#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/63/2226316.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_2226316
loop_
_publ_author_name
'Fu, Chun-Hua'
'Zhou, Xiang'
'Yu, Qing'
'Bian, He-Dong'
_publ_section_title
;
 Hexaaquamagnesium(II)
 bis{[2-(1-phenyl-1H-tetrazol-5-yl)sulfanyl]acetate}
;
_journal_coeditor_code           WM2320
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m657
_journal_paper_doi               10.1107/S1600536810016983
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Mg (H2 O)6] (C9 H7 N4 O2 S)2'
_chemical_formula_moiety         'H12 Mg1 O6 2+, 2(C9 H7 N4 O2 S -)'
_chemical_formula_sum            'C18 H26 Mg N8 O10 S2'
_chemical_formula_weight         602.92
_chemical_name_systematic
;
Hexaaquamagnesium(II)
bis{[2-(1-phenyl-1H-tetrazol-5-yl)sulfanyl]acetate}
;
_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                92.57(3)
_cell_angle_beta                 99.14(3)
_cell_angle_gamma                100.07(3)
_cell_formula_units_Z            1
_cell_length_a                   6.8380(14)
_cell_length_b                   7.5220(15)
_cell_length_c                   13.556(3)
_cell_measurement_reflns_used    1867
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     675.9(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXS97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3914
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.05
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.286
_exptl_absorpt_correction_T_max  0.9314
_exptl_absorpt_correction_T_min  0.8061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2001)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             314.0
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.296
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         2347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0670P)²+0.2500P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1224
_reflns_number_gt                1867
_reflns_number_total             2347
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wm2320.cif
_cod_data_source_block           I
_cod_original_cell_volume        675.9(2)
_cod_original_formula_sum        'C18 H26 Mg N8 O10 S2 '
_cod_database_code               2226316
_cod_database_fobs_code          2226316
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mg Mg1 1.0000 0.0000 1.0000 0.0290(3) Uani d S 1 . .
C C1 0.5668(4) 0.3487(4) 0.8626(2) 0.0316(6) Uani d . 1 . .
C C2 0.4066(4) 0.4641(4) 0.8376(2) 0.0334(7) Uani d . 1 . .
H H2A 0.4655 0.5792 0.8155 0.040 Uiso calc R 1 . .
H H2B 0.3472 0.4874 0.8962 0.040 Uiso calc R 1 . .
C C3 0.0428(4) 0.4804(4) 0.72657(19) 0.0292(6) Uani d . 1 . .
C C4 -0.1942(4) 0.3060(4) 0.5768(2) 0.0321(7) Uani d . 1 . .
C C5 -0.1784(4) 0.1299(4) 0.5934(2) 0.0393(7) Uani d . 1 . .
H H5 -0.1309 0.0985 0.6572 0.047 Uiso calc R 1 . .
C C6 -0.2343(4) 0.0001(4) 0.5137(3) 0.0491(9) Uani d . 1 . .
H H6A -0.2206 -0.1191 0.5232 0.059 Uiso calc R 1 . .
C C7 -0.3105(5) 0.0470(5) 0.4198(2) 0.0503(9) Uani d . 1 . .
H H7A -0.3477 -0.0407 0.3664 0.060 Uiso calc R 1 . .
C C8 -0.3314(5) 0.2215(5) 0.4051(2) 0.0526(9) Uani d . 1 . .
H H8A -0.3861 0.2511 0.3420 0.063 Uiso calc R 1 . .
C C9 -0.2721(5) 0.3546(4) 0.4831(2) 0.0431(8) Uani d . 1 . .
H H9A -0.2842 0.4740 0.4730 0.052 Uiso calc R 1 . .
N N1 -0.1273(3) 0.4464(3) 0.65654(16) 0.0326(6) Uani d . 1 . .
N N2 -0.2303(4) 0.5835(4) 0.66553(19) 0.0449(7) Uani d . 1 . .
N N3 -0.1245(4) 0.6943(4) 0.73682(19) 0.0465(7) Uani d . 1 . .
N N4 0.0470(4) 0.6354(3) 0.77710(17) 0.0364(6) Uani d . 1 . .
O O1 0.5227(3) 0.1854(3) 0.83268(16) 0.0427(6) Uani d . 1 . .
