#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:32:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179115 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/77/4307740.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_4307740
loop_
_publ_author_name
'Morsy A. M. Abu-Youssef'
'Franz A. Mautner'
'Ramon Vicente'
_publ_section_title
;
1D and 2D End-to-End Azide-Bridged Cobalt(II) Complexes: Syntheses,
Crystal Structures, and Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4654
_journal_page_last               4659
_journal_paper_doi               10.1021/ic0622297
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C10 H12 Co N8 O'
_chemical_formula_sum            'C10 H12 Co N8 O'
_chemical_formula_weight         319.21
_chemical_name_common            '[Co(C5H5N)2(N3)2(H2O)]n'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   10.642(3)
_cell_length_b                   16.477(5)
_cell_length_c                   29.817(8)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    99(2)
_cell_measurement_theta_max      15.5
_cell_measurement_theta_min      7.3
_cell_volume                     5228(3)
_computing_molecular_graphics    'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)'
_computing_publication_material  'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      99(2)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device       'mod. STOE 4-circle diffractometer'
_diffrn_measurement_method       ω-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            2103
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.82
_diffrn_standards_decay_%        3
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  '1 h'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.323
_exptl_absorpt_correction_T_max  0.768
_exptl_absorpt_correction_T_min  0.567
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   DIFABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.812
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.056
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1906
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0335P)²+15.6553P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1050
_refine_ls_wR_factor_ref         0.0910
_reflns_number_gt                1525
_reflns_number_total             1910
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0622297-file001_1.cif
_cod_data_source_block           cob03b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        5228.4(26)
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               4307740
#BEGIN Tags that were not found in dictionaries:
_refine_ls_restrained_s_ref      1.040
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'-x+1/4, -y+1/4, z'
'x, y+1/2, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'-x+1/4, -y+3/4, z+1/2'
'x+1/2, y, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'-x+3/4, -y+3/4, z'
'-x, -y, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'x-1/4, y-1/4, -z'
'-x, -y+1/2, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'x-1/4, y+1/4, -z+1/2'
'-x+1/2, -y, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, -y+1/2, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'
'x+1/4, y+1/4, -z'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Co1 Co 0.3750 0.3750 0.110832(13) 0.01520(12) Uani 1 d S .
N1 N 0.3750 0.3750 0.18316(9) 0.0234(5) Uani 1 d S .
C1 C 0.3986(3) 0.4426(2) 0.20660(8) 0.0329(6) Uani 1 d . .
H1 H 0.4143 0.4904 0.19101 0.040 Uiso 1 calc R .
C2 C 0.4005(3) 0.4445(2) 0.25285(8) 0.0396(7) Uani 1 d . .
H2 H 0.4190 0.4925 0.26784 0.047 Uiso 1 calc R .
C3 C 0.3750 0.3750 0.27660(12) 0.0363(8) Uani 1 d S .
H3 H 0.3750 0.3750 0.30779 0.044 Uiso 1 calc SR .
N2 N 0.3750 0.3750 0.03883(9) 0.0244(5) Uani 1 d S .
C4 C 0.2735(3) 0.35383(15) 0.01531(9) 0.0364(6) Uani 1 d . .
H4 H 0.2013 0.33884 0.03080 0.044 Uiso 1 calc R .
C5 C 0.2708(4) 0.3532(2) -0.03125(10) 0.0544(10) Uani 1 d . .
H5 H 0.1981 0.3379 -0.04637 0.065 Uiso 1 calc R .
C6 C 0.3750 0.3750 -0.05452(13) 0.066(2) Uani 1 d S .
H6 H 0.3750 0.3750 -0.08571 0.080 Uiso 1 calc SR .
N11 N 0.2266(2) 0.29070(12) 0.11069(7) 0.0261(4) Uani 1 d . .
N12 N 0.1250 0.29256(14) 0.1250 0.0160(4) Uani 1 d S .
N21 N 0.5009(2) 0.27579(10) 0.10983(6) 0.0227(4) Uani 0.50 d P 1
N22 N 0.4673(4) 0.2049(2) 0.11762(12) 0.0191(7) Uani 0.50 d P 1
N23 N 0.4349(4) 0.1393(2) 0.1226(3) 0.0261(11) Uani 0.50 d P 1
O1 O 0.5009(2) 0.27579(10) 0.10983(6) 0.0227(4) Uani 0.50 d P 2
H7 H 0.5722 0.2819 0.1194 0.027 Uiso 0.50 d P 2
H8 H 0.4783 0.2283 0.1106 0.027 Uiso 0.50 d P 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'
O O 0.0106 0.0060 '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
N11 Co1 N11 179.77(12) . 16 yes
N11 Co1 O1 88.00(8) . . ?
