#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/24/2202401.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_2202401
loop_
_publ_author_name
'Shiu, Kom-Bei'
'Chen, Zheng-Wei'
'Liao, Fen-Ling'
'Wang, Sue-Lein'
_publ_section_title
;cis-Tetraaqua(η²-pyridine-2,5-dicarboxylato-κ²O,N)nickel(II)
 dihydrate
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1072
_journal_page_last               m1074
_journal_paper_doi               10.1107/S1600536803024383
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Ni (C7 H3 N O4) (H2 O)4], 2H2 O'
_chemical_formula_moiety         'C7 H11 N Ni O8, 2H2 O'
_chemical_formula_sum            'C7 H15 N Ni O10'
_chemical_formula_weight         331.91
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                107.1280(10)
_cell_angle_beta                 99.0390(10)
_cell_angle_gamma                102.7480(10)
_cell_formula_units_Z            2
_cell_length_a                   7.0177(5)
_cell_length_b                   8.3138(6)
_cell_length_c                   11.3906(8)
_cell_measurement_reflns_used    1951
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.5
_cell_volume                     601.60(7)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker SMART-CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0786
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6432
_diffrn_reflns_theta_full        25.69
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.664
_exptl_absorpt_correction_T_max  0.847
_exptl_absorpt_correction_T_min  0.733
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1995)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Tabular
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.348
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.817
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2857
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.817
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0207P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0518
_refine_ls_wR_factor_ref         0.0538
_reflns_number_gt                1894
_reflns_number_total             2857
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bt6372.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               2202401
_cod_database_fobs_code          2202401
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_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Ni1 0.29853(5) 0.09956(4) 0.28490(3) 0.02255(9) Uani d . 1 . . Ni
O1 0.0884(2) 0.24173(19) 0.31830(14) 0.0313(4) Uani d . 1 . . O
O2 0.2677(3) 0.13524(18) 0.11561(13) 0.0364(4) Uani d . 1 . . O
O3 0.5141(2) -0.02726(17) 0.24019(13) 0.0264(4) Uani d . 1 . . O
O4 0.5353(2) 0.32882(18) 0.36459(13) 0.0292(4) Uani d . 1 . . O
O5 0.3134(2) 0.07225(17) 0.45736(13) 0.0253(4) Uani d . 1 . . O
O6 0.1749(2) -0.09596(18) 0.55793(13) 0.0282(4) Uani d . 1 . . O
O7 -0.3715(2) -0.67513(18) -0.04316(13) 0.0309(4) Uani d . 1 . . O
O8 -0.2744(2) -0.46006(18) -0.11866(14) 0.0343(4) Uani d . 1 . . O
O9 0.5834(2) 0.37772(18) 0.62690(14) 0.0365(4) Uani d . 1 . . O
O10 0.2509(2) -0.12741(19) -0.09770(14) 0.0344(4) Uani d . 1 . . O
N1 0.0810(3) -0.1366(2) 0.23546(15) 0.0202(4) Uani d . 1 . . N
C1 0.0527(3) -0.1845(3) 0.33560(19) 0.0203(5) Uani d . 1 . . C
C2 -0.0890(3) -0.3346(3) 0.3258(2) 0.0259(5) Uani d . 1 . . C
C3 -0.2038(3) -0.4434(3) 0.2068(2) 0.0260(5) Uani d . 1 . . C
C4 -0.1725(3) -0.3986(3) 0.10192(19) 0.0216(5) Uani d . 1 . . C
C5 -0.0307(3) -0.2435(3) 0.12032(19) 0.0211(5) Uani d . 1 . . C
C6 0.1910(3) -0.0606(3) 0.4613(2) 0.0212(5) Uani d . 1 . . C
C7 -0.2839(3) -0.5204(3) -0.0307(2) 0.0237(5) Uani d . 1 . . C
H1A 0.0075 0.2228 0.2440 0.050 Uiso d . 1 . . H
H1B 0.0050 0.1932 0.3649 0.050 Uiso d . 1 . . H
H2A 0.2599 0.2367 0.1088 0.050 Uiso d . 1 . . H
H2B 0.2546 0.0624 0.0446 0.050 Uiso d . 1 . . H
H2C -0.1063 -0.3589 0.3995 0.050 Uiso d . 1 . . H
H3A 0.6165 -0.0151 0.3010 0.050 Uiso d . 1 . . H
H3B 0.4725 -0.1429 0.1886 0.050 Uiso d . 1 . . H
H3C -0.3158 -0.5443 0.2012 0.050 Uiso d . 1 . . H
H4A 0.5890 0.3344 0.4464 0.050 Uiso d . 1 . . H
H4B 0.5009 0.4342 0.3798 0.050 Uiso d . 1 . . H
H5A 0.0006 -0.2126 0.0411 0.050 Uiso d . 1 . . H
H9A 0.4954 0.2637 0.5979 0.050 Uiso d . 1 . . H
H9B 0.6211 0.3998 0.7071 0.050 Uiso d . 1 . . H
H10A 0.3102 -0.1960 -0.0583 0.050 Uiso d . 1 . . H
H10B 0.3606 -0.0873 -0.1414 0.050 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
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_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O1 Ni1 O3 174.32(6) yes
O2 Ni1 O5 175.81(7) yes
O4 Ni1 N1 169.62(6) yes
O2 Ni1 N1 99.76(7) ?
