Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2002

data_010320b 

_database_code_CSD	171153


_journal_coden_Cambridge      186

_publ_requested_journal       'Dalton Transactions'

loop_
_publ_author_name
'Jiang, Zong-Hui'
'Li, Licun'
'Liao, Daizheng'
'Yan, Shi-Ping'

_publ_contact_author_name     	'Dr Licun Li' 
_publ_contact_author_address 
;
Department of Chemistry
Nankai University
Tianjin
300071
CHINA
;

_publ_contact_author_email       'LLICUN@EYOU.COM'

_publ_section_title		
;
A novel two dimensional copper (II)-radical complex
[Cu(NITmPy)2(N3)2]n: structure and magnetic properties
;

_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C24 H32 Cu N12 O4' 
_chemical_formula_weight          616.16 

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' 
'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' 
'N'  'N'   0.0061   0.0033 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/c 

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' 

_cell_length_a                    10.239(3) 
_cell_length_b                    11.040(4) 
_cell_length_c                    12.383(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  101.761(6) 
_cell_angle_gamma                 90.00 
_cell_volume                      1370.3(7) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.30 
_exptl_crystal_size_mid           0.25 
_exptl_crystal_size_min           0.20 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.493 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              642 
_exptl_absorpt_coefficient_mu     0.853 
_exptl_absorpt_correction_type    none 
_exptl_absorpt_correction_T_min   0.7840 
_exptl_absorpt_correction_T_max   0.8480 
_exptl_absorpt_process_details    ? 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'CCD area detector' 
_diffrn_measurement_method        'phi and omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             5575 
_diffrn_reflns_av_R_equivalents   0.0577 
_diffrn_reflns_av_sigmaI/netI     0.0915 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        10 
_diffrn_reflns_theta_min          2.03 
_diffrn_reflns_theta_max          25.03 
_reflns_number_total              2417 
_reflns_number_gt                 1460 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SMART' 
_computing_data_reduction         'Bruker SHELXTL' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 

_refine_special_details 
; 
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
goodness of fit S are based on F^2^, conventional R-factors R are based 
on F, with F set to zero for negative F^2^. The threshold expression of 
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F^2^ are statistically about twice as large as those based on F, and R- 
factors based on ALL data will be even larger. 
; 

_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
'calc w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          2417 
_refine_ls_number_parameters      187 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0893 
_refine_ls_R_factor_gt            0.0422 
_refine_ls_wR_factor_ref          0.0910 
_refine_ls_wR_factor_gt           0.0796 
_refine_ls_goodness_of_fit_ref    0.909 
_refine_ls_restrained_S_all       0.909 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 

