#------------------------------------------------------------------------------
#$Date: 2016-02-20 21:30:07 +0100 (Sat 20 de Feb de 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/94/2229439.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_2229439
loop_
_publ_author_name
'Starosta, Wojciech'
'Leciejewicz, Janusz'
_publ_section_title
;
 trans-Tetraaquabis(pyridazine-4-carboxylato-κO)magnesium(II)
 dihydrate
;
_journal_coeditor_code           KP2307
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m316
_journal_paper_doi               10.1107/S1600536811004168
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Mg (C5 H3 N2 O2)2 (H 2O)4], 2H2O'
_chemical_formula_moiety         'C10 H14 Mg N4 O8, 2(H2 O)'
_chemical_formula_sum            'C10 H18 Mg N4 O10'
_chemical_formula_weight         378.59
_chemical_name_common            'Magnesium pyridazinate hydrate'
_chemical_name_systematic
;
trans-Tetraaquabis(pyridazine-4-carboxylato-κO)magnesium(II)
dihydrate
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 108.36(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.2571(15)
_cell_length_b                   11.688(2)
_cell_length_c                   10.550(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      6
_cell_volume                     849.3(3)
_computing_cell_refinement       'KM-4 Software (Kuma, 1996)'
_computing_data_collection       'KM-4 Software (Kuma, 1996)'
_computing_data_reduction        'DATAPROC (Kuma, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Kuma KM-4 four-circle'
_diffrn_measurement_method       'profile data from 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  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2007
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.71
_diffrn_reflns_theta_min         2.68
_diffrn_standards_decay_%        1.25
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.164
_exptl_absorpt_correction_T_max  0.98655
_exptl_absorpt_correction_T_min  0.96836
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.238
_exptl_crystal_size_mid          0.223
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         1873
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0628P)²+0.2930P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1219
_reflns_number_gt                1136
_reflns_number_total             1873
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            kp2307.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2229439
_cod_database_fobs_code          2229439
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.5000 0.5000 0.0236(3) Uani d S 1 . .
O O1 0.3810(2) 0.54000(14) 0.29844(14) 0.0318(4) Uani d . 1 . .
O O2 0.2156(3) 0.38329(15) 0.20927(16) 0.0453(5) Uani d . 1 . .
N N1 0.2554(3) 0.58217(18) -0.19230(18) 0.0339(5) Uani d . 1 . .
C C7 0.2921(3) 0.47760(19) 0.2019(2) 0.0284(5) Uani d . 1 . .
N N2 0.1945(3) 0.47789(17) -0.16963(18) 0.0336(5) Uani d . 1 . .
C C5 0.3386(3) 0.62622(19) 0.0395(2) 0.0311(5) Uani d . 1 . .
H H5 0.3895 0.6782 0.1084 0.037 Uiso calc R 1 . .
C C4 0.2765(3) 0.52021(19) 0.0639(2) 0.0260(5) Uani d . 1 . .
C C3 0.2036(3) 0.4491(2) -0.0472(2) 0.0312(5) Uani d . 1 . .
H H3 0.1587 0.3770 -0.0338 0.037 Uiso calc R 1 . .
C C6 0.3231(4) 0.6534(2) -0.0916(2) 0.0344(5) Uani d . 1 . .
H H6 0.3626 0.7257 -0.1092 0.041 Uiso calc R 1 . .
O O4 0.2870(2) 0.59132(16) 0.54856(16) 0.0347(4) Uani d D 1 . .
O O5 0.9316(3) 0.67116(16) 0.38743(16) 0.0358(4) Uani d D 1 . .
O O3 0.6662(3) 0.64863(14) 0.52618(17) 0.0338(4) Uani d D 1 . .
H H31 0.751(4) 0.642(3) 0.489(3) 0.056(10) Uiso d D 1 . .
H H42 0.267(5) 0.586(3) 0.620(2) 0.058(10) Uiso d D 1 . .
H H51 0.896(4) 0.628(2) 0.323(2) 0.041(8) Uiso d D 1 . .
H H32 0.711(5) 0.656(3) 0.6052(19) 0.062(10) Uiso d D 1 . .
H H52 0.905(5) 0.7357(18) 0.360(3) 0.065(11) Uiso d D 1 . .
H H41 0.187(3) 0.614(2) 0.498(3) 0.048(9) Uiso d D 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 0.0276(5) 0.0249(5) 0.0176(5) -0.0002(4) 0.0061(4) 0.0006(4)
O1 0.0389(9) 0.0329(8) 0.0207(7) -0.0020(7) 0.0052(6) -0.0005(6)
O2 0.0681(13) 0.0384(10) 0.0276(8) -0.0184(9) 0.0126(8) -0.0026(7)
N1 0.0380(11) 0.0409(11) 0.0239(9) 0.0057(9) 0.0111(8) 0.0042(8)
C7 0.0290(11) 0.0335(12) 0.0221(10) 0.0032(9) 0.0073(9) -0.0013(8)
N2 0.0374(11) 0.0386(11) 0.0221(9) 0.0020(8) 0.0056(8) -0.0031(7)
C5 0.0363(12) 0.0314(12) 0.0242(10) 0.0000(9) 0.0077(9) -0.0046(9)
C4 0.0223(10) 0.0325(12) 0.0221(10) 0.0044(8) 0.0052(8) -0.0014(8)
C3 0.0353(12) 0.0309(12) 0.0252(11) 0.0003(10) 0.0063(9) -0.0028(9)
C6 0.0408(13) 0.0328(12) 0.0305(11) 0.0024(10) 0.0125(10) 0.0013(10)
O4 0.0337(9) 0.0476(10) 0.0230(8) 0.0114(8) 0.0091(7) 0.0051(7)
O5 0.0403(10) 0.0352(10) 0.0269(8) 0.0016(8) 0.0035(7) -0.0006(7)
O3 0.0407(10) 0.0342(9) 0.0276(9) -0.0055(7) 0.0123(8) 0.0010(7)
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'
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 Mg1 O4 3_666 . 180.00(6) ?
