data_2005src0396r
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. B. J. Coe
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          
 'C22 H34 N8 Ru, C2 H3 N, 4(F6 P), H2 O'
_chemical_formula_sum
 'C24 H39 F24 N9 O P4 Ru'
_chemical_formula_weight          1150.59
 
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'
 '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    P2(1)
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y+1/2, -z'
 
_cell_length_a                    11.0075(11)
_cell_length_b                    18.0498(19)
_cell_length_c                    11.1488(11)
_cell_angle_alpha                 90.00
_cell_angle_beta                  103.942(7)
_cell_angle_gamma                 90.00
_cell_volume                      2149.8(4)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     5015
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Shard
_exptl_crystal_colour             'Opaque Dark Red'
_exptl_crystal_size_max           0.14
_exptl_crystal_size_mid           0.10
_exptl_crystal_size_min           0.05
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.777
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1148
_exptl_absorpt_coefficient_mu     0.654
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9141
_exptl_absorpt_correction_T_max   0.9681
_exptl_absorpt_process_details       'SADABS V2.10 (Sheldrick, G.M., 2003)'

_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             25951
_diffrn_reflns_av_R_equivalents   0.0514
_diffrn_reflns_av_sigmaI/netI     0.0761
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_k_min        -23
_diffrn_reflns_limit_k_max        22
_diffrn_reflns_limit_l_min        -14
_diffrn_reflns_limit_l_max        14
_diffrn_reflns_theta_min          2.94
_diffrn_reflns_theta_max          27.47
_reflns_number_total              9747
_reflns_number_gt                 8030
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997b)' 
_computing_molecular_graphics     'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² 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/[σ²(Fo²)+(0.0392P)²+1.0494P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0011(4)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    0.00(2)
_refine_ls_number_reflns          9747
_refine_ls_number_parameters      582
_refine_ls_number_restraints      4
_refine_ls_R_factor_all           0.0656
_refine_ls_R_factor_gt            0.0476
_refine_ls_wR_factor_ref          0.1015
_refine_ls_wR_factor_gt           0.0936
_refine_ls_goodness_of_fit_ref    1.025
_refine_ls_restrained_S_all       1.025
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.5917(4) 0.4563(2) 0.3370(4) 0.0223(9) Uani 1 1 d . . .
H1 H 0.5450 0.4195 0.2846 0.027 Uiso 1 1 calc R . .
C2 C 0.6512(4) 0.5099(2) 0.2845(4) 0.0245(10) Uani 1 1 d . . .
H2 H 0.6425 0.5107 0.1977 0.029 Uiso 1 1 calc R . .
C3 C 0.7242(4) 0.5627(2) 0.3593(4) 0.0218(9) Uani 1 1 d . . .
C4 C 0.7322(4) 0.5593(2) 0.4853(4) 0.0247(9) Uani 1 1 d . . .
H4 H 0.7828 0.5938 0.5398 0.030 Uiso 1 1 calc R . .
C5 C 0.6668(4) 0.5062(2) 0.5303(4) 0.0251(9) Uani 1 1 d . . .
H5 H 0.6709 0.5062 0.6164 0.030 Uiso 1 1 calc R . .
C6 C 0.7941(4) 0.6190(2) 0.3040(4) 0.0240(10) Uani 1 1 d . . .
C7 C 0.7320(4) 0.6624(2) 0.2048(4) 0.0238(9) Uani 1 1 d . . .
H7 H 0.6438 0.6587 0.1753 0.029 Uiso 1 1 calc R . .
C8 C 0.7991(4) 0.7108(2) 0.1493(4) 0.0279(10) Uani 1 1 d . . .
H8 H 0.7575 0.7394 0.0800 0.034 Uiso 1 1 calc R . .
C9 C 0.9841(5) 0.6782(3) 0.2924(4) 0.0339(11) Uani 1 1 d . . .
H9 H 1.0717 0.6846 0.3231 0.041 Uiso 1 1 calc R . .
C10 C 0.9205(4) 0.6289(2) 0.3498(4) 0.0277(10) Uani 1 1 d . . .
H10 H 0.9638 0.6020 0.4204 0.033 Uiso 1 1 calc R . .
