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


#######################################################################
#
#                 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 
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data_matt2-pytpHCl
_database_code_depnum_ccdc_archive 'CCDC 887723'
#TrackingRef '12038_web_deposit_cif_file_0_MatthewPolson_1340246597.pytpHCl.cif'

_audit_creation_date             2012-06-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H12 N6, H2 O, 2(Cl)'
_chemical_formula_sum            'C18 H14 Cl2 N6 O'
_chemical_formula_weight         401.25
_chemical_compound_source        'Synthesized by the authors. See text'
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
# END OF CIF
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   8.3203(2)
_cell_length_b                   9.8047(3)
_cell_length_c                   11.3191(4)
_cell_angle_alpha                112.3820(10)
_cell_angle_beta                 93.764(2)
_cell_angle_gamma                93.041(2)
_cell_volume                     848.93(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    118(2)
_cell_measurement_theta_max      34.29
_cell_measurement_theta_min      2.35
_exptl_absorpt_coefficient_mu    0.406
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.797845
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'SADABS (Bruker, 2007) '
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_special_details           
;
Spectroscopic data:
^1^H NMR (CDCl~3~): \d zz(zzH, s, zz).
Mass Spec: (ESI-TOF) zz {M+} calc zz.
;
_diffrn_reflns_av_R_equivalents  0.0863
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22950
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.46
_diffrn_ambient_temperature      118(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         0
_reflns_number_gt                4150
_reflns_number_total             4919
_reflns_threshold_expression     I>2\s(I)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4919
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0366
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0659P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1054
_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.
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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
N11 N 1.16013(11) 0.47333(11) 0.86754(9) 0.0160(2) Uani 1 1 d D . .
H11 H 1.1776(18) 0.5561(12) 0.9303(11) 0.024 Uiso 1 1 d D . .
C12 C 1.01345(13) 0.44191(13) 0.80041(11) 0.0143(2) Uani 1 1 d . . .
C13 C 0.97893(13) 0.30402(13) 0.69989(11) 0.0147(2) Uani 1 1 d . . .
C14 C 1.09697(13) 0.20219(14) 0.67254(11) 0.0176(2) Uani 1 1 d . . .
H14 H 1.0750 0.1076 0.6049 0.021 Uiso 1 1 calc R . .
C15 C 1.24579(14) 0.23974(14) 0.74446(12) 0.0200(2) Uani 1 1 d . . .
H15 H 1.3265 0.1714 0.7271 0.024 Uiso 1 1 calc R . .
C16 C 1.27482(13) 0.37906(14) 0.84245(12) 0.0189(2) Uani 1 1 d . . .
H16 H 1.3768 0.4072 0.8917 0.023 Uiso 1 1 calc R . .
N21 N 0.94486(12) 0.68211(11) 0.93474(10) 0.0178(2) Uani 1 1 d . . .
C22 C 0.89704(13) 0.55308(13) 0.83572(11) 0.0147(2) Uani 1 1 d . . .
C23 C 0.74328(13) 0.52159(13) 0.76802(11) 0.0148(2) Uani 1 1 d . . .
C24 C 0.63167(13) 0.62903(14) 0.80654(12) 0.0178(2) Uani 1 1 d . . .
H24 H 0.5258 0.6111 0.7640 0.021 Uiso 1 1 calc R . .
C25 C 0.67929(14) 0.76117(14) 0.90755(12) 0.0193(2) Uani 1 1 d . . .
H25 H 0.6068 0.8363 0.9360 0.023 Uiso 1 1 calc R . .
C26 C 0.83682(14) 0.78254(13) 0.96748(12) 0.0193(2) Uani 1 1 d . . .
H26 H 0.8686 0.8748 1.0360 0.023 Uiso 1 1 calc R . .
N31 N 0.78791(12) 0.14236(11) 0.52923(10) 0.0174(2) Uani 1 1 d . . .
N32 N 0.64448(12) 0.11361(12) 0.46154(10) 0.0188(2) Uani 1 1 d . . .
C33 C 0.53999(13) 0.21905(13) 0.49662(11) 0.0156(2) Uani 1 1 d . . .
N34 N 0.56084(11) 0.34966(11) 0.59469(9) 0.0159(2) Uani 1 1 d . . .
C35 C 0.70574(13) 0.37982(13) 0.66167(11) 0.0143(2) Uani 1 1 d . . .
C36 C 0.82061(13) 0.27385(13) 0.62739(10) 0.0147(2) Uani 1 1 d . . .
N41 N 0.27546(11) 0.28765(11) 0.45231(9) 0.0164(2) Uani 1 1 d D . .
H41 H 0.3043(18) 0.3685(12) 0.5143(12) 0.025 Uiso 1 1 d D . .
C42 C 0.38261(13) 0.18380(13) 0.41778(11) 0.0157(2) Uani 1 1 d . . .
C43 C 0.33951(14) 0.05283(14) 0.31374(12) 0.0195(2) Uani 1 1 d . . .
H43 H 0.4139 -0.0207 0.2862 0.023 Uiso 1 1 calc R . .
C44 C 0.18537(14) 0.02995(14) 0.24965(12) 0.0211(2) Uani 1 1 d . . .
H44 H 0.1543 -0.0600 0.1783 0.025 Uiso 1 1 calc R . .
C45 C 0.07731(14) 0.13770(15) 0.28947(12) 0.0212(3) Uani 1 1 d . . .
H45 H -0.0285 0.1221 0.2471 0.025 Uiso 1 1 calc R . .
C46 C 0.12681(14) 0.26842(14) 0.39213(12) 0.0194(2) Uani 1 1 d . . .
H46 H 0.0555 0.3447 0.4200 0.023 Uiso 1 1 calc R . .
Cl1 Cl 0.76715(3) 0.40319(3) 0.36494(3) 0.01988(9) Uani 1 1 d . . .
Cl2 Cl 0.64543(3) 0.28606(3) 0.91173(3) 0.02043(9) Uani 1 1 d . . .
O100 O 0.70812(14) 0.10971(12) 0.10651(11) 0.0346(3) Uani 1 1 d D . .
H10A H 0.700(2) 0.144(2) 0.0505(15) 0.052 Uiso 1 1 d D . .
H10B H 0.709(2) 0.1810(16) 0.1746(12) 0.052 Uiso 1 1 d 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
N11 0.0133(4) 0.0155(5) 0.0176(5) 0.0050(4) -0.0007(3) 0.0022(4)
C12 0.0129(5) 0.0150(5) 0.0160(5) 0.0070(4) 0.0009(4) 0.0026(4)
C13 0.0125(5) 0.0147(5) 0.0168(5) 0.0061(4) 0.0010(4) 0.0026(4)
C14 0.0156(5) 0.0175(5) 0.0190(5) 0.0059(4) 0.0008(4) 0.0039(4)
C15 0.0152(5) 0.0211(6) 0.0232(6) 0.0075(5) 0.0010(4) 0.0076(4)
C16 0.0129(5) 0.0217(6) 0.0220(6) 0.0085(5) -0.0007(4) 0.0040(4)
N21 0.0188(4) 0.0140(5) 0.0180(5) 0.0035(4) -0.0005(4) 0.0015(4)
C22 0.0146(5) 0.0139(5) 0.0156(5) 0.0054(4) 0.0017(4) 0.0026(4)
C23 0.0144(5) 0.0136(5) 0.0165(5) 0.0057(4) 0.0017(4) 0.0026(4)
C24 0.0142(5) 0.0174(6) 0.0216(6) 0.0069(5) 0.0017(4) 0.0035(4)
C25 0.0179(5) 0.0171(6) 0.0219(6) 0.0058(5) 0.0029(4) 0.0052(4)
C26 0.0207(5) 0.0152(5) 0.0194(5) 0.0039(4) 0.0006(4) 0.0026(4)
N31 0.0151(4) 0.0150(5) 0.0197(5) 0.0042(4) -0.0017(4) 0.0040(4)
N32 0.0154(4) 0.0173(5) 0.0209(5) 0.0048(4) -0.0023(4) 0.0029(4)
C33 0.0149(5) 0.0143(5) 0.0168(5) 0.0053(4) -0.0010(4) 0.0025(4)
N34 0.0137(4) 0.0156(5) 0.0171(5) 0.0049(4) 0.0002(3) 0.0023(4)
C35 0.0132(5) 0.0143(5) 0.0155(5) 0.0057(4) 0.0013(4) 0.0018(4)
C36 0.0134(5) 0.0141(5) 0.0160(5) 0.0051(4) 0.0008(4) 0.0020(4)
N41 0.0146(4) 0.0156(5) 0.0167(5) 0.0035(4) -0.0003(4) 0.0036(4)
C42 0.0132(5) 0.0166(5) 0.0174(5) 0.0065(4) 0.0003(4) 0.0027(4)
C43 0.0170(5) 0.0168(6) 0.0224(6) 0.0050(5) -0.0014(4) 0.0046(4)
C44 0.0187(5) 0.0184(6) 0.0223(6) 0.0046(5) -0.0039(4) 0.0008(4)
C45 0.0155(5) 0.0231(6) 0.0235(6) 0.0078(5) -0.0027(4) 0.0018(4)
C46 0.0140(5) 0.0222(6) 0.0222(6) 0.0084(5) 0.0008(4) 0.0056(4)
Cl1 0.01921(14) 0.01824(15) 0.02080(15) 0.00546(11) 0.00158(11) 0.00601(11)
Cl2 0.01788(14) 0.01784(15) 0.02101(15) 0.00302(11) -0.00305(10) 0.00285(10)
O100 0.0427(6) 0.0214(5) 0.0331(6) 0.0036(4) -0.0037(5) 0.0077(4)

