#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/58/4315868.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_4315868
loop_
_publ_author_name
'Ai-Yun Fu'
'Yu-Lin Jiang'
'Yao-Yu Wang'
'Xiao-Nan Gao'
'Guo-Ping Yang'
'Lei Hou'
'Qi-Zhen Shi'
_publ_contact_author_email       wyaoyu@nwu.edu.cn
_publ_section_title
;
 DMF/H2O Volume Ratio Controls the Syntheses and Transformations of a
 Series of Cobalt Complexes Constructed Using a Rigid Angular Multitopic
 Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5495
_journal_page_last               5502
_journal_paper_doi               10.1021/ic902548f
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C25.5 H19.5 Co N10.5 O0.5'
_chemical_formula_weight         539.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            9
_cell_length_a                   27.720(3)
_cell_length_b                   27.720(3)
_cell_length_c                   9.7135(9)
_cell_measurement_reflns_used    2060
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.109
_cell_measurement_theta_min      2.262
_cell_volume                     6463.9(12)
_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      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_sigmaI/netI    0.0774
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10844
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.630
_exptl_absorpt_correction_T_max  0.8501
_exptl_absorpt_correction_T_min  0.8369
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             265
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         2532
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1326
_refine_ls_R_factor_gt           0.0560
_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)+(0.0953P)²+0.4401P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1457
_refine_ls_wR_factor_ref         0.1849
_reflns_number_gt                1343
_reflns_number_total             2532
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902548f_si_001_4.cif
_cod_data_source_block           compound_3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        6463.8(10)
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C25.50 H19.50 Co N10.50 O0.50 '
_cod_database_code               4315868
loop_
_publ_contact_author
;    
      Wang, Yao-Yu
      Key Laboratory of Synthetic and Natural Functional Molecule Chemistry 
      of Ministry of Education, Department of Chemistry and Shaanxi 
      Key Laboratory of Physico-Inorganic Chemistry
      Northwest University
      Xi'an, 710069
      P. R. China
;
;  
      Yu-Lin Jiang
      Department of Chemistry, East Tennessee State University
      Johnson City
      TN 37614
;
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Co1 Co 0.5000 1.0000 0.0000 0.0587(4) Uani 1 2 d S . 1
N1 N 0.54530(17) 1.01374(19) 0.1748(4) 0.0601(12) Uani 1 1 d . A 1
N2 N 0.59614(16) 1.05335(18) 0.2204(4) 0.0574(11) Uani 1 1 d . A 1
N3 N 0.55466(18) 0.98684(19) 0.3853(4) 0.0674(12) Uani 1 1 d . A 1
N4 N 0.44403(17) 0.92957(19) 0.1282(4) 0.0676(13) Uani 1 1 d . B 1
N5 N 0.74893(17) 1.12606(18) 0.5765(4) 0.0663(12) Uani 1 1 d . . 1
N6 N 0.32(18) 0.65(15) 0.27(6) 0.2(5) Uani 0.110(7) 1 d P . 1
O1 O 0.285(8) 0.691(8) 0.41(3) 0.21(7) Uani 0.110(7) 1 d P . 1
N6' N 0.284(8) 0.716(7) 0.703(18) 0.20(4) Uani 0.140(7) 1 d P . 2
O1' O 0.221(4) 0.696(6) 0.556(10) 0.20(3) Uani 0.140(7) 1 d P . 2
C1 C 0.3918(3) 0.8898(3) 0.1022(7) 0.0866(19) Uani 1 1 d . . .
H1 H 0.3768 0.8888 0.0159 0.104 Uiso 1 1 calc R B 1
C2 C 0.3592(3) 0.8505(3) 0.1970(8) 0.105(2) Uani 1 1 d . B .
H2 H 0.3227 0.8239 0.1758 0.125 Uiso 1 1 calc R . .
C3 C 0.3812(3) 0.8506(3) 0.3245(8) 0.103(2) Uani 1 1 d . . .
H3 H 0.3598 0.8238 0.3897 0.124 Uiso 1 1 calc R B .
C4 C 0.4343(3) 0.8903(3) 0.3541(7) 0.0869(19) Uani 1 1 d . B .
H4 H 0.4495 0.8912 0.4399 0.104 Uiso 1 1 calc R . .
