# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1404 data_global #================================================================= # SUBMISSION DETAILS _publ_contact_author ; Dr. Michael Ward School of Chemistry University of Bristol Cantock's Close BS8 1TS Bristol UK ; _publ_contact_author_phone '0117 9287655' _publ_contact_author_fax '0117 9290509' _publ_contact_author_email mike.ward@bristol.ac.uk _publ_contact_letter ; This CIF file contains details of the four crystal structures in the paper 'Effects of metal coordination geometry on self-assembly: a monomeric complex with trigonal prismatic metal coordination vs. tetrameric complexes with octahedral metal coordination.' by Rowena L. Paul et al., submitted to Dalton Transactions for publication. ; #================================================================= data_beth _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C25 H21 B Cl2 Co F6 N9 P' _chemical_formula_weight 733.12 _chemical_melting_point ? _chemical_compound_source ? 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' 'F' 'F' 0.0171 0.0103 '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' '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 11.240(2) _cell_length_b 12.224(3) _cell_length_c 12.359(3) _cell_angle_alpha 62.36(2) _cell_angle_beta 77.69(2) _cell_angle_gamma 85.73(2) _cell_volume 1469.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour pink _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method ? _exptl_crystal_F_000 738 _exptl_absorpt_coefficient_mu 0.894 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.97 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12659 _diffrn_reflns_av_R_equivalents 0.0833 _diffrn_reflns_av_sigmaI/netI 0.1303 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5160 _reflns_number_observed 3050 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 32 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1066P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5128 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1372 _refine_ls_R_factor_obs 0.0737 _refine_ls_wR_factor_all 0.2078 _refine_ls_wR_factor_obs 0.1733 _refine_ls_goodness_of_fit_all 1.009 _refine_ls_goodness_of_fit_obs 1.130 _refine_ls_restrained_S_all 1.021 _refine_ls_restrained_S_obs 1.130 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.59037(8) 0.81763(8) -0.20061(8) 0.0182(3) Uani 1 d . . N11 N 0.5264(4) 0.8234(5) -0.0342(5) 0.0195(12) Uani 1 d . . N12 N 0.4091(5) 0.8330(5) 0.0159(5) 0.0211(12) Uani 1 d . . N21 N 0.7533(5) 0.8073(5) -0.1137(5) 0.0193(12) Uani 1 d . . N31 N 0.4536(5) 0.9419(5) -0.2513(5) 0.0239(13) Uani 1 d . . N32 N 0.3387(5) 0.9316(5) -0.1848(5) 0.0229(13) Uani 1 d . . N41 N 0.6673(5) 0.9780(5) -0.3905(5) 0.0218(13) Uani 1 d . . N51 N 0.4432(5) 0.6955(5) -0.1291(5) 0.0245(13) Uani 1 d . . N52 N 0.3327(5) 0.7039(5) -0.0635(5) 0.0231(13) Uani 1 d . . N61 N 0.6430(5) 0.6647(5) -0.2543(5) 0.0200(12) Uani 1 d . . C13 C 0.4060(6) 0.8488(5) 0.1176(6) 0.022(2) Uani 1 d . . H13A H 0.3350(6) 0.8587(5) 0.1694(6) 0.027 Uiso 1 calc R . C14 C 0.5240(6) 0.8480(6) 0.1330(6) 0.023(2) Uani 1 d . . H14A H 0.5502(6) 0.8571(6) 0.1966(6) 0.027 Uiso 1 calc R . C15 C 0.5969(6) 0.8309(5) 0.0355(6) 0.0183(14) Uani 1 d . . C22 C 0.7258(6) 0.8214(6) -0.0094(6) 0.0219(15) Uani 1 d . . C23 C 0.8150(6) 0.8223(6) 0.0532(7) 0.030(2) Uani 1 d . . H23A H 0.7937(6) 0.8323(6) 0.1267(7) 0.036 Uiso 1 calc R . C24 C 0.9367(6) 0.8082(7) 0.0056(7) 0.036(2) Uani 1 d . . H24A H 0.9994(6) 0.8111(7) 0.0451(7) 0.043 Uiso 1 calc R . C25 C 0.9646(6) 0.7902(7) -0.0981(7) 0.033(2) Uani 1 d . . H25A H 1.0462(6) 0.7781(7) -0.1307(7) 0.040 Uiso 1 calc R . C26 C 0.8716(6) 0.7901(6) -0.1537(6) 0.026(2) Uani 1 d . . H26A H 0.8914(6) 0.7769(6) -0.2253(6) 0.031 Uiso 1 calc R . C33 C 0.2758(6) 1.0287(6) -0.2568(7) 0.027(2) Uani 1 d . . H33A H 0.1925(6) 1.0436(6) -0.2334(7) 0.033 Uiso 1 calc R . C34 C 0.3506(6) 1.1010(6) -0.3672(7) 0.027(2) Uani 1 d . . H34A H 0.3312(6) 1.1748(6) -0.4342(7) 0.032 Uiso 1 calc R . C35 C 0.4626(6) 1.0421(6) -0.3599(6) 0.025(2) Uani 1 d . . C42 C 0.5863(6) 1.0653(6) -0.4393(6) 0.022(2) Uani 1 d . . C43 C 0.6181(7) 1.1673(6) -0.5524(6) 0.032(2) Uani 1 d . . H43A H 0.5588(7) 1.2272(6) -0.5835(6) 0.038 Uiso 1 calc R . C44 C 0.7338(7) 1.1842(7) -0.6210(7) 0.035(2) Uani 1 d . . H44A H 0.7559(7) 1.2544(7) -0.7000(7) 0.042 Uiso 1 calc R . C45 C 0.8182(7) 1.0955(6) -0.5716(6) 0.031(2) Uani 1 d . . H45A H 0.9000(7) 1.1034(6) -0.6156(6) 0.037 Uiso 1 calc R . C46 C 0.7800(6) 0.9966(6) -0.4580(6) 0.027(2) Uani 1 d . . H46A H 0.8383(6) 0.9364(6) -0.4246(6) 0.032 Uiso 1 calc R . C53 C 0.2659(6) 0.6006(6) -0.0274(6) 0.025(2) Uani 1 d . . H53A H 0.1853(6) 0.5825(6) 0.0208(6) 0.030 Uiso 1 calc R . C54 C 0.3343(6) 0.5259(6) -0.0721(6) 0.027(2) Uani 1 d . . H54A H 0.3107(6) 0.4481(6) -0.0620(6) 0.032 Uiso 1 calc R . C55 C 0.4450(6) 0.5895(5) -0.1351(6) 0.0186(14) Uani 1 d . . C62 C 0.5579(6) 0.5720(6) -0.2076(6) 0.0206(15) Uani 1 d . . C63 C 0.5785(6) 0.4705(6) -0.2303(6) 0.025(2) Uani 1 d . . H63A H 0.5178(6) 0.4067(6) -0.1961(6) 0.030 Uiso 1 calc R . C64 C 0.6874(7) 0.4622(6) -0.3027(7) 0.032(2) Uani 1 d . . H64A H 0.7023(7) 0.3937(6) -0.3197(7) 0.038 Uiso 1 calc R . C65 C 0.7746(7) 0.5564(6) -0.3500(7) 0.032(2) Uani 1 d . . H65A H 0.8507(7) 0.5535(6) -0.3998(7) 0.038 Uiso 1 calc R . C66 C 0.7482(6) 0.6541(6) -0.3231(6) 0.028(2) Uani 1 d . . H66A H 0.8085(6) 0.7180(6) -0.3555(6) 0.034 Uiso 1 calc R . B1 B 0.3107(8) 0.8246(7) -0.0511(7) 0.025(2) Uani 1 d . . H1 H 0.2262(8) 0.8273(7) -0.0061(7) 0.030 Uiso 1 calc R . C1 C 0.1320(10) 0.4913(10) -0.3203(10) 0.079(3) Uani 1 d . . H1A H 0.0936(10) 0.4151(10) -0.3084(10) 0.095 Uiso 1 calc R . H1B H 0.1177(10) 0.5593(10) -0.4003(10) 0.095 Uiso 1 calc R . Cl1 Cl 0.0594(3) 0.5256(3) -0.1971(3) 0.0913(10) Uani 1 d . . Cl2 Cl 0.2844(4) 0.4713(3) -0.3300(3) 0.1145(12) Uani 1 d . . P1 P 1.0439(2) -0.2097(2) 0.3556(2) 0.0362(5) Uani 1 d . . F1 F 1.1825(4) -0.1954(6) 0.3602(5) 0.070(2) Uani 1 d . . F2 F 0.9060(4) -0.2292(5) 0.3535(5) 0.066(2) Uani 1 d . . F3 F 1.0567(5) -0.3545(5) 0.4089(7) 0.086(2) Uani 1 d . . F4 F 1.0056(5) -0.2342(6) 0.4976(5) 0.078(2) Uani 1 d . . F5 F 1.0256(7) -0.0705(5) 0.3170(8) 0.132(3) Uani 1 d . . F6 F 1.0835(6) -0.1930(10) 0.2228(6) 0.161(4) Uani 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 Co1 0.0142(5) 0.0219(5) 0.0182(5) -0.0095(4) -0.0023(4) 0.0006(4) N11 0.010(3) 0.031(3) 0.021(3) -0.015(3) -0.003(2) 0.000(2) N12 0.015(3) 0.028(3) 0.020(3) -0.011(3) -0.005(2) 0.002(2) N21 0.014(3) 0.025(3) 0.019(3) -0.010(2) -0.001(2) -0.003(2) N31 0.020(3) 0.025(3) 0.025(3) -0.011(3) -0.004(3) 0.003(2) N32 0.016(3) 0.030(3) 0.021(3) -0.010(3) -0.002(2) 0.002(2) N41 0.025(3) 0.023(3) 0.018(3) -0.009(2) -0.006(3) -0.002(2) N51 0.017(3) 0.030(3) 0.026(3) -0.015(3) 0.000(3) 0.000(2) N52 0.015(3) 0.028(3) 0.026(3) -0.012(3) -0.003(3) -0.003(2) N61 0.017(3) 0.022(3) 0.020(3) -0.008(2) -0.004(2) 0.001(2) C13 0.028(4) 0.018(3) 0.022(4) -0.012(3) -0.003(3) 0.003(3) C14 0.025(4) 0.026(4) 0.015(3) -0.008(3) -0.003(3) -0.006(3) C15 0.016(4) 0.014(3) 0.022(4) -0.008(3) -0.002(3) 0.002(3) C22 0.022(4) 0.018(3) 0.024(4) -0.006(3) -0.008(3) -0.001(3) C23 0.024(4) 0.030(4) 0.032(4) -0.009(3) -0.007(3) 0.003(3) C24 0.021(4) 0.049(5) 0.043(5) -0.022(4) -0.013(4) -0.002(3) C25 0.015(4) 0.051(5) 0.034(4) -0.019(4) -0.007(3) 0.005(3) C26 0.027(4) 0.029(4) 0.020(4) -0.009(3) -0.005(3) -0.001(3) C33 0.019(4) 0.035(4) 0.038(4) -0.024(4) -0.015(3) 0.013(3) C34 0.029(4) 0.023(4) 0.031(4) -0.012(3) -0.020(4) 0.018(3) C35 0.027(4) 0.028(4) 0.021(4) -0.010(3) -0.011(3) 0.000(3) C42 0.034(4) 0.017(3) 0.015(3) -0.006(3) -0.007(3) -0.004(3) C43 0.044(5) 0.026(4) 0.025(4) -0.009(3) -0.011(4) -0.005(3) C44 0.048(5) 0.029(4) 0.018(4) -0.002(3) -0.002(4) -0.015(4) C45 0.030(4) 0.037(4) 0.019(4) -0.009(3) 0.003(3) -0.012(3) C46 0.024(4) 0.030(4) 0.025(4) -0.013(3) 0.000(3) -0.005(3) C53 0.013(4) 0.030(4) 0.025(4) -0.007(3) -0.001(3) -0.004(3) C54 0.025(4) 0.026(4) 0.033(4) -0.015(3) -0.011(3) -0.004(3) C55 0.017(4) 0.018(3) 0.021(4) -0.008(3) -0.007(3) 0.002(3) C62 0.023(4) 0.024(4) 0.012(3) -0.005(3) -0.006(3) 0.000(3) C63 0.021(4) 0.017(3) 0.028(4) -0.006(3) 0.001(3) -0.003(3) C64 0.040(5) 0.022(4) 0.037(4) -0.018(4) -0.006(4) 0.005(3) C65 0.030(4) 0.026(4) 0.034(4) -0.013(3) 0.002(4) 0.003(3) C66 0.024(4) 0.025(4) 0.031(4) -0.009(3) -0.002(3) -0.002(3) B1 0.022(4) 0.033(5) 0.019(4) -0.012(4) -0.001(4) 0.003(4) C1 0.091(9) 0.086(8) 0.077(8) -0.041(7) -0.048(7) 0.021(7) Cl1 0.079(2) 0.072(2) 0.111(2) -0.022(2) -0.037(2) -0.014(2) Cl2 0.123(3) 0.122(3) 0.104(3) -0.052(2) -0.034(2) 0.003(2) P1 0.0239(11) 0.0406(12) 0.0404(12) -0.0178(10) -0.0011(10) 0.0000(9) F1 0.025(3) 0.134(5) 0.084(4) -0.083(4) 0.009(3) -0.014(3) F2 0.030(3) 0.062(3) 0.102(4) -0.031(3) -0.029(3) 0.013(2) F3 0.070(4) 0.060(4) 0.156(6) -0.061(4) -0.058(4) 0.032(3) F4 0.060(4) 0.116(5) 0.067(4) -0.058(4) 0.018(3) -0.030(3) F5 0.118(6) 0.035(3) 0.223(9) -0.021(4) -0.087(6) 0.003(3) F6 0.089(5) 0.352(13) 0.056(4) -0.103(6) 0.019(4) -0.108(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 Co1 N31 2.060(5) . ? Co1 N11 2.061(5) . ? Co1 N51 2.066(6) . ? Co1 N61 2.259(5) . ? Co1 N21 2.281(5) . ? Co1 N41 2.284(5) . ? N11 C15 1.324(8) . ? N11 N12 1.354(7) . ? N12 C13 1.350(8) . ? N12 B1 1.551(9) . ? N21 C22 1.346(8) . ? N21 C26 1.353(8) . ? N31 C35 1.322(8) . ? N31 N32 1.355(7) . ? N32 C33 1.365(8) . ? N32 B1 1.541(9) . ? N41 C46 1.330(8) . ? N41 C42 1.351(8) . ? N51 C55 1.330(8) . ? N51 N52 1.356(7) . ? N52 C53 1.354(8) . ? N52 B1 1.549(9) . ? N61 C66 1.337(8) . ? N61 C62 1.361(8) . ? C13 C14 1.378(9) . ? C14 C15 1.398(8) . ? C15 C22 1.454(9) . ? C22 C23 1.395(9) . ? C23 C24 1.401(10) . ? C24 C25 1.368(10) . ? C25 C26 1.368(9) . ? C33 C34 1.361(10) . ? C34 C35 1.402(9) . ? C35 C42 1.482(9) . ? C42 C43 1.368(9) . ? C43 C44 1.363(10) . ? C44 C45 1.389(10) . ? C45 C46 1.365(9) . ? C53 C54 1.383(9) . ? C54 C55 1.389(9) . ? C55 C62 1.453(8) . ? C62 C63 1.388(9) . ? C63 C64 1.381(9) . ? C64 C65 1.388(10) . ? C65 C66 1.378(9) . ? C1 Cl2 1.699(11) . ? C1 Cl1 1.781(11) . ? P1 F6 1.524(6) . ? P1 F5 1.550(6) . ? P1 F3 1.583(5) . ? P1 F2 1.594(5) . ? P1 F1 1.596(5) . ? P1 F4 1.602(6) . ? 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 N31 Co1 N11 80.7(2) . . ? N31 Co1 N51 80.6(2) . . ? N11 Co1 N51 80.3(2) . . ? N31 Co1 N61 127.6(2) . . ? N11 Co1 N61 134.5(2) . . ? N51 Co1 N61 72.2(2) . . ? N31 Co1 N21 133.9(2) . . ? N11 Co1 N21 72.0(2) . . ? N51 Co1 N21 128.1(2) . . ? N61 Co1 N21 97.5(2) . . ? N31 Co1 N41 72.4(2) . . ? N11 Co1 N41 127.7(2) . . ? N51 Co1 N41 135.2(2) . . ? N61 Co1 N41 96.9(2) . . ? N21 Co1 N41 95.8(2) . . ? C15 N11 N12 108.4(5) . . ? C15 N11 Co1 124.3(4) . . ? N12 N11 Co1 126.9(4) . . ? C13 N12 N11 108.9(5) . . ? C13 N12 B1 134.3(6) . . ? N11 N12 B1 116.8(5) . . ? C22 N21 C26 117.1(5) . . ? C22 N21 Co1 114.3(4) . . ? C26 N21 Co1 128.5(4) . . ? C35 N31 N32 108.7(5) . . ? C35 N31 Co1 124.5(5) . . ? N32 N31 Co1 126.7(4) . . ? N31 N32 C33 107.3(5) . . ? N31 N32 B1 117.1(5) . . ? C33 N32 B1 135.4(6) . . ? C46 N41 C42 116.5(6) . . ? C46 N41 Co1 128.8(4) . . ? C42 N41 Co1 114.7(4) . . ? C55 N51 N52 108.3(5) . . ? C55 N51 Co1 124.1(4) . . ? N52 N51 Co1 127.4(4) . . ? C53 N52 N51 108.2(5) . . ? C53 N52 B1 135.7(6) . . ? N51 N52 B1 116.1(5) . . ? C66 N61 C62 117.3(6) . . ? C66 N61 Co1 127.5(4) . . ? C62 N61 Co1 115.2(4) . . ? N12 C13 C14 108.0(6) . . ? C13 C14 C15 105.6(6) . . ? N11 C15 C14 109.0(6) . . ? N11 C15 C22 113.4(6) . . ? C14 C15 C22 137.6(6) . . ? N21 C22 C23 122.0(6) . . ? N21 C22 C15 115.5(6) . . ? C23 C22 C15 122.5(6) . . ? C22 C23 C24 118.7(7) . . ? C25 C24 C23 119.5(7) . . ? C24 C25 C26 118.1(7) . . ? N21 C26 C25 124.6(6) . . ? C34 C33 N32 109.7(6) . . ? C33 C34 C35 104.6(6) . . ? N31 C35 C34 109.7(6) . . ? N31 C35 C42 113.5(6) . . ? C34 C35 C42 136.8(6) . . ? N41 C42 C43 121.9(7) . . ? N41 C42 C35 114.6(5) . . ? C43 C42 C35 123.5(6) . . ? C44 C43 C42 120.9(7) . . ? C43 C44 C45 117.9(6) . . ? C46 C45 C44 118.0(7) . . ? N41 C46 C45 124.9(7) . . ? N52 C53 C54 108.9(6) . . ? C53 C54 C55 104.8(6) . . ? N51 C55 C54 109.8(6) . . ? N51 C55 C62 113.5(6) . . ? C54 C55 C62 136.7(6) . . ? N61 C62 C63 121.7(6) . . ? N61 C62 C55 114.8(6) . . ? C63 C62 C55 123.5(6) . . ? C64 C63 C62 119.9(6) . . ? C63 C64 C65 118.5(6) . . ? C66 C65 C64 118.4(7) . . ? N61 C66 C65 124.2(7) . . ? N32 B1 N52 106.3(5) . . ? N32 B1 N12 106.7(6) . . ? N52 B1 N12 106.7(5) . . ? Cl2 C1 Cl1 114.0(6) . . ? F6 P1 F5 95.4(6) . . ? F6 P1 F3 90.3(5) . . ? F5 P1 F3 174.2(5) . . ? F6 P1 F2 90.2(3) . . ? F5 P1 F2 91.8(3) . . ? F3 P1 F2 87.4(3) . . ? F6 P1 F1 90.1(3) . . ? F5 P1 F1 90.2(4) . . ? F3 P1 F1 90.5(3) . . ? F2 P1 F1 178.0(3) . . ? F6 P1 F4 177.0(5) . . ? F5 P1 F4 87.5(4) . . ? F3 P1 F4 86.8(4) . . ? F2 P1 F4 90.7(3) . . ? F1 P1 F4 88.9(3) . . ? _refine_diff_density_max 0.765 _refine_diff_density_min -1.046 _refine_diff_density_rms 0.116 #=END data_bri6m _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C108 H98 B4 F24 Mn4 N40 O P4' _chemical_formula_weight 2815.14 _chemical_melting_point ? _chemical_compound_source ? 