# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Parkin, Gerard' _publ_contact_author_name 'Parkin, Gerard' _publ_contact_author_email PARKIN@COLUMBIA.EDU _publ_section_title ; Synthesis and Structural Characterization of Tris(2-oxo-1-t-butylimidazolyl) and Tris(2-oxo-1-methylbenzimidazolyl) hydroborato Complexes: A New Class of Tripodal Oxygen Donor Ligand ; # Attachment '- BTMRES10.cif' data_btmres10 _database_code_depnum_ccdc_archive 'CCDC 794058' #TrackingRef '- BTMRES10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H28 B N6 O3 Re S3' _chemical_formula_weight 849.80 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' 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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 16.147(3) _cell_length_b 10.510(2) _cell_length_c 19.719(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.087(3) _cell_angle_gamma 90.00 _cell_volume 3341.5(12) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9828 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 32.11 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 3.868 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5592 _exptl_absorpt_correction_T_max 0.8301 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 49786 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 29.57 _reflns_number_total 9381 _reflns_number_gt 7614 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0270P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9381 _refine_ls_number_parameters 431 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0581 _refine_ls_wR_factor_gt 0.0538 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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 Re Re 0.289166(6) 0.547887(9) 0.425307(5) 0.01759(3) Uani 1 1 d . . . B B 0.24479(18) 0.9353(3) 0.40390(15) 0.0162(6) Uani 1 1 d . . . H1 H 0.2346(17) 1.038(2) 0.3966(14) 0.017(7) Uiso 1 1 d . . . S1 S 0.40097(4) 0.71092(6) 0.40572(3) 0.01803(13) Uani 1 1 d . . . S2 S 0.22802(4) 0.68678(6) 0.51521(3) 0.02022(14) Uani 1 1 d . . . S3 S 0.19159(4) 0.64417(6) 0.33410(3) 0.02068(13) Uani 1 1 d . . . N11 N 0.31987(13) 0.92061(19) 0.45554(11) 0.0158(4) Uani 1 1 d . . . N12 N 0.43262(13) 0.8595(2) 0.51597(11) 0.0178(4) Uani 1 1 d . . . N21 N 0.16455(12) 0.8792(2) 0.43123(11) 0.0162(4) Uani 1 1 d . . . N22 N 0.07187(13) 0.7676(2) 0.48365(11) 0.0186(4) Uani 1 1 d . . . N31 N 0.26699(13) 0.8800(2) 0.33419(11) 0.0164(4) Uani 1 1 d . . . N32 N 0.29000(15) 0.7601(2) 0.24535(11) 0.0234(5) Uani 1 1 d . . . O1 O 0.16207(13) 0.3383(2) 0.44783(13) 0.0430(6) Uani 1 1 d . . . O2 O 0.37244(14) 0.3761(2) 0.32388(12) 0.0369(5) Uani 1 1 d . . . O3 O 0.40524(14) 0.4465(2) 0.54069(11) 0.0368(5) Uani 1 1 d . . . C1 C 0.20879(19) 0.4181(3) 0.43922(16) 0.0280(6) Uani 1 1 d . . . C2 C 0.34094(17) 0.4412(3) 0.36115(15) 0.0239(6) Uani 1 1 d . . . C3 C 0.36086(18) 0.4823(3) 0.49766(15) 0.0235(6) Uani 1 1 d . . . C4 C 0.1006(3) 0.2081(4) 0.7446(2) 0.0538(10) Uani 1 1 d . . . H4A H 0.0949 0.1320 0.7699 0.065 Uiso 1 1 calc R . . C5 C 0.0313(2) 0.2689(4) 0.7163(2) 0.0505(10) Uani 1 1 d . . . H5A H -0.0223 0.2343 0.7216 0.061 Uiso 1 1 calc R . . C6 C 0.0401(2) 0.3785(4) 0.6809(2) 0.0516(10) Uani 1 1 d . . . H6A H -0.0077 0.4214 0.6622 0.062 Uiso 1 1 calc R . . C7 C 0.1175(2) 0.4276(4) 0.67180(19) 0.0489(10) Uani 1 1 d . . . H7A H 0.1230 0.5035 0.6463 0.059 Uiso 1 1 calc R . . C8 C 0.1869(2) 0.3679(4) 0.69932(18) 0.0442(9) Uani 1 1 d . . . H8A H 0.2403 0.4024 0.6929 0.053 Uiso 1 1 calc R . . C9 C 0.1793(2) 0.2591(4) 0.73588(19) 0.0492(10) Uani 1 1 d . . . H9A H 0.2272 0.2180 0.7554 0.059 Uiso 1 1 calc R . . C11 C 0.50487(16) 0.7851(3) 0.53939(14) 0.0239(6) Uani 1 1 d . . . H11B H 0.5139 0.7946 0.5887 0.036 Uiso 1 1 calc R . . H11C H 0.5538 0.8154 0.5169 0.036 Uiso 1 1 calc R . . H11A H 0.4954 0.6952 0.5283 0.036 Uiso 1 1 calc R . . C12 C 0.38214(15) 0.8340(2) 0.46025(13) 0.0166(5) Uani 1 1 d . . . C13 C 0.40222(16) 0.9657(2) 0.54882(13) 0.0190(5) Uani 1 1 d . . . C14 C 0.33084(16) 1.0032(2) 0.51104(13) 0.0173(5) Uani 1 1 d . . . C15 C 0.28499(17) 1.1079(3) 0.53000(14) 0.0216(6) Uani 1 1 d . . . H15A H 0.2362 1.1338 0.5047 0.026 Uiso 1 1 calc R . . C16 C 0.31375(18) 1.1725(3) 0.58745(15) 0.0267(6) Uani 1 1 d . . . H16A H 0.2838 1.2445 0.6018 0.032 Uiso 1 1 calc R . . C17 C 0.38541(19) 1.1356(3) 0.62516(15) 0.0301(7) Uani 1 1 d . . . H17A H 0.4029 1.1827 0.6645 0.036 Uiso 1 1 calc R . . C18 C 0.43157(18) 1.0312(3) 0.60625(14) 0.0242(6) Uani 1 1 d . . . H18A H 0.4807 1.0059 0.6314 0.029 Uiso 1 1 calc R . . C21 C 0.03374(18) 0.6701(3) 0.52477(16) 0.0272(6) Uani 1 1 d . . . H21A H 0.0738 0.6018 0.5349 0.041 Uiso 1 1 calc R . . H21B H -0.0151 0.6352 0.4996 0.041 Uiso 1 1 calc R . . H21C H 0.0170 0.7080 0.5673 0.041 Uiso 1 1 calc R . . C22 C 0.15369(16) 0.7815(2) 0.47412(13) 0.0172(5) Uani 1 1 d . . . C23 C 0.02747(15) 0.8594(2) 0.44635(13) 0.0182(5) Uani 1 1 d . . . C24 C 0.08565(15) 0.9290(2) 0.41231(13) 0.0167(5) Uani 1 1 d . . . C25 C 0.06086(17) 1.0278(2) 0.36881(14) 0.0211(6) Uani 1 1 d . . . H25A H 0.0997 1.0755 0.3447 0.025 Uiso 1 1 calc R . . C26 C -0.02393(17) 1.0533(3) 0.36246(15) 0.0251(6) Uani 1 1 d . . . H26A H -0.0433 1.1196 0.3330 0.030 Uiso 1 1 calc R . . C27 C -0.08135(17) 0.9838(3) 0.39833(15) 0.0249(6) Uani 1 1 d . . . H27A H -0.1385 1.0055 0.3933 0.030 Uiso 1 1 calc R . . C28 C -0.05711(16) 0.8853(3) 0.44049(14) 0.0226(6) Uani 1 1 d . . . H28A H -0.0960 0.8373 0.4644 0.027 Uiso 1 1 calc R . . C31 C 0.2897(2) 0.6523(3) 0.19867(16) 0.0385(8) Uani 1 1 d . . . H31A H 0.2504 0.5879 0.2131 0.058 Uiso 1 1 calc R . . H31B H 0.3454 0.6153 0.1988 0.058 Uiso 1 1 calc R . . H31C H 0.2730 0.6813 0.1527 0.058 Uiso 1 1 calc R . . C32 C 0.25024(16) 0.7668(2) 0.30400(13) 0.0193(5) Uani 1 1 d . . . C33 C 0.33721(17) 0.8698(3) 0.23879(14) 0.0223(6) Uani 1 1 d . . . C34 C 0.32309(15) 0.9449(2) 0.29469(13) 0.0180(5) Uani 1 1 d . . . C35 C 0.36252(16) 1.0616(2) 0.30463(14) 0.0198(5) Uani 1 1 d . . . H35A H 0.3529 1.1136 0.3428 0.024 Uiso 1 1 calc R . . C36 C 0.41677(17) 1.0982(3) 0.25583(14) 0.0241(6) Uani 1 1 d . . . H36A H 0.4451 1.1771 0.2610 0.029 Uiso 1 1 calc R . . C37 C 0.43074(19) 1.0229(3) 0.19957(16) 0.0303(7) Uani 1 1 d . . . H37A H 0.4685 1.0512 0.1674 0.036 Uiso 1 1 calc R . . C38 C 0.3905(2) 0.9068(3) 0.18945(16) 0.0320(7) Uani 1 1 d . . . H38A H 0.3991 0.8555 0.1508 0.038 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 Re 0.01645(5) 0.01446(5) 0.02202(6) 0.00103(4) 0.00267(4) 0.00169(4) B 0.0146(13) 0.0163(14) 0.0179(14) -0.0011(11) 0.0024(11) 0.0009(11) S1 0.0156(3) 0.0171(3) 0.0216(3) -0.0039(2) 0.0029(2) 0.0015(2) S2 0.0201(3) 0.0209(3) 0.0200(3) 0.0040(3) 0.0044(3) 0.0060(3) S3 0.0192(3) 0.0189(3) 0.0236(3) 0.0005(3) -0.0020(3) -0.0032(3) N11 0.0150(10) 0.0155(10) 0.0169(11) -0.0017(8) 0.0014(8) -0.0003(8) N12 0.0149(10) 0.0196(11) 0.0186(11) -0.0004(9) -0.0005(8) -0.0001(9) N21 0.0130(10) 0.0164(11) 0.0192(11) 0.0010(8) 0.0021(8) 0.0021(8) N22 0.0170(11) 0.0169(11) 0.0223(12) 0.0008(9) 0.0041(9) 0.0019(8) N31 0.0157(10) 0.0165(11) 0.0169(11) 0.0018(8) 0.0005(8) -0.0006(8) N32 0.0307(13) 0.0209(11) 0.0191(12) -0.0014(9) 0.0054(10) -0.0011(10) O1 0.0284(12) 0.0310(12) 0.0702(18) 0.0141(12) 0.0092(12) -0.0036(10) O2 0.0379(13) 0.0292(12) 0.0444(14) -0.0130(10) 0.0104(11) -0.0003(10) O3 0.0411(13) 0.0361(12) 0.0326(12) 0.0024(10) -0.0028(10) 0.0168(10) C1 0.0267(15) 0.0221(14) 0.0357(17) 0.0065(12) 0.0054(13) 0.0072(12) C2 0.0211(13) 0.0179(13) 0.0325(16) 0.0001(12) -0.0014(11) -0.0031(11) C3 0.0244(14) 0.0189(14) 0.0275(15) 0.0002(11) 0.0045(12) 0.0062(11) C4 0.075(3) 0.045(2) 0.042(2) -0.0164(18) 0.006(2) -0.001(2) C5 0.037(2) 0.068(3) 0.047(2) -0.032(2) 0.0061(17) -0.0079(19) C6 0.032(2) 0.068(3) 0.053(2) -0.023(2) -0.0108(17) 0.0124(19) C7 0.051(2) 0.057(2) 0.038(2) -0.0103(18) -0.0085(18) 0.0021(19) C8 0.0308(18) 0.060(2) 0.042(2) -0.0243(19) -0.0010(15) -0.0021(17) C9 0.042(2) 0.059(2) 0.045(2) -0.0251(19) -0.0145(17) 0.0197(19) C11 0.0159(13) 0.0281(15) 0.0272(15) 0.0016(12) -0.0036(11) 0.0028(11) C12 0.0155(12) 0.0159(12) 0.0186(13) 0.0004(10) 0.0036(10) 0.0002(9) C13 0.0197(13) 0.0197(13) 0.0183(13) -0.0012(10) 0.0057(10) -0.0041(10) C14 0.0190(13) 0.0165(11) 0.0168(13) -0.0002(10) 0.0050(10) -0.0025(10) C15 0.0190(13) 0.0196(13) 0.0267(15) -0.0030(11) 0.0056(11) 0.0000(10) C16 0.0313(16) 0.0226(14) 0.0272(15) -0.0077(12) 0.0108(12) -0.0017(12) C17 0.0380(17) 0.0301(16) 0.0223(15) -0.0091(12) 0.0031(13) -0.0086(13) C18 0.0249(14) 0.0272(15) 0.0205(14) -0.0024(11) 0.0006(11) -0.0066(11) C21 0.0239(14) 0.0225(14) 0.0361(17) 0.0075(12) 0.0085(12) -0.0023(11) C22 0.0186(13) 0.0157(12) 0.0175(13) -0.0032(10) 0.0031(10) 0.0008(10) C23 0.0157(12) 0.0183(12) 0.0208(13) -0.0022(10) 0.0015(10) -0.0001(10) C24 0.0140(12) 0.0175(13) 0.0185(13) -0.0044(10) 0.0012(10) 0.0005(9) C25 0.0215(13) 0.0218(14) 0.0202(13) 0.0043(10) 0.0020(11) 0.0022(10) C26 0.0233(14) 0.0261(14) 0.0257(14) 0.0035(12) -0.0016(11) 0.0066(12) C27 0.0154(13) 0.0287(15) 0.0304(16) -0.0034(12) 0.0002(11) 0.0036(11) C28 0.0153(13) 0.0275(15) 0.0252(14) -0.0038(12) 0.0036(11) 0.0003(11) C31 0.064(2) 0.0263(16) 0.0258(16) -0.0091(13) 0.0090(16) -0.0036(16) C32 0.0182(13) 0.0216(13) 0.0178(13) 0.0020(10) -0.0024(10) 0.0019(10) C33 0.0264(14) 0.0209(13) 0.0197(13) 0.0026(11) 0.0034(11) 0.0038(11) C34 0.0143(12) 0.0225(13) 0.0173(12) 0.0045(11) 0.0023(9) 0.0021(10) C35 0.0193(13) 0.0192(13) 0.0210(13) 0.0030(10) 0.0004(10) 0.0008(10) C36 0.0196(13) 0.0259(14) 0.0266(15) 0.0090(12) 0.0008(11) -0.0021(11) C37 0.0294(16) 0.0349(17) 0.0280(16) 0.0085(13) 0.0133(13) 0.0013(13) C38 0.0392(18) 0.0336(16) 0.0244(16) 0.0000(13) 0.0132(13) 0.0030(14) _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 Re C1 1.913(3) . ? Re C2 1.916(3) . ? Re C3 1.917(3) . ? Re S1 2.5337(7) . ? Re S3 2.5369(8) . ? Re S2 2.5372(7) . ? B H1 1.10(3) . ? B N21 1.547(3) . ? B N11 1.548(4) . ? B N31 1.552(4) . ? S1 C12 1.720(3) . ? S2 C22 1.727(3) . ? S3 C32 1.724(3) . ? N11 C12 1.356(3) . ? N11 C14 1.401(3) . ? N12 C12 1.359(3) . ? N12 C13 1.394(3) . ? N12 C11 1.458(3) . ? N21 C22 1.348(3) . ? N21 C24 1.409(3) . ? N22 C22 1.352(3) . ? N22 C23 1.389(3) . ? N22 C21 1.463(3) . ? N31 C32 1.351(3) . ? N31 C34 1.403(3) . ? N32 C32 1.354(3) . ? N32 C33 1.392(3) . ? N32 C31 1.460(4) . ? O1 C1 1.147(3) . ? O2 C2 1.144(3) . ? O3 C3 1.144(3) . ? C4 C5 1.381(6) . ? C4 C9 1.398(6) . ? C5 C6 1.358(6) . ? C6 C7 1.373(5) . ? C7 C8 1.371(5) . ? C8 C9 1.361(5) . ? C13 C18 1.387(4) . ? C13 C14 1.395(4) . ? C14 C15 1.389(4) . ? C15 C16 1.380(4) . ? C16 C17 1.396(4) . ? C17 C18 1.388(4) . ? C23 C28 1.391(3) . ? C23 C24 1.392(3) . ? C24 C25 1.392(4) . ? C25 C26 1.394(4) . ? C26 C27 1.401(4) . ? C27 C28 1.372(4) . ? C33 C34 1.384(4) . ? C33 C38 1.389(4) . ? C34 C35 1.391(4) . ? C35 C36 1.390(4) . ? C36 C37 1.391(4) . ? C37 C38 1.391(4) . ? 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 C1 Re C2 90.06(12) . . ? C1 Re C3 91.37(13) . . ? C2 Re C3 90.77(12) . . ? C1 Re S1 177.06(9) . . ? C2 Re S1 87.43(8) . . ? C3 Re S1 87.13(9) . . ? C1 Re S3 89.19(9) . . ? C2 Re S3 92.39(9) . . ? C3 Re S3 176.79(8) . . ? S1 Re S3 92.44(2) . . ? C1 Re S2 91.00(9) . . ? C2 Re S2 176.56(9) . . ? C3 Re S2 85.93(8) . . ? S1 Re S2 91.42(2) . . ? S3 Re S2 90.90(3) . . ? H1 B N21 107.3(15) . . ? H1 B N11 106.9(15) . . ? N21 B N11 111.9(2) . . ? H1 B N31 106.9(15) . . ? N21 B N31 113.8(2) . . ? N11 B N31 109.6(2) . . ? C12 S1 Re 105.19(9) . . ? C22 S2 Re 106.89(9) . . ? C32 S3 Re 102.16(9) . . ? C12 N11 C14 107.5(2) . . ? C12 N11 B 131.6(2) . . ? C14 N11 B 120.9(2) . . ? C12 N12 C13 108.8(2) . . ? C12 N12 C11 125.8(2) . . ? C13 N12 C11 125.3(2) . . ? C22 N21 C24 107.6(2) . . ? C22 N21 B 130.5(2) . . ? C24 N21 B 121.9(2) . . ? C22 N22 C23 109.4(2) . . ? C22 N22 C21 126.6(2) . . ? C23 N22 C21 124.0(2) . . ? C32 N31 C34 107.6(2) . . ? C32 N31 B 132.0(2) . . ? C34 N31 B 119.8(2) . . ? C32 N32 C33 108.9(2) . . ? C32 N32 C31 126.4(2) . . ? C33 N32 C31 124.6(2) . . ? O1 C1 Re 178.4(3) . . ? O2 C2 Re 178.7(3) . . ? O3 C3 Re 177.8(3) . . ? C5 C4 C9 119.7(4) . . ? C6 C5 C4 119.7(4) . . ? C5 C6 C7 120.4(4) . . ? C8 C7 C6 120.5(4) . . ? C9 C8 C7 119.9(4) . . ? C8 C9 C4 119.8(4) . . ? N11 C12 N12 109.5(2) . . ? N11 C12 S1 128.1(2) . . ? N12 C12 S1 122.33(19) . . ? C18 C13 N12 131.6(3) . . ? C18 C13 C14 122.2(2) . . ? N12 C13 C14 106.3(2) . . ? C15 C14 C13 121.1(2) . . ? C15 C14 N11 130.9(2) . . ? C13 C14 N11 107.9(2) . . ? C16 C15 C14 116.8(3) . . ? C15 C16 C17 122.2(3) . . ? C18 C17 C16 121.2(3) . . ? C13 C18 C17 116.5(3) . . ? N21 C22 N22 109.3(2) . . ? N21 C22 S2 128.5(2) . . ? N22 C22 S2 122.13(19) . . ? N22 C23 C28 131.0(2) . . ? N22 C23 C24 106.1(2) . . ? C28 C23 C24 122.8(2) . . ? C23 C24 C25 120.7(2) . . ? C23 C24 N21 107.5(2) . . ? C25 C24 N21 131.8(2) . . ? C24 C25 C26 116.5(2) . . ? C25 C26 C27 121.9(3) . . ? C28 C27 C26 121.6(3) . . ? C27 C28 C23 116.4(3) . . ? N31 C32 N32 109.2(2) . . ? N31 C32 S3 127.4(2) . . ? N32 C32 S3 123.3(2) . . ? C34 C33 C38 122.2(3) . . ? C34 C33 N32 106.5(2) . . ? C38 C33 N32 131.3(3) . . ? C33 C34 C35 121.4(2) . . ? C33 C34 N31 107.7(2) . . ? C35 C34 N31 130.9(2) . . ? C36 C35 C34 116.6(3) . . ? C35 C36 C37 122.0(3) . . ? C38 C37 C36 121.3(3) . . ? C33 C38 C37 116.6(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.57 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.337 _refine_diff_density_min -0.441 _refine_diff_density_rms 0.109 # Attachment '- BTORES10.cif' data_btores10 _database_code_depnum_ccdc_archive 'CCDC 794059' #TrackingRef '- BTORES10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H22 B N6 O6 Re' _chemical_formula_weight 723.52 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' 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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3 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 15.5893(14) _cell_length_b 15.5893(14) _cell_length_c 19.0929(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4018.4(6) _cell_formula_units_Z 6 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9238 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 32.51 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.794 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2124 _exptl_absorpt_coefficient_mu 4.590 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.5460 _exptl_absorpt_correction_T_max 0.5460 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23365 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0158 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 32.71 _reflns_number_total 3200 _reflns_number_gt 3025 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+3.9801P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3200 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0187 _refine_ls_R_factor_gt 0.0167 _refine_ls_wR_factor_ref 0.0418 _refine_ls_wR_factor_gt 0.0410 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Re Re 0.0000 0.0000 0.347969(5) 0.01942(3) Uani 1 3 d S . . B B 0.0000 0.0000 0.14054(14) 0.0185(4) Uani 1 3 d S . . C11 C 0.11320(12) 0.05717(12) 0.40683(8) 0.0258(3) Uani 1 1 d . . . O11 O 0.18295(10) 0.09211(11) 0.44205(7) 0.0364(3) Uani 1 1 d . . . O1 O 0.06203(8) -0.06253(8) 0.27592(5) 0.02156(19) Uani 1 1 d . . . N1 N 0.09983(9) 0.01211(9) 0.16473(6) 0.0179(2) Uani 1 1 d . . . N2 N 0.20860(9) -0.01826(9) 0.21783(6) 0.0210(2) Uani 1 1 d . . . C1 C 0.11829(10) -0.02487(10) 0.22357(7) 0.0186(2) Uani 1 1 d . . . C2 C 0.18398(10) 0.04855(10) 0.12196(7) 0.0183(2) Uani 1 1 d . . . C3 C 0.20618(11) 0.09928(11) 0.05879(8) 0.0230(3) Uani 1 1 d . . . H3A H 0.1603 0.1134 0.0363 0.028 Uiso 1 1 calc R . . C4 C 0.29901(12) 0.12858(12) 0.02982(8) 0.0274(3) Uani 1 1 d . . . H4A H 0.3164 0.1628 -0.0137 0.033 Uiso 1 1 calc R . . C5 C 0.36676(12) 0.10893(13) 0.06299(9) 0.0292(3) Uani 1 1 d . . . H5A H 0.4295 0.1306 0.0419 0.035 Uiso 1 1 calc R . . C6 C 0.34464(11) 0.05813(13) 0.12651(9) 0.0267(3) Uani 1 1 d . . . H6A H 0.3907 0.0443 0.1491 0.032 Uiso 1 1 calc R . . C7 C 0.25207(10) 0.02866(11) 0.15532(7) 0.0206(2) Uani 1 1 d . . . C8 C 0.25251(13) -0.05140(14) 0.27058(9) 0.0298(3) Uani 1 1 d . . . H8A H 0.2153 -0.0646 0.3144 0.045 Uiso 1 1 calc R . . H8B H 0.3215 0.0002 0.2784 0.045 Uiso 1 1 calc R . . H8C H 0.2504 -0.1121 0.2545 0.045 Uiso 1 1 calc R . . H1 H 0.0000 0.0000 0.0832(16) 0.011(7) Uiso 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 Re 0.02166(4) 0.02166(4) 0.01496(5) 0.000 0.000 0.01083(2) B 0.0187(7) 0.0187(7) 0.0180(11) 0.000 0.000 0.0093(3) C11 0.0286(7) 0.0291(7) 0.0192(6) 0.0028(5) 0.0022(5) 0.0142(6) O11 0.0312(6) 0.0451(7) 0.0272(6) -0.0012(5) -0.0073(5) 0.0147(6) O1 0.0249(5) 0.0221(5) 0.0190(5) 0.0034(4) 0.0038(4) 0.0127(4) N1 0.0178(5) 0.0191(5) 0.0168(5) 0.0014(4) 0.0010(4) 0.0092(4) N2 0.0206(5) 0.0243(6) 0.0207(5) -0.0002(4) -0.0015(4) 0.0133(5) C1 0.0200(6) 0.0177(6) 0.0187(6) -0.0005(4) -0.0004(5) 0.0099(5) C2 0.0174(5) 0.0175(5) 0.0180(6) -0.0024(4) 0.0009(4) 0.0071(5) C3 0.0234(6) 0.0218(6) 0.0188(6) -0.0011(5) 0.0007(5) 0.0076(5) C4 0.0254(7) 0.0257(7) 0.0213(6) -0.0033(5) 0.0048(5) 0.0055(6) C5 0.0202(6) 0.0316(8) 0.0274(7) -0.0093(6) 0.0040(5) 0.0066(6) C6 0.0196(6) 0.0313(7) 0.0285(7) -0.0086(6) -0.0007(5) 0.0121(6) C7 0.0200(6) 0.0214(6) 0.0202(6) -0.0041(5) -0.0008(5) 0.0102(5) C8 0.0306(8) 0.0358(8) 0.0299(8) 0.0040(6) -0.0040(6) 0.0217(7) _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 Re C11 1.8970(16) 2 ? Re C11 1.8970(17) 3 ? Re C11 1.8970(17) . ? Re O1 2.1727(11) 3 ? Re O1 2.1727(11) 2 ? Re O1 2.1727(11) . ? B H1 1.10(3) . ? B N1 1.5417(14) . ? B N1 1.5418(14) 3 ? B N1 1.5418(14) 2 ? C11 O11 1.157(2) . ? O1 C1 1.2641(17) . ? N1 C1 1.3577(17) . ? N1 C2 1.4019(17) . ? N2 C1 1.3637(18) . ? N2 C7 1.3869(19) . ? N2 C8 1.4503(19) . ? C2 C3 1.388(2) . ? C2 C7 1.399(2) . ? C3 C4 1.396(2) . ? C4 C5 1.391(3) . ? C5 C6 1.394(2) . ? C6 C7 1.390(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 C11 Re C11 88.49(7) 2 3 ? C11 Re C11 88.49(7) 2 . ? C11 Re C11 88.49(7) 3 . ? C11 Re O1 93.38(6) 2 3 ? C11 Re O1 93.88(6) 3 3 ? C11 Re O1 177.02(5) . 3 ? C11 Re O1 93.88(6) 2 2 ? C11 Re O1 177.02(5) 3 2 ? C11 Re O1 93.38(6) . 2 ? O1 Re O1 84.19(4) 3 2 ? C11 Re O1 177.02(5) 2 . ? C11 Re O1 93.38(6) 3 . ? C11 Re O1 93.88(6) . . ? O1 Re O1 84.18(4) 3 . ? O1 Re O1 84.18(4) 2 . ? H1 B N1 107.43(11) . . ? H1 B N1 107.43(11) . 3 ? N1 B N1 111.43(10) . 3 ? H1 B N1 107.43(11) . 2 ? N1 B N1 111.43(10) . 