# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_I _database_code_depnum_ccdc_archive 'CCDC 902693' #TrackingRef 'web_deposit_cif_file_0_AaronD.Sadow_1348401140.ToMZnOCHO.cif' _audit_creation_method 'APEX2 v2009.11-0' _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H30 B N3 O5 Zn' _chemical_formula_iupac ? _chemical_formula_weight 492.67 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.1030(5) _cell_length_b 13.3614(5) _cell_length_c 16.2115(7) _cell_angle_alpha 90 _cell_angle_beta 95.7950(10) _cell_angle_gamma 90 _cell_volume 2392.71(18) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 173.(2) _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 1.063 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; ; _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.92 _exptl_special_details ; A X-ray quality crystal was selected under ambient conditions and covered with PARATONE oil The crystal was mounted and centered in the X-ray beam by using a video camera.The crystal evaluation and data collection were performed on APEX-2 CCD diffractometer with the detector to crystal distance of 5cm. The initial cell constants were obtained from three series of OMEGA scans at different starting angles. Each series consisted of 30 frames collected at intervals of 0.3 in a 10 range about OMEGA with the exposure time of 10 seconds per frame. The obtained reflections were successfully indexed by an automated indexing routine built to APEX2 program package. The final cell constants were calculated from a set of strong reflections from the actual data collection. The data were collected using the full sphere routine by collecting four sets of frames with 0.3 scans in \w with an exposure time 10 sec per frame. This dataset was corrected for Lorentz and polarization effects. The absorption correction was based on a fit of a spherical harmonic function to the empirical transmission surface as sampled by multiple equivalent measurements using SADABS software. ; _diffrn_ambient_temperature 173.(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source ? _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ' BRUKER APEX2 CCD Diffractometer' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24027 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 28.31 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _refine_special_details ; The systematic absences in the diffraction data were consistent for the stated space group. The position of almost all non-hydrogen atoms were found by direct methods. The remaining atoms were located in an alternating series of least-squares cycles on difference Fourier maps. All non-hydrogen atoms were refined in full-matrix anisotropic approximation. All hydrogen atoms were placed in the structure factor calculation at idealized positions and were allowed to ride on the neighboring atoms with relative isotropic displacement coefficients. Final results were tested with CHECKCIF routine and all A-warnings (if any) were addressed on the very top of this file. ; _reflns_number_total 5942 _reflns_number_gt 4678 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.0765 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_number_reflns 5942 _refine_ls_number_parameters 295 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+0.7620P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.383 _refine_diff_density_min -0.297 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' _computing_data_collection 'APEX2 Suite (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT V7.66A (Bruker AXS, 2009)' _computing_data_reduction 'SAINT V7.66A (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XSHELL (Bruker AXS, 2007)' _computing_publication_material 'APEX2 Suite (Bruker AXS, 2009)' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn1 0.686734(17) 0.212435(14) 0.047205(12) 0.02105(6) Uani d . 1 . . B B1 0.95054(16) 0.21325(13) 0.11853(11) 0.0182(2) Uani d . 1 . . C C1 0.86073(17) 0.48790(12) 0.13513(12) 0.0315(4) Uani d . 1 . . H H1A 0.8949 0.5455 0.107 0.038 Uiso calc R 1 . . H H1B 0.8414 0.5094 0.1907 0.038 Uiso calc R 1 . . C C2 0.74699(17) 0.44784(12) 0.08362(11) 0.0254(4) Uani d . 1 . . C C3 0.7373(2) 0.48489(16) -0.00576(12) 0.0444(5) Uani d . 1 . . H H3A 0.8134 0.4714 -0.0295 0.067 Uiso calc R 1 . . H H3B 0.7215 0.557 -0.0069 0.067 Uiso calc R 1 . . H H3C 0.6709 0.45 -0.0383 0.067 Uiso calc R 1 . . C C4 0.63079(18) 0.46705(14) 0.12315(13) 0.0390(5) Uani d . 1 . . H H4A 0.5629 0.4348 0.09 0.059 Uiso calc R 1 . . H H4B 0.6162 0.5393 0.1255 0.059 Uiso calc R 1 . . H H4C 0.6383 0.4395 0.1795 0.059 Uiso calc R 1 . . C C5 0.88314(14) 0.32276(12) 0.11401(10) 0.0197(2) Uani d . 1 . . C C6 0.9654(2) 0.09499(14) -0.09692(11) 0.0349(5) Uani d . 1 . . H H6A 0.9769 0.0216 -0.0985 0.042 Uiso calc R 1 . . H H6B 1.0022 0.1253 -0.1441 0.042 Uiso calc R 1 . . C C7 0.83065(18) 0.12104(12) -0.10079(10) 0.0277(4) Uani d . 1 . . C C8 0.7937(2) 0.20224(16) -0.16450(12) 0.0429(5) Uani d . 1 . . H H8A 0.71 0.2226 -0.1594 0.064 Uiso calc R 1 . . H H8B 0.8 0.1761 -0.2204 0.064 Uiso calc R 1 . . H H8C 0.8475 0.2601 -0.1546 0.064 Uiso calc R 1 . . C C9 0.7495(2) 0.02968(16) -0.11315(12) 0.0432(5) Uani d . 1 . . H H9A 0.7714 -0.0187 -0.0687 0.065 Uiso calc R 1 . . H H9B 0.76 -0.0011 -0.1668 0.065 Uiso calc R 1 . . H H9C 0.6649 0.0499 -0.1119 0.065 Uiso calc R 1 . . C C10 0.92816(16) 0.17002(12) 0.02306(10) 0.0213(2) Uani d . 1 . . C C11 0.81069(14) 0.01376(12) 0.25031(11) 0.0252(4) Uani d . 1 . . H H11A 0.7993 0.033 0.308 0.03 Uiso calc R 1 . . H H11B 0.8243 -0.0594 0.2482 0.03 Uiso calc R 1 . . C C12 0.70068(14) 0.04408(12) 0.19097(11) 0.0225(2) Uani d . 1 . . C C13 0.59073(17) 0.06977(16) 0.23526(12) 0.0351(5) Uani d . 1 . . H H13A 0.6123 0.1217 0.2768 0.053 Uiso calc R 1 . . H H13B 0.5631 0.0098 0.2626 0.053 Uiso calc R 1 . . H H13C 0.5258 0.0944 0.1949 0.053 Uiso calc R 1 . . C C14 0.6684(2) -0.03387(13) 0.12348(12) 0.0323(4) Uani d . 1 . . H H14A 0.6072 -0.0063 0.0819 0.048 Uiso calc R 1 . . H H14B 0.6362 -0.0939 0.1482 0.048 Uiso calc R 1 . . H H14C 0.7411 -0.0515 0.097 0.048 Uiso calc R 1 . . C C15 0.86366(14) 0.13844(12) 0.16694(9) 0.0181(2) Uani d . 1 . . C C16 1.08805(14) 0.22245(12) 0.15946(11) 0.0220(2) Uani d . 1 . . C C17 1.18350(18) 0.24762(18) 0.11454(13) 0.0407(5) Uani d . 1 . . H H17 1.1681 0.2575 0.0564 0.049 Uiso calc R 1 . . C C18 1.3011(2) 0.2588(2) 0.15191(16) 0.0538(7) Uani d . 1 . . H H18 1.3643 0.2761 0.1192 0.065 Uiso calc R 1 . . C C19 1.3263(2) 0.24511(17) 0.23555(16) 0.0450(5) Uani d . 1 . . H H19 1.4069 0.2513 0.2609 0.054 Uiso calc R 1 . . C C20 1.2337(2) 0.22242(13) 0.28213(13) 0.0396(5) Uani d . 1 . . H H20 1.2498 0.2139 0.3404 0.048 Uiso calc R 1 . . C C21 1.11674(18) 0.21186(12) 0.24461(11) 0.0297(4) Uani d . 1 . . H H21 1.0538 0.1968 0.2782 0.036 Uiso calc R 1 . . C C22 0.4714(2) 0.24300(17) -0.03433(12) 0.0391(5) Uani d . 1 . . H H22 0.3859 0.2408 -0.0463 0.047 Uiso calc R 1 . . N N1 0.77351(12) 0.33881(10) 0.08407(8) 0.0215(2) Uani d . 1 . . N N2 0.82254(12) 0.16305(11) -0.01682(8) 0.0236(2) Uani d . 1 . . N N3 0.74862(12) 0.13375(10) 0.15076(8) 0.0202(2) Uani d . 1 . . O O1 0.94568(11) 0.40457(9) 0.14176(8) 0.0275(2) Uani d . 1 . . O O2 1.01987(11) 0.13630(9) -0.01832(6) 0.0290(2) Uani d . 1 . . O O3 0.91222(10) 0.06824(8) 0.22085(6) 0.0216(2) Uani d . 1 . . O O4 0.51665(12) 0.19004(12) 0.02588(9) 0.0406(4) Uani d . 1 . . O O5 0.5259(2) 0.29556(13) -0.07773(12) 0.0686(5) Uani d . 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zn1 0.02163(11) 0.02108(10) 0.01975(10) 0.00387(8) -0.00137(6) -0.00195(8) B1 0.0194(9) 0.0179(8) 0.0177(8) 0.0029(7) 0.0036(7) 0.0011(7) C1 0.0355(10) 0.0188(8) 0.0394(11) 0.0058(8) -0.0001(8) -0.0042(8) C2 0.0309(9) 0.0178(8) 0.0275(9) 0.0059(7) 0.0024(7) -0.0001(7) C3 0.0616(15) 0.0338(11) 0.0364(11) 0.0024(10) -0.0026(10) 0.0122(9) C4 0.0325(11) 0.0337(11) 0.0510(13) 0.0111(9) 0.0051(9) -0.0089(9) C5 0.0249(8) 0.0183(8) 0.0166(8) 0.0009(5) 0.0053(5) -0.0004(5) C6 0.0492(11) 0.0341(10) 0.0229(9) 0.0114(9) 0.0107(9) -0.0040(8) C7 0.0429(11) 0.0251(9) 0.0155(8) 0.0084(8) 0.0049(7) -0.0007(7) C8 0.0646(15) 0.0415(11) 0.0223(9) 0.0153(11) 0.0036(10) 0.0072(9) C9 0.0637(15) 0.0356(11) 0.0308(11) -0.0036(10) 0.0067(10) -0.0104(9) C10 0.0272(9) 0.0180(8) 0.0197(8) 0.0066(7) 0.0073(7) 0.0033(5) C11 0.0268(9) 0.0255(9) 0.0232(9) -0.0044(7) 0.0024(7) 0.0050(7) C12 0.0232(9) 0.0216(8) 0.0230(8) -0.0015(7) 0.0038(7) 0.0010(7) C13 0.0286(10) 0.0378(11) 0.0409(11) -0.0017(8) 0.0128(9) -0.0001(9) C14 0.0409(11) 0.0239(9) 0.0309(10) -0.0046(8) -0.0016(8) -0.0024(8) C15 0.0241(8) 0.0167(7) 0.0135(7) 0.0040(5) 0.0023(5) -0.0021(5) C16 0.0213(8) 0.0170(8) 0.0279(9) 0.0044(5) 0.0032(7) 0.0003(7) C17 0.0276(10) 0.0621(14) 0.0332(11) -0.0040(10) 0.0074(8) -0.0073(10) C18 0.0234(11) 0.0786(18) 0.0615(16) -0.0061(11) 0.0150(10) -0.0262(14) C19 0.0247(11) 0.0375(11) 0.0695(16) 0.0093(9) -0.0120(10) -0.0194(11) C20 0.0459(13) 0.0248(10) 0.0435(11) -0.0054(9) -0.0181(10) 0.0036(9) C21 0.0339(10) 0.0249(9) 0.0289(9) -0.0069(8) -0.0036(8) 0.0031(8) C22 0.0402(11) 0.0411(11) 0.0325(11) 0.0110(10) -0.0127(9) -0.0124(9) N1 0.0254(7) 0.0174(7) 0.0217(7) 0.0041(5) 0.0015(5) -0.0003(5) N2 0.0304(8) 0.0241(7) 0.0163(7) 0.0065(5) 0.0028(5) -0.0022(5) N3 0.0208(7) 0.0189(7) 0.0209(7) 0.0008(5) 0.0026(5) 0.0009(5) O1 0.0270(7) 0.0173(5) 0.0373(7) 0.0019(5) -0.0011(5) -0.0036(5) O2 0.0317(7) 0.0323(7) 0.0247(5) 0.0095(5) 0.0111(5) -0.0019(5) O3 0.0215(5) 0.0212(5) 0.0216(5) 0.0003(5) 0.0001(5) 0.0055(5) O4 0.0250(7) 0.0595(10) 0.0355(8) 0.0036(7) -0.0054(5) 0.0048(7) O5 0.0776(14) 0.0624(11) 0.0609(11) -0.0036(10) -0.0164(10) 0.0207(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 O4 . 