Redetermination of katayamalite, KLi~3~Ca~7~Ti~2~(SiO~3~)~12~(OH)~2~
Andrade, Marcelo B.; Doell, Donald; Downs, Robert T.; Yang, Hexiong; Acta Crystallographica Section E 69 (2013) i41–; doi:10.1107/S1600536813016620

data_2238282
_publ_section_title
;
 Redetermination of katayamalite, KLi~3~Ca~7~Ti~2~(SiO~3~)~12~(OH)~2~
;
_journal_coeditor_code           WM2749
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i41
_journal_paper_doi               10.1107/S1600536813016620
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'K Li3 Ca7 Ti2 (Si O3)12 (O H)2'
_chemical_formula_moiety         '2(O18 Si6 Ti), 2(H O), 7(Ca), K, 3(Li)'
_chemical_formula_structural     'K Li3 Ca7 Ti2 (Si O3)12 (O H)2'
_chemical_formula_sum            'Ca7 H2 K Li3 O38 Si12 Ti2'
_chemical_formula_weight         1383.38
_chemical_name_common            ' katayamalite'
_chemical_name_systematic
;
Potassium trilithium heptacalcium dititanium dodecasilicate dihydroxide
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.396(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.9093(10)
_cell_length_b                   9.7287(5)
_cell_length_c                   20.9019(12)
_cell_measurement_reflns_used    5222
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.180
_cell_measurement_theta_min      2.654
_cell_volume                     3179.1(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'Xtal-Draw (Downs & Hall-Wallace, 2003)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.853
_diffrn_measurement_device_type  'Bruker X8 APEXII CCD'
_diffrn_measurement_method       '\f and \w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26611
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         32.40
_diffrn_reflns_theta_min         2.11
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.361
_exptl_absorpt_correction_T_max  0.8911
_exptl_absorpt_correction_T_min  0.8713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.890
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.561
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4873
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+0.7329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0825
_reflns_number_gt                3632
_reflns_number_total             4873
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            wm2749.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2238282
_cod_database_fobs_code          2238282