_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
N11 H11 0.848(9) . ?
N11 C12 1.3497(13) . ?
N11 C16 1.3322(15) . ?
C12 C13 1.3962(15) . ?
C12 C22 1.4550(16) . ?
C13 C14 1.4020(15) . ?
C13 C36 1.4588(14) . ?
C14 H14 0.9500 . ?
C14 C15 1.3866(15) . ?
C15 H15 0.9500 . ?
C15 C16 1.3894(17) . ?
C16 H16 0.9500 . ?
N21 C22 1.3503(14) . ?
N21 C26 1.3322(15) . ?
C22 C23 1.4030(14) . ?
C23 C24 1.4034(16) . ?
C23 C35 1.4523(16) . ?
C24 H24 0.9500 . ?
C24 C25 1.3787(17) . ?
C25 H25 0.9500 . ?
C25 C26 1.4028(15) . ?
C26 H26 0.9500 . ?
N31 N32 1.3306(12) . ?
N31 C36 1.3427(14) . ?
N32 C33 1.3455(15) . ?
C33 N34 1.3307(15) . ?
C33 C42 1.4813(14) . ?
N34 C35 1.3368(13) . ?
C35 C36 1.4109(16) . ?
N41 H41 0.844(9) . ?
N41 C42 1.3503(15) . ?
N41 C46 1.3402(14) . ?
C42 C43 1.3815(16) . ?
C43 H43 0.9500 . ?
C43 C44 1.3946(15) . ?
C44 H44 0.9500 . ?
C44 C45 1.3852(18) . ?
C45 H45 0.9500 . ?
C45 C46 1.3819(17) . ?
C46 H46 0.9500 . ?
O100 H10A 0.826(9) . ?
O100 H10B 0.819(9) . ?

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
C12 N11 H11 117.6(11) . . ?
C16 N11 H11 119.2(11) . . ?
C16 N11 C12 123.19(10) . . ?
N11 C12 C13 118.85(10) . . ?
N11 C12 C22 118.71(10) . . ?
C13 C12 C22 122.45(9) . . ?
C12 C13 C14 119.06(10) . . ?
C12 C13 C36 117.75(10) . . ?
C14 C13 C36 123.18(10) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 C13 119.88(11) . . ?
C15 C14 H14 120.1 . . ?
C14 C15 H15 120.6 . . ?
C14 C15 C16 118.81(11) . . ?
C16 C15 H15 120.6 . . ?
N11 C16 C15 120.21(10) . . ?
N11 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C26 N21 C22 116.43(9) . . ?
N21 C22 C12 116.83(10) . . ?
N21 C22 C23 123.70(10) . . ?
C23 C22 C12 119.47(10) . . ?
C22 C23 C24 118.30(10) . . ?
C22 C23 C35 119.00(10) . . ?
C24 C23 C35 122.69(10) . . ?
C23 C24 H24 120.8 . . ?
C25 C24 C23 118.45(10) . . ?
C25 C24 H24 120.8 . . ?
C24 C25 H25 120.6 . . ?
C24 C25 C26 118.74(11) . . ?
C26 C25 H25 120.6 . . ?
N21 C26 C25 124.36(11) . . ?
N21 C26 H26 117.8 . . ?
C25 C26 H26 117.8 . . ?
N32 N31 C36 118.69(10) . . ?
N31 N32 C33 117.47(10) . . ?
N32 C33 C42 115.86(10) . . ?
N34 C33 N32 127.57(10) . . ?
N34 C33 C42 116.56(10) . . ?
C33 N34 C35 115.06(10) . . ?
N34 C35 C23 119.60(10) . . ?
N34 C35 C36 119.52(10) . . ?
C36 C35 C23 120.89(9) . . ?
N31 C36 C13 117.96(10) . . ?
N31 C36 C35 121.63(10) . . ?
C35 C36 C13 120.40(10) . . ?
C42 N41 H41 118.1(11) . . ?
C46 N41 H41 118.8(11) . . ?
C46 N41 C42 123.03(10) . . ?
N41 C42 C33 116.74(10) . . ?
N41 C42 C43 118.90(10) . . ?
C43 C42 C33 124.36(11) . . ?
C42 C43 H43 120.4 . . ?
C42 C43 C44 119.17(11) . . ?
C44 C43 H43 120.4 . . ?
C43 C44 H44 119.8 . . ?
C45 C44 C43 120.34(11) . . ?
C45 C44 H44 119.8 . . ?
C44 C45 H45 120.7 . . ?
C46 C45 C44 118.54(10) . . ?
C46 C45 H45 120.7 . . ?
N41 C46 C45 119.99(11) . . ?
N41 C46 H46 120.0 . . ?
C45 C46 H46 120.0 . . ?
H10A O100 H10B 105(2) . . ?

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
N11 H11 Cl2 0.848(9) 2.251(11) 3.0001(10) 147.4(14) 2_767
N41 H41 Cl1 0.844(9) 2.269(12) 3.0047(11) 145.8(14) 2_666
O100 H10A Cl2 0.826(9) 2.498(10) 3.3121(12) 168.7(19) 1_554
O100 H10B Cl1 0.819(9) 2.407(10) 3.2138(11) 168.3(19) .

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N11 C12 C13 C14 0.53(17) . . . . ?
N11 C12 C13 C36 -178.93(10) . . . . ?
N11 C12 C22 N21 0.09(16) . . . . ?
N11 C12 C22 C23 -179.19(10) . . . . ?
C12 N11 C16 C15 -1.04(19) . . . . ?
C12 C13 C14 C15 -0.46(18) . . . . ?
C12 C13 C36 N31 178.87(10) . . . . ?
C12 C13 C36 C35 -2.02(16) . . . . ?
C12 C22 C23 C24 178.11(10) . . . . ?
C12 C22 C23 C35 -1.73(17) . . . . ?
C13 C12 C22 N21 179.98(11) . . . . ?
C13 C12 C22 C23 0.70(17) . . . . ?
C13 C14 C15 C16 -0.32(19) . . . . ?
C14 C13 C36 N31 -0.56(17) . . . . ?
C14 C13 C36 C35 178.55(11) . . . . ?
C14 C15 C16 N11 1.06(19) . . . . ?
C16 N11 C12 C13 0.23(17) . . . . ?
C16 N11 C12 C22 -179.88(11) . . . . ?
N21 C22 C23 C24 -1.12(18) . . . . ?
N21 C22 C23 C35 179.04(11) . . . . ?
C22 C12 C13 C14 -179.37(11) . . . . ?
C22 C12 C13 C36 1.18(16) . . . . ?
C22 N21 C26 C25 1.05(18) . . . . ?
C22 C23 C24 C25 1.06(18) . . . . ?
C22 C23 C35 N34 -178.62(10) . . . . ?
C22 C23 C35 C36 0.89(17) . . . . ?
C23 C24 C25 C26 -0.05(18) . . . . ?
C23 C35 C36 C13 1.02(17) . . . . ?
C23 C35 C36 N31 -179.91(10) . . . . ?
C24 C23 C35 N34 1.55(18) . . . . ?
C24 C23 C35 C36 -178.94(11) . . . . ?
C24 C25 C26 N21 -1.1(2) . . . . ?
C26 N21 C22 C12 -179.17(10) . . . . ?
C26 N21 C22 C23 0.08(17) . . . . ?
N31 N32 C33 N34 -2.01(19) . . . . ?
N31 N32 C33 C42 179.13(10) . . . . ?
N32 N31 C36 C13 -179.49(10) . . . . ?
N32 N31 C36 C35 1.42(17) . . . . ?
N32 C33 N34 C35 2.96(18) . . . . ?
N32 C33 C42 N41 179.33(10) . . . . ?
N32 C33 C42 C43 -0.07(18) . . . . ?
C33 N34 C35 C23 177.89(10) . . . . ?
C33 N34 C35 C36 -1.62(16) . . . . ?
C33 C42 C43 C44 177.65(11) . . . . ?
N34 C33 C42 N41 0.34(16) . . . . ?
N34 C33 C42 C43 -179.05(11) . . . . ?
N34 C35 C36 C13 -179.47(10) . . . . ?
N34 C35 C36 N31 -0.40(18) . . . . ?
C35 C23 C24 C25 -179.11(11) . . . . ?
C36 C13 C14 C15 178.96(11) . . . . ?
C36 N31 N32 C33 -0.32(17) . . . . ?
N41 C42 C43 C44 -1.74(19) . . . . ?
C42 C33 N34 C35 -178.19(10) . . . . ?
C42 N41 C46 C45 -0.15(19) . . . . ?
C42 C43 C44 C45 0.4(2) . . . . ?
C43 C44 C45 C46 1.1(2) . . . . ?
C44 C45 C46 N41 -1.2(2) . . . . ?
C46 N41 C42 C33 -177.77(11) . . . . ?
C46 N41 C42 C43 1.66(18) . . . . ?

