# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Manuel Martinez'
_publ_contact_author_email       MANEL.MARTINEZ@QI.UB.ES

_publ_section_title              
;
Mechanistic Aspects of the Chemistry
of Mononuclear CrIII complexes with Pendant-arm Macrocyclic
Ligands and Formation of Discrete CrIII/FeII and CrIII/FeII/CoIII
Cyano-Bridged Mixed Valence Compounds.
;
loop_
_publ_author_name
'Manuel Martinez'
'Manuel Basallote'
'Paul V. Bernhardt'
'T. Calvet'
'Carmen E. Castillo'
;
M.Font-Bardia
;
'Carlos Rodriguez'

# Attachment 'newcif.cif'

# CIFs 736218 & 736219 Basalotte et al., Dalton

data_1334pb31
_database_code_depnum_ccdc_archive 'CCDC 736218'

_audit_creation_date             2009-06-25T16:37:39-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_formula_moiety         'C11 H30 Cl Cr N5 O,3(Cl O4),2(H2 O)'
_chemical_formula_sum            'C11 H34 Cl4 Cr N5 O15'
_chemical_formula_weight         670.23
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_Int_Tables_number      62
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   15.920(10)
_cell_length_b                   13.841(2)
_cell_length_c                   11.964(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2636.3(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    20
_cell_measurement_theta_min      11.21
_cell_measurement_theta_max      12.58
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1388
_exptl_special_details           
;
?
;

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.914
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   
;
A.C.T. North, D.C. Phillips, F.S. Mathews, Acta. Cryst. Sect A, 1968, 24, 351
;
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_T_max  0.9966

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       '\w-2\q scans'
_diffrn_standards_number         3
_diffrn_standards_interval_count 120
_diffrn_standards_decay_%        'less than 5%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_number            2419
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_full        24.96
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_reflns_number_total             2419
_reflns_number_gt                1930
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_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^)+(0.1243P)^2^+4.3240P] 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         2419
_refine_ls_number_parameters     226
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0636
_refine_ls_wR_factor_ref         0.1944
_refine_ls_wR_factor_gt          0.1798
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.117

