#------------------------------------------------------------------------------
#$Date: 2019-11-25 21:58:09 +0200 (Mon, 25 Nov 2019) $
#$Revision: 241918 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/17/4131750.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_4131750
loop_
_publ_author_name
'Sun, Cai'
'Xu, Gang'
'Jiang, Xiao-Ming'
'Wang, Guan-E'
'Guo, Pei-Yu'
'Wang, Ming-Sheng'
'Guo, Guo-Cong'
_publ_section_title
;
 Design Strategy for Improving Optical and Electrical Properties and
 Stability of Lead-Halide Semiconductors.
;
_journal_issue                   8
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2805
_journal_page_last               2811
_journal_paper_doi               10.1021/jacs.7b10101
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C32 H32 Cl2 N4 O8 Pb2, 2(Cl)'
_chemical_formula_sum            'C32 H32 Cl4 N4 O8 Pb2'
_chemical_formula_weight         1156.79
_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
_audit_creation_date             2017-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.257(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.4033(14)
_cell_length_b                   7.6867(4)
_cell_length_c                   17.4828(14)
_cell_measurement_temperature    293(2)
_cell_volume                     1799.8(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'multiwire proportional'
_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  0.1934
_diffrn_reflns_av_unetI/netI     0.1457
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16405
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.679
_diffrn_reflns_theta_min         2.733
_exptl_absorpt_coefficient_mu    9.694
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    2.135
_exptl_crystal_F_000             1096
_refine_diff_density_max         6.607
_refine_diff_density_min         -2.427
_refine_diff_density_rms         0.397
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3412
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0768
_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)+(0.0924P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1780
_refine_ls_wR_factor_ref         0.2071
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2400
_reflns_number_total             3412
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja7b10101_si_004.cif
_cod_data_source_block           14
_cod_database_code               4131750
_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 C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C20(H20A,H20B), C26(H26A,H26B), C34(H34A,H34B)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C29(H29), C31(H31), C32(H32), C33(H33), C53(H53), C58(H58), C4(H4)
;
_shelx_shelxl_version_number     2014/7
_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
Pb1 Pb -0.01728(4) -0.46714(7) -0.28244(3) 0.0350(3) Uani 1 1 d .
Cl7 Cl -0.0579(3) -0.3148(5) -0.1409(2) 0.0479(10) Uani 1 1 d .
O1 O -0.1905(8) -0.5477(14) -0.3036(7) 0.050(3) Uani 1 1 d .
O2 O -0.1006(8) -0.1922(12) -0.3222(5) 0.041(3) Uani 1 1 d .
O4 O -0.0473(8) -0.3443(13) -0.4203(5) 0.046(3) Uani 1 1 d .
O17 O -0.1531(8) -0.7531(15) -0.2152(7) 0.055(3) Uani 1 1 d .
N7 N -0.2222(9) 0.2008(15) -0.4622(7) 0.034(3) Uani 1 1 d .
N12 N -0.3648(9) -0.3764(15) -0.2112(6) 0.031(3) Uani 1 1 d .
C6 C -0.1418(12) -0.087(2) -0.4492(10) 0.043(4) Uani 1 1 d .
H6A H -0.0925 -0.0388 -0.4825 0.052 Uiso 1 1 calc R
H6B H -0.1921 -0.1453 -0.4812 0.052 Uiso 1 1 calc R
C11 C -0.3001(10) -0.2559(18) -0.2327(8) 0.034(3) Uani 1 1 d .
H11 H -0.2727 -0.2635 -0.2806 0.041 Uiso 1 1 calc R
C13 C -0.2811(11) 0.4629(17) -0.5600(8) 0.033(3) Uani 1 1 d .
C19 C -0.2111(13) -0.662(2) -0.2541(9) 0.042(4) Uani 1 1 d .
C20 C -0.3907(13) -0.5275(18) -0.2596(10) 0.042(4) Uani 1 1 d .
H20A H -0.3834 -0.4960 -0.3129 0.051 Uiso 1 1 calc R
H20B H -0.4601 -0.5574 -0.2531 0.051 Uiso 1 1 calc R
C21 C -0.0920(11) -0.2175(19) -0.3961(8) 0.036(4) Uani 1 1 d .
C26 C -0.1900(11) 0.0592(17) -0.4073(9) 0.032(3) Uani 1 1 d .