1.9088(14) ? Zn1 N1 . 2.0051(14) ? Zn1 N2 . 2.0255(14) ? Zn1 N3 . 2.0403(14) ? B1 C16 . 1.607(2) ? B1 C5 . 1.642(2) ? B1 C15 . 1.643(2) ? B1 C10 . 1.647(2) ? C1 O1 . 1.456(2) ? C1 C2 . 1.538(3) ? C1 H1A . 0.99 ? C1 H1B . 0.99 ? C2 N1 . 1.486(2) ? C2 C4 . 1.519(3) ? C2 C3 . 1.525(3) ? C3 H3A . 0.98 ? C3 H3B . 0.98 ? C3 H3C . 0.98 ? C4 H4A . 0.98 ? C4 H4B . 0.98 ? C4 H4C . 0.98 ? C5 N1 . 1.282(2) ? C5 O1 . 1.348(2) ? C6 O2 . 1.462(2) ? C6 C7 . 1.531(3) ? C6 H6A . 0.99 ? C6 H6B . 0.99 ? C7 N2 . 1.483(2) ? C7 C9 . 1.518(3) ? C7 C8 . 1.525(3) ? C8 H8A . 0.98 ? C8 H8B . 0.98 ? C8 H8C . 0.98 ? C9 H9A . 0.98 ? C9 H9B . 0.98 ? C9 H9C . 0.98 ? C10 N2 . 1.284(2) ? C10 O2 . 1.352(2) ? C11 O3 . 1.462(2) ? C11 C12 . 1.531(2) ? C11 H11A . 0.99 ? C11 H11B . 0.99 ? C12 N3 . 1.488(2) ? C12 C13 . 1.517(2) ? C12 C14 . 1.527(2) ? 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 N3 . 1.279(2) ? C15 O3 . 1.356(2) ? C16 C17 . 1.387(3) ? C16 C21 . 1.392(2) ? C17 C18 . 1.391(3) ? C17 H17 . 0.95 ? C18 C19 . 1.369(4) ? C18 H18 . 0.95 ? C19 C20 . 1.369(3) ? C19 H19 . 0.95 ? C20 C21 . 1.385(3) ? C20 H20 . 0.95 ? C21 H21 . 0.95 ? C22 O5 . 1.200(3) ? C22 O4 . 1.268(2) ? C22 H22 . 0.95 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O4 Zn1 N1 . . 128.53(6) ? O4 Zn1 N2 . . 129.07(6) ? N1 Zn1 N2 . . 93.84(6) ? O4 Zn1 N3 . . 108.24(6) ? N1 Zn1 N3 . . 94.41(6) ? N2 Zn1 N3 . . 92.72(5) ? C16 B1 C5 . . 111.11(14) ? C16 B1 C15 . . 115.38(13) ? C5 B1 C15 . . 106.06(13) ? C16 B1 C10 . . 117.50(14) ? C5 B1 C10 . . 104.23(13) ? C15 B1 C10 . . 101.26(13) ? O1 C1 C2 . . 105.32(14) ? O1 C1 H1A . . 110.7 ? C2 C1 H1A . . 110.7 ? O1 C1 H1B . . 110.7 ? C2 C1 H1B . . 110.7 ? H1A C1 H1B . . 108.8 ? N1 C2 C4 . . 109.87(15) ? N1 C2 C3 . . 108.53(15) ? C4 C2 C3 . . 111.40(17) ? N1 C2 C1 . . 100.78(13) ? C4 C2 C1 . . 113.45(16) ? C3 C2 C1 . . 112.21(16) ? C2 C3 H3A . . 109.5 ? C2 C3 H3B . . 109.5 ? H3A C3 H3B . . 109.5 ? C2 C3 H3C . . 109.5 ? H3A C3 H3C . . 109.5 ? H3B C3 H3C . . 109.5 ? C2 C4 H4A . . 109.5 ? C2 C4 H4B . . 109.5 ? H4A C4 H4B . . 109.5 ? C2 C4 H4C . . 109.5 ? H4A C4 H4C . . 109.5 ? H4B C4 H4C . . 109.5 ? N1 C5 O1 . . 115.36(14) ? N1 C5 B1 . . 125.24(15) ? O1 C5 B1 . . 119.39(14) ? O2 C6 C7 . . 105.45(13) ? O2 C6 H6A . . 110.7 ? C7 C6 H6A . . 110.7 ? O2 C6 H6B . . 110.7 ? C7 C6 H6B . . 110.7 ? H6A C6 H6B . . 108.8 ? N2 C7 C9 . . 109.59(15) ? N2 C7 C8 . . 108.38(15) ? C9 C7 C8 . . 111.55(17) ? N2 C7 C6 . . 101.42(14) ? C9 C7 C6 . . 112.75(16) ? C8 C7 C6 . . 112.58(17) ? C7 C8 H8A . . 109.5 ? C7 C8 H8B . . 109.5 ? H8A C8 H8B . . 109.5 ? C7 C8 H8C . . 109.5 ? H8A C8 H8C . . 109.5 ? H8B C8 H8C . . 109.5 ? C7 C9 H9A . . 109.5 ? C7 C9 H9B . . 109.5 ? H9A C9 H9B . . 109.5 ? C7 C9 H9C . . 109.5 ? H9A C9 H9C . . 109.5 ? H9B C9 H9C . . 109.5 ? N2 C10 O2 . . 114.92(15) ? N2 C10 B1 . . 122.82(14) ? O2 C10 B1 . . 122.23(14) ? O3 C11 C12 . . 104.81(13) ? O3 C11 H11A . . 110.8 ? C12 C11 H11A . . 110.8 ? O3 C11 H11B . . 110.8 ? C12 C11 H11B . . 110.8 ? H11A C11 H11B . . 108.9 ? N3 C12 C13 . . 111.46(14) ? N3 C12 C14 . . 107.69(14) ? C13 C12 C14 . . 110.58(15) ? N3 C12 C11 . . 100.98(13) ? C13 C12 C11 . . 113.06(15) ? C14 C12 C11 . . 112.61(15) ? 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 ? N3 C15 O3 . . 114.96(14) ? N3 C15 B1 . . 123.65(14) ? O3 C15 B1 . . 120.95(13) ? C17 C16 C21 . . 115.78(17) ? C17 C16 B1 . . 123.13(16) ? C21 C16 B1 . . 120.95(15) ? C16 C17 C18 . . 122.1(2) ? C16 C17 H17 . . 119.0 ? C18 C17 H17 . . 119.0 ? C19 C18 C17 . . 120.4(2) ? C19 C18 H18 . . 119.8 ? C17 C18 H18 . . 119.8 ? C18 C19 C20 . . 119.1(2) ? C18 C19 H19 . . 120.5 ? C20 C19 H19 . . 120.5 ? C19 C20 C21 . . 120.2(2) ? C19 C20 H20 . . 119.9 ? C21 C20 H20 . . 119.9 ? C20 C21 C16 . . 122.4(2) ? C20 C21 H21 . . 118.8 ? C16 C21 H21 . . 118.8 ? O5 C22 O4 . . 126.5(2) ? O5 C22 H22 . . 116.8 ? O4 C22 H22 . . 116.8 ? C5 N1 C2 . . 110.23(14) ? C5 N1 Zn1 . . 112.41(11) ? C2 N1 Zn1 . . 137.31(12) ? C10 N2 C7 . . 110.64(14) ? C10 N2 Zn1 . . 114.06(11) ? C7 N2 Zn1 . . 135.29(12) ? C15 N3 C12 . . 110.09(14) ? C15 N3 Zn1 . . 112.94(11) ? C12 N3 Zn1 . . 132.05(11) ? C5 O1 C1 . . 106.71(13) ? C10 O2 C6 . . 106.98(14) ? C15 O3 C11 . . 106.58(12) ? C22 O4 Zn1 . . 111.08(15) ? data_Ia _database_code_depnum_ccdc_archive 'CCDC 902694' #TrackingRef 'web_deposit_cif_file_1_AaronD.Sadow_1348401140.ToMMgOMe.cif' _audit_creation_method 'APEX2 v2010.11-3' _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C44 H64 B2 Mg2 N6 O8, 2(C6 H6)' _chemical_formula_sum 'C56 H76 B2 Mg2 N6 O8' _chemical_formula_iupac ? _chemical_formula_weight 1031.47 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' 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 9.500(2) _cell_length_b 26.648(6) _cell_length_c 22.844(5) _cell_angle_alpha 90 _cell_angle_beta 97.235(3) _cell_angle_gamma 90 _cell_volume 5737.(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8581 _cell_measurement_theta_min 2.2924 _cell_measurement_theta_max 28.5164 _cell_measurement_temperature 173.(2) _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 0.098 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 0.99 _exptl_special_details ; A X-ray quality crystal was selected under ambient conditions and covered with PARATONE oil The crystal was mounted and centered in the X-ray beam by using a video camera.The crystal evaluation and data collection were performed on APEX-2 CCD diffractometer with the detector to crystal distance of 5cm. The initial cell constants were obtained from three series of OMEGA scans at different starting angles. Each series consisted of 30 frames collected at intervals of 0.3 in a 10 range about OMEGA with the exposure time of 10 seconds per frame. The obtained reflections were successfully indexed by an automated indexing routine built to APEX2 program package. The final cell constants were calculated from a set of strong reflections from the actual data collection. The data were collected using the full sphere routine by collecting four sets of frames with 0.3 scans in \w with an exposure time 10 sec per frame. This dataset was corrected for Lorentz and polarization effects. The absorption correction was based on a fit of a spherical harmonic function to the empirical transmission surface as sampled by multiple equivalent measurements using SADABS software. ; _diffrn_ambient_temperature 173.(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source ? _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ' BRUKER APEX2 CCD Diffractometer' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 29698 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 28.65 _diffrn_reflns_theta_full 28.65 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _refine_special_details ; The systematic absences in the diffraction data were consistent for the stated space group. The position of almost all non-hydrogen atoms were found by direct methods. The remaining atoms were located in an alternating series of least-squares cycles on difference Fourier maps. All non-hydrogen atoms were refined in full-matrix anisotropic approximation. All hydrogen atoms were placed in the structure factor calculation at idealized positions and were allowed to ride on the neighboring atoms with relative isotropic displacement coefficients. One half of a dimer in asymmetric unit. Final results were tested with CHECKCIF routine and all A-warnings (if any) were addressed on the very top of this file. ; _reflns_number_total 7356 _reflns_number_gt 5683 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_gt 0.1001 _refine_ls_wR_factor_ref 0.1105 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_number_reflns 7356 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+3.7204P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.305 _refine_diff_density_min -0.252 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' _computing_data_collection 'APEX2 Suite (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT V7.66A (Bruker AXS, 2009)' _computing_data_reduction 'SAINT V7.66A (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XSHELL (Bruker AXS, 2007)' _computing_publication_material 'APEX2 Suite (Bruker AXS, 2009)' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mg Mg1 0.53646(4) 0.85285(15) 0.318317(16) 0.01947(10) Uani d . 1 . . B B1 0.54042(15) 0.85561(5) 0.46200(6) 0.0220(3) Uani d . 1 . . C C1 0.65688(16) 0.98361(5) 0.35005(6) 0.0329(3) Uani d . 1 . . H H1A 0.7226 0.976 0.3855 0.049 Uiso calc R 1 . . H H1B 0.6634 1.0193 0.3406 0.049 Uiso calc R 1 . . H H1C 0.6818 0.9635 0.317 0.049 Uiso calc R 1 . . C C2 0.50562(14) 0.97126(5) 0.36112(5) 0.0244(3) Uani d . 1 . . C C3 0.39467(16) 0.98695(5) 0.31076(6) 0.0331(3) Uani d . 