#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:53:20 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179429 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/26/4332660.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4332660
loop_
_publ_author_name
'Li, Licun'
'Liao, Daizheng'
'Jiang, Zonghui'
'Mouesca, Jean-Marie'
'Rey, Paul'
_publ_section_title
;
 An Unprecedented Asymmetric End-On Azido-Bridged Copper(II) Imino
 Nitroxide Complex: Structure, Magnetic Properties, and Density Functional
 Theory Analysis
;
_journal_issue                   19
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7665
_journal_page_last               7670
_journal_paper_doi               10.1021/ic0606429
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C24 H32 Cu2 N18 O2'
_chemical_formula_weight         731.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 103.571(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.9638(15)
_cell_length_b                   19.811(3)
_cell_length_c                   7.2993(10)
_cell_measurement_temperature    298(2)
_cell_volume                     1541.2(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6339
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    1.437
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             752
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0421
_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)+(0.0590P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1141
_reflns_number_gt                1732
_reflns_number_total             2720
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0606429sup1.cif
_cod_data_source_block           000913a
_cod_database_code               4332660
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Cu1 Cu 0.39795(5) 0.04166(3) 1.08500(7) 0.0410(2) Uani 1 1 d .
O1 O 0.2278(3) 0.25564(14) 0.7102(4) 0.0494(8) Uani 1 1 d .
N1 N 0.4966(3) 0.12986(17) 1.0806(5) 0.0379(9) Uani 1 1 d .
N2 N 0.2635(3) 0.10075(15) 0.9279(4) 0.0333(8) Uani 1 1 d .
N3 N 0.2129(3) 0.19701(16) 0.7710(5) 0.0360(8) Uani 1 1 d .
N4 N 0.4488(3) 0.00574(18) 0.7927(5) 0.0447(9) Uani 1 1 d .
N5 N 0.4410(3) 0.0468(2) 0.6688(6) 0.0485(10) Uani 1 1 d .
N6 N 0.4275(4) 0.0856(3) 0.5495(7) 0.0854(17) Uani 1 1 d .
N7 N 0.2830(4) -0.0267(2) 1.1321(6) 0.0724(14) Uani 1 1 d .
N8 N 0.2705(3) -0.0484(2) 1.2729(7) 0.0497(10) Uani 1 1 d .
N9 N 0.2500(5) -0.0731(3) 1.4062(7) 0.0885(17) Uani 1 1 d .
C1 C 0.6158(4) 0.1409(2) 1.1664(6) 0.0492(12) Uani 1 1 d .
H1A H 0.6630 0.1053 1.2295 0.059 Uiso 1 1 calc R
C2 C 0.6718(4) 0.2027(2) 1.1655(7) 0.0514(13) Uani 1 1 d .
H2A H 0.7560 0.2084 1.2250 0.062 Uiso 1 1 calc R
C3 C 0.6024(4) 0.2563(3) 1.0757(7) 0.0523(13) Uani 1 1 d .
H3A H 0.6383 0.2990 1.0789 0.063 Uiso 1 1 calc R
C4 C 0.4783(4) 0.2460(2) 0.9804(6) 0.0439(11) Uani 1 1 d .
H4A H 0.4298 0.2809 0.9159 0.053 Uiso 1 1 calc R
C5 C 0.4296(4) 0.1818(2) 0.9854(6) 0.0345(10) Uani 1 1 d .
C6 C 0.3019(4) 0.15995(19) 0.8959(5) 0.0327(9) Uani 1 1 d .
C7 C 0.1272(4) 0.09346(19) 0.8357(6) 0.0334(10) Uani 1 1 d .
C8 C 0.0583(4) 0.0992(2) 0.9934(6) 0.0498(12) Uani 1 1 d .
H8A H 0.0784 0.0610 1.0758 0.075 Uiso 1 1 calc R
H8B H -0.0305 0.1004 0.9404 0.075 Uiso 1 1 calc R
H8C H 0.0836 0.1399 1.0635 0.075 Uiso 1 1 calc R
C9 C 0.1027(4) 0.02517(19) 0.7423(6) 0.0449(12) Uani 1 1 d .
