# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2014
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# CCDC
#
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# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
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# fide research purposes only. It may contain copyright material
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data_2
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C48 H47 O2 P3 Ru'
_chemical_formula_sum 'C48 H47 O2 P3 Ru'
_chemical_formula_weight 849.84
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'
O O 0.0106 0.0060 '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 Monoclinic
_symmetry_space_group_name_H-M 'C 2/c'
_symmetry_space_group_name_Hall '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 22.1396(15)
_cell_length_b 11.6632(8)
_cell_length_c 33.324(2)
_cell_angle_alpha 90.00
_cell_angle_beta 104.066(2)
_cell_angle_gamma 90.00
_cell_volume 8346.9(9)
_cell_formula_units_Z 8
_cell_measurement_temperature 150(2)
_cell_measurement_reflns_used 9900
_cell_measurement_theta_min 2.47
_cell_measurement_theta_max 27.52
_exptl_crystal_description block
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.28
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.20
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.353
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3520
_exptl_absorpt_coefficient_mu 0.529
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.7122
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'Bruker Microsource'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker Kappa APEX-DUO CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 20144
_diffrn_reflns_av_R_equivalents 0.0543
_diffrn_reflns_av_sigmaI/netI 0.0405
_diffrn_reflns_limit_h_min -28
_diffrn_reflns_limit_h_max 27
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -43
_diffrn_reflns_limit_l_max 43
_diffrn_reflns_theta_min 1.90
_diffrn_reflns_theta_max 27.52
_reflns_number_total 9592
_reflns_number_gt 7782
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement APEX2
_computing_data_reduction 'SAINT (Bruker, 2007)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'PLATON (Spek, 2009)'
_computing_publication_material 'SHELXTL (Sheldrick, 2008)'
_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^)+(0.0297P)^2^+9.8399P] 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 9592
_refine_ls_number_parameters 492
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0474
_refine_ls_R_factor_gt 0.0350
_refine_ls_wR_factor_ref 0.0800
_refine_ls_wR_factor_gt 0.0758
_refine_ls_goodness_of_fit_ref 1.040
_refine_ls_restrained_S_all 1.040
_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 0.377142(8) 0.493822(15) 0.352487(5) 0.01924(5) Uani 1 1 d . . .
P1 P 0.35786(3) 0.44491(5) 0.414409(17) 0.02174(12) Uani 1 1 d . . .
P2 P 0.47820(3) 0.44900(5) 0.385264(17) 0.01996(12) Uani 1 1 d . . .
P3 P 0.39832(3) 0.69285(5) 0.363003(17) 0.02109(12) Uani 1 1 d . . .
O1 O 0.47002(7) 0.54012(13) 0.45904(4) 0.0219(3) Uani 1 1 d . . .
O2 O 0.43482(7) 0.73792(14) 0.33319(5) 0.0268(4) Uani 1 1 d . . .
C1 C 0.48688(9) 0.43584(18) 0.44142(6) 0.0199(4) Uani 1 1 d . . .
H1A H 0.5225 0.3899 0.4579 0.024 Uiso 1 1 calc R . .
C2 C 0.42936(9) 0.44280(18) 0.45608(6) 0.0191(4) Uani 1 1 d . . .
H2A H 0.4283 0.4015 0.4822 0.023 Uiso 1 1 calc R . .
C3 C 0.30227(11) 0.5149(2) 0.43936(8) 0.0327(6) Uani 1 1 d . . .
C4 C 0.23859(12) 0.5094(3) 0.42029(10) 0.0528(9) Uani 1 1 d . . .
H4A H 0.2249 0.4739 0.3940 0.063 Uiso 1 1 calc R . .
C5 C 0.19522(15) 0.5561(4) 0.43987(15) 0.0762(14) Uani 1 1 d . . .
H5A H 0.1521 0.5529 0.4267 0.091 Uiso 1 1 calc R . .
C6 C 0.21443(19) 0.6062(4) 0.47789(15) 0.0824(15) Uani 1 1 d . . .
H6A H 0.1846 0.6369 0.4912 0.099 Uiso 1 1 calc R . .
C7 C 0.27639(17) 0.6121(3) 0.49683(11) 0.0627(11) Uani 1 1 d . . .
H7A H 0.2895 0.6472 0.5232 0.075 Uiso 1 1 calc R . .
C8 C 0.32033(13) 0.5670(2) 0.47767(8) 0.0408(7) Uani 1 1 d . . .
H8A H 0.3633 0.5720 0.4911 0.049 Uiso 1 1 calc R . .
C9 C 0.33894(10) 0.2944(2) 0.42381(7) 0.0292(5) Uani 1 1 d . . .
C10 C 0.35378(13) 0.2082(2) 0.39956(8) 0.0386(6) Uani 1 1 d . . .
H10A H 0.3688 0.2275 0.3761 0.046 Uiso 1 1 calc R . .
C11 C 0.34703(14) 0.0925(2) 0.40898(9) 0.0479(8) Uani 1 1 d . . .
H11A H 0.3575 0.0338 0.3921 0.057 Uiso 1 1 calc R . .
C12 C 0.32504(13) 0.0648(3) 0.44298(9) 0.0477(8) Uani 1 1 d . . .
H12A H 0.3198 -0.0134 0.4494 0.057 Uiso 1 1 calc R . .
C13 C 0.31062(12) 0.1493(3) 0.46769(9) 0.0411(7) Uani 1 1 d . . .
H13A H 0.2962 0.1292 0.4914 0.049 Uiso 1 1 calc R . .
C14 C 0.31692(11) 0.2638(2) 0.45847(8) 0.0344(6) Uani 1 1 d . . .
H14A H 0.3063 0.3217 0.4756 0.041 Uiso 1 1 calc R . .
C15 C 0.50919(11) 0.3091(2) 0.37541(7) 0.0306(5) Uani 1 1 d . . .
C16 C 0.54268(14) 0.2958(3) 0.34515(8) 0.0490(8) Uani 1 1 d . . .
H16A H 0.5522 0.3610 0.3307 0.059 Uiso 1 1 calc R . .
C17 C 0.5620(2) 0.1882(3) 0.33607(11) 0.0761(13) Uani 1 1 d . . .
H17A H 0.5846 0.1802 0.3154 0.091 Uiso 1 1 calc R . .
C18 C 0.5490(2) 0.0934(3) 0.35640(12) 0.0860(15) Uani 1 1 d . . .
H18A H 0.5618 0.0198 0.3494 0.103 Uiso 1 1 calc R . .
C19 C 0.51728(18) 0.1045(3) 0.38724(10) 0.0644(10) Uani 1 1 d . . .
H19A H 0.5088 0.0388 0.4018 0.077 Uiso 1 1 calc R . .
C20 C 0.49788(14) 0.2119(2) 0.39675(8) 0.0405(6) Uani 1 1 d . . .
H20A H 0.4765 0.2193 0.4181 0.049 Uiso 1 1 calc R . .
C21 C 0.54684(10) 0.5364(2) 0.38462(7) 0.0277(5) Uani 1 1 d . . .
C22 C 0.55067(11) 0.5981(2) 0.34998(8) 0.0334(6) Uani 1 1 d . . .
H22A H 0.5168 0.5977 0.3262 0.040 Uiso 1 1 calc R . .
C23 C 0.60427(13) 0.6611(3) 0.34996(10) 0.0460(7) Uani 1 1 d . . .
H23A H 0.6069 0.7030 0.3260 0.055 Uiso 1 1 calc R . .
C24 C 0.65307(14) 0.6629(3) 0.38428(11) 0.0611(10) Uani 1 1 d . . .
H24A H 0.6894 0.7062 0.3841 0.073 Uiso 1 1 calc R . .
C25 C 0.64947(14) 0.6026(4) 0.41861(11) 0.0739(12) Uani 1 1 d . . .
H25A H 0.6833 0.6041 0.4424 0.089 Uiso 1 1 calc R . .
C26 C 0.59690(12) 0.5395(3) 0.41899(10) 0.0547(9) Uani 1 1 d . . .
H26A H 0.5950 0.4976 0.4431 0.066 Uiso 1 1 calc R . .
C27 C 0.43903(10) 0.75361(18) 0.41362(7) 0.0230(5) Uani 1 1 d . . .
C28 C 0.50083(11) 0.7865(2) 0.41819(7) 0.0281(5) Uani 1 1 d . . .
H28A H 0.5198 0.7771 0.3957 0.034 Uiso 1 1 calc R . .
C29 C 0.53506(12) 0.8326(2) 0.45510(8) 0.0367(6) Uani 1 1 d . . .
H29A H 0.5774 0.8532 0.4577 0.044 Uiso 1 1 calc R . .
C30 C 0.50853(13) 0.8487(2) 0.48785(8) 0.0381(6) Uani 1 1 d . . .
H30A H 0.5323 0.8796 0.5132 0.046 Uiso 1 1 calc R . .
C31 C 0.44672(13) 0.8195(2) 0.48355(8) 0.0363(6) Uani 1 1 d . . .
H31A H 0.4278 0.8317 0.5059 0.044 Uiso 1 1 calc R . .
C32 C 0.41215(11) 0.7727(2) 0.44689(7) 0.0305(5) Uani 1 1 d . . .
H32A H 0.3697 0.7533 0.4444 0.037 Uiso 1 1 calc R . .
C33 C 0.32630(11) 0.7799(2) 0.35374(7) 0.0284(5) Uani 1 1 d . . .
C34 C 0.31948(12) 0.8681(2) 0.32463(7) 0.0332(6) Uani 1 1 d . . .
H34A H 0.3517 0.8826 0.3110 0.040 Uiso 1 1 calc R . .
C35 C 0.26602(14) 0.9346(2) 0.31555(9) 0.0450(7) Uani 1 1 d . . .
H35A H 0.2613 0.9926 0.2950 0.054 Uiso 1 1 calc R . .
C36 C 0.21985(14) 0.9176(3) 0.33588(9) 0.0540(8) Uani 1 1 d . . .
H36A H 0.1837 0.9645 0.3297 0.065 Uiso 1 1 calc R . .
C37 C 0.22600(13) 0.8314(3) 0.36554(9) 0.0510(8) Uani 1 1 d . . .
H37A H 0.1944 0.8199 0.3800 0.061 Uiso 1 1 calc R . .
C38 C 0.27871(11) 0.7624(2) 0.37378(8) 0.0375(6) Uani 1 1 d . . .
H38A H 0.2824 0.7022 0.3934 0.045 Uiso 1 1 calc R . .
C39 C 0.28645(11) 0.5070(2) 0.30299(7) 0.0316(6) Uani 1 1 d . . .
C40 C 0.29703(12) 0.3879(2) 0.31303(7) 0.0338(6) Uani 1 1 d . . .
C41 C 0.35262(12) 0.3524(2) 0.30278(7) 0.0325(6) Uani 1 1 d . . .
C42 C 0.37727(12) 0.4511(2) 0.28596(7) 0.0290(5) Uani 1 1 d . . .
C43 C 0.33546(11) 0.5429(2) 0.28485(7) 0.0291(5) Uani 1 1 d . . .
C44 C 0.22652(11) 0.5691(3) 0.30089(9) 0.0449(7) Uani 1 1 d . . .
H44A H 0.1944 0.5401 0.2775 0.067 Uiso 1 1 calc R . .
H44B H 0.2325 0.6514 0.2972 0.067 Uiso 1 1 calc R . .
H44C H 0.2134 0.5566 0.3266 0.067 Uiso 1 1 calc R . .
C45 C 0.24861(13) 0.3124(3) 0.32447(8) 0.0489(8) Uani 1 1 d . . .
H45A H 0.2104 0.3142 0.3022 0.073 Uiso 1 1 calc R . .
H45B H 0.2397 0.3403 0.3502 0.073 Uiso 1 1 calc R . .
H45C H 0.2642 0.2335 0.3284 0.073 Uiso 1 1 calc R . .
C46 C 0.37451(15) 0.2321(2) 0.29903(8) 0.0440(7) Uani 1 1 d . . .
H46A H 0.3686 0.2126 0.2697 0.066 Uiso 1 1 calc R . .
H46B H 0.3505 0.1791 0.3119 0.066 Uiso 1 1 calc R . .
H46C H 0.4188 0.2261 0.3130 0.066 Uiso 1 1 calc R . .
C47 C 0.42900(14) 0.4486(3) 0.26425(8) 0.0415(7) Uani 1 1 d . . .
H47A H 0.4124 0.4264 0.2353 0.062 Uiso 1 1 calc R . .
H47B H 0.4605 0.3928 0.2778 0.062 Uiso 1 1 calc R . .
H47C H 0.4480 0.5248 0.2654 0.062 Uiso 1 1 calc R . .
C48 C 0.33603(13) 0.6506(2) 0.26041(7) 0.0358(6) Uani 1 1 d . . .
H48A H 0.3270 0.6319 0.2309 0.054 Uiso 1 1 calc R . .
H48B H 0.3771 0.6867 0.2689 0.054 Uiso 1 1 calc R . .
H48C H 0.3043 0.7035 0.2655 0.054 Uiso 1 1 calc R . .
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 0.01782(9) 0.02386(10) 0.01335(8) 0.00161(7) -0.00140(6) -0.00525(7)
P1 0.0155(3) 0.0312(3) 0.0164(3) 0.0050(2) -0.0003(2) -0.0035(2)
P2 0.0185(3) 0.0233(3) 0.0174(3) 0.0022(2) 0.0030(2) 0.0001(2)
P3 0.0190(3) 0.0235(3) 0.0178(3) 0.0027(2) -0.0012(2) -0.0005(2)
O1 0.0219(8) 0.0211(8) 0.0199(8) -0.0014(6) -0.0005(6) -0.0027(6)
O2 0.0274(8) 0.0287(9) 0.0223(8) 0.0046(7) 0.0021(7) -0.0042(7)
C1 0.0170(10) 0.0219(11) 0.0183(10) 0.0022(8) -0.0004(8) 0.0007(8)
C2 0.0188(10) 0.0215(11) 0.0153(10) 0.0016(8) 0.0009(8) -0.0013(8)
C3 0.0224(11) 0.0453(15) 0.0326(13) 0.0204(12) 0.0108(10) 0.0090(11)
C4 0.0235(13) 0.073(2) 0.061(2) 0.0384(17) 0.0099(13) 0.0080(14)
C5 0.0298(16) 0.092(3) 0.116(3) 0.075(3) 0.035(2) 0.0277(17)
C6 0.078(3) 0.090(3) 0.105(3) 0.070(3) 0.071(3) 0.058(2)
C7 0.085(3) 0.059(2) 0.061(2) 0.0318(17) 0.051(2) 0.0428(19)
C8 0.0463(16) 0.0486(17) 0.0332(14) 0.0186(13) 0.0205(12) 0.0238(13)
C9 0.0206(11) 0.0396(14) 0.0219(12) 0.0077(10) -0.0056(9) -0.0112(10)
C10 0.0459(16) 0.0410(15) 0.0234(13) 0.0040(11) -0.0025(11) -0.0157(13)
C11 0.0611(19) 0.0364(15) 0.0363(16) 0.0013(12) -0.0071(14) -0.0166(14)
C12 0.0407(16) 0.0445(17) 0.0474(17) 0.0201(14) -0.0096(13) -0.0205(13)
C13 0.0265(13) 0.0529(18) 0.0398(15) 0.0207(14) 0.0004(11) -0.0123(12)
C14 0.0213(12) 0.0468(16) 0.0323(14) 0.0132(12) 0.0011(10) -0.0094(11)
C15 0.0344(13) 0.0324(13) 0.0232(12) 0.0007(10) 0.0033(10) 0.0105(11)
C16 0.0607(19) 0.0563(19) 0.0314(15) 0.0022(13) 0.0140(14) 0.0255(15)
C17 0.107(3) 0.078(3) 0.0444(19) -0.0032(18) 0.020(2) 0.059(2)
C18 0.138(4) 0.058(2) 0.051(2) -0.0086(18) 0.000(2) 0.061(2)
C19 0.099(3) 0.0336(17) 0.0471(19) 0.0036(14) -0.0079(19) 0.0210(17)
C20 0.0566(18) 0.0295(14) 0.0294(14) 0.0020(11) -0.0011(12) 0.0077(12)
C21 0.0196(11) 0.0318(13) 0.0330(13) 0.0068(10) 0.0091(10) -0.0001(9)
C22 0.0269(13) 0.0384(14) 0.0371(14) 0.0060(11) 0.0120(11) 0.0011(11)
C23 0.0385(16) 0.0499(18) 0.0575(19) 0.0185(15) 0.0271(14) 0.0014(13)
C24 0.0284(15) 0.078(2) 0.079(2) 0.018(2) 0.0169(16) -0.0167(15)
C25 0.0277(16) 0.118(3) 0.068(2) 0.031(2) -0.0031(15) -0.0258(18)
C26 0.0222(13) 0.089(2) 0.0473(18) 0.0288(17) -0.0023(12) -0.0136(14)
C27 0.0281(12) 0.0159(10) 0.0207(11) 0.0037(9) -0.0024(9) 0.0022(9)
C28 0.0291(12) 0.0258(12) 0.0261(12) 0.0033(10) 0.0000(10) -0.0046(10)
C29 0.0381(14) 0.0304(14) 0.0327(14) 0.0010(11) -0.0087(11) -0.0133(11)
C30 0.0517(17) 0.0261(13) 0.0261(13) -0.0024(10) -0.0109(12) -0.0008(12)
C31 0.0460(16) 0.0353(14) 0.0241(13) -0.0001(11) 0.0015(11) 0.0145(12)
C32 0.0287(12) 0.0320(13) 0.0278(13) 0.0020(10) 0.0011(10) 0.0087(10)
C33 0.0253(12) 0.0307(13) 0.0243(12) -0.0010(10) -0.0034(9) 0.0045(10)
C34 0.0378(14) 0.0319(13) 0.0253(12) 0.0005(10) -0.0014(10) 0.0068(11)
C35 0.0521(18) 0.0363(16) 0.0374(15) 0.0050(12) -0.0071(13) 0.0161(13)
C36 0.0428(17) 0.063(2) 0.0471(18) 0.0030(15) -0.0059(14) 0.0311(15)
C37 0.0293(14) 0.074(2) 0.0469(18) 0.0035(16) 0.0042(13) 0.0196(14)
C38 0.0278(13) 0.0437(16) 0.0366(15) 0.0095(12) -0.0006(11) 0.0080(11)
C39 0.0267(12) 0.0436(15) 0.0171(11) 0.0048(10) -0.0088(9) -0.0101(11)
C40 0.0361(14) 0.0422(15) 0.0152(11) 0.0028(10) -0.0088(10) -0.0209(12)
C41 0.0468(15) 0.0305(13) 0.0135(11) -0.0023(9) -0.0053(10) -0.0135(11)
C42 0.0380(14) 0.0324(13) 0.0136(10) -0.0016(9) 0.0008(9) -0.0096(11)
C43 0.0342(13) 0.0349(13) 0.0123(10) 0.0014(9) -0.0056(9) -0.0129(11)
C44 0.0246(13) 0.064(2) 0.0365(15) 0.0133(14) -0.0107(11) -0.0061(13)
C45 0.0457(16) 0.0590(19) 0.0314(15) 0.0073(13) -0.0111(12) -0.0336(15)
C46 0.071(2) 0.0329(14) 0.0229(13) -0.0060(11) 0.0009(13) -0.0094(14)
C47 0.0569(18) 0.0479(17) 0.0214(13) -0.0010(12) 0.0127(12) -0.0042(14)
C48 0.0467(15) 0.0396(15) 0.0159(11) 0.0067(10) -0.0026(10) -0.0105(12)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 C42 2.273(2) . ?
