#------------------------------------------------------------------------------
#$Date: 2016-11-08 21:35:23 +0200 (Tue, 08 Nov 2016) $
#$Revision: 188108 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/65/7226591.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_7226591
loop_
_publ_author_name
'Gómez, Verónica'
'Fuhr, Olaf'
'Ruben, Mario'
_publ_section_title
;
 Structural diversity in substituted-pyridinium iodo- and bromoplumbates:
 a matter of halide and temperature
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              8207
_journal_paper_doi               10.1039/C6CE01684G
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'I3 Pb, C5 H5 Cl N'
_chemical_formula_sum            'C5 H5 Cl I3 N Pb'
_chemical_formula_weight         702.44
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-25 deposited with the CCDC.
2016-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.140(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0224(7)
_cell_length_b                   14.7278(7)
_cell_length_c                   8.0001(5)
_cell_measurement_reflns_used    11875
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      26.20
_cell_measurement_theta_min      2.33
_cell_volume                     1278.42(13)
_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_temperature      180.15
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            8435
_diffrn_reflns_point_group_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.621
_diffrn_reflns_theta_min         2.331
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_target            Mo
_diffrn_source_type              'sealed X-ray tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    20.603
_exptl_absorpt_correction_T_max  0.1832
_exptl_absorpt_correction_T_min  0.0188
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.650
_exptl_crystal_description       plate
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.548
_refine_diff_density_min         -1.862
_refine_diff_density_rms         0.212
_refine_ls_extinction_coef       0.00199(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         2388
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0277
_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)+(0.0449P)²+1.4012P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0717
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2188
_reflns_number_total             2388
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ce01684g2.cif
_cod_data_source_block           vp-121bis4
_cod_depositor_comments
'Adding full bibliography for 7226587--7226601.cif.'
_cod_database_code               7226591
_shelxl_version_number           2014/6
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C1(H1A), C3(H3), C4(H4), C5(H5)
;
_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 0.30253(2) 0.75027(2) 0.03273(2) 0.02751(12) Uani 1 1 d .
I1 I 0.11073(4) 0.84042(2) 0.23288(5) 0.03184(13) Uani 1 1 d .
I2 I 0.30903(4) 0.92049(2) -0.21670(4) 0.03144(13) Uani 1 1 d .
I3 I 0.50778(4) 0.66034(2) -0.17033(5) 0.03088(13) Uani 1 1 d .
Cl1 Cl -0.08162(18) 0.89870(13) 0.5487(2) 0.0539(4) Uani 1 1 d .
N1 N -0.3562(5) 0.9407(3) 0.7851(6) 0.0347(11) Uani 1 1 d .
H1 H -0.4249 0.9725 0.7669 0.042 Uiso 1 1 calc R
C1 C -0.2812(6) 0.9457(4) 0.6700(8) 0.0326(12) Uani 1 1 d .
H1A H -0.3012 0.9829 0.5721 0.039 Uiso 1 1 calc R
C2 C -0.1747(6) 0.8952(4) 0.6984(7) 0.0340(12) Uani 1 1 d .
C3 C -0.1455(7) 0.8440(4) 0.8426(8) 0.0400(14) Uani 1 1 d .
H3 H -0.0708 0.8103 0.8634 0.048 Uiso 1 1 calc R
C4 C -0.2254(7) 0.8417(4) 0.9577(8) 0.0439(15) Uani 1 1 d .
H4 H -0.2059 0.8066 1.0585 0.053 Uiso 1 1 calc R
C5 C -0.3323(7) 0.8901(4) 0.9256(8) 0.0381(13) Uani 1 1 d .
H5 H -0.3890 0.8880 1.0022 0.046 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 0.0033 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'
N N 0.0061 0.0033 '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'
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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.0570
-1 0 0 0.0400
1 2 0 0.0910
0 -1 -1 0.2300
0 1 1 0.1820
1 -1 0 0.0880
-1 -2 0 0.1250
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
I1 Pb1 I1 98.206(13) . 4_575
I1 Pb1 I2 94.412(11) . .
I1 Pb1 I2 87.484(10) . 4_576
I1 Pb1 I2 86.796(11) 4_575 .
I1 Pb1 I2 94.610(11) 4_575 4_576
I1 Pb1 I3 177.447(11) 4_575 4_576
I1 Pb1 I3 83.257(11) 4_575 .
I1 Pb1 I3 178.442(11) . .
I1 Pb1 I3 84.339(11) . 4_576
I2 Pb1 I2 177.463(15) 4_576 .
I2 Pb1 I3 85.691(10) 4_576 4_576
I2 Pb1 I3 92.943(11) 4_576 .
I2 Pb1 I3 85.118(10) . .
I2 Pb1 I3 92.811(11) . 4_576
I3 Pb1 I3 94.197(13) 4_576 .
Pb1 I1 Pb1 77.977(10) . 4_576
Pb1 I2 Pb1 77.055(9) 4_575 .
Pb1 I3 Pb1 75.369(10) 4_575 .
C1 N1 H1 118.2 . .
C5 N1 H1 118.2 . .
C5 N1 C1 123.6(6) . .
N1 C1 H1A 121.0 . .
N1 C1 C2 117.9(6) . .
C2 C1 H1A 121.0 . .
C1 C2 Cl1 117.9(5) . .
C3 C2 Cl1 121.7(5) . .
C3 C2 C1 120.3(6) . .
C2 C3 H3 120.3 . .
C2 C3 C4 119.5(6) . .
C4 C3 H3 120.3 . .
C3 C4 H4 120.2 . .
C5 C4 C3 119.5(6) . .
C5 C4 H4 120.2 . .
N1 C5 C4 119.1(6) . .
N1 C5 H5 120.4 . .
C4 C5 H5 120.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 I1 3.1604(4) .
Pb1 I1 3.1972(4) 4_575
Pb1 I2 3.2128(4) .
Pb1 I2 3.2090(4) 4_576
Pb1 I3 3.2561(4) 4_576
Pb1 I3 3.2872(4) .
I1 Pb1 3.1972(4) 4_576
I2 Pb1 3.2090(4) 4_575
I3 Pb1 3.2561(4) 4_575
Cl1 C2 1.710(6) .
N1 H1 0.8800 .
N1 C1 1.343(8) .
N1 C5 1.336(8) .
C1 H1A 0.9500 .
C1 C2 1.375(9) .
C2 C3 1.368(9) .
C3 H3 0.9500 .
C3 C4 1.382(10) .
C4 H4 0.9500 .
C4 C5 1.363(10) .
C5 H5 0.9500 .
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
Cl1 C2 C3 C4 -178.4(5)
N1 C1 C2 Cl1 178.0(4)
N1 C1 C2 C3 -2.0(9)
C1 N1 C5 C4 1.2(9)
C1 C2 C3 C4 1.6(10)
C2 C3 C4 C5 0.3(10)
C3 C4 C5 N1 -1.6(10)
C5 N1 C1 C2 0.6(9)
