# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

loop_
_publ_author_name
_publ_author_address

A.Grohmann
; Institut f\"ur Chemie
Technische Universit\"at Berlin
Strasse des 17. Juni 135
10623 Berlin
Germany
;
J.P.Boyd
; Institut f\"ur Chemie
Technische Universit\"at Berlin
Strasse des 17. Juni 135
10623 Berlin
Germany
;
E.Irran
; Institut f\"ur Chemie
Technische Universit\"at Berlin
Strasse des 17. Juni 135
10623 Berlin
Germany
;

_publ_section_title              
;
Tetrapodal amidoxime ligands I.
Coordination isomerism due to self-complementary
dimerization of a pyramidal cobalt(III) coordination module
;

# Attachment '- BOYD18_revised.CIF'
loop_
_publ_contact_author_name
_publ_contact_author_address
'Andreas Grohmann'
;
Institut f\"ur Chemie
Technische Universit\"at Berlin
Strasse des 16. Juni 135
10623 Berlin
Germany
;

_publ_contact_author_phone       '049 30 314 79877'
_publ_contact_author_fax         '049 30 314 22935'
_publ_contact_author_email       andreas.grohmann@chem.tu-berlin.de
_publ_requested_coeditor_name    ?

# Attachment '- BOYD30_revised.CIF'

_publ_contact_author             
;
Andreas Grohmann
Institut f\"ur Chemie
Technische Universit\"at Berlin
Strasse des 16. Juni 135
10623 Berlin
Germany
;

_publ_contact_letter             
;
Andreas Grohmann
Institut f\"ur Chemie
Technische Universit\"at Berlin
Strasse des 17. Juni 135
10623 Berlin
Germany
;

data_boyd18
_database_code_depnum_ccdc_archive 'CCDC 825623'
#TrackingRef '- BOYD18_revised.CIF'

_audit_creation_method           
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H8 N6'
_chemical_formula_weight         236.24

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

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                   6.6056(2)
_cell_length_b                   10.9046(4)
_cell_length_c                   16.8884(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.859(3)
_cell_angle_gamma                90.00
_cell_volume                     1205.07(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3825
_cell_measurement_theta_min      3.0615
_cell_measurement_theta_max      32.3330

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             488
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9499
_exptl_absorpt_correction_T_max  0.9745
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5796
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2107
_reflns_number_gt                1772
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The pyrimidine ring is disordered over two positions (refined occupancies
0.78/0.22) for atoms N3, C4, and C5 therefore restrained C-C and C-N distances
for the pyrimidine ring were defined as follows:
DFIX 2.66 0.02 N1 C4 N1 C4a
DFIX 1.32 0.01 C2 N3 C6 N3A
DFIX 1.33 0.01 C4 N3 C4A N3A
DFIX 1.38 0.01 C5 C4 C5A C4A
DFIX 1.39 0.01 C6 C5 C2 C5A
FLAT N1 C2 C6 C5 C5A C4 C4A N3 N3A
Equal anisotropic displacement parameters:
EADP C5 N3A
EADP C5A N3
EADP C4 C4A
;

_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^)+(0.0385P)^2^+0.2226P] 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         2107
_refine_ls_number_parameters     181
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0349
_refine_ls_wR_factor_ref         0.0800
_refine_ls_wR_factor_gt          0.0760
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N3A N 0.6120(12) 0.2887(8) 0.6895(4) 0.0243(6) Uani 0.763(3) 1 d PD A 1
C5A C 0.5364(13) 0.4939(10) 0.7244(4) 0.0229(9) Uani 0.763(3) 1 d PD A 1
H5A H 0.5610(15) 0.5597(17) 0.7573(10) 0.027 Uiso 0.763(3) 1 calc PR A 1
C4A C 0.6466(10) 0.3865(9) 0.7378(4) 0.0242(10) Uani 0.763(3) 1 d PD A 1
H4A H 0.751(3) 0.3817(9) 0.7827(14) 0.029 Uiso 0.763(3) 1 calc PR A 1
C5 C 0.618(5) 0.299(3) 0.6938(15) 0.0243(6) Uani 0.24 1 d PD A 2
H5 H 0.706(8) 0.231(6) 0.7055(19) 0.029 Uiso 0.237(3) 1 calc PR A 2
N3 N 0.516(4) 0.503(3) 0.7250(12) 0.0229(9) Uani 0.24 1 d PD A 2
C4 C 0.622(4) 0.401(3) 0.7419(13) 0.0242(10) Uani 0.24 1 d PD A 2
H4 H 0.715(9) 0.399(3) 0.795(5) 0.029 Uiso 0.237(3) 1 calc PR A 2
N1 N 0.35494(15) 0.40247(10) 0.60821(6) 0.0201(3) Uani 1 1 d D A .
C23 C 0.42076(19) 0.19488(13) 0.57051(7) 0.0214(3) Uani 1 1 d . A .
C6 C 0.47092(18) 0.30451(12) 0.62648(7) 0.0197(3) Uani 1 1 d D . .
C12 C 0.23133(19) 0.60021(12) 0.64082(8) 0.0211(3) Uani 1 1 d . A .
C2 C 0.38685(18) 0.49646(12) 0.65872(8) 0.0195(3) Uani 1 1 d D . .
C22 C 0.38060(19) 0.23815(13) 0.48648(8) 0.0222(3) Uani 1 1 d . . .
C13 C 0.29865(19) 0.71432(14) 0.68426(8) 0.0241(3) Uani 1 1 d . . .
C21 C 0.5947(2) 0.10830(13) 0.57699(8) 0.0240(3) Uani 1 1 d . . .
N13 N 0.34917(18) 0.26889(12) 0.42155(7) 0.0313(3) Uani 1 1 d . A .
C11 C 0.19770(19) 0.62749(12) 0.55411(9) 0.0235(3) Uani 1 1 d . . .
C14 C 0.0269(2) 0.55680(14) 0.66750(8) 0.0253(3) Uani 1 1 d . . .
H14A H -0.0757(10) 0.6239(6) 0.6587(5) 0.038 Uiso 1 1 calc R A .
H14B H 0.0501(4) 0.5350(8) 0.7252(5) 0.038 Uiso 1 1 calc R . .
H14C H -0.0245(9) 0.4837(8) 0.6357(5) 0.038 Uiso 1 1 calc R . .
N12 N 0.16837(19) 0.65011(12) 0.48757(7) 0.0330(3) Uani 1 1 d . A .
N14 N 0.7254(2) 0.03884(12) 0.58242(8) 0.0346(3) Uani 1 1 d . A .
N11 N 0.34131(19) 0.80203(12) 0.71949(8) 0.0373(3) Uani 1 1 d . A .
C24 C 0.2271(2) 0.12912(14) 0.59184(9) 0.0299(4) Uani 1 1 d . . .
H24A H 0.1899(9) 0.0603(9) 0.5534(5) 0.045 Uiso 1 1 calc R A .
H24B H 0.1114(12) 0.1889(6) 0.5884(6) 0.045 Uiso 1 1 calc R . .
H24C H 0.2552(5) 0.0958(8) 0.6474(6) 0.045 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
N3A 0.0232(8) 0.0307(16) 0.0186(10) -0.0009(8) 0.0013(6) 0.0030(10)
C5A 0.022(2) 0.027(2) 0.0190(7) -0.0036(8) 0.0007(9) -0.0023(16)
C4A 0.017(2) 0.036(3) 0.0187(10) 0.0000(12) 0.0004(12) 0.0026(13)
C5 0.0232(8) 0.0307(16) 0.0186(10) -0.0009(8) 0.0013(6) 0.0030(10)
N3 0.022(2) 0.027(2) 0.0190(7) -0.0036(8) 0.0007(9) -0.0023(16)
C4 0.017(2) 0.036(3) 0.0187(10) 0.0000(12) 0.0004(12) 0.0026(13)
N1 0.0200(6) 0.0225(6) 0.0177(6) -0.0020(5) 0.0025(4) -0.0003(5)
C23 0.0231(7) 0.0227(7) 0.0179(7) -0.0007(6) 0.0008(5) 0.0025(6)
C6 0.0197(6) 0.0222(7) 0.0175(7) 0.0004(6) 0.0043(5) -0.0010(6)
C12 0.0233(7) 0.0210(7) 0.0183(7) -0.0016(6) 0.0006(5) -0.0006(6)
C2 0.0195(7) 0.0217(7) 0.0176(7) 0.0002(6) 0.0042(5) -0.0029(6)
C22 0.0215(7) 0.0207(7) 0.0239(7) -0.0048(6) 0.0012(5) 0.0020(6)
C13 0.0224(7) 0.0257(8) 0.0247(7) -0.0007(7) 0.0045(5) 0.0009(6)
C21 0.0311(8) 0.0212(8) 0.0187(7) -0.0023(6) -0.0001(5) -0.0015(7)
N13 0.0335(7) 0.0363(8) 0.0231(7) -0.0003(6) 0.0010(5) 0.0073(6)
C11 0.0229(7) 0.0199(7) 0.0272(8) -0.0025(6) 0.0013(5) -0.0019(6)
C14 0.0214(7) 0.0279(8) 0.0261(7) 0.0000(7) 0.0018(5) 0.0000(6)
N12 0.0382(7) 0.0343(8) 0.0253(7) 0.0032(6) -0.0003(5) -0.0025(6)
N14 0.0385(7) 0.0279(7) 0.0356(8) -0.0023(6) -0.0017(6) 0.0070(6)
N11 0.0376(7) 0.0334(8) 0.0415(8) -0.0146(7) 0.0073(6) -0.0039(6)
C24 0.0316(8) 0.0311(8) 0.0275(8) -0.0032(7) 0.0058(6) -0.0056(7)

