Extraordinary structural complexity of ilmajokite: a multilevel hierarchical framework structure of natural origin
Zolotarev, Jr, Andrey A.; Krivovichev, Sergey V.; Cámara, Fernando; Bindi, Luca; Zhitova, Elena S.; Hawthorne, Frank; Sokolova, Elena; IUCrJ 7 (2020) 121–128; doi:10.1107/S2052252519016622

data_1556729
_publ_section_title
;
 Extraordinary structural complexity of ilmajokite: a multilevel
 hierarchical framework structure of natural origin
;
_journal_coeditor_code           LT5023SUP1
_journal_issue                   1
_journal_name_full               IUCrJ
_journal_page_first              121
_journal_page_last               128
_journal_paper_doi               10.1107/S2052252519016622
_journal_volume                  7
_journal_year                    2020
_chemical_formula_moiety
'0.06(Ba7.21 Ce16.68 K8.85 Na90.08 O1228.82 Si300.33 Ti96)'
_chemical_formula_sum
'Ba0.45 Ce1.04 K0.55 Na5.62 O76.74 Si18.76 Ti6'
_chemical_formula_weight         2445.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 96.494(3)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   35.908(5)
_cell_length_b                   27.784(3)
_cell_length_c                   33.126(4)
_cell_measurement_reflns_used    21527
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.52
_cell_measurement_theta_min      2.37
_cell_volume                     32837(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1301
_diffrn_reflns_av_unetI/netI     0.1048
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            108441
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        22.694
_diffrn_reflns_theta_max         22.694
_diffrn_reflns_theta_min         0.929
_exptl_absorpt_coefficient_mu    1.784
_exptl_absorpt_correction_T_max  0.7448
_exptl_absorpt_correction_T_min  0.5744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1858 before and 0.0891 after correction. The Ratio of minimum to maximum transmission is 0.7712. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_description       prism
_exptl_crystal_F_000             18664
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.890
_refine_diff_density_min         -2.798
_refine_diff_density_rms         0.233
_refine_ls_extinction_coef       0.000146(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014)'
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1847
_refine_ls_number_reflns         21527
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0807
_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/[\s^2^(Fo^2^)+(0.1738P)^2^+608.3564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2338
_refine_ls_wR_factor_ref         0.2638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14797
_reflns_number_total             21527
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5023.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 1556729.cif.'
_cod_original_cell_volume        32836(7)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1556729
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              56878
_shelx_hkl_checksum              10015