# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
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#  except for the purpose of generating routine backup copies
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#  from this site to visualise CIF-encoded structures and 
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data_crystal1

_audit_update_record             
;
2013-07-31 # Formatted by publCIF
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            '[Ru(CN)6][bipy2M2]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H50 N10, C6 N6 Ru, 10(H2 O)'
_chemical_formula_sum            'C40 H70 N16 O10 Ru'
_chemical_formula_weight         1036.19

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'
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   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'


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

_cell_length_a                   18.4060(4)
_cell_length_b                   14.9168(4)
_cell_length_c                   20.8645(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 121.577(2)
_cell_angle_gamma                90.00
_cell_volume                     4880.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    10385
_cell_measurement_theta_min      2.2869
_cell_measurement_theta_max      29.3951

_exptl_crystal_description       well-shaped
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2184
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_T_min  0.9125
_exptl_absorpt_correction_T_max  0.9454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
    Crystal obtained from potentiometry samples, initially 
at basic pH (c.a. 11). The original mix contained 22.97mg
of the ligand (FW 1146.83) and 17.59mg of K2[Ru(CN)6]
along with 30ml of 0.15M NaCl water solution. The vessel
was left open to the environment and crystals appeared
in 1 week time. When the crystals were measured with XRD
the vessel had pH = 7.
;

_diffrn_ambient_temperature      120(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, Gemini'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measurement_method       ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27703
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0759
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         27.50
_reflns_number_total             10802
_reflns_number_gt                6209
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_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. 
;

_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^)+(0.0580P)^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         10802
_refine_ls_number_parameters     735
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0377
_refine_ls_wR_factor_ref         0.1030
_refine_ls_wR_factor_gt          0.0969
_refine_ls_goodness_of_fit_ref   0.884
_refine_ls_restrained_S_all      0.890
_refine_ls_shift/su_max          0.004
_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
N4 N 0.33378(14) 0.56963(18) 0.61727(12) 0.0167(6) Uani 1 1 d . . .
N5 N 0.36223(14) 0.54599(18) 0.46114(12) 0.0158(5) Uani 1 1 d . . .
N6 N 0.45820(14) 0.26992(17) 0.62864(12) 0.0149(5) Uani 1 1 d . . .
H6C H 0.3996 0.2669 0.6025 0.018 Uiso 1 1 calc R . .
H6D H 0.4751 0.3109 0.6669 0.018 Uiso 1 1 calc R . .
N7 N 0.36864(17) 0.1524(2) 0.67058(16) 0.0307(7) Uani 1 1 d . . .
N8 N 0.22319(17) 0.2603(2) 0.62720(17) 0.0219(6) Uani 1 1 d . . .
H8C H 0.266(2) 0.297(3) 0.6503(18) 0.029(10) Uiso 1 1 d . . .
H8D H 0.2256(16) 0.247(2) 0.5882(16) 0.013(8) Uiso 1 1 d . . .
N12 N 0.11501(14) 0.54927(19) 0.48834(12) 0.0167(6) Uani 1 1 d . . .
N13 N 0.18244(14) 0.40268(18) 0.39360(13) 0.0181(6) Uani 1 1 d . . .
N1 N 0.09138(17) 0.70334(19) 0.26337(14) 0.0182(6) Uani 1 1 d . . .
H1C H 0.146(2) 0.710(2) 0.3011(19) 0.033(10) Uiso 1 1 d . . .
H1D H 0.057(2) 0.705(3) 0.2812(19) 0.045(12) Uiso 1 1 d . . .
N2 N 0.14773(14) 0.88886(19) 0.31120(13) 0.0206(6) Uani 1 1 d . . .
N3 N 0.24424(17) 0.85363(19) 0.46990(14) 0.0164(6) Uani 1 1 d . . .
H3C H 0.2038(19) 0.821(2) 0.4595(15) 0.012(8) Uiso 1 1 d . . .
H3D H 0.268(2) 0.835(2) 0.4462(17) 0.024(9) Uiso 1 1 d . . .
C1 C 0.08558(18) 0.6144(2) 0.22913(15) 0.0204(7) Uani 1 1 d . . .
H1A H 0.1186 0.6156 0.2040 0.024 Uiso 1 1 calc R . .
H1B H 0.0253 0.6019 0.1904 0.024 Uiso 1 1 calc R . .
C2 C 0.0677(2) 0.7791(3) 0.20905(18) 0.0300(9) Uani 1 1 d . . .
H2A H 0.113(2) 0.778(3) 0.1948(17) 0.036 Uiso 1 1 d . . .
H2B H 0.010(2) 0.765(2) 0.1653(18) 0.031(9) Uiso 1 1 d . . .
C3 C 0.06476(19) 0.8661(2) 0.24488(18) 0.0304(9) Uani 1 1 d . . .
H3A H 0.0465 0.9150 0.2075 0.036 Uiso 1 1 calc R . .
H3B H 0.0220 0.8609 0.2598 0.036 Uiso 1 1 calc R . .
C5 C 0.1356(2) 0.9437(3) 0.36337(18) 0.0239(8) Uani 1 1 d . . .
H5A H 0.0912(19) 0.918(2) 0.3703(16) 0.026(9) Uiso 1 1 d . . .
H5B H 0.122(2) 1.001(3) 0.346(2) 0.040(11) Uiso 1 1 d . . .
C6 C 0.21288(18) 0.9463(2) 0.44251(17) 0.0223(7) Uani 1 1 d . . .
H6A H 0.2587 0.9819 0.4431 0.025(9) Uiso 1 1 calc R . .
H6B H 0.1977 0.9758 0.4764 0.022(9) Uiso 1 1 calc R . .
C7 C 0.30559(19) 0.8476(2) 0.55297(16) 0.0185(7) Uani 1 1 d . . .
H7A H 0.2740(18) 0.883(2) 0.5759(16) 0.028(9) Uiso 1 1 d . . .
H7B H 0.3561(19) 0.875(2) 0.5633(16) 0.025(9) Uiso 1 1 d . . .
C10 C 0.31810(16) 0.7509(2) 0.57698(15) 0.0158(6) Uani 1 1 d . . .
C11 C 0.34554(17) 0.6881(2) 0.54552(15) 0.0164(7) Uani 1 1 d . . .
H11 H 0.3603 0.7064 0.5102 0.017(8) Uiso 1 1 calc R . .
C9 C 0.29878(17) 0.7209(2) 0.62984(15) 0.0189(7) Uani 1 1 d . . .
H9 H 0.2792 0.7615 0.6526 0.023 Uiso 1 1 calc R . .
C8 C 0.30876(17) 0.6316(2) 0.64819(16) 0.0196(7) Uani 1 1 d . . .
H8 H 0.2998(17) 0.603(2) 0.6849(16) 0.021(8) Uiso 1 1 d . . .
C4 C 0.20084(19) 0.9356(3) 0.28913(18) 0.0296(8) Uani 1 1 d . . .
H4A H 0.2082 0.8978 0.2545 0.044 Uiso 1 1 calc R . .
H4B H 0.2567 0.9483 0.3339 0.044 Uiso 1 1 calc R . .
