#------------------------------------------------------------------------------
#$Date: 2021-05-29 00:24:37 +0300 (Sat, 29 May 2021) $
#$Revision: 265588 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/87/4518744.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_4518744
loop_
_publ_author_name
'Wu, Siqin'
'Zhou, Bo'
'Yan, Dongpeng'
_publ_section_title
;
 Low-Dimensional Organic Metal Halide Hybrids with Excitation-Dependent
 Optical Waveguides from Visible to Near-Infrared Emission.
;
_journal_name_full               'ACS applied materials & interfaces'
_journal_paper_doi               10.1021/acsami.1c03926
_journal_year                    2021
_chemical_formula_sum            'C20 H18 Cl8 N2 O0 Pb3'
_chemical_formula_weight         1191.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                98.133(3)
_cell_angle_beta                 95.017(3)
_cell_angle_gamma                96.152(3)
_cell_formula_units_Z            1
_cell_length_a                   4.28160(10)
_cell_length_b                   12.0065(4)
_cell_length_c                   14.4461(5)
_cell_measurement_reflns_used    7408
_cell_measurement_temperature    100(10)
_cell_measurement_theta_max      75.7700
_cell_measurement_theta_min      3.7200
_cell_volume                     726.95(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(10)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8443
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.738
_diffrn_reflns_theta_min         3.746
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    40.096
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.722
_exptl_crystal_description       plate
_exptl_crystal_F_000             534
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.358
_refine_diff_density_min         -2.809
_refine_diff_density_rms         0.269
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0351
_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)+(0.0742P)²+0.2473P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.0986
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2748
_reflns_number_total             2898
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            am1c03926_si_004.cif
_cod_data_source_block           1
_cod_original_cell_volume        726.94(4)
_cod_database_code               4518744
_shelx_shelxl_version_number     2016/6
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
Pb1 Pb 0.500000 1.000000 1.000000 0.03910(13) Uani 1 2 d S . P . .
Pb2 Pb 0.86042(5) 0.86272(2) 0.73303(2) 0.03597(12) Uani 1 1 d . . . . .
C1 C 0.9178(16) 0.5837(5) 0.9511(5) 0.0473(15) Uani 1 1 d . . . . .
H1A H 0.863626 0.641012 0.917989 0.057 Uiso 1 1 calc R U . . .
C2 C 0.7764(16) 0.4738(6) 0.9202(5) 0.0433(13) Uani 1 1 d . . . . .
C3 C 0.8661(17) 0.3894(5) 0.9714(5) 0.0507(16) Uani 1 1 d . . . . .
H3 H 0.777780 0.314563 0.952439 0.061 Uiso 1 1 calc R U . . .
C4 C 0.5529(17) 0.4537(6) 0.8358(6) 0.0515(17) Uani 1 1 d . . . . .
H4 H 0.509090 0.516140 0.807634 0.062 Uiso 1 1 calc R U . . .
C5 C 0.4076(18) 0.3531(5) 0.7961(5) 0.0498(16) Uani 1 1 d . . . . .
H5 H 0.446100 0.291075 0.825426 0.060 Uiso 1 1 calc R U . . .
C6 C 0.1939(16) 0.3325(6) 0.7107(5) 0.0458(14) Uani 1 1 d . . . . .
C7 C 0.0825(17) 0.4174(5) 0.6605(5) 0.0495(15) Uani 1 1 d . . . . .
H7 H 0.145975 0.493723 0.682765 0.059 Uiso 1 1 calc R U . . .
C8 C -0.1131(18) 0.3868(6) 0.5814(6) 0.0559(17) Uani 1 1 d . . . . .
H8 H -0.184011 0.442655 0.549216 0.067 Uiso 1 1 calc R U . . .
C9 C -0.109(2) 0.1963(6) 0.5925(6) 0.064(2) Uani 1 1 d . . . . .
H9 H -0.175684 0.120659 0.568129 0.077 Uiso 1 1 calc R U . . .
C10 C 0.083(2) 0.2218(6) 0.6712(6) 0.0607(19) Uani 1 1 d . . . . .
H10 H 0.145414 0.163118 0.701373 0.073 Uiso 1 1 calc R U . . .
Cl1 Cl -0.0079(6) 1.08190(16) 0.89170(15) 0.0549(4) Uani 1 1 d . . . . .
Cl2 Cl 0.4029(5) 0.79959(15) 0.85719(14) 0.0528(4) Uani 1 1 d . . . . .
Cl3 Cl 0.3800(4) 0.94738(13) 0.62988(13) 0.0486(4) Uani 1 1 d . . . . .
Cl4 Cl 0.6959(4) 0.66626(13) 0.62128(14) 0.0560(4) Uani 1 1 d . . . . .
N1 N -0.2094(19) 0.2775(7) 0.5475(5) 0.0597(19) Uani 1 1 d . . . . .
