#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:27:48 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180340 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/09/7200978.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_7200978
loop_
_publ_author_name
'Walsh, David P.'
'Clérac, Rodolphe'
'Hearns, Nigel G. R.'
'Kruger, Paul E.'
'Schmitt, Wolfgang'
_publ_section_title
;
 Modulating topologies and magnetic properties of coordination polymers
 using 2,2′-bipyridine and 5-aminodiacetic isophthalic acid as
 ligands
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              1666
_journal_paper_doi               10.1039/b902010a
_journal_volume                  11
_journal_year                    2009
_chemical_formula_sum            'C22 H29 Co2 N3 O15'
_chemical_formula_weight         693.34
_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                103.8970(10)
_cell_angle_beta                 105.9730(10)
_cell_angle_gamma                107.5480(10)
_cell_formula_units_Z            2
_cell_length_a                   10.1987(7)
_cell_length_b                   12.1765(8)
_cell_length_c                   12.6676(8)
_cell_measurement_reflns_used    114
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.26
_cell_volume                     1349.43(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0495
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18836
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    1.310
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.515
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         6713
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0370
_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)+(0.0604P)²+0.8475P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1082
_reflns_number_gt                6024
_reflns_number_total             6713
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b902010a.txt
_cod_data_source_block           dwcu2m
_cod_original_cell_volume        1349.43(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7200978
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 -0.43233(3) -0.53945(2) 0.39977(2) 0.01446(8) Uani 1 1 d . . .
Co2 Co 0.18759(3) -0.14002(2) 0.15257(3) 0.01890(9) Uani 1 1 d . . .
O5 O -0.00537(18) -0.28237(14) 0.12820(16) 0.0278(4) Uani 1 1 d . . .
O3 O -0.57507(16) -0.45437(13) 0.43620(12) 0.0178(3) Uani 1 1 d . . .
O1 O -0.60173(16) -0.70565(13) 0.31341(13) 0.0209(3) Uani 1 1 d . . .
O2 O -0.83137(17) -0.80781(15) 0.18112(15) 0.0282(4) Uani 1 1 d . . .
C2 C -0.4499(2) -0.61931(18) 0.09768(17) 0.0170(4) Uani 1 1 d . . .
H2 H -0.5196 -0.6941 0.0891 0.020 Uiso 1 1 calc R . .
N1 N -0.54715(18) -0.51324(15) 0.22784(15) 0.0151(3) Uani 1 1 d . . .
O6 O -0.13629(18) -0.17843(14) 0.18411(16) 0.0282(4) Uani 1 1 d . . .
C12 C -0.6236(2) -0.39744(18) 0.37122(18) 0.0179(4) Uani 1 1 d . . .
C1 C -0.4488(2) -0.50956(17) 0.16461(16) 0.0151(3) Uani 1 1 d . . .
C8 C -0.1175(2) -0.27682(18) 0.14782(19) 0.0200(4) Uani 1 1 d . . .
C6 C -0.2407(2) -0.50689(19) 0.05907(19) 0.0206(4) Uani 1 1 d . . .
H6 H -0.1712 -0.5059 0.0244 0.025 Uiso 1 1 calc R . .
C10 C -0.5700(2) -0.39892(18) 0.26976(18) 0.0172(4) Uani 1 1 d . . .
H10A H -0.6428 -0.3930 0.2059 0.021 Uiso 1 1 calc R . .
H10B H -0.4775 -0.3284 0.2955 0.021 Uiso 1 1 calc R . .
O4 O -0.7035(2) -0.34371(19) 0.38718(17) 0.0373(5) Uani 1 1 d . . .
C5 C -0.2377(2) -0.39727(18) 0.12627(18) 0.0175(4) Uani 1 1 d . . .
C3 C -0.3432(2) -0.39857(18) 0.17679(17) 0.0166(4) Uani 1 1 d . . .
H3 H -0.3432 -0.3246 0.2190 0.020 Uiso 1 1 calc R . .
C11 C -0.7083(2) -0.71861(18) 0.22629(18) 0.0181(4) Uani 1 1 d . . .
