# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Dr Sylvie Chardon'
_publ_contact_author_email       SYLVIE.CHARDON@UJF-GRENOBLE.FR

_publ_section_title              
;
An easy electrochemical and chemical synthesis of
[Ru(bpy)(CH3CN)2Cl2]: a synthon for heteroleptic tris-diimine Ru(II)
complexes
;
loop_
_publ_author_name
'Sylvie Chardon'
'Alain Deronzier'
'Matti Haukka'
'Minna Jakonen'
'Frederic Lafolet'
'Elina Laurila'
;
A.Renfrew
;

# Attachment 'elar1ds.cif'

# An easy electrochemical and chemical synthesis of [Ru(bpy)(CH3CN)2Cl2]: a
# synthon for heteroleptic tris-diimine Ru(II) complexes
# by Sylvie Chardon-Noblat, Anna Renfrew, Fr\'ed\'eric Lafolet, Alain Deronzier,
# Minna Jakonen, Elina Laurila, and Matti Haukka

data_elar1ds
_database_code_depnum_ccdc_archive 'CCDC 688366'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H20 Cl2 N4 Ru, 3(C H Cl3)'
_chemical_formula_sum            'C25 H23 Cl11 N4 Ru'
_chemical_formula_weight         870.49

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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

_cell_length_a                   12.9977(7)
_cell_length_b                   16.1554(9)
_cell_length_c                   16.1347(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.813(3)
_cell_angle_gamma                90.00
_cell_volume                     3383.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    12649
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            'dark purple'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1728
_exptl_absorpt_coefficient_mu    1.357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6432
_exptl_absorpt_correction_T_max  0.7595
_exptl_absorpt_process_details   'SADABS v.2.10 (Sheldrick, 2003)'

_publ_section_exptl_refinement   
;
The Ru atom is located on a two-fold rotation axis and is coordinated by four N
atoms and two Cl atoms in a slightly distorted octahedral geometry.

