# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Yanhui Yang' _publ_contact_author_email YHYANG@NTU.EDU.SG _publ_section_title ; Mesostructured molecular solid material |Co(en)3|(Zr2F11H2O) with enhanced photoelectronic effect ; loop_ _publ_author_name 'Yanhui Yang' 'Yuan Chen' 'Yu Du' 'Jihong Yu' # Attachment 'C.CIF' data_c _database_code_depnum_ccdc_archive 'CCDC 687043' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C6 H26 Co F11 N6 O Zr2' _chemical_formula_sum 'C6 H26 Co F11 N6 O Zr2' _chemical_formula_weight 648.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.4266(6) _cell_length_b 14.9640(11) _cell_length_c 14.1234(10) _cell_angle_alpha 90.00 _cell_angle_beta 97.234(2) _cell_angle_gamma 90.00 _cell_volume 1766.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 252 _cell_measurement_theta_min 1.99 _cell_measurement_theta_max 28.22 _exptl_crystal_description block-like _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 2.208 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3509 _exptl_absorpt_correction_T_max 0.5572 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 10817 _diffrn_reflns_av_R_equivalents 0.0620 _diffrn_reflns_av_sigmaI/netI 0.0705 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 28.22 _reflns_number_total 4008 _reflns_number_gt 3134 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+5.8396P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4008 _refine_ls_number_parameters 252 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1096 _refine_ls_wR_factor_gt 0.0991 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.09336(7) 0.10480(4) 0.45969(4) 0.01955(15) Uani 1 1 d . . . Zr2 Zr 0.24379(7) 0.32144(4) 0.38577(4) 0.01867(14) Uani 1 1 d . . . Co1 Co 0.31106(10) 0.69170(5) 0.33224(6) 0.01993(19) Uani 1 1 d . . . F1 F -0.1275(4) 0.0315(2) 0.4901(2) 0.0270(8) Uani 1 1 d . . . F2 F 0.0325(4) 0.0360(2) 0.3374(2) 0.0286(8) Uani 1 1 d . . . F3 F 0.3238(4) 0.0882(3) 0.4700(3) 0.0406(10) Uani 1 1 d . . . F4 F -0.0997(4) 0.1877(2) 0.4325(3) 0.0321(9) Uani 1 1 d . . . F5 F 0.1896(5) 0.2395(2) 0.5044(2) 0.0298(9) Uani 1 1 d . . . F6 F 0.1541(5) 0.1907(2) 0.3431(2) 0.0314(9) Uani 1 1 d . . . F7 F 0.0226(4) 0.3627(3) 0.3551(3) 0.0381(10) Uani 1 1 d . . . F8 F 0.2974(5) 0.3957(2) 0.5038(3) 0.0320(9) Uani 1 1 d . . . F9 F 0.4753(4) 0.2793(2) 0.4080(3) 0.0314(9) Uani 1 1 d . . . F10 F 0.2670(5) 0.3034(2) 0.2418(2) 0.0310(9) Uani 1 1 d . . . F11 F 0.3158(6) 0.4403(3) 0.3368(3) 0.0472(12) Uani 1 1 d . . . O1 