#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/53/2015300.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_2015300
loop_
_publ_author_name
'M. Enriqueta Díaz de Vivar'
'Sergio Baggio'
'María Teresa Garland'
'Ricardo Baggio'
_publ_section_title
;Di-μ₂-sulfito-κ⁸O,O':O',O''-bis[(2,4,6-tri-2-pyridyl-1,3,5-triazine-κ³N²,N¹,N⁶)cadmium(II)]
 octahydrate
;
_journal_coeditor_code           FG3013
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m195
_journal_page_last               m198
_journal_paper_doi               10.1107/S0108270106012078
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Cd2 (S O3)2 (C18 H12 N6)2], 8H2 O'
_chemical_formula_moiety         'C36 H24 Cd2 N12 O6 S2, 8H2 O'
_chemical_formula_sum            'C36 H40 Cd2 N12 O14 S2'
_chemical_formula_weight         1153.72
_chemical_name_systematic
;
Di-μ₂-sulfito-κ⁴O,O':κ⁴O',O''-[2,4,6-tris(2-pyridyl)-
1,3,5-triazine-κ³N²,N¹,N⁶]cadmium(II) octahydrate
;
_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                103.902(2)
_cell_angle_beta                 107.988(2)
_cell_angle_gamma                91.639(2)
_cell_formula_units_Z            1
_cell_length_a                   8.5826(12)
_cell_length_b                   10.5117(14)
_cell_length_c                   13.1078(17)
_cell_measurement_temperature    295(2)
_cell_volume                     1085.0(3)
_computing_cell_refinement       'SAINT-NT (Bruker, 2000)'
_computing_data_collection       'SMART-NT (Bruker, 2001)'
_computing_data_reduction        SAINT-NT
_computing_molecular_graphics    'SHELXTL-NT (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL-NT and PLATON (Spek, 2005)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_device_type  'Bruker 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  0.0193
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9107
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         1.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.157
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.128
_refine_diff_density_min         -0.376
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.843
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         4665
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.842
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0703P)²+0.6306P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0881
_reflns_number_gt                4289
_reflns_number_total             4665
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fg3013.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2015300
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Cd Cd1 0.51459(2) 0.596554(17) 0.641740(14) 0.03450(8) Uani d . 1
S S1 0.69658(9) 0.36093(7) 0.57426(5) 0.03723(15) Uani d . 1
O O1 0.7434(3) 0.3759(2) 0.47503(17) 0.0477(5) Uani d . 1
O O2 0.7513(2) 0.4936(2) 0.66154(16) 0.0440(5) Uani d . 1
O O3 0.5088(2) 0.3598(2) 0.53321(16) 0.0432(4) Uani d . 1
N N1 0.6839(3) 0.8109(2) 0.71068(18) 0.0369(5) Uani d . 1