C9 C -0.6918(2) -0.61969(18) 0.17046(18) 0.0173(4) Uani 1 1 d . . .
H9A H -0.7069 -0.6573 0.0890 0.021 Uiso 1 1 calc R . .
H9B H -0.7697 -0.5898 0.1714 0.021 Uiso 1 1 calc R . .
C4 C -0.3478(2) -0.61832(18) 0.04356(17) 0.0169(4) Uani 1 1 d . . .
C7 C -0.3498(2) -0.73632(18) -0.03041(18) 0.0181(4) Uani 1 1 d . . .
O8 O -0.45749(18) -0.83620(14) -0.05692(16) 0.0286(4) Uani 1 1 d . . .
N3 N -0.23670(19) -0.38280(16) 0.44995(15) 0.0178(3) Uani 1 1 d . . .
O7 O -0.24310(18) -0.72663(14) -0.06323(16) 0.0267(3) Uani 1 1 d . . .
N2 N -0.28397(19) -0.61549(16) 0.36012(16) 0.0194(3) Uani 1 1 d . . .
O13 O 0.38371(18) 0.00511(14) 0.17263(15) 0.0259(3) Uani 1 1 d D . .
O10 O 0.13690(19) -0.00551(14) 0.25177(16) 0.0265(3) Uani 1 1 d D . .
O12 O 0.0882(2) -0.11500(18) -0.00092(18) 0.0381(4) Uani 1 1 d D . .
C17 C -0.1290(2) -0.40427(19) 0.41644(18) 0.0189(4) Uani 1 1 d . . .
C22 C -0.3171(3) -0.7366(2) 0.3153(2) 0.0265(4) Uani 1 1 d . . .
H22 H -0.4032 -0.7920 0.3149 0.032 Uiso 1 1 calc R . .
O11 O 0.3008(3) -0.15151(18) 0.31127(18) 0.0444(5) Uani 1 1 d D . .
C13 C -0.2164(2) -0.2661(2) 0.5021(2) 0.0235(4) Uani 1 1 d . . .
H13 H -0.2888 -0.2512 0.5274 0.028 Uiso 1 1 calc R . .
C15 C 0.0164(3) -0.1885(2) 0.4828(2) 0.0326(5) Uani 1 1 d . . .
H15 H 0.1002 -0.1232 0.4923 0.039 Uiso 1 1 calc R . .
C21 C -0.2273(3) -0.7818(2) 0.2695(2) 0.0330(5) Uani 1 1 d . . .
H21 H -0.2539 -0.8661 0.2375 0.040 Uiso 1 1 calc R . .
C19 C -0.0611(3) -0.5743(2) 0.3210(2) 0.0271(5) Uani 1 1 d . . .
H19 H 0.0264 -0.5173 0.3251 0.033 Uiso 1 1 calc R . .
C16 C -0.0010(2) -0.3084(2) 0.4315(2) 0.0269(5) Uani 1 1 d . . .
H16 H 0.0716 -0.3249 0.4075 0.032 Uiso 1 1 calc R . .
C18 C -0.1571(2) -0.53550(19) 0.36359(17) 0.0189(4) Uani 1 1 d . . .
C14 C -0.0912(3) -0.1664(2) 0.5198(2) 0.0295(5) Uani 1 1 d . . .
H14 H -0.0803 -0.0863 0.5558 0.035 Uiso 1 1 calc R . .
C20 C -0.0979(3) -0.6999(2) 0.2720(2) 0.0323(5) Uani 1 1 d . . .
H20 H -0.0363 -0.7283 0.2414 0.039 Uiso 1 1 calc R . .
O23 O 0.2795(2) 0.08295(17) -0.02684(18) 0.0342(4) Uani 1 1 d D . .
O21 O -0.3122(3) -0.0934(2) 0.2923(2) 0.0516(5) Uani 1 1 d D . .
O22 O 0.3788(4) 0.0590(4) 0.5094(5) 0.0454(10) Uani 0.50 1 d PD . .
O20 O -0.9363(4) -0.5099(4) 0.1313(4) 0.0407(9) Uani 0.50 1 d P . .