O O2 0.7301(3) 0.4261(3) 0.91271(18) 0.0550(7) Uani d . 1 . .
O O3 1.0502(3) 0.2699(3) 0.97908(17) 0.0371(5) Uani d . 1 . .
O O4 1.2154(4) -0.0513(3) 0.91404(18) 0.0453(6) Uani d . 1 . .
O O5 0.7751(3) -0.0466(3) 0.87611(17) 0.0465(6) Uani d . 1 . .
S S1 0.21753(11) 0.33953(10) 0.73900(5) 0.0384(2) Uani d . 1 . .
H H5B 0.700(5) 0.027(5) 0.857(2) 0.050(10) Uiso d . 1 . .
H H3B 1.122(5) 0.338(5) 1.016(3) 0.048(11) Uiso d . 1 . .
H H5A 0.793(6) -0.110(5) 0.827(3) 0.069(12) Uiso d . 1 . .
H H4B 1.194(6) -0.160(6) 0.877(3) 0.088(14) Uiso d . 1 . .
H H4A 1.291(6) 0.020(5) 0.893(3) 0.058(13) Uiso d . 1 . .
H H3A 0.935(8) 0.313(7) 0.944(4) 0.13(2) Uiso 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'
Mg Mg 0.0486 0.0363 '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'
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
O3 Mg1 O3 2_757 . 180.0000(10) ?
O3 Mg1 O5 2_757 2_757 90.36(10) ?
O3 Mg1 O5 . 2_757 89.64(10) ?
O3 Mg1 O5 2_757 . 89.64(10) ?
O3 Mg1 O5 . . 90.36(10) ?
O5 Mg1 O5 2_757 . 180.0000(10) ?
O3 Mg1 O4 2_757 . 87.11(10) ?
O3 Mg1 O4 . . 92.89(10) ?
O5 Mg1 O4 2_757 . 88.33(10) ?
O5 Mg1 O4 . . 91.67(10) ?
O3 Mg1 O4 2_757 2_757 92.89(10) ?
O3 Mg1 O4 . 2_757 87.11(10) ?
O5 Mg1 O4 2_757 2_757 91.67(10) ?
O5 Mg1 O4 . 2_757 88.33(10) ?
O4 Mg1 O4 . 2_757 180.0000(10) ?
O2 C1 O1 . . 125.7(3) ?
O2 C1 C2 . . 116.6(2) ?
O1 C1 C2 . . 117.6(2) ?
C1 C2 S1 . . 107.16(18) ?
C1 C2 H2A . . 110.3 ?
S1 C2 H2A . . 110.3 ?
C1 C2 H2B . . 110.3 ?
S1 C2 H2B . . 110.3 ?
H2A C2 H2B . . 108.5 ?
N4 C3 N1 . . 108.1(2) ?
N4 C3 S1 . . 129.0(2) ?
N1 C3 S1 . . 122.93(19) ?
C5 C4 C9 . . 121.5(3) ?
C5 C4 N1 . . 120.5(2) ?
C9 C4 N1 . . 118.0(3) ?
C4 C5 C6 . . 118.9(3) ?
C4 C5 H5 . . 120.6 ?
C6 C5 H5 . . 120.6 ?
C7 C6 C5 . . 120.1(3) ?
C7 C6 H6A . . 119.9 ?
C5 C6 H6A . . 119.9 ?
C8 C7 C6 . . 120.4(3) ?
C8 C7 H7A . . 119.8 ?
C6 C7 H7A . . 119.8 ?
C7 C8 C9 . . 120.6(3) ?
C7 C8 H8A . . 119.7 ?
C9 C8 H8A . . 119.7 ?
C8 C9 C4 . . 118.5(3) ?
C8 C9 H9A . . 120.8 ?
C4 C9 H9A . . 120.8 ?
N2 N1 C3 . . 108.3(2) ?
N2 N1 C4 . . 120.9(2) ?
C3 N1 C4 . . 130.5(2) ?
N3 N2 N1 . . 106.2(2) ?
N2 N3 N4 . . 111.7(2) ?
C3 N4 N3 . . 105.8(2) ?
Mg1 O3 H3B . . 123(3) ?