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' 'F' 'F' 0.0171 0.0103 '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' 'Mn' 'Mn' 0.3368 0.7283 '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 21.778(8) _cell_length_b 20.352(6) _cell_length_c 28.898(9) _cell_angle_alpha 90.00 _cell_angle_beta 103.83(3) _cell_angle_gamma 90.00 _cell_volume 12437.0(70) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.75 _exptl_crystal_size_min 0.60 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method ? _exptl_crystal_F_000 5720 _exptl_absorpt_coefficient_mu 0.550 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (XEMP)' _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 0.73 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42954 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 23.26 _reflns_number_total 17194 _reflns_number_observed 13399 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 fullcycle _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+22.4812P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17194 _refine_ls_number_parameters 1673 _refine_ls_number_restraints 46 _refine_ls_R_factor_all 0.0857 _refine_ls_R_factor_obs 0.0643 _refine_ls_wR_factor_all 0.1690 _refine_ls_wR_factor_obs 0.1529 _refine_ls_goodness_of_fit_all 1.092 _refine_ls_goodness_of_fit_obs 1.135 _refine_ls_restrained_S_all 1.097 _refine_ls_restrained_S_obs 1.140 _refine_ls_shift/esd_max 3.631 _refine_ls_shift/esd_mean 0.155 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mn1 Mn 0.29411(3) 0.05651(3) 0.13379(2) 0.0445(2) Uani 1 d . . Mn2 Mn 0.39460(3) 0.27577(3) 0.02141(2) 0.0421(2) Uani 1 d . . Mn3 Mn 0.10630(3) 0.24937(3) 0.00132(3) 0.0461(2) Uani 1 d . . Mn4 Mn 0.24894(3) 0.03162(3) -0.08515(3) 0.0455(2) Uani 1 d . . B1 B 0.2697(3) 0.2353(3) 0.0895(2) 0.0422(12) Uani 1 d . . H1 H 0.2661(3) 0.2053(3) 0.0625(2) 0.063 Uiso 1 calc R . N111 N 0.3424(2) 0.1535(2) 0.14364(13) 0.0422(9) Uani 1 d . . N112 N 0.3261(2) 0.2174(2) 0.13083(13) 0.0424(9) Uani 1 d . . C113 C 0.3658(2) 0.2579(2) 0.1608(2) 0.0498(12) Uani 1 d . . H113 H 0.3644(2) 0.3036(2) 0.1594(2) 0.075 Uiso 1 calc R . C114 C 0.4081(2) 0.2224(2) 0.1931(2) 0.0529(13) Uani 1 d . . H114 H 0.4406(2) 0.2382(2) 0.2177(2) 0.079 Uiso 1 calc R . C115 C 0.3923(2) 0.1572(2) 0.1816(2) 0.0455(11) Uani 1 d . . C116 C 0.4229(2) 0.0965(2) 0.2024(2) 0.0516(12) Uani 1 d . . C117 C 0.4805(3) 0.0972(3) 0.2357(2) 0.067(2) Uani 1 d . . H117 H 0.5002(3) 0.1367(3) 0.2465(2) 0.100 Uiso 1 calc R . C118 C 0.5078(3) 0.0378(3) 0.2525(2) 0.084(2) Uani 1 d . . H118 H 0.5465(3) 0.0369(3) 0.2747(2) 0.127 Uiso 1 calc R . C119 C 0.4777(3) -0.0196(3) 0.2362(2) 0.079(2) Uani 1 d . . H119 H 0.4958(3) -0.0599(3) 0.2467(2) 0.119 Uiso 1 calc R . C120 C 0.4208(3) -0.0165(3) 0.2042(2) 0.0634(15) Uani 1 d . . H120 H 0.4002(3) -0.0557(3) 0.1939(2) 0.095 Uiso 1 calc R . N121 N 0.3926(2) 0.0401(2) 0.18647(14) 0.0534(10) Uani 1 d . . N131 N 0.3167(2) 0.3241(2) 0.04620(13) 0.0414(9) Uani 1 d . . N132 N 0.2788(2) 0.3075(2) 0.07518(13) 0.0413(9) Uani 1 d . . C133 C 0.2532(2) 0.3619(2) 0.0894(2) 0.0521(12) Uani 1 d . . H133 H 0.2253(2) 0.3628(2) 0.1092(2) 0.078 Uiso 1 calc R . C134 C 0.2751(2) 0.4161(2) 0.0695(2) 0.0547(13) Uani 1 d . . H134 H 0.2658(2) 0.4601(2) 0.0733(2) 0.082 Uiso 1 calc R . C135 C 0.3143(2) 0.3898(2) 0.0426(2) 0.0467(12) Uani 1 d . . C136 C 0.3500(2) 0.4237(2) 0.0132(2) 0.0530(13) Uani 1 d . . C137 C 0.3454(3) 0.4913(3) 0.0056(2) 0.079(2) Uani 1 d . . H137 H 0.3184(3) 0.5166(3) 0.0189(2) 0.119 Uiso 1 calc R . C138 C 0.3812(4) 0.5197(3) -0.0217(3) 0.106(3) Uani 1 d . . H138 H 0.3791(4) 0.5648(3) -0.0268(3) 0.159 Uiso 1 calc R . C139 C 0.4204(4) 0.4819(3) -0.0417(3) 0.098(2) Uani 1 d . . H139 H 0.4447(4) 0.5006(3) -0.0607(3) 0.147 Uiso 1 calc R . C140 C 0.4224(3) 0.4155(3) -0.0327(2) 0.070(2) Uani 1 d . . H140 H 0.4487(3) 0.3895(3) -0.0462(2) 0.105 Uiso 1 calc R . N141 N 0.3886(2) 0.3864(2) -0.00576(14) 0.0526(10) Uani 1 d . . N151 N 0.1505(2) 0.2326(2) 0.07928(13) 0.0451(9) Uani 1 d . . N152 N 0.2096(2) 0.2344(2) 0.10893(13) 0.0446(9) Uani 1 d . . C153 C 0.2048(3) 0.2414(2) 0.1544(2) 0.0508(12) Uani 1 d . . H153 H 0.2387(3) 0.2438(2) 0.1809(2) 0.076 Uiso 1 calc R . C154 C 0.1426(3) 0.2445(2) 0.1552(2) 0.0532(13) Uani 1 d . . H154 H 0.1257(3) 0.2497(2) 0.1816(2) 0.080 Uiso 1 calc R . C155 C 0.1102(2) 0.2380(2) 0.1080(2) 0.0486(12) Uani 1 d . . C156 C 0.0417(2) 0.2358(2) 0.0868(2) 0.0547(13) Uani 1 d . . C157 C -0.0010(3) 0.2347(3) 0.1151(2) 0.080(2) Uani 1 d . . H157 H 0.0128(3) 0.2341(3) 0.1482(2) 0.120 Uiso 1 calc R . C158 C -0.0648(3) 0.2347(4) 0.0935(3) 0.098(2) Uani 1 d . . H158 H -0.0946(3) 0.2339(4) 0.1118(3) 0.147 Uiso 1 calc R . C159 C -0.0834(3) 0.2359(4) 0.0448(3) 0.091(2) Uani 1 d . . H159 H -0.1261(3) 0.2368(4) 0.0295(3) 0.137 Uiso 1 calc R . C160 C -0.0388(3) 0.2357(3) 0.0187(2) 0.075(2) Uani 1 d . . H160 H -0.0520(3) 0.2358(3) -0.0143(2) 0.112 Uiso 1 calc R . N161 N 0.0240(2) 0.2354(2) 0.0391(2) 0.0574(11) Uani 1 d . . B2 B 0.2378(3) 0.2170(3) -0.0639(2) 0.0431(13) Uani 1 d . . H2 H 0.2455(3) 0.1929(3) -0.0337(2) 0.065 Uiso 1 calc R . N211 N 0.3560(2) 0.2373(2) -0.05312(13) 0.0416(9) Uani 1 d . . N212 N 0.2988(2) 0.2221(2) -0.08238(13) 0.0421(9) Uani 1 d . . C213 C 0.3047(2) 0.2169(2) -0.1276(2) 0.0516(12) Uani 1 d . . H213 H 0.2721(2) 0.2071(2) -0.1540(2) 0.077 Uiso 1 calc R . C214 C 0.3660(2) 0.2283(2) -0.1285(2) 0.0535(13) Uani 1 d . . H214 H 0.3835(2) 0.2278(2) -0.1548(2) 0.080 Uiso 1 calc R . C215 C 0.3965(2) 0.2409(2) -0.0813(2) 0.0440(11) Uani 1 d . . C216 C 0.4632(2) 0.2561(2) -0.0609(2) 0.0452(11) Uani 1 d . . C217 C 0.5063(3) 0.2591(3) -0.0893(2) 0.0593(14) Uani 1 d . . H217 H 0.4937(3) 0.2500(3) -0.1217(2) 0.089 Uiso 1 calc R . C218 C 0.5679(3) 0.2756(3) -0.0686(2) 0.067(2) Uani 1 d . . H218 H 0.5973(3) 0.2787(3) -0.0871(2) 0.100 Uiso 1 calc R . C219 C 0.5858(2) 0.2875(3) -0.0207(2) 0.0645(15) Uani 1 d . . H219 H 0.6274(2) 0.2985(3) -0.0062(2) 0.097 Uiso 1 calc R . C220 C 0.5409(2) 0.2828(3) 0.0055(2) 0.0645(15) Uani 1 d . . H220 H 0.5533(2) 0.2901(3) 0.0382(2) 0.097 Uiso 1 calc R . N221 N 0.4796(2) 0.2680(2) -0.01399(14) 0.0496(10) Uani 1 d . . N231 N 0.1763(2) 0.3034(2) -0.02962(13) 0.0444(9) Uani 1 d . . N232 N 0.2155(2) 0.2878(2) -0.05813(13) 0.0438(9) Uani 1 d . . C233 C 0.2303(2) 0.3433(2) -0.0792(2) 0.0566(13) Uani 1 d . . H233 H 0.2564(2) 0.3455(2) -0.1004(2) 0.085 Uiso 1 calc R . C234 C 0.2006(3) 0.3952(3) -0.0643(2) 0.0644(15) Uani 1 d . . H234 H 0.2022(3) 0.4390(3) -0.0730(2) 0.097 Uiso 1 calc R . C235 C 0.1676(2) 0.3689(2) -0.0333(2) 0.0493(12) Uani 1 d . . C236 C 0.1292(2) 0.4015(2) -0.0050(2) 0.0517(12) Uani 1 d . . C237 C 0.1294(3) 0.4696(3) 0.0005(2) 0.070(2) Uani 1 d . . H237 H 0.1539(3) 0.4960(3) -0.0142(2) 0.105 Uiso 1 calc R . C238 C 0.0929(3) 0.4971(3) 0.0281(2) 0.079(2) Uani 1 d . . H238 H 0.0925(3) 0.5424(3) 0.0323(2) 0.118 Uiso 1 calc R . C239 C 0.0569(3) 0.4570(3) 0.0493(2) 0.078(2) Uani 1 d . . H239 H 0.0318(3) 0.4747(3) 0.0681(2) 0.117 Uiso 1 calc R . C240 C 0.0588(3) 0.3904(3) 0.0422(2) 0.069(2) Uani 1 d . . H240 H 0.0341(3) 0.3635(3) 0.0565(2) 0.103 Uiso 1 calc R . N241 N 0.0942(2) 0.3620(2) 0.01559(15) 0.0541(11) Uani 1 d . . N251 N 0.1839(2) 0.1158(2) -0.10707(13) 0.0466(10) Uani 1 d . . N252 N 0.1869(2) 0.1828(2) -0.10259(13) 0.0455(9) Uani 1 d . . C253 C 0.1405(2) 0.2100(3) -0.1369(2) 0.0556(13) Uani 1 d . . H253 H 0.1330(2) 0.2548(3) -0.1414(2) 0.083 Uiso 1 calc R . C254 C 0.1067(3) 0.1616(3) -0.1639(2) 0.0595(14) Uani 1 d . . H254 H 0.0724(3) 0.1664(3) -0.1900(2) 0.089 Uiso 1 calc R . C255 C 0.1343(2) 0.1035(2) -0.1443(2) 0.0497(12) Uani 1 d . . C256 C 0.1165(2) 0.0351(3) -0.1577(2) 0.0542(13) Uani 1 d . . C257 C 0.0618(3) 0.0189(3) -0.1904(2) 0.074(2) Uani 1 d . . H257 H 0.0342(3) 0.0516(3) -0.2051(2) 0.111 Uiso 1 calc R . C258 C 0.0481(3) -0.0461(3) -0.2013(2) 0.090(2) Uani 1 d . . H258 H 0.0112(3) -0.0577(3) -0.2234(2) 0.135 Uiso 1 calc R . C259 C 0.0889(3) -0.0930(3) -0.1797(2) 0.085(2) Uani 1 d . . H259 H 0.0802(3) -0.1371(3) -0.1865(2) 0.127 Uiso 1 calc R . C260 C 0.1436(3) -0.0743(3) -0.1473(2) 0.076(2) Uani 1 d . . H260 H 0.1718(3) -0.1068(3) -0.1330(2) 0.113 Uiso 1 calc R . N261 N 0.1578(2) -0.0113(2) -0.1356(2) 0.0588(11) Uani 1 d . . B3 B 0.1652(3) 0.0708(3) 0.0169(2) 0.0454(13) Uani 1 d . . H3 H 0.1995(3) 0.1019(3) 0.0167(2) 0.068 Uiso 1 calc R . N311 N 0.0874(2) 0.1501(2) -0.03355(13) 0.0461(9) Uani 1 d . . N312 N 0.1062(2) 0.0868(2) -0.02249(14) 0.0468(10) Uani 1 d . . C313 C 0.0654(3) 0.0454(3) -0.0510(2) 0.0597(14) Uani 1 d . . H313 H 0.0681(3) -0.0002(3) -0.0501(2) 0.090 Uiso 1 calc R . C314 C 0.0198(3) 0.0808(3) -0.0813(2) 0.0615(14) Uani 1 d . . H314 H -0.0139(3) 0.0649(3) -0.1048(2) 0.092 Uiso 1 calc R . C315 C 0.0348(2) 0.1462(3) -0.0694(2) 0.0530(13) Uani 1 d . . C316 C 0.0050(2) 0.2066(3) -0.0912(2) 0.0569(13) Uani 1 d . . C317 C -0.0435(3) 0.2060(3) -0.1322(2) 0.085(2) Uani 1 d . . H317 H -0.0596(3) 0.1665(3) -0.1462(2) 0.128 Uiso 1 calc R . C318 C -0.0674(4) 0.2654(4) -0.1517(3) 0.111(3) Uani 1 d . . H318 H -0.0997(4) 0.2663(4) -0.1794(3) 0.166 Uiso 1 calc R . C319 C -0.0436(4) 0.3224(4) -0.1304(3) 0.107(3) Uani 1 d . . H319 H -0.0593(4) 0.3627(4) -0.1432(3) 0.161 Uiso 1 calc R . C320 C 0.0042(3) 0.3195(3) -0.0895(2) 0.084(2) Uani 1 d . . H320 H 0.0200(3) 0.3587(3) -0.0749(2) 0.126 Uiso 1 calc R . N321 N 0.0290(2) 0.2630(2) -0.0697(2) 0.0596(11) Uani 1 d . . N331 N 0.2198(2) -0.0164(2) -0.02272(13) 0.0431(9) Uani 1 d . . N332 N 0.1855(2) -0.0006(2) 0.00939(14) 0.0460(9) Uani 1 d . . C333 C 0.1720(2) -0.0563(2) 0.0309(2) 0.0547(13) Uani 1 d . . H333 H 0.1485(2) -0.0585(2) 0.0538(2) 0.082 Uiso 1 calc R . C334 C 0.1986(2) -0.1089(2) 0.0132(2) 0.0556(13) Uani 1 d . . H334 H 0.1972(2) -0.1528(2) 0.0217(2) 0.083 Uiso 1 calc R . C335 C 0.2278(2) -0.0823(2) -0.0199(2) 0.0457(11) Uani 1 d . . C336 C 0.2641(2) -0.1144(2) -0.0502(2) 0.0490(12) Uani 1 d . . C337 C 0.2745(3) -0.1819(2) -0.0481(2) 0.0638(15) Uani 1 d . . H337 H 0.2597(3) -0.2077(2) -0.0265(2) 0.096 Uiso 1 calc R . C338 C 0.3069(3) -0.2097(3) -0.0783(2) 0.074(2) Uani 1 d . . H338 H 0.3143(3) -0.2547(3) -0.0774(2) 0.112 Uiso 1 calc R . C339 C 0.3283(3) -0.1709(3) -0.1098(2) 0.078(2) Uani 1 d . . H339 H 0.3500(3) -0.1892(3) -0.1307(2) 0.117 Uiso 1 calc R . C340 C 0.3170(3) -0.1038(3) -0.1100(2) 0.067(2) Uani 1 d . . H340 H 0.3322(3) -0.0774(3) -0.1310(2) 0.100 Uiso 1 calc R . N341 N 0.2852(2) -0.0759(2) -0.08084(15) 0.0525(10) Uani 1 d . . N351 N 0.1899(2) 0.0768(2) 0.10756(13) 0.0434(9) Uani 1 d . . N352 N 0.1462(2) 0.0720(2) 0.06544(14) 0.0457(9) Uani 1 d . . C353 C 0.0878(2) 0.0702(3) 0.0739(2) 0.0590(14) Uani 1 d . . H353 H 0.0500(2) 0.0669(3) 0.0508(2) 0.088 Uiso 1 calc R . C354 C 0.0932(2) 0.0738(3) 0.1216(2) 