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
Cr1 Cr 0.07624(6) 0.2500 0.22190(8) 0.0347(3) Uani 1 2 d S . .
Cl1 Cl 0.20280(11) 0.2500 0.31257(16) 0.0591(5) Uani 1 2 d S . .
N1 N 0.0304(3) 0.1409(3) 0.3195(3) 0.0526(10) Uani 1 1 d . . .
H1 H -0.0248 0.1339 0.3016 0.063 Uiso 1 1 calc R . .
N2 N 0.1202(2) 0.1410(2) 0.1197(3) 0.0415(8) Uani 1 1 d . . .
H2 H 0.1756 0.1331 0.1358 0.050 Uiso 1 1 d R . .
N3 N 0.1530(5) 0.2500 -0.1649(5) 0.0667(18) Uani 1 2 d S . .
H3A H 0.0992 0.2500 -0.1848 0.100 Uiso 1 2 d SR . .
H3B H 0.1780 0.1975 -0.1921 0.100 Uiso 1 1 d R . .
O1 O -0.0335(3) 0.2500 0.1412(4) 0.0446(10) Uani 1 2 d S . .
H11 H -0.0549 0.2064 0.1281 0.053 Uiso 1 1 d R . .
O2 O -0.1309(2) 0.1073(3) 0.0805(4) 0.0703(11) Uani 1 1 d . . .
H21 H -0.1467 0.1335 0.0149 0.084 Uiso 1 1 d R . .
H22 H -0.1770 0.0983 0.1227 0.084 Uiso 1 1 d R . .
C1 C -0.0092(6) 0.2500 0.4754(7) 0.086(3) Uani 1 2 d S . .
H1D H -0.0170 0.2500 0.5558 0.103 Uiso 1 2 d SR . .
H1E H -0.0644 0.2500 0.4411 0.103 Uiso 1 2 d SR . .
C2 C 0.0343(4) 0.1575(5) 0.4417(5) 0.0787(19) Uani 1 1 d . . .
H2A H 0.0926 0.1603 0.4649 0.094 Uiso 1 1 calc R . .
H2B H 0.0081 0.1036 0.4799 0.094 Uiso 1 1 calc R . .
C3 C 0.0742(3) 0.0501(4) 0.2829(5) 0.0605(14) Uani 1 1 d . . .
H3D H 0.0451 -0.0067 0.3106 0.073 Uiso 1 1 d R . .
H3E H 0.1310 0.0497 0.3123 0.073 Uiso 1 1 d R . .
C4 C 0.0765(3) 0.0508(3) 0.1566(5) 0.0559(13) Uani 1 1 d . . .
H4A H 0.1063 -0.0056 0.1294 0.067 Uiso 1 1 d R . .
H4B H 0.0198 0.0496 0.1272 0.067 Uiso 1 1 d R . .
C5 C 0.1148(3) 0.1566(3) -0.0020(4) 0.0464(11) Uani 1 1 d . . .
H5A H 0.0560 0.1606 -0.0229 0.056 Uiso 1 1 d R . .
H5B H 0.1393 0.1020 -0.0410 0.056 Uiso 1 1 d R . .
C6 C 0.1592(4) 0.2500 -0.0388(5) 0.0443(14) Uani 1 2 d S . .
C7 C 0.2513(4) 0.2500 -0.0089(6) 0.0562(17) Uani 1 2 d S . .
H7A H 0.2764 0.3095 -0.0333 0.084 Uiso 1 1 d R . .
H7B H 0.2576 0.2500 0.0705 0.084 Uiso 1 2 d SR . .
Cl2 Cl 0.31761(8) 0.52085(10) 0.16294(12) 0.0614(4) Uani 1 1 d D . .
O21A O 0.2715(6) 0.5587(8) 0.2531(8) 0.117(6) Uani 0.519(17) 1 d PD A 1
O22A O 0.3966(4) 0.5628(9) 0.1630(9) 0.096(5) Uani 0.519(17) 1 d PD A 1
O23A O 0.2760(8) 0.5396(10) 0.0642(7) 0.172(12) Uani 0.519(17) 1 d PD A 1
O24A O 0.3254(9) 0.4213(4) 0.1791(9) 0.117(6) Uani 0.519(17) 1 d PD A 1
O21B O 0.2705(8) 0.5053(15) 0.2593(9) 0.222(16) Uani 0.481(17) 1 d PD A 2
O22B O 0.3744(10) 0.4455(11) 0.1489(14) 0.264(19) Uani 0.481(17) 1 d PD A 2