_iucr_refine_instructions_details 
;
TITL AMD2 in P-1
CELL 0.71073 8.3203 9.8047 11.3191 112.382 93.764 93.041
ZERR 2.00 0.0002 0.0003 0.0004 0.001 0.002 0.002
LATT 1
SFAC C H N O Cl
UNIT 36 28 12 2 4
EQIV $1 -x+2, -y+1, -z+2
EQIV $2 -x+1, -y+1, -z+1
EQIV $3 x, y, z-1
OMIT -2 60
OMIT 0 0 1
OMIT 0 -1 1
OMIT 1 6 5
OMIT 0 1 0
L.S. 10
ACTA
BOND $H
HTAB
HTAB N11 Cl2_$1
HTAB N41 Cl1_$2
HTAB O100 Cl2_$3
HTAB O100 Cl1
FMAP 2
PLAN 20
SIZE 0.17 0.19 0.24
CONF
DFIX 0.82 0.01 O100 H10A
DFIX 0.82 0.01 O100 H10B
DFIX 0.86 0.01 N41 H41
DFIX 0.86 0.01 N11 H11
TEMP -155
WGHT 0.065900
FVAR 0.44885
N11 3 1.160126 0.473326 0.867543 11.00000 0.01330 0.01553 =
0.01761 0.00497 -0.00073 0.00221
H11 2 1.177560 0.556055 0.930259 11.00000 -1.50000
C12 1 1.013452 0.441910 0.800408 11.00000 0.01292 0.01503 =
0.01601 0.00704 0.00093 0.00263
C13 1 0.978934 0.304018 0.699886 11.00000 0.01250 0.01474 =
0.01680 0.00605 0.00100 0.00255
C14 1 1.096968 0.202193 0.672536 11.00000 0.01555 0.01754 =
0.01898 0.00595 0.00076 0.00386
AFIX 43
H14 2 1.075024 0.107642 0.604850 11.00000 -1.20000
AFIX 0
C15 1 1.245794 0.239744 0.744462 11.00000 0.01520 0.02114 =
0.02323 0.00747 0.00100 0.00756
AFIX 43
H15 2 1.326466 0.171433 0.727053 11.00000 -1.20000
AFIX 0
C16 1 1.274822 0.379061 0.842447 11.00000 0.01292 0.02173 =
0.02197 0.00854 -0.00072 0.00402
AFIX 43
H16 2 1.376778 0.407190 0.891704 11.00000 -1.20000
AFIX 0
N21 3 0.944864 0.682114 0.934742 11.00000 0.01878 0.01403 =
0.01797 0.00351 -0.00053 0.00147
C22 1 0.897041 0.553083 0.835718 11.00000 0.01464 0.01389 =
0.01559 0.00544 0.00166 0.00263
C23 1 0.743283 0.521587 0.768023 11.00000 0.01441 0.01363 =
0.01645 0.00575 0.00166 0.00260
C24 1 0.631667 0.629028 0.806536 11.00000 0.01420 0.01742 =
0.02159 0.00690 0.00167 0.00355
AFIX 43
H24 2 0.525771 0.611127 0.763996 11.00000 -1.20000
AFIX 0
C25 1 0.679287 0.761165 0.907552 11.00000 0.01789 0.01706 =
0.02194 0.00577 0.00290 0.00524
AFIX 43
H25 2 0.606790 0.836317 0.936035 11.00000 -1.20000
AFIX 0
C26 1 0.836817 0.782543 0.967480 11.00000 0.02068 0.01522 =
0.01939 0.00387 0.00062 0.00257
AFIX 43
H26 2 0.868568 0.874780 1.035971 11.00000 -1.20000
AFIX 0
N31 3 0.787908 0.142358 0.529234 11.00000 0.01507 0.01501 =
0.01972 0.00423 -0.00170 0.00404
N32 3 0.644477 0.113609 0.461544 11.00000 0.01535 0.01725 =
0.02094 0.00477 -0.00228 0.00295
C33 1 0.539994 0.219054 0.496619 11.00000 0.01490 0.01426 =
0.01680 0.00528 -0.00102 0.00254
N34 3 0.560836 0.349660 0.594695 11.00000 0.01371 0.01556 =
0.01711 0.00492 0.00015 0.00235
C35 1 0.705736 0.379817 0.661665 11.00000 0.01320 0.01426 =
0.01549 0.00573 0.00132 0.00181
C36 1 0.820609 0.273846 0.627395 11.00000 0.01341 0.01408 =
0.01595 0.00515 0.00078 0.00200
N41 3 0.275457 0.287648 0.452314 11.00000 0.01457 0.01557 =
0.01665 0.00349 -0.00032 0.00361
H41 2 0.304262 0.368543 0.514281 11.00000 -1.50000
C42 1 0.382613 0.183800 0.417780 11.00000 0.01317 0.01655 =
0.01736 0.00646 0.00025 0.00266
C43 1 0.339514 0.052827 0.313742 11.00000 0.01702 0.01683 =
0.02236 0.00501 -0.00142 0.00458
AFIX 43
H43 2 0.413949 -0.020738 0.286200 11.00000 -1.20000
AFIX 0
C44 1 0.185366 0.029952 0.249651 11.00000 0.01868 0.01843 =
0.02233 0.00461 -0.00387 0.00084
AFIX 43
H44 2 0.154307 -0.059986 0.178319 11.00000 -1.20000
AFIX 0
C45 1 0.077311 0.137700 0.289470 11.00000 0.01550 0.02308 =
0.02350 0.00782 -0.00273 0.00184
AFIX 43
H45 2 -0.028496 0.122070 0.247133 11.00000 -1.20000
AFIX 0
C46 1 0.126809 0.268423 0.392132 11.00000 0.01397 0.02220 =
0.02221 0.00837 0.00084 0.00563
AFIX 43
H46 2 0.055478 0.344651 0.420044 11.00000 -1.20000
AFIX 0
CL1 5 0.767154 0.403185 0.364936 11.00000 0.01921 0.01824 =
0.02080 0.00546 0.00158 0.00601
CL2 5 0.645430 0.286058 0.911733 11.00000 0.01788 0.01784 =
0.02101 0.00302 -0.00305 0.00285
O100 4 0.708120 0.109710 0.106512 11.00000 0.04270 0.02139 =
0.03310 0.00359 -0.00373 0.00770
H10A 2 0.699897 0.144222 0.050466 11.00000 -1.50000
H10B 2 0.709331 0.181036 0.174630 11.00000 -1.50000
HKLF 4

REM AMD2 in P-1
REM R1 = 0.0366 for 4150 Fo > 4sig(Fo) and 0.0427 for all 4919 data
REM 256 parameters refined using 4 restraints

END
;




data_mattc-RuBipy2pztpPF6
_database_code_depnum_ccdc_archive 'CCDC 887724'
#TrackingRef '12039_web_deposit_cif_file_0_MatthewPolson_1340246752.RuBipy2pztpPF6.cif'

