# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
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data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1472239'
_audit_update_record
;
2016-06-30 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;
_audit_creation_date 2016-06-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C52 H49 Cl2 F2 N4 O2 Ru2, P F6'
_chemical_formula_sum 'C52 H49 Cl2 F8 N4 O2 P Ru2'
_chemical_formula_weight 1217.96
_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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
_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.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.2730(2)
_cell_length_b 9.9670(2)
_cell_length_c 13.7840(4)
_cell_angle_alpha 101.1000(10)
_cell_angle_beta 93.4140(10)
_cell_angle_gamma 100.4010(10)
_cell_volume 1223.71(5)
_cell_formula_units_Z 1
_cell_measurement_reflns_used 24304
_cell_measurement_temperature 148(2)
_cell_measurement_theta_max 27.485
_cell_measurement_theta_min 0.998
_shelx_estimated_absorpt_T_max 0.975
_shelx_estimated_absorpt_T_min 0.831
_exptl_absorpt_coefficient_mu 0.836
_exptl_absorpt_correction_T_max 0.9754
_exptl_absorpt_correction_T_min 0.8310
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
Using multiple and symmetry related data measurements via the program SORTAV
See R. H. Blessing, Acta Cryst (1995), A51, 33-38
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour Orange
_exptl_crystal_density_diffrn 1.653
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Prism
_exptl_crystal_F_000 614
_exptl_crystal_size_max 0.23
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.03
_exptl_special_details
;
Detector set at 30 mm from sample with different 2theta offsets
1 degree phi exposures for chi=0 degree settings
1 degree omega exposures for chi=90 degree settings
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0751
_diffrn_reflns_av_unetI/netI 0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 24560
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 27.492
_diffrn_reflns_theta_min 2.244
_diffrn_ambient_temperature 148.15
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer'
_diffrn_measurement_method '\w and \f scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4914
_reflns_number_total 5582
_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 'DENZO-SMN (Otwinowski and Minor, 1997)'
_computing_data_collection 'COLLECT (Nonius, 1999)'
_computing_data_reduction 'DENZO-SMN (Otwinowski and Minor, 1997)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max 1.086
_refine_diff_density_min -0.940
_refine_diff_density_rms 0.141
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.042
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 358
_refine_ls_number_reflns 5582
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0441
_refine_ls_R_factor_gt 0.0351
_refine_ls_restrained_S_all 1.042
_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^)+(0.0548P)^2^+0.4451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0895
_refine_ls_wR_factor_ref 0.0953
_refine_special_details
;
Reflections -1 0 1, 0 0 1, 0 1 0 omitted as obscured by beamstop.
;
_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. Others
Fixed Sof: Ru1(0.5) F2A(0.5) F4A(0.5) F3A(0.5) F4B(0.5) F2B(0.5) F3B(0.5)
Ru2(0.5)
Fixed X: Ru1(0.289399) P1(0.5)
Fixed Y: Ru1(0.3998) P1(0)
Fixed Z: Ru1(0.2538) P1(0.5)
3.a Ternary CH refined with riding coordinates:
C24(H24)
3.b Aromatic/amide H refined with riding coordinates:
C2(H2), C8(H8), C12(H12), C20(H20), C7(H7), C4(H4), C22(H22), C19(H19),
C3(H3), C23(H23), C15(H15), C13(H13), C14(H14), C5(H5)
3.c Idealised Me refined as rotating group:
C17(H17A,H17B,H17C), 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
Ru1 Ru 0.2894 0.3998 0.2538 0.0225(7) Uani 0.5 1 d . . . A 1
Cl1 Cl 0.41584(7) 0.52720(6) 0.14403(5) 0.02984(14) Uani 1 1 d . . . . .
O1 O 0.12181(19) 0.07305(18) 0.01011(13) 0.0308(4) Uani 1 1 d . . . . .
N1 N 0.2708(2) 0.2225(2) 0.13982(15) 0.0250(4) Uani 1 1 d . . . . .
N2 N 0.0997(2) 0.4017(2) 0.16041(15) 0.0238(4) Uani 1 1 d . . . . .
C2 C 0.0745(3) 0.6351(3) 0.2375(2) 0.0308(5) Uani 1 1 d . . . . .
H2 H 0.1666 0.6489 0.2758 0.037 Uiso 1 1 calc R . . . .
C10 C 0.1520(3) 0.1857(2) 0.07808(18) 0.0256(5) Uani 1 1 d . . . . .
