#------------------------------------------------------------------------------
#$Date: 2019-11-05 11:46:51 +0200 (Tue, 05 Nov 2019) $
#$Revision: 223317 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/16/7701605.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_7701605
loop_
_publ_author_name
'Venkatesan, Naveen R.'
'Mahdi, Ali'
'Barraza, Brian'
'Wu, Guang'
'Chabinyc, Michael L.'
'Seshadri, Ram'
_publ_section_title
;
 Enhanced yield-mobility products in hybrid halide Ruddlesden-Popper
 compounds with aromatic ammonium spacers.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14019
_journal_page_last               14026
_journal_paper_doi               10.1039/c9dt03074c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C28 H28 I4 N2 Pb'
_chemical_formula_weight         1107.31
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-07-16 deposited with the CCDC.	2019-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   42.920(6)
_cell_length_b                   8.7431(11)
_cell_length_c                   8.6629(14)
_cell_measurement_reflns_used    873
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.6
_cell_measurement_theta_min      2.76
_cell_volume                     3250.8(8)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker kappa Apex II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0953
_diffrn_reflns_av_unetI/netI     0.0855
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            10433
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.439
_diffrn_reflns_theta_min         1.898
_exptl_absorpt_coefficient_mu    9.007
_exptl_absorpt_correction_T_max  0.662
_exptl_absorpt_correction_T_min  0.345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.263
_exptl_crystal_description       plate
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.612
_refine_diff_density_min         -1.446
_refine_diff_density_rms         0.315
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.436
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         2500
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.427
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0533
_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)+0.4397P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0892
_reflns_Friedel_coverage         0.866
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                1780
_reflns_number_total             2500
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt03074c2.cif
_cod_data_source_block           check
_cod_database_code               7701605
_shelx_shelxl_version_number     2014/7
_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_min   0.345
_shelx_estimated_absorpt_t_max   0.662
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, 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
C4 C 0.3670(5) 0.134(3) 0.594(2) 0.032(4) Uani 1 1 d D . .
H4 H 0.3767 0.0411 0.5720 0.038 Uiso 1 1 calc R U .
C5 C 0.3464(5) 0.140(2) 0.720(2) 0.025(4) Uani 1 1 d . . .
H5 H 0.3423 0.0514 0.7754 0.030 Uiso 1 1 calc R U .
C6 C 0.3324(6) 0.272(3) 0.761(3) 0.034(5) Uani 1 1 d . . .
C7 C 0.3379(5) 0.406(2) 0.669(2) 0.025(4) Uani 1 1 d . . .
H7 H 0.3279 0.4977 0.6926 0.030 Uiso 1 1 calc R U .
C8 C 0.3587(5) 0.400(3) 0.541(3) 0.032(4) Uani 1 1 d D . .
H8 H 0.3627 0.4872 0.4823 0.038 Uiso 1 1 calc R U .
C9 C 0.3095(4) 0.285(3) 0.887(2) 0.021(4) Uani 1 1 d D . .
C10 C 0.3152(5) 0.197(3) 1.022(2) 0.042(6) Uani 1 1 d D . .
H10 H 0.3326 0.1337 1.0272 0.051 Uiso 1 1 calc R U .
C11 C 0.2943(5) 0.206(3) 1.148(2) 0.065(7) Uani 1 1 d D . .
H11 H 0.2985 0.1522 1.2388 0.078 Uiso 1 1 calc R U .
C12 C 0.2669(4) 0.296(2) 1.137(2) 0.034(5) Uani 1 1 d D . .
H12 H 0.2522 0.2937 1.2161 0.041 Uiso 1 1 calc R U .
C13 C 0.2620(5) 0.390(3) 1.006(2) 0.065(7) Uani 1 1 d D . .
H13 H 0.2448 0.4546 1.0012 0.078 Uiso 1 1 calc R U .
C14 C 0.2834(5) 0.384(2) 0.881(2) 0.042(6) Uani 1 1 d D . .
H14 H 0.2803 0.4451 0.7946 0.051 Uiso 1 1 calc R U .
I1 I 0.5000 0.9414(3) 0.1268(3) 0.0152(10) Uani 1 2 d S T P
I2 I 0.42531(3) 0.7545(5) 0.4347(6) 0.0278(4) Uani 1 1 d . . .
I3 I 0.5000 0.4399(4) 0.2479(3) 0.0162(10) Uani 1 2 d S T P
Pb1 Pb 0.5000 0.7453(3) 0.4417(5) 0.0116(2) Uani 1 2 d S T P
N1 N 0.4376(6) 0.334(2) 0.515(2) 0.034(7) Uani 1 1 d . . .
H1A H 0.4338 0.4271 0.4780 0.051 Uiso 1 1 calc R U .
H1B H 0.4579 0.3246 0.5352 0.051 Uiso 1 1 calc R U .
H1C H 0.4267 0.3192 0.6007 0.051 Uiso 1 1 calc R U .
C1 C 0.4285(5) 0.219(3) 0.399(3) 0.036(5) Uani 1 1 d D . .
H1D H 0.4311 0.1162 0.4391 0.044 Uiso 1 1 calc R U .