The methyl substituents (C20 and C21) on the 4,4'-dimethyl-2,2'-bipyridine ring
and the corresponding hydrogens (H12 and H17) on the 2,2'-bipyridine ring were
disordered over two alternative sites, i.e. the 4,4-dimethyl-2,2'-bipyridine
ligand and 2,2'-bipyridine ligand were located on two alternative sites.
The disordered methyl groups and hydrogens were refined with equal occupancies
0.5.
Both determined CHCl~3~ solvent molecules were also disordered. The carbon atom
C23 was located on a two-fold rotation axis and each chloride attached to it
were disordered over several sites with variable occupancies.
In the second independent CHCl~3~ solvent molecule (C22) the chlorides Cl3 and
Cl4 were disordered over two positions with occupancies 0.86/0.14 and 0.54/0.46
respectively. The anisotropic displacement parameters of each disordered
chloride were set to be equal with their counterparts.
The hydrogen atoms were positioned geometrically and were constrained
to ride on their parent atoms, with C---H = 0.95-1.00 \%A, and
U~iso~ = 1.2-1.5 U~eq~(parent atom).
The highest peak is located 0.75 \%A from atom Cl4A and the deepest hole is
located 0.55 \%A from atom Cl4B.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_method       '\f scans and \w scans with \k offset'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22619
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.34
_diffrn_reflns_theta_max         27.51
_reflns_number_total             3884
_reflns_number_gt                3121
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond v.3.1e (Brandenburg, 2007)'
_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^)+(0.0528P)^2^+18.8223P] 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         3884
_refine_ls_number_parameters     231
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0520
_refine_ls_wR_factor_ref         0.1385
_refine_ls_wR_factor_gt          0.1291
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.5000 0.05162(3) 0.7500 0.03580(15) Uani 1 2 d S . .
Cl1 Cl 0.42347(8) 0.15593(7) 0.65768(7) 0.0443(3) Uani 1 1 d . . .
Cl2 Cl 0.87437(13) 0.19961(10) 0.97919(9) 0.0706(4) Uani 1 1 d . A .
Cl3A Cl 0.8735(2) 0.25262(14) 0.80669(12) 0.0866(8) Uani 0.861(4) 1 d P A 1
Cl3B Cl 0.8049(14) 0.2840(9) 0.8342(8) 0.0866(8) Uani 0.139(4) 1 d P A 2
Cl4A Cl 0.9201(4) 0.0990(4) 0.8324(3) 0.0763(8) Uani 0.465(5) 1 d P A 3
Cl4B Cl 0.8878(4) 0.0719(3) 0.8550(3) 0.0763(8) Uani 0.535(5) 1 d P A 4
Cl5A Cl 0.873(3) 0.143(2) 0.239(3) 0.094(3) Uani 0.094(10) 1 d P B 5
Cl5B Cl 0.8756(7) 0.1203(6) 0.2025(6) 0.094(3) Uani 0.406(10) 1 d P B 6
Cl6A Cl 1.0105(11) 0.1203(4) 0.1497(4) 0.092(3) Uani 0.339(6) 1 d P B 7
Cl6B Cl 0.927(2) 0.1052(10) 0.1807(11) 0.092(3) Uani 0.161(6) 1 d P B 8
Cl7A Cl 0.9374(10) 0.1392(7) 0.3423(15) 0.126(6) Uani 0.276(6) 1 d P B 9
Cl7B Cl 0.8911(13) 0.1342(8) 0.2862(18) 0.126(6) Uani 0.224(6) 1 d P B 10
N1 N 0.5505(3) -0.0365(2) 0.8310(2) 0.0378(8) Uani 1 1 d . D .
N2 N 0.6202(3) 0.0462(2) 0.6728(2) 0.0401(8) Uani 1 1 d . E .
C10 C 0.6403(4) -0.0780(3) 0.8283(3) 0.0466(10) Uani 1 1 d . . .
H10 H 0.6860 -0.0647 0.7861 0.056 Uiso 1 1 calc R . .
C11 C 0.6679(4) -0.1391(3) 0.8844(3) 0.0509(11) Uani 1 1 d . D .
H11 H 0.7308 -0.1682 0.8795 0.061 Uiso 1 1 calc R . .
C12 C 0.6043(4) -0.1583(3) 0.9481(3) 0.0474(11) Uani 1 1 d . . .
C17 C 0.7769(4) 0.0273(4) 0.5633(3) 0.0626(15) Uani 1 1 d . . .
H12 H 0.6233 -0.2027 0.9882 0.075 Uiso 0.50 1 d PR C 11
H17 H 0.8312 0.0214 0.5264 0.075 Uiso 0.50 1 d PR C 11
C20 C 0.6248(9) -0.2233(6) 1.0089(6) 0.055(2) Uani 0.50 1 d P D 12
H20A H 0.6968 -0.2199 1.0299 0.083 Uiso 0.50 1 calc PR D 12
H20B H 0.6123 -0.2773 0.9828 0.083 Uiso 0.50 1 calc PR D 12
H20C H 0.5793 -0.2164 1.0551 0.083 Uiso 0.50 1 calc PR D 12
C21 C 0.8627(7) 0.0274(7) 0.5084(6) 0.053(2) Uani 0.50 1 d P E 12
H21A H 0.9077 -0.0200 0.5216 0.079 Uiso 0.50 1 calc PR E 12
H21B H 0.9019 0.0788 0.5160 0.079 Uiso 0.50 1 calc PR E 12
H21C H 0.8361 0.0232 0.4506 0.079 Uiso 0.50 1 calc PR E 12
C13 C 0.5125(4) -0.1151(3) 0.9517(3) 0.0435(10) Uani 1 1 d . D .
H13 H 0.4673 -0.1263 0.9948 0.052 Uiso 1 1 calc R . .
C14 C 0.4866(3) -0.0558(2) 0.8927(2) 0.0362(8) Uani 1 1 d . . .
C15 C 0.6107(3) -0.0093(3) 0.6106(3) 0.0392(9) Uani 1 1 d . . .
C16 C 0.6881(4) -0.0203(3) 0.5551(3) 0.0518(12) Uani 1 1 d . E .
H16 H 0.6803 -0.0602 0.5120 0.062 Uiso 1 1 calc R . .
C18 C 0.7855(4) 0.0856(4) 0.6262(3) 0.0592(14) Uani 1 1 d . E .
H18 H 0.8450 0.1197 0.6326 0.071 Uiso 1 1 calc R . .
C19 C 0.7062(3) 0.0933(4) 0.6794(3) 0.0531(12) Uani 1 1 d . . .
H19 H 0.7122 0.1333 0.7225 0.064 Uiso 1 1 calc R E .
C22 C 0.8401(4) 0.1745(3) 0.8754(3) 0.0568(13) Uani 1 1 d . . .
H22 H 0.7636 0.1666 0.8676 0.085 Uiso 1 1 d R A .
C23 C 1.0000 0.1594(5) 0.2500 0.0621(19) Uani 1 2 d S . .
H23 H 1.0000 0.2213 0.2500 0.093 Uiso 1 2 d SR B .