H26A H -0.1431 0.1059 -0.3690 0.038 Uiso 1 1 calc R
H26B H -0.2475 0.0155 -0.3814 0.038 Uiso 1 1 calc R
C28 C -0.3124(10) -0.1086(19) -0.1132(8) 0.032(3) Uani 1 1 d .
C29 C -0.1537(12) 0.3106(19) -0.4910(8) 0.040(4) Uani 1 1 d .
H29 H -0.0865 0.2975 -0.4768 0.047 Uiso 1 1 calc R
C31 C -0.2727(11) -0.1177(19) -0.1837(8) 0.035(3) Uani 1 1 d .
H31 H -0.2281 -0.0334 -0.1993 0.042 Uiso 1 1 calc R
C32 C -0.1826(10) 0.4391(18) -0.5402(9) 0.034(4) Uani 1 1 d .
H32 H -0.1348 0.5116 -0.5605 0.041 Uiso 1 1 calc R
C33 C -0.4023(12) -0.366(2) -0.1413(9) 0.043(4) Uani 1 1 d .
H33 H -0.4447 -0.4535 -0.1253 0.052 Uiso 1 1 calc R
C34 C -0.3266(11) -0.6850(19) -0.2414(9) 0.041(4) Uani 1 1 d .
H34A H -0.3510 -0.7812 -0.2728 0.049 Uiso 1 1 calc R
H34B H -0.3351 -0.7166 -0.1883 0.049 Uiso 1 1 calc R
C53 C -0.3189(12) 0.219(2) -0.4817(9) 0.045(4) Uani 1 1 d .
H53 H -0.3652 0.1418 -0.4627 0.054 Uiso 1 1 calc R
C58 C -0.3510(11) 0.353(2) -0.5301(9) 0.041(4) Uani 1 1 d .
H58 H -0.4186 0.3681 -0.5422 0.049 Uiso 1 1 calc R
C4 C -0.3798(12) -0.231(2) -0.0935(9) 0.046(4) Uani 1 1 d .
H4 H -0.4108 -0.2225 -0.0470 0.055 Uiso 1 1 calc R
Cl1 Cl -0.4229(3) -0.1760(6) -0.3961(2) 0.0523(11) 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
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'
O O 0.0106 0.0060 '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_3
O1 Pb1 Cl7 91.3(3) .
O1 Pb1 O2 75.9(3) .
O1 Pb1 O4 80.7(4) .
O2 Pb1 Cl7 77.9(2) .
O2 Pb1 O4 51.6(3) .
O4 Pb1 Cl7 129.4(2) .
C19 O1 Pb1 107.8(10) .
C21 O2 Pb1 95.4(8) .
C21 O4 Pb1 91.7(9) .
C29 N7 C26 120.3(12) .
C53 N7 C26 119.4(12) .
C53 N7 C29 120.2(13) .
C11 N12 C20 121.9(12) .
C11 N12 C33 119.1(12) .
C33 N12 C20 118.8(13) .
H6A C6 H6B 107.8 .
C21 C6 H6A 109.0 .
C21 C6 H6B 109.0 .
C26 C6 H6A 109.0 .
C26 C6 H6B 109.0 .
C26 C6 C21 112.8(14) .
N12 C11 H11 119.6 .
N12 C11 C31 120.8(13) .
C31 C11 H11 119.6 .
C32 C13 C28 120.0(13) 4_565
C32 C13 C58 119.1(14) .
C58 C13 C28 120.9(14) 4_565
O1 C19 C34 114.3(14) .
O17 C19 O1 128.2(16) .
O17 C19 C34 117.5(14) .
N12 C20 H20A 109.0 .
N12 C20 H20B 109.0 .
N12 C20 C34 113.1(13) .
H20A C20 H20B 107.8 .
C34 C20 H20A 109.0 .
C34 C20 H20B 109.0 .
O2 C21 C6 116.9(13) .
O4 C21 O2 121.2(13) .
O4 C21 C6 121.9(13) .
N7 C26 H26A 109.6 .
N7 C26 H26B 109.6 .
C6 C26 N7 110.4(13) .
C6 C26 H26A 109.6 .
C6 C26 H26B 109.6 .
H26A C26 H26B 108.1 .
C31 C28 C13 119.2(13) 4_566
C4 C28 C13 122.1(13) 4_566
C4 C28 C31 118.7(14) .
N7 C29 H29 119.8 .