H1E H 0.4410 0.2292 0.3059 0.044 Uiso 1 1 calc R U .
C3 C 0.3735(5) 0.258(3) 0.503(2) 0.021(4) Uani 1 1 d . . .
C2 C 0.3947(5) 0.251(3) 0.365(3) 0.036(5) Uani 1 1 d D . .
H2A H 0.3934 0.3482 0.3110 0.044 Uiso 1 1 calc R U .
H2B H 0.3870 0.1728 0.2958 0.044 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
H H 0.0000 0.0000 '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
C3 C4 C5 123(2) . .
C3 C4 H4 118.5 . .
C5 C4 H4 118.5 . .
C6 C5 C4 121(2) . .
C6 C5 H5 119.4 . .
C4 C5 H5 119.4 . .
C5 C6 C7 119(2) . .
C5 C6 C9 124(2) . .
C7 C6 C9 117(2) . .
C8 C7 C6 120(2) . .
C8 C7 H7 119.9 . .
C6 C7 H7 119.9 . .
C7 C8 C3 119(2) . .
C7 C8 H8 120.3 . .
C3 C8 H8 120.3 . .
C14 C9 C10 120.0(6) . .
C14 C9 C6 122.9(16) . .
C10 C9 C6 117.0(16) . .
C9 C10 C11 119.7(6) . .
C9 C10 H10 120.1 . .
C11 C10 H10 120.1 . .
C12 C11 C10 120.1(6) . .
C12 C11 H11 120.0 . .
C10 C11 H11 120.0 . .
C11 C12 C13 119.9(6) . .
C11 C12 H12 120.0 . .
C13 C12 H12 120.0 . .
C14 C13 C12 119.6(6) . .
C14 C13 H13 120.2 . .
C12 C13 H13 120.2 . .
C9 C14 C13 120.3(6) . .
C9 C14 H14 119.9 . .
C13 C14 H14 119.9 . .
Pb1 I1 Pb1 152.48(16) 2_674 .
Pb1 I3 Pb1 153.57(17) 2_664 .
I3 Pb1 I3 90.78(8) 2_665 .
I3 Pb1 I1 91.06(17) 2_665 2_675
I3 Pb1 I1 178.2(2) . 2_675
I3 Pb1 I2 91.68(7) 2_665 4_655
I3 Pb1 I2 90.65(7) . 4_655
I1 Pb1 I2 89.30(7) 2_675 4_655
I3 Pb1 I2 91.68(7) 2_665 .
I3 Pb1 I2 90.65(7) . .
I1 Pb1 I2 89.30(7) 2_675 .
I2 Pb1 I2 176.38(13) 4_655 .
I3 Pb1 I1 179.25(17) 2_665 .
I3 Pb1 I1 89.98(16) . .
I1 Pb1 I1 88.19(8) 2_675 .
I2 Pb1 I1 88.31(7) 4_655 .
I2 Pb1 I1 88.31(7) . .
C1 N1 H1A 109.5 . .
C1 N1 H1B 109.5 . .
H1A N1 H1B 109.5 . .
C1 N1 H1C 109.5 . .
H1A N1 H1C 109.5 . .
H1B N1 H1C 109.5 . .
N1 C1 C2 104.9(19) . .
N1 C1 H1D 110.8 . .
C2 C1 H1D 110.8 . .
N1 C1 H1E 110.8 . .
C2 C1 H1E 110.8 . .
H1D C1 H1E 108.8 . .
C4 C3 C8 118(2) . .
C4 C3 C2 123.3(19) . .
C8 C3 C2 119.0(18) . .
C3 C2 C1 116.1(18) . .
C3 C2 H2A 108.3 . .
C1 C2 H2A 108.3 . .
C3 C2 H2B 108.3 . .
C1 C2 H2B 108.3 . .
H2A C2 H2B 107.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C4 C3 1.38(3) .
C4 C5 1.40(3) .
C4 H4 0.9300 .
C5 C6 1.35(3) .
C5 H5 0.9300 .
C6 C7 1.44(3) .
C6 C9 1.48(3) .
C7 C8 1.43(3) .
C7 H7 0.9300 .
C8 C3 1.43(3) .
C8 H8 0.9300 .
C9 C14 1.416(12) .
C9 C10 1.418(12) .
C10 C11 1.419(12) .
C10 H10 0.9300 .
C11 C12 1.418(12) .
C11 H11 0.9300 .
C12 C13 1.420(12) .
C12 H12 0.9300 .
C13 C14 1.420(12) .
C13 H13 0.9300 .
C14 H14 0.9300 .
I1 Pb1 3.174(5) 2_674
I1 Pb1 3.222(5) .
I2 Pb1 3.2071(13) .
I3 Pb1 3.107(5) 2_664
I3 Pb1 3.154(5) .
Pb1 I3 3.107(5) 2_665
Pb1 I1 3.174(5) 2_675
Pb1 I2 3.2070(13) 4_655
N1 C1 1.47(3) .
N1 H1A 0.8900 .
N1 H1B 0.8900 .
N1 H1C 0.8900 .
C1 C2 1.509(11) .
C1 H1D 0.9700 .
C1 H1E 0.9700 .
C3 C2 1.50(3) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
