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###                                                                        ###
###        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 2.4.    #
#                                                                            #
# 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                                                              #
#                                                                            #
# This file may be used for bona fide research purposes within the           #
# scientific community so long as proper attribution is given to the journal # 
# article from which it was obtained.                                        #
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##############################################################################
                                             
data_I
_audit_creation_method     SHELXL-97
_chemical_name_systematic
;
poly[bis(trimethylammonium) [hexa-μ~1,1~-azido-tetraazidotricobaltate(II,III)]]
;
_chemical_name_common     ?
_chemical_formula_moiety     'Co3 N30, 2(C3 H10 N)'
_chemical_formula_sum     'C6 H20 Co3 N32'
_chemical_formula_iupac     '(C3 H10 N)2 [Co3 (N3)10]'
_chemical_formula_weight     717.33
_chemical_melting_point     ?
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'C 2/c'
_symmetry_space_group_name_Hall     '-C 2yc'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, y, -z+1/2'
    'x+1/2, y+1/2, z'
    '-x+1/2, y+1/2, -z+1/2'
    '-x, -y, -z'
    'x, -y, z-1/2'
    '-x+1/2, -y+1/2, -z'
    'x+1/2, -y+1/2, z-1/2'
_cell_length_a     21.7200(6)
_cell_length_b     11.3812(4)
_cell_length_c     12.1628(4)
_cell_angle_alpha     90.00
_cell_angle_beta     115.524(2)
_cell_angle_gamma     90.00
_cell_volume     2713.21(15)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     14377
_cell_measurement_theta_min     3.395
_cell_measurement_theta_max     25.028
_cell_measurement_temperature     293(2)
_exptl_crystal_description     'pillar'
_exptl_crystal_colour     'red'
_exptl_crystal_size_max     0.10
_exptl_crystal_size_mid     0.06
_exptl_crystal_size_min     0.05
_exptl_crystal_density_diffrn     1.756
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     1444
_exptl_absorpt_coefficient_mu     1.878
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details     '(REQAB; Jacobson, 1998)'
_exptl_absorpt_correction_T_min     0.708
_exptl_absorpt_correction_T_max     0.823
_exptl_special_details
;
;
_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     'Rigaku Saturn'
_diffrn_measurement_method     'dtprofit.ref scans'
_diffrn_detector_area_resol_mean     0.76
_diffrn_reflns_number     22049
_diffrn_reflns_av_R_equivalents     0.1028
_diffrn_reflns_av_sigmaI/netI     0.0719
_diffrn_reflns_theta_min     3.58
_diffrn_reflns_theta_max     25.03
_diffrn_reflns_theta_full     25.03
_diffrn_measured_fraction_theta_max     0.997
_diffrn_measured_fraction_theta_full     0.997
_diffrn_reflns_limit_h_min     -25
_diffrn_reflns_limit_h_max     25
_diffrn_reflns_limit_k_min     -13
_diffrn_reflns_limit_k_max     13
_diffrn_reflns_limit_l_min     -14
_diffrn_reflns_limit_l_max     14
_diffrn_standards_number     0
_diffrn_standards_interval_count     .
_diffrn_standards_interval_time     .
_diffrn_standards_decay_%     ?
_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 >
σ(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     2389
_reflns_number_gt     1481
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0722
_refine_ls_R_factor_gt     0.0317
_refine_ls_wR_factor_gt     0.0558
_refine_ls_wR_factor_ref     0.0611
_refine_ls_goodness_of_fit_ref     0.983
_refine_ls_restrained_S_all     1.006
_refine_ls_number_reflns     2389
_refine_ls_number_parameters     190
_refine_ls_number_restraints     24
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
         'calc w=1/[σ²(Fo²)+(0.0204P)²+0.0000P] 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     0.001
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.313
_refine_diff_density_min     -0.346
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_extinction_coef     0.00084(18)
_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'
    'Co' 'Co' 0.3494 0.9721
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'CrystalClear (Rigaku/MSC, 2006)'
_computing_cell_refinement     'CrystalClear (Rigaku/MSC, 2006)'
_computing_data_reduction     'CrystalClear (Rigaku/MSC, 2006)'
_computing_structure_solution     'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics     'SHELXTL (Sheldrick, 2008)'
_computing_publication_material     'publCIF (Westrip, 2010)'
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_disorder_assembly
    _atom_site_disorder_group
    Co Co1 0.04965(2) 0.10300(4) 0.05706(4) 0.03529(17) Uani d . 1 . .
    Co Co2 0.0000 -0.04737(5) 0.2500 0.0402(2) Uani d S 1 . .
    N N1 0.06948(14) 0.0409(2) 0.2209(3) 0.0428(6) Uani d U 1 . .
    N N2 0.12002(17) 0.0827(3) 0.3042(3) 0.0448(6) Uani d U 1 . .