0.0610(14) Uani 1 d . . H354 H 0.0607(2) 0.0734(3) 0.1374(2) 0.092 Uiso 1 calc R . C355 C 0.1575(2) 0.0783(2) 0.1418(2) 0.0498(12) Uani 1 d . . C356 C 0.1920(3) 0.0889(2) 0.1913(2) 0.0514(12) Uani 1 d . . C357 C 0.1616(3) 0.1095(3) 0.2260(2) 0.065(2) Uani 1 d . . H357 H 0.1178(3) 0.1140(3) 0.2189(2) 0.098 Uiso 1 calc R . C358 C 0.1975(4) 0.1232(3) 0.2710(2) 0.077(2) Uani 1 d . . H358 H 0.1784(4) 0.1381(3) 0.2945(2) 0.116 Uiso 1 calc R . C359 C 0.2615(4) 0.1145(3) 0.2808(2) 0.082(2) Uani 1 d . . H359 H 0.2864(4) 0.1232(3) 0.3111(2) 0.123 Uiso 1 calc R . C360 C 0.2887(3) 0.0929(3) 0.2453(2) 0.071(2) Uani 1 d . . H360 H 0.3322(3) 0.0867(3) 0.2523(2) 0.106 Uiso 1 calc R . N361 N 0.2546(2) 0.0804(2) 0.20068(15) 0.0553(11) Uani 1 d . . B4 B 0.3689(2) 0.0881(3) 0.0272(2) 0.0406(12) Uani 1 d . . H4 H 0.3291(2) 0.1125(3) 0.0232(2) 0.061 Uiso 1 calc R . N411 N 0.3488(2) 0.0701(2) -0.06182(13) 0.0430(9) Uani 1 d . . N412 N 0.3901(2) 0.0838(2) -0.01964(13) 0.0421(9) Uani 1 d . . C413 C 0.4483(2) 0.0910(2) -0.0272(2) 0.0492(12) Uani 1 d . . H413 H 0.4846(2) 0.1008(2) -0.0038(2) 0.074 Uiso 1 calc R . C414 C 0.4462(2) 0.0817(3) -0.0741(2) 0.0534(13) Uani 1 d . . H414 H 0.4796(2) 0.0833(3) -0.0889(2) 0.080 Uiso 1 calc R . C415 C 0.3827(2) 0.0691(2) -0.0949(2) 0.0468(12) Uani 1 d . . C416 C 0.3505(2) 0.0589(2) -0.1447(2) 0.0524(12) Uani 1 d . . C417 C 0.3813(3) 0.0656(3) -0.1814(2) 0.075(2) Uani 1 d . . H417 H 0.4242(3) 0.0756(3) -0.1746(2) 0.113 Uiso 1 calc R . C418 C 0.3481(4) 0.0572(4) -0.2274(2) 0.093(2) Uani 1 d . . H418 H 0.3683(4) 0.0611(4) -0.2522(2) 0.140 Uiso 1 calc R . C419 C 0.2848(4) 0.0431(4) -0.2369(2) 0.089(2) Uani 1 d . . H419 H 0.2612(4) 0.0379(4) -0.2680(2) 0.133 Uiso 1 calc R . C420 C 0.2570(3) 0.0367(3) -0.1987(2) 0.072(2) Uani 1 d . . H420 H 0.2143(3) 0.0262(3) -0.2050(2) 0.108 Uiso 1 calc R . N421 N 0.2887(2) 0.0447(2) -0.15333(14) 0.0547(11) Uani 1 d . . N431 N 0.3308(2) 0.0023(2) 0.07782(13) 0.0405(9) Uani 1 d . . N432 N 0.3622(2) 0.0167(2) 0.04386(13) 0.0411(9) Uani 1 d . . C433 C 0.3877(2) -0.0390(2) 0.0306(2) 0.0468(12) Uani 1 d . . H433 H 0.4116(2) -0.0417(2) 0.0080(2) 0.070 Uiso 1 calc R . C434 C 0.3724(2) -0.0904(2) 0.0561(2) 0.0518(12) Uani 1 d . . H434 H 0.3837(2) -0.1343(2) 0.0545(2) 0.078 Uiso 1 calc R . C435 C 0.3365(2) -0.0630(2) 0.0848(2) 0.0461(11) Uani 1 d . . C436 C 0.3048(2) -0.0947(2) 0.1183(2) 0.0489(12) Uani 1 d . . C437 C 0.3031(3) -0.1619(2) 0.1237(2) 0.067(2) Uani 1 d . . H437 H 0.3240(3) -0.1892(2) 0.1067(2) 0.101 Uiso 1 calc R . C438 C 0.2704(4) -0.1880(3) 0.1540(3) 0.089(2) Uani 1 d . . H438 H 0.2684(4) -0.2333(3) 0.1576(3) 0.133 Uiso 1 calc R . C439 C 0.2406(4) -0.1470(3) 0.1791(3) 0.093(2) Uani 1 d . . H439 H 0.2186(4) -0.1637(3) 0.2004(3) 0.139 Uiso 1 calc R . C440 C 0.2439(3) -0.0795(3) 0.1719(2) 0.073(2) Uani 1 d . . H440 H 0.2227(3) -0.0514(3) 0.1883(2) 0.110 Uiso 1 calc R . N441 N 0.2760(2) -0.0537(2) 0.14278(15) 0.0531(10) Uani 1 d . . N451 N 0.4298(2) 0.1875(2) 0.06739(12) 0.0402(9) Uani 1 d . . N452 N 0.4227(2) 0.1208(2) 0.06441(13) 0.0406(9) Uani 1 d . . C453 C 0.4692(2) 0.0921(2) 0.0970(2) 0.0501(12) Uani 1 d . . H453 H 0.4745(2) 0.0471(2) 0.1016(2) 0.075 Uiso 1 calc R . C454 C 0.5076(2) 0.1393(2) 0.1224(2) 0.0518(12) Uani 1 d . . H454 H 0.5435(2) 0.1332(2) 0.1470(2) 0.078 Uiso 1 calc R . C455 C 0.4813(2) 0.1984(2) 0.1033(2) 0.0449(11) Uani 1 d . . C456 C 0.4991(2) 0.2661(2) 0.1176(2) 0.0479(12) Uani 1 d . . C457 C 0.5457(3) 0.2797(3) 0.1582(2) 0.066(2) Uani 1 d . . H457 H 0.5676(3) 0.2458(3) 0.1766(2) 0.100 Uiso 1 calc R . C458 C 0.5589(3) 0.3447(3) 0.1708(2) 0.083(2) Uani 1 d . . H458 H 0.5901(3) 0.3552(3) 0.1979(2) 0.124 Uiso 1 calc R . C459 C 0.5255(3) 0.3937(3) 0.1428(2) 0.082(2) Uani 1 d . . H459 H 0.5330(3) 0.4377(3) 0.1509(2) 0.122 Uiso 1 calc R . C460 C 0.4811(3) 0.3763(3) 0.1030(2) 0.0647(15) Uani 1 d . . H460 H 0.4590(3) 0.4096(3) 0.0841(2) 0.097 Uiso 1 calc R . N461 N 0.4671(2) 0.3137(2) 0.08927(14) 0.0492(10) Uani 1 d . . P1 P 0.47444(10) 0.76336(10) 0.22912(6) 0.0858(5) Uani 1 d . . F11 F 0.5272(3) 0.7300(4) 0.2120(2) 0.210(3) Uani 1 d . . F12 F 0.4659(4) 0.7060(3) 0.2612(2) 0.200(3) Uani 1 d . . F13 F 0.4238(4) 0.7997(5) 0.2459(3) 0.242(4) Uani 1 d . . F14 F 0.5202(4) 0.7929(5) 0.2710(2) 0.255(4) Uani 1 d . . F15 F 0.4285(3) 0.7332(3) 0.1853(2) 0.171(2) Uani 1 d . . F16 F 0.4802(5) 0.8204(3) 0.1970(3) 0.252(5) Uani 1 d . . P2 P 0.38426(8) 0.41658(8) 0.24291(6) 0.0716(4) Uani 1 d . . F21 F 0.3739(2) 0.4107(2) 0.18715(13) 0.1121(14) Uani 1 d . . F22 F 0.3469(2) 0.3501(2) 0.2439(2) 0.1135(14) Uani 1 d . . F23 F 0.3951(2) 0.4232(2) 0.29888(14) 0.125(2) Uani 1 d . . F24 F 0.4221(2) 0.4827(2) 0.24227(15) 0.1043(13) Uani 1 d . . F25 F 0.3210(2) 0.4563(2) 0.2369(2) 0.1176(15) Uani 1 d . . F26 F 0.4472(2) 0.3757(2) 0.2500(2) 0.123(2) Uani 1 d . . P3 P 0.67267(9) 0.15080(11) 0.26109(7) 0.0871(5) Uani 1 d . . F31 F 0.6146(2) 0.1758(3) 0.2785(2) 0.186(3) Uani 1 d . . F32 F 0.7306(2) 0.1266(3) 0.2418(2) 0.133(2) Uani 1 d . . F33 F 0.6748(3) 0.0873(3) 0.2906(2) 0.172(2) Uani 1 d . . F34 F 0.6712(3) 0.2140(3) 0.2291(2) 0.176(2) Uani 1 d . . F35 F 0.6264(2) 0.1159(3) 0.2178(2) 0.144(2) Uani 1 d . . F36 F 0.7180(2) 0.1871(3) 0.3032(2) 0.137(2) Uani 1 d . . P4 P 0.22711(9) 0.65574(8) 0.05335(8) 0.0844(5) Uani 1 d . . F41 F 0.2393(3) 0.5829(2) 0.0614(3) 0.222(4) Uani 1 d . . F42 F 0.2697(7) 0.6517(6) 0.0219(5) 0.425(11) Uani 1 d . . F43 F 0.2173(4) 0.7279(2) 0.0430(3) 0.247(5) Uani 1 d . . F44 F 0.1904(5) 0.6574(5) 0.0874(3) 0.279(5) Uani 1 d . . F45 F 0.2836(3) 0.6764(3) 0.0943(3) 0.219(4) Uani 1 d . . F46 F 0.1697(4) 0.6368(3) 0.0148(3) 0.226(4) Uani 1 d . . C1 C 0.3427(8) -0.0831(6) 0.3053(5) 0.236(8) Uani 1 d . . H1A H 0.3325(60) -0.0818(34) 0.2711(5) 0.354 Uiso 1 calc R . H1B H 0.3044(33) -0.0855(37) 0.3162(42) 0.354 Uiso 1 calc R . H1C H 0.3683(27) -0.1211(7) 0.3161(42) 0.354 Uiso 1 calc R . C2 C 0.3761(7) -0.0264(7) 0.3234(4) 0.150(4) Uani 1 d . . N1 N 0.4062(7) 0.0175(6) 0.3361(4) 0.210(5) Uani 1 d . . C3 C 0.6264(6) 0.6120(6) 0.1822(5) 0.231(8) Uani 1 d . . H3A H 0.6527(52) 0.6208(16) 0.1605(39) 0.347 Uiso 1 calc R . H3B H 0.6399(63) 0.6387(6) 0.2101(7) 0.347 Uiso 1 calc R . H3C H 0.5832(13) 0.6222(18) 0.1670(46) 0.347 Uiso 1 calc R . C4 C 0.6311(5) 0.5481(6) 0.1946(5) 0.157(5) Uani 1 d . . N2 N 0.6355(5) 0.4937(5) 0.2048(5) 0.219(6) Uani 1 d . . C5 C 0.1784(7) -0.2407(9) -0.1688(7) 0.207(11) Uani 1 d D . H5A H 0.1393(32) -0.2169(60) -0.1737(11) 0.310 Uiso 1 calc R . H5B H 0.2130(36) -0.2117(54) -0.1559(25) 0.310 Uiso 1 calc R . H5C H 0.1783(68) -0.2762(10) -0.1470(18) 0.310 Uiso 1 calc R . C6 C 0.1852(10) -0.2660(14) -0.2126(12) 0.249(19) Uani 1 d D . N3 N 0.1997(25) -0.2848(24) -0.2437(15) 0.433(42) Uani 0.70(5) d PDU . C7 C 0.6073(5) 0.4327(5) -0.1451(4) 0.159(4) Uani 1 d . . H7A H 0.6388(20) 0.4036(34) -0.1272(17) 0.238 Uiso 1 calc R . H7B H 0.6257(27) 0.4751(9) -0.1472(28) 0.238 Uiso 1 calc R . H7C H 0.5913(9) 0.4153(40) -0.1766(12) 0.238 Uiso 1 calc R . C8 C 0.5582(4) 0.4387(4) -0.1225(3) 0.101(2) Uani 1 d . . N4 N 0.5190(5) 0.4427(5) -0.1044(4) 0.186(4) Uani 1 d . . C9 C 0.0689(10) 0.5572(16) -0.1288(8) 0.391(19) Uani 1 d DU . H9A H 0.0480(52) 0.5725(133) -0.1051(67) 0.586 Uiso 1 calc R . H9B H 0.0695(10) 0.5100(17) -0.1287(113) 0.586 Uiso 1 calc R . H9C H 0.0467(47) 0.5727(130) -0.1596(49) 0.586 Uiso 1 calc R . C10 C 0.1316(15) 0.5812(14) -0.1182(11) 0.418(25) Uani 1 d DU . H10A H 0.1284(15) 0.6197(14) -0.0992(11) 0.501 Uiso 1 calc R . H10B H 0.1535(15) 0.5489(14) -0.0955(11) 0.501 Uiso 1 calc R . O O 0.1756(13) 0.5987(19) -0.1393(13) 0.873(43) Uani 1 d DU . C11 C 0.2357(15) 0.5612(17) -0.1215(16) 0.696(46) Uani 1 d DU . H11A H 0.2371(15) 0.5234(17) -0.1418(16) 0.835 Uiso 1 calc R . H11B H 0.2388(15) 0.5458(17) -0.0893(16) 0.835 Uiso 1 calc R . C12 C 0.2884(13) 0.6073(12) -0.1228(11) 0.436(19) Uani 1 d DU . H12A H 0.2734(50) 0.6517(13) -0.1234(145) 0.653 Uiso 1 calc R . H12B H 0.3035(126) 0.5991(133) -0.1508(71) 0.653 Uiso 1 calc R . H12C H 0.3222(80) 0.6008(137) -0.0950(71) 0.653 Uiso 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 Mn1 0.0531(4) 0.0331(4) 0.0484(4) -0.0011(3) 0.0143(3) -0.0005(3) Mn2 0.0449(4) 0.0368(4) 0.0451(4) 0.0013(3) 0.0118(3) -0.0007(3) Mn3 0.0494(4) 0.0385(4) 0.0503(4) -0.0027(3) 0.0118(3) -0.0014(3) Mn4 0.0474(4) 0.0386(4) 0.0483(4) -0.0023(3) 0.0069(3) -0.0005(3) B1 0.052(3) 0.037(3) 0.039(3) -0.004(2) 0.014(3) -0.003(2) N111 0.050(2) 0.032(2) 0.045(2) 0.000(2) 0.013(2) 0.001(2) N112 0.052(2) 0.033(2) 0.044(2) -0.004(2) 0.015(2) -0.003(2) C113 0.058(3) 0.036(3) 0.054(3) -0.010(2) 0.010(3) -0.003(2) C114 0.061(3) 0.041(3) 0.052(3) -0.007(2) 0.005(3) -0.006(2) C115 0.051(3) 0.046(3) 0.037(3) 0.001(2) 0.006(2) 0.001(2) C116 0.063(3) 0.045(3) 0.047(3) 0.004(2) 0.014(3) 0.001(2) C117 0.059(3) 0.065(4) 0.068(4) 0.005(3) -0.003(3) -0.004(3) C118 0.074(4) 0.074(4) 0.088(5) 0.016(4) -0.015(4) 0.010(4) C119 0.083(4) 0.063(4) 0.083(4) 0.018(3) 0.003(4) 0.013(3) C120 0.072(4) 0.047(3) 0.067(4) 0.004(3) 0.008(3) 0.004(3) N121 0.060(3) 0.042(2) 0.056(3) 0.001(2) 0.009(2) 0.005(2) N131 0.050(2) 0.032(2) 0.043(2) 0.002(2) 0.012(2) -0.001(2) N132 0.049(2) 0.031(2) 0.045(2) -0.001(2) 0.014(2) 0.001(2) C133 0.060(3) 0.044(3) 0.056(3) -0.005(2) 0.022(3) 0.008(2) C134 0.069(3) 0.034(3) 0.064(3) -0.007(2) 0.021(3) 0.004(2) C135 0.053(3) 0.032(3) 0.052(3) 0.003(2) 0.005(2) 0.001(2) C136 0.058(3) 0.038(3) 0.061(3) 0.005(2) 0.011(3) -0.005(2) C137 0.108(5) 0.037(3) 0.105(5) 0.014(3) 0.051(4) 0.002(3) C138 0.144(7) 0.041(4) 0.153(7) 0.026(4) 0.075(6) -0.001(4) C139 0.121(6) 0.060(4) 0.134(6) 0.025(4) 0.071(5) -0.002(4) C140 0.085(4) 0.050(3) 0.085(4) 0.018(3) 0.040(4) -0.005(3) N141 0.061(3) 0.041(2) 0.057(3) 0.008(2) 0.017(2) -0.002(2) N151 0.049(2) 0.037(2) 0.051(2) 0.000(2) 0.015(2) 0.000(2) N152 0.051(2) 0.037(2) 0.048(2) -0.004(2) 0.015(2) 0.000(2) C153 0.065(3) 0.043(3) 0.047(3) -0.003(2) 0.018(3) 0.002(2) C154 0.069(3) 0.050(3) 0.046(3) 0.000(2) 0.025(3) 0.000(3) C155 0.054(3) 0.039(3) 0.059(3) 0.000(2) 0.024(3) -0.003(2) C156 0.057(3) 0.043(3) 0.070(4) -0.002(3) 0.026(3) -0.005(2) C157 0.064(4) 0.102(5) 0.081(4) 0.006(4) 0.032(3) -0.002(4) C158 0.068(5) 0.128(7) 0.111(6) 0.002(5) 0.046(4) -0.007(4) C159 0.050(4) 0.112(6) 0.113(6) -0.011(5) 0.024(4) -0.016(4) C160 0.058(4) 0.081(4) 0.084(4) -0.019(3) 0.016(3) -0.013(3) N161 0.050(3) 0.054(3) 0.068(3) -0.011(2) 0.015(2) -0.008(2) B2 0.051(3) 0.036(3) 0.044(3) 0.003(2) 0.013(3) 0.000(2) N211 0.043(2) 0.041(2) 0.041(2) -0.001(2) 0.010(2) 0.000(2) N212 0.046(2) 0.041(2) 0.039(2) 0.004(2) 0.010(2) 0.001(2) C213 0.061(3) 0.054(3) 0.040(3) 0.001(2) 0.011(2) 0.001(3) C214 0.061(3) 0.057(3) 0.046(3) 0.005(2) 0.020(3) 0.003(3) C215 0.053(3) 0.036(3) 0.044(3) 0.003(2) 0.015(2) 0.004(2) C216 0.053(3) 0.036(3) 0.050(3) 0.007(2) 0.020(2) 0.005(2) C217 0.063(4) 0.058(3) 0.062(3) 0.007(3) 0.025(3) 0.003(3) C218 0.064(4) 0.060(4) 0.083(4) 0.013(3) 0.033(3) 0.004(3) C219 0.044(3) 0.068(4) 0.081(4) 0.013(3) 0.014(3) -0.001(3) C220 0.051(3) 0.073(4) 0.068(4) 0.007(3) 0.012(3) -0.005(3) N221 0.048(2) 0.045(2) 0.055(3) 0.003(2) 0.013(2) -0.002(2) N231 0.047(2) 0.036(2) 0.051(2) -0.006(2) 0.013(2) 0.001(2) N232 0.049(2) 0.036(2) 0.046(2) 0.001(2) 0.011(2) -0.001(2) C233 0.064(3) 0.046(3) 0.064(3) 0.007(3) 0.023(3) -0.003(3) C234 0.074(4) 0.035(3) 0.087(4) 0.006(3) 0.024(3) 0.001(3) C235 0.052(3) 0.037(3) 0.057(3) -0.002(2) 0.010(3) 0.001(2) C236 0.049(3) 0.039(3) 0.063(3) -0.004(2) 0.006(3) 0.001(2) C237 0.074(4) 0.036(3) 0.100(5) -0.004(3) 0.020(3) 0.002(3) C238 0.087(4) 0.041(3) 0.110(5) -0.015(3) 0.027(4) 0.012(3) C239 0.089(4) 0.059(4) 0.091(5) -0.013(3) 0.030(4) 0.015(3) C240 0.075(4) 0.053(3) 0.084(4) -0.006(3) 0.029(3) 0.007(3) N241 0.059(3) 0.041(2) 0.061(3) -0.006(2) 0.013(2) 0.007(2) N251 0.050(2) 0.038(2) 0.050(2) -0.004(2) 0.006(2) -0.003(2) N252 0.053(2) 0.035(2) 0.047(2) 0.001(2) 0.010(2) 0.000(2) C253 0.060(3) 0.045(3) 0.057(3) 0.008(3) 