H4C H 0.1733 0.9920 0.2641 0.044 Uiso 1 1 calc R . .
C12 C 0.35161(16) 0.5980(2) 0.56555(14) 0.0149(6) Uani 1 1 d . . .
C13 C 0.37826(16) 0.5295(2) 0.53096(15) 0.0140(6) Uani 1 1 d . . .
C17 C 0.38541(18) 0.4827(2) 0.42966(17) 0.0191(8) Uani 1 1 d . . .
H17 H 0.371(2) 0.496(2) 0.3783(19) 0.027(9) Uiso 1 1 d . . .
C16 C 0.42438(17) 0.4033(2) 0.46472(16) 0.0183(7) Uani 1 1 d . . .
H16 H 0.4377(19) 0.359(2) 0.4347(17) 0.030(9) Uiso 1 1 d . . .
C15 C 0.44135(16) 0.3869(2) 0.53666(15) 0.0140(6) Uani 1 1 d . . .
C18 C 0.48575(19) 0.3018(2) 0.57720(18) 0.0173(7) Uani 1 1 d . . .
H18A H 0.4776(18) 0.255(2) 0.5474(17) 0.023(9) Uiso 1 1 d . . .
H18B H 0.5427(19) 0.307(2) 0.6052(16) 0.017(8) Uiso 1 1 d . . .
C19 C 0.4938(2) 0.1801(2) 0.66198(19) 0.0204(7) Uani 1 1 d . . .
H19A H 0.480(2) 0.143(3) 0.6257(19) 0.033(10) Uiso 1 1 d . . .
H19B H 0.551(2) 0.190(2) 0.6906(18) 0.030(9) Uiso 1 1 d . . .
C20 C 0.46251(19) 0.1525(2) 0.71261(17) 0.0274(8) Uani 1 1 d . . .
H20A H 0.4840 0.0918 0.7328 0.033 Uiso 1 1 calc R . .
H20B H 0.4845 0.1946 0.7555 0.033 Uiso 1 1 calc R . .
C21 C 0.3342(2) 0.0733(3) 0.6200(2) 0.0417(10) Uani 1 1 d . . .
H21A H 0.3581 0.0714 0.5877 0.063 Uiso 1 1 calc R . .
H21B H 0.2719 0.0779 0.5887 0.063 Uiso 1 1 calc R . .
H21C H 0.3498 0.0185 0.6503 0.063 Uiso 1 1 calc R . .
C22 C 0.3334(2) 0.1557(3) 0.7173(2) 0.0399(10) Uani 1 1 d U . .
H22A H 0.3638 0.2018 0.7567 0.048 Uiso 1 1 calc R . .
H22B H 0.3420 0.0971 0.7425 0.048 Uiso 1 1 calc R . .
C23 C 0.2393(2) 0.1775(3) 0.6726(2) 0.0254(8) Uani 1 1 d U . .
H23A H 0.208(2) 0.135(3) 0.6401(18) 0.033(10) Uiso 1 1 d . . .
H23B H 0.220(2) 0.191(3) 0.7083(19) 0.041(10) Uiso 1 1 d . . .
C24 C 0.13908(17) 0.3015(2) 0.60404(17) 0.0217(7) Uani 1 1 d . . .
H24A H 0.1358 0.3132 0.6492 0.026 Uiso 1 1 calc R . .
H24B H 0.0927 0.2594 0.5712 0.026 Uiso 1 1 calc R . .
C25 C 0.10605(17) 0.5457(2) 0.54788(16) 0.0209(7) Uani 1 1 d . . .
H25 H 0.0935 0.5999 0.5640 0.025 Uiso 1 1 calc R . .
C26 C 0.11389(18) 0.4684(2) 0.58754(17) 0.0204(7) Uani 1 1 d . . .
H26 H 0.1023(19) 0.468(2) 0.6299(17) 0.028(9) Uiso 1 1 d . . .
C27 C 0.12755(16) 0.3877(2) 0.56276(15) 0.0174(7) Uani 1 1 d . . .
C28 C 0.13223(16) 0.3893(2) 0.49835(15) 0.0161(7) Uani 1 1 d . . .
H28 H 0.1379 0.3350 0.4776 0.019 Uiso 1 1 calc R . .
C29 C 0.12854(16) 0.4703(2) 0.46464(15) 0.0154(7) Uani 1 1 d . . .
C30 C 0.14031(16) 0.4722(2) 0.39936(15) 0.0144(7) Uani 1 1 d . . .
C34 C 0.19144(18) 0.4010(2) 0.33349(16) 0.0203(7) Uani 1 1 d . . .
H34 H 0.2197 0.3513 0.3276 0.024 Uiso 1 1 calc R . .
C33 C 0.16160(18) 0.4682(2) 0.28004(16) 0.0191(7) Uani 1 1 d . . .
H33 H 0.1703 0.4647 0.2391 0.023 Uiso 1 1 calc R . .
C32 C 0.11902(16) 0.5404(2) 0.28663(15) 0.0148(6) Uani 1 1 d . . .
C31 C 0.10715(16) 0.5418(2) 0.34735(15) 0.0161(6) Uani 1 1 d . . .
H31 H 0.0769 0.5896 0.3531 0.019 Uiso 1 1 calc R . .
C14 C 0.41885(16) 0.4518(2) 0.57022(15) 0.0160(7) Uani 1 1 d . . .
H14 H 0.4311 0.4435 0.6201 0.019 Uiso 1 1 calc R . .
Ru1 Ru 0.5000 0.0000 0.5000 0.01084(9) Uani 1 2 d S . .
N36 N 0.62735(14) 0.16649(18) 0.57071(13) 0.0177(6) Uani 1 1 d . . .
N35 N 0.52448(15) -0.0537(2) 0.65901(13) 0.0227(6) Uani 1 1 d . . .
N37 N 0.34241(15) 0.12947(19) 0.45608(13) 0.0226(6) Uani 1 1 d . . .
C36 C 0.58082(16) 0.1057(2) 0.54564(14) 0.0144(6) Uani 1 1 d . . .
C35 C 0.51572(17) -0.0325(2) 0.60200(16) 0.0166(6) Uani 1 1 d . . .
C37 C 0.39960(17) 0.0817(2) 0.47287(15) 0.0158(7) Uani 1 1 d . . .
Ru2 Ru 0.0000 0.5000 0.0000 0.01382(9) Uani 1 2 d S . .
N39 N -0.09632(16) 0.6459(2) 0.04178(14) 0.0258(7) Uani 1 1 d . . .
N40 N -0.02751(14) 0.64541(19) -0.12367(13) 0.0199(6) Uani 1 1 d . . .
N38 N 0.18173(15) 0.5819(2) 0.11888(13) 0.0254(7) Uani 1 1 d . . .
C39 C -0.06126(17) 0.5912(2) 0.02886(15) 0.0180(7) Uani 1 1 d . . .
C40 C -0.01596(16) 0.5908(2) -0.07966(15) 0.0169(7) Uani 1 1 d . . .
C38 C 0.11617(18) 0.5525(2) 0.07537(16) 0.0186(7) Uani 1 1 d . . .
O1 O 0.11838(15) 0.7326(2) 0.43900(14) 0.0254(6) Uani 1 1 d . . .
H1E H 0.119(2) 0.687(3) 0.457(2) 0.031(12) Uiso 1 1 d . . .
H1F H 0.076(2) 0.755(3) 0.429(2) 0.039(12) Uiso 1 1 d . . .
O2 O 0.27293(13) 0.68444(18) 0.35087(12) 0.0195(5) Uani 1 1 d D . .
H2E H 0.292(2) 0.644(2) 0.3818(17) 0.041(12) Uiso 1 1 d D . .
H2F H 0.296(2) 0.7316(16) 0.3665(19) 0.035(12) Uiso 1 1 d D . .
O3 O 0.32363(12) 0.59129(17) 0.26035(11) 0.0287(6) Uani 1 1 d . . .
H3E H 0.3050(6) 0.6235(9) 0.2757(4) 0.034 Uiso 1 1 d R . .
H3F H 0.2816(12) 0.58917(18) 0.2205(11) 0.034 Uiso 1 1 d R . .
O4 O 0.33849(13) 0.09749(17) 0.19002(12) 0.0354(6) Uani 1 1 d D . .
H4E H 0.32874(19) 0.0512(7) 0.1648(4) 0.042 Uiso 1 1 d RD . .
H4F H 0.3776(6) 0.0812(3) 0.2309(6) 0.042 Uiso 1 1 d RD . .
O5 O 0.54041(13) 0.12865(17) 0.25371(12) 0.0319(6) Uani 1 1 d . . .
H5E H 0.5319(2) 0.1007(8) 0.2823(8) 0.038 Uiso 1 1 d R . .
H5F H 0.5849(12) 0.1075(6) 0.25842(18) 0.038 Uiso 1 1 d R . .
O6 O 0.04439(12) 0.20391(18) 0.21536(12) 0.0282(6) Uani 1 1 d D . .
H6E H 0.04676(14) 0.2472(9) 0.1965(4) 0.048(14) Uiso 1 1 d R . .
H6F H 0.0860(8) 0.20114(19) 0.2608(9) 0.068(15) Uiso 1 1 d RD . .
O7 O 0.0612(2) 0.7528(2) 0.05770(17) 0.0733(10) Uani 1 1 d D . .
H7C H 0.0140(7) 0.7249(5) 0.06024(18) 0.088 Uiso 1 1 d RD . .
H7D H 0.0939(5) 0.7014(8) 0.05737(17) 0.088 Uiso 1 1 d RD . .
O8 O 0.2870(3) 0.1695(3) 0.2953(2) 0.1161(17) Uani 1 1 d D . .
H8E H 0.2655(5) 0.1237(9) 0.2567(8) 0.139 Uiso 1 1 d RD . .
H8F H 0.3465(12) 0.1633(3) 0.3384(9) 0.139 Uiso 1 1 d R . .
O9 O 0.15887(14) 0.17640(17) 0.36147(12) 0.0288(6) Uani 1 1 d . . .
H9E H 0.2069(15) 0.1632(4) 0.3818(7) 0.055(14) Uiso 1 1 d R . .
H9F H 0.1419(5) 0.1622(5) 0.3947(10) 0.061(13) Uiso 1 1 d R . .
O10 O 0.28314(12) 0.26838(16) 0.51576(11) 0.0212(5) Uani 1 1 d D . .
H10E H 0.29298(19) 0.2275(6) 0.4934(4) 0.059(14) Uiso 1 1 d RD . .
H10F H 0.2589(4) 0.3056(6) 0.4818(5) 0.049(13) Uiso 1 1 d RD . .

