#------------------------------------------------------------------------------
#$Date: 2016-02-16 17:55:33 +0100 (mar 16 de feb de 2016) $
#$Revision: 176466 $
#$URL: svn://www.crystallography.net/cod/cif/8/00/00/8000029.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_8000029
loop_
_publ_author_name
'Takashi Komiyama'
'Satoshi Igarashi'
'Yoshimasa Hoshino'
'Yasuhiko Yukawa'
_publ_section_title
;
 Changing Mixed-valence State of Hexacobalt Cluster by Substituting
 Central Metal Ion and by Electrochemical Reduction -- Different
 Mixed-valence States of [M{Co(prolinato)2}6]4+ (M =Ba2+ and La3+)
;
_journal_issue                   3
_journal_name_full               'Chemistry Letters'
_journal_page_first              300
_journal_paper_doi               10.1246/cl.2005.300
_journal_volume                  34
_journal_year                    2005
_chemical_formula_sum            'C60 H96 Ba Cl4 Co6 N12 O40'
_chemical_formula_weight         2258.22
_chemical_name_common
;bis{bis(L-prolinato)cobaltl(III)}tetrakis{bis(L-prolinato)cobaltl(II)}
barium(II) perchlorate
;
_space_group_IT_number           196
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      196
_symmetry_space_group_name_Hall  'F 2 2 3'
_symmetry_space_group_name_H-M   'F 2 3'
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.3922(5)
_cell_length_b                   21.3922(5)
_cell_length_c                   21.3922(5)
_cell_measurement_reflns_used    40416
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      32.6
_cell_measurement_theta_min      1.6
_cell_volume                     9789.7(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    'DIRDIF94 (PATTY)'
_diffrn_ambient_temperature      296.2
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_diffrn_measurement_device_type  'Rigaku RAXIS-IV Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            28600
_diffrn_reflns_theta_full        32.53
_diffrn_reflns_theta_max         32.53
_exptl_absorpt_coefficient_mu    1.581
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.856
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Higashi, 1999)'
_exptl_crystal_colour            darkbrown
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tetrahedral
_exptl_crystal_F_000             4584.00
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.32
_refine_diff_density_min         -0.55
_refine_ls_abs_structure_Flack   0.1(1)
_refine_ls_extinction_coef       0.0016(2)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     80
_refine_ls_number_reflns         789
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.0025
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo) + 0.00281|Fo|²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0682
_reflns_number_gt                789
_reflns_number_total             1604
_reflns_threshold_expression     F²>3.0σ(F²)
_cod_original_sg_symbol_H-M      'F 2 3        '
_cod_original_formula_sum        'C60 H96 Ba Cl4 Co6 N12 O40 '
_cod_database_code               8000029
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
z,x,y
y,z,x
x,-y,-z
z,-x,-y
y,-z,-x
-x,y,-z
-z,x,-y
-y,z,-x
-x,-y,z
-z,-x,y
-y,-z,x
x,1/2+y,1/2+z
z,1/2+x,1/2+y
y,1/2+z,1/2+x
x,1/2-y,1/2-z
z,1/2-x,1/2-y
y,1/2-z,1/2-x
-x,1/2+y,1/2-z
-z,1/2+x,1/2-y
-y,1/2+z,1/2-x
-x,1/2-y,1/2+z
-z,1/2-x,1/2+y
-y,1/2-z,1/2+x
1/2+x,y,1/2+z
1/2+z,x,1/2+y
1/2+y,z,1/2+x
1/2+x,-y,1/2-z
1/2+z,-x,1/2-y
1/2+y,-z,1/2-x
1/2-x,y,1/2-z
1/2-z,x,1/2-y
1/2-y,z,1/2-x
1/2-x,-y,1/2+z
1/2-z,-x,1/2+y
1/2-y,-z,1/2+x
1/2+x,1/2+y,z
1/2+z,1/2+x,y
1/2+y,1/2+z,x
1/2+x,1/2-y,-z
1/2+z,1/2-x,-y
1/2+y,1/2-z,-x
1/2-x,1/2+y,-z
1/2-z,1/2+x,-y
1/2-y,1/2+z,-x
1/2-x,1/2-y,z
1/2-z,1/2-x,y
1/2-y,1/2-z,x
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Ba(1) Ba 0.0000 0.0000 0.0000 0.04081(6) Uani 1.00 d SP
Co(1) Co 0.17471(6) 0.0000 0.0000 0.0496(3) Uani 1.00 d S
Cl(1) Cl 0.3761 0.3761 0.3761 0.2288 Uani 0.75 d SP
Cl(2) Cl -0.2500 -0.2500 -0.2500 0.0936 Uani 1.00 d SP
O(1) O 0.1111(2) 0.0699(2) 0.0010(6) 0.051(1) Uani 1.00 d .
