#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/77/2207778.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_2207778
loop_
_publ_author_name
'M. Enriqueta Díaz de Vivar'
'Sergio Baggio'
'María Teresa Garland '
'Ricardo Baggio'
_publ_section_title
;Di-μ-sulfato-κ³O,O':O'';κ³O,O':O''-bis{aqua[2,4,6-tris(2-pyridyl)-1,3,5-triazine-κ³N¹,N²,N⁶]manganese(II)}
 tetrahydrate
;
_journal_coeditor_code           HB6305
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m141
_journal_page_last               m143
_journal_paper_doi               10.1107/S1600536805041528
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Mn2 (S O4)2 (C16 H12 N6)2 (H2 O)2], 4H2 O1'
_chemical_formula_moiety         'C36 H28 Mn2 N12 O10 S2, 4H2 O'
_chemical_formula_sum            'C36 H36 Mn2 N12 O14 S2'
_chemical_formula_weight         1034.77
_chemical_name_systematic
;
Di-μ-sulfato-κ³O,O':O'';κ³O,O':O''-bis{aqua[2,4,6-tris(2-pyridyl)-
1,3,5-triazine-κ³N¹,N²,N⁶]manganese(II)} tetrahydrate
;
_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                103.566(3)
_cell_angle_beta                 97.981(3)
_cell_angle_gamma                110.409(3)
_cell_formula_units_Z            1
_cell_length_a                   8.8737(16)
_cell_length_b                   10.5634(19)
_cell_length_c                   12.587(2)
_cell_measurement_reflns_used    1017
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      43.905
_cell_measurement_theta_min      5.048
_cell_volume                     1042.9(3)
_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      291(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART CCD'
_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  0.058
_diffrn_reflns_av_sigmaI/netI    0.076
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8696
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.789
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             530
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.385
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         4041
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0661
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.013P)²+2.08P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1093
_reflns_number_gt                2775
_reflns_number_total             4041
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb6305.cif
_cod_data_source_block           I
_cod_database_code               2207778
_cod_database_fobs_code          2207778
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_type_symbol
Mn 0.08793(9) -0.00477(7) 0.18395(6) 0.0322(2) Uani d . 1 Mn
S -0.00324(15) -0.20172(12) -0.03890(10) 0.0339(3) Uani d . 1 S
O1 0.1636(4) -0.0991(4) 0.0266(3) 0.0535(9) Uani d . 1 O
O2 -0.1108(4) -0.1846(3) 0.0360(3) 0.0476(8) Uani d . 1 O
O3 -0.0078(5) -0.3444(3) -0.0699(3) 0.0562(9) Uani d . 1 O
O4 -0.0533(4) -0.1707(3) -0.1423(3) 0.0479(8) Uani d . 1 O
N1 0.3790(5) 0.1289(4) 0.2420(3) 0.0366(10) Uani d . 1 N