C8 C -0.0718(3) 0.2713(3) 0.0213(2) 0.0304(5) Uani 1 1 d . . . . .
H8 H -0.0979 0.1910 -0.0307 0.036 Uiso 1 1 calc R . . . .
C9 C 0.0548(3) 0.2895(3) 0.08751(18) 0.0254(5) Uani 1 1 d . . . . .
C12 C 0.5155(3) 0.1684(3) 0.1147(2) 0.0332(6) Uani 1 1 d . . . . .
H12 H 0.5478 0.2576 0.1000 0.040 Uiso 1 1 calc R . . . .
C1 C 0.0214(3) 0.5084(3) 0.16892(18) 0.0265(5) Uani 1 1 d . . . . .
C11 C 0.3723(3) 0.1295(3) 0.13736(18) 0.0262(5) Uani 1 1 d . . . . .
C6 C -0.1120(3) 0.4924(3) 0.1080(2) 0.0306(5) Uani 1 1 d . . . . .
C20 C 0.3047(3) 0.2641(3) 0.35995(18) 0.0297(5) Uani 1 1 d . . . . .
H20 H 0.2931 0.1656 0.3494 0.036 Uiso 1 1 calc R . . A .
C7 C -0.1570(3) 0.3707(3) 0.0330(2) 0.0325(6) Uani 1 1 d . . . . .
H7 H -0.2455 0.3582 -0.0090 0.039 Uiso 1 1 calc R . . . .
C4 C -0.1435(3) 0.7193(3) 0.1931(2) 0.0391(6) Uani 1 1 d . . . . .
H4 H -0.2010 0.7897 0.2047 0.047 Uiso 1 1 calc R . . . .
C22 C 0.2055(3) 0.4743(3) 0.39339(19) 0.0323(6) Uani 1 1 d . . . . .
H22 H 0.1246 0.5195 0.4054 0.039 Uiso 1 1 calc R . . A .
C19 C 0.4470(3) 0.3452(3) 0.35804(19) 0.0317(6) Uani 1 1 d . . . . .
H19 H 0.5282 0.3001 0.3465 0.038 Uiso 1 1 calc R . . A .
C18 C 0.4691(3) 0.4915(3) 0.37303(19) 0.0320(6) Uani 1 1 d . . . . .
C3 C -0.0068(3) 0.7385(3) 0.2489(2) 0.0358(6) Uani 1 1 d . . . . .
H3 H 0.0297 0.8238 0.2949 0.043 Uiso 1 1 calc R . . . .
P1 P 0.5000 0.0000 0.5000 0.0471(3) Uani 1 2 d S T P B 1
F1 F 0.19236(18) -0.03277(16) 0.18892(13) 0.0402(4) Uani 1 1 d . . . . .
C16 C 0.3313(3) 0.0014(3) 0.16247(19) 0.0311(5) Uani 1 1 d . . . . .
C17 C 0.6167(3) 0.5768(4) 0.3639(2) 0.0459(7) Uani 1 1 d . . . . .
H17A H 0.6745 0.5178 0.3241 0.069 Uiso 1 1 calc GR . . . .
H17B H 0.6688 0.6150 0.4301 0.069 Uiso 1 1 calc GR . . . .
H17C H 0.6030 0.6535 0.3314 0.069 Uiso 1 1 calc GR . . . .
C23 C 0.3461(3) 0.5563(3) 0.39238(19) 0.0325(6) Uani 1 1 d . . . . .
H23 H 0.3587 0.6550 0.4046 0.039 Uiso 1 1 calc R . . A .
C15 C 0.4251(3) -0.0916(3) 0.1625(2) 0.0396(7) Uani 1 1 d . . . . .
H15 H 0.3938 -0.1793 0.1799 0.047 Uiso 1 1 calc R . . . .
C13 C 0.6120(3) 0.0760(3) 0.1137(2) 0.0414(7) Uani 1 1 d . . . . .
H13 H 0.7099 0.1016 0.0975 0.050 Uiso 1 1 calc R . . . .
C21 C 0.1803(3) 0.3250(3) 0.37697(19) 0.0308(5) Uani 1 1 d . . . . .
C14 C 0.5646(4) -0.0536(3) 0.1365(2) 0.0453(7) Uani 1 1 d . . . . .
H14 H 0.6302 -0.1170 0.1341 0.054 Uiso 1 1 calc R . . . .
