#------------------------------------------------------------------------------
#$Date: 2016-02-20 04:06:23 +0100 (Sat 20 de Feb de 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/30/2203060.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_2203060
loop_
_publ_author_name
'Shiu, Kom-Bei'
'Yen, Chia-Hung'
'Liao, Fen-Ling'
'Wang, Sue-Lein'
_publ_section_title
;
 cis-Diaquabis(ethylenediamine)nickel(II)
 benzene-1,4-dicarboxylate monohydrate
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m121
_journal_page_last               m122
_journal_paper_doi               10.1107/S1600536803028988
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Ni (C2 H8 N2)2 (H2 O)2] (C8 H4 O4), H2 O'
_chemical_formula_moiety         'C4 H20 N4 Ni O4 2+, C8 H4 O4 2-, H2 O'
_chemical_formula_sum            'C12 H26 N4 Ni O7'
_chemical_formula_weight         397.08
_chemical_name_systematic        ?
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 122.1910(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4890(10)
_cell_length_b                   20.4936(16)
_cell_length_c                   8.4365(6)
_cell_measurement_reflns_used    3931
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.5
_cell_volume                     1827.3(2)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0466
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6464
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    1.101
_exptl_absorpt_correction_T_max  0.71786
_exptl_absorpt_correction_T_min  0.61976
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1995)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       Columnar
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.317
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         2269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0330
_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)+(0.0632P)²+0.0602P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.0973
_reflns_number_gt                2024
_reflns_number_total             2269
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cv6254.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2203060
_cod_database_fobs_code          2203060
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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 0.5000 0.595504(11) 0.7500 0.03685(11) Uani d S 1 Ni
O1 0.36711(10) 0.52091(5) 0.59740(14) 0.0492(3) Uani d . 1 O
H1A 0.3335 0.5094 0.6539 0.059 Uiso calc R 1 H
H1B 0.3156 0.5306 0.4860 0.059 Uiso d R 1 H
O2 0.18596(18) 0.35714(9) 0.7373(2) 0.0980(6) Uani d . 1 O
O3 0.24480(12) 0.45756(7) 0.72807(17) 0.0648(4) Uani d . 1 O
O4 0.5000 0.79167(10) 0.7500 0.0987(9) Uani d S 1 O
H4A 0.5524 0.8164 0.7391 0.118 Uiso d . 1 H
N1 0.47423(9) 0.59892(4) 0.97726(14) 0.0507(3) Uani d . 1 N
H1C 0.4338 0.5628 0.9788 0.061 Uiso calc R 1 H
H1D 0.5497 0.6011 1.0860 0.061 Uiso calc R 1 H
N2 0.64459(9) 0.66553(4) 0.86145(14) 0.0465(3) Uani d R 1 N
H2A 0.6125 0.7054 0.8562 0.056 Uiso calc R 1 H
H2B 0.7026 0.6562 0.9820 0.056 Uiso calc R 1 H
C1 0.3986(2) 0.65715(9) 0.9542(3) 0.0630(5) Uani d . 1 C
H1E 0.4523 0.6955 0.9965 0.076 Uiso calc R 1 H
H1F 0.3610 0.6529 1.0289 0.076 Uiso calc R 1 H
C2 0.70362(18) 0.66435(11) 0.7493(3) 0.0645(5) Uani d . 1 C
H2C 0.7624 0.6281 0.7883 0.077 Uiso calc R 1 H
H2D 0.7502 0.7045 0.7682 0.077 Uiso calc R 1 H
C3 0.04189(16) 0.35018(9) 0.3456(2) 0.0547(4) Uani d . 1 C
H3A 0.0691 0.3108 0.4100 0.066 Uiso calc R 1 H
C4 0.08581(15) 0.40847(8) 0.4425(2) 0.0457(4) Uani d . 1 C
C5 0.04392(15) 0.46678(9) 0.3461(2) 0.0480(4) Uani d . 1 C
H5A 0.0745 0.5061 0.4097 0.058 Uiso calc R 1 H
C6 0.17865(18) 0.40756(9) 0.6520(2) 0.0540(4) Uani d . 1 C
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 0.03501(16) 0.04103(17) 0.02896(16) 0.000 0.01331(12) 0.000
O1 0.0459(6) 0.0557(6) 0.0323(5) -0.0087(5) 0.0116(5) 0.0008(5)
O2 0.0963(11) 0.1083(12) 0.0415(8) -0.0294(10) 0.0045(7) 0.0250(8)
O3 0.0595(7) 0.0904(9) 0.0287(6) -0.0192(7) 0.0130(5) 0.0005(6)
O4 0.1116(19) 0.0499(11) 0.160(3) 0.000 0.090(2) 0.000
N1 0.0556(9) 0.0558(8) 0.0412(8) 0.0000(6) 0.0261(7) 0.0014(5)
N2 0.0409(6) 0.0491(7) 0.0396(7) -0.0034(5) 0.0148(6) 0.0005(5)
C1 0.0743(12) 0.0696(11) 0.0567(11) 0.0094(9) 0.0427(10) -0.0021(9)
C2 0.0548(10) 0.0789(12) 0.0639(12) -0.0160(9) 0.0343(9) -0.0044(10)
C3 0.0493(9) 0.0586(10) 0.0436(9) 0.0000(8) 0.0163(8) 0.0058(7)
C4 0.0351(7) 0.0660(10) 0.0297(8) -0.0024(6) 0.0130(6) 0.0042(6)
C5 0.0438(8) 0.0606(9) 0.0305(8) -0.0043(7) 0.0138(7) -0.0041(6)
C6 0.0409(8) 0.0804(13) 0.0303(8) -0.0054(7) 0.0120(7) 0.0077(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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 Ni1 N2 . 2_656 93.60(5) ?
