#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/52/2225289.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_2225289
loop_
_publ_author_name
'Xie, Bu-Yun'
'Huang, Wei'
'Zhang, Ying'
'Yang, Rui-Qing'
'Xie, Yong-Rong'
_publ_section_title
;
 Pentaaqua(acetonitrile-κN)zinc(II)
 4,6-dihydroxybenzene-1,3-disulfonate trihydrate
;
_journal_coeditor_code           HY2283
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m341
_journal_paper_doi               10.1107/S1600536810006525
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Zn (C2 H3 N) (H2 O)5] (C6 H4 O8 S2), 3H2 O'
_chemical_formula_moiety         'C2 H13 N O5 Zn 2+, C6 H4 O8 S2 2-, 3(H2 O)'
_chemical_formula_sum            'C8 H23 N O16 S2 Zn'
_chemical_formula_weight         518.80
_chemical_name_systematic
;Pentaaqua(acetonitrile-κN)zinc(II)
 4,6-dihydroxybenzene-1,3-disulfonate
trihydrate
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8731(10)
_cell_length_b                   6.9972(6)
_cell_length_c                   22.9980(17)
_cell_measurement_reflns_used    2210
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      2.37
_cell_volume                     2071.6(3)
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Mercury2 CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            10992
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    1.462
_exptl_absorpt_correction_T_max  0.790
_exptl_absorpt_correction_T_min  0.661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.433
_refine_ls_extinction_coef       0.0021(5)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0371
_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)+(0.0457P)²+0.7072P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                1891
_reflns_number_total             2581
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hy2283.cif
_cod_data_source_block           I
_cod_database_code               2225289
_cod_database_fobs_code          2225289
loop_
_symmetry_equiv_pos_as_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_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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn Zn1 0.05196(4) 0.2500 0.648181(17) 0.04642(16) Uani d S 1 . .
O O1W 0.1416(2) 0.0416(4) 0.60984(10) 0.0831(8) Uani d . 1 . .
H H1WB 0.1599 -0.0361 0.6336 0.117(17) Uiso d R 1 . .
H H1WA 0.1627 0.0469 0.5736 0.17(2) Uiso d R 1 . .
O O2W -0.04689(16) 0.0412(3) 0.68120(8) 0.0615(6) Uani d . 1 . .
H H2WB -0.0611 -0.0355 0.6555 0.075(11) Uiso d R 1 . .
H H2WA -0.0580 -0.0096 0.7164 0.122(16) Uiso d R 1 . .
O O3W -0.0392(2) 0.2500 0.57265(12) 0.0579(8) Uani d S 1 . .
H H3WA -0.0285 0.3485 0.5542 0.15(2) Uiso d R 1 . .
N N1 0.1330(3) 0.2500 0.72832(15) 0.0672(11) Uani d S 1 . .
C C7 0.2069(4) 0.2500 0.8316(2) 0.0734(14) Uani d S 1 . .
H H7A 0.1782 0.1343 0.8467 0.17(2) Uiso d R 1 . .
H H7B 0.2756 0.2500 0.8350 0.11(2) Uiso d SR 1 . .
C C8 0.1698(4) 0.2500 0.7727(2) 0.0621(12) Uani d S 1 . .
S S1 0.49094(8) 0.2500 0.30660(3) 0.0414(2) Uani d S 1 . .
S S2 0.15787(7) 0.2500 0.44987(3) 0.0375(2) Uani d S 1 . .
O O1 0.4012(2) 0.2500 0.26982(10) 0.0735(10) Uani d S 1 . .
O O2 0.55305(17) 0.0800(3) 0.29897(8) 0.0669(6) Uani d . 1 . .
O O3 0.13088(14) 0.0779(3) 0.48192(7) 0.0494(5) Uani d . 1 . .
O O4 0.11538(19) 0.2500 0.39111(10) 0.0464(6) Uani d S 1 . .
O O5 0.6117(2) 0.2500 0.41697(10) 0.0594(8) Uani d S 1 . .
H H5 0.6426 0.2500 0.4482 0.044(11) Uiso d SR 1 . .
