#------------------------------------------------------------------------------
#$Date: 2017-06-19 12:02:37 +0300 (Mon, 19 Jun 2017) $
#$Revision: 197922 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/00/74/2007490.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_2007490
loop_
_publ_author_name
'Ng, Seik Weng'
_publ_section_title
;
 Bis[2,2'-iminodipyridinium(1+)]
 Bis[μ-4-hydroxy-2,6-pyridinedicarboxylato(3
 --)]bis[aquadibutyltin(IV)] Dihydrate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              914
_journal_page_last               916
_journal_paper_doi               10.1107/S0108270198001322
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety
'(C10 H10 N3) [Sn (C7 H2 N O5) (C4 H9)2 (H2 O)] , H2 O'
_chemical_formula_sum            'C25 H34 N4 O7 Sn'
_chemical_formula_weight         621.25
_chemical_name_systematic
;
Bis[2,2'-iminodipyridinium(1+)]
bis[μ-4-hydroxy-2,6-pyridinedicarboxylato(3-)]bis[aquadibutyltin(IV)]
dihydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 99.030(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2260(10)
_cell_length_b                   15.164(2)
_cell_length_c                   18.868(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      13.0
_cell_measurement_theta_min      12.0
_cell_volume                     2607.0(5)
_computing_cell_refinement       'CELDIM in CAD-4 VAX/PC (Enraf Nonius, 1988)'
_computing_data_collection       'CAD-4/PC (Kretschmar, 1994)'
_computing_data_reduction        'XCAD4 (Harms, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_av_sigmaI/netI    0.030
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10063
_diffrn_reflns_theta_max         25.69
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.032
_exptl_absorpt_correction_T_max  0.822
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   '\y scan (North et al., 1968)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'Irregular block'
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.402
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.002
_refine_ls_goodness_of_fit_obs   1.040
_refine_ls_hydrogen_treatment
;
H atoms: see text
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         4724
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_restrained_S_obs      1.040
_refine_ls_R_factor_all          0.040
_refine_ls_R_factor_obs          .028
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0384P)²+1.1434P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.072
_refine_ls_wR_factor_obs         .067
_reflns_number_observed          3854
_reflns_number_total             4724
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ta1200.cif
_cod_data_source_block           ta1200
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

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

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'Not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0384P)^2^+1.1434P] 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^)+(0.0384P)^2^+1.1434P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

2017-05-31
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C50 H68 N8 O14 Sn2'
_cod_original_formula_weight         1242.50
_cod_original_formula_moiety
'(C10 H10 N3)2 [Sn2 (C7 H2 N O5)2 (C4 H9)4 (H2 O)2] , 2H2 O'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        2606.9(5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2007490
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Sn1 .06557(2) .136700(10) .025680(10) .03060(8) Uani d . 1 . Sn
O1 .0655(2) -.00130(10) .07620(10) .0328(4) Uani d . 1 . O
O2 .1142(3) -.07690(10) .17700(10) .0523(6) Uani d . 1 . O
O3 .1233(3) .26950(10) .05280(10) .0410(5) Uani d . 1 . O
O4 .2029(3) .36420(10) .13760(10) .0544(6) Uani d . 1 . O
O5 .3552(3) .1545(2) .34950(10) .0502(6) Uani d . 1 . O
O6 -.0026(3) .2046(2) -.09020(10) .0408(6) Uani d . 1 . O
H61 -.028(4) .172(3) -.115(2) .050 Uiso d . 1 . H
H62 -.051(4) .253(3) -.108(2) .050 Uiso d . 1 . H
O7 .3595(4) .0272(3) .4447(2) .0870(10) Uani d . 1 . O