1 . . H H3A 0.4078 0.9677 0.2753 0.05 Uiso calc R 1 . . H H3B 0.4048 1.0228 0.3028 0.05 Uiso calc R 1 . . H H3C 0.2997 0.9805 0.3216 0.05 Uiso calc R 1 . . C C4 0.47321(17) 0.99225(5) 0.42025(5) 0.0322(3) Uani d . 1 . . H H4A 0.5337 1.0217 0.4322 0.039 Uiso calc R 1 . . H H4B 0.3723 1.0022 0.4182 0.039 Uiso calc R 1 . . C C5 0.50897(13) 0.90868(4) 0.42770(5) 0.0217(2) Uani d . 1 . . C C6 0.49104(17) 0.71199(6) 0.36483(7) 0.0399(3) Uani d . 1 . . H H6A 0.5432 0.719 0.3314 0.06 Uiso calc R 1 . . H H6B 0.4526 0.6778 0.3613 0.06 Uiso calc R 1 . . H H6C 0.5553 0.7151 0.4017 0.06 Uiso calc R 1 . . C C7 0.36982(14) 0.74938(5) 0.36490(5) 0.0251(3) Uani d . 1 . . C C8 0.26644(17) 0.74503(6) 0.30863(6) 0.0369(3) Uani d . 1 . . H H8A 0.1926 0.7707 0.3086 0.055 Uiso calc R 1 . . H H8B 0.2226 0.7117 0.3067 0.055 Uiso calc R 1 . . H H8C 0.3175 0.7499 0.2744 0.055 Uiso calc R 1 . . C C9 0.29745(15) 0.74424(5) 0.42081(6) 0.0292(3) Uani d . 1 . . H H9A 0.1953 0.7526 0.4128 0.035 Uiso calc R 1 . . H H9B 0.3075 0.7097 0.4368 0.035 Uiso calc R 1 . . C C10 0.44025(13) 0.81199(4) 0.42817(5) 0.0213(2) Uani d . 1 . . C C11 0.87080(17) 0.77305(6) 0.34934(7) 0.0395(3) Uani d . 1 . . H H11A 0.8006 0.7481 0.358 0.059 Uiso calc R 1 . . H H11B 0.9648 0.7574 0.3526 0.059 Uiso calc R 1 . . H H11C 0.8455 0.7859 0.3092 0.059 Uiso calc R 1 . . C C12 0.87307(14) 0.81603(6) 0.39299(6) 0.0305(3) Uani d . 1 . . C C13 0.97567(17) 0.85718(7) 0.38030(7) 0.0425(4) Uani d . 1 . . H H13A 0.948 0.8704 0.3405 0.064 Uiso calc R 1 . . H H13B 1.0719 0.8434 0.383 0.064 Uiso calc R 1 . . H H13C 0.9733 0.8843 0.4092 0.064 Uiso calc R 1 . . C C14 0.90522(17) 0.79728(8) 0.45707(7) 0.0463(4) Uani d . 1 . . H H14A 0.9027 0.7602 0.4586 0.056 Uiso calc R 1 . . H H14B 0.9998 0.8089 0.4751 0.056 Uiso calc R 1 . . C C15 0.69527(14) 0.83830(5) 0.44475(5) 0.0244(3) Uani d . 1 . . C C16 0.52047(16) 0.86139(5) 0.53094(5) 0.0274(3) Uani d . 1 . . C C17 0.6302(2) 0.86236(6) 0.57789(6) 0.0414(4) Uani d . 1 . . H H17 0.7253 0.8578 0.5701 0.05 Uiso calc R 1 . . C C18 0.6030(3) 0.86987(7) 0.63608(7) 0.0570(5) Uani d . 1 . . H H18 0.6797 0.8701 0.6671 0.068 Uiso calc R 1 . . C C19 0.4675(3) 0.87692(6) 0.64883(7) 0.0547(5) Uani d . 1 . . H H19 0.4498 0.8817 0.6885 0.066 Uiso calc R 1 . . C C20 0.3570(2) 0.87699(6) 0.60355(7) 0.0480(4) Uani d . 1 . . H H20 0.2626 0.8823 0.6118 0.058 Uiso calc R 1 . . C C21 0.38357(17) 0.86926(6) 0.54565(6) 0.0361(3) Uani d . 1 . . H H21 0.306 0.8693 0.515 0.043 Uiso calc R 1 . . C C22 0.76462(14) 0.87096(6) 0.23300(6) 0.0312(3) Uani d . 1 . . H H22A 0.7957 0.9007 0.2564 0.047 Uiso calc R 1 . . H H22B 0.7577 0.8792 0.1909 0.047 Uiso calc R 1 . . H H22C 0.8335 0.8438 0.2421 0.047 Uiso calc R 1 . . C C23 1.0 1.00661(15) 0.75 0.126(3) Uani d S 1 . . H H23 1.0 1.0423 0.75 0.151 Uiso calc SR 1 . . C C24 0.9991(3) 0.98058(13) 0.80189(19) 0.1108(13) Uani d . 1 . . H H24 0.9982 0.9983 0.8379 0.133 Uiso calc R 1 . . C C25 0.9994(5) 0.93090(14) 0.80174(18) 0.1296(14) Uani d . 1 . . H H25 0.9992 0.9128 0.8375 0.156 Uiso calc R 1 . . C C26 1.0 0.90630(17) 0.75 0.167(3) Uani d S 1 . . H H26 1.0 0.8707 0.75 0.2 Uiso calc SR 1 . . C C27 0.9791(2) 0.95038(8) 0.98604(9) 0.0604(5) Uani d . 1 . . H H27 0.9648 0.9159 0.9765 0.072 Uiso calc R 1 . . C C28 0.8676(2) 0.97896(9) 0.99973(9) 0.0624(5) Uani d . 1 . . H H28 0.7764 0.9643 0.9994 0.075 Uiso calc R 1 . . C C29 0.8878(2) 1.02857(9) 1.01388(9) 0.0629(5) Uani d . 1 . . H H29 0.811 1.0484 1.0236 0.075 Uiso calc R 1 . . N N1 0.50003(11) 0.91597(4) 0.37173(4) 0.0218(2) Uani d . 1 . . N N2 0.43417(11) 0.80047(4) 0.37319(4) 0.0229(2) Uani d . 1 . . N N3 0.72754(11) 0.83755(4) 0.39187(5) 0.0268(2) Uani d . 1 . . O O1 0.50552(11) 0.95066(3) 0.46120(4) 0.0289(2) Uani d . 1 . . O O2 0.37190(10) 0.78001(3) 0.46150(4) 0.0262(2) Uani d . 1 . . O O3 0.79418(11) 0.81875(4) 0.48715(4) 0.0360(2) Uani d . 1 . . O O4 0.63110(9) 0.85549(3) 0.24671(4) 0.02399(19) Uani d . 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mg1 0.0256(2) 0.0197(2) 0.01373(18) -0.00032(15) 0.00491(15) -0.00036(14) B1 0.0292(7) 0.0219(6) 0.0150(6) -0.0009(5) 0.0037(5) 0.0012(5) C1 0.0410(8) 0.0327(7) 0.0257(6) -0.0077(6) 0.0067(6) 0.0002(5) C2 0.0369(7) 0.0191(6) 0.0180(6) 0.0000(5) 0.0067(5) -0.0012(4) C3 0.0443(8) 0.0297(7) 0.0250(6) 0.0059(6) 0.0036(6) 0.0035(5) C4 0.0563(9) 0.0218(6) 0.0202(6) 0.0032(6) 0.0116(6) 0.0004(5) C5 0.0264(6) 0.0222(6) 0.0172(5) -0.0022(5) 0.0057(4) -0.0023(4) C6 0.0453(9) 0.0290(7) 0.0464(9) 0.0017(6) 0.0101(7) -0.0061(6) C7 0.0326(7) 0.0227(6) 0.0203(6) -0.0055(5) 0.0040(5) 0.0002(4) C8 0.0487(9) 0.0370(8) 0.0236(6) -0.0165(7) -0.0009(6) 0.0004(5) C9 0.0363(7) 0.0280(7) 0.0233(6) -0.0097(5) 0.0041(5) 0.0008(5) C10 0.0251(6) 0.0206(6) 0.0185(5) 0.0016(5) 0.0048(4) 0.0036(4) C11 0.0337(8) 0.0417(8) 0.0424(8) 0.0077(6) 0.0021(6) -0.0027(7) C12 0.0235(6) 0.0428(8) 0.0248(6) 0.0047(6) 0.0020(5) 0.0023(5) C13 0.0328(8) 0.0550(10) 0.0399(8) -0.0073(7) 0.0057(6) -0.0068(7) C14 0.0355(8) 0.0718(12) 0.0313(8) 0.0201(8) 0.0027(6) 0.0107(7) C15 0.0276(6) 0.0262(6) 0.0187(6) -0.0007(5) -0.0006(5) 0.0025(4) C16 0.0462(8) 0.0194(6) 0.0174(5) -0.0037(5) 0.0070(5) 0.0009(4) C17 0.0619(10) 0.0397(8) 0.0211(6) 0.0099(7) -0.0007(6) -0.0028(6) C18 0.1007(16) 0.0481(10) 0.0191(7) 0.0143(10) -0.0039(8) -0.0036(6) C19 0.1129(17) 0.0339(8) 0.0217(7) -0.0072(9) 0.0264(9) -0.0029(6) C20 0.0771(12) 0.0349(8) 0.0393(8) -0.0207(8) 0.0354(9) -0.0125(7) C21 0.0495(9) 0.0330(7) 0.0287(7) -0.0138(6) 0.0171(6) -0.0076(6) C22 0.0267(7) 0.0391(8) 0.0287(7) -0.0002(6) 0.0077(5) 0.0029(6) C23 0.0354(17) 0.044(2) 0.292(8) 0 -0.004(3) 0 C24 0.0518(15) 0.097(2) 0.188(4) -0.0121(16) 0.0320(19) -0.058(2) C25 0.188(4) 0.087(2) 0.126(3) -0.033(2) 0.069(3) -0.002(2) C26 0.324(10) 0.050(2) 0.142(5) 0 0.086(6) 0 C27 0.0702(13) 0.0614(12) 0.0486(11) -0.0046(10) 0.0034(9) 0.0098(9) C28 0.0493(11) 0.0804(15) 0.0566(12) -0.0060(10) 0.0036(9) 0.0120(10) C29 0.0551(12) 0.0753(15) 0.0583(12) 0.0088(10) 0.0079(9) 0.0105(10) N1 0.0299(5) 0.0194(5) 0.0164(4) 0.0004(4) 0.0043(4) -0.0001(4) N2 0.0294(5) 0.0216(5) 0.0179(5) -0.0039(4) 0.0034(4) 0.0005(4) N3 0.0243(5) 0.0348(6) 0.0214(5) 0.0045(4) 0.0034(4) 0.0035(4) O1 0.0507(6) 0.0209(4) 0.0166(4) -0.0009(4) 0.0094(4) -0.0020(3) O2 0.0358(5) 0.0254(5) 0.0185(4) -0.0068(4) 0.0072(4) 0.0013(3) O3 0.0340(5) 0.0524(6) 0.0206(5) 0.0098(5) -0.0009(4) 0.0055(4) O4 0.0236(4) 0.0329(5) 0.0162(4) -0.0007(4) 0.0057(3) -0.0002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mg1 O4 . 1.9645(10) ? Mg1 O4 2_655 2.0372(10) ? Mg1 N1 . 2.1317(11) ? Mg1 N2 . 2.1843(11) ? Mg1 N3 . 2.3487(12) ? Mg1 Mg1 2_655 3.1108(10) ? B1 C16 . 1.6170(18) ? B1 C5 . 1.6262(18) ? B1 C10 . 1.6337(18) ? B1 C15 . 1.6365(19) ? C1 C2 . 1.5260(19) ? C1 H1A . 0.98 ? C1 H1B . 0.98 ? C1 H1C . 0.98 ? C2 N1 . 1.4952(16) ? C2 C3 . 1.5179(19) ? C2 C4 . 1.5287(17) ? C3 H3A . 0.98 ? C3 H3B . 0.98 ? C3 H3C . 0.98 ? C4 O1 . 1.4578(15) ? C4 H4A . 0.99 ? C4 H4B . 0.99 ? C5 N1 . 1.2854(15) ? C5 O1 . 1.3579(14) ? C6 C7 . 1.523(2) ? C6 H6A . 0.98 ? C6 H6B . 0.98 ? C6 H6C . 0.98 ? C7 N2 . 1.4946(16) ? C7 C8 . 1.5206(18) ? C7 C9 . 1.5308(18) ? C8 H8A . 0.98 ? C8 H8B . 0.98 ? C8 H8C . 0.98 ? C9 O2 . 1.4517(15) ? C9 H9A . 0.99 ? C9 H9B . 0.99 ? C10 N2 . 1.2871(15) ? C10 O2 . 1.3609(14) ? C11 C12 . 1.517(2) ? C11 H11A . 0.98 ? C11 H11B . 0.98 ? C11 H11C . 0.98 ? C12 N3 . 1.4940(17) ? C12 C13 . 1.519(2) ? C12 C14 . 1.540(2) ? C13 H13A . 0.98 ? C13 H13B . 0.98 ? C13 H13C . 0.98 ? C14 O3 . 1.4473(19) ? C14 H14A . 0.99 ? C14 H14B . 0.99 ? C15 N3 . 1.2833(16) ? C15 O3 . 1.3650(15) ? C16 C17 . 1.398(2) ? C16 C21 . 1.399(2) ? C17 C18 . 1.400(2) ? C17 H17 . 0.95 ? C18 C19 . 1.368(3) ? C18 H18 . 0.95 ? C19 C20 . 1.378(3) ? C19 H19 . 0.95 ? C20 C21 . 1.393(2) ? C20 H20 . 0.95 ? C21 H21 . 0.95 ? C22 O4 . 1.4061(16) ? C22 H22A . 0.98 ? C22 H22B . 0.98 ? C22 H22C . 0.98 ? C23 C24 . 1.374(4) ? C23 C24 2_756 1.374(4) ? C23 H23 . 0.95 ? C24 C25 . 1.324(5) ? C24 H24 . 0.95 ? C25 C26 . 1.352(4) ? C25 H25 . 0.95 ? C26 C25 2_756 1.352(4) ? C26 H26 . 0.95 ? C27 C28 . 1.372(3) ? C27 C29 5_777 1.383(3) ? C27 H27 . 0.95 ? C28 C29 . 1.369(3) ? C28 H28 . 0.95 ? C29 C27 5_777 1.383(3) ? C29 H29 . 0.95 ? O4 Mg1 2_655 2.0371(10) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O4 Mg1 O4 . 2_655 77.83(4) ? O4 Mg1 N1 . . 124.94(4) ? O4 Mg1 N1 2_655 . 102.81(4) ? O4 Mg1 N2 . . 141.63(4) ? O4 Mg1 N2 2_655 . 94.43(4) ? N1 Mg1 N2 . . 93.42(4) ? O4 Mg1 N3 . . 102.03(4) ? O4 Mg1 N3 2_655 . 171.98(4) ? N1 Mg1 N3 . . 83.92(4) ? N2 Mg1 N3 . . 80.68(4) ? O4 Mg1 Mg1 . 2_655 39.83(3) ? O4 Mg1 Mg1 2_655 2_655 38.15(3) ? N1 Mg1 Mg1 . 2_655 122.86(3) ? N2 Mg1 Mg1 . 2_655 121.12(3) ? N3 Mg1 Mg1 . 2_655 140.55(3) ? C16 B1 C5 . . 110.45(10) ? C16 B1 C10 . . 113.32(10) ? C5 B1 C10 . . 109.28(10) ? C16 B1 C15 . . 118.72(11) ? C5 B1 C15 . . 104.19(10) ? C10 B1 C15 . . 99.98(10) ? C2 C1 H1A . . 109.5 ? C2 C1 H1B . . 109.5 ? H1A C1 H1B . . 109.5 ? C2 C1 H1C . . 109.5 ? H1A C1 H1C . . 109.5 ? H1B C1 H1C . . 109.5 ? N1 C2 C3 . . 111.03(10) ? N1 C2 C1 . . 107.03(11) ? C3 C2 C1 . . 113.17(11) ? N1 C2 C4 . . 101.66(9) ? C3 C2 C4 . . 111.78(11) ? C1 C2 C4 . . 111.47(11) ? C2 C3 H3A . . 109.5 ? C2 C3 H3B . . 109.5 ? H3A C3 H3B . . 109.5 ? C2 C3 H3C . . 109.5 ? H3A C3 H3C . . 109.5 ? H3B C3 H3C . . 109.5 ? O1 C4 C2 . . 103.84(10) ? O1 C4 H4A . . 