#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/47/2014714.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_2014714
loop_
_publ_author_name
'M. Enriqueta Díaz de Vivar'
'Sergio Baggio'
'Muõz, Juan Carlos'
'Ricardo Baggio'
_publ_section_title
;Di-μ-sulfito-bis[(4,4'-dimethyl-2,2'-bipyridine)zinc(II)] dihydrate and
 poly[[aqua(1,10-phenanthroline)zinc(II)]-μ₃-sulfito-zinc(II)-μ₃-sulfito]
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m30
_journal_page_last               m33
_journal_paper_doi               10.1107/S0108270104029865
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Zn2 (S O3)2 (C12 H12 N2)], 2H2 O'
_chemical_formula_moiety         'C24 H24 N4 O6 S2 Zn2, 2H2 O'
_chemical_formula_sum            'C24 H28 N4 O8 S2 Zn2'
_chemical_formula_weight         695.36
_chemical_name_systematic
;
di-μ-sulfito-κ³O,O':O'';κ³O:O',O''-bis[(4,4'-dimethyl-2,2'-bipyridine-
κ²N,N')zinc(II)] dihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                113.233(8)
_cell_angle_beta                 96.932(9)
_cell_angle_gamma                106.746(9)
_cell_formula_units_Z            1
_cell_length_a                   7.534(4)
_cell_length_b                   9.621(5)
_cell_length_c                   11.051(5)
_cell_measurement_reflns_used    273
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.45
_cell_measurement_theta_min      4.02
_cell_volume                     679.4(6)
_computing_cell_refinement       'SAINT-NT (Bruker, 2000)'
_computing_data_collection       'SMART-NT (Bruker, 2001)'
_computing_data_reduction        SAINT-NT
_computing_molecular_graphics    'XP in SHELXTL-PC (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.740
_diffrn_measured_fraction_theta_max 0.644
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_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     0.71070
_diffrn_reflns_av_R_equivalents  0.079
_diffrn_reflns_av_sigmaI/netI    0.042
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2037
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.60
_diffrn_reflns_theta_min         2.08
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.975
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[SADABS (Sheldrick, 1996) in SAINT-NT (Bruker, 2000)]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.947
_refine_diff_density_min         -1.296
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2037
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0639
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1397P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1765
_refine_ls_wR_factor_ref         0.1820
_reflns_number_gt                1623
_reflns_number_total             2037
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ob1207.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P_-1
_cod_database_code               2014714
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_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Zn1 0.57473(9) 0.72053(8) 0.51318(8) 0.0329(3) Uani d . 1 . . Zn
S1 0.2636(2) 0.5645(2) 0.5775(2) 0.0426(5) Uani d . 1 . . S
O1 0.2433(6) 0.3882(5) 0.5324(6) 0.0444(13) Uani d . 1 . . O
O2 0.2877(6) 0.5956(6) 0.4537(5) 0.0465(13) Uani d . 1 . . O
O3 0.4638(7) 0.6687(6) 0.6720(6) 0.0530(14) Uani d . 1 . . O
N1 0.5933(7) 0.8282(6) 0.3794(6) 0.0326(12) Uani d . 1 . . N
N2 0.7506(7) 0.9559(6) 0.6438(6) 0.0340(12) Uani d . 1 . . N
C1 0.5070(9) 0.7535(8) 0.2435(7) 0.0411(17) Uani d . 1 . . C
H1 0.4134 0.6495 0.2049 0.049 Uiso calc R 1 . . H
C2 0.5531(9) 0.8261(8) 0.1609(7) 0.0395(16) Uani d . 1 . . C
H2 0.4917 0.7717 0.0679 0.047 Uiso calc R 1 . . H
C3 0.6921(8) 0.9812(8) 0.2173(7) 0.0356(15) Uani d . 1 . . C
C4 0.7788(8) 1.0570(7) 0.3549(6) 0.0289(13) Uani d . 1 . . C
H4 0.8734 1.1607 0.3950 0.035 Uiso calc R 1 . . H
C5 0.7249(8) 0.9785(7) 0.4350(7) 0.0276(13) Uani d . 1 . . C
C6 0.8084(7) 1.0543(7) 0.5838(7) 0.0294(14) Uani d . 1 . . C
C7 0.9384(8) 1.2139(7) 0.6608(7) 0.0324(14) Uani d . 1 . . C
H7 0.9761 1.2794 0.6181 0.039 Uiso calc R 1 . . H
C8 1.0115(8) 1.2754(7) 0.7989(7) 0.0358(15) Uani d . 1 . . C
C9 0.9502(9) 1.1742(8) 0.8575(7) 0.0386(16) Uani d . 1 . . C
H9 0.9974 1.2119 0.9509 0.046 Uiso calc R 1 . . H
C10 0.8212(9) 1.0196(8) 0.7802(7) 0.0403(17) Uani d . 1 . . C
H10 0.7799 0.9550 0.8232 0.048 Uiso calc R 1 . . H
C11 0.7470(11) 1.0632(10) 0.1271(8) 0.0514(19) Uani d . 1 . . C
H11A 0.6412 1.0876 0.0950 0.077 Uiso calc R 1 . . H
H11B 0.7773 0.9915 0.0505 0.077 Uiso calc R 1 . . H
H11C 0.8570 1.1621 0.1790 0.077 Uiso calc R 1 . . H
C12 1.1555(10) 1.4472(8) 0.8816(8) 0.0473(18) Uani d . 1 . . C
H12A 1.0891 1.5192 0.9185 0.071 Uiso calc R 1 . . H
H12B 1.2252 1.4795 0.8240 0.071 Uiso calc R 1 . . H
H12C 1.2436 1.4522 0.9550 0.071 Uiso calc R 1 . . H
O1W 0.2283(12) 0.3627(9) 0.1817(8) 0.081(2) Uani d D 1 . . O
H1WB 0.315(9) 0.332(9) 0.200(6) 0.06(3) Uiso d D 1 . . H
H1WA 0.215(10) 0.428(7) 0.251(4) 0.04(2) Uiso d 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'
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
O1 Zn1 O2 2_666 . 121.9(2) y
O1 Zn1 N2 2_666 . 102.8(2) y
O2 Zn1 N2 . . 134.7(2) y
O1 Zn1 N1 2_666 . 99.3(2) y
O2 Zn1 N1 . . 99.28(19) y
N2 Zn1 N1 . . 78.6(2) y
O1 Zn1 O3 2_666 . 107.4(2) y
O2 Zn1 O3 . . 66.9(2) y
N2 Zn1 O3 . . 94.9(2) y
N1 Zn1 O3 . . 153.3(2) y
O3 S1 O1 . . 106.8(3) no
O3 S1 O2 . . 99.8(3) no
O1 S1 O2 . . 105.5(3) no
O3 S1 Zn1 . . 53.4(2) ?
