#------------------------------------------------------------------------------ #$Date: 2025-08-20 20:19:29 +0100 (Wed, 20 Aug 2025) $ #$Revision: 301836 $ #$URL: svn://www.crystallography.net/cod/cif/4/30/82/4308213.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_4308213 loop_ _publ_author_name 'Timothy J. Boyle' 'Leigh Anna M. Ottley' 'Sherrika D. Daniel-Taylor' 'Louis J. Tribby' 'Scott D. Bunge' 'Alison L. Costello' 'Todd M. Alam' 'John C. Gordon' 'T. Mark MCleskey' _publ_contact_author_address '1001 University Blvd, Albuquerque, NM 87106' _publ_contact_author_email tjboyle@sandia.gov _publ_contact_author_fax '(505) 272-7336' _publ_contact_author_name 'Timothy J. Boyle et.al.' _publ_section_title ; Isostructural neo-Pentoxide Derivatives of Group 3 and the Lanthanide Series Metals for the Production of Ln2O3 Nanoparticles ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3705 _journal_page_last 3713 _journal_paper_doi 10.1021/ic070253u _journal_volume 46 _journal_year 2007 _chemical_formula_moiety 'C60 H132 Ho4 O12' _chemical_formula_sum 'C60 H132 Ho4 O12' _chemical_formula_weight 1705.38 _chemical_name_common '(12) [Ho(m-ONep)2(ONep)]4' _space_group_IT_number 114 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'P -4 2n' _symmetry_space_group_name_H-M 'P -4 21 c' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 18.0400(12) _cell_length_b 18.0400(12) _cell_length_c 11.7617(15) _cell_measurement_reflns_used 849 _cell_measurement_temperature 203(2) _cell_measurement_theta_max 20.60 _cell_measurement_theta_min 2.52 _cell_volume 3827.7(6) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 203(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _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 0.0616 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 26077 _diffrn_reflns_theta_full 25.28 _diffrn_reflns_theta_max 25.28 _diffrn_reflns_theta_min 1.60 _exptl_absorpt_coefficient_mu 4.136 _exptl_absorpt_correction_T_max 0.456 _exptl_absorpt_correction_T_min 0.316 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details SADABS _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_meas ? _exptl_crystal_density_method . _exptl_crystal_description irregular _exptl_crystal_F_000 1712 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.19 _refine_diff_density_max 1.052 _refine_diff_density_min -1.086 _refine_diff_density_rms 0.122 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -10(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.285 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 181 _refine_ls_number_reflns 3480 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.285 _refine_ls_R_factor_all 0.0660 _refine_ls_R_factor_gt 0.0615 _refine_ls_shift/su_max 0.125 _refine_ls_shift/su_mean 0.009 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0163P)^2^+23.6933P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0976 _refine_ls_wR_factor_ref 0.0989 _reflns_number_gt 3349 _reflns_number_total 3480 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic070253usi20070208_065126_09.cif _cod_data_source_block jun073s _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 4308213 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' 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 Ho1 Ho 0.95487(2) 0.86839(2) 1.00066(8) 0.03265(14) Uani 1 1 d . . . O1 O 0.9183(3) 0.7618(3) 1.0034(14) 0.0467(18) Uani 1 1 d . . . O2 O 1.0458(5) 0.9068(4) 0.8844(6) 