# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_cambridge 0222
#TrackingRef '- Structures combined.cif'
_audit_creation_method SHELXL-97
_publ_section_title
;
Syntheses of 8-quinolinatocobalt(III) complexes containing
cyclen based auxiliary ligands as models for
;
_publ_section_abstract ' Abstract '
_publ_section_comment ' Comment '
_publ_contact_author_name 'George R. Clark'
_publ_contact_author_address
;
Department of Chemistry
The University of Auckland
Private Bag 92019
Auckland
New Zealand
;
_publ_contact_author_email g.clark@auckland.ac.nz
_publ_contact_author_phone '0064 9 3737599 Ext 88294'
_publ_contact_author_fax '0064 9 3737422'
loop_
_publ_author_name
_publ_author_address
J.Yu.Chang
;
Department of Chemistry
The University of Auckland
Private Bag 92019
Auckland
New Zealand
;
R.Stephenson
;
Auckland Cancer Society Research Centre
The University of Auckland
Private Bag 92019
Auckland
New Zealand
;
G.-L.Lu
;
Auckland Cancer Society Research Centre
The University of Auckland
Private Bag 92019
Auckland
New Zealand
;
P.J.Brothers
;
Department of Chemistry
The University of Auckland
Private Bag 92019
Auckland
New Zealand
;
G.R.Clark
;
Department of Chemistry
The University of Auckland
Private Bag 92019
Auckland
New Zealand
;
;
W.A.Denny
;
;
Auckland Cancer Society Research Centre
The University of Auckland
Private Bag 92019
Auckland
New Zealand
;
D.C.Ware
;
Department of Chemistry
The University of Auckland
Private Bag 92019
Auckland
New Zealand
;
_publ_section_exptl_refinement
;
Hydrogen atoms were placed in calculated positions and refined using the
riding model [C-H 0.93-0.97 \%A), with U~iso~(H) = 1.2 or 1.5 times
U~eq~(C). The two perchlorate anions are disordered.
;
_publ_section_figure_captions
;
Fig. 1: Structure showing 50 % probability displacement ellipsoids
for non-hydrogen atoms and hydrogen atoms as arbitary spheres (Burnett
& Johnson, 1996).
;
_publ_section_acknowledgements
;
No acknowledgements
;
_publ_section_references
;
Burnett, M.N. and Johnson, C.K. (1996). ORTEP-III: Report ORNL-6895.
Oak Ridge National Laboratory, Tennessee, USA.
Sheldrick, G.M. (1996). SADABS. Univ. of G\"ottingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Siemens (1995). SMART (Version 4.050) and
SAINT (Version 4.050). Siemens Analytical X-ray Instruments
Inc., Madison, Wisconsin, USA.
;
data_jyc013
_database_code_depnum_ccdc_archive 'CCDC 791378'
#TrackingRef '- Structures combined.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C17 H26 Co N5 O, 2(Cl O4)'
_chemical_formula_sum 'C17 H26 Cl2 Co N5 O9'
_chemical_formula_weight 574.26
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'
Cl Cl 0.1484 0.1585 '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'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M P21/c
_symmetry_space_group_name_Hall -p_2ybc
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 15.2420(2)
_cell_length_b 9.4131(2)
_cell_length_c 16.3816(2)
_cell_angle_alpha 90.00
_cell_angle_beta 92.145(1)
_cell_angle_gamma 90.00
_cell_volume 2348.69(7)
_cell_formula_units_Z 4
_cell_measurement_temperature 291(2)
_cell_measurement_reflns_used 6149
_cell_measurement_theta_min 2.49
_cell_measurement_theta_max 26.39
_exptl_crystal_description fragment
_exptl_crystal_colour red
_exptl_crystal_size_max 0.36
_exptl_crystal_size_mid 0.28
_exptl_crystal_size_min 0.10
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.624
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1184
_exptl_absorpt_coefficient_mu 1.016
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS; Sheldrick, 1996'
_exptl_absorpt_correction_T_min 0.7111
_exptl_absorpt_correction_T_max 0.9052
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 291(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 'Siemens SMART CCD'
_diffrn_measurement_method 'Area detector \w scans'
_diffrn_standards_decay_% <2%
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_reflns_number 13277
_diffrn_reflns_av_R_equivalents 0.0273
_diffrn_reflns_av_sigmaI/netI 0.0360
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_theta_min 2.49
_diffrn_reflns_theta_max 26.39
_reflns_number_total 4797
_reflns_number_gt 3472
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'SMART (Siemens, 1995)'
_computing_cell_refinement 'SAINT (Siemens, 1995)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics 'Ortep-III (Burnett & Johnson, 1996)'
_computing_publication_material 'SHELXTL (Sheldrick, 2008)'
_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^)+(0.1510P)^2^+4.0954P] 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 4797
_refine_ls_number_parameters 302
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1019
_refine_ls_R_factor_gt 0.0760
_refine_ls_wR_factor_ref 0.2469
_refine_ls_wR_factor_gt 0.2204
_refine_ls_goodness_of_fit_ref 1.012
_refine_ls_restrained_S_all 1.012
_refine_ls_shift/su_max 0.009
_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
Co Co 0.27730(4) 0.20425(7) 0.57469(4) 0.0459(3) Uani 1 1 d . . .
N1 N 0.2066(3) 0.3620(6) 0.5292(3) 0.0636(12) Uani 1 1 d . . .
H1 H 0.1727 0.3294 0.4863 0.076 Uiso 1 1 calc R . .
N2 N 0.3747(3) 0.3356(5) 0.5709(3) 0.0607(12) Uani 1 1 d . . .
H2 H 0.3719 0.3927 0.6155 0.073 Uiso 1 1 calc R . .
N3 N 0.3603(3) 0.0809(5) 0.6351(3) 0.0525(10) Uani 1 1 d . . .
H3 H 0.3502 -0.0105 0.6194 0.063 Uiso 1 1 calc R . .
N4 N 0.2397(3) 0.2672(5) 0.6819(3) 0.0538(11) Uani 1 1 d . . .
H4 H 0.1953 0.2083 0.6956 0.065 Uiso 1 1 calc R . .
N5 N 0.1847(3) 0.0599(5) 0.5612(3) 0.0535(11) Uani 1 1 d . . .
O1 O 0.3141(3) 0.1375(5) 0.4727(2) 0.0620(10) Uani 1 1 d . . .
C1 C 0.2636(5) 0.4768(8) 0.5005(5) 0.083(2) Uani 1 1 d . . .
H1A H 0.2603 0.5578 0.5369 0.100 Uiso 1 1 calc R . .
H1B H 0.2435 0.5068 0.4464 0.100 Uiso 1 1 calc R . .
C2 C 0.3572(5) 0.4266(7) 0.4981(5) 0.0768(19) Uani 1 1 d . . .
H2A H 0.3658 0.3728 0.4485 0.092 Uiso 1 1 calc R . .
H2B H 0.3969 0.5071 0.4990 0.092 Uiso 1 1 calc R . .
C3 C 0.4575(4) 0.2598(9) 0.5777(6) 0.091(3) Uani 1 1 d . . .
H3A H 0.4806 0.2503 0.5237 0.109 Uiso 1 1 calc R . .
H3B H 0.4989 0.3163 0.6103 0.109 Uiso 1 1 calc R . .
C4 C 0.4522(4) 0.1203(7) 0.6139(5) 0.0756(18) Uani 1 1 d . . .
H4A H 0.4897 0.1173 0.6630 0.091 Uiso 1 1 calc R . .
H4B H 0.4740 0.0507 0.5760 0.091 Uiso 1 1 calc R . .
C5 C 0.3445(4) 0.0928(7) 0.7239(3) 0.0618(14) Uani 1 1 d . . .
H5A H 0.3984 0.0737 0.7553 0.074 Uiso 1 1 calc R . .
H5B H 0.3009 0.0237 0.7392 0.074 Uiso 1 1 calc R . .
C6 C 0.3125(4) 0.2414(7) 0.7423(3) 0.0568(13) Uani 1 1 d . . .
H6A H 0.2920 0.2472 0.7975 0.068 Uiso 1 1 calc R . .
H6B H 0.3591 0.3103 0.7361 0.068 Uiso 1 1 calc R . .
C7 C 0.2014(5) 0.4104(7) 0.6747(4) 0.0692(17) Uani 1 1 d . . .
H7A H 0.2473 0.4818 0.6745 0.083 Uiso 1 1 calc R . .
H7B H 0.1638 0.4293 0.7200 0.083 Uiso 1 1 calc R . .
C8 C 0.1486(5) 0.4115(8) 0.5945(4) 0.0760(19) Uani 1 1 d . . .
H8A H 0.0983 0.3491 0.5979 0.091 Uiso 1 1 calc R . .
H8B H 0.1277 0.5068 0.5825 0.091 Uiso 1 1 calc R . .
C9 C 0.2702(4) 0.0249(6) 0.4462(3) 0.0545(13) Uani 1 1 d . . .
C10 C 0.2876(6) -0.0513(7) 0.3770(4) 0.0751(19) Uani 1 1 d . . .
H10 H 0.3351 -0.0274 0.3457 0.090 Uiso 1 1 calc R . .
C11 C 0.2324(7) -0.1667(8) 0.3538(5) 0.090(3) Uani 1 1 d . . .
H11 H 0.2442 -0.2165 0.3064 0.109 Uiso 1 1 calc R . .
C12 C 0.1650(7) -0.2067(7) 0.3965(5) 0.088(2) Uani 1 1 d . . .
H12 H 0.1309 -0.2836 0.3789 0.106 Uiso 1 1 calc R . .
C13 C 0.1443(5) -0.1339(6) 0.4686(4) 0.0707(18) Uani 1 1 d . . .
C14 C 0.1987(4) -0.0191(6) 0.4916(3) 0.0539(13) Uani 1 1 d . . .
C15 C 0.0756(6) -0.1671(8) 0.5198(5) 0.092(3) Uani 1 1 d . . .
H15 H 0.0385 -0.2432 0.5075 0.110 Uiso 1 1 calc R . .
C16 C 0.0637(5) -0.0884(9) 0.5866(5) 0.092(2) Uani 1 1 d . . .
H16 H 0.0188 -0.1116 0.6212 0.110 Uiso 1 1 calc R . .
C17 C 0.1171(5) 0.0265(9) 0.6050(4) 0.078(2) Uani 1 1 d . . .
H17 H 0.1048 0.0823 0.6500 0.093 Uiso 1 1 calc R . .
Cl1 Cl 0.57617(11) 0.21202(15) 0.83740(10) 0.0665(4) Uani 1 1 d . . .
O2 O 0.6042(8) 0.0803(12) 0.7998(7) 0.079(3) Uiso 0.50 1 d P . .
O2' O 0.5638(11) 0.0658(17) 0.8237(10) 0.117(5) Uiso 0.50 1 d P . .
O3 O 0.5593(8) 0.3028(12) 0.7680(8) 0.088(3) Uiso 0.50 1 d P . .
O3' O 0.5212(9) 0.3096(13) 0.7993(9) 0.100(4) Uiso 0.50 1 d P . .
O4 O 0.6225(7) 0.2676(11) 0.9077(7) 0.082(3) Uiso 0.50 1 d P . .
O4' O 0.6615(8) 0.2577(13) 0.8673(8) 0.095(3) Uiso 0.50 1 d P . .
O5 O 0.4999(17) 0.243(3) 0.8740(15) 0.189(8) Uiso 0.50 1 d P . .
O5' O 0.5071(13) 0.125(2) 0.8834(12) 0.161(7) Uiso 0.50 1 d P . .
Cl2 Cl 0.08067(10) 0.11137(18) 0.83121(9) 0.0670(4) Uani 1 1 d . . .
O6 O 0.1531(4) 0.0355(7) 0.8044(4) 0.106(2) Uani 1 1 d . . .
O7 O 0.0570(10) 0.2165(15) 0.7707(9) 0.109(4) Uiso 0.50 1 d P . .
O7' O 0.0103(9) 0.1342(15) 0.7803(8) 0.106(4) Uiso 0.50 1 d P . .
O8 O 0.1211(6) 0.2418(10) 0.8668(7) 0.169(4) Uani 1 1 d . . .
O9 O 0.0538(5) 0.0619(12) 0.9051(5) 0.159(4) Uani 1 1 d . . .
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
Co 0.0471(4) 0.0430(4) 0.0475(4) -0.0006(3) 0.0015(3) -0.0075(3)
N1 0.062(3) 0.061(3) 0.067(3) 0.006(2) -0.009(2) -0.002(2)
N2 0.061(3) 0.050(3) 0.071(3) 0.010(2) -0.003(2) -0.012(2)
N3 0.057(3) 0.041(2) 0.060(3) 0.0009(19) 0.005(2) -0.0004(19)
N4 0.053(2) 0.050(2) 0.058(3) -0.009(2) 0.002(2) -0.002(2)
N5 0.059(3) 0.054(3) 0.048(2) -0.001(2) 0.001(2) -0.019(2)
O1 0.072(3) 0.064(2) 0.052(2) -0.0026(18) 0.0166(19) -0.015(2)
C1 0.099(5) 0.059(4) 0.089(5) 0.022(4) -0.018(4) -0.009(4)
C2 0.083(5) 0.062(4) 0.086(5) 0.023(3) 0.007(4) -0.020(3)
C3 0.050(4) 0.082(5) 0.142(7) 0.034(5) 0.014(4) -0.005(3)
C4 0.055(3) 0.071(4) 0.101(5) 0.014(4) 0.012(3) 0.010(3)
C5 0.070(4) 0.063(4) 0.052(3) 0.009(3) 0.000(3) 0.001(3)
C6 0.062(3) 0.063(3) 0.046(3) -0.004(2) -0.001(2) -0.002(3)
C7 0.070(4) 0.065(4) 0.073(4) -0.016(3) 0.003(3) 0.018(3)
C8 0.066(4) 0.075(4) 0.086(5) -0.009(4) -0.008(3) 0.020(3)
C9 0.070(3) 0.047(3) 0.047(3) 0.001(2) 0.000(2) 0.003(3)
C10 0.115(6) 0.059(4) 0.052(3) 0.001(3) 0.008(3) 0.019(4)
C11 0.147(8) 0.058(4) 0.065(4) -0.017(3) -0.010(5) 0.011(5)
C12 0.132(7) 0.050(4) 0.080(5) -0.009(3) -0.023(5) -0.012(4)
C13 0.097(5) 0.047(3) 0.067(4) 0.003(3) -0.020(3) -0.015(3)
C14 0.068(3) 0.046(3) 0.047(3) 0.005(2) -0.008(2) -0.010(2)
C15 0.097(6) 0.077(5) 0.098(6) 0.016(4) -0.034(5) -0.045(4)
C16 0.086(5) 0.109(6) 0.081(5) 0.005(4) 0.002(4) -0.051(5)
C17 0.074(4) 0.102(5) 0.058(3) -0.006(3) 0.011(3) -0.038(4)
Cl1 0.0753(10) 0.0488(8) 0.0747(10) -0.0065(7) -0.0058(8) 0.0027(7)
Cl2 0.0640(9) 0.0766(10) 0.0608(8) 0.0067(7) 0.0091(7) 0.0157(8)
O6 0.103(4) 0.115(4) 0.103(4) 0.031(3) 0.051(3) 0.043(4)
O8 0.145(7) 0.114(6) 0.249(12) -0.029(7) 0.005(7) -0.003(6)
O9 0.102(5) 0.269(11) 0.110(5) 0.026(6) 0.047(4) 0.030(6)
_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
Co O1 1.889(4) . ?
