# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2012
data_global
_journal_name_full CrystEngComm
_journal_coden_cambridge 1350
_journal_year ?
_journal_volume ?
_journal_page_first ?
_publ_author_name 'Jianqiang Liu'
_publ_contact_author_name 'Jianqiang Liu '
_publ_contact_author_email jianqiangliu2010@126.com
data_1
_database_code_depnum_ccdc_archive 'CCDC 843286'
#TrackingRef '- All cif.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C29 H32 Co N4 O6'
_chemical_formula_sum 'C29 H32 Co N4 O6'
_chemical_formula_weight 591.52
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'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M p-1
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 8.2543(11)
_cell_length_b 12.6631(16)
_cell_length_c 14.1054(18)
_cell_angle_alpha 99.035(2)
_cell_angle_beta 98.947(2)
_cell_angle_gamma 95.887(2)
_cell_volume 1426.1(3)
_cell_formula_units_Z 2
_cell_measurement_temperature 298(2)
_cell_measurement_reflns_used 5015
_cell_measurement_theta_min 2.01
_cell_measurement_theta_max 25.19
_exptl_crystal_description block
_exptl_crystal_colour pink
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.12
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.377
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 618
_exptl_absorpt_coefficient_mu 0.650
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.8543
_exptl_absorpt_correction_T_max 0.9260
_exptl_absorpt_process_details SADABS
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 298(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker APEX SMART II'
_diffrn_measurement_method \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% ?
_diffrn_reflns_number 7189
_diffrn_reflns_av_R_equivalents 0.0223
_diffrn_reflns_av_sigmaI/netI 0.0483
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_theta_min 2.01
_diffrn_reflns_theta_max 25.19
_reflns_number_total 5003
_reflns_number_gt 3795
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2004)'
_computing_cell_refinement APEX2
_computing_data_reduction APEX2
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics APEX2
_computing_publication_material APEX2
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+0.0100P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 5003
_refine_ls_number_parameters 363
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0604
_refine_ls_R_factor_gt 0.0435
_refine_ls_wR_factor_ref 0.1498
_refine_ls_wR_factor_gt 0.1306
_refine_ls_goodness_of_fit_ref 0.851
_refine_ls_restrained_S_all 0.851
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
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
C23 C 0.5028(4) 0.0488(2) 0.5399(3) 0.0604(8) Uani 1 1 d . . .
H23A H 0.4856 0.0235 0.5994 0.073 Uiso 1 1 calc R . .
H23B H 0.6123 0.0896 0.5521 0.073 Uiso 1 1 calc R . .
C29 C -0.0442(4) 0.5311(3) 0.0369(3) 0.0686(10) Uani 1 1 d . . .
H29A H -0.1172 0.5741 0.0036 0.082 Uiso 1 1 calc R . .
H29B H -0.1120 0.4801 0.0637 0.082 Uiso 1 1 calc R . .
C28 C 0.0735(5) 0.6046(3) 0.1199(3) 0.0691(10) Uani 1 1 d . . .
H28A H 0.1446 0.6539 0.0934 0.083 Uiso 1 1 calc R . .
H28B H 0.0103 0.6471 0.1604 0.083 Uiso 1 1 calc R . .
O5 O 0.7346(3) 1.33171(19) 1.19006(18) 0.0692(6) Uani 1 1 d . . .
C17 C 0.6556(5) 1.2709(3) 1.1122(3) 0.0657(9) Uani 1 1 d . . .
C14 C 0.7603(4) 1.2135(3) 1.0481(3) 0.0601(8) Uani 1 1 d . . .
C13 C 0.9301(4) 1.2223(3) 1.0729(2) 0.0592(8) Uani 1 1 d . . .
H13 H 0.9815 1.2623 1.1331 0.071 Uiso 1 1 calc R . .
C12 C 1.0261(4) 1.1738(3) 1.0116(2) 0.0618(8) Uani 1 1 d . . .
H12 H 1.1404 1.1805 1.0302 0.074 Uiso 1 1 calc R . .
C15 C 0.6856(5) 1.1508(3) 0.9597(3) 0.0759(11) Uani 1 1 d . . .
H15 H 0.5710 1.1415 0.9424 0.091 Uiso 1 1 calc R . .
C16 C 0.7787(5) 1.1023(3) 0.8973(3) 0.0819(12) Uani 1 1 d . . .
H16 H 0.7265 1.0607 0.8380 0.098 Uiso 1 1 calc R . .
C11 C 0.9492(4) 1.1146(3) 0.9213(3) 0.0660(9) Uani 1 1 d . . .
O4 O 1.0286(3) 1.0691(2) 0.85063(19) 0.0840(8) Uani 1 1 d . . .
C10 C 1.2064(4) 1.0755(3) 0.8708(3) 0.0698(10) Uani 1 1 d . . .
H10A H 1.2400 1.0279 0.9156 0.084 Uiso 1 1 calc R . .
H10B H 1.2558 1.1486 0.8995 0.084 Uiso 1 1 calc R . .
C9 C 1.2591(5) 1.0417(3) 0.7745(3) 0.0700(10) Uani 1 1 d . . .
H9A H 1.3788 1.0476 0.7845 0.084 Uiso 1 1 calc R . .
H9B H 1.2248 1.0908 0.7313 0.084 Uiso 1 1 calc R . .
C8 C 1.1876(4) 0.9267(3) 0.7253(2) 0.0606(8) Uani 1 1 d . . .
H8A H 1.2592 0.8759 0.7470 0.073 Uiso 1 1 calc R . .
H8B H 1.0790 0.9082 0.7410 0.073 Uiso 1 1 calc R . .
Co1 Co 0.59437(4) 0.39951(3) 0.27507(3) 0.04542(17) Uani 1 1 d . . .
N3 N 0.3814(3) 0.4631(2) 0.24018(17) 0.0487(6) Uani 1 1 d . . .
O1 O 0.7416(3) 0.49323(17) 0.38681(16) 0.0574(6) Uani 1 1 d . . .
O2 O 0.7632(3) 0.58423(19) 0.26786(17) 0.0638(6) Uani 1 1 d . . .
C20 C 0.4984(3) 0.2599(2) 0.4264(2) 0.0483(7) Uani 1 1 d . . .
O3 O 1.1763(3) 0.92379(18) 0.62286(16) 0.0649(6) Uani 1 1 d . . .
C1 C 0.7965(4) 0.5756(2) 0.3551(2) 0.0487(7) Uani 1 1 d . . .
N2 N 0.3968(3) 0.16975(19) 0.4296(2) 0.0541(7) Uani 1 1 d . . .
N4 N 0.1766(3) 0.5432(2) 0.18054(19) 0.0567(7) Uani 1 1 d . . .
C7 C 0.9582(4) 0.7600(2) 0.3982(2) 0.0516(7) Uani 1 1 d . . .
H7 H 0.9331 0.7669 0.3331 0.062 Uiso 1 1 calc R . .
C2 C 0.9043(3) 0.6642(2) 0.4269(2) 0.0428(6) Uani 1 1 d . . .
C3 C 0.9497(4) 0.6540(2) 0.5237(2) 0.0478(7) Uani 1 1 d . . .
H3 H 0.9172 0.5896 0.5434 0.057 Uiso 1 1 calc R . .
N1 N 0.4947(3) 0.27346(19) 0.33473(19) 0.0516(6) Uani 1 1 d . . .
C4 C 1.0424(4) 0.7380(2) 0.5914(2) 0.0521(7) Uani 1 1 d . . .
H4 H 1.0729 0.7299 0.6559 0.063 Uiso 1 1 calc R . .
C5 C 1.0892(4) 0.8341(2) 0.5623(2) 0.0495(7) Uani 1 1 d . . .
C18 C 0.3870(4) 0.1887(3) 0.2777(3) 0.0625(9) Uani 1 1 d . . .
