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# 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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data_aks02252013_0m_compd1
_audit_creation_date 2013-02-25
_audit_creation_method
;
Olex2 1.2
(compiled Dec 5 2012 16:17:34, GUI svn.r4385)
;
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C21 H44 N P3 Ru'
_chemical_formula_sum 'C21 H44 N P3 Ru'
_chemical_formula_weight 504.55
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'
_cell_length_a 13.9737(11)
_cell_length_b 11.6625(9)
_cell_length_c 17.3011(13)
_cell_angle_alpha 90.00
_cell_angle_beta 109.7670(10)
_cell_angle_gamma 90.00
_cell_volume 2653.4(4)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 8272
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max 24.60
_cell_measurement_theta_min 2.33
_exptl_absorpt_coefficient_mu 0.778
_exptl_absorpt_correction_T_max 0.7451
_exptl_absorpt_correction_T_min 0.6640
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0630 before and 0.0543 after correction.
The Ratio of minimum to maximum transmission is 0.8912.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour red
_exptl_crystal_colour_primary red
_exptl_crystal_density_diffrn 1.263
_exptl_crystal_density_meas .
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Chunk
_exptl_crystal_F_000 1064
_exptl_crystal_size_max 0.18
_exptl_crystal_size_mid 0.113
_exptl_crystal_size_min 0.088
_exptl_special_details
;
?
;
_diffrn_reflns_av_R_equivalents 0.0522
_diffrn_reflns_av_unetI/netI 0.0427
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 20134
_diffrn_reflns_theta_full 24.62
_diffrn_reflns_theta_max 24.62
_diffrn_reflns_theta_min 2.15
_diffrn_ambient_temperature 173.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed tube'
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number 0
_reflns_number_gt 3569
_reflns_number_total 4475
_reflns_threshold_expression >2sigma(I)
_computing_cell_refinement ?
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max 0.429
_refine_diff_density_min -0.321
_refine_diff_density_rms 0.074
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.028
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 248
_refine_ls_number_reflns 4475
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0454
_refine_ls_R_factor_gt 0.0316
_refine_ls_restrained_S_all 1.028
_refine_ls_shift/su_max 0.126
_refine_ls_shift/su_mean 0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+0.8249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0686
_refine_ls_wR_factor_ref 0.0751
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
H10 of C10, H5 of C5, H4 of C4, H3 of C3, H7 of C7
At 1.5 times of:
{H13A,H13B,H13C} of C13, {H11A,H11B,H11C} of C11, {H12A,H12B,H12C} of C12,
{H9A,H9B,H9C} of C9, {H8A,H8B,H8C} of C8, {H21A,H21B,H21C} of C21, {H20A,H20B,
H20C} of C20, {H19A,H19B,H19C} of C19, {H18A,H18B,H18C} of C18, {H17A,H17B,
H17C} of C17, {H16A,H16B,H16C} of C16, {H15A,H15B,H15C} of C15, {H14A,H14B,
H14C} of C14
2.a Ternary CH refined with riding coordinates:
C7(H7), C10(H10)
2.b Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5)
2.c Idealised Me refined as rotating group:
C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,
H20B,H20C), C21(H21A,H21B,H21C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.414999(17) 0.05756(2) 0.210148(15) 0.02021(9) Uani 1 1 d . . .
P1 P 0.53901(6) 0.07247(7) 0.33215(5) 0.0299(2) Uani 1 1 d . . .
P2 P 0.30526(6) 0.16337(8) 0.25033(5) 0.0315(2) Uani 1 1 d . . .
P3 P 0.46638(7) 0.20214(8) 0.15002(6) 0.0340(2) Uani 1 1 d . . .
N1 N 0.39059(17) -0.0735(2) 0.15052(15) 0.0221(6) Uani 1 1 d . . .
C1 C 0.3776(2) -0.1689(3) 0.10173(17) 0.0221(7) Uani 1 1 d . . .
C2 C 0.4530(2) -0.2567(3) 0.12071(18) 0.0246(7) Uani 1 1 d . . .
C3 C 0.4361(2) -0.3535(3) 0.0718(2) 0.0314(8) Uani 1 1 d . . .
H3 H 0.4861 -0.4123 0.0846 0.038 Uiso 1 1 calc R . .
C4 C 0.3492(3) -0.3668(3) 0.0054(2) 0.0352(8) Uani 1 1 d . . .
H4 H 0.3395 -0.4341 -0.0273 0.042 Uiso 1 1 calc R . .
C5 C 0.2758(2) -0.2823(3) -0.0140(2) 0.0326(8) Uani 1 1 d . . .
H5 H 0.2162 -0.2919 -0.0606 0.039 Uiso 1 1 calc R . .
C6 C 0.2869(2) -0.1841(3) 0.03282(18) 0.0244(7) Uani 1 1 d . . .
C7 C 0.2085(2) -0.0885(3) 0.0114(2) 0.0330(8) Uani 1 1 d . . .
H7 H 0.2113 -0.0513 0.0642 0.040 Uiso 1 1 calc R . .
C8 C 0.2358(3) 0.0031(3) -0.0405(2) 0.0440(9) Uani 1 1 d . . .
H8A H 0.3055 0.0297 -0.0124 0.066 Uiso 1 1 calc R . .
H8B H 0.1888 0.0679 -0.0485 0.066 Uiso 1 1 calc R . .
H8C H 0.2308 -0.0293 -0.0940 0.066 Uiso 1 1 calc R . .
C9 C 0.0993(2) -0.1302(3) -0.0303(2) 0.0457(10) Uani 1 1 d . . .
H9A H 0.0916 -0.1594 -0.0852 0.069 Uiso 1 1 calc R . .
H9B H 0.0521 -0.0663 -0.0350 0.069 Uiso 1 1 calc R . .
H9C H 0.0843 -0.1916 0.0025 0.069 Uiso 1 1 calc R . .
C10 C 0.5521(2) -0.2398(3) 0.19102(19) 0.0299(8) Uani 1 1 d . . .
H10 H 0.5382 -0.1865 0.2312 0.036 Uiso 1 1 calc R . .
C11 C 0.5965(3) -0.3493(3) 0.2369(2) 0.0469(10) Uani 1 1 d . . .
H11A H 0.5450 -0.3877 0.2545 0.070 Uiso 1 1 calc R . .
H11B H 0.6556 -0.3305 0.2851 0.070 Uiso 1 1 calc R . .
H11C H 0.6175 -0.4004 0.2005 0.070 Uiso 1 1 calc R . .
C12 C 0.6299(2) -0.1820(3) 0.1598(2) 0.0451(10) Uani 1 1 d . . .
H12A H 0.6437 -0.2314 0.1189 0.068 Uiso 1 1 calc R . .
H12B H 0.6931 -0.1691 0.2058 0.068 Uiso 1 1 calc R . .
H12C H 0.6030 -0.1083 0.1345 0.068 Uiso 1 1 calc R . .
C13 C 0.6669(2) 0.0505(3) 0.3283(2) 0.0493(10) Uani 1 1 d . . .
H13A H 0.7164 0.0526 0.3841 0.074 Uiso 1 1 calc R . .
H13B H 0.6825 0.1112 0.2953 0.074 Uiso 1 1 calc R . .
H13C H 0.6702 -0.0242 0.3034 0.074 Uiso 1 1 calc R . .
C14 C 0.5327(3) -0.0440(3) 0.4007(2) 0.0440(10) Uani 1 1 d . . .
H14A H 0.5334 -0.1178 0.3738 0.066 Uiso 1 1 calc R . .
H14B H 0.4699 -0.0373 0.4137 0.066 Uiso 1 1 calc R . .
H14C H 0.5914 -0.0396 0.4515 0.066 Uiso 1 1 calc R . .
C15 C 0.5642(3) 0.1920(3) 0.4049(2) 0.0555(11) Uani 1 1 d . . .
H15A H 0.6246 0.1749 0.4525 0.083 Uiso 1 1 calc R . .
H15B H 0.5056 0.2032 0.4230 0.083 Uiso 1 1 calc R . .
H15C H 0.5760 0.2620 0.3780 0.083 Uiso 1 1 calc R . .
C16 C 0.2745(3) 0.1037(3) 0.3365(2) 0.0455(10) Uani 1 1 d . . .
H16A H 0.3314 0.1169 0.3875 0.068 Uiso 1 1 calc R . .
H16B H 0.2623 0.0212 0.3282 0.068 Uiso 1 1 calc R . .
H16C H 0.2133 0.1411 0.3400 0.068 Uiso 1 1 calc R . .
C17 C 0.3215(3) 0.3143(3) 0.2805(2) 0.0468(10) Uani 1 1 d . . .
H17A H 0.2610 0.3412 0.2918 0.070 Uiso 1 1 calc R . .
H17B H 0.3305 0.3599 0.2359 0.070 Uiso 1 1 calc R . .
H17C H 0.3814 0.3228 0.3300 0.070 Uiso 1 1 calc R . .
C18 C 0.1782(3) 0.1679(4) 0.1725(2) 0.0599(12) Uani 1 1 d . . .
H18A H 0.1312 0.2066 0.1950 0.090 Uiso 1 1 calc R . .
H18B H 0.1544 0.0895 0.1564 0.090 Uiso 1 1 calc R . .
H18C H 0.1810 0.2099 0.1242 0.090 Uiso 1 1 calc R . .
C19 C 0.5473(3) 0.3207(3) 0.2037(3) 0.0596(12) Uani 1 1 d . . .
H19A H 0.6088 0.2900 0.2450 0.089 Uiso 1 1 calc R . .
H19B H 0.5101 0.3681 0.2308 0.089 Uiso 1 1 calc R . .
H19C H 0.5663 0.3675 0.1641 0.089 Uiso 1 1 calc R . .
C20 C 0.3699(3) 0.2840(3) 0.0718(2) 0.0503(10) Uani 1 1 d . . .
H20A H 0.4028 0.3334 0.0424 0.076 Uiso 1 1 calc R . .
H20B H 0.3317 0.3315 0.0981 0.076 Uiso 1 1 calc R . .
H20C H 0.3232 0.2312 0.0330 0.076 Uiso 1 1 calc R . .
C21 C 0.5399(3) 0.1452(3) 0.0897(3) 0.0572(12) Uani 1 1 d . . .
H21A H 0.5005 0.0857 0.0525 0.086 Uiso 1 1 calc R . .
H21B H 0.6035 0.1122 0.1265 0.086 Uiso 1 1 calc R . .
H21C H 0.5555 0.2072 0.0575 0.086 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 0.01880(14) 0.01974(15) 0.02272(15) -0.00113(11) 0.00785(10) 0.00109(10)
P1 0.0260(4) 0.0303(5) 0.0285(5) -0.0014(4) 0.0029(4) 0.0029(4)
P2 0.0264(5) 0.0336(5) 0.0360(5) -0.0058(4) 0.0123(4) 0.0064(4)
P3 0.0370(5) 0.0262(5) 0.0428(6) 0.0075(4) 0.0185(4) 0.0009(4)
N1 0.0211(13) 0.0230(15) 0.0230(14) -0.0007(11) 0.0085(11) -0.0007(10)
C1 0.0255(16) 0.0253(18) 0.0200(16) 0.0011(14) 0.0137(13) -0.0067(13)
C2 0.0302(17) 0.0201(17) 0.0279(18) -0.0009(14) 0.0158(14) -0.0015(13)
C3 0.040(2) 0.0242(18) 0.035(2) 0.0002(16) 0.0199(17) -0.0002(15)
C4 0.050(2) 0.0244(19) 0.033(2) -0.0069(16) 0.0173(18) -0.0066(16)
C5 0.0348(19) 0.037(2) 0.0263(18) -0.0043(16) 0.0104(15) -0.0111(16)
C6 0.0263(17) 0.0283(18) 0.0209(16) 0.0008(14) 0.0113(14) -0.0046(14)
C7 0.0287(18) 0.041(2) 0.0275(18) -0.0026(16) 0.0076(15) 0.0005(15)
C8 0.041(2) 0.034(2) 0.048(2) 0.0074(19) 0.0036(18) 0.0045(17)
C9 0.030(2) 0.060(3) 0.042(2) 0.000(2) 0.0048(17) 0.0007(18)
C10 0.0292(18) 0.0320(19) 0.0285(18) -0.0033(15) 0.0096(15) 0.0070(15)
C11 0.053(2) 0.047(2) 0.037(2) 0.0101(19) 0.0103(18) 0.0086(19)
C12 0.0285(19) 0.043(2) 0.058(3) 0.003(2) 0.0081(18) -0.0021(17)
C13 0.0245(19) 0.058(3) 0.058(3) 0.005(2) 0.0040(17) 0.0046(18)
C14 0.047(2) 0.051(2) 0.032(2) 0.0082(18) 0.0098(17) 0.0114(18)
C15 0.051(2) 0.050(3) 0.047(2) -0.017(2) -0.0072(19) 0.004(2)
C16 0.051(2) 0.043(2) 0.056(2) -0.011(2) 0.038(2) 0.0001(19)
C17 0.052(2) 0.036(2) 0.057(3) -0.0041(19) 0.025(2) 0.0113(18)
C18 0.032(2) 0.079(3) 0.063(3) -0.013(2) 0.0085(19) 0.020(2)
C19 0.060(3) 0.036(2) 0.080(3) 0.010(2) 0.020(2) -0.015(2)
C20 0.069(3) 0.037(2) 0.046(2) 0.0116(19) 0.019(2) 0.010(2)
C21 0.069(3) 0.048(3) 0.077(3) 0.020(2) 0.055(3) 0.009(2)
_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 P1 2.2393(9) . ?
Ru1 P2 2.2536(9) . ?
Ru1 P3 2.2240(9) . ?
Ru1 N1 1.811(2) . ?
P1 C13 1.828(3) . ?
P1 C14 1.825(3) . ?
P1 C15 1.831(4) . ?
P2 C16 1.823(4) . ?
P2 C17 1.829(3) . ?
P2 C18 1.831(3) . ?
P3 C19 1.828(4) . ?
P3 C20 1.824(3) . ?
P3 C21 1.820(4) . ?
N1 C1 1.372(4) . ?
C1 C2 1.425(4) . ?
C1 C6 1.427(4) . ?
C2 C3 1.382(4) . ?
C2 C10 1.515(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.369(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.380(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.381(4) . ?
C6 C7 1.518(4) . ?
C7 H7 1.0000 . ?
C7 C8 1.527(5) . ?
C7 C9 1.530(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 1.0000 . ?
C10 C11 1.521(4) . ?
C10 C12 1.526(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 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
P1 Ru1 P2 93.27(3) . . ?
P3 Ru1 P1 96.47(3) . . ?
P3 Ru1 P2 95.17(3) . . ?
N1 Ru1 P1 122.63(8) . . ?
N1 Ru1 P2 128.40(8) . . ?
N1 Ru1 P3 113.69(8) . . ?
C13 P1 Ru1 114.14(13) . . ?
C13 P1 C15 99.70(18) . . ?
C14 P1 Ru1 111.27(12) . . ?
C14 P1 C13 100.47(17) . . ?
C14 P1 C15 99.25(18) . . ?
C15 P1 Ru1 127.93(12) . . ?
C16 P2 Ru1 114.61(12) . . ?
C16 P2 C17 100.04(17) . . ?
C16 P2 C18 100.06(19) . . ?
C17 P2 Ru1 125.73(13) . . ?
C17 P2 C18 100.26(18) . . ?
C18 P2 Ru1 112.35(13) . . ?
C19 P3 Ru1 125.29(14) . . ?
C20 P3 Ru1 117.98(13) . . ?
C20 P3 C19 98.97(18) . . ?
C21 P3 Ru1 109.03(13) . . ?
C21 P3 C19 101.3(2) . . ?
C21 P3 C20 100.66(18) . . ?
C1 N1 Ru1 174.9(2) . . ?
N1 C1 C2 120.5(3) . . ?
N1 C1 C6 120.7(3) . . ?
C2 C1 C6 118.8(3) . . ?
C1 C2 C10 119.7(3) . . ?
C3 C2 C1 119.0(3) . . ?
C3 C2 C10 121.2(3) . . ?
C2 C3 H3 119.1 . . ?
C4 C3 C2 121.7(3) . . ?
C4 C3 H3 119.1 . . ?
C3 C4 H4 120.1 . . ?
C3 C4 C5 119.9(3) . . ?
C5 C4 H4 120.1 . . ?
C4 C5 H5 119.2 . . ?
C4 C5 C6 121.5(3) . . ?
C6 C5 H5 119.2 . . ?
C1 C6 C7 118.5(3) . . ?
C5 C6 C1 119.0(3) . . ?
C5 C6 C7 122.5(3) . . ?
C6 C7 H7 107.1 . . ?
C6 C7 C8 110.7(3) . . ?
C6 C7 C9 113.8(3) . . ?
C8 C7 H7 107.1 . . ?
C8 C7 C9 110.7(3) . . ?
C9 C7 H7 107.1 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C2 C10 H10 107.5 . . ?
C2 C10 C11 114.3(3) . . ?
C2 C10 C12 109.9(3) . . ?
C11 C10 H10 107.5 . . ?
C11 C10 C12 110.0(3) . . ?
C12 C10 H10 107.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
P1 C13 H13A 109.5 . . ?
P1 C13 H13B 109.5 . . ?
P1 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
P1 C14 H14A 109.5 . . ?
P1 C14 H14B 109.5 . . ?
P1 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
P1 C15 H15A 109.5 . . ?
P1 C15 H15B 109.5 . . ?
P1 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
P2 C16 H16A 109.5 . . ?
P2 C16 H16B 109.5 . . ?
P2 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
P2 C17 H17A 109.5 . . ?
P2 C17 H17B 109.5 . . ?
P2 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
P2 C18 H18A 109.5 . . ?
P2 C18 H18B 109.5 . . ?
P2 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
P3 C19 H19A 109.5 . . ?
P3 C19 H19B 109.5 . . ?
P3 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
P3 C20 H20A 109.5 . . ?
P3 C20 H20B 109.5 . . ?
P3 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
P3 C21 H21A 109.5 . . ?
P3 C21 H21B 109.5 . . ?
P3 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 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
Ru1 N1 C1 C2 81(2) . . . . ?
Ru1 N1 C1 C6 -102(2) . . . . ?
P1 Ru1 P2 C16 -60.73(14) . . . . ?
P1 Ru1 P2 C17 63.71(16) . . . . ?
P1 Ru1 P2 C18 -174.07(16) . . . . ?
P1 Ru1 P3 C19 -22.15(18) . . . . ?
P1 Ru1 P3 C20 -148.47(15) . . . . ?
P1 Ru1 P3 C21 97.65(16) . . . . ?
P1 Ru1 N1 C1 -94(2) . . . . ?
P2 Ru1 P1 C13 -157.22(14) . . . . ?
P2 Ru1 P1 C14 89.94(13) . . . . ?
P2 Ru1 P1 C15 -31.53(19) . . . . ?
P2 Ru1 P3 C19 71.75(18) . . . . ?
P2 Ru1 P3 C20 -54.58(15) . . . . ?
P2 Ru1 P3 C21 -168.45(15) . . . . ?
P2 Ru1 N1 C1 140(2) . . . . ?
P3 Ru1 P1 C13 -61.63(14) . . . . ?
P3 Ru1 P1 C14 -174.47(13) . . . . ?
P3 Ru1 P1 C15 64.05(19) . . . . ?
P3 Ru1 P2 C16 -157.54(14) . . . . ?
P3 Ru1 P2 C17 -33.09(16) . . . . ?
P3 Ru1 P2 C18 89.13(16) . . . . ?
P3 Ru1 N1 C1 21(2) . . . . ?
N1 Ru1 P1 C13 61.93(16) . . . . ?
N1 Ru1 P1 C14 -50.91(16) . . . . ?
N1 Ru1 P1 C15 -172.4(2) . . . . ?
N1 Ru1 P2 C16 76.54(17) . . . . ?
N1 Ru1 P2 C17 -159.01(18) . . . . ?
N1 Ru1 P2 C18 -36.79(19) . . . . ?
N1 Ru1 P3 C19 -152.12(19) . . . . ?
N1 Ru1 P3 C20 81.55(17) . . . . ?
N1 Ru1 P3 C21 -32.32(18) . . . . ?
N1 C1 C2 C3 177.9(3) . . . . ?
N1 C1 C2 C10 -5.1(4) . . . . ?
N1 C1 C6 C5 -178.8(3) . . . . ?
N1 C1 C6 C7 4.1(4) . . . . ?
C1 C2 C3 C4 0.5(5) . . . . ?
C1 C2 C10 C11 146.3(3) . . . . ?
C1 C2 C10 C12 -89.5(3) . . . . ?
C1 C6 C7 C8 83.6(3) . . . . ?
C1 C6 C7 C9 -151.0(3) . . . . ?
C2 C1 C6 C5 -1.0(4) . . . . ?
C2 C1 C6 C7 -178.1(3) . . . . ?
C2 C3 C4 C5 -0.1(5) . . . . ?
C3 C2 C10 C11 -36.8(4) . . . . ?
C3 C2 C10 C12 87.4(4) . . . . ?
C3 C4 C5 C6 -0.8(5) . . . . ?
C4 C5 C6 C1 1.4(5) . . . . ?
C4 C5 C6 C7 178.4(3) . . . . ?
C5 C6 C7 C8 -93.4(4) . . . . ?
C5 C6 C7 C9 32.0(4) . . . . ?
C6 C1 C2 C3 0.1(4) . . . . ?
C6 C1 C2 C10 177.0(3) . . . . ?
C10 C2 C3 C4 -176.4(3) . . . . ?
_database_code_depnum_ccdc_archive 'CCDC 957943'
#######################################################################
#
# 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
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# to carry out CIF format checking respectively.
