data_shelx _audit_creation_method 'SHELXL-2018/1' _shelx_SHELXL_version_number '2018/1' _chemical_name_systematic ? _chemical_name_common Hydroxykenopyrochlor _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ce6.80 H8 Nb11.75 O56 Ti4.25' _chemical_formula_weight 3152.15 _publ_contact_author_name 'Ritsuro Miyawaki' _publ_contact_author_address ; Department of Geology and Paleontology, National Museum of Nature and. Science 4-1-1, Amakubo, Tsukuba 305-0005, Japan ; _publ_contact_author_email 'miyawaki@kahaku.go.jp' _publ_contact_author_fax '+81-29-853-8167' _publ_contact_author_phone '+81-29-853-8167' _publ_requested_journal ? _publ_section_title ? loop_ _publ_author_name 'RITSURO MIYAWAKI' 'KOICHI MOMMA' 'SATOSHI MATSUBARA' 'TAKASHI SANO' 'MASAKO SHIGEOKA' 'HIROYUKI HORIUCHI' _publ_author_address ; Department of Geology and Paleontology, National Museum of Nature and. Science 4-1-1, Amakubo, Tsukuba 305-0005, Japan ; _publ_section_abstract ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ce' 'Ce' -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nb' 'Nb' -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system cubic _space_group_IT_number 227 _space_group_name_H-M_alt 'F d -3 m' _space_group_name_Hall '-F 4vw 2vw 3' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' 'y, z, x' 'z, x, y' 'x+1/4, y+1/4, -z' 'y+1/4, z+1/4, -x' 'z+1/4, x+1/4, -y' 'y+1/2, -z+1/4, -x+3/4' 'z+1/2, -x+1/4, -y+3/4' '-z+1/4, x+1/2, -y+3/4' '-x+1/4, y+1/2, -z+3/4' '-y+1/4, z+1/2, -x+3/4' 'x+1/2, -y+1/4, -z+3/4' 'y, x, z' 'z, y, x' 'x, z, y' 'y+1/4, x+1/4, -z' 'z+1/4, y+1/4, -x' 'x+1/4, z+1/4, -y' '-z+1/4, y+1/2, -x+3/4' '-x+1/4, z+1/2, -y+3/4' 'x+1/2, -z+1/4, -y+3/4' 'y+1/2, -x+1/4, -z+3/4' 'z+1/2, -y+1/4, -x+3/4' '-y+1/4, x+1/2, -z+3/4' 'x, y+1/2, z+1/2' 'y, z+1/2, x+1/2' 'z, x+1/2, y+1/2' 'x+1/4, y+3/4, -z+1/2' 'y+1/4, z+3/4, -x+1/2' 'z+1/4, x+3/4, -y+1/2' 'y+1/2, -z+3/4, -x+5/4' 'z+1/2, -x+3/4, -y+5/4' '-z+1/4, x+1, -y+5/4' '-x+1/4, y+1, -z+5/4' '-y+1/4, z+1, -x+5/4' 'x+1/2, -y+3/4, -z+5/4' 'y, x+1/2, z+1/2' 'z, y+1/2, x+1/2' 'x, z+1/2, y+1/2' 'y+1/4, x+3/4, -z+1/2' 'z+1/4, y+3/4, -x+1/2' 'x+1/4, z+3/4, -y+1/2' '-z+1/4, y+1, -x+5/4' '-x+1/4, z+1, -y+5/4' 'x+1/2, -z+3/4, -y+5/4' 'y+1/2, -x+3/4, -z+5/4' 