data_shelx _audit_creation_method 'SHELXL-2018/1' _shelx_SHELXL_version_number '2018/1' _chemical_name_systematic ? _chemical_name_common Hydropyrochlore _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ba4 H16 Nb15 O56 Ti' _chemical_formula_weight 2903.04 _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 'Ba' 'Ba' -0.3244 2.2819 '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 10.6014(4) _cell_length_b 10.6014(4) _cell_length_c 10.6014(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1191.47(12) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 4.046 _exptl_crystal_F_000 1325 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.040 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.030 _exptl_absorpt_coefficient_mu 6.986 _shelx_estimated_absorpt_T_min 0.767 _shelx_estimated_absorpt_T_max 0.818 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3403 _diffrn_reflns_av_unetI/netI 0.0097 _diffrn_reflns_av_R_equivalents 0.0275 _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 -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.329 _diffrn_reflns_theta_max 29.741 _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 108 _reflns_number_gt 99 _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 ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0228P)^2^+4.9050P] 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 108 _refine_ls_number_parameters 14 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0190 _refine_ls_R_factor_gt 0.0180 _refine_ls_wR_factor_ref 0.0511 _refine_ls_wR_factor_gt 0.0503 _refine_ls_goodness_of_fit_ref 1.302 _refine_ls_restrained_S_all 1.302 _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 0.0224(3) Uani 0.92(2) 12 d S T P . . Ti1 Ti 0.000000 0.000000 0.000000 0.0224(3) Uani 0.08(2) 12 d S T P . . Ba1 Ba 0.500000 0.000000 0.000000 0.0183(6) Uani 0.252(4) 12 d S T . . . O1 O 0.375000 0.375000 0.0620(2) 0.0148(6) Uani 1 4 d S T P . . O2 O -0.3476(7) 0.0976(7) 0.0976(7) 0.045(4) 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 0.0224(3) 0.0224(3) 0.0224(3) -0.00481(10) -0.00481(10) -0.00481(10) Ti1 0.0224(3) 0.0224(3) 0.0224(3) -0.00481(10) -0.00481(10) -0.00481(10) Ba1 0.0183(6) 0.0183(6) 0.0183(6) 0.0077(3) 0.0077(3) 0.0077(3) O1 0.0150(7) 0.0150(7) 0.0144(11) 0.000 0.000 -0.0032(8) O2 0.045(4) 0.045(4) 0.045(4) -0.008(3) 0.008(3) 0.008(3) _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 1.9861(7) 123 ? Nb1 O1 1.9861(7) 27_544 ? Nb1 O1 1.9861(7) 146 ? Nb1 O1 1.9861(7) 