0.0279(17) Uani 1 1 d . . . O3 O 0.8755(4) 0.9385(4) 0.8981(7) 0.0294(18) Uani 1 1 d . . . C1 C 0.8813(9) 0.6973(7) 1.0381(12) 0.082(6) Uani 1 1 d . . . H1A H 0.8280 0.7061 1.0304 0.098 Uiso 1 1 calc R . . H1B H 0.8915 0.6899 1.1191 0.098 Uiso 1 1 calc R . . C2 C 0.8992(7) 0.6274(6) 0.9780(13) 0.052(4) Uani 1 1 d . . . C3 C 0.9790(9) 0.6114(9) 0.980(4) 0.175(14) Uani 1 1 d . . . H3A H 0.9885 0.5656 0.9392 0.262 Uiso 1 1 calc R . . H3B H 0.9955 0.6063 1.0580 0.262 Uiso 1 1 calc R . . H3C H 1.0057 0.6517 0.9437 0.262 Uiso 1 1 calc R . . C4 C 0.8544(11) 0.5641(8) 1.024(2) 0.119(9) Uani 1 1 d . . . H4A H 0.8058 0.5639 0.9887 0.179 Uiso 1 1 calc R . . H4B H 0.8488 0.5698 1.1058 0.179 Uiso 1 1 calc R . . H4C H 0.8794 0.5177 1.0080 0.179 Uiso 1 1 calc R . . C5 C 0.8872(14) 0.6347(11) 0.8538(16) 0.129(9) Uani 1 1 d . . . H5A H 0.9263 0.6649 0.8212 0.194 Uiso 1 1 calc R . . H5B H 0.8396 0.6579 0.8400 0.194 Uiso 1 1 calc R . . H5C H 0.8879 0.5859 0.8191 0.194 Uiso 1 1 calc R . . C6 C 1.0412(7) 0.9120(6) 0.7640(9) 0.041(3) Uani 1 1 d . . . H6A H 1.0639 0.9587 0.7399 0.050 Uiso 1 1 calc R . . H6B H 0.9888 0.9136 0.7421 0.050 Uiso 1 1 calc R . . C7 C 1.0780(6) 0.8494(6) 0.7016(10) 0.040(3) Uani 1 1 d . . . C8 C 1.1622(7) 0.8500(9) 0.7233(15) 0.068(5) Uani 1 1 d . . . H8A H 1.1826 0.8971 0.6990 0.102 Uiso 1 1 calc R . . H8B H 1.1853 0.8102 0.6808 0.102 Uiso 1 1 calc R . . H8C H 1.1716 0.8431 0.8038 0.102 Uiso 1 1 calc R . . C9 C 1.0625(12) 0.8588(10) 0.5751(11) 0.107(7) Uani 1 1 d . . . H9A H 1.0104 0.8499 0.5603 0.160 Uiso 1 1 calc R . . H9B H 1.0922 0.8237 0.5322 0.160 Uiso 1 1 calc R . . H9C H 1.0752 0.9089 0.5521 0.160 Uiso 1 1 calc R . . C10 C 1.0477(8) 0.7738(7) 0.7387(12) 0.062(4) Uani 1 1 d . . . H10A H 1.0629 0.7637 0.8163 0.093 Uiso 1 1 calc R . . H10B H 1.0671 0.7355 0.6889 0.093 Uiso 1 1 calc R . . H10C H 0.9940 0.7742 0.7343 0.093 Uiso 1 1 calc R . . C11 C 0.8346(13) 0.9237(18) 0.8078(13) 0.204(18) Uani 1 1 d . . . H11A H 0.8701 0.9054 0.7514 0.245 Uiso 1 1 calc R . . H11B H 0.8188 0.9724 0.7802 0.245 Uiso 1 1 calc R . . C12 C 0.7717(6) 0.8782(7) 0.7930(10) 0.040(3) Uani 1 1 d . . . C13 C 0.799(3) 0.8169(13) 0.731(3) 0.29(3) Uani 1 1 d . . . H13A H 0.8009 0.8292 0.6511 0.439 Uiso 1 1 calc R . . H13B H 0.7663 0.7748 0.7426 0.439 Uiso 1 1 calc R . . H13C H 0.8483 0.8045 0.7580 0.439 Uiso 1 1 calc R . . C14 C 0.7399(7) 0.8521(7) 0.9047(10) 0.049(3) Uani 1 1 d . . . H14A H 0.7123 0.8067 0.8928 0.073 Uiso 1 1 calc R . . H14B H 0.7071 0.8899 0.9350 0.073 Uiso 1 1 calc R . . H14C H 0.7799 0.8431 0.9581 0.073 Uiso 1 1 calc R . . C15 C 0.7192(11) 0.916(2) 0.727(2) 0.26(2) Uani 1 1 d . . . H15A H 0.7387 0.9237 0.6509 0.386 Uiso 1 1 calc R . . H15B H 0.7086 0.9639 0.7615 0.386 Uiso 1 1 calc R . . H15C H 0.6740 0.8872 0.7227 0.386 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ho1 0.0334(2) 0.0244(2) 0.0402(2) 0.0079(4) 0.0096(5) -0.00284(16) O1 0.054(4) 0.024(3) 0.062(5) 0.013(8) -0.006(9) -0.012(3) O2 0.034(5) 0.017(4) 0.032(4) 0.007(3) -0.001(4) 0.004(3) O3 0.015(4) 0.035(5) 0.038(4) 0.002(3) 0.005(4) -0.008(4) C1 0.114(13) 0.046(8) 0.085(13) -0.023(7) 0.059(10) -0.036(8) C2 0.063(7) 0.031(6) 0.061(13) -0.005(7) -0.009(7) -0.009(5) C3 0.086(13) 0.048(9) 0.39(4) 0.02(3) 0.00(3) -0.001(8) C4 0.165(17) 0.056(9) 0.14(2) -0.017(13) 0.028(18) -0.048(10) C5 0.21(3) 0.082(14) 0.096(14) -0.016(12) 0.026(16) -0.066(16) C6 0.047(7) 0.040(7) 0.038(6) 0.010(5) -0.001(6) 0.006(5) C7 0.040(7) 0.035(7) 