O O6 0.3153(2) 0.2500 0.54301(9) 0.0527(7) Uani d S 1 . .
H H6 0.3605 0.2500 0.5681 0.086(17) Uiso d SR 1 . .
C C1 0.5087(3) 0.2500 0.42656(13) 0.0394(8) Uani d S 1 . .
C C3 0.3602(3) 0.2500 0.48999(13) 0.0359(8) Uani d S 1 . .
C C4 0.2939(3) 0.2500 0.44165(13) 0.0351(8) Uani d S 1 . .
C C2 0.4660(3) 0.2500 0.48202(13) 0.0407(9) Uani d S 1 . .
H H2 0.5097 0.2500 0.5142 0.047(10) Uiso calc SR 1 . .
C C5 0.3365(3) 0.2500 0.38655(13) 0.0349(8) Uani d S 1 . .
H H5A 0.2929 0.2500 0.3543 0.028(8) Uiso calc SR 1 . .
C C6 0.4421(3) 0.2500 0.37869(13) 0.0357(8) Uani d S 1 . .
O O4W 0.4428(2) 0.2500 0.62998(12) 0.0598(8) Uani d S 1 . .
H H4WA 0.4421 0.1514 0.6522 0.108(16) Uiso d R 1 . .
O O5W 0.7285(2) 0.2500 0.51114(13) 0.0664(8) Uani d S 1 . .
H H5WA 0.7607 0.1441 0.5160 0.108(16) Uiso d R 1 . .
O O6W 0.2208(2) 0.7500 0.67248(12) 0.0559(7) Uani d S 1 . .
H H6WB 0.2849 0.7500 0.6800 0.12(2) Uiso d SR 1 . .
H H6WA 0.1983 0.7500 0.7077 0.092(18) Uiso d SR 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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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
O1W Zn1 O1W . 8_565 90.26(14) ?
O1W Zn1 O2W . 8_565 175.32(9) ?
O1W Zn1 O2W 8_565 8_565 90.09(10) ?
O1W Zn1 O2W . . 90.09(10) ?
O1W Zn1 O2W 8_565 . 175.32(9) ?
O2W Zn1 O2W 8_565 . 89.19(12) ?
O1W Zn1 O3W . . 87.63(9) ?
O1W Zn1 O3W 8_565 . 87.63(9) ?
O2W Zn1 O3W 8_565 . 87.72(8) ?
O2W Zn1 O3W . . 87.72(8) ?
O1W Zn1 N1 . . 95.54(10) ?
O1W Zn1 N1 8_565 . 95.54(10) ?
O2W Zn1 N1 8_565 . 89.07(9) ?
O2W Zn1 N1 . . 89.07(9) ?
O3W Zn1 N1 . . 175.50(13) ?
Zn1 O1W H1WB . . 110.5 ?
Zn1 O1W H1WA . . 123.4 ?
H1WB O1W H1WA . . 125.6 ?
Zn1 O2W H2WB . . 109.4 ?
Zn1 O2W H2WA . . 134.9 ?
H2WB O2W H2WA . . 110.9 ?
Zn1 O3W H3WA . . 109.5 ?
C8 N1 Zn1 . . 175.3(4) ?
C8 C7 H7A . . 102.4 ?
C8 C7 H7B . . 114.5 ?
H7A C7 H7B . . 110.7 ?
N1 C8 C7 . . 174.6(6) ?
O1 S1 O2 . 8_565 112.01(11) ?
O1 S1 O2 . . 112.01(11) ?
O2 S1 O2 8_565 . 110.9(2) ?
O1 S1 C6 . . 105.47(16) ?
O2 S1 C6 8_565 . 108.06(10) ?
O2 S1 C6 . . 108.06(10) ?
O3 S2 O3 8_565 . 111.83(16) ?
O3 S2 O3 8_565 1 111.83(16) ?
O3 S2 O4 8_565 . 112.35(9) ?
O3 S2 O4 . . 112.35(9) ?
O3 S2 O4 1 . 112.35(9) ?
O3 S2 C4 8_565 . 106.98(10) ?