H71 .371(4) .062(3) .413(2) .050 Uiso d . 1 . H
H72 .390(4) .072(3) .477(2) .050 Uiso d . 1 . H
N1 .1593(3) .1409(2) .14020(10) .0295(5) Uani d . 1 . N
N2 .1322(5) .1016(3) .5081(2) .0830(10) Uani d . 1 . N
H2 .2097(5) .0955(3) .4886(2) .124 Uiso calc R 1 . H
N3 -.1200(4) .1127(2) .4878(2) .0569(8) Uani d . 1 . N
N4 .0428(4) .1175(2) .6129(2) .0675(9) Uani d . 1 . N
C1 .2490(3) .0933(2) -.0193(2) .0369(7) Uani d . 1 . C
H1A .3153(3) .0645(2) .0187(2) .055 Uiso calc R 1 . H
H1B .2144(3) .0482(2) -.0543(2) .055 Uiso calc R 1 . H
C2 .3384(4) .1569(2) -.0548(2) .0428(8) Uani d . 1 . C
H2A .3860(4) .1978(2) -.0190(2) .064 Uiso calc R 1 . H
H2B .2730(4) .1908(2) -.0899(2) .064 Uiso calc R 1 . H
C3 .4544(4) .1142(2) -.0918(2) .0474(8) Uani d . 1 . C
H3A .5197(4) .0806(2) -.0565(2) .071 Uiso calc R 1 . H
H3B .4064(4) .0728(2) -.1271(2) .071 Uiso calc R 1 . H
C4 .5444(5) .1757(3) -.1283(2) .0700(10) Uani d . 1 . C
H4A .6140(5) .1427(3) -.1504(2) .105 Uiso calc R 1 . H
H4B .5956(5) .2158(3) -.0938(2) .105 Uiso calc R 1 . H
H4C .4815(5) .2084(3) -.1644(2) .105 Uiso calc R 1 . H
C5 -.1588(3) .1498(2) .0345(2) .0383(7) Uani d . 1 . C
H5A -.1911(3) .2079(2) .0171(2) .057 Uiso calc R 1 . H
H5B -.2137(3) .1070(2) .0028(2) .057 Uiso calc R 1 . H
C6 -.1987(3) .1382(2) .1084(2) .0422(7) Uani d . 1 . C
H6A -.1523(3) .1843(2) .1397(2) .063 Uiso calc R 1 . H
H6B -.1613(3) .0820(2) .1279(2) .063 Uiso calc R 1 . H
C7 -.3638(4) .1415(3) .1076(2) .0550(9) Uani d . 1 . C
H7A -.4001(4) .1985(3) .0895(2) .082 Uiso calc R 1 . H
H7B -.4100(4) .0969(3) .0747(2) .082 Uiso calc R 1 . H
C8 -.4079(5) .1268(3) .1797(2) .0770(10) Uani d . 1 . C
H8A -.5129(5) .1295(3) .1755(2) .116 Uiso calc R 1 . H
H8B -.3649(5) .1717(3) .2123(2) .116 Uiso calc R 1 . H
H8C -.3743(5) .0699(3) .1976(2) .116 Uiso calc R 1 . H
C9 .1145(3) -.0101(2) .1425(2) .0317(6) Uani d . 1 . C
C10 .1754(3) .0702(2) .1811(2) .0292(6) Uani d . 1 . C
C11 .2399(3) .0720(2) .2520(2) .0346(7) Uani d . 1 . C
H11 .2493(3) .0200(2) .2784(2) .052 Uiso calc R 1 . H
C12 .2912(3) .1509(2) .2846(2) .0352(7) Uani d . 1 . C
C13 .2639(3) .2253(2) .2405(2) .0353(7) Uani d . 1 . C
H13 .2882(3) .2809(2) .2594(2) .053 Uiso calc R 1 . H
C14 .2018(3) .2171(2) .1699(2) .0305(6) Uani d . 1 . C
C15 .1747(3) .2906(2) .1176(2) .0360(7) Uani d . 1 . C
C16 .0058(4) .1013(2) .4589(2) .0534(9) Uani d . 1 . C
C17 -.0003(5) .0935(3) .3862(2) .0670(10) Uani d . 1 . C
H17 .0853(5) .0850(3) .3669(2) .100 Uiso calc R 1 . H
C18 -.1302(5) .0981(3) .3430(2) .0690(10) Uani d . 1 . C
H18 -.1346(5) .0937(3) .2935(2) .103 Uiso calc R 1 . H
C19 -.2591(5) .1097(3) .3724(2) .0630(10) Uani d . 1 . C
H19 -.3498(5) .1128(3) .3429(2) .095 Uiso calc R 1 . H
C20 -.2496(5) .1161(2) .4439(2) .0560(10) Uani d . 1 . C
H20 -.3351(5) .1232(2) .4636(2) .083 Uiso calc R 1 . H
C21 .1629(5) .1092(2) .5808(2) .0590(10) Uani d . 1 . C
C22 .3046(5) .1091(3) .6174(3) .0760(10) Uani d . 1 . C
H22 .3848(5) .1042(3) .5933(3) .114 Uiso calc R 1 . H
C23 .3227(6) .1165(3) .6897(3) .090(2) Uani d . 1 . C
H23 .4165(6) .1165(3) .7162(3) .135 Uiso calc R 1 . H
C24 .2017(7) .1240(3) .7239(3) .094(2) Uani d . 1 . C
H24 .2136(7) .1292(3) .7736(3) .141 Uiso calc R 1 . H
C25 .0633(6) .1238(3) .6840(2) .0780(10) Uani d . 1 . C
H25 -.0179(6) .1280(3) .7074(2) .116 Uiso calc R 1 . H
H34 -.071(4) .107(2) .560(2) .050 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'
Sn Sn -0.6537 1.4246 '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
C1 Sn1 C5 . . 156.60(10) yes
C1 Sn1 N1 . . 100.80(10) yes
C1 Sn1 O1 . . 86.30(10) yes
C1 Sn1 O1 . 3 78.10(10) yes
C1 Sn1 O3 . . 101.80(10) yes
C1 Sn1 O6 . . 83.10(10) yes
C5 Sn1 N1 . . 99.20(10) yes
C5 Sn1 O1 . . 89.40(10) yes
C5 Sn1 O1 . 3 79.00(10) yes
C5 Sn1 O3 . . 95.90(10) yes
C5 Sn1 O6 . . 84.90(10) yes
N1 Sn1 O1 . . 69.20(10) yes
N1 Sn1 O1 . 3 136.10(10) yes
N1 Sn1 O6 . . 152.40(10) yes
N1 Sn1 O3 . . 72.00(10) yes
O1 Sn1 O1 . 3 66.90(10) yes
O1 Sn1 O3 . . 141.20(10) yes
O1 Sn1 O6 . . 138.40(10) yes
O1 Sn1 O3 3 . 151.80(10) yes
O1 Sn1 O6 3 . 71.50(10) yes
O3 Sn1 O6 . . 80.40(10) yes
C9 O1 Sn1 . . 118.7(2) ?
