#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/84/2208477.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_2208477
loop_
_publ_author_name
'Hao-Long Xu'
'Han-Dong Yin'
'Gang Li'
_publ_section_title
;
 Aqua(2-chloronicotinato)triphenyltin(IV)
;
_journal_coeditor_code           AT2006
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m685
_journal_page_last               m686
_journal_paper_doi               10.1107/S160053680600626X
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Sn (C6 H5)3 (C6 H3 Cl N O2) (H2 O)]'
_chemical_formula_moiety         'C24 H20 Cl N O3 Sn'
_chemical_formula_sum            'C24 H20 Cl N O3 Sn'
_chemical_formula_weight         524.55
_chemical_melting_point          468.5(5)
_chemical_name_systematic
;
Aqua(2-chloronicotinato)triphenyltin(IV)
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.198(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.328(3)
_cell_length_b                   13.861(3)
_cell_length_c                   15.628(4)
_cell_measurement_reflns_used    4754
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.279
_cell_measurement_theta_min      2.289
_cell_volume                     2231.2(10)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11356
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.29
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.290
_exptl_absorpt_correction_T_max  0.6469
_exptl_absorpt_correction_T_min  0.5481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.410
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3938
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0479P)²+1.6414P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0908
_reflns_number_gt                3128
_reflns_number_total             3938
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            at2006.cif
_cod_data_source_block           I
_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:

'_chemical_melting_point' value '468-469' was changed to '468.5(5)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '468-469' was changed to '468.5(5)' -
the average value was taken and precision was
estimated.

'_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2208477
_cod_database_fobs_code          2208477
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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Sn Sn1 0.77593(3) 0.340855(18) 0.200520(16) 0.03313(12) Uani d . 1
Cl Cl1 1.08020(11) 0.15251(8) 0.02281(8) 0.0519(3) Uani d . 1
N N1 0.9610(4) 0.0852(3) -0.1153(2) 0.0518(10) Uani d . 1
O O1 0.8313(3) 0.25736(18) 0.08996(16) 0.0391(6) Uani d . 1
O O2 0.7428(3) 0.1226(2) 0.1357(2) 0.0535(8) Uani d . 1
O O3 0.7037(3) 0.4389(2) 0.31179(18) 0.0509(8) Uani d . 1
H H25 0.7299 0.4933 0.3244 0.061 Uiso d R 1
H H26 0.6307 0.4335 0.3332 0.061 Uiso d R 1
C C1 0.7973(4) 0.1691(3) 0.0819(3) 0.0370(9) Uani d . 1
C C2 0.9408(4) 0.1178(3) -0.0375(3) 0.0380(9) Uani d . 1
C C3 0.8210(4) 0.1231(3) -0.0029(2) 0.0364(9) Uani d . 1
C C4 0.7171(5) 0.0860(3) -0.0537(3) 0.0554(12) Uani d . 1