_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
N3A C6 1.327(3) . ?
N3A C4A 1.342(4) . ?
C5A C4A 1.381(4) . ?
C5A C2 1.381(4) . ?
C5 C4 1.383(10) . ?
C5 C6 1.390(10) . ?
N3 C2 1.313(10) . ?
N3 C4 1.322(10) . ?
N1 C6 1.3260(17) . ?
N1 C2 1.3317(17) . ?
C23 C21 1.4796(19) . ?
C23 C22 1.4846(19) . ?
C23 C6 1.5319(18) . ?
C23 C24 1.5512(19) . ?
C12 C11 1.4809(19) . ?
C12 C13 1.4816(19) . ?
C12 C2 1.5303(18) . ?
C12 C14 1.5545(18) . ?
C22 N13 1.1383(18) . ?
C13 N11 1.1413(18) . ?
C21 N14 1.1427(18) . ?
C11 N12 1.1408(18) . ?

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
C6 N3A C4A 115.2(5) . . ?
C4A C5A C2 116.8(6) . . ?
N3A C4A C5A 122.2(5) . . ?
C4 C5 C6 113.5(19) . . ?
C2 N3 C4 113.5(19) . . ?
N3 C4 C5 125.9(18) . . ?
C6 N1 C2 115.79(10) . . ?
C21 C23 C22 108.00(11) . . ?
C21 C23 C6 110.62(10) . . ?
C22 C23 C6 109.70(11) . . ?
C21 C23 C24 110.15(11) . . ?
C22 C23 C24 108.89(11) . . ?
C6 C23 C24 109.46(10) . . ?
N1 C6 N3A 127.7(4) . . ?
N1 C6 C5 122.9(14) . . ?
N3A C6 C5 4.9(17) . . ?
N1 C6 C23 114.56(10) . . ?
N3A C6 C23 117.6(4) . . ?
C5 C6 C23 122.4(14) . . ?
C11 C12 C13 108.37(11) . . ?
C11 C12 C2 110.47(11) . . ?
C13 C12 C2 112.03(10) . . ?
C11 C12 C14 109.21(10) . . ?
C13 C12 C14 109.03(11) . . ?
C2 C12 C14 107.69(11) . . ?
N3 C2 N1 128.1(14) . . ?
N3 C2 C5A 6.7(17) . . ?
N1 C2 C5A 122.1(4) . . ?
N3 C2 C12 117.8(13) . . ?
N1 C2 C12 113.53(10) . . ?
C5A C2 C12 124.1(4) . . ?
N13 C22 C23 178.59(15) . . ?
N11 C13 C12 176.42(14) . . ?
N14 C21 C23 178.07(15) . . ?
N12 C11 C12 178.52(15) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.148
_refine_diff_density_min         -0.146
_refine_diff_density_rms         0.030

data_boyd30
_database_code_depnum_ccdc_archive 'CCDC 825624'
#TrackingRef '- BOYD30_revised.CIF'

_audit_creation_method           
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H38 Co2 N20 O8, 4(C2 F3 O2), 12(H2 O)'
_chemical_formula_sum            'C32 H62 Co2 F12 N20 O28'
_chemical_formula_weight         1520.88

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'
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

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.2213(4)
_cell_length_b                   12.9948(6)
_cell_length_c                   13.4621(8)
_cell_angle_alpha                69.118(5)
_cell_angle_beta                 83.997(4)
_cell_angle_gamma                73.435(4)
_cell_volume                     1444.63(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5417
_cell_measurement_theta_min      3.2742
_cell_measurement_theta_max      32.4308