C15 O3 Sn1 . . 120.5(2) ?
C14 N1 C10 . . 117.7(2) ?
C14 N1 Sn1 . . 119.3(2) ?
C10 N1 Sn1 . . 123.0(2) ?
C21 N2 C16 . . 134.7(4) ?
C20 N3 C16 . . 119.2(3) ?
C25 N4 C21 . . 117.6(4) ?
C2 C1 Sn1 . . 120.8(2) ?
C1 C2 C3 . . 114.2(3) ?
C4 C3 C2 . . 115.5(3) ?
C6 C5 Sn1 . . 116.5(2) ?
C5 C6 C7 . . 112.0(3) ?
C8 C7 C6 . . 113.6(3) ?
O2 C9 O1 . . 126.1(3) ?
O2 C9 C10 . . 117.3(2) ?
O1 C9 C10 . . 116.6(2) ?
N1 C10 C11 . . 123.1(3) ?
N1 C10 C9 . . 112.4(2) ?
C11 C10 C9 . . 124.5(3) ?
C10 C11 C12 . . 120.8(3) ?
O5 C12 C11 . . 122.3(3) ?
O5 C12 C13 . . 123.4(3) ?
C11 C12 C13 . . 114.3(3) ?
C14 C13 C12 . . 120.9(3) ?
N1 C14 C13 . . 123.0(3) ?
N1 C14 C15 . . 111.5(2) ?
C13 C14 C15 . . 125.4(3) ?
O4 C15 O3 . . 124.4(3) ?
O4 C15 C14 . . 119.1(3) ?
O3 C15 C14 . . 116.5(3) ?
N2 C16 N3 . . 114.5(4) ?
N2 C16 C17 . . 125.1(4) ?
N3 C16 C17 . . 120.4(4) ?
C18 C17 C16 . . 119.8(4) ?
C17 C18 C19 . . 119.9(4) ?
C20 C19 C18 . . 118.8(4) ?
C19 C20 N3 . . 121.9(4) ?
N4 C21 N2 . . 113.8(4) ?
N4 C21 C22 . . 123.8(4) ?
N2 C21 C22 . . 122.4(4) ?
C23 C22 C21 . . 117.5(5) ?
C22 C23 C24 . . 119.9(5) ?
C23 C24 C25 . . 119.5(5) ?
N4 C25 C24 . . 121.7(5) ?
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
Sn1 C1 . 2.114(3) yes
Sn1 C5 . 2.112(3) yes
Sn1 N1 . 2.198(2) yes
Sn1 O1 . 2.299(2) yes
Sn1 O1 3 2.939(2) yes
Sn1 O3 . 2.125(2) yes
Sn1 O6 . 2.409(2) yes
O1 C9 . 1.270(3) ?
O2 C9 . 1.205(3) ?
O3 C15 . 1.280(4) ?
O4 C15 . 1.195(4) ?
O5 C12 . 1.274(4) ?
N1 C14 . 1.316(3) ?
N1 C10 . 1.316(3) ?
N2 C21 . 1.361(6) ?
N2 C16 . 1.372(6) ?
N3 C20 . 1.345(5) ?
N3 C16 . 1.369(5) ?
N4 C25 . 1.328(6) ?
N4 C21 . 1.349(6) ?
C1 C2 . 1.494(4) ?
C2 C3 . 1.512(5) ?
C3 C4 . 1.488(5) ?
C5 C6 . 1.508(4) ?
C6 C7 . 1.521(5) ?
C7 C8 . 1.498(5) ?
C9 C10 . 1.483(4) ?
C10 C11 . 1.376(4) ?
C11 C12 . 1.394(4) ?
C12 C13 . 1.400(4) ?
C13 C14 . 1.370(4) ?
C14 C15 . 1.484(4) ?
C16 C17 . 1.370(6) ?
C17 C18 . 1.342(6) ?
C18 C19 . 1.400(6) ?
C19 C20 . 1.342(6) ?
C21 C22 . 1.379(6) ?
C22 C23 . 1.352(7) ?
C23 C24 . 1.379(8) ?
C24 C25 . 1.377(7) ?
O5 O7 . 2.633(4) ?
O7 N2 . 2.810(5) ?
O7 O7 3_656 3.172(8) ?
O7 O4 2_545 2.927(5) ?