O 0.0817(6) 0.1173(3) 0.6146(3) 0.0296(11) Uani 1 1 d . . . H1W H 0.147(7) 0.144(4) 0.651(4) 0.013(16) Uiso 1 1 d . . . H2W H 0.048(12) 0.064(7) 0.625(7) 0.10(4) Uiso 1 1 d . . . C1 C 0.2900(10) 0.8735(5) 0.2776(6) 0.045(2) Uani 1 1 d . . . H1A H 0.3330 0.9173 0.2370 0.080 Uiso 1 1 calc . . . H1B H 0.1809 0.8905 0.2843 0.080 Uiso 1 1 calc . . . C2 C 0.3863(10) 0.8732(5) 0.3720(5) 0.0415(18) Uani 1 1 d . . . H2A H 0.3636 0.9261 0.4075 0.080 Uiso 1 1 calc . . . H2B H 0.4993 0.8730 0.3649 0.080 Uiso 1 1 calc . . . C3 C 0.0391(8) 0.6099(5) 0.3935(5) 0.0337(16) Uani 1 1 d . . . H3A H 0.0372 0.5564 0.3546 0.080 Uiso 1 1 calc . . . H3B H -0.0648 0.6169 0.4155 0.080 Uiso 1 1 calc . . . C4 C 0.1684(8) 0.6032(5) 0.4773(5) 0.0325(15) Uani 1 1 d . . . H4A H 0.1627 0.6535 0.5201 0.080 Uiso 1 1 calc . . . H4B H 0.1571 0.5484 0.5125 0.080 Uiso 1 1 calc . . . C5 C 0.4422(8) 0.5874(4) 0.1936(5) 0.0303(15) Uani 1 1 d . . . H5A H 0.4539 0.6331 0.1463 0.080 Uiso 1 1 calc . . . H5B H 0.4454 0.5293 0.1635 0.080 Uiso 1 1 calc . . . C6 C 0.5738(8) 0.5952(4) 0.2761(5) 0.0306(15) Uani 1 1 d . . . H6A H 0.5734 0.5436 0.3177 0.080 Uiso 1 1 calc . . . H6B H 0.6772 0.5987 0.2530 0.080 Uiso 1 1 calc . . . N1 N 0.2910(6) 0.7839(3) 0.2328(4) 0.0253(12) Uani 1 1 d . . . H1C H 0.3735 0.7799 0.1982 0.080 Uiso 1 1 calc . . . H1D H 0.1997 0.7757 0.1932 0.080 Uiso 1 1 calc . . . N2 N 0.3450(6) 0.7921(4) 0.4232(4) 0.0284(12) Uani 1 1 d . . . H2C H 0.2555 0.8017 0.4504 0.080 Uiso 1 1 calc . . . H2D H 0.4247 0.7787 0.4696 0.080 Uiso 1 1 calc . . . N3 N 0.0777(6) 0.6902(4) 0.3370(4) 0.0286(12) Uani 1 1 d . . . H3C H 0.0474 0.7404 0.3648 0.080 Uiso 1 1 calc . . . H3D H 0.0252 0.6873 0.2775 0.080 Uiso 1 1 calc . . . N4 N 0.3228(6) 0.6039(3) 0.4368(4) 0.0259(12) Uani 1 1 d . . . H4C H 0.3428 0.5492 0.4146 0.080 Uiso 1 1 calc . . . H4D H 0.4029 0.6184 0.4825 0.080 Uiso 1 1 calc . . . N5 N 0.2882(6) 0.5993(3) 0.2342(4) 0.0244(11) Uani 1 1 d . . . H5C H 0.2601 0.5474 0.2597 0.080 Uiso 1 1 calc . . . H5D H 0.2105 0.6148 0.1875 0.080 Uiso 1 1 calc . . . N6 N 0.5418(6) 0.6783(3) 0.3285(4) 0.0248(11) Uani 1 1 d . . . H6C H 0.5792 0.7259 0.2992 0.080 Uiso 1 1 calc . . . H6D H 0.5928 0.6758 0.3884 0.080 Uiso 1 1 calc . . . 