C5 C 0.4656(2) 0.9295(2) 0.2545(6) 0.0642(15) Uani 1 1 d . . .
C6 C 0.5220(2) 0.9756(2) 0.2743(6) 0.0601(14) Uani 1 1 d . A .
C7 C 0.5993(2) 1.0347(2) 0.3463(5) 0.0572(13) Uani 1 1 d . . .
C8 C 0.65021(19) 1.0667(2) 0.4294(5) 0.0552(13) Uani 1 1 d . A .
C9 C 0.6915(2) 1.1183(2) 0.3879(6) 0.0726(16) Uani 1 1 d . . .
H9 H 0.6871 1.1341 0.3079 0.087 Uiso 1 1 calc R A .
C10 C 0.7390(2) 1.1463(2) 0.4635(6) 0.0737(17) Uani 1 1 d . A .
H10 H 0.7659 1.1816 0.4340 0.088 Uiso 1 1 calc R C 1
C11 C 0.7086(2) 1.0758(2) 0.6162(6) 0.0820(19) Uani 1 1 d . . .
H11 H 0.7143 1.0603 0.6952 0.098 Uiso 1 1 calc R . 1
C12 C 0.6593(2) 1.0457(2) 0.5471(6) 0.0786(18) Uani 1 1 d . A .
H12 H 0.6322 1.0112 0.5803 0.094 Uiso 1 1 calc R . .
C13 C 0.292(19) 0.684(16) 0.29(5) 0.20(11) Uani 0.110(7) 1 d P . 1
H13 H 0.2812 0.7074 0.2441 0.245 Uiso 0.110(7) 1 d PR . 1
C14 C 0.336(19) 0.63(2) 0.39(5) 0.21(10) Uani 0.110(7) 1 d P . 1
H14A H 0.3196 0.6257 0.4790 0.308 Uiso 0.110(7) 1 d PR . 1
H14B H 0.3757 0.6543 0.3966 0.308 Uiso 0.110(7) 1 d PR . 1
H14C H 0.3236 0.6015 0.3364 0.308 Uiso 0.110(7) 1 d PR . 1
C15 C 0.33(12) 0.64(7) 0.13(7) 0.2(4) Uani 0.110(7) 1 d P . 1
H15A H 0.2962 0.6237 0.0898 0.306 Uiso 0.110(7) 1 d PR . 1
H15B H 0.3540 0.6269 0.1071 0.306 Uiso 0.110(7) 1 d PR . 1
H15C H 0.3506 0.6817 0.1065 0.306 Uiso 0.110(7) 1 d PR . 1
C13' C 0.262(9) 0.734(7) 0.61(2) 0.20(5) Uani 0.140(7) 1 d P . 2
H13' H 0.2760 0.7703 0.5787 0.244 Uiso 0.140(7) 1 d PR . 2
C14' C 0.260(6) 0.656(10) 0.729(15) 0.21(4) Uani 0.140(7) 1 d P . 2
H14D H 0.2624 0.6331 0.6574 0.308 Uiso 0.140(7) 1 d PR . 2
H14E H 0.2214 0.6407 0.7542 0.308 Uiso 0.140(7) 1 d PR . 2
H14F H 0.2806 0.6556 0.8076 0.308 Uiso 0.140(7) 1 d PR . 2
C15' C 0.334(7) 0.753(8) 0.782(18) 0.21(5) Uani 0.140(7) 1 d P . 2
H15D H 0.3452 0.7895 0.7450 0.308 Uiso 0.140(7) 1 d PR . 2
H15E H 0.3622 0.7437 0.7609 0.308 Uiso 0.140(7) 1 d PR . 2
H15F H 0.3305 0.7542 0.8804 0.308 Uiso 0.140(7) 1 d PR . 2
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'
Co Co 0.3494 0.9721 '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'
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
N1 Co1 N1 180.000(1) . 10_675 ?
N1 Co1 N4 102.32(17) . 10_675 ?
N1 Co1 N4 77.68(17) 10_675 10_675 ?
N1 Co1 N4 77.68(17) . . ?
N1 Co1 N4 102.32(17) 10_675 . ?
N4 Co1 N4 180.000(1) 10_675 . ?
N1 Co1 N5 89.91(15) . 5_664 ?
N1 Co1 N5 90.09(15) 10_675 5_664 ?
N4 Co1 N5 86.32(16) 10_675 5_664 ?
