# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2010
data_global
_journal_name_full Chem.Commun.
_journal_coden_Cambridge 0182
_publ_contact_author_name R.Morris
_publ_contact_author_address
;
80 St George Street
Toronto
Ontario
Canada
M5S 1A1
;
_publ_contact_author_email rmorris@chem.utoronto.ca
loop_
_publ_author_name
W.N.O.Wylie
'Alan J. Lough'
'Robert H. Morris'
# end Validation Reply Form
data_3
_database_code_depnum_ccdc_archive 'CCDC 784228'
#TrackingRef '- OLoughMorris RuCpNHC.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C34 H38 N2 P Ru, F6 P'
_chemical_formula_sum 'C34 H38 F6 N2 P2 Ru'
_chemical_formula_weight 751.67
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'
P P 0.1023 0.0942 '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'
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 8.6982(2)
_cell_length_b 20.6135(8)
_cell_length_c 19.4091(7)
_cell_angle_alpha 90.00
_cell_angle_beta 92.051(2)
_cell_angle_gamma 90.00
_cell_volume 3477.8(2)
_cell_formula_units_Z 4
_cell_measurement_temperature 150(1)
_cell_measurement_reflns_used 16975
_cell_measurement_theta_min 2.6
_cell_measurement_theta_max 27.5
_exptl_crystal_description block
_exptl_crystal_colour orange
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.14
_exptl_crystal_size_min 0.08
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.436
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1536
_exptl_absorpt_coefficient_mu 0.601
# Absorption correction
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.863
_exptl_absorpt_correction_T_max 0.951
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Nonius KappaCCD'
_diffrn_measurement_method '\f scans and \w scans with \k offsets'
_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number 23696
_diffrn_reflns_av_R_equivalents 0.050
_diffrn_reflns_av_sigmaI/netI 0.063
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -26
_diffrn_reflns_limit_k_max 26
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_theta_min 2.72
_diffrn_reflns_theta_max 27.45
_reflns_number_total 7870
_reflns_number_gt 5540
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'Collect (Nonius B.V., 1997-2002)'
_computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction Denzo-SMN
_computing_structure_solution 'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_molecular_graphics 'PLATON (Spek, 2009)'
_computing_publication_material 'SHELXTL V6.1'
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A.,
Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst.
27, 435.
Blessing, R. H. (1995). Acta Cryst. A51, 33-38.
Nonius B.V (1997-2002). Collect. Data collection software, Delft,
The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
Macromolecular Crystallography, Part A edited by C. W. Carter &
R. M. Sweet pp. 307-326. London: Academic press.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A. L. (2009). Acta Cryst. D65, 148--155.
;
_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^)+(0.0617P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 7870
_refine_ls_number_parameters 411
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0754
_refine_ls_R_factor_gt 0.0448
_refine_ls_wR_factor_ref 0.1154
_refine_ls_wR_factor_gt 0.1036
_refine_ls_goodness_of_fit_ref 1.025
_refine_ls_restrained_S_all 1.025
_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
Ru1 Ru 0.48748(2) 0.633127(12) 0.688178(12) 0.02384(9) Uani 1 1 d . . .
P1 P 0.56360(8) 0.73056(4) 0.64098(4) 0.02507(18) Uani 1 1 d . . .
N1 N 0.5639(3) 0.59049(13) 0.59203(12) 0.0287(6) Uani 1 1 d . . .
H1C H 0.5542 0.5462 0.5962 0.034 Uiso 1 1 calc R . .
H1D H 0.4948 0.6033 0.5577 0.034 Uiso 1 1 calc R . .
N2 N 0.7117(3) 0.60822(13) 0.73338(12) 0.0274(6) Uani 1 1 d . . .
C1 C 0.7198(3) 0.60315(15) 0.56675(16) 0.0301(7) Uani 1 1 d . . .
H1A H 0.7431 0.5704 0.5313 0.036 Uiso 1 1 calc R . .
H1B H 0.7958 0.5978 0.6055 0.036 Uiso 1 1 calc R . .
C2 C 0.7384(3) 0.67010(15) 0.53619(15) 0.0272(7) Uani 1 1 d . . .
C3 C 0.8299(3) 0.67395(17) 0.47844(15) 0.0329(7) Uani 1 1 d . . .
H3A H 0.8757 0.6356 0.4615 0.040 Uiso 1 1 calc R . .
C4 C 0.8552(3) 0.73225(17) 0.44550(15) 0.0349(8) Uani 1 1 d . . .
H4A H 0.9195 0.7339 0.4070 0.042 Uiso 1 1 calc R . .
C5 C 0.7859(3) 0.78823(17) 0.46906(16) 0.0363(8) Uani 1 1 d . . .
H5A H 0.7997 0.8283 0.4460 0.044 Uiso 1 1 calc R . .
C6 C 0.6966(3) 0.78512(16) 0.52654(15) 0.0322(7) Uani 1 1 d . . .
H6A H 0.6495 0.8236 0.5426 0.039 Uiso 1 1 calc R . .
C7 C 0.6739(3) 0.72656(16) 0.56161(15) 0.0273(7) Uani 1 1 d . . .
C8 C 0.3688(3) 0.55913(16) 0.74898(16) 0.0300(7) Uani 1 1 d . . .
C9 C 0.3794(3) 0.62002(15) 0.78716(16) 0.0293(7) Uani 1 1 d . . .
C10 C 0.2924(3) 0.66766(15) 0.74824(16) 0.0283(7) Uani 1 1 d . . .
C11 C 0.2340(3) 0.63757(15) 0.68572(16) 0.0282(7) Uani 1 1 d . . .
C12 C 0.2809(3) 0.57090(15) 0.68775(15) 0.0293(7) Uani 1 1 d . . .
C13 C 0.4276(3) 0.49461(17) 0.77486(17) 0.0378(8) Uani 1 1 d . . .
H13A H 0.3462 0.4723 0.7993 0.057 Uiso 1 1 calc R . .
H13B H 0.5166 0.5014 0.8064 0.057 Uiso 1 1 calc R . .
H13C H 0.4582 0.4681 0.7358 0.057 Uiso 1 1 calc R . .
C14 C 0.4501(4) 0.62962(17) 0.85762(16) 0.0394(8) Uani 1 1 d . . .
H14A H 0.3726 0.6219 0.8921 0.059 Uiso 1 1 calc R . .
H14B H 0.4885 0.6742 0.8621 0.059 Uiso 1 1 calc R . .
H14C H 0.5356 0.5991 0.8649 0.059 Uiso 1 1 calc R . .
C15 C 0.2483(3) 0.73347(16) 0.77390(17) 0.0375(8) Uani 1 1 d . . .
H15A H 0.1411 0.7327 0.7878 0.056 Uiso 1 1 calc R . .
H15B H 0.2596 0.7655 0.7371 0.056 Uiso 1 1 calc R . .
H15C H 0.3153 0.7453 0.8136 0.056 Uiso 1 1 calc R . .
C16 C 0.1136(3) 0.66638(17) 0.63765(17) 0.0373(8) Uani 1 1 d . . .
H16A H 0.0113 0.6574 0.6550 0.056 Uiso 1 1 calc R . .
H16B H 0.1218 0.6471 0.5918 0.056 Uiso 1 1 calc R . .
H16C H 0.1290 0.7134 0.6348 0.056 Uiso 1 1 calc R . .
C17 C 0.2362(3) 0.52126(16) 0.63392(16) 0.0348(8) Uani 1 1 d . . .
H17A H 0.1319 0.5056 0.6419 0.052 Uiso 1 1 calc R . .
H17B H 0.3085 0.4848 0.6367 0.052 Uiso 1 1 calc R . .
H17C H 0.2390 0.5411 0.5881 0.052 Uiso 1 1 calc R . .
C18 C 0.7651(3) 0.54697(16) 0.72484(16) 0.0328(7) Uani 1 1 d . . .
H18A H 0.7089 0.5188 0.6945 0.039 Uiso 1 1 calc R . .
C19 C 0.8962(3) 0.52365(17) 0.75774(17) 0.0369(8) Uani 1 1 d . . .
H19A H 0.9296 0.4805 0.7499 0.044 Uiso 1 1 calc R . .
C20 C 0.9781(3) 0.56349(19) 0.80208(17) 0.0398(8) Uani 1 1 d . . .
H20A H 1.0696 0.5486 0.8251 0.048 Uiso 1 1 calc R . .
C21 C 0.9249(3) 0.62574(16) 0.81263(16) 0.0329(8) Uani 1 1 d . . .
H21A H 0.9790 0.6542 0.8434 0.039 Uiso 1 1 calc R . .
C22 C 0.7929(3) 0.64600(16) 0.77802(15) 0.0294(7) Uani 1 1 d . . .
H22A H 0.7571 0.6888 0.7860 0.035 Uiso 1 1 calc R . .
C23 C 0.4104(3) 0.78535(15) 0.60899(15) 0.0291(7) Uani 1 1 d . . .
C24 C 0.3283(3) 0.76634(17) 0.54910(16) 0.0358(8) Uani 1 1 d . . .
H24A H 0.3546 0.7269 0.5271 0.043 Uiso 1 1 calc R . .