0.046(7) -0.003(5) 0.001(5) 0.008(5) C8 0.044(8) 0.060(10) 0.099(13) -0.045(9) 0.028(8) -0.019(7) C9 0.18(2) 0.111(15) 0.034(8) -0.008(9) 0.023(10) 0.016(15) C10 0.052(9) 0.053(9) 0.080(10) -0.026(8) 0.019(8) 0.003(7) C11 0.17(2) 0.42(5) 0.031(9) 0.031(16) -0.022(11) -0.21(3) C12 0.038(6) 0.039(7) 0.044(7) -0.007(5) -0.010(5) -0.004(5) C13 0.61(8) 0.082(18) 0.19(3) -0.047(19) 0.28(4) -0.12(3) C14 0.041(7) 0.054(8) 0.052(7) -0.013(6) 0.007(6) -0.009(6) C15 0.068(14) 0.46(6) 0.24(3) 0.30(4) 0.048(18) 0.06(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O1 Ho1 O2 121.4(4) . 3_577 ? O1 Ho1 O2 122.6(4) . . ? O2 Ho1 O2 116.1(3) 3_577 . ? O1 Ho1 O3 109.4(3) . . ? O2 Ho1 O3 71.8(2) 3_577 . ? O2 Ho1 O3 88.0(3) . . ? O1 Ho1 O3 108.7(3) . 4_757 ? O2 Ho1 O3 88.4(3) 3_577 4_757 ? O2 Ho1 O3 71.5(2) . 4_757 ? O3 Ho1 O3 141.9(3) . 4_757 ? O1 Ho1 Ho1 135.00(18) . 4_757 ? O2 Ho1 Ho1 92.70(18) 3_577 4_757 ? O2 Ho1 Ho1 37.38(19) . 4_757 ? O3 Ho1 Ho1 108.70(17) . 4_757 ? O3 Ho1 Ho1 38.3(2) 4_757 4_757 ? O1 Ho1 Ho1 135.00(18) . 3_577 ? O2 Ho1 Ho1 37.7(2) 3_577 3_577 ? O2 Ho1 Ho1 92.38(17) . 3_577 ? O3 Ho1 Ho1 38.4(2) . 3_577 ? O3 Ho1 Ho1 108.94(18) 4_757 3_577 ? Ho1 Ho1 Ho1 90.0 4_757 3_577 ? C1 O1 Ho1 160.7(11) . . ? C6 O2 Ho1 128.2(7) . 4_757 ? C6 O2 Ho1 125.7(7) . . ? Ho1 O2 Ho1 105.0(3) 4_757 . ? C11 O3 Ho1 132.0(17) . . ? C11 O3 Ho1 124.3(17) . 3_577 ? Ho1 O3 Ho1 103.3(3) . 3_577 ? O1 C1 C2 117.7(11) . . ? O1 C1 H1A 107.9 . . ? C2 C1 H1A 107.9 . . ? O1 C1 H1B 107.9 . . ? C2 C1 H1B 107.9 . . ? H1A C1 H1B 107.2 . . ? C3 C2 C5 100(2) . . ? C3 C2 C1 112.0(16) . . ? C5 C2 C1 111.3(14) . . ? C3 C2 C4 111.9(15) . . ? C5 C2 C4 110.2(15) . . ? C1 C2 C4 111.0(14) . . ? C2 C3 H3A 109.6 . . ? C2 C3 H3B 109.2 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.6 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O2 C6 C7 114.3(9) . . ? O2 C6 H6A 108.7 . . ? C7 C6 H6A 108.7 . . ? O2 C6 H6B 108.7 . . ? C7 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? C6 C7 C9 108.2(11) . . ? C6 C7 C10 111.9(10) . . ? C9 C7 C10 108.2(12) . . ? C6 C7 C8 110.5(10) . . ? C9 C7 C8 110.0(13) . . ? C10 C7 C8 108.1(11) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O3 C11 C12 131.8(14) . . ? O3 C11 H11A 104.3 . . ? C12 C11 H11A 104.3 . . ? O3 C11 H11B 104.3 . . ? C12 C11 H11B 104.3 . . ? H11A C11 H11B 105.6 . . ? C15 C12 C13 109(2) . . ? C15 C12 C11 109(2) . . ? C13 C12 C11 104(2) . . ? C15 C12 C14 112.2(13) . . ? C13 C12 C14 109.6(13) . . ? C11 C12 C14 112.3(11) . . ? C12 C13 H13A 109.4 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.4 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? 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 Ho1 O1 2.032(6) . ? Ho1 O2 2.231(8) 3_577 ? Ho1 O2 2.245(8) . ? Ho1 O3 2.260(8) . ? Ho1 O3 2.265(8) 4_757 ? Ho1 Ho1 3.5497(6) 4_757 ? Ho1 Ho1 3.5498(6) 3_577 ? O1 C1 1.402(13) . ? O2 C6 1.422(13) . ? O2 Ho1 2.231(8) 4_757 ? O3 C11 1.321(17) . ? O3 Ho1 2.265(8) 3_577 ? C1 C2 1.481(17) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C2 C3 1.47(2) . ? C2 C5 1.48(2) . ? C2 C4 1.50(2) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 C7 1.501(15) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 C9 1.524(18) . ? C7 C10 1.533(18) . ? C7 C8 1.539(17) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C12 1.41(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 C15 1.40(2) . ? C12 C13 1.41(3) . ? C12 C14 1.509(16) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 139129175