F2A F 0.394(3) -0.082(2) 0.4026(19) 0.094(6) Uani 0.5 1 d . . . B 1
F4A F 0.389(2) 0.0802(15) 0.5422(13) 0.139(7) Uani 0.5 1 d . . . B 1
C24 C 0.0311(3) 0.2344(4) 0.3803(2) 0.0461(7) Uani 1 1 d . . . . .
H24 H 0.0272 0.1437 0.3330 0.055 Uiso 1 1 calc R . . . .
C25 C 0.0220(4) 0.2025(5) 0.4844(3) 0.0670(11) Uani 1 1 d . . . . .
H25A H 0.0268 0.2894 0.5331 0.100 Uiso 1 1 calc GR . . . .
H25B H 0.1045 0.1590 0.5007 0.100 Uiso 1 1 calc GR . . . .
H25C H -0.0712 0.1388 0.4862 0.100 Uiso 1 1 calc GR . . . .
C26 C -0.0989(4) 0.2897(5) 0.3513(3) 0.0676(11) Uani 1 1 d . . . . .
H26A H -0.1033 0.3748 0.3995 0.101 Uiso 1 1 calc GR . . . .
H26B H -0.1885 0.2199 0.3502 0.101 Uiso 1 1 calc GR . . . .
H26C H -0.0911 0.3111 0.2851 0.101 Uiso 1 1 calc GR . . . .
C5 C -0.1948(3) 0.6016(3) 0.1229(2) 0.0368(6) Uani 1 1 d . . . . .
H5 H -0.2853 0.5917 0.0837 0.044 Uiso 1 1 calc R . . . .
F3A F 0.441(2) -0.1146(16) 0.5567(13) 0.080(4) Uani 0.5 1 d . . . B 1
F4B F 0.3981(16) 0.1143(13) 0.5371(8) 0.075(2) Uani 0.5 1 d . . . B 1
F2B F 0.367(2) -0.069(3) 0.4198(18) 0.092(6) Uani 0.5 1 d . . . B 1
F3B F 0.425(2) -0.105(2) 0.5673(17) 0.095(5) Uani 0.5 1 d . . . B 1
Ru2 Ru 0.28768(5) 0.39270(8) 0.25153(4) 0.0223(7) Uani 0.5 1 d . . . A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.0234(11) 0.0215(8) 0.0215(11) 0.0036(6) -0.0027(7) 0.0044(6)
Cl1 0.0273(3) 0.0317(3) 0.0304(3) 0.0110(2) -0.0009(2) 0.0019(2)
O1 0.0290(9) 0.0285(9) 0.0290(9) -0.0027(7) -0.0016(7) 0.0011(7)
N1 0.0236(10) 0.0254(10) 0.0255(10) 0.0057(8) -0.0003(8) 0.0043(8)
N2 0.0221(10) 0.0247(10) 0.0256(10) 0.0071(8) 0.0012(8) 0.0051(8)
C2 0.0325(14) 0.0315(13) 0.0312(14) 0.0108(10) 0.0042(11) 0.0089(10)
C10 0.0238(12) 0.0268(12) 0.0256(12) 0.0063(9) 0.0028(9) 0.0026(9)
C8 0.0259(13) 0.0341(14) 0.0293(13) 0.0099(10) -0.0036(10) -0.0009(10)
C9 0.0235(12) 0.0274(12) 0.0244(12) 0.0066(9) 0.0013(10) 0.0020(9)
C12 0.0296(13) 0.0333(14) 0.0344(14) 0.0022(11) 0.0009(11) 0.0058(10)
C1 0.0238(12) 0.0298(12) 0.0292(13) 0.0118(10) 0.0045(10) 0.0070(9)
C11 0.0260(12) 0.0265(12) 0.0250(12) 0.0024(9) -0.0025(10) 0.0068(9)
C6 0.0263(13) 0.0362(14) 0.0332(14) 0.0154(11) 0.0055(10) 0.0068(10)
C20 0.0420(15) 0.0272(12) 0.0207(12) 0.0081(9) -0.0026(10) 0.0069(10)
C7 0.0220(12) 0.0420(15) 0.0354(15) 0.0164(12) -0.0016(10) 0.0038(10)
C4 0.0403(16) 0.0429(16) 0.0449(17) 0.0191(13) 0.0120(13) 0.0224(13)