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
Ru1 0.0278(2) 0.0435(3) 0.0361(3) 0.000 0.00233(17) 0.000
Cl1 0.0405(5) 0.0501(6) 0.0417(6) -0.0001(4) -0.0035(4) 0.0060(5)
Cl2 0.0811(10) 0.0709(9) 0.0590(8) 0.0035(7) -0.0049(7) -0.0198(8)
Cl3A 0.1128(19) 0.0898(14) 0.0558(10) 0.0077(9) -0.0114(11) -0.0531(14)
Cl3B 0.1128(19) 0.0898(14) 0.0558(10) 0.0077(9) -0.0114(11) -0.0531(14)
Cl4A 0.073(2) 0.088(3) 0.068(2) 0.0024(15) 0.0011(14) 0.0155(17)
Cl4B 0.073(2) 0.088(3) 0.068(2) 0.0024(15) 0.0011(14) 0.0155(17)
Cl5A 0.098(4) 0.102(5) 0.079(5) 0.005(4) -0.016(4) -0.066(4)
Cl5B 0.098(4) 0.102(5) 0.079(5) 0.005(4) -0.016(4) -0.066(4)
Cl6A 0.138(7) 0.069(3) 0.065(3) -0.027(3) -0.036(4) 0.043(5)
Cl6B 0.138(7) 0.069(3) 0.065(3) -0.027(3) -0.036(4) 0.043(5)
Cl7A 0.050(5) 0.106(4) 0.227(19) 0.039(8) 0.050(7) -0.015(5)
Cl7B 0.050(5) 0.106(4) 0.227(19) 0.039(8) 0.050(7) -0.015(5)
N1 0.0354(17) 0.046(2) 0.0321(17) -0.0047(14) 0.0056(13) -0.0011(15)
N2 0.0329(17) 0.049(2) 0.0384(18) 0.0101(16) 0.0012(14) 0.0003(15)
C10 0.043(2) 0.061(3) 0.037(2) 0.003(2) 0.0063(18) 0.010(2)
C11 0.056(3) 0.055(3) 0.042(2) 0.000(2) 0.000(2) 0.016(2)
C12 0.064(3) 0.042(2) 0.036(2) -0.0005(18) -0.005(2) 0.000(2)
C17 0.034(2) 0.099(4) 0.056(3) 0.031(3) 0.016(2) 0.012(3)
C20 0.069(7) 0.050(5) 0.046(5) 0.004(4) -0.013(5) 0.016(5)
C21 0.044(5) 0.066(6) 0.051(5) -0.004(5) 0.022(4) 0.002(4)
C13 0.055(3) 0.041(2) 0.035(2) -0.0067(17) 0.0043(18) -0.012(2)
C14 0.040(2) 0.036(2) 0.033(2) -0.0062(16) 0.0030(16) -0.0092(17)
C15 0.035(2) 0.044(2) 0.038(2) 0.0133(18) 0.0045(17) 0.0101(18)
C16 0.047(3) 0.065(3) 0.044(2) 0.016(2) 0.013(2) 0.018(2)
C18 0.035(2) 0.091(4) 0.053(3) 0.018(3) 0.006(2) -0.009(2)
C19 0.034(2) 0.074(3) 0.052(3) 0.009(2) 0.0005(19) -0.010(2)
C22 0.050(3) 0.058(3) 0.061(3) 0.005(2) -0.013(2) -0.012(2)
C23 0.069(5) 0.042(4) 0.074(5) 0.000 -0.011(4) 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
Ru1 N1 2.020(4) 2_656 ?
Ru1 N1 2.020(4) . yes
Ru1 N2 2.047(3) . yes
Ru1 N2 2.047(3) 2_656 ?
Ru1 Cl1 2.4296(11) 2_656 ?
Ru1 Cl1 2.4296(11) . yes
Cl2 C22 1.759(5) . ?
Cl3A C22 1.748(6) . ?
Cl3B C22 1.937(17) . ?
Cl4A C22 1.767(8) . ?
Cl4B C22 1.806(7) . ?
Cl5A C23 1.68(3) . ?
Cl5B C23 1.866(7) . ?
Cl6A C23 1.748(7) . ?
Cl6B C23 1.677(18) . ?
Cl7A C23 1.762(16) . ?
Cl7B C23 1.610(10) . ?
N1 C10 1.349(6) . ?
N1 C14 1.363(5) . ?
N2 C15 1.348(6) . ?
N2 C19 1.351(6) . ?
C10 C11 1.375(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.385(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.386(7) . ?
C12 C20 1.452(10) . yes
C12 H12 0.9891 . ?
C17 C18 1.385(9) . ?
C17 C16 1.388(8) . ?
C17 C21 1.458(9) . yes
C17 H17 0.9500 . ?
C20 H12 0.4705 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H17 0.5226 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C13 C14 1.380(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.470(6) 2_656 ?
C15 C16 1.391(6) . ?
C15 C14 1.470(6) 2_656 ?
C16 H16 0.9500 . ?
C18 C19 1.379(7) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C22 H22 1.0044 . ?
C23 Cl7B 1.610(10) 2_755 ?
C23 Cl5A 1.68(3) 2_755 ?
C23 Cl6B 1.677(18) 2_755 ?
C23 Cl6A 1.749(7) 2_755 ?
C23 Cl7A 1.762(16) 2_755 ?
C23 Cl5B 1.866(7) 2_755 ?
C23 H23 1.0000 . ?

