#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/20/2222098.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_2222098
loop_
_publ_author_name
'Starosta, Wojciech'
'Leciejewicz, Janusz'
_publ_section_title
;trans-Diaquabis(6-methoxycarbonylpyridazine-3-carboxylato-κ²N,O)zinc(II)
 dihydrate
;
_journal_coeditor_code           LH2816
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m640
_journal_paper_doi               10.1107/S1600536809017115
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Zn (C7 H5 N2 O4)2 (H2 O)2] , 2H2 O'
_chemical_formula_moiety         'C14 H14 N4 O10 Zn , 2H2 O'
_chemical_formula_sum            'C14 H18 N4 O12 Zn'
_chemical_formula_weight         499.69
_chemical_name_systematic
;
trans-Diaquabis(6-methoxycarbonylpyridazine-3-carboxylato-
κ²N,O)zinc(II) dihydrate
;
_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           SHELXL97
_cell_angle_alpha                102.99(3)
_cell_angle_beta                 108.90(3)
_cell_angle_gamma                94.97(3)
_cell_formula_units_Z            1
_cell_length_a                   6.3678(13)
_cell_length_b                   8.3178(17)
_cell_length_c                   9.7717(19)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      6
_cell_volume                     469.9(2)
_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  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Kuma KM4 four-circle'
_diffrn_measurement_method       'profile data from ω/2θ 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  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2787
_diffrn_reflns_theta_full        30.07
_diffrn_reflns_theta_max         30.07
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.383
_exptl_absorpt_correction_T_max  0.94171
_exptl_absorpt_correction_T_min  0.69869
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             256
_exptl_crystal_size_max          0.312
_exptl_crystal_size_mid          0.253
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.754
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         2595
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0761P)²+0.0253P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1005
_reflns_number_gt                2235
_reflns_number_total             2595
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            lh2816.cif
_cod_data_source_block           I
_cod_original_cell_volume        469.93(17)
_cod_database_code               2222098
_cod_database_fobs_code          2222098
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
Zn Zn1 0.5000 0.5000 0.5000 0.02700(11) Uani d S 1 . .
O O11 0.8125(2) 0.43757(16) 0.58939(15) 0.0313(3) Uani d . 1 . .
O O12 1.0055(2) 0.22915(17) 0.57098(18) 0.0371(3) Uani d . 1 . .
N N11 0.2403(2) 0.15325(19) 0.29574(15) 0.0255(3) Uani d . 1 . .
N N12 0.4382(2) 0.24189(17) 0.39017(15) 0.0235(3) Uani d . 1 . .
C C17 0.8332(3) 0.2900(2) 0.53776(18) 0.0253(3) Uani d . 1 . .
C C13 0.6217(3) 0.1734(2) 0.42383(17) 0.0226(3) Uani d . 1 . .
C C14 0.6202(3) 0.0068(2) 0.36089(19) 0.0278(3) Uani d . 1 . .
H H14 0.7511 -0.0393 0.3832 0.033 Uiso calc R 1 . .
O O1 0.4013(2) 0.44171(18) 0.67752(15) 0.0326(3) Uani d . 1 . .
H H11 0.382(6) 0.535(5) 0.738(4) 0.060(9) Uiso d . 1 . .
O O21 -0.1599(2) -0.0300(2) 0.10069(19) 0.0436(3) Uani d . 1 . .
C C16 0.2308(3) -0.0079(2) 0.23612(17) 0.0242(3) Uani d . 1 . .
C C18 -0.0011(3) -0.0981(2) 0.13509(17) 0.0272(3) Uani d . 1 . .
C C15 0.4172(3) -0.0876(2) 0.26422(19) 0.0297(3) Uani d . 1 . .
H H15 0.4048 -0.2008 0.2191 0.036 Uiso calc R 1 . .
O O22 -0.0035(2) -0.25921(17) 0.09206(16) 0.0378(3) Uani d . 1 . .
C C19 -0.2178(4) -0.3623(3) -0.0046(3) 0.0479(5) Uani d . 1 . .
H H191 -0.3354 -0.2966 -0.0089 0.072 Uiso calc R 1 . .
H H192 -0.2459 -0.4546 0.0346 0.072 Uiso calc R 1 . .
H H193 -0.2146 -0.4041 -0.1036 0.072 Uiso calc R 1 . .
O O2 0.1965(3) 0.6755(3) 0.8035(2) 0.0493(4) Uani d . 1 . .
H H12 0.274(5) 0.379(4) 0.639(3) 0.043(7) Uiso d . 1 . .
