Structural elucidation of triclinic and monoclinic SFCA-III ‒ killing two birds with one stone
Kahlenberg, Volker; Krüger, Hannes; Goettgens, Valerie Sue; Acta Crystallographica Section B 75 (2019) –; doi:10.1107/S2052520619014380

data_2108540
_publ_section_title
;
 Structural elucidation of triclinic and monoclinic SFCA-III -- killing
 two birds with one stone
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520619014380
_journal_volume                  75
_journal_year                    2019
_chemical_formula_sum            'Al18.241 Ca11.96 Fe61.4 Mg10.68 O144 Si1.72'
_chemical_formula_weight         7012.3
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 109.668(2)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   10.3277(2)
_cell_length_b                   27.0134(4)
_cell_length_c                   10.4344(2)
_cell_measurement_reflns_used    9772
_cell_measurement_temperature    293
_cell_measurement_theta_max      34.05
_cell_measurement_theta_min      2.25
_cell_volume                     2741.22(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_diffrn_ambient_temperature      295(3)
_diffrn_detector                 'hybrid pixel CMOS'
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            PILATUS2M-F
_diffrn_measured_fraction_theta_full 0.9951
_diffrn_measured_fraction_theta_max 0.8753
_diffrn_measurement_details
;
 Swiss Light Source, Paul Scherrer Insitute, Villigen, Switzerland
 Beamline X06DA (PXIII)
 single omega-scan
 1800 frames, detector distance = 80 mm
 oscillation 0.1 deg, 0.2 sec exposure
;
_diffrn_measurement_device       'singlei-axis goniometer'
_diffrn_measurement_device_type  Aerotech
_diffrn_measurement_method       'rotation method'
_diffrn_measurement_specimen_support fiber
_diffrn_radiation_monochromator
;Bartels Monochromator with dual channel cut crystals (DCCM) 
 in (+--+) geometry
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'SLS super-bending magnet 2.9T, X06DA'
_diffrn_radiation_wavelength     0.72931
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0733
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            26137
_diffrn_reflns_theta_full        27.1176
_diffrn_reflns_theta_max         33.6992
_diffrn_reflns_theta_min         1.5471
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    9.16
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    4.2478
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3357
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    1.82
_refine_ls_goodness_of_fit_ref   1.58
_refine_ls_number_constraints    435
_refine_ls_number_parameters     1171
_refine_ls_number_reflns         14341
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.0390
_refine_ls_shift/su_mean         0.0077
_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          0.0543
_refine_ls_wR_factor_ref         0.0564
_reflns_number_gt                10407
_reflns_number_total             14341
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            dk5093sup1.cif
_cod_data_source_block           SFCA-III-monoclinic
_cod_original_sg_symbol_Hall     '-P 2yabc'
_cod_original_formula_sum        'Al18.241 Ca11.96 Fe61.4 O144 Mg10.68 Si1.72'
_cod_database_code               2108540