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 H8 Nb11 O56 Ti5' _chemical_formula_weight 3006.29 _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 10.590(5) _cell_length_b 10.590(5) _cell_length_c 10.590(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1187.6(18) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3161 _cell_measurement_theta_min 3.332 _cell_measurement_theta_max 29.551 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 4.204 _exptl_crystal_F_000 1365 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.050 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 9.073 _shelx_estimated_absorpt_T_min 0.660 _shelx_estimated_absorpt_T_max 0.839 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7630 _exptl_absorpt_correction_T_max 0.8988 _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 3161 _diffrn_reflns_av_unetI/netI 0.0080 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.332 _diffrn_reflns_theta_max 29.551 _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 104 _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^)+(0.0028P)^2^+29.6877P] 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 14 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0513 _refine_ls_wR_factor_gt 0.0512 _refine_ls_goodness_of_fit_ref 1.487 _refine_ls_restrained_S_all 1.487 _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 0.0154(4) Uani 0.67(3) 12 d S T P . . Ti1 Ti 0.000000 0.000000 0.000000 0.0154(4) Uani 0.33(3) 12 d S T P . . Ce1 Ce 0.500000 0.000000 0.000000 0.0193(6) Uani 0.376(6) 12 d S T . . . O1 O 0.375000 0.375000 0.0666(5) 0.0259(15) Uani 1 4 d S T P . . O2 O -0.353(3) 0.103(3) 0.103(3) 0.06(2) Uani 0.25 6 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 0.0154(4) 0.0154(4) 0.0154(4) -0.0023(3) -0.0023(3) -0.0023(3) Ti1 0.0154(4) 0.0154(4) 0.0154(4) -0.0023(3) -0.0023(3) -0.0023(3) Ce1 0.0193(6) 0.0193(6) 0.0193(6) 0.0039(5) 0.0039(5) 0.0039(5) O1 0.0186(18) 0.0186(18) 0.041(3) 0.000 0.000 -0.007(2) O2 0.06(2) 0.06(2) 0.06(2) 0.022(18) -0.022(18) -0.022(18) _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 2.001(2) 123 ? Nb1 O1 2.001(2) 27_544 ? Nb1 O1 2.001(2) 146 ? Nb1 O1 2.001(2) 50_454 ? Nb1 O1 2.001(2) 169 ? Nb1 O1 2.001(2) 73_445 ? Nb1 Ce1 3.7441(19) 4_455 ? Nb1 Ce1 3.7441(19) 57_444 ? Nb1 Ce1 3.7441(19) 9_544 ? Nb1 Ce1 3.7441(19) 79_445 ? Nb1 Ce1 3.7441(19) 55_454 ? Nb1 Ce1 3.7441(19) 76_445 ? Ce1 O2 2.191(8) 146_554 ? Ce1 O2 2.191(8) 50 ? Ce1 O2 2.191(8) 171_545 ? Ce1 O2 2.191(8) 75 ? Ce1 O2 2.191(8) 97 ? Ce1 O2 2.191(8) 1_655 ? Ce1 O1 2.697(4) 154_565 ? Ce1 O1 2.697(4) 58_544 ? Ce1 O1 2.697(4) 126_654 ? Ce1 O1 2.697(4) 30_545 ? Ce1 O1 2.697(4) 125_654 ? Ce1 O1 2.697(4) 29_545 ? O2 O2 0.66(8) 125 ? O2 O2 0.66(8) 75_455 ? O2 O2 0.66(8) 50_455 ? 