C25 C 0.2105(4) 0.80347(18) 0.52130(18) 0.0427(9) Uani 1 1 d . . .
H25A H 0.1575 0.7898 0.4802 0.051 Uiso 1 1 calc R . .
C26 C 0.1687(4) 0.86052(19) 0.5529(2) 0.0476(10) Uani 1 1 d . . .
H26A H 0.0853 0.8855 0.5343 0.057 Uiso 1 1 calc R . .
C27 C 0.2493(4) 0.88112(18) 0.61183(19) 0.0441(9) Uani 1 1 d . . .
H27A H 0.2221 0.9208 0.6331 0.053 Uiso 1 1 calc R . .
C28 C 0.3701(4) 0.84411(16) 0.64014(16) 0.0338(7) Uani 1 1 d . . .
H28A H 0.4250 0.8586 0.6804 0.041 Uiso 1 1 calc R . .
C29 C 0.6867(3) 0.78419(14) 0.69518(15) 0.0254(6) Uani 1 1 d . . .
C30 C 0.6304(3) 0.80429(15) 0.75860(15) 0.0267(7) Uani 1 1 d . . .
H30A H 0.5301 0.7914 0.7709 0.032 Uiso 1 1 calc R . .
C31 C 0.7178(3) 0.84243(16) 0.80361(16) 0.0297(7) Uani 1 1 d . . .
H31A H 0.6763 0.8567 0.8456 0.036 Uiso 1 1 calc R . .
C32 C 0.8661(3) 0.85979(15) 0.78717(16) 0.0310(7) Uani 1 1 d . . .
H32A H 0.9274 0.8854 0.8182 0.037 Uiso 1 1 calc R . .
C33 C 0.9246(3) 0.83952(16) 0.72501(16) 0.0318(7) Uani 1 1 d . . .
H33A H 1.0262 0.8514 0.7137 0.038 Uiso 1 1 calc R . .
C34 C 0.8356(3) 0.80202(15) 0.67934(16) 0.0297(7) Uani 1 1 d . . .
H34A H 0.8768 0.7885 0.6370 0.036 Uiso 1 1 calc R . .
P2 P 0.70518(9) 0.38944(4) 0.59738(4) 0.0299(2) Uani 1 1 d . . .
F1 F 0.5715(2) 0.44342(10) 0.59630(12) 0.0612(6) Uani 1 1 d . . .
F2 F 0.8317(2) 0.44577(10) 0.59944(10) 0.0508(5) Uani 1 1 d . . .
F3 F 0.7075(3) 0.38912(11) 0.67978(10) 0.0567(6) Uani 1 1 d . . .
F4 F 0.8361(2) 0.33609(10) 0.59816(11) 0.0484(5) Uani 1 1 d . . .
F5 F 0.5780(2) 0.33398(10) 0.59515(10) 0.0448(5) Uani 1 1 d . . .
F6 F 0.7018(2) 0.39097(11) 0.51474(9) 0.0497(5) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.02343(14) 0.02259(15) 0.02557(15) -0.00187(10) 0.00182(9) -0.00291(10)
P1 0.0264(4) 0.0229(4) 0.0260(4) -0.0020(3) 0.0026(3) -0.0040(3)
N1 0.0290(13) 0.0268(15) 0.0304(14) -0.0045(12) 0.0030(10) -0.0066(11)
N2 0.0275(13) 0.0280(15) 0.0266(14) -0.0001(12) 0.0016(10) -0.0032(11)
C1 0.0300(16) 0.0275(18) 0.0331(18) -0.0049(14) 0.0060(13) -0.0016(13)
C2 0.0274(15) 0.0298(18) 0.0243(16) -0.0012(13) -0.0030(12) -0.0029(13)
C3 0.0326(16) 0.040(2) 0.0262(17) -0.0047(15) 0.0018(13) -0.0038(14)
C4 0.0329(16) 0.049(2) 0.0234(16) -0.0025(16) 0.0043(13) -0.0099(15)
C5 0.0344(17) 0.039(2) 0.0355(19) 0.0079(16) 0.0042(14) -0.0075(15)
C6 0.0302(16) 0.034(2) 0.0325(18) -0.0009(15) 0.0045(13) -0.0029(14)
C7 0.0256(15) 0.0323(19) 0.0240(16) -0.0017(14) 0.0006(12) -0.0040(13)
C8 0.0286(15) 0.0292(18) 0.0327(18) 0.0026(14) 0.0061(12) -0.0056(13)
C9 0.0270(15) 0.0331(19) 0.0282(17) -0.0010(14) 0.0066(12) -0.0076(13)
C10 0.0233(14) 0.0262(18) 0.0360(18) -0.0039(14) 0.0103(12) -0.0033(12)
C11 0.0195(14) 0.0297(18) 0.0358(18) 0.0013(14) 0.0038(12) -0.0045(12)
C12 0.0284(15) 0.0284(18) 0.0311(17) -0.0009(14) 0.0024(12) -0.0096(13)
C13 0.0378(17) 0.036(2) 0.040(2) 0.0103(16) 0.0042(14) -0.0021(15)
C14 0.0430(19) 0.046(2) 0.0289(18) -0.0002(16) 0.0045(14) -0.0079(16)
C15 0.0312(16) 0.035(2) 0.047(2) -0.0050(16) 0.0151(14) -0.0025(14)
C16 0.0288(16) 0.040(2) 0.043(2) 0.0039(17) 0.0017(14) -0.0011(14)
C17 0.0341(17) 0.032(2) 0.0381(19) -0.0029(15) -0.0005(14) -0.0097(14)
C18 0.0359(17) 0.0277(19) 0.0348(18) -0.0018(15) 0.0033(13) -0.0010(14)
C19 0.0372(18) 0.034(2) 0.040(2) 0.0011(16) 0.0068(15) 0.0062(15)
C20 0.0271(16) 0.050(2) 0.042(2) 0.0088(18) 0.0014(14) 0.0043(16)
C21 0.0274(16) 0.043(2) 0.0282(17) 0.0019(15) -0.0018(13) -0.0081(14)
C22 0.0292(16) 0.0290(18) 0.0301(17) -0.0005(14) 0.0040(13) -0.0034(13)
C23 0.0277(15) 0.0318(18) 0.0280(16) 0.0015(14) 0.0016(12) -0.0065(13)
C24 0.0344(17) 0.035(2) 0.0376(19) 0.0003(16) -0.0011(14) -0.0063(15)
C25 0.0386(18) 0.045(2) 0.044(2) 0.0040(18) -0.0084(15) -0.0058(17)
C26 0.0350(19) 0.053(3) 0.054(2) 0.013(2) -0.0106(16) 0.0072(17)
C27 0.045(2) 0.037(2) 0.051(2) 0.0039(18) 0.0061(17) 0.0103(16)
C28 0.0388(18) 0.0324(19) 0.0299(18) 0.0009(15) -0.0005(13) -0.0004(15)
C29 0.0259(15) 0.0205(16) 0.0297(16) 0.0014(13) -0.0021(12) -0.0006(12)
C30 0.0274(15) 0.0227(17) 0.0300(17) 0.0006(14) 0.0006(12) -0.0009(13)
C31 0.0371(17) 0.0252(17) 0.0266(17) 0.0001(14) -0.0002(13) 0.0052(14)
C32 0.0304(16) 0.0255(18) 0.0362(19) -0.0028(14) -0.0099(13) -0.0051(13)
C33 0.0259(15) 0.0295(18) 0.0399(19) 0.0024(15) 0.0008(13) -0.0034(13)
C34 0.0273(15) 0.0274(18) 0.0347(18) 0.0003(14) 0.0050(13) 0.0000(13)
P2 0.0310(4) 0.0276(5) 0.0310(5) -0.0017(4) 0.0017(3) -0.0006(3)
F1 0.0504(12) 0.0361(13) 0.0973(18) 0.0006(12) 0.0063(11) 0.0142(10)
F2 0.0520(12) 0.0451(13) 0.0554(13) -0.0033(10) 0.0018(9) -0.0205(10)
F3 0.0891(16) 0.0510(14) 0.0306(11) -0.0059(10) 0.0101(10) -0.0083(12)
F4 0.0380(10) 0.0471(13) 0.0600(14) 0.0004(11) -0.0019(9) 0.0094(9)
F5 0.0356(10) 0.0380(12) 0.0613(13) -0.0041(10) 0.0082(9) -0.0093(8)
F6 0.0628(13) 0.0558(14) 0.0303(11) 0.0041(10) -0.0039(9) -0.0088(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
Ru1 N2 2.171(2) . ?
Ru1 C9 2.186(3) . ?
Ru1 N1 2.188(2) . ?
Ru1 C11 2.206(3) . ?
Ru1 C8 2.207(3) . ?
Ru1 C12 2.208(3) . ?
Ru1 C10 2.210(3) . ?
Ru1 P1 2.3140(8) . ?
P1 C23 1.838(3) . ?
P1 C29 1.843(3) . ?
P1 C7 1.846(3) . ?
N1 C1 1.481(3) . ?
N2 C22 1.346(4) . ?
N2 C18 1.358(4) . ?
C1 C2 1.513(4) . ?
C2 C7 1.390(4) . ?
C2 C3 1.400(4) . ?
C3 C4 1.383(5) . ?
