data_Kyzulkumite _ccdc_journal_manuscript_code 'Mineral. Mag.' _publ_contact_author_name 'Thomas Armbruster' _publ_contact_author_address ;Mineralogical Crystallography Institute of Geological Sciences University of Bern Freiestr. 3, CH- 3012 Bern Switzerland ; _publ_contact_author_email thomas.armbruster@krist.unibe.ch loop_ _publ_author_name _publ_author_address 'Armbruster, T.' ;Mineralogical Crystallography Institute of Geological Sciences University of Bern Freiestr. 3, CH- 3012 Bern Switzerland ; 'Lazic, B.' ;Mineralogical Crystallography Institute of Geological Sciences University of Bern Freiestr. 3, CH- 3012 Bern Switzerland ; 'Reznitsky, L.Z.' ;Institute of the Earth?s crust (IZK) SB RAS 664033 Irkutsk-33 Russia ; 'Sklyarov, E.V.' ;Institute of the Earth?s crust (IZK) SB RAS 664033 Irkutsk-33 Russia ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'H2 O12 Ti5 V' _chemical_melting_point ? #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description irregular _exptl_crystal_colour blue #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _chemical_formula_weight 484.46 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.47870(10) _cell_length_b 4.56240(10) _cell_length_c 10.03300(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.1740(10) _cell_angle_gamma 90.00 _cell_volume 387.513(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1925 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 61.06 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.152 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 462 _exptl_absorpt_coefficient_mu 6.137 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.733 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details TWINABS _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Apex II Smart' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1150 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0127 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 30.51 _reflns_number_total 1150 _reflns_number_gt 936 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ATOMS V6.3' _computing_publication_material 'Bruker SHELXTL' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+0.1255P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0019(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1150 _refine_ls_number_parameters 87 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0624 _refine_ls_wR_factor_gt 0.0582 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 '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' V V 0.3005 0.5294 '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' 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 M1 Ti 0.08253(4) -0.00466(7) -0.12620(3) 0.00721(10) Uani 1 1 d . . . M2 Ti 0.22693(5) -0.00921(7) -0.38492(3) 