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             780
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7626
_exptl_absorpt_correction_T_max  0.9254
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10144
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.28
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5065
_reflns_number_gt                3966
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_structure_solution    SIR-2004
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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.
One of the trifluoromethyl groups is disordered over two positions
(occupancies 0.6/0.4) for atoms F36 F37 F38 therefore similarity
restraints were imposed on C-F distances and angles as well as F
atomic displacement parameters:
SADI C36 F36 C36 F36A C36 F37 C36 F37A C36 F38 C36 F38A
SADI C37 F36 C37 F36A C37 F37 C37 F37A C37 F38 C37 F38A
SADI C30 F33 C30 F34 C30 F35
SADI C29 F33 C29 F34 C29 F35
SIMU 0.005 F38 F38A F36 F36A F37 F37A
DELU 0.003 F38 F38A F36 F36A F37 F37A
The pyrimidine ring is disordered over two positions (occupancies
0.5/0.5) for atoms N26, C26, and C25 therefore restrained C-C
and C-N distances for the pyrimidine ring were defined as follows:
DFIX 2.66 0.01 N4 C25A N4 C25B
DFIX 1.32 0.02 C19 N26B C20 N26A
DFIX 1.33 0.02 C25B N26B C25A N26A
DFIX 1.38 0.02 C25A C26A C25B C26B
DFIX 1.39 0.02 C19 C26A C20 C26B
ISOR 0.150 C26B N26B C26A N26A
Equal anisotropic displacement parameters:
DELU 0.010 0.010 C25A C26A
DELU 0.010 0.010 C25B N26B
DELU 0.010 0.010 C25A N26A
DELU 0.010 0.010 C25B C26B
DELU 0.010 0.010 N26B C20
DELU 0.010 0.010 C26A C20
DELU 0.010 0.010 C26B C19
DELU 0.010 0.010 N26A C19
EADP C25B C25A
EADP C26B N26A
EADP N26B C26A
Additional restraints were used to fix the H-Atom positions
belonging to water of crystallization.
;

