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#$Date: 2016-03-24 02:38:42 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179590 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/55/4505509.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_4505509
loop_
_publ_author_name
'Ali, Afsar'
'Hundal, Geeta'
'Gupta, Rajeev'
_publ_section_title
;
 Co3+-Based Building Blocks with Appended Phenol and Catechol Groups:
 Examples of Placing Hydrogen-Bond Donors and Acceptors in a Single
 Molecule
;
_journal_issue                   3
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1308
_journal_paper_doi               10.1021/cg201369g
_journal_volume                  12
_journal_year                    2012
_chemical_formula_sum            'C38 H29 Co N6 O13'
_chemical_formula_weight         836.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           23
_symmetry_space_group_name_Hall  'I 2 2'
_symmetry_space_group_name_H-M   'I 2 2 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            2
_cell_length_a                   10.3708(3)
_cell_length_b                   15.3526(5)
_cell_length_c                   15.0072(6)
_cell_measurement_temperature    150(2)
_cell_volume                     2389.43(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.930
_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  0.0468
_diffrn_reflns_av_sigmaI/netI    0.0815
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12480
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.84
_diffrn_reflns_theta_min         3.57
_exptl_absorpt_coefficient_mu    0.419
_exptl_absorpt_correction_T_max  0.9284
_exptl_absorpt_correction_T_min  0.8917
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.524
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.159
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         4056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0783
_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)+(0.1546P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2198
_refine_ls_wR_factor_ref         0.2277
_reflns_number_gt                3055
_reflns_number_total             4056
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201369g_si_001.cif
_cod_data_source_block           3
_cod_database_code               4505509
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, 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 0.0000 0.0000 0.0000 0.0152(2) Uani 1 4 d S
O1 O 0.2665(3) 0.1287(2) -0.1426(2) 0.0342(7) Uani 1 1 d .
O2 O 0.1573(3) -0.2278(3) -0.2844(3) 0.0550(12) Uani 1 1 d .
H21 H 0.2095 -0.2657 -0.3024 0.083 Uiso 1 1 calc R
O3 O 0.4031(3) -0.2602(3) -0.2384(3) 0.0593(13) Uani 1 1 d .
H31 H 0.4795 -0.2636 -0.2200 0.089 Uiso 1 1 calc R
O4 O 0.381(3) 0.0457(12) -0.2942(17) 0.087(8) Uani 0.25 1 d P
N2 N 0.1363(3) 0.0186(2) -0.0891(2) 0.0268(7) Uani 1 1 d .
N1 N 0.0000 0.1207(2) 0.0000 0.0264(8) Uani 1 2 d S
C1 C 0.1729(4) 0.1002(2) -0.0991(3) 0.0239(7) Uani 1 1 d .
C2 C 0.0893(4) 0.1622(3) -0.0486(3) 0.0322(9) Uani 1 1 d .
C3 C 0.0888(7) 0.2523(3) -0.0500(5) 0.0539(15) Uani 1 1 d .
H3 H 0.1493 0.2833 -0.0853 0.065 Uiso 1 1 calc R
C4 C 0.0000 0.2958(4) 0.0000 0.072(3) Uani 1 2 d S
H4 H 0.0000 0.3577 0.0000 0.086 Uiso 1 2 calc SR
C5 C 0.2088(4) -0.0490(3) -0.1287(3) 0.0279(8) Uani 1 1 d .
C6 C 0.1485(4) -0.1057(3) -0.1888(3) 0.0324(9) Uani 1 1 d .
H6 H 0.0617 -0.0960 -0.2063 0.039 Uiso 1 1 calc R
C7 C 0.2164(4) -0.1760(3) -0.2225(4) 0.0372(10) Uani 1 1 d .
C8 C 0.3442(4) -0.1904(3) -0.2001(4) 0.0392(11) Uani 1 1 d .
C9 C 0.4046(4) -0.1331(4) -0.1406(4) 0.0440(12) Uani 1 1 d .
H9 H 0.4920 -0.1421 -0.1241 0.053 Uiso 1 1 calc R
C10 C 0.3371(4) -0.0638(4) -0.1063(4) 0.0414(11) Uani 1 1 d .
H10 H 0.3790 -0.0251 -0.0663 0.050 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'
N N 0.0061 0.0033 '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
N1 Co1 N1 180.0 . 2
N1 Co1 N2 98.36(9) . 3
N1 Co1 N2 81.64(9) 2 3
N1 Co1 N2 81.64(9) . 4
N1 Co1 N2 98.36(9) 2 4
N2 Co1 N2 94.4(2) 3 4
N1 Co1 N2 81.64(9) . .
N1 Co1 N2 98.37(9) 2 .
N2 Co1 N2 88.1(2) 3 .
N2 Co1 N2 163.27(18) 4 .
N1 Co1 N2 98.36(9) . 2
N1 Co1 N2 81.64(9) 2 2
N2 Co1 N2 163.27(18) 3 2
N2 Co1 N2 88.1(2) 4 2
N2 Co1 N2 94.4(2) . 2
C7 O2 H21 109.5 . .
C8 O3 H31 109.5 . .
C1 N2 C5 119.8(3) . .
C1 N2 Co1 115.0(3) . .
C5 N2 Co1 124.2(3) . .
C2 N1 C2 123.2(5) 4 .
C2 N1 Co1 118.4(2) 4 .
