#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:38:42 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179590 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/55/4505508.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_4505508
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 O9'
_chemical_formula_weight         772.60
_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                   10.039(4)
_cell_length_b                   15.446(5)
_cell_length_c                   14.872(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2306.1(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0491
_diffrn_reflns_av_sigmaI/netI    0.1091
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3266
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.60
_exptl_absorpt_coefficient_mu    0.423
_exptl_absorpt_correction_T_max  0.9354
_exptl_absorpt_correction_T_min  0.9278
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.688
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.173
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         2200
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.1239
_refine_ls_R_factor_gt           0.1120
_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)+(0.1906P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2871
_refine_ls_wR_factor_ref         0.3059
_reflns_number_gt                1852
_reflns_number_total             2200
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201369g_si_001.cif
_cod_data_source_block           2
_cod_database_code               4505508
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
C1 C 0.0837(9) 0.9462(5) 0.1652(6) 0.041(2) Uani 1 1 d .
C2 C 0.0868(14) 0.9455(8) 0.2589(6) 0.069(4) Uani 1 1 d .
H2 H 0.1448 0.9098 0.2905 0.083 Uiso 1 1 calc R
C4 C 0.1663(9) 0.8970(5) 0.1020(6) 0.0387(19) Uani 1 1 d .
C5 C 0.2085(9) 0.8708(5) -0.0532(6) 0.041(2) Uani 1 1 d .
C6 C 0.3332(11) 0.9009(9) -0.0771(9) 0.078(4) Uani 1 1 d .
H6 H 0.3757 0.9443 -0.0447 0.093 Uiso 1 1 calc R
C7 C 0.3922(12) 0.8629(10) -0.1526(10) 0.092(5) Uani 1 1 d .
H7 H 0.4737 0.8831 -0.1735 0.110 Uiso 1 1 calc R
C8 C 0.3305(11) 0.7963(8) -0.1954(8) 0.067(3) Uani 1 1 d .
H8 H 0.3742 0.7698 -0.2431 0.080 Uiso 1 1 calc R
C9 C 0.2098(10) 0.7672(6) -0.1721(7) 0.051(2) Uani 1 1 d .
C10 C 0.1462(9) 0.8030(6) -0.0985(6) 0.047(2) Uani 1 1 d .
H10 H 0.0638 0.7824 -0.0797 0.056 Uiso 1 1 calc R
N1 N 0.0000 1.0000 0.1229(6) 0.0367(18) Uani 1 2 d S
N2 N 0.1367(7) 0.9133(4) 0.0198(4) 0.0336(17) Uani 1 1 d .
O1 O 0.2542(7) 0.8428(5) 0.1311(5) 0.059(2) Uani 1 1 d .
O2 O 0.1449(8) 0.7048(5) -0.2149(6) 0.073(2) Uani 1 1 d .
H2A H 0.1893 0.6883 -0.2579 0.088 Uiso 1 1 calc R
Co1 Co 0.0000 1.0000 0.0000 0.0248(6) Uani 1 4 d S
C3 C 0.0000 1.0000 0.3021(9) 0.115(9) Uani 1 2 d S
H3 H 0.0000 1.0000 0.3646 0.138 Uiso 1 2 calc SR
O3 O 0.377(2) 0.7015(14) 0.0507(16) 0.046(6) Uani 0.25 1 d P
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 C1 C2 119.3(9) . .
N1 C1 C4 112.1(8) . .
C2 C1 C4 128.6(8) . .
C3 C2 C1 116.7(10) . .
C3 C2 H2 121.7 . .
C1 C2 H2 121.7 . .
N2 C4 O1 127.3(9) . .
N2 C4 C1 112.2(8) . .
O1 C4 C1 120.5(8) . .
C6 C5 C10 122.3(9) . .
C6 C5 N2 119.2(8) . .
C10 C5 N2 118.4(8) . .
C5 C6 C7 116.7(11) . .
C5 C6 H6 121.7 . .
C7 C6 H6 121.7 . .
C8 C7 C6 120.1(11) . .
C8 C7 H7 120.0 . .
C6 C7 H7 120.0 . .
C9 C8 C7 123.1(10) . .
C9 C8 H8 118.4 . .
C7 C8 H8 118.4 . .
O2 C9 C8 124.4(9) . .
O2 C9 C10 116.4(9) . .
C8 C9 C10 119.2(10) . .
C9 C10 C5 118.4(9) . .
C9 C10 H10 120.8 . .
C5 C10 H10 120.8 . .
C1 N1 C1 124.0(10) . 2_575
C1 N1 Co1 118.0(5) . .
C1 N1 Co1 118.0(5) 2_575 .
C4 N2 C5 120.3(8) . .
C4 N2 Co1 116.4(6) . .
C5 N2 Co1 123.2(5) . .
C9 O2 H2A 109.5 . .
