ? O4 Sr N4 N3 101.10(13) . . . . ? C15 Sr N4 N3 179.53(15) . . . . ? C7 Sr N4 N3 58.26(14) . . . . ? I Sr N4 N3 156.07(10) . . . . ? C19 N5 N6 C17 0.4(2) . . . . ? B N5 N6 C17 -176.50(17) . . . . ? C19 N5 N6 Sr -175.05(12) . . . . ? B N5 N6 Sr 8.0(2) . . . . ? O3 Sr N6 C17 5.02(18) . . . . ? O2 Sr N6 C17 -75.85(19) . . . . ? N2 Sr N6 C17 138.51(19) . . . . ? O1 Sr N6 C17 75.90(19) . . . . ? N4 Sr N6 C17 -136.83(19) . . . . ? O4 Sr N6 C17 -178.70(17) . . . . ? C15 Sr N6 C17 -96.59(19) . . . . ? C7 Sr N6 C17 98.39(19) . . . . ? I Sr N6 C17 1.7(2) . . . . ? O3 Sr N6 N5 178.57(13) . . . . ? O2 Sr N6 N5 97.71(12) . . . . ? N2 Sr N6 N5 -47.93(12) . . . . ? O1 Sr N6 N5 -110.54(12) . . . . ? N4 Sr N6 N5 36.73(12) . . . . ? O4 Sr N6 N5 -5.15(15) . . . . ? C15 Sr N6 N5 76.96(13) . . . . ? C7 Sr N6 N5 -88.06(12) . . . . ? I Sr N6 N5 175.23(8) . . . . ? N1 N2 C1 C2 -0.4(2) . . . . ? Sr N2 C1 C2 178.81(14) . . . . ? N1 N2 C1 C4 179.72(17) . . . . ? Sr N2 C1 C4 -1.0(3) . . . . ? N2 C1 C2 C3 0.2(2) . . . . ? C4 C1 C2 C3 -179.99(19) . . . . ? N2 N1 C3 C2 -0.5(2) . . . . ? B N1 C3 C2 -169.78(18) . . . . ? C1 C2 C3 N1 0.2(2) . . . . ? N2 C1 C4 C7 -4.9(3) . . . . ? C2 C1 C4 C7 175.32(19) . . . . ? N2 C1 C4 C6 117.9(2) . . . . ? C2 C1 C4 C6 -61.9(3) . . . . ? N2 C1 C4 C5 -122.5(2) . . . . ? C2 C1 C4 C5 57.7(3) . . . . ? C8 O1 C7 C4 116.81(19) . . . . ? Sr O1 C7 C4 -100.48(16) . . . . ? C8 O1 C7 Sr -142.71(17) . . . . ? C1 C4 C7 O1 63.4(2) . . . . ? C6 C4 C7 O1 -58.9(2) . . . . ? C5 C4 C7 O1 -177.50(16) . . . . ? C1 C4 C7 Sr 6.6(2) . . . . ? C6 C4 C7 Sr -115.75(15) . . . . ? C5 C4 C7 Sr 125.66(14) . . . . ? O3 Sr C7 O1 9.63(11) . . . . ? O2 Sr C7 O1 106.97(13) . . . . ? N2 Sr C7 O1 -107.76(12) . . . . ? N4 Sr C7 O1 -146.09(10) . . . . ? N6 Sr C7 O1 -61.17(11) . . . . ? O4 Sr C7 O1 171.60(12) . . . . ? C15 Sr C7 O1 137.80(11) . . . . ? I Sr C7 O1 90.36(10) . . . . ? O3 Sr C7 C4 112.37(14) . . . . ? O2 Sr C7 C4 -150.29(12) . . . . ? N2 Sr C7 C4 -5.02(12) . . . . ? O1 Sr C7 C4 102.74(18) . . . . ? N4 Sr C7 C4 -43.35(16) . . . . ? N6 Sr C7 C4 41.57(15) . . . . ? O4 Sr C7 C4 -85.66(14) . . . . ? C15 Sr C7 C4 -119.46(14) . . . . ? I Sr C7 C4 -166.90(14) . . . . ? N3 N4 C9 C10 0.3(2) . . . . ? Sr N4 C9 C10 178.80(14) . . . . ? N3 N4 C9 C12 177.96(18) . . . . ? Sr N4 C9 C12 -3.6(3) . . . . ? N4 C9 C10 C11 -0.2(2) . . . . ? C12 C9 C10 C11 -177.7(2) . . . . ? N4 N3 C11 C10 0.2(2) . . . . ? B N3 C11 C10 169.80(19) . . . . ? C9 C10 C11 N3 0.0(2) . . . . ? N4 C9 C12 C15 4.1(3) . . . . ? C10 C9 C12 C15 -178.7(2) . . . . ? N4 C9 C12 C14 -118.7(2) . . . . ? C10 C9 C12 C14 58.6(3) . . . . ? N4 C9 C12 C13 121.9(2) . . . . ? C10 C9 C12 C13 -60.9(3) . . . . ? C16 O2 C15 C12 -111.7(2) . . . . ? Sr O2 C15 C12 102.78(16) . . . . ? C16 O2 C15 Sr 145.48(19) . . . . ? C9 C12 C15 O2 -59.8(2) . . . . ? C14 C12 C15 O2 62.2(2) . . . . ? C13 C12 C15 O2 -179.94(18) . . . . ? C9 C12 C15 Sr -2.8(2) . . . . ? C14 C12 C15 Sr 119.16(16) . . . . ? C13 C12 C15 Sr -122.99(16) . . . . ? O3 Sr C15 O2 -19.49(12) . . . . ? N2 Sr C15 O2 137.27(11) . . . . ? O1 Sr C15 O2 -111.53(12) . . . . ? N4 Sr C15 O2 102.41(12) . . . . ? N6 Sr C15 O2 54.27(12) . . . . ? O4 Sr C15 O2 -179.14(12) . . . . ? C7 Sr C15 O2 -144.95(10) . . . . ? I Sr C15 O2 -97.24(11) . . . . ? O3 Sr C15 C12 -120.76(14) . . . . ? O2 Sr C15 C12 -101.27(18) . . . . ? N2 Sr C15 C12 36.00(16) . . . . ? O1 Sr C15 C12 147.20(12) . . . . ? N4 Sr C15 C12 1.14(12) . . . . ? N6 Sr C15 C12 -47.00(15) . . . . ? O4 Sr C15 C12 79.59(14) . . . . ? C7 Sr C15 C12 113.78(14) . . . . ? I Sr C15 C12 161.49(15) . . . . ? N5 N6 C17 C18 -0.5(2) . . . . ? Sr N6 C17 C18 173.50(13) . . . . ? N5 N6 C17 C20 179.02(17) . . . . ? Sr N6 C17 C20 -6.9(3) . . . . ? N6 C17 C18 C19 0.5(2) . . . . ? C20 C17 C18 C19 -179.07(19) . . . . ? N6 N5 C19 C18 -0.1(2) . . . . ? B N5 C19 C18 176.72(17) . . . . ? C17 C18 C19 N5 -0.2(2) . . . . ? N6 C17 C20 C23 -28.5(3) . . . . ? C18 C17 C20 C23 151.0(2) . . . . ? N6 C17 C20 C22 95.6(2) . . . . ? C18 C17 C20 C22 -84.9(3) . . . . ? N6 C17 C20 C21 -144.4(2) . . . . ? C18 C17 C20 C21 35.1(3) . . . . ? C24 O3 C23 C20 110.3(2) . . . . ? Sr O3 C23 C20 -84.69(19) . . . . ? C17 C20 C23 O3 76.6(2) . . . . ? C22 C20 C23 O3 -46.4(2) . . . . ? C21 C20 C23 O3 -165.55(19) . . . . ? C19 N5 B N3 114.4(2) . . . . ? N6 N5 B N3 -69.2(2) . . . . ? C19 N5 B N1 -118.9(2) . . . . ? N6 N5 B N1 57.5(2) . . . . ? C11 N3 B N5 -110.9(2) . . . . ? N4 N3 B N5 57.3(2) . . . . ? C11 N3 B N1 124.8(2) . . . . ? N4 N3 B N1 -67.1(2) . . . . ? C3 N1 B N5 109.5(2) . . . . ? N2 N1 B N5 -58.3(2) . . . . ? C3 N1 B N3 -125.9(2) . . . . ? N2 N1 B N3 66.3(2) . . . . ? O3 Sr O4 C25 -13.0(3) . . . . ? O2 Sr O4 C25 73.75(19) . . . . ? N2 Sr O4 C25 -140.23(19) . . . . ? O1 Sr O4 C25 -76.48(19) . . . . ? N4 Sr O4 C25 134.45(19) . . . . ? N6 Sr O4 C25 177.49(17) . . . . ? C15 Sr O4 C25 74.13(19) . . . . ? C7 Sr O4 C25 -80.13(19) . . . . ? I Sr O4 C25 -2.69(18) . . . . ? O3 Sr O4 C28 162.12(16) . . . . ? O2 Sr O4 C28 -111.10(15) . . . . ? N2 Sr O4 C28 34.92(15) . . . . ? O1 Sr O4 C28 98.66(15) . . . . ? N4 Sr O4 C28 -50.40(15) . . . . ? N6 Sr O4 C28 -7.36(17) . . . . ? C15 Sr O4 C28 -110.73(16) . . . . ? C7 Sr O4 C28 95.02(16) . . . . ? I Sr O4 C28 172.46(15) . . . . ? C28 O4 C25 C26 21.4(3) . . . . ? Sr O4 C25 C26 -163.01(15) . . . . ? O4 C25 C26 C27A -1.7(4) . . . . ? O4 C25 C26 C27B -36.3(5) . . . . ? C25 C26 C27A C28 -17.4(5) . . . . ? C27B C26 C27A C28 66.5(5) . . . . ? C25 C26 C27B C28 37.0(8) . . . . ? C27A C26 C27B C28 -67.0(6) . . . . ? C25 O4 C28 C27B 3.8(6) . . . . ? Sr O4 C28 C27B -172.5(6) . . . . ? C25 O4 C28 C27A -33.2(4) . . . . ? Sr O4 C28 C27A 150.5(3) . . . . ? C26 C27B C28 O4 -26.3(9) . . . . ? C26 C27B C28 C27A 65.6(6) . . . . ? C26 C27A C28 O4 30.8(5) . . . . ? C26 C27A C28 C27B -68.7(5) . . . . ? #END OF CIF#\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2008-06-10 at 15:24:28 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : shelxl dreduc import struct data_Chisholm1530 _database_code_depnum_ccdc_archive 'CCDC 695435' _audit_creation_date 2008-06-10T15:24:28-00:00 _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_name_common 'Chisholm 1530' _chemical_formula_moiety 'C32 H54 B1 Ba1 I1 N8 O4' _chemical_formula_sum 'C32 H54 B Ba I N8 O4' _chemical_formula_weight 889.88 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 11.0753(1) _cell_length_b 11.7463(1) _cell_length_c 30.4946(3) _cell_angle_alpha 90 _cell_angle_beta 91.149(1) _cell_angle_gamma 90 _cell_volume 3966.36(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9279 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description 'almost cube' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.23 _exptl_crystal_density_diffrn 1.49 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_special_details ;The data collection crystal was a colorless, approximately cube-shaped block, which was cut from a very large rectangular plate. Examination of the diffraction pattern on a Nonius Kappa CCD diffractometer indicated a monoclinic crystal system. All work was done at 150 K using an Oxford Cryosystems Cryostream Cooler. The data collection strategy was set up to measure a quadrant of reciprocal space with a redundancy factor of 3.7, which means that 90% of the reflections were measured at least 3.7 times. Phi and omega scans with a frame width of 1.0\% were used. Data integration was done with Denzo, and scaling and merging of the data was done with Scalepack. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.823 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.573 _exptl_absorpt_correction_T_max 0.658 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor, 1997)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.509241E-1 _diffrn_orient_matrix_ub_12 -0.675126E-1 _diffrn_orient_matrix_ub_13 -0.316944E-1 _diffrn_orient_matrix_ub_21 -0.379993E-1 _diffrn_orient_matrix_ub_22 -0.69526E-2 _diffrn_orient_matrix_ub_23 0.758642E-1 _diffrn_orient_matrix_ub_31 -0.231566E-1 _diffrn_orient_matrix_ub_32 0.211233E-1 _diffrn_orient_matrix_ub_33 -0.9663E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_av_unetI/netI ? _diffrn_reflns_number 69067 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 9053 _reflns_number_gt 6226 _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 'w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 9053 _refine_ls_number_parameters 428 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0646 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0541 _refine_ls_wR_factor_gt 0.0486 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.819 _refine_diff_density_min -0.784 _refine_diff_density_rms 0.093 #----------------------------------------------------------------------------# # 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 N1 N -0.06464(17) 0.10949(17) 0.06370(7) 0.0218(5) Uani 1 1 d . . . C2 C -0.0945(2) 0.0108(2) 0.04425(9) 0.0265(6) Uani 1 1 d . . . H2 H -0.1323 0.0033 0.0162 0.032 Uiso 1 1 calc R . . C3 C -0.0619(2) -0.0769(2) 0.07115(9) 0.0295(7) Uani 1 1 d . . . H3 H -0.0724 -0.156 0.0658 0.035 Uiso 1 1 calc R . . C4 C 0.0404(2) -0.0861(2) 0.14878(9) 0.0280(7) Uani 1 1 d . . . C5 C 0.1049(2) -0.0066(2) 0.18090(9) 0.0314(7) Uani 1 1 d . . . H5A H 0.1355 -0.0514 0.2063 0.038 Uiso 1 1 calc R . . H5B H 0.1753 0.0276 0.1664 0.038 Uiso 1 1 calc R . . C6 C 0.0261(3) 0.0930(2) 0.24299(9) 0.0434(8) Uani 1 1 d . . . H6A H -0.0288 0.1545 0.2512 0.065 Uiso 1 1 calc R . . H6B H 0.1076 0.1098 0.2543 0.065 Uiso 1 1 calc R . . H6C H -0.0019 0.0211 0.2555 0.065 Uiso 1 1 calc R . . C7 C 0.1355(2) -0.1731(2) 0.13463(10) 