    N N3 0.16669(18) 0.1210(3) 0.3810(3) 0.0740(10) Uani d . 1 . .
    N N4 0.14720(14) 0.1256(2) 0.1097(3) 0.0523(7) Uani d U 1 . .
    N N5 0.16894(15) 0.1348(3) 0.0363(3) 0.0540(7) Uani d U 1 . .
    N N6 0.1925(2) 0.1442(4) -0.0308(4) 0.1069(15) Uani d . 1 . .
    N N7 0.04578(16) 0.2621(2) 0.1120(3) 0.0489(8) Uani d . 1 . .
    N N8 -0.00656(18) 0.3009(3) 0.1097(3) 0.0504(8) Uani d . 1 . .
    N N9 -0.05415(18) 0.3426(3) 0.1100(3) 0.0806(12) Uani d . 1 . .
    N N10 0.02748(13) 0.1593(3) -0.1084(2) 0.0434(6) Uani d U 1 . .
    N N11 0.04393(15) 0.2609(3) -0.1156(2) 0.0492(6) Uani d U 1 . .
    N N12 0.0599(2) 0.3555(3) -0.1195(3) 0.0930(13) Uani d . 1 . .
    N N13 -0.04827(13) 0.0595(2) 0.0083(2) 0.0384(6) Uani d U 1 . .
    N N14 -0.09288(16) 0.1253(3) -0.0627(3) 0.0425(6) Uani d U 1 . .
    N N15 -0.13450(17) 0.1858(3) -0.1255(3) 0.0715(10) Uani d . 1 . .
    N N16 0.16193(14) 0.4179(3) 0.2144(3) 0.0539(8) Uani d . 1 . .
    H H16 0.1336 0.3554 0.1828 0.065 Uiso calc R 1 . .
    C C1 0.2022(2) 0.3949(5) 0.3459(4) 0.1044(17) Uani d . 1 . .
    H H1A 0.2292 0.4628 0.3840 0.157 Uiso calc R 1 . .
    H H1B 0.2316 0.3287 0.3565 0.157 Uiso calc R 1 . .
    H H1C 0.1719 0.3783 0.3826 0.157 Uiso calc R 1 . .
    C C2 0.1190(3) 0.5217(4) 0.1950(5) 0.1125(19) Uani d . 1 . .
    H H2A 0.0852 0.5067 0.2242 0.169 Uiso calc R 1 . .
    H H2B 0.0970 0.5396 0.1096 0.169 Uiso calc R 1 . .
    H H2C 0.1468 0.5871 0.2384 0.169 Uiso calc R 1 . .
    C C3 0.2062(2) 0.4251(5) 0.1509(4) 0.1121(19) Uani d . 1 . .
    H H3A 0.1787 0.4379 0.0655 0.168 Uiso calc R 1 . .
    H H3B 0.2311 0.3529 0.1621 0.168 Uiso calc R 1 . .
    H H3C 0.2377 0.4891 0.1837 0.168 Uiso calc R 1 . .
_geom_special_details
;
All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s 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 N7 . 1.944(3) yes
    Co1 N4 . 1.948(3) yes
    Co1 N10 . 1.964(3) yes
    Co1 N1 . 1.979(3) yes
    Co1 N13 5 2.008(3) yes
    Co1 N13 . 2.008(3) yes
    Co2 N1 2 1.968(3) yes
    Co2 N1 . 1.968(3) yes
    Co2 N10 5 2.014(3) yes
    Co2 N10 6_556 2.014(3) yes
    N1 N2 . 1.224(4) ?
    N2 N3 . 1.129(4) ?
    N4 N5 . 1.181(4) ?
    N5 N6 . 1.140(4) ?
    N7 N8 . 1.209(4) ?
    N8 N9 . 1.139(4) ?
    N10 N11 . 1.225(4) ?
    N10 Co2 5 2.014(3) ?
    N11 N12 . 1.139(4) ?
    N13 N14 . 1.234(4) ?
    N13 Co1 5 2.008(3) ?
    N14 N15 . 1.131(4) ?
    N16 C2 . 1.460(5) ?
    N16 C3 . 1.473(4) ?
    N16 C1 . 1.478(5) ?
    N16 H16 . 0.9100 ?
    C1 H1A . 0.9600 ?
    C1 H1B . 0.9600 ?
    C1 H1C . 0.9600 ?
    C2 H2A . 0.9600 ?
    C2 H2B . 0.9600 ?
    C2 H2C . 0.9600 ?
    C3 H3A . 0.9600 ?
    C3 H3B . 0.9600 ?
    C3 H3C . 0.9600 ?
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
    N7 Co1 N4 . . 88.05(12) ?
    N7 Co1 N10 . . 91.18(12) ?
    N4 Co1 N10 . . 92.62(12) ?
    N7 Co1 N1 . . 90.55(12) ?
