data_global
#=============================================================================

_audit_creation_method            SHELXL-97
_audit_creation_date              '13 February 2006'

#==========================================================================

# PROCESSING SUMMARY  (IUCr Office Use Only)

_journal_date_recd_electronic      ?
_journal_date_to_coeditor         ?
_journal_date_from_coeditor       ?
_journal_date_accepted     ?
_journal_date_printers_first      ?
_journal_date_printers_final      ?
_journal_date_proofs_out          ?
_journal_date_proofs_in           ?
_journal_coeditor_name            ?
_journal_coeditor_code      ?
_journal_paper_category      ?
_journal_coeditor_notes
; ?
;
_journal_techeditor_code      ?
_iucr_compatibility_tag          ACTA95
_journal_techeditor_notes
; ?
;
_journal_coden_ASTM               ?
_journal_name_full                ?
_journal_year                     ?
_journal_volume                   ?
_journal_issue                    ?
_journal_page_first               ?
_journal_page_last                ?
_journal_suppl_publ_number        ?
_journal_suppl_publ_pages         ?

#==========================================================================

# SUBMISSION DETAILS

_publ_contact_letter
;
Date of submission:  2000-10-23

Please consider this CIF submission for publication in Acta Cryst.,
Section E.  All authors have seen and approved this submission.

The CIF has passed the Chester CHECKCIF routines and gives a
satisfactory PRINTCIF file.

Best wishes,
 Lee Daniels
;

_publ_contact_author_name  'Lee Daniels' 
_publ_contact_author_address     
; 
Rigaku Americas Corp.
9009 New Trails Dr.
The Woodlands, TX 77381
U.S.A.
;

_publ_contact_author_phone  1-281-362-2300
_publ_contact_author_fax   1-281-364-3628
_publ_contact_author_email  ldaniels@Rigaku.com
_publ_requested_journal        'Acta Crystallographica E'
_publ_requested_category     EI

#=============================================================================
# 3. TITLE AND AUTHOR LIST

_publ_section_title
; 
Redetermination of bis(l-phenyl-2-amino-l,3-dihydroxypropano)ethylenediamino
cobalt(III) iodide water solvate
;

loop_
  _publ_author_name
  _publ_author_address

   'Benson, Ronald E.'
; Rigaku Americas Corporation,
  9009 New Trails Dr.,
  The Woodlands, TX 77381
  U.S.A.
;

  'Clearfield, Abraham'
; Department of Chemistry,
  PO Box 30012,
  Texas A&M University,
  College Station, TX 77842-3012
  U.S.A.
;

  'Daniels, Lee M.'
; Rigaku Americas Corporation,
  9009 New Trails Dr.,
  The Woodlands, TX 77381
  U.S.A.
; 

  'Wardeska, Jeff G.'
; Department of Chemistry,
  P.O. Box 70695,
  East Tennessee State University,
  Johnson City, TN 37614-0695
  U.S.A.
;
#=============================================================================

# 4. TEXT

_publ_section_abstract
;
New data for the title complex, C~20~H~32~CoN~4~O~4~, I, H~2~O, allows the
modelling of previously unresolved disorder in the ethylenediamine ligand
coordinated to the octahedral cation.
;

#=============================================================================

_publ_section_comment
; 
The title complex (I) was synthesized and crystallized in about 1978, and
published the following year as part of a synthetic and spectroscopic
project (Wardeska et al., 1979).
Crystals of this obviously robust material were recently rediscovered in
perfect condition after 28 years in a glass vial and its structure has
been redetermined in order to resolve some disorder in the earlier
determination.
While the structure in the original report gave very good residuals, the 
disorder in the ethylenediamine ligand was not resolved and the determination
of the absolute structure was based only on a comparison of the R values 
given by the correct versus the inverted structure.
We also take this opportunity to present the first published structure from
data collected on a new type of single-crystal diffraction instrument, the 
Rigaku SCXmini benchtop crystallography system. This structure was used as a 
test of the efficacy of this new paradigm for crystallographic 
instrumentation.

As shown in Fig. 1, there are two distinct conformations of the 
NH~2~-CH~2~-CH~2~-NH~2~ ligand.  The occupancy of the major orientation 
(specified by the letter A) refined to 0.66(1).