0.0477(9) Uani 1 1 d . . . H7A H 0.0986 -0.2273 0.1139 0.072 Uiso 1 1 calc R . . H7B H 0.1665 -0.2142 0.1605 0.072 Uiso 1 1 calc R . . H7C H 0.2021 -0.1334 0.1205 0.072 Uiso 1 1 calc R . . C8 C -0.0623(2) -0.1475(2) 0.17216(9) 0.0396(8) Uani 1 1 d . . . H8A H -0.1042 -0.1984 0.1514 0.059 Uiso 1 1 calc R . . H8B H -0.1195 -0.0912 0.1833 0.059 Uiso 1 1 calc R . . H8C H -0.0289 -0.1921 0.1967 0.059 Uiso 1 1 calc R . . C9 C -0.2111(2) 0.3999(2) 0.13729(8) 0.0238(6) Uani 1 1 d . . . C10 C -0.3193(2) 0.3783(2) 0.11408(9) 0.0364(7) Uani 1 1 d . . . H10 H -0.3981 0.4031 0.1213 0.044 Uiso 1 1 calc R . . C11 C -0.2874(2) 0.3141(2) 0.07887(9) 0.0320(7) Uani 1 1 d . . . H11 H -0.3415 0.2861 0.0568 0.038 Uiso 1 1 calc R . . C12 C -0.1961(2) 0.4683(2) 0.17852(9) 0.0287(7) Uani 1 1 d . . . C13 C -0.0639(2) 0.5026(2) 0.18773(9) 0.0307(7) Uani 1 1 d . . . H13A H -0.0299 0.5347 0.1606 0.037 Uiso 1 1 calc R . . H13B H -0.0618 0.563 0.2104 0.037 Uiso 1 1 calc R . . C14 C 0.0484(3) 0.4175(2) 0.24742(9) 0.0434(8) Uani 1 1 d . . . H14A H 0.0983 0.3513 0.2552 0.065 Uiso 1 1 calc R . . H14B H -0.0226 0.4195 0.2661 0.065 Uiso 1 1 calc R . . H14C H 0.0957 0.4872 0.2518 0.065 Uiso 1 1 calc R . . C15 C -0.2462(2) 0.4020(2) 0.21764(9) 0.0391(8) Uani 1 1 d . . . H15A H -0.2354 0.4472 0.2445 0.059 Uiso 1 1 calc R . . H15B H -0.2028 0.3297 0.2209 0.059 Uiso 1 1 calc R . . H15C H -0.3324 0.3869 0.2125 0.059 Uiso 1 1 calc R . . C16 C -0.2666(2) 0.5809(2) 0.17274(10) 0.0489(9) Uani 1 1 d . . . H16A H -0.2572 0.627 0.1994 0.073 Uiso 1 1 calc R . . H16B H -0.3523 0.5642 0.1674 0.073 Uiso 1 1 calc R . . H16C H -0.2349 0.623 0.1477 0.073 Uiso 1 1 calc R . . C17 C 0.1807(2) 0.3936(2) 0.03272(8) 0.0216(6) Uani 1 1 d . . . C18 C 0.1323(2) 0.4054(2) -0.00964(8) 0.0265(6) Uani 1 1 d . . . H18 H 0.1646 0.4468 -0.0334 0.032 Uiso 1 1 calc R . . C19 C 0.0274(2) 0.3436(2) -0.00903(8) 0.0263(6) Uani 1 1 d . . . H19 H -0.0278 0.3353 -0.0331 0.032 Uiso 1 1 calc R . . C20 C 0.2991(2) 0.4443(2) 0.04966(9) 0.0248(6) Uani 1 1 d . . . C21 C 0.3232(2) 0.4232(2) 0.09840(8) 0.0286(7) Uani 1 1 d . . . H21A H 0.3301 0.3402 0.1036 0.034 Uiso 1 1 calc R . . H21B H 0.4012 0.4585 0.1071 0.034 Uiso 1 1 calc R . . C22 C 0.2735(2) 0.5398(2) 0.15990(9) 0.0378(8) Uani 1 1 d . . . H22A H 0.2052 0.5682 0.1766 0.057 Uiso 1 1 calc R . . H22B H 0.3176 0.6042 0.1475 0.057 Uiso 1 1 calc R . . H22C H 0.3277 0.4962 0.1793 0.057 Uiso 1 1 calc R . . C23 C 0.4032(2) 0.3864(2) 0.02534(9) 0.0385(8) Uani 1 1 d . . . H23A H 0.3921 0.3978 -0.0063 0.058 Uiso 1 1 calc R . . H23B H 0.4035 0.3047 0.0318 0.058 Uiso 1 1 calc R . . H23C H 0.4803 0.4199 0.035 0.058 Uiso 1 1 calc R . . C24 C 0.3004(2) 0.5729(2) 0.04117(9) 0.0351(7) Uani 1 1 d . . . H24A H 0.2849 0.5874 0.0099 0.053 Uiso 1 1 calc R . . H24B H 0.3796 0.604 0.0497 0.053 Uiso 1 1 calc R . . H24C H 0.2377 0.6096 0.0584 0.053 Uiso 1 1 calc R . . C25 C 0.2707(2) 0.0765(2) 0.06184(9) 0.0363(8) Uani 1 1 d . . . H25 H 0.2065 0.0973 0.0423 0.044 Uiso 1 1 calc R . . C26 C 0.3556(2) -0.0080(2) 0.05303(9) 0.0348(7) Uani 1 1 d . . . H26 H 0.3594 -0.0541 0.0275 0.042 Uiso 1 1 calc R . . C27 C 0.4323(2) -0.0105(2) 0.08902(8) 0.0227(6) Uani 1 1 d . . . C28 C 0.5393(2) -0.0854(2) 0.10051(9) 0.0264(6) Uani 1 1 d . . . C29 C 0.6418(2) -0.0138(2) 0.12061(9) 0.0316(7) Uani 1 1 d . . . H29A H 0.715 -0.0613 0.1246 0.038 Uiso 1 1 calc R . . H29B H 0.6612 0.0499 0.1007 0.038 Uiso 1 1 calc R . . C30 C 0.6882(2) 0.1121(2) 0.17880(9) 0.0390(8) Uani 1 1 d . . . H30A H 0.6601 0.1396 0.2072 0.059 Uiso 1 1 calc R . . H30B H 0.6932 0.1761 0.1583 0.059 Uiso 1 1 calc R . . H30C H 0.7682 0.0774 0.1826 0.059 Uiso 1 1 calc R . . C31 C 0.5865(2) -0.1414(2) 0.05877(9) 0.0432(8) Uani 1 1 d . . . H31A H 0.6556 -0.1902 0.0663 0.065 Uiso 1 1 calc R . . H31B H 0.6118 -0.0823 0.0382 0.065 Uiso 1 1 calc R . . H31C H 0.5223 -0.1874 0.0451 0.065 Uiso 1 1 calc R . . C32 C 0.5011(2) -0.1772(2) 0.13276(9) 0.0385(8) Uani 1 1 d . . . H32A H 0.5706 -0.2257 0.1402 0.058 Uiso 1 1 calc R . . H32B H 0.4368 -0.2236 0.1194 0.058 Uiso 1 1 calc R . . H32C H 0.4715 -0.1412 0.1595 0.058 Uiso 1 1 calc R . . B B -0.0962(2) 0.2295(2) 0.04621(10) 0.0243(7) Uani 1 1 d . . . H1B H -0.1509 0.2188 0.02 0.029 Uiso 1 1 calc R . . Ba Ba 0.111844(12) 0.264404(12) 0.145239(5) 0.01885(5) Uani 1 1 d . . . I I 0.361489(15) 0.242623(15) 0.216997(6) 0.03084(6) Uani 1 1 d . . . C1 C -0.0098(2) -0.0256(2) 0.10825(9) 0.0226(6) Uani 1 1 d . . . N2 N -0.01214(17) 0.08779(16) 0.10388(7) 0.0234(5) Uani 1 1 d . . . N3 N -0.16791(17) 0.29679(17) 0.08027(7) 0.0215(5) Uani 1 1 d . . . N4 N -0.11927(17) 0.34948(16) 0.11682(7) 0.0218(5) Uani 1 1 d . . . N5 N 0.01445(17) 0.29680(17) 0.03059(6) 0.0211(5) Uani 1 1 d . . . N6 N 0.11054(16) 0.32783(17) 0.05738(6) 0.0206(5) Uani 1 1 d . . . N7 N 0.29059(18) 0.12415(17) 0.10069(7) 0.0271(5) Uani 1 1 d . . . N8 N 0.38977(19) 0.06904(18) 0.11648(8) 0.0242(5) Uani 1 1 d . . . H1N8 H 0.419(2) 0.089(2) 0.1412(8) 0.032(8) Uiso 1 1 d . . . O1 O 0.02824(15) 0.08357(14) 0.19663(6) 0.0307(5) Uani 1 1 d . . . O2 O 0.01022(15) 0.40948(15) 0.20236(6) 0.0307(5) Uani 1 1 d . . . O3 O 0.23004(14) 0.46826(14) 0.12531(5) 0.0268(4) Uani 1 1 d . . . O4 O 0.60578(14) 0.02979(14) 0.16182(6) 0.0290(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0211(12) 0.0223(12) 0.0218(13) -0.0027(10) -0.0033(10) -0.0012(9) C2 0.0237(15) 0.0287(16) 0.0269(17) -0.0097(13) 0.0002(12) -0.0056(12) C3 0.0333(17) 0.0191(15) 0.0362(19) -0.0068(13) 0.0037(14) -0.0039(13) C4 0.0237(15) 0.0194(15) 0.0406(19) 0.0037(13) -0.0040(13) 0.0013(12) C5 0.0281(16) 0.0280(16) 0.0376(18) 0.0090(14) -0.0088(13) 0.0029(13) C6 0.050(2) 0.050(2) 0.030(2) 0.0086(16) 0.0032(16) -0.0075(16) C7 0.0419(19) 0.0281(18) 0.073(3) 0.0005(16) -0.0119(17) 0.0143(14) C8 0.0384(17) 0.0318(17) 0.048(2) 0.0158(15) -0.0125(15) -0.0099(14) C9 0.0211(14) 0.0224(15) 0.0281(17) 0.0063(12) 0.0051(12) 0.0017(12) C10 0.0204(15) 0.055(2) 0.0340(19) -0.0002(16) 0.0041(14) 0.0137(14) C11 0.0178(15) 0.0460(19) 0.0320(18) 0.0075(15) -0.0056(13) 0.0011(13) C12 0.0274(15) 0.0198(15) 0.0393(19) -0.0030(13) 0.0088(13) 0.0015(12) C13 0.0352(17) 0.0224(15) 0.0346(18) -0.0027(13) 0.0052(14) 0.0017(13) C14 0.057(2) 0.0406(19) 0.032(2) -0.0100(15) -0.0040(16) 0.0090(16) C15 0.0407(18) 0.0396(19) 0.038(2) -0.0134(15) 0.0147(15) -0.0085(14) C16 0.0374(18) 0.0300(18) 0.080(3) -0.0091(17) 0.0089(17) 0.0077(14) C17 0.0214(14) 0.0206(14) 0.0228(16) 0.0010(12) 0.0024(12) 0.0055(11) C18 0.0302(16) 0.0300(16) 0.0193(16) 0.0047(13) 0.0029(13) 0.0012(13) C19 0.0344(16) 0.0270(16) 0.0175(16) 0.0011(12) -0.0031(13) 0.0117(13) C20 0.0208(14) 0.0263(15) 0.0272(17) 0.0058(13) 0.0031(12) 0.0010(12) C21 0.0203(15) 0.0305(16) 0.0348(18) 0.0036(14) -0.0019(13) -0.0023(12) C22 0.0444(18) 0.0263(17) 0.042(2) -0.0050(14) -0.0081(15) -0.0068(14) C23 0.0271(16) 0.0436(19) 0.045(2) 0.0029(16) 0.0087(14) 0.0036(14) C24 0.0322(16) 0.0337(18) 0.0392(19) 0.0111(14) -0.0019(14) -0.0035(13) C25 0.0396(18) 0.0419(19) 0.0267(18) -0.0093(14) -0.0141(14) 0.0167(14) C26 0.0438(18) 0.0364(18) 0.0239(17) -0.0137(14) -0.0036(14) 0.0131(14) C27 0.0252(15) 0.0216(15) 0.0214(16) -0.0018(12) 0.0051(12) 0.0029(12) C28 0.0261(15) 0.0253(16) 0.0278(17) -0.0023(13) 0.0021(13) 0.0054(12) C29 0.0259(15) 0.0383(18) 0.0309(18) 0.0044(14) 0.0046(13) 0.0053(13) C30 0.0388(17) 0.0377(18) 0.040(2) 0.0006(15) -0.0049(15) -0.0030(15) C31 0.0405(18) 0.046(2) 0.043(2) -0.0093(16) 0.0027(15) 0.0176(15) C32 0.0447(18) 0.0252(17) 0.045(2) 0.0041(14) -0.0058(15) 0.0044(14) B 0.0210(15) 0.0285(18) 0.0230(17) -0.0021(14) -0.0106(13) 0.0022(14) Ba 0.01909(8) 0.01851(9) 0.01885(9) -0.00040(7) -0.00196(6) 0.00168(7) I 0.03229(10) 0.03012(12) 0.02962(11) -0.00693(8) -0.01149(8) 0.00580(8) C1 0.0183(14) 0.0206(15) 0.0289(17) 0.0008(12) 0.0032(12) 0.0010(11) N2 0.0216(12) 0.0197(12) 0.0284(14) 0.0014(10) -0.0089(10) 0.0010(9) N3 0.0183(11) 0.0244(12) 0.0218(13) 0.0054(10) -0.0035(10) 0.0020(9) N4 0.0192(11) 0.0181(12) 0.0280(14) -0.0022(10) -0.0011(10) 0.0019(9) N5 0.0214(12) 0.0229(12) 0.0187(12) -0.0001(10) -0.0039(10) 0.0038(9) N6 0.0163(11) 0.0272(13) 0.0182(12) 0.0019(10) -0.0045(9) 0.0028(9) N7 0.0258(13) 0.0280(13) 0.0274(14) -0.0056(11) -0.0046(11) 0.0113(10) N8 0.0240(13) 0.0267(14) 0.0215(14) -0.0043(11) -0.0050(11) 0.0047(10) O1 0.0389(11) 0.0275(11) 0.0258(12) 0.0042(9) -0.0017(9) 0.0038(9) O2 0.0363(11) 0.0313(11) 0.0244(12) -0.0092(9) -0.0001(9) 0.0063(9) O3 0.0247(10) 0.0332(11) 0.0224(11) -0.0046(9) 0.0015(8) -0.0043(8) O4 0.0245(10) 0.0319(11) 0.0304(12) -0.0056(9) -0.0011(9) -0.0036(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ;For the methyl groups, the hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5 *Ueq(bonded carbon atom). The hydrogen atom bonded to N(8) was refined isotropically. The remaining hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(attached atom). All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C2 1.340(3) . ? N1 N2 1.369(3) . ? N1 B 1.545(3) . ? C2 C3 1.362(3) . ? C2 H2 0.95 . ? C3 C1 1.396(3) . ? C3 H3 0.95 . ? C4 C1 1.521(3) . ? C4 C5 1.521(3) . ? C4 C8 1.535(3) . ? C4 C7 1.536(3) . ? C5 O1 1.445(3) . ? C5 Ba 3.365(3) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 O1 1.419(3) . ? 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 . ? C9 N4 1.342(3) . ? C9 C10 1.403(3) . ? C9 C12 1.498(3) . ? C10 C11 1.364(4) . ? C10 H10 0.95 . ? C11 N3 1.339(3) . ? C11 H11 0.95 . ? C12 C15 1.537(3) . ? C12 C13 1.539(3) . ? C12 C16 1.544(3) . ? C13 O2 1.434(3) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 O2 1.433(3) . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 N6 1.338(3) . ? C17 C18 1.396(3) . ? C17 C20 1.521(3) . ? C18 C19 1.370(3) . ? C18 H18 0.95 . ? C19 N5 1.338(3) . ? C19 H19 0.95 . ? C20 C21 1.525(3) . ? C20 C24 1.533(3) . ? C20 C23 1.542(3) . ? C21 O3 1.432(3) . ? C21 Ba 3.336(2) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 O3 1.425(3) . ? 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 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 N7 1.325(3) . ? C25 C26 1.396(3) . ? C25 H25 0.95 . ? C26 C27 1.375(3) . ? C26 H26 0.95 . ? C27 N8 1.346(3) . ? C27 C28 1.512(3) . ? C28 C32 1.525(3) . ? C28 C29 1.530(3) . ? C28 C31 1.534(3) . ? C29 O4 1.421(3) . ? C29 H29A 0.99 . ? C29 H29B 0.99 . ? C30 O4 1.420(3) . ? 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 . ? B N3 1.539(3) . ? B N5 1.542(3) . ? B H1B 1 . ? Ba O2 2.6988(16) . ? Ba N2 2.7769(19) . ? Ba N6 2.781(2) . ? Ba O3 2.8015(16) . ? Ba O1 2.8078(17) . ? Ba N4 2.8657(19) . ? Ba N7 2.930(2) . ? Ba I 3.5008(2) . ? C1 N2 1.339(3) . ? N3 N4 1.375(3) . ? N5 N6 1.378(2) . ? N7 N8 1.355(3) . ? N8 H1N8 0.85(2) . ? 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 C2 N1 N2 109.4(2) . . ? C2 N1 B 125.7(2) . . ? N2 N1 B 124.6(2) . . ? N1 C2 C3 109.1(2) . . ? N1 C2 H2 125.4 . . ? C3 C2 H2 125.4 . . ? C2 C3 C1 105.2(2) . . ? C2 C3 H3 127.4 . . ? C1 C3 H3 127.4 . . ? C1 C4 C5 113.3(2) . . ? C1 C4 C8 109.5(2) . . ? C5 C4 C8 109.4(2) . . ? C1 C4 C7 108.9(2) . . ? C5 C4 C7 105.9(2) . . ? C8 C4 C7 109.7(2) . . ? O1 C5 C4 113.1(2) . . ? O1 C5 Ba 55.37(11) . . ? C4 C5 Ba 112.72(16) . . ? O1 C5 H5A 109 . . ? C4 C5 H5A 109 . . ? Ba C5 H5A 138.3 . . ? O1 C5 H5B 109 . . ? C4 C5 H5B 109 . . ? Ba C5 H5B 56.5 . . ? H5A C5 H5B 107.8 . . ? O1 C6 H6A 109.5 . . ? O1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 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 . . ? N4 C9 C10 109.5(2) . . ? N4 C9 C12 123.7(2) . . ? C10 C9 C12 126.8(2) . . ? C11 C10 C9 105.4(2) . . ? C11 C10 H10 127.3 . . ? C9 C10 H10 127.3 . . ? N3 C11 C10 109.3(2) . . ? N3 C11 H11 125.4 . . ? C10 C11 H11 125.4 . . ? C9 C12 C15 110.1(2) . . ? C9 C12 C13 112.5(2) . . ? C15 C12 C13 110.4(2) . . ? C9 C12 C16 108.4(2) . . ? C15 C12 C16 109.4(2) . . ? C13 C12 C16 105.8(2) . . ? O2 C13 C12 113.2(2) . . ? O2 C13 H13A 108.9 . . ? C12 C13 H13A 108.9 . . ? O2 C13 H13B 108.9 . . ? C12 C13 H13B 108.9 . . ? H13A C13 H13B 107.8 . . ? O2 C14 H14A 109.5 . . ? O2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N6 C17 C18 111.2(2) . . ? N6 C17 C20 122.8(2) . . ? C18 C17 C20 126.0(2) . . ? C19 C18 C17 104.2(2) . . ? C19 C18 H18 127.9 . . ? C17 C18 H18 127.9 . . ? N5 C19 C18 109.6(2) . . ? N5 C19 H19 125.2 . . ? C18 C19 H19 125.2 . . ? C17 C20 C21 113.6(2) . . ? C17 C20 C24 109.9(2) . . ? C21 C20 C24 108.8(2) . . ? C17 C20 C23 108.2(2) . . ? C21 C20 C23 106.2(2) . . ? C24 C20 C23 110.1(2) . . ? O3 C21 C20 112.6(2) . . ? O3 C21 Ba 56.08(11) . . ? C20 C21 Ba 113.44(15) . . ? O3 C21 H21A 109.1 . . ? C20 C21 H21A 109.1 . . ? Ba C21 H21A 55.5 . . ? O3 C21 H21B 109.1 . . ? C20 C21 H21B 109.1 . . ? Ba C21 H21B 137.4 . . ? H21A C21 H21B 107.8 . . ? O3 C22 H22A 109.5 . . ? O3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O3 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 . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N7 C25 C26 111.8(2) . . ? N7 C25 H25 124.1 . . ? C26 C25 H25 124.1 . . ? C27 C26 C25 105.6(2) . . ? C27 C26 H26 127.2 . . ? C25 C26 H26 127.2 . . ? N8 C27 C26 105.2(2) . . ? N8 C27 C28 122.8(2) . . ? C26 C27 C28 131.8(2) . . ? C27 C28 C32 109.6(2) . . ? C27 C28 C29 110.2(2) . . ? C32 C28 C29 110.1(2) . . ? C27 C28 C31 109.6(2) . . ? C32 C28 C31 109.6(2) . . ? C29 C28 C31 107.8(2) . . ? O4 C29 C28 109.5(2) . . ? O4 C29 H29A 109.8 . . ? C28 C29 H29A 109.8 . . ? O4 C29 H29B 109.8 . . ? C28 C29 H29B 109.8 . . ? H29A C29 H29B 108.2 . . ? O4 C30 H30A 109.5 . . ? O4 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O4 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C28 C32 H32A 109.5 . . ? C28 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C28 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N3 B N5 111.7(2) . . ? N3 B N1 110.6(2) . . ? N5 B N1 113.5(2) . . ? N3 B H1B 106.9 . . ? N5 B H1B 106.9 . . ? N1 B H1B 106.9 . . ? O2 Ba N2 123.78(5) . . ? O2 Ba N6 117.29(5) . . ? N2 Ba N6 76.68(6) . . ? O2 Ba O3 78.64(5) . . ? N2 Ba O3 140.26(5) . . ? N6 Ba O3 63.60(5) . . ? O2 Ba O1 88.34(5) . . ? N2 Ba O1 61.49(5) . . ? N6 Ba O1 138.17(5) . . ? O3 Ba O1 158.19(5) . . ? O2 Ba N4 66.01(5) . . ? N2 Ba N4 72.10(5) . . ? N6 Ba N4 68.15(5) . . ? O3 Ba N4 93.14(5) . . ? O1 Ba N4 97.47(5) . . ? O2 Ba N7 161.55(5) . . ? N2 Ba N7 72.66(6) . . ? N6 Ba N7 72.21(6) . . ? O3 Ba N7 93.27(5) . . ? O1 Ba N7 93.83(5) . . ? N4 Ba N7 131.57(6) . . ? O2 Ba C21 103.21(6) . . ? N2 Ba C21 124.61(6) . . ? N6 Ba C21 55.10(6) . . ? O3 Ba C21 25.10(5) . . ? O1 Ba C21 154.68(5) . . ? N4 Ba C21 107.79(6) . . ? N7 Ba C21 68.26(6) . . ? O2 Ba C5 112.10(6) . . ? N2 Ba C5 54.96(6) . . ? N6 Ba C5 124.41(6) . . ? O3 Ba C5 153.18(5) . . ? O1 Ba C5 25.05(5) . . ? N4 Ba C5 113.67(6) . . ? N7 Ba C5 68.78(6) . . ? C21 Ba C5 133.47(6) . . ? O2 Ba I 88.69(4) . . ? N2 Ba I 127.34(4) . . ? N6 Ba I 127.63(4) . . ? O3 Ba I 80.29(3) . . ? O1 Ba I 82.01(3) . . ? N4 Ba I 154.68(4) . . ? N7 Ba I 73.51(4) . . ? C21 Ba I 75.91(4) . . ? C5 Ba I 75.63(4) . . ? N2 C1 C3 110.0(2) . . ? N2 C1 C4 123.4(2) . . ? C3 C1 C4 126.6(2) . . ? C1 N2 N1 106.3(2) . . ? C1 N2 Ba 133.61(16) . . ? N1 N2 Ba 117.68(14) . . ? C11 N3 N4 109.2(2) . . ? C11 N3 B 125.4(2) . . ? N4 N3 B 125.41(19) . . ? C9 N4 N3 106.70(19) . . ? C9 N4 Ba 133.95(17) . . ? N3 N4 Ba 114.90(13) . . ? C19 N5 N6 109.4(2) . . ? C19 N5 B 126.1(2) . . ? N6 N5 B 124.2(2) . . ? C17 N6 N5 105.64(19) . . ? C17 N6 Ba 134.81(16) . . ? N5 N6 Ba 119.31(14) . . ? C25 N7 N8 103.6(2) . . ? C25 N7 Ba 123.39(16) . . ? N8 N7 Ba 130.87(16) . . ? C27 N8 N7 113.7(2) . . ? C27 N8 H1N8 127.9(17) . . ? N7 N8 H1N8 118.4(17) . . ? C6 O1 C5 114.2(2) . . ? C6 O1 Ba 120.63(15) . . ? C5 O1 Ba 99.58(14) . . ? C14 O2 C13 113.86(19) . . ? C14 O2 Ba 122.79(14) . . ? C13 O2 Ba 121.65(15) . . ? C22 O3 C21 113.94(19) . . ? C22 O3 Ba 119.73(15) . . ? C21 O3 Ba 98.82(13) . . ? C30 O4 C29 112.21(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 N1 C2 C3 -0.2(3) . . . . ? B N1 C2 C3 -174.1(2) . . . . ? N1 C2 C3 C1 -0.2(3) . . . . ? C1 C4 C5 O1 59.0(3) . . . . ? C8 C4 C5 O1 -63.6(3) . . . . ? C7 C4 C5 O1 178.3(2) . . . . ? C1 C4 C5 Ba -1.6(3) . . . . ? C8 C4 C5 Ba -124.15(17) . . . . ? C7 C4 C5 Ba 117.74(18) . . . . ? N4 C9 C10 C11 -0.6(3) . . . . ? C12 C9 C10 C11 179.2(3) . . . . ? C9 C10 C11 N3 0.2(3) . . . . ? N4 C9 C12 C15 -107.5(3) . . . . ? C10 C9 C12 C15 72.6(3) . . . . ? N4 C9 C12 C13 16.0(3) . . . . ? C10 C9 C12 C13 -163.8(2) . . . . ? N4 C9 C12 C16 132.7(2) . . . . ? C10 C9 C12 C16 -47.1(3) . . . . ? C9 C12 C13 O2 -73.2(3) . . . . ? C15 C12 C13 O2 50.2(3) . . . . ? C16 C12 C13 O2 168.6(2) . . . . ? N6 C17 C18 C19 0.6(3) . . . . ? C20 C17 C18 C19 179.0(2) . . . . ? C17 C18 C19 N5 -0.8(3) . . . . ? N6 C17 C20 C21 -5.9(3) . . . . ? C18 C17 C20 C21 175.9(2) . . . . ? N6 C17 C20 C24 -128.1(2) . . . . ? C18 C17 C20 C24 53.8(3) . . . . ? N6 C17 C20 C23 111.7(3) . . . . ? C18 C17 C20 C23 -66.4(3) . . . . ? C17 C20 C21 O3 -58.6(3) . . . . ? C24 C20 C21 O3 64.1(3) . . . . ? C23 C20 C21 O3 -177.4(2) . . . . ? C17 C20 C21 Ba 2.8(2) . . . . ? C24 C20 C21 Ba 125.50(17) . . . . ? C23 C20 C21 Ba -116.01(17) . . . . ? N7 C25 C26 C27 -0.5(3) . . . . ? C25 C26 C27 N8 0.6(3) . . . . ? C25 C26 C27 C28 177.4(3) . . . . ? N8 C27 C28 C32 75.6(3) . . . . ? C26 C27 C28 C32 -100.8(3) . . . . ? N8 C27 C28 C29 -45.7(3) . . . . ? C26 C27 C28 C29 138.0(3) . . . . ? N8 C27 C28 C31 -164.1(2) . . . . ? C26 C27 C28 C31 19.5(4) . . . . ? C27 C28 C29 O4 66.6(3) . . . . ? C32 C28 C29 O4 -54.4(3) . . . . ? C31 C28 C29 O4 -173.8(2) . . . . ? C2 N1 B N3 122.8(2) . . . . ? N2 N1 B N3 -50.2(3) . . . . ? C2 N1 B N5 -110.8(3) . . . . ? N2 N1 B N5 76.2(3) . . . . ? O3 C21 Ba O2 -12.02(14) . . . . ? C20 C21 Ba O2 -114.37(16) . . . . ? O3 C21 Ba N2 136.84(12) . . . . ? C20 C21 Ba N2 34.49(19) . . . . ? O3 C21 Ba N6 102.21(14) . . . . ? C20 C21 Ba N6 -0.13(15) . . . . ? C20 C21 Ba O3 -102.3(2) . . . . ? O3 C21 Ba O1 -127.27(14) . . . . ? C20 C21 Ba O1 130.38(16) . . . . ? O3 C21 Ba N4 56.67(14) . . . . ? C20 C21 Ba N4 -45.67(18) . . . . ? O3 C21 Ba N7 -174.85(14) . . . . ? C20 C21 Ba N7 82.81(17) . . . . ? O3 C21 Ba C5 -151.05(12) . . . . ? C20 C21 Ba C5 106.61(17) . . . . ? O3 C21 Ba I -97.25(13) . . . . ? C20 C21 Ba I 160.40(17) . . . . ? O1 C5 Ba O2 19.53(14) . . . . ? C4 C5 Ba O2 122.67(16) . . . . ? O1 C5 Ba N2 -97.11(14) . . . . ? C4 C5 Ba N2 6.04(15) . . . . ? O1 C5 Ba N6 -131.86(12) . . . . ? C4 C5 Ba N6 -28.72(19) . . . . ? O1 C5 Ba O3 128.90(14) . . . . ? C4 C5 Ba O3 -127.95(16) . . . . ? C4 C5 Ba O1 103.1(2) . . . . ? O1 C5 Ba N4 -52.95(14) . . . . ? C4 C5 Ba N4 50.20(18) . . . . ? O1 C5 Ba N7 179.68(15) . . . . ? C4 C5 Ba N7 -77.17(17) . . . . ? O1 C5 Ba C21 155.97(12) . . . . ? C4 C5 Ba C21 -100.88(17) . . . . ? O1 C5 Ba I 102.08(13) . . . . ? C4 C5 Ba I -154.77(17) . . . . ? C2 C3 C1 N2 0.5(3) . . . . ? C2 C3 C1 C4 179.1(2) . . . . ? C5 C4 C1 N2 -8.8(3) . . . . ? C8 C4 C1 N2 113.8(3) . . . . ? C7 C4 C1 N2 -126.3(2) . . . . ? C5 C4 C1 C3 172.8(2) . . . . ? C8 C4 C1 C3 -64.7(3) . . . . ? C7 C4 C1 C3 55.2(3) . . . . ? C3 C1 N2 N1 -0.6(3) . . . . ? C4 C1 N2 N1 -179.3(2) . . . . ? C3 C1 N2 Ba -162.00(17) . . . . ? C4 C1 N2 Ba 19.3(4) . . . . ? C2 N1 N2 C1 0.5(3) . . . . ? B N1 N2 C1 174.5(2) . . . . ? C2 N1 N2 Ba 165.36(14) . . . . ? B N1 N2 Ba -20.6(3) . . . . ? O2 Ba N2 C1 -108.2(2) . . . . ? N6 Ba N2 C1 137.7(2) . . . . ? O3 Ba N2 C1 136.1(2) . . . . ? O1 Ba N2 C1 -42.0(2) . . . . ? N4 Ba N2 C1 -151.3(2) . . . . ? N7 Ba N2 C1 62.5(2) . . . . ? C21 Ba N2 C1 109.1(2) . . . . ? C5 Ba N2 C1 -13.4(2) . . . . ? I Ba N2 C1 10.2(2) . . . . ? O2 Ba N2 N1 92.06(16) . . . . ? N6 Ba N2 N1 -22.05(15) . . . . ? O3 Ba N2 N1 -23.66(19) . . . . ? O1 Ba N2 N1 158.29(17) . . . . ? N4 Ba N2 N1 48.97(15) . . . . ? N7 Ba N2 N1 -97.27(16) . . . . ? C21 Ba N2 N1 -50.66(17) . . . . ? C5 Ba N2 N1 -173.14(18) . . . . ? I Ba N2 N1 -149.53(13) . . . . ? C10 C11 N3 N4 0.2(3) . . . . ? C10 C11 N3 B -179.3(2) . . . . ? N5 B N3 C11 130.3(2) . . . . ? N1 B N3 C11 -102.3(3) . . . . ? N5 B N3 N4 -49.2(3) . . . . ? N1 B N3 N4 78.2(3) . . . . ? C10 C9 N4 N3 0.7(3) . . . . ? C12 C9 N4 N3 -179.1(2) . . . . ? C10 C9 N4 Ba -153.42(18) . . . . ? C12 C9 N4 Ba 26.7(4) . . . . ? C11 N3 N4 C9 -0.6(3) . . . . ? B N3 N4 C9 179.0(2) . . . . ? C11 N3 N4 Ba 159.17(15) . . . . ? B N3 N4 Ba -21.3(3) . . . . ? O2 Ba N4 C9 -17.7(2) . . . . ? N2 Ba N4 C9 123.9(2) . . . . ? N6 Ba N4 C9 -153.7(2) . . . . ? O3 Ba N4 C9 -93.8(2) . . . . ? O1 Ba N4 C9 67.1(2) . . . . ? N7 Ba N4 C9 169.0(2) . . . . ? C21 Ba N4 C9 -114.6(2) . . . . ? C5 Ba N4 C9 87.0(2) . . . . ? I Ba N4 C9 -20.0(3) . . . . ? O2 Ba N4 N3 -170.28(16) . . . . ? N2 Ba N4 N3 -28.71(14) . . . . ? N6 Ba N4 N3 53.73(14) . . . . ? O3 Ba N4 N3 113.62(15) . . . . ? O1 Ba N4 N3 -85.47(15) . . . . ? N7 Ba N4 N3 16.44(18) . . . . ? C21 Ba N4 N3 92.83(15) . . . . ? C5 Ba N4 N3 -65.54(16) . . . . ? I Ba N4 N3 -172.57(9) . . . . ? C18 C19 N5 N6 0.6(3) . . . . ? C18 C19 N5 B 174.4(2) . . . . ? N3 B N5 C19 -109.2(3) . . . . ? N1 B N5 C19 125.0(3) . . . . ? N3 B N5 N6 63.7(3) . . . . ? N1 B N5 N6 -62.2(3) . . . . ? C18 C17 N6 N5 -0.3(3) . . . . ? C20 C17 N6 N5 -178.6(2) . . . . ? C18 C17 N6 Ba -174.35(15) . . . . ? C20 C17 N6 Ba 7.3(4) . . . . ? C19 N5 N6 C17 -0.2(2) . . . . ? B N5 N6 C17 -174.1(2) . . . . ? C19 N5 N6 Ba 174.96(14) . . . . ? B N5 N6 Ba 1.1(3) . . . . ? O2 Ba N6 C17 83.6(2) . . . . ? N2 Ba N6 C17 -155.0(2) . . . . ? O3 Ba N6 C17 23.8(2) . . . . ? O1 Ba N6 C17 -154.56(19) . . . . ? N4 Ba N6 C17 129.2(2) . . . . ? N7 Ba N6 C17 -79.2(2) . . . . ? C21 Ba N6 C17 -3.7(2) . . . . ? C5 Ba N6 C17 -126.3(2) . . . . ? I Ba N6 C17 -27.8(2) . . . . ? O2 Ba N6 N5 -89.86(15) . . . . ? N2 Ba N6 N5 31.53(15) . . . . ? O3 Ba N6 N5 -149.63(16) . . . . ? O1 Ba N6 N5 31.97(18) . . . . ? N4 Ba N6 N5 -44.27(14) . . . . ? N7 Ba N6 N5 107.30(16) . . . . ? C21 Ba N6 N5 -177.20(18) . . . . ? C5 Ba N6 N5 60.19(17) . . . . ? I Ba N6 N5 158.71(13) . . . . ? C26 C25 N7 N8 0.2(3) . . . . ? C26 C25 N7 Ba -164.70(18) . . . . ? O2 Ba N7 C25 -167.41(19) . . . . ? N2 Ba N7 C25 37.8(2) . . . . ? N6 Ba N7 C25 -43.4(2) . . . . ? O3 Ba N7 C25 -104.3(2) . . . . ? O1 Ba N7 C25 96.3(2) . . . . ? N4 Ba N7 C25 -7.2(2) . . . . ? C21 Ba N7 C25 -102.1(2) . . . . ? C5 Ba N7 C25 96.2(2) . . . . ? I Ba N7 C25 176.8(2) . . . . ? O2 Ba N7 N8 32.1(3) . . . . ? N2 Ba N7 N8 -122.7(2) . . . . ? N6 Ba N7 N8 156.2(2) . . . . ? O3 Ba N7 N8 95.2(2) . . . . ? O1 Ba N7 N8 -64.1(2) . . . . ? N4 Ba N7 N8 -167.63(18) . . . . ? C21 Ba N7 N8 97.4(2) . . . . ? C5 Ba N7 N8 -64.3(2) . . . . ? I Ba N7 N8 16.38(19) . . . . ? C26 C27 N8 N7 -0.5(3) . . . . ? C28 C27 N8 N7 -177.7(2) . . . . ? C25 N7 N8 C27 0.2(3) . . . . ? Ba N7 N8 C27 163.48(16) . . . . ? C4 C5 O1 C6 127.6(2) . . . . ? Ba C5 O1 C6 -129.9(2) . . . . ? C4 C5 O1 Ba -102.5(2) . . . . ? O2 Ba O1 C6 -36.34(18) . . . . ? N2 Ba O1 C6 -166.79(19) . . . . ? N6 Ba O1 C6 -167.28(16) . . . . ? O3 Ba O1 C6 16.6(2) . . . . ? N4 Ba O1 C6 -101.88(18) . . . . ? N7 Ba O1 C6 125.32(18) . . . . ? C21 Ba O1 C6 81.9(2) . . . . ? C5 Ba O1 C6 125.6(2) . . . . ? I Ba O1 C6 52.57(17) . . . . ? O2 Ba O1 C5 -161.95(13) . . . . ? N2 Ba O1 C5 67.60(13) . . . . ? N6 Ba O1 C5 67.11(15) . . . . ? O3 Ba O1 C5 -109.04(17) . . . . ? N4 Ba O1 C5 132.51(13) . . . . ? N7 Ba O1 C5 -0.30(14) . . . . ? C21 Ba O1 C5 -43.7(2) . . . . ? I Ba O1 C5 -73.04(13) . . . . ? C12 C13 O2 C14 -110.5(2) . . . . ? C12 C13 O2 Ba 84.0(2) . . . . ? N2 Ba O2 C14 117.03(18) . . . . ? N6 Ba O2 C14 -151.07(18) . . . . ? O3 Ba O2 C14 -98.95(18) . . . . ? O1 Ba O2 C14 63.46(18) . . . . ? N4 Ba O2 C14 162.4(2) . . . . ? N7 Ba O2 C14 -33.7(3) . . . . ? C21 Ba O2 C14 -93.78(19) . . . . ? C5 Ba O2 C14 55.32(19) . . . . ? I Ba O2 C14 -18.58(18) . . . . ? N2 Ba O2 C13 -78.75(17) . . . . ? N6 Ba O2 C13 13.15(18) . . . . ? O3 Ba O2 C13 65.28(16) . . . . ? O1 Ba O2 C13 -132.31(16) . . . . ? N4 Ba O2 C13 -33.38(15) . . . . ? N7 Ba O2 C13 130.5(2) . . . . ? C21 Ba O2 C13 70.45(17) . . . . ? C5 Ba O2 C13 -140.45(16) . . . . ? I Ba O2 C13 145.64(16) . . . . ? C20 C21 O3 C22 -128.0(2) . . . . ? Ba C21 O3 C22 128.2(2) . . . . ? C20 C21 O3 Ba 103.83(18) . . . . ? O2 Ba O3 C22 43.90(16) . . . . ? N2 Ba O3 C22 174.11(15) . . . . ? N6 Ba O3 C22 172.35(18) . . . . ? O1 Ba O3 C22 -10.5(2) . . . . ? N4 Ba O3 C22 108.67(17) . . . . ? N7 Ba O3 C22 -119.36(17) . . . . ? C21 Ba O3 C22 -124.2(2) . . . . ? C5 Ba O3 C22 -73.0(2) . . . . ? I Ba O3 C22 -46.71(16) . . . . ? O2 Ba O3 C21 168.06(14) . . . . ? N2 Ba O3 C21 -61.73(16) . . . . ? N6 Ba O3 C21 -63.49(13) . . . . ? O1 Ba O3 C21 113.64(16) . . . . ? N4 Ba O3 C21 -127.18(13) . . . . ? N7 Ba O3 C21 4.79(13) . . . . ? C5 Ba O3 C21 51.1(2) . . . . ? I Ba O3 C21 77.45(13) . . . . ? C28 C29 O4 C30 -170.1(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N8 H1N8 O4 0.85(2) 2.26(2) 2.778(3) 119(2) . N8 H1N8 I 0.85(2) 3.01(2) 3.700(2) 140(2) . #END OF CIF#\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2008-07-08 at 14:39:30 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : shelxl dreduc import struct data_Chisholm1539 _database_code_depnum_ccdc_archive 'CCDC 695436' _audit_creation_date 2008-07-08T14:39:30-00:00 _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_name_common 'Chisholm 1539' _chemical_formula_moiety 'C24 H40 B1 Ba1 I1 N6 O3, C3.5 H4' _chemical_formula_sum 'C27.50 H44 B Ba I N6 O3' _chemical_formula_weight 781.74 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.3403(2) _cell_length_b 12.3916(1) _cell_length_c 26.6151(2) _cell_angle_alpha 90 _cell_angle_beta 109.575(1) _cell_angle_gamma 90 _cell_volume 6631.33(10) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7860 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3112 _exptl_special_details ; The data collection crystal was a colorless plate with an irregular circumference. Examination of the diffraction pattern on a Nonius Kappa CCD diffractometer indicated a monoclinic crystal system. All work was done at 150 K using an Oxford Cryosystems Cryostream Cooler. The data collection strategy was set up to measure a quadrant of reciprocal space with a redundancy factor of 3.8, which means that 90% of the reflections were measured at least 3.8 times. Phi and omega scans with a frame width of 1.0 degree were used. Data integration was done with Denzo, and scaling and merging of the data was done with Scalepack. In addition to the Ba complex, the asymmetric unit contains a toluene molecule on a crystallographic two-fold rotation axis. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.165 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.580 _exptl_absorpt_correction_T_max 0.723 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor, 1997)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.132053E-1 _diffrn_orient_matrix_ub_12 -0.3961E-3 _diffrn_orient_matrix_ub_13 -0.479474E-1 _diffrn_orient_matrix_ub_21 0.61833E-1 _diffrn_orient_matrix_ub_22 -0.488388E-1 _diffrn_orient_matrix_ub_23 0.17433E-1 _diffrn_orient_matrix_ub_31 -0.184388E-1 _diffrn_orient_matrix_ub_32 -0.300158E-1 _diffrn_orient_matrix_ub_33 -0.18689E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_av_unetI/netI ? _diffrn_reflns_number 55260 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.912 _diffrn_measured_fraction_theta_max 0.912 _reflns_number_total 13433 _reflns_number_gt 10175 _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 ;For the methyl groups, the hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5 *Ueq(bonded carbon atom). The remaining hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(attached atom). At this point, there were several large peaks in the difference electron density map (starting at 3.1 e/Ang**3), which did not make chemical sense. As the precession images assembled from the data frames indicated that non-merohedral twinning was a possibility, Rotax was used to generate various twin laws(5). The twin law which corresponds to a 180 degree rotation about the (-3 -1 1) reciprocal lattice direction was applied to the data set and gave a reasonable improvement in the model in terms of slightly lower R factors and much smaller peaks in the difference electron density map. This twin law in matrix form is as follows: [0.537 1.481 0.092 / 0.512 -0.506 0.031 / -0.512 -0.494 -1.031] Since this is a non-merohedral twin, it was necessary to generate and test several data sets based on different overlap criteria for the reflections. The set of overlap criteria which minimized the R factors was chosen as the best set. The final results are based on this modified data set, which contains some reflections exactly overlapped due to twinning and others which are not overlapped. Still other reflections are omitted from the data set because they are partially overlapped with their twin component reflection. 