_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^)+(0.0515P)^2^+0.0000P] 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         5065
_refine_ls_number_parameters     535
_refine_ls_number_restraints     110
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0389
_refine_ls_wR_factor_ref         0.0928
_refine_ls_wR_factor_gt          0.0892
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_restrained_S_all      0.982
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C25B C 1.026(2) 0.710(3) 0.3887(19) 0.015(3) Uani 0.50 1 d PDU A 1
H25B H 1.1255 0.7194 0.3741 0.018 Uiso 0.50 1 calc PR A 1
C26B C 0.962(3) 0.679(4) 0.320(3) 0.015(3) Uani 0.50 1 d PDU A 1
H26B H 1.0155 0.6691 0.2580 0.018 Uiso 0.50 1 calc PR A 1
N26B N 0.955(3) 0.728(4) 0.476(2) 0.018(2) Uani 0.50 1 d PDU A 1
C25A C 1.015(2) 0.722(3) 0.3659(19) 0.015(3) Uani 0.50 1 d PDU A 2
H25A H 1.1081 0.7409 0.3417 0.018 Uiso 0.50 1 calc PR A 2
C26A C 0.956(3) 0.733(4) 0.462(3) 0.018(2) Uani 0.50 1 d PDU A 2
H26A H 1.0071 0.7583 0.5029 0.022 Uiso 0.50 1 calc PR A 2
N26A N 0.949(2) 0.686(3) 0.306(2) 0.015(3) Uani 0.50 1 d PDU A 2
Co1 Co 0.56610(4) 0.63317(3) 0.47598(3) 0.01099(11) Uani 1 1 d . . .
O8 O 0.6464(2) 0.44091(17) 0.67709(17) 0.0183(5) Uani 1 1 d . . .
H8 H 0.646(4) 0.414(3) 0.634(3) 0.027 Uiso 1 1 d . . .
O11 O 0.3563(2) 0.84570(17) 0.47989(18) 0.0238(5) Uani 1 1 d . . .
O3 O 0.62990(19) 0.39534(14) 0.49665(14) 0.0117(4) Uani 1 1 d . . .
O10 O 0.3505(2) 0.79501(17) 0.31152(17) 0.0189(5) Uani 1 1 d . . .
H10 H 0.342(4) 0.816(3) 0.361(3) 0.023 Uiso 1 1 d . . .
C19 C 0.8200(3) 0.7073(2) 0.4952(2) 0.0138(6) Uani 1 1 d D . .
C20 C 0.8199(3) 0.6621(2) 0.3424(2) 0.0144(6) Uani 1 1 d D . .
N4 N 0.7533(2) 0.67200(18) 0.43373(18) 0.0132(5) Uani 1 1 d D A .
N2 N 0.6418(2) 0.50287(18) 0.43279(18) 0.0122(5) Uani 1 1 d . A .
N5 N 0.6524(2) 0.55208(18) 0.61521(18) 0.0133(5) Uani 1 1 d . A .
N12 N 0.7611(3) 0.4207(2) 0.3090(2) 0.0193(6) Uani 1 1 d . A .
H12A H 0.749(3) 0.356(3) 0.351(3) 0.023 Uiso 1 1 d . . .
H12B H 0.778(4) 0.427(3) 0.251(3) 0.023 Uiso 1 1 d . . .
N13 N 0.7794(3) 0.5411(2) 0.7604(2) 0.0183(5) Uani 1 1 d . A .
H13A H 0.770(3) 0.472(3) 0.795(3) 0.022 Uiso 1 1 d . . .
H13B H 0.810(3) 0.576(3) 0.793(3) 0.022 Uiso 1 1 d . . .
N14 N 0.5295(3) 0.8870(2) 0.5982(2) 0.0216(6) Uani 1 1 d . A .
H14A H 0.442(4) 0.919(3) 0.590(3) 0.026 Uiso 1 1 d . . .
H14B H 0.573(4) 0.901(3) 0.638(3) 0.026 Uiso 1 1 d . . .
N15 N 0.5225(3) 0.7654(2) 0.1522(2) 0.0202(6) Uani 1 1 d . A .
H15A H 0.434(4) 0.804(3) 0.147(3) 0.024 Uiso 1 1 d . . .
H15B H 0.577(4) 0.771(3) 0.099(3) 0.024 Uiso 1 1 d . . .
N7 N 0.4979(2) 0.72212(18) 0.33365(18) 0.0133(5) Uani 1 1 d . A .
N6 N 0.4960(2) 0.76594(18) 0.51645(18) 0.0145(5) Uani 1 1 d . A .
C22 C 0.7329(3) 0.6269(2) 0.2741(2) 0.0138(6) Uani 1 1 d . A .
C17 C 0.7366(3) 0.7151(2) 0.5990(2) 0.0138(6) Uani 1 1 d . A .
C27 C 0.8203(3) 0.6240(2) 0.1719(2) 0.0183(6) Uani 1 1 d . . .
H27A H 0.7615(13) 0.6069(15) 0.1275(10) 0.028 Uiso 1 1 calc R A .
H27B H 0.9152(18) 0.5659(14) 0.1892(3) 0.028 Uiso 1 1 calc R . .
H27C H 0.8395(18) 0.6974(13) 0.1343(10) 0.028 Uiso 1 1 calc R . .
C28 C 0.8244(3) 0.7590(2) 0.6579(2) 0.0201(7) Uani 1 1 d . . .
H28A H 0.8355(17) 0.8354(14) 0.6112(9) 0.030 Uiso 1 1 calc R A .
H28B H 0.9264(19) 0.7047(12) 0.6770(13) 0.030 Uiso 1 1 calc R . .
H28C H 0.7686(14) 0.7655(14) 0.7237(13) 0.030 Uiso 1 1 calc R . .
C23 C 0.7090(3) 0.5094(2) 0.3416(2) 0.0137(6) Uani 1 1 d . . .
C16 C 0.7201(3) 0.5958(2) 0.6633(2) 0.0135(6) Uani 1 1 d . . .
C21 C 0.5744(3) 0.7122(2) 0.2499(2) 0.0139(6) Uani 1 1 d . . .
C18 C 0.5766(3) 0.7962(2) 0.5694(2) 0.0153(6) Uani 1 1 d . . .
H11 H 0.292(3) 0.830(2) 0.535(3) 0.018 Uiso 1 1 d . . .
C30 C 0.0151(4) 0.9391(3) 0.7303(3) 0.0335(8) Uani 1 1 d D . .
C29 C 0.1418(3) 0.9237(3) 0.6516(3) 0.0261(7) Uani 1 1 d D . .
O32 O 0.2133(2) 0.99817(18) 0.62182(18) 0.0331(6) Uani 1 1 d . . .
O31 O 0.1603(2) 0.83949(19) 0.6224(2) 0.0363(6) Uani 1 1 d . . .
F33 F 0.0334(3) 0.9945(2) 0.7906(2) 0.0724(8) Uani 1 1 d D . .
F34 F -0.0114(2) 0.84144(18) 0.79443(17) 0.0495(6) Uani 1 1 d D . .
F35 F -0.1143(2) 1.00065(19) 0.6766(2) 0.0606(7) Uani 1 1 d D . .
C36 C 0.7569(3) 0.3690(3) 0.0436(2) 0.0237(7) Uani 1 1 d D B .
C37 C 0.6222(4) 0.3228(3) 0.1002(3) 0.0362(8) Uani 1 1 d D . .
O38 O 0.7993(3) 0.34776(19) -0.03875(18) 0.0355(6) Uani 1 1 d . . .
O39 O 0.8090(2) 0.42218(18) 0.08604(17) 0.0251(5) Uani 1 1 d . . .
F38 F 0.5690(13) 0.3555(12) 0.1819(7) 0.067(3) Uani 0.60 1 d PDU B 1
F37 F 0.5061(9) 0.3608(14) 0.0348(11) 0.066(3) Uani 0.60 1 d PDU B 1
F36 F 0.6609(15) 0.2088(7) 0.1383(9) 0.065(3) Uani 0.60 1 d PDU B 1
F38A F 0.604(2) 0.3212(19) 0.1988(10) 0.070(5) Uani 0.40 1 d PDU B 2
F37A F 0.4944(14) 0.380(2) 0.0485(18) 0.080(6) Uani 0.40 1 d PDU B 2
F36A F 0.637(2) 0.2175(9) 0.1022(13) 0.063(4) Uani 0.40 1 d PDU B 2
O800 O 0.5887(3) 0.9680(2) 0.76302(19) 0.0343(6) Uani 1 1 d D C 2
H801 H 0.626(4) 1.021(3) 0.741(3) 0.041 Uiso 1 1 d D D 2
H802 H 0.483(4) 1.007(3) 0.777(3) 0.041 Uiso 1 1 d D E 2
O400 O 0.8735(2) 0.61639(18) 0.91703(17) 0.0220(5) Uani 1 1 d D F 2
H401 H 0.976(3) 0.604(3) 0.921(2) 0.026 Uiso 1 1 d D G 2
H402 H 0.856(3) 0.561(3) 0.969(2) 0.026 Uiso 1 1 d D H 2
O500 O 0.7011(3) 0.8179(2) 0.95520(18) 0.0286(5) Uani 1 1 d D I 2
H502 H 0.751(4) 0.760(3) 0.943(3) 0.034 Uiso 1 1 d D J 2
H501 H 0.656(4) 0.871(3) 0.894(3) 0.034 Uiso 1 1 d D K 2
O300 O 0.8371(3) 0.9300(2) 0.0503(2) 0.0458(7) Uani 1 1 d D L 2
H301 H 0.777(4) 1.0018(18) 0.000(2) 0.055 Uiso 1 1 d D M 2
H302 H 0.796(4) 0.897(3) 0.009(3) 0.055 Uiso 1 1 d D N 2
O600 O 0.6943(3) 0.9129(2) 0.2421(2) 0.0392(6) Uani 1 1 d D O 2
H601 H 0.735(4) 0.952(3) 0.286(3) 0.047 Uiso 1 1 d D P 2
H602 H 0.765(3) 0.924(3) 0.181(2) 0.047 Uiso 1 1 d D Q 2
O700 O 0.1661(3) 0.8507(2) 0.0873(2) 0.0477(7) Uani 1 1 d D R 2
H701 H 0.191(4) 0.789(3) 0.066(3) 0.057 Uiso 1 1 d D S 2
H702 H 0.064(4) 0.850(3) 0.103(3) 0.057 Uiso 1 1 d D T 2