O(2) O 0.0964(3) 0.1733(2) 0.0012(6) 0.063(2) Uani 1.00 d .
O(3) O 0.3172 0.4174 0.3739 0.2778 Uani 0.75 d P
O(4) O 0.4168 0.4168 0.4168 0.3404 Uani 0.75 d SP
O(5) O -0.2115 -0.2115 -0.2115 0.2679 Uani 1.00 d SP
N(1) N 0.2357(3) 0.0758(4) 0.0055(8) 0.066(2) Uani 1.00 d .
C(1) C 0.1308(4) 0.1250(4) -0.002(1) 0.060(2) Uani 1.00 d .
C(2) C 0.2003(4) 0.1346(5) 0.001(1) 0.091(3) Uani 1.00 d .
C(3) C 0.223(1) 0.169(1) -0.051(2) 0.21(1) Uani 1.00 d .
C(4) C 0.285(1) 0.146(1) -0.061(1) 0.153(10) Uani 1.00 d .
C(5) C 0.2822(7) 0.0805(9) -0.0475(10) 0.118(6) Uani 1.00 d .
H(1) H 0.2580 0.0732 0.0442 0.0752 Uiso 1.00 calc .
H(2) H 0.2106 0.1610 0.0385 0.1069 Uiso 1.00 calc .
H(3) H 0.1977 0.1534 -0.0919 0.2497 Uiso 1.00 calc .
H(4) H 0.2200 0.2113 -0.0542 0.2497 Uiso 1.00 calc .
H(5) H 0.2988 0.1532 -0.1077 0.1704 Uiso 1.00 calc .
H(6) H 0.3127 0.1704 -0.0386 0.1704 Uiso 1.00 calc .
H(7) H 0.3230 0.0659 -0.0350 0.1284 Uiso 1.00 calc .
H(8) H 0.2693 0.0557 -0.0827 0.1284 Uiso 1.00 calc .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ba Ba -0.324 2.282
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Co Co 0.349 0.972
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Cl Cl 0.148 0.159
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O(1) Ba(1) O(1) 62.5(4) . 2_555 yes
O(1) Ba(1) O(1) 62.5(4) . 3_555 yes
O(1) Ba(1) O(1) 64.4(2) . 4_555 yes
O(1) Ba(1) O(1) 116.6(1) . 5_555 yes
O(1) Ba(1) O(1) 63.9(4) . 6_555 yes
O(1) Ba(1) O(1) 115.6(2) . 7_555 yes
O(1) Ba(1) O(1) 63.9(4) . 8_555 yes
O(1) Ba(1) O(1) 116.95(10) . 9_555 yes
O(1) Ba(1) O(1) 179.1(5) . 10_555 yes
O(1) Ba(1) O(1) 116.95(10) . 11_555 yes
O(1) Ba(1) O(1) 116.6(1) . 12_555 yes
O(1) Ba(1) O(1) 62.5(4) 2_555 3_555 yes
O(1) Ba(1) O(1) 116.6(1) 2_555 4_555 yes
O(1) Ba(1) O(1) 179.1(5) 2_555 5_555 yes
O(1) Ba(1) O(1) 116.95(10) 2_555 6_555 yes
O(1) Ba(1) O(1) 63.9(4) 2_555 7_555 yes
O(1) Ba(1) O(1) 64.4(2) 2_555 8_555 yes
O(1) Ba(1) O(1) 116.6(1) 2_555 9_555 yes
O(1) Ba(1) O(1) 116.95(10) 2_555 10_555 yes
O(1) Ba(1) O(1) 115.6(2) 2_555 11_555 yes
O(1) Ba(1) O(1) 63.9(4) 2_555 12_555 yes
O(1) Ba(1) O(1) 63.9(4) 3_555 4_555 yes
O(1) Ba(1) O(1) 116.95(10) 3_555 5_555 yes
O(1) Ba(1) O(1) 115.6(2) 3_555 6_555 yes
O(1) Ba(1) O(1) 116.95(10) 3_555 7_555 yes
O(1) Ba(1) O(1) 116.6(1) 3_555 8_555 yes
O(1) Ba(1) O(1) 179.1(5) 3_555 9_555 yes
O(1) Ba(1) O(1) 116.6(1) 3_555 10_555 yes
O(1) Ba(1) O(1) 63.9(4) 3_555 11_555 yes
O(1) Ba(1) O(1) 64.4(2) 3_555 12_555 yes
