#------------------------------------------------------------------------------
#$Date: 2016-03-21 19:18:39 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178844 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/98/4109824.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_4109824
loop_
_publ_author_name
'Zhuojia Lin'
'David S. Wragg'
'John E. Warren'
'Russell E. Morris'
_publ_section_title
;
 Anion Control in the Ionothermal Synthesis of Coordination Polymers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10334
_journal_page_last               10335
_journal_paper_doi               10.1021/ja0737671
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C22 H12 Co3 O16'
_chemical_formula_sum            'C22 H12 Co3 O16'
_chemical_formula_weight         709.11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c 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                   14.2616(4)
_cell_length_b                   16.1525(5)
_cell_length_c                   16.4867(5)
_cell_measurement_reflns_used    7055
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.20
_cell_measurement_theta_min      2.98
_cell_volume                     3797.9(2)
_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      90(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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           synchrotron
_diffrn_radiation_wavelength     0.67130
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0191
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37410
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    1.349
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_meas      0
_exptl_crystal_F_000             1412
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         4882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0315
_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)+(0.0698P)²+4.0020P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1019
_reflns_number_gt                4250
_reflns_number_total             4882
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0737671si20070525_064752.cif
_cod_data_source_block           compound_1
_cod_database_code               4109824
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, 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
Co1 Co 0.5000 0.0000 0.5000 0.01345(9) Uani 1 2 d S
Co2 Co 0.478017(17) 0.180576(15) 0.609317(15) 0.01525(9) Uani 1 1 d .
C1 C 0.25588(13) 0.00323(11) 0.65704(12) 0.0186(3) Uani 1 1 d .
C2 C 0.21356(13) 0.04475(11) 0.72163(11) 0.0184(3) Uani 1 1 d .
H2A H 0.2336 0.0988 0.7362 0.022 Uiso 1 1 calc R
C3 C 0.14173(13) 0.00622(11) 0.76461(11) 0.0171(3) Uani 1 1 d .
C4 C 0.11188(13) -0.07272(11) 0.74271(12) 0.0186(3) Uani 1 1 d .
H4A H 0.0658 -0.1002 0.7745 0.022 Uiso 1 1 calc R
C5 C 0.14889(13) -0.11165(11) 0.67482(12) 0.0187(3) Uani 1 1 d .
C6 C 0.22175(13) -0.07329(11) 0.63189(12) 0.0192(3) Uani 1 1 d .
H6A H 0.2479 -0.0996 0.5856 0.023 Uiso 1 1 calc R
C7 C 0.34072(13) 0.03968(11) 0.61636(11) 0.0181(3) Uani 1 1 d .
C8 C 0.09400(12) 0.04751(11) 0.83540(11) 0.0166(3) Uani 1 1 d .
C9 C 0.10902(13) -0.19257(11) 0.64687(12) 0.0192(4) Uani 1 1 d .
C10 C 0.54800(14) 0.19182(12) 0.46913(12) 0.0201(4) Uani 1 1 d .
C11 C 0.57907(18) 0.19411(14) 0.38223(13) 0.0287(4) Uani 1 1 d .
H11A H 0.6176 0.2435 0.3730 0.043 Uiso 1 1 calc R
H11B H 0.5239 0.1959 0.3468 0.043 Uiso 1 1 calc R
H11C H 0.6160 0.1444 0.3701 0.043 Uiso 1 1 calc R
O1 O 0.36775(9) 0.00469(8) 0.55185(8) 0.0198(3) Uani 1 1 d .
O2 O 0.37804(10) 0.10134(8) 0.65041(9) 0.0233(3) Uani 1 1 d .
O3 O 0.09043(9) 0.12568(8) 0.83581(8) 0.0193(3) Uani 1 1 d .
O4 O 0.06050(10) -0.00049(8) 0.88762(8) 0.0198(3) Uani 1 1 d .
O5 O 0.04423(10) -0.22480(8) 0.68949(9) 0.0215(3) Uani 1 1 d .
O6 O 0.13716(11) -0.22539(9) 0.58271(9) 0.0257(3) Uani 1 1 d .
O7 O 0.49656(10) 0.13162(9) 0.49365(8) 0.0197(3) Uani 1 1 d .
O8 O 0.56694(11) 0.24871(9) 0.51732(9) 0.0278(3) Uani 1 1 d .
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
O4 Co1 O4 180.0 6_657 2_554
O4 Co1 O1 89.40(6) 6_657 5_656
O4 Co1 O1 90.60(6) 2_554 5_656
O4 Co1 O1 90.60(6) 6_657 .
O4 Co1 O1 89.40(6) 2_554 .
O1 Co1 O1 180.0 5_656 .
O4 Co1 O7 86.66(5) 6_657 5_656
O4 Co1 O7 93.34(5) 2_554 5_656
O1 Co1 O7 87.87(5) 5_656 5_656
O1 Co1 O7 92.13(5) . 5_656
O4 Co1 O7 93.34(5) 6_657 .
O4 Co1 O7 86.66(5) 2_554 .
O1 Co1 O7 92.13(5) 5_656 .
O1 Co1 O7 87.87(5) . .
O7 Co1 O7 180.0 5_656 .
O4 Co1 Co2 64.36(4) 6_657 .
O4 Co1 Co2 115.64(4) 2_554 .
O1 Co1 Co2 109.26(4) 5_656 .