    N4 Co1 N1 . . 88.97(12) ?
    N10 Co1 N1 . . 177.69(12) ?
    N7 Co1 N13 . 5 176.56(13) ?
    N4 Co1 N13 . 5 94.61(11) ?
    N10 Co1 N13 . 5 86.53(11) ?
    N1 Co1 N13 . 5 91.67(11) ?
    N7 Co1 N13 . . 97.71(11) ?
    N4 Co1 N13 . . 173.16(12) ?
    N10 Co1 N13 . . 90.96(11) ?
    N1 Co1 N13 . . 87.29(11) ?
    N13 Co1 N13 5 . 79.78(11) ?
    N1 Co2 N1 2 . 118.61(16) ?
    N1 Co2 N10 2 5 120.58(11) ?
    N1 Co2 N10 . 5 97.86(11) ?
    N1 Co2 N10 2 6_556 97.86(11) ?
    N1 Co2 N10 . 6_556 120.58(11) ?
    N10 Co2 N10 5 6_556 101.58(16) ?
    N2 N1 Co2 . . 122.3(2) ?
    N2 N1 Co1 . . 115.0(2) ?
    Co2 N1 Co1 . . 120.82(15) ?
    N3 N2 N1 . . 179.9(5) ?
    N5 N4 Co1 . . 119.7(3) ?
    N6 N5 N4 . . 177.2(4) ?
    N8 N7 Co1 . . 120.8(2) ?
    N9 N8 N7 . . 176.5(4) ?
    N11 N10 Co1 . . 115.5(2) ?
    N11 N10 Co2 . 5 121.6(2) ?
    Co1 N10 Co2 . 5 121.43(14) ?
    N12 N11 N10 . . 178.5(4) ?
    N14 N13 Co1 . 5 114.1(2) ?
    N14 N13 Co1 . . 118.0(2) ?
    Co1 N13 Co1 5 . 100.22(11) ?
    N15 N14 N13 . . 178.2(4) ?
    C2 N16 C3 . . 112.7(4) ?
    C2 N16 C1 . . 110.9(4) ?
    C3 N16 C1 . . 111.2(3) ?
    C2 N16 H16 . . 107.3 ?
    C3 N16 H16 . . 107.3 ?
    C1 N16 H16 . . 107.3 ?
    N16 C1 H1A . . 109.5 ?
    N16 C1 H1B . . 109.5 ?
    H1A C1 H1B . . 109.5 ?
    N16 C1 H1C . . 109.5 ?
    H1A C1 H1C . . 109.5 ?
    H1B C1 H1C . . 109.5 ?
    N16 C2 H2A . . 109.5 ?
    N16 C2 H2B . . 109.5 ?
    H2A C2 H2B . . 109.5 ?
    N16 C2 H2C . . 109.5 ?
    H2A C2 H2C . . 109.5 ?
    H2B C2 H2C . . 109.5 ?
    N16 C3 H3A . . 109.5 ?
    N16 C3 H3B . . 109.5 ?
    H3A C3 H3B . . 109.5 ?
    N16 C3 H3C . . 109.5 ?
    H3A C3 H3C . . 109.5 ?
    H3B C3 H3C . . 109.5 ?
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
    N16 H16 N7 . 0.910 2.023 2.890 158.68
data_global
_journal_date_recd_electronic     2010-11-14
_journal_date_accepted     2010-11-26
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2011
_journal_volume     67
_journal_issue      1
_journal_page_first     m27
_journal_page_last     m27
_journal_paper_category     QM
_journal_coeditor_code     WM2430
_publ_contact_author_name     'Yan-Ju Liu'
_publ_contact_author_address
;
Pharmacy College, Henan University of Traditional Chinese Medicine, Zhengzhou
450008, People's Republic of China
;
_publ_contact_author_email     'liuyanju886@163.com'
_publ_contact_author_fax     '86-371-65962746'
_publ_contact_author_phone     '86-371-65962746'
_publ_section_title
;
The azide-bridged mixed-valent cobalt(II,III) compound
[(CH₃)₃NH]₂[CoIICoIII₂(N₃)₁₀]
;
loop_
    _publ_author_name
    _publ_author_footnote
    _publ_author_address
    'Liu, Yan-Ju' .
;
Pharmacy College, Henan University of Traditional Chinese Medicine
Zhengzhou 450008, People's Republic of China
;
    'Li, Yu-Xian' .
;
Pharmacy College, Henan University of Traditional Chinese Medicine
Zhengzhou 450008, People's Republic of China
;
    'Xu, Min' .
;
Pharmacy College, Henan University of Traditional Chinese Medicine
Zhengzhou 450008, People's Republic of China
;
    'Wang, Xia' .
;
Pharmacy College, Henan University of Traditional Chinese Medicine
Zhengzhou 450008, People's Republic of China
;