2 ? N1 B N1 111.43(10) 3 2 ? O11 C11 Re 179.18(15) . . ? C1 O1 Re 130.80(9) . . ? C1 N1 C2 107.45(11) . . ? C1 N1 B 127.67(13) . . ? C2 N1 B 123.92(13) . . ? C1 N2 C7 108.83(12) . . ? C1 N2 C8 124.80(13) . . ? C7 N2 C8 126.32(13) . . ? O1 C1 N1 127.32(13) . . ? O1 C1 N2 123.30(13) . . ? N1 C1 N2 109.36(12) . . ? C3 C2 C7 121.41(13) . . ? C3 C2 N1 130.78(13) . . ? C7 C2 N1 107.76(12) . . ? C2 C3 C4 116.95(15) . . ? C5 C4 C3 121.65(15) . . ? C4 C5 C6 121.46(14) . . ? C7 C6 C5 116.93(15) . . ? N2 C7 C6 131.87(14) . . ? N2 C7 C2 106.49(12) . . ? C6 C7 C2 121.59(14) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 32.71 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.290 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.084 # Attachment '- TO2COS10.cif' data_to2cos10 _database_code_depnum_ccdc_archive 'CCDC 794060' #TrackingRef '- TO2COS10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H46 B2 Cl6 Co N12 O6' _chemical_formula_weight 1204.24 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.027(2) _cell_length_b 11.171(2) _cell_length_c 11.536(2) _cell_angle_alpha 85.955(3) _cell_angle_beta 78.386(3) _cell_angle_gamma 74.761(3) _cell_volume 1342.8(4) _cell_formula_units_Z 1 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 4234 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 26.02 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 617 _exptl_absorpt_coefficient_mu 0.680 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.9229 _exptl_absorpt_correction_T_max 0.9932 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21660 _diffrn_reflns_av_R_equivalents 0.0761 _diffrn_reflns_av_sigmaI/netI 0.1153 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 30.47 _reflns_number_total 8101 _reflns_number_gt 3917 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.9860P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8101 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1520 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1701 _refine_ls_wR_factor_gt 0.1400 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Co Co 0.5000 0.5000 0.5000 0.02751(18) Uani 1 2 d S . . B B 0.3507(4) 0.3342(4) 0.3119(3) 0.0265(8) Uani 1 1 d . . . H1 H 0.314(3) 0.281(3) 0.254(3) 0.023(9) Uiso 1 1 d . . . N11 N 0.3922(3) 0.4396(3) 0.2350(2) 0.0259(6) Uani 1 1 d . . . N12 N 0.4813(3) 0.5939(3) 0.1675(3) 0.0321(7) Uani 1 1 d . . . N21 N 0.2470(3) 0.3855(2) 0.4213(2) 0.0260(6) Uani 1 1 d . . . N22 N 0.1482(3) 0.4795(3) 0.5902(3) 0.0336(7) Uani 1 1 d . . . N31 N 0.4645(3) 0.2385(2) 0.3518(2) 0.0260(6) Uani 1 1 d . . . N32 N 0.6054(3) 0.1313(3) 0.4582(2) 0.0280(6) Uani 1 1 d . . . O1 O 0.5584(2) 0.4693(2) 0.3196(2) 0.0304(6) Uani 1 1 d . . . O2 O 0.3128(2) 0.5533(2) 0.4756(2) 0.0309(6) Uani 1 1 d . . . O3 O 0.4785(2) 0.3186(2) 0.5299(2) 0.0304(6) Uani 1 1 d . . . C11 C 0.5588(4) 0.6811(4) 0.1613(4) 0.0429(10) Uani 1 1 d . . . H11A H 0.6037 0.6660 0.2282 0.064 Uiso 1 1 calc R . . H11B H 0.5038 0.7659 0.1645 0.064 Uiso 1 1 calc R . . H11C H 0.6215 0.6705 0.0869 0.064 Uiso 1 1 calc R . . C12 C 0.4835(3) 0.4975(3) 0.2481(3) 0.0273(7) Uani 1 1 d . . . C13 C 0.3874(4) 0.5986(3) 0.1020(3) 0.0322(8) Uani 1 1 d . . . C14 C 0.3311(3) 0.5024(3) 0.1443(3) 0.0288(8) Uani 1 1 d . . . C15 C 0.2322(3) 0.4826(4) 0.0978(3) 0.0337(8) Uani 1 1 d . . . H15A H 0.1938 0.4167 0.1261 0.040 Uiso 1 1 calc R . . C16 C 0.1911(4) 0.5632(4) 0.0080(4) 0.0464(11) Uani 1 1 d . . . H16A H 0.1220 0.5528 -0.0245 0.056 Uiso 1 1 calc R . . C17 C 0.2479(4) 0.6582(4) -0.0355(4) 0.0485(11) Uani 1 1 d . . . H17A H 0.2185 0.7104 -0.0981 0.058 Uiso 1 1 calc R . . C18 C 0.3475(4) 0.6779(4) 0.0117(3) 0.0424(10) Uani 1 1 d . . . H18A H 0.3866 0.7433 -0.0170 0.051 Uiso 1 1 calc R . . C21 C 0.1239(4) 0.5605(4) 0.6893(3) 0.0468(11) Uani 1 1 d . . . H21A H 0.1770 0.6197 0.6706 0.070 Uiso 1 1 calc R . . H21B H 0.1448 0.5109 0.7595 0.070 Uiso 1 1 calc R . . H21C H 0.0333 0.6058 0.7051 0.070 Uiso 1 1 calc R . . C22 C 0.2438(3) 0.4796(3) 0.4930(3) 0.0273(8) Uani 1 1 d . . . C23 C 0.0907(3) 0.3849(3) 0.5817(3) 0.0326(8) Uani 1 1 d . . . C24 C 0.1522(3) 0.3264(3) 0.4757(3) 0.0274(7) Uani 1 1 d . . . C25 C 0.1156(4) 0.2277(3) 0.4396(4) 0.0364(9) Uani 1 1 d . . . H25A H 0.1579 0.1863 0.3678 0.044 Uiso 1 1 calc R . . C26 C 0.0142(4) 0.1915(4) 0.5132(4) 0.0460(10) Uani 1 1 d . . . H26A H -0.0144 0.1253 0.4901 0.055 Uiso 1 1 calc R . . C27 C -0.0456(4) 0.2496(4) 0.6185(4) 0.0509(11) Uani 1 1 d . . . H27A H -0.1137 0.2216 0.6668 0.061 Uiso 1 1 calc R . . C28 C -0.0090(4) 0.3479(4) 0.6559(4) 0.0430(10) Uani 1 1 d . . . H28A H -0.0502 0.3878 0.7286 0.052 Uiso 1 1 calc R . . C31 C 0.6735(4) 0.0999(4) 0.5562(3) 0.0395(9) Uani 1 1 d . . . H31A H 0.6675 0.1757 0.5973 0.059 Uiso 1 1 calc R . . H31B H 0.7637 0.0597 0.5259 0.059 Uiso 1 1 calc R . . H31C H 0.6353 0.0432 0.6115 0.059 Uiso 1 1 calc R . . C32 C 0.5116(3) 0.2380(3) 0.4529(3) 0.0275(7) Uani 1 1 d . . . C33 C 0.6213(3) 0.0611(3) 0.3599(3) 0.0274(7) Uani 1 1 d . . . C34 C 0.5334(3) 0.1295(3) 0.2920(3) 0.0252(7) Uani 1 1 d . . . C35 C 0.5268(3) 0.0860(3) 0.1834(3) 0.0284(8) Uani 1 1 d . . . H35A H 0.4677 0.1311 0.1365 0.034 Uiso 1 1 calc R . . C36 C 0.6116(4) -0.0270(3) 0.1479(3) 0.0347(9) Uani 1 1 d . . . H36A H 0.6105 -0.0589 0.0740 0.042 Uiso 1 1 calc R . . C37 C 0.6970(4) -0.0948(3) 0.2150(4) 0.0385(9) Uani 1 1 d . . . H37A H 0.7525 -0.1717 0.1867 0.046 Uiso 1 1 calc R . . C38 C 0.7033(4) -0.0521(3) 0.3238(3) 0.0359(9) Uani 1 1 d . . . H38A H 0.7614 -0.0988 0.3710 0.043 Uiso 1 1 calc R . . Cl1 Cl 1.24253(11) -0.01854(12) 0.17813(10) 0.0598(3) Uani 1 1 d . . . Cl2 Cl 1.10534(14) 0.20443(12) 0.07480(12) 0.0700(4) Uani 1 1 d . . . Cl3 Cl 0.97561(13) 0.01732(16) 0.17093(13) 0.0817(5) Uani 1 1 d . . . C40 C 1.1213(4) 0.0443(4) 0.0977(4) 0.0478(11) Uani 1 1 d . . . H40B H 1.1455 0.0037 0.0189 0.057 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 Co 0.0297(4) 0.0277(4) 0.0278(4) -0.0050(3) -0.0114(3) -0.0064(3) B 0.027(2) 0.029(2) 0.026(2) -0.0021(16) -0.0104(16) -0.0063(17) N11 0.0289(15) 0.0294(15) 0.0213(14) -0.0013(12) -0.0085(12) -0.0080(13) N12 0.0354(17) 0.0314(16) 0.0305(16) -0.0005(13) -0.0044(14) -0.0116(14) N21 0.0257(15) 0.0254(15) 0.0273(15) -0.0028(12) -0.0076(12) -0.0047(12) N22 0.0281(16) 0.0422(18) 0.0266(16) -0.0062(13) -0.0065(13) 0.0001(14) N31 0.0302(16) 0.0236(14) 0.0272(15) -0.0018(12) -0.0108(12) -0.0076(12) N32 0.0314(16) 0.0267(15) 0.0292(16) 0.0003(12) -0.0153(13) -0.0063(13) O1 0.0285(13) 0.0375(14) 0.0285(13) -0.0052(11) -0.0093(11) -0.0101(11) O2 0.0299(13) 0.0307(13) 0.0338(14) -0.0071(10) -0.0125(11) -0.0040(11) O3 0.0372(14) 0.0281(13) 0.0272(13) -0.0032(10) -0.0121(11) -0.0052(11) C11 0.051(3) 0.037(2) 0.045(2) 0.0039(18) -0.006(2) -0.022(2) C12 0.0290(18) 0.0268(18) 0.0250(17) -0.0075(14) -0.0040(15) -0.0045(15) C13 0.035(2) 0.0295(19) 0.0283(19) -0.0001(15) -0.0036(16) -0.0030(16) C14 0.034(2) 0.0270(18) 0.0232(17) -0.0018(14) -0.0071(15) -0.0021(15) C15 0.033(2) 0.042(2) 0.0241(18) -0.0020(16) -0.0078(16) -0.0036(17) C16 0.046(3) 0.056(3) 0.037(2) -0.002(2) -0.0187(19) -0.003(2) C17 0.054(3) 0.052(3) 0.034(2) 0.0063(19) -0.017(2) 0.003(2) C18 0.051(3) 0.037(2) 0.033(2) 0.0047(17) -0.0039(19) -0.0045(19) C21 0.041(2) 0.062(3) 0.031(2) -0.0175(19) -0.0085(18) 0.004(2) C22 0.0254(18) 0.0298(18) 0.0253(18) -0.0032(14) -0.0117(15) 0.0013(15) C23 0.0265(19) 0.038(2) 0.0301(19) 0.0039(16) -0.0092(15) -0.0019(16) C24 0.0207(17) 0.0322(19) 0.0277(18) 0.0055(15) -0.0086(14) -0.0028(15) C25 0.036(2) 0.033(2) 0.042(2) 0.0068(17) -0.0133(18) -0.0106(17) C26 0.039(2) 0.040(2) 0.063(3) 0.012(2) -0.017(2) -0.0141(19) C27 0.034(2) 0.054(3) 0.063(3) 0.021(2) -0.010(2) -0.012(2) C28 0.029(2) 0.056(3) 0.038(2) 0.0064(19) -0.0048(17) -0.0012(19) C31 0.044(2) 0.040(2) 0.039(2) 0.0006(17) -0.0243(18) -0.0055(18) C32 0.0307(19) 0.0263(18) 0.0280(18) 0.0010(14) -0.0095(15) -0.0090(15) C33 0.0292(18) 0.0266(18) 0.0275(18) 0.0017(14) -0.0059(15) -0.0090(15) C34 0.0257(17) 0.0223(16) 0.0276(18) 0.0010(14) -0.0019(14) -0.0089(14) C35 0.0344(19) 0.0299(18) 0.0253(18) 0.0003(14) -0.0073(15) -0.0149(16) C36 0.044(2) 0.033(2) 0.0304(19) -0.0069(16) -0.0046(17) -0.0151(18) C37 0.039(2) 0.029(2) 0.046(2) -0.0065(17) -0.0021(18) -0.0092(17) C38 0.036(2) 0.0263(19) 0.046(2) 0.0006(16) -0.0139(18) -0.0045(16) Cl1 0.0541(7) 0.0751(8) 0.0538(7) -0.0032(6) -0.0267(6) -0.0097(6) Cl2 0.0795(9) 0.0514(7) 0.0695(9) -0.0006(6) -0.0024(7) -0.0090(7) Cl3 0.0633(8) 0.1283(13) 0.0701(9) 0.0301(8) -0.0252(7) -0.0522(9) C40 0.048(3) 0.056(3) 0.047(3) 0.000(2) -0.021(2) -0.016(2) _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 Co O2 2.064(2) . ? Co O2 2.064(2) 2_666 ? Co O1 2.076(2) 2_666 ? Co O1 2.076(2) . ? Co O3 2.098(2) . ? Co O3 2.098(2) 2_666 ? B H1 1.12(3) . ? B N11 1.534(5) . ? B N31 1.546(5) . ? B N21 1.551(5) . ? N11 C12 1.369(4) . ? N11 C14 1.405(4) . ? N12 C12 1.370(4) . ? N12 C13 1.387(5) . ? N12 C11 1.445(5) . ? N21 C22 1.372(4) . ? N21 C24 1.400(4) . ? N22 C22 1.376(5) . ? N22 C23 1.386(5) . ? N22 C21 1.447(5) . ? N31 C32 1.368(4) . ? N31 C34 1.399(4) . ? N32 C32 1.364(4) . ? N32 C33 1.380(4) . ? N32 C31 1.454(4) . ? O1 C12 1.250(4) . ? O2 C22 1.241(4) . ? O3 C32 1.242(4) . ? C13 C18 1.384(5) . ? C13 C14 1.390(5) . ? C14 C15 1.380(5) . ? C15 C16 1.390(5) . ? C16 C17 1.385(6) . ? C17 C18 1.391(6) . ? C23 C28 1.386(5) . ? C23 C24 1.389(5) . ? C24 C25 1.386(5) . ? C25 C26 1.393(6) . ? C26 C27 1.376(6) . ? C27 C28 1.388(6) . ? C33 C38 1.384(5) . ? C33 C34 1.403(5) . ? C34 C35 1.397(5) . ? C35 C36 1.391(5) . ? C36 C37 1.377(5) . ? C37 C38 1.394(5) . ? Cl1 C40 1.748(4) . ? Cl2 C40 1.757(5) . ? Cl3 C40 1.749(5) . ? 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 Co O2 179.999(1) . 2_666 ? O2 Co O1 91.16(9) . 2_666 ? O2 Co O1 88.84(9) 2_666 2_666 ? O2 Co O1 88.84(9) . . ? O2 Co O1 91.16(9) 2_666 . ? O1 Co O1 180.00(13) 2_666 . ? O2 Co O3 87.72(9) . . ? O2 Co O3 92.28(9) 2_666 . ? O1 Co O3 89.15(9) 2_666 . ? O1 Co O3 90.85(9) . . ? O2 Co O3 92.28(9) . 2_666 ? O2 Co O3 87.72(9) 2_666 2_666 ? O1 Co O3 90.85(9) 2_666 2_666 ? O1 Co O3 89.15(9) . 2_666 ? O3 Co O3 180.0 . 2_666 ? H1 B N11 106.5(17) . . ? H1 B N31 104.8(16) . . ? N11 B N31 112.5(3) . . ? H1 B N21 111.5(17) . . ? N11 B N21 111.3(3) . . ? N31 B N21 110.0(3) . . ? C12 N11 C14 107.7(3) . . ? C12 N11 B 127.7(3) . . ? C14 N11 B 124.3(3) . . ? C12 N12 C13 109.3(3) . . ? C12 N12 C11 123.7(3) . . ? C13 N12 C11 126.8(3) . . ? C22 N21 C24 107.9(3) . . ? C22 N21 B 127.4(3) . . ? C24 N21 B 123.7(3) . . ? C22 N22 C23 109.8(3) . . ? C22 N22 C21 122.9(3) . . ? C23 N22 C21 127.0(3) . . ? C32 N31 C34 107.2(3) . . ? C32 N31 B 128.0(3) . . ? C34 N31 B 124.7(3) . . ? C32 N32 C33 109.8(3) . . ? C32 N32 C31 123.0(3) . . ? C33 N32 C31 127.2(3) . . ? C12 O1 Co 123.1(2) . . ? C22 O2 Co 121.4(2) . . ? C32 O3 Co 124.2(2) . . ? O1 C12 N11 127.3(3) . . ? O1 C12 N12 124.4(3) . . ? N11 C12 N12 108.4(3) . . ? C18 C13 N12 131.6(4) . . ? C18 C13 C14 121.7(4) . . ? N12 C13 C14 106.7(3) . . ? C15 C14 C13 121.1(3) . . ? C15 C14 N11 131.0(3) . . ? C13 C14 N11 107.9(3) . . ? C14 C15 C16 117.3(4) . . ? C17 C16 C15 121.9(4) . . ? C16 C17 C18 120.7(4) . . ? C13 C18 C17 117.4(4) . . ? O2 C22 N21 127.5(3) . . ? O2 C22 N22 124.9(3) . . ? N21 C22 N22 107.6(3) . . ? N22 C23 C28 131.6(4) . . ? N22 C23 C24 106.3(3) . . ? C28 C23 C24 122.1(4) . . ? C25 C24 C23 120.8(3) . . ? C25 C24 N21 130.9(3) . . ? C23 C24 N21 108.4(3) . . ? C24 C25 C26 117.2(4) . . ? C27 C26 C25 121.6(4) . . ? C26 C27 C28 121.7(4) . . ? C23 C28 C27 116.6(4) . . ? O3 C32 N32 123.2(3) . . ? O3 C32 N31 128.0(3) . . ? N32 C32 N31 108.8(3) . . ? N32 C33 C38 132.2(3) . . ? N32 C33 C34 105.9(3) . . ? C38 C33 C34 121.9(3) . . ? C35 C34 N31 130.8(3) . . ? C35 C34 C33 120.8(3) . . ? N31 C34 C33 108.4(3) . . ? C36 C35 C34 116.3(3) . . ? C37 C36 C35 122.9(3) . . ? C36 C37 C38 121.0(4) . . ? C33 C38 C37 117.0(3) . . ? Cl1 C40 Cl3 111.0(2) . . ? Cl1 C40 Cl2 110.0(2) . . ? Cl3 C40 Cl2 110.0(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 30.47 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.535 _refine_diff_density_min -0.702 _refine_diff_density_rms 0.083 # Attachment '- TOZRCL.cif' data_tozrcl _database_code_depnum_ccdc_archive 'CCDC 794061' #TrackingRef '- TOZRCL.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H52 B Cl3 N6 O3 Zr' _chemical_formula_weight 861.25 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' 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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 16.242(2) _cell_length_b 16.242(2) _cell_length_c 9.4661(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2162.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9885 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 29.77 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.482 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.8932 _exptl_absorpt_correction_T_max 0.9763 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 35051 _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 30.50 _reflns_number_total 4410 _reflns_number_gt 3381 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+0.8094P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4410 _refine_ls_number_parameters 111 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1139 _refine_ls_wR_factor_gt 0.1087 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.018 922 264 ' ' _platon_squeeze_details ; The unit cell contains 6 benzene molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; 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 Zr Zr 0.3333 0.6667 0.10566(3) 0.03010(10) Uani 1 3 d S . . B B 0.3333 0.6667 0.5244(4) 0.0316(8) Uani 1 3 d S . . H1 H 0.3333 0.6667 0.642(4) 0.024(9) Uiso 1 3 d S . . Cl Cl 0.24008(4) 0.71851(5) -0.03216(6) 0.04857(16) Uani 1 1 d . . . O O 0.21815(10) 0.60246(10) 0.24335(14) 0.0341(3) Uani 1 1 d . . . N11 N 0.24238(12) 0.57398(12) 0.47769(16) 0.0321(4) Uani 1 1 d . . . C11 C 0.19197(14) 0.55285(14) 0.3581(2) 0.0299(4) Uani 1 1 d . . . N12 N 0.10844(12) 0.47045(13) 0.37418(18) 0.0360(4) Uani 1 1 d . . . C12 C 0.18984(15) 0.49999(15) 0.5735(2) 0.0366(4) Uani 1 1 d . . . H12A H 0.2083 0.4958 0.6672 0.044 Uiso 1 1 calc R . . C13 C 0.10918(17) 0.43624(16) 0.5100(2) 0.0423(5) Uani 1 1 d . . . H13A H 0.0611 0.3783 0.5497 0.051 Uiso 1 1 calc R . . C14 C 0.02816(17) 0.42471(19) 0.2709(2) 0.0480(6) Uani 1 1 d . . . C15 C 0.0511(3) 0.3717(3) 0.1605(4) 0.1097(17) Uani 1 1 d . . . H15A H 0.0631 0.3248 0.2069 0.165 Uiso 1 1 calc R . . H15B H 0.1077 0.4168 0.1075 0.165 Uiso 1 1 calc R . . H15C H -0.0028 0.3391 0.0955 0.165 Uiso 1 1 calc R . . C16 C 0.0132(2) 0.5019(3) 0.2000(3) 0.0776(10) Uani 1 1 d . . . H16A H -0.0468 0.4715 0.1474 0.116 Uiso 1 1 calc R . . H16B H 0.0659 0.5392 0.1349 0.116 Uiso 1 1 calc R . . H16C H 0.0111 0.5438 0.2725 0.116 Uiso 1 1 calc R . . C17 C -0.06255(18) 0.3588(2) 0.3508(3) 0.0626(8) Uani 1 1 d . . . H17A H -0.1169 0.3345 0.2861 0.094 Uiso 1 1 calc R . . H17B H -0.0715 0.3939 0.4278 0.094 Uiso 1 1 calc R . . H17C H -0.0578 0.3055 0.3899 0.094 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 Zr 0.03496(13) 0.03496(13) 0.02038(15) 0.000 0.000 0.01748(6) B 0.0357(12) 0.0357(12) 0.0235(16) 0.000 0.000 0.0179(6) Cl 0.0550(3) 0.0612(4) 0.0365(3) 0.0096(2) -0.0046(2) 0.0343(3) O 0.0368(7) 0.0389(8) 0.0253(6) 0.0049(6) 0.0001(5) 0.0181(6) N11 0.0366(9) 0.0348(9) 0.0261(8) 0.0038(6) 0.0018(6) 0.0187(7) C11 0.0328(10) 0.0323(9) 0.0270(9) 0.0028(7) 0.0016(7) 0.0180(8) N12 0.0347(9) 0.0384(9) 0.0311(8) 0.0037(7) 0.0009(7) 0.0155(8) C12 0.0427(11) 0.0399(11) 0.0289(9) 0.0095(8) 0.0043(8) 0.0219(9) C13 0.0468(12) 0.0386(11) 0.0360(11) 0.0090(9) 0.0065(9) 0.0171(10) C14 0.0341(11) 0.0551(14) 0.0394(12) -0.0068(10) -0.0004(9) 0.0107(10) C15 0.059(2) 0.137(4) 0.099(3) -0.076(3) -0.0075(19) 0.023(2) C16 0.0485(16) 0.099(3) 0.0619(18) 0.0324(17) -0.0112(14) 0.0192(16) C17 0.0399(13) 0.0702(18) 0.0536(15) 0.0112(14) -0.0022(11) 0.0094(13) _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 Zr O 2.0821(14) . ? Zr O 2.0821(14) 3_565 ? Zr O 2.0821(14) 2_665 ? Zr Cl 2.4455(6) . ? Zr Cl 2.4455(6) 3_565 ? Zr Cl 2.4455(6) 2_665 ? B H1 1.11(3) . ? B N11 1.556(2) 3_565 ? B N11 1.556(2) . ? B N11 1.556(2) 2_665 ? O C11 1.291(2) . ? N11 C11 1.337(2) . ? N11 C12 1.403(3) . ? C11 N12 1.356(3) . ? N12 C13 1.403(3) . ? N12 C14 1.496(3) . ? C12 C13 1.339(3) . ? C14 C15 1.514(4) . ? C14 C17 1.520(3) . ? C14 C16 1.544(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O Zr O 84.96(6) . 3_565 ? O Zr O 84.96(6) . 2_665 ? O Zr O 84.96(6) 3_565 2_665 ? O Zr Cl 87.15(4) . . ? O Zr Cl 93.50(4) 3_565 . ? O Zr Cl 172.07(4) 2_665 . ? O Zr Cl 172.07(4) . 3_565 ? O Zr Cl 87.15(4) 3_565 3_565 ? O Zr Cl 93.50(4) 2_665 3_565 ? Cl Zr Cl 94.19(2) . 3_565 ? O Zr Cl 93.50(4) . 2_665 ? O Zr Cl 172.07(4) 3_565 2_665 ? O Zr Cl 87.15(4) 2_665 2_665 ? Cl Zr Cl 94.19(2) . 2_665 ? Cl Zr Cl 94.19(2) 3_565 2_665 ? H1 B N11 106.51(14) . 3_565 ? H1 B N11 106.51(14) . . ? N11 B N11 112.26(12) 3_565 . ? H1 B N11 106.51(14) . 2_665 ? N11 B N11 112.26(12) 3_565 2_665 ? N11 B N11 112.26(12) . 2_665 ? C11 O Zr 140.55(13) . . ? C11 N11 C12 107.16(17) . . ? C11 N11 B 130.70(18) . . ? C12 N11 B 121.45(19) . . ? O C11 N11 125.70(18) . . ? O C11 N12 124.41(18) . . ? N11 C11 N12 109.88(16) . . ? C11 N12 C13 106.94(17) . . ? C11 N12 C14 127.60(17) . . ? C13 N12 C14 125.43(18) . . ? C13 C12 N11 108.25(18) . . ? C12 C13 N12 107.68(19) . . ? N12 C14 C15 109.4(2) . . ? N12 C14 C17 108.79(19) . . ? C15 C14 C17 111.7(3) . . ? N12 C14 C16 109.4(2) . . ? C15 C14 C16 110.1(3) . . ? C17 C14 C16 107.3(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.767 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.061 # Attachment '- cpzrtos10.cif' data_cpzrtos10 _database_code_depnum_ccdc_archive 'CCDC 794062' #TrackingRef '- cpzrtos10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H33 B Cl2 N6 O3 Zr' _chemical_formula_weight 758.60 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' 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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0122(17) _cell_length_b 12.326(2) _cell_length_c 15.991(3) _cell_angle_alpha 69.229(2) _cell_angle_beta 72.820(2) _cell_angle_gamma 71.988(2) _cell_volume 1716.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 7908 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 30.42 _exptl_crystal_description PLATE _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 0.521 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.9120 _exptl_absorpt_correction_T_max 0.9948 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 28027 _diffrn_reflns_av_R_equivalents 0.0722 _diffrn_reflns_av_sigmaI/netI 0.1005 _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 -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 30.61 _reflns_number_total 10491 _reflns_number_gt 6878 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0290P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10491 _refine_ls_number_parameters 439 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0939 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.0922 _refine_ls_wR_factor_gt 0.0798 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Zr Zr 0.22896(3) 0.17182(2) 0.096671(17) 0.01468(7) Uani 1 1 d . . . Cl1 Cl 0.46355(7) 0.23117(6) 0.04395(4) 0.02218(14) Uani 1 1 d . . . Cl2 Cl 0.33170(7) -0.03529(5) 0.17990(4) 0.02095(14) Uani 1 1 d . . . B B -0.0473(3) 0.3520(3) 0.27492(19) 0.0155(6) Uani 1 1 d . . . H1 H -0.124(3) 0.403(2) 0.3216(17) 0.019 Uiso 1 1 d . . . N12 N 0.1891(2) 0.52073(19) 0.07780(14) 0.0194(5) Uani 1 1 d . . . N11 N 0.0423(2) 0.43815(17) 0.20146(14) 0.0140(4) Uani 1 1 d . . . N22 N -0.2196(2) 0.18267(18) 0.20345(14) 0.0163(4) Uani 1 1 d . . . N21 N -0.1378(2) 0.30903(18) 0.23487(14) 0.0146(4) Uani 1 1 d . . . N32 N 0.2348(2) 0.10125(19) 0.37480(14) 0.0170(5) Uani 1 1 d . . . N31 N 0.0491(2) 0.24505(18) 0.33187(13) 0.0136(4) Uani 1 1 d . . . O1 O 0.12114(18) 0.35641(15) 0.07892(11) 0.0181(4) Uani 1 1 d . . . O2 O 0.02561(17) 0.14624(15) 0.19057(11) 0.0162(4) Uani 1 1 d . . . O3 O 0.25027(17) 0.20163(15) 0.21979(11) 0.0151(4) Uani 1 1 d . . . C1 C 0.2941(3) 0.0641(3) -0.0241(2) 0.0310(7) Uani 1 1 d . . . H1A H 0.3709 -0.0101 -0.0263 0.037 Uiso 1 1 calc R . . C2 C 0.1482(3) 0.0682(3) 0.0168(2) 0.0286(7) Uani 1 1 d . . . H2A H 0.1036 -0.0022 0.0471 0.034 Uiso 1 1 calc R . . C3 C 0.0733(3) 0.1880(3) -0.00693(18) 0.0265(7) Uani 1 1 d . . . H3A H -0.0335 0.2171 0.0038 0.032 Uiso 1 1 calc R . . C4 C 0.1727(3) 0.2568(3) -0.06216(18) 0.0291(7) Uani 1 1 d . . . H4A H 0.1485 0.3434 -0.0961 0.035 Uiso 1 1 calc R . . C5 C 0.3086(3) 0.1800(3) -0.07310(18) 0.0294(7) Uani 1 1 d . . . H5A H 0.3980 0.2030 -0.1153 0.035 Uiso 1 1 calc R . . C11 C 0.2753(3) 0.5440(3) -0.01433(19) 0.0319(7) Uani 1 1 d . . . H11A H 0.3288 0.4683 -0.0270 0.048 Uiso 1 1 calc R . . H11B H 0.3429 0.5906 -0.0203 0.048 Uiso 1 1 calc R . . H11C H 0.2125 0.5890 -0.0580 0.048 Uiso 1 1 calc R . . C12 C 0.1183(3) 0.4316(2) 0.11767(17) 0.0165(5) Uani 1 1 d . . . C13 C 0.1603(3) 0.5868(2) 0.13823(18) 0.0203(6) Uani 1 1 d . . . C14 C 0.0679(3) 0.5353(2) 0.21621(18) 0.0178(5) Uani 1 1 d . . . C15 C 0.0208(3) 0.5788(2) 0.2911(2) 0.0246(6) Uani 1 1 d . . . H15A H -0.0414 0.5433 0.3447 0.029 Uiso 1 1 calc R . . C16 C 0.0684(3) 0.6766(3) 0.2843(2) 0.0322(7) Uani 1 1 d . . . H16A H 0.0372 0.7094 0.3343 0.039 Uiso 1 1 calc R . . C17 C 0.1606(3) 0.7278(3) 0.2062(2) 0.0333(7) Uani 1 1 d . . . H17A H 0.1915 0.7944 0.2042 0.040 Uiso 1 1 calc R . . C18 C 0.2086(3) 