N2 0.1627(4) 0.1351(4) 0.3642(3) 0.0296(9) Uani d . 1 N
N3 -0.1453(5) -0.0318(4) 0.2632(3) 0.0324(9) Uani d . 1 N
N4 0.3713(5) 0.3076(4) 0.5194(3) 0.0379(10) Uani d . 1 N
N5 0.0920(5) 0.2204(4) 0.5326(3) 0.0336(9) Uani d . 1 N
N6 0.1878(5) 0.3821(4) 0.7507(3) 0.0408(10) Uani d . 1 N
C1 0.4866(7) 0.1244(5) 0.1782(5) 0.0491(14) Uani d . 1 C
H1A 0.4457 0.0650 0.1043 0.059 Uiso calc R 1 H
C2 0.6538(7) 0.2024(6) 0.2159(5) 0.0532(15) Uani d . 1 C
H2A 0.7237 0.1951 0.1682 0.064 Uiso calc R 1 H
C3 0.7176(6) 0.2916(6) 0.3245(5) 0.0517(14) Uani d . 1 C
H3A 0.8309 0.3448 0.3518 0.062 Uiso calc R 1 H
C4 0.6106(6) 0.3005(5) 0.3918(5) 0.0473(14) Uani d . 1 C
H4A 0.6495 0.3602 0.4657 0.057 Uiso calc R 1 H
C5 0.4436(6) 0.2185(5) 0.3474(4) 0.0321(11) Uani d . 1 C
C6 0.3202(5) 0.2225(5) 0.4149(4) 0.0303(11) Uani d . 1 C
C7 0.2523(6) 0.3022(5) 0.5748(4) 0.0352(11) Uani d . 1 C
C8 0.0548(5) 0.1394(4) 0.4272(4) 0.0290(10) Uani d . 1 C
C9 -0.1206(5) 0.0439(4) 0.3712(4) 0.0284(10) Uani d . 1 C
C10 -0.2459(6) 0.0329(5) 0.4254(4) 0.0391(12) Uani d . 1 C
H10A -0.2234 0.0862 0.5002 0.047 Uiso calc R 1 H
C11 -0.4039(6) -0.0570(5) 0.3684(4) 0.0436(13) Uani d . 1 C
H11A -0.4906 -0.0664 0.4038 0.052 Uiso calc R 1 H
C12 -0.4331(6) -0.1339(5) 0.2575(4) 0.0434(13) Uani d . 1 C
H12A -0.5399 -0.1953 0.2162 0.052 Uiso calc R 1 H
C13 -0.2998(6) -0.1174(5) 0.2089(4) 0.0403(12) Uani d . 1 C
H13A -0.3199 -0.1695 0.1340 0.048 Uiso calc R 1 H
C14 0.3072(6) 0.3939(5) 0.6944(4) 0.0334(11) Uani d . 1 C
C15 0.4708(6) 0.4828(5) 0.7432(4) 0.0444(13) Uani d . 1 C
H15A 0.5505 0.4872 0.7018 0.053 Uiso calc R 1 H
C16 0.5140(6) 0.5636(5) 0.8519(4) 0.0469(14) Uani d . 1 C
H16A 0.6237 0.6248 0.8861 0.056 Uiso calc R 1 H
C17 0.3942(6) 0.5542(5) 0.9109(4) 0.0477(14) Uani d . 1 C
H17A 0.4207 0.6088 0.9858 0.057 Uiso calc R 1 H
C18 0.2355(7) 0.4629(5) 0.8576(4) 0.0485(14) Uani d . 1 C
H18A 0.1551 0.4567 0.8985 0.058 Uiso calc R 1 H
O1W 0.1254(4) -0.1645(3) 0.2654(3) 0.0420(9) Uani d D 1 O
H1WA 0.038(4) -0.214(3) 0.279(4) 0.050 Uiso d D 1 H
H1WB 0.167(5) -0.214(3) 0.228(4) 0.050 Uiso d D 1 H
O2W 0.8636(6) 0.5572(6) 0.6678(4) 0.118(2) Uani d D 1 O
H2WA 0.894(4) 0.539(3) 0.7259(18) 0.141 Uiso d D 1 H
H2WB 0.867(4) 0.639(2) 0.6819(19) 0.141 Uiso d D 1 H
O3W 0.1945(4) 0.6358(3) 0.1152(3) 0.0495(10) Uani d D 1 O
H3WA 0.169(6) 0.550(2) 0.106(3) 0.059 Uiso d D 1 H
H3WB 0.146(6) 0.651(4) 0.061(3) 0.059 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'
Mn Mn 0.3368 0.7283 '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
O4 Mn O1W 2 . 167.75(12) n
O4 Mn N1 2 . 90.03(13) n
O4 Mn N2 2 . 85.09(12) n
O4 Mn N3 2 . 86.45(13) n
O4 Mn O1 2 . 99.97(13) n
O4 Mn O2 2 . 98.15(13) n
O1W Mn N1 . . 88.63(12) n
O1W Mn N2 . . 83.06(12) n
O1W Mn N3 . . 86.35(12) n
O1W Mn O1 . . 91.80(13) n
O1W Mn O2 . . 90.55(12) n
O2 Mn O1 . . 60.49(11) n
O1 Mn N1 . . 80.35(12) n
N1 Mn N2 . . 69.08(13) n
N2 Mn N3 . . 68.52(13) n
N3 Mn O2 . . 81.38(12) n
N2 Mn O2 . . 149.52(12) ?