111.0 ? C2 C4 H4A . . 111.0 ? O1 C4 H4B . . 111.0 ? C2 C4 H4B . . 111.0 ? H4A C4 H4B . . 109.0 ? N1 C5 O1 . . 115.65(11) ? N1 C5 B1 . . 126.56(11) ? O1 C5 B1 . . 117.45(10) ? C7 C6 H6A . . 109.5 ? C7 C6 H6B . . 109.5 ? H6A C6 H6B . . 109.5 ? C7 C6 H6C . . 109.5 ? H6A C6 H6C . . 109.5 ? H6B C6 H6C . . 109.5 ? N2 C7 C8 . . 112.76(10) ? N2 C7 C6 . . 107.38(11) ? C8 C7 C6 . . 110.93(12) ? N2 C7 C9 . . 101.26(10) ? C8 C7 C9 . . 112.85(11) ? C6 C7 C9 . . 111.20(11) ? C7 C8 H8A . . 109.5 ? C7 C8 H8B . . 109.5 ? H8A C8 H8B . . 109.5 ? C7 C8 H8C . . 109.5 ? H8A C8 H8C . . 109.5 ? H8B C8 H8C . . 109.5 ? O2 C9 C7 . . 103.99(10) ? O2 C9 H9A . . 111.0 ? C7 C9 H9A . . 111.0 ? O2 C9 H9B . . 111.0 ? C7 C9 H9B . . 111.0 ? H9A C9 H9B . . 109.0 ? N2 C10 O2 . . 115.51(11) ? N2 C10 B1 . . 125.68(11) ? O2 C10 B1 . . 118.11(10) ? C12 C11 H11A . . 109.5 ? C12 C11 H11B . . 109.5 ? H11A C11 H11B . . 109.5 ? C12 C11 H11C . . 109.5 ? H11A C11 H11C . . 109.5 ? H11B C11 H11C . . 109.5 ? N3 C12 C11 . . 110.00(11) ? N3 C12 C13 . . 109.52(12) ? C11 C12 C13 . . 112.08(12) ? N3 C12 C14 . . 102.31(11) ? C11 C12 C14 . . 111.38(13) ? C13 C12 C14 . . 111.12(13) ? 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 ? O3 C14 C12 . . 104.70(11) ? O3 C14 H14A . . 110.8 ? C12 C14 H14A . . 110.8 ? O3 C14 H14B . . 110.8 ? C12 C14 H14B . . 110.8 ? H14A C14 H14B . . 108.9 ? N3 C15 O3 . . 115.92(12) ? N3 C15 B1 . . 124.03(11) ? O3 C15 B1 . . 119.74(10) ? C17 C16 C21 . . 116.01(13) ? C17 C16 B1 . . 125.53(13) ? C21 C16 B1 . . 118.33(12) ? C16 C17 C18 . . 121.48(17) ? C16 C17 H17 . . 119.3 ? C18 C17 H17 . . 119.3 ? C19 C18 C17 . . 120.84(17) ? C19 C18 H18 . . 119.6 ? C17 C18 H18 . . 119.6 ? C18 C19 C20 . . 119.26(14) ? C18 C19 H19 . . 120.4 ? C20 C19 H19 . . 120.4 ? C19 C20 C21 . . 120.03(17) ? C19 C20 H20 . . 120.0 ? C21 C20 H20 . . 120.0 ? C20 C21 C16 . . 122.37(16) ? C20 C21 H21 . . 118.8 ? C16 C21 H21 . . 118.8 ? O4 C22 H22A . . 109.5 ? O4 C22 H22B . . 109.5 ? H22A C22 H22B . . 109.5 ? O4 C22 H22C . . 109.5 ? H22A C22 H22C . . 109.5 ? H22B C22 H22C . . 109.5 ? C24 C23 C24 . 2_756 119.4(4) ? C24 C23 H23 . . 120.3 ? C24 C23 H23 2_756 . 120.3 ? C25 C24 C23 . . 120.2(4) ? C25 C24 H24 . . 119.9 ? C23 C24 H24 . . 119.9 ? C24 C25 C26 . . 119.2(4) ? C24 C25 H25 . . 120.4 ? C26 C25 H25 . . 120.4 ? C25 C26 C25 . 2_756 122.0(5) ? C25 C26 H26 . . 119.0 ? C25 C26 H26 2_756 . 119.0 ? C28 C27 C29 . 5_777 120.4(2) ? C28 C27 H27 . . 119.8 ? C29 C27 H27 5_777 . 119.8 ? C29 C28 C27 . . 120.0(2) ? C29 C28 H28 . . 120.0 ? C27 C28 H28 . . 120.0 ? C28 C29 C27 . 5_777 119.5(2) ? C28 C29 H29 . . 120.2 ? C27 C29 H29 5_777 . 120.2 ? C5 N1 C2 . . 108.10(10) ? C5 N1 Mg1 . . 117.07(8) ? C2 N1 Mg1 . . 132.31(7) ? C10 N2 C7 . . 107.96(10) ? C10 N2 Mg1 . . 116.04(8) ? C7 N2 Mg1 . . 135.55(8) ? C15 N3 C12 . . 108.67(10) ? C15 N3 Mg1 . . 114.58(9) ? C12 N3 Mg1 . . 135.16(8) ? C5 O1 C4 . . 106.43(9) ? C10 O2 C9 . . 106.32(9) ? C15 O3 C14 . . 106.97(10) ? C22 O4 Mg1 . . 135.75(8) ? C22 O4 Mg1 . 2_655 119.45(8) ? Mg1 O4 Mg1 . 2_655 102.02(4) ? data_I _database_code_depnum_ccdc_archive 'CCDC 902695' #TrackingRef 'web_deposit_cif_file_0_AaronSadow_1352927324.ToMZnSi(SiHMe2)3_1.cif' _audit_creation_method 'APEX2 v2010.11-3' _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H47 B N3 O3 Si4 Zn' _chemical_formula_iupac ? _chemical_formula_weight 650.22 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.4488(12) _cell_length_b 27.824(4) _cell_length_c 13.6110(18) _cell_angle_alpha 90 _cell_angle_beta 93.087(2) _cell_angle_gamma 90 _cell_volume 3573.2(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9935 _cell_measurement_theta_min 2.6082 _cell_measurement_theta_max 29.1631 _cell_measurement_temperature 173.(2) _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 1.209 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1380 _exptl_absorpt_coefficient_mu 0.851 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _exptl_absorpt_correction_T_min 0.64 _exptl_absorpt_correction_T_max 0.87 _exptl_special_details ; A X-ray quality crystal was selected under ambient conditions and covered with PARATONE oil The crystal was mounted and centered in the X-ray beam by using a video camera.The crystal evaluation and data collection were performed on APEX-2 CCD diffractometer with the detector to crystal distance of 5cm. The initial cell constants were obtained from three series of OMEGA scans at different starting angles. Each series consisted of 30 frames collected at intervals of 0.3 in a 10 range about OMEGA with the exposure time of 10 seconds per frame. The obtained reflections were successfully indexed by an automated indexing routine built to APEX2 program package. The final cell constants were calculated from a set of strong reflections from the actual data collection. The data were collected using the full sphere routine by collecting four sets of frames with 0.3 scans in \w with an exposure time 10 sec per frame. This dataset was corrected for Lorentz and polarization effects. The absorption correction was based on a fit of a spherical harmonic function to the empirical transmission surface as sampled by multiple equivalent measurements using SADABS software. ; _diffrn_ambient_temperature 173.(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source ? _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ' BRUKER APEX2 CCD Diffractometer' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 38908 _diffrn_reflns_av_R_equivalents 0.0609 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 29.54 _diffrn_reflns_theta_full 29.54 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _refine_special_details ; The systematic absences in the diffraction data were consistent for the stated space group. The position of almost all non-hydrogen atoms were found by direct methods. The remaining atoms were located in an alternating series of least-squares cycles on difference Fourier maps. All non-hydrogen atoms were refined in full-matrix anisotropic approximation. Hydrogens of Si were found objectively on a difference Fourier map and were refined with relative to basic Si atom isotropic displacement coefficients. All other hydrogen atoms were placed in the structure factor calculation at idealized positions and were allowed to ride on the neighboring atoms with relative isotropic displacement coefficients. Three SiMe~3~ groups are disordered by two positions with occupancy factors 0.5. EADP restrains were applied to C atoms of disordered group together with DFIX restrain for Si- H distance. Final results were tested with CHECKCIF routine and all A-warnings (if any) were addressed on the very top of this file. ; _reflns_number_total 9895 _reflns_number_gt 7943 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_gt 0.1285 _refine_ls_wR_factor_ref 0.1388 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_number_reflns 9895 _refine_ls_number_parameters 422 _refine_ls_number_restraints 2 _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0679P)^2^+3.0567P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.037 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.042 _refine_diff_density_min -0.731 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' _computing_data_collection 'APEX2 Suite (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT V7.66A (Bruker AXS, 2009)' _computing_data_reduction 'SAINT V7.66A (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XSHELL (Bruker AXS, 2007)' _computing_publication_material 'APEX2 Suite (Bruker AXS, 2009)' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn1 0.62291(17) 0.12907(6) 0.298866(12) 0.02106(4) Uani d . 1.0 A . B B1 0.80907(18) 0.13408(6) 0.49688(12) 0.0240(3) Uani d . 1.0 . . C C1 0.7256(3) -0.00452(8) 0.2989(3) 0.1167(15) Uani d . 1.0 . . H H1A 0.689 -0.0079 0.3645 0.175 Uiso calc R 1.0 . . H H1B 0.7683 -0.0349 0.2795 0.175 Uiso calc R 1.0 . . H H1C 0.6477 0.0038 0.2515 0.175 Uiso calc R 1.0 . . C C2 0.8846(3) 0.04440(11) 0.20016(15) 0.0891(8) Uani d . 1.0 . . H H2A 0.8033 0.0534 0.1563 0.134 Uiso calc R 1.0 . . H H2B 0.9295 0.0155 0.1747 0.134 Uiso calc R 1.0 . . H H2C 0.9533 0.0708 0.2036 0.134 Uiso calc R 1.0 . . C C3 0.83556(17) 0.03445(5) 0.30059(12) 0.0294(3) Uani d . 1.0 . . C C4 0.9573(2) 0.02288(7) 0.37424(13) 0.0474(5) Uani d . 1.0 . . H H4A 0.9485 -0.0103 0.3994 0.057 Uiso calc R 1.0 . . H H4B 1.0493 0.026 0.3433 0.057 Uiso calc R 1.0 . . C C5 0.84091(15) 0.08809(5) 0.42630(10) 0.0238(3) Uani d . 1.0 . . C C6 0.3324(3) 0.18018(15) 0.4394(3) 0.1492(12) Uani d . 1.0 . . H H6A 0.3928 0.2075 0.4591 0.224 Uiso calc R 1.0 . . H H6B 0.239 0.1841 0.4664 0.224 Uiso calc R 1.0 . . H H6C 0.3218 0.1786 0.3675 0.224 Uiso calc R 1.0 . . C C7 0.4008(2) 0.13351(9) 0.47913(14) 0.0478(6) Uani d . 1.0 . . C C8 0.3140(3) 0.09114(16) 0.4536(2) 0.1383(12) Uani d . 1.0 . . H H8A 0.2886 0.0913 0.3829 0.207 Uiso calc R 1.0 . . H H8B 0.2276 0.0919 0.4903 0.207 Uiso calc R 1.0 . . H H8C 0.368 0.062 0.4707 0.207 Uiso calc R 1.0 . . C C9 0.4353(2) 0.13661(9) 0.58906(14) 0.0472(5) Uani d . 1.0 . . H H9A 0.3919 0.1656 0.6169 0.057 Uiso calc R 1.0 . . H H9B 0.3996 0.1079 0.6229 0.057 Uiso calc R 1.0 . . C C10 0.63794(17) 0.13358(5) 0.50945(11) 0.0264(3) Uani d . 