The molecular structure of the cation, Table 1, and H bonding scheme, Table 2,
involving all components of the unit cell contents, are, of course, similar to
that originally described, although in the present structure the positions of 
the O-bound H atoms were fully refined.
;

_publ_section_exptl_prep
; 
The compound was synthesized from a methanol/water solution of 
(1S,2S)-(+)-1-phenyl-2-amino-1,3-dihydroxypropane to which was added
sodium hexanitrocobaltate(III). The resulting solids were dissolved in 
a 2:1 methanol/water solution and treated with ethylenediamine, warmed
and filtered, then converted to the iodide salt by 
recrystallizing twice from potassium iodide solution.
The complete experimental preparation is described in 
Wardeska et al. (1979).
;


_publ_section_exptl_refinement
;
The positions of H atoms bonded to O were fully refined; all other H atoms 
were used in idealized positions with C-H = 0.98 \%A (methine), 0.93 \%A 
(phenyl), 0.97 \%A (methylene), and N-H = 0.90 \%A. U(H) was set to 1.2 times 
that of the attached atom for C and N, and 1.5 times for O. For the disordered
group, only the positions of the two C atoms were split; the N positions were 
not distinct enough to allow modelling over two positions. 
The isotropic displacement parameters for disordered atoms C7A and C7B were 
constrained to be equal, as were those for C8A and C8B.
The error in the C-C distance introduced by the disorder is greatly reduced 
in this resolved model as compared to that in the earlier report.  When these
disordered C atoms are not resolved and they are allowed to refine 
anisotropically, the resulting apparent C-C distance is 1.395(10) 
(Wardeska et al., 1979).  
The present refinement allows for two separate positions for this C-C group,
and the distances refine to 1.506(6) for the A group and 1.497(10) for the
lower-occupancy B group (i.e. statistically indistinguishable at the 
2\s level).
;

_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M., 
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435-436.

Flack, H. D. (1983).  Acta Cryst. A39, 876--881.

Higashi, T. (1995). ABSCOR: Empirical Absorption Correction based on 
Fourier Series Approximation. Rigaku Corporation, 3-9-12 Matsubara, Akishima,
Tokyo 196-8666, JAPAN.

Rigaku (1998). Process-Auto: Automatic Data Acquisition and Processing
Package for Imaging Plate and CCD Diffractometers. Rigaku Corporation, 
3-9-12 Matsubara, Akishima, Tokyo 196-8666, JAPAN.

Rigaku (2005). CrystalStructure: Structure Solution and
Refinement program, Version 3.7. Rigaku Americas Corp., 9009 New Trails Drive, 
The Woodlands, TX 77381-5209, USA.

Rigaku (2006). SCXmini Benchtop Crystallography System software, 
Version 1.0. Rigaku Americas Corp., 9009 New Trails Drive, The Woodlands,
TX 77381-5209, USA.

Sheldrick, G. M. (1997) SHELXL97. University of G\"ottingen, Germany.

Wardeska, J. G., Clearfield, A. & Troup, J. M. (1979). Inorg. Chem. 18, 
1641--1648.
;

_publ_section_figure_captions
;
Figure 1
View of the cation in (I). The atoms and bonds in 
the minor orientation of the disordered ethylenediamine ligand are shown
with dashed lines.
;

_publ_section_table_legends
; 
;

_publ_section_acknowledgements
; 
;

data_enpaco10

_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_formula_moiety          'C20 H32 Co N4 O4, I, H2 O'
_chemical_formula_sum             'C20 H34 Co I N4 O5' 
_chemical_formula_weight          596.34
_chemical_absolute_configuration  ad

loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Co'  'Co'   0.3494   0.9721 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'I'  'I'  -0.4742   1.8119 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            orthorhombic
_symmetry_space_group_name_H-M    'P 21 21 21'
_symmetry_space_group_name_Hall   'P 21 21 21'
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'x+1/2, -y+1/2, -z' 
 '-x, y+1/2, -z+1/2' 
 '-x+1/2, -y, z+1/2' 
 
_cell_length_a                    6.7895(2) 
_cell_length_b                    14.5013(4) 
_cell_length_c                    24.8565(8) 
_cell_angle_alpha                 90
_cell_angle_beta                  90 
_cell_angle_gamma                 90 
_cell_volume                      2447.29(13) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     294(2) 
_cell_measurement_reflns_used     19448
_cell_measurement_theta_min       3.0
_cell_measurement_theta_max       27.5
 
