Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2001

data_cov 

_database_code_CSD	167670


_journal_coden_Cambridge      182

_publ_requested_journal       'Chemical Communications'

loop_
_publ_author_name
'Gao, S.'
'Hu, Huai-Ming'
'Liu, Cai-Ming'
'Wang, Zhe-Ming'


_publ_contact_author_name     	'Prof S Gao'  
_publ_contact_author_address 
;
College of Chemistry & Molecular Eng.
Peking University
State Key Laboratory of Rare Earth
Beijing
100871
CHINA
;

_publ_contact_author_email       'GAOSONG@PKU.EDU.CN'

_publ_section_title		
;
A novel bimetallic cage complex constructed from six V4Co pentatomic
rings: hydrothermal synthesis and crystal structure of
[(2,2-'Py2-NH)2Co]3V8O23
;
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C60 H54 Co3 N18 O23 V8' 
_chemical_formula_weight          1979.52 

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' 

_symmetry_cell_setting            ? 
_symmetry_space_group_name_H-M    ? 

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' 

_cell_length_a                    22.596(3) 
_cell_length_b                    22.596(3) 
_cell_length_c                    27.515(6) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      12167(3) 
_cell_formula_units_Z             6 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.621 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              5934 
_exptl_absorpt_coefficient_mu     1.551 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             5972 
_diffrn_reflns_av_R_equivalents   0.0143 
_diffrn_reflns_av_sigmaI/netI     0.0199 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        29 
_diffrn_reflns_limit_k_min        -24 
_diffrn_reflns_limit_k_max        0 
_diffrn_reflns_limit_l_min        -35 
_diffrn_reflns_limit_l_max        35 
_diffrn_reflns_theta_min          3.83 
_diffrn_reflns_theta_max          27.49 
_reflns_number_total              3107 
_reflns_number_gt                 2259 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 

_refine_special_details 
; 
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
goodness of fit S are based on F^2^, conventional R-factors R are based 
on F, with F set to zero for negative F^2^. The threshold expression of 
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F^2^ are statistically about twice as large as those based on F, and R- 
factors based on ALL data will be even larger. 
; 

_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
'calc w=1/[\s^2^(Fo^2^)+(0.0791P)^2^+50.3396P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3107 
_refine_ls_number_parameters      173 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0774 
_refine_ls_R_factor_gt            0.0532 
_refine_ls_wR_factor_ref          0.1629 
_refine_ls_wR_factor_gt           0.1397 
_refine_ls_goodness_of_fit_ref    1.055 
_refine_ls_restrained_S_all       1.055 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 

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_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
Co1 0.0408(3) 0.0408(3) 0.0485(4) -0.00195(13) 0.00195(13) 0.0207(3) 
V1 0.0589(4) 0.0413(4) 0.0772(5) 0.0065(3) 0.0033(3) 0.0276(3) 
V2 0.0633(6) 0.0633(6) 0.0690(9) 0.000 0.000 0.0316(3) 
C1 0.088(3) 0.075(3) 0.061(3) 0.012(2) 0.016(2) 0.054(3) 
C2 0.125(5) 0.099(4) 0.074(3) 0.031(3) 0.027(3) 0.070(4) 
C3 0.149(6) 0.076(4) 0.099(5) 0.038(3) 0.054(4) 0.058(4) 
C4 0.095(4) 0.055(3) 0.093(4) 0.014(3) 0.033(3) 0.029(3) 
C5 0.056(2) 0.049(2) 0.071(3) 0.0074(19) 0.0151(19) 0.0303(18) 
C6 0.055(2) 0.050(2) 0.058(2) -0.0041(16) -0.0018(17) 0.0366(18) 
C7 0.076(3) 0.064(3) 0.065(3) -0.014(2) -0.009(2) 0.045(2) 
C8 0.105(4) 0.096(4) 0.051(2) -0.005(2) 0.006(2) 0.072(3) 
C9 0.077(3) 0.086(3) 0.064(3) 0.014(2) 0.020(2) 0.054(3) 
C10 0.053(2) 0.055(2) 0.063(2) 0.0057(18) 0.0120(18) 0.0327(18) 
N1 0.0590(19) 0.0498(17) 0.0568(18) 0.0054(14) 0.0086(15) 0.0333(16) 
N2 0.0486(16) 0.0466(16) 0.0549(17) 0.0002(13) 0.0070(13) 0.0276(14) 
N3 0.0581(19) 0.0379(16) 0.074(2) -0.0077(15) -0.0010(17) 0.0194(14) 
O1 0.106(3) 0.0459(16) 0.087(2) 0.0076(15) 0.0237(19) 0.0380(17) 
O3 0.131(4) 0.145(4) 0.135(4) 0.022(3) -0.009(3) 0.106(4) 
O2 0.150(5) 0.100(5) 0.176(7) -0.084(5) -0.042(3) 0.050(2) 
O4 0.079(3) 0.117(4) 0.153(4) 0.038(3) 0.041(3) 0.041(3) 
O5 0.201(8) 0.201(8) 0.082(6) 0.000 0.000 0.100(4) 

_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_distance 
_geom_bond_site_symmetry_2 
_geom_bond_publ_flag 
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 ? 

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 
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 . ? 

_diffrn_measured_fraction_theta_max    0.995 
_diffrn_reflns_theta_full              27.49 
_diffrn_measured_fraction_theta_full   0.995 
_refine_diff_density_max    0.662 
_refine_diff_density_min   -0.667 
_refine_diff_density_rms    0.079