#------------------------------------------------------------------------------
#$Date: 2011-09-17 21:27:16 +0100 (Sat, 17 Sep 2011) $
#$Revision: 26029 $
#$URL: svn://www.crystallography.net/cod/cif/2/2206769.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_2206769
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_[local]_cod_cif_authors_sg_H-M  'P 21/n'
loop_
_publ_author_name
'Liu, Ying'
'Dou, Jianmin'
'Wang, Daqi'
'Li, Dacheng'
_publ_section_title
;
Poly[diaquabis(\m~3~-malonato)(\m-pyrazine)dinickel(II)]
;
_journal_coeditor_code           OB6558
_journal_issue                   9
_journal_name_full               'Acta Crystallographica, Section E'
_journal_page_first              m1834
_journal_page_last               m1836
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Ni2 (C3 H2 O4)2 (C4 H4 N2) (H2 O)2]'
_chemical_formula_moiety         'C10 H12 N2 Ni2 O10'
_chemical_formula_sum            'C10 H12 N2 Ni2 O10'
_chemical_formula_weight         437.6
_chemical_name_systematic
;
Poly[diaquabis(\m~3~-malonato)(\m-pyrazine)dinickel(II)]
;
_symmetry_cell_setting           monoclinic
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.181(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.9783(5)
_cell_length_b                   14.5612(9)
_cell_length_c                   7.3348(5)
_cell_measurement_reflns_used    1338
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.16
_cell_measurement_theta_min      1.71
_cell_volume                     744.77(9)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2429
_diffrn_reflns_theta_full        25.16
_diffrn_reflns_theta_max         25.16
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    2.585
_exptl_absorpt_correction_T_max  0.426
_exptl_absorpt_correction_T_min  0.375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.951
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.396
_refine_ls_extinction_coef       0.018(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997a)'
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         1338
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0643P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0893
_reflns_number_gt                1118
_reflns_number_total             1338
_reflns_threshold_expression     I>2\s(I)
_[local]_cod_data_source_file    ob6558.cif
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
Ni1 0.66238(5) 0.69131(3) -0.08101(5) 0.0187(2) Uani d D 1 Ni
C1 0.4150(5) 0.6682(2) 0.2436(4) 0.0262(7) Uani d . 1 C
C2 0.3873(6) 0.6085(3) 0.4106(5) 0.0337(8) Uani d D 1 C
C3 0.9173(5) 0.8403(2) 0.0878(4) 0.0260(7) Uani d . 1 C
C4 1.0475(5) 0.5745(3) -0.0907(6) 0.0415(10) Uani d D 1 C
C5 0.8212(5) 0.4954(3) 0.0546(5) 0.0382(9) Uani d D 1 C
N1 0.8671(4) 0.57184(19) -0.0373(4) 0.0293(6) Uani d . 1 N
O1 0.5251(3) 0.62248(17) -0.2949(3) 0.0330(6) Uani d . 1 O
O2 0.8363(3) 0.75257(17) -0.2697(3) 0.0328(6) Uani d . 1 O
O3 0.4672(4) 0.81041(18) -0.0870(3) 0.0371(6) Uani d D 1 O
O4 0.8300(3) 0.7640(2) 0.1097(3) 0.0362(6) Uani d . 1 O
O5 0.5142(3) 0.63277(17) 0.1252(3) 0.0334(6) Uani d . 1 O
H1 1.074(6) 0.622(2) -0.156(5) 0.059(13) Uiso d D 1 H
H2 0.703(3) 0.495(3) 0.096(4) 0.039(10) Uiso d D 1 H
H3 0.465(4) 0.5595(19) 0.408(5) 0.042(11) Uiso d D 1 H
H4 0.271(3) 0.584(3) 0.407(7) 0.070(16) Uiso d D 1 H
H5 0.388(5) 0.797(3) -0.004(5) 0.055(14) Uiso d D 1 H
H6 0.409(8) 0.802(5) -0.190(4) 0.059(13) Uiso d D 1 H
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
Ni1 0.0229(3) 0.0177(3) 0.0157(3) -0.00064(15) 0.00199(16) 0.00056(15)
C1 0.0295(16) 0.0246(19) 0.0246(16) -0.0007(14) 0.0019(13) -0.0041(14)
C2 0.053(2) 0.024(2) 0.0239(17) 0.0054(18) 0.0030(15) 0.0010(15)
C3 0.0305(16) 0.0230(19) 0.0247(16) -0.0020(15) 0.0032(13) -0.0051(14)
C4 0.038(2) 0.034(2) 0.054(2) 0.0056(17) 0.0166(17) 0.0159(19)
C5 0.0317(18) 0.029(2) 0.055(2) 0.0014(16) 0.0129(17) 0.0089(18)
N1 0.0305(14) 0.0263(16) 0.0312(15) 0.0016(12) 0.0016(11) 0.0009(13)
O1 0.0423(13) 0.0255(13) 0.0306(12) 0.0016(11) -0.0055(10) 0.0028(11)
O2 0.0448(14) 0.0288(15) 0.0256(12) -0.0079(11) 0.0105(10) -0.0027(10)
O3 0.0398(14) 0.0416(17) 0.0303(14) 0.0022(11) 0.0046(11) 0.0016(11)
O4 0.0469(15) 0.0352(16) 0.0261(12) -0.0122(12) -0.0048(10) 0.0040(11)
O5 0.0395(12) 0.0294(14) 0.0324(13) 0.0033(11) 0.0149(10) -0.0003(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
Ni1 O5 . 2.050(2) yes
Ni1 O1 . 2.066(2) yes
Ni1 O2 . 2.076(2) yes
Ni1 O4 . 2.079(2) yes
Ni1 O3 . 2.205(3) yes
Ni1 N1 . 2.266(3) yes
Ni1 H6 . 2.50(5) ?
