#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/72/4317284.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_4317284
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 Co0.6 Cu N8 Ni0.4 O4'
_chemical_formula_weight         450.65
_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                   12.890(3)
_cell_length_b                   13.350(3)
_cell_length_c                   10.496(2)
_cell_measurement_reflns_used    8004
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     1749.0(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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0312
_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            7429
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    2.251
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.711
_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          0.16
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1535
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0355
_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)+(0.0237P)²+3.9377P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0687
_reflns_number_gt                1302
_reflns_number_total             1535
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101089n_si_002_4.cif
_cod_data_source_block           4
_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        1749.1(6)
_cod_original_formula_sum        'C12 H8 Co0.60 Cu N8 Ni0.40 O4'
_cod_database_code               4317284
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 0.35290(4) 0.2500 0.01470(17) Uani 0.40 2 d SP . .
Co1 Co 0.5000 0.35290(4) 0.2500 0.01470(17) Uani 0.60 2 d SP . .
O2 O 0.39534(19) 0.56217(17) 0.0829(2) 0.0304(6) Uani 1 1 d . . .
N1 N 0.4565(2) 0.36466(19) 0.0441(3) 0.0222(6) Uani 1 1 d . . .
C1 C 0.3629(2) 0.5415(2) 0.1840(3) 0.0194(7) Uani 1 1 d . . .
Cu1 Cu 0.5000 0.5000 0.0000 0.01984(17) Uani 1 2 d S . .
O1 O 0.39086(17) 0.46942(16) 0.2611(2) 0.0224(5) Uani 1 1 d . . .
N2 N 0.4626(2) 0.2920(2) -0.0228(3) 0.0318(7) Uani 1 1 d . . .
C2 C 0.2808(3) 0.6137(2) 0.2113(3) 0.0209(7) Uani 1 1 d . . .
N3 N 0.4690(4) 0.2225(3) -0.0836(4) 0.0645(12) Uani 1 1 d . . .
C3 C 0.2721(3) 0.7086(2) 0.1585(3) 0.0261(8) Uani 1 1 d . . .
H3A H 0.3197 0.7301 0.1108 0.031 Uiso 1 1 calc R . .
N4 N 0.1224(2) 0.7458(2) 0.2463(3) 0.0213(6) Uani 1 1 d . . .
C4 C 0.1925(3) 0.7711(2) 0.1768(3) 0.0266(8) Uani 1 1 d . . .
H4A H 0.1870 0.8345 0.1389 0.032 Uiso 1 1 calc R . .
C5 C 0.1347(3) 0.6556(3) 0.3024(4) 0.0339(9) Uani 1 1 d . . .
H5A H 0.0887 0.6371 0.3538 0.041 Uiso 1 1 calc R . .
C6 C 0.2122(3) 0.5880(3) 0.2881(4) 0.0347(10) Uani 1 1 d . . .
H6A H 0.2181 0.5260 0.3298 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'
Cu Cu 0.3201 1.2651 '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'
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 171.42(15) . 2_655 ?
N1 Ni1 O1 84.21(10) . 2_655 ?
N1 Ni1 O1 89.49(10) 2_655 2_655 ?
N1 Ni1 O1 89.49(10) . . ?
N1 Ni1 O1 84.21(10) 2_655 . ?
O1 Ni1 O1 85.59(12) 2_655 . ?
N1 Ni1 N4 92.30(10) . 3_545 ?
N1 Ni1 N4 93.44(11) 2_655 3_545 ?
O1 Ni1 N4 89.24(9) 2_655 3_545 ?
O1 Ni1 N4 174.34(10) . 3_545 ?
N1 Ni1 N4 93.44(11) . 4_545 ?
N1 Ni1 N4 92.30(10) 2_655 4_545 ?
O1 Ni1 N4 174.34(10) 2_655 4_545 ?
O1 Ni1 N4 89.24(9) . 4_545 ?
N4 Ni1 N4 96.00(14) 3_545 4_545 ?
C1 O2 Cu1 133.5(2) . . ?
N2 N1 Cu1 122.1(2) . . ?
N2 N1 Ni1 119.8(2) . . ?
Cu1 N1 Ni1 106.87(12) . . ?
O1 C1 O2 127.5(3) . . ?
O1 C1 C2 118.0(3) . . ?
O2 C1 C2 114.5(3) . . ?
O2 Cu1 O2 180.00(9) 5_665 . ?
O2 Cu1 N1 89.08(10) 5_665 . ?
O2 Cu1 N1 90.92(10) . . ?
O2 Cu1 N1 90.92(10) 5_665 5_665 ?
O2 Cu1 N1 89.08(10) . 5_665 ?
N1 Cu1 N1 180.00(15) . 5_665 ?
O2 Cu1 O1 84.53(9) 5_665 6_565 ?
O2 Cu1 O1 95.47(9) . 6_565 ?
N1 Cu1 O1 104.68(9) . 6_565 ?
N1 Cu1 O1 75.32(9) 5_665 6_565 ?
O2 Cu1 O1 95.47(9) 5_665 2_655 ?
O2 Cu1 O1 84.53(9) . 2_655 ?
N1 Cu1 O1 75.32(9) . 2_655 ?
N1 Cu1 O1 104.68(9) 5_665 2_655 ?
O1 Cu1 O1 180.00(9) 6_565 2_655 ?
C1 O1 Ni1 128.1(2) . . ?
C1 O1 Cu1 120.4(2) . 2_655 ?
Ni1 O1 Cu1 87.78(8) . 2_655 ?
N3 N2 N1 178.7(4) . . ?
C3 C2 C6 117.7(3) . . ?
C3 C2 C1 120.1(3) . . ?
C6 C2 C1 122.2(3) . . ?
C4 C3 C2 119.5(3) . . ?
C5 N4 C4 116.5(3) . . ?
C5 N4 Co1 127.2(2) . 3_455 ?
C4 N4 Co1 116.3(2) . 3_455 ?
C5 N4 Ni1 127.2(2) . 3_455 ?
C4 N4 Ni1 116.3(2) . 3_455 ?
Co1 N4 Ni1 0.0 3_455 3_455 ?
N4 C4 C3 123.5(3) . . ?
N4 C5 C6 123.5(3) . . ?
C2 C6 C5 119.1(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 2.099(3) . ?
Ni1 N1 2.099(3) 2_655 ?
Ni1 O1 2.120(2) 2_655 ?
Ni1 O1 2.120(2) . ?
Ni1 N4 2.137(3) 3_545 ?
Ni1 N4 2.137(3) 4_545 ?
O2 C1 1.265(4) . ?
O2 Cu1 1.962(2) . ?
N1 N2 1.211(4) . ?
N1 Cu1 1.981(3) . ?
C1 O1 1.252(4) . ?
C1 C2 1.510(4) . ?
Cu1 O2 1.962(2) 5_665 ?
Cu1 N1 1.981(3) 5_665 ?
Cu1 O1 2.583(2) 6_565 ?
Cu1 O1 2.583(2) 2_655 ?
O1 Cu1 2.583(2) 2_655 ?
N2 N3 1.141(4) . ?
C2 C3 1.376(4) . ?
C2 C6 1.381(4) . ?
C3 C4 1.373(4) . ?
N4 C5 1.333(4) . ?
N4 C4 1.338(4) . ?
N4 Co1 2.137(3) 3_455 ?
N4 Ni1 2.137(3) 3_455 ?
C5 C6 1.381(5) . ?