1.0 . . C C11 0.8748(3) 0.21411(10) 0.19448(17) 0.0780(8) Uani d . 1.0 . . H H11A 0.9523 0.1913 0.2083 0.117 Uiso calc R 1.0 . . H H11B 0.9115 0.2427 0.1624 0.117 Uiso calc R 1.0 . . H H11C 0.8017 0.199 0.1509 0.117 Uiso calc R 1.0 . . C C12 0.81170(18) 0.22844(6) 0.28921(12) 0.0319(4) Uani d . 1.0 . . C C13 0.6908(3) 0.26328(8) 0.2700(3) 0.0822(9) Uani d . 1.0 . . H H13A 0.6177 0.2483 0.2264 0.123 Uiso calc R 1.0 . . H H13B 0.726 0.2923 0.2386 0.123 Uiso calc R 1.0 . . H H13C 0.6503 0.2719 0.3324 0.123 Uiso calc R 1.0 . . C C14 0.9230(2) 0.24847(7) 0.36381(15) 0.0524(5) Uani d . 1.0 . . H H14A 1.0166 0.2504 0.3347 0.063 Uiso calc R 1.0 . . H H14B 0.8959 0.281 0.3854 0.063 Uiso calc R 1.0 . . C C15 0.83144(16) 0.18005(5) 0.42361(11) 0.0262(3) Uani d . 1.0 . . C C16 0.90011(17) 0.13048(5) 0.60045(11) 0.0271(3) Uani d . 1.0 . . C C17 0.86416(19) 0.09437(7) 0.66701(12) 0.0357(4) Uani d . 1.0 . . H H17 0.7856 0.0741 0.6501 0.043 Uiso calc R 1.0 . . C C18 0.9391(2) 0.08712(7) 0.75656(13) 0.0388(4) Uani d . 1.0 . . H H18 0.9112 0.0624 0.7997 0.047 Uiso calc R 1.0 . . C C19 1.0543(2) 0.11587(7) 0.78270(13) 0.0405(4) Uani d . 1.0 . . H H19 1.1061 0.1112 0.8437 0.049 Uiso calc R 1.0 . . C C20 1.09318(19) 0.15151(8) 0.71884(13) 0.0413(4) Uani d . 1.0 . . H H20 1.1725 0.1713 0.7361 0.05 Uiso calc R 1.0 . . C C21 1.01692(17) 0.15869(6) 0.62905(12) 0.0328(4) Uani d . 1.0 . . H H21 1.0456 0.1835 0.5865 0.039 Uiso calc R 1.0 . . C C22A 0.3338(5) 0.01635(18) 0.2247(4) 0.0618(7) Uani d P 0.5420(6) A 1 H H22A 0.4133 0.0093 0.2717 0.093 Uiso calc PR 0.5420(6) A 1 H H22B 0.287 -0.0137 0.2042 0.093 Uiso calc PR 0.5420(6) A 1 H H22C 0.2658 0.0372 0.256 0.093 Uiso calc PR 0.5420(6) A 1 C C23A 0.1918(4) 0.05580(16) 0.0345(3) 0.0524(9) Uani d P 0.5420(6) A 1 C C24A 0.4894(5) 0.11156(19) -0.1144(3) 0.0568(13) Uani d P 0.5420(6) A 1 H H24A 0.3868 0.1169 -0.116 0.085 Uiso calc PR 0.5420(6) A 1 H H24B 0.5089 0.077 -0.1093 0.085 Uiso calc PR 0.5420(6) A 1 H H24C 0.5272 0.1241 -0.175 0.085 Uiso calc PR 0.5420(6) A 1 C C25A 0.7661(4) 0.1276(2) -0.0116(3) 0.0569(15) Uani d P 0.5420(6) A 1 H H25A 0.828 0.1417 0.0408 0.085 Uiso calc PR 0.5420(6) A 1 H H25B 0.7959 0.1387 -0.0757 0.085 Uiso calc PR 0.5420(6) A 1 H H25C 0.7726 0.0925 -0.0083 0.085 Uiso calc PR 0.5420(6) A 1 C C26A 0.3125(6) 0.23558(19) 0.1822(5) 0.0702(11) Uani d P 0.5420(6) A 1 H H26A 0.368 0.2372 0.2451 0.105 Uiso calc PR 0.5420(6) A 1 H H26B 0.2233 0.2531 0.1876 0.105 Uiso calc PR 0.5420(6) A 1 H H26C 0.3666 0.2501 0.1305 0.105 Uiso calc PR 0.5420(6) A 1 C C27A 0.1680(5) 0.17536(19) 0.0292(4) 0.0678(11) Uani d P 0.5420(6) A 1 H H27A 0.1469 0.1429 0.0045 0.102 Uiso calc PR 0.5420(6) A 1 H H27B 0.2231 0.1928 -0.0183 0.102 Uiso calc PR 0.5420(6) A 1 H H27C 0.0791 0.1925 0.0384 0.102 Uiso calc PR 0.5420(6) A 1 C C22B 0.3470(7) 0.0144(2) 0.2275(6) 0.0618(7) Uani d P 0.4580(6) A 2 H H22D 0.373 0.0227 0.2961 0.093 Uiso calc PR 0.4580(6) A 2 H H22E 0.4283 -0.0003 0.1976 0.093 Uiso calc PR 0.4580(6) A 2 H H22F 0.2676 -0.0083 0.2253 0.093 Uiso calc PR 0.4580(6) A 2 C C23B 0.2496(5) 0.0396(2) 0.0229(4) 0.0524(9) Uani d P 0.4580(6) A 2 C C24B 0.4719(7) 0.1316(2) -0.1126(4) 0.0568(13) Uani d P 0.4580(6) A 2 H H24D 0.3736 0.1208 -0.1097 0.085 Uiso calc PR 0.4580(6) A 2 H H24E 0.509 0.1217 -0.1754 0.085 Uiso calc PR 0.4580(6) A 2 H H24F 0.4756 0.1667 -0.1072 0.085 Uiso calc PR 0.4580(6) A 2 C C25B 0.7662(9) 0.1214(3) -0.0087(6) 0.074(2) Uani d P 0.4580(6) A 2 H H25D 0.8282 0.1081 0.0447 0.111 Uiso calc PR 0.4580(6) A 2 H H25E 0.7677 0.1566 -0.0052 0.111 Uiso calc PR 0.4580(6) A 2 H H25F 0.7997 0.111 -0.0722 0.111 Uiso calc PR 0.4580(6) A 2 C C26B 0.3021(8) 0.2316(3) 0.2055(6) 0.0702(11) Uani d P 0.4580(6) A 2 H H26D 0.3768 0.2368 0.2571 0.105 Uiso calc PR 0.4580(6) A 2 H H26E 0.2266 0.212 0.2315 0.105 Uiso calc PR 0.4580(6) A 2 H H26F 0.2631 0.2627 0.1836 0.105 Uiso calc PR 0.4580(6) A 2 C C27B 0.2167(6) 0.1950(2) 0.0135(5) 0.0678(11) Uani d P 0.4580(6) A 2 H H27D 0.2391 0.1766 -0.045 0.102 Uiso calc PR 0.4580(6) A 2 H H27E 0.1849 0.2273 -0.0062 0.102 Uiso calc PR 0.4580(6) A 2 H H27F 0.1413 0.1787 0.0473 0.102 Uiso calc PR 0.4580(6) A 2 N N1 0.77493(13) 0.07855(4) 0.34374(9) 0.0250(3) Uani d . 1.0 . . N N2 0.54295(14) 0.12924(5) 0.43892(10) 0.0274(3) Uani d . 1.0 . . N N3 0.76251(14) 0.18473(5) 0.34000(9) 0.0271(3) Uani d . 1.0 . . O O1 0.94718(12) 0.05764(4) 0.45370(8) 0.0319(3) Uani d . 1.0 . . O O2 0.58858(13) 0.13910(5) 0.60052(8) 0.0381(3) Uani d . 1.0 . . O O3 0.92764(13) 0.21506(4) 0.44637(9) 0.0368(3) Uani d . 1.0 . . Si Si1 0.48030(4) 0.124938(15) 0.14752(3) 0.02472(9) Uani d . 1.0 . . Si Si2A 0.39705(9) 0.04551(3) 0.12141(6) 0.03131(19) Uani d P 0.5420(6) A 1 H H21S 0.520(4) 0.0224(13) 0.094(3) 0.038 Uiso d P 0.5420(6) A 1 Si Si3A 0.58347(10) 0.14613(3) 0.00392(6) 0.0343(2) Uani d P 0.5420(6) A 1 H H31S 0.575(4) 0.2049(14) -0.002(3) 0.041 Uiso d P 0.5420(6) A 1 Si Si4A 0.27348(9) 0.17124(3) 0.15077(6) 0.03028(19) Uani d P 0.5420(6) A 1 H H41S 0.180(4) 0.1502(14) 0.218(3) 0.036 Uiso d P 0.5420(6) A 1 Si Si2B 0.29072(11) 0.07296(4) 0.15454(8) 0.0391(3) Uani d PD 0.4580(6) A 2 H H22S 0.1901(4) 0.0986(2) 0.2217(4) 0.047 Uiso d PD 0.4580(6) A 2 Si Si3B 0.59469(12) 0.10106(4) 0.00317(7) 0.0341(2) Uani d P 0.4580(6) A 2 H H32S 0.625(4) 0.0485(16) 0.011(3) 0.041 Uiso d P 0.4580(6) A 2 Si Si4B 0.37840(11) 0.19974(4) 0.09831(8) 0.0385(3) Uani d PD 0.4580(6) A 2 H H42S 0.4773(4) 0.23200(17) 0.0420(4) 0.046 Uiso d PD 0.4580(6) 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zn1 0.02159(7) 0.02036(7) 0.02106(7) 0.00047(6) -0.00051(6) -0.00029(6) B1 0.0260(7) 0.0236(7) 0.0219(7) 0.0003(6) -0.0012(6) -0.0012(6) C1 0.0514(14) 0.0320(10) 0.266(5) -0.0002(10) 0.003(2) -0.0488(18) C2 0.1322(19) 0.1058(17) 0.0310(10) 0.0836(14) 0.0197(12) 0.0122(10) C3 0.0323(7) 0.0244(7) 0.0311(7) 0.0079(6) -0.0012(6) -0.0050(6) C4 0.0594(10) 0.0504(10) 0.0311(8) 0.0316(9) -0.0098(8) -0.0097(7) C5 0.0249(6) 0.0236(6) 0.0230(6) 0.0022(5) 0.0012(5) 0.0032(5) C6 0.1241(17) 0.226(3) 0.105(2) 0.1331(19) 0.0703(15) 0.086(2) C7 0.0291(8) 0.0860(15) 0.0290(8) 0.0056(9) 0.0080(6) 0.0014(9) C8 0.0958(14) 0.256(3) 0.0678(15) -0.1240(17) 0.0462(12) -0.0756(18) C9 0.0360(9) 0.0748(14) 0.0318(9) 0.0019(9) 0.0101(7) -0.0071(9) C10 0.0312(7) 0.0250(6) 0.0232(6) 0.0025(6) 0.0038(5) -0.0011(5) C11 0.1076(17) 0.0728(15) 0.0571(13) -0.0486(13) 0.0373(13) -0.0124(11) C12 0.0371(8) 0.0239(7) 0.0341(8) -0.0088(6) -0.0037(6) 0.0046(6) C13 0.0624(14) 0.0375(11) 0.144(3) -0.0002(11) -0.0222(16) 0.0323(14) C14 0.0663(11) 0.0397(9) 0.0486(10) -0.0281(9) -0.0194(9) 0.0141(8) C15 0.0283(7) 0.0222(6) 0.0278(7) -0.0022(5) -0.0003(6) -0.0029(5) C16 0.0294(7) 0.0289(7) 0.0226(6) 0.0050(6) -0.0017(5) -0.0050(5) C17 0.0413(8) 0.0362(8) 0.0290(8) 0.0002(7) -0.0047(7) -0.0001(7) C18 0.0496(10) 0.0397(9) 0.0265(8) 0.0068(8) -0.0027(7) 0.0038(7) C19 0.0447(9) 0.0509(10) 0.0251(8) 0.0126(8) -0.0066(7) -0.0050(7) C20 0.0334(8) 0.0528(10) 0.0365(9) 0.0009(8) -0.0081(7) -0.0094(8) C21 0.0293(7) 0.0392(8) 0.0297(7) 0.0009(7) -0.0019(6) -0.0025(7) C22A 0.0490(12) 0.0435(11) 0.0919(18) -0.0114(10) -0.0056(12) 0.0133(12) C23A 0.0462(18) 0.064(2) 0.0455(14) -0.0175(14) -0.0097(14) -0.0096(14) C24A 0.0606(16) 0.085(4) 0.0246(10) -0.002(2) -0.0024(10) 0.0034(16) C25A 0.0340(18) 0.104(4) 0.0336(19) -0.003(2) 0.0104(15) -0.004(2) C26A 0.0701(17) 0.0500(14) 0.091(3) 0.0093(13) 0.0096(18) -0.0071(16) C27A 0.0566(19) 0.075(3) 0.0678(18) 0.0185(18) -0.0306(15) -0.0038(18) C22B 0.0490(12) 0.0435(11) 0.0919(18) -0.0114(10) -0.0056(12) 0.0133(12) C23B 0.0462(18) 0.064(2) 0.0455(14) -0.0175(14) -0.0097(14) -0.0096(14) C24B 0.0606(16) 0.085(4) 0.0246(10) -0.002(2) -0.0024(10) 0.0034(16) C25B 0.103(5) 0.055(3) 0.068(4) 0.018(3) 0.045(4) 0.009(3) C26B 0.0701(17) 0.0500(14) 0.091(3) 0.0093(13) 0.0096(18) -0.0071(16) C27B 0.0566(19) 0.075(3) 0.0678(18) 0.0185(18) -0.0306(15) -0.0038(18) N1 0.0287(6) 0.0221(5) 0.0240(6) 0.0057(5) -0.0009(5) -0.0026(4) N2 0.0228(5) 0.0348(7) 0.0248(6) 0.0019(5) 0.0038(5) -0.0014(5) N3 0.0310(6) 0.0217(5) 0.0281(6) -0.0049(5) -0.0023(5) 0.0031(5) O1 0.0360(5) 0.0343(6) 0.0248(5) 0.0138(5) -0.0044(4) -0.0021(4) O2 0.0345(6) 0.0564(7) 0.0238(5) 0.0057(6) 0.0043(5) -0.0051(5) O3 0.0425(6) 0.0307(5) 0.0357(6) -0.0143(5) -0.0110(5) 0.0031(5) Si1 0.02476(18) 0.02595(19) 0.02307(18) 0.00013(15) -0.00228(15) -0.00103(15) Si2A 0.0310(4) 0.0275(4) 0.0355(4) -0.0032(3) 0.0016(3) -0.0092(3) Si3A 0.0419(4) 0.0387(4) 0.0224(4) -0.0040(4) 0.0037(3) 0.0029(3) Si4A 0.0293(4) 0.0307(4) 0.0302(4) 0.0055(3) -0.0048(3) 0.0001(3) Si2B 0.0304(5) 0.0508(6) 0.0354(5) -0.0140(4) -0.0038(4) 0.0060(5) Si3B 0.0430(5) 0.0346(5) 0.0248(4) 0.0023(4) 0.0022(4) -0.0026(4) Si4B 0.0381(5) 0.0337(5) 0.0426(6) 0.0089(4) -0.0083(4) 0.0001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 N1 . 2.0779(12) ? Zn1 N2 . 2.0880(13) ? Zn1 N3 . 2.0910(13) ? Zn1 Si1 . 2.4028(5) ? B1 C16 . 1.615(2) ? B1 C10 . 1.635(2) ? B1 C5 . 1.638(2) ? B1 C15 . 1.642(2) ? C1 C3 . 1.501(3) ? C1 H1A . 0.98 ? C1 H1B . 0.98 ? C1 H1C . 0.98 ? C2 C3 . 1.493(3) ? C2 H2A . 0.98 ? C2 H2B . 0.98 ? C2 H2C . 0.98 ? C3 N1 . 1.4884(19) ? C3 C4 . 1.519(2) ? C4 O1 . 1.458(2) ? C4 H4A . 0.99 ? C4 H4B . 0.99 ? C5 N1 . 1.2832(18) ? C5 O1 . 1.3508(18) ? C6 C7 . 