Ru1 C39 2.273(2) . ?
Ru1 P1 2.2790(6) . ?
Ru1 C43 2.291(2) . ?
Ru1 C40 2.295(2) . ?
Ru1 P2 2.2987(6) . ?
Ru1 C41 2.307(2) . ?
Ru1 P3 2.3772(6) . ?
P1 C2 1.835(2) . ?
P1 C3 1.836(2) . ?
P1 C9 1.849(2) . ?
P2 C15 1.830(2) . ?
P2 C21 1.834(2) . ?
P2 C1 1.840(2) . ?
P3 O2 1.5186(16) . ?
P3 C27 1.850(2) . ?
P3 C33 1.852(2) . ?
O1 C2 1.437(3) . ?
O1 C1 1.439(3) . ?
C1 C2 1.473(3) . ?
C1 H1A 1.0000 . ?
C2 H2A 1.0000 . ?
C3 C8 1.382(4) . ?
C3 C4 1.400(4) . ?
C4 C5 1.396(5) . ?
C4 H4A 0.9500 . ?
C5 C6 1.366(6) . ?
C5 H5A 0.9500 . ?
C6 C7 1.365(6) . ?
C6 H6A 0.9500 . ?
C7 C8 1.390(4) . ?
C7 H7A 0.9500 . ?
C8 H8A 0.9500 . ?
C9 C10 1.379(4) . ?
C9 C14 1.405(3) . ?
C10 C11 1.402(4) . ?
C10 H10A 0.9500 . ?
C11 C12 1.376(4) . ?
C11 H11A 0.9500 . ?
C12 C13 1.371(4) . ?
C12 H12A 0.9500 . ?
C13 C14 1.384(4) . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?
C15 C20 1.394(4) . ?
C15 C16 1.398(4) . ?
C16 C17 1.383(4) . ?
C16 H16A 0.9500 . ?
C17 C18 1.363(6) . ?
C17 H17A 0.9500 . ?
C18 C19 1.385(5) . ?
C18 H18A 0.9500 . ?
C19 C20 1.385(4) . ?
C19 H19A 0.9500 . ?
C20 H20A 0.9500 . ?
C21 C22 1.381(3) . ?
C21 C26 1.387(4) . ?
C22 C23 1.396(4) . ?
C22 H22A 0.9500 . ?
C23 C24 1.369(4) . ?
C23 H23A 0.9500 . ?
C24 C25 1.362(5) . ?
C24 H24A 0.9500 . ?
C25 C26 1.380(4) . ?
C25 H25A 0.9500 . ?
C26 H26A 0.9500 . ?
C27 C28 1.393(3) . ?
C27 C32 1.398(3) . ?
C28 C29 1.387(3) . ?
C28 H28A 0.9500 . ?
C29 C30 1.372(4) . ?
C29 H29A 0.9500 . ?
C30 C31 1.383(4) . ?
C30 H30A 0.9500 . ?
C31 C32 1.387(3) . ?
C31 H31A 0.9500 . ?
C32 H32A 0.9500 . ?
C33 C38 1.393(3) . ?
C33 C34 1.397(3) . ?
C34 C35 1.386(4) . ?
C34 H34A 0.9500 . ?
C35 C36 1.371(4) . ?
C35 H35A 0.9500 . ?
C36 C37 1.393(4) . ?
C36 H36A 0.9500 . ?
C37 C38 1.389(4) . ?
C37 H37A 0.9500 . ?
C38 H38A 0.9500 . ?
C39 C43 1.427(3) . ?
C39 C40 1.434(4) . ?
C39 C44 1.499(4) . ?
C40 C41 1.417(4) . ?
C40 C45 1.506(3) . ?
C41 C42 1.445(3) . ?
C41 C46 1.499(4) . ?
C42 C43 1.410(4) . ?
C42 C47 1.496(4) . ?
C43 C48 1.498(3) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
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
C42 Ru1 C39 61.13(9) . . ?
C42 Ru1 P1 150.83(6) . . ?
C39 Ru1 P1 110.31(6) . . ?
C42 Ru1 C43 35.99(9) . . ?
C39 Ru1 C43 36.45(8) . . ?
P1 Ru1 C43 146.52(6) . . ?
C42 Ru1 C40 60.48(9) . . ?
C39 Ru1 C40 36.59(9) . . ?
P1 Ru1 C40 95.47(6) . . ?
C43 Ru1 C40 60.03(8) . . ?
C42 Ru1 P2 100.48(7) . . ?
C39 Ru1 P2 161.14(7) . . ?
P1 Ru1 P2 83.55(2) . . ?
C43 Ru1 P2 129.58(7) . . ?
C40 Ru1 P2 132.63(7) . . ?
C42 Ru1 C41 36.76(8) . . ?
C39 Ru1 C41 60.99(10) . . ?
P1 Ru1 C41 114.08(6) . . ?
C43 Ru1 C41 60.27(9) . . ?
C40 Ru1 C41 35.86(9) . . ?
P2 Ru1 C41 102.16(7) . . ?
C42 Ru1 P3 108.11(6) . . ?
C39 Ru1 P3 98.56(7) . . ?
P1 Ru1 P3 100.64(2) . . ?
C43 Ru1 P3 85.34(6) . . ?
C40 Ru1 P3 135.01(7) . . ?
P2 Ru1 P3 91.01(2) . . ?
C41 Ru1 P3 143.86(6) . . ?
C2 P1 C3 102.31(11) . . ?
C2 P1 C9 92.77(10) . . ?
C3 P1 C9 98.12(11) . . ?
C2 P1 Ru1 111.82(7) . . ?
C3 P1 Ru1 126.33(8) . . ?
C9 P1 Ru1 119.41(8) . . ?
C15 P2 C21 98.35(11) . . ?
C15 P2 C1 99.04(10) . . ?
C21 P2 C1 100.14(10) . . ?
C15 P2 Ru1 118.78(8) . . ?
C21 P2 Ru1 125.56(8) . . ?
C1 P2 Ru1 110.56(7) . . ?
O2 P3 C27 104.19(10) . . ?
O2 P3 C33 105.95(10) . . ?
C27 P3 C33 98.69(10) . . ?
O2 P3 Ru1 111.03(7) . . ?
C27 P3 Ru1 122.92(7) . . ?
C33 P3 Ru1 112.31(8) . . ?
C2 O1 C1 61.61(13) . . ?
O1 C1 C2 59.14(13) . . ?
O1 C1 P2 111.79(14) . . ?
C2 C1 P2 116.59(15) . . ?
O1 C1 H1A 118.5 . . ?
C2 C1 H1A 118.5 . . ?
P2 C1 H1A 118.5 . . ?
O1 C2 C1 59.25(13) . . ?
O1 C2 P1 116.89(14) . . ?
C1 C2 P1 113.96(15) . . ?
O1 C2 H2A 117.8 . . ?
C1 C2 H2A 117.8 . . ?
P1 C2 H2A 117.8 . . ?
C8 C3 C4 118.2(3) . . ?
C8 C3 P1 122.59(19) . . ?
C4 C3 P1 119.1(2) . . ?
C5 C4 C3 120.1(4) . . ?
C5 C4 H4A 120.0 . . ?
C3 C4 H4A 120.0 . . ?
C6 C5 C4 120.4(3) . . ?
C6 C5 H5A 119.8 . . ?
C4 C5 H5A 119.8 . . ?
C7 C6 C5 120.1(3) . . ?
C7 C6 H6A 119.9 . . ?
C5 C6 H6A 119.9 . . ?
C6 C7 C8 120.3(4) . . ?
C6 C7 H7A 119.8 . . ?
C8 C7 H7A 119.8 . . ?
C3 C8 C7 120.9(3) . . ?
C3 C8 H8A 119.6 . . ?
C7 C8 H8A 119.6 . . ?
C10 C9 C14 118.4(2) . . ?
C10 C9 P1 119.81(18) . . ?
C14 C9 P1 121.3(2) . . ?
C9 C10 C11 121.2(3) . . ?
C9 C10 H10A 119.4 . . ?
C11 C10 H10A 119.4 . . ?
C12 C11 C10 119.3(3) . . ?
C12 C11 H11A 120.4 . . ?
C10 C11 H11A 120.4 . . ?
C13 C12 C11 120.4(3) . . ?
C13 C12 H12A 119.8 . . ?
C11 C12 H12A 119.8 . . ?
C12 C13 C14 120.6(3) . . ?
C12 C13 H13A 119.7 . . ?
C14 C13 H13A 119.7 . . ?
C13 C14 C9 120.1(3) . . ?
C13 C14 H14A 119.9 . . ?
C9 C14 H14A 119.9 . . ?
C20 C15 C16 118.1(2) . . ?
C20 C15 P2 120.80(19) . . ?
C16 C15 P2 121.1(2) . . ?
C17 C16 C15 120.3(3) . . ?
C17 C16 H16A 119.8 . . ?
C15 C16 H16A 119.8 . . ?
C18 C17 C16 120.9(3) . . ?
C18 C17 H17A 119.5 . . ?
C16 C17 H17A 119.5 . . ?
C17 C18 C19 119.9(3) . . ?
C17 C18 H18A 120.0 . . ?
C19 C18 H18A 120.0 . . ?
C20 C19 C18 119.7(3) . . ?
C20 C19 H19A 120.1 . . ?
C18 C19 H19A 120.1 . . ?
C19 C20 C15 121.0(3) . . ?
C19 C20 H20A 119.5 . . ?
C15 C20 H20A 119.5 . . ?
C22 C21 C26 118.5(2) . . ?
C22 C21 P2 121.27(19) . . ?
C26 C21 P2 120.19(19) . . ?
C21 C22 C23 120.0(2) . . ?
C21 C22 H22A 120.0 . . ?
C23 C22 H22A 120.0 . . ?
C24 C23 C22 120.4(3) . . ?
C24 C23 H23A 119.8 . . ?
C22 C23 H23A 119.8 . . ?
C25 C24 C23 119.9(3) . . ?
C25 C24 H24A 120.1 . . ?
C23 C24 H24A 120.1 . . ?
C24 C25 C26 120.3(3) . . ?
C24 C25 H25A 119.8 . . ?
C26 C25 H25A 119.8 . . ?
C25 C26 C21 120.8(3) . . ?
C25 C26 H26A 119.6 . . ?
C21 C26 H26A 119.6 . . ?
C28 C27 C32 117.8(2) . . ?
C28 C27 P3 116.93(17) . . ?
C32 C27 P3 125.26(18) . . ?
C29 C28 C27 120.9(2) . . ?
C29 C28 H28A 119.5 . . ?
C27 C28 H28A 119.5 . . ?
C30 C29 C28 120.7(2) . . ?
C30 C29 H29A 119.6 . . ?
C28 C29 H29A 119.6 . . ?
C29 C30 C31 119.2(2) . . ?
C29 C30 H30A 120.4 . . ?
C31 C30 H30A 120.4 . . ?
C30 C31 C32 120.6(2) . . ?
C30 C31 H31A 119.7 . . ?
C32 C31 H31A 119.7 . . ?
C31 C32 C27 120.8(2) . . ?
C31 C32 H32A 119.6 . . ?
C27 C32 H32A 119.6 . . ?
C38 C33 C34 118.3(2) . . ?
C38 C33 P3 124.13(19) . . ?
C34 C33 P3 117.58(19) . . ?
C35 C34 C33 120.4(3) . . ?
C35 C34 H34A 119.8 . . ?
C33 C34 H34A 119.8 . . ?
C36 C35 C34 120.7(3) . . ?
C36 C35 H35A 119.6 . . ?
C34 C35 H35A 119.6 . . ?
C35 C36 C37 119.9(3) . . ?
C35 C36 H36A 120.0 . . ?
C37 C36 H36A 120.0 . . ?
C38 C37 C36 119.4(3) . . ?
C38 C37 H37A 120.3 . . ?
C36 C37 H37A 120.3 . . ?
C37 C38 C33 121.2(3) . . ?
C37 C38 H38A 119.4 . . ?
C33 C38 H38A 119.4 . . ?
C43 C39 C40 106.6(2) . . ?
C43 C39 C44 126.4(2) . . ?
C40 C39 C44 124.9(2) . . ?
C43 C39 Ru1 72.47(13) . . ?
C40 C39 Ru1 72.54(13) . . ?
C44 C39 Ru1 133.04(18) . . ?
C41 C40 C39 109.2(2) . . ?
C41 C40 C45 127.1(3) . . ?
C39 C40 C45 122.6(3) . . ?
C41 C40 Ru1 72.54(13) . . ?
C39 C40 Ru1 70.87(12) . . ?
C45 C40 Ru1 131.93(17) . . ?
C40 C41 C42 107.0(2) . . ?
C40 C41 C46 127.7(2) . . ?
C42 C41 C46 123.6(2) . . ?
C40 C41 Ru1 71.60(13) . . ?
C42 C41 Ru1 70.33(13) . . ?
C46 C41 Ru1 134.79(17) . . ?
C43 C42 C41 107.9(2) . . ?
C43 C42 C47 125.3(2) . . ?
C41 C42 C47 125.3(2) . . ?
C43 C42 Ru1 72.71(13) . . ?
C41 C42 Ru1 72.91(13) . . ?
C47 C42 Ru1 131.18(17) . . ?
C42 C43 C39 109.1(2) . . ?
C42 C43 C48 123.9(2) . . ?
C39 C43 C48 125.7(2) . . ?
C42 C43 Ru1 71.30(13) . . ?
C39 C43 Ru1 71.09(12) . . ?
C48 C43 Ru1 133.60(16) . . ?
C39 C44 H44A 109.5 . . ?
C39 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C39 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C40 C45 H45A 109.5 . . ?
C40 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C40 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C41 C46 H46A 109.5 . . ?
C41 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C41 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C42 C47 H47A 109.5 . . ?
C42 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C42 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C43 C48 H48A 109.5 . . ?
C43 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C43 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
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
C42 Ru1 P1 C2 117.00(15) . . . . ?
C39 Ru1 P1 C2 -176.15(10) . . . . ?
C43 Ru1 P1 C2 -170.50(13) . . . . ?
C40 Ru1 P1 C2 149.41(10) . . . . ?
P2 Ru1 P1 C2 17.04(8) . . . . ?
C41 Ru1 P1 C2 117.50(11) . . . . ?
P3 Ru1 P1 C2 -72.79(8) . . . . ?
C42 Ru1 P1 C3 -117.59(17) . . . . ?
C39 Ru1 P1 C3 -50.73(13) . . . . ?
C43 Ru1 P1 C3 -45.09(16) . . . . ?