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
C25B 0.010(2) 0.017(6) 0.015(8) 0.000(8) -0.002(4) -0.004(4)
C26B 0.010(3) 0.017(4) 0.015(6) -0.003(5) -0.002(4) -0.001(4)
N26B 0.0165(15) 0.018(4) 0.020(6) -0.006(5) -0.003(2) -0.0054(12)
C25A 0.010(2) 0.017(6) 0.015(8) 0.000(8) -0.002(4) -0.004(4)
C26A 0.0165(15) 0.018(4) 0.020(6) -0.006(5) -0.003(2) -0.0054(12)
N26A 0.010(3) 0.017(4) 0.015(6) -0.003(5) -0.002(4) -0.001(4)
Co1 0.00927(19) 0.0135(2) 0.0112(2) -0.00555(15) -0.00090(14) -0.00260(14)
O8 0.0245(11) 0.0159(11) 0.0155(12) -0.0035(9) -0.0031(9) -0.0081(8)
O11 0.0156(11) 0.0244(12) 0.0293(13) -0.0130(10) -0.0069(9) 0.0050(9)
O3 0.0105(9) 0.0105(9) 0.0135(10) -0.0035(8) -0.0006(7) -0.0026(7)
O10 0.0128(10) 0.0223(11) 0.0199(12) -0.0087(9) -0.0037(8) 0.0011(8)
C19 0.0124(14) 0.0124(14) 0.0159(16) -0.0046(12) -0.0024(11) -0.0017(11)
C20 0.0118(14) 0.0127(14) 0.0171(16) -0.0039(12) -0.0012(11) -0.0020(11)
N4 0.0109(11) 0.0141(12) 0.0142(13) -0.0050(10) -0.0011(9) -0.0022(9)
N2 0.0096(11) 0.0144(12) 0.0133(13) -0.0053(10) -0.0001(9) -0.0036(9)
N5 0.0138(12) 0.0127(12) 0.0136(13) -0.0035(10) -0.0013(9) -0.0045(9)
N12 0.0271(14) 0.0187(14) 0.0129(14) -0.0083(12) 0.0050(11) -0.0055(11)
N13 0.0234(14) 0.0170(14) 0.0163(15) -0.0054(11) -0.0078(11) -0.0057(11)
N14 0.0212(14) 0.0203(14) 0.0261(16) -0.0135(12) -0.0076(12) 0.0001(11)
N15 0.0168(14) 0.0277(15) 0.0125(14) -0.0070(12) -0.0017(11) 0.0002(11)
N7 0.0087(11) 0.0140(12) 0.0167(14) -0.0060(10) -0.0005(9) -0.0011(9)
N6 0.0108(12) 0.0147(12) 0.0164(14) -0.0057(10) -0.0030(10) 0.0007(9)
C22 0.0121(14) 0.0162(14) 0.0143(15) -0.0072(12) 0.0009(11) -0.0034(11)
C17 0.0114(14) 0.0167(15) 0.0158(16) -0.0080(12) -0.0012(11) -0.0038(11)
C27 0.0187(15) 0.0211(15) 0.0142(16) -0.0072(12) 0.0015(12) -0.0027(12)
C28 0.0221(16) 0.0206(16) 0.0223(18) -0.0104(13) -0.0046(13) -0.0076(12)
C23 0.0081(13) 0.0194(15) 0.0141(16) -0.0076(12) -0.0020(11) -0.0016(11)
C16 0.0080(13) 0.0180(15) 0.0161(16) -0.0100(12) 0.0008(11) -0.0010(11)
C21 0.0143(14) 0.0136(14) 0.0154(16) -0.0051(12) -0.0018(11) -0.0052(11)
C18 0.0171(15) 0.0151(15) 0.0132(15) -0.0048(12) 0.0014(11) -0.0039(12)
C30 0.032(2) 0.035(2) 0.044(2) -0.0227(18) 0.0011(16) -0.0119(16)
C29 0.0231(17) 0.0263(18) 0.033(2) -0.0181(15) 0.0000(14) -0.0029(14)
O32 0.0313(13) 0.0285(13) 0.0421(16) -0.0146(11) 0.0053(11) -0.0110(10)
O31 0.0327(13) 0.0312(13) 0.0512(17) -0.0224(12) 0.0085(11) -0.0104(10)
F33 0.0681(17) 0.112(2) 0.090(2) -0.0841(18) 0.0431(15) -0.0558(15)
F34 0.0522(14) 0.0558(15) 0.0438(14) -0.0182(12) 0.0159(11) -0.0237(11)
F35 0.0290(12) 0.0584(15) 0.0800(19) -0.0220(13) 0.0050(12) 0.0061(10)
C36 0.0289(18) 0.0199(16) 0.0198(18) -0.0031(14) -0.0024(14) -0.0067(13)
C37 0.032(2) 0.042(2) 0.041(2) -0.0168(19) -0.0017(17) -0.0156(17)
O38 0.0542(16) 0.0337(14) 0.0243(14) -0.0130(11) 0.0035(11) -0.0179(11)
O39 0.0272(12) 0.0269(12) 0.0266(13) -0.0130(10) 0.0037(9) -0.0119(9)
F38 0.042(5) 0.128(8) 0.068(5) -0.067(6) 0.032(4) -0.047(5)
F37 0.044(4) 0.097(6) 0.075(4) -0.029(3) -0.024(3) -0.036(4)
F36 0.071(4) 0.046(3) 0.069(7) 0.003(3) 0.005(4) -0.031(2)
F38A 0.062(8) 0.139(11) 0.031(4) -0.024(5) 0.014(4) -0.075(8)
F37A 0.037(5) 0.092(8) 0.086(8) -0.004(7) -0.006(5) -0.012(4)
F36A 0.069(7) 0.041(4) 0.091(10) -0.026(5) 0.028(7) -0.036(4)
O800 0.0375(15) 0.0346(14) 0.0331(15) -0.0128(12) -0.0010(11) -0.0114(11)
O400 0.0241(12) 0.0248(12) 0.0181(12) -0.0065(9) -0.0022(9) -0.0086(9)
O500 0.0336(14) 0.0280(13) 0.0244(13) -0.0125(10) 0.0003(10) -0.0040(10)
O300 0.0581(18) 0.0415(15) 0.0469(18) -0.0207(13) -0.0017(13) -0.0193(13)
O600 0.0340(14) 0.0369(14) 0.0524(18) -0.0208(13) 0.0025(12) -0.0120(11)
O700 0.0608(18) 0.0360(15) 0.0474(18) -0.0235(13) -0.0041(14) -0.0011(14)

