#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/75/1517579.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_1517579
loop_
_publ_author_name
'Ling-Yan Pang'
'Ping Liu'
'Cui-Ping Zhang'
'Xin Chen'
'Bo Chen'
'Yao-Yu Wang'
'Qi-Zhen Shi'
_publ_section_title
;
 Four cobalt(II) complexes constructed from a butterfly-shaped
 tetracarboxylic acid with N-donor ligands: Structures, magnetism and
 influence of coordination modes on dihedral angles
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              43
_journal_page_last               52
_journal_volume                  403
_journal_year                    2013
_chemical_formula_sum            'C80 H54 Co3 N6 O18'
_chemical_formula_weight         1564.08
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                110.57(2)
_cell_angle_beta                 109.52(2)
_cell_angle_gamma                102.764(15)
_cell_formula_units_Z            1
_cell_length_a                   12.082(9)
_cell_length_b                   13.647(10)
_cell_length_c                   14.324(18)
_cell_measurement_temperature    296(2)
_cell_volume                     1925(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0904
_diffrn_reflns_av_sigmaI/netI    0.2863
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9735
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  0.849
_exptl_absorpt_correction_T_min  0.637
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             801
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.934
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.817
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         6793
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.817
_refine_ls_R_factor_all          0.2026
_refine_ls_R_factor_gt           0.0908
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2051
_refine_ls_wR_factor_ref         0.2472
_reflns_number_gt                2366
_reflns_number_total             6793
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-403-43-52-4.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               1517579
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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 1.0000 0.5000 0.0000 0.0324(5) Uani 1 2 d S
Co2 Co 0.61517(12) 0.42306(11) -0.09812(12) 0.0360(4) Uani 1 1 d .
N3 N 1.0065(7) 0.6609(7) 0.0148(8) 0.040(2) Uani 1 1 d .
N1 N 0.6168(6) 0.2697(6) -0.0933(7) 0.037(2) Uani 1 1 d .
N2 N 0.6144(7) 0.5809(7) -0.0980(7) 0.038(2) Uani 1 1 d .
O1 O 0.9059(6) 0.5031(5) 0.1015(6) 0.0426(18) Uani 1 1 d .
O5 O 0.4271(5) 0.3676(6) -0.1399(6) 0.0415(17) Uani 1 1 d .
H15 H 0.3858 0.3475 -0.2065 0.062 Uiso 1 1 calc R
O6 O 0.8799(6) 0.7266(5) 0.2672(6) 0.0460(19) Uani 1 1 d .
H5 H 0.8647 0.7808 0.2625 0.069 Uiso 1 1 calc R
O4 O 0.6230(6) 0.3836(5) -0.2452(6) 0.0418(17) Uani 1 1 d .
O9 O 0.8885(6) -0.0888(5) 0.2734(7) 0.055(2) Uani 1 1 d .
C17 C 0.9844(9) 0.6823(8) -0.0727(9) 0.042(3) Uani 1 1 d .
H22 H 0.9676 0.6239 -0.1401 0.050 Uiso 1 1 calc R
C19 C 0.7946(8) 0.4452(7) 0.5012(9) 0.034(2) Uani 1 1 d .
C21 C 0.8113(7) 0.4627(7) 0.4104(8) 0.028(2) Uani 1 1 d .
O8 O 0.6818(7) -0.1409(6) 0.2305(7) 0.061(2) Uani 1 1 d .
C24 C 0.6414(9) 0.1898(8) -0.1654(9) 0.042(3) Uani 1 1 d .
H12 H 0.6513 0.2009 -0.2230 0.050 Uiso 1 1 calc R
O2 O 0.7133(6) 0.5071(5) 0.0678(6) 0.0405(17) Uani 1 1 d .
O3 O 0.8256(6) 0.4220(6) -0.1452(6) 0.0487(19) Uani 1 1 d .
C33 C 0.8315(7) 0.4040(7) 0.2386(8) 0.028(2) Uani 1 1 d .
H6 H 0.8381 0.3498 0.1816 0.033 Uiso 1 1 calc R
C34 C 0.6243(9) 0.7780(9) -0.1251(10) 0.040(3) Uani 1 1 d .
C37 C 0.8316(7) 0.5049(8) 0.2349(9) 0.030(2) Uani 1 1 d .
O7 O 0.8205(7) 0.7700(6) 0.4034(7) 0.061(2) Uani 1 1 d .
C42 C 0.7028(9) 0.7809(8) -0.0285(9) 0.044(3) Uani 1 1 d .