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
N4 0.0159(11) 0.0158(16) 0.0171(12) 0.0016(11) 0.0076(10) 0.0002(11)
N5 0.0170(12) 0.0137(16) 0.0176(12) -0.0013(11) 0.0097(10) -0.0019(11)
N6 0.0140(11) 0.0139(15) 0.0164(12) -0.0022(10) 0.0076(10) 0.0004(10)
N7 0.0346(15) 0.0227(19) 0.0402(17) 0.0097(14) 0.0233(14) 0.0094(13)
N8 0.0209(14) 0.0233(19) 0.0247(15) 0.0101(13) 0.0142(12) 0.0013(13)
N12 0.0151(11) 0.0176(17) 0.0154(12) -0.0011(11) 0.0066(10) -0.0003(11)
N13 0.0204(12) 0.0162(16) 0.0192(12) -0.0006(11) 0.0113(10) -0.0006(11)
N1 0.0163(13) 0.0181(17) 0.0162(13) 0.0021(11) 0.0057(11) -0.0010(11)
N2 0.0162(12) 0.0186(17) 0.0274(14) 0.0058(12) 0.0118(11) 0.0012(11)
N3 0.0172(13) 0.0130(16) 0.0228(13) 0.0005(12) 0.0130(12) -0.0010(12)
C1 0.0236(15) 0.020(2) 0.0168(15) -0.0015(13) 0.0102(12) -0.0005(14)
C2 0.0295(18) 0.025(2) 0.0229(17) 0.0121(15) 0.0051(15) 0.0008(16)
C3 0.0208(16) 0.020(2) 0.0354(19) 0.0119(16) 0.0045(14) 0.0023(15)
C5 0.0240(16) 0.019(2) 0.0338(18) 0.0097(16) 0.0186(15) 0.0049(15)
C6 0.0293(17) 0.0112(19) 0.0326(17) 0.0036(14) 0.0204(14) 0.0027(14)
C7 0.0198(15) 0.0160(19) 0.0223(16) -0.0028(14) 0.0129(13) -0.0008(14)
C10 0.0126(13) 0.0147(18) 0.0170(14) -0.0051(13) 0.0055(11) -0.0023(12)
C11 0.0178(14) 0.0182(19) 0.0139(14) 0.0010(13) 0.0089(12) 0.0003(13)
C9 0.0182(14) 0.019(2) 0.0195(15) -0.0049(13) 0.0098(12) 0.0000(13)
C8 0.0204(15) 0.024(2) 0.0171(15) -0.0001(14) 0.0121(13) 0.0013(14)
C4 0.0272(16) 0.036(2) 0.0289(18) 0.0095(16) 0.0170(14) 0.0011(16)
C12 0.0121(13) 0.0152(18) 0.0134(14) -0.0008(12) 0.0039(11) 0.0008(12)
C13 0.0144(13) 0.0120(18) 0.0169(14) -0.0043(12) 0.0091(12) -0.0038(12)
C17 0.0208(15) 0.019(2) 0.0160(15) -0.0031(13) 0.0090(12) -0.0027(13)
C16 0.0201(14) 0.0169(19) 0.0210(15) -0.0033(14) 0.0128(13) 0.0007(14)
C15 0.0127(13) 0.0113(17) 0.0181(14) -0.0001(12) 0.0081(11) -0.0016(12)
C18 0.0177(15) 0.016(2) 0.0209(15) -0.0007(14) 0.0120(13) 0.0005(13)
C19 0.0225(17) 0.016(2) 0.0231(17) 0.0012(15) 0.0118(14) 0.0039(14)
C20 0.0314(17) 0.021(2) 0.0292(18) 0.0033(15) 0.0155(14) 0.0028(15)
C21 0.043(2) 0.038(3) 0.043(2) -0.0007(19) 0.0213(18) -0.0032(19)
C22 0.043(2) 0.039(3) 0.042(2) 0.0128(19) 0.0245(18) 0.0091(19)
C23 0.0239(16) 0.022(2) 0.0311(19) 0.0108(16) 0.0146(15) -0.0004(15)
C24 0.0201(15) 0.023(2) 0.0256(16) 0.0055(14) 0.0144(13) 0.0000(14)
C25 0.0183(14) 0.025(2) 0.0197(15) -0.0056(15) 0.0104(13) 0.0028(14)
C26 0.0201(15) 0.026(2) 0.0164(15) -0.0015(14) 0.0105(13) -0.0006(14)
C27 0.0111(13) 0.022(2) 0.0187(14) 0.0007(13) 0.0077(11) -0.0028(13)
C28 0.0147(13) 0.0158(19) 0.0181(14) -0.0024(13) 0.0087(12) 0.0010(12)
C29 0.0110(13) 0.0182(19) 0.0130(14) 0.0007(13) 0.0036(11) -0.0013(12)
C30 0.0124(13) 0.0142(18) 0.0155(14) -0.0041(12) 0.0064(11) -0.0044(12)
C34 0.0238(15) 0.018(2) 0.0247(16) -0.0047(14) 0.0167(13) -0.0004(14)
C33 0.0214(14) 0.0202(19) 0.0185(15) -0.0049(13) 0.0124(12) -0.0054(14)
C32 0.0119(13) 0.0157(17) 0.0142(14) -0.0025(13) 0.0051(11) -0.0058(13)
C31 0.0147(13) 0.0147(18) 0.0182(14) -0.0043(13) 0.0083(12) -0.0007(13)
C14 0.0154(14) 0.0173(19) 0.0158(14) 0.0000(13) 0.0086(12) 0.0001(13)
Ru1 0.01002(14) 0.01117(19) 0.01152(15) -0.00082(15) 0.00578(12) -0.00083(15)
N36 0.0156(11) 0.0153(16) 0.0237(13) -0.0040(11) 0.0114(10) -0.0008(11)
N35 0.0254(13) 0.0243(18) 0.0194(13) 0.0008(12) 0.0124(11) -0.0015(12)
N37 0.0183(12) 0.0211(17) 0.0279(14) -0.0024(12) 0.0118(11) 0.0022(12)
C36 0.0136(13) 0.0184(19) 0.0129(13) 0.0022(13) 0.0082(11) 0.0038(13)
C35 0.0134(13) 0.0155(17) 0.0203(15) -0.0030(13) 0.0084(12) -0.0012(12)
C37 0.0176(14) 0.0151(19) 0.0161(14) -0.0031(13) 0.0097(12) -0.0057(13)
Ru2 0.01109(15) 0.0197(2) 0.01174(15) -0.00064(16) 0.00672(12) -0.00094(15)
N39 0.0242(13) 0.0266(19) 0.0307(15) -0.0031(13) 0.0172(12) -0.0014(13)
N40 0.0195(12) 0.0231(18) 0.0189(13) -0.0001(12) 0.0112(11) -0.0001(11)
N38 0.0188(13) 0.038(2) 0.0210(13) -0.0045(13) 0.0113(11) -0.0059(13)
C39 0.0141(13) 0.026(2) 0.0116(14) 0.0031(13) 0.0052(12) -0.0042(14)
C40 0.0090(12) 0.024(2) 0.0178(15) -0.0059(14) 0.0069(11) -0.0015(13)
C38 0.0191(15) 0.024(2) 0.0178(15) 0.0019(14) 0.0131(13) 0.0004(14)
O1 0.0186(12) 0.0180(16) 0.0346(14) 0.0052(12) 0.0104(11) -0.0001(11)
O2 0.0188(11) 0.0142(15) 0.0202(12) -0.0003(11) 0.0067(9) -0.0027(11)
O3 0.0217(10) 0.0442(18) 0.0192(11) -0.0048(11) 0.0100(9) 0.0001(11)
O4 0.0312(12) 0.0287(16) 0.0278(12) -0.0096(11) 0.0027(10) 0.0090(11)
O5 0.0275(11) 0.0402(18) 0.0340(13) 0.0212(12) 0.0202(10) 0.0095(11)
O6 0.0234(12) 0.0358(17) 0.0224(12) 0.0079(12) 0.0100(10) -0.0016(11)
O7 0.091(2) 0.061(3) 0.081(2) -0.0085(19) 0.0537(19) -0.0051(19)
O8 0.185(4) 0.106(4) 0.107(3) 0.056(3) 0.110(3) 0.064(3)
O9 0.0238(12) 0.0370(18) 0.0250(12) 0.0020(11) 0.0124(10) 0.0035(11)
O10 0.0199(10) 0.0203(14) 0.0189(10) 0.0020(11) 0.0071(9) 0.0029(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
N4 C8 1.339(4) . ?
N4 C12 1.350(4) . ?
N5 C17 1.341(4) . ?
N5 C13 1.349(4) . ?
N6 C18 1.485(4) . ?
N6 C19 1.493(4) . ?
N6 H6C 0.9200 . ?
N6 H6D 0.9200 . ?
N7 C22 1.426(4) . ?
N7 C20 1.472(4) . ?
N7 C21 1.486(5) . ?
N8 C23 1.489(4) . ?
N8 C24 1.492(4) . ?
N8 H8C 0.87(4) . ?
N8 H8D 0.86(3) . ?
N12 C25 1.337(4) . ?
N12 C29 1.350(4) . ?
N13 C30 1.338(4) . ?
N13 C34 1.349(4) . ?
N1 C1 1.484(4) . ?
N1 C2 1.495(4) . ?
N1 H1C 0.90(3) . ?
N1 H1D 0.88(4) . ?
N2 C4 1.458(4) . ?
N2 C3 1.466(4) . ?
N2 C5 1.469(4) . ?
N3 C6 1.492(4) . ?
N3 C7 1.496(4) . ?
N3 H3C 0.82(3) . ?
N3 H3D 0.86(3) . ?
C1 C32 1.504(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.512(5) . ?
C2 H2A 1.02(3) . ?
C2 H2B 1.00(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C5 C6 1.514(4) . ?
C5 H5A 0.98(3) . ?
C5 H5B 0.91(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C10 1.504(4) . ?
C7 H7A 1.07(3) . ?
C7 H7B 0.93(3) . ?
C10 C11 1.382(4) . ?
C10 C9 1.398(4) . ?
C11 C12 1.394(4) . ?
C11 H11 0.9500 . ?
C9 C8 1.372(5) . ?
C9 H9 0.9500 . ?
C8 H8 0.96(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C12 C13 1.475(4) . ?
C13 C14 1.390(4) . ?
C17 C16 1.380(4) . ?
C17 H17 0.98(3) . ?
C16 C15 1.385(4) . ?
C16 H16 1.02(3) . ?
C15 C14 1.380(4) . ?
C15 C18 1.507(4) . ?
C18 H18A 0.90(3) . ?
C18 H18B 0.90(3) . ?
C19 C20 1.502(4) . ?
C19 H19A 0.86(4) . ?
C19 H19B 0.91(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.512(5) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.89(4) . ?
C23 H23B 1.00(4) . ?
C24 C27 1.499(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.382(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.384(5) . ?
C26 H26 1.01(3) . ?
C27 C28 1.391(4) . ?
C28 C29 1.382(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.487(4) . ?
C30 C31 1.391(4) . ?
C34 C33 1.381(4) . ?
C34 H34 0.9500 . ?
C33 C32 1.381(4) . ?
C33 H33 0.9500 . ?
C32 C31 1.394(4) . ?
C31 H31 0.9500 . ?
C14 H14 0.9500 . ?
Ru1 C36 2.031(3) . ?
Ru1 C36 2.031(3) 3_656 ?
Ru1 C37 2.031(3) 3_656 ?
Ru1 C37 2.031(3) . ?
Ru1 C35 2.050(3) 3_656 ?
Ru1 C35 2.050(3) . ?
N36 C36 1.166(4) . ?
N35 C35 1.157(4) . ?
N37 C37 1.163(4) . ?
Ru2 C38 2.034(3) 3_565 ?
Ru2 C38 2.034(3) . ?
Ru2 C40 2.043(3) 3_565 ?
Ru2 C40 2.043(3) . ?
Ru2 C39 2.049(3) 3_565 ?
Ru2 C39 2.049(3) . ?
N39 C39 1.156(4) . ?
N40 C40 1.161(4) . ?
N38 C38 1.151(4) . ?
O1 H1E 0.77(4) . ?
O1 H1F 0.78(4) . ?
O1 H1E 0.77(4) . ?
O1 H1F 0.78(4) . ?
O2 H2E 0.817(18) . ?
O2 H2F 0.800(19) . ?
O3 H3E 0.7515 . ?
O3 H3F 0.7857 . ?
O4 H4E 0.8280 . ?
O4 H4F 0.8130 . ?
O5 H5E 0.8074 . ?
O5 H5F 0.8342 . ?
O6 H6E 0.7702 . ?
O6 H6F 0.8526 . ?
O6 H6E 0.7702 . ?
O6 H6F 0.8526 . ?
O7 H7D 0.9773 . ?
O7 H7C 0.9903 . ?
O7 H7C 0.9903 . ?
O7 H7D 0.9773 . ?
O8 H8E 0.9685 . ?
O8 H8F 0.9928 . ?
O8 H8E 0.9685 . ?
O8 H8F 0.9928 . ?
O9 H9E 0.7791 . ?
O9 H9F 0.9215 . ?
O10 H10F 0.8232 . ?
O10 H10E 0.8435 . ?
O10 H10E 0.8435 . ?
O10 H10F 0.8232 . ?

