#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/72/4317282.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_4317282
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 Co0.3 Cu N8 Ni0.7 O4'
_chemical_formula_weight         450.58
_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                 104.39(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.868(3)
_cell_length_b                   13.351(3)
_cell_length_c                   10.526(2)
_cell_measurement_reflns_used    7121
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      3.0
_cell_volume                     1751.6(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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1114
_diffrn_reflns_av_sigmaI/netI    0.0815
_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            7235
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    2.286
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             899
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.989
_refine_diff_density_min         -1.134
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1524
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0644
_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)+(0.0722P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1520
_reflns_number_gt                1187
_reflns_number_total             1524
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101089n_si_002_2.cif
_cod_data_source_block           2
_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        1751.5(6)
_cod_original_formula_sum        'C12 H8 Co0.30 Cu N8 Ni0.70 O4'
_cod_database_code               4317282
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
Cu1 Cu 0.5000 0.5000 0.0000 0.0294(4) Uani 1 2 d S . .
Co1 Co 0.0000 0.85321(7) 0.2500 0.0245(4) Uani 0.30 2 d SP . .
Ni1 Ni 0.0000 0.85321(7) 0.2500 0.0245(4) Uani 0.70 2 d SP . .
O1 O 0.3906(3) 0.4691(3) 0.2606(4) 0.0339(11) Uani 1 1 d . . .
O2 O 0.3957(3) 0.5623(3) 0.0835(4) 0.0389(11) Uani 1 1 d . . .
N4 N 0.1223(4) 0.7462(4) 0.2458(5) 0.0322(12) Uani 1 1 d . . .
N1 N 0.5437(4) 0.6356(3) -0.0439(5) 0.0290(12) Uani 1 1 d . . .
N2 N 0.5372(4) 0.7080(4) 0.0221(5) 0.0401(13) Uani 1 1 d . . .
N3 N 0.5312(6) 0.7763(5) 0.0844(7) 0.075(2) Uani 1 1 d . . .
C2 C 0.2808(5) 0.6138(4) 0.2125(6) 0.0301(14) Uani 1 1 d . . .
C6 C 0.2119(5) 0.5888(5) 0.2876(7) 0.0457(19) Uani 1 1 d . . .
H6A H 0.2163 0.5263 0.3278 0.055 Uiso 1 1 calc R . .
C5 C 0.1354(5) 0.6577(5) 0.3030(7) 0.0419(18) Uani 1 1 d . . .
H5A H 0.0908 0.6404 0.3568 0.050 Uiso 1 1 calc R . .
C1 C 0.3626(5) 0.5419(4) 0.1837(6) 0.0308(15) Uani 1 1 d . . .
C4 C 0.1926(5) 0.7724(4) 0.1766(6) 0.0348(15) Uani 1 1 d . . .
H4A H 0.1877 0.8361 0.1397 0.042 Uiso 1 1 calc R . .
C3 C 0.2715(5) 0.7089(4) 0.1584(6) 0.0351(15) Uani 1 1 d . . .
H3A H 0.3187 0.7297 0.1096 0.042 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'
Ni Ni 0.3393 1.1124 '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'
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
O2 Cu1 O2 180.0 . 5_665 ?
O2 Cu1 N1 91.01(18) . 5_665 ?
O2 Cu1 N1 88.99(18) 5_665 5_665 ?
O2 Cu1 N1 88.99(18) . . ?
O2 Cu1 N1 91.01(18) 5_665 . ?
N1 Cu1 N1 180.0 5_665 . ?
O2 Cu1 O1 84.19(15) . 2_655 ?
O2 Cu1 O1 95.81(15) 5_665 2_655 ?
N1 Cu1 O1 75.25(17) 5_665 2_655 ?
N1 Cu1 O1 104.75(17) . 2_655 ?
O2 Cu1 O1 95.81(15) . 6_565 ?
O2 Cu1 O1 84.19(15) 5_665 6_565 ?
N1 Cu1 O1 104.75(17) 5_665 6_565 ?
N1 Cu1 O1 75.25(17) . 6_565 ?