H18 H 0.3598 0.1773 0.2101 0.075 Uiso 1 1 calc R . .
C22 C 0.3760(4) 0.1232(3) 0.5158(3) 0.0645(9) Uani 1 1 d . . .
H22A H 0.2662 0.0832 0.5053 0.077 Uiso 1 1 calc R . .
H22B H 0.3845 0.1810 0.5710 0.077 Uiso 1 1 calc R . .
C6 C 1.0483(4) 0.8446(2) 0.4649(2) 0.0531(8) Uani 1 1 d . . .
H6 H 1.0818 0.9089 0.4451 0.064 Uiso 1 1 calc R . .
C26 C 0.3364(4) 0.5290(3) 0.1801(2) 0.0559(8) Uani 1 1 d . . .
C24 C 0.2436(4) 0.4356(3) 0.2802(2) 0.0556(8) Uani 1 1 d . . .
H24 H 0.2390 0.3904 0.3259 0.067 Uiso 1 1 calc R . .
O6 O 0.5040(4) 1.2584(3) 1.0884(2) 0.0953(9) Uani 1 1 d . . .
C21 C 0.5905(4) 0.3340(3) 0.5145(2) 0.0587(8) Uani 1 1 d . . .
H21A H 0.6661 0.2960 0.5508 0.088 Uiso 1 1 calc R . .
H21B H 0.5140 0.3603 0.5544 0.088 Uiso 1 1 calc R . .
H21C H 0.6511 0.3936 0.4954 0.088 Uiso 1 1 calc R . .
C25 C 0.1188(4) 0.4837(3) 0.2432(2) 0.0592(8) Uani 1 1 d . . .
H25 H 0.0124 0.4779 0.2576 0.071 Uiso 1 1 calc R . .
C19 C 0.3276(4) 0.1251(3) 0.3357(3) 0.0655(9) Uani 1 1 d . . .
H19 H 0.2530 0.0624 0.3156 0.079 Uiso 1 1 calc R . .
C27 C 0.4431(5) 0.5786(4) 0.1188(3) 0.1023(17) Uani 1 1 d . . .
H27A H 0.5356 0.5392 0.1132 0.153 Uiso 1 1 calc R . .
H27B H 0.4825 0.6522 0.1484 0.153 Uiso 1 1 calc R . .
H27C H 0.3802 0.5764 0.0551 0.153 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C23 0.058(2) 0.0555(18) 0.081(2) 0.0270(16) 0.0323(17) 0.0149(15)
C29 0.052(2) 0.090(3) 0.066(2) 0.0250(19) -0.0026(16) 0.0202(18)
C28 0.061(2) 0.080(2) 0.069(2) 0.0198(19) 0.0026(17) 0.0262(18)
O5 0.0723(16) 0.0637(14) 0.0725(16) -0.0022(12) 0.0293(13) 0.0102(12)
C17 0.070(2) 0.068(2) 0.066(2) 0.0143(18) 0.0274(19) 0.0122(18)
C14 0.058(2) 0.0574(18) 0.064(2) 0.0028(15) 0.0155(16) 0.0095(15)
C13 0.062(2) 0.0567(18) 0.0547(19) -0.0039(15) 0.0100(15) 0.0101(15)
C12 0.0520(19) 0.066(2) 0.061(2) -0.0034(16) 0.0042(15) 0.0093(16)
C15 0.049(2) 0.089(3) 0.080(3) -0.011(2) 0.0099(18) 0.0055(18)
C16 0.057(2) 0.095(3) 0.075(3) -0.031(2) 0.0042(19) 0.004(2)
C11 0.057(2) 0.070(2) 0.065(2) -0.0113(17) 0.0099(17) 0.0138(17)
O4 0.0542(15) 0.1036(19) 0.0775(17) -0.0343(14) 0.0084(12) 0.0146(13)
C10 0.054(2) 0.076(2) 0.070(2) -0.0150(18) 0.0091(17) 0.0090(17)
C9 0.062(2) 0.068(2) 0.070(2) -0.0123(17) 0.0131(18) 0.0014(17)
C8 0.058(2) 0.0609(19) 0.058(2) -0.0057(15) 0.0113(15) 0.0079(15)
Co1 0.0374(3) 0.0491(3) 0.0485(3) 0.00606(18) 0.00588(17) 0.00619(17)
N3 0.0382(13) 0.0608(15) 0.0473(14) 0.0109(12) 0.0058(11) 0.0072(11)
O1 0.0548(13) 0.0483(11) 0.0645(14) 0.0089(10) 0.0052(10) -0.0047(10)
O2 0.0548(14) 0.0752(15) 0.0547(14) 0.0049(11) -0.0004(11) 0.0028(11)
C20 0.0403(16) 0.0423(15) 0.065(2) 0.0115(13) 0.0124(13) 0.0111(12)
O3 0.0717(16) 0.0562(13) 0.0574(14) -0.0036(10) 0.0097(11) -0.0129(11)
C1 0.0369(15) 0.0535(17) 0.0550(19) 0.0036(14) 0.0086(13) 0.0109(13)
N2 0.0461(15) 0.0450(13) 0.0757(19) 0.0159(13) 0.0182(13) 0.0066(11)
N4 0.0431(15) 0.0718(17) 0.0568(16) 0.0162(13) 0.0025(12) 0.0173(12)
C7 0.0496(18) 0.0554(17) 0.0531(18) 0.0155(14) 0.0104(14) 0.0116(14)
C2 0.0354(15) 0.0433(15) 0.0497(17) 0.0047(12) 0.0106(12) 0.0061(12)
C3 0.0479(17) 0.0453(15) 0.0515(17) 0.0093(13) 0.0131(13) 0.0039(13)
N1 0.0456(15) 0.0471(14) 0.0589(16) 0.0059(12) 0.0028(12) 0.0056(11)
C4 0.0526(18) 0.0554(18) 0.0477(17) 0.0074(14) 0.0103(14) 0.0040(14)
C5 0.0439(17) 0.0474(16) 0.0543(18) -0.0011(13) 0.0127(13) 0.0010(13)
C18 0.057(2) 0.0533(18) 0.069(2) 0.0052(16) -0.0024(16) 0.0010(15)
C22 0.061(2) 0.0522(18) 0.093(3) 0.0204(17) 0.0401(19) 0.0134(15)
C6 0.0526(18) 0.0449(16) 0.062(2) 0.0118(14) 0.0156(15) -0.0031(13)
C26 0.0449(18) 0.072(2) 0.0524(18) 0.0184(16) 0.0056(14) 0.0069(15)
C24 0.0477(18) 0.0655(19) 0.0607(19) 0.0204(15) 0.0179(14) 0.0140(15)
O6 0.0657(19) 0.128(3) 0.094(2) 0.0036(18) 0.0275(15) 0.0272(17)
C21 0.065(2) 0.0528(17) 0.0577(19) 0.0075(14) 0.0134(16) 0.0035(15)
C25 0.0436(18) 0.075(2) 0.063(2) 0.0143(17) 0.0170(15) 0.0132(15)
C19 0.055(2) 0.0462(17) 0.090(3) 0.0060(17) 0.0068(18) -0.0012(15)
C27 0.061(3) 0.166(5) 0.099(3) 0.083(3) 0.015(2) 0.015(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
C23 C22 1.514(4) . ?
C23 C23 1.525(7) 2_656 ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C29 C28 1.516(5) . ?
C29 C29 1.529(8) 2_565 ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C28 N4 1.476(4) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
O5 C17 1.278(4) . ?
O5 Co1 1.956(2) 1_566 ?
C17 O6 1.231(4) . ?
C17 C14 1.502(5) . ?
C14 C13 1.379(5) . ?
C14 C15 1.384(5) . ?
C13 C12 1.379(5) . ?
C13 H13 0.9300 . ?
C12 C11 1.392(5) . ?