1.535(4) ? C6 H6A . 0.98 ? C6 H6B . 0.98 ? C6 H6C . 0.98 ? C7 C8 . 1.467(4) ? C7 N2 . 1.483(2) ? C7 C9 . 1.517(3) ? C8 H8A . 0.98 ? C8 H8B . 0.98 ? C8 H8C . 0.98 ? C9 O2 . 1.450(2) ? C9 H9A . 0.99 ? C9 H9B . 0.99 ? C10 N2 . 1.284(2) ? C10 O2 . 1.3564(19) ? C11 C12 . 1.503(3) ? C11 H11A . 0.98 ? C11 H11B . 0.98 ? C11 H11C . 0.98 ? C12 N3 . 1.486(2) ? C12 C13 . 1.510(3) ? C12 C14 . 1.527(2) ? C13 H13A . 0.98 ? C13 H13B . 0.98 ? C13 H13C . 0.98 ? C14 O3 . 1.457(2) ? C14 H14A . 0.99 ? C14 H14B . 0.99 ? C15 N3 . 1.2870(19) ? C15 O3 . 1.3569(18) ? C16 C21 . 1.393(2) ? C16 C17 . 1.407(2) ? C17 C18 . 1.391(2) ? C17 H17 . 0.95 ? C18 C19 . 1.382(3) ? C18 H18 . 0.95 ? C19 C20 . 1.381(3) ? C19 H19 . 0.95 ? C20 C21 . 1.399(2) ? C20 H20 . 0.95 ? C21 H21 . 0.95 ? C22A Si2A . 1.756(6) ? C22A H22A . 0.98 ? C22A H22B . 0.98 ? C22A H22C . 0.98 ? C23A Si2A . 2.235(4) ? C24A Si3A . 2.039(4) ? C24A H24A . 0.98 ? C24A H24B . 0.98 ? C24A H24C . 0.98 ? C25A Si3A . 1.824(5) ? C25A H25A . 0.98 ? C25A H25B . 0.98 ? C25A H25C . 0.98 ? C26A Si4A . 1.873(5) ? C26A H26A . 0.98 ? C26A H26B . 0.98 ? C26A H26C . 0.98 ? C27A Si4A . 1.888(5) ? C27A H27A . 0.98 ? C27A H27B . 0.98 ? C27A H27C . 0.98 ? C22B Si2B . 1.966(7) ? C22B H22D . 0.98 ? C22B H22E . 0.98 ? C22B H22F . 0.98 ? C23B Si2B . 2.037(5) ? C24B Si3B . 2.087(6) ? C24B H24D . 0.98 ? C24B H24E . 0.98 ? C24B H24F . 0.98 ? C25B Si3B . 1.732(9) ? C25B H25D . 0.98 ? C25B H25E . 0.98 ? C25B H25F . 0.98 ? C26B Si4B . 1.884(8) ? C26B H26D . 0.98 ? C26B H26E . 0.98 ? C26B H26F . 0.98 ? C27B Si4B . 1.869(5) ? C27B H27D . 0.98 ? C27B H27E . 0.98 ? C27B H27F . 0.98 ? Si1 Si3A . 2.3073(10) ? Si1 Si2B . 2.3083(11) ? Si1 Si4A . 2.3430(9) ? Si1 Si2A . 2.3662(10) ? Si1 Si4B . 2.3745(11) ? Si1 Si3B . 2.3872(11) ? Si2A H21S . 1.40(4) ? Si3A H31S . 1.64(4) ? Si4A H41S . 1.43(4) ? Si2B H22S . 1.5298(19) ? Si3B H32S . 1.49(5) ? Si4B H42S . 1.531(2) ? Si4B H42S . 1.531(2) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 Zn1 N2 . . 90.66(5) ? N1 Zn1 N3 . . 90.36(5) ? N2 Zn1 N3 . . 90.45(5) ? N1 Zn1 Si1 . . 124.51(4) ? N2 Zn1 Si1 . . 124.68(4) ? N3 Zn1 Si1 . . 125.56(4) ? C16 B1 C10 . . 113.05(13) ? C16 B1 C5 . . 110.95(12) ? C10 B1 C5 . . 105.58(12) ? C16 B1 C15 . . 119.90(13) ? C10 B1 C15 . . 103.33(12) ? C5 B1 C15 . . 102.62(12) ? C3 C1 H1A . . 109.5 ? C3 C1 H1B . . 109.5 ? H1A C1 H1B . . 109.5 ? C3 C1 H1C . . 109.5 ? H1A C1 H1C . . 109.5 ? H1B C1 H1C . . 109.5 ? C3 C2 H2A . . 109.5 ? C3 C2 H2B . . 109.5 ? H2A C2 H2B . . 109.5 ? C3 C2 H2C . . 109.5 ? H2A C2 H2C . . 109.5 ? H2B C2 H2C . . 109.5 ? N1 C3 C2 . . 110.70(15) ? N1 C3 C1 . . 108.72(16) ? C2 C3 C1 . . 111.6(2) ? N1 C3 C4 . . 102.01(12) ? C2 C3 C4 . . 112.47(17) ? C1 C3 C4 . . 110.9(2) ? O1 C4 C3 . . 105.75(14) ? O1 C4 H4A . . 110.6 ? C3 C4 H4A . . 110.6 ? O1 C4 H4B . . 110.6 ? C3 C4 H4B . . 110.6 ? H4A C4 H4B . . 108.7 ? N1 C5 O1 . . 115.52(13) ? N1 C5 B1 . . 125.41(13) ? O1 C5 B1 . . 119.04(12) ? C7 C6 H6A . . 109.5 ? C7 C6 H6B . . 109.5 ? H6A C6 H6B . . 109.5 ? C7 C6 H6C . . 109.5 ? H6A C6 H6C . . 109.5 ? H6B C6 H6C . . 109.5 ? C8 C7 N2 . . 110.7(2) ? C8 C7 C9 . . 111.5(2) ? N2 C7 C9 . . 102.57(14) ? C8 C7 C6 . . 112.2(3) ? N2 C7 C6 . . 108.07(19) ? C9 C7 C6 . . 111.3(2) ? C7 C8 H8A . . 109.5 ? C7 C8 H8B . . 109.5 ? H8A C8 H8B . . 109.5 ? C7 C8 H8C . . 109.5 ? H8A C8 H8C . . 109.5 ? H8B C8 H8C . . 109.5 ? O2 C9 C7 . . 105.63(14) ? O2 C9 H9A . . 110.6 ? C7 C9 H9A . . 110.6 ? O2 C9 H9B . . 110.6 ? C7 C9 H9B . . 110.6 ? H9A C9 H9B . . 108.7 ? N2 C10 O2 . . 115.65(14) ? N2 C10 B1 . . 125.30(13) ? O2 C10 B1 . . 119.03(13) ? C12 C11 H11A . . 109.5 ? C12 C11 H11B . . 109.5 ? H11A C11 H11B . . 109.5 ? C12 C11 H11C . . 109.5 ? H11A C11 H11C . . 109.5 ? H11B C11 H11C . . 109.5 ? N3 C12 C11 . . 109.30(15) ? N3 C12 C13 . . 110.70(16) ? C11 C12 C13 . . 110.6(2) ? N3 C12 C14 . . 102.17(13) ? C11 C12 C14 . . 112.12(17) ? C13 C12 C14 . . 111.60(17) ? 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 ? O3 C14 C12 . . 105.73(14) ? O3 C14 H14A . . 110.6 ? C12 C14 H14A . . 110.6 ? O3 C14 H14B . . 110.6 ? C12 C14 H14B . . 110.6 ? H14A C14 H14B . . 108.7 ? N3 C15 O3 . . 115.47(13) ? N3 C15 B1 . . 122.69(13) ? O3 C15 B1 . . 121.80(13) ? C21 C16 C17 . . 115.96(14) ? C21 C16 B1 . . 125.88(14) ? C17 C16 B1 . . 118.09(14) ? C18 C17 C16 . . 122.60(17) ? C18 C17 H17 . . 118.7 ? C16 C17 H17 . . 118.7 ? C19 C18 C17 . . 119.90(17) ? C19 C18 H18 . . 120.0 ? C17 C18 H18 . . 120.0 ? C20 C19 C18 . . 119.07(16) ? C20 C19 H19 . . 120.5 ? C18 C19 H19 . . 120.5 ? C19 C20 C21 . . 120.69(17) ? C19 C20 H20 . . 119.7 ? C21 C20 H20 . . 119.7 ? C16 C21 C20 . . 121.78(17) ? C16 C21 H21 . . 119.1 ? C20 C21 H21 . . 119.1 ? Si2A C22A H22A . . 109.5 ? Si2A C22A H22B . . 109.5 ? H22A C22A H22B . . 109.5 ? Si2A C22A H22C . . 109.5 ? H22A C22A H22C . . 109.5 ? H22B C22A H22C . . 109.5 ? Si3A C24A H24A . . 109.5 ? Si3A C24A H24B . . 109.5 ? H24A C24A H24B . . 109.5 ? Si3A C24A H24C . . 109.5 ? H24A C24A H24C . . 109.5 ? H24B C24A H24C . . 109.5 ? Si3A C25A H25A . . 109.5 ? Si3A C25A H25B . . 109.5 ? H25A C25A H25B . . 109.5 ? Si3A C25A H25C . . 109.5 ? H25A C25A H25C . . 109.5 ? H25B C25A H25C . . 109.5 ? Si4A C26A H26A . . 109.5 ? Si4A C26A H26B . . 109.5 ? H26A C26A H26B . . 109.5 ? Si4A C26A H26C . . 109.5 ? H26A C26A H26C . . 109.5 ? H26B C26A H26C . . 109.5 ? Si4A C27A H27A . . 109.5 ? Si4A C27A H27B . . 109.5 ? H27A C27A H27B . . 109.5 ? Si4A C27A H27C . . 109.5 ? H27A C27A H27C . . 109.5 ? H27B C27A H27C . . 109.5 ? Si2B C22B H22D . . 109.5 ? Si2B C22B H22E . . 109.5 ? H22D C22B H22E . . 109.5 ? Si2B C22B H22F . . 109.5 ? H22D C22B H22F . . 109.5 ? H22E C22B H22F . . 109.5 ? Si3B C24B H24D . . 109.5 ? Si3B C24B H24E . . 109.5 ? H24D C24B H24E . . 109.5 ? Si3B C24B H24F . . 109.5 ? H24D C24B H24F . . 109.5 ? H24E C24B H24F . . 109.5 ? Si3B C25B H25D . . 109.5 ? Si3B C25B H25E . . 109.5 ? H25D C25B H25E . . 109.5 ? Si3B C25B H25F . . 109.5 ? H25D C25B H25F . . 109.5 ? H25E C25B H25F . . 109.5 ? Si4B C26B H26D . . 109.5 ? Si4B C26B H26E . . 109.5 ? H26D C26B H26E . . 109.5 ? Si4B C26B H26F . . 109.5 ? H26D C26B H26F . . 109.5 ? H26E C26B H26F . . 109.5 ? Si4B C27B H27D . . 109.5 ? Si4B C27B H27E . . 109.5 ? H27D C27B H27E . . 109.5 ? Si4B C27B H27F . . 109.5 ? H27D C27B H27F . . 109.5 ? H27E C27B H27F . . 109.5 ? C5 N1 C3 . . 109.69(12) ? C5 N1 Zn1 . . 114.39(10) ? C3 N1 Zn1 . . 135.76(10) ? C10 N2 C7 . . 109.11(13) ? C10 N2 Zn1 . . 114.20(11) ? C7 N2 Zn1 . . 135.80(11) ? C15 N3 C12 . . 109.77(12) ? C15 N3 Zn1 . . 116.34(10) ? C12 N3 Zn1 . . 133.65(10) ? C5 O1 C4 . . 106.78(12) ? C10 O2 C9 . . 106.68(13) ? C15 O3 C14 . . 106.85(12) ? Si3A Si1 Si2B . . 124.02(4) ? Si3A Si1 Si4A . . 105.45(4) ? Si2B Si1 Si4A . . 72.17(4) ? Si3A Si1 Si2A . . 105.29(4) ? Si2B Si1 Si2A . . 33.75(4) ? Si4A Si1 Si2A . . 104.21(3) ? Si3A Si1 Si4B . . 73.77(4) ? Si2B Si1 Si4B . . 104.90(4) ? Si4A Si1 Si4B . . 36.63(3) ? Si2A Si1 Si4B . . 130.53(4) ? Si3A Si1 Si3B . . 31.04(4) ? Si2B Si1 Si3B . . 104.27(4) ? Si4A Si1 Si3B . . 125.71(4) ? Si2A Si1 Si3B . . 77.17(4) ? Si4B Si1 Si3B . . 101.92(4) ? Si3A Si1 Zn1 . . 118.10(3) ? Si2B Si1 Zn1 . . 113.27(3) ? Si4A Si1 Zn1 . . 112.79(3) ? Si2A Si1 Zn1 . . 109.88(3) ? Si4B Si1 Zn1 . . 113.58(3) ? Si3B Si1 Zn1 . . 117.45(3) ? C22A Si2A C23A . . 99.2(2) ? C22A Si2A Si1 . . 115.84(18) ? C23A Si2A Si1 . . 103.41(12) ? C22A Si2A H21S . . 109.0(15) ? C23A Si2A H21S . . 129.0(14) ? Si1 Si2A H21S . . 101.2(15) ? C25A Si3A C24A . . 98.6(2) ? C25A Si3A Si1 . . 118.13(16) ? C24A Si3A Si1 . . 111.26(14) ? C25A Si3A H31S . . 108.7(13) ? C24A Si3A H31S . . 114.3(12) ? Si1 Si3A H31S . . 106.1(13) ? C26A Si4A C27A . . 103.3(2) ? C26A Si4A Si1 . . 112.07(19) ? C27A Si4A Si1 . . 114.74(16) ? C26A Si4A H41S . . 111.5(15) ? C27A Si4A H41S . . 105.4(14) ? Si1 Si4A H41S . . 109.5(15) ? C22B Si2B C23B . . 95.8(3) ? C22B Si2B Si1 . . 110.5(2) ? C23B Si2B Si1 . . 111.14(15) ? C22B Si2B H22S . . 104.1(4) ? C23B Si2B H22S . . 130.0(2) ? Si1 Si2B H22S . . 104.0(2) ? C25B Si3B C24B . . 106.3(3) ? C25B Si3B Si1 . . 116.9(3) ? C24B Si3B Si1 . . 104.50(17) ? C25B Si3B H32S . . 98.5(16) ? C24B Si3B H32S . . 123.4(16) ? Si1 Si3B H32S . . 107.9(17) ? H42S Si4B C27B . . 103.5(3) ? H42S Si4B C26B . . 112.4(3) ? C27B Si4B C26B . . 100.2(3) ? H42S Si4B Si1 . . 113.95(18) ? C27B Si4B Si1 . . 114.7(2) ? C26B Si4B Si1 . . 111.2(2) ? H42S Si4B H42S . . 0.0(3) ? C27B Si4B H42S . . 103.5(3) ? C26B Si4B H42S . . 112.4(3) ? Si1 Si4B H42S . . 113.95(18) ? data_Ic _database_code_depnum_ccdc_archive 'CCDC 902696' #TrackingRef 'web_deposit_cif_file_3_AaronD.Sadow_1348401140.ToMZnSi(SiMe3)3.cif' _audit_creation_method 'APEX2 v2010.11-3' _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H56 B N3 O3 Si4 Zn' _chemical_formula_iupac ? _chemical_formula_weight 695.32 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.242(4) _cell_length_b 11.576(4) _cell_length_c 17.786(7) _cell_angle_alpha 92.073(6) _cell_angle_beta 106.240(6) _cell_angle_gamma 103.685(6) _cell_volume 1955.2(13) _cell_formula_units_Z 2 _cell_measurement_reflns_used 1732 _cell_measurement_theta_min 2.3999 _cell_measurement_theta_max 20.7061 _cell_measurement_temperature 173.