N2 Ni1 N1 . . 94.69(4) yes
N2 Ni1 N1 2_656 . 82.69(4) ?
N2 Ni1 N1 . 2_656 82.69(4) ?
N2 Ni1 N1 2_656 2_656 94.69(4) ?
N1 Ni1 N1 . 2_656 176.19(5) ?
N2 Ni1 O1 . . 167.68(4) yes
N2 Ni1 O1 2_656 . 90.73(4) ?
N1 Ni1 O1 . . 97.31(4) yes
N1 Ni1 O1 2_656 . 85.46(4) ?
N2 Ni1 O1 . 2_656 90.73(4) ?
N2 Ni1 O1 2_656 2_656 167.68(4) ?
N1 Ni1 O1 . 2_656 85.46(4) ?
N1 Ni1 O1 2_656 2_656 97.31(4) ?
O1 Ni1 O1 . 2_656 87.42(6) ?
Ni1 O1 H1A . . 109.5 ?
Ni1 O1 H1B . . 113.5 ?
H1A O1 H1B . . 113.5 ?
C1 N1 Ni1 . . 107.79(9) ?
C1 N1 H1C . . 110.1 ?
Ni1 N1 H1C . . 110.1 ?
C1 N1 H1D . . 110.1 ?
Ni1 N1 H1D . . 110.1 ?
H1C N1 H1D . . 108.5 ?
C2 N2 Ni1 . . 107.82(9) ?
C2 N2 H2A . . 110.1 ?
Ni1 N2 H2A . . 110.1 ?
C2 N2 H2B . . 110.1 ?
Ni1 N2 H2B . . 110.1 ?
H2A N2 H2B . . 108.5 ?
N1 C1 C2 . 2_656 108.99(14) ?
N1 C1 H1E . . 109.9 ?
C2 C1 H1E 2_656 . 109.9 ?
N1 C1 H1F . . 109.9 ?
C2 C1 H1F 2_656 . 109.9 ?
H1E C1 H1F . . 108.3 ?
N2 C2 C1 . 2_656 108.84(14) ?
N2 C2 H2C . . 109.9 ?
C1 C2 H2C 2_656 . 109.9 ?
N2 C2 H2D . . 109.9 ?
C1 C2 H2D 2_656 . 109.9 ?
H2C C2 H2D . . 108.3 ?
C3 C3 C4 2 . 120.40(9) ?
C3 C3 H3A 2 . 119.8 ?
C4 C3 H3A . . 119.8 ?
C5 C4 C3 . . 119.44(15) ?
C5 C4 C6 . . 120.87(15) ?
C3 C4 C6 . . 119.70(15) ?
C4 C5 C5 . 2 120.14(9) ?
C4 C5 H5A . . 119.9 ?
C5 C5 H5A 2 . 119.9 ?
O2 C6 O3 . . 124.08(17) ?
O2 C6 C4 . . 117.67(16) ?
O3 C6 C4 . . 118.24(15) ?
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 N2 . 2.0965(11) yes
Ni1 N2 2_656 2.0965(11) ?
Ni1 N1 . 2.1076(10) yes
Ni1 N1 2_656 2.1076(10) ?
Ni1 O1 . 2.1148(10) yes
Ni1 O1 2_656 2.1148(10) ?
O1 H1A . 0.8200 ?
O1 H1B . 0.8323 ?
O2 C6 . 1.235(2) ?
O3 C6 . 1.257(2) ?
O4 H4A . 0.8705 ?
N1 C1 . 1.469(2) ?
N1 H1C . 0.9000 ?
N1 H1D . 0.9000 ?
N2 C2 . 1.477(2) ?
N2 H2A . 0.9000 ?
N2 H2B . 0.9000 ?
C1 C2 2_656 1.505(3) ?
C1 H1E . 0.9700 ?
C1 H1F . 0.9700 ?
C2 C1 2_656 1.505(3) ?
C2 H2C . 0.9700 ?
C2 H2D . 0.9700 ?
C3 C3 2 1.378(3) ?
C3 C4 . 1.385(2) ?
C3 H3A . 0.9300 ?
C4 C5 . 1.382(2) ?
C4 C6 . 1.511(2) ?
C5 C5 2 1.392(3) ?
C5 H5A . 0.9300 ?
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
O1 H1A O3 . 0.82 1.87 2.651(2) 160
O1 H1B O3 6_565 0.83 1.88 2.677(2) 161
N2 H2A O4 . 0.90 2.14 3.003(2) 161
N2 H2B O2 5_667 0.90 2.03 2.919(3) 171
O4 H4A O2 3 0.87 1.87 2.733(3) 170
