#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/99/2229910.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_2229910
loop_
_publ_author_name
'Feng, Miao'
'Tian, Hui-Juan'
'Mi, Huai-Feng'
'Hu, Tong-Liang'
_publ_section_title
;
 catena-Poly[[diaquabis(formato-κO)nickel(II)]-μ-2,4,6-tris(4-pyridyl)-1,3,5-triazine-κ²N²:N⁴]
;
_journal_coeditor_code           BQ2289
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m563
_journal_paper_doi               10.1107/S1600536811012281
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Ni (C H O2)2 (C18 H12 N6) (H2 O)2]'
_chemical_formula_moiety         'C20 H18 N6 Ni O6'
_chemical_formula_sum            'C20 H18 N6 Ni O6'
_chemical_formula_weight         497.11
_chemical_name_systematic
;
catena-Poly[[diaquabis(formato-κO)nickel(II)]-μ-
2,4,6-tris(4-pyridyl)-1,3,5-triazine-κ²N²:N⁴]
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.23(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.725(5)
_cell_length_b                   10.969(2)
_cell_length_c                   7.4196(15)
_cell_measurement_reflns_used    9569
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     2012.2(7)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku SCX-mini'
_diffrn_measurement_method       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  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10365
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.019
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.280
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2302
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0337
_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)+(0.0334P)²+2.3183P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0775
_reflns_number_gt                1937
_reflns_number_total             2302
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            bq2289.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2229910
_cod_database_fobs_code          2229910
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_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 0.2500 0.7500 1.0000 0.01798(11) Uani d S 1 . .
O O1 0.22888(6) 0.64439(12) 0.78618(18) 0.0263(3) Uani d . 1 . .
O O2 0.19168(7) 0.61015(14) 0.5190(2) 0.0337(4) Uani d . 1 . .
O O3 0.29896(6) 0.86926(12) 0.85264(19) 0.0263(3) Uani d . 1 . .
H H6 0.3027 0.9430 0.8884 0.039 Uiso d R 1 . .
H H7 0.3001 0.8711 0.7403 0.039 Uiso d R 1 . .
N N1 0.18044(6) 0.86186(14) 0.9633(2) 0.0204(4) Uani d . 1 . .
N N2 0.04510(7) 1.19452(15) 0.8071(2) 0.0251(4) Uani d . 1 . .
N N3 0.0000 1.0076(2) 0.7500 0.0245(5) Uani d S 1 . .
N N4 0.0000 1.6408(2) 0.7500 0.0428(7) Uani d S 1 . .
C C1 0.13264(8) 0.81007(18) 0.9265(3) 0.0241(4) Uani d . 1 . .
H H1 0.1299 0.7257 0.9355 0.029 Uiso calc R 1 . .
C C2 0.08733(8) 0.87491(18) 0.8760(3) 0.0248(4) Uani d . 1 . .
H H2 0.0551 0.8349 0.8495 0.030 Uiso calc R 1 . .
C C3 0.09060(8) 1.00126(18) 0.8654(3) 0.0210(4) Uani d . 1 . .
C C4 0.13930(8) 1.05662(18) 0.9086(3) 0.0239(4) Uani d . 1 . .
H H4 0.1427 1.1410 0.9053 0.029 Uiso calc R 1 . .
C C5 0.18282(8) 0.98373(18) 0.9569(3) 0.0240(4) Uani d . 1 . .
H H5 0.2154 1.0215 0.9864 0.029 Uiso calc R 1 . .
C C6 0.04255(8) 1.07256(18) 0.8045(3) 0.0208(4) Uani d . 1 . .
C C7 0.0000 1.2503(3) 0.7500 0.0229(6) Uani d S 1 . .
C C8 0.0000 1.3860(3) 0.7500 0.0252(6) Uani d S 1 . .
C C9 -0.04675(9) 1.4505(2) 0.7877(3) 0.0327(5) Uani d . 1 . .
H H9 -0.0791 1.4101 0.8097 0.039 Uiso calc R 1 . .