C12 H12 0.9300 . ?
C15 C16 1.372(5) . ?
C15 H15 0.9300 . ?
C16 C11 1.382(5) . ?
C16 H16 0.9300 . ?
C11 O4 1.362(4) . ?
O4 C10 1.442(4) . ?
C10 C9 1.502(5) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C9 C8 1.526(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C8 O3 1.428(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
Co1 O5 1.956(2) 1_544 ?
Co1 O1 1.973(2) . ?
Co1 N3 2.031(2) . ?
Co1 N1 2.074(3) . ?
N3 C26 1.319(4) . ?
N3 C24 1.383(4) . ?
O1 C1 1.267(4) . ?
O2 C1 1.243(4) . ?
C20 N1 1.327(4) . ?
C20 N2 1.356(4) . ?
C20 C21 1.482(4) . ?
O3 C5 1.369(3) . ?
C1 C2 1.495(4) . ?
N2 C19 1.365(4) . ?
N2 C22 1.458(4) . ?
N4 C26 1.350(4) . ?
N4 C25 1.357(4) . ?
C7 C6 1.374(4) . ?
C7 C2 1.390(4) . ?
C7 H7 0.9300 . ?
C2 C3 1.388(4) . ?
C3 C4 1.385(4) . ?
C3 H3 0.9300 . ?
N1 C18 1.379(4) . ?
C4 C5 1.381(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.393(4) . ?
C18 C19 1.345(5) . ?
C18 H18 0.9300 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C6 H6 0.9300 . ?
C26 C27 1.488(5) . ?
C24 C25 1.329(4) . ?
C24 H24 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C25 H25 0.9300 . ?
C19 H19 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
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
C22 C23 C23 114.2(4) . 2_656 ?
C22 C23 H23A 108.7 . . ?
C23 C23 H23A 108.7 2_656 . ?
C22 C23 H23B 108.7 . . ?
C23 C23 H23B 108.7 2_656 . ?
H23A C23 H23B 107.6 . . ?
C28 C29 C29 113.2(4) . 2_565 ?
C28 C29 H29A 108.9 . . ?
C29 C29 H29A 108.9 2_565 . ?
C28 C29 H29B 108.9 . . ?
C29 C29 H29B 108.9 2_565 . ?
H29A C29 H29B 107.8 . . ?
N4 C28 C29 111.9(3) . . ?
N4 C28 H28A 109.2 . . ?
C29 C28 H28A 109.2 . . ?
N4 C28 H28B 109.2 . . ?
C29 C28 H28B 109.2 . . ?
H28A C28 H28B 107.9 . . ?
C17 O5 Co1 114.6(2) . 1_566 ?
O6 C17 O5 124.1(3) . . ?
O6 C17 C14 120.3(4) . . ?
O5 C17 C14 115.6(3) . . ?
C13 C14 C15 118.0(3) . . ?
C13 C14 C17 122.5(3) . . ?
C15 C14 C17 119.4(3) . . ?
C12 C13 C14 122.2(3) . . ?
C12 C13 H13 118.9 . . ?
C14 C13 H13 118.9 . . ?
C13 C12 C11 118.9(3) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
C16 C15 C14 120.8(3) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C15 C16 C11 120.8(3) . . ?
C15 C16 H16 119.6 . . ?
C11 C16 H16 119.6 . . ?
O4 C11 C16 115.3(3) . . ?
O4 C11 C12 125.4(3) . . ?
C16 C11 C12 119.2(3) . . ?
C11 O4 C10 118.9(3) . . ?
O4 C10 C9 106.2(3) . . ?
O4 C10 H10A 110.5 . . ?
C9 C10 H10A 110.5 . . ?
O4 C10 H10B 110.5 . . ?
C9 C10 H10B 110.5 . . ?
H10A C10 H10B 108.7 . . ?
C10 C9 C8 113.5(3) . . ?
C10 C9 H9A 108.9 . . ?
C8 C9 H9A 108.9 . . ?
C10 C9 H9B 108.9 . . ?
C8 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
O3 C8 C9 106.5(3) . . ?
O3 C8 H8A 110.4 . . ?
C9 C8 H8A 110.4 . . ?
O3 C8 H8B 110.4 . . ?
C9 C8 H8B 110.4 . . ?
H8A C8 H8B 108.6 . . ?
O5 Co1 O1 107.44(10) 1_544 . ?
O5 Co1 N3 129.74(10) 1_544 . ?
O1 Co1 N3 110.86(10) . . ?
O5 Co1 N1 103.78(10) 1_544 . ?
O1 Co1 N1 103.97(9) . . ?
N3 Co1 N1 97.31(10) . . ?
C26 N3 C24 105.9(3) . . ?
C26 N3 Co1 133.2(2) . . ?
C24 N3 Co1 120.9(2) . . ?
C1 O1 Co1 106.19(19) . . ?
N1 C20 N2 110.1(3) . . ?
N1 C20 C21 126.3(3) . . ?
N2 C20 C21 123.5(3) . . ?
C5 O3 C8 117.2(2) . . ?
O2 C1 O1 122.3(3) . . ?
O2 C1 C2 120.1(3) . . ?
O1 C1 C2 117.6(3) . . ?
C20 N2 C19 107.2(3) . . ?
C20 N2 C22 126.7(3) . . ?
C19 N2 C22 125.8(3) . . ?
C26 N4 C25 107.9(3) . . ?
C26 N4 C28 128.0(3) . . ?
C25 N4 C28 123.9(3) . . ?
C6 C7 C2 120.8(3) . . ?
C6 C7 H7 119.6 . . ?
C2 C7 H7 119.6 . . ?
C3 C2 C7 118.5(3) . . ?
C3 C2 C1 121.1(3) . . ?
C7 C2 C1 120.4(3) . . ?
C4 C3 C2 121.2(3) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C20 N1 C18 106.4(3) . . ?
C20 N1 Co1 131.8(2) . . ?
C18 N1 Co1 121.3(2) . . ?
C5 C4 C3 119.3(3) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
O3 C5 C4 124.8(3) . . ?
O3 C5 C6 115.1(3) . . ?
C4 C5 C6 120.1(3) . . ?
C19 C18 N1 109.0(3) . . ?
C19 C18 H18 125.5 . . ?
N1 C18 H18 125.5 . . ?
N2 C22 C23 112.9(3) . . ?
N2 C22 H22A 109.0 . . ?
C23 C22 H22A 109.0 . . ?
N2 C22 H22B 109.0 . . ?
C23 C22 H22B 109.0 . . ?
H22A C22 H22B 107.8 . . ?
C7 C6 C5 119.9(3) . . ?
C7 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
N3 C26 N4 109.9(3) . . ?
N3 C26 C27 125.6(3) . . ?
N4 C26 C27 124.6(3) . . ?
C25 C24 N3 109.6(3) . . ?
C25 C24 H24 125.2 . . ?
N3 C24 H24 125.2 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C24 C25 N4 106.8(3) . . ?
C24 C25 H25 126.6 . . ?
N4 C25 H25 126.6 . . ?
C18 C19 N2 107.3(3) . . ?
C18 C19 H19 126.3 . . ?
N2 C19 H19 126.3 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full 25.19
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max 0.246
_refine_diff_density_min -0.310
_refine_diff_density_rms 0.048
#===END
data_2
_database_code_depnum_ccdc_archive 'CCDC 843287'
#TrackingRef '- All cif.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C22 H25 Co N2 O8'
_chemical_formula_sum 'C22 H25 Co N2 O8'
_chemical_formula_weight 504.37
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'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M p-1
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.866(6)
_cell_length_b 11.392(7)
_cell_length_c 11.936(7)
_cell_angle_alpha 63.328(8)
_cell_angle_beta 79.908(8)
_cell_angle_gamma 88.633(8)
_cell_volume 1177.9(12)
_cell_formula_units_Z 2
_cell_measurement_temperature 298(2)
_cell_measurement_reflns_used 3888
_cell_measurement_theta_min 1.95
_cell_measurement_theta_max 25.20
_exptl_crystal_description block
_exptl_crystal_colour pink
_exptl_crystal_size_max 0.29
_exptl_crystal_size_mid 0.17
_exptl_crystal_size_min 0.12
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.422
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 524
_exptl_absorpt_coefficient_mu 0.777
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.8060
_exptl_absorpt_correction_T_max 0.9125
_exptl_absorpt_process_details SADABS
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 298(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker APEX SMART II'
_diffrn_measurement_method \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% ?
