#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:07:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179094 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/56/4305608.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_4305608
loop_
_publ_author_name
'Man-Li Cao'
'Hong-Guo Hao'
'Wei-Xiong Zhang'
'Bao-Hui Ye'
_publ_section_title
;
Assembly of a Cubic Nanocage Co8L12 and a Hydrogen-Bonded 3D NbO Net Based
on the [(HCO3)2]2- Synthon and Water
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8126
_journal_page_last               8133
_journal_paper_doi               10.1021/ic800585d
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C162 H168 Co9 N60 O60'
_chemical_formula_weight         4445.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           204
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-I 2 2 3'
_symmetry_space_group_name_H-M   'I m -3'
_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                90.00
_cell_formula_units_Z            2
_cell_length_a                   21.3615(9)
_cell_length_b                   21.3615(9)
_cell_length_c                   21.3615(9)
_cell_measurement_reflns_used    1729
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      1.35
_cell_volume                     9747.5(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0939
_diffrn_reflns_av_sigmaI/netI    0.0679
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            9832
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.35
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.845
_exptl_absorpt_correction_T_max  0.9218
_exptl_absorpt_correction_T_min  0.9017
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4566
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1729
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0644
_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)+(0.1171P)²+0.3463P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1729
_refine_ls_wR_factor_ref         0.1993
_reflns_number_gt                1103
_reflns_number_total             1729
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800585d_si_002.cif
_cod_data_source_block           1
_cod_database_code               4305608
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z+1/2, x+1/2, y+1/2'
'z+1/2, x+1/2, -y+1/2'
'z+1/2, -x+1/2, y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z+1/2, x+1/2'
'-y+1/2, z+1/2, x+1/2'
'y+1/2, z+1/2, -x+1/2'
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 0.14813(3) 0.14813(3) 0.14813(3) 0.0322(4) Uani 1 3 d S . .
Co2 Co 0.0000 0.0000 0.0000 0.0441(9) Uani 1 24 d SD . .
C1 C 0.1229(2) 0.2748(2) 0.2187(2) 0.0494(13) Uani 1 1 d . . .
H1A H 0.1349 0.2520 0.2556 0.059 Uiso 1 1 d R . .
C2 C 0.1024(3) 0.3358(3) 0.2253(3) 0.0563(15) Uani 1 1 d . . .
H2A H 0.0999 0.3547 0.2660 0.068 Uiso 1 1 d R . .
C3 C 0.0856(3) 0.3681(3) 0.1736(3) 0.0609(17) Uani 1 1 d . . .
H3A H 0.0729 0.4111 0.1770 0.073 Uiso 1 1 d R . .
C4 C 0.0889(3) 0.3388(2) 0.1152(3) 0.0563(15) Uani 1 1 d . . .
H4A H 0.0755 0.3601 0.0780 0.068 Uiso 1 1 d R . .
C5 C 0.1100(2) 0.2778(2) 0.1124(2) 0.0363(11) Uani 1 1 d . . .
C6 C 0.1167(2) 0.2437(2) 0.0520(2) 0.0351(11) Uani 1 1 d . . .
C7 C 0.1473(3) 0.1538(3) 0.0000 0.0308(14) Uani 1 2 d S . .
C8 C 0.0918(7) 0.0000 0.5000 0.061(3) Uani 1 4 d S . .
N1 N 0.12705(18) 0.24604(18) 0.16347(18) 0.0379(10) Uani 1 1 d . . .
N2 N 0.13444(16) 0.18476(16) 0.05597(16) 0.0310(9) Uani 1 1 d . . .
N3 N 0.1075(3) 0.2764(2) 0.0000 0.0398(14) Uani 1 2 d S . .
O1 O 0.1704(2) 0.1013(2) 0.0000 0.0386(12) Uani 1 2 d S . .
O1W O 0.0955(3) 0.0000 0.0000 0.065(2) Uani 1 4 d S . .
H1WA H 0.1188 0.0312 0.0000 0.037(19) Uiso 1 2 d SRD . .
O2 O 0.1492(4) 0.0000 0.5000 0.086(3) Uani 1 4 d S . .
O2W O 0.2673(7) 0.0000 0.5000 0.60(4) Uani 1 4 d S . .
H2WA H 0.2255 0.0000 0.5000 0.895 Uiso 1 4 d SR . .
H2WB H 0.2843 0.0000 0.4641 0.895 Uiso 0.50 2 d SPR . .
O3 O 0.0610(3) 0.0504(3) 0.5000 0.118(3) Uani 1 2 d S . .
H3B H 0.0209 0.0504 0.5000 0.142 Uiso 1 2 d SR . .
O3W O 0.1078(5) 0.1659(4) 0.5000 0.150(4) Uani 1 2 d S . .
