High pressure synthesis and crystal structure of a ternary superconductor Ca2Al3Si4 containing layer structured calcium sub-network isomorphous with black phosphorus
Tanaka, Masashi; Zhang, Shuai; Tanaka, Yuki; Inumaru, Kei; Yamanaka, Shoji; Journal of Solid State Chemistry 198 (2013) 445–451; doi:10.1016/j.jssc.2012.11.011

data_1562774
_publ_section_title
;
 High pressure synthesis and crystal structure of a ternary superconductor
 Ca2Al3Si4 containing layer structured calcium sub-network isomorphous
 with black phosphorus
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              445
_journal_page_last               451
_journal_paper_doi               10.1016/j.jssc.2012.11.011
_journal_volume                  198
_journal_year                    2013
_chemical_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'Al3 Ca2 Si4'
_chemical_formula_sum            'Al3 Ca2 Si4'
_chemical_formula_weight         273.46
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      36
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_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                   5.8846(8)
_cell_length_b                   14.9730(10)
_cell_length_c                   7.7966(5)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     686.96(11)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2639
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.72
_exptl_absorpt_coefficient_mu    2.624
_exptl_absorpt_correction_T_max  0.769
_exptl_absorpt_correction_T_min  0.737
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrystalClear, Rigaku, 2007'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.144
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.44(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.13
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         709
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.13
_refine_ls_R_factor_all          0.034
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0433P)^2^+1.9235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.0913
_reflns_number_gt                667
_reflns_number_total             709
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2013-198-445.cif
_cod_data_source_block           struct
_cod_database_code               1562774