#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/68/2206869.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_2206869
loop_
_publ_author_name
'Gryz Michał '
'Starosta Wojciech'
'Leciejewicz Janusz'
_publ_section_title
;
 Bis[hexaquamagnesium(II)] pyrazine-2,3,5,6-tetracarboxylate
 tetrahydrate
;
_journal_coeditor_code           BT6725
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1920
_journal_page_last               m1922
_journal_paper_doi               10.1107/S1600536805027406
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Mg (H2 O1)6]2 (C8 N2 O8), 4H2 O'
_chemical_formula_moiety         '2H12 Mg O6 2+, C8 N2 O8 2-, 4H2 O'
_chemical_formula_sum            'C8 H32 Mg2 N2 O24'
_chemical_formula_weight         588.98
_chemical_name_common            'magnesium pyrazinetetracarboxylate'
_chemical_name_systematic
;
Bis[hexaquamagnesium(II)] pyrazine-2,3,5,6-tetracarboxylate 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                102.95(3)
_cell_angle_beta                 103.29(3)
_cell_angle_gamma                100.02(3)
_cell_formula_units_Z            1
_cell_length_a                   6.7467(13)
_cell_length_b                   9.1779(18)
_cell_length_c                   10.731(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      6
_cell_volume                     612.2(3)
_computing_cell_refinement       'KM-4 Software'
_computing_data_collection       'KM-4 Software (Kuma, 1996)'
_computing_data_reduction        'DATAPROC (Kuma, 2001)'
_computing_molecular_graphics    'XP (Siemens, 1992)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Kuma KM-4 four-circle'
_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  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3839
_diffrn_reflns_theta_full        30.09
_diffrn_reflns_theta_max         30.09
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        3.05
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.206
_exptl_absorpt_correction_T_max  0.97720
_exptl_absorpt_correction_T_min  0.95512
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             310
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.558
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3565
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0419
_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)+(0.0859P)²+0.0954P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1271
_refine_ls_wR_factor_ref         0.1374
_reflns_number_gt                2752
_reflns_number_total             3565
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bt6725.cif
_cod_data_source_block           I
_cod_original_cell_volume        612.2(2)
_cod_database_code               2206869
_cod_database_fobs_code          2206869
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
Mg1 0.10048(7) 0.38447(5) 0.74376(5) 0.02107(14) Uani d . 1 Mg
O12 -0.1200(2) 0.38242(14) 0.84634(14) 0.0353(3) Uani d . 1 O
O14 0.33647(18) 0.40732(15) 0.65134(13) 0.0337(3) Uani d . 1 O