0.6840(2) 0.1313(2) 0.0280(7) Uani 1 1 d . . . H18A H 0.2715 0.7190 0.0778 0.034 Uiso 1 1 calc R . . C21 C -0.2227(3) 0.0803(2) 0.1797(2) 0.0278(7) Uani 1 1 d . . . H21A H -0.1262 0.0284 0.1730 0.042 Uiso 1 1 calc R . . H21B H -0.2550 0.1075 0.1219 0.042 Uiso 1 1 calc R . . H21C H -0.2891 0.0360 0.2282 0.042 Uiso 1 1 calc R . . C22 C -0.1001(3) 0.2094(2) 0.20812(16) 0.0142(5) Uani 1 1 d . . . C23 C -0.3383(3) 0.2687(2) 0.22701(17) 0.0179(5) Uani 1 1 d . . . C24 C -0.2870(3) 0.3494(2) 0.24515(16) 0.0157(5) Uani 1 1 d . . . C25 C -0.3780(3) 0.4507(2) 0.26587(17) 0.0210(6) Uani 1 1 d . . . H25A H -0.3432 0.5069 0.2768 0.025 Uiso 1 1 calc R . . C26 C -0.5232(3) 0.4660(3) 0.26985(19) 0.0284(7) Uani 1 1 d . . . H26A H -0.5895 0.5341 0.2844 0.034 Uiso 1 1 calc R . . C27 C -0.5738(3) 0.3839(3) 0.25305(19) 0.0279(7) Uani 1 1 d . . . H27A H -0.6739 0.3971 0.2571 0.034 Uiso 1 1 calc R . . C28 C -0.4825(3) 0.2845(3) 0.23072(18) 0.0247(6) Uani 1 1 d . . . H28A H -0.5169 0.2292 0.2184 0.030 Uiso 1 1 calc R . . C31 C 0.3755(3) 0.0208(2) 0.37031(19) 0.0235(6) Uani 1 1 d . . . H31A H 0.4209 0.0243 0.3064 0.035 Uiso 1 1 calc R . . H31B H 0.3657 -0.0607 0.4050 0.035 Uiso 1 1 calc R . . H31C H 0.4352 0.0444 0.3966 0.035 Uiso 1 1 calc R . . C32 C 0.1822(3) 0.1838(2) 0.30200(17) 0.0146(5) Uani 1 1 d . . . C33 C 0.1313(3) 0.1083(2) 0.45380(17) 0.0176(5) Uani 1 1 d . . . C34 C 0.0141(3) 0.1981(2) 0.42730(16) 0.0157(5) Uani 1 1 d . . . C35 C -0.1094(3) 0.2247(2) 0.49032(18) 0.0200(6) Uani 1 1 d . . . H35A H -0.1894 0.2859 0.4723 0.024 Uiso 1 1 calc R . . C36 C -0.1121(3) 0.1585(2) 0.58110(18) 0.0232(6) Uani 1 1 d . . . H36A H -0.1958 0.1748 0.6261 0.028 Uiso 1 1 calc R . . C37 C 0.0042(3) 0.0693(2) 0.60767(18) 0.0247(6) Uani 1 1 d . . . H37A H -0.0013 0.0258 0.6705 0.030 Uiso 1 1 calc R . . C38 C 0.1284(3) 0.0420(2) 0.54453(18) 0.0228(6) Uani 1 1 d . . . H38A H 0.2082 -0.0195 0.5626 0.027 Uiso 1 1 calc R . . C51 C 0.6361(5) 0.7271(4) 0.4741(3) 0.0614(12) Uani 1 1 d . . . H51A H 0.6653 0.7276 0.5253 0.074 Uiso 1 1 calc R . . C52 C 0.6991(4) 0.7840(3) 0.3869(3) 0.0493(10) Uani 1 1 d . . . H52A H 0.7714 0.8246 0.3774 0.059 Uiso 1 1 calc R . . C53 C 0.6561(4) 0.7815(3) 0.3136(2) 0.0368(8) Uani 1 1 d . . . H53A H 0.6991 0.8204 0.2532 0.044 Uiso 1 1 calc R . . C54 C 0.5520(3) 0.7235(3) 0.3270(2) 0.0335(7) Uani 1 1 d . . . H54A H 0.5226 0.7228 0.2759 0.040 Uiso 1 1 calc R . . C55 C 0.4899(4) 0.6664(3) 0.4134(2) 0.0432(9) Uani 1 1 d . . . H55A H 0.4188 0.6248 0.4224 0.052 Uiso 1 1 calc R . . C56 C 0.5304(5) 0.6692(4) 0.4870(3) 0.0608(12) Uani 1 1 d . . . H56A H 0.4856 0.6311 0.5473 0.073 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 Zr 0.01370(12) 0.01644(13) 0.01322(13) -0.00535(10) -0.00277(9) -0.00133(10) Cl1 0.0182(3) 0.0266(4) 0.0197(3) -0.0065(3) 0.0012(3) -0.0075(3) Cl2 0.0220(3) 0.0161(3) 0.0241(3) -0.0053(3) -0.0072(3) -0.0018(3) B 0.0173(14) 0.0169(15) 0.0122(14) -0.0039(11) -0.0015(11) -0.0057(12) N12 0.0184(11) 0.0164(11) 0.0181(12) -0.0001(9) -0.0015(9) -0.0047(9) N11 0.0145(10) 0.0130(10) 0.0149(11) -0.0040(8) -0.0035(8) -0.0032(8) N22 0.0150(11) 0.0183(11) 0.0177(11) -0.0043(9) -0.0043(9) -0.0071(9) N21 0.0123(10) 0.0151(11) 0.0166(11) -0.0042(9) -0.0035(8) -0.0031(8) N32 0.0163(11) 0.0194(11) 0.0162(11) -0.0059(9) -0.0053(9) -0.0027(9) N31 0.0123(10) 0.0165(11) 0.0119(10) -0.0032(8) -0.0017(8) -0.0051(8) O1 0.0214(10) 0.0165(9) 0.0139(9) -0.0037(7) -0.0034(7) -0.0020(8) O2 0.0120(9) 0.0160(9) 0.0195(9) -0.0055(7) -0.0034(7) -0.0012(7) O3 0.0140(9) 0.0194(9) 0.0129(9) -0.0055(7) -0.0012(7) -0.0058(7) C1 0.0301(17) 0.0398(19) 0.0283(16) -0.0263(15) -0.0117(13) 0.0094(14) C2 0.0364(17) 0.0343(17) 0.0264(16) -0.0170(13) -0.0119(13) -0.0088(14) C3 0.0206(14) 0.0399(18) 0.0209(15) -0.0141(13) -0.0096(12) 0.0015(13) C4 0.0370(18) 0.0319(17) 0.0157(14) -0.0061(12) -0.0117(13) 0.0007(14) C5 0.0296(16) 0.048(2) 0.0132(14) -0.0139(13) -0.0023(12) -0.0085(15) C11 0.0348(18) 0.0253(16) 0.0210(15) 0.0013(12) 0.0065(13) -0.0079(13) C12 0.0146(12) 0.0144(13) 0.0168(13) -0.0009(10) -0.0054(10) -0.0002(10) C13 0.0182(13) 0.0144(13) 0.0247(15) -0.0003(11) -0.0076(11) -0.0022(11) C14 0.0191(13) 0.0137(12) 0.0228(14) -0.0035(11) -0.0101(11) -0.0034(10) C15 0.0229(15) 0.0262(15) 0.0287(16) -0.0120(13) -0.0034(12) -0.0083(12) C16 0.0353(18) 0.0300(17) 0.0408(19) -0.0193(15) -0.0085(15) -0.0096(14) C17 0.0342(18) 0.0199(15) 0.052(2) -0.0077(15) -0.0162(16) -0.0106(13) C18 0.0239(15) 0.0203(15) 0.0376(18) 0.0001(13) -0.0104(13) -0.0083(12) C21 0.0277(16) 0.0261(16) 0.0372(17) -0.0134(13) -0.0080(13) -0.0104(13) C22 0.0145(12) 0.0165(13) 0.0121(12) -0.0025(10) -0.0031(10) -0.0056(10) C23 0.0150(13) 0.0205(14) 0.0152(13) -0.0019(11) -0.0030(10) -0.0038(11) C24 0.0115(12) 0.0218(14) 0.0122(12) -0.0025(10) -0.0036(10) -0.0033(10) C25 0.0190(14) 0.0245(15) 0.0193(14) -0.0062(11) -0.0075(11) -0.0014(11) C26 0.0214(15) 0.0318(16) 0.0262(16) -0.0103(13) -0.0081(12) 0.0072(13) C27 0.0130(13) 0.0410(18) 0.0275(16) -0.0102(14) -0.0065(12) -0.0005(13) C28 0.0197(14) 0.0335(17) 0.0221(15) -0.0035(12) -0.0073(12) -0.0102(12) C31 0.0199(14) 0.0249(15) 0.0259(15) -0.0075(12) -0.0084(12) -0.0018(12) C32 0.0155(12) 0.0149(12) 0.0158(13) -0.0050(10) -0.0035(10) -0.0060(10) C33 0.0224(14) 0.0193(13) 0.0161(13) -0.0068(11) -0.0042(11) -0.0092(11) C34 0.0210(13) 0.0152(13) 0.0135(12) -0.0029(10) -0.0054(10) -0.0073(10) C35 0.0231(14) 0.0206(14) 0.0204(14) -0.0087(11) -0.0036(11) -0.0086(11) C36 0.0296(16) 0.0251(15) 0.0152(13) -0.0076(11) 0.0044(11) -0.0134(12) C37 0.0383(17) 0.0254(15) 0.0136(13) -0.0019(11) -0.0030(12) -0.0183(13) C38 0.0343(16) 0.0197(14) 0.0171(14) -0.0023(11) -0.0094(12) -0.0097(12) C51 0.070(3) 0.074(3) 0.039(2) -0.027(2) -0.025(2) 0.010(2) C52 0.040(2) 0.059(3) 0.059(3) -0.035(2) -0.0078(19) -0.0068(19) C53 0.046(2) 0.0314(18) 0.0296(18) -0.0114(14) 0.0038(15) -0.0125(16) C54 0.0413(19) 0.0261(16) 0.0326(18) -0.0124(14) -0.0096(15) -0.0005(14) C55 0.044(2) 0.0323(19) 0.040(2) -0.0083(16) 0.0063(16) -0.0068(16) C56 0.076(3) 0.058(3) 0.024(2) -0.0015(18) -0.001(2) -0.003(2) _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 Zr O1 2.1508(17) . ? Zr O2 2.1805(17) . ? Zr O3 2.2059(17) . ? Zr Cl2 2.4741(7) . ? Zr Cl1 2.4936(8) . ? Zr C3 2.512(3) . ? Zr C2 2.515(3) . ? Zr C4 2.541(3) . ? Zr C1 2.542(3) . ? Zr C5 2.568(3) . ? B H1 1.11(2) . ? B N31 1.543(3) . ? B N21 1.546(3) . ? B N11 1.547(3) . ? N12 C12 1.355(3) . ? N12 C13 1.388(3) . ? N12 C11 1.449(3) . ? N11 C12 1.348(3) . ? N11 C14 1.408(3) . ? N22 C22 1.364(3) . ? N22 C23 1.385(3) . ? N22 C21 1.452(3) . ? N21 C22 1.351(3) . ? N21 C24 1.400(3) . ? N32 C32 1.363(3) . ? N32 C33 1.388(3) . ? N32 C31 1.449(3) . ? N31 C32 1.353(3) . ? N31 C34 1.403(3) . ? O1 C12 1.274(3) . ? O2 C22 1.268(3) . ? O3 C32 1.265(3) . ? C1 C5 1.395(4) . ? C1 C2 1.406(4) . ? C2 C3 1.405(4) . ? C3 C4 1.400(4) . ? C4 C5 1.400(4) . ? C13 C18 1.383(4) . ? C13 C14 1.391(4) . ? C14 C15 1.381(4) . ? C15 C16 1.388(4) . ? C16 C17 1.389(4) . ? C17 C18 1.384(4) . ? C23 C28 1.382(3) . ? C23 C24 1.394(3) . ? C24 C25 1.383(4) . ? C25 C26 1.392(4) . ? C26 C27 1.394(4) . ? C27 C28 1.376(4) . ? C33 C38 1.387(3) . ? C33 C34 1.392(3) . ? C34 C35 1.378(3) . ? C35 C36 1.387(4) . ? C36 C37 1.384(4) . ? C37 C38 1.386(4) . ? C51 C52 1.377(5) . ? C51 C56 1.380(6) . ? C52 C53 1.375(5) . ? C53 C54 1.365(4) . ? C54 C55 1.365(4) . ? C55 C56 1.367(5) . ? 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 Zr O2 81.88(6) . . ? O1 Zr O3 78.08(6) . . ? O2 Zr O3 77.51(6) . . ? O1 Zr Cl2 157.05(5) . . ? O2 Zr Cl2 86.14(5) . . ? O3 Zr Cl2 80.26(5) . . ? O1 Zr Cl1 88.99(5) . . ? O2 Zr Cl1 155.19(5) . . ? O3 Zr Cl1 78.05(5) . . ? Cl2 Zr Cl1 93.89(2) . . ? O1 Zr C3 82.06(8) . . ? O2 Zr C3 76.86(8) . . ? O3 Zr C3 149.43(8) . . ? Cl2 Zr C3 114.19(7) . . ? Cl1 Zr C3 124.81(7) . . ? O1 Zr C2 114.46(8) . . ? O2 Zr C2 80.70(8) . . ? O3 Zr C2 152.98(8) . . ? Cl2 Zr C2 82.54(7) . . ? Cl1 Zr C2 123.95(7) . . ? C3 Zr C2 32.46(9) . . ? O1 Zr C4 72.23(8) . . ? O2 Zr C4 105.51(8) . . ? O3 Zr C4 149.25(8) . . ? Cl2 Zr C4 130.16(7) . . ? Cl1 Zr C4 93.41(7) . . ? C3 Zr C4 32.15(9) . . ? C2 Zr C4 53.31(10) . . ? O1 Zr C1 125.04(8) . . ? O2 Zr C1 112.01(9) . . ? O3 Zr C1 155.13(8) . . ? Cl2 Zr C1 77.65(7) . . ? Cl1 Zr C1 92.13(7) . . ? C3 Zr C1 53.34(9) . . ? C2 Zr C1 32.29(9) . . ? C4 Zr C1 52.85(10) . . ? O1 Zr C5 97.64(8) . . ? O2 Zr C5 129.09(8) . . ? O3 Zr C5 152.64(8) . . ? Cl2 Zr C5 105.10(7) . . ? Cl1 Zr C5 74.84(7) . . ? C3 Zr C5 52.99(9) . . ? C2 Zr C5 53.02(10) . . ? C4 Zr C5 31.79(9) . . ? C1 Zr C5 31.68(10) . . ? H1 B N31 108.0(13) . . ? H1 B N21 107.0(13) . . ? N31 B N21 110.8(2) . . ? H1 B N11 106.6(13) . . ? N31 B N11 111.0(2) . . ? N21 B N11 113.2(2) . . ? C12 N12 C13 108.7(2) . . ? C12 N12 C11 124.5(2) . . ? C13 N12 C11 126.7(2) . . ? C12 N11 C14 107.4(2) . . ? C12 N11 B 128.8(2) . . ? C14 N11 B 123.6(2) . . ? C22 N22 C23 108.4(2) . . ? C22 N22 C21 126.0(2) . . ? C23 N22 C21 125.7(2) . . ? C22 N21 C24 107.2(2) . . ? C22 N21 B 127.4(2) . . ? C24 N21 B 123.2(2) . . ? C32 N32 C33 108.4(2) . . ? C32 N32 C31 125.7(2) . . ? C33 N32 C31 125.9(2) . . ? C32 N31 C34 107.6(2) . . ? C32 N31 B 127.8(2) . . ? C34 N31 B 124.5(2) . . ? C12 O1 Zr 132.31(16) . . ? C22 O2 Zr 137.14(16) . . ? C32 O3 Zr 135.07(15) . . ? C5 C1 C2 108.2(3) . . ? C5 C1 Zr 75.18(16) . . ? C2 C1 Zr 72.82(15) . . ? C3 C2 C1 107.6(3) . . ? C3 C2 Zr 73.64(15) . . ? C1 C2 Zr 74.89(16) . . ? C4 C3 C2 108.0(3) . . ? C4 C3 Zr 75.09(16) . . ? C2 C3 Zr 73.90(15) . . ? C3 C4 C5 108.1(3) . . ? C3 C4 Zr 72.76(15) . . ? C5 C4 Zr 75.13(16) . . ? C1 C5 C4 108.1(3) . . ? C1 C5 Zr 73.13(16) . . ? C4 C5 Zr 73.08(15) . . ? O1 C12 N11 126.3(2) . . ? O1 C12 N12 123.9(2) . . ? N11 C12 N12 109.8(2) . . ? C18 C13 N12 131.4(3) . . ? C18 C13 C14 122.0(3) . . ? N12 C13 C14 106.6(2) . . ? C15 C14 C13 121.2(2) . . ? C15 C14 N11 131.2(2) . . ? C13 C14 N11 107.5(2) . . ? C14 C15 C16 117.0(3) . . ? C15 C16 C17 121.6(3) . . ? C18 C17 C16 121.6(3) . . ? C13 C18 C17 116.7(3) . . ? O2 C22 N21 127.0(2) . . ? O2 C22 N22 123.1(2) . . ? N21 C22 N22 109.9(2) . . ? C28 C23 N22 131.4(3) . . ? C28 C23 C24 121.9(2) . . ? N22 C23 C24 106.7(2) . . ? C25 C24 C23 121.5(2) . . ? C25 C24 N21 130.6(2) . . ? C23 C24 N21 107.9(2) . . ? C24 C25 C26 116.4(3) . . ? C25 C26 C27 121.7(3) . . ? C28 C27 C26 121.6(3) . . ? C27 C28 C23 116.9(3) . . ? O3 C32 N31 125.9(2) . . ? O3 C32 N32 124.6(2) . . ? N31 C32 N32 109.5(2) . . ? C38 C33 N32 131.5(2) . . ? C38 C33 C34 121.4(2) . . ? N32 C33 C34 107.0(2) . . ? C35 C34 C33 121.3(2) . . ? C35 C34 N31 131.3(2) . . ? C33 C34 N31 107.4(2) . . ? C34 C35 C36 117.3(3) . . ? C37 C36 C35 121.6(3) . . ? C36 C37 C38 121.3(2) . . ? C37 C38 C33 117.1(3) . . ? C52 C51 C56 119.9(4) . . ? C53 C52 C51 119.2(4) . . ? C54 C53 C52 120.5(3) . . ? C55 C54 C53 120.4(3) . . ? C54 C55 C56 119.8(4) . . ? C55 C56 C51 120.2(4) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.61 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.496 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.103 # Attachment '- klres10.cif' data_klres10 _database_code_depnum_ccdc_archive 'CCDC 794063' #TrackingRef '- klres10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H35 Co O12 P3 Re' _chemical_formula_weight 805.52 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 11.4131(7) _cell_length_b 18.4005(11) _cell_length_c 13.6761(8) _cell_angle_alpha 90.00 _cell_angle_beta 92.8560(10) _cell_angle_gamma 90.00 _cell_volume 2868.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9926 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 31.79 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.865 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 5.018 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6083 _exptl_absorpt_correction_T_max 0.9063 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 48946 _diffrn_reflns_av_R_equivalents 0.0705 _diffrn_reflns_av_sigmaI/netI 0.0632 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 32.48 _reflns_number_total 10043 _reflns_number_gt 7105 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+1.0814P] 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_extinction_coef ? _refine_ls_number_reflns 10043 _refine_ls_number_parameters 341 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0694 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0686 _refine_ls_wR_factor_gt 0.0601 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Re Re 0.643867(11) 0.104665(8) 0.260487(10) 0.01638(4) Uani 1 1 d . . . Co Co 0.31485(4) 0.19375(3) 0.26119(3) 0.01671(10) Uani 1 1 d . . . P1 P 0.47735(8) 0.25215(5) 0.28281(7) 0.01761(18) Uani 1 1 d . . . P2 P 0.38508(8) 0.13586(5) 0.13997(6) 0.01683(18) Uani 1 1 d . . . P3 P 0.38268(8) 0.11060(5) 0.36089(6) 0.01765(17) Uani 1 1 d . . . O1 O 0.7176(3) -0.04578(15) 0.1937(2) 0.0335(7) Uani 1 1 d . . . O2 O 0.8168(3) 0.08298(18) 0.4356(2) 0.0420(8) Uani 1 1 d . . . O3 O 0.8509(2) 0.16195(17) 0.1514(2) 0.0382(7) Uani 1 1 d . . . O11 O 0.5887(2) 0.20999(13) 0.30947(17) 0.0201(5) Uani 1 1 d . . . O12 O 0.4947(2) 0.29930(14) 0.18627(18) 0.0249(6) Uani 1 1 d . . . O13 O 0.4640(2) 0.31356(14) 0.36381(19) 0.0271(6) Uani 1 1 d . . . O21 O 0.5173(2) 0.12499(13) 0.14097(17) 0.0193(5) Uani 1 1 d . . . O22 O 0.3464(2) 0.16962(14) 0.03546(17) 0.0229(5) Uani 1 1 d . . . O23 O 0.3197(2) 0.05933(13) 0.12948(17) 0.0204(5) Uani 1 1 d . . . O31 O 0.4904(2) 0.06853(13) 0.33242(17) 0.0182(5) Uani 1 1 d . . . O32 O 0.2873(2) 0.05190(13) 0.39108(18) 0.0239(6) Uani 1 1 d . . . O33 O 0.4057(2) 0.14869(13) 0.46493(17) 0.0219(5) Uani 1 1 d . . . C1 C 0.6871(3) 0.0110(2) 0.2188(2) 0.0215(7) Uani 1 1 d . . . C2 C 0.7498(3) 0.0913(2) 0.3696(3) 0.0244(8) Uani 1 1 d . . . C3 C 0.7717(3) 0.1406(2) 0.1927(3) 0.0254(8) Uani 1 1 d . . . C43 C 0.1885(3) 0.2517(2) 0.1790(3) 0.0287(9) Uani 1 1 d . . . H4A H 0.1937 0.2667 0.1091 0.034 Uiso 1 1 calc R . . C44 C 0.1394(3) 0.1856(2) 0.2126(3) 0.0293(9) Uani 1 1 d . . . H5A H 0.1036 0.1461 0.1708 0.035 Uiso 1 1 calc R . . C45 C 0.1480(3) 0.1871(2) 0.3164(3) 0.0298(9) Uani 1 1 d . . . H6A H 0.1202 0.1482 0.3607 0.036 Uiso 1 1 calc R . . C41 C 0.2037(3) 0.2526(2) 0.3467(3) 0.0271(8) Uani 1 1 d . . . H7A H 0.2207 0.2687 0.4158 0.033 Uiso 1 1 calc R . . C42 C 0.2266(3) 0.2925(2) 0.2609(3) 0.0274(8) Uani 1 1 d . . . H8A H 0.2640 0.3415 0.2592 0.033 Uiso 1 1 calc R . . C11 C 0.6005(4) 0.3390(3) 0.1745(4) 0.0667(19) Uani 1 1 d . . . H11A H 0.6679 0.3053 0.1815 0.080 Uiso 1 1 calc R . . H11B H 0.6095 0.3758 0.2272 0.080 Uiso 1 1 calc R . . C12 C 0.6029(4) 0.3754(2) 0.0803(3) 0.0390(11) Uani 1 1 d . . . H12A H 0.6705 0.4082 0.0803 0.059 Uiso 1 1 calc R . . H12B H 0.5305 0.4034 0.0686 0.059 Uiso 1 1 calc R . . H12C H 0.6093 0.3391 0.0284 0.059 Uiso 1 1 calc R . . C13 C 0.5440(5) 0.3278(3) 0.4436(4) 0.0556(16) Uani 1 1 d . . . H13A H 0.6241 0.3139 0.4259 0.067 Uiso 1 1 calc R . . H13B H 0.5232 0.2980 0.5005 0.067 Uiso 1 1 calc R . . C14 C 0.5425(5) 0.4050(3) 0.4703(3) 0.0476(13) Uani 1 1 d . . . H14A H 0.6074 0.4153 0.5180 0.071 Uiso 1 1 calc R . . H14B H 0.4679 0.4166 0.4993 0.071 Uiso 1 1 calc R . . H14C H 0.5511 0.4348 0.4117 0.071 Uiso 1 1 calc R . . C21 C 0.4144(4) 0.2217(3) -0.0151(3) 0.0384(11) Uani 1 1 d . . . H21A H 0.4985 0.2087 -0.0081 0.046 Uiso 1 1 calc R . . H21B H 0.4043 0.2705 0.0139 0.046 Uiso 1 1 calc R . . C22 C 0.3762(4) 0.2233(2) -0.1200(3) 0.0322(9) Uani 1 1 d . . . H22A H 0.4211 0.2602 -0.1537 0.048 Uiso 1 1 calc R . . H22B H 0.2924 0.2352 -0.1267 0.048 Uiso 1 1 calc R . . H22C H 0.3896 0.1756 -0.1492 0.048 Uiso 1 1 calc R . . C23 C 0.3547(5) 0.0096(3) 0.0546(4) 0.0532(15) Uani 1 1 d . . . H23A H 0.3261 0.0290 -0.0098 0.064 Uiso 1 1 calc R . . H23B H 0.4414 0.0090 0.0553 0.064 Uiso 1 1 calc R . . C24 C 0.3169(8) -0.0597(3) 0.0616(5) 0.113(3) Uani 1 1 d . . . H24A H 0.3648 -0.0852 0.1122 0.169 Uiso 1 1 calc R . . H24B H 0.3237 -0.0843 -0.0014 0.169 Uiso 1 1 calc R . . H24C H 0.2347 -0.0599 0.0792 0.169 Uiso 1 1 calc R . . C31 C 0.2606(3) -0.0146(2) 0.3383(3) 0.0273(8) Uani 1 1 d . . . H31A H 0.2691 -0.0565 0.3834 0.033 Uiso 1 1 calc R . . H31B H 0.3163 -0.0210 0.2858 0.033 Uiso 1 1 calc R . . C32 C 0.1373(4) -0.0118(2) 0.2944(4) 0.0393(11) Uani 1 1 d . . . H32A H 0.1156 -0.0595 0.2673 0.059 Uiso 1 1 calc R . . H32B H 0.1324 0.0246 0.2420 0.059 Uiso 1 1 calc R . . H32C H 0.0834 0.0014 0.3451 0.059 Uiso 1 1 calc R . . C33 C 0.4694(4) 0.1087(3) 0.5421(3) 0.0370(10) Uani 1 1 d . . . H33A H 0.5548 0.1115 0.5328 0.044 Uiso 1 1 calc R . . H33B H 0.4459 0.0569 0.5400 0.044 Uiso 1 1 calc R . . C34 C 0.4423(3) 0.1410(2) 0.6384(3) 0.0298(9) Uani 1 1 d . . . H34A H 0.4873 0.1157 0.6909 0.045 Uiso 1 1 calc R . . H34B H 0.3583 0.1360 0.6484 0.045 Uiso 1 1 calc R . . H34C H 0.4635 0.1926 0.6391 0.045 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 Re 0.01373(6) 0.02020(7) 0.01520(6) -0.00021(6) 0.00043(4) 0.00261(6) Co 0.0141(2) 0.0188(2) 0.0172(2) -0.00010(18) 0.00067(17) 0.00239(18) P1 0.0166(4) 0.0178(4) 0.0183(4) -0.0008(4) -0.0001(3) 0.0010(3) P2 0.0152(4) 0.0219(5) 0.0134(4) 0.0010(3) 0.0001(3) 0.0011(3) P3 0.0175(4) 0.0196(5) 0.0161(4) 0.0004(4) 0.0034(3) 0.0017(4) O1 0.0384(17) 0.0268(15) 0.0357(16) -0.0028(13) 0.0051(13) 0.0089(13) O2 0.0342(17) 0.060(2) 0.0308(16) 0.0048(15) -0.0122(13) 0.0058(15) O3 0.0278(15) 0.0457(19) 0.0421(18) -0.0033(15) 0.0120(13) -0.0090(14) O11 0.0185(12) 0.0199(13) 0.0218(13) -0.0014(10) -0.0007(10) 0.0015(10) O12 0.0212(13) 0.0267(14) 0.0269(14) 0.0065(11) 0.0014(11) -0.0040(11) O13 0.0249(14) 0.0242(14) 0.0315(15) -0.0108(12) -0.0069(11) 0.0049(11) O21 0.0151(11) 0.0280(14) 0.0148(11) -0.0006(10) 0.0025(9) 0.0031(10) O22 0.0182(12) 0.0332(15) 0.0169(12) 0.0069(11) -0.0016(10) -0.0013(11) O23 0.0215(13) 0.0211(13) 0.0188(12) -0.0042(10) 0.0042(10) -0.0009(10) O31 0.0189(12) 0.0197(13) 0.0163(12) 0.0015(10) 0.0047(9) 0.0039(10) O32 0.0258(14) 0.0227(14) 0.0239(13) 0.0025(11) 0.0097(11) -0.0008(11) O33 0.0266(14) 0.0253(14) 0.0138(12) 0.0001(10) -0.0002(10) 0.0070(11) C1 0.0194(17) 0.030(2) 0.0156(17) 0.0037(15) 0.0037(13) 0.0025(15) C2 0.0229(18) 0.029(2) 0.0214(18) 0.0000(15) 0.0024(14) 0.0044(15) C3 0.0200(18) 0.032(2) 0.0238(19) -0.0022(16) -0.0003(15) -0.0017(16) C43 0.0203(19) 0.037(2) 0.028(2) 0.0045(18) -0.0051(15) 0.0139(17) C44 0.0146(17) 0.028(2) 0.045(3) -0.0069(19) -0.0034(16) 0.0050(15) C45 0.0174(18) 0.030(2) 0.043(3) 0.0036(19) 0.0099(17) 0.0055(16) C41 0.026(2) 0.028(2) 0.028(2) -0.0016(16) 0.0050(16) 0.0098(16) C42 0.0210(19) 0.023(2) 0.039(2) 0.0008(17) 0.0015(16) 0.0062(15) C11 0.032(3) 0.100(5) 0.067(4) 0.057(3) -0.019(2) -0.035(3) C12 0.034(2) 0.040(3) 0.044(3) 0.011(2) 0.013(2) -0.0048(19) C13 0.062(3) 0.058(3) 0.044(3) -0.028(2) -0.028(2) 0.031(3) C14 0.070(3) 0.042(3) 0.029(2) -0.005(2) -0.010(2) -0.025(3) C21 0.032(2) 0.050(3) 0.033(2) 0.018(2) -0.0053(18) -0.013(2) C22 0.030(2) 0.048(3) 0.0191(19) 0.0089(18) 0.0015(16) -0.0046(19) C23 0.074(4) 0.040(3) 0.049(3) -0.026(2) 0.037(3) -0.017(3) C24 0.220(9) 0.034(3) 0.094(5) -0.027(3) 0.105(6) -0.038(4) C31 0.030(2) 0.0209(19) 0.031(2) 0.0036(16) 0.0084(17) -0.0009(16) C32 0.029(2) 0.027(2) 0.063(3) -0.006(2) 0.004(2) -0.0041(18) C33 0.044(3) 0.045(3) 0.0212(19) -0.0026(19) -0.0040(17) 0.022(2) C34 0.029(2) 0.043(3) 0.0174(18) -0.0004(17) 0.0015(15) -0.0036(18) _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 Re C3 1.887(4) . ? Re C1 1.888(4) . ? Re C2 1.889(4) . ? Re O11 2.155(2) . ? Re O31 2.156(2) . ? Re O21 2.159(2) . ? Co C41 2.073(4) . ? Co C42 2.077(4) . ? Co C43 2.078(4) . ? Co C44 2.084(4) . ? Co C45 2.086(4) . ? Co P1 2.1511(10) . ? Co P2 2.1582(10) . ? Co P3 2.1665(10) . ? P1 O11 1.518(2) . ? P1 O13 1.595(3) . ? P1 O12 1.600(3) . ? P2 O21 1.522(2) . ? P2 O23 1.597(3) . ? P2 O22 1.600(2) . ? P3 O31 1.520(2) . ? P3 O33 1.596(2) . ? P3 O32 1.602(3) . ? O1 C1 1.159(4) . ? O2 C2 1.163(4) . ? O3 C3 1.157(4) . ? O12 C11 1.427(5) . ? O13 C13 1.412(5) . ? O22 C21 1.433(5) . ? O23 C23 1.444(5) . ? O32 C31 1.445(4) . ? O33 C33 1.452(4) . ? C43 C42 1.399(5) . ? C43 C44 1.424(6) . ? C44 C45 1.419(6) . ? C45 C41 1.414(6) . ? C41 C42 1.420(5) . ? C11 C12 1.454(6) . ? C13 C14 1.468(6) . ? C21 C22 1.479(5) . ? C23 C24 1.352(7) . ? C31 C32 1.503(5) . ? C33 C34 1.492(5) . ? 