#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/72/4317283.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_4317283
loop_
_publ_author_name
'Jiong-Peng Zhao'
'Bo-Wen Hu'
'Xiao-Feng Zhang'
'Qian Yang'
'M. S. El Fallah'
'J. Ribas'
'Xian-He Bu'
_publ_section_title
;
 One Pot Synthesis of Heterometallic 3d-3d Azide Coordination
 Architectures: Effect of the Single-Ion Anisotropy
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11325
_journal_page_last               11332
_journal_paper_doi               10.1021/ic101089n
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C12 H8 Co0.5 Cu N8 Ni0.5 O4'
_chemical_formula_weight         450.62
_chemical_name_systematic
; 
 ? 
;
_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                 104.45(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.848(3)
_cell_length_b                   13.275(3)
_cell_length_c                   10.443(2)
_cell_measurement_reflns_used    7163
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.7
_cell_measurement_theta_min      3.1
_cell_volume                     1724.8(7)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω 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  0.1013
_diffrn_reflns_av_sigmaI/netI    0.0735
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7177
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    2.296
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             898
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0922
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0422P)²+0.7877P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1133
_reflns_number_gt                1155
_reflns_number_total             1511
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101089n_si_002_3.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1724.7(6)
_cod_original_formula_sum        'C12 H8 Co0.50 Cu N8 Ni0.50 O4'
_cod_database_code               4317283
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_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 0.5000 0.35253(7) 0.2500 0.0207(3) Uani 0.50 2 d SP . .
Co1 Co 0.5000 0.35253(7) 0.2500 0.0207(3) Uani 0.50 2 d SP . .
O2 O 0.3950(3) 0.5618(3) 0.0827(4) 0.0362(11) Uani 1 1 d . . .
N1 N 0.4565(4) 0.3641(3) 0.0453(5) 0.0269(11) Uani 1 1 d . . .
C1 C 0.3630(4) 0.5402(4) 0.1828(6) 0.0269(14) Uani 1 1 d . . .
Cu1 Cu 0.5000 0.5000 0.0000 0.0260(3) Uani 1 2 d S . .
O1 O 0.3912(3) 0.4690(3) 0.2609(4) 0.0272(10) Uani 1 1 d . . .
N2 N 0.4631(4) 0.2915(4) -0.0231(5) 0.0375(13) Uani 1 1 d . . .
C2 C 0.2803(4) 0.6128(4) 0.2120(5) 0.0268(14) Uani 1 1 d . . .
N3 N 0.4689(6) 0.2218(4) -0.0842(6) 0.070(2) Uani 1 1 d . . .
C3 C 0.2706(5) 0.7082(4) 0.1575(6) 0.0320(15) Uani 1 1 d . . .
H3A H 0.3171 0.7294 0.1076 0.038 Uiso 1 1 calc R . .
N4 N 0.1226(4) 0.7457(3) 0.2456(4) 0.0281(12) Uani 1 1 d . . .
C4 C 0.1929(5) 0.7707(4) 0.1773(6) 0.0309(14) Uani 1 1 d . . .
H4A H 0.1886 0.8349 0.1409 0.037 Uiso 1 1 calc R . .
C5 C 0.1353(5) 0.6554(4) 0.3031(6) 0.0395(17) Uani 1 1 d . . .
H5A H 0.0898 0.6374 0.3560 0.047 Uiso 1 1 calc R . .
C6 C 0.2118(5) 0.5877(4) 0.2884(6) 0.0388(17) Uani 1 1 d . . .
H6A H 0.2172 0.5252 0.3299 0.047 Uiso 1 1 calc R . .
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'
Co Co 0.3494 0.9721 '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'
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
N1 Ni1 N1 171.5(3) 2_655 . ?
N1 Ni1 O1 89.40(16) 2_655 2_655 ?
N1 Ni1 O1 84.37(16) . 2_655 ?
N1 Ni1 O1 84.37(16) 2_655 . ?
N1 Ni1 O1 89.40(16) . . ?
O1 Ni1 O1 85.6(2) 2_655 . ?
N1 Ni1 N4 92.15(17) 2_655 4_545 ?
N1 Ni1 N4 93.50(18) . 4_545 ?
O1 Ni1 N4 174.20(17) 2_655 4_545 ?
O1 Ni1 N4 89.04(16) . 4_545 ?
N1 Ni1 N4 93.50(18) 2_655 3_545 ?