0.006(3) 0.005(3) C254 0.059(3) 0.053(3) 0.057(3) 0.005(3) -0.004(3) 0.002(3) C255 0.049(3) 0.043(3) 0.054(3) -0.001(2) 0.004(2) -0.003(2) C256 0.054(3) 0.053(3) 0.051(3) -0.005(3) 0.005(3) -0.004(3) C257 0.062(4) 0.065(4) 0.080(4) -0.009(3) -0.015(3) -0.001(3) C258 0.082(4) 0.069(4) 0.096(5) -0.023(4) -0.025(4) -0.014(4) C259 0.087(5) 0.055(4) 0.095(5) -0.007(3) -0.014(4) -0.012(3) C260 0.081(4) 0.046(3) 0.084(4) -0.011(3) -0.011(3) -0.012(3) N261 0.058(3) 0.048(3) 0.062(3) -0.004(2) -0.002(2) -0.008(2) B3 0.049(3) 0.038(3) 0.051(3) -0.004(3) 0.015(3) -0.005(2) N311 0.050(2) 0.038(2) 0.049(2) -0.004(2) 0.009(2) -0.002(2) N312 0.051(2) 0.036(2) 0.052(2) -0.008(2) 0.011(2) -0.006(2) C313 0.062(3) 0.044(3) 0.069(4) -0.014(3) 0.008(3) -0.008(3) C314 0.060(3) 0.051(3) 0.066(3) -0.012(3) -0.002(3) -0.006(3) C315 0.047(3) 0.055(3) 0.054(3) -0.008(3) 0.007(3) -0.004(2) C316 0.050(3) 0.058(3) 0.057(3) -0.003(3) 0.002(3) 0.000(3) C317 0.071(4) 0.077(4) 0.089(5) -0.010(4) -0.017(4) 0.006(3) C318 0.104(6) 0.095(6) 0.101(6) 0.002(5) -0.041(5) 0.011(5) C319 0.104(6) 0.071(5) 0.118(6) 0.012(4) -0.030(5) 0.020(4) C320 0.086(5) 0.066(4) 0.084(4) 0.007(3) -0.013(4) 0.007(3) N321 0.060(3) 0.049(3) 0.064(3) 0.003(2) 0.003(2) 0.002(2) N331 0.048(2) 0.034(2) 0.046(2) -0.002(2) 0.009(2) -0.004(2) N332 0.049(2) 0.035(2) 0.055(2) -0.005(2) 0.014(2) -0.004(2) C333 0.063(3) 0.041(3) 0.064(3) -0.001(3) 0.021(3) -0.010(2) C334 0.069(3) 0.033(3) 0.066(3) 0.001(2) 0.017(3) -0.007(2) C335 0.049(3) 0.032(3) 0.052(3) -0.005(2) 0.002(2) -0.005(2) C336 0.045(3) 0.042(3) 0.054(3) -0.007(2) 0.001(2) 0.002(2) C337 0.082(4) 0.038(3) 0.067(4) 0.000(3) 0.011(3) 0.008(3) C338 0.095(5) 0.040(3) 0.089(4) -0.008(3) 0.025(4) 0.019(3) C339 0.093(5) 0.057(4) 0.089(5) -0.014(3) 0.031(4) 0.017(3) C340 0.074(4) 0.052(3) 0.078(4) -0.007(3) 0.025(3) 0.006(3) N341 0.057(3) 0.044(2) 0.057(3) -0.004(2) 0.016(2) 0.004(2) N351 0.050(2) 0.034(2) 0.048(2) -0.002(2) 0.017(2) -0.004(2) N352 0.046(2) 0.036(2) 0.057(3) -0.002(2) 0.016(2) -0.004(2) C353 0.049(3) 0.059(3) 0.070(4) -0.006(3) 0.017(3) -0.009(3) C354 0.054(3) 0.059(3) 0.078(4) -0.009(3) 0.032(3) -0.008(3) C355 0.066(3) 0.035(3) 0.056(3) -0.001(2) 0.028(3) -0.003(2) C356 0.069(4) 0.035(3) 0.056(3) 0.000(2) 0.026(3) -0.003(2) C357 0.085(4) 0.054(3) 0.069(4) -0.002(3) 0.044(3) -0.007(3) C358 0.111(5) 0.073(4) 0.062(4) -0.007(3) 0.050(4) -0.010(4) C359 0.106(5) 0.087(5) 0.059(4) -0.010(3) 0.033(4) -0.013(4) C360 0.082(4) 0.080(4) 0.054(3) -0.004(3) 0.025(3) -0.005(3) N361 0.069(3) 0.048(2) 0.052(3) 0.000(2) 0.020(2) -0.004(2) B4 0.041(3) 0.037(3) 0.043(3) -0.001(2) 0.010(2) 0.001(2) N411 0.046(2) 0.041(2) 0.041(2) -0.002(2) 0.009(2) 0.002(2) N412 0.040(2) 0.039(2) 0.045(2) -0.002(2) 0.006(2) 0.002(2) C413 0.039(3) 0.048(3) 0.059(3) -0.002(2) 0.009(2) 0.005(2) C414 0.047(3) 0.060(3) 0.057(3) -0.001(3) 0.020(3) 0.003(2) C415 0.053(3) 0.042(3) 0.045(3) -0.003(2) 0.012(2) 0.001(2) C416 0.061(3) 0.044(3) 0.056(3) -0.004(2) 0.023(3) 0.004(2) C417 0.076(4) 0.094(5) 0.061(4) -0.003(3) 0.028(3) 0.006(3) C418 0.102(6) 0.126(6) 0.057(4) -0.015(4) 0.029(4) 0.000(5) C419 0.105(6) 0.109(6) 0.051(4) -0.010(4) 0.015(4) 0.006(4) C420 0.076(4) 0.085(4) 0.053(3) -0.008(3) 0.012(3) -0.003(3) N421 0.065(3) 0.053(3) 0.043(2) -0.006(2) 0.008(2) -0.002(2) N431 0.048(2) 0.031(2) 0.042(2) -0.001(2) 0.011(2) 0.000(2) N432 0.042(2) 0.036(2) 0.045(2) 0.000(2) 0.010(2) 0.002(2) C433 0.045(3) 0.045(3) 0.051(3) -0.006(2) 0.015(2) 0.005(2) C434 0.054(3) 0.035(3) 0.067(3) -0.003(2) 0.015(3) 0.005(2) C435 0.052(3) 0.027(2) 0.057(3) -0.003(2) 0.008(2) 0.001(2) C436 0.054(3) 0.037(3) 0.055(3) 0.003(2) 0.011(2) -0.001(2) C437 0.088(4) 0.034(3) 0.087(4) 0.000(3) 0.035(4) 0.002(3) C438 0.131(6) 0.034(3) 0.115(5) 0.011(3) 0.059(5) -0.007(4) C439 0.132(6) 0.052(4) 0.116(6) 0.012(4) 0.074(5) -0.015(4) C440 0.098(5) 0.050(3) 0.084(4) 0.004(3) 0.047(4) -0.004(3) N441 0.065(3) 0.036(2) 0.062(3) 0.002(2) 0.023(2) -0.004(2) N451 0.047(2) 0.033(2) 0.041(2) -0.001(2) 0.011(2) -0.001(2) N452 0.045(2) 0.032(2) 0.043(2) 0.000(2) 0.008(2) 0.003(2) C453 0.050(3) 0.041(3) 0.056(3) 0.004(2) 0.006(2) 0.004(2) C454 0.046(3) 0.052(3) 0.050(3) 0.002(2) -0.003(2) 0.004(2) C455 0.042(3) 0.047(3) 0.045(3) 0.000(2) 0.008(2) -0.002(2) C456 0.044(3) 0.047(3) 0.051(3) -0.006(2) 0.007(2) -0.007(2) C457 0.066(4) 0.060(4) 0.065(4) -0.007(3) 0.000(3) -0.005(3) C458 0.082(4) 0.074(4) 0.077(4) -0.017(4) -0.012(4) -0.017(4) C459 0.094(5) 0.050(4) 0.086(4) -0.016(3) -0.009(4) -0.012(3) C460 0.067(4) 0.043(3) 0.076(4) -0.005(3) 0.001(3) -0.004(3) N461 0.050(2) 0.040(2) 0.056(2) -0.003(2) 0.009(2) -0.004(2) P1 0.1040(14) 0.0953(14) 0.0651(11) 0.0019(10) 0.0338(10) 0.0061(11) F11 0.157(5) 0.340(10) 0.145(5) -0.008(5) 0.062(4) 0.099(6) F12 0.324(9) 0.159(5) 0.136(5) 0.048(4) 0.091(6) -0.008(6) F13 0.253(8) 0.324(10) 0.186(6) 0.001(6) 0.126(6) 0.139(8) F14 0.199(7) 0.407(13) 0.148(6) -0.098(7) 0.021(5) -0.101(8) F15 0.173(5) 0.221(7) 0.109(4) -0.030(4) 0.015(4) -0.032(5) F16 0.503(15) 0.112(5) 0.185(6) 0.008(4) 0.168(8) -0.044(7) P2 0.0836(11) 0.0554(9) 0.0751(10) -0.0113(8) 0.0173(9) 0.0037(8) F21 0.177(4) 0.082(3) 0.080(2) -0.019(2) 0.035(3) -0.026(3) F22 0.145(4) 0.075(3) 0.141(4) -0.025(2) 0.076(3) -0.027(2) F23 0.184(5) 0.110(3) 0.073(2) -0.012(2) 0.013(3) 0.025(3) F24 0.113(3) 0.064(2) 0.121(3) -0.008(2) -0.001(2) -0.020(2) F25 0.091(3) 0.104(3) 0.147(4) -0.028(3) 0.006(3) 0.022(2) F26 0.107(3) 0.088(3) 0.180(5) 0.002(3) 0.045(3) 0.029(2) P3 0.0798(12) 0.0995(14) 0.0709(11) -0.0176(11) -0.0040(9) -0.0017(10) F31 0.103(4) 0.224(7) 0.239(6) -0.141(6) 0.060(4) -0.032(4) F32 0.103(3) 0.158(4) 0.136(4) -0.034(3) 0.023(3) 0.011(3) F33 0.243(7) 0.131(4) 0.133(4) 0.020(4) 0.028(4) -0.030(4) F34 0.167(5) 0.150(5) 0.191(6) 0.058(4) -0.001(4) 0.017(4) F35 0.109(3) 0.196(5) 0.105(3) -0.052(3) -0.016(3) -0.018(3) F36 0.113(3) 0.165(5) 0.112(3) -0.061(3) -0.013(3) -0.022(3) P4 0.0884(12) 0.0537(10) 0.1145(15) -0.0014(10) 0.0308(12) -0.0119(9) F41 0.201(6) 0.065(3) 0.360(10) -0.025(5) -0.011(7) 0.029(4) F42 0.528(19) 0.373(16) 0.533(20) -0.248(14) 0.443(18) -0.284(15) F43 0.365(10) 0.065(3) 0.228(7) 0.041(4) -0.095(7) -0.044(5) F44 0.275(10) 0.359(13) 0.275(10) -0.060(9) 0.204(9) -0.045(9) F45 0.170(6) 0.114(4) 0.306(9) -0.048(5) -0.077(6) 0.011(4) F46 0.243(7) 0.124(5) 0.227(7) 0.025(5) -0.106(6) -0.060(5) C1 0.358(22) 0.143(11) 0.227(15) 0.030(11) 0.112(15) -0.084(13) C2 0.207(13) 0.123(9) 0.107(8) 0.029(7) 0.010(8) -0.015(9) N1 0.290(16) 0.161(10) 0.171(10) -0.010(8) 0.039(10) -0.052(10) C3 0.199(13) 0.135(10) 0.300(18) 0.077(11) -0.057(12) -0.043(9) C4 0.133(8) 0.098(7) 0.197(11) 0.000(8) -0.049(7) -0.032(7) N2 0.171(9) 0.133(8) 0.278(13) -0.004(9) -0.094(9) -0.032(7) C5 0.075(7) 0.155(16) 0.371(32) 0.069(18) 0.013(13) -0.012(8) C6 0.129(12) 0.211(21) 0.413(63) -0.055(32) 0.074(24) -0.013(12) N3 0.633(85) 0.313(56) 0.468(60) -0.142(41) 0.356(56) -0.100(49) C7 0.175(10) 0.164(10) 0.163(9) 0.053(8) 0.092(8) 0.039(8) C8 0.126(7) 0.076(5) 0.114(6) 0.021(4) 0.056(5) 0.026(5) N4 0.207(10) 0.144(8) 0.252(12) 0.027(7) 0.145(9) 0.041(7) C9 0.255(23) 0.692(62) 0.205(18) -0.093(28) 0.015(17) -0.083(29) C10 0.619(60) 0.345(34) 0.345(37) -0.065(27) 0.225(44) -0.236(44) O 0.802(60) 1.111(82) 0.734(68) -0.318(57) 0.240(53) 0.358(59) C11 0.909(83) 0.641(68) 0.443(45) 0.335(49) -0.024(52) -0.320(59) C12 0.605(54) 0.296(32) 0.382(36) 0.007(28) 0.072(38) 0.112(37) _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 Mn1 N111 2.222(4) . ? Mn1 N351 2.251(4) . ? Mn1 N431 2.256(4) . ? Mn1 N441 2.304(4) . ? Mn1 N121 2.338(4) . ? Mn1 N361 2.347(4) . ? Mn2 N131 2.224(4) . ? Mn2 N451 2.257(4) . ? Mn2 N211 2.257(4) . ? Mn2 N221 2.324(4) . ? Mn2 N461 2.336(4) . ? Mn2 N141 2.378(4) . ? Mn3 N231 2.233(4) . ? Mn3 N311 2.251(4) . ? Mn3 N151 2.254(4) . ? Mn3 N161 2.329(5) . ? Mn3 N321 2.339(5) . ? Mn3 N241 2.354(4) . ? Mn4 N251 2.216(4) . ? Mn4 N411 2.256(4) . ? Mn4 N331 2.271(4) . ? Mn4 N341 2.319(4) . ? Mn4 N261 2.333(4) . ? Mn4 N421 2.350(4) . ? B1 N112 1.537(7) . ? B1 N152 1.543(7) . ? B1 N132 1.552(6) . ? N111 C115 1.350(6) . ? N111 N112 1.376(5) . ? N112 C113 1.349(6) . ? C113 C114 1.354(7) . ? C114 C115 1.391(7) . ? C115 C116 1.464(7) . ? C116 N121 1.348(6) . ? C116 C117 1.386(7) . ? C117 C118 1.383(8) . ? C118 C119 1.367(9) . ? C119 C120 1.359(8) . ? C120 N121 1.348(7) . ? N131 C135 1.341(6) . ? N131 N132 1.351(5) . ? N132 C133 1.347(6) . ? C133 C134 1.379(7) . ? C134 C135 1.390(7) . ? C135 C136 1.455(7) . ? C136 N141 1.343(7) . ? C136 C137 1.394(7) . ? C137 C138 1.364(9) . ? C138 C139 1.375(10) . ? C139 C140 1.375(9) . ? C140 N141 1.332(7) . ? N151 C155 1.348(6) . ? N151 N152 1.366(5) . ? N152 C153 1.350(6) . ? C153 C154 1.362(7) . ? C154 C155 1.384(7) . ? C155 C156 1.472(7) . ? C156 N161 1.340(7) . ? C156 C157 1.379(8) . ? C157 C158 1.379(9) . ? C158 C159 1.370(10) . ? C159 C160 1.363(9) . ? C160 N161 1.353(7) . ? B2 N252 1.540(7) . ? B2 N232 1.543(7) . ? B2 N212 1.550(7) . ? N211 C215 1.339(6) . ? N211 N212 1.363(5) . ? N212 C213 1.348(6) . ? C213 C214 1.361(7) . ? C214 C215 1.390(7) . ? C215 C216 1.465(7) . ? C216 N221 1.340(6) . ? C216 C217 1.385(7) . ? C217 C218 1.375(8) . ? C218 C219 1.366(8) . ? C219 C220 1.376(8) . ? C220 N221 1.353(7) . ? N231 C235 1.347(6) . ? N231 N232 1.358(5) . ? N232 C233 1.358(6) . ? C233 C234 1.360(7) . ? C234 C235 1.383(7) . ? C235 C236 1.462(7) . ? C236 N241 1.341(7) . ? C236 C237 1.394(7) . ? C237 C238 1.371(9) . ? C238 C239 1.373(9) . ? C239 C240 1.374(8) . ? C240 N241 1.344(7) . ? N251 C255 1.355(6) . ? N251 N252 1.370(5) . ? N252 C253 1.353(6) . ? C253 C254 1.359(7) . ? C254 C255 1.385(7) . ? C255 C256 1.471(7) . ? C256 N261 1.353(7) . ? C256 C257 1.373(7) . ? C257 C258 1.376(8) . ? C258 C259 1.350(9) . ? C259 C260 1.379(8) . ? C260 N261 1.344(7) . ? B3 N312 1.534(7) . ? B3 N332 1.548(7) . ? B3 N352 1.554(7) . ? N311 C315 1.352(6) . ? N311 N312 1.367(5) . ? N312 C313 1.352(6) . ? C313 C314 1.363(8) . ? C314 C315 1.393(7) . ? C315 C316 1.461(7) . ? C316 N321 1.350(7) . ? C316 C317 1.386(8) . ? C317 C318 1.382(10) . ? C318 C319 1.357(10) . ? C319 C320 1.376(9) . ? C320 N321 1.340(7) . ? N331 C335 1.352(6) . ? N331 N332 1.363(5) . ? N332 C333 1.359(6) . ? C333 C334 1.371(7) . ? C334 C335 1.379(7) . ? C335 C336 1.467(7) . ? C336 N341 1.343(7) . ? C336 C337 1.391(7) . ? C337 C338 1.369(8) . ? C338 C339 1.369(9) . ? C339 C340 1.387(8) . ? C340 N341 1.339(7) . ? N351 C355 1.346(6) . ? N351 N352 1.358(5) . ? N352 C353 1.351(6) . ? C353 C354 1.357(8) . ? C354 C355 1.384(7) . ? C355 C356 1.466(7) . ? C356 N361 1.337(7) . ? C356 C357 1.390(7) . ? C357 C358 1.376(8) . ? C358 C359 1.366(9) . ? C359 C360 1.373(8) . ? C360 N361 1.349(7) . ? B4 N412 1.535(6) . ? B4 N452 1.540(6) . ? B4 N432 1.547(6) . ? N411 C415 1.342(6) . ? N411 N412 1.360(5) . ? N412 C413 1.345(6) . ? C413 C414 1.358(7) . ? C414 C415 1.394(7) . ? C415 C416 1.458(7) . ? C416 N421 1.340(7) . ? C416 C417 1.389(8) . ? C417 C418 1.363(9) . ? C418 C419 1.370(10) . ? C419 C420 1.384(9) . ? C420 N421 1.339(7) . ? N431 C435 1.346(6) . ? N431 N432 1.355(5) . ? N432 C433 1.357(6) . ? C433 C434 1.365(7) . ? C434 C435 1.386(7) . ? C435 C436 1.467(7) . ? C436 N441 1.342(6) . ? C436 C437 1.376(7) . ? C437 C438 1.361(8) . ? C438 C439 1.367(9) . ? C439 C440 1.393(8) . ? C440 N441 1.325(7) . ? N451 C455 1.351(6) . ? N451 N452 1.367(5) . ? N452 C453 1.340(6) . ? C453 C454 1.366(7) . ? C454 C455 1.389(7) . ? C455 C456 1.465(7) . ? C456 N461 1.351(6) . ? C456 C457 1.382(7) . ? C457 C458 1.385(8) . ? C458 C459 1.378(9) . ? C459 C460 1.361(8) . ? C460 N461 1.346(6) . ? P1 F14 1.497(7) . ? P1 F13 1.502(6) . ? P1 F16 1.509(6) . ? P1 F11 1.516(6) . ? P1 F12 1.531(6) . ? P1 F15 1.542(6) . ? P2 F25 1.571(4) . ? P2 F26 1.574(4) . ? P2 F21 1.577(4) . ? P2 F24 1.580(4) . ? P2 F22 1.583(4) . ? P2 F23 1.584(4) . ? P3 F33 1.542(6) . ? P3 F31 1.554(5) . ? P3 F36 1.559(4) . ? P3 F32 1.574(5) . ? P3 F35 1.575(4) . ? P3 