(2) _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.181 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 0.782 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.95 _exptl_special_details ; A X-ray quality crystal was selected under ambient conditions and covered with PARATONE oil The crystal was mounted and centered in the X-ray beam by using a video camera.The crystal evaluation and data collection were performed on APEX-2 CCD diffractometer with the detector to crystal distance of 5cm. The initial cell constants were obtained from three series of OMEGA scans at different starting angles. Each series consisted of 30 frames collected at intervals of 0.3 in a 10 range about OMEGA with the exposure time of 10 seconds per frame. The obtained reflections were successfully indexed by an automated indexing routine built to APEX2 program package. The final cell constants were calculated from a set of strong reflections from the actual data collection. The data were collected using the full sphere routine by collecting four sets of frames with 0.3 scans in \w with an exposure time 10 sec per frame. This dataset was corrected for Lorentz and polarization effects. The absorption correction was based on a fit of a spherical harmonic function to the empirical transmission surface as sampled by multiple equivalent measurements using SADABS software. ; _diffrn_ambient_temperature 173.(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source ? _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ' BRUKER APEX2 CCD Diffractometer' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 15694 _diffrn_reflns_av_R_equivalents 0.0690 _diffrn_reflns_av_sigmaI/netI 0.1050 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 25.18 _diffrn_reflns_theta_full 25.18 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _refine_special_details ; The systematic absences in the diffraction data were consistent for the stated space group. The position of almost all non-hydrogen atoms were found by direct methods. The remaining atoms were located in an alternating series of least-squares cycles on difference Fourier maps. All non-hydrogen atoms were refined in full-matrix anisotropic approximation. All hydrogen atoms were placed in the structure factor calculation at idealized positions and were allowed to ride on the neighboring atoms with relative isotropic displacement coefficients. Final results were tested with CHECKCIF routine and all A-warnings (if any) were addressed on the very top of this file. ; _reflns_number_total 6954 _reflns_number_gt 4382 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_gt 0.0783 _refine_ls_wR_factor_ref 0.0919 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _refine_ls_number_reflns 6954 _refine_ls_number_parameters 394 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.363 _refine_diff_density_min -0.515 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' _computing_data_collection 'APEX2 Suite (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT V7.66A (Bruker AXS, 2009)' _computing_data_reduction 'SAINT V7.66A (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XSHELL (Bruker AXS, 2007)' _computing_publication_material 'APEX2 Suite (Bruker AXS, 2009)' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn1 0.48329(4) 0.26330(3) 0.28891(2) 0.02104(12) Uani d . 1 . . B B1 0.6981(4) 0.2095(3) 0.4425(2) 0.0223(10) Uani d . 1 . . C C1 0.5980(4) 0.0120(3) 0.1928(2) 0.0438(11) Uani d . 1 . . H H1A 0.5692 0.0749 0.1618 0.066 Uiso calc R 1 . . H H1B 0.5765 -0.0617 0.1578 0.066 Uiso calc R 1 . . H H1C 0.6994 0.0375 0.2196 0.066 Uiso calc R 1 . . C C2 0.5185(4) -0.0106(3) 0.2539(2) 0.0248(9) Uani d . 1 . . C C3 0.3624(4) -0.0586(3) 0.2165(2) 0.0358(10) Uani d . 1 . . H H3A 0.3157 -0.0722 0.2577 0.054 Uiso calc R 1 . . H H3B 0.3438 -0.1343 0.184 0.054 Uiso calc R 1 . . H H3C 0.3259 -0.0006 0.1834 0.054 Uiso calc R 1 . . C C4 0.5795(4) -0.0897(3) 0.3146(2) 0.0344(10) Uani d . 1 . . H H4A 0.5037 -0.1455 0.3294 0.041 Uiso calc R 1 . . H H4B 0.633 -0.1367 0.2933 0.041 Uiso calc R 1 . . C C5 0.6356(4) 0.0999(3) 0.3715(2) 0.0211(8) Uani d . 1 . . C C6 0.7754(4) 0.4916(3) 0.2437(2) 0.0325(10) Uani d . 1 . . H H6A 0.8132 0.4287 0.2263 0.049 Uiso calc R 1 . . H H6B 0.8348 0.5701 0.2406 0.049 Uiso calc R 1 . . H H6C 0.6794 0.4832 0.2096 0.049 Uiso calc R 1 . . C C7 0.7733(3) 0.4805(3) 0.3278(2) 0.0228(8) Uani d . 1 . . C C8 0.7069(4) 0.5711(3) 0.3567(2) 0.0377(10) Uani d . 1 . . H H8A 0.6072 0.5539 0.3263 0.057 Uiso calc R 1 . . H H8B 0.7554 0.6519 0.3496 0.057 Uiso calc R 1 . . H H8C 0.7152 0.5658 0.4126 0.057 Uiso calc R 1 . . C C9 0.9178(4) 0.4853(3) 0.3841(2) 0.0342(10) Uani d . 1 . . H H9A 0.9808 0.4656 0.3552 0.041 Uiso calc R 1 . . H H9B 0.962 0.5657 0.4138 0.041 Uiso calc R 1 . . C C10 0.7585(4) 0.3248(3) 0.4007(2) 0.0207(8) Uani d . 1 . . C C11 0.2738(4) 0.3598(3) 0.4145(2) 0.0397(11) Uani d . 1 . . H H11A 0.3472 0.4315 0.4418 0.06 Uiso calc R 1 . . H H11B 0.1925 0.3519 0.4344 0.06 Uiso calc R 1 . . H H11C 0.245 0.3668 0.3578 0.06 Uiso calc R 1 . . C C12 0.3307(4) 0.2503(3) 0.4290(2) 0.0246(9) Uani d . 1 . . C C13 0.2221(4) 0.1369(3) 0.3858(2) 0.0458(11) Uani d . 1 . . H H13A 0.1995 0.1416 0.3288 0.069 Uiso calc R 1 . . H H13B 0.1366 0.1285 0.4019 0.069 Uiso calc R 1 . . H H13C 0.2601 0.0676 0.3987 0.069 Uiso calc R 1 . . C C14 0.3919(4) 0.2393(4) 0.5164(2) 0.0446(12) Uani d . 1 . . H H14A 0.4112 0.3165 0.5485 0.053 Uiso calc R 1 . . H H14B 0.3259 0.1777 0.5347 0.053 Uiso calc R 1 . . C C15 0.5537(4) 0.2304(3) 0.4546(2) 0.0229(8) Uani d . 1 . . C C16 0.8146(4) 0.1886(3) 0.5197(2) 0.0230(8) Uani d . 1 . . C C17 0.9263(4) 0.1445(3) 0.5115(2) 0.0296(9) Uani d . 1 . . H H17 0.931 0.1262 0.46 0.036 Uiso calc R 1 . . C C18 1.0305(4) 0.1264(3) 0.5754(2) 0.0334(10) Uani d . 1 . . H H18 1.104 0.0955 0.5672 0.04 Uiso calc R 1 . . C C19 1.0276(4) 0.1530(3) 0.6509(2) 0.0377(10) Uani d . 1 . . H H19 1.0975 0.1389 0.6949 0.045 Uiso calc R 1 . . C C20 0.9228(4) 0.2000(3) 0.6617(2) 0.0349(10) Uani d . 1 . . H H20 0.9213 0.2207 0.7136 0.042 Uiso calc R 1 . . C C21 0.8181(4) 0.2177(3) 0.5972(2) 0.0300(9) Uani d . 1 . . H H21 0.7466 0.2507 0.6063 0.036 Uiso calc R 1 . . C C22 0.2941(4) 0.0971(3) 0.0191(2) 0.0449(11) Uani d . 1 . . H H22A 0.1946 0.0694 0.0163 0.067 Uiso calc R 1 . . H H22B 0.3488 0.0525 0.0556 0.067 Uiso calc R 1 . . H H22C 0.3047 0.0838 -0.0334 0.067 Uiso calc R 1 . . C C23 0.2730(5) 0.3392(4) -0.0284(2) 0.0490(12) Uani d . 1 . . H H23A 0.295 0.3167 -0.0761 0.073 Uiso calc R 1 . . H H23B 0.3078 0.426 -0.0145 0.073 Uiso calc R 1 . . H H23C 0.1708 0.3156 -0.0378 0.073 Uiso calc R 1 . . C C24 0.5528(4) 0.3025(4) 0.0649(2) 0.0437(11) Uani d . 1 . . H H24A 0.5678 0.2701 0.0172 0.066 Uiso calc R 1 . . H H24B 0.603 0.269 0.1106 0.066 Uiso calc R 1 . . H H24C 0.5882 0.3898 0.0719 0.066 Uiso calc R 1 . . C C25 0.2943(4) 0.5740(3) 0.2704(2) 0.0388(10) Uani d . 1 . . H H25A 0.3764 0.5672 0.3126 0.058 Uiso calc R 1 . . H H25B 0.2081 0.5315 0.2815 0.058 Uiso calc R 1 . . H H25C 0.2955 0.6586 0.2672 0.058 Uiso calc R 1 . . C C26 0.4525(4) 0.6069(3) 0.1501(2) 0.0396(11) Uani d . 1 . . H H26A 0.4333 0.6849 0.1402 0.059 Uiso calc R 1 . . H H26B 0.4659 0.5708 0.1031 0.059 Uiso calc R 1 . . H H26C 0.5379 0.6175 0.1946 0.059 Uiso calc R 1 . . C C27 0.1387(4) 0.5282(3) 0.0998(2) 0.0520(13) Uani d . 1 . . H H27A 0.1423 0.6136 0.1009 0.078 Uiso calc R 1 . . H H27B 0.0544 0.4851 0.1126 0.078 Uiso calc R 1 . . H H27C 0.1353 0.4971 0.0471 0.078 Uiso calc R 1 . . C C28 -0.0338(4) 0.2077(3) 0.0444(2) 0.0466(12) Uani d . 1 . . H H28A -0.1325 0.1661 0.0364 0.07 Uiso calc R 1 . . H H28B 0.0024 0.17 0.0071 0.07 Uiso calc R 1 . . H H28C -0.0265 0.2918 0.0355 0.07 Uiso calc R 1 . . C C29 0.0402(4) 0.0351(3) 0.1600(2) 0.0373(10) Uani d . 1 . . H H29A 0.0907 0.0245 0.2139 0.056 Uiso calc R 1 . . H H29B 0.0739 -0.0048 0.1225 0.056 Uiso calc R 1 . . H H29C -0.0609 0.0001 0.15 0.056 Uiso calc R 1 . . C C30 -0.0147(4) 0.2628(4) 0.2133(2) 0.0449(11) Uani d . 1 . . H H30A 0.0105 0.3502 0.2154 0.067 Uiso calc R 1 . . H H30B 0.0169 0.2395 0.2664 0.067 Uiso calc R 1 . . H H30C -0.1171 0.232 0.192 0.067 Uiso calc R 1 . . N N1 0.5491(3) 0.1037(2) 0.30437(16) 0.0227(7) Uani d . 1 . . N N2 0.6915(3) 0.3597(2) 0.33739(16) 0.0211(7) Uani d . 1 . . N N3 0.4580(3) 0.2620(2) 0.40205(16) 0.0230(7) Uani d . 1 . . O O1 0.6719(2) -0.00589(19) 0.38194(13) 0.0275(6) Uani d . 1 . . O O2 0.8893(2) 0.3951(2) 0.43721(13) 0.0297(6) Uani d . 1 . . O O3 0.5205(2) 0.2050(2) 0.52239(14) 0.0300(6) Uani d . 1 . . Si Si1 0.31257(11) 0.30394(8) 0.17448(6) 0.0248(3) Uani d . 1 . . Si Si2 0.35984(12) 0.26128(9) 0.05495(6) 0.0325(3) Uani d . 1 . . Si Si3 0.29988(12) 0.50644(9) 0.17421(6) 0.0303(3) Uani d . 1 . . Si Si4 0.07241(11) 0.19880(9) 0.14801(6) 0.0320(3) Uani d . 