C22 0.0389(15) 0.0362(14) 0.0229(12) 0.0044(10) 0.0026(11) 0.0123(11)
C19 0.0317(14) 0.0416(15) 0.0236(12) 0.0080(11) -0.0032(10) 0.0128(11)
C18 0.0296(13) 0.0384(14) 0.0227(12) 0.0038(10) -0.0083(10) -0.0014(10)
C3 0.0439(16) 0.0322(14) 0.0376(15) 0.0124(11) 0.0126(12) 0.0157(12)
P1 0.0656(8) 0.0318(6) 0.0463(7) 0.0118(5) -0.0052(6) 0.0151(5)
F1 0.0404(9) 0.0341(8) 0.0442(10) 0.0111(7) 0.0058(7) -0.0012(7)
C16 0.0323(14) 0.0306(13) 0.0276(13) 0.0027(10) -0.0007(10) 0.0039(10)
C17 0.0372(16) 0.0573(19) 0.0357(16) 0.0117(14) -0.0086(13) -0.0081(14)
C23 0.0435(15) 0.0292(13) 0.0215(12) 0.0019(10) -0.0031(11) 0.0041(11)
C15 0.0541(19) 0.0307(14) 0.0360(15) 0.0082(11) -0.0039(13) 0.0152(12)
C13 0.0319(15) 0.0493(17) 0.0427(17) 0.0040(13) 0.0016(12) 0.0135(12)
C21 0.0315(13) 0.0394(14) 0.0208(12) 0.0088(10) -0.0015(10) 0.0035(11)
C14 0.0451(18) 0.0498(18) 0.0444(17) 0.0040(14) -0.0039(14) 0.0271(14)
F2A 0.148(16) 0.069(5) 0.050(5) 0.008(4) -0.025(8) -0.005(8)
F4A 0.166(10) 0.071(7) 0.228(13) 0.068(6) 0.104(9) 0.081(7)
C24 0.0384(16) 0.0577(19) 0.0380(17) 0.0150(14) 0.0031(13) -0.0067(14)
C25 0.046(2) 0.100(3) 0.057(2) 0.045(2) 0.0030(17) -0.008(2)
C26 0.045(2) 0.092(3) 0.068(3) 0.033(2) 0.0055(18) 0.0021(19)
C5 0.0281(14) 0.0463(16) 0.0435(16) 0.0205(13) 0.0060(12) 0.0142(12)
F3A 0.092(8) 0.063(6) 0.086(7) 0.054(5) -0.018(7) -0.009(6)
F4B 0.106(6) 0.052(5) 0.080(4) 0.014(3) 0.011(4) 0.048(4)
F2B 0.075(5) 0.109(10) 0.079(12) 0.006(7) -0.029(6) 0.007(5)
F3B 0.101(8) 0.104(9) 0.111(9) 0.066(7) 0.042(6) 0.042(6)
Ru2 0.0221(11) 0.0212(8) 0.0218(11) 0.0025(6) -0.0014(7) 0.0025(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
Ru1 Cl1 2.3853(6) . ?
Ru1 N1 2.100(2) . ?
Ru1 N2 2.123(2) . ?
Ru1 C20 2.190(2) . ?
Ru1 C22 2.167(3) . ?
Ru1 C19 2.199(2) . ?
Ru1 C18 2.204(2) . ?
Ru1 C23 2.190(3) . ?
Ru1 C21 2.209(3) . ?
Cl1 Ru2 2.4092(8) . ?
O1 C10 1.291(3) . ?
N1 C10 1.301(3) . ?
N1 C11 1.433(3) . ?
N1 Ru2 2.036(2) . ?
N2 C9 1.336(3) . ?
N2 C1 1.383(3) . ?
N2 Ru2 2.113(2) . ?
C2 H2 0.9500 . ?
C2 C1 1.411(4) . ?
C2 C3 1.374(4) . ?
C10 C9 1.482(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.406(3) . ?
C8 C7 1.366(4) . ?
C12 H12 0.9500 . ?
C12 C11 1.386(4) . ?
C12 C13 1.393(4) . ?
C1 C6 1.419(4) . ?
C11 C16 1.380(4) . ?
C6 C7 1.414(4) . ?
C6 C5 1.431(4) . ?
C20 H20 0.9500 . ?
C20 C19 1.422(4) . ?
C20 C21 1.408(4) . ?
C20 Ru2 2.164(2) . ?
C7 H7 0.9500 . ?
