#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/84/7218418.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_7218418
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         'C44 H64 Co4 O20, 2(H2 O) '
_chemical_formula_sum            'C44 H68 Co4 O22'
_chemical_formula_weight         1184.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           130
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c c :2'
_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            4
_cell_length_a                   17.0166(4)
_cell_length_b                   17.0166(4)
_cell_length_c                   18.7995(8)
_cell_measurement_reflns_used    3915
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      3.935
_cell_volume                     5443.7(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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_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     0.0238
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12303
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.89
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.271
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.340
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         2432
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1260P)²+10.4802P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1788
_refine_ls_wR_factor_ref         0.2013
_reflns_number_gt                1872
_reflns_number_total             2432
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra09687h2.cif
_cod_data_source_block           co
_cod_original_sg_symbol_Hall     ' -P 4a 2ac '
_cod_original_sg_symbol_H-M      'P 4/n c c'
_cod_database_code               7218418
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/2, x, z'
'x+1/2, -y, -z+1/2'
'-x+1/2, -y+1/2, z'
'-y, -x, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'y, -x+1/2, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'y-1/2, -x, -z'
'-x-1/2, y, z-1/2'
'x-1/2, y-1/2, -z'
'y, x, z-1/2'
'-y-1/2, -x-1/2, z-1/2'
'-y, x-1/2, -z'
'x, -y-1/2, z-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
Co1 Co 0.71772(4) 1.16191(4) 0.55610(3) 0.0406(3) Uani 1 1 d U
O4 O 0.6747(2) 1.27509(18) 0.55375(16) 0.0398(8) Uani 1 1 d .
O2 O 0.7053(2) 1.1503(2) 0.6651(2) 0.0584(10) Uani 1 1 d .
O1 O 0.7740(2) 1.0564(2) 0.55574(16) 0.0475(8) Uani 1 1 d .
O3 O 0.8470(2) 0.9256(2) 0.5239(2) 0.0666(11) Uani 1 1 d .
O5 O 0.6003(2) 1.1160(3) 0.5449(2) 0.0628(10) Uani 1 1 d U
H5B H 0.5728 1.1388 0.5075 0.094 Uiso 1 1 calc R
C1 C 0.7854(3) 1.0083(3) 0.6072(3) 0.0451(11) Uani 1 1 d .
C6 C 0.7603(3) 1.0211(3) 0.6788(3) 0.0533(13) Uani 1 1 d .
C8 C 0.8791(5) 0.8515(4) 0.5039(4) 0.094(2) Uani 1 1 d .
H8A H 0.8442 0.8094 0.5186 0.112 Uiso 1 1 calc R
H8B H 0.9296 0.8437 0.5266 0.112 Uiso 1 1 calc R
C7 C 0.7221(3) 1.0919(3) 0.7013(3) 0.0573(14) Uani 1 1 d .
H7A H 0.7081 1.0943 0.7490 0.069 Uiso 1 1 calc R
C2 C 0.8255(3) 0.9353(3) 0.5933(3) 0.0510(12) Uani 1 1 d .
C5 C 0.7740(4) 0.9633(4) 0.7316(3) 0.0663(16) Uani 1 1 d .
H5A H 0.7564 0.9719 0.7778 0.080 Uiso 1 1 calc R
C10 C 0.6131(3) 1.2982(3) 0.6001(3) 0.0568(14) Uani 1 1 d .
H10A H 0.6004 1.3524 0.5918 0.085 Uiso 1 1 calc R
H10B H 0.6296 1.2914 0.6485 0.085 Uiso 1 1 calc R
H10C H 0.5676 1.2663 0.5912 0.085 Uiso 1 1 calc R
C3 C 0.8383(4) 0.8821(3) 0.6461(3) 0.0627(15) Uani 1 1 d .
H3A H 0.8651 0.8358 0.6357 0.075 Uiso 1 1 calc R
C4 C 0.8122(4) 0.8954(4) 0.7158(3) 0.0706(17) Uani 1 1 d .
H4A H 0.8210 0.8580 0.7509 0.085 Uiso 1 1 calc R
C9 C 0.8884(7) 0.8510(6) 0.4245(5) 0.126(4) Uani 1 1 d .
