#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/48/2224802.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_2224802
loop_
_publ_author_name
'Fan, Zhen-Zhong'
'Wang, Guo-Ping'
'Li, Yu-Sheng'
_publ_section_title
Poly[aqua[μ₂-cis-1,2-bis(4-pyridyl)ethylene-κ²N:N'](μ₂-5-nitroisophthalato-κ³O:O',O'')nickel(II)]
_journal_coeditor_code           WM2289
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m80
_journal_page_last               m81
_journal_paper_doi               10.1107/S1600536809053872
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Ni (C8 H3 N O6) (C12 H10 N2) (H2 O)]'
_chemical_formula_moiety         'C20 H15 N3 Ni O7'
_chemical_formula_sum            'C20 H15 N3 Ni O7'
_chemical_formula_weight         468.06
_chemical_name_systematic
;
Poly[aqua[μ₂-cis-1,2-bis(4-pyridyl)ethylene-
κ²N:N'](μ₂-5-nitroisophthalato-
κ³O:O',O'')nickel(II)]
;
_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           SHELXL-97
_cell_angle_alpha                109.9700(10)
_cell_angle_beta                 90.1900(10)
_cell_angle_gamma                110.7270(10)
_cell_formula_units_Z            2
_cell_length_a                   9.3723(6)
_cell_length_b                   10.9947(7)
_cell_length_c                   11.1704(8)
_cell_measurement_reflns_used    563
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.23
_cell_measurement_theta_min      2.30
_cell_volume                     1001.68(12)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω 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  0.0114
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5380
_diffrn_reflns_theta_full        25.30
_diffrn_reflns_theta_max         25.30
_diffrn_reflns_theta_min         1.96
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.017
_exptl_absorpt_correction_T_max  0.8624
_exptl_absorpt_correction_T_min  0.6688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.046
_refine_diff_density_min         -0.287
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         3580
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0313
_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)+(0.0584P)²+0.2791P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0887
_reflns_number_gt                3332
_reflns_number_total             3580
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wm2289.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 
;
_cod_database_code               2224802
_cod_database_fobs_code          2224802
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
Ni Ni1 -0.10441(3) 0.65566(2) 0.40788(2) 0.02504(11) Uani d . 1 . .
O O1 0.08218(16) 0.83742(14) 0.52003(14) 0.0310(3) Uani d . 1 . .
O O2 0.12955(16) 0.65335(15) 0.40496(14) 0.0317(3) Uani d . 1 . .
O O3 0.72083(17) 0.72162(16) 0.46313(14) 0.0335(3) Uani d . 1 . .
O O4 0.7598(2) 0.76834(19) 0.67483(15) 0.0452(4) Uani d . 1 . .
O O5 0.7148(2) 1.2514(2) 0.8534(2) 0.0669(6) Uani d . 1 . .
O O6 0.4914(3) 1.2513(2) 0.8145(3) 0.0922(9) Uani d . 1 . .
O O7 -0.10853(19) 0.59321(17) 0.56426(15) 0.0368(4) Uani d D 1 . .
H H7C -0.1478 0.6361 0.6203 0.055 Uiso calc R 1 . .
N N1 -0.2423(2) 0.45995(18) 0.28631(17) 0.0310(4) Uani d . 1 . .
N N2 -0.0886(2) 0.73429(18) 0.26156(16) 0.0295(4) Uani d . 1 . .
N N3 0.5841(2) 1.1956(2) 0.79624(19) 0.0459(5) Uani d . 1 . .
C C1 0.1744(2) 0.7762(2) 0.48722(19) 0.0267(4) Uani d . 1 . .
C C2 0.3389(2) 0.8505(2) 0.55081(19) 0.0274(4) Uani d . 1 . .
C C3 0.4422(2) 0.7831(2) 0.52789(19) 0.0288(4) Uani d . 1 . .
H H3 0.4126 0.6938 0.4655 0.035 Uiso calc R 1 . .
C C4 0.5902(2) 0.8484(2) 0.59767(18) 0.0291(4) Uani d . 1 . .
C C5 0.6353(2) 0.9824(2) 0.6881(2) 0.0328(5) Uani d . 1 . .
H H5 0.7322 1.0259 0.7372 0.039 Uiso calc R 1 . .
C C6 0.5339(2) 1.0506(2) 0.70426(19) 0.0314(4) Uani d . 1 . .
C C7 0.3861(2) 0.9872(2) 0.63851(19) 0.0307(4) Uani d . 1 . .
H H7A 0.3195 1.0348 0.6525 0.037 Uiso calc R 1 . .
C C8 0.6993(2) 0.7724(2) 0.57767(19) 0.0296(4) Uani d . 1 . .
C C9 -0.1887(3) 0.3572(2) 0.2488(2) 0.0427(6) Uani d . 1 . .
H H9 -0.0886 0.3762 0.2815 0.051 Uiso calc R 1 . .