Co N2 1.935(5) . ?
Co N3 1.958(5) . ?
Co N4 1.959(5) . ?
Co N1 1.965(5) . ?
Co N5 1.966(4) . ?
N1 C1 1.475(9) . ?
N1 C8 1.488(9) . ?
N1 H1 0.9100 . ?
N2 C3 1.452(9) . ?
N2 C2 1.484(8) . ?
N2 H2 0.9100 . ?
N3 C5 1.488(7) . ?
N3 C4 1.502(8) . ?
N3 H3 0.9100 . ?
N4 C7 1.472(7) . ?
N4 C6 1.478(7) . ?
N4 H4 0.9100 . ?
N5 C17 1.315(8) . ?
N5 C14 1.385(7) . ?
O1 C9 1.319(7) . ?
C1 C2 1.504(11) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.444(10) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.515(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.515(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.377(8) . ?
C9 C14 1.404(8) . ?
C10 C11 1.417(11) . ?
C10 H10 0.9300 . ?
C11 C12 1.319(12) . ?
C11 H11 0.9300 . ?
C12 C13 1.412(11) . ?
C12 H12 0.9300 . ?
C13 C15 1.401(11) . ?
C13 C14 1.405(8) . ?
C15 C16 1.339(12) . ?
C15 H15 0.9300 . ?
C16 C17 1.380(10) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
Cl1 O5 1.36(3) . ?
Cl1 O3' 1.376(13) . ?
Cl1 O2' 1.406(16) . ?
Cl1 O4 1.427(11) . ?
Cl1 O3 1.438(12) . ?
Cl1 O4' 1.439(12) . ?
Cl1 O2 1.456(11) . ?
Cl1 O5' 1.55(2) . ?
O2 O2' 0.756(16) . ?
O2' O5' 1.44(2) . ?
O3 O3' 0.792(15) . ?
O3' O5 1.42(3) . ?
O4 O4' 0.911(13) . ?
O5 O5' 1.13(3) . ?
Cl2 O7' 1.352(13) . ?
Cl2 O9 1.373(7) . ?
Cl2 O6 1.399(5) . ?
Cl2 O7 1.437(15) . ?
Cl2 O8 1.484(9) . ?
O7 O7' 1.067(16) . ?
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 Co N2 86.0(2) . . ?
O1 Co N3 92.41(19) . . ?
N2 Co N3 85.1(2) . . ?
O1 Co N4 178.13(19) . . ?
N2 Co N4 94.9(2) . . ?
N3 Co N4 86.04(19) . . ?
O1 Co N1 95.3(2) . . ?
N2 Co N1 85.1(2) . . ?
N3 Co N1 167.0(2) . . ?
N4 Co N1 86.4(2) . . ?
O1 Co N5 84.65(18) . . ?
N2 Co N5 170.6(2) . . ?
N3 Co N5 95.4(2) . . ?
N4 Co N5 94.43(19) . . ?
N1 Co N5 95.6(2) . . ?
C1 N1 C8 111.9(6) . . ?
C1 N1 Co 110.7(4) . . ?
C8 N1 Co 107.2(4) . . ?
C1 N1 H1 109.0 . . ?
C8 N1 H1 109.0 . . ?
Co N1 H1 109.0 . . ?
C3 N2 C2 118.4(6) . . ?
C3 N2 Co 110.4(4) . . ?
C2 N2 Co 106.2(4) . . ?
C3 N2 H2 107.1 . . ?
C2 N2 H2 107.1 . . ?
Co N2 H2 107.1 . . ?
C5 N3 C4 113.2(5) . . ?
C5 N3 Co 108.9(3) . . ?
C4 N3 Co 109.1(4) . . ?
C5 N3 H3 108.5 . . ?
C4 N3 H3 108.5 . . ?
Co N3 H3 108.5 . . ?
C7 N4 C6 119.3(5) . . ?
C7 N4 Co 109.5(4) . . ?
C6 N4 Co 108.2(3) . . ?
C7 N4 H4 106.3 . . ?
C6 N4 H4 106.3 . . ?
Co N4 H4 106.3 . . ?
C17 N5 C14 117.9(5) . . ?
C17 N5 Co 132.7(4) . . ?
C14 N5 Co 109.4(3) . . ?
C9 O1 Co 113.2(3) . . ?
N1 C1 C2 110.4(5) . . ?
N1 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N1 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N2 C2 C1 107.6(5) . . ?
N2 C2 H2A 110.2 . . ?
C1 C2 H2A 110.2 . . ?
N2 C2 H2B 110.2 . . ?
C1 C2 H2B 110.2 . . ?
H2A C2 H2B 108.5 . . ?
C4 C3 N2 114.6(6) . . ?
C4 C3 H3A 108.6 . . ?
N2 C3 H3A 108.6 . . ?
C4 C3 H3B 108.6 . . ?
N2 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
C3 C4 N3 112.8(5) . . ?
C3 C4 H4A 109.0 . . ?
N3 C4 H4A 109.0 . . ?
C3 C4 H4B 109.0 . . ?
N3 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
N3 C5 C6 109.2(4) . . ?
N3 C5 H5A 109.8 . . ?
C6 C5 H5A 109.8 . . ?
N3 C5 H5B 109.8 . . ?
C6 C5 H5B 109.8 . . ?
H5A C5 H5B 108.3 . . ?
N4 C6 C5 105.0(5) . . ?
N4 C6 H6A 110.8 . . ?
C5 C6 H6A 110.8 . . ?
N4 C6 H6B 110.8 . . ?
C5 C6 H6B 110.8 . . ?
H6A C6 H6B 108.8 . . ?
N4 C7 C8 105.8(5) . . ?
N4 C7 H7A 110.6 . . ?
C8 C7 H7A 110.6 . . ?
N4 C7 H7B 110.6 . . ?
C8 C7 H7B 110.6 . . ?
H7A C7 H7B 108.7 . . ?
N1 C8 C7 108.1(5) . . ?
N1 C8 H8A 110.1 . . ?
C7 C8 H8A 110.1 . . ?
N1 C8 H8B 110.1 . . ?
C7 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
O1 C9 C10 125.4(6) . . ?
O1 C9 C14 117.2(5) . . ?
C10 C9 C14 117.4(6) . . ?
C9 C10 C11 119.3(7) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 H10 120.4 . . ?
C12 C11 C10 123.0(7) . . ?
C12 C11 H11 118.5 . . ?
C10 C11 H11 118.5 . . ?
C11 C12 C13 120.5(7) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C15 C13 C14 117.2(6) . . ?
C15 C13 C12 126.1(7) . . ?
C14 C13 C12 116.7(7) . . ?
N5 C14 C9 115.1(5) . . ?
N5 C14 C13 121.7(6) . . ?
C9 C14 C13 123.2(6) . . ?
C16 C15 C13 119.5(6) . . ?
C16 C15 H15 120.2 . . ?
C13 C15 H15 120.2 . . ?
C15 C16 C17 121.0(7) . . ?
C15 C16 H16 119.5 . . ?
C17 C16 H16 119.5 . . ?
N5 C17 C16 122.5(7) . . ?
N5 C17 H17 118.8 . . ?
C16 C17 H17 118.8 . . ?
O5 Cl1 O3' 62.7(12) . . ?
O5 Cl1 O2' 99.6(13) . . ?
O3' Cl1 O2' 120.3(8) . . ?
O5 Cl1 O4 88.3(12) . . ?
O3' Cl1 O4 113.3(7) . . ?
O2' Cl1 O4 123.1(8) . . ?
O5 Cl1 O3 95.3(12) . . ?
O3' Cl1 O3 32.6(6) . . ?
O2' Cl1 O3 115.9(8) . . ?
O4 Cl1 O3 119.3(7) . . ?
O5 Cl1 O4' 124.3(12) . . ?
O3' Cl1 O4' 118.8(8) . . ?
O2' Cl1 O4' 117.5(8) . . ?
O4 Cl1 O4' 37.1(5) . . ?
O3 Cl1 O4' 103.0(7) . . ?
O5 Cl1 O2 129.6(13) . . ?
O3' Cl1 O2 124.0(7) . . ?
O2' Cl1 O2 30.6(7) . . ?
O4 Cl1 O2 120.6(6) . . ?
O3 Cl1 O2 102.6(7) . . ?
O4' Cl1 O2 97.1(7) . . ?
O5 Cl1 O5' 44.9(12) . . ?
O3' Cl1 O5' 99.2(10) . . ?
O2' Cl1 O5' 58.0(9) . . ?
O4 Cl1 O5' 97.2(9) . . ?
O3 Cl1 O5' 126.4(9) . . ?
O4' Cl1 O5' 127.9(9) . . ?
O2 Cl1 O5' 88.3(9) . . ?
O2' O2 Cl1 71.1(16) . . ?
O2 O2' Cl1 78.4(17) . . ?
O2 O2' O5' 144(2) . . ?
Cl1 O2' O5' 66.1(11) . . ?
O3' O3 Cl1 69.4(14) . . ?
O3 O3' Cl1 78.0(15) . . ?
O3 O3' O5 136(2) . . ?
Cl1 O3' O5 58.0(12) . . ?
O4' O4 Cl1 72.2(11) . . ?
O4 O4' Cl1 70.8(11) . . ?
O5' O5 Cl1 77(2) . . ?
O5' O5 O3' 122(3) . . ?
Cl1 O5 O3' 59.2(12) . . ?
O5 O5' O2' 110(2) . . ?
O5 O5' Cl1 58.4(17) . . ?
O2' O5' Cl1 55.9(10) . . ?
O7' Cl2 O9 110.0(7) . . ?
O7' Cl2 O6 120.3(6) . . ?
O9 Cl2 O6 111.6(4) . . ?
O7' Cl2 O7 44.9(7) . . ?
O9 Cl2 O7 139.9(7) . . ?
O6 Cl2 O7 108.4(6) . . ?
O7' Cl2 O8 114.8(7) . . ?
O9 Cl2 O8 93.9(6) . . ?
O6 Cl2 O8 103.0(5) . . ?
O7 Cl2 O8 77.9(7) . . ?
O7' O7 Cl2 63.3(11) . . ?
O7 O7' Cl2 71.8(12) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O8 0.91 2.19 3.078(13) 165.7 4_565
N1 H1 O9 0.91 2.43 3.118(10) 132.1 4_565
N2 H2 O2' 0.91 2.13 2.904(16) 142.5 2_656
N2 H2 O2 0.91 2.27 3.138(12) 160.2 2_656
N3 H3 O4 0.91 2.18 3.045(12) 158.8 2_646
N3 H3 O4' 0.91 2.20 3.060(13) 157.3 2_646
N4 H4 O7 0.91 2.48 3.227(15) 139.2 .
N4 H4 O6 0.91 2.51 3.276(7) 141.4 .
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full 26.39
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max 1.470
_refine_diff_density_min -0.633
_refine_diff_density_rms 0.112
#===END
data_jyc24a
_database_code_depnum_ccdc_archive 'CCDC 791379'
#TrackingRef '- Structures combined.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C23 H36 Co N5 O7 S2, 2(H2 O)'
_chemical_formula_sum 'C23 H40 Co N5 O9 S2'
_chemical_formula_weight 653.65
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'
S S 0.1246 0.1234 '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'
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_H-M P212121
_symmetry_space_group_name_Hall p_2ab_2ac
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
_cell_length_a 10.0472(3)
_cell_length_b 11.1403(3)
_cell_length_c 24.8215(7)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 2778.24(14)
_cell_formula_units_Z 4
_cell_measurement_temperature 150(2)
_cell_measurement_reflns_used 8192
_cell_measurement_theta_min 1.64
_cell_measurement_theta_max 25.71
_exptl_crystal_description needle
_exptl_crystal_colour green
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.24
_exptl_crystal_size_min 0.14
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.563
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1376
_exptl_absorpt_coefficient_mu 0.828
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS; Sheldrick, 1996'
_exptl_absorpt_correction_T_min 0.7069
_exptl_absorpt_correction_T_max 0.8928
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(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 'Siemens SMART CCD'
_diffrn_measurement_method 'Area detector \w scans'
_diffrn_standards_decay_% <2%
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_reflns_number 25699
_diffrn_reflns_av_R_equivalents 0.0242
_diffrn_reflns_av_sigmaI/netI 0.0222
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 30
_diffrn_reflns_theta_min 1.64
_diffrn_reflns_theta_max 25.71
_reflns_number_total 5283
_reflns_number_gt 5093
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'SMART (Siemens, 1995)'
_computing_cell_refinement 'SAINT (Siemens, 1995)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics 'Ortep-III (Burnett & Johnson, 1996)'
_computing_publication_material 'SHELXTL (Sheldrick, 2008)'
_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^)+(0.0302P)^2^+1.1441P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens mixed
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.001(9)
_refine_ls_number_reflns 5283
_refine_ls_number_parameters 379
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0256
_refine_ls_R_factor_gt 0.0237
_refine_ls_wR_factor_ref 0.0598
_refine_ls_wR_factor_gt 0.0587
_refine_ls_goodness_of_fit_ref 1.074
_refine_ls_restrained_S_all 1.074
_refine_ls_shift/su_max 0.002
_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
Co Co 0.78768(3) 0.90841(2) 0.880670(10) 0.01261(7) Uani 1 1 d . . .
S1 S 0.63181(6) 0.87466(5) 0.63879(2) 0.02652(13) Uani 1 1 d . . .
S2 S 1.33839(5) 0.99709(5) 0.96600(2) 0.02010(11) Uani 1 1 d . . .
O1 O 0.87064(14) 1.01380(12) 0.83119(6) 0.0176(3) Uani 1 1 d . . .
O2 O 0.49901(18) 0.83319(16) 0.62425(8) 0.0389(4) Uani 1 1 d . . .
O3 O 0.62856(19) 0.97555(14) 0.67603(7) 0.0334(4) Uani 1 1 d . . .
O4 O 0.7184(2) 0.89431(18) 0.59204(7) 0.0427(5) Uani 1 1 d . . .
O5 O 1.31630(18) 0.96786(17) 0.90943(7) 0.0369(4) Uani 1 1 d . . .
O6 O 1.32314(17) 0.89549(15) 1.00159(8) 0.0362(4) Uani 1 1 d . . .
O7 O 1.46775(15) 1.05672(15) 0.97353(7) 0.0303(4) Uani 1 1 d . . .
N1 N 0.66265(17) 0.83736(15) 0.82378(7) 0.0156(3) Uani 1 1 d . . .
N2 N 0.65427(18) 1.03279(15) 0.88648(7) 0.0165(3) Uani 1 1 d . . .
H2 H 0.592(3) 1.014(2) 0.9097(10) 0.020 Uiso 1 1 d . . .
N3 N 0.86818(16) 0.98698(15) 0.94698(6) 0.0150(3) Uani 1 1 d . . .
N4 N 0.70547(19) 0.79543(15) 0.93015(7) 0.0161(3) Uani 1 1 d . . .
H4 H 0.758(3) 0.733(2) 0.9322(10) 0.019 Uiso 1 1 d . . .
N5 N 0.94252(17) 0.80249(15) 0.86611(6) 0.0154(3) Uani 1 1 d . . .
C1 C 0.5500(2) 0.92626(18) 0.81425(8) 0.0186(4) Uani 1 1 d . . .
H1A H 0.5271 0.9284 0.7755 0.022 Uiso 1 1 calc R . .