H H21 0.207(6) 0.765(5) 0.830(4) 0.061(11) Uiso d . 1 . .
H H22 0.054(7) 0.622(6) 0.738(4) 0.074(10) 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'
Zn Zn 0.2839 1.4301 '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 Zn1 O11 . 2_666 180.0 ?
O11 Zn1 N12 . 2_666 101.21(6) ?
O11 Zn1 N12 2_666 2_666 78.79(6) ?
O11 Zn1 N12 . . 78.79(6) ?
O11 Zn1 N12 2_666 . 101.21(6) ?
N12 Zn1 N12 2_666 . 180.0 ?
O11 Zn1 O1 . 2_666 89.08(6) ?
O11 Zn1 O1 2_666 2_666 90.91(6) ?
N12 Zn1 O1 2_666 2_666 89.79(6) ?
N12 Zn1 O1 . 2_666 90.20(6) ?
O11 Zn1 O1 . . 90.92(6) ?
O11 Zn1 O1 2_666 . 89.08(6) ?
N12 Zn1 O1 2_666 . 90.21(6) ?
N12 Zn1 O1 . . 89.80(6) ?
O1 Zn1 O1 2_666 . 180.00(6) ?
C17 O11 Zn1 . . 116.33(11) ?
C16 N11 N12 . . 117.85(14) ?
C13 N12 N11 . . 121.74(14) ?
C13 N12 Zn1 . . 112.69(11) ?
N11 N12 Zn1 . . 125.56(11) ?
O12 C17 O11 . . 126.85(16) ?
O12 C17 C13 . . 116.54(15) ?
O11 C17 C13 . . 116.61(14) ?
N12 C13 C14 . . 122.16(15) ?
N12 C13 C17 . . 115.37(14) ?
C14 C13 C17 . . 122.46(14) ?
C15 C14 C13 . . 117.11(16) ?
C15 C14 H14 . . 121.4 ?
C13 C14 H14 . . 121.4 ?
Zn1 O1 H11 . . 111(2) ?
Zn1 O1 H12 . . 108.5(18) ?
H11 O1 H12 . . 106(3) ?
N11 C16 C15 . . 123.58(15) ?
N11 C16 C18 . . 113.77(15) ?
C15 C16 C18 . . 122.66(15) ?
O21 C18 O22 . . 125.50(16) ?
O21 C18 C16 . . 123.73(16) ?
O22 C18 C16 . . 110.77(15) ?
C14 C15 C16 . . 117.52(16) ?
C14 C15 H15 . . 121.2 ?
C16 C15 H15 . . 121.2 ?
C18 O22 C19 . . 116.76(16) ?
O22 C19 H191 . . 109.5 ?
O22 C19 H192 . . 109.5 ?
H191 C19 H192 . . 109.5 ?
O22 C19 H193 . . 109.5 ?
H191 C19 H193 . . 109.5 ?
H192 C19 H193 . . 109.5 ?
H21 O2 H22 . . 114(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
Zn1 O11 . 2.0617(13) ?
Zn1 O11 2_666 2.0617(13) ?
Zn1 N12 2_666 2.1118(15) ?
Zn1 N12 . 2.1118(15) ?
Zn1 O1 2_666 2.1612(14) ?
Zn1 O1 . 2.1612(14) ?
O11 C17 . 1.253(2) ?
O12 C17 . 1.227(2) ?
N11 C16 . 1.324(2) ?
N11 N12 . 1.3277(19) ?
N12 C13 . 1.323(2) ?
C17 C13 . 1.520(2) ?
C13 C14 . 1.382(2) ?
C14 C15 . 1.371(2) ?
C14 H14 . 0.9300 ?
O1 H11 . 0.90(4) ?
O1 H12 . 0.84(3) ?
O21 C18 . 1.192(2) ?
C16 C15 . 1.390(2) ?
C16 C18 . 1.500(2) ?
C18 O22 . 1.309(2) ?
C15 H15 . 0.9300 ?
O22 C19 . 1.445(2) ?
C19 H191 . 0.9600 ?
C19 H192 . 0.9600 ?
C19 H193 . 0.9600 ?
O2 H21 . 0.72(4) ?
O2 H22 . 0.93(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
O2 H22 O11 1_455 0.93(4) 1.99(4) 2.874(3) 158(4)
O2 H21 O21 2_566 0.72(4) 2.23(4) 2.940(3) 168(4)
O1 H12 O12 1_455 0.84(3) 1.86(3) 2.695(2) 174(3)
O1 H11 O2 . 0.90(4) 1.89(4) 2.720(2) 152(3)