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 Zr1 0.0209(3) 0.0186(3) 0.0190(3) 0.0009(2) 0.0020(2) -0.0009(2) Zr2 0.0202(3) 0.0181(3) 0.0178(3) 0.0013(2) 0.0027(2) -0.0005(2) Co1 0.0212(4) 0.0197(4) 0.0187(4) 0.0008(3) 0.0020(3) 0.0001(3) F1 0.026(2) 0.0239(18) 0.031(2) 0.0035(16) 0.0032(15) 0.0000(15) F2 0.039(2) 0.0257(18) 0.0211(18) -0.0030(15) 0.0028(16) -0.0036(17) F3 0.024(2) 0.039(2) 0.059(3) 0.012(2) 0.0056(19) -0.0009(18) F4 0.031(2) 0.0240(19) 0.041(2) 0.0029(17) 0.0041(17) 0.0004(16) F5 0.043(2) 0.0265(19) 0.0200(18) -0.0005(15) 0.0048(16) -0.0084(17) F6 0.047(2) 0.0244(19) 0.0234(19) -0.0025(15) 0.0074(17) -0.0066(17) F7 0.027(2) 0.045(2) 0.043(2) 0.007(2) 0.0040(18) 0.0113(19) F8 0.044(2) 0.0240(19) 0.028(2) -0.0066(16) 0.0042(17) -0.0041(17) F9 0.024(2) 0.039(2) 0.031(2) 0.0020(17) 0.0036(16) 0.0050(17) F10 0.042(2) 0.030(2) 0.0214(18) 0.0026(16) 0.0071(16) 0.0084(18) F11 0.082(3) 0.026(2) 0.036(2) 0.0014(18) 0.018(2) -0.010(2) O1 0.037(3) 0.027(3) 0.023(2) -0.005(2) -0.003(2) -0.014(2) C1 0.063(6) 0.028(4) 0.042(4) 0.004(3) 0.005(4) 0.003(4) C2 0.057(5) 0.029(4) 0.040(4) -0.001(3) 0.010(4) -0.009(4) C3 0.026(4) 0.038(4) 0.039(4) 0.002(3) 0.008(3) -0.006(3) C4 0.035(4) 0.036(4) 0.029(3) 0.001(3) 0.016(3) -0.006(3) C5 0.041(4) 0.020(3) 0.031(4) -0.003(3) 0.010(3) 0.006(3) C6 0.025(3) 0.031(3) 0.037(4) -0.004(3) 0.008(3) 0.002(3) N1 0.030(3) 0.021(3) 0.025(3) 0.004(2) 0.005(2) 0.002(2) N2 0.031(3) 0.032(3) 0.021(3) -0.005(2) 0.000(2) 0.002(2) N3 0.026(3) 0.034(3) 0.027(3) -0.002(2) 0.004(2) -0.004(2) N4 0.027(3) 0.024(3) 0.027(3) 0.003(2) 0.002(2) 0.000(2) N5 0.021(3) 0.024(3) 0.027(3) -0.003(2) -0.001(2) -0.002(2) N6 0.022(3) 0.030(3) 0.022(3) 0.003(2) -0.002(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 F3 1.945(4) . ? Zr1 F2 2.020(3) . ? Zr1 F4 2.044(4) . ? Zr1 F1 2.167(3) 3_556 ? Zr1 F6 2.200(4) . ? Zr1 O1 2.210(5) . ? Zr1 F5 2.234(3) . ? Zr1 F1 2.247(4) . ? Zr1 Zr2 3.6795(8) . ? Zr2 F7 1.960(4) . ? Zr2 F8 2.008(3) . ? Zr2 F11 2.029(4) . ? Zr2 F9 2.037(4) . ? Zr2 F10 2.085(4) . ? Zr2 F6 2.156(3) . ? Zr2 F5 2.170(3) . ? Co1 N5 1.949(5) . ? Co1 N1 1.961(5) . ? Co1 N6 1.962(5) . ? Co1 N4 1.970(5) . ? Co1 N2 1.973(5) . ? Co1 N3 1.976(5) . ? F1 Zr1 2.167(3) 3_556 ? O1 H1W 0.81(6) . ? O1 H2W 0.86(11) . ? C1 C2 1.471(10) . ? C1 N1 1.484(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.477(9) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N3 1.501(8) . ? C3 C4 1.507(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N4 1.486(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N5 1.493(8) . ? C5 C6 1.509(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N6 1.489(8) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? N1 H1C 0.9000 . ? N1 H1D 0.9000 . ? N2 H2C 0.9000 . ? N2 H2D 0.9000 . ? N3 H3C 0.9000 . ? N3 H3D 0.9000 . ? N4 H4C 0.9000 . ? N4 H4D 0.9000 . ? N5 H5C 0.9000 . ? N5 H5D 0.9000 . ? N6 H6C 0.9000 . ? N6 H6D 0.9000 . ? 