_diffrn_reflns_number 7134
_diffrn_reflns_av_R_equivalents 0.0579
_diffrn_reflns_av_sigmaI/netI 0.0666
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_theta_min 1.94
_diffrn_reflns_theta_max 25.20
_reflns_number_total 3888
_reflns_number_gt 2962
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2004)'
_computing_cell_refinement APEX2
_computing_data_reduction APEX2
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics APEX2
_computing_publication_material APEX2
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 3888
_refine_ls_number_parameters 301
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0682
_refine_ls_R_factor_gt 0.0559
_refine_ls_wR_factor_ref 0.1789
_refine_ls_wR_factor_gt 0.1721
_refine_ls_goodness_of_fit_ref 1.177
_refine_ls_restrained_S_all 1.177
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
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 -0.10562(5) 0.91268(5) 0.50824(6) 0.0376(2) Uani 1 1 d . . .
O1 O 0.0247(3) 0.8690(3) 0.3836(3) 0.0599(9) Uani 1 1 d . . .
O2 O 0.1933(3) 0.9913(3) 0.3894(3) 0.0544(9) Uani 1 1 d . . .
O6 O 0.8435(3) 0.0747(3) 0.3536(3) 0.0531(8) Uani 1 1 d . . .
O5 O 1.0093(3) 0.2073(3) 0.3484(3) 0.0510(8) Uani 1 1 d . . .
O4 O 0.6794(4) 0.6158(4) -0.0543(3) 0.0705(11) Uani 1 1 d . . .
O3 O 0.5116(4) 0.7795(4) 0.0186(4) 0.0646(10) Uani 1 1 d . . .
N1 N -0.2823(4) 0.8051(3) 0.5404(4) 0.0452(9) Uani 1 1 d . . .
N2 N -0.4492(4) 0.6538(4) 0.6036(4) 0.0536(10) Uani 1 1 d . . .
C1 C 0.1482(5) 0.9150(4) 0.3533(4) 0.0452(11) Uani 1 1 d . . .
C2 C 0.2466(4) 0.8775(4) 0.2665(4) 0.0406(10) Uani 1 1 d . . .
C3 C 0.3868(5) 0.9060(4) 0.2465(5) 0.0479(11) Uani 1 1 d . . .
H3 H 0.4193 0.9488 0.2879 0.057 Uiso 1 1 calc R . .
C4 C 0.4792(5) 0.8725(4) 0.1667(5) 0.0490(12) Uani 1 1 d . . .
H4 H 0.5733 0.8898 0.1566 0.059 Uiso 1 1 calc R . .
C5 C 0.4319(5) 0.8136(4) 0.1022(5) 0.0491(12) Uani 1 1 d . . .
C6 C 0.2919(5) 0.7849(5) 0.1189(5) 0.0564(13) Uani 1 1 d . . .
H6 H 0.2592 0.7449 0.0750 0.068 Uiso 1 1 calc R . .
C7 C 0.2012(5) 0.8172(5) 0.2029(5) 0.0540(13) Uani 1 1 d . . .
H7 H 0.1072 0.7970 0.2158 0.065 Uiso 1 1 calc R . .
C8 C 0.6569(5) 0.7931(5) 0.0046(5) 0.0604(15) Uani 1 1 d . . .
H8A H 0.6859 0.7384 0.0849 0.072 Uiso 1 1 calc R . .
H8B H 0.6865 0.8839 -0.0225 0.072 Uiso 1 1 calc R . .
C16 C 0.9045(5) 0.1871(4) 0.3128(4) 0.0448(11) Uani 1 1 d . . .
C13 C 0.8461(4) 0.3014(4) 0.2167(4) 0.0416(10) Uani 1 1 d . . .
C14 C 0.7336(5) 0.2870(5) 0.1680(5) 0.0522(12) Uani 1 1 d . . .
H14 H 0.6941 0.2029 0.1959 0.063 Uiso 1 1 calc R . .
C15 C 0.6781(6) 0.3931(5) 0.0795(5) 0.0573(13) Uani 1 1 d . . .
H15 H 0.6014 0.3810 0.0494 0.069 Uiso 1 1 calc R . .
C10 C 0.7385(5) 0.5183(5) 0.0361(5) 0.0532(13) Uani 1 1 d . . .
C11 C 0.8494(5) 0.5358(5) 0.0821(5) 0.0579(14) Uani 1 1 d . . .
H11 H 0.8897 0.6198 0.0526 0.070 Uiso 1 1 calc R . .
C12 C 0.9027(5) 0.4272(4) 0.1738(5) 0.0517(12) Uani 1 1 d . . .
H12 H 0.9771 0.4399 0.2063 0.062 Uiso 1 1 calc R . .
C9 C 0.7179(6) 0.7503(5) -0.0946(5) 0.0729(19) Uani 1 1 d . . .
H9A H 0.6864 0.8046 -0.1737 0.087 Uiso 1 1 calc R . .
H9B H 0.8176 0.7625 -0.1105 0.087 Uiso 1 1 calc R . .
C20 C -0.4019(5) 0.8652(5) 0.5077(5) 0.0574(14) Uani 1 1 d . . .
H20 H -0.4099 0.9556 0.4661 0.069 Uiso 1 1 calc R . .
C19 C -0.5039(5) 0.7746(5) 0.5446(5) 0.0638(15) Uani 1 1 d . . .
H19 H -0.5947 0.7895 0.5330 0.077 Uiso 1 1 calc R . .
C17 C -0.3150(5) 0.6768(4) 0.5979(5) 0.0489(12) Uani 1 1 d . . .
C18 C -0.2195(7) 0.5746(5) 0.6523(8) 0.091(2) Uani 1 1 d . . .
H18A H -0.1281 0.6144 0.6314 0.136 Uiso 1 1 calc R . .
H18B H -0.2203 0.5130 0.6178 0.136 Uiso 1 1 calc R . .
H18C H -0.2478 0.5294 0.7433 0.136 Uiso 1 1 calc R . .
C21 C -0.5238(6) 0.5252(5) 0.6535(6) 0.0705(16) Uani 1 1 d . . .
H21A H -0.4747 0.4582 0.7134 0.085 Uiso 1 1 calc R . .
H21B H -0.6146 0.5270 0.6995 0.085 Uiso 1 1 calc R . .
C22 C -0.5387(13) 0.4898(10) 0.5526(8) 0.178(6) Uani 1 1 d . . .
H22A H -0.5570 0.3951 0.5970 0.213 Uiso 1 1 calc R . .
H22B H -0.6251 0.5254 0.5282 0.213 Uiso 1 1 calc R . .
O1W O 0.162(3) 0.304(4) 0.703(4) 0.24(2) Uani 0.30(2) 1 d P . .