O1 Cu1 O1 180.0 2_655 6_565 ?
N1 Co1 N1 171.9(3) 8_466 7_565 ?
N1 Co1 O1 89.52(17) 8_466 4 ?
N1 Co1 O1 84.53(17) 7_565 4 ?
N1 Co1 O1 84.53(17) 8_466 3_455 ?
N1 Co1 O1 89.52(17) 7_565 3_455 ?
O1 Co1 O1 85.9(2) 4 3_455 ?
N1 Co1 N4 92.04(18) 8_466 2 ?
N1 Co1 N4 93.40(19) 7_565 2 ?
O1 Co1 N4 174.60(18) 4 2 ?
O1 Co1 N4 89.15(18) 3_455 2 ?
N1 Co1 N4 93.40(19) 8_466 . ?
N1 Co1 N4 92.04(18) 7_565 . ?
O1 Co1 N4 89.15(18) 4 . ?
O1 Co1 N4 174.60(18) 3_455 . ?
N4 Co1 N4 95.9(3) 2 . ?
C1 O1 Ni1 128.3(4) . 3_545 ?
C1 O1 Co1 128.3(4) . 3_545 ?
Ni1 O1 Co1 0.00(4) 3_545 3_545 ?
C1 O1 Cu1 120.0(4) . 2_655 ?
Ni1 O1 Cu1 87.71(14) 3_545 2_655 ?
Co1 O1 Cu1 87.71(14) 3_545 2_655 ?
C1 O2 Cu1 133.9(4) . . ?
C5 N4 C4 117.1(5) . . ?
C5 N4 Co1 127.1(4) . . ?
C4 N4 Co1 115.9(4) . . ?
N2 N1 Cu1 122.2(4) . . ?
N2 N1 Ni1 119.9(4) . 7_565 ?
Cu1 N1 Ni1 106.6(2) . 7_565 ?
N2 N1 Co1 119.9(4) . 7_565 ?
Cu1 N1 Co1 106.6(2) . 7_565 ?
Ni1 N1 Co1 0.00(5) 7_565 7_565 ?
N3 N2 N1 179.9(8) . . ?
C6 C2 C3 117.3(5) . . ?
C6 C2 C1 123.0(6) . . ?
C3 C2 C1 119.6(5) . . ?
C2 C6 C5 119.2(6) . . ?
N4 C5 C6 123.8(6) . . ?
O1 C1 O2 126.9(5) . . ?
O1 C1 C2 117.7(5) . . ?
O2 C1 C2 115.3(5) . . ?
N4 C4 C3 122.4(6) . . ?
C4 C3 C2 120.1(6) . . ?
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
Cu1 O2 1.962(4) . ?
Cu1 O2 1.962(4) 5_665 ?
Cu1 N1 1.984(5) 5_665 ?
Cu1 N1 1.984(5) . ?
Cu1 O1 2.596(4) 2_655 ?
Cu1 O1 2.596(4) 6_565 ?
Co1 N1 2.106(5) 8_466 ?
Co1 N1 2.106(5) 7_565 ?
Co1 O1 2.113(4) 4 ?
Co1 O1 2.113(4) 3_455 ?
Co1 N4 2.134(5) 2 ?
Co1 N4 2.134(5) . ?
O1 C1 1.258(7) . ?
O1 Ni1 2.113(4) 3_545 ?
O1 Co1 2.113(4) 3_545 ?
O1 Cu1 2.596(4) 2_655 ?
O2 C1 1.263(7) . ?
N4 C5 1.318(8) . ?
N4 C4 1.341(7) . ?
N1 N2 1.205(7) . ?
N1 Ni1 2.106(5) 7_565 ?
N1 Co1 2.106(5) 7_565 ?
N2 N3 1.137(7) . ?
C2 C6 1.367(8) . ?
C2 C3 1.385(8) . ?
C2 C1 1.509(8) . ?
C6 C5 1.386(9) . ?
C4 C3 1.373(8) . ?
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
O2 Cu1 O2 C1 142(100) 5_665 . . . ?
