#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:46:10 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179305 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/02/4320200.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_4320200
loop_
_publ_author_name
'Ponnaiyan Ayyappan'
'Owen R. Evans'
'Wenbin Lin'
_publ_section_title
;
 Three-Dimensional Open Frameworks Based on Cobalt(II) and Nickel(II)
 m-Pyridinecarboxylates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4627
_journal_page_last               4632
_journal_paper_doi               10.1021/ic010343d
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C25 H24 Co2 N4 O9'
_chemical_formula_weight         642.34
_chemical_name_systematic
;
   ?
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.6450(10)
_cell_angle_beta                 101.9770(10)
_cell_angle_gamma                112.0780(10)
_cell_formula_units_Z            2
_cell_length_a                   10.53440(10)
_cell_length_b                   11.9073(2)
_cell_length_c                   14.0461(3)
_cell_measurement_temperature    198(2)
_cell_volume                     1462.40(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(2)
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.903
_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  0.0553
_diffrn_reflns_av_sigmaI/netI    0.0849
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9384
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    1.189
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             656
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.0039(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6525
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.1245
_refine_ls_R_factor_gt           0.0740
_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)+(0.0221P)²+5.8730P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1630
_reflns_number_gt                4478
_reflns_number_total             6525
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010343d_1.cif
_cod_data_source_block           Compound1
_cod_original_cell_volume        1462.39(4)
_cod_database_code               4320200
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.19149(8) -0.00864(7) 0.21280(5) 0.0235(2) Uani 1 1 d . . .
Co2 Co 0.55129(8) 0.27080(7) 0.31163(5) 0.0236(2) Uani 1 1 d . . .
O1 O 0.4012(4) 0.3005(4) 0.3818(3) 0.0319(9) Uani 1 1 d . . .
O2 O 0.2152(4) 0.1112(4) 0.3602(3) 0.0297(9) Uani 1 1 d . . .
O3 O 0.5973(5) 0.0705(4) 0.4237(3) 0.0465(12) Uani 1 1 d . . .
O4 O 0.6665(4) 0.2843(4) 0.4565(3) 0.0306(9) Uani 1 1 d . . .
O5 O 0.2159(4) 0.1358(4) 0.1508(3) 0.0298(9) Uani 1 1 d . . .
O6 O 0.4466(4) 0.2541(4) 0.1623(3) 0.0291(9) Uani 1 1 d . . .
O7 O 0.1610(4) -0.1336(4) 0.0598(3) 0.0292(9) Uani 1 1 d . . .
O8 O 0.3918(4) -0.0805(5) 0.0692(3) 0.0455(12) Uani 1 1 d . . .
O9 O 0.4252(4) 0.0602(4) 0.2584(3) 0.0277(9) Uani 1 1 d . . .
H9A H 0.436(9) 0.025(8) 0.210(7) 0.06(3) Uiso 1 1 d . . .
H9B H 0.476(9) 0.045(8) 0.311(7) 0.08(3) Uiso 1 1 d . . .
N1 N 0.3293(5) 0.5177(4) 0.6310(3) 0.0269(10) Uani 1 1 d . . .
N2 N 0.8360(5) 0.1624(5) 0.7321(3) 0.0282(10) Uani 1 1 d . . .
N3 N 0.0395(5) 0.0714(5) -0.1581(3) 0.0277(10) Uani 1 1 d . . .
N4 N 0.2786(5) -0.2489(4) -0.2516(3) 0.0267(10) Uani 1 1 d . . .
C1 C 0.2996(6) 0.2333(5) 0.4061(4) 0.0255(11) Uani 1 1 d . . .
C2 C 0.2758(6) 0.3076(6) 0.5019(4) 0.0293(12) Uani 1 1 d . . .
C3 C 0.1996(9) 0.2432(7) 0.5556(6) 0.058(2) Uani 1 1 d . . .
H3 H 0.1542 0.1494 0.5301 0.070 Uiso 1 1 calc R . .
C4 C 0.1911(11) 0.3184(7) 0.6468(6) 0.071(3) Uani 1 1 d . . .
H4 H 0.1388 0.2769 0.6849 0.085 Uiso 1 1 calc R . .
C5 C 0.2589(8) 0.4536(6) 0.6820(5) 0.0489(19) Uani 1 1 d . . .