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) 123 27_544 ? O1 Nb1 O1 91.7(2) 123 146 ? O1 Nb1 O1 88.3(2) 27_544 146 ? O1 Nb1 O1 88.3(2) 123 50_454 ? O1 Nb1 O1 91.7(2) 27_544 50_454 ? O1 Nb1 O1 180.0(3) 146 50_454 ? O1 Nb1 O1 91.7(2) 123 169 ? O1 Nb1 O1 88.3(2) 27_544 169 ? O1 Nb1 O1 91.7(2) 146 169 ? O1 Nb1 O1 88.3(2) 50_454 169 ? O1 Nb1 O1 88.3(2) 123 73_445 ? O1 Nb1 O1 91.7(2) 27_544 73_445 ? O1 Nb1 O1 88.3(2) 146 73_445 ? O1 Nb1 O1 91.7(2) 50_454 73_445 ? O1 Nb1 O1 180.0(3) 169 73_445 ? O1 Nb1 Ce1 44.17(11) 123 4_455 ? O1 Nb1 Ce1 135.83(11) 27_544 4_455 ? O1 Nb1 Ce1 135.83(11) 146 4_455 ? O1 Nb1 Ce1 44.17(11) 50_454 4_455 ? O1 Nb1 Ce1 90.0 169 4_455 ? O1 Nb1 Ce1 90.0 73_445 4_455 ? O1 Nb1 Ce1 44.17(11) 123 57_444 ? O1 Nb1 Ce1 135.83(11) 27_544 57_444 ? O1 Nb1 Ce1 90.0 146 57_444 ? O1 Nb1 Ce1 90.0 50_454 57_444 ? O1 Nb1 Ce1 135.83(11) 169 57_444 ? O1 Nb1 Ce1 44.17(11) 73_445 57_444 ? Ce1 Nb1 Ce1 60.0 4_455 57_444 ? O1 Nb1 Ce1 135.83(11) 123 9_544 ? O1 Nb1 Ce1 44.17(11) 27_544 9_544 ? O1 Nb1 Ce1 90.0 146 9_544 ? O1 Nb1 Ce1 90.0 50_454 9_544 ? O1 Nb1 Ce1 44.17(11) 169 9_544 ? O1 Nb1 Ce1 135.83(11) 73_445 9_544 ? Ce1 Nb1 Ce1 120.0 4_455 9_544 ? Ce1 Nb1 Ce1 180.0 57_444 9_544 ? O1 Nb1 Ce1 90.0 123 79_445 ? O1 Nb1 Ce1 90.0 27_544 79_445 ? O1 Nb1 Ce1 44.17(11) 146 79_445 ? O1 Nb1 Ce1 135.83(11) 50_454 79_445 ? O1 Nb1 Ce1 135.83(11) 169 79_445 ? O1 Nb1 Ce1 44.17(11) 73_445 79_445 ? Ce1 Nb1 Ce1 120.0 4_455 79_445 ? Ce1 Nb1 Ce1 60.0 57_444 79_445 ? Ce1 Nb1 Ce1 120.0 9_544 79_445 ? O1 Nb1 Ce1 90.0 123 55_454 ? O1 Nb1 Ce1 90.0 27_544 55_454 ? O1 Nb1 Ce1 135.83(11) 146 55_454 ? O1 Nb1 Ce1 44.17(11) 50_454 55_454 ? O1 Nb1 Ce1 44.17(11) 169 55_454 ? O1 Nb1 Ce1 135.83(11) 73_445 55_454 ? Ce1 Nb1 Ce1 60.0 4_455 55_454 ? Ce1 Nb1 Ce1 120.0 57_444 55_454 ? Ce1 Nb1 Ce1 60.0 9_544 55_454 ? Ce1 Nb1 Ce1 180.0 79_445 55_454 ? O1 Nb1 Ce1 135.83(11) 123 76_445 ? O1 Nb1 Ce1 44.17(11) 27_544 76_445 ? O1 Nb1 Ce1 44.17(11) 146 76_445 ? O1 Nb1 Ce1 135.83(11) 50_454 76_445 ? O1 Nb1 Ce1 90.0 169 76_445 ? O1 Nb1 Ce1 90.0 73_445 76_445 ? Ce1 Nb1 Ce1 180.0 4_455 76_445 ? Ce1 Nb1 Ce1 120.0 57_444 76_445 ? Ce1 Nb1 Ce1 60.0 9_544 76_445 ? Ce1 Nb1 Ce1 60.0 79_445 76_445 ? Ce1 Nb1 Ce1 120.0 55_454 76_445 ? O2 Ce1 O2 180.0(15) 146_554 50 ? O2 Ce1 O2 17(2) 146_554 171_545 ? O2 Ce1 O2 163(2) 50 171_545 ? O2 Ce1 O2 163(2) 146_554 75 ? O2 Ce1 O2 17(2) 50 75 ? O2 Ce1 O2 180.0(15) 171_545 75 ? O2 Ce1 O2 17(2) 146_554 97 ? O2 Ce1 O2 163(2) 50 97 ? O2 Ce1 O2 17(2) 171_545 97 ? O2 Ce1 O2 163(2) 75 97 ? O2 Ce1 O2 