#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:25:48 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179969 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/63/7026359.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_7026359
loop_
_publ_author_name
'Gole, Bappaditya'
'Chakrabarty, Rajesh'
'Mukherjee, Sandip'
'Song, You'
'Mukherjee, Partha Sarathi'
_publ_section_title
;
 Use of 2-pyrimidineamidoxime to generate polynuclear homo-/heterometallic
 assemblies: synthesis, crystal structures and magnetic study with
 theoretical investigations on the exchange mechanism.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9766
_journal_page_last               9778
_journal_paper_doi               10.1039/c0dt00353k
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C20 H18 Cl2 Cu2 N16 Ni2 O4, 2(O)'
_chemical_formula_sum            'C20 H18 Cl2 Cu2 N16 Ni2 O5'
_chemical_formula_weight         893.85
_chemical_name_systematic
;
?
;
_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                66.030(2)
_cell_angle_beta                 83.795(2)
_cell_angle_gamma                65.826(2)
_cell_formula_units_Z            1
_cell_length_a                   8.6134(11)
_cell_length_b                   9.7382(12)
_cell_length_c                   10.3083(13)
_cell_measurement_temperature    293(2)
_cell_volume                     719.03(16)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    'ORTEP-3 for Windows(Farrugia, 1997)'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scan'
_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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7421
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    3.005
_exptl_absorpt_correction_T_max  0.5448
_exptl_absorpt_correction_T_min  0.4975
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS: Blessing, R. (1995), Acta Cryst., A51, 33'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    2.074
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             450
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         2921
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0376P)²+0.9348P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0817
_reflns_number_gt                2527
_reflns_number_total             2921
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c0dt00353k.txt
_cod_data_source_block           complex3
_cod_database_code               7026359
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Cl1 Cl 1.16341(10) -0.28291(10) 0.34233(9) 0.0311(2) Uani 1 1 d
Cu1 Cu 1.21676(5) -0.19123(4) 0.51808(4) 0.02468(13) Uani 1 1 d
Ni1 Ni 0.99514(5) 0.38129(4) 0.24691(4) 0.02128(12) Uani 1 1 d
N1 N 0.9703(4) 0.5993(3) 0.1156(3) 0.0276(6) Uani 1 1 d
N2 N 0.7542(4) 0.8693(3) 0.0063(3) 0.0324(7) Uani 1 1 d
N3 N 0.7566(3) 0.4885(3) 0.2522(3) 0.0250(6) Uani 1 1 d
N4 N 0.5169(4) 0.7390(4) 0.1561(4) 0.0344(7) Uani 1 1 d
H4A H 0.457(6) 0.691(6) 0.200(5) 0.059(15) Uiso 1 1 d
H4B H 0.491(5) 0.830(6) 0.100(4) 0.039(12) Uiso 1 1 d
N5 N 1.4453(3) -0.1837(3) 0.4543(3) 0.0235(6) Uani 1 1 d
N6 N 1.5678(3) 0.0036(3) 0.3125(3) 0.0296(6) Uani 1 1 d
N7 N 1.1451(3) 0.0491(3) 0.4061(3) 0.0244(6) Uani 1 1 d
N8 N 1.2267(4) 0.2551(3) 0.2532(3) 0.0261(6) Uani 1 1 d
H8A H 1.316(5) 0.273(4) 0.212(4) 0.029(10) Uiso 1 1 d
C1 C 0.8066(4) 0.7112(4) 0.0909(3) 0.0246(7) Uani 1 1 d
C2 C 0.8760(6) 0.9179(5) -0.0611(4) 0.0386(9) Uani 1 1 d
H2 H 0.845(6) 1.016(6) -0.125(5) 0.058(14) Uiso 1 1 d
C3 C 1.0451(6) 0.8126(5) -0.0453(4) 0.0420(9) Uani 1 1 d
H3 H 1.132(6) 0.846(6) -0.097(5) 0.054(13) Uiso 1 1 d
C4 C 1.0900(5) 0.6519(5) 0.0475(4) 0.0365(8) Uani 1 1 d
H4 H 1.200(5) 0.577(5) 0.068(4) 0.031(10) Uiso 1 1 d
C5 C 0.6833(4) 0.6437(4) 0.1696(3) 0.0247(7) Uani 1 1 d
C6 C 1.4367(4) -0.0331(4) 0.3687(3) 0.0216(6) Uani 1 1 d
C7 C 1.6001(4) -0.3090(4) 0.4868(4) 0.0291(7) Uani 1 1 d
H7 H 1.598(5) -0.413(5) 0.546(4) 0.038(11) Uiso 1 1 d
C8 C 1.7442(4) -0.2809(4) 0.4345(4) 0.0317(8) Uani 1 1 d
H8 H 1.865(6) -0.368(5) 0.458(5) 0.054(13) Uiso 1 1 d
C9 C 1.7227(4) -0.1232(4) 0.3477(4) 0.0327(8) Uani 1 1 d
H9 H 1.829(5) -0.099(4) 0.316(4) 0.030(10) Uiso 1 1 d
C10 C 1.2636(4) 0.0989(4) 0.3385(3) 0.0224(6) Uani 1 1 d
O1 O 0.6565(3) 0.4129(3) 0.3321(2) 0.0293(5) Uani 1 1 d
O2 O 0.9847(3) 0.1816(3) 0.3706(2) 0.0273(5) Uani 1 1 d
O1W O 0.4789(5) 0.6358(6) 0.8721(4) 0.0847(13) Uani 1 1 d
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
O2 Cu1 O1 87.79(9) 2_756 2_756
O2 Cu1 N7 97.85(9) 2_756 .