_audit_creation_date             2012-06-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C37 H25 N11 Ru), 4(F6 P), 3(C2 H3 N)'
_chemical_formula_sum            'C40 H29.5 F12 N12.5 P2 Ru'
_chemical_formula_weight         1076.27
_chemical_compound_source        'Synthesized by the authors. See text'
_chemical_melting_point          ?
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
# END OF CIF
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   11.8919(7)
_cell_length_b                   12.3372(7)
_cell_length_c                   15.9036(10)
_cell_angle_alpha                81.000(4)
_cell_angle_beta                 77.789(4)
_cell_angle_gamma                66.668(4)
_cell_volume                     2087.1(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    118(2)
_cell_measurement_theta_max      34.29
_cell_measurement_theta_min      2.35
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.853436
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2007) '
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1078
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_special_details           
;
Spectroscopic data:
^1^H NMR (CDCl~3~): \d zz(zzH, s, zz).
Mass Spec: (ESI-TOF) zz {M+} calc zz.
;
_diffrn_reflns_av_R_equivalents  0.1090
_diffrn_reflns_av_unetI/netI     0.1096
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34975
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.19
_diffrn_ambient_temperature      118(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         0
_reflns_number_gt                4408
_reflns_number_total             7380
_reflns_threshold_expression     I>2\s(I)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         7380
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1193
_refine_ls_R_factor_gt           0.0559
_refine_ls_restrained_S_all      1.003
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+0.3600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1393
_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.
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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
Ru Ru 0.74666(5) 0.84692(4) 0.75076(3) 0.03354(16) Uani 1 1 d . A 4
N11 N 0.8816(4) 0.9039(4) 0.7644(3) 0.0376(12) Uani 1 1 d . A 4
C12 C 0.9296(5) 0.8611(4) 0.8386(4) 0.0337(14) Uani 1 1 d . A 4
C13 C 1.0141(5) 0.8987(5) 0.8629(4) 0.0400(15) Uani 1 1 d . A 4
C14 C 1.0506(6) 0.9818(5) 0.8077(4) 0.0446(16) Uani 1 1 d . A 4
H14 H 1.1054 1.0098 0.8223 0.054 Uiso 1 1 calc R A 4
C15 C 1.0061(6) 1.0221(5) 0.7324(4) 0.0485(17) Uani 1 1 d . A 4
H15 H 1.0326 1.0757 0.6941 0.058 Uiso 1 1 calc R A 4
C16 C 0.9212(6) 0.9831(5) 0.7127(4) 0.0449(16) Uani 1 1 d . A 4
H16 H 0.8901 1.0131 0.6614 0.054 Uiso 1 1 calc R A 4
N21 N 0.8064(4) 0.7444(4) 0.8586(3) 0.0326(11) Uani 1 1 d . A 4
C22 C 0.8882(5) 0.7732(5) 0.8915(4) 0.0328(13) Uani 1 1 d . A 4
C23 C 0.9335(5) 0.7185(5) 0.9672(4) 0.0360(14) Uani 1 1 d . A 4
C24 C 0.8910(5) 0.6337(5) 1.0142(4) 0.0370(14) Uani 1 1 d . A 4
H24 H 0.9159 0.5989 1.0668 0.044 Uiso 1 1 calc R A 4
C25 C 0.8107(5) 0.6021(5) 0.9810(4) 0.0394(15) Uani 1 1 d . A 4
H25 H 0.7845 0.5425 1.0099 0.047 Uiso 1 1 calc R A 4
C26 C 0.7695(5) 0.6592(5) 0.9047(4) 0.0363(14) Uani 1 1 d . A 4
H26 H 0.7139 0.6380 0.8844 0.044 Uiso 1 1 calc R A 4
N31 N 1.1353(5) 0.8848(4) 0.9715(3) 0.0462(13) Uani 1 1 d . A 4
N32 N 1.1755(5) 0.8393(5) 1.0437(3) 0.0469(13) Uani 1 1 d . A 4
C33 C 1.1398(5) 0.7506(5) 1.0892(4) 0.0429(15) Uani 1 1 d . A 4
N34 N 1.0664(4) 0.7065(4) 1.0674(3) 0.0421(13) Uani 1 1 d . A 4
C35 C 1.0206(5) 0.7577(5) 0.9950(4) 0.0380(14) Uani 1 1 d . A 4
C36 C 1.0566(5) 0.8463(5) 0.9437(4) 0.0410(15) Uani 1 1 d . A 4
N41 N 1.2552(5) 0.7494(5) 1.1991(4) 0.0600(16) Uani 1 1 d . A 4
C42 C 1.1872(6) 0.7025(5) 1.1708(4) 0.0488(17) Uani 1 1 d . A 4
C43 C 1.1550(6) 0.6127(6) 1.2210(5) 0.0581(19) Uani 1 1 d . A 4
H43 H 1.1052 0.5835 1.2012 0.070 Uiso 1 1 calc R A 4
N44 N 1.1933(6) 0.5670(5) 1.2969(4) 0.0715(18) Uani 1 1 d . A 4
C45 C 1.2634(7) 0.6123(7) 1.3217(5) 0.071(2) Uani 1 1 d . A 4
H45 H 1.2943 0.5812 1.3730 0.085 Uiso 1 1 calc R A 4
C46 C 1.2924(7) 0.7031(6) 1.2746(5) 0.063(2) Uani 1 1 d . A 4
H46 H 1.3397 0.7337 1.2961 0.075 Uiso 1 1 calc R A 4
N51 N 0.6100(4) 0.9636(4) 0.8311(3) 0.0379(12) Uani 1 1 d . A 4
C52 C 0.5004(5) 0.9464(5) 0.8520(4) 0.0381(14) Uani 1 1 d . A 4
C53 C 0.4018(6) 1.0194(6) 0.9061(4) 0.0502(17) Uani 1 1 d . A 4
H53 H 0.3284 1.0057 0.9209 0.060 Uiso 1 1 calc R A 4
C54 C 0.4109(6) 1.1112(6) 0.9380(4) 0.0538(19) Uani 1 1 d . A 4
H54 H 0.3440 1.1605 0.9741 0.065 Uiso 1 1 calc R A 4
C55 C 0.5200(7) 1.1299(5) 0.9163(4) 0.0515(18) Uani 1 1 d . A 4
H55 H 0.5282 1.1925 0.9369 0.062 Uiso 1 1 calc R A 4
C56 C 0.6166(6) 1.0545(5) 0.8637(4) 0.0402(15) Uani 1 1 d . A 4
H56 H 0.6908 1.0670 0.8497 0.048 Uiso 1 1 calc R A 4
N61 N 0.6015(4) 0.7948(4) 0.7556(3) 0.0344(11) Uani 1 1 d . A 4
C62 C 0.4960(5) 0.8533(5) 0.8084(4) 0.0370(14) Uani 1 1 d . A 4
C63 C 0.3917(6) 0.8268(6) 0.8168(4) 0.0522(17) Uani 1 1 d . A 4
H63 H 0.3206 0.8657 0.8548 0.063 Uiso 1 1 calc R A 4
C64 C 0.3933(7) 0.7433(6) 0.7690(5) 0.063(2) Uani 1 1 d . A 4
H64 H 0.3229 0.7256 0.7739 0.076 Uiso 1 1 calc R A 4
C65 C 0.4991(7) 0.6856(6) 0.7137(5) 0.0597(19) Uani 1 1 d . A 4
H65 H 0.5014 0.6288 0.6804 0.072 Uiso 1 1 calc R A 4
C66 C 0.6010(6) 0.7133(5) 0.7085(4) 0.0455(16) Uani 1 1 d . A 4
H66 H 0.6728 0.6744 0.6710 0.055 Uiso 1 1 calc R A 4
N71 N 0.6985(4) 0.9449(4) 0.6381(3) 0.0385(12) Uani 1 1 d . A 4
C72 C 0.7581(6) 0.8914(5) 0.5647(4) 0.0404(15) Uani 1 1 d . A 4
C73 C 0.7266(6) 0.9414(6) 0.4849(4) 0.0548(18) Uani 1 1 d . A 4
H73 H 0.7693 0.9027 0.4353 0.066 Uiso 1 1 calc R A 4
C74 C 0.6305(7) 1.0498(6) 0.4803(4) 0.065(2) Uani 1 1 d . A 4
H74 H 0.6062 1.0842 0.4274 0.078 Uiso 1 1 calc R A 4
C75 C 0.5712(6) 1.1063(6) 0.5533(5) 0.0561(18) Uani 1 1 d . A 4
H75 H 0.5082 1.1809 0.5509 0.067 Uiso 1 1 calc R A 4
C76 C 0.6068(6) 1.0504(5) 0.6317(4) 0.0456(16) Uani 1 1 d . A 4
H76 H 0.5647 1.0882 0.6818 0.055 Uiso 1 1 calc R A 4
N81 N 0.8712(4) 0.7359(4) 0.6603(3) 0.0376(12) Uani 1 1 d . A 4
C82 C 0.8591(6) 0.7760(5) 0.5760(4) 0.0405(15) Uani 1 1 d . A 4
C83 C 0.9402(7) 0.7111(6) 0.5088(4) 0.062(2) Uani 1 1 d . A 4
H83 H 0.9308 0.7389 0.4519 0.074 Uiso 1 1 calc R A 4
C84 C 1.0345(7) 0.6055(6) 0.5269(5) 0.069(2) Uani 1 1 d . A 4
H84 H 1.0888 0.5615 0.4823 0.083 Uiso 1 1 calc R A 4
C85 C 1.0476(7) 0.5657(6) 0.6117(4) 0.064(2) Uani 1 1 d . A 4
H85 H 1.1111 0.4949 0.6249 0.077 Uiso 1 1 calc R A 4
