#------------------------------------------------------------------------------
#$Date: 2019-10-02 04:07:17 +0300 (Wed, 02 Oct 2019) $
#$Revision: 218988 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/12/7701281.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_7701281
loop_
_publ_author_name
'Oswald, Iain W. H.'
'Ahn, Hyochul'
'Neilson, James Richmond'
_publ_section_title
;
 Influence of organic cation planarity on structural templating in hybrid
 metal-halides
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03207J
_journal_year                    2019
_chemical_formula_sum            'C20 H20 I10 N4 Pb3'
_chemical_formula_weight         2206.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-08-06 deposited with the CCDC.    2019-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.4910(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.0581(9)
_cell_length_b                   9.6584(4)
_cell_length_c                   20.2649(8)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      26.48
_cell_measurement_theta_min      2.32
_cell_volume                     4073.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'APEX3 (Bruker-AXS, 2015)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Vesta (K. Momma and F. Izumi, 2011)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Quest ECO CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'HELIOS optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27016
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         2.754
_diffrn_source                   'I\ms microfocus tube'
_exptl_absorpt_coefficient_mu    19.964
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    3.598
_exptl_crystal_description       Needle
_exptl_crystal_F_000             3776
_exptl_crystal_size_max          0.069
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.244
_refine_diff_density_min         -1.070
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         4203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0283
_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)+(0.0326P)²+17.4976P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0702
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3436
_reflns_number_total             4203
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt03207j2.cif
_cod_data_source_block           jrn089_a2_C2c_a
_cod_database_code               7701281
_shelx_shelxl_version_number     2017/1
_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   0.340
_shelx_estimated_absorpt_t_max   0.691
_publcif_funding_html
;
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Pb1 Pb 0.35414(2) 0.73440(3) 0.55324(2) 0.03809(9) Uani 1 1 d . . .
Pb2 Pb 0.500000 0.72704(4) 0.750000 0.04067(11) Uani 1 2 d S T P
I1 I 0.24478(2) 0.50023(5) 0.49378(2) 0.03932(12) Uani 1 1 d . . .
I2 I 0.46307(2) 0.96512(5) 0.62693(3) 0.04497(13) Uani 1 1 d . . .
I3 I 0.34868(3) 0.69645(6) 0.71471(3) 0.04736(13) Uani 1 1 d . . .
I4 I 0.46668(2) 0.50470(5) 0.62091(3) 0.04738(13) Uani 1 1 d . . .
I5 I 0.35964(3) 0.72084(5) 0.40329(3) 0.04879(14) Uani 1 1 d . . .
N1 N 0.1956(3) 0.1828(7) 0.3353(4) 0.066(2) Uani 1 1 d . . .
H1A H 0.211071 0.108885 0.360414 0.079 Uiso 1 1 calc R U .
N2 N 0.3451(3) 0.3628(6) 0.4013(3) 0.0429(14) Uani 1 1 d . . .
H2A H 0.328379 0.444268 0.393051 0.051 Uiso 1 1 calc R U .
C1 C 0.1325(5) 0.1930(10) 0.2985(6) 0.078(3) Uani 1 1 d . . .
H1 H 0.106510 0.119972 0.299387 0.094 Uiso 1 1 calc R U .
C2 C 0.1051(4) 0.3085(9) 0.2595(5) 0.055(2) Uani 1 1 d . . .
H2 H 0.060768 0.316610 0.233651 0.066 Uiso 1 1 calc R U .
C3 C 0.1446(4) 0.4107(8) 0.2597(4) 0.055(2) Uani 1 1 d . . .
H3 H 0.127285 0.491669 0.233873 0.066 Uiso 1 1 calc R U .
C4 C 0.2103(4) 0.3977(7) 0.2976(4) 0.053(2) Uani 1 1 d . . .
H4 H 0.236717 0.469985 0.296962 0.063 Uiso 1 1 calc R U .
C5 C 0.2370(4) 0.2814(7) 0.3356(4) 0.0345(15) Uani 1 1 d . . .
C6 C 0.3055(4) 0.2526(7) 0.3761(4) 0.0374(16) Uani 1 1 d . . .
C7 C 0.3329(4) 0.1238(7) 0.3899(4) 0.0434(17) Uani 1 1 d . . .
H7 H 0.306999 0.045849 0.372904 0.052 Uiso 1 1 calc R U .
C8 C 0.3981(4) 0.1084(8) 0.4284(4) 0.0499(19) Uani 1 1 d . . .
H8 H 0.416151 0.020279 0.438099 0.060 Uiso 1 1 calc R U .
C9 C 0.4368(4) 0.2233(9) 0.4526(5) 0.055(2) Uani 1 1 d . . .
H9 H 0.481157 0.214692 0.478153 0.066 Uiso 1 1 calc R U .
C10 C 0.4079(4) 0.3518(9) 0.4377(4) 0.0498(19) Uani 1 1 d . . .