50_454 ? Nb1 O1 1.9861(7) 169 ? Nb1 O1 1.9861(7) 73_445 ? Nb1 Ba1 3.74814(12) 4_455 ? Nb1 Ba1 3.74814(12) 57_444 ? Nb1 Ba1 3.74814(12) 9_544 ? Nb1 Ba1 3.74814(12) 79_445 ? Nb1 Ba1 3.74814(12) 55_454 ? Nb1 Ba1 3.74814(12) 76_445 ? Ba1 O2 2.1797(16) 171_545 ? Ba1 O2 2.1797(16) 75 ? Ba1 O2 2.1797(16) 146_554 ? Ba1 O2 2.1797(16) 50 ? Ba1 O2 2.1797(16) 97 ? Ba1 O2 2.1797(15) 1_655 ? Ba1 O1 2.7355(16) 126_654 ? Ba1 O1 2.7355(16) 30_545 ? Ba1 O1 2.7355(16) 154_565 ? Ba1 O1 2.7355(16) 58_544 ? Ba1 O1 2.7355(16) 125_654 ? Ba1 O1 2.7355(16) 29_545 ? O2 O2 0.82(2) 125 ? O2 O2 0.82(2) 75_455 ? O2 O2 0.82(2) 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 180.00(12) 123 27_544 ? O1 Nb1 O1 89.81(8) 123 146 ? O1 Nb1 O1 90.19(8) 27_544 146 ? O1 Nb1 O1 90.19(8) 123 50_454 ? O1 Nb1 O1 89.81(8) 27_544 50_454 ? O1 Nb1 O1 180.00(12) 146 50_454 ? O1 Nb1 O1 89.81(8) 123 169 ? O1 Nb1 O1 90.19(8) 27_544 169 ? O1 Nb1 O1 89.81(8) 146 169 ? O1 Nb1 O1 90.19(8) 50_454 169 ? O1 Nb1 O1 90.19(8) 123 73_445 ? O1 Nb1 O1 89.81(8) 27_544 73_445 ? O1 Nb1 O1 90.19(8) 146 73_445 ? O1 Nb1 O1 89.81(8) 50_454 73_445 ? O1 Nb1 O1 180.00(12) 169 73_445 ? O1 Nb1 Ba1 45.10(4) 123 4_455 ? O1 Nb1 Ba1 134.90(4) 27_544 4_455 ? O1 Nb1 Ba1 134.90(4) 146 4_455 ? O1 Nb1 Ba1 45.10(4) 50_454 4_455 ? O1 Nb1 Ba1 90.0 169 4_455 ? O1 Nb1 Ba1 90.0 73_445 4_455 ? O1 Nb1 Ba1 45.10(4) 123 57_444 ? O1 Nb1 Ba1 134.90(4) 27_544 57_444 ? O1 Nb1 Ba1 90.0 146 57_444 ? O1 Nb1 Ba1 90.0 50_454 57_444 ? O1 Nb1 Ba1 134.90(4) 169 57_444 ? O1 Nb1 Ba1 45.10(4) 73_445 57_444 ? Ba1 Nb1 Ba1 60.0 4_455 57_444 ? O1 Nb1 Ba1 134.90(4) 123 9_544 ? O1 Nb1 Ba1 45.10(4) 27_544 9_544 ? O1 Nb1 Ba1 90.0 146 9_544 ? O1 Nb1 Ba1 90.0 50_454 9_544 ? O1 Nb1 Ba1 45.10(4) 169 9_544 ? O1 Nb1 Ba1 134.90(4) 73_445 9_544 ? Ba1 Nb1 Ba1 120.0 4_455 9_544 ? Ba1 Nb1 Ba1 180.0 57_444 9_544 ? O1 Nb1 Ba1 90.0 123 79_445 ? O1 Nb1 Ba1 90.0 27_544 79_445 ? O1 Nb1 Ba1 45.10(4) 146 79_445 ? O1 Nb1 Ba1 134.90(4) 50_454 79_445 ? O1 Nb1 Ba1 134.90(4) 169 79_445 ? O1 Nb1 Ba1 45.10(4) 73_445 79_445 ? Ba1 Nb1 Ba1 120.0 4_455 79_445 ? Ba1 Nb1 Ba1 60.0 57_444 79_445 ? Ba1 Nb1 Ba1 120.0 9_544 79_445 ? O1 Nb1 Ba1 90.0 123 55_454 ? O1 Nb1 Ba1 90.0 27_544 55_454 ? O1 Nb1 Ba1 134.90(4) 146 55_454 ? O1 Nb1 Ba1 45.10(4) 50_454 55_454 ? O1 Nb1 Ba1 45.10(4) 169 55_454 ? O1 Nb1 Ba1 134.90(4) 73_445 55_454 ? Ba1 Nb1 Ba1 60.0 4_455 55_454 ? Ba1 Nb1 Ba1 120.0 57_444 55_454 ? Ba1 Nb1 Ba1 60.0 9_544 55_454 ? Ba1 Nb1 Ba1 180.0 79_445 55_454 ? O1 Nb1 Ba1 134.90(4) 123 76_445 ? O1 Nb1 