H5 H 0.2551 0.5040 0.7464 0.059 Uiso 1 1 calc R . .
C6 C 0.3362(6) 0.4436(5) 0.5416(4) 0.0243(11) Uani 1 1 d . . .
H6 H 0.3858 0.4877 0.5036 0.029 Uiso 1 1 calc R . .
C7 C 0.6669(6) 0.1906(6) 0.4813(4) 0.0310(13) Uani 1 1 d . . .
C8 C 0.7629(6) 0.2300(6) 0.5939(4) 0.0330(13) Uani 1 1 d . . .
C9 C 0.8561(7) 0.3619(6) 0.6622(5) 0.0442(17) Uani 1 1 d . . .
H9 H 0.8618 0.4304 0.6388 0.053 Uiso 1 1 calc R . .
C10 C 0.9402(8) 0.3924(6) 0.7644(5) 0.0494(19) Uani 1 1 d . . .
H10 H 1.0063 0.4816 0.8117 0.059 Uiso 1 1 calc R . .
C11 C 0.9260(7) 0.2910(6) 0.7960(5) 0.0391(15) Uani 1 1 d . . .
H11 H 0.9827 0.3125 0.8668 0.047 Uiso 1 1 calc R . .
C12 C 0.7572(6) 0.1345(6) 0.6321(4) 0.0279(12) Uani 1 1 d . . .
H12 H 0.6944 0.0443 0.5856 0.033 Uiso 1 1 calc R . .
C13 C 0.3092(6) 0.1830(5) 0.1118(4) 0.0256(12) Uani 1 1 d . . .
C14 C 0.2526(6) 0.1497(5) -0.0056(4) 0.0255(11) Uani 1 1 d . . .
C15 C 0.3375(6) 0.1513(6) -0.0689(5) 0.0364(14) Uani 1 1 d . . .
H15 H 0.4396 0.1806 -0.0389 0.044 Uiso 1 1 calc R . .
C16 C 0.2688(7) 0.1088(7) -0.1779(5) 0.0426(16) Uani 1 1 d . . .
H16 H 0.3232 0.1059 -0.2239 0.051 Uiso 1 1 calc R . .
C17 C 0.1218(6) 0.0712(6) -0.2182(4) 0.0363(14) Uani 1 1 d . . .
H17 H 0.0768 0.0438 -0.2925 0.044 Uiso 1 1 calc R . .
C18 C 0.1054(6) 0.1089(5) -0.0537(4) 0.0250(11) Uani 1 1 d . . .
H18 H 0.0473 0.1072 -0.0102 0.030 Uiso 1 1 calc R . .
C19 C 0.2569(6) -0.1307(5) 0.0196(4) 0.0278(12) Uani 1 1 d . . .
C20 C 0.2076(6) -0.1892(5) -0.1001(4) 0.0250(11) Uani 1 1 d . . .
C21 C 0.0665(6) -0.2310(6) -0.1667(4) 0.0290(12) Uani 1 1 d . . .
H21 H -0.0067 -0.2262 -0.1384 0.035 Uiso 1 1 calc R . .
C22 C 0.0354(6) -0.2801(6) -0.2757(4) 0.0338(14) Uani 1 1 d . . .
H22 H -0.0594 -0.3074 -0.3232 0.041 Uiso 1 1 calc R . .
C23 C 0.1420(6) -0.2891(6) -0.3145(4) 0.0301(13) Uani 1 1 d . . .
H23 H 0.1179 -0.3254 -0.3893 0.036 Uiso 1 1 calc R . .
C24 C 0.3097(6) -0.1978(5) -0.1460(4) 0.0292(12) Uani 1 1 d . . .
H24 H 0.4071 -0.1658 -0.1004 0.035 Uiso 1 1 calc R . .
O10 O 1.3999(6) 0.6107(5) 1.1887(4) 0.69(3) Uiso 1 1 d R A 1
C25 C 1.4509(6) 0.5062(5) 1.0962(4) 0.188(14) Uiso 0.605(18) 1 d PR . 1
C26 C 1.5862(6) 0.4963(5) 1.0361(4) 0.230(18) Uiso 0.605(18) 1 d PR . 1
O11 O 1.2719(6) 0.5504(5) 1.0522(4) 0.372(12) Uiso 1 1 d R . 2
C28 C 1.3253(6) 0.4785(5) 1.2459(4) 0.176(19) Uiso 0.395(18) 1 d PR . 2
C27 C 1.2762(6) 0.4683(5) 1.1154(4) 0.154(17) Uiso 0.395(18) 1 d PR . 2
O12 O 1.2928(6) 0.5234(5) 0.9467(4) 0.205(16) Uiso 0.53(3) 1 d PR . .
