#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/74/2007480.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2007480
loop_
_publ_author_name
'Ragan, Colman'
'Jai-nhuknan, Jaran'
'Hughes, John M.'
'Cantrell, Joseph S.'
_publ_section_title
;
 Poly[[(2-fluorobenzoato)lead(II)-di-μ-thiourea-S:S]
 2-Fluorobenzoate Monohydrate]
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9800032
_journal_paper_doi               10.1107/S0108270198099570
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac
'[Pb (C7 H4 F1 O2) (C1 H4 N2 S1)2] (C7 H4 F1 O2), H2 O1'
_chemical_formula_moiety
;
C9 H12 F N4 O2 Pb S2 1+ , C7 H4 F O2 1- , H2 O
;
_chemical_formula_sum            'C16 H18 F2 N4 O5 Pb S2'
_chemical_formula_weight         655.65
_chemical_name_common
;
Lead(II)bis(2-fluorobenzoato)-bis(thiourea)monohydrate
;
_chemical_name_systematic
;
(catena-(bis(μ-thiourea-S,S)-2-fluorobenzoato)-lead(II))
2-fluorobenzoate - water (1/1)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                105.90(2)
_cell_angle_beta                 101.60(2)
_cell_angle_gamma                91.27(2)
_cell_formula_units_Z            2
_cell_length_a                   7.4060(10)
_cell_length_b                   12.386(2)
_cell_length_c                   12.409(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      46.09
_cell_measurement_theta_min      13.91
_cell_volume                     1068.8(4)
_computing_cell_refinement       'CAD-4 software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'SDP/PDP (Enraf-Nonius, 1985)'
_computing_molecular_graphics
;
XPMA and ZORTEP (Zsolnai & Huttner, 1994), and ORTEPIII (Burnett & Johnson,
1996)
;
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       θ/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.015
_diffrn_reflns_av_sigmaI/netI    0.032
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4660
_diffrn_reflns_theta_max         26.96
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        -0.7
_diffrn_standards_interval_time  240
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.141
_exptl_absorpt_correction_T_max  0.142
_exptl_absorpt_correction_T_min  0.073
_exptl_absorpt_correction_type   '\y scan (North et al., 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.037
_exptl_crystal_density_meas      2.04
_exptl_crystal_density_method    'flotation in CHBr~3~/CHCl~3~'
_exptl_crystal_description       block
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.304
_refine_diff_density_min         -1.633
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.997
_refine_ls_goodness_of_fit_obs   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4450
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_restrained_S_obs      1.002
_refine_ls_R_factor_all          0.042
_refine_ls_R_factor_obs          .035
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0373P)²+3.0856P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.080
_refine_ls_wR_factor_obs         .076
_reflns_number_observed          4044
_reflns_number_total             4450
