#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:38:02 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179539 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/08/4500896.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_4500896
loop_
_publ_author_name
'Croitor, Lilia'
'Coropceanu, Eduard B.'
'Siminel, Anatolii V.'
'Kravtsov, Victor Ch.'
'Fonari, Marina S.'
_publ_section_title
;
 Polymeric Zn(II) and Cd(II) Sulfates with Bipyridine and Dioxime Ligands:
 Supramolecular Isomerism, Chirality, and Luminescence
;
_journal_issue                   8
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3536
_journal_paper_doi               10.1021/cg200465f
_journal_volume                  11
_journal_year                    2011
_chemical_formula_moiety         'C18 H22 N4 O6 S Zn'
_chemical_formula_sum            'C18 H22 N4 O6 S Zn'
_chemical_formula_weight         487.83
_chemical_name_common
; 
 (mu2-1,2-bis(4-pyridyl)-ethane)-
(1,2-cyclohexanedione dioxime)-(sulfato-zinc(II)) 
;
_chemical_name_systematic
; 
 (mu2-1,2-bis(4-pyridyl)-ethane)-
(1,2-cyclohexanedione dioxime)-(sulfato-zinc(II)) 
;
_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                 91.317(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8002(8)
_cell_length_b                   9.3425(9)
_cell_length_c                   23.470(4)
_cell_measurement_reflns_used    1419
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6702
_cell_measurement_theta_min      2.9912
_cell_volume                     2148.3(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1687
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            5641
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    1.282
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79355
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.849
_refine_diff_density_min         -1.486
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0769
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0813P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1692
_refine_ls_wR_factor_ref         0.1832
_reflns_number_gt                3442
_reflns_number_total             5772
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg200465f_si_001.cif
_cod_data_source_block           cl_379_zn6_twin1_hklf5
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4500896
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_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 1.23545(10) 0.51208(8) 0.18366(4) 0.0235(3) Uani 1 1 d . . .
S1 S 1.0716(2) 0.7477(2) 0.26557(10) 0.0254(5) Uani 1 1 d . . .
O1 O 1.3934(8) 0.3340(8) 0.0805(3) 0.069(3) Uani 1 1 d . . .
H1 H 1.4196 0.2922 0.1095 0.104 Uiso 1 1 calc R . .
O2 O 1.0218(8) 0.7408(6) 0.1196(3) 0.054(2) Uani 1 1 d . . .
H2 H 1.0000 0.7460 0.1530 0.080 Uiso 1 1 calc R . .
O3 O 1.1597(6) 0.6266(5) 0.2504(2) 0.0284(16) Uani 1 1 d . . .
O4 O 0.9554(5) 0.7517(6) 0.2241(3) 0.0325(15) Uani 1 1 d . . .
O5 O 1.0227(6) 0.7264(5) 0.3235(3) 0.0288(15) Uani 1 1 d . . .
O6 O 1.1498(6) 0.8826(5) 0.2630(3) 0.0292(15) Uani 1 1 d . . .
N1 N 1.3034(7) 0.4360(7) 0.0943(3) 0.0263(18) Uani 1 1 d . . .
N2 N 1.1157(7) 0.6381(7) 0.1139(3) 0.0257(18) Uani 1 1 d . . .
N3 N 1.0783(7) 0.3544(6) 0.1785(3) 0.0186(16) Uani 1 1 d . . .
N4 N 0.4023(7) -0.3439(6) 0.1728(3) 0.0264(19) Uani 1 1 d . . .
C1 C 1.2548(9) 0.5093(10) 0.0509(3) 0.036(2) Uani 1 1 d . B .
C2 C 1.1584(10) 0.6206(11) 0.0628(4) 0.042(3) Uani 1 1 d . B .
C3 C 1.1053(15) 0.7169(12) 0.0163(5) 0.068(4) Uani 1 1 d . . .
