#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:36:42 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179756 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/52/7005236.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7005236
loop_
_publ_author_name
'Wu, Da-Yu'
'Huang, Wei'
'Hua, Wei-Jie'
'Song, You'
'Duan, Chun-Ying'
'Li, Shu-Hua'
'Meng, Qing-Jin'
_publ_section_title
;
 Metal complexes formed by metal-assisted solvolysis of
 di-pyridylketone azine: structures and magnetic properties.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1838
_journal_page_last               1845
_journal_paper_doi               10.1039/b618286k
_journal_year                    2007
_chemical_formula_sum            'C48 H48 N20 Ni4 O10'
_chemical_formula_weight         1299.90
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 90.5860(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.4319(10)
_cell_length_b                   10.9629(8)
_cell_length_c                   20.1630(14)
_cell_measurement_temperature    293(2)
_cell_volume                     2968.9(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14570
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    1.319
_exptl_absorpt_correction_T_max  0.785
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark-blue
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5205
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0537
_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)+(0.1255P)²+0.7556P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1715
_refine_ls_wR_factor_ref         0.1857
_reflns_number_gt                3903
_reflns_number_total             5205
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b618286k.txt
_cod_data_source_block           t
_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 
;
_cod_original_sg_symbol_H-M      'P2(1)/c '
_cod_database_code               7005236
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.42939(5) 0.61050(5) 0.51431(3) 0.0334(2) Uani 1 1 d . . .
Ni2 Ni 0.33195(5) 0.35686(6) 0.50522(3) 0.0359(2) Uani 1 1 d . . .
O1 O 0.4581(2) 0.4423(3) 0.55107(14) 0.0326(7) Uani 1 1 d . . .
O2 O 0.5481(3) 0.4470(4) 0.65099(17) 0.0535(10) Uani 1 1 d . . .
H2A H 0.5905 0.4595 0.6229 0.080 Uiso 1 1 calc R . .
O3 O 0.3287(2) 0.5149(3) 0.45210(15) 0.0347(7) Uani 1 1 d . . .
O4 O 0.1766(3) 0.5448(4) 0.39662(18) 0.0497(9) Uani 1 1 d . . .
N1 N 0.0780(7) 0.1684(8) 0.4999(5) 0.124(3) Uani 1 1 d U . .
N2 N 0.1593(6) 0.2090(7) 0.4749(4) 0.096(2) Uani 1 1 d U . .
N3 N 0.2337(4) 0.2455(4) 0.4536(3) 0.0549(12) Uani 1 1 d . . .
N4 N 0.5571(5) 0.8100(7) 0.6526(3) 0.096(2) Uani 1 1 d U . .
N5 N 0.5536(4) 0.7609(4) 0.6025(2) 0.0530(12) Uani 1 1 d . . .
N6 N 0.5486(3) 0.7121(4) 0.5499(2) 0.0403(10) Uani 1 1 d . . .
N7 N 0.3593(3) 0.2479(4) 0.5887(2) 0.0418(10) Uani 1 1 d . . .
N8 N 0.3592(3) 0.6169(4) 0.6067(2) 0.0381(9) Uani 1 1 d . . .
N9 N 0.3520(3) 0.7484(4) 0.4699(2) 0.0417(10) Uani 1 1 d . . .
N10 N 0.2097(3) 0.4499(4) 0.5464(2) 0.0413(10) Uani 1 1 d . . .
C1 C 0.3269(5) 0.1337(5) 0.5986(3) 0.0566(15) Uani 1 1 d . . .
H1A H 0.2853 0.0988 0.5667 0.068 Uiso 1 1 calc R . .
C2 C 0.3517(6) 0.0670(6) 0.6526(3) 0.0712(19) Uani 1 1 d . . .
H2B H 0.3268 -0.0114 0.6583 0.085 Uiso 1 1 calc R . .
C3 C 0.4148(6) 0.1179(6) 0.6989(3) 0.0683(19) Uani 1 1 d . . .
H3B H 0.4337 0.0731 0.7361 0.082 Uiso 1 1 calc R . .
C4 C 0.4501(5) 0.2339(5) 0.6908(3) 0.0567(15) Uani 1 1 d . . .
H4A H 0.4929 0.2692 0.7219 0.068 Uiso 1 1 calc R . .
C5 C 0.4193(4) 0.2976(5) 0.6341(2) 0.0394(11) Uani 1 1 d . . .
C6 C 0.4543(4) 0.4273(5) 0.6193(2) 0.0382(11) Uani 1 1 d . . .
C7 C 0.3841(4) 0.5242(5) 0.6483(2) 0.0393(12) Uani 1 1 d . . .