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 'w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+164.5556P] 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 13433 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0589 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.1133 _refine_ls_wR_factor_gt 0.0994 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.515 _refine_diff_density_min -0.949 _refine_diff_density_rms 0.121 #----------------------------------------------------------------------------# # 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0358(3) 0.8403(4) 0.0520(2) 0.0231(11) Uani 1 1 d . . . C2 C -0.0664(3) 0.8952(5) 0.0042(2) 0.0291(12) Uani 1 1 d . . . H2 H -0.1038 0.942 -0.0042 0.035 Uiso 1 1 calc R . . C3 C -0.0303(3) 0.8665(5) -0.0278(2) 0.0286(12) Uani 1 1 d . . . H3 H -0.0383 0.8909 -0.0633 0.034 Uiso 1 1 calc R . . C4 C -0.0534(3) 0.8422(5) 0.1027(2) 0.0262(11) Uani 1 1 d . . . C5 C -0.0369(3) 0.7346(5) 0.1329(2) 0.0297(12) Uani 1 1 d . . . H5A H -0.0482 0.739 0.1656 0.045 Uiso 1 1 calc R . . H5B H 0.0107 0.7195 0.1421 0.045 Uiso 1 1 calc R . . H5C H -0.0626 0.6765 0.1102 0.045 Uiso 1 1 calc R . . C6 C -0.1277(3) 0.8652(5) 0.0897(3) 0.0360(14) Uani 1 1 d . . . H6A H -0.1384 0.8663 0.1227 0.054 Uiso 1 1 calc R . . H6B H -0.1537 0.8087 0.0661 0.054 Uiso 1 1 calc R . . H6C H -0.1385 0.9354 0.0719 0.054 Uiso 1 1 calc R . . C7 C -0.0158(3) 0.9342(5) 0.1385(2) 0.0317(13) Uani 1 1 d . . . H7A H -0.0323 1.0042 0.1211 0.038 Uiso 1 1 calc R . . H7B H -0.0243 0.9319 0.1728 0.038 Uiso 1 1 calc R . . C8 C 0.0897(3) 1.0050(5) 0.1861(3) 0.0402(15) Uani 1 1 d . . . H8A H 0.1374 0.9981 0.1923 0.06 Uiso 1 1 calc R . . H8B H 0.0812 0.9939 0.2198 0.06 Uiso 1 1 calc R . . H8C H 0.0747 1.0773 0.1724 0.06 Uiso 1 1 calc R . . C9 C 0.2176(3) 0.9138(4) 0.0408(2) 0.0228(11) Uani 1 1 d . . . C10 C 0.2259(3) 0.8939(5) -0.0083(2) 0.0280(12) Uani 1 1 d . . . H10 H 0.2607 0.9189 -0.0201 0.034 Uiso 1 1 calc R . . C11 C 0.1728(3) 0.8302(4) -0.0356(2) 0.0265(11) Uani 1 1 d . . . H11 H 0.1639 0.8035 -0.0708 0.032 Uiso 1 1 calc R . . C12 C 0.2602(3) 0.9863(5) 0.0848(2) 0.0260(11) Uani 1 1 d . . . C13 C 0.2681(4) 1.0962(5) 0.0604(3) 0.0387(15) Uani 1 1 d . . . H13A H 0.2956 1.144 0.0885 0.058 Uiso 1 1 calc R . . H13B H 0.2243 1.129 0.0436 0.058 Uiso 1 1 calc R . . H13C H 0.2896 1.0855 0.0334 0.058 Uiso 1 1 calc R . . C14 C 0.3297(3) 0.9371(5) 0.1103(2) 0.0350(13) Uani 1 1 d . . . H14A H 0.3571 0.9856 0.1381 0.053 Uiso 1 1 calc R . . H14B H 0.3506 0.9272 0.083 0.053 Uiso 1 1 calc R . . H14C H 0.3258 0.8671 0.1262 0.053 Uiso 1 1 calc R . . C15 C 0.2290(3) 1.0102(4) 0.1272(2) 0.0270(11) Uani 1 1 d . . . H15A H 0.2531 1.071 0.1495 0.032 Uiso 1 1 calc R . . H15B H 0.1823 1.0332 0.1095 0.032 Uiso 1 1 calc R . . C16 C 0.2762(3) 0.9316(6) 0.2145(2) 0.0383(15) Uani 1 1 d . . . H16A H 0.2748 0.8674 0.2356 0.057 Uiso 1 1 calc R . . H16B H 0.2642 0.9953 0.2311 0.057 Uiso 1 1 calc R . . H16C H 0.3212 0.9405 0.2131 0.057 Uiso 1 1 calc R . . C17 C 0.1255(3) 0.4980(4) 0.0567(2) 0.0230(11) Uani 1 1 d . . . C18 C 0.0901(3) 0.4507(5) 0.0077(2) 0.0283(12) Uani 1 1 d . . . H18 H 0.0844 0.376 -0.0005 0.034 Uiso 1 1 calc R . . C19 C 0.0657(3) 0.5357(4) -0.0260(2) 0.0251(11) Uani 1 1 d . . . H19 H 0.0394 0.5302 -0.0625 0.03 Uiso 1 1 calc R . . C20 C 0.1624(3) 0.4422(4) 0.1090(2) 0.0290(12) Uani 1 1 d . . . C21 C 0.1754(4) 0.3244(6) 0.0975(3) 0.060(2) Uani 1 1 d . . . H21A H 0.1992 0.2877 0.1311 0.09 Uiso 1 1 calc R . . H21B H 0.2023 0.3225 0.0741 0.09 Uiso 1 1 calc R . . H21C H 0.1329 0.288 0.08 0.09 Uiso 1 1 calc R . . C22 C 0.1212(4) 0.4461(6) 0.1462(3) 0.0452(17) Uani 1 1 d . . . H22A H 0.1455 0.41 0.1799 0.068 Uiso 1 1 calc R . . H22B H 0.0787 0.4092 0.1293 0.068 Uiso 1 1 calc R . . H22C H 0.1129 0.5214 0.1532 0.068 Uiso 1 1 calc R . . C23 C 0.2314(3) 0.4903(4) 0.1358(2) 0.0291(12) Uani 1 1 d . . . H23A H 0.2564 0.4435 0.166 0.035 Uiso 1 1 calc R . . H23B H 0.2556 0.491 0.1099 0.035 Uiso 1 1 calc R . . C24 C 0.2945(3) 0.6333(6) 0.1852(3) 0.0478(18) Uani 1 1 d . . . H24A H 0.2921 0.7065 0.1983 0.072 Uiso 1 1 calc R . . H24B H 0.3225 0.6334 0.1626 0.072 Uiso 1 1 calc R . . H24C H 0.3138 0.5847 0.2155 0.072 Uiso 1 1 calc R . . B B 0.0710(3) 0.7453(5) -0.0210(2) 0.0210(11) Uani 1 1 d . . . H0 H 0.0527 0.7419 -0.0608 0.025 Uiso 1 1 calc R . . Ba Ba 0.136646(15) 0.76284(2) 0.129960(11) 0.01871(9) Uani 1 1 d . . . I I 0.15714(2) 0.73892(3) 0.263496(14) 0.03194(11) Uani 1 1 d . . . N1 N 0.0183(2) 0.7980(4) -0.00089(16) 0.0226(9) Uani 1 1 d . . . N2 N 0.0153(2) 0.7816(4) 0.04925(16) 0.0229(9) Uani 1 1 d . . . N3 N 0.1355(2) 0.8118(4) -0.00478(16) 0.0214(9) Uani 1 1 d . . . N4 N 0.1633(2) 0.8630(3) 0.04340(16) 0.0217(9) Uani 1 1 d . . . N5 N 0.0849(2) 0.6279(4) 0.00090(16) 0.0224(9) Uani 1 1 d . . . N6 N 0.1222(2) 0.6057(4) 0.05267(16) 0.0240(9) Uani 1 1 d . . . O1 O 0.0544(2) 0.9264(3) 0.14837(16) 0.0310(9) Uani 1 1 d . . . O2 O 0.2299(2) 0.9190(3) 0.16126(15) 0.0296(9) Uani 1 1 d . . . O3 O 0.2296(2) 0.5974(3) 0.15505(16) 0.0324(9) Uani 1 1 d . . . C1A C 0 0.4082(9) 0.25 0.050(3) Uani 1 2 d S . . C2A C -0.0155(4) 0.3494(8) 0.2030(3) 0.053(2) Uani 1 1 d . . . H2A H -0.026 0.3866 0.17 0.063 Uiso 1 1 calc R . . C3A C -0.0160(4) 0.2379(8) 0.2033(3) 0.058(2) Uani 1 1 d . . . H3A H -0.0275 0.1987 0.1708 0.07 Uiso 1 1 calc R . . C4A C 0 0.1860(9) 0.25 0.060(3) Uani 1 2 d S . . H4A H 0 0.1094 0.25 0.072 Uiso 1 2 calc SR . . C5A C 0 0.5273(12) 0.25 0.111(7) Uani 1 2 d S . . H5A1 H -0.012 0.5536 0.2133 0.167 Uiso 0.5 1 calc PR . . H5A2 H 0.0444 0.5536 0.2708 0.167 Uiso 0.5 1 calc PR . . H5A3 H -0.0324 0.5536 0.2659 0.167 Uiso 0.5 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.018(3) 0.020(3) 0.030(3) -0.001(2) 0.006(2) 0.000(2) C2 0.024(3) 0.023(3) 0.037(3) 0.006(2) 0.007(2) 0.004(2) C3 0.027(3) 0.030(3) 0.025(3) 0.008(2) 0.003(2) 0.000(2) C4 0.022(3) 0.024(3) 0.034(3) 0.000(2) 0.012(2) 0.003(2) C5 0.028(3) 0.030(3) 0.034(3) 0.004(2) 0.015(2) 0.004(2) C6 0.026(3) 0.037(4) 0.046(4) 0.007(3) 0.015(3) 0.007(3) C7 0.030(3) 0.028(3) 0.040(3) -0.007(2) 0.015(3) 0.007(2) C8 0.033(3) 0.036(4) 0.048(4) -0.021(3) 0.009(3) -0.001(3) C9 0.024(3) 0.019(3) 0.027(3) 0.0041(19) 0.010(2) 0.004(2) C10 0.029(3) 0.024(3) 0.037(3) 0.004(2) 0.019(2) 0.002(2) C11 0.034(3) 0.024(3) 0.025(3) 0.003(2) 0.013(2) 0.001(2) C12 0.022(3) 0.025(3) 0.031(3) 0.001(2) 0.009(2) -0.002(2) C13 0.047(4) 0.024(3) 0.046(4) 0.000(2) 0.017(3) -0.006(3) C14 0.022(3) 0.041(4) 0.041(3) -0.003(3) 0.009(2) 0.002(3) C15 0.026(3) 0.021(3) 0.033(3) -0.004(2) 0.008(2) -0.003(2) C16 0.041(4) 0.044(4) 0.025(3) -0.005(2) 0.004(3) -0.014(3) C17 0.024(3) 0.023(3) 0.023(3) -0.0027(19) 0.009(2) 0.000(2) C18 0.031(3) 0.024(3) 0.031(3) -0.006(2) 0.012(2) -0.003(2) C19 0.024(3) 0.029(3) 0.022(3) -0.007(2) 0.008(2) -0.003(2) C20 0.028(3) 0.019(3) 0.033(3) 0.001(2) 0.001(2) 0.002(2) C21 0.066(5) 0.025(4) 0.061(5) -0.002(3) -0.014(4) 0.013(3) C22 0.039(4) 0.057(4) 0.034(3) 0.015(3) 0.005(3) -0.016(3) C23 0.026(3) 0.023(3) 0.035(3) 0.000(2) 0.006(2) 0.011(2) C24 0.031(4) 0.040(4) 0.054(4) 0.000(3) -0.009(3) -0.002(3) B 0.022(3) 0.024(3) 0.015(2) -0.002(2) 0.003(2) -0.011(2) Ba 0.01881(15) 0.01918(16) 0.01731(15) -0.00161(10) 0.00494(10) 0.00086(12) I 0.0390(2) 0.0348(2) 0.02148(19) 0.00069(14) 0.00945(15) -0.00172(16) N1 0.021(2) 0.023(2) 0.022(2) 0.0025(16) 0.0039(17) -0.0010(18) N2 0.022(2) 0.025(2) 0.019(2) -0.0013(16) 0.0041(17) 0.0022(18) N3 0.025(2) 0.021(2) 0.020(2) -0.0001(16) 0.0083(17) 0.0020(18) N4 0.024(2) 0.020(2) 0.021(2) -0.0009(16) 0.0066(17) -0.0008(18) N5 0.022(2) 0.026(2) 0.019(2) -0.0028(16) 0.0058(17) -0.0023(18) N6 0.028(2) 0.022(2) 0.019(2) -0.0014(16) 0.0046(18) 0.0036(18) O1 0.025(2) 0.031(2) 0.036(2) -0.0130(16) 0.0083(17) 0.0023(17) O2 0.031(2) 0.031(2) 0.025(2) -0.0049(15) 0.0080(16) -0.0102(17) O3 0.023(2) 0.028(2) 0.038(2) -0.0060(16) -0.0008(17) 0.0029(16) C1A 0.028(5) 0.039(6) 0.081(8) 0 0.018(5) 0 C2A 0.038(4) 0.071(6) 0.052(4) 0.020(4) 0.019(3) 0.014(4) C3A 0.044(5) 0.075(6) 0.064(5) -0.022(4) 0.030(4) -0.001(4) C4A 0.073(8) 0.036(6) 0.091(9) 0 0.053(7) 0 C5A 0.073(11) 0.042(8) 0.21(2) 0 0.029(12) 0 #----------------------------------------------------------------------------# # 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 C1 N2 1.333(7) . ? C1 C2 1.397(7) . ? C1 C4 1.517(8) . ? C2 C3 1.375(8) . ? C2 H2 0.95 . ? C3 N1 1.346(7) . ? C3 H3 0.95 . ? C4 C7 1.529(8) . ? C4 C6 1.532(8) . ? C4 C5 1.535(8) . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 O1 1.433(7) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 O1 1.422(7) . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 N4 1.341(7) . ? C9 C10 1.399(7) . ? C9 C12 1.513(8) . ? C10 C11 1.373(8) . ? C10 H10 0.95 . ? C11 N3 1.341(7) . ? C11 H11 0.95 . ? C12 C15 1.519(8) . ? C12 C14 1.536(8) . ? C12 C13 1.544(8) . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 O2 1.445(7) . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 O2 1.440(7) . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 N6 1.338(7) . ? C17 C18 1.400(7) . ? C17 C20 1.517(7) . ? C18 C19 1.367(8) . ? C18 H18 0.95 . ? C19 N5 1.336(7) . ? C19 H19 0.95 . ? C20 C23 1.524(8) . ? C20 C22 1.530(9) . ? C20 C21 1.535(9) . ? 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 O3 1.427(7) . ? C23 H23A 0.99 . ? C23 H23B 0.99 . ? C24 O3 1.420(7) . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? B N3 1.537(7) . ? B N1 1.542(8) . ? B N5 1.558(7) . ? B H0 1 . ? Ba O2 2.699(4) . ? Ba N2 2.766(4) . ? Ba N6 2.774(4) . ? Ba O3 2.775(4) . ? Ba O1 2.830(4) . ? Ba N4 2.837(4) . ? Ba I 3.4451(4) . ? N1 N2 1.373(6) . ? N3 N4 1.375(6) . ? N5 N6 1.369(6) . ? C1A C2A 1.388(10) 2 ? C1A C2A 1.388(10) . ? C1A C5A 1.475(18) . ? C2A C3A 1.381(13) . ? C2A H2A 0.95 . ? C3A C4A 1.339(11) . ? C3A H3A 0.95 . ? C4A C3A 1.339(11) 2 ? C4A H4A 0.95 . ? C5A H5A1 0.98 . ? C5A H5A2 0.98 . ? C5A H5A3 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 N2 C1 C2 110.9(5) . . ? N2 C1 C4 120.5(5) . . ? C2 C1 C4 128.6(5) . . ? C3 C2 C1 104.5(5) . . ? C3 C2 H2 127.7 . . ? C1 C2 H2 127.7 . . ? N1 C3 C2 108.9(5) . . ? N1 C3 H3 125.5 . . ? C2 C3 H3 125.5 . . ? C1 C4 C7 109.3(5) . . ? C1 C4 C6 110.3(5) . . ? C7 C4 C6 106.9(5) . . ? C1 C4 C5 111.7(4) . . ? C7 C4 C5 110.0(5) . . ? C6 C4 C5 108.6(5) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O1 C7 C4 111.2(4) . . ? O1 C7 H7A 109.4 . . ? C4 C7 H7A 109.4 . . ? O1 C7 H7B 109.4 . . ? C4 C7 H7B 109.4 . . ? H7A C7 H7B 108 . . ? O1 C8 H8A 109.5 . . ? O1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N4 C9 C10 110.3(5) . . ? N4 C9 C12 122.9(5) . . ? C10 C9 C12 126.6(5) . . ? C11 C10 C9 104.8(5) . . ? C11 C10 H10 127.6 . . ? C9 C10 H10 127.6 . . ? N3 C11 C10 109.2(5) . . ? N3 C11 H11 125.4 . . ? C10 C11 H11 125.4 . . ? C9 C12 C15 113.0(5) . . ? C9 C12 C14 110.3(5) . . ? C15 C12 C14 110.4(5) . . ? C9 C12 C13 108.6(5) . . ? C15 C12 C13 106.2(5) . . ? C14 C12 C13 108.1(5) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 C15 C12 113.4(4) . . ? O2 C15 H15A 108.9 . . ? C12 C15 H15A 108.9 . . ? O2 C15 H15B 108.9 . . ? C12 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? O2 C16 H16A 109.5 . . ? O2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N6 C17 C18 110.2(5) . . ? N6 C17 C20 121.7(5) . . ? C18 C17 C20 128.1(5) . . ? C19 C18 C17 104.8(5) . . ? C19 C18 H18 127.6 . . ? C17 C18 H18 127.6 . . ? N5 C19 C18 109.1(5) . . ? N5 C19 H19 125.4 . . ? C18 C19 H19 125.4 . . ? C17 C20 C23 112.0(5) . . ? C17 C20 C22 110.1(5) . . ? C23 C20 C22 111.1(5) . . ? C17 C20 C21 108.9(5) . . ? C23 C20 C21 104.8(5) . . ? C22 C20 C21 109.8(6) . . ? 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 . . ? O3 C23 C20 113.2(4) . . ? O3 C23 H23A 108.9 . . ? C20 C23 H23A 108.9 . . ? O3 C23 H23B 108.9 . . ? C20 C23 H23B 108.9 . . ? H23A C23 H23B 107.8 . . ? O3 C24 H24A 109.5 . . ? O3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 B N1 111.3(4) . . ? N3 B N5 110.9(4) . . ? N1 B N5 109.6(4) . . ? N3 B H0 108.3 . . ? N1 B H0 108.3 . . ? N5 B H0 108.3 . . ? O2 Ba N2 125.53(13) . . ? O2 Ba N6 128.29(13) . . ? N2 Ba N6 68.93(13) . . ? O2 Ba O3 93.56(13) . . ? N2 Ba O3 131.08(12) . . ? N6 Ba O3 63.42(12) . . ? O2 Ba O1 82.47(12) . . ? N2 Ba O1 66.44(12) . . ? N6 Ba O1 135.23(12) . . ? O3 Ba O1 157.33(12) . . ? O2 Ba N4 67.01(12) . . ? N2 Ba N4 73.92(13) . . ? N6 Ba N4 73.01(13) . . ? O3 Ba N4 101.37(13) . . ? O1 Ba N4 97.59(12) . . ? O2 Ba I 85.27(8) . . ? N2 Ba I 124.79(9) . . ? N6 Ba I 130.45(9) . . ? O3 Ba I 81.65(9) . . ? O1 Ba I 75.80(8) . . ? N4 Ba I 152.20(9) . . ? C3 N1 N2 109.4(4) . . ? C3 N1 B 127.1(4) . . ? N2 N1 B 123.5(4) . . ? C1 N2 N1 106.2(4) . . ? C1 N2 Ba 125.0(3) . . ? N1 N2 Ba 115.5(3) . . ? C11 N3 N4 109.5(4) . . ? C11 N3 B 125.4(4) . . ? N4 N3 B 125.1(4) . . ? C9 N4 N3 106.2(4) . . ? C9 N4 Ba 131.2(3) . . ? N3 N4 Ba 114.5(3) . . ? C19 N5 N6 109.7(4) . . ? C19 N5 B 127.8(4) . . ? N6 N5 B 122.5(4) . . ? C17 N6 N5 106.2(4) . . ? C17 N6 Ba 130.5(3) . . ? N5 N6 Ba 119.2(3) . . ? C8 O1 C7 110.9(4) . . ? C8 O1 Ba 113.6(3) . . ? C7 O1 Ba 133.4(3) . . ? C16 O2 C15 113.2(4) . . ? C16 O2 Ba 125.0(3) . . ? C15 O2 Ba 120.9(3) . . ? C24 O3 C23 110.8(5) . . ? C24 O3 Ba 112.8(4) . . ? C23 O3 Ba 134.7(3) . . ? C2A C1A C2A 116.6(11) 2 . ? C2A C1A C5A 121.7(5) 2 . ? C2A C1A C5A 121.7(5) . . ? C3A C2A C1A 121.4(8) . . ? C3A C2A H2A 119.3 . . ? C1A C2A H2A 119.3 . . ? C4A C3A C2A 119.0(8) . . ? C4A C3A H3A 120.5 . . ? C2A C3A H3A 120.5 . . ? C3A C4A C3A 122.6(12) 2 . ? C3A C4A H4A 118.7 2 . ? C3A C4A H4A 118.7 . . ? C1A C5A H5A1 109.5 . . ? C1A C5A H5A2 109.5 . . ? H5A1 C5A H5A2 109.5 . . ? C1A C5A H5A3 109.5 . . ? H5A1 C5A H5A3 109.5 . . ? H5A2 C5A H5A3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C1 C2 C3 -0.3(6) . . . . ? C4 C1 C2 C3 178.9(5) . . . . ? C1 C2 C3 N1 0.5(6) . . . . ? N2 C1 C4 C7 90.4(6) . . . . ? C2 C1 C4 C7 -88.8(7) . . . . ? N2 C1 C4 C6 -152.5(5) . . . . ? C2 C1 C4 C6 28.4(8) . . . . ? N2 C1 C4 C5 -31.6(7) . . . . ? C2 C1 C4 C5 149.2(6) . . . . ? C1 C4 C7 O1 -54.5(6) . . . . ? C6 C4 C7 O1 -173.8(5) . . . . ? C5 C4 C7 O1 68.5(6) . . . . ? N4 C9 C10 C11 1.3(6) . . . . ? C12 C9 C10 C11 -175.7(5) . . . . ? C9 C10 C11 N3 -0.8(6) . . . . ? N4 C9 C12 C15 -9.7(7) . . . . ? C10 C9 C12 C15 166.9(5) . . . . ? N4 C9 C12 C14 114.5(6) . . . . ? C10 C9 C12 C14 -69.0(7) . . . . ? N4 C9 C12 C13 -127.2(6) . . . . ? C10 C9 C12 C13 49.3(7) . . . . ? C9 C12 C15 O2 72.4(6) . . . . ? C14 C12 C15 O2 -51.6(6) . . . . ? C13 C12 C15 O2 -168.5(5) . . . . ? N6 C17 C18 C19 0.1(6) . . . . ? C20 C17 C18 C19 179.2(6) . . . . ? C17 C18 C19 N5 -0.1(6) . . . . ? N6 C17 C20 C23 -47.5(7) . . . . ? C18 C17 C20 C23 133.5(6) . . . . ? N6 C17 C20 C22 76.6(7) . . . . ? C18 C17 C20 C22 -102.3(7) . . . . ? N6 C17 C20 C21 -162.9(6) . . . . ? C18 C17 C20 C21 18.1(9) . . . . ? C17 C20 C23 O3 68.6(6) . . . . ? C22 C20 C23 O3 -54.9(7) . . . . ? C21 C20 C23 O3 -173.5(5) . . . . ? C2 C3 N1 N2 -0.5(6) . . . . ? C2 C3 N1 B -179.8(5) . . . . ? N3 B N1 C3 93.8(6) . . . . ? N5 B N1 C3 -143.2(5) . . . . ? N3 B N1 N2 -85.3(6) . . . . ? N5 B N1 N2 37.7(6) . . . . ? C2 C1 N2 N1 0.0(6) . . . . ? C4 C1 N2 N1 -179.3(5) . . . . ? C2 C1 N2 Ba 138.6(4) . . . . ? C4 C1 N2 Ba -40.7(7) . . . . ? C3 N1 N2 C1 0.3(6) . . . . ? B N1 N2 C1 179.6(5) . . . . ? C3 N1 N2 Ba -142.8(4) . . . . ? B N1 N2 Ba 36.5(6) . . . . ? O2 Ba N2 C1 -71.6(4) . . . . ? N6 Ba N2 C1 165.6(5) . . . . ? O3 Ba N2 C1 152.0(4) . . . . ? O1 Ba N2 C1 -10.8(4) . . . . ? N4 Ba N2 C1 -116.8(4) . . . . ? I Ba N2 C1 40.2(5) . . . . ? O2 Ba N2 N1 63.6(4) . . . . ? N6 Ba N2 N1 -59.1(3) . . . . ? O3 Ba N2 N1 -72.7(4) . . . . ? O1 Ba N2 N1 124.5(4) . . . . ? N4 Ba N2 N1 18.5(3) . . . . ? I Ba N2 N1 175.5(3) . . . . ? C10 C11 N3 N4 0.0(6) . . . . ? C10 C11 N3 B 179.2(5) . . . . ? N1 B N3 C11 -139.9(5) . . . . ? N5 B N3 C11 97.8(6) . . . . ? N1 B N3 N4 39.1(7) . . . . ? N5 B N3 N4 -83.2(6) . . . . ? C10 C9 N4 N3 -1.3(6) . . . . ? C12 C9 N4 N3 175.8(5) . . . . ? C10 C9 N4 Ba 144.6(4) . . . . ? C12 C9 N4 Ba -38.3(7) . . . . ? C11 N3 N4 C9 0.8(6) . . . . ? B N3 N4 C9 -178.4(5) . . . . ? C11 N3 N4 Ba -151.6(3) . . . . ? B N3 N4 Ba 29.2(6) . . . . ? O2 Ba N4 C9 25.8(4) . . . . ? N2 Ba N4 C9 167.0(5) . . . . ? N6 Ba N4 C9 -120.7(5) . . . . ? O3 Ba N4 C9 -63.3(5) . . . . ? O1 Ba N4 C9 104.2(4) . . . . ? I Ba N4 C9 30.4(6) . . . . ? O2 Ba N4 N3 169.5(4) . . . . ? N2 Ba N4 N3 -49.3(3) . . . . ? N6 Ba N4 N3 23.0(3) . . . . ? O3 Ba N4 N3 80.4(3) . . . . ? O1 Ba N4 N3 -112.1(3) . . . . ? I Ba N4 N3 174.1(2) . . . . ? C18 C19 N5 N6 0.0(6) . . . . ? C18 C19 N5 B 177.9(5) . . . . ? N3 B N5 C19 -130.0(5) . . . . ? N1 B N5 C19 106.7(6) . . . . ? N3 B N5 N6 47.7(6) . . . . ? N1 B N5 N6 -75.6(6) . . . . ? C18 C17 N6 N5 -0.1(6) . . . . ? C20 C17 N6 N5 -179.3(5) . . . . ? C18 C17 N6 Ba 156.4(4) . . . . ? C20 C17 N6 Ba -22.8(8) . . . . ? C19 N5 N6 C17 0.1(6) . . . . ? B N5 N6 C17 -178.0(5) . . . . ? C19 N5 N6 Ba -159.6(3) . . . . ? B N5 N6 Ba 22.4(6) . . . . ? O2 Ba N6 C17 117.3(5) . . . . ? N2 Ba N6 C17 -123.4(5) . . . . ? O3 Ba N6 C17 45.2(5) . . . . ? O1 Ba N6 C17 -118.7(5) . . . . ? N4 Ba N6 C17 157.7(5) . . . . ? I Ba N6 C17 -5.0(5) . . . . ? O2 Ba N6 N5 -88.7(4) . . . . ? N2 Ba N6 N5 30.6(3) . . . . ? O3 Ba N6 N5 -160.8(4) . . . . ? O1 Ba N6 N5 35.3(4) . . . . ? N4 Ba N6 N5 -48.3(4) . . . . ? I Ba N6 N5 149.0(3) . . . . ? C4 C7 O1 C8 -173.7(5) . . . . ? C4 C7 O1 Ba -11.6(7) . . . . ? O2 Ba O1 C8 -25.7(4) . . . . ? N2 Ba O1 C8 -159.9(4) . . . . ? N6 Ba O1 C8 -164.6(4) . . . . ? O3 Ba O1 C8 55.5(6) . . . . ? N4 Ba O1 C8 -91.1(4) . . . . ? I Ba O1 C8 61.3(4) . . . . ? O2 Ba O1 C7 172.6(5) . . . . ? N2 Ba O1 C7 38.4(5) . . . . ? N6 Ba O1 C7 33.6(5) . . . . ? O3 Ba O1 C7 -106.3(5) . . . . ? N4 Ba O1 C7 107.1(5) . . . . ? I Ba O1 C7 -100.4(5) . . . . ? C12 C15 O2 C16 108.5(6) . . . . ? C12 C15 O2 Ba -81.9(5) . . . . ? N2 Ba O2 C16 150.1(4) . . . . ? N6 Ba O2 C16 -119.8(4) . . . . ? O3 Ba O2 C16 -61.3(5) . . . . ? O1 Ba O2 C16 96.3(5) . . . . ? N4 Ba O2 C16 -162.1(5) . . . . ? I Ba O2 C16 20.0(4) . . . . ? N2 Ba O2 C15 -18.2(4) . . . . ? N6 Ba O2 C15 71.9(4) . . . . ? O3 Ba O2 C15 130.4(4) . . . . ? O1 Ba O2 C15 -72.0(4) . . . . ? N4 Ba O2 C15 29.5(4) . . . . ? I Ba O2 C15 -148.3(4) . . . . ? C20 C23 O3 C24 172.9(5) . . . . ? C20 C23 O3 Ba -23.2(7) . . . . ? O2 Ba O3 C24 11.4(4) . . . . ? N2 Ba O3 C24 157.1(4) . . . . ? N6 Ba O3 C24 142.9(5) . . . . ? O1 Ba O3 C24 -67.6(6) . . . . ? N4 Ba O3 C24 78.6(4) . . . . ? I Ba O3 C24 -73.3(4) . . . . ? O2 Ba O3 C23 -152.3(5) . . . . ? N2 Ba O3 C23 -6.6(6) . . . . ? N6 Ba O3 C23 -20.8(5) . . . . ? O1 Ba O3 C23 128.7(5) . . . . ? N4 Ba O3 C23 -85.1(5) . . . . ? I Ba O3 C23 123.0(5) . . . . ? C2A C1A C2A C3A 0.6(5) 2 . . . ? C5A C1A C2A C3A -179.4(5) . . . . ? C1A C2A C3A C4A -1.2(10) . . . . ? C2A C3A C4A C3A 0.6(5) . . . 