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
N1 Ru1 N1 90.41(19) 2_656 . ?
N1 Ru1 N2 79.02(14) 2_656 . yes
N1 Ru1 N2 97.51(13) . . ?
N1 Ru1 N2 97.50(13) 2_656 2_656 ?
N1 Ru1 N2 79.02(14) . 2_656 ?
N2 Ru1 N2 175.1(2) . 2_656 ?
N1 Ru1 Cl1 174.63(10) 2_656 2_656 ?
N1 Ru1 Cl1 88.95(10) . 2_656 ?
N2 Ru1 Cl1 95.78(11) . 2_656 ?
N2 Ru1 Cl1 87.60(10) 2_656 2_656 ?
N1 Ru1 Cl1 88.96(10) 2_656 . ?
N1 Ru1 Cl1 174.64(10) . . ?
N2 Ru1 Cl1 87.60(10) . . ?
N2 Ru1 Cl1 95.78(11) 2_656 . ?
Cl1 Ru1 Cl1 92.17(5) 2_656 . yes
C10 N1 C14 118.0(4) . . ?
C10 N1 Ru1 125.7(3) . . ?
C14 N1 Ru1 116.4(3) . . ?
C15 N2 C19 118.6(4) . . ?
C15 N2 Ru1 115.9(3) . . ?
C19 N2 Ru1 125.6(3) . . ?
N1 C10 C11 122.2(4) . . ?
N1 C10 H10 118.9 . . ?
C11 C10 H10 118.9 . . ?
C10 C11 C12 120.3(4) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C13 117.6(4) . . ?
C11 C12 C20 124.5(6) . . ?
C13 C12 C20 117.8(6) . . ?
C11 C12 H12 120.6 . . ?
C13 C12 H12 121.7 . . ?
C18 C17 C16 118.9(4) . . ?
C18 C17 C21 114.1(6) . . ?
C16 C17 C21 126.8(7) . . ?
C18 C17 H17 119.5 . . ?
C16 C17 H17 121.6 . . ?
C12 C20 H20A 109.5 . . ?
C12 C20 H20B 109.5 . . ?
C12 C20 H20C 109.5 . . ?
C17 C21 H21A 109.5 . . ?
C17 C21 H21B 109.5 . . ?
C17 C21 H21C 109.5 . . ?
C14 C13 C12 120.2(4) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
N1 C14 C13 121.7(4) . . ?
N1 C14 C15 114.2(4) . 2_656 ?
C13 C14 C15 124.1(4) . 2_656 ?
N2 C15 C16 121.4(4) . . ?
N2 C15 C14 114.5(3) . 2_656 ?
C16 C15 C14 124.1(4) . 2_656 ?
C17 C16 C15 119.5(5) . . ?
C17 C16 H16 120.3 . . ?
C15 C16 H16 120.3 . . ?
C19 C18 C17 118.8(5) . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 120.6 . . ?
N2 C19 C18 122.8(5) . . ?
N2 C19 H19 118.6 . . ?
C18 C19 H19 118.6 . . ?
Cl3A C22 Cl2 112.2(3) . . ?
Cl3A C22 Cl4A 94.6(3) . . ?
Cl2 C22 Cl4A 114.0(3) . . ?
Cl3A C22 Cl4B 116.7(4) . . ?
Cl2 C22 Cl4B 108.2(3) . . ?
Cl2 C22 Cl3B 99.2(5) . . ?
Cl4A C22 Cl3B 129.1(6) . . ?
Cl4B C22 Cl3B 148.6(6) . . ?
Cl3A C22 H22 106.7 . . ?
Cl2 C22 H22 110.5 . . ?
Cl4A C22 H22 117.5 . . ?
Cl4B C22 H22 102.0 . . ?
Cl3B C22 H22 81.8 . . ?
Cl7B C23 Cl7B 150.8(11) 2_755 . ?
Cl7B C23 Cl5A 143.5(17) 2_755 . ?
Cl7B C23 Cl5A 143.5(17) . 2_755 ?
