#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:38:45 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180149 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/46/7104638.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_7104638
loop_
_publ_author_name
'Livage, Carine'
'Guillou, Nathalie'
'Rabu, Pierre'
'Pattison, Philip'
'Marrot, Jérôme'
'Férey, Gérard'
_publ_section_title
;
 Bulk homochirality of a 3-D inorganic framework: ligand control of
 inorganic network chirality.
;
_journal_issue                   30
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4551
_journal_page_last               4553
_journal_paper_doi               10.1039/b904622d
_journal_volume                  34
_journal_year                    2009
_chemical_absolute_configuration '80% right 20% left'
_chemical_formula_moiety         'C30 H52 Co5 O26'
_chemical_formula_sum            'C30 H52 Co5 O26'
_chemical_formula_weight         1123.37
_chemical_name_common
'Diaqua penta 2-methylglutarate cobalt (ii) hydrate'
_chemical_name_systematic
;
Diaqua penta 2-methylglutarate cobalt (II) hydrate
;
_space_group_IT_number           213
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P 4bd 2ab 3'
_symmetry_space_group_name_H-M   'P 41 3 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                   16.6130(1)
_cell_length_b                   16.6130(1)
_cell_length_c                   16.6130(1)
_cell_measurement_reflns_used    1561
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.87
_cell_measurement_theta_min      1.71
_cell_volume                     4585.05(5)
_computing_data_reduction        'CrysAlis software package'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  MAR345
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_source         'BM01 at ESFR, Grenoble France'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.70000
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0146
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21639
_diffrn_reflns_theta_full        25.87
_diffrn_reflns_theta_max         25.87
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    1.856
_exptl_absorpt_correction_T_max  0.9817
_exptl_absorpt_correction_T_min  0.9817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, V2.10)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             2300
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.20(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         1561
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0369
_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)+(0.0650P)²+12.7165P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1240
_reflns_number_gt                1557
_reflns_number_total             1561
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b904622d.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      P4(1)32
_cod_database_code               7104638
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'z, x, y'
'y, z, x'
'-z+1/2, -x, y+1/2'
'-y, z+1/2, -x+1/2'
'z+1/2, -x+1/2, -y'
'-y+1/2, -z, x+1/2'
'-z, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x'
'-y+3/4, -x+3/4, -z+3/4'
'y+3/4, x+1/4, -z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'-x+3/4, -z+3/4, -y+3/4'
'-z+3/4, -y+3/4, -x+3/4'
'x+3/4, z+1/4, -y+1/4'
'-z+1/4, y+3/4, x+1/4'
'x+1/4, -z+1/4, y+3/4'
'z+3/4, y+1/4, -x+1/4'
'-x+1/4, z+3/4, y+1/4'
'z+1/4, -y+1/4, x+3/4'
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 0.19647(3) 0.19647(3) 0.19647(3) 0.0143(3) Uani 1 3 d S . .
Co2 Co 0.32441(4) 0.1250 0.07441(4) 0.0159(2) Uani 1 2 d S . .
O1 O 0.21110(17) 0.18436(18) 0.07028(18) 0.0175(6) Uani 1 1 d . . .
O2 O 0.1229(2) 0.2744(2) 0.02424(19) 0.0233(7) Uani 1 1 d . . .
O3 O 0.18267(19) 0.18752(18) 0.32056(18) 0.0204(6) Uani 1 1 d . . .
O4 O 0.2706(3) 0.2693(4) 0.3696(4) 0.0352(13) Uani 0.67 1 d P . .
C1 C 0.1768(3) 0.2229(3) 0.0135(2) 0.0171(8) Uani 1 1 d . . .
C2 C 0.1977(3) 0.2020(3) -0.0721(3) 0.0241(9) Uani 1 1 d . . .
H2 H 0.2558 0.1926 -0.0761 0.029 Uiso 1 1 calc R . .
