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#$Date: 2019-11-11 03:11:33 +0200 (Mon, 11 Nov 2019) $
#$Revision: 226226 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/31/4003121.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_4003121
loop_
_publ_author_name
'Liu, Mei'
'Zhao, Jiangtao'
'Luo, Zhenlin'
'Sun, Zhihu'
'Pan, Nan'
'Ding, Huaiyi'
'Wang, Xiaoping'
_publ_section_title
;
 Unveiling Solvent-Related Effect on Phase Transformations in CsBr--PbBr2
 System: Coordination and Ratio of Precursors
;
_journal_issue                   17
_journal_name_full               'Chemistry of Materials'
_journal_page_first              5846
_journal_paper_doi               10.1021/acs.chemmater.8b00537
_journal_volume                  30
_journal_year                    2018
_chemical_formula_sum            'C3 H7 Br2 N O Pb'
_chemical_formula_weight         440.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 93.576(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.3483(2)
_cell_length_b                   17.6677(12)
_cell_length_c                   11.4806(7)
_cell_measurement_reflns_used    1737
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.9520
_cell_measurement_theta_min      3.7460
_cell_volume                     880.27(9)
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies)'
_computing_data_collection       'CrysAlisPro (Agilent Technologies)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies)'
_computing_molecular_graphics    'Ortep-3 (L. J. Farrugia, 2001)'
_computing_publication_material  SHELXL-2013
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9149
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Gemini S Ultra, Agilent Technologies'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.1013
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8975
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         37.613
_diffrn_reflns_theta_min         3.556
_exptl_absorpt_coefficient_mu    28.169
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.321
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.383
_refine_diff_density_min         -2.925
_refine_diff_density_rms         0.326
_refine_ls_extinction_coef       0.0100(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         4394
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1239
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0344P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1223
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2497
_reflns_number_total             4394
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm8b00537_si_002.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4003121
_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   0.101
_shelx_estimated_absorpt_t_max   0.165
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Pb1 Pb 0.73239(6) 0.52275(2) 0.32591(3) 0.03388(12) Uani 1 1 d . .
Br1 Br 0.25724(18) 0.60160(5) 0.47096(9) 0.0430(2) Uani 1 1 d . .
Br2 Br 1.2098(2) 0.46089(7) 0.17619(10) 0.0601(3) Uani 1 1 d . .
O1 O 0.6793(16) 0.6365(4) 0.2122(6) 0.0580(18) Uani 1 1 d . .
N1 N 0.3916(17) 0.7017(4) 0.0791(7) 0.0432(17) Uani 1 1 d . .
C2 C 0.557(2) 0.6439(6) 0.1117(9) 0.050(2) Uani 1 1 d . .
H2 H 0.5871 0.6059 0.0575 0.060 Uiso 1 1 calc R U
C1 C 0.322(2) 0.7601(6) 0.1622(9) 0.056(3) Uani 1 1 d . .
H1A H 0.3028 0.7378 0.2376 0.083 Uiso 1 1 calc R U
H1B H 0.1323 0.7846 0.1372 0.083 Uiso 1 1 calc R U
H1C H 0.4856 0.7968 0.1670 0.083 Uiso 1 1 calc R U
C3 C 0.263(2) 0.7100(6) -0.0428(9) 0.060(3) Uani 1 1 d . .
H3A H 0.3571 0.6735 -0.0913 0.089 Uiso 1 1 calc R U
H3B H 0.3047 0.7601 -0.0702 0.089 Uiso 1 1 calc R U
H3C H 0.0446 0.7018 -0.0458 0.089 Uiso 1 1 calc R U
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
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'
O O 0.0106 0.0060 '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
O1 Pb1 Br2 87.10(17) . 1_455
O1 Pb1 Br2 92.31(17) . .
Br2 Pb1 Br2 93.81(3) 1_455 .
O1 Pb1 Br1 82.51(17) . .
Br2 Pb1 Br1 87.96(3) 1_455 .
Br2 Pb1 Br1 174.44(3) . .
O1 Pb1 Br1 87.59(17) . 1_655
Br2 Pb1 Br1 174.55(3) 1_455 1_655
Br2 Pb1 Br1 87.62(3) . 1_655
Br1 Pb1 Br1 90.14(3) . 1_655
O1 Pb1 Br1 165.28(18) . 3_666
Br2 Pb1 Br1 98.31(3) 1_455 3_666
Br2 Pb1 Br1 100.92(3) . 3_666
Br1 Pb1 Br1 84.01(3) . 3_666
Br1 Pb1 Br1 86.57(3) 1_655 3_666
Pb1 Br1 Pb1 90.14(3) . 1_455
Pb1 Br1 Pb1 95.99(3) . 3_666
Pb1 Br1 Pb1 93.43(2) 1_455 3_666
Pb1 Br2 Pb1 93.81(3) 1_655 .
C2 O1 Pb1 127.7(7) . .
C2 N1 C1 120.5(9) . .
C2 N1 C3 121.5(9) . .
C1 N1 C3 118.0(8) . .
O1 C2 N1 123.2(10) . .
O1 C2 H2 118.4 . .
N1 C2 H2 118.4 . .
N1 C1 H1A 109.5 . .
N1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
N1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
N1 C3 H3A 109.5 . .
N1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
N1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O1 2.400(7) .
Pb1 Br2 2.9708(11) 1_455
Pb1 Br2 2.9838(10) .
Pb1 Br1 3.0679(9) .
Pb1 Br1 3.0738(10) 1_655
Pb1 Br1 3.2022(10) 3_666
Br1 Pb1 3.0738(10) 1_455
Br1 Pb1 3.2022(10) 3_666
Br2 Pb1 2.9708(11) 1_655
O1 C2 1.246(12) .
N1 C2 1.292(12) .
N1 C1 1.451(12) .
N1 C3 1.481(12) .
C2 H2 0.9300 .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
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
Pb1 O1 C2 N1 141.5(8)
C1 N1 C2 O1 -3.9(15)
C3 N1 C2 O1 177.0(9)