O16 -0.1000(2) 0.44752(15) 0.59307(12) 0.0349(3) Uani d D 1 O
H162 -0.146(4) 0.526(2) 0.618(2) 0.052 Uiso d D 1 H
H161 -0.128(3) 0.429(2) 0.5161(16) 0.052 Uiso d D 1 H
O13 0.22688(19) 0.61361(14) 0.85011(14) 0.0355(3) Uani d . 1 O
O11 0.2736(2) 0.29726(17) 0.87786(13) 0.0389(3) Uani d . 1 O
O15 -0.0305(2) 0.16429(13) 0.62377(13) 0.0331(3) Uani d . 1 O
C6 1.11871(19) 0.12801(13) 0.09160(12) 0.0175(2) Uani d . 1 C
N1 0.93117(16) 0.13464(12) 0.02238(11) 0.0194(2) Uani d . 1 N
O4 1.33092(17) 0.37946(12) 0.15286(11) 0.0274(2) Uani d . 1 O
O3 1.23274(18) 0.29073(13) 0.31122(11) 0.0302(2) Uani d . 1 O
C8 1.24105(19) 0.27660(14) 0.19462(13) 0.0198(2) Uani d . 1 C
C2 0.81111(18) 0.00722(14) -0.06940(13) 0.0183(2) Uani d . 1 C
C7 0.5984(2) 0.01594(15) -0.14738(14) 0.0227(3) Uani d . 1 C
O21 0.90832(19) 0.09816(14) 0.35451(12) 0.0308(2) Uani d . 1 O
O1 0.57634(17) 0.14607(13) -0.15418(14) 0.0348(3) Uani d . 1 O
O2 0.46520(18) -0.10839(14) -0.19901(15) 0.0434(4) Uani d . 1 O
O22 0.5024(3) 0.1799(3) 0.50952(17) 0.0796(7) Uani d D 1 O
H222 0.6140 0.2569 0.5319 0.119 Uiso d D 1 H
H221 0.4601 0.1692 0.4188 0.119 Uiso d D 1 H
H112 0.300(4) 0.324(3) 0.963(3) 0.046(6) Uiso d . 1 H
H142 0.377(4) 0.326(3) 0.611(3) 0.054(7) Uiso d . 1 H
H212 0.790(5) 0.101(3) 0.300(3) 0.055(7) Uiso d . 1 H
H111 0.358(6) 0.241(4) 0.863(4) 0.080(10) Uiso d . 1 H
H151 -0.057(4) 0.140(3) 0.542(3) 0.039(6) Uiso d . 1 H
H141 0.463(5) 0.478(4) 0.707(3) 0.065(9) Uiso d . 1 H
H131 0.349(6) 0.666(4) 0.844(4) 0.081(10) Uiso d . 1 H
H152 0.017(5) 0.091(3) 0.645(3) 0.055(7) Uiso d . 1 H
H122 -0.202(5) 0.302(4) 0.850(3) 0.074(9) Uiso d . 1 H
H132 0.179(5) 0.673(4) 0.905(3) 0.067(8) Uiso d . 1 H
H121 -0.185(5) 0.454(3) 0.854(3) 0.055(7) Uiso d . 1 H
H211 0.992(5) 0.159(3) 0.339(3) 0.057(8) Uiso d . 1 H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mg Mg 0.0486 0.0363 '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'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 '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
O11 Mg1 O12 . . 89.20(6) yes
O11 Mg1 O15 . . 88.92(7) ?
O12 Mg1 O15 . . 94.29(6) ?
O11 Mg1 O14 . . 90.84(6) ?
O12 Mg1 O14 . . 174.61(6) ?
O15 Mg1 O14 . . 91.09(6) yes
O11 Mg1 O13 . . 95.64(7) ?
O12 Mg1 O13 . . 87.90(6) yes
O15 Mg1 O13 . . 174.97(6) yes
O14 Mg1 O13 . . 86.74(6) yes
O11 Mg1 O16 . . 173.12(6) ?
O12 Mg1 O16 . . 89.93(6) ?
O15 Mg1 O16 . . 84.34(6) yes
O14 Mg1 O16 . . 90.67(6) ?
O13 Mg1 O16 . . 91.14(6) ?
Mg1 O12 H122 . . 126(2) ?
Mg1 O12 H121 . . 120.3(19) ?
H122 O12 H121 . . 107(3) ?
Mg1 O14 H142 . . 121.9(18) ?
Mg1 O14 H141 . . 113.5(18) ?
H142 O14 H141 . . 105(3) ?
Mg1 O16 H162 . . 116.6(17) ?
Mg1 O16 H161 . . 136.7(19) ?
H162 O16 H161 . . 105(2) ?
Mg1 O13 H131 . . 121(2) ?
Mg1 O13 H132 . . 129(2) ?
H131 O13 H132 . . 110(3) ?
Mg1 O11 H112 . . 128.1(18) ?
Mg1 O11 H111 . . 127(2) ?
H112 O11 H111 . . 104(3) ?
Mg1 O15 H151 . . 123.9(16) ?
Mg1 O15 H152 . . 119.0(19) ?
H151 O15 H152 . . 104(2) ?
N1 C6 C2 . 2_755 121.42(11) ?
N1 C6 C8 . . 114.00(11) ?
C2 C6 C8 2_755 . 124.57(11) ?
