#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:04:30 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180167 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/63/7106345.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_7106345
loop_
_publ_author_name
'Philipp Wollmann'
'Matthias Leistner'
'Ulrich Stoeck'
'Ronny Grunker'
'Kristina Gedrich'
'Nicole Klein'
'Oliver Throl'
'Wulf Grahlert'
'Irena Senkovska'
'Frieder Dreisbach'
'Stefan Kaskel'
_publ_section_title
;
 High-throughput discovery of porous materials
;
_journal_name_full               Chem.Commun.
_journal_page_first              5151
_journal_paper_doi               10.1039/c1cc10674k
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C54 H30 Co3 O14'
_chemical_formula_sum            'C54 H30 Co3 O14'
_chemical_formula_weight         1079.57
_chemical_name_common            Co3O(H2btb)2(H2O)
_chemical_properties_physical    moisture-sensitive
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   17.551(4)
_cell_length_b                   25.356(5)
_cell_length_c                   21.148(4)
_cell_measurement_reflns_used    3199
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.00
_cell_measurement_theta_min      1.88
_cell_volume                     9411(3)
_computing_cell_refinement       XDS
_computing_data_collection       'marCCD 1994-2002'
_computing_data_reduction        XDSCONV
_computing_molecular_graphics    'Diamond 3.1'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007)'
_diffrn_ambient_pressure         100
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.890
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_device_type  'MX-225 CCD'
_diffrn_measurement_method       'Δφ scans'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_wavelength     0.88561
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0208
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            56458
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         31.00
_diffrn_reflns_theta_min         1.88
_diffrn_source                   synchrotron
_diffrn_source_type              'BESSY BL MX-14.2'
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    0.739
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2188
_platon_squeeze_details
;
;
_refine_diff_density_max         1.676
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         7076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0758
_refine_ls_shift/su_max          0.136
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1687P)²+5.1686P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2221
_refine_ls_wR_factor_ref         0.2266
_reflns_number_gt                6506
_reflns_number_total             7076
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc10674k_2.txt
_cod_data_source_block           rg-68-ds1
_cod_database_code               7106345
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co01 Co 0.61277(3) 0.7500 0.66324(2) 0.0191(2) Uani 1 2 d S . .
Co02 Co 0.50325(2) 0.680786(16) 0.56379(2) 0.0289(2) Uani 1 1 d . . .
O7 O 0.60643(14) 0.66042(10) 0.53421(12) 0.0449(6) Uani 1 1 d . . .
O4 O 0.51577(17) 0.7500 0.60699(14) 0.0262(6) Uani 1 2 d S . .
O8 O 0.56122(14) 0.69148(8) 0.71655(9) 0.0365(5) Uani 1 1 d . . .
O5 O 0.70046(19) 0.7500 0.73070(14) 0.0372(7) Uani 1 2 d S . .
O9 O 0.50030(15) 0.63924(11) 0.64716(12) 0.0519(8) Uani 1 1 d . . .
C008 C 0.0793(2) 0.57067(15) 0.45540(18) 0.0461(9) Uani 1 1 d . . .
O6 O 0.67289(14) 0.69265(10) 0.61533(11) 0.0450(6) Uani 1 1 d . . .
C010 C 0.3778(3) 0.64880(19) 0.53052(17) 0.0546(11) Uani 1 1 d . . .
C011 C 0.56250(19) 0.61051(13) 0.80516(16) 0.0384(8) Uani 1 1 d . . .
H011 H 0.5970 0.6379 0.8108 0.046 Uiso 1 1 calc R . .
C012 C 1.00298(19) 0.51048(16) 0.39270(19) 0.0447(10) Uani 1 1 d . . .
C013 C 0.0734(2) 0.53087(16) 0.41032(19) 0.0498(10) Uani 1 1 d . . .
H013 H 0.1174 0.5177 0.3916 0.060 Uiso 1 1 calc R . .
C014 C 0.5180(2) 0.60907(13) 0.75080(17) 0.0389(8) Uani 1 1 d . . .
C015 C 0.8022(2) 0.59229(17) 0.4589(2) 0.0593(12) Uani 1 1 d . . .
H015 H 0.8010 0.5760 0.4195 0.071 Uiso 1 1 calc R . .
C016 C 0.1557(2) 0.59005(16) 0.47470(19) 0.0530(10) Uani 1 1 d . . .
C017 C 0.2999(2) 0.62656(19) 0.51103(19) 0.0576(11) Uani 1 1 d . . .
C018 C 0.5036(2) 0.53185(15) 0.84510(19) 0.0440(10) Uani 1 1 d . . .
C019 C 1.0130(2) 0.59107(16) 0.4819(2) 0.0473(10) Uani 1 1 d . . .
H019 H 1.0165 0.6184 0.5111 0.057 Uiso 1 1 calc R . .
C020 C 0.7370(2) 0.63982(13) 0.54094(16) 0.0386(8) Uani 1 1 d . . .
C021 C 0.4585(2) 0.52969(15) 0.78945(19) 0.0510(10) Uani 1 1 d . . .
H021 H 0.4240 0.5022 0.7836 0.061 Uiso 1 1 calc R . .