O2W O 0.1690(10) 0.0600(12) 0.8051(11) 0.180(7) Uani 0.756(19) 1 d P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0376(4) 0.0329(3) 0.0437(4) -0.0190(3) -0.0058(2) 0.0018(2)
O1 0.048(2) 0.074(2) 0.068(2) -0.046(2) 0.0016(16) 0.0067(17)
O2 0.063(2) 0.0500(19) 0.059(2) -0.0346(18) -0.0064(16) 0.0096(16)
O6 0.065(2) 0.0379(17) 0.054(2) -0.0153(16) -0.0187(16) 0.0056(15)
O5 0.0449(18) 0.0465(18) 0.054(2) -0.0138(16) -0.0159(15) 0.0044(14)
O4 0.092(3) 0.063(2) 0.050(2) -0.0205(18) -0.0173(19) 0.043(2)
O3 0.060(2) 0.072(2) 0.068(2) -0.044(2) 0.0034(17) 0.0159(18)
N1 0.039(2) 0.039(2) 0.059(3) -0.0232(19) -0.0088(17) 0.0015(16)
N2 0.055(2) 0.052(2) 0.052(3) -0.024(2) -0.0001(19) -0.0190(19)
C1 0.048(3) 0.038(2) 0.044(3) -0.016(2) -0.005(2) 0.010(2)
C2 0.044(2) 0.034(2) 0.044(3) -0.019(2) -0.0053(19) 0.0067(18)
C3 0.051(3) 0.049(3) 0.050(3) -0.027(2) -0.013(2) 0.008(2)
C4 0.039(2) 0.051(3) 0.059(3) -0.028(3) -0.009(2) 0.009(2)
C5 0.052(3) 0.043(2) 0.048(3) -0.021(2) 0.002(2) 0.014(2)
C6 0.058(3) 0.059(3) 0.067(3) -0.043(3) -0.005(2) 0.005(2)
C7 0.045(3) 0.057(3) 0.062(3) -0.032(3) 0.000(2) 0.001(2)
C8 0.056(3) 0.054(3) 0.055(3) -0.016(3) 0.005(2) 0.019(2)
C16 0.045(3) 0.042(2) 0.043(3) -0.018(2) 0.000(2) 0.007(2)
C13 0.044(2) 0.043(2) 0.036(2) -0.017(2) -0.0058(18) 0.0110(19)
C14 0.066(3) 0.046(3) 0.051(3) -0.026(2) -0.017(2) 0.013(2)
C15 0.070(3) 0.061(3) 0.056(3) -0.036(3) -0.027(3) 0.028(3)
C10 0.062(3) 0.053(3) 0.039(3) -0.018(2) -0.006(2) 0.029(2)
C11 0.060(3) 0.039(2) 0.057(3) -0.010(2) 0.002(2) 0.009(2)
C12 0.046(3) 0.044(3) 0.055(3) -0.014(2) -0.009(2) 0.007(2)
C9 0.083(4) 0.057(3) 0.051(3) -0.008(3) 0.005(3) 0.036(3)
C20 0.042(3) 0.048(3) 0.080(4) -0.028(3) -0.009(2) 0.003(2)
C19 0.042(3) 0.068(3) 0.079(4) -0.032(3) -0.008(2) 0.001(2)
C17 0.055(3) 0.038(2) 0.054(3) -0.019(2) -0.016(2) -0.004(2)
C18 0.110(5) 0.043(3) 0.124(6) -0.029(3) -0.061(4) 0.012(3)
C21 0.082(4) 0.063(3) 0.060(4) -0.027(3) 0.007(3) -0.036(3)
C22 0.261(13) 0.161(8) 0.115(8) -0.103(7) 0.090(7) -0.166(8)
O1W 0.14(2) 0.31(5) 0.27(4) -0.16(4) 0.03(2) -0.09(2)
O2W 0.169(10) 0.269(15) 0.192(11) -0.166(11) -0.089(7) 0.054(8)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 2.020(3) . ?
Co1 O5 2.027(3) 2_666 ?
Co1 N1 2.033(4) . ?
Co1 O2 2.055(3) 2_576 ?
Co1 O6 2.071(3) 1_465 ?
Co1 Co1 2.8361(17) 2_576 ?
O1 C1 1.263(6) . ?
O2 C1 1.249(6) . ?
O2 Co1 2.055(3) 2_576 ?
O6 C16 1.270(5) . ?
O6 Co1 2.071(3) 1_645 ?
O5 C16 1.247(6) . ?
O5 Co1 2.027(3) 2_666 ?
O4 C10 1.361(5) . ?
O4 C9 1.423(7) . ?
O3 C5 1.350(5) . ?
O3 C8 1.417(6) . ?
N1 C17 1.325(6) . ?
N1 C20 1.377(6) . ?
N2 C17 1.340(6) . ?
N2 C19 1.382(6) . ?
N2 C21 1.469(6) . ?
C1 C2 1.491(6) . ?
C2 C7 1.359(7) . ?
C2 C3 1.383(6) . ?
C3 C4 1.375(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.366(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.385(7) . ?
C6 C7 1.395(6) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.502(7) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C16 C13 1.483(6) . ?
C13 C12 1.381(6) . ?
C13 C14 1.385(7) . ?
C14 C15 1.379(6) . ?
C14 H14 0.9300 . ?
C15 C10 1.388(7) . ?
C15 H15 0.9300 . ?
C10 C11 1.363(8) . ?
C11 C12 1.400(6) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C20 C19 1.326(7) . ?
C20 H20 0.9300 . ?
C19 H19 0.9300 . ?
C17 C18 1.466(7) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C21 C22 1.461(10) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C22 1.276(14) 2_466 ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
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 O5 90.39(15) . 2_666 ?
O1 Co1 N1 103.32(16) . . ?
O5 Co1 N1 103.06(14) 2_666 . ?
O1 Co1 O2 161.43(14) . 2_576 ?
O5 Co1 O2 91.91(15) 2_666 2_576 ?
N1 Co1 O2 94.10(15) . 2_576 ?
O1 Co1 O6 88.10(15) . 1_465 ?
O5 Co1 O6 162.73(13) 2_666 1_465 ?
N1 Co1 O6 94.02(14) . 1_465 ?
O2 Co1 O6 84.26(14) 2_576 1_465 ?
O1 Co1 Co1 88.53(11) . 2_576 ?
O5 Co1 Co1 78.54(10) 2_666 2_576 ?
N1 Co1 Co1 167.98(11) . 2_576 ?
O2 Co1 Co1 73.90(11) 2_576 2_576 ?
O6 Co1 Co1 84.22(11) 1_465 2_576 ?
C1 O1 Co1 117.5(3) . . ?
C1 O2 Co1 134.6(3) . 2_576 ?
C16 O6 Co1 121.0(3) . 1_645 ?
C16 O5 Co1 131.1(3) . 2_666 ?
C10 O4 C9 120.5(5) . . ?
C5 O3 C8 118.4(4) . . ?
C17 N1 C20 106.1(4) . . ?
C17 N1 Co1 132.7(3) . . ?
C20 N1 Co1 121.1(3) . . ?
C17 N2 C19 107.2(4) . . ?
C17 N2 C21 127.2(5) . . ?
C19 N2 C21 125.5(5) . . ?
O2 C1 O1 124.7(4) . . ?
O2 C1 C2 117.6(4) . . ?
O1 C1 C2 117.7(4) . . ?
C7 C2 C3 118.3(4) . . ?
C7 C2 C1 121.2(4) . . ?
C3 C2 C1 120.5(4) . . ?
C4 C3 C2 121.4(5) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C5 C4 C3 119.6(4) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
O3 C5 C4 125.2(4) . . ?
O3 C5 C6 114.3(5) . . ?
C4 C5 C6 120.5(4) . . ?
C5 C6 C7 118.5(5) . . ?
C5 C6 H6 120.8 . . ?
C7 C6 H6 120.8 . . ?
C2 C7 C6 121.7(5) . . ?
C2 C7 H7 119.1 . . ?
C6 C7 H7 119.1 . . ?
O3 C8 C9 106.7(5) . . ?
O3 C8 H8A 110.4 . . ?
C9 C8 H8A 110.4 . . ?
O3 C8 H8B 110.4 . . ?
C9 C8 H8B 110.4 . . ?