H1B H 0.4699 0.9009 0.8346 0.022 Uiso 1 1 calc R . .
C2 C 0.5932(2) 1.04905(18) 0.83264(8) 0.0197(4) Uani 1 1 d . . .
H2A H 0.6586 1.0835 0.8071 0.024 Uiso 1 1 calc R . .
H2B H 0.5157 1.1038 0.8349 0.024 Uiso 1 1 calc R . .
C3 C 0.7210(2) 1.14228(18) 0.90773(8) 0.0201(4) Uani 1 1 d . . .
H3A H 0.6548 1.2054 0.9161 0.024 Uiso 1 1 calc R . .
H3B H 0.7853 1.1744 0.8811 0.024 Uiso 1 1 calc R . .
C4 C 0.7917(2) 1.10236(18) 0.95805(8) 0.0195(4) Uani 1 1 d . . .
H4A H 0.7261 1.0886 0.9872 0.023 Uiso 1 1 calc R . .
H4B H 0.8540 1.1658 0.9700 0.023 Uiso 1 1 calc R . .
C5 C 0.8426(2) 0.90048(19) 0.99247(8) 0.0179(4) Uani 1 1 d . . .
H5A H 0.8484 0.9430 1.0274 0.021 Uiso 1 1 calc R . .
H5B H 0.9104 0.8360 0.9921 0.021 Uiso 1 1 calc R . .
C6 C 0.7049(2) 0.84681(19) 0.98559(8) 0.0191(4) Uani 1 1 d . . .
H6A H 0.6885 0.7834 1.0128 0.023 Uiso 1 1 calc R . .
H6B H 0.6354 0.9093 0.9892 0.023 Uiso 1 1 calc R . .
C7 C 0.5782(2) 0.7494(2) 0.90749(8) 0.0194(4) Uani 1 1 d . . .
H7A H 0.5067 0.8100 0.9111 0.023 Uiso 1 1 calc R . .
H7B H 0.5503 0.6751 0.9262 0.023 Uiso 1 1 calc R . .
C8 C 0.6081(2) 0.72459(18) 0.84848(8) 0.0182(4) Uani 1 1 d . . .
H8A H 0.6740 0.6589 0.8453 0.022 Uiso 1 1 calc R . .
H8B H 0.5258 0.7000 0.8295 0.022 Uiso 1 1 calc R . .
C9 C 0.7297(2) 0.81077(19) 0.77121(8) 0.0176(4) Uani 1 1 d . . .
H9A H 0.8129 0.7661 0.7787 0.021 Uiso 1 1 calc R . .
H9B H 0.7549 0.8879 0.7542 0.021 Uiso 1 1 calc R . .
C10 C 0.6472(2) 0.73837(18) 0.73073(8) 0.0185(4) Uani 1 1 d . . .
H10A H 0.5540 0.7671 0.7309 0.022 Uiso 1 1 calc R . .
H10B H 0.6475 0.6525 0.7410 0.022 Uiso 1 1 calc R . .
C11 C 0.7075(2) 0.75356(19) 0.67412(8) 0.0220(4) Uani 1 1 d . . .
H11A H 0.6951 0.6784 0.6534 0.026 Uiso 1 1 calc R . .
H11B H 0.8043 0.7686 0.6773 0.026 Uiso 1 1 calc R . .
C12 C 1.0136(2) 1.01517(19) 0.94176(8) 0.0170(4) Uani 1 1 d . . .
H12A H 1.0250 1.0778 0.9139 0.020 Uiso 1 1 calc R . .
H12B H 1.0607 0.9423 0.9292 0.020 Uiso 1 1 calc R . .
C13 C 1.0786(2) 1.05850(19) 0.99397(8) 0.0193(4) Uani 1 1 d . . .
H13A H 1.0229 1.1225 1.0100 0.023 Uiso 1 1 calc R . .
H13B H 1.0821 0.9910 1.0199 0.023 Uiso 1 1 calc R . .
C14 C 1.2190(2) 1.10674(18) 0.98522(8) 0.0181(4) Uani 1 1 d . . .
H14A H 1.2494 1.1454 1.0190 0.022 Uiso 1 1 calc R . .
H14B H 1.2157 1.1695 0.9570 0.022 Uiso 1 1 calc R . .
C15 C 0.9804(2) 0.69663(18) 0.88587(9) 0.0204(4) Uani 1 1 d . . .
H15 H 0.9271 0.6591 0.9126 0.024 Uiso 1 1 calc R . .
C16 C 1.0977(2) 0.6384(2) 0.86823(9) 0.0273(5) Uani 1 1 d . . .
H16 H 1.1236 0.5645 0.8842 0.033 Uiso 1 1 calc R . .
C17 C 1.1737(2) 0.6875(2) 0.82867(10) 0.0284(5) Uani 1 1 d . . .
H17 H 1.2510 0.6468 0.8164 0.034 Uiso 1 1 calc R . .
C18 C 1.1376(2) 0.7989(2) 0.80582(9) 0.0226(5) Uani 1 1 d . . .
C19 C 1.2048(3) 0.8563(2) 0.76329(9) 0.0315(5) Uani 1 1 d . . .
H19 H 1.2810 0.8200 0.7475 0.038 Uiso 1 1 calc R . .
C20 C 1.1597(3) 0.9650(2) 0.74466(9) 0.0315(6) Uani 1 1 d . . .
H20 H 1.2052 1.0023 0.7156 0.038 Uiso 1 1 calc R . .
C21 C 1.0485(2) 1.0227(2) 0.76721(9) 0.0263(5) Uani 1 1 d . . .
H21 H 1.0214 1.0991 0.7542 0.032 Uiso 1 1 calc R . .
C22 C 0.9790(2) 0.96790(18) 0.80832(8) 0.0180(4) Uani 1 1 d . . .
C23 C 1.0217(2) 0.85435(18) 0.82715(8) 0.0166(4) Uani 1 1 d . . .
O8 O 0.2572(2) 0.97505(17) 0.61749(9) 0.0445(5) Uani 1 1 d . . .
H8C H 0.336(3) 0.921(3) 0.6200(13) 0.053 Uiso 1 1 d . . .
H8D H 0.189(3) 0.922(3) 0.6090(13) 0.053 Uiso 1 1 d . . .
O9 O 1.4956(2) 1.1540(2) 1.07816(9) 0.0490(5) Uani 1 1 d . . .
H9C H 1.502(3) 1.118(3) 1.0393(14) 0.059 Uiso 1 1 d . . .
H9D H 1.592(4) 1.154(3) 1.0852(14) 0.059 Uiso 1 1 d . . .
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
Co 0.01172(12) 0.01338(12) 0.01275(12) 0.00077(10) -0.00044(10) 0.00172(11)
S1 0.0322(3) 0.0267(3) 0.0206(3) 0.0048(2) -0.0072(2) -0.0136(2)
S2 0.0151(2) 0.0204(2) 0.0248(3) -0.0020(2) -0.0001(2) 0.0034(2)
O1 0.0150(7) 0.0167(7) 0.0210(7) 0.0031(6) 0.0014(6) 0.0004(6)
O2 0.0366(10) 0.0342(9) 0.0457(11) 0.0082(9) -0.0201(9) -0.0131(8)
O3 0.0427(11) 0.0231(8) 0.0344(9) 0.0028(7) -0.0087(8) -0.0091(8)
O4 0.0548(12) 0.0494(11) 0.0239(8) 0.0079(8) 0.0015(9) -0.0199(11)
O5 0.0317(10) 0.0500(11) 0.0291(9) -0.0162(8) -0.0011(7) 0.0119(8)
O6 0.0364(10) 0.0254(8) 0.0468(10) 0.0096(8) 0.0034(8) 0.0063(8)
O7 0.0150(8) 0.0359(9) 0.0400(10) -0.0054(7) 0.0019(7) -0.0005(7)
N1 0.0163(8) 0.0167(8) 0.0139(8) 0.0011(7) -0.0001(7) 0.0009(7)
N2 0.0154(8) 0.0169(8) 0.0173(8) -0.0015(7) -0.0013(7) 0.0023(7)
N3 0.0125(9) 0.0163(8) 0.0161(8) -0.0001(7) -0.0008(6) 0.0027(7)
N4 0.0144(8) 0.0184(8) 0.0156(8) 0.0012(7) -0.0001(7) 0.0012(8)
N5 0.0150(8) 0.0169(8) 0.0143(8) -0.0024(6) -0.0018(7) 0.0015(7)
C1 0.0158(10) 0.0220(11) 0.0181(10) 0.0001(8) -0.0041(8) 0.0032(8)
C2 0.0197(11) 0.0200(10) 0.0194(10) 0.0017(8) -0.0069(9) 0.0064(8)
C3 0.0200(10) 0.0156(9) 0.0248(10) -0.0036(8) -0.0037(10) 0.0044(9)
C4 0.0178(10) 0.0169(9) 0.0239(10) -0.0056(8) -0.0025(9) 0.0048(10)
C5 0.0191(10) 0.0228(10) 0.0117(9) 0.0018(8) -0.0013(8) 0.0042(9)
C6 0.0187(10) 0.0248(10) 0.0139(9) 0.0014(8) 0.0046(8) 0.0006(9)
C7 0.0161(10) 0.0229(11) 0.0191(10) 0.0006(8) 0.0010(9) -0.0035(8)
C8 0.0173(10) 0.0194(10) 0.0180(10) 0.0013(8) 0.0000(8) -0.0029(8)
C9 0.0163(10) 0.0213(10) 0.0152(9) -0.0017(8) 0.0010(8) -0.0008(8)
C10 0.0190(10) 0.0186(10) 0.0178(10) -0.0006(8) -0.0005(9) -0.0035(8)
C11 0.0219(11) 0.0263(10) 0.0179(10) -0.0041(8) -0.0006(10) -0.0069(10)
C12 0.0136(10) 0.0209(10) 0.0163(9) -0.0012(8) -0.0018(8) 0.0012(8)
C13 0.0150(10) 0.0258(11) 0.0169(10) -0.0038(8) -0.0021(8) 0.0017(8)
C14 0.0164(10) 0.0172(9) 0.0208(9) -0.0031(8) -0.0013(8) 0.0014(9)
C15 0.0213(10) 0.0188(10) 0.0209(10) 0.0001(9) -0.0025(9) 0.0026(8)
C16 0.0283(12) 0.0206(10) 0.0331(13) -0.0016(9) -0.0060(10) 0.0087(9)
C17 0.0196(12) 0.0286(12) 0.0369(13) -0.0109(11) -0.0001(10) 0.0077(9)
C18 0.0162(11) 0.0271(11) 0.0245(11) -0.0098(9) -0.0015(9) -0.0018(9)
C19 0.0223(12) 0.0413(13) 0.0308(12) -0.0126(10) 0.0090(10) -0.0044(11)
C20 0.0293(13) 0.0407(14) 0.0246(12) -0.0029(10) 0.0098(10) -0.0131(11)
C21 0.0245(12) 0.0293(12) 0.0251(11) 0.0026(9) 0.0014(9) -0.0067(9)
C22 0.0179(11) 0.0194(10) 0.0165(9) -0.0010(8) -0.0022(8) -0.0040(8)
C23 0.0140(10) 0.0210(10) 0.0149(9) -0.0042(8) -0.0007(8) -0.0019(8)
O8 0.0504(12) 0.0407(11) 0.0425(10) -0.0075(9) 0.0056(10) -0.0035(9)
O9 0.0531(13) 0.0509(12) 0.0431(11) -0.0038(10) -0.0065(10) 0.0070(11)
_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
Co O1 1.8925(14) . ?
Co N2 1.9332(17) . ?
Co N4 1.9429(17) . ?
Co N5 1.9858(17) . ?
Co N3 2.0321(17) . ?
Co N1 2.0491(17) . ?
S1 O3 1.4557(18) . ?
S1 O2 1.4574(18) . ?
S1 O4 1.4667(19) . ?
S1 C11 1.780(2) . ?
S2 O6 1.4441(18) . ?
S2 O5 1.4583(17) . ?
S2 O7 1.4716(17) . ?
S2 C14 1.777(2) . ?
O1 C22 1.330(3) . ?
N1 C9 1.498(2) . ?
N1 C8 1.501(3) . ?
N1 C1 1.523(3) . ?
N2 C2 1.482(3) . ?
N2 C3 1.489(3) . ?
N2 H2 0.87(3) . ?
N3 C12 1.500(3) . ?
N3 C5 1.506(3) . ?
N3 C4 1.523(2) . ?
N4 C7 1.488(3) . ?
N4 C6 1.490(2) . ?
N4 H4 0.87(3) . ?
N5 C15 1.333(3) . ?
N5 C23 1.379(3) . ?
C1 C2 1.506(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.504(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.517(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.521(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.532(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.539(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.529(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.526(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.414(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.358(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.412(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.406(3) . ?
C18 C23 1.420(3) . ?
C19 C20 1.373(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.406(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.379(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.415(3) . ?
O8 H8C 0.99(3) . ?
O8 H8D 0.93(4) . ?
O9 H9C 1.05(3) . ?
O9 H9D 0.98(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 Co N2 84.79(7) . . ?
O1 Co N4 177.95(7) . . ?
N2 Co N4 97.03(8) . . ?
O1 Co N5 84.57(6) . . ?
N2 Co N5 169.32(7) . . ?
N4 Co N5 93.62(7) . . ?
O1 Co N3 94.77(7) . . ?
N2 Co N3 84.66(7) . . ?
N4 Co N3 86.34(7) . . ?
N5 Co N3 95.25(7) . . ?
O1 Co N1 93.58(6) . . ?
N2 Co N1 84.45(7) . . ?
N4 Co N1 85.69(7) . . ?
N5 Co N1 97.20(7) . . ?
N3 Co N1 165.61(7) . . ?
O3 S1 O2 112.43(12) . . ?
O3 S1 O4 113.61(11) . . ?
O2 S1 O4 113.23(11) . . ?
O3 S1 C11 106.37(10) . . ?
O2 S1 C11 105.84(10) . . ?
O4 S1 C11 104.45(12) . . ?
O6 S2 O5 113.44(12) . . ?
O6 S2 O7 111.70(11) . . ?
O5 S2 O7 110.95(11) . . ?
O6 S2 C14 107.63(10) . . ?
O5 S2 C14 108.02(10) . . ?
O7 S2 C14 104.58(10) . . ?
C22 O1 Co 113.52(13) . . ?
C9 N1 C8 110.75(15) . . ?
C9 N1 C1 109.13(15) . . ?
C8 N1 C1 109.65(16) . . ?
C9 N1 Co 113.65(13) . . ?
C8 N1 Co 105.39(12) . . ?
C1 N1 Co 108.15(12) . . ?
C2 N2 C3 113.96(16) . . ?
C2 N2 Co 107.91(12) . . ?
C3 N2 Co 107.54(13) . . ?
C2 N2 H2 109.3(16) . . ?
C3 N2 H2 106.4(16) . . ?
Co N2 H2 111.8(16) . . ?
C12 N3 C5 111.40(15) . . ?
C12 N3 C4 109.29(16) . . ?
C5 N3 C4 108.58(15) . . ?
C12 N3 Co 114.08(12) . . ?
C5 N3 Co 105.29(12) . . ?
C4 N3 Co 107.99(12) . . ?
C7 N4 C6 118.54(17) . . ?
C7 N4 Co 110.46(13) . . ?
C6 N4 Co 109.67(13) . . ?