C40 Ru1 P1 C3 -85.18(13) . . . . ?
P2 Ru1 P1 C3 142.45(11) . . . . ?
C41 Ru1 P1 C3 -117.09(13) . . . . ?
P3 Ru1 P1 C3 52.63(11) . . . . ?
C42 Ru1 P1 C9 10.41(16) . . . . ?
C39 Ru1 P1 C9 77.27(11) . . . . ?
C43 Ru1 P1 C9 82.91(14) . . . . ?
C40 Ru1 P1 C9 42.82(11) . . . . ?
P2 Ru1 P1 C9 -89.55(9) . . . . ?
C41 Ru1 P1 C9 10.91(11) . . . . ?
P3 Ru1 P1 C9 -179.37(8) . . . . ?
C42 Ru1 P2 C15 -50.57(11) . . . . ?
C39 Ru1 P2 C15 -38.4(2) . . . . ?
P1 Ru1 P2 C15 100.21(9) . . . . ?
C43 Ru1 P2 C15 -74.40(12) . . . . ?
C40 Ru1 P2 C15 8.70(13) . . . . ?
C41 Ru1 P2 C15 -13.09(11) . . . . ?
P3 Ru1 P2 C15 -159.20(9) . . . . ?
C42 Ru1 P2 C21 76.05(12) . . . . ?
C39 Ru1 P2 C21 88.3(2) . . . . ?
P1 Ru1 P2 C21 -133.16(10) . . . . ?
C43 Ru1 P2 C21 52.22(13) . . . . ?
C40 Ru1 P2 C21 135.33(13) . . . . ?
C41 Ru1 P2 C21 113.53(12) . . . . ?
P3 Ru1 P2 C21 -32.57(10) . . . . ?
C42 Ru1 P2 C1 -163.99(10) . . . . ?
C39 Ru1 P2 C1 -151.8(2) . . . . ?
P1 Ru1 P2 C1 -13.21(8) . . . . ?
C43 Ru1 P2 C1 172.18(11) . . . . ?
C40 Ru1 P2 C1 -104.72(11) . . . . ?
C41 Ru1 P2 C1 -126.51(10) . . . . ?
P3 Ru1 P2 C1 87.38(8) . . . . ?
C42 Ru1 P3 O2 -25.51(10) . . . . ?
C39 Ru1 P3 O2 -87.84(9) . . . . ?
P1 Ru1 P3 O2 159.49(7) . . . . ?
C43 Ru1 P3 O2 -53.78(9) . . . . ?
C40 Ru1 P3 O2 -91.54(11) . . . . ?
P2 Ru1 P3 O2 75.86(7) . . . . ?
C41 Ru1 P3 O2 -36.56(14) . . . . ?
C42 Ru1 P3 C27 -149.69(11) . . . . ?
C39 Ru1 P3 C27 147.98(11) . . . . ?
P1 Ru1 P3 C27 35.31(9) . . . . ?
C43 Ru1 P3 C27 -177.95(11) . . . . ?
C40 Ru1 P3 C27 144.28(13) . . . . ?
P2 Ru1 P3 C27 -48.32(9) . . . . ?
C41 Ru1 P3 C27 -160.74(14) . . . . ?
C42 Ru1 P3 C33 92.91(11) . . . . ?
C39 Ru1 P3 C33 30.58(11) . . . . ?
P1 Ru1 P3 C33 -82.10(8) . . . . ?
C43 Ru1 P3 C33 64.64(10) . . . . ?
C40 Ru1 P3 C33 26.87(13) . . . . ?
P2 Ru1 P3 C33 -165.72(8) . . . . ?
C41 Ru1 P3 C33 81.86(14) . . . . ?
C2 O1 C1 P2 108.82(16) . . . . ?
C15 P2 C1 O1 175.52(15) . . . . ?
C21 P2 C1 O1 75.27(15) . . . . ?
Ru1 P2 C1 O1 -59.01(14) . . . . ?
C15 P2 C1 C2 -119.17(17) . . . . ?
C21 P2 C1 C2 140.58(17) . . . . ?
Ru1 P2 C1 C2 6.31(18) . . . . ?
C1 O1 C2 P1 -103.19(17) . . . . ?
P2 C1 C2 O1 -100.63(16) . . . . ?
O1 C1 C2 P1 108.15(16) . . . . ?
P2 C1 C2 P1 7.5(2) . . . . ?
C3 P1 C2 O1 -89.91(17) . . . . ?
C9 P1 C2 O1 171.16(16) . . . . ?
Ru1 P1 C2 O1 47.86(16) . . . . ?
C3 P1 C2 C1 -156.21(16) . . . . ?
C9 P1 C2 C1 104.86(17) . . . . ?
Ru1 P1 C2 C1 -18.44(17) . . . . ?
C2 P1 C3 C8 10.0(2) . . . . ?
C9 P1 C3 C8 104.7(2) . . . . ?
Ru1 P1 C3 C8 -119.24(19) . . . . ?
C2 P1 C3 C4 -165.8(2) . . . . ?
C9 P1 C3 C4 -71.1(2) . . . . ?
Ru1 P1 C3 C4 65.0(2) . . . . ?
C8 C3 C4 C5 0.2(4) . . . . ?
P1 C3 C4 C5 176.2(2) . . . . ?
C3 C4 C5 C6 -0.7(5) . . . . ?
C4 C5 C6 C7 0.7(5) . . . . ?
C5 C6 C7 C8 -0.2(5) . . . . ?
C4 C3 C8 C7 0.3(4) . . . . ?
P1 C3 C8 C7 -175.5(2) . . . . ?
C6 C7 C8 C3 -0.4(4) . . . . ?
C2 P1 C9 C10 -98.3(2) . . . . ?
C3 P1 C9 C10 158.8(2) . . . . ?
Ru1 P1 C9 C10 18.7(2) . . . . ?
C2 P1 C9 C14 73.5(2) . . . . ?
C3 P1 C9 C14 -29.4(2) . . . . ?
Ru1 P1 C9 C14 -169.50(16) . . . . ?
C14 C9 C10 C11 0.2(4) . . . . ?
P1 C9 C10 C11 172.2(2) . . . . ?
C9 C10 C11 C12 0.2(4) . . . . ?
C10 C11 C12 C13 -0.8(4) . . . . ?
C11 C12 C13 C14 1.1(4) . . . . ?
C12 C13 C14 C9 -0.7(4) . . . . ?
C10 C9 C14 C13 0.1(3) . . . . ?
P1 C9 C14 C13 -171.78(18) . . . . ?
C21 P2 C15 C20 138.5(2) . . . . ?
C1 P2 C15 C20 36.7(2) . . . . ?
Ru1 P2 C15 C20 -82.8(2) . . . . ?
C21 P2 C15 C16 -44.2(2) . . . . ?
C1 P2 C15 C16 -145.9(2) . . . . ?
Ru1 P2 C15 C16 94.5(2) . . . . ?
C20 C15 C16 C17 2.0(4) . . . . ?
P2 C15 C16 C17 -175.4(3) . . . . ?
C15 C16 C17 C18 -0.2(6) . . . . ?
C16 C17 C18 C19 -1.4(6) . . . . ?
C17 C18 C19 C20 1.1(6) . . . . ?
C18 C19 C20 C15 0.7(5) . . . . ?
C16 C15 C20 C19 -2.3(4) . . . . ?
P2 C15 C20 C19 175.2(2) . . . . ?
C15 P2 C21 C22 99.4(2) . . . . ?
C1 P2 C21 C22 -159.8(2) . . . . ?
Ru1 P2 C21 C22 -35.3(2) . . . . ?
C15 P2 C21 C26 -79.2(3) . . . . ?
C1 P2 C21 C26 21.7(3) . . . . ?
Ru1 P2 C21 C26 146.2(2) . . . . ?
C26 C21 C22 C23 0.5(4) . . . . ?
P2 C21 C22 C23 -178.1(2) . . . . ?
C21 C22 C23 C24 -0.5(4) . . . . ?
C22 C23 C24 C25 0.2(5) . . . . ?
C23 C24 C25 C26 0.1(6) . . . . ?
C24 C25 C26 C21 -0.2(6) . . . . ?
C22 C21 C26 C25 -0.1(5) . . . . ?
P2 C21 C26 C25 178.4(3) . . . . ?
O2 P3 C27 C28 -22.36(19) . . . . ?
C33 P3 C27 C28 -131.34(18) . . . . ?
Ru1 P3 C27 C28 104.84(17) . . . . ?
O2 P3 C27 C32 155.30(19) . . . . ?
C33 P3 C27 C32 46.3(2) . . . . ?
Ru1 P3 C27 C32 -77.5(2) . . . . ?
C32 C27 C28 C29 2.3(3) . . . . ?
P3 C27 C28 C29 -179.83(18) . . . . ?
C27 C28 C29 C30 -1.1(4) . . . . ?
C28 C29 C30 C31 -0.7(4) . . . . ?
C29 C30 C31 C32 1.1(4) . . . . ?
C30 C31 C32 C27 0.2(4) . . . . ?
C28 C27 C32 C31 -1.9(3) . . . . ?
P3 C27 C32 C31 -179.55(18) . . . . ?
O2 P3 C33 C38 177.2(2) . . . . ?
C27 P3 C33 C38 -75.3(2) . . . . ?
Ru1 P3 C33 C38 55.8(2) . . . . ?
O2 P3 C33 C34 -2.5(2) . . . . ?
C27 P3 C33 C34 105.1(2) . . . . ?
Ru1 P3 C33 C34 -123.87(18) . . . . ?
C38 C33 C34 C35 -1.3(4) . . . . ?
P3 C33 C34 C35 178.5(2) . . . . ?
C33 C34 C35 C36 2.2(4) . . . . ?
C34 C35 C36 C37 -1.1(5) . . . . ?
C35 C36 C37 C38 -0.9(5) . . . . ?
C36 C37 C38 C33 1.8(5) . . . . ?
C34 C33 C38 C37 -0.7(4) . . . . ?
P3 C33 C38 C37 179.6(2) . . . . ?
C42 Ru1 C39 C43 -36.02(14) . . . . ?
P1 Ru1 C39 C43 174.76(13) . . . . ?
C40 Ru1 C39 C43 -114.4(2) . . . . ?
P2 Ru1 C39 C43 -49.7(3) . . . . ?
C41 Ru1 C39 C43 -78.26(16) . . . . ?
P3 Ru1 C39 C43 70.00(14) . . . . ?
C42 Ru1 C39 C40 78.38(16) . . . . ?
P1 Ru1 C39 C40 -70.85(15) . . . . ?
C43 Ru1 C39 C40 114.4(2) . . . . ?
P2 Ru1 C39 C40 64.7(3) . . . . ?
C41 Ru1 C39 C40 36.14(14) . . . . ?
P3 Ru1 C39 C40 -175.60(14) . . . . ?
C42 Ru1 C39 C44 -159.9(3) . . . . ?
P1 Ru1 C39 C44 50.9(3) . . . . ?
C43 Ru1 C39 C44 -123.8(3) . . . . ?
C40 Ru1 C39 C44 121.8(3) . . . . ?
P2 Ru1 C39 C44 -173.59(16) . . . . ?
C41 Ru1 C39 C44 157.9(3) . . . . ?
P3 Ru1 C39 C44 -53.8(2) . . . . ?
C43 C39 C40 C41 2.2(2) . . . . ?
C44 C39 C40 C41 166.5(2) . . . . ?
Ru1 C39 C40 C41 -62.79(16) . . . . ?
C43 C39 C40 C45 -166.9(2) . . . . ?
C44 C39 C40 C45 -2.6(4) . . . . ?
Ru1 C39 C40 C45 128.2(2) . . . . ?
C43 C39 C40 Ru1 64.96(15) . . . . ?
C44 C39 C40 Ru1 -130.8(2) . . . . ?
C42 Ru1 C40 C41 37.99(14) . . . . ?
C39 Ru1 C40 C41 118.3(2) . . . . ?
P1 Ru1 C40 C41 -124.54(13) . . . . ?
C43 Ru1 C40 C41 79.67(15) . . . . ?
P2 Ru1 C40 C41 -38.28(16) . . . . ?
P3 Ru1 C40 C41 124.48(13) . . . . ?
C42 Ru1 C40 C39 -80.33(16) . . . . ?
P1 Ru1 C40 C39 117.13(14) . . . . ?
C43 Ru1 C40 C39 -38.65(14) . . . . ?
P2 Ru1 C40 C39 -156.60(12) . . . . ?
C41 Ru1 C40 C39 -118.3(2) . . . . ?
P3 Ru1 C40 C39 6.15(19) . . . . ?
C42 Ru1 C40 C45 162.5(3) . . . . ?
C39 Ru1 C40 C45 -117.1(3) . . . . ?
P1 Ru1 C40 C45 0.0(3) . . . . ?
C43 Ru1 C40 C45 -155.8(3) . . . . ?
P2 Ru1 C40 C45 86.3(3) . . . . ?
C41 Ru1 C40 C45 124.5(3) . . . . ?
P3 Ru1 C40 C45 -111.0(3) . . . . ?
C39 C40 C41 C42 -0.1(2) . . . . ?
C45 C40 C41 C42 168.4(2) . . . . ?
Ru1 C40 C41 C42 -61.79(15) . . . . ?
C39 C40 C41 C46 -165.3(2) . . . . ?
C45 C40 C41 C46 3.1(4) . . . . ?
Ru1 C40 C41 C46 132.9(2) . . . . ?
C39 C40 C41 Ru1 61.74(16) . . . . ?
C45 C40 C41 Ru1 -129.8(2) . . . . ?
C42 Ru1 C41 C40 -116.5(2) . . . . ?
C39 Ru1 C41 C40 -36.87(14) . . . . ?
P1 Ru1 C41 C40 63.90(14) . . . . ?
C43 Ru1 C41 C40 -78.92(15) . . . . ?
P2 Ru1 C41 C40 152.21(13) . . . . ?
P3 Ru1 C41 C40 -98.78(16) . . . . ?
C39 Ru1 C41 C42 79.63(15) . . . . ?
P1 Ru1 C41 C42 -179.59(12) . . . . ?
C43 Ru1 C41 C42 37.58(14) . . . . ?
C40 Ru1 C41 C42 116.5(2) . . . . ?
P2 Ru1 C41 C42 -91.29(14) . . . . ?
P3 Ru1 C41 C42 17.7(2) . . . . ?
C42 Ru1 C41 C46 118.2(3) . . . . ?
C39 Ru1 C41 C46 -162.1(3) . . . . ?
P1 Ru1 C41 C46 -61.4(3) . . . . ?
C43 Ru1 C41 C46 155.8(3) . . . . ?
C40 Ru1 C41 C46 -125.3(3) . . . . ?
P2 Ru1 C41 C46 26.9(3) . . . . ?
P3 Ru1 C41 C46 135.9(2) . . . . ?
C40 C41 C42 C43 -2.1(2) . . . . ?
C46 C41 C42 C43 163.9(2) . . . . ?
Ru1 C41 C42 C43 -64.76(15) . . . . ?
C40 C41 C42 C47 -168.6(2) . . . . ?
C46 C41 C42 C47 -2.6(4) . . . . ?
Ru1 C41 C42 C47 128.8(2) . . . . ?
C40 C41 C42 Ru1 62.62(15) . . . . ?
C46 C41 C42 Ru1 -131.4(2) . . . . ?
C39 Ru1 C42 C43 36.48(14) . . . . ?
P1 Ru1 C42 C43 116.44(15) . . . . ?
C40 Ru1 C42 C43 78.62(15) . . . . ?
P2 Ru1 C42 C43 -148.00(13) . . . . ?
C41 Ru1 C42 C43 115.7(2) . . . . ?
P3 Ru1 C42 C43 -53.44(14) . . . . ?
C39 Ru1 C42 C41 -79.20(16) . . . . ?
P1 Ru1 C42 C41 0.8(2) . . . . ?
C43 Ru1 C42 C41 -115.7(2) . . . . ?
C40 Ru1 C42 C41 -37.05(15) . . . . ?
P2 Ru1 C42 C41 96.33(14) . . . . ?
P3 Ru1 C42 C41 -169.11(13) . . . . ?
C39 Ru1 C42 C47 158.5(3) . . . . ?
P1 Ru1 C42 C47 -121.5(2) . . . . ?
C43 Ru1 C42 C47 122.1(3) . . . . ?
C40 Ru1 C42 C47 -159.3(3) . . . . ?
P2 Ru1 C42 C47 -25.9(2) . . . . ?
C41 Ru1 C42 C47 -122.3(3) . . . . ?
P3 Ru1 C42 C47 68.6(2) . . . . ?
C41 C42 C43 C39 3.5(2) . . . . ?
C47 C42 C43 C39 170.0(2) . . . . ?
Ru1 C42 C43 C39 -61.35(15) . . . . ?
C41 C42 C43 C48 -164.6(2) . . . . ?
C47 C42 C43 C48 1.9(4) . . . . ?
Ru1 C42 C43 C48 130.5(2) . . . . ?
C41 C42 C43 Ru1 64.89(15) . . . . ?