C4 H4 0.9500 . ?
C4 C3 1.405(4) . ?
C4 C5 1.359(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.411(4) . ?
C22 C21 1.434(4) . ?
C22 Ru2 2.203(3) . ?
C19 H19 0.9500 . ?
C19 C18 1.409(4) . ?
C19 Ru2 2.197(2) . ?
C18 C17 1.501(4) . ?
C18 C23 1.422(4) . ?
C18 Ru2 2.244(3) . ?
C3 H3 0.9500 . ?
P1 F2A 1.60(2) . ?
P1 F2A 1.60(2) 2_656 ?
P1 F4A 1.491(16) 2_656 ?
P1 F4A 1.491(16) . ?
P1 F3A 1.544(14) . ?
P1 F3A 1.544(14) 2_656 ?
P1 F4B 1.635(12) . ?
P1 F4B 1.635(12) 2_656 ?
P1 F2B 1.56(2) . ?
P1 F2B 1.56(2) 2_656 ?
P1 F3B 1.62(2) . ?
P1 F3B 1.62(2) 2_656 ?
F1 C16 1.362(3) . ?
C16 C15 1.382(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C23 H23 0.9500 . ?
C23 Ru2 2.249(3) . ?
C15 H15 0.9500 . ?
C15 C14 1.370(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.388(5) . ?
C21 C24 1.518(4) . ?
C21 Ru2 2.202(3) . ?
C14 H14 0.9500 . ?
C24 H24 1.0000 . ?
C24 C25 1.533(4) . ?
C24 C26 1.479(5) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C5 H5 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ru1 Cl1 86.48(6) . . ?
N1 Ru1 N2 75.42(8) . . ?
N1 Ru1 C20 87.67(9) . . ?
N1 Ru1 C22 142.27(9) . . ?
N1 Ru1 C19 97.75(9) . . ?
N1 Ru1 C18 129.07(9) . . ?
N1 Ru1 C23 164.98(9) . . ?
N1 Ru1 C21 105.59(9) . . ?
N2 Ru1 Cl1 83.65(5) . . ?
N2 Ru1 C20 126.50(9) . . ?
N2 Ru1 C22 96.70(9) . . ?
N2 Ru1 C19 164.03(9) . . ?
N2 Ru1 C18 154.55(9) . . ?
N2 Ru1 C23 118.83(9) . . ?
N2 Ru1 C21 99.13(9) . . ?
C20 Ru1 Cl1 146.43(7) . . ?
C20 Ru1 C19 37.82(10) . . ?
C20 Ru1 C18 68.12(10) . . ?
C20 Ru1 C21 37.34(10) . . ?
C22 Ru1 Cl1 129.94(7) . . ?
C22 Ru1 C20 67.23(10) . . ?
C22 Ru1 C19 79.77(10) . . ?
C22 Ru1 C18 68.36(10) . . ?
C22 Ru1 C23 37.78(10) . . ?
C22 Ru1 C21 38.24(10) . . ?
C19 Ru1 Cl1 110.65(7) . . ?
C19 Ru1 C18 37.31(10) . . ?
C19 Ru1 C21 68.42(10) . . ?
C18 Ru1 Cl1 90.52(7) . . ?
C18 Ru1 C21 81.95(10) . . ?
C23 Ru1 Cl1 99.28(7) . . ?
C23 Ru1 C20 79.85(10) . . ?
C23 Ru1 C19 67.25(10) . . ?
C23 Ru1 C18 37.77(10) . . ?
C23 Ru1 C21 69.04(10) . . ?
C21 Ru1 Cl1 167.93(7) . . ?
C10 N1 Ru1 118.41(16) . . ?
C10 N1 C11 118.8(2) . . ?
C10 N1 Ru2 118.45(17) . . ?
C11 N1 Ru1 122.02(15) . . ?
C11 N1 Ru2 121.85(15) . . ?
C9 N2 Ru1 115.92(16) . . ?
C9 N2 C1 118.5(2) . . ?
C9 N2 Ru2 114.10(16) . . ?
C1 N2 Ru1 125.55(16) . . ?
C1 N2 Ru2 127.36(17) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
C3 C2 C1 120.0(3) . . ?
O1 C10 N1 124.4(2) . . ?
O1 C10 C9 121.3(2) . . ?
N1 C10 C9 114.2(2) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C7 C8 C9 119.1(2) . . ?