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 C3 Re C1 87.20(16) . . ? C3 Re C2 87.33(16) . . ? C1 Re C2 87.29(15) . . ? C3 Re O11 94.75(14) . . ? C1 Re O11 177.99(12) . . ? C2 Re O11 93.28(13) . . ? C3 Re O31 176.22(13) . . ? C1 Re O31 94.98(12) . . ? C2 Re O31 95.85(13) . . ? O11 Re O31 83.05(9) . . ? C3 Re O21 94.14(13) . . ? C1 Re O21 96.01(12) . . ? C2 Re O21 176.45(13) . . ? O11 Re O21 83.38(9) . . ? O31 Re O21 82.58(9) . . ? C41 Co C42 40.01(15) . . ? C41 Co C43 67.02(16) . . ? C42 Co C43 39.36(15) . . ? C41 Co C44 67.17(16) . . ? C42 Co C44 66.67(15) . . ? C43 Co C44 40.03(16) . . ? C41 Co C45 39.74(15) . . ? C42 Co C45 66.46(16) . . ? C43 Co C45 66.70(16) . . ? C44 Co C45 39.78(16) . . ? C41 Co P1 102.08(12) . . ? C42 Co P1 88.74(11) . . ? C43 Co P1 112.86(12) . . ? C44 Co P1 152.63(12) . . ? C45 Co P1 140.84(12) . . ? C41 Co P2 162.23(11) . . ? C42 Co P2 128.95(12) . . ? C43 Co P2 96.43(12) . . ? C44 Co P2 96.16(12) . . ? C45 Co P2 129.04(12) . . ? P1 Co P2 90.08(4) . . ? C41 Co P3 102.90(11) . . ? C42 Co P3 140.98(12) . . ? C43 Co P3 156.82(12) . . ? C44 Co P3 117.23(12) . . ? C45 Co P3 92.00(12) . . ? P1 Co P3 89.29(4) . . ? P2 Co P3 90.01(4) . . ? O11 P1 O13 107.63(14) . . ? O11 P1 O12 109.78(14) . . ? O13 P1 O12 102.06(15) . . ? O11 P1 Co 118.91(10) . . ? O13 P1 Co 109.76(11) . . ? O12 P1 Co 107.40(10) . . ? O21 P2 O23 110.11(14) . . ? O21 P2 O22 106.76(14) . . ? O23 P2 O22 98.92(13) . . ? O21 P2 Co 117.65(10) . . ? O23 P2 Co 108.33(10) . . ? O22 P2 Co 113.45(10) . . ? O31 P3 O33 110.66(13) . . ? O31 P3 O32 106.92(14) . . ? O33 P3 O32 98.63(14) . . ? O31 P3 Co 117.82(10) . . ? O33 P3 Co 106.78(10) . . ? O32 P3 Co 114.35(10) . . ? P1 O11 Re 129.73(14) . . ? C11 O12 P1 120.7(2) . . ? C13 O13 P1 126.0(3) . . ? P2 O21 Re 130.94(14) . . ? C21 O22 P2 124.0(2) . . ? C23 O23 P2 118.5(2) . . ? P3 O31 Re 130.21(14) . . ? C31 O32 P3 124.8(2) . . ? C33 O33 P3 118.7(2) . . ? O1 C1 Re 177.7(3) . . ? O2 C2 Re 178.7(3) . . ? O3 C3 Re 179.3(4) . . ? C42 C43 C44 108.2(4) . . ? C42 C43 Co 70.3(2) . . ? C44 C43 Co 70.2(2) . . ? C45 C44 C43 107.3(4) . . ? C45 C44 Co 70.2(2) . . ? C43 C44 Co 69.7(2) . . ? C41 C45 C44 108.5(4) . . ? C41 C45 Co 69.6(2) . . ? C44 C45 Co 70.0(2) . . ? C45 C41 C42 107.3(4) . . ? C45 C41 Co 70.6(2) . . ? C42 C41 Co 70.1(2) . . ? C43 C42 C41 108.8(4) . . ? C43 C42 Co 70.4(2) . . ? C41 C42 Co 69.8(2) . . ? O12 C11 C12 112.9(4) . . ? O13 C13 C14 110.9(4) . . ? O22 C21 C22 109.9(3) . . ? C24 C23 O23 116.5(4) . . ? O32 C31 C32 109.9(3) . . ? O33 C33 C34 108.7(3) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 32.48 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.943 _refine_diff_density_min -0.952 _refine_diff_density_rms 0.174 # Attachment '- natos10.cif' data_natos10 _database_code_depnum_ccdc_archive 'CCDC 794064' #TrackingRef '- natos10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H36 B N6 Na O6' _chemical_formula_weight 610.45 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' 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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.7551(9) _cell_length_b 14.9081(10) _cell_length_c 15.2676(10) _cell_angle_alpha 82.3230(10) _cell_angle_beta 89.7710(10) _cell_angle_gamma 81.6210(10) _cell_volume 3069.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9829 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 31.92 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 0.105 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.9525 _exptl_absorpt_correction_T_max 0.9683 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 46277 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 29.57 _reflns_number_total 17158 _reflns_number_gt 10948 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+0.3764P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17158 _refine_ls_number_parameters 811 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0832 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1341 _refine_ls_wR_factor_gt 0.1134 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Na1 Na 0.11747(4) 0.96794(4) 0.26416(4) 0.03708(15) Uani 1 1 d . . . B1 B 0.34366(12) 0.98271(10) 0.41134(10) 0.0263(3) Uani 1 1 d . . . H1 H 0.4137(10) 0.9824(9) 0.4475(9) 0.021(3) Uiso 1 1 d . . . O1 O 0.19040(9) 0.98852(8) 0.11010(7) 0.0427(3) Uani 1 1 d . . . O2 O 0.02227(8) 0.91579(7) 0.13867(7) 0.0416(3) Uani 1 1 d . . . O3 O -0.04795(8) 0.92686(9) 0.30231(8) 0.0497(3) Uani 1 1 d . . . O11 O 0.25845(7) 0.86125(7) 0.28983(7) 0.0351(2) Uani 1 1 d . . . O21 O 0.12488(8) 0.96118(9) 0.42310(8) 0.0454(3) Uani 1 1 d . . . O31 O 0.19184(8) 1.09991(7) 0.27380(7) 0.0369(2) Uani 1 1 d . . . N11 N 0.37228(8) 0.95631(7) 0.31923(7) 0.0260(2) Uani 1 1 d . . . N12 N 0.39329(9) 0.88211(8) 0.20154(8) 0.0334(3) Uani 1 1 d . . . N21 N 0.28916(9) 0.91164(8) 0.46608(8) 0.0307(3) Uani 1 1 d . . . N22 N 0.17313(12) 0.83943(10) 0.53306(9) 0.0490(4) Uani 1 1 d . . . N31 N 0.28391(8) 1.07966(8) 0.40620(7) 0.0272(2) Uani 1 1 d . . . N32 N 0.18025(9) 1.20878(8) 0.36983(8) 0.0326(3) Uani 1 1 d . . . C11 C 0.37770(13) 0.82091(12) 0.13861(11) 0.0449(4) Uani 1 1 d . . . H11A H 0.4366 0.7756 0.1366 0.067 Uiso 1 1 calc R . . H11B H 0.3644 0.8561 0.0799 0.067 Uiso 1 1 calc R . . H11C H 0.3215 0.7896 0.1567 0.067 Uiso 1 1 calc R . . C12 C 0.33297(10) 0.89664(9) 0.27287(9) 0.0290(3) Uani 1 1 d . . . C13 C 0.46747(11) 0.93563(10) 0.20017(10) 0.0311(3) Uani 1 1 d . . . C14 C 0.45403(10) 0.98229(9) 0.27404(9) 0.0266(3) Uani 1 1 d . . . C15 C 0.51630(11) 1.04290(10) 0.29103(10) 0.0319(3) Uani 1 1 d . . . H15A H 0.5069 1.0755 0.3405 0.038 Uiso 1 1 calc R . . C16 C 0.59322(12) 1.05448(11) 0.23316(11) 0.0411(4) Uani 1 1 d . . . H16A H 0.6377 1.0951 0.2439 0.049 Uiso 1 1 calc R . . C17 C 0.60634(13) 1.00819(13) 0.16033(12) 0.0470(4) Uani 1 1 d . . . H17A H 0.6596 1.0176 0.1221 0.056 Uiso 1 1 calc R . . C18 C 0.54289(12) 0.94798(12) 0.14196(11) 0.0420(4) Uani 1 1 d . . . H18A H 0.5512 0.9168 0.0915 0.050 Uiso 1 1 calc R . . C21 C 0.07592(17) 0.81812(17) 0.55693(14) 0.0707(7) Uani 1 1 d . . . H21A H 0.0730 0.7537 0.5517 0.106 Uiso 1 1 calc R . . H21B H 0.0266 0.8572 0.5172 0.106 Uiso 1 1 calc R . . H21C H 0.0625 0.8291 0.6180 0.106 Uiso 1 1 calc R . . C22 C 0.18963(12) 0.91053(11) 0.46817(10) 0.0379(4) Uani 1 1 d . . . C23 C 0.26176(15) 0.79541(11) 0.57000(11) 0.0454(4) Uani 1 1 d . . . C24 C 0.33490(12) 0.83970(10) 0.52733(9) 0.0346(3) Uani 1 1 d . . . C25 C 0.43276(14) 0.80925(10) 0.54731(10) 0.0410(4) Uani 1 1 d . . . H25A H 0.4829 0.8386 0.5179 0.049 Uiso 1 1 calc R . . C26 C 0.45563(18) 0.73372(12) 0.61232(12) 0.0574(5) Uani 1 1 d . . . H26A H 0.5226 0.7110 0.6267 0.069 Uiso 1 1 calc R . . C27 C 0.3834(2) 0.69152(13) 0.65591(13) 0.0694(7) Uani 1 1 d . . . H27A H 0.4015 0.6412 0.7007 0.083 Uiso 1 1 calc R . . C28 C 0.2849(2) 0.72095(13) 0.63585(12) 0.0657(6) Uani 1 1 d . . . H28A H 0.2351 0.6916 0.6658 0.079 Uiso 1 1 calc R . . C31 C 0.11615(12) 1.28069(11) 0.31650(11) 0.0419(4) Uani 1 1 d . . . H31A H 0.0651 1.3083 0.3537 0.063 Uiso 1 1 calc R . . H31B H 0.0853 1.2550 0.2697 0.063 Uiso 1 1 calc R . . H31C H 0.1545 1.3275 0.2899 0.063 Uiso 1 1 calc R . . C32 C 0.21710(10) 1.12511(9) 0.34290(9) 0.0287(3) Uani 1 1 d . . . C33 C 0.22044(11) 1.21409(10) 0.45156(10) 0.0306(3) Uani 1 1 d . . . C34 C 0.28579(10) 1.13319(9) 0.47418(9) 0.0270(3) Uani 1 1 d . . . C35 C 0.33657(11) 1.11725(11) 0.55415(10) 0.0334(3) Uani 1 1 d . . . H35A H 0.3812 1.0626 0.5700 0.040 Uiso 1 1 calc R . . C36 C 0.32023(12) 1.18378(12) 0.61076(11) 0.0418(4) Uani 1 1 d . . . H36A H 0.3549 1.1745 0.6657 0.050 Uiso 1 1 calc R . . C37 C 0.25416(13) 1.26342(12) 0.58840(11) 0.0448(4) Uani 1 1 d . . . H37A H 0.2435 1.3072 0.6286 0.054 Uiso 1 1 calc R . . C38 C 0.20336(12) 1.27985(11) 0.50787(11) 0.0406(4) Uani 1 1 d . . . H38A H 0.1585 1.3344 0.4921 0.049 Uiso 1 1 calc R . . C71 C -0.10590(15) 0.96352(17) 0.36977(14) 0.0670(6) Uani 1 1 d . . . H41A H -0.1395 0.9158 0.4018 0.101 Uiso 1 1 calc R . . H41B H -0.1547 1.0143 0.3432 0.101 Uiso 1 1 calc R . . H41C H -0.0635 0.9858 0.4109 0.101 Uiso 1 1 calc R . . C72 C -0.10599(13) 0.89774(15) 0.23812(13) 0.0558(5) Uani 1 1 d . . . H42A H -0.1489 0.9509 0.2060 0.067 Uiso 1 1 calc R . . H42B H -0.1481 0.8544 0.2671 0.067 Uiso 1 1 calc R . . C73 C -0.03817(14) 0.85195(13) 0.17506(12) 0.0510(5) Uani 1 1 d . . . H43A H 0.0024 0.7969 0.2065 0.061 Uiso 1 1 calc R . . H43B H -0.0764 0.8330 0.1277 0.061 Uiso 1 1 calc R . . C74 C 0.09273(13) 0.87932(12) 0.07916(12) 0.0460(4) Uani 1 1 d . . . H44A H 0.0595 0.8550 0.0319 0.055 Uiso 1 1 calc R . . H44B H 0.1397 0.8290 0.1110 0.055 Uiso 1 1 calc R . . C75 C 0.14536(13) 0.95551(13) 0.04047(11) 0.0462(4) Uani 1 1 d . . . H45A H 0.1957 0.9332 -0.0012 0.055 Uiso 1 1 calc R . . H45B H 0.0984 1.0052 0.0077 0.055 Uiso 1 1 calc R . . C76 C 0.24415(15) 1.06005(13) 0.07864(13) 0.0527(5) Uani 1 1 d . . . H46A H 0.2978 1.0367 0.0416 0.079 Uiso 1 1 calc R . . H46B H 0.2714 1.0833 0.1289 0.079 Uiso 1 1 calc R . . H46C H 0.2004 1.1096 0.0437 0.079 Uiso 1 1 calc R . . Na2 Na 0.37025(4) 0.56236(4) 0.22056(4) 0.03585(14) Uani 1 1 d . . . B2 B 0.14430(12) 0.53571(11) 0.08592(11) 0.0277(3) Uani 1 1 d . . . H2 H 0.0758(11) 0.5260(10) 0.0519(9) 0.026(4) Uiso 1 1 d . . . O4 O 0.33485(10) 0.54633(9) 0.38061(8) 0.0543(3) Uani 1 1 d . . . O5 O 0.46866(9) 0.64734(8) 0.30127(8) 0.0491(3) Uani 1 1 d . . . O6 O 0.54551(8) 0.51906(8) 0.19849(7) 0.0444(3) Uani 1 1 d . . . O41 O 0.29831(8) 0.42951(7) 0.22777(7) 0.0383(3) Uani 1 1 d . . . O51 O 0.35503(7) 0.58251(8) 0.06676(7) 0.0373(2) Uani 1 1 d . . . O61 O 0.22134(8) 0.66395(7) 0.20480(7) 0.0393(3) Uani 1 1 d . . . N41 N 0.21563(8) 0.44399(8) 0.09135(8) 0.0283(2) Uani 1 1 d . . . N42 N 0.32698(9) 0.32104(8) 0.13170(8) 0.0345(3) Uani 1 1 d . . . N51 N 0.18738(8) 0.61303(8) 0.02855(7) 0.0277(2) Uani 1 1 d . . . N52 N 0.29022(9) 0.69960(9) -0.04151(8) 0.0356(3) Uani 1 1 d . . . N61 N 0.11522(8) 0.56072(8) 0.17844(8) 0.0285(3) Uani 1 1 d . . . N62 N 0.09832(10) 0.62712(9) 0.30122(9) 0.0394(3) Uani 1 1 d . . . C41 C 0.39017(13) 0.25244(12) 0.18990(12) 0.0469(4) Uani 1 1 d . . . H71A H 0.4412 0.2210 0.1552 0.070 Uiso 1 1 calc R . . H71B H 0.3511 0.2079 0.2199 0.070 Uiso 1 1 calc R . . H71C H 0.4210 0.2819 0.2339 0.070 Uiso 1 1 calc R . . C42 C 0.28095(11) 0.40245(10) 0.15722(10) 0.0309(3) Uani 1 1 d . . . C43 C 0.29390(11) 0.31298(10) 0.04809(10) 0.0313(3) Uani 1 1 d . . . C44 C 0.22387(10) 0.39018(9) 0.02312(9) 0.0274(3) Uani 1 1 d . . . C45 C 0.17684(11) 0.40244(10) -0.05832(10) 0.0329(3) Uani 1 1 d . . . H75A H 0.1297 0.4549 -0.0761 0.040 Uiso 1 1 calc R . . C46 C 0.20070(12) 0.33562(11) -0.11364(11) 0.0399(4) Uani 1 1 d . . . H76A H 0.1682 0.3421 -0.1694 0.048 Uiso 1 1 calc R . . C47 C 0.27100(13) 0.25973(11) -0.08899(11) 0.0436(4) Uani 1 1 d . . . H77A H 0.2863 0.2155 -0.1283 0.052 Uiso 1 1 calc R . . C48 C 0.31933(12) 0.24760(10) -0.00746(11) 0.0404(4) Uani 1 1 d . . . H78A H 0.3681 0.1962 0.0094 0.048 Uiso 1 1 calc R . . C51 C 0.38114(13) 0.73105(13) -0.07020(11) 0.0472(4) Uani 1 1 d . . . H51A H 0.3766 0.7965 -0.0659 0.071 Uiso 1 1 calc R . . H51B H 0.3930 0.7208 -0.1316 0.071 Uiso 1 1 calc R . . H51C H 0.4355 0.6972 -0.0325 0.071 Uiso 1 1 calc R . . C52 C 0.28401(11) 0.62628(10) 0.02357(9) 0.0307(3) Uani 1 1 d . . . C53 C 0.19752(11) 0.73340(10) -0.07676(10) 0.0335(3) Uani 1 1 d . . . C54 C 0.13285(11) 0.67993(9) -0.03190(9) 0.0286(3) Uani 1 1 d . . . C55 C 0.03281(11) 0.69971(10) -0.04949(10) 0.0350(3) Uani 1 1 d . . . H55A H -0.0122 0.6647 -0.0186 0.042 Uiso 1 1 calc R . . C56 C 0.00064(13) 0.77321(12) -0.11446(11) 0.0445(4) Uani 1 1 d . . . H56A H -0.0677 0.7884 -0.1278 0.053 Uiso 1 1 calc R . . C57 C 0.06570(15) 0.82464(12) -0.16000(12) 0.0503(5) Uani 1 1 d . . . H57A H 0.0414 0.8735 -0.2045 0.060 Uiso 1 1 calc R . . C58 C 0.16544(14) 0.80575(12) -0.14153(11) 0.0456(4) Uani 1 1 d . . . H58A H 0.2103 0.8411 -0.1721 0.055 Uiso 1 1 calc R . . C61 C 0.11425(15) 0.68715(13) 0.36557(12) 0.0547(5) Uani 1 1 d . . . H61A H 0.1656 0.7236 0.3447 0.082 Uiso 1 1 calc R . . H61B H 0.1348 0.6504 0.4223 0.082 Uiso 1 1 calc R . . H61C H 0.0531 0.7280 0.3731 0.082 Uiso 1 1 calc R . . C62 C 0.15265(11) 0.62149(10) 0.22495(10) 0.0321(3) Uani 1 1 d . . . C63 C 0.02907(11) 0.56813(11) 0.30453(10) 0.0370(3) Uani 1 1 d . . . C64 C 0.04002(10) 0.52656(9) 0.22730(9) 0.0292(3) Uani 1 1 d . . . C65 C -0.01821(11) 0.46227(10) 0.21093(11) 0.0354(3) Uani 1 1 d . . . H65A H -0.0099 0.4327 0.1595 0.042 Uiso 1 1 calc R . . C66 C -0.08953(13) 0.44248(13) 0.27269(13) 0.0499(5) Uani 1 1 d . . . H66A H -0.1316 0.3997 0.2623 0.060 Uiso 1 1 calc R . . C67 C -0.10048(14) 0.48351(15) 0.34830(14) 0.0592(5) Uani 1 1 d . . . H67A H -0.1499 0.4685 0.3890 0.071 Uiso 1 1 calc R . . C68 C -0.04038(14) 0.54679(14) 0.36650(12) 0.0535(5) Uani 1 1 d . . . H68A H -0.0470 0.5741 0.4194 0.064 Uiso 1 1 calc R . . C81 C 0.58141(17) 0.50118(17) 0.11448(13) 0.0722(7) Uani 1 1 d . . . H81A H 0.6467 0.4643 0.1216 0.108 Uiso 1 1 calc R . . H81B H 0.5859 0.5592 0.0771 0.108 Uiso 1 1 calc R . . H81C H 0.5365 0.4677 0.0867 0.108 Uiso 1 1 calc R . . C82 C 0.60699(14) 0.56983(15) 0.24010(15) 0.0624(6) Uani 1 1 d . . . H82A H 0.6146 0.6270 0.2012 0.075 Uiso 1 1 calc R . . H82B H 0.6729 0.5335 0.2522 0.075 Uiso 1 1 calc R . . C83 C 0.56050(14) 0.59145(16) 0.32400(15) 0.0635(6) Uani 1 1 d . . . H83A H 0.5502 0.5345 0.3620 0.076 Uiso 1 1 calc R . . H83B H 0.6029 0.6245 0.3565 0.076 Uiso 1 1 calc R . . C84 C 0.41608(17) 0.67508(13) 0.37616(13) 0.0597(5) Uani 1 1 d . . . H84A H 0.3583 0.7207 0.3555 0.072 Uiso 1 1 calc R . . H84B H 0.4590 0.7052 0.4113 0.072 Uiso 1 1 calc R . . C85 C 0.38199(16) 0.59719(14) 0.43423(12) 0.0577(5) Uani 1 1 d . . . H85A H 0.4388 0.5579 0.4659 0.069 Uiso 1 1 calc R . . H85C H 0.3358 0.6207 0.4786 0.069 Uiso 1 1 calc R . . C86 C 0.30037(19) 0.46957(15) 0.42850(14) 0.0728(7) Uani 1 1 d . . . H86D H 0.2546 0.4899 0.4736 0.109 Uiso 1 1 calc R . . H86A H 0.3561 0.4275 0.4570 0.109 Uiso 1 1 calc R . . H86B H 0.2666 0.4382 0.3880 0.109 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 Na1 0.0335(3) 0.0393(3) 0.0404(3) -0.0101(3) 0.0003(3) -0.0079(3) B1 0.0286(8) 0.0240(7) 0.0260(8) -0.0016(6) 0.0016(6) -0.0043(6) O1 0.0544(7) 0.0432(6) 0.0339(6) -0.0054(5) 0.0011(5) -0.0180(5) O2 0.0455(6) 0.0377(6) 0.0451(7) -0.0107(5) 0.0051(5) -0.0129(5) O3 0.0366(6) 0.0708(9) 0.0467(7) -0.0170(6) 0.0070(5) -0.0162(6) O11 0.0350(6) 0.0304(5) 0.0428(6) -0.0081(5) 0.0032(5) -0.0117(4) O21 0.0329(6) 0.0614(8) 0.0438(7) -0.0090(6) 0.0058(5) -0.0112(6) O31 0.0458(6) 0.0354(6) 0.0300(5) -0.0058(4) -0.0065(5) -0.0058(5) N11 0.0277(6) 0.0229(5) 0.0282(6) -0.0037(4) 0.0030(5) -0.0058(4) N12 0.0366(7) 0.0311(6) 0.0349(7) -0.0127(5) 0.0036(5) -0.0053(5) N21 0.0353(7) 0.0292(6) 0.0278(6) -0.0013(5) 0.0043(5) -0.0078(5) N22 0.0606(10) 0.0519(9) 0.0411(8) -0.0056(7) 0.0186(7) -0.0313(8) N31 0.0308(6) 0.0245(6) 0.0262(6) -0.0042(5) 0.0000(5) -0.0023(5) N32 0.0370(7) 0.0258(6) 0.0327(7) -0.0025(5) -0.0045(5) 0.0018(5) C11 0.0523(10) 0.0410(9) 0.0455(10) -0.0216(8) 0.0006(8) -0.0061(8) C12 0.0311(7) 0.0224(7) 0.0329(7) -0.0043(6) 0.0001(6) -0.0018(6) C13 0.0318(7) 0.0282(7) 0.0323(8) -0.0039(6) 0.0022(6) -0.0011(6) C14 0.0278(7) 0.0226(6) 0.0276(7) 0.0007(5) 0.0021(5) -0.0013(5) C15 0.0342(8) 0.0280(7) 0.0327(8) -0.0004(6) 0.0001(6) -0.0053(6) C16 0.0359(8) 0.0409(9) 0.0465(10) 0.0036(7) 0.0022(7) -0.0144(7) C17 0.0390(9) 0.0550(11) 0.0456(10) 0.0017(8) 0.0149(7) -0.0102(8) C18 0.0428(9) 0.0460(9) 0.0370(9) -0.0091(7) 0.0120(7) -0.0027(7) C21 0.0781(15) 0.0869(16) 0.0626(13) -0.0214(12) 0.0335(11) -0.0538(13) C22 0.0427(9) 0.0428(9) 0.0324(8) -0.0095(7) 0.0102(7) -0.0162(7) C23 0.0740(13) 0.0353(9) 0.0310(8) -0.0051(7) 0.0095(8) -0.0217(8) C24 0.0577(10) 0.0239(7) 0.0234(7) -0.0037(5) 0.0014(7) -0.0099(7) C25 0.0626(11) 0.0278(8) 0.0318(8) -0.0058(6) -0.0089(7) -0.0017(7) C26 0.0959(16) 0.0319(9) 0.0413(10) -0.0044(8) -0.0211(10) 0.0013(10) C27 0.133(2) 0.0352(10) 0.0374(11) 0.0047(8) -0.0156(12) -0.0127(12) C28 0.123(2) 0.0429(11) 0.0374(10) 0.0016(8) 0.0112(11) -0.0385(12) C31 0.0427(9) 0.0314(8) 0.0468(10) 0.0030(7) -0.0058(7) 0.0036(7) C32 0.0316(7) 0.0251(7) 0.0291(7) -0.0019(6) 0.0016(6) -0.0047(6) C33 0.0327(7) 0.0269(7) 0.0329(8) -0.0047(6) 0.0013(6) -0.0054(6) C34 0.0273(7) 0.0272(7) 0.0275(7) -0.0048(5) 0.0047(5) -0.0066(5) C35 0.0330(8) 0.0361(8) 0.0311(8) -0.0047(6) -0.0001(6) -0.0048(6) C36 0.0454(9) 0.0511(10) 0.0334(8) -0.0145(7) -0.0002(7) -0.0137(8) C37 0.0530(10) 0.0429(9) 0.0438(10) -0.0206(8) 0.0059(8) -0.0112(8) C38 0.0451(9) 0.0301(8) 0.0479(10) -0.0131(7) 0.0063(7) -0.0029(7) C71 0.0472(11) 0.0952(17) 0.0654(14) -0.0277(12) 0.0195(10) -0.0177(11) C72 0.0389(10) 0.0751(14) 0.0587(12) -0.0086(10) -0.0007(9) -0.0264(9) C73 0.0588(11) 0.0501(11) 0.0504(11) -0.0085(8) -0.0009(9) -0.0277(9) C74 0.0473(10) 0.0474(10) 0.0477(10) -0.0211(8) 0.0005(8) -0.0082(8) C75 0.0483(10) 0.0575(11) 0.0347(9) -0.0107(8) -0.0002(7) -0.0107(8) C76 0.0643(12) 0.0464(10) 0.0517(11) -0.0084(8) 0.0159(9) -0.0214(9) Na2 0.0376(3) 0.0384(3) 0.0332(3) -0.0056(3) -0.0031(3) -0.0105(3) B2 0.0297(8) 0.0250(7) 0.0284(8) -0.0031(6) 0.0008(6) -0.0044(6) O4 0.0825(10) 0.0473(7) 0.0332(6) -0.0044(5) 0.0004(6) -0.0115(7) O5 0.0558(8) 0.0366(6) 0.0567(8) -0.0132(6) -0.0107(6) -0.0058(6) O6 0.0424(6) 0.0502(7) 0.0402(6) -0.0059(5) 0.0022(5) -0.0051(5) O41 0.0470(6) 0.0368(6) 0.0321(6) -0.0036(5) -0.0079(5) -0.0105(5) O51 0.0298(5) 0.0472(6) 0.0333(6) -0.0004(5) -0.0010(4) -0.0045(5) O61 0.0413(6) 0.0354(6) 0.0449(6) -0.0114(5) 0.0003(5) -0.0131(5) N41 0.0319(6) 0.0256(6) 0.0275(6) -0.0046(5) -0.0009(5) -0.0040(5) N42 0.0369(7) 0.0269(6) 0.0375(7) 0.0006(5) -0.0052(5) -0.0011(5) N51 0.0283(6) 0.0268(6) 0.0277(6) -0.0015(5) 0.0002(5) -0.0046(5) N52 0.0348(7) 0.0385(7) 0.0328(7) 0.0023(5) 0.0044(5) -0.0104(6) N61 0.0304(6) 0.0255(6) 0.0299(6) -0.0046(5) 0.0035(5) -0.0050(5) N62 0.0461(8) 0.0377(7) 0.0356(7) -0.0136(6) 0.0046(6) -0.0022(6) C41 0.0432(9) 0.0403(9) 0.0507(10) 0.0080(8) -0.0086(8) 0.0026(7) C42 0.0327(7) 0.0283(7) 0.0322(8) -0.0007(6) -0.0014(6) -0.0092(6) C43 0.0315(7) 0.0255(7) 0.0365(8) -0.0018(6) 0.0013(6) -0.0055(6) C44 0.0288(7) 0.0239(7) 0.0307(7) -0.0049(5) 0.0031(6) -0.0067(5) C45 0.0322(8) 0.0344(8) 0.0323(8) -0.0058(6) -0.0009(6) -0.0044(6) C46 0.0469(9) 0.0426(9) 0.0339(8) -0.0107(7) 0.0026(7) -0.0132(7) C47 0.0547(10) 0.0349(8) 0.0448(10) -0.0155(7) 0.0105(8) -0.0096(8) C48 0.0450(9) 0.0244(7) 0.0515(10) -0.0070(7) 0.0091(8) -0.0026(6) C51 0.0465(10) 0.0553(11) 0.0430(10) -0.0019(8) 0.0120(8) -0.0226(8) C52 0.0335(8) 0.0334(7) 0.0262(7) -0.0054(6) 0.0041(6) -0.0072(6) C53 0.0417(8) 0.0309(8) 0.0286(7) -0.0050(6) 0.0029(6) -0.0062(6) C54 0.0354(8) 0.0248(7) 0.0265(7) -0.0075(5) -0.0011(6) -0.0035(6) C55 0.0379(8) 0.0315(8) 0.0365(8) -0.0109(6) -0.0035(6) -0.0024(6) C56 0.0470(10) 0.0399(9) 0.0442(10) -0.0100(7) -0.0142(8) 0.0060(7) C57 0.0659(12) 0.0384(9) 0.0400(9) 0.0035(7) -0.0104(8) 0.0062(8) C58 0.0604(11) 0.0376(9) 0.0361(9) 0.0040(7) 0.0022(8) -0.0061(8) C61 0.0675(12) 0.0541(11) 0.0441(10) -0.0249(9) -0.0017(9) 0.0024(9) C62 0.0348(8) 0.0286(7) 0.0328(8) -0.0075(6) 0.0000(6) -0.0013(6) C63 0.0375(8) 0.0356(8) 0.0345(8) -0.0020(6) 0.0054(6) 0.0031(7) C64 0.0276(7) 0.0267(7) 0.0306(7) 0.0015(6) 0.0026(6) 0.0009(5) C65 0.0327(8) 0.0291(7) 0.0413(9) 0.0063(6) -0.0008(6) -0.0043(6) C66 0.0369(9) 0.0467(10) 0.0613(12) 0.0128(9) 0.0061(8) -0.0092(8) C67 0.0457(11) 0.0671(13) 0.0581(12) 0.0117(10) 0.0219(9) -0.0047(9) C68 0.0530(11) 0.0607(12) 0.0415(10) -0.0029(9) 0.0172(8) 0.0048(9) C81 0.0666(14) 0.0898(17) 0.0518(12) -0.0115(12) 0.0105(10) 0.0180(12) C82 0.0386(10) 0.0698(14) 0.0817(15) -0.0094(12) 0.0019(10) -0.0185(9) C83 0.0498(11) 0.0718(14) 0.0735(14) -0.0235(11) -0.0209(10) -0.0109(10) C84 0.0826(14) 0.0399(10) 0.0584(12) -0.0236(9) -0.0115(11) 0.0011(10) C85 0.0766(14) 0.0554(12) 0.0386(10) -0.0158(9) -0.0119(9) 0.0077(10) C86 0.1120(19) 0.0586(13) 0.0471(12) -0.0013(10) 0.0218(12) -0.0160(13) _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 Na1 O11 2.3205(12) . ? Na1 O31 2.3672(12) . ? Na1 O21 2.4171(13) . ? Na1 O3 2.4884(13) . ? Na1 O1 2.5517(13) . ? Na1 O2 2.5892(12) . ? Na1 C12 2.9969(15) . ? B1 H1 1.112(14) . ? B1 N21 1.5405(19) . ? B1 N11 1.5446(19) . ? B1 N31 1.5473(19) . ? O1 C75 1.4107(19) . ? O1 C76 1.416(2) . ? O2 C73 1.411(2) . ? O2 C74 1.425(2) . ? O3 C72 1.417(2) . ? O3 C71 1.418(2) . ? O11 C12 1.2309(17) . ? O21 C22 1.228(2) . ? O31 C32 1.2337(17) . ? N11 C12 1.3769(17) . ? N11 C14 1.3928(17) . ? N12 C13 1.3824(19) . ? N12 C12 1.3874(18) . ? N12 C11 1.4471(19) . ? N21 C22 1.372(2) . ? N21 C24 1.4002(19) . ? N22 C23 1.381(2) . ? N22 C22 1.394(2) . ? N22 C21 1.453(2) . ? N31 C32 1.3742(17) . ? N31 C34 1.3936(17) . ? N32 C33 1.3833(18) . ? N32 C32 1.3903(18) . ? N32 C31 1.4445(18) . ? C13 C18 1.380(2) . ? C13 C14 1.4002(19) . ? C14 C15 1.381(2) . ? C15 C16 1.391(2) . ? C16 C17 1.383(2) . ? C17 C18 1.394(2) . ? C23 C28 1.395(3) . ? C23 C24 1.395(2) . ? C24 C25 1.378(2) . ? C25 C26 1.397(2) . ? C26 C27 1.375(3) . ? C27 C28 1.384(3) . ? C33 C38 1.383(2) . ? C33 C34 1.399(2) . ? C34 C35 1.3842(19) . ? C35 C36 1.394(2) . ? C36 C37 1.390(2) . ? C37 C38 1.392(2) . ? C72 C73 1.499(3) . ? C74 C75 1.490(2) . ? Na2 O41 2.3293(12) . ? Na2 O51 2.3335(12) . ? Na2 O61 2.3558(13) . ? Na2 O5 2.4261(13) . ? Na2 O6 2.4372(13) . ? Na2 O4 2.4766(13) . ? Na2 C62 2.9975(16) . ? Na2 C42 3.0993(15) . ? B2 H2 1.115(14) . ? B2 N51 1.5402(19) . ? B2 N61 1.5450(19) . ? B2 N41 1.5553(19) . ? O4 C85 1.407(2) . ? O4 C86 1.414(2) . ? O5 C83 1.425(2) . ? O5 C84 1.426(2) . ? O6 C81 1.417(2) . ? O6 C82 1.418(2) . ? O41 C42 1.2354(17) . ? O51 C52 1.2328(17) . ? O61 C62 1.2280(18) . ? N41 C42 1.3714(18) . ? N41 C44 1.3918(17) . ? N42 C43 1.3829(19) . ? N42 C42 1.3879(19) . ? N42 C41 1.4475(19) . ? N51 C52 1.3722(18) . ? N51 C54 1.3967(17) . ? N52 C53 1.3839(19) . ? N52 C52 1.3877(19) . ? N52 C51 1.4447(19) . ? N61 C62 1.3788(18) . ? N61 C64 1.3898(18) . ? N62 C63 1.384(2) . ? N62 C62 1.3865(19) . ? N62 C61 1.452(2) . ? C43 C48 1.382(2) . ? C43 C44 1.4001(19) . ? C44 C45 1.3818(19) . ? C45 C46 1.393(2) . ? C46 C47 1.388(2) . ? C47 C48 1.391(2) . ? C53 C58 1.384(2) . ? C53 C54 1.397(2) . ? C54 C55 1.384(2) . ? C55 C56 1.397(2) . ? C56 C57 1.387(3) . ? C57 C58 1.382(3) . ? C63 C68 1.382(2) . ? C63 C64 1.401(2) . ? C64 C65 1.383(2) . ? C65 C66 1.393(2) . ? C66 C67 1.375(3) . ? C67 C68 1.396(3) . ? C82 C83 1.482(3) . ? C84 C85 1.495(3) . ? 