_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
C25B N26B 1.341(14) . ?
C25B C26B 1.372(15) . ?
C25B H25B 0.9500 . ?
C26B C20 1.378(16) . ?
C26B H26B 0.9500 . ?
N26B C19 1.325(13) . ?
C25A N26A 1.334(13) . ?
C25A C26A 1.390(16) . ?
C25A H25A 0.9500 . ?
C26A C19 1.380(16) . ?
C26A H26A 0.9500 . ?
N26A C20 1.317(13) . ?
Co1 N2 1.907(2) . ?
Co1 N4 1.909(2) . ?
Co1 N6 1.911(2) . ?
Co1 N7 1.913(2) . ?
Co1 N5 1.919(2) . ?
Co1 O3 1.9196(17) 2_666 ?
O8 N5 1.401(3) . ?
O8 H8 0.77(3) . ?
O11 N6 1.408(3) . ?
O11 H11 0.90(3) . ?
O3 N2 1.384(3) . ?
O3 Co1 1.9196(17) 2_666 ?
O10 N7 1.408(3) . ?
O10 H10 0.79(3) . ?
C19 N4 1.347(3) . ?
C19 C17 1.545(4) . ?
C20 N4 1.348(3) . ?
C20 C22 1.537(4) . ?
N2 C23 1.302(3) . ?
N5 C16 1.297(3) . ?
N12 C23 1.324(4) . ?
N12 H12A 0.86(3) . ?
N12 H12B 0.76(3) . ?
N13 C16 1.333(4) . ?
N13 H13A 0.87(3) . ?
N13 H13B 0.85(3) . ?
N14 C18 1.316(4) . ?
N14 H14A 0.79(3) . ?
N14 H14B 0.79(3) . ?
N15 C21 1.316(4) . ?
N15 H15A 0.82(3) . ?
N15 H15B 0.82(3) . ?
N7 C21 1.293(3) . ?
N6 C18 1.301(4) . ?
C22 C27 1.527(4) . ?
C22 C23 1.538(4) . ?
C22 C21 1.545(4) . ?
C17 C28 1.525(4) . ?
C17 C16 1.525(4) . ?
C17 C18 1.544(4) . ?
C27 H27A 0.9650 . ?
C27 H27B 0.9650 . ?
C27 H27C 0.9650 . ?
C28 H28A 0.9957 . ?
C28 H28B 0.9957 . ?
C28 H28C 0.9957 . ?
C30 F33 1.313(4) . ?
C30 F34 1.329(4) . ?
C30 F35 1.345(4) . ?
C30 C29 1.512(4) . ?
C29 O32 1.251(4) . ?
C29 O31 1.252(4) . ?
C36 O38 1.235(4) . ?
C36 O39 1.250(4) . ?
C36 C37 1.544(4) . ?
C37 F38A 1.314(12) . ?
C37 F37A 1.315(12) . ?
C37 F38 1.316(8) . ?
C37 F37 1.323(8) . ?
C37 F36A 1.327(11) . ?
C37 F36 1.334(8) . ?
O800 H801 0.81(4) . ?
O800 H802 0.99(3) . ?
O400 H401 0.92(3) . ?
O400 H402 0.85(3) . ?
O500 H502 0.82(3) . ?
O500 H501 0.91(3) . ?
O300 H301 0.985(10) . ?
O300 H302 0.962(10) . ?
O600 H601 1.063(19) . ?
O600 H602 0.993(19) . ?
O700 H701 0.90(3) . ?
O700 H702 0.94(3) . ?