#
data_aks03132013_0m_compd2
_audit_creation_date 2013-05-30
_audit_creation_method
;
Olex2 1.2
(compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C21 H44 Cu I N P3 Ru'
_chemical_formula_sum 'C21 H44 Cu I N P3 Ru'
_chemical_formula_weight 694.99
_chemical_absolute_configuration ?
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_H-M_alt 'P 21 21 21'
_space_group_name_Hall 'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'
_cell_length_a 10.4473(2)
_cell_length_b 16.2159(2)
_cell_length_c 17.5870(2)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 2979.46(8)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 5537
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max 24.63
_cell_measurement_theta_min 2.27
_exptl_absorpt_coefficient_mu 2.426
_exptl_absorpt_correction_T_max 0.7452
_exptl_absorpt_correction_T_min 0.6696
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0726 before and 0.0659 after correction.
The Ratio of minimum to maximum transmission is 0.8986.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour ?
_exptl_crystal_density_diffrn 1.549
_exptl_crystal_density_meas .
_exptl_crystal_density_method ?
_exptl_crystal_description ?
_exptl_crystal_F_000 1392
_exptl_crystal_size_max ?
_exptl_crystal_size_mid ?
_exptl_crystal_size_min ?
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0682
_diffrn_reflns_av_unetI/netI 0.0860
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 16754
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.319
_diffrn_reflns_theta_min 1.708
_diffrn_ambient_temperature 173.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.758
_reflns_Friedel_fraction_full 0.983
_reflns_Friedel_fraction_max 0.980
_reflns_number_gt 4110
_reflns_number_total 5401
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement ?
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max 0.473
_refine_diff_density_min -0.505
_refine_diff_density_rms 0.120
_refine_ls_abs_structure_details
;
Flack x determined using 1429 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack -0.004(19)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.991
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 266
_refine_ls_number_reflns 5401
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0674
_refine_ls_R_factor_gt 0.0425
_refine_ls_restrained_S_all 0.991
_refine_ls_shift/su_max 0.100
_refine_ls_shift/su_mean 0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0157P)^2^]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0610
_refine_ls_wR_factor_ref 0.0693
_refine_special_details
;
?
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
C10(H10), C7(H7)
2.b Aromatic/amide H refined with riding coordinates:
C5(H5), C4(H4), C3(H3)
2.c Idealised Me refined as rotating group:
C18(H18A,H18B,H18C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C12(H12A,H12B,
H12C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C19(H19A,H19B,
H19C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C14(H14A,H14B,H14C), C15(H15A,
H15B,H15C), C13(H13A,H13B,H13C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.13053(7) 0.46233(4) 0.87745(4) 0.02156(18) Uani 1 1 d . . . . .
I1 I 0.31008(6) 0.67073(4) 0.72516(4) 0.0445(2) Uani 1 1 d . . . . .
Cu1 Cu 0.14631(10) 0.59624(6) 0.79197(6) 0.0295(3) Uani 1 1 d . . . . .
P2 P 0.2047(3) 0.35202(14) 0.81322(13) 0.0307(6) Uani 1 1 d . . . . .
P3 P 0.0173(2) 0.39298(15) 0.96278(14) 0.0311(6) Uani 1 1 d . . . . .
P1 P 0.3111(2) 0.47262(14) 0.94760(13) 0.0300(6) Uani 1 1 d . . . . .
N1 N 0.0159(6) 0.5428(4) 0.8451(3) 0.0233(17) Uani 1 1 d . . . . .
C18 C 0.0801(9) 0.2842(5) 0.7775(5) 0.050(3) Uani 1 1 d . . . . .
H18A H 0.1168 0.2460 0.7402 0.074 Uiso 1 1 calc R U . . .
H18B H 0.0130 0.3171 0.7531 0.074 Uiso 1 1 calc R U . . .
H18C H 0.0432 0.2528 0.8197 0.074 Uiso 1 1 calc R U . . .
C16 C 0.2806(10) 0.3856(6) 0.7242(5) 0.052(3) Uani 1 1 d . . . . .
H16A H 0.3078 0.3372 0.6951 0.078 Uiso 1 1 calc R U . . .
H16B H 0.3554 0.4198 0.7359 0.078 Uiso 1 1 calc R U . . .
H16C H 0.2192 0.4177 0.6942 0.078 Uiso 1 1 calc R U . . .
C17 C 0.3205(10) 0.2755(5) 0.8471(5) 0.048(3) Uani 1 1 d . . . . .
H17A H 0.2910 0.2524 0.8955 0.072 Uiso 1 1 calc R U . . .
H17B H 0.4039 0.3020 0.8544 0.072 Uiso 1 1 calc R U . . .
H17C H 0.3286 0.2313 0.8094 0.072 Uiso 1 1 calc R U . . .
C1 C -0.1054(8) 0.5809(5) 0.8454(5) 0.021(2) Uani 1 1 d . . . . .
C6 C -0.1998(8) 0.5550(5) 0.7926(5) 0.025(2) Uani 1 1 d . . . . .
C5 C -0.3169(8) 0.5950(5) 0.7925(5) 0.029(2) Uani 1 1 d . . . . .
H5 H -0.3805 0.5785 0.7570 0.035 Uiso 1 1 calc R U . . .
C4 C -0.3434(9) 0.6576(5) 0.8421(5) 0.032(2) Uani 1 1 d . . . . .
H4 H -0.4242 0.6843 0.8407 0.038 Uiso 1 1 calc R U . . .
C3 C -0.2518(9) 0.6820(5) 0.8947(5) 0.029(2) Uani 1 1 d . . . . .
H3 H -0.2714 0.7247 0.9297 0.035 Uiso 1 1 calc R U . . .
C2 C -0.1328(9) 0.6451(5) 0.8968(4) 0.025(2) Uani 1 1 d . . . . .
C10 C -0.0318(8) 0.6741(6) 0.9530(5) 0.032(2) Uani 1 1 d . . . . .
H10 H 0.0329 0.6290 0.9581 0.038 Uiso 1 1 calc R U . . .
C12 C -0.0862(9) 0.6911(5) 1.0325(5) 0.038(3) Uani 1 1 d . . . . .
H12A H -0.1364 0.7422 1.0314 0.057 Uiso 1 1 calc R U . . .
H12B H -0.0157 0.6969 1.0688 0.057 Uiso 1 1 calc R U . . .
H12C H -0.1413 0.6452 1.0479 0.057 Uiso 1 1 calc R U . . .
C11 C 0.0374(10) 0.7501(5) 0.9221(5) 0.045(3) Uani 1 1 d . . . . .
H11A H 0.0767 0.7368 0.8730 0.067 Uiso 1 1 calc R U . . .
H11B H 0.1041 0.7671 0.9581 0.067 Uiso 1 1 calc R U . . .
H11C H -0.0240 0.7952 0.9155 0.067 Uiso 1 1 calc R U . . .
C7 C -0.1723(8) 0.4852(5) 0.7368(5) 0.031(2) Uani 1 1 d . . . . .
H7 H -0.1050 0.4496 0.7605 0.037 Uiso 1 1 calc R U . . .
C9 C -0.1160(11) 0.5199(7) 0.6639(5) 0.055(3) Uani 1 1 d . . . . .
H9A H -0.0903 0.4745 0.6305 0.083 Uiso 1 1 calc R U . . .
H9B H -0.0412 0.5539 0.6760 0.083 Uiso 1 1 calc R U . . .
H9C H -0.1804 0.5538 0.6381 0.083 Uiso 1 1 calc R U . . .
C8 C -0.2857(9) 0.4305(5) 0.7200(6) 0.046(3) Uani 1 1 d . . . . .
H8A H -0.3526 0.4628 0.6947 0.070 Uiso 1 1 calc R U . . .
H8B H -0.3193 0.4078 0.7676 0.070 Uiso 1 1 calc R U . . .
H8C H -0.2589 0.3852 0.6866 0.070 Uiso 1 1 calc R U . . .
C19 C 0.0674(10) 0.2924(5) 0.9984(5) 0.045(3) Uani 1 1 d . . . . .
H19A H 0.0028 0.2712 1.0338 0.068 Uiso 1 1 calc R U . . .
H19B H 0.1495 0.2979 1.0249 0.068 Uiso 1 1 calc R U . . .
H19C H 0.0769 0.2540 0.9558 0.068 Uiso 1 1 calc R U . . .
C21 C -0.0138(10) 0.4482(6) 1.0509(5) 0.048(3) Uani 1 1 d . . . . .
H21A H -0.0449 0.5038 1.0392 0.071 Uiso 1 1 calc R U . . .
H21B H 0.0654 0.4520 1.0805 0.071 Uiso 1 1 calc R U . . .
H21C H -0.0786 0.4185 1.0804 0.071 Uiso 1 1 calc R U . . .
C20 C -0.1465(9) 0.3721(6) 0.9312(6) 0.057(3) Uani 1 1 d . . . . .
H20A H -0.1444 0.3358 0.8866 0.085 Uiso 1 1 calc R U . . .
H20B H -0.1886 0.4241 0.9177 0.085 Uiso 1 1 calc R U . . .
H20C H -0.1941 0.3451 0.9723 0.085 Uiso 1 1 calc R U . . .
C14 C 0.4598(9) 0.4864(7) 0.8958(6) 0.062(4) Uani 1 1 d . . . . .
H14A H 0.4467 0.5263 0.8546 0.093 Uiso 1 1 calc R U . . .
H14B H 0.4869 0.4335 0.8744 0.093 Uiso 1 1 calc R U . . .
H14C H 0.5259 0.5070 0.9305 0.093 Uiso 1 1 calc R U . . .
C15 C 0.3620(10) 0.4011(5) 1.0208(5) 0.044(3) Uani 1 1 d . . . . .
H15A H 0.3715 0.3459 0.9987 0.066 Uiso 1 1 calc R U . . .
H15B H 0.2978 0.3995 1.0614 0.066 Uiso 1 1 calc R U . . .
H15C H 0.4443 0.4191 1.0418 0.066 Uiso 1 1 calc R U . . .
C13 C 0.3051(11) 0.5685(6) 1.0023(6) 0.066(4) Uani 1 1 d . . . . .
H13A H 0.3795 0.5715 1.0361 0.100 Uiso 1 1 calc R U . . .
H13B H 0.2265 0.5699 1.0326 0.100 Uiso 1 1 calc R U . . .
H13C H 0.3062 0.6157 0.9674 0.100 Uiso 1 1 calc R U . . .
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 0.0223(4) 0.0197(3) 0.0227(4) -0.0005(3) 0.0004(4) 0.0004(4)
I1 0.0397(4) 0.0508(4) 0.0431(4) 0.0097(4) 0.0063(4) -0.0094(4)
Cu1 0.0283(6) 0.0288(6) 0.0313(7) 0.0049(5) 0.0029(6) 0.0003(6)
P2 0.0354(15) 0.0288(14) 0.0280(14) -0.0048(11) -0.0022(13) 0.0056(12)
P3 0.0284(14) 0.0311(14) 0.0337(16) 0.0020(13) 0.0040(12) -0.0019(12)
P1 0.0299(14) 0.0274(13) 0.0326(14) 0.0022(12) -0.0052(12) -0.0034(13)
N1 0.025(4) 0.021(4) 0.024(4) -0.001(4) 0.000(3) 0.003(4)
C18 0.055(7) 0.041(6) 0.052(7) -0.024(6) -0.011(6) 0.003(5)
C16 0.083(8) 0.041(6) 0.032(6) -0.004(5) 0.013(6) 0.005(6)
C17 0.063(8) 0.041(6) 0.041(6) -0.006(5) -0.005(6) 0.025(6)
C1 0.022(5) 0.020(5) 0.021(5) 0.011(4) 0.000(4) -0.002(4)
C6 0.028(5) 0.021(5) 0.026(5) 0.000(4) 0.013(5) -0.003(4)
C5 0.024(5) 0.030(5) 0.035(6) -0.001(5) 0.004(5) 0.000(5)
C4 0.022(6) 0.031(5) 0.042(6) 0.007(5) 0.011(5) 0.004(5)
C3 0.034(6) 0.021(5) 0.032(6) 0.002(5) 0.008(5) 0.006(5)
C2 0.029(5) 0.021(5) 0.025(5) 0.010(4) 0.005(5) 0.000(5)
C10 0.035(6) 0.030(5) 0.031(6) -0.011(5) -0.008(5) 0.016(5)
C12 0.047(7) 0.035(6) 0.032(6) -0.009(5) -0.002(5) 0.009(5)
C11 0.048(7) 0.038(6) 0.049(7) -0.006(5) -0.010(6) -0.015(6)
C7 0.027(6) 0.032(5) 0.033(6) -0.005(4) -0.005(5) 0.005(4)
C9 0.053(8) 0.076(8) 0.037(6) -0.018(6) 0.016(6) -0.009(7)
C8 0.052(7) 0.039(6) 0.048(7) -0.007(5) -0.002(6) -0.006(5)
C19 0.046(7) 0.036(6) 0.054(7) 0.011(5) 0.017(6) -0.011(5)
C21 0.059(7) 0.043(7) 0.041(6) 0.005(6) 0.018(6) 0.005(6)
C20 0.032(7) 0.063(7) 0.076(8) 0.019(6) 0.010(6) -0.011(6)
C14 0.036(7) 0.086(9) 0.063(8) 0.016(7) 0.000(6) -0.019(7)
C15 0.052(7) 0.047(6) 0.034(6) -0.002(5) -0.010(6) 0.008(6)
C13 0.077(9) 0.047(7) 0.076(9) -0.014(6) -0.048(7) -0.009(7)
_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 Cu1 2.6462(12) . ?
Ru1 P2 2.253(2) . ?
Ru1 P3 2.217(2) . ?
Ru1 P1 2.260(3) . ?
Ru1 N1 1.861(7) . ?
I1 Cu1 2.4014(12) . ?
Cu1 N1 1.866(7) . ?
P2 C18 1.817(9) . ?
P2 C16 1.837(9) . ?
P2 C17 1.832(9) . ?
P3 C19 1.824(9) . ?
P3 C21 1.819(9) . ?
P3 C20 1.831(10) . ?
P1 C14 1.814(10) . ?
P1 C15 1.813(9) . ?
P1 C13 1.830(9) . ?
N1 C1 1.409(10) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C1 C6 1.419(11) . ?
C1 C2 1.408(11) . ?
C6 C5 1.384(11) . ?
C6 C7 1.525(10) . ?
C5 H5 0.9500 . ?
C5 C4 1.367(11) . ?
C4 H4 0.9500 . ?
C4 C3 1.387(12) . ?
C3 H3 0.9500 . ?
C3 C2 1.381(11) . ?
C2 C10 1.520(11) . ?
C10 H10 1.0000 . ?
C10 C12 1.533(10) . ?
C10 C11 1.530(12) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C7 H7 1.0000 . ?
C7 C9 1.518(11) . ?
C7 C8 1.510(11) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 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
P2 Ru1 Cu1 110.20(7) . . ?
P2 Ru1 P1 92.59(9) . . ?
P3 Ru1 Cu1 146.51(7) . . ?
P3 Ru1 P2 96.90(9) . . ?
P3 Ru1 P1 96.51(9) . . ?
P1 Ru1 Cu1 101.39(7) . . ?
N1 Ru1 Cu1 44.8(2) . . ?
N1 Ru1 P2 128.7(2) . . ?
N1 Ru1 P3 102.7(2) . . ?
N1 Ru1 P1 130.7(2) . . ?
I1 Cu1 Ru1 137.32(5) . . ?
N1 Cu1 Ru1 44.7(2) . . ?
N1 Cu1 I1 177.5(2) . . ?
C18 P2 Ru1 114.1(3) . . ?
C18 P2 C16 101.2(5) . . ?
C18 P2 C17 100.1(4) . . ?
C16 P2 Ru1 109.9(3) . . ?
C17 P2 Ru1 127.0(3) . . ?
C17 P2 C16 101.1(5) . . ?
C19 P3 Ru1 122.2(3) . . ?
C19 P3 C20 101.9(5) . . ?
C21 P3 Ru1 115.0(3) . . ?
C21 P3 C19 101.5(4) . . ?
C21 P3 C20 100.5(5) . . ?
C20 P3 Ru1 112.8(3) . . ?
C14 P1 Ru1 116.7(3) . . ?
C14 P1 C13 100.9(5) . . ?
C15 P1 Ru1 125.8(3) . . ?
C15 P1 C14 100.6(5) . . ?
C15 P1 C13 100.4(4) . . ?
C13 P1 Ru1 108.7(4) . . ?
Ru1 N1 Cu1 90.5(3) . . ?
C1 N1 Ru1 152.2(6) . . ?
C1 N1 Cu1 117.1(5) . . ?
P2 C18 H18A 109.5 . . ?
P2 C18 H18B 109.5 . . ?
P2 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
P2 C16 H16A 109.5 . . ?
P2 C16 H16B 109.5 . . ?
P2 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
P2 C17 H17A 109.5 . . ?
P2 C17 H17B 109.5 . . ?
P2 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N1 C1 C6 119.6(7) . . ?
C2 C1 N1 120.6(8) . . ?
C2 C1 C6 119.8(8) . . ?
C1 C6 C7 120.6(8) . . ?
C5 C6 C1 118.5(7) . . ?
C5 C6 C7 120.9(8) . . ?
C6 C5 H5 119.2 . . ?
C4 C5 C6 121.7(8) . . ?
C4 C5 H5 119.2 . . ?
C5 C4 H4 120.1 . . ?
C5 C4 C3 119.9(8) . . ?
C3 C4 H4 120.1 . . ?
C4 C3 H3 119.5 . . ?
C2 C3 C4 121.1(8) . . ?
C2 C3 H3 119.5 . . ?
C1 C2 C10 120.3(8) . . ?
C3 C2 C1 119.1(8) . . ?
C3 C2 C10 120.6(8) . . ?
C2 C10 H10 107.5 . . ?
C2 C10 C12 113.0(7) . . ?
C2 C10 C11 110.3(7) . . ?
C12 C10 H10 107.5 . . ?
C11 C10 H10 107.5 . . ?
C11 C10 C12 110.7(8) . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C6 C7 H7 107.1 . . ?
C9 C7 C6 109.9(7) . . ?
C9 C7 H7 107.1 . . ?
C8 C7 C6 114.5(8) . . ?
C8 C7 H7 107.1 . . ?
C8 C7 C9 110.9(8) . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
P3 C19 H19A 109.5 . . ?
P3 C19 H19B 109.5 . . ?
P3 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
P3 C21 H21A 109.5 . . ?
P3 C21 H21B 109.5 . . ?
P3 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
P3 C20 H20A 109.5 . . ?
P3 C20 H20B 109.5 . . ?
P3 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
P1 C14 H14A 109.5 . . ?
P1 C14 H14B 109.5 . . ?
P1 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
P1 C15 H15A 109.5 . . ?
P1 C15 H15B 109.5 . . ?
P1 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
P1 C13 H13A 109.5 . . ?
P1 C13 H13B 109.5 . . ?
P1 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 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
Ru1 Cu1 N1 C1 176.6(7) . . . . ?
Ru1 N1 C1 C6 -90.6(13) . . . . ?
Ru1 N1 C1 C2 90.4(13) . . . . ?
Cu1 Ru1 N1 C1 -173.4(14) . . . . ?
Cu1 N1 C1 C6 96.9(8) . . . . ?
Cu1 N1 C1 C2 -82.2(8) . . . . ?
P2 Ru1 N1 Cu1 -79.7(3) . . . . ?
P2 Ru1 N1 C1 106.9(12) . . . . ?
P3 Ru1 N1 Cu1 170.54(17) . . . . ?
P3 Ru1 N1 C1 -2.9(13) . . . . ?
P1 Ru1 N1 Cu1 60.3(3) . . . . ?
P1 Ru1 N1 C1 -113.1(12) . . . . ?
N1 C1 C6 C5 -178.1(7) . . . . ?
N1 C1 C6 C7 1.4(11) . . . . ?
N1 C1 C2 C3 178.9(7) . . . . ?
N1 C1 C2 C10 -0.2(11) . . . . ?
C1 C6 C5 C4 -0.6(12) . . . . ?
C1 C6 C7 C9 -90.1(9) . . . . ?
C1 C6 C7 C8 144.4(8) . . . . ?
C1 C2 C10 C12 -138.6(8) . . . . ?
C1 C2 C10 C11 96.8(9) . . . . ?
C6 C1 C2 C3 -0.2(11) . . . . ?
C6 C1 C2 C10 -179.2(7) . . . . ?
C6 C5 C4 C3 -0.5(13) . . . . ?
C5 C6 C7 C9 89.5(10) . . . . ?
C5 C6 C7 C8 -36.1(11) . . . . ?
C5 C4 C3 C2 1.3(13) . . . . ?
C4 C3 C2 C1 -0.9(12) . . . . ?
C4 C3 C2 C10 178.1(8) . . . . ?
C3 C2 C10 C12 42.3(11) . . . . ?
C3 C2 C10 C11 -82.2(10) . . . . ?
C2 C1 C6 C5 0.9(12) . . . . ?
C2 C1 C6 C7 -179.6(7) . . . . ?
C7 C6 C5 C4 179.9(7) . . . . ?