N4 Co1 N5 93.68(16) . 5_664 ?
N1 Co1 N5 90.09(15) . 17_455 ?
N1 Co1 N5 89.91(15) 10_675 17_455 ?
N4 Co1 N5 93.68(16) 10_675 17_455 ?
N4 Co1 N5 86.32(16) . 17_455 ?
N5 Co1 N5 180.000(1) 5_664 17_455 ?
C6 N1 N2 107.6(4) . . ?
C6 N1 Co1 116.4(3) . . ?
N2 N1 Co1 136.0(4) . . ?
C7 N2 N1 103.0(4) . . ?
C7 N3 C6 100.7(4) . . ?
C1 N4 C5 117.7(5) . . ?
C1 N4 Co1 128.7(4) . . ?
C5 N4 Co1 113.5(3) . . ?
C10 N5 C11 116.2(4) . . ?
C10 N5 Co1 120.3(3) . 9_565 ?
C11 N5 Co1 122.5(3) . 9_565 ?
C14 N6 N6 109(10) 3_565 2_665 ?
N6 N6 N6 60.0(4) 3_565 2_665 ?
C14 N6 C13 44(10) 3_565 . ?
C13' N6' C15' 122(10) . . ?
C13' N6' C14' 122(10) . . ?
C15' N6' C14' 116(10) . . ?
C13' N6' C14' 83(10) . 14_456 ?
C15' N6' C14' 79(10) . 14_456 ?
C14' N6' C14' 108(9) . 14_456 ?
C13' N6' C15' 57(10) . 15_556 ?
C15' N6' C15' 153(10) . 15_556 ?
C14' N6' C15' 72(9) . 15_556 ?
C14' N6' C15' 74(10) 14_456 15_556 ?
C15' O1' C13' 82(10) 15_556 . ?
N4 C1 C2 123.0(6) . . ?
N4 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C1 C2 C3 119.2(6) . . ?
C1 C2 H2 120.4 . . ?
C3 C2 H2 120.4 . . ?
C4 C3 C2 119.5(7) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C4 C5 119.0(6) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
N4 C5 C4 121.7(5) . . ?
N4 C5 C6 113.5(5) . . ?
C4 C5 C6 124.7(5) . . ?
N1 C6 N3 113.1(5) . . ?
N1 C6 C5 118.8(5) . . ?
N3 C6 C5 128.1(5) . . ?
N3 C7 N2 115.6(4) . . ?
N3 C7 C8 125.0(5) . . ?
N2 C7 C8 119.4(5) . . ?
C12 C8 C9 117.2(4) . . ?
C12 C8 C7 121.8(5) . . ?
C9 C8 C7 121.0(5) . . ?
C10 C9 C8 120.0(5) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
N5 C10 C9 123.6(5) . . ?
N5 C10 H10 118.2 . . ?
C9 C10 H10 118.2 . . ?
N5 C11 C12 123.5(5) . . ?
N5 C11 H11 118.2 . . ?
C12 C11 H11 118.2 . . ?
C8 C12 C11 119.6(5) . . ?
C8 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
O1 C13 N6 113(10) . . ?
C14 C14 C14 60.00(8) 2_665 3_565 ?
C14 C14 H14C 143.9 2_665 . ?
C15 C15 C15 60.0(6) 3_565 2_665 ?
C15 C15 C15 90.0(2) 3_565 15 ?
C15 C15 C15 90.0(3) 2_665 14_455 ?
C14 C15 N6 140(10) 14_455 . ?
O1' C13' C15' 47(9) . 15_556 ?
N6' C13' C15' 78(10) . 15_556 ?
O1' C13' C14' 117(10) . 14_456 ?
N6' C13' C14' 54(10) . 14_456 ?
C15' C13' C14' 71(10) 15_556 14_456 ?
N6' C14' N6' 110(10) . 15_556 ?
N6' C14' C13' 43(8) 15_556 15_556 ?
N6' C14' C15' 63(7) . 15_556 ?
N6' C14' C15' 48(9) 15_556 15_556 ?
C13' C14' C15' 78(10) 15_556 15_556 ?
H14D C14' H14E 109.5 . . ?
H14D C14' H14F 109.5 . . ?
H14E C14' H14F 109.5 . . ?
O1' C15' C13' 51(10) 14_456 14_456 ?
