#------------------------------------------------------------------------------ #$Date: 2010-12-09 18:44:53 +0000 (Thu, 09 Dec 2010) $ #$Revision: 3898 $ #$URL: svn://www.crystallography.net/cod/cif/7/7051290.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7051290 loop_ _publ_author_name 'Mondry, Anna' 'Starynowicz, Przemys\/law' _publ_section_title ; Structure and optical spectroscopy of holmium(III) triethylenetetraaminehexaacetate in single crystal and in solution ; _journal_issue 8 _journal_name_full 'New Journal of Chemistry' _journal_page_first 603 _journal_volume 24 _journal_year 2000 _chemical_formula_sum 'C21 H48 Ho N13 O15' _chemical_formula_weight 887.65 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 71.89(3) _cell_angle_beta 81.55(3) _cell_angle_gamma 68.90(3) _cell_formula_units_Z 2 _cell_length_a 9.535(2) _cell_length_b 12.520(3) _cell_length_c 17.012(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 13.5 _cell_measurement_theta_min 9 _cell_volume 1799.4(8) _computing_cell_refinement 'Kuma KM4 software (1996)' _computing_data_collection 'Kuma KM4 software (1996)' _computing_data_reduction 'Kuma KM4 software (1996)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS (Sheldrick, 1986)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type 'Kuma KM4' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0138 _diffrn_reflns_av_sigmaI/netI 0.0194 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 5333 _diffrn_reflns_theta_full 23.05 _diffrn_reflns_theta_max 23. _diffrn_reflns_theta_min 2. _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.280 _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_meas 1.65 _exptl_crystal_density_method 'flotation in CH3Cl/CH3Br' _exptl_crystal_description parallelepiped _exptl_crystal_F_000 904 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _refine_diff_density_max 2.289 _refine_diff_density_min -1.556 _refine_diff_density_rms 0.121 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 5.609 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 451 _refine_ls_number_reflns 4975 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 5.609 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0351 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_gt 0.1021 _refine_ls_wR_factor_ref 0.1022 _reflns_number_gt 4960 _reflns_number_total 5332 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file b001480j.txt _[local]_cod_data_source_block anka4 _cod_original_cell_volume 