0.00843(10) Uani 1 1 d . . . M3 Ti 0.39733(4) 0.00554(6) -0.65117(4) 0.00821(10) Uani 1 1 d . . . O1 O 0.07493(19) -0.2216(3) -0.29701(15) 0.0082(3) Uani 1 1 d . . . O2 O 0.25205(19) 0.2163(3) -0.21405(15) 0.0087(3) Uani 1 1 d . . . O3 O -0.0892(2) -0.2159(3) -0.04235(15) 0.0089(3) Uani 1 1 d . . . O4 O -0.24574(19) 0.2820(3) 0.05147(15) 0.0086(3) Uani 1 1 d . . . O5 O -0.41865(19) -0.2119(3) 0.45759(15) 0.0082(3) Uani 1 1 d D . . O6 O 0.4144(2) -0.2463(3) -0.80111(16) 0.0092(3) Uani 1 1 d . . . H5 H -0.421(4) -0.420(2) 0.452(3) 0.050 Uiso 1 1 d D . . 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 M1 0.00681(19) 0.00821(16) 0.00667(18) -0.00016(10) 0.00079(13) -0.00003(11) M2 0.00867(19) 0.00946(17) 0.00726(17) 0.00006(11) 0.00144(12) 0.00050(12) M3 0.00677(18) 0.00808(15) 0.00986(17) 0.00082(11) 0.00128(12) 0.00139(12) O1 0.0087(8) 0.0090(5) 0.0072(7) -0.0006(4) 0.0017(5) -0.0024(5) O2 0.0075(8) 0.0095(5) 0.0091(7) 0.0002(5) -0.0002(6) -0.0016(5) O3 0.0088(8) 0.0095(5) 0.0082(7) -0.0001(4) 0.0007(5) -0.0024(5) O4 0.0080(8) 0.0097(5) 0.0082(7) 0.0015(4) 0.0003(6) 0.0024(5) O5 0.0077(7) 0.0080(5) 0.0088(7) 0.0003(4) 0.0009(5) -0.0009(5) O6 0.0066(8) 0.0104(5) 0.0106(7) -0.0022(4) 0.0011(6) -0.0006(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 M1 O3 1.9659(15) 3 ? M1 O3 1.9727(16) . ? M1 O1 1.9770(14) . ? M1 O1 1.9824(14) 2_554 ? M1 O4 1.9908(14) 3 ? M1 O2 1.9997(16) . ? M1 M2 2.9307(4) . ? M1 M1 2.9607(6) 3 ? M2 O1 1.8718(16) . ? M2 O3 1.8956(15) 2_554 ? M2 O4 1.9376(15) 2_544 ? M2 O2 2.0006(14) . ? M2 O5 2.0791(16) 3 ? M2 O6 2.0812(16) 4_556 ? M2 M3 3.1072(5) . ? M2 M3 3.1864(5) 3_654 ? M3 O2 1.8548(14) 4_565 ? M3 O6 1.9047(15) . ? M3 O4 1.9583(15) 2_544 ? M3 O6 2.0355(16) 2_653 ? M3 O5 2.1025(15) 1_654 ? M3 O5 2.1568(15) 3 ? M3 M2 3.1864(5) 3_654 ? O1 M1 1.9824(14) 2_544 ? O2 M3 1.8548(14) 4_566 ? O3 M2 1.8956(15) 2_544 ? O3 M1 1.9659(15) 3 ? O4 M2 1.9376(15) 2_554 ? O4 M3 1.9583(15) 2_554 ? O4 M1 1.9908(14) 3 ? O5 M2 2.0791(16) 3 ? O5 M3 2.1025(15) 1_456 ? O5 M3 2.1568(15) 3 ? O5 H5 0.951(10) . ? O6 M3 2.0355(16) 2_643 ? O6 M2 2.0812(16) 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 O3 M1 O3 82.52(7) 3 . ? O3 M1 O1 179.23(6) 3 . ? O3 M1 O1 97.80(6) . . ? O3 M1 O1 89.28(6) 3 2_554 ? O3 M1 O1 89.25(7) . 2_554 ? O1 M1 O1 90.02(4) . 2_554 ? O3 M1 O4 90.87(6) 3 3 ? O3 M1 O4 92.46(7) . 3 ? O1 M1 O4 89.82(6) . 3 ? O1 M1 O4 178.29(6) 2_554 3 ? O3 M1 O2 97.70(6) 3 . ? O3 M1 O2 178.39(7) . . ? O1 M1 O2 81.95(6) . . ? O1 M1 O2 89.16(6) 2_554 . ? O4 M1 O2 89.13(6) 3 . ? O3 M1 M2 140.54(5) 3 . ? O3 M1 M2 136.77(5) . . ? O1 M1 M2 39.09(4) . . ? O1 M1 M2 88.04(5) 2_554 . ? O4 M1 M2 90.76(5) 3 . ? O2 M1 M2 42.90(4) . . ? O3 M1 M1 41.35(5) 3 3 ? O3 M1 M1 41.17(4) . 3 ? O1 M1 M1 138.97(5) . 3 ? O1 M1 M1 89.02(5) 2_554 3 ? O4 M1 M1 92.21(5) 3 3 ? O2 M1 M1 139.03(5) . 