C C10 -0.04418(10) 1.5768(2) 0.7918(4) 0.0400(6) Uani d . 1 . .
H H10 -0.0750 1.6194 0.8257 0.048 Uiso calc R 1 . .
C C11 0.20837(8) 0.67816(19) 0.6412(3) 0.0246(4) Uani d . 1 . .
H H11 0.2052 0.7617 0.6226 0.029 Uiso calc R 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'
Ni Ni 0.3393 1.1124 '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'
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
O1 Ni1 O1 7_567 . 180.0 ?
O1 Ni1 O3 7_567 7_567 95.50(6) ?
O1 Ni1 O3 . 7_567 84.50(6) ?
O1 Ni1 O3 7_567 . 84.50(6) ?
O1 Ni1 O3 . . 95.50(6) ?
O3 Ni1 O3 7_567 . 180.0 ?
O1 Ni1 N1 7_567 . 88.64(6) ?
O1 Ni1 N1 . . 91.36(6) ?
O3 Ni1 N1 7_567 . 87.62(6) ?
O3 Ni1 N1 . . 92.38(6) ?
O1 Ni1 N1 7_567 7_567 91.36(6) ?
O1 Ni1 N1 . 7_567 88.64(6) ?
O3 Ni1 N1 7_567 7_567 92.39(6) ?
O3 Ni1 N1 . 7_567 87.61(6) ?
N1 Ni1 N1 . 7_567 180.0 ?
C11 O1 Ni1 . . 127.47(13) ?
Ni1 O3 H6 . . 119.3 ?
Ni1 O3 H7 . . 124.0 ?
H6 O3 H7 . . 106.4 ?
C1 N1 C5 . . 117.10(16) ?
C1 N1 Ni1 . . 119.57(13) ?
C5 N1 Ni1 . . 122.98(13) ?
C7 N2 C6 . . 114.35(18) ?
C6 N3 C6 2_556 . 115.4(2) ?
C10 N4 C10 . 2_556 116.6(3) ?
N1 C1 C2 . . 123.56(18) ?
N1 C1 H1 . . 118.2 ?
C2 C1 H1 . . 118.2 ?
C1 C2 C3 . . 118.84(18) ?
C1 C2 H2 . . 120.6 ?
C3 C2 H2 . . 120.6 ?
C4 C3 C2 . . 118.34(18) ?
C4 C3 C6 . . 122.08(18) ?
C2 C3 C6 . . 119.57(18) ?
C3 C4 C5 . . 118.69(18) ?
C3 C4 H4 . . 120.7 ?
C5 C4 H4 . . 120.7 ?
N1 C5 C4 . . 123.41(18) ?
N1 C5 H5 . . 118.3 ?
C4 C5 H5 . . 118.3 ?
N3 C6 N2 . . 125.14(19) ?
N3 C6 C3 . . 116.04(18) ?
N2 C6 C3 . . 118.82(17) ?
N2 C7 N2 2_556 . 125.7(3) ?
N2 C7 C8 2_556 . 117.17(13) ?
N2 C7 C8 . . 117.17(13) ?
C9 C8 C9 2_556 . 118.5(3) ?
C9 C8 C7 2_556 . 120.74(14) ?
C9 C8 C7 . . 120.74(14) ?
C8 C9 C10 . . 118.5(2) ?
C8 C9 H9 . . 120.8 ?
C10 C9 H9 . . 120.8 ?
N4 C10 C9 . . 123.8(2) ?
N4 C10 H10 . . 118.1 ?
C9 C10 H10 . . 118.1 ?
O2 C11 O1 . . 125.8(2) ?
O2 C11 H11 . . 117.1 ?
O1 C11 H11 . . 117.1 ?
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 7_567 2.0309(14) ?
Ni1 O1 . 2.0309(14) ?
Ni1 O3 7_567 2.0934(14) ?
Ni1 O3 . 2.0935(14) ?
Ni1 N1 . 2.1293(16) ?
Ni1 N1 7_567 2.1294(16) ?
O1 C11 . 1.244(2) ?
O2 C11 . 1.244(2) ?
O3 H6 . 0.8557 ?