_exptl_crystal_description        prism
_exptl_crystal_colour             'translucent pale-brown'
_exptl_crystal_size_max           0.42 
_exptl_crystal_size_mid           0.39 
_exptl_crystal_size_min           0.28 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.619 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1208 
_exptl_absorpt_coefficient_mu     1.999 
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.466
_exptl_absorpt_correction_T_max   0.57 
_exptl_absorpt_process_details    'ABSCOR (Higashi, 1995)'
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       294(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'long-fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Rigaku SCXmini'
_diffrn_measurement_method        \w-scans
_diffrn_detector_area_resol_mean  6.85
_diffrn_standards_number          0
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   0
_diffrn_standards_decay_%         <0.2
_diffrn_reflns_number             19627 
_diffrn_reflns_av_R_equivalents   0.029 
_diffrn_reflns_av_sigmaI/netI     0.027 
_diffrn_reflns_limit_h_min        -8 
_diffrn_reflns_limit_h_max        8 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        18 
_diffrn_reflns_limit_l_min        -30 
_diffrn_reflns_limit_l_max        32 
_diffrn_reflns_theta_min          3.1 
_diffrn_reflns_theta_max          27.5 
_reflns_number_total              5482 
_reflns_number_gt                 5172 
_reflns_threshold_expression      'I>2\s(I)' 
 
_computing_data_collection        'SCXmini (Rigaku, 2006)'
_computing_cell_refinement        'Process-Auto (Rigaku, 1998)'
_computing_data_reduction         'Process-Auto'
_computing_structure_solution     'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'CrystalStructure V3.7 (Rigaku, 2005)'
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)' 
 