C6 N1 C2 . . 117.87(11) ?
O3 C8 O4 . . 125.59(12) ?
O3 C8 C6 . . 117.64(12) ?
O4 C8 C6 . . 116.57(12) ?
N1 C2 C6 . 2_755 120.71(11) ?
N1 C2 C7 . . 117.45(11) ?
C6 C2 C7 2_755 . 121.84(11) ?
O2 C7 O1 . . 127.18(13) ?
O2 C7 C2 . . 116.19(12) ?
O1 C7 C2 . . 116.62(12) ?
H212 O21 H211 . . 102(3) ?
H222 O22 H221 . . 98.9(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
Mg1 O11 . 2.0359(14) yes
Mg1 O12 . 2.0437(13) yes
Mg1 O15 . 2.0523(15) yes
Mg1 O14 . 2.0654(13) yes
Mg1 O13 . 2.0748(15) yes
Mg1 O16 . 2.1130(14) yes
O12 H122 . 0.86(4) ?
O12 H121 . 0.85(3) ?
O14 H142 . 0.90(3) ?
O14 H141 . 0.95(3) ?
O16 H162 . 0.848(16) ?
O16 H161 . 0.776(16) ?
O13 H131 . 0.90(4) ?
O13 H132 . 0.86(3) ?
O11 H112 . 0.86(3) ?
O11 H111 . 0.85(4) ?
O15 H151 . 0.83(3) ?
O15 H152 . 0.85(3) ?
C6 N1 . 1.3310(16) ?
C6 C2 2_755 1.3947(16) ?
C6 C8 . 1.5088(18) ?
N1 C2 . 1.3346(17) ?
O4 C8 . 1.2550(17) ?
O3 C8 . 1.2440(18) ?
C2 C6 2_755 1.3947(16) ?
C2 C7 . 1.5113(17) ?
C7 O2 . 1.2440(18) ?
C7 O1 . 1.2449(17) ?
O21 H212 . 0.88(3) ?
O21 H211 . 0.79(3) ?
O22 H222 . 0.883(3) ?
O22 H221 . 0.9266(18) ?
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
O11 H112 O4 1_456 0.86(3) 1.94(3) 2.7935(18) 174(2) yes
O11 H111 O1 1_556 0.85(4) 1.86(4) 2.7037(18) 171(3) yes
O12 H121 O4 2_666 0.85(3) 1.97(3) 2.8074(17) 172(3) yes
O12 H122 O1 1_456 0.86(4) 1.86(4) 2.7103(19) 168(3) yes
O13 H132 N1 2_666 0.86(3) 2.10(3) 2.9084(18) 156(3) yes
O13 H131 O2 1_566 0.90(4) 2.27(4) 2.990(2) 136(3) no
O13 H131 O4 2_766 0.90(4) 2.26(4) 2.9806(17) 136(3) no
O14 H142 O22 . 0.90(3) 1.96(3) 2.846(2) 167(3) yes
O14 H141 O4 2_766 0.95(3) 1.85(3) 2.782(2) 165(3) yes
O15 H151 O21 1_455 0.83(3) 1.91(3) 2.7323(19) 174(2) yes
O15 H152 O21 2_656 0.85(3) 1.89(3) 2.7185(18) 165(3) yes
O16 H162 O3 2_666 0.848(16) 1.928(16) 2.7739(18) 175(3) yes
O16 H161 O16 2_566 0.776(16) 2.415(10) 2.896(3) 121.4(11) no
O21 H211 O3 . 0.79(3) 1.98(3) 2.7604(19) 171(3) no
O21 H212 O2 2_655 0.88(3) 1.83(3) 2.7135(18) 175(3) yes
O22 H221 O3 1_455 0.9266(18) 2.2996(14) 2.951(2) 126.93(12) no
O22 H221 O2 2_655 0.9266(18) 2.4865(18) 3.315(3) 148.89(12) no
O22 H222 O16 1_655 0.883(3) 2.2234(17) 3.106(3) 178.19(14) ' '