1799.4(7) _cod_database_code 7051290 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ho Ho 0.21269(4) 0.30125(3) 0.25427(2) 0.02301(13) Uani 1 d . . . O1 O 0.1433(6) 0.5079(4) 0.2284(3) 0.0322(13) Uani 1 d . . . O2 O 0.1042(9) 0.6918(5) 0.1470(4) 0.074(3) Uani 1 d . . . O3 O 0.0743(6) 0.3485(5) 0.1330(3) 0.0338(13) Uani 1 d . . . O4 O 0.1010(7) 0.3113(5) 0.0109(3) 0.0468(16) Uani 1 d . . . O5 O 0.2134(6) 0.3266(5) 0.3839(3) 0.0330(13) Uani 1 d . . . O6 O 0.2760(8) 0.4110(6) 0.4638(4) 0.064(2) Uani 1 d . . . O7 O 0.3308(7) 0.1549(5) 0.1880(3) 0.0393(15) Uani 1 d . . . O8 O 0.4668(8) -0.0208(6) 0.1713(4) 0.064(2) Uani 1 d . . . O9 O -0.0411(6) 0.3731(4) 0.2911(3) 0.0316(13) Uani 1 d . . . O10 O -0.2240(7) 0.3749(5) 0.3868(4) 0.0489(17) Uani 1 d . . . O11 O -0.0854(7) -0.0196(5) 0.3822(4) 0.0468(16) Uani 1 d . . . O12 O -0.1198(8) 0.0176(6) 0.2482(4) 0.0568(19) Uani 1 d . . . OW1 O 0.3088(9) 0.0661(7) 0.0289(5) 0.079(2) Uani 1 d . . . OW2 O 0.5039(16) 0.2717(9) 0.5887(9) 0.205(7) Uani 1 d . . . OW3 O -0.2806(14) 0.3507(10) 0.5521(8) 0.159(5) Uani 1 d . . . N1 N 0.3215(7) 0.4052(6) 0.1121(4) 0.0305(16) Uani 1 d . . . N2 N 0.4527(7) 0.3435(6) 0.2741(4) 0.0323(16) Uani 1 d . . . N3 N 0.4164(7) 0.1039(6) 0.3435(4) 0.0304(16) Uani 1 d . . . N4 N 0.0947(7) 0.1386(5) 0.3415(4) 0.0256(15) Uani 1 d . . . N21 N -0.2255(10) 0.0258(8) 0.0986(5) 0.072(3) Uani 1 d . . . H21A H -0.2716 -0.0096 0.0810 0.086 Uiso 1 calc R . . H21B H -0.2134 0.0087 0.1507 0.086 Uiso 1 calc R . . N22 N -0.1041(10) 0.1615(7) 0.0741(5) 0.065(3) Uani 1 d . . . H22A H -0.0710 0.2149 0.0401 0.078 Uiso 1 calc R . . H22B H -0.0925 0.1438 0.1264 0.078 Uiso 1 calc R . . N23 N -0.1929(12) 0.1307(7) -0.0332(5) 0.081(3) Uani 1 d . . . H23A H -0.2392 0.0947 -0.0499 0.097 Uiso 1 calc R . . H23B H -0.1594 0.1830 -0.0684 0.097 Uiso 1 calc R . . N31 N 0.6500(10) 0.6167(7) 0.2663(5) 0.062(2) Uani 1 d . . . H31A H 0.6899 0.5450 0.2966 0.074 Uiso 1 calc R . . H31B H 0.5781 0.6671 0.2864 0.074 Uiso 1 calc R . . N32 N 0.8068(8) 0.5749(6) 0.1578(4) 0.048(2) Uani 1 d . . . H32A H 0.8481 0.5029 0.1871 0.058 Uiso 1 calc R . . H32B H 0.8373 0.5979 0.1073 0.058 Uiso 1 calc R . . N33 N 0.6309(11) 0.7605(7) 0.1437(5) 0.084(3) Uani 1 d . . . H33A H 0.6592 0.7831 0.0927 0.101 Uiso 1 calc R . . H33B H 0.5591 0.8094 0.1651 0.101 Uiso 1 calc R . . N41 N -0.1417(9) 0.7598(7) 0.4190(5) 0.057(2) Uani 1 d . . . H41A H -0.1531 0.8342 0.4083 0.069 Uiso 1 calc R . . H41B H -0.1697 0.7225 0.4668 0.069 Uiso 1 