O1 Cu1 N7 157.98(11) 2_756 .
O2 Cu1 N5 160.84(11) 2_756 .
O1 Cu1 N5 88.01(10) 2_756 .
N7 Cu1 N5 79.69(10) . .
O2 Cu1 Cl1 101.28(8) 2_756 .
O1 Cu1 Cl1 97.32(8) 2_756 .
N7 Cu1 Cl1 102.37(9) . .
N5 Cu1 Cl1 97.80(8) . .
N8 Ni1 O2 84.45(10) . .
N8 Ni1 N3 173.84(11) . .
O2 Ni1 N3 89.42(10) . .
N8 Ni1 N1 103.59(12) . .
O2 Ni1 N1 171.68(11) . .
N3 Ni1 N1 82.52(11) . .
C4 N1 C1 117.4(3) . .
C4 N1 Ni1 129.4(3) . .
C1 N1 Ni1 113.2(2) . .
C1 N2 C2 115.6(3) . .
C5 N3 O1 118.0(3) . .
C5 N3 Ni1 117.6(2) . .
O1 N3 Ni1 124.27(19) . .
C5 N4 H4A 115(4) . .
C5 N4 H4B 115(3) . .
H4A N4 H4B 130(5) . .
C6 N5 C7 117.6(3) . .
C6 N5 Cu1 114.3(2) . .
C7 N5 Cu1 128.1(2) . .
C6 N6 C9 115.9(3) . .
C10 N7 O2 110.2(2) . .
C10 N7 Cu1 117.0(2) . .
O2 N7 Cu1 132.47(19) . .
C10 N8 Ni1 110.7(2) . .
C10 N8 H8A 114(2) . .
Ni1 N8 H8A 136(2) . .
N2 C1 N1 125.6(3) . .
N2 C1 C5 120.3(3) . .
N1 C1 C5 114.0(3) . .
N2 C2 C3 123.0(3) . .
N2 C2 H2 118(3) . .
C3 C2 H2 119(3) . .
C4 C3 C2 117.9(4) . .
C4 C3 H3 119(3) . .
C2 C3 H3 123(3) . .
N1 C4 C3 120.4(4) . .
N1 C4 H4 117(2) . .
C3 C4 H4 123(2) . .
N3 C5 N4 126.4(3) . .
N3 C5 C1 112.5(3) . .
N4 C5 C1 121.1(3) . .
N6 C6 N5 125.7(3) . .
N6 C6 C10 119.4(3) . .
N5 C6 C10 114.9(3) . .
N5 C7 C8 120.3(3) . .
N5 C7 H7 114(2) . .
C8 C7 H7 126(2) . .
C9 C8 C7 117.8(3) . .
C9 C8 H8 117(3) . .
C7 C8 H8 125(3) . .
N6 C9 C8 122.6(3) . .
N6 C9 H9 119(2) . .
C8 C9 H9 118(2) . .
N7 C10 N8 121.7(3) . .
N7 C10 C6 113.9(3) . .
N8 C10 C6 124.4(3) . .
N3 O1 Cu1 114.58(17) . 2_756
N7 O2 Ni1 112.98(17) . .
N7 O2 Cu1 125.75(18) . 2_756
Ni1 O2 Cu1 117.59(10) . 2_756
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cl1 Cu1 2.4740(10) .
Cu1 O2 1.965(2) 2_756
Cu1 O1 1.990(2) 2_756
Cu1 N7 1.992(3) .
Cu1 N5 2.028(3) .
Ni1 N8 1.857(3) .
Ni1 O2 1.875(2) .
Ni1 N3 1.892(3) .
Ni1 N1 1.934(3) .
N1 C4 1.343(5) .
N1 C1 1.354(4) .
N2 C1 1.327(4) .
N2 C2 1.337(5) .
N3 C5 1.303(4) .
N3 O1 1.355(3) .
N4 C5 1.336(4) .
N4 H4A 0.82(5) .
N4 H4B 0.79(4) .
N5 C6 1.345(4) .
N5 C7 1.346(4) .
N6 C6 1.327(4) .
N6 C9 1.352(4) .
N7 C10 1.319(4) .
N7 O2 1.404(3) .
N8 C10 1.329(4) .
N8 H8A 0.89(4) .
C1 C5 1.473(5) .
C2 C3 1.375(6) .
C2 H2 0.86(5) .
C3 C4 1.372(5) .
C3 H3 0.96(5) .
C4 H4 0.91(4) .
C6 C10 1.475(4) .
C7 C8 1.385(5) .
C7 H7 0.96(4) .
C8 C9 1.371(5) .
C8 H8 1.01(5) .
C9 H9 1.02(4) .
O1 Cu1 1.990(2) 2_756
O2 Cu1 1.965(2) 2_756
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N4 H4A Cl1 0.82(5) 2.75(5) 3.455(4) 145(4) 1_465
N4 H4B N2 0.79(4) 2.65(4) 3.341(4) 146(4) 2_675
N8 H8A O1W 0.89(4) 2.23(4) 3.100(4) 166(3) 2_766