C11 C 0.9948(5) 0.7670(3) 0.1298(5) 0.0365(12) Uani 1 1 d . . .
H11A H 0.9520 0.7705 0.0420 0.055 Uiso 1 1 calc R . .
H11B H 1.0792 0.7470 0.1380 0.055 Uiso 1 1 calc R . .
H11C H 1.0004 0.8164 0.1673 0.055 Uiso 1 1 calc R . .
C21 C 0.5081(4) 0.2375(2) 0.3808(4) 0.0239(9) Uani 1 1 d . . .
H21 H 0.4239 0.2330 0.3872 0.029 Uiso 1 1 calc R . .
C22 C 0.5531(4) 0.1862(3) 0.3108(4) 0.0301(10) Uani 1 1 d . . .
H22 H 0.4995 0.1484 0.2684 0.036 Uiso 1 1 calc R . .
C23 C 0.6751(4) 0.1896(3) 0.3022(4) 0.0263(10) Uani 1 1 d . . .
C24 C 0.7498(4) 0.2467(3) 0.3655(4) 0.0271(10) Uani 1 1 d . . .
H24 H 0.8350 0.2509 0.3624 0.032 Uiso 1 1 calc R . .
C25 C 0.6983(4) 0.2967(2) 0.4327(4) 0.0258(10) Uani 1 1 d . . .
H25 H 0.7502 0.3352 0.4753 0.031 Uiso 1 1 calc R . .
C26 C 0.7253(4) 0.1362(3) 0.2223(4) 0.0286(10) Uani 1 1 d . . .
C27 C 0.6457(5) 0.1013(3) 0.1236(4) 0.0366(12) Uani 1 1 d . . .
H27 H 0.5588 0.1125 0.1038 0.044 Uiso 1 1 calc R . .
C28 C 0.6913(5) 0.0511(3) 0.0549(5) 0.0417(13) Uani 1 1 d . . .
H28 H 0.6354 0.0273 -0.0123 0.050 Uiso 1 1 calc R . .
C29 C 0.8924(5) 0.0681(3) 0.1730(4) 0.0346(11) Uani 1 1 d . . .
H29 H 0.9789 0.0560 0.1905 0.042 Uiso 1 1 calc R . .
C30 C 0.8520(4) 0.1203(3) 0.2450(5) 0.0327(11) Uani 1 1 d . . .
H30 H 0.9102 0.1450 0.3093 0.039 Uiso 1 1 calc R . .
C31 C 0.8597(5) -0.0227(3) 0.0073(5) 0.0409(12) Uani 1 1 d . . .
H31A H 0.8689 -0.0011 -0.0707 0.061 Uiso 1 1 calc R . .
H31B H 0.7998 -0.0638 -0.0101 0.061 Uiso 1 1 calc R . .
H31C H 0.9410 -0.0411 0.0544 0.061 Uiso 1 1 calc R . .
N1 N 0.5961(4) 0.4532(2) 0.4595(3) 0.0209(8) Uani 1 1 d . . .
N2 N 0.9231(4) 0.7170(2) 0.1936(3) 0.0267(8) Uani 1 1 d . . .
N21 N 0.5782(4) 0.2940(2) 0.4410(3) 0.0254(9) Uani 1 1 d . . .
N22 N 0.8137(4) 0.0342(2) 0.0798(3) 0.0317(9) Uani 1 1 d . . .
N41 N 0.3464(3) 0.3839(2) 0.3785(3) 0.0320(9) Uani 1 1 d . . .
H41A H 0.3392 0.4319 0.3527 0.048 Uiso 1 1 calc R . .
H41B H 0.2756 0.3701 0.4011 0.048 Uiso 1 1 calc R . .
H41C H 0.3573 0.3543 0.3158 0.048 Uiso 1 1 calc R . .
N42 N 0.4070(4) 0.2895(2) 0.6142(4) 0.0334(11) Uani 1 1 d . . .
H42A H 0.4569 0.2489 0.6342 0.050 Uiso 1 1 calc R . .
H42B H 0.3350 0.2764 0.5589 0.050 Uiso 1 1 calc R . .
H42C H 0.3884 0.3080 0.6836 0.050 Uiso 1 1 calc R . .
