#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/32/2013279.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_2013279
loop_
_publ_author_name
'Miguel Harvey'
'Sergio Baggio'
'Silvia Russi'
'Ricardo Baggio'
_publ_section_title
;
 Two new dimeric cadmium(II) and zinc(II) sulfate complexes with
 2,4,6-tris(2-pyridyl)-1,3,5-triazine and 2,2:6',2''-terpyridine
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m171
_journal_page_last               m174
_journal_paper_doi               10.1107/S0108270103006462
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Cd2 (S O4)2 (C15 H11 N3)2], 2H2 O'
_chemical_formula_moiety         'C30 H22 N6 O8 S2 Zn2, 2H2 O'
_chemical_formula_sum            'C30 H26 N6 O10 S2 Zn2'
_chemical_formula_weight         825.43
_chemical_name_systematic
;
di-μ-sulfato-κ²O:O'-bis[(2,2':6',2''-terpyridine-
κ³N¹,N^1'^,N^1''^)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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                110.34(2)
_cell_angle_beta                 116.59(2)
_cell_angle_gamma                98.83(2)
_cell_formula_units_Z            1
_cell_length_a                   9.700(2)
_cell_length_b                   9.755(2)
_cell_length_c                   10.324(2)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7.5
_cell_volume                     761.4(4)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software (Molecular Structure
Corporation, 1988)
;
_computing_data_reduction        'MSC/AFC Diffractometer Control Software'
_computing_molecular_graphics    'XP in SHELXTL/PC (Sheldrick, 1994)'
_computing_publication_material  'XP in SHELXTL/PC'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device       'Rigaku AFC-7S'
_diffrn_measurement_method       ω/2θ
_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  0.039
_diffrn_reflns_av_sigmaI/netI    0.084
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4216
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.40
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.785
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details
'(MSC/AFC Diffractometer Control Software; Molecular Structure Corp, 1988)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.354
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.848
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         2890
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.848
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0178P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0728