H18 H 0.7626 0.8505 0.0309 0.053 Uiso 1 1 calc R
C43 C 0.8163(8) 0.5636(8) 0.4074(8) 0.038(2) Uani 1 1 d .
H4 H 0.8103 0.6185 0.4643 0.046 Uiso 1 1 calc R
C44 C 0.8221(8) 0.3804(8) 0.3237(8) 0.034(2) Uani 1 1 d .
C45 C 0.6959(9) 0.6842(8) -0.0169(9) 0.041(3) Uani 1 1 d .
H17 H 0.7507 0.6911 0.0508 0.049 Uiso 1 1 calc R
C48 C 0.6365(9) 1.0777(8) -0.0711(10) 0.044(3) Uani 1 1 d .
C49 C 0.8177(8) 0.2691(7) 0.3150(8) 0.030(2) Uani 1 1 d .
C53 C 0.7953(8) 0.0479(8) 0.2792(9) 0.037(3) Uani 1 1 d .
C54 C 0.6422(9) 0.9770(9) -0.0593(10) 0.048(3) Uani 1 1 d .
H20 H 0.6602 0.9821 0.0110 0.057 Uiso 1 1 calc R
C57 C 0.9845(9) 0.7846(9) -0.0707(10) 0.050(3) Uani 1 1 d .
H23 H 0.9625 0.7920 -0.1359 0.060 Uiso 1 1 calc R
C58 C 0.7564(9) 0.4188(8) -0.3242(9) 0.040(3) Uani 1 1 d .
C60 C 0.8624(8) 0.3971(8) 0.5571(8) 0.033(2) Uani 1 1 d .
H3 H 0.9201 0.3720 0.5363 0.039 Uiso 1 1 calc R
C61 C 0.5973(8) 0.2476(8) -0.0168(8) 0.038(3) Uani 1 1 d .
H11 H 0.5744 0.2974 0.0292 0.046 Uiso 1 1 calc R
C62 C 0.6245(8) 0.8789(8) -0.1377(10) 0.047(3) Uani 1 1 d .
H21 H 0.6110 0.8744 -0.2072 0.056 Uiso 1 1 calc R
C63 C 0.8445(9) 0.7056(8) 0.3363(9) 0.043(3) Uani 1 1 d .
C66 C 0.9129(9) 0.2329(8) 0.3060(9) 0.043(3) Uani 1 1 d .
H7 H 0.9833 0.2813 0.3092 0.052 Uiso 1 1 calc R
C69 C 0.5356(9) 0.5770(9) -0.1936(10) 0.047(3) Uani 1 1 d .
H16 H 0.4777 0.5063 -0.2523 0.056 Uiso 1 1 calc R
C76 C 0.7014(8) 0.0847(8) 0.2889(10) 0.048(3) Uani 1 1 d .
H9 H 0.6307 0.0363 0.2853 0.057 Uiso 1 1 calc R
C77 C 0.8188(9) 0.5093(8) 0.1296(9) 0.040(3) Uani 1 1 d .
C78 C 0.8298(8) 0.5885(7) 0.3231(8) 0.029(2) Uani 1 1 d .
C82 C 0.7090(8) 0.1910(8) 0.3038(9) 0.042(3) Uani 1 1 d .
H10 H 0.6417 0.2123 0.3066 0.050 Uiso 1 1 calc R
C84 C 1.0184(8) 0.8768(7) 0.0314(10) 0.039(3) Uani 1 1 d .
C85 C 0.5357(10) 0.6707(9) -0.2094(10) 0.047(3) Uani 1 1 d .
H19 H 0.4771 0.6627 -0.2760 0.056 Uiso 1 1 calc R
C86 C 0.6081(8) 0.1563(8) 0.0008(9) 0.040(3) Uani 1 1 d .
H14 H 0.5969 0.1474 0.0589 0.048 Uiso 1 1 calc R
C88 C 1.0223(8) 0.9876(9) 0.0413(9) 0.044(3) Uani 1 1 d .
H24 H 1.0602 1.0471 0.1134 0.052 Uiso 1 1 calc R
C91 C 0.7401(10) 0.4084(7) -0.2301(10) 0.038(3) Uani 1 1 d .
C95 C 0.6859(9) 0.4658(8) -0.3831(8) 0.041(3) Uani 1 1 d .
H95 H 0.6252 0.4877 -0.3648 0.050 Uiso 1 1 calc R
C97 C 0.6517(9) 0.0965(8) -0.1570(10) 0.046(3) Uani 1 1 d .