Ba1 45.10(4) 27_544 76_445 ? O1 Nb1 Ba1 45.10(4) 146 76_445 ? O1 Nb1 Ba1 134.90(4) 50_454 76_445 ? O1 Nb1 Ba1 90.0 169 76_445 ? O1 Nb1 Ba1 90.0 73_445 76_445 ? Ba1 Nb1 Ba1 180.0 4_455 76_445 ? Ba1 Nb1 Ba1 120.0 57_444 76_445 ? Ba1 Nb1 Ba1 60.0 9_544 76_445 ? Ba1 Nb1 Ba1 60.0 79_445 76_445 ? Ba1 Nb1 Ba1 120.0 55_454 76_445 ? O2 Ba1 O2 180.0(7) 171_545 75 ? O2 Ba1 O2 21.7(6) 171_545 146_554 ? O2 Ba1 O2 158.3(6) 75 146_554 ? O2 Ba1 O2 158.3(6) 171_545 50 ? O2 Ba1 O2 21.7(6) 75 50 ? O2 Ba1 O2 180.0(7) 146_554 50 ? O2 Ba1 O2 21.7(6) 171_545 97 ? O2 Ba1 O2 158.3(6) 75 97 ? O2 Ba1 O2 21.7(6) 146_554 97 ? O2 Ba1 O2 158.3(6) 50 97 ? O2 Ba1 O2 158.3(6) 171_545 1_655 ? O2 Ba1 O2 21.7(6) 75 1_655 ? O2 Ba1 O2 158.3(6) 146_554 1_655 ? O2 Ba1 O2 21.7(6) 50 1_655 ? O2 Ba1 O2 180.0(4) 97 1_655 ? O2 Ba1 O1 75.92(16) 171_545 126_654 ? O2 Ba1 O1 104.08(16) 75 126_654 ? O2 Ba1 O1 75.92(16) 146_554 126_654 ? O2 Ba1 O1 104.08(16) 50 126_654 ? O2 Ba1 O1 94.6(3) 97 126_654 ? O2 Ba1 O1 85.4(3) 1_655 126_654 ? O2 Ba1 O1 104.08(16) 171_545 30_545 ? O2 Ba1 O1 75.92(16) 75 30_545 ? O2 Ba1 O1 104.08(16) 146_554 30_545 ? O2 Ba1 O1 75.92(16) 50 30_545 ? O2 Ba1 O1 85.4(3) 97 30_545 ? O2 Ba1 O1 94.6(3) 1_655 30_545 ? O1 Ba1 O1 180.00(6) 126_654 30_545 ? O2 Ba1 O1 104.08(16) 171_545 154_565 ? O2 Ba1 O1 75.92(16) 75 154_565 ? O2 Ba1 O1 85.4(3) 146_554 154_565 ? O2 Ba1 O1 94.6(3) 50 154_565 ? O2 Ba1 O1 104.08(16) 97 154_565 ? O2 Ba1 O1 75.92(16) 1_655 154_565 ? O1 Ba1 O1 61.894(14) 126_654 154_565 ? O1 Ba1 O1 118.106(14) 30_545 154_565 ? O2 Ba1 O1 75.92(16) 171_545 58_544 ? O2 Ba1 O1 104.08(16) 75 58_544 ? O2 Ba1 O1 94.6(3) 146_554 58_544 ? O2 Ba1 O1 85.4(3) 50 58_544 ? O2 Ba1 O1 75.92(16) 97 58_544 ? O2 Ba1 O1 104.08(16) 1_655 58_544 ? O1 Ba1 O1 118.106(14) 126_654 58_544 ? O1 Ba1 O1 61.894(14) 30_545 58_544 ? O1 Ba1 O1 180.00(6) 154_565 58_544 ? O2 Ba1 O1 94.6(3) 171_545 125_654 ? O2 Ba1 O1 85.4(3) 75 125_654 ? O2 Ba1 O1 75.92(16) 146_554 125_654 ? O2 Ba1 O1 104.08(16) 50 125_654 ? O2 Ba1 O1 75.92(16) 97 125_654 ? O2 Ba1 O1 104.08(16) 1_655 125_654 ? O1 Ba1 O1 118.106(14) 126_654 125_654 ? O1 Ba1 O1 61.894(14) 30_545 125_654 ? O1 Ba1 O1 61.894(14) 154_565 125_654 ? O1 Ba1 O1 118.106(14) 58_544 125_654 ? O2 Ba1 O1 85.4(3) 171_545 29_545 ? O2 Ba1 O1 94.6(3) 75 29_545 ? O2 Ba1 O1 104.08(16) 146_554 29_545 ? O2 Ba1 O1 75.92(16) 50 29_545 ? O2 Ba1 O1 104.08(16) 97 29_545 ? O2 Ba1 O1 75.92(16) 1_655 29_545 ? O1 Ba1 O1 61.894(14) 126_654 29_545 ? O1 Ba1 O1 118.106(14) 30_545 29_545 ? O1 Ba1 O1 