#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:41:59 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180515 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/84/7218417.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_7218417
loop_
_publ_author_name
'zhang, shu hua'
'Zhao, Ru-Xiao'
'li, gui'
'ZHANG, hai yang'
'Zhang, Chun Lian'
'Muller, Gilles'
_publ_section_title
;
 Structural Variation from Heterometallic Heptanuclear, Heptanuclear to
 Cubane Clusters Based on 2-hydroxy-3-ethoxy-benzaldehyde: Effects of pH
 and Temperature
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA09687H
_journal_year                    2014
_chemical_formula_moiety         'C60 H72 Co7 O24, 2(Cl O4)'
_chemical_formula_sum            'C60 H72 Cl2 Co7 O32'
_chemical_formula_weight         1788.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           147
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -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                120.00
_cell_formula_units_Z            1
_cell_length_a                   14.8180(11)
_cell_length_b                   14.8180(11)
_cell_length_c                   9.3912(11)
_cell_measurement_reflns_used    1397
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      3.496
_cell_volume                     1785.8(3)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_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_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova (Mo) X-ray Source'
_diffrn_measurement_method       'ω 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  0.0296
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3653
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.17
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.747
_exptl_absorpt_correction_T_max  0.811
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             911
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.187
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2108
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0566
_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)+(0.0679P)²+5.3753P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1464
_refine_ls_wR_factor_ref         0.1657
_reflns_number_gt                1602
_reflns_number_total             2108
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra09687h2.cif
_cod_data_source_block           co5
_cod_original_cell_volume        1785.8(4)
_cod_database_code               7218417
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
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
C1 C 0.0700(4) 0.3239(4) 0.2915(6) 0.0416(13) Uani 1 1 d .
C2 C 0.1753(5) 0.3851(5) 0.2505(6) 0.0504(14) Uani 1 1 d .
C3 C 0.2022(6) 0.4486(6) 0.1321(7) 0.070(2) Uani 1 1 d .
H3A H 0.2717 0.4881 0.1053 0.085 Uiso 1 1 calc R
C4 C 0.1266(7) 0.4538(7) 0.0536(8) 0.081(2) Uani 1 1 d .
H4A H 0.1455 0.4971 -0.0257 0.097 Uiso 1 1 calc R
C5 C 0.0246(6) 0.3965(6) 0.0908(7) 0.069(2) Uani 1 1 d .
H5A H -0.0254 0.4011 0.0367 0.083 Uiso 1 1 calc R
C6 C -0.0064(5) 0.3300(5) 0.2100(6) 0.0476(14) Uani 1 1 d .
C7 C -0.1156(5) 0.2741(5) 0.2436(6) 0.0520(15) Uani 1 1 d .
H7A H -0.1591 0.2878 0.1875 0.062 Uiso 1 1 calc R
C8 C 0.3546(6) 0.4325(7) 0.3239(10) 0.095(3) Uani 1 1 d DU
H8A H 0.3743 0.4398 0.2243 0.142 Uiso 1 1 calc R
H8B H 0.3870 0.3983 0.3728 0.142 Uiso 1 1 calc R
C9 C 0.3903(10) 0.5365(9) 0.3872(13) 0.162(5) Uani 1 1 d DU
H9B H 0.4643 0.5791 0.3753 0.243 Uiso 1 1 calc R
H9C H 0.3736 0.5290 0.4868 0.243 Uiso 1 1 calc R
H9D H 0.3561 0.5689 0.3405 0.243 Uiso 1 1 calc R
C10 C 0.1418(6) 0.1305(7) 0.2311(9) 0.084(2) Uani 1 1 d .
H10A H 0.2092 0.1881 0.2080 0.126 Uiso 1 1 calc R
H10B H 0.0888 0.1442 0.1971 0.126 Uiso 1 1 calc R
H10C H 0.1335 0.0684 0.1869 0.126 Uiso 1 1 calc R
Cl1 Cl 0.6667 0.3333 0.2506(4) 0.0647(8) Uani 1 3 d S
Co1 Co 0.15315(5) 0.24290(5) 0.51373(8) 0.0396(3) Uani 1 1 d .
Co2 Co 0.0000 0.0000 0.5000 0.0472(5) Uani 1 6 d S
O1 O 0.0482(3) 0.2659(3) 0.4065(4) 0.0445(9) Uani 1 1 d .
O2 O -0.1591(4) 0.2062(4) 0.3447(5) 0.0714(13) Uani 1 1 d .
O3 O 0.2420(3) 0.3707(3) 0.3373(5) 0.0586(12) Uani 1 1 d U
O4 O 0.1324(3) 0.1160(3) 0.3881(5) 0.0441(10) Uani 1 1 d .
O5 O 0.5868(4) 0.3516(4) 0.2950(7) 0.0935(19) Uani 1 1 d .
O6 O 0.6667 0.3333 0.0965(12) 0.129(5) Uani 1 3 d S
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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 C1 C6 123.0(5) . .
O1 C1 C2 118.4(5) . .
C6 C1 C2 118.5(5) . .
O3 C2 C3 126.7(6) . .
O3 C2 C1 112.8(5) . .
C3 C2 C1 120.5(6) . .
C4 C3 C2 120.3(7) . .