C022 C 0.8707(2) 0.59423(14) 0.49270(18) 0.0440(9) Uani 1 1 d . . .
C023 C 0.5273(2) 0.65010(12) 0.70043(15) 0.0345(7) Uani 1 1 d . . .
O3 O 0.37920(19) 0.68598(12) 0.56513(17) 0.0649(9) Uani 1 1 d . . .
C025 C 0.4658(2) 0.56853(14) 0.74389(18) 0.0465(9) Uani 1 1 d . . .
H025 H 0.4351 0.5674 0.7080 0.056 Uiso 1 1 calc R . .
C026 C 0.7358(2) 0.61442(17) 0.48351(19) 0.0532(11) Uani 1 1 d . . .
H026 H 0.6904 0.6120 0.4610 0.064 Uiso 1 1 calc R . .
C027 C 0.5563(2) 0.57196(14) 0.85085(17) 0.0425(8) Uani 1 1 d . . .
H027 H 0.5880 0.5730 0.8860 0.051 Uiso 1 1 calc R . .
C028 C 0.6658(2) 0.66609(13) 0.56625(14) 0.0333(8) Uani 1 1 d . . .
C029 C 0.9413(2) 0.57136(15) 0.46556(19) 0.0454(9) Uani 1 1 d . . .
C030 C 0.8707(2) 0.61905(16) 0.55119(18) 0.0479(10) Uani 1 1 d . . .
H030 H 0.9154 0.6203 0.5747 0.057 Uiso 1 1 calc R . .
C031 C 0.8050(2) 0.64209(15) 0.57507(17) 0.0458(9) Uani 1 1 d . . .
H031 H 0.8063 0.6591 0.6140 0.055 Uiso 1 1 calc R . .
C033 C 0.2367(3) 0.65651(18) 0.5179(3) 0.0680(13) Uani 1 1 d . . .
H033 H 0.2409 0.6896 0.5365 0.082 Uiso 1 1 calc R . .
C035 C 0.9371(2) 0.53058(15) 0.42172(19) 0.0462(9) Uani 1 1 d . . .
H035 H 0.8899 0.5164 0.4114 0.055 Uiso 1 1 calc R . .
O1 O 0.4351(2) 0.6249(2) 0.51169(18) 0.1037(16) Uani 1 1 d . . .
C037 C 0.1677(2) 0.63973(18) 0.4985(3) 0.0694(14) Uani 1 1 d . . .
H037 H 0.1266 0.6627 0.5014 0.083 Uiso 1 1 calc R . .
C038 C 0.2178(3) 0.5552(2) 0.4759(3) 0.099(2) Uani 1 1 d . . .
H038 H 0.2109 0.5196 0.4667 0.119 Uiso 1 1 calc R . .
C039 C 0.2883(3) 0.5739(3) 0.4907(3) 0.109(3) Uani 1 1 d . . .
H039 H 0.3301 0.5514 0.4874 0.131 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
_geom_angle_publ_flag
O6 Co01 O6 89.66(17) 8_575 . ?
O6 Co01 O8 89.18(11) 8_575 8_575 ?
O6 Co01 O8 174.71(9) . 8_575 ?
O6 Co01 O8 174.71(9) 8_575 . ?
O6 Co01 O8 89.18(11) . . ?
O8 Co01 O8 91.51(13) 8_575 . ?
O6 Co01 O4 97.93(9) 8_575 . ?
O6 Co01 O4 97.93(9) . . ?
O8 Co01 O4 87.35(9) 8_575 . ?
O8 Co01 O4 87.35(9) . . ?
O6 Co01 O5 87.64(9) 8_575 . ?
O6 Co01 O5 87.64(9) . . ?
O8 Co01 O5 87.16(9) 8_575 . ?
O8 Co01 O5 87.16(9) . . ?
O4 Co01 O5 172.12(12) . . ?
O7 Co02 O4 105.87(11) . . ?
O7 Co02 O9 99.21(12) . . ?
O4 Co02 O9 93.50(11) . . ?
O7 Co02 O1 100.03(12) . . ?
O4 Co02 O1 151.02(14) . . ?
O9 Co02 O1 95.00(16) . . ?
O7 Co02 O3 158.54(11) . . ?
O4 Co02 O3 92.92(11) . . ?
O9 Co02 O3 89.69(12) . . ?
O1 Co02 O3 59.52(13) . . ?
O7 Co02 C010 130.06(12) . . ?
O4 Co02 C010 121.53(13) . . ?
O9 Co02 C010 93.09(12) . . ?
O1 Co02 C010 30.38(13) . . ?
O3 Co02 C010 29.15(12) . . ?
C028 O7 Co02 124.0(2) . . ?
Co02 O4 Co02 123.68(15) 8_575 . ?
Co02 O4 Co01 110.69(9) 8_575 . ?
Co02 O4 Co01 110.69(9) . . ?
C023 O8 Co01 131.22(19) . . ?
C023 O9 Co02 130.5(2) . . ?
C019 C008 C013 118.9(3) 1_455 . ?
C019 C008 C016 121.4(3) 1_455 . ?