'z+1/2, -y+3/4, -x+5/4' '-y+1/4, x+1, -z+5/4' 'x+1/2, y, z+1/2' 'y+1/2, z, x+1/2' 'z+1/2, x, y+1/2' 'x+3/4, y+1/4, -z+1/2' 'y+3/4, z+1/4, -x+1/2' 'z+3/4, x+1/4, -y+1/2' 'y+1, -z+1/4, -x+5/4' 'z+1, -x+1/4, -y+5/4' '-z+3/4, x+1/2, -y+5/4' '-x+3/4, y+1/2, -z+5/4' '-y+3/4, z+1/2, -x+5/4' 'x+1, -y+1/4, -z+5/4' 'y+1/2, x, z+1/2' 'z+1/2, y, x+1/2' 'x+1/2, z, y+1/2' 'y+3/4, x+1/4, -z+1/2' 'z+3/4, y+1/4, -x+1/2' 'x+3/4, z+1/4, -y+1/2' '-z+3/4, y+1/2, -x+5/4' '-x+3/4, z+1/2, -y+5/4' 'x+1, -z+1/4, -y+5/4' 'y+1, -x+1/4, -z+5/4' 'z+1, -y+1/4, -x+5/4' '-y+3/4, x+1/2, -z+5/4' 'x+1/2, y+1/2, z' 'y+1/2, z+1/2, x' 'z+1/2, x+1/2, y' 'x+3/4, y+3/4, -z' 'y+3/4, z+3/4, -x' 'z+3/4, x+3/4, -y' 'y+1, -z+3/4, -x+3/4' 'z+1, -x+3/4, -y+3/4' '-z+3/4, x+1, -y+3/4' '-x+3/4, y+1, -z+3/4' '-y+3/4, z+1, -x+3/4' 'x+1, -y+3/4, -z+3/4' 'y+1/2, x+1/2, z' 'z+1/2, y+1/2, x' 'x+1/2, z+1/2, y' 'y+3/4, x+3/4, -z' 'z+3/4, y+3/4, -x' 'x+3/4, z+3/4, -y' '-z+3/4, y+1, -x+3/4' '-x+3/4, z+1, -y+3/4' 'x+1, -z+3/4, -y+3/4' 'y+1, -x+3/4, -z+3/4' 'z+1, -y+3/4, -x+3/4' '-y+3/4, x+1, -z+3/4' '-x, -y, -z' '-y, -z, -x' '-z, -x, -y' '-x-1/4, -y-1/4, z' '-y-1/4, -z-1/4, x' '-z-1/4, -x-1/4, y' '-y-1/2, z-1/4, x-3/4' '-z-1/2, x-1/4, y-3/4' 'z-1/4, -x-1/2, y-3/4' 'x-1/4, -y-1/2, z-3/4' 'y-1/4, -z-1/2, x-3/4' '-x-1/2, y-1/4, z-3/4' '-y, -x, -z' '-z, -y, -x' '-x, -z, -y' '-y-1/4, -x-1/4, z' '-z-1/4, -y-1/4, x' '-x-1/4, -z-1/4, y' 'z-1/4, -y-1/2, x-3/4' 'x-1/4, -z-1/2, y-3/4' '-x-1/2, z-1/4, y-3/4' '-y-1/2, x-1/4, z-3/4' '-z-1/2, y-1/4, x-3/4' 'y-1/4, -x-1/2, z-3/4' '-x, -y+1/2, -z+1/2' '-y, -z+1/2, -x+1/2' '-z, -x+1/2, -y+1/2' '-x-1/4, -y+1/4, z+1/2' '-y-1/4, -z+1/4, x+1/2' '-z-1/4, -x+1/4, y+1/2' '-y-1/2, z+1/4, x-1/4' '-z-1/2, x+1/4, y-1/4' 'z-1/4, -x, y-1/4' 'x-1/4, -y, z-1/4' 'y-1/4, -z, x-1/4' '-x-1/2, y+1/4, z-1/4' '-y, -x+1/2, -z+1/2' '-z, -y+1/2, -x+1/2' '-x, -z+1/2, -y+1/2' '-y-1/4, -x+1/4, z+1/2' '-z-1/4, -y+1/4, x+1/2' '-x-1/4, -z+1/4, y+1/2' 'z-1/4, -y, x-1/4' 'x-1/4, -z, y-1/4' '-x-1/2, z+1/4, y-1/4' '-y-1/2, x+1/4, z-1/4' '-z-1/2, y+1/4, x-1/4' 'y-1/4, -x, z-1/4' '-x+1/2, -y, -z+1/2' '-y+1/2, -z, -x+1/2' '-z+1/2, -x, -y+1/2' '-x+1/4, -y-1/4, z+1/2' '-y+1/4, -z-1/4, x+1/2' '-z+1/4, -x-1/4, y+1/2' '-y, z-1/4, x-1/4' '-z, x-1/4, y-1/4' 'z+1/4, -x-1/2, y-1/4' 'x+1/4, -y-1/2, z-1/4' 