#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:59:21 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180054 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/00/7050073.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_7050073
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            'C13 H12 Cu N8'
_chemical_formula_weight         343.85
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.01(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0150(4)
_cell_length_b                   6.3940(2)
_cell_length_c                   19.1148(8)
_cell_measurement_reflns_used    15733
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     1436.33(18)
_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 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.1247
_diffrn_reflns_av_sigmaI/netI    0.0794
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19983
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.42
_diffrn_reflns_theta_min         3.47
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.530
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.731
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       0.0017(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3215
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0467
_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)+(0.0534P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1128
_reflns_number_gt                2071
_reflns_number_total             3215
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b418239a.txt
_cod_data_source_block           3
_cod_original_cell_volume        1436.35(9)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7050073
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 0.05671(3) 0.22719(5) -0.00807(2) 0.03510(17) Uani 1 1 d . . .
N1 N 0.1192(2) 0.2459(3) 0.09799(14) 0.0361(6) Uani 1 1 d . . .
N2 N 0.2230(2) 0.2787(4) -0.00660(14) 0.0363(6) Uani 1 1 d . . .
N3 N -0.0973(2) 0.1562(4) 0.00837(14) 0.0421(6) Uani 1 1 d . . .
N4 N -0.1838(2) 0.1928(4) -0.03520(15) 0.0393(6) Uani 1 1 d . . .
N5 N -0.2689(3) 0.2194(5) -0.07467(18) 0.0559(8) Uani 1 1 d . . .
N6 N -0.0054(3) 0.2894(5) -0.10724(17) 0.0553(8) Uani 1 1 d . . .
N7 N 0.0260(2) 0.2613(4) -0.16124(17) 0.0457(7) Uani 1 1 d . . .
N8 N 0.0501(3) 0.2410(6) -0.2157(2) 0.0794(12) Uani 1 1 d . . .
C1 C 0.0601(3) 0.2367(5) 0.14955(19) 0.0448(8) Uani 1 1 d . . .
H1 H -0.0184 0.2194 0.1371 0.054 Uiso 1 1 calc R . .
C2 C 0.1120(4) 0.2520(5) 0.2211(2) 0.0511(9) Uani 1 1 d . . .
H2 H 0.0688 0.2471 0.2562 0.061 Uiso 1 1 calc R . .
C3 C 0.2270(4) 0.2743(5) 0.2395(2) 0.0548(10) Uani 1 1 d . . .
H3 H 0.2632 0.2840 0.2874 0.066 Uiso 1 1 calc R . .
C4 C 0.2897(3) 0.2825(5) 0.18673(19) 0.0487(9) Uani 1 1 d . . .
H4 H 0.3684 0.2963 0.1982 0.058 Uiso 1 1 calc R . .
C5 C 0.2323(3) 0.2698(4) 0.11676(18) 0.0381(7) Uani 1 1 d . . .
C6 C 0.2890(3) 0.2843(4) 0.05481(19) 0.0404(8) Uani 1 1 d . . .
C7 C 0.4152(3) 0.3081(6) 0.0690(2) 0.0608(10) Uani 1 1 d . . .
H7A H 0.4397 0.3187 0.0245 0.091 Uiso 1 1 calc R . .
H7B H 0.4503 0.1886 0.0951 0.091 Uiso 1 1 calc R . .
H7C H 0.4369 0.4323 0.0967 0.091 Uiso 1 1 calc R . .
C8 C 0.2691(3) 0.2964(5) -0.06974(18) 0.0386(7) Uani 1 1 d . . .
C9 C 0.2677(3) 0.4897(5) -0.10217(19) 0.0480(8) Uani 1 1 d . . .
H9 H 0.2384 0.6058 -0.0829 0.058 Uiso 1 1 calc R . .
C10 C 0.3102(3) 0.5081(6) -0.1634(2) 0.0554(9) Uani 1 1 d . . .
H10 H 0.3105 0.6380 -0.1852 0.066 Uiso 1 1 calc R . .
C11 C 0.3512(3) 0.3405(7) -0.1920(2) 0.0602(10) Uani 1 1 d . . .
H11 H 0.3790 0.3553 -0.2337 0.072 Uiso 1 1 calc R . .
C12 C 0.3526(3) 0.1464(6) -0.1603(2) 0.0640(11) Uani 1 1 d . . .
H12 H 0.3812 0.0310 -0.1804 0.077 Uiso 1 1 calc R . .
C13 C 0.3114(3) 0.1246(6) -0.0986(2) 0.0541(9) Uani 1 1 d . . .
H13 H 0.3123 -0.0054 -0.0767 0.065 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
N6 Cu1 N3 91.13(12) . . ?
N6 Cu1 N1 164.63(11) . . ?
N3 Cu1 N1 91.09(11) . . ?
N6 Cu1 N2 99.18(12) . . ?
N3 Cu1 N2 169.58(11) . . ?
N1 Cu1 N2 79.37(11) . . ?
C1 N1 C5 118.3(3) . . ?
C1 N1 Cu1 126.7(2) . . ?
C5 N1 Cu1 114.9(2) . . ?
C6 N2 C8 119.9(3) . . ?
C6 N2 Cu1 116.2(2) . . ?
C8 N2 Cu1 123.8(2) . . ?
N4 N3 Cu1 122.7(2) . . ?
N5 N4 N3 176.2(3) . . ?
N7 N6 Cu1 134.2(2) . . ?
N8 N7 N6 175.5(4) . . ?
N1 C1 C2 121.9(3) . . ?
C3 C2 C1 119.2(4) . . ?
C2 C3 C4 119.6(3) . . ?
C5 C4 C3 118.0(3) . . ?
N1 C5 C4 122.9(3) . . ?
N1 C5 C6 113.6(3) . . ?
C4 C5 C6 123.5(3) . . ?
N2 C6 C5 115.6(3) . . ?
N2 C6 C7 125.8(3) . . ?
C5 C6 C7 118.6(3) . . ?
C13 C8 C9 120.4(3) . . ?
C13 C8 N2 121.0(3) . . ?
C9 C8 N2 118.6(3) . . ?
C10 C9 C8 119.1(3) . . ?
C11 C10 C9 120.7(4) . . ?
C10 C11 C12 120.7(4) . . ?
C13 C12 C11 119.6(4) . . ?
C8 C13 C12 119.5(4) . . ?
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 N6 1.929(3) . ?
Cu1 N3 1.993(3) . ?
Cu1 N1 2.014(3) . ?
Cu1 N2 2.019(3) . ?
N1 C1 1.331(4) . ?
N1 C5 1.340(4) . ?
N2 C6 1.273(4) . ?
N2 C8 1.434(4) . ?
N3 N4 1.212(4) . ?
N4 N5 1.150(4) . ?
N6 N7 1.184(4) . ?
N7 N8 1.144(5) . ?
C1 C2 1.384(5) . ?
C2 C3 1.361(6) . ?
C3 C4 1.379(6) . ?
C4 C5 1.374(5) . ?
C5 C6 1.487(5) . ?
C6 C7 1.492(5) . ?
C8 C13 1.374(5) . ?
C8 C9 1.381(4) . ?
C9 C10 1.376(5) . ?
C10 C11 1.343(5) . ?
C11 C12 1.380(6) . ?
C12 C13 1.376(5) . ?