H1 H -0.335809 0.259845 0.496651 0.072 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 0.0181 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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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'
Pb Pb -4.0753 8.5060 '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
Cl1 Pb1 Cl1 180.0 2_577 1_655 ?
Cl1 Pb1 Cl1 85.01(6) 2_577 . ?
Cl1 Pb1 Cl1 94.99(6) 1_655 . ?
Cl1 Pb1 Cl1 94.99(6) 2_577 2_677 ?
Cl1 Pb1 Cl1 85.01(6) 1_655 2_677 ?
Cl1 Pb1 Cl1 180.0 . 2_677 ?
Cl1 Pb1 Cl2 94.42(5) 2_577 . ?
Cl1 Pb1 Cl2 85.58(5) 1_655 . ?
Cl1 Pb1 Cl2 86.24(6) . . ?
Cl1 Pb1 Cl2 93.76(6) 2_677 . ?
Cl1 Pb1 Cl2 85.58(5) 2_577 2_677 ?
Cl1 Pb1 Cl2 94.42(5) 1_655 2_677 ?
Cl1 Pb1 Cl2 93.76(6) . 2_677 ?
Cl1 Pb1 Cl2 86.24(6) 2_677 2_677 ?
Cl2 Pb1 Cl2 180.00(7) . 2_677 ?
Cl4 Pb2 Cl3 87.17(6) . . ?
Cl4 Pb2 Cl2 90.16(6) . . ?
Cl3 Pb2 Cl2 88.00(5) . . ?
Cl4 Pb2 Cl3 97.06(6) . 1_655 ?
Cl3 Pb2 Cl3 96.19(5) . 1_655 ?
Cl2 Pb2 Cl3 171.81(6) . 1_655 ?
Cl4 Pb2 Cl2 99.65(6) . 1_655 ?
Cl3 Pb2 Cl2 173.15(5) . 1_655 ?
Cl2 Pb2 Cl2 92.63(5) . 1_655 ?
Cl3 Pb2 Cl2 82.39(5) 1_655 1_655 ?
C3 C1 C2 122.2(6) 2_767 . ?
C1 C2 C3 117.3(7) . . ?
C1 C2 C4 117.9(6) . . ?
C3 C2 C4 124.8(6) . . ?
C1 C3 C2 120.5(6) 2_767 . ?
C5 C4 C2 124.8(6) . . ?
C4 C5 C6 124.9(6) . . ?
C10 C6 C7 115.0(7) . . ?
C10 C6 C5 119.2(6) . . ?
C7 C6 C5 125.8(6) . . ?
C8 C7 C6 119.9(6) . . ?
C7 C8 N1 121.5(7) . . ?
C10 C9 N1 120.8(7) . . ?
C9 C10 C6 122.6(7) . . ?
Pb1 Cl1 Pb1 94.99(6) 1_455 . ?
Pb2 Cl2 Pb1 100.31(6) . . ?
Pb2 Cl2 Pb2 92.63(5) . 1_455 ?
Pb1 Cl2 Pb2 99.15(5) . 1_455 ?
Pb2 Cl3 Pb2 96.19(5) . 1_455 ?
C9 N1 C8 120.1(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 2.902(2) 2_577 ?
Pb1 Cl1 2.902(2) 1_655 ?
Pb1 Cl1 2.905(2) . ?
Pb1 Cl1 2.905(2) 2_677 ?
Pb1 Cl2 2.907(2) . ?
Pb1 Cl2 2.907(2) 2_677 ?
Pb2 Cl4 2.6521(17) . ?
Pb2 Cl3 2.7973(18) . ?
Pb2 Cl2 2.8826(18) . ?
Pb2 Cl3 2.9540(18) 1_655 ?
Pb2 Cl2 3.037(2) 1_655 ?
C1 C3 1.366(11) 2_767 ?
C1 C2 1.386(9) . ?
C2 C3 1.402(9) . ?
C2 C4 1.458(11) . ?
C4 C5 1.325(10) . ?
C5 C6 1.445(11) . ?
C6 C10 1.387(10) . ?
C6 C7 1.430(9) . ?
C7 C8 1.338(11) . ?
C8 N1 1.341(10) . ?
C9 C10 1.322(12) . ?
C9 N1 1.333(11) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 Cl4 0.86 2.52 3.259(8) 145.2 2_566
N1 H1 Cl3 0.86 2.85 3.418(8) 125.2 2_566
C10 H10 Cl3 0.93 2.96 3.648(8) 131.9 1_545
C9 H9 Cl3 0.93 2.89 3.462(8) 120.9 2_566
C9 H9 Cl3 0.93 2.95 3.642(7) 132.1 1_445
C8 H8 Cl4 0.93 2.86 3.518(7) 129.2 1_455