C4 C3 H3A 119.8 . .
C2 C3 H3A 119.8 . .
C5 C4 C3 120.6(7) . .
C5 C4 H4A 119.7 . .
C3 C4 H4A 119.7 . .
C4 C5 C6 121.0(7) . .
C4 C5 H5A 119.5 . .
C6 C5 H5A 119.5 . .
C1 C6 C5 119.1(6) . .
C1 C6 C7 123.6(5) . .
C5 C6 C7 117.3(6) . .
O2 C7 C6 126.1(5) . .
O2 C7 H7A 117.0 . .
C6 C7 H7A 117.0 . .
O3 C8 C9 108.8(8) . .
O3 C8 H8A 109.9 . .
C9 C8 H8A 109.9 . .
O3 C8 H8B 109.9 . .
C9 C8 H8B 109.9 . .
H8A C8 H8B 108.3 . .
C8 C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C8 C9 H9D 109.5 . .
H9B C9 H9D 109.5 . .
H9C C9 H9D 109.5 . .
O4 C10 H10A 109.5 . .
O4 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
O4 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
O5 Cl1 O5 111.6(3) 2_655 3_665
O5 Cl1 O5 111.6(3) 2_655 .
O5 Cl1 O5 111.6(3) 3_665 .
O5 Cl1 O6 107.3(3) 2_655 .
O5 Cl1 O6 107.3(3) 3_665 .
O5 Cl1 O6 107.3(3) . .
O1 Co1 O1 171.78(9) . 5_556
O1 Co1 O2 99.20(18) . 5_556
O1 Co1 O2 86.37(17) 5_556 5_556
O1 Co1 O4 79.90(15) . 6_556
O1 Co1 O4 105.04(16) 5_556 6_556
O2 Co1 O4 101.54(18) 5_556 6_556
O1 Co1 O4 95.19(16) . .
O1 Co1 O4 79.00(14) 5_556 .
O2 Co1 O4 165.28(17) 5_556 .
O4 Co1 O4 84.0(2) 6_556 .
O1 Co1 O3 71.49(14) . .
O1 Co1 O3 103.06(15) 5_556 .
O2 Co1 O3 86.12(18) 5_556 .
O4 Co1 O3 151.24(15) 6_556 .
O4 Co1 O3 95.56(16) . .
O4 Co2 O4 82.26(14) 5_556 3
O4 Co2 O4 97.74(14) 5_556 6_556
O4 Co2 O4 180.00(17) 3 6_556
O4 Co2 O4 82.26(14) 5_556 .
O4 Co2 O4 97.74(14) 3 .
O4 Co2 O4 82.26(14) 6_556 .
O4 Co2 O4 97.74(14) 5_556 4_556
O4 Co2 O4 82.26(14) 3 4_556
O4 Co2 O4 97.74(14) 6_556 4_556
O4 Co2 O4 180.00(18) . 4_556
O4 Co2 O4 180.00(11) 5_556 2
O4 Co2 O4 97.74(14) 3 2
O4 Co2 O4 82.26(14) 6_556 2
O4 Co2 O4 97.74(14) . 2
O4 Co2 O4 82.26(14) 4_556 2
C1 O1 Co1 124.1(3) . .
C1 O1 Co1 131.2(3) . 6_556
Co1 O1 Co1 102.72(16) . 6_556
C7 O2 Co1 128.2(4) . 6_556
C2 O3 C8 122.5(6) . .
C2 O3 Co1 112.6(3) . .
C8 O3 Co1 124.8(5) . .
C10 O4 Co1 116.2(4) . 5_556
C10 O4 Co1 117.7(4) . .
Co1 O4 Co1 98.13(16) 5_556 .
C10 O4 Co2 126.0(4) . .
Co1 O4 Co2 97.14(16) 5_556 .
Co1 O4 Co2 96.23(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.315(6) .
C1 C6 1.407(8) .
C1 C2 1.411(8) .
C2 O3 1.378(7) .
C2 C3 1.381(9) .
C3 C4 1.374(10) .
C3 H3A 0.9300 .
C4 C5 1.358(10) .
C4 H4A 0.9300 .
C5 C6 1.408(8) .
C5 H5A 0.9300 .
C6 C7 1.436(8) .
C7 O2 1.297(7) .
C7 H7A 0.9300 .
C8 O3 1.452(8) .
C8 C9 1.481(9) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C9 H9D 0.9600 .
C10 O4 1.486(9) .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
Cl1 O5 1.402(5) 2_655
Cl1 O5 1.402(5) 3_665
Cl1 O5 1.402(5) .
Cl1 O6 1.447(11) .
Co1 O1 2.021(4) .
Co1 O1 2.029(4) 5_556
Co1 O2 2.062(5) 5_556
Co1 O4 2.078(4) 6_556
Co1 O4 2.108(4) .
Co1 O3 2.360(4) .
Co2 O4 2.129(4) 5_556
Co2 O4 2.129(4) 3
Co2 O4 2.129(4) 6_556
Co2 O4 2.129(4) .
Co2 O4 2.129(4) 4_556
Co2 O4 2.129(4) 2
O1 Co1 2.029(4) 6_556
O2 Co1 2.062(5) 6_556
O4 Co1 2.078(4) 5_556
