#------------------------------------------------------------------------------
#$Date: 2021-06-30 01:38:57 +0300 (Wed, 30 Jun 2021) $
#$Revision: 266790 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/39/4003969.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_4003969
loop_
_publ_author_name
'Denis, Paul-Henry'
'Mertens, Martijn'
'Van Gompel, Wouter T. M.'
'Van Hecke, Kristof'
'Ruttens, Bart'
'D’Haen, Jan'
'Lutsen, Laurence'
'Vanderzande, Dirk'
_publ_section_title
;
 Directing the Self-Assembly of Conjugated Organic Ammonium Cations in
 Low-Dimensional Perovskites by Halide Substitution
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.1c01221
_journal_year                    2021
_chemical_formula_moiety         'Cl4 Pb, 2(C11 H14 N S2)'
_chemical_formula_sum            'C22 H28 Cl4 N2 Pb S4'
_chemical_formula_weight         797.70
_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     direct
_audit_creation_date             2020-07-28
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.5692(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   24.7740(5)
_cell_length_b                   7.35765(14)
_cell_length_c                   7.86657(15)
_cell_measurement_reflns_used    10166
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.7770
_cell_measurement_theta_min      3.5410
_cell_volume                     1433.37(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -66.00  33.00   1.00    5.00    --  -41.68  38.00 -90.00   99
  2  ω   -122.00  -1.00   1.00    5.00    --  -41.68 -19.00  90.00  121
  3  ω    -21.00  74.00   1.00    5.00    --   41.68 -77.00  90.00   95
  4  ω     17.00 116.00   1.00    5.00    --   41.68  38.00 -60.00   99
  5  ω     23.00 107.00   1.00   25.00    --  106.01 -94.00 150.00   84
  6  ω     30.00 134.00   1.00   25.00    --  106.01 -30.00 150.00  104
  7  ω     33.00 112.00   1.00   25.00    --  106.01-125.00 -30.00   79
  8  ω     30.00 139.00   1.00   25.00    --  106.01 -77.00-150.00  109
  9  ω    103.00 178.00   1.00   25.00    --  106.01  77.00-120.00   75
 10  ω     78.00 178.00   1.00   25.00    --  106.01  30.00 -90.00  100
 11  ω     23.00 107.00   1.00   25.00    --  106.01 -94.00  90.00   84
 12  ω     33.00 112.00   1.00   25.00    --  106.01-125.00  60.00   79
 13  ω     23.00 107.00   1.00   25.00    --  106.01 -94.00-180.00   84
 14  ω     78.00 178.00   1.00   25.00    --  106.01  30.00 -30.00  100
 15  ω    102.00 178.00   1.00   25.00    --  106.01  87.00-169.00   76
 16  ω     14.00 115.00   1.00    5.00    --   41.68  57.00 -30.00  101
 17  ω     14.00 115.00   1.00    5.00    --   41.68  57.00 120.00  101
 18  ω     14.00 115.00   1.00    5.00    --   41.68  57.00  30.00  101
 19  ω     27.00  98.00   1.00    5.00    --   41.68-125.00  30.00   71
 20  ω     14.00 115.00   1.00    5.00    --   41.68  57.00-150.00  101
 21  ω     80.00 178.00   1.00   25.00    --  106.01  45.00  60.00   98
 22  ω     77.00 178.00   1.00   25.00    --  106.01  61.00 -90.00  101
 23  ω     78.00 178.00   1.00   25.00    --  106.01  30.00 150.00  100
 24  ω     77.00 178.00   1.00   25.00    --  106.01  61.00-150.00  101
 25  ω     76.00 178.00   1.00   25.00    --  106.01  66.00  84.00  102
 26  ω     77.00 178.00   1.00   25.00    --  106.01  61.00   0.00  101
 27  ω     77.00 178.00   1.00   25.00    --  106.01  61.00 -30.00  101
 28  ω     77.00 178.00   1.00   25.00    --  106.01  61.00 150.00  101
 29  ω     77.00 178.00   1.00   25.00    --  106.01  61.00  60.00  101
 30  ω     77.00 178.00   1.00   25.00    --  106.01  61.00-180.00  101
 31  ω     14.00 115.00   1.00    5.00    --   41.68  57.00-120.00  101
;
_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      0.0460969000
_diffrn_orient_matrix_UB_12      -0.1229249000
_diffrn_orient_matrix_UB_13      0.0676212000
_diffrn_orient_matrix_UB_21      0.0137136000
_diffrn_orient_matrix_UB_22      0.1401198000
_diffrn_orient_matrix_UB_23      0.1400003000
_diffrn_orient_matrix_UB_31      -0.0394695000
_diffrn_orient_matrix_UB_32      -0.0954504000
_diffrn_orient_matrix_UB_33      0.1191057000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            25920
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.861
_diffrn_reflns_theta_min         3.570
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.718
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_description       plate
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2878
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0265
_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)+(0.0331P)²+2.4221P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0681
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2396
_reflns_number_total             2878
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm1c01221_si_003.cif
_cod_data_source_block           dvdz019b
_cod_database_code               4003969
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C22 H28 Cl4 N2 Pb S4'
_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.