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            qc0003.cif
_cod_data_source_block           qc0003
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (12
times).

'_geom_bond_publ_flag' value 'No' changed to 'no' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (23 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0373P)^2^+3.0856P] where P = (Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0373P)^2^+3.0856P] where P = (Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1068.8(3)
_cod_database_code               2007480
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
_atom_site_type_symbol
Pb .74721(3) .98569(2) .99037(2) .04491(9) Uani d . 1 . Pb
S1 .9929(2) .83631(11) 1.07184(11) .0371(3) Uani d . 1 . S
C1 .9218(7) .7123(4) .9636(5) .0348(11) Uani d . 1 . C
N1 .9204(8) .7066(4) .8562(4) .0495(12) Uani d . 1 . N
N2 .8654(8) .6225(4) .9874(4) .0500(12) Uani d . 1 . N
O1A .9510(5) 1.0915(3) 1.1855(3) .0427(9) Uani d . 1 . O
O2A .6779(5) 1.0137(3) 1.1785(3) .0402(9) Uani d . 1 . O
C7A .8309(8) 1.0670(4) 1.2352(4) .0350(11) Uani d . 1 . C
C1A .8692(8) 1.1014(4) 1.3631(5) .0375(12) Uani d . 1 . C
C2A .7702(9) 1.0601(5) 1.4270(5) .0464(14) Uani d . 1 . C
F2A .6257(7) .9831(4) 1.3750(4) .0856(15) Uani d . 1 . F
C3A .8086(11) 1.0918(6) 1.5447(6) .063(2) Uani d . 1 . C
H3A .7367(11) 1.0611(6) 1.5842(6) .064(8) Uiso calc R 1 . H
C4A .9540(11) 1.1689(6) 1.6029(6) .066(2) Uani d . 1 . C
H4A .9827(11) 1.1911(6) 1.6827(6) .064(8) Uiso calc R 1 . H
C5A 1.0588(12) 1.2141(6) 1.5429(6) .069(2) Uani d . 1 . C
H5A 1.1573(12) 1.2673(6) 1.5825(6) .064(8) Uiso calc R 1 . H
C6A 1.0180(10) 1.1807(5) 1.4251(5) .055(2) Uani d . 1 . C
H6A 1.0902(10) 1.2111(5) 1.3857(5) .064(8) Uiso calc R 1 . H
S2 .5542(2) 1.19548(11) 1.05501(11) .0354(3) Uani d . 1 . S
C2 .5519(7) 1.2574(4) .9459(5) .0352(11) Uani d . 1 . C
N3 .4798(7) 1.2039(4) .8376(4) .0485(12) Uani d . 1 . N
N4 .6225(7) 1.3622(4) .9704(4) .0479(12) Uani d . 1 . N
O1B .7948(8) .4559(4) .7758(4) .0692(14) Uani d . 1 . O
O2B .5086(8) .3757(5) .7298(5) .076(2) Uani d . 1 . O
C7B .6485(9) .4109(5) .7045(5) .0470(14) Uani d . 1 . C
C1B .6436(8) .3950(5) .5799(5) .0444(13) Uani d . 1 . C
C2B .7464(10) .4669(6) .5428(6) .054(2) Uani d . 1 . C
F2B .8540(8) .5564(4) .6213(4) .094(2) Uani d . 1 . F
C3B .7421(14) .4564(7) .4300(7) .080(3) Uani d . 1 . C
H3B .8117(14) .5074(7) .4088(7) .064(8) Uiso calc R 1 . H
C4B .6375(14) .3729(8) .3522(7) .083(3) Uani d . 1 . C
H4B .6352(14) .3652(8) .2752(7) .064(8) Uiso calc R 1 . H
C5B .5325(13) .2973(8) .3793(7) .084(3) Uani d . 1 . C
H5B .4601(13) .2390(8) .3218(7) .064(8) Uiso calc R 1 . H
C6B .5344(11) .3082(7) .4968(7) .070(2) Uani d . 1 . C
H6B .4628(11) .2574(7) .5170(7) .064(8) Uiso calc R 1 . H
O1W .8046(7) .5437(4) 1.1794(4) .0572(11) Uani d . 1 . O
H11 .9600 .7619 .8400 .090 Uiso d . 1 . H
H12 .9013 .6558 .7977 .090 Uiso d . 1 . H
H21 .8389 .5679 .9172 .090 Uiso d . 1 . H
H22 .8854 .6217 1.0573 .090 Uiso d . 1 . H
H31 .4160 1.1388 .8242 .090 Uiso d . 1 . H
H32 .4811 1.2322 .7844 .090 Uiso d . 1 . H
H41 .6939 1.3986 1.0364 .090 Uiso d . 1 . H