C47 C42 C43 Ru1 -128.6(2) . . . . ?
C40 C39 C43 C42 -3.5(2) . . . . ?
C44 C39 C43 C42 -167.5(2) . . . . ?
Ru1 C39 C43 C42 61.48(16) . . . . ?
C40 C39 C43 C48 164.3(2) . . . . ?
C44 C39 C43 C48 0.4(4) . . . . ?
Ru1 C39 C43 C48 -130.7(2) . . . . ?
C40 C39 C43 Ru1 -65.01(15) . . . . ?
C44 C39 C43 Ru1 131.0(3) . . . . ?
C39 Ru1 C43 C42 -118.8(2) . . . . ?
P1 Ru1 C43 C42 -127.72(14) . . . . ?
C40 Ru1 C43 C42 -79.98(16) . . . . ?
P2 Ru1 C43 C42 42.54(16) . . . . ?
C41 Ru1 C43 C42 -38.40(14) . . . . ?
P3 Ru1 C43 C42 130.01(13) . . . . ?
C42 Ru1 C43 C39 118.8(2) . . . . ?
P1 Ru1 C43 C39 -8.9(2) . . . . ?
C40 Ru1 C43 C39 38.81(15) . . . . ?
P2 Ru1 C43 C39 161.33(12) . . . . ?
C41 Ru1 C43 C39 80.39(16) . . . . ?
P3 Ru1 C43 C39 -111.21(15) . . . . ?
C42 Ru1 C43 C48 -119.5(3) . . . . ?
C39 Ru1 C43 C48 121.8(3) . . . . ?
P1 Ru1 C43 C48 112.8(2) . . . . ?
C40 Ru1 C43 C48 160.6(3) . . . . ?
P2 Ru1 C43 C48 -76.9(3) . . . . ?
C41 Ru1 C43 C48 -157.9(3) . . . . ?
P3 Ru1 C43 C48 10.5(3) . . . . ?
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 27.52
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 0.376
_refine_diff_density_min -0.417
_refine_diff_density_rms 0.066
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 -0.067 0.250 151 36 ' '
2 0.500 0.067 0.750 151 36 ' '
3 1.000 0.433 0.250 151 36 ' '
4 0.000 0.567 0.750 151 36 ' '
_platon_squeeze_details
;
During the
refinement of the structure, electron density peaks were located
that were believed to be highly disordered
solvent molecules (probably butanol). Attempts
made to model the solvent molecule were not successful.
The SQUEEZE option in PLATON (Spek, 2003) indicated there was a
large solvent cavity. 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.
;
_iucr_refine_instructions_details
;
TITL d1292 P2(1)/n R = New: C2/c
CELL 0.71073 22.1396 11.6632 33.3240 90.000 104.066 90.000
ZERR 8 0.0015 0.0008 0.0020 0.000 0.002 0.000
LATT 7
SYMM - X , Y , 0.50000 - Z
SFAC C H O P Ru
UNIT 384 376 16 24 8
L.S. 5
FMAP 2
PLAN -20
TEMP -123
SIZE 0.200 0.200 0.280
ACTA
BOND $H
CONF
WGHT 0.0297 9.8399
FVAR 1.03699
RU1 5 0.377142 0.493817 0.352487 11.00000 0.01778 0.02380 =
0.01331 0.00161 -0.00140 -0.00525
P1 4 0.357865 0.444911 0.414410 11.00000 0.01543 0.03110 =
0.01635 0.00506 -0.00031 -0.00347
P2 4 0.478200 0.448993 0.385264 11.00000 0.01840 0.02317 =
0.01736 0.00220 0.00295 0.00013
P3 4 0.398318 0.692833 0.363002 11.00000 0.01896 0.02344 =
0.01777 0.00266 -0.00120 -0.00046
O1 3 0.470019 0.540112 0.459043 11.00000 0.02190 0.02116 =
0.01982 -0.00139 -0.00046 -0.00269
O2 3 0.434816 0.737908 0.333189 11.00000 0.02744 0.02873 =
0.02213 0.00456 0.00210 -0.00420
C1 1 0.486871 0.435830 0.441411 11.00000 0.01678 0.02208 =
0.01822 0.00222 -0.00058 0.00078
AFIX 13
H1A 2 0.521756 0.390774 0.457567 11.00000 -1.20000
AFIX 0
C2 1 0.429368 0.442810 0.456069 11.00000 0.01871 0.02164 =
0.01519 0.00172 0.00099 -0.00124
AFIX 13
H2A 2 0.428345 0.402348 0.481669 11.00000 -1.20000
AFIX 0
C3 1 0.302281 0.514933 0.439365 11.00000 0.02232 0.04561 =
0.03269 0.02038 0.01086 0.00914
C4 1 0.238609 0.509453 0.420309 11.00000 0.02337 0.07371 =
0.06154 0.03852 0.00986 0.00800
AFIX 43
H4A 2 0.225176 0.474673 0.394566 11.00000 -1.20000
AFIX 0
C5 1 0.195250 0.556132 0.439901 11.00000 0.02982 0.09238 =
0.11660 0.07557 0.03491 0.02801
AFIX 43
H5A 2 0.153024 0.553096 0.426985 11.00000 -1.20000
AFIX 0
C6 1 0.214451 0.606224 0.477913 11.00000 0.07783 0.09027 =
0.10516 0.07019 0.07107 0.05780
AFIX 43
H6A 2 0.185282 0.636371 0.490928 11.00000 -1.20000
AFIX 0
C7 1 0.276422 0.612099 0.496834 11.00000 0.08553 0.05923 =
0.06117 0.03204 0.05123 0.04311
AFIX 43
H7A 2 0.289328 0.646481 0.522685 11.00000 -1.20000
AFIX 0
C8 1 0.320303 0.566978 0.477668 11.00000 0.04626 0.04875 =
0.03334 0.01860 0.02051 0.02393
AFIX 43
H8A 2 0.362392 0.571871 0.490802 11.00000 -1.20000
AFIX 0
C9 1 0.338949 0.294432 0.423808 11.00000 0.02052 0.03957 =
0.02196 0.00774 -0.00555 -0.01121
C10 1 0.353786 0.208190 0.399561 11.00000 0.04599 0.04121 =
0.02325 0.00407 -0.00251 -0.01582
AFIX 43
H10A 2 0.368545 0.227097 0.376556 11.00000 -1.20000
AFIX 0
C11 1 0.347001 0.092524 0.408999 11.00000 0.06146 0.03647 =
0.03635 0.00131 -0.00697 -0.01660
AFIX 43
H11A 2 0.357237 0.035095 0.392450 11.00000 -1.20000
AFIX 0
C12 1 0.325055 0.064864 0.442979 11.00000 0.04097 0.04442 =
0.04765 0.02026 -0.00959 -0.02059
AFIX 43
H12A 2 0.319966 -0.011688 0.449245 11.00000 -1.20000
AFIX 0
C13 1 0.310624 0.149343 0.467687 11.00000 0.02650 0.05283 =
0.03989 0.02071 0.00050 -0.01236
AFIX 43
H13A 2 0.296474 0.129615 0.490858 11.00000 -1.20000
AFIX 0
C14 1 0.316928 0.263749 0.458453 11.00000 0.02142 0.04692 =
0.03240 0.01318 0.00124 -0.00933
AFIX 43
H14A 2 0.306556 0.320441 0.475230 11.00000 -1.20000
AFIX 0
C15 1 0.509207 0.309139 0.375411 11.00000 0.03451 0.03246 =
0.02318 0.00079 0.00336 0.01055
C16 1 0.542669 0.295760 0.345159 11.00000 0.06104 0.05648 =
0.03136 0.00233 0.01419 0.02558
AFIX 43
H16A 2 0.552001 0.359582 0.331054 11.00000 -1.20000
AFIX 0
C17 1 0.561982 0.188198 0.336075 11.00000 0.10675 0.07861 =
0.04443 -0.00332 0.02038 0.05925
AFIX 43
H17A 2 0.584116 0.180406 0.315817 11.00000 -1.20000
AFIX 0
C18 1 0.549023 0.093408 0.356405 11.00000 0.13832 0.05785 =
0.05079 -0.00848 0.00062 0.06147
AFIX 43
H18A 2 0.561489 0.021339 0.349582 11.00000 -1.20000
AFIX 0
C19 1 0.517279 0.104572 0.387226 11.00000 0.09951 0.03353 =
0.04703 0.00352 -0.00766 0.02100
AFIX 43
H19A 2 0.509002 0.040227 0.401485 11.00000 -1.20000
AFIX 0
C20 1 0.497900 0.211856 0.396746 11.00000 0.05670 0.02949 =
0.02941 0.00216 -0.00110 0.00763
AFIX 43
H20A 2 0.477022 0.219112 0.417692 11.00000 -1.20000
AFIX 0
C21 1 0.546848 0.536357 0.384634 11.00000 0.01961 0.03184 =
0.03301 0.00678 0.00905 -0.00006
C22 1 0.550707 0.598098 0.349995 11.00000 0.02689 0.03850 =
0.03707 0.00617 0.01189 0.00109
AFIX 43
H22A 2 0.517579 0.597713 0.326673 11.00000 -1.20000
AFIX 0
C23 1 0.604275 0.661067 0.349958 11.00000 0.03859 0.05009 =
0.05748 0.01872 0.02710 0.00132
AFIX 43
H23A 2 0.606858 0.702018 0.326486 11.00000 -1.20000
AFIX 0
C24 1 0.653065 0.662923 0.384277 11.00000 0.02825 0.07799 =
0.07960 0.01823 0.01697 -0.01668
AFIX 43
H24A 2 0.688603 0.705282 0.384140 11.00000 -1.20000
AFIX 0
C25 1 0.649460 0.602657 0.418597 11.00000 0.02758 0.11856 =
0.06804 0.03133 -0.00316 -0.02584
AFIX 43
H25A 2 0.682586 0.604077 0.441914 11.00000 -1.20000
AFIX 0
C26 1 0.596907 0.539467 0.418969 11.00000 0.02234 0.08903 =
0.04714 0.02895 -0.00226 -0.01379
AFIX 43
H26A 2 0.595040 0.498420 0.442563 11.00000 -1.20000
AFIX 0
C27 1 0.439027 0.753614 0.413626 11.00000 0.02804 0.01596 =
0.02068 0.00366 -0.00233 0.00214
C28 1 0.500819 0.786479 0.418191 11.00000 0.02910 0.02596 =
0.02610 0.00323 0.00015 -0.00465
AFIX 43
H28A 2 0.519385 0.777379 0.396178 11.00000 -1.20000
AFIX 0
C29 1 0.535034 0.832580 0.455107 11.00000 0.03798 0.03058 =
0.03266 0.00087 -0.00874 -0.01329
AFIX 43
H29A 2 0.576440 0.852785 0.457693 11.00000 -1.20000
AFIX 0
C30 1 0.508533 0.848733 0.487852 11.00000 0.05172 0.02625 =
0.02609 -0.00250 -0.01105 -0.00085
AFIX 43
H30A 2 0.531821 0.878946 0.512631 11.00000 -1.20000
AFIX 0
C31 1 0.446718 0.819509 0.483550 11.00000 0.04612 0.03546 =
0.02404 -0.00014 0.00160 0.01453
AFIX 43
H31A 2 0.428185 0.831402 0.505434 11.00000 -1.20000
AFIX 0
C32 1 0.412173 0.772642 0.446887 11.00000 0.02863 0.03229 =
0.02787 0.00198 0.00110 0.00882
AFIX 43
H32A 2 0.370630 0.753646 0.444407 11.00000 -1.20000
AFIX 0
C33 1 0.326308 0.779844 0.353744 11.00000 0.02528 0.03064 =
0.02431 -0.00090 -0.00336 0.00449
C34 1 0.319475 0.868060 0.324634 11.00000 0.03782 0.03210 =
0.02532 0.00057 -0.00135 0.00680
AFIX 43
H34A 2 0.351021 0.882256 0.311266 11.00000 -1.20000
AFIX 0
C35 1 0.266036 0.934535 0.315545 11.00000 0.05233 0.03634 =
0.03744 0.00525 -0.00710 0.01623
AFIX 43
H35A 2 0.261429 0.991310 0.295432 11.00000 -1.20000
AFIX 0
C36 1 0.219835 0.917568 0.335876 11.00000 0.04290 0.06349 =
0.04728 0.00329 -0.00585 0.03138
AFIX 43
H36A 2 0.184440 0.963502 0.329861 11.00000 -1.20000
AFIX 0
C37 1 0.226021 0.831462 0.365530 11.00000 0.02932 0.07434 =
0.04722 0.00352 0.00437 0.01966
AFIX 43
H37A 2 0.195130 0.820261 0.379704 11.00000 -1.20000
AFIX 0
C38 1 0.278714 0.762426 0.373770 11.00000 0.02789 0.04376 =
0.03665 0.00955 -0.00046 0.00818
AFIX 43
H38A 2 0.282273 0.703507 0.393009 11.00000 -1.20000
AFIX 0
C39 1 0.286456 0.506974 0.302984 11.00000 0.02656 0.04367 =
0.01719 0.00485 -0.00886 -0.01018
C40 1 0.297032 0.387925 0.313029 11.00000 0.03615 0.04214 =
0.01530 0.00280 -0.00875 -0.02093
C41 1 0.352630 0.352368 0.302788 11.00000 0.04683 0.03049 =
0.01358 -0.00219 -0.00521 -0.01356
C42 1 0.377283 0.451114 0.285963 11.00000 0.03814 0.03232 =
0.01370 -0.00159 0.00081 -0.00963
C43 1 0.335456 0.542919 0.284856 11.00000 0.03404 0.03486 =
0.01236 0.00138 -0.00555 -0.01286
C44 1 0.226525 0.569153 0.300899 11.00000 0.02468 0.06435 =
0.03656 0.01350 -0.01076 -0.00616
AFIX 137
H44A 2 0.195038 0.540780 0.277940 11.00000 -1.50000
H44B 2 0.232446 0.649710 0.297337 11.00000 -1.50000
H44C 2 0.213706 0.556795 0.326087 11.00000 -1.50000
AFIX 0
C45 1 0.248615 0.312422 0.324463 11.00000 0.04582 0.05911 =
0.03138 0.00746 -0.01117 -0.03374
AFIX 137
H45A 2 0.211140 0.314316 0.302721 11.00000 -1.50000
H45B 2 0.239973 0.339673 0.349674 11.00000 -1.50000
H45C 2 0.263871 0.235151 0.328282 11.00000 -1.50000
AFIX 0
C46 1 0.374518 0.232163 0.299033 11.00000 0.07100 0.03300 =
0.02270 -0.00588 0.00072 -0.00963
AFIX 137
H46A 2 0.368764 0.213033 0.270331 11.00000 -1.50000
H46B 2 0.350948 0.180179 0.311602 11.00000 -1.50000
H46C 2 0.417865 0.226268 0.312760 11.00000 -1.50000
AFIX 0
C47 1 0.428970 0.448549 0.264250 11.00000 0.05697 0.04805 =
0.02147 -0.00093 0.01262 -0.00409
AFIX 137
H47A 2 0.412669 0.427119 0.235864 11.00000 -1.50000
H47B 2 0.459770 0.393727 0.277456 11.00000 -1.50000
H47C 2 0.447653 0.523154 0.265492 11.00000 -1.50000
AFIX 0
C48 1 0.336023 0.650551 0.260417 11.00000 0.04666 0.03972 =
0.01593 0.00657 -0.00261 -0.01047
AFIX 137
H48A 2 0.327208 0.632270 0.231486 11.00000 -1.50000
H48B 2 0.376279 0.685955 0.268734 11.00000 -1.50000
H48C 2 0.304944 0.702401 0.265371 11.00000 -1.50000
HKLF 4
REM d1292 P2(1)/n R = New: C2/c
REM R1 = 0.0349 for 7782 Fo > 4sig(Fo) and 0.0473 for all 9592 data
REM 492 parameters refined using 0 restraints
END
REM Highest difference peak 0.373, deepest hole -0.418, 1-sigma level 0.066
Q1 1 0.2519 0.5938 0.4798 11.00000 0.05 0.37
Q2 1 0.2097 0.5665 0.4581 11.00000 0.05 0.35
Q3 1 0.4585 0.4020 0.4451 11.00000 0.05 0.35
Q4 1 0.2378 0.4578 0.4116 11.00000 0.05 0.34
Q5 1 0.4982 0.3796 0.3781 11.00000 0.05 0.33
Q6 1 0.5176 0.4956 0.3815 11.00000 0.05 0.31
Q7 1 0.4210 0.7938 0.4256 11.00000 0.05 0.31
Q8 1 0.4793 0.4455 0.4153 11.00000 0.05 0.31
Q9 1 0.0000 0.2642 0.2500 10.50000 0.05 0.30
Q10 1 0.4137 0.4388 0.3429 11.00000 0.05 0.29
Q11 1 0.5004 0.2626 0.3822 11.00000 0.05 0.29
Q12 1 0.3398 0.4566 0.3574 11.00000 0.05 0.29
Q13 1 0.2812 0.6566 0.5003 11.00000 0.05 0.28
Q14 1 0.3695 0.5076 0.2955 11.00000 0.05 0.28
Q15 1 0.3588 0.4006 0.2858 11.00000 0.05 0.28
Q16 1 0.3081 0.5029 0.2780 11.00000 0.05 0.28
Q17 1 0.3693 0.3996 0.2960 11.00000 0.05 0.27
Q18 1 0.4085 0.5462 0.3376 11.00000 0.05 0.27
Q19 1 0.3111 0.1193 0.4485 11.00000 0.05 0.27
Q20 1 0.5188 0.2968 0.3579 11.00000 0.05 0.27
;
_vrf_PLAT220_2
;
PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.5 Ratio
RESPONSE: There is no evidence to suggest a disorder model should
be used.