N1 Co1 N1 180.0 3_575 .
N1 Co1 N2 98.74(17) 3_575 .
N1 Co1 N2 81.26(17) . .
N1 Co1 N2 98.74(17) 3_575 2_575
N1 Co1 N2 81.26(17) . 2_575
N2 Co1 N2 162.5(3) . 2_575
N1 Co1 N2 81.26(17) 3_575 4
N1 Co1 N2 98.74(17) . 4
N2 Co1 N2 92.7(4) . 4
N2 Co1 N2 90.0(4) 2_575 4
N1 Co1 N2 81.26(17) 3_575 3_575
N1 Co1 N2 98.74(17) . 3_575
N2 Co1 N2 90.0(4) . 3_575
N2 Co1 N2 92.7(4) 2_575 3_575
N2 Co1 N2 162.5(3) 4 3_575
C2 C3 C2 124.1(12) 2_575 .
C2 C3 H3 117.9 2_575 .
C2 C3 H3 117.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.338(9) .
C1 C2 1.395(12) .
C1 C4 1.466(13) .
C2 C3 1.372(13) .
C2 H2 0.9300 .
C4 N2 1.283(10) .
C4 O1 1.290(10) .
C5 C6 1.382(14) .
C5 C10 1.393(13) .
C5 N2 1.460(10) .
C6 C7 1.398(15) .
C6 H6 0.9300 .
C7 C8 1.358(16) .
C7 H7 0.9300 .
C8 C9 1.338(16) .
C8 H8 0.9300 .
C9 O2 1.326(12) .
C9 C10 1.383(13) .
C10 H10 0.9300 .
N1 C1 1.338(9) 2_575
N1 Co1 1.828(9) .
N2 Co1 1.939(7) .
O2 H2A 0.8200 .
Co1 N1 1.828(9) 3_575
Co1 N2 1.939(7) 2_575
Co1 N2 1.939(7) 4
Co1 N2 1.939(7) 3_575
C3 C2 1.372(13) 2_575
C3 H3 0.9300 .
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 C1 C2 C3 1.3(15) . .
C4 C1 C2 C3 178.3(8) . .
N1 C1 C4 N2 -2.9(10) . .
C2 C1 C4 N2 179.9(10) . .
N1 C1 C4 O1 179.0(7) . .
C2 C1 C4 O1 1.8(16) . .
C10 C5 C6 C7 3.1(19) . .
N2 C5 C6 C7 -174.4(11) . .
C5 C6 C7 C8 -4(2) . .
C6 C7 C8 C9 4(2) . .
C7 C8 C9 O2 177.1(12) . .
C7 C8 C9 C10 -3(2) . .
O2 C9 C10 C5 -177.8(9) . .
C8 C9 C10 C5 2.4(16) . .
C6 C5 C10 C9 -2.5(16) . .
N2 C5 C10 C9 175.0(8) . .
C2 C1 N1 C1 -0.7(8) . 2_575
C4 C1 N1 C1 -178.2(8) . 2_575
C2 C1 N1 Co1 179.3(8) . .
C4 C1 N1 Co1 1.8(8) . .
O1 C4 N2 C5 -2.2(13) . .
C1 C4 N2 C5 179.7(7) . .
O1 C4 N2 Co1 -179.4(7) . .
C1 C4 N2 Co1 2.6(9) . .
C6 C5 N2 C4 -78.9(12) . .
C10 C5 N2 C4 103.5(10) . .
C6 C5 N2 Co1 98.0(11) . .
C10 C5 N2 Co1 -79.6(9) . .
C1 N1 Co1 N1 -135(26) . 3_575
C1 N1 Co1 N1 45(26) 2_575 3_575
C1 N1 Co1 N2 -0.4(5) . .
C1 N1 Co1 N2 179.6(5) 2_575 .
C1 N1 Co1 N2 179.6(5) . 2_575
C1 N1 Co1 N2 -0.4(5) 2_575 2_575
C1 N1 Co1 N2 91.0(5) . 4
C1 N1 Co1 N2 -89.0(5) 2_575 4
C1 N1 Co1 N2 -89.0(5) . 3_575
C1 N1 Co1 N2 91.0(5) 2_575 3_575
C4 N2 Co1 N1 178.6(6) . 3_575
C5 N2 Co1 N1 1.6(6) . 3_575
C4 N2 Co1 N1 -1.4(6) . .
C5 N2 Co1 N1 -178.4(6) . .
C4 N2 Co1 N2 -1.4(6) . 2_575
C5 N2 Co1 N2 -178.4(6) . 2_575
C4 N2 Co1 N2 -99.8(6) . 4
C5 N2 Co1 N2 83.2(6) . 4
C4 N2 Co1 N2 97.5(6) . 3_575
C5 N2 Co1 N2 -79.6(6) . 3_575
C1 C2 C3 C2 -0.6(8) . 2_575
