#------------------------------------------------------------------------------
#$Date: 2016-02-14 15:26:36 +0100 (Sun 14 de Feb de 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/16/2001621.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_2001621
loop_
_publ_author_name
'Bacchi, A.'
'Ferranti, F.'
'Pelizzi, G.'
_publ_section_title
;
 Structures of two cobalt(III) sepulchrate complexes
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1163
_journal_page_last               1169
_journal_paper_doi               10.1107/S0108270192012265
_journal_volume                  49
_journal_year                    1993
_chemical_formula_moiety
' [Co (C12 H30 N8)] 3+ (Cl O4) 1- (S2 O3) 2- '
_chemical_formula_structural     ' Co (C12 H30 N8) (Cl O4) (S2 O3) '
_chemical_formula_sum            'C12 H30 Cl Co N8 O7 S2'
_chemical_formula_weight         556.93
_chemical_name_common
;
Cobalt(III)sepulchrate perchlorate thiosulphate
;
_chemical_name_systematic
;
(1,3,6,8,10,13,16,19-octaazabicyclo[6.6.6]eicosane)cobalt(III)perchlorate
thiosulphate
;
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 63 2 2'
_cell_angle_alpha                90.00000
_cell_angle_beta                 90.00000
_cell_angle_gamma                120.00000
_cell_formula_units_Z            2
_cell_length_a                   8.5520(10)
_cell_length_b                   8.5520(10)
_cell_length_c                   17.064(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      12.7
_cell_measurement_theta_min      6.6
_cell_volume                     1080.8(2)
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       'ω/2θ scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3792
_diffrn_reflns_reduction_process
;
correction for Lorentz and polarization effects
;
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         3
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  160
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    1.15
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.7113
_exptl_crystal_description       'Hexagonal plates'
_exptl_crystal_F_000             580.0
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.58
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.92
_refine_diff_density_min         -0.96
_refine_ls_abs_structure_details
;
It has not been possible to determine  the absolute configuration
unambigously because heavy atoms occupy symmetry sites
;
_refine_ls_abs_structure_Flack   0.5(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   2.49
_refine_ls_hydrogen_treatment
' refall for H21, H22 and H2N, only U's refined for H11 and H12'
_refine_ls_matrix_type           full
_refine_ls_number_constraints    33
_refine_ls_number_parameters     75
_refine_ls_number_reflns         607
_refine_ls_R_factor_obs          0.0897
_refine_ls_shift/esd_max         0.25
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         0.0968
_reflns_number_observed          3618
_reflns_number_total             644
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            al1026.cif
_cod_data_source_block           CompoundI
_cod_original_cell_volume        1080.8(3)
_cod_original_sg_symbol_H-M      ' P 63 2 2 '
_cod_original_formula_sum        ' C12 H30 Cl Co N8 O7 S2 '
_cod_database_code               2001621
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 0.0134(8) 0.0134(8) 0.0158(11) 0.0000 0.0000 0.0067(4)
N1 0.053(5) 0.053(5) 0.025(6) 0.0000 0.0000 0.027(3)