C86 C 0.9652(6) 0.6322(5) 0.6768(4) 0.0454(16) Uani 1 1 d . A 4
H86 H 0.9744 0.6051 0.7338 0.054 Uiso 1 1 calc R A 4
N100 N 0.0955(18) 0.8886(18) 0.4827(11) 0.158(10) Uani 0.50 1 d P . .
C100 C 0.1432(15) 0.8360(15) 0.5341(10) 0.067(4) Uani 0.50 1 d P . .
C101 C 0.1980(12) 0.7760(11) 0.6048(9) 0.060(4) Uani 0.50 1 d P . .
H10A H 0.2672 0.7055 0.5875 0.089 Uiso 0.50 1 calc PR . .
H10B H 0.1385 0.7549 0.6478 0.089 Uiso 0.50 1 calc PR . .
H10C H 0.2265 0.8258 0.6283 0.089 Uiso 0.50 1 calc PR . .
N200 N 0.8400(6) 0.3961(5) 0.1827(4) 0.0656(17) Uani 1 1 d . B 2
C200 C 0.7463(7) 0.4676(6) 0.1940(4) 0.0464(16) Uani 1 1 d . B 2
C201 C 0.6215(6) 0.5607(6) 0.2097(5) 0.063(2) Uani 1 1 d . B 2
H20A H 0.6206 0.6317 0.1746 0.094 Uiso 1 1 calc R B 2
H20B H 0.6003 0.5763 0.2695 0.094 Uiso 1 1 calc R B 2
H20C H 0.5622 0.5348 0.1953 0.094 Uiso 1 1 calc R B 2
P10 P 0.22457(17) 0.22065(15) 0.72977(11) 0.0470(4) Uani 1 1 d . C 2
F10 F 0.1815(3) 0.1744(3) 0.8260(2) 0.0584(10) Uani 1 1 d . C 2
F11 F 0.3520(3) 0.2086(3) 0.7548(3) 0.0662(11) Uani 1 1 d . C 2
F12 F 0.1609(3) 0.3530(3) 0.7572(2) 0.0593(10) Uani 1 1 d . C 2
F13 F 0.2664(4) 0.2670(3) 0.6333(2) 0.0636(11) Uani 1 1 d . C 2
F14 F 0.0986(3) 0.2309(3) 0.7031(2) 0.0603(10) Uani 1 1 d . C 2
F15 F 0.2882(4) 0.0871(3) 0.7036(2) 0.0629(11) Uani 1 1 d . C 2
P20 P 0.5000 0.5000 1.0000 0.0474(6) Uani 1 2 d S . 2
F21 F 0.6309(3) 0.4276(3) 1.0308(3) 0.0686(11) Uani 1 1 d . D 2
F22 F 0.5094(4) 0.6193(3) 1.0147(3) 0.0777(13) Uani 1 1 d . E 2
F23 F 0.5673(4) 0.5083(4) 0.9025(2) 0.0748(12) Uani 1 1 d . F 2
P30 P 0.5000 0.5000 0.5000 0.0810(10) Uani 1 2 d S . 2
F30 F 0.5685(11) 0.3766(6) 0.5488(7) 0.141(4) Uani 0.80 1 d P G 1
F31 F 0.4195(9) 0.5412(9) 0.5881(5) 0.152(3) Uani 0.80 1 d P H 1
F32 F 0.5957(9) 0.5555(7) 0.5147(5) 0.113(3) Uani 0.80 1 d P I 1
F35 F 0.530(6) 0.425(4) 0.578(4) 0.141(4) Uani 0.20 1 d P J 2
F36 F 0.482(5) 0.595(4) 0.559(2) 0.152(3) Uani 0.20 1 d P K 2
F37 F 0.644(3) 0.481(3) 0.474(2) 0.113(3) Uani 0.20 1 d P L 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru 0.0342(3) 0.0356(3) 0.0303(3) -0.00226(19) 0.0017(2) -0.0161(2)
N11 0.041(3) 0.033(3) 0.037(3) -0.002(2) 0.002(2) -0.017(2)
C12 0.030(3) 0.032(3) 0.035(3) 0.000(3) 0.008(3) -0.014(3)
C13 0.037(4) 0.040(3) 0.041(4) -0.006(3) 0.005(3) -0.017(3)
C14 0.039(4) 0.045(4) 0.053(4) -0.003(3) -0.001(3) -0.022(3)
C15 0.045(4) 0.044(4) 0.058(5) 0.001(3) 0.006(4) -0.028(3)
C16 0.044(4) 0.043(4) 0.045(4) 0.003(3) 0.006(3) -0.024(3)
N21 0.028(3) 0.031(3) 0.036(3) -0.008(2) 0.006(2) -0.013(2)
C22 0.030(3) 0.032(3) 0.033(3) -0.011(3) 0.008(3) -0.012(3)
C23 0.033(3) 0.043(3) 0.029(3) -0.005(3) 0.004(3) -0.016(3)
C24 0.037(3) 0.038(3) 0.035(4) 0.000(3) 0.000(3) -0.017(3)
C25 0.041(4) 0.035(3) 0.044(4) 0.000(3) 0.002(3) -0.022(3)
C26 0.038(4) 0.040(3) 0.033(3) -0.004(3) 0.002(3) -0.020(3)
N31 0.039(3) 0.049(3) 0.049(4) -0.010(3) 0.004(3) -0.019(3)
N32 0.044(3) 0.057(3) 0.046(3) -0.011(3) -0.003(3) -0.025(3)
C33 0.033(4) 0.051(4) 0.041(4) -0.011(3) 0.006(3) -0.015(3)
N34 0.032(3) 0.049(3) 0.045(3) -0.014(3) 0.006(3) -0.017(3)
C35 0.032(3) 0.046(4) 0.035(4) -0.006(3) 0.002(3) -0.017(3)
C36 0.032(3) 0.044(4) 0.041(4) -0.011(3) 0.011(3) -0.014(3)
N41 0.057(4) 0.060(4) 0.071(4) -0.009(3) -0.018(3) -0.025(3)
C42 0.048(4) 0.051(4) 0.051(4) -0.009(3) -0.003(3) -0.022(3)
C43 0.049(4) 0.068(5) 0.057(5) 0.009(4) -0.017(4) -0.023(4)
N44 0.066(4) 0.081(4) 0.070(5) 0.009(4) -0.022(4) -0.031(4)
C45 0.062(5) 0.084(6) 0.081(6) 0.003(5) -0.025(5) -0.038(5)
C46 0.063(5) 0.074(5) 0.060(5) 0.001(4) -0.031(4) -0.028(4)
N51 0.039(3) 0.036(3) 0.036(3) 0.000(2) -0.004(2) -0.013(2)
C52 0.035(4) 0.043(3) 0.030(3) 0.004(3) -0.002(3) -0.012(3)
C53 0.039(4) 0.059(4) 0.039(4) -0.002(3) -0.004(3) -0.006(3)
C54 0.052(5) 0.051(4) 0.037(4) -0.010(3) -0.004(3) 0.004(4)
C55 0.064(5) 0.036(4) 0.046(4) -0.009(3) -0.009(4) -0.007(3)
C56 0.052(4) 0.033(3) 0.033(3) 0.000(3) -0.005(3) -0.015(3)
N61 0.035(3) 0.035(3) 0.036(3) -0.001(2) -0.007(2) -0.016(2)
C62 0.033(3) 0.039(3) 0.035(3) 0.010(3) -0.005(3) -0.014(3)
C63 0.043(4) 0.052(4) 0.053(4) 0.005(3) -0.001(3) -0.016(3)
C64 0.047(5) 0.055(5) 0.090(6) 0.005(4) -0.014(4) -0.025(4)
C65 0.066(5) 0.052(4) 0.076(5) -0.004(4) -0.017(4) -0.036(4)
C66 0.047(4) 0.049(4) 0.050(4) 0.001(3) -0.006(3) -0.031(3)
N71 0.033(3) 0.042(3) 0.041(3) -0.001(2) 0.001(2) -0.018(2)
C72 0.045(4) 0.040(3) 0.038(4) 0.001(3) -0.006(3) -0.020(3)
C73 0.053(4) 0.063(5) 0.045(4) -0.001(3) -0.006(4) -0.020(4)
C74 0.071(5) 0.072(5) 0.040(4) 0.011(4) -0.017(4) -0.017(4)
C75 0.047(4) 0.056(4) 0.057(5) 0.008(4) -0.011(4) -0.014(3)
C76 0.041(4) 0.054(4) 0.037(4) 0.002(3) -0.001(3) -0.017(3)
N81 0.042(3) 0.041(3) 0.033(3) -0.002(2) -0.001(2) -0.022(2)
C82 0.047(4) 0.043(4) 0.032(4) 0.001(3) 0.000(3) -0.021(3)
C83 0.083(6) 0.063(5) 0.028(4) 0.000(3) 0.004(4) -0.022(4)
C84 0.076(6) 0.060(5) 0.045(5) -0.012(4) 0.009(4) -0.005(4)
C85 0.070(5) 0.049(4) 0.050(5) -0.004(3) 0.007(4) -0.006(4)
C86 0.048(4) 0.037(4) 0.038(4) 0.002(3) 0.000(3) -0.007(3)
N100 0.186(19) 0.27(2) 0.114(14) 0.135(16) -0.103(14) -0.202(18)
C100 0.077(11) 0.103(13) 0.051(10) 0.005(9) -0.004(9) -0.073(10)
C101 0.041(8) 0.055(9) 0.071(11) -0.016(8) 0.013(8) -0.013(7)
N200 0.047(4) 0.059(4) 0.084(5) -0.008(3) -0.005(4) -0.016(3)
C200 0.047(4) 0.052(4) 0.046(4) -0.001(3) -0.005(4) -0.027(4)
C201 0.062(5) 0.058(4) 0.071(5) -0.008(4) -0.009(4) -0.025(4)
P10 0.0512(11) 0.0471(10) 0.0428(11) -0.0005(8) -0.0070(9) -0.0201(9)
F10 0.061(2) 0.068(2) 0.041(2) 0.0060(18) -0.0042(19) -0.025(2)
F11 0.051(2) 0.072(3) 0.077(3) 0.005(2) -0.015(2) -0.026(2)
F12 0.063(2) 0.048(2) 0.065(3) -0.0099(18) -0.011(2) -0.0166(19)
F13 0.072(3) 0.063(2) 0.049(2) 0.0096(18) -0.003(2) -0.027(2)
F14 0.060(2) 0.071(2) 0.060(3) 0.0003(19) -0.015(2) -0.035(2)
F15 0.082(3) 0.043(2) 0.053(2) -0.0029(17) -0.004(2) -0.017(2)
P20 0.0475(15) 0.0486(14) 0.0515(16) -0.0160(12) 0.0029(13) -0.0248(12)
F21 0.051(2) 0.071(3) 0.082(3) -0.009(2) -0.012(2) -0.019(2)
F22 0.084(3) 0.056(2) 0.107(4) -0.026(2) -0.012(3) -0.036(2)
F23 0.073(3) 0.095(3) 0.051(3) -0.012(2) 0.011(2) -0.035(2)
P30 0.127(3) 0.078(2) 0.0471(19) 0.0005(16) -0.034(2) -0.041(2)
F30 0.220(11) 0.069(7) 0.161(10) 0.024(5) -0.116(8) -0.050(7)
F31 0.216(10) 0.179(9) 0.080(6) -0.057(5) 0.024(6) -0.100(7)
F32 0.174(8) 0.119(6) 0.090(6) 0.017(4) -0.067(6) -0.090(6)
F35 0.220(11) 0.069(7) 0.161(10) 0.024(5) -0.116(8) -0.050(7)
F36 0.216(10) 0.179(9) 0.080(6) -0.057(5) 0.024(6) -0.100(7)
F37 0.174(8) 0.119(6) 0.090(6) 0.017(4) -0.067(6) -0.090(6)