C4 C5 1.387(5) . ?
C5 C6 1.384(4) . ?
C6 C7 1.403(4) . ?
C8 C12 1.411(4) . ?
C8 C9 1.459(4) . ?
C8 C13 1.505(4) . ?
C9 C10 1.437(4) . ?
C9 C14 1.493(4) . ?
C10 C11 1.439(4) . ?
C10 C15 1.500(4) . ?
C11 C12 1.434(4) . ?
C11 C16 1.500(4) . ?
C12 C17 1.504(4) . ?
C18 C19 1.373(4) . ?
C19 C20 1.371(5) . ?
C20 C21 1.382(5) . ?
C21 C22 1.375(4) . ?
C23 C24 1.398(4) . ?
C23 C28 1.404(4) . ?
C24 C25 1.374(4) . ?
C25 C26 1.381(5) . ?
C26 C27 1.387(5) . ?
C27 C28 1.395(5) . ?
C29 C34 1.392(4) . ?
C29 C30 1.404(4) . ?
C30 C31 1.383(4) . ?
C31 C32 1.387(4) . ?
C32 C33 1.390(4) . ?
C33 C34 1.390(4) . ?
P2 F4 1.583(2) . ?
P2 F5 1.591(2) . ?
P2 F3 1.599(2) . ?
P2 F2 1.599(2) . ?
P2 F6 1.603(2) . ?
P2 F1 1.609(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
N2 Ru1 C9 91.38(10) . . ?
N2 Ru1 N1 87.35(9) . . ?
C9 Ru1 N1 148.60(11) . . ?
N2 Ru1 C11 154.33(10) . . ?
C9 Ru1 C11 64.08(11) . . ?
N1 Ru1 C11 109.41(10) . . ?
N2 Ru1 C8 92.93(10) . . ?
C9 Ru1 C8 38.79(11) . . ?
N1 Ru1 C8 109.92(10) . . ?
C11 Ru1 C8 63.51(11) . . ?
N2 Ru1 C12 125.69(11) . . ?
C9 Ru1 C12 63.62(11) . . ?
N1 Ru1 C12 92.04(10) . . ?
C11 Ru1 C12 37.91(11) . . ?
C8 Ru1 C12 37.27(11) . . ?
N2 Ru1 C10 123.94(10) . . ?
C9 Ru1 C10 38.16(11) . . ?
N1 Ru1 C10 147.32(10) . . ?
C11 Ru1 C10 38.04(11) . . ?
C8 Ru1 C10 63.77(11) . . ?
C12 Ru1 C10 63.20(11) . . ?
N2 Ru1 P1 95.72(7) . . ?
C9 Ru1 P1 126.40(9) . . ?
N1 Ru1 P1 84.89(7) . . ?
C11 Ru1 P1 104.80(8) . . ?
C8 Ru1 P1 163.20(8) . . ?
C12 Ru1 P1 138.35(8) . . ?
C10 Ru1 P1 99.51(8) . . ?
C23 P1 C29 102.93(14) . . ?
C23 P1 C7 97.91(13) . . ?
C29 P1 C7 101.22(13) . . ?
C23 P1 Ru1 116.92(9) . . ?
C29 P1 Ru1 117.61(10) . . ?
C7 P1 Ru1 117.15(11) . . ?
C1 N1 Ru1 121.43(18) . . ?
C22 N2 C18 116.3(3) . . ?
C22 N2 Ru1 124.5(2) . . ?
C18 N2 Ru1 118.5(2) . . ?
N1 C1 C2 113.7(2) . . ?
C7 C2 C3 119.0(3) . . ?
C7 C2 C1 125.0(3) . . ?
C3 C2 C1 115.9(3) . . ?
C4 C3 C2 121.6(3) . . ?
C3 C4 C5 119.5(3) . . ?
C6 C5 C4 119.4(3) . . ?
C5 C6 C7 121.6(3) . . ?
C2 C7 C6 118.8(3) . . ?
C2 C7 P1 124.2(2) . . ?
C6 C7 P1 116.9(2) . . ?
C12 C8 C9 107.6(3) . . ?
C12 C8 C13 126.9(3) . . ?
C9 C8 C13 125.2(3) . . ?
C12 C8 Ru1 71.38(17) . . ?
C9 C8 Ru1 69.80(17) . . ?
C13 C8 Ru1 129.0(2) . . ?
C10 C9 C8 107.4(3) . . ?
C10 C9 C14 125.6(3) . . ?
C8 C9 C14 126.6(3) . . ?
C10 C9 Ru1 71.85(16) . . ?
C8 C9 Ru1 71.41(16) . . ?
C14 C9 Ru1 127.8(2) . . ?
C9 C10 C11 108.2(3) . . ?
C9 C10 C15 125.4(3) . . ?
C11 C10 C15 125.6(3) . . ?
C9 C10 Ru1 69.99(16) . . ?
C11 C10 Ru1 70.81(16) . . ?
C15 C10 Ru1 132.6(2) . . ?
C12 C11 C10 107.4(3) . . ?
C12 C11 C16 126.0(3) . . ?
C10 C11 C16 124.9(3) . . ?
C12 C11 Ru1 71.11(16) . . ?
C10 C11 Ru1 71.15(15) . . ?
C16 C11 Ru1 134.8(2) . . ?
C8 C12 C11 109.5(3) . . ?
C8 C12 C17 126.0(3) . . ?
C11 C12 C17 124.5(3) . . ?
C8 C12 Ru1 71.35(16) . . ?
C11 C12 Ru1 70.97(16) . . ?
C17 C12 Ru1 126.0(2) . . ?
N2 C18 C19 123.4(3) . . ?
C20 C19 C18 119.1(3) . . ?
C19 C20 C21 118.7(3) . . ?
C22 C21 C20 119.2(3) . . ?
N2 C22 C21 123.3(3) . . ?
C24 C23 C28 118.2(3) . . ?
C24 C23 P1 116.8(2) . . ?
C28 C23 P1 125.0(2) . . ?
C25 C24 C23 121.5(3) . . ?
C24 C25 C26 120.3(3) . . ?
C25 C26 C27 119.6(3) . . ?
C26 C27 C28 120.6(3) . . ?
C27 C28 C23 119.9(3) . . ?
C34 C29 C30 118.2(3) . . ?
C34 C29 P1 124.0(2) . . ?
C30 C29 P1 117.6(2) . . ?
C31 C30 C29 121.4(3) . . ?
C30 C31 C32 119.7(3) . . ?
C31 C32 C33 119.6(3) . . ?
C34 C33 C32 120.5(3) . . ?
C33 C34 C29 120.5(3) . . ?
F4 P2 F5 90.02(11) . . ?
F4 P2 F3 90.24(12) . . ?
F5 P2 F3 90.47(11) . . ?
F4 P2 F2 90.57(11) . . ?
F5 P2 F2 179.40(13) . . ?
F3 P2 F2 89.65(11) . . ?
F4 P2 F6 90.62(11) . . ?
F5 P2 F6 89.94(11) . . ?
F3 P2 F6 179.05(13) . . ?
F2 P2 F6 89.94(11) . . ?
F4 P2 F1 179.68(14) . . ?
F5 P2 F1 89.72(11) . . ?
F3 P2 F1 89.95(13) . . ?
F2 P2 F1 89.69(12) . . ?
F6 P2 F1 89.19(12) . . ?
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 F1 0.92 2.12 3.033(3) 169.2 .
N1 H1D F6 0.92 2.18 3.072(3) 163.9 3_666
_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max 1.106
_refine_diff_density_min -0.858
_refine_diff_density_rms 0.098
_vrf_PLAT601_k10135
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of 179.00 A**3
RESPONSE:
During the
refinement of the structure, electron density peaks were located
that were believed to be highly disordered
solvent molecules (possibly dichloromethane and/or diethylether).
Attempts made to model the solvent molecule were not successful.
The SQUEEZE option in PLATON (Spek, 2003) indicated there was a
solvent cavity of volume 179.0 \%A^3^ containing approximately 32
electrons. In the final cycles of refinement, this contribution to the
electron density was removed from the observed data. The
density, the F(000) value, the molecular weight and the formula are
given without taking into account the results obtained with the
SQUEEZE option PLATON (Spek, 2003). Similar treatments of disordered
solvent molecules were carried out by St\"ahler et al. (2001),
Cox et al. (2003), Mohamed et al. (2003) and Athimoolam et al. (2005).
References:
Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13
Athimoolam, S., Kumar, J., Ramakrishnan, V. & Rajaram, R.K. (2005).
Acta Cryst. E61, m2014-m2017.
Cox, J.P., Kumarasammy, Y., Nahar, L., Sarkar D.S. & Shoeb, M.
(2003). Acta Cryst. E59, o975-o977.
Mohamed, A.A., Krause Bauer, A.J., Bruce, E.A. & Bruce M.R.M.
(2003). Acta Cryst. C59, m84-m86.
St\"ahler, R., N\"ather, C. & Bensch, W. (2001). Acta Cryst.
C57, 26-27.