O23B O 0.3606(11) 0.6075(8) 0.1721(14) 0.167(11) Uani 0.481(17) 1 d PD A 2
O24B O 0.2639(8) 0.5242(10) 0.0710(8) 0.112(7) Uani 0.481(17) 1 d PD A 2
Cl3 Cl -0.09377(12) 0.2500 -0.20037(15) 0.0556(5) Uani 1 2 d SD . .
O31A O -0.1382(11) 0.2500 -0.1020(10) 0.21(7) Uiso 0.391(8) 2 d SPD B 1
O32A O -0.0338(6) 0.1787(8) -0.2042(10) 0.092(4) Uiso 0.391(8) 1 d PD B 1
O33A O -0.1451(10) 0.2500 -0.2924(11) 0.127(8) Uiso 0.391(8) 2 d SPD B 1
O31B O -0.0088(5) 0.2500 -0.182(2) 0.37(4) Uiso 0.391(8) 2 d SPD B 2
O32B O -0.1184(10) 0.1790(10) -0.2738(10) 0.133(6) Uiso 0.391(8) 1 d PD B 2
O33B O -0.1397(13) 0.2500 -0.1034(11) 0.15(4) Uiso 0.391(8) 2 d SPD B 2
O31C O -0.0368(19) 0.2500 -0.287(2) 0.31(6) Uiso 0.218(17) 2 d SPD B 3
O32C O -0.0792(14) 0.1738(11) -0.1281(12) 0.093(10) Uiso 0.218(17) 1 d PD B 3
O33C O -0.1753(9) 0.2500 -0.239(3) 0.35(7) Uiso 0.218(17) 2 d SPD B 3

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
Cr1 0.0304(5) 0.0362(5) 0.0375(6) 0.000 0.0017(4) 0.000
Cl1 0.0415(9) 0.0765(12) 0.0593(10) 0.000 -0.0105(8) 0.000
N1 0.044(2) 0.060(3) 0.054(2) 0.019(2) 0.0047(18) -0.0007(18)
N2 0.0398(19) 0.0320(17) 0.053(2) 0.0029(16) 0.0058(16) 0.0046(15)
N3 0.078(5) 0.079(5) 0.043(3) 0.000 0.012(3) 0.000
O1 0.035(2) 0.034(2) 0.065(3) 0.000 -0.010(2) 0.000
O2 0.058(2) 0.066(2) 0.086(3) -0.018(2) -0.007(2) -0.0068(19)
C1 0.079(6) 0.133(9) 0.045(4) 0.000 0.020(4) 0.000
C2 0.083(4) 0.104(5) 0.049(3) 0.026(3) 0.011(3) -0.006(4)
C3 0.058(3) 0.047(3) 0.077(4) 0.025(3) 0.012(3) 0.006(2)
C4 0.052(3) 0.032(2) 0.084(4) 0.004(2) 0.010(2) 0.000(2)
C5 0.052(3) 0.041(2) 0.046(2) -0.0079(19) 0.003(2) 0.0005(19)
C6 0.048(4) 0.046(3) 0.039(3) 0.000 0.006(3) 0.000
C7 0.045(4) 0.067(4) 0.057(4) 0.000 0.013(3) 0.000
Cl2 0.0418(7) 0.0644(9) 0.0780(9) 0.0028(7) -0.0041(6) -0.0097(5)
O21A 0.101(9) 0.141(11) 0.110(9) -0.078(9) 0.044(8) -0.039(8)
O22A 0.050(5) 0.131(11) 0.106(9) -0.003(8) 0.000(5) -0.030(6)
O23A 0.127(15) 0.29(3) 0.098(13) 0.052(15) -0.035(11) 0.026(17)
O24A 0.190(16) 0.068(7) 0.093(8) 0.006(6) -0.017(9) -0.036(8)
O21B 0.073(10) 0.40(4) 0.192(19) 0.21(2) 0.027(11) 0.017(16)
O22B 0.122(15) 0.21(2) 0.46(4) -0.17(3) -0.12(2) 0.114(16)
O23B 0.188(19) 0.149(16) 0.163(15) -0.083(14) 0.071(15) -0.105(16)
O24B 0.073(9) 0.128(12) 0.136(16) -0.060(11) -0.055(9) 0.028(8)
Cl3 0.0612(11) 0.0562(10) 0.0494(9) 0.000 -0.0045(8) 0.000