_reflns_number_gt                2008
_reflns_number_total             2890
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ga1011.cif
_cod_data_source_block           II
_cod_database_code               2013279
_cod_database_fobs_code          2013279
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
Zn 0.76317(5) 0.85637(5) 0.90932(5) 0.03576(15) Uani d . 1 . . Zn
S 1.07896(11) 1.02598(11) 1.26397(12) 0.0368(2) Uani d . 1 . . S
O1 0.9204(3) 0.8918(3) 1.1321(3) 0.0613(8) Uani d . 1 . . O
O2 1.0570(3) 1.1164(3) 1.3913(3) 0.0640(8) Uani d . 1 . . O
O3 1.2096(3) 0.9697(3) 1.3206(4) 0.0722(9) Uani d . 1 . . O
O4 1.1123(3) 1.1279(3) 1.1934(3) 0.0431(7) Uani d . 1 . . O
N1 0.7047(3) 0.6013(3) 0.8129(4) 0.0379(8) Uani d . 1 . . N
N2 0.6833(3) 1.0545(4) 0.9480(4) 0.0388(8) Uani d . 1 . . N
N3 0.5075(3) 0.7529(3) 0.7496(3) 0.0340(7) Uani d . 1 . . N
C1 0.8151(5) 0.5312(5) 0.8482(5) 0.0472(11) Uani d . 1 . . C
H1A 0.9260 0.5939 0.9286 0.057 Uiso calc R 1 . . H
C2 0.7722(5) 0.3712(5) 0.7711(5) 0.0497(11) Uani d . 1 . . C
H2A 0.8521 0.3264 0.7978 0.060 Uiso calc R 1 . . H
C3 0.6085(5) 0.2790(5) 0.6538(5) 0.0488(11) Uani d . 1 . . C
H3A 0.5760 0.1702 0.6002 0.059 Uiso calc R 1 . . H
C4 0.4921(5) 0.3477(4) 0.6155(5) 0.0437(10) Uani d . 1 . . C
H4A 0.3804 0.2866 0.5372 0.052 Uiso calc R 1 . . H
C5 0.5458(4) 0.5102(4) 0.6965(4) 0.0334(9) Uani d . 1 . . C
C6 0.4318(4) 0.5967(4) 0.6603(4) 0.0338(9) Uani d . 1 . . C
C7 0.2630(4) 0.5270(5) 0.5452(4) 0.0442(10) Uani d . 1 . . C
H7A 0.2107 0.4181 0.4844 0.053 Uiso calc R 1 . . H
C8 0.1744(5) 0.6239(5) 0.5230(5) 0.0521(11) Uani d . 1 . . C
H8A 0.0612 0.5802 0.4440 0.063 Uiso calc R 1 . . H
C9 0.2521(4) 0.7834(5) 0.6163(5) 0.0486(11) Uani d . 1 . . C
H9A 0.1918 0.8483 0.6023 0.058 Uiso calc R 1 . . H
C10 0.4199(4) 0.8476(5) 0.7310(5) 0.0394(9) Uani d . 1 . . C
C11 0.5197(5) 1.0156(5) 0.8442(5) 0.0396(9) Uani d . 1 . . C
C12 0.4499(5) 1.1292(5) 0.8477(5) 0.0520(11) Uani d . 1 . . C
H12A 0.3371 1.1020 0.7756 0.062 Uiso calc R 1 . . H
C13 0.5517(6) 1.2840(5) 0.9610(5) 0.0565(12) Uani d . 1 . . C
H13A 0.5069 1.3620 0.9653 0.068 Uiso calc R 1 . . H
C14 0.7174(5) 1.3244(5) 1.0669(5) 0.0541(11) Uani d . 1 . . C
H14A 0.7865 1.4284 1.1440 0.065 Uiso calc R 1 . . H
C15 0.7781(5) 1.2044(5) 1.0550(5) 0.0487(11) Uani d . 1 . . C
H15A 0.8909 1.2300 1.1254 0.058 Uiso calc R 1 . . H
O1W 0.8391(4) 0.7034(3) 0.2766(4) 0.0644(10) Uani d D 1 . . O
H1WA 0.858(5) 0.757(4) 0.367(4) 0.077 Uiso d D 1 . . H
H1WB 0.879(5) 0.757(4) 0.249(5) 0.077 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
