#------------------------------------------------------------------------------
#$Date: 2016-02-20 17:35:30 +0100 (Sat 20 de Feb de 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/90/2219059.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_2219059
loop_
_publ_author_name
'Xuan, Zhen-Yu'
'Che, Yong'
'Huang, Yong-Chun'
_publ_section_title
catena-Poly[[bis(pyridine-κN)nickel(II)]-μ-oxalato-κ⁴O¹,O²:O^1'^,O^2'^]
_journal_coeditor_code           HY2144
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1040
_journal_paper_doi               10.1107/S1600536808021703
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ni (C2 O4) (C5 H5 N)2]'
_chemical_formula_moiety         'C12 H10 N2 Ni O4'
_chemical_formula_sum            'C12 H10 N2 Ni O4'
_chemical_formula_weight         304.93
_chemical_name_systematic
;
catena-Poly[[bis(pyridine-\kN)nickel(II)]-
μ-oxalato-κ⁴O¹,O²:O^1'^,O^2'^]
;
_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                 91.52(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.357(3)
_cell_length_b                   10.801(2)
_cell_length_c                   8.6669(17)
_cell_measurement_reflns_used    1532
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.31
_cell_volume                     1343.5(5)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'PROCESS-AUTO (Rigaku, 1998)'
_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_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6433
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.31
_exptl_absorpt_coefficient_mu    1.454
_exptl_absorpt_correction_T_max  0.7257
_exptl_absorpt_correction_T_min  0.6401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.300
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         1519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0487P)²+1.5041P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1026
_reflns_number_gt                1297
_reflns_number_total             1519
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hy2144.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               2219059
_cod_database_fobs_code          2219059
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
Ni Ni1 0.5000 0.35667(4) 0.2500 0.04167(19) Uani d S 1
O O1 0.57949(11) 0.49601(17) 0.1553(2) 0.0468(4) Uani d . 1
O O2 0.57299(12) 0.62481(16) -0.0453(2) 0.0465(4) Uani d . 1
N N1 0.59041(14) 0.2248(2) 0.1633(3) 0.0491(5) Uani d . 1
C C1 0.5679(2) 0.1569(3) 0.0391(5) 0.0726(10) Uani d . 1
H H1 0.5088 0.1664 -0.0059 0.090 Uiso calc . 1
C C2 0.6274(3) 0.0743(4) -0.0251(6) 0.0911(13) Uani d . 1
H H2 0.6085 0.0290 -0.1116 0.090 Uiso calc . 1
C C3 0.7145(3) 0.0584(3) 0.0378(5) 0.0790(11) Uani d . 1
H H3 0.7558 0.0019 -0.0040 0.090 Uiso calc . 1
C C4 0.7395(2) 0.1274(4) 0.1630(5) 0.0725(10) Uani d . 1
H H4 0.7986 0.1190 0.2083 0.090 Uiso calc . 1
C C5 0.6764(2) 0.2103(3) 0.2231(4) 0.0592(8) Uani d . 1
H H5 0.6946 0.2577 0.3083 0.090 Uiso calc . 1
C C6 0.54390(16) 0.5345(2) 0.0324(3) 0.0405(5) Uani d . 1
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 0.0290(2) 0.0460(3) 0.0499(3) 0.000 -0.00167(18) 0.000
O1 0.0341(9) 0.0554(11) 0.0503(11) -0.0087(7) -0.0082(8) 0.0032(8)
O2 0.0358(9) 0.0508(10) 0.0527(11) -0.0083(7) -0.0047(8) 0.0002(8)
N1 0.0351(11) 0.0486(12) 0.0637(15) 0.0030(9) 0.0034(10) 0.0006(10)
C1 0.0480(17) 0.074(2) 0.096(3) 0.0063(15) -0.0007(17) -0.0296(19)
C2 0.067(2) 0.089(3) 0.118(3) 0.007(2) 0.011(2) -0.043(3)
C3 0.060(2) 0.068(2) 0.110(3) 0.0157(17) 0.025(2) -0.009(2)
C4 0.0438(16) 0.086(2) 0.088(3) 0.0185(15) 0.0097(16) 0.021(2)
C5 0.0401(14) 0.070(2) 0.067(2) 0.0114(13) 0.0028(13) 0.0074(15)
C6 0.0293(11) 0.0451(13) 0.0470(14) -0.0015(10) 0.0014(10) -0.0054(11)
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
O2 Ni1 O2 6_566 5_665 168.78(10) y
O2 Ni1 O1 6_566 . 89.88(7) y
O2 Ni1 O1 5_665 . 81.96(7) y
O2 Ni1 O1 6_566 2_655 81.96(7) ?
O2 Ni1 O1 5_665 2_655 89.88(7) ?
O1 Ni1 O1 . 2_655 86.81(11) y
O2 Ni1 N1 6_566 . 94.02(8) y
O2 Ni1 N1 5_665 . 93.66(9) y
O1 Ni1 N1 . . 89.92(9) y
O1 Ni1 N1 2_655 . 174.81(8) y
O2 Ni1 N1 6_566 2_655 93.66(9) ?
O2 Ni1 N1 5_665 2_655 94.02(8) ?
O1 Ni1 N1 . 2_655 174.81(8) ?
O1 Ni1 N1 2_655 2_655 89.92(9) ?
N1 Ni1 N1 . 2_655 93.61(13) y
C6 O1 Ni1 . . 111.39(15) ?
C6 O2 Ni1 . 5_665 111.64(15) ?
C1 N1 C5 . . 116.8(3) ?
C1 N1 Ni1 . . 121.8(2) ?
C5 N1 Ni1 . . 121.3(2) ?
N1 C1 C2 . . 123.1(3) ?
N1 C1 H1 . . 118.4 ?
C2 C1 H1 . . 118.4 ?
C3 C2 C1 . . 119.9(4) ?
C3 C2 H2 . . 120.1 ?
C1 C2 H2 . . 120.1 ?
C4 C3 C2 . . 118.1(3) ?
C4 C3 H3 . . 121.0 ?
C2 C3 H3 . . 121.0 ?
C3 C4 C5 . . 119.7(3) ?
C3 C4 H4 . . 120.2 ?
C5 C4 H4 . . 120.2 ?
N1 C5 C4 . . 122.4(3) ?
N1 C5 H5 . . 118.8 ?
C4 C5 H5 . . 118.8 ?
O1 C6 O2 . . 125.6(2) ?
O1 C6 C6 . 5_665 117.5(3) ?
O2 C6 C6 . 5_665 116.9(3) ?
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 O2 6_566 2.046(2) y
Ni1 O2 5_665 2.046(2) ?
Ni1 O1 . 2.0716(18) y
Ni1 O1 2_655 2.0716(18) ?
Ni1 N1 . 2.081(2) y
Ni1 N1 2_655 2.081(2) ?
O1 C6 . 1.240(3) ?
O2 C6 . 1.263(3) ?
O2 Ni1 5_665 2.046(2) ?
N1 C1 . 1.335(4) ?
N1 C5 . 1.336(3) ?
C1 C2 . 1.364(5) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.362(6) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.357(6) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.385(5) ?
C4 H4 . 0.9300 ?
C5 H5 . 0.9300 ?
C6 C6 5_665 1.556(4) ?