'y+1/4, -z-1/2, x-1/4' '-x, y-1/4, z-1/4' '-y+1/2, -x, -z+1/2' '-z+1/2, -y, -x+1/2' '-x+1/2, -z, -y+1/2' '-y+1/4, -x-1/4, z+1/2' '-z+1/4, -y-1/4, x+1/2' '-x+1/4, -z-1/4, y+1/2' 'z+1/4, -y-1/2, x-1/4' 'x+1/4, -z-1/2, y-1/4' '-x, z-1/4, y-1/4' '-y, x-1/4, z-1/4' '-z, y-1/4, x-1/4' 'y+1/4, -x-1/2, z-1/4' '-x+1/2, -y+1/2, -z' '-y+1/2, -z+1/2, -x' '-z+1/2, -x+1/2, -y' '-x+1/4, -y+1/4, z' '-y+1/4, -z+1/4, x' '-z+1/4, -x+1/4, y' '-y, z+1/4, x-3/4' '-z, x+1/4, y-3/4' 'z+1/4, -x, y-3/4' 'x+1/4, -y, z-3/4' 'y+1/4, -z, x-3/4' '-x, y+1/4, z-3/4' '-y+1/2, -x+1/2, -z' '-z+1/2, -y+1/2, -x' '-x+1/2, -z+1/2, -y' '-y+1/4, -x+1/4, z' '-z+1/4, -y+1/4, x' '-x+1/4, -z+1/4, y' 'z+1/4, -y, x-3/4' 'x+1/4, -z, y-3/4' '-x, z+1/4, y-3/4' '-y, x+1/4, z-3/4' '-z, y+1/4, x-3/4' 'y+1/4, -x, z-3/4' _cell_length_a 10.4659(9) _cell_length_b 10.4659(9) _cell_length_c 10.4659(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1146.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3104 _cell_measurement_theta_min 3.372 _cell_measurement_theta_max 29.937 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 4.566 _exptl_crystal_F_000 1426 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.050 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 10.231 _shelx_estimated_absorpt_T_min 0.629 _shelx_estimated_absorpt_T_max 0.822 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4365 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source 'rotating-anode X-ray tube' _diffrn_measurement_device_type 'Rigaku VariMax with RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3104 _diffrn_reflns_av_unetI/netI 0.0083 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.372 _diffrn_reflns_theta_max 29.937 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 105 _reflns_number_gt 93 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_cell_refinement 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_data_reduction 'CrystalStructure (Rigaku/MSC, 2002)' _computing_structure_solution 'SUPERFLIP (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+16.1493P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 105 _refine_ls_number_parameters 12 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0289 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0744 _refine_ls_wR_factor_gt 0.0729 _refine_ls_goodness_of_fit_ref 1.211 _refine_ls_restrained_S_all 1.211 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.000000 0.000000 0.000000 0.0167(4) Uani 0.74(3) 12 d S T P . . Ti1 Ti 0.000000 0.000000 0.000000 0.0167(4) Uani 0.26(3) 12 d S T P . . Ce1 Ce 0.500000 0.000000 0.000000 0.0194(5) Uani 0.425(7) 12 d S T . . . O1 O 0.0666(4) -0.125000 -0.125000 0.0256(12) Uani 1 4 d S T P . . O2 O 0.125000 0.125000 -0.375000 0.092(6) Uani 1 24 d S T P . . 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 Nb1 0.0167(4) 0.0167(4) 0.0167(4) -0.00181(18) -0.00181(18) -0.00181(18) Ti1 0.0167(4) 0.0167(4) 0.0167(4) -0.00181(18) -0.00181(18) -0.00181(18) Ce1 0.0194(5) 0.0194(5) 0.0194(5) 0.0023(3) 0.0023(3) 0.0023(3) O1 0.036(3) 0.0204(14) 0.0204(14) -0.0062(17) 0.000 0.000 O2 0.092(6) 0.092(6) 0.092(6) 0.000 0.000 0.000 _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 Nb1 O1 1.9769(17) 99 ? Nb1 O1 1.9769(17) 3 ? Nb1 O1 1.9769(17) 98 ? Nb1 O1 1.9769(17) 2 ? Nb1 O1 1.9769(17) 97 ? Nb1 O1 1.9769(17) . ? Nb1 Ce1 3.7003(3) 9_544 ? Nb1 Ce1 3.7003(3) 57_444 ? Nb1 Ce1 3.7003(3) 79_445 ? Nb1 Ce1 3.7003(3) 55_454 ? Nb1 Ce1 3.7003(3) 76_445 ? Nb1 Ce1 3.7003(3) 4_455 ? Ce1 O2 2.2659(2) 145_554 ? Ce1 O2 2.2659(2) 49 ? Ce1 O1 2.666(3) 127_655 ? Ce1 O1 2.666(3) 31_544 ? Ce1 O1 2.666(3) 174 ? Ce1 O1 2.666(3) 78_545 ? Ce1 O1 2.666(3) 100_655 ? Ce1 O1 2.666(3) 4 ? Ce1 Ce1 3.7003(3) 4 ? Ce1 Ce1 3.7003(3) 7 ? Ce1 Ce1 3.7003(3) 31_544 ? Ce1 Ce1 3.7003(3) 9_544 ? 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 Nb1 O1 180.0(3) 99 3 ? O1 Nb1 O1 91.63(18) 99 98 ? O1 Nb1 O1 88.37(18) 3 98 ? O1 Nb1 O1 88.37(18) 99 2 ? O1 Nb1 O1 91.63(18) 3 2 ? O1 Nb1 O1 180.0(3) 98 2 ? O1 Nb1 O1 91.63(18) 99 97 ? O1 Nb1 O1 88.37(18) 3 97 ? O1 Nb1 O1 91.63(18) 98 97 ? O1 Nb1 O1 88.37(18) 2 97 ? O1 Nb1 O1 88.37(18) 99 . ? O1 Nb1 O1 91.63(18) 3 . ? O1 Nb1 O1 88.37(18) 98 . ? O1 Nb1 O1 91.63(18) 2 . ? O1 Nb1 O1 180.0 97 . ? O1 Nb1 Ce1 90.0 99 9_544 ? O1 Nb1 Ce1 90.0 3 9_544 ? O1 Nb1 Ce1 44.19(9) 98 9_544 ? O1 Nb1 Ce1 135.81(9) 2 9_544 ? O1 Nb1 Ce1 135.81(9) 97 9_544 ? O1 Nb1 Ce1 44.18(9) . 9_544 ? O1 Nb1 Ce1 90.0 99 57_444 ? O1 Nb1 Ce1 90.0 3 57_444 ? O1 Nb1 Ce1 135.81(9) 98 57_444 ? O1 Nb1 Ce1 44.19(9) 2 57_444 ? O1 Nb1 Ce1 44.19(9) 97 57_444 ? O1 Nb1 Ce1 135.82(9) . 