Ca5.45Li3.55[SiO4]3O0.45F1.55 and Ca7K[SiO4]3F3: single-crystal synthesis and structures of two trigonal oxyfluorides
Krüger, Hannes; Zeitschrift für Kristallographie - Crystalline Materials 225 (2010) 418–424; doi:10.1524/zkri.2010.1268

data_8103064
_publ_contact_author_address
;
 Institut f\"ur Mineralogie und Petrographie
 Universit\"at Innsbruck
 Innrain 52
 6020 Innsbruck
 Austria
;
_publ_contact_author_email       Hannes.Krueger@uibk.ac.at
_publ_contact_author_fax         43(512)5072926
_publ_contact_author_name        'Kr\"uger, Hannes'
_publ_contact_author_phone       43(512)5075502
_publ_section_title
;
 Ca5.45Li3.55[SiO4]3O0.45F1.55 and Ca7K[SiO4]3F3: single-crystal synthesis
 and structures of two trigonal oxyfluorides
;
_journal_issue                   10
_journal_name_full
'Zeitschrift f\"ur Kristallographie - Crystalline Materials'
_journal_page_first              418
_journal_page_last               424
_journal_paper_doi               10.1524/zkri.2010.1268
_journal_volume                  225
_journal_year                    2010
_chemical_formula_sum            'Ca5.45 F1.55 Li3.55 O12.45 Si3'
_chemical_formula_weight         556
_space_group_IT_number           166
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_audit_contact_author_address
;
 Institut f\"ur Mineralogie und Petrographie
 Universit\"at Innsbruck
 Innrain 52
 6020 Innsbruck
 Austria
;
_audit_contact_author_email      Hannes.Krueger@uibk.ac.at
_audit_contact_author_fax        43(512)5072926
_audit_contact_author_name       'Kr\"uger, Hannes'
_audit_contact_author_phone      43(512)5075502
_audit_creation_date             2010-03-17
_audit_creation_method
;
 Jana2000 Version : 18/12/2007
 STOE X-RED
 enCIFer 1.3
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   7.1365(6)
_cell_length_b                   7.1365(6)
_cell_length_c                   41.459(3)
_cell_measurement_reflns_used    3534
_cell_measurement_temperature    298
_cell_measurement_theta_max      32.00
_cell_measurement_theta_min      5.02
_cell_volume                     1828.6(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    DRAWxtl
_computing_publication_material
'Jana2000 (Petricek, Dusek & Palatinus, 2000)'
_computing_structure_refinement
'Jana2000 (Petricek, Dusek & Palatinus, 2000)'
_computing_structure_solution
'Superflip (Palatinus & Chapuis, 2007, J. Appl. Cryst. 40, 786-790)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measurement_details
;
 360 frames, detector distance = 80 mm
 one run 180 frames, exposure time 30 sec
 one run 180 frames, exposure time 3 min
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0039
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            14478
_diffrn_reflns_reduction_process
;
 STOE X-AREA/INTEGRATE 1.39
 two runs integrated seperately
;
_diffrn_reflns_theta_full        31.84
_diffrn_reflns_theta_max         31.84
_diffrn_reflns_theta_min         2.95
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.77
_exptl_absorpt_correction_T_max  0.6083
_exptl_absorpt_correction_T_min  0.4860
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
 STOE XRED32 1.31
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.028
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1650
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.317
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.74
_refine_diff_density_min         -1.07
_refine_ls_extinction_coef       19925(1391)
_refine_ls_extinction_method
'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)'
_refine_ls_goodness_of_fit_gt    3.44
_refine_ls_goodness_of_fit_ref   3.33
_refine_ls_number_parameters     65
_refine_ls_number_reflns         1675
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/(\s^2^(F)+0.0001F^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0432
_refine_ls_wR_factor_ref         0.0436
_reflns_d_resolution_high        0.673
_reflns_d_resolution_low         6.910
_reflns_number_gt                1545
_reflns_number_total             1675
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            Ca5.45Li3.55Si3O12.45F1.55.cif
_cod_data_source_block           Ca5.45Li3.55Si3O12.45F1.55
_cod_original_sg_symbol_Hall     '-R 3;-2'
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               8103064