118.106(14) 154_565 29_545 ? O1 Ba1 O1 61.894(14) 58_544 29_545 ? O1 Ba1 O1 180.00(6) 125_654 29_545 ? Nb1 O1 Nb1 141.33(12) 4 73 ? Nb1 O1 Ba1 103.96(3) 4 33_544 ? Nb1 O1 Ba1 103.96(3) 73 33_544 ? Nb1 O1 Ba1 103.96(3) 4 7 ? Nb1 O1 Ba1 103.96(3) 73 7 ? Ba1 O1 Ba1 86.49(6) 33_544 7 ? O2 O2 O2 59.997(2) 125 75_455 ? O2 O2 O2 59.997(3) 125 50_455 ? O2 O2 O2 59.997(3) 75_455 50_455 ? O2 O2 Ba1 132.2(3) 125 1_455 ? O2 O2 Ba1 79.1(3) 75_455 1_455 ? O2 O2 Ba1 79.1(3) 50_455 1_455 ? O2 O2 Ba1 79.1(3) 125 57_444 ? O2 O2 Ba1 132.2(3) 75_455 57_444 ? O2 O2 Ba1 79.1(3) 50_455 57_444 ? Ba1 O2 Ba1 118.58(14) 1_455 57_444 ? O2 O2 Ba1 79.1(3) 125 4_455 ? O2 O2 Ba1 79.1(3) 75_455 4_455 ? O2 O2 Ba1 132.2(3) 50_455 4_455 ? Ba1 O2 Ba1 118.58(14) 1_455 4_455 ? Ba1 O2 Ba1 118.58(14) 57_444 4_455 ? O2 O2 Ba1 35.262(2) 125 7_455 ? O2 O2 Ba1 35.262(1) 75_455 7_455 ? O2 O2 Ba1 35.262(1) 50_455 7_455 ? Ba1 O2 Ba1 96.9(3) 1_455 7_455 ? Ba1 O2 Ba1 96.9(3) 57_444 7_455 ? Ba1 O2 Ba1 96.9(3) 4_455 7_455 ? _refine_diff_density_max 0.439 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.103 _shelx_res_file ; TITL Horiuchi166b shelx.res created by SHELXL-2018/1 at 11:09:31 on 11-Aug-2020 CELL 0.71075 10.60135 10.60135 10.60135 90.000 90.000 90.000 ZERR 1 0.00035 0.00035 0.00035 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 BA NB TI O H UNIT 4 15 1 56 16 SHEL 99999.000000 0.000000 L.S. 5 FMAP 2 PLAN -21 WPDB -2 HTAB BOND $H CONF LIST 3 TEMP 23.0 ACTA SIZE 0.040 0.040 0.030 EXYZ NB1 TI1 EADP NB1 TI1 WGHT 0.022800 4.905000 FVAR 0.20426 0.91881 NB1 2 0.000000 0.000000 0.000000 20.08333 0.02241 0.02241 = 0.02241 -0.00481 -0.00481 -0.00481 TI1 3 0.000000 0.000000 0.000000 -20.08333 0.02241 0.02241 = 0.02241 -0.00481 -0.00481 -0.00481 BA1 1 0.500000 0.000000 0.000000 0.02102 0.01827 0.01827 = 0.01827 0.00772 0.00772 0.00772 O1 4 0.375000 0.375000 0.062032 10.25000 0.01499 0.01499 = 0.01438 0.00000 0.00000 -0.00315 O2 4 -0.347576 0.097576 0.097576 10.04167 0.04463 0.04463 = 0.04463 -0.00836 0.00836 0.00836 HKLF 4 REM Horiuchi166b REM R1 = 0.0180 for 99 Fo > 4sig(Fo) and 0.0190 for all 108 data REM 14 parameters refined using 0 restraints END WGHT 0.0227 4.9141 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.439, deepest hole -0.323, 1-sigma level 0.103 Q1 1 -0.3349 0.1651 0.0849 10.16667 0.05 0.24 Q2 1 -0.1347 -0.1871 0.1022 11.00000 0.05 0.24 Q3 1 -0.0207 0.1791 0.1292 11.00000 0.05 0.21 Q4 1 -0.0733 0.0587 0.1048 11.00000 0.05 0.19 Q5 1 0.1250 -0.2710 0.1250 10.25000 0.05 