H8A C8 H8B 108.6 . . ?
O5 C16 O6 124.4(4) . . ?
O5 C16 C13 118.3(4) . . ?
O6 C16 C13 117.3(4) . . ?
C12 C13 C14 117.8(4) . . ?
C12 C13 C16 120.2(4) . . ?
C14 C13 C16 122.0(4) . . ?
C15 C14 C13 122.2(5) . . ?
C15 C14 H14 118.9 . . ?
C13 C14 H14 118.9 . . ?
C14 C15 C10 118.9(5) . . ?
C14 C15 H15 120.5 . . ?
C10 C15 H15 120.5 . . ?
O4 C10 C11 125.2(5) . . ?
O4 C10 C15 114.5(5) . . ?
C11 C10 C15 120.3(4) . . ?
C10 C11 C12 120.0(5) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C13 C12 C11 120.8(5) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
O4 C9 C8 111.1(4) . . ?
O4 C9 H9A 109.4 . . ?
C8 C9 H9A 109.4 . . ?
O4 C9 H9B 109.4 . . ?
C8 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
C19 C20 N1 109.7(4) . . ?
C19 C20 H20 125.1 . . ?
N1 C20 H20 125.1 . . ?
C20 C19 N2 106.6(4) . . ?
C20 C19 H19 126.7 . . ?
N2 C19 H19 126.7 . . ?
N1 C17 N2 110.3(4) . . ?
N1 C17 C18 124.9(5) . . ?
N2 C17 C18 124.7(5) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C22 C21 N2 112.4(5) . . ?
C22 C21 H21A 109.1 . . ?
N2 C21 H21A 109.1 . . ?
C22 C21 H21B 109.1 . . ?
N2 C21 H21B 109.1 . . ?
H21A C21 H21B 107.9 . . ?
C22 C22 C21 133.1(11) 2_466 . ?
C22 C22 H22A 104.0 2_466 . ?
C21 C22 H22A 104.0 . . ?
C22 C22 H22B 104.0 2_466 . ?
C21 C22 H22B 104.0 . . ?
H22A C22 H22B 105.4 . . ?
_diffrn_measured_fraction_theta_max 0.915
_diffrn_reflns_theta_full 25.20
_diffrn_measured_fraction_theta_full 0.915
_refine_diff_density_max 1.514
_refine_diff_density_min -0.459
_refine_diff_density_rms 0.094
#===END
data_3
_database_code_depnum_ccdc_archive 'CCDC 843288'
#TrackingRef '- All cif.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C26 H28 Co N4 O6'
_chemical_formula_sum 'C26 H28 Co N4 O6'
_chemical_formula_weight 551.45
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'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M p-1
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.3520(19)
_cell_length_b 12.509(3)
_cell_length_c 12.643(3)
_cell_angle_alpha 66.32(3)
_cell_angle_beta 80.84(3)
_cell_angle_gamma 79.86(3)
_cell_volume 1326.9(5)
_cell_formula_units_Z 2
_cell_measurement_temperature 298(2)
_cell_measurement_reflns_used 4665
_cell_measurement_theta_min 3.02
_cell_measurement_theta_max 25.20
_exptl_crystal_description block
_exptl_crystal_colour pink
_exptl_crystal_size_max 0.23
_exptl_crystal_size_mid 0.16
_exptl_crystal_size_min 0.10
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.380
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 574
_exptl_absorpt_coefficient_mu 0.693
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.8568
_exptl_absorpt_correction_T_max 0.9339
_exptl_absorpt_process_details SADABS
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 298(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker APEX SMART II'
_diffrn_measurement_method \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% ?
_diffrn_reflns_number 10073
_diffrn_reflns_av_R_equivalents 0.0302
_diffrn_reflns_av_sigmaI/netI 0.0401
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_theta_min 3.02
_diffrn_reflns_theta_max 25.20
_reflns_number_total 4665
_reflns_number_gt 3728
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2004)'
_computing_cell_refinement APEX2
_computing_data_reduction APEX2
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics APEX2
_computing_publication_material APEX2
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The H atoms of free water molecule
were located in a difference Fourier
map and then refined as riding in their as-found relative positions with
distance restraints of O---H = 0.84 \%A, and H---H = 1.38 \%A, each within a
standard deviation of 0.01 and 0.02 \%A, respectively,
and with U~iso~(H) = 1.5 U~eq~(O).
The distance restraints of C26---C26 = 1.55 \%A and C25---C26 =1.50 \%A,
each within a standard deviation of 0.005 \%A.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1300P)^2^+0.2101P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 4665
_refine_ls_number_parameters 336
_refine_ls_number_restraints 5
_refine_ls_R_factor_all 0.0732
_refine_ls_R_factor_gt 0.0609
_refine_ls_wR_factor_ref 0.1883
_refine_ls_wR_factor_gt 0.1739
_refine_ls_goodness_of_fit_ref 1.053
_refine_ls_restrained_S_all 1.059
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
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 0.11236(5) 0.38437(4) 0.27204(4) 0.0448(2) Uani 1 1 d . . .
O1 O 0.2062(3) 0.5074(2) 0.1410(3) 0.0670(8) Uani 1 1 d . . .
O2 O 0.2099(4) 0.5862(3) 0.2666(3) 0.0718(8) Uani 1 1 d . . .
O4 O 0.1368(3) 1.2816(2) -0.5570(2) 0.0595(7) Uani 1 1 d . . .
O5 O 0.3475(3) 1.3041(3) -0.6614(2) 0.0679(8) Uani 1 1 d . . .
O3 O 0.5567(3) 0.9330(3) -0.1772(3) 0.0800(10) Uani 1 1 d . . .
N1 N 0.1089(4) 0.2486(3) 0.2205(3) 0.0563(8) Uani 1 1 d . . .
N3 N -0.1082(3) 0.4359(3) 0.2804(3) 0.0507(7) Uani 1 1 d . . .
N4 N -0.3281(3) 0.5247(3) 0.3075(3) 0.0548(8) Uani 1 1 d . . .
C14 C 0.2749(5) 1.2564(3) -0.5673(3) 0.0522(9) Uani 1 1 d . . .
C11 C 0.3476(4) 1.1693(3) -0.4649(3) 0.0517(9) Uani 1 1 d . . .
C10 C 0.4980(5) 1.1572(4) -0.4630(4) 0.0699(12) Uani 1 1 d . . .
H10 H 0.5548 1.2024 -0.5276 0.084 Uiso 1 1 calc R . .
C12 C 0.2683(5) 1.0986(4) -0.3697(4) 0.0771(14) Uani 1 1 d . . .
H12 H 0.1675 1.1060 -0.3688 0.092 Uiso 1 1 calc R . .
C13 C 0.3359(5) 1.0158(4) -0.2741(4) 0.0850(17) Uani 1 1 d . . .
H13 H 0.2810 0.9664 -0.2112 0.102 Uiso 1 1 calc R . .
C1 C 0.2421(4) 0.5844(3) 0.1690(3) 0.0515(9) Uani 1 1 d . . .
C2 C 0.3280(4) 0.6753(3) 0.0770(3) 0.0474(8) Uani 1 1 d . . .
C3 C 0.3857(5) 0.6629(4) -0.0266(3) 0.0626(10) Uani 1 1 d . . .
H3 H 0.3722 0.5969 -0.0388 0.075 Uiso 1 1 calc R . .
C4 C 0.4624(5) 0.7476(4) -0.1109(4) 0.0699(12) Uani 1 1 d . . .
H4 H 0.5018 0.7388 -0.1797 0.084 Uiso 1 1 calc R . .
C5 C 0.4804(4) 0.8448(4) -0.0926(3) 0.0605(11) Uani 1 1 d . . .
C6 C 0.4273(5) 0.8572(4) 0.0104(4) 0.0648(11) Uani 1 1 d . . .