C7 N4 H4 105.7(16) . . ?
C6 N4 H4 104.6(16) . . ?
Co N4 H4 107.1(16) . . ?
C15 N5 C23 117.64(18) . . ?
C15 N5 Co 133.06(15) . . ?
C23 N5 Co 109.31(13) . . ?
C2 C1 N1 109.22(16) . . ?
C2 C1 H1A 109.8 . . ?
N1 C1 H1A 109.8 . . ?
C2 C1 H1B 109.8 . . ?
N1 C1 H1B 109.8 . . ?
H1A C1 H1B 108.3 . . ?
N2 C2 C1 106.36(16) . . ?
N2 C2 H2A 110.5 . . ?
C1 C2 H2A 110.5 . . ?
N2 C2 H2B 110.5 . . ?
C1 C2 H2B 110.5 . . ?
H2A C2 H2B 108.6 . . ?
N2 C3 C4 105.35(16) . . ?
N2 C3 H3A 110.7 . . ?
C4 C3 H3A 110.7 . . ?
N2 C3 H3B 110.7 . . ?
C4 C3 H3B 110.7 . . ?
H3A C3 H3B 108.8 . . ?
C3 C4 N3 109.75(15) . . ?
C3 C4 H4A 109.7 . . ?
N3 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
N3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
N3 C5 C6 108.87(15) . . ?
N3 C5 H5A 109.9 . . ?
C6 C5 H5A 109.9 . . ?
N3 C5 H5B 109.9 . . ?
C6 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
N4 C6 C5 104.57(16) . . ?
N4 C6 H6A 110.8 . . ?
C5 C6 H6A 110.8 . . ?
N4 C6 H6B 110.8 . . ?
C5 C6 H6B 110.8 . . ?
H6A C6 H6B 108.9 . . ?
N4 C7 C8 104.89(17) . . ?
N4 C7 H7A 110.8 . . ?
C8 C7 H7A 110.8 . . ?
N4 C7 H7B 110.8 . . ?
C8 C7 H7B 110.8 . . ?
H7A C7 H7B 108.8 . . ?
N1 C8 C7 108.25(17) . . ?
N1 C8 H8A 110.0 . . ?
C7 C8 H8A 110.0 . . ?
N1 C8 H8B 110.0 . . ?
C7 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
N1 C9 C10 115.62(17) . . ?
N1 C9 H9A 108.4 . . ?
C10 C9 H9A 108.4 . . ?
N1 C9 H9B 108.4 . . ?
C10 C9 H9B 108.4 . . ?
H9A C9 H9B 107.4 . . ?
C9 C10 C11 109.16(17) . . ?
C9 C10 H10A 109.8 . . ?
C11 C10 H10A 109.8 . . ?
C9 C10 H10B 109.8 . . ?
C11 C10 H10B 109.8 . . ?
H10A C10 H10B 108.3 . . ?
C10 C11 S1 111.42(16) . . ?
C10 C11 H11A 109.3 . . ?
S1 C11 H11A 109.3 . . ?
C10 C11 H11B 109.3 . . ?
S1 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
N3 C12 C13 114.14(16) . . ?
N3 C12 H12A 108.7 . . ?
C13 C12 H12A 108.7 . . ?
N3 C12 H12B 108.7 . . ?
C13 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
C14 C13 C12 112.69(17) . . ?
C14 C13 H13A 109.1 . . ?
C12 C13 H13A 109.1 . . ?
C14 C13 H13B 109.1 . . ?
C12 C13 H13B 109.1 . . ?
H13A C13 H13B 107.8 . . ?
C13 C14 S2 114.86(14) . . ?
C13 C14 H14A 108.6 . . ?
S2 C14 H14A 108.6 . . ?
C13 C14 H14B 108.6 . . ?
S2 C14 H14B 108.6 . . ?
H14A C14 H14B 107.5 . . ?
N5 C15 C16 122.0(2) . . ?
N5 C15 H15 119.0 . . ?
C16 C15 H15 119.0 . . ?
C17 C16 C15 120.5(2) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C16 C17 C18 120.0(2) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C19 C18 C17 125.3(2) . . ?
C19 C18 C23 118.4(2) . . ?
C17 C18 C23 116.3(2) . . ?
C20 C19 C18 119.7(2) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C19 C20 C21 122.1(2) . . ?
C19 C20 H20 118.9 . . ?
C21 C20 H20 118.9 . . ?
C22 C21 C20 119.6(2) . . ?
C22 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
O1 C22 C21 124.0(2) . . ?
O1 C22 C23 116.79(18) . . ?
C21 C22 C23 119.1(2) . . ?
N5 C23 C22 115.55(18) . . ?
N5 C23 C18 123.51(19) . . ?
C22 C23 C18 120.9(2) . . ?
H8C O8 H8D 103(3) . . ?
H9C O9 H9D 96(3) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2 O7 0.87(3) 2.07(3) 2.873(2) 152(2) 1_455
N4 H4 O6 0.87(3) 2.28(2) 2.965(2) 136(2) 4_467
O8 H8C O2 0.99(3) 1.91(3) 2.904(3) 174(3) .
O8 H8D O9 0.93(4) 2.17(4) 3.077(3) 163(3) 2_674
O9 H9C O7 1.05(3) 1.80(4) 2.828(3) 165(3) .
O9 H9D O4 0.98(4) 1.99(4) 2.943(3) 163(3) 2_775
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 25.71
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 0.524
_refine_diff_density_min -0.322
_refine_diff_density_rms 0.053
#===END
data_jyc113
_database_code_depnum_ccdc_archive 'CCDC 791380'
#TrackingRef '- Structures combined.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C10 H24 Co F6 N4 O8 S2, C F3 O3 S'
_chemical_formula_sum 'C11 H24 Co F9 N4 O11 S3'
_chemical_formula_weight 714.45
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'
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M P21/n
_symmetry_space_group_name_Hall -p_2yn
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 8.7978(1)
_cell_length_b 22.2897(4)
_cell_length_c 12.9870(2)
_cell_angle_alpha 90.00
_cell_angle_beta 96.716(1)
_cell_angle_gamma 90.00
_cell_volume 2529.28(7)
_cell_formula_units_Z 4
_cell_measurement_temperature 85(2)
_cell_measurement_reflns_used 5689
_cell_measurement_theta_min 1.82
_cell_measurement_theta_max 26.41
_exptl_crystal_description plate
_exptl_crystal_colour red
_exptl_crystal_size_max 0.42
_exptl_crystal_size_mid 0.24
_exptl_crystal_size_min 0.10
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.876
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1448
_exptl_absorpt_coefficient_mu 1.051
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS; Sheldrick, 1996'
_exptl_absorpt_correction_T_min 0.6993
_exptl_absorpt_correction_T_max 0.8310
_diffrn_ambient_temperature 85
_diffrn_measurement_device_type 'Siemens SMART CCD'
_diffrn_measurement_method 'Area detector \w scans'
_diffrn_standards_decay_% <2%
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_reflns_number 15193
_diffrn_reflns_av_R_equivalents 0.0204
_diffrn_reflns_av_sigmaI/netI 0.0249
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 27
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_theta_min 1.82
_diffrn_reflns_theta_max 26.41
_reflns_number_total 5150
_reflns_number_gt 4583
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'SMART (Siemens, 1995)'
_computing_cell_refinement 'SAINT (Siemens, 1995)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics 'Ortep-III (Burnett & Johnson, 1996)'
_computing_publication_material 'SHELXTL (Sheldrick, 2008)'
_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^)+(0.0168P)^2^+2.5473P] 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 mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 5150
_refine_ls_number_parameters 368
_refine_ls_number_restraints 4
_refine_ls_R_factor_all 0.0348
_refine_ls_R_factor_gt 0.0283
_refine_ls_wR_factor_ref 0.0640
_refine_ls_wR_factor_gt 0.0611
_refine_ls_goodness_of_fit_ref 1.098
_refine_ls_restrained_S_all 1.097
_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
Co Co 0.67340(3) 0.169160(11) 0.494554(19) 0.01351(7) Uani 1 1 d . . .
S1 S 0.73436(6) 0.34521(2) 0.21607(4) 0.01863(11) Uani 1 1 d . . .
O1 O 0.51727(16) 0.12476(6) 0.55876(11) 0.0192(3) Uani 1 1 d D . .
F1 F 0.82393(16) 0.41216(6) 0.37785(11) 0.0372(3) Uani 1 1 d . . .
N1 N 0.82322(18) 0.13306(7) 0.59476(12) 0.0161(3) Uani 1 1 d . . .
H1 H 0.9181 0.1454 0.5827 0.019 Uiso 1 1 calc R . .
C1 C 0.7926(2) 0.15423(9) 0.69923(15) 0.0189(4) Uani 1 1 d . . .
H1A H 0.8752 0.1425 0.7515 0.023 Uiso 1 1 calc R . .
H1B H 0.6977 0.1373 0.7174 0.023 Uiso 1 1 calc R . .
S2 S 0.26879(6) 0.08183(2) 0.30993(4) 0.01816(11) Uani 1 1 d . . .
O2 O 0.50995(16) 0.20524(6) 0.39907(11) 0.0177(3) Uani 1 1 d D . .
F2 F 0.83860(17) 0.45527(6) 0.23063(12) 0.0400(4) Uani 1 1 d . . .
N2 N 0.69152(19) 0.23884(7) 0.58985(13) 0.0177(3) Uani 1 1 d . . .
H2 H 0.5964 0.2512 0.6013 0.021 Uiso 1 1 calc R . .
C2 C 0.7814(2) 0.22176(9) 0.69172(15) 0.0203(4) Uani 1 1 d . . .
H2A H 0.7309 0.2373 0.7487 0.024 Uiso 1 1 calc R . .
H2B H 0.8831 0.2390 0.6963 0.024 Uiso 1 1 calc R . .
S3 S 0.20180(6) -0.18654(2) -0.05413(4) 0.02090(11) Uani 1 1 d . . .
F3 F 0.61929(16) 0.44305(6) 0.28635(12) 0.0366(3) Uani 1 1 d . . .
N3 N 0.80829(18) 0.21210(7) 0.41630(13) 0.0171(3) Uani 1 1 d . . .
H3 H 0.7464 0.2319 0.3665 0.021 Uiso 1 1 calc R . .
O3 O 0.65433(16) 0.36019(7) 0.11560(11) 0.0234(3) Uani 1 1 d . . .
C3 C 0.7702(2) 0.28820(9) 0.53799(16) 0.0216(4) Uani 1 1 d . . .
H3A H 0.8172 0.3162 0.5893 0.026 Uiso 1 1 calc R . .
H3B H 0.6969 0.3099 0.4902 0.026 Uiso 1 1 calc R . .
F4 F 0.31239(18) -0.01470(6) 0.20417(11) 0.0380(3) Uani 1 1 d . . .
O4 O 0.89148(16) 0.32576(7) 0.21241(12) 0.0245(3) Uani 1 1 d . . .
N4 N 0.71062(19) 0.09941(7) 0.40669(13) 0.0173(3) Uani 1 1 d . . .
H4 H 0.6196 0.0821 0.3829 0.021 Uiso 1 1 calc R . .
C4 C 0.8911(2) 0.25955(9) 0.48007(16) 0.0210(4) Uani 1 1 d . . .
H4A H 0.9348 0.2887 0.4366 0.025 Uiso 1 1 calc R . .
H4B H 0.9725 0.2424 0.5280 0.025 Uiso 1 1 calc R . .
O5 O 0.65002(16) 0.30961(7) 0.28231(11) 0.0235(3) Uani 1 1 d . . .
F5 F 0.22014(19) 0.05998(7) 0.11152(11) 0.0447(4) Uani 1 1 d . . .
O6 O 0.11691(16) 0.06246(7) 0.32173(12) 0.0258(3) Uani 1 1 d . . .
F6 F 0.45836(18) 0.05963(7) 0.17523(12) 0.0455(4) Uani 1 1 d . . .
C5 C 0.8992(2) 0.17012(9) 0.35937(16) 0.0200(4) Uani 1 1 d . . .
H5A H 0.9818 0.1525 0.4056 0.024 Uiso 1 1 calc R . .
H5B H 0.9423 0.1906 0.3036 0.024 Uiso 1 1 calc R . .
O7 O 0.38642(16) 0.06008(6) 0.39018(11) 0.0215(3) Uani 1 1 d . . .
F7 F 0.22599(19) -0.07024(6) -0.07090(12) 0.0438(4) Uani 1 1 d . . .
C6 C 0.7856(2) 0.12257(9) 0.31682(15) 0.0201(4) Uani 1 1 d . . .
H6A H 0.7097 0.1397 0.2649 0.024 Uiso 1 1 calc R . .
H6B H 0.8377 0.0903 0.2852 0.024 Uiso 1 1 calc R . .
F8 F 0.35200(17) -0.10831(7) 0.06642(12) 0.0476(4) Uani 1 1 d . . .
O8 O 0.28682(18) 0.14497(6) 0.28659(12) 0.0264(3) Uani 1 1 d . . .
C7 C 0.8114(2) 0.05378(9) 0.46785(16) 0.0207(4) Uani 1 1 d . . .
H7A H 0.7724 0.0137 0.4525 0.025 Uiso 1 1 calc R . .
H7B H 0.9146 0.0560 0.4488 0.025 Uiso 1 1 calc R . .
F9 F 0.10650(17) -0.09891(7) 0.05569(11) 0.0420(4) Uani 1 1 d . . .
O9 O 0.20315(19) -0.22502(8) 0.03657(13) 0.0340(4) Uani 1 1 d . . .
C8 C 0.8128(2) 0.06671(8) 0.58220(16) 0.0200(4) Uani 1 1 d . . .
H8A H 0.7199 0.0518 0.6068 0.024 Uiso 1 1 calc R . .
H8B H 0.8999 0.0474 0.6215 0.024 Uiso 1 1 calc R . .
O10 O 0.05575(17) -0.18424(7) -0.11766(11) 0.0253(3) Uani 1 1 d . . .
C9 C 0.7556(2) 0.41793(10) 0.28195(17) 0.0260(5) Uani 1 1 d . . .
O11 O 0.33277(17) -0.19261(7) -0.10958(12) 0.0261(3) Uani 1 1 d . . .
C10 C 0.3169(3) 0.04445(10) 0.19297(18) 0.0280(5) Uani 1 1 d . . .
C11 C 0.2221(3) -0.11176(11) 0.00197(18) 0.0299(5) Uani 1 1 d . . .
HO2B H 0.456(2) 0.2292(9) 0.4263(19) 0.039(8) Uiso 1 1 d D . .
HO2A H 0.453(3) 0.1831(10) 0.3621(18) 0.043(8) Uiso 1 1 d D . .
HO1A H 0.461(3) 0.1083(12) 0.5126(15) 0.043(8) Uiso 1 1 d D . .
HO1B H 0.472(3) 0.1431(12) 0.6009(17) 0.046(9) Uiso 1 1 d D . .
