#------------------------------------------------------------------------------
#$Date: 2016-02-20 21:30:07 +0100 (Sat 20 de Feb de 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/84/2228444.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_2228444
loop_
_publ_author_name
'Pasdar, Hoda'
'Heidari, Sanaz'
'Aghabozorg, Hossein'
'Notash, Behrouz'
_publ_section_title
;
 Hexaaquamagnesium(II) bis(pyridinium-2,6-dicarboxylate)
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1581
_journal_paper_doi               10.1107/S1600536810046696
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Mg (H2 O)6] (C7 H4 N O4)2'
_chemical_formula_moiety         'H12 Mg O6 2+, 2(C7 H4 N O4 -)'
_chemical_formula_sum            'C14 H20 Mg N2 O14'
_chemical_formula_weight         464.63
_chemical_name_systematic
;
Hexaaquamagnesium(II) bis(pyridinium-2,6-dicarboxylate)
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.79(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.432(3)
_cell_length_b                   11.108(2)
_cell_length_c                   6.5845(13)
_cell_measurement_reflns_used    1383
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.12
_cell_measurement_theta_min      2.38
_cell_volume                     981.3(3)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2005)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2005)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2005)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 0.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       'rotation method'
_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  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0184
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5499
_diffrn_reflns_theta_full        29.12
_diffrn_reflns_theta_max         29.12
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.940
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'(X-RED and X-SHAPE; Stoe & Cie, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             484.0
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1383
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0414P)²+0.5177P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                1178
_reflns_number_total             1383
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            jj2069.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               2228444
_cod_database_fobs_code          2228444
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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 0.5000 0.0000 0.0000 0.0249(2) Uani d S 1 . .
O O1 0.40364(11) 0.31353(9) 0.27234(16) 0.0499(3) Uani d . 1 . .
O O2 0.36594(9) 0.18375(8) 0.51657(15) 0.0396(3) Uani d . 1 . .
O O3 0.5000 0.18182(12) 0.0000 0.0360(3) Uani d S 1 . .
O O4 0.41819(12) 0.0000 0.2566(2) 0.0357(3) Uani d S 1 . .
O O5 0.36739(11) 0.0000 -0.1931(2) 0.0341(3) Uani d S 1 . .
N N1 0.37142(12) 0.5000 0.4931(2) 0.0257(3) Uani d S 1 . .
C C1 0.31770(16) 0.5000 0.8796(3) 0.0347(4) Uani d S 1 . .
H H1 0.2989 0.5000 1.0137 0.042 Uiso calc SR 1 . .
C C2 0.33156(11) 0.39121(12) 0.78070(19) 0.0312(3) Uani d . 1 . .
H H2 0.3225 0.3186 0.8476 0.037 Uiso calc R 1 . .
C C3 0.35898(9) 0.39277(10) 0.58164(18) 0.0253(3) Uani d . 1 . .
C C4 0.37779(11) 0.28571(11) 0.4447(2) 0.0310(3) Uani d . 1 . .
H H3 0.4708(14) 0.2281(19) 0.084(3) 0.053(5) Uiso d . 1 . .
H H4 0.4046(15) 0.0617(19) 0.327(3) 0.057(6) Uiso d . 1 . .
H H5 0.3664(16) 0.0661(19) -0.270(3) 0.065(6) Uiso d . 1 . .
H H1A 0.3899(19) 0.5000 0.366(4) 0.046(7) Uiso d S 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Mg1 0.0367(5) 0.0173(4) 0.0211(4) 0.000 0.0062(3) 0.000
O1 0.0892(9) 0.0278(5) 0.0351(5) 0.0102(5) 0.0267(6) -0.0011(4)
O2 0.0626(7) 0.0192(4) 0.0374(5) 0.0041(4) 0.0054(5) 0.0011(4)
O3 0.0602(10) 0.0177(6) 0.0315(7) 0.000 0.0172(6) 0.000
O4 0.0566(9) 0.0226(6) 0.0296(7) 0.000 0.0179(6) 0.000
O5 0.0467(8) 0.0295(7) 0.0262(6) 0.000 0.0034(6) 0.000
N1 0.0353(8) 0.0203(7) 0.0220(6) 0.000 0.0081(6) 0.000
C1 0.0486(12) 0.0344(10) 0.0217(8) 0.000 0.0080(7) 0.000
C2 0.0422(8) 0.0253(6) 0.0265(6) 0.0000(5) 0.0059(5) 0.0048(5)
C3 0.0303(6) 0.0192(5) 0.0267(5) 0.0018(4) 0.0036(4) 0.0007(4)
C4 0.0410(7) 0.0210(6) 0.0312(6) 0.0050(5) 0.0048(5) -0.0027(5)
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 5_655 . 180.0 ?