_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^)+(0.022P)^2^+P] 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_abs_structure_details 
 '(Flack, 1983)' 
_refine_ls_abs_structure_Flack    0.007(14) 
_refine_ls_number_reflns          5482 
_refine_ls_number_parameters      291 
_refine_ls_number_restraints      215 
_refine_ls_R_factor_all           0.030 
_refine_ls_R_factor_gt            0.027 
_refine_ls_wR_factor_ref          0.062 
_refine_ls_wR_factor_gt           0.061 
_refine_ls_goodness_of_fit_ref    1.10
_refine_ls_restrained_S_all       1.08 
_refine_ls_shift/su_max           0.003 
_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 
I1 I 0.24806(3) 1.289623(13) 0.701876(8) 0.05308(7) Uani 1 1 d . . . 
Co1 Co 0.21430(5) 0.93696(2) 0.673829(13) 0.02590(7) Uani 1 1 d . . . 
O4 O 0.8157(3) 1.08284(14) 0.62835(8) 0.0383(4) Uani 1 1 d DU . . 
H4 H 0.930(3) 1.062(2) 0.6145(12) 0.042(8) Uiso 1 1 d D . . 
O5 O 0.6808(5) 1.1481(2) 0.72736(12) 0.0804(9) Uani 1 1 d D . . 
H2W H 0.739(7) 1.151(4) 0.6947(11) 0.121 Uiso 1 1 d D . . 
H1W H 0.571(5) 1.175(3) 0.740(2) 0.121 Uiso 1 1 d D . . 
O1 O 0.3046(2) 0.83092(11) 0.63805(7) 0.0294(4) Uani 1 1 d U A . 
O3 O -0.3187(3) 0.81759(15) 0.60232(9) 0.0474(5) Uani 1 1 d DU A . 
H3 H -0.441(3) 0.809(3) 0.6175(14) 0.071 Uiso 1 1 d D . . 
O2 O 0.1432(2) 0.99710(12) 0.60874(7) 0.0301(4) Uani 1 1 d U A . 
N1A N 0.2831(3) 0.88261(14) 0.74411(8) 0.0357(5) Uani 0.657(6) 1 d PU A 1 
H1A1 H 0.1910 0.8413 0.7540 0.043 Uiso 0.657(6) 1 calc PR A 1 
H1A2 H 0.3999 0.8535 0.7419 0.043 Uiso 0.657(6) 1 calc PR A 1 
N3A N 0.1217(3) 1.04309(15) 0.71760(9) 0.0369(5) Uani 0.657(6) 1 d PU A 1 
H3A1 H 0.2014 1.0917 0.7119 0.044 Uiso 0.657(6) 1 calc PR A 1 
H3A2 H -0.0006 1.0589 0.7072 0.044 Uiso 0.657(6) 1 calc PR A 1 
N1B N 0.2831(3) 0.88261(14) 0.74411(8) 0.0357(5) Uani 0.343(6) 1 d PU A 2 
H1B1 H 0.2280 0.8263 0.7463 0.043 Uiso 0.343(6) 1 calc PR A 2 
H1B2 H 0.4146 0.8751 0.7455 0.043 Uiso 0.343(6) 1 calc PR A 2 
N3B N 0.1217(3) 1.04309(15) 0.71760(9) 0.0369(5) Uani 0.343(6) 1 d PU A 2 
H3B1 H 0.1555 1.0966 0.7017 0.044 Uiso 0.343(6) 1 calc PR A 2 
H3B2 H -0.0101 1.0415 0.7211 0.044 Uiso 0.343(6) 1 calc PR A 2 
N2 N -0.0417(3) 0.87671(13) 0.67324(9) 0.0286(4) Uani 1 1 d U A . 
H2A H -0.0911 0.8754 0.7068 0.034 Uiso 1 1 calc R . . 
H2B H -0.1254 0.9089 0.6523 0.034 Uiso 1 1 calc R . . 
N4 N 0.4763(3) 0.98935(14) 0.66224(8) 0.0282(4) Uani 1 1 d U A . 
H4A H 0.5135 1.0216 0.6915 0.034 Uiso 1 1 calc R . . 
H4B H 0.5641 0.9438 0.6570 0.034 Uiso 1 1 calc R . . 
C1 C 0.1466(3) 0.78521(18) 0.61191(10) 0.0288(5) Uani 1 1 d U . . 
H1 H 0.1054 0.8216 0.5806 0.035 Uiso 1 1 calc R A . 
C2 C -0.0230(3) 0.78085(17) 0.65230(11) 0.0293(5) Uani 1 1 d U A . 
H2 H 0.0169 0.7408 0.6821 0.035 Uiso 1 1 calc R . . 
C15 C 0.2218(4) 0.69206(16) 0.59293(10) 0.0312(5) Uani 1 1 d U A . 
C16 C 0.2528(5) 0.61960(17) 0.62874(11) 0.0431(6) Uani 1 1 d U . . 
H16 H 0.2211 0.6266 0.6649 0.052 Uiso 1 1 calc R A . 
C17 C 0.3307(5) 0.5371(2) 0.61045(15) 0.0540(9) Uani 1 1 d U A . 
H17 H 0.3467 0.4882 0.6343 0.065 Uiso 1 1 calc R . . 
C18 C 0.3844(5) 0.5268(2) 0.55766(15) 0.0560(9) Uani 1 1 d U . . 
H18 H 0.4380 0.4713 0.5458 0.067 Uiso 1 1 calc R A . 