N1 Ni1 N4 92.15(17) . 3_545 ?
O1 Ni1 N4 89.04(16) 2_655 3_545 ?
O1 Ni1 N4 174.20(17) . 3_545 ?
N4 Ni1 N4 96.4(3) 4_545 3_545 ?
C1 O2 Cu1 133.0(4) . . ?
N2 N1 Cu1 121.1(4) . . ?
N2 N1 Ni1 120.4(4) . . ?
Cu1 N1 Ni1 107.1(2) . . ?
O1 C1 O2 128.4(5) . . ?
O1 C1 C2 117.0(5) . . ?
O2 C1 C2 114.6(5) . . ?
O2 Cu1 O2 180.0 . 5_665 ?
O2 Cu1 N1 89.45(16) . 5_665 ?
O2 Cu1 N1 90.55(16) 5_665 5_665 ?
O2 Cu1 N1 90.55(16) . . ?
O2 Cu1 N1 89.45(16) 5_665 . ?
N1 Cu1 N1 180.0 5_665 . ?
O2 Cu1 O1 95.39(14) . 6_565 ?
O2 Cu1 O1 84.61(14) 5_665 6_565 ?
N1 Cu1 O1 74.93(16) 5_665 6_565 ?
N1 Cu1 O1 105.07(16) . 6_565 ?
O2 Cu1 O1 84.61(14) . 2_655 ?
O2 Cu1 O1 95.39(14) 5_665 2_655 ?
N1 Cu1 O1 105.07(16) 5_665 2_655 ?
N1 Cu1 O1 74.93(16) . 2_655 ?
O1 Cu1 O1 180.00(15) 6_565 2_655 ?
C1 O1 Ni1 127.7(4) . . ?
C1 O1 Cu1 120.9(4) . 2_655 ?
Ni1 O1 Cu1 87.83(13) . 2_655 ?
N3 N2 N1 178.0(6) . . ?
C6 C2 C3 117.3(5) . . ?
C6 C2 C1 123.1(5) . . ?
C3 C2 C1 119.6(5) . . ?
C4 C3 C2 119.6(5) . . ?
C4 C3 H3A 120.2 . . ?
C2 C3 H3A 120.2 . . ?
C4 N4 C5 116.3(5) . . ?
C4 N4 Co1 116.9(4) . 3_455 ?
C5 N4 Co1 126.7(4) . 3_455 ?
C4 N4 Ni1 116.9(4) . 3_455 ?
C5 N4 Ni1 126.7(4) . 3_455 ?
Co1 N4 Ni1 0.0 3_455 3_455 ?
N4 C4 C3 123.9(5) . . ?
N4 C4 H4A 118.1 . . ?
C3 C4 H4A 118.1 . . ?
N4 C5 C6 123.5(5) . . ?
N4 C5 H5A 118.3 . . ?
C6 C5 H5A 118.3 . . ?
C2 C6 C5 119.3(5) . . ?
C2 C6 H6A 120.3 . . ?
C5 C6 H6A 120.3 . . ?
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 N1 2.076(5) 2_655 ?
Ni1 N1 2.076(5) . ?
Ni1 O1 2.107(3) 2_655 ?
Ni1 O1 2.107(3) . ?
Ni1 N4 2.128(4) 4_545 ?
Ni1 N4 2.128(4) 3_545 ?
O2 C1 1.248(6) . ?
O2 Cu1 1.954(4) . ?
N1 N2 1.216(6) . ?
N1 Cu1 1.981(4) . ?
C1 O1 1.241(6) . ?
C1 C2 1.521(7) . ?
Cu1 O2 1.954(4) 5_665 ?
Cu1 N1 1.981(4) 5_665 ?
Cu1 O1 2.572(4) 6_565 ?
Cu1 O1 2.572(4) 2_655 ?
O1 Cu1 2.572(4) 2_655 ?
N2 N3 1.137(7) . ?
C2 C6 1.367(7) . ?
C2 C3 1.382(7) . ?
C3 C4 1.352(7) . ?
C3 H3A 0.9300 . ?
N4 C4 1.325(6) . ?
N4 C5 1.333(7) . ?
N4 Co1 2.128(4) 3_455 ?
N4 Ni1 2.128(4) 3_455 ?
C4 H4A 0.9300 . ?
C5 C6 1.368(7) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Ni1 N1 N2 165.0(4) 2_655 . . . ?