_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
Cr1 O1 1.997(4) . ?
Cr1 N1 2.044(4) 7_565 ?
Cr1 N1 2.044(4) . ?
Cr1 N2 2.064(4) . ?
Cr1 N2 2.064(4) 7_565 ?
Cr1 Cl1 2.288(2) . ?
N1 C2 1.480(7) . ?
N1 C3 1.502(7) . ?
N1 H1 0.9100 . ?
N2 C5 1.475(6) . ?
N2 C4 1.495(6) . ?
N2 H2 0.9101 . ?
N3 C6 1.512(8) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
O1 H11 0.7104 . ?
O2 H21 0.8997 . ?
O2 H22 0.9001 . ?
C1 C2 1.510(8) . ?
C1 C2 1.510(8) 7_565 ?
C1 H1D 0.9699 . ?
C1 H1E 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.511(8) . ?
C3 H3D 0.9700 . ?
C3 H3E 0.9701 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.538(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9701 . ?
C6 C7 1.509(9) . ?
C6 C5 1.538(6) 7_565 ?
C7 H7A 0.9600 . ?
C7 H7B 0.9561 . ?
Cl2 O23A 1.379(5) . ?
Cl2 O22A 1.385(5) . ?
Cl2 O23B 1.386(5) . ?
Cl2 O22B 1.390(6) . ?
Cl2 O21B 1.392(6) . ?
Cl2 O24B 1.394(5) . ?
Cl2 O24A 1.396(5) . ?
Cl2 O21A 1.405(5) . ?
Cl3 O31B 1.370(6) . ?
Cl3 O33A 1.371(6) . ?
Cl3 O33B 1.371(6) . ?
Cl3 O31A 1.373(6) . ?
Cl3 O32A 1.374(5) . ?
Cl3 O32A 1.374(5) 7_565 ?
Cl3 O32B 1.375(6) . ?
Cl3 O32B 1.375(6) 7_565 ?
Cl3 O33C 1.377(6) . ?
Cl3 O31C 1.379(6) . ?
Cl3 O32C 1.384(6) . ?
Cl3 O32C 1.384(6) 7_565 ?