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
C8 N4 C12 117.2(3) . . ?
C17 N5 C13 117.1(3) . . ?
C18 N6 C19 113.0(2) . . ?
C18 N6 H6C 109.0 . . ?
C19 N6 H6C 109.0 . . ?
C18 N6 H6D 109.0 . . ?
C19 N6 H6D 109.0 . . ?
H6C N6 H6D 107.8 . . ?
C22 N7 C20 113.9(3) . . ?
C22 N7 C21 109.5(3) . . ?
C20 N7 C21 110.8(3) . . ?
C23 N8 C24 112.0(2) . . ?
C23 N8 H8C 111(2) . . ?
C24 N8 H8C 114(2) . . ?
C23 N8 H8D 109(2) . . ?
C24 N8 H8D 110.2(18) . . ?
H8C N8 H8D 101(3) . . ?
C25 N12 C29 116.2(3) . . ?
C30 N13 C34 117.2(3) . . ?
C1 N1 C2 113.1(3) . . ?
C1 N1 H1C 107(2) . . ?
C2 N1 H1C 109(2) . . ?
C1 N1 H1D 110(3) . . ?
C2 N1 H1D 108(3) . . ?
H1C N1 H1D 110(3) . . ?
C4 N2 C3 110.6(2) . . ?
C4 N2 C5 110.8(3) . . ?
C3 N2 C5 109.9(2) . . ?
C6 N3 C7 113.9(2) . . ?
C6 N3 H3C 110(2) . . ?
C7 N3 H3C 107(2) . . ?
C6 N3 H3D 107(2) . . ?
C7 N3 H3D 110(2) . . ?
H3C N3 H3D 109(3) . . ?
N1 C1 C32 112.1(2) . . ?
N1 C1 H1A 109.2 . . ?
C32 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
C32 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
N1 C2 C3 110.2(3) . . ?
N1 C2 H2A 104(2) . . ?
C3 C2 H2A 114(2) . . ?
N1 C2 H2B 106(2) . . ?
C3 C2 H2B 110(2) . . ?
H2A C2 H2B 112(3) . . ?
N2 C3 C2 112.1(3) . . ?
N2 C3 H3A 109.2 . . ?
C2 C3 H3A 109.2 . . ?
N2 C3 H3B 109.2 . . ?
C2 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
N2 C5 C6 113.7(3) . . ?
N2 C5 H5A 110.9(19) . . ?
C6 C5 H5A 103.2(17) . . ?
N2 C5 H5B 110(2) . . ?
C6 C5 H5B 108(2) . . ?
H5A C5 H5B 110(3) . . ?
N3 C6 C5 110.4(3) . . ?
N3 C6 H6A 109.6 . . ?
C5 C6 H6A 109.6 . . ?
N3 C6 H6B 109.6 . . ?
C5 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?
N3 C7 C10 109.6(2) . . ?
N3 C7 H7A 103.4(16) . . ?
C10 C7 H7A 110.7(18) . . ?
N3 C7 H7B 107.3(18) . . ?
C10 C7 H7B 113(2) . . ?
H7A C7 H7B 113(3) . . ?
C11 C10 C9 117.7(3) . . ?
C11 C10 C7 121.5(3) . . ?
C9 C10 C7 120.8(3) . . ?
C10 C11 C12 120.2(3) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C8 C9 C10 118.6(3) . . ?
C8 C9 H9 120.7 . . ?
C10 C9 H9 120.7 . . ?
N4 C8 C9 124.4(3) . . ?
N4 C8 H8 109(2) . . ?
C9 C8 H8 126(2) . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N4 C12 C11 121.8(3) . . ?
N4 C12 C13 117.2(3) . . ?
C11 C12 C13 121.0(3) . . ?
N5 C13 C14 122.3(3) . . ?
N5 C13 C12 117.5(3) . . ?
C14 C13 C12 120.2(3) . . ?
N5 C17 C16 123.7(3) . . ?
N5 C17 H17 114.7(19) . . ?
C16 C17 H17 121.6(19) . . ?
C17 C16 C15 119.0(3) . . ?
C17 C16 H16 116.8(18) . . ?
C15 C16 H16 124.1(18) . . ?
C14 C15 C16 118.0(3) . . ?
C14 C15 C18 121.7(3) . . ?
C16 C15 C18 120.3(3) . . ?
N6 C18 C15 112.7(2) . . ?
N6 C18 H18A 105(2) . . ?
C15 C18 H18A 115(2) . . ?
N6 C18 H18B 106.5(18) . . ?
C15 C18 H18B 113(2) . . ?
H18A C18 H18B 104(3) . . ?
N6 C19 C20 109.7(3) . . ?
N6 C19 H19A 108(2) . . ?
C20 C19 H19A 114(2) . . ?
N6 C19 H19B 104(2) . . ?
C20 C19 H19B 109(2) . . ?
H19A C19 H19B 113(3) . . ?
N7 C20 C19 110.1(3) . . ?
N7 C20 H20A 109.6 . . ?
C19 C20 H20A 109.6 . . ?
N7 C20 H20B 109.6 . . ?
C19 C20 H20B 109.6 . . ?
H20A C20 H20B 108.1 . . ?
N7 C21 H21A 109.5 . . ?
N7 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N7 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N7 C22 C23 111.7(3) . . ?
N7 C22 H22A 109.3 . . ?
C23 C22 H22A 109.3 . . ?
N7 C22 H22B 109.3 . . ?
C23 C22 H22B 109.3 . . ?
H22A C22 H22B 107.9 . . ?
N8 C23 C22 110.6(3) . . ?
N8 C23 H23A 106(2) . . ?
C22 C23 H23A 113(2) . . ?
N8 C23 H23B 106(2) . . ?
C22 C23 H23B 109.0(19) . . ?
H23A C23 H23B 111(3) . . ?
N8 C24 C27 110.5(2) . . ?
N8 C24 H24A 109.6 . . ?
C27 C24 H24A 109.6 . . ?
N8 C24 H24B 109.6 . . ?
C27 C24 H24B 109.6 . . ?
H24A C24 H24B 108.1 . . ?
N12 C25 C26 124.4(3) . . ?
N12 C25 H25 117.8 . . ?
C26 C25 H25 117.8 . . ?
C25 C26 C27 119.0(3) . . ?
C25 C26 H26 121(2) . . ?
C27 C26 H26 119(2) . . ?
C26 C27 C28 117.5(3) . . ?
C26 C27 C24 122.0(3) . . ?
C28 C27 C24 120.5(3) . . ?
C29 C28 C27 119.7(3) . . ?
C29 C28 H28 120.2 . . ?
C27 C28 H28 120.2 . . ?
N12 C29 C28 123.1(3) . . ?
N12 C29 C30 117.5(3) . . ?
C28 C29 C30 119.4(3) . . ?
N13 C30 C31 123.2(3) . . ?
N13 C30 C29 115.9(3) . . ?
C31 C30 C29 120.9(3) . . ?
N13 C34 C33 123.2(3) . . ?
N13 C34 H34 118.4 . . ?
C33 C34 H34 118.4 . . ?
C34 C33 C32 119.5(3) . . ?
C34 C33 H33 120.3 . . ?
C32 C33 H33 120.3 . . ?
C33 C32 C31 118.0(3) . . ?
C33 C32 C1 120.6(3) . . ?
C31 C32 C1 121.4(3) . . ?
C30 C31 C32 119.0(3) . . ?
C30 C31 H31 120.5 . . ?
C32 C31 H31 120.5 . . ?
C15 C14 C13 119.8(3) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C36 Ru1 C36 180.0 . 3_656 ?
C36 Ru1 C37 89.96(12) . 3_656 ?
C36 Ru1 C37 90.04(12) 3_656 3_656 ?
C36 Ru1 C37 90.05(12) . . ?
C36 Ru1 C37 89.95(12) 3_656 . ?
C37 Ru1 C37 179.997(1) 3_656 . ?
C36 Ru1 C35 88.48(11) . 3_656 ?
C36 Ru1 C35 91.52(11) 3_656 3_656 ?
C37 Ru1 C35 92.55(11) 3_656 3_656 ?
C37 Ru1 C35 87.45(11) . 3_656 ?
C36 Ru1 C35 91.52(11) . . ?
C36 Ru1 C35 88.48(11) 3_656 . ?
C37 Ru1 C35 87.45(11) 3_656 . ?
C37 Ru1 C35 92.55(11) . . ?
C35 Ru1 C35 179.999(1) 3_656 . ?
N36 C36 Ru1 178.8(2) . . ?
N35 C35 Ru1 177.9(3) . . ?
N37 C37 Ru1 178.4(3) . . ?
C38 Ru2 C38 180.0 3_565 . ?
C38 Ru2 C40 91.06(11) 3_565 3_565 ?
C38 Ru2 C40 88.93(11) . 3_565 ?
C38 Ru2 C40 88.94(11) 3_565 . ?
C38 Ru2 C40 91.07(11) . . ?
C40 Ru2 C40 180.0 3_565 . ?
C38 Ru2 C39 91.96(11) 3_565 3_565 ?
C38 Ru2 C39 88.04(11) . 3_565 ?
C40 Ru2 C39 86.10(12) 3_565 3_565 ?
C40 Ru2 C39 93.90(12) . 3_565 ?
C38 Ru2 C39 88.03(11) 3_565 . ?
C38 Ru2 C39 91.97(11) . . ?
C40 Ru2 C39 93.90(12) 3_565 . ?
C40 Ru2 C39 86.10(12) . . ?
C39 Ru2 C39 180.00(14) 3_565 . ?
N39 C39 Ru2 176.0(3) . . ?
N40 C40 Ru2 176.2(3) . . ?
N38 C38 Ru2 179.0(3) . . ?
H1E O1 H1F 104(4) . . ?
H1E O1 H1F 104(4) . . ?
H2E O2 H2F 115(4) . . ?
H3E O3 H3F 93.5 . . ?
H4E O4 H4F 101.3 . . ?
H5E O5 H5F 106.0 . . ?
H6E O6 H6F 110.6 . . ?
H7D O7 H7C 103.3 . . ?
H8E O8 H8F 117.7 . . ?
H9E O9 H9F 105.4 . . ?
H10F O10 H10E 100.8 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1C O2 0.90(3) 2.03(3) 2.862(3) 152(3) .
N1 H1D O6 0.88(4) 1.91(4) 2.757(3) 161(3) 2
N3 H3C O1 0.82(3) 1.92(3) 2.734(4) 173(3) .
N3 H3D N36 0.86(3) 2.13(3) 2.914(4) 151(3) 3_666
N6 H6D O5 0.92 1.81 2.693(3) 161.3 4_566
N6 H6C O10 0.92 1.95 2.825(3) 157.9 .
N8 H8C O4 0.87(4) 1.94(4) 2.794(4) 165(3) 4_566
N8 H8D O10 0.86(3) 2.28(3) 3.054(3) 151(3) .
O1 H1E N12 0.77(4) 2.17(4) 2.934(4) 170(4) .
O1 H1F N40 0.78(4) 2.20(4) 2.925(4) 155(4) 4_576
O2 H2E N5 0.817(18) 2.08(2) 2.881(3) 168(4) .
O2 H2F N36 0.800(19) 2.02(2) 2.801(4) 166(4) 3_666
O3 H3E O2 0.75 2.15 2.866(3) 160.5 .
O3 H3F N38 0.79 1.95 2.735(3) 176.4 .
O4 H4E N4 0.83 2.08 2.896(3) 167.0 4_565
O4 H4F N35 0.81 2.09 2.897(3) 173.0 3_656
O5 H5E N35 0.81 2.10 2.876(3) 161.9 3_656
O5 H5F O3 0.83 1.93 2.726(3) 158.3 2_645
O6 H6E N40 0.77 2.11 2.861(4) 167.0 3_565
O6 H6F O9 0.85 1.84 2.679(3) 166.2 .
O7 H7C N39 0.99 2.20 3.171(4) 166.3 .
O7 H7D N38 0.98 2.29 3.175(5) 149.6 .
O8 H8E O4 0.97 2.42 3.009(4) 118.9 .
O8 H8F N37 0.99 2.54 3.012(4) 108.6 .
O9 H9E N37 0.78 2.20 2.969(3) 170.8 .
O9 H9F N39 0.92 1.92 2.836(3) 172.4 2_545
O10 H10E N37 0.84 2.08 2.908(4) 168.5 .
O10 H10F N13 0.82 2.18 3.000(3) 173.5 .