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 O11 Na1 O31 97.26(4) . . ? O11 Na1 O21 82.26(4) . . ? O31 Na1 O21 80.72(4) . . ? O11 Na1 O3 121.42(5) . . ? O31 Na1 O3 133.41(5) . . ? O21 Na1 O3 80.05(4) . . ? O11 Na1 O1 81.37(4) . . ? O31 Na1 O1 80.51(4) . . ? O21 Na1 O1 153.23(4) . . ? O3 Na1 O1 126.67(4) . . ? O11 Na1 O2 105.65(4) . . ? O31 Na1 O2 132.86(4) . . ? O21 Na1 O2 142.07(4) . . ? O3 Na1 O2 64.00(4) . . ? O1 Na1 O2 63.46(4) . . ? O11 Na1 C12 22.49(4) . . ? O31 Na1 C12 76.40(4) . . ? O21 Na1 C12 87.19(4) . . ? O3 Na1 C12 143.78(5) . . ? O1 Na1 C12 69.93(4) . . ? O2 Na1 C12 114.42(4) . . ? H1 B1 N21 106.3(7) . . ? H1 B1 N11 106.3(7) . . ? N21 B1 N11 112.50(11) . . ? H1 B1 N31 108.1(7) . . ? N21 B1 N31 110.68(11) . . ? N11 B1 N31 112.51(11) . . ? C75 O1 C76 111.85(13) . . ? C75 O1 Na1 118.93(10) . . ? C76 O1 Na1 124.07(10) . . ? C73 O2 C74 112.85(13) . . ? C73 O2 Na1 109.67(10) . . ? C74 O2 Na1 107.65(9) . . ? C72 O3 C71 112.07(14) . . ? C72 O3 Na1 120.33(10) . . ? C71 O3 Na1 122.87(11) . . ? C12 O11 Na1 111.37(9) . . ? C22 O21 Na1 121.88(10) . . ? C32 O31 Na1 125.48(9) . . ? C12 N11 C14 108.13(11) . . ? C12 N11 B1 128.33(12) . . ? C14 N11 B1 123.08(11) . . ? C13 N12 C12 109.51(12) . . ? C13 N12 C11 126.54(13) . . ? C12 N12 C11 123.94(13) . . ? C22 N21 C24 108.61(13) . . ? C22 N21 B1 127.03(13) . . ? C24 N21 B1 124.23(12) . . ? C23 N22 C22 109.68(14) . . ? C23 N22 C21 126.78(16) . . ? C22 N22 C21 123.54(18) . . ? C32 N31 C34 108.36(11) . . ? C32 N31 B1 129.25(11) . . ? C34 N31 B1 122.20(11) . . ? C33 N32 C32 109.34(12) . . ? C33 N32 C31 126.14(13) . . ? C32 N32 C31 124.36(13) . . ? O11 C12 N11 127.69(13) . . ? O11 C12 N12 124.81(13) . . ? N11 C12 N12 107.50(12) . . ? O11 C12 Na1 46.14(7) . . ? N11 C12 Na1 103.68(8) . . ? N12 C12 Na1 126.29(9) . . ? C18 C13 N12 131.86(14) . . ? C18 C13 C14 121.70(14) . . ? N12 C13 C14 106.44(12) . . ? C15 C14 N11 130.91(13) . . ? C15 C14 C13 120.76(13) . . ? N11 C14 C13 108.33(12) . . ? C14 C15 C16 117.65(14) . . ? C17 C16 C15 121.42(15) . . ? C16 C17 C18 121.28(15) . . ? C13 C18 C17 117.18(15) . . ? O21 C22 N21 128.35(15) . . ? O21 C22 N22 124.64(15) . . ? N21 C22 N22 107.02(15) . . ? N22 C23 C28 132.03(19) . . ? N22 C23 C24 106.67(14) . . ? C28 C23 C24 121.3(2) . . ? C25 C24 C23 120.75(15) . . ? C25 C24 N21 131.25(14) . . ? C23 C24 N21 107.98(15) . . ? C24 C25 C26 117.71(18) . . ? C27 C26 C25 121.5(2) . . ? C26 C27 C28 121.31(18) . . ? C27 C28 C23 117.4(2) . . ? O31 C32 N31 128.64(13) . . ? O31 C32 N32 123.90(13) . . ? N31 C32 N32 107.46(12) . . ? C38 C33 N32 131.60(14) . . ? C38 C33 C34 121.73(14) . . ? N32 C33 C34 106.62(12) . . ? C35 C34 N31 131.42(13) . . ? C35 C34 C33 120.40(13) . . ? N31 C34 C33 108.15(12) . . ? C34 C35 C36 118.04(14) . . ? C37 C36 C35 121.25(15) . . ? C36 C37 C38 120.84(15) . . ? C33 C38 C37 117.72(15) . . ? O3 C72 C73 108.12(14) . . ? O2 C73 C72 107.33(15) . . ? O2 C74 C75 107.08(14) . . ? O1 C75 C74 108.24(13) . . ? O41 Na2 O51 89.94(4) . . ? O41 Na2 O61 95.65(4) . . ? O51 Na2 O61 81.13(4) . . ? O41 Na2 O5 144.46(5) . . ? O51 Na2 O5 123.65(5) . . ? O61 Na2 O5 100.41(4) . . ? O41 Na2 O6 107.06(5) . . ? O51 Na2 O6 86.12(4) . . ? O61 Na2 O6 153.91(5) . . ? O5 Na2 O6 68.21(4) . . ? O41 Na2 O4 82.64(4) . . ? O51 Na2 O4 163.68(5) . . ? O61 Na2 O4 85.15(5) . . ? O5 Na2 O4 67.52(5) . . ? O6 Na2 O4 109.93(5) . . ? O41 Na2 C62 73.75(4) . . ? O51 Na2 C62 87.29(4) . . ? O61 Na2 C62 22.72(4) . . ? O5 Na2 C62 115.13(5) . . ? O6 Na2 C62 173.36(5) . . ? O4 Na2 C62 76.70(5) . . ? O41 Na2 C42 20.71(4) . . ? O51 Na2 C42 69.34(4) . . ? O61 Na2 C42 94.17(4) . . ? O5 Na2 C42 161.70(5) . . ? O6 Na2 C42 102.50(4) . . ? O4 Na2 C42 103.11(5) . . ? C62 Na2 C42 75.87(4) . . ? H2 B2 N51 107.0(7) . . ? H2 B2 N61 107.3(7) . . ? N51 B2 N61 112.25(11) . . ? H2 B2 N41 107.2(7) . . ? N51 B2 N41 110.81(12) . . ? N61 B2 N41 112.02(12) . . ? C85 O4 C86 113.33(15) . . ? C85 O4 Na2 118.32(11) . . ? C86 O4 Na2 124.53(11) . . ? C83 O5 C84 113.21(15) . . ? C83 O5 Na2 108.22(10) . . ? C84 O5 Na2 109.70(11) . . ? C81 O6 C82 111.39(16) . . ? C81 O6 Na2 120.72(11) . . ? C82 O6 Na2 114.60(11) . . ? C42 O41 Na2 117.46(9) . . ? C52 O51 Na2 125.37(10) . . ? C62 O61 Na2 109.46(10) . . ? C42 N41 C44 107.98(11) . . ? C42 N41 B2 129.53(12) . . ? C44 N41 B2 122.46(11) . . ? C43 N42 C42 109.33(12) . . ? C43 N42 C41 126.84(13) . . ? C42 N42 C41 123.45(13) . . ? C52 N51 C54 108.15(12) . . ? C52 N51 B2 127.37(12) . . ? C54 N51 B2 124.40(12) . . ? C53 N52 C52 109.43(12) . . ? C53 N52 C51 126.23(13) . . ? C52 N52 C51 124.25(13) . . ? C62 N61 C64 108.19(12) . . ? C62 N61 B2 128.23(12) . . ? C64 N61 B2 123.50(12) . . ? C63 N62 C62 109.49(13) . . ? C63 N62 C61 127.08(14) . . ? C62 N62 C61 123.42(14) . . ? O41 C42 N41 128.27(14) . . ? O41 C42 N42 123.91(13) . . ? N41 C42 N42 107.83(12) . . ? O41 C42 Na2 41.83(7) . . ? N41 C42 Na2 104.30(9) . . ? N42 C42 Na2 130.09(10) . . ? C48 C43 N42 131.98(14) . . ? C48 C43 C44 121.73(14) . . ? N42 C43 C44 106.28(12) . . ? C45 C44 N41 131.09(13) . . ? C45 C44 C43 120.39(13) . . ? N41 C44 C43 108.52(12) . . ? C44 C45 C46 118.01(14) . . ? C47 C46 C45 121.37(15) . . ? C46 C47 C48 120.82(15) . . ? C43 C48 C47 117.65(15) . . ? O51 C52 N51 128.30(13) . . ? O51 C52 N52 124.07(13) . . ? N51 C52 N52 107.63(12) . . ? N52 C53 C58 131.43(15) . . ? N52 C53 C54 106.49(12) . . ? C58 C53 C54 122.07(15) . . ? C55 C54 N51 131.28(14) . . ? C55 C54 C53 120.43(14) . . ? N51 C54 C53 108.26(12) . . ? C54 C55 C56 117.30(15) . . ? C57 C56 C55 121.81(16) . . ? C58 C57 C56 120.89(15) . . ? C57 C58 C53 117.47(17) . . ? O61 C62 N61 127.84(14) . . ? O61 C62 N62 124.66(14) . . ? N61 C62 N62 107.50(13) . . ? O61 C62 Na2 47.82(8) . . ? N61 C62 Na2 103.15(9) . . ? N62 C62 Na2 124.94(10) . . ? C68 C63 N62 132.29(16) . . ? C68 C63 C64 121.31(16) . . ? N62 C63 C64 106.39(13) . . ? C65 C64 N61 130.73(14) . . ? C65 C64 C63 120.88(14) . . ? N61 C64 C63 108.38(13) . . ? C64 C65 C66 117.56(16) . . ? C67 C66 C65 121.52(18) . . ? C66 C67 C68 121.33(17) . . ? C63 C68 C67 117.36(18) . . ? O6 C82 C83 107.90(15) . . ? O5 C83 C82 106.98(17) . . ? O5 C84 C85 113.02(14) . . ? O4 C85 C84 108.20(14) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.57 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.282 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.043 # Attachment '- nattos10.cif' data_nattos10 _database_code_depnum_ccdc_archive 'CCDC 794065' #TrackingRef '- nattos10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H68 B2 N12 Na2 O6' _chemical_formula_weight 904.68 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' 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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.357(3) _cell_length_b 10.900(3) _cell_length_c 12.135(4) _cell_angle_alpha 104.306(5) _cell_angle_beta 92.511(5) _cell_angle_gamma 108.015(5) _cell_volume 1251.6(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2702 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 23.17 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.200 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 484 _exptl_absorpt_coefficient_mu 0.096 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9909 _exptl_absorpt_correction_T_max 0.9974 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15155 _diffrn_reflns_av_R_equivalents 0.0880 _diffrn_reflns_av_sigmaI/netI 0.1137 _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 -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 26.37 _reflns_number_total 5123 _reflns_number_gt 2434 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5123 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1517 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.0932 _refine_ls_wR_factor_gt 0.0784 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Na Na 0.65148(10) 0.58627(10) -0.01897(8) 0.0451(3) Uani 1 1 d . . . B B 0.4359(3) 0.3166(3) -0.2360(3) 0.0367(8) Uani 1 1 d . . . H1 H 0.4611(19) 0.3406(19) -0.1380(17) 0.029(6) Uiso 1 1 d . . . O1 O 0.22046(17) 0.20681(17) -0.09714(14) 0.0467(5) Uani 1 1 d . . . O2 O 0.71638(17) 0.49951(17) -0.18714(15) 0.0476(5) Uani 1 1 d . . . O3 O 0.42553(17) 0.57305(17) -0.08382(15) 0.0454(5) Uani 1 1 d . . . N11 N 0.3058(2) 0.1919(2) -0.27490(17) 0.0347(6) Uani 1 1 d . . . N12 N 0.0999(2) 0.0506(2) -0.26907(17) 0.0355(6) Uani 1 1 d . . . N21 N 0.5600(2) 0.2910(2) -0.29192(17) 0.0372(6) Uani 1 1 d . . . N22 N 0.7809(2) 0.3338(2) -0.31295(17) 0.0366(6) Uani 1 1 d . . . N31 N 0.41116(19) 0.4374(2) -0.26899(18) 0.0356(6) Uani 1 1 d . . . N32 N 0.3849(2) 0.6365(2) -0.24957(19) 0.0394(6) Uani 1 1 d . . . C11 C 0.2105(3) 0.1551(3) -0.2026(2) 0.0364(7) Uani 1 1 d . . . C12 C 0.2497(3) 0.1131(3) -0.3859(2) 0.0387(7) Uani 1 1 d . . . H12A H 0.2911 0.1208 -0.4533 0.046 Uiso 1 1 calc R . . C13 C 0.1272(3) 0.0242(3) -0.3822(2) 0.0376(7) Uani 1 1 d . . . H13A H 0.0698 -0.0442 -0.4455 0.045 Uiso 1 1 calc R . . C14 C -0.0219(3) -0.0230(2) -0.2234(2) 0.0352(7) Uani 1 1 d . . . C15 C -0.1228(3) -0.1296(3) -0.3227(2) 0.0532(9) Uani 1 1 d . . . H15A H -0.0776 -0.1907 -0.3638 0.080 Uiso 1 1 calc R . . H15B H -0.1533 -0.0860 -0.3754 0.080 Uiso 1 1 calc R . . H15C H -0.2020 -0.1804 -0.2925 0.080 Uiso 1 1 calc R . . C16 C -0.0914(2) 0.0750(3) -0.1617(2) 0.0455(8) Uani 1 1 d . . . H16A H -0.0247 0.1476 -0.1022 0.068 Uiso 1 1 calc R . . H16B H -0.1674 0.0274 -0.1264 0.068 Uiso 1 1 calc R . . H16C H -0.1265 0.1126 -0.2172 0.068 Uiso 1 1 calc R . . C17 C 0.0226(3) -0.0917(3) -0.1414(2) 0.0508(8) Uani 1 1 d . . . H17A H 0.0921 -0.0248 -0.0804 0.076 Uiso 1 1 calc R . . H17B H 0.0611 -0.1584 -0.1833 0.076 Uiso 1 1 calc R . . H17C H -0.0567 -0.1363 -0.1076 0.076 Uiso 1 1 calc R . . C21 C 0.6883(3) 0.3858(3) -0.2571(2) 0.0378(7) Uani 1 1 d . . . C22 C 0.5761(3) 0.1773(3) -0.3652(2) 0.0428(8) Uani 1 1 d . . . H22A H 0.5051 0.0943 -0.3981 0.051 Uiso 1 1 calc R . . C23 C 0.7093(3) 0.2048(3) -0.3818(2) 0.0405(7) Uani 1 1 d . . . H23A H 0.7472 0.1467 -0.4313 0.049 Uiso 1 1 calc R . . C24 C 0.9293(3) 0.4085(3) -0.3016(2) 0.0393(7) Uani 1 1 d . . . C25 C 0.9917(3) 0.4460(3) -0.1770(2) 0.0590(9) Uani 1 1 d . . . H25A H 0.9736 0.3647 -0.1510 0.088 Uiso 1 1 calc R . . H25B H 0.9509 0.5071 -0.1293 0.088 Uiso 1 1 calc R . . H25C H 1.0908 0.4904 -0.1703 0.088 Uiso 1 1 calc R . . C26 C 0.9989(3) 0.3208(3) -0.3771(2) 0.0562(9) Uani 1 1 d . . . H26A H 0.9884 0.2403 -0.3512 0.084 Uiso 1 1 calc R . . H26B H 1.0965 0.3712 -0.3717 0.084 Uiso 1 1 calc R . . H26C H 0.9565 0.2945 -0.4569 0.084 Uiso 1 1 calc R . . C27 C 0.9460(3) 0.5335(3) -0.3415(2) 0.0563(9) Uani 1 1 d . . . H27A H 0.9029 0.5908 -0.2920 0.084 Uiso 1 1 calc R . . H27B H 0.9021 0.5075 -0.4208 0.084 Uiso 1 1 calc R . . H27C H 1.0436 0.5828 -0.3375 0.084 Uiso 1 1 calc R . . C31 C 0.4083(2) 0.5505(3) -0.1905(3) 0.0378(7) Uani 1 1 d . . . C32 C 0.3936(3) 0.4550(3) -0.3786(2) 0.0441(8) Uani 1 1 d . . . H32A H 0.3879 0.3906 -0.4492 0.053 Uiso 1 1 calc R . . C33 C 0.3859(3) 0.5812(3) -0.3668(2) 0.0530(8) Uani 1 1 d . . . H33A H 0.3820 0.6229 -0.4265 0.064 Uiso 1 1 calc R . . C34 C 0.3992(3) 0.7793(3) -0.1941(3) 0.0501(8) Uani 1 1 d . . . C35 C 0.3527(3) 0.8388(3) -0.2832(3) 0.0768(11) Uani 1 1 d . . . H35A H 0.4167 0.8449 -0.3403 0.115 Uiso 1 1 calc R . . H35B H 0.3506 0.9285 -0.2455 0.115 Uiso 1 1 calc R . . H35C H 0.2609 0.7811 -0.3212 0.115 Uiso 1 1 calc R . . C36 C 0.3082(3) 0.7855(3) -0.0983(2) 0.0561(9) Uani 1 1 d . . . H36A H 0.3408 0.7525 -0.0381 0.084 Uiso 1 1 calc R . . H36B H 0.2136 0.7294 -0.1296 0.084 Uiso 1 1 calc R . . H36C H 0.3119 0.8784 -0.0659 0.084 Uiso 1 1 calc R . . C37 C 0.5474(3) 0.8569(3) -0.1446(3) 0.0994(14) Uani 1 1 d . . . H37A H 0.5724 0.8244 -0.0812 0.149 Uiso 1 1 calc R . . H37B H 0.5591 0.9526 -0.1162 0.149 Uiso 1 1 calc R . . H37C H 0.6064 0.8441 -0.2043 0.149 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 Na 0.0368(7) 0.0553(7) 0.0329(6) -0.0066(5) 0.0033(5) 0.0157(6) B 0.0322(19) 0.039(2) 0.033(2) -0.0007(16) 0.0076(15) 0.0113(16) O1 0.0403(11) 0.0556(13) 0.0271(11) -0.0066(10) 0.0056(9) 0.0058(10) O2 0.0422(12) 0.0392(12) 0.0461(12) -0.0125(10) 0.0122(9) 0.0100(9) O3 0.0468(12) 0.0522(13) 0.0306(12) -0.0061(10) -0.0020(9) 0.0221(10) N11 0.0306(13) 0.0371(14) 0.0273(13) -0.0034(11) 0.0027(11) 0.0082(11) N12 0.0302(13) 0.0397(14) 0.0279(13) 0.0015(11) 0.0034(11) 0.0054(11) N21 0.0294(13) 0.0362(14) 0.0345(14) -0.0051(11) 0.0054(11) 0.0063(11) N22 0.0290(13) 0.0314(14) 0.0422(14) -0.0008(11) 0.0103(11) 0.0076(11) N31 0.0296(13) 0.0378(14) 0.0331(14) -0.0021(12) 0.0061(10) 0.0113(11) N32 0.0377(14) 0.0341(15) 0.0405(15) 0.0031(13) 0.0073(11) 0.0088(12) C11 0.0319(17) 0.0395(18) 0.0317(17) 0.0002(14) 0.0039(14) 0.0106(14) C12 0.0392(18) 0.0445(18) 0.0261(16) -0.0002(14) 0.0057(13) 0.0124(15) C13 0.0368(17) 0.0393(17) 0.0284(17) -0.0016(13) 0.0022(13) 0.0095(14) C14 0.0323(16) 0.0375(17) 0.0308(16) 0.0054(14) 0.0027(13) 0.0079(14) C15 0.0455(19) 0.049(2) 0.049(2) 0.0052(16) 0.0064(16) 0.0006(16) C16 0.0357(17) 0.0492(19) 0.0504(19) 0.0114(15) 0.0079(14) 0.0137(15) C17 0.059(2) 0.047(2) 0.047(2) 0.0118(16) 0.0079(16) 0.0199(16) C21 0.0342(18) 0.0408(19) 0.0337(17) -0.0002(15) 0.0090(14) 0.0134(15) C22 0.0388(18) 0.0355(18) 0.0445(18) -0.0041(15) 0.0070(15) 0.0106(14) C23 0.0373(18) 0.0330(17) 0.0435(18) -0.0058(14) 0.0067(14) 0.0136(14) C24 0.0312(17) 0.0310(17) 0.053(2) 0.0079(15) 0.0137(14) 0.0082(14) C25 0.0448(19) 0.053(2) 0.067(2) 0.0062(17) -0.0048(17) 0.0083(16) C26 0.0411(18) 0.0430(19) 0.085(2) 0.0122(17) 0.0294(17) 0.0158(15) C27 0.054(2) 0.046(2) 0.067(2) 0.0119(17) 0.0245(17) 0.0156(16) C31 0.0262(16) 0.0426(19) 0.0384(19) 0.0012(16) 0.0037(14) 0.0104(14) C32 0.0515(19) 0.047(2) 0.0293(18) 0.0051(15) 0.0082(14) 0.0132(15) C33 0.071(2) 0.049(2) 0.041(2) 0.0137(16) 0.0185(16) 0.0200(17) C34 0.0438(19) 0.0346(19) 0.061(2) -0.0015(16) 0.0065(16) 0.0098(15) C35 0.102(3) 0.048(2) 0.088(3) 0.025(2) 0.031(2) 0.030(2) C36 0.056(2) 0.050(2) 0.061(2) 0.0008(16) 0.0066(17) 0.0266(16) C37 0.041(2) 0.062(2) 0.152(4) -0.024(2) 0.011(2) -0.0020(18) _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 Na O2 2.2518(19) . ? Na O1 2.291(2) 2_665 ? Na O3 2.347(2) 2_665 ? Na O3 2.385(2) . ? Na C31 3.059(3) . ? Na Na 3.240(2) 2_665 ? B H1 1.152(19) . ? B N11 1.543(3) . ? B N21 1.548(3) . ? B N31 1.556(4) . ? O1 C11 1.250(3) . ? O1 Na 2.291(2) 2_665 ? O2 C21 1.256(3) . ? O3 C31 1.251(3) . ? O3 Na 2.347(2) 2_665 ? N11 C11 1.382(3) . ? N11 C12 1.393(3) . ? N12 C11 1.385(3) . ? N12 C13 1.391(3) . ? N12 C14 1.482(3) . ? N21 C21 1.377(3) . ? N21 C22 1.396(3) . ? N22 C21 1.380(3) . ? N22 C23 1.395(3) . ? N22 C24 1.482(3) . ? N31 C31 1.368(3) . ? N31 C32 1.403(3) . ? N32 C31 1.382(3) . ? N32 C33 1.404(3) . ? N32 C34 1.493(3) . ? C12 C13 1.348(3) . ? C14 C17 1.519(3) . ? C14 C15 1.529(3) . ? C14 C16 1.531(3) . ? C22 C23 1.353(3) . ? C24 C27 1.519(3) . ? C24 C25 1.523(3) . ? C24 C26 1.524(3) . ? C32 C33 1.375(3) . ? C34 C37 1.515(4) . ? C34 C35 1.521(4) . ? C34 C36 1.530(3) . ? 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 Na O1 120.97(7) . 2_665 ? O2 Na O3 112.28(7) . 2_665 ? O1 Na O3 112.56(8) 2_665 2_665 ? O2 Na O3 99.95(7) . . ? O1 Na O3 113.37(7) 2_665 . ? O3 Na O3 93.58(7) 2_665 . ? O2 Na C31 78.08(7) . . ? O1 Na C31 121.53(8) 2_665 . ? O3 Na C31 106.74(8) 2_665 . ? O3 Na C31 22.49(6) . . ? O2 Na Na 113.69(6) . 2_665 ? O1 Na Na 124.74(6) 2_665 2_665 ? O3 Na Na 47.29(5) 2_665 2_665 ? O3 Na Na 46.30(5) . 2_665 ? C31 Na Na 61.86(6) . 2_665 ? H1 B N11 107.8(10) . . ? H1 B N21 108.3(10) . . ? N11 B N21 111.7(2) . . ? H1 B N31 110.4(10) . . ? N11 B N31 110.1(2) . . ? N21 B N31 108.5(2) . . ? C11 O1 Na 132.05(17) . 2_665 ? C21 O2 Na 136.67(17) . . ? C31 O3 Na 125.81(17) . 