On the ambient pressure polymorph of K2Ca3Si3O10—An unusual mixed-anion silicate and its structural and spectroscopic characterization
Schmidmair, Daniela; Kahlenberg, Volker; Perfler, Lukas; Tribus, Martina; Hildebrandt, Johannes; Többens, Daniel M.; Journal of Solid State Chemistry 228 (2015) 90–98; doi:10.1016/j.jssc.2015.04.019

data_1561885
_publ_section_title
;
 On the ambient pressure polymorph of K2Ca3Si3O10---An unusual mixed-anion
 silicate and its structural and spectroscopic characterization
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              90
_journal_page_last               98
_journal_paper_doi               10.1016/j.jssc.2015.04.019
_journal_volume                  228
_journal_year                    2015
_chemical_formula_moiety         'O6 Si2, 0.5(O8 Si2), 3(Ca), 2(K)'
_chemical_formula_sum            'Ca3 K2 O10 Si3'
_chemical_formula_weight         442.71
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                86.199(11)
_cell_angle_beta                 80.625(9)
_cell_angle_gamma                88.700(11)
_cell_formula_units_Z            2
_cell_length_a                   5.6699(6)
_cell_length_b                   7.3754(12)
_cell_length_c                   11.8310(13)
_cell_measurement_reflns_used    1556
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.5038
_cell_measurement_theta_min      2.7624
_cell_volume                     487.03(11)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
        (compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
        (compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
        (compiled Jul 11 2012,15:38:31)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 10.3575
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0572049
_diffrn_orient_matrix_UB_12      -0.0816129
_diffrn_orient_matrix_UB_13      -0.0189462
_diffrn_orient_matrix_UB_21      -0.084381
_diffrn_orient_matrix_UB_22      -0.0083589
_diffrn_orient_matrix_UB_23      -0.0374562
_diffrn_orient_matrix_UB_31      0.0754088
_diffrn_orient_matrix_UB_32      0.0506004
_diffrn_orient_matrix_UB_33      -0.0441057
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2972
_diffrn_reflns_theta_full        25.33
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    2.967
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.92922
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
        (compiled Jul 11 2012,15:38:31)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.019
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    .
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         1761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0261
_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^)+(0.0254P)^2^+0.0778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0622
_reflns_number_gt                1490
_reflns_number_total             1761
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2015-228-90.cif
_cod_data_source_block           kristall05_rt_lang
_cod_database_code               1561885