F34 1.580(6) . ? P4 F44 1.408(7) . ? P4 F42 1.447(8) . ? P4 F43 1.503(5) . ? P4 F41 1.514(6) . ? P4 F46 1.513(6) . ? P4 F45 1.547(6) . ? C1 C2 1.40(2) . ? C2 N1 1.117(14) . ? C3 C4 1.347(14) . ? C4 N2 1.143(13) . ? C5 C6 1.41(3) . ? C6 N3 1.09(3) . ? C7 C8 1.384(12) . ? C8 N4 1.106(11) . ? C9 C10 1.41(2) . ? C10 O 1.30(3) . ? O C11 1.49(3) . ? C11 C12 1.49(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 N111 Mn1 N351 106.74(14) . . ? N111 Mn1 N431 106.75(14) . . ? N351 Mn1 N431 110.45(14) . . ? N111 Mn1 N441 159.9(2) . . ? N351 Mn1 N441 91.73(15) . . ? N431 Mn1 N441 72.81(14) . . ? N111 Mn1 N121 73.22(14) . . ? N351 Mn1 N121 159.86(15) . . ? N431 Mn1 N121 88.28(15) . . ? N441 Mn1 N121 86.7(2) . . ? N111 Mn1 N361 88.05(15) . . ? N351 Mn1 N361 72.6(2) . . ? N431 Mn1 N361 162.59(14) . . ? N441 Mn1 N361 90.1(2) . . ? N121 Mn1 N361 87.3(2) . . ? N131 Mn2 N451 109.95(14) . . ? N131 Mn2 N211 108.79(14) . . ? N451 Mn2 N211 106.41(14) . . ? N131 Mn2 N221 157.10(14) . . ? N451 Mn2 N221 90.61(14) . . ? N211 Mn2 N221 73.18(14) . . ? N131 Mn2 N461 89.88(14) . . ? N451 Mn2 N461 72.70(14) . . ? N211 Mn2 N461 159.87(14) . . ? N221 Mn2 N461 86.69(15) . . ? N131 Mn2 N141 72.62(14) . . ? N451 Mn2 N141 158.77(14) . . ? N211 Mn2 N141 91.98(14) . . ? N221 Mn2 N141 84.57(15) . . ? N461 Mn2 N141 86.36(15) . . ? N231 Mn3 N311 109.36(14) . . ? N231 Mn3 N151 107.79(14) . . ? N311 Mn3 N151 107.49(14) . . ? N231 Mn3 N161 157.50(15) . . ? N311 Mn3 N161 91.26(15) . . ? N151 Mn3 N161 72.9(2) . . ? N231 Mn3 N321 90.4(2) . . ? N311 Mn3 N321 72.4(2) . . ? N151 Mn3 N321 160.1(2) . . ? N161 Mn3 N321 87.3(2) . . ? N231 Mn3 N241 72.92(15) . . ? N311 Mn3 N241 159.37(15) . . ? N151 Mn3 N241 90.62(15) . . ? N161 Mn3 N241 84.6(2) . . ? N321 Mn3 N241 87.2(2) . . ? N251 Mn4 N411 108.74(14) . . ? N251 Mn4 N331 106.22(15) . . ? N411 Mn4 N331 110.10(14) . . ? N251 Mn4 N341 158.52(15) . . ? N411 Mn4 N341 91.15(15) . . ? N331 Mn4 N341 72.98(15) . . ? N251 Mn4 N261 73.8(2) . . ? N411 Mn4 N261 158.6(2) . . ? N331 Mn4 N261 88.8(2) . . ? N341 Mn4 N261 84.7(2) . . ? N251 Mn4 N421 90.6(2) . . ? N411 Mn4 N421 71.88(15) . . ? N331 Mn4 N421 160.71(15) . . ? N341 Mn4 N421 87.9(2) . . ? N261 Mn4 N421 87.0(2) . . ? N112 B1 N152 107.7(4) . . ? N112 B1 N132 107.7(4) . . ? N152 B1 N132 106.4(4) . . ? C115 N111 N112 105.8(4) . . ? C115 N111 Mn1 114.8(3) . . ? N112 N111 Mn1 136.2(3) . . ? C113 N112 N111 108.7(4) . . ? C113 N112 B1 128.6(4) . . ? N111 N112 B1 122.7(4) . . ? N112 C113 C114 110.1(4) . . ? C113 C114 C115 104.8(4) . . ? N111 C115 C114 110.7(4) . . ? N111 C115 C116 119.0(4) . . ? C114 C115 C116 130.2(5) . . ? N121 C116 C117 122.3(5) . . ? N121 C116 C115 116.2(4) . . ? C117 C116 C115 121.5(5) . . ? C118 C117 C116 118.4(6) . . ? C119 C118 C117 119.8(6) . . ? C120 C119 C118 118.6(6) . . ? N121 C120 C119 123.9(6) . . ? C116 N121 C120 117.1(5) . . ? C116 N121 Mn1 113.5(3) . . ? C120 N121 Mn1 129.3(4) . . ? C135 N131 N132 106.2(4) . . ? C135 N131 Mn2 115.8(3) . . ? N132 N131 Mn2 135.6(3) . . ? C133 N132 N131 110.0(4) . . ? C133 N132 B1 127.5(4) . . ? N131 N132 B1 122.5(4) . . ? N132 C133 C134 108.7(4) . . ? C133 C134 C135 104.2(4) . . ? N131 C135 C134 110.9(4) . . ? N131 C135 C136 120.1(5) . . ? C134 C135 C136 129.0(5) . . ? N141 C136 C137 121.5(5) . . ? N141 C136 C135 116.4(4) . . ? C137 C136 C135 122.1(5) . . ? C138 C137 C136 118.6(6) . . ? C137 C138 C139 120.3(6) . . ? C138 C139 C140 117.8(6) . . ? N141 C140 C139 123.4(6) . . ? C140 N141 C136 118.4(5) . . ? C140 N141 Mn2 128.3(4) . . ? C136 N141 Mn2 113.0(3) . . ? C155 N151 N152 105.4(4) . . ? C155 N151 Mn3 114.7(3) . . ? N152 N151 Mn3 137.4(3) . . ? C153 N152 N151 109.4(4) . . ? C153 N152 B1 128.4(4) . . ? N151 N152 B1 121.8(4) . . ? N152 C153 C154 109.3(5) . . ? C153 C154 C155 104.7(4) . . ? N151 C155 C154 111.2(5) . . ? N151 C155 C156 119.0(5) . . ? C154 C155 C156 129.8(5) . . ? N161 C156 C157 122.7(5) . . ? N161 C156 C155 116.3(5) . . ? C157 C156 C155 121.0(5) . . ? C156 C157 C158 118.7(7) . . ? C159 C158 C157 119.0(7) . . ? C160 C159 C158 119.5(7) . . ? N161 C160 C159 122.6(6) . . ? C156 N161 C160 117.4(5) . . ? C156 N161 Mn3 114.6(3) . . ? C160 N161 Mn3 127.3(4) . . ? N252 B2 N232 108.1(4) . . ? N252 B2 N212 107.9(4) . . ? N232 B2 N212 107.0(4) . . ? C215 N211 N212 105.8(4) . . ? C215 N211 Mn2 114.4(3) . . ? N212 N211 Mn2 138.4(3) . . ? C213 N212 N211 109.6(4) . . ? C213 N212 B2 128.1(4) . . ? N211 N212 B2 122.2(4) . . ? N212 C213 C214 108.9(5) . . ? C213 C214 C215 104.8(5) . . ? N211 C215 C214 110.9(4) . . ? N211 C215 C216 120.1(4) . . ? C214 C215 C216 129.0(5) . . ? N221 C216 C217 122.5(5) . . ? N221 C216 C215 116.3(4) . . ? C217 C216 C215 121.2(5) . . ? C218 C217 C216 118.8(6) . . ? C219 C218 C217 119.8(6) . . ? C218 C219 C220 118.5(5) . . ? N221 C220 C219 123.1(6) . . ? C216 N221 C220 117.4(5) . . ? C216 N221 Mn2 114.3(3) . . ? C220 N221 Mn2 127.7(4) . . ? C235 N231 N232 106.2(4) . . ? C235 N231 Mn3 115.0(3) . . ? N232 N231 Mn3 135.8(3) . . ? N231 N232 C233 109.2(4) . . ? N231 N232 B2 122.9(4) . . ? C233 N232 B2 127.9(4) . . ? N232 C233 C234 108.7(5) . . ? C233 C234 C235 105.4(5) . . ? N231 C235 C234 110.4(5) . . ? N231 C235 C236 119.6(5) . . ? C234 C235 C236 129.9(5) . . ? N241 C236 C237 122.1(5) . . ? N241 C236 C235 115.9(4) . . ? C237 C236 C235 122.0(5) . . ? C238 C237 C236 119.1(6) . . ? C239 C238 C237 119.3(6) . . ? C238 C239 C240 118.6(6) . . ? N241 C240 C239 123.6(6) . . ? C236 N241 C240 117.4(5) . . ? C236 N241 Mn3 114.1(3) . . ? C240 N241 Mn3 128.5(4) . . ? C255 N251 N252 105.7(4) . . ? C255 N251 Mn4 114.7(3) . . ? N252 N251 Mn4 136.9(3) . . ? C253 N252 N251 109.1(4) . . ? C253 N252 B2 129.0(4) . . ? N251 N252 B2 121.9(4) . . ? N252 C253 C254 109.4(5) . . ? C253 C254 C255 105.2(5) . . ? N251 C255 C254 110.7(4) . . ? N251 C255 C256 119.6(4) . . ? C254 C255 C256 129.8(5) . . ? N261 C256 C257 121.8(5) . . ? N261 C256 C255 115.7(4) . . ? C257 C256 C255 122.5(5) . . ? C256 C257 C258 119.6(6) . . ? C259 C258 C257 119.4(6) . . ? C258 C259 C260 119.0(6) . . ? N261 C260 C259 122.9(6) . . ? C260 N261 C256 117.3(5) . . ? C260 N261 Mn4 128.7(4) . . ? C256 N261 Mn4 113.8(3) . . ? N312 B3 N332 108.1(4) . . ? N312 B3 N352 108.1(4) . . ? N332 B3 N352 106.7(4) . . ? C315 N311 N312 105.9(4) . . ? C315 N311 Mn3 115.3(3) . . ? N312 N311 Mn3 136.8(3) . . ? C313 N312 N311 109.2(4) . . ? C313 N312 B3 129.2(4) . . ? N311 N312 B3 121.6(4) . . ? N312 C313 C314 109.5(5) . . ? C313 C314 C315 104.8(5) . . ? N311 C315 C314 110.6(5) . . ? N311 C315 C316 119.2(5) . . ? C314 C315 C316 130.1(5) . . ? N321 C316 C317 122.2(5) . . ? N321 C316 C315 115.7(4) . . ? C317 C316 C315 122.0(5) . . ? C316 C317 C318 118.5(6) . . ? C319 C318 C317 119.8(6) . . ? C318 C319 C320 118.8(7) . . ? N321 C320 C319 123.3(6) . . ? C320 N321 C316 117.4(5) . . ? C320 N321 Mn3 127.6(4) . . ? C316 N321 Mn3 114.9(3) . . ? C335 N331 N332 106.0(4) . . ? C335 N331 Mn4 114.8(3) . . ? N332 N331 Mn4 137.9(3) . . ? C333 N332 N331 109.1(4) . . ? C333 N332 B3 128.3(4) . . ? N331 N332 B3 122.6(4) . . ? N332 C333 C334 108.9(5) . . ? C333 C334 C335 105.0(4) . . ? N331 C335 C334 111.0(5) . . ? N331 C335 C336 119.0(5) . . ? C334 C335 C336 130.0(5) . . ? N341 C336 C337 121.9(5) . . ? N341 C336 C335 116.8(4) . . ? C337 C336 C335 121.3(5) . . ? C338 C337 C336 118.9(6) . . ? C339 C338 C337 119.7(5) . . ? C338 C339 C340 118.8(6) . . ? N341 C340 C339 122.3(6) . . ? C340 N341 C336 118.4(5) . . ? C340 N341 Mn4 126.0(4) . . ? C336 N341 Mn4 114.9(3) . . ? C355 N351 N352 106.3(4) . . ? C355 N351 Mn1 114.9(3) . . ? N352 N351 Mn1 136.3(3) . . ? C353 N352 N351 109.2(4) . . ? C353 N352 B3 128.9(4) . . ? N351 N352 B3 121.9(4) . . ? N352 C353 C354 109.0(5) . . ? C353 C354 C355 105.3(5) . . ? N351 C355 C354 110.2(5) . . ? N351 C355 C356 119.0(5) . . ? C354 C355 C356 130.6(5) . . ? N361 C356 C357 122.1(5) . . ? N361 C356 C355 116.0(5) . . ? C357 C356 C355 121.8(5) . . ? C358 C357 C356 118.7(6) . . ? C359 C358 C357 119.5(6) . . ? C358 C359 C360 119.0(6) . . ? N361 C360 C359 122.6(6) . . ? C356 N361 C360 118.0(5) . . ? C356 N361 Mn1 114.7(3) . . ? C360 N361 Mn1 126.9(4) . . ? N412 B4 N452 107.5(4) . . ? N412 B4 N432 106.9(4) . . ? N452 B4 N432 107.5(4) . . ? C415 N411 N412 106.4(4) . . ? C415 N411 Mn4 116.0(3) . . ? N412 N411 Mn4 136.3(3) . . ? C413 N412 N411 109.0(4) . . ? C413 N412 B4 129.1(4) . . ? N411 N412 B4 121.9(4) . . ? N412 C413 C414 109.7(4) . . ? C413 C414 C415 104.5(5) . . ? N411 C415 C414 110.4(4) . . ? N411 C415 C416 119.3(4) . . ? C414 C415 C416 130.3(5) . . ? N421 C416 C417 121.8(5) . . ? N421 C416 C415 116.0(5) . . ? C417 C416 C415 122.2(5) . . ? C418 C417 C416 119.4(6) . . ? C417 C418 C419 119.7(6) . . ? C418 C419 C420 118.1(6) . . ? N421 C420 C419 123.2(6) . . ? C420 N421 C416 117.9(5) . . ? C420 N421 Mn4 126.9(4) . . ? C416 N421 Mn4 115.1(3) . . ? C435 N431 N432 106.2(4) . . ? C435 N431 Mn1 114.3(3) . . ? N432 N431 Mn1 137.7(3) . . ? C433 N432 N431 109.5(4) . . ? C433 N432 B4 128.5(4) . . ? N431 N432 B4 122.0(4) . . ? N432 C433 C434 108.7(4) . . ? C433 C434 C435 105.0(4) . . ? N431 C435 C434 110.6(4) . . ? N431 C435 C436 119.5(4) . . ? C434 C435 C436 129.9(4) . . ? N441 C436 C437 122.0(5) . . ? N441 C436 C435 115.3(4) . . ? C437 C436 C435 122.7(5) . . ? C438 C437 C436 119.4(6) . . ? C437 C438 C439 119.4(6) . . ? C438 C439 C440 118.4(6) . . ? N441 C440 C439 122.5(6) . . ? C440 N441 C436 118.2(5) . . ? C440 N441 Mn1 126.0(4) . . ? C436 N441 Mn1 115.6(3) . . ? C455 N451 N452 105.8(4) . . ? C455 N451 Mn2 115.1(3) . . ? N452 N451 Mn2 137.4(3) . . ? C453 N452 N451 109.4(4) . . ? C453 N452 B4 128.6(4) . . ? N451 N452 B4 121.9(4) . . ? N452 C453 C454 109.6(4) . . ? C453 C454 C455 104.6(4) . . ? N451 C455 C454 110.6(4) . . ? N451 C455 C456 119.1(4) . . ? C454 C455 C456 130.2(4) . . ? N461 C456 C457 122.6(5) . . ? N461 C456 C455 116.1(4) . . ? C457 C456 C455 121.3(5) . . ? C458 C457 C456 118.6(6) . . ? C459 C458 C457 119.3(6) . . ? C460 C459 C458 118.5(6) . . ? N461 C460 C459 124.1(5) . . ? C456 N461 C460 116.9(4) . . ? C456 N461 Mn2 114.8(3) . . ? C460 N461 Mn2 128.3(4) . . ? F14 P1 F13 86.6(5) . . ? F14 P1 F16 92.9(6) . . ? F13 P1 F16 89.7(5) . . ? F14 P1 F11 91.9(5) . . ? F13 P1 F11 177.0(6) . . ? F16 P1 F11 87.9(5) . . ? F14 P1 F12 88.3(5) . . ? F13 P1 F12 88.6(5) . . ? F16 P1 F12 177.8(6) . . ? F11 P1 F12 93.9(5) . . ? F14 P1 F15 178.6(4) . . ? F13 P1 F15 94.5(5) . . ? F16 P1 F15 86.2(4) . . ? F11 P1 F15 87.0(4) . . ? F12 P1 F15 92.6(4) . . ? F25 P2 F26 178.5(3) . . ? F25 P2 F21 91.0(3) . . ? F26 P2 F21 90.0(3) . . ? F25 P2 F24 90.4(3) . . ? F26 P2 F24 90.6(3) . . ? F21 P2 F24 90.1(2) . . ? F25 P2 F22 90.1(3) . . ? F26 P2 F22 88.9(3) . . ? F21 P2 F22 90.3(2) . . ? F24 P2 F22 179.4(3) . . ? F25 P2 F23 89.0(3) . . ? F26 P2 F23 90.0(3) . . ? F21 P2 F23 179.4(3) . . ? F24 P2 F23 89.3(3) . . ? F22 P2 F23 90.3(3) . . ? F33 P3 F31 90.9(4) . . ? F33 P3 F36 92.1(3) . . ? F31 P3 F36 90.2(3) . . ? F33 P3 F32 90.7(4) . . ? F31 P3 F32 178.1(4) . . ? F36 P3 F32 90.8(3) . . ? F33 P3 F35 89.4(3) . . ? F31 P3 F35 89.4(3) . . ? F36 P3 F35 178.5(4) . . ? F32 P3 F35 89.6(3) . . ? F33 P3 F34 177.5(4) . . ? F31 P3 F34 91.1(4) . . ? F36 P3 F34 89.5(4) . . ? F32 P3 F34 87.3(4) . . ? F35 P3 F34 89.0(4) . . ? F44 P4 F42 174.5(9) . . ? F44 P4 F43 92.2(6) . . ? F42 P4 F43 90.7(7) . . ? F44 P4 F41 91.4(6) . . ? F42 P4 F41 85.7(7) . . ? F43 P4 F41 176.5(6) . . ? F44 P4 F46 90.8(6) . . ? F42 P4 F46 93.7(7) . . ? F43 P4 F46 92.8(4) . . ? F41 P4 F46 87.0(4) . . ? F44 P4 F45 86.5(6) . . ? F42 P4 F45 89.0(7) . . ? F43 P4 F45 86.3(4) . . ? F41 P4 F45 94.1(4) . . ? F46 P4 F45 177.2(6) . . ? N1 C2 C1 174.7(19) . . ? N2 C4 C3 179.3(19) . . ? N3 C6 C5 169.5(43) . . ? N4 C8 C7 179.2(11) . . ? O C10 C9 140.8(34) . . ? C10 O C11 112.4(59) . . ? O C11 C12 106.6(27) . . ? _refine_diff_density_max 0.652 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.073 #=END data_j _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C120 H149 B4 F18 N36 O13 P3 Zn4' _chemical_formula_weight 3043.38 _chemical_melting_point ? _chemical_compound_source ? 