#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:53:41 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176768 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/49/2104964.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2104964 loop_ _publ_author_name 'Andrusenko, Iryna' 'Mugnaioli, Enrico' 'Gorelik, Tatiana E.' 'Koll, Dominik' 'Panth\"ofer, Martin' 'Tremel, Wolfgang' 'Kolb, Ute' _publ_section_title ; Structure analysis of titanate nanorods by automated electron diffraction tomography ; _journal_coeditor_code KD5050 _journal_issue 3 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 218 _journal_page_last 225 _journal_paper_doi 10.1107/S0108768111014534 _journal_volume 67 _journal_year 2011 _chemical_formula_sum 'Na O3 Ti1.25' _chemical_formula_weight 130.86 _space_group_IT_number 12 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 1 2/m 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_type_scat_source 'P.A. Doyle, P.S. Turner, Acta Crystallogr. A 1968, 24, 390-397' _cell_angle_alpha 90.0000 _cell_angle_beta 136.14(2) _cell_angle_gamma 90.0000 _cell_formula_units_Z 8 _cell_length_a 21.555(7) _cell_length_b 3.7583(9) _cell_length_c 11.926(5) _cell_volume 669.4(5) _computing_structure_refinement SHELXL-97 _computing_structure_solution Sir2008 _diffrn_ambient_temperature 295 _diffrn_measured_fraction_theta_full 0.784 _diffrn_measured_fraction_theta_max 0.784 _diffrn_measurement_device_type ; FEI TECNAI F-30 S-TWIN TEM with automated diffraction topography (ADT) and precession electron diffraction (PED) attachments ; _diffrn_radiation_monochromator not _diffrn_radiation_type electron _diffrn_radiation_wavelength 0.0197 _diffrn_reflns_av_R_equivalents 0.1583 _diffrn_reflns_av_sigmaI/netI 0.1154 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 1749 _diffrn_reflns_theta_full 0.70 _diffrn_reflns_theta_max 0.70 _diffrn_reflns_theta_min 0.05 _exptl_absorpt_coefficient_mu 0.012 _exptl_absorpt_correction_type none _exptl_crystal_density_diffrn 2.587 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'elongated wire' _exptl_crystal_F_000 173 _exptl_crystal_size_max 1.0 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.730 _refine_diff_density_min -0.514 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 3.725 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 40 _refine_ls_number_reflns 628 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 3.725 _refine_ls_R_factor_all 0.2679 _refine_ls_R_factor_gt 0.2665 _refine_ls_shift/su_max 0.863 _refine_ls_shift/su_mean 0.305 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.5834 _refine_ls_wR_factor_ref 0.5921 _reflns_number_total 628 _cod_data_source_file kd5050.cif _cod_data_source_block I _cod_original_cell_volume 669.5(4) _cod_original_sg_symbol_H-M C2/M _cod_database_code 2104964 