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_shelx_hkl_checksum 23742
_shelx_hkl_file
;
1 0 0 -0.64 0.31
-1 0 0 -0.67 0.33
2 0 0 385.94 12.36
-2 0 0 388.49 12.41
-3 0 0 -1.31 0.62
-3 0 0 -1.12 0.69
-4 0 0 214.60 7.76
-4 0 0 203.15 8.66
5 0 0 -0.25 1.00
-5 0 0 -1.14 0.76
-5 0 0 -0.11 0.76
6 0 0 448.40 16.83
-6 0 0 422.94 16.85
-6 0 0 440.51 15.08
7 0 0 -1.03 1.16
-7 0 0 0.55 1.48
8 0 0 -0.11 1.48
-8 0 0 1.25 1.79
-9 0 0 -1.39 1.72
9 0 0 -0.05 1.89
10 0 0 6.25 2.90
-10 0 0 8.68 3.05
-11 0 0 1.10 2.49
11 0 0 1.15 2.85
12 0 0 32.35 6.49
-1 1 0 699.29 20.81
1 1 0 725.02 20.95
-1 -1 0 693.45 20.91
1 -1 0 741.67 20.89
2 1 0 130.90 5.27
2 -1 0 130.65 5.19
2 1 0 125.54 5.14
-2 -1 0 127.45 5.24
-2 1 0 128.39 4.99
-2 1 0 133.95 5.21
-3 -1 0 22.02 2.34
3 1 0 25.39 2.38
-3 1 0 24.55 2.35
-4 -1 0 36.32 3.17
-4 1 0 28.53 2.87
-4 -1 0 30.09 2.09
4 1 0 29.66 2.90
-5 1 0 151.16 7.69
-5 -1 0 154.84 7.83
5 1 0 167.51 7.96
-5 -1 0 161.05 6.37
-6 1 0 94.24 6.27
6 1 0 99.77 6.44
-6 -1 0 110.02 6.68
-6 1 0 111.55 5.85
-7 1 0 24.58 3.43
7 -1 0 22.26 3.40
7 1 0 21.74 3.74
-7 -1 0 24.57 3.65
8 -1 0 28.60 4.02
8 1 0 25.55 3.82
-8 1 0 24.22 3.90
-8 -1 0 25.41 4.09
-9 -1 0 15.15 3.74
-9 1 0 26.82 5.05
9 1 0 25.51 4.80
9 -1 0 25.10 4.73
10 1 0 2.50 2.33
-10 1 0 0.95 2.18
-10 -1 0 1.97 2.29
10 -1 0 0.13 2.03
11 1 0 13.67 4.40
-11 -1 0 8.16 3.81
-11 1 0 7.02 3.47
11 -1 0 12.54 3.99
12 1 0 29.12 6.07
12 -1 0 32.91 6.62
0 -2 0 251.09 8.11
0 2 0 244.66 8.10
1 -2 0 51.84 2.60
1 2 0 49.05 2.65
-1 2 0 53.20 2.67
-1 2 0 50.75 2.62
-2 2 0 4.43 1.18
2 2 0 4.71 1.31
-2 2 0 5.09 1.25
2 2 0 3.71 1.12
2 -2 0 3.31 1.19
-2 -2 0 7.04 1.40
3 2 0 52.46 3.57
-3 2 0 57.27 3.53
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-2 -2 9 26.41 3.07
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3 2 -9 27.49 3.28
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3 2 9 20.54 1.79
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-3 -2 9 17.19 3.12
3 2 9 16.27 1.96
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-4 -2 -9 19.89 3.09
4 2 -9 18.00 3.50
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4 2 9 12.97 1.91
-4 -2 9 16.87 3.03
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4 2 9 10.62 1.61
5 2 -9 6.70 2.55
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-5 2 9 2.37 1.34
-5 -2 -9 3.60 1.85
-5 2 -9 2.43 1.86
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-5 -2 9 2.29 1.52
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-6 -2 9 84.61 6.44
-6 -2 9 102.36 7.75
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-7 -2 -9 6.89 2.51
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-7 -2 9 9.27 2.79
-7 -2 9 16.39 3.96
8 2 -9 18.44 4.46
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-8 -2 9 24.38 5.00
-8 2 -9 27.59 5.04
-8 -2 9 28.01 4.81
9 2 -9 7.16 3.84
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-9 -2 9 7.14 3.58
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-9 -2 9 9.73 3.04
10 2 -9 21.19 5.28
-10 -2 9 16.42 4.19
11 2 -9 2.04 3.49
-11 -2 9 3.78 3.09
11 -2 -9 0.96 3.23
0 3 -9 53.01 3.23
0 3 -9 52.05 4.42
0 3 9 50.15 3.67
0 -3 9 58.75 4.66
1 -3 9 25.43 3.35
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1 3 -9 29.28 2.80
1 3 -9 31.37 3.40
-1 3 -9 34.21 3.73
1 3 9 33.39 2.75
-1 3 -9 33.85 1.99
-1 -3 9 41.24 3.86
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2 3 -9 51.22 4.01
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-2 -3 -9 47.20 4.47
2 3 -9 52.91 4.29
2 3 9 47.67 3.19
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3 3 -9 36.24 3.63
-3 -3 -9 36.06 3.83
3 3 -9 41.26 3.79
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-3 -3 9 32.62 3.62
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3 3 9 34.38 2.90
3 3 9 33.46 2.68
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4 3 -9 25.93 3.15
-4 -3 -9 31.29 3.55
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4 3 9 26.65 2.74
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4 3 9 23.34 2.39
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5 3 -9 103.06 7.34
-5 -3 -9 87.86 6.19
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5 3 9 90.84 5.26
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5 3 9 83.31 5.08
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-6 -3 9 8.62 2.66
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-7 -3 -9 24.02 3.60
-7 -3 9 19.19 4.01
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11 3 -9 19.59 5.76
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0 4 -9 125.55 5.64
0 4 -9 121.07 7.16
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1 4 -9 56.68 3.90
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1 4 -9 59.82 4.62
1 -4 9 56.05 4.82
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1 4 9 51.26 3.82
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2 -4 9 14.84 3.16
2 4 -9 14.18 2.64
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3 4 -9 134.66 7.53
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3 4 9 127.59 6.22
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4 4 -9 23.58 3.00
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4 4 9 20.29 2.56
4 4 9 20.31 2.76
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5 4 -9 0.75 1.23
5 4 -9 1.20 2.03
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5 4 9 6.54 1.99
-5 -4 9 5.04 2.35
5 4 9 2.25 1.34
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6 4 -9 29.26 4.73
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7 4 -9 52.58 6.21
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8 4 -9 -0.04 2.73
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10 4 -9 14.08 4.52
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11 4 -9 3.61 4.36
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0 -5 9 8.88 2.62
0 5 -9 13.57 1.91
0 5 -9 8.67 2.37
0 5 9 12.75 2.50
1 5 -9 70.45 4.68
1 -5 9 79.44 5.96
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1 5 -9 69.18 5.24
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1 5 9 80.87 5.13
-1 5 -9 88.24 6.16
-1 5 -9 81.48 4.25
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2 -5 9 69.01 5.73
2 5 -9 71.86 5.09
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3 5 -9 33.54 3.51
3 5 9 25.61 3.04
3 5 9 22.04 2.81
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4 5 -9 29.40 3.82
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4 5 -9 31.62 3.45
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4 5 9 25.29 3.18
4 5 9 29.61 3.23
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5 5 -9 30.77 4.31
-5 5 -9 29.54 4.35
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5 5 9 36.74 3.84
5 5 9 29.27 3.40
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10 5 -9 9.00 4.35
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0 6 -9 18.78 2.30
0 6 -9 16.19 3.18
1 6 -9 57.87 4.34
1 6 -9 63.51 4.98
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1 -6 9 61.66 5.45
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2 6 -9 20.57 2.95
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2 6 9 20.19 2.99
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3 6 -9 20.48 2.91
3 6 -9 21.85 3.33
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3 6 9 25.77 3.29
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4 6 -9 66.65 4.90
4 6 -9 68.74 6.03
4 6 9 73.95 5.45
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4 6 9 67.58 5.08
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5 6 9 17.05 3.15
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1 -7 9 -0.55 1.46
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1 7 -9 -0.21 1.07
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3 7 -9 2.60 1.79
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3 -8 9 14.69 3.70
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3 -9 9 48.98 5.81
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-2 -8 18 2.20 3.26
-2 8 -18 2.69 3.30
-3 -8 -18 1.36 2.90
-3 8 -18 0.02 2.70
-3 -8 18 1.59 3.53
-4 -8 -18 -0.93 2.23
-4 8 -18 -1.22 2.74
-4 -8 18 0.75 2.72
0 9 -18 4.90 3.23
0 -9 18 21.20 5.58
1 9 -18 10.31 4.23
1 -9 18 24.83 6.54
-1 9 -18 16.54 5.08
-1 -9 18 6.33 3.93
-2 -9 -18 1.48 3.17
2 9 -18 1.97 2.81
-2 -9 18 0.75 3.18
-2 9 -18 -3.73 2.58
-3 -9 -18 6.38 3.57
-3 9 -18 10.41 4.88
-3 -9 18 3.20 4.10
0 -10 18 6.88 4.47
0 10 -18 4.87 3.23
1 -10 18 20.61 6.01
1 10 -18 16.89 5.15
-1 -10 18 19.96 6.08
-1 10 -18 30.55 6.90
0 0 -19 1.34 2.68
1 0 -19 -0.21 2.41
-1 0 -19 -1.85 1.81
2 0 -19 4.16 3.01
-2 0 -19 6.13 3.16
3 0 -19 -3.76 2.01
-3 0 -19 0.39 2.66
-4 0 -19 1.04 3.15
4 0 -19 0.53 2.63
5 0 -19 31.95 6.36
-5 0 -19 37.21 7.20
0 -1 -19 17.34 4.86
0 1 -19 18.52 4.93
-1 -1 -19 6.46 3.84
1 1 -19 5.82 3.21
1 -1 -19 13.11 4.67
-1 1 -19 5.61 3.31
-2 -1 -19 7.10 3.27
2 1 -19 8.16 3.68
-2 1 -19 0.44 2.76
2 -1 -19 9.38 4.18
-3 -1 -19 11.10 4.44
3 1 -19 4.84 3.08
-3 1 -19 5.66 3.37
3 -1 -19 4.65 3.37
-4 -1 -19 1.84 2.91
4 1 -19 7.05 3.42
-4 1 -19 0.87 3.32
4 -1 -19 -0.18 2.92
-5 -1 -19 1.36 3.04
5 1 -19 -2.12 2.77
5 -1 -19 -1.64 2.40
-5 1 -19 0.05 2.70
0 2 -19 3.13 3.11
0 -2 -19 -0.66 2.36
1 2 -19 8.77 3.70
-1 -2 -19 6.43 3.52
1 -2 -19 12.17 4.67
-1 2 -19 18.76 4.84
2 2 -19 1.66 2.61
-2 -2 -19 6.70 3.31
2 -2 -19 6.47 3.33
-2 2 -19 5.46 3.58
-3 -2 -19 15.88 4.76
3 2 -19 25.18 5.74
-3 2 -19 13.60 4.56
3 -2 -19 18.87 5.12
-4 -2 -19 -1.64 2.44
4 2 -19 10.71 4.12
-4 2 -19 7.42 3.84
4 -2 -19 9.91 4.45
5 2 -19 7.08 3.33
-5 -2 -19 4.79 3.59
-5 2 -19 5.94 3.71
0 -3 -19 28.13 6.10
0 3 -19 31.73 6.39
1 3 -19 6.49 3.46
-1 -3 -19 6.20 3.26
1 -3 -19 4.17 2.93
-1 3 -19 9.45 3.89
-1 -3 19 0.58 2.76
2 3 -19 30.19 6.16
-2 -3 -19 30.71 6.01
2 -3 -19 35.46 6.85
-2 3 -19 24.11 5.79
3 3 -19 7.00 3.71
-3 -3 -19 0.98 2.71
3 -3 -19 0.82 2.39
-3 3 -19 0.56 2.70
4 3 -19 25.95 5.59
-4 -3 -19 20.16 5.48
-4 3 -19 29.56 6.18
5 3 -19 10.11 4.97
-5 -3 -19 12.54 4.63
-5 3 -19 5.69 3.98
0 4 -19 47.33 6.78
0 -4 -19 42.83 6.45
1 4 -19 23.36 5.41
-1 -4 -19 19.29 5.35
-1 -4 19 13.81 4.22
-1 4 -19 12.93 4.52
1 -4 -19 13.75 4.62
-2 -4 -19 26.29 5.93
2 4 -19 20.70 5.07
-2 -4 19 40.98 6.29
-2 4 -19 19.09 5.35
2 -4 -19 26.41 5.73
3 4 -19 15.46 4.38
-3 -4 -19 8.12 3.67
-3 4 -19 13.01 4.45
-4 -4 -19 11.88 4.39
4 4 -19 15.40 4.26
-4 4 -19 8.92 3.93
0 5 -19 -0.24 2.78
0 -5 -19 1.80 2.88
-1 -5 -19 34.43 6.76
1 5 -19 18.39 5.13
-1 -5 19 34.71 6.70
1 -5 -19 32.07 6.28
-1 5 -19 27.63 6.06
-2 -5 -19 1.86 3.15
2 5 -19 3.99 3.54
-2 5 -19 3.13 3.02
-2 -5 19 0.53 2.91
3 5 -19 19.05 4.94
-3 -5 -19 9.59 4.03
-3 -5 19 24.57 5.62
-3 5 -19 17.51 5.13
-4 -5 -19 7.22 3.79
4 5 -19 8.60 4.12
-4 5 -19 2.21 3.46
-4 -5 19 4.51 3.77
0 -6 19 10.59 4.28
0 6 -19 20.06 5.41
0 -6 -19 12.29 4.56
-1 -6 -19 0.25 2.70
1 6 -19 -1.39 2.28
-1 -6 19 -1.06 2.78
-1 6 -19 -1.27 2.35
-2 -6 -19 10.67 4.40
2 6 -19 9.07 4.43
-2 -6 19 9.85 4.04
-2 6 -19 6.78 3.88
3 6 -19 9.35 4.28
-3 -6 -19 10.42 4.44
-3 6 -19 10.46 4.32
-3 -6 19 8.26 3.89
0 7 -19 0.35 2.86
0 -7 19 2.42 3.22
0 -7 -19 -1.76 2.33
1 7 -19 0.75 2.79
-1 -7 -19 0.15 2.93
-1 -7 19 0.41 3.64
-1 7 -19 0.30 2.94
-2 -7 -19 1.04 2.38
2 7 -19 0.67 2.95
-2 7 -19 2.37 3.14
-2 -7 19 4.26 3.61
-3 -7 -19 10.29 4.02
3 7 -19 10.33 4.38
-3 -7 19 18.52 5.66
-3 7 -19 15.71 5.35
0 8 -19 2.05 3.39
0 -8 19 -3.45 2.55
1 8 -19 -1.92 2.46
-1 -8 -19 0.42 2.66
-1 8 -19 -1.91 3.15
-1 -8 19 0.69 3.12
-2 -8 -19 8.70 4.28
2 8 -19 7.24 3.99
-2 8 -19 9.61 4.27
-2 -8 19 9.00 4.54
0 0 -20 16.81 5.14
1 0 -20 -0.76 2.54
-1 0 -20 -1.89 2.21
2 0 -20 8.19 3.96
-2 0 -20 4.74 3.35
-3 0 -20 4.17 3.37
3 0 -20 2.15 2.89
4 0 -20 9.24 4.81
-4 0 -20 6.83 4.30
0 1 -20 5.34 3.63
0 -1 -20 9.12 4.12
1 1 -20 10.13 3.91
-1 -1 -20 10.71 4.22
1 -1 -20 8.73 4.17
-1 1 -20 15.13 4.62
-2 -1 -20 15.56 5.08
2 1 -20 14.12 4.81
-2 1 -20 15.12 5.04
2 -1 -20 8.20 4.02
3 1 -20 3.85 3.17
-3 -1 -20 3.86 3.51
3 -1 -20 5.59 3.54
-3 1 -20 1.22 2.88
4 1 -20 31.85 6.63
-4 -1 -20 30.96 6.62
-4 1 -20 19.11 6.06
4 -1 -20 24.37 6.03
0 -2 -20 0.22 2.26
0 2 -20 2.29 2.62
-1 -2 -20 9.59 4.08
1 2 -20 7.97 3.60
1 -2 -20 2.09 2.92
-1 2 -20 11.89 4.24
-2 -2 -20 2.88 2.81
2 2 -20 6.13 4.05
-2 2 -20 1.09 3.07
2 -2 -20 4.76 3.46
3 2 -20 28.80 6.31
-3 -2 -20 23.65 5.71
3 -2 -20 29.73 6.36
-3 2 -20 25.88 6.40
0 -3 -20 7.08 4.08
0 3 -20 -0.55 2.93
-1 -3 -20 7.82 3.82
1 3 -20 16.66 4.81
-1 3 -20 9.29 4.31
1 -3 -20 10.57 4.58
-2 -3 -20 8.45 4.19
2 3 -20 10.18 4.26
2 -3 -20 4.76 3.75
-2 3 -20 8.50 4.43
-3 -3 -20 9.82 4.28
3 3 -20 11.01 4.24
3 -3 -20 16.81 5.36
-3 3 -20 7.43 4.37
0 -4 -20 3.99 3.17
0 4 -20 -1.24 2.59
-1 -4 -20 3.36 3.16
1 4 -20 3.27 3.32
1 -4 -20 1.68 2.91
-1 -4 20 0.86 2.75
-1 4 -20 3.31 3.41
-2 -4 -20 0.99 3.20
2 4 -20 -0.01 2.58
2 -4 -20 -1.02 3.02
-2 4 -20 2.30 3.32
-3 -4 -20 1.42 2.65
3 4 -20 -2.34 2.42
3 -4 -20 2.50 2.90
-3 4 -20 -1.22 2.54
0 5 -20 -0.29 2.68
0 -5 -20 2.57 2.96
-1 -5 -20 8.25 4.15
1 5 -20 4.99 3.51
1 -5 -20 1.75 3.23
-1 5 -20 5.62 3.86
-1 -5 20 8.65 4.14
-2 -5 -20 5.52 3.81
2 5 -20 8.01 4.02
-2 5 -20 2.55 3.26
-2 -5 20 10.15 4.41
2 -5 -20 2.54 2.84
0 -6 -20 13.62 4.76
0 6 -20 22.20 6.00
-1 -6 -20 6.00 3.52
1 6 -20 8.00 4.61
-1 6 -20 3.57 3.55
1 -6 -20 16.06 5.18
-1 -6 20 9.08 4.10
0 0 -21 0.55 2.90
1 0 -21 1.19 2.73
-1 0 -21 0.71 2.74
0 -1 -21 3.53 3.09
0 1 -21 1.54 3.34
-1 -1 -21 8.28 4.32
1 1 -21 9.54 4.22
1 -1 -21 -0.04 3.11
-1 1 -21 6.23 4.06
0 -2 -21 4.03 3.41
0 2 -21 3.27 3.23
0 0 0 0.00 0.00
;
_shelx_res_checksum 1059
_shelx_res_file
;
TITL AKS03132013_0m in P2(1)2(1)2(1)
CELL 0.71073 10.4473 16.2159 17.587 90 90 90
ZERR 4 0.0002 0.0002 0.0002 0 0 0
LATT -1
SYMM 0.5+X,0.5-Y,-Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5-X,-Y,0.5+Z
SFAC C H N P Cu Ru I
UNIT 84 176 4 12 4 4 4
L.S. 1
PLAN -5 0 0
TEMP -100
HTAB
BOND $H
CONF
fmap 2
acta
REM D:/Documents/My%20Box%20Files/MSU/Data/Xray/AKS03132013/work/AKS03132
REM 013_0m.hkl
WGHT 0.015700
FVAR 0.09648
RU1 6 0.130529 0.462330 0.877450 11.00000 0.02229 0.01971 =
0.02269 -0.00047 0.00036 0.00038
I1 7 0.310079 0.670726 0.725160 11.00000 0.03967 0.05079 =
0.04312 0.00974 0.00625 -0.00936
CU1 5 0.146312 0.596238 0.791969 11.00000 0.02831 0.02881 =
0.03130 0.00486 0.00291 0.00030
P2 4 0.204723 0.352019 0.813223 11.00000 0.03542 0.02884 =
0.02798 -0.00478 -0.00217 0.00561
P3 4 0.017308 0.392979 0.962779 11.00000 0.02844 0.03115 =
0.03374 0.00196 0.00403 -0.00190
P1 4 0.311110 0.472622 0.947597 11.00000 0.02991 0.02737 =
0.03263 0.00217 -0.00517 -0.00343
N1 3 0.015890 0.542832 0.845129 11.00000 0.02500 0.02110 =
0.02374 -0.00116 -0.00034 0.00308
C18 1 0.080077 0.284159 0.777459 11.00000 0.05511 0.04148 =
0.05235 -0.02377 -0.01084 0.00290
AFIX 137
H18A 2 0.116829 0.245974 0.740192 11.00000 -1.50000
H18B 2 0.012958 0.317134 0.753149 11.00000 -1.50000
H18C 2 0.043224 0.252774 0.819747 11.00000 -1.50000
AFIX 0
C16 1 0.280625 0.385590 0.724222 11.00000 0.08310 0.04131 =
0.03227 -0.00393 0.01299 0.00499
AFIX 137
H16A 2 0.307754 0.337154 0.695053 11.00000 -1.50000
H16B 2 0.355377 0.419833 0.735898 11.00000 -1.50000
H16C 2 0.219232 0.417691 0.694239 11.00000 -1.50000
AFIX 0
C17 1 0.320501 0.275527 0.847060 11.00000 0.06258 0.04064 =
0.04135 -0.00561 -0.00494 0.02484
AFIX 137
H17A 2 0.290966 0.252406 0.895462 11.00000 -1.50000
H17B 2 0.403921 0.301998 0.854388 11.00000 -1.50000
H17C 2 0.328553 0.231255 0.809431 11.00000 -1.50000
AFIX 0
C1 1 -0.105358 0.580899 0.845429 11.00000 0.02245 0.02041 =
0.02055 0.01059 -0.00043 -0.00184