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
Co 0.01271(13) 0.01334(12) 0.01442(13) 0.00037(10) 0.00129(9) 0.00009(9)
S1 0.0157(2) 0.0204(2) 0.0200(2) 0.00337(19) 0.00307(19) 0.00027(18)
O1 0.0179(7) 0.0221(7) 0.0180(7) -0.0010(6) 0.0033(6) -0.0026(6)
F1 0.0407(8) 0.0395(8) 0.0285(7) -0.0057(6) -0.0083(6) 0.0000(6)
N1 0.0158(8) 0.0154(8) 0.0174(8) 0.0005(6) 0.0031(6) -0.0012(6)
C1 0.0188(10) 0.0221(10) 0.0154(10) 0.0006(8) 0.0002(8) 0.0003(8)
S2 0.0175(2) 0.0141(2) 0.0223(3) -0.00172(18) 0.00019(19) -0.00101(18)
O2 0.0176(7) 0.0162(7) 0.0187(7) -0.0015(6) -0.0010(6) 0.0011(6)
F2 0.0424(8) 0.0269(7) 0.0508(9) 0.0058(6) 0.0061(7) -0.0137(6)
N2 0.0172(8) 0.0168(8) 0.0183(8) 0.0000(7) -0.0008(7) 0.0011(6)
C2 0.0220(10) 0.0221(10) 0.0158(10) -0.0029(8) -0.0027(8) 0.0019(8)
S3 0.0210(3) 0.0217(2) 0.0194(3) 0.00374(19) 0.0000(2) -0.00455(19)
F3 0.0306(7) 0.0311(7) 0.0469(9) -0.0092(6) -0.0002(6) 0.0094(6)
N3 0.0167(8) 0.0167(8) 0.0178(8) 0.0028(6) 0.0014(7) -0.0013(6)
O3 0.0205(7) 0.0295(8) 0.0199(7) 0.0030(6) 0.0011(6) 0.0013(6)
C3 0.0246(11) 0.0135(9) 0.0258(11) 0.0002(8) -0.0006(9) -0.0018(8)
F4 0.0622(10) 0.0195(7) 0.0338(8) -0.0069(6) 0.0124(7) 0.0008(6)
O4 0.0169(7) 0.0309(8) 0.0261(8) 0.0048(6) 0.0044(6) 0.0039(6)
N4 0.0164(8) 0.0172(8) 0.0183(8) -0.0003(6) 0.0022(6) -0.0007(6)
C4 0.0203(10) 0.0178(10) 0.0242(11) 0.0021(8) -0.0002(8) -0.0046(8)
O5 0.0210(8) 0.0237(7) 0.0266(8) 0.0052(6) 0.0064(6) -0.0016(6)
F5 0.0685(11) 0.0400(8) 0.0226(7) -0.0016(6) -0.0073(7) -0.0027(7)
O6 0.0182(7) 0.0206(7) 0.0387(9) -0.0018(6) 0.0040(7) -0.0007(6)
F6 0.0467(9) 0.0474(9) 0.0480(9) -0.0017(7) 0.0286(8) -0.0036(7)
C5 0.0168(10) 0.0240(10) 0.0203(10) 0.0015(8) 0.0068(8) 0.0012(8)
O7 0.0197(7) 0.0200(7) 0.0236(8) 0.0007(6) -0.0018(6) -0.0020(6)
F7 0.0674(11) 0.0216(7) 0.0446(9) -0.0016(6) 0.0159(8) -0.0079(7)
C6 0.0201(10) 0.0244(10) 0.0164(10) -0.0005(8) 0.0050(8) 0.0010(8)
F8 0.0370(8) 0.0564(10) 0.0468(9) -0.0233(8) -0.0062(7) -0.0112(7)
O8 0.0297(8) 0.0154(7) 0.0318(9) 0.0009(6) -0.0061(7) -0.0032(6)
C7 0.0220(10) 0.0156(9) 0.0245(11) 0.0012(8) 0.0025(8) 0.0042(8)
F9 0.0433(9) 0.0535(9) 0.0311(8) -0.0101(7) 0.0124(7) 0.0053(7)
O9 0.0317(9) 0.0408(10) 0.0279(9) 0.0157(7) -0.0029(7) -0.0122(7)
C8 0.0229(11) 0.0122(9) 0.0245(11) 0.0029(8) 0.0012(8) 0.0020(8)
O10 0.0228(8) 0.0280(8) 0.0238(8) 0.0040(6) -0.0032(6) -0.0055(6)
C9 0.0239(11) 0.0257(11) 0.0276(11) 0.0001(9) -0.0001(9) -0.0010(9)
O11 0.0242(8) 0.0277(8) 0.0263(8) 0.0045(6) 0.0032(6) 0.0038(6)
C10 0.0372(13) 0.0228(11) 0.0246(11) -0.0014(9) 0.0061(10) -0.0018(9)
C11 0.0315(12) 0.0336(13) 0.0249(12) -0.0059(10) 0.0049(10) -0.0065(10)
_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
Co N3 1.9077(16) . ?
Co N1 1.9175(16) . ?
Co O1 1.9570(14) . ?
Co O2 1.9584(14) . ?
Co N4 1.9783(16) . ?
Co N2 1.9807(16) . ?
S1 O5 1.4387(15) . ?
S1 O3 1.4474(15) . ?
S1 O4 1.4548(15) . ?
S1 C9 1.832(2) . ?
O1 HO1A 0.8200(10) . ?
O1 HO1B 0.8200(10) . ?
F1 C9 1.325(3) . ?
N1 C8 1.489(2) . ?
N1 C1 1.491(2) . ?
N1 H1 0.9100 . ?
C1 C2 1.511(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
S2 O6 1.4295(15) . ?
S2 O8 1.4521(15) . ?
S2 O7 1.4629(15) . ?
S2 C10 1.825(2) . ?
O2 HO2B 0.8200(10) . ?
O2 HO2A 0.8200(10) . ?
F2 C9 1.336(3) . ?
N2 C3 1.501(3) . ?
N2 C2 1.508(2) . ?
N2 H2 0.9100 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
S3 O11 1.4347(16) . ?
S3 O10 1.4444(15) . ?
S3 O9 1.4561(16) . ?
S3 C11 1.820(2) . ?
F3 C9 1.330(3) . ?
N3 C4 1.481(2) . ?
N3 C5 1.483(2) . ?
N3 H3 0.9100 . ?
C3 C4 1.514(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
F4 C10 1.327(3) . ?
N4 C6 1.498(2) . ?
N4 C7 1.512(2) . ?
N4 H4 0.9100 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
F5 C10 1.324(3) . ?
F6 C10 1.336(3) . ?
C5 C6 1.516(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
F7 C11 1.327(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
F8 C11 1.337(3) . ?
C7 C8 1.511(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
F9 C11 1.330(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 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
N3 Co N1 98.69(7) . . ?
N3 Co O1 172.80(7) . . ?
N1 Co O1 87.68(7) . . ?
N3 Co O2 85.01(7) . . ?
N1 Co O2 176.01(7) . . ?
O1 Co O2 88.71(6) . . ?
N3 Co N4 86.09(7) . . ?
N1 Co N4 85.11(7) . . ?
O1 Co N4 91.15(6) . . ?
O2 Co N4 96.68(6) . . ?
N3 Co N2 85.98(7) . . ?
N1 Co N2 84.62(7) . . ?
O1 Co N2 98.02(7) . . ?
O2 Co N2 94.19(6) . . ?
N4 Co N2 165.93(7) . . ?
O5 S1 O3 115.83(9) . . ?
O5 S1 O4 114.43(9) . . ?
O3 S1 O4 113.78(9) . . ?
O5 S1 C9 103.91(10) . . ?
O3 S1 C9 103.25(9) . . ?
O4 S1 C9 103.51(10) . . ?
Co O1 HO1A 108(2) . . ?
Co O1 HO1B 117(2) . . ?
HO1A O1 HO1B 114(3) . . ?
C8 N1 C1 113.49(15) . . ?
C8 N1 Co 108.28(12) . . ?
C1 N1 Co 107.57(12) . . ?
C8 N1 H1 109.1 . . ?
C1 N1 H1 109.1 . . ?
Co N1 H1 109.1 . . ?
N1 C1 C2 105.91(16) . . ?
N1 C1 H1A 110.6 . . ?
C2 C1 H1A 110.6 . . ?
N1 C1 H1B 110.6 . . ?
C2 C1 H1B 110.6 . . ?
H1A C1 H1B 108.7 . . ?
O6 S2 O8 116.20(9) . . ?
O6 S2 O7 114.57(9) . . ?
O8 S2 O7 112.61(9) . . ?
O6 S2 C10 105.18(10) . . ?
O8 S2 C10 103.13(10) . . ?
O7 S2 C10 103.18(10) . . ?
Co O2 HO2B 114.4(19) . . ?
Co O2 HO2A 119(2) . . ?
HO2B O2 HO2A 107(3) . . ?
C3 N2 C2 110.90(15) . . ?
C3 N2 Co 107.58(12) . . ?
C2 N2 Co 110.22(12) . . ?
C3 N2 H2 109.4 . . ?
C2 N2 H2 109.4 . . ?
Co N2 H2 109.4 . . ?
N2 C2 C1 109.37(16) . . ?
N2 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
N2 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
O11 S3 O10 115.45(9) . . ?
O11 S3 O9 114.80(10) . . ?
O10 S3 O9 113.92(9) . . ?
O11 S3 C11 103.91(10) . . ?
O10 S3 C11 103.62(10) . . ?
O9 S3 C11 102.98(11) . . ?
C4 N3 C5 118.06(15) . . ?
C4 N3 Co 110.87(12) . . ?
C5 N3 Co 110.76(12) . . ?
C4 N3 H3 105.4 . . ?
C5 N3 H3 105.4 . . ?
Co N3 H3 105.4 . . ?
N2 C3 C4 107.55(16) . . ?
N2 C3 H3A 110.2 . . ?
C4 C3 H3A 110.2 . . ?
N2 C3 H3B 110.2 . . ?
C4 C3 H3B 110.2 . . ?
H3A C3 H3B 108.5 . . ?
C6 N4 C7 110.90(15) . . ?
C6 N4 Co 107.23(12) . . ?
C7 N4 Co 110.61(12) . . ?
C6 N4 H4 109.4 . . ?
C7 N4 H4 109.4 . . ?
Co N4 H4 109.4 . . ?
N3 C4 C3 104.54(16) . . ?
N3 C4 H4A 110.8 . . ?
C3 C4 H4A 110.8 . . ?
N3 C4 H4B 110.8 . . ?
C3 C4 H4B 110.8 . . ?
H4A C4 H4B 108.9 . . ?
N3 C5 C6 104.55(15) . . ?
N3 C5 H5A 110.8 . . ?
C6 C5 H5A 110.8 . . ?
N3 C5 H5B 110.8 . . ?
C6 C5 H5B 110.8 . . ?
H5A C5 H5B 108.9 . . ?
N4 C6 C5 106.77(16) . . ?
N4 C6 H6A 110.4 . . ?
C5 C6 H6A 110.4 . . ?
N4 C6 H6B 110.4 . . ?
C5 C6 H6B 110.4 . . ?
H6A C6 H6B 108.6 . . ?
C8 C7 N4 108.95(16) . . ?
C8 C7 H7A 109.9 . . ?
N4 C7 H7A 109.9 . . ?
C8 C7 H7B 109.9 . . ?
N4 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
N1 C8 C7 106.87(16) . . ?
N1 C8 H8A 110.3 . . ?
C7 C8 H8A 110.3 . . ?
N1 C8 H8B 110.3 . . ?
C7 C8 H8B 110.3 . . ?
H8A C8 H8B 108.6 . . ?
F1 C9 F3 108.23(19) . . ?
F1 C9 F2 108.36(18) . . ?
F3 C9 F2 107.91(18) . . ?
F1 C9 S1 111.31(15) . . ?
F3 C9 S1 110.45(15) . . ?
F2 C9 S1 110.49(15) . . ?
F5 C10 F4 108.83(19) . . ?
F5 C10 F6 108.72(19) . . ?
F4 C10 F6 108.11(19) . . ?
F5 C10 S2 110.83(16) . . ?
F4 C10 S2 110.45(15) . . ?
F6 C10 S2 109.84(16) . . ?
F7 C11 F9 108.0(2) . . ?
F7 C11 F8 108.36(19) . . ?
F9 C11 F8 108.01(18) . . ?
F7 C11 S3 111.27(15) . . ?
F9 C11 S3 111.22(16) . . ?
F8 C11 S3 109.88(17) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O3 0.91 2.08 2.898(2) 149.6 4_666
N2 H2 O10 0.91 1.99 2.826(2) 151.5 2
N3 H3 O5 0.91 2.17 3.021(2) 156.0 .
N4 H4 O7 0.91 2.12 2.968(2) 154.1 .
O2 HO2B O9 0.8200(10) 1.843(7) 2.645(2) 165(3) 2
O2 HO2A O8 0.8200(10) 1.864(7) 2.669(2) 167(3) .
O1 HO1A O7 0.8200(10) 1.966(9) 2.758(2) 162(3) .
O1 HO1B O4 0.8200(10) 1.824(6) 2.634(2) 169(3) 4_566
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full 26.41
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max 0.445
_refine_diff_density_min -0.370
_refine_diff_density_rms 0.056
#===END
data_jyc0352
_database_code_depnum_ccdc_archive 'CCDC 791381'
#TrackingRef '- Structures combined.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C25 H42 Co N5 O P2, 6(H2 O)'
_chemical_formula_sum 'C25 H54 Co N5 O13 P2'
_chemical_formula_weight 753.60
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'
P P 0.1023 0.0942 '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'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M P21/n
_symmetry_space_group_name_Hall -p_2yac
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 12.9933(4)
_cell_length_b 13.0099(4)
_cell_length_c 19.4916(2)
_cell_angle_alpha 90.00
_cell_angle_beta 96.783(2)
_cell_angle_gamma 90.00
_cell_volume 3271.83(15)
_cell_formula_units_Z 4
_cell_measurement_temperature 83(2)
_cell_measurement_reflns_used 3547
_cell_measurement_theta_min 2.0
_cell_measurement_theta_max 25.75
_exptl_crystal_description plate
_exptl_crystal_colour brown
_exptl_crystal_size_max 0.12
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.05
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.501
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1544
_exptl_absorpt_coefficient_mu 0.692
_exptl_absorpt_correction_T_min 0.9215
_exptl_absorpt_correction_T_max 0.9662
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 83(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 'Siemens SMART CCD'
_diffrn_measurement_method 'Area detector \w scans'
_diffrn_standards_decay_% <2%
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS; Sheldrick, 1997'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_reflns_number 20547
_diffrn_reflns_av_R_equivalents 0.1366
_diffrn_reflns_av_sigmaI/netI 0.1666
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_theta_min 2.00
_diffrn_reflns_theta_max 25.75
_reflns_number_total 6122
_reflns_number_gt 3528
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'SADABS (Sheldrick, 1997)'
_computing_cell_refinement 'SMART (Siemens, 1995)'
_computing_data_reduction 'SAINT (Siemens, 1995)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics 'Ortep-III (Burnett & Johnson, 1996)'
_computing_publication_material 'SHELXTL (Siemens, 1995)'
_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^)+(0.0000P)^2^+57.7258P] 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 6122
_refine_ls_number_parameters 415
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.2342
_refine_ls_R_factor_gt 0.1436
_refine_ls_wR_factor_ref 0.2861
_refine_ls_wR_factor_gt 0.2458
_refine_ls_goodness_of_fit_ref 1.244
_refine_ls_restrained_S_all 1.244
_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 0.03139(12) 0.02160(13) 0.82340(8) 0.0225(4) Uani 1 1 d . . .
P1 P 0.0685(2) -0.4871(2) 0.62233(16) 0.0252(7) Uani 1 1 d . . .
P2 P -0.3951(3) 0.3747(4) 1.00393(18) 0.0439(11) Uani 1 1 d . . .