N2 Mn O1 . . 149.06(13) ?
O2 Mn N1 . . 140.79(12) ?
O1 Mn N3 . . 141.83(12) ?
N1 Mn N3 . . 137.59(13) ?
O3 S O2 . . 112.2(2) ?
O3 S O4 . . 108.09(19) ?
O2 S O4 . . 110.3(2) ?
O3 S O1 . . 110.4(2) ?
O2 S O1 . . 104.37(19) ?
O4 S O1 . . 111.5(2) ?
O3 S Mn . . 127.87(15) ?
O2 S Mn . . 52.15(13) ?
O4 S Mn . . 124.04(14) ?
O1 S Mn . . 52.25(13) ?
S O1 Mn . . 97.30(16) ?
S O2 Mn . . 97.79(17) ?
S O4 Mn . 2 136.16(19) ?
C1 N1 C5 . . 116.0(4) ?
C1 N1 Mn . . 125.6(3) ?
C5 N1 Mn . . 118.4(3) ?
C8 N2 C6 . . 115.0(4) ?
C8 N2 Mn . . 123.2(3) ?
C6 N2 Mn . . 121.8(3) ?
C13 N3 C9 . . 116.8(4) ?
C13 N3 Mn . . 124.6(3) ?
C9 N3 Mn . . 118.6(3) ?
C6 N4 C7 . . 115.1(4) ?
C8 N5 C7 . . 114.4(4) ?
C18 N6 C14 . . 116.1(4) ?
N1 C1 C2 . . 123.5(5) ?
N1 C1 H1A . . 118.2 ?
C2 C1 H1A . . 118.2 ?
C1 C2 C3 . . 119.5(5) ?
C1 C2 H2A . . 120.2 ?
C3 C2 H2A . . 120.3 ?
C4 C3 C2 . . 118.6(5) ?
C4 C3 H3A . . 120.7 ?
C2 C3 H3A . . 120.7 ?
C3 C4 C5 . . 118.4(5) ?
C3 C4 H4A . . 120.8 ?
C5 C4 H4A . . 120.8 ?
N1 C5 C4 . . 124.0(4) ?
N1 C5 C6 . . 114.5(4) ?
C4 C5 C6 . . 121.5(4) ?
N4 C6 N2 . . 124.7(4) ?
N4 C6 C5 . . 119.1(4) ?
N2 C6 C5 . . 116.2(4) ?
N5 C7 N4 . . 125.4(4) ?
N5 C7 C14 . . 118.4(4) ?
N4 C7 C14 . . 116.2(4) ?
N5 C8 N2 . . 125.5(4) ?
N5 C8 C9 . . 119.2(4) ?
N2 C8 C9 . . 115.3(4) ?
N3 C9 C10 . . 123.0(4) ?
N3 C9 C8 . . 114.4(4) ?
C10 C9 C8 . . 122.6(4) ?
C11 C10 C9 . . 119.2(4) ?
C11 C10 H10A . . 120.4 ?
C9 C10 H10A . . 120.4 ?
C10 C11 C12 . . 119.0(4) ?
C10 C11 H11A . . 120.5 ?
C12 C11 H11A . . 120.5 ?
C11 C12 C13 . . 118.3(5) ?
C11 C12 H12A . . 120.8 ?
C13 C12 H12A . . 120.8 ?
N3 C13 C12 . . 123.6(4) ?
N3 C13 H13A . . 118.2 ?
C12 C13 H13A . . 118.2 ?
N6 C14 C15 . . 122.8(5) ?