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zn1 0.0219(2) 0.0174(2) 0.0213(2) 0.00341(18) 0.0036(2) 0.00429(18) B1 0.023(2) 0.021(2) 0.019(2) 0.0036(19) 0.0018(19) 0.0059(18) C1 0.051(3) 0.042(3) 0.040(3) 0.010(2) 0.019(2) 0.002(2) C2 0.025(2) 0.022(2) 0.026(2) 0.0079(17) 0.0046(18) 0.0013(17) C3 0.033(2) 0.025(2) 0.041(3) 0.0015(19) 0.002(2) 0.0010(19) C4 0.043(3) 0.017(2) 0.035(2) 0.0050(19) 0.001(2) -0.0050(18) C5 0.021(2) 0.0181(19) 0.027(2) 0.0062(16) 0.0100(18) 0.0089(16) C6 0.037(2) 0.029(2) 0.032(2) 0.0093(19) 0.010(2) 0.0093(18) C7 0.021(2) 0.0196(19) 0.023(2) -0.0010(16) 0.0044(17) 0.0028(16) C8 0.047(3) 0.027(2) 0.039(3) 0.005(2) 0.018(2) -0.0025(19) C9 0.033(2) 0.030(2) 0.029(2) -0.0060(19) 0.0027(19) 0.0113(18) C10 0.019(2) 0.0167(19) 0.024(2) 0.0020(16) 0.0040(17) -0.0020(16) C11 0.041(3) 0.045(3) 0.040(3) 0.022(2) 0.014(2) 0.006(2) C12 0.026(2) 0.031(2) 0.023(2) 0.0121(18) 0.0116(18) 0.0114(17) C13 0.034(3) 0.039(3) 0.060(3) 0.001(2) 0.013(2) 0.010(2) C14 0.037(3) 0.077(3) 0.037(3) 0.033(2) 0.020(2) 0.023(2) C15 0.032(2) 0.0161(19) 0.019(2) 0.0012(17) 0.0101(18) 0.0040(16) C16 0.024(2) 0.0153(19) 0.026(2) 0.0010(16) 0.0042(17) 0.0051(16) C17 0.026(2) 0.030(2) 0.030(2) 0.0045(18) 0.0071(19) 0.0040(18) C18 0.023(2) 0.027(2) 0.047(3) 0.0062(18) 0.004(2) 0.006(2) C19 0.025(2) 0.043(3) 0.035(3) 0.002(2) -0.003(2) 0.015(2) C20 0.027(2) 0.044(3) 0.025(2) -0.003(2) 0.003(2) 0.0066(19) C21 0.023(2) 0.036(2) 0.030(2) 0.0098(18) 0.0037(19) 0.0026(18) C22 0.054(3) 0.042(3) 0.028(2) 0.002(2) 0.004(2) -0.006(2) C23 0.064(3) 0.047(3) 0.031(3) 0.010(2) 0.009(2) 0.016(2) C24 0.054(3) 0.044(3) 0.034(3) 0.005(2) 0.021(2) 0.006(2) C25 0.044(3) 0.026(2) 0.047(3) 0.009(2) 0.014(2) 0.0052(19) C26 0.053(3) 0.026(2) 0.042(3) 0.013(2) 0.014(2) 0.0103(19) C27 0.053(3) 0.036(3) 0.058(3) 0.021(2) -0.006(2) 0.014(2) C28 0.041(3) 0.035(2) 0.046(3) 0.001(2) -0.009(2) 0.009(2) C29 0.032(2) 0.032(2) 0.042(3) 0.0040(19) 0.004(2) 0.0044(19) C30 0.021(2) 0.051(3) 0.060(3) 0.010(2) 0.006(2) 0.002(2) N1 0.0254(18) 0.0146(16) 0.0221(17) 0.0018(13) 0.0007(15) 0.0003(13) N2 0.0184(17) 0.0179(16) 0.0220(17) -0.0010(13) 0.0029(14) 0.0021(13) N3 0.0206(17) 0.0242(17) 0.0260(18) 0.0066(14) 0.0085(15) 0.0079(14) O1 0.0286(15) 0.0193(14) 0.0288(15) 0.0069(12) -0.0012(12) 0.0021(11) O2 0.0223(15) 0.0280(14) 0.0274(15) -0.0058(12) -0.0010(12) 0.0075(12) O3 0.0263(15) 0.0453(16) 0.0252(15) 0.0156(13) 0.0113(12) 0.0172(12) Si1 0.0277(6) 0.0195(5) 0.0234(6) 0.0055(5) 0.0017(5) 0.0053(4) Si2 0.0422(7) 0.0274(6) 0.0213(6) 0.0016(5) 0.0047(5) 0.0037(5) Si3 0.0363(7) 0.0204(6) 0.0307(6) 0.0088(5) 0.0025(5) 0.0060(5) Si4 0.0259(6) 0.0270(6) 0.0361(7) 0.0049(5) -0.0005(5) 0.0028(5) _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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 N2 . 2.076(3) ? Zn1 N3 . 2.100(3) ? Zn1 N1 . 2.113(3) ? Zn1 Si1 . 2.4266(12) ? B1 C16 . 1.616(5) ? B1 C15 . 1.623(5) ? B1 C10 . 1.629(5) ? B1 C5 . 1.631(5) ? C1 C2 . 1.525(5) ? C1 H1A . 0.98 ? C1 H1B . 0.98 ? C1 H1C . 0.98 ? C2 N1 . 1.489(4) ? C2 C3 . 1.506(5) ? C2 C4 . 1.535(5) ? C3 H3A . 0.98 ? C3 H3B . 0.98 ? C3 H3C . 0.98 ? C4 O1 . 1.456(4) ? C4 H4A . 0.99 ? C4 H4B . 0.99 ? C5 N1 . 1.282(4) ? C5 O1 . 1.366(4) ? C6 C7 . 1.511(5) ? C6 H6A . 0.98 ? C6 H6B . 0.98 ? C6 H6C . 0.98 ? C7 N2 . 1.493(4) ? C7 C8 . 1.524(5) ? C7 C9 . 1.525(5) ? C8 H8A . 0.98 ? C8 H8B . 0.98 ? C8 H8C . 0.98 ? C9 O2 . 1.466(4) ? C9 H9A . 0.99 ? C9 H9B . 0.99 ? C10 N2 . 1.279(4) ? C10 O2 . 1.355(4) ? C11 C12 . 1.518(5) ? C11 H11A . 0.98 ? C11 H11B . 0.98 ? C11 H11C . 0.98 ? C12 N3 . 1.489(4) ? C12 C13 . 1.519(5) ? C12 C14 . 1.528(5) ? C13 H13A . 0.98 ? C13 H13B . 0.98 ? C13 H13C . 0.98 ? C14 O3 . 1.442(4) ? C14 H14A . 0.99 ? C14 H14B . 0.99 ? C15 N3 . 1.285(4) ? C15 O3 . 1.364(4) ? C16 C21 . 1.396(5) ? C16 C17 . 1.398(5) ? C17 C18 . 1.386(5) ? C17 H17 . 0.95 ? C18 C19 . 1.376(5) ? C18 H18 . 0.95 ? C19 C20 . 1.368(5) ? C19 H19 . 0.95 ? C20 C21 . 1.393(5) ? C20 H20 . 0.95 ? C21 H21 . 0.95 ? C22 Si2 . 1.881(4) ? C22 H22A . 0.98 ? C22 H22B . 0.98 ? C22 H22C . 0.98 ? C23 Si2 . 1.882(4) ? C23 H23A . 0.98 ? C23 H23B . 0.98 ? C23 H23C . 0.98 ? C24 Si2 . 1.875(4) ? C24 H24A . 0.98 ? C24 H24B . 0.98 ? C24 H24C . 0.98 ? C25 Si3 . 1.876(4) ? C25 H25A . 0.98 ? C25 H25B . 0.98 ? C25 H25C . 0.98 ? C26 Si3 . 1.879(4) ? C26 H26A . 0.98 ? C26 H26B . 0.98 ? C26 H26C . 0.98 ? C27 Si3 . 1.881(4) ? C27 H27A . 0.98 ? C27 H27B . 0.98 ? C27 H27C . 0.98 ? C28 Si4 . 1.881(4) ? C28 H28A . 0.98 ? C28 H28B . 0.98 ? C28 H28C . 0.98 ? C29 Si4 . 1.876(4) ? C29 H29A . 0.98 ? C29 H29B . 0.98 ? C29 H29C . 0.98 ? C30 Si4 . 1.877(4) ? C30 H30A . 0.98 ? C30 H30B . 0.98 ? C30 H30C . 0.98 ? Si1 Si2 . 2.3687(17) ? Si1 Si4 . 2.3764(17) ? Si1 Si3 . 2.3784(16) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N2 Zn1 N3 . . 89.69(11) ? N2 Zn1 N1 . . 88.88(11) ? N3 Zn1 N1 . . 89.07(11) ? N2 Zn1 Si1 . . 126.98(8) ? N3 Zn1 Si1 . . 123.69(8) ? N1 Zn1 Si1 . . 126.76(8) ? C16 B1 C15 . . 117.1(3) ? C16 B1 C10 . . 112.5(3) ? C15 B1 C10 . . 104.7(3) ? C16 B1 C5 . . 115.8(3) ? C15 B1 C5 . . 101.0(3) ? C10 B1 C5 . . 104.2(3) ? C2 C1 H1A . . 109.5 ? C2 C1 H1B . . 109.5 ? H1A C1 H1B . . 109.5 ? C2 C1 H1C . . 109.5 ? H1A C1 H1C . . 109.5 ? H1B C1 H1C . . 109.5 ? N1 C2 C3 . . 110.4(3) ? N1 C2 C1 . . 108.3(3) ? C3 C2 C1 . . 112.2(3) ? N1 C2 C4 . . 101.3(3) ? C3 C2 C4 . . 112.2(3) ? C1 C2 C4 . . 111.8(3) ? C2 C3 H3A . . 109.5 ? C2 C3 H3B . . 109.5 ? H3A C3 H3B . . 109.5 ? C2 C3 H3C . . 109.5 ? H3A C3 H3C . . 109.5 ? H3B C3 H3C . . 109.5 ? O1 C4 C2 . . 104.6(3) ? O1 C4 H4A . . 110.8 ? C2 C4 H4A . . 110.8 ? O1 C4 H4B . . 110.8 ? C2 C4 H4B . . 110.8 ? H4A C4 H4B . . 108.9 ? N1 C5 O1 . . 115.3(3) ? N1 C5 B1 . . 124.3(3) ? O1 C5 B1 . . 120.3(3) ? C7 C6 H6A . . 109.5 ? C7 C6 H6B . . 109.5 ? H6A C6 H6B . . 109.5 ? C7 C6 H6C . . 109.5 ? H6A C6 H6C . . 109.5 ? H6B C6 H6C . . 109.5 ? N2 C7 C6 . . 112.1(3) ? N2 C7 C8 . . 106.7(3) ? C6 C7 C8 . . 112.1(3) ? N2 C7 C9 . . 100.9(3) ? C6 C7 C9 . . 112.9(3) ? C8 C7 C9 . . 111.5(3) ? C7 C8 H8A . . 109.5 ? C7 C8 H8B . . 109.5 ? H8A C8 H8B . . 109.5 ? C7 C8 H8C . . 109.5 ? H8A C8 H8C . . 109.5 ? H8B C8 H8C . . 109.5 ? O2 C9 C7 . . 104.3(3) ? O2 C9 H9A . . 110.9 ? C7 C9 H9A . . 110.9 ? O2 C9 H9B . . 110.9 ? C7 C9 H9B . . 110.9 ? H9A C9 H9B . . 108.9 ? N2 C10 O2 . . 115.5(3) ? N2 C10 B1 . . 126.0(3) ? O2 C10 B1 . . 118.3(3) ? C12 C11 H11A . . 109.5 ? C12 C11 H11B . . 109.5 ? H11A C11 H11B . . 109.5 ? C12 C11 H11C . . 109.5 ? H11A C11 H11C . . 109.5 ? H11B C11 H11C . . 109.5 ? N3 C12 C11 . . 110.7(3) ? N3 C12 C13 . . 108.2(3) ? C11 C12 C13 . . 111.5(3) ? N3 C12 C14 . . 100.6(3) ? C11 C12 C14 . . 113.0(3) ? C13 C12 C14 . . 112.2(3) ? 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 ? O3 C14 C12 . . 105.0(3) ? O3 C14 H14A . . 110.7 ? C12 C14 H14A . . 110.7 ? O3 C14 H14B . . 110.7 ? C12 C14 H14B . . 110.7 ? H14A C14 H14B . . 108.8 ? N3 C15 O3 . . 114.4(3) ? N3 C15 B1 . . 125.0(3) ? O3 C15 B1 . . 120.3(3) ? C21 C16 C17 . . 115.2(3) ? C21 C16 B1 . . 124.6(3) ? C17 C16 B1 . . 120.1(3) ? C18 C17 C16 . . 122.7(4) ? C18 C17 H17 . . 118.6 ? C16 C17 H17 . . 118.6 ? C19 C18 C17 . . 120.2(4) ? C19 C18 H18 . . 119.9 ? C17 C18 H18 . . 119.9 ? C20 C19 C18 . . 119.1(4) ? C20 C19 H19 . . 120.5 ? C18 C19 H19 . . 120.5 ? C19 C20 C21 . . 120.5(4) ? C19 C20 H20 . . 119.8 ? C21 C20 H20 . . 119.8 ? C20 C21 C16 . . 122.3(4) ? C20 C21 H21 . . 118.9 ? C16 C21 H21 . . 118.9 ? Si2 C22 H22A . . 109.5 ? Si2 C22 H22B . . 109.5 ? H22A C22 H22B . . 109.5 ? Si2 C22 H22C . . 109.5 ? H22A C22 H22C . . 109.5 ? H22B C22 H22C . . 109.5 ? Si2 C23 H23A . . 109.5 ? Si2 C23 H23B . . 109.5 ? H23A C23 H23B . . 109.5 ? Si2 C23 H23C . . 109.5 ? H23A C23 H23C . . 109.5 ? H23B C23 H23C . . 109.5 ? Si2 C24 H24A . . 109.5 ? Si2 C24 H24B . . 109.5 ? H24A C24 H24B . . 109.5 ? Si2 C24 H24C . . 109.5 ? H24A C24 H24C . . 109.5 ? H24B C24 H24C . . 109.5 ? Si3 C25 H25A . . 109.5 ? Si3 C25 H25B . . 109.5 ? H25A C25 H25B . . 109.5 ? Si3 C25 H25C . . 109.5 ? H25A C25 H25C . . 109.5 ? H25B C25 H25C . . 109.5 ? Si3 C26 H26A . . 109.5 ? Si3 C26 H26B . . 109.5 ? H26A C26 H26B . . 109.5 ? Si3 C26 H26C . . 109.5 ? H26A C26 H26C . . 109.5 ? H26B C26 H26C . . 109.5 ? Si3 C27 H27A . . 109.5 ? Si3 C27 H27B . . 109.5 ? H27A C27 H27B . . 109.5 ? Si3 C27 H27C . . 109.5 ? H27A C27 H27C . . 109.5 ? H27B C27 H27C . . 109.5 ? Si4 C28 H28A . . 109.5 ? Si4 C28 H28B . . 109.5 ? H28A C28 H28B . . 109.5 ? Si4 C28 H28C . . 109.5 ? H28A C28 H28C . . 109.5 ? H28B C28 H28C . . 109.5 ? Si4 C29 H29A . . 109.5 ? Si4 C29 H29B . . 109.5 ? H29A C29 H29B . . 109.5 ? Si4 C29 H29C . . 109.5 ? H29A C29 H29C . . 109.5 ? H29B C29 H29C . . 109.5 ? Si4 C30 H30A . . 109.5 ? Si4 C30 H30B . . 109.5 ? H30A C30 H30B . . 109.5 ? Si4 C30 H30C . . 109.5 ? H30A C30 H30C . . 109.5 ? H30B C30 H30C . . 109.5 ? C5 N1 C2 . . 109.4(3) ? C5 N1 Zn1 . . 116.0(2) ? C2 N1 Zn1 . . 134.6(2) ? C10 N2 C7 . . 108.9(3) ? C10 N2 Zn1 . . 115.3(2) ? C7 N2 Zn1 . . 133.6(2) ? C15 N3 C12 . . 109.6(3) ? C15 N3 Zn1 . . 115.4(2) ? C12 N3 Zn1 . . 131.4(2) ? C5 O1 C4 . . 106.1(2) ? C10 O2 C9 . . 105.9(2) ? C15 O3 C14 . . 106.5(3) ? Si2 Si1 Si4 . . 102.70(6) ? Si2 Si1 Si3 . . 104.29(5) ? Si4 Si1 Si3 . . 102.10(6) ? Si2 Si1 Zn1 . . 112.78(6) ? Si4 Si1 Zn1 . . 118.43(5) ? Si3 Si1 Zn1 . . 114.79(5) ? C24 Si2 C22 . . 106.05(18) ? C24 Si2 C23 . . 106.94(19) ? C22 Si2 C23 . . 105.50(18) ? C24 Si2 Si1 . . 112.69(13) ? C22 Si2 Si1 . . 111.55(13) ? C23 Si2 Si1 . . 113.55(15) ? C25 Si3 C26 . . 106.48(17) ? C25 Si3 C27 . . 104.32(19) ? C26 Si3 C27 . . 105.09(18) ? C25 Si3 Si1 . . 113.87(12) ? C26 Si3 Si1 . . 112.60(13) ? C27 Si3 Si1 . . 113.66(13) ? C29 Si4 C30 . . 105.98(18) ? C29 Si4 C28 . . 105.51(17) ? C30 Si4 C28 . . 105.48(19) ? C29 Si4 Si1 . . 115.23(13) ? C30 Si4 Si1 . . 111.94(13) ? C28 Si4 Si1 . . 111.98(14) ?