;
# end Validation Reply Form
# Attachment '- OLoughMorris RuCpNHC.cif'
data_2a
_database_code_depnum_ccdc_archive 'CCDC 784229'
#TrackingRef '- OLoughMorris RuCpNHC.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C26 H33 N4 Ru, F6 P'
_chemical_formula_sum 'C26 H33 F6 N4 P Ru'
_chemical_formula_weight 647.60
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'
F F 0.0171 0.0103 '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'
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'
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 12.973(1)
_cell_length_b 13.1208(7)
_cell_length_c 17.1470(14)
_cell_angle_alpha 73.954(4)
_cell_angle_beta 73.396(3)
_cell_angle_gamma 88.187(4)
_cell_volume 2684.5(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 150(1)
_cell_measurement_reflns_used 25132
_cell_measurement_theta_min 2.6
_cell_measurement_theta_max 27.5
_exptl_crystal_description plate
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.14
_exptl_crystal_size_min 0.04
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.602
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1320
_exptl_absorpt_coefficient_mu 0.709
# Absorption correction
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.826
_exptl_absorpt_correction_T_max 0.990
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(1)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Nonius KappaCCD'
_diffrn_measurement_method '\f scans and \w scans with \k offsets'
_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number 12107
_diffrn_reflns_av_R_equivalents 0.092
_diffrn_reflns_av_sigmaI/netI 0.1448
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_theta_min 2.58
_diffrn_reflns_theta_max 27.65
_reflns_number_total 12107
_reflns_number_gt 6520
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'Collect (Nonius B.V., 1997-2002)'
_computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction Denzo-SMN
_computing_structure_solution 'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_molecular_graphics 'PLATON (Spek, 2009)'
_computing_publication_material 'SHELXTL V6.1'
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A.,
Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst.
27, 435.
Blessing, R. H. (1995). Acta Cryst. A51, 33-38.
Nonius B.V (1997-2002). Collect. Data collection software, Delft,
The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
Macromolecular Crystallography, Part A edited by C. W. Carter &
R. M. Sweet pp. 307-326. London: Academic press.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A. L. (2009). Acta Cryst. D65, 148--155.
;
_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^)+(0.1173P)^2^+1.3981P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 12107
_refine_ls_number_parameters 719
_refine_ls_number_restraints 7
_refine_ls_R_factor_all 0.1650
_refine_ls_R_factor_gt 0.0854
_refine_ls_wR_factor_ref 0.2473
_refine_ls_wR_factor_gt 0.2046
_refine_ls_goodness_of_fit_ref 1.033
_refine_ls_restrained_S_all 1.034
_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
Ru1A Ru 0.66721(6) 0.33242(5) 0.66050(5) 0.0363(2) Uani 1 1 d . . .
N1A N 0.6837(8) 0.0896(6) 0.7363(6) 0.055(2) Uani 1 1 d . . .
N2A N 0.6235(7) 0.1632(5) 0.8361(5) 0.0409(19) Uani 1 1 d . . .
N3A N 0.7434(6) 0.4130(6) 0.7278(5) 0.0393(18) Uani 1 1 d . . .
H3A1 H 0.8134 0.4316 0.6950 0.047 Uiso 1 1 calc R . .
H3A2 H 0.7092 0.4752 0.7295 0.047 Uiso 1 1 calc R . .
N4A N 0.8334(7) 0.3163(6) 0.5962(6) 0.046(2) Uani 1 1 d . . .
C1A C 0.6629(9) 0.1897(7) 0.7470(7) 0.046(2) Uani 1 1 d . . .
C2A C 0.6593(11) 0.0091(8) 0.8123(8) 0.062(3) Uani 1 1 d . . .
H2AA H 0.6681 -0.0646 0.8187 0.075 Uiso 1 1 calc R . .
C3A C 0.6217(9) 0.0541(8) 0.8735(8) 0.053(3) Uani 1 1 d . . .
H3AA H 0.5977 0.0189 0.9324 0.064 Uiso 1 1 calc R . .
C4A C 0.5778(8) 0.2348(7) 0.8850(6) 0.042(2) Uani 1 1 d . . .
C5A C 0.4763(9) 0.2081(9) 0.9442(7) 0.052(3) Uani 1 1 d . . .
H5AA H 0.4389 0.1438 0.9506 0.063 Uiso 1 1 calc R . .
C6A C 0.4301(9) 0.2738(9) 0.9931(7) 0.053(3) Uani 1 1 d . . .
H6AA H 0.3607 0.2558 1.0327 0.064 Uiso 1 1 calc R . .
C7A C 0.4851(10) 0.3653(9) 0.9844(7) 0.057(3) Uani 1 1 d . . .
H7AA H 0.4540 0.4110 1.0182 0.068 Uiso 1 1 calc R . .
C8A C 0.5861(10) 0.3917(8) 0.9264(7) 0.051(3) Uani 1 1 d . . .
H8AA H 0.6230 0.4553 0.9220 0.061 Uiso 1 1 calc R . .
C9A C 0.6356(8) 0.3287(7) 0.8743(6) 0.042(2) Uani 1 1 d . . .
C10A C 0.7467(8) 0.3590(8) 0.8146(6) 0.041(2) Uani 1 1 d . . .
H10A H 0.7843 0.4066 0.8347 0.049 Uiso 1 1 calc R . .
H10B H 0.7881 0.2943 0.8142 0.049 Uiso 1 1 calc R . .
C11A C 0.7281(11) 0.0682(9) 0.6538(8) 0.065(3) Uani 1 1 d . . .
H11F H 0.7386 0.1350 0.6086 0.098 Uiso 1 1 calc R . .
H11G H 0.6780 0.0200 0.6463 0.098 Uiso 1 1 calc R . .
H11H H 0.7974 0.0353 0.6516 0.098 Uiso 1 1 calc R . .
C12A C 0.5406(8) 0.2910(7) 0.6128(6) 0.042(2) Uani 1 1 d . . .
C13A C 0.6069(7) 0.3743(8) 0.5471(6) 0.039(2) Uani 1 1 d . . .
C14A C 0.6041(8) 0.4654(7) 0.5784(7) 0.043(2) Uani 1 1 d . . .
C15A C 0.5341(7) 0.4366(7) 0.6627(6) 0.034(2) Uani 1 1 d . . .
C16A C 0.4922(8) 0.3299(8) 0.6864(6) 0.042(2) Uani 1 1 d . . .
C17A C 0.5075(9) 0.1871(9) 0.6032(8) 0.061(3) Uani 1 1 d . . .
H17D H 0.4480 0.1978 0.5776 0.091 Uiso 1 1 calc R . .
H17E H 0.4842 0.1351 0.6591 0.091 Uiso 1 1 calc R . .
H17F H 0.5689 0.1608 0.5667 0.091 Uiso 1 1 calc R . .
C18A C 0.6621(9) 0.3675(10) 0.4586(6) 0.057(3) Uani 1 1 d . . .
H18D H 0.6079 0.3543 0.4322 0.085 Uiso 1 1 calc R . .
H18E H 0.7113 0.3092 0.4611 0.085 Uiso 1 1 calc R . .
H18F H 0.7029 0.4345 0.4250 0.085 Uiso 1 1 calc R . .
C19A C 0.6538(9) 0.5746(8) 0.5263(7) 0.052(3) Uani 1 1 d . . .
H19D H 0.6036 0.6139 0.4973 0.077 Uiso 1 1 calc R . .
H19E H 0.7210 0.5676 0.4842 0.077 Uiso 1 1 calc R . .
H19F H 0.6691 0.6130 0.5637 0.077 Uiso 1 1 calc R . .
C20A C 0.5008(9) 0.5107(8) 0.7189(8) 0.055(3) Uani 1 1 d . . .
H20D H 0.4320 0.5405 0.7138 0.082 Uiso 1 1 calc R . .
H20E H 0.5560 0.5683 0.7010 0.082 Uiso 1 1 calc R . .
H20F H 0.4929 0.4709 0.7779 0.082 Uiso 1 1 calc R . .
C21A C 0.4054(8) 0.2747(8) 0.7625(7) 0.052(3) Uani 1 1 d . . .
H21D H 0.3369 0.2787 0.7486 0.078 Uiso 1 1 calc R . .
H21E H 0.4000 0.3086 0.8076 0.078 Uiso 1 1 calc R . .
H21F H 0.4218 0.2001 0.7816 0.078 Uiso 1 1 calc R . .
C22A C 0.8997(9) 0.2496(10) 0.6330(7) 0.059(3) Uani 1 1 d . . .
H22B H 0.8718 0.2086 0.6902 0.071 Uiso 1 1 calc R . .
C23A C 1.0041(10) 0.2392(10) 0.5913(8) 0.067(3) Uani 1 1 d . . .
H23B H 1.0458 0.1898 0.6195 0.080 Uiso 1 1 calc R . .
C24A C 1.0498(9) 0.2979(9) 0.5101(7) 0.053(3) Uani 1 1 d . . .
H24B H 1.1231 0.2914 0.4815 0.064 Uiso 1 1 calc R . .
C25A C 0.9875(8) 0.3654(8) 0.4720(7) 0.046(2) Uani 1 1 d . . .
H25C H 1.0153 0.4069 0.4148 0.056 Uiso 1 1 calc R . .
C26A C 0.8835(8) 0.3732(8) 0.5170(7) 0.048(2) Uani 1 1 d . . .
