#------------------------------------------------------------------------------
#$Date: 2020-01-14 02:31:34 +0200 (Tue, 14 Jan 2020) $
#$Revision: 246790 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/70/1557023.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_1557023
loop_
_publ_author_name
'Bakthavatsalam, Rangarajan'
'Haris, Muhammed P. U.'
'Shaikh, Samir R.'
'Lohar, Amruta'
'Mohanty, Ashutosh'
'Moghe, Dhanashree'
'Sharma, Shivani'
'Biswas, Chinmoy'
'Raavi, Sai Santhosh Kumar'
'Gonnade, Rajesh G.'
'Kundu, Janardan'
_publ_section_title
;
 Ligand Structure Directed Dimensionality Reduction (2D → 1D)
 in Lead Bromide Perovskite
;
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_paper_doi               10.1021/acs.jpcc.9b11033
_journal_year                    2020
_chemical_formula_moiety         'Pb Br4, C3 H11 N3 S'
_chemical_formula_sum            'C3 H11 Br4 N3 Pb S'
_chemical_formula_weight         648.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.406(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3113(5)
_cell_length_b                   8.5838(4)
_cell_length_c                   12.0368(5)
_cell_measurement_reflns_used    6667
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      3.06
_cell_volume                     1375.31(10)
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Photon II CPAD Area Detector'
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON II CPAD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16587
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.344
_diffrn_reflns_theta_min         2.824
_diffrn_source                   'micro-focus sealed tube'
_diffrn_source_type              'Incoatech I\mS HB'
_exptl_absorpt_coefficient_mu    24.004
_exptl_absorpt_correction_T_max  0.380
_exptl_absorpt_correction_T_min  0.086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (BRUKER, 2016)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.130
_exptl_crystal_description       plate
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.609
_refine_diff_density_min         -1.352
_refine_diff_density_rms         0.261
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         3423
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0479P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0887
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2814
_reflns_number_total             3423
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            jp9b11033_si_002.cif
_cod_data_source_block           iso_PbBr4_0ma_a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1557023
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_min   0.086
_shelx_estimated_absorpt_t_max   0.380
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Pb01 Pb 0.15080(2) 0.77880(3) 0.26883(2) 0.02487(10) Uani 1 1 d . .
Br1 Br -0.04910(5) 0.60684(8) 0.26629(5) 0.04090(18) Uani 1 1 d . .
Br2 Br 0.25156(6) 0.48718(8) 0.24996(5) 0.04471(19) Uani 1 1 d . .
Br3 Br 0.34764(4) 0.94003(8) 0.28762(5) 0.03622(16) Uani 1 1 d . .
Br4 Br 0.14443(5) 0.77446(9) 0.01786(5) 0.04341(19) Uani 1 1 d . .
S1 S 0.59030(14) 0.7189(2) -0.06863(14) 0.0442(4) Uani 1 1 d . .
N1 N 0.8778(4) 0.8120(7) 0.0364(5) 0.0434(14) Uani 1 1 d . .
H1NA H 0.9032 0.8367 -0.0314 0.065 Uiso 1 1 calc R U
H1NB H 0.9230 0.7525 0.0744 0.065 Uiso 1 1 calc R U
H1NC H 0.8656 0.9009 0.0752 0.065 Uiso 1 1 calc R U
N2 N 0.4204(5) 0.7277(8) 0.0334(6) 0.062(2) Uani 1 1 d . .
H2NA H 0.3775 0.7529 0.0857 0.074 Uiso 1 1 calc R U
H2NB H 0.4004 0.6714 -0.0237 0.074 Uiso 1 1 calc R U
N3 N 0.5431(5) 0.8568(8) 0.1242(5) 0.0545(17) Uani 1 1 d . .
H3NA H 0.5005 0.8822 0.1768 0.065 Uiso 1 1 calc R U
H3NB H 0.6060 0.8878 0.1286 0.065 Uiso 1 1 calc R U
C1 C 0.7820(5) 0.7229(7) 0.0215(6) 0.0354(15) Uani 1 1 d . .