N6' C15' C13' 139(10) . 14_456 ?
O1' C15' N6' 89(10) 14_456 14_456 ?
N6' C15' N6' 98(10) . 14_456 ?
C13' C15' N6' 45(8) 14_456 14_456 ?
O1' C15' C14' 111(10) 14_456 14_456 ?
N6' C15' C14' 53(10) . 14_456 ?
C13' C15' C14' 88(10) 14_456 14_456 ?
N6' C15' C14' 46(7) 14_456 14_456 ?
H15D C15' H15E 109.5 . . ?
O1' C15' H15F 90.6 14_456 . ?
H15D C15' H15F 109.5 . . ?
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
Co1 N1 2.033(4) . ?
Co1 N1 2.033(4) 10_675 ?
Co1 N4 2.177(5) 10_675 ?
Co1 N4 2.177(5) . ?
Co1 N5 2.208(4) 5_664 ?
Co1 N5 2.208(4) 17_455 ?
N1 C6 1.338(6) . ?
N1 N2 1.357(5) . ?
N2 C7 1.348(6) . ?
N3 C7 1.340(6) . ?
N3 C6 1.341(6) . ?
N4 C1 1.334(7) . ?
N4 C5 1.365(6) . ?
N5 C10 1.321(6) . ?
N5 C11 1.337(6) . ?
N5 Co1 2.208(4) 9_565 ?
N6 C15 0.6(10) 15 ?
N6 C15 0.7(16) 14_455 ?
N6 C14 0.8(13) 3_565 ?
N6 N6 1.1(10) 3_565 ?
N6 N6 1.1(10) 2_665 ?
N6 C15 1.1(7) 13_565 ?
N6 C13 1.3(12) . ?
N6 C14 1.5(7) . ?
N6 C15 1.5(6) . ?
N6 C14 1.6(10) 2_665 ?
N6 C15 1.7(8) 2_665 ?
N6 C15 1.8(5) 3_565 ?
O1 C13 1.2(3) . ?
O1 C14 1.4(5) 3_565 ?
N6' C13' 1.3(2) . ?
N6' C15' 1.5(2) . ?
N6' C14' 1.47(15) . ?
N6' C14' 1.57(18) 14_456 ?
N6' C15' 1.8(2) 15_556 ?
O1' C15' 1.14(17) 15_556 ?
O1' C13' 1.2(2) . ?
C1 C2 1.366(8) . ?
C1 H1 0.9300 . ?
C2 C3 1.381(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.359(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.391(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.452(7) . ?
C7 C8 1.474(6) . ?
C8 C12 1.362(7) . ?
C8 C9 1.372(7) . ?
C9 C10 1.363(7) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.370(7) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 0.9(6) 3_565 ?
C13 H13 0.9300 . ?
C14 N6 0.8(13) 2_665 ?
C14 C13 0.9(6) 2_665 ?
C14 C15 1.3(19) 15 ?
C14 C15 1.3(9) 13_565 ?
C14 O1 1.4(5) 2_665 ?
C14 C14 1.5(8) 2_665 ?
C14 C14 1.5(8) 3_565 ?
C14 N6 1.6(10) 3_565 ?
C14 C15 1.7(8) 14_455 ?
C14 H14B 0.9600 . ?
C15 N6 0.6(10) 14_455 ?
C15 N6 0.7(16) 15 ?
C15 C15 0.8(19) 3_565 ?
C15 C15 0.8(19) 2_665 ?
C15 N6 1.1(7) 13_565 ?
C15 C15 1(2) 15 ?
C15 C15 1(2) 14_455 ?
C15 C14 1.3(19) 14_455 ?
C15 C14 1.3(9) 13_565 ?
C15 C15 1(3) 13_565 ?
C15 C14 1.7(8) 15 ?
C13' C15' 1.6(2) 15_556 ?
C13' H13' 0.9300 . ?
C14' N6' 1.57(18) 15_556 ?
C14' H14D 0.9600 . ?
C14' H14E 0.9600 . ?
C14' H14F 0.9600 . ?
C15' O1' 1.14(17) 14_456 ?
C15' C13' 1.6(2) 14_456 ?
C15' N6' 1.8(2) 14_456 ?
C15' H15D 0.9600 . ?
C15' H15E 0.9600 . ?