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
N26B C25B C26B 123.2(13) . . ?
N26B C25B H25B 118.4 . . ?
C26B C25B H25B 118.4 . . ?
C25B C26B C20 118.5(17) . . ?
C25B C26B H26B 120.7 . . ?
C20 C26B H26B 120.7 . . ?
C19 N26B C25B 115.8(14) . . ?
N26A C25A C26A 123.5(12) . . ?
N26A C25A H25A 118.2 . . ?
C26A C25A H25A 118.2 . . ?
C19 C26A C25A 117.6(18) . . ?
C19 C26A H26A 121.2 . . ?
C25A C26A H26A 121.2 . . ?
C20 N26A C25A 115.9(14) . . ?
N2 Co1 N4 89.35(9) . . ?
N2 Co1 N6 177.94(10) . . ?
N4 Co1 N6 88.66(9) . . ?
N2 Co1 N7 88.95(9) . . ?
N4 Co1 N7 87.18(9) . . ?
N6 Co1 N7 90.40(9) . . ?
N2 Co1 N5 92.63(9) . . ?
N4 Co1 N5 86.65(9) . . ?
N6 Co1 N5 87.80(9) . . ?
N7 Co1 N5 173.62(9) . . ?
N2 Co1 O3 90.92(8) . 2_666 ?
N4 Co1 O3 173.81(9) . 2_666 ?
N6 Co1 O3 90.99(8) . 2_666 ?
N7 Co1 O3 86.64(8) . 2_666 ?
N5 Co1 O3 99.51(8) . 2_666 ?
N5 O8 H8 102(3) . . ?
N6 O11 H11 105(2) . . ?
N2 O3 Co1 119.32(14) . 2_666 ?
N7 O10 H10 98(2) . . ?
N26B C19 N4 124.2(11) . . ?
N26B C19 C26A 7(3) . . ?
N4 C19 C26A 118.4(13) . . ?
N26B C19 C17 119.1(11) . . ?
N4 C19 C17 116.5(2) . . ?
C26A C19 C17 125.1(13) . . ?
N26A C20 N4 124.6(11) . . ?
N26A C20 C26B 9(3) . . ?
N4 C20 C26B 118.0(13) . . ?
N26A C20 C22 118.6(10) . . ?
N4 C20 C22 116.7(2) . . ?
C26B C20 C22 125.2(13) . . ?
C19 N4 C20 119.9(2) . . ?
C19 N4 Co1 120.55(17) . . ?
C20 N4 Co1 119.52(18) . . ?
C23 N2 O3 115.8(2) . . ?
C23 N2 Co1 122.04(19) . . ?
O3 N2 Co1 122.16(15) . . ?
C16 N5 O8 112.5(2) . . ?
C16 N5 Co1 123.31(19) . . ?
O8 N5 Co1 124.13(16) . . ?
C23 N12 H12A 117(2) . . ?
C23 N12 H12B 123(2) . . ?
H12A N12 H12B 118(3) . . ?
C16 N13 H13A 119(2) . . ?
C16 N13 H13B 121(2) . . ?
H13A N13 H13B 119(3) . . ?
C18 N14 H14A 116(2) . . ?
C18 N14 H14B 125(2) . . ?
H14A N14 H14B 116(3) . . ?
C21 N15 H15A 116(2) . . ?
C21 N15 H15B 123(2) . . ?
H15A N15 H15B 120(3) . . ?
C21 N7 O10 113.7(2) . . ?
C21 N7 Co1 123.92(18) . . ?
O10 N7 Co1 121.92(16) . . ?
C18 N6 O11 114.7(2) . . ?
C18 N6 Co1 123.91(18) . . ?
O11 N6 Co1 121.03(17) . . ?
C27 C22 C20 110.3(2) . . ?
C27 C22 C23 111.9(2) . . ?
C20 C22 C23 107.6(2) . . ?
C27 C22 C21 111.3(2) . . ?
C20 C22 C21 108.6(2) . . ?
C23 C22 C21 107.0(2) . . ?
C28 C17 C16 112.9(2) . . ?
C28 C17 C18 111.1(2) . . ?
C16 C17 C18 108.0(2) . . ?
C28 C17 C19 110.0(2) . . ?
C16 C17 C19 106.6(2) . . ?
C18 C17 C19 108.0(2) . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C17 C28 H28A 109.5 . . ?
C17 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C17 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N2 C23 N12 123.4(3) . . ?
N2 C23 C22 115.9(2) . . ?
N12 C23 C22 120.7(2) . . ?
N5 C16 N13 124.1(3) . . ?
N5 C16 C17 115.5(2) . . ?
N13 C16 C17 120.3(2) . . ?
N7 C21 N15 124.1(3) . . ?
N7 C21 C22 114.0(2) . . ?
N15 C21 C22 121.8(2) . . ?
N6 C18 N14 124.5(3) . . ?
N6 C18 C17 114.7(2) . . ?
N14 C18 C17 120.8(3) . . ?
F33 C30 F34 107.2(3) . . ?
F33 C30 F35 106.0(3) . . ?
F34 C30 F35 105.9(3) . . ?
F33 C30 C29 114.6(3) . . ?
F34 C30 C29 113.6(3) . . ?
F35 C30 C29 109.0(3) . . ?
O32 C29 O31 127.8(3) . . ?
O32 C29 C30 116.0(3) . . ?
O31 C29 C30 116.1(3) . . ?
O38 C36 O39 128.4(3) . . ?
O38 C36 C37 114.7(3) . . ?
O39 C36 C37 116.9(3) . . ?
F38A C37 F37A 109.0(14) . . ?
F38A C37 F38 20.4(15) . . ?
F37A C37 F38 90.9(13) . . ?
F38A C37 F37 121.5(11) . . ?
F37A C37 F37 15.3(19) . . ?
F38 C37 F37 104.9(9) . . ?
F38A C37 F36A 107.5(13) . . ?
F37A C37 F36A 102.5(14) . . ?
F38 C37 F36A 122.2(10) . . ?
F37 C37 F36A 89.7(11) . . ?
F38A C37 F36 88.2(12) . . ?
F37A C37 F36 120.6(12) . . ?
F38 C37 F36 105.9(9) . . ?
F37 C37 F36 109.8(9) . . ?
F36A C37 F36 22.4(11) . . ?
F38A C37 C36 113.0(9) . . ?
F37A C37 C36 112.3(9) . . ?
F38 C37 C36 113.9(7) . . ?
F37 C37 C36 110.7(7) . . ?
F36A C37 C36 111.9(8) . . ?
F36 C37 C36 111.3(6) . . ?
H801 O800 H802 101(3) . . ?
H401 O400 H402 103(3) . . ?
H502 O500 H501 109(3) . . ?
H301 O300 H302 82(3) . . ?
H601 O600 H602 99(3) . . ?
H701 O700 H702 96(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N26B C25B C26B C20 -2(6) . . . . ?
C26B C25B N26B C19 4(6) . . . . ?
N26A C25A C26A C19 -1(6) . . . . ?
C26A C25A N26A C20 1(6) . . . . ?
C25B N26B C19 N4 -1(5) . . . . ?
C25B N26B C19 C17 174(3) . . . . ?
C25A C26A C19 N4 0(5) . . . . ?
C25A C26A C19 C17 -180(3) . . . . ?
C25A N26A C20 N4 0(4) . . . . ?
C25A N26A C20 C26B -41(20) . . . . ?
C25A N26A C20 C22 176(3) . . . . ?
C25B C26B C20 N26A 139(25) . . . . ?
C25B C26B C20 N4 -3(5) . . . . ?
C25B C26B C20 C22 -180(3) . . . . ?
N26B C19 N4 C20 -4(2) . . . . ?
C26A C19 N4 C20 0(2) . . . . ?
C17 C19 N4 C20 -179.4(2) . . . . ?
N26B C19 N4 Co1 175(2) . . . . ?
C26A C19 N4 Co1 179(2) . . . . ?
C17 C19 N4 Co1 -0.5(3) . . . . ?
N26A C20 N4 C19 0(2) . . . . ?
C26B C20 N4 C19 6(2) . . . . ?
C22 C20 N4 C19 -177.1(2) . . . . ?