N43 N 0.4213(4) 0.4573(2) 0.6261(4) 0.0319(10) Uani 1 1 d . . .
H43A H 0.4702 0.4644 0.7036 0.048 Uiso 1 1 calc R . .
H43B H 0.3436 0.4426 0.6311 0.048 Uiso 1 1 calc R . .
H43C H 0.4154 0.5005 0.5829 0.048 Uiso 1 1 calc R . .
N44 N 0.6593(4) 0.3608(2) 0.6902(3) 0.0323(9) Uani 1 1 d . . .
H44A H 0.7239 0.3897 0.6802 0.049 Uiso 1 1 calc R . .
H44B H 0.6840 0.3126 0.6975 0.049 Uiso 1 1 calc R . .
H44C H 0.6359 0.3750 0.7597 0.049 Uiso 1 1 calc R . .
Ru1 Ru 0.50385(3) 0.373061(17) 0.53293(3) 0.02323(9) Uani 1 1 d . . .
F1 F -0.0662(4) 0.4097(2) 0.4518(3) 0.0739(11) Uani 1 1 d . . .
F2 F 0.0254(5) 0.3198(2) 0.5779(5) 0.0922(15) Uani 1 1 d . . .
F3 F 0.1406(3) 0.4036(2) 0.5024(4) 0.0857(14) Uani 1 1 d . . .
F4 F 0.0426(5) 0.4944(2) 0.5732(4) 0.0915(15) Uani 1 1 d . . .
F5 F -0.0671(4) 0.4107(2) 0.6528(3) 0.0839(13) Uani 1 1 d . . .
F6 F 0.1377(4) 0.4054(3) 0.7035(4) 0.0955(15) Uani 1 1 d . . .
P1 P 0.03711(12) 0.40601(8) 0.57768(13) 0.0335(3) Uani 1 1 d . . .
F11 F 0.1080(3) 0.09699(17) 0.0226(2) 0.0466(8) Uani 1 1 d . . .
F12 F 0.1751(3) -0.01071(17) 0.1229(3) 0.0495(8) Uani 1 1 d . . .
F13 F 0.2756(3) 0.03706(16) -0.0142(2) 0.0462(8) Uani 1 1 d . . .
F14 F 0.3038(3) 0.14453(17) 0.0930(3) 0.0529(8) Uani 1 1 d . . .
F15 F 0.2011(3) 0.0957(2) 0.2276(3) 0.0597(10) Uani 1 1 d . . .
F16 F 0.3686(3) 0.03663(16) 0.1907(2) 0.0398(7) Uani 1 1 d . . .
P11 P 0.23902(12) 0.06708(8) 0.10624(11) 0.0327(3) Uani 1 1 d . . .
F21 F 0.5763(4) 0.0954(2) -0.4160(3) 0.0808(13) Uani 1 1 d . . .
F22 F 0.6515(3) 0.03358(15) -0.2383(3) 0.0465(8) Uani 1 1 d . . .
F23 F 0.7816(4) 0.0757(2) -0.3524(4) 0.0818(13) Uani 1 1 d . . .
F24 F 0.7096(3) 0.19176(17) -0.3437(3) 0.0517(8) Uani 1 1 d . . .
F25 F 0.5765(3) 0.1487(2) -0.2350(4) 0.0771(12) Uani 1 1 d . . .
F26 F 0.7843(3) 0.12838(18) -0.1704(3) 0.0611(10) Uani 1 1 d . . .
P21 P 0.67940(12) 0.11231(7) -0.29166(13) 0.0332(3) Uani 1 1 d . . .
F31 F 0.3894(4) 0.3626(3) -0.1257(3) 0.1039(16) Uani 1 1 d . . .
F32 F 0.4744(4) 0.2607(2) -0.0339(5) 0.1096(19) Uani 1 1 d . . .
F33 F 0.5986(5) 0.3503(4) -0.0659(4) 0.136(3) Uani 1 1 d . . .
F34 F 0.4999(4) 0.4281(2) 0.0350(5) 0.111(2) Uani 1 1 d . . .
F35 F 0.3781(4) 0.3387(3) 0.0631(5) 0.1140(18) Uani 1 1 d . . .
