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_4319068
_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            'C12 H36 I9 N3 O0 Pb3'
_chemical_formula_weight         1986.11
_chemical_name_common            (diethylammonium)lead(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                 110.917(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.281(7)
_cell_length_b                   24.917(15)
_cell_length_c                   14.371(8)
_cell_measurement_temperature    183(2)
_cell_volume                     3773(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0718
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34298
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    20.722
_exptl_crystal_density_diffrn    3.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3408
_refine_diff_density_max         2.040
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         6651
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          6.184
_refine_ls_shift/su_mean         0.025
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0730
_reflns_number_gt                4142
_reflns_number_total             6651
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020455k_2.cif
_cod_data_source_block           bt311
_cod_original_cell_volume        3774(4)
_cod_database_code               4319068