C6 1 -0.199808 0.555047 0.792592 11.00000 0.02849 0.02076 =
0.02581 -0.00041 0.01265 -0.00283
C5 1 -0.316930 0.594988 0.792489 11.00000 0.02367 0.02951 =
0.03483 -0.00080 0.00395 0.00014
AFIX 43
H5 2 -0.380541 0.578484 0.757015 11.00000 -1.20000
AFIX 0
C4 1 -0.343359 0.657563 0.842130 11.00000 0.02219 0.03104 =
0.04222 0.00717 0.01132 0.00410
AFIX 43
H4 2 -0.424240 0.684289 0.840667 11.00000 -1.20000
AFIX 0
C3 1 -0.251823 0.681963 0.894654 11.00000 0.03446 0.02148 =
0.03234 0.00227 0.00773 0.00564
AFIX 43
H3 2 -0.271365 0.724748 0.929681 11.00000 -1.20000
AFIX 0
C2 1 -0.132785 0.645073 0.896845 11.00000 0.02864 0.02072 =
0.02523 0.01003 0.00459 -0.00044
C10 1 -0.031849 0.674080 0.953042 11.00000 0.03542 0.02957 =
0.03058 -0.01088 -0.00761 0.01554
AFIX 13
H10 2 0.032891 0.628992 0.958118 11.00000 -1.20000
AFIX 0
C12 1 -0.086215 0.691122 1.032472 11.00000 0.04710 0.03522 =
0.03195 -0.00943 -0.00213 0.00862
AFIX 137
H12A 2 -0.136369 0.742180 1.031430 11.00000 -1.50000
H12B 2 -0.015703 0.696900 1.068834 11.00000 -1.50000
H12C 2 -0.141326 0.645179 1.047926 11.00000 -1.50000
AFIX 0
C11 1 0.037446 0.750130 0.922123 11.00000 0.04761 0.03800 =
0.04916 -0.00590 -0.00965 -0.01483
AFIX 137
H11A 2 0.076667 0.736804 0.873018 11.00000 -1.50000
H11B 2 0.104101 0.767104 0.958071 11.00000 -1.50000
H11C 2 -0.024043 0.795196 0.915473 11.00000 -1.50000
AFIX 0
C7 1 -0.172272 0.485243 0.736804 11.00000 0.02677 0.03176 =
0.03319 -0.00480 -0.00522 0.00541
AFIX 13
H7 2 -0.105022 0.449639 0.760457 11.00000 -1.20000
AFIX 0
C9 1 -0.116048 0.519933 0.663902 11.00000 0.05329 0.07579 =
0.03707 -0.01797 0.01601 -0.00910
AFIX 137
H9A 2 -0.090263 0.474474 0.630533 11.00000 -1.50000
H9B 2 -0.041170 0.553882 0.676017 11.00000 -1.50000
H9C 2 -0.180421 0.553835 0.638102 11.00000 -1.50000
AFIX 0
C8 1 -0.285728 0.430470 0.719971 11.00000 0.05188 0.03906 =
0.04821 -0.00662 -0.00241 -0.00625
AFIX 137
H8A 2 -0.352577 0.462821 0.694705 11.00000 -1.50000
H8B 2 -0.319292 0.407839 0.767637 11.00000 -1.50000
H8C 2 -0.258927 0.385214 0.686649 11.00000 -1.50000
AFIX 0
C19 1 0.067436 0.292399 0.998438 11.00000 0.04558 0.03625 =
0.05434 0.01106 0.01734 -0.01051
AFIX 137
H19A 2 0.002788 0.271234 1.033784 11.00000 -1.50000
H19B 2 0.149518 0.297896 1.024930 11.00000 -1.50000
H19C 2 0.076933 0.254033 0.955754 11.00000 -1.50000
AFIX 0
C21 1 -0.013798 0.448197 1.050886 11.00000 0.05872 0.04276 =
0.04143 0.00453 0.01836 0.00527
AFIX 137
H21A 2 -0.044938 0.503777 1.039197 11.00000 -1.50000
H21B 2 0.065428 0.452045 1.080510 11.00000 -1.50000
H21C 2 -0.078644 0.418520 1.080423 11.00000 -1.50000
AFIX 0
C20 1 -0.146483 0.372062 0.931188 11.00000 0.03156 0.06317 =
0.07601 0.01916 0.01008 -0.01052
AFIX 137
H20A 2 -0.144426 0.335781 0.886641 11.00000 -1.50000
H20B 2 -0.188581 0.424059 0.917733 11.00000 -1.50000
H20C 2 -0.194117 0.345148 0.972281 11.00000 -1.50000
AFIX 0
C14 1 0.459766 0.486411 0.895810 11.00000 0.03647 0.08632 =
0.06332 0.01637 0.00025 -0.01928
AFIX 137
H14A 2 0.446736 0.526252 0.854630 11.00000 -1.50000
H14B 2 0.486945 0.433457 0.874353 11.00000 -1.50000
H14C 2 0.525916 0.506975 0.930471 11.00000 -1.50000
AFIX 0
C15 1 0.362011 0.401052 1.020772 11.00000 0.05241 0.04676 =
0.03368 -0.00184 -0.01033 0.00794
AFIX 137
H15A 2 0.371463 0.345878 0.998738 11.00000 -1.50000
H15B 2 0.297823 0.399477 1.061381 11.00000 -1.50000
H15C 2 0.444265 0.419108 1.041759 11.00000 -1.50000
AFIX 0
C13 1 0.305142 0.568529 1.002277 11.00000 0.07678 0.04658 =
0.07579 -0.01449 -0.04831 -0.00864
AFIX 137
H13A 2 0.379533 0.571458 1.036114 11.00000 -1.50000
H13B 2 0.226485 0.569852 1.032614 11.00000 -1.50000
H13C 2 0.306212 0.615650 0.967391 11.00000 -1.50000
AFIX 0
HKLF 4
REM AKS03132013_0m in P2(1)2(1)2(1)
REM R1 = 0.0425 for 4110 Fo > 4sig(Fo) and 0.0674 for all 5401 data
REM 266 parameters refined using 0 restraints
END
WGHT 0.0157 0.0000
REM Instructions for potential hydrogen bonds
EQIV $1 -x+1/2, -y+1, z+1/2
HTAB C15 I1_$1
REM Highest difference peak 0.473, deepest hole -0.505, 1-sigma level 0.120
Q1 1 0.1781 0.5427 0.8762 11.00000 0.05 0.47
Q2 1 0.2391 0.4124 0.8444 11.00000 0.05 0.45
Q3 1 -0.2433 0.5765 0.7680 11.00000 0.05 0.44
Q4 1 0.3336 0.3991 0.7534 11.00000 0.05 0.44
Q5 1 0.3571 0.3000 0.8782 11.00000 0.05 0.43
;
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number 2013-2
_database_code_depnum_ccdc_archive 'CCDC 957944'
#######################################################################
#
# 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_compd3
_audit_creation_date 2013-05-14
_audit_creation_method
;
Olex2 1.2
(compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C26 H56 N3 P3 Ru'
_chemical_formula_sum 'C26 H54 N3 P3 Ru'
_chemical_formula_weight 602.70
_chemical_absolute_configuration ?
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 7
_space_group_name_H-M_alt 'P 1 n 1'
_space_group_name_Hall 'P -2yac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y, z+1/2'
_cell_length_a 10.1761(14)
_cell_length_b 16.041(2)
_cell_length_c 10.2601(14)
_cell_angle_alpha 90
_cell_angle_beta 109.369(2)
_cell_angle_gamma 90
_cell_volume 1580.0(4)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 5200
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max 21.817
_cell_measurement_theta_min 2.443
_exptl_absorpt_coefficient_mu 0.666
_exptl_absorpt_correction_T_max 0.7452
_exptl_absorpt_correction_T_min 0.6067
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0915 before and 0.0776 after correction.
The Ratio of minimum to maximum transmission is 0.8141.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.267
_exptl_crystal_density_meas .
_exptl_crystal_density_method ?
_exptl_crystal_description ?
_exptl_crystal_F_000 640
_exptl_crystal_size_max ?
_exptl_crystal_size_mid ?
_exptl_crystal_size_min ?
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.1237
_diffrn_reflns_av_unetI/netI 0.1118
_diffrn_reflns_Laue_measured_fraction_full 1.001
_diffrn_reflns_Laue_measured_fraction_max 1.004
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 26237
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.003
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.476
_diffrn_reflns_theta_min 2.104
_diffrn_ambient_temperature 173.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.001
_diffrn_measured_fraction_theta_max 1.004
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.992
_reflns_Friedel_fraction_full 0.999
_reflns_Friedel_fraction_max 1.002
_reflns_number_gt 4413
_reflns_number_total 5843
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement ?
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution ?
_refine_diff_density_max 1.742
_refine_diff_density_min -0.656
_refine_diff_density_rms 0.110
_refine_ls_abs_structure_details
;
Flack x determined using 1750 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack 0.06(3)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.010
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 312
_refine_ls_number_reflns 5843
_refine_ls_number_restraints 2
_refine_ls_R_factor_all 0.0907
_refine_ls_R_factor_gt 0.0579
_refine_ls_restrained_S_all 1.009
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0555P)^2^]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1109
_refine_ls_wR_factor_ref 0.1242
_refine_special_details
;
Refined as a 2-component twin.
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
C12(H12), C15(H15)
2.b Secondary CH2 refined with riding coordinates:
C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B)
2.c Aromatic/amide H refined with riding coordinates:
N2(H2), N3(H3), C8(H8), C9(H9), C10(H10)
2.d Idealised Me refined as rotating group:
C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,
H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru2 Ru 0.19648(8) 0.73515(5) 0.46044(8) 0.0216(2) Uani 1 1 d . . . . .
P1 P 0.0267(3) 0.63857(18) 0.3688(3) 0.0289(8) Uani 1 1 d . . . . .
P2 P 0.0404(3) 0.83763(18) 0.4245(3) 0.0305(8) Uani 1 1 d . . . . .
P3 P 0.2083(3) 0.7118(2) 0.6841(3) 0.0258(8) Uani 1 1 d . . . . .
N1 N 0.5024(8) 0.7577(5) 0.6554(8) 0.0181(19) Uani 1 1 d . . . . .
N2 N 0.3969(10) 0.7498(5) 0.5237(9) 0.028(2) Uani 1 1 d . . . . .
H2 H 0.4307 0.7522 0.4551 0.033 Uiso 1 1 calc R U . . .
N3 N 0.2175(10) 0.7550(6) 0.2573(10) 0.027(2) Uani 1 1 d . . . . .
H3 H 0.1404 0.7666 0.1893 0.032 Uiso 1 1 calc R U . . .
C1 C 0.5578(12) 0.8430(7) 0.6766(12) 0.030(3) Uani 1 1 d . . . . .
H1A H 0.4802 0.8827 0.6642 0.036 Uiso 1 1 calc R U . . .
H1B H 0.6020 0.8558 0.6064 0.036 Uiso 1 1 calc R U . . .
C2 C 0.6618(13) 0.8537(8) 0.8171(12) 0.039(3) Uani 1 1 d . . . . .
H2A H 0.6154 0.8454 0.8869 0.046 Uiso 1 1 calc R U . . .
H2B H 0.6984 0.9114 0.8267 0.046 Uiso 1 1 calc R U . . .
C3 C 0.7826(14) 0.7929(7) 0.8448(14) 0.041(3) Uani 1 1 d . . . . .
H3A H 0.8394 0.8067 0.7859 0.049 Uiso 1 1 calc R U . . .
H3B H 0.8428 0.7966 0.9427 0.049 Uiso 1 1 calc R U . . .
C4 C 0.7247(12) 0.7053(7) 0.8130(12) 0.032(3) Uani 1 1 d . . . . .
H4A H 0.6827 0.6881 0.8831 0.039 Uiso 1 1 calc R U . . .
H4B H 0.8014 0.6662 0.8179 0.039 Uiso 1 1 calc R U . . .
C5 C 0.6153(12) 0.7008(7) 0.6704(12) 0.030(3) Uani 1 1 d . . . . .
H5A H 0.6594 0.7138 0.6000 0.036 Uiso 1 1 calc R U . . .
H5B H 0.5782 0.6433 0.6535 0.036 Uiso 1 1 calc R U . . .
C6 C 0.3373(10) 0.7515(6) 0.2237(10) 0.019(2) Uani 1 1 d . . . . .
C7 C 0.4019(13) 0.6741(7) 0.2108(12) 0.023(3) Uani 1 1 d . . . . .
C8 C 0.5132(12) 0.6721(7) 0.1646(11) 0.028(3) Uani 1 1 d . . . . .
H8 H 0.5521 0.6197 0.1541 0.033 Uiso 1 1 calc R U . . .
C9 C 0.5710(12) 0.7437(7) 0.1327(12) 0.030(3) Uani 1 1 d . . . . .
H9 H 0.6465 0.7410 0.0978 0.036 Uiso 1 1 calc R U . . .
C10 C 0.5159(12) 0.8197(7) 0.1529(11) 0.031(3) Uani 1 1 d . . . . .
H10 H 0.5564 0.8694 0.1329 0.037 Uiso 1 1 calc R U . . .
C11 C 0.4053(12) 0.8262(6) 0.2007(11) 0.024(3) Uani 1 1 d . . . . .
C12 C 0.3436(12) 0.5924(6) 0.2454(11) 0.026(3) Uani 1 1 d . . . . .
H12 H 0.2691 0.6071 0.2851 0.031 Uiso 1 1 calc R U . . .
C13 C 0.2762(14) 0.5406(7) 0.1168(13) 0.042(3) Uani 1 1 d . . . . .
H13A H 0.2018 0.5729 0.0508 0.064 Uiso 1 1 calc R U . . .
H13B H 0.2368 0.4897 0.1420 0.064 Uiso 1 1 calc R U . . .
H13C H 0.3463 0.5255 0.0746 0.064 Uiso 1 1 calc R U . . .
C14 C 0.4545(14) 0.5431(7) 0.3550(13) 0.041(3) Uani 1 1 d . . . . .
H14A H 0.5280 0.5261 0.3183 0.061 Uiso 1 1 calc R U . . .
H14B H 0.4121 0.4934 0.3801 0.061 Uiso 1 1 calc R U . . .
H14C H 0.4948 0.5779 0.4370 0.061 Uiso 1 1 calc R U . . .
C15 C 0.3504(12) 0.9109(6) 0.2217(11) 0.026(3) Uani 1 1 d . . . . .
H15 H 0.3028 0.9038 0.2921 0.032 Uiso 1 1 calc R U . . .
C16 C 0.4656(14) 0.9742(8) 0.2793(14) 0.048(4) Uani 1 1 d . . . . .
H16A H 0.5291 0.9545 0.3684 0.072 Uiso 1 1 calc R U . . .
H16B H 0.4250 1.0277 0.2921 0.072 Uiso 1 1 calc R U . . .
H16C H 0.5172 0.9813 0.2146 0.072 Uiso 1 1 calc R U . . .
C17 C 0.2428(14) 0.9417(7) 0.0923(13) 0.045(4) Uani 1 1 d . . . . .
H17A H 0.2866 0.9526 0.0222 0.068 Uiso 1 1 calc R U . . .
H17B H 0.2014 0.9933 0.1121 0.068 Uiso 1 1 calc R U . . .
H17C H 0.1700 0.8994 0.0579 0.068 Uiso 1 1 calc R U . . .
C18 C -0.1424(12) 0.6326(8) 0.3925(13) 0.037(3) Uani 1 1 d . . . . .
H18A H -0.1977 0.6818 0.3514 0.056 Uiso 1 1 calc R U . . .
H18B H -0.1296 0.6306 0.4915 0.056 Uiso 1 1 calc R U . . .
H18C H -0.1911 0.5822 0.3475 0.056 Uiso 1 1 calc R U . . .
C19 C -0.0338(14) 0.6279(8) 0.1825(13) 0.044(4) Uani 1 1 d . . . . .
H19A H -0.0844 0.5752 0.1564 0.066 Uiso 1 1 calc R U . . .
H19B H 0.0463 0.6283 0.1495 0.066 Uiso 1 1 calc R U . . .
H19C H -0.0959 0.6745 0.1408 0.066 Uiso 1 1 calc R U . . .
C20 C 0.0940(13) 0.5338(7) 0.4266(13) 0.040(3) Uani 1 1 d . . . . .
H20A H 0.0251 0.4920 0.3776 0.060 Uiso 1 1 calc R U . . .
H20B H 0.1121 0.5288 0.5262 0.060 Uiso 1 1 calc R U . . .
H20C H 0.1808 0.5248 0.4068 0.060 Uiso 1 1 calc R U . . .
C21 C 0.1297(14) 0.9365(7) 0.4839(15) 0.048(4) Uani 1 1 d . . . . .
H21A H 0.0610 0.9815 0.4667 0.072 Uiso 1 1 calc R U . . .
H21B H 0.1947 0.9478 0.4337 0.072 Uiso 1 1 calc R U . . .
H21C H 0.1814 0.9330 0.5831 0.072 Uiso 1 1 calc R U . . .
C22 C -0.0636(14) 0.8652(8) 0.2467(13) 0.047(4) Uani 1 1 d . . . . .
H22A H -0.1274 0.8194 0.2050 0.070 Uiso 1 1 calc R U . . .
H22B H -0.0016 0.8751 0.1928 0.070 Uiso 1 1 calc R U . . .
H22C H -0.1174 0.9158 0.2472 0.070 Uiso 1 1 calc R U . . .
C23 C -0.0942(13) 0.8441(7) 0.5034(14) 0.042(3) Uani 1 1 d . . . . .
H23A H -0.0512 0.8504 0.6036 0.062 Uiso 1 1 calc R U . . .
H23B H -0.1504 0.7931 0.4833 0.062 Uiso 1 1 calc R U . . .
H23C H -0.1540 0.8923 0.4659 0.062 Uiso 1 1 calc R U . . .
C24 C 0.2636(14) 0.7990(8) 0.8073(13) 0.044(3) Uani 1 1 d . . . . .
H24A H 0.2884 0.7776 0.9019 0.066 Uiso 1 1 calc R U . . .
H24B H 0.1872 0.8391 0.7904 0.066 Uiso 1 1 calc R U . . .
H24C H 0.3447 0.8266 0.7951 0.066 Uiso 1 1 calc R U . . .
C25 C 0.0601(14) 0.6748(9) 0.7304(13) 0.041(4) Uani 1 1 d . . . . .
H25A H 0.0299 0.6204 0.6872 0.062 Uiso 1 1 calc R U . . .
H25B H -0.0168 0.7147 0.6979 0.062 Uiso 1 1 calc R U . . .
H25C H 0.0874 0.6693 0.8310 0.062 Uiso 1 1 calc R U . . .
C26 C 0.3311(14) 0.6312(8) 0.7701(12) 0.038(3) Uani 1 1 d . . . . .
H26A H 0.3427 0.6310 0.8688 0.058 Uiso 1 1 calc R U . . .
H26B H 0.4212 0.6422 0.7581 0.058 Uiso 1 1 calc R U . . .
H26C H 0.2960 0.5769 0.7299 0.058 Uiso 1 1 calc R U . . .
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
Ru2 0.0280(5) 0.0127(3) 0.0253(4) 0.0006(6) 0.0106(3) -0.0011(6)
P1 0.0294(19) 0.0175(16) 0.0365(19) 0.0017(13) 0.0065(15) -0.0029(13)
P2 0.040(2) 0.0184(17) 0.0395(19) 0.0036(14) 0.0221(17) 0.0076(14)
P3 0.0294(19) 0.0259(17) 0.0236(18) 0.0028(14) 0.0110(15) 0.0012(15)
N1 0.018(5) 0.014(5) 0.018(5) -0.001(3) 0.001(4) -0.001(4)
N2 0.041(6) 0.023(6) 0.017(5) -0.004(4) 0.008(4) 0.000(4)
N3 0.027(6) 0.030(6) 0.025(6) 0.004(5) 0.009(5) 0.005(5)
C1 0.033(8) 0.024(7) 0.033(7) -0.006(5) 0.009(6) -0.006(6)
C2 0.044(9) 0.037(8) 0.033(7) -0.011(6) 0.010(6) -0.007(6)
C3 0.044(9) 0.044(7) 0.034(8) -0.007(6) 0.012(6) -0.011(7)
C4 0.032(7) 0.031(7) 0.035(7) -0.002(5) 0.012(6) 0.008(5)
C5 0.038(8) 0.021(6) 0.035(7) -0.002(5) 0.016(6) 0.002(5)
C6 0.018(6) 0.026(7) 0.010(5) -0.002(4) 0.001(4) 0.002(4)
C7 0.033(7) 0.013(6) 0.027(7) -0.008(5) 0.013(6) 0.000(5)
C8 0.032(7) 0.028(7) 0.026(7) -0.005(5) 0.011(6) 0.006(5)
C9 0.028(7) 0.038(8) 0.025(7) 0.009(5) 0.009(6) 0.006(6)
C10 0.036(8) 0.027(7) 0.030(7) 0.004(5) 0.012(6) 0.001(6)
C11 0.038(7) 0.009(5) 0.026(6) 0.001(4) 0.013(6) -0.003(5)
C12 0.039(8) 0.014(6) 0.026(6) 0.001(5) 0.013(6) 0.002(5)
C13 0.057(9) 0.026(7) 0.040(8) -0.014(6) 0.011(7) -0.006(6)
C14 0.058(10) 0.025(7) 0.036(8) -0.002(6) 0.012(7) 0.004(6)
C15 0.036(7) 0.015(6) 0.029(7) 0.000(5) 0.012(6) 0.001(5)
C16 0.062(10) 0.030(8) 0.057(10) -0.013(6) 0.025(8) -0.010(7)
C17 0.072(12) 0.029(8) 0.037(8) 0.002(6) 0.021(8) 0.012(7)
C18 0.030(8) 0.035(7) 0.045(8) 0.006(6) 0.010(6) -0.010(6)
C19 0.049(9) 0.037(8) 0.048(9) -0.005(6) 0.019(7) -0.012(6)
C20 0.051(9) 0.016(6) 0.048(8) 0.001(5) 0.011(7) -0.008(6)
C21 0.057(10) 0.016(6) 0.085(11) 0.007(6) 0.044(9) 0.005(6)
C22 0.047(9) 0.053(9) 0.038(8) 0.017(6) 0.009(7) 0.019(7)
C23 0.051(9) 0.026(7) 0.058(9) 0.006(6) 0.032(8) 0.013(6)
C24 0.048(9) 0.049(8) 0.036(8) -0.014(6) 0.016(7) 0.007(7)
C25 0.040(9) 0.056(10) 0.035(8) 0.015(7) 0.021(7) 0.012(7)
C26 0.045(9) 0.045(8) 0.021(7) 0.010(6) 0.006(6) 0.003(6)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru2 P1 2.279(3) . ?
