#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:06:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179093 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/55/4305588.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_4305588
loop_
_publ_author_name
'Ru-Yin Li'
'Xin-Yi Wang'
'Tao Liu'
'Hong-Bin Xu'
'Fei Zhao'
'Zhe-Ming Wang'
'Song Gao'
_publ_section_title
;
Synthesis, Structure, and Magnetism of Three Azido-Bridged Co2+ Compounds
with a Flexible Coligand 1,2-(Tetrazole-1-yl)ethane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8134
_journal_page_last               8142
_journal_paper_doi               10.1021/ic800570a
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C8 H12 Co N22'
_chemical_formula_weight         475.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 101.1850(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.1781(2)
_cell_length_b                   6.2444(2)
_cell_length_c                   9.8825(5)
_cell_measurement_reflns_used    9508
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     918.85(6)
_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 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0567
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16061
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.54
_exptl_absorpt_coefficient_mu    0.988
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       piece
_exptl_crystal_F_000             482
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2105
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0434
_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)+(0.0764P)²+0.2361P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1293
_reflns_number_gt                1527
_reflns_number_total             2105
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800570a-file002_2.cif
_cod_data_source_block           2-Co
_cod_database_code               4305588
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'
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 0.0000 0.0000 0.0000 0.0246(2) Uani 1 2 d S . .
N2 N 0.05405(15) -0.2803(4) -0.2347(2) 0.0261(5) Uani 1 1 d . . .
N7 N 0.20362(16) 0.4460(4) -0.0381(3) 0.0292(5) Uani 1 1 d . . .
N5 N 0.16360(17) 0.1454(4) -0.1303(3) 0.0377(6) Uani 1 1 d . . .
N4 N 0.11231(15) 0.1848(4) -0.0328(2) 0.0291(5) Uani 1 1 d . . .
N8 N 0.37859(16) 0.4919(4) 0.1480(3) 0.0306(6) Uani 1 1 d . . .
N1 N 0.02714(17) -0.2414(4) -0.1349(3) 0.0373(6) Uani 1 1 d . . .
N6 N 0.21861(17) 0.3025(4) -0.1334(3) 0.0394(6) Uani 1 1 d . . .
C1 C 0.13907(19) 0.3711(5) 0.0216(3) 0.0314(7) Uani 1 1 d . . .
H1 H 0.1163 0.4395 0.0911 0.038 Uiso 1 1 calc R . .
C3 C 0.35296(19) 0.6123(5) 0.0202(3) 0.0348(7) Uani 1 1 d . . .
H3A H 0.3722 0.5349 -0.0540 0.042 Uiso 1 1 calc R . .
H3B H 0.3834 0.7497 0.0299 0.042 Uiso 1 1 calc R . .
N11 N 0.4067(2) 0.4381(5) 0.3629(3) 0.0481(7) Uani 1 1 d . . .
C4 C 0.3734(2) 0.5735(5) 0.2704(3) 0.0300(6) Uani 1 1 d . . .
H4 H 0.3496 0.7064 0.2859 0.036 Uiso 1 1 calc R . .
N10 N 0.4347(2) 0.2612(5) 0.3038(3) 0.0513(8) Uani 1 1 d . . .
C2 C 0.2527(2) 0.6486(5) -0.0168(3) 0.0360(7) Uani 1 1 d . . .
H2A H 0.2334 0.7280 0.0567 0.043 Uiso 1 1 calc R . .
H2B H 0.2387 0.7338 -0.1003 0.043 Uiso 1 1 calc R . .
N9 N 0.4168(2) 0.3003(6) 0.1698(4) 0.0644(9) Uani 1 1 d . . .
N3 N 0.08272(17) -0.3271(4) -0.3329(2) 0.0351(6) Uani 1 1 d . . .
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
N1 Co1 N1 180.00(14) 3 . ?
N1 Co1 N4 91.77(9) 3 3 ?
N1 Co1 N4 88.23(9) . 3 ?
N1 Co1 N4 88.23(9) 3 . ?
N1 Co1 N4 91.77(9) . . ?
N4 Co1 N4 180.00(16) 3 . ?
N1 Co1 N3 88.29(10) 3 2_554 ?
N1 Co1 N3 91.71(10) . 2_554 ?
N4 Co1 N3 91.34(9) 3 2_554 ?
N4 Co1 N3 88.66(9) . 2_554 ?
N1 Co1 N3 91.71(10) 3 4_556 ?
N1 Co1 N3 88.29(10) . 4_556 ?
N4 Co1 N3 88.66(9) 3 4_556 ?
N4 Co1 N3 91.34(9) . 4_556 ?
N3 Co1 N3 180.00(17) 2_554 4_556 ?
N1 N2 N3 177.3(3) . . ?
C1 N7 N6 108.4(2) . . ?
C1 N7 C2 129.9(3) . . ?
N6 N7 C2 121.6(2) . . ?
N6 N5 N4 109.7(2) . . ?
C1 N4 N5 105.9(2) . . ?
C1 N4 Co1 127.58(19) . . ?
N5 N4 Co1 125.97(18) . . ?
N9 N8 C4 107.4(3) . . ?
N9 N8 C3 129.8(3) . . ?
C4 N8 C3 122.6(3) . . ?
N2 N1 Co1 146.1(2) . . ?
N5 N6 N7 106.9(2) . . ?
N4 C1 N7 109.1(3) . . ?
N4 C1 H1 125.4 . . ?
N7 C1 H1 125.4 . . ?
N8 C3 C2 112.0(2) . . ?
N8 C3 H3A 109.2 . . ?
C2 C3 H3A 109.2 . . ?
N8 C3 H3B 109.2 . . ?
C2 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C4 N11 N10 110.2(3) . . ?
N11 C4 N8 108.2(3) . . ?
N11 C4 H4 125.9 . . ?
N8 C4 H4 125.9 . . ?
N9 N10 N11 105.1(3) . . ?
N7 C2 C3 111.4(2) . . ?
N7 C2 H2A 109.3 . . ?
C3 C2 H2A 109.3 . . ?
N7 C2 H2B 109.3 . . ?
C3 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
N10 N9 N8 109.1(3) . . ?
N2 N3 Co1 120.2(2) . 2_544 ?
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 N1 2.105(2) 3 ?
Co1 N1 2.105(2) . ?
Co1 N4 2.135(2) 3 ?
Co1 N4 2.135(2) . ?
Co1 N3 2.160(2) 2_554 ?
Co1 N3 2.160(2) 4_556 ?
N2 N1 1.164(3) . ?
N2 N3 1.174(3) . ?
N7 C1 1.323(3) . ?
N7 N6 1.351(4) . ?
N7 C2 1.462(4) . ?
N5 N6 1.293(3) . ?
N5 N4 1.374(3) . ?
N4 C1 1.312(4) . ?
N8 N9 1.329(4) . ?
N8 C4 1.329(4) . ?
N8 C3 1.456(4) . ?
C1 H1 0.9300 . ?
C3 C2 1.512(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
N11 C4 1.276(4) . ?
N11 N10 1.356(4) . ?
C4 H4 0.9300 . ?
N10 N9 1.322(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
N3 Co1 2.160(2) 2_544 ?