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 Cr1 N1 87.93(15) . 7_565 ?
O1 Cr1 N1 87.93(15) . . ?
N1 Cr1 N1 95.3(2) 7_565 . ?
O1 Cr1 N2 90.60(14) . . ?
N1 Cr1 N2 178.37(16) 7_565 . ?
N1 Cr1 N2 85.37(16) . . ?
O1 Cr1 N2 90.60(14) . 7_565 ?
N1 Cr1 N2 85.37(16) 7_565 7_565 ?
N1 Cr1 N2 178.37(16) . 7_565 ?
N2 Cr1 N2 93.9(2) . 7_565 ?
O1 Cr1 Cl1 179.40(14) . . ?
N1 Cr1 Cl1 92.47(13) 7_565 . ?
N1 Cr1 Cl1 92.47(13) . . ?
N2 Cr1 Cl1 88.99(12) . . ?
N2 Cr1 Cl1 88.99(12) 7_565 . ?
C2 N1 C3 113.5(4) . . ?
C2 N1 Cr1 115.8(4) . . ?
C3 N1 Cr1 106.7(3) . . ?
C2 N1 H1 106.8 . . ?
C3 N1 H1 106.8 . . ?
Cr1 N1 H1 106.8 . . ?
C5 N2 C4 112.8(4) . . ?
C5 N2 Cr1 117.2(3) . . ?
C4 N2 Cr1 106.1(3) . . ?
C5 N2 H2 106.4 . . ?
C4 N2 H2 106.8 . . ?
Cr1 N2 H2 107.0 . . ?
C6 N3 H3A 109.3 . . ?
C6 N3 H3B 109.6 . . ?
H3A N3 H3B 109.5 . . ?
Cr1 O1 H11 121.8 . . ?
H21 O2 H22 108.5 . . ?
C2 C1 C2 115.9(7) . 7_565 ?
C2 C1 H1D 108.9 . . ?
C2 C1 H1D 108.9 7_565 . ?
C2 C1 H1E 107.6 . . ?
C2 C1 H1E 107.6 7_565 . ?
H1D C1 H1E 107.6 . . ?
N1 C2 C1 112.1(6) . . ?
N1 C2 H2A 109.2 . . ?
C1 C2 H2A 109.2 . . ?
N1 C2 H2B 109.2 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
N1 C3 C4 107.3(4) . . ?
N1 C3 H3D 110.9 . . ?
C4 C3 H3D 111.0 . . ?
N1 C3 H3E 109.3 . . ?
C4 C3 H3E 109.8 . . ?
H3D C3 H3E 108.5 . . ?
N2 C4 C3 108.2(4) . . ?
N2 C4 H4A 110.2 . . ?
C3 C4 H4A 110.0 . . ?
N2 C4 H4B 109.9 . . ?
C3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.6 . . ?
N2 C5 C6 112.3(4) . . ?
N2 C5 H5A 108.7 . . ?
C6 C5 H5A 108.8 . . ?
N2 C5 H5B 109.7 . . ?
C6 C5 H5B 109.4 . . ?
H5A C5 H5B 107.9 . . ?
C7 C6 N3 107.4(6) . . ?
C7 C6 C5 112.3(3) . . ?
N3 C6 C5 104.8(4) . . ?
C7 C6 C5 112.3(3) . 7_565 ?
N3 C6 C5 104.8(4) . 7_565 ?
C5 C6 C5 114.4(5) . 7_565 ?
C6 C7 H7A 109.4 . . ?
C6 C7 H7B 109.7 . . ?
H7A C7 H7B 105.0 . . ?
O23A Cl2 O22A 110.9(4) . . ?
O23B Cl2 O22B 109.7(4) . . ?
O23B Cl2 O21B 109.5(4) . . ?
O22B Cl2 O21B 109.6(4) . . ?
O23B Cl2 O24B 109.6(4) . . ?
O22B Cl2 O24B 109.2(4) . . ?
O21B Cl2 O24B 109.2(4) . . ?
O22A Cl2 O24A 109.4(4) . . ?
O23A Cl2 O21A 109.7(4) . . ?
O22A Cl2 O21A 108.5(4) . . ?
O24A Cl2 O21A 107.9(4) . . ?
O31B Cl3 O33B 112.8(5) . . ?
O33A Cl3 O31A 112.4(5) . . ?
O33A Cl3 O32A 112.8(4) . . ?
O31A Cl3 O32A 112.8(4) . . ?
O33A Cl3 O32A 112.8(4) . 7_565 ?
O31A Cl3 O32A 112.8(4) . 7_565 ?
O32A Cl3 O32A 91.8(11) . 7_565 ?
O31B Cl3 O32B 112.7(5) . . ?
O33B Cl3 O32B 112.9(5) . . ?
O31B Cl3 O32B 112.7(5) . 7_565 ?
O33B Cl3 O32B 112.9(5) . 7_565 ?
O32B Cl3 O32B 91.2(14) . 7_565 ?
O33C Cl3 O31C 111.5(5) . . ?
O33C Cl3 O32C 111.5(5) . . ?
O31C Cl3 O32C 111.1(5) . . ?
O33C Cl3 O32C 111.5(5) . 7_565 ?
O31C Cl3 O32C 111.1(5) . 7_565 ?
O32C Cl3 O32C 99.4(16) . 7_565 ?

# Attachment 'tIIICrL15Cl.cif'

data_mmmm95b
_database_code_depnum_ccdc_archive 'CCDC 736219'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 Cl Cr N5, 2(Cl O4)'
_chemical_formula_sum            'C12 H29 Cl3 Cr N5 O8'
_chemical_formula_weight         529.75

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.225(5)
_cell_length_b                   13.727(3)
_cell_length_c                   23.329(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4235(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    313
_cell_measurement_theta_min      3
_cell_measurement_theta_max      31

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2200
_exptl_absorpt_coefficient_mu    0.969
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  'MAR345 with image plate detector'
_diffrn_measurement_method       'phi scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            41669
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.76
_diffrn_reflns_theta_max         32.41
_reflns_number_total             6564
_reflns_number_gt                5157
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       MARXDS
_computing_cell_refinement       AUTOMAR
_computing_data_reduction        MARSCALE
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP (Brueggermann and Smith, 1990)'
_computing_publication_material  'PLATON (Spek, 1990)'