N1 Cu1 O2 C1 36.6(6) 5_665 . . . ?
N1 Cu1 O2 C1 -143.4(6) . . . . ?
O1 Cu1 O2 C1 -38.4(6) 2_655 . . . ?
O1 Cu1 O2 C1 141.6(6) 6_565 . . . ?
N1 Co1 N4 C5 58.7(6) 8_466 . . . ?
N1 Co1 N4 C5 -127.3(6) 7_565 . . . ?
O1 Co1 N4 C5 148.2(6) 4 . . . ?
O1 Co1 N4 C5 126.0(17) 3_455 . . . ?
N4 Co1 N4 C5 -33.7(5) 2 . . . ?
N1 Co1 N4 C4 -121.7(4) 8_466 . . . ?
N1 Co1 N4 C4 52.3(4) 7_565 . . . ?
O1 Co1 N4 C4 -32.2(4) 4 . . . ?
O1 Co1 N4 C4 -54.4(19) 3_455 . . . ?
N4 Co1 N4 C4 145.9(5) 2 . . . ?
O2 Cu1 N1 N2 28.8(5) . . . . ?
O2 Cu1 N1 N2 -151.2(5) 5_665 . . . ?
N1 Cu1 N1 N2 124(100) 5_665 . . . ?
O1 Cu1 N1 N2 -54.9(5) 2_655 . . . ?
O1 Cu1 N1 N2 125.1(5) 6_565 . . . ?
O2 Cu1 N1 Ni1 -114.6(2) . . . 7_565 ?
O2 Cu1 N1 Ni1 65.4(2) 5_665 . . 7_565 ?
N1 Cu1 N1 Ni1 -20(100) 5_665 . . 7_565 ?
O1 Cu1 N1 Ni1 161.67(17) 2_655 . . 7_565 ?
O1 Cu1 N1 Ni1 -18.33(17) 6_565 . . 7_565 ?
O2 Cu1 N1 Co1 -114.6(2) . . . 7_565 ?
O2 Cu1 N1 Co1 65.4(2) 5_665 . . 7_565 ?
N1 Cu1 N1 Co1 -20(100) 5_665 . . 7_565 ?
O1 Cu1 N1 Co1 161.67(17) 2_655 . . 7_565 ?
O1 Cu1 N1 Co1 -18.33(17) 6_565 . . 7_565 ?
Cu1 N1 N2 N3 116(100) . . . . ?
Ni1 N1 N2 N3 -105(100) 7_565 . . . ?
Co1 N1 N2 N3 -105(100) 7_565 . . . ?
C3 C2 C6 C5 1.6(10) . . . . ?
C1 C2 C6 C5 -176.5(6) . . . . ?
C4 N4 C5 C6 -4.9(10) . . . . ?
Co1 N4 C5 C6 174.8(5) . . . . ?
C2 C6 C5 N4 2.2(11) . . . . ?
Ni1 O1 C1 O2 -1.2(10) 3_545 . . . ?
Co1 O1 C1 O2 -1.2(10) 3_545 . . . ?
Cu1 O1 C1 O2 112.3(6) 2_655 . . . ?
Ni1 O1 C1 C2 178.9(4) 3_545 . . . ?
Co1 O1 C1 C2 178.9(4) 3_545 . . . ?
Cu1 O1 C1 C2 -67.6(6) 2_655 . . . ?
Cu1 O2 C1 O1 -0.8(10) . . . . ?
Cu1 O2 C1 C2 179.0(4) . . . . ?
C6 C2 C1 O1 -21.7(9) . . . . ?
C3 C2 C1 O1 160.3(6) . . . . ?
C6 C2 C1 O2 158.5(6) . . . . ?
C3 C2 C1 O2 -19.6(8) . . . . ?
C5 N4 C4 C3 3.8(9) . . . . ?
Co1 N4 C4 C3 -175.9(5) . . . . ?
N4 C4 C3 C2 -0.1(9) . . . . ?
C6 C2 C3 C4 -2.6(9) . . . . ?
C1 C2 C3 C4 175.6(6) . . . . ?
