##############################################################################
###                                                                        ###
###        Electronic paper (Acta Crystallographica Section E)             ###
###                                                                        ###
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#                                                                            #
# 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/  #
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#            Copyright International Union of Crystallography                #
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data_global
_audit_creation_method     'form.cif (version 2.0)'
_journal_data_validation_number     ?
_journal_date_recd_electronic     2006-02-14
_journal_date_accepted     2006-03-08
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2006
_journal_volume     62
_journal_issue      4
_journal_page_first     m776
_journal_page_last     m778
_journal_paper_category     EM
_journal_coeditor_code     CI2007
_publ_contact_author_name     'Sun, Yu-Xi'
_publ_contact_author_address
;
      Department of Chemistry
      Qufu Normal University
      Qufu 273165
      People's Republic of China
;
_publ_contact_author_email     yuxisun@163.com
_publ_contact_author_fax     '0086-537-4456305'
_publ_contact_author_phone     '0086-537-4451672'
_publ_section_title
;
Bis(N,N-dimethylethane-1,2-diamine)dithiocyanatocobalt(III)
perchlorate
;
loop_
    _publ_author_name
    _publ_author_address
    'Sun, Yu-Xi'
;     Department of Chemistry
      Qufu Normal University
      Qufu 273165
      People's Republic of China
;
    'Gu, Ke-Qiang'
;     Department of Chemistry
      Qufu Normal University
      Qufu 273165
      People's Republic of China
;
    'Yang, Guang'
;     Department of Capital Management
      Qufu Normal University
      Qufu 273165
      People's Republic of China
;
    'Xie, Fei'
;     Department of Chemistry
      Qufu Normal University
      Qufu 273165
      People's Republic of China
;
    'Sun, Yun-Jin'
;     No. 2 Middle School of Junan
      Junan 276600
      People's Republic of China
;
data_I
_audit_creation_method     SHELXL-97
_chemical_name_systematic
;
Bis(N,N-dimethylethane-1,2-diamine)dithiocyanatocobalt(III) perchlorate
;
_chemical_name_common     ?
_chemical_formula_moiety     'C10 H24 Co N6 S2 +, Cl O4 -'
_chemical_formula_sum     'C10 H24 Cl Co N6 O4 S2'
_chemical_formula_iupac     '[Co (N C S)2 (C4 H12 N2)2] Cl O4'
_chemical_formula_weight     450.85
_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     14.075(3)
_cell_length_b     11.481(3)
_cell_length_c     12.366(3)
_cell_angle_alpha     90.00
_cell_angle_beta     106.380(3)
_cell_angle_gamma     90.00
_cell_volume     1917.2(8)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     1131
_cell_measurement_theta_min     2.328
_cell_measurement_theta_max     20.408
_cell_measurement_temperature     298(2)
_exptl_crystal_description     Block
_exptl_crystal_colour     brown
_exptl_crystal_size_max     0.11
_exptl_crystal_size_mid     0.11
_exptl_crystal_size_min     0.07
_exptl_crystal_density_diffrn     1.562
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     936
_exptl_absorpt_coefficient_mu     1.279
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details     '(SADABS; Sheldrick, 1996)'
_exptl_absorpt_correction_T_min     0.8721
_exptl_absorpt_correction_T_max     0.9158
_exptl_special_details
;
;
_diffrn_ambient_temperature     298(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 SMART APEX area-detector'
_diffrn_measurement_method     'φ and ω'
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     8063
_diffrn_reflns_av_R_equivalents     0.0464
_diffrn_reflns_av_sigmaI/netI     0.0519
_diffrn_reflns_theta_min     2.33
_diffrn_reflns_theta_max     27.50
_diffrn_reflns_theta_full     27.50
_diffrn_measured_fraction_theta_max     0.995
_diffrn_measured_fraction_theta_full     0.995
_diffrn_reflns_limit_h_min     -18
_diffrn_reflns_limit_h_max     18
_diffrn_reflns_limit_k_min     -14
_diffrn_reflns_limit_k_max     14
_diffrn_reflns_limit_l_min     -16
_diffrn_reflns_limit_l_max     15
_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 > 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     2199
_reflns_number_gt     1505
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0823
_refine_ls_R_factor_gt     0.0522
_refine_ls_wR_factor_gt     0.1225
_refine_ls_wR_factor_ref     0.1379
_refine_ls_goodness_of_fit_ref     1.030
_refine_ls_restrained_S_all     1.086
_refine_ls_number_reflns     2199
_refine_ls_number_parameters     150
_refine_ls_number_restraints     37
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
         'calc w=1/[σ²(Fo²)+(0.0561P)²+3.9721P] 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     0.548
_refine_diff_density_min     -0.355
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
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'
    'S' 'S' 0.1246 0.1234
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Cl' 'Cl' 0.1484 0.1585
                         '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     'SMART (Bruker, 2002)'
_computing_cell_refinement     'SAINT (Bruker, 2002)'
_computing_data_reduction     'SAINT'
_computing_structure_solution     'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics     'SHELXTL (Bruker, 1998)'
_computing_publication_material     SHELXTL
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 0.2500 0.2500 0.0000 0.0282(2) Uani d S 1 . .