H9A H 0.9096 0.8014 0.4097 0.190 Uiso 1 1 calc R
H9B H 0.9235 0.8925 0.4106 0.190 Uiso 1 1 calc R
H9C H 0.8381 0.8589 0.4025 0.190 Uiso 1 1 calc R
O6 O 0.4904(16) 0.9904(16) 0.7500 0.466(19) Uani 1 2 d S
H6 H 0.5000 1.0180 0.7147 0.699 Uiso 0.50 1 d PR
H6A H 0.4563 0.9563 0.7500 0.699 Uiso 1 2 d SR
C11 C 0.5583(7) 1.0622(8) 0.5798(9) 0.172(5) Uani 1 1 d U
H11A H 0.5076 1.0570 0.5579 0.258 Uiso 1 1 calc R
H11B H 0.5520 1.0782 0.6284 0.258 Uiso 1 1 calc R
H11C H 0.5851 1.0126 0.5781 0.258 Uiso 1 1 calc R
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'
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 O4 172.62(14) . .
O1 Co1 O2 88.11(13) . .
O4 Co1 O2 94.25(13) . .
O1 Co1 O4 93.50(13) . 15_766
O4 Co1 O4 84.38(13) . 15_766
O2 Co1 O4 177.48(15) . 15_766
O1 Co1 O4 92.27(13) . 4_675
O4 Co1 O4 80.45(15) . 4_675
O2 Co1 O4 99.01(15) . 4_675
O4 Co1 O4 82.87(13) 15_766 4_675
O1 Co1 O5 96.67(16) . .
O4 Co1 O5 90.41(15) . .
O2 Co1 O5 88.15(16) . .
O4 Co1 O5 89.74(14) 15_766 .
O4 Co1 O5 168.73(14) 4_675 .
C10 O4 Co1 120.6(3) . .
C10 O4 Co1 121.1(3) . 10_576
Co1 O4 Co1 96.51(13) . 10_576
C10 O4 Co1 119.0(3) . 4_675
Co1 O4 Co1 99.49(14) . 4_675
Co1 O4 Co1 94.65(13) 10_576 4_675
C7 O2 Co1 126.7(4) . .
C1 O1 Co1 129.2(3) . .
C2 O3 C8 117.5(5) . .
C11 O5 Co1 134.2(6) . .
C11 O5 H5B 112.9 . .
Co1 O5 H5B 112.9 . .
O1 C1 C6 124.5(4) . .
O1 C1 C2 119.0(4) . .
C6 C1 C2 116.4(4) . .
C5 C6 C1 120.3(5) . .
C5 C6 C7 116.9(5) . .
C1 C6 C7 122.8(5) . .
O3 C8 C9 107.9(6) . .
O3 C8 H8A 110.1 . .
C9 C8 H8A 110.1 . .
O3 C8 H8B 110.1 . .
C9 C8 H8B 110.1 . .
H8A C8 H8B 108.4 . .
O2 C7 C6 128.2(5) . .
O2 C7 H7A 115.9 . .
C6 C7 H7A 115.9 . .
C3 C2 O3 125.0(5) . .
C3 C2 C1 121.1(5) . .
O3 C2 C1 113.9(4) . .
C4 C5 C6 121.0(5) . .
C4 C5 H5A 119.5 . .
C6 C5 H5A 119.5 . .
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 . .
C2 C3 C4 121.6(5) . .
C2 C3 H3A 119.2 . .
C4 C3 H3A 119.2 . .
C5 C4 C3 119.6(5) . .
C5 C4 H4A 120.2 . .
C3 C4 H4A 120.2 . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
H6 O6 H6A 122.6 . .
O5 C11 H11A 109.5 . .
O5 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
O5 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O1 2.034(3) .
Co1 O4 2.061(3) .
Co1 O2 2.069(4) .
Co1 O4 2.080(3) 15_766
Co1 O4 2.122(3) 4_675
Co1 O5 2.156(4) .
O4 C10 1.418(6) .
O4 Co1 2.080(3) 10_576
O4 Co1 2.122(3) 4_675
O2 C7 1.237(6) .
O1 C1 1.283(6) .
O3 C2 1.365(7) .
O3 C8 1.424(7) .
O5 C11 1.334(11) .
O5 H5B 0.9300 .
C1 C6 1.429(7) .
C1 C2 1.440(7) .
C6 C5 1.417(7) .
C6 C7 1.433(8) .
C8 C9 1.501(11) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C7 H7A 0.9300 .
C2 C3 1.362(8) .
C5 C4 1.360(8) .
C5 H5A 0.9300 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C3 C4 1.401(9) .
C3 H3A 0.9300 .
C4 H4A 0.9300 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
O6 H6 0.8293 .
O6 H6A 0.8209 .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
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
O5 H5B O1 0.93 1.92 2.764(5) 149.7 10_576
O5 H5B O3 0.93 2.58 3.302(6) 134.3 10_576