_diffrn_measured_fraction_theta_max 0.963
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.963
_refine_diff_density_max         1.024
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.083
_database_code_depnum_ccdc_archive 'CCDC 953539'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_crystal2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            (H2bipy2M2)(ClO42)2
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H48 N10, 2(Cl O4), 4(H2 O)'
_chemical_formula_sum            'C34 H56 Cl2 N10 O12'
_chemical_formula_weight         867.79

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'
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           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   20.026(4)
_cell_length_b                   15.4487(19)
_cell_length_c                   14.706(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.555(17)
_cell_angle_gamma                90.00
_cell_volume                     4313.2(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    1186
_cell_measurement_theta_min      2.8412
_cell_measurement_theta_max      28.9633

_exptl_crystal_description       ?
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1840
_exptl_absorpt_coefficient_mu    0.220
_exptl_absorpt_correction_T_min  0.9649
_exptl_absorpt_correction_T_max  0.9811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           ?

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  
'SuperNova, Single source at offset), Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26286
_diffrn_reflns_av_R_equivalents  0.1110
_diffrn_reflns_av_sigmaI/netI    0.2110
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.85
_diffrn_reflns_theta_max         27.50
_reflns_number_total             9604
_reflns_number_gt                2326
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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. 
;

_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^)+(0.2000P)^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         9604
_refine_ls_number_parameters     539
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.3696
_refine_ls_R_factor_gt           0.1309
_refine_ls_wR_factor_ref         0.4729
_refine_ls_wR_factor_gt          0.3350
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_restrained_S_all      0.977
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3814(8) 0.3238(15) 0.7371(11) 0.159(6) Uani 1 1 d . . .
H1A H 0.4027 0.3218 0.8077 0.190 Uiso 1 1 calc R . .
H1B H 0.4203 0.3256 0.7092 0.190 Uiso 1 1 calc R . .
N1 N 0.3408(6) 0.4021(9) 0.7113(7) 0.128(3) Uani 1 1 d D . .
H1F H 0.304(4) 0.412(8) 0.731(8) 0.154 Uiso 1 1 d D . .
C2 C 0.3784(7) 0.4833(12) 0.7542(9) 0.158(6) Uani 1 1 d . . .
H2A H 0.3430 0.5274 0.7557 0.190 Uiso 1 1 calc R . .
H2B H 0.4073 0.4712 0.8213 0.190 Uiso 1 1 calc R . .
C3 C 0.4234(6) 0.5187(8) 0.7040(9) 0.134(4) Uani 1 1 d . . .
H3A H 0.4651 0.4809 0.7143 0.160 Uiso 1 1 calc R . .
H3B H 0.4401 0.5766 0.7304 0.160 Uiso 1 1 calc R . .
N2 N 0.3865(4) 0.5261(5) 0.6020(6) 0.095(2) Uani 1 1 d . . .
C4 C 0.4385(8) 0.5539(10) 0.5551(13) 0.200(7) Uani 1 1 d . . .
H4A H 0.4241 0.6097 0.5232 0.299 Uiso 1 1 calc R . .
H4B H 0.4408 0.5106 0.5075 0.299 Uiso 1 1 calc R . .
H4C H 0.4850 0.5598 0.6035 0.299 Uiso 1 1 calc R . .
C5 C 0.3267(7) 0.5859(7) 0.5758(8) 0.136(5) Uani 1 1 d . . .
H5A H 0.3093 0.5907 0.6316 0.163 Uiso 1 1 calc R . .
H5B H 0.3445 0.6436 0.5658 0.163 Uiso 1 1 calc R . .
C6 C 0.2723(7) 0.5680(6) 0.5001(15) 0.222(10) Uani 1 1 d U . .
H6A H 0.2786 0.5986 0.4442 0.266 Uiso 1 1 calc R . .
H6B H 0.2295 0.5919 0.5106 0.266 Uiso 1 1 calc R . .
N3 N 0.2598(4) 0.4753(5) 0.4752(9) 0.150(5) Uani 1 1 d . . .
H3X H 0.3020 0.4466 0.4999 0.180 Uiso 1 1 calc R . .
H3Y H 0.2298 0.4542 0.5061 0.180 Uiso 1 1 calc R . .
C7 C 0.2323(7) 0.4541(6) 0.3799(10) 0.117(4) Uani 1 1 d . . .
H7A H 0.2634 0.4775 0.3452 0.140 Uiso 1 1 calc R . .
H7B H 0.1855 0.4817 0.3530 0.140 Uiso 1 1 calc R . .
N4 N 0.2117(4) 0.1807(4) 0.3337(5) 0.0691(18) Uani 1 1 d . . .
C8 C 0.1608(5) 0.2348(7) 0.2883(7) 0.084(3) Uani 1 1 d . . .
H8 H 0.1188 0.2113 0.2451 0.101 Uiso 1 1 calc R . .
C9 C 0.1655(6) 0.3230(8) 0.3003(8) 0.099(3) Uani 1 1 d . . .
H9 H 0.1280 0.3594 0.2648 0.119 Uiso 1 1 calc R . .
C10 C 0.2248(6) 0.3577(5) 0.3638(7) 0.082(3) Uani 1 1 d . . .
C11 C 0.2787(5) 0.3012(6) 0.4145(6) 0.076(2) Uani 1 1 d . . .
H11 H 0.3203 0.3226 0.4603 0.091 Uiso 1 1 calc R . .
C12 C 0.2696(4) 0.2138(5) 0.3962(5) 0.063(2) Uani 1 1 d . . .
N5 N 0.3893(4) 0.1811(4) 0.4938(5) 0.0763(19) Uani 1 1 d . . .