0.19 Q6 1 0.0808 -0.0279 0.1054 11.00000 0.05 0.18 Q7 1 0.6250 0.1250 0.1250 10.04167 0.05 0.18 Q8 1 0.1250 0.0169 0.1250 10.25000 0.05 0.17 Q9 1 0.0096 -0.2596 0.0972 10.50000 0.05 0.15 ; _shelx_res_checksum 87536 _shelx_hkl_file ; 1 -1 -1 2187.28 52.86 -1 1 -1 2059.87 49.06 -1 -1 1 2056.64 51.00 -1 1 -1 2146.27 55.16 1 1 1 2134.21 56.53 1 -1 1 2140.76 50.79 1 1 -1 2094.69 50.96 1 1 -1 2136.20 54.86 -1 -1 -1 2196.26 52.87 -1 1 1 2065.06 50.73 -2 0 0 1.26 1.81 -2 0 0 1.61 0.92 0 -2 0 1.20 2.14 0 0 2 1.11 3.25 2 0 0 2.42 3.25 0 2 0 1.39 2.11 0 0 -2 1.32 1.72 2 -2 0 -0.17 1.53 -2 0 -2 -0.17 3.34 -2 -2 0 0.03 1.59 0 -2 -2 0.13 3.77 2 0 -2 1.09 0.87 -2 0 2 1.34 1.53 2 0 2 1.68 3.27 2 2 0 2.67 1.78 -2 2 0 1.50 2.83 0 2 -2 6.99 3.57 0 2 2 2.83 2.06 2 2 0 1.89 1.70 -2 -2 0 0.07 3.39 2 -2 0 -0.35 1.59 2 2 218261.90 715.59 -2 2 -217661.00 682.15 2 -2 -217894.00 689.07 -2 2 -217119.70 654.10 2 2 -217904.00 690.46 2 -2 217439.30 672.15 2 2 -217379.10 678.90 -2 2 217074.70 651.44 -2 -2 -218506.90 717.27 -1 1 -3 1568.32 39.15 -3 -1 1 1598.25 45.09 -1 -3 1 1566.60 37.05 -3 1 -1 1581.63 39.16 1 -1 -3 1568.14 37.61 -1 3 -1 1593.36 41.29 3 -1 -1 1466.89 37.41 -1 -1 3 1565.58 42.04 -1 -3 1 1588.66 47.96 1 3 1 1602.49 40.77 -3 1 -1 1566.97 43.02 3 1 1 1593.23 40.14 3 1 1 1587.24 40.49 1 1 3 1587.09 39.73 1 -3 -1 1557.94 39.21 -3 -1 1 1574.62 36.41 -3 1 1 1492.49 31.69 -1 3 1 1606.81 39.90 1 -1 3 1585.17 45.32 1 -3 1 1512.11 32.03 -1 -3 -1 1591.59 41.02 3 -1 1 1541.44 37.96 1 1 -3 1630.60 43.50 -3 -1 -1 1560.62 38.86 3 -1 1 1589.33 43.49 3 1 -1 1536.24 35.21 -1 1 3 1560.44 37.16 1 3 -1 1592.94 41.14 -1 -1 -3 1585.00 46.00 3 1 -1 1523.05 38.07 -3 -1 -1 1647.75 42.43 3 1 3 15.91 2.67 3 -3 -1 13.11 1.99 -3 1 -3 0.20 4.37 -3 -3 1 14.93 3.55 1 3 3 16.51 3.05 3 -1 -3 13.01 2.15 -3 1 -3 12.65 3.85 -3 3 -1 14.65 3.15 -3 -3 1 16.13 2.54 1 -3 -3 13.21 2.70 3 3 1 15.19 2.65 -3 3 -1 14.51 4.55 -1 3 -3 13.98 2.79 3 1 -3 12.81 4.49 -3 1 3 14.88 2.08 3 1 -3 13.47 1.36 1 3 -3 11.48 4.39 3 -1 3 13.57 4.29 -3 -3 -1 16.25 4.73 -1 3 3 15.42 2.54 3 3 -1 14.52 4.24 -3 3 1 13.06 1.88 -1 -3 -3 -0.14 3.17 -3 -1 -3 12.66 4.69 3 3 -1 13.23 2.08 1 3 -3 12.08 1.94 3 -3 1 12.95 3.05 -3 3 -3 3106.56 82.38 3 3 3 3258.29 89.15 3 -3 -3 3139.79 82.77 -3 3 -3 3088.92 84.45 3 3 -3 3069.98 80.25 -3 -3 -3 3204.35 88.59 -3 3 3 3149.39 84.79 3 3 -3 3144.72 89.24 -4 0 0 6427.66 185.61 0 4 0 6417.83 200.04 0 -4 0 6402.34 199.70 0 0 4 6392.84 194.80 -4 0 0 6521.79 206.97 0 0 -4 6691.64 210.36 4 0 0 6306.58 181.67 