;
_database_code_depnum_ccdc_archive 'CCDC 951750'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_5
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C48 H47 P3 Ru S'
_chemical_formula_sum 'C48 H47 P3 Ru S'
_chemical_formula_weight 849.90
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru 0.0552 3.2960 '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 10.6911(4)
_cell_length_b 12.0014(5)
_cell_length_c 19.0065(8)
_cell_angle_alpha 73.029(3)
_cell_angle_beta 88.592(3)
_cell_angle_gamma 70.042(3)
_cell_volume 2184.75(15)
_cell_formula_units_Z 2
_cell_measurement_temperature 147(2)
_cell_measurement_reflns_used 4489
_cell_measurement_theta_min 4.11
_cell_measurement_theta_max 65.53
_exptl_crystal_description needle
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.03
_exptl_crystal_size_mid 0.02
_exptl_crystal_size_min 0.02
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.292
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 880
_exptl_absorpt_coefficient_mu 4.619
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6458
_exptl_absorpt_correction_T_max 0.7528
_exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 147(2)
_diffrn_radiation_wavelength 1.54178
_diffrn_radiation_type CuK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 43998
_diffrn_reflns_av_R_equivalents 0.0972
_diffrn_reflns_av_sigmaI/netI 0.0584
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_theta_min 4.10
_diffrn_reflns_theta_max 66.74
_reflns_number_total 7367
_reflns_number_gt 5873
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'Bruker APEX2'
_computing_cell_refinement 'Bruker SAINT'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_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^)+(0.1056P)^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 7367
_refine_ls_number_parameters 483
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0694
_refine_ls_R_factor_gt 0.0556
_refine_ls_wR_factor_ref 0.1713
_refine_ls_wR_factor_gt 0.1615
_refine_ls_goodness_of_fit_ref 1.147
_refine_ls_restrained_S_all 1.148
_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
Ru1 Ru 0.21664(4) 0.45522(3) 0.26685(2) 0.01427(15) Uani 1 1 d . . .
P1 P 0.00918(14) 0.43158(12) 0.26641(7) 0.0159(3) Uani 1 1 d . . .
P2 P 0.16470(14) 0.47323(12) 0.38089(7) 0.0167(3) Uani 1 1 d . . .
P3 P 0.11127(14) 0.67382(12) 0.21577(8) 0.0164(3) Uani 1 1 d . . .
S1 S -0.03409(14) 0.77173(12) 0.26707(8) 0.0214(3) Uani 1 1 d . . .
C1 C -0.0110(6) 0.5035(5) 0.3902(3) 0.0199(12) Uani 1 1 d . . .
H1A H -0.0537 0.5331 0.4290 0.024 Uiso 1 1 calc R . .
C2 C -0.0777(6) 0.4828(5) 0.3409(3) 0.0201(12) Uani 1 1 d . . .
H2A H -0.1699 0.4944 0.3443 0.024 Uiso 1 1 calc R . .
C3 C -0.1253(5) 0.5132(5) 0.1913(3) 0.0180(12) Uani 1 1 d . . .
C4 C -0.1479(6) 0.4592(5) 0.1387(3) 0.0203(12) Uani 1 1 d . . .
H4A H -0.0944 0.3762 0.1417 0.024 Uiso 1 1 calc R . .
C5 C -0.2487(6) 0.5275(6) 0.0827(3) 0.0288(14) Uani 1 1 d . . .
H5A H -0.2648 0.4900 0.0479 0.035 Uiso 1 1 calc R . .
C6 C -0.3261(6) 0.6487(6) 0.0761(3) 0.0278(14) Uani 1 1 d . . .
H6A H -0.3944 0.6942 0.0369 0.033 Uiso 1 1 calc R . .
C7 C -0.3040(6) 0.7038(6) 0.1268(4) 0.0301(14) Uani 1 1 d . . .
H7A H -0.3567 0.7876 0.1225 0.036 Uiso 1 1 calc R . .
C8 C -0.2037(6) 0.6358(5) 0.1845(3) 0.0220(12) Uani 1 1 d . . .
H8A H -0.1890 0.6737 0.2195 0.026 Uiso 1 1 calc R . .
C9 C -0.0004(6) 0.2740(5) 0.2883(3) 0.0185(12) Uani 1 1 d . . .
C10 C 0.0497(6) 0.1996(5) 0.2432(4) 0.0263(13) Uani 1 1 d . . .
H10A H 0.0928 0.2289 0.2013 0.032 Uiso 1 1 calc R . .
C11 C 0.0384(6) 0.0833(5) 0.2578(4) 0.0309(15) Uani 1 1 d . . .
H11A H 0.0724 0.0347 0.2255 0.037 Uiso 1 1 calc R . .
C12 C -0.0219(7) 0.0384(6) 0.3191(4) 0.0366(16) Uani 1 1 d . . .
H12A H -0.0301 -0.0411 0.3295 0.044 Uiso 1 1 calc R . .
C13 C -0.0709(8) 0.1116(6) 0.3656(4) 0.0377(17) Uani 1 1 d . . .
H13A H -0.1113 0.0808 0.4085 0.045 Uiso 1 1 calc R . .
C14 C -0.0615(7) 0.2282(6) 0.3502(4) 0.0303(14) Uani 1 1 d . . .
H14A H -0.0969 0.2774 0.3821 0.036 Uiso 1 1 calc R . .
C15 C 0.2273(6) 0.3292(5) 0.4608(3) 0.0183(12) Uani 1 1 d . . .
C16 C 0.2748(6) 0.3247(6) 0.5294(3) 0.0246(13) Uani 1 1 d . . .
H16A H 0.2849 0.3968 0.5358 0.029 Uiso 1 1 calc R . .
C17 C 0.3077(7) 0.2166(6) 0.5887(3) 0.0311(14) Uani 1 1 d . . .
H17A H 0.3398 0.2150 0.6353 0.037 Uiso 1 1 calc R . .
C18 C 0.2932(7) 0.1107(6) 0.5792(4) 0.0369(16) Uani 1 1 d . . .
H18A H 0.3148 0.0364 0.6194 0.044 Uiso 1 1 calc R . .
C19 C 0.2470(7) 0.1147(6) 0.5105(3) 0.0301(14) Uani 1 1 d . . .
H19A H 0.2382 0.0424 0.5035 0.036 Uiso 1 1 calc R . .
C20 C 0.2141(6) 0.2217(5) 0.4530(3) 0.0245(13) Uani 1 1 d . . .
H20A H 0.1814 0.2231 0.4066 0.029 Uiso 1 1 calc R . .
C21 C 0.2017(6) 0.5832(5) 0.4197(3) 0.0223(13) Uani 1 1 d . . .
C22 C 0.3334(6) 0.5731(5) 0.4277(3) 0.0225(12) Uani 1 1 d . . .
H22A H 0.4016 0.5092 0.4146 0.027 Uiso 1 1 calc R . .
C23 C 0.3671(7) 0.6560(6) 0.4547(4) 0.0310(15) Uani 1 1 d . . .
H23A H 0.4582 0.6475 0.4607 0.037 Uiso 1 1 calc R . .
C24 C 0.2696(7) 0.7502(6) 0.4729(3) 0.0297(15) Uani 1 1 d . . .
H24A H 0.2929 0.8071 0.4910 0.036 Uiso 1 1 calc R . .
C25 C 0.1366(7) 0.7614(5) 0.4644(3) 0.0263(14) Uani 1 1 d . . .
H25A H 0.0685 0.8272 0.4760 0.032 Uiso 1 1 calc R . .
C26 C 0.1030(6) 0.6779(5) 0.4394(3) 0.0214(12) Uani 1 1 d . . .
H26A H 0.0121 0.6847 0.4354 0.026 Uiso 1 1 calc R . .
C27 C 0.2289(6) 0.7600(5) 0.2037(3) 0.0213(12) Uani 1 1 d . . .
C28 C 0.2673(6) 0.7859(5) 0.2644(3) 0.0206(12) Uani 1 1 d . . .
H28A H 0.2341 0.7583 0.3106 0.025 Uiso 1 1 calc R . .
C29 C 0.3534(6) 0.8515(6) 0.2589(4) 0.0310(15) Uani 1 1 d . . .
H29A H 0.3808 0.8658 0.3016 0.037 Uiso 1 1 calc R . .
C30 C 0.3994(7) 0.8960(6) 0.1923(4) 0.0315(15) Uani 1 1 d . . .
H30A H 0.4587 0.9407 0.1887 0.038 Uiso 1 1 calc R . .
C31 C 0.3584(6) 0.8749(6) 0.1306(4) 0.0307(15) Uani 1 1 d . . .
H31A H 0.3868 0.9081 0.0839 0.037 Uiso 1 1 calc R . .
C32 C 0.2763(6) 0.8060(5) 0.1363(3) 0.0222(12) Uani 1 1 d . . .
H32A H 0.2517 0.7896 0.0937 0.027 Uiso 1 1 calc R . .
C33 C 0.0412(6) 0.7234(5) 0.1188(3) 0.0217(12) Uani 1 1 d . . .
C34 C -0.0264(6) 0.8501(5) 0.0838(3) 0.0232(12) Uani 1 1 d U . .
H34A H -0.0331 0.9090 0.1093 0.028 Uiso 1 1 calc R . .
C35 C -0.0834(6) 0.8898(5) 0.0124(3) 0.0244(13) Uani 1 1 d U . .
H35A H -0.1285 0.9760 -0.0112 0.029 Uiso 1 1 calc R . .
C36 C -0.0749(6) 0.8038(6) -0.0253(3) 0.0270(14) Uani 1 1 d . . .
H36A H -0.1136 0.8309 -0.0745 0.032 Uiso 1 1 calc R . .
C37 C -0.0101(6) 0.6803(6) 0.0096(3) 0.0230(13) Uani 1 1 d . . .
H37A H -0.0055 0.6215 -0.0156 0.028 Uiso 1 1 calc R . .
C38 C 0.0484(6) 0.6392(5) 0.0803(3) 0.0206(12) Uani 1 1 d . . .
H38A H 0.0940 0.5529 0.1031 0.025 Uiso 1 1 calc R . .
C39 C 0.3745(6) 0.4403(5) 0.1828(3) 0.0219(12) Uani 1 1 d . . .
C40 C 0.3301(5) 0.3372(5) 0.1946(3) 0.0160(11) Uani 1 1 d . . .
C41 C 0.3658(5) 0.2630(5) 0.2698(3) 0.0175(11) Uani 1 1 d . . .
C42 C 0.4299(6) 0.3224(5) 0.3050(3) 0.0192(12) Uani 1 1 d . . .
C43 C 0.4345(5) 0.4328(5) 0.2512(3) 0.0154(11) Uani 1 1 d . . .
C44 C 0.3865(6) 0.5216(6) 0.1076(3) 0.0253(13) Uani 1 1 d . . .
H44A H 0.4496 0.4708 0.0812 0.038 Uiso 1 1 calc R . .
H44B H 0.4189 0.5860 0.1132 0.038 Uiso 1 1 calc R . .
H44C H 0.2989 0.5610 0.0796 0.038 Uiso 1 1 calc R . .
C45 C 0.2894(6) 0.2977(6) 0.1331(3) 0.0248(13) Uani 1 1 d . . .
H45A H 0.3514 0.3028 0.0945 0.037 Uiso 1 1 calc R . .
H45B H 0.1987 0.3526 0.1124 0.037 Uiso 1 1 calc R . .
H45C H 0.2914 0.2119 0.1526 0.037 Uiso 1 1 calc R . .
C46 C 0.3676(6) 0.1327(5) 0.3030(4) 0.0269(14) Uani 1 1 d . . .
H46A H 0.4423 0.0754 0.2859 0.040 Uiso 1 1 calc R . .
H46B H 0.2835 0.1272 0.2877 0.040 Uiso 1 1 calc R . .
H46C H 0.3780 0.1104 0.3569 0.040 Uiso 1 1 calc R . .
C47 C 0.5089(6) 0.2642(5) 0.3777(3) 0.0229(12) Uani 1 1 d . . .
H47A H 0.6019 0.2199 0.3709 0.034 Uiso 1 1 calc R . .
H47B H 0.4716 0.2054 0.4100 0.034 Uiso 1 1 calc R . .
H47C H 0.5055 0.3288 0.4003 0.034 Uiso 1 1 calc R . .
C48 C 0.5172(6) 0.5075(6) 0.2594(4) 0.0264(13) Uani 1 1 d . . .
H48A H 0.6110 0.4627 0.2545 0.040 Uiso 1 1 calc R . .
H48B H 0.5085 0.5206 0.3081 0.040 Uiso 1 1 calc R . .
H48C H 0.4864 0.5881 0.2209 0.040 Uiso 1 1 calc R . .
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 0.0145(2) 0.0115(2) 0.0173(2) -0.00544(16) 0.00417(16) -0.00433(16)
P1 0.0148(7) 0.0144(6) 0.0203(7) -0.0063(5) 0.0048(6) -0.0065(6)
P2 0.0176(7) 0.0130(6) 0.0188(7) -0.0048(5) 0.0046(6) -0.0047(6)
P3 0.0179(7) 0.0117(6) 0.0204(7) -0.0057(5) 0.0042(6) -0.0056(6)
S1 0.0226(7) 0.0172(7) 0.0247(8) -0.0090(6) 0.0044(6) -0.0052(6)
C1 0.029(3) 0.015(3) 0.016(3) -0.005(2) 0.003(2) -0.008(2)
C2 0.016(3) 0.016(3) 0.032(3) -0.011(2) 0.013(2) -0.008(2)
C3 0.013(3) 0.022(3) 0.026(3) -0.009(2) 0.008(2) -0.012(2)
C4 0.022(3) 0.021(3) 0.019(3) -0.008(2) 0.000(2) -0.008(2)
C5 0.028(3) 0.036(4) 0.026(3) -0.013(3) -0.001(3) -0.013(3)
C6 0.019(3) 0.032(3) 0.023(3) 0.004(3) -0.006(2) -0.007(3)
C7 0.021(3) 0.026(3) 0.042(4) -0.011(3) 0.007(3) -0.007(3)
C8 0.023(3) 0.022(3) 0.024(3) -0.009(2) 0.005(2) -0.010(3)
C9 0.018(3) 0.017(3) 0.021(3) -0.006(2) -0.002(2) -0.005(2)
C10 0.020(3) 0.020(3) 0.035(4) -0.006(3) 0.001(3) -0.003(2)
C11 0.025(3) 0.017(3) 0.048(4) -0.015(3) -0.008(3) 0.001(3)
C12 0.046(4) 0.020(3) 0.045(4) -0.005(3) -0.006(3) -0.016(3)
C13 0.048(4) 0.035(4) 0.038(4) -0.005(3) 0.007(3) -0.028(4)
C14 0.039(4) 0.022(3) 0.032(4) -0.008(3) 0.006(3) -0.014(3)
C15 0.020(3) 0.021(3) 0.009(3) -0.002(2) 0.000(2) -0.004(2)
C16 0.018(3) 0.023(3) 0.028(3) -0.007(3) -0.002(2) -0.002(3)
C17 0.035(4) 0.032(3) 0.019(3) -0.004(3) 0.000(3) -0.006(3)
C18 0.037(4) 0.026(3) 0.032(4) 0.010(3) 0.004(3) -0.007(3)
C19 0.033(4) 0.021(3) 0.030(4) 0.000(3) 0.002(3) -0.009(3)
C20 0.029(3) 0.021(3) 0.022(3) -0.005(2) 0.004(3) -0.009(3)
C21 0.029(3) 0.014(3) 0.021(3) -0.002(2) 0.008(2) -0.008(3)
C22 0.026(3) 0.024(3) 0.017(3) -0.008(2) -0.006(2) -0.007(3)
C23 0.028(3) 0.027(3) 0.039(4) -0.007(3) -0.006(3) -0.013(3)
C24 0.045(4) 0.023(3) 0.018(3) -0.003(2) -0.016(3) -0.011(3)
C25 0.042(4) 0.023(3) 0.021(3) -0.017(2) 0.007(3) -0.010(3)
C26 0.023(3) 0.018(3) 0.016(3) 0.002(2) 0.000(2) -0.003(2)
C27 0.023(3) 0.014(3) 0.026(3) -0.006(2) 0.000(2) -0.005(2)
C28 0.023(3) 0.019(3) 0.021(3) -0.004(2) 0.000(2) -0.012(2)
C29 0.027(3) 0.025(3) 0.048(4) -0.017(3) 0.002(3) -0.013(3)
C30 0.030(4) 0.025(3) 0.048(4) -0.014(3) 0.006(3) -0.017(3)
C31 0.025(3) 0.029(3) 0.039(4) -0.007(3) 0.010(3) -0.014(3)
C32 0.023(3) 0.020(3) 0.022(3) -0.004(2) 0.004(2) -0.008(2)
C33 0.021(3) 0.017(3) 0.029(3) -0.007(2) 0.013(3) -0.009(2)
C34 0.023(3) 0.015(3) 0.032(3) -0.009(2) 0.002(2) -0.007(2)
C35 0.027(3) 0.018(3) 0.016(3) 0.008(2) -0.006(2) -0.004(3)
C36 0.030(3) 0.034(3) 0.020(3) -0.007(3) 0.001(3) -0.015(3)
C37 0.030(3) 0.033(3) 0.010(3) -0.008(2) -0.002(2) -0.012(3)
C38 0.022(3) 0.018(3) 0.027(3) -0.012(2) 0.008(2) -0.010(2)
C39 0.017(3) 0.017(3) 0.033(3) -0.013(2) 0.011(2) -0.003(2)
C40 0.012(3) 0.016(3) 0.020(3) -0.008(2) 0.003(2) -0.001(2)
C41 0.014(3) 0.015(3) 0.024(3) -0.009(2) 0.002(2) -0.004(2)
C42 0.015(3) 0.018(3) 0.019(3) -0.003(2) 0.000(2) 0.000(2)
C43 0.009(3) 0.021(3) 0.017(3) -0.007(2) 0.007(2) -0.006(2)
C44 0.028(3) 0.026(3) 0.024(3) -0.009(2) 0.010(3) -0.010(3)
C45 0.030(3) 0.025(3) 0.023(3) -0.012(2) 0.005(3) -0.011(3)
C46 0.025(3) 0.018(3) 0.036(4) -0.009(3) 0.011(3) -0.006(3)
C47 0.019(3) 0.026(3) 0.023(3) -0.011(2) -0.003(2) -0.004(3)
C48 0.015(3) 0.028(3) 0.041(4) -0.016(3) 0.009(3) -0.009(3)
_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 C43 2.274(5) . ?