O1 O -0.0462(6) -0.0644(6) 0.8768(4) 0.0243(19) Uani 1 1 d . . .
O2 O 0.0367(7) -0.5585(6) 0.5562(5) 0.042(2) Uani 1 1 d . . .
O3 O 0.0855(6) -0.5543(6) 0.6853(4) 0.028(2) Uani 1 1 d . . .
O4 O 0.1598(6) -0.4215(6) 0.6100(4) 0.028(2) Uani 1 1 d . . .
O5 O -0.3973(7) 0.4583(8) 1.0585(4) 0.046(3) Uani 1 1 d . . .
O6 O -0.4505(7) 0.4166(9) 0.9324(4) 0.060(3) Uani 1 1 d . . .
O7 O -0.4427(7) 0.2733(9) 1.0212(5) 0.056(3) Uani 1 1 d . . .
O8 O 0.0849(7) -0.5064(7) 0.8245(4) 0.044(2) Uani 1 1 d . . .
O9 O 0.1566(7) -0.2613(7) 0.5184(4) 0.038(2) Uani 1 1 d . . .
O10 O -0.2385(7) 0.5946(7) 1.0743(4) 0.039(2) Uani 1 1 d . . .
O11 O -0.4485(7) 0.2580(6) 1.1592(5) 0.038(2) Uani 1 1 d . . .
O12 O 0.0168(11) -0.3316(9) 0.8872(6) 0.084(4) Uani 1 1 d . . .
O13 O -0.0776(10) 0.5766(12) 0.9895(7) 0.102(5) Uani 1 1 d . . .
N1 N 0.0890(7) -0.0983(7) 0.7706(4) 0.021(2) Uani 1 1 d . . .
N2 N 0.0104(7) 0.1494(7) 0.8802(5) 0.024(2) Uani 1 1 d . . .
N3 N 0.1469(7) -0.0059(6) 0.8925(4) 0.020(2) Uani 1 1 d . . .
H3N H 0.2036 0.0282 0.8811 0.024 Uiso 1 1 calc R . .
N4 N 0.1077(7) 0.1086(6) 0.7691(4) 0.016(2) Uani 1 1 d . . .
H4N H 0.0615 0.1310 0.7336 0.019 Uiso 1 1 calc R . .
N5 N -0.0991(7) 0.0337(7) 0.7608(5) 0.025(2) Uani 1 1 d . . .
C1 C -0.1447(10) -0.0791(9) 0.8489(6) 0.024(3) Uani 1 1 d . . .
C2 C -0.2146(10) -0.1439(10) 0.8759(7) 0.035(3) Uani 1 1 d . . .
H2 H -0.1951 -0.1807 0.9162 0.042 Uiso 1 1 calc R . .
C3 C -0.3148(10) -0.1531(10) 0.8413(7) 0.034(3) Uani 1 1 d . . .
H3 H -0.3627 -0.1941 0.8604 0.041 Uiso 1 1 calc R . .
C4 C -0.3442(11) -0.1035(10) 0.7803(7) 0.038(3) Uani 1 1 d . . .
H4 H -0.4114 -0.1120 0.7588 0.045 Uiso 1 1 calc R . .
C5 C -0.2746(9) -0.0390(9) 0.7489(7) 0.032(3) Uani 1 1 d . . .
C6 C -0.1743(9) -0.0306(9) 0.7852(6) 0.025(3) Uani 1 1 d . . .
C7 C -0.1236(10) 0.0800(9) 0.7008(6) 0.028(3) Uani 1 1 d . . .
H7 H -0.0736 0.1201 0.6832 0.034 Uiso 1 1 calc R . .
C8 C -0.2219(10) 0.0713(10) 0.6621(6) 0.033(3) Uani 1 1 d . . .
H8 H -0.2363 0.1060 0.6204 0.040 Uiso 1 1 calc R . .
C9 C -0.2957(10) 0.0116(9) 0.6864(6) 0.034(3) Uani 1 1 d . . .
H9 H -0.3605 0.0048 0.6609 0.041 Uiso 1 1 calc R . .
C11 C 0.1332(9) -0.0484(8) 0.7114(6) 0.024(3) Uani 1 1 d . . .
H11A H 0.0783 -0.0334 0.6746 0.029 Uiso 1 1 calc R . .
H11B H 0.1824 -0.0943 0.6934 0.029 Uiso 1 1 calc R . .
C12 C 0.1756(9) -0.1475(9) 0.8181(6) 0.025(3) Uani 1 1 d . . .
H12A H 0.1716 -0.2217 0.8135 0.030 Uiso 1 1 calc R . .
H12B H 0.2419 -0.1253 0.8053 0.030 Uiso 1 1 calc R . .
C13 C 0.1673(9) -0.1177(9) 0.8919(5) 0.021(3) Uani 1 1 d . . .
H13A H 0.1112 -0.1551 0.9093 0.026 Uiso 1 1 calc R . .
H13B H 0.2313 -0.1335 0.9208 0.026 Uiso 1 1 calc R . .
C14 C 0.1212(9) 0.0325(10) 0.9594(6) 0.028(3) Uani 1 1 d . . .
H14A H 0.1826 0.0324 0.9929 0.034 Uiso 1 1 calc R . .
H14B H 0.0696 -0.0115 0.9765 0.034 Uiso 1 1 calc R . .
C15 C 0.0799(9) 0.1395(9) 0.9496(5) 0.023(3) Uani 1 1 d . . .
H15A H 0.1372 0.1875 0.9507 0.027 Uiso 1 1 calc R . .
H15B H 0.0402 0.1568 0.9871 0.027 Uiso 1 1 calc R . .
C16 C 0.0462(10) 0.2380(9) 0.8405(6) 0.031(3) Uani 1 1 d . . .
H16A H 0.0621 0.2965 0.8707 0.038 Uiso 1 1 calc R . .
H16B H -0.0074 0.2580 0.8040 0.038 Uiso 1 1 calc R . .
C17 C 0.1427(9) 0.2028(8) 0.8099(6) 0.023(3) Uani 1 1 d . . .
H17A H 0.1665 0.2554 0.7802 0.028 Uiso 1 1 calc R . .
H17B H 0.1981 0.1865 0.8460 0.028 Uiso 1 1 calc R . .
C18 C 0.1874(9) 0.0512(8) 0.7370(6) 0.022(3) Uani 1 1 d . . .
H18A H 0.2470 0.0369 0.7705 0.026 Uiso 1 1 calc R . .
H18B H 0.2101 0.0896 0.6989 0.026 Uiso 1 1 calc R . .
C19 C -0.1014(9) 0.1663(10) 0.8914(7) 0.033(3) Uani 1 1 d . . .
H19A H -0.1251 0.1067 0.9150 0.039 Uiso 1 1 calc R . .
H19B H -0.1427 0.1706 0.8467 0.039 Uiso 1 1 calc R . .
C20 C -0.1224(9) 0.2638(9) 0.9336(6) 0.029(3) Uani 1 1 d . . .
H20A H -0.0842 0.2595 0.9794 0.034 Uiso 1 1 calc R . .
H20B H -0.0990 0.3244 0.9109 0.034 Uiso 1 1 calc R . .
C21 C -0.2396(9) 0.2730(10) 0.9396(6) 0.033(3) Uani 1 1 d . . .
H21A H -0.2762 0.2890 0.8946 0.040 Uiso 1 1 calc R . .
H21B H -0.2652 0.2076 0.9545 0.040 Uiso 1 1 calc R . .
C22 C -0.2613(9) 0.3558(10) 0.9906(6) 0.031(3) Uani 1 1 d . . .
H22A H -0.2348 0.4204 0.9751 0.037 Uiso 1 1 calc R . .
H22B H -0.2224 0.3397 1.0349 0.037 Uiso 1 1 calc R . .
C23 C 0.0067(9) -0.1754(8) 0.7462(6) 0.023(3) Uani 1 1 d . . .
H23A H -0.0524 -0.1391 0.7226 0.027 Uiso 1 1 calc R . .
H23B H -0.0160 -0.2091 0.7862 0.027 Uiso 1 1 calc R . .
C24 C 0.0413(9) -0.2584(9) 0.6972(6) 0.024(3) Uani 1 1 d . . .
H24A H 0.0513 -0.2282 0.6530 0.029 Uiso 1 1 calc R . .
H24B H 0.1063 -0.2890 0.7169 0.029 Uiso 1 1 calc R . .
C25 C -0.0434(9) -0.3398(8) 0.6878(5) 0.020(3) Uani 1 1 d . . .
H25A H -0.1100 -0.3057 0.6866 0.024 Uiso 1 1 calc R . .
H25B H -0.0358 -0.3845 0.7279 0.024 Uiso 1 1 calc R . .
C26 C -0.0446(9) -0.4062(9) 0.6230(6) 0.023(3) Uani 1 1 d . . .
H26A H -0.0499 -0.3617 0.5829 0.028 Uiso 1 1 calc R . .
H26B H -0.1058 -0.4495 0.6191 0.028 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
Co1 0.0186(9) 0.0279(8) 0.0217(8) -0.0017(8) 0.0052(6) -0.0002(8)
P1 0.0217(18) 0.0169(15) 0.0363(17) 0.0016(14) 0.0013(14) 0.0025(14)
P2 0.021(2) 0.084(3) 0.0270(18) -0.026(2) 0.0051(15) 0.002(2)
O1 0.018(5) 0.025(4) 0.031(4) 0.001(4) 0.010(4) -0.003(4)
O2 0.041(6) 0.026(5) 0.055(6) -0.020(4) -0.003(5) -0.007(4)
O3 0.027(5) 0.022(4) 0.034(5) 0.001(4) -0.002(4) 0.003(4)
O4 0.018(5) 0.025(4) 0.040(5) 0.005(4) 0.005(4) 0.007(4)
O5 0.024(5) 0.085(8) 0.029(5) -0.028(5) 0.000(4) 0.007(5)
O6 0.030(6) 0.119(10) 0.030(5) -0.028(6) -0.004(4) 0.026(6)
O7 0.033(6) 0.096(9) 0.043(6) -0.033(6) 0.017(5) -0.033(6)
O8 0.039(6) 0.055(6) 0.039(5) 0.014(5) 0.009(4) 0.001(5)
O9 0.028(6) 0.041(5) 0.045(5) 0.004(5) 0.008(4) -0.004(4)
O10 0.040(6) 0.053(6) 0.025(5) -0.004(4) 0.012(4) 0.001(5)
O11 0.047(6) 0.022(4) 0.044(5) -0.002(4) -0.001(5) -0.008(4)
O12 0.131(12) 0.059(8) 0.054(7) 0.004(6) -0.015(7) -0.010(8)
O13 0.074(10) 0.152(14) 0.088(10) -0.038(10) 0.041(8) -0.047(9)
N1 0.026(6) 0.016(5) 0.021(5) 0.002(4) 0.003(4) -0.001(4)
N2 0.015(6) 0.027(5) 0.029(5) -0.005(4) 0.000(4) 0.001(5)
N3 0.021(5) 0.017(5) 0.024(5) 0.003(4) 0.005(4) -0.005(4)
N4 0.009(5) 0.016(5) 0.021(5) 0.001(4) -0.003(4) -0.002(4)
N5 0.029(6) 0.017(5) 0.030(5) 0.004(4) 0.006(5) 0.005(5)
C1 0.024(7) 0.024(6) 0.022(6) -0.011(5) -0.003(5) -0.003(6)
C2 0.029(8) 0.033(7) 0.043(8) -0.017(6) -0.002(6) -0.002(6)
C3 0.018(7) 0.029(7) 0.058(9) -0.012(7) 0.014(6) -0.006(6)
C4 0.027(8) 0.036(8) 0.047(8) 0.002(7) -0.008(7) 0.003(6)
C5 0.015(7) 0.031(7) 0.050(8) -0.016(6) 0.010(6) 0.006(6)
C6 0.020(7) 0.024(6) 0.031(6) -0.019(6) 0.006(5) -0.008(6)
C7 0.029(8) 0.019(6) 0.036(7) -0.007(6) 0.005(6) -0.004(6)
C8 0.035(9) 0.035(7) 0.026(7) 0.004(6) -0.017(6) -0.001(7)
C9 0.034(8) 0.023(6) 0.039(7) -0.006(6) -0.018(6) 0.003(6)
C11 0.032(8) 0.021(6) 0.022(6) 0.007(5) 0.014(5) 0.008(5)
C12 0.025(7) 0.019(6) 0.031(7) 0.008(5) 0.010(5) 0.004(5)
C13 0.015(7) 0.032(7) 0.016(5) 0.007(5) -0.001(5) 0.004(5)
C14 0.017(7) 0.046(8) 0.022(6) -0.005(6) 0.004(5) -0.001(6)
C15 0.022(7) 0.029(6) 0.018(6) 0.001(5) 0.004(5) -0.003(5)
C16 0.034(8) 0.027(7) 0.033(7) -0.006(6) 0.003(6) -0.012(6)
C17 0.021(7) 0.023(6) 0.025(6) -0.001(5) 0.007(5) 0.006(5)
C18 0.026(7) 0.020(6) 0.023(6) 0.005(5) 0.012(5) -0.002(5)
C19 0.016(7) 0.047(8) 0.038(7) -0.009(6) 0.012(6) -0.007(6)
C20 0.023(8) 0.034(7) 0.030(7) -0.017(6) 0.006(5) -0.001(6)
C21 0.021(8) 0.045(8) 0.033(7) -0.010(6) -0.001(6) -0.001(6)
C22 0.022(7) 0.041(8) 0.031(7) -0.009(6) 0.005(6) 0.003(6)
C23 0.019(7) 0.018(6) 0.033(7) 0.003(5) 0.011(5) 0.008(5)
C24 0.018(7) 0.027(6) 0.029(6) -0.001(5) 0.010(5) 0.001(5)
C25 0.018(7) 0.023(6) 0.021(6) 0.006(5) 0.006(5) 0.005(5)
C26 0.013(7) 0.021(6) 0.035(7) -0.001(5) -0.001(5) -0.007(5)
_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 1.896(8) . ?
Co1 N4 1.906(9) . ?
Co1 N3 1.927(9) . ?
Co1 N5 1.974(10) . ?
Co1 N2 2.034(9) . ?
Co1 N1 2.058(9) . ?
P1 O3 1.502(8) . ?
P1 O4 1.503(8) . ?
P1 O2 1.604(9) . ?
P1 C26 1.808(11) . ?
P2 O7 1.511(11) . ?
P2 O5 1.524(9) . ?
P2 O6 1.588(10) . ?
P2 C22 1.805(12) . ?
O1 C1 1.344(13) . ?
N1 C11 1.497(13) . ?
N1 C23 1.502(14) . ?
N1 C12 1.512(14) . ?
N2 C16 1.492(15) . ?
N2 C19 1.511(14) . ?
N2 C15 1.541(14) . ?
N3 C14 1.471(13) . ?
N3 C13 1.479(14) . ?
N3 H3N 0.9100 . ?
N4 C18 1.474(13) . ?
N4 C17 1.502(13) . ?
N4 H4N 0.9100 . ?
N5 C7 1.321(14) . ?
N5 C6 1.411(14) . ?
C1 C2 1.387(17) . ?
C1 C6 1.405(16) . ?
C2 C3 1.398(17) . ?
C2 H2 0.9300 . ?
C3 C4 1.368(18) . ?
C3 H3 0.9300 . ?