_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
Ru N11 2.051(5) . ?
Ru N21 2.042(5) . ?
Ru N51 2.047(4) . ?
Ru N61 2.050(4) . ?
Ru N71 2.051(5) . ?
Ru N81 2.061(4) . ?
N11 C12 1.358(7) . ?
N11 C16 1.342(7) . ?
C12 C13 1.402(8) . ?
C12 C22 1.445(7) . ?
C13 C14 1.386(8) . ?
C13 C36 1.441(8) . ?
C14 H14 0.9300 . ?
C14 C15 1.355(8) . ?
C15 H15 0.9300 . ?
C15 C16 1.384(8) . ?
C16 H16 0.9300 . ?
N21 C22 1.376(7) . ?
N21 C26 1.351(7) . ?
C22 C23 1.388(8) . ?
C23 C24 1.387(7) . ?
C23 C35 1.469(8) . ?
C24 H24 0.9300 . ?
C24 C25 1.383(8) . ?
C25 H25 0.9300 . ?
C25 C26 1.385(8) . ?
C26 H26 0.9300 . ?
N31 N32 1.297(7) . ?
N31 C36 1.374(7) . ?
N32 C33 1.376(8) . ?
C33 N34 1.318(7) . ?
C33 C42 1.470(9) . ?
N34 C35 1.337(7) . ?
C35 C36 1.411(8) . ?
N41 C42 1.340(8) . ?
N41 C46 1.332(8) . ?
C42 C43 1.393(9) . ?
C43 H43 0.9300 . ?
C43 N44 1.340(8) . ?
N44 C45 1.319(9) . ?
C45 H45 0.9300 . ?
C45 C46 1.368(9) . ?
C46 H46 0.9300 . ?
N51 C52 1.367(7) . ?
N51 C56 1.342(7) . ?
C52 C53 1.380(8) . ?
C52 C62 1.455(8) . ?
C53 H53 0.9300 . ?
C53 C54 1.361(9) . ?
C54 H54 0.9300 . ?
C54 C55 1.370(9) . ?
C55 H55 0.9300 . ?
C55 C56 1.370(8) . ?
C56 H56 0.9300 . ?
N61 C62 1.351(7) . ?
N61 C66 1.348(7) . ?
C62 C63 1.378(8) . ?
C63 H63 0.9300 . ?
C63 C64 1.365(9) . ?
C64 H64 0.9300 . ?
C64 C65 1.372(9) . ?
C65 H65 0.9300 . ?
C65 C66 1.368(8) . ?
C66 H66 0.9300 . ?
N71 C72 1.350(7) . ?
N71 C76 1.333(7) . ?
C72 C73 1.381(8) . ?
C72 C82 1.470(8) . ?
C73 H73 0.9300 . ?
C73 C74 1.375(9) . ?
C74 H74 0.9300 . ?
C74 C75 1.361(9) . ?
C75 H75 0.9300 . ?
C75 C76 1.389(8) . ?
C76 H76 0.9300 . ?
N81 C82 1.372(7) . ?
N81 C86 1.357(7) . ?
C82 C83 1.390(8) . ?
C83 H83 0.9300 . ?
C83 C84 1.378(9) . ?
C84 H84 0.9300 . ?
C84 C85 1.381(9) . ?
C85 H85 0.9300 . ?
C85 C86 1.380(8) . ?
C86 H86 0.9300 . ?
N100 C100 1.072(19) . ?
C100 C101 1.38(2) . ?
C101 H10A 0.9600 . ?
C101 H10B 0.9600 . ?
C101 H10C 0.9600 . ?
N200 C200 1.113(7) . ?
C200 C201 1.472(9) . ?
C201 H20A 0.9600 . ?
C201 H20B 0.9600 . ?
C201 H20C 0.9600 . ?
P10 F10 1.599(4) . ?
P10 F11 1.592(4) . ?
P10 F12 1.592(4) . ?
P10 F13 1.598(4) . ?
P10 F14 1.595(4) . ?
P10 F15 1.598(4) . ?
P20 F21 1.595(4) . ?
P20 F21 1.595(4) 2_667 ?
P20 F22 1.576(3) . ?
P20 F22 1.576(3) 2_667 ?
P20 F23 1.595(4) . ?
P20 F23 1.595(4) 2_667 ?
P30 F35 1.44(5) . ?
P30 F35 1.44(5) 2_666 ?
P30 F36 1.54(3) 2_666 ?
P30 F36 1.54(3) . ?
P30 F37 1.60(4) 2_666 ?
P30 F37 1.60(4) . ?