H42 .6185 1.3967 .9160 .090 Uiso d . 1 . H
H1 .7096 .5726 1.1965 .110 Uiso d . 1 . H
H2 .9219 .5515 1.2176 .110 Uiso d . 1 . H
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2A Pb O1A . . 52.17(12) yes
O2A Pb S1 . . 81.00(10) yes
O1A Pb S1 . . 70.47(9) yes
O2A Pb S2 . 2_677 77.87(9) yes
O1A Pb S2 . 2_677 126.83(9) yes
S1 Pb S2 . 2_677 86.55(4) yes
O2A Pb S2 . . 69.26(9) yes
O1A Pb S2 . . 78.05(9) yes
S1 Pb S2 . . 145.88(4) yes
S2 Pb S2 2_677 . 102.58(3) yes
O2A Pb S1 . 2_777 123.46(9) yes
O1A Pb S1 . 2_777 76.72(9) yes
S1 Pb S1 . 2_777 105.50(3) yes
S2 Pb S1 2_677 2_777 156.40(4) yes
S2 Pb S1 . 2_777 78.98(4) yes
C1 S1 Pb . . 100.6(2) no
N2 C1 N1 . . 118.7(5) no
N2 C1 S1 . . 120.3(4) no
N1 C1 S1 . . 121.0(4) no
C7A O1A Pb . . 90.2(3) no
C7A O2A Pb . . 96.4(3) no
O1A C7A O2A . . 121.1(5) no
O1A C7A C1A . . 119.3(5) no
O2A C7A C1A . . 119.6(5) no
C2A C1A C6A . . 116.0(5) no
C2A C1A C7A . . 124.7(5) no
C6A C1A C7A . . 119.3(5) no
F2A C2A C1A . . 120.2(5) no
F2A C2A C3A . . 115.8(6) no
C1A C2A C3A . . 124.0(6) no
C4A C3A C2A . . 118.9(7) no
C3A C4A C5A . . 119.8(6) no
C6A C5A C4A . . 120.2(7) no
C5A C6A C1A . . 121.2(7) no
C2 S2 Pb . 2_677 115.3(2) no
C2 S2 Pb . . 105.4(2) no
Pb S2 Pb 2_677 . 77.42(3) yes
N4 C2 N3 . . 118.1(5) no
N4 C2 S2 . . 119.7(4) no
N3 C2 S2 . . 122.2(4) no
O2B C7B O1B . . 124.6(6) no
O2B C7B C1B . . 117.3(6) no
O1B C7B C1B . . 118.0(6) no
C6B C1B C2B . . 117.0(6) no
C6B C1B C7B . . 121.0(7) no
C2B C1B C7B . . 122.0(6) no
C3B C2B F2B . . 116.8(7) no
C3B C2B C1B . . 123.5(7) no
F2B C2B C1B . . 119.7(6) no
C4B C3B C2B . . 118.5(9) no
C3B C4B C5B . . 122.7(8) no
C4B C5B C6B . . 119.3(8) no
C1B C6B C5B . . 119.0(8) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pb O2A . 2.424(4) yes
Pb O1A . 2.562(4) yes
Pb S1 . 2.862(2) yes
Pb S2 2_677 2.9859(15) yes
Pb S2 . 2.9871(15) yes
Pb S1 2_777 3.241(2) yes
Pb O1A 2_777 3.404(4) yes
Pb O2A 2_677 3.414(4) yes
S1 C1 . 1.729(5) yes
C1 N2 . 1.306(7) yes
C1 N1 . 1.314(7) yes
O1A C7A . 1.255(6) no
O2A C7A . 1.267(6) no
C7A C1A . 1.492(7) no
C1A C2A . 1.366(8) no
C1A C6A . 1.402(8) no
C2A F2A . 1.346(7) no
C2A C3A . 1.372(9) no
C3A C4A . 1.363(11) no
C4A C5A . 1.382(11) no
C5A C6A . 1.373(9) no
S2 C2 . 1.727(5) no
S2 Pb 2_677 2.9859(15) yes
C2 N4 . 1.318(7) no
C2 N3 . 1.319(7) no
O1B C7B . 1.259(8) no
O2B C7B . 1.244(8) no
C7B C1B . 1.497(8) no
C1B C6B . 1.376(9) no
C1B C2B . 1.385(9) no
C2B C3B . 1.363(10) no
C2B F2B . 1.367(8) no
C3B C4B . 1.311(13) no
C4B C5B . 1.356(13) no
C5B C6B . 1.424(12) no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N3 H31 F2A 2_677 0.883 2.472 2.947(6) 114.2
N3 H31 O2A 2_677 0.883 1.989 2.855(6) 166.3
N1 H11 O1A 2_777 0.829 2.043 2.869(6) 173.8
N2 H21 O1B . 0.925 1.878 2.801(7) 177.6
N2 H22 O1W . 0.853 2.173 2.917(7) 145.5
N4 H41 O1W 1_565 0.877 2.156 2.978(7) 155.8
N1 H12 F2B . 0.807 2.152 2.937(7) 164.8
N1 H12 O1B . 0.807 2.510 3.053(7) 126.0
N4 H42 O1B 1_565 0.890 2.613 3.393(7) 146.8
N4 H42 O2B 1_565 0.890 2.230 2.986(7) 142.7
O1W H2 O1B 2_767 0.892 2.089 2.906(8) 152.0
O1W H1 O2B 2_667 0.837 2.043 2.862(7) 165.5