H3A H 1.0076 0.7272 0.0204 0.082 Uiso 0.50 1 calc PR A 1
H3B H 1.1459 0.8108 0.0216 0.082 Uiso 0.50 1 calc PR A 1
H3C H 1.0147 0.6862 0.0042 0.082 Uiso 0.50 1 calc PR A 2
H3D H 1.0990 0.8141 0.0305 0.082 Uiso 0.50 1 calc PR A 2
C4A C 1.131(4) 0.669(5) -0.0426(13) 0.077(15) Uani 0.50 1 d P B 1
H4A1 H 1.0640 0.5975 -0.0535 0.095 Uiso 0.50 1 calc PR B 1
H4A2 H 1.1196 0.7499 -0.0682 0.095 Uiso 0.50 1 calc PR B 1
C5A C 1.252(7) 0.616(3) -0.049(2) 0.083(14) Uani 0.50 1 d P B 1
H5A1 H 1.3178 0.6925 -0.0435 0.099 Uiso 0.50 1 calc PR B 1
H5A2 H 1.2584 0.5836 -0.0881 0.099 Uiso 0.50 1 calc PR B 1
C4B C 1.194(6) 0.713(5) -0.031(2) 0.077(15) Uani 0.50 1 d P B 2
H4B1 H 1.2792 0.7608 -0.0208 0.130 Uiso 0.50 1 calc PR B 2
H4B2 H 1.1525 0.7651 -0.0627 0.130 Uiso 0.50 1 calc PR B 2
C5B C 1.228(6) 0.551(3) -0.0518(15) 0.068(16) Uani 0.50 1 d P B 2
H5B1 H 1.1441 0.5000 -0.0612 0.082 Uiso 0.50 1 calc PR B 2
H5B2 H 1.2843 0.5525 -0.0852 0.082 Uiso 0.50 1 calc PR B 2
C6 C 1.2958(15) 0.4847(17) -0.0075(4) 0.095(5) Uani 1 1 d . . .
H6A H 1.2539 0.3971 -0.0215 0.114 Uiso 0.50 1 calc PR B 1
H6B H 1.3940 0.4725 -0.0081 0.114 Uiso 0.50 1 calc PR B 1
H6C H 1.3912 0.5113 -0.0096 0.114 Uiso 0.50 1 calc PR B 2
H6D H 1.2907 0.3824 -0.0143 0.114 Uiso 0.50 1 calc PR B 2
C7 C 1.1000(10) 0.2236(10) 0.1632(4) 0.038(3) Uani 1 1 d . . .
H7 H 1.1856 0.2003 0.1497 0.046 Uiso 1 1 calc R . .
C8 C 1.0015(9) 0.1146(9) 0.1659(4) 0.033(3) Uani 1 1 d . . .
H8 H 1.0228 0.0219 0.1548 0.040 Uiso 1 1 calc R . .
C9 C 0.8771(8) 0.1451(8) 0.1844(4) 0.0224(19) Uani 1 1 d . . .
C10 C 0.8444(8) 0.2834(8) 0.1965(4) 0.029(2) Uani 1 1 d . . .
H10 H 0.7556 0.3083 0.2055 0.035 Uiso 1 1 calc R . .
C11 C 0.9493(8) 0.3888(8) 0.1953(4) 0.026(2) Uani 1 1 d . . .
H11 H 0.9300 0.4824 0.2059 0.032 Uiso 1 1 calc R . .
C12 C 0.7684(8) 0.0274(8) 0.1895(4) 0.032(2) Uani 1 1 d . . .
H12A H 0.6893 0.0688 0.2073 0.038 Uiso 1 1 calc R . .
H12B H 0.8043 -0.0459 0.2149 0.038 Uiso 1 1 calc R . .
C13 C 0.7197(10) -0.0461(8) 0.1333(4) 0.045(3) Uani 1 1 d . . .
H13A H 0.6861 0.0258 0.1067 0.054 Uiso 1 1 calc R . .
H13B H 0.7961 -0.0946 0.1162 0.054 Uiso 1 1 calc R . .
C14 C 0.6082(10) -0.1527(9) 0.1445(4) 0.035(2) Uani 1 1 d . . .
C15 C 0.6328(9) -0.2926(9) 0.1560(4) 0.042(3) Uani 1 1 d . . .
H15 H 0.7221 -0.3259 0.1550 0.050 Uiso 1 1 calc R . .
C16 C 0.5327(9) -0.3855(9) 0.1690(4) 0.034(3) Uani 1 1 d . . .
H16 H 0.5548 -0.4811 0.1754 0.041 Uiso 1 1 calc R . .
C17 C 0.3768(9) -0.2037(8) 0.1651(4) 0.032(3) Uani 1 1 d . . .
H17 H 0.2874 -0.1722 0.1688 0.039 Uiso 1 1 calc R . .
C18 C 0.4732(9) -0.1054(8) 0.1522(4) 0.034(3) Uani 1 1 d . . .
H18 H 0.4507 -0.0091 0.1485 0.041 Uiso 1 1 calc R . .
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O3 Zn1 O6 92.5(2) . 2_745
O3 Zn1 N3 97.5(2) . .
O6 Zn1 N3 90.7(2) 2_745 .
