#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:59:21 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180054 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/00/7050071.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_7050071
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 Co N9'
_chemical_formula_weight         330.23
_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                 128.8435(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.2866(4)
_cell_length_b                   8.1348(2)
_cell_length_c                   18.8753(4)
_cell_measurement_reflns_used    21852
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     2904.48(11)
_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, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.76
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_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  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0332
_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            29747
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.61
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.190
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.0022(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3337
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0303
_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)+(0.0480P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0740
_refine_ls_wR_factor_ref         0.0802
_reflns_number_gt                2514
_reflns_number_total             3337
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b418239a.txt
_cod_data_source_block           1
_cod_original_cell_volume        2904.47(11)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7050071
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
Co1 Co 0.067117(11) 0.87835(3) 0.072506(16) 0.03513(11) Uani 1 1 d . . .
N1 N 0.07757(7) 0.66953(18) 0.15027(10) 0.0358(3) Uani 1 1 d . . .
N2 N 0.14510(8) 0.98133(19) 0.19561(11) 0.0427(4) Uani 1 1 d . . .
N3 N 0.14740(8) 0.9533(2) 0.26901(11) 0.0434(4) Uani 1 1 d . . .
N4 N 0.09503(9) 0.7518(2) 0.01066(12) 0.0538(4) Uani 1 1 d . . .
N5 N 0.08358(9) 0.8020(2) -0.05729(14) 0.0551(5) Uani 1 1 d . . .
N6 N 0.07119(15) 0.8468(3) -0.12389(17) 0.0861(7) Uani 1 1 d . . .
N7 N -0.03707(8) 0.90123(19) 0.01195(11) 0.0412(4) Uani 1 1 d . . .
N8 N -0.06794(8) 0.8180(2) 0.02964(11) 0.0464(4) Uani 1 1 d . . .
N9 N -0.09747(10) 0.7401(3) 0.04674(15) 0.0782(7) Uani 1 1 d . . .
C1 C 0.07430(10) 0.5155(2) 0.12325(14) 0.0443(4) Uani 1 1 d . . .
H1 H 0.0707 0.4995 0.0717 0.053 Uiso 1 1 calc R . .
C2 C 0.07599(12) 0.3805(3) 0.16748(17) 0.0574(6) Uani 1 1 d . . .
H2 H 0.0736 0.2753 0.1464 0.069 Uiso 1 1 calc R . .
C3 C 0.08134(13) 0.4025(3) 0.24373(18) 0.0634(6) Uani 1 1 d . . .
H3 H 0.0815 0.3127 0.2743 0.076 Uiso 1 1 calc R . .
C4 C 0.08649(11) 0.5602(3) 0.27409(15) 0.0544(5) Uani 1 1 d . . .
H4 H 0.0915 0.5777 0.3266 0.065 Uiso 1 1 calc R . .
C5 C 0.08413(9) 0.6919(2) 0.22624(12) 0.0382(4) Uani 1 1 d . . .
C6 C 0.08864(10) 0.8668(2) 0.25516(14) 0.0452(5) Uani 1 1 d . . .
H6A H 0.0448 0.9232 0.2089 0.054 Uiso 1 1 calc R . .
H6B H 0.0949 0.8681 0.3112 0.054 Uiso 1 1 calc R . .
C7 C 0.20923(11) 1.0070(3) 0.34677(14) 0.0574(6) Uani 1 1 d . . .
C8 C 0.24712(11) 1.0720(3) 0.32294(17) 0.0644(7) Uani 1 1 d . . .
H8 H 0.2917 1.1195 0.3621 0.077 Uiso 1 1 calc R . .
C9 C 0.20678(10) 1.0543(3) 0.22911(16) 0.0534(5) Uani 1 1 d . . .
C10 C 0.22442(13) 1.0979(4) 0.16907(19) 0.0808(9) Uani 1 1 d . . .
H10A H 0.2005 1.0243 0.1181 0.121 Uiso 1 1 calc R . .
H10B H 0.2745 1.0889 0.2026 0.121 Uiso 1 1 calc R . .
H10C H 0.2097 1.2087 0.1478 0.121 Uiso 1 1 calc R . .
C11 C 0.22785(15) 0.9871(4) 0.43822(16) 0.0886(10) Uani 1 1 d . . .
H11A H 0.1955 1.0496 0.4406 0.133 Uiso 1 1 calc R . .
H11B H 0.2751 1.0259 0.4842 0.133 Uiso 1 1 calc R . .
H11C H 0.2249 0.8731 0.4486 0.133 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'
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
N4 Co1 N7 119.05(7) . . ?
N4 Co1 N2 118.09(7) . . ?
N7 Co1 N2 122.86(7) . . ?
N4 Co1 N1 93.11(7) . . ?
N7 Co1 N1 91.64(6) . . ?
N2 Co1 N1 85.37(6) . . ?
N4 Co1 N7 94.47(7) . 5_575 ?
N7 Co1 N7 77.71(6) . 5_575 ?
N2 Co1 N7 98.03(6) . 5_575 ?
N1 Co1 N7 169.00(5) . 5_575 ?
C1 N1 C5 118.06(16) . . ?
C1 N1 Co1 121.75(13) . . ?
C5 N1 Co1 120.12(12) . . ?
C9 N2 N3 105.73(16) . . ?
C9 N2 Co1 132.93(15) . . ?
N3 N2 Co1 120.19(11) . . ?
C7 N3 N2 110.87(17) . . ?
C7 N3 C6 130.10(19) . . ?
N2 N3 C6 118.93(15) . . ?
N5 N4 Co1 121.35(15) . . ?
N6 N5 N4 178.1(3) . . ?
N8 N7 Co1 124.50(13) . . ?
N8 N7 Co1 132.81(12) . 5_575 ?
Co1 N7 Co1 102.29(6) . 5_575 ?
N9 N8 N7 179.4(2) . . ?
N1 C1 C2 123.3(2) . . ?
C1 C2 C3 118.9(2) . . ?
C2 C3 C4 118.8(2) . . ?
C3 C4 C5 119.7(2) . . ?
N1 C5 C4 121.24(19) . . ?
N1 C5 C6 116.48(16) . . ?
C4 C5 C6 122.28(19) . . ?
N3 C6 C5 111.20(16) . . ?
N3 C7 C8 106.7(2) . . ?
N3 C7 C11 122.9(2) . . ?
C8 C7 C11 130.4(2) . . ?
C7 C8 C9 107.36(19) . . ?
N2 C9 C8 109.3(2) . . ?
N2 C9 C10 121.1(2) . . ?
C8 C9 C10 129.5(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
Co1 N4 1.9686(17) . ?
Co1 N7 2.0288(14) . ?
Co1 N2 2.0415(15) . ?
Co1 N1 2.1534(15) . ?
Co1 N7 2.1977(15) 5_575 ?
N1 C1 1.337(2) . ?
N1 C5 1.352(2) . ?
N2 C9 1.345(2) . ?
N2 N3 1.370(2) . ?
N3 C7 1.355(2) . ?
N3 C6 1.460(2) . ?
N4 N5 1.201(3) . ?
N5 N6 1.153(3) . ?
N7 N8 1.203(2) . ?
N7 Co1 2.1977(15) 5_575 ?
N8 N9 1.145(2) . ?
C1 C2 1.364(3) . ?
C2 C3 1.373(4) . ?
C3 C4 1.378(3) . ?
C4 C5 1.379(3) . ?
C5 C6 1.503(3) . ?
C7 C8 1.359(3) . ?
C7 C11 1.494(3) . ?
C8 C9 1.393(3) . ?
C9 C10 1.484(3) . ?