;
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_olex2_exptl_crystal_mounting_method 'mounted on a LithoLoop'
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 2.837
_oxdiff_exptl_absorpt_empirical_full_min 0.409
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
Pb1 Pb 0.000000 0.500000 0.500000 0.02170(8) Uani 1 2 d S T P . .
Cl1 Cl 0.02404(6) 0.31987(17) 0.81348(14) 0.0422(3) Uani 1 1 d . . . . .
Cl2 Cl 0.11207(4) 0.57363(18) 0.47341(13) 0.0349(2) Uani 1 1 d . . . . .
S1 S -0.37991(6) 0.3864(2) 1.8164(2) 0.0537(4) Uani 1 1 d . . . . .
S2 S -0.33780(5) 0.60371(17) 1.32129(14) 0.0346(2) Uani 1 1 d . . . . .
N1 N -0.10898(17) 0.4947(6) 0.9251(5) 0.0362(9) Uani 1 1 d . . . . .
H1A H -0.097320 0.507253 0.816989 0.043 Uiso 1 1 calc GR . . . .
H1B H -0.108962 0.374988 0.953961 0.043 Uiso 1 1 calc GR . . . .
H1C H -0.086574 0.556921 0.997866 0.043 Uiso 1 1 calc GR . . . .
C1 C -0.4445(3) 0.4433(10) 1.8610(8) 0.0543(15) Uani 1 1 d . . . . .
H1 H -0.462018 0.408635 1.961913 0.065 Uiso 1 1 calc R . . . .
C2 C -0.4679(2) 0.5433(10) 1.7359(8) 0.0550(16) Uani 1 1 d . . . . .
H2 H -0.504007 0.585656 1.742033 0.066 Uiso 1 1 calc R . . . .
C3 C -0.43493(19) 0.5823(7) 1.5925(6) 0.0336(10) Uani 1 1 d . . . . .
H3 H -0.445359 0.651104 1.494876 0.040 Uiso 1 1 calc R . . . .
C4 C -0.3829(2) 0.4969(7) 1.6247(6) 0.0336(10) Uani 1 1 d . . . . .
C5 C -0.33628(19) 0.4976(6) 1.5183(6) 0.0304(9) Uani 1 1 d . . . . .
C6 C -0.2873(2) 0.4145(7) 1.5458(6) 0.0344(10) Uani 1 1 d . . . . .
H6 H -0.278276 0.348211 1.646226 0.041 Uiso 1 1 calc R . . . .
C7 C -0.2517(2) 0.4370(7) 1.4102(6) 0.0327(10) Uani 1 1 d . . . . .
H7 H -0.216241 0.387402 1.411004 0.039 Uiso 1 1 calc R . . . .
C8 C -0.27268(19) 0.5360(6) 1.2788(6) 0.0321(10) Uani 1 1 d . . . . .
C9 C -0.2469(2) 0.5867(7) 1.1152(6) 0.0358(10) Uani 1 1 d . . . . .
H9A H -0.246638 0.720785 1.104488 0.043 Uiso 1 1 calc R . . . .
H9B H -0.268980 0.537417 1.019073 0.043 Uiso 1 1 calc R . . . .
C10 C -0.18946(19) 0.5167(6) 1.1023(6) 0.0307(9) Uani 1 1 d . . . . .
H10A H -0.167057 0.567080 1.197259 0.037 Uiso 1 1 calc R . . . .