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,-z -x,-y,-z x,-y,z x+1/2,y+1/2,z -x+1/2,y+1/2,-z -x+1/2,-y+1/2,-z x+1/2,-y+1/2,z loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti1 0.7514(4) 0.0000 0.3943(9) 0.029(2) Uiso d S 1 2 . . Ti Ti2 0.5712(5) -0.5000 0.5130(11) 0.036(2) Uiso d S 1 2 . . Ti Ti3 0.5764(4) 0.0000 0.3019(9) 0.028(2) Uiso d S 1 2 . . O O1 0.7286(9) 0.0000 0.537(2) 0.024(3) Uiso d S 1 2 . . O O2 0.6272(13) 0.0000 0.222(3) 0.049(5) Uiso d S 1 2 . . O OW1 0.3705(12) 0.0000 0.158(3) 0.048(5) Uiso d S 1 2 . . O O3 0.7073(10) -0.5000 0.692(2) 0.035(4) Uiso d S 1 2 . . O O4 0.6009(10) -0.5000 0.370(2) 0.035(4) Uiso d S 1 2 . . O O5 0.5691(11) -0.5000 0.668(2) 0.044(5) Uiso d S 1 2 . . O O6 0.5637(10) 0.0000 0.452(2) 0.033(4) Uiso d S 1 2 . . Na Na2 0.7682(11) 0.0000 0.916(3) 0.052(4) Uiso d S 1 2 . . O OW2 0.9124(14) 0.0000 0.950(3) 0.067(7) Uiso d S 1 2 . . O OH 0.4636(9) 0.0000 0.119(2) 0.031(4) Uiso d S 1 2 . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O3 Ti1 O2 7_646 . 106.4(10) ? O3 Ti1 O1 7_646 7_656 100.8(5) ? O2 Ti1 O1 . 7_656 99.6(4) ? O3 Ti1 O1 7_646 7_646 100.8(5) ? O2 Ti1 O1 . 7_646 99.6(4) ? O1 Ti1 O1 7_656 7_646 145.7(10) ? O3 Ti1 O1 7_646 . 169.1(7) ? O2 Ti1 O1 . . 84.5(8) ? O1 Ti1 O1 7_656 . 76.9(5) ? O1 Ti1 O1 7_646 . 76.9(5) ? O5 Ti2 O5 . 5_646 88.2(8) ? O5 Ti2 O6 . 1_545 107.7(6) ? O5 Ti2 O6 5_646 1_545 87.0(5) ? O5 Ti2 O6 . . 107.7(6) ? O5 Ti2 O6 5_646 . 87.0(5) ? O6 Ti2 O6 1_545 . 143.9(12) ? O5 Ti2 O3 . . 90.7(8) ? O5 Ti2 O3 5_646 . 179.0(9) ? O6 Ti2 O3 1_545 . 93.3(5) ? O6 Ti2 O3 . . 93.3(5) ? OH Ti3 O4 . 1_565 103.4(5) ? OH Ti3 O4 . . 103.4(5) ? O4 Ti3 O4 1_565 . 146.8(11) ? OH Ti3 O6 . . 98.7(8) ? O4 Ti3 O6 1_565 . 78.4(6) ? O4 Ti3 O6 . . 78.4(6) ? OH Ti3 O2 . . 99.3(9) ? O4 Ti3 O2 1_565 . 97.3(6) ? O4 Ti3 O2 . . 97.3(6) ? O6 Ti3 O2 . . 162.0(9) ? Ti1 O1 Ti1 7_656 7_646 145.7(10) ? Ti1 O1 Ti1 7_656 . 103.1(5) ? Ti1 O1 Ti1 7_646 . 103.1(5) ? Ti1 O2 Ti3 . . 109.6(12) ? Ti1 O3 Ti2 7_646 . 110.0(10) ? Ti3 O4 Ti3 . 1_545 146.8(11) ? Ti2 O5 Ti2 . 5_646 91.8(8) ? Ti2 O6 Ti2 1_565 . 143.9(12) ? Ti2 O6 Ti3 1_565 . 107.3(6) ? Ti2 O6 Ti3 . . 107.3(6) ? OW1 Na2 Na2 5_656 7_657 56.0(6) ? OW1 Na2 Na2 5_656 7_647 56.0(6) ? Na2 Na2 Na2 7_657 7_647 71.8(9) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 O3 7_646 1.775(19) ? Ti1 O2 . 1.85(2) ? Ti1 O1 7_656 1.983(5) ? Ti1 O1 7_646 1.983(5) ? Ti1 O1 . 2.086(18) ? Ti2 O5 . 1.88(2) ? Ti2 O5 5_646 2.088(18) ? Ti2 O6 1_545 1.993(7) ? Ti2 O6 . 1.993(7) ? Ti2 O3 . 2.025(16) ? Ti3 OH . 1.731(16) ? Ti3 O4 1_565 1.978(6) ? Ti3 O4 . 1.978(5) ? Ti3 O6 . 2.00(2) ? Ti3 O2 . 1.90(2) ? O1 Ti1 7_656 1.983(5) ? O1 Ti1 7_646 1.983(5) ? OW1 Na2 5_656 2.42(3) ? O3 Ti1 7_646 1.775(19) ? O4 Ti3 1_545 1.978(5) ? O5 Ti2 5_646 2.088(18) ? O6 Ti2 1_565 1.993(7) ? Na2 OW1 5_656 2.42(3) ? Na2 Na2 7_657 3.23(3) ? Na2 Na2 7_647 3.23(3) ?