H13 H 0.6688 0.0452 -0.2077 0.056 Uiso 1 1 calc R
C98 C 1.0368(9) 0.7526(9) 0.1133(10) 0.043(3) Uani 1 1 d .
H26 H 1.0552 0.7436 0.1775 0.052 Uiso 1 1 calc R
C101 C 0.8446(8) 0.3867(8) 0.6428(9) 0.040(3) Uani 1 1 d .
H1 H 0.8935 0.3567 0.6810 0.048 Uiso 1 1 calc R
C103 C 0.7888(10) -0.0685(8) 0.2621(10) 0.048(3) Uani 1 1 d .
C104 C 0.7060(10) 0.4792(9) 0.5334(10) 0.052(3) Uani 1 1 d .
H2 H 0.6598 0.5119 0.4966 0.063 Uiso 1 1 calc R
C106 C 0.9060(10) 0.1252(9) 0.2920(10) 0.057(3) Uani 1 1 d .
H8 H 0.9738 0.1039 0.2911 0.069 Uiso 1 1 calc R
C108 C 1.0409(8) 0.8529(8) 0.1205(10) 0.046(3) Uani 1 1 d .
H25 H 1.0599 0.9104 0.1893 0.056 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'
Co Co 0.3494 0.9721 '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'
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
O3 Co1 O3 180.0(4) . 2_765
O3 Co1 N3 89.8(3) . 2_765
O3 Co1 N3 90.2(3) 2_765 2_765
O3 Co1 N3 90.2(3) . .
O3 Co1 N3 89.8(3) 2_765 .
N3 Co1 N3 180.000(1) 2_765 .
O3 Co1 O1 88.6(3) . 2_765
O3 Co1 O1 91.4(3) 2_765 2_765
N3 Co1 O1 92.8(3) 2_765 2_765
N3 Co1 O1 87.2(3) . 2_765
O3 Co1 O1 91.4(3) . .
O3 Co1 O1 88.6(3) 2_765 .
N3 Co1 O1 87.2(3) 2_765 .
N3 Co1 O1 92.8(3) . .
O1 Co1 O1 180.000(1) 2_765 .
O2 Co2 O4 145.9(3) . .
O2 Co2 O5 108.7(3) . .
O4 Co2 O5 104.9(3) . .
O2 Co2 N1 89.9(3) . .
O4 Co2 N1 96.6(3) . .
O5 Co2 N1 88.9(3) . .
O2 Co2 N2 88.5(3) . .
O4 Co2 N2 85.0(3) . .
O5 Co2 N2 91.0(3) . .
N1 Co2 N2 178.3(3) . .
C17 N3 C98 114.4(8) . .
C17 N3 Co1 121.5(7) . .
C98 N3 Co1 124.1(7) . .
C61 N1 C24 115.9(8) . .
C61 N1 Co2 120.3(7) . .
C24 N1 Co2 123.8(6) . .
C45 N2 C69 115.5(8) . .
C45 N2 Co2 125.9(7) . .
C69 N2 Co2 118.1(7) . .
C77 O1 Co1 156.1(6) . .
C91 O4 Co2 110.9(7) . .
N3 C17 C57 125.2(11) . .
C60 C19 C104 118.2(9) . .
C60 C19 C21 123.2(7) . .
C104 C19 C21 118.7(8) . .
C43 C21 C44 117.3(9) . .
C43 C21 C19 119.3(8) . .
C44 C21 C19 123.4(7) . .
C97 C24 N1 123.7(10) . .
C77 O2 Co2 128.3(7) . .
C91 O3 Co1 159.4(6) . .
C37 C33 C44 123.3(9) . .
C42 C34 C85 115.5(9) . .
C42 C34 C62 123.3(10) . .
C85 C34 C62 121.1(10) . .
C78 C37 C33 118.5(9) . .
C78 C37 C77 124.3(8) . .
C33 C37 C77 116.9(9) . .
C34 C42 C45 122.0(10) . .
C21 C43 C78 124.0(9) . .
C33 C44 C21 118.5(8) . .
C33 C44 C49 117.8(9) . .
C21 C44 C49 123.7(8) . .
N2 C45 C42 123.1(10) . .
C86 C48 C97 117.8(9) 1_565 1_565
C86 C48 C54 119.9(10) 1_565 .
C97 C48 C54 122.2(10) 1_565 .
C66 C49 C82 117.8(8) . .
C66 C49 C44 121.1(7) . .
C82 C49 C44 120.8(7) . .
C76 C53 C106 118.4(9) . .