H10B H -0.189460 0.382676 1.113450 0.037 Uiso 1 1 calc R . . . .
C11 C -0.1649(2) 0.5687(7) 0.9355(6) 0.0368(10) Uani 1 1 d . . . . .
H11A H -0.187511 0.520315 0.840125 0.044 Uiso 1 1 calc R . . . .
H11B H -0.163938 0.702731 0.925185 0.044 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 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-8 3 3 0.0010
8 -3 -3 0.0359
1 5 0 0.0777
-6 -4 2 0.0425
-13 2 -2 0.0260
13 -2 2 0.0010
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
Cl1 Pb1 Cl1 180.0 4_565 2_556 ?
Cl1 Pb1 Cl1 88.862(16) 2_556 . ?
Cl1 Pb1 Cl1 180.0 3_566 . ?
Cl1 Pb1 Cl1 91.138(16) 4_565 . ?
Cl1 Pb1 Cl1 91.138(16) 2_556 3_566 ?
Cl1 Pb1 Cl1 88.862(16) 4_565 3_566 ?
Cl2 Pb1 Cl1 84.32(4) 3_566 2_556 ?
Cl2 Pb1 Cl1 88.33(4) 3_566 3_566 ?
Cl2 Pb1 Cl1 88.33(4) . . ?
Cl2 Pb1 Cl1 84.32(4) . 4_565 ?
Cl2 Pb1 Cl1 91.67(4) . 3_566 ?
Cl2 Pb1 Cl1 95.68(4) 3_566 4_565 ?
Cl2 Pb1 Cl1 91.67(4) 3_566 . ?
Cl2 Pb1 Cl1 95.68(4) . 2_556 ?
Cl2 Pb1 Cl2 180.0 . 3_566 ?
Pb1 Cl1 Pb1 142.16(4) 2_546 . ?
C1 S1 C4 92.7(3) . . ?
C8 S2 C5 92.6(2) . . ?
C2 C1 S1 111.9(5) . . ?
C1 C2 C3 116.1(5) . . ?
C2 C3 C4 107.3(5) . . ?
C3 C4 S1 112.0(4) . . ?
C5 C4 S1 119.8(4) . . ?
C5 C4 C3 128.2(4) . . ?
C4 C5 S2 121.4(4) . . ?
C6 C5 S2 109.8(4) . . ?
C6 C5 C4 128.7(4) . . ?
C5 C6 C7 113.4(4) . . ?
C8 C7 C6 113.7(4) . . ?
C7 C8 S2 110.4(4) . . ?
C7 C8 C9 128.6(5) . . ?
C9 C8 S2 121.0(4) . . ?
C8 C9 C10 113.2(4) . . ?
C11 C10 C9 111.8(4) . . ?
N1 C11 C10 110.6(4) . . ?
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 2.8451(11) 4_565 ?
Pb1 Cl1 2.8451(11) 2_556 ?
Pb1 Cl1 2.8481(10) 3_566 ?
Pb1 Cl1 2.8481(10) . ?
Pb1 Cl2 2.8420(11) . ?
Pb1 Cl2 2.8420(11) 3_566 ?
S1 C1 1.700(7) . ?
S1 C4 1.713(5) . ?
S2 C5 1.735(5) . ?
S2 C8 1.730(5) . ?
N1 C11 1.493(7) . ?
C1 C2 1.346(10) . ?
C2 C3 1.439(8) . ?
C3 C4 1.451(7) . ?
C4 C5 1.444(7) . ?
C5 C6 1.370(7) . ?
C6 C7 1.414(7) . ?
C7 C8 1.357(7) . ?
C8 C9 1.500(7) . ?
C9 C10 1.519(7) . ?
C10 C11 1.511(6) . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-8.0391 2.9305 3.1999 -0.5144 0.7484 0.4187
8.0391 -2.9305 -3.1999 0.5144 -0.7484 -0.4187
1.1720 4.7493 0.3671 -0.5050 0.7329 -0.4559
-6.2346 -3.9057 2.2117 0.3423 -0.3231 0.8823
-13.2432 1.5421 -2.2669 -0.9533 -0.2829 0.1055
13.2432 -1.5421 2.2669 0.9533 0.2829 -0.1055