C2 N1 Co1 118.4(2) . .
O1 C1 N2 128.1(4) . .
O1 C1 C2 119.6(4) . .
N2 C1 C2 112.4(3) . .
N1 C2 C3 118.8(5) . .
N1 C2 C1 112.0(3) . .
C3 C2 C1 129.1(4) . .
C4 C3 C2 119.0(5) . .
C4 C3 H3 120.5 . .
C2 C3 H3 120.5 . .
C3 C4 C3 121.3(6) . 4
C3 C4 H4 119.4 . .
C3 C4 H4 119.4 4 .
C10 C5 C6 118.7(4) . .
C10 C5 N2 121.8(4) . .
C6 C5 N2 119.4(4) . .
C7 C6 C5 119.5(4) . .
C7 C6 H6 120.2 . .
C5 C6 H6 120.2 . .
O2 C7 C6 118.3(4) . .
O2 C7 C8 120.0(4) . .
C6 C7 C8 121.5(4) . .
O3 C8 C7 117.0(4) . .
O3 C8 C9 124.2(4) . .
C7 C8 C9 118.8(4) . .
C10 C9 C8 119.8(4) . .
C10 C9 H9 120.1 . .
C8 C9 H9 120.1 . .
C9 C10 C5 121.6(4) . .
C9 C10 H10 119.2 . .
C5 C10 H10 119.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N1 1.853(4) .
Co1 N1 1.853(4) 2
Co1 N2 1.966(4) 3
Co1 N2 1.966(4) 4
Co1 N2 1.966(4) .
Co1 N2 1.966(4) 2
O1 C1 1.248(5) .
O2 C7 1.368(6) .
O2 H21 0.8400 .
O3 C8 1.361(5) .
O3 H31 0.8400 .
N2 C1 1.317(5) .
N2 C5 1.413(5) .
N1 C2 1.340(5) 4
N1 C2 1.340(5) .
C1 C2 1.494(6) .
C2 C3 1.384(6) .
C3 C4 1.363(7) .
C3 H3 0.9500 .
C4 C3 1.363(7) 4
C4 H4 0.9500 .
C5 C10 1.392(6) .
C5 C6 1.400(6) .
C6 C7 1.384(6) .
C6 H6 0.9500 .
C7 C8 1.385(6) .
C8 C9 1.402(6) .
C9 C10 1.373(6) .
C9 H9 0.9500 .
C10 H10 0.9500 .
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N1 Co1 N2 C1 7.3(3) . .
N1 Co1 N2 C1 -172.7(3) 2 .
N2 Co1 N2 C1 -91.5(3) 3 .
N2 Co1 N2 C1 7.3(3) 4 .
N2 Co1 N2 C1 105.1(3) 2 .
N1 Co1 N2 C5 175.9(3) . .
N1 Co1 N2 C5 -4.1(3) 2 .
N2 Co1 N2 C5 77.1(3) 3 .
N2 Co1 N2 C5 175.9(3) 4 .
N2 Co1 N2 C5 -86.3(3) 2 .
N1 Co1 N1 C2 -52(2) 2 4
N2 Co1 N1 C2 -98.4(2) 3 4
N2 Co1 N1 C2 -5.2(2) 4 4
N2 Co1 N1 C2 174.8(2) . 4
N2 Co1 N1 C2 81.6(2) 2 4
N1 Co1 N1 C2 128(2) 2 .
N2 Co1 N1 C2 81.6(2) 3 .
N2 Co1 N1 C2 174.8(2) 4 .
N2 Co1 N1 C2 -5.2(2) . .
N2 Co1 N1 C2 -98.4(2) 2 .
C5 N2 C1 O1 1.6(7) . .
Co1 N2 C1 O1 170.8(4) . .
C5 N2 C1 C2 -176.8(4) . .
Co1 N2 C1 C2 -7.7(4) . .
C2 N1 C2 C3 -1.0(4) 4 .
Co1 N1 C2 C3 179.0(4) . .
C2 N1 C2 C1 -177.6(4) 4 .
Co1 N1 C2 C1 2.4(4) . .
O1 C1 C2 N1 -175.0(3) . .
N2 C1 C2 N1 3.7(5) . .
O1 C1 C2 C3 8.9(8) . .
N2 C1 C2 C3 -172.5(6) . .
N1 C2 C3 C4 1.9(8) . .
C1 C2 C3 C4 177.8(4) . .
C2 C3 C4 C3 -0.9(4) . 4
C1 N2 C5 C10 61.3(6) . .
Co1 N2 C5 C10 -106.8(5) . .
C1 N2 C5 C6 -122.1(4) . .
Co1 N2 C5 C6 69.8(5) . .
C10 C5 C6 C7 1.7(7) . .
N2 C5 C6 C7 -175.0(4) . .
C5 C6 C7 O2 -176.8(5) . .
C5 C6 C7 C8 -1.9(8) . .
O2 C7 C8 O3 -3.7(8) . .
C6 C7 C8 O3 -178.5(5) . .
O2 C7 C8 C9 176.1(5) . .
C6 C7 C8 C9 1.3(9) . .
O3 C8 C9 C10 179.3(6) . .
C7 C8 C9 C10 -0.5(9) . .
C8 C9 C10 C5 0.4(9) . .
C6 C5 C10 C9 -1.0(8) . .
N2 C5 C10 C9 175.7(5) . .