C76 C53 C103 122.5(8) . .
C106 C53 C103 119.0(8) . .
C62 C54 C48 127.1(11) . .
C17 C57 C84 118.8(10) . .
C101 C58 C95 116.6(8) 1_554 .
C101 C58 C91 122.2(8) 1_554 .
C95 C58 C91 121.2(9) . .
C101 C60 C19 120.0(8) . .
N1 C61 C86 125.2(9) . .
C54 C62 C34 125.9(11) . .
O7 C63 O6 125.4(9) . .
O7 C63 C78 121.9(9) . .
O6 C63 C78 112.7(9) . .
C49 C66 C106 121.2(8) . .
N2 C69 C85 124.2(10) . .
C82 C76 C53 121.5(8) . .
O1 C77 O2 123.9(9) . .
O1 C77 C37 118.7(8) . .
O2 C77 C37 117.0(8) . .
C37 C78 C43 118.2(8) . .
C37 C78 C63 124.0(9) . .
C43 C78 C63 117.7(9) . .
C76 C82 C49 121.0(8) . .
C108 C84 C57 115.0(9) . .
C108 C84 C88 122.5(10) . .
C57 C84 C88 122.4(10) . .
C69 C85 C34 119.7(10) . .
C61 C86 C48 118.1(9) . 1_545
C88 C88 C84 126.8(14) 2_775 .
O3 C91 O4 121.9(9) . .
O3 C91 C58 125.1(9) . .
O4 C91 C58 113.0(10) . .
C104 C95 C58 120.4(9) 1_554 .
C24 C97 C48 119.2(10) . 1_545
C108 C98 N3 122.9(10) . .
C60 C101 C58 123.1(8) . 1_556
O8 C103 O9 124.8(9) . .
O8 C103 C53 117.1(9) . .
O9 C103 C53 118.0(8) . .
C95 C104 C19 121.8(9) 1_556 .
C66 C106 C53 119.9(9) . .
C98 C108 C84 123.6(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O3 2.104(7) .
Co1 O3 2.104(7) 2_765
Co1 N3 2.111(8) 2_765
Co1 N3 2.111(8) .
Co1 O1 2.119(7) 2_765
Co1 O1 2.119(7) .
Co2 O2 1.993(7) .
Co2 O4 2.024(7) .
Co2 O5 2.027(6) .
Co2 N1 2.123(7) .
Co2 N2 2.156(7) .
N3 C17 1.341(12) .
N3 C98 1.379(13) .
N1 C61 1.312(11) .
N1 C24 1.377(11) .
N2 C45 1.333(11) .
N2 C69 1.356(12) .
O1 C77 1.254(10) .
O6 C63 1.294(11) .
O4 C91 1.303(10) .
O9 C103 1.266(11) .
C17 C57 1.386(12) .
C19 C60 1.382(11) .
C19 C104 1.405(11) .
C19 C21 1.471(12) .
C21 C43 1.383(11) .
C21 C44 1.419(13) .
O8 C103 1.258(11) .
C24 C97 1.349(11) .
O2 C77 1.274(10) .
O3 C91 1.223(11) .
C33 C37 1.396(10) .
C33 C44 1.398(12) .
C34 C42 1.372(13) .
C34 C85 1.396(13) .
C34 C62 1.451(12) .
C37 C78 1.384(13) .
C37 C77 1.488(13) .
O7 C63 1.218(11) .
C42 C45 1.377(12) .
C43 C78 1.413(12) .
C44 C49 1.467(11) .
C48 C86 1.397(13) 1_565
C48 C97 1.403(14) 1_565
C48 C54 1.456(12) .
C49 C66 1.375(11) .
C49 C82 1.417(11) .
C53 C76 1.367(11) .
C53 C106 1.418(12) .
C53 C103 1.498(12) .
C54 C62 1.325(14) .
C57 C84 1.404(14) .
C58 C101 1.396(12) 1_554
C58 C95 1.411(12) .
C58 C91 1.474(13) .
C60 C101 1.363(12) .
C61 C86 1.379(11) .
C63 C78 1.504(12) .
C66 C106 1.390(12) .
C69 C85 1.375(12) .
C76 C82 1.367(12) .
C84 C108 1.382(14) .
C84 C88 1.456(12) .
C86 C48 1.397(13) 1_545
C88 C88 1.320(17) 2_775
C95 C104 1.362(13) 1_554
C97 C48 1.403(14) 1_545
C98 C108 1.325(12) .
C101 C58 1.396(12) 1_556
C104 C95 1.362(13) 1_556
