##############################################################################
###                                                                        ###
###        Electronic paper (Acta Crystallographica Section E)             ###
###                                                                        ###
##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section E. It conforms to the requirements of Notes      #
# for Authors for Section E, and has been peer reviewed under the auspices   #
# of the IUCr Commission on Journals.                                        #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
# cif/home.html                                                              #
#                                                                            #
#            Copyright International Union of Crystallography                #
#                                                                            #
##############################################################################
                                             
data_I
_audit_creation_method     SHELXL-97
_chemical_name_systematic
;
(aqua)bis(dimethylglyoxime)cobalt(III) azide hydrate
;
_chemical_formula_moiety     'C8 H16 Co N7 O5, H2 O'
_chemical_formula_sum     'C8 H18 Co N7 O6'
_chemical_formula_iupac
                           '[Co (N3) (H2 O1) (C2 H6 N2 O2) (C2 H8 N2 O2)], H2 O'
_chemical_formula_weight     367.22
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'P 21/n'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x+1/2, y+1/2, -z+1/2'
    '-x, -y, -z'
    'x-1/2, -y-1/2, z-1/2'
_cell_length_a     7.6739(18)
_cell_length_b     17.515(4)
_cell_length_c     11.261(2)
_cell_angle_alpha     90.00
_cell_angle_beta     91.243(14)
_cell_angle_gamma     90.00
_cell_volume     1513.2(6)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     31
_cell_measurement_theta_min     5.0
_cell_measurement_theta_max     12.6
_cell_measurement_temperature     293(2)
_exptl_crystal_description     plate
_exptl_crystal_colour     brown
_exptl_crystal_size_max     0.4
_exptl_crystal_size_mid     0.2
_exptl_crystal_size_min     0.04
_exptl_crystal_density_diffrn     1.612
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     760
_exptl_absorpt_coefficient_mu     1.175
_exptl_absorpt_correction_type     '\y scan'
_exptl_absorpt_process_details     '(North et al., 1968)'
_exptl_absorpt_correction_T_min     0.225
_exptl_absorpt_correction_T_max     0.269
_diffrn_ambient_temperature     293(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Bruker P4'
_diffrn_measurement_method     ω
_diffrn_reflns_number     3523
_diffrn_reflns_av_R_equivalents     0.0377
_diffrn_reflns_av_sigmaI/netI     0.0518
_diffrn_reflns_theta_min     2.15
_diffrn_reflns_theta_max     25.00
_diffrn_reflns_theta_full     25.00
_diffrn_measured_fraction_theta_max     0.988
_diffrn_measured_fraction_theta_full     0.988
_diffrn_reflns_limit_h_min     -9
_diffrn_reflns_limit_h_max     1
_diffrn_reflns_limit_k_min     -1
_diffrn_reflns_limit_k_max     20
_diffrn_reflns_limit_l_min     -13
_diffrn_reflns_limit_l_max     13
_diffrn_standards_number     3
_diffrn_standards_interval_count     100
_diffrn_standards_decay_%     0
