#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/05/2240560.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2240560
loop_
_publ_author_name
'Laachir, Abdelhakim'
'Bentiss, Fouad'
'Guesmi, Salaheddine'
'Saadi, Mohamed'
'El Ammari, Lahcen'
_publ_section_title
;
 Crystal structure of
 bis(azido-κN)bis[2,5-bis(pyridin-2-yl)-1,3,4-thiadiazole-κ²N²,N³]cobalt(II)
;
_journal_coeditor_code           RZ5153
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              452
_journal_page_last               454
_journal_paper_doi               10.1107/S2056989015006544
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Co (N3)2 (C12 H8 N4 S)2]'
_chemical_formula_moiety         'C24 H16 Co N14 S2'
_chemical_formula_sum            'C24 H16 Co N14 S2'
_chemical_formula_weight         623.56
_chemical_name_systematic
Bis(azido-κN)bis[2,5-bis(pyridin-2-yl)-1,3,4-thiadiazole-κ²N²,N³]cobalt(II)
_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                 92.910(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.8004(3)
_cell_length_b                   8.2439(3)
_cell_length_c                   20.3222(8)
_cell_measurement_reflns_used    3667
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      2.61
_cell_volume                     1305.15(9)
_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT (Bruker, 2009)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            27415
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2009)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             634
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3667
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0346
_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)+(0.0381P)²+0.5683P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0884
_reflns_number_gt                2884
_reflns_number_total             3667
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            rz5153sup1.cf
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               2240560
_cod_database_fobs_code          2240560
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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
C C1 0.7907(3) 0.4986(3) 0.07266(12) 0.0486(5) Uani d . 1 1
H H1 0.8731 0.5035 0.0412 0.058 Uiso calc R 1 1
C C2 0.8166(3) 0.5770(3) 0.13200(13) 0.0540(6) Uani d . 1 1
H H2 0.9169 0.6353 0.1416 0.065 Uiso calc R 1 1
C C3 0.6910(3) 0.5672(3) 0.17662(13) 0.0568(6) Uani d . 1 1
H H3 0.7097 0.6203 0.2167 0.068 Uiso calc R 1 1
N N1 0.5445(2) 0.4873(2) 0.16646(9) 0.0448(4) Uani d . 1 1
C C5 0.5212(2) 0.4114(2) 0.10851(9) 0.0316(4) Uani d . 1 1
C C6 0.3585(2) 0.3225(2) 0.10077(8) 0.0298(4) Uani d . 1 1
C C7 0.0891(2) 0.1991(2) 0.11550(8) 0.0285(3) Uani d . 1 1
C C8 -0.0761(2) 0.1314(2) 0.13257(8) 0.0276(3) Uani d . 1 1
C C9 -0.1510(2) 0.1627(2) 0.19143(8) 0.0338(4) Uani d . 1 1
H H9 -0.0963 0.2283 0.2233 0.041 Uiso calc R 1 1
C C10 -0.3087(2) 0.0943(2) 0.20186(9) 0.0369(4) Uani d . 1 1
H H10 -0.3623 0.1133 0.2410 0.044 Uiso calc R 1 1
C C11 -0.3856(2) -0.0022(2) 0.15379(10) 0.0382(4) Uani d . 1 1
H H11 -0.4920 -0.0493 0.1599 0.046 Uiso calc R 1 1