57_444 ? Ce1 Nb1 Ce1 180.0 9_544 57_444 ? O1 Nb1 Ce1 44.19(9) 99 79_445 ? O1 Nb1 Ce1 135.81(9) 3 79_445 ? O1 Nb1 Ce1 135.81(9) 98 79_445 ? O1 Nb1 Ce1 44.19(9) 2 79_445 ? O1 Nb1 Ce1 90.0 97 79_445 ? O1 Nb1 Ce1 90.0 . 79_445 ? Ce1 Nb1 Ce1 120.0 9_544 79_445 ? Ce1 Nb1 Ce1 60.0 57_444 79_445 ? O1 Nb1 Ce1 135.81(9) 99 55_454 ? O1 Nb1 Ce1 44.19(9) 3 55_454 ? O1 Nb1 Ce1 44.19(9) 98 55_454 ? O1 Nb1 Ce1 135.81(9) 2 55_454 ? O1 Nb1 Ce1 90.0 97 55_454 ? O1 Nb1 Ce1 90.0 . 55_454 ? Ce1 Nb1 Ce1 60.0 9_544 55_454 ? Ce1 Nb1 Ce1 120.0 57_444 55_454 ? Ce1 Nb1 Ce1 180.0 79_445 55_454 ? O1 Nb1 Ce1 44.19(9) 99 76_445 ? O1 Nb1 Ce1 135.81(9) 3 76_445 ? O1 Nb1 Ce1 90.0 98 76_445 ? O1 Nb1 Ce1 90.0 2 76_445 ? O1 Nb1 Ce1 135.81(9) 97 76_445 ? O1 Nb1 Ce1 44.18(9) . 76_445 ? Ce1 Nb1 Ce1 60.0 9_544 76_445 ? Ce1 Nb1 Ce1 120.0 57_444 76_445 ? Ce1 Nb1 Ce1 60.0 79_445 76_445 ? Ce1 Nb1 Ce1 120.0 55_454 76_445 ? O1 Nb1 Ce1 135.81(9) 99 4_455 ? O1 Nb1 Ce1 44.19(9) 3 4_455 ? O1 Nb1 Ce1 90.0 98 4_455 ? O1 Nb1 Ce1 90.0 2 4_455 ? O1 Nb1 Ce1 44.19(9) 97 4_455 ? O1 Nb1 Ce1 135.82(9) . 4_455 ? Ce1 Nb1 Ce1 120.0 9_544 4_455 ? Ce1 Nb1 Ce1 60.0 57_444 4_455 ? Ce1 Nb1 Ce1 120.0 79_445 4_455 ? Ce1 Nb1 Ce1 60.0 55_454 4_455 ? Ce1 Nb1 Ce1 180.0 76_445 4_455 ? O2 Ce1 O2 180.0 145_554 49 ? O2 Ce1 O1 98.68(7) 145_554 127_655 ? O2 Ce1 O1 81.32(7) 49 127_655 ? O2 Ce1 O1 81.32(7) 145_554 31_544 ? O2 Ce1 O1 98.68(7) 49 31_544 ? O1 Ce1 O1 180.0 127_655 31_544 ? O2 Ce1 O1 81.32(7) 145_554 174 ? O2 Ce1 O1 98.68(7) 49 174 ? O1 Ce1 O1 62.23(4) 127_655 174 ? O1 Ce1 O1 117.77(4) 31_544 174 ? O2 Ce1 O1 98.68(7) 145_554 78_545 ? O2 Ce1 O1 81.32(7) 49 78_545 ? O1 Ce1 O1 117.77(4) 127_655 78_545 ? O1 Ce1 O1 62.23(4) 31_544 78_545 ? O1 Ce1 O1 180.00(14) 174 78_545 ? O2 Ce1 O1 81.32(7) 145_554 100_655 ? O2 Ce1 O1 98.68(7) 49 100_655 ? O1 Ce1 O1 62.23(4) 127_655 100_655 ? O1 Ce1 O1 117.77(4) 31_544 100_655 ? O1 Ce1 O1 117.77(4) 174 100_655 ? O1 Ce1 O1 62.23(4) 78_545 100_655 ? O2 Ce1 O1 98.68(7) 145_554 4 ? O2 Ce1 O1 81.32(7) 49 4 ? O1 Ce1 O1 117.77(4) 127_655 4 ? O1 Ce1 O1 62.23(4) 31_544 4 ? O1 Ce1 O1 62.23(4) 174 4 ? O1 Ce1 O1 117.77(4) 78_545 4 ? O1 Ce1 O1 180.00(14) 100_655 4 ? O2 Ce1 Ce1 144.7 145_554 4 ? O2 Ce1 Ce1 35.3 49 4 ? O1 