H26B H 0.8426 0.4242 0.4891 0.057 Uiso 1 1 calc R . .
Ru1B Ru 0.84755(6) 0.18158(6) 1.15748(5) 0.0360(2) Uani 1 1 d . . .
N1B N 0.6047(7) 0.2212(7) 1.2263(6) 0.050(2) Uani 1 1 d . . .
N2B N 0.6684(6) 0.1490(6) 1.3292(5) 0.0441(19) Uani 1 1 d . . .
N3B N 0.9302(6) 0.2488(6) 1.2277(5) 0.0384(18) Uani 1 1 d . . .
H3B1 H 0.9908 0.2113 1.2303 0.046 Uiso 1 1 calc R . .
H3B2 H 0.9534 0.3172 1.1959 0.046 Uiso 1 1 calc R . .
N4B N 0.8417(7) 0.3482(6) 1.0934(5) 0.0421(19) Uani 1 1 d . . .
C1B C 0.6996(7) 0.1885(8) 1.2422(7) 0.041(2) Uani 1 1 d . . .
C2B C 0.5224(8) 0.2022(10) 1.2981(8) 0.060(3) Uani 1 1 d . . .
H2BA H 0.4496 0.2179 1.3012 0.072 Uiso 1 1 calc R . .
C3B C 0.5591(8) 0.1580(9) 1.3634(7) 0.050(3) Uani 1 1 d . . .
H3BA H 0.5191 0.1370 1.4216 0.060 Uiso 1 1 calc R . .
C4B C 0.7361(8) 0.0972(7) 1.3817(6) 0.039(2) Uani 1 1 d . . .
C5B C 0.6955(9) 0.0016(9) 1.4396(7) 0.058(3) Uani 1 1 d . . .
H5BA H 0.6279 -0.0283 1.4433 0.070 Uiso 1 1 calc R . .
C6B C 0.7569(11) -0.0511(10) 1.4934(8) 0.065(3) Uani 1 1 d . . .
H6BA H 0.7298 -0.1161 1.5354 0.078 Uiso 1 1 calc R . .
C7B C 0.8560(9) -0.0077(8) 1.4847(7) 0.052(3) Uani 1 1 d . . .
H7BA H 0.8995 -0.0452 1.5182 0.062 Uiso 1 1 calc R . .
C8B C 0.8932(9) 0.0907(8) 1.4271(7) 0.046(2) Uani 1 1 d . . .
H8BA H 0.9604 0.1216 1.4231 0.056 Uiso 1 1 calc R . .
C9B C 0.8317(8) 0.1436(7) 1.3753(6) 0.038(2) Uani 1 1 d . . .
C11B C 0.5922(10) 0.2680(10) 1.1421(8) 0.066(3) Uani 1 1 d . . .
H11A H 0.5283 0.2352 1.1374 0.099 Uiso 1 1 calc R . .
H11B H 0.6561 0.2558 1.0993 0.099 Uiso 1 1 calc R . .
H11C H 0.5839 0.3445 1.1330 0.099 Uiso 1 1 calc R . .
C10B C 0.8724(8) 0.2528(7) 1.3158(6) 0.039(2) Uani 1 1 d . . .
H10D H 0.8107 0.2988 1.3142 0.046 Uiso 1 1 calc R . .
H10E H 0.9218 0.2849 1.3381 0.046 Uiso 1 1 calc R . .
C12B C 0.7926(9) 0.0515(7) 1.1193(7) 0.046(3) Uani 1 1 d . . .
C13B C 0.8729(9) 0.1145(7) 1.0489(6) 0.047(2) Uani 1 1 d . . .
C14B C 0.9717(8) 0.1127(7) 1.0689(6) 0.042(2) Uani 1 1 d . . .
C15B C 0.9513(8) 0.0482(7) 1.1563(7) 0.043(2) Uani 1 1 d . . .
C16B C 0.8428(8) 0.0097(7) 1.1871(6) 0.040(2) Uani 1 1 d . . .
C17B C 0.6814(9) 0.0229(9) 1.1231(8) 0.059(3) Uani 1 1 d . . .
H17A H 0.6802 -0.0453 1.1103 0.089 Uiso 1 1 calc R . .
H17B H 0.6571 0.0780 1.0815 0.089 Uiso 1 1 calc R . .
H17C H 0.6335 0.0170 1.1800 0.089 Uiso 1 1 calc R . .
C18B C 0.8534(9) 0.1614(9) 0.9615(7) 0.056(3) Uiso 1 1 d . . .
H18A H 0.8386 0.1036 0.9397 0.083 Uiso 1 1 calc R . .
H18B H 0.9176 0.2039 0.9220 0.083 Uiso 1 1 calc R . .
H18C H 0.7916 0.2066 0.9674 0.083 Uiso 1 1 calc R . .
C19B C 1.0786(10) 0.1569(9) 1.0080(9) 0.068(4) Uani 1 1 d . . .
H19A H 1.1103 0.1057 0.9769 0.101 Uiso 1 1 calc R . .
H19B H 1.1267 0.1706 1.0393 0.101 Uiso 1 1 calc R . .
H19C H 1.0690 0.2235 0.9679 0.101 Uiso 1 1 calc R . .
C20B C 1.0370(9) 0.0187(9) 1.2017(8) 0.057(3) Uani 1 1 d . . .
H20A H 1.0627 -0.0512 1.1975 0.086 Uiso 1 1 calc R . .
H20B H 1.0064 0.0163 1.2615 0.086 Uiso 1 1 calc R . .
H20C H 1.0972 0.0719 1.1756 0.086 Uiso 1 1 calc R . .
C21B C 0.7958(10) -0.0748(8) 1.2668(7) 0.055(3) Uani 1 1 d . . .
H21A H 0.8006 -0.1439 1.2550 0.083 Uiso 1 1 calc R . .
H21B H 0.7201 -0.0617 1.2907 0.083 Uiso 1 1 calc R . .
H21C H 0.8356 -0.0745 1.3075 0.083 Uiso 1 1 calc R . .
C22B C 0.7939(10) 0.4169(8) 1.1351(7) 0.055(3) Uani 1 1 d . . .
H22A H 0.7653 0.3927 1.1950 0.066 Uiso 1 1 calc R . .
C23B C 0.7839(10) 0.5265(8) 1.0928(8) 0.060(3) Uani 1 1 d . . .
H23A H 0.7499 0.5740 1.1241 0.072 Uiso 1 1 calc R . .
C24B C 0.8248(11) 0.5608(8) 1.0060(8) 0.063(3) Uani 1 1 d . . .
H24A H 0.8170 0.6319 0.9761 0.076 Uiso 1 1 calc R . .
C25B C 0.8771(9) 0.4909(8) 0.9629(7) 0.051(3) Uani 1 1 d . . .
H25B H 0.9086 0.5137 0.9032 0.061 Uiso 1 1 calc R . .
C26B C 0.8829(9) 0.3854(8) 1.0089(7) 0.048(3) Uani 1 1 d . . .
H26A H 0.9180 0.3374 0.9786 0.057 Uiso 1 1 calc R . .
P1A P 1.0854(3) 0.3908(3) 0.7406(2) 0.0756(11) Uani 1 1 d D . .
F1A F 0.9942(11) 0.4270(10) 0.6896(10) 0.089(4) Uani 0.634(13) 1 d P A 1
F2A F 1.1534(12) 0.3267(10) 0.7976(10) 0.084(4) Uani 0.634(13) 1 d P A 1
F3A F 1.0190(9) 0.2669(7) 0.7637(7) 0.061(3) Uani 0.634(13) 1 d P A 1
F4A F 0.9991(9) 0.4022(10) 0.8233(8) 0.080(4) Uani 0.634(13) 1 d P A 1
F5A F 1.1302(14) 0.5008(10) 0.7151(10) 0.109(6) Uani 0.634(13) 1 d P A 1
F6A F 1.1606(17) 0.358(2) 0.6659(18) 0.154(15) Uani 0.634(13) 1 d P A 1
F1C F 1.053(3) 0.4900(18) 0.780(2) 0.115(10) Uiso 0.366(13) 1 d PD A 2
F2C F 1.157(2) 0.337(3) 0.671(2) 0.097(14) Uiso 0.366(13) 1 d PD A 2
F3C F 0.9652(13) 0.350(3) 0.761(3) 0.160(14) Uiso 0.366(13) 1 d PD A 2
F4C F 1.088(2) 0.4819(16) 0.6549(11) 0.099(8) Uiso 0.366(13) 1 d PD A 2
F5C F 1.1989(14) 0.454(2) 0.7281(18) 0.104(9) Uiso 0.366(13) 1 d PD A 2
F6C F 1.112(3) 0.342(2) 0.8284(12) 0.108(12) Uiso 0.366(13) 1 d PD A 2
P1B P 1.2220(2) 0.28542(18) 0.24987(19) 0.0387(5) Uani 1 1 d . . .
F1B F 1.3097(7) 0.3728(6) 0.1851(5) 0.096(3) Uani 1 1 d . . .
F2B F 1.1342(7) 0.1980(6) 0.3145(5) 0.084(2) Uani 1 1 d . . .
F3B F 1.1352(6) 0.3697(6) 0.2564(7) 0.097(3) Uani 1 1 d . . .
