#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:34:58 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179252 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/72/4317281.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_4317281
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 Cu N8 Ni O4'
_chemical_formula_weight         450.51
_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                 104.44(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.843(3)
_cell_length_b                   13.229(3)
_cell_length_c                   10.517(2)
_cell_measurement_reflns_used    7855
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      3.1
_cell_volume                     1730.4(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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  SCX-MINI
_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  0.0537
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8853
_diffrn_reflns_theta_full        27.60
_diffrn_reflns_theta_max         27.60
_diffrn_reflns_theta_min         3.08
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  0
_diffrn_standards_number         8853
_exptl_absorpt_coefficient_mu    2.353
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0419P)²+7.1860P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0946
_reflns_number_gt                1630
_reflns_number_total             1991
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101089n_si_002_1.cif
_cod_data_source_block           1
_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        1730.4(6)
_cod_database_code               4317281
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 0.64693(4) -0.2500 0.01645(16) Uani 1 2 d S . .
Cu1 Cu 0.5000 0.5000 0.0000 0.02136(17) Uani 1 2 d S . .
N4 N 0.3783(2) 0.7524(2) -0.2461(3) 0.0231(6) Uani 1 1 d . . .
N1 N 0.5440(2) 0.6359(2) -0.0447(3) 0.0238(6) Uani 1 1 d . . .
N2 N 0.5373(3) 0.7087(2) 0.0218(3) 0.0328(7) Uani 1 1 d . . .
C5 C 0.2279(3) 0.7906(3) -0.1582(4) 0.0283(8) Uani 1 1 d . . .
H5A H 0.1803 0.7692 -0.1100 0.034 Uiso 1 1 calc R . .
C4 C 0.3075(3) 0.7270(3) -0.1765(4) 0.0276(8) Uani 1 1 d . . .
H4A H 0.3127 0.6630 -0.1388 0.033 Uiso 1 1 calc R . .
C3 C 0.3652(3) 0.8432(3) -0.3032(4) 0.0342(9) Uani 1 1 d . . .
H3A H 0.4110 0.8614 -0.3554 0.041 Uiso 1 1 calc R . .
N3 N 0.5308(4) 0.7783(3) 0.0826(4) 0.0633(12) Uani 1 1 d . . .
O2 O 0.1046(2) 0.93748(19) -0.0833(2) 0.0325(6) Uani 1 1 d . . .
C1 C 0.2189(3) 0.8862(3) -0.2118(3) 0.0237(7) Uani 1 1 d . . .
C6 C 0.1367(3) 0.9589(2) -0.1838(3) 0.0215(7) Uani 1 1 d . . .
C2 C 0.2879(3) 0.9117(3) -0.2894(4) 0.0356(9) Uani 1 1 d . . .
H2A H 0.2821 0.9740 -0.3315 0.043 Uiso 1 1 calc R . .
O1 O 0.10885(19) 1.03100(17) -0.2611(2) 0.0240(5) 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'
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 172.00(15) . 2_654 ?
N1 Ni1 O1 84.49(10) . 4_544 ?
N1 Ni1 O1 89.65(10) 2_654 4_544 ?
N1 Ni1 O1 89.65(10) . 3_545 ?
N1 Ni1 O1 84.49(10) 2_654 3_545 ?
O1 Ni1 O1 86.06(13) 4_544 3_545 ?
N1 Ni1 N4 93.17(11) . 2_654 ?
N1 Ni1 N4 92.14(11) 2_654 2_654 ?
O1 Ni1 N4 174.16(11) 4_544 2_654 ?
O1 Ni1 N4 88.59(10) 3_545 2_654 ?
N1 Ni1 N4 92.14(11) . . ?
N1 Ni1 N4 93.17(11) 2_654 . ?
O1 Ni1 N4 88.59(10) 4_544 . ?
O1 Ni1 N4 174.16(11) 3_545 . ?
N4 Ni1 N4 96.86(16) 2_654 . ?
O2 Cu1 O2 180.00(12) 7_565 3_545 ?
O2 Cu1 N1 90.51(11) 7_565 5_665 ?
O2 Cu1 N1 89.49(11) 3_545 5_665 ?
O2 Cu1 N1 89.49(11) 7_565 . ?
O2 Cu1 N1 90.51(11) 3_545 . ?
N1 Cu1 N1 180.0 5_665 . ?
C3 N4 C4 116.3(3) . . ?
C3 N4 Ni1 126.8(2) . . ?
C4 N4 Ni1 116.8(2) . . ?
N2 N1 Cu1 121.5(2) . . ?
N2 N1 Ni1 120.1(2) . . ?
Cu1 N1 Ni1 106.79(13) . . ?
N3 N2 N1 178.8(4) . . ?
C4 C5 C1 119.6(3) . . ?
C4 C5 H5A 120.2 . . ?
C1 C5 H5A 120.2 . . ?
N4 C4 C5 123.4(3) . . ?
N4 C4 H4A 118.3 . . ?
C5 C4 H4A 118.3 . . ?
N4 C3 C2 123.9(3) . . ?
N4 C3 H3A 118.1 . . ?
C2 C3 H3A 118.1 . . ?