C8 C 0.3528(5) 0.5221(6) 0.7128(3) 0.0586(16) Uani 1 1 d . . .
H8A H 0.3706 0.4585 0.7411 0.070 Uiso 1 1 calc R . .
C9 C 0.2938(6) 0.6176(6) 0.7346(3) 0.076(2) Uani 1 1 d . . .
H9A H 0.2733 0.6194 0.7785 0.091 Uiso 1 1 calc R . .
C10 C 0.2661(6) 0.7074(6) 0.6931(3) 0.0708(19) Uani 1 1 d . . .
H10A H 0.2242 0.7695 0.7074 0.085 Uiso 1 1 calc R . .
C11 C 0.3004(4) 0.7059(5) 0.6296(3) 0.0513(14) Uani 1 1 d . . .
H11A H 0.2823 0.7690 0.6012 0.062 Uiso 1 1 calc R . .
C12 C 0.3791(5) 0.8668(5) 0.4664(3) 0.0541(14) Uani 1 1 d . . .
H12A H 0.4417 0.8892 0.4822 0.065 Uiso 1 1 calc R . .
C13 C 0.3185(5) 0.9548(6) 0.4406(3) 0.0643(17) Uani 1 1 d . . .
H13A H 0.3391 1.0357 0.4395 0.077 Uiso 1 1 calc R . .
C14 C 0.2269(6) 0.9219(6) 0.4165(3) 0.0692(19) Uani 1 1 d . . .
H14A H 0.1847 0.9806 0.3983 0.083 Uiso 1 1 calc R . .
C15 C 0.1963(5) 0.7990(6) 0.4192(3) 0.0582(16) Uani 1 1 d . . .
H15A H 0.1340 0.7748 0.4036 0.070 Uiso 1 1 calc R . .
C16 C 0.2636(4) 0.7154(5) 0.4461(3) 0.0426(12) Uani 1 1 d . . .
C17 C 0.2410(4) 0.5782(5) 0.4507(2) 0.0380(11) Uani 1 1 d . . .
C18 C 0.1778(4) 0.5473(5) 0.5123(3) 0.0428(12) Uani 1 1 d . . .
C19 C 0.0937(4) 0.6101(5) 0.5299(3) 0.0522(14) Uani 1 1 d . . .
H19A H 0.0728 0.6771 0.5051 0.063 Uiso 1 1 calc R . .
C20 C 0.0415(5) 0.5742(6) 0.5832(3) 0.0651(17) Uani 1 1 d . . .
H20A H -0.0152 0.6168 0.5957 0.078 Uiso 1 1 calc R . .
C21 C 0.0724(4) 0.4749(6) 0.6189(3) 0.0621(17) Uani 1 1 d . . .
H21A H 0.0373 0.4487 0.6558 0.074 Uiso 1 1 calc R . .
C22 C 0.1569(4) 0.4150(6) 0.5987(3) 0.0534(14) Uani 1 1 d . . .
H22A H 0.1781 0.3471 0.6226 0.064 Uiso 1 1 calc R . .
C23 C 0.2180(6) 0.5430(8) 0.3344(3) 0.085(2) Uani 1 1 d . . .
H23A H 0.1667 0.5296 0.3017 0.127 Uiso 1 1 calc R . .
H23B H 0.2662 0.4785 0.3321 0.127 Uiso 1 1 calc R . .
H23C H 0.2500 0.6197 0.3260 0.127 Uiso 1 1 calc R . .
O5 O 0.0950(11) 0.5640(14) 0.0795(7) 0.130(5) Uiso 0.50 1 d PDU . .
C24 C 0.062(2) 0.539(3) 0.1517(9) 0.167(10) Uiso 0.50 1 d PDU . .
O6 O 0.073(2) 0.225(3) 0.2621(15) 0.150(10) Uiso 0.25 1 d PDU A 1
C25 C 0.177(3) 0.205(4) 0.292(2) 0.104(11) Uiso 0.25 1 d PDU A 1
C25' C 0.214(4) 0.243(5) 0.2687(17) 0.143(15) Uiso 0.25 1 d PDU B 2
O6' O 0.163(2) 0.226(3) 0.3349(15) 0.130(9) Uiso 0.25 1 d PDU B 2
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 N9 158.77(16) . . ?
O1 Ni1 N6 102.67(14) . . ?
N9 Ni1 N6 98.18(17) . . ?
O1 Ni1 O1 80.95(13) . 3_666 ?
N9 Ni1 O1 107.23(14) . 3_666 ?
N6 Ni1 O1 78.86(14) . 3_666 ?
O1 Ni1 N8 77.94(14) . . ?
N9 Ni1 N8 97.67(16) . . ?
N6 Ni1 N8 91.58(16) . . ?