O4 Zn O1 2_777 . 107.54(10)
O4 Zn N3 2_777 . 115.24(11)
O1 Zn N3 . . 134.66(11)
O4 Zn N2 2_777 . 107.83(10)
O1 Zn N2 . . 104.58(12)
N3 Zn N2 . . 76.52(12)
O4 Zn N1 2_777 . 91.75(10)
O1 Zn N1 . . 90.39(11)
N3 Zn N1 . . 74.44(11)
N2 Zn N1 . . 149.88(11)
O3 S O2 . . 112.92(19)
O3 S O1 . . 109.95(17)
O2 S O1 . . 108.10(17)
O3 S O4 . . 110.37(16)
O2 S O4 . . 107.69(16)
O1 S O4 . . 107.63(15)
S O1 Zn . . 128.49(16)
S O4 Zn . 2_777 135.32(15)
C5 N1 C1 . . 118.1(3)
C5 N1 Zn . . 115.7(2)
C1 N1 Zn . . 125.9(2)
C15 N2 C11 . . 119.1(3)
C15 N2 Zn . . 127.0(3)
C11 N2 Zn . . 113.8(3)
C6 N3 C10 . . 120.6(3)
C6 N3 Zn . . 120.9(2)
C10 N3 Zn . . 118.4(2)
N1 C1 C2 . . 123.0(4)
N1 C1 H1A . . 118.5
C2 C1 H1A . . 118.5
C3 C2 C1 . . 118.4(4)
C3 C2 H2A . . 120.8
C1 C2 H2A . . 120.8
C2 C3 C4 . . 119.9(4)
C2 C3 H3A . . 120.0
C4 C3 H3A . . 120.0
C3 C4 C5 . . 118.2(4)
C3 C4 H4A . . 120.9
C5 C4 H4A . . 120.9
N1 C5 C4 . . 122.4(3)
N1 C5 C6 . . 114.9(3)
C4 C5 C6 . . 122.7(3)
N3 C6 C7 . . 121.3(4)
N3 C6 C5 . . 113.7(3)
C7 C6 C5 . . 124.9(3)
C8 C7 C6 . . 118.0(4)
C8 C7 H7A . . 121.0
C6 C7 H7A . . 121.0
C9 C8 C7 . . 120.4(4)
C9 C8 H8A . . 119.8
C7 C8 H8A . . 119.8
C8 C9 C10 . . 119.6(4)
C8 C9 H9A . . 120.2
C10 C9 H9A . . 120.2
N3 C10 C9 . . 120.0(4)
N3 C10 C11 . . 113.9(3)
C9 C10 C11 . . 126.1(4)
N2 C11 C12 . . 121.1(4)
N2 C11 C10 . . 116.8(3)
C12 C11 C10 . . 122.0(4)
C13 C12 C11 . . 118.3(4)
C13 C12 H12A . . 120.8
C11 C12 H12A . . 120.8
C14 C13 C12 . . 120.9(4)
C14 C13 H13A . . 119.5
C12 C13 H13A . . 119.5
C13 C14 C15 . . 117.3(4)
C13 C14 H14A . . 121.3
C15 C14 H14A . . 121.3
N2 C15 C14 . . 123.1(4)
N2 C15 H15A . . 118.4
C14 C15 H15A . . 118.4
H1WA O1W H1WB . . 110(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
Zn O4 2_777 1.952(2) y
Zn O1 . 1.970(3) y
Zn N3 . 2.074(3) y
Zn N2 . 2.166(3) y
Zn N1 . 2.201(3) y
S O3 . 1.422(3) y
S O2 . 1.434(3) y
S O1 . 1.483(3) y
S O4 . 1.496(2) y
O4 Zn 2_777 1.952(2) ?
N1 C5 . 1.337(4) ?
N1 C1 . 1.340(4) ?
N2 C15 . 1.327(4) ?
N2 C11 . 1.350(4) ?
N3 C6 . 1.336(4) ?
N3 C10 . 1.353(4) ?
C1 C2 . 1.373(5) ?
C1 H1A . 0.9300 ?
C2 C3 . 1.371(5) ?
C2 H2A . 0.9300 ?
C3 C4 . 1.377(5) ?
C3 H3A . 0.9300 ?
C4 C5 . 1.385(5) ?
C4 H4A . 0.9300 ?
C5 C6 . 1.487(4) ?
C6 C7 . 1.382(4) ?
C7 C8 . 1.381(5) ?
C7 H7A . 0.9300 ?
C8 C9 . 1.366(5) ?
C8 H8A . 0.9300 ?
C9 C10 . 1.375(5) ?
C9 H9A . 0.9300 ?
C10 C11 . 1.469(5) ?
C11 C12 . 1.383(5) ?
C12 C13 . 1.379(5) ?
C12 H12A . 0.9300 ?
C13 C14 . 1.367(5) ?
C13 H13A . 0.9300 ?
C14 C15 . 1.381(5) ?
C14 H14A . 0.9300 ?
C15 H15A . 0.9300 ?
O1W H1WA . 0.81(3) ?
O1W H1WB . 0.81(3) ?