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
_geom_angle_publ_flag
O2 Co1 O5 94.19(15) . . ?
O2 Co1 O7 178.45(15) . . ?
O5 Co1 O7 85.79(15) . . ?
O2 Co1 N2 88.72(16) . 2_656 ?
O5 Co1 N2 177.07(16) . 2_656 ?
O7 Co1 N2 91.29(16) . 2_656 ?
O2 Co1 N3 90.60(16) . 2 ?
O5 Co1 N3 87.49(16) . 2 ?
O7 Co1 N3 87.84(16) . 2 ?
N2 Co1 N3 92.13(17) 2_656 2 ?
O2 Co1 O9 91.64(16) . . ?
O5 Co1 O9 88.57(16) . . ?
O7 Co1 O9 89.91(15) . . ?
N2 Co1 O9 91.70(17) 2_656 . ?
N3 Co1 O9 175.60(17) 2 . ?
O4 Co2 O6 175.85(16) . . ?
O4 Co2 O1 86.79(16) . . ?
O6 Co2 O1 97.34(15) . . ?
O4 Co2 N1 88.62(16) . 2_666 ?
O6 Co2 N1 91.93(16) . 2_666 ?
O1 Co2 N1 86.95(16) . 2_666 ?
O4 Co2 O9 90.87(16) . . ?
O6 Co2 O9 88.77(16) . . ?
O1 Co2 O9 90.35(15) . . ?
N1 Co2 O9 177.27(17) 2_666 . ?
O4 Co2 N4 89.08(16) . 2_655 ?
O6 Co2 N4 86.81(15) . 2_655 ?
O1 Co2 N4 175.34(15) . 2_655 ?
N1 Co2 N4 90.82(17) 2_666 2_655 ?
O9 Co2 N4 91.86(16) . 2_655 ?
C1 O1 Co2 137.0(4) . . ?
C1 O2 Co1 124.9(3) . . ?
C7 O4 Co2 127.5(3) . . ?
C13 O5 Co1 128.2(4) . . ?
C13 O6 Co2 123.3(3) . . ?
C19 O7 Co1 127.3(3) . . ?
Co2 O9 Co1 113.88(19) . . ?
C5 N1 C6 116.7(5) . . ?
C5 N1 Co2 124.7(4) . 2_666 ?
C6 N1 Co2 118.3(4) . 2_666 ?
C12 N2 C11 117.1(5) . . ?
C12 N2 Co1 120.6(4) . 2_656 ?
C11 N2 Co1 122.2(4) . 2_656 ?
C17 N3 C18 117.2(5) . . ?
C17 N3 Co1 126.3(4) . 2 ?
C18 N3 Co1 116.5(3) . 2 ?
C23 N4 C24 117.2(5) . . ?
C23 N4 Co2 123.6(3) . 2_655 ?
C24 N4 Co2 119.1(3) . 2_655 ?
O1 C1 O2 127.6(5) . . ?
O1 C1 C2 116.4(5) . . ?
O2 C1 C2 116.0(5) . . ?
C6 C2 C3 117.8(5) . . ?
C6 C2 C1 120.3(5) . . ?
C3 C2 C1 121.8(5) . . ?
C4 C3 C2 118.5(6) . . ?
C5 C4 C3 119.3(6) . . ?
N1 C5 C4 123.5(6) . . ?
N1 C6 C2 124.0(5) . . ?
O3 C7 O4 127.0(5) . . ?
O3 C7 C8 116.9(5) . . ?
O4 C7 C8 116.0(5) . . ?
C12 C8 C9 118.0(5) . . ?
C12 C8 C7 120.1(5) . . ?
C9 C8 C7 121.8(5) . . ?
C10 C9 C8 119.4(6) . . ?
C11 C10 C9 118.5(6) . . ?
N2 C11 C10 123.5(5) . . ?
N2 C12 C8 123.4(5) . . ?
O5 C13 O6 125.8(5) . . ?