O3 Mg1 O4 5_655 5_655 90.0 ?
O3 Mg1 O4 . 5_655 90.0 ?
O3 Mg1 O4 5_655 . 90.0 ?
O3 Mg1 O4 . . 90.0 ?
O4 Mg1 O4 5_655 . 180.00(8) ?
O3 Mg1 O5 5_655 5_655 90.0 ?
O3 Mg1 O5 . 5_655 90.0 ?
O4 Mg1 O5 5_655 5_655 91.46(6) ?
O4 Mg1 O5 . 5_655 88.54(6) ?
O3 Mg1 O5 5_655 . 90.0 ?
O3 Mg1 O5 . . 90.0 ?
O4 Mg1 O5 5_655 . 88.54(6) ?
O4 Mg1 O5 . . 91.46(6) ?
O5 Mg1 O5 5_655 . 180.00(8) ?
Mg1 O3 H3 . . 126.6(13) ?
Mg1 O4 H4 . . 125.5(14) ?
Mg1 O5 H5 . . 109.1(13) ?
C3 N1 C3 6_565 . 125.46(15) ?
C3 N1 H1A 6_565 . 117.27(8) ?
C3 N1 H1A . . 117.27(8) ?
C2 C1 C2 . 6_565 120.82(17) ?
C2 C1 H1 . . 119.6 ?
C2 C1 H1 6_565 . 119.6 ?
C3 C2 C1 . . 118.87(12) ?
C3 C2 H2 . . 120.6 ?
C1 C2 H2 . . 120.6 ?
N1 C3 C2 . . 117.99(12) ?
N1 C3 C4 . . 114.17(11) ?
C2 C3 C4 . . 127.84(11) ?
O2 C4 O1 . . 128.49(12) ?
O2 C4 C3 . . 117.37(12) ?
O1 C4 C3 . . 114.14(11) ?
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 5_655 2.0197(14) ?
Mg1 O3 . 2.0197(14) ?
Mg1 O4 5_655 2.0601(15) ?
Mg1 O4 . 2.0601(15) ?
Mg1 O5 5_655 2.1375(16) ?
Mg1 O5 . 2.1375(16) ?
O1 C4 . 1.2422(17) ?
O2 C4 . 1.2406(16) ?
O3 H3 . 0.862(19) ?
O4 H4 . 0.85(2) ?
O5 H5 . 0.89(2) ?
N1 C3 6_565 1.3401(13) ?
N1 C3 . 1.3401(13) ?
N1 H1A . 0.89(3) ?
C1 C2 . 1.3897(16) ?
C1 C2 6_565 1.3897(16) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.3788(17) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.5208(17) ?
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
_geom_hbond_publ_flag
O3 H3 O1 . 0.862(19) 1.834(19) 2.6940(14) 174.6(19) yes
O4 H4 O2 . 0.85(2) 1.93(2) 2.7758(14) 171(2) yes
O5 H5 O2 1_554 0.89(2) 1.92(2) 2.7960(14) 167.5(19) yes
C1 H1 O5 4_556 0.93 2.58 3.308(3) 135.8 yes
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
C2 C1 C2 C3 6_565 . . . -0.3(3) ?
C3 N1 C3 C2 6_565 . . . -0.3(3) ?
C3 N1 C3 C4 6_565 . . . 179.77(12) ?
C1 C2 C3 N1 . . . . 0.3(2) ?
C1 C2 C3 C4 . . . . -179.83(15) ?
N1 C3 C4 O2 . . . . -178.85(14) ?
C2 C3 C4 O2 . . . . 1.3(2) ?
N1 C3 C4 O1 . . . . 1.23(19) ?
C2 C3 C4 O1 . . . . -178.66(14) ?