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 1.0000 0.0000 1.0000 0.0301(2) Uani 1 2 d S . . 
O2 O 0.7783(3) 0.4394(2) 0.5856(2) 0.0467(7) Uani 1 1 d . . . 
N1 N 0.9035(3) 0.0788(2) 0.8559(2) 0.0254(7) Uani 1 1 d . . . 
N3 N 0.7240(3) 0.4481(2) 0.6694(2) 0.0290(7) Uani 1 1 d . . . 
N2 N 0.6590(3) 0.4064(2) 0.8226(2) 0.0308(7) Uani 1 1 d . . . 
C3 C 0.7990(3) 0.1870(3) 0.6543(3) 0.0313(9) Uani 1 1 d . . . 
H3A H 0.7660 0.2238 0.5867 0.038 Uiso 1 1 calc R . . 
N5 N 1.0897(3) 0.2403(3) 1.0056(3) 0.0413(9) Uani 1 1 d . . . 
C2 C 0.8564(4) 0.0743(3) 0.6595(3) 0.0339(9) Uani 1 1 d . . . 
H2A H 0.8607 0.0327 0.5949 0.041 Uiso 1 1 calc R . . 
C5 C 0.8446(3) 0.1877(3) 0.8514(3) 0.0241(8) Uani 1 1 d . . . 
H5A H 0.8393 0.2264 0.9171 0.029 Uiso 1 1 calc R . . 
N4 N 1.0859(3) 0.1506(3) 1.0553(2) 0.0476(10) Uani 1 1 d . . . 
C4 C 0.7914(3) 0.2450(3) 0.7523(3) 0.0235(8) Uani 1 1 d . . . 
C6 C 0.7281(3) 0.3637(3) 0.7494(3) 0.0261(8) Uani 1 1 d . . . 
O1 O 0.6415(3) 0.3519(2) 0.9085(2) 0.0559(8) Uani 1 1 d . . . 
C1 C 0.9073(3) 0.0233(3) 0.7597(3) 0.0308(9) Uani 1 1 d . . . 
H1A H 0.9463 -0.0530 0.7616 0.037 Uiso 1 1 calc R . . 
C7 C 0.5814(3) 0.5185(3) 0.7813(3) 0.0327(9) Uani 1 1 d . . . 
C8 C 0.6641(4) 0.5655(3) 0.6988(3) 0.0315(9) Uani 1 1 d . . . 
C9 C 0.5738(4) 0.6030(3) 0.8768(3) 0.0495(11) Uani 1 1 d . . . 
H9A H 0.5204 0.5663 0.9232 0.074 Uiso 1 1 calc R . . 
H9B H 0.5342 0.6783 0.8485 0.074 Uiso 1 1 calc R . . 
H9C H 0.6620 0.6175 0.9188 0.074 Uiso 1 1 calc R . . 
C12 C 0.5861(4) 0.6268(3) 0.5966(3) 0.0519(12) Uani 1 1 d . . . 
H12A H 0.6463 0.6529 0.5511 0.078 Uiso 1 1 calc R . . 
H12B H 0.5398 0.6956 0.6177 0.078 Uiso 1 1 calc R . . 
H12C H 0.5228 0.5707 0.5562 0.078 Uiso 1 1 calc R . . 
C11 C 0.7818(4) 0.6443(3) 0.7523(3) 0.0449(11) Uani 1 1 d . . . 
H11A H 0.8291 0.6707 0.6971 0.067 Uiso 1 1 calc R . . 
H11B H 0.8406 0.5983 0.8076 0.067 Uiso 1 1 calc R . . 
H11C H 0.7496 0.7136 0.7858 0.067 Uiso 1 1 calc R . . 
C10 C 0.4435(4) 0.4741(3) 0.7271(3) 0.0516(12) Uani 1 1 d . . . 
H10A H 0.3977 0.4462 0.7828 0.077 Uiso 1 1 calc R . . 
H10B H 0.4514 0.4088 0.6777 0.077 Uiso 1 1 calc R . . 
H10C H 0.3941 0.5393 0.6866 0.077 Uiso 1 1 calc R . . 
N6 N 1.0954(5) 0.3299(3) 0.9604(3) 0.0898(16) Uani 1 1 d . . . 

loop_ 
_atom_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
Cu1 0.0351(4) 0.0174(3) 0.0330(4) 0.0026(3) -0.0042(3) -0.0019(3) 
O2 0.070(2) 0.0368(15) 0.0408(16) 0.0060(13) 0.0277(15) 0.0066(14) 
N1 0.0257(17) 0.0203(16) 0.0293(17) 0.0014(13) 0.0030(13) 0.0001(14) 
N3 0.0365(19) 0.0248(16) 0.0262(17) 0.0010(14) 0.0074(15) 0.0050(14) 
N2 0.0350(19) 0.0302(17) 0.0282(18) 0.0062(15) 0.0091(15) 0.0067(15) 
C3 0.036(2) 0.031(2) 0.028(2) 0.0024(17) 0.0065(17) 0.0034(18) 
N5 0.051(2) 0.030(2) 0.037(2) -0.0017(17) -0.0040(16) -0.0129(18) 
C2 0.048(3) 0.026(2) 0.028(2) -0.0069(17) 0.0079(18) 0.0038(19) 
C5 0.024(2) 0.024(2) 0.023(2) -0.0015(16) 0.0012(16) 0.0005(16) 
N4 0.073(3) 0.0223(18) 0.037(2) 0.0044(16) -0.0117(18) -0.0110(18) 
C4 0.022(2) 0.0198(18) 0.029(2) -0.0048(16) 0.0057(16) 0.0011(15) 
C6 0.027(2) 0.029(2) 0.0200(19) -0.0010(17) -0.0007(17) 0.0033(17) 
O1 0.065(2) 0.0598(19) 0.0475(18) 0.0120(15) 0.0224(16) 0.0151(16) 
C1 0.031(2) 0.023(2) 0.039(2) -0.0033(18) 0.0067(17) 0.0008(16) 
C7 0.029(2) 0.026(2) 0.043(2) -0.0024(18) 0.0063(17) 0.0096(17) 
C8 0.033(2) 0.024(2) 0.035(2) -0.0011(17) 0.0012(18) 0.0080(18) 
C9 0.054(3) 0.043(3) 0.055(3) -0.011(2) 0.020(2) 0.007(2) 
C12 0.068(3) 0.031(2) 0.051(3) 0.007(2) 0.000(2) 0.013(2) 
C11 0.050(3) 0.036(2) 0.049(3) -0.005(2) 0.009(2) -0.001(2) 
C10 0.031(2) 0.049(3) 0.071(3) -0.002(2) 0.001(2) 0.007(2) 
N6 0.135(4) 0.047(2) 0.070(3) 0.022(2) -0.019(3) -0.043(3) 

