#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:22:30 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180335 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/04/7200425.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_7200425
loop_
_publ_author_name
'Shu-Hua Zhang'
'You Song'
'Hong Liang'
'Ming-Hua Zeng'
_publ_section_title
;
 Microwave-assisted synthesis, crystal structure and properties of a
 disc-like heptanuclear Co(II) cluster and a heterometallic cubanic
 Co(II) cluster
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              865
_journal_page_last               872
_journal_paper_doi               10.1039/b815675a
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety         '2(C36 H43 Co3 N6 Na O16 S3), (C2 H3 N)'
_chemical_formula_sum            'C74 H89 Co6 N13 Na2 O32 S6'
_chemical_formula_weight         2264.50
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :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            3
_cell_length_a                   17.1568(12)
_cell_length_b                   17.1568(12)
_cell_length_c                   27.247(3)
_cell_measurement_reflns_used    2606
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.87
_cell_measurement_theta_min      2.37
_cell_volume                     6945.8(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  '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  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            10304
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.282
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3480
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.510
_refine_diff_density_min         -1.138
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         2719
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0515
_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)+(0.0952P)²+44.0845P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1455
_refine_ls_wR_factor_ref         0.1732
_reflns_number_gt                1833
_reflns_number_total             2719
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b815675a.txt
_cod_data_source_block           co
_cod_original_cell_volume        6945.9(11)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7200425
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'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'
'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'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-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'
'-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'
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 0.74294(5) 0.28783(5) 0.08484(3) 0.0224(3) Uani 1 1 d . . .
Na1 Na 0.6667 0.3333 0.18674(13) 0.0321(9) Uani 1 3 d S . .
S1 S 0.73787(11) 0.15633(10) -0.00067(6) 0.0354(4) Uani 1 1 d . . .
C1 C 0.8500(5) 0.2425(5) -0.0088(3) 0.0536(19) Uani 1 1 d . . .
H1B H 0.8868 0.2331 0.0148 0.064 Uiso 1 1 calc R . .
H1A H 0.8691 0.2355 -0.0412 0.064 Uiso 1 1 calc R . .
C2 C 0.8703(5) 0.3370(4) -0.0040(2) 0.0429(16) Uani 1 1 d . . .
H2B H 0.9308 0.3768 -0.0160 0.051 Uiso 1 1 calc R . .
H2A H 0.8290 0.3455 -0.0245 0.051 Uiso 1 1 calc R . .
C3 C 0.9327(4) 0.4303(4) 0.0654(2) 0.0326(14) Uani 1 1 d . . .
H3 H 0.9838 0.4583 0.0457 0.039 Uiso 1 1 d R . .
C4 C 0.9395(4) 0.4680(4) 0.1146(2) 0.0311(13) Uani 1 1 d . . .
C5 C 1.0257(4) 0.5225(4) 0.1324(2) 0.0397(15) Uani 1 1 d . . .
H5 H 1.0749 0.5348 0.1129 0.048 Uiso 1 1 calc R . .
C6 C 1.0393(5) 0.5591(5) 0.1791(3) 0.0507(19) Uani 1 1 d . . .
H6 H 1.0974 0.5957 0.1910 0.061 Uiso 1 1 calc R . .
C7 C 0.9657(4) 0.5405(4) 0.2079(2) 0.0441(17) Uani 1 1 d . . .
H7 H 0.9745 0.5655 0.2391 0.053 Uiso 1 1 calc R . .
C8 C 0.8793(4) 0.4852(4) 0.1909(2) 0.0329(14) Uani 1 1 d . . .
C9 C 0.8638(4) 0.4498(3) 0.14299(19) 0.0257(12) Uani 1 1 d . . .
C10 C 0.8126(6) 0.5034(7) 0.2633(3) 0.082(3) Uani 1 1 d U . .
H10A H 0.8432 0.4857 0.2864 0.124 Uiso 1 1 calc R . .