C19 C 0.3591(6) 0.5977(2) 0.52268(15) 0.0568(9) Uani 1 1 d U A . 
H19 H 0.3981 0.5909 0.4870 0.068 Uiso 1 1 calc R . . 
C20 C 0.2757(5) 0.67989(19) 0.53957(11) 0.0453(7) Uani 1 1 d U . . 
H20 H 0.2558 0.7273 0.5150 0.054 Uiso 1 1 calc R A . 
C5 C 0.4717(3) 1.05122(18) 0.61421(10) 0.0271(5) Uani 1 1 d U . . 
H5 H 0.4302 1.1130 0.6255 0.033 Uiso 1 1 calc R A . 
C3 C -0.2219(4) 0.74665(18) 0.63105(12) 0.0403(6) Uani 1 1 d U . . 
H3A H -0.2014 0.6941 0.6076 0.048 Uiso 1 1 calc R A . 
H3B H -0.3036 0.7270 0.6609 0.048 Uiso 1 1 calc R . . 
C9 C 0.2787(4) 1.07077(16) 0.52822(9) 0.0294(5) Uani 1 1 d U . . 
C14 C 0.1607(4) 1.14859(19) 0.52991(12) 0.0371(6) Uani 1 1 d U A . 
H14 H 0.0962 1.1642 0.5616 0.045 Uiso 1 1 calc R . . 
C13 C 0.1378(4) 1.2035(2) 0.48459(14) 0.0465(7) Uani 1 1 d U . . 
H13 H 0.0554 1.2547 0.4859 0.056 Uiso 1 1 calc R A . 
C12 C 0.2360(5) 1.1829(2) 0.43779(12) 0.0512(8) Uani 1 1 d U A . 
H12 H 0.2208 1.2201 0.4076 0.061 Uiso 1 1 calc R . . 
C11 C 0.3566(5) 1.1070(2) 0.43583(12) 0.0500(8) Uani 1 1 d U . . 
H11 H 0.4257 1.0937 0.4045 0.060 Uiso 1 1 calc R A . 
C10 C 0.3762(4) 1.0500(2) 0.48032(11) 0.0404(6) Uani 1 1 d U A . 
H10 H 0.4548 0.9976 0.4782 0.048 Uiso 1 1 calc R . . 
C6 C 0.6744(3) 1.05765(19) 0.58866(10) 0.0317(5) Uani 1 1 d U A . 
H6A H 0.7098 0.9987 0.5730 0.038 Uiso 1 1 calc R . . 
H6B H 0.6729 1.1034 0.5602 0.038 Uiso 1 1 calc R . . 
C4 C 0.3141(3) 1.01045(16) 0.57716(10) 0.0279(5) Uani 1 1 d U A . 
H4C H 0.3600 0.9500 0.5647 0.034 Uiso 1 1 calc R . . 
C7A C 0.2942(8) 0.9589(3) 0.78466(19) 0.0429(10) Uiso 0.657(6) 1 d PDU A 1 
H7A1 H 0.4162 0.9929 0.7806 0.051 Uiso 0.657(6) 1 calc PR A 1 
H7A2 H 0.2886 0.9340 0.8209 0.051 Uiso 0.657(6) 1 calc PR A 1 
C8A C 0.1202(9) 1.0209(4) 0.77437(19) 0.0448(10) Uiso 0.657(6) 1 d PDU A 1 
H8A1 H -0.0013 0.9897 0.7839 0.054 Uiso 0.657(6) 1 calc PR A 1 
H8A2 H 0.1307 1.0766 0.7957 0.054 Uiso 0.657(6) 1 calc PR A 1 
C7B C 0.2222(16) 0.9357(6) 0.7904(3) 0.0429(10) Uiso 0.343(6) 1 d PDU A 2 
H7B1 H 0.3118 0.9252 0.8201 0.051 Uiso 0.343(6) 1 calc PR A 2 
H7B2 H 0.0909 0.9175 0.8015 0.051 Uiso 0.343(6) 1 calc PR A 2 
C8B C 0.2241(19) 1.0347(5) 0.7749(3) 0.0448(10) Uiso 0.343(6) 1 d PDU A 2 
H8B1 H 0.3585 1.0573 0.7731 0.054 Uiso 0.343(6) 1 calc PR A 2 
H8B2 H 0.1528 1.0711 0.8012 0.054 Uiso 0.343(6) 1 calc PR A 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 
I1 0.05905(14) 0.04394(11) 0.05623(12) -0.00782(8) 0.01004(12) -0.00603(12) 
Co1 0.02083(15) 0.02368(14) 0.03319(15) 0.00319(12) 0.00077(13) 0.00013(13) 
O4 0.0212(9) 0.0493(11) 0.0442(11) 0.0009(9) -0.0001(8) -0.0008(8) 
O5 0.071(2) 0.102(2) 0.0673(18) -0.0235(17) 0.0020(15) 0.0044(17) 
O1 0.0201(9) 0.0284(8) 0.0397(9) -0.0011(7) 0.0017(7) 0.0000(7) 
O3 0.0312(11) 0.0498(12) 0.0613(13) 0.0091(10) -0.0030(10) -0.0049(9) 
O2 0.0182(8) 0.0349(10) 0.0374(10) 0.0081(8) -0.0008(7) -0.0007(7) 
N1A 0.0300(12) 0.0387(11) 0.0383(11) 0.0069(9) 0.0025(10) -0.0002(11) 
N3A 0.0307(12) 0.0318(12) 0.0481(14) 0.0005(10) 0.0028(10) 0.0000(9) 
N1B 0.0300(12) 0.0387(11) 0.0383(11) 0.0069(9) 0.0025(10) -0.0002(11) 
N3B 0.0307(12) 0.0318(12) 0.0481(14) 0.0005(10) 0.0028(10) 0.0000(9) 