O5 Ni1 N1 80.00(6) ?
O2 Ni1 O3 88.92(6) ?
O5 Ni1 O3 95.27(6) ?
N1 Ni1 O3 91.47(6) ?
O2 Ni1 O4 90.34(6) ?
O5 Ni1 O4 90.09(6) ?
O3 Ni1 O4 86.32(6) ?
O2 Ni1 O1 86.03(6) ?
O5 Ni1 O1 89.80(6) ?
N1 Ni1 O1 91.95(6) ?
O4 Ni1 O1 91.10(6) ?
Ni1 O1 H1A 107.9 ?
Ni1 O1 H1B 108.3 ?
H1A O1 H1B 105.8 ?
Ni1 O2 H2A 121.1 ?
Ni1 O2 H2B 128.5 ?
H2A O2 H2B 110.3 ?
Ni1 O3 H3A 119.0 ?
Ni1 O3 H3B 118.7 ?
H3A O3 H3B 107.5 ?
Ni1 O4 H4A 106.6 ?
Ni1 O4 H4B 116.4 ?
H4A O4 H4B 101.7 ?
C6 O5 Ni1 116.43(13) ?
H9A O9 H9B 103.1 ?
H10A O10 H10B 100.5 ?
C1 N1 C5 118.10(18) ?
C1 N1 Ni1 112.76(13) ?
C5 N1 Ni1 129.14(15) ?
N1 C1 C2 122.96(19) ?
N1 C1 C6 114.74(18) ?
C2 C1 C6 122.3(2) ?
C1 C2 C3 118.4(2) ?
C1 C2 H2C 119.3 ?
C3 C2 H2C 122.3 ?
C2 C3 C4 119.4(2) ?
C2 C3 H3C 117.9 ?
C4 C3 H3C 122.4 ?
C5 C4 C3 118.53(18) ?
C5 C4 C7 120.3(2) ?
C3 C4 C7 121.07(19) ?
N1 C5 C4 122.6(2) ?
N1 C5 H5A 118.2 ?
C4 C5 H5A 119.0 ?
O6 C6 O5 125.33(19) ?
O6 C6 C1 118.67(19) ?
O5 C6 C1 115.99(19) ?
O8 C7 O7 125.6(2) ?
O8 C7 C4 117.42(19) ?
O7 C7 C4 116.9(2) ?
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 O1 . 2.0970(16) yes
Ni1 O2 . 2.0217(15) yes
Ni1 O3 . 2.0709(15) yes
Ni1 O5 . 2.0324(14) yes
Ni1 O4 . 2.0801(14) yes
Ni1 N1 . 2.0637(16) yes
O5 C6 . 1.258(2) yes
O6 C6 . 1.235(2) yes
O7 C7 . 1.253(2) yes
O8 C7 . 1.250(3) yes
N1 C1 . 1.343(3) ?
N1 C5 . 1.344(2) ?
C1 C2 . 1.376(3) ?
C1 C6 . 1.518(3) ?
C2 C3 . 1.385(3) ?
C3 C4 . 1.386(3) ?
C4 C5 . 1.381(3) ?
C4 C7 . 1.516(3) ?
C5 H5A . 1.0499 ?
O1 H1A . 0.8913 ?
O1 H1B . 0.9521 ?
O2 H2A . 0.8820 ?
O2 H2B . 0.8325 ?
O3 H3A . 0.8814 ?
O3 H3B . 0.9189 ?
O4 H4A . 0.9322 ?
O4 H4B . 0.9343 ?
O9 H9A . 0.9393 ?
O9 H9B . 0.8614 ?
O10 H10A . 0.9468 ?
O10 H10B . 1.0277 ?
C2 H2C . 0.9394 ?
C3 H3C . 0.9940 ?
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
O1 H1A O10 2_555 0.89 2.08 2.933(2) 160 yes
O1 H1B O6 2_556 0.95 1.83 2.776(2) 175 yes
O2 H2A O8 2_555 0.88 1.81 2.680(2) 171 yes
O2 H2B O10 1_555 0.83 1.89 2.712(2) 168 yes
O3 H3A O6 2_656 0.88 1.84 2.674(2) 158 yes
O3 H3B O7 2_545 0.92 1.79 2.663(2) 157 yes
O4 H4A O9 1_555 0.93 1.99 2.848(2) 153 yes
O4 H4B O9 2_666 0.93 1.81 2.727(2) 168 yes
O9 H9A O5 1_555 0.94 1.92 2.758(2) 147 yes
O9 H9B O8 1_666 0.86 1.91 2.722(2) 157 yes
O10 H10A O7 2_545 0.95 1.86 2.779(2) 164 yes
O10 H10B O3 2_655 1.03 1.88 2.853(2) 158 yes