H3WA H 0.0888 0.1310 0.5000 0.224 Uiso 1 2 d SR . .
H3WB H 0.1452 0.1613 0.5000 0.224 Uiso 0.50 2 d SPR . .
H3WC H 0.0861 0.2033 0.5000 0.224 Uiso 0.50 2 d SPR . .
O4W O 0.2475(8) 0.1671(8) 0.5000 0.112(5) Uiso 0.50 2 d SP . .
H4WA H 0.2786 0.1401 0.5000 0.169 Uiso 0.50 2 d SPR . .
H4WB H 0.2522 0.2054 0.5000 0.169 Uiso 0.50 2 d SPR . .
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'
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
_geom_angle_publ_flag
N2 Co1 N2 105.13(11) 5 9 ?
N2 Co1 N2 105.13(11) 5 . ?
N2 Co1 N2 105.13(11) 9 . ?
N2 Co1 N1 170.54(14) 5 9 ?
N2 Co1 N1 75.96(14) 9 9 ?
N2 Co1 N1 83.41(14) . 9 ?
N2 Co1 N1 75.96(14) 5 5 ?
N2 Co1 N1 83.41(14) 9 5 ?
N2 Co1 N1 170.54(14) . 5 ?
N1 Co1 N1 94.95(14) 9 5 ?
N2 Co1 N1 83.41(14) 5 . ?
N2 Co1 N1 170.54(14) 9 . ?
N2 Co1 N1 75.96(14) . . ?
N1 Co1 N1 94.95(14) 9 . ?
N1 Co1 N1 94.95(14) 5 . ?
O1W Co2 O1W 90.0 33 . ?
O1W Co2 O1W 180.0 33 9 ?
O1W Co2 O1W 90.0 . 9 ?
O1W Co2 O1W 90.0 33 5 ?
O1W Co2 O1W 90.0 . 5 ?
O1W Co2 O1W 90.0 9 5 ?
O1W Co2 O1W 90.0 33 29 ?
O1W Co2 O1W 90.0 . 29 ?
O1W Co2 O1W 90.0 9 29 ?
O1W Co2 O1W 180.0 5 29 ?
O1W Co2 O1W 90.0 33 25 ?
O1W Co2 O1W 180.0 . 25 ?
O1W Co2 O1W 90.0 9 25 ?
O1W Co2 O1W 90.0 5 25 ?
O1W Co2 O1W 90.0 29 25 ?
N1 C1 C2 123.0(5) . . ?
N1 C1 H1A 118.3 . . ?
C2 C1 H1A 118.7 . . ?
C3 C2 C1 118.9(5) . . ?
C3 C2 H2A 120.7 . . ?
C1 C2 H2A 120.4 . . ?
C2 C3 C4 119.2(5) . . ?
C2 C3 H3A 120.0 . . ?
C4 C3 H3A 120.7 . . ?
C5 C4 C3 118.6(5) . . ?
C5 C4 H4A 120.6 . . ?
C3 C4 H4A 120.8 . . ?
N1 C5 C4 122.2(4) . . ?
N1 C5 C6 115.7(4) . . ?
C4 C5 C6 122.1(4) . . ?
N2 C6 N3 126.8(4) . . ?
N2 C6 C5 116.1(4) . . ?
N3 C6 C5 117.0(4) . . ?
O1 C7 N2 120.9(3) . . ?
O1 C7 N2 120.9(3) . 26 ?
N2 C7 N2 118.3(5) . 26 ?
O2 C8 O3 121.4(6) . 27 ?
O2 C8 O3 121.4(6) . . ?
O3 C8 O3 117.2(13) 27 . ?
C1 N1 C5 118.1(4) . . ?
C1 N1 Co1 126.4(3) . . ?
C5 N1 Co1 115.1(3) . . ?
C6 N2 C7 117.0(4) . . ?
C6 N2 Co1 116.6(3) . . ?
C7 N2 Co1 126.1(3) . . ?
C6 N3 C6 113.7(5) 26 . ?
Co2 O1W H1WA 126.8 . . ?
H2WA O2W H2WB 115.4 . . ?
C8 O3 H3B 121.4 . . ?
H3WA O3W H3WB 111.4 . . ?
H3WA O3W H3WC 121.4 . . ?
H3WB O3W H3WC 127.2 . . ?
H4WA O4W H4WB 123.9 . . ?
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 N2 2.138(3) 5 ?
Co1 N2 2.138(3) 9 ?
Co1 N2 2.138(3) . ?
Co1 N1 2.164(4) 9 ?
Co1 N1 2.164(4) 5 ?
Co1 N1 2.164(4) . ?
Co2 O1W 2.040(7) 33 ?
Co2 O1W 2.040(7) . ?
Co2 O1W 2.040(7) 9 ?