F4B F 1.1894(6) 0.2591(6) 0.1743(5) 0.078(2) Uani 1 1 d . . .
F5B F 1.3096(6) 0.2014(6) 0.2427(7) 0.094(3) Uani 1 1 d . . .
F6B F 1.2572(6) 0.3111(6) 0.3231(5) 0.078(2) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1A 0.0415(5) 0.0371(4) 0.0295(4) -0.0091(3) -0.0094(4) 0.0049(3)
N1A 0.080(7) 0.036(4) 0.051(6) -0.014(4) -0.020(5) 0.011(4)
N2A 0.060(5) 0.025(4) 0.037(5) -0.005(3) -0.019(4) 0.007(3)
N3A 0.043(5) 0.037(4) 0.038(5) -0.010(3) -0.011(4) -0.002(3)
N4A 0.046(5) 0.044(4) 0.049(6) -0.018(4) -0.014(4) 0.014(4)
C1A 0.064(7) 0.039(5) 0.038(6) -0.020(4) -0.009(5) 0.004(5)
C2A 0.092(9) 0.027(5) 0.073(9) -0.012(5) -0.036(7) 0.011(5)
C3A 0.065(7) 0.036(5) 0.052(7) -0.003(5) -0.015(6) 0.005(5)
C4A 0.049(6) 0.040(5) 0.043(6) -0.010(4) -0.021(5) 0.001(4)
C5A 0.044(6) 0.068(7) 0.035(6) 0.000(5) -0.010(5) -0.008(5)
C6A 0.055(7) 0.066(7) 0.030(6) -0.007(5) -0.006(5) 0.009(5)
C7A 0.069(8) 0.060(7) 0.037(6) -0.020(5) -0.004(6) 0.017(6)
C8A 0.070(8) 0.042(5) 0.049(7) -0.018(5) -0.026(6) 0.013(5)
C9A 0.052(6) 0.047(5) 0.031(6) -0.013(4) -0.017(5) 0.013(5)
C10A 0.040(6) 0.050(5) 0.030(5) -0.009(4) -0.008(4) -0.002(4)
C11A 0.101(10) 0.047(6) 0.055(8) -0.023(6) -0.028(7) 0.022(6)
C12A 0.044(6) 0.047(5) 0.039(6) -0.017(5) -0.013(5) -0.003(4)
C13A 0.027(5) 0.062(6) 0.027(5) -0.011(4) -0.007(4) 0.003(4)
C14A 0.047(6) 0.040(5) 0.043(6) -0.008(4) -0.020(5) 0.012(4)
C15A 0.035(5) 0.044(5) 0.021(5) -0.008(4) -0.003(4) 0.005(4)
C16A 0.041(6) 0.052(6) 0.036(6) -0.018(5) -0.011(5) 0.004(4)
C17A 0.048(7) 0.064(7) 0.080(9) -0.036(7) -0.018(6) -0.009(5)
C18A 0.051(7) 0.084(8) 0.035(6) -0.020(6) -0.008(5) -0.012(6)
C19A 0.041(6) 0.058(6) 0.047(7) 0.000(5) -0.012(5) -0.003(5)
C20A 0.064(7) 0.047(6) 0.061(8) -0.023(5) -0.026(6) 0.027(5)
C21A 0.045(6) 0.059(6) 0.046(7) -0.003(5) -0.016(5) 0.003(5)
C22A 0.053(7) 0.079(8) 0.039(7) -0.010(6) -0.009(6) 0.001(6)
C23A 0.055(8) 0.076(8) 0.060(9) -0.014(7) -0.010(7) 0.020(6)
C24A 0.053(7) 0.062(6) 0.043(7) -0.021(5) -0.008(6) 0.008(5)
C25A 0.047(6) 0.047(5) 0.035(6) -0.006(5) 0.000(5) -0.001(5)
C26A 0.042(6) 0.050(5) 0.036(6) 0.002(5) -0.003(5) 0.001(5)
Ru1B 0.0415(5) 0.0365(4) 0.0314(5) -0.0099(3) -0.0124(4) 0.0047(3)
N1B 0.035(5) 0.083(6) 0.038(5) -0.019(5) -0.019(4) 0.009(4)
N2B 0.035(5) 0.055(5) 0.038(5) -0.008(4) -0.009(4) 0.003(4)
N3B 0.042(5) 0.041(4) 0.033(5) -0.009(3) -0.014(4) 0.006(3)
N4B 0.053(5) 0.030(4) 0.038(5) -0.005(3) -0.010(4) 0.004(3)
C1B 0.027(5) 0.055(6) 0.045(6) -0.019(5) -0.012(5) 0.001(4)
C2B 0.026(5) 0.093(8) 0.067(8) -0.022(7) -0.020(6) -0.002(5)
C3B 0.027(5) 0.082(7) 0.035(6) -0.020(5) 0.001(5) -0.005(5)
C4B 0.046(6) 0.046(5) 0.024(5) -0.015(4) -0.004(4) 0.005(4)
C5B 0.049(7) 0.069(7) 0.050(7) -0.017(6) -0.004(6) -0.015(5)
C6B 0.090(10) 0.064(7) 0.035(7) -0.011(5) -0.012(7) 0.009(7)
C7B 0.055(7) 0.058(6) 0.038(6) -0.005(5) -0.018(5) 0.018(5)
C8B 0.046(6) 0.057(6) 0.041(6) -0.013(5) -0.024(5) 0.012(5)
C9B 0.043(6) 0.043(5) 0.026(5) -0.011(4) -0.007(4) 0.004(4)
C11B 0.060(8) 0.089(9) 0.048(7) -0.008(6) -0.025(6) 0.012(6)
C10B 0.041(5) 0.040(5) 0.033(5) -0.009(4) -0.008(4) 0.001(4)
C12B 0.060(7) 0.040(5) 0.049(7) -0.016(5) -0.027(6) -0.005(5)
C13B 0.070(7) 0.040(5) 0.031(6) -0.009(4) -0.015(5) 0.003(5)
C14B 0.048(6) 0.037(5) 0.035(6) -0.007(4) -0.007(5) -0.001(4)
C15B 0.054(6) 0.038(5) 0.039(6) -0.008(4) -0.019(5) 0.007(4)
C16B 0.049(6) 0.035(5) 0.032(5) 0.002(4) -0.013(5) -0.004(4)
C17B 0.068(8) 0.058(6) 0.054(7) -0.008(6) -0.029(6) -0.004(5)
C19B 0.055(7) 0.061(7) 0.072(9) -0.025(6) 0.011(7) 0.000(6)
C20B 0.053(7) 0.057(6) 0.073(9) -0.027(6) -0.028(6) 0.016(5)
C21B 0.073(8) 0.044(6) 0.044(7) -0.010(5) -0.012(6) 0.001(5)
C22B 0.074(8) 0.041(5) 0.044(7) -0.014(5) -0.009(6) 0.010(5)
C23B 0.076(8) 0.039(5) 0.063(8) -0.008(5) -0.024(7) 0.015(5)
C24B 0.101(10) 0.028(5) 0.051(8) 0.010(5) -0.027(7) -0.001(5)
C25B 0.061(7) 0.049(6) 0.041(6) -0.008(5) -0.017(6) 0.002(5)
C26B 0.067(7) 0.040(5) 0.037(6) -0.009(5) -0.016(5) 0.000(5)
P1A 0.081(3) 0.077(2) 0.048(2) -0.0029(16) -0.0042(18) 0.0362(19)
F1A 0.094(10) 0.079(8) 0.101(11) -0.026(8) -0.036(8) 0.009(7)
F2A 0.086(9) 0.087(9) 0.106(10) -0.044(8) -0.059(9) 0.061(8)
F3A 0.079(7) 0.046(5) 0.055(7) -0.008(5) -0.021(6) 0.003(5)
F4A 0.064(8) 0.096(9) 0.064(8) -0.027(7) 0.011(6) -0.002(6)
F5A 0.118(13) 0.074(8) 0.103(12) -0.025(8) 0.023(10) -0.043(8)
F6A 0.101(14) 0.16(2) 0.19(2) -0.14(2) 0.074(13) -0.063(12)
P1B 0.0399(14) 0.0394(12) 0.0378(14) -0.0125(11) -0.0117(12) 0.0060(10)
F1B 0.095(6) 0.094(5) 0.075(6) -0.007(4) 0.000(5) -0.042(5)
F2B 0.086(6) 0.085(5) 0.063(5) 0.010(4) -0.018(4) -0.034(4)
F3B 0.078(5) 0.089(5) 0.149(8) -0.061(5) -0.049(6) 0.048(4)
F4B 0.074(5) 0.118(6) 0.052(5) -0.027(4) -0.027(4) 0.001(4)
F5B 0.078(5) 0.073(4) 0.177(8) -0.069(5) -0.075(6) 0.036(4)
F6B 0.079(5) 0.108(5) 0.069(5) -0.046(4) -0.035(4) 0.000(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
Ru1A C1A 2.033(10) . ?
Ru1A N4A 2.156(8) . ?
Ru1A C15A 2.166(9) . ?
Ru1A C12A 2.176(9) . ?
Ru1A C16A 2.185(10) . ?