O3 S2 C4 . . 106.98(10) ?
O3 S2 C4 1 . 106.98(10) ?
O4 S2 C4 . . 105.87(15) ?
C1 O5 H5 . . 109.6 ?
C3 O6 H6 . . 109.5 ?
O5 C1 C2 . . 122.7(3) ?
O5 C1 C6 . . 118.4(3) ?
C2 C1 C6 . . 118.8(3) ?
O6 C3 C2 1 . 123.0(3) ?
O6 C3 C2 . . 123.0(3) ?
O6 C3 C4 1 . 117.2(3) ?
O6 C3 C4 . . 117.2(3) ?
C2 C3 C4 . . 119.8(3) ?
C5 C4 C3 . . 119.1(3) ?
C5 C4 S2 . . 119.6(2) ?
C3 C4 S2 . . 121.3(2) ?
C3 C2 C1 . . 120.9(3) ?
C3 C2 H2 . . 119.5 ?
C1 C2 H2 . . 119.5 ?
C6 C5 C4 . . 121.0(3) ?
C6 C5 H5A . . 119.5 ?
C4 C5 H5A . . 119.5 ?
C5 C6 C1 . . 120.3(3) ?
C5 C6 S1 . . 118.3(2) ?
C1 C6 S1 . . 121.4(3) ?
H6WB O6W H6WA . . 97.8 ?
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
Zn1 O1W . 2.058(2) ?
Zn1 O2W . 2.081(2) ?
Zn1 O3W . 2.096(3) ?
Zn1 N1 . 2.118(3) ?
O1W H1WB . 0.8063 ?
O1W H1WA . 0.8769 ?
O2W H2WB . 0.8197 ?
O2W H2WA . 0.8948 ?
O3W H3WA . 0.8204 ?
N1 C8 . 1.126(5) ?
C7 C8 . 1.435(6) ?
C7 H7A . 0.9553 ?
C7 H7B . 0.8878 ?
S1 O1 . 1.432(3) ?
S1 O2 8_565 1.444(2) ?
S1 O2 . 1.444(2) ?
S1 C6 . 1.773(3) ?
S2 O3 8_565 1.4541(19) ?
S2 O3 . 1.4541(19) ?
S2 O3 1 1.4541(19) ?
S2 O4 . 1.458(2) ?
S2 C4 . 1.762(4) ?
O5 C1 . 1.344(4) ?
O5 H5 . 0.8206 ?
O6 C3 . 1.349(4) ?
O6 H6 . 0.8201 ?
C1 C2 . 1.389(4) ?
C1 C6 . 1.395(4) ?
C3 O6 1 1.349(4) ?
C3 C2 . 1.375(5) ?
C3 C4 . 1.402(4) ?
C4 C5 . 1.381(4) ?
C2 H2 . 0.9300 ?
C5 C6 . 1.371(5) ?
C5 H5A . 0.9300 ?
O4W H4WA . 0.8585 ?
O5W H5WA . 0.8563 ?
O6W H6WB . 0.8433 ?
O6W H6WA . 0.8611 ?
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
O5 H5 O5W 1 0.82 1.82 2.636(4) 172 y
O6 H6 O4W 1 0.82 1.77 2.587(4) 172 y
O1W H1WA O3 1 0.88 2.16 2.956(3) 151 y
O1W H1WA O6 1 0.88 2.53 3.081(3) 122 y
O1W H1WB O6W 1_545 0.81 1.91 2.698(3) 165 y
O2W H2WA O2 2 0.89 1.96 2.839(3) 166 y
O2W H2WB O4 5_556 0.82 1.97 2.774(3) 166 y
O3W H3WA O3 4_556 0.82 2.24 2.869(2) 134 y
O4W H4WA O2 5_656 0.86 1.97 2.829(3) 177 y
O5W H5WA O3 5_656 0.86 2.09 2.927(3) 166 y
O6W H6WA O1 2_565 0.86 1.92 2.734(4) 158 y
O6W H6WB O2 5_666 0.84 2.45 3.213(4) 151 y