C C10 -0.2739(3) 0.2259(2) 0.1648(2) 0.0444(6) Uani d . 1 . .
H H10 -0.2310 0.1581 0.1412 0.053 Uiso calc R 1 . .
C C11 -0.4237(3) 0.1925(2) 0.1143(2) 0.0363(5) Uani d . 1 . .
C C12 -0.4787(3) 0.2997(3) 0.1542(2) 0.0475(6) Uani d . 1 . .
H H12 -0.5788 0.2831 0.1235 0.057 Uiso calc R 1 . .
C C13 -0.3868(3) 0.4297(2) 0.2382(2) 0.0436(6) Uani d . 1 . .
H H13 -0.4263 0.4998 0.2628 0.052 Uiso calc R 1 . .
C C14 -0.5208(3) 0.0535(3) 0.0252(2) 0.0428(5) Uani d . 1 . .
C C15 -0.0938(3) 0.6642(2) 0.1362(2) 0.0435(6) Uani d . 1 . .
H H15 -0.1075 0.5704 0.1097 0.052 Uiso calc R 1 . .
C C16 -0.0798(3) 0.7238(3) 0.0449(2) 0.0478(6) Uani d . 1 . .
H H16 -0.0861 0.6701 -0.0412 0.057 Uiso calc R 1 . .
C C17 -0.0564(3) 0.8640(2) 0.0810(2) 0.0354(5) Uani d . 1 . .
C C18 -0.0545(2) 0.9364(2) 0.2110(2) 0.0322(5) Uani d . 1 . .
H H18 -0.0422 1.0300 0.2400 0.039 Uiso calc R 1 . .
C C19 -0.0710(2) 0.8682(2) 0.2961(2) 0.0309(4) Uani d . 1 . .
H H19 -0.0697 0.9182 0.3824 0.037 Uiso calc R 1 . .
C C20 -0.0330(3) 0.9319(2) -0.0139(2) 0.0388(5) Uani d . 1 . .
H H20 -0.0673 0.8748 -0.1000 0.047 Uiso calc R 1 . .
H H14 -0.618(3) 0.041(3) 0.004(3) 0.047 Uiso d . 1 . .
H H7B -0.133(3) 0.5144(15) 0.564(3) 0.058 Uiso d 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'
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
O3 Ni1 N1 1_455 . 95.70(7) ?
O3 Ni1 N2 1_455 . 89.29(6) ?
N1 Ni1 N2 . . 91.76(7) ?
O3 Ni1 O7 1_455 . 90.31(6) ?
N1 Ni1 O7 . . 92.91(7) ?
N2 Ni1 O7 . . 175.33(6) ?
O3 Ni1 O1 1_455 . 98.89(6) ?
N1 Ni1 O1 . . 165.38(6) ?
N2 Ni1 O1 . . 89.30(6) ?
O7 Ni1 O1 . . 86.16(6) ?
O3 Ni1 O2 1_455 . 159.73(6) ?
N1 Ni1 O2 . . 104.19(6) ?
N2 Ni1 O2 . . 93.84(6) ?
O7 Ni1 O2 . . 84.95(6) ?
O1 Ni1 O2 . . 61.19(5) ?
O3 Ni1 C1 1_455 . 129.22(6) ?
N1 Ni1 C1 . . 134.81(7) ?
N2 Ni1 C1 . . 93.28(7) ?
O7 Ni1 C1 . . 83.37(6) ?
O1 Ni1 C1 . . 30.59(6) ?
O2 Ni1 C1 . . 30.66(6) ?
C1 O1 Ni1 . . 91.05(12) ?
C1 O2 Ni1 . . 86.48(11) ?
C8 O3 Ni1 . 1_655 125.17(13) ?
Ni1 O7 H7C . . 109.5 ?
Ni1 O7 H7B . . 128(2) ?
H7C O7 H7B . . 108.7 ?
C9 N1 C13 . . 117.23(19) ?
C9 N1 Ni1 . . 120.54(15) ?
C13 N1 Ni1 . . 122.20(15) ?
C19 N2 C15 . . 116.78(18) ?
C19 N2 Ni1 . . 116.73(14) ?
C15 N2 Ni1 . . 126.49(15) ?
O6 N3 O5 . . 123.4(2) ?
O6 N3 C6 . . 118.2(2) ?
O5 N3 C6 . . 118.3(2) ?
O1 C1 O2 . . 121.02(18) ?
O1 C1 C2 . . 118.64(18) ?
O2 C1 C2 . . 120.31(17) ?
O1 C1 Ni1 . . 58.36(10) ?
O2 C1 Ni1 . . 62.86(10) ?
C2 C1 Ni1 . . 173.30(14) ?
C3 C2 C7 . . 119.69(19) ?
C3 C2 C1 . . 121.18(18) ?
C7 C2 C1 . . 119.07(18) ?
C2 C3 C4 . . 120.61(19) ?
C2 C3 H3 . . 119.7 ?