O4 Mg1 O1 3_666 3_666 92.02(7) ?
O4 Mg1 O1 . 3_666 87.99(7) ?
O4 Mg1 O1 3_666 . 87.98(7) ?
O4 Mg1 O1 . . 92.02(7) ?
O1 Mg1 O1 3_666 . 180.0 ?
O4 Mg1 O3 3_666 . 90.95(7) ?
O4 Mg1 O3 . . 89.05(7) ?
O1 Mg1 O3 3_666 . 90.88(7) ?
O1 Mg1 O3 . . 89.12(7) ?
O4 Mg1 O3 3_666 3_666 89.05(7) ?
O4 Mg1 O3 . 3_666 90.95(7) ?
O1 Mg1 O3 3_666 3_666 89.12(7) ?
O1 Mg1 O3 . 3_666 90.88(7) ?
O3 Mg1 O3 . 3_666 180.0000(10) ?
O4 Mg1 H32 3_666 . 95.0(8) ?
O4 Mg1 H32 . . 85.0(8) ?
O1 Mg1 H32 3_666 . 72.6(6) ?
O1 Mg1 H32 . . 107.4(6) ?
O3 Mg1 H32 . . 18.6(6) ?
O3 Mg1 H32 3_666 . 161.4(6) ?
C7 O1 Mg1 . . 129.89(15) ?
C6 N1 N2 . . 119.35(19) ?
O2 C7 O1 . . 126.0(2) ?
O2 C7 C4 . . 116.88(19) ?
O1 C7 C4 . . 117.1(2) ?
C3 N2 N1 . . 119.28(19) ?
C4 C5 C6 . . 117.8(2) ?
C4 C5 H5 . . 121.1 ?
C6 C5 H5 . . 121.1 ?
C5 C4 C3 . . 116.1(2) ?
C5 C4 C7 . . 123.40(19) ?
C3 C4 C7 . . 120.4(2) ?
N2 C3 C4 . . 124.0(2) ?
N2 C3 H3 . . 118.0 ?
C4 C3 H3 . . 118.0 ?
N1 C6 C5 . . 123.5(2) ?
N1 C6 H6 . . 118.3 ?
C5 C6 H6 . . 118.3 ?
Mg1 O4 H42 . . 123(2) ?
Mg1 O4 H41 . . 127(2) ?
H42 O4 H41 . . 105(3) ?
H51 O5 H52 . . 108(3) ?
Mg1 O3 H31 . . 110(2) ?
Mg1 O3 H32 . . 105(2) ?
H31 O3 H32 . . 112(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 O4 3_666 2.0714(17) ?
Mg1 O4 . 2.0714(17) ?
Mg1 O1 3_666 2.0807(16) ?
Mg1 O1 . 2.0807(16) ?
Mg1 O3 . 2.0829(17) ?
Mg1 O3 3_666 2.0829(17) ?
Mg1 H32 . 2.42(3) ?
O1 C7 . 1.254(3) ?
O2 C7 . 1.248(3) ?
N1 C6 . 1.317(3) ?
N1 N2 . 1.343(3) ?
C7 C4 . 1.509(3) ?
N2 C3 . 1.316(3) ?
C5 C4 . 1.370(3) ?
C5 C6 . 1.389(3) ?
C5 H5 . 0.9300 ?
C4 C3 . 1.398(3) ?
C3 H3 . 0.9300 ?
C6 H6 . 0.9300 ?
O4 H42 . 0.809(18) ?
O4 H41 . 0.798(18) ?
O5 H51 . 0.819(17) ?
O5 H52 . 0.809(18) ?
O3 H31 . 0.828(18) ?
O3 H32 . 0.799(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
O3 H31 O5 . 0.828(18) 1.97(2) 2.775(3) 164(3)
O4 H42 N1 1_556 0.809(18) 2.013(19) 2.817(2) 172(3)
O5 H51 N2 3_665 0.819(17) 1.979(18) 2.798(3) 179(3)
O3 H32 O2 3_666 0.799(18) 1.92(2) 2.675(2) 159(3)
O5 H52 O2 2_655 0.809(18) 1.968(19) 2.765(3) 168(3)
O4 H41 O5 1_455 0.798(18) 1.970(18) 2.766(3) 175(3)