_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^)+(0.1044P)^2^+2.4045P] 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     SHELXL
_refine_ls_extinction_coef       0.0043(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         6564
_refine_ls_number_parameters     299
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0589
_refine_ls_wR_factor_ref         0.2138
_refine_ls_wR_factor_gt          0.2052
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_restrained_S_all      1.268
_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
Cr1 Cr 0.91375(4) 0.15627(3) 0.624158(19) 0.03329(16) Uani 1 1 d U . .
Cl1 Cl 0.82487(7) 0.28355(7) 0.66481(4) 0.0516(2) Uani 1 1 d U . .
N1 N 0.8433(2) 0.0591(2) 0.67938(12) 0.0391(5) Uani 1 1 d . . .
H1A H 0.8495 0.0859 0.7149 0.047 Uiso 1 1 calc R . .
N2 N 0.8182(2) 0.1340(2) 0.55487(12) 0.0452(6) Uani 1 1 d U . .
H2A H 0.8358 0.0751 0.5401 0.054 Uiso 1 1 calc R . .
N3 N 0.9870(2) 0.2431(2) 0.56491(12) 0.0446(6) Uani 1 1 d U . .
H3A H 1.0241 0.2031 0.5420 0.054 Uiso 1 1 calc R . .
N4 N 1.0213(2) 0.1624(2) 0.68944(13) 0.0465(6) Uani 1 1 d U . .
H4A H 0.9836 0.1702 0.7218 0.056 Uiso 1 1 calc R . .
N5 N 0.9972(2) 0.0343(2) 0.60338(12) 0.0394(5) Uani 1 1 d U . .
H5A H 0.9631 -0.0047 0.5792 0.047 Uiso 1 1 calc R . .
H5B H 1.0568 0.0507 0.5874 0.047 Uiso 1 1 calc R . .
C1 C 0.7288(3) 0.0454(3) 0.67009(17) 0.0538(8) Uani 1 1 d . . .
H1B H 0.6931 0.1016 0.6851 0.065 Uiso 1 1 calc R . .
H1C H 0.7062 -0.0115 0.6912 0.065 Uiso 1 1 calc R . .
C2 C 0.7018(4) 0.0324(4) 0.6048(2) 0.0688(11) Uani 1 1 d . . .
H2B H 0.7454 -0.0175 0.5887 0.083 Uiso 1 1 calc R . .
H2C H 0.6327 0.0092 0.6019 0.083 Uiso 1 1 calc R . .
C3 C 0.7125(4) 0.1274(4) 0.5674(2) 0.0643(10) Uani 1 1 d . . .
H3B H 0.6733 0.1222 0.5324 0.077 Uiso 1 1 calc R . .
H3C H 0.6899 0.1842 0.5886 0.077 Uiso 1 1 calc R . .
C4 C 0.8332(4) 0.2039(4) 0.5088(2) 0.0654(11) Uani 1 1 d . . .
H4B H 0.7685 0.2311 0.4974 0.078 Uiso 1 1 calc R . .
H4C H 0.8622 0.1712 0.4758 0.078 Uiso 1 1 calc R . .
C5 C 0.9041(4) 0.2862(3) 0.5284(2) 0.0617(10) Uani 1 1 d . . .
H5C H 0.9332 0.3185 0.4953 0.074 Uiso 1 1 calc R . .
H5D H 0.8664 0.3340 0.5504 0.074 Uiso 1 1 calc R . .
C6 C 1.0607(4) 0.3187(4) 0.5911(2) 0.0701(12) Uani 1 1 d U . .
H6A H 1.0962 0.3524 0.5605 0.084 Uiso 1 1 calc R . .
H6B H 1.0228 0.3666 0.6128 0.084 Uiso 1 1 calc R . .
C7 C 1.1353(4) 0.2699(4) 0.6293(2) 0.0712(12) Uani 1 1 d . . .
H7A H 1.1945 0.3112 0.6327 0.085 Uiso 1 1 calc R . .
H7B H 1.1564 0.2093 0.6115 0.085 Uiso 1 1 calc R . .
C8 C 1.0936(4) 0.2473(4) 0.6910(2) 0.0682(11) Uani 1 1 d . . .
H8A H 1.1495 0.2322 0.7164 0.082 Uiso 1 1 calc R . .
H8B H 1.0591 0.3043 0.7059 0.082 Uiso 1 1 calc R . .
C9 C 1.0662(3) 0.0651(3) 0.69639(16) 0.0498(8) Uani 1 1 d . . .
H9A H 1.0624 0.0461 0.7364 0.060 Uiso 1 1 calc R . .
H9B H 1.1370 0.0676 0.6856 0.060 Uiso 1 1 calc R . .
C10 C 1.0116(3) -0.0124(3) 0.65923(16) 0.0477(7) Uani 1 1 d . . .
C11 C 0.9001(3) -0.0310(3) 0.68155(16) 0.0491(7) Uani 1 1 d . . .
H11A H 0.8674 -0.0798 0.6578 0.059 Uiso 1 1 calc R . .
H11B H 0.9021 -0.0551 0.7206 0.059 Uiso 1 1 calc R . .
C12 C 1.0657(4) -0.1112(4) 0.6582(2) 0.0703(12) Uani 1 1 d . . .
H12A H 1.0275 -0.1563 0.6354 0.105 Uiso 1 1 calc R . .
H12B H 1.0717 -0.1357 0.6966 0.105 Uiso 1 1 calc R . .
H12C H 1.1319 -0.1034 0.6419 0.105 Uiso 1 1 calc R . .
Cl2 Cl 1.10156(10) -0.40018(10) 0.65997(6) 0.0736(3) Uani 1 1 d D . .
O1 O 1.1338(5) -0.3816(5) 0.6004(2) 0.0664(15) Uani 0.50 1 d PD A 1
O2 O 1.0850(6) -0.5058(4) 0.6730(3) 0.0671(16) Uani 0.50 1 d PD A 1
O3 O 1.1766(5) -0.3554(5) 0.7020(3) 0.0606(17) Uani 0.50 1 d PD A 1
O4 O 0.9987(4) -0.3454(4) 0.6716(3) 0.0655(15) Uani 0.50 1 d PD A 1
O1' O 1.0288(5) -0.4775(4) 0.6795(3) 0.0630(15) Uani 0.50 1 d PD A 2
O2' O 1.1950(4) -0.4512(5) 0.6362(3) 0.0722(17) Uani 0.50 1 d PD A 2