163(2) 146_554 1_655 ? O2 Ce1 O2 17(2) 50 1_655 ? O2 Ce1 O2 163(2) 171_545 1_655 ? O2 Ce1 O2 17(2) 75 1_655 ? O2 Ce1 O2 180.0(15) 97 1_655 ? O2 Ce1 O1 88.6(13) 146_554 154_565 ? O2 Ce1 O1 91.4(13) 50 154_565 ? O2 Ce1 O1 103.6(6) 171_545 154_565 ? O2 Ce1 O1 76.4(6) 75 154_565 ? O2 Ce1 O1 103.6(6) 97 154_565 ? O2 Ce1 O1 76.4(6) 1_655 154_565 ? O2 Ce1 O1 91.4(13) 146_554 58_544 ? O2 Ce1 O1 88.6(13) 50 58_544 ? O2 Ce1 O1 76.4(6) 171_545 58_544 ? O2 Ce1 O1 103.6(6) 75 58_544 ? O2 Ce1 O1 76.4(6) 97 58_544 ? O2 Ce1 O1 103.6(6) 1_655 58_544 ? O1 Ce1 O1 180.00(17) 154_565 58_544 ? O2 Ce1 O1 76.4(6) 146_554 126_654 ? O2 Ce1 O1 103.6(6) 50 126_654 ? O2 Ce1 O1 76.4(6) 171_545 126_654 ? O2 Ce1 O1 103.6(6) 75 126_654 ? O2 Ce1 O1 91.4(13) 97 126_654 ? O2 Ce1 O1 88.6(13) 1_655 126_654 ? O1 Ce1 O1 62.24(4) 154_565 126_654 ? O1 Ce1 O1 117.76(4) 58_544 126_654 ? O2 Ce1 O1 103.6(6) 146_554 30_545 ? O2 Ce1 O1 76.4(6) 50 30_545 ? O2 Ce1 O1 103.6(6) 171_545 30_545 ? O2 Ce1 O1 76.4(6) 75 30_545 ? O2 Ce1 O1 88.6(13) 97 30_545 ? O2 Ce1 O1 91.4(13) 1_655 30_545 ? O1 Ce1 O1 117.76(4) 154_565 30_545 ? O1 Ce1 O1 62.24(4) 58_544 30_545 ? O1 Ce1 O1 180.00(17) 126_654 30_545 ? O2 Ce1 O1 76.4(6) 146_554 125_654 ? O2 Ce1 O1 103.6(6) 50 125_654 ? O2 Ce1 O1 91.4(13) 171_545 125_654 ? O2 Ce1 O1 88.6(13) 75 125_654 ? O2 Ce1 O1 76.4(6) 97 125_654 ? O2 Ce1 O1 103.6(6) 1_655 125_654 ? O1 Ce1 O1 62.24(4) 154_565 125_654 ? O1 Ce1 O1 117.76(4) 58_544 125_654 ? O1 Ce1 O1 117.76(4) 126_654 125_654 ? O1 Ce1 O1 62.24(4) 30_545 125_654 ? O2 Ce1 O1 103.6(6) 146_554 29_545 ? O2 Ce1 O1 76.4(6) 50 29_545 ? O2 Ce1 O1 88.6(13) 171_545 29_545 ? O2 Ce1 O1 91.4(13) 75 29_545 ? O2 Ce1 O1 103.6(6) 97 29_545 ? O2 Ce1 O1 76.4(6) 1_655 29_545 ? O1 Ce1 O1 117.76(4) 154_565 29_545 ? O1 Ce1 O1 62.24(4) 58_544 29_545 ? O1 Ce1 O1 62.24(4) 126_654 29_545 ? O1 Ce1 O1 117.76(4) 30_545 29_545 ? O1 Ce1 O1 180.00(17) 125_654 29_545 ? Nb1 O1 Nb1 138.7(3) 4 73 ? Nb1 O1 Ce1 104.71(9) 4 33_544 ? Nb1 O1 Ce1 104.71(9) 73 33_544 ? Nb1 O1 Ce1 104.71(9) 4 7 ? Nb1 O1 Ce1 104.71(9) 73 7 ? Ce1 O1 Ce1 87.90(17) 33_544 7 ? O2 O2 O2 60.005(18) 125 75_455 ? O2 O2 O2 60.005(18) 125 50_455 ? O2 O2 O2 60.005(17) 75_455 50_455 ? O2 O2 Ce1 134.7(13) 125 1_455 ? O2 O2 Ce1 81.3(11) 75_455 1_455 ? O2 O2 Ce1 81.3(11) 50_455 1_455 ? O2 O2 Ce1 81.3(11) 125 57_444 ? O2 O2 Ce1 134.7(13) 75_455 57_444 ? O2 O2 Ce1 81.3(11) 50_455 57_444 ? Ce1 O2 Ce1 117.4(7) 1_455 57_444 ? O2 O2 Ce1 81.3(11) 125 4_455 ? O2 O2 Ce1 81.3(11) 75_455 4_455 ? O2 O2 Ce1 134.7(13) 50_455 4_455 ? Ce1 O2 Ce1 117.4(7) 1_455 4_455 ? Ce1 O2 Ce1 117.4(7) 57_444 4_455 ? O2 O2 Ce1 35.267(10) 125 7_455 ? O2 O2 Ce1 35.267(10) 