Ru2 P2 2.230(3) . ?
Ru2 P3 2.288(3) . ?
Ru2 N2 1.939(10) . ?
Ru2 N3 2.188(10) . ?
P1 C18 1.818(12) . ?
P1 C19 1.812(13) . ?
P1 C20 1.837(11) . ?
P2 C21 1.829(12) . ?
P2 C22 1.834(12) . ?
P2 C23 1.811(12) . ?
P3 C24 1.844(12) . ?
P3 C25 1.825(13) . ?
P3 C26 1.811(12) . ?
N1 N2 1.426(12) . ?
N1 C1 1.467(13) . ?
N1 C5 1.435(14) . ?
N2 H2 0.8800 . ?
N3 H3 0.8800 . ?
N3 C6 1.373(14) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.488(15) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.520(17) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.516(16) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.518(15) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.432(14) . ?
C6 C11 1.442(14) . ?
C7 C8 1.366(15) . ?
C7 C12 1.528(15) . ?
C8 H8 0.9500 . ?
C8 C9 1.378(15) . ?
C9 H9 0.9500 . ?
C9 C10 1.386(15) . ?
C10 H10 0.9500 . ?
C10 C11 1.373(15) . ?
C11 C15 1.511(14) . ?
C12 H12 1.0000 . ?
C12 C13 1.518(15) . ?
C12 C14 1.524(15) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15 1.0000 . ?
C15 C16 1.515(16) . ?
C15 C17 1.497(16) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 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
P1 Ru2 P3 94.76(12) . . ?
P2 Ru2 P1 91.83(12) . . ?
P2 Ru2 P3 94.85(12) . . ?
N2 Ru2 P1 142.2(3) . . ?
N2 Ru2 P2 125.3(2) . . ?
N2 Ru2 P3 89.1(3) . . ?
N2 Ru2 N3 82.9(4) . . ?
N3 Ru2 P1 90.4(3) . . ?
N3 Ru2 P2 91.4(3) . . ?
N3 Ru2 P3 171.8(3) . . ?
C18 P1 Ru2 127.0(4) . . ?
C18 P1 C20 100.2(6) . . ?
C19 P1 Ru2 116.4(4) . . ?
C19 P1 C18 97.5(6) . . ?
C19 P1 C20 102.4(6) . . ?
C20 P1 Ru2 109.8(4) . . ?
C21 P2 Ru2 109.6(4) . . ?
C21 P2 C22 100.5(6) . . ?
C22 P2 Ru2 119.1(4) . . ?
C23 P2 Ru2 124.8(4) . . ?
C23 P2 C21 99.6(6) . . ?
C23 P2 C22 99.1(6) . . ?
C24 P3 Ru2 117.8(5) . . ?
C25 P3 Ru2 122.8(5) . . ?
C25 P3 C24 99.1(7) . . ?
C26 P3 Ru2 113.8(4) . . ?
C26 P3 C24 101.7(6) . . ?
C26 P3 C25 97.9(6) . . ?
N2 N1 C1 110.8(8) . . ?
N2 N1 C5 111.7(8) . . ?
C5 N1 C1 108.8(9) . . ?
Ru2 N2 H2 112.6 . . ?
N1 N2 Ru2 134.9(7) . . ?
N1 N2 H2 112.6 . . ?
Ru2 N3 H3 116.3 . . ?
C6 N3 Ru2 127.5(8) . . ?
C6 N3 H3 116.3 . . ?
N1 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
N1 C1 C2 111.5(9) . . ?
H1A C1 H1B 108.0 . . ?
C2 C1 H1A 109.3 . . ?
C2 C1 H1B 109.3 . . ?
C1 C2 H2A 109.2 . . ?
C1 C2 H2B 109.2 . . ?
C1 C2 C3 112.2(10) . . ?
H2A C2 H2B 107.9 . . ?
C3 C2 H2A 109.2 . . ?
C3 C2 H2B 109.2 . . ?
C2 C3 H3A 109.9 . . ?
C2 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?
C4 C3 C2 108.8(10) . . ?
C4 C3 H3A 109.9 . . ?
C4 C3 H3B 109.9 . . ?
C3 C4 H4A 109.4 . . ?
C3 C4 H4B 109.4 . . ?
C3 C4 C5 111.1(10) . . ?
H4A C4 H4B 108.0 . . ?
C5 C4 H4A 109.4 . . ?
C5 C4 H4B 109.4 . . ?
N1 C5 C4 112.2(9) . . ?
N1 C5 H5A 109.2 . . ?
N1 C5 H5B 109.2 . . ?
C4 C5 H5A 109.2 . . ?
C4 C5 H5B 109.2 . . ?
H5A C5 H5B 107.9 . . ?
N3 C6 C7 122.1(9) . . ?
N3 C6 C11 121.4(9) . . ?
C7 C6 C11 116.5(10) . . ?
C6 C7 C12 119.8(10) . . ?
C8 C7 C6 120.7(10) . . ?
C8 C7 C12 119.4(10) . . ?
C7 C8 H8 118.9 . . ?
C7 C8 C9 122.1(10) . . ?
C9 C8 H8 118.9 . . ?
C8 C9 H9 120.9 . . ?
C8 C9 C10 118.2(11) . . ?
C10 C9 H9 120.9 . . ?
C9 C10 H10 118.7 . . ?
C11 C10 C9 122.7(11) . . ?
C11 C10 H10 118.7 . . ?
C6 C11 C15 120.2(10) . . ?
C10 C11 C6 119.4(9) . . ?
C10 C11 C15 120.3(9) . . ?
C7 C12 H12 107.3 . . ?
C13 C12 C7 111.5(9) . . ?
C13 C12 H12 107.3 . . ?
C13 C12 C14 111.5(9) . . ?
C14 C12 C7 111.5(10) . . ?
C14 C12 H12 107.3 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 H15 106.9 . . ?
C11 C15 C16 112.5(10) . . ?
C16 C15 H15 106.9 . . ?
C17 C15 C11 111.5(9) . . ?
C17 C15 H15 106.9 . . ?
C17 C15 C16 111.6(10) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
P1 C18 H18A 109.5 . . ?
P1 C18 H18B 109.5 . . ?
P1 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
P1 C19 H19A 109.5 . . ?
P1 C19 H19B 109.5 . . ?
P1 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
P1 C20 H20A 109.5 . . ?
P1 C20 H20B 109.5 . . ?
P1 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
P2 C21 H21A 109.5 . . ?
P2 C21 H21B 109.5 . . ?
P2 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
P2 C22 H22A 109.5 . . ?
P2 C22 H22B 109.5 . . ?
P2 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
P2 C23 H23A 109.5 . . ?
P2 C23 H23B 109.5 . . ?
P2 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
P3 C24 H24A 109.5 . . ?
P3 C24 H24B 109.5 . . ?
P3 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
P3 C25 H25A 109.5 . . ?
P3 C25 H25B 109.5 . . ?
P3 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
P3 C26 H26A 109.5 . . ?
P3 C26 H26B 109.5 . . ?
P3 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 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
Ru2 N3 C6 C7 75.5(12) . . . . ?
Ru2 N3 C6 C11 -104.0(10) . . . . ?
N1 C1 C2 C3 57.5(14) . . . . ?
N2 N1 C1 C2 176.5(9) . . . . ?
N2 N1 C5 C4 -176.9(9) . . . . ?
N3 C6 C7 C8 173.7(11) . . . . ?
N3 C6 C7 C12 -4.7(16) . . . . ?
N3 C6 C11 C10 -173.0(10) . . . . ?
N3 C6 C11 C15 3.7(15) . . . . ?
C1 N1 N2 Ru2 -109.6(9) . . . . ?
C1 N1 C5 C4 60.5(12) . . . . ?
C1 C2 C3 C4 -52.1(14) . . . . ?
C2 C3 C4 C5 51.1(13) . . . . ?
C3 C4 C5 N1 -57.7(13) . . . . ?
C5 N1 N2 Ru2 129.0(9) . . . . ?
C5 N1 C1 C2 -60.4(12) . . . . ?
C6 C7 C8 C9 2.1(17) . . . . ?
C6 C7 C12 C13 110.6(12) . . . . ?
C6 C7 C12 C14 -123.9(11) . . . . ?
C6 C11 C15 C16 144.8(10) . . . . ?
C6 C11 C15 C17 -89.0(13) . . . . ?
C7 C6 C11 C10 7.5(15) . . . . ?
C7 C6 C11 C15 -175.8(10) . . . . ?
C7 C8 C9 C10 2.1(17) . . . . ?
C8 C7 C12 C13 -67.8(14) . . . . ?
C8 C7 C12 C14 57.7(14) . . . . ?
C8 C9 C10 C11 -1.2(17) . . . . ?
C9 C10 C11 C6 -3.7(17) . . . . ?
C9 C10 C11 C15 179.6(10) . . . . ?
C10 C11 C15 C16 -38.5(15) . . . . ?
C10 C11 C15 C17 87.7(13) . . . . ?
C11 C6 C7 C8 -6.8(16) . . . . ?
C11 C6 C7 C12 174.8(9) . . . . ?
C12 C7 C8 C9 -179.5(10) . . . . ?
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_shelx_hkl_checksum 91422
_shelx_hkl_file
;
1 0 0 0.46 0.42
1 0 0 0.05 0.45
-1 0 0 0.33 0.52
-1 0 0 -0.11 0.60
1 0 0 0.90 0.56
-2 0 0 31.91 2.47
-2 0 0 29.15 2.45
2 0 0 30.07 2.18
2 0 0 28.11 1.96
2 0 0 29.96 2.24
3 0 0 -0.94 1.15
3 0 0 -1.27 1.04
-3 0 0 -0.12 1.35
-3 0 0 0.83 1.56
3 0 0 0.05 1.26
-4 0 0 64.66 4.57
4 0 0 57.77 3.84
4 0 0 60.42 3.89
-4 0 0 58.61 4.18
4 0 0 61.19 3.70
-5 0 0 0.59 1.81
-5 0 0 0.04 1.80
5 0 0 1.77 1.72
5 0 0 -2.35 1.27
5 0 0 -2.08 1.28
6 0 0 166.49 8.01
6 0 0 149.82 7.91
6 0 0 166.45 7.66
-6 0 0 149.73 8.83
-6 0 0 162.16 8.76
-7 0 0 -1.81 2.09
-7 0 0 -0.24 2.54
7 0 0 -4.17 1.60
7 0 0 0.37 1.73
7 0 0 -0.09 1.91
8 0 0 24.20 3.82
8 0 0 27.59 4.54
-8 0 0 28.28 4.92
8 0 0 20.21 3.74
-8 0 0 23.30 4.56
-9 0 0 3.69 3.80
9 0 0 -3.85 2.46
9 0 0 0.60 2.74
-9 0 0 0.13 3.07
-10 0 0 19.75 5.75
10 0 0 7.18 3.63
10 0 0 11.67 4.06
11 0 0 1.82 3.62
11 0 0 0.97 3.67
-11 0 0 -3.00 4.74
1 -1 0 366.87 12.06
-1 -1 0 346.21 12.64
1 -1 0 350.96 12.73
-1 -1 0 353.01 13.04
1 -1 0 366.97 12.48
-1 -1 0 347.37 12.22
1 -1 0 370.84 12.60
1 1 0 368.52 12.09
1 1 0 363.25 12.40
1 1 0 364.17 12.39
-1 1 0 335.43 12.72
-2 -1 0 1.89 0.78
2 -1 0 1.15 0.98
-2 -1 0 -0.30 1.24
2 -1 0 3.04 1.01
2 -1 0 2.47 1.21
-2 -1 0 1.29 1.31
2 1 0 2.88 1.11
-2 1 0 1.10 0.96
2 1 0 2.40 1.09
-2 1 0 0.26 1.22
2 1 0 2.31 0.94
3 -1 0 89.21 4.23
-3 -1 0 76.99 4.65
3 -1 0 89.48 4.42
-3 -1 0 75.09 3.50
-3 -1 0 82.74 4.76
3 -1 0 81.21 4.20
-3 1 0 92.85 4.53
-3 1 0 82.78 4.76
3 1 0 85.37 4.26
3 1 0 81.12 4.26
3 1 0 82.89 4.07
4 -1 0 4.30 1.71
-4 -1 0 2.31 0.90
-4 -1 0 5.35 1.98
4 -1 0 5.22 1.64
4 -1 0 4.24 1.50
-4 -1 0 1.67 1.85
-4 1 0 3.68 1.93
-4 1 0 4.92 1.88
4 1 0 2.84 1.53
4 1 0 1.04 1.44
4 1 0 4.22 1.46
5 -1 0 112.26 5.69
-5 -1 0 112.17 6.71
-5 -1 0 108.81 4.36
-5 -1 0 108.25 6.64
5 -1 0 112.96 5.98
5 -1 0 114.51 6.17
-5 1 0 110.82 6.27
5 1 0 116.13 5.98
5 1 0 111.53 5.99
5 1 0 111.86 5.65
-5 1 0 113.78 6.82
-6 -1 0 3.99 2.39
6 -1 0 4.09 2.12
6 -1 0 0.20 1.74
-6 -1 0 2.33 2.17
6 -1 0 1.27 1.72
6 1 0 -0.61 1.48
-6 1 0 4.00 2.09
-6 1 0 2.80 2.22
6 1 0 2.70 1.96
6 1 0 1.08 1.62
-7 -1 0 73.64 6.29
7 -1 0 69.11 5.09
7 -1 0 75.70 5.76
7 -1 0 72.08 5.42
-7 -1 0 77.28 6.48
-7 1 0 75.58 6.55
7 1 0 65.94 4.99
7 1 0 78.12 5.55
-7 1 0 72.33 5.83
7 1 0 63.43 5.22
-8 -1 0 4.36 3.15
8 -1 0 0.83 2.27
-8 -1 0 8.38 3.50
8 -1 0 -0.40 2.31
8 -1 0 4.37 2.55
8 1 0 1.23 2.51
8 1 0 1.08 2.06
-8 1 0 0.46 2.63
-8 1 0 2.32 3.01
8 1 0 -1.59 2.03
-9 -1 0 22.43 4.85
9 -1 0 20.57 4.20
-9 -1 0 14.43 4.61
9 -1 0 15.73 4.01
9 1 0 23.82 4.37
-9 1 0 18.74 4.80
9 1 0 16.37 4.01
-9 1 0 13.85 4.30
-10 -1 0 -3.94 3.48
10 -1 0 2.50 3.32
-10 -1 0 5.80 4.34
10 -1 0 2.57 2.97
10 1 0 3.62 3.32
10 1 0 2.63 3.37
-10 1 0 1.07 3.76
11 -1 0 6.91 3.93
-11 -1 0 6.44 4.92
11 -1 0 17.54 4.92
-11 1 0 12.96 5.69
11 1 0 10.32 4.21
11 1 0 5.67 3.89
0 -2 0 1000.00 32.59
0 -2 0 961.93 33.82
0 -2 0 968.56 31.86
0 -2 0 987.45 33.00
0 2 0 973.78 31.87
0 2 0 924.34 32.97
-1 -2 0 28.36 1.84
1 -2 0 24.98 1.86
1 -2 0 25.73 1.85
-1 -2 0 27.31 2.10
1 -2 0 25.35 1.92
-1 -2 0 26.30 1.63
1 -2 0 28.60 1.80
-1 -2 0 26.72 1.95
1 -2 0 26.98 1.89
-1 2 0 28.73 1.88
1 2 0 27.12 1.59
1 2 0 26.58 1.77
1 2 0 25.45 1.84
-2 -2 0 116.39 4.90
2 -2 0 116.99 5.14
2 -2 0 105.07 4.46
2 -2 0 125.88 5.32
2 -2 0 124.45 4.98
-2 -2 0 111.76 5.69
-2 -2 0 115.08 5.20
2 2 0 124.00 5.10
2 2 0 117.17 4.87
2 2 0 121.18 4.99
-2 2 0 121.56 5.54
-2 2 0 121.59 4.95
3 -2 0 4.35 1.37
-3 -2 0 4.21 1.82
-3 -2 0 4.07 1.20
3 -2 0 5.91 1.67
3 -2 0 8.01 1.61
-3 -2 0 4.34 1.77
3 2 0 5.78 1.40
3 2 0 6.35 1.50
3 2 0 4.00 1.48
-3 2 0 6.03 1.81
-3 2 0 6.43 1.41
-4 -2 0 79.93 5.14
-4 -2 0 76.52 5.23
4 -2 0 80.76 4.55
4 -2 0 78.22 4.76
-4 -2 0 77.80 3.80
4 -2 0 85.57 4.58
-4 2 0 85.13 4.64
4 2 0 71.04 4.50
-4 2 0 67.66 5.01
4 2 0 76.52 4.23
4 2 0 76.57 4.32
5 -2 0 11.16 2.13
-5 -2 0 13.45 2.89
-5 -2 0 11.32 1.77
-5 -2 0 14.85 2.77
5 -2 0 14.67 2.68
5 -2 0 12.75 2.48
5 2 0 12.37 2.14
-5 2 0 13.58 2.83
-5 2 0 12.88 2.41
5 2 0 13.36 2.40
5 2 0 8.56 2.18
6 -2 0 134.57 6.76
6 -2 0 111.73 6.73
-6 -2 0 124.76 7.70
6 -2 0 124.25 7.07
-6 -2 0 131.94 7.92
-6 2 0 131.23 7.90
6 2 0 116.13 6.75
-6 2 0 124.03 7.08
6 2 0 124.48 6.75
6 2 0 124.07 6.37
-7 -2 0 1.16 2.59
7 -2 0 3.65 2.40
-7 -2 0 1.91 2.58
7 -2 0 1.62 2.14
7 -2 0 6.77 2.34
7 2 0 1.63 1.97
-7 2 0 6.89 2.77
-7 2 0 3.63 2.66
7 2 0 0.13 2.00
7 2 0 1.06 1.86
8 -2 0 20.17 3.95
-8 -2 0 26.94 4.94
-8 -2 0 20.18 4.87
8 -2 0 16.67 3.52
8 -2 0 27.20 4.15
8 2 0 21.62 3.79
-8 2 0 15.37 3.77
8 2 0 20.70 3.86
-8 2 0 27.76 4.99
8 2 0 25.07 3.95
-9 -2 0 4.16 4.08
9 -2 0 6.54 2.95
9 -2 0 1.65 2.89
-9 -2 0 4.00 3.74
9 -2 0 3.16 2.89
-9 2 0 3.00 3.22
9 2 0 4.73 3.25
9 2 0 1.62 2.91
-10 -2 0 22.83 5.55
10 -2 0 24.63 4.91
-10 -2 0 29.14 5.93
10 -2 0 25.46 4.98
10 2 0 27.12 5.08
-10 2 0 25.94 5.85
10 2 0 14.94 4.28
11 -2 0 -2.93 3.00
-11 -2 0 5.25 4.95
-11 -2 0 -1.87 4.74
11 -2 0 -1.66 3.77
11 2 0 2.11 3.66
-11 2 0 6.42 4.91
0 -3 0 10.00 1.57
0 -3 0 13.79 1.62
0 -3 0 13.44 1.60
0 -3 0 14.13 1.81
0 3 0 9.51 1.52
0 3 0 12.79 1.48
1 -3 0 78.00 3.86
-1 -3 0 78.63 3.77
1 -3 0 80.81 3.34
-1 -3 0 70.83 4.06
1 -3 0 77.91 3.83
1 -3 0 82.19 3.58
-1 -3 0 67.60 3.80
-1 -3 0 75.52 3.17
1 -3 0 77.43 3.71
1 -3 0 79.93 3.71
-1 3 0 81.39 3.56
-1 3 0 75.76 3.88
1 3 0 75.14 3.69
1 3 0 79.85 3.42
2 -3 0 18.62 1.70
2 -3 0 20.03 2.26
-2 -3 0 18.35 2.12
2 -3 0 20.36 1.94
-2 -3 0 19.87 2.26
2 -3 0 16.70 2.35
2 -3 0 16.29 2.15
-2 -3 0 18.99 2.60
2 3 0 20.78 2.37
-2 3 0 19.61 1.74
-2 3 0 23.91 2.41
2 3 0 23.71 2.28
2 3 0 18.11 1.85
3 -3 0 159.53 6.79
3 -3 0 151.77 6.13
3 -3 0 158.90 7.22
-3 -3 0 153.00 7.70
-3 -3 0 166.96 7.23
-3 -3 0 162.97 6.72
3 -3 0 164.18 7.04
3 3 0 168.12 6.89
3 3 0 163.22 6.63
3 3 0 160.08 6.89
-3 3 0 145.80 7.33
-3 3 0 164.96 6.73
4 -3 0 14.88 2.51
-4 -3 0 15.08 2.53
-4 -3 0 18.25 3.18
4 -3 0 15.99 2.70
4 -3 0 11.19 1.34
-4 -3 0 10.34 1.82
4 -3 0 15.30 2.45
-4 3 0 14.94 2.15
4 3 0 13.01 2.22
-4 3 0 14.33 2.64
4 3 0 17.07 2.40
4 3 0 16.18 2.39
-5 -3 0 106.40 6.62
5 -3 0 99.33 5.99
-5 -3 0 102.39 6.28
5 -3 0 92.67 5.44
5 -3 0 97.35 5.52
-5 -3 0 96.32 4.90
5 3 0 104.32 5.76
-5 3 0 100.52 5.59
5 3 0 101.77 5.37
-5 3 0 99.18 6.45
5 3 0 103.05 5.44
6 -3 0 14.56 2.94
-6 -3 0 13.89 3.16
6 -3 0 17.49 2.92
-6 -3 0 19.00 3.59
6 -3 0 16.29 2.98
6 3 0 17.70 3.01
-6 3 0 20.34 3.72
6 3 0 15.36 2.76
6 3 0 17.59 2.97
-6 3 0 18.54 3.19
7 -3 0 37.89 4.71
-7 -3 0 32.60 4.67
7 -3 0 33.65 4.28
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AFIX 23
H4A 2 0.682706 0.688079 0.883144 11.00000 -1.20000
H4B 2 0.801417 0.666171 0.817926 11.00000 -1.20000
AFIX 0
C5 1 0.615328 0.700786 0.670370 11.00000 0.03800 0.02147 =
0.03456 -0.00212 0.01598 0.00174
AFIX 23
H5A 2 0.659400 0.713767 0.600026 11.00000 -1.20000
H5B 2 0.578189 0.643290 0.653457 11.00000 -1.20000
AFIX 0
C6 1 0.337310 0.751524 0.223729 11.00000 0.01778 0.02608 =
0.01004 -0.00182 0.00095 0.00176
C7 1 0.401922 0.674096 0.210802 11.00000 0.03259 0.01281 =
0.02713 -0.00757 0.01291 0.00004
C8 1 0.513235 0.672143 0.164607 11.00000 0.03172 0.02759 =
0.02560 -0.00467 0.01111 0.00559
AFIX 43
H8 2 0.552086 0.619748 0.154120 11.00000 -1.20000
AFIX 0
C9 1 0.571026 0.743723 0.132711 11.00000 0.02794 0.03762 =
0.02494 0.00866 0.00874 0.00564
AFIX 43
H9 2 0.646517 0.741045 0.097823 11.00000 -1.20000
AFIX 0
C10 1 0.515939 0.819748 0.152949 11.00000 0.03577 0.02701 =
0.03047 0.00430 0.01247 0.00090
AFIX 43
H10 2 0.556410 0.869410 0.132937 11.00000 -1.20000
AFIX 0
C11 1 0.405322 0.826208 0.200717 11.00000 0.03824 0.00947 =
0.02564 0.00113 0.01323 -0.00285
C12 1 0.343618 0.592411 0.245398 11.00000 0.03896 0.01418 =
