#------------------------------------------------------------------------------
#$Date: 2025-01-06 13:12:01 +0200 (Mon, 06 Jan 2025) $
#$Revision: 297095 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/29/1572980.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_1572980
loop_
_publ_author_name
'Zhang, Zixuan'
'Wu, Jin'
'Lu, Haipeng'
_publ_section_title
;
 Deciphering the electronic and structural origin of chiroptical activity
 of chiral 2D perovskites.
;
_journal_issue                   48
_journal_name_full               'Chemical science'
_journal_page_first              20440
_journal_page_last               20447
_journal_paper_doi               10.1039/d4sc04915b
_journal_volume                  15
_journal_year                    2024
_chemical_absolute_configuration R
_chemical_formula_moiety         'Br4 Pb, 2(C8 H11 Cl N)'
_chemical_formula_sum            'C16 H22 Br4 Cl2 N2 Pb'
_chemical_formula_weight         840.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-04-16 deposited with the CCDC.	2024-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.984(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7598(2)
_cell_length_b                   7.7798(2)
_cell_length_c                   17.5050(4)
_cell_measurement_reflns_used    5213
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.6200
_cell_measurement_theta_min      2.3390
_cell_volume                     1181.39(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.90 (release 15-09-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -40.00  49.00   1.00    2.50    --   15.85 -77.00-120.00   89
  2  ω    -40.00  50.00   1.00    2.50    --   15.85 -77.00 120.00   90
  3  ω    -41.00  50.00   1.00    2.50    --   15.85 -77.00   0.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0112390000
_diffrn_orient_matrix_UB_12      -0.0078378000
_diffrn_orient_matrix_UB_13      0.0392060000
_diffrn_orient_matrix_UB_21      0.0255938000
_diffrn_orient_matrix_UB_22      0.0858594000
_diffrn_orient_matrix_UB_23      0.0068711000
_diffrn_orient_matrix_UB_31      -0.0768147000
_diffrn_orient_matrix_UB_32      0.0297264000
_diffrn_orient_matrix_UB_33      -0.0094563000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7306
_diffrn_reflns_point_group_measured_fraction_full 0.934
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.731
_diffrn_reflns_theta_min         2.348
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.135
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.362
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.942
_refine_diff_density_min         -1.389
_refine_diff_density_rms         0.182
_refine_ls_abs_structure_details
;
 Flack x determined using 1708 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.040(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         4643
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0307
_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)+(0.0325P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0691
_reflns_Friedel_coverage         0.724
_reflns_Friedel_fraction_full    0.858
_reflns_Friedel_fraction_max     0.842
_reflns_number_gt                4383
_reflns_number_total             4643
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4sc04915b2.cif
_cod_data_source_block           3-cl-mba-pbbr
_cod_depositor_comments
'Adding full bibliography for 1572979--1572983.cif.'
_cod_database_code               1572980
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Pb I Cl C N'
_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_max   0.438
_shelx_estimated_absorpt_t_min   0.305
_diffrn_oxdiff_digest_frames
;
01a077a30a747393495c3aa531c2a1f46e00284d2b5
;
_diffrn_oxdiff_digest_hkl
;
01ba0dc6263eeef0982004e0b2d5abaac0ed6e
;
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C00B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Ternary CH refined with riding coordinates:
 C00G(H00S), C00H(H00H)
3.b Aromatic/amide H refined with riding coordinates:
 C00C(H00Q), C00D(H00R), C00F(H00F), C00J(H00T), C00L(H00U), C00O(H00O),
 C00P(H00P), C1(H1)
3.c Idealised Me refined as rotating group:
 N008(H00A,H00B,H00C), N009(H00I,H00J,H00K), C00B(H00L,H00M,H00N), C00K(H00D,
 H00E,H00G)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.727
_oxdiff_exptl_absorpt_empirical_full_min 0.734
loop_
_space_group_symop_operation_xyz
'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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb01 Pb 0.74903(3) 0.52345(6) 0.50036(2) 0.00767(9) Uani 1 1 d . . . . .
Br02 Br 0.92573(10) 0.18840(13) 0.51951(5) 0.0117(2) Uani 1 1 d . . . . .
Br03 Br 0.46052(10) 0.33366(13) 0.50918(5) 0.0132(2) Uani 1 1 d . . . . .
Br04 Br 0.83375(11) 0.58574(12) 0.66815(6) 0.0119(2) Uani 1 1 d . . . . .