H9A H 0.1203 -0.0095 0.8366 0.067 Uiso 1 1 calc R
H9B H 0.1558 0.0193 0.6559 0.067 Uiso 1 1 calc R
H9C H 0.0164 0.0223 0.6749 0.067 Uiso 1 1 calc R
C10 C 0.1007(4) 0.1536(2) 0.6922(6) 0.0358(10) Uani 1 1 d .
C11 C -0.0175(4) 0.1937(2) 0.6886(7) 0.0534(13) Uani 1 1 d .
H11A H -0.0254 0.2292 0.5970 0.080 Uiso 1 1 calc R
H11B H -0.0129 0.2129 0.8108 0.080 Uiso 1 1 calc R
H11C H -0.0891 0.1645 0.6558 0.080 Uiso 1 1 calc R
C12 C 0.1069(5) 0.1357(2) 0.4925(6) 0.0502(12) Uani 1 1 d .
H12A H 0.0898 0.1752 0.4144 0.075 Uiso 1 1 calc R
H12B H 0.0458 0.1015 0.4441 0.075 Uiso 1 1 calc R
H12C H 0.1892 0.1191 0.4927 0.075 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'
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
N7 Cu1 N4 96.26(17) . 3_657
N7 Cu1 N2 95.02(16) . .
N4 Cu1 N2 167.69(15) 3_657 .
N7 Cu1 N1 164.36(19) . .
N4 Cu1 N1 90.95(15) 3_657 .
N2 Cu1 N1 79.34(13) . .
N7 Cu1 N4 104.13(17) . .
N4 Cu1 N4 84.85(15) 3_657 .
N2 Cu1 N4 87.63(13) . .
N1 Cu1 N4 90.29(13) . .
C1 N1 C5 118.1(4) . .
C1 N1 Cu1 126.5(3) . .
C5 N1 Cu1 115.4(3) . .
C6 N2 C7 110.0(3) . .
C6 N2 Cu1 114.0(3) . .
C7 N2 Cu1 136.1(3) . .
O1 N3 C6 126.1(3) . .
O1 N3 C10 123.5(3) . .
C6 N3 C10 109.7(3) . .
N5 N4 Cu1 124.8(3) . 3_657
N5 N4 Cu1 118.0(3) . .
Cu1 N4 Cu1 95.15(15) 3_657 .
N6 N5 N4 176.8(5) . .
N8 N7 Cu1 129.7(4) . .
N7 N8 N9 174.6(5) . .
N1 C1 C2 122.5(4) . .
C1 C2 C3 119.5(4) . .
C2 C3 C4 119.3(4) . .
C5 C4 C3 117.4(4) . .
N1 C5 C4 123.0(4) . .
N1 C5 C6 110.5(3) . .
C4 C5 C6 126.5(4) . .
N2 C6 N3 113.2(3) . .
N2 C6 C5 120.5(4) . .
N3 C6 C5 126.2(3) . .
N2 C7 C9 110.1(3) . .
N2 C7 C8 105.9(3) . .
C9 C7 C8 109.9(3) . .
N2 C7 C10 103.7(3) . .
C9 C7 C10 113.2(3) . .
C8 C7 C10 113.6(3) . .
N3 C10 C11 109.1(3) . .
N3 C10 C12 106.5(3) . .
C11 C10 C12 109.7(4) . .
N3 C10 C7 99.9(3) . .
C11 C10 C7 115.7(4) . .
C12 C10 C7 114.9(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N7 1.935(4) .
Cu1 N4 1.948(4) 3_657
Cu1 N2 2.016(3) .
Cu1 N1 2.059(3) .
Cu1 N4 2.434(4) .
O1 N3 1.268(4) .
N1 C1 1.328(5) .
N1 C5 1.357(5) .
N2 C6 1.286(5) .
N2 C7 1.495(5) .
N3 C6 1.380(5) .
N3 C10 1.500(5) .
N4 N5 1.205(5) .
N4 Cu1 1.948(4) 3_657
N5 N6 1.144(5) .
N7 N8 1.152(5) .
N8 N9 1.157(6) .
C1 C2 1.370(6) .
C2 C3 1.380(6) .
C3 C4 1.390(6) .
C4 C5 1.383(5) .
C5 C6 1.465(5) .
C7 C9 1.511(5) .
C7 C8 1.522(6) .
C7 C10 1.568(5) .
C10 C11 1.515(6) .
C10 C12 1.518(6) .