75_455 7_455 ? O2 O2 Ce1 35.267(5) 50_455 7_455 ? Ce1 O2 Ce1 99.4(13) 1_455 7_455 ? Ce1 O2 Ce1 99.4(13) 57_444 7_455 ? Ce1 O2 Ce1 99.4(13) 4_455 7_455 ? _refine_diff_density_max 0.395 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.084 _shelx_res_file ; TITL Horiuchi164Ra shelx.res created by SHELXL-2018/1 at 09:55:44 on 11-Aug-2020 CELL 0.71075 10.58980 10.58980 10.58980 90.000 90.000 90.000 ZERR 1 0.00530 0.00530 0.00530 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 11 5 56 8 SHEL 99999.000000 0.000000 L.S. 50 FMAP 2 PLAN -21 WPDB -2 HTAB BOND $H CONF LIST 3 TEMP 23.0 ACTA SIZE 0.050 0.050 0.020 EXYZ NB1 TI1 EADP NB1 TI1 WGHT 0.002800 29.687700 FVAR 0.18393 0.67383 NB1 2 0.000000 0.000000 0.000000 20.08333 0.01542 0.01542 = 0.01542 -0.00226 -0.00226 -0.00226 TI1 3 0.000000 0.000000 0.000000 -20.08333 0.01542 0.01542 = 0.01542 -0.00226 -0.00226 -0.00226 CE1 1 0.500000 0.000000 0.000000 0.03136 0.01928 0.01928 = 0.01928 0.00393 0.00393 0.00393 O1 4 0.375000 0.375000 0.066621 10.25000 0.01859 0.01859 = 0.04054 0.00000 0.00000 -0.00664 O2 4 -0.352831 0.102831 0.102831 10.04167 0.05611 0.05611 = 0.05611 0.02185 -0.02185 -0.02185 HKLF 4 REM Horiuchi164Ra REM R1 = 0.0330 for 104 Fo > 4sig(Fo) and 0.0333 for all 105 data REM 14 parameters refined using 0 restraints END WGHT 0.0029 29.7561 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.395, deepest hole -0.273, 1-sigma level 0.084 Q1 1 -0.2051 0.1250 0.1250 10.25000 0.05 0.40 Q2 1 0.2188 0.2188 0.0312 10.16667 0.05 0.27 Q3 1 0.7007 0.2007 0.0493 10.16667 0.05 0.23 Q4 1 0.1318 -0.3057 -0.1149 11.00000 0.05 0.22 Q5 1 0.0423 -0.2923 0.0423 10.16667 0.05 0.22 Q6 1 -0.3038 0.0538 0.1274 10.50000 0.05 0.21 Q7 1 0.1490 -0.1408 0.0631 11.00000 0.05 0.21 Q8 1 0.1033 -0.0763 -0.0763 10.50000 0.05 0.20 Q9 1 -0.1021 0.0322 0.1247 11.00000 0.05 0.20 Q10 1 0.1136 0.1617 0.0883 10.50000 0.05 0.17 Q11 1 -0.1150 0.1150 0.0000 10.50000 0.05 0.17 Q12 1 0.0455 0.2045 0.0455 10.16667 0.05 0.16 Q13 1 0.3226 0.0181 0.0181 10.50000 0.05 0.15 Q14 1 0.1250 0.1250 0.1250 10.04167 0.05 0.15 Q15 1 0.2500 -0.2165 0.0336 10.50000 0.05 0.14 Q16 1 -0.1250 0.2669 -0.1250 10.25000 0.05 0.13 Q17 1 0.1375 -0.1714 0.0389 11.00000 0.05 0.12 Q18 1 0.1250 0.1250 0.0124 10.25000 0.05 0.12 Q19 1 -0.0896 -0.0895 0.0592 10.50000 0.05 0.12 Q20 1 0.0421 0.0694 0.1280 11.00000 0.05 0.12 Q21 1 0.2212 -0.0396 0.1012 11.00000 0.05 0.12 ; _shelx_res_checksum 44553 _shelx_hkl_file ; 1 1 1 584.37 10.75 -1 1 -1 580.93 8.90 -1 1 -1 557.30 9.11 -1 -1 1 568.37 9.45 1 -1 -1 597.95 11.60 -1 1 1 570.69 10.21 1 -1 1 568.20 9.83 -1 -1 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