N6 C14 C7 . . 115.6(4) ?
C15 C14 C7 . . 121.6(4) ?
C16 C15 C14 . . 119.2(5) ?
C16 C15 H15A . . 120.4 ?
C14 C15 H15A . . 120.4 ?
C15 C16 C17 . . 119.1(5) ?
C15 C16 H16A . . 120.4 ?
C17 C16 H16A . . 120.4 ?
C18 C17 C16 . . 118.4(5) ?
C18 C17 H17A . . 120.8 ?
C16 C17 H17A . . 120.8 ?
N6 C18 C17 . . 124.3(5) ?
N6 C18 H18A . . 117.8 ?
C17 C18 H18A . . 117.8 ?
Mn O1W H1WA . . 112(3) ?
Mn O1W H1WB . . 112(3) ?
H1WA O1W H1WB . . 112.(4) ?
H2WA O2W H2WB . . 112.(5) ?
H3WA O3W H3WB . . 112.(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
Mn O4 2 2.148(3) y
Mn N2 . 2.257(3) y
Mn O1W . 2.262(3) y
Mn O2 . 2.297(3) y
Mn O1 . 2.298(3) y
Mn N1 . 2.376(4) y
Mn N3 . 2.378(4) y
S O3 . 1.450(3) y
S O2 . 1.457(3) y
S O4 . 1.463(3) y
S O1 . 1.473(3) y
O4 Mn 2 2.148(3) ?
N1 C1 . 1.336(6) ?
N1 C5 . 1.343(6) ?
N2 C8 . 1.331(5) ?
N2 C6 . 1.338(5) ?
N3 C13 . 1.323(5) ?
N3 C9 . 1.350(5) ?
N4 C6 . 1.320(5) ?
N4 C7 . 1.336(5) ?
N5 C8 . 1.323(5) ?
N5 C7 . 1.330(5) ?
N6 C18 . 1.330(6) ?
N6 C14 . 1.341(5) ?
C1 C2 . 1.369(7) ?
C1 H1A . 0.9300 ?
C2 C3 . 1.373(7) ?
C2 H2A . 0.9300 ?
C3 C4 . 1.370(7) ?
C3 H3A . 0.9300 ?
C4 C5 . 1.381(6) ?
C4 H4A . 0.9300 ?
C5 C6 . 1.481(6) ?
C7 C14 . 1.491(6) ?
C8 C9 . 1.485(6) ?
C9 C10 . 1.368(6) ?
C10 C11 . 1.362(6) ?
C10 H10A . 0.9300 ?
C11 C12 . 1.377(6) ?
C11 H11A . 0.9300 ?
C12 C13 . 1.382(6) ?
C12 H12A . 0.9300 ?
C13 H13A . 0.9300 ?
C14 C15 . 1.377(6) ?
C15 C16 . 1.351(6) ?
C15 H15A . 0.9300 ?
C16 C17 . 1.369(7) ?
C16 H16A . 0.9300 ?
C17 C18 . 1.360(7) ?
C17 H17A . 0.9300 ?
C18 H18A . 0.9300 ?
O1W H1WA . 0.83(4) ?
O1W H1WB . 0.83(4) ?
O2W H2WA . 0.83(4) ?
O2W H2WB . 0.83(4) ?
O3W H3WA . 0.83(4) ?
O3W H3WB . 0.83(4) ?
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
O3W H3WA O3 2 0.83(4) 2.04(3) 2.811(5) 155(4)
O3W H3WB O3 1_565 0.83(4) 2.01(2) 2.833(5) 169(4)
O2W H2WB O4 1_666 0.83(4) 2.43(2) 3.052(6) 132(4)
O2W H2WA O3 1_666 0.83(4) 2.46(2) 3.130(5) 139(4)
O1W H1WA N6 2_556 0.83(4) 2.08(2) 2.867(5) 158(4)
O1W H1WB O3W 1_545 0.83(4) 1.98(2) 2.785(5) 162(4)