2_665 ? C31 O3 Na 110.66(16) . . ? Na O3 Na 86.41(7) 2_665 . ? C11 N11 C12 107.6(2) . . ? C11 N11 B 122.9(2) . . ? C12 N11 B 128.5(2) . . ? C11 N12 C13 108.3(2) . . ? C11 N12 C14 124.5(2) . . ? C13 N12 C14 127.1(2) . . ? C21 N21 C22 107.4(2) . . ? C21 N21 B 119.6(2) . . ? C22 N21 B 132.3(2) . . ? C21 N22 C23 108.1(2) . . ? C21 N22 C24 124.0(2) . . ? C23 N22 C24 127.9(2) . . ? C31 N31 C32 107.9(2) . . ? C31 N31 B 123.7(2) . . ? C32 N31 B 128.4(2) . . ? C31 N32 C33 108.4(2) . . ? C31 N32 C34 123.8(2) . . ? C33 N32 C34 125.5(3) . . ? O1 C11 N11 126.9(2) . . ? O1 C11 N12 125.9(2) . . ? N11 C11 N12 107.2(2) . . ? C13 C12 N11 109.0(2) . . ? C12 C13 N12 107.8(2) . . ? N12 C14 C17 109.1(2) . . ? N12 C14 C15 109.3(2) . . ? C17 C14 C15 108.9(2) . . ? N12 C14 C16 109.7(2) . . ? C17 C14 C16 110.5(2) . . ? C15 C14 C16 109.3(2) . . ? O2 C21 N21 126.3(2) . . ? O2 C21 N22 125.9(2) . . ? N21 C21 N22 107.9(2) . . ? C23 C22 N21 108.8(2) . . ? C22 C23 N22 107.7(2) . . ? N22 C24 C27 108.1(2) . . ? N22 C24 C25 109.5(2) . . ? C27 C24 C25 110.7(2) . . ? N22 C24 C26 109.4(2) . . ? C27 C24 C26 109.5(2) . . ? C25 C24 C26 109.7(2) . . ? O3 C31 N31 126.1(3) . . ? O3 C31 N32 125.8(2) . . ? N31 C31 N32 108.1(2) . . ? O3 C31 Na 46.85(13) . . ? N31 C31 Na 98.31(16) . . ? N32 C31 Na 130.60(17) . . ? C33 C32 N31 108.5(2) . . ? C32 C33 N32 106.7(3) . . ? N32 C34 C37 109.4(2) . . ? N32 C34 C35 109.0(2) . . ? C37 C34 C35 110.5(3) . . ? N32 C34 C36 109.4(2) . . ? C37 C34 C36 109.7(3) . . ? C35 C34 C36 108.8(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.224 _refine_diff_density_min -0.208 _refine_diff_density_rms 0.045 # Attachment '- reds10.cif' data_reds10 _database_code_depnum_ccdc_archive 'CCDC 794066' #TrackingRef '- reds10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H14 N2 O' _chemical_formula_weight 142.20 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 12.2165(13) _cell_length_b 6.1075(6) _cell_length_c 10.7386(11) _cell_angle_alpha 90.00 _cell_angle_beta 96.338(2) _cell_angle_gamma 90.00 _cell_volume 796.33(14) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 4998 _cell_measurement_theta_min 3.36 _cell_measurement_theta_max 32.26 _exptl_crystal_description NEEDLE _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.186 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 312 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.9569 _exptl_absorpt_correction_T_max 0.9976 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12129 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 30.50 _reflns_number_total 2430 _reflns_number_gt 1824 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0768P)^2^+0.1551P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2430 _refine_ls_number_parameters 98 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1420 _refine_ls_wR_factor_gt 0.1277 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 O O 0.34794(8) 0.45075(16) 0.51375(9) 0.0337(2) Uani 1 1 d . . . N1 N 0.47431(9) 0.25754(18) 0.41380(10) 0.0277(2) Uani 1 1 d . . . H1 H 0.5273(15) 0.346(3) 0.4322(16) 0.039(4) Uiso 1 1 d . . . N2 N 0.29957(8) 0.15288(17) 0.38178(9) 0.0247(2) Uani 1 1 d . . . C1 C 0.19033(9) 0.1036(2) 0.42408(11) 0.0257(3) Uani 1 1 d . . . C2 C 0.37160(10) 0.30095(19) 0.44315(10) 0.0239(2) Uani 1 1 d . . . C3 C 0.36203(11) -0.0172(2) 0.32617(12) 0.0306(3) Uani 1 1 d . . . H3A H 0.3282 -0.0543 0.2407 0.037 Uiso 1 1 calc R . . H3B H 0.3667 -0.1514 0.3782 0.037 Uiso 1 1 calc R . . C4 C 0.47437(11) 0.0848(2) 0.32275(12) 0.0298(3) Uani 1 1 d . . . H4A H 0.5338 -0.0224 0.3468 0.036 Uiso 1 1 calc R . . H4B H 0.4832 0.1437 0.2385 0.036 Uiso 1 1 calc R . . C11 C 0.12135(11) 0.3127(2) 0.42282(14) 0.0357(3) Uani 1 1 d . . . H11A H 0.1169 0.3801 0.3396 0.053 Uiso 1 1 calc R . . H11B H 0.1559 0.4154 0.4854 0.053 Uiso 1 1 calc R . . H11C H 0.0471 0.2768 0.4427 0.053 Uiso 1 1 calc R . . C12 C 0.20621(11) 0.0027(2) 0.55566(12) 0.0326(3) Uani 1 1 d . . . H12A H 0.2444 0.1076 0.6144 0.049 Uiso 1 1 calc R . . H12B H 0.2502 -0.1312 0.5541 0.049 Uiso 1 1 calc R . . H12C H 0.1342 -0.0326 0.5825 0.049 Uiso 1 1 calc R . . C13 C 0.13119(12) -0.0597(3) 0.33151(14) 0.0377(3) Uani 1 1 d . . . H13A H 0.1260 0.0012 0.2466 0.057 Uiso 1 1 calc R . . H13B H 0.0570 -0.0876 0.3544 0.057 Uiso 1 1 calc R . . H13C H 0.1727 -0.1973 0.3342 0.057 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 O 0.0313(5) 0.0323(5) 0.0386(5) -0.0148(4) 0.0088(4) -0.0097(4) N1 0.0251(5) 0.0309(5) 0.0276(5) -0.0081(4) 0.0043(4) -0.0092(4) N2 0.0258(5) 0.0236(5) 0.0247(5) -0.0034(4) 0.0035(4) -0.0062(4) C1 0.0227(5) 0.0265(6) 0.0277(6) -0.0007(4) 0.0014(4) -0.0061(4) C2 0.0260(5) 0.0240(5) 0.0214(5) -0.0003(4) 0.0018(4) -0.0061(4) C3 0.0296(6) 0.0330(7) 0.0290(6) -0.0078(5) 0.0023(5) -0.0029(5) C4 0.0299(6) 0.0303(6) 0.0297(6) -0.0062(5) 0.0063(5) -0.0071(5) C11 0.0268(6) 0.0331(7) 0.0464(8) 0.0017(6) 0.0011(5) -0.0002(5) C12 0.0297(6) 0.0381(7) 0.0306(6) 0.0053(5) 0.0059(5) -0.0062(5) C13 0.0323(7) 0.0393(8) 0.0406(7) -0.0085(6) 0.0002(5) -0.0148(6) _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 O C2 1.2425(14) . ? N1 C2 1.3533(16) . ? N1 C4 1.4386(16) . ? N2 C2 1.3778(14) . ? N2 C3 1.4555(17) . ? N2 C1 1.4871(15) . ? C1 C11 1.5296(19) . ? C1 C13 1.5318(18) . ? C1 C12 1.5339(18) . ? C3 C4 1.5112(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 N1 C4 111.84(10) . . ? C2 N2 C3 109.18(10) . . ? C2 N2 C1 122.28(10) . . ? C3 N2 C1 120.64(10) . . ? N2 C1 C11 109.90(10) . . ? N2 C1 C13 107.97(10) . . ? C11 C1 C13 108.55(11) . . ? N2 C1 C12 109.64(10) . . ? C11 C1 C12 110.91(11) . . ? C13 C1 C12 109.81(11) . . ? O C2 N1 124.78(10) . . ? O C2 N2 126.57(11) . . ? N1 C2 N2 108.64(10) . . ? N2 C3 C4 103.56(10) . . ? N1 C4 C3 102.54(10) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.398 _refine_diff_density_min -0.256 _refine_diff_density_rms 0.050 # Attachment '- tmbs10.cif' data_tmbs10 _database_code_depnum_ccdc_archive 'CCDC 794067' #TrackingRef '- tmbs10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H68 B2 N12 Na2 O3 S6' _chemical_formula_weight 1265.22 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' 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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 34.381(13) _cell_length_b 16.553(6) _cell_length_c 11.073(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.783(6) _cell_angle_gamma 90.00 _cell_volume 6257(4) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 8221 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 30.37 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2656 _exptl_absorpt_coefficient_mu 0.288 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.9527 _exptl_absorpt_correction_T_max 0.9829 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 37010 _diffrn_reflns_av_R_equivalents 0.0796 _diffrn_reflns_av_sigmaI/netI 0.0812 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 30.55 _reflns_number_total 9564 _reflns_number_gt 5774 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9564 _refine_ls_number_parameters 391 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1018 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1176 _refine_ls_wR_factor_gt 0.0990 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Na Na 0.04658(2) 0.25726(5) 0.22753(7) 0.02121(18) Uani 1 1 d . . . B B 0.16642(7) 0.24115(14) 0.1922(2) 0.0198(5) Uani 1 1 d . . . H1 H 0.1990(5) 0.2359(10) 0.1845(16) 0.010(5) Uiso 1 1 d . . . N12 N 0.13569(5) 0.44406(10) 0.29488(15) 0.0235(4) Uani 1 1 d . . . N11 N 0.15930(5) 0.32674(9) 0.24084(14) 0.0190(3) Uani 1 1 d . . . N22 N 0.13484(5) 0.09667(10) 0.42361(14) 0.0199(4) Uani 1 1 d . . . N21 N 0.15636(5) 0.17355(9) 0.28149(14) 0.0176(3) Uani 1 1 d . . . N32 N 0.10632(5) 0.19797(10) -0.10581(14) 0.0206(4) Uani 1 1 d . . . N31 N 0.14594(5) 0.22663(9) 0.06138(14) 0.0167(3) Uani 1 1 d . . . S1 S 0.089996(15) 0.37472(3) 0.10715(5) 0.02212(12) Uani 1 1 d . . . S2 S 0.106150(16) 0.24873(3) 0.42298(4) 0.02258(12) Uani 1 1 d . . . S3 S 0.080400(15) 0.13606(3) 0.09516(5) 0.02187(12) Uani 1 1 d . . . O1 O 0.0000 0.14605(11) 0.2500 0.0219(4) Uani 1 2 d S . . O2 O 0.01058(4) 0.31677(8) 0.39194(12) 0.0240(3) Uani 1 1 d . . . C11 C 0.12933(6) 0.38043(12) 0.21587(17) 0.0202(4) Uani 1 1 d . . . C12 C 0.16983(6) 0.43084(12) 0.37241(19) 0.0256(5) Uani 1 1 d . . . C13 C 0.18796(7) 0.47655(14) 0.4686(2) 0.0340(6) Uani 1 1 d . . . H13A H 0.1772 0.5262 0.4920 0.041 Uiso 1 1 calc R . . C14 C 0.22253(7) 0.44601(15) 0.5287(2) 0.0387(6) Uani 1 1 d . . . H14A H 0.2357 0.4752 0.5953 0.046 Uiso 1 1 calc R . . C15 C 0.23823(7) 0.37393(15) 0.4938(2) 0.0361(6) Uani 1 1 d . . . H15A H 0.2623 0.3554 0.5358 0.043 Uiso 1 1 calc R . . C16 C 0.21970(6) 0.32769(14) 0.39860(19) 0.0281(5) Uani 1 1 d . . . H16A H 0.2304 0.2777 0.3761 0.034 Uiso 1 1 calc R . . C17 C 0.18490(6) 0.35787(12) 0.33788(18) 0.0225(4) Uani 1 1 d . . . C18 C 0.11210(7) 0.51713(13) 0.2955(2) 0.0343(5) Uani 1 1 d . . . H18A H 0.0875 0.5096 0.2423 0.051 Uiso 1 1 calc R . . H18B H 0.1265 0.5627 0.2660 0.051 Uiso 1 1 calc R . . H18C H 0.1064 0.5282 0.3785 0.051 Uiso 1 1 calc R . . C21 C 0.13330(6) 0.17273(12) 0.37337(17) 0.0196(4) Uani 1 1 d . . . C22 C 0.15874(6) 0.04792(11) 0.36215(17) 0.0185(4) Uani 1 1 d . . . C23 C 0.16945(6) -0.03291(12) 0.37761(19) 0.0245(5) Uani 1 1 d . . . H23A H 0.1600 -0.0654 0.4385 0.029 Uiso 1 1 calc R . . C24 C 0.19457(6) -0.06358(12) 0.2997(2) 0.0272(5) Uani 1 1 d . . . H24A H 0.2027 -0.1184 0.3077 0.033 Uiso 1 1 calc R . . C25 C 0.20809(6) -0.01572(13) 0.2101(2) 0.0266(5) Uani 1 1 d . . . H25A H 0.2252 -0.0387 0.1582 0.032 Uiso 1 1 calc R . . C26 C 0.19723(6) 0.06473(12) 0.19442(18) 0.0224(4) Uani 1 1 d . . . H26A H 0.2065 0.0970 0.1329 0.027 Uiso 1 1 calc R . . C27 C 0.17212(5) 0.09616(11) 0.27287(17) 0.0183(4) Uani 1 1 d . . . C28 C 0.11586(6) 0.07143(13) 0.52837(18) 0.0273(5) Uani 1 1 d . . . H28A H 0.0939 0.1077 0.5379 0.041 Uiso 1 1 calc R . . H28B H 0.1348 0.0735 0.6017 0.041 Uiso 1 1 calc R . . H28C H 0.1061 0.0161 0.5159 0.041 Uiso 1 1 calc R . . C31 C 0.11178(6) 0.18896(11) 0.01825(17) 0.0185(4) Uani 1 1 d . . . C32 C 0.13733(6) 0.24097(12) -0.14304(18) 0.0211(4) Uani 1 1 d . . . C33 C 0.14527(7) 0.26319(13) -0.25897(19) 0.0287(5) Uani 1 1 d . . . H33A H 0.1280 0.2501 -0.3296 0.034 Uiso 1 1 calc R . . C34 C 0.17960(7) 0.30520(14) -0.2657(2) 0.0335(5) Uani 1 1 d . . . H34A H 0.1861 0.3217 -0.3430 0.040 Uiso 1 1 calc R . . C35 C 0.20499(7) 0.32409(14) -0.1618(2) 0.0334(5) Uani 1 1 d . . . H35A H 0.2285 0.3526 -0.1702 0.040 Uiso 1 1 calc R . . C36 C 0.19671(6) 0.30210(13) -0.0454(2) 0.0275(5) Uani 1 1 d . . . H36A H 0.2139 0.3157 0.0253 0.033 Uiso 1 1 calc R . . C37 C 0.16224(6) 0.25935(11) -0.03800(18) 0.0187(4) Uani 1 1 d . . . C38 C 0.07467(6) 0.16258(14) -0.18694(19) 0.0313(5) Uani 1 1 d . . . H38A H 0.0505 0.1634 -0.1479 0.047 Uiso 1 1 calc R . . H38B H 0.0813 0.1066 -0.2051 0.047 Uiso 1 1 calc R . . H38C H 0.0708 0.1938 -0.2626 0.047 Uiso 1 1 calc R . . C41 C 0.01601(7) 0.09500(13) 0.3501(2) 0.0316(5) Uani 1 1 d . . . H41A H 0.0070 0.1134 0.4273 0.038 Uiso 1 1 calc R . . H41B H 0.0450 0.0961 0.3590 0.038 Uiso 1 1 calc R . . C51 C 0.01041(7) 0.29021(14) 0.51684(19) 0.0311(5) Uani 1 1 d . . . H51A H 0.0298 0.2465 0.5364 0.037 Uiso 1 1 calc R . . H51B H -0.0158 0.2699 0.5302 0.037 Uiso 1 1 calc R . . C52 C 0.02116(8) 0.36444(15) 0.5955(2) 0.0444(7) Uani 1 1 d . . . H52A H -0.0025 0.3948 0.6116 0.053 Uiso 1 1 calc R . . H52B H 0.0363 0.3492 0.6739 0.053 Uiso 1 1 calc R . . C53 C 0.04600(7) 0.41321(14) 0.5175(2) 0.0379(6) Uani 1 1 d . . . H53A H 0.0467 0.4711 0.5402 0.046 Uiso 1 1 calc R . . H53B H 0.0731 0.3922 0.5228 0.046 Uiso 1 1 calc R . . C54 C 0.02405(7) 0.39982(13) 0.3927(2) 0.0297(5) Uani 1 1 d . . . H54A H 0.0016 0.4374 0.3782 0.036 Uiso 1 1 calc R . . H54B H 0.0415 0.4084 0.3289 0.036 Uiso 1 1 calc R . . C55 C 0.00092(8) 0.01075(14) 0.3180(2) 0.0472(7) Uani 1 1 d . . . H55A H 0.0192 -0.0311 0.3550 0.057 Uiso 1 1 calc R . . H55B H -0.0253 0.0020 0.3444 0.057 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 Na 0.0205(4) 0.0223(4) 0.0207(4) 0.0003(3) 0.0021(3) 0.0002(3) B 0.0186(11) 0.0214(11) 0.0188(11) 0.0024(9) 0.0000(9) -0.0006(9) N12 0.0312(10) 0.0166(8) 0.0218(9) -0.0006(7) 0.0001(7) -0.0012(7) N11 0.0214(9) 0.0176(8) 0.0170(8) 0.0017(6) -0.0023(7) -0.0033(7) N22 0.0237(9) 0.0206(9) 0.0154(8) 0.0018(7) 0.0029(7) 0.0006(7) N21 0.0201(8) 0.0181(8) 0.0146(8) -0.0004(6) 0.0021(6) -0.0004(7) N32 0.0226(9) 0.0222(9) 0.0167(8) -0.0008(7) 0.0012(7) -0.0016(7) N31 0.0171(8) 0.0178(8) 0.0156(8) 0.0010(6) 0.0033(6) -0.0021(6) S1 0.0227(3) 0.0213(3) 0.0213(3) 0.0024(2) -0.0018(2) 0.0001(2) S2 0.0260(3) 0.0240(3) 0.0177(2) -0.0010(2) 0.0021(2) 0.0053(2) S3 0.0211(3) 0.0210(3) 0.0245(3) -0.0018(2) 0.0071(2) -0.0042(2) O1 0.0212(10) 0.0197(10) 0.0249(11) 0.000 0.0030(8) 0.000 O2 0.0244(8) 0.0248(8) 0.0227(8) -0.0046(6) 0.0026(6) -0.0021(6) C11 0.0245(10) 0.0178(9) 0.0179(10) 0.0017(8) 0.0014(8) -0.0036(8) C12 0.0330(12) 0.0232(11) 0.0199(10) 0.0032(8) 0.0007(9) -0.0089(9) C13 0.0514(15) 0.0267(12) 0.0229(11) -0.0004(9) -0.0005(11) -0.0158(11) C14 0.0515(16) 0.0402(14) 0.0218(12) 0.0016(10) -0.0063(11) -0.0276(12) C15 0.0336(13) 0.0432(15) 0.0280(12) 0.0120(11) -0.0112(10) -0.0188(11) C16 0.0286(12) 0.0296(12) 0.0246(11) 0.0079(9) -0.0031(9) -0.0088(10) C17 0.0265(11) 0.0209(10) 0.0194(10) 0.0033(8) -0.0007(8) -0.0087(8) C18 0.0427(14) 0.0208(11) 0.0392(14) -0.0053(10) 0.0044(11) 0.0028(10) C21 0.0195(10) 0.0239(10) 0.0142(9) -0.0004(8) -0.0035(8) 0.0011(8) C22 0.0191(10) 0.0200(10) 0.0154(9) -0.0009(8) -0.0019(8) -0.0005(8) C23 0.0266(11) 0.0198(10) 0.0255(11) 0.0029(8) -0.0043(9) -0.0017(9) C24 0.0292(12) 0.0184(10) 0.0318(12) -0.0058(9) -0.0057(9) 0.0028(9) C25 0.0218(11) 0.0290(12) 0.0282(12) -0.0079(9) 0.0005(9) 0.0019(9) C26 0.0214(10) 0.0261(11) 0.0193(10) -0.0021(8) 0.0008(8) -0.0025(8) C27 0.0171(9) 0.0182(9) 0.0183(10) -0.0006(8) -0.0030(8) -0.0005(8) C28 0.0296(12) 0.0312(12) 0.0218(11) 0.0074(9) 0.0061(9) -0.0003(9) C31 0.0193(10) 0.0168(9) 0.0196(10) -0.0013(8) 0.0035(8) 0.0026(8) C32 0.0268(11) 0.0194(10) 0.0181(10) 0.0000(8) 0.0073(8) 0.0035(8) C33 0.0398(13) 0.0291(12) 0.0180(10) 0.0016(9) 0.0066(9) 0.0021(10) C34 0.0454(15) 0.0336(13) 0.0246(12) 0.0066(10) 0.0170(11) 0.0024(11) C35 0.0331(13) 0.0327(13) 0.0370(13) 0.0080(10) 0.0149(11) -0.0066(10) C36 0.0255(11) 0.0276(11) 0.0297(12) 0.0029(9) 0.0050(9) -0.0031(9) C37 0.0216(10) 0.0158(9) 0.0198(10) 0.0029(8) 0.0066(8) 0.0016(8) C38 0.0308(12) 0.0392(13) 0.0223(11) -0.0052(10) -0.0040(9) -0.0071(10) C41 0.0264(12) 0.0310(12) 0.0370(13) 0.0116(10) 0.0019(10) 0.0047(10) C51 0.0338(13) 0.0371(13) 0.0233(11) 0.0004(10) 0.0067(9) -0.0010(10) C52 0.0623(18) 0.0454(16) 0.0256(12) -0.0100(11) 0.0060(12) 0.0036(14) C53 0.0408(14) 0.0300(13) 0.0413(14) -0.0144(11) -0.0025(12) -0.0022(11) C54 0.0339(13) 0.0224(11) 0.0334(12) -0.0051(9) 0.0073(10) -0.0042(9) C55 0.0537(17) 0.0244(12) 0.0689(19) 0.0094(12) 0.0298(16) 0.0090(12) _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 Na O2 2.4430(17) 2 ? Na O1 2.4715(17) . ? Na O2 2.5195(17) . ? Na S2 2.8021(12) . ? Na S3 2.8157(11) . ? Na S1 2.8734(11) . ? Na Na 3.2987(19) 2 ? B H1 1.138(18) . ? B N11 1.545(3) . ? B N31 1.553(3) . ? B N21 1.559(3) . ? N12 C11 1.370(2) . ? N12 C12 1.387(3) . ? N12 C18 1.457(3) . ? N11 C11 1.364(3) . ? N11 C17 1.404(2) . ? N22 C21 1.375(2) . ? N22 C22 1.386(2) . ? N22 C28 1.458(3) . ? N21 C21 1.362(2) . ? N21 C27 1.399(2) . ? N32 C31 1.373(2) . ? N32 C32 1.385(3) . ? N32 C38 1.450(2) . ? N31 C31 1.365(2) . ? N31 C37 1.401(2) . ? S1 C11 1.704(2) . ? S2 C21 1.696(2) . ? S3 C31 1.695(2) . ? O1 C41 1.450(2) 2 ? O1 C41 1.450(2) . ? O1 Na 2.4716(17) 2 ? O2 C54 1.450(2) . ? O2 C51 1.452(3) . ? O2 Na 2.4431(17) 2 ? C12 C17 1.386(3) . ? C12 C13 1.393(3) . ? C13 C14 1.387(3) . ? C14 C15 1.383(4) . ? C15 C16 1.395(3) . ? C16 C17 1.394(3) . ? C22 C27 1.391(3) . ? C22 C23 1.393(3) . ? C23 C24 1.387(3) . ? C24 C25 1.392(3) . ? C25 C26 1.388(3) . ? C26 C27 1.396(3) . ? C32 C33 1.393(3) . ? C32 C37 1.394(3) . ? C33 C34 1.379(3) . ? C34 C35 1.395(3) . ? C35 C36 1.400(3) . ? C36 C37 1.391(3) . ? C41 C55 1.515(3) . ? C51 C52 1.526(3) . ? C52 C53 1.517(4) . ? C53 C54 1.510(3) . ? C55 C55 1.501(5) 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 O2 Na O1 82.27(5) 2 . ? O2 Na O2 78.54(6) 2 . ? O1 Na O2 80.74(5) . . ? O2 Na S2 155.01(5) 2 . ? O1 Na S2 107.93(4) . . ? O2 Na S2 80.69(5) . . ? O2 Na S3 111.14(5) 2 . ? O1 Na S3 80.45(4) . . ? O2 Na S3 157.37(5) . . ? S2 Na S3 93.27(3) . . ? O2 Na S1 84.53(5) 2 . ? O1 Na S1 158.28(3) . . ? O2 Na S1 113.39(5) . . ? S2 Na S1 91.14(3) . . ? S3 Na S1 88.37(4) . . ? O2 Na Na 49.34(4) 2 2 ? O1 Na Na 48.14(4) . 2 ? O2 Na Na 47.36(4) . 2 ? S2 Na Na 121.18(4) . 2 ? S3 Na Na 123.13(3) . 2 ? S1 Na Na 129.56(3) . 2 ? H1 B N11 107.1(9) . . ? H1 B N31 105.1(9) . . ? N11 B N31 113.18(16) . . ? H1 B N21 106.7(9) . . ? N11 B N21 112.41(17) . . ? N31 B N21 111.73(16) . . ? C11 N12 C12 109.47(17) . . ? C11 N12 C18 126.46(17) . . ? C12 N12 C18 123.99(17) . . ? C11 N11 C17 107.84(16) . . ? C11 N11 B 132.36(16) . . ? C17 N11 B 119.47(16) . . ? C21 N22 C22 109.34(16) . . ? C21 N22 C28 125.80(17) . . ? C22 N22 C28 124.81(17) . . ? C21 N21 C27 107.84(16) . . ? C21 N21 B 132.32(17) . . ? C27 N21 B 119.83(16) . . ? C31 N32 C32 109.55(16) . . ? C31 N32 C38 125.45(17) . . ? C32 N32 C38 124.83(17) . . ? C31 N31 C37 108.01(16) . . ? C31 N31 B 132.34(16) . . ? C37 N31 B 119.57(16) . . ? C11 S1 Na 97.02(7) . . ? C21 S2 Na 99.63(7) . . ? C31 S3 Na 102.71(7) . . ? C41 O1 C41 108.7(2) 2 . ? C41 O1 Na 123.30(10) 2 . ? C41 O1 Na 108.61(10) . . ? C41 O1 Na 108.61(10) 2 2 ? C41 O1 Na 123.30(10) . 2 ? Na O1 Na 83.72(7) . 2 ? C54 O2 C51 108.58(15) . . ? C54 O2 Na 128.40(12) . 2 ? C51 O2 Na 107.46(12) . 2 ? C54 O2 Na 101.02(12) . . ? C51 O2 Na 128.87(12) . . ? Na O2 Na 83.30(6) 2 . ? N11 C11 N12 108.15(16) . . ? N11 C11 S1 128.66(15) . . ? N12 C11 S1 123.18(15) . . ? C17 C12 N12 106.46(17) . . ? C17 C12 C13 122.4(2) . . ? N12 C12 C13 131.1(2) . . ? C14 C13 C12 116.7(2) . . ? C15 C14 C13 121.4(2) . . ? C14 C15 C16 121.7(2) . . ? C17 C16 C15 117.2(2) . . ? C12 C17 C16 120.46(19) . . ? C12 C17 N11 108.05(18) . . ? C16 C17 N11 131.5(2) . . ? N21 C21 N22 108.26(17) . . ? N21 C21 S2 128.75(15) . . ? N22 C21 S2 123.00(15) . . ? N22 C22 C27 106.25(16) . . ? N22 C22 C23 131.47(19) . . ? C27 C22 C23 122.28(19) . . ? C24 C23 C22 116.8(2) . . ? C23 C24 C25 121.3(2) . . ? C26 C25 C24 121.8(2) . . ? C25 C26 C27 117.18(19) . . ? C22 C27 C26 120.62(18) . . ? C22 C27 N21 108.30(17) . . ? C26 C27 N21 131.07(18) . . ? N31 C31 N32 108.11(16) . . ? N31 C31 S3 129.24(15) . . ? N32 C31 S3 122.61(15) . . ? N32 C32 C33 130.68(19) . . ? N32 C32 C37 106.41(17) . . ? C33 C32 C37 122.9(2) . . ? C34 C33 C32 116.4(2) . . ? C33 C34 C35 121.6(2) . . ? C34 C35 C36 121.7(2) . . ? C37 C36 C35 117.0(2) . . ? C36 C37 C32 120.36(19) . . ? C36 C37 N31 131.72(18) . . ? C32 C37 N31 107.91(17) . . ? O1 C41 C55 105.59(19) . . ? O2 C51 C52 105.76(18) . . ? C53 C52 C51 102.62(19) . . ? C54 C53 C52 100.87(19) . . ? O2 C54 C53 105.61(17) . . ? C55 C55 C41 102.01(15) 2 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.55 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.594 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.071 # Attachment '- tofes10.cif' data_tofes10 _database_code_depnum_ccdc_archive 'CCDC 794068' #TrackingRef '- tofes10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H46 B2 Cl6 Fe N12 O6' _chemical_formula_weight 1201.16 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.765(7) _cell_length_b 11.496(8) _cell_length_c 13.698(9) _cell_angle_alpha 87.906(10) _cell_angle_beta 69.479(10) _cell_angle_gamma 72.277(10) _cell_volume 1367.6(16) _cell_formula_units_Z 1 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 4178 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 26.61 _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 0.629 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9115 _exptl_absorpt_correction_T_max 0.9692 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16628 _diffrn_reflns_av_R_equivalents 0.0727 _diffrn_reflns_av_sigmaI/netI 0.1430 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 30.62 _reflns_number_total 8255 _reflns_number_gt 4061 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8255 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1569 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.1527 _refine_ls_wR_factor_gt 0.1219 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Fe Fe 0.5000 0.0000 0.5000 0.01870(17) Uani 1 2 d S . . B B 0.7401(4) 0.1608(3) 0.2898(3) 0.0184(8) Uani 1 1 d . . . H1 H 0.803(3) 0.203(3) 0.226(2) 0.011(8) Uiso 1 1 d . . . O1 O 0.7311(2) -0.0101(2) 0.46887(17) 0.0209(5) Uani 1 1 d . . . O2 O 0.4579(2) 0.18994(19) 0.49093(17) 0.0201(5) Uani 1 1 d . . . O3 O 0.5522(3) -0.0212(2) 0.33674(17) 0.0234(5) Uani 1 1 d . . . N11 N 0.8499(3) 0.0331(2) 0.2955(2) 0.0173(6) Uani 1 1 d . . . N12 N 0.9638(3) -0.1363(2) 0.3564(2) 0.0219(6) Uani 1 1 d . . . N21 N 0.6791(3) 0.2415(2) 0.3927(2) 0.0168(6) Uani 1 1 d . . . N22 N 0.5410(3) 0.3300(2) 0.5538(2) 0.0191(6) Uani 1 1 d . . . N31 N 0.6051(3) 0.1532(2) 0.2595(2) 0.0185(6) Uani 1 1 d . . . N32 N 0.4051(3) 0.1055(3) 0.2503(2) 0.0289(7) Uani 1 1 d . . . C11 C 0.9857(4) -0.2292(3) 0.4288(3) 0.0348(9) Uani 1 1 d . . . H11A H 0.8885 -0.2177 0.4874 0.052 Uiso 1 1 calc R . . H11B H 1.0643 -0.2221 0.4551 0.052 Uiso 1 1 calc R . . H11C H 1.0190 -0.3105 0.3927 0.052 Uiso 1 1 calc R . . C12 C 