Br05 Br 0.67210(10) 0.54976(12) 0.32906(5) 0.0102(2) Uani 1 1 d . . . . .
Cl06 Cl 0.3634(4) 0.1292(4) 0.08550(16) 0.0314(7) Uani 1 1 d . . . . .
Cl07 Cl 0.8654(3) 0.3734(4) 0.04957(16) 0.0300(7) Uani 1 1 d . . . . .
N008 N 0.2935(8) 0.5135(11) 0.3434(4) 0.0137(17) Uani 1 1 d . . . . .
H00A H 0.270520 0.399686 0.338146 0.016 Uiso 1 1 calc GR . . . .
H00B H 0.254924 0.555914 0.385290 0.016 Uiso 1 1 calc GR . . . .
H00C H 0.397586 0.527616 0.349928 0.016 Uiso 1 1 calc GR . . . .
N009 N 0.8115(8) -0.0430(10) 0.3542(5) 0.0112(17) Uani 1 1 d . . . . .
H00I H 0.774774 -0.149252 0.339783 0.013 Uiso 1 1 calc GR . . . .
H00J H 0.793637 -0.020709 0.403186 0.013 Uiso 1 1 calc GR . . . .
H00K H 0.914715 -0.039244 0.352117 0.013 Uiso 1 1 calc GR . . . .
C00A C 0.7695(10) 0.0640(11) 0.2194(5) 0.010(2) Uani 1 1 d . . . . .
C00B C 0.5600(11) 0.0836(12) 0.3060(6) 0.015(2) Uani 1 1 d . U . . .
H00L H 0.518519 -0.028729 0.288308 0.023 Uiso 1 1 calc GR . . . .
H00M H 0.507051 0.174178 0.273604 0.023 Uiso 1 1 calc GR . . . .
H00N H 0.543883 0.101489 0.359717 0.023 Uiso 1 1 calc GR . . . .
C00C C 0.7958(10) 0.2064(14) 0.1762(6) 0.015(2) Uani 1 1 d . . . . .
H00Q H 0.789271 0.317819 0.197696 0.017 Uiso 1 1 calc R . . . .
C00D C 0.7729(11) -0.0965(13) 0.1849(6) 0.014(2) Uani 1 1 d . . . . .
H00R H 0.749158 -0.196060 0.212384 0.017 Uiso 1 1 calc R . . . .
C00E C 0.2999(10) 0.5547(12) 0.2043(5) 0.010(2) Uani 1 1 d . . . . .
C00F C 0.2943(11) 0.3851(13) 0.1784(6) 0.015(2) Uani 1 1 d . . . . .
H00F H 0.237962 0.300728 0.201999 0.018 Uiso 1 1 calc R . . . .
C00G C 0.7314(11) 0.0896(13) 0.3004(5) 0.012(2) Uani 1 1 d . . . . .
H00S H 0.770740 0.205205 0.318657 0.015 Uiso 1 1 calc R . . . .
C00H C 0.2222(11) 0.6094(14) 0.2715(6) 0.016(2) Uani 1 1 d . . . . .
H00H H 0.238216 0.735561 0.280000 0.019 Uiso 1 1 calc R . . . .
C00I C 0.8313(11) 0.1896(14) 0.1024(6) 0.016(2) Uani 1 1 d . . . . .
C00J C 0.8411(11) 0.0292(16) 0.0689(6) 0.021(2) Uani 1 1 d . . . . .
H00T H 0.868316 0.018080 0.018480 0.025 Uiso 1 1 calc R . . . .
C00K C 0.0504(11) 0.5716(13) 0.2603(6) 0.024(3) Uani 1 1 d . . . . .
H00D H 0.033236 0.450144 0.246962 0.036 Uiso 1 1 calc GR . . . .
H00E H -0.001410 0.643561 0.218596 0.036 Uiso 1 1 calc GR . . . .
H00G H 0.008453 0.596770 0.308172 0.036 Uiso 1 1 calc GR . . . .
C00L C 0.8104(11) -0.1137(15) 0.1107(6) 0.021(2) Uani 1 1 d . . . . .
H00U H 0.814896 -0.224807 0.088615 0.025 Uiso 1 1 calc R . . . .
C00M C 0.3721(11) 0.3422(14) 0.1178(5) 0.016(2) Uani 1 1 d . . . . .