O3 Zn1 N4 93.1(2) . 1_665
O6 Zn1 N4 92.0(2) 2_745 1_665
N3 Zn1 N4 169.0(2) . 1_665
O3 Zn1 N2 95.1(2) . .
O6 Zn1 N2 172.3(3) 2_745 .
N3 Zn1 N2 87.6(2) . .
N4 Zn1 N2 88.4(2) 1_665 .
O3 Zn1 N1 164.7(2) . .
O6 Zn1 N1 101.9(2) 2_745 .
N3 Zn1 N1 87.7(2) . .
N4 Zn1 N1 81.3(2) 1_665 .
N2 Zn1 N1 70.6(3) . .
O5 S1 O3 109.0(3) . .
O5 S1 O6 109.6(3) . .
O3 S1 O6 109.8(3) . .
O5 S1 O4 110.5(4) . .
O3 S1 O4 107.9(3) . .
O6 S1 O4 110.0(3) . .
N1 O1 H1 109.5 . .
N2 O2 H2 109.5 . .
S1 O3 Zn1 144.2(4) . .
S1 O6 Zn1 138.9(4) . 2_755
C1 N1 O1 114.4(8) . .
C1 N1 Zn1 115.8(5) . .
O1 N1 Zn1 129.6(6) . .
C2 N2 O2 115.0(8) . .
C2 N2 Zn1 115.0(7) . .
O2 N2 Zn1 129.2(6) . .
C7 N3 C11 117.4(7) . .
C7 N3 Zn1 123.1(6) . .
C11 N3 Zn1 119.4(5) . .
C16 N4 C17 116.6(7) . .
C16 N4 Zn1 123.9(5) . 1_445
C17 N4 Zn1 119.3(6) . 1_445
N1 C1 C2 117.2(8) . .
N1 C1 C6 123.2(9) . .
C2 C1 C6 119.7(9) . .
N2 C2 C1 120.1(9) . .
N2 C2 C3 119.1(10) . .
C1 C2 C3 120.8(10) . .
C4B C3 C4A 31(2) . .
C4B C3 C2 110(2) . .
C4A C3 C2 115.8(19) . .
C4B C3 H3A 134.5 . .
C4A C3 H3A 108.3 . .
C2 C3 H3A 108.3 . .
C4B C3 H3B 82.4 . .
C4A C3 H3B 108.3 . .
C2 C3 H3B 108.3 . .
H3A C3 H3B 107.4 . .
C4B C3 H3C 109.6 . .
C4A C3 H3C 79.3 . .
C2 C3 H3C 109.6 . .
H3A C3 H3C 32.7 . .
H3B C3 H3C 132.4 . .
C4B C3 H3D 109.6 . .
C4A C3 H3D 128.1 . .
C2 C3 H3D 109.6 . .
H3A C3 H3D 78.5 . .
H3B C3 H3D 30.4 . .
H3C C3 H3D 108.2 . .
C5A C4A C3 114(3) . .
C5A C4A H4A1 108.8 . .
C3 C4A H4A1 108.8 . .
C5A C4A H4A2 108.8 . .
C3 C4A H4A2 108.8 . .
H4A1 C4A H4A2 107.7 . .
C4A C5A C6 117(4) . .
C4A C5A H5A1 108.1 . .
C6 C5A H5A1 108.1 . .
C4A C5A H5A2 108.1 . .
C6 C5A H5A2 108.1 . .
H5A1 C5A H5A2 107.3 . .
C3 C4B C5B 113(3) . .
C3 C4B H4B1 109.1 . .
C5B C4B H4B1 109.0 . .
C3 C4B H4B2 109.1 . .
C5B C4B H4B2 109.0 . .
H4B1 C4B H4B2 107.8 . .
C6 C5B C4B 107(3) . .
C6 C5B H5B1 110.3 . .
C4B C5B H5B1 110.3 . .
C6 C5B H5B2 110.3 . .
C4B C5B H5B2 110.3 . .
H5B1 C5B H5B2 108.6 . .
C5B C6 C1 120(2) . .
C5B C6 C5A 24(3) . .
C1 C6 C5A 111.8(19) . .
C5B C6 H6A 85.8 . .
C1 C6 H6A 109.3 . .
C5A C6 H6A 109.3 . .
C5B C6 H6B 120.4 . .
C1 C6 H6B 109.3 . .
C5A C6 H6B 109.3 . .
H6A C6 H6B 107.9 . .
C5B C6 H6C 107.2 . .
C1 C6 H6C 107.2 . .