C3 C 0.1524(3) 0.1250 -0.0976(3) 0.0270(15) Uani 1 2 d S . .
H3A H 0.1608 0.1166 -0.1547 0.032 Uiso 0.50 1 calc PR . .
H3B H 0.0953 0.1334 -0.0892 0.032 Uiso 0.50 1 calc PR . .
C4 C 0.1742(7) 0.2711(7) -0.1289(6) 0.037(3) Uani 0.50 1 d P . .
H4A H 0.1168 0.2781 -0.1279 0.055 Uiso 0.50 1 calc PR . .
H4B H 0.1911 0.2584 -0.1827 0.055 Uiso 0.50 1 calc PR . .
H4C H 0.1999 0.3198 -0.1116 0.055 Uiso 0.50 1 calc PR . .
C5 C 0.2032(9) 0.2381(8) 0.3705(6) 0.078(5) Uani 0.67 1 d P . .
C6 C 0.2043(6) 0.2145(4) 0.4599(4) 0.059(3) Uani 0.67 1 d P . .
H6 H 0.2051 0.1557 0.4650 0.070 Uiso 0.67 1 calc PR . .
C7 C 0.1250(6) 0.2487(4) 0.4987(4) 0.057(4) Uani 0.67 2 d SPR . .
H7A H 0.1231 0.3064 0.4898 0.069 Uiso 0.33 1 calc PR . .
H7B H 0.1269 0.2398 0.5564 0.069 Uiso 0.33 1 calc PR . .
C8 C 0.2703(6) 0.2481(4) 0.5027(4) 0.077(8) Uani 0.33 1 d PR . .
H8A H 0.3188 0.2404 0.4723 0.116 Uiso 0.33 1 calc PR . .
H8B H 0.2754 0.2219 0.5540 0.116 Uiso 0.33 1 calc PR . .
H8C H 0.2614 0.3046 0.5107 0.116 Uiso 0.33 1 calc PR . .
OW1 O 0.2007(6) 0.3159(4) 0.3494(4) 0.071(6) Uani 0.33 1 d PR . .
OW2 O 0.3807(6) 0.4478(4) 0.6607(4) 0.077(12) Uani 0.17 1 d PR . .
OW3 O 0.3456(6) 0.3507(4) 0.4320(4) 0.119(18) Uiso 0.17 1 d PR . .
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
_geom_angle_publ_flag
O3 Co1 O3 99.93(11) 6 . ?
O3 Co1 O3 99.93(11) 6 5 ?
O3 Co1 O3 99.93(11) . 5 ?
O3 Co1 O1 78.77(11) 6 5 ?
O3 Co1 O1 89.61(12) . 5 ?
O3 Co1 O1 170.45(12) 5 5 ?
O3 Co1 O1 170.45(12) 6 6 ?
O3 Co1 O1 78.77(11) . 6 ?
O3 Co1 O1 89.61(12) 5 6 ?
O1 Co1 O1 91.74(12) 5 6 ?
O3 Co1 O1 89.61(12) 6 . ?
O3 Co1 O1 170.45(12) . . ?
O3 Co1 O1 78.77(11) 5 . ?
O1 Co1 O1 91.74(12) 5 . ?
O1 Co1 O1 91.74(12) 6 . ?
O2 Co2 O2 179.0(2) 21_554 6 ?
O2 Co2 O3 90.12(13) 21_554 5 ?
O2 Co2 O3 90.47(14) 6 5 ?
O2 Co2 O3 90.47(14) 21_554 15_554 ?
O2 Co2 O3 90.12(13) 6 15_554 ?
O3 Co2 O3 105.07(16) 5 15_554 ?
O2 Co2 O1 91.89(13) 21_554 24_554 ?
O2 Co2 O1 87.49(13) 6 24_554 ?
O3 Co2 O1 176.36(12) 5 24_554 ?
O3 Co2 O1 77.95(11) 15_554 24_554 ?