Ru1A N3A 2.195(7) . ?
Ru1A C14A 2.215(9) . ?
Ru1A C13A 2.224(9) . ?
N1A C1A 1.382(12) . ?
N1A C2A 1.392(14) . ?
N1A C11A 1.468(14) . ?
N2A C3A 1.395(12) . ?
N2A C1A 1.410(12) . ?
N2A C4A 1.432(12) . ?
N3A C10A 1.473(12) . ?
N4A C26A 1.338(13) . ?
N4A C22A 1.364(14) . ?
C2A C3A 1.310(16) . ?
C4A C5A 1.398(15) . ?
C4A C9A 1.404(13) . ?
C5A C6A 1.374(15) . ?
C6A C7A 1.366(16) . ?
C7A C8A 1.384(16) . ?
C8A C9A 1.392(14) . ?
C9A C10A 1.501(14) . ?
C12A C13A 1.423(14) . ?
C12A C16A 1.460(13) . ?
C12A C17A 1.507(13) . ?
C13A C14A 1.435(13) . ?
C13A C18A 1.508(13) . ?
C14A C15A 1.424(14) . ?
C14A C19A 1.512(14) . ?
C15A C16A 1.424(13) . ?
C15A C20A 1.521(13) . ?
C16A C21A 1.477(14) . ?
C22A C23A 1.360(16) . ?
C23A C24A 1.359(16) . ?
C24A C25A 1.342(15) . ?
C25A C26A 1.367(14) . ?
Ru1B C1B 2.067(10) . ?
Ru1B C16B 2.169(9) . ?
Ru1B N4B 2.169(7) . ?
Ru1B C15B 2.175(9) . ?
Ru1B N3B 2.183(7) . ?
Ru1B C12B 2.193(8) . ?
Ru1B C13B 2.210(10) . ?
Ru1B C14B 2.233(10) . ?
N1B C2B 1.346(14) . ?
N1B C1B 1.366(12) . ?
N1B C11B 1.459(14) . ?
N2B C1B 1.378(13) . ?
N2B C3B 1.386(12) . ?
N2B C4B 1.456(12) . ?
N3B C10B 1.497(12) . ?
N4B C22B 1.333(12) . ?
N4B C26B 1.344(13) . ?
C2B C3B 1.322(15) . ?
C4B C9B 1.362(13) . ?
C4B C5B 1.375(14) . ?
C5B C6B 1.413(17) . ?
C6B C7B 1.375(17) . ?
C7B C8B 1.392(15) . ?
C8B C9B 1.392(13) . ?
C9B C10B 1.518(13) . ?
C12B C13B 1.418(15) . ?
C12B C16B 1.460(13) . ?
C12B C17B 1.481(14) . ?
C13B C14B 1.415(15) . ?
C13B C18B 1.545(14) . ?
C14B C15B 1.456(14) . ?
C14B C19B 1.497(15) . ?
C15B C16B 1.409(14) . ?
C15B C20B 1.514(14) . ?
C16B C21B 1.483(14) . ?
C22B C23B 1.441(14) . ?
C23B C24B 1.376(17) . ?
C24B C25B 1.377(15) . ?
C25B C26B 1.404(14) . ?
P1A F5A 1.473(12) . ?
P1A F6A 1.532(15) . ?
P1A F2A 1.560(11) . ?
P1A F3C 1.573(10) . ?
P1A F4A 1.576(11) . ?
P1A F6C 1.596(10) . ?
P1A F2C 1.605(10) . ?
P1A F4C 1.610(10) . ?
P1A F1C 1.620(10) . ?
P1A F5C 1.646(10) . ?
P1A F1A 1.648(13) . ?
P1A F3A 1.755(10) . ?
P1B F3B 1.556(6) . ?
P1B F5B 1.561(6) . ?
P1B F6B 1.571(7) . ?
P1B F2B 1.581(7) . ?
P1B F1B 1.581(8) . ?
P1B F4B 1.595(7) . ?
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
C1A Ru1A N4A 90.9(4) . . ?
C1A Ru1A C15A 124.6(4) . . ?
N4A Ru1A C15A 144.4(3) . . ?
C1A Ru1A C12A 96.3(4) . . ?
N4A Ru1A C12A 119.7(3) . . ?
C15A Ru1A C12A 63.6(3) . . ?
C1A Ru1A C16A 93.0(4) . . ?
N4A Ru1A C16A 158.8(3) . . ?
C15A Ru1A C16A 38.2(3) . . ?
C12A Ru1A C16A 39.1(3) . . ?
C1A Ru1A N3A 91.9(3) . . ?
N4A Ru1A N3A 81.3(3) . . ?
C15A Ru1A N3A 94.2(3) . . ?
C12A Ru1A N3A 157.1(3) . . ?
C16A Ru1A N3A 119.3(3) . . ?
C1A Ru1A C14A 157.0(4) . . ?
N4A Ru1A C14A 108.5(4) . . ?
C15A Ru1A C14A 37.9(4) . . ?
C12A Ru1A C14A 63.6(4) . . ?
C16A Ru1A C14A 64.5(4) . . ?
N3A Ru1A C14A 102.9(3) . . ?
C1A Ru1A C13A 129.8(4) . . ?
N4A Ru1A C13A 97.5(3) . . ?
C15A Ru1A C13A 63.0(3) . . ?
C12A Ru1A C13A 37.7(4) . . ?
C16A Ru1A C13A 64.4(3) . . ?
N3A Ru1A C13A 138.3(3) . . ?
C14A Ru1A C13A 37.7(4) . . ?
C1A N1A C2A 113.4(9) . . ?
C1A N1A C11A 124.3(9) . . ?
C2A N1A C11A 122.3(8) . . ?
C3A N2A C1A 112.1(8) . . ?
C3A N2A C4A 121.6(9) . . ?
C1A N2A C4A 125.9(7) . . ?
C10A N3A Ru1A 120.3(5) . . ?
C26A N4A C22A 112.7(9) . . ?
C26A N4A Ru1A 123.6(7) . . ?
C22A N4A Ru1A 123.6(8) . . ?
N1A C1A N2A 99.9(8) . . ?
N1A C1A Ru1A 130.7(8) . . ?
N2A C1A Ru1A 128.9(6) . . ?
C3A C2A N1A 107.2(9) . . ?
C2A C3A N2A 107.4(10) . . ?
C5A C4A C9A 121.1(9) . . ?
C5A C4A N2A 118.8(8) . . ?
C9A C4A N2A 120.1(9) . . ?
C6A C5A C4A 120.7(10) . . ?
C7A C6A C5A 119.3(11) . . ?
C6A C7A C8A 120.3(10) . . ?
C7A C8A C9A 122.7(10) . . ?
C8A C9A C4A 115.9(10) . . ?
C8A C9A C10A 120.6(9) . . ?
C4A C9A C10A 123.4(9) . . ?
N3A C10A C9A 111.6(8) . . ?
C13A C12A C16A 109.0(8) . . ?
C13A C12A C17A 125.8(9) . . ?
C16A C12A C17A 124.2(9) . . ?
C13A C12A Ru1A 73.0(5) . . ?
C16A C12A Ru1A 70.8(5) . . ?
C17A C12A Ru1A 131.4(8) . . ?
C12A C13A C14A 108.1(8) . . ?
C12A C13A C18A 124.5(9) . . ?
C14A C13A C18A 127.2(9) . . ?
C12A C13A Ru1A 69.3(5) . . ?
C14A C13A Ru1A 70.8(5) . . ?
C18A C13A Ru1A 129.1(7) . . ?
C15A C14A C13A 106.8(8) . . ?
C15A C14A C19A 127.2(9) . . ?
C13A C14A C19A 125.5(10) . . ?
C15A C14A Ru1A 69.2(5) . . ?
C13A C14A Ru1A 71.5(5) . . ?
C19A C14A Ru1A 130.8(7) . . ?
C14A C15A C16A 111.0(8) . . ?
C14A C15A C20A 125.4(8) . . ?
C16A C15A C20A 123.5(9) . . ?
C14A C15A Ru1A 72.9(5) . . ?
C16A C15A Ru1A 71.6(5) . . ?
C20A C15A Ru1A 125.9(7) . . ?
C15A C16A C12A 105.0(8) . . ?
C15A C16A C21A 128.2(9) . . ?
C12A C16A C21A 126.1(9) . . ?
C15A C16A Ru1A 70.2(5) . . ?
C12A C16A Ru1A 70.1(5) . . ?
C21A C16A Ru1A 131.1(7) . . ?
C23A C22A N4A 123.0(11) . . ?
C24A C23A C22A 121.4(12) . . ?
C25A C24A C23A 117.4(11) . . ?
C24A C25A C26A 118.7(10) . . ?
N4A C26A C25A 126.6(10) . . ?
C1B Ru1B C16B 95.2(4) . . ?
C1B Ru1B N4B 89.5(4) . . ?
C16B Ru1B N4B 162.4(3) . . ?
C1B Ru1B C15B 128.4(4) . . ?
C16B Ru1B C15B 37.9(4) . . ?
N4B Ru1B C15B 141.9(4) . . ?
C1B Ru1B N3B 91.4(3) . . ?
C16B Ru1B N3B 115.2(3) . . ?