C1 O5 . 1.243(4) ?
C1 O2 4_576 1.280(4) ?
C1 C2 . 1.520(5) ?
C2 C3 4_576 1.506(5) ?
C2 H3 . 0.896(18) ?
C2 H4 . 0.886(19) ?
C3 O1 4_676 1.245(4) ?
C3 O4 . 1.280(5) ?
C3 C2 4_675 1.506(5) ?
C4 N1 . 1.334(4) ?
C4 C5 3_765 1.388(5) ?
C4 H1 . 0.87(2) ?
C5 N1 . 1.346(5) ?
C5 C4 3_765 1.388(5) ?
C5 H2 . 0.890(19) ?
O1 C3 4_575 1.245(4) ?
O2 C1 4_675 1.280(4) ?
O3 H6 . 0.85(2) ?
O3 H5 . 0.86(2) ?
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
O5 Ni1 O1 . . 97.24(10) yes
O5 Ni1 O2 . . 173.93(9) yes
O1 Ni1 O2 . . 88.19(10) yes
O5 Ni1 O4 . . 90.12(10) yes
O1 Ni1 O4 . . 172.21(9) yes
O2 Ni1 O4 . . 84.35(9) yes
O5 Ni1 O3 . . 90.76(9) yes
O1 Ni1 O3 . . 95.62(10) yes
O2 Ni1 O3 . . 91.43(10) yes
O4 Ni1 O3 . . 86.81(11) yes
O5 Ni1 N1 . . 84.79(9) yes
O1 Ni1 N1 . . 90.39(9) yes
O2 Ni1 N1 . . 92.46(10) yes
O4 Ni1 N1 . . 87.72(10) yes
O3 Ni1 N1 . . 172.94(10) yes
O5 Ni1 H6 . . 97.6(16) ?
O1 Ni1 H6 . . 76.6(11) ?
O2 Ni1 H6 . . 86.3(17) ?
O4 Ni1 H6 . . 105.0(13) ?
O3 Ni1 H6 . . 19.6(9) ?
N1 Ni1 H6 . . 167.0(11) ?
O5 C1 O2 . 4_576 124.7(3) ?
O5 C1 C2 . . 114.7(3) ?
O2 C1 C2 4_576 . 120.6(3) ?
C3 C2 C1 4_576 . 113.3(3) ?
C3 C2 H3 4_576 . 110(2) ?
C1 C2 H3 . . 110(2) ?
C3 C2 H4 4_576 . 109(3) ?
C1 C2 H4 . . 110(3) ?
H3 C2 H4 . . 104(2) ?
O1 C3 O4 4_676 . 124.6(3) ?
O1 C3 C2 4_676 4_675 116.2(3) ?
O4 C3 C2 . 4_675 119.1(3) ?
N1 C4 C5 . 3_765 123.1(3) ?
N1 C4 H1 . . 114(3) ?
C5 C4 H1 3_765 . 123(3) ?
N1 C5 C4 . 3_765 122.3(3) ?
N1 C5 H2 . . 115(3) ?
C4 C5 H2 3_765 . 123(3) ?
C4 N1 C5 . . 114.6(3) ?
C4 N1 Ni1 . . 122.2(2) ?
C5 N1 Ni1 . . 123.1(2) ?
C3 O1 Ni1 4_575 . 124.3(2) ?
C1 O2 Ni1 4_675 . 126.6(2) ?
Ni1 O3 H6 . . 100(4) ?
Ni1 O3 H5 . . 103(3) ?
H6 O3 H5 . . 107(4) ?
C3 O4 Ni1 . . 128.0(2) ?
C1 O5 Ni1 . . 130.8(2) ?
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 H5 O2 4_576 0.86(2) 1.91(4) 2.693(3) 151(4) yes
O3 H6 O4 4_575 0.85(2) 1.82(5) 2.623(3) 155(7) yes
_cod_database_code 2206769