calc R . . N42 N -0.0685(10) 0.5883(7) 0.3796(6) 0.067(3) Uani 1 d . . . H42A H -0.0996 0.5526 0.4271 0.080 Uiso 1 calc R . . H42B H -0.0292 0.5501 0.3432 0.080 Uiso 1 calc R . . N43 N -0.0387(11) 0.7607(7) 0.2897(5) 0.072(3) Uani 1 d . . . H43A H -0.0505 0.8351 0.2792 0.086 Uiso 1 calc R . . H43B H 0.0009 0.7240 0.2524 0.086 Uiso 1 calc R . . C1 C 0.1572(10) 0.5816(8) 0.1605(5) 0.040(2) Uani 1 d . . . C2 C 0.2407(10) 0.5347(7) 0.0894(5) 0.037(2) Uani 1 d . . . H2A H 0.1695 0.5539 0.0477 0.044 Uiso 1 calc R . . H2B H 0.3125 0.5755 0.0648 0.044 Uiso 1 calc R . . C3 C 0.1445(10) 0.3380(7) 0.0658(5) 0.033(2) Uani 1 d . . . C4 C 0.2942(9) 0.3548(7) 0.0498(5) 0.036(2) Uani 1 d . . . H4A H 0.3724 0.2787 0.0518 0.043 Uiso 1 calc R . . H4B H 0.2983 0.4082 -0.0051 0.043 Uiso 1 calc R . . C5 C 0.4831(9) 0.3788(8) 0.1215(5) 0.038(2) Uani 1 d . . . H5A H 0.5243 0.4219 0.0714 0.046 Uiso 1 calc R . . H5B H 0.5359 0.2942 0.1292 0.046 Uiso 1 calc R . . C6 C 0.5086(10) 0.4136(8) 0.1946(5) 0.041(2) Uani 1 d . . . H6A H 0.6151 0.3986 0.1975 0.049 Uiso 1 calc R . . H6B H 0.4560 0.4981 0.1871 0.049 Uiso 1 calc R . . C7 C 0.2912(10) 0.3813(7) 0.3996(5) 0.038(2) Uani 1 d . . . C8 C 0.4098(10) 0.4117(7) 0.3370(5) 0.038(2) Uani 1 d . . . H8A H 0.3733 0.4963 0.3088 0.046 Uiso 1 calc R . . H8B H 0.4989 0.3960 0.3658 0.046 Uiso 1 calc R . . C9 C 0.5765(9) 0.2301(7) 0.3043(5) 0.041(2) Uani 1 d . . . H9A H 0.6553 0.2467 0.3234 0.050 Uiso 1 calc R . . H9B H 0.6186 0.1958 0.2586 0.050 Uiso 1 calc R . . C10 C 0.5274(9) 0.1414(7) 0.3727(5) 0.039(2) Uani 1 d . . . H10A H 0.4818 0.1761 0.4178 0.046 Uiso 1 calc R . . H10B H 0.6143 0.0721 0.3933 0.046 Uiso 1 calc R . . C11 C 0.4268(10) 0.0509(7) 0.2124(5) 0.037(2) Uani 1 d . . . C12 C 0.4981(10) 0.0182(7) 0.2947(5) 0.039(2) Uani 1 d . . . H12A H 0.4989 -0.0611 0.3266 0.047 Uiso 1 calc R . . H12B H 0.6016 0.0164 0.2844 0.047 Uiso 1 calc R . . C13 C 0.3332(9) 0.0477(7) 0.4141(5) 0.035(2) Uani 1 d . . . H13A H 0.2933 0.0991 0.4504 0.042 Uiso 1 calc R . . H13B H 0.4016 -0.0273 0.4453 0.042 Uiso 1 calc R . . C14 C 0.2053(9) 0.0252(7) 0.3866(5) 0.037(2) Uani 1 d . . . H14A H 0.2448 -0.0270 0.3509 0.044 Uiso 1 calc R . . H14B H 0.1556 -0.0144 0.4347 0.044 Uiso 1 calc R . . C15 C -0.1004(9) 0.3242(7) 0.3556(5) 0.0281(18) Uani 1 d . . . C16 C -0.0199(9) 0.1971(7) 0.3975(5) 0.0306(19) Uani 1 d . . . H16A H 0.0286 0.1922 0.4454 0.037 Uiso 1 calc R . . H16B H -0.0919 0.1552 0.4167 0.037 Uiso 1 calc R . . C17 C -0.0680(10) 0.0298(7) 