Tropochemical Cell-Twinning in the New Quaternary Bismuth Selenides KxSn6-2xBi2+xSe9 and KSn5Bi5Se13
Antje Mrotzek; Mercouri G. Kanatzidis; Inorganic Chemistry 42 (2003) 7200–7206; doi:10.1021/ic034252n

data_4312377
_publ_section_title
;
 Tropochemical Cell-Twinning in the New Quaternary Bismuth Selenides
 KxSn6-2xBi2+xSe9 and KSn5Bi5Se13
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7200
_journal_page_last               7206
_journal_paper_doi               10.1021/ic034252n
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'Bi5 K Se13 Sn5'
_chemical_formula_weight         2703.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.012(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.879(4)
_cell_length_b                   4.2050(11)
_cell_length_c                   23.363(6)
_cell_measurement_temperature    298(2)
_cell_volume                     1346.7(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.907
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0656
_diffrn_reflns_av_sigmaI/netI    0.0559
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            6270
_diffrn_reflns_theta_full        28.71
_diffrn_reflns_theta_max         28.71
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    54.808
_exptl_crystal_density_diffrn    6.668
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2252
_refine_diff_density_max         6.426
_refine_diff_density_min         -3.861
_refine_diff_density_rms         0.720
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         1795
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0752
_refine_ls_shift/su_max          0.221
_refine_ls_shift/su_mean         0.023
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0059P)^2^+488.1357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1427
_refine_ls_wR_factor_ref         0.1503
_reflns_number_gt                1364
_reflns_number_total             1795
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034252nsi20030308_085121_1.cif
_cod_data_source_block           KSn5Bi5Se13"
_cod_original_cell_volume        1346.6(6)
_cod_database_code               4312377