C4 C5 1.424(18) . ?
C4 H4 0.9300 . ?
C5 C9 1.382(17) . ?
C5 C6 1.412(16) . ?
C7 C8 1.410(16) . ?
C7 H7 0.9300 . ?
C8 C9 1.362(17) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C11 C18 1.530(15) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.505(15) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.495(16) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.521(16) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.553(16) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.545(16) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.515(16) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.543(15) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C25 1.523(15) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C26 1.529(15) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 H26A 0.9700 . ?
C26 H26B 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 N4 179.3(4) . . ?
O1 Co1 N3 85.9(4) . . ?
N4 Co1 N3 94.9(4) . . ?
O1 Co1 N5 85.0(4) . . ?
N4 Co1 N5 94.3(4) . . ?
N3 Co1 N5 170.8(4) . . ?
O1 Co1 N2 94.0(4) . . ?
N4 Co1 N2 85.9(4) . . ?
N3 Co1 N2 85.1(4) . . ?
N5 Co1 N2 96.3(4) . . ?
O1 Co1 N1 94.3(4) . . ?
N4 Co1 N1 85.9(4) . . ?
N3 Co1 N1 84.8(4) . . ?
N5 Co1 N1 95.1(4) . . ?
N2 Co1 N1 166.4(4) . . ?
O3 P1 O4 114.8(5) . . ?
O3 P1 O2 108.6(5) . . ?
O4 P1 O2 109.5(5) . . ?
O3 P1 C26 111.9(5) . . ?
O4 P1 C26 109.2(5) . . ?
O2 P1 C26 102.2(5) . . ?
O7 P2 O5 115.2(6) . . ?
O7 P2 O6 109.9(6) . . ?
O5 P2 O6 108.9(6) . . ?
O7 P2 C22 109.9(6) . . ?
O5 P2 C22 107.1(5) . . ?
O6 P2 C22 105.3(6) . . ?
C1 O1 Co1 113.9(7) . . ?
C11 N1 C23 111.7(9) . . ?
C11 N1 C12 109.3(9) . . ?
C23 N1 C12 111.2(8) . . ?
C11 N1 Co1 104.6(6) . . ?
C23 N1 Co1 112.2(7) . . ?
C12 N1 Co1 107.6(6) . . ?
C16 N2 C19 109.0(9) . . ?
C16 N2 C15 109.5(9) . . ?
C19 N2 C15 111.0(9) . . ?
C16 N2 Co1 106.2(7) . . ?
C19 N2 Co1 113.0(7) . . ?
C15 N2 Co1 107.9(7) . . ?
C14 N3 C13 113.6(9) . . ?
C14 N3 Co1 108.5(7) . . ?
C13 N3 Co1 107.6(7) . . ?
C14 N3 H3N 109.0 . . ?
C13 N3 H3N 109.0 . . ?
Co1 N3 H3N 109.0 . . ?
C18 N4 C17 117.0(8) . . ?
C18 N4 Co1 111.9(6) . . ?
C17 N4 Co1 109.6(6) . . ?
C18 N4 H4N 105.8 . . ?
C17 N4 H4N 105.8 . . ?
Co1 N4 H4N 105.8 . . ?
C7 N5 C6 117.7(10) . . ?
C7 N5 Co1 133.1(8) . . ?
C6 N5 Co1 108.8(7) . . ?
O1 C1 C2 124.7(11) . . ?
O1 C1 C6 116.1(10) . . ?
C2 C1 C6 119.0(11) . . ?
C1 C2 C3 118.9(13) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C4 C3 C2 121.8(13) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C3 C4 C5 121.7(12) . . ?
C3 C4 H4 119.2 . . ?
C5 C4 H4 119.2 . . ?
C9 C5 C6 118.7(12) . . ?
C9 C5 C4 126.1(12) . . ?
C6 C5 C4 115.2(12) . . ?
C1 C6 N5 115.9(10) . . ?
C1 C6 C5 123.2(11) . . ?
N5 C6 C5 120.8(11) . . ?
N5 C7 C8 123.1(12) . . ?
N5 C7 H7 118.5 . . ?
C8 C7 H7 118.5 . . ?
C9 C8 C7 119.4(11) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C8 C9 C5 120.2(11) . . ?
C8 C9 H9 119.9 . . ?
C5 C9 H9 119.9 . . ?
N1 C11 C18 108.7(9) . . ?
N1 C11 H11A 110.0 . . ?
C18 C11 H11A 110.0 . . ?
N1 C11 H11B 110.0 . . ?
C18 C11 H11B 110.0 . . ?
H11A C11 H11B 108.3 . . ?
C13 C12 N1 110.1(9) . . ?
C13 C12 H12A 109.6 . . ?
N1 C12 H12A 109.6 . . ?
C13 C12 H12B 109.6 . . ?
N1 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
N3 C13 C12 107.1(9) . . ?
N3 C13 H13A 110.3 . . ?
C12 C13 H13A 110.3 . . ?
N3 C13 H13B 110.3 . . ?
C12 C13 H13B 110.3 . . ?
H13A C13 H13B 108.5 . . ?
N3 C14 C15 108.5(9) . . ?
N3 C14 H14A 110.0 . . ?
C15 C14 H14A 110.0 . . ?
N3 C14 H14B 110.0 . . ?
C15 C14 H14B 110.0 . . ?
H14A C14 H14B 108.4 . . ?
C14 C15 N2 110.8(9) . . ?
C14 C15 H15A 109.5 . . ?
N2 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
N2 C15 H15B 109.5 . . ?
H15A C15 H15B 108.1 . . ?
N2 C16 C17 107.0(10) . . ?
N2 C16 H16A 110.3 . . ?
C17 C16 H16A 110.3 . . ?
N2 C16 H16B 110.3 . . ?
C17 C16 H16B 110.3 . . ?
H16A C16 H16B 108.6 . . ?
N4 C17 C16 104.0(9) . . ?
N4 C17 H17A 111.0 . . ?
C16 C17 H17A 111.0 . . ?
N4 C17 H17B 111.0 . . ?
C16 C17 H17B 111.0 . . ?
H17A C17 H17B 109.0 . . ?
N4 C18 C11 104.4(9) . . ?
N4 C18 H18A 110.9 . . ?
C11 C18 H18A 110.9 . . ?
N4 C18 H18B 110.9 . . ?
C11 C18 H18B 110.9 . . ?
H18A C18 H18B 108.9 . . ?
N2 C19 C20 115.3(10) . . ?
N2 C19 H19A 108.4 . . ?
C20 C19 H19A 108.4 . . ?
N2 C19 H19B 108.4 . . ?
C20 C19 H19B 108.4 . . ?
H19A C19 H19B 107.5 . . ?
C21 C20 C19 109.8(10) . . ?
C21 C20 H20A 109.7 . . ?
C19 C20 H20A 109.7 . . ?
C21 C20 H20B 109.7 . . ?
C19 C20 H20B 109.7 . . ?
H20A C20 H20B 108.2 . . ?
C22 C21 C20 111.5(10) . . ?
C22 C21 H21A 109.3 . . ?
C20 C21 H21A 109.3 . . ?
C22 C21 H21B 109.3 . . ?
C20 C21 H21B 109.3 . . ?
H21A C21 H21B 108.0 . . ?
C21 C22 P2 116.6(9) . . ?
C21 C22 H22A 108.1 . . ?
P2 C22 H22A 108.1 . . ?
C21 C22 H22B 108.1 . . ?
P2 C22 H22B 108.1 . . ?
H22A C22 H22B 107.3 . . ?
N1 C23 C24 114.5(9) . . ?
N1 C23 H23A 108.6 . . ?
C24 C23 H23A 108.6 . . ?
N1 C23 H23B 108.6 . . ?
C24 C23 H23B 108.6 . . ?
H23A C23 H23B 107.6 . . ?
C25 C24 C23 107.5(9) . . ?
C25 C24 H24A 110.2 . . ?
C23 C24 H24A 110.2 . . ?
C25 C24 H24B 110.2 . . ?
C23 C24 H24B 110.2 . . ?
H24A C24 H24B 108.5 . . ?
C24 C25 C26 115.4(9) . . ?
C24 C25 H25A 108.4 . . ?
C26 C25 H25A 108.4 . . ?
C24 C25 H25B 108.4 . . ?
C26 C25 H25B 108.4 . . ?
H25A C25 H25B 107.5 . . ?
C25 C26 P1 114.0(8) . . ?
C25 C26 H26A 108.8 . . ?
P1 C26 H26A 108.8 . . ?
C25 C26 H26B 108.8 . . ?
P1 C26 H26B 108.8 . . ?
H26A C26 H26B 107.6 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3N O4 0.91 1.88 2.748(12) 158.5 2_556
N4 H4N O11 0.91 2.04 2.787(12) 138.5 4_665
_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full 25.75
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max 0.871
_refine_diff_density_min -0.584
_refine_diff_density_rms 0.150
#===END
data_jyc405a
_database_code_depnum_ccdc_archive 'CCDC 791382'
#TrackingRef '- Structures combined.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C18 H36 Cl2 Co N4 O4, H2 O, Cl'
_chemical_formula_sum 'C18 H38 Cl3 Co N4 O5'
_chemical_formula_weight 555.80
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'
Cl Cl 0.1484 0.1585 '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'
_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 6.6328(1)
_cell_length_b 11.8056(2)
_cell_length_c 15.7524(2)
_cell_angle_alpha 97.266(1)
_cell_angle_beta 92.720(1)
_cell_angle_gamma 97.839(1)
_cell_volume 1209.51(3)
_cell_formula_units_Z 2
_cell_measurement_temperature 84(2)
_cell_measurement_reflns_used 8192
_cell_measurement_theta_min 2.04
_cell_measurement_theta_max 27.11
_exptl_crystal_description block
_exptl_crystal_colour blue
_exptl_crystal_size_max 0.42
_exptl_crystal_size_mid 0.38
_exptl_crystal_size_min 0.32
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.526
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 584
_exptl_absorpt_coefficient_mu 1.077
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS; Sheldrick, 1996'
_exptl_absorpt_correction_T_min 0.6604
_exptl_absorpt_correction_T_max 0.7243
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 84(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 'Siemens SMART CCD'
_diffrn_measurement_method 'Area detector \w scans'
_diffrn_standards_decay_% <2%
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_reflns_number 12294
_diffrn_reflns_av_R_equivalents 0.0245
_diffrn_reflns_av_sigmaI/netI 0.0283
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_theta_min 2.04
_diffrn_reflns_theta_max 27.11
_reflns_number_total 5253
_reflns_number_gt 4818
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'SMART (Siemens, 1995)'
_computing_cell_refinement 'SAINT (Siemens, 1995)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics 'Ortep-III (Burnett & Johnson, 1996)'
_computing_publication_material 'SHELXTL (Sheldrick, 2008)'
_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^)+(0.0254P)^2^+4.4693P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens mixed
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 5253
_refine_ls_number_parameters 292
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0481
_refine_ls_R_factor_gt 0.0441
_refine_ls_wR_factor_ref 0.1128
_refine_ls_wR_factor_gt 0.1110
_refine_ls_goodness_of_fit_ref 1.089
_refine_ls_restrained_S_all 1.089
_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
Co Co 0.17640(6) -0.00620(3) 0.21907(2) 0.01433(11) Uani 1 1 d . . .
Cl1 Cl 0.48328(11) -0.05509(6) 0.26058(5) 0.01885(16) Uani 1 1 d . . .
N1 N 0.0753(4) -0.0857(2) 0.31263(16) 0.0177(5) Uani 1 1 d . . .
H1N H 0.1874 -0.1087 0.3369 0.021 Uiso 1 1 calc R . .
O1 O 1.0126(4) 0.5384(2) 0.36152(16) 0.0311(6) Uani 1 1 d . . .
C1 C 0.0071(5) -0.0046(3) 0.3807(2) 0.0228(7) Uani 1 1 d . . .
H1A H -0.0043 -0.0384 0.4336 0.027 Uiso 1 1 calc R . .
H1B H -0.1241 0.0160 0.3637 0.027 Uiso 1 1 calc R . .
Cl2 Cl 0.32607(12) 0.08179(6) 0.11320(5) 0.02003(16) Uani 1 1 d . . .
O2 O 0.9535(4) 0.6494(2) 0.48118(16) 0.0274(5) Uani 1 1 d . . .
HO2 H 1.0604 0.6878 0.4713 0.033 Uiso 1 1 calc R . .
N2 N 0.1968(4) 0.1409(2) 0.30514(17) 0.0181(5) Uani 1 1 d . . .
C2 C 0.1707(5) 0.1000(3) 0.3917(2) 0.0232(7) Uani 1 1 d . . .
H2A H 0.1311 0.1608 0.4320 0.028 Uiso 1 1 calc R . .
H2B H 0.2983 0.0799 0.4137 0.028 Uiso 1 1 calc R . .
N3 N -0.0856(4) 0.0342(2) 0.18510(18) 0.0214(6) Uani 1 1 d . . .
HN3 H -0.1760 0.0060 0.2216 0.026 Uiso 1 1 calc R . .
O3 O 0.4117(4) -0.5954(2) -0.18490(18) 0.0381(7) Uani 1 1 d . . .
HO3 H 0.4954 -0.6064 -0.2206 0.046 Uiso 1 1 calc R . .
C3 C 0.0187(5) 0.2028(3) 0.2862(2) 0.0257(7) Uani 1 1 d . . .
H3A H -0.0820 0.1903 0.3281 0.031 Uiso 1 1 calc R . .
H3B H 0.0650 0.2851 0.2909 0.031 Uiso 1 1 calc R . .
Cl3 Cl 1.31176(13) 0.82377(7) 0.47208(5) 0.02723(19) Uani 1 1 d . . .
N4 N 0.0798(4) -0.1594(2) 0.14202(16) 0.0165(5) Uani 1 1 d . . .
C4 C -0.0773(5) 0.1597(3) 0.1975(2) 0.0220(6) Uani 1 1 d . . .
H4A H -0.2136 0.1802 0.1920 0.026(10) Uiso 1 1 calc R . .
H4B H 0.0035 0.1935 0.1549 0.031(11) Uiso 1 1 calc R . .
O4 O 0.6258(5) -0.4328(3) -0.1435(2) 0.0532(9) Uani 1 1 d . . .
C5 C -0.1541(5) -0.0250(3) 0.0989(2) 0.0231(7) Uani 1 1 d . . .
H5A H -0.0774 0.0115 0.0563 0.039(12) Uiso 1 1 calc R . .
H5B H -0.2976 -0.0207 0.0872 0.009(8) Uiso 1 1 calc R . .
O5 O 0.6112(4) -0.6404(2) -0.32014(17) 0.0299(6) Uani 1 1 d . . .
C6 C -0.1208(5) -0.1487(3) 0.0951(2) 0.0233(7) Uani 1 1 d . . .
H6A H -0.1206 -0.1822 0.0356 0.028 Uiso 1 1 calc R . .
H6B H -0.2321 -0.1914 0.1206 0.028 Uiso 1 1 calc R . .
C7 C -0.0588(5) -0.1934(3) 0.2800(2) 0.0193(6) Uani 1 1 d . . .
H7A H -0.1940 -0.1777 0.2635 0.023 Uiso 1 1 calc R . .
H7B H -0.0704 -0.2448 0.3235 0.023 Uiso 1 1 calc R . .
C8 C 0.0393(5) -0.2466(3) 0.20316(19) 0.0181(6) Uani 1 1 d . . .