O1 Co1 Co2 70.74(4) . .
O7 Co1 Co2 145.31(4) 5_656 .
O7 Co1 Co2 34.69(4) . .
O2 Co2 O3 97.45(6) . 6_657
O2 Co2 O5 98.42(6) . 8_665
O3 Co2 O5 99.20(5) 6_657 8_665
O2 Co2 O7 98.94(6) . .
O3 Co2 O7 98.11(6) 6_657 .
O5 Co2 O7 153.60(6) 8_665 .
O2 Co2 O8 157.37(6) . .
O3 Co2 O8 93.90(6) 6_657 .
O5 Co2 O8 99.01(6) 8_665 .
O7 Co2 O8 59.96(5) . .
O2 Co2 O6 88.75(6) . 8_665
O3 Co2 O6 159.99(5) 6_657 8_665
O5 Co2 O6 60.97(5) 8_665 8_665
O7 Co2 O6 99.69(5) . 8_665
O8 Co2 O6 87.18(6) . 8_665
O2 Co2 C9 94.94(6) . 8_665
O3 Co2 C9 129.96(6) 6_657 8_665
O5 Co2 C9 30.88(6) 8_665 8_665
O7 Co2 C9 127.42(6) . 8_665
O8 Co2 C9 92.64(6) . 8_665
O6 Co2 C9 30.12(6) 8_665 8_665
O2 Co2 Co1 72.84(4) . .
O3 Co2 Co1 78.03(4) 6_657 .
O5 Co2 Co1 170.21(4) 8_665 .
O7 Co2 Co1 35.60(4) . .
O8 Co2 Co1 90.58(4) . .
O6 Co2 Co1 121.96(4) 8_665 .
C9 Co2 Co1 151.43(5) 8_665 .
C6 C1 C2 120.19(17) . .
C6 C1 C7 119.76(17) . .
C2 C1 C7 120.01(16) . .
C3 C2 C1 119.44(16) . .
C4 C3 C2 120.17(17) . .
C4 C3 C8 117.92(16) . .
C2 C3 C8 121.91(16) . .
C5 C4 C3 120.52(17) . .
C4 C5 C6 119.27(16) . .
C4 C5 C9 119.93(16) . .
C6 C5 C9 120.78(17) . .
C1 C6 C5 120.10(17) . .
O2 C7 O1 126.78(17) . .
O2 C7 C1 116.77(16) . .
O1 C7 C1 116.45(16) . .
O4 C8 O3 126.81(17) . .
O4 C8 C3 115.50(15) . .
O3 C8 C3 117.68(16) . .
O6 C9 O5 121.83(17) . .
O6 C9 C5 120.57(17) . .
O5 C9 C5 117.57(16) . .
O6 C9 Co2 66.30(10) . 8_655
O5 C9 Co2 55.60(9) . 8_655
C5 C9 Co2 171.86(14) . 8_655
O8 C10 O7 118.84(18) . .
O8 C10 C11 121.83(18) . .
O7 C10 C11 119.23(18) . .
C7 O1 Co1 129.85(12) . .
C7 O2 Co2 130.17(13) . .
C8 O3 Co2 117.88(12) . 6_557
C8 O4 Co1 141.38(12) . 2
C9 O5 Co2 93.52(11) . 8_655
C9 O6 Co2 83.59(11) . 8_655
C10 O7 Co2 94.21(12) . .
C10 O7 Co1 139.36(13) . .
Co2 O7 Co1 109.71(6) . .
C10 O8 Co2 86.97(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O4 2.0438(13) 6_657
Co1 O4 2.0438(13) 2_554
Co1 O1 2.0722(13) 5_656
Co1 O1 2.0722(13) .
Co1 O7 2.1291(14) 5_656
Co1 O7 2.1291(14) .
Co1 Co2 3.4430(2) .
Co2 O2 2.0323(14) .
Co2 O3 2.0433(13) 6_657
Co2 O5 2.0455(13) 8_665
Co2 O7 2.0813(14) .
Co2 O8 2.2627(15) .
Co2 O6 2.2798(14) 8_665
Co2 C9 2.4743(18) 8_665
C1 C6 1.392(2) .
C1 C2 1.396(3) .
C1 C7 1.503(3) .
C2 C3 1.392(3) .
C3 C4 1.392(2) .
C3 C8 1.507(2) .
C4 C5 1.388(3) .
C5 C6 1.402(3) .
C5 C9 1.498(2) .
C7 O2 1.261(2) .
C7 O1 1.265(2) .
C8 O4 1.253(2) .
C8 O3 1.264(2) .
C9 O6 1.249(2) .
C9 O5 1.272(2) .
C9 Co2 2.4743(18) 8_655
C10 O8 1.244(2) .
C10 O7 1.283(2) .
C10 C11 1.500(3) .
O3 Co2 2.0433(13) 6_557
O4 Co1 2.0438(13) 2
O5 Co2 2.0455(13) 8_655
O6 Co2 2.2798(14) 8_655
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
O1 C7 C1 C2 -170.87(18)
O3 C8 C3 C4 -151.37(18)
O5 C9 C5 C6 178.68(18)
O2 C7 C1 C2 9.8(3)
O4 C8 C3 C4 27.6(2)
O6 C9 C5 C6 -3.3(3)
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
1 0.009 -0.015 0.500 840.9 145.9
2 -0.080 0.377 0.000 840.9 145.9