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_reflns_number_total     2635
_reflns_number_gt     1853
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0654
_refine_ls_R_factor_gt     0.0417
_refine_ls_wR_factor_gt     0.0867
_refine_ls_wR_factor_ref     0.1002
_refine_ls_goodness_of_fit_ref     1.018
_refine_ls_restrained_S_all     1.018
_refine_ls_number_reflns     2635
_refine_ls_number_parameters     200
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
           'calc w = 1/[σ²(Fo²)+(0.001P)²+2P] where P = (Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.004
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.299
_refine_diff_density_min     -0.260
_refine_ls_extinction_method     SHELXL97
_refine_ls_extinction_coef     0.0018(2)
_refine_ls_extinction_expression
                                  'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
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'
    'O' 'O' 0.0106 0.0060
                         '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'
_computing_data_collection     'XSCANS (Bruker, 1997)'
_computing_cell_refinement     'XSCANS'
_computing_data_reduction     'XSCANS'
_computing_structure_solution     'SHELXTL (Sheldrick, 1995)'
_computing_structure_refinement     'SHELXTL'
_computing_molecular_graphics     'SHELXTL'
_computing_publication_material     'SHELXTL'
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
    Co1 0.03698(7) 0.13454(3) 0.16493(4) 0.04133(18) Uani d . 1 . . Co
    O1 -0.0583(4) 0.29237(15) 0.1988(3) 0.0629(8) Uani d . 1 . . O
    H1F -0.1561 0.2553 0.2302 0.076 Uiso d R 1 . . H
    O2 0.3519(4) 0.07993(16) 0.0533(2) 0.0569(7) Uani d . 1 . . O
    H2A 0.2546 0.0301 0.0844 0.068 Uiso d R 1 . . H
    O3 -0.2602(4) 0.19309(15) 0.2768(3) 0.0560(7) Uani d . 1 . . O
    O4 0.1384(3) -0.01871(15) 0.1260(2) 0.0521(7) Uani d . 1 . . O
    O5 -0.0936(3) 0.13720(14) 0.0150(2) 0.0465(6) Uani d . 1 . . O
    H5A -0.0951 0.0864 -0.0392 0.056 Uiso d R 1 . . H
    H5B -0.0722 0.1807 -0.0452 0.056 Uiso d R 1 . . H
    N1 0.0612(4) 0.24297(17) 0.1568(3) 0.0483(8) Uani d . 1 . . N
    N2 0.2565(4) 0.14171(18) 0.0862(3) 0.0459(8) Uani d . 1 . . N
    N3 -0.1777(4) 0.13010(18) 0.2440(3) 0.0452(8) Uani d . 1 . . N
    N4 0.0155(4) 0.02748(17) 0.1692(3) 0.0430(7) Uani d . 1 . . N
    N5 0.1633(4) 0.13874(18) 0.3137(3) 0.0507(8) Uani d . 1 . . N
    N6 0.1613(5) 0.0866(2) 0.3842(3) 0.0583(9) Uani d . 1 . . N
    N7 0.1673(7) 0.0404(3) 0.4553(4) 0.1052(17) Uani d . 1 . . N
    C1 0.2388(7) 0.3530(2) 0.0999(4) 0.0745(14) Uani d . 1 . . C
    H1A 0.1449 0.3818 0.1326 0.112 Uiso calc R 1 . . H
    H1B 0.2507 0.3660 0.0176 0.112 Uiso calc R 1 . . H
    H1C 0.3452 0.3648 0.1424 0.112 Uiso calc R 1 . . H
    C2 0.2012(6) 0.2697(2) 0.1108(3) 0.0510(10) Uani d . 1 . . C
    C3 0.3186(5) 0.2091(2) 0.0694(3) 0.0498(10) Uani d . 1 . . C
    C4 0.4918(6) 0.2240(3) 0.0167(4) 0.0674(13) Uani d . 1 . . C
    H4A 0.5451 0.1764 -0.0042 0.101 Uiso calc R 1 . . H
    H4B 0.5650 0.2503 0.0735 0.101 Uiso calc R 1 . . H
    H4C 0.4767 0.2550 -0.0531 0.101 Uiso calc R 1 . . H
    C5 -0.4121(5) 0.0458(3) 0.3129(4) 0.0607(11) Uani d . 1 . . C
    H5C -0.4670 0.0929 0.3344 0.091 Uiso calc R 1 . . H