H10B H 0.7545 0.4881 0.2760 0.124 Uiso 1 1 calc R . .
H10C H 0.8473 0.5672 0.2580 0.124 Uiso 1 1 calc R . .
C11 C 0.8667(4) 0.2741(4) 0.1713(2) 0.0351(14) Uani 1 1 d . . .
C12 C 0.9327(5) 0.3042(5) 0.2106(3) 0.0492(18) Uani 1 1 d . . .
H12A H 0.9762 0.3667 0.2060 0.074 Uiso 1 1 calc R . .
H12B H 0.9625 0.2695 0.2102 0.074 Uiso 1 1 calc R . .
H12C H 0.9030 0.2963 0.2415 0.074 Uiso 1 1 calc R . .
C13 C 0.6667 0.3333 0.9449(7) 0.089(6) Uani 0.25 3 d SPDU . .
H13 H 0.7121 0.3780 0.9550 0.133 Uiso 0.25 1 d PR . .
C14 C 0.6667 0.3333 0.9002(6) 0.089(6) Uani 0.25 3 d SPDU . .
C13' C 0.6667 0.3333 0.8555(7) 0.089(6) Uani 0.25 3 d SPD . .
H13' H 0.6446 0.3651 0.8480 0.133 Uiso 0.25 1 d PR . .
C14' C 0.6667 0.3333 0.9002(6) 0.089(6) Uani 0.25 3 d SPD . .
N1 N 0.8635(3) 0.3625(3) 0.04691(17) 0.0287(11) Uani 1 1 d . . .
N2 N 0.8153(4) 0.2519(3) 0.14025(19) 0.0370(13) Uani 1 1 d . . .
N3 N 0.6667 0.3333 0.8496(7) 0.055(4) Uani 0.25 3 d SPDU . .
N3' N 0.6667 0.3333 0.9508(7) 0.055(4) Uani 0.25 3 d SPDU . .
O1 O 0.7794(2) 0.3991(2) 0.12751(13) 0.0226(8) Uani 1 1 d . . .
O2 O 0.8021(3) 0.4577(3) 0.21805(15) 0.0424(11) Uani 1 1 d . . .
O3 O 0.6667 0.3333 0.0493(2) 0.0224(14) Uani 1 3 d S . .
H3A H 0.6667 0.3333 0.0181 0.034 Uiso 1 3 d SR . .
O4 O 0.6851(4) 0.1575(5) -0.04009(19) 0.0793(18) Uani 1 1 d . . .
O5 O 0.7083(3) 0.1719(3) 0.04685(14) 0.0358(10) Uani 1 1 d . . .
O6 O 0.7421(4) 0.0744(4) 0.0005(2) 0.0750(17) Uani 1 1 d U . .
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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
O1 Co1 O5 175.52(15) . . ?
O1 Co1 O3 82.53(14) . . ?
O5 Co1 O3 101.41(16) . . ?
O1 Co1 N1 87.81(16) . . ?
O5 Co1 N1 93.65(17) . . ?
O3 Co1 N1 98.97(16) . . ?
O1 Co1 O1 87.32(19) . 3_665 ?
O5 Co1 O1 91.27(15) . 3_665 ?
O3 Co1 O1 79.63(14) . 3_665 ?
N1 Co1 O1 175.07(16) . 3_665 ?
O1 Co1 N2 85.45(16) . . ?
O5 Co1 N2 90.32(18) . . ?
O3 Co1 N2 165.1(2) . . ?
N1 Co1 N2 89.28(18) . . ?
O1 Co1 N2 91.10(16) 3_665 . ?
O1 Na1 O1 77.35(16) 3_665 . ?
O1 Na1 O1 77.35(16) 3_665 2_655 ?
O1 Na1 O1 77.35(16) . 2_655 ?
O1 Na1 O2 67.33(13) 3_665 3_665 ?
O1 Na1 O2 111.15(14) . 3_665 ?
O1 Na1 O2 139.95(15) 2_655 3_665 ?