H H4 0.6349 0.0840 -0.0331 0.066 Uiso calc R 1
C C5 0.7359(6) 0.0519(4) -0.1350(3) 0.0706(15) Uani d . 1
H H5 0.6668 0.0275 -0.1700 0.085 Uiso calc R 1
C C6 0.8571(6) 0.0548(4) -0.1623(3) 0.0658(14) Uani d . 1
H H6 0.8682 0.0341 -0.2179 0.079 Uiso calc R 1
C C7 0.5736(4) 0.3266(3) 0.1685(3) 0.0410(10) Uani d . 1
C C8 0.5013(5) 0.2472(4) 0.1877(3) 0.0597(13) Uani d . 1
H H8 0.5416 0.1949 0.2158 0.072 Uiso calc R 1
C C9 0.3676(6) 0.2441(5) 0.1652(4) 0.0833(19) Uani d . 1
H H9 0.3184 0.1912 0.1798 0.100 Uiso calc R 1
C C10 0.3097(6) 0.3212(5) 0.1208(5) 0.096(2) Uani d . 1
H H10 0.2210 0.3198 0.1052 0.116 Uiso calc R 1
C C11 0.3813(6) 0.3989(5) 0.0997(4) 0.0813(19) Uani d . 1
H H11 0.3423 0.4495 0.0684 0.098 Uiso calc R 1
C C12 0.5103(5) 0.4021(4) 0.1245(3) 0.0575(13) Uani d . 1
H H12 0.5577 0.4566 0.1115 0.069 Uiso calc R 1
C C13 0.8702(4) 0.4651(3) 0.1538(3) 0.0382(9) Uani d . 1
C C14 0.8151(4) 0.5549(3) 0.1423(3) 0.0543(12) Uani d . 1
H H14 0.7294 0.5646 0.1549 0.065 Uiso calc R 1
C C15 0.8855(5) 0.6310(4) 0.1120(4) 0.0657(15) Uani d . 1
H H15 0.8466 0.6913 0.1051 0.079 Uiso calc R 1
C C16 1.0093(5) 0.6194(4) 0.0923(4) 0.0811(19) Uani d . 1
H H16 1.0546 0.6697 0.0689 0.097 Uiso calc R 1
C C17 1.0658(6) 0.5326(5) 0.1075(5) 0.108(2) Uani d U 1
H H17 1.1531 0.5245 0.0983 0.130 Uiso calc R 1
C C18 0.9961(5) 0.4555(4) 0.1365(5) 0.093(2) Uani d U 1
H H18 1.0365 0.3959 0.1443 0.112 Uiso calc R 1
C C19 0.9032(4) 0.2666(3) 0.2925(2) 0.0361(9) Uani d . 1
C C20 0.9013(4) 0.2818(3) 0.3798(3) 0.0465(11) Uani d . 1
H H20 0.8380 0.3215 0.4005 0.056 Uiso calc R 1
C C21 0.9923(5) 0.2387(4) 0.4367(3) 0.0588(13) Uani d . 1
H H21 0.9885 0.2487 0.4953 0.071 Uiso calc R 1
C C22 1.0876(5) 0.1819(4) 0.4081(3) 0.0606(13) Uani d . 1
H H22 1.1492 0.1540 0.4469 0.073 Uiso calc R 1
C C23 1.0921(5) 0.1660(3) 0.3215(3) 0.0622(14) Uani d . 1
H H23 1.1569 0.1273 0.3013 0.075 Uiso calc R 1
C C24 1.0001(5) 0.2076(3) 0.2646(3) 0.0521(12) Uani d . 1
H H24 1.0031 0.1959 0.2062 0.063 Uiso calc R 1
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'
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'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
C7 Sn1 C13 117.42(16) y
C7 Sn1 C19 131.29(16) y
C13 Sn1 C19 110.17(15) y
C7 Sn1 O1 94.27(13) y
C13 Sn1 O1 90.27(13) y
C19 Sn1 O1 95.33(13) y
C7 Sn1 O3 82.45(13) y
C13 Sn1 O3 87.95(13) y
C19 Sn1 O3 89.63(13) y
O1 Sn1 O3 175.03(10) y
C6 N1 C2 116.2(4) ?
C1 O1 Sn1 119.9(2) ?
Sn1 O3 H25 125.9 ?
Sn1 O3 H26 125.1 ?
H25 O3 H26 105.8 ?
O2 C1 O1 124.9(4) ?
O2 C1 C3 119.5(4) ?
O1 C1 C3 115.6(3) ?
N1 C2 C3 125.4(4) ?
N1 C2 Cl1 114.4(3) ?
C3 C2 Cl1 120.2(3) ?
C4 C3 C2 115.6(4) ?
C4 C3 C1 119.5(4) ?
C2 C3 C1 124.9(4) ?
C5 C4 C3 119.9(5) ?
C5 C4 H4 120.0 ?
C3 C4 H4 120.0 ?
C6 C5 C4 118.4(5) ?
C6 C5 H5 120.8 ?
C4 C5 H5 120.8 ?
N1 C6 C5 124.4(5) ?
N1 C6 H6 117.8 ?
C5 C6 H6 117.8 ?
C8 C7 C12 117.9(4) ?
C8 C7 Sn1 124.3(4) ?
C12 C7 Sn1 117.8(3) ?
C7 C8 C9 120.7(5) ?
C7 C8 H8 119.7 ?
C9 C8 H8 119.7 ?
C10 C9 C8 119.0(5) ?
