#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:14:31 +0100 (vie 25 de mar de 2016) $
#$Revision: 180067 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/13/7051371.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_7051371
loop_
_publ_author_name
'Sun, Bai-Wang'
'Gao, Song'
'Ma, Bao-Qing'
'Wang, Zhe-Ming'
_publ_section_title
;
 A two-fold interpenetrated three-dimensional cobalt(II) complex with
 dual dicyanamide and 4,4'-bipyridine bridges
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              953
_journal_paper_doi               10.1039/b006602h
_journal_volume                  24
_journal_year                    2000
_chemical_formula_sum            'C14 H8 Co N8'
_chemical_formula_weight         347.21
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthogonal
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.9221(7)
_cell_length_b                   11.4251(4)
_cell_length_c                   8.6147(3)
_cell_measurement_reflns_used    22052
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.87
_cell_measurement_theta_min      3.57
_cell_volume                     1665.54(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, 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'
_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  0.0865
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            22052
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         3.57
_exptl_absorpt_coefficient_mu    1.041
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.843
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.509
_refine_diff_density_min         -1.598
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       0.0042(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2075
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0772
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0840P)²+14.2933P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2543
_refine_ls_wR_factor_ref         0.2644
_reflns_number_gt                1632
_reflns_number_total             2075
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b006602h.txt
_cod_data_source_block           Co(4,4'-bpy)(N(CN)2)2
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7051371
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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 0.13830(7) 0.2500 0.17637(13) 0.0272(4) Uani 1 2 d S . .
N1 N 0.0134(5) 0.2500 0.2179(12) 0.054(3) Uani 1 2 d S . .
N21 N -0.097(2) 0.221(2) 0.386(4) 0.043(11) Uani 0.25 1 d P . .
N22 N -0.104(2) 0.167(3) 0.350(6) 0.068(14) Uani 0.25 1 d P . .
N3 N -0.2376(5) 0.2500 0.3492(12) 0.049(2) Uani 1 2 d S . .
N4 N 0.1215(6) 0.2500 -0.0667(10) 0.046(2) Uani 1 2 d S . .
N51 N 0.079(2) 0.218(3) -0.333(5) 0.057(15) Uani 0.25 1 d P . .
N52 N 0.110(4) 0.165(4) -0.326(4) 0.10(2) Uani 0.25 1 d P . .
N6 N 0.1504(7) 0.2500 -0.5784(11) 0.057(3) Uani 1 2 d S . .
N7 N 0.1384(4) 0.0611(5) 0.1763(7) 0.0409(13) Uani 1 1 d . . .
C1 C -0.0405(8) 0.2500 0.2809(18) 0.086(5) Uani 1 2 d S . .
C2 C -0.1732(8) 0.2500 0.3476(17) 0.085(6) Uani 1 2 d S . .
C3 C 0.1113(9) 0.2500 -0.1902(15) 0.090(6) Uani 1 2 d S . .
C4 C 0.1242(10) 0.2500 -0.4581(15) 0.096(6) Uani 1 2 d S . .
C5 C 0.1359(5) -0.1842(7) 0.1752(9) 0.0463(17) Uani 1 1 d . . .