C13 C 0.3248(4) 0.1492(5) 0.4483(5) 0.061(2) Uani 1 1 d . . .
C14 C 0.4385(5) 0.1242(7) 0.5378(6) 0.090(3) Uani 1 1 d . . .
H14 H 0.4848 0.1451 0.5684 0.108 Uiso 1 1 calc R . .
C15 C 0.4266(5) 0.0356(7) 0.5421(7) 0.090(3) Uani 1 1 d . . .
H15 H 0.4631 -0.0021 0.5773 0.108 Uiso 1 1 calc R . .
C16 C 0.3608(5) 0.0043(5) 0.4941(6) 0.070(2) Uani 1 1 d . . .
C17 C 0.3099(4) 0.0623(5) 0.4473(5) 0.061(2) Uani 1 1 d . . .
H17 H 0.2637 0.0423 0.4137 0.074 Uiso 1 1 calc R . .
C18 C 0.3472(5) -0.0920(6) 0.4908(6) 0.088(3) Uani 1 1 d . . .
H18A H 0.3707 -0.1199 0.4486 0.106 Uiso 1 1 calc R . .
H18B H 0.3674 -0.1166 0.5560 0.106 Uiso 1 1 calc R . .
N6 N 0.2728(4) -0.1100(4) 0.4554(5) 0.090(2) Uani 1 1 d D . .
H6C H 0.2535 -0.0789 0.3998 0.108 Uiso 1 1 calc RD . .
H6D H 0.2527 -0.0901 0.4997 0.108 Uiso 1 1 calc RD . .
C19 C 0.2535(6) -0.2015(6) 0.4355(8) 0.114(3) Uani 1 1 d . . .
H19A H 0.2629 -0.2336 0.4966 0.136 Uiso 1 1 calc R . .
H19B H 0.2822 -0.2276 0.3989 0.136 Uiso 1 1 calc R . .
C20 C 0.1773(6) -0.2076(6) 0.3790(9) 0.118(4) Uani 1 1 d . . .
H20A H 0.1491 -0.1865 0.4189 0.142 Uiso 1 1 calc R . .
H20B H 0.1650 -0.2691 0.3635 0.142 Uiso 1 1 calc R . .
N7 N 0.1582(4) -0.1565(5) 0.2878(7) 0.097(2) Uani 1 1 d D . .
C21 C 0.1952(8) -0.1911(7) 0.2215(10) 0.153(5) Uani 1 1 d . . .
H21A H 0.1971 -0.2545 0.2255 0.230 Uiso 1 1 calc R . .
H21B H 0.2432 -0.1679 0.2400 0.230 Uiso 1 1 calc R . .
H21C H 0.1695 -0.1736 0.1555 0.230 Uiso 1 1 calc R . .
C22 C 0.0817(6) -0.1569(7) 0.2367(11) 0.150(5) Uani 1 1 d . . .
H22A H 0.0724 -0.1220 0.1775 0.179 Uiso 1 1 calc R . .
H22B H 0.0667 -0.2170 0.2173 0.179 Uiso 1 1 calc R . .
C23 C 0.0397(6) -0.1235(8) 0.2918(11) 0.152(5) Uani 1 1 d D . .
H23A H 0.0399 -0.1649 0.3432 0.182 Uiso 1 1 calc R . .
H23B H -0.0095 -0.1159 0.2499 0.182 Uiso 1 1 calc R . .
N8 N 0.0687(5) -0.0386(6) 0.3349(8) 0.123(3) Uani 1 1 d D . .
H8F H 0.077(6) -0.0059(15) 0.290(4) 0.148 Uiso 1 1 d D . .
C24 C 0.0266(7) -0.0032(8) 0.3846(10) 0.139(5) Uani 1 1 d D . .
H24A H 0.0218 -0.0457 0.4325 0.167 Uiso 1 1 calc R . .
H24B H -0.0209 0.0080 0.3390 0.167 Uiso 1 1 calc R . .
N9 N 0.1236(7) 0.2336(6) 0.5346(7) 0.127(4) Uani 1 1 d . . .
C25 C 0.0586(10) 0.2323(8) 0.4774(10) 0.144(5) Uani 1 1 d . . .
H25 H 0.0330 0.2851 0.4671 0.173 Uiso 1 1 calc R . .
C26 C 0.0240(7) 0.1587(9) 0.4303(8) 0.127(4) Uani 1 1 d . . .
H26 H -0.0242 0.1629 0.3928 0.153 Uiso 1 1 calc R . .
C27 C 0.0569(9) 0.0819(10) 0.4362(11) 0.123(5) Uani 1 1 d . . .
C28 C 0.1258(10) 0.0820(7) 0.4957(11) 0.120(5) Uani 1 1 d . . .
H28 H 0.1526 0.0302 0.5045 0.144 Uiso 1 1 calc R . .
C29 C 0.1572(8) 0.1580(9) 0.5438(8) 0.100(4) Uani 1 1 d . . .
N10 N 0.2594(7) 0.0841(7) 0.6436(8) 0.138(4) Uani 1 1 d . . .
C30 C 0.3285(14) 0.0881(13) 0.7072(14) 0.170(9) Uani 1 1 d . . .
H30 H 0.3504 0.0344 0.7309 0.204 Uiso 1 1 calc R . .
C31 C 0.3676(10) 0.1610(14) 0.7387(13) 0.163(7) Uani 1 1 d . . .
H31 H 0.4136 0.1576 0.7839 0.195 Uiso 1 1 calc R . .
C32 C 0.3385(11) 0.2396(12) 0.7033(11) 0.141(6) Uani 1 1 d . . .
C35 C 0.2686(8) 0.2376(10) 0.6397(8) 0.115(4) Uani 1 1 d . . .
H35 H 0.2473 0.2913 0.6155 0.138 Uiso 1 1 calc R . .
C33 C 0.2276(11) 0.1611(9) 0.6093(11) 0.129(6) Uani 1 1 d . . .
Cl1 Cl 0.04920(15) 0.59517(19) 0.3914(2) 0.1016(10) Uani 1 1 d . . .
O11 O -0.0047(7) 0.6412(9) 0.3426(9) 0.259(7) Uani 1 1 d . . .
O12 O 0.0912(7) 0.5920(10) 0.3338(10) 0.264(7) Uani 1 1 d . . .
O13 O 0.0288(7) 0.5107(7) 0.3973(9) 0.273(8) Uani 1 1 d . . .
O14 O 0.0876(6) 0.6273(7) 0.4786(7) 0.198(4) Uani 1 1 d . . .
Cl2 Cl 0.6053(2) 0.1992(2) 0.2254(3) 0.1254(12) Uani 1 1 d . . .
O21 O 0.5590(11) 0.2348(14) 0.2672(17) 0.357(11) Uani 1 1 d . . .
O22 O 0.5782(7) 0.1196(7) 0.2124(11) 0.263(7) Uani 1 1 d . . .
O23 O 0.6687(6) 0.2045(10) 0.2882(13) 0.309(10) Uani 1 1 d . . .
O24 O 0.5943(7) 0.2513(11) 0.1561(11) 0.294(9) Uani 1 1 d . . .
O1 O 0.1865(3) 0.0140(4) 0.2368(4) 0.106(2) Uani 1 1 d D . .
H1D H 0.1947(4) 0.0619(8) 0.2658(6) 0.127 Uiso 1 1 d RD . .
H1E H 0.1745(4) 0.0327(5) 0.1838(9) 0.127 Uiso 1 1 d RD . .
O2 O 0.4428(6) 0.3610(7) 0.5368(8) 0.241(6) Uani 1 1 d D . .
H2E H 0.4267(6) 0.3078(11) 0.5243(8) 0.290 Uiso 1 1 d RD . .
H2D H 0.4753(8) 0.3665(7) 0.5795(10) 0.290 Uiso 1 1 d RD . .
O3 O 0.1425(4) 0.0818(4) 0.0524(4) 0.115(2) Uani 1 1 d D . .
H3D H 0.1141(6) 0.0586(5) 0.0141(7) 0.138 Uiso 1 1 d RD . .
H3E H 0.1367(4) 0.1380(10) 0.0471(4) 0.138 Uiso 1 1 d RD . .
O4 O 0.2080(10) 0.5920(7) 0.1392(8) 0.310(9) Uani 1 1 d D . .
H4D H 0.2287(10) 0.5474(10) 0.1604(9) 0.372 Uiso 1 1 d RD . .
H4E H 0.2439(11) 0.6251(8) 0.1611(9) 0.372 Uiso 1 1 d RD . .