H10 H 0.432891 0.431175 0.453529 0.060 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'
H H 0.0000 0.0000 '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'
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
I5 Pb1 I2 97.563(15) . .
I5 Pb1 I1 87.662(14) . .
I2 Pb1 I1 174.740(15) . .
I5 Pb1 I4 91.303(15) . .
I2 Pb1 I4 87.394(15) . .
I1 Pb1 I4 91.897(15) . .
I5 Pb1 I1 93.717(14) . 7_566
I2 Pb1 I1 84.252(14) . 7_566
I1 Pb1 I1 96.059(14) . 7_566
I4 Pb1 I1 170.752(15) . 7_566
I5 Pb1 I3 171.291(16) . .
I2 Pb1 I3 88.415(14) . .
I1 Pb1 I3 86.325(14) . .
I4 Pb1 I3 82.612(14) . .
I1 Pb1 I3 93.177(14) 7_566 .
I4 Pb2 I4 96.08(2) 2_656 .
I4 Pb2 I2 175.884(15) 2_656 .
I4 Pb2 I2 87.470(14) . .
I4 Pb2 I2 87.469(14) 2_656 2_656
I4 Pb2 I2 175.885(15) . 2_656
I2 Pb2 I2 89.06(2) . 2_656
I4 Pb2 I3 88.642(14) 2_656 .
I4 Pb2 I3 84.402(14) . .
I2 Pb2 I3 89.629(14) . .
I2 Pb2 I3 97.800(14) 2_656 .
I4 Pb2 I3 84.403(14) 2_656 2_656
I4 Pb2 I3 88.644(14) . 2_656
I2 Pb2 I3 97.800(14) . 2_656
I2 Pb2 I3 89.628(14) 2_656 2_656
I3 Pb2 I3 169.60(2) . 2_656
Pb1 I1 Pb1 83.942(14) . 7_566
Pb1 I2 Pb2 75.985(13) . .
Pb2 I3 Pb1 73.596(12) . .
Pb2 I4 Pb1 75.751(12) . .
C1 N1 C5 123.8(7) . .
C1 N1 H1A 118.1 . .
C5 N1 H1A 118.1 . .
C10 N2 C6 123.3(7) . .
C10 N2 H2A 118.4 . .
C6 N2 H2A 118.4 . .
N1 C1 C2 120.8(9) . .
N1 C1 H1 119.6 . .
C2 C1 H1 119.6 . .
C3 C2 C1 117.3(9) . .
C3 C2 H2 121.3 . .
C1 C2 H2 121.3 . .
C2 C3 C4 121.1(7) . .
C2 C3 H3 119.5 . .
C4 C3 H3 119.5 . .
C5 C4 C3 120.9(7) . .
C5 C4 H4 119.5 . .
C3 C4 H4 119.5 . .
N1 C5 C4 116.0(7) . .
N1 C5 C6 117.5(6) . .
C4 C5 C6 126.5(7) . .
N2 C6 C7 117.6(7) . .
N2 C6 C5 117.0(6) . .
C7 C6 C5 125.5(7) . .
C6 C7 C8 120.7(7) . .
C6 C7 H7 119.6 . .
C8 C7 H7 119.6 . .
C7 C8 C9 119.9(8) . .
C7 C8 H8 120.0 . .
C9 C8 H8 120.0 . .
C8 C9 C10 118.0(8) . .
C8 C9 H9 121.0 . .
C10 C9 H9 121.0 . .
N2 C10 C9 120.5(7) . .
N2 C10 H10 119.7 . .
C9 C10 H10 119.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 I5 3.0984(6) .
Pb1 I2 3.2056(5) .
Pb1 I1 3.2109(5) .
Pb1 I4 3.2363(6) .
Pb1 I1 3.2877(5) 7_566
Pb1 I3 3.3485(6) .
Pb2 I4 3.2118(6) 2_656
Pb2 I4 3.2118(6) .
Pb2 I2 3.2257(6) .
Pb2 I2 3.2257(6) 2_656
Pb2 I3 3.2596(5) .
Pb2 I3 3.2597(5) 2_656
N1 C1 1.323(11) .
N1 C5 1.346(9) .
N1 H1A 0.8600 .
N2 C10 1.316(9) .
N2 C6 1.350(9) .
N2 H2A 0.8600 .
C1 C2 1.356(12) .
C1 H1 0.9300 .
C2 C3 1.341(12) .
C2 H2 0.9300 .
C3 C4 1.380(11) .
C3 H3 0.9300 .
C4 C5 1.351(10) .
C4 H4 0.9300 .
C5 C6 1.461(11) .
C6 C7 1.368(9) .
C7 C8 1.372(10) .
C7 H7 0.9300 .
C8 C9 1.376(11) .
C8 H8 0.9300 .
C9 C10 1.379(11) .
C9 H9 0.9300 .
C10 H10 0.9300 .