O1 Ni1 N8 154.29(15) 3_666 . ?
O1 Ni1 O3 83.33(12) . . ?
N9 Ni1 O3 77.68(15) . . ?
N6 Ni1 O3 163.61(14) . . ?
O1 Ni1 O3 87.17(12) 3_666 . ?
N8 Ni1 O3 104.65(14) . . ?
O3 Ni2 N3 103.13(17) . . ?
O3 Ni2 N7 155.58(14) . . ?
N3 Ni2 N7 100.00(18) . . ?
O3 Ni2 N6 92.31(14) . 3_666 ?
N3 Ni2 N6 90.48(18) . 3_666 ?
N7 Ni2 N6 95.24(17) . 3_666 ?
O3 Ni2 N10 77.52(14) . . ?
N3 Ni2 N10 89.34(18) . . ?
N7 Ni2 N10 95.13(17) . . ?
N6 Ni2 N10 169.50(17) 3_666 . ?
O3 Ni2 O1 82.38(12) . . ?
N3 Ni2 O1 166.87(17) . . ?
N7 Ni2 O1 76.72(14) . . ?
N6 Ni2 O1 77.29(14) 3_666 . ?
N10 Ni2 O1 103.56(14) . . ?
C6 O1 Ni1 117.5(3) . . ?
C6 O1 Ni1 128.7(3) . 3_666 ?
Ni1 O1 Ni1 99.05(13) . 3_666 ?
C6 O1 Ni2 109.9(3) . . ?
Ni1 O1 Ni2 95.36(13) . . ?
Ni1 O1 Ni2 100.39(12) 3_666 . ?
C6 O2 H2A 109.5 . . ?
C17 O3 Ni2 117.1(3) . . ?
C17 O3 Ni1 107.8(3) . . ?
Ni2 O3 Ni1 95.73(12) . . ?
C23 O4 C17 116.8(4) . . ?
N3 N2 N1 178.5(9) . . ?
N2 N3 Ni2 124.3(5) . . ?
N4 N5 N6 178.5(7) . . ?
N5 N6 Ni1 125.9(4) . . ?
N5 N6 Ni2 126.6(4) . 3_666 ?
Ni1 N6 Ni2 102.42(17) . 3_666 ?
C5 N7 C1 118.4(5) . . ?
C5 N7 Ni2 114.8(3) . . ?
C1 N7 Ni2 126.7(4) . . ?
C11 N8 C7 118.2(4) . . ?
C11 N8 Ni1 127.1(4) . . ?
C7 N8 Ni1 114.5(3) . . ?
C16 N9 C12 118.9(5) . . ?
C16 N9 Ni1 114.1(3) . . ?
C12 N9 Ni1 126.9(4) . . ?
C22 N10 C18 117.7(5) . . ?
C22 N10 Ni2 126.5(4) . . ?
C18 N10 Ni2 115.5(3) . . ?
N7 C1 C2 123.2(6) . . ?
N7 C1 H1A 118.4 . . ?
C2 C1 H1A 118.4 . . ?
C1 C2 C3 118.2(6) . . ?
C1 C2 H2B 120.9 . . ?
C3 C2 H2B 120.9 . . ?
C4 C3 C2 120.6(6) . . ?
C4 C3 H3B 119.7 . . ?
C2 C3 H3B 119.7 . . ?
C3 C4 C5 117.5(6) . . ?
C3 C4 H4A 121.2 . . ?
C5 C4 H4A 121.2 . . ?
N7 C5 C4 122.0(5) . . ?
N7 C5 C6 115.7(4) . . ?
C4 C5 C6 122.4(5) . . ?
O1 C6 O2 112.7(4) . . ?
O1 C6 C5 108.6(4) . . ?
O2 C6 C5 109.0(4) . . ?
O1 C6 C7 108.9(4) . . ?
O2 C6 C7 105.5(4) . . ?
C5 C6 C7 112.2(4) . . ?
N8 C7 C8 121.6(5) . . ?
N8 C7 C6 115.4(4) . . ?
C8 C7 C6 122.9(5) . . ?
C7 C8 C9 117.9(6) . . ?
C7 C8 H8A 121.0 . . ?
C9 C8 H8A 121.0 . . ?
C10 C9 C8 120.8(6) . . ?
C10 C9 H9A 119.6 . . ?
C8 C9 H9A 119.6 . . ?
C9 C10 C11 118.7(6) . . ?
C9 C10 H10A 120.6 . . ?
C11 C10 H10A 120.6 . . ?
N8 C11 C10 122.6(6) . . ?
N8 C11 H11A 118.7 . . ?
C10 C11 H11A 118.7 . . ?
N9 C12 C13 122.8(6) . . ?
N9 C12 H12A 118.6 . . ?
