#------------------------------------------------------------------------------
#$Date: 2016-11-08 21:35:23 +0200 (Tue, 08 Nov 2016) $
#$Revision: 188108 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/65/7226595.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_7226595
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         '0.5(I6 Pb2), C6 H8 N'
_chemical_formula_sum            'C6 H8 I3 N Pb'
_chemical_formula_weight         682.02
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.23 svn.r3337 for OlexSys, GUI svn.r5217)
;
_audit_update_record
;
2016-08-30 deposited with the CCDC.
2016-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9441(6)
_cell_length_b                   10.5453(3)
_cell_length_c                   15.6630(6)
_cell_measurement_reflns_used    9204
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      26.04
_cell_measurement_theta_min      2.33
_cell_volume                     1312.14(12)
_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 0.953
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8374
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.596
_diffrn_reflns_theta_min         2.328
_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    19.871
_exptl_absorpt_correction_T_max  0.2210
_exptl_absorpt_correction_T_min  0.0396
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.452
_exptl_crystal_description       plate
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.938
_refine_diff_density_min         -1.714
_refine_diff_density_rms         0.192
_refine_ls_extinction_coef       0.00091(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     60
_refine_ls_number_reflns         1301
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0256
_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)+(0.0441P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0635
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1078
_reflns_number_total             1301
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ce01684g2.cif
_cod_data_source_block           vp-125bis3p
_cod_depositor_comments
'Adding full bibliography for 7226587--7226601.cif.'
_cod_database_code               7226595
_shelxl_version_number           2013-4
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H4A(0.5) H4B(0.5) H4C(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C1(H1A), C2(H2)
3.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_shelx_res_file
;
TITL Vp-125bis3p in Pnma #62
REM reset to Pnma #62
CELL 0.71073 7.9441 10.5453 15.663 90 90 90
ZERR 4 0.0006 0.0003 0.0006 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,0.5-Z
SYMM -X,0.5+Y,-Z
SFAC C H I N Pb
UNIT 24 32 12 4 4

L.S. 4 0 0
PLAN  20
TEMP -93
BOND
MORE -1
BOND $H
CONF
fmap 2 53
acta 52
REM <olex2.extras>
REM <HklSrc "%.\\Vp-125bis3p.hkl">
REM </olex2.extras>

WGHT    0.044100
EXTI    0.000908
FVAR       0.17474
PB1   5    0.627997    0.250000    0.248227    10.50000    0.01702    0.03963 =
         0.03490    0.00000    0.00000    0.00000
I1    3    0.357442    0.250000    0.411519    10.50000    0.02996    0.04973 =
         0.03331    0.00000   -0.00468    0.00000
I2    3    0.887677    0.048040    0.339391    11.00000    0.02897    0.03503 =
         0.03773    0.00097    0.00223   -0.00019
N1    4    0.782463    0.250000    0.527670    10.50000    0.04255    0.09023 =
         0.02704    0.00000    0.01026    0.00000
AFIX  43
H1    2    0.861080    0.250000    0.488089    10.50000   -1.20000
AFIX   0
C1    1    0.724845    0.360877    0.556680    11.00000    0.05522    0.06584 =
         0.03749   -0.00089    0.00256   -0.02451
AFIX  43
H1A   2    0.768052    0.437978    0.534231    11.00000   -1.20000
AFIX   0
C2    1    0.604561    0.363510    0.618233    11.00000    0.04771    0.03946 =
         0.03858   -0.00281   -0.00321   -0.01023
AFIX  43
H2    2    0.564395    0.442340    0.639374    11.00000   -1.20000
AFIX   0
C3    1    0.540141    0.250000    0.650333    10.50000    0.03032    0.03755 =
         0.03897    0.00000   -0.01003    0.00000
C4    1    0.406022    0.250000    0.716926    10.50000    0.03223    0.04521 =
         0.05733    0.00000    0.00583    0.00000
PART -1
AFIX 137
H4A   2    0.448641    0.290801    0.768820    10.50000   -1.50000
H4B   2    0.373449    0.162450    0.729864    10.50000   -1.50000
H4C   2    0.307824    0.296749    0.695865    10.50000   -1.50000
AFIX   0
HKLF 4

REM  Vp-125bis3p in Pnma #62
REM R1 =  0.0256 for    1078 Fo > 4sig(Fo)  and  0.0326 for all    1301 data
REM     60 parameters refined using      0 restraints

