#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:59:21 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180054 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/00/7050072.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_7050072
loop_
_publ_author_name
'Bai, Shi-Qiang'
'Gao, En-Qing'
'He, Zheng'
'Fang, Chen-Jie'
'Yan, Chun-Hua'
_publ_section_title
;
 Crystal structures and magnetic behaviour of three new azido-bridged
 dinuclear cobalt(ii) and copper(ii) complexes
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              935
_journal_paper_doi               10.1039/b418239a
_journal_volume                  29
_journal_year                    2005
_chemical_formula_sum            'C11 H13 Cu N9'
_chemical_formula_weight         334.84
_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                 128.6544(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.3949(3)
_cell_length_b                   8.04680(10)
_cell_length_c                   18.7195(3)
_cell_measurement_reflns_used    12162
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     2869.64(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.76
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'NONIUS KappaCCD Diffractometer'
_diffrn_measurement_method       CCD
_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  0.0672
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24923
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.41
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.531
_exptl_absorpt_correction_T_max  0.806
_exptl_absorpt_correction_T_min  0.709
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.0017(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3300
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0324
_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)+(0.0424P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0775
_reflns_number_gt                2248
_reflns_number_total             3300
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b418239a.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7050072
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 0.072944(13) 0.89258(3) 0.074903(16) 0.03339(12) Uani 1 1 d . . .
N1 N 0.07823(8) 0.6931(2) 0.14612(10) 0.0298(4) Uani 1 1 d . . .
N2 N 0.14593(9) 1.0050(2) 0.19745(12) 0.0385(4) Uani 1 1 d . . .
N3 N 0.14582(9) 0.9765(2) 0.26961(11) 0.0385(4) Uani 1 1 d . . .
N4 N 0.09198(11) 0.7544(3) 0.00503(13) 0.0529(5) Uani 1 1 d . . .
N5 N 0.07824(10) 0.7989(2) -0.06499(14) 0.0452(5) Uani 1 1 d . . .
N6 N 0.06390(14) 0.8376(3) -0.13401(16) 0.0719(7) Uani 1 1 d . . .
N7 N -0.04267(9) 0.9055(2) 0.00347(12) 0.0392(4) Uani 1 1 d . . .
N8 N -0.07173(9) 0.8277(2) 0.02539(12) 0.0407(4) Uani 1 1 d . . .
N9 N -0.09725(12) 0.7494(3) 0.04856(16) 0.0738(7) Uani 1 1 d . . .
C1 C 0.07457(11) 0.5378(3) 0.11774(14) 0.0373(5) Uani 1 1 d . . .
H1 H 0.0723 0.5230 0.0667 0.045 Uiso 1 1 calc R . .
C2 C 0.07403(12) 0.4005(3) 0.15984(16) 0.0463(6) Uani 1 1 d . . .
H2 H 0.0710 0.2947 0.1376 0.056 Uiso 1 1 calc R . .
C3 C 0.07811(14) 0.4216(3) 0.23626(17) 0.0529(7) Uani 1 1 d . . .
H3 H 0.0780 0.3301 0.2666 0.063 Uiso 1 1 calc R . .
C4 C 0.08228(12) 0.5794(3) 0.26668(15) 0.0451(6) Uani 1 1 d . . .
H4 H 0.0852 0.5961 0.3181 0.054 Uiso 1 1 calc R . .
C5 C 0.08215(10) 0.7133(3) 0.22091(13) 0.0329(5) Uani 1 1 d . . .
C6 C 0.08649(12) 0.8898(3) 0.25166(15) 0.0398(5) Uani 1 1 d . . .
H6A H 0.0436 0.9483 0.2046 0.048 Uiso 1 1 calc R . .
H6B H 0.0907 0.8886 0.3067 0.048 Uiso 1 1 calc R . .
C7 C 0.20758(13) 1.0255(3) 0.34949(15) 0.0506(6) Uani 1 1 d . . .
C8 C 0.24656(13) 1.0888(3) 0.32759(17) 0.0584(7) Uani 1 1 d . . .
H8 H 0.2913 1.1340 0.3685 0.070 Uiso 1 1 calc R . .