0.02594 0.00109 0.01316 0.00198
AFIX 13
H12 2 0.269150 0.607090 0.285071 11.00000 -1.20000
AFIX 0
C13 1 0.276173 0.540551 0.116811 11.00000 0.05749 0.02608 =
0.04008 -0.01410 0.01124 -0.00556
AFIX 137
H13A 2 0.201836 0.572904 0.050807 11.00000 -1.50000
H13B 2 0.236804 0.489734 0.141992 11.00000 -1.50000
H13C 2 0.346326 0.525525 0.074598 11.00000 -1.50000
AFIX 0
C14 1 0.454510 0.543056 0.354981 11.00000 0.05829 0.02461 =
0.03588 -0.00219 0.01157 0.00378
AFIX 137
H14A 2 0.527954 0.526106 0.318324 11.00000 -1.50000
H14B 2 0.412129 0.493399 0.380068 11.00000 -1.50000
H14C 2 0.494753 0.577929 0.437014 11.00000 -1.50000
AFIX 0
C15 1 0.350365 0.910871 0.221698 11.00000 0.03580 0.01500 =
0.02944 -0.00014 0.01201 0.00082
AFIX 13
H15 2 0.302849 0.903805 0.292096 11.00000 -1.20000
AFIX 0
C16 1 0.465594 0.974170 0.279269 11.00000 0.06233 0.02961 =
0.05660 -0.01326 0.02467 -0.00991
AFIX 137
H16A 2 0.529051 0.954511 0.368356 11.00000 -1.50000
H16B 2 0.425031 1.027679 0.292078 11.00000 -1.50000
H16C 2 0.517235 0.981264 0.214613 11.00000 -1.50000
AFIX 0
C17 1 0.242792 0.941724 0.092300 11.00000 0.07179 0.02858 =
0.03682 0.00245 0.02071 0.01228
AFIX 137
H17A 2 0.286613 0.952641 0.022153 11.00000 -1.50000
H17B 2 0.201371 0.993301 0.112122 11.00000 -1.50000
H17C 2 0.169985 0.899424 0.057933 11.00000 -1.50000
AFIX 0
C18 1 -0.142398 0.632614 0.392532 11.00000 0.03036 0.03460 =
0.04549 0.00627 0.01047 -0.00983
AFIX 137
H18A 2 -0.197656 0.681837 0.351394 11.00000 -1.50000
H18B 2 -0.129572 0.630569 0.491456 11.00000 -1.50000
H18C 2 -0.191095 0.582225 0.347518 11.00000 -1.50000
AFIX 0
C19 1 -0.033773 0.627929 0.182513 11.00000 0.04930 0.03655 =
0.04849 -0.00473 0.01894 -0.01207
AFIX 137
H19A 2 -0.084412 0.575228 0.156416 11.00000 -1.50000
H19B 2 0.046257 0.628339 0.149547 11.00000 -1.50000
H19C 2 -0.095867 0.674466 0.140786 11.00000 -1.50000
AFIX 0
C20 1 0.094046 0.533842 0.426581 11.00000 0.05122 0.01644 =
0.04812 0.00068 0.01133 -0.00773
AFIX 137
H20A 2 0.025143 0.492038 0.377554 11.00000 -1.50000
H20B 2 0.112127 0.528763 0.526198 11.00000 -1.50000
H20C 2 0.180810 0.524849 0.406800 11.00000 -1.50000
AFIX 0
C21 1 0.129744 0.936468 0.483887 11.00000 0.05687 0.01606 =
0.08516 0.00745 0.04356 0.00511
AFIX 137
H21A 2 0.061047 0.981524 0.466702 11.00000 -1.50000
H21B 2 0.194676 0.947829 0.433716 11.00000 -1.50000
H21C 2 0.181384 0.933016 0.583089 11.00000 -1.50000
AFIX 0
C22 1 -0.063613 0.865186 0.246675 11.00000 0.04654 0.05255 =
0.03818 0.01661 0.00949 0.01871
AFIX 137
H22A 2 -0.127417 0.819364 0.205025 11.00000 -1.50000
H22B 2 -0.001630 0.875129 0.192780 11.00000 -1.50000
H22C 2 -0.117383 0.915792 0.247204 11.00000 -1.50000
AFIX 0
C23 1 -0.094243 0.844123 0.503358 11.00000 0.05111 0.02626 =
0.05765 0.00575 0.03185 0.01295
AFIX 137
H23A 2 -0.051160 0.850441 0.603557 11.00000 -1.50000
H23B 2 -0.150417 0.793123 0.483315 11.00000 -1.50000
H23C 2 -0.154017 0.892322 0.465902 11.00000 -1.50000
AFIX 0
C24 1 0.263633 0.799009 0.807329 11.00000 0.04794 0.04855 =
0.03623 -0.01397 0.01553 0.00665
AFIX 137
H24A 2 0.288410 0.777631 0.901901 11.00000 -1.50000
H24B 2 0.187175 0.839141 0.790447 11.00000 -1.50000
H24C 2 0.344696 0.826597 0.795139 11.00000 -1.50000
AFIX 0
C25 1 0.060064 0.674758 0.730409 11.00000 0.04003 0.05551 =
0.03499 0.01470 0.02125 0.01181
AFIX 137
H25A 2 0.029939 0.620413 0.687191 11.00000 -1.50000
H25B 2 -0.016757 0.714722 0.697886 11.00000 -1.50000
H25C 2 0.087400 0.669251 0.831024 11.00000 -1.50000
AFIX 0
C26 1 0.331136 0.631207 0.770054 11.00000 0.04502 0.04488 =
0.02143 0.00950 0.00567 0.00269
AFIX 137
H26A 2 0.342722 0.630962 0.868763 11.00000 -1.50000
H26B 2 0.421177 0.642188 0.758072 11.00000 -1.50000
H26C 2 0.295955 0.576859 0.729853 11.00000 -1.50000
AFIX 0
HKLF 4
REM aks1 in Pn
REM R1 = 0.0579 for 4413 Fo > 4sig(Fo) and 0.0907 for all 5843 data
REM 312 parameters refined using 2 restraints
END
WGHT 0.0553 0.0000
REM Instructions for potential hydrogen bonds
HTAB C19 N3
HTAB C26 N1
REM Highest difference peak 1.742, deepest hole -0.656, 1-sigma level 0.110
Q1 1 0.0970 0.7376 0.3683 11.00000 0.05 1.74
Q2 1 0.2945 0.7380 0.5550 11.00000 0.05 1.37
Q3 1 0.2971 0.7409 0.4285 11.00000 0.05 0.67
Q4 1 0.1960 0.7669 0.4617 11.00000 0.05 0.65
Q5 1 0.2151 0.7716 0.3404 11.00000 0.05 0.60
Q6 1 0.0686 0.6885 0.4335 11.00000 0.05 0.59
Q7 1 0.1419 0.6972 0.5640 11.00000 0.05 0.58
Q8 1 0.1346 0.8204 0.5056 11.00000 0.05 0.57
Q9 1 0.1868 0.7744 0.5762 11.00000 0.05 0.57
Q10 1 0.1396 0.6420 0.4855 11.00000 0.05 0.55
Q11 1 0.2417 0.6890 0.3639 11.00000 0.05 0.52
Q12 1 0.3265 0.7675 0.3359 11.00000 0.05 0.52
;
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number 2013-2
_database_code_depnum_ccdc_archive 'CCDC 957945'
#######################################################################
#
# 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_compd5
_audit_creation_date 2013-06-03
_audit_creation_method
;
Olex2 1.2
(compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C28 H49 N2 O P3 Ru, C7 H8'
_chemical_formula_sum 'C35 H57 N2 O P3 Ru'
_chemical_formula_weight 715.83
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 10.4066(7)
_cell_length_b 21.1342(15)
_cell_length_c 17.1162(12)
_cell_angle_alpha 90
_cell_angle_beta 95.0540(10)
_cell_angle_gamma 90
_cell_volume 3749.8(5)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 4269
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max 25.25
_cell_measurement_theta_min 2.19
_exptl_absorpt_coefficient_mu 0.574
_exptl_absorpt_correction_T_max 1
_exptl_absorpt_correction_T_min 0.687942
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
For component 1:
wR2(int) was 0.0643 before and 0.0582 after correction.
The Ratio of minimum to maximum transmission is 0.93.
The \l/2 correction factor is Not present
For component 2:
wR2(int) was 0.1063 before and 0.0631 after correction.
The Ratio of minimum to maximum transmission not present.
The \l/2 correction factor is Not present
Final HKLF 4 output contains 84247 reflections, Rint = 0.0861
(24631 with I > 3sig(I), Rint = 0.0485)
;
_exptl_crystal_colour red
_exptl_crystal_colour_lustre ?
_exptl_crystal_colour_modifier ?
_exptl_crystal_colour_primary red
_exptl_crystal_density_diffrn 1.268
_exptl_crystal_density_meas .
_exptl_crystal_density_method ?
_exptl_crystal_description ?
_exptl_crystal_F_000 1512
_exptl_crystal_size_max 0.172
_exptl_crystal_size_mid 0.166
_exptl_crystal_size_min 0.128
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents ?
_diffrn_reflns_av_unetI/netI 0.0591
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 25
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 12583
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.422
_diffrn_reflns_theta_min 1.927
_diffrn_ambient_temperature 173.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 9968
_reflns_number_total 12583
_reflns_special_details
;
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement ?
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution ?
_refine_diff_density_max 0.405
_refine_diff_density_min -0.356
_refine_diff_density_rms 0.074
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.029
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 394
_refine_ls_number_reflns 12583
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0600
_refine_ls_R_factor_gt 0.0392
_refine_ls_restrained_S_all 1.029
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0286P)^2^+1.4614P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0719
_refine_ls_wR_factor_ref 0.0786
_refine_special_details
;
Refined as a 2-component twin.
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
C10(H10), C7(H7)
2.b Aromatic/amide H refined with riding coordinates:
C32(H32), C33(H33), C34(H34), C30(H30), C31(H31), C24(H24), C25(H25),
C26(H26), C27(H27), C28(H28), C5(H5), C4(H4), C3(H3)
2.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C35(H35A,H35B,H35C), C20(H20A,H20B,H20C), C21(H21A,H21B,
H21C), C19(H19A,H19B,H19C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C15(H15A,
H15B,H15C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C),
C11(H11A,H11B,H11C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.47553(3) 0.17544(2) 0.03323(2) 0.01869(8) Uani 1 1 d . . . . .
P3 P 0.45003(9) 0.24517(4) 0.13082(6) 0.0253(2) Uani 1 1 d . . . . .
P1 P 0.38657(9) 0.09328(4) 0.08865(6) 0.0270(2) Uani 1 1 d . . . . .
P2 P 0.28824(9) 0.19703(5) -0.03693(6) 0.0277(2) Uani 1 1 d . . . . .
O1 O 0.5559(2) 0.12280(10) -0.05792(13) 0.0236(6) Uani 1 1 d . . . . .
N2 N 0.7754(3) 0.14104(13) -0.07573(17) 0.0236(7) Uani 1 1 d . . . . .
N1 N 0.6652(3) 0.18926(12) 0.02191(16) 0.0216(7) Uani 1 1 d . . . . .
C12 C 0.8621(4) 0.1350(2) 0.2436(2) 0.0611(14) Uani 1 1 d . . . . .
H12A H 0.9566 0.1338 0.2503 0.092 Uiso 1 1 calc R U . . .
H12B H 0.8274 0.0958 0.2640 0.092 Uiso 1 1 calc R U . . .
H12C H 0.8312 0.1713 0.2724 0.092 Uiso 1 1 calc R U . . .
C32 C 0.7733(7) 0.5618(2) 0.0036(3) 0.0743(18) Uani 1 1 d . . . . .
H32 H 0.7715 0.5858 -0.0433 0.089 Uiso 1 1 calc R U . . .
C33 C 0.6631(6) 0.5380(2) 0.0292(3) 0.0721(16) Uani 1 1 d . . . . .
H33 H 0.5828 0.5464 0.0003 0.087 Uiso 1 1 calc R U . . .
C34 C 0.6659(5) 0.5020(2) 0.0960(3) 0.0597(14) Uani 1 1 d . . . . .
H34 H 0.5877 0.4860 0.1129 0.072 Uiso 1 1 calc R U . . .
C29 C 0.7810(4) 0.48880(19) 0.1386(3) 0.0435(11) Uani 1 1 d . . . . .
C35 C 0.7858(5) 0.4479(2) 0.2099(3) 0.0596(14) Uani 1 1 d . . . . .
H35A H 0.7259 0.4124 0.2004 0.089 Uiso 1 1 calc R U . . .
H35B H 0.7609 0.4729 0.2544 0.089 Uiso 1 1 calc R U . . .
H35C H 0.8736 0.4317 0.2216 0.089 Uiso 1 1 calc R U . . .
C30 C 0.8891(5) 0.5143(3) 0.1140(4) 0.084(2) Uani 1 1 d . . . . .
H30 H 0.9697 0.5075 0.1433 0.101 Uiso 1 1 calc R U . . .
C31 C 0.8834(6) 0.5503(3) 0.0463(5) 0.111(3) Uani 1 1 d . . . . .
H31 H 0.9610 0.5674 0.0298 0.133 Uiso 1 1 calc R U . . .
C20 C 0.5150(4) 0.32322(17) 0.1127(2) 0.0438(11) Uani 1 1 d . . . . .
H20A H 0.6070 0.3196 0.1053 0.066 Uiso 1 1 calc R U . . .
H20B H 0.5037 0.3508 0.1575 0.066 Uiso 1 1 calc R U . . .
H20C H 0.4692 0.3413 0.0653 0.066 Uiso 1 1 calc R U . . .
C21 C 0.5373(4) 0.2274(2) 0.2251(2) 0.0419(11) Uani 1 1 d . . . . .
H21A H 0.5213 0.2608 0.2627 0.063 Uiso 1 1 calc R U . . .
H21B H 0.6299 0.2250 0.2189 0.063 Uiso 1 1 calc R U . . .
H21C H 0.5077 0.1867 0.2444 0.063 Uiso 1 1 calc R U . . .
C19 C 0.2924(3) 0.26759(18) 0.1605(2) 0.0337(10) Uani 1 1 d . . . . .
H19A H 0.2478 0.2299 0.1775 0.050 Uiso 1 1 calc R U . . .
H19B H 0.2413 0.2870 0.1160 0.050 Uiso 1 1 calc R U . . .
H19C H 0.3034 0.2979 0.2038 0.050 Uiso 1 1 calc R U . . .
C14 C 0.3212(4) 0.03325(17) 0.0205(3) 0.0427(11) Uani 1 1 d . . . . .
H14A H 0.3185 -0.0075 0.0477 0.064 Uiso 1 1 calc R U . . .
H14B H 0.3760 0.0295 -0.0229 0.064 Uiso 1 1 calc R U . . .
H14C H 0.2337 0.0453 0.0000 0.064 Uiso 1 1 calc R U . . .
C13 C 0.5124(4) 0.04910(18) 0.1464(2) 0.0422(11) Uani 1 1 d . . . . .
H13A H 0.5424 0.0736 0.1931 0.063 Uiso 1 1 calc R U . . .
H13B H 0.5848 0.0415 0.1146 0.063 Uiso 1 1 calc R U . . .
H13C H 0.4775 0.0085 0.1623 0.063 Uiso 1 1 calc R U . . .
C15 C 0.2659(4) 0.09851(19) 0.1590(2) 0.0404(11) Uani 1 1 d . . . . .
H15A H 0.2403 0.0558 0.1736 0.061 Uiso 1 1 calc R U . . .
H15B H 0.1903 0.1214 0.1353 0.061 Uiso 1 1 calc R U . . .
H15C H 0.3021 0.1211 0.2058 0.061 Uiso 1 1 calc R U . . .
C17 C 0.1247(3) 0.18462(19) -0.0097(2) 0.0401(11) Uani 1 1 d . . . . .
H17A H 0.1106 0.1394 -0.0012 0.060 Uiso 1 1 calc R U . . .
H17B H 0.0626 0.1999 -0.0518 0.060 Uiso 1 1 calc R U . . .
H17C H 0.1129 0.2079 0.0387 0.060 Uiso 1 1 calc R U . . .
C16 C 0.2810(4) 0.1571(2) -0.1316(2) 0.0467(12) Uani 1 1 d . . . . .
H16A H 0.2782 0.1112 -0.1235 0.070 Uiso 1 1 calc R U . . .
H16B H 0.3575 0.1680 -0.1582 0.070 Uiso 1 1 calc R U . . .
H16C H 0.2033 0.1705 -0.1638 0.070 Uiso 1 1 calc R U . . .
C18 C 0.2789(4) 0.27957(19) -0.0663(3) 0.0515(13) Uani 1 1 d . . . . .
H18A H 0.2079 0.2852 -0.1073 0.077 Uiso 1 1 calc R U . . .
H18B H 0.3602 0.2922 -0.0866 0.077 Uiso 1 1 calc R U . . .
H18C H 0.2634 0.3059 -0.0209 0.077 Uiso 1 1 calc R U . . .
C22 C 0.6694(3) 0.14965(15) -0.0418(2) 0.0203(8) Uani 1 1 d . . . . .
C23 C 0.7795(3) 0.10640(15) -0.1444(2) 0.0213(8) Uani 1 1 d . . . . .
C24 C 0.8966(3) 0.07771(17) -0.1575(2) 0.0327(10) Uani 1 1 d . . . . .
H24 H 0.9666 0.0807 -0.1181 0.039 Uiso 1 1 calc R U . . .
C25 C 0.9139(4) 0.04516(18) -0.2257(2) 0.0368(10) Uani 1 1 d . . . . .
H25 H 0.9949 0.0263 -0.2326 0.044 Uiso 1 1 calc R U . . .
C26 C 0.8145(4) 0.03997(17) -0.2836(2) 0.0337(10) Uani 1 1 d . . . . .
H26 H 0.8260 0.0174 -0.3305 0.040 Uiso 1 1 calc R U . . .
C27 C 0.6971(4) 0.06813(17) -0.2726(2) 0.0325(10) Uani 1 1 d . . . . .
H27 H 0.6280 0.0652 -0.3126 0.039 Uiso 1 1 calc R U . . .
C28 C 0.6793(3) 0.10032(16) -0.2042(2) 0.0269(9) Uani 1 1 d . . . . .
H28 H 0.5977 0.1187 -0.1976 0.032 Uiso 1 1 calc R U . . .
C1 C 0.7719(3) 0.22623(16) 0.0524(2) 0.0235(9) Uani 1 1 d . . . . .
C6 C 0.7980(3) 0.28447(17) 0.0180(2) 0.0294(9) Uani 1 1 d . . . . .
C5 C 0.8938(4) 0.32276(19) 0.0562(3) 0.0408(10) Uani 1 1 d . . . . .
H5 H 0.9128 0.3626 0.0342 0.049 Uiso 1 1 calc R U . . .
C4 C 0.9607(4) 0.3037(2) 0.1249(3) 0.0452(12) Uani 1 1 d . . . . .
H4 H 1.0245 0.3307 0.1501 0.054 Uiso 1 1 calc R U . . .
C3 C 0.9363(3) 0.2461(2) 0.1574(2) 0.0386(10) Uani 1 1 d . . . . .
H3 H 0.9840 0.2335 0.2047 0.046 Uiso 1 1 calc R U . . .
C2 C 0.8429(3) 0.20610(18) 0.1220(2) 0.0271(9) Uani 1 1 d . . . . .
