#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:55:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179161 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/22/4312212.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4312212
loop_
_publ_author_name
'Nicolas Mercier'
'Sylvain Poiroux'
'Amédée Riou'
'Patrick Batail'
_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       'κ-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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0126P)²+4.9855P] where P=(Fo²+2Fc²)/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
#BEGIN Tags that were not found in dictionaries:
_exptl_absorpt_correction_t_ave  0.134
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O O 0.3227(5) 0.0572(6) 0.0280(3) 0.0527(13) Uani 1 1 d . . .
N N 0.5786(7) -0.0134(6) 0.1103(3) 0.0493(14) Uani 1 1 d . . .
H2A H 0.6301 -0.0376 0.1478 0.074 Uiso 1 1 calc R . .
H2B H 0.6475 -0.0011 0.077 0.074 Uiso 1 1 calc R . .
H2C H 0.5116 -0.0892 0.1 0.074 Uiso 1 1 calc R . .
C2 C 0.4003(11) 0.1755(8) 0.0631(4) 0.062(2) Uani 1 1 d . . .
H2D H 0.3217 0.2488 0.0789 0.075 Uiso 1 1 calc R . .
H2E H 0.469 0.2299 0.0321 0.075 Uiso 1 1 calc R . .
C1 C 0.4936(10) 0.1256(10) 0.1201(5) 0.078(3) Uani 1 1 d . . .
H1A H 0.568 0.2069 0.1312 0.094 Uiso 1 1 calc R . .
H1B H 0.4238 0.1124 0.1583 0.094 Uiso 1 1 calc R . .
H1 H 0.2312 0.0278 0.0386 0.07(3) Uiso 1 1 d . . .
Pb Pb 0 0.08752(3) 0.25 0.02269(11) Uani 1 2 d S . .
Br1 Br -0.23989(7) 0.34989(7) 0.25839(3) 0.04349(18) Uani 1 1 d . . .
Br2 Br -0.03391(7) 0.09373(7) 0.10064(3) 0.04078(17) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O 0.038(2) 0.066(3) 0.053(3) -0.012(3) -0.002(2) -0.003(2)
N 0.053(3) 0.049(3) 0.046(4) 0.007(3) -0.014(3) 0.000(3)
C2 0.094(6) 0.037(4) 0.056(5) -0.001(4) -0.010(5) 0.004(4)
C1 0.081(6) 0.072(5) 0.082(7) -0.034(5) -0.025(5) 0.017(5)
Pb 0.02098(14) 0.02036(14) 0.02674(16) 0 0.00004(12) 0
Br1 0.0411(3) 0.0416(3) 0.0478(4) 0.0111(3) 0.0116(3) 0.0190(3)
Br2 0.0470(4) 0.0455(3) 0.0299(3) -0.0012(3) 0.0027(3) 0.0009(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.29 2.46 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.394 10.111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.2
0 0 1 0.03
0 0 -1 0.03
-1 -2 0 0.24
1 2 0 0.15
1 -1 0 0.2
-1 1 0 0.2
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O C2 C1 115.4(6) . . ?
N C1 C2 115.0(7) . . ?
Br2 Pb Br2 177.94(3) 4 . ?
Br2 Pb Br1 91.556(18) 4 7 ?
Br2 Pb Br1 89.846(18) . 7 ?
Br2 Pb Br1 89.846(18) 4 6_656 ?
Br2 Pb Br1 91.556(18) . 6_656 ?
Br1 Pb Br1 94.10(3) 7 6_656 ?
Br2 Pb Br1 88.697(18) 4 4 ?
Br2 Pb Br1 89.771(18) . 4 ?
Br1 Pb Br1 174.86(3) 7 4 ?
Br1 Pb Br1 91.030(8) 6_656 4 ?
Br2 Pb Br1 89.771(18) 4 . ?
Br2 Pb Br1 88.697(18) . . ?
Br1 Pb Br1 91.030(8) 7 . ?
Br1 Pb Br1 174.86(3) 6_656 . ?
Br1 Pb Br1 83.84(3) 4 . ?
Pb Br1 Pb 171.85(3) 6_566 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O C2 1.403(8) . ?
N C1 1.414(9) . ?
C2 C1 1.448(12) . ?
Pb Br2 2.9892(7) 4 ?
Pb Br2 2.9892(7) . ?
Pb Br1 3.0158(6) 7 ?
Pb Br1 3.0158(6) 6_656 ?
Pb Br1 3.0490(6) 4 ?
Pb Br1 3.0490(6) . ?
Br1 Pb 3.0158(6) 6_566 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N H2A Br1 0.89 2.58 3.458(6) 168.9 7_655
N H2B O 0.89 2.16 2.903(8) 140.4 5_655
N H2B Br2 0.89 2.86 3.413(6) 122 1_655
N H2C Br2 0.89 2.75 3.423(6) 133.6 7_655
O H1 Br2 0.842(5) 2.62 3.362(5) 147.0(3) .