C9 C 0.20842(12) 1.0747(3) 0.23318(16) 0.0469(6) Uani 1 1 d . . .
C10 C 0.22797(14) 1.1157(4) 0.1754(2) 0.0758(10) Uani 1 1 d . . .
H10A H 0.2080 1.0352 0.1272 0.114 Uiso 1 1 calc R . .
H10B H 0.2782 1.1145 0.2118 0.114 Uiso 1 1 calc R . .
H10C H 0.2105 1.2243 0.1494 0.114 Uiso 1 1 calc R . .
C11 C 0.22355(16) 1.0027(4) 0.44009(17) 0.0796(10) Uani 1 1 d . . .
H11A H 0.1917 1.0683 0.4421 0.119 Uiso 1 1 calc R . .
H11B H 0.2709 1.0375 0.4880 0.119 Uiso 1 1 calc R . .
H11C H 0.2184 0.8876 0.4483 0.119 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'
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
N4 Cu1 N7 95.92(8) . 5_575 ?
N4 Cu1 N2 126.34(8) . . ?
N7 Cu1 N2 97.36(7) 5_575 . ?
N4 Cu1 N1 92.57(7) . . ?
N7 Cu1 N1 164.76(7) 5_575 . ?
N2 Cu1 N1 87.68(6) . . ?
N4 Cu1 N7 110.99(8) . . ?
N7 Cu1 N7 76.95(8) 5_575 . ?
N2 Cu1 N7 122.63(7) . . ?
N1 Cu1 N7 88.21(6) . . ?
C1 N1 C5 117.83(18) . . ?
C1 N1 Cu1 120.94(13) . . ?
C5 N1 Cu1 121.16(13) . . ?
C9 N2 N3 106.18(18) . . ?
C9 N2 Cu1 131.81(17) . . ?
N3 N2 Cu1 119.77(13) . . ?
C7 N3 N2 110.61(19) . . ?
C7 N3 C6 131.1(2) . . ?
N2 N3 C6 118.01(16) . . ?
N5 N4 Cu1 122.63(16) . . ?
N6 N5 N4 178.0(3) . . ?
N8 N7 Cu1 130.74(15) . 5_575 ?
N8 N7 Cu1 124.44(14) . . ?
Cu1 N7 Cu1 103.05(8) 5_575 . ?
N9 N8 N7 177.3(2) . . ?
N1 C1 C2 123.4(2) . . ?
C1 C2 C3 118.6(2) . . ?
C4 C3 C2 118.9(2) . . ?
C3 C4 C5 119.8(2) . . ?
N1 C5 C4 121.50(19) . . ?
N1 C5 C6 116.74(18) . . ?
C4 C5 C6 121.76(19) . . ?
N3 C6 C5 111.36(17) . . ?
C8 C7 N3 106.4(2) . . ?
C8 C7 C11 131.1(2) . . ?
N3 C7 C11 122.5(3) . . ?
C7 C8 C9 108.4(2) . . ?
N2 C9 C8 108.4(2) . . ?
N2 C9 C10 121.1(2) . . ?
C8 C9 C10 130.5(2) . . ?
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 1.9803(19) . ?
Cu1 N7 1.9960(17) 5_575 ?
Cu1 N2 2.0369(17) . ?
Cu1 N1 2.0385(16) . ?
Cu1 N7 2.2455(18) . ?
N1 C1 1.339(3) . ?
N1 C5 1.352(2) . ?
N2 C9 1.346(3) . ?
N2 N3 1.372(2) . ?
N3 C7 1.359(3) . ?
N3 C6 1.445(3) . ?
N4 N5 1.187(2) . ?
N5 N6 1.151(3) . ?
N7 N8 1.194(2) . ?
N7 Cu1 1.9960(17) 5_575 ?
N8 N9 1.145(3) . ?
C1 C2 1.362(3) . ?
C2 C3 1.381(3) . ?
C3 C4 1.370(3) . ?
C4 C5 1.375(3) . ?
C5 C6 1.511(3) . ?
C7 C8 1.349(4) . ?
C7 C11 1.495(3) . ?
C8 C9 1.396(3) . ?
C9 C10 1.466(4) . ?