    H5D -0.3954 0.0147 0.3825 0.091 Uiso calc R 1 . . H
    H5E -0.4848 0.0192 0.2562 0.091 Uiso calc R 1 . . H
    C6 -0.2405(5) 0.0621(2) 0.2599(3) 0.0472(9) Uani d . 1 . . C
    C7 -0.1262(5) 0.0013(2) 0.2175(3) 0.0456(9) Uani d . 1 . . C
    C8 -0.1677(6) -0.0815(2) 0.2305(4) 0.0607(11) Uani d . 1 . . C
    H8A -0.0760 -0.1115 0.1974 0.091 Uiso calc R 1 . . H
    H8B -0.2756 -0.0927 0.1894 0.091 Uiso calc R 1 . . H
    H8C -0.1782 -0.0937 0.3132 0.091 Uiso calc R 1 . . H
    O1W 0.4305(4) 0.24869(17) 0.3647(3) 0.0701(9) Uani d . 1 . . O
    H1D 0.3396 0.2100 0.3667 0.084 Uiso d R 1 . . H
    H1E 0.5334 0.2184 0.3410 0.084 Uiso d R 1 . . H
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    Co1 0.0382(3) 0.0401(3) 0.0456(3) 0.0002(2) 0.0000(2) -0.0012(2)
    O1 0.067(2) 0.0441(16) 0.078(2) 0.0101(15) 0.0086(16) -0.0062(15)
    O2 0.0477(16) 0.0617(18) 0.0617(17) 0.0110(14) 0.0074(14) -0.0011(14)
    O3 0.0479(16) 0.0512(16) 0.0694(18) 0.0106(14) 0.0118(14) -0.0079(14)
    O4 0.0496(16) 0.0444(15) 0.0623(17) 0.0050(13) 0.0033(13) -0.0067(13)
    O5 0.0502(15) 0.0447(14) 0.0443(14) 0.0004(13) -0.0057(12) 0.0005(12)
    N1 0.052(2) 0.0382(17) 0.0543(19) 0.0004(16) -0.0014(16) -0.0002(15)
    N2 0.0415(18) 0.0509(19) 0.0454(17) 0.0006(16) -0.0010(14) 0.0021(15)
    N3 0.0418(18) 0.0477(18) 0.0461(17) 0.0002(16) -0.0006(14) 0.0000(15)
    N4 0.0411(18) 0.0423(17) 0.0453(17) 0.0001(15) -0.0041(14) -0.0032(14)
    N5 0.053(2) 0.0477(19) 0.0510(19) -0.0040(17) -0.0077(16) 0.0004(16)
    N6 0.056(2) 0.062(2) 0.057(2) -0.0036(19) -0.0022(18) -0.003(2)
    N7 0.140(5) 0.100(4) 0.074(3) -0.024(3) -0.025(3) 0.036(3)
    C1 0.089(4) 0.042(2) 0.092(4) -0.016(2) -0.003(3) 0.010(2)
    C2 0.056(3) 0.045(2) 0.052(2) -0.008(2) -0.010(2) 0.0029(18)
    C3 0.044(2) 0.061(3) 0.044(2) -0.008(2) -0.0099(18) 0.0084(19)
    C4 0.048(3) 0.085(3) 0.069(3) -0.009(2) 0.005(2) 0.015(3)
    C5 0.046(2) 0.070(3) 0.066(3) -0.003(2) 0.003(2) 0.003(2)
    C6 0.045(2) 0.054(2) 0.043(2) -0.002(2) -0.0030(17) 0.0044(18)
    C7 0.047(2) 0.047(2) 0.043(2) -0.0014(19) -0.0061(18) 0.0004(18)
    C8 0.073(3) 0.049(2) 0.061(3) -0.010(2) 0.003(2) 0.003(2)
    O1W 0.0538(19) 0.0640(19) 0.093(2) -0.0060(15) 0.0054(16) -0.0280(17)
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
    Co1 N4 . 1.883(3) yes
    Co1 N3 . 1.891(3) yes
    Co1 N1 . 1.911(3) yes
    Co1 N5 . 1.919(3) yes
    Co1 N2 . 1.924(3) yes
    Co1 O5 . 1.945(2) yes
    O1 N1 . 1.354(4) yes
    O2 N2 . 1.362(4) yes
    O3 N3 . 1.328(4) yes
    O4 N4 . 1.342(4) yes
    N1 C2 . 1.290(5) yes
    N2 C3 . 1.288(5) yes
    N3 C6 . 1.298(5) yes
    N4 C7 . 1.309(5) yes
    N5 N6 . 1.210(4) yes
    N6 N7 . 1.139(5) yes
    C1 C2 . 1.493(5) no
    C2 C3 . 1.475(6) no
    C3 C4 . 1.490(6) no
    C5 C6 . 1.486(5) no
    C6 C7 . 1.467(5) no
    C7 C8 . 1.493(5) no
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
    N4 Co1 N3 . . 82.49(14) yes
    N4 Co1 N1 . . 178.59(14) yes
    N3 Co1 N1 . . 98.64(14) yes
    N4 Co1 N5 . . 93.36(13) yes
    N3 Co1 N5 . . 91.10(14) yes
    N1 Co1 N5 . . 87.47(14) yes
    N4 Co1 N2 . . 98.91(14) yes
    N3 Co1 N2 . . 178.48(14) yes
    N1 Co1 N2 . . 79.97(14) yes
    N5 Co1 N2 . . 88.24(14) yes
    N4 Co1 O5 . . 90.13(12) yes
    N3 Co1 O5 . . 88.39(12) yes