0.8366(4) -0.0340(3) 0.3814(2) 0.0182(7) Uani 1 1 d . . . C13 C 1.0594(4) -0.1350(3) 0.2540(3) 0.0225(7) Uani 1 1 d . . . C14 C 0.9879(3) -0.0288(3) 0.2159(2) 0.0167(7) Uani 1 1 d . . . C15 C 1.0556(4) -0.0033(3) 0.1140(3) 0.0228(7) Uani 1 1 d . . . H15A H 1.0077 0.0682 0.0866 0.027 Uiso 1 1 calc R . . C16 C 1.1966(4) -0.0856(3) 0.0526(3) 0.0305(9) Uani 1 1 d . . . H16A H 1.2454 -0.0692 -0.0174 0.037 Uiso 1 1 calc R . . C17 C 1.2665(4) -0.1904(3) 0.0914(3) 0.0321(9) Uani 1 1 d . . . H17A H 1.3620 -0.2450 0.0475 0.039 Uiso 1 1 calc R . . C18 C 1.2002(4) -0.2174(3) 0.1929(3) 0.0275(8) Uani 1 1 d . . . H18A H 1.2484 -0.2891 0.2199 0.033 Uiso 1 1 calc R . . C21 C 0.4261(4) 0.3538(3) 0.6585(3) 0.0278(8) Uani 1 1 d . . . H21A H 0.3683 0.2951 0.6697 0.042 Uiso 1 1 calc R . . H21B H 0.3554 0.4373 0.6668 0.042 Uiso 1 1 calc R . . H21C H 0.4770 0.3451 0.7098 0.042 Uiso 1 1 calc R . . C22 C 0.5520(4) 0.2475(3) 0.4798(2) 0.0182(7) Uani 1 1 d . . . C23 C 0.6584(4) 0.3819(3) 0.5137(3) 0.0190(7) Uani 1 1 d . . . C24 C 0.7471(4) 0.3244(3) 0.4131(2) 0.0180(7) Uani 1 1 d . . . C25 C 0.8774(4) 0.3542(3) 0.3527(3) 0.0224(7) Uani 1 1 d . . . H25A H 0.9402 0.3143 0.2852 0.027 Uiso 1 1 calc R . . C26 C 0.9123(4) 0.4455(3) 0.3952(3) 0.0265(8) Uani 1 1 d . . . H26A H 1.0014 0.4671 0.3561 0.032 Uiso 1 1 calc R . . C27 C 0.8200(4) 0.5051(3) 0.4931(3) 0.0272(8) Uani 1 1 d . . . H27A H 0.8451 0.5688 0.5182 0.033 Uiso 1 1 calc R . . C28 C 0.6916(4) 0.4737(3) 0.5554(3) 0.0234(7) Uani 1 1 d . . . H28A H 0.6296 0.5131 0.6231 0.028 Uiso 1 1 calc R . . C31 C 0.2915(5) 0.0418(4) 0.2683(3) 0.0461(11) Uani 1 1 d . . . H31A H 0.3189 -0.0315 0.3050 0.069 Uiso 1 1 calc R . . H31B H 0.2893 0.0178 0.2010 0.069 Uiso 1 1 calc R . . H31C H 0.1897 0.0962 0.3109 0.069 Uiso 1 1 calc R . . C32 C 0.5250(4) 0.0707(3) 0.2870(2) 0.0219(7) Uani 1 1 d . . . C33 C 0.4036(4) 0.2147(4) 0.2036(3) 0.0306(9) Uani 1 1 d . . . C34 C 0.5281(4) 0.2459(3) 0.2113(2) 0.0225(7) Uani 1 1 d . . . C35 C 0.5553(4) 0.3532(3) 0.1744(3) 0.0274(8) Uani 1 1 d . . . H35A H 0.6386 0.3753 0.1800 0.033 Uiso 1 1 calc R . . C36 C 0.4569(5) 0.4280(4) 0.1287(3) 0.0366(10) Uani 1 1 d . . . H36A H 0.4732 0.5023 0.1029 0.044 Uiso 1 1 calc R . . C37 C 0.3366(5) 0.3962(4) 0.1203(3) 0.0487(12) Uani 1 1 d . . . H37A H 0.2715 0.4494 0.0887 0.058 Uiso 1 1 calc R . . C38 C 0.3070(4) 0.2880(4) 0.1569(3) 0.0434(11) Uani 1 1 d . . . H38A H 0.2245 0.2660 0.1499 0.052 Uiso 1 1 calc R . . C1 C 0.0668(5) 0.2735(4) 0.9163(3) 0.0406(10) Uani 1 1 d . . . H1A H 0.0145 0.2133 0.9096 0.049 Uiso 1 1 calc R . . Cl1 Cl 0.06123(12) 0.37465(10) 0.81788(8) 0.0438(3) Uani 1 1 d . . . Cl2 Cl 0.25667(16) 0.19270(13) 0.90207(10) 0.0787(5) Uani 1 1 d . . . Cl3 Cl -0.02980(14) 0.35069(11) 1.04124(8) 0.0568(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0177(4) 0.0169(4) 0.0217(4) 0.0037(3) -0.0057(3) -0.0074(3) B 0.0179(18) 0.0167(19) 0.0187(19) 0.0039(15) -0.0059(15) -0.0038(15) O1 0.0161(11) 0.0244(13) 0.0202(12) 0.0044(10) -0.0055(10) -0.0050(10) O2 0.0164(11) 0.0149(12) 0.0267(13) 0.0026(10) -0.0061(10) -0.0039(9) O3 0.0277(13) 0.0221(13) 0.0236(13) 0.0025(10) -0.0100(10) -0.0113(10) N11 0.0178(13) 0.0149(14) 0.0193(14) 0.0036(11) -0.0076(11) -0.0045(11) N12 0.0201(14) 0.0189(15) 0.0264(16) 0.0069(12) -0.0112(12) -0.0030(12) N21 0.0173(13) 0.0126(13) 0.0209(14) 0.0014(11) -0.0074(11) -0.0045(11) N22 0.0191(14) 0.0164(14) 0.0182(14) -0.0003(11) -0.0051(11) -0.0019(11) N31 0.0189(14) 0.0187(14) 0.0174(14) 0.0016(11) -0.0087(11) -0.0027(11) N32 0.0212(15) 0.0425(19) 0.0272(16) 0.0030(14) -0.0111(13) -0.0126(14) C11 0.037(2) 0.026(2) 0.036(2) 0.0106(17) -0.0150(18) -0.0011(17) C12 0.0168(16) 0.0171(17) 0.0228(17) 0.0000(13) -0.0083(14) -0.0066(13) C13 0.0231(17) 0.0214(18) 0.0247(18) -0.0023(14) -0.0102(15) -0.0066(15) C14 0.0154(15) 0.0168(16) 0.0203(17) 0.0017(13) -0.0089(13) -0.0052(13) C15 0.0229(17) 0.0242(18) 0.0214(18) -0.0009(14) -0.0101(14) -0.0045(15) C16 0.0272(19) 0.040(2) 0.0198(18) -0.0059(16) -0.0045(15) -0.0083(18) C17 0.0211(18) 0.033(2) 0.030(2) -0.0106(17) -0.0038(16) 0.0026(16) C18 0.0246(19) 0.0216(19) 0.031(2) -0.0044(15) -0.0117(16) 0.0036(15) C21 0.0265(19) 0.028(2) 0.0225(18) -0.0033(15) -0.0040(15) -0.0045(16) C22 0.0194(16) 0.0149(16) 0.0204(17) 0.0041(13) -0.0087(14) -0.0038(13) C23 0.0185(16) 0.0126(15) 0.0255(18) 0.0057(13) -0.0121(14) 0.0000(13) C24 0.0191(16) 0.0149(16) 0.0216(17) 0.0044(13) -0.0107(14) -0.0039(13) C25 0.0232(18) 0.0246(19) 0.0209(18) 0.0057(14) -0.0099(14) -0.0075(15) C26 0.0267(19) 0.0239(19) 0.035(2) 0.0117(16) -0.0163(16) -0.0111(15) C27 0.036(2) 0.0201(18) 0.037(2) 0.0074(16) -0.0253(18) -0.0105(16) C28 0.0262(18) 0.0186(17) 0.0272(19) -0.0003(14) -0.0155(15) -0.0020(15) C31 0.035(2) 0.075(3) 0.044(3) 0.009(2) -0.020(2) -0.034(2) C32 0.0208(17) 0.030(2) 0.0168(17) -0.0006(14) -0.0078(14) -0.0088(15) C33 0.0195(18) 0.047(2) 0.0214(19) 0.0012(17) -0.0092(15) -0.0029(17) C34 0.0182(17) 0.0266(19) 0.0168(17) 0.0010(14) -0.0071(14) 0.0023(15) C35 0.0249(19) 0.028(2) 0.0212(18) 0.0008(15) -0.0076(15) 0.0022(16) C36 0.039(2) 0.031(2) 0.022(2) 0.0026(16) -0.0055(17) 0.0092(18) C37 0.031(2) 0.063(3) 0.027(2) 0.009(2) -0.0083(18) 0.018(2) C38 0.021(2) 0.072(3) 0.031(2) 0.007(2) -0.0127(17) -0.002(2) C1 0.051(3) 0.038(2) 0.037(2) 0.0091(19) -0.016(2) -0.020(2) Cl1 0.0434(6) 0.0498(7) 0.0376(6) 0.0118(5) -0.0130(5) -0.0161(5) Cl2 0.0665(9) 0.0789(10) 0.0508(8) 0.0166(7) -0.0081(7) 0.0165(7) Cl3 0.0578(7) 0.0611(8) 0.0330(6) 0.0055(5) 0.0013(5) -0.0133(6) _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 Fe O2 2.103(2) . ? Fe O2 2.103(2) 2_656 ? Fe O1 2.111(3) 2_656 ? Fe O1 2.111(3) . ? Fe O3 2.118(3) . ? Fe O3 2.118(3) 2_656 ? B H1 1.08(3) . ? B N21 1.540(5) . ? B N31 1.541(5) . ? B N11 1.550(4) . ? O1 C12 1.249(4) . ? O2 C22 1.253(4) . ? O3 C32 1.247(4) . ? N11 C12 1.373(4) . ? N11 C14 1.398(4) . ? N12 C12 1.373(4) . ? N12 C13 1.389(4) . ? N12 C11 1.449(4) . ? N21 C22 1.373(4) . ? N21 C24 1.401(4) . ? N22 C22 1.367(4) . ? N22 C23 1.387(4) . ? N22 C21 1.451(4) . ? N31 C32 1.368(4) . ? N31 C34 1.395(4) . ? N32 C32 1.377(4) . ? N32 C33 1.386(5) . ? N32 C31 1.456(4) . ? C13 C14 1.393(4) . ? C13 C18 1.395(5) . ? C14 C15 1.382(4) . ? C15 C16 1.397(5) . ? C16 C17 1.381(5) . ? C17 C18 1.381(5) . ? C23 C28 1.387(5) . ? C23 C24 1.402(4) . ? C24 C25 1.389(4) . ? C25 C26 1.399(5) . ? C26 C27 1.387(5) . ? C27 C28 1.391(5) . ? C33 C38 1.382(5) . ? C33 C34 1.407(5) . ? C34 C35 1.381(5) . ? C35 C36 1.390(5) . ? C36 C37 1.373(6) . ? C37 C38 1.397(6) . ? C1 Cl2 1.747(4) . ? C1 Cl1 1.752(4) . ? C1 Cl3 1.754(4) . ? 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 Fe O2 179.999(1) . 2_656 ? O2 Fe O1 94.08(8) . 2_656 ? O2 Fe O1 85.92(8) 2_656 2_656 ? O2 Fe O1 85.92(8) . . ? O2 Fe O1 94.08(8) 2_656 . ? O1 Fe O1 180.0 2_656 . ? O2 Fe O3 89.64(8) . . ? O2 Fe O3 90.36(8) 2_656 . ? O1 Fe O3 91.48(8) 2_656 . ? O1 Fe O3 88.52(8) . . ? O2 Fe O3 90.36(8) . 2_656 ? O2 Fe O3 89.64(8) 2_656 2_656 ? O1 Fe O3 88.52(8) 2_656 2_656 ? O1 Fe O3 91.48(8) . 2_656 ? O3 Fe O3 180.0 . 2_656 ? H1 B N21 110.6(15) . . ? H1 B N31 103.4(15) . . ? N21 B N31 110.2(3) . . ? H1 B N11 107.7(15) . . ? N21 B N11 111.7(3) . . ? N31 B N11 112.9(3) . . ? C12 O1 Fe 126.0(2) . . ? C22 O2 Fe 126.8(2) . . ? C32 O3 Fe 120.0(2) . . ? C12 N11 C14 108.0(3) . . ? C12 N11 B 126.5(3) . . ? C14 N11 B 125.4(3) . . ? C12 N12 C13 109.3(3) . . ? C12 N12 C11 122.9(3) . . ? C13 N12 C11 127.8(3) . . ? C22 N21 C24 107.3(3) . . ? C22 N21 B 128.1(3) . . ? C24 N21 B 124.6(3) . . ? C22 N22 C23 109.3(3) . . ? C22 N22 C21 124.0(3) . . ? C23 N22 C21 126.6(3) . . ? C32 N31 C34 108.0(3) . . ? C32 N31 B 128.5(3) . . ? C34 N31 B 122.8(3) . . ? C32 N32 C33 109.1(3) . . ? C32 N32 C31 123.9(3) . . ? C33 N32 C31 126.7(3) . . ? O1 C12 N11 128.2(3) . . ? O1 C12 N12 123.6(3) . . ? N11 C12 N12 108.1(3) . . ? N12 C13 C14 106.6(3) . . ? N12 C13 C18 131.3(3) . . ? C14 C13 C18 122.1(3) . . ? C15 C14 C13 119.9(3) . . ? C15 C14 N11 132.0(3) . . ? C13 C14 N11 108.0(3) . . ? C14 C15 C16 118.1(3) . . ? C17 C16 C15 121.4(3) . . ? C18 C17 C16 121.2(3) . . ? C17 C18 C13 117.3(3) . . ? O2 C22 N22 124.4(3) . . ? O2 C22 N21 126.7(3) . . ? N22 C22 N21 108.8(3) . . ? C28 C23 N22 131.4(3) . . ? C28 C23 C24 122.3(3) . . ? N22 C23 C24 106.3(3) . . ? C25 C24 N21 131.3(3) . . ? C25 C24 C23 120.5(3) . . ? N21 C24 C23 108.2(3) . . ? C24 C25 C26 117.2(3) . . ? C27 C26 C25 121.7(3) . . ? C26 C27 C28 121.5(3) . . ? C23 C28 C27 116.7(3) . . ? O3 C32 N31 127.4(3) . . ? O3 C32 N32 124.2(3) . . ? N31 C32 N32 108.4(3) . . ? C38 C33 N32 132.1(4) . . ? C38 C33 C34 121.5(4) . . ? N32 C33 C34 106.4(3) . . ? C35 C34 N31 131.5(3) . . ? C35 C34 C33 120.6(3) . . ? N31 C34 C33 107.9(3) . . ? C34 C35 C36 117.9(4) . . ? C37 C36 C35 121.2(4) . . ? C36 C37 C38 122.0(4) . . ? C33 C38 C37 116.8(4) . . ? Cl2 C1 Cl1 110.7(2) . . ? Cl2 C1 Cl3 109.5(2) . . ? Cl1 C1 Cl3 111.6(2) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 30.62 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.478 _refine_diff_density_min -0.786 _refine_diff_density_rms 0.093 # Attachment '- ttores10.cif' data_ttores10 _database_code_depnum_ccdc_archive 'CCDC 794069' #TrackingRef '- ttores10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H52 B N6 O6 Re' _chemical_formula_weight 933.91 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' 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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 16.131(2) _cell_length_b 16.131(2) _cell_length_c 9.6857(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2182.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9884 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 27.77 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 948 _exptl_absorpt_coefficient_mu 2.835 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.8712 _exptl_absorpt_correction_T_max 0.9722 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 34854 _diffrn_reflns_av_R_equivalents 0.0818 _diffrn_reflns_av_sigmaI/netI 0.0550 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 30.71 _reflns_number_total 4523 _reflns_number_gt 3279 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0147P)^2^+2.0982P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4523 _refine_ls_number_parameters 175 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0822 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0714 _refine_ls_wR_factor_gt 0.0586 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.131 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Re Re 0.6667 0.3333 0.38047(3) 0.03708(8) Uani 1 3 d S . . B B 0.6667 0.3333 -0.0297(7) 0.0334(15) Uani 1 3 d S . . H1 H 0.6667 0.3333 -0.126(8) 0.049(17) Uiso 1 3 d S . . N11 N 0.5712(2) 0.3255(2) 0.0184(3) 0.0322(7) Uani 1 1 d . . . N12 N 0.4627(2) 0.3456(2) 0.1294(4) 0.0375(7) Uani 1 1 d . . . O1 O 0.7302(3) 0.5029(3) 0.5762(3) 0.0647(10) Uani 1 1 d . . . O11 O 0.61054(19) 0.39638(19) 0.2381(3) 0.0367(6) Uani 1 1 d . . . C1 C 0.7071(3) 0.4387(3) 0.5000(4) 0.0481(11) Uani 1 1 d . . . C11 C 0.5534(3) 0.3578(2) 0.1375(4) 0.0328(8) Uani 1 1 d . . . C12 C 0.4906(3) 0.2912(3) -0.0647(4) 0.0363(9) Uani 1 1 d . . . H12A H 0.4833 0.2636 -0.1537 0.044 Uiso 1 1 calc R . . C13 C 0.4249(3) 0.3036(3) 0.0018(4) 0.0410(9) Uani 1 1 d . . . H13A H 0.3632 0.2868 -0.0321 0.049 Uiso 1 1 calc R . . C14 C 0.4204(3) 0.3857(3) 0.2272(4) 0.0455(10) Uani 1 1 d . . . C15 C 0.4700(5) 0.4912(4) 0.2095(7) 0.105(3) Uani 1 1 d . . . H15A H 0.4580 0.5065 0.1163 0.157 Uiso 1 1 calc R . . H15B H 0.5389 0.5180 0.2228 0.157 Uiso 1 1 calc R . . H15C H 0.4457 0.5187 0.2777 0.157 Uiso 1 1 calc R . . C16 C 0.3137(4) 0.3407(5) 0.1978(7) 0.0867(19) Uani 1 1 d . . . H16A H 0.3045 0.3613 0.1067 0.130 Uiso 1 1 calc R . . H16B H 0.2841 0.3611 0.2684 0.130 Uiso 1 1 calc R . . H16C H 0.2839 0.2708 0.1994 0.130 Uiso 1 1 calc R . . C17 C 0.4301(5) 0.3600(5) 0.3743(6) 0.0885(19) Uani 1 1 d . . . H17A H 0.4981 0.3892 0.3980 0.133 Uiso 1 1 calc R . . H17B H 0.3993 0.2903 0.3832 0.133 Uiso 1 1 calc R . . H17C H 0.3992 0.3841 0.4371 0.133 Uiso 1 1 calc R . . C100 C 0.7481(7) 0.7024(7) 0.3361(9) 0.139(4) Uani 1 1 d . . . H10F H 0.7096 0.6490 0.3936 0.167 Uiso 1 1 calc R . . C101 C 0.7745(8) 0.7943(7) 0.3806(11) 0.160(4) Uani 1 1 d . . . H10D H 0.7533 0.8033 0.4679 0.192 Uiso 1 1 calc R . . C102 C 0.8308(6) 0.8720(6) 0.2994(9) 0.108(2) Uani 1 1 d . . . H10E H 0.8488 0.9351 0.3282 0.130 Uiso 1 1 calc R . . C103 C 0.8600(5) 0.8552(6) 0.1756(8) 0.097(2) Uani 1 1 d . . . H10C H 0.9002 0.9076 0.1175 0.116 Uiso 1 1 calc R . . C104 C 0.8325(4) 0.7646(6) 0.1341(8) 0.0898(19) Uani 1 1 d . . . H10A H 0.8534 0.7548 0.0471 0.108 Uiso 1 1 calc R . . C105 C 0.7764(5) 0.6888(5) 0.2131(7) 0.0886(19) Uani 1 1 d . . . H10B H 0.7570 0.6258 0.1818 0.106 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 Re 0.04507(11) 0.04507(11) 0.02112(10) 0.000 0.000 0.02253(5) B 0.037(2) 0.037(2) 0.027(3) 0.000 0.000 0.0183(12) N11 0.0342(17) 0.0367(18) 0.0281(15) -0.0003(13) -0.0015(13) 0.0194(15) N12 0.0378(18) 0.0387(18) 0.0389(17) 0.0012(16) 0.0016(16) 0.0212(15) O1 0.082(3) 0.067(2) 0.0424(18) -0.0169(16) -0.0009(17) 0.036(2) O11 0.0456(16) 0.0399(15) 0.0273(13) -0.0033(12) -0.0030(12) 0.0235(13) C1 0.060(3) 0.062(3) 0.028(2) 0.000(2) 0.005(2) 0.034(3) C11 0.039(2) 0.0294(19) 0.0283(19) 0.0032(16) 0.0050(17) 0.0162(17) C12 0.037(2) 0.036(2) 0.0340(19) -0.0010(16) -0.0054(16) 0.0174(18) C13 0.038(2) 0.040(2) 0.045(2) 0.0006(19) -0.0038(19) 0.020(2) C14 0.048(3) 0.050(3) 0.047(2) 0.002(2) 0.010(2) 0.032(2) C15 0.134(6) 0.051(3) 0.127(6) 0.002(4) 0.068(5) 0.044(4) C16 0.073(4) 0.103(5) 0.104(5) -0.030(4) 0.003(3) 0.059(4) C17 0.107(5) 0.137(5) 0.056(3) 0.014(4) 0.032(4) 0.087(4) C100 0.177(9) 0.129(7) 0.115(7) 0.056(6) 0.083(7) 0.080(7) C101 0.202(10) 0.131(8) 0.135(8) 0.022(7) 0.104(8) 0.076(8) C102 0.101(6) 0.103(6) 0.119(7) 0.014(5) 0.023(5) 0.051(5) C103 0.077(5) 0.114(6) 0.094(5) 0.040(5) 0.017(4) 0.045(5) C104 0.068(4) 0.125(6) 0.079(4) 0.023(5) 0.009(4) 0.050(4) C105 0.077(4) 0.105(5) 0.095(5) 0.016(4) 0.015(4) 0.054(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_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re C1 1.883(5) 3_665 ? Re C1 1.883(5) 2_655 ? Re C1 1.883(5) . ? Re O11 2.162(3) . ? Re O11 2.162(3) 2_655 ? Re O11 2.162(3) 3_665 ? B H1 0.94(8) . ? B N11 1.553(4) 2_655 ? B N11 1.553(4) 3_665 ? B N11 1.553(4) . ? B H1 0.94(8) . ? N11 C11 1.354(5) . ? N11 C12 1.388(5) . ? N12 C11 1.378(5) . ? N12 C13 1.395(5) . ? N12 C14 1.490(5) . ? O1 C1 1.171(5) . ? O11 C11 1.270(4) . ? C12 C13 1.338(6) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.485(7) . ? C14 C17 1.514(7) . ? C14 C16 1.523(7) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C100 C105 1.332(10) . ? C100 C101 1.391(11) . ? C100 H10F 0.9500 . ? C101 C102 1.369(11) . ? C101 H10D 0.9500 . ? C102 C103 1.365(10) . ? C102 H10E 0.9500 . ? C103 C104 1.358(9) . ? C103 H10C 0.9500 . ? C104 C105 1.340(9) . ? C104 H10A 0.9500 . ? C105 H10B 0.9500 . ? 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 C1 Re C1 86.1(2) 3_665 2_655 ? C1 Re C1 86.1(2) 3_665 . ? C1 Re C1 86.1(2) 2_655 . ? C1 Re O11 172.38(16) 3_665 . ? C1 Re O11 100.36(15) 2_655 . ? C1 Re O11 90.31(15) . . ? C1 Re O11 100.36(15) 3_665 2_655 ? C1 Re O11 90.31(15) 2_655 2_655 ? C1 Re O11 172.38(16) . 2_655 ? O11 Re O11 83.69(10) . 2_655 ? C1 Re O11 90.31(15) 3_665 3_665 ? C1 Re O11 172.38(16) 2_655 3_665 ? C1 Re O11 100.36(15) . 3_665 ? O11 Re O11 83.69(10) . 3_665 ? O11 Re O11 83.69(10) 2_655 3_665 ? H1 B N11 107.5(3) . 2_655 ? H1 B N11 107.5(3) . 3_665 ? N11 B N11 111.4(2) 2_655 3_665 ? H1 B N11 107.5(3) . . ? N11 B N11 111.4(2) 2_655 . ? N11 B N11 111.4(2) 3_665 . ? H1 B H1 0.000(6) . . ? N11 B H1 107.5(3) 2_655 . ? N11 B H1 107.5(3) 3_665 . ? N11 B H1 107.5(3) . . ? C11 N11 C12 108.2(3) . . ? C11 N11 B 128.1(3) . . ? C12 N11 B 123.5(3) . . ? C11 N12 C13 107.1(3) . . ? C11 N12 C14 125.9(3) . . ? C13 N12 C14 126.2(3) . . ? C11 O11 Re 129.1(2) . . ? O1 C1 Re 178.3(4) . . ? O11 C11 N11 126.9(3) . . ? O11 C11 N12 124.9(3) . . ? N11 C11 N12 108.1(3) . . ? C13 C12 N11 108.4(3) . . ? C13 C12 H12A 125.8 . . ? N11 C12 H12A 125.8 . . ? C12 C13 N12 108.2(3) . . ? C12 C13 H13A 125.9 . . ? N12 C13 H13A 125.9 . . ? C15 C14 N12 108.8(4) . . ? C15 C14 C17 110.6(5) . . ? N12 C14 C17 110.3(4) . . ? C15 C14 C16 110.9(5) . . ? N12 C14 C16 109.1(4) . . ? C17 C14 C16 107.0(4) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C105 C100 C101 120.3(8) . . ? C105 C100 H10F 119.8 . . ? C101 C100 H10F 119.8 . . ? C102 C101 C100 120.5(8) . . ? C102 C101 H10D 119.7 . . ? C100 C101 H10D 119.7 . . ? C103 C102 C101 117.4(8) . . ? C103 C102 H10E 121.3 . . ? C101 C102 H10E 121.3 . . ? C104 C103 C102 120.9(7) . . ? C104 C103 H10C 119.5 . . ? C102 C103 H10C 119.5 . . ? C105 C104 C103 121.4(7) . . ? C105 C104 H10A 119.3 . . ? C103 C104 H10A 119.3 . . ? C100 C105 C104 119.4(8) . . ? C100 C105 H10B 120.3 . . ? C104 C105 H10B 120.3 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.71 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 4.813 _refine_diff_density_min -6.921 _refine_diff_density_rms 0.242 # Attachment '- znbtos10.cif' data_znbtos10 _database_code_depnum_ccdc_archive 'CCDC 794070' #TrackingRef '- znbtos10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H50 B2 Cl6 I2 N12 O6 Zn2' _chemical_formula_weight 1545.89 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' 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 0.0060 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.361(5) _cell_length_b 11.221(7) _cell_length_c 17.165(13) _cell_angle_alpha 96.785(11) _cell_angle_beta 103.212(11) _cell_angle_gamma 113.522(8) _cell_volume 1564.5(18) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 6614 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 28.02 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 766 _exptl_absorpt_coefficient_mu 2.065 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.7897 _exptl_absorpt_correction_T_max 0.9599 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24328 _diffrn_reflns_av_R_equivalents 0.0531 _diffrn_reflns_av_sigmaI/netI 0.0751 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 30.15 _reflns_number_total 9138 _reflns_number_gt 5194 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0531P)^2^+1.0111P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9138 _refine_ls_number_parameters 368 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1108 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1335 _refine_ls_wR_factor_gt 0.1122 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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 0.35446(6) 3.03391(5) 0.26116(3) 0.03261(13) Uani 1 1 d . . . I I 0.39554(4) 2.83098(3) 0.27450(2) 0.05111(12) Uani 1 1 d . . . B B 0.3246(6) 3.3310(5) 0.2400(3) 0.0284(10) Uani 1 1 d . . . H1 H 0.312(5) 3.420(4) 0.232(3) 0.034 Uiso 1 1 d . . . O1 O 0.1330(3) 3.0236(3) 0.22761(17) 0.0330(6) Uani 1 1 d . . . O2 O 0.4536(4) 3.1823(3) 0.35902(18) 0.0379(7) Uani 1 1 d . . . O3 O 0.4516(4) 3.1297(3) 0.18268(19) 0.0363(7) Uani 1 1 d . . . N11 N 0.1770(4) 3.2143(3) 0.1737(2) 0.0275(7) Uani 1 1 d . . . N12 N -0.0446(4) 3.0235(4) 0.1105(2) 0.0342(8) Uani 1 1 d . . . N21 N 0.3247(4) 3.3198(3) 0.3293(2) 0.0290(7) Uani 1 1 d . . . N22 N 0.3727(4) 3.2818(3) 0.4539(2) 0.0346(8) Uani 1 1 d . . . N31 N 0.4893(4) 3.3487(3) 0.2276(2) 0.0285(7) Uani 1 1 d . . . N32 N 0.6895(4) 3.3166(4) 0.1962(2) 0.0367(8) Uani 1 1 d . . . C11 C 0.0937(5) 3.0841(4) 0.1755(3) 0.0298(9) Uani 1 1 d . . . C14 C 0.0894(5) 3.2342(4) 0.1026(2) 0.0331(9) Uani 1 1 d . . . C15 C 0.1216(7) 3.3468(5) 0.0707(3) 0.0452(12) Uani 1 1 d . . . H13A H 0.2152 3.4290 0.0977 0.054 Uiso 1 1 calc R . . C16 C 0.0101(8) 3.3333(6) -0.0024(3) 0.0593(15) Uani 1 1 d . . . H14A H 0.0294 3.4079 -0.0266 0.071 Uiso 1 1 calc R . . C17 C -0.1265(8) 3.2162(7) -0.0408(3) 0.0639(17) Uani 1 1 d . . . H15A H -0.1997 3.2124 -0.0907 0.077 Uiso 1 1 calc R . . C18 C -0.1622(7) 