O1 Na1 O2 139.95(15) 3_665 . ?
O1 Na1 O2 67.33(13) . . ?
O1 Na1 O2 111.15(14) 2_655 . ?
O2 Na1 O2 108.01(14) 3_665 . ?
O1 Na1 O2 111.15(14) 3_665 2_655 ?
O1 Na1 O2 139.95(15) . 2_655 ?
O1 Na1 O2 67.33(13) 2_655 2_655 ?
O2 Na1 O2 108.01(14) 3_665 2_655 ?
O2 Na1 O2 108.01(14) . 2_655 ?
O1 Na1 Co1 37.53(9) 3_665 3_665 ?
O1 Na1 Co1 79.53(13) . 3_665 ?
O1 Na1 Co1 40.55(9) 2_655 3_665 ?
O2 Na1 Co1 100.76(12) 3_665 3_665 ?
O2 Na1 Co1 141.99(15) . 3_665 ?
O2 Na1 Co1 85.35(12) 2_655 3_665 ?
O1 Na1 Co1 79.53(13) 3_665 2_655 ?
O1 Na1 Co1 40.55(9) . 2_655 ?
O1 Na1 Co1 37.53(9) 2_655 2_655 ?
O2 Na1 Co1 141.99(15) 3_665 2_655 ?
O2 Na1 Co1 85.35(12) . 2_655 ?
O2 Na1 Co1 100.76(11) 2_655 2_655 ?
Co1 Na1 Co1 56.89(6) 3_665 2_655 ?
O4 S1 O6 112.0(4) . . ?
O4 S1 O5 112.8(3) . . ?
O6 S1 O5 110.5(3) . . ?
O4 S1 C1 109.4(4) . . ?
O6 S1 C1 104.7(4) . . ?
O5 S1 C1 107.0(3) . . ?
C2 C1 S1 117.9(5) . . ?
C2 C1 H1B 107.8 . . ?
S1 C1 H1B 107.8 . . ?
C2 C1 H1A 107.8 . . ?
S1 C1 H1A 107.8 . . ?
H1B C1 H1A 107.2 . . ?
N1 C2 C1 113.4(5) . . ?
N1 C2 H2B 108.9 . . ?
C1 C2 H2B 108.9 . . ?
N1 C2 H2A 108.9 . . ?
C1 C2 H2A 108.9 . . ?
H2B C2 H2A 107.7 . . ?
N1 C3 C4 126.4(5) . . ?
N1 C3 H3 116.7 . . ?
C4 C3 H3 116.9 . . ?
C5 C4 C9 120.8(6) . . ?
C5 C4 C3 116.3(5) . . ?
C9 C4 C3 122.9(5) . . ?
C4 C5 C6 120.7(6) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C7 C6 C5 119.2(6) . . ?
C7 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
C8 C7 C6 120.8(6) . . ?
C8 C7 H7 119.6 . . ?
C6 C7 H7 119.6 . . ?
O2 C8 C7 125.0(6) . . ?
O2 C8 C9 114.1(5) . . ?
C7 C8 C9 120.9(6) . . ?
O1 C9 C4 123.6(5) . . ?
O1 C9 C8 119.0(5) . . ?
C4 C9 C8 117.4(5) . . ?
O2 C10 H10A 109.5 . . ?
O2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 C12 178.8(6) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 H13 109.5 . . ?
C13' C14 C13 180.000(17) . . ?
C13' C14 N3' 180.000(8) . . ?
C13 C14 N3' 0.000(6) . . ?
C13' C14 N3 0.000(5) . . ?
C13 C14 N3 180.000(8) . . ?
N3' C14 N3 180.000(8) . . ?
N3 C13' C13' 0.001(5) 16_656 16_656 ?
N3 C13' H13' 75.8 16_656 . ?
C13' C13' H13' 75.8 16_656 . ?
C14 C13' H13' 104.2 . . ?
