Polytypism in Columnar Group 14 Halide Salts: Structures of (Et2NH2)3Pb3X9.nH2O (X = Cl, Br) and (β-alaninium)2SnI4
Roger D. Willett; Karen R. Maxcy; Brendan Twamley; Inorganic Chemistry 41 (2002) 7024–7030; doi:10.1021/ic020455k

data_4319069
_publ_section_title
;
 Polytypism in Columnar Group 14 Halide Salts: Structures of
 (Et2NH2)3Pb3X9.nH2O (X = Cl, Br) and (\b-alaninium)2SnI4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7024
_journal_page_last               7030
_journal_paper_doi               10.1021/ic020455k
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C6 H16 I6 N2 O4 Sn2'
_chemical_formula_weight         1178.99
_chemical_name_common            (beta-alaninium)tin(II)iodide
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 95.75(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.604(3)
_cell_length_b                   13.1461(17)
_cell_length_c                   8.4823(11)
_cell_measurement_temperature    81(2)
_cell_volume                     2286.0(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      81(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            18535
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         0.99
_exptl_absorpt_coefficient_mu    10.297
_exptl_absorpt_correction_T_max  0.4258
_exptl_absorpt_correction_T_min  0.1828
_exptl_crystal_density_diffrn    3.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.132
_refine_diff_density_min         -1.842
_refine_diff_density_rms         0.273
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         5687
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0230P)^2^+2.7382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0730
_reflns_number_gt                4899
_reflns_number_total             5687
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020455k_3.cif
_cod_data_source_block           bt393
_cod_database_code               4319069