#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/29/2202985.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_2202985
loop_
_publ_author_name
'Zhao, Qihua'
'Wang, Xiaofeng'
'Fang, Ruibin'
'Tiekink, Edward R. T.'
_publ_section_title
;
 Diazidobis(1,10-phenathroline)cobalt(III) nitrate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m690
_journal_page_last               m691
_journal_paper_doi               10.1107/S1600536803016489
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Co (C12 H8 N2)2 (N3)2] N O3'
_chemical_formula_moiety         'C24 H16 Co N10 1+, N O3 1-'
_chemical_formula_sum            'C24 H16 Co N11 O3'
_chemical_formula_weight         565.41
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           45
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 -2c'
_symmetry_space_group_name_H-M   'I b a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4858(6)
_cell_length_b                   9.7359(4)
_cell_length_c                   14.7769(8)
_cell_measurement_reflns_used    3743
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      29.0
_cell_measurement_theta_min      2.5
_cell_volume                     2227.89(17)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SHELXTL (Bruker, 2000)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'PATTY in DIRDIF92 (Beurskens et al., 1992)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker AXS SMART CCD'
_diffrn_measurement_method       ω
_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  0.037
_diffrn_reflns_av_sigmaI/netI    0.040
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8877
_diffrn_reflns_theta_full        30.0
_diffrn_reflns_theta_max         30.0
_diffrn_reflns_theta_min         2.5
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 2000; Blessing, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.56
_refine_diff_density_min         -0.25
_refine_ls_abs_structure_details 'Flack (1983), 0000 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.033(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.00
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3200
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.00
_refine_ls_R_factor_all          0.038
_refine_ls_R_factor_gt           0.033
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0514P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.080
_refine_ls_wR_factor_ref         0.082
_reflns_number_gt                2868
_reflns_number_total             3200
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ww6100.cif
_cod_data_source_block           I
_cod_database_code               2202985
_cod_database_fobs_code          2202985
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, z+1/2'
'x, -y, z+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1'
'x+1/2, -y+1/2, z+1'
loop_
_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_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Co 0.0000 0.0000 -0.00392(3) 0.01734(8) Uani d S 1 . . Co
O1 -0.5000 0.0000 -0.5083(3) 0.0612(8) Uani d S 1 . . O
O2 -0.56843(13) -0.0141(2) -0.38222(17) 0.0564(6) Uani d . 1 . . O
N1 -0.03337(12) -0.13482(19) 0.08542(13) 0.0275(4) Uani d . 1 . . N
N2 -0.08184(10) -0.10418(18) 0.14527(10) 0.0254(3) Uani d . 1 . . N
N3 -0.12953(15) -0.0837(2) 0.20354(14) 0.0444(5) Uani d . 1 . . N
N4 0.11657(8) -0.07178(13) -0.00368(13) 0.0200(3) Uani d . 1 . . N
N5 0.04371(10) 0.12165(17) -0.09839(10) 0.0203(3) Uani d . 1 . . N
N6 -0.5000 0.0000 -0.4248(2) 0.0349(6) Uani d S 1 . . N
C1 0.14995(12) -0.1709(2) 0.04744(13) 0.0258(4) Uani d . 1 . . C
H1 0.1131 -0.2253 0.0831 0.031 Uiso calc R 1 . . H
C2 0.23908(13) -0.1956(2) 0.04898(14) 0.0292(4) Uani d . 1 . . C
H2 0.2614 -0.2648 0.0866 0.035 Uiso calc R 1 . . H
C3 0.29422(10) -0.11938(19) -0.00410(16) 0.0275(3) Uani d . 1 . . C
H3 0.3541 -0.1348 -0.0022 0.033 Uiso calc R 1 . . H
C4 0.25943(12) -0.01814(19) -0.06115(16) 0.0245(4) Uani d . 1 . . C
C5 0.17009(12) 0.00255(17) -0.05818(14) 0.0205(3) Uani d . 1 . . C
C6 0.13025(11) 0.10457(18) -0.11180(12) 0.0207(3) Uani d . 1 . . C
C7 0.17810(12) 0.1817(2) -0.17410(13) 0.0244(4) Uani d . 1 . . C
C8 0.13255(13) 0.2782(2) -0.22603(13) 0.0278(4) Uani d . 1 . . C
H8 0.1616 0.3322 -0.2691 0.033 Uiso calc R 1 . . H
C9 0.04523(14) 0.2931(2) -0.21343(14) 0.0288(4) Uani d . 1 . . C
H9 0.0140 0.3563 -0.2486 0.035 Uiso calc R 1 . . H
C10 0.00285(11) 0.2142(2) -0.14820(15) 0.0246(4) Uani d . 1 . . C
H10 -0.0567 0.2271 -0.1394 0.030 Uiso calc R 1 . . H
C11 0.30841(12) 0.0648(2) -0.12395(16) 0.0309(4) Uani d . 1 . . C
H11 0.3687 0.0541 -0.1270 0.037 Uiso calc R 1 . . H
C12 0.26935(14) 0.1572(2) -0.17825(15) 0.0317(4) Uani d . 1 . . C
H12 0.3029 0.2070 -0.2200 0.038 Uiso calc R 1 . . H
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'
Co Co 0.3494 0.9721 '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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Co N4 . . 90.16(7) y
N1 Co N5 . . 173.57(8) y
N1 Co N1 . 2 93.80(12) y
N1 Co N4 . 2 89.69(7) y
N1 Co N5 . 2 89.06(6) y
N4 Co N5 . . 84.09(7) y
N4 Co N4 . 2 179.79(12) y
N4 Co N5 . 2 96.06(7) y
N5 Co N5 . 2 88.68(9) y
N1 Co N4 2 . 89.69(7) ?