Cl5A C23 Cl5A 162(3) . 2_755 ?
Cl7B C23 Cl6B 96.1(9) 2_755 . ?
Cl7B C23 Cl6B 68.3(11) . . ?
Cl5A C23 Cl6B 47.5(16) . . ?
Cl5A C23 Cl6B 120.7(12) 2_755 . ?
Cl7B C23 Cl6B 68.3(11) 2_755 2_755 ?
Cl7B C23 Cl6B 96.1(9) . 2_755 ?
Cl5A C23 Cl6B 120.7(12) . 2_755 ?
Cl5A C23 Cl6B 47.5(16) 2_755 2_755 ?
Cl6B C23 Cl6B 117.2(10) . 2_755 ?
Cl7B C23 Cl6A 57.5(9) 2_755 . ?
Cl7B C23 Cl6A 110.8(9) . . ?
Cl5A C23 Cl6A 88.2(16) . . ?
Cl5A C23 Cl6A 85.2(12) 2_755 . ?
Cl6B C23 Cl6A 111.2(9) 2_755 . ?
Cl7B C23 Cl6A 110.8(9) 2_755 2_755 ?
Cl7B C23 Cl6A 57.5(9) . 2_755 ?
Cl5A C23 Cl6A 85.2(12) . 2_755 ?
Cl5A C23 Cl6A 88.2(16) 2_755 2_755 ?
Cl6B C23 Cl6A 111.2(9) . 2_755 ?
Cl6A C23 Cl6A 137.7(7) . 2_755 ?
Cl7B C23 Cl7A 135.3(8) 2_755 . ?
Cl5A C23 Cl7A 64.1(14) . . ?
Cl5A C23 Cl7A 112.2(16) 2_755 . ?
Cl6B C23 Cl7A 101.3(10) . . ?
Cl6B C23 Cl7A 67.1(9) 2_755 . ?
Cl6A C23 Cl7A 140.9(6) . . ?
Cl7B C23 Cl7A 135.3(8) . 2_755 ?
Cl5A C23 Cl7A 112.2(16) . 2_755 ?
Cl5A C23 Cl7A 64.1(14) 2_755 2_755 ?
Cl6B C23 Cl7A 67.1(9) . 2_755 ?
Cl6B C23 Cl7A 101.3(10) 2_755 2_755 ?
Cl6A C23 Cl7A 140.9(6) 2_755 2_755 ?
Cl7A C23 Cl7A 158.7(9) . 2_755 ?
Cl7B C23 Cl5B 121.7(8) 2_755 . ?
Cl7B C23 Cl5B 45.9(10) . . ?
Cl5A C23 Cl5B 145.1(11) 2_755 . ?
Cl6B C23 Cl5B 123.3(7) 2_755 . ?
Cl6A C23 Cl5B 66.6(4) . . ?
Cl6A C23 Cl5B 98.8(4) 2_755 . ?
Cl7A C23 Cl5B 81.8(6) . . ?
Cl7A C23 Cl5B 91.0(6) 2_755 . ?
Cl7B C23 Cl5B 45.9(10) 2_755 2_755 ?
Cl7B C23 Cl5B 121.7(8) . 2_755 ?
Cl5A C23 Cl5B 145.1(11) . 2_755 ?
Cl6B C23 Cl5B 123.3(7) . 2_755 ?
Cl6A C23 Cl5B 98.8(4) . 2_755 ?
Cl6A C23 Cl5B 66.6(4) 2_755 2_755 ?
Cl7A C23 Cl5B 91.0(6) . 2_755 ?
Cl7A C23 Cl5B 81.8(6) 2_755 2_755 ?
Cl5B C23 Cl5B 140.4(8) . 2_755 ?
Cl7B C23 H23 104.6 2_755 . ?
Cl7B C23 H23 104.6 . . ?
Cl5A C23 H23 99.1 . . ?
Cl5A C23 H23 99.1 2_755 . ?
Cl6B C23 H23 121.4 . . ?
Cl6B C23 H23 121.4 2_755 . ?
Cl6A C23 H23 111.2 . . ?
Cl6A C23 H23 111.2 2_755 . ?
Cl7A C23 H23 100.7 . . ?
Cl7A C23 H23 100.7 2_755 . ?
Cl5B C23 H23 109.8 . . ?
Cl5B C23 H23 109.8 2_755 . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.635
_refine_diff_density_min         -1.108
_refine_diff_density_rms         0.095