H6 H 0.4423 0.9227 0.0228 0.078 Uiso 1 1 calc R . .
C7 C 0.3517(5) 0.7715(3) 0.0950(3) 0.0564(9) Uani 1 1 d . . .
H7 H 0.3163 0.7790 0.1650 0.068 Uiso 1 1 calc R . .
C8 C 0.4823(4) 1.0076(4) -0.2733(4) 0.0630(11) Uani 1 1 d . . .
C9 C 0.5641(5) 1.0784(4) -0.3658(4) 0.0760(14) Uani 1 1 d . . .
H9 H 0.6640 1.0737 -0.3637 0.091 Uiso 1 1 calc R . .
C17 C 0.1187(4) 0.2415(4) 0.1201(4) 0.0593(10) Uani 1 1 d . . .
C16 C 0.0795(5) 0.0665(4) 0.2465(4) 0.0703(12) Uani 1 1 d . . .
H16 H 0.0648 -0.0123 0.2797 0.084 Uiso 1 1 calc R . .
C15 C 0.0824(5) 0.1354(4) 0.3013(4) 0.0652(11) Uani 1 1 d . . .
H15 H 0.0691 0.1131 0.3815 0.078 Uiso 1 1 calc R . .
C19 C 0.1141(6) 0.0878(6) 0.0395(5) 0.0912(18) Uani 1 1 d . . .
H19A H 0.1220 0.1514 -0.0362 0.109 Uiso 1 1 calc R . .
H19B H 0.2042 0.0345 0.0456 0.109 Uiso 1 1 calc R . .
C20 C -0.0038(5) 0.0252(5) 0.0439(5) 0.0797(14) Uani 1 1 d . . .
H20A H -0.0937 0.0786 0.0384 0.096 Uiso 1 1 calc R . .
H20B H -0.0112 -0.0383 0.1197 0.096 Uiso 1 1 calc R . .
N2 N 0.1033(4) 0.1365(3) 0.1260(3) 0.0618(9) Uani 1 1 d . . .
C18 C 0.1466(6) 0.3422(4) 0.0097(4) 0.0784(13) Uani 1 1 d . . .
H18A H 0.0639 0.3640 -0.0342 0.118 Uiso 1 1 calc R . .
H18B H 0.2316 0.3202 -0.0342 0.118 Uiso 1 1 calc R . .
H18C H 0.1623 0.4076 0.0260 0.118 Uiso 1 1 calc R . .
C25 C -0.4469(5) 0.6011(4) 0.3395(4) 0.0667(11) Uani 1 1 d D . .
H25A H -0.4066 0.6619 0.3503 0.080 Uiso 1 1 calc R . .
H25B H -0.5081 0.6393 0.2761 0.080 Uiso 1 1 calc R . .
C21 C -0.2094(5) 0.3899(4) 0.2486(4) 0.0628(10) Uani 1 1 d . . .
H21 H -0.1875 0.3303 0.2201 0.075 Uiso 1 1 calc R . .
C23 C -0.1850(4) 0.5165(3) 0.3170(3) 0.0532(9) Uani 1 1 d . . .
C24 C -0.1251(6) 0.5868(6) 0.3666(6) 0.102(2) Uani 1 1 d . . .
H24A H -0.0233 0.5600 0.3750 0.153 Uiso 1 1 calc R . .
H24B H -0.1765 0.5776 0.4413 0.153 Uiso 1 1 calc R . .
H24C H -0.1370 0.6683 0.3157 0.153 Uiso 1 1 calc R . .
C26 C -0.5386(6) 0.5388(6) 0.4466(3) 0.157(4) Uani 1 1 d D . .
H26A H -0.5945 0.4905 0.4293 0.188 Uiso 1 1 calc R . .
H26B H -0.6077 0.5974 0.4660 0.188 Uiso 1 1 calc R . .
C22 C -0.3444(5) 0.4429(4) 0.2643(4) 0.0672(11) Uani 1 1 d . . .
H22 H -0.4311 0.4275 0.2491 0.081 Uiso 1 1 calc R . .
O1W O 0.1152(5) 0.7676(3) 0.3696(4) 0.1037(13) Uani 1 1 d D . .
H1WA H 0.1546 0.7098 0.3529 0.156 Uiso 1 1 d RD . .
H1WB H 0.1307 0.7577 0.4371 0.156 Uiso 1 1 d RD . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0525(4) 0.0393(3) 0.0453(3) -0.0173(2) -0.0062(2) -0.0091(2)
O1 0.075(2) 0.0540(16) 0.0695(17) -0.0106(13) -0.0158(15) -0.0249(14)
O2 0.077(2) 0.0685(19) 0.0603(17) -0.0168(14) 0.0141(15) -0.0215(16)
O4 0.0568(18) 0.0638(17) 0.0564(15) -0.0228(12) -0.0140(13) 0.0033(13)
O5 0.073(2) 0.0652(18) 0.0536(15) -0.0058(13) -0.0086(14) -0.0184(15)
O3 0.0499(18) 0.075(2) 0.0771(19) 0.0191(15) -0.0151(15) -0.0217(14)
N1 0.059(2) 0.0536(18) 0.066(2) -0.0309(15) -0.0103(16) -0.0078(15)
N3 0.0511(18) 0.0560(18) 0.0500(16) -0.0245(13) -0.0093(14) -0.0053(14)
N4 0.0464(19) 0.067(2) 0.0531(17) -0.0259(15) -0.0061(14) -0.0036(15)
C14 0.063(3) 0.0439(19) 0.054(2) -0.0214(16) -0.0117(18) -0.0041(17)
C11 0.052(2) 0.0452(19) 0.053(2) -0.0140(15) -0.0079(17) -0.0051(16)
C10 0.056(3) 0.066(3) 0.061(2) 0.0041(19) -0.002(2) -0.012(2)
C12 0.042(2) 0.082(3) 0.074(3) 0.005(2) -0.007(2) -0.009(2)
C13 0.044(3) 0.085(3) 0.077(3) 0.022(2) -0.003(2) -0.018(2)
C1 0.047(2) 0.0423(19) 0.058(2) -0.0083(15) -0.0074(17) -0.0100(15)
C2 0.047(2) 0.0430(18) 0.0482(18) -0.0108(14) -0.0109(15) -0.0067(15)
C3 0.077(3) 0.057(2) 0.056(2) -0.0192(18) -0.006(2) -0.018(2)
C4 0.077(3) 0.075(3) 0.051(2) -0.016(2) -0.002(2) -0.017(2)
C5 0.044(2) 0.055(2) 0.059(2) 0.0071(17) -0.0102(18) -0.0137(17)
C6 0.068(3) 0.043(2) 0.079(3) -0.0172(18) -0.004(2) -0.0152(19)
C7 0.062(3) 0.050(2) 0.055(2) -0.0172(16) -0.0008(18) -0.0156(18)
C8 0.047(2) 0.057(2) 0.061(2) 0.0042(18) -0.0094(18) -0.0093(18)
C9 0.045(2) 0.078(3) 0.073(3) 0.008(2) -0.010(2) -0.016(2)
C17 0.050(2) 0.070(3) 0.074(3) -0.041(2) -0.0164(19) -0.0039(18)
C16 0.076(3) 0.052(2) 0.087(3) -0.025(2) -0.011(2) -0.021(2)
C15 0.086(3) 0.053(2) 0.055(2) -0.0161(17) -0.010(2) -0.012(2)
C19 0.081(4) 0.120(4) 0.120(4) -0.093(4) 0.013(3) -0.039(3)
C20 0.067(3) 0.100(4) 0.108(4) -0.075(3) -0.006(3) -0.017(3)
N2 0.062(2) 0.063(2) 0.082(2) -0.0464(18) -0.0122(18) -0.0105(16)
C18 0.094(4) 0.071(3) 0.068(3) -0.020(2) -0.006(2) -0.023(3)
C25 0.053(3) 0.077(3) 0.067(2) -0.028(2) -0.009(2) 0.006(2)
C21 0.058(3) 0.073(3) 0.074(3) -0.043(2) -0.011(2) -0.011(2)
C23 0.050(2) 0.059(2) 0.058(2) -0.0290(17) -0.0051(17) -0.0076(17)
C24 0.059(3) 0.131(5) 0.171(6) -0.118(5) -0.004(3) -0.009(3)
C26 0.146(7) 0.140(6) 0.101(4) -0.015(4) 0.048(5) 0.062(5)
C22 0.056(3) 0.091(3) 0.073(3) -0.046(2) -0.014(2) -0.013(2)
O1W 0.110(3) 0.081(2) 0.126(3) -0.045(2) 0.016(3) -0.038(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 1.962(3) . ?