Co2 O1W 2.040(7) 5 ?
Co2 O1W 2.040(7) 29 ?
Co2 O1W 2.040(7) 25 ?
C1 N1 1.334(6) . ?
C1 C2 1.382(7) . ?
C1 H1A 0.9598 . ?
C2 C3 1.351(8) . ?
C2 H2A 0.9593 . ?
C3 C4 1.397(7) . ?
C3 H3A 0.9593 . ?
C4 C5 1.380(7) . ?
C4 H4A 0.9602 . ?
C5 N1 1.336(6) . ?
C5 C6 1.488(6) . ?
C6 N2 1.318(5) . ?
C6 N3 1.327(5) . ?
C7 O1 1.227(7) . ?
C7 N2 1.393(5) . ?
C7 N2 1.393(5) 26 ?
C8 O2 1.228(14) . ?
C8 O3 1.261(9) 27 ?
C8 O3 1.261(9) . ?
N3 C6 1.327(5) 26 ?
O1W H1WA 0.8322 . ?
O2W H2WA 0.8927 . ?
O2W H2WB 0.8501 . ?
O3 H3B 0.8570 . ?
O3W H3WA 0.8499 . ?
O3W H3WB 0.8044 . ?
O3W H3WC 0.9218 . ?
O4W H4WA 0.8790 . ?
O4W H4WB 0.8234 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3B O3 0.86 1.75 2.606(15) 180.0 3_556
O3W H3WA O3 0.85 1.82 2.663(11) 170.5 .
O1W H1WA O1 0.83 1.86 2.691(6) 179.6 .
O2W H2WA O2 0.89 1.63 2.521(17) 180.0 .
O2W H2WB O3W 0.85 1.87 2.709(13) 170.7 45
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 0.1(9) . . . . ?
C1 C2 C3 C4 0.5(9) . . . . ?
C2 C3 C4 C5 -0.7(9) . . . . ?
C3 C4 C5 N1 0.2(8) . . . . ?
C3 C4 C5 C6 -178.1(5) . . . . ?
N1 C5 C6 N2 4.7(6) . . . . ?
C4 C5 C6 N2 -176.9(5) . . . . ?
N1 C5 C6 N3 -172.0(5) . . . . ?
C4 C5 C6 N3 6.5(7) . . . . ?
C2 C1 N1 C5 -0.6(8) . . . . ?
C2 C1 N1 Co1 -172.5(4) . . . . ?
C4 C5 N1 C1 0.5(7) . . . . ?
C6 C5 N1 C1 178.9(4) . . . . ?
C4 C5 N1 Co1 173.3(4) . . . . ?
C6 C5 N1 Co1 -8.3(5) . . . . ?
N2 Co1 N1 C1 71.5(4) 5 . . . ?
N2 Co1 N1 C1 -83.2(10) 9 . . . ?
N2 Co1 N1 C1 179.0(4) . . . . ?
N1 Co1 N1 C1 -99.1(3) 9 . . . ?
N1 Co1 N1 C1 -3.7(4) 5 . . . ?
N2 Co1 N1 C5 -100.6(3) 5 . . . ?
N2 Co1 N1 C5 104.6(9) 9 . . . ?
N2 Co1 N1 C5 6.8(3) . . . . ?
N1 Co1 N1 C5 88.8(4) 9 . . . ?
N1 Co1 N1 C5 -175.8(3) 5 . . . ?
N3 C6 N2 C7 2.7(7) . . . . ?
C5 C6 N2 C7 -173.6(4) . . . . ?
N3 C6 N2 Co1 177.7(4) . . . . ?
C5 C6 N2 Co1 1.4(5) . . . . ?
O1 C7 N2 C6 172.0(5) . . . . ?
N2 C7 N2 C6 -6.5(8) 26 . . . ?
O1 C7 N2 Co1 -2.5(8) . . . . ?
N2 C7 N2 Co1 179.0(2) 26 . . . ?
N2 Co1 N2 C6 74.7(4) 5 . . . ?
N2 Co1 N2 C6 -174.6(3) 9 . . . ?
N1 Co1 N2 C6 -101.1(3) 9 . . . ?
N1 Co1 N2 C6 -20.6(10) 5 . . . ?
N1 Co1 N2 C6 -4.3(3) . . . . ?
N2 Co1 N2 C7 -110.8(3) 5 . . . ?
N2 Co1 N2 C7 -0.1(4) 9 . . . ?
N1 Co1 N2 C7 73.4(4) 9 . . . ?
N1 Co1 N2 C7 153.9(8) 5 . . . ?
N1 Co1 N2 C7 170.2(4) . . . . ?
N2 C6 N3 C6 1.2(9) . . . 26 ?
C5 C6 N3 C6 177.4(3) . . . 26 ?