END

WGHT      0.0441      0.0000

REM Highest difference peak  0.938,  deepest hole -1.714,  1-sigma level  0.192
Q1    1   0.9028  0.2500  0.4083  10.50000  0.05    0.94
Q2    1   0.5267  0.3411  0.2469  11.00000  0.05    0.82
Q3    1   0.7275  0.3408  0.2473  11.00000  0.05    0.79
Q4    1   0.6205  0.3401  0.3219  11.00000  0.05    0.79
Q5    1   0.5692  0.2500  0.2832  10.50000  0.05    0.79
Q6    1   0.6848  0.2500  0.2773  10.50000  0.05    0.78
Q7    1   0.6255  0.5438  0.6655  11.00000  0.05    0.73
Q8    1   0.3824  0.3399  0.3416  11.00000  0.05    0.68
Q9    1   0.2959  0.2500  0.4441  10.50000  0.05    0.68
Q10   1   0.5854  0.2500  0.2183  10.50000  0.05    0.55
Q11   1   0.8651  0.1593  0.4024  11.00000  0.05    0.55
Q12   1   0.1544  0.2500  0.4151  10.50000  0.05    0.55
Q13   1   0.6233  0.1534  0.1763  11.00000  0.05    0.54
Q14   1   0.1325  0.1972  0.4033  11.00000  0.05    0.54
Q15   1   0.3700  0.1400  0.7541  11.00000  0.05    0.53
Q16   1   0.8201  0.0483  0.3764  11.00000  0.05    0.53
Q17   1   0.7928 -0.0395  0.3372  11.00000  0.05    0.52
Q18   1   0.8800  0.5677  0.5141  11.00000  0.05    0.52
Q19   1   0.7180  0.2500  0.1974  10.50000  0.05    0.50
Q20   1   0.8649  0.5109  0.4871  11.00000  0.05    0.50
;
_shelx_res_checksum              77695
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.62800(3) 0.2500 0.24823(2) 0.03052(14) Uani 1 2 d S T P . .
I1 I 0.35744(6) 0.2500 0.41152(4) 0.03767(18) Uani 1 2 d S T P . .
I2 I 0.88768(4) 0.04804(4) 0.33939(3) 0.03391(15) Uani 1 1 d . . . . .
N1 N 0.7825(9) 0.2500 0.5277(5) 0.053(2) Uani 1 2 d S T P . .
H1 H 0.8611 0.2500 0.4881 0.064 Uiso 1 2 calc RS T P . .
C1 C 0.7248(8) 0.3609(8) 0.5567(5) 0.0529(19) Uani 1 1 d . . . . .
H1A H 0.7681 0.4380 0.5342 0.063 Uiso 1 1 calc R . . . .
C2 C 0.6046(7) 0.3635(7) 0.6182(5) 0.0419(15) Uani 1 1 d . . . . .
H2 H 0.5644 0.4423 0.6394 0.050 Uiso 1 1 calc R . . . .
C3 C 0.5401(9) 0.2500 0.6503(6) 0.0356(19) Uani 1 2 d S T P . .
C4 C 0.4060(10) 0.2500 0.7169(7) 0.045(2) Uani 1 2 d S T P . .
H4A H 0.4486 0.2908 0.7688 0.067 Uiso 0.5 1 calc GR . . A -1
H4B H 0.3734 0.1624 0.7299 0.067 Uiso 0.5 1 calc GR . . A -1
H4C H 0.3078 0.2967 0.6959 0.067 Uiso 0.5 1 calc GR . . A -1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.01702(19) 0.0396(2) 0.0349(2) 0.000 0.00000(10) 0.000
I1 0.0300(2) 0.0497(4) 0.0333(3) 0.000 -0.0047(2) 0.000
I2 0.0290(2) 0.0350(2) 0.0377(3) 0.00097(18) 0.00223(13) -0.00019(14)
N1 0.043(4) 0.090(8) 0.027(4) 0.000 0.010(3) 0.000
C1 0.055(3) 0.066(5) 0.037(4) -0.001(4) 0.003(3) -0.025(4)
C2 0.048(3) 0.039(4) 0.039(4) -0.003(3) -0.003(3) -0.010(3)
C3 0.030(4) 0.038(5) 0.039(5) 0.000 -0.010(3) 0.000
C4 0.032(4) 0.045(5) 0.057(7) 0.000 0.006(4) 0.000
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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0860
0 0 1 0.1010
0 -1 0 0.0300
0 1 0 0.0390
1 0 -1 0.0820
-1 0 1 0.1070
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 176.030(16) 6_656 .
I1 Pb1 I2 90.269(13) 6_656 6_556
I1 Pb1 I2 88.947(12) 6_656 .
I1 Pb1 I2 88.946(12) 6_656 8_565
I1 Pb1 I2 90.269(13) 6_656 3_455
I2 Pb1 I1 94.078(12) . .
I2 Pb1 I1 86.790(12) 6_556 .
I2 Pb1 I1 94.078(12) 8_565 .
I2 Pb1 I1 86.790(12) 3_455 .
I2 Pb1 I2 178.003(9) 6_556 8_565
I2 Pb1 I2 80.654(15) 8_565 .
I2 Pb1 I2 178.004(9) 3_455 .
I2 Pb1 I2 97.497(13) 3_455 8_565
I2 Pb1 I2 97.498(12) 6_556 .
I2 Pb1 I2 84.341(15) 6_556 3_455
Pb1 I1 Pb1 76.115(14) 6_556 .
Pb1 I2 Pb1 75.823(10) 6_656 .
C1 N1 H1 118.9 . .
C1 N1 H1 118.9 8_565 .
C1 N1 C1 122.2(8) 8_565 .
N1 C1 H1A 120.0 . .
N1 C1 C2 120.1(8) . .
C2 C1 H1A 120.0 . .
C1 C2 H2 120.1 . .
C1 C2 C3 119.8(7) . .
C3 C2 H2 120.1 . .
C2 C3 C2 118.1(8) 8_565 .
C2 C3 C4 120.9(4) . .
C2 C3 C4 120.9(4) 8_565 .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4B 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 I1 3.0956(6) 6_656
Pb1 I1 3.3408(6) .
Pb1 I2 3.2909(4) .
Pb1 I2 3.1723(4) 6_556
Pb1 I2 3.2909(4) 8_565
Pb1 I2 3.1723(4) 3_455
I1 Pb1 3.0956(6) 6_556
I2 Pb1 3.1724(4) 6_656
N1 H1 0.8800 .
N1 C1 1.335(9) .
N1 C1 1.335(9) 8_565
C1 H1A 0.9500 .
C1 C2 1.358(9) .
C2 H2 0.9500 .
C2 C3 1.396(8) .
C3 C2 1.396(8) 8_565
C3 C4 1.491(13) .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
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
_geom_torsion_site_symmetry_4
N1 C1 C2 C3 -0.7(11) . .
C1 N1 C1 C2 0.5(14) 8_565 .
C1 C2 C3 C2 0.9(12) . 8_565
C1 C2 C3 C4 -179.0(7) . .