0.3095(6) 0.039(2) Uani 1 d . . . C18 C 0.0180(9) 0.1197(7) 0.2795(5) 0.033(2) Uani 1 d . . . H18A H 0.0934 0.0944 0.2380 0.040 Uiso 1 calc R . . H18B H -0.0526 0.1963 0.2519 0.040 Uiso 1 calc R . . C20 C -0.1734(12) 0.1059(8) 0.0458(6) 0.053(3) Uani 1 d . . . C30 C 0.6987(11) 0.6489(8) 0.1898(6) 0.046(2) Uani 1 d . . . C40 C -0.0812(11) 0.7030(8) 0.3625(6) 0.047(2) 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 Ho 0.0274(2) 0.0205(2) 0.0208(2) -0.00400(16) -0.00110(16) -0.00902(17) O1 0.048(4) 0.022(3) 0.027(3) -0.004(3) 0.006(3) -0.017(3) O2 0.132(7) 0.020(4) 0.048(4) -0.005(3) 0.025(4) -0.016(4) O3 0.037(3) 0.034(3) 0.026(3) -0.003(3) -0.006(3) -0.010(3) O4 0.064(4) 0.054(4) 0.033(4) -0.013(3) -0.007(3) -0.029(4) O5 0.044(4) 0.033(3) 0.024(3) -0.005(3) -0.001(3) -0.017(3) O6 0.100(6) 0.089(6) 0.036(4) -0.035(4) 0.013(4) -0.061(5) O7 0.050(4) 0.027(3) 0.030(3) -0.010(3) -0.010(3) 0.005(3) O8 0.082(5) 0.041(4) 0.067(5) -0.040(4) -0.017(4) 0.009(4) O9 0.033(3) 0.026(3) 0.030(3) -0.002(3) 0.003(3) -0.010(3) O10 0.043(4) 0.040(4) 0.053(4) -0.012(3) 0.012(3) -0.008(3) O11 0.066(5) 0.041(4) 0.042(4) -0.006(3) 0.000(3) -0.032(3) O12 0.073(5) 0.056(4) 0.061(5) -0.019(4) -0.016(4) -0.037(4) OW1 0.102(7) 0.074(5) 0.072(5) -0.034(4) -0.023(5) -0.025(5) OW2 0.228(16) 0.080(8) 0.300(18) -0.054(10) -0.133(14) 0.005(9) OW3 0.186(13) 0.153(11) 0.167(12) -0.075(9) 0.040(10) -0.084(10) N1 0.037(4) 0.030(4) 0.026(4) -0.011(3) 0.003(3) -0.012(3) N2 0.036(4) 0.033(4) 0.030(4) -0.006(3) -0.001(3) -0.017(3) N3 0.029(4) 0.031(4) 0.027(4) -0.007(3) -0.011(3) -0.002(3) N4 0.033(4) 0.024(4) 0.022(3) -0.004(3) -0.003(3) -0.014(3) N21 0.101(8) 0.090(7) 0.048(5) -0.003(5) -0.003(5) -0.074(7) N22 0.085(7) 0.055(6) 0.066(6) -0.009(5) -0.012(5) -0.040(5) N23 0.147(10) 0.063(6) 0.043(6) 0.003(5) -0.015(6) -0.058(7) N31 0.082(7) 0.042(5) 0.048(5) -0.013(4) 0.011(5) -0.010(5) N32 0.051(5) 0.039(5) 0.036(4) -0.005(4) -0.001(4) 0.002(4) N33 0.130(9) 0.031(5) 0.054(6) -0.007(4) 0.004(6) 0.008(5) N41 0.098(7) 0.039(5) 0.044(5) -0.017(4) 0.017(5) -0.036(5) N42 0.090(7) 0.036(5) 0.080(7) -0.023(5) 0.002(6) -0.024(5) N43 0.126(9) 0.046(5) 0.049(5) -0.029(4) 0.025(6) -0.033(6) C1 0.052(6) 0.034(5) 0.033(5) -0.010(4) 0.006(4) -0.016(5) C2 0.047(6) 0.032(5) 0.028(5) -0.003(4) 0.000(4) -0.016(4) C3 0.044(5) 0.026(5) 0.023(5) 0.002(4) -0.008(4) -0.008(4) C4 0.048(6) 0.039(5) 0.023(4) -0.010(4) 0.006(4) -0.018(4) C5 0.041(5) 0.045(5) 0.033(5) -0.013(4) 0.010(4) -0.021(4) C6 0.040(5) 