#------------------------------------------------------------------------------
#$Date: 2019-11-11 03:11:49 +0200 (Mon, 11 Nov 2019) $
#$Revision: 226227 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/31/4003122.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_4003122
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            'Br3 H2 O Pb1.5'
_chemical_formula_weight         568.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 101.398(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2606(7)
_cell_length_b                   4.3331(2)
_cell_length_c                   12.5000(8)
_cell_measurement_reflns_used    2039
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      36.1430
_cell_measurement_theta_min      4.0270
_cell_volume                     650.98(6)
_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      298(2)
_diffrn_detector_area_resol_mean 15.9149
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.947
_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  0.0613
_diffrn_reflns_av_unetI/netI     0.1027
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6433
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         37.580
_diffrn_reflns_theta_min         3.325
_exptl_absorpt_coefficient_mu    57.073
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.05286
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    5.801
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_refine_diff_density_max         7.692
_refine_diff_density_min         -8.201
_refine_diff_density_rms         0.966
_refine_ls_extinction_coef       0.044(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         3602
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1218
_refine_ls_R_factor_gt           0.0811
_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)+(0.1022P)²+16.6455P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1895
_refine_ls_wR_factor_ref         0.2260
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2415
_reflns_number_total             3602
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm8b00537_si_001.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_original_formula_sum        'H2 Br3 O Pb1.50'
_cod_database_code               4003122
_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   0.056
_shelx_estimated_absorpt_t_max   0.070
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
Pb1 Pb 0.57429(7) 0.2500 0.19514(8) 0.0280(2) Uani 1 2 d S T P
Pb2 Pb 0.19173(8) 0.7500 0.06529(8) 0.0343(3) Uani 1 2 d S T P
Pb3 Pb -0.04401(8) 0.2500 0.32390(9) 0.0363(3) Uani 1 2 d S T P
Br2 Br 0.36655(16) 0.2500 -0.01003(16) 0.0217(4) Uani 1 2 d S T P
Br5 Br 0.10162(16) -0.2500 0.44369(17) 0.0223(4) Uani 1 2 d S T P
Br3 Br 0.17952(15) 0.2500 0.22513(17) 0.0213(4) Uani 1 2 d S T P
Br4 Br -0.05623(16) 0.7500 0.10334(18) 0.0240(4) Uani 1 2 d S T P
Br1 Br 0.42723(15) 0.7500 0.23983(17) 0.0211(4) Uani 1 2 d S T P
Br6 Br -0.23373(16) -0.2500 0.30929(18) 0.0242(4) Uani 1 2 d S T P
O1 O 0.5818(14) 0.2500 0.3989(13) 0.026(3) Uani 1 2 d S T P
H1 H 0.6119 0.0706 0.4323 0.039 Uiso 1 1 d R U .
O2 O 0.6308(16) 0.7500 0.5325(17) 0.037(4) Uani 1 2 d GS T P
H2 H 0.5913 0.8158 0.5755 0.055 Uiso 1 1 d G U .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pb Pb -3.3944 10.1111 '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'
H H 0.0000 0.0000 '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 Br1 73.2(2) . .
O1 Pb1 Br1 73.2(2) . 1_545
Br1 Pb1 Br1 94.85(6) . 1_545
O1 Pb1 Br2 131.6(4) . .
Br1 Pb1 Br2 74.62(5) . .
Br1 Pb1 Br2 74.61(5) 1_545 .
Br3 Pb2 Br3 93.65(6) . 1_565
Br3 Pb2 Br4 73.84(5) . .
Br3 Pb2 Br4 73.84(5) 1_565 .
Br5 Pb3 Br5 92.03(6) 1_565 .
Br5 Pb3 Br5 76.01(5) 1_565 3_556
Br5 Pb3 Br5 76.01(5) . 3_556
Br5 Pb3 Br6 151.66(7) 1_565 .
Br5 Pb3 Br6 83.84(4) . .
Br5 Pb3 Br6 75.78(5) 3_556 .
Br5 Pb3 Br6 83.84(4) 1_565 1_565
Br5 Pb3 Br6 151.65(7) . 1_565
Br5 Pb3 Br6 75.78(5) 3_556 1_565
Br6 Pb3 Br6 86.65(5) . 1_565
Br5 Pb3 Br3 74.02(5) 1_565 .
Br5 Pb3 Br3 74.02(5) . .
Br5 Pb3 Br3 136.29(6) 3_556 .
Br6 Pb3 Br3 130.60(4) . .
Br6 Pb3 Br3 130.60(4) 1_565 .
Pb3 Br5 Pb3 92.03(6) 1_545 .
Pb3 Br5 Pb3 103.99(5) 1_545 3_556
Pb3 Br5 Pb3 103.99(5) . 3_556
Pb2 Br3 Pb2 93.65(6) 1_545 .
Pb2 Br3 Pb3 114.68(5) 1_545 .
Pb2 Br3 Pb3 114.68(5) . .
Pb1 Br1 Pb1 94.85(6) . 1_565
Pb3 Br6 Pb3 86.65(5) 1_545 .
Pb1 O1 H1 112.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O1 2.531(16) .
Pb1 Br1 2.9420(13) .
Pb1 Br1 2.9420(13) 1_545
Pb1 Br2 3.238(2) .
Pb2 Br3 2.9709(15) .
Pb2 Br3 2.9709(15) 1_565
Pb2 Br4 3.169(2) .
Pb3 Br5 3.0112(16) 1_565
Pb3 Br5 3.0112(16) .
Pb3 Br5 3.122(2) 3_556
Pb3 Br6 3.1575(15) .
Pb3 Br6 3.1575(15) 1_565
Pb3 Br3 3.221(2) .
Br5 Pb3 3.0112(16) 1_545
Br5 Pb3 3.122(2) 3_556
Br3 Pb2 2.9709(15) 1_545
Br1 Pb1 2.9420(13) 1_565
Br6 Pb3 3.1575(15) 1_545
O1 H1 0.9237 .
O2 H2 0.8415 .