_geom_special_details 
; 
All esds (except the esd in the dihedral angle between two l.s. planes) 
are estimated using the full covariance matrix.  The cell esds are taken 
into account individually in the estimation of esds in distances, angles 
and torsion angles; correlations between esds in cell parameters are only 
used when they are defined by crystal symmetry.  An approximate (isotropic) 
treatment of cell esds is used for estimating esds involving l.s. planes. 
; 

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 N4 1.939(3) . ? 
Cu1 N4 1.939(3) 3_757 ? 
Cu1 N1 2.049(3) 3_757 ? 
Cu1 N1 2.049(3) . ? 
O2 N3 1.277(3) . ? 
N1 C5 1.341(4) . ? 
N1 C1 1.347(4) . ? 
N3 C6 1.354(4) . ? 
N3 C8 1.509(4) . ? 
N2 O1 1.266(3) . ? 
N2 C6 1.344(4) . ? 
N2 C7 1.503(4) . ? 
C3 C2 1.373(4) . ? 
C3 C4 1.389(4) . ? 
N5 N6 1.144(4) . ? 
N5 N4 1.171(4) . ? 
C2 C1 1.365(4) . ? 
C5 C4 1.389(4) . ? 
C4 C6 1.459(4) . ? 
C7 C10 1.516(5) . ? 
C7 C9 1.520(4) . ? 
C7 C8 1.544(5) . ? 
C8 C12 1.512(5) . ? 
C8 C11 1.524(5) . ? 

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 
N4 Cu1 N4 180.000(1) . 3_757 ? 
N4 Cu1 N1 87.28(11) . 3_757 ? 
N4 Cu1 N1 92.72(11) 3_757 3_757 ? 
N4 Cu1 N1 92.72(11) . . ? 
N4 Cu1 N1 87.28(11) 3_757 . ? 
N1 Cu1 N1 180.00(9) 3_757 . ? 
C5 N1 C1 117.7(3) . . ? 
C5 N1 Cu1 123.3(2) . . ? 
C1 N1 Cu1 118.8(2) . . ? 
O2 N3 C6 126.1(3) . . ? 
O2 N3 C8 121.7(3) . . ? 
C6 N3 C8 111.6(3) . . ? 
O1 N2 C6 125.7(3) . . ? 
O1 N2 C7 121.4(3) . . ? 
C6 N2 C7 112.0(3) . . ? 
C2 C3 C4 118.5(3) . . ? 
N6 N5 N4 177.6(4) . . ? 
C1 C2 C3 119.8(3) . . ? 
N1 C5 C4 122.5(3) . . ? 
N5 N4 Cu1 126.9(3) . . ? 
C3 C4 C5 118.7(3) . . ? 
C3 C4 C6 119.7(3) . . ? 
C5 C4 C6 121.6(3) . . ? 
N2 C6 N3 108.0(3) . . ? 
N2 C6 C4 126.2(3) . . ? 
N3 C6 C4 125.7(3) . . ? 
N1 C1 C2 122.8(3) . . ? 
N2 C7 C10 105.4(3) . . ? 
N2 C7 C9 110.4(3) . . ? 
C10 C7 C9 110.6(3) . . ? 
N2 C7 C8 100.3(3) . . ? 
C10 C7 C8 113.8(3) . . ? 
C9 C7 C8 115.5(3) . . ? 
N3 C8 C12 110.7(3) . . ? 
N3 C8 C11 105.8(3) . . ? 
C12 C8 C11 110.1(3) . . ? 
N3 C8 C7 100.1(3) . . ? 
C12 C8 C7 115.9(3) . . ? 
C11 C8 C7 113.3(3) . . ? 