H22A H 0.389(8) 0.082(6) 0.459(4) 0.049 Uiso 0.50 1 d PD . .
H11A H 0.318(4) -0.098(2) 0.373(2) 0.049 Uiso 1 1 d D . .
H11B H 0.296(4) -0.212(2) 0.333(3) 0.049 Uiso 1 1 d D . .
H10C H 0.142(3) 0.056(2) 0.230(3) 0.049 Uiso 1 1 d D . .
H10D H 0.045(2) -0.042(3) 0.229(3) 0.049 Uiso 1 1 d D . .
H13A H 0.419(4) -0.030(3) 0.127(3) 0.049 Uiso 1 1 d D . .
H13B H 0.368(4) 0.055(3) 0.138(3) 0.049 Uiso 1 1 d D . .
H12A H 0.126(3) -0.054(2) -0.021(3) 0.049 Uiso 1 1 d D . .
H12B H 0.001(2) -0.138(3) -0.049(3) 0.049 Uiso 1 1 d D . .
H23A H 0.235(3) 0.113(3) -0.069(3) 0.049 Uiso 1 1 d D . .
H23B H 0.361(2) 0.103(3) -0.037(3) 0.049 Uiso 1 1 d D . .
H22B H 0.408(8) 0.108(4) 0.567(3) 0.049 Uiso 0.50 1 d PD . .
H21A H -0.392(3) -0.112(3) 0.231(2) 0.049 Uiso 1 1 d D . .
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
O1 Co1 O3 93.33(6) . 2_446 ?
O1 Co1 N2 90.28(7) . . ?
O3 Co1 N2 105.99(6) 2_446 . ?
O1 Co1 N3 163.57(7) . . ?
O3 Co1 N3 100.05(6) 2_446 . ?
N2 Co1 N3 76.96(7) . . ?
O1 Co1 O3 92.12(6) . . ?
O3 Co1 O3 76.44(6) 2_446 . ?
N2 Co1 O3 176.49(6) . . ?
N3 Co1 O3 100.21(6) . . ?
O1 Co1 N1 79.53(6) . . ?
O3 Co1 N1 149.60(6) 2_446 . ?
N2 Co1 N1 103.58(6) . . ?
N3 Co1 N1 93.30(6) . . ?
O3 Co1 N1 74.36(5) . . ?
O7 Co2 O12 91.40(8) 2_545 . ?
O7 Co2 O5 86.99(6) 2_545 . ?
O12 Co2 O5 92.77(7) . . ?
O7 Co2 O11 90.17(8) 2_545 . ?
O12 Co2 O11 175.48(8) . . ?
O5 Co2 O11 91.54(8) . . ?
O7 Co2 O10 176.94(7) 2_545 . ?
O12 Co2 O10 91.65(8) . . ?
O5 Co2 O10 92.98(6) . . ?
O11 Co2 O10 86.77(8) . . ?
O7 Co2 O13 92.39(6) 2_545 . ?
O12 Co2 O13 85.84(7) . . ?
O5 Co2 O13 178.46(7) . . ?
O11 Co2 O13 89.86(8) . . ?
O10 Co2 O13 87.72(6) . . ?
C8 O5 Co2 129.17(14) . . ?
C12 O3 Co1 134.83(13) . 2_446 ?
C12 O3 Co1 120.45(12) . . ?
Co1 O3 Co1 103.56(6) 2_446 . ?
C11 O1 Co1 119.05(13) . . ?
C4 C2 C1 120.81(17) . . ?
C1 N1 C10 116.47(15) . . ?
C1 N1 C9 115.22(15) . . ?
C10 N1 C9 109.82(15) . . ?
C1 N1 Co1 106.17(11) . . ?
C10 N1 Co1 103.40(11) . . ?
C9 N1 Co1 104.20(11) . . ?
O4 C12 O3 124.87(18) . . ?
O4 C12 C10 120.56(18) . . ?
O3 C12 C10 114.56(17) . . ?
C3 C1 C2 118.74(17) . . ?
C3 C1 N1 121.38(17) . . ?
C2 C1 N1 119.65(16) . . ?