F36 F 0.5861(4) 0.3252(2) 0.1214(3) 0.0718(11) Uani 1 1 d . . .
P31 P 0.48888(14) 0.34378(8) -0.00278(13) 0.0382(3) Uani 1 1 d . . .
C51 C -0.0268(7) 0.3549(4) 0.1794(5) 0.070(2) Uani 1 1 d . . .
C52 C -0.1278(7) 0.4061(4) 0.1630(6) 0.076(2) Uani 1 1 d . . .
H52A H -0.1807 0.4016 0.0790 0.114 Uiso 1 1 calc R . .
H52B H -0.0946 0.4567 0.1760 0.114 Uiso 1 1 calc R . .
H52C H -0.1776 0.3955 0.2229 0.114 Uiso 1 1 calc R . .
N51 N 0.0493(8) 0.3130(5) 0.1897(6) 0.111(3) Uani 1 1 d . . .
O1 O 0.1701(5) 0.2335(3) 0.4205(5) 0.0699(13) Uani 1 1 d D . .
H1W H 0.171(7) 0.227(5) 0.345(3) 0.105 Uiso 1 1 d D . .
H2W H 0.106(5) 0.260(4) 0.418(6) 0.105 Uiso 1 1 d D . .
 
 
_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 1.356(5) . ?
C1 C2 1.375(6) . ?
C1 H1 0.9500 . ?
C2 C3 1.387(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.387(6) . ?
C3 C6 1.495(6) . ?
C4 C5 1.367(6) . ?
C4 H4 0.9500 . ?
C5 N1 1.359(5) . ?
C5 H5 0.9500 . ?
C6 C10 1.373(6) . ?
C6 C7 1.392(6) . ?
C7 C8 1.382(6) . ?
C7 H7 0.9500 . ?
C8 N2 1.339(6) . ?
C8 H8 0.9500 . ?
C9 N2 1.342(6) . ?
C9 C10 1.380(6) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 N2 1.488(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C21 N21 1.355(6) . ?
C21 C22 1.377(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.371(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.399(6) . ?
C23 C26 1.504(6) . ?
C24 C25 1.379(6) . ?
C24 H24 0.9500 . ?
C25 N21 1.348(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.382(6) . ?
C26 C30 1.386(6) . ?
C27 C28 1.359(7) . ?
C27 H27 0.9500 . ?
C28 N22 1.343(6) . ?
C28 H28 0.9500 . ?
C29 N22 1.330(6) . ?
C29 C30 1.379(7) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 N22 1.471(6) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
N1 Ru1 2.048(4) . ?
N21 Ru1 2.041(4) . ?
N41 Ru1 2.138(3) . ?
N41 H41A 0.9100 . ?
N41 H41B 0.9100 . ?
N41 H41C 0.9100 . ?
N42 Ru1 2.168(4) . ?
N42 H42A 0.9100 . ?
N42 H42B 0.9100 . ?
N42 H42C 0.9100 . ?
N43 Ru1 2.162(4) . ?
N43 H43A 0.9100 . ?
N43 H43B 0.9100 . ?
N43 H43C 0.9100 . ?
N44 Ru1 2.146(3) . ?
N44 H44A 0.9100 . ?
N44 H44B 0.9100 . ?
N44 H44C 0.9100 . ?
F1 P1 1.580(4) . ?
F2 P1 1.562(4) . ?
F3 P1 1.571(4) . ?
F4 P1 1.598(4) . ?
F5 P1 1.576(4) . ?
F6 P1 1.564(4) . ?
F11 P11 1.610(3) . ?
F12 P11 1.601(3) . ?
F13 P11 1.587(3) . ?
F14 P11 1.592(3) . ?
F15 P11 1.595(3) . ?
F16 P11 1.605(3) . ?
F21 P21 1.595(4) . ?
F22 P21 1.598(3) . ?
F23 P21 1.589(4) . ?
F24 P21 1.611(3) . ?
F25 P21 1.568(4) . ?
F26 P21 1.579(3) . ?
F31 P31 1.572(3) . ?
F32 P31 1.539(4) . ?
F33 P31 1.542(4) . ?
F34 P31 1.576(4) . ?
F35 P31 1.570(4) . ?
F36 P31 1.569(3) . ?