C00O C 0.4497(11) 0.4615(15) 0.0799(6) 0.023(3) Uani 1 1 d . . . . .
H00O H 0.500950 0.428244 0.037794 0.027 Uiso 1 1 calc R . . . .
C00P C 0.3776(11) 0.6770(14) 0.1661(5) 0.018(2) Uani 1 1 d . . . . .
H00P H 0.379719 0.793255 0.182818 0.022 Uiso 1 1 calc R . . . .
C1 C 0.4517(12) 0.6321(15) 0.1042(6) 0.024(3) Uani 1 1 d . . . . .
H1 H 0.503643 0.716983 0.078471 0.029 Uiso 1 1 calc R . . . .
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'
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
Br02 Pb01 Br02 84.704(14) . 2_756 ?
Br03 Pb01 Br02 102.57(3) 2_656 2_756 ?
Br03 Pb01 Br02 89.53(3) . . ?
Br03 Pb01 Br02 172.37(3) 2_656 . ?
Br03 Pb01 Br02 173.03(3) . 2_756 ?
Br03 Pb01 Br03 83.362(11) . 2_656 ?
Br03 Pb01 Br04 97.37(3) . . ?
Br03 Pb01 Br05 90.65(3) . . ?
Br04 Pb01 Br02 88.70(3) . . ?
Br04 Pb01 Br02 86.44(3) . 2_756 ?
Br04 Pb01 Br03 89.47(3) . 2_656 ?
Br04 Pb01 Br05 166.58(3) . . ?
Br05 Pb01 Br02 102.17(3) . . ?
Br05 Pb01 Br02 86.75(3) . 2_756 ?
Br05 Pb01 Br03 80.75(3) . 2_656 ?
Pb01 Br02 Pb01 141.80(4) . 2_746 ?
Pb01 Br03 Pb01 156.20(4) . 2_646 ?
C00C C00A C00D 117.9(9) . . ?
C00C C00A C00G 118.9(8) . . ?
C00D C00A C00G 123.1(8) . . ?
C00I C00C C00A 121.0(10) . . ?
C00L C00D C00A 121.0(9) . . ?
C00F C00E C00H 121.6(9) . . ?
C00P C00E C00F 119.2(9) . . ?
C00P C00E C00H 119.2(9) . . ?
C00M C00F C00E 118.7(9) . . ?
N009 C00G C00A 110.6(8) . . ?
N009 C00G C00B 108.6(8) . . ?
C00A C00G C00B 113.9(8) . . ?
C00E C00H N008 109.4(8) . . ?
C00E C00H C00K 113.2(8) . . ?
C00K C00H N008 107.3(8) . . ?
C00C C00I Cl07 119.7(9) . . ?
C00C C00I C00J 121.2(10) . . ?
C00J C00I Cl07 119.1(8) . . ?
C00L C00J C00I 118.3(9) . . ?
C00J C00L C00D 120.5(10) . . ?
C00F C00M Cl06 118.3(8) . . ?
C00O C00M Cl06 119.1(8) . . ?
C00O C00M C00F 122.6(10) . . ?
C00M C00O C1 118.8(10) . . ?
C1 C00P C00E 121.1(10) . . ?
C00P C1 C00O 119.5(10) . . ?
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 Br02 3.0263(11) . ?
Pb01 Br02 3.1875(10) 2_756 ?
Pb01 Br03 2.9495(10) . ?
Pb01 Br03 3.0227(11) 2_656 ?
Pb01 Br04 2.9676(10) . ?
Pb01 Br05 2.9878(10) . ?
Cl06 C00M 1.749(11) . ?
Cl07 C00I 1.751(11) . ?
N008 C00H 1.521(12) . ?
N009 C00G 1.503(12) . ?
C00A C00C 1.379(13) . ?
C00A C00D 1.390(13) . ?
C00A C00G 1.514(13) . ?
C00B C00G 1.519(13) . ?
C00C C00I 1.376(14) . ?
C00D C00L 1.389(14) . ?
C00E C00F 1.394(14) . ?
C00E C00H 1.501(13) . ?
C00E C00P 1.394(13) . ?
C00F C00M 1.379(13) . ?
C00H C00K 1.519(13) . ?
C00I C00J 1.387(15) . ?
C00J C00L 1.377(15) . ?
C00M C00O 1.375(14) . ?
C00O C1 1.394(15) . ?
C00P C1 1.382(15) . ?