C C12 -0.3022(2) -0.0285(2) 0.09601(9) 0.0348(4) Uani d . 1 1
H H12 -0.3547 -0.0941 0.0637 0.042 Uiso calc R 1 1
C C4 0.6406(2) 0.4123(2) 0.06039(10) 0.0383(4) Uani d . 1 1
H H4 0.6204 0.3565 0.0210 0.046 Uiso calc R 1 1
N N2 0.30958(18) 0.23430(19) 0.05046(7) 0.0314(3) Uani d . 1 1
N N3 0.15296(18) 0.16405(19) 0.05884(7) 0.0307(3) Uani d . 1 1
N N4 -0.14945(18) 0.03680(18) 0.08497(7) 0.0285(3) Uani d . 1 1
N N5 0.1294(2) -0.1959(2) 0.04761(8) 0.0425(4) Uani d . 1 1
N N6 0.1687(2) -0.1872(2) 0.10472(8) 0.0394(4) Uani d . 1 1
N N7 0.2046(3) -0.1805(3) 0.16093(9) 0.0650(6) Uani d . 1 1
S S1 0.21579(6) 0.32700(6) 0.16328(2) 0.03604(12) Uani d . 1 1
Co Co1 0.0000 0.0000 0.0000 0.02677(10) Uani d S 1 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'
S S 0.1246 0.1234 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
C2 C1 C4 . . 119.10(19)
C2 C1 H1 . . 120.5
C4 C1 H1 . . 120.5
C3 C2 C1 . . 118.31(19)
C3 C2 H2 . . 120.8
C1 C2 H2 . . 120.8
N1 C3 C2 . . 124.4(2)
N1 C3 H3 . . 117.8
C2 C3 H3 . . 117.8
C3 N1 C5 . . 116.54(18)
N1 C5 C4 . . 123.60(17)
N1 C5 C6 . . 113.95(15)
C4 C5 C6 . . 122.44(17)
N2 C6 C5 . . 125.69(15)
N2 C6 S1 . . 114.57(12)
C5 C6 S1 . . 119.72(13)
N3 C7 C8 . . 120.22(15)
N3 C7 S1 . . 113.57(13)
C8 C7 S1 . . 126.20(12)
N4 C8 C9 . . 123.13(16)
N4 C8 C7 . . 113.46(14)
C9 C8 C7 . . 123.40(16)
C10 C9 C8 . . 118.44(17)
C10 C9 H9 . . 120.8
C8 C9 H9 . . 120.8
C11 C10 C9 . . 119.22(16)
C11 C10 H10 . . 120.4
C9 C10 H10 . . 120.4
C10 C11 C12 . . 119.01(17)
C10 C11 H11 . . 120.5
C12 C11 H11 . . 120.5
N4 C12 C11 . . 122.64(17)
N4 C12 H12 . . 118.7
C11 C12 H12 . . 118.7
C1 C4 C5 . . 118.00(19)
C1 C4 H4 . . 121.0
C5 C4 H4 . . 121.0
C6 N2 N3 . . 111.59(13)
C7 N3 N2 . . 113.40(14)
C7 N3 Co1 . . 113.97(11)
N2 N3 Co1 . . 132.53(10)
C12 N4 C8 . . 117.54(15)
C12 N4 Co1 . . 126.96(12)
C8 N4 Co1 . . 115.44(11)
N6 N5 Co1 . . 119.66(14)
N7 N6 N5 . . 178.7(2)
C7 S1 C6 . . 86.85(8)
N5 Co1 N5 . 3 180.0
N5 Co1 N3 . 3 90.73(6)
N5 Co1 N3 3 3 89.27(6)
N5 Co1 N3 . . 89.27(6)
N5 Co1 N3 3 . 90.73(6)
N3 Co1 N3 3 . 180.0
N5 Co1 N4 . . 90.35(6)
N5 Co1 N4 3 . 89.65(6)
N3 Co1 N4 3 . 103.24(5)
N3 Co1 N4 . . 76.76(5)
N5 Co1 N4 . 3 89.65(6)
N5 Co1 N4 3 3 90.34(6)
N3 Co1 N4 3 3 76.76(5)
N3 Co1 N4 . 3 103.24(5)
N4 Co1 N4 . 3 180.0
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 C2 . 1.374(3)
C1 C4 . 1.382(3)
C1 H1 . 0.9300
C2 C3 . 1.371(3)
C2 H2 . 0.9300
C3 N1 . 1.326(3)
C3 H3 . 0.9300
N1 C5 . 1.338(2)
C5 C4 . 1.384(3)
C5 C6 . 1.467(2)
C6 N2 . 1.297(2)
C6 S1 . 1.7317(16)
C7 N3 . 1.310(2)
C7 C8 . 1.462(2)
C7 S1 . 1.7128(17)
C8 N4 . 1.347(2)
C8 C9 . 1.382(2)
C9 C10 . 1.380(3)
C9 H9 . 0.9300
C10 C11 . 1.374(3)
C10 H10 . 0.9300
C11 C12 . 1.388(3)
C11 H11 . 0.9300
C12 N4 . 1.337(2)
C12 H12 . 0.9300
C4 H4 . 0.9300
N2 N3 . 1.3704(19)
N3 Co1 . 2.1301(14)
N4 Co1 . 2.1535(14)
N5 N6 . 1.187(2)
N5 Co1 . 2.1132(17)
N6 N7 . 1.164(2)
Co1 N5 3 2.1132(17)
Co1 N3 3 2.1301(14)
Co1 N4 3 2.1535(14)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C2 H2 N6 1_665 0.93 2.59 3.432(3) 150.7
C11 H11 N7 1_455 0.93 2.60 3.528(3) 172.8
C10 H10 N1 2_545 0.93 2.63 3.438(2) 145.9