N2 0.0212(10) 0.0273(10) 0.0375(11) 0.0019(9) 0.0039(9) 0.0016(8) 
N4 0.0236(10) 0.0272(10) 0.0337(11) 0.0036(9) -0.0006(8) -0.0013(8) 
C1 0.0241(12) 0.0294(12) 0.0328(13) 0.0054(11) 0.0012(10) -0.0006(11) 
C2 0.0235(12) 0.0246(11) 0.0397(14) 0.0022(11) 0.0006(10) 0.0001(10) 
C15 0.0246(12) 0.0334(11) 0.0357(12) -0.0017(9) 0.0001(11) -0.0017(11) 
C16 0.0481(17) 0.0389(13) 0.0422(14) 0.0038(11) 0.0066(16) 0.0119(16) 
C17 0.056(2) 0.0372(16) 0.069(2) 0.0037(15) 0.0014(16) 0.0143(14) 
C18 0.0459(19) 0.0424(17) 0.080(3) -0.0226(18) 0.0101(17) 0.0035(15) 
C19 0.063(2) 0.059(2) 0.0489(19) -0.0207(16) 0.0134(16) -0.0081(17) 
C20 0.0544(19) 0.0433(14) 0.0380(14) -0.0040(11) 0.0038(15) -0.0080(16) 
C5 0.0192(11) 0.0264(12) 0.0358(13) 0.0054(11) 0.0016(9) 0.0003(10) 
C3 0.0271(14) 0.0319(12) 0.0619(17) 0.0002(12) 0.0009(14) -0.0030(12) 
C9 0.0228(11) 0.0331(11) 0.0325(11) 0.0023(9) -0.0034(10) -0.0017(12) 
C14 0.0344(14) 0.0350(14) 0.0420(15) 0.0076(12) 0.0035(12) 0.0013(11) 
C13 0.0398(16) 0.0389(16) 0.061(2) 0.0165(15) -0.0013(14) 0.0048(14) 
C12 0.053(2) 0.0556(17) 0.0450(16) 0.0191(13) -0.0038(16) 0.0007(18) 
C11 0.0536(19) 0.065(2) 0.0309(15) 0.0038(14) 0.0015(13) 0.0033(17) 
C10 0.0395(15) 0.0459(16) 0.0356(14) -0.0006(13) -0.0034(12) 0.0052(13) 
C6 0.0227(12) 0.0356(13) 0.0367(14) 0.0055(11) 0.0016(10) -0.0001(11) 
C4 0.0204(12) 0.0270(11) 0.0364(13) 0.0022(10) 0.0007(10) 0.0007(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 
Co1 O1 1.8793(17) . y 
Co1 O2 1.9002(18) . y 
Co1 N2 1.9456(19) . y 
Co1 N4 1.955(2) . y 
Co1 N1A 1.973(2) . y 
Co1 N3A 1.987(2) . y 
O4 C6 1.424(3) . y 
O4 H4 0.899(17) . y 
O5 H2W 0.91(2) . y 
O5 H1W 0.90(3) . y 
O1 C1 1.419(3) . y 
O3 C3 1.414(3) . y 
O3 H3 0.919(18) . y 
O2 C4 1.415(3) . y 
N1A C7A 1.498(5) . y 
N1A H1A1 0.9000 . ? 
N1A H1A2 0.9000 . ? 
N3A C8A 1.448(5) . y 
N3A H3A1 0.9000 . ? 
N3A H3A2 0.9000 . ? 
N2 C2 1.490(3) . y 
N2 H2A 0.9000 . ? 
N2 H2B 0.9000 . ? 
N4 C5 1.494(3) . y 
N4 H4A 0.9000 . ? 
N4 H4B 0.9000 . ? 
C1 C15 1.519(3) . y 
C1 C2 1.529(3) . y 
C1 H1 0.9800 . ? 
C2 C3 1.532(4) . y 
C2 H2 0.9800 . ? 
C15 C20 1.387(4) . y 
C15 C16 1.393(3) . y 
C16 C17 1.385(4) . y 
C16 H16 0.9300 . ? 
C17 C18 1.370(5) . y 
C17 H17 0.9300 . ? 
C18 C19 1.357(5) . y 
C18 H18 0.9300 . ? 
C19 C20 1.385(4) . y 
C19 H19 0.9300 . ? 
C20 H20 0.9300 . ? 
C5 C6 1.519(3) . y 
C5 C4 1.531(3) . y 
C5 H5 0.9800 . ? 
C3 H3A 0.9700 . ? 
C3 H3B 0.9700 . ? 
C9 C14 1.384(4) . y 
C9 C10 1.395(4) . y 
C9 C4 1.517(3) . y 
C14 C13 1.389(4) . y 
C14 H14 0.9300 . ? 
C13 C12 1.374(4) . y 
C13 H13 0.9300 . ? 
C12 C11 1.373(4) . y 
C12 H12 0.9300 . ? 
C11 C10 1.387(4) . y 
C11 H11 0.9300 . ? 
C10 H10 0.9300 . ? 
C6 H6A 0.9700 . ? 
C6 H6B 0.9700 . ? 
C4 H4C 0.9800 . ? 
C7A C8A 1.506(6) . y 
C7A H7A1 0.9700 . ? 
C7A H7A2 0.9700 . ? 
C8A H8A1 0.9700 . ? 
C8A H8A2 0.9700 . ? 
C7B C8B 1.487(10) . y 
C7B H7B1 0.9700 . ? 
C7B H7B2 0.9700 . ? 
C8B H8B1 0.9700 . ? 
C8B H8B2 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 O2 93.18(8) . . y 
O1 Co1 N2 85.45(8) . . y 
O2 Co1 N2 88.43(8) . . y 
O1 Co1 N4 87.21(8) . . y 
O2 Co1 N4 85.83(8) . . y 
N2 Co1 N4 170.41(9) . . y 
O1 Co1 N1A 90.85(8) . . y 
O2 Co1 N1A 175.95(9) . . y 
N2 Co1 N1A 92.23(10) . . y 