N N2 0.5413(3) 0.7031(2) 0.82694(17) 0.0347(5) Uani d . 1
N N3 0.3430(3) 0.4824(2) 0.71436(18) 0.0362(5) Uani d . 1
N N4 0.4820(3) 0.7009(2) 0.98974(18) 0.0371(5) Uani d . 1
N N5 0.6551(3) 0.8803(2) 0.98680(19) 0.0384(5) Uani d . 1
N N6 0.6872(3) 0.9952(3) 1.2021(2) 0.0464(6) Uani d . 1
C C1 0.7557(4) 0.8613(3) 0.6501(2) 0.0429(6) Uani d . 1
H H1B 0.7319 0.8178 0.5755 0.051 Uiso calc R 1
C C2 0.8636(4) 0.9750(3) 0.6936(3) 0.0499(7) Uani d . 1
H H2A 0.9113 1.0072 0.6487 0.060 Uiso calc R 1
C C3 0.9001(4) 1.0403(3) 0.8032(3) 0.0520(8) Uani d . 1
H H3A 0.9747 1.1161 0.8342 0.062 Uiso calc R 1
C C4 0.8243(4) 0.9918(3) 0.8671(2) 0.0437(6) Uani d . 1
H H4B 0.8440 1.0357 0.9413 0.052 Uiso calc R 1
C C5 0.7187(3) 0.8768(3) 0.8181(2) 0.0348(5) Uani d . 1
C C6 0.6347(3) 0.8171(3) 0.8818(2) 0.0339(5) Uani d . 1
C C7 0.5751(3) 0.8164(3) 1.0366(2) 0.0350(5) Uani d . 1
C C8 0.4653(3) 0.6493(3) 0.8837(2) 0.0338(5) Uani d . 1
C C9 0.3518(3) 0.5281(3) 0.8207(2) 0.0338(5) Uani d . 1
C C10 0.2536(4) 0.4707(3) 0.8676(3) 0.0433(6) Uani d . 1
H H10A 0.2650 0.5020 0.9424 0.052 Uiso calc R 1
C C11 0.1387(4) 0.3657(3) 0.8002(3) 0.0491(7) Uani d . 1
H H11A 0.0700 0.3256 0.8288 0.059 Uiso calc R 1
C C12 0.1266(4) 0.3211(3) 0.6902(3) 0.0473(7) Uani d . 1
H H12A 0.0486 0.2513 0.6433 0.057 Uiso calc R 1
C C13 0.2316(4) 0.3812(3) 0.6505(2) 0.0428(6) Uani d . 1
H H13A 0.2244 0.3497 0.5764 0.051 Uiso calc R 1
C C14 0.5919(3) 0.8798(3) 1.1547(2) 0.0363(6) Uani d . 1
C C15 0.5113(4) 0.8197(3) 1.2102(2) 0.0443(6) Uani d . 1
H H15A 0.4450 0.7400 1.1744 0.053 Uiso calc R 1
C C16 0.5315(4) 0.8808(3) 1.3198(3) 0.0501(7) Uani d . 1
H H16A 0.4796 0.8424 1.3594 0.060 Uiso calc R 1
C C17 0.6287(4) 0.9984(3) 1.3695(2) 0.0511(8) Uani d . 1
H H17A 0.6446 1.0412 1.4434 0.061 Uiso calc R 1
C C18 0.7029(5) 1.0524(3) 1.3075(3) 0.0536(8) Uani d . 1
H H18A 0.7675 1.1332 1.3413 0.064 Uiso calc R 1
O O1W 1.1519(4) 0.7983(3) 0.8610(2) 0.0656(7) Uani d D 1
H H1WA 1.108(5) 0.754(3) 0.7968(14) 0.066(13) Uiso d D 1
H H1WB 1.195(5) 0.870(2) 0.863(3) 0.076(14) Uiso d D 1
O O2W 0.7897(4) 0.4772(3) 0.8799(2) 0.0662(7) Uani d D 1
H H2WA 0.859(6) 0.541(4) 0.912(3) 0.13(2) Uiso d D 1
H H2WB 0.773(5) 0.458(4) 0.8130(10) 0.082(14) Uiso d D 1
O O3W 1.0118(3) 0.6592(3) 0.6336(3) 0.0638(6) Uani d D 1
H H3WA 0.950(5) 0.603(3) 0.641(4) 0.097(18) Uiso d D 1
H H3WB 1.065(5) 0.625(4) 0.594(3) 0.077(14) Uiso d D 1
O O4W 1.0274(4) 0.6911(3) 1.0013(2) 0.0685(7) Uani d D 1
H H4WA 1.065(4) 0.715(4) 0.958(3) 0.062(12) Uiso d D 1
H H4WB 1.094(5) 0.654(7) 1.040(5) 0.16(3) Uiso d D 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'
Cd Cd -0.8075 1.2024 '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
O2 Cd1 O1 . 2_666 148.00(7) ?
O2 Cd1 N2 . . 102.30(7) ?
O1 Cd1 N2 2_666 . 109.26(8) ?
O2 Cd1 O3 . 2_666 97.32(7) ?
O1 Cd1 O3 2_666 2_666 60.25(7) ?
N2 Cd1 O3 . 2_666 141.88(7) ?
O2 Cd1 N3 . . 106.51(8) ?
O1 Cd1 N3 2_666 . 81.46(7) ?
N2 Cd1 N3 . . 67.59(7) ?
O3 Cd1 N3 2_666 . 136.23(7) ?
O2 Cd1 N1 . . 89.26(7) ?
O1 Cd1 N1 2_666 . 107.68(8) ?
N2 Cd1 N1 . . 66.77(7) ?