    N1 Co1 O5 . . 89.06(12) yes
    N5 Co1 O5 . . 176.37(12) yes
    N2 Co1 O5 . . 92.19(12) yes
    C2 N1 O1 . . 119.0(3) yes
    C2 N1 Co1 . . 117.6(3) yes
    O1 N1 Co1 . . 123.4(3) yes
    C3 N2 O2 . . 119.0(3) yes
    C3 N2 Co1 . . 117.3(3) yes
    O2 N2 Co1 . . 123.7(2) yes
    C6 N3 O3 . . 122.9(3) yes
    C6 N3 Co1 . . 115.6(3) yes
    O3 N3 Co1 . . 121.5(2) yes
    C7 N4 O4 . . 122.4(3) yes
    C7 N4 Co1 . . 115.7(3) yes
    O4 N4 Co1 . . 121.9(2) yes
    N6 N5 Co1 . . 122.1(3) yes
    N7 N6 N5 . . 175.3(5) yes
    N1 C2 C3 . . 112.7(3) no
    N1 C2 C1 . . 123.5(4) no
    C3 C2 C1 . . 123.8(4) no
    N2 C3 C2 . . 112.5(4) no
    N2 C3 C4 . . 123.8(4) no
    C2 C3 C4 . . 123.7(4) no
    N3 C6 C7 . . 113.3(3) no
    N3 C6 C5 . . 124.5(4) no
    C7 C6 C5 . . 122.2(4) no
    N4 C7 C6 . . 112.8(3) no
    N4 C7 C8 . . 124.2(4) no
    C6 C7 C8 . . 122.9(4) no
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
    O1 H1F O3 . 1.06 1.45 2.501(4) 168
    O2 H2A O4 . 1.21 1.33 2.529(4) 174
    O1W H1D N5 . 0.97 1.93 2.862(4) 161
    O1W H1E O3 1_655 0.99 1.81 2.769(4) 161
    O5 H5A O4 3 1.08 1.57 2.631(3) 167
    O5 H5B O1W 4_565 1.04 1.60 2.628(4) 171
data_global
_journal_date_recd_electronic     2002-11-21
_journal_date_accepted     2003-02-12
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2003
_journal_volume     59
_journal_issue      5
_journal_page_first     m260
_journal_page_last     m262
_journal_paper_category     EM
_publ_contact_author_name     'Guang-Qiu Shen'
_publ_contact_author_address
;
Department of Chemistry
Tsinghua University
Beijing 100084
People's Republic of China
;
_publ_contact_author_email     shengq@tsinghua.edu.cn
_publ_contact_author_fax     '(86-010)62771149'
_publ_contact_author_phone     '(86-010)62772351'
_publ_section_title
;
Aqua(azido)(dimethylglyoximato)(dimethylglyoxime)cobalt(III)
monohydrate
;
loop_
    _publ_author_name
    _publ_author_address
    'Dong, Zhi-Yong'
;
Department of Chemistry
Tsinghua University
Beijing 100084
People's Republic of China
;
    'Liu, Xuan-Wen'
;
Department of Chemistry
Tsinghua University
Beijing 100084
People's Republic of China
;
    'Wang, Xiao-Qing'
;
Department of Chemistry
Tsinghua University
Beijing 100084
People's Republic of China
;
    'Wang, Ru-Ji'
;
Department of Chemistry
Tsinghua University
Beijing 100084
People's Republic of China
;
    'Shen, Guang-Qiu'
;
Department of Chemistry
Tsinghua University
Beijing 100084
People's Republic of China
;
_exptl_special_details
;
A single crystal was selected for structure analysis by X-ray diffraction.
Intensity data were collected on a Bruker P4 diffractometer equipped with
graphite monochromatized Mo Kα. The unit cell was determined and the
parameters refined using 31 well-centered reflections with 5.0 < θ < 12.6°.
Data collection was monitored by three standards every 100 reflections. No
decay was observed except the statistical fluctuation in the range of +-4.5%.
Raw intensities were corrected for Lorentz and polarization effects, and for
absorption by an empirical method based on ψ-scan data (North et al., 1968).
;
_refine_special_details
;
The structure was solved by the direct phase determination method. All non-H
atoms were subjected to anisotropic refinement.
;