C013 C008 C016 119.7(3) . . ?
C028 O6 Co01 137.8(2) . . ?
O3 C010 O1 124.5(4) . . ?
O3 C010 C017 118.2(4) . . ?
O1 C010 C017 117.1(4) . . ?
O3 C010 Co02 62.9(3) . . ?
O1 C010 Co02 61.7(2) . . ?
C017 C010 Co02 177.6(3) . . ?
C027 C011 C014 121.1(3) . . ?
C013 C012 C035 118.6(3) 1_655 . ?
C013 C012 C018 121.5(3) 1_655 2_664 ?
C035 C012 C018 119.8(3) . 2_664 ?
C012 C013 C008 121.3(3) 1_455 . ?
C025 C014 C011 118.6(3) . . ?
C025 C014 C023 120.8(3) . . ?
C011 C014 C023 120.6(3) . . ?
C026 C015 C022 120.9(3) . . ?
C037 C016 C038 116.9(4) . . ?
C037 C016 C008 122.9(4) . . ?
C038 C016 C008 119.8(4) . . ?
C033 C017 C039 116.4(4) . . ?
C033 C017 C010 119.7(4) . . ?
C039 C017 C010 123.7(4) . . ?
C027 C018 C021 118.4(3) . . ?
C027 C018 C012 121.9(3) . 2_665 ?
C021 C018 C012 119.6(3) . 2_665 ?
C008 C019 C029 121.3(3) 1_655 . ?
C026 C020 C031 119.3(3) . . ?
C026 C020 C028 120.3(3) . . ?
C031 C020 C028 120.3(3) . . ?
C025 C021 C018 119.9(3) . . ?
C030 C022 C015 118.1(3) . . ?
C030 C022 C029 121.5(3) . . ?
C015 C022 C029 120.4(3) . . ?
O9 C023 O8 127.5(3) . . ?
O9 C023 C014 116.5(3) . . ?
O8 C023 C014 116.1(3) . . ?
C010 O3 Co02 88.0(3) . . ?
C021 C025 C014 121.1(3) . . ?
C020 C026 C015 120.3(3) . . ?
C011 C027 C018 120.9(3) . . ?
O6 C028 O7 126.7(3) . . ?
O6 C028 C020 116.8(3) . . ?
O7 C028 C020 116.5(3) . . ?
C035 C029 C019 118.6(3) . . ?
C035 C029 C022 120.3(3) . . ?
C019 C029 C022 121.1(3) . . ?
C022 C030 C031 121.0(3) . . ?
C030 C031 C020 120.3(3) . . ?
C037 C033 C017 121.8(4) . . ?
C029 C035 C012 121.2(3) . . ?
C010 O1 Co02 87.9(3) . . ?
C033 C037 C016 122.6(4) . . ?
C039 C038 C016 119.4(5) . . ?
C038 C039 C017 121.8(5) . . ?
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
Co01 O6 2.063(2) 8_575 ?
Co01 O6 2.063(2) . ?
Co01 O8 2.072(2) 8_575 ?
Co01 O8 2.072(2) . ?
Co01 O4 2.077(3) . ?
Co01 O5 2.098(3) . ?
Co02 O7 1.984(2) . ?
Co02 O4 1.9907(14) . ?
Co02 O9 2.054(2) . ?
Co02 O1 2.158(3) . ?
Co02 O3 2.182(3) . ?
Co02 C010 2.449(5) . ?
O7 C028 1.251(4) . ?
O4 Co02 1.9907(14) 8_575 ?
O8 C023 1.254(4) . ?
O9 C023 1.253(4) . ?
C008 C019 1.391(5) 1_455 ?
C008 C013 1.392(5) . ?
C008 C016 1.485(5) . ?
O6 C028 1.244(4) . ?
C010 O3 1.194(5) . ?
C010 O1 1.239(5) . ?
C010 C017 1.536(6) . ?
C011 C027 1.379(5) . ?
C011 C014 1.390(5) . ?
C012 C013 1.390(5) 1_655 ?
C012 C035 1.404(5) . ?
C012 C018 1.476(5) 2_664 ?
C013 C012 1.390(5) 1_455 ?
C014 C025 1.385(5) . ?
C014 C023 1.498(4) . ?
C015 C026 1.395(5) . ?
C015 C022 1.399(5) . ?
C016 C037 1.373(5) . ?
C016 C038 1.404(7) . ?
C017 C033 1.352(6) . ?
C017 C039 1.419(7) . ?
C018 C027 1.380(5) . ?
C018 C021 1.420(5) . ?
C018 C012 1.476(5) 2_665 ?
C019 C008 1.391(5) 1_655 ?
C019 C029 1.397(5) . ?
C020 C026 1.375(5) . ?
C020 C031 1.396(5) . ?
C020 C028 1.514(5) . ?
C021 C025 1.384(5) . ?
C022 C030 1.388(5) . ?
C022 C029 1.484(5) . ?
C029 C035 1.391(5) . ?
C030 C031 1.388(5) . ?
C033 C037 1.347(6) . ?
C038 C039 1.361(7) . ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.011 0.000 -0.002 5741 1739 ' '