H8A H 0.1663 -0.2710 0.2215 0.022 Uiso 1 1 calc R . .
H8B H -0.0504 -0.3139 0.1747 0.022 Uiso 1 1 calc R . .
C9 C 0.3955(5) 0.2186(3) 0.3056(2) 0.0197(6) Uani 1 1 d . . .
H9A H 0.4048 0.2447 0.2497 0.024 Uiso 1 1 calc R . .
H9B H 0.5050 0.1732 0.3127 0.024 Uiso 1 1 calc R . .
C10 C 0.4323(5) 0.3244(3) 0.3737(2) 0.0210(6) Uani 1 1 d . . .
H10A H 0.3290 0.3738 0.3664 0.025 Uiso 1 1 calc R . .
H10B H 0.4257 0.3010 0.4305 0.025 Uiso 1 1 calc R . .
C11 C 0.6424(5) 0.3887(3) 0.3635(2) 0.0234(7) Uani 1 1 d . . .
H11A H 0.7429 0.3370 0.3686 0.028 Uiso 1 1 calc R . .
H11B H 0.6459 0.4117 0.3066 0.028 Uiso 1 1 calc R . .
C12 C 0.6998(5) 0.4951(3) 0.4296(2) 0.0196(6) Uani 1 1 d . . .
H12A H 0.5972 0.5457 0.4253 0.024 Uiso 1 1 calc R . .
H12B H 0.6986 0.4717 0.4864 0.024 Uiso 1 1 calc R . .
C13 C 0.9052(5) 0.5615(3) 0.4195(2) 0.0203(6) Uani 1 1 d . . .
C14 C 0.2318(5) -0.1962(3) 0.0804(2) 0.0214(6) Uani 1 1 d . . .
H14A H 0.3624 -0.1911 0.1121 0.026 Uiso 1 1 calc R . .
H14B H 0.2481 -0.1416 0.0392 0.026 Uiso 1 1 calc R . .
C15 C 0.1801(5) -0.3175(3) 0.0309(2) 0.0259(7) Uani 1 1 d . . .
H15A H 0.0524 -0.3237 -0.0032 0.031 Uiso 1 1 calc R . .
H15B H 0.1643 -0.3738 0.0708 0.031 Uiso 1 1 calc R . .
C16 C 0.3509(6) -0.3423(3) -0.0278(2) 0.0279(7) Uani 1 1 d . . .
H16A H 0.3694 -0.2841 -0.0662 0.033 Uiso 1 1 calc R . .
H16B H 0.4775 -0.3378 0.0066 0.033 Uiso 1 1 calc R . .
C17 C 0.3015(6) -0.4613(3) -0.0803(3) 0.0363(9) Uani 1 1 d . . .
H17A H 0.2797 -0.5186 -0.0414 0.044 Uiso 1 1 calc R . .
H17B H 0.1751 -0.4647 -0.1148 0.044 Uiso 1 1 calc R . .
C18 C 0.4656(6) -0.4924(3) -0.1390(2) 0.0325(8) Uani 1 1 d . . .
H2O5 H 0.600(6) -0.699(4) -0.359(3) 0.022(10) Uiso 1 1 d . . .
H1O5 H 0.719(8) -0.604(4) -0.329(3) 0.043(14) Uiso 1 1 d . . .
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
Co 0.0130(2) 0.0149(2) 0.0142(2) -0.00137(14) 0.00027(14) 0.00229(14)
Cl1 0.0140(3) 0.0206(3) 0.0215(4) -0.0003(3) 0.0005(3) 0.0037(3)
N1 0.0165(13) 0.0195(13) 0.0160(12) -0.0016(10) 0.0012(10) 0.0029(10)
O1 0.0300(14) 0.0322(13) 0.0280(13) -0.0036(10) 0.0105(11) -0.0021(11)
C1 0.0247(17) 0.0242(16) 0.0182(15) -0.0032(12) 0.0057(12) 0.0031(13)
Cl2 0.0235(4) 0.0190(3) 0.0163(3) 0.0011(3) 0.0016(3) -0.0001(3)
O2 0.0233(12) 0.0255(12) 0.0290(13) -0.0061(10) 0.0054(10) -0.0044(10)
N2 0.0135(12) 0.0178(12) 0.0214(13) -0.0038(10) 0.0001(10) 0.0030(10)
C2 0.0219(16) 0.0264(17) 0.0192(15) -0.0044(12) 0.0055(12) 0.0018(13)
N3 0.0179(13) 0.0217(13) 0.0236(14) 0.0002(11) -0.0039(11) 0.0033(10)
O3 0.0368(15) 0.0296(14) 0.0419(16) -0.0153(12) 0.0236(12) -0.0055(11)
C3 0.0200(16) 0.0242(16) 0.0320(18) -0.0033(14) -0.0029(13) 0.0078(13)
Cl3 0.0264(4) 0.0263(4) 0.0264(4) 0.0028(3) -0.0023(3) -0.0034(3)
N4 0.0159(12) 0.0172(12) 0.0156(12) -0.0005(9) 0.0010(10) 0.0016(10)
C4 0.0186(15) 0.0250(16) 0.0226(16) 0.0008(12) -0.0017(12) 0.0071(13)
O4 0.053(2) 0.0350(16) 0.063(2) -0.0179(14) 0.0338(17) -0.0117(14)
C5 0.0184(16) 0.0321(18) 0.0174(15) -0.0032(13) -0.0029(12) 0.0063(13)
O5 0.0300(15) 0.0303(14) 0.0297(14) 0.0013(11) 0.0090(11) 0.0053(11)
C6 0.0229(17) 0.0243(16) 0.0201(15) -0.0012(12) -0.0059(12) 0.0004(13)
C7 0.0201(15) 0.0195(15) 0.0178(14) 0.0014(11) 0.0025(12) 0.0023(12)
C8 0.0182(15) 0.0160(14) 0.0187(14) 0.0002(11) 0.0027(11) -0.0009(11)
C9 0.0164(15) 0.0183(15) 0.0215(15) -0.0036(12) 0.0017(12) -0.0016(12)
C10 0.0192(16) 0.0192(15) 0.0228(16) -0.0050(12) 0.0005(12) 0.0033(12)
C11 0.0222(17) 0.0228(16) 0.0225(16) -0.0048(12) 0.0034(13) 0.0001(13)
C12 0.0158(15) 0.0188(15) 0.0223(15) -0.0023(12) 0.0013(11) 0.0002(12)
C13 0.0217(16) 0.0189(15) 0.0201(15) 0.0024(12) 0.0008(12) 0.0030(12)
C14 0.0224(16) 0.0199(15) 0.0202(15) -0.0040(12) 0.0080(12) 0.0011(12)
C15 0.0294(18) 0.0208(16) 0.0247(17) -0.0067(13) 0.0091(14) -0.0002(13)
C16 0.0318(19) 0.0204(16) 0.0288(18) -0.0052(13) 0.0123(15) -0.0018(14)
C17 0.039(2) 0.0248(18) 0.040(2) -0.0112(16) 0.0210(17) -0.0039(15)
C18 0.037(2) 0.0236(17) 0.0336(19) -0.0059(14) 0.0156(16) -0.0016(15)
_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
Co N3 1.933(3) . ?
Co N1 1.942(3) . ?
Co N2 2.048(3) . ?
Co N4 2.051(2) . ?
Co Cl2 2.2715(8) . ?
Co Cl1 2.2790(8) . ?
N1 C7 1.468(4) . ?
N1 C1 1.474(4) . ?
N1 H1N 0.9100 . ?
O1 C13 1.212(4) . ?
C1 C2 1.515(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
O2 C13 1.323(4) . ?
O2 HO2 0.8200 . ?
N2 C9 1.498(4) . ?
N2 C3 1.509(4) . ?
N2 C2 1.512(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
N3 C4 1.462(4) . ?
N3 C5 1.467(4) . ?
N3 HN3 0.9100 . ?
O3 C18 1.328(4) . ?
O3 HO3 0.8200 . ?
C3 C4 1.505(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
N4 C14 1.501(4) . ?
N4 C8 1.504(4) . ?
N4 C6 1.520(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
O4 C18 1.202(5) . ?
C5 C6 1.500(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
O5 H2O5 0.86(4) . ?
O5 H1O5 0.81(5) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.510(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.525(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.519(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.519(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.501(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C14 C15 1.528(4) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.531(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.524(5) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.513(5) . ?
C17 H17A 0.9700 . ?
C17 H17B 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
N3 Co N1 94.55(12) . . ?
N3 Co N2 83.90(11) . . ?
N1 Co N2 85.31(11) . . ?
N3 Co N4 84.97(11) . . ?
N1 Co N4 85.85(10) . . ?
N2 Co N4 165.18(10) . . ?
N3 Co Cl2 91.27(9) . . ?
N1 Co Cl2 174.19(8) . . ?
N2 Co Cl2 95.45(8) . . ?
N4 Co Cl2 94.55(7) . . ?
N3 Co Cl1 179.21(9) . . ?
N1 Co Cl1 84.66(8) . . ?
N2 Co Cl1 96.04(7) . . ?
N4 Co Cl1 94.96(7) . . ?
Cl2 Co Cl1 89.52(3) . . ?
C7 N1 C1 119.3(2) . . ?
C7 N1 Co 111.06(19) . . ?
C1 N1 Co 111.1(2) . . ?
C7 N1 H1N 104.7 . . ?
C1 N1 H1N 104.7 . . ?
Co N1 H1N 104.7 . . ?
N1 C1 C2 104.8(3) . . ?
N1 C1 H1A 110.8 . . ?
C2 C1 H1A 110.8 . . ?
N1 C1 H1B 110.8 . . ?
C2 C1 H1B 110.8 . . ?
H1A C1 H1B 108.9 . . ?
C13 O2 HO2 109.5 . . ?
C9 N2 C3 111.3(3) . . ?
C9 N2 C2 110.6(2) . . ?
C3 N2 C2 107.5(2) . . ?
C9 N2 Co 113.17(18) . . ?
C3 N2 Co 108.67(19) . . ?
C2 N2 Co 105.38(18) . . ?
N2 C2 C1 108.3(3) . . ?
N2 C2 H2A 110.0 . . ?
C1 C2 H2A 110.0 . . ?
N2 C2 H2B 110.0 . . ?
C1 C2 H2B 110.0 . . ?
H2A C2 H2B 108.4 . . ?
C4 N3 C5 116.2(3) . . ?
C4 N3 Co 109.9(2) . . ?
C5 N3 Co 109.7(2) . . ?
C4 N3 HN3 106.8 . . ?
C5 N3 HN3 106.8 . . ?
Co N3 HN3 106.8 . . ?
C18 O3 HO3 109.5 . . ?
C4 C3 N2 110.6(3) . . ?
C4 C3 H3A 109.5 . . ?
N2 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
C14 N4 C8 109.8(2) . . ?
C14 N4 C6 111.2(2) . . ?
C8 N4 C6 108.6(2) . . ?
C14 N4 Co 114.34(19) . . ?
C8 N4 Co 104.75(18) . . ?
C6 N4 Co 107.84(18) . . ?
N3 C4 C3 107.1(3) . . ?
N3 C4 H4A 110.3 . . ?
C3 C4 H4A 110.3 . . ?
N3 C4 H4B 110.3 . . ?
C3 C4 H4B 110.3 . . ?
H4A C4 H4B 108.6 . . ?
N3 C5 C6 108.3(3) . . ?
N3 C5 H5A 110.0 . . ?
C6 C5 H5A 110.0 . . ?
N3 C5 H5B 110.0 . . ?
C6 C5 H5B 110.0 . . ?
H5A C5 H5B 108.4 . . ?
H2O5 O5 H1O5 102(4) . . ?
C5 C6 N4 111.5(3) . . ?
C5 C6 H6A 109.3 . . ?
N4 C6 H6A 109.3 . . ?
C5 C6 H6B 109.3 . . ?
N4 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
N1 C7 C8 105.9(2) . . ?
N1 C7 H7A 110.6 . . ?
C8 C7 H7A 110.6 . . ?
N1 C7 H7B 110.6 . . ?
C8 C7 H7B 110.6 . . ?
H7A C7 H7B 108.7 . . ?
N4 C8 C7 109.3(2) . . ?
N4 C8 H8A 109.8 . . ?
C7 C8 H8A 109.8 . . ?
N4 C8 H8B 109.8 . . ?
C7 C8 H8B 109.8 . . ?
H8A C8 H8B 108.3 . . ?
N2 C9 C10 116.7(3) . . ?
N2 C9 H9A 108.1 . . ?
C10 C9 H9A 108.1 . . ?
N2 C9 H9B 108.1 . . ?
C10 C9 H9B 108.1 . . ?
H9A C9 H9B 107.3 . . ?
C11 C10 C9 107.7(3) . . ?
C11 C10 H10A 110.2 . . ?
C9 C10 H10A 110.2 . . ?
C11 C10 H10B 110.2 . . ?
C9 C10 H10B 110.2 . . ?
H10A C10 H10B 108.5 . . ?
C12 C11 C10 112.9(3) . . ?
C12 C11 H11A 109.0 . . ?
C10 C11 H11A 109.0 . . ?
C12 C11 H11B 109.0 . . ?
C10 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
C13 C12 C11 113.9(3) . . ?
C13 C12 H12A 108.8 . . ?
C11 C12 H12A 108.8 . . ?
C13 C12 H12B 108.8 . . ?
C11 C12 H12B 108.8 . . ?
H12A C12 H12B 107.7 . . ?
O1 C13 O2 124.0(3) . . ?
O1 C13 C12 124.3(3) . . ?
O2 C13 C12 111.7(3) . . ?
N4 C14 C15 116.2(3) . . ?
N4 C14 H14A 108.2 . . ?
C15 C14 H14A 108.2 . . ?
N4 C14 H14B 108.2 . . ?
C15 C14 H14B 108.2 . . ?
H14A C14 H14B 107.4 . . ?
C14 C15 C16 109.7(3) . . ?
C14 C15 H15A 109.7 . . ?
C16 C15 H15A 109.7 . . ?
C14 C15 H15B 109.7 . . ?
C16 C15 H15B 109.7 . . ?
H15A C15 H15B 108.2 . . ?
C17 C16 C15 111.2(3) . . ?
C17 C16 H16A 109.4 . . ?
C15 C16 H16A 109.4 . . ?
C17 C16 H16B 109.4 . . ?
C15 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
C18 C17 C16 114.1(3) . . ?
C18 C17 H17A 108.7 . . ?
C16 C17 H17A 108.7 . . ?
C18 C17 H17B 108.7 . . ?
C16 C17 H17B 108.7 . . ?
H17A C17 H17B 107.6 . . ?
O4 C18 O3 123.7(3) . . ?
O4 C18 C17 124.9(3) . . ?
O3 C18 C17 111.4(3) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1N Cl3 0.91 2.51 3.267(3) 141.2 1_445
O2 HO2 Cl3 0.82 2.15 2.945(2) 163.7 .
N3 HN3 Cl1 0.91 2.41 3.243(3) 152.4 1_455
O3 HO3 O5 0.82 1.80 2.597(4) 162.8 .
O5 H2O5 Cl3 0.86(4) 2.31(4) 3.128(3) 159(4) 2_755
O5 H1O5 O1 0.81(5) 1.96(5) 2.762(4) 171(5) 2_755
_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full 27.11
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max 1.942
_refine_diff_density_min -0.609
_refine_diff_density_rms 0.090
#===END