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
C1 0.119(12) 0.25(2) 0.131(11) 0.060(14) 0.078(10) 0.068(14)
N1 0.103(8) 0.182(10) 0.114(7) 0.044(8) 0.055(6) 0.025(8)
C2 0.108(10) 0.253(18) 0.120(10) -0.037(11) 0.047(8) -0.051(11)
C3 0.106(9) 0.153(11) 0.123(10) -0.003(8) 0.009(8) -0.006(8)
N2 0.083(6) 0.092(5) 0.099(6) 0.006(5) 0.012(5) 0.001(5)
C4 0.184(16) 0.199(15) 0.243(18) 0.013(13) 0.107(14) -0.064(12)
C5 0.133(11) 0.078(7) 0.144(10) -0.031(7) -0.031(8) 0.013(7)
C6 0.118(11) 0.049(7) 0.40(3) -0.013(11) -0.050(14) 0.019(6)
N3 0.094(7) 0.055(5) 0.220(11) -0.024(6) -0.063(7) 0.023(4)
C7 0.154(11) 0.069(7) 0.153(11) 0.006(7) 0.083(10) 0.005(7)
N4 0.059(4) 0.066(4) 0.077(5) 0.005(4) 0.014(4) -0.002(4)
C8 0.060(6) 0.077(7) 0.107(7) 0.018(6) 0.015(5) 0.000(5)
C9 0.067(7) 0.108(9) 0.127(9) 0.022(7) 0.037(7) 0.014(6)
C10 0.123(9) 0.058(6) 0.097(7) 0.007(6) 0.080(7) 0.012(6)
C11 0.093(7) 0.066(6) 0.071(6) -0.017(5) 0.030(5) -0.002(5)
C12 0.057(5) 0.072(6) 0.067(5) -0.007(5) 0.031(4) 0.005(5)
N5 0.066(5) 0.080(5) 0.079(5) -0.005(4) 0.016(4) 0.011(4)
C13 0.065(6) 0.065(5) 0.055(5) -0.011(4) 0.022(4) -0.001(5)
C14 0.064(6) 0.099(8) 0.088(6) -0.005(6) -0.003(5) -0.004(6)
C15 0.065(6) 0.097(8) 0.095(7) 0.001(6) 0.007(5) 0.019(5)
C16 0.073(6) 0.064(5) 0.069(5) 0.000(5) 0.017(5) 0.014(5)
C17 0.052(5) 0.070(5) 0.058(5) -0.013(4) 0.012(4) 0.005(4)
C18 0.084(7) 0.076(6) 0.093(6) 0.023(5) 0.012(5) 0.022(5)
N6 0.110(7) 0.056(5) 0.101(5) 0.012(4) 0.027(5) 0.008(4)
C19 0.143(11) 0.067(7) 0.118(8) 0.017(6) 0.024(8) 0.021(7)
C20 0.111(9) 0.073(6) 0.163(11) 0.026(7) 0.034(8) -0.015(6)
N7 0.068(5) 0.067(5) 0.151(7) -0.004(5) 0.027(5) 0.005(4)
C21 0.186(13) 0.084(8) 0.191(12) -0.028(8) 0.062(11) -0.019(8)
C22 0.074(8) 0.099(9) 0.249(15) -0.040(9) 0.014(9) -0.010(7)
C23 0.081(8) 0.110(10) 0.268(16) -0.023(10) 0.060(10) -0.020(7)
N8 0.112(7) 0.100(7) 0.185(10) -0.017(6) 0.084(8) -0.012(6)
C24 0.169(12) 0.091(8) 0.188(13) -0.003(9) 0.100(11) -0.028(9)
N9 0.187(11) 0.102(7) 0.082(7) 0.022(5) 0.029(7) 0.080(8)
C25 0.226(18) 0.075(8) 0.110(10) 0.006(8) 0.024(10) 0.052(10)
C26 0.179(12) 0.090(8) 0.115(9) 0.029(8) 0.050(8) 0.058(9)
C27 0.143(12) 0.128(13) 0.140(11) 0.033(9) 0.102(10) 0.030(10)
C28 0.216(17) 0.056(7) 0.141(11) 0.012(7) 0.132(12) 0.033(9)
C29 0.132(10) 0.114(11) 0.065(7) 0.038(7) 0.046(7) 0.056(9)
N10 0.192(12) 0.136(9) 0.109(8) 0.025(7) 0.081(8) 0.084(9)
C30 0.25(3) 0.163(16) 0.137(14) 0.082(14) 0.126(16) 0.125(17)
C31 0.160(15) 0.191(16) 0.176(15) 0.044(15) 0.109(13) 0.098(15)
C32 0.166(15) 0.176(15) 0.119(11) 0.070(11) 0.098(12) 0.116(14)
C35 0.161(12) 0.138(12) 0.077(7) 0.051(8) 0.081(8) 0.085(10)
C33 0.240(18) 0.072(8) 0.125(11) 0.049(8) 0.131(13) 0.084(11)
Cl1 0.0795(18) 0.101(2) 0.116(2) 0.0183(18) 0.0187(17) 0.0017(15)
O11 0.201(12) 0.279(14) 0.225(11) 0.021(10) -0.033(9) 0.135(11)
O12 0.210(12) 0.371(18) 0.254(13) -0.094(13) 0.137(11) -0.099(12)
O13 0.335(17) 0.152(8) 0.238(12) 0.064(8) -0.044(11) -0.122(10)
O14 0.199(10) 0.207(10) 0.139(7) -0.036(7) -0.015(7) -0.026(8)
Cl2 0.115(3) 0.115(3) 0.127(3) 0.032(2) 0.011(2) -0.025(2)
O21 0.30(2) 0.38(3) 0.44(3) -0.10(2) 0.20(2) -0.080(17)
O22 0.249(14) 0.127(8) 0.346(17) -0.011(10) -0.002(12) -0.060(9)
O23 0.100(8) 0.334(16) 0.41(2) 0.225(16) -0.027(10) -0.047(9)
O24 0.210(13) 0.41(2) 0.282(15) 0.234(16) 0.103(11) 0.108(13)
O1 0.145(6) 0.073(4) 0.082(4) -0.003(3) 0.012(4) -0.016(4)
O2 0.201(11) 0.164(9) 0.288(13) 0.050(9) -0.023(10) -0.053(8)
O3 0.146(6) 0.100(5) 0.102(5) -0.016(4) 0.044(4) -0.037(4)
O4 0.52(3) 0.147(9) 0.209(11) -0.034(8) 0.034(13) -0.123(12)

_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
C1 N1 1.440(17) . ?
C1 C32 1.55(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
N1 C2 1.496(16) . ?
N1 H1F 0.89(2) . ?
C2 C3 1.442(15) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N2 1.450(12) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
N2 C5 1.464(12) . ?
N2 C4 1.485(13) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.315(15) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N3 1.480(12) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
N3 C7 1.372(13) . ?
N3 H3X 0.9200 . ?
N3 H3Y 0.9200 . ?
C7 C10 1.509(12) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
N4 C8 1.322(10) . ?
N4 C12 1.331(9) . ?
C8 C9 1.374(12) . ?
C8 H8 0.9500 . ?
C9 C10 1.366(12) . ?
C9 H9 0.9500 . ?
C10 C11 1.403(12) . ?
C11 C12 1.376(10) . ?
C11 H11 0.9500 . ?
C12 C13 1.505(11) . ?
N5 C14 1.324(10) . ?
N5 C13 1.346(9) . ?
C13 C17 1.375(10) . ?
C14 C15 1.394(12) . ?
C14 H14 0.9500 . ?
C15 C16 1.369(11) . ?
C15 H15 0.9500 . ?
C16 C17 1.367(10) . ?
C16 C18 1.511(11) . ?
C17 H17 0.9500 . ?
C18 N6 1.440(10) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
N6 C19 1.471(10) . ?
N6 H6C 0.9200 . ?
N6 H6D 0.9200 . ?
C19 C20 1.490(13) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 N7 1.497(12) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
N7 C22 1.476(12) . ?
N7 C21 1.500(13) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.436(15) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 N8 1.491(14) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
N8 C24 1.390(13) . ?
N8 H8F 0.89(2) . ?
C24 C27 1.542(17) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
N9 C25 1.306(16) . ?
N9 C29 1.333(13) . ?
C25 C26 1.395(16) . ?
C25 H25 0.9500 . ?
C26 C27 1.346(15) . ?
C26 H26 0.9500 . ?
C27 C28 1.380(16) . ?
C28 C29 1.411(16) . ?
C28 H28 0.9500 . ?
C29 C33 1.433(18) . ?
N10 C33 1.367(14) . ?
N10 C30 1.40(2) . ?
C30 C31 1.37(2) . ?
C30 H30 0.9500 . ?
C31 C32 1.375(19) . ?
C31 H31 0.9500 . ?
C32 C35 1.414(19) . ?
C35 C33 1.427(18) . ?
C35 H35 0.9500 . ?
Cl1 O11 1.301(9) . ?
Cl1 O14 1.362(9) . ?
Cl1 O12 1.371(11) . ?
Cl1 O13 1.378(9) . ?
Cl2 O24 1.261(11) . ?
Cl2 O23 1.313(12) . ?
Cl2 O22 1.334(10) . ?
Cl2 O21 1.381(19) . ?
O1 H1D 0.8447 . ?
O1 H1E 0.7935 . ?
O2 H2E 0.8794 . ?
O2 H2D 0.7521 . ?
O3 H3D 0.7521 . ?
O3 H3E 0.8755 . ?
O4 H4D 0.8145 . ?
O4 H4E 0.8575 . ?

