#------------------------------------------------------------------------------
#$Date: 2022-08-02 01:08:37 +0300 (Tue, 02 Aug 2022) $
#$Revision: 277025 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/74/1567409.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_1567409
loop_
_publ_author_name
'Crace, Ethan'
'Su, Alexander'
'Karunadasa, Hemamala I.'
_publ_section_title
;
 Reliably obtaining white light from layered halide perovskites at room
 temperature
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC02381D
_journal_year                    2022
_chemical_formula_moiety         'Cl4 Pb, C5 H11 N3'
_chemical_formula_sum            'C5 H11 Cl4 N3 Pb'
_chemical_formula_weight         462.16
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-04-27 deposited with the CCDC.	2022-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.608(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7314(4)
_cell_length_b                   11.3143(4)
_cell_length_c                   11.5207(5)
_cell_measurement_reflns_used    6251
_cell_measurement_temperature    300
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.83
_cell_volume                     1215.56(9)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      300.15
_diffrn_detector                 'Bruker Photon II'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4837
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.319
_diffrn_reflns_theta_min         2.578
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.721
_exptl_absorpt_correction_T_max  0.431128
_exptl_absorpt_correction_T_min  0.228460
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 46179 reflections, Rint = 0.0634
 (25055 with I > 3sig(I), Rint = 0.0504)
;
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.525
_exptl_crystal_description       plate
_exptl_crystal_F_000             848
_exptl_crystal_preparation
;
 'Crystals were prepared by dissolving precursors in 6M HCl 
  at 100C and cooling the solution to room temperature 
  at a rate of 2C/hr.'
;
_exptl_crystal_recrystallization_method
"'Large crystals are light brown plates. Smaller crystals   or fragments of larger crystals appear colorless under   the microscope.'"
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.993
_refine_diff_density_min         -1.928
_refine_diff_density_rms         0.276
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         4837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0380
_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)+(0.0601P)²+9.5365P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1267
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4225
_reflns_number_total             4837
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2sc02381d2.cif
_cod_data_source_block           twin4_a_CCDC1
_cod_database_code               1567409
_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.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7776
 0.2224
2.a Secondary CH2 refined with riding coordinates:
 C00A(H00D,H00E), C00C(H00G,H00H)
2.b Aromatic/amide H refined with riding coordinates:
 N007(H007), N008(H008), C00B(H00F), C00D(H00I)
2.c Idealised Me refined as rotating group:
 N006(H00A,H00B,H00C)
;
_olex2_exptl_crystal_mounting_method
;
 'Crystals were seperated from the mother liquor in paratone oil and placed
  on a kapton loop using the paratone to adhere the crystal to the loop.'
;
_olex2_submission_special_instructions 'No special instructions were received'
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb01 Pb 0.51696(4) 0.29073(3) 0.23072(3) 0.02316(13) Uani 1 1 d . . . . .
Cl02 Cl 0.5451(3) 0.0432(2) 0.2334(2) 0.0357(6) Uani 1 1 d . . . . .
Cl03 Cl 0.4877(4) 0.2680(3) 0.4555(2) 0.0360(6) Uani 1 1 d . . . . .
Cl04 Cl 0.2065(4) 0.2463(2) 0.1327(3) 0.0345(6) Uani 1 1 d . . . . .
Cl05 Cl 0.8084(3) 0.3232(3) 0.3466(3) 0.0380(6) Uani 1 1 d . . . . .
N006 N 0.2769(11) 0.4921(10) 0.4752(9) 0.036(2) Uani 1 1 d . . . . .
H00A H 0.334894 0.532365 0.442338 0.044 Uiso 1 1 calc R U . . .
H00B H 0.322638 0.428946 0.513544 0.044 Uiso 1 1 calc R U . . .
H00C H 0.250325 0.538076 0.527737 0.044 Uiso 1 1 calc R U . . .
N007 N -0.1692(11) 0.5686(9) 0.1669(9) 0.035(2) Uani 1 1 d . . . . .
H007 H -0.193206 0.627913 0.203515 0.042 Uiso 1 1 calc R U . . .
N008 N -0.0468(11) 0.4321(9) 0.1177(9) 0.038(2) Uani 1 1 d . . . . .
H008 H 0.023531 0.386697 0.116199 0.045 Uiso 1 1 calc R U . . .
C009 C -0.0409(13) 0.5186(11) 0.1964(11) 0.034(2) Uani 1 1 d . . . . .
C00A C 0.0846(14) 0.5561(11) 0.2977(12) 0.042(3) Uani 1 1 d . . . . .
H00D H 0.054536 0.616689 0.344857 0.050 Uiso 1 1 calc R U . . .
H00E H 0.156863 0.590114 0.264684 0.050 Uiso 1 1 calc R U . . .
C00B C -0.2577(14) 0.5118(12) 0.0694(11) 0.042(3) Uani 1 1 d . . . . .
H00F H -0.353299 0.529603 0.031269 0.051 Uiso 1 1 calc R U . . .