O5 C13 C14 116.4(5) . . ?
O6 C13 C14 117.9(5) . . ?
C18 C14 C15 118.2(5) . . ?
C18 C14 C13 117.8(5) . . ?
C15 C14 C13 124.0(5) . . ?
C14 C15 C16 118.1(5) . . ?
C17 C16 C15 119.5(5) . . ?
N3 C17 C16 123.0(5) . . ?
N3 C18 C14 124.1(5) . . ?
O7 C19 O8 126.2(5) . . ?
O7 C19 C20 117.4(5) . . ?
O8 C19 C20 116.4(5) . . ?
C24 C20 C21 118.2(5) . . ?
C24 C20 C19 118.2(5) . . ?
C21 C20 C19 123.6(5) . . ?
C22 C21 C20 118.2(5) . . ?
C23 C22 C21 119.7(5) . . ?
N4 C23 C22 122.9(5) . . ?
N4 C24 C20 123.7(5) . . ?
C26 C25 C26 64.3(3) 2_867 . ?
C26 C25 O10 116.7(3) 2_867 . ?
C26 C25 O10 147.5 . . ?
O12 C26 C25 103.4(6) 2_867 2_867 ?
O12 C26 C25 140.5(4) 2_867 . ?
C25 C26 C25 115.7(3) 2_867 . ?
O12 C26 C26 160.9(7) 2_867 2_867 ?
C25 C26 C26 58.3(3) 2_867 2_867 ?
C25 C26 C26 57.4(3) . 2_867 ?
O12 O11 C27 123.9 . . ?
O11 C27 C28 142.4 . . ?
C26 O12 O11 103.3(4) 2_867 . ?
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 O2 2.052(4) . ?
Co1 O5 2.098(4) . ?
Co1 O7 2.111(3) . ?
Co1 N2 2.131(5) 2_656 ?
Co1 N3 2.144(4) 2 ?
Co1 O9 2.161(4) . ?
Co2 O4 2.069(4) . ?
Co2 O6 2.072(4) . ?
Co2 O1 2.112(4) . ?
Co2 N1 2.147(4) 2_666 ?
Co2 O9 2.150(4) . ?
Co2 N4 2.200(5) 2_655 ?
O1 C1 1.251(6) . ?
O2 C1 1.255(6) . ?
O3 C7 1.242(7) . ?
O4 C7 1.261(7) . ?
O5 C13 1.251(6) . ?
O6 C13 1.274(6) . ?
O7 C19 1.251(6) . ?
O8 C19 1.255(7) . ?
N1 C5 1.325(7) . ?
N1 C6 1.346(6) . ?
N1 Co2 2.147(4) 2_666 ?
N2 C12 1.346(6) . ?
N2 C11 1.348(7) . ?
N2 Co1 2.131(5) 2_656 ?
N3 C17 1.330(7) . ?
N3 C18 1.342(6) . ?
N3 Co1 2.144(4) 2 ?
N4 C23 1.340(7) . ?
N4 C24 1.345(6) . ?
N4 Co2 2.200(5) 2_655 ?
C1 C2 1.510(7) . ?
C2 C6 1.378(7) . ?
C2 C3 1.386(8) . ?
C3 C4 1.379(9) . ?
C4 C5 1.371(9) . ?
C7 C8 1.516(7) . ?
C8 C12 1.377(8) . ?
C8 C9 1.393(8) . ?
C9 C10 1.382(8) . ?
C10 C11 1.369(9) . ?
C13 C14 1.508(7) . ?
C14 C18 1.381(7) . ?
C14 C15 1.384(8) . ?
C15 C16 1.395(8) . ?
C16 C17 1.375(8) . ?
C19 C20 1.508(7) . ?
C20 C24 1.384(7) . ?
C20 C21 1.390(7) . ?
C21 C22 1.389(7) . ?
C22 C23 1.371(8) . ?
O10 C25 1.8407 . ?
C25 C26 1.807(10) 2_867 ?
C25 C26 1.8244 . ?
C26 O12 1.368(10) 2_867 ?
C26 C25 1.807(10) 2_867 ?
C26 C26 1.933(10) 2_867 ?
O11 O12 1.5043 . ?
O11 C27 1.5044 . ?
C28 C27 1.7535 . ?
O12 C26 1.368(10) 2_867 ?