C6 C 0.0832(10) -0.1224(12) 0.104(2) 0.055(4) Uani 0.530(11) 1 d P A 1
H6 H 0.0426 -0.1609 0.0517 0.066 Uiso 0.530(11) 1 calc PR A 1
C7 C 0.0848(10) -0.0013(13) 0.101(2) 0.056(4) Uani 0.530(11) 1 d P A 1
H7 H 0.0465 0.0380 0.0437 0.068 Uiso 0.530(11) 1 calc PR A 1
C8 C 0.1892(9) 0.0001(12) 0.265(2) 0.051(4) Uani 0.530(11) 1 d P A 1
H8 H 0.2266 0.0414 0.3221 0.061 Uiso 0.530(11) 1 calc PR A 1
C9 C 0.1889(9) -0.1225(12) 0.277(2) 0.050(4) Uani 0.530(11) 1 d P A 1
H9 H 0.2213 -0.1617 0.3467 0.060 Uiso 0.530(11) 1 calc PR A 1
C10 C 0.0927(15) -0.1197(17) 0.264(2) 0.075(7) Uani 0.470(11) 1 d P A 2
H10 H 0.0560 -0.1572 0.3275 0.090 Uiso 0.470(11) 1 calc PR A 2
C11 C 0.0969(14) -0.0012(14) 0.272(2) 0.062(6) Uani 0.470(11) 1 d P A 2
H11 H 0.0690 0.0370 0.3504 0.074 Uiso 0.470(11) 1 calc PR A 2
C12 C 0.1774(12) 0.0009(14) 0.065(2) 0.056(5) Uani 0.470(11) 1 d P A 2
H12 H 0.2052 0.0435 -0.0092 0.067 Uiso 0.470(11) 1 calc PR A 2
C13 C 0.1785(13) -0.1190(14) 0.054(2) 0.058(5) Uani 0.470(11) 1 d P A 2
H13 H 0.2050 -0.1571 -0.0261 0.069 Uiso 0.470(11) 1 calc PR A 2
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 N3 91.8(4) . 6_656 y
N4 Co1 N6 177.8(4) . 1_556 y
N3 Co1 N6 90.4(4) 6_656 1_556 y
N4 Co1 N1 91.9(4) . . y
N3 Co1 N1 176.4(4) 6_656 . y
N6 Co1 N1 85.9(4) 1_556 . y
N4 Co1 N7 89.98(17) . . y
N3 Co1 N7 89.97(17) 6_656 . y
N6 Co1 N7 90.02(17) 1_556 . y
N1 Co1 N7 90.04(17) . . y
N4 Co1 N7 89.98(17) . 7_565 y
N3 Co1 N7 89.97(17) 6_656 7_565 y
N6 Co1 N7 90.02(17) 1_556 7_565 y
N1 Co1 N7 90.04(17) . 7_565 y
N7 Co1 N7 179.9(4) . 7_565 y
C1 N1 Co1 158.9(12) . . y
N21 N21 N22 152(6) 7_565 . y
N21 N21 N22 15(3) 7_565 7_565 y
N22 N21 N22 137(9) . 7_565 ?
N21 N21 C1 76.0(11) 7_565 . ?
N22 N21 C1 92(6) . . ?
N22 N21 C1 71(3) 7_565 . ?
N21 N21 C2 76.2(10) 7_565 . ?
N22 N21 C2 86(5) . . ?
N22 N21 C2 68(3) 7_565 . ?
C1 N21 C2 116(3) . . ?
N21 N22 N21 14(3) . 7_565 ?
N21 N22 C2 66(5) . . ?
N21 N22 C2 58(3) 7_565 . ?
N21 N22 C1 61(4) . . ?
N21 N22 C1 56(2) 7_565 . ?
C2 N22 C1 99(2) . . ?
N21 N22 N22 28(6) . 7_565 ?
N21 N22 N22 15(3) 7_565 7_565 ?
C2 N22 N22 50.9(13) . 7_565 ?
C1 N22 N22 52.4(15) . 7_565 ?
C2 N3 Co1 173.3(12) . 6_556 y
C3 N4 Co1 178.6(12) . . y
N51 N51 N52 139(6) 7_565 . ?
N51 N51 C4 74.7(14) 7_565 . ?
N52 N51 C4 84(6) . . ?
N51 N51 C3 74.9(14) 7_565 . ?
N52 N51 C3 83(5) . . ?
C4 N51 C3 114(2) . . ?
N51 N51 N52 22(3) 7_565 7_565 ?
N52 N51 N52 117(9) . 7_565 ?
C4 N51 N52 65(3) . 7_565 ?
C3 N51 N52 65(3) . 7_565 ?
N51 N52 N51 19(3) . 7_565 ?
N51 N52 C4 64(5) . . ?
N51 N52 C4 55(3) 7_565 . ?
N51 N52 C3 65(4) . . ?
N51 N52 C3 56(3) 7_565 . ?
C4 N52 C3 99(3) . . ?
C4 N6 Co1 151.3(12) . 1_554 y
C11 N7 C7 69.4(13) . . ?
C11 N7 C8 72.4(13) . . ?
C7 N7 C8 116.0(10) . . ?
C11 N7 C12 116.0(11) . . ?
C7 N7 C12 73.3(12) . . ?
C8 N7 C12 80.1(12) . . ?
C11 N7 Co1 123.2(9) . . y
C7 N7 Co1 122.6(8) . . y
C8 N7 Co1 121.2(7) . . y
C12 N7 Co1 120.6(7) . . y
N1 C1 N21 161.2(16) . . ?
N1 C1 N21 161.2(16) . 7_565 ?
N21 C1 N21 28(2) . 7_565 ?
N1 C1 N22 142.4(15) . 7_565 ?
N21 C1 N22 53(2) . 7_565 ?
N21 C1 N22 27(2) 7_565 7_565 ?
N1 C1 N22 142.4(15) . . ?
N21 C1 N22 27(2) . . ?
N21 C1 N22 53(2) 7_565 . ?
N22 C1 N22 75(3) 7_565 . ?
N3 C2 N21 159.7(17) . 7_565 ?
N3 C2 N21 159.7(17) . . ?