3 ? M2 M1 M1 176.46(2) . 3 ? O1 M2 O3 96.96(7) . 2_554 ? O1 M2 O4 104.10(6) . 2_544 ? O3 M2 O4 95.37(6) 2_554 2_544 ? O1 M2 O2 84.60(6) . . ? O3 M2 O2 90.05(6) 2_554 . ? O4 M2 O2 169.07(7) 2_544 . ? O1 M2 O5 171.29(7) . 3 ? O3 M2 O5 89.97(6) 2_554 3 ? O4 M2 O5 80.37(6) 2_544 3 ? O2 M2 O5 90.16(6) . 3 ? O1 M2 O6 93.59(7) . 4_556 ? O3 M2 O6 167.06(6) 2_554 4_556 ? O4 M2 O6 89.28(6) 2_544 4_556 ? O2 M2 O6 83.49(6) . 4_556 ? O5 M2 O6 78.88(6) 3 4_556 ? O1 M2 M1 41.76(4) . . ? O3 M2 M1 93.28(5) 2_554 . ? O4 M2 M1 145.65(5) 2_544 . ? O2 M2 M1 42.88(4) . . ? O5 M2 M1 132.86(4) 3 . ? O6 M2 M1 89.61(5) 4_556 . ? O1 M2 M3 141.38(5) . . ? O3 M2 M3 87.69(5) 2_554 . ? O4 M2 M3 37.33(4) 2_544 . ? O2 M2 M3 133.87(5) . . ? O5 M2 M3 43.80(4) 3 . ? O6 M2 M3 88.73(5) 4_556 . ? M1 M2 M3 176.563(17) . . ? O1 M2 M3 131.25(5) . 3_654 ? O3 M2 M3 129.12(5) 2_554 3_654 ? O4 M2 M3 88.34(5) 2_544 3_654 ? O2 M2 M3 80.89(5) . 3_654 ? O5 M2 M3 40.63(4) 3 3_654 ? O6 M2 M3 38.77(4) 4_556 3_654 ? M1 M2 M3 111.309(15) . 3_654 ? M3 M2 M3 65.671(14) . 3_654 ? O2 M3 O6 102.84(7) 4_565 . ? O2 M3 O4 95.04(6) 4_565 2_544 ? O6 M3 O4 99.80(6) . 2_544 ? O2 M3 O6 93.09(6) 4_565 2_653 ? O6 M3 O6 93.14(4) . 2_653 ? O4 M3 O6 162.78(7) 2_544 2_653 ? O2 M3 O5 163.57(6) 4_565 1_654 ? O6 M3 O5 92.21(6) . 1_654 ? O4 M3 O5 88.76(6) 2_544 1_654 ? O6 M3 O5 79.37(6) 2_653 1_654 ? O2 M3 O5 91.64(6) 4_565 3 ? O6 M3 O5 165.50(6) . 3 ? O4 M3 O5 78.00(6) 2_544 3 ? O6 M3 O5 86.63(6) 2_653 3 ? O5 M3 O5 73.49(6) 1_654 3 ? O2 M3 M2 88.60(5) 4_565 . ? O6 M3 M2 136.49(5) . . ? O4 M3 M2 36.87(4) 2_544 . ? O6 M3 M2 128.48(5) 2_653 . ? O5 M3 M2 84.87(5) 1_654 . ? O5 M3 M2 41.85(4) 3 . ? O2 M3 M2 132.54(5) 4_565 3_654 ? O6 M3 M2 88.48(5) . 3_654 ? O4 M3 M2 128.68(5) 2_544 3_654 ? O6 M3 M2 39.81(4) 2_653 3_654 ? O5 M3 M2 40.09(4) 1_654 3_654 ? O5 M3 M2 82.07(4) 3 3_654 ? M2 M3 M2 114.329(14) . 3_654 ? M2 O1 M1 99.15(6) . . ? M2 O1 M1 128.36(8) . 2_544 ? M1 O1 M1 130.69(8) . 2_544 ? M3 O2 M1 132.46(8) 4_566 . ? M3 O2 M2 132.89(9) 4_566 . ? M1 O2 M2 94.21(6) . . ? M2 O3 M1 132.86(9) 2_544 3 ? M2 O3 M1 129.37(8) 2_544 . ? M1 O3 M1 97.48(7) 3 . ? M2 O4 M3 105.79(6) 2_554 2_554 ? M2 O4 M1 123.27(8) 2_554 3 ? M3 O4 M1 126.93(8) 2_554 3 ? M2 O5 M3 99.28(6) 3 1_456 ? M2 O5 M3 94.35(6) 3 3 ? M3 O5 M3 106.51(6) 1_456 3 ? M2 O5 H5 119(2) 3 . ? M3 O5 H5 115(2) 1_456 . ? M3 O5 H5 120(2) 3 . ? M3 O6 M3 128.05(9) . 2_643 ? M3 O6 M2 123.54(9) . 4 ? M3 O6 M2 101.43(6) 2_643 4 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5 O6 0.951(10) 2.12(2) 2.901(2) 138(3) 2_544 O5 H5 O5 0.951(10) 2.37(3) 3.110(3) 134(3) 3_446 O5 H5 O4 0.951(10) 2.40(3) 3.106(2) 130(3) 4_556 _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.504 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.111