C32 C29 N7 120.5(14) .
C32 C29 H29 119.8 .
C11 C31 H31 120.4 .
C28 C31 C11 119.2(14) .
C28 C31 H31 120.4 .
C13 C32 H32 119.7 .
C29 C32 C13 120.5(14) .
C29 C32 H32 119.7 .
N12 C33 H33 119.2 .
N12 C33 C4 121.6(15) .
C4 C33 H33 119.2 .
C19 C34 H34A 108.4 .
C19 C34 H34B 108.4 .
C20 C34 C19 115.7(13) .
C20 C34 H34A 108.4 .
C20 C34 H34B 108.4 .
H34A C34 H34B 107.4 .
N7 C53 H53 119.7 .
N7 C53 C58 120.5(14) .
C58 C53 H53 119.7 .
C13 C58 C53 119.1(14) .
C13 C58 H58 120.4 .
C53 C58 H58 120.4 .
C28 C4 C33 120.5(14) .
C28 C4 H4 119.8 .
C33 C4 H4 119.8 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 Cl7 2.810(4) .
Pb1 O1 2.417(11) .
Pb1 O2 2.477(10) .
Pb1 O4 2.605(10) .
O1 C19 1.273(18) .
O2 C21 1.316(17) .
O4 C21 1.227(17) .
O17 C19 1.230(18) .
N7 C26 1.503(17) .
N7 C29 1.358(18) .
N7 C53 1.336(18) .
N12 C11 1.333(17) .
N12 C20 1.470(18) .
N12 C33 1.342(18) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C6 C21 1.51(2) .
C6 C26 1.50(2) .
C11 H11 0.9300 .
C11 C31 1.40(2) .
C13 C28 1.50(2) 4_565
C13 C32 1.36(2) .
C13 C58 1.38(2) .
C19 C34 1.58(2) .
C20 H20A 0.9700 .
C20 H20B 0.9700 .
C20 C34 1.51(2) .
C26 H26A 0.9700 .
C26 H26B 0.9700 .
C28 C13 1.50(2) 4_566
C28 C31 1.365(19) .
C28 C4 1.36(2) .
C29 H29 0.9300 .
C29 C32 1.36(2) .
C31 H31 0.9300 .
C32 H32 0.9300 .
C33 H33 0.9300 .
C33 C4 1.36(2) .
C34 H34A 0.9700 .
C34 H34B 0.9700 .
C53 H53 0.9300 .
C53 C58 1.39(2) .
C58 H58 0.9300 .
C4 H4 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
Pb1 O1 C19 O17 -17.9(19) .
Pb1 O1 C19 C34 160.9(9) .
Pb1 O2 C21 O4 -3.7(15) .
Pb1 O2 C21 C6 174.6(11) .
Pb1 O4 C21 O2 3.5(14) .
Pb1 O4 C21 C6 -174.7(13) .
O1 C19 C34 C20 -25.8(19) .
O17 C19 C34 C20 153.1(14) .
N7 C29 C32 C13 2(2) .
N7 C53 C58 C13 2(2) .
N12 C11 C31 C28 1(2) .
N12 C20 C34 C19 -62.3(18) .
N12 C33 C4 C28 -5(3) .
C11 N12 C20 C34 92.8(17) .
C11 N12 C33 C4 3(2) .
C13 C28 C31 C11 178.5(13) 4_566
C13 C28 C4 C33 -176.5(14) 4_566
C20 N12 C11 C31 -176.7(13) .
C20 N12 C33 C4 178.9(14) .
C21 C6 C26 N7 169.9(12) .
C26 N7 C29 C32 -179.7(13) .
C26 N7 C53 C58 177.7(14) .
C26 C6 C21 O2 3(2) .
C26 C6 C21 O4 -178.8(14) .
C28 C13 C32 C29 178.5(14) 4_565
C28 C13 C58 C53 179.5(14) 4_565
C29 N7 C26 C6 -75.5(16) .
C29 N7 C53 C58 -2(2) .
C31 C28 C4 C33 4(2) .
C32 C13 C58 C53 -1(2) .
C33 N12 C11 C31 -1(2) .
C33 N12 C20 C34 -82.6(18) .
C53 N7 C26 C6 105.3(16) .
C53 N7 C29 C32 0(2) .
C58 C13 C32 C29 -1(2) .
C4 C28 C31 C11 -2(2) .
