#------------------------------------------------------------------------------
#$Date: 2021-02-05 01:26:50 +0200 (Fri, 05 Feb 2021) $
#$Revision: 261734 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/02/7060209.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_7060209
loop_
_publ_author_name
'Zhu, Liang'
'Jin, Wenqi'
'Yang, Zhihua'
'Yang, Yun'
'Pan, Shilie'
_publ_section_title
;
 The synthesis, characterization, and theoretical analysis of (NH4)3PbCl5
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2038
_journal_page_last               2043
_journal_paper_doi               10.1039/D0NJ05771A
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'Cl3 Pb, 3(H4 N), 2(Cl)'
_chemical_formula_sum            'Cl5 H12 N3 Pb'
_chemical_formula_weight         438.57
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-11-18 deposited with the CCDC.	2020-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.435(7)
_cell_length_b                   15.806(13)
_cell_length_c                   8.468(7)
_cell_measurement_reflns_used    2082
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.083
_cell_measurement_theta_min      2.578
_cell_volume                     1129.0(16)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6559
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.577
_diffrn_reflns_theta_min         2.577
_exptl_absorpt_coefficient_mu    16.070
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5048
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_refine_diff_density_max         0.852
_refine_diff_density_min         -1.040
_refine_diff_density_rms         0.216
_refine_ls_extinction_coef       0.0052(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   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         1351
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0262
_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)+(0.0362P)²] 
 where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0712
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1177
_reflns_number_total             1351
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0nj05771a2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7060209.cif.'
_cod_original_formula_sum        'H12 Cl5 N3 Pb'
_cod_database_code               7060209
_shelxl_version_number           2013-2
_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. 
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups, All N(H,H,H,H) groups
2.a Riding coordinates:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C,H2D)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, 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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.58048(3) 0.7500 0.65317(3) 0.02632(14) Uani 1 2 d S T P . .
N1 N 0.4224(7) 0.7500 0.1479(6) 0.0169(12) Uani 1 2 d S T P . .
H1A H 0.4395 0.7500 0.0448 0.020 Uiso 1 2 d RS T P . .
H1B H 0.3208 0.7500 0.1667 0.020 Uiso 1 2 d RS T P . .
H1C H 0.4642 0.7959 0.1903 0.020 Uiso 1 1 d R . . . .
N2 N 0.2564(6) 0.5467(3) 0.4645(6) 0.0395(12) Uani 1 1 d . . . . .
H2A H 0.2553 0.5361 0.3613 0.047 Uiso 1 1 d R . . . .
H2B H 0.3401 0.5216 0.5083 0.047 Uiso 1 1 d R . . . .
H2C H 0.1680 0.5267 0.5083 0.047 Uiso 1 1 d R . . . .
H2D H 0.2626 0.6022 0.4801 0.047 Uiso 1 1 d R . . . .
Cl1 Cl 0.2789(2) 0.7500 0.5217(2) 0.0269(4) Uani 1 2 d S T P . .
Cl2 Cl 0.61389(18) 0.87824(9) 0.37199(16) 0.0312(3) Uani 1 1 d . . . . .
Cl3 Cl 0.4431(2) 0.87939(11) 0.82441(17) 0.0405(4) 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
H H 0.0000 0.0000 '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'
Cl Cl 0.1484 0.1585 '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'
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
Cl3 Pb1 Cl1 79.99(6) 7_575 . ?
Cl3 Pb1 Cl1 79.99(6) . . ?
Cl3 Pb1 Cl3 95.54(10) 7_575 . ?
H1A N1 H1B 110.0 . . ?
H1A N1 H1C 109.6 . . ?
H1B N1 H1C 108.6 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2A N2 H2D 109.4 . . ?
H2B N2 H2C 109.5 . . ?
H2B N2 H2D 109.3 . . ?
H2C N2 H2D 109.7 . . ?
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 Cl1 2.777(3) . ?
Pb1 Cl3 2.762(2) 7_575 ?
Pb1 Cl3 2.762(2) . ?
N1 H1A 0.8853 . ?
N1 H1B 0.8716 . ?
N1 H1C 0.8826 . ?
N2 H2A 0.8901 . ?
N2 H2B 0.8902 . ?
N2 H2C 0.8899 . ?
N2 H2D 0.8884 . ?