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' 'F' 'F' 0.0171 0.0103 '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' 'Zn' 'Zn' 0.2839 1.4301 '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 Trigonal _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 26.528(6) _cell_length_b 26.528(6) _cell_length_c 36.863(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 22466.2(107) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description clear _exptl_crystal_colour block _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method ? _exptl_crystal_F_000 9432 _exptl_absorpt_coefficient_mu 0.754 _exptl_absorpt_correction_type 'azimuthal scans' _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.83 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens R3m/V 4-circle diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7038 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 22.50 _reflns_number_total 6532 _reflns_number_observed 4253 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 63 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1480P)^2^+70.7000P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6469 _refine_ls_number_parameters 534 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1281 _refine_ls_R_factor_obs 0.0828 _refine_ls_wR_factor_all 0.2662 _refine_ls_wR_factor_obs 0.2166 _refine_ls_goodness_of_fit_all 1.047 _refine_ls_goodness_of_fit_obs 1.111 _refine_ls_restrained_S_all 1.091 _refine_ls_restrained_S_obs 1.111 _refine_ls_shift/esd_max 0.179 _refine_ls_shift/esd_mean 0.005 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn1 Zn 0.90196(4) 0.84489(4) 0.24504(3) 0.0580(3) Uani 1 d . . Zn2 Zn 1.0000 1.0000 0.38209(4) 0.0530(4) Uani 1 d S . B11 B 0.8958(4) 0.9624(4) 0.3020(2) 0.051(2) Uani 1 d . . H11 H 0.9353(4) 0.9764(4) 0.2929(2) 0.061 Uiso 1 calc R . N110 N 0.8753(3) 0.7609(3) 0.2755(2) 0.070(2) Uani 1 d . . C111 C 0.8789(5) 0.7139(4) 0.2661(3) 0.087(3) Uani 1 d . . H111 H 0.8978(5) 0.7155(4) 0.2445(3) 0.105 Uiso 1 calc R . C112 C 0.8573(6) 0.6647(5) 0.2856(4) 0.103(4) Uani 1 d . . H112 H 0.8620(6) 0.6340(5) 0.2779(4) 0.123 Uiso 1 calc R . C113 C 0.8283(6) 0.6605(5) 0.3169(4) 0.118(4) Uani 1 d . . H113 H 0.8118(6) 0.6266(5) 0.3307(4) 0.142 Uiso 1 calc R . C114 C 0.8244(5) 0.7085(4) 0.3276(3) 0.101(3) Uani 1 d . . H114 H 0.8055(5) 0.7074(4) 0.3491(3) 0.121 Uiso 1 calc R . C115 C 0.8481(4) 0.7578(4) 0.3066(3) 0.069(2) Uani 1 d . . C120 C 0.8457(4) 0.8093(3) 0.3170(2) 0.061(2) Uani 1 d . . C121 C 0.8167(4) 0.8181(4) 0.3455(2) 0.072(2) Uani 1 d . . H121 H 0.7922(4) 0.7913(4) 0.3626(2) 0.087 Uiso 1 calc R . C122 C 0.8325(4) 0.8752(4) 0.3424(2) 0.067(2) Uani 1 d . . H122 H 0.8200(4) 0.8945(4) 0.3578(2) 0.080 Uiso 1 calc R . N123 N 0.8679(3) 0.8994(3) 0.3147(2) 0.053(2) Uani 1 d . . N124 N 0.8764(3) 0.8579(3) 0.2980(2) 0.054(2) Uani 1 d . . N130 N 0.8088(3) 0.8031(3) 0.2269(2) 0.066(2) Uani 1 d . . C131 C 0.7634(4) 0.7518(4) 0.2376(3) 0.081(3) Uani 1 d . . H131 H 0.7685(4) 0.7320(4) 0.2568(3) 0.097 Uiso 1 calc R . C132 C 0.7108(5) 0.7284(5) 0.2216(4) 0.102(4) Uani 1 d . . H132 H 0.6804(5) 0.6926(5) 0.2293(4) 0.122 Uiso 1 calc R . C133 C 0.7031(5) 0.7584(6) 0.1936(4) 0.107(4) Uani 1 d . . H133 H 0.6674(5) 0.7423(6) 0.1818(4) 0.128 Uiso 1 calc R . C134 C 0.7475(4) 0.8116(5) 0.1831(3) 0.089(3) Uani 1 d . . H134 H 0.7422(4) 0.8331(5) 0.1651(3) 0.107 Uiso 1 calc R . C135 C 0.8011(4) 0.8325(4) 0.2002(3) 0.071(2) Uani 1 d . . C140 C 0.8515(4) 0.8876(4) 0.1899(2) 0.065(2) Uani 1 d . . C141 C 0.8583(4) 0.9254(4) 0.1624(3) 0.081(3) Uani 1 d . . H141 H 0.8309(4) 0.9208(4) 0.1451(3) 0.097 Uiso 1 calc R . C142 C 0.9130(4) 0.9706(5) 0.1659(2) 0.077(3) Uani 1 d . . H142 H 0.9307(4) 1.0031(5) 0.1510(2) 0.092 Uiso 1 calc R . N143 N 0.9379(3) 0.9604(3) 0.1951(2) 0.060(2) Uani 1 d . . N144 N 0.8996(3) 0.9083(3) 0.2101(2) 0.057(2) Uani 1 d . . N150 N 0.9140(3) 0.7995(3) 0.1963(2) 0.074(2) Uani 1 d . . C151 C 0.8770(5) 0.7704(5) 0.1694(3) 0.100(3) Uani 1 d . . H151 H 0.8414(5) 0.7694(5) 0.1685(3) 0.121 Uiso 1 calc R . C152 C 0.8900(6) 0.7415(6) 0.1426(3) 0.123(5) Uani 1 d . . H152 H 0.8641(6) 0.7222(6) 0.1237(3) 0.148 Uiso 1 calc R . C153 C 0.9411(6) 0.7424(6) 0.1448(3) 0.118(4) Uani 1 d . . H153 H 0.9500(6) 0.7220(6) 0.1278(3) 0.142 Uiso 1 calc R . C154 C 0.9790(5) 0.7719(5) 0.1709(3) 0.091(3) Uani 1 d . . H154 H 1.0148(5) 0.7736(5) 0.1717(3) 0.109 Uiso 1 calc R . C155 C 0.9646(4) 0.8004(4) 0.1970(2) 0.066(2) Uani 1 d . . C160 C 1.0033(4) 0.8322(3) 0.2264(2) 0.060(2) Uani 1 d . . C161 C 1.0557(4) 0.8379(4) 0.2366(3) 0.073(2) Uani 1 d . . H161 H 1.0747(4) 0.8202(4) 0.2261(3) 0.088 Uiso 1 calc R . C162 C 1.0739(4) 0.8749(4) 0.2654(2) 0.065(2) Uani 1 d . . H162 H 1.1082(4) 0.8868(4) 0.2783(2) 0.078 Uiso 1 calc R . N163 N 1.0348(3) 0.8915(3) 0.2722(2) 0.054(2) Uani 1 d . . N164 N 0.9904(3) 0.8657(3) 0.2480(2) 0.054(2) Uani 1 d . . B12 B 1.0000 1.0000 0.2108(4) 0.058(4) Uani 1 d S . C240 C 0.9233(3) 1.0509(3) 0.3835(2) 0.055(2) Uani 1 d . . C241 C 0.8720(4) 1.0479(4) 0.3726(2) 0.065(2) Uani 1 d . . H241 H 0.8524(4) 1.0646(4) 0.3838(2) 0.078 Uiso 1 calc R . C242 C 0.8565(3) 1.0153(4) 0.3419(2) 0.062(2) Uani 1 d . . H242 H 0.8233(3) 1.0054(4) 0.3283(2) 0.075 Uiso 1 calc R . N243 N 0.8960(3) 0.9991(3) 0.3340(2) 0.053(2) Uani 1 d . . N244 N 0.9381(2) 1.0209(2) 0.36033(15) 0.0473(14) Uani 1 d . . N210 N 0.9300(3) 0.9344(3) 0.4195(2) 0.061(2) Uani 1 d . . C211 C 0.9189(3) 0.8805(3) 0.4132(2) 0.054(2) Uani 1 d . . C212 C 0.8783(4) 0.8337(4) 0.4336(2) 0.073(2) Uani 1 d . . H212 H 0.8709(4) 0.7963(4) 0.4286(2) 0.088 Uiso 1 calc R . C213 C 0.8491(5) 0.8432(5) 0.4613(3) 0.087(3) Uani 1 d . . H213 H 0.8218(5) 0.8123(5) 0.4752(3) 0.104 Uiso 1 calc R . C214 C 0.8609(5) 0.8980(5) 0.4678(3) 0.089(3) Uani 1 d . . H214 H 0.8418(5) 0.9054(5) 0.4864(3) 0.107 Uiso 1 calc R . C215 C 0.9014(4) 0.9431(4) 0.4467(2) 0.082(3) Uani 1 d . . H215 H 0.9092(4) 0.9807(4) 0.4515(2) 0.099 Uiso 1 calc R . H1 H 1.0000 1.0000 0.2434(30) 0.042(29) Uiso 1 d S . P121 P 0.1295(2) 0.7700(2) 0.13292(10) 0.1130(12) Uani 1 d . . F121 F 0.1928(5) 0.8142(7) 0.1431(4) 0.274(8) Uani 1 d . . F122 F 0.1155(5) 0.8200(5) 0.1305(4) 0.238(6) Uani 1 d . . F123 F 0.0667(4) 0.7334(5) 0.1230(4) 0.256(7) Uani 1 d . . F124 F 0.1522(7) 0.7280(6) 0.1345(4) 0.259(7) Uani 1 d . . F125 F 0.1490(6) 0.7791(7) 0.0933(3) 0.227(6) Uani 1 d . . F126 F 0.1123(7) 0.7648(11) 0.1708(3) 0.345(12) Uani 1 d . . C1 C 0.7227(22) 0.6971(19) 0.1155(11) 0.364(20) Uiso 1 d . . C2 C 0.6594(21) 0.6717(18) 0.1058(11) 0.336(19) Uiso 1 d . . C3 C 0.6398(23) 0.6944(23) 0.0806(14) 0.415(26) Uiso 1 d . . C4 C 0.6985(15) 0.8807(15) 0.3620(9) 0.299(14) Uiso 1 d . . C5 C 0.7048(14) 0.8398(15) 0.3975(9) 0.276(13) Uiso 1 d . . C6 C 0.7378(15) 0.9003(16) 0.4157(9) 0.296(14) Uiso 1 d . . C7 C 0.6802(26) 1.0706(28) 0.3721(16) 0.505(33) Uiso 1 d . . C8 C 0.6985(18) 1.0222(21) 0.3560(12) 0.356(20) Uiso 1 d . . C9 C 0.6921(18) 0.9725(19) 0.3297(12) 0.357(20) Uiso 1 d . . C11 C 0.8491(49) 0.5215(44) 0.2422(26) 0.642(58) Uiso 1 d . . C10 C 0.8797(30) 0.4988(29) 0.2737(19) 0.527(37) Uiso 1 d . . C12 C 0.7902(53) 0.4777(48) 0.2602(29) 0.722(68) Uiso 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 Zn1 0.0546(6) 0.0563(6) 0.0636(6) -0.0073(4) -0.0017(4) 0.0280(5) Zn2 0.0530(6) 0.0530(6) 0.0529(9) 0.000 0.000 0.0265(3) B11 0.041(5) 0.049(5) 0.058(5) -0.006(4) 0.004(4) 0.019(4) N110 0.064(4) 0.066(5) 0.078(5) -0.001(4) -0.004(4) 0.030(4) C111 0.111(8) 0.064(6) 0.095(7) -0.011(5) 0.004(6) 0.049(6) C112 0.127(10) 0.062(7) 0.125(10) 0.005(6) 0.020(8) 0.053(7) C113 0.141(11) 0.068(7) 0.142(11) 0.021(7) 0.019(9) 0.049(8) C114 0.111(9) 0.069(7) 0.118(9) 0.011(6) 0.029(7) 0.042(6) C115 0.063(5) 0.050(5) 0.075(6) 0.002(4) -0.005(5) 0.014(4) C120 0.062(5) 0.049(5) 0.068(5) -0.002(4) -0.003(4) 0.025(4) C121 0.067(6) 0.068(6) 0.073(6) 0.010(5) 0.016(5) 0.027(5) C122 0.060(5) 0.071(6) 0.070(6) 0.005(5) 0.011(4) 0.033(5) N123 0.048(4) 0.058(4) 0.050(4) -0.005(3) 0.002(3) 0.024(3) N124 0.051(4) 0.053(4) 0.058(4) -0.003(3) 0.002(3) 0.026(3) N130 0.055(4) 0.062(4) 0.074(5) -0.012(4) -0.005(4) 0.025(4) C131 0.068(6) 0.078(6) 0.088(7) -0.012(5) -0.006(5) 0.030(5) C132 0.073(7) 0.091(8) 0.119(9) -0.007(7) -0.010(7) 0.024(6) C133 0.070(7) 0.099(9) 0.134(11) -0.043(8) -0.026(7) 0.029(7) C134 0.078(7) 0.090(8) 0.098(7) -0.020(6) -0.028(6) 0.040(6) C135 0.066(6) 0.076(6) 0.075(6) -0.020(5) -0.008(5) 0.038(5) C140 0.059(5) 0.065(5) 0.066(5) -0.013(4) -0.019(4) 0.027(4) C141 0.070(6) 0.095(7) 0.070(6) -0.010(5) -0.030(5) 0.035(6) C142 0.095(7) 0.096(7) 0.051(5) -0.003(5) -0.018(5) 0.057(6) N143 0.066(4) 0.069(4) 0.049(4) 0.000(3) -0.002(3) 0.036(4) N144 0.054(4) 0.057(4) 0.056(4) -0.006(3) 0.001(3) 0.026(3) N150 0.072(5) 0.075(5) 0.072(5) -0.022(4) -0.005(4) 0.035(4) C151 0.096(8) 0.111(9) 0.102(8) -0.037(7) -0.016(7) 0.058(7) C152 0.130(11) 0.129(11) 0.106(9) -0.060(8) -0.032(8) 0.062(9) C153 0.119(10) 0.139(11) 0.121(10) -0.067(9) -0.024(8) 0.083(9) C154 0.093(7) 0.109(8) 0.082(7) -0.033(6) 0.000(6) 0.058(7) C155 0.068(6) 0.072(6) 0.062(5) -0.015(4) 0.008(4) 0.038(5) C160 0.066(5) 0.059(5) 0.057(5) -0.006(4) 0.012(4) 0.033(4) C161 0.073(6) 0.084(6) 0.084(6) -0.010(5) 0.008(5) 0.055(5) C162 0.066(5) 0.068(5) 0.068(5) -0.001(4) 0.004(4) 0.039(5) N163 0.054(4) 0.050(4) 0.062(4) 0.002(3) 0.009(3) 0.029(3) N164 0.053(4) 0.059(4) 0.056(4) -0.009(3) -0.005(3) 0.031(3) B12 0.060(6) 0.060(6) 0.053(9) 0.000 0.000 0.030(3) C240 0.058(5) 0.058(5) 0.051(4) 0.000(4) 0.000(4) 0.031(4) C241 0.065(5) 0.068(5) 0.073(6) -0.012(4) 0.001(4) 0.042(5) C242 0.052(5) 0.071(5) 0.068(5) -0.008(4) -0.002(4) 0.034(4) N243 0.047(4) 0.056(4) 0.054(4) -0.006(3) -0.001(3) 0.025(3) N244 0.049(3) 0.051(3) 0.045(3) -0.004(3) -0.001(3) 0.027(3) N210 0.061(4) 0.059(4) 0.057(4) 0.011(3) 0.008(3) 0.027(3) C211 0.059(5) 0.057(5) 0.049(4) 0.007(4) 0.001(4) 0.031(4) C212 0.082(6) 0.066(6) 0.064(5) 0.018(4) 0.015(5) 0.031(5) C213 0.090(7) 0.080(7) 0.075(6) 0.018(5) 0.025(6) 0.031(6) C214 0.090(7) 0.105(8) 0.066(6) 0.003(6) 0.025(5) 0.044(7) C215 0.095(7) 0.079(6) 0.072(6) 0.000(5) 0.019(6) 0.042(6) P121 0.091(2) 0.141(3) 0.116(3) -0.033(2) 0.005(2) 0.064(2) F121 0.130(8) 0.339(18) 0.330(17) -0.176(14) -0.015(9) 0.100(10) F122 0.203(11) 0.206(11) 0.344(18) -0.107(12) -0.011(11) 0.131(10) F123 0.091(6) 0.224(12) 0.372(18) -0.153(12) -0.020(8) 0.017(7) F124 0.339(18) 0.256(15) 0.287(15) 0.046(12) 0.031(14) 0.228(15) F125 0.291(14) 0.402(18) 0.122(7) -0.005(9) 0.038(8) 0.273(14) F126 0.273(17) 0.700(38) 0.122(9) 0.060(15) 0.060(10) 0.289(22) _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 Zn1 N164 2.126(6) . ? Zn1 N144 2.146(7) . ? Zn1 N124 2.149(6) . ? Zn1 N130 2.246(7) . ? Zn1 N110 2.269(7) . ? Zn1 N150 2.272(7) . ? Zn2 N244 2.134(6) 3_675 ? Zn2 N244 2.134(6) 2_765 ? Zn2 N244 2.134(6) . ? Zn2 N210 2.270(6) . ? Zn2 N210 2.270(6) 3_675 ? Zn2 N210 2.270(6) 2_765 ? B11 N123 1.526(10) . ? B11 N243 1.529(10) . ? B11 N163 1.536(11) 3_675 ? N110 C115 1.334(11) . ? N110 C111 1.345(11) . ? C111 C112 1.342(14) . ? C112 C113 1.36(2) . ? C113 C114 1.39(2) . ? C114 C115 1.372(13) . ? C115 C120 1.452(12) . ? C120 N124 1.330(10) . ? C120 C121 1.388(11) . ? C121 C122 1.358(12) . ? C122 N123 1.319(10) . ? N123 N124 1.375(8) . ? N130 C135 1.332(11) . ? N130 C131 1.348(11) . ? C131 C132 1.345(14) . ? C132 C133 1.38(2) . ? C133 C134 1.37(2) . ? C134 C135 1.393(13) . ? C135 C140 1.454(12) . ? C140 N144 1.334(10) . ? C140 C141 1.371(12) . ? C141 C142 1.350(13) . ? C142 N143 1.357(10) . ? N143 N144 1.358(9) . ? N143 B12 1.556(9) . ? N150 C155 1.332(11) . ? N150 C151 1.335(12) . ? C151 C152 1.397(15) . ? C152 C153 1.35(2) . ? C153 C154 1.328(14) . ? C154 C155 1.390(12) . ? C155 C160 1.439(12) . ? C160 N164 1.361(9) . ? C160 C161 1.373(11) . ? C161 C162 1.359(12) . ? C162 N163 1.338(10) . ? N163 N164 1.359(8) . ? N163 B11 1.536(11) 2_765 ? B12 N143 1.556(9) 3_675 ? B12 N143 1.556(9) 2_765 ? C240 N244 1.351(9) . ? C240 C241 1.385(11) . ? C240 C211 1.435(10) 3_675 ? C241 C242 1.355(11) . ? C242 N243 1.346(9) . ? N243 N244 1.371(8) . ? N210 C211 1.328(10) . ? N210 C215 1.344(11) . ? C211 C212 1.390(11) . ? C211 C240 1.435(10) 2_765 ? C212 C213 1.379(13) . ? C213 C214 1.347(14) . ? C214 C215 1.380(13) . ? P121 F126 1.453(11) . ? P121 F123 1.495(9) . ? P121 F124 1.512(11) . ? P121 F125 1.528(10) . ? P121 F121 1.538(11) . ? P121 F122 1.547(12) . ? C1 C2 1.51(5) . ? C2 C3 1.35(5) . ? C4 C5 1.76(4) . ? C5 C6 1.54(4) . ? C7 C8 1.69(6) . ? C8 C9 1.58(5) . ? C11 C12 1.55(12) . ? C11 C10 1.69(10) . ? 