C3 N1 C2 117.6(5) . . ?
C3 N1 Co1 123.4(4) . . ?
C2 N1 Co1 119.1(4) . . ?
C11 N2 Co1 148.7(5) . . ?
N3 N3 C13' 0.001(6) 16_656 16_656 ?
N3 N3 H13' 87.0 16_656 . ?
C13' N3 H13' 87.0 16_656 . ?
C14 N3 H13' 93.0 . . ?
C14 N3' H13 98.4 . . ?
C9 O1 Co1 120.9(3) . . ?
C9 O1 Co1 121.8(3) . 2_655 ?
Co1 O1 Co1 97.27(14) . 2_655 ?
C9 O1 Na1 117.7(3) . . ?
Co1 O1 Na1 98.57(14) . . ?
Co1 O1 Na1 95.15(14) 2_655 . ?
C8 O2 C10 116.1(5) . . ?
C8 O2 Na1 116.9(3) . . ?
C10 O2 Na1 126.9(5) . . ?
Co1 O3 Co1 99.83(18) . 3_665 ?
Co1 O3 Co1 99.83(18) . 2_655 ?
Co1 O3 Co1 99.83(18) 3_665 2_655 ?
Co1 O3 H3A 117.9 . . ?
Co1 O3 H3A 117.9 3_665 . ?
Co1 O3 H3A 117.9 2_655 . ?
S1 O5 Co1 131.7(3) . . ?
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 2.048(3) . ?
Co1 O5 2.048(4) . ?
Co1 O3 2.070(3) . ?
Co1 N1 2.082(5) . ?
Co1 O1 2.170(3) 3_665 ?
Co1 N2 2.228(5) . ?
Na1 O1 2.331(4) 3_665 ?
Na1 O1 2.331(4) . ?
Na1 O1 2.331(4) 2_655 ?
Na1 O2 2.392(4) 3_665 ?
Na1 O2 2.392(4) . ?
Na1 O2 2.392(4) 2_655 ?
Na1 Co1 3.325(3) 3_665 ?
Na1 Co1 3.325(3) 2_655 ?
S1 O4 1.411(6) . ?
S1 O6 1.444(5) . ?
S1 O5 1.464(4) . ?
S1 C1 1.759(7) . ?
C1 C2 1.484(9) . ?
C1 H1B 0.9700 . ?
C1 H1A 0.9700 . ?
C2 N1 1.478(7) . ?
C2 H2B 0.9700 . ?
C2 H2A 0.9700 . ?
C3 N1 1.279(7) . ?
C3 C4 1.467(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.383(8) . ?
C4 C9 1.407(8) . ?
C5 C6 1.387(9) . ?
C5 H5 0.9300 . ?
C6 C7 1.381(10) . ?
C6 H6 0.9300 . ?
C7 C8 1.380(8) . ?
C7 H7 0.9300 . ?
C8 O2 1.379(7) . ?
C8 C9 1.408(8) . ?
C9 O1 1.332(6) . ?
C10 O2 1.422(8) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N2 1.141(8) . ?
C11 C12 1.453(9) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.218(10) . ?
C13 H13 0.8200 . ?
C14 C13' 1.218(10) . ?
C14 N3' 1.378(10) . ?
C14 N3 1.379(10) . ?
C13' N3 1.05(3) 16_656 ?
C13' C13' 1.21(4) 16_656 ?
C13' H13' 0.8299 . ?
N3 N3 0.89(4) 16_656 ?
N3 C13' 1.05(3) 16_656 ?
N3 H13' 0.8057 . ?
N3' H13 0.7815 . ?
O1 Co1 2.170(3) 2_655 ?
O3 Co1 2.070(3) 3_665 ?
O3 Co1 2.070(3) 2_655 ?
O3 H3A 0.8501 . ?
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
N3' H13 O4 0.78 2.42 3.197(7) 170.7 2_656
O3 H3A N3' 0.85 1.83 2.68(2) 180.0 1_554