0.051(6) 0.038(5) -0.009(4) 0.007(4) -0.030(5) C7 0.050(6) 0.034(5) 0.034(5) -0.005(4) -0.007(4) -0.020(5) C8 0.047(6) 0.041(5) 0.036(5) -0.013(4) -0.001(4) -0.024(5) C9 0.035(5) 0.042(5) 0.046(6) -0.010(4) -0.008(4) -0.012(4) C10 0.030(5) 0.039(5) 0.044(5) -0.008(4) -0.010(4) -0.008(4) C11 0.035(5) 0.033(5) 0.039(5) -0.010(4) 0.003(4) -0.007(4) C12 0.037(5) 0.032(5) 0.041(5) -0.008(4) -0.009(4) -0.003(4) C13 0.038(5) 0.032(5) 0.029(5) 0.003(4) -0.009(4) -0.012(4) C14 0.044(5) 0.028(5) 0.034(5) -0.003(4) -0.005(4) -0.011(4) C15 0.030(5) 0.029(5) 0.032(5) -0.013(4) -0.001(4) -0.014(4) C16 0.038(5) 0.034(5) 0.025(4) -0.008(4) -0.002(4) -0.019(4) C17 0.038(5) 0.031(5) 0.056(6) -0.018(5) -0.007(5) -0.013(4) C18 0.041(5) 0.036(5) 0.030(5) -0.013(4) -0.001(4) -0.019(4) C20 0.066(7) 0.041(6) 0.047(6) -0.004(5) 0.000(5) -0.022(5) C30 0.067(7) 0.037(6) 0.034(5) -0.006(4) -0.006(5) -0.018(5) C40 0.058(7) 0.034(6) 0.056(7) -0.019(5) -0.004(5) -0.017(5) 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' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Ho O9 127.8(2) . . yes O7 Ho O5 137.28(19) . . yes O9 Ho O5 76.41(19) . . yes O7 Ho O1 139.81(18) . . yes O9 Ho O1 72.22(18) . . yes O5 Ho O1 76.25(18) . . yes O7 Ho O3 72.09(19) . . yes O9 Ho O3 72.97(19) . . yes O5 Ho O3 147.79(19) . . yes O1 Ho O3 85.07(19) . . yes O7 Ho N2 97.3(2) . . yes O9 Ho N2 134.9(2) . . yes O5 Ho N2 67.49(19) . . yes O1 Ho N2 73.6(2) . . yes O3 Ho N2 131.74(19) . . yes O7 Ho N1 73.6(2) . . yes O9 Ho N1 120.76(19) . . yes O5 Ho N1 128.53(19) . . yes O1 Ho N1 66.53(18) . . yes O3 Ho N1 63.11(19) . . yes N2 Ho N1 68.7(2) . . yes O7 Ho N4 80.4(2) . . yes O9 Ho N4 64.58(18) . . yes O5 Ho N4 81.79(18) . . yes O1 Ho N4 134.96(19) . . yes O3 Ho N4 93.81(18) . . yes N2 Ho N4 131.71(19) . . yes N1 Ho N4 149.42(19) . . yes O7 Ho N3 64.76(18) . . yes O9 Ho N3 125.21(19) . . yes O5 Ho N3 72.55(19) . . yes O1 Ho N3 137.71(19) . . yes O3 Ho N3 134.84(18) . . yes N2 Ho N3 68.5(2) . . yes N1 Ho N3 113.9(2) . . yes N4 Ho N3 67.2(2) . . yes C1 O1 Ho 126.7(5) . . no C3 O3 Ho 119.5(5) . . no C7 O5 Ho 123.4(5) . . no C11 O7 Ho 131.6(5) . . no C15 O9 Ho 123.7(5) . . no C2 N1 C5 111.0(6) . . no C2 N1 C4 109.0(6) . . no C5 N1 C4 112.8(6) . . no C2 N1 Ho 110.1(4) . . no C5 N1 Ho 107.5(5) . . no C4 N1 Ho 106.3(4) . . no C9 N2 C8 109.9(6) . . no C9 N2 C6 107.5(6) . . no C8 N2 C6 110.3(6) . . no C9 N2 Ho 110.3(5) . . no C8 N2 Ho 106.5(5) . . no C6 N2 Ho 112.3(5) . . no C13 N3 C12 109.7(6) . . no