O1 Ni1 N1 N2 122.1(4) 2_655 . . . ?
O1 Ni1 N1 N2 -152.3(4) . . . . ?
N4 Ni1 N1 N2 -63.3(4) 4_545 . . . ?
N4 Ni1 N1 N2 33.2(5) 3_545 . . . ?
N1 Ni1 N1 Cu1 21.12(16) 2_655 . . . ?
O1 Ni1 N1 Cu1 -21.80(19) 2_655 . . . ?
O1 Ni1 N1 Cu1 63.8(2) . . . . ?
N4 Ni1 N1 Cu1 152.8(2) 4_545 . . . ?
N4 Ni1 N1 Cu1 -110.6(2) 3_545 . . . ?
Cu1 O2 C1 O1 -0.3(10) . . . . ?
Cu1 O2 C1 C2 178.6(4) . . . . ?
C1 O2 Cu1 O2 39(100) . . . 5_665 ?
C1 O2 Cu1 N1 -143.3(6) . . . 5_665 ?
C1 O2 Cu1 N1 36.7(6) . . . . ?
C1 O2 Cu1 O1 141.9(5) . . . 6_565 ?
C1 O2 Cu1 O1 -38.1(5) . . . 2_655 ?
N2 N1 Cu1 O2 150.4(5) . . . . ?
Ni1 N1 Cu1 O2 -66.0(2) . . . . ?
N2 N1 Cu1 O2 -29.6(5) . . . 5_665 ?
Ni1 N1 Cu1 O2 114.0(2) . . . 5_665 ?
N2 N1 Cu1 N1 -24(100) . . . 5_665 ?
Ni1 N1 Cu1 N1 119(100) . . . 5_665 ?
N2 N1 Cu1 O1 54.7(5) . . . 6_565 ?
Ni1 N1 Cu1 O1 -161.73(16) . . . 6_565 ?
N2 N1 Cu1 O1 -125.3(5) . . . 2_655 ?
Ni1 N1 Cu1 O1 18.27(16) . . . 2_655 ?
O2 C1 O1 Ni1 -2.8(9) . . . . ?
C2 C1 O1 Ni1 178.3(3) . . . . ?
O2 C1 O1 Cu1 111.3(6) . . . 2_655 ?
C2 C1 O1 Cu1 -67.6(6) . . . 2_655 ?
N1 Ni1 O1 C1 144.3(5) 2_655 . . . ?
N1 Ni1 O1 C1 -29.9(5) . . . . ?
O1 Ni1 O1 C1 54.5(4) 2_655 . . . ?
N4 Ni1 O1 C1 -123.5(5) 4_545 . . . ?
N4 Ni1 O1 C1 75.6(17) 3_545 . . . ?
N1 Ni1 O1 Cu1 15.87(14) 2_655 . . 2_655 ?
N1 Ni1 O1 Cu1 -158.36(15) . . . 2_655 ?
O1 Ni1 O1 Cu1 -73.96(12) 2_655 . . 2_655 ?
N4 Ni1 O1 Cu1 108.12(14) 4_545 . . 2_655 ?
N4 Ni1 O1 Cu1 -52.9(16) 3_545 . . 2_655 ?
Cu1 N1 N2 N3 167(20) . . . . ?
Ni1 N1 N2 N3 28(21) . . . . ?
O1 C1 C2 C6 -22.0(9) . . . . ?
O2 C1 C2 C6 159.0(6) . . . . ?
O1 C1 C2 C3 159.5(5) . . . . ?
O2 C1 C2 C3 -19.5(8) . . . . ?
C6 C2 C3 C4 -2.3(9) . . . . ?
C1 C2 C3 C4 176.2(5) . . . . ?
C5 N4 C4 C3 4.0(9) . . . . ?
Co1 N4 C4 C3 -175.2(5) 3_455 . . . ?
Ni1 N4 C4 C3 -175.2(5) 3_455 . . . ?
C2 C3 C4 N4 -1.0(9) . . . . ?
C4 N4 C5 C6 -3.8(9) . . . . ?
Co1 N4 C5 C6 175.3(5) 3_455 . . . ?
Ni1 N4 C5 C6 175.3(5) 3_455 . . . ?
C3 C2 C6 C5 2.5(9) . . . . ?
C1 C2 C6 C5 -176.0(6) . . . . ?
N4 C5 C6 C2 0.6(10) . . . . ?
