#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:38:42 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179590 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/55/4505507.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_4505507
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           82
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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                   13.948(5)
_cell_length_b                   13.948(5)
_cell_length_c                   13.771(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2679.1(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0629
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22736
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    0.364
_exptl_absorpt_correction_T_max  0.9441
_exptl_absorpt_correction_T_min  0.9374
_exptl_crystal_density_diffrn    0.958
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         3162
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0515
_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)+(0.0871P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1281
_refine_ls_wR_factor_ref         0.1350
_reflns_number_gt                2453
_reflns_number_total             3162
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201369g_si_001.cif
_cod_data_source_block           1
_cod_database_code               4505507
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+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 0.4600(2) 0.0748(2) 0.5702(2) 0.0315(7) Uani 1 1 d .
C2 C 0.4582(3) 0.0762(3) 0.4691(2) 0.0492(9) Uani 1 1 d .
H2 H 0.4297 0.1268 0.4359 0.059 Uiso 1 1 calc R
C3 C 0.5000 0.0000 0.4188(3) 0.0574(12) Uani 1 2 d S
H3 H 0.5000 0.0000 0.3512 0.069 Uiso 1 2 calc SR
C4 C 0.4196(2) 0.1465(2) 0.6389(2) 0.0320(6) Uani 1 1 d .
C5 C 0.3963(2) 0.1786(2) 0.8087(2) 0.0273(6) Uani 1 1 d .
C6 C 0.4558(2) 0.2411(2) 0.8594(3) 0.0383(7) Uani 1 1 d .
H6 H 0.5182 0.2510 0.8377 0.046 Uiso 1 1 calc R
C7 C 0.4244(3) 0.2882(3) 0.9406(3) 0.0542(10) Uani 1 1 d .
H7 H 0.4660 0.3273 0.9755 0.065 Uiso 1 1 calc R
C8 C 0.3305(3) 0.2771(3) 0.9703(3) 0.0481(9) Uani 1 1 d .
C9 C 0.2709(2) 0.2152(2) 0.9202(3) 0.0455(8) Uani 1 1 d .
H9 H 0.2079 0.2067 0.9407 0.055 Uiso 1 1 calc R
C10 C 0.3035(2) 0.1665(2) 0.8410(2) 0.0334(7) Uani 1 1 d .
H10 H 0.2628 0.1247 0.8084 0.040 Uiso 1 1 calc R
N1 N 0.5000 0.0000 0.61595(18) 0.0224(5) Uani 1 2 d S
N2 N 0.43347(15) 0.12158(15) 0.73018(14) 0.0243(5) Uani 1 1 d .
O1 O 0.37591(19) 0.21973(17) 0.60830(17) 0.0501(7) Uani 1 1 d .
O2 O 0.3029(2) 0.3262(2) 1.0520(2) 0.0664(8) Uani 1 1 d .
H2A H 0.2464 0.3149 1.0636 0.080 Uiso 1 1 calc R
O3 O 0.0000 0.0000 1.0000 0.405(19) Uani 1 4 d S
Co1 Co 0.5000 0.0000 0.7500 0.0235(2) Uani 1 4 d S
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 119.2(3) . .
N1 C1 C4 112.4(2) . .
C2 C1 C4 128.3(3) . .
C1 C2 C3 118.5(3) . .
C1 C2 H2 120.7 . .
C3 C2 H2 120.7 . .
C2 C3 C2 120.5(4) 2_655 .
C2 C3 H3 119.8 2_655 .
C2 C3 H3 119.8 . .
O1 C4 N2 127.1(3) . .
O1 C4 C1 120.9(3) . .
N2 C4 C1 112.0(3) . .
C10 C5 C6 118.3(3) . .
C10 C5 N2 120.9(3) . .
C6 C5 N2 120.5(3) . .
C7 C6 C5 121.3(3) . .
C7 C6 H6 119.4 . .
C5 C6 H6 119.4 . .
C6 C7 C8 119.5(3) . .
C6 C7 H7 120.3 . .
C8 C7 H7 120.3 . .
O2 C8 C7 117.0(3) . .
O2 C8 C9 123.5(3) . .
C7 C8 C9 119.5(3) . .
C10 C9 C8 120.6(3) . .
C10 C9 H9 119.7 . .
C8 C9 H9 119.7 . .
C9 C10 C5 120.8(3) . .
C9 C10 H10 119.6 . .
C5 C10 H10 119.6 . .
C1 N1 C1 123.9(3) 2_655 .
C1 N1 Co1 118.04(16) 2_655 .
C1 N1 Co1 118.04(16) . .
C4 N2 C5 121.2(2) . .
C4 N2 Co1 115.61(19) . .
C5 N2 Co1 123.12(16) . .
C8 O2 H2A 109.5 . .