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 
N4 Cu1 N1 C5 -42.8(3) . . . . ? 
N4 Cu1 N1 C5 137.2(3) 3_757 . . . ? 
N1 Cu1 N1 C5 1(100) 3_757 . . . ? 
N4 Cu1 N1 C1 132.1(3) . . . . ? 
N4 Cu1 N1 C1 -47.9(3) 3_757 . . . ? 
N1 Cu1 N1 C1 176(100) 3_757 . . . ? 
C4 C3 C2 C1 -1.7(5) . . . . ? 
C1 N1 C5 C4 -1.5(5) . . . . ? 
Cu1 N1 C5 C4 173.4(2) . . . . ? 
N6 N5 N4 Cu1 171(11) . . . . ? 
N4 Cu1 N4 N5 143(100) 3_757 . . . ? 
N1 Cu1 N4 N5 168.8(4) 3_757 . . . ? 
N1 Cu1 N4 N5 -11.2(4) . . . . ? 
C2 C3 C4 C5 1.4(5) . . . . ? 
C2 C3 C4 C6 -178.6(3) . . . . ? 
N1 C5 C4 C3 0.2(5) . . . . ? 
N1 C5 C4 C6 -179.9(3) . . . . ? 
O1 N2 C6 N3 180.0(3) . . . . ? 
C7 N2 C6 N3 10.7(4) . . . . ? 
O1 N2 C6 C4 2.6(5) . . . . ? 
C7 N2 C6 C4 -166.8(3) . . . . ? 
O2 N3 C6 N2 -179.9(3) . . . . ? 
C8 N3 C6 N2 8.9(4) . . . . ? 
O2 N3 C6 C4 -2.4(5) . . . . ? 
C8 N3 C6 C4 -173.6(3) . . . . ? 
C3 C4 C6 N2 147.3(3) . . . . ? 
C5 C4 C6 N2 -32.6(5) . . . . ? 
C3 C4 C6 N3 -29.7(5) . . . . ? 
C5 C4 C6 N3 150.4(3) . . . . ? 
C5 N1 C1 C2 1.2(5) . . . . ? 
Cu1 N1 C1 C2 -173.9(3) . . . . ? 
C3 C2 C1 N1 0.3(5) . . . . ? 
O1 N2 C7 C10 -76.0(4) . . . . ? 
C6 N2 C7 C10 93.8(3) . . . . ? 
O1 N2 C7 C9 43.4(4) . . . . ? 
C6 N2 C7 C9 -146.8(3) . . . . ? 
O1 N2 C7 C8 165.6(3) . . . . ? 
C6 N2 C7 C8 -24.5(3) . . . . ? 
O2 N3 C8 C12 42.2(4) . . . . ? 
C6 N3 C8 C12 -146.2(3) . . . . ? 
O2 N3 C8 C11 -77.1(4) . . . . ? 
C6 N3 C8 C11 94.6(3) . . . . ? 
O2 N3 C8 C7 165.0(3) . . . . ? 
C6 N3 C8 C7 -23.3(3) . . . . ? 
N2 C7 C8 N3 26.3(3) . . . . ? 
C10 C7 C8 N3 -85.7(3) . . . . ? 
C9 C7 C8 N3 144.8(3) . . . . ? 
N2 C7 C8 C12 145.4(3) . . . . ? 
C10 C7 C8 C12 33.4(4) . . . . ? 
C9 C7 C8 C12 -96.1(4) . . . . ? 
N2 C7 C8 C11 -85.9(3) . . . . ? 
C10 C7 C8 C11 162.1(3) . . . . ? 
C9 C7 C8 C11 32.6(4) . . . . ? 

_diffrn_measured_fraction_theta_max    1.000 
_diffrn_reflns_theta_full              25.03 
_diffrn_measured_fraction_theta_full   1.000 
_refine_diff_density_max    0.272 
_refine_diff_density_min   -0.462 
_refine_diff_density_rms    0.064