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 O1 1_554 0.81(3) 2.17(3) 2.957(4) 166(4)
O1W H1WA O2 2_777 0.81(3) 2.04(3) 2.834(4) 169(4)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
O3 S O1 Zn . . -126.3(2)
O2 S O1 Zn . . 110.1(2)
O4 S O1 Zn . . -6.0(3)
O4 Zn O1 S 2_777 . 53.6(2)
N3 Zn O1 S . . -146.17(19)
N2 Zn O1 S . . -60.8(2)
N1 Zn O1 S . . 145.6(2)
O3 S O4 Zn . 2_777 26.6(3)
O2 S O4 Zn . 2_777 150.3(2)
O1 S O4 Zn . 2_777 -93.4(2)
O4 Zn N1 C5 2_777 . -110.8(2)
O1 Zn N1 C5 . . 141.7(3)
N3 Zn N1 C5 . . 5.0(2)
N2 Zn N1 C5 . . 20.8(4)
O4 Zn N1 C1 2_777 . 62.1(3)
O1 Zn N1 C1 . . -45.4(3)
N3 Zn N1 C1 . . 177.9(3)
N2 Zn N1 C1 . . -166.3(3)
O4 Zn N2 C15 2_777 . -70.2(3)
O1 Zn N2 C15 . . 44.1(3)
N3 Zn N2 C15 . . 177.3(3)
N1 Zn N2 C15 . . 161.6(3)
O4 Zn N2 C11 2_777 . 106.7(3)
O1 Zn N2 C11 . . -139.0(2)
N3 Zn N2 C11 . . -5.8(2)
N1 Zn N2 C11 . . -21.5(4)
O4 Zn N3 C6 2_777 . 79.6(3)
O1 Zn N3 C6 . . -79.5(3)
N2 Zn N3 C6 . . -176.8(3)
N1 Zn N3 C6 . . -4.9(2)
O4 Zn N3 C10 2_777 . -96.7(2)
O1 Zn N3 C10 . . 104.2(3)
N2 Zn N3 C10 . . 6.9(2)
N1 Zn N3 C10 . . 178.8(3)
C5 N1 C1 C2 . . -0.3(5)
Zn N1 C1 C2 . . -173.1(3)
N1 C1 C2 C3 . . -0.7(6)
C1 C2 C3 C4 . . 0.3(6)
C2 C3 C4 C5 . . 0.9(6)
C1 N1 C5 C4 . . 1.6(5)
Zn N1 C5 C4 . . 175.1(3)
C1 N1 C5 C6 . . -178.0(3)
Zn N1 C5 C6 . . -4.5(4)
C3 C4 C5 N1 . . -1.9(5)
C3 C4 C5 C6 . . 177.7(3)
C10 N3 C6 C7 . . 0.8(5)
Zn N3 C6 C7 . . -175.4(2)
C10 N3 C6 C5 . . -179.7(3)
Zn N3 C6 C5 . . 4.1(4)
N1 C5 C6 N3 . . 0.6(4)
C4 C5 C6 N3 . . -179.1(3)
N1 C5 C6 C7 . . -180.0(3)
C4 C5 C6 C7 . . 0.3(5)
N3 C6 C7 C8 . . 1.0(5)
C5 C6 C7 C8 . . -178.4(3)
C6 C7 C8 C9 . . -1.9(6)
C7 C8 C9 C10 . . 1.0(6)
C6 N3 C10 C9 . . -1.7(5)
Zn N3 C10 C9 . . 174.6(3)
C6 N3 C10 C11 . . 176.9(3)
Zn N3 C10 C11 . . -6.8(4)
C8 C9 C10 N3 . . 0.7(6)
C8 C9 C10 C11 . . -177.7(4)
C15 N2 C11 C12 . . 0.0(5)
Zn N2 C11 C12 . . -177.2(3)
C15 N2 C11 C10 . . -178.6(3)
Zn N2 C11 C10 . . 4.2(4)
N3 C10 C11 N2 . . 1.4(5)
C9 C10 C11 N2 . . 179.9(3)
N3 C10 C11 C12 . . -177.2(3)
C9 C10 C11 C12 . . 1.3(6)
N2 C11 C12 C13 . . -0.3(6)
C10 C11 C12 C13 . . 178.2(3)
C11 C12 C13 C14 . . 0.1(6)
C12 C13 C14 C15 . . 0.4(6)
C11 N2 C15 C14 . . 0.6(6)
Zn N2 C15 C14 . . 177.3(3)
C13 C14 C15 N2 . . -0.7(6)