N21 C2 N21 28(2) 7_565 . ?
N3 C2 N22 140.9(12) . 7_565 ?
N21 C2 N22 27.9(18) 7_565 7_565 ?
N21 C2 N22 54(2) . 7_565 ?
N3 C2 N22 140.9(12) . . ?
N21 C2 N22 54(2) 7_565 . ?
N21 C2 N22 27.9(18) . . ?
N22 C2 N22 78(3) 7_565 . ?
N4 C3 N51 159.1(19) . . ?
N4 C3 N51 159.1(19) . 7_565 ?
N51 C3 N51 30(3) . 7_565 ?
N4 C3 N52 139.4(17) . . ?
N51 C3 N52 32(2) . . ?
N51 C3 N52 59(3) 7_565 . ?
N4 C3 N52 139.4(17) . 7_565 ?
N51 C3 N52 59(3) . 7_565 ?
N51 C3 N52 32(2) 7_565 7_565 ?
N52 C3 N52 80(3) . 7_565 ?
N6 C4 N51 160.6(15) . . ?
N6 C4 N51 160.6(15) . 7_565 ?
N51 C4 N51 31(3) . 7_565 ?
N6 C4 N52 138.7(19) . 7_565 ?
N51 C4 N52 59(3) . 7_565 ?
N51 C4 N52 32(3) 7_565 7_565 ?
N6 C4 N52 138.7(19) . . ?
N51 C4 N52 32(3) . . ?
N51 C4 N52 59(3) 7_565 . ?
N52 C4 N52 80(3) 7_565 . ?
C10 C5 C6 65.3(14) . . ?
C10 C5 C9 73.2(14) . . ?
C6 C5 C9 116.9(10) . . ?
C10 C5 C13 114.3(12) . . ?
C6 C5 C13 73.9(12) . . ?
C9 C5 C13 83.0(11) . . ?
C10 C5 C5 124.8(9) . 7 ?
C6 C5 C5 123.1(7) . 7 ?
C9 C5 C5 119.4(6) . 7 ?
C13 C5 C5 120.4(7) . 7 ?
C5 C6 C7 122.6(14) . . ?
N7 C7 C6 122.9(14) . . ?
N7 C8 C9 123.7(13) . . ?
C8 C9 C5 116.6(12) . . ?
C5 C10 C11 124.7(16) . . ?
N7 C11 C10 122.9(16) . . ?
N7 C12 C13 124.2(14) . . ?
C12 C13 C5 116.7(14) . . ?
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 2.113(9) . y
Co1 N3 2.112(9) 6_656 y
Co1 N6 2.122(9) 1_556 y
Co1 N1 2.143(9) . y
Co1 N7 2.158(6) . y
Co1 N7 2.158(6) 7_565 y
N1 C1 1.062(15) . y
N21 N21 0.65(5) 7_565 y
N21 N22 0.70(4) . y
N21 N22 1.32(5) 7_565 ?
N21 C1 1.36(4) . ?
N21 C2 1.37(4) . ?
N22 N21 1.32(5) 7_565 ?
N22 C2 1.50(4) . ?
N22 C1 1.55(3) . ?
N22 N22 1.90(7) 7_565 ?
N3 C2 1.090(16) . ?
N3 Co1 2.112(9) 6_556 y
N4 C3 1.078(15) . ?
N51 N51 0.72(6) 7_565 ?
N51 N52 0.81(6) . ?
N51 C4 1.37(5) . ?
N51 C3 1.39(4) . ?
N51 N52 1.44(7) 7_565 ?
N52 N51 1.44(7) 7_565 ?
N52 C4 1.52(4) . ?
N52 C3 1.52(4) . ?
N6 C4 1.128(17) . ?
N6 Co1 2.122(9) 1_554 y
N7 C11 1.298(17) . ?
N7 C7 1.323(16) . ?
N7 C8 1.346(15) . ?
N7 C12 1.353(17) . ?
C1 N21 1.36(4) 7_565 ?
C1 N22 1.55(3) 7_565 ?
C2 N21 1.37(4) 7_565 ?
C2 N22 1.50(4) 7_565 ?
C3 N51 1.39(4) 7_565 ?
C3 N52 1.52(4) 7_565 ?
C4 N51 1.37(5) 7_565 ?
C4 N52 1.52(4) 7_565 ?
C5 C10 1.29(2) . ?
C5 C6 1.295(16) . ?
C5 C9 1.438(16) . ?
C5 C13 1.472(18) . ?
C5 C5 1.503(15) 7 ?
C6 C7 1.38(2) . ?
C8 C9 1.404(19) . ?
C10 C11 1.36(3) . ?
C12 C13 1.37(2) . ?