O5 C8 O6 124.98(19) . . ?
O5 C8 C5 116.60(18) . . ?
O6 C8 C5 118.41(18) . . ?
C5 C6 C4 119.91(18) . . ?
N1 C10 C12 110.65(15) . . ?
C6 C5 C3 120.11(18) . . ?
C6 C5 C8 119.97(18) . . ?
C3 C5 C8 119.90(18) . . ?
C5 C3 C1 120.62(18) . . ?
O2 C11 O1 124.47(19) . . ?
O2 C11 C9 116.10(18) . . ?
O1 C11 C9 119.42(17) . . ?
N1 C9 C11 115.07(16) . . ?
C6 C4 C2 119.75(18) . . ?
C6 C4 C7 119.07(17) . . ?
C2 C4 C7 121.17(17) . . ?
O7 C7 O8 124.66(19) . . ?
O7 C7 C4 116.21(17) . . ?
O8 C7 C4 119.12(18) . . ?
C13 N3 C17 118.59(18) . . ?
C13 N3 Co1 125.77(14) . . ?
C17 N3 Co1 115.39(14) . . ?
C7 O7 Co2 130.60(14) . 2_545 ?
C22 N2 C18 118.73(18) . . ?
C22 N2 Co1 124.53(15) . . ?
C18 N2 Co1 115.89(14) . . ?
N3 C17 C16 121.7(2) . . ?
N3 C17 C18 115.40(17) . . ?
C16 C17 C18 122.91(19) . . ?
N2 C22 C21 122.2(2) . . ?
N3 C13 C14 122.5(2) . . ?
C14 C15 C16 119.5(2) . . ?
C20 C21 C22 119.1(2) . . ?
C18 C19 C20 118.9(2) . . ?
C15 C16 C17 118.9(2) . . ?
N2 C18 C19 122.1(2) . . ?
N2 C18 C17 114.71(18) . . ?
C19 C18 C17 123.18(19) . . ?
C15 C14 C13 118.7(2) . . ?
C21 C20 C19 119.0(2) . . ?
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 O1 2.0163(15) . ?
Co1 O3 2.0787(14) 2_446 ?
Co1 N2 2.1068(17) . ?
Co1 N3 2.1090(17) . ?
Co1 O3 2.1107(14) . ?
Co1 N1 2.3177(17) . ?
Co2 O7 2.0645(15) 2_545 ?
Co2 O12 2.0706(18) . ?
Co2 O5 2.0794(15) . ?
Co2 O11 2.085(2) . ?
Co2 O10 2.0996(16) . ?
Co2 O13 2.1357(16) . ?
O5 C8 1.253(3) . ?
O3 C12 1.288(2) . ?
O3 Co1 2.0787(14) 2_446 ?
O1 C11 1.256(3) . ?
O2 C11 1.251(2) . ?
C2 C4 1.394(3) . ?
C2 C1 1.395(3) . ?
N1 C1 1.443(2) . ?
N1 C10 1.477(2) . ?
N1 C9 1.480(2) . ?
O6 C8 1.267(3) . ?
C12 O4 1.218(3) . ?
C12 C10 1.527(3) . ?
C1 C3 1.393(3) . ?
C8 C5 1.506(3) . ?
C6 C5 1.387(3) . ?
C6 C4 1.390(3) . ?
C5 C3 1.393(3) . ?
C11 C9 1.527(3) . ?
C4 C7 1.506(3) . ?
C7 O7 1.251(2) . ?
C7 O8 1.263(2) . ?
N3 C13 1.340(3) . ?
N3 C17 1.353(3) . ?
O7 Co2 2.0645(15) 2_545 ?
N2 C22 1.343(3) . ?
N2 C18 1.347(3) . ?
C17 C16 1.393(3) . ?
C17 C18 1.479(3) . ?
C22 C21 1.386(3) . ?
C13 C14 1.390(3) . ?
C15 C14 1.377(4) . ?
C15 C16 1.383(4) . ?
C21 C20 1.380(4) . ?
C19 C18 1.385(3) . ?
C19 C20 1.391(4) . ?