C13 C12 H12A 118.6 . . ?
C12 C13 C14 118.8(6) . . ?
C12 C13 H13A 120.6 . . ?
C14 C13 H13A 120.6 . . ?
C13 C14 C15 120.0(6) . . ?
C13 C14 H14A 120.0 . . ?
C15 C14 H14A 120.0 . . ?
C16 C15 C14 117.1(6) . . ?
C16 C15 H15A 121.4 . . ?
C14 C15 H15A 121.4 . . ?
N9 C16 C15 122.4(5) . . ?
N9 C16 C17 114.9(4) . . ?
C15 C16 C17 122.7(5) . . ?
O3 C17 O4 113.5(4) . . ?
O3 C17 C16 109.1(4) . . ?
O4 C17 C16 108.7(4) . . ?
O3 C17 C18 110.6(4) . . ?
O4 C17 C18 102.9(4) . . ?
C16 C17 C18 111.9(4) . . ?
N10 C18 C19 121.9(5) . . ?
N10 C18 C17 114.2(4) . . ?
C19 C18 C17 123.8(5) . . ?
C20 C19 C18 119.7(6) . . ?
C20 C19 H19A 120.2 . . ?
C18 C19 H19A 120.2 . . ?
C19 C20 C21 119.7(6) . . ?
C19 C20 H20A 120.2 . . ?
C21 C20 H20A 120.2 . . ?
C20 C21 C22 118.1(6) . . ?
C20 C21 H21A 121.0 . . ?
C22 C21 H21A 121.0 . . ?
N10 C22 C21 123.0(6) . . ?
N10 C22 H22A 118.5 . . ?
C21 C22 H22A 118.5 . . ?
O4 C23 H23A 109.5 . . ?
O4 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
O4 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.023(3) . ?
Ni1 N9 2.037(4) . ?
Ni1 N6 2.072(4) . ?
Ni1 O1 2.097(3) 3_666 ?
Ni1 N8 2.097(4) . ?
Ni1 O3 2.113(3) . ?
Ni2 O3 2.037(3) . ?
Ni2 N3 2.072(5) . ?
Ni2 N7 2.094(4) . ?
Ni2 N6 2.102(4) 3_666 ?
Ni2 N10 2.110(4) . ?
Ni2 O1 2.138(3) . ?
O1 C6 1.387(5) . ?
O1 Ni1 2.097(3) 3_666 ?
O2 C6 1.423(6) . ?
O2 H2A 0.8200 . ?
O3 C17 1.367(6) . ?
O4 C23 1.377(8) . ?
O4 C17 1.432(6) . ?
N1 N2 1.286(11) . ?
N2 N3 1.163(9) . ?
N4 N5 1.144(7) . ?
N5 N6 1.190(6) . ?
N6 Ni2 2.102(4) 3_666 ?
N7 C5 1.329(6) . ?
N7 C1 1.340(7) . ?
N8 C11 1.340(7) . ?
N8 C7 1.358(6) . ?
N9 C16 1.327(7) . ?
N9 C12 1.350(7) . ?
N10 C22 1.332(7) . ?
N10 C18 1.338(7) . ?
C1 C2 1.351(8) . ?
C1 H1A 0.9300 . ?
C2 C3 1.372(9) . ?
C2 H2B 0.9300 . ?
C3 C4 1.368(8) . ?
C3 H3B 0.9300 . ?
C4 C5 1.399(7) . ?
C4 H4A 0.9300 . ?
C5 C6 1.528(7) . ?
C6 C7 1.541(7) . ?
C7 C8 1.371(7) . ?
C8 C9 1.387(9) . ?
C8 H8A 0.9300 . ?
C9 C10 1.343(9) . ?
C9 H9A 0.9300 . ?
C10 C11 1.366(8) . ?
C10 H10A 0.9300 . ?
C11 H11A 0.9300 . ?
C12 C13 1.361(8) . ?
C12 H12A 0.9300 . ?
C13 C14 1.367(9) . ?
C13 H13A 0.9300 . ?
C14 C15 1.409(9) . ?
C14 H14A 0.9300 . ?
C15 C16 1.393(8) . ?
C15 H15A 0.9300 . ?
C16 C17 1.538(7) . ?
C17 C18 1.550(7) . ?
C18 C19 1.372(7) . ?
C19 C20 1.348(9) . ?
C19 H19A 0.9300 . ?
C20 C21 1.367(9) . ?
C20 H20A 0.9300 . ?
C21 C22 1.378(8) . ?
C21 H21A 0.9300 . ?
C22 H22A 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
O5 C24 1.550(10) . ?
O6 C25 1.536(10) . ?
C25' O6' 1.518(10) . ?