C4 C3 H3 . . 119.7 ?
C5 C4 C3 . . 119.60(18) ?
C5 C4 C8 . . 119.83(18) ?
C3 C4 C8 . . 120.55(18) ?
C4 C5 C6 . . 118.92(19) ?
C4 C5 H5 . . 120.5 ?
C6 C5 H5 . . 120.5 ?
C7 C6 C5 . . 122.42(19) ?
C7 C6 N3 . . 118.54(19) ?
C5 C6 N3 . . 119.04(19) ?
C6 C7 C2 . . 118.61(19) ?
C6 C7 H7A . . 120.7 ?
C2 C7 H7A . . 120.7 ?
O4 C8 O3 . . 127.14(19) ?
O4 C8 C4 . . 117.32(18) ?
O3 C8 C4 . . 115.52(17) ?
N1 C9 C10 . . 123.1(2) ?
N1 C9 H9 . . 118.5 ?
C10 C9 H9 . . 118.5 ?
C9 C10 C11 . . 120.5(2) ?
C9 C10 H10 . . 119.7 ?
C11 C10 H10 . . 119.7 ?
C10 C11 C12 . . 116.1(2) ?
C10 C11 C14 . . 123.0(2) ?
C12 C11 C14 . . 121.0(2) ?
C13 C12 C11 . . 120.5(2) ?
C13 C12 H12 . . 119.7 ?
C11 C12 H12 . . 119.7 ?
N1 C13 C12 . . 122.6(2) ?
N1 C13 H13 . . 118.7 ?
C12 C13 H13 . . 118.7 ?
C14 C14 C11 2_455 . 126.5(3) ?
C14 C14 H14 2_455 . 117.9(18) ?
C11 C14 H14 . . 115.6(18) ?
N2 C15 C16 . . 123.3(2) ?
N2 C15 H15 . . 118.3 ?
C16 C15 H15 . . 118.3 ?
C15 C16 C17 . . 120.0(2) ?
C15 C16 H16 . . 120.0 ?
C17 C16 H16 . . 120.0 ?
C16 C17 C18 . . 116.7(2) ?
C16 C17 C20 . . 121.1(2) ?
C18 C17 C20 . . 122.2(2) ?
C19 C18 C17 . . 119.4(2) ?
C19 C18 H18 . . 120.3 ?
C17 C18 H18 . . 120.3 ?
N2 C19 C18 . . 123.63(19) ?
N2 C19 H19 . . 118.2 ?
C18 C19 H19 . . 118.2 ?
C20 C20 C17 2_575 . 124.9(3) ?
C20 C20 H20 2_575 . 117.6 ?
C17 C20 H20 . . 117.6 ?
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 O3 1_455 2.0326(14) y
Ni1 N1 . 2.0417(17) y
Ni1 N2 . 2.0777(17) y
Ni1 O7 . 2.0797(15) y
Ni1 O1 . 2.1031(14) y
Ni1 O2 . 2.2021(14) y
Ni1 C1 . 2.470(2) ?
O1 C1 . 1.257(2) ?
O2 C1 . 1.262(2) ?
O3 C8 . 1.258(2) ?
O3 Ni1 1_655 2.0326(14) ?
O4 C8 . 1.244(3) ?
O5 N3 . 1.217(3) ?
O6 N3 . 1.210(3) ?
O7 H7C . 0.8200 ?
O7 H7B . 0.814(10) ?
N1 C9 . 1.335(3) ?
N1 C13 . 1.337(3) ?
N2 C19 . 1.336(3) ?
N2 C15 . 1.339(3) ?
N3 C6 . 1.471(3) ?
C1 C2 . 1.501(3) ?
C2 C3 . 1.390(3) ?
C2 C7 . 1.391(3) ?
C3 C4 . 1.397(3) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.382(3) ?
C4 C8 . 1.507(3) ?
C5 C6 . 1.383(3) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.380(3) ?
C7 H7A . 0.9300 ?
C9 C10 . 1.363(3) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.383(3) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.388(3) ?
C11 C14 . 1.458(3) ?
C12 C13 . 1.368(3) ?
C12 H12 . 0.9300 ?
C13 H13 . 0.9300 ?
C14 C14 2_455 1.314(5) ?
C14 H14 . 0.89(3) ?
C15 C16 . 1.372(3) ?
C15 H15 . 0.9300 ?
C16 C17 . 1.387(3) ?
C16 H16 . 0.9300 ?
C17 C18 . 1.394(3) ?
C17 C20 . 1.468(3) ?
C18 C19 . 1.377(3) ?
C18 H18 . 0.9300 ?
C19 H19 . 0.9300 ?
C20 C20 2_575 1.322(5) ?
C20 H20 . 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
O7 H7C O4 1_455 0.82 1.88 2.612(2) 148.5
O7 H7B O2 2_566 0.814(10) 1.999(13) 2.786(2) 163(3)