O3 H7 . 0.8343 ?
N1 C1 . 1.338(3) ?
N1 C5 . 1.339(3) ?
N2 C7 . 1.339(2) ?
N2 C6 . 1.339(3) ?
N3 C6 2_556 1.332(2) ?
N3 C6 . 1.332(2) ?
N4 C10 . 1.336(3) ?
N4 C10 2_556 1.336(3) ?
C1 C2 . 1.378(3) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.391(3) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.385(3) ?
C3 C6 . 1.491(3) ?
C4 C5 . 1.387(3) ?
C4 H4 . 0.9300 ?
C5 H5 . 0.9300 ?
C7 N2 2_556 1.339(2) ?
C7 C8 . 1.489(4) ?
C8 C9 2_556 1.385(3) ?
C8 C9 . 1.385(3) ?
C9 C10 . 1.387(3) ?
C9 H9 . 0.9300 ?
C10 H10 . 0.9300 ?
C11 H11 . 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
_geom_hbond_publ_flag
O3 H6 O2 4_556 0.86 1.96 2.818(2) 177 yes
O3 H7 O2 7_566 0.83 1.95 2.777(2) 174 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O3 Ni1 O1 C11 7_567 . . . 125.73(18) ?
O3 Ni1 O1 C11 . . . . -54.27(18) ?
N1 Ni1 O1 C11 . . . . 38.26(18) ?
N1 Ni1 O1 C11 7_567 . . . -141.74(18) ?
O1 Ni1 N1 C1 7_567 . . . -137.13(16) ?
O1 Ni1 N1 C1 . . . . 42.87(16) ?
O3 Ni1 N1 C1 7_567 . . . -41.57(15) ?
O3 Ni1 N1 C1 . . . . 138.43(15) ?
O1 Ni1 N1 C5 7_567 . . . 49.91(16) ?
O1 Ni1 N1 C5 . . . . -130.09(16) ?
O3 Ni1 N1 C5 7_567 . . . 145.47(16) ?
O3 Ni1 N1 C5 . . . . -34.53(16) ?
C5 N1 C1 C2 . . . . 2.8(3) ?
Ni1 N1 C1 C2 . . . . -170.57(17) ?
N1 C1 C2 C3 . . . . -1.2(3) ?
C1 C2 C3 C4 . . . . -0.9(3) ?
C1 C2 C3 C6 . . . . 177.77(19) ?
C2 C3 C4 C5 . . . . 1.3(3) ?
C6 C3 C4 C5 . . . . -177.31(19) ?
C1 N1 C5 C4 . . . . -2.3(3) ?
Ni1 N1 C5 C4 . . . . 170.79(16) ?
C3 C4 C5 N1 . . . . 0.3(3) ?
C6 N3 C6 N2 2_556 . . . -0.22(15) ?
C6 N3 C6 C3 2_556 . . . -179.8(2) ?
C7 N2 C6 N3 . . . . 0.4(3) ?
C7 N2 C6 C3 . . . . 180.00(15) ?
C4 C3 C6 N3 . . . . 173.55(17) ?
C2 C3 C6 N3 . . . . -5.0(3) ?
C4 C3 C6 N2 . . . . -6.1(3) ?
C2 C3 C6 N2 . . . . 175.33(19) ?
C6 N2 C7 N2 . . . 2_556 -0.19(13) ?
C6 N2 C7 C8 . . . . 179.82(13) ?
N2 C7 C8 C9 2_556 . . 2_556 -145.57(15) ?
N2 C7 C8 C9 . . . 2_556 34.43(15) ?
N2 C7 C8 C9 2_556 . . . 34.43(15) ?
N2 C7 C8 C9 . . . . -145.57(15) ?
C9 C8 C9 C10 2_556 . . . -2.10(17) ?
C7 C8 C9 C10 . . . . 177.90(17) ?
C10 N4 C10 C9 2_556 . . . -2.33(18) ?
C8 C9 C10 N4 . . . . 4.5(4) ?
Ni1 O1 C11 O2 . . . . -173.47(16) ?
