#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/18/2221811.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_2221811
loop_
_publ_author_name
'Yu, Jian'
_publ_section_title
;catena-Poly[[[di-μ₂-hydroxido-bis[(di-2-pyridylamine)nickel(II)]]-μ-fumarato]
 dihydrate]
;
_journal_coeditor_code           SJ2613
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m535
_journal_page_last               m536
_journal_paper_doi               10.1107/S1600536809013580
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Ni2 (C4 H2 O4) (O H)2 (C10 H9 N3)2], 2H2 O'
_chemical_formula_moiety         'C24 H22 N6 Ni2 O6, 2(H2 O)'
_chemical_formula_sum            'C24 H26 N6 Ni2 O8'
_chemical_formula_weight         643.92
_chemical_name_systematic
;catena-Poly[[[di-μ₂hydroxido-bis[(di-2-pyridylamine)nickel(II)]]-μ-
fumarato]
 dihydrate]
;
_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                70.545(4)
_cell_angle_beta                 71.103(4)
_cell_angle_gamma                75.785(4)
_cell_formula_units_Z            1
_cell_length_a                   8.135(2)
_cell_length_b                   8.834(3)
_cell_length_c                   10.015(3)
_cell_measurement_reflns_used    2216
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      2.24
_cell_volume                     634.4(3)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia,
1997)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEXII 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  0.0143
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3238
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         2.24
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.547
_exptl_absorpt_correction_T_max  0.8362
_exptl_absorpt_correction_T_min  0.7272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.346
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2216
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0231
_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)+(0.0374P)²+0.2972P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0630
_reflns_number_gt                1984
_reflns_number_total             2216
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sj2613.cif
_cod_data_source_block           I
_cod_original_cell_volume        634.3(3)
_cod_database_code               2221811
_cod_database_fobs_code          2221811
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 0.04021(3) 0.15037(3) 0.87985(3) 0.02129(10) Uani d . 1 . .
N N1 -0.0829(2) 0.3069(2) 0.73316(19) 0.0298(4) Uani d . 1 . .
N N2 -0.0529(2) 0.5376(2) 0.7868(2) 0.0345(4) Uani d . 1 . .
H H2B -0.1179 0.6218 0.8116 0.041 Uiso calc R 1 . .
N N3 0.1739(2) 0.3286(2) 0.85495(19) 0.0287(4) Uani d . 1 . .
O O1 0.2311(2) 0.0443(2) 0.70594(17) 0.0452(4) Uani d . 1 . .
C C12 0.5204(3) -0.0107(3) 0.5612(2) 0.0325(5) Uani d . 1 . .
H H12 0.6387 -0.0250 0.5576 0.039 Uiso calc R 1 . .
O O1W 0.1972(2) 0.1399(2) 0.22330(18) 0.0381(4) Uani d D 1 . .
O O4 0.13677(18) -0.00305(18) 1.03993(15) 0.0272(3) Uani d D 1 . .
C C1 -0.1404(3) 0.2457(3) 0.6520(2) 0.0369(5) Uani d . 1 . .
H H1 -0.1120 0.1347 0.6615 0.044 Uiso calc R 1 . .
C C2 -0.2378(3) 0.3391(3) 0.5568(3) 0.0423(6) Uani d . 1 . .
H H2 -0.2765 0.2925 0.5039 0.051 Uiso calc R 1 . .
C C3 -0.2782(3) 0.5056(3) 0.5407(3) 0.0440(6) Uani d . 1 . .
H H3 -0.3457 0.5719 0.4776 0.053 Uiso calc R 1 . .
C C4 -0.2178(3) 0.5707(3) 0.6181(3) 0.0396(6) Uani d . 1 . .
H H4 -0.2429 0.6819 0.6076 0.048 Uiso calc R 1 . .
C C5 -0.1178(3) 0.4688(3) 0.7134(2) 0.0304(5) Uani d . 1 . .
C C6 0.1043(3) 0.4872(3) 0.8252(2) 0.0301(5) Uani d . 1 . .
C C7 0.1878(3) 0.6062(3) 0.8296(3) 0.0376(5) Uani d . 1 . .
H H7 0.1352 0.7144 0.8122 0.045 Uiso calc R 1 . .
C C8 0.3477(3) 0.5600(3) 0.8600(3) 0.0420(6) Uani d . 1 . .
H H8 0.4049 0.6367 0.8643 0.050 Uiso calc R 1 . .
C C9 0.4246(3) 0.3974(3) 0.8844(3) 0.0393(6) Uani d . 1 . .
H H9 0.5349 0.3642 0.9026 0.047 Uiso calc R 1 . .
C C10 0.3345(3) 0.2878(3) 0.8812(2) 0.0336(5) Uani d . 1 . .
H H10 0.3861 0.1792 0.8978 0.040 Uiso calc R 1 . .
C C11 0.3878(3) -0.0135(3) 0.7062(2) 0.0324(5) Uani d . 1 . .
O O2 0.4437(2) -0.0761(2) 0.81955(17) 0.0375(4) Uani d . 1 . .
H H1WB 0.168(4) 0.101(4) 0.169(3) 0.080 Uiso d D 1 . .
H H1WA 0.3066(15) 0.122(4) 0.212(4) 0.080 Uiso d D 1 . .
H H4A 0.231(3) -0.046(4) 0.995(3) 0.080 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
O4 Ni1 O4 . 2_557 81.87(6) ?