    Cl Cl1 0.0000 0.30076(18) 0.2500 0.0585(5) Uani d SD 1 . .
    S S1 0.38506(9) 0.24371(10) 0.38787(9) 0.0522(3) Uani d . 1 C .
    O O1 0.0560(6) 0.3822(7) 0.2081(7) 0.125(3) Uani d PDU 0.695(7) A 1
    O O2 -0.0504(7) 0.2615(8) 0.1463(6) 0.141(3) Uani d PDU 0.695(7) A 1
    O O1' 0.1002(8) 0.3220(17) 0.2590(16) 0.125(3) Uani d PDU 0.305(7) A 2
    O O2' -0.0033(15) 0.1953(11) 0.1946(15) 0.141(3) Uani d PDU 0.305(7) . 2
    N N1 0.3706(2) 0.1736(3) -0.0102(3) 0.0425(8) Uani d . 1 C .
    H H1A 0.3803 0.1891 -0.0777 0.051 Uiso calc R 1 B 3
    H H1B 0.4227 0.2018 0.0436 0.051 Uiso calc R 1 B 3
    N N3 0.3061(3) 0.2630(3) 0.1569(3) 0.0420(8) Uani d . 1 C .
    C C1 0.3641(4) 0.0471(4) 0.0037(6) 0.0777(18) Uani d P 0.637(15) C 3
    H H1C 0.3453 0.0101 -0.0698 0.093 Uiso calc PR 0.637(15) C 3
    H H1D 0.4284 0.0171 0.0454 0.093 Uiso calc PR 0.637(15) C 3
    C C2 0.2912(6) 0.0182(7) 0.0640(11) 0.055(3) Uani d P 0.637(15) C 3
    H H2A 0.2754 -0.0641 0.0548 0.066 Uiso calc PR 0.637(15) C 3
    H H2B 0.3197 0.0332 0.1438 0.066 Uiso calc PR 0.637(15) C 3
    N N2 0.2006(2) 0.0859(3) 0.0228(3) 0.0399(8) Uani d PD 0.637(15) C 3
    C C3 0.1417(8) 0.0835(8) 0.1063(8) 0.057(3) Uani d PD 0.637(15) C 3
    H H3A 0.1299 0.0042 0.1234 0.085 Uiso calc PR 0.637(15) C 3
    H H3B 0.0796 0.1222 0.0750 0.085 Uiso calc PR 0.637(15) C 3
    H H3C 0.1778 0.1226 0.1740 0.085 Uiso calc PR 0.637(15) C 3
    C C4 0.1330(8) 0.0314(10) -0.0789(7) 0.056(3) Uani d PD 0.637(15) C 3
    H H4A 0.1142 -0.0447 -0.0601 0.084 Uiso calc PR 0.637(15) C 3
    H H4B 0.1662 0.0247 -0.1366 0.084 Uiso calc PR 0.637(15) C 3
    H H4C 0.0750 0.0788 -0.1058 0.084 Uiso calc PR 0.637(15) C 3
    C C1' 0.3641(4) 0.0471(4) 0.0037(6) 0.0777(18) Uani d P 0.363(15) C 4
    H H1'1 0.3971 0.0086 -0.0455 0.093 Uiso calc PR 0.363(15) C 4
    H H1'2 0.3996 0.0268 0.0807 0.093 Uiso calc PR 0.363(15) C 4
    C C2' 0.2702(10) 0.0052(12) -0.019(2) 0.058(5) Uani d P 0.363(15) C 4
    H H2'1 0.2719 -0.0705 0.0164 0.069 Uiso calc PR 0.363(15) C 4
    H H2'2 0.2438 -0.0054 -0.0997 0.069 Uiso calc PR 0.363(15) C 4
    N N2' 0.2006(2) 0.0859(3) 0.0228(3) 0.0399(8) Uani d PD 0.363(15) C 4
    C C3' 0.210(2) 0.0507(14) 0.1413(9) 0.072(7) Uani d PD 0.363(15) C 4
    H H3'A 0.1912 -0.0295 0.1430 0.108 Uiso calc PR 0.363(15) C 4
    H H3'B 0.1679 0.0986 0.1715 0.108 Uiso calc PR 0.363(15) C 4
    H H3'C 0.2777 0.0601 0.1858 0.108 Uiso calc PR 0.363(15) C 4
    C C4' 0.0988(9) 0.0579(17) -0.0466(19) 0.069(6) Uani d PD 0.363(15) C 4
    H H4'A 0.0863 -0.0237 -0.0403 0.104 Uiso calc PR 0.363(15) C 4
    H H4'B 0.0922 0.0768 -0.1240 0.104 Uiso calc PR 0.363(15) C 4
    H H4'C 0.0519 0.1024 -0.0204 0.104 Uiso calc PR 0.363(15) C 4
    C C5 0.3403(3) 0.2553(3) 0.2527(4) 0.0391(9) Uani d . 1 . .