Co1 N3 2.049(3) . ?
Co1 O4 2.049(3) 1_546 ?
Co1 N1 2.056(3) . ?
Co1 O5 2.385(3) 1_546 ?
O1 C1 1.262(5) . ?
O2 C1 1.231(5) . ?
O4 C14 1.273(5) . ?
O4 Co1 2.049(3) 1_564 ?
O5 C14 1.244(5) . ?
O5 Co1 2.385(3) 1_564 ?
O3 C8 1.401(5) . ?
O3 C5 1.398(5) . ?
N1 C17 1.295(5) . ?
N1 C15 1.411(5) . ?
N3 C23 1.327(5) . ?
N3 C21 1.374(5) . ?
N4 C23 1.344(5) . ?
N4 C22 1.378(5) . ?
N4 C25 1.451(5) . ?
C14 C11 1.487(5) . ?
C11 C12 1.369(6) . ?
C11 C10 1.391(6) . ?
C10 C9 1.385(6) . ?
C10 H10 0.9300 . ?
C12 C13 1.394(6) . ?
C12 H12 0.9300 . ?
C13 C8 1.355(6) . ?
C13 H13 0.9300 . ?
C1 C2 1.501(5) . ?
C2 C7 1.370(5) . ?
C2 C3 1.393(6) . ?
C3 C4 1.375(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.368(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.377(6) . ?
C6 C7 1.378(6) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.364(6) . ?
C9 H9 0.9300 . ?
C17 N2 1.318(5) . ?
C17 C18 1.479(6) . ?
C16 C15 1.311(6) . ?
C16 N2 1.424(6) . ?
C16 H16 0.9300 . ?
C15 H15 0.9300 . ?
C19 C20 1.443(6) . ?
C19 N2 1.434(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C20 1.469(8) 2 ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C25 C26 1.481(4) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C21 C22 1.343(6) . ?
C21 H21 0.9300 . ?
C23 C24 1.487(5) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C26 C26 1.515(5) 2_466 ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C22 H22 0.9300 . ?
O1W H1WA 0.8420 . ?
O1W H1WB 0.8443 . ?
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 N3 108.24(13) . . ?
O1 Co1 O4 139.63(12) . 1_546 ?
N3 Co1 O4 100.68(12) . 1_546 ?
O1 Co1 N1 107.14(14) . . ?
N3 Co1 N1 96.98(13) . . ?
O4 Co1 N1 96.37(13) 1_546 . ?
O1 Co1 O5 88.08(12) . 1_546 ?
N3 Co1 O5 158.43(11) . 1_546 ?
O4 Co1 O5 58.46(11) 1_546 1_546 ?
N1 Co1 O5 91.29(12) . 1_546 ?
C1 O1 Co1 113.0(3) . . ?
C14 O4 Co1 97.6(2) . 1_564 ?
C14 O5 Co1 83.0(2) . 1_564 ?
C8 O3 C5 115.9(3) . . ?
C17 N1 C15 104.7(3) . . ?
C17 N1 Co1 133.5(3) . . ?
C15 N1 Co1 121.6(3) . . ?
C23 N3 C21 105.1(3) . . ?
C23 N3 Co1 129.6(3) . . ?
C21 N3 Co1 125.3(3) . . ?
C23 N4 C22 107.2(3) . . ?
C23 N4 C25 127.9(3) . . ?
C22 N4 C25 124.9(4) . . ?
O5 C14 O4 120.5(3) . . ?
O5 C14 C11 120.7(4) . . ?
O4 C14 C11 118.8(4) . . ?
C12 C11 C10 118.0(4) . . ?
C12 C11 C14 120.9(4) . . ?
C10 C11 C14 121.1(4) . . ?
C11 C10 C9 120.6(4) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C11 C12 C13 121.2(4) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 H12 119.4 . . ?
C8 C13 C12 119.6(4) . . ?
C8 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
O2 C1 O1 122.6(4) . . ?
O2 C1 C2 120.6(3) . . ?
O1 C1 C2 116.7(3) . . ?
C7 C2 C3 119.2(4) . . ?
C7 C2 C1 119.9(3) . . ?
C3 C2 C1 120.9(3) . . ?
C4 C3 C2 120.3(4) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 119.4(4) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C6 C5 C4 121.1(4) . . ?
C6 C5 O3 118.2(4) . . ?
C4 C5 O3 120.7(4) . . ?
C7 C6 C5 119.2(4) . . ?
C7 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
C6 C7 C2 120.7(4) . . ?
C6 C7 H7 119.6 . . ?
C2 C7 H7 119.6 . . ?
C9 C8 C13 120.7(4) . . ?
C9 C8 O3 116.2(4) . . ?
C13 C8 O3 123.0(4) . . ?
C8 C9 C10 119.8(4) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
N1 C17 N2 113.7(4) . . ?
N1 C17 C18 122.7(4) . . ?
N2 C17 C18 123.6(4) . . ?
C15 C16 N2 106.3(4) . . ?
C15 C16 H16 126.9 . . ?
N2 C16 H16 126.9 . . ?
C16 C15 N1 109.8(4) . . ?
C16 C15 H15 125.1 . . ?
N1 C15 H15 125.1 . . ?
C20 C19 N2 116.8(4) . . ?
C20 C19 H19A 108.1 . . ?
N2 C19 H19A 108.1 . . ?
C20 C19 H19B 108.1 . . ?
N2 C19 H19B 108.1 . . ?
H19A C19 H19B 107.3 . . ?
C19 C20 C20 118.1(6) . 2 ?
C19 C20 H20A 107.8 . . ?
C20 C20 H20A 107.8 2 . ?
C19 C20 H20B 107.8 . . ?
C20 C20 H20B 107.8 2 . ?
H20A C20 H20B 107.1 . . ?
C17 N2 C16 105.5(3) . . ?
C17 N2 C19 132.7(4) . . ?
C16 N2 C19 121.7(4) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C26 C25 N4 113.7(4) . . ?
C26 C25 H25A 108.8 . . ?
N4 C25 H25A 108.8 . . ?
C26 C25 H25B 108.8 . . ?
N4 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
C22 C21 N3 110.5(4) . . ?
C22 C21 H21 124.7 . . ?
N3 C21 H21 124.7 . . ?
N3 C23 N4 111.2(3) . . ?
N3 C23 C24 125.7(4) . . ?
N4 C23 C24 123.1(4) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C25 C26 C26 117.4(6) . 2_466 ?
C25 C26 H26A 107.9 . . ?
C26 C26 H26A 107.9 2_466 . ?
C25 C26 H26B 107.9 . . ?
C26 C26 H26B 107.9 2_466 . ?
H26A C26 H26B 107.2 . . ?
C21 C22 N4 105.9(3) . . ?
C21 C22 H22 127.0 . . ?
N4 C22 H22 127.0 . . ?
H1WA O1W H1WB 111.1 . . ?
_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full 25.20
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max 1.303
_refine_diff_density_min -0.996
_refine_diff_density_rms 0.078