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 N164 Zn1 N144 106.7(2) . . ? N164 Zn1 N124 107.9(2) . . ? N144 Zn1 N124 106.5(2) . . ? N164 Zn1 N130 160.4(2) . . ? N144 Zn1 N130 75.6(3) . . ? N124 Zn1 N130 89.6(2) . . ? N164 Zn1 N110 89.5(3) . . ? N144 Zn1 N110 161.9(2) . . ? N124 Zn1 N110 74.9(3) . . ? N130 Zn1 N110 86.4(3) . . ? N164 Zn1 N150 75.5(2) . . ? N144 Zn1 N150 90.4(3) . . ? N124 Zn1 N150 160.4(3) . . ? N130 Zn1 N150 85.0(3) . . ? N110 Zn1 N150 85.9(3) . . ? N244 Zn2 N244 106.7(2) 3_675 2_765 ? N244 Zn2 N244 106.7(2) 3_675 . ? N244 Zn2 N244 106.7(2) 2_765 . ? N244 Zn2 N210 162.0(2) 3_675 . ? N244 Zn2 N210 75.4(2) 2_765 . ? N244 Zn2 N210 89.2(2) . . ? N244 Zn2 N210 89.2(2) 3_675 3_675 ? N244 Zn2 N210 162.0(2) 2_765 3_675 ? N244 Zn2 N210 75.4(2) . 3_675 ? N210 Zn2 N210 86.9(2) . 3_675 ? N244 Zn2 N210 75.4(2) 3_675 2_765 ? N244 Zn2 N210 89.2(2) 2_765 2_765 ? N244 Zn2 N210 162.0(2) . 2_765 ? N210 Zn2 N210 86.9(2) . 2_765 ? N210 Zn2 N210 86.9(2) 3_675 2_765 ? N123 B11 N243 107.8(6) . . ? N123 B11 N163 107.7(6) . 3_675 ? N243 B11 N163 108.0(6) . 3_675 ? C115 N110 C111 116.8(8) . . ? C115 N110 Zn1 112.3(6) . . ? C111 N110 Zn1 130.7(7) . . ? C112 C111 N110 124.6(10) . . ? C111 C112 C113 119.1(10) . . ? C112 C113 C114 117.7(11) . . ? C115 C114 C113 120.3(11) . . ? N110 C115 C114 121.4(9) . . ? N110 C115 C120 116.5(8) . . ? C114 C115 C120 122.0(9) . . ? N124 C120 C121 111.0(7) . . ? N124 C120 C115 118.5(8) . . ? C121 C120 C115 130.5(8) . . ? C122 C121 C120 103.8(8) . . ? N123 C122 C121 110.7(8) . . ? C122 N123 N124 108.7(6) . . ? C122 N123 B11 127.5(7) . . ? N124 N123 B11 123.9(6) . . ? C120 N124 N123 105.9(6) . . ? C120 N124 Zn1 114.5(5) . . ? N123 N124 Zn1 136.6(5) . . ? C135 N130 C131 119.0(8) . . ? C135 N130 Zn1 112.5(6) . . ? C131 N130 Zn1 128.2(7) . . ? C132 C131 N130 122.4(11) . . ? C131 C132 C133 118.6(11) . . ? C134 C133 C132 120.6(11) . . ? C133 C134 C135 117.5(11) . . ? N130 C135 C134 121.8(9) . . ? N130 C135 C140 116.7(8) . . ? C134 C135 C140 121.5(9) . . ? N144 C140 C141 111.2(8) . . ? N144 C140 C135 118.5(8) . . ? C141 C140 C135 130.3(8) . . ? C142 C141 C140 105.6(8) . . ? C141 C142 N143 108.3(9) . . ? C142 N143 N144 109.4(7) . . ? C142 N143 B12 128.1(8) . . ? N144 N143 B12 122.5(7) . . ? C140 N144 N143 105.6(6) . . ? C140 N144 Zn1 114.1(5) . . ? N143 N144 Zn1 137.8(5) . . ? C155 N150 C151 117.9(8) . . ? C155 N150 Zn1 112.5(5) . . ? C151 N150 Zn1 129.5(7) . . ? N150 C151 C152 122.1(11) . . ? C153 C152 C151 118.1(11) . . ? C154 C153 C152 120.8(11) . . ? C153 C154 C155 119.4(10) . . ? N150 C155 C154 121.8(9) . . ? N150 C155 C160 116.3(7) . . ? C154 C155 C160 121.9(9) . . ? N164 C160 C161 109.8(7) . . ? N164 C160 C155 119.0(7) . . ? C161 C160 C155 131.1(7) . . ? C162 C161 C160 105.6(7) . . ? N163 C162 C161 109.3(8) . . ? C162 N163 N164 109.3(6) . . ? C162 N163 B11 127.4(7) . 2_765 ? N164 N163 B11 123.3(6) . 2_765 ? N163 N164 C160 106.0(6) . . ? N163 N164 Zn1 137.0(5) . . ? C160 N164 Zn1 113.9(5) . . ? N143 B12 N143 106.9(7) 3_675 . ? N143 B12 N143 106.9(6) 3_675 2_765 ? N143 B12 N143 106.9(7) . 2_765 ? N244 C240 C241 110.5(7) . . ? N244 C240 C211 118.5(7) . 3_675 ? C241 C240 C211 130.9(7) . 3_675 ? C242 C241 C240 104.7(7) . . ? N243 C242 C241 110.4(7) . . ? C242 N243 N244 108.3(6) . . ? C242 N243 B11 127.8(6) . . ? N244 N243 B11 123.9(6) . . ? C240 N244 N243 106.2(6) . . ? C240 N244 Zn2 113.8(5) . . ? N243 N244 Zn2 136.7(4) . . ? C211 N210 C215 118.4(7) . . ? C211 N210 Zn2 111.9(5) . . ? C215 N210 Zn2 129.6(6) . . ? N210 C211 C212 121.4(7) . . ? N210 C211 C240 117.1(7) . 2_765 ? C212 C211 C240 121.5(8) . 2_765 ? C213 C212 C211 119.6(9) . . ? C214 C213 C212 118.7(9) . . ? C213 C214 C215 119.7(9) . . ? N210 C215 C214 122.2(9) . . ? F126 P121 F123 88.8(9) . . ? F126 P121 F124 96.5(11) . . ? F123 P121 F124 104.8(9) . . ? F126 P121 F125 177.0(13) . . ? F123 P121 F125 92.7(8) . . ? F124 P121 F125 85.6(7) . . ? F126 P121 F121 90.5(10) . . ? F123 P121 F121 172.8(9) . . ? F124 P121 F121 82.4(8) . . ? F125 P121 F121 87.6(8) . . ? F126 P121 F122 86.6(10) . . ? F123 P121 F122 82.9(7) . . ? F124 P121 F122 171.7(8) . . ? F125 P121 F122 91.0(8) . . ? F121 P121 F122 89.9(8) . . ? C3 C2 C1 123.9(48) . . ? C6 C5 C4 82.0(23) . . ? C9 C8 C7 154.0(43) . . ? C12 C11 C10 85.6(71) . . ? _refine_diff_density_max 0.659 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.093 #=END data_znts2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C78 H84 B2 F18 N24 O8 P4 Zn4' _chemical_formula_weight 2234.67 _chemical_melting_point ? _chemical_compound_source ? 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' 'F' 'F' 0.0171 0.0103 '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' 'Zn' 'Zn' 0.2839 1.4301 '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 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 18.291(2) _cell_length_b 22.321(3) _cell_length_c 24.103(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.946(13) _cell_angle_gamma 90.00 _cell_volume 9507.6(20) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour clear _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method ? _exptl_crystal_F_000 4544 _exptl_absorpt_coefficient_mu 1.165 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.62 _exptl_absorpt_correction_T_max 0.64 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24571 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0796 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8328 _reflns_number_observed 5208 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 27 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0767P)^2^+20.1303P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8301 _refine_ls_number_parameters 623 _refine_ls_number_restraints 102 _refine_ls_R_factor_all 0.1106 _refine_ls_R_factor_obs 0.0592 _refine_ls_wR_factor_all 0.1643 _refine_ls_wR_factor_obs 0.1382 _refine_ls_goodness_of_fit_all 1.025 _refine_ls_goodness_of_fit_obs 1.118 _refine_ls_restrained_S_all 1.028 _refine_ls_restrained_S_obs 1.112 _refine_ls_shift/esd_max 0.371 _refine_ls_shift/esd_mean 0.013 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn1 Zn 0.94731(3) 0.03863(3) 0.85234(2) 0.0295(2) Uani 1 d . . Zn2 Zn 0.83869(4) 0.10685(3) 0.73263(3) 0.0343(2) Uani 1 d . . P1 P 1.0000 0.03403(9) 0.7500 0.0300(5) Uani 1 d S . O1 O 1.0381(2) -0.0024(2) 0.8026(2) 0.0437(10) Uani 1 d . . O2 O 0.9427(2) 0.0732(2) 0.7720(2) 0.0352(9) Uani 1 d . . B1 B 0.8388(4) 0.1704(3) 0.8796(3) 0.039(2) Uani 1 d . . H1 H 0.8075(4) 0.1955(3) 0.8991(3) 0.047 Uiso 1 calc R . N111 N 0.9120(3) 0.1516(2) 0.9249(2) 0.0391(12) Uani 1 d . . N112 N 0.9563(3) 0.1054(2) 0.9166(2) 0.0348(11) Uani 1 d . . C113 C 1.0084(3) 0.0969(2) 0.9667(2) 0.0356(13) Uani 1 d . . C114 C 0.9997(4) 0.1394(3) 1.0067(2) 0.044(2) Uani 1 d . . H11A H 1.0298(4) 0.1446(3) 1.0449(2) 0.052 Uiso 1 calc R . C115 C 0.9378(4) 0.1721(3) 0.9786(2) 0.044(2) Uani 1 d . . H11B H 0.9164(4) 0.2043(3) 0.9947(2) 0.052 Uiso 1 calc R . N121 N 1.0400(3) 0.0085(2) 0.9239(2) 0.0331(11) Uani 1 d . . C122 C 1.0583(3) 0.0453(3) 0.9700(2) 0.0358(13) Uani 1 d . . C123 C 1.1186(3) 0.0346(3) 1.0162(2) 0.0427(15) Uani 1 d . . H12A H 1.1305(3) 0.0618(3) 1.0476(2) 0.051 Uiso 1 calc R . C124 C 1.1621(4) -0.0163(3) 1.0166(3) 0.052(2) Uani 1 d . . H12B H 1.2037(4) -0.0250(3) 1.0484(3) 0.062 Uiso 1 calc R . C125 C 1.1437(3) -0.0539(3) 0.9699(3) 0.046(2) Uani 1 d . . H12C H 1.1728(3) -0.0889(3) 0.9689(3) 0.056 Uiso 1 calc R . C126 C 1.0827(3) -0.0405(3) 0.9247(2) 0.0422(14) Uani 1 d . . H12D H 1.0705(3) -0.0670(3) 0.8927(2) 0.051 Uiso 1 calc R . N211 N 0.7933(3) 0.1138(2) 0.8558(2) 0.0344(11) Uani 1 d . . N212 N 0.8284(3) 0.0654(2) 0.8392(2) 0.0346(11) Uani 1 d . . C213 C 0.7781(3) 0.0206(2) 0.8290(2) 0.0307(13) Uani 1 d . . C214 C 0.7090(3) 0.0402(3) 0.8370(2) 0.0392(14) Uani 1 d . . H21A H 0.6634(3) 0.0179(3) 0.8317(2) 0.047 Uiso 1 calc R . C215 C 0.7215(3) 0.0989(3) 0.8542(2) 0.0392(14) Uani 1 d . . H21B H 0.6852(3) 0.1248(3) 0.8636(2) 0.047 Uiso 1 calc R . N221 N 0.8831(2) -0.0419(2) 0.8259(2) 0.0304(10) Uani 1 d . . C222 C 0.8070(3) -0.0380(2) 0.8159(2) 0.0347(13) Uani 1 d . . C223 C 0.7600(4) -0.0855(3) 0.7951(3) 0.053(2) Uani 1 d . . H22A H 0.7067(4) -0.0819(3) 0.7885(3) 0.064 Uiso 1 calc R . C224 C 0.7924(4) -0.1388(3) 0.7839(4) 0.068(2) Uani 1 d . . H22B H 0.7613(4) -0.1726(3) 0.7703(4) 0.081 Uiso 1 calc R . C225 C 0.8691(4) -0.1426(3) 0.7926(3) 0.056(2) Uani 1 d . . H22C H 0.8920(4) -0.1785(3) 0.7842(3) 0.067 Uiso 1 calc R . C226 C 0.9128(4) -0.0930(2) 0.8138(2) 0.0400(14) Uani 1 d . . H22D H 0.9661(4) -0.0956(2) 0.8199(2) 0.048 Uiso 1 calc R . N311 N 0.8570(3) 0.2080(2) 0.8309(2) 0.0385(12) Uani 1 d . . N312 N 0.8612(3) 0.1857(2) 0.7797(2) 0.0359(11) Uani 1 d . . C313 C 0.8812(3) 0.2311(3) 0.7503(3) 0.0427(15) Uani 1 d . . C314 C 0.8909(4) 0.2834(3) 0.7833(3) 0.060(2) Uani 1 d . . H31A H 0.9052(4) 0.3219(3) 0.7731(3) 0.072 Uiso 1 calc R . C315 C 0.8751(4) 0.2669(3) 0.8336(3) 0.061(2) Uani 1 d . . H31B H 0.8766(4) 0.2926(3) 0.8653(3) 0.073 Uiso 1 calc R . N321 N 0.8657(3) 0.1638(2) 0.6719(2) 0.0503(14) Uani 1 d D . C322 C 0.8856(4) 0.2194(3) 0.6917(3) 0.054(2) Uani 1 d D . C323 C 0.9085(5) 0.2620(4) 0.6587(4) 0.087(3) Uani 1 d D . H32A H 0.9250(5) 0.3005(4) 0.6737(4) 0.104 Uiso 1 calc R . C324 C 0.9066(7) 0.2466(5) 0.6019(5) 0.123(5) Uani 1 d DU . H32B H 0.9209(7) 0.2755(5) 0.5777(5) 0.148 Uiso 1 calc R . C325 C 0.8841(7) 0.1901(4) 0.5804(4) 0.115(4) Uani 1 d DU . H32C H 0.8817(7) 0.1796(4) 0.5418(4) 0.138 Uiso 1 calc R . C326 C 0.8655(5) 0.1500(3) 0.6179(3) 0.078(3) Uani 1 d D . H32D H 0.8518(5) 0.1104(3) 0.6047(3) 0.093 Uiso 1 calc R . N411 N 0.8171(3) -0.0218(2) 0.6760(2) 0.0425(13) Uani 1 d . . H41A H 0.8654(3) -0.0301(2) 0.6810(2) 0.051 Uiso 1 calc R . N412 N 0.7905(3) 0.0299(2) 0.6908(2) 0.0345(11) Uani 1 d . . C413 C 0.7150(3) 0.0249(3) 0.6765(2) 0.0403(14) Uani 1 d . . C414 C 0.6936(4) -0.0311(3) 0.6518(3) 0.051(2) Uani 1 d . . H41B H 0.6438(4) -0.0464(3) 0.6375(3) 0.062 Uiso 1 calc R . C415 C 0.7605(4) -0.0589(3) 0.6526(3) 0.051(2) Uani 1 d . . H41C H 0.7657(4) -0.0982(3) 0.6388(3) 0.061 Uiso 1 calc R . N421 N 0.7147(3) 0.1221(2) 0.7163(2) 0.0344(11) Uani 1 d . . C422 C 0.6721(3) 0.0766(3) 0.6899(2) 0.0353(14) Uani 1 d . . C423 C 0.5937(3) 0.0770(3) 0.6773(3) 0.045(2) Uani 1 d . . H42A H 0.5647(3) 0.0439(3) 0.6588(3) 0.054 Uiso 1 calc R . C424 C 0.5593(4) 0.1274(3) 0.6925(3) 0.050(2) Uani 1 d . . H42B H 0.5057(4) 0.1295(3) 0.6841(3) 0.060 Uiso 1 calc R . C425 C 0.6026(4) 0.1742(3) 0.7196(3) 0.046(2) Uani 1 d . . H42C H 0.5795(4) 0.2089(3) 0.7304(3) 0.055 Uiso 1 calc R . C426 C 0.6806(3) 0.1700(3) 0.7311(2) 0.0393(14) Uani 1 d . . H42D H 0.7107(3) 0.2023(3) 0.7501(2) 0.047 Uiso 1 calc R . P2 P 0.89319(10) -0.22014(8) 0.63709(7) 0.0476(4) Uani 1 d . . F21 F 0.8355(3) -0.2117(4) 0.5786(2) 0.178(4) Uani 1 d U . F22 F 0.8942(3) -0.1506(2) 0.6488(3) 0.138(3) Uani 1 d U . F23 F 0.8933(4) -0.2891(2) 0.6289(3) 0.125(2) Uani 1 d . . F24 F 0.9600(3) -0.2129(2) 0.6073(2) 0.0905(15) Uani 1 d . . F25 F 0.8264(2) -0.2269(2) 0.6675(2) 0.0775(13) Uani 1 d . . F26 F 0.9531(2) -0.2279(2) 0.6958(2) 0.094(2) Uani 1 d . . P3 P 0.5000 -0.05439(12) 0.7500 0.0792(11) Uani 1 d S . F31 F 0.5342(3) -0.0048(3) 0.7946(4) 0.157(3) Uani 1 d U . F32 F 0.5344(4) -0.1048(3) 0.7934(3) 0.150(3) Uani 1 d U . F33 F 0.4251(3) -0.0540(2) 0.7709(3) 0.110(2) Uani 1 d U . C1 C 0.6861(19) -0.2803(16) 1.0715(12) 0.416(26) Uani 1 d DU . C2 C 0.6425(17) -0.2286(12) 1.0749(11) 0.275(16) Uani 1 d DU . O3 O 0.6619(7) -0.1640(6) 1.0303(8) 0.296(9) Uani 1 d DU . C4 C 0.6686(17) -0.0867(12) 1.0056(11) 0.304(13) Uani 1 d DU . C5 C 0.6640(21) -0.0888(12) 0.9434(11) 0.428(26) Uani 1 d DU . C6 C 0.9356(16) -0.3987(11) 0.5386(8) 0.347(18) Uani 1 d U . C7 C 0.8256(8) -0.3421(8) 0.4878(6) 0.165(6) Uani 1 d U . C8 C 0.9023(12) -0.3618(7) 0.4908(5) 0.164(7) Uani 1 d U . O8 O 0.9274(8) -0.3524(6) 0.4502(5) 0.232(6) Uani 1 d U . 