Ru1 P2 2.2771(14) . ?
Ru1 C42 2.278(6) . ?
Ru1 C40 2.291(5) . ?
Ru1 C39 2.294(5) . ?
Ru1 C41 2.298(5) . ?
Ru1 P1 2.3307(14) . ?
Ru1 P3 2.3757(13) . ?
P1 C2 1.816(6) . ?
P1 C3 1.841(6) . ?
P1 C9 1.852(5) . ?
P2 C1 1.802(6) . ?
P2 C21 1.839(6) . ?
P2 C15 1.863(5) . ?
P3 C33 1.853(6) . ?
P3 C27 1.855(6) . ?
P3 S1 2.0235(19) . ?
C1 C2 1.319(8) . ?
C1 H1A 0.9500 . ?
C2 H2A 0.9500 . ?
C3 C8 1.392(8) . ?
C3 C4 1.405(8) . ?
C4 C5 1.382(9) . ?
C4 H4A 0.9500 . ?
C5 C6 1.375(9) . ?
C5 H5A 0.9500 . ?
C6 C7 1.384(9) . ?
C6 H6A 0.9500 . ?
C7 C8 1.398(9) . ?
C7 H7A 0.9500 . ?
C8 H8A 0.9500 . ?
C9 C10 1.384(8) . ?
C9 C14 1.394(8) . ?
C10 C11 1.389(8) . ?
C10 H10A 0.9500 . ?
C11 C12 1.378(10) . ?
C11 H11A 0.9500 . ?
C12 C13 1.394(10) . ?
C12 H12A 0.9500 . ?
C13 C14 1.382(9) . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?
C15 C16 1.390(8) . ?
C15 C20 1.394(8) . ?
C16 C17 1.389(8) . ?
C16 H16A 0.9500 . ?
C17 C18 1.394(9) . ?
C17 H17A 0.9500 . ?
C18 C19 1.391(10) . ?
C18 H18A 0.9500 . ?
C19 C20 1.363(8) . ?
C19 H19A 0.9500 . ?
C20 H20A 0.9500 . ?
C21 C22 1.380(9) . ?
C21 C26 1.398(8) . ?
C22 C23 1.391(8) . ?
C22 H22A 0.9500 . ?
C23 C24 1.374(10) . ?
C23 H23A 0.9500 . ?
C24 C25 1.391(9) . ?
C24 H24A 0.9500 . ?
C25 C26 1.376(8) . ?
C25 H25A 0.9500 . ?
C26 H26A 0.9500 . ?
C27 C28 1.384(8) . ?
C27 C32 1.397(8) . ?
C28 C29 1.385(8) . ?
C28 H28A 0.9500 . ?
C29 C30 1.373(9) . ?
C29 H29A 0.9500 . ?
C30 C31 1.379(9) . ?
C30 H30A 0.9500 . ?
C31 C32 1.380(8) . ?
C31 H31A 0.9500 . ?
C32 H32A 0.9500 . ?
C33 C38 1.392(8) . ?
C33 C34 1.401(8) . ?
C34 C35 1.380(8) . ?
C34 H34A 0.9500 . ?
C35 C36 1.397(9) . ?
C35 H35A 0.9500 . ?
C36 C37 1.366(9) . ?
C36 H36A 0.9500 . ?
C37 C38 1.373(8) . ?
C37 H37A 0.9500 . ?
C38 H38A 0.9500 . ?
C39 C40 1.429(8) . ?
C39 C43 1.430(8) . ?
C39 C44 1.508(8) . ?
C40 C41 1.427(8) . ?
C40 C45 1.505(8) . ?
C41 C42 1.436(8) . ?
C41 C46 1.499(7) . ?
C42 C43 1.434(7) . ?
C42 C47 1.483(8) . ?
C43 C48 1.496(8) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
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
C43 Ru1 P2 110.73(14) . . ?
C43 Ru1 C42 36.72(19) . . ?
P2 Ru1 C42 94.62(14) . . ?
C43 Ru1 C40 61.07(19) . . ?
P2 Ru1 C40 149.61(14) . . ?
C42 Ru1 C40 60.8(2) . . ?
C43 Ru1 C39 36.5(2) . . ?
P2 Ru1 C39 147.03(16) . . ?
C42 Ru1 C39 60.6(2) . . ?
C40 Ru1 C39 36.32(19) . . ?
C43 Ru1 C41 61.14(18) . . ?
P2 Ru1 C41 113.39(14) . . ?
C42 Ru1 C41 36.56(19) . . ?
C40 Ru1 C41 36.22(19) . . ?
C39 Ru1 C41 60.46(19) . . ?
C43 Ru1 P1 163.02(14) . . ?
P2 Ru1 P1 81.93(5) . . ?
C42 Ru1 P1 134.49(14) . . ?
C40 Ru1 P1 102.23(14) . . ?
C39 Ru1 P1 130.74(15) . . ?
C41 Ru1 P1 103.96(14) . . ?
C43 Ru1 P3 101.21(14) . . ?
P2 Ru1 P3 89.37(5) . . ?
C42 Ru1 P3 135.60(14) . . ?
C40 Ru1 P3 120.47(14) . . ?
C39 Ru1 P3 94.30(14) . . ?
C41 Ru1 P3 154.54(14) . . ?
P1 Ru1 P3 89.87(5) . . ?
C2 P1 C3 99.7(3) . . ?
C2 P1 C9 100.6(2) . . ?
C3 P1 C9 98.6(2) . . ?
C2 P1 Ru1 107.95(19) . . ?
C3 P1 Ru1 125.86(16) . . ?
C9 P1 Ru1 119.86(19) . . ?
C1 P2 C21 104.2(3) . . ?
C1 P2 C15 97.2(2) . . ?
C21 P2 C15 99.9(3) . . ?
C1 P2 Ru1 110.51(19) . . ?
C21 P2 Ru1 123.93(18) . . ?
C15 P2 Ru1 117.23(18) . . ?
C33 P3 C27 99.4(2) . . ?
C33 P3 S1 104.84(19) . . ?
C27 P3 S1 101.56(19) . . ?
C33 P3 Ru1 113.89(18) . . ?
C27 P3 Ru1 113.47(19) . . ?
S1 P3 Ru1 120.88(7) . . ?
C2 C1 P2 117.1(4) . . ?
C2 C1 H1A 121.5 . . ?
P2 C1 H1A 121.5 . . ?
C1 C2 P1 119.0(4) . . ?
C1 C2 H2A 120.5 . . ?
P1 C2 H2A 120.5 . . ?
C8 C3 C4 118.8(5) . . ?
C8 C3 P1 118.2(4) . . ?
C4 C3 P1 122.9(4) . . ?
C5 C4 C3 119.5(6) . . ?
C5 C4 H4A 120.2 . . ?
C3 C4 H4A 120.2 . . ?
C6 C5 C4 121.6(6) . . ?
C6 C5 H5A 119.2 . . ?
C4 C5 H5A 119.2 . . ?
C5 C6 C7 119.6(6) . . ?
C5 C6 H6A 120.2 . . ?
C7 C6 H6A 120.2 . . ?
C6 C7 C8 119.8(6) . . ?
C6 C7 H7A 120.1 . . ?
C8 C7 H7A 120.1 . . ?
C3 C8 C7 120.7(5) . . ?
C3 C8 H8A 119.7 . . ?
C7 C8 H8A 119.7 . . ?
C10 C9 C14 118.1(5) . . ?
C10 C9 P1 121.3(4) . . ?
C14 C9 P1 120.5(4) . . ?
C9 C10 C11 121.7(6) . . ?
C9 C10 H10A 119.2 . . ?
C11 C10 H10A 119.2 . . ?
C12 C11 C10 120.0(6) . . ?
C12 C11 H11A 120.0 . . ?
C10 C11 H11A 120.0 . . ?
C11 C12 C13 118.9(6) . . ?
C11 C12 H12A 120.6 . . ?
C13 C12 H12A 120.6 . . ?
C14 C13 C12 121.0(6) . . ?
C14 C13 H13A 119.5 . . ?
C12 C13 H13A 119.5 . . ?
C13 C14 C9 120.4(6) . . ?
C13 C14 H14A 119.8 . . ?
C9 C14 H14A 119.8 . . ?
C16 C15 C20 118.1(5) . . ?
C16 C15 P2 124.3(4) . . ?
C20 C15 P2 117.4(4) . . ?
C17 C16 C15 121.2(6) . . ?
C17 C16 H16A 119.4 . . ?
C15 C16 H16A 119.4 . . ?
C16 C17 C18 119.4(6) . . ?
C16 C17 H17A 120.3 . . ?
C18 C17 H17A 120.3 . . ?
C19 C18 C17 119.4(6) . . ?
C19 C18 H18A 120.3 . . ?
C17 C18 H18A 120.3 . . ?
C20 C19 C18 120.4(6) . . ?
C20 C19 H19A 119.8 . . ?
C18 C19 H19A 119.8 . . ?
C19 C20 C15 121.4(6) . . ?
C19 C20 H20A 119.3 . . ?
C15 C20 H20A 119.3 . . ?
C22 C21 C26 118.8(5) . . ?
C22 C21 P2 117.9(4) . . ?
C26 C21 P2 123.3(5) . . ?
C21 C22 C23 120.4(6) . . ?
C21 C22 H22A 119.8 . . ?
C23 C22 H22A 119.8 . . ?
C24 C23 C22 120.6(6) . . ?
C24 C23 H23A 119.7 . . ?
C22 C23 H23A 119.7 . . ?
C23 C24 C25 119.3(5) . . ?
C23 C24 H24A 120.4 . . ?
C25 C24 H24A 120.4 . . ?
C26 C25 C24 120.4(6) . . ?
C26 C25 H25A 119.8 . . ?
C24 C25 H25A 119.8 . . ?
C25 C26 C21 120.5(6) . . ?
C25 C26 H26A 119.8 . . ?
C21 C26 H26A 119.8 . . ?
C28 C27 C32 117.7(5) . . ?
C28 C27 P3 118.2(4) . . ?
C32 C27 P3 124.0(4) . . ?
C27 C28 C29 121.1(5) . . ?
C27 C28 H28A 119.5 . . ?
C29 C28 H28A 119.5 . . ?
C30 C29 C28 120.7(6) . . ?
C30 C29 H29A 119.7 . . ?
C28 C29 H29A 119.7 . . ?
C29 C30 C31 119.0(5) . . ?
C29 C30 H30A 120.5 . . ?
C31 C30 H30A 120.5 . . ?
C30 C31 C32 120.5(6) . . ?
C30 C31 H31A 119.7 . . ?
C32 C31 H31A 119.7 . . ?
C31 C32 C27 120.9(6) . . ?
C31 C32 H32A 119.5 . . ?
C27 C32 H32A 119.5 . . ?
C38 C33 C34 118.5(6) . . ?
C38 C33 P3 122.6(4) . . ?
C34 C33 P3 118.8(4) . . ?
C35 C34 C33 120.3(5) . . ?
C35 C34 H34A 119.9 . . ?
C33 C34 H34A 119.9 . . ?
C34 C35 C36 120.3(5) . . ?
C34 C35 H35A 119.9 . . ?
C36 C35 H35A 119.9 . . ?
C37 C36 C35 119.1(5) . . ?
C37 C36 H36A 120.5 . . ?
C35 C36 H36A 120.5 . . ?
C36 C37 C38 121.5(5) . . ?
C36 C37 H37A 119.3 . . ?
C38 C37 H37A 119.3 . . ?
C37 C38 C33 120.4(5) . . ?
C37 C38 H38A 119.8 . . ?
C33 C38 H38A 119.8 . . ?
C40 C39 C43 108.4(5) . . ?
C40 C39 C44 124.0(5) . . ?
C43 C39 C44 125.9(5) . . ?
C40 C39 Ru1 71.7(3) . . ?
C43 C39 Ru1 71.0(3) . . ?
C44 C39 Ru1 134.7(4) . . ?
C41 C40 C39 108.1(5) . . ?
C41 C40 C45 126.1(5) . . ?
C39 C40 C45 123.8(5) . . ?
C41 C40 Ru1 72.2(3) . . ?
C39 C40 Ru1 72.0(3) . . ?
C45 C40 Ru1 134.4(4) . . ?
C40 C41 C42 107.7(4) . . ?
C40 C41 C46 126.8(5) . . ?
C42 C41 C46 124.0(5) . . ?
C40 C41 Ru1 71.6(3) . . ?
C42 C41 Ru1 71.0(3) . . ?
C46 C41 Ru1 133.7(4) . . ?
C43 C42 C41 108.3(5) . . ?
C43 C42 C47 124.5(5) . . ?
C41 C42 C47 125.5(5) . . ?
C43 C42 Ru1 71.5(3) . . ?
C41 C42 Ru1 72.5(3) . . ?
C47 C42 Ru1 133.8(4) . . ?
C39 C43 C42 107.4(5) . . ?
C39 C43 C48 124.9(5) . . ?
C42 C43 C48 125.9(5) . . ?
C39 C43 Ru1 72.5(3) . . ?
C42 C43 Ru1 71.8(3) . . ?
C48 C43 Ru1 132.9(4) . . ?
C39 C44 H44A 109.5 . . ?
C39 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C39 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C40 C45 H45A 109.5 . . ?
C40 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C40 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C41 C46 H46A 109.5 . . ?
C41 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C41 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C42 C47 H47A 109.5 . . ?
C42 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C42 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C43 C48 H48A 109.5 . . ?
C43 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C43 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
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
C43 Ru1 P1 C2 154.5(5) . . . . ?
P2 Ru1 P1 C2 15.01(19) . . . . ?
C42 Ru1 P1 C2 103.6(3) . . . . ?
C40 Ru1 P1 C2 164.4(2) . . . . ?
C39 Ru1 P1 C2 -169.9(3) . . . . ?
C41 Ru1 P1 C2 127.2(2) . . . . ?
P3 Ru1 P1 C2 -74.37(19) . . . . ?
C43 Ru1 P1 C3 -88.6(5) . . . . ?
P2 Ru1 P1 C3 132.0(2) . . . . ?
C42 Ru1 P1 C3 -139.5(3) . . . . ?
C40 Ru1 P1 C3 -78.6(3) . . . . ?
C39 Ru1 P1 C3 -53.0(3) . . . . ?
C41 Ru1 P1 C3 -115.8(3) . . . . ?
P3 Ru1 P1 C3 42.6(2) . . . . ?
C43 Ru1 P1 C9 40.4(5) . . . . ?
P2 Ru1 P1 C9 -99.1(2) . . . . ?
C42 Ru1 P1 C9 -10.6(3) . . . . ?
C40 Ru1 P1 C9 50.3(2) . . . . ?
C39 Ru1 P1 C9 75.9(3) . . . . ?
C41 Ru1 P1 C9 13.1(3) . . . . ?
P3 Ru1 P1 C9 171.5(2) . . . . ?
C43 Ru1 P2 C1 175.4(2) . . . . ?