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 0.0290(4) 0.0288(4) 0.0277(4) -0.0022(3) 0.0096(3) -0.0010(3)
    Cl1 0.0609(10) 0.0812(12) 0.0376(8) 0.000 0.0206(8) 0.000
    S1 0.0611(7) 0.0521(7) 0.0355(6) 0.0039(6) 0.0008(5) 0.0037(5)
    O1 0.149(5) 0.133(6) 0.117(5) -0.028(4) 0.078(4) 0.022(4)
    O2 0.156(6) 0.153(6) 0.091(5) 0.003(5) -0.004(4) -0.044(4)
    O1' 0.149(5) 0.133(6) 0.117(5) -0.028(4) 0.078(4) 0.022(4)
    O2' 0.156(6) 0.153(6) 0.091(5) 0.003(5) -0.004(4) -0.044(4)
    N1 0.0377(18) 0.043(2) 0.049(2) 0.0010(15) 0.0150(15) -0.0025(16)
    N3 0.0463(19) 0.048(2) 0.0299(17) -0.0052(15) 0.0073(14) -0.0034(15)
    C1 0.075(4) 0.038(3) 0.139(6) 0.012(3) 0.062(4) 0.002(3)
    C2 0.057(5) 0.032(4) 0.073(7) 0.006(3) 0.013(5) 0.006(4)
    N2 0.0442(19) 0.0323(18) 0.043(2) -0.0077(15) 0.0128(15) 0.0006(15)
    C3 0.064(6) 0.050(5) 0.068(6) -0.011(4) 0.036(5) 0.009(4)
    C4 0.062(6) 0.045(5) 0.055(5) -0.015(5) 0.008(4) -0.008(4)
    C1' 0.075(4) 0.038(3) 0.139(6) 0.012(3) 0.062(4) 0.002(3)
    C2' 0.047(8) 0.036(7) 0.090(15) -0.004(6) 0.019(9) -0.004(8)
    N2' 0.0442(19) 0.0323(18) 0.043(2) -0.0077(15) 0.0128(15) 0.0006(15)
    C3' 0.122(18) 0.040(8) 0.056(9) -0.024(10) 0.029(10) 0.010(6)
    C4' 0.053(9) 0.040(10) 0.107(17) -0.016(8) 0.011(9) 0.000(9)
    C5 0.044(2) 0.0317(19) 0.041(2) -0.0029(17) 0.0105(18) -0.0037(18)
_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 N1 . 1.946(3) y
    Co1 N2 . 2.055(3) y
    Co1 N3 7 1.883(4) ?
    Co1 N3 . 1.883(4) y
    Co1 N1 7 1.946(3) ?
    Co1 N2' 7 2.055(3) ?
    Co1 N2 7 2.055(3) ?
    Cl1 O2 . 1.355(6) ?
    Cl1 O2 2 1.355(6) ?
    Cl1 O2' . 1.386(8) ?
    Cl1 O2' 2 1.386(8) ?
    Cl1 O1' 2 1.405(8) ?
    Cl1 O1' . 1.405(8) ?
    Cl1 O1 2 1.412(5) ?
    Cl1 O1 . 1.412(5) ?
    S1 C5 . 1.616(4) ?
    O2' O2' 2 1.35(4) ?
    N1 C1 . 1.469(6) ?
    N1 H1A . 0.90 ?
    N1 H1B . 0.90 ?
    N3 C5 . 1.150(6) ?
    C1 C2 . 1.466(10) ?
    C1 H1C . 0.97 ?
    C1 H1D . 0.97 ?
    C2 N2 . 1.457(8) ?
    C2 H2A . 0.97 ?
    C2 H2B . 0.97 ?
    N2 C4 . 1.485(6) ?
    N2 C3 . 1.495(6) ?
    C3 H3A . 0.96 ?
    C3 H3B . 0.96 ?
    C3 H3C . 0.96 ?
    C4 H4A . 0.96 ?
    C4 H4B . 0.96 ?
    C4 H4C . 0.96 ?
    C2' H2'1 . 0.97 ?
    C2' H2'2 . 0.97 ?
    C3' H3'A . 0.96 ?
    C3' H3'B . 0.96 ?
