Synthesis, Crystal Structure, and Vibrational Spectroscopy of K2Ca4Si8O21 - An Unusual Single-Layer Silicate Containing Q2 and Q3 Units
Erik Arroyabe; Reinhard Kaindl; Daniel M. Többens; Volker Kahlenberg; Inorganic Chemistry 48 (2009) 11929–11934; doi:10.1021/ic901762u

data_4303862
_publ_contact_author_address
;
Institute of Mineralogy and Petrography
University of Innsbruck
Innrain 52
A-6020 Innsbruck
Austria
;
_publ_contact_author_email       volker.kahlenberg@uibk.ac.at
_publ_contact_author_fax         43(512)5072926
_publ_contact_author_name        'Kahlenberg, Volker'
_publ_contact_author_phone       43(512)5075503
_publ_section_title
;
Synthesis, Crystal Structure, and Vibrational Spectroscopy of
K2Ca4Si8O21 - An Unusual Single-Layer Silicate Containing Q2 and Q3 Units
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11929
_journal_page_last               11934
_journal_paper_doi               10.1021/ic901762u
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'Ca4 K2 O21 Si8'
_chemical_formula_weight         799.24
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2009-09-04T10:48:01-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                96.680(4)
_cell_angle_beta                 105.280(4)
_cell_angle_gamma                109.259(4)
_cell_formula_units_Z            1
_cell_length_a                   6.8052(3)
_cell_length_b                   7.1049(3)
_cell_length_c                   11.2132(5)
_cell_measurement_reflns_used    2792
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.3304
_cell_measurement_theta_min      3.1081
_cell_volume                     481.27(4)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
        (compiled Jan 27 2009,14:17:37)
;
_computing_data_collection
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
        (compiled Jan 27 2009,14:17:37)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
        (compiled Jan 27 2009,14:17:37)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 10.3822
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.838
_diffrn_measurement_device_type
'Goniometer Xcalibur, detector: Ruby (Gemini ultra Mo)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0294613181
_diffrn_orient_matrix_UB_12      0.0459437538
_diffrn_orient_matrix_UB_13      0.0485891902
_diffrn_orient_matrix_UB_21      -0.0097543577
_diffrn_orient_matrix_UB_22      -0.0863432253
_diffrn_orient_matrix_UB_23      0.0273921867
_diffrn_orient_matrix_UB_31      0.1124896784
_diffrn_orient_matrix_UB_32      0.0468824243
_diffrn_orient_matrix_UB_33      0.0375993602
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3987
_diffrn_reflns_theta_full        25.5
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    2.166
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.84822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
        (compiled Jan 27 2009,14:17:37)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.758
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular fragment'
_exptl_crystal_F_000             398
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.48
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+0.1285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0682
_reflns_number_gt                1736
_reflns_number_total             2026
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic901762u_si_001.cif
_cod_data_source_block           kristall_2
_cod_database_code               4303862