O3' O 1.0549(5) -0.3416(4) 0.6127(2) 0.0659(15) Uani 0.50 1 d PD A 2
O4' O 1.1322(5) -0.3361(5) 0.7082(3) 0.0582(16) Uani 0.50 1 d PD A 2
Cl3 Cl 1.12205(10) 0.10516(9) 0.48415(5) 0.0693(3) Uani 1 1 d . . .
O5 O 1.1254(4) 0.0939(4) 0.4202(2) 0.1066(15) Uani 1 1 d . . .
O6 O 1.1747(4) 0.0197(4) 0.5110(2) 0.1110(16) Uani 1 1 d . . .
O7 O 1.1719(4) 0.1975(4) 0.5008(2) 0.1095(15) Uani 1 1 d . . .
O8 O 1.0125(5) 0.1057(4) 0.5037(2) 0.1121(16) 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
Cr1 0.0342(3) 0.0321(3) 0.0336(3) -0.00065(15) 0.00086(16) 0.00034(16)
Cl1 0.0551(5) 0.0464(4) 0.0535(5) -0.0027(3) 0.0032(3) 0.0042(3)
N1 0.0419(13) 0.0383(12) 0.0370(12) -0.0014(10) 0.0024(10) -0.0008(10)
N2 0.0466(15) 0.0463(14) 0.0428(13) -0.0039(11) -0.0046(9) 0.0020(11)
N3 0.0480(14) 0.0422(13) 0.0436(13) 0.0035(9) 0.0080(10) 0.0005(10)
N4 0.0470(15) 0.0512(16) 0.0414(13) -0.0009(11) -0.0048(9) -0.0027(12)
N5 0.0399(13) 0.0381(12) 0.0400(13) -0.0028(10) 0.0007(10) 0.0005(10)
C1 0.053(2) 0.054(2) 0.055(2) -0.0018(16) 0.0031(15) -0.0018(16)
C2 0.066(3) 0.069(3) 0.072(3) -0.007(2) 0.001(2) 0.002(2)
C3 0.055(2) 0.073(3) 0.064(2) -0.006(2) -0.0028(19) 0.002(2)
C4 0.069(3) 0.066(3) 0.061(2) 0.003(2) -0.0036(19) 0.005(2)
C5 0.070(3) 0.058(2) 0.057(2) 0.0027(18) -0.0008(18) -0.0006(19)
C6 0.073(3) 0.066(3) 0.071(3) -0.005(2) 0.006(2) -0.015(2)
C7 0.066(3) 0.072(3) 0.076(3) -0.009(2) 0.002(2) -0.005(2)
C8 0.069(3) 0.067(3) 0.068(3) -0.004(2) -0.003(2) -0.009(2)
C9 0.0475(18) 0.0532(19) 0.0488(18) -0.0011(15) -0.0015(14) 0.0010(15)
C10 0.0479(18) 0.0464(18) 0.0487(18) -0.0002(13) -0.0008(14) 0.0030(14)
C11 0.0521(19) 0.0474(18) 0.0477(18) 0.0010(14) 0.0036(14) -0.0005(14)
C12 0.072(3) 0.064(3) 0.075(3) -0.002(2) -0.005(2) 0.008(2)
Cl2 0.0758(8) 0.0777(8) 0.0671(7) 0.0014(5) -0.0029(5) -0.0071(6)
O1 0.070(4) 0.076(4) 0.053(3) 0.005(3) -0.006(3) -0.004(3)
O2 0.071(4) 0.063(4) 0.068(4) 0.000(3) 0.009(3) 0.003(3)
O3 0.053(4) 0.069(4) 0.060(4) 0.007(3) 0.002(3) -0.002(3)
O4 0.062(4) 0.069(4) 0.065(4) 0.001(3) -0.002(3) -0.004(3)
O1' 0.059(4) 0.064(4) 0.067(4) 0.002(3) 0.002(3) -0.007(3)
O2' 0.062(4) 0.084(5) 0.071(4) -0.011(3) 0.000(3) 0.001(3)
O3' 0.075(4) 0.061(4) 0.062(3) -0.003(3) -0.003(3) -0.002(3)
O4' 0.051(4) 0.061(4) 0.062(4) 0.002(3) -0.002(3) 0.001(3)
Cl3 0.0670(7) 0.0703(7) 0.0706(7) -0.0099(5) 0.0058(5) -0.0032(5)
O5 0.103(3) 0.107(4) 0.110(4) -0.001(3) -0.002(3) 0.008(3)
O6 0.108(4) 0.118(4) 0.108(4) -0.006(3) 0.000(3) 0.007(3)
O7 0.110(4) 0.109(4) 0.110(4) -0.008(3) 0.001(3) 0.000(3)
O8 0.111(4) 0.120(4) 0.105(3) 0.003(3) 0.000(3) -0.005(3)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cr1 N5 2.062(3) . ?
Cr1 N3 2.066(3) . ?
Cr1 N2 2.074(3) . ?
Cr1 N1 2.075(3) . ?
Cr1 N4 2.086(3) . ?
Cr1 Cl1 2.3095(11) . ?
N1 C11 1.448(5) . ?
N1 C1 1.542(5) . ?
N1 H1A 0.9100 . ?
N2 C3 1.431(6) . ?
N2 C4 1.455(6) . ?
N2 H2A 0.9100 . ?
N3 C5 1.508(5) . ?
N3 C6 1.550(6) . ?
N3 H3A 0.9100 . ?
N4 C9 1.471(5) . ?
N4 C8 1.507(6) . ?
N4 H4A 0.9100 . ?
N5 C10 1.465(5) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
C1 C2 1.576(6) . ?
C1 H1B 0.9700 . ?
C1 H1C 0.9700 . ?
C2 C3 1.576(7) . ?
C2 H2B 0.9700 . ?
C2 H2C 0.9700 . ?
C3 H3B 0.9700 . ?
C3 H3C 0.9700 . ?
C4 C5 1.539(7) . ?
C4 H4B 0.9700 . ?
C4 H4C 0.9700 . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C6 C7 1.489(8) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.574(7) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.550(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C12 1.534(6) . ?
C10 C11 1.585(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
Cl2 O1 1.476(5) . ?
Cl2 O4' 1.484(5) . ?
Cl2 O2 1.497(6) . ?
Cl2 O3' 1.499(5) . ?
Cl2 O1' 1.504(5) . ?
Cl2 O2' 1.524(5) . ?
Cl2 O3 1.525(6) . ?
Cl2 O4 1.578(6) . ?
Cl3 O7 1.481(6) . ?
Cl3 O5 1.501(6) . ?
Cl3 O6 1.501(6) . ?
Cl3 O8 1.519(6) . ?