4 0 0 6041.76 186.22 -4 0 -2 -0.39 2.07 4 -2 0 1.29 1.54 4 0 -2 0.89 0.37 4 2 0 1.54 2.82 2 0 -4 2.73 2.05 -4 2 0 0.67 1.19 -4 -2 0 0.81 2.75 4 0 -2 -0.03 0.34 -4 2 0 1.44 2.67 0 2 -4 0.47 1.63 -2 -4 0 2.28 3.34 -2 0 -4 -0.11 3.01 -2 4 0 2.11 2.93 -4 2 0 0.73 1.45 0 -2 4 0.94 1.65 0 4 -2 1.31 2.11 -2 -4 0 0.11 0.99 2 -4 0 1.87 1.72 -4 -2 0 0.18 1.86 0 2 4 1.31 1.69 4 0 2 1.50 1.14 0 4 2 0.44 1.78 4 0 -2 1.00 1.74 0 -2 -4 -0.48 2.96 4 2 0 0.67 1.02 0 -4 -2 0.39 1.91 -4 0 -2 0.77 1.61 -2 0 4 1.09 1.96 2 0 4 0.94 1.72 4 -2 -2 311.03 7.05 2 -4 -2 315.36 9.15 -4 2 -2 327.04 11.42 2 4 2 342.51 14.75 2 -2 -4 338.74 11.17 2 2 4 340.95 14.23 -2 4 -2 319.36 10.64 -4 -2 2 319.96 12.38 -2 2 -4 322.12 9.83 4 2 2 340.34 12.06 4 -2 -2 311.82 9.84 -2 -4 2 321.67 7.98 -4 2 -2 324.40 10.69 -2 2 4 332.92 11.06 4 2 -2 310.10 6.96 2 4 -2 321.83 14.12 -2 4 2 334.02 12.32 -4 -2 -2 340.12 12.30 -2 -2 -4 335.12 10.30 4 2 -2 312.15 8.79 -4 2 2 311.73 6.69 2 -2 4 330.70 13.52 -4 -2 -2 314.36 9.59 2 4 -2 332.87 8.11 -2 -4 -2 341.06 10.81 4 -2 2 325.73 11.33 2 -4 2 329.79 7.46 2 2 -4 330.27 11.44 4 -2 2 337.57 11.06 -4 0 -415350.40 585.76 -4 -4 015537.50 591.16 0 4 415670.90 590.95 -4 0 414419.30 527.76 4 4 015719.20 596.92 4 0 415361.20 582.79 0 4 -415345.80 586.54 4 -4 014937.50 562.27 -4 4 015279.80 577.22 -4 0 -411925.50 455.45 0 -4 -415361.70 589.77 -4 -4 015450.80 582.45 4 0 -415216.90 556.03 4 -4 -2 2.00 2.12 2 4 4 3.35 2.14 -4 4 -2 1.68 1.84 4 4 2 1.11 1.84 -4 -4 2 1.10 1.31 -4 -4 2 0.73 2.73 -4 2 -4 2.02 2.89 -4 4 -2 2.11 1.87 4 -2 -4 1.88 1.47 -2 4 -4 1.22 3.36 4 2 4 2.16 1.83 -4 4 -2 1.73 1.44 -4 2 -4 1.03 1.44 2 -4 -4 2.44 1.64 -2 4 -4 2.28 1.02 4 4 -2 1.29 1.25 -4 4 2 1.15 1.95 -4 2 4 1.39 1.40 -4 -2 -4 2.36 3.20 4 2 -4 2.27 2.72 4 2 -4 1.62 1.66 4 4 -2 1.68 1.54 -2 -4 -4 1.48 3.83 4 -4 2 1.26 1.74 2 4 -4 3.10 1.41 2 4 -4 1.55 2.07 -4 -4 -2 -0.11 3.19 -4 -4 -2 3.45 3.23 4 2 -4 1.10 1.22 2 4 -4 2.09 1.72 -2 4 4 0.97 1.60 4 -2 4 2.22 1.64 4 -4 -4 7737.32 254.91 -4 4 -4 8241.12 267.45 4 4 4 8702.73 290.56 -4 4 -4 8103.93 275.18 4 4 -4 7988.63 264.31 -4 -4 -4 8563.60 295.07 4 4 -4 8086.84 270.18 -4 4 4 8437.56 278.51 4 4 -4 8122.77 270.28 5 1 1 56.78 3.67 -1 -1 5 51.24 5.93 1 -5 -1 56.92 7.50 -1 -5 1 54.55 2.29 -5 1 -1 55.61 2.09 -5 -1 1 57.11 2.79 5 -1 -1 58.17 6.79 -5 -1 1 54.59 4.18 -1 -5 1 53.99 4.94 1 1 5 59.24 7.02 -1 1 -5 55.17 4.23 1 5 1 56.91 7.55 1 -1 -5 60.03 6.06 -1 5 -1 55.99 4.78 5 1 1 59.22 6.70 -5 1 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