O4 Ni1 N1 . . 173.85(7) ?
O4 Ni1 N1 2_557 . 94.01(7) ?
O4 Ni1 N3 . . 94.06(7) ?
O4 Ni1 N3 2_557 . 161.16(7) ?
N1 Ni1 N3 . . 88.38(7) ?
O4 Ni1 O1 . . 94.61(6) ?
O4 Ni1 O1 2_557 . 101.31(7) ?
N1 Ni1 O1 . . 90.68(7) ?
N3 Ni1 O1 . . 97.33(7) ?
O4 Ni1 Ni1 . 2_557 40.99(4) ?
O4 Ni1 Ni1 2_557 2_557 40.88(4) ?
N1 Ni1 Ni1 . 2_557 134.72(5) ?
N3 Ni1 Ni1 . 2_557 132.37(5) ?
O1 Ni1 Ni1 . 2_557 100.55(5) ?
C5 N1 C1 . . 117.87(19) ?
C5 N1 Ni1 . . 124.23(15) ?
C1 N1 Ni1 . . 117.85(15) ?
C5 N2 C6 . . 127.58(19) ?
C5 N2 H2B . . 116.2 ?
C6 N2 H2B . . 116.2 ?
C6 N3 C10 . . 117.40(19) ?
C6 N3 Ni1 . . 122.94(15) ?
C10 N3 Ni1 . . 119.42(15) ?
C11 O1 Ni1 . . 123.67(14) ?
C12 C12 C11 2_656 . 124.0(3) ?
C12 C12 H12 2_656 . 118.0 ?
C11 C12 H12 . . 118.0 ?
H1WB O1W H1WA . . 112(2) ?
Ni1 O4 Ni1 . 2_557 98.13(6) ?
Ni1 O4 H4A . . 103(2) ?
Ni1 O4 H4A 2_557 . 111(3) ?
N1 C1 C2 . . 123.1(2) ?
N1 C1 H1 . . 118.4 ?
C2 C1 H1 . . 118.4 ?
C1 C2 C3 . . 118.5(2) ?
C1 C2 H2 . . 120.8 ?
C3 C2 H2 . . 120.8 ?
C4 C3 C2 . . 119.5(2) ?
C4 C3 H3 . . 120.3 ?
C2 C3 H3 . . 120.3 ?
C3 C4 C5 . . 119.4(2) ?
C3 C4 H4 . . 120.3 ?
C5 C4 H4 . . 120.3 ?
N1 C5 N2 . . 119.92(19) ?
N1 C5 C4 . . 121.6(2) ?
N2 C5 C4 . . 118.5(2) ?
N3 C6 N2 . . 120.05(19) ?
N3 C6 C7 . . 122.1(2) ?
N2 C6 C7 . . 117.8(2) ?
C8 C7 C6 . . 118.8(2) ?
C8 C7 H7 . . 120.6 ?
C6 C7 H7 . . 120.6 ?
C7 C8 C9 . . 119.6(2) ?
C7 C8 H8 . . 120.2 ?
C9 C8 H8 . . 120.2 ?
C10 C9 C8 . . 118.5(2) ?
C10 C9 H9 . . 120.8 ?
C8 C9 H9 . . 120.8 ?
N3 C10 C9 . . 123.5(2) ?
N3 C10 H10 . . 118.2 ?
C9 C10 H10 . . 118.2 ?
O1 C11 O2 . . 125.1(2) ?
O1 C11 C12 . . 118.0(2) ?
O2 C11 C12 . . 116.88(19) ?
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 O4 . 1.9671(15) y
Ni1 O4 2_557 1.9713(15) y
Ni1 N1 . 1.9984(18) y
Ni1 N3 . 2.0314(18) y
Ni1 O1 . 2.2232(16) y
Ni1 Ni1 2_557 2.9753(8) y
N1 C5 . 1.347(3) ?
N1 C1 . 1.355(3) ?
N2 C5 . 1.377(3) ?
N2 C6 . 1.381(3) ?
N2 H2B . 0.8600 ?
N3 C6 . 1.347(3) ?
N3 C10 . 1.354(3) ?
O1 C11 . 1.252(3) ?
C12 C12 2_656 1.313(4) ?
C12 C11 . 1.499(3) ?
C12 H12 . 0.9300 ?
O1W H1WB . 0.85(3) ?
O1W H1WA . 0.840(10) ?
O4 Ni1 2_557 1.9713(15) ?
O4 H4A . 0.83(3) ?
C1 C2 . 1.364(3) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.392(4) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.362(4) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.397(3) ?
C4 H4 . 0.9300 ?
C6 C7 . 1.404(3) ?
C7 C8 . 1.365(3) ?
C7 H7 . 0.9300 ?
C8 C9 . 1.392(4) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.364(3) ?
C9 H9 . 0.9300 ?
C10 H10 . 0.9300 ?
C11 O2 . 1.263(3) ?
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
O4 H4A O2 . 0.83(3) 2.068(16) 2.848(2) 158(3)
O1W H1WA O2 2_656 0.840(10) 1.912(10) 2.752(2) 178(3)
O1W H1WB O4 1_554 0.85(3) 1.92(3) 2.765(2) 172(3)
N2 H2B O1W 2_566 0.86 1.99 2.784(3) 153.0
