#------------------------------------------------------------------------------
#$Date: 2021-04-28 10:38:16 +0300 (Wed, 28 Apr 2021) $
#$Revision: 264623 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/21/1562191.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1562191
loop_
_publ_author_name
'Moetakef, Pouya'
'Larson, Amber M.'
'Hodges, Brenna C.'
'Zavalij, Peter'
'Gaskell, Karen J.'
'Piccoli, Philip M.'
'Rodriguez, Efrain E.'
_publ_section_title
;
 Synthesis and crystal chemistry of microporous titanates K (Ti,M)8O16
 where M=Sc--Ni
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              45
_journal_page_last               53
_journal_paper_doi               10.1016/j.jssc.2014.08.012
_journal_volume                  220
_journal_year                    2014
_chemical_formula_moiety         '8(O2 Ti),  1.36(K)'
_chemical_formula_sum            'K1.36 O16 Ti8'
_chemical_formula_weight         692.49
_chemical_name_common            'Potassium titanium oxide'
_chemical_name_systematic
;
Potassium titanium oxide
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   10.2386(17)
_cell_length_b                   10.2386(17)
_cell_length_c                   2.9794(5)
_cell_measurement_reflns_used    1887
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      2.8
_cell_volume                     312.33(9)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2010)'
_computing_data_reduction        'Apex2, Saint'
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  'Apex2, SHELXL-2012'
_computing_structure_refinement  'ShelXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'ShelXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart Apex II diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0917035
_diffrn_orient_matrix_UB_12      0.0245393
_diffrn_orient_matrix_UB_13      -0.0787762
_diffrn_orient_matrix_UB_21      0.0246178
_diffrn_orient_matrix_UB_22      0.0944963
_diffrn_orient_matrix_UB_23      0.0085348
_diffrn_orient_matrix_UB_31      0.0227930
_diffrn_orient_matrix_UB_32      -0.0034327
_diffrn_orient_matrix_UB_33      -0.3261517
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_av_unetI/netI     0.0102
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            2420
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         31.241
_diffrn_reflns_theta_min         2.813
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    5.389
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.682
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             330
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.018
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.0129(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     29
_refine_ls_number_reflns         302
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.0158
_refine_ls_R_factor_gt           0.0147
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0100P)²+1.7350P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0391
_refine_ls_wR_factor_ref         0.0396
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                288
_reflns_number_total             302
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            JSSC-2014-220-45-2.cif
_cod_data_source_block           2559
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Tetragonal' was changed to
'tetragonal' in accordance with the built-in table derived from the
CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated
on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 
;
_cod_original_cell_volume        312.33(12)
_cod_original_sg_symbol_H-M      I4/m
_cod_database_code               1562191
_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.
;
_shelx_estimated_absorpt_t_min   0.314
_shelx_estimated_absorpt_t_max   0.909
_shelxl_version_number           2012-9
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
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
K1 K 0.0000 0.0000 0.139(12) 0.013(3) Uani 0.21(3) 4 d S TU . . .
K2 K 0.0000 0.0000 0.241(13) 0.012(4) Uani 0.10(2) 4 d S TU . . .
K3 K 0.0000 0.0000 0.0000 0.012(5) Uani 0.07(4) 8 d S T . . .
Ti1 Ti 0.66718(3) 0.14986(4) 0.0000 0.00593(14) Uani 1 2 d S T P . .
O1 O 0.53948(14) 0.16603(14) 0.5000 0.0064(3) Uani 1 2 d S T P . .
O2 O 0.70448(14) 0.34385(14) 0.0000 0.0056(3) Uani 1 2 d S T P . .
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'
K K 0.2009 0.2494 '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'
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
O1 Ti1 O2 92.09(5) 15 13_655
O1 Ti1 O2 92.09(5) 15 13_654
O2 Ti1 O2 97.10(6) 13_655 13_654
O1 Ti1 O1 94.54(7) 15 .
O2 Ti1 O1 82.56(5) 13_655 .
O2 Ti1 O1 173.37(6) 13_654 .
O1 Ti1 O1 94.54(7) 15 1_554
O2 Ti1 O1 173.37(6) 13_655 1_554
O2 Ti1 O1 82.56(5) 13_654 1_554
O1 Ti1 O1 97.00(6) . 1_554
O1 Ti1 O2 169.46(6) 15 .
O2 Ti1 O2 80.99(5) 13_655 .
O2 Ti1 O2 80.99(5) 13_654 .
O1 Ti1 O2 92.43(5) . .
O1 Ti1 O2 92.43(5) 1_554 .
Ti1 O1 Ti1 131.14(3) 7_545 1_556
Ti1 O1 Ti1 131.14(3) 7_545 .
Ti1 O1 Ti1 97.00(6) 1_556 .
Ti1 O2 Ti1 97.10(6) 13_655 13_654
Ti1 O2 Ti1 99.02(5) 13_655 .
Ti1 O2 Ti1 99.02(5) 13_654 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 O2 2.846(14) 7_545
K1 O2 2.846(14) 15_455
K1 O2 2.846(14) 5_445
K1 O2 2.846(14) 13
K2 O2 2.745(11) 7_545
K2 O2 2.745(11) 15_455
K2 O2 2.745(11) 5_445
K2 O2 2.745(11) 13
K3 O2 3.0263(13) 15_454
K3 O2 3.0263(13) 7_545
K3 O2 3.0263(13) 15_455
Ti1 O1 1.9386(15) 15
Ti1 O2 1.9875(10) 13_655
Ti1 O2 1.9875(10) 13_654
Ti1 O1 1.9890(10) .
Ti1 O1 1.9890(10) 1_554
Ti1 O2 2.0225(15) .
Ti1 Ti1 2.9794(5) 1_556
Ti1 Ti1 2.9794(5) 1_554
Ti1 Ti1 3.0497(7) 13_655
Ti1 Ti1 3.0497(7) 13_654
O1 Ti1 1.9386(15) 7_545
O1 Ti1 1.9890(10) 1_556
O2 Ti1 1.9875(10) 13_655
O2 Ti1 1.9875(10) 13_654
O2 K2 2.745(11) 5_554
O2 K2 2.745(11) 13
O2 K1 2.845(14) 5_554
O2 K1 2.845(14) 13
O2 K3 3.0263(13) 5_554
O2 K3 3.0263(13) 5
O2 K1 3.25(2) 13_554
O2 K1 3.25(2) 5