N1 Co1 N1 180.0 7_556 .
N1 Co1 N2 98.04(6) 7_556 2_655
N1 Co1 N2 81.96(6) . 2_655
N1 Co1 N2 98.04(6) 7_556 .
N1 Co1 N2 81.96(6) . .
N2 Co1 N2 163.93(11) 2_655 .
N1 Co1 N2 81.96(6) 7_556 7_556
N1 Co1 N2 98.04(6) . 7_556
N2 Co1 N2 91.120(16) 2_655 7_556
N2 Co1 N2 91.119(16) . 7_556
N1 Co1 N2 81.96(6) 7_556 8_546
N1 Co1 N2 98.04(6) . 8_546
N2 Co1 N2 91.120(16) 2_655 8_546
N2 Co1 N2 91.122(16) . 8_546
N2 Co1 N2 163.92(11) 7_556 8_546
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.341(3) .
C1 C2 1.392(4) .
C1 C4 1.488(4) .
C2 C3 1.397(4) .
C2 H2 0.9300 .
C3 C2 1.397(4) 2_655
C3 H3 0.9300 .
C4 O1 1.262(4) .
C4 N2 1.318(3) .
C5 C10 1.379(4) .
C5 C6 1.392(4) .
C5 N2 1.438(3) .
C6 C7 1.369(5) .
C6 H6 0.9300 .
C7 C8 1.380(5) .
C7 H7 0.9300 .
C8 O2 1.373(4) .
C8 C9 1.384(5) .
C9 C10 1.363(5) .
C9 H9 0.9300 .
C10 H10 0.9300 .
N1 C1 1.341(3) 2_655
N1 Co1 1.846(3) .
N2 Co1 1.952(2) .
O2 H2A 0.8200 .
Co1 N1 1.846(3) 7_556
Co1 N2 1.952(2) 2_655
Co1 N2 1.952(2) 7_556
Co1 N2 1.952(2) 8_546
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(4) . .
C4 C1 C2 C3 -179.3(3) . .
C1 C2 C3 C2 0.6(2) . 2_655
N1 C1 C4 O1 -177.2(2) . .
C2 C1 C4 O1 0.9(5) . .
N1 C1 C4 N2 1.1(3) . .
C2 C1 C4 N2 179.2(3) . .
C10 C5 C6 C7 1.4(5) . .
N2 C5 C6 C7 -173.0(3) . .
C5 C6 C7 C8 -3.1(6) . .
C6 C7 C8 O2 -179.8(4) . .
C6 C7 C8 C9 3.0(6) . .
O2 C8 C9 C10 -178.2(4) . .
C7 C8 C9 C10 -1.2(6) . .
C8 C9 C10 C5 -0.6(5) . .
C6 C5 C10 C9 0.5(5) . .
N2 C5 C10 C9 174.8(3) . .
C2 C1 N1 C1 0.6(2) . 2_655
C4 C1 N1 C1 179.0(3) . 2_655
C2 C1 N1 Co1 -179.4(2) . .
C4 C1 N1 Co1 -1.0(3) . .
O1 C4 N2 C5 1.0(5) . .
C1 C4 N2 C5 -177.1(2) . .
O1 C4 N2 Co1 177.5(3) . .
C1 C4 N2 Co1 -0.7(3) . .
C10 C5 N2 C4 85.1(3) . .
C6 C5 N2 C4 -100.8(3) . .
C10 C5 N2 Co1 -91.1(3) . .
C6 C5 N2 Co1 83.0(3) . .
C1 N1 Co1 N1 0(100) 2_655 7_556
C1 N1 Co1 N1 0(34) . 7_556
C1 N1 Co1 N2 0.56(15) 2_655 2_655
C1 N1 Co1 N2 -179.43(15) . 2_655
C1 N1 Co1 N2 -179.44(15) 2_655 .
C1 N1 Co1 N2 0.56(16) . .
C1 N1 Co1 N2 90.56(15) 2_655 7_556
C1 N1 Co1 N2 -89.43(15) . 7_556
C1 N1 Co1 N2 -89.44(15) 2_655 8_546
C1 N1 Co1 N2 90.57(15) . 8_546
C4 N2 Co1 N1 -179.89(19) . 7_556
C5 N2 Co1 N1 -3.5(2) . 7_556
C4 N2 Co1 N1 0.11(19) . .
C5 N2 Co1 N1 176.5(2) . .
C4 N2 Co1 N2 0.11(19) . 2_655
C5 N2 Co1 N2 176.5(2) . 2_655
C4 N2 Co1 N2 98.1(2) . 7_556
C5 N2 Co1 N2 -85.5(2) . 7_556
C4 N2 Co1 N2 -97.9(2) . 8_546
C5 N2 Co1 N2 78.5(2) . 8_546
