One-pot occurrence of two polymorphs of Rb 2 Sc[Si 4 O 10 ]F and their structural, spectroscopic and computational characterization
Kahlenberg, Volker; Manninger, Tanja; Perfler, Lukas; Többens, Daniel M.; Journal of Solid State Chemistry 220 (2014) 79–90; doi:10.1016/j.jssc.2014.08.002

data_1562201
_publ_section_title
;
 One-pot occurrence of two polymorphs of Rb 2 Sc[Si 4 O 10 ]F and their
 structural, spectroscopic and computational characterization
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              79
_journal_page_last               90
_journal_paper_doi               10.1016/j.jssc.2014.08.002
_journal_volume                  220
_journal_year                    2014
_chemical_formula_moiety         'F O10 Sc Si4, 2(Rb)'
_chemical_formula_sum            'F O10 Rb2 Sc Si4'
_chemical_formula_weight         507.26
_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_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2619(3)
_cell_length_b                   11.2619(3)
_cell_length_c                   8.3053(4)
_cell_measurement_reflns_used    2649
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.5934
_cell_measurement_theta_min      3.0414
_cell_volume                     1053.36(6)
_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      298(2)
_diffrn_detector_area_resol_mean 10.3575
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0226744
_diffrn_orient_matrix_UB_12      0.0188063
_diffrn_orient_matrix_UB_13      0.0755011
_diffrn_orient_matrix_UB_21      0.0187751
_diffrn_orient_matrix_UB_22      0.0542047
_diffrn_orient_matrix_UB_23      -0.0352079
_diffrn_orient_matrix_UB_31      -0.055691
_diffrn_orient_matrix_UB_32      0.0259218
_diffrn_orient_matrix_UB_33      0.0188876
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6887
_diffrn_reflns_theta_full        25.33
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    10.396
_exptl_absorpt_correction_T_max  0.685
_exptl_absorpt_correction_T_min  0.535
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         516
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0231
_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^)+(0.0356P)^2^+0.1944P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0581
_refine_ls_wR_factor_ref         0.0585
_reflns_number_gt                510
_reflns_number_total             516
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2014-220-79.cif
_cod_data_source_block           rbf_sc2o3_b_rt
_cod_database_code               1562201