Synthesis and crystal chemistry of microporous titanates K (Ti,M)8O16 where M=Sc‒Ni
Moetakef, Pouya; Larson, Amber M.; Hodges, Brenna C.; Zavalij, Peter; Gaskell, Karen J.; Piccoli, Philip M.; Rodriguez, Efrain E.; Journal of Solid State Chemistry 220 (2014) 45–53; doi:10.1016/j.jssc.2014.08.012

data_1562187
_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         'Ni0.78 O16 Ti7.22, K1.55'
_chemical_formula_sum            'K1.55 Ni0.78 O16 Ti7.22'
_chemical_formula_weight         708.24
_chemical_name_common            'Potassium Titanium Nickel Oxide'
_chemical_name_systematic
;
Potassium Titanium Nickel 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
_audit_creation_method           'SHELXL-2014 & ZCIF'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   10.192(4)
_cell_length_b                   10.192(4)
_cell_length_c                   2.9764(13)
_cell_measurement_reflns_used    934
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.1
_cell_measurement_theta_min      2.8
_cell_volume                     309.2(2)
_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-2014, Platon (Spek, 1990)'
_computing_structure_refinement  'ShelXL-2014 (Sheldrick, 2014)'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.0521263
_diffrn_orient_matrix_UB_12      0.0831463
_diffrn_orient_matrix_UB_13      0.0032973
_diffrn_orient_matrix_UB_21      0.0612548
_diffrn_orient_matrix_UB_22      -0.0376956
_diffrn_orient_matrix_UB_23      -0.2284666
_diffrn_orient_matrix_UB_31      -0.0561934
_diffrn_orient_matrix_UB_32      0.0359803
_diffrn_orient_matrix_UB_33      -0.2463300
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_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            2156
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         31.426
_diffrn_reflns_theta_min         2.827
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    6.192
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.804
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             338.1
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.014
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.0065(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-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         303
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0175
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+1.6450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0395
_refine_ls_wR_factor_ref         0.0405
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                281
_reflns_number_total             303
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2014-220-45-2.cif
_cod_data_source_block           2533
_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        309.1(3)
_cod_original_sg_symbol_H-M      I4/m
_cod_database_code               1562187
_shelx_estimated_absorpt_t_min   0.402
_shelx_estimated_absorpt_t_max   0.941
_shelxl_version_number           2014-3
_shelx_res_checksum              58413
_shelx_hkl_checksum              82947