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 C1 C32 114.3(13) . . ?
N1 C1 H1A 108.7 . . ?
C32 C1 H1A 108.7 . . ?
N1 C1 H1B 108.7 . . ?
C32 C1 H1B 108.7 . . ?
H1A C1 H1B 107.6 . . ?
C1 N1 C2 115.3(13) . . ?
C1 N1 H1F 121(8) . . ?
C2 N1 H1F 95(8) . . ?
C3 C2 N1 114.6(11) . . ?
C3 C2 H2A 108.6 . . ?
N1 C2 H2A 108.6 . . ?
C3 C2 H2B 108.6 . . ?
N1 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
C2 C3 N2 111.3(10) . . ?
C2 C3 H3A 109.4 . . ?
N2 C3 H3A 109.4 . . ?
C2 C3 H3B 109.4 . . ?
N2 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
C3 N2 C5 115.2(9) . . ?
C3 N2 C4 107.6(11) . . ?
C5 N2 C4 109.4(10) . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 N2 118.5(10) . . ?
C6 C5 H5A 107.7 . . ?
N2 C5 H5A 107.7 . . ?
C6 C5 H5B 107.7 . . ?
N2 C5 H5B 107.7 . . ?
H5A C5 H5B 107.1 . . ?
C5 C6 N3 116.2(10) . . ?
C5 C6 H6A 108.2 . . ?
N3 C6 H6A 108.2 . . ?
C5 C6 H6B 108.2 . . ?
N3 C6 H6B 108.2 . . ?
H6A C6 H6B 107.4 . . ?
C7 N3 C6 117.7(11) . . ?
C7 N3 H3X 107.9 . . ?
C6 N3 H3X 107.9 . . ?
C7 N3 H3Y 107.9 . . ?
C6 N3 H3Y 107.9 . . ?
H3X N3 H3Y 107.2 . . ?
N3 C7 C10 112.5(9) . . ?
N3 C7 H7A 109.1 . . ?
C10 C7 H7A 109.1 . . ?
N3 C7 H7B 109.1 . . ?
C10 C7 H7B 109.1 . . ?
H7A C7 H7B 107.8 . . ?
C8 N4 C12 117.9(7) . . ?
N4 C8 C9 123.5(9) . . ?
N4 C8 H8 118.3 . . ?
C9 C8 H8 118.3 . . ?
C10 C9 C8 119.1(9) . . ?
C10 C9 H9 120.5 . . ?
C8 C9 H9 120.5 . . ?
C9 C10 C11 118.3(9) . . ?
C9 C10 C7 121.1(11) . . ?
C11 C10 C7 120.6(11) . . ?
C12 C11 C10 118.3(8) . . ?
C12 C11 H11 120.8 . . ?
C10 C11 H11 120.8 . . ?
N4 C12 C11 122.9(8) . . ?
N4 C12 C13 115.7(7) . . ?
C11 C12 C13 121.4(8) . . ?
C14 N5 C13 116.6(7) . . ?
N5 C13 C17 122.2(7) . . ?
N5 C13 C12 116.4(7) . . ?
C17 C13 C12 121.4(7) . . ?
N5 C14 C15 124.2(8) . . ?
N5 C14 H14 117.9 . . ?
C15 C14 H14 117.9 . . ?
C16 C15 C14 118.2(8) . . ?
C16 C15 H15 120.9 . . ?
C14 C15 H15 120.9 . . ?
C17 C16 C15 118.0(8) . . ?
C17 C16 C18 122.1(8) . . ?
C15 C16 C18 119.8(8) . . ?
C16 C17 C13 120.7(8) . . ?
C16 C17 H17 119.7 . . ?
C13 C17 H17 119.7 . . ?
N6 C18 C16 110.9(7) . . ?
N6 C18 H18A 109.5 . . ?
C16 C18 H18A 109.5 . . ?
N6 C18 H18B 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
C18 N6 C19 115.7(8) . . ?
C18 N6 H6C 108.4 . . ?
C19 N6 H6C 108.4 . . ?
C18 N6 H6D 108.4 . . ?
C19 N6 H6D 108.4 . . ?
H6C N6 H6D 107.4 . . ?
N6 C19 C20 109.3(8) . . ?
N6 C19 H19A 109.8 . . ?
C20 C19 H19A 109.8 . . ?
N6 C19 H19B 109.8 . . ?
C20 C19 H19B 109.8 . . ?
H19A C19 H19B 108.3 . . ?
C19 C20 N7 113.0(8) . . ?
C19 C20 H20A 109.0 . . ?
N7 C20 H20A 109.0 . . ?
C19 C20 H20B 109.0 . . ?
N7 C20 H20B 109.0 . . ?
H20A C20 H20B 107.8 . . ?
C22 N7 C20 112.5(9) . . ?
C22 N7 C21 108.4(10) . . ?
C20 N7 C21 110.9(8) . . ?
N7 C21 H21A 109.5 . . ?
N7 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N7 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 N7 114.2(11) . . ?
C23 C22 H22A 108.7 . . ?
N7 C22 H22A 108.7 . . ?
C23 C22 H22B 108.7 . . ?
N7 C22 H22B 108.7 . . ?
H22A C22 H22B 107.6 . . ?
C22 C23 N8 109.8(9) . . ?
C22 C23 H23A 109.7 . . ?
N8 C23 H23A 109.7 . . ?
C22 C23 H23B 109.7 . . ?
N8 C23 H23B 109.7 . . ?
H23A C23 H23B 108.2 . . ?
C24 N8 C23 110.5(10) . . ?
C24 N8 H8F 117(4) . . ?
C23 N8 H8F 109(4) . . ?
N8 C24 C27 112.6(10) . . ?
N8 C24 H24A 109.1 . . ?
C27 C24 H24A 109.1 . . ?
N8 C24 H24B 109.1 . . ?
C27 C24 H24B 109.1 . . ?
H24A C24 H24B 107.8 . . ?
C25 N9 C29 114.8(12) . . ?
N9 C25 C26 124.6(12) . . ?
N9 C25 H25 117.7 . . ?
C26 C25 H25 117.7 . . ?
C27 C26 C25 122.1(14) . . ?
C27 C26 H26 119.0 . . ?
C25 C26 H26 119.0 . . ?
C26 C27 C28 114.2(15) . . ?
C26 C27 C24 127.7(16) . . ?
C28 C27 C24 118.1(13) . . ?
C27 C28 C29 121.1(12) . . ?
C27 C28 H28 119.5 . . ?
C29 C28 H28 119.5 . . ?
N9 C29 C28 123.2(13) . . ?
N9 C29 C33 113.4(13) . . ?
C28 C29 C33 123.4(13) . . ?
C33 N10 C30 117.0(16) . . ?
C31 C30 N10 126.8(17) . . ?
C31 C30 H30 116.6 . . ?
N10 C30 H30 116.6 . . ?
C30 C31 C32 118(2) . . ?
C30 C31 H31 120.9 . . ?
C32 C31 H31 120.9 . . ?
C31 C32 C35 116.2(19) . . ?
C31 C32 C1 119.6(19) . . ?
C35 C32 C1 124.1(13) . . ?
C32 C35 C33 125.1(14) . . ?
C32 C35 H35 117.5 . . ?
C33 C35 H35 117.5 . . ?
N10 C33 C35 116.8(17) . . ?
N10 C33 C29 117.6(16) . . ?
C35 C33 C29 125.6(12) . . ?
O11 Cl1 O14 116.2(8) . . ?
O11 Cl1 O12 104.1(10) . . ?
O14 Cl1 O12 108.7(8) . . ?
O11 Cl1 O13 110.0(9) . . ?
O14 Cl1 O13 112.0(7) . . ?
O12 Cl1 O13 104.9(10) . . ?
O24 Cl2 O23 114.3(9) . . ?
O24 Cl2 O22 120.9(11) . . ?
O23 Cl2 O22 114.6(8) . . ?
O24 Cl2 O21 97.8(12) . . ?
O23 Cl2 O21 107.3(13) . . ?
O22 Cl2 O21 97.5(10) . . ?
H1D O1 H1E 97.3 . . ?
H2E O2 H2D 116.3 . . ?
H3D O3 H3E 111.0 . . ?
H4D O4 H4E 95.5 . . ?

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
O1 H1D N4 0.84 2.07 2.910(8) 178.1 .
O1 H1E O3 0.79 1.98 2.776(9) 178.2 .
O2 H2E N5 0.88 2.09 2.973(12) 179.3 .
O2 H2D O22 0.75 2.36 3.108(17) 178.6 4_566
O3 H3D O13 0.75 2.27 3.021(13) 179.3 4_565
O3 H3E N9 0.88 2.00 2.877(12) 179.9 4_565
O4 H4E O23 0.86 2.07 2.930(19) 178.9 2_655
N1 H1F O1 0.89(2) 2.64(5) 3.478(12) 158(10) 4_566
N3 H3Y O3 0.92 2.14 3.047(14) 167.4 4_566
N3 H3X N2 0.92 2.24 2.742(11) 113.8 .
N6 H6C N7 0.92 2.41 2.874(12) 111.5 .
N6 H6D O4 0.92 2.49 3.362(16) 159.0 4_566
N8 H8F O1 0.89(2) 2.58(9) 3.237(11) 132(9) .

_diffrn_measured_fraction_theta_max 0.970
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.970
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.068

#===END

_database_code_depnum_ccdc_archive 'CCDC 953540'