C51 N51 1.114(8) . ?
C51 C52 1.424(9) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
O1 H1W 0.86(2) . ?
O1 H2W 0.85(2) . ?
 
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 C2 123.6(4) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C1 C2 C3 119.6(4) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C4 C3 C2 117.7(4) . . ?
C4 C3 C6 122.2(4) . . ?
C2 C3 C6 120.0(4) . . ?
C5 C4 C3 119.5(4) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
N1 C5 C4 124.0(4) . . ?
N1 C5 H5 118.0 . . ?
C4 C5 H5 118.0 . . ?
C10 C6 C7 118.8(4) . . ?
C10 C6 C3 120.7(4) . . ?
C7 C6 C3 120.5(4) . . ?
C8 C7 C6 119.9(4) . . ?
C8 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
N2 C8 C7 119.6(4) . . ?
N2 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
N2 C9 C10 120.5(4) . . ?
N2 C9 H9 119.7 . . ?
C10 C9 H9 119.7 . . ?
C6 C10 C9 119.5(4) . . ?
C6 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N21 C21 C22 123.1(4) . . ?
N21 C21 H21 118.4 . . ?
C22 C21 H21 118.4 . . ?
C23 C22 C21 120.2(4) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C22 C23 C24 117.6(4) . . ?
C22 C23 C26 121.3(4) . . ?
C24 C23 C26 121.1(4) . . ?
C25 C24 C23 119.3(4) . . ?
C25 C24 H24 120.4 . . ?
C23 C24 H24 120.4 . . ?
N21 C25 C24 123.4(4) . . ?
N21 C25 H25 118.3 . . ?
C24 C25 H25 118.3 . . ?
C27 C26 C30 117.9(4) . . ?
C27 C26 C23 120.7(4) . . ?
C30 C26 C23 121.4(4) . . ?
C28 C27 C26 120.2(5) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
N22 C28 C27 121.5(5) . . ?
N22 C28 H28 119.2 . . ?
C27 C28 H28 119.2 . . ?
N22 C29 C30 121.8(4) . . ?
N22 C29 H29 119.1 . . ?
C30 C29 H29 119.1 . . ?
C29 C30 C26 119.1(5) . . ?
C29 C30 H30 120.4 . . ?
C26 C30 H30 120.4 . . ?
N22 C31 H31A 109.5 . . ?
N22 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N22 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C1 N1 C5 115.6(4) . . ?
C1 N1 Ru1 122.1(3) . . ?
C5 N1 Ru1 122.3(3) . . ?
C8 N2 C9 121.5(4) . . ?
C8 N2 C11 119.0(4) . . ?
C9 N2 C11 119.4(4) . . ?
C25 N21 C21 116.4(4) . . ?
C25 N21 Ru1 121.8(3) . . ?
C21 N21 Ru1 121.7(3) . . ?
C29 N22 C28 119.3(4) . . ?
C29 N22 C31 120.3(4) . . ?
C28 N22 C31 120.4(4) . . ?
Ru1 N41 H41A 109.5 . . ?
Ru1 N41 H41B 109.5 . . ?
H41A N41 H41B 109.5 . . ?
Ru1 N41 H41C 109.5 . . ?
H41A N41 H41C 109.5 . . ?
H41B N41 H41C 109.5 . . ?
Ru1 N42 H42A 109.5 . . ?
Ru1 N42 H42B 109.5 . . ?
H42A N42 H42B 109.5 . . ?
Ru1 N42 H42C 109.5 . . ?
H42A N42 H42C 109.5 . . ?
H42B N42 H42C 109.5 . . ?
Ru1 N43 H43A 109.5 . . ?
Ru1 N43 H43B 109.5 . . ?
H43A N43 H43B 109.5 . . ?
Ru1 N43 H43C 109.5 . . ?
H43A N43 H43C 109.5 . . ?
H43B N43 H43C 109.5 . . ?
Ru1 N44 H44A 109.5 . . ?
Ru1 N44 H44B 109.5 . . ?
H44A N44 H44B 109.5 . . ?
Ru1 N44 H44C 109.5 . . ?
H44A N44 H44C 109.5 . . ?
H44B N44 H44C 109.5 . . ?