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
N5 Cr1 N3 93.46(11) . . ?
N5 Cr1 N2 91.32(12) . . ?
N3 Cr1 N2 81.33(13) . . ?
N5 Cr1 N1 82.21(11) . . ?
N3 Cr1 N1 175.20(11) . . ?
N2 Cr1 N1 96.65(12) . . ?
N5 Cr1 N4 80.77(12) . . ?
N3 Cr1 N4 98.37(12) . . ?
N2 Cr1 N4 172.07(12) . . ?
N1 Cr1 N4 83.03(12) . . ?
N5 Cr1 Cl1 169.33(8) . . ?
N3 Cr1 Cl1 94.40(9) . . ?
N2 Cr1 Cl1 96.98(9) . . ?
N1 Cr1 Cl1 90.16(8) . . ?
N4 Cr1 Cl1 90.95(9) . . ?
C11 N1 C1 114.2(3) . . ?
C11 N1 Cr1 109.8(2) . . ?
C1 N1 Cr1 115.6(2) . . ?
C11 N1 H1A 105.4 . . ?
C1 N1 H1A 105.4 . . ?
Cr1 N1 H1A 105.4 . . ?
C3 N2 C4 109.0(3) . . ?
C3 N2 Cr1 116.4(3) . . ?
C4 N2 Cr1 113.4(3) . . ?
C3 N2 H2A 105.7 . . ?
C4 N2 H2A 105.7 . . ?
Cr1 N2 H2A 105.7 . . ?
C5 N3 C6 114.7(3) . . ?
C5 N3 Cr1 105.2(2) . . ?
C6 N3 Cr1 114.7(3) . . ?
C5 N3 H3A 107.3 . . ?
C6 N3 H3A 107.3 . . ?
Cr1 N3 H3A 107.3 . . ?
C9 N4 C8 116.3(3) . . ?
C9 N4 Cr1 108.6(2) . . ?
C8 N4 Cr1 118.8(3) . . ?
C9 N4 H4A 103.7 . . ?
C8 N4 H4A 103.7 . . ?
Cr1 N4 H4A 103.7 . . ?
C10 N5 Cr1 102.5(2) . . ?
C10 N5 H5A 111.3 . . ?
Cr1 N5 H5A 111.3 . . ?
C10 N5 H5B 111.3 . . ?
Cr1 N5 H5B 111.3 . . ?
H5A N5 H5B 109.2 . . ?
N1 C1 C2 111.9(3) . . ?
N1 C1 H1B 109.2 . . ?
C2 C1 H1B 109.2 . . ?
N1 C1 H1C 109.2 . . ?
C2 C1 H1C 109.2 . . ?
H1B C1 H1C 107.9 . . ?
C3 C2 C1 114.9(4) . . ?
C3 C2 H2B 108.5 . . ?
C1 C2 H2B 108.5 . . ?
C3 C2 H2C 108.5 . . ?
C1 C2 H2C 108.5 . . ?
H2B C2 H2C 107.5 . . ?
N2 C3 C2 104.7(4) . . ?
N2 C3 H3B 110.8 . . ?
C2 C3 H3B 110.8 . . ?
N2 C3 H3C 110.8 . . ?
C2 C3 H3C 110.8 . . ?
H3B C3 H3C 108.9 . . ?
N2 C4 C5 110.3(4) . . ?
N2 C4 H4B 109.6 . . ?
C5 C4 H4B 109.6 . . ?
N2 C4 H4C 109.6 . . ?
C5 C4 H4C 109.6 . . ?
H4B C4 H4C 108.1 . . ?
N3 C5 C4 108.9(3) . . ?
N3 C5 H5C 109.9 . . ?
C4 C5 H5C 109.9 . . ?
N3 C5 H5D 109.9 . . ?
C4 C5 H5D 109.9 . . ?
H5C C5 H5D 108.3 . . ?
C7 C6 N3 110.6(4) . . ?
C7 C6 H6A 109.5 . . ?
N3 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
C6 C7 C8 113.9(4) . . ?
C6 C7 H7A 108.8 . . ?
C8 C7 H7A 108.8 . . ?
C6 C7 H7B 108.8 . . ?
C8 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
N4 C8 C7 110.7(4) . . ?
N4 C8 H8A 109.5 . . ?
C7 C8 H8A 109.5 . . ?
N4 C8 H8B 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
N4 C9 C10 111.9(3) . . ?
N4 C9 H9A 109.2 . . ?
C10 C9 H9A 109.2 . . ?
N4 C9 H9B 109.2 . . ?
C10 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
N5 C10 C12 115.7(3) . . ?
N5 C10 C9 104.9(3) . . ?
C12 C10 C9 113.5(3) . . ?
N5 C10 C11 104.0(3) . . ?
C12 C10 C11 107.3(3) . . ?
C9 C10 C11 111.1(3) . . ?
N1 C11 C10 109.5(3) . . ?
N1 C11 H11A 109.8 . . ?
C10 C11 H11A 109.8 . . ?
N1 C11 H11B 109.8 . . ?
C10 C11 H11B 109.8 . . ?
H11A C11 H11B 108.2 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O1 Cl2 O4' 122.2(4) . . ?
O1 Cl2 O2 113.7(4) . . ?
O4' Cl2 O2 117.3(4) . . ?
O1 Cl2 O3' 48.2(4) . . ?
O4' Cl2 O3' 110.6(4) . . ?
O2 Cl2 O3' 127.6(4) . . ?
O1 Cl2 O1' 126.3(4) . . ?
O4' Cl2 O1' 111.3(4) . . ?
O2 Cl2 O1' 33.0(3) . . ?
O3' Cl2 O1' 109.8(4) . . ?
O1 Cl2 O2' 60.2(4) . . ?
O4' Cl2 O2' 109.1(4) . . ?
O2 Cl2 O2' 75.4(4) . . ?
O3' Cl2 O2' 108.2(4) . . ?
O1' Cl2 O2' 107.8(4) . . ?
O1 Cl2 O3 110.4(4) . . ?
O4' Cl2 O3 25.3(3) . . ?
O2 Cl2 O3 110.7(4) . . ?
O3' Cl2 O3 121.7(4) . . ?
O1' Cl2 O3 120.4(4) . . ?
O2' Cl2 O3 83.8(4) . . ?
O1 Cl2 O4 109.2(3) . . ?
O4' Cl2 O4 79.8(3) . . ?
O2 Cl2 O4 107.5(4) . . ?
O3' Cl2 O4 61.1(4) . . ?
O1' Cl2 O4 74.5(4) . . ?
O2' Cl2 O4 168.6(4) . . ?
O3 Cl2 O4 104.9(3) . . ?
O7 Cl3 O5 109.7(3) . . ?
O7 Cl3 O6 110.7(3) . . ?
O5 Cl3 O6 108.7(3) . . ?
O7 Cl3 O8 110.0(3) . . ?
O5 Cl3 O8 109.1(3) . . ?
O6 Cl3 O8 108.7(3) . . ?

_diffrn_measured_fraction_theta_max 0.863
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.100