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 Zn1 0.0283(4) 0.0355(4) 0.0241(3) -0.0006(3) 0.0057(3) 0.0001(3) Zn2 0.0361(4) 0.0356(4) 0.0325(4) -0.0027(3) 0.0111(3) 0.0022(3) P1 0.0281(11) 0.0380(12) 0.0249(10) 0.000 0.0088(9) 0.000 O1 0.033(2) 0.064(3) 0.031(2) 0.015(2) 0.002(2) -0.008(2) O2 0.031(2) 0.039(2) 0.040(2) -0.006(2) 0.017(2) -0.002(2) B1 0.041(4) 0.043(4) 0.036(4) -0.008(3) 0.014(3) 0.011(3) N111 0.045(3) 0.041(3) 0.029(3) -0.007(2) 0.006(2) 0.007(2) N112 0.036(3) 0.042(3) 0.025(2) -0.003(2) 0.006(2) 0.005(2) C113 0.036(3) 0.047(4) 0.025(3) -0.001(2) 0.009(3) -0.003(3) C114 0.047(4) 0.059(4) 0.021(3) -0.007(3) 0.002(3) 0.000(3) C115 0.051(4) 0.050(4) 0.029(3) -0.006(3) 0.007(3) 0.003(3) N121 0.032(3) 0.041(3) 0.027(2) 0.000(2) 0.008(2) 0.001(2) C122 0.038(3) 0.043(3) 0.026(3) 0.004(3) 0.008(3) -0.001(3) C123 0.040(4) 0.060(4) 0.026(3) -0.001(3) 0.005(3) -0.001(3) C124 0.040(4) 0.076(5) 0.032(3) 0.012(3) -0.002(3) 0.013(4) C125 0.041(4) 0.053(4) 0.043(4) 0.005(3) 0.006(3) 0.013(3) C126 0.042(4) 0.050(4) 0.035(3) 0.002(3) 0.012(3) 0.008(3) N211 0.036(3) 0.038(3) 0.031(2) -0.002(2) 0.011(2) 0.009(2) N212 0.032(3) 0.043(3) 0.029(3) -0.004(2) 0.009(2) 0.006(2) C213 0.027(3) 0.039(3) 0.023(3) 0.005(2) 0.001(2) -0.005(3) C214 0.024(3) 0.058(4) 0.033(3) 0.003(3) 0.004(3) -0.004(3) C215 0.031(3) 0.059(4) 0.029(3) 0.006(3) 0.010(3) 0.008(3) N221 0.030(3) 0.031(3) 0.029(2) 0.005(2) 0.005(2) 0.002(2) C222 0.030(3) 0.040(3) 0.032(3) 0.006(3) 0.004(3) -0.001(3) C223 0.032(4) 0.047(4) 0.077(5) -0.003(3) 0.011(3) -0.007(3) C224 0.046(5) 0.041(4) 0.112(7) -0.014(4) 0.011(4) -0.011(3) C225 0.051(5) 0.037(4) 0.083(5) -0.011(3) 0.022(4) -0.001(3) C226 0.038(4) 0.034(3) 0.048(4) 0.003(3) 0.012(3) 0.003(3) N311 0.041(3) 0.033(3) 0.038(3) -0.004(2) 0.003(2) 0.006(2) N312 0.034(3) 0.035(3) 0.040(3) -0.003(2) 0.011(2) 0.004(2) C313 0.038(4) 0.036(3) 0.052(4) 0.005(3) 0.009(3) 0.000(3) C314 0.074(5) 0.037(4) 0.061(5) 0.008(3) 0.002(4) -0.011(3) C315 0.081(6) 0.035(4) 0.055(4) -0.005(3) -0.004(4) -0.001(3) N321 0.063(4) 0.050(3) 0.044(3) 0.011(3) 0.025(3) 0.012(3) C322 0.061(5) 0.046(4) 0.068(5) 0.009(3) 0.039(4) 0.001(3) C323 0.125(8) 0.058(5) 0.094(7) 0.025(5) 0.057(6) 0.011(5) C324 0.214(13) 0.088(7) 0.113(8) 0.040(6) 0.123(9) 0.036(8) C325 0.215(13) 0.079(6) 0.084(6) 0.030(5) 0.099(8) 0.058(7) C326 0.132(8) 0.059(5) 0.060(5) 0.006(4) 0.058(5) 0.025(5) N411 0.030(3) 0.049(3) 0.045(3) -0.015(2) 0.005(2) 0.010(2) N412 0.030(3) 0.045(3) 0.027(2) -0.007(2) 0.005(2) 0.004(2) C413 0.033(4) 0.047(4) 0.037(3) -0.002(3) 0.003(3) 0.006(3) C414 0.030(4) 0.063(5) 0.059(4) -0.020(3) 0.005(3) 0.000(3) C415 0.038(4) 0.049(4) 0.063(4) -0.021(3) 0.008(3) -0.001(3) N421 0.034(3) 0.042(3) 0.028(2) 0.002(2) 0.010(2) 0.011(2) C422 0.033(4) 0.041(3) 0.031(3) 0.004(3) 0.006(3) 0.009(3) C423 0.038(4) 0.051(4) 0.044(4) 0.001(3) 0.008(3) 0.001(3) C424 0.037(4) 0.070(5) 0.045(4) 0.011(3) 0.015(3) 0.020(4) C425 0.049(4) 0.052(4) 0.039(4) 0.007(3) 0.016(3) 0.019(3) C426 0.043(4) 0.042(4) 0.033(3) 0.005(3) 0.010(3) 0.010(3) P2 0.0444(10) 0.0480(10) 0.0487(10) 0.0160(8) 0.0093(8) -0.0041(8) F21 0.084(4) 0.341(10) 0.081(4) 0.094(5) -0.029(3) -0.032(5) F22 0.117(5) 0.051(3) 0.275(8) 0.022(4) 0.104(5) 0.000(3) F23 0.154(5) 0.061(3) 0.188(6) -0.035(3) 0.093(5) -0.028(3) F24 0.077(3) 0.136(4) 0.072(3) 0.021(3) 0.043(3) -0.015(3) F25 0.050(3) 0.089(3) 0.101(3) 0.003(3) 0.034(2) -0.011(2) F26 0.059(3) 0.164(5) 0.058(3) 0.016(3) 0.010(2) -0.012(3) P3 0.041(2) 0.040(2) 0.160(3) 0.000 0.032(2) 0.000 F31 0.055(3) 0.124(5) 0.284(9) -0.098(5) 0.027(4) -0.026(3) F32 0.143(6) 0.125(5) 0.207(7) 0.082(5) 0.086(5) 0.044(4) F33 0.058(3) 0.092(3) 0.196(6) -0.038(4) 0.060(4) -0.017(3) C1 0.295(38) 0.766(77) 0.167(23) -0.008(37) 0.023(23) -0.161(46) C2 0.360(35) 0.317(27) 0.224(21) -0.151(20) 0.211(24) -0.207(26) O3 0.154(10) 0.240(15) 0.485(26) -0.122(17) 0.064(14) -0.054(11) C4 0.366(33) 0.326(31) 0.239(25) 0.056(24) 0.111(25) 0.004(27) C5 0.688(60) 0.376(35) 0.224(23) -0.007(23) 0.128(32) -0.393(41) C6 0.504(41) 0.399(34) 0.133(15) 0.106(19) 0.072(21) 0.259(31) C7 0.090(9) 0.238(17) 0.154(13) -0.046(12) 0.010(9) -0.040(10) C8 0.258(21) 0.165(13) 0.065(8) 0.012(8) 0.034(11) 0.061(13) O8 0.265(14) 0.298(14) 0.137(9) 0.090(10) 0.061(10) 0.112(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 Zn1 O2 2.067(4) . ? Zn1 N112 2.124(4) . ? Zn1 N221 2.151(4) . ? Zn1 N121 2.190(4) . ? Zn1 N212 2.198(4) . ? Zn1 O1 2.462(4) . ? Zn1 P1 2.8724(7) . ? Zn2 O2 2.037(4) . ? Zn2 N412 2.069(4) . ? Zn2 N312 2.076(4) . ? Zn2 N321 2.091(5) . ? Zn2 N421 2.225(5) . ? P1 O1 1.515(4) . ? P1 O1 1.515(4) 2_756 ? P1 O2 1.559(4) 2_756 ? P1 O2 1.559(4) . ? P1 Zn1 2.8725(7) 2_756 ? B1 N211 1.541(8) . ? B1 N311 1.547(8) . ? B1 N111 1.552(8) . ? N111 C115 1.338(7) . ? N111 N112 1.358(6) . ? N112 C113 1.346(7) . ? C113 C114 1.391(7) . ? C113 C122 1.459(8) . ? C114 C115 1.370(8) . ? N121 C126 1.341(7) . ? N121 C122 1.353(7) . ? C122 C123 1.370(8) . ? C123 C124 1.386(8) . ? C124 C125 1.373(8) . ? C125 C126 1.376(8) . ? N211 C215 1.345(7) . ? N211 N212 1.368(6) . ? N212 C213 1.338(7) . ? C213 C214 1.397(8) . ? C213 C222 1.475(7) . ? C214 C215 1.376(8) . ? N221 C226 1.329(7) . ? N221 C222 1.352(7) . ? C222 C223 1.377(8) . ? C223 C224 1.385(9) . ? C224 C225 1.368(9) . ? C225 C226 1.383(8) . ? N311 N312 1.352(6) . ? N311 C315 1.353(8) . ? N312 C313 1.341(7) . ? C313 C314 1.398(9) . ? C313 C322 1.459(9) . ? C314 C315 1.366(9) . ? N321 C326 1.339(8) . ? N321 C322 1.345(8) . ? C322 C323 1.375(9) . ? C323 C324 1.402(12) . ? C324 C325 1.384(14) . ? C325 C326 1.375(10) . ? N411 C415 1.334(7) . ? N411 N412 1.337(6) . ? N412 C413 1.340(7) . ? C413 C414 1.396(8) . ? C413 C422 1.476(8) . ? C414 C415 1.369(8) . ? N421 C426 1.333(7) . ? N421 C422 1.337(7) . ? C422 C423 1.387(8) . ? C423 C424 1.383(8) . ? C424 C425 1.371(9) . ? C425 C426 1.384(8) . ? P2 F21 1.540(5) . ? P2 F23 1.553(5) . ? P2 F26 1.560(5) . ? P2 F24 1.577(4) . ? P2 F22 1.577(5) . ? P2 F25 1.586(4) . ? P3 F32 1.554(6) . ? P3 F32 1.554(6) 2_656 ? P3 F31 1.556(6) . ? P3 F31 1.556(6) 2_656 ? P3 F33 1.578(4) . ? P3 F33 1.578(4) 2_656 ? C1 C2 1.42(3) . ? C2 O3 1.88(2) . ? O3 C4 1.84(2) . ? C4 C5 1.48(3) . ? C6 C8 1.42(2) . ? C7 C8 1.45(2) . ? C8 O8 1.20(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 Zn1 N112 113.4(2) . . ? O2 Zn1 N221 98.50(15) . . ? N112 Zn1 N221 137.3(2) . . ? O2 Zn1 N121 133.6(2) . . ? N112 Zn1 N121 75.1(2) . . ? N221 Zn1 N121 103.2(2) . . ? O2 Zn1 N212 87.94(15) . . ? N112 Zn1 N212 78.6(2) . . ? N221 Zn1 N212 74.9(2) . . ? N121 Zn1 N212 137.2(2) . . ? O2 Zn1 O1 63.38(13) . . ? N112 Zn1 O1 132.9(2) . . ? N221 Zn1 O1 86.02(15) . . ? N121 Zn1 O1 77.70(14) . . ? N212 Zn1 O1 142.89(14) . . ? O2 Zn1 P1 31.80(10) . . ? N112 Zn1 P1 132.15(13) . . ? N221 Zn1 P1 89.69(12) . . ? N121 Zn1 P1 107.60(11) . . ? N212 Zn1 P1 115.14(11) . . ? O1 Zn1 P1 31.84(9) . . ? O2 Zn2 N412 98.7(2) . . ? O2 Zn2 N312 91.6(2) . . ? N412 Zn2 N312 165.6(2) . . ? O2 Zn2 N321 100.9(2) . . ? N412 Zn2 N321 108.2(2) . . ? N312 Zn2 N321 79.5(2) . . ? O2 Zn2 N421 157.67(15) . . ? N412 Zn2 N421 75.8(2) . . ? N312 Zn2 N421 90.9(2) . . ? N321 Zn2 N421 101.4(2) . . ? O1 P1 O1 115.1(3) . 2_756 ? O1 P1 O2 112.4(2) . 2_756 ? O1 P1 O2 102.8(2) 2_756 2_756 ? O1 P1 O2 102.8(2) . . ? O1 P1 O2 112.4(2) 2_756 . ? O2 P1 O2 111.7(3) 2_756 . ? O1 P1 Zn1 59.0(2) . . ? O1 P1 Zn1 123.6(2) 2_756 . ? O2 P1 Zn1 132.5(2) 2_756 . ? O2 P1 Zn1 44.31(13) . . ? O1 P1 Zn1 123.6(2) . 2_756 ? O1 P1 Zn1 59.0(2) 2_756 2_756 ? O2 P1 Zn1 44.31(13) 2_756 2_756 ? O2 P1 Zn1 132.5(2) . 2_756 ? Zn1 P1 Zn1 175.90(8) . 2_756 ? P1 O1 Zn1 89.2(2) . . ? P1 O2 Zn2 132.6(2) . . ? P1 O2 Zn1 103.9(2) . . ? Zn2 O2 Zn1 112.4(2) . . ? N211 B1 N311 111.4(5) . . ? N211 B1 N111 109.0(5) . . ? N311 B1 N111 111.4(5) . . ? C115 N111 N112 109.1(5) . . ? C115 N111 B1 127.8(5) . . ? N112 N111 B1 122.7(4) . . ? C113 N112 N111 106.6(4) . . ? C113 N112 Zn1 117.3(4) . . ? N111 N112 Zn1 134.7(3) . . ? N112 C113 C114 110.2(5) . . ? N112 C113 C122 116.7(5) . . ? C114 C113 C122 133.0(5) . . ? C115 C114 C113 104.4(5) . . ? N111 C115 C114 109.7(5) . . ? C126 N121 C122 117.7(5) . . ? C126 N121 Zn1 126.2(4) . . ? C122 N121 Zn1 116.0(4) . . ? N121 C122 C123 122.5(5) . . ? N121 C122 C113 114.6(5) . . ? C123 C122 C113 122.9(5) . . ? C122 C123 C124 119.2(6) . . ? C125 C124 C123 118.4(6) . . ? C124 C125 C126 119.7(6) . . ? N121 C126 C125 122.4(6) . . ? C215 N211 N212 109.0(5) . . ? C215 N211 B1 130.0(5) . . ? N212 N211 B1 120.5(4) . . ? C213 N212 N211 106.9(4) . . ? C213 N212 Zn1 115.6(4) . . ? N211 N212 Zn1 134.0(4) . . ? N212 C213 C214 110.2(5) . . ? N212 C213 C222 115.7(5) . . ? C214 C213 C222 134.0(5) . . ? C215 C214 C213 104.7(5) . . ? N211 C215 C214 109.2(5) . . ? C226 N221 C222 118.4(5) . . ? C226 N221 Zn1 124.0(4) . . ? C222 N221 Zn1 117.2(4) . . ? N221 C222 C223 122.2(5) . . ? N221 C222 C213 115.4(5) . . ? C223 C222 C213 122.4(5) . . ? C222 C223 C224 118.3(6) . . ? C225 C224 C223 119.8(6) . . ? C224 C225 C226 118.7(6) . . ? N221 C226 C225 122.6(6) . . ? N312 N311 C315 109.3(5) . . ? N312 N311 B1 124.5(4) . . ? C315 N311 B1 126.1(5) . . ? C313 N312 N311 106.9(4) . . ? C313 N312 Zn2 113.3(4) . . ? N311 N312 Zn2 139.6(4) . . ? N312 C313 C314 110.1(5) . . ? N312 C313 C322 117.7(5) . . ? C314 C313 C322 132.1(6) . . ? C315 C314 C313 104.7(6) . . ? N311 C315 C314 109.0(6) . . ? C326 N321 C322 119.4(6) . . ? C326 N321 Zn2 126.8(5) . . ? C322 N321 Zn2 113.8(4) . . ? N321 C322 C323 121.9(7) . . ? N321 C322 C313 115.6(5) . . ? C323 C322 C313 122.5(7) . . ? C322 C323 C324 117.5(8) . . ? C325 C324 C323 121.2(8) . . ? C326 C325 C324 116.7(8) . . ? N321 C326 C325 123.3(8) . . ? C415 N411 N412 110.7(5) . . ? N411 N412 C413 106.3(5) . . ? N411 N412 Zn2 135.1(4) . . ? C413 N412 Zn2 118.5(4) . . ? N412 C413 C414 110.0(5) . . ? N412 C413 C422 116.6(5) . . ? C414 C413 C422 133.3(6) . . ? C415 C414 C413 104.4(6) . . ? N411 C415 C414 108.5(5) . . ? C426 N421 C422 118.8(5) . . ? C426 N421 Zn2 127.0(4) . . ? C422 N421 Zn2 114.2(3) . . ? N421 C422 C423 122.8(5) . . ? N421 C422 C413 114.9(5) . . ? C423 C422 C413 122.3(6) . . ? C424 C423 C422 117.6(6) . . ? C425 C424 C423 120.0(6) . . ? C424 C425 C426 118.8(6) . . ? N421 C426 C425 122.1(6) . . ? F21 P2 F23 91.6(4) . . ? F21 P2 F26 178.6(3) . . ? F23 P2 F26 89.0(3) . . ? F21 P2 F24 89.9(3) . . ? F23 P2 F24 91.0(3) . . ? F26 P2 F24 88.8(2) . . ? F21 P2 F22 91.0(4) . . ? F23 P2 F22 177.1(4) . . ? F26 P2 F22 88.5(4) . . ? F24 P2 F22 90.3(3) . . ? F21 P2 F25 90.4(3) . . ? F23 P2 F25 89.5(3) . . ? F26 P2 F25 90.8(2) . . ? F24 P2 F25 179.4(3) . . ? F22 P2 F25 89.1(3) . . ? F32 P3 F32 87.3(6) . 2_656 ? F32 P3 F31 91.6(4) . . ? F32 P3 F31 178.7(4) 2_656 . ? F32 P3 F31 178.7(4) . 2_656 ? F32 P3 F31 91.6(4) 2_656 2_656 ? F31 P3 F31 89.4(6) . 2_656 ? F32 P3 F33 91.3(3) . . ? F32 P3 F33 89.1(3) 2_656 . ? F31 P3 F33 90.2(3) . . ? F31 P3 F33 89.4(3) 2_656 . ? F32 P3 F33 89.1(3) . 2_656 ? F32 P3 F33 91.3(3) 2_656 2_656 ? F31 P3 F33 89.4(3) . 2_656 ? F31 P3 F33 90.2(3) 2_656 2_656 ? F33 P3 F33 179.4(4) . 2_656 ? C1 C2 O3 113.5(19) . . ? C4 O3 C2 160.0(15) . . ? C5 C4 O3 108.0(19) . . ? O8 C8 C6 126.0(19) . . ? O8 C8 C7 118.3(15) . . ? C6 C8 C7 115.0(18) . . ? _refine_diff_density_max 0.787 _refine_diff_density_min -0.670 _refine_diff_density_rms 0.092 #=END