3.1022(6) -0.0094(3) 0.0515(13) Uani 1 1 d . . . H16A H -0.2575 3.0208 -0.0359 0.062 Uiso 1 1 calc R . . C13 C -0.0486(5) 3.1156(4) 0.0633(3) 0.0355(10) Uani 1 1 d . . . C12 C -0.1673(5) 2.8871(5) 0.0947(3) 0.0445(12) Uani 1 1 d . . . H18A H -0.1248 2.8395 0.1307 0.067 Uiso 1 1 calc R . . H18B H -0.1948 2.8424 0.0371 0.067 Uiso 1 1 calc R . . H18C H -0.2656 2.8870 0.1057 0.067 Uiso 1 1 calc R . . C21 C 0.3865(5) 3.2549(4) 0.3780(3) 0.0305(9) Uani 1 1 d . . . C24 C 0.2696(5) 3.3923(4) 0.3774(2) 0.0296(9) Uani 1 1 d . . . C25 C 0.1986(5) 3.4762(4) 0.3595(3) 0.0372(10) Uani 1 1 d . . . H23A H 0.1758 3.4924 0.3061 0.045 Uiso 1 1 calc R . . C26 C 0.1615(6) 3.5361(5) 0.4224(3) 0.0454(12) Uani 1 1 d . . . H24A H 0.1123 3.5944 0.4119 0.054 Uiso 1 1 calc R . . C27 C 0.1952(6) 3.5121(5) 0.5006(3) 0.0503(13) Uani 1 1 d . . . H25A H 0.1692 3.5547 0.5427 0.060 Uiso 1 1 calc R . . C28 C 0.2647(5) 3.4287(5) 0.5181(3) 0.0424(11) Uani 1 1 d . . . H26A H 0.2867 3.4120 0.5715 0.051 Uiso 1 1 calc R . . C23 C 0.3023(5) 3.3689(4) 0.4556(3) 0.0346(10) Uani 1 1 d . . . C22 C 0.4188(6) 3.2235(5) 0.5212(3) 0.0504(13) Uani 1 1 d . . . H28A H 0.4566 3.1589 0.5020 0.076 Uiso 1 1 calc R . . H28B H 0.3240 3.1781 0.5400 0.076 Uiso 1 1 calc R . . H28C H 0.5069 3.2944 0.5669 0.076 Uiso 1 1 calc R . . C31 C 0.5352(5) 3.2551(4) 0.2010(3) 0.0315(9) Uani 1 1 d . . . C34 C 0.6205(5) 3.4743(4) 0.2398(2) 0.0302(9) Uani 1 1 d . . . C35 C 0.6368(6) 3.6015(4) 0.2648(3) 0.0378(10) Uani 1 1 d . . . H33A H 0.5511 3.6155 0.2785 0.045 Uiso 1 1 calc R . . C36 C 0.7816(6) 3.7080(5) 0.2694(3) 0.0511(13) Uani 1 1 d . . . H34A H 0.7955 3.7967 0.2864 0.061 Uiso 1 1 calc R . . C37 C 0.9075(6) 3.6872(5) 0.2496(4) 0.0572(15) Uani 1 1 d . . . H35A H 1.0065 3.7621 0.2540 0.069 Uiso 1 1 calc R . . C38 C 0.8911(6) 3.5603(5) 0.2238(3) 0.0492(13) Uani 1 1 d . . . H36A H 0.9761 3.5459 0.2093 0.059 Uiso 1 1 calc R . . C33 C 0.7455(5) 3.4541(4) 0.2198(3) 0.0343(10) Uani 1 1 d . . . C32 C 0.7763(6) 3.2470(5) 0.1679(4) 0.0545(14) Uani 1 1 d . . . H38A H 0.7100 3.1503 0.1575 0.082 Uiso 1 1 calc R . . H38B H 0.8806 3.2736 0.2101 0.082 Uiso 1 1 calc R . . H38C H 0.7969 3.2701 0.1169 0.082 Uiso 1 1 calc R . . C41 C 0.1524(9) 3.8401(8) 0.5959(5) 0.101(3) Uani 1 1 d . . . H41A H 0.1068 3.7436 0.5951 0.121 Uiso 1 1 calc R . . H41B H 0.2722 3.8798 0.6217 0.121 Uiso 1 1 calc R . . Cl41 Cl 0.0702(2) 3.91492(17) 0.65363(14) 0.0953(6) Uani 1 1 d . . . Cl42 Cl 0.1095(4) 3.8604(2) 0.49145(17) 0.1345(10) Uani 1 1 d . . . C51 C 0.428(2) 2.4841(17) -0.0455(11) 0.1105(10) Uiso 0.50 1 d PD A -1 H51A H 0.3159 2.4121 -0.0734 0.133 Uiso 0.50 1 calc PR A -1 H51B H 0.4814 2.5105 -0.0882 0.133 Uiso 0.50 1 calc PR A -1 Cl51 Cl 0.5357(6) 2.4248(5) 0.0205(3) 0.1105(10) Uiso 0.50 1 d PD A -1 Cl52 Cl 0.4145(6) 2.6269(5) 0.0084(3) 0.1105(10) Uiso 0.50 1 d PD A -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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.0327(3) 0.0261(2) 0.0381(3) 0.0080(2) 0.0052(2) 0.0149(2) I 0.0587(2) 0.03847(18) 0.0553(2) 0.01287(15) -0.00173(16) 0.03033(16) B 0.030(2) 0.029(2) 0.032(3) 0.0100(19) 0.014(2) 0.017(2) O1 0.0323(16) 0.0322(15) 0.0374(17) 0.0131(13) 0.0095(13) 0.0163(13) O2 0.0423(18) 0.0337(16) 0.0356(17) 0.0038(13) 0.0019(14) 0.0213(14) O3 0.0419(17) 0.0266(15) 0.0463(18) 0.0072(13) 0.0206(15) 0.0173(14) N11 0.0255(17) 0.0315(17) 0.0301(18) 0.0099(14) 0.0095(14) 0.0157(15) N12 0.0292(19) 0.039(2) 0.034(2) 0.0028(16) 0.0068(16) 0.0171(16) N21 0.0285(18) 0.0276(17) 0.0303(18) 0.0063(14) 0.0088(15) 0.0119(15) N22 0.036(2) 0.0356(19) 0.0277(19) 0.0089(15) 0.0061(16) 0.0126(16) N31 0.0330(19) 0.0245(16) 0.0306(18) 0.0077(14) 0.0119(15) 0.0138(15) N32 0.033(2) 0.036(2) 0.051(2) 0.0145(17) 0.0218(18) 0.0191(17) C11 0.027(2) 0.035(2) 0.031(2) 0.0050(18) 0.0111(17) 0.0156(18) C14 0.041(2) 0.047(3) 0.026(2) 0.0108(19) 0.0114(19) 0.032(2) C15 0.064(3) 0.052(3) 0.038(3) 0.017(2) 0.021(2) 0.038(3) C16 0.095(5) 0.074(4) 0.040(3) 0.028(3) 0.022(3) 0.063(4) C17 0.088(4) 0.094(5) 0.030(3) 0.010(3) 0.004(3) 0.068(4) C18 0.056(3) 0.077(4) 0.029(3) 0.000(2) 0.003(2) 0.045(3) C13 0.036(2) 0.043(2) 0.034(2) 0.004(2) 0.010(2) 0.027(2) C12 0.031(2) 0.041(3) 0.046(3) -0.004(2) 0.003(2) 0.010(2) C21 0.030(2) 0.0234(19) 0.032(2) 0.0036(17) 0.0058(18) 0.0076(17) C24 0.024(2) 0.027(2) 0.031(2) 0.0018(17) 0.0066(17) 0.0064(17) C25 0.036(2) 0.040(2) 0.040(3) 0.009(2) 0.015(2) 0.019(2) C26 0.043(3) 0.041(3) 0.057(3) 0.003(2) 0.024(2) 0.021(2) C27 0.044(3) 0.053(3) 0.050(3) -0.007(2) 0.023(2) 0.018(3) C28 0.035(3) 0.051(3) 0.029(2) -0.001(2) 0.013(2) 0.008(2) C23 0.027(2) 0.034(2) 0.036(2) 0.0047(18) 0.0080(19) 0.0075(18) C22 0.056(3) 0.054(3) 0.033(3) 0.016(2) 0.002(2) 0.020(3) C31 0.035(2) 0.032(2) 0.033(2) 0.0077(18) 0.0142(19) 0.0180(19) C34 0.034(2) 0.028(2) 0.028(2) 0.0116(17) 0.0111(18) 0.0112(18) C35 0.049(3) 0.032(2) 0.029(2) 0.0087(18) 0.009(2) 0.016(2) C36 0.054(3) 0.027(2) 0.057(3) 0.010(2) 0.004(3) 0.009(2) C37 0.041(3) 0.041(3) 0.072(4) 0.027(3) 0.006(3) 0.002(2) C38 0.032(3) 0.052(3) 0.063(3) 0.029(3) 0.016(2) 0.013(2) C33 0.031(2) 0.036(2) 0.036(2) 0.0127(19) 0.0098(19) 0.0150(19) C32 0.049(3) 0.056(3) 0.078(4) 0.019(3) 0.034(3) 0.033(3) C41 0.065(4) 0.077(5) 0.138(7) -0.007(5) 0.010(5) 0.029(4) Cl41 0.0827(12) 0.0538(10) 0.1243(16) -0.0042(10) 0.0318(12) 0.0121(9) Cl42 0.153(2) 0.0817(15) 0.134(2) 0.0103(14) 0.0617(18) 0.0119(15) _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 1.962(3) . ? Zn O1 1.972(3) . ? Zn O3 1.979(3) . ? Zn I 2.4834(14) . ? B H1 1.07(4) . ? B N31 1.542(6) . ? B N11 1.550(6) . ? B N21 1.553(6) . ? O1 C11 1.260(5) . ? O2 C21 1.267(5) . ? O3 C31 1.263(5) . ? N11 C11 1.362(5) . ? N11 C14 1.402(5) . ? N12 C11 1.357(5) . ? N12 C13 1.393(6) . ? N12 C12 1.446(6) . ? N21 C21 1.351(5) . ? N21 C24 1.407(5) . ? N22 C21 1.349(5) . ? N22 C23 1.381(6) . ? N22 C22 1.458(6) . ? N31 C31 1.354(5) . ? N31 C34 1.403(5) . ? N32 C31 1.357(5) . ? N32 C33 1.389(5) . ? N32 C32 1.451(6) . ? C14 C13 1.382(6) . ? C14 C15 1.386(6) . ? C15 C16 1.385(7) . ? C16 C17 1.365(8) . ? C17 C18 1.395(8) . ? C18 C13 1.390(6) . ? C24 C25 1.377(6) . ? C24 C23 1.386(6) . ? C25 C26 1.387(6) . ? C26 C27 1.390(7) . ? C27 C28 1.361(7) . ? C28 C23 1.384(6) . ? C34 C35 1.377(6) . ? C34 C33 1.384(6) . ? C35 C36 1.381(7) . ? C36 C37 1.394(8) . ? C37 C38 1.376(7) . ? C38 C33 1.387(6) . ? C41 Cl41 1.716(8) . ? C41 Cl42 1.808(9) . ? C51 Cl51 1.716(12) . ? C51 Cl52 1.816(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn O1 99.06(12) . . ? O2 Zn O3 99.54(14) . . ? O1 Zn O3 101.31(12) . . ? O2 Zn I 117.52(9) . . ? O1 Zn I 121.03(8) . . ? O3 Zn I 114.85(9) . . ? H1 B N31 108(2) . . ? H1 B N11 106(2) . . ? N31 B N11 112.3(3) . . ? H1 B N21 106(2) . . ? N31 B N21 110.8(3) . . ? N11 B N21 113.1(3) . . ? C11 O1 Zn 121.7(3) . . ? C21 O2 Zn 123.9(3) . . ? C31 O3 Zn 121.7(3) . . ? C11 N11 C14 106.9(3) . . ? C11 N11 B 130.0(3) . . ? C14 N11 B 122.5(3) . . ? C11 N12 C13 108.3(4) . . ? C11 N12 C12 125.2(4) . . ? C13 N12 C12 126.5(4) . . ? C21 N21 C24 107.1(3) . . ? C21 N21 B 129.9(3) . . ? C24 N21 B 122.8(3) . . ? C21 N22 C23 108.6(3) . . ? C21 N22 C22 125.1(4) . . ? C23 N22 C22 126.3(4) . . ? C31 N31 C34 107.3(3) . . ? C31 N31 B 129.5(3) . . ? C34 N31 B 123.1(3) . . ? C31 N32 C33 109.0(3) . . ? C31 N32 C32 124.3(4) . . ? C33 N32 C32 126.7(4) . . ? O1 C11 N12 122.6(4) . . ? O1 C11 N11 127.7(4) . . ? N12 C11 N11 109.7(4) . . ? C13 C14 C15 121.1(4) . . ? C13 C14 N11 108.2(4) . . ? C15 C14 N11 130.7(4) . . ? C16 C15 C14 116.6(5) . . ? C17 C16 C15 122.2(5) . . ? C16 C17 C18 122.2(5) . . ? C13 C18 C17 115.4(5) . . ? C14 C13 C18 122.5(5) . . ? C14 C13 N12 106.8(4) . . ? C18 C13 N12 130.7(5) . . ? O2 C21 N22 123.0(4) . . ? O2 C21 N21 127.0(4) . . ? N22 C21 N21 110.0(4) . . ? C25 C24 C23 120.9(4) . . ? C25 C24 N21 131.8(4) . . ? C23 C24 N21 107.3(4) . . ? C24 C25 C26 117.6(4) . . ? C25 C26 C27 121.0(5) . . ? C28 C27 C26 121.3(4) . . ? C27 C28 C23 117.9(5) . . ? N22 C23 C28 131.6(4) . . ? N22 C23 C24 107.1(4) . . ? C28 C23 C24 121.3(4) . . ? O3 C31 N31 127.2(4) . . ? O3 C31 N32 123.6(4) . . ? N31 C31 N32 109.2(4) . . ? C35 C34 C33 120.9(4) . . ? C35 C34 N31 131.0(4) . . ? C33 C34 N31 108.1(4) . . ? C34 C35 C36 118.0(5) . . ? C35 C36 C37 120.9(5) . . ? C38 C37 C36 121.3(5) . . ? C37 C38 C33 117.2(5) . . ? C34 C33 C38 121.7(4) . . ? C34 C33 N32 106.4(4) . . ? C38 C33 N32 131.9(4) . . ? Cl41 C41 Cl42 111.7(4) . . ? Cl51 C51 Cl52 111.6(11) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 30.15 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.376 _refine_diff_density_min -1.187 _refine_diff_density_rms 0.106 # Attachment '- zrtos10.cif' data_zrtos10 _database_code_depnum_ccdc_archive 'CCDC 794071' #TrackingRef '- zrtos10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H23 B Cl6 N6 O3 Zr' _chemical_formula_weight 770.22 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 15.611(3) _cell_length_b 12.966(3) _cell_length_c 15.764(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.384(4) _cell_angle_gamma 90.00 _cell_volume 3104.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 4760 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 23.68 _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.648 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 0.910 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9390 _exptl_absorpt_correction_T_max 0.9820 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 36423 _diffrn_reflns_av_R_equivalents 0.1740 _diffrn_reflns_av_sigmaI/netI 0.1243 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6363 _reflns_number_gt 3527 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+2.2020P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6363 _refine_ls_number_parameters 385 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1321 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1052 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Zr Zr 0.59197(3) 0.83647(4) 0.83260(3) 0.01906(13) Uani 1 1 d . . . B B 0.4109(4) 0.7522(5) 0.6178(4) 0.0192(13) Uani 1 1 d . . . H1 H 0.362(3) 0.734(4) 0.556(3) 0.040 Uiso 1 1 d . . . O1 O 0.5711(2) 0.6940(2) 0.7675(2) 0.0203(8) Uani 1 1 d . . . O2 O 0.5702(2) 0.8919(3) 0.7035(2) 0.0202(8) Uani 1 1 d . . . O3 O 0.4548(2) 0.8378(3) 0.8057(2) 0.0205(8) Uani 1 1 d . . . N11 N 0.4961(2) 0.6890(3) 0.6200(2) 0.0151(9) Uani 1 1 d . . . N12 N 0.6309(3) 0.6224(3) 0.6590(3) 0.0205(10) Uani 1 1 d . . . N21 N 0.4308(2) 0.8700(3) 0.6097(2) 0.0156(10) Uani 1 1 d . . . N22 N 0.4954(3) 1.0236(3) 0.6184(3) 0.0173(10) Uani 1 1 d . . . N31 N 0.3713(2) 0.7319(3) 0.6975(3) 0.0153(9) Uani 1 1 d . . . N32 N 0.3392(3) 0.7377(3) 0.8277(3) 0.0217(10) Uani 1 1 d . . . C11 C 0.5653(3) 0.6703(4) 0.6873(3) 0.0173(11) Uani 1 1 d . . . C12 C 0.6048(3) 0.6112(4) 0.5694(3) 0.0208(12) Uani 1 1 d . . . C13 C 0.6481(3) 0.5712(4) 0.5095(3) 0.0235(13) Uani 1 1 d . . . H13A H 0.7062 0.5447 0.5270 0.028 Uiso 1 1 calc R . . C14 C 0.6032(4) 0.5715(4) 0.4231(4) 0.0270(13) Uani 1 1 d . . . H14A H 0.6309 0.5456 0.3798 0.032 Uiso 1 1 calc R . . C15 C 0.5172(4) 0.6096(4) 0.3987(3) 0.0252(13) Uani 1 1 d . . . H15A H 0.4877 0.6079 0.3388 0.030 Uiso 1 1 calc R . . C16 C 0.4733(3) 0.6498(4) 0.4580(3) 0.0219(12) Uani 1 1 d . . . H16A H 0.4148 0.6753 0.4405 0.026 Uiso 1 1 calc R . . C17 C 0.5191(3) 0.6508(4) 0.5439(3) 0.0166(11) Uani 1 1 d . . . C18 C 0.7154(3) 0.5918(4) 0.7142(4) 0.0334(15) Uani 1 1 d . . . H18A H 0.7160 0.6071 0.7753 0.050 Uiso 1 1 calc R . . H18B H 0.7628 0.6300 0.6970 0.050 Uiso 1 1 calc R . . H18C H 0.7242 0.5176 0.7077 0.050 Uiso 1 1 calc R . . C21 C 0.5030(3) 0.9247(4) 0.6479(3) 0.0155(11) Uani 1 1 d . . . C22 C 0.4149(3) 1.0329(4) 0.5573(3) 0.0152(11) Uani 1 1 d . . . C23 C 0.3764(3) 1.1171(4) 0.5078(3) 0.0254(13) Uani 1 1 d . . . H23A H 0.4053 1.1819 0.5108 0.031 Uiso 1 1 calc R . . C24 C 0.2943(3) 1.1011(4) 0.4544(3) 0.0279(14) Uani 1 1 d . . . H24A H 0.2662 1.1560 0.4187 0.033 Uiso 1 1 calc R . . C25 C 0.2515(4) 1.0067(4) 0.4514(3) 0.0274(13) Uani 1 1 d . . . H25A H 0.1941 0.9993 0.4149 0.033 Uiso 1 1 calc R . . C26 C 0.2903(3) 0.9229(4) 0.5002(3) 0.0222(12) Uani 1 1 d . . . H26A H 0.2610 0.8584 0.4975 0.027 Uiso 1 1 calc R . . C27 C 0.3742(3) 0.9374(4) 0.5535(3) 0.0162(11) Uani 1 1 d . . . C28 C 0.5594(3) 1.1041(4) 0.6501(3) 0.0269(13) Uani 1 1 d . . . H28A H 0.6047 1.0777 0.6990 0.040 Uiso 1 1 calc R . . H28B H 0.5297 1.1632 0.6695 0.040 Uiso 1 1 calc R . . H28C H 0.5869 1.1258 0.6031 0.040 Uiso 1 1 calc R . . C31 C 0.3926(3) 0.7728(4) 0.7781(3) 0.0163(11) Uani 1 1 d . . . C32 C 0.2779(3) 0.6713(4) 0.7761(3) 0.0229(12) Uani 1 1 d . . . C33 C 0.2075(3) 0.6192(4) 0.7963(4) 0.0315(14) Uani 1 1 d . . . H33A H 0.1958 0.6217 0.8527 0.038 Uiso 1 1 calc R . . C34 C 0.1556(4) 0.5632(4) 0.7286(4) 0.0342(15) Uani 1 1 d . . . H34A H 0.1061 0.5266 0.7385 0.041 Uiso 1 1 calc R . . C35 C 0.1740(3) 0.5592(4) 0.6470(4) 0.0303(14) Uani 1 1 d . . . H35A H 0.1370 0.5193 0.6026 0.036 Uiso 1 1 calc R . . C36 C 0.2445(3) 0.6112(4) 0.6277(3) 0.0205(12) Uani 1 1 d . . . H36A H 0.2561 0.6087 0.5711 0.025 Uiso 1 1 calc R . . C37 C 0.2975(3) 0.6670(4) 0.6947(3) 0.0174(11) Uani 1 1 d . . . C38 C 0.3440(4) 0.7667(5) 0.9178(3) 0.0363(15) Uani 1 1 d . . . H38A H 0.3950 0.8116 0.9386 0.054 Uiso 1 1 calc R . . H38B H 0.3501 0.7045 0.9541 0.054 Uiso 1 1 calc R . . H38C H 0.2902 0.8034 0.9216 0.054 Uiso 1 1 calc R . . Cl1 Cl 0.74861(8) 0.82236(11) 0.83925(9) 0.0337(4) Uani 1 1 d . . . Cl2 Cl 0.59749(9) 1.01066(10) 0.88990(9) 0.0298(3) Uani 1 1 d . . . Cl3 Cl 0.59612(9) 0.74722(11) 0.96725(8) 0.0304(3) Uani 1 1 d . . . C40 C 0.5529(4) 0.6035(5) 1.1318(4) 0.0470(18) Uani 1 1 d . . . H40A H 0.5568 0.6095 1.0695 0.056 Uiso 1 1 calc R . . Cl41 Cl 0.50779(12) 0.48353(14) 1.14651(16) 0.0783(7) Uani 1 1 d . . . Cl42 Cl 0.48459(16) 0.70281(15) 1.15406(12) 0.0791(7) Uani 1 1 d . . . Cl43 Cl 0.65926(13) 0.61214(16) 1.19818(12) 0.0689(6) 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 Zr 0.0143(2) 0.0212(3) 0.0205(3) 0.0023(3) 0.0017(2) -0.0009(3) B 0.013(3) 0.025(4) 0.020(3) -0.003(3) 0.004(3) -0.001(3) O1 0.0231(19) 0.024(2) 0.0138(19) 0.0023(16) 0.0041(16) 0.0017(16) O2 0.0108(18) 0.024(2) 0.024(2) 0.0046(17) 0.0010(16) 0.0004(16) O3 0.0177(18) 0.0191(19) 0.0240(19) -0.0011(17) 0.0035(15) -0.0026(17) N11 0.016(2) 0.011(2) 0.019(2) 0.0027(18) 0.0045(19) 0.0002(17) N12 0.021(2) 0.018(2) 0.023(2) 0.003(2) 0.006(2) 0.0072(19) N21 0.013(2) 0.018(2) 0.016(2) 0.0040(18) 0.0040(18) 0.0018(18) N22 0.020(2) 0.016(2) 0.018(2) 0.0017(19) 0.0073(19) -0.0026(19) N31 0.015(2) 0.013(2) 0.018(2) -0.0021(19) 0.0059(19) -0.0013(18) N32 0.019(2) 0.030(3) 0.018(2) -0.001(2) 0.008(2) -0.005(2) C11 0.019(3) 0.010(3) 0.024(3) 0.001(2) 0.006(2) 0.000(2) C12 0.023(3) 0.021(3) 0.022(3) 0.003(2) 0.012(2) 0.002(2) C13 0.024(3) 0.024(3) 0.025(3) 0.005(3) 0.012(3) 0.008(2) C14 0.033(3) 0.029(3) 0.025(3) -0.002(3) 0.019(3) 0.006(3) C15 0.038(3) 0.019(3) 0.018(3) -0.003(2) 0.003(3) -0.006(3) C16 0.018(3) 0.020(3) 0.029(3) 0.000(3) 0.009(2) 0.000(2) C17 0.018(3) 0.012(3) 0.020(3) 0.001(2) 0.004(2) -0.002(2) C18 0.025(3) 0.041(4) 0.030(3) -0.002(3) -0.004(3) 0.018(3) C21 0.017(3) 0.020(3) 0.013(3) 0.003(2) 0.011(2) -0.001(2) C22 0.015(3) 0.020(3) 0.013(3) 0.002(2) 0.008(2) 0.002(2) C23 0.030(3) 0.021(3) 0.029(3) 0.009(3) 0.015(3) 0.007(3) C24 0.026(3) 0.031(3) 0.027(3) 0.010(3) 0.006(3) 0.012(3) C25 0.023(3) 0.036(4) 0.022(3) 0.005(3) 0.004(3) 0.007(3) C26 0.017(3) 0.028(3) 0.022(3) -0.001(3) 0.006(2) 0.003(2) C27 0.013(3) 0.022(3) 0.015(3) 0.000(2) 0.005(2) 0.002(2) C28 0.024(3) 0.020(3) 0.035(3) 0.002(3) 0.003(3) -0.002(2) C31 0.015(3) 0.015(3) 0.018(3) 0.005(2) 0.003(2) 0.002(2) C32 0.027(3) 0.021(3) 0.022(3) 0.001(3) 0.008(2) -0.001(3) C33 0.031(3) 0.040(4) 0.026(3) -0.001(3) 0.012(3) -0.014(3) C34 0.030(3) 0.040(4) 0.034(4) 0.000(3) 0.012(3) -0.017(3) C35 0.027(3) 0.025(3) 0.038(4) -0.006(3) 0.007(3) -0.006(3) C36 0.017(3) 0.023(3) 0.021(3) 0.001(2) 0.004(2) 0.003(2) C37 0.014(2) 0.015(3) 0.024(3) -0.002(3) 0.006(2) 0.000(2) C38 0.035(3) 0.050(4) 0.025(3) -0.004(3) 0.010(3) -0.007(3) Cl1 0.0148(7) 0.0368(9) 0.0469(9) 0.0062(8) 0.0017(6) 0.0006(6) Cl2 0.0287(8) 0.0260(8) 0.0347(8) -0.0059(7) 0.0076(7) -0.0043(6) Cl3 0.0336(8) 0.0342(8) 0.0225(7) 0.0060(7) 0.0043(6) -0.0010(7) C40 0.065(5) 0.033(4) 0.042(4) 0.008(3) 0.011(4) -0.013(3) Cl41 0.0455(11) 0.0416(11) 0.135(2) 0.0288(12) -0.0044(12) -0.0134(9) Cl42 0.127(2) 0.0626(13) 0.0520(12) 0.0092(10) 0.0287(13) 0.0295(13) Cl43 0.0701(13) 0.0713(14) 0.0611(13) -0.0009(11) 0.0063(11) -0.0334(11) _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 Zr O3 2.084(3) . ? Zr O1 2.102(3) . ? Zr O2 2.110(3) . ? Zr Cl3 2.4054(15) . ? Zr Cl2 2.4267(15) . ? Zr Cl1 2.4301(15) . ? B H1 1.11(5) . ? B N31 1.547(7) . ? B N11 1.555(7) . ? B N21 1.570(7) . ? O1 C11 1.283(5) . ? O2 C21 1.276(5) . ? O3 C31 1.283(5) . ? N11 C11 1.349(6) . ? N11 C17 1.419(6) . ? N12 C11 1.359(6) . ? N12 C12 1.384(6) . ? N12 C18 1.457(6) . ? N21 C21 1.349(6) . ? N21 C27 1.403(6) . ? N22 C21 1.360(6) . ? N22 C22 1.400(6) . ? N22 C28 1.451(6) . ? N31 C31 1.345(6) . ? N31 C37 1.418(6) . ? N32 C31 1.346(6) . ? N32 C32 1.400(6) . ? N32 C38 1.456(6) . ? C12 C13 1.384(7) . ? C12 C17 1.402(6) . ? C13 C14 1.380(7) . ? C14 C15 1.398(7) . ? C15 C16 1.383(7) . ? C16 C17 1.377(6) . ? C22 C27 1.387(6) . ? C22 C23 1.394(7) . ? C23 C24 1.377(7) . ? C24 C25 1.391(7) . ? C25 C26 1.387(7) . ? C26 C27 1.395(6) . ? C32 C33 1.388(7) . ? C32 C37 1.388(7) . ? C33 C34 1.387(7) . ? C34 C35 1.384(7) . ? C35 C36 1.383(7) . ? C36 C37 1.386(6) . ? C40 Cl41 1.745(6) . ? C40 Cl43 1.750(6) . ? C40 Cl42 1.758(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 O3 Zr O1 82.64(13) . . ? O3 Zr O2 82.68(12) . . ? O1 Zr O2 81.74(12) . . ? O3 Zr Cl3 90.01(10) . . ? O1 Zr Cl3 88.71(10) . . ? O2 Zr Cl3 168.62(10) . . ? O3 Zr Cl2 90.83(10) . . ? O1 Zr Cl2 171.12(10) . . ? O2 Zr Cl2 91.49(10) . . ? Cl3 Zr Cl2 97.35(5) . . ? O3 Zr Cl1 170.21(10) . . ? O1 Zr Cl1 89.75(10) . . ? O2 Zr Cl1 90.16(9) . . ? Cl3 Zr Cl1 95.99(5) . . ? Cl2 Zr Cl1 96.04(5) . . ? H1 B N31 111(3) . . ? H1 B N11 109(3) . . ? N31 B N11 113.1(4) . . ? H1 B N21 104(3) . . ? N31 B N21 110.7(4) . . ? N11 B N21 109.3(4) . . ? C11 O1 Zr 131.2(3) . . ? C21 O2 Zr 134.4(3) . . ? C31 O3 Zr 136.4(3) . . ? C11 N11 C17 106.8(4) . . ? C11 N11 B 129.6(4) . . ? C17 N11 B 123.1(4) . . ? C11 N12 C12 108.4(4) . . ? C11 N12 C18 125.1(4) . . ? C12 N12 C18 126.4(4) . . ? C21 N21 C27 107.0(4) . . ? C21 N21 B 129.5(4) . . ? C27 N21 B 123.4(4) . . ? C21 N22 C22 108.0(4) . . ? C21 N22 C28 124.3(4) . . ? C22 N22 C28 127.7(4) . . ? C31 N31 C37 106.6(4) . . ? C31 N31 B 130.0(4) . . ? C37 N31 B 123.4(4) . . ? C31 N32 C32 107.7(4) . . ? C31 N32 C38 125.5(4) . . ? C32 N32 C38 126.8(4) . . ? O1 C11 N11 126.3(4) . . ? O1 C11 N12 123.1(4) . . ? N11 C11 N12 110.6(4) . . ? C13 C12 N12 131.4(5) . . ? C13 C12 C17 121.7(5) . . ? N12 C12 C17 106.9(4) . . ? C14 C13 C12 117.1(5) . . ? C13 C14 C15 120.6(5) . . ? C16 C15 C14 122.8(5) . . ? C17 C16 C15 116.3(5) . . ? C16 C17 C12 121.5(5) . . ? C16 C17 N11 131.3(4) . . ? C12 C17 N11 107.2(4) . . ? O2 C21 N21 126.9(4) . . ? O2 C21 N22 122.8(4) . . ? N21 C21 N22 110.3(4) . . ? C27 C22 C23 122.7(5) . . ? C27 C22 N22 106.4(4) . . ? C23 C22 N22 130.9(5) . . ? C24 C23 C22 116.4(5) . . ? C23 C24 C25 121.7(5) . . ? C26 C25 C24 121.7(5) . . ? C25 C26 C27 117.2(5) . . ? C22 C27 C26 120.2(5) . . ? C22 C27 N21 108.3(4) . . ? C26 C27 N21 131.5(5) . . ? O3 C31 N31 125.5(4) . . ? O3 C31 N32 123.2(4) . . ? N31 C31 N32 111.3(4) . . ? C33 C32 C37 123.3(5) . . ? C33 C32 N32 129.6(5) . . ? C37 C32 N32 107.1(4) . . ? C34 C33 C32 115.6(5) . . ? C35 C34 C33 121.6(5) . . ? C36 C35 C34 122.3(5) . . ? C35 C36 C37 116.9(5) . . ? C36 C37 C32 120.3(4) . . ? C36 C37 N31 132.1(4) . . ? C32 C37 N31 107.4(4) . . ? Cl41 C40 Cl43 109.5(3) . . ? Cl41 C40 Cl42 110.2(4) . . ? Cl43 C40 Cl42 111.7(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.763 _refine_diff_density_min -1.008 _refine_diff_density_rms 0.118