C42 Ru1 P2 C1 -150.7(2) . . . . ?
C40 Ru1 P2 C1 -116.8(3) . . . . ?
C39 Ru1 P2 C1 170.5(3) . . . . ?
C41 Ru1 P2 C1 -118.1(2) . . . . ?
P1 Ru1 P2 C1 -16.35(18) . . . . ?
P3 Ru1 P2 C1 73.61(19) . . . . ?
C43 Ru1 P2 C21 50.7(3) . . . . ?
C42 Ru1 P2 C21 84.7(3) . . . . ?
C40 Ru1 P2 C21 118.6(4) . . . . ?
C39 Ru1 P2 C21 45.9(4) . . . . ?
C41 Ru1 P2 C21 117.3(3) . . . . ?
P1 Ru1 P2 C21 -141.0(2) . . . . ?
P3 Ru1 P2 C21 -51.0(2) . . . . ?
C43 Ru1 P2 C15 -74.6(2) . . . . ?
C42 Ru1 P2 C15 -40.6(2) . . . . ?
C40 Ru1 P2 C15 -6.8(3) . . . . ?
C39 Ru1 P2 C15 -79.4(3) . . . . ?
C41 Ru1 P2 C15 -8.1(3) . . . . ?
P1 Ru1 P2 C15 93.7(2) . . . . ?
P3 Ru1 P2 C15 -176.4(2) . . . . ?
C43 Ru1 P3 C33 97.5(2) . . . . ?
P2 Ru1 P3 C33 -151.52(19) . . . . ?
C42 Ru1 P3 C33 112.5(3) . . . . ?
C40 Ru1 P3 C33 34.6(2) . . . . ?
C39 Ru1 P3 C33 61.3(2) . . . . ?
C41 Ru1 P3 C33 54.2(4) . . . . ?
P1 Ru1 P3 C33 -69.58(19) . . . . ?
C43 Ru1 P3 C27 -15.4(2) . . . . ?
P2 Ru1 P3 C27 95.7(2) . . . . ?
C42 Ru1 P3 C27 -0.3(3) . . . . ?
C40 Ru1 P3 C27 -78.3(3) . . . . ?
C39 Ru1 P3 C27 -51.5(3) . . . . ?
C41 Ru1 P3 C27 -58.6(4) . . . . ?
P1 Ru1 P3 C27 177.6(2) . . . . ?
C43 Ru1 P3 S1 -136.30(16) . . . . ?
P2 Ru1 P3 S1 -25.27(9) . . . . ?
C42 Ru1 P3 S1 -121.2(2) . . . . ?
C40 Ru1 P3 S1 160.81(17) . . . . ?
C39 Ru1 P3 S1 -172.48(17) . . . . ?
C41 Ru1 P3 S1 -179.5(3) . . . . ?
P1 Ru1 P3 S1 56.66(9) . . . . ?
C21 P2 C1 C2 150.5(4) . . . . ?
C15 P2 C1 C2 -107.3(5) . . . . ?
Ru1 P2 C1 C2 15.3(5) . . . . ?
P2 C1 C2 P1 -2.2(6) . . . . ?
C3 P1 C2 C1 -144.3(4) . . . . ?
C9 P1 C2 C1 115.0(5) . . . . ?
Ru1 P1 C2 C1 -11.4(5) . . . . ?
C2 P1 C3 C8 42.4(4) . . . . ?
C9 P1 C3 C8 144.8(4) . . . . ?
Ru1 P1 C3 C8 -78.2(5) . . . . ?
C2 P1 C3 C4 -140.5(4) . . . . ?
C9 P1 C3 C4 -38.2(5) . . . . ?
Ru1 P1 C3 C4 98.8(4) . . . . ?
C8 C3 C4 C5 -1.3(8) . . . . ?
P1 C3 C4 C5 -178.3(4) . . . . ?
C3 C4 C5 C6 1.3(9) . . . . ?
C4 C5 C6 C7 -0.5(9) . . . . ?
C5 C6 C7 C8 -0.3(9) . . . . ?
C4 C3 C8 C7 0.5(8) . . . . ?
P1 C3 C8 C7 177.6(4) . . . . ?
C6 C7 C8 C3 0.3(9) . . . . ?
C2 P1 C9 C10 177.3(5) . . . . ?
C3 P1 C9 C10 75.6(5) . . . . ?
Ru1 P1 C9 C10 -64.7(5) . . . . ?
C2 P1 C9 C14 -1.2(6) . . . . ?
C3 P1 C9 C14 -102.9(5) . . . . ?
Ru1 P1 C9 C14 116.7(5) . . . . ?
C14 C9 C10 C11 1.0(9) . . . . ?
P1 C9 C10 C11 -177.6(5) . . . . ?
C9 C10 C11 C12 -1.1(10) . . . . ?
C10 C11 C12 C13 0.0(10) . . . . ?
C11 C12 C13 C14 1.1(11) . . . . ?
C12 C13 C14 C9 -1.2(11) . . . . ?
C10 C9 C14 C13 0.1(9) . . . . ?
P1 C9 C14 C13 178.7(5) . . . . ?
C1 P2 C15 C16 -101.0(5) . . . . ?
C21 P2 C15 C16 4.9(6) . . . . ?
Ru1 P2 C15 C16 141.5(4) . . . . ?
C1 P2 C15 C20 73.0(5) . . . . ?
C21 P2 C15 C20 178.8(5) . . . . ?
Ru1 P2 C15 C20 -44.6(5) . . . . ?
C20 C15 C16 C17 -0.3(9) . . . . ?
P2 C15 C16 C17 173.6(5) . . . . ?
C15 C16 C17 C18 0.2(10) . . . . ?
C16 C17 C18 C19 0.4(10) . . . . ?
C17 C18 C19 C20 -1.0(10) . . . . ?
C18 C19 C20 C15 0.9(10) . . . . ?
C16 C15 C20 C19 -0.3(9) . . . . ?
P2 C15 C20 C19 -174.6(5) . . . . ?
C1 P2 C21 C22 173.1(4) . . . . ?
C15 P2 C21 C22 73.0(5) . . . . ?
Ru1 P2 C21 C22 -59.5(5) . . . . ?
C1 P2 C21 C26 -8.8(5) . . . . ?
C15 P2 C21 C26 -108.9(5) . . . . ?
Ru1 P2 C21 C26 118.5(4) . . . . ?
C26 C21 C22 C23 0.0(8) . . . . ?
P2 C21 C22 C23 178.1(4) . . . . ?
C21 C22 C23 C24 -1.0(9) . . . . ?
C22 C23 C24 C25 0.5(9) . . . . ?
C23 C24 C25 C26 1.1(9) . . . . ?
C24 C25 C26 C21 -2.1(8) . . . . ?
C22 C21 C26 C25 1.6(8) . . . . ?
P2 C21 C26 C25 -176.5(4) . . . . ?
C33 P3 C27 C28 157.0(5) . . . . ?
S1 P3 C27 C28 49.6(5) . . . . ?
Ru1 P3 C27 C28 -81.7(5) . . . . ?
C33 P3 C27 C32 -19.7(6) . . . . ?
S1 P3 C27 C32 -127.1(5) . . . . ?
Ru1 P3 C27 C32 101.6(5) . . . . ?
C32 C27 C28 C29 -2.2(9) . . . . ?
P3 C27 C28 C29 -179.1(5) . . . . ?
C27 C28 C29 C30 2.1(9) . . . . ?
C28 C29 C30 C31 0.2(10) . . . . ?
C29 C30 C31 C32 -2.5(10) . . . . ?
C30 C31 C32 C27 2.4(10) . . . . ?
C28 C27 C32 C31 -0.1(9) . . . . ?
P3 C27 C32 C31 176.6(5) . . . . ?
C27 P3 C33 C38 122.0(5) . . . . ?
S1 P3 C33 C38 -133.3(4) . . . . ?
Ru1 P3 C33 C38 1.0(5) . . . . ?
C27 P3 C33 C34 -60.7(5) . . . . ?
S1 P3 C33 C34 44.0(5) . . . . ?
Ru1 P3 C33 C34 178.3(4) . . . . ?
C38 C33 C34 C35 -0.5(8) . . . . ?
P3 C33 C34 C35 -178.0(4) . . . . ?
C33 C34 C35 C36 0.5(9) . . . . ?
C34 C35 C36 C37 0.3(9) . . . . ?
C35 C36 C37 C38 -1.0(9) . . . . ?
C36 C37 C38 C33 1.0(9) . . . . ?
C34 C33 C38 C37 -0.2(8) . . . . ?
P3 C33 C38 C37 177.2(4) . . . . ?
C43 Ru1 C39 C40 117.8(5) . . . . ?
P2 Ru1 C39 C40 125.4(3) . . . . ?
C42 Ru1 C39 C40 79.6(4) . . . . ?
C41 Ru1 C39 C40 37.4(3) . . . . ?
P1 Ru1 C39 C40 -45.6(4) . . . . ?
P3 Ru1 C39 C40 -139.1(3) . . . . ?
P2 Ru1 C39 C43 7.6(5) . . . . ?
C42 Ru1 C39 C43 -38.2(3) . . . . ?
C40 Ru1 C39 C43 -117.8(5) . . . . ?
C41 Ru1 C39 C43 -80.4(3) . . . . ?
P1 Ru1 C39 C43 -163.4(2) . . . . ?
P3 Ru1 C39 C43 103.1(3) . . . . ?
C43 Ru1 C39 C44 -122.1(7) . . . . ?
P2 Ru1 C39 C44 -114.6(5) . . . . ?
C42 Ru1 C39 C44 -160.3(6) . . . . ?
C40 Ru1 C39 C44 120.1(7) . . . . ?
C41 Ru1 C39 C44 157.5(6) . . . . ?
P1 Ru1 C39 C44 74.5(6) . . . . ?
P3 Ru1 C39 C44 -19.1(6) . . . . ?
C43 C39 C40 C41 -1.7(6) . . . . ?
C44 C39 C40 C41 164.3(5) . . . . ?
Ru1 C39 C40 C41 -63.6(4) . . . . ?
C43 C39 C40 C45 -166.2(5) . . . . ?
C44 C39 C40 C45 -0.3(9) . . . . ?
Ru1 C39 C40 C45 131.9(5) . . . . ?
C43 C39 C40 Ru1 61.9(4) . . . . ?
C44 C39 C40 Ru1 -132.2(6) . . . . ?
C43 Ru1 C40 C41 79.7(3) . . . . ?
P2 Ru1 C40 C41 -2.1(5) . . . . ?
C42 Ru1 C40 C41 37.5(3) . . . . ?
C39 Ru1 C40 C41 116.6(5) . . . . ?
P1 Ru1 C40 C41 -97.0(3) . . . . ?
P3 Ru1 C40 C41 165.8(2) . . . . ?
C43 Ru1 C40 C39 -36.9(3) . . . . ?
P2 Ru1 C40 C39 -118.7(3) . . . . ?
C42 Ru1 C40 C39 -79.2(4) . . . . ?
C41 Ru1 C40 C39 -116.6(5) . . . . ?
P1 Ru1 C40 C39 146.4(3) . . . . ?
P3 Ru1 C40 C39 49.2(4) . . . . ?
C43 Ru1 C40 C45 -156.9(6) . . . . ?
P2 Ru1 C40 C45 121.3(5) . . . . ?
C42 Ru1 C40 C45 160.9(6) . . . . ?
C39 Ru1 C40 C45 -120.0(7) . . . . ?
C41 Ru1 C40 C45 123.4(6) . . . . ?
P1 Ru1 C40 C45 26.4(5) . . . . ?
P3 Ru1 C40 C45 -70.8(5) . . . . ?
C39 C40 C41 C42 1.3(6) . . . . ?
C45 C40 C41 C42 165.4(5) . . . . ?
Ru1 C40 C41 C42 -62.2(4) . . . . ?
C39 C40 C41 C46 -165.2(5) . . . . ?
C45 C40 C41 C46 -1.1(9) . . . . ?
Ru1 C40 C41 C46 131.4(6) . . . . ?
C39 C40 C41 Ru1 63.4(4) . . . . ?
C45 C40 C41 Ru1 -132.5(5) . . . . ?
C43 Ru1 C41 C40 -79.5(3) . . . . ?
P2 Ru1 C41 C40 178.9(3) . . . . ?
C42 Ru1 C41 C40 -117.0(4) . . . . ?
C39 Ru1 C41 C40 -37.5(3) . . . . ?
P1 Ru1 C41 C40 91.7(3) . . . . ?
P3 Ru1 C41 C40 -29.4(5) . . . . ?
C43 Ru1 C41 C42 37.5(3) . . . . ?
P2 Ru1 C41 C42 -64.2(3) . . . . ?
C40 Ru1 C41 C42 117.0(4) . . . . ?
C39 Ru1 C41 C42 79.5(3) . . . . ?
P1 Ru1 C41 C42 -151.3(3) . . . . ?
P3 Ru1 C41 C42 87.6(4) . . . . ?
C43 Ru1 C41 C46 156.8(6) . . . . ?
P2 Ru1 C41 C46 55.1(6) . . . . ?
C42 Ru1 C41 C46 119.3(7) . . . . ?
C40 Ru1 C41 C46 -123.7(7) . . . . ?
C39 Ru1 C41 C46 -161.2(6) . . . . ?
P1 Ru1 C41 C46 -32.0(6) . . . . ?
P3 Ru1 C41 C46 -153.1(4) . . . . ?
C40 C41 C42 C43 -0.4(6) . . . . ?
C46 C41 C42 C43 166.6(5) . . . . ?
Ru1 C41 C42 C43 -62.9(4) . . . . ?
C40 C41 C42 C47 -165.6(5) . . . . ?
C46 C41 C42 C47 1.3(9) . . . . ?
Ru1 C41 C42 C47 131.8(6) . . . . ?
C40 C41 C42 Ru1 62.6(4) . . . . ?
C46 C41 C42 Ru1 -130.5(5) . . . . ?
P2 Ru1 C42 C43 -119.1(3) . . . . ?
C40 Ru1 C42 C43 79.8(3) . . . . ?
C39 Ru1 C42 C43 37.9(3) . . . . ?
C41 Ru1 C42 C43 116.9(5) . . . . ?
P1 Ru1 C42 C43 157.7(2) . . . . ?
P3 Ru1 C42 C43 -25.2(4) . . . . ?
C43 Ru1 C42 C41 -116.9(5) . . . . ?
P2 Ru1 C42 C41 124.0(3) . . . . ?
C40 Ru1 C42 C41 -37.1(3) . . . . ?
C39 Ru1 C42 C41 -79.0(3) . . . . ?
P1 Ru1 C42 C41 40.8(4) . . . . ?
P3 Ru1 C42 C41 -142.1(3) . . . . ?
C43 Ru1 C42 C47 120.4(7) . . . . ?
P2 Ru1 C42 C47 1.3(5) . . . . ?
C40 Ru1 C42 C47 -159.8(6) . . . . ?
C39 Ru1 C42 C47 158.3(6) . . . . ?
C41 Ru1 C42 C47 -122.7(7) . . . . ?
P1 Ru1 C42 C47 -81.9(6) . . . . ?
P3 Ru1 C42 C47 95.1(5) . . . . ?
C40 C39 C43 C42 1.5(6) . . . . ?
C44 C39 C43 C42 -164.2(5) . . . . ?
Ru1 C39 C43 C42 63.8(4) . . . . ?
C40 C39 C43 C48 167.0(5) . . . . ?
C44 C39 C43 C48 1.4(9) . . . . ?
Ru1 C39 C43 C48 -130.6(5) . . . . ?
C40 C39 C43 Ru1 -62.3(4) . . . . ?
C44 C39 C43 Ru1 132.0(6) . . . . ?
C41 C42 C43 C39 -0.7(6) . . . . ?
C47 C42 C43 C39 164.8(5) . . . . ?
Ru1 C42 C43 C39 -64.3(4) . . . . ?
C41 C42 C43 C48 -166.1(5) . . . . ?
C47 C42 C43 C48 -0.6(9) . . . . ?
Ru1 C42 C43 C48 130.3(5) . . . . ?
C41 C42 C43 Ru1 63.6(4) . . . . ?
C47 C42 C43 Ru1 -131.0(6) . . . . ?
P2 Ru1 C43 C39 -175.6(3) . . . . ?
C42 Ru1 C43 C39 115.7(4) . . . . ?
C40 Ru1 C43 C39 36.8(3) . . . . ?
C41 Ru1 C43 C39 78.4(3) . . . . ?
P1 Ru1 C43 C39 47.9(6) . . . . ?
P3 Ru1 C43 C39 -82.0(3) . . . . ?
P2 Ru1 C43 C42 68.7(3) . . . . ?
C40 Ru1 C43 C42 -78.9(3) . . . . ?
C39 Ru1 C43 C42 -115.7(4) . . . . ?
C41 Ru1 C43 C42 -37.3(3) . . . . ?
P1 Ru1 C43 C42 -67.8(6) . . . . ?
P3 Ru1 C43 C42 162.3(3) . . . . ?
P2 Ru1 C43 C48 -53.8(5) . . . . ?