C10 C 0.8173(4) 0.14160(19) 0.1564(2) 0.0345(10) Uani 1 1 d . . . . .
H10 H 0.7216 0.1354 0.1512 0.041 Uiso 1 1 calc R U . . .
C11 C 0.8746(4) 0.08841(18) 0.1109(2) 0.0397(11) Uani 1 1 d . . . . .
H11A H 0.8471 0.0930 0.0549 0.059 Uiso 1 1 calc R U . . .
H11B H 0.8448 0.0476 0.1296 0.059 Uiso 1 1 calc R U . . .
H11C H 0.9690 0.0903 0.1187 0.059 Uiso 1 1 calc R U . . .
C7 C 0.7265(4) 0.30572(18) -0.0585(2) 0.0401(11) Uani 1 1 d . . . . .
H7 H 0.6458 0.2800 -0.0669 0.048 Uiso 1 1 calc R U . . .
C8 C 0.6877(4) 0.3758(2) -0.0595(3) 0.0594(14) Uani 1 1 d . . . . .
H8A H 0.6307 0.3846 -0.1069 0.089 Uiso 1 1 calc R U . . .
H8B H 0.7652 0.4021 -0.0591 0.089 Uiso 1 1 calc R U . . .
H8C H 0.6424 0.3852 -0.0130 0.089 Uiso 1 1 calc R U . . .
C9 C 0.8074(5) 0.2928(2) -0.1269(3) 0.0728(17) Uani 1 1 d . . . . .
H9A H 0.8849 0.3194 -0.1217 0.109 Uiso 1 1 calc R U . . .
H9B H 0.7566 0.3027 -0.1764 0.109 Uiso 1 1 calc R U . . .
H9C H 0.8327 0.2482 -0.1266 0.109 Uiso 1 1 calc R U . . .
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 0.01813(14) 0.01912(14) 0.01909(14) -0.00206(14) 0.00316(12) -0.00181(13)
P3 0.0226(5) 0.0287(5) 0.0252(5) -0.0083(4) 0.0061(4) -0.0028(4)
P1 0.0249(5) 0.0244(5) 0.0321(6) 0.0027(4) 0.0043(5) -0.0046(4)
P2 0.0268(5) 0.0314(6) 0.0242(6) -0.0025(5) -0.0009(5) 0.0047(4)
O1 0.0217(13) 0.0251(13) 0.0243(14) -0.0093(11) 0.0043(10) -0.0034(11)
N2 0.0213(16) 0.0262(17) 0.0237(18) -0.0084(14) 0.0046(14) -0.0009(13)
N1 0.0215(15) 0.0242(17) 0.0198(17) -0.0038(13) 0.0051(13) -0.0057(12)
C12 0.062(3) 0.088(4) 0.033(3) 0.011(3) -0.001(2) 0.010(3)
C32 0.133(6) 0.039(3) 0.055(4) 0.010(3) 0.028(4) 0.015(4)
C33 0.099(5) 0.061(4) 0.052(4) 0.011(3) -0.018(3) -0.003(3)
C34 0.055(3) 0.065(3) 0.056(3) 0.000(3) -0.012(3) -0.011(3)
C29 0.056(3) 0.033(3) 0.043(3) -0.002(2) 0.011(2) 0.003(2)
C35 0.072(3) 0.057(3) 0.050(3) 0.005(3) 0.002(3) -0.005(3)
C30 0.048(3) 0.092(4) 0.115(5) 0.059(4) 0.022(3) 0.012(3)
C31 0.080(5) 0.099(5) 0.163(8) 0.069(5) 0.063(5) 0.018(4)
C20 0.042(2) 0.034(2) 0.058(3) -0.021(2) 0.020(2) -0.007(2)
C21 0.032(2) 0.066(3) 0.028(2) -0.016(2) 0.0003(18) 0.003(2)
C19 0.029(2) 0.037(2) 0.036(3) -0.013(2) 0.0081(19) -0.0002(18)
C14 0.048(3) 0.024(2) 0.056(3) -0.002(2) 0.001(2) -0.0083(19)
C13 0.040(2) 0.034(2) 0.052(3) 0.015(2) 0.001(2) -0.0040(19)
C15 0.036(2) 0.044(3) 0.043(3) 0.006(2) 0.012(2) -0.011(2)
C17 0.027(2) 0.050(3) 0.043(3) -0.012(2) -0.0002(19) 0.0038(19)
C16 0.043(3) 0.063(3) 0.032(3) -0.012(2) -0.008(2) 0.015(2)
C18 0.063(3) 0.042(3) 0.047(3) 0.012(2) -0.010(2) 0.011(2)
C22 0.0229(19) 0.0176(18) 0.020(2) 0.0010(16) -0.0021(17) -0.0016(15)
C23 0.0223(19) 0.0201(19) 0.022(2) 0.0010(16) 0.0054(16) -0.0028(15)
C24 0.024(2) 0.042(2) 0.032(2) -0.0045(19) 0.0051(18) 0.0021(18)
C25 0.035(2) 0.041(2) 0.036(3) -0.003(2) 0.015(2) 0.009(2)
C26 0.050(3) 0.028(2) 0.025(2) -0.0046(18) 0.014(2) 0.003(2)
C27 0.038(2) 0.033(2) 0.026(2) -0.0021(18) 0.0026(19) -0.0051(19)
C28 0.024(2) 0.026(2) 0.030(2) -0.0013(18) 0.0066(18) 0.0020(16)
C1 0.0187(18) 0.030(2) 0.024(2) -0.0121(17) 0.0103(16) -0.0021(16)
C6 0.028(2) 0.025(2) 0.037(3) -0.0066(18) 0.0152(18) -0.0052(17)
C5 0.031(2) 0.029(2) 0.065(3) -0.013(2) 0.018(2) -0.008(2)
C4 0.019(2) 0.050(3) 0.067(3) -0.035(3) 0.005(2) -0.0101(19)
C3 0.024(2) 0.053(3) 0.038(3) -0.020(2) -0.0006(19) -0.002(2)
C2 0.0181(19) 0.037(2) 0.027(2) -0.0076(18) 0.0050(17) -0.0004(17)
C10 0.019(2) 0.052(3) 0.032(2) 0.008(2) -0.0010(18) -0.0030(19)
C11 0.036(2) 0.037(2) 0.044(3) 0.008(2) -0.003(2) 0.0022(19)
C7 0.047(3) 0.035(2) 0.040(3) 0.006(2) 0.012(2) -0.010(2)
C8 0.072(3) 0.047(3) 0.063(4) 0.014(3) 0.027(3) 0.009(3)
C9 0.129(5) 0.049(3) 0.045(3) 0.004(3) 0.031(3) 0.005(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 P3 2.2606(10) . ?
Ru1 P1 2.2196(10) . ?
Ru1 P2 2.2442(10) . ?
Ru1 O1 2.145(2) . ?
Ru1 N1 2.022(3) . ?
Ru1 C22 2.545(3) . ?
P3 C20 1.820(4) . ?
P3 C21 1.820(4) . ?
P3 C19 1.822(3) . ?
P1 C14 1.814(4) . ?
P1 C13 1.826(4) . ?
P1 C15 1.818(4) . ?
P2 C17 1.823(4) . ?
P2 C16 1.823(4) . ?
P2 C18 1.816(4) . ?
O1 C22 1.318(4) . ?
N2 C22 1.304(4) . ?
N2 C23 1.388(4) . ?
N1 C22 1.379(4) . ?
N1 C1 1.419(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C12 C10 1.530(5) . ?
C32 H32 0.9500 . ?
C32 C33 1.360(7) . ?
C32 C31 1.325(8) . ?
C33 H33 0.9500 . ?
C33 C34 1.370(6) . ?
C34 H34 0.9500 . ?
C34 C29 1.374(6) . ?
C29 C35 1.492(6) . ?
C29 C30 1.349(6) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C30 H30 0.9500 . ?
C30 C31 1.383(8) . ?
C31 H31 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C23 C24 1.396(5) . ?
C23 C28 1.402(5) . ?
C24 H24 0.9500 . ?
C24 C25 1.381(5) . ?
C25 H25 0.9500 . ?
C25 C26 1.372(5) . ?
C26 H26 0.9500 . ?
C26 C27 1.387(5) . ?
C27 H27 0.9500 . ?
C27 C28 1.381(5) . ?
C28 H28 0.9500 . ?
C1 C6 1.402(5) . ?
C1 C2 1.411(5) . ?
C6 C5 1.400(5) . ?
C6 C7 1.515(5) . ?
C5 H5 0.9500 . ?
C5 C4 1.373(6) . ?
C4 H4 0.9500 . ?
C4 C3 1.370(5) . ?
C3 H3 0.9500 . ?
C3 C2 1.387(5) . ?
C2 C10 1.518(5) . ?
C10 H10 1.0000 . ?
C10 C11 1.520(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C7 H7 1.0000 . ?
C7 C8 1.534(5) . ?
C7 C9 1.526(6) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 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
P3 Ru1 C22 131.50(8) . . ?
P1 Ru1 P3 96.53(4) . . ?
P1 Ru1 P2 90.72(4) . . ?
P1 Ru1 C22 115.30(8) . . ?
P2 Ru1 P3 96.31(4) . . ?
P2 Ru1 C22 117.60(8) . . ?
O1 Ru1 P3 162.60(6) . . ?
O1 Ru1 P1 96.26(7) . . ?
O1 Ru1 P2 95.28(6) . . ?
O1 Ru1 C22 31.18(9) . . ?
N1 Ru1 P3 98.96(8) . . ?
N1 Ru1 P1 126.98(8) . . ?
N1 Ru1 P2 136.77(9) . . ?
N1 Ru1 O1 63.82(9) . . ?
N1 Ru1 C22 32.67(10) . . ?
C20 P3 Ru1 113.27(13) . . ?
C20 P3 C19 99.74(17) . . ?
C21 P3 Ru1 116.01(13) . . ?
C21 P3 C20 100.08(19) . . ?
C21 P3 C19 101.42(18) . . ?
C19 P3 Ru1 122.85(12) . . ?
C14 P1 Ru1 114.79(14) . . ?
C14 P1 C13 101.56(19) . . ?
C14 P1 C15 103.07(19) . . ?
C13 P1 Ru1 108.97(12) . . ?
C15 P1 Ru1 125.02(14) . . ?
C15 P1 C13 100.21(19) . . ?
C17 P2 Ru1 128.33(14) . . ?
C16 P2 Ru1 110.33(13) . . ?
C16 P2 C17 101.20(19) . . ?
C18 P2 Ru1 111.50(15) . . ?
C18 P2 C17 100.4(2) . . ?
C18 P2 C16 101.6(2) . . ?
C22 O1 Ru1 91.40(19) . . ?
C22 N2 C23 122.7(3) . . ?
C22 N1 Ru1 95.01(19) . . ?
C22 N1 C1 123.2(3) . . ?
C1 N1 Ru1 141.6(2) . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
C33 C32 H32 121.1 . . ?
C31 C32 H32 121.1 . . ?
C31 C32 C33 117.9(5) . . ?
C32 C33 H33 119.4 . . ?
C32 C33 C34 121.1(5) . . ?
C34 C33 H33 119.4 . . ?
C33 C34 H34 119.7 . . ?
C33 C34 C29 120.6(5) . . ?
C29 C34 H34 119.7 . . ?
C34 C29 C35 121.1(4) . . ?
C30 C29 C34 117.7(5) . . ?
C30 C29 C35 121.2(5) . . ?
C29 C35 H35A 109.5 . . ?
C29 C35 H35B 109.5 . . ?
C29 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C29 C30 H30 119.8 . . ?
C29 C30 C31 120.4(5) . . ?
C31 C30 H30 119.8 . . ?
C32 C31 C30 122.3(6) . . ?
C32 C31 H31 118.9 . . ?
C30 C31 H31 118.9 . . ?
P3 C20 H20A 109.5 . . ?
P3 C20 H20B 109.5 . . ?
P3 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
P3 C21 H21A 109.5 . . ?
P3 C21 H21B 109.5 . . ?
P3 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
P3 C19 H19A 109.5 . . ?
P3 C19 H19B 109.5 . . ?
P3 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
P1 C14 H14A 109.5 . . ?
P1 C14 H14B 109.5 . . ?
P1 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
P1 C13 H13A 109.5 . . ?
P1 C13 H13B 109.5 . . ?
P1 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
P1 C15 H15A 109.5 . . ?
P1 C15 H15B 109.5 . . ?
P1 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
P2 C17 H17A 109.5 . . ?
P2 C17 H17B 109.5 . . ?
P2 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
P2 C16 H16A 109.5 . . ?
P2 C16 H16B 109.5 . . ?
P2 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
P2 C18 H18A 109.5 . . ?
P2 C18 H18B 109.5 . . ?
P2 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O1 C22 Ru1 57.42(16) . . ?
O1 C22 N1 109.7(3) . . ?
N2 C22 Ru1 173.9(3) . . ?
N2 C22 O1 128.7(3) . . ?
N2 C22 N1 121.6(3) . . ?
N1 C22 Ru1 52.32(15) . . ?
N2 C23 C24 117.2(3) . . ?
N2 C23 C28 126.2(3) . . ?
C24 C23 C28 116.5(3) . . ?
C23 C24 H24 118.9 . . ?
C25 C24 C23 122.2(4) . . ?
C25 C24 H24 118.9 . . ?
C24 C25 H25 119.9 . . ?
C26 C25 C24 120.3(4) . . ?
C26 C25 H25 119.9 . . ?
C25 C26 H26 120.5 . . ?
C25 C26 C27 119.0(4) . . ?
C27 C26 H26 120.5 . . ?
C26 C27 H27 119.6 . . ?
C28 C27 C26 120.8(4) . . ?
C28 C27 H27 119.6 . . ?
C23 C28 H28 119.4 . . ?
C27 C28 C23 121.2(3) . . ?
C27 C28 H28 119.4 . . ?
C6 C1 N1 120.2(3) . . ?
C6 C1 C2 120.9(3) . . ?
C2 C1 N1 118.6(3) . . ?
C1 C6 C7 121.7(3) . . ?
C5 C6 C1 117.9(4) . . ?
C5 C6 C7 120.5(4) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 C6 121.1(4) . . ?
C4 C5 H5 119.5 . . ?
C5 C4 H4 119.7 . . ?
C3 C4 C5 120.7(4) . . ?
C3 C4 H4 119.7 . . ?
C4 C3 H3 119.6 . . ?
C4 C3 C2 120.8(4) . . ?
C2 C3 H3 119.6 . . ?
C1 C2 C10 120.1(3) . . ?
C3 C2 C1 118.6(4) . . ?
C3 C2 C10 121.3(4) . . ?
C12 C10 H10 106.9 . . ?
C2 C10 C12 114.3(3) . . ?
C2 C10 H10 106.9 . . ?
C2 C10 C11 112.0(3) . . ?
C11 C10 C12 109.5(3) . . ?
C11 C10 H10 106.9 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C6 C7 H7 107.8 . . ?
C6 C7 C8 113.8(4) . . ?
C6 C7 C9 110.3(4) . . ?
C8 C7 H7 107.8 . . ?
C9 C7 H7 107.8 . . ?
C9 C7 C8 109.0(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 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
Ru1 O1 C22 N2 -179.6(3) . . . . ?
Ru1 O1 C22 N1 3.0(3) . . . . ?
Ru1 N1 C22 O1 -3.1(3) . . . . ?
Ru1 N1 C22 N2 179.2(3) . . . . ?
Ru1 N1 C1 C6 -90.0(4) . . . . ?
Ru1 N1 C1 C2 84.0(4) . . . . ?
N2 C23 C24 C25 -176.2(3) . . . . ?
N2 C23 C28 C27 175.4(3) . . . . ?
N1 C1 C6 C5 171.9(3) . . . . ?
N1 C1 C6 C7 -8.6(5) . . . . ?
N1 C1 C2 C3 -171.8(3) . . . . ?
N1 C1 C2 C10 8.7(5) . . . . ?
C32 C33 C34 C29 -0.3(8) . . . . ?
C33 C32 C31 C30 1.4(10) . . . . ?
C33 C34 C29 C35 -178.0(4) . . . . ?
C33 C34 C29 C30 2.3(8) . . . . ?
C34 C29 C30 C31 -2.5(9) . . . . ?
C29 C30 C31 C32 0.7(11) . . . . ?
C35 C29 C30 C31 177.8(5) . . . . ?
C31 C32 C33 C34 -1.5(9) . . . . ?
C22 N2 C23 C24 -153.4(3) . . . . ?
C22 N2 C23 C28 30.4(5) . . . . ?
C22 N1 C1 C6 82.4(4) . . . . ?
C22 N1 C1 C2 -103.5(4) . . . . ?
C23 N2 C22 O1 9.2(6) . . . . ?
C23 N2 C22 N1 -173.6(3) . . . . ?
C23 C24 C25 C26 -0.1(6) . . . . ?
C24 C23 C28 C27 -0.7(5) . . . . ?
C24 C25 C26 C27 0.3(6) . . . . ?
C25 C26 C27 C28 -0.8(6) . . . . ?
C26 C27 C28 C23 1.0(6) . . . . ?
C28 C23 C24 C25 0.2(5) . . . . ?
C1 N1 C22 Ru1 -175.3(4) . . . . ?
C1 N1 C22 O1 -178.4(3) . . . . ?
C1 N1 C22 N2 3.9(5) . . . . ?
C1 C6 C5 C4 0.4(5) . . . . ?
C1 C6 C7 C8 138.1(4) . . . . ?
C1 C6 C7 C9 -98.9(4) . . . . ?
C1 C2 C10 C12 -159.1(3) . . . . ?
C1 C2 C10 C11 75.7(4) . . . . ?
C6 C1 C2 C3 2.2(5) . . . . ?
C6 C1 C2 C10 -177.3(3) . . . . ?
C6 C5 C4 C3 0.8(6) . . . . ?
C5 C6 C7 C8 -42.5(5) . . . . ?
C5 C6 C7 C9 80.5(4) . . . . ?
C5 C4 C3 C2 -0.5(6) . . . . ?
C4 C3 C2 C1 -0.9(5) . . . . ?
C4 C3 C2 C10 178.5(3) . . . . ?
C3 C2 C10 C12 21.4(5) . . . . ?
C3 C2 C10 C11 -103.8(4) . . . . ?
C2 C1 C6 C5 -2.0(5) . . . . ?
C2 C1 C6 C7 177.5(3) . . . . ?
C7 C6 C5 C4 -179.0(4) . . . . ?