C10 C9 H9 120.5 ?
C8 C9 H9 120.5 ?
C11 C10 C9 120.6(5) ?
C11 C10 H10 119.7 ?
C9 C10 H10 119.7 ?
C10 C11 C12 119.7(6) ?
C10 C11 H11 120.2 ?
C12 C11 H11 120.2 ?
C11 C12 C7 122.1(5) ?
C11 C12 H12 118.9 ?
C7 C12 H12 118.9 ?
C18 C13 C14 117.2(4) ?
C18 C13 Sn1 117.2(3) ?
C14 C13 Sn1 125.5(3) ?
C13 C14 C15 120.8(4) ?
C13 C14 H14 119.6 ?
C15 C14 H14 119.6 ?
C16 C15 C14 121.2(5) ?
C16 C15 H15 119.4 ?
C14 C15 H15 119.4 ?
C15 C16 C17 118.2(5) ?
C15 C16 H16 120.9 ?
C17 C16 H16 120.9 ?
C16 C17 C18 121.1(6) ?
C16 C17 H17 119.4 ?
C18 C17 H17 119.4 ?
C13 C18 C17 121.3(5) ?
C13 C18 H18 119.3 ?
C17 C18 H18 119.3 ?
C20 C19 C24 117.5(4) ?
C20 C19 Sn1 122.5(3) ?
C24 C19 Sn1 119.7(3) ?
C21 C20 C19 120.8(4) ?
C21 C20 H20 119.6 ?
C19 C20 H20 119.6 ?
C22 C21 C20 120.8(5) ?
C22 C21 H21 119.6 ?
C20 C21 H21 119.6 ?
C21 C22 C23 119.6(5) ?
C21 C22 H22 120.2 ?
C23 C22 H22 120.2 ?
C22 C23 C24 119.7(5) ?
C22 C23 H23 120.1 ?
C24 C23 H23 120.1 ?
C23 C24 C19 121.6(4) ?
C23 C24 H24 119.2 ?
C19 C24 H24 119.2 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Sn1 C7 2.122(4) y
Sn1 C13 2.133(4) y
Sn1 C19 2.139(4) y
Sn1 O1 2.190(3) y
Sn1 O3 2.370(3) y
Cl1 C2 1.730(4) ?
N1 C6 1.325(6) ?
N1 C2 1.328(5) ?
O1 C1 1.277(4) ?
O2 C1 1.228(5) ?
O3 H25 0.8203 ?
O3 H26 0.8503 ?
C1 C3 1.506(5) ?
C2 C3 1.389(6) ?
C3 C4 1.385(6) ?
C4 C5 1.382(7) ?
C4 H4 0.9300 ?
C5 C6 1.353(8) ?
C5 H5 0.9300 ?
C6 H6 0.9300 ?
C7 C8 1.376(6) ?
C7 C12 1.389(6) ?
C8 C9 1.400(7) ?
C8 H8 0.9300 ?
C9 C10 1.385(9) ?
C9 H9 0.9300 ?
C10 C11 1.361(9) ?
C10 H10 0.9300 ?
C11 C12 1.361(7) ?
C11 H11 0.9300 ?
C12 H12 0.9300 ?
C13 C18 1.354(6) ?
C13 C14 1.374(6) ?
C14 C15 1.385(6) ?
C14 H14 0.9300 ?
C15 C16 1.347(7) ?
C15 H15 0.9300 ?
C16 C17 1.351(8) ?
C16 H16 0.9300 ?
C17 C18 1.383(8) ?
C17 H17 0.9300 ?
C18 H18 0.9300 ?
C19 C20 1.382(5) ?
C19 C24 1.387(6) ?
C20 C21 1.382(6) ?
C20 H20 0.9300 ?
C21 C22 1.361(7) ?
C21 H21 0.9300 ?
C22 C23 1.376(7) ?
C22 H22 0.9300 ?
C23 C24 1.379(6) ?
C23 H23 0.9300 ?
C24 H24 0.9300 ?
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
_geom_hbond_publ_flag
O3 H25 O2 2_655 0.82 1.91 2.72(8) 168 yes
O3 H26 N1 4_566 0.85 1.99 2.84(8) 177 yes