C13 N3 C10 110.7(6) . . no C12 N3 C10 109.1(6) . . no C13 N3 Ho 106.8(4) . . no C12 N3 Ho 112.4(4) . . no C10 N3 Ho 108.1(5) . . no C16 N4 C14 112.7(6) . . no C16 N4 C18 109.2(6) . . no C14 N4 C18 111.2(6) . . no C16 N4 Ho 104.8(4) . . no C14 N4 Ho 114.4(5) . . no C18 N4 Ho 104.0(4) . . no O2 C1 O1 124.7(8) . . no O2 C1 C2 116.8(7) . . no O1 C1 C2 118.5(7) . . no N1 C2 C1 114.5(7) . . no O4 C3 O3 125.2(8) . . no O4 C3 C4 116.2(7) . . no O3 C3 C4 118.5(7) . . no N1 C4 C3 110.8(7) . . no N1 C5 C6 111.6(7) . . no N2 C6 C5 110.6(7) . . no O6 C7 O5 124.0(8) . . no O6 C7 C8 117.0(8) . . no O5 C7 C8 119.0(7) . . no N2 C8 C7 113.6(7) . . no N2 C9 C10 113.1(7) . . no C9 C10 N3 110.9(7) . . no O8 C11 O7 122.9(8) . . no O8 C11 C12 119.5(8) . . no O7 C11 C12 117.5(7) . . no N3 C12 C11 112.2(6) . . no N3 C13 C14 111.9(6) . . no N4 C14 C13 110.9(6) . . no O9 C15 O10 124.2(8) . . no O9 C15 C16 117.8(7) . . no O10 C15 C16 118.0(7) . . no N4 C16 C15 111.8(6) . . no O11 C17 O12 125.9(8) . . no O11 C17 C18 122.9(8) . . no O12 C17 C18 111.2(8) . . no N4 C18 C17 118.5(7) . . no N23 C20 N21 119.1(10) . . no N23 C20 N22 121.6(9) . . no N21 C20 N22 119.3(9) . . no N32 C30 N31 121.4(9) . . no N32 C30 N33 120.3(9) . . no N31 C30 N33 118.3(9) . . no N41 C40 N43 119.6(8) . . no N41 C40 N42 119.1(9) . . no N43 C40 N42 121.3(9) . . no 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 Ho O7 2.307(5) . yes Ho O9 2.323(5) . yes Ho O5 2.326(5) . yes Ho O1 2.340(5) . yes Ho O3 2.415(5) . yes Ho N2 2.615(6) . yes Ho N1 2.626(6) . yes Ho N4 2.627(6) . yes Ho N3 2.695(6) . yes O1 C1 1.257(9) . no O2 C1 1.244(10) . no O3 C3 1.256(9) . no O4 C3 1.251(9) . no O5 C7 1.275(9) . no O6 C7 1.233(10) . no O7 C11 1.274(9) . no O8 C11 1.226(9) . no O9 C15 1.244(9) . no O10 C15 1.249(9) . no O11 C17 1.216(10) . no O12 C17 1.287(10) . no N1 C2 1.473(9) . no N1 C5 1.477(10) . no N1 C4 1.485(9) . no N2 C9 1.480(10) . no N2 C8 1.495(9) . no N2 C6 1.506(10) . no N3 C13 1.471(10) . no N3 C12 1.486(10) . no N3 C10 1.499(10) . no N4 C16 1.479(9) . no N4 C14 1.483(9) . no N4 C18 1.487(9) . no N21 C20 1.314(11) . no N22 C20 1.337(12) . no N23 C20 1.308(12) . no N31 C30 1.305(11) . no N32 C30 1.295(11) . no N33 C30 1.343(11) . no N41 C40 1.315(11) . no N42 C40 1.337(11) . no N43 C40 1.315(11) . no C1 C2 1.505(11) . no C3 C4 1.490(11) . no C5 C6 1.515(11) . no C7 C8 1.504(11) . no C9 C10 1.489(11) . no C11 C12 1.521(11) . no C13 C14 1.511(11) . no C15 C16 1.485(10) . no C17 C18 1.544(11) . no