O(1) Ba(1) O(1) 62.5(4) 4_555 5_555 yes
O(1) Ba(1) O(1) 62.5(4) 4_555 6_555 yes
O(1) Ba(1) O(1) 179.1(5) 4_555 7_555 yes
O(1) Ba(1) O(1) 116.95(10) 4_555 8_555 yes
O(1) Ba(1) O(1) 116.6(1) 4_555 9_555 yes
O(1) Ba(1) O(1) 115.6(2) 4_555 10_555 yes
O(1) Ba(1) O(1) 63.9(4) 4_555 11_555 yes
O(1) Ba(1) O(1) 116.95(10) 4_555 12_555 yes
O(1) Ba(1) O(1) 62.5(4) 5_555 6_555 yes
O(1) Ba(1) O(1) 116.95(10) 5_555 7_555 yes
O(1) Ba(1) O(1) 115.6(2) 5_555 8_555 yes
O(1) Ba(1) O(1) 63.9(4) 5_555 9_555 yes
O(1) Ba(1) O(1) 63.9(4) 5_555 10_555 yes
O(1) Ba(1) O(1) 64.4(2) 5_555 11_555 yes
O(1) Ba(1) O(1) 116.6(1) 5_555 12_555 yes
O(1) Ba(1) O(1) 116.6(1) 6_555 7_555 yes
O(1) Ba(1) O(1) 63.9(4) 6_555 8_555 yes
O(1) Ba(1) O(1) 64.4(2) 6_555 9_555 yes
O(1) Ba(1) O(1) 116.95(10) 6_555 10_555 yes
O(1) Ba(1) O(1) 116.6(1) 6_555 11_555 yes
O(1) Ba(1) O(1) 179.1(5) 6_555 12_555 yes
O(1) Ba(1) O(1) 62.5(4) 7_555 8_555 yes
O(1) Ba(1) O(1) 62.5(4) 7_555 9_555 yes
O(1) Ba(1) O(1) 64.4(2) 7_555 10_555 yes
O(1) Ba(1) O(1) 116.6(1) 7_555 11_555 yes
O(1) Ba(1) O(1) 63.9(4) 7_555 12_555 yes
O(1) Ba(1) O(1) 62.5(4) 8_555 9_555 yes
O(1) Ba(1) O(1) 116.6(1) 8_555 10_555 yes
O(1) Ba(1) O(1) 179.1(5) 8_555 11_555 yes
O(1) Ba(1) O(1) 116.95(10) 8_555 12_555 yes
O(1) Ba(1) O(1) 63.9(4) 9_555 10_555 yes
O(1) Ba(1) O(1) 116.95(10) 9_555 11_555 yes
O(1) Ba(1) O(1) 115.6(2) 9_555 12_555 yes
O(1) Ba(1) O(1) 62.5(4) 10_555 11_555 yes
O(1) Ba(1) O(1) 62.5(4) 10_555 12_555 yes
O(1) Ba(1) O(1) 62.5(4) 11_555 12_555 yes
O(1) Co(1) O(1) 95.4(3) . 4_555 yes
O(1) Co(1) O(2) 88.3(5) . 3_555 yes
O(1) Co(1) O(2) 90.6(5) . 6_555 yes
O(1) Co(1) N(1) 81.1(3) . . yes
O(1) Co(1) N(1) 175.6(5) . 4_555 yes
O(1) Co(1) O(2) 90.6(5) 4_555 3_555 yes
O(1) Co(1) O(2) 88.3(5) 4_555 6_555 yes
O(1) Co(1) N(1) 175.6(5) 4_555 . yes
O(1) Co(1) N(1) 81.1(3) 4_555 4_555 yes
O(2) Co(1) O(2) 178.3(3) 3_555 6_555 yes
O(2) Co(1) N(1) 86.7(5) 3_555 . yes
O(2) Co(1) N(1) 94.3(5) 3_555 4_555 yes
O(2) Co(1) N(1) 94.3(5) 6_555 . yes
O(2) Co(1) N(1) 86.7(5) 6_555 4_555 yes
N(1) Co(1) N(1) 102.5(5) . 4_555 yes
O(3) Cl(1) O(3) 117.4917(5) . 2_555 yes
O(3) Cl(1) O(3) 117.4917(7) . 3_555 yes
O(3) Cl(1) O(4) 99.204(1) . . yes
O(3) Cl(1) O(3) 117.4917(2) 2_555 3_555 yes
O(3) Cl(1) O(4) 99.2 2_555 . yes
O(3) Cl(1) O(4) 99.204(1) 3_555 . yes
O(5) Cl(2) O(5) 109.4712(6) . 46_445 yes
O(5) Cl(2) O(5) 109.4712(6) . 31_454 yes
O(5) Cl(2) O(5) 109.471(1) . 16_544 yes
O(5) Cl(2) O(5) 109.471(1) 46_445 31_454 yes