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
N11 Ru N81 89.75(18) . . ?
N21 Ru N11 79.28(18) . . ?
N21 Ru N51 87.63(17) . . ?
N21 Ru N61 95.49(18) . . ?
N21 Ru N71 176.18(18) . . ?
N21 Ru N81 97.82(17) . . ?
N51 Ru N11 94.21(18) . . ?
N51 Ru N61 78.95(19) . . ?
N51 Ru N71 95.81(18) . . ?
N51 Ru N81 173.79(19) . . ?
N61 Ru N11 171.64(18) . . ?
N61 Ru N71 86.83(18) . . ?
N61 Ru N81 97.48(18) . . ?
N71 Ru N11 98.75(18) . . ?
N71 Ru N81 78.84(18) . . ?
C12 N11 Ru 114.6(4) . . ?
C16 N11 Ru 128.2(4) . . ?
C16 N11 C12 117.0(5) . . ?
N11 C12 C13 122.8(5) . . ?
N11 C12 C22 115.7(5) . . ?
C13 C12 C22 121.5(5) . . ?
C12 C13 C36 116.8(5) . . ?
C14 C13 C12 117.8(6) . . ?
C14 C13 C36 125.4(6) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 C13 119.7(6) . . ?
C15 C14 H14 120.2 . . ?
C14 C15 H15 120.1 . . ?
C14 C15 C16 119.7(6) . . ?
C16 C15 H15 120.1 . . ?
N11 C16 C15 122.9(6) . . ?
N11 C16 H16 118.5 . . ?
C15 C16 H16 118.5 . . ?
C22 N21 Ru 114.7(3) . . ?
C26 N21 Ru 128.6(4) . . ?
C26 N21 C22 116.4(5) . . ?
N21 C22 C12 114.8(5) . . ?
N21 C22 C23 123.3(5) . . ?
C23 C22 C12 121.9(5) . . ?
C22 C23 C35 117.7(5) . . ?
C24 C23 C22 118.7(5) . . ?
C24 C23 C35 123.5(5) . . ?
C23 C24 H24 120.7 . . ?
C25 C24 C23 118.5(6) . . ?
C25 C24 H24 120.7 . . ?
C24 C25 H25 120.0 . . ?
C24 C25 C26 120.0(5) . . ?
C26 C25 H25 120.0 . . ?
N21 C26 C25 122.9(5) . . ?
N21 C26 H26 118.6 . . ?
C25 C26 H26 118.6 . . ?
N32 N31 C36 119.9(5) . . ?
N31 N32 C33 118.0(5) . . ?
N32 C33 C42 115.9(6) . . ?
N34 C33 N32 126.6(6) . . ?
N34 C33 C42 117.5(6) . . ?
C33 N34 C35 115.0(5) . . ?
N34 C35 C23 119.3(5) . . ?
N34 C35 C36 121.3(6) . . ?
C36 C35 C23 119.4(6) . . ?
N31 C36 C13 118.4(5) . . ?
N31 C36 C35 119.0(6) . . ?
C35 C36 C13 122.7(6) . . ?
C46 N41 C42 116.7(6) . . ?
N41 C42 C33 120.1(6) . . ?
N41 C42 C43 120.2(6) . . ?
C43 C42 C33 119.6(6) . . ?
C42 C43 H43 118.8 . . ?
N44 C43 C42 122.4(7) . . ?
N44 C43 H43 118.8 . . ?
C45 N44 C43 116.0(7) . . ?
N44 C45 H45 118.8 . . ?
N44 C45 C46 122.3(8) . . ?
C46 C45 H45 118.8 . . ?
N41 C46 C45 122.3(7) . . ?
N41 C46 H46 118.9 . . ?
C45 C46 H46 118.9 . . ?
C52 N51 Ru 115.3(4) . . ?
C56 N51 Ru 127.0(4) . . ?
C56 N51 C52 117.6(5) . . ?
N51 C52 C53 120.4(6) . . ?
N51 C52 C62 114.7(5) . . ?
C53 C52 C62 124.8(6) . . ?
C52 C53 H53 119.6 . . ?
C54 C53 C52 120.8(7) . . ?
C54 C53 H53 119.6 . . ?
C53 C54 H54 120.5 . . ?
C53 C54 C55 119.1(6) . . ?
C55 C54 H54 120.5 . . ?
C54 C55 H55 120.7 . . ?
C56 C55 C54 118.6(6) . . ?
C56 C55 H55 120.7 . . ?
N51 C56 C55 123.5(6) . . ?
N51 C56 H56 118.2 . . ?
C55 C56 H56 118.2 . . ?
C62 N61 Ru 115.5(4) . . ?
C66 N61 Ru 126.0(4) . . ?
C66 N61 C62 118.4(5) . . ?
N61 C62 C52 115.4(5) . . ?
N61 C62 C63 121.0(6) . . ?
C63 C62 C52 123.6(6) . . ?
C62 C63 H63 120.1 . . ?
C64 C63 C62 119.7(6) . . ?
C64 C63 H63 120.1 . . ?
C63 C64 H64 120.2 . . ?
C63 C64 C65 119.7(7) . . ?
C65 C64 H64 120.2 . . ?
C64 C65 H65 120.7 . . ?
C66 C65 C64 118.5(6) . . ?
C66 C65 H65 120.7 . . ?
N61 C66 C65 122.6(6) . . ?
N61 C66 H66 118.7 . . ?
C65 C66 H66 118.7 . . ?
C72 N71 Ru 116.1(4) . . ?
C76 N71 Ru 126.0(4) . . ?
C76 N71 C72 117.6(5) . . ?
N71 C72 C73 122.5(6) . . ?
N71 C72 C82 115.0(5) . . ?
C73 C72 C82 122.4(6) . . ?
C72 C73 H73 120.7 . . ?
C74 C73 C72 118.6(6) . . ?
C74 C73 H73 120.7 . . ?
C73 C74 H74 120.1 . . ?
C75 C74 C73 119.8(6) . . ?
C75 C74 H74 120.1 . . ?
C74 C75 H75 120.7 . . ?
C74 C75 C76 118.6(6) . . ?
C76 C75 H75 120.7 . . ?
N71 C76 C75 122.8(6) . . ?
N71 C76 H76 118.6 . . ?
C75 C76 H76 118.6 . . ?
C82 N81 Ru 115.3(4) . . ?
C86 N81 Ru 126.1(4) . . ?
C86 N81 C82 118.5(5) . . ?
N81 C82 C72 114.5(5) . . ?
N81 C82 C83 120.8(5) . . ?
C83 C82 C72 124.7(6) . . ?
C82 C83 H83 120.1 . . ?
C84 C83 C82 119.7(6) . . ?
C84 C83 H83 120.1 . . ?
C83 C84 H84 120.3 . . ?
C83 C84 C85 119.5(6) . . ?
C85 C84 H84 120.3 . . ?
C84 C85 H85 120.4 . . ?
C86 C85 C84 119.2(6) . . ?
C86 C85 H85 120.4 . . ?
N81 C86 C85 122.2(6) . . ?
N81 C86 H86 118.9 . . ?
C85 C86 H86 118.9 . . ?
N100 C100 C101 175(2) . . ?
C100 C101 H10A 109.5 . . ?
C100 C101 H10B 109.5 . . ?
C100 C101 H10C 109.5 . . ?
H10A C101 H10B 109.5 . . ?
H10A C101 H10C 109.5 . . ?
H10B C101 H10C 109.5 . . ?
N200 C200 C201 179.0(8) . . ?
C200 C201 H20A 109.5 . . ?
C200 C201 H20B 109.5 . . ?
C200 C201 H20C 109.5 . . ?
H20A C201 H20B 109.5 . . ?
H20A C201 H20C 109.5 . . ?
H20B C201 H20C 109.5 . . ?
F11 P10 F10 90.4(2) . . ?
F11 P10 F12 90.6(2) . . ?
F11 P10 F13 90.2(2) . . ?
F11 P10 F14 178.8(2) . . ?
F11 P10 F15 89.3(2) . . ?
F12 P10 F10 89.5(2) . . ?
F12 P10 F13 90.5(2) . . ?
F12 P10 F14 90.5(2) . . ?
F12 P10 F15 179.2(2) . . ?
F13 P10 F10 179.4(2) . . ?
F13 P10 F15 90.2(2) . . ?
F14 P10 F10 90.3(2) . . ?
F14 P10 F13 89.2(2) . . ?
F14 P10 F15 89.7(2) . . ?
F15 P10 F10 89.8(2) . . ?
F21 P20 F21 180.00(16) 2_667 . ?
F21 P20 F23 90.6(2) 2_667 2_667 ?
F21 P20 F23 89.4(2) . 2_667 ?
F21 P20 F23 89.4(2) 2_667 . ?
F21 P20 F23 90.6(2) . . ?
F22 P20 F21 89.7(2) 2_667 2_667 ?
F22 P20 F21 89.7(2) . . ?
F22 P20 F21 90.3(2) 2_667 . ?
F22 P20 F21 90.3(2) . 2_667 ?
F22 P20 F22 179.999(1) 2_667 . ?
F22 P20 F23 90.0(2) 2_667 2_667 ?
F22 P20 F23 90.0(2) . . ?
F22 P20 F23 90.0(2) 2_667 . ?
F22 P20 F23 90.0(2) . 2_667 ?
F23 P20 F23 180.0(3) . 2_667 ?
F35 P30 F35 180(3) . 2_666 ?
F35 P30 F36 99(2) . 2_666 ?
F35 P30 F36 81(2) 2_666 2_666 ?
F35 P30 F36 81(2) . . ?
F35 P30 F36 99(2) 2_666 . ?
F35 P30 F37 88(3) 2_666 2_666 ?
F35 P30 F37 92(3) . 2_666 ?
F35 P30 F37 92(3) 2_666 . ?
F35 P30 F37 88(3) . . ?
F36 P30 F36 180(4) 2_666 . ?
F36 P30 F37 91(2) . 2_666 ?
F36 P30 F37 89(2) 2_666 2_666 ?
F36 P30 F37 91(2) 2_666 . ?
F36 P30 F37 89(2) . . ?
F37 P30 F37 179.998(2) 2_666 . ?