C5A C6 H6C 91.0 . .
H6A C6 H6C 126.8 . .
H6B C6 H6C 21.7 . .
C5B C6 H6D 107.3 . .
C1 C6 H6D 107.2 . .
C5A C6 H6D 129.4 . .
H6A C6 H6D 24.9 . .
H6B C6 H6D 85.9 . .
H6C C6 H6D 106.9 . .
N3 C7 C8 123.7(9) . .
N3 C7 H7 118.2 . .
C8 C7 H7 118.2 . .
C9 C8 C7 119.6(8) . .
C9 C8 H8 120.2 . .
C7 C8 H8 120.2 . .
C8 C9 C10 119.4(7) . .
C8 C9 C12 120.9(7) . .
C10 C9 C12 119.6(7) . .
C9 C10 C11 118.5(7) . .
C9 C10 H10 120.7 . .
C11 C10 H10 120.7 . .
N3 C11 C10 120.9(7) . .
N3 C11 H11 119.5 . .
C10 C11 H11 119.5 . .
C9 C12 C13 116.8(7) . .
C9 C12 H12A 108.1 . .
C13 C12 H12A 108.1 . .
C9 C12 H12B 108.1 . .
C13 C12 H12B 108.1 . .
H12A C12 H12B 107.3 . .
C14 C13 C12 110.8(7) . .
C14 C13 H13A 109.5 . .
C12 C13 H13A 109.5 . .
C14 C13 H13B 109.5 . .
C12 C13 H13B 109.5 . .
H13A C13 H13B 108.1 . .
C15 C14 C18 116.0(8) . .
C15 C14 C13 123.1(9) . .
C18 C14 C13 120.1(8) . .
C16 C15 C14 122.6(9) . .
C16 C15 H15 118.7 . .
C14 C15 H15 118.7 . .
N4 C16 C15 121.8(8) . .
N4 C16 H16 119.1 . .
C15 C16 H16 119.1 . .
N4 C17 C18 124.1(8) . .
N4 C17 H17 117.9 . .
C18 C17 H17 117.9 . .
C17 C18 C14 118.5(8) . .
C17 C18 H18 120.8 . .
C14 C18 H18 120.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O3 2.050(5) .
Zn1 O6 2.057(6) 2_745
Zn1 N3 2.133(6) .
Zn1 N4 2.137(7) 1_665
Zn1 N2 2.315(7) .
Zn1 N1 2.326(7) .
S1 O5 1.466(6) .
S1 O3 1.472(5) .
S1 O6 1.477(6) .
S1 O4 1.481(6) .
O1 N1 1.343(8) .
O1 H1 0.8200 .
O2 N2 1.338(9) .
O2 H2 0.8200 .
O6 Zn1 2.057(6) 2_755
N1 C1 1.308(10) .
N2 C2 1.289(12) .
N3 C7 1.293(10) .
N3 C11 1.371(10) .
N4 C16 1.341(10) .
N4 C17 1.344(9) .
N4 Zn1 2.137(7) 1_445
C1 C2 1.436(13) .
C1 C6 1.455(12) .
C2 C3 1.499(14) .
C3 C4B 1.43(6) .
C3 C4A 1.48(4) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C3 H3C 0.9700 .
C3 H3D 0.9700 .
C4A C5A 1.29(7) .
C4A H4A1 0.9700 .
C4A H4A2 0.9700 .
C5A C6 1.62(4) .
C5A H5A1 0.9700 .
C5A H5A2 0.9700 .
C4B C5B 1.63(6) .
C4B H4B1 0.9700 .
C4B H4B2 0.9700 .
C5B C6 1.37(4) .
C5B H5B1 0.9700 .
C5B H5B2 0.9700 .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C6 H6C 0.9700 .
C6 H6D 0.9700 .
C7 C8 1.405(11) .
C7 H7 0.9300 .
C8 C9 1.334(11) .
C8 H8 0.9300 .
C9 C10 1.363(10) .
C9 C12 1.538(10) .
C10 C11 1.425(10) .
C10 H10 0.9300 .
C11 H11 0.9300 .
C12 C13 1.552(11) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C13 C14 1.506(11) .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C14 C15 1.355(12) .
C14 C18 1.411(12) .
C15 C16 1.349(11) .
C15 H15 0.9300 .
C16 H16 0.9300 .
C17 C18 1.357(11) .
C17 H17 0.9300 .
C18 H18 0.9300 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O5 0.82 1.77 2.584(9) 171.8 2_745
O2 H2 O4 0.82 1.74 2.555(10) 178.3 .
