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#$Date: 2021-04-01 01:29:13 +0300 (Thu, 01 Apr 2021) $
#$Revision: 263498 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/38/4003897.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_4003897
loop_
_publ_author_name
'Mączka, Mirosław'
'Zaręba, Jan K.'
'Gągor, Anna'
'Stefańska, Dagmara'
'Ptak, Maciej'
'Roleder, Krystian'
'Kajewski, Dariusz'
'Soszyński, Andrzej'
'Fedoruk, Katarzyna'
'Sieradzki, Adam'
_publ_section_title
;
 [Methylhydrazinium]2PbBr4, a Ferroelectric Hybrid Organic--Inorganic
 Perovskite with Multiple Nonlinear Optical Outputs
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.0c04440
_journal_year                    2021
_chemical_formula_moiety         'Br4 Pb, 2(C H5 N2)'
_chemical_formula_sum            'C2 H14 Br4 N4 Pb'
_chemical_formula_weight         621.00
_space_group_crystal_system      orthorhombic
_space_group_IT_number           59
_space_group_name_Hall           '-P 2c 2a'
_space_group_name_H-M_alt        'P m n m :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.1597(12)
_cell_length_b                   6.0526(3)
_cell_length_c                   6.0368(3)
_cell_measurement_reflns_used    2219
_cell_measurement_temperature    380.1(2)
_cell_measurement_theta_max      28.8770
_cell_measurement_theta_min      4.0080
_cell_volume                     663.53(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      380.1(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4115
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.682
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         3.366
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    24.720
_exptl_absorpt_correction_T_max  0.419
_exptl_absorpt_correction_T_min  0.043
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    3.108
_exptl_crystal_description       plate
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.273
_exptl_crystal_size_min          0.114
_refine_diff_density_max         1.955
_refine_diff_density_min         -1.210
_refine_diff_density_rms         0.288
_refine_ls_extinction_coef       0.0024(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         726
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0647P)²+1.2623P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1053
_reflns_Friedel_coverage         0.000
_reflns_number_gt                659
_reflns_number_total             726
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm0c04440_si_002.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P m n m'
_cod_database_code               4003897
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.565
_oxdiff_exptl_absorpt_empirical_full_max 1.944
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, z+1/2'
'x+1/2, -y, -z'
'-x, -y, -z'
'x-1/2, -y, z-1/2'
'x, y, -z-1/2'
'-x-1/2, y, z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.250000 0.92110(9) 0.750000 0.0381(3) Uani 1 4 d S T P . .
Br1 Br 0.250000 0.8745(4) 0.250000 0.0658(7) Uani 1 4 d S T P . .
Br2 Br 0.08559(10) 0.9077(3) 0.750000 0.0790(6) Uani 1 2 d S T P . .
Br3 Br 0.250000 0.4323(3) 0.750000 0.0924(11) Uani 1 4 d S T P . .
N1 N 0.0245(17) 0.639(4) 0.250000 0.155(11) Uani 1 2 d DS T P . .
N2 N 0.0839(13) 0.527(4) 0.172(4) 0.111(10) Uani 0.5 1 d D . P . .
H2A H 0.120296 0.625439 0.170525 0.134 Uiso 0.5 1 calc R U P . .
H2B H 0.073570 0.499538 0.030283 0.134 Uiso 0.5 1 calc R U P . .
C3 C 0.1152(15) 0.336(4) 0.250000 0.114(9) Uani 1 2 d DS T P . .
H3A H 0.082580 0.213883 0.222763 0.171 Uiso 0.5 1 calc R U P . .
H3B H 0.123729 0.349209 0.406353 0.171 Uiso 0.5 1 calc R U P . .
H3C H 0.161137 0.310405 0.175571 0.171 Uiso 0.5 1 calc R U P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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
-10 -9 1 0.1264
-24 0 0 0.0536
24 0 0 0.0604
6 10 2 0.0843
-22 4 1 0.0658
-3 0 -8 0.1267
2 -1 8 0.1436
4 8 0 0.0933
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
Br3 Pb1 Br2 88.45(4) . 2_556 ?
Br3 Pb1 Br2 88.45(4) . . ?
Br2 Pb1 Br2 176.89(7) 2_556 . ?
Br3 Pb1 Br1 84.66(4) . . ?
Br2 Pb1 Br1 89.855(4) 2_556 . ?
Br2 Pb1 Br1 89.855(4) . . ?
Br3 Pb1 Br1 84.66(4) . 1_556 ?
Br2 Pb1 Br1 89.855(4) 2_556 1_556 ?
Br2 Pb1 Br1 89.855(4) . 1_556 ?
Br1 Pb1 Br1 169.32(9) . 1_556 ?
Br3 Pb1 Br3 180.0 . 1_565 ?
Br2 Pb1 Br3 91.55(4) 2_556 1_565 ?
Br2 Pb1 Br3 91.55(4) . 1_565 ?
Br1 Pb1 Br3 95.34(4) . 1_565 ?
Br1 Pb1 Br3 95.34(4) 1_556 1_565 ?
Pb1 Br1 Pb1 169.32(9) 1_554 . ?
Pb1 Br3 Pb1 180.0 . 1_545 ?
N1 N2 C3 129(2) . . ?
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
Pb1 Br3 2.9587(18) . ?
Pb1 Br2 2.9868(19) 2_556 ?
Pb1 Br2 2.9868(18) . ?
Pb1 Br1 3.0316(3) . ?
Pb1 Br1 3.0316(3) 1_556 ?
Pb1 Br3 3.0938(18) 1_565 ?
N1 N2 1.358(18) 7_556 ?
N1 N2 1.358(18) . ?
N2 C3 1.374(17) . ?