O3 Cd1 N1 2_666 . 81.29(7) ?
N3 Cd1 N1 . . 133.89(7) ?
O2 Cd1 O3 . . 58.63(7) ?
O1 Cd1 O3 2_666 . 93.89(7) ?
N2 Cd1 O3 . . 135.42(7) ?
O3 Cd1 O3 2_666 . 82.66(7) ?
N3 Cd1 O3 . . 79.44(7) ?
N1 Cd1 O3 . . 141.63(7) ?
O2 Cd1 S1 . 2_666 123.66(5) ?
O1 Cd1 S1 2_666 2_666 29.88(5) ?
N2 Cd1 S1 . 2_666 131.50(6) ?
O3 Cd1 S1 2_666 2_666 30.48(5) ?
N3 Cd1 S1 . 2_666 108.36(6) ?
N1 Cd1 S1 . 2_666 96.83(6) ?
O3 Cd1 S1 . 2_666 86.26(5) ?
O1 S1 O2 . . 106.54(12) y
O1 S1 O3 . . 102.60(12) y
O2 S1 O3 . . 102.16(12) y
O1 S1 Cd1 . 2_666 50.36(8) ?
O2 S1 Cd1 . 2_666 109.41(8) ?
O3 S1 Cd1 . 2_666 52.46(8) ?
S1 O1 Cd1 . 2_666 99.76(10) ?
S1 O2 Cd1 . . 104.31(10) ?
S1 O3 Cd1 . 2_666 97.06(9) ?
S1 O3 Cd1 . . 94.14(9) ?
Cd1 O3 Cd1 2_666 . 97.34(7) ?
C1 N1 C5 . . 117.4(2) ?
C1 N1 Cd1 . . 123.55(18) ?
C5 N1 Cd1 . . 118.77(17) ?
C6 N2 C8 . . 116.3(2) ?
C6 N2 Cd1 . . 122.73(17) ?
C8 N2 Cd1 . . 120.96(17) ?
C13 N3 C9 . . 118.6(2) ?
C13 N3 Cd1 . . 122.27(18) ?
C9 N3 Cd1 . . 119.00(17) ?
C8 N4 C7 . . 115.3(2) ?
C6 N5 C7 . . 113.8(2) ?
C18 N6 C14 . . 117.2(3) ?
N1 C1 C2 . . 122.7(3) ?
N1 C1 H1B . . 118.6 ?
C2 C1 H1B . . 118.6 ?
C3 C2 C1 . . 119.5(3) ?
C3 C2 H2A . . 120.3 ?
C1 C2 H2A . . 120.3 ?
C2 C3 C4 . . 118.9(3) ?
C2 C3 H3A . . 120.5 ?
C4 C3 H3A . . 120.5 ?
C5 C4 C3 . . 118.3(3) ?
C5 C4 H4B . . 120.9 ?
C3 C4 H4B . . 120.9 ?
N1 C5 C4 . . 123.2(2) ?
N1 C5 C6 . . 115.3(2) ?
C4 C5 C6 . . 121.5(2) ?
N5 C6 N2 . . 124.9(2) ?
N5 C6 C5 . . 119.0(2) ?
N2 C6 C5 . . 116.1(2) ?
N4 C7 N5 . . 125.8(2) ?
N4 C7 C14 . . 116.8(2) ?
N5 C7 C14 . . 117.4(2) ?
N4 C8 N2 . . 123.9(2) ?
N4 C8 C9 . . 119.8(2) ?
N2 C8 C9 . . 116.3(2) ?
N3 C9 C10 . . 122.5(3) ?
N3 C9 C8 . . 115.8(2) ?
C10 C9 C8 . . 121.6(2) ?
C11 C10 C9 . . 118.2(3) ?
C11 C10 H10A . . 120.9 ?
C9 C10 H10A . . 120.9 ?
C12 C11 C10 . . 119.3(3) ?
C12 C11 H11A . . 120.3 ?
C10 C11 H11A . . 120.3 ?
C11 C12 C13 . . 119.0(3) ?
C11 C12 H12A . . 120.5 ?
C13 C12 H12A . . 120.5 ?
N3 C13 C12 . . 122.4(3) ?
N3 C13 H13A . . 118.8 ?
