#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:28:44 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180264 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/50/7115040.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_7115040
loop_
_publ_author_name
'Liu, Cai-Ming'
'Gao, Song'
'Wang, Zhe-Ming'
'Hu, Huai-Ming'
_publ_section_title
;
 A novel bimetallic cage complex constructed from six V4Co pentatomic
 rings: hydrothermal synthesis and crystal structure of
 [(2,2′-Py2NH)2Co]3V8O23
;
_journal_issue                   17
_journal_name_full               'Chemical Communications'
_journal_page_first              1636
_journal_paper_doi               10.1039/b104273b
_journal_year                    2001
_chemical_formula_sum            'C60 H54 Co3 N18 O23 V8'
_chemical_formula_weight         1979.52
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           167
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   22.596(3)
_cell_length_b                   22.596(3)
_cell_length_c                   27.515(6)
_cell_measurement_temperature    293(2)
_cell_volume                     12166(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0143
_diffrn_reflns_av_sigmaI/netI    0.0199
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            5972
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.83
_exptl_absorpt_coefficient_mu    1.551
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5934
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3107
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0791P)²+50.3396P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1397
_refine_ls_wR_factor_ref         0.1629
_reflns_number_gt                2259
_reflns_number_total             3107
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b104273b.txt
_cod_data_source_block           cov
_cod_original_cell_volume        12167(3)
_cod_database_code               7115040
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.44101(3) 0.10768(3) 0.0833 0.0432(2) Uani 1 2 d S . .
V1 V 0.51038(4) 0.27876(3) 0.03400(3) 0.0580(2) Uani 1 1 d . . .
V2 V 0.6667 0.3333 -0.02142(6) 0.0652(4) Uani 0.90 3 d SP . 1
V2' V 0.6667 0.3333 0.0179(3) 0.0232(14) Uiso 0.10 3 d SP . 2
C1 C 0.4211(3) 0.0016(3) 0.15926(17) 0.0687(12) Uani 1 1 d . . .
H1A H 0.4492 0.0405 0.1774 0.082 Uiso 1 1 calc R . .
C2 C 0.3913(4) -0.0597(3) 0.1822(2) 0.0932(18) Uani 1 1 d . . .
H2A H 0.3988 -0.0627 0.2151 0.112 Uiso 1 1 calc R . .
C3 C 0.3498(4) -0.1173(3) 0.1557(3) 0.107(2) Uani 1 1 d . . .
H3A H 0.3281 -0.1599 0.1706 0.128 Uiso 1 1 calc R . .
C4 C 0.3407(3) -0.1117(3) 0.1076(2) 0.0847(16) Uani 1 1 d . . .
H4A H 0.3121 -0.1503 0.0894 0.102 Uiso 1 1 calc R . .
C5 C 0.3750(2) -0.0466(2) 0.08532(16) 0.0571(10) Uani 1 1 d . . .
C6 C 0.4181(2) 0.00570(19) 0.00414(15) 0.0503(8) Uani 1 1 d . . .
C7 C 0.4181(2) -0.0144(2) -0.04381(17) 0.0639(11) Uani 1 1 d . . .
H7A H 0.3871 -0.0586 -0.0538 0.077 Uiso 1 1 calc R . .
C8 C 0.4644(3) 0.0319(3) -0.07601(17) 0.0740(13) Uani 1 1 d . . .
H8A H 0.4646 0.0196 -0.1083 0.089 Uiso 1 1 calc R . .
C9 C 0.5103(3) 0.0961(3) -0.06026(17) 0.0700(12) Uani 1 1 d . . .
H9A H 0.5425 0.1280 -0.0815 0.084 Uiso 1 1 calc R . .
C10 C 0.5081(2) 0.1129(2) -0.01249(15) 0.0546(9) Uani 1 1 d . . .
H10A H 0.5400 0.1564 -0.0017 0.065 Uiso 1 1 calc R . .
N1 N 0.41244(17) 0.00944(16) 0.11157(12) 0.0525(7) Uani 1 1 d . . .
N2 N 0.46161(15) 0.06893(15) 0.01936(11) 0.0484(7) Uani 1 1 d . . .
N3 N 0.37071(18) -0.04206(16) 0.03568(14) 0.0587(8) Uani 1 1 d . . .
H3B H 0.3335 -0.0731 0.0225 0.070 Uiso 1 1 calc R . .
O1 O 0.4798(2) 0.20208(15) 0.05239(13) 0.0796(10) Uani 1 1 d . . .
O3 O 0.4513(3) 0.2801(3) 0.00136(19) 0.1205(17) Uani 1 1 d . . .
O2 O 0.5268(4) 0.3333 0.0833 0.147(3) Uani 1 2 d S . .