N4 Co1 N1A 94.03(9) . . y 
O1 Co1 N3A 175.03(9) . . y 
O2 Co1 N3A 91.74(9) . . y 
N2 Co1 N3A 93.98(9) . . y 
N4 Co1 N3A 93.87(9) . . y 
N1A Co1 N3A 84.23(9) . . y 
C6 O4 H4 103(2) . . y 
H2W O5 H1W 131(5) . . y 
C1 O1 Co1 110.63(14) . . y 
C3 O3 H3 96(2) . . y 
C4 O2 Co1 109.08(14) . . y 
C7A N1A Co1 108.2(2) . . y 
C7A N1A H1A1 110.1 . . ? 
Co1 N1A H1A1 110.1 . . ? 
C7A N1A H1A2 110.1 . . ? 
Co1 N1A H1A2 110.1 . . ? 
H1A1 N1A H1A2 108.4 . . ? 
C8A N3A Co1 111.3(2) . . y 
C8A N3A H3A1 109.4 . . ? 
Co1 N3A H3A1 109.4 . . ? 
C8A N3A H3A2 109.4 . . ? 
Co1 N3A H3A2 109.4 . . ? 
H3A1 N3A H3A2 108.0 . . ? 
C2 N2 Co1 110.22(14) . . y 
C2 N2 H2A 109.6 . . ? 
Co1 N2 H2A 109.6 . . ? 
C2 N2 H2B 109.6 . . ? 
Co1 N2 H2B 109.6 . . ? 
H2A N2 H2B 108.1 . . ? 
C5 N4 Co1 109.41(14) . . y 
C5 N4 H4A 109.8 . . ? 
Co1 N4 H4A 109.8 . . ? 
C5 N4 H4B 109.8 . . ? 
Co1 N4 H4B 109.8 . . ? 
H4A N4 H4B 108.2 . . ? 
O1 C1 C15 107.69(19) . . ?
O1 C1 C2 106.8(2) . . ? 
C15 C1 C2 114.8(2) . . ? 
O1 C1 H1 109.1 . . ? 
C15 C1 H1 109.1 . . ? 
C2 C1 H1 109.1 . . ? 
N2 C2 C1 104.8(2) . . ? 
N2 C2 C3 110.3(2) . . ? 
C1 C2 C3 116.8(2) . . ? 
N2 C2 H2 108.2 . . ? 
C1 C2 H2 108.2 . . ? 
C3 C2 H2 108.2 . . ? 
C20 C15 C16 118.4(2) . . ? 
C20 C15 C1 119.9(2) . . ? 
C16 C15 C1 121.5(2) . . ? 
C17 C16 C15 120.0(3) . . ? 
C17 C16 H16 120.0 . . ? 
C15 C16 H16 120.0 . . ? 
C18 C17 C16 120.7(3) . . ? 
C18 C17 H17 119.6 . . ? 
C16 C17 H17 119.6 . . ? 
C19 C18 C17 119.8(3) . . ? 
C19 C18 H18 120.1 . . ? 
C17 C18 H18 120.1 . . ? 
C18 C19 C20 120.6(3) . . ? 
C18 C19 H19 119.7 . . ? 
C20 C19 H19 119.7 . . ? 
C19 C20 C15 120.5(3) . . ? 
C19 C20 H20 119.8 . . ? 
C15 C20 H20 119.8 . . ? 
N4 C5 C6 110.6(2) . . ? 
N4 C5 C4 105.27(19) . . ? 
C6 C5 C4 113.9(2) . . ? 
N4 C5 H5 109.0 . . ? 
C6 C5 H5 109.0 . . ? 
C4 C5 H5 109.0 . . ? 
O3 C3 C2 110.4(2) . . ? 
O3 C3 H3A 109.6 . . ? 
C2 C3 H3A 109.6 . . ? 
O3 C3 H3B 109.6 . . ? 
C2 C3 H3B 109.6 . . ? 
H3A C3 H3B 108.1 . . ? 
C14 C9 C10 118.4(2) . . ? 
C14 C9 C4 122.5(2) . . ? 
C10 C9 C4 119.0(2) . . ? 
C9 C14 C13 120.5(3) . . ? 
C9 C14 H14 119.7 . . ? 
C13 C14 H14 119.7 . . ? 
C12 C13 C14 120.5(3) . . ? 
C12 C13 H13 119.7 . . ? 
C14 C13 H13 119.7 . . ? 
C11 C12 C13 119.6(3) . . ? 
C11 C12 H12 120.2 . . ? 
C13 C12 H12 120.2 . . ? 
C12 C11 C10 120.4(3) . . ? 
C12 C11 H11 119.8 . . ? 
C10 C11 H11 119.8 . . ? 
C11 C10 C9 120.4(3) . . ? 
C11 C10 H10 119.8 . . ? 
C9 C10 H10 119.8 . . ? 
O4 C6 C5 109.7(2) . . ? 
O4 C6 H6A 109.7 . . ? 
C5 C6 H6A 109.7 . . ? 
O4 C6 H6B 109.7 . . ? 
C5 C6 H6B 109.7 . . ? 
H6A C6 H6B 108.2 . . ? 
O2 C4 C9 113.18(19) . . ? 
O2 C4 C5 107.0(2) . . ? 
C9 C4 C5 111.8(2) . . ? 
O2 C4 H4C 108.3 . . ? 
C9 C4 H4C 108.3 . . ? 
C5 C4 H4C 108.3 . . ? 
N1A C7A C8A 106.7(4) . . ? 
N1A C7A H7A1 110.4 . . ? 
C8A C7A H7A1 110.4 . . ? 
N1A C7A H7A2 110.4 . . ? 
C8A C7A H7A2 110.4 . . ? 
H7A1 C7A H7A2 108.6 . . ? 
N3A C8A C7A 107.0(4) . . ? 
N3A C8A H8A1 110.3 . . ? 
C7A C8A H8A1 110.3 . . ? 
N3A C8A H8A2 110.3 . . ? 
C7A C8A H8A2 110.3 . . ? 
H8A1 C8A H8A2 108.6 . . ? 
C8B C7B H7B1 110.1 . . ? 
C8B C7B H7B2 110.1 . . ? 
H7B1 C7B H7B2 108.5 . . ? 
C7B C8B H8B1 110.2 . . ? 
C7B C8B H8B2 110.2 . . ? 
H8B1 C8B H8B2 108.5 . . ? 
 