    C3' H3'C . 0.96 ?
    C4' H4'A . 0.96 ?
    C4' H4'B . 0.96 ?
    C4' H4'C . 0.96 ?
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 Co1 N1 . 7 180 y
    N2 Co1 N2 . 7 180 y
    N3 Co1 N3 7 . 180 y
    N1 Co1 N2 . . 86.03(13) y
    N3 Co1 N1 . . 89.00(14) y
    N3 Co1 N2 . . 89.46(13) y
    N1 Co1 N2 7 7 86.03(13) ?
    N3 Co1 N1 7 . 91.00(14) ?
    N3 Co1 N1 7 7 89.00(14) ?
    N3 Co1 N1 . 7 91.00(14) y
    N3 Co1 N2 7 . 90.54(13) y
    N1 Co1 N2 7 . 93.97(13) ?
    N3 Co1 N2' 7 7 89.46(13) ?
    N3 Co1 N2' . 7 90.54(13) ?
    N1 Co1 N2' . 7 93.97(13) ?
    N1 Co1 N2' 7 7 86.03(13) ?
    N2 Co1 N2' . 7 180.00(19) ?
    N3 Co1 N2 7 7 89.46(13) ?
    N3 Co1 N2 . 7 90.54(13) ?
    N1 Co1 N2 . 7 93.97(13) y
    N2' Co1 N2 7 7 0.00(19) ?
    O2 Cl1 O2 . 2 141.2(8) ?
    O2 Cl1 O2' . . 46.1(7) ?
    O2 Cl1 O2' 2 . 96.5(10) ?
    O2 Cl1 O2' . 2 96.5(10) ?
    O2 Cl1 O2' 2 2 46.1(7) ?
    O2' Cl1 O2' . 2 58.2(17) ?
    O2 Cl1 O1' . 2 74.8(8) ?
    O2 Cl1 O1' 2 2 112.2(9) ?
    O2' Cl1 O1' . 2 102.7(12) ?
    O2' Cl1 O1' 2 2 94.8(10) ?
    O2 Cl1 O1' . . 112.2(9) ?
    O2 Cl1 O1' 2 . 74.8(8) ?
    O2' Cl1 O1' . . 94.8(10) ?
    O2' Cl1 O1' 2 . 102.7(12) ?
    O1' Cl1 O1' 2 . 160.0(16) ?
    O2 Cl1 O1 . 2 111.7(5) ?
    O2 Cl1 O1 2 2 94.0(5) ?
    O2' Cl1 O1 . 2 144.7(9) ?
    O2' Cl1 O1 2 2 109.9(10) ?
    O1' Cl1 O1 . 2 120.5(9) ?
    O2 Cl1 O1 . . 94.0(5) ?
    O2 Cl1 O1 2 . 111.7(5) ?
    O2' Cl1 O1 . . 109.9(10) ?
    O2' Cl1 O1 2 . 144.7(9) ?
    O1' Cl1 O1 2 . 120.5(9) ?
    O1 Cl1 O1 2 . 97.1(8) ?
    O2' O2' Cl1 2 . 60.9(8) ?
    C1 N1 Co1 . . 110.7(3) ?
    C1 N1 H1A . . 109.5 ?
    Co1 N1 H1A . . 109.5 ?
    C1 N1 H1B . . 109.5 ?
    Co1 N1 H1B . . 109.5 ?
    H1A N1 H1B . . 108.1 ?
    C5 N3 Co1 . . 171.1(3) ?
    C2 C1 N1 . . 111.0(5) ?
    C2 C1 H1C . . 109.4 ?
    N1 C1 H1C . . 109.4 ?
    C2 C1 H1D . . 109.4 ?
    N1 C1 H1D . . 109.4 ?
    H1C C1 H1D . . 108.0 ?
    N2 C2 C1 . . 111.8(7) ?
    N2 C2 H2A . . 109.3 ?
    C1 C2 H2A . . 109.3 ?
    N2 C2 H2B . . 109.3 ?
    C1 C2 H2B . . 109.3 ?
    H2A C2 H2B . . 107.9 ?
    C2 N2 C4 . . 111.1(6) ?
    C2 N2 C3 . . 110.5(5) ?
    C4 N2 C3 . . 103.3(6) ?
    C2 N2 Co1 . . 103.9(4) ?
    C4 N2 Co1 . . 115.5(5) ?
    C3 N2 Co1 . . 112.7(4) ?
    H2'1 C2' H2'2 . . 107.8 ?
    N3 C5 S1 . . 178.3(4) ?
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
    N1 H1B S1 2_655 0.90 2.64 3.439(3) 148
    N1 H1A O1' 7 0.90 2.34 3.217(18) 165
    N1 H1A O1 7 0.90 2.21 2.982(8) 143