O1 S1 Zn1 . . 109.56(18) ?
O2 S1 Zn1 . . 46.85(17) ?
S1 O1 Zn1 . 2_666 131.6(3) ?
S1 O2 Zn1 . . 99.6(2) ?
S1 O3 Zn1 . . 93.0(3) ?
C5 N1 C1 . . 118.8(5) ?
C5 N1 Zn1 . . 113.7(4) ?
C1 N1 Zn1 . . 126.8(4) ?
C10 N2 C6 . . 117.5(5) ?
C10 N2 Zn1 . . 126.8(4) ?
C6 N2 Zn1 . . 115.5(4) ?
N1 C1 C2 . . 122.3(6) ?
N1 C1 H1 . . 118.9 ?
C2 C1 H1 . . 118.9 ?
C1 C2 C3 . . 119.3(6) ?
C1 C2 H2 . . 120.3 ?
C3 C2 H2 . . 120.3 ?
C4 C3 C2 . . 118.4(6) ?
C4 C3 C11 . . 121.4(6) ?
C2 C3 C11 . . 120.2(6) ?
C3 C4 C5 . . 120.0(5) ?
C3 C4 H4 . . 120.0 ?
C5 C4 H4 . . 120.0 ?
N1 C5 C4 . . 121.1(6) ?
N1 C5 C6 . . 116.0(5) ?
C4 C5 C6 . . 122.9(5) ?
N2 C6 C7 . . 120.9(6) ?
N2 C6 C5 . . 115.0(5) ?
C7 C6 C5 . . 124.1(6) ?
C8 C7 C6 . . 120.7(6) ?
C8 C7 H7 . . 119.6 ?
C6 C7 H7 . . 119.6 ?
C7 C8 C9 . . 117.4(6) ?
C7 C8 C12 . . 120.6(6) ?
C9 C8 C12 . . 122.0(6) ?
C10 C9 C8 . . 120.6(6) ?
C10 C9 H9 . . 119.7 ?
C8 C9 H9 . . 119.7 ?
N2 C10 C9 . . 122.8(6) ?
N2 C10 H10 . . 118.6 ?
C9 C10 H10 . . 118.6 ?
C3 C11 H11A . . 109.5 ?
C3 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
C3 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C8 C12 H12A . . 109.5 ?
C8 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
C8 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
H1WB O1W H1WA . . 111(3) ?
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 O1 2_666 1.951(4) y
Zn1 O2 . 2.022(4) y
Zn1 N2 . 2.049(5) y
Zn1 N1 . 2.110(5) y
Zn1 O3 . 2.198(5) y
S1 O3 . 1.514(5) y
S1 O1 . 1.522(5) y
S1 O2 . 1.532(5) y
N1 C5 . 1.333(7) ?
N1 C1 . 1.356(9) ?
N2 C10 . 1.349(9) ?
N2 C6 . 1.361(8) ?
C1 C2 . 1.371(9) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.385(8) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.371(9) ?
C3 C11 . 1.523(9) ?
C4 C5 . 1.399(8) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.474(9) ?
C6 C7 . 1.394(8) ?
C7 C8 . 1.371(9) ?
C7 H7 . 0.9300 ?
C8 C9 . 1.375(9) ?
C8 C12 . 1.510(9) ?
C9 C10 . 1.361(9) ?
C9 H9 . 0.9300 ?
C10 H10 . 0.9300 ?
C11 H11A . 0.9600 ?
C11 H11B . 0.9600 ?
C11 H11C . 0.9600 ?
C12 H12A . 0.9600 ?
C12 H12B . 0.9600 ?
C12 H12C . 0.9600 ?
O1W H1WB . 0.83(8) ?
O1W H1WA . 0.82(5) ?
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
O1W H1WB O3 2_666 0.83(8) 2.06(7) 2.823(10) 155(6)
O1W H1WA O2 . 0.82(5) 2.07(6) 2.835(10) 157(6)
C7 H7 O1 1_665 0.93 2.46 3.247(7) 142
C9 H9 O1W 1_666 0.93 2.49 3.374(9) 159