Ce1 Ce1 46.06(7) 127_655 4 ? O1 Ce1 Ce1 133.94(7) 31_544 4 ? O1 Ce1 Ce1 80.66(6) 174 4 ? O1 Ce1 Ce1 99.34(6) 78_545 4 ? O1 Ce1 Ce1 80.66(6) 100_655 4 ? O1 Ce1 Ce1 99.34(6) 4 4 ? O2 Ce1 Ce1 144.7 145_554 7 ? O2 Ce1 Ce1 35.3 49 7 ? O1 Ce1 Ce1 99.34(6) 127_655 7 ? O1 Ce1 Ce1 80.66(6) 31_544 7 ? O1 Ce1 Ce1 80.66(6) 174 7 ? O1 Ce1 Ce1 99.34(6) 78_545 7 ? O1 Ce1 Ce1 133.94(7) 100_655 7 ? O1 Ce1 Ce1 46.06(7) 4 7 ? Ce1 Ce1 Ce1 60.0 4 7 ? O2 Ce1 Ce1 35.3 145_554 31_544 ? O2 Ce1 Ce1 144.7 49 31_544 ? O1 Ce1 Ce1 80.66(6) 127_655 31_544 ? O1 Ce1 Ce1 99.34(6) 31_544 31_544 ? O1 Ce1 Ce1 99.34(6) 174 31_544 ? O1 Ce1 Ce1 80.66(6) 78_545 31_544 ? O1 Ce1 Ce1 46.06(7) 100_655 31_544 ? O1 Ce1 Ce1 133.94(7) 4 31_544 ? Ce1 Ce1 Ce1 120.0 4 31_544 ? Ce1 Ce1 Ce1 180.0 7 31_544 ? O2 Ce1 Ce1 35.3 145_554 9_544 ? O2 Ce1 Ce1 144.7 49 9_544 ? O1 Ce1 Ce1 80.66(6) 127_655 9_544 ? O1 Ce1 Ce1 99.34(6) 31_544 9_544 ? O1 Ce1 Ce1 46.06(7) 174 9_544 ? O1 Ce1 Ce1 133.94(7) 78_545 9_544 ? O1 Ce1 Ce1 99.34(6) 100_655 9_544 ? O1 Ce1 Ce1 80.66(6) 4 9_544 ? Ce1 Ce1 Ce1 120.0 4 9_544 ? Ce1 Ce1 Ce1 120.0 7 9_544 ? Ce1 Ce1 Ce1 60.0 31_544 9_544 ? Nb1 O1 Nb1 138.7(3) 79_444 . ? Nb1 O1 Ce1 104.70(7) 79_444 76_445 ? Nb1 O1 Ce1 104.70(7) . 76_445 ? Nb1 O1 Ce1 104.70(7) 79_444 9_544 ? Nb1 O1 Ce1 104.70(7) . 9_544 ? Ce1 O1 Ce1 87.88(14) 76_445 9_544 ? Ce1 O2 Ce1 109.5 49_454 9_544 ? Ce1 O2 Ce1 109.5 49_454 52_454 ? Ce1 O2 Ce1 109.5 9_544 52_454 ? Ce1 O2 Ce1 109.5 49_454 55_454 ? Ce1 O2 Ce1 109.5 9_544 55_454 ? Ce1 O2 Ce1 109.5 52_454 55_454 ? _refine_diff_density_max 0.626 _refine_diff_density_min -0.530 _refine_diff_density_rms 0.124 _shelx_res_file ; TITL Horiuchi18Za shelx.res created by SHELXL-2018/1 at 11:24:45 on 11-Aug-2020 CELL 0.71075 10.46590 10.46590 10.46590 90.000 90.000 90.000 ZERR 1 0.00093 0.00093 0.00093 0.000 0.000 0.000 LATT 4 SYMM +Y, +Z, +X SYMM +Z, +X, +Y SYMM .25+X, .25+Y, -Z SYMM .25+Y, .25+Z, -X SYMM .25+Z, .25+X, -Y SYMM .50+Y, .25-Z, .75-X SYMM .50+Z, .25-X, .75-Y SYMM .25-Z, .50+X, .75-Y SYMM .25-X, .50+Y, .75-Z SYMM .25-Y, .50+Z, .75-X SYMM .50+X, .25-Y, .75-Z SYMM +Y, +X, +Z SYMM +Z, +Y, +X SYMM +X, +Z, +Y SYMM .25+Y, .25+X, -Z SYMM .25+Z, .25+Y, -X SYMM .25+X, .25+Z, -Y SYMM .25-Z, .50+Y, .75-X SYMM .25-X, .50+Z, .75-Y SYMM .50+X, .25-Z, .75-Y