2 ? #END OF CIF#\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2008-05-30 at 11:00:21 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : shelxl dreduc import struct data_Chisholm1604 _database_code_depnum_ccdc_archive 'CCDC 695437' _audit_creation_date 2008-05-30T11:00:21-00:00 _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_name_common 'Chisholm 1604' _chemical_formula_moiety 'C24 H40 B1 I1 N6 O3 Zn1' _chemical_formula_sum 'C24 H40 B I N6 O3 Zn' _chemical_formula_weight 663.7 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3 _symmetry_space_group_name_Hall '-R 3' _symmetry_Int_Tables_number 148 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 12.08910(10) _cell_length_b 12.08910(10) _cell_length_c 34.8231(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 4407.43(8) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2263 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description chunk _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.5 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2028 _exptl_special_details ;Examination of the diffraction pattern on a Nonius Kappa CCD diffractometer indicated a trigonal (rhombohedral) crystal system. All work was done at 150K using an Oxford Cryosystems Cryostream Cooler. Phi and omega scans with a frame width of 1.0 degree were used for data collection. Data integration was done with Denzo and scaling and merging of the data was done with Scalepack. The Zn(Tp)*I complex contains a crystallographic three-fold rotation axis, which passes through the Zn, I and B atoms. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.921 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.767 _exptl_absorpt_correction_T_max 0.858 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor, 1997)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.37708E-1 _diffrn_orient_matrix_ub_12 0.46557E-2 _diffrn_orient_matrix_ub_13 -0.259195E-1 _diffrn_orient_matrix_ub_21 0.870792E-1 _diffrn_orient_matrix_ub_22 0.395086E-1 _diffrn_orient_matrix_ub_23 0.117169E-1 _diffrn_orient_matrix_ub_31 -0.108906E-1 _diffrn_orient_matrix_ub_32 -0.86837E-1 _diffrn_orient_matrix_ub_33 0.39412E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_av_unetI/netI ? _diffrn_reflns_number 19579 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 2265 _reflns_number_gt 1858 _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 ;For the methyl groups, the hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5*Ueq(bonded carbon atom). The torsion angle, which defines the orientation of the methyl group about the O-C or C-C bond, was refined. The remaining hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(attached atom). Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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 'w=1/[\s^2^(Fo^2^)+(0.0259P)^2^+26.5815P] 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 2265 _refine_ls_number_parameters 112 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0757 _refine_ls_goodness_of_fit_ref 1.07 _refine_ls_restrained_S_all 1.07 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.255 _refine_diff_density_min -1.048 _refine_diff_density_rms 0.09 #----------------------------------------------------------------------------# # 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9042(3) 0.3001(3) 0.04738(9) 0.0170(6) Uani 1 1 d . . . C2 C 0.9621(3) 0.3201(3) 0.01133(9) 0.0222(6) Uani 1 1 d . . . H2 H 1.0386 0.3199 0.0052 0.027 Uiso 1 1 calc R . . C3 C 0.8847(3) 0.3400(3) -0.01341(9) 0.0211(6) Uani 1 1 d . . . H3 H 0.8992 0.3567 -0.0401 0.025 Uiso 1 1 calc R . . C4 C 0.9453(3) 0.2695(3) 0.08494(9) 0.0221(6) Uani 1 1 d . . . C5 C 0.8324(3) 0.1504(3) 0.10308(11) 0.0288(7) Uani 1 1 d . . . H5A H 0.7642 0.1688 0.1094 0.043 Uiso 1 1 calc R . . H5B H 0.861 0.1274 0.1265 0.043 Uiso 1 1 calc R . . H5C H 0.8001 0.0792 0.0848 0.043 Uiso 1 1 calc R . . C6 C 1.0540(3) 0.2410(4) 0.07822(11) 0.0342(8) Uani 1 1 d . . . H6A H 1.0253 0.1689 0.0604 0.051 Uiso 1 1 calc R . . H6B H 1.0785 0.2194 0.1027 0.051 Uiso 1 1 calc R . . H6C H 1.1277 0.3164 0.0672 0.051 Uiso 1 1 calc R . . C7 C 0.9899(3) 0.3812(3) 0.11290(9) 0.0266(7) Uani 1 1 d . . . H7A H 0.9191 0.3982 0.1179 0.032 Uiso 1 1 calc R . . H7B H 1.0146 0.3592 0.1376 0.032 Uiso 1 1 calc R . . C8 C 1.1280(3) 0.6007(3) 0.12011(10) 0.0326(8) Uani 1 1 d . . . H8A H 1.0558 0.6161 0.1209 0.049 Uiso 1 1 calc R . . H8B H 1.2025 0.6752 0.109 0.049 Uiso 1 1 calc R . . H8C H 1.1483 0.5863 0.1462 0.049 Uiso 1 1 calc R . . N1 N 0.7859(2) 0.3320(2) 0.00626(7) 0.0171(5) Uani 1 1 d . . . N2 N 0.7967(2) 0.3080(2) 0.04431(7) 0.0167(5) Uani 1 1 d . . . O O 1.0955(2) 0.4917(2) 0.09730(7) 0.0307(5) Uani 1 1 d . . . B B 0.6667 0.3333 -0.00890(17) 0.0180(11) Uani 1 3 d S . . H0 H 0.6667 0.3333 -0.0376 0.022 Uiso 1 3 calc SR . . Zn Zn 0.6667 0.3333 0.075831(16) 0.01499(14) Uani 1 3 d S . . I I 0.6667 0.3333 0.149367(10) 0.02720(12) Uani 1 3 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0130(13) 0.0103(13) 0.0257(16) -0.0019(11) -0.0001(11) 0.0043(11) C2 0.0162(14) 0.0220(15) 0.0293(17) -0.0015(13) 0.0047(12) 0.0102(13) C3 0.0203(15) 0.0160(14) 0.0239(16) -0.0008(12) 0.0054(12) 0.0067(12) C4 0.0175(15) 0.0221(15) 0.0276(17) 0.0046(13) 0.0008(12) 0.0104(13) C5 0.0275(17) 0.0212(16) 0.039(2) 0.0075(14) 0.0015(14) 0.0134(14) C6 0.0271(18) 0.039(2) 0.045(2) 0.0077(17) 0.0013(16) 0.0227(16) C7 0.0202(16) 0.0296(18) 0.0251(17) 0.0019(14) -0.0020(13) 0.0089(14) C8 0.0327(19) 0.0281(18) 0.0332(19) -0.0024(15) -0.0076(15) 0.0124(15) N1 0.0176(12) 0.0153(12) 0.0187(12) -0.0004(10) 0.0015(10) 0.0084(10) N2 0.0158(12) 0.0164(12) 0.0183(12) -0.0001(10) -0.0001(10) 0.0084(10) O 0.0202(11) 0.0268(12) 0.0335(13) -0.0044(10) 0.0003(10) 0.0030(10) B 0.0195(17) 0.0195(17) 0.015(3) 0 0 0.0097(9) Zn 0.01395(19) 0.01395(19) 0.0171(3) 0 0 0.00698(9) I 0.03065(15) 0.03065(15) 0.02029(19) 0 0 0.01532(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 C1 N2 1.355(4) . ? C1 C2 1.398(4) . ? C1 C4 1.510(4) . ? C2 C3 1.379(4) . ? C2 H2 0.95 . ? C3 N1 1.338(4) . ? C3 H3 0.95 . ? C4 C7 1.528(5) . ? C4 C6 1.533(4) . ? C4 C5 1.539(4) . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 O 1.416(4) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 O 1.415(4) . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? N1 N2 1.377(3) . ? N1 B 1.542(3) . ? N2 Zn 2.062(2) . ? B H0 1 . ? Zn I 2.5607(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 C2 109.4(3) . . ? N2 C1 C4 122.1(3) . . ? C2 C1 C4 128.5(3) . . ? C3 C2 C1 105.5(3) . . ? C3 C2 H2 127.3 . . ? C1 C2 H2 127.3 . . ? N1 C3 C2 109.1(3) . . ? N1 C3 H3 125.5 . . ? C2 C3 H3 125.5 . . ? C1 C4 C7 110.4(3) . . ? C1 C4 C6 110.3(3) . . ? C7 C4 C6 109.5(3) . . ? C1 C4 C5 109.8(2) . . ? C7 C4 C5 108.7(3) . . ? C6 C4 C5 108.1(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O C7 C4 110.0(3) . . ? O C7 H7A 109.7 . . ? C4 C7 H7A 109.7 . . ? O C7 H7B 109.7 . . ? C4 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? O C8 H8A 109.5 . . ? O C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C3 N1 N2 109.4(2) . . ? C3 N1 B 129.0(3) . . ? N2 N1 B 121.3(3) . . ? C1 N2 N1 106.6(2) . . ? C1 N2 Zn 143.0(2) . . ? N1 N2 Zn 108.75(17) . . ? C8 O C7 111.3(3) . . ? N1 B N1 108.9(2) . 3_665 ? N1 B H0 110 . . ? N2 Zn N2 94.30(9) . 3_665 ? N2 Zn I 122.16(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C1 C2 C3 -0.1(3) . . . . ? C4 C1 C2 C3 177.8(3) . . . . ? C1 C2 C3 N1 -0.3(3) . . . . ? N2 C1 C4 C7 -70.0(3) . . . . ? C2 C1 C4 C7 112.2(3) . . . . ? N2 C1 C4 C6 168.9(3) . . . . ? C2 C1 C4 C6 -8.9(4) . . . . ? N2 C1 C4 C5 49.8(4) . . . . ? C2 C1 C4 C5 -127.9(3) . . . . ? C1 C4 C7 O -60.7(3) . . . . ? C6 C4 C7 O 60.9(3) . . . . ? C5 C4 C7 O 178.9(2) . . . . ? C2 C3 N1 N2 0.6(3) . . . . ? C2 C3 N1 B -173.1(2) . . . . ? C2 C1 N2 N1 0.5(3) . . . . ? C4 C1 N2 N1 -177.6(2) . . . . ? C2 C1 N2 Zn -162.0(2) . . . . ? C4 C1 N2 Zn 19.9(5) . . . . ? C3 N1 N2 C1 -0.7(3) . . . . ? B N1 N2 C1 173.6(2) . . . . ? C3 N1 N2 Zn 168.30(18) . . . . ? B N1 N2 Zn -17.5(3) . . . . ? C4 C7 O C8 172.1(3) . . . . ? C3 N1 B N1 125.9(4) . . . 3_665 ? N2 N1 B N1 -47.2(4) . . . 3_665 ? C3 N1 B N1 -115.4(4) . . . 2_655 ? N2 N1 B N1 71.5(3) . . . 2_655 ? C1 N2 Zn N2 -141.3(3) . . . 3_665 ? N1 N2 Zn N2 56.43(14) . . . 3_665 ? C1 N2 Zn N2 124.0(4) . . . 2_655 ? N1 N2 Zn N2 -38.21(15) . . . 2_655 ? C1 N2 Zn I -8.6(3) . . . . ? N1 N2 Zn I -170.89(13) . . . . ? #END OF CIF#\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2008-05-30 at 15:08:58 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : shelxl dreduc import struct data_Chisholm1614 _database_code_depnum_ccdc_archive 'CCDC 695438' _audit_creation_date 2008-05-30T15:08:58-00:00 _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_name_common 'Chisholm 1614' _chemical_formula_moiety 'C27 H49 B1 N6 O4 Si1 Zn1' _chemical_formula_sum 'C27 H49 B N6 O4 Si Zn' _chemical_formula_weight 625.99 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R3 _symmetry_space_group_name_Hall 'R 3' _symmetry_Int_Tables_number 146 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 16.0519(4) _cell_length_b 16.0519(4) _cell_length_c 11.0188(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 2458.77(10) _cell_formula_units_Z 3 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1255 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description 'rectangular-shaped wedge' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.23 _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1002 _exptl_special_details ;Examination of the diffraction pattern on a Nonius Kappa CCD diffractometer indicated a trigonal crystal system. All work was done at 150K using an Oxford Cryosystems Cryostream Cooler. Phi and omega scans with a frame width of 2.0 degrees were used for data collection. Data integration was done with Denzo and scaling and merging of the data was done with Scalepack. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.825 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.726 _exptl_absorpt_correction_T_max 0.827 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor, 1997)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.70645E-1 _diffrn_orient_matrix_ub_12 -0.464233E-1 _diffrn_orient_matrix_ub_13 -0.55985E-2 _diffrn_orient_matrix_ub_21 0.2412E-2 _diffrn_orient_matrix_ub_22 0.109816E-1 _diffrn_orient_matrix_ub_23 -0.89578E-1 _diffrn_orient_matrix_ub_31 0.133484E-1 _diffrn_orient_matrix_ub_32 -0.538422E-1 _diffrn_orient_matrix_ub_33 -0.134432E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method "phi and omega scans'" _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_av_unetI/netI ? _diffrn_reflns_number 11122 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 2498 _reflns_number_gt 2456 _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 ;Initially, the Laue group appeared to be -3m, based on the R(int) value for averaging in this group and the fact that the axial photos for the a and b axes exhibit mirror planes. With Z=3, the only possible space group is R3m (No. 160), which would require the molecule to have 3m symmetry. While 3m symmetry is possible, it is not likely because it is too restrictive. We tried to develop a model in this space group, but there appeared to be lots of disorder for the tail portion of the Tp* ligand and for the trimethylsilyl group. We next decided to try the R3 space group, which would require the molecule to only have a threefold rotation axis. The same disorder as seen in R3m is also observed in R3. The isotropic refinement converged to R1=0.1069 for I > 2*sigma(I). Application of the twin law: (1 0 0/-1 -1 0/0 0 -1) resulted in the R factor dropping to 0.046 and the large peaks in the difference map, which looked like disorder, have disappeared. This is a case of merohedral twinning, which makes the true -3 Laue group look like -3m. After anisotropic refinement with all of the hydrogen atoms included in the model, the following TWIN 1 0 0 -1 -1 0 0 0 -1 -4 command was applied and resulted in the BASF parameters as follows: 0.0052, 0.00001, and 0.4808. The first BASF value (0.0052) indicates that the component present from application of the original twin law is now essentially zero, the second BASF value indicates that the Flack parameter is zero so that this is the correct enantiomer, and the third BASF value (0.4808) indicates that the component due to the inversion of the original twin law is present: (-1 0 0/1 1 0/0 0 1) and this is now the twin law used for the final cycles of refinement. The final value of this twin component is 0.489(1). The Zn, B, O(2) and Si atoms lie on the crystallographic three-fold rotation axis. For each methyl group, the hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5*Ueq(bonded carbon atom). The torsion angle, which defines the orientation of the methyl group about the Si-C or O-C bond, was refined. The remaining hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(attached atom). Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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 'w=1/[\s^2^(Fo^2^)+(0.0194P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2498 _refine_ls_number_parameters 124 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0211 _refine_ls_R_factor_gt 0.0201 _refine_ls_wR_factor_ref 0.0427 _refine_ls_wR_factor_gt 0.0424 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.05 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.004(7) _refine_diff_density_max 0.152 _refine_diff_density_min -0.21 _refine_diff_density_rms 0.034 #----------------------------------------------------------------------------# # 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' B B 0.0013 0.0007 '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' Zn Zn 0.2839 1.4301 '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 Zn Zn 0 0 0.048497(5) 0.01322(8) Uani 1 3 d S . . Si Si 0 0 0.35964(7) 0.01722(18) Uani 1 3 d S . . O1 O -0.27200(12) -0.00061(12) 0.10689(13) 0.0284(4) Uani 1 1 d . . . O2 O 0 0 0.21490(17) 0.0203(4) Uani 1 3 d S . . N1 N -0.05414(19) 0.0503(2) -0.17397(10) 0.0148(3) Uani 1 1 d . . . N2 N -0.05806(19) 0.06637(19) -0.05226(12) 0.0143(3) Uani 1 1 d . . . C1 C -0.1068(2) 0.1142(2) -0.04119(14) 0.0157(3) Uani 1 1 d . . . C2 C -0.1320(3) 0.1302(3) -0.15652(14) 0.0199(3) Uani 1 1 d . . . H2 H -0.1659 0.163 -0.1756 0.024 Uiso 1 1 calc R . . C3 C -0.0980(2) 0.0888(2) -0.23672(14) 0.0183(4) Uani 1 1 d . . . H3 H -0.1044 0.0877 -0.3225 0.022 Uiso 1 1 calc R . . C4 C -0.12199(18) 0.14749(18) 0.08172(17) 0.0198(6) Uani 1 1 d . . . C5 C -0.17388(19) 0.20532(18) 0.0644(2) 0.0296(7) Uani 1 1 d . . . H5A H -0.1352 0.2608 0.0118 0.044 Uiso 1 1 calc R . . H5B H -0.1827 0.2278 0.1434 0.044 Uiso 1 1 calc R . . H5C H -0.2368 0.1642 0.0268 0.044 Uiso 1 1 calc R . . C6 C -0.02423(19) 0.2118(2) 0.1416(3) 0.0269(6) Uani 1 1 d . . . H6A H 0.0147 0.2675 0.0894 0.04 Uiso 1 1 calc R . . H6B H 0.009 0.1752 0.1533 0.04 Uiso 1 1 calc R . . H6C H -0.0338 0.2341 0.2204 0.04 Uiso 1 1 calc R . . C7 C -0.18211(18) 0.06168(19) 0.1633(2) 0.0217(6) Uani 1 1 d . . . H7A H -0.1473 0.0263 0.1788 0.026 Uiso 1 1 calc R . . H7B H -0.1931 0.0842 0.2422 0.026 Uiso 1 1 calc R . . C8 C -0.33467(17) -0.07542(17) 0.1861(2) 0.0318(5) Uani 1 1 d . . . H8A H -0.3059 -0.1147 0.2079 0.048 Uiso 1 1 calc R . . H8B H -0.3964 -0.1158 0.1454 0.048 Uiso 1 1 calc R . . H8C H -0.345 -0.0475 0.2597 0.048 Uiso 1 1 calc R . . C9 C -0.12169(16) -0.08763(17) 0.4226(2) 0.0299(6) Uani 1 1 d . . . H9A H -0.1712 -0.0811 0.3788 0.045 Uiso 1 1 calc R . . H9B H -0.124 -0.0742 0.5089 0.045 Uiso 1 1 calc R . . H9C H -0.1333 -0.1533 0.4131 0.045 Uiso 1 1 calc R . . B B 0 0 -0.2214(3) 0.0149(7) Uani 1 3 d S . . H0 H 0 0 -0.3122 0.018 Uiso 1 3 calc SR . . 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 Zn 0.01373(10) 0.01373(10) 0.01219(14) 0 0 0.00686(5) Si 0.0193(3) 0.0193(3) 0.0130(4) 0 0 0.00966(13) O1 0.0213(9) 0.0333(9) 0.0247(8) 0.0047(7) 0.0020(7) 0.0093(7) O2 0.0237(5) 0.0237(5) 0.0135(9) 0 0 0.0118(3) N1 0.0152(13) 0.0159(14) 0.0125(6) 0.0004(13) -0.0009(12) 0.0073(5) N2 0.0170(11) 0.0129(10) 0.0137(6) 0.0039(11) 0.0037(11) 0.0081(6) C1 0.0114(12) 0.0159(13) 0.0197(8) 0.0030(14) 0.0012(13) 0.0068(7) C2 0.0154(14) 0.0242(16) 0.0241(8) 0.0043(16) -0.0012(16) 0.0129(7) C3 0.0170(13) 0.0201(15) 0.0173(7) 0.0041(14) -0.0024(14) 0.0090(8) C4 0.0214(15) 0.0194(15) 0.0236(8) 0.0015(9) 0.0030(9) 0.0140(13) C5 0.0365(18) 0.0322(18) 0.0334(10) -0.0019(10) 0.0001(10) 0.0272(17) C6 0.0283(16) 0.0273(15) 0.0258(14) -0.0096(12) -0.0045(11) 0.0143(13) C7 0.0232(13) 0.0282(14) 0.0193(12) -0.0026(10) -0.0005(10) 0.0171(11) C8 0.0272(12) 0.0313(12) 0.0316(12) 0.0066(10) 0.0080(10) 0.0107(10) C9 0.0306(12) 0.0335(12) 0.0192(10) 0.0040(9) 0.0048(9) 0.0112(10) B 0.0136(9) 0.0136(9) 0.0175(15) 0 0 0.0068(5) #----------------------------------------------------------------------------# # 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 Zn O2 1.8336(19) . ? Zn N2 2.0565(12) . ? Si O2 1.595(2) . ? Si C9 1.878(2) . ? O1 C8 1.417(3) . ? O1 C7 1.423(3) . ? N1 C3 1.337(2) . ? N1 N2 1.3730(17) . ? N1 B 1.5437(16) . ? N2 C1 1.3470(19) . ? C1 C2 1.397(2) . ? C1 C4 1.520(2) . ? C2 C3 1.373(2) . ? C2 H2 0.95 . ? C3 H3 0.95 . ? C4 C7 1.519(4) . ? C4 C6 1.531(4) . ? C4 C5 1.538(3) . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.99 . ? C7 H7B 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 . ? B N1 1.5437(16) 3 ? B N1 1.5437(16) 2 ? B H0 1 . ? 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 Zn N2 122.68(4) . . ? N2 Zn N2 93.60(5) 2 . ? O2 Si C9 111.69(7) . . ? C9 Si C9 107.17(8) 3 . ? C8 O1 C7 111.54(17) . . ? Si O2 Zn 180 . . ? C3 N1 N2 109.53(12) . . ? C3 N1 B 129.07(14) . . ? N2 N1 B 121.30(14) . . ? C1 N2 N1 106.82(13) . . ? C1 N2 Zn 142.05(11) . . ? N1 N2 Zn 110.79(9) . . ? N2 C1 C2 109.12(14) . . ? N2 C1 C4 121.49(15) . . ? C2 C1 C4 129.28(14) . . ? C3 C2 C1 105.88(13) . . ? C3 C2 H2 127.1 . . ? C1 C2 H2 127.1 . . ? N1 C3 C2 108.64(13) . . ? N1 C3 H3 125.7 . . ? C2 C3 H3 125.7 . . ? C7 C4 C1 110.4(2) . . ? C7 C4 C6 109.2(2) . . ? C1 C4 C6 109.3(2) . . ? C7 C4 C5 109.31(19) . . ? C1 C4 C5 109.43(16) . . ? C6 C4 C5 109.1(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O1 C7 C4 109.86(19) . . ? O1 C7 H7A 109.7 . . ? C4 C7 H7A 109.7 . . ? O1 C7 H7B 109.7 . . ? C4 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? O1 C8 H8A 109.5 . . ? O1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si C9 H9A 109.5 . . ? Si C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 B N1 109.15(11) 3 . ? N1 B N1 109.15(11) 3 2 ? N1 B N1 109.15(11) . 2 ? N1 B H0 109.8 3 . ? N1 B H0 109.8 . . ? N1 B H0 109.8 2 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 N1 N2 C1 1.0(4) . . . . ? B N1 N2 C1 177.7(3) . . . . ? C3 N1 N2 Zn 176.0(2) . . . . ? B N1 N2 Zn -7.4(3) . . . . ? O2 Zn N2 C1 -4.1(5) . . . . ? N2 Zn N2 C1 129.0(5) 2 . . . ? N2 Zn N2 C1 -137.2(5) 3 . . . ? O2 Zn N2 N1 -176.13(17) . . . . ? N2 Zn N2 N1 -43.05(17) 2 . . . ? N2 Zn N2 N1 50.79(17) 3 . . . ? N1 N2 C1 C2 -1.2(4) . . . . ? Zn N2 C1 C2 -173.5(3) . . . . ? N1 N2 C1 C4 -177.7(3) . . . . ? Zn N2 C1 C4 10.0(6) . . . . ? N2 C1 C2 C3 1.0(4) . . . . ? C4 C1 C2 C3 177.1(3) . . . . ? N2 N1 C3 C2 -0.4(4) . . . . ? B N1 C3 C2 -176.8(3) . . . . ? C1 C2 C3 N1 -0.3(4) . . . . ? N2 C1 C4 C7 -63.3(4) . . . . ? C2 C1 C4 C7 121.0(4) . . . . ? N2 C1 C4 C6 56.8(4) . . . . ? C2 C1 C4 C6 -118.9(4) . . . . ? N2 C1 C4 C5 176.3(3) . . . . ? C2 C1 C4 C5 0.6(5) . . . . ? C8 O1 C7 C4 -172.94(18) . . . . ? C1 C4 C7 O1 -57.8(2) . . . . ? C6 C4 C7 O1 -178.0(2) . . . . ? C5 C4 C7 O1 62.7(2) . . . . ? C3 N1 B N1 121.4(4) . . . 3 ? N2 N1 B N1 -54.6(3) . . . 3 ? C3 N1 B N1 -119.4(4) . . . 2 ? N2 N1 B N1 64.7(3) . . . 2 ? #END OF CIF