_iucr_refine_instructions_details 
;
TITL amdc in P-1 #2
CELL 0.71073 11.8919 12.3372 15.9036 81 77.789 66.668
ZERR 2 0.0007 0.0007 0.001 0.004 0.004 0.004
LATT 1
SFAC C H N F P Ru
UNIT 80 59 25 24 4 2
OMIT -2 50.1
OMIT 1 1 0
OMIT 0 0 1
OMIT -1 0 1
OMIT 1 0 1
OMIT 0 1 1
OMIT 1 0 0
EADP F30 F35
EADP F31 F36
EADP F32 F37
L.S. 10
ACTA
BOND $H
FMAP 2
PLAN 20
SIZE 0.02 0.11 0.35
TEMP 23
WGHT 0.059600 0.360000
FVAR 0.08927
PART 4
RU 6 0.746656 0.846917 0.750761 11.00000 0.03418 0.03557 =
0.03027 -0.00226 0.00166 -0.01612
N11 3 0.881643 0.903892 0.764389 11.00000 0.04114 0.03322 =
0.03683 -0.00239 0.00193 -0.01673
C12 1 0.929551 0.861135 0.838552 11.00000 0.02951 0.03208 =
0.03492 0.00020 0.00806 -0.01443
C13 1 1.014093 0.898669 0.862946 11.00000 0.03705 0.04008 =
0.04055 -0.00629 0.00528 -0.01678
C14 1 1.050622 0.981789 0.807721 11.00000 0.03941 0.04496 =
0.05263 -0.00329 -0.00140 -0.02244
AFIX 43
H14 2 1.105411 1.009787 0.822308 11.00000 -1.20000
AFIX 0
C15 1 1.006134 1.022055 0.732392 11.00000 0.04527 0.04424 =
0.05778 0.00104 0.00555 -0.02773
AFIX 43
H15 2 1.032559 1.075659 0.694080 11.00000 -1.20000
AFIX 0
C16 1 0.921182 0.983062 0.712702 11.00000 0.04433 0.04337 =
0.04514 0.00326 0.00559 -0.02359
AFIX 43
H16 2 0.890131 1.013082 0.661357 11.00000 -1.20000
AFIX 0
N21 3 0.806422 0.744443 0.858623 11.00000 0.02840 0.03136 =
0.03569 -0.00790 0.00642 -0.01286
C22 1 0.888231 0.773221 0.891484 11.00000 0.02971 0.03204 =
0.03296 -0.01094 0.00830 -0.01155
C23 1 0.933518 0.718507 0.967202 11.00000 0.03342 0.04265 =
0.02940 -0.00459 0.00388 -0.01551
C24 1 0.890981 0.633717 1.014164 11.00000 0.03662 0.03839 =
0.03547 -0.00036 0.00008 -0.01740
AFIX 43
H24 2 0.915862 0.598866 1.066813 11.00000 -1.20000
AFIX 0
C25 1 0.810738 0.602109 0.980990 11.00000 0.04092 0.03476 =
0.04423 -0.00014 0.00183 -0.02161
AFIX 43
H25 2 0.784489 0.542501 1.009890 11.00000 -1.20000
AFIX 0
C26 1 0.769469 0.659216 0.904737 11.00000 0.03771 0.04033 =
0.03257 -0.00439 0.00154 -0.01968
AFIX 43
H26 2 0.713880 0.637954 0.884390 11.00000 -1.20000
AFIX 0
N31 3 1.135281 0.884800 0.971465 11.00000 0.03934 0.04905 =
0.04894 -0.01009 0.00405 -0.01864
N32 3 1.175502 0.839335 1.043701 11.00000 0.04358 0.05726 =
0.04641 -0.01103 -0.00324 -0.02530
C33 1 1.139761 0.750594 1.089158 11.00000 0.03344 0.05133 =
0.04050 -0.01141 0.00581 -0.01549
N34 3 1.066426 0.706499 1.067417 11.00000 0.03244 0.04892 =
0.04471 -0.01432 0.00643 -0.01744
C35 1 1.020550 0.757673 0.995008 11.00000 0.03205 0.04587 =
0.03527 -0.00563 0.00195 -0.01661
C36 1 1.056638 0.846263 0.943660 11.00000 0.03190 0.04443 =
0.04104 -0.01099 0.01093 -0.01435
N41 3 1.255239 0.749380 1.199069 11.00000 0.05662 0.06030 =
0.07097 -0.00854 -0.01822 -0.02529
C42 1 1.187225 0.702480 1.170837 11.00000 0.04779 0.05073 =
0.05069 -0.00882 -0.00350 -0.02195
C43 1 1.155008 0.612736 1.221026 11.00000 0.04932 0.06770 =
0.05689 0.00935 -0.01677 -0.02293
AFIX 43
H43 2 1.105156 0.583510 1.201198 11.00000 -1.20000
AFIX 0
N44 3 1.193267 0.566988 1.296867 11.00000 0.06596 0.08129 =
0.07005 0.00932 -0.02172 -0.03105
C45 1 1.263419 0.612251 1.321681 11.00000 0.06226 0.08365 =
0.08073 0.00331 -0.02492 -0.03819
AFIX 43
H45 2 1.294262 0.581249 1.373004 11.00000 -1.20000
AFIX 0
C46 1 1.292398 0.703128 1.274624 11.00000 0.06338 0.07371 =
0.06043 0.00068 -0.03066 -0.02791
AFIX 43
H46 2 1.339684 0.733704 1.296110 11.00000 -1.20000
AFIX 0
N51 3 0.609981 0.963595 0.831147 11.00000 0.03933 0.03557 =
0.03620 0.00020 -0.00433 -0.01334
C52 1 0.500364 0.946372 0.852025 11.00000 0.03520 0.04269 =
0.02959 0.00372 -0.00182 -0.01175
C53 1 0.401839 1.019388 0.906117 11.00000 0.03871 0.05946 =
0.03881 -0.00231 -0.00385 -0.00613
AFIX 43
H53 2 0.328367 1.005689 0.920930 11.00000 -1.20000
AFIX 0
C54 1 0.410889 1.111201 0.938046 11.00000 0.05201 0.05088 =
0.03687 -0.00989 -0.00355 0.00361
AFIX 43
H54 2 0.343995 1.160531 0.974112 11.00000 -1.20000
AFIX 0
C55 1 0.519958 1.129949 0.916310 11.00000 0.06372 0.03584 =
0.04631 -0.00885 -0.00935 -0.00747
AFIX 43
H55 2 0.528207 1.192529 0.936853 11.00000 -1.20000
AFIX 0
C56 1 0.616590 1.054507 0.863659 11.00000 0.05155 0.03329 =
0.03332 -0.00015 -0.00532 -0.01515
AFIX 43
H56 2 0.690751 1.066995 0.849709 11.00000 -1.20000
AFIX 0
N61 3 0.601523 0.794845 0.755617 11.00000 0.03536 0.03504 =
0.03569 -0.00081 -0.00711 -0.01649
C62 1 0.495995 0.853254 0.808383 11.00000 0.03255 0.03907 =
0.03507 0.01021 -0.00508 -0.01417
C63 1 0.391731 0.826817 0.816753 11.00000 0.04317 0.05248 =
0.05280 0.00521 -0.00111 -0.01638
AFIX 43
H63 2 0.320587 0.865722 0.854797 11.00000 -1.20000
AFIX 0
C64 1 0.393267 0.743305 0.768990 11.00000 0.04702 0.05547 =
0.09023 0.00514 -0.01358 -0.02487
AFIX 43
H64 2 0.322924 0.725623 0.773928 11.00000 -1.20000
AFIX 0
C65 1 0.499052 0.685566 0.713665 11.00000 0.06625 0.05245 =
0.07570 -0.00438 -0.01740 -0.03570
AFIX 43
H65 2 0.501405 0.628819 0.680400 11.00000 -1.20000
AFIX 0
C66 1 0.600997 0.713310 0.708511 11.00000 0.04693 0.04867 =
0.05016 0.00068 -0.00553 -0.03067
AFIX 43
H66 2 0.672791 0.674352 0.671006 11.00000 -1.20000
AFIX 0
N71 3 0.698496 0.944854 0.638139 11.00000 0.03297 0.04161 =
0.04089 -0.00099 0.00083 -0.01833
C72 1 0.758085 0.891442 0.564702 11.00000 0.04527 0.03991 =
0.03839 0.00127 -0.00627 -0.02049
C73 1 0.726558 0.941450 0.484875 11.00000 0.05311 0.06285 =
0.04494 -0.00116 -0.00623 -0.02031
AFIX 43
H73 2 0.769337 0.902719 0.435278 11.00000 -1.20000
AFIX 0
C74 1 0.630542 1.049758 0.480280 11.00000 0.07135 0.07158 =
0.04022 0.01053 -0.01658 -0.01666
AFIX 43
H74 2 0.606225 1.084239 0.427417 11.00000 -1.20000
AFIX 0
C75 1 0.571225 1.106316 0.553337 11.00000 0.04691 0.05553 =
0.05707 0.00801 -0.01105 -0.01353
AFIX 43
H75 2 0.508184 1.180895 0.550872 11.00000 -1.20000
AFIX 0
C76 1 0.606753 1.050387 0.631675 11.00000 0.04059 0.05365 =
0.03721 0.00226 -0.00115 -0.01704
AFIX 43
H76 2 0.564725 1.088197 0.681755 11.00000 -1.20000
AFIX 0
N81 3 0.871164 0.735907 0.660306 11.00000 0.04186 0.04094 =
0.03294 -0.00174 -0.00102 -0.02158
C82 1 0.859130 0.776000 0.575984 11.00000 0.04692 0.04276 =
0.03163 0.00109 -0.00004 -0.02134
C83 1 0.940172 0.711143 0.508805 11.00000 0.08301 0.06269 =
0.02831 -0.00049 0.00397 -0.02242
AFIX 43
H83 2 0.930815 0.738894 0.451871 11.00000 -1.20000
AFIX 0
C84 1 1.034451 0.605550 0.526894 11.00000 0.07624 0.06043 =
0.04532 -0.01233 0.00948 -0.00490
AFIX 43
H84 2 1.088829 0.561462 0.482307 11.00000 -1.20000
AFIX 0
C85 1 1.047573 0.565692 0.611735 11.00000 0.06961 0.04919 =
0.04953 -0.00426 0.00698 -0.00569
AFIX 43
H85 2 1.111150 0.494879 0.624857 11.00000 -1.20000
AFIX 0
C86 1 0.965190 0.632232 0.676793 11.00000 0.04799 0.03698 =
0.03783 0.00158 -0.00043 -0.00708
AFIX 43
H86 2 0.974416 0.605121 0.733832 11.00000 -1.20000
PART 0
AFIX 0
N100 3 0.095470 0.888550 0.482667 10.50000 0.18646 0.26823 =
0.11425 0.13532 -0.10330 -0.20201
C100 1 0.143211 0.836043 0.534060 10.50000 0.07689 0.10309 =
0.05122 0.00521 -0.00422 -0.07261
C101 1 0.198008 0.775978 0.604771 10.50000 0.04112 0.05464 =
0.07141 -0.01641 0.01273 -0.01279
AFIX 137
H10A 2 0.267176 0.705457 0.587459 10.50000 -1.50000
H10B 2 0.138464 0.754946 0.647774 10.50000 -1.50000
H10C 2 0.226498 0.825754 0.628262 10.50000 -1.50000
PART 2
AFIX 0
N200 3 0.840035 0.396122 0.182651 11.00000 0.04721 0.05910 =
0.08413 -0.00761 -0.00468 -0.01589
C200 1 0.746300 0.467625 0.194006 11.00000 0.04686 0.05224 =
0.04581 -0.00052 -0.00499 -0.02728
C201 1 0.621472 0.560692 0.209719 11.00000 0.06202 0.05791 =
0.07141 -0.00790 -0.00895 -0.02512
AFIX 137
H20A 2 0.620566 0.631703 0.174597 11.00000 -1.50000
H20B 2 0.600284 0.576258 0.269496 11.00000 -1.50000
H20C 2 0.562164 0.534806 0.195312 11.00000 -1.50000
AFIX 0
P10 5 0.224574 0.220649 0.729771 11.00000 0.05123 0.04713 =
0.04283 -0.00046 -0.00697 -0.02012
F10 4 0.181491 0.174443 0.826041 11.00000 0.06109 0.06798 =
0.04117 0.00605 -0.00417 -0.02498
F11 4 0.351966 0.208564 0.754812 11.00000 0.05080 0.07201 =
0.07696 0.00467 -0.01495 -0.02591
F12 4 0.160919 0.353020 0.757173 11.00000 0.06256 0.04830 =
0.06539 -0.00986 -0.01146 -0.01663
F13 4 0.266375 0.266972 0.633339 11.00000 0.07212 0.06253 =
0.04905 0.00963 -0.00306 -0.02651
F14 4 0.098580 0.230875 0.703128 11.00000 0.05982 0.07122 =
0.06020 0.00026 -0.01525 -0.03493
F15 4 0.288232 0.087103 0.703566 11.00000 0.08217 0.04312 =
0.05339 -0.00288 -0.00423 -0.01704
P20 5 0.500000 0.500000 1.000000 10.50000 0.04746 0.04862 =
0.05150 -0.01603 0.00290 -0.02480
F21 4 0.630865 0.427650 1.030840 11.00000 0.05073 0.07104 =
0.08155 -0.00934 -0.01163 -0.01882
F22 4 0.509443 0.619350 1.014705 11.00000 0.08417 0.05574 =
0.10716 -0.02614 -0.01214 -0.03570
F23 4 0.567344 0.508338 0.902525 11.00000 0.07269 0.09534 =
0.05131 -0.01190 0.01057 -0.03454
P30 5 0.500000 0.500000 0.500000 10.50000 0.12690 0.07846 =
0.04712 0.00050 -0.03407 -0.04071
PART 1
F30 4 0.568488 0.376621 0.548823 10.80000 0.21952 0.06856 =
0.16086 0.02356 -0.11609 -0.04965
F31 4 0.419464 0.541211 0.588077 10.80000 0.21564 0.17938 =
0.07994 -0.05665 0.02449 -0.10032
F32 4 0.595714 0.555455 0.514723 10.80000 0.17435 0.11938 =
0.08986 0.01720 -0.06683 -0.09022
PART 2
F35 4 0.529831 0.425441 0.578083 10.20000 0.21952 0.06856 =
0.16086 0.02356 -0.11609 -0.04965
F36 4 0.481659 0.595250 0.559130 10.20000 0.21564 0.17938 =
0.07994 -0.05665 0.02449 -0.10032
F37 4 0.643718 0.480992 0.474326 10.20000 0.17435 0.11938 =
0.08986 0.01720 -0.06683 -0.09022
PART
HKLF 4

REM amdc in P-1 #2
REM R1 = 0.0559 for 4408 Fo > 4sig(Fo) and 0.1193 for all 7380 data
REM 636 parameters refined using 0 restraints

END
;