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_shelx_hkl_checksum 22846
_shelx_hkl_file
;
1 0 0 0.29714 0.70064 2
1 0 0 1.18104 0.61735 1
2 0 0 538.704 7.33186 1
2 0 0 378.163 6.35029 2
-3 0 1 556.204 14.3029 -2
3 0 0 556.204 14.3029 1
3 0 0 -0.4643 1.90966 1
3 0 0 0.22242 1.65660 2
-4 0 1 1047.07 20.0228 -2
4 0 0 1047.07 20.0228 1
4 0 0 1031.97 20.7283 1
4 0 0 711.497 15.2635 2
5 0 0 -1.4151 1.85465 2
5 0 0 -1.4577 1.83134 1
6 0 0 144.826 7.34785 2
-6 0 2 218.494 12.7327 -2
6 0 0 218.494 12.7327 1
6 0 0 221.801 10.9522 1
-7 0 2 2.20080 2.96910 -2
7 0 0 2.20080 2.96910 1
8 0 0 -2.3205 3.27362 1
8 0 0 -0.9296 2.71090 2
-8 0 2 2.39792 9.80803 -2
8 0 0 2.39792 9.80803 1
9 0 0 1.70031 4.03739 1
9 0 0 -2.0052 3.60789 2
-10 0 3 17.1615 8.16021 -2
10 0 0 17.1615 8.16021 1
-11 0 3 14.3993 10.8130 -2
11 0 0 14.3993 10.8130 1
12 0 0 176.258 16.7751 1
12 0 0 130.686 13.7969 2
1 1 0 1047.25 7.67179 1
1 1 0 739.322 5.83957 2
2 1 0 2184.09 15.0030 1
2 1 0 1526.43 11.1868 2
3 1 0 217.146 5.07616 1
3 1 0 155.320 3.92173 2
-3 1 1 1059.56 15.3211 -2
3 1 0 1059.56 15.3211 1
4 1 0 33.9387 3.50350 1
-4 1 1 118.524 4.89003 -2
4 1 0 118.524 4.89003 1
4 1 0 22.6316 2.59916 2
5 1 0 130.599 3.95890 1
5 1 0 89.9075 3.49610 2
-6 1 2 1884.23 28.2647 -2
6 1 0 1884.23 28.2647 1
6 1 0 874.566 12.8540 2
6 1 0 1222.41 19.1924 1
-7 1 2 40.7048 3.45178 -2
7 1 0 40.7048 3.45178 1
8 1 0 11.3186 2.94132 1
8 1 0 8.60939 2.55396 2
-8 1 2 48.6826 11.6049 -2
8 1 0 48.6826 11.6049 1
9 1 0 15.9045 3.64844 2
9 1 0 30.8238 4.34088 1
-10 1 3 473.512 13.2247 -2
10 1 0 473.512 13.2247 1
-11 1 3 122.019 10.9524 -2
11 1 0 122.019 10.9524 1
12 1 0 16.9446 6.26740 1
12 1 0 40.5236 6.32811 2
0 2 0 4097.18 41.0430 -2
0 2 0 4097.18 41.0430 1
1 2 0 33.5944 1.21465 1
1 2 0 22.5833 1.05094 2
2 2 0 356.554 3.61492 2
2 2 0 506.864 4.75083 1
3 2 0 18.4918 1.47613 2
-3 2 1 534.220 9.49928 -2
3 2 0 534.220 9.49928 1
3 2 0 31.4548 1.92808 1
-4 2 1 1385.42 18.6754 -2
4 2 0 1385.42 18.6754 1
4 2 0 922.631 11.3050 2
4 2 0 1333.93 12.3789 1
5 2 0 272.113 4.81880 2
5 2 0 396.386 5.91867 1
6 2 0 40.2435 3.56364 1
-6 2 2 76.1019 7.35807 -2
6 2 0 76.1019 7.35807 1
6 2 0 28.5466 2.92593 2
-7 2 2 133.371 5.02290 -2
7 2 0 133.371 5.02290 1
8 2 0 15.1626 3.11042 2
8 2 0 26.5906 3.92894 1
-8 2 2 137.498 11.5516 -2
8 2 0 137.498 11.5516 1
9 2 0 187.902 8.05092 1
9 2 0 150.430 6.63390 2
-10 2 3 190.039 10.1920 -2
10 2 0 190.039 10.1920 1
-11 2 3 340.636 15.2261 -2
11 2 0 340.636 15.2261 1
12 2 0 37.1579 6.13747 2
12 2 0 67.7334 8.52744 1
0 3 0 0.34467 1.05688 -2
0 3 0 0.34467 1.05688 1
1 3 0 1104.33 8.38855 2
1 3 0 1607.95 11.3561 1
2 3 0 0.99430 0.93940 1
2 3 0 -0.8952 0.85706 2
3 3 0 794.128 9.23195 1
3 3 0 554.633 6.77731 2
-3 3 1 809.504 12.3540 -2
3 3 0 809.504 12.3540 1
4 3 0 15.5354 1.58984 1
4 3 0 8.81895 1.40991 2
-4 3 1 126.585 5.62636 -2
4 3 0 126.585 5.62636 1
5 3 0 232.389 4.14339 2
5 3 0 340.734 4.75938 1
6 3 0 867.745 13.6506 1
6 3 0 595.664 9.46212 2
-6 3 2 888.809 20.4267 -2
6 3 0 888.809 20.4267 1
-7 3 2 21.8463 3.08090 -2
7 3 0 21.8463 3.08090 1
8 3 0 37.4401 4.74044 2
-8 3 2 178.395 10.6225 -2
8 3 0 178.395 10.6225 1
8 3 0 55.9800 5.83249 1
9 3 0 5.86206 2.82728 2
9 3 0 4.08238 3.00424 1
-10 3 3 43.2985 6.88278 -2
10 3 0 43.2985 6.88278 1
-11 3 3 -5.8369 8.60846 -2
11 3 0 -5.8369 8.60846 1
12 3 0 3.28243 5.31322 1
12 3 0 1.85208 4.72276 2
0 4 0 0.90962 1.40347 -2
0 4 0 0.90962 1.40347 1
1 4 0 954.411 8.03919 1
1 4 0 658.503 6.17703 2
2 4 0 4.78629 1.05217 2
2 4 0 4.26598 1.06867 1
-3 4 1 661.082 10.2426 -2
3 4 0 661.082 10.2426 1
3 4 0 613.656 8.64499 1
3 4 0 418.412 6.23326 2
4 4 0 18.0470 1.90242 2
4 4 0 24.1842 2.20385 1
-4 4 1 112.368 5.62104 -2
4 4 0 112.368 5.62104 1
5 4 0 671.048 7.37585 1
5 4 0 457.616 5.69756 2
6 4 0 10.7714 1.70106 2
6 4 0 13.2600 2.43311 1
-6 4 2 124.669 8.80914 -2
6 4 0 124.669 8.80914 1
-7 4 2 554.442 9.82954 -2
7 4 0 554.442 9.82954 1
8 4 0 77.8511 6.26278 2
8 4 0 102.720 6.36409 1
-8 4 2 126.321 11.1204 -2
8 4 0 126.321 11.1204 1
9 4 0 151.653 7.00258 1
9 4 0 114.645 6.49325 2
-10 4 3 95.2396 8.39311 -2
10 4 0 95.2396 8.39311 1
-11 4 3 428.087 15.2525 -2
11 4 0 428.087 15.2525 1
12 4 0 3.62662 5.33371 1
12 4 0 9.80682 4.93927 2
0 5 0 0.29269 1.09872 -2
0 5 0 0.29269 1.09872 1
1 5 0 753.135 7.23148 1
1 5 0 537.492 5.78993 2
2 5 0 204.682 3.39618 2
2 5 0 297.283 4.21080 1
3 5 0 229.757 4.93470 2
3 5 0 343.112 7.39725 1
-3 5 1 385.544 7.50476 -2
3 5 0 385.544 7.50476 1
-4 5 1 229.867 6.79728 -2
4 5 0 229.867 6.79728 1
4 5 0 46.1812 2.69146 2
4 5 0 63.4127 3.14793 1
5 5 0 531.336 7.04784 1
5 5 0 394.054 5.83115 2
6 5 0 14.7363 2.07377 1
6 5 0 9.87036 1.80008 2
-6 5 2 245.474 11.4681 -2
6 5 0 245.474 11.4681 1
-7 5 2 75.2866 4.25992 -2
7 5 0 75.2866 4.25992 1
8 5 0 74.5335 5.64043 1
-8 5 2 188.024 13.3988 -2
8 5 0 188.024 13.3988 1
8 5 0 51.2375 5.03496 2
9 5 0 6.94998 2.99517 2
9 5 0 5.50936 2.86079 1
-10 5 3 205.177 10.3061 -2
10 5 0 205.177 10.3061 1
-11 5 3 50.8343 8.95786 -2
11 5 0 50.8343 8.95786 1
12 5 0 100.299 10.0340 1
12 5 0 79.4731 8.57873 2
0 6 0 542.316 6.57206 -2
0 6 0 542.316 6.57206 1
1 6 0 66.0422 2.36715 1
1 6 0 46.4823 2.08503 2
1 6 0 120.198 8.19333 -2
1 6 0 120.198 8.19333 1
2 6 0 258.759 3.94482 2
2 6 0 366.024 4.86816 1
-3 6 1 217.949 5.53557 -2
3 6 0 217.949 5.53557 1
3 6 0 21.4514 2.43945 2
3 6 0 28.6667 3.04426 1
4 6 0 449.339 10.3167 1
-4 6 1 690.669 9.88951 -2
4 6 0 690.669 9.88951 1
4 6 0 317.839 6.55118 2
5 6 0 192.472 4.04403 2
5 6 0 285.912 5.04423 1
6 6 0 625.546 9.96429 1
6 6 0 438.558 7.63370 2
-6 6 2 753.830 18.2231 -2
6 6 0 753.830 18.2231 1
-7 6 2 232.979 6.60308 -2
7 6 0 232.979 6.60308 1
-8 6 2 84.9955 8.46640 -2
8 6 0 84.9955 8.46640 1
8 6 0 39.1604 5.33227 2
8 6 0 44.0105 5.26872 1
9 6 0 2.09319 2.93459 2
9 6 0 9.38758 3.06204 1
-10 6 3 23.4118 6.85449 -2
10 6 0 23.4118 6.85449 1
-11 6 3 83.6825 9.60823 -2
11 6 0 83.6825 9.60823 1
12 6 0 -3.4567 5.17113 1
12 6 0 3.63674 5.28125 2
0 7 0 0.13539 1.37108 -2
0 7 0 0.13539 1.37108 1
1 7 0 22.5820 1.77011 1
1 7 0 35.9206 6.85980 -2
1 7 0 35.9206 6.85980 1
1 7 0 15.0860 1.51700 2
2 7 0 3.53095 1.02974 2
2 7 0 7.58245 1.23016 1
3 7 0 107.049 4.91352 1
3 7 0 85.1397 4.34173 2
-3 7 1 172.087 5.25169 -2
3 7 0 172.087 5.25169 1
-4 7 1 58.9599 4.12876 -2
4 7 0 58.9599 4.12876 1
4 7 0 1.37046 1.52779 2
4 7 0 1.01505 1.97444 1
5 7 0 89.9161 3.20113 1
5 7 0 66.0341 2.75759 2
-6 7 2 1529.26 27.7459 -2
6 7 0 1529.26 27.7459 1
6 7 0 386.553 8.47929 2
6 7 0 547.033 10.3480 1
-7 7 2 20.6121 3.11686 -2
7 7 0 20.6121 3.11686 1
-8 7 2 422.203 16.2992 -2
8 7 0 422.203 16.2992 1
8 7 0 183.828 9.05351 2
8 7 0 249.242 9.18651 1
9 7 0 -0.3808 2.69892 2
9 7 0 6.30128 3.04814 1
-10 7 3 66.7529 8.64625 -2
10 7 0 66.7529 8.64625 1
-11 7 3 126.700 11.6449 -2
11 7 0 126.700 11.6449 1
12 7 0 125.614 12.2998 1
12 7 0 93.8111 10.3502 2
0 8 0 2016.93 19.8028 -2
0 8 0 2016.93 19.8028 1
1 8 0 4.44381 1.26863 2
1 8 0 13.2920 4.88760 -2
1 8 0 13.2920 4.88760 1
1 8 0 7.56245 1.49817 1
2 8 0 114.384 3.31126 2
2 8 0 158.934 3.39503 1
-3 8 1 147.794 5.09486 -2
3 8 0 147.794 5.09486 1
3 8 0 1.42934 1.68037 2
3 8 0 0.84531 1.56665 1
-4 8 1 233.030 6.70052 -2
4 8 0 233.030 6.70052 1
4 8 0 138.473 5.93848 2
4 8 0 187.697 6.98146 1
5 8 0 145.544 4.05663 1
5 8 0 103.178 3.28425 2
6 8 0 200.785 6.54057 1
6 8 0 155.496 5.89980 2
-6 8 2 389.793 13.9931 -2
6 8 0 389.793 13.9931 1
-7 8 2 185.122 5.94077 -2
7 8 0 185.122 5.94077 1
-8 8 2 147.297 10.2723 -2
8 8 0 147.297 10.2723 1
8 8 0 143.342 8.38190 1
8 8 0 108.801 8.97864 2
9 8 0 95.3428 7.06627 1
9 8 0 71.6002 6.21657 2
-10 8 3 138.882 10.4864 -2
10 8 0 138.882 10.4864 1
-11 8 3 71.0198 10.7666 -2
11 8 0 71.0198 10.7666 1
0 9 0 0.86507 1.58446 -2
0 9 0 0.86507 1.58446 1
1 9 0 349.329 5.91534 1
1 9 0 253.954 4.92880 2
1 9 0 627.098 15.1110 -2
1 9 0 627.098 15.1110 1
2 9 0 26.5997 1.73569 1
2 9 0 16.9717 1.79084 2
-3 9 1 136.809 5.13349 -2
3 9 0 136.809 5.13349 1
3 9 0 130.129 5.39860 1
3 9 0 80.7645 4.19145 2
-4 9 1 334.726 7.99357 -2
4 9 0 334.726 7.99357 1
4 9 0 78.7446 4.81182 2
4 9 0 91.4151 5.27266 1
5 9 0 335.609 5.70194 2
5 9 0 501.315 7.54235 1
-6 9 2 190.385 8.53053 -2
6 9 0 190.385 8.53053 1
6 9 0 1.72654 2.00763 1
6 9 0 1.47279 2.00583 2
-7 9 2 65.1351 4.30865 -2
7 9 0 65.1351 4.30865 1
8 9 0 4.45277 4.06274 2
8 9 0 2.09727 4.12133 1
-8 9 2 136.821 11.9630 -2
8 9 0 136.821 11.9630 1
9 9 0 17.1374 4.07282 2
9 9 0 19.4299 4.23339 1
-10 9 3 185.583 11.4779 -2
10 9 0 185.583 11.4779 1
-11 9 3 102.024 11.8196 -2
11 9 0 102.024 11.8196 1
0 10 0 190.996 5.13207 -2
0 10 0 190.996 5.13207 1
1 10 0 136.101 3.83307 2
1 10 0 341.653 11.5157 -2
1 10 0 341.653 11.5157 1
1 10 0 210.385 4.64010 1
2 10 0 248.548 4.99127 1
2 10 0 176.890 3.99000 2
3 10 0 236.356 8.64316 1
3 10 0 172.216 6.48691 2
-3 10 1 237.186 5.85357 -2
3 10 0 237.186 5.85357 1
-4 10 1 291.488 7.70730 -2
4 10 0 291.488 7.70730 1
4 10 0 30.5074 3.64915 1
4 10 0 23.1430 4.37400 2
5 10 0 440.874 8.12301 1
5 10 0 304.288 6.47717 2
-6 10 2 60.2741 6.08052 -2
6 10 0 60.2741 6.08052 1
6 10 0 1.03605 2.64796 1
6 10 0 -2.0313 2.24507 2
-7 10 2 205.218 6.59307 -2
7 10 0 205.218 6.59307 1
-8 10 2 63.3331 9.24582 -2
8 10 0 63.3331 9.24582 1
8 10 0 53.0750 6.82381 2
8 10 0 75.2988 9.20685 1
9 10 0 287.726 10.5658 1
9 10 0 189.794 8.85888 2
-10 10 3 78.5591 9.34632 -2
10 10 0 78.5591 9.34632 1
-11 10 3 251.148 14.7838 -2
11 10 0 251.148 14.7838 1
0 11 0 -2.4577 1.41932 -2
0 11 0 -2.4577 1.41932 1
1 11 0 641.157 8.58628 1
1 11 0 443.476 6.87805 2
1 11 0 1091.41 22.2782 -2
1 11 0 1091.41 22.2782 1
2 11 0 3.89782 1.31128 2
2 11 0 11.9991 1.76751 1
-3 11 1 137.366 4.70777 -2
3 11 0 137.366 4.70777 1
-4 11 1 668.578 10.5535 -2
4 11 0 668.578 10.5535 1
4 11 0 466.393 26.2484 2
4 11 0 612.701 30.6621 1
5 11 0 193.580 5.66720 1
5 11 0 129.022 4.39708 2
-6 11 2 38.4778 5.77702 -2
6 11 0 38.4778 5.77702 1
6 11 0 14.6106 3.62959 2
6 11 0 15.1411 3.80866 1
-7 11 2 8.39297 3.28660 -2
7 11 0 8.39297 3.28660 1
8 11 0 80.0531 8.25420 1
8 11 0 71.2978 7.27456 2
-8 11 2 100.457 11.7066 -2
8 11 0 100.457 11.7066 1
9 11 0 81.2024 6.99751 1
9 11 0 44.5246 5.10007 2
-10 11 3 84.9510 10.1511 -2
10 11 0 84.9510 10.1511 1
-11 11 3 18.8545 10.4628 -2
11 11 0 18.8545 10.4628 1
0 12 0 277.028 6.62418 -2
0 12 0 277.028 6.62418 1
1 12 0 622.273 8.76038 1
1 12 0 434.201 7.06958 2
1 12 0 1060.08 22.6867 -2
1 12 0 1060.08 22.6867 1
2 12 0 1181.70 11.9280 1
2 12 0 816.075 9.48524 2
-3 12 1 117.889 4.42876 -2
3 12 0 117.889 4.42876 1
-4 12 1 32.2280 3.71924 -2
4 12 0 32.2280 3.71924 1
5 12 0 137.803 4.72075 2
5 12 0 201.515 5.97933 1
6 12 0 5.47079 2.89616 2
6 12 0 12.6223 3.30698 1
-6 12 2 20.9583 5.80196 -2
6 12 0 20.9583 5.80196 1
-7 12 2 29.1162 4.03237 -2
7 12 0 29.1162 4.03237 1
8 12 0 49.9367 6.43720 2
-8 12 2 113.855 12.8993 -2
8 12 0 113.855 12.8993 1
8 12 0 59.7748 8.44121 1
9 12 0 71.5683 6.65183 1
9 12 0 48.0942 5.70986 2
-10 12 3 9.22351 8.32605 -2
10 12 0 9.22351 8.32605 1
-11 12 3 197.251 14.2230 -2
11 12 0 197.251 14.2230 1
0 13 0 -2.2128 2.10630 -2
0 13 0 -2.2128 2.10630 1
1 13 0 24.8718 2.63425 2
1 13 0 37.7432 2.75584 1
1 13 0 61.8763 7.57373 -2
1 13 0 61.8763 7.57373 1
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TITL twin4 in P2(1)/n
CELL 0.71073 10.4066 21.1342 17.1162 90 95.054 90
ZERR 4 0.0007 0.0015 0.0012 0 0.001 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N O P Ru
UNIT 140 228 8 4 12 4
L.S. 12
PLAN 5 0 0
TEMP -100
HTAB
BOND $H
CONF
fmap 2
acta
REM D:/Documents/My%20Box%20Files/MSU/Data/Xray/AKS03152013/work/twin5.hk
REM l
WGHT 0.028600 1.461400
BASF 0.41234
FVAR 0.31352
RU1 6 0.475530 0.175441 0.033231 11.00000 0.01813 0.01912 =
0.01909 -0.00206 0.00316 -0.00181
P3 5 0.450029 0.245174 0.130819 11.00000 0.02265 0.02868 =
0.02520 -0.00827 0.00608 -0.00276
P1 5 0.386571 0.093282 0.088650 11.00000 0.02492 0.02440 =
0.03212 0.00266 0.00431 -0.00464
P2 5 0.288242 0.197034 -0.036927 11.00000 0.02684 0.03145 =
0.02417 -0.00253 -0.00086 0.00465
O1 4 0.555866 0.122801 -0.057917 11.00000 0.02168 0.02512 =
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N2 3 0.775409 0.141043 -0.075729 11.00000 0.02129 0.02620 =
0.02370 -0.00838 0.00462 -0.00094
N1 3 0.665206 0.189262 0.021908 11.00000 0.02145 0.02418 =
0.01982 -0.00376 0.00506 -0.00569
C12 1 0.862143 0.135026 0.243609 11.00000 0.06179 0.08780 =
0.03279 0.01054 -0.00058 0.01045
AFIX 137
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AFIX 0
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AFIX 43
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AFIX 0
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AFIX 43
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AFIX 137
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AFIX 43
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AFIX 43
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AFIX 137
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AFIX 0
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AFIX 137
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AFIX 0
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AFIX 137
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AFIX 137
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AFIX 137
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AFIX 0
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AFIX 137
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AFIX 0
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AFIX 137
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AFIX 0
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AFIX 0
C22 1 0.669402 0.149648 -0.041822 11.00000 0.02289 0.01764 =
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C23 1 0.779517 0.106399 -0.144372 11.00000 0.02229 0.02012 =
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C24 1 0.896571 0.077712 -0.157482 11.00000 0.02441 0.04162 =
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AFIX 43
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AFIX 0
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AFIX 43
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AFIX 0
C26 1 0.814518 0.039974 -0.283608 11.00000 0.05041 0.02780 =
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AFIX 0
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AFIX 43
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AFIX 0
C28 1 0.679331 0.100319 -0.204211 11.00000 0.02448 0.02639 =
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AFIX 43
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AFIX 0
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C6 1 0.797964 0.284468 0.017963 11.00000 0.02775 0.02546 =
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C5 1 0.893767 0.322762 0.056152 11.00000 0.03068 0.02865 =
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AFIX 43
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AFIX 0
C4 1 0.960671 0.303681 0.124854 11.00000 0.01872 0.05015 =
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AFIX 43
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AFIX 0
C3 1 0.936318 0.246135 0.157357 11.00000 0.02430 0.05335 =
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AFIX 43
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AFIX 13
H10 2 0.721627 0.135408 0.151232 11.00000 -1.20000
AFIX 0
C11 1 0.874628 0.088412 0.110861 11.00000 0.03608 0.03728 =
0.04449 0.00822 -0.00270 0.00217
AFIX 137
H11A 2 0.847087 0.093036 0.054912 11.00000 -1.50000
H11B 2 0.844810 0.047598 0.129571 11.00000 -1.50000
H11C 2 0.968973 0.090308 0.118723 11.00000 -1.50000
AFIX 0
C7 1 0.726486 0.305724 -0.058472 11.00000 0.04691 0.03483 =
0.04010 0.00649 0.01222 -0.00952
AFIX 13
H7 2 0.645771 0.280025 -0.066894 11.00000 -1.20000
AFIX 0
C8 1 0.687710 0.375760 -0.059452 11.00000 0.07196 0.04659 =
0.06343 0.01436 0.02680 0.00894
AFIX 137
H8A 2 0.630741 0.384645 -0.106859 11.00000 -1.50000
H8B 2 0.765204 0.402140 -0.059116 11.00000 -1.50000
H8C 2 0.642409 0.385242 -0.013007 11.00000 -1.50000
AFIX 0
C9 1 0.807408 0.292837 -0.126903 11.00000 0.12896 0.04891 =
0.04466 0.00437 0.03142 0.00452
AFIX 137
H9A 2 0.884872 0.319404 -0.121716 11.00000 -1.50000
H9B 2 0.756641 0.302669 -0.176371 11.00000 -1.50000
H9C 2 0.832674 0.248161 -0.126566 11.00000 -1.50000
AFIX 0
HKLF 5
REM twin4 in P2(1)/n
REM R1 = 0.0392 for 9968 Fo > 4sig(Fo) and 0.0600 for all 12583 data
REM 394 parameters refined using 0 restraints
END
WGHT 0.0286 1.4612
REM Instructions for potential hydrogen bonds
HTAB C28 O1
REM Highest difference peak 0.405, deepest hole -0.356, 1-sigma level 0.074
Q1 1 0.4338 0.1212 0.0527 11.00000 0.05 0.41
Q2 1 0.2946 0.2388 -0.0428 11.00000 0.05 0.38
Q3 1 0.7225 0.1656 -0.0771 11.00000 0.05 0.36
Q4 1 0.5195 0.5246 -0.0374 11.00000 0.05 0.35
Q5 1 0.5755 0.1747 -0.1012 11.00000 0.05 0.35
;
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number 2013-2
_database_code_depnum_ccdc_archive 'CCDC 957946'