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 F3 Zr1 F2 98.19(17) . . ? F3 Zr1 F4 148.81(16) . . ? F2 Zr1 F4 92.22(15) . . ? F3 Zr1 F1 76.40(15) . 3_556 ? F2 Zr1 F1 78.99(14) . 3_556 ? F4 Zr1 F1 134.64(14) . 3_556 ? F3 Zr1 F6 78.86(16) . . ? F2 Zr1 F6 73.51(13) . . ? F4 Zr1 F6 76.08(15) . . ? F1 Zr1 F6 139.60(14) 3_556 . ? F3 Zr1 O1 96.04(18) . . ? F2 Zr1 O1 148.29(16) . . ? F4 Zr1 O1 90.05(17) . . ? F1 Zr1 O1 77.05(16) 3_556 . ? F6 Zr1 O1 137.33(16) . . ? F3 Zr1 F5 76.76(16) . . ? F2 Zr1 F5 138.20(13) . . ? F4 Zr1 F5 75.94(14) . . ? F1 Zr1 F5 136.76(13) 3_556 . ? F6 Zr1 F5 64.76(12) . . ? O1 Zr1 F5 72.79(16) . . ? F3 Zr1 F1 140.01(15) . . ? F2 Zr1 F1 77.71(14) . . ? F4 Zr1 F1 70.93(13) . . ? F1 Zr1 F1 63.71(15) 3_556 . ? F6 Zr1 F1 134.78(13) . . ? O1 Zr1 F1 73.20(16) . . ? F5 Zr1 F1 131.77(13) . . ? F3 Zr1 Zr2 75.97(11) . . ? F2 Zr1 Zr2 105.43(10) . . ? F4 Zr1 Zr2 72.92(10) . . ? F1 Zr1 Zr2 152.38(10) 3_556 . ? F6 Zr1 Zr2 31.98(9) . . ? O1 Zr1 Zr2 105.45(13) . . ? F5 Zr1 Zr2 32.79(9) . . ? F1 Zr1 Zr2 143.82(9) . . ? F7 Zr2 F8 96.71(16) . . ? F7 Zr2 F11 88.01(18) . . ? F8 Zr2 F11 75.62(15) . . ? F7 Zr2 F9 176.09(16) . . ? F8 Zr2 F9 86.15(15) . . ? F11 Zr2 F9 90.13(18) . . ? F7 Zr2 F10 91.67(16) . . ? F8 Zr2 F10 147.46(15) . . ? F11 Zr2 F10 73.31(15) . . ? F9 Zr2 F10 84.50(15) . . ? F7 Zr2 F6 86.22(16) . . ? F8 Zr2 F6 140.28(14) . . ? F11 Zr2 F6 144.08(15) . . ? F9 Zr2 F6 93.28(15) . . ? F10 Zr2 F6 71.46(14) . . ? F7 Zr2 F5 93.54(15) . . ? F8 Zr2 F5 73.68(14) . . ? F11 Zr2 F5 149.23(15) . . ? F9 Zr2 F5 89.82(14) . . ? F10 Zr2 F5 137.24(13) . . ? F6 Zr2 F5 66.60(13) . . ? F7 Zr2 Zr1 89.34(12) . . ? F8 Zr2 Zr1 107.57(11) . . ? F11 Zr2 Zr1 176.09(13) . . ? F9 Zr2 Zr1 92.34(11) . . ? F10 Zr2 Zr1 103.91(10) . . ? F6 Zr2 Zr1 32.72(9) . . ? F5 Zr2 Zr1 33.89(9) . . ? N5 Co1 N1 89.9(2) . . ? N5 Co1 N6 85.3(2) . . ? N1 Co1 N6 92.8(2) . . ? N5 Co1 N4 92.9(2) . . ? N1 Co1 N4 176.4(2) . . ? N6 Co1 N4 89.7(2) . . ? N5 Co1 N2 174.6(2) . . ? N1 Co1 N2 85.6(2) . . ? N6 Co1 N2 91.8(2) . . ? N4 Co1 N2 91.7(2) . . ? N5 Co1 N3 90.4(2) . . ? N1 Co1 N3 92.0(2) . . ? N6 Co1 N3 173.5(2) . . ? N4 Co1 N3 85.6(2) . . ? N2 Co1 N3 92.9(2) . . ? Zr1 F1 Zr1 116.29(15) 3_556 . ? Zr2 F5 Zr1 113.32(15) . . ? Zr2 F6 Zr1 115.30(15) . . ? Zr1 O1 H1W 124(4) . . ? Zr1 O1 H2W 99(7) . . ? H1W O1 H2W 124(8) . . ? C2 C1 N1 110.6(6) . . ? C2 C1 H1A 109.5 . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? C1 C2 N2 108.1(6) . . ? C1 C2 H2A 110.1 . . ? N2 C2 H2A 110.1 . . ? C1 C2 H2B 110.1 . . ? N2 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? N3 C3 C4 106.7(5) . . ? N3 C3 H3A 110.4 . . ? C4 C3 H3A 110.4 . . ? N3 C3 H3B 110.4 . . ? C4 C3 H3B 110.4 . . ? H3A C3 H3B 108.6 . . ? N4 C4 C3 106.2(5) . . ? N4 C4 H4A 110.5 . . ? C3 C4 H4A 110.5 . . ? N4 C4 H4B 110.5 . . ? C3 C4 H4B 110.5 . . ? H4A C4 H4B 108.7 . . ? N5 C5 C6 106.5(5) . . ? N5 C5 H5A 110.4 . . ? C6 C5 H5A 110.4 . . ? N5 C5 H5B 110.4 . . ? C6 C5 H5B 110.4 . . ? H5A C5 H5B 108.6 . . ? N6 C6 C5 106.7(5) . . ? N6 C6 H6A 110.4 . . ? C5 C6 H6A 110.4 . . ? N6 C6 H6B 110.4 . . ? C5 C6 H6B 110.4 . . ? H6A C6 H6B 108.6 . . ? C1 N1 Co1 109.6(4) . . ? C1 N1 H1C 109.8 . . ? Co1 N1 H1C 109.8 . . ? C1 N1 H1D 109.8 . . ? Co1 N1 H1D 109.8 . . ? H1C N1 H1D 108.2 . . ? C2 N2 Co1 109.3(4) . . ? C2 N2 H2C 109.8 . . ? Co1 N2 H2C 109.8 . . ? C2 N2 H2D 109.8 . . ? Co1 N2 H2D 109.8 . . ? H2C N2 H2D 108.3 . . ? C3 N3 Co1 108.1(4) . . ? C3 N3 H3C 110.1 . . ? Co1 N3 H3C 110.1 . . ? C3 N3 H3D 110.1 . . ? Co1 N3 H3D 110.1 . . ? H3C N3 H3D 108.4 . . ? C4 N4 Co1 109.2(4) . . ? C4 N4 H4C 109.8 . . ? Co1 N4 H4C 109.8 . . ? C4 N4 H4D 109.8 . . ? Co1 N4 H4D 109.8 . . ? H4C N4 H4D 108.3 . . ? C5 N5 Co1 110.1(4) . . ? C5 N5 H5C 109.6 . . ? Co1 N5 H5C 109.6 . . ? C5 N5 H5D 109.6 . . ? Co1 N5 H5D 109.6 . . ? H5C N5 H5D 108.1 . . ? C6 N6 Co1 109.9(4) . . ? C6 N6 H6C 109.7 . . ? Co1 N6 H6C 109.7 . . ? C6 N6 H6D 109.7 . . ? Co1 N6 H6D 109.7 . . ? H6C N6 H6D 108.2 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1W F10 0.81(6) 1.72(6) 2.524(6) 171(6) 4_566 O1 H2W F2 0.86(11) 1.76(11) 2.609(6) 171(10) 3_556 N1 H1C F9 0.90 2.09 2.970(6) 166.6 2_655 N1 H1D F4 0.90 2.28 3.028(6) 139.8 2 N1 H1D F7 0.90 2.31 3.015(6) 134.7 2 N2 H2C F4 0.90 2.24 3.095(7) 157.8 3_566 N2 H2D F9 0.90 2.02 2.865(6) 155.6 3_666 N3 H3C O1 0.90 2.43 3.287(7) 160.3 3_566 N3 H3D F6 0.90 2.13 3.005(6) 163.9 2 N4 H4C F11 0.90 1.96 2.822(6) 159.5 . N4 H4D F9 0.90 2.32 3.134(6) 149.9 3_666 N4 H4D F8 0.90 2.52 3.204(6) 133.6 3_666 N5 H5C F11 0.90 1.96 2.780(6) 150.5 . N5 H5D F4 0.90 2.13 2.980(6) 157.1 2 N5 H5D F2 0.90 2.35 2.922(6) 121.3 2 N6 H6C F10 0.90 1.88 2.736(6) 157.3 2_655 N6 H6D F8 0.90 1.99 2.804(6) 149.6 3_666 N6 H6D F5 0.90 2.56 3.296(6) 139.1 3_666 _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.847 _refine_diff_density_min -0.702 _refine_diff_density_rms 0.160