C00C C 0.1489(13) 0.4541(10) 0.3793(11) 0.038(3) Uani 1 1 d . . . . .
H00G H 0.078423 0.422509 0.415871 0.045 Uiso 1 1 calc R U . . .
H00H H 0.175148 0.391836 0.331822 0.045 Uiso 1 1 calc R U . . .
C00D C -0.1809(15) 0.4260(12) 0.0397(11) 0.043(3) Uani 1 1 d . . . . .
H00I H -0.213023 0.371890 -0.022974 0.052 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
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'
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'
Pb Pb -3.3944 10.1111 '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
Cl02 Pb01 Cl02 167.97(2) . 2_655 ?
Cl02 Pb01 Cl03 77.47(8) . 4_565 ?
Cl02 Pb01 Cl03 112.12(7) 2_655 4_565 ?
Cl02 Pb01 Cl04 85.44(8) . . ?
Cl03 Pb01 Cl02 86.05(8) . . ?
Cl03 Pb01 Cl02 82.92(8) . 2_655 ?
Cl03 Pb01 Cl03 159.37(7) . 4_565 ?
Cl03 Pb01 Cl04 88.50(10) . . ?
Cl03 Pb01 Cl05 85.72(10) . . ?
Cl04 Pb01 Cl02 89.45(8) . 2_655 ?
Cl04 Pb01 Cl03 77.99(9) . 4_565 ?
Cl05 Pb01 Cl02 91.49(9) . 2_655 ?
Cl05 Pb01 Cl02 92.49(9) . . ?
Cl05 Pb01 Cl03 107.11(9) . 4_565 ?
Cl05 Pb01 Cl04 173.98(9) . . ?
Pb01 Cl02 Pb01 159.24(12) . 2_645 ?
H00A N006 H00B 109.5 . . ?
H00A N006 H00C 109.5 . . ?
H00B N006 H00C 109.5 . . ?
C00C N006 H00A 109.5 . . ?
C00C N006 H00B 109.5 . . ?
C00C N006 H00C 109.5 . . ?
C009 N007 H007 125.1 . . ?
C009 N007 C00B 109.7(10) . . ?
C00B N007 H007 125.1 . . ?
C009 N008 H008 125.2 . . ?
C009 N008 C00D 109.6(10) . . ?
C00D N008 H008 125.2 . . ?
N007 C009 N008 106.6(10) . . ?
N007 C009 C00A 125.6(12) . . ?
N008 C009 C00A 127.8(12) . . ?
C009 C00A H00D 109.2 . . ?
C009 C00A H00E 109.2 . . ?
C009 C00A C00C 111.9(10) . . ?
H00D C00A H00E 107.9 . . ?
C00C C00A H00D 109.2 . . ?
C00C C00A H00E 109.2 . . ?
N007 C00B H00F 126.7 . . ?
C00D C00B N007 106.7(11) . . ?
C00D C00B H00F 126.7 . . ?
N006 C00C C00A 110.8(10) . . ?
N006 C00C H00G 109.5 . . ?
N006 C00C H00H 109.5 . . ?
C00A C00C H00G 109.5 . . ?
C00A C00C H00H 109.5 . . ?
H00G C00C H00H 108.1 . . ?
N008 C00D H00I 126.3 . . ?
C00B C00D N008 107.3(11) . . ?
C00B C00D H00I 126.3 . . ?
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
Pb01 Cl02 2.814(3) . ?
Pb01 Cl02 2.973(3) 2_655 ?
Pb01 Cl03 3.172(3) 4_565 ?
Pb01 Cl03 2.697(3) . ?
Pb01 Cl04 2.950(3) . ?
Pb01 Cl05 2.792(3) . ?
N006 H00A 0.8900 . ?
N006 H00B 0.8900 . ?
N006 H00C 0.8900 . ?
N006 C00C 1.473(14) . ?
N007 H007 0.8600 . ?
N007 C009 1.324(15) . ?
N007 C00B 1.365(15) . ?
N008 H008 0.8600 . ?
N008 C009 1.324(15) . ?
N008 C00D 1.359(16) . ?
C009 C00A 1.489(17) . ?
C00A H00D 0.9700 . ?
C00A H00E 0.9700 . ?
C00A C00C 1.507(16) . ?
C00B H00F 0.9300 . ?
C00B C00D 1.328(19) . ?
C00C H00G 0.9700 . ?
C00C H00H 0.9700 . ?
C00D H00I 0.9300 . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N007 C009 C00A C00C 127.9(14) . . . . ?
N007 C00B C00D N008 -0.7(15) . . . . ?
N008 C009 C00A C00C -53.3(18) . . . . ?
C009 N007 C00B C00D -0.1(16) . . . . ?
C009 N008 C00D C00B 1.3(15) . . . . ?
C009 C00A C00C N006 177.2(11) . . . . ?
C00B N007 C009 N008 0.9(14) . . . . ?
C00B N007 C009 C00A 179.8(12) . . . . ?
C00D N008 C009 N007 -1.3(14) . . . . ?
C00D N008 C009 C00A 179.8(12) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.7776
2 0.2224