O2 Co2 O1 87.49(13) 21_554 . ?
O2 Co2 O1 91.89(13) 6 . ?
O3 Co2 O1 77.95(11) 5 . ?
O3 Co2 O1 176.36(12) 15_554 . ?
O1 Co2 O1 99.09(16) 24_554 . ?
C1 O1 Co1 129.3(3) . . ?
C1 O1 Co2 130.8(3) . . ?
Co1 O1 Co2 96.52(12) . . ?
C1 O2 Co2 132.9(3) . 5 ?
C5 O3 Co1 126.1(6) . . ?
C5 O3 Co2 135.6(6) . 6 ?
Co1 O3 Co2 98.27(13) . 6 ?
C5 O4 OW1 59.7(9) . . ?
O2 C1 O1 123.9(4) . . ?
O2 C1 C2 117.3(4) . . ?
O1 C1 C2 118.7(4) . . ?
C1 C2 C4 110.5(5) . . ?
C1 C2 C3 109.7(3) . . ?
C4 C2 C3 109.1(6) . . ?
C1 C2 H2 109.2 . . ?
C4 C2 H2 109.2 . . ?
C3 C2 H2 109.2 . . ?
C2 C3 C2 114.9(5) . 24_554 ?
C2 C3 H3A 108.5 . . ?
C2 C3 H3A 108.5 24_554 . ?
C2 C3 H3B 108.5 . . ?
C2 C3 H3B 108.5 24_554 . ?
H3A C3 H3B 107.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O3 C5 O4 122.1(11) . . ?
O3 C5 OW1 118.3(11) . . ?
O4 C5 OW1 67.7(7) . . ?
O3 C5 C6 118.8(9) . . ?
O4 C5 C6 96.2(10) . . ?
OW1 C5 C6 119.9(8) . . ?
C8 C6 C5 113.1(5) . . ?
C8 C6 C7 107.5 . . ?
C5 C6 C7 107.2(7) . . ?
C8 C6 H6 109.7 . . ?
C5 C6 H6 109.7 . . ?
C7 C6 H6 109.7 . . ?
C6 C7 C6 113.9(4) . 23_545 ?
C6 C7 H7A 108.8 . . ?
C6 C7 H7A 108.8 23_545 . ?
C6 C7 H7B 108.8 . . ?
C6 C7 H7B 108.8 23_545 . ?
H7A C7 H7B 107.7 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 OW1 O4 52.6(7) . . ?
OW3 OW3 OW3 119.68(13) 18 17 ?
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 O3 2.079(3) 6 ?
Co1 O3 2.079(3) . ?
Co1 O3 2.079(3) 5 ?
Co1 O1 2.120(3) 5 ?
Co1 O1 2.120(3) 6 ?
Co1 O1 2.120(3) . ?
Co2 O2 2.035(3) 21_554 ?
Co2 O2 2.035(3) 6 ?
Co2 O3 2.110(3) 5 ?
Co2 O3 2.110(3) 15_554 ?
Co2 O1 2.126(3) 24_554 ?
Co2 O1 2.126(3) . ?
O1 C1 1.276(5) . ?
O2 C1 1.250(5) . ?
O2 Co2 2.035(3) 5 ?
O3 C5 1.228(10) . ?
O3 Co2 2.110(3) 6 ?
O4 C5 1.234(13) . ?
O4 OW1 1.436(11) . ?
C1 C2 1.505(6) . ?
C2 C4 1.535(11) . ?
C2 C3 1.543(6) . ?
C2 H2 0.9800 . ?
C3 C2 1.543(6) 24_554 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 OW1 1.341(16) . ?
C5 C6 1.537(13) . ?
C6 C8 1.4212 . ?
C6 C7 1.5721 . ?
C6 H6 0.9800 . ?
C7 C6 1.572(15) 23_545 ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
OW3 OW3 1.035(18) 18 ?
OW3 OW3 1.243(17) 17 ?