SYMM .50+Y, .25-X, .75-Z SYMM .50+Z, .25-Y, .75-X SYMM .25-Y, .50+X, .75-Z SFAC CE NB TI O H UNIT 6.800000 11.750000 4.250000 56 8 SHEL 99999.000000 0.000000 L.S. 50 FMAP 2 PLAN -10 WPDB -2 HTAB BOND $H CONF LIST 3 TEMP 23.0 ACTA EXYZ Nb1 Ti1 EADP Nb1 Ti1 SIZE 0.050 0.040 0.020 WGHT 0.030600 16.149302 FVAR 0.14039 0.73531 NB1 2 0.000000 0.000000 0.000000 20.08333 0.01665 0.01665 = 0.01665 -0.00181 -0.00181 -0.00181 TI1 3 0.000000 0.000000 0.000000 -20.08333 0.01665 0.01665 = 0.01665 -0.00181 -0.00181 -0.00181 CE1 1 0.500000 0.000000 0.000000 0.03541 0.01937 0.01937 = 0.01937 0.00226 0.00226 0.00226 O1 4 0.066560 -0.125000 -0.125000 10.25000 0.03615 0.02036 = 0.02036 -0.00620 0.00000 0.00000 O2 4 0.125000 0.125000 -0.375000 10.04167 0.09216 0.09216 = 0.09216 0.00000 0.00000 0.00000 HKLF 4 REM Horiuchi18Za REM R1 = 0.0268 for 93 Fo > 4sig(Fo) and 0.0289 for all 105 data REM 12 parameters refined using 0 restraints END WGHT 0.0306 16.1624 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.626, deepest hole -0.530, 1-sigma level 0.124 Q1 1 0.0577 -0.3077 0.0577 10.16667 0.05 0.37 Q2 1 -0.0783 -0.1124 0.1296 11.00000 0.05 0.35 Q3 1 0.2023 -0.2977 0.0477 10.16667 0.05 0.34 Q4 1 0.1250 -0.1631 0.1250 10.25000 0.05 0.32 Q5 1 0.3148 -0.1252 -0.0403 11.00000 0.05 0.25 Q6 1 -0.2159 0.1250 0.1250 10.25000 0.05 0.22 Q7 1 -0.1987 -0.0268 0.1225 11.00000 0.05 0.22 Q8 1 -0.1250 0.2565 -0.1250 10.25000 0.05 0.19 Q9 1 0.0030 0.2848 0.1215 11.00000 0.05 0.18 Q10 1 0.0315 -0.0152 0.1282 11.00000 0.05 0.18 ; _shelx_res_checksum 96962 _shelx_hkl_file ; 1 -1 -1 248.38 7.14 -1 -1 1 255.81 6.18 1 1 1 260.36 6.94 1 1 -1 255.37 6.68 -1 -1 -1 251.95 6.90 -1 1 1 247.73 7.14 2 0 0 0.81 1.91 0 0 2 1.84 1.08 0 0 2 0.39 1.38 -2 0 0 1.07 1.72 0 0 -2 0.52 1.23 0 -2 0 2.20 1.55 0 2 0 0.19 1.52 0 -2 2 -0.34 1.30 -2 2 0 0.17 1.66 0 2 -2 1.36 2.09 0 2 2 0.40 1.57 2 -2 0 0.30 2.04 2 0 2 1.88 2.08 0 -2 -2 0.72 1.31 2 0 -2 0.61 1.21 -2 -2 0 -0.48 1.89 2 2 0 0.63 1.99 0 2 2 1.44 1.79 -2 0 2 0.25 0.87 0 -2 -2 0.53 2.01 -2 0 -2 0.16 1.40 2 -2 -210866.21 338.14 2 2 211012.84 340.70 -2 -2 210988.45 336.62 -2 2 -210869.91 322.43 -2 -2 -210730.77 332.12 -2 2 210924.25 339.49 2 -2 2 9894.28 302.56 2 2 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