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 
O4 H4 O2  0.899(17) 1.73(2) 2.594(2) 159(3) 1_655 
O5 H2W O4  0.906(19) 1.99(3) 2.792(3) 146(5) . 
O5 H1W I1  0.90(3) 2.91(4) 3.639(3) 140(5) . 
O3 H3 O1  0.919(18) 1.83(2) 2.714(3) 160(4) 1_455 
N1A H1A1 I1  0.90 3.26 4.078(2) 152 3_546 
N1A H1A2 I1  0.90 2.92 3.709(2) 147 3_646 
N3A H3A1 I1  0.90 2.90 3.697(2) 149 . 
N3A H3A2 O4  0.90 2.35 3.094(3) 140 1_455 
N3A H3A2 O5  0.90 2.57 3.368(4) 148 1_455 
N1B H1B2 I1  0.90 2.91 3.709(2) 148 3_646 
N3B H3B1 I1  0.90 2.87 3.697(2) 154 . 
N3B H3B2 O5  0.90 2.61 3.368(4) 142 1_455 
N3B H3B2 O4  0.90 2.66 3.094(3) 111 1_455 
N2 H2A I1  0.90 2.80 3.632(2) 155 3_546 
N4 H4A O5  0.90 2.34 3.139(4) 149 . 
N4 H4B O3  0.90 2.41 3.219(3) 149 1_655 
 
_diffrn_measured_fraction_theta_max    0.994 
_diffrn_reflns_theta_full              27.5 
_diffrn_measured_fraction_theta_full   0.994 
_refine_diff_density_max    0.58 
_refine_diff_density_min   -0.69 
_refine_diff_density_rms    0.054