Unique Hydrogen Bonding Correlating with a Reduced Band Gap and Phase Transition in the Hybrid Perovskites (HO(CH2)2NH3)2PbX4 (X = I, Br)
Nicolas Mercier; Sylvain Poiroux; Amédée Riou; Patrick Batail; Inorganic Chemistry 43 (2004) 8361–8366; doi:10.1021/ic048814u

data_4312212
_publ_contact_author_address
;
Laboratoire Ingenierie Moleculaire Materiaux Organiques
UMR CNRS 6501, Faculte des Sciences, 2 Bd Lavoisier, F-49045 Angers, France
;
_publ_contact_author_email       nicolas.mercier@univ-angers.fr
_publ_contact_author_fax         (33)2.41.73.54.05
_publ_contact_author_name        'Mercier, Nicolas'
_publ_contact_author_phone       (33)2.41.73.50.83
_publ_section_title
;
 Unique Hydrogen Bonding Correlating with a Reduced Band Gap and Phase
 Transition in the Hybrid Perovskites (HO(CH2)2NH3)2PbX4 (X = I, Br)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8361
_journal_page_last               8366
_journal_paper_doi               10.1021/ic048814u
_journal_volume                  43
_journal_year                    2004
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C4 H16 Br4 N2 O2 Pb1'
_chemical_formula_sum            'C4 H16 Br4 N2 O2 Pb'
_chemical_formula_weight         651
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2004-03-03T10:02:11-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4625(6)
_cell_length_b                   8.6470(10)
_cell_length_c                   19.918(2)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     1457.5(2)
_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-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  area_detector
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1178
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            28871
_diffrn_reflns_theta_full        30.09
_diffrn_reflns_theta_max         30.09
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    22.521
_exptl_absorpt_correction_T_max  0.2603
_exptl_absorpt_correction_T_min  0.0068
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
        a grid of 46 x 44 x  8 = 16192 sampling points was used
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.967
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.018
_refine_diff_density_min         -1.703
_refine_diff_density_rms         0.215
_refine_ls_extinction_coef       0.00493(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         2119
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0126P)^2^+4.9855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.058
_refine_ls_wR_factor_ref         0.0647
_reflns_number_gt                1540
_reflns_number_total             2119
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048814usi20040826_080724_1.cif
_cod_data_source_block           (NH3-CH2-CH2-OH)PbBr4
_cod_database_code               4312212
_exptl_absorpt_correction_t_ave  0.134