Mg1 O3 H3A . . 115(3) ?
H3B O3 H3A . . 115(4) ?
Mg1 O4 H4B . . 119(3) ?
Mg1 O4 H4A . . 127(3) ?
H4B O4 H4A . . 111(4) ?
Mg1 O5 H5B . . 125(2) ?
Mg1 O5 H5A . . 118(3) ?
H5B O5 H5A . . 110(3) ?
C3 S1 C2 . . 100.91(12) ?
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
Mg1 O3 2_757 2.039(2) ?
Mg1 O3 . 2.039(2) y
Mg1 O5 2_757 2.061(2) ?
Mg1 O5 . 2.061(2) y
Mg1 O4 . 2.093(2) y
Mg1 O4 2_757 2.093(2) ?
C1 O2 . 1.242(3) ?
C1 O1 . 1.246(3) ?
C1 C2 . 1.519(4) ?
C2 S1 . 1.803(3) ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C3 N4 . 1.319(3) ?
C3 N1 . 1.358(3) ?
C3 S1 . 1.725(3) ?
C4 C5 . 1.373(4) ?
C4 C9 . 1.388(4) ?
C4 N1 . 1.438(3) ?
C5 C6 . 1.383(4) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.382(5) ?
C6 H6A . 0.9300 ?
C7 C8 . 1.365(5) ?
C7 H7A . 0.9300 ?
C8 C9 . 1.383(4) ?
C8 H8A . 0.9300 ?
C9 H9A . 0.9300 ?
N1 N2 . 1.358(3) ?
N2 N3 . 1.284(3) ?
N3 N4 . 1.367(3) ?
O3 H3B . 0.75(4) ?
O3 H3A . 0.97(6) ?
O4 H4B . 0.91(5) ?
O4 H4A . 0.77(4) ?
O5 H5B . 0.84(4) ?
O5 H5A . 0.84(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
O3 H3A O2 1_555 0.97(5) 1.77(6) 2.711(3) 164(5)
O3 H3B O2 2_767 0.75(4) 2.00(4) 2.727(3) 162(4)
O4 H4A O1 1_655 0.77(4) 2.13(4) 2.899(3) 172(4)
O4 H4B N4 1_645 0.92(4) 2.01(4) 2.882(3) 158(4)
O5 H5A N3 1_645 0.84(4) 2.08(4) 2.896(4) 164(4)
O5 H5B O1 1_555 0.84(4) 1.85(4) 2.682(3) 172(3)
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O2 C1 C2 S1 . . . . 164.8(2) ?
O1 C1 C2 S1 . . . . -16.2(3) ?
C9 C4 C5 C6 . . . . 2.6(4) ?
N1 C4 C5 C6 . . . . -176.6(3) ?
C4 C5 C6 C7 . . . . -2.0(5) ?
C5 C6 C7 C8 . . . . -0.1(5) ?
C6 C7 C8 C9 . . . . 1.6(5) ?
C7 C8 C9 C4 . . . . -1.0(5) ?
C5 C4 C9 C8 . . . . -1.1(5) ?
N1 C4 C9 C8 . . . . 178.1(3) ?
N4 C3 N1 N2 . . . . -0.7(3) ?
S1 C3 N1 N2 . . . . -179.1(2) ?
N4 C3 N1 C4 . . . . 173.4(3) ?
S1 C3 N1 C4 . . . . -5.0(4) ?
C5 C4 N1 N2 . . . . -142.3(3) ?
C9 C4 N1 N2 . . . . 38.4(4) ?
C5 C4 N1 C3 . . . . 44.2(4) ?
C9 C4 N1 C3 . . . . -135.0(3) ?
C3 N1 N2 N3 . . . . 0.7(3) ?
C4 N1 N2 N3 . . . . -174.0(3) ?
N1 N2 N3 N4 . . . . -0.5(4) ?
N1 C3 N4 N3 . . . . 0.3(3) ?
S1 C3 N4 N3 . . . . 178.7(2) ?
N2 N3 N4 C3 . . . . 0.1(4) ?
N4 C3 S1 C2 . . . . -0.9(3) ?
N1 C3 S1 C2 . . . . 177.1(2) ?
C1 C2 S1 C3 . . . . 176.0(2) ?
