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_4319067
_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            'C4 H12 Br3 N Pb'
_chemical_formula_weight         521.07
_chemical_name_common            (diethylammonium)lead(II)bromide
_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                 111.50(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   10.753(6)
_cell_length_b                   23.976(11)
_cell_length_c                   14.239(6)
_cell_measurement_temperature    293(2)
_cell_volume                     3416(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.856
_diffrn_measured_fraction_theta_max 0.856
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0662
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4196
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    25.284
_exptl_crystal_density_diffrn    3.040
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2760
_refine_diff_density_max         1.606
_refine_diff_density_min         -1.605
_refine_diff_density_rms         0.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4196
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0538P)^2^+79.5476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1409
_refine_ls_wR_factor_ref         0.1489
_reflns_number_gt                3596
_reflns_number_total             4196
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020455k_1.cif
_cod_data_source_block           p21c-a
_cod_database_code               4319067