O4 O 0.5834(2) 0.3020(3) -0.0051(2) 0.1201(16) Uani 1 1 d . . .
O5 O 0.6667 0.3333 -0.0784(3) 0.161(5) Uani 0.90 3 d SP A 1
O5' O 0.6667 0.3333 0.0833 0.048(7) Uiso 0.20 6 d SP B 2
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'
V V 0.3005 0.5294 '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'
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
O1 Co1 O1 85.1(2) . 16_544
O1 Co1 N2 97.23(13) . 16_544
O1 Co1 N2 90.97(12) 16_544 16_544
O1 Co1 N2 90.96(12) . .
O1 Co1 N2 97.22(13) 16_544 .
N2 Co1 N2 168.90(17) 16_544 .
O1 Co1 N1 90.17(15) . 16_544
O1 Co1 N1 172.21(13) 16_544 16_544
N2 Co1 N1 83.51(12) 16_544 16_544
N2 Co1 N1 89.00(12) . 16_544
O1 Co1 N1 172.21(13) . .
O1 Co1 N1 90.17(15) 16_544 .
N2 Co1 N1 89.00(12) 16_544 .
N2 Co1 N1 83.51(12) . .
N1 Co1 N1 95.20(19) 16_544 .
O1 V1 O3 106.5(2) . .
O1 V1 O2 110.18(14) . .
O3 V1 O2 107.7(3) . .
O1 V1 O4 109.9(2) . .
O3 V1 O4 107.7(3) . .
O2 V1 O4 114.5(3) . .
O5 V2 O4 105.3(2) . 2_655
O5 V2 O4 105.3(2) . 3_665
O4 V2 O4 113.32(16) 2_655 3_665
O5 V2 O4 105.3(2) . .
O4 V2 O4 113.32(16) 2_655 .
O4 V2 O4 113.32(16) 3_665 .
O4 V2' O4 107.9(3) 2_655 3_665
O4 V2' O4 107.9(3) 2_655 .
O4 V2' O4 107.9(3) 3_665 .
O4 V2' O5' 111.0(3) 2_655 .
O4 V2' O5' 111.0(3) 3_665 .
O4 V2' O5' 111.0(3) . .
N1 C1 C2 123.7(5) . .
C1 C2 C3 118.4(6) . .
C4 C3 C2 119.7(5) . .
C3 C4 C5 119.4(6) . .
N1 C5 N3 120.2(3) . .
N1 C5 C4 120.8(4) . .
N3 C5 C4 119.1(4) . .
N2 C6 N3 120.5(4) . .
N2 C6 C7 121.7(4) . .
N3 C6 C7 117.8(4) . .
C8 C7 C6 119.2(4) . .
C9 C8 C7 119.3(4) . .
C8 C9 C10 118.9(4) . .
N2 C10 C9 122.7(4) . .
C5 N1 C1 117.9(4) . .
C5 N1 Co1 120.8(3) . .
C1 N1 Co1 120.2(3) . .
C6 N2 C10 118.1(3) . .
C6 N2 Co1 120.4(3) . .
C10 N2 Co1 119.1(3) . .
C5 N3 C6 128.7(4) . .
V1 O1 Co1 173.8(2) . .
V1 O2 V1 163.9(6) 17_554 .
V2 O4 V2' 36.3(3) . .
V2 O4 V1 158.7(4) . .
V2' O4 V1 122.5(4) . .
V2' O5' V2' 179.997(1) 16_544 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O1 2.043(3) .
Co1 O1 2.043(3) 16_544
Co1 N2 2.119(3) 16_544
Co1 N2 2.119(3) .
Co1 N1 2.125(3) 16_544
Co1 N1 2.125(3) .
V1 O1 1.593(3) .
V1 O3 1.622(4) .
V1 O2 1.7445(15) .
V1 O4 1.813(4) .
V2 O5 1.568(10) .
V2 O4 1.707(4) 2_655
V2 O4 1.707(4) 3_665
V2 O4 1.707(4) .
V2' O4 1.764(6) 2_655
V2' O4 1.764(6) 3_665
V2' O4 1.764(6) .
V2' O5' 1.800(8) .
C1 N1 1.351(6) .
C1 C2 1.357(7) .
C2 C3 1.373(9) .
C3 C4 1.354(9) .
C4 C5 1.414(6) .
C5 N1 1.331(5) .
C5 N3 1.377(6) .
C6 N2 1.334(5) .
C6 N3 1.381(5) .
C6 C7 1.395(6) .
C7 C8 1.371(7) .
C8 C9 1.365(8) .
C9 C10 1.376(6) .
C10 N2 1.347(5) .
O2 V1 1.7444(15) 17_554
O5' V2' 1.800(8) 16_544