N2 0.032(5) 0.050(6) 0.030(4) 0.002(5) -0.005(4) -0.001(4)
C1 0.039(7) 0.059(8) 0.026(5) 0.002(6) -0.001(5) 0.003(6)
C2 0.143(14) 0.016(5) 0.043(6) -0.001(5) -0.038(11) -0.029(11)
Cl1 0.052(2) 0.052(2) 0.068(4) 0.0000 0.0000 0.0262(12)
O1 0.18(3) 0.18(3) 0.012(12) 0.000 0.000 0.090(13)
O2 0.084(17) 0.082(19) 0.068(10) 0.021(12) 0.015(12) 0.066(16)
S1 0.0303(18) 0.0303(18) 0.089(5) 0.0000 0.0000 0.0151(9)
S2 0.094(6) 0.094(6) 0.064(7) 0.0000 0.0000 0.047(3)
O3 0.035(8) 0.029(8) 0.129(19) 0.028(10) 0.056(10) 0.013(6)
loop_
_atom_site_label
_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_calc_flag
_atom_site_calc_attached_atom
_atom_site_type_symbol
Co1 -0.33333 -0.66667 -0.25000 0.0142(6) Uani . . Co
N1 -0.33333 -0.66667 -0.0750(7) 0.044(4) Uani . . N
N2 -0.1491(13) -0.4732(14) -0.1833(5) 0.047(4) Uani . . N
C1 -0.1667(16) -0.5050(18) -0.0956(6) 0.051(6) Uani . . C
C2 -0.145(4) -0.3042(14) -0.2068(6) 0.098(8) Uani . . C
Cl1 0.00000 0.00000 0.00000 0.058(2) Uani . . Cl
O1 0.00000 0.00000 0.0769(15) 0.067(14) Uani . . O
O2 0.122(3) -0.059(3) -0.0453(9) 0.067(14) Uani . . O
S1 0.33333 -0.33333 -0.25000 0.050(2) Uani . . S
S2 0.33333 -0.33333 -0.3744(7) 0.084(5) Uani . . S
O3 0.190(2) -0.492(2) -0.2266(11) 0.066(8) Uani . . O
H11 -0.1601(16) -0.3890(18) -0.0672(6) 0.07(4) Uiso calc C1 H
H12 -0.0558(16) -0.5214(18) -0.0759(6) 0.04(3) Uiso calc C1 H
H2N -0.05(2) -0.49(3) -0.190(9) 0.13(7) Uiso . N2 H
H21 -0.208(12) -0.271(12) -0.192(5) 0.03(3) Uiso . C2 H
H22 -0.04(2) -0.181(19) -0.193(7) 0.09(5) Uiso . C2 H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Co Cobalt 0.299 0.973 IntTabIV_Table_2.2A_2.3.1
N Nitrogen 0.004 0.003 IntTabIV_Table_2.2A_2.3.1
C Carbon 0.002 0.002 IntTabIV_Table_2.2A_2.3.1
Cl Chlorine 0.132 0.159 IntTabIV_Table_2.2A_2.3.1
O Oxygen 0.008 0.006 IntTabIV_Table_2.2A_2.3.1
S Sulphur 0.110 0.124 IntTabIV_Table_2.2A_2.3.1
H Hydrogen 0.000 0.000 IntTabIV_Table_2.2C
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
3 3 4
-1 -4 8
-6 1 1
3 0 12
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
Co1 N2 H2N 101.6(8) no
Co1 N2 C2 106.4(7) yes
Co1 N2 C1 116.9(8) yes
C2 N2 H2N 123(2) no
C1 N2 H2N 95.6(2) no
C1 N2 C2 113.2(9) yes
N1 C1 N2 112.0(10) yes
N2 C1 H12 108.0(10) no
N2 C1 H11 109.0(10) no
N1 C1 H12 108.0(10) no
N1 C1 H11 110.0(10) no
H11 C1 H12 109.0(10) no
N2 C2 H22 122(9) no
N2 C2 H21 126(6) no
H21 C2 H22 87.8(5) no
O1 Cl1 O2 119.0(10) yes
S2 S1 O3 107.1(8) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 N2 1.977(8) yes
N1 C1 1.450(10) yes
N2 C1 1.520(10) yes
N2 C2 1.48(2) yes
N2 H2N 0.9(2) no
C1 H11 1.08(2) no
C1 H12 1.08(2) no
C2 H21 0.77(12) no
C2 H22 1.01(12) no
Cl1 O1 1.31(2) yes
Cl1 O2 1.57(2) yes
S1 S2 2.120(10) yes
S1 O3 1.360(10) yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
Co1 N1 2.986(13)
Co1 N2 1.977(8)
Co1 C1 2.985(10)
Co1 C2 2.785(11)
Co1 H2N 2.35(16)
N1 N2 2.455(12)
N1 C1 1.448(11)
N1 H11 2.081(12)
N1 H12 2.057(12)
N1 H2N 2.88(16)
N2 C1 1.515(13)
N2 C2 1.48(2)
N2 H11 2.126(14)
N2 H12 2.121(15)
N2 H2N 0.9(2)
N2 H21 2.03(12)
N2 H22 2.19(15)
C1 C2 2.501(19)
C1 H11 1.08(2)
C1 H12 1.08(2)
C1 H2N 1.86(17)
C1 H21 2.74(11)
C1 H22 2.93(14)
C2 H11 2.473(15)
C2 H2N 2.1(3)
C2 H21 0.77(12)
C2 H22 1.01(12)
Cl1 O1 1.31(3)
Cl1 O2 1.57(3)
O1 O2 2.50(3)
O2 H11 2.67(2)
O2 H22 2.81(13)
S1 S2 2.123(13)
S1 O3 1.357(13)
S2 O3 2.84(2)
O3 H2N 2.1(2)
H11 H12 1.76(3)
H11 H2N 2.6(2)
H11 H21 2.47(9)
H11 H22 2.64(13)
H12 H2N 1.95(15)
H2N H21 2.8(3)
H2N H22 2.6(3)
H21 H22 1.25(18)