N26A C20 N4 Co1 -179(2) . . . . ?
C26B C20 N4 Co1 -173(2) . . . . ?
C22 C20 N4 Co1 3.9(3) . . . . ?
N2 Co1 N4 C19 -137.1(2) . . . . ?
N6 Co1 N4 C19 43.4(2) . . . . ?
N7 Co1 N4 C19 133.9(2) . . . . ?
N5 Co1 N4 C19 -44.5(2) . . . . ?
O3 Co1 N4 C19 130.3(7) 2_666 . . . ?
N2 Co1 N4 C20 41.8(2) . . . . ?
N6 Co1 N4 C20 -137.6(2) . . . . ?
N7 Co1 N4 C20 -47.2(2) . . . . ?
N5 Co1 N4 C20 134.5(2) . . . . ?
O3 Co1 N4 C20 -50.8(9) 2_666 . . . ?
Co1 O3 N2 C23 -112.5(2) 2_666 . . . ?
Co1 O3 N2 Co1 68.0(2) 2_666 . . . ?
N4 Co1 N2 C23 -47.3(2) . . . . ?
N6 Co1 N2 C23 -32(3) . . . . ?
N7 Co1 N2 C23 39.9(2) . . . . ?
N5 Co1 N2 C23 -133.9(2) . . . . ?
O3 Co1 N2 C23 126.6(2) 2_666 . . . ?
N4 Co1 N2 O3 132.25(18) . . . . ?
N6 Co1 N2 O3 148(3) . . . . ?
N7 Co1 N2 O3 -140.56(18) . . . . ?
N5 Co1 N2 O3 45.63(18) . . . . ?
O3 Co1 N2 O3 -53.9(2) 2_666 . . . ?
N2 Co1 N5 C16 137.8(2) . . . . ?
N4 Co1 N5 C16 48.6(2) . . . . ?
N6 Co1 N5 C16 -40.2(2) . . . . ?
N7 Co1 N5 C16 33.5(9) . . . . ?
O3 Co1 N5 C16 -130.84(19) 2_666 . . . ?
N2 Co1 N5 O8 -43.89(19) . . . . ?
N4 Co1 N5 O8 -133.09(19) . . . . ?
N6 Co1 N5 O8 138.13(19) . . . . ?
N7 Co1 N5 O8 -148.1(7) . . . . ?
O3 Co1 N5 O8 47.49(19) 2_666 . . . ?
N2 Co1 N7 C21 -40.4(2) . . . . ?
N4 Co1 N7 C21 49.0(2) . . . . ?
N6 Co1 N7 C21 137.7(2) . . . . ?
N5 Co1 N7 C21 64.1(9) . . . . ?
O3 Co1 N7 C21 -131.4(2) 2_666 . . . ?
N2 Co1 N7 O10 131.72(19) . . . . ?
N4 Co1 N7 O10 -138.88(19) . . . . ?
N6 Co1 N7 O10 -50.24(19) . . . . ?
N5 Co1 N7 O10 -123.8(8) . . . . ?
O3 Co1 N7 O10 40.74(18) 2_666 . . . ?
N2 Co1 N6 C18 -60(3) . . . . ?
N4 Co1 N6 C18 -44.2(2) . . . . ?
N7 Co1 N6 C18 -131.4(2) . . . . ?
N5 Co1 N6 C18 42.5(2) . . . . ?
O3 Co1 N6 C18 142.0(2) 2_666 . . . ?
N2 Co1 N6 O11 113(3) . . . . ?
N4 Co1 N6 O11 128.6(2) . . . . ?
N7 Co1 N6 O11 41.5(2) . . . . ?
N5 Co1 N6 O11 -144.7(2) . . . . ?
O3 Co1 N6 O11 -45.2(2) 2_666 . . . ?
N26A C20 C22 C27 1(2) . . . . ?
N4 C20 C22 C27 177.8(2) . . . . ?
C26B C20 C22 C27 -5(2) . . . . ?
N26A C20 C22 C23 123(2) . . . . ?
N4 C20 C22 C23 -59.9(3) . . . . ?
C26B C20 C22 C23 117(2) . . . . ?
N26A C20 C22 C21 -121(2) . . . . ?
N4 C20 C22 C21 55.6(3) . . . . ?
C26B C20 C22 C21 -128(2) . . . . ?
N26B C19 C17 C28 6(2) . . . . ?
N4 C19 C17 C28 -178.6(2) . . . . ?
C26A C19 C17 C28 2(3) . . . . ?
N26B C19 C17 C16 -117(2) . . . . ?
N4 C19 C17 C16 58.7(3) . . . . ?
C26A C19 C17 C16 -121(3) . . . . ?
N26B C19 C17 C18 127(2) . . . . ?
N4 C19 C17 C18 -57.2(3) . . . . ?
C26A C19 C17 C18 123(3) . . . . ?
O3 N2 C23 N12 1.2(4) . . . . ?
Co1 N2 C23 N12 -179.2(2) . . . . ?
O3 N2 C23 C22 -175.6(2) . . . . ?
Co1 N2 C23 C22 3.9(3) . . . . ?
C27 C22 C23 N2 176.7(2) . . . . ?
C20 C22 C23 N2 55.5(3) . . . . ?
C21 C22 C23 N2 -61.1(3) . . . . ?
C27 C22 C23 N12 -0.3(4) . . . . ?
C20 C22 C23 N12 -121.5(3) . . . . ?
C21 C22 C23 N12 121.9(3) . . . . ?
O8 N5 C16 N13 0.8(3) . . . . ?
Co1 N5 C16 N13 179.34(19) . . . . ?
O8 N5 C16 C17 177.6(2) . . . . ?
Co1 N5 C16 C17 -3.9(3) . . . . ?
C28 C17 C16 N5 -176.9(2) . . . . ?
C18 C17 C16 N5 59.9(3) . . . . ?
C19 C17 C16 N5 -56.0(3) . . . . ?
C28 C17 C16 N13 0.0(3) . . . . ?
C18 C17 C16 N13 -123.2(3) . . . . ?
C19 C17 C16 N13 120.9(3) . . . . ?
O10 N7 C21 N15 0.8(4) . . . . ?
Co1 N7 C21 N15 173.5(2) . . . . ?
O10 N7 C21 C22 -176.6(2) . . . . ?
Co1 N7 C21 C22 -3.9(3) . . . . ?
C27 C22 C21 N7 -176.9(2) . . . . ?
C20 C22 C21 N7 -55.3(3) . . . . ?
C23 C22 C21 N7 60.6(3) . . . . ?
C27 C22 C21 N15 5.6(4) . . . . ?
C20 C22 C21 N15 127.2(3) . . . . ?
C23 C22 C21 N15 -116.9(3) . . . . ?
O11 N6 C18 N14 7.1(4) . . . . ?
Co1 N6 C18 N14 -179.7(2) . . . . ?
O11 N6 C18 C17 -173.7(2) . . . . ?
Co1 N6 C18 C17 -0.5(3) . . . . ?
C28 C17 C18 N6 178.3(2) . . . . ?
C16 C17 C18 N6 -57.4(3) . . . . ?
C19 C17 C18 N6 57.6(3) . . . . ?
C28 C17 C18 N14 -2.5(4) . . . . ?
C16 C17 C18 N14 121.8(3) . . . . ?
C19 C17 C18 N14 -123.2(3) . . . . ?
F33 C30 C29 O32 -27.5(5) . . . . ?
F34 C30 C29 O32 -151.2(3) . . . . ?
F35 C30 C29 O32 91.0(3) . . . . ?
F33 C30 C29 O31 154.0(3) . . . . ?
F34 C30 C29 O31 30.3(4) . . . . ?
F35 C30 C29 O31 -87.5(3) . . . . ?
O38 C36 C37 F38A 164.0(11) . . . . ?
O39 C36 C37 F38A -15.8(11) . . . . ?
O38 C36 C37 F37A -72.1(13) . . . . ?
O39 C36 C37 F37A 108.0(13) . . . . ?
O38 C36 C37 F38 -173.7(7) . . . . ?
O39 C36 C37 F38 6.4(8) . . . . ?
O38 C36 C37 F37 -55.8(9) . . . . ?
O39 C36 C37 F37 124.4(9) . . . . ?
O38 C36 C37 F36A 42.6(9) . . . . ?
O39 C36 C37 F36A -137.3(9) . . . . ?
O38 C36 C37 F36 66.6(6) . . . . ?
O39 C36 C37 F36 -113.2(6) . . . . ?
Co1 N2 O3 Co1 -158.06(9) . . 2_666 2_666 ?

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
O8 H8 O3 0.77(3) 1.98(3) 2.725(3) 162(4) .
O10 H10 O11 0.79(3) 1.80(3) 2.585(3) 169(3) .

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.067