C6 O2 Cu1 133.2(2) . 3_455 ?
C5 C1 C2 117.5(3) . . ?
C5 C1 C6 119.7(3) . . ?
C2 C1 C6 122.7(3) . . ?
O1 C6 O2 128.3(3) . . ?
O1 C6 C1 117.4(3) . . ?
O2 C6 C1 114.3(3) . . ?
C3 C2 C1 119.0(3) . . ?
C3 C2 H2A 120.5 . . ?
C1 C2 H2A 120.5 . . ?
C6 O1 Ni1 127.6(2) . 3_455 ?
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 2.096(3) . ?
Ni1 N1 2.096(3) 2_654 ?
Ni1 O1 2.098(2) 4_544 ?
Ni1 O1 2.098(2) 3_545 ?
Ni1 N4 2.103(3) 2_654 ?
Ni1 N4 2.103(3) . ?
Cu1 O2 1.960(2) 7_565 ?
Cu1 O2 1.960(2) 3_545 ?
Cu1 N1 1.976(3) 5_665 ?
Cu1 N1 1.976(3) . ?
N4 C3 1.335(4) . ?
N4 C4 1.344(4) . ?
N1 N2 1.206(4) . ?
N2 N3 1.136(5) . ?
C5 C4 1.375(5) . ?
C5 C1 1.378(5) . ?
C5 H5A 0.9300 . ?
C4 H4A 0.9300 . ?
C3 C2 1.377(5) . ?
C3 H3A 0.9300 . ?
O2 C6 1.258(4) . ?
O2 Cu1 1.960(2) 3_455 ?
C1 C2 1.388(5) . ?
C1 C6 1.511(4) . ?
C6 O1 1.247(4) . ?
C2 H2A 0.9300 . ?
O1 Ni1 2.098(2) 3_455 ?
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 N4 C3 126.4(3) . . . . ?
N1 Ni1 N4 C3 -59.6(3) 2_654 . . . ?
O1 Ni1 N4 C3 -149.1(3) 4_544 . . . ?
O1 Ni1 N4 C3 -125.7(9) 3_545 . . . ?
N4 Ni1 N4 C3 33.0(3) 2_654 . . . ?
N1 Ni1 N4 C4 -52.0(3) . . . . ?
N1 Ni1 N4 C4 122.1(3) 2_654 . . . ?
O1 Ni1 N4 C4 32.5(3) 4_544 . . . ?
O1 Ni1 N4 C4 55.9(11) 3_545 . . . ?
N4 Ni1 N4 C4 -145.4(3) 2_654 . . . ?
O2 Cu1 N1 N2 28.7(3) 7_565 . . . ?
O2 Cu1 N1 N2 -151.3(3) 3_545 . . . ?
N1 Cu1 N1 N2 136(100) 5_665 . . . ?
O2 Cu1 N1 Ni1 -114.32(13) 7_565 . . . ?
O2 Cu1 N1 Ni1 65.68(13) 3_545 . . . ?
N1 Cu1 N1 Ni1 -7(100) 5_665 . . . ?
N1 Ni1 N1 N2 -165.0(3) 2_654 . . . ?
O1 Ni1 N1 N2 -121.9(3) 4_544 . . . ?
O1 Ni1 N1 N2 152.1(3) 3_545 . . . ?
N4 Ni1 N1 N2 63.5(3) 2_654 . . . ?
N4 Ni1 N1 N2 -33.5(3) . . . . ?
N1 Ni1 N1 Cu1 -21.35(10) 2_654 . . . ?
O1 Ni1 N1 Cu1 21.81(12) 4_544 . . . ?
O1 Ni1 N1 Cu1 -64.26(12) 3_545 . . . ?
N4 Ni1 N1 Cu1 -152.83(13) 2_654 . . . ?
N4 Ni1 N1 Cu1 110.18(13) . . . . ?
Cu1 N1 N2 N3 -153(22) . . . . ?
Ni1 N1 N2 N3 -15(22) . . . . ?
C3 N4 C4 C5 -2.7(5) . . . . ?
Ni1 N4 C4 C5 175.8(3) . . . . ?
C1 C5 C4 N4 -0.7(6) . . . . ?
C4 N4 C3 C2 3.0(6) . . . . ?
Ni1 N4 C3 C2 -175.4(3) . . . . ?
C4 C5 C1 C2 3.9(6) . . . . ?
C4 C5 C1 C6 -175.7(3) . . . . ?
Cu1 O2 C6 O1 0.8(6) 3_455 . . . ?
Cu1 O2 C6 C1 -179.0(2) 3_455 . . . ?
C5 C1 C6 O1 -159.5(3) . . . . ?
C2 C1 C6 O1 21.0(5) . . . . ?
C5 C1 C6 O2 20.3(5) . . . . ?
C2 C1 C6 O2 -159.2(4) . . . . ?
N4 C3 C2 C1 0.1(7) . . . . ?
C5 C1 C2 C3 -3.6(6) . . . . ?
C6 C1 C2 C3 175.9(4) . . . . ?
O2 C6 O1 Ni1 1.7(5) . . . 3_455 ?
C1 C6 O1 Ni1 -178.6(2) . . . 3_455 ?