N21 Ru1 N1 89.75(12) . . ?
N21 Ru1 N41 90.29(16) . . ?
N1 Ru1 N41 89.84(15) . . ?
N21 Ru1 N44 90.07(15) . . ?
N1 Ru1 N44 91.42(15) . . ?
N41 Ru1 N44 178.69(15) . . ?
N21 Ru1 N43 178.54(18) . . ?
N1 Ru1 N43 90.09(17) . . ?
N41 Ru1 N43 88.26(16) . . ?
N44 Ru1 N43 91.39(15) . . ?
N21 Ru1 N42 91.16(17) . . ?
N1 Ru1 N42 178.82(17) . . ?
N41 Ru1 N42 90.89(16) . . ?
N44 Ru1 N42 87.84(16) . . ?
N43 Ru1 N42 89.01(13) . . ?
F2 P1 F6 91.8(3) . . ?
F2 P1 F3 92.5(3) . . ?
F6 P1 F3 91.8(2) . . ?
F2 P1 F5 88.9(3) . . ?
F6 P1 F5 88.4(2) . . ?
F3 P1 F5 178.5(3) . . ?
F2 P1 F1 90.1(3) . . ?
F6 P1 F1 177.8(3) . . ?
F3 P1 F1 89.2(2) . . ?
F5 P1 F1 90.5(2) . . ?
F2 P1 F4 177.3(3) . . ?
F6 P1 F4 90.7(2) . . ?
F3 P1 F4 88.5(2) . . ?
F5 P1 F4 90.1(2) . . ?
F1 P1 F4 87.4(2) . . ?
F13 P11 F14 90.64(17) . . ?
F13 P11 F15 178.9(2) . . ?
F14 P11 F15 90.5(2) . . ?
F13 P11 F12 90.36(17) . . ?
F14 P11 F12 178.69(18) . . ?
F15 P11 F12 88.51(19) . . ?
F13 P11 F16 90.51(17) . . ?
F14 P11 F16 90.03(16) . . ?
F15 P11 F16 89.46(16) . . ?
F12 P11 F16 89.13(16) . . ?
F13 P11 F11 89.92(16) . . ?
F14 P11 F11 90.60(17) . . ?
F15 P11 F11 90.09(17) . . ?
F12 P11 F11 90.24(17) . . ?
F16 P11 F11 179.23(18) . . ?
F25 P21 F26 91.6(2) . . ?
F25 P21 F23 178.6(3) . . ?
F26 P21 F23 89.7(2) . . ?
F25 P21 F21 89.9(2) . . ?
F26 P21 F21 178.5(2) . . ?
F23 P21 F21 88.8(2) . . ?
F25 P21 F22 90.00(19) . . ?
F26 P21 F22 90.64(17) . . ?
F23 P21 F22 90.5(2) . . ?
F21 P21 F22 89.62(18) . . ?
F25 P21 F24 90.27(19) . . ?
F26 P21 F24 88.46(17) . . ?
F23 P21 F24 89.30(19) . . ?
F21 P21 F24 91.28(18) . . ?
F22 P21 F24 179.07(18) . . ?
F32 P31 F33 91.2(3) . . ?
F32 P31 F36 90.2(2) . . ?
F33 P31 F36 88.7(2) . . ?
F32 P31 F35 89.9(3) . . ?
F33 P31 F35 178.8(4) . . ?
F36 P31 F35 90.9(3) . . ?
F32 P31 F31 90.1(3) . . ?
F33 P31 F31 92.4(3) . . ?
F36 P31 F31 178.8(3) . . ?
F35 P31 F31 87.9(3) . . ?
F32 P31 F34 176.8(3) . . ?
F33 P31 F34 91.7(3) . . ?
F36 P31 F34 88.7(2) . . ?
F35 P31 F34 87.1(3) . . ?
F31 P31 F34 91.0(2) . . ?
N51 C51 C52 177.5(9) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
H1W O1 H2W 104(3) . . ?
 
_diffrn_measured_fraction_theta_max    0.997
_diffrn_reflns_theta_full              27.47
_diffrn_measured_fraction_theta_full   0.997
_refine_diff_density_max    0.667
_refine_diff_density_min   -0.444
_refine_diff_density_rms    0.083