N1 Co N4 2 2 90.16(7) ?
N1 Co N5 2 2 173.57(8) ?
N4 Co N5 2 2 84.09(7) ?
N1 Co N5 2 . 89.06(6) ?
N4 Co N5 2 . 96.06(7) ?
Co N1 N2 . . 120.19(15) y
N1 N2 N3 . . 175.6(2) y
C1 N4 C5 . . 118.97(15) ?
C1 N4 Co . . 128.71(13) ?
C5 N4 Co . . 111.97(12) ?
C10 N5 C6 . . 118.12(16) ?
C10 N5 Co . . 130.13(13) ?
C6 N5 Co . . 111.74(12) ?
O1 N6 O2 . 2_455 120.48(18) ?
O1 N6 O2 . . 120.48(18) ?
O2 N6 O2 2_455 . 119.0(4) ?
N4 C1 C2 . . 121.08(18) ?
N4 C1 H1 . . 119.5 ?
C2 C1 H1 . . 119.5 ?
C3 C2 C1 . . 120.64(19) ?
C3 C2 H2 . . 119.7 ?
C1 C2 H2 . . 119.7 ?
C2 C3 C4 . . 118.83(16) ?
C2 C3 H3 . . 120.6 ?
C4 C3 H3 . . 120.6 ?
C5 C4 C3 . . 117.49(18) ?
C5 C4 C11 . . 117.30(19) ?
C3 C4 C11 . . 125.19(18) ?
N4 C5 C4 . . 122.90(18) ?
N4 C5 C6 . . 116.05(16) ?
C4 C5 C6 . . 121.05(18) ?
N5 C6 C7 . . 123.36(17) ?
N5 C6 C5 . . 115.67(16) ?
C7 C6 C5 . . 120.98(16) ?
C6 C7 C8 . . 116.90(17) ?
C6 C7 C12 . . 117.42(18) ?
C8 C7 C12 . . 125.67(18) ?
C9 C8 C7 . . 119.47(18) ?
C9 C8 H8 . . 120.3 ?
C7 C8 H8 . . 120.3 ?
C8 C9 C10 . . 119.89(18) ?
C8 C9 H9 . . 120.1 ?
C10 C9 H9 . . 120.1 ?
N5 C10 C9 . . 122.23(17) ?
N5 C10 H10 . . 118.9 ?
C9 C10 H10 . . 118.9 ?
C12 C11 C4 . . 121.30(17) ?
C12 C11 H11 . . 119.4 ?
C4 C11 H11 . . 119.4 ?
C11 C12 C7 . . 121.81(18) ?
C11 C12 H12 . . 119.1 ?
C7 C12 H12 . . 119.1 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Co N1 2 1.9320(18) ?
Co N1 . 1.9320(18) y
Co N4 2 1.9358(12) ?
Co N4 . 1.9358(12) y
Co N5 2 1.9518(16) ?
Co N5 . 1.9518(16) y
O1 N6 . 1.233(6) y
O2 N6 . 1.240(3) y
N1 N2 . 1.198(2) y
N2 N3 . 1.152(2) y
N4 C1 . 1.330(2) ?
N4 C5 . 1.364(2) ?
N5 C10 . 1.324(3) ?
N5 C6 . 1.365(2) ?
N6 O2 2_455 1.240(3) ?
C1 C2 . 1.401(3) ?
C1 H1 . 0.9400 ?
C2 C3 . 1.376(3) ?
C2 H2 . 0.9400 ?
C3 C4 . 1.404(3) ?
C3 H3 . 0.9400 ?
C4 C5 . 1.399(3) ?
C4 C11 . 1.445(3) ?
C5 C6 . 1.412(3) ?
C6 C7 . 1.400(3) ?
C7 C8 . 1.403(3) ?
C7 C12 . 1.434(3) ?
C8 C9 . 1.373(3) ?
C8 H8 . 0.9400 ?
C9 C10 . 1.397(3) ?
C9 H9 . 0.9400 ?
C10 H10 . 0.9400 ?
C11 C12 . 1.349(3) ?
C11 H11 . 0.9400 ?
C12 H12 . 0.9400 ?