C12 C13 H13A . . 118.8 ?
N6 C14 C15 . . 123.0(3) ?
N6 C14 C7 . . 116.7(2) ?
C15 C14 C7 . . 120.2(3) ?
C16 C15 C14 . . 118.4(3) ?
C16 C15 H15A . . 120.8 ?
C14 C15 H15A . . 120.8 ?
C17 C16 C15 . . 119.3(3) ?
C17 C16 H16A . . 120.4 ?
C15 C16 H16A . . 120.4 ?
C16 C17 C18 . . 118.5(3) ?
C16 C17 H17A . . 120.7 ?
C18 C17 H17A . . 120.7 ?
N6 C18 C17 . . 123.6(3) ?
N6 C18 H18A . . 118.2 ?
C17 C18 H18A . . 118.2 ?
H1WA O1W H1WB . . 111(4) ?
H2WA O2W H2WB . . 111(4) ?
H3WA O3W H3WB . . 110(4) ?
H4WA O4W H4WB . . 111(4) ?
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
Cd1 O1 2_666 2.342(2) y
Cd1 O2 . 2.302(2) y
Cd1 O3 . 2.543(2) y
Cd1 O3 2_666 2.395(2) y
Cd1 N1 . 2.455(2) y
Cd1 N2 . 2.353(2) y
Cd1 N3 . 2.414(2) y
S1 O1 . 1.515(2) y
S1 O2 . 1.529(2) y
S1 O3 . 1.532(2) y
N1 C1 . 1.332(4) ?
N1 C5 . 1.346(3) ?
N2 C6 . 1.331(3) ?
N2 C8 . 1.334(3) ?
N3 C13 . 1.329(4) ?
N3 C9 . 1.338(3) ?
N4 C8 . 1.325(3) ?
N4 C7 . 1.331(4) ?
N5 C6 . 1.331(3) ?
N5 C7 . 1.345(4) ?
N6 C18 . 1.330(4) ?
N6 C14 . 1.339(4) ?
C1 C2 . 1.377(4) ?
C1 H1B . 0.9300 ?
C2 C3 . 1.367(5) ?
C2 H2A . 0.9300 ?
C3 C4 . 1.381(4) ?
C3 H3A . 0.9300 ?
C4 C5 . 1.379(4) ?
C4 H4B . 0.9300 ?
C5 C6 . 1.486(4) ?
C7 C14 . 1.491(4) ?
C8 C9 . 1.477(4) ?
C9 C10 . 1.386(4) ?
C10 C11 . 1.379(4) ?
C10 H10A . 0.9300 ?
C11 C12 . 1.374(5) ?
C11 H11A . 0.9300 ?
C12 C13 . 1.378(4) ?
C12 H12A . 0.9300 ?
C13 H13A . 0.9300 ?
C14 C15 . 1.383(4) ?
C15 C16 . 1.379(4) ?
C15 H15A . 0.9300 ?
C16 C17 . 1.366(5) ?
C16 H16A . 0.9300 ?
C17 C18 . 1.382(5) ?
C17 H17A . 0.9300 ?
C18 H18A . 0.9300 ?
O1W H1WA . 0.82(2) ?
O1W H1WB . 0.82(3) ?
O2W H2WA . 0.82(5) ?
O2W H2WB . 0.82(2) ?
O3W H3WA . 0.83(4) ?
O3W H3WB . 0.82(4) ?
O4W H4WA . 0.81(4) ?
O4W H4WB . 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 H1WA O3W . 0.82(2) 2.02(2) 2.838(4) 174(3)
O1W H1WB N6 2_777 0.82(3) 2.19(3) 2.950(4) 154(4)
O2W H2WA O4W . 0.82(5) 1.97(4) 2.785(4) 175(5)
O2W H2WB O2 . 0.82(2) 2.06(2) 2.827(3) 156(4)
O3W H3WA O2 . 0.83(4) 2.15(4) 2.958(3) 166(4)
O3W H3WB O1 2_766 0.82(4) 2.11(4) 2.867(3) 154(4)
O4W H4WA O1W . 0.82(4) 2.01(4) 2.817(4) 173(4)
O4W H4WB O2W 2_767 0.82(5) 2.03(5) 2.827(5) 165(7)