N11 Co1 O1 92.00(8) 16 . yes
N11 Co1 N21 88.00(8) . . ?
N11 Co1 N21 92.00(8) 16 . yes
O1 Co1 O1 178.38(11) . 16 yes
N11 Co1 N21 92.00(8) . 16 ?
N21 Co1 N21 178.38(11) . 16 yes
N11 Co1 N2 89.89(6) . . yes
O1 Co1 N2 89.19(5) . . ?
N21 Co1 N2 89.19(5) . . ?
O1 Co1 N2 89.19(5) 16 . ?
N21 Co1 N2 89.19(5) 16 . ?
N11 Co1 N1 90.11(6) 16 . ?
O1 Co1 N1 90.81(5) . . yes
O1 Co1 N1 90.81(5) 16 . ?
N2 Co1 N1 180.0 . . yes
C1 N1 C1 117.0(3) . 16 ?
C1 N1 Co1 121.49(14) . . ?
C1 N1 Co1 121.49(14) 16 . ?
N1 C1 C2 123.0(2) . . ?
N1 C1 H1 118.52 . . ?
C2 C1 H1 118.5 . . ?
C3 C2 C1 119.6(3) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C2 C3 C2 117.9(3) 16 . ?
C2 C3 H3 121.0 16 . ?
C2 C3 H3 121.0 . . ?
C4 N2 C4 116.6(3) 16 . ?
C4 N2 Co1 121.7(2) 16 . ?
C4 N2 Co1 121.7(2) . . ?
N2 C4 C5 123.0(3) . . ?
N2 C4 H4 118.5 . . ?
C5 C4 H4 118.5 . . ?
C6 C5 C4 119.5(3) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C5 C6 C5 118.5(4) . 16 ?
C5 C6 H6 120.7 . . ?
C5 C6 H6 120.7 16 . ?
N12 N11 Co1 132.8(2) . . yes
N11 N12 N11 177.0(3) . 3 yes
N22 N21 Co1 122.8(2) . . yes
N23 N22 N21 176.7(6) . . yes
H7 O1 H8 112.4 . . ?
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
Co1 N11 2.103(2) . yes
Co1 N11 2.103(2) 16 yes
Co1 O1 2.114(2) . yes
Co1 N21 2.114(2) . yes
Co1 O1 2.114(2) 16 yes
Co1 N21 2.114(2) 16 yes
Co1 N2 2.147(3) . yes
Co1 N1 2.157(3) . yes
N1 C1 1.338(3) . ?
N1 C1 1.338(3) 16 ?
C1 C2 1.379(3) . ?
C1 H1 0.93 . ?
C2 C3 1.374(3) . ?
C2 H2 0.93 . ?
C3 C2 1.374(3) 16 ?
C3 H3 0.93 . ?
N2 C4 1.334(3) 16 ?
N2 C4 1.334(3) . ?
C4 C5 1.389(4) . ?
C4 H4 0.93 . ?
C5 C6 1.357(5) . ?
C5 H5 0.93 . ?
C6 C5 1.357(5) 16 ?
C6 H6 0.93 . ?
N11 N12 1.163(2) . yes
N12 N11 1.163(2) 3 yes
N21 N22 1.243(4) . yes
N22 N23 1.146(5) . yes
O1 H7 0.818 . ?
O1 H8 0.819 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N11 Co1 N1 C1 -144.0(2) . . . . ?
N11 Co1 N1 C1 36.0(2) 16 . . . ?
O1 Co1 N1 C1 128.0(2) . . . . ?
O1 Co1 N1 C1 -52.0(2) 16 . . . ?
N21 Co1 N1 C1 128.0(2) 16 . . 16 ?
C1 N1 C1 C2 0.7(2) 16 . . . ?
N1 C1 C2 C3 -1.3(4) . . . . ?
C1 C2 C3 C2 0.6(2) . . . 16 ?
C4 N2 C4 C5 0.1(2) 16 . . . ?
N2 C4 C5 C6 -0.1(4) . . . . ?
C4 C5 C6 C5 0.1(2) . . . 16 ?