H1A H 0.7537 0.6968 0.0951 0.042 Uiso 1 1 calc R U
H1B H 0.7953 0.6244 -0.0185 0.042 Uiso 1 1 calc R U
C2 C 0.7076(5) 0.8204(8) -0.0438(5) 0.0344(14) Uani 1 1 d . .
H2A H 0.7376 0.8492 -0.1160 0.041 Uiso 1 1 calc R U
H2B H 0.6940 0.9178 -0.0025 0.041 Uiso 1 1 calc R U
C3 C 0.5131(5) 0.7738(8) 0.0403(5) 0.0359(15) Uani 1 1 d . .
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'
Br Br -0.2901 2.4595 '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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
Br2 Pb01 Br3 89.99(2) . .
Br2 Pb01 Br4 85.374(18) . .
Br3 Pb01 Br4 95.759(18) . .
Br2 Pb01 Br4 87.87(2) . 4_576
Br3 Pb01 Br4 91.476(18) . 4_576
Br4 Pb01 Br4 170.091(12) . 4_576
Br2 Pb01 Br1 89.15(2) . .
Br3 Pb01 Br1 176.035(17) . .
Br4 Pb01 Br1 88.031(19) . .
Br4 Pb01 Br1 84.624(18) 4_576 .
Br2 Pb01 Br1 167.452(19) . 2
Br3 Pb01 Br1 88.380(18) . 2
Br4 Pb01 Br1 82.413(18) . 2
Br4 Pb01 Br1 104.606(19) 4_576 2
Br1 Pb01 Br1 93.285(10) . 2
Pb01 Br1 Pb01 144.05(3) . 2_545
Pb01 Br4 Pb01 171.42(3) . 4_575
C3 S1 C2 105.0(3) . .
C1 N1 H1NA 109.5 . .
C1 N1 H1NB 109.5 . .
H1NA N1 H1NB 109.5 . .
C1 N1 H1NC 109.5 . .
H1NA N1 H1NC 109.5 . .
H1NB N1 H1NC 109.5 . .
C3 N2 H2NA 120.0 . .
C3 N2 H2NB 120.0 . .
H2NA N2 H2NB 120.0 . .
C3 N3 H3NA 120.0 . .
C3 N3 H3NB 120.0 . .
H3NA N3 H3NB 120.0 . .
N1 C1 C2 109.5(5) . .
N1 C1 H1A 109.8 . .
C2 C1 H1A 109.8 . .
N1 C1 H1B 109.8 . .
C2 C1 H1B 109.8 . .
H1A C1 H1B 108.2 . .
C1 C2 S1 112.3(5) . .
C1 C2 H2A 109.1 . .
S1 C2 H2A 109.1 . .
C1 C2 H2B 109.1 . .
S1 C2 H2B 109.1 . .
H2A C2 H2B 107.9 . .
N3 C3 N2 120.3(7) . .
N3 C3 S1 123.9(5) . .
N2 C3 S1 115.8(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb01 Br2 2.8498(7) .
Pb01 Br3 2.9705(6) .
Pb01 Br4 3.0217(6) .
Pb01 Br4 3.0340(6) 4_576
Pb01 Br1 3.0428(6) .
Pb01 Br1 3.1515(7) 2
Br1 Pb01 3.1515(7) 2_545
Br4 Pb01 3.0339(6) 4_575
S1 C3 1.737(7) .
S1 C2 1.812(6) .
N1 C1 1.497(9) .
N1 H1NA 0.9100 .
N1 H1NB 0.9100 .
N1 H1NC 0.9100 .
N2 C3 1.299(9) .
N2 H2NA 0.8800 .
N2 H2NB 0.8800 .
N3 C3 1.297(8) .
N3 H3NA 0.8800 .
N3 H3NB 0.8800 .
C1 C2 1.513(9) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
N1 C1 C2 S1 178.5(4)
C3 S1 C2 C1 93.1(5)
C2 S1 C3 N3 -6.5(7)
C2 S1 C3 N2 172.8(6)