N4B Ru1B N3B 81.6(3) . . ?
C15B Ru1B N3B 93.3(3) . . ?
C1B Ru1B C12B 93.5(4) . . ?
C16B Ru1B C12B 39.1(4) . . ?
N4B Ru1B C12B 123.8(3) . . ?
C15B Ru1B C12B 64.1(4) . . ?
N3B Ru1B C12B 154.2(3) . . ?
C1B Ru1B C13B 124.8(4) . . ?
C16B Ru1B C13B 63.8(4) . . ?
N4B Ru1B C13B 99.6(3) . . ?
C15B Ru1B C13B 63.4(4) . . ?
N3B Ru1B C13B 143.7(4) . . ?
C12B Ru1B C13B 37.6(4) . . ?
C1B Ru1B C14B 156.1(4) . . ?
C16B Ru1B C14B 63.8(4) . . ?
N4B Ru1B C14B 107.2(3) . . ?
C15B Ru1B C14B 38.6(4) . . ?
N3B Ru1B C14B 107.5(3) . . ?
C12B Ru1B C14B 63.2(4) . . ?
C13B Ru1B C14B 37.1(4) . . ?
C2B N1B C1B 111.8(9) . . ?
C2B N1B C11B 123.5(9) . . ?
C1B N1B C11B 124.6(9) . . ?
C1B N2B C3B 111.6(8) . . ?
C1B N2B C4B 126.6(8) . . ?
C3B N2B C4B 121.7(9) . . ?
C10B N3B Ru1B 120.0(6) . . ?
C22B N4B C26B 117.3(8) . . ?
C22B N4B Ru1B 121.9(7) . . ?
C26B N4B Ru1B 120.8(6) . . ?
N1B C1B N2B 102.0(8) . . ?
N1B C1B Ru1B 129.1(8) . . ?
N2B C1B Ru1B 128.4(7) . . ?
C3B C2B N1B 109.0(9) . . ?
C2B C3B N2B 105.5(9) . . ?
C9B C4B C5B 122.7(10) . . ?
C9B C4B N2B 121.3(9) . . ?
C5B C4B N2B 115.9(9) . . ?
C4B C5B C6B 118.3(11) . . ?
C7B C6B C5B 119.5(11) . . ?
C6B C7B C8B 120.6(10) . . ?
C7B C8B C9B 119.8(10) . . ?
C4B C9B C8B 119.0(9) . . ?
C4B C9B C10B 122.6(9) . . ?
C8B C9B C10B 118.4(9) . . ?
N3B C10B C9B 112.4(7) . . ?
C13B C12B C16B 107.1(9) . . ?
C13B C12B C17B 127.7(10) . . ?
C16B C12B C17B 124.9(10) . . ?
C13B C12B Ru1B 71.9(5) . . ?
C16B C12B Ru1B 69.6(5) . . ?
C17B C12B Ru1B 128.2(8) . . ?
C14B C13B C12B 109.8(9) . . ?
C14B C13B C18B 127.6(10) . . ?
C12B C13B C18B 122.0(9) . . ?
C14B C13B Ru1B 72.3(6) . . ?
C12B C13B Ru1B 70.6(5) . . ?
C18B C13B Ru1B 130.5(7) . . ?
C13B C14B C15B 106.7(9) . . ?
C13B C14B C19B 126.0(10) . . ?
C15B C14B C19B 126.9(10) . . ?
C13B C14B Ru1B 70.5(6) . . ?
C15B C14B Ru1B 68.5(5) . . ?
C19B C14B Ru1B 131.6(7) . . ?
C16B C15B C14B 108.7(9) . . ?
C16B C15B C20B 126.5(10) . . ?
C14B C15B C20B 124.5(10) . . ?
C16B C15B Ru1B 70.8(5) . . ?
C14B C15B Ru1B 72.9(5) . . ?
C20B C15B Ru1B 127.4(7) . . ?
C15B C16B C12B 107.6(8) . . ?
C15B C16B C21B 125.2(9) . . ?
C12B C16B C21B 126.1(9) . . ?
C15B C16B Ru1B 71.3(5) . . ?
C12B C16B Ru1B 71.3(5) . . ?
C21B C16B Ru1B 132.1(7) . . ?
N4B C22B C23B 122.5(10) . . ?
C24B C23B C22B 118.4(10) . . ?
C23B C24B C25B 119.3(9) . . ?
C24B C25B C26B 118.6(10) . . ?
N4B C26B C25B 123.9(9) . . ?
F5A P1A F6A 96.5(11) . . ?
F5A P1A F2A 104.1(10) . . ?
F6A P1A F2A 88.4(14) . . ?
F5A P1A F3C 129.0(16) . . ?
F6A P1A F3C 112.5(17) . . ?
F2A P1A F3C 117.2(18) . . ?
F5A P1A F4A 94.5(7) . . ?
F6A P1A F4A 169.0(11) . . ?
F2A P1A F4A 88.6(8) . . ?
F3C P1A F4A 59.9(15) . . ?
F5A P1A F6C 102.2(15) . . ?
F6A P1A F6C 114.0(18) . . ?
F2A P1A F6C 25.7(11) . . ?
F3C P1A F6C 103(2) . . ?
F4A P1A F6C 63.0(13) . . ?
F5A P1A F2C 105.5(14) . . ?
F6A P1A F2C 9(2) . . ?
F2A P1A F2C 84.4(15) . . ?
F3C P1A F2C 107.0(17) . . ?
F4A P1A F2C 159.9(14) . . ?
F6C P1A F2C 109.5(19) . . ?
F5A P1A F4C 52.9(11) . . ?
F6A P1A F4C 72.0(16) . . ?
F2A P1A F4C 145.8(12) . . ?
F3C P1A F4C 96.5(19) . . ?
F4A P1A F4C 115.5(10) . . ?
F6C P1A F4C 155.0(15) . . ?
F2C P1A F4C 79.5(17) . . ?
F5A P1A F1C 47.3(12) . . ?
F6A P1A F1C 143.7(16) . . ?
F2A P1A F1C 101.6(12) . . ?
F3C P1A F1C 93.9(18) . . ?
F4A P1A F1C 47.3(12) . . ?
F6C P1A F1C 81.8(16) . . ?
F2C P1A F1C 152.8(17) . . ?
F4C P1A F1C 81.0(15) . . ?
F5A P1A F5C 41.0(10) . . ?
F6A P1A F5C 78.9(15) . . ?
F2A P1A F5C 66.9(12) . . ?
F3C P1A F5C 167.4(16) . . ?
F4A P1A F5C 109.6(11) . . ?
F6C P1A F5C 76.2(16) . . ?
F2C P1A F5C 85.0(6) . . ?
F4C P1A F5C 81.6(14) . . ?
F1C P1A F5C 73.5(14) . . ?
F5A P1A F1A 91.7(9) . . ?
F6A P1A F1A 91.9(14) . . ?
F2A P1A F1A 164.1(8) . . ?
F3C P1A F1A 48.5(15) . . ?
F4A P1A F1A 88.2(7) . . ?
F6C P1A F1A 148.6(14) . . ?
F2C P1A F1A 93.4(14) . . ?
F4C P1A F1A 48.0(10) . . ?
F1C P1A F1A 87.5(11) . . ?
F5C P1A F1A 128.6(12) . . ?
F5A P1A F3A 172.2(9) . . ?
F6A P1A F3A 84.2(9) . . ?
F2A P1A F3A 83.7(7) . . ?
F3C P1A F3A 44.5(14) . . ?
F4A P1A F3A 85.0(6) . . ?
F6C P1A F3A 84.5(12) . . ?
F2C P1A F3A 75.5(13) . . ?
F4C P1A F3A 120.5(11) . . ?
F1C P1A F3A 131.2(13) . . ?
F5C P1A F3A 146.2(10) . . ?
F1A P1A F3A 80.5(6) . . ?
F3B P1B F5B 179.6(7) . . ?
F3B P1B F6B 89.8(5) . . ?
F5B P1B F6B 90.3(5) . . ?
F3B P1B F2B 88.8(5) . . ?
F5B P1B F2B 91.5(5) . . ?
F6B P1B F2B 92.4(4) . . ?
F3B P1B F1B 91.1(5) . . ?
F5B P1B F1B 88.5(5) . . ?
F6B P1B F1B 87.7(4) . . ?
F2B P1B F1B 179.9(5) . . ?
F3B P1B F4B 91.3(5) . . ?
F5B P1B F4B 88.6(5) . . ?
F6B P1B F4B 178.5(4) . . ?
F2B P1B F4B 88.6(4) . . ?
F1B P1B F4B 91.3(5) . . ?
_diffrn_measured_fraction_theta_max 0.967
_diffrn_reflns_theta_full 25.24
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max 1.466
_refine_diff_density_min -1.040
_refine_diff_density_rms 0.163
_vrf_PLAT201_k1018twin
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 1
RESPONSE: One of the two independent PF6 anions is disordered
over two sites and the minor components of the F aroms are
refined isotropically
;
# end Validation Reply Form
_vrf_PLAT432_k1018twin
;
PROBLEM: Short Inter X...Y Contact C10A .. F3C .. 2.73 Ang.
RESPONSE: The minor component of disorder of an F atom.
;