C42 Ru1 C43 C48 -122.5(7) . . . . ?
C40 Ru1 C43 C48 158.5(6) . . . . ?
C39 Ru1 C43 C48 121.8(7) . . . . ?
C41 Ru1 C43 C48 -159.9(6) . . . . ?
P1 Ru1 C43 C48 169.6(4) . . . . ?
P3 Ru1 C43 C48 39.8(5) . . . . ?
_diffrn_measured_fraction_theta_max 0.951
_diffrn_reflns_theta_full 66.74
_diffrn_measured_fraction_theta_full 0.951
_refine_diff_density_max 1.274
_refine_diff_density_min -2.671
_refine_diff_density_rms 0.144
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.327 0.865 0.871 138 26 ' '
2 0.675 0.136 0.130 138 26 ' '
_platon_squeeze_details
;
During the
refinement of the structure, electron density peaks were located
that were believed to be highly disordered
solvent molecules (possibly THF). Attempts
made to model the solvent molecule were not successful.
The SQUEEZE option in PLATON (Spek, 2003) indicated there was a
large solvent cavity (279.2\%A^3^). In the final cycles of refinement,
this contribution (52 electrons) 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. (2009). Acta Cryst. D65, 148--155.
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.
;
_vrf_PLAT029_5
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.951
RESPONSE: Data were collected using CuKalpha
radiation using a Bruker Microsource system eqipped with
multi layer optics. Without this type of instrumentation we would
not have been able to collect sufficient data to aquire a
crystal structure. We feel that the precision of the structure
is good enough to support any claims made regadring the
geometry of the molecule and the intermolecular distances.
;
# end Validation Reply Form
_iucr_refine_instructions_details
;
TITL cu_d12276_0m in P-1
CELL 1.54178 10.6911 12.0014 19.0065 73.029 88.592 70.042
ZERR 2.00 0.0004 0.0005 0.0008 0.003 0.003 0.003
LATT 1
SFAC C H P S RU
UNIT 96 94 6 2 2
TEMP -126.150
SIZE 0.020 0.020 0.030
ACTA
OMIT 5 1 17
OMIT 4 3 20
OMIT 5 3 19
L.S. 4
FMAP 2
DELU 0.005 C34 C35
PLAN 20
HTAB
BOND $H
CONF
WGHT 0.105600
FVAR 1.01231
RU1 5 0.216644 0.455218 0.266849 11.00000 0.01449 0.01147 =
0.01729 -0.00544 0.00417 -0.00433
P1 3 0.009176 0.431584 0.266414 11.00000 0.01478 0.01441 =
0.02033 -0.00628 0.00479 -0.00654
P2 3 0.164704 0.473227 0.380886 11.00000 0.01759 0.01302 =
0.01881 -0.00484 0.00460 -0.00474
P3 3 0.111267 0.673818 0.215766 11.00000 0.01793 0.01173 =
0.02042 -0.00574 0.00415 -0.00557
S1 4 -0.034092 0.771727 0.267069 11.00000 0.02256 0.01721 =
0.02467 -0.00895 0.00437 -0.00524
C1 1 -0.010984 0.503503 0.390225 11.00000 0.02925 0.01464 =
0.01599 -0.00493 0.00322 -0.00778
AFIX 43
H1A 2 -0.053674 0.533104 0.428975 11.00000 -1.20000
AFIX 0
C2 1 -0.077749 0.482769 0.340901 11.00000 0.01642 0.01565 =
0.03179 -0.01053 0.01336 -0.00774
AFIX 43
H2A 2 -0.169908 0.494437 0.344296 11.00000 -1.20000
AFIX 0
C3 1 -0.125272 0.513236 0.191263 11.00000 0.01286 0.02155 =
0.02601 -0.00950 0.00835 -0.01226
C4 1 -0.147914 0.459158 0.138745 11.00000 0.02243 0.02116 =
0.01916 -0.00806 0.00006 -0.00797
AFIX 43
H4A 2 -0.094354 0.376167 0.141719 11.00000 -1.20000
AFIX 0
C5 1 -0.248676 0.527548 0.082706 11.00000 0.02818 0.03602 =
0.02621 -0.01299 -0.00077 -0.01300
AFIX 43
H5A 2 -0.264801 0.489957 0.047943 11.00000 -1.20000
AFIX 0
C6 1 -0.326137 0.648674 0.076060 11.00000 0.01889 0.03202 =
0.02276 0.00410 -0.00638 -0.00667
AFIX 43
H6A 2 -0.394401 0.694209 0.036888 11.00000 -1.20000
AFIX 0
C7 1 -0.303972 0.703801 0.126830 11.00000 0.02127 0.02622 =
0.04216 -0.01101 0.00658 -0.00735
AFIX 43
H7A 2 -0.356721 0.787576 0.122490 11.00000 -1.20000
AFIX 0
C8 1 -0.203739 0.635848 0.184514 11.00000 0.02315 0.02231 =
0.02407 -0.00940 0.00461 -0.01049
AFIX 43
H8A 2 -0.189030 0.673725 0.219453 11.00000 -1.20000
AFIX 0
C9 1 -0.000421 0.274012 0.288337 11.00000 0.01819 0.01694 =
0.02055 -0.00640 -0.00215 -0.00545
C10 1 0.049672 0.199631 0.243236 11.00000 0.01958 0.01977 =
0.03545 -0.00634 0.00099 -0.00327
AFIX 43
H10A 2 0.092849 0.228941 0.201250 11.00000 -1.20000
AFIX 0
C11 1 0.038435 0.083286 0.257781 11.00000 0.02531 0.01677 =
0.04791 -0.01545 -0.00790 0.00138
AFIX 43
H11A 2 0.072356 0.034663 0.225487 11.00000 -1.20000
AFIX 0
C12 1 -0.021937 0.038410 0.319076 11.00000 0.04645 0.01979 =
0.04454 -0.00498 -0.00604 -0.01626
AFIX 43
H12A 2 -0.030082 -0.041078 0.329473 11.00000 -1.20000
AFIX 0
C13 1 -0.070864 0.111569 0.365579 11.00000 0.04757 0.03459 =
0.03796 -0.00527 0.00664 -0.02790
AFIX 43
H13A 2 -0.111253 0.080829 0.408451 11.00000 -1.20000
AFIX 0
C14 1 -0.061477 0.228192 0.350227 11.00000 0.03897 0.02201 =
0.03238 -0.00808 0.00559 -0.01378
AFIX 43
H14A 2 -0.096853 0.277401 0.382052 11.00000 -1.20000
AFIX 0
C15 1 0.227315 0.329165 0.460809 11.00000 0.01980 0.02125 =
0.00940 -0.00163 -0.00013 -0.00397
C16 1 0.274793 0.324676 0.529362 11.00000 0.01846 0.02329 =
0.02760 -0.00738 -0.00176 -0.00199
AFIX 43
H16A 2 0.284943 0.396799 0.535796 11.00000 -1.20000
AFIX 0
C17 1 0.307687 0.216644 0.588661 11.00000 0.03487 0.03234 =
0.01925 -0.00445 0.00014 -0.00584
AFIX 43
H17A 2 0.339754 0.215017 0.635257 11.00000 -1.20000
AFIX 0
C18 1 0.293241 0.110690 0.579209 11.00000 0.03696 0.02588 =
0.03218 0.00973 0.00357 -0.00736
AFIX 43
H18A 2 0.314828 0.036366 0.619384 11.00000 -1.20000
AFIX 0
C19 1 0.246953 0.114707 0.510454 11.00000 0.03278 0.02131 =
0.03023 0.00003 0.00244 -0.00882
AFIX 43
H19A 2 0.238199 0.042392 0.503496 11.00000 -1.20000
AFIX 0
C20 1 0.214061 0.221692 0.452987 11.00000 0.02929 0.02140 =
0.02192 -0.00465 0.00351 -0.00937
AFIX 43
H20A 2 0.181395 0.223066 0.406593 11.00000 -1.20000
AFIX 0
C21 1 0.201688 0.583174 0.419726 11.00000 0.02947 0.01437 =
0.02102 -0.00182 0.00752 -0.00837
C22 1 0.333424 0.573138 0.427656 11.00000 0.02582 0.02420 =
0.01740 -0.00781 -0.00557 -0.00695
AFIX 43
H22A 2 0.401571 0.509199 0.414562 11.00000 -1.20000
AFIX 0
C23 1 0.367074 0.656045 0.454700 11.00000 0.02754 0.02721 =
0.03902 -0.00668 -0.00597 -0.01259
AFIX 43
H23A 2 0.458189 0.647462 0.460667 11.00000 -1.20000
AFIX 0
C24 1 0.269637 0.750238 0.472852 11.00000 0.04531 0.02322 =
0.01819 -0.00263 -0.01561 -0.01091
AFIX 43
H24A 2 0.292883 0.807078 0.490957 11.00000 -1.20000
AFIX 0
C25 1 0.136601 0.761448 0.464429 11.00000 0.04179 0.02293 =
0.02079 -0.01741 0.00676 -0.01044
AFIX 43
H25A 2 0.068516 0.827167 0.476044 11.00000 -1.20000
AFIX 0
C26 1 0.103010 0.677924 0.439372 11.00000 0.02259 0.01792 =
0.01566 0.00172 -0.00025 -0.00261
AFIX 43
H26A 2 0.012132 0.684682 0.435394 11.00000 -1.20000
AFIX 0
C27 1 0.228926 0.759974 0.203748 11.00000 0.02344 0.01352 =
0.02609 -0.00616 0.00032 -0.00496
C28 1 0.267316 0.785906 0.264438 11.00000 0.02298 0.01947 =
0.02126 -0.00395 0.00002 -0.01164
AFIX 43
H28A 2 0.234096 0.758276 0.310647 11.00000 -1.20000
AFIX 0
C29 1 0.353354 0.851464 0.258887 11.00000 0.02712 0.02477 =
0.04800 -0.01658 0.00222 -0.01267
AFIX 43
H29A 2 0.380807 0.865773 0.301609 11.00000 -1.20000
AFIX 0
C30 1 0.399406 0.896011 0.192264 11.00000 0.02956 0.02523 =
0.04846 -0.01448 0.00587 -0.01749
AFIX 43
H30A 2 0.458680 0.940706 0.188665 11.00000 -1.20000
AFIX 0
C31 1 0.358354 0.874924 0.130637 11.00000 0.02487 0.02918 =
0.03935 -0.00711 0.00986 -0.01434
AFIX 43
H31A 2 0.386793 0.908137 0.083923 11.00000 -1.20000
AFIX 0
C32 1 0.276298 0.805967 0.136283 11.00000 0.02262 0.02019 =
0.02222 -0.00416 0.00370 -0.00759
AFIX 43
H32A 2 0.251693 0.789554 0.093683 11.00000 -1.20000
AFIX 0
C33 1 0.041239 0.723351 0.118844 11.00000 0.02124 0.01651 =
0.02902 -0.00685 0.01274 -0.00926
C34 1 -0.026409 0.850124 0.083798 11.00000 0.02323 0.01550 =
0.03247 -0.00942 0.00222 -0.00704
AFIX 43
H34A 2 -0.033092 0.908995 0.109281 11.00000 -1.20000
AFIX 0
C35 1 -0.083372 0.889822 0.012413 11.00000 0.02726 0.01795 =
0.01646 0.00764 -0.00629 -0.00378
AFIX 43
H35A 2 -0.128543 0.975973 -0.011189 11.00000 -1.20000
AFIX 0
C36 1 -0.074879 0.803817 -0.025293 11.00000 0.02993 0.03369 =
0.01980 -0.00739 0.00120 -0.01458
AFIX 43
H36A 2 -0.113602 0.830892 -0.074532 11.00000 -1.20000
AFIX 0
C37 1 -0.010135 0.680280 0.009616 11.00000 0.02965 0.03261 =
0.00964 -0.00832 -0.00233 -0.01239
AFIX 43
H37A 2 -0.005487 0.621466 -0.015590 11.00000 -1.20000
AFIX 0
C38 1 0.048363 0.639228 0.080311 11.00000 0.02231 0.01818 =
0.02680 -0.01151 0.00771 -0.01023
AFIX 43
H38A 2 0.093988 0.552887 0.103083 11.00000 -1.20000
AFIX 0
C39 1 0.374546 0.440305 0.182797 11.00000 0.01655 0.01710 =
0.03262 -0.01267 0.01127 -0.00299
C40 1 0.330135 0.337177 0.194558 11.00000 0.01185 0.01555 =
0.01972 -0.00842 0.00299 -0.00114
C41 1 0.365756 0.263023 0.269822 11.00000 0.01448 0.01505 =
0.02400 -0.00930 0.00212 -0.00354
C42 1 0.429917 0.322400 0.305036 11.00000 0.01502 0.01763 =
0.01888 -0.00337 -0.00011 0.00014
C43 1 0.434507 0.432840 0.251221 11.00000 0.00940 0.02097 =
0.01689 -0.00666 0.00715 -0.00621
C44 1 0.386537 0.521642 0.107630 11.00000 0.02776 0.02591 =
0.02368 -0.00942 0.01045 -0.01008
AFIX 137
H44A 2 0.449585 0.470808 0.081201 11.00000 -1.50000
H44B 2 0.418942 0.586011 0.113211 11.00000 -1.50000
H44C 2 0.298879 0.560980 0.079615 11.00000 -1.50000
AFIX 0
C45 1 0.289374 0.297676 0.133149 11.00000 0.02980 0.02536 =
0.02331 -0.01169 0.00497 -0.01112
AFIX 137
H45A 2 0.351404 0.302823 0.094513 11.00000 -1.50000
H45B 2 0.198746 0.352624 0.112351 11.00000 -1.50000
H45C 2 0.291437 0.211865 0.152604 11.00000 -1.50000
AFIX 0
C46 1 0.367554 0.132704 0.302955 11.00000 0.02493 0.01807 =
0.03622 -0.00855 0.01080 -0.00583
AFIX 137
H46A 2 0.442343 0.075361 0.285872 11.00000 -1.50000
H46B 2 0.283495 0.127158 0.287749 11.00000 -1.50000
H46C 2 0.377996 0.110415 0.356900 11.00000 -1.50000
AFIX 0
C47 1 0.508938 0.264198 0.377698 11.00000 0.01948 0.02598 =
0.02263 -0.01108 -0.00329 -0.00359
AFIX 137
H47A 2 0.601891 0.219893 0.370867 11.00000 -1.50000
H47B 2 0.471628 0.205432 0.409980 11.00000 -1.50000
H47C 2 0.505502 0.328818 0.400252 11.00000 -1.50000
AFIX 0
C48 1 0.517221 0.507485 0.259361 11.00000 0.01540 0.02807 =
0.04079 -0.01637 0.00856 -0.00915
AFIX 137
H48A 2 0.611046 0.462685 0.254463 11.00000 -1.50000
H48B 2 0.508454 0.520572 0.308051 11.00000 -1.50000
H48C 2 0.486362 0.588108 0.220904 11.00000 -1.50000
HKLF 4 1 1 0 0 0 1 0 0 0 1
REM cu_d12276_0m in P-1
REM R1 = 0.0556 for 5873 Fo > 4sig(Fo) and 0.0694 for all 7367 data
REM 483 parameters refined using 1 restraints
END
WGHT 0.1056 0.0000
REM Highest difference peak 1.274, deepest hole -2.671, 1-sigma level 0.144
Q1 1 0.2202 0.4370 0.3499 11.00000 0.05 1.27
Q2 1 0.2021 0.4770 0.1842 11.00000 0.05 1.12
Q3 1 0.1616 0.4631 0.3083 11.00000 0.05 1.05
Q4 1 0.1594 0.5049 0.1943 11.00000 0.05 0.98
Q5 1 0.2816 0.4632 0.2227 11.00000 0.05 0.90
Q6 1 0.1065 0.5438 0.1469 11.00000 0.05 0.73
Q7 1 0.0813 0.4697 0.2721 11.00000 0.05 0.72
Q8 1 -0.0546 0.5020 0.2056 11.00000 0.05 0.69
Q9 1 0.1990 0.4949 0.1206 11.00000 0.05 0.65
Q10 1 0.6278 1.0846 0.0993 11.00000 0.05 0.63
Q11 1 0.0239 0.4407 0.3412 11.00000 0.05 0.58
Q12 1 0.0776 0.5366 0.2666 11.00000 0.05 0.58
Q13 1 0.3024 0.4357 0.3876 11.00000 0.05 0.57
Q14 1 0.1399 0.4671 0.1474 11.00000 0.05 0.56
Q15 1 0.0354 0.7154 0.3302 11.00000 0.05 0.56
Q16 1 0.2571 0.3995 0.4038 11.00000 0.05 0.56
Q17 1 0.3066 0.3607 0.3931 11.00000 0.05 0.54
Q18 1 0.3624 0.4188 0.2644 11.00000 0.05 0.53
Q19 1 0.1813 0.5845 0.2842 11.00000 0.05 0.52
Q20 1 0.0196 0.5610 0.2186 11.00000 0.05 0.51
;
_database_code_depnum_ccdc_archive 'CCDC 951751'