O(5) Cl(2) O(5) 109.4712(6) 46_445 16_544 yes
O(5) Cl(2) O(5) 109.4712(6) 31_454 16_544 yes
Ba(1) O(1) Co(1) 100.1(2) . . yes
Ba(1) O(1) C(1) 141.8(5) . . yes
Co(1) O(1) C(1) 117.9(5) . . yes
Co(1) O(2) C(1) 126.2(5) 2_555 . yes
Co(1) N(1) C(2) 109.8(5) . . yes
Co(1) N(1) C(5) 114(1) . . yes
Co(1) N(1) H(1) 108.4 . . no
C(2) N(1) C(5) 103(1) . . yes
C(2) N(1) H(1) 111.3 . . no
C(5) N(1) H(1) 109.0 . . no
O(1) C(1) O(2) 124.6(8) . . yes
O(1) C(1) C(2) 117.4(8) . . yes
O(2) C(1) C(2) 117.4(7) . . yes
N(1) C(2) C(1) 113.3(7) . . yes
N(1) C(2) C(3) 108(1) . . yes
N(1) C(2) H(2) 108.3 . . no
C(1) C(2) C(3) 112(2) . . yes
C(1) C(2) H(2) 108.9 . . no
C(3) C(2) H(2) 105.2 . . no
C(2) C(3) C(4) 104(1) . . yes
C(2) C(3) H(3) 107.0 . . no
C(2) C(3) H(4) 122.4 . . no
C(4) C(3) H(3) 104.9 . . no
C(4) C(3) H(4) 114.1 . . no
H(3) C(3) H(4) 102.4 . . no
C(3) C(4) C(5) 105(1) . . yes
C(3) C(4) H(5) 109.4 . . no
C(3) C(4) H(6) 109.2 . . no
C(5) C(4) H(5) 109.8 . . no
C(5) C(4) H(6) 119.3 . . no
H(5) C(4) H(6) 103.5 . . no
N(1) C(5) C(4) 104(1) . . yes
N(1) C(5) H(7) 111.5 . . no
N(1) C(5) H(8) 111.2 . . no
C(4) C(5) H(7) 109.2 . . no
C(4) C(5) H(8) 113.7 . . no
H(7) C(5) H(8) 107.3 . . no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ba(1) O(1) 2.807(4) . yes
Ba(1) O(1) 2.807(4) 2_555 yes
Ba(1) O(1) 2.807(4) 3_555 yes
Ba(1) O(1) 2.807(4) 4_555 yes
Ba(1) O(1) 2.807(4) 5_555 yes
Ba(1) O(1) 2.807(4) 6_555 yes
Ba(1) O(1) 2.807(4) 7_555 yes
Ba(1) O(1) 2.807(4) 8_555 yes
Ba(1) O(1) 2.807(4) 9_555 yes
Ba(1) O(1) 2.807(4) 10_555 yes
Ba(1) O(1) 2.807(4) 11_555 yes
Ba(1) O(1) 2.807(4) 12_555 yes
Co(1) O(1) 2.022(5) . yes
Co(1) O(1) 2.022(5) 4_555 yes
Co(1) O(2) 2.063(6) 3_555 yes
Co(1) O(2) 2.063(6) 6_555 yes
Co(1) N(1) 2.085(8) . yes
Co(1) N(1) 2.085(8) 4_555 yes
Cl(1) O(3) 1.540 . yes
Cl(1) O(3) 1.540 2_555 yes
Cl(1) O(3) 1.540 3_555 yes
Cl(1) O(4) 1.507 . yes
Cl(2) O(5) 1.427 . yes
Cl(2) O(5) 1.427 46_445 yes
Cl(2) O(5) 1.427 31_454 yes
Cl(2) O(5) 1.427 16_544 yes
O(1) C(1) 1.255(9) . yes
O(2) C(1) 1.269(10) . yes
N(1) C(2) 1.47(1) . yes
N(1) C(5) 1.51(2) . yes
N(1) H(1) 0.959 . no
C(1) C(2) 1.50(1) . yes
C(2) C(3) 1.43(3) . yes
C(2) H(2) 1.007 . no
C(3) C(4) 1.43(3) . yes
C(3) H(3) 1.079 . no
C(3) H(4) 0.908 . no
C(4) C(5) 1.43(3) . yes
C(4) H(5) 1.059 . no
C(4) H(6) 0.913 . no
C(5) H(7) 0.965 . no
C(5) H(8) 0.962 . no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Ba(1) Co(1) 3.737(1) . yes
Co(1) Co(1) 5.285(2) 2_555 yes
Co(1) Co(1) 7.475(2) 7_555 yes