N2 C9 C10 115.1(2) . . ?
N2 C9 C8 123.3(2) . . ?
C8 C9 C10 121.5(2) . . ?
C11 C12 H12 120.1 . . ?
C11 C12 C13 119.7(3) . . ?
C13 C12 H12 120.1 . . ?
N2 C1 C2 120.2(2) . . ?
N2 C1 C6 120.4(2) . . ?
C2 C1 C6 119.3(2) . . ?
C12 C11 N1 121.1(2) . . ?
C16 C11 N1 120.4(2) . . ?
C16 C11 C12 118.4(2) . . ?
C1 C6 C5 119.0(2) . . ?
C7 C6 C1 118.9(2) . . ?
C7 C6 C5 122.1(2) . . ?
Ru1 C20 H20 130.4 . . ?
C19 C20 Ru1 71.44(14) . . ?
C19 C20 H20 118.9 . . ?
C19 C20 Ru2 72.22(14) . . ?
C21 C20 Ru1 72.07(14) . . ?
C21 C20 H20 118.9 . . ?
C21 C20 C19 122.2(2) . . ?
C21 C20 Ru2 72.64(14) . . ?
C8 C7 C6 119.3(2) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C5 C4 C3 120.9(3) . . ?
Ru1 C22 H22 129.3 . . ?
C23 C22 Ru1 71.99(15) . . ?
C23 C22 H22 118.8 . . ?
C23 C22 C21 122.4(2) . . ?
C23 C22 Ru2 73.30(15) . . ?
C21 C22 Ru1 72.47(15) . . ?
C21 C22 H22 118.8 . . ?
C21 C22 Ru2 70.94(15) . . ?
Ru1 C19 H19 130.8 . . ?
C20 C19 Ru1 70.74(14) . . ?
C20 C19 H19 119.6 . . ?
C20 C19 Ru2 69.72(14) . . ?
C18 C19 Ru1 71.54(14) . . ?
C18 C19 C20 120.8(2) . . ?
C18 C19 H19 119.6 . . ?
C18 C19 Ru2 73.34(15) . . ?
C19 C18 Ru1 71.15(14) . . ?
C19 C18 C17 121.0(3) . . ?
C19 C18 C23 118.3(2) . . ?
C19 C18 Ru2 69.69(14) . . ?
C17 C18 Ru1 127.19(19) . . ?
C17 C18 Ru2 127.53(19) . . ?
C23 C18 Ru1 70.56(14) . . ?
C23 C18 C17 120.6(3) . . ?
C23 C18 Ru2 71.74(14) . . ?
C2 C3 C4 120.6(3) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
F2A P1 F2A 180.0 . 2_656 ?
F2A P1 F4B 96.5(10) . . ?
F2A P1 F4B 83.5(10) . 2_656 ?
F2A P1 F4B 83.5(10) 2_656 . ?
F2A P1 F4B 96.5(10) 2_656 2_656 ?
F2A P1 F3B 87.4(11) . 2_656 ?
F2A P1 F3B 87.4(11) 2_656 . ?
F2A P1 F3B 92.6(11) . . ?
F2A P1 F3B 92.6(11) 2_656 2_656 ?
F4A P1 F2A 85.6(12) 2_656 . ?
F4A P1 F2A 94.4(12) 2_656 2_656 ?
F4A P1 F2A 94.4(12) . . ?
F4A P1 F2A 85.6(12) . 2_656 ?
F4A P1 F4A 180.0 2_656 . ?
F4A P1 F3A 88.8(11) . . ?
F4A P1 F3A 91.2(11) . 2_656 ?
F4A P1 F3A 91.2(11) 2_656 . ?
F4A P1 F3A 88.8(11) 2_656 2_656 ?
F4A P1 F4B 12.0(11) 2_656 2_656 ?
F4A P1 F4B 12.0(11) . . ?
F4A P1 F4B 168.0(11) 2_656 . ?
F4A P1 F4B 168.0(11) . 2_656 ?
F4A P1 F2B 98.5(12) . 2_656 ?
F4A P1 F2B 81.5(12) 2_656 2_656 ?
F4A P1 F2B 98.5(12) 2_656 . ?
F4A P1 F2B 81.5(12) . . ?
F4A P1 F3B 99.0(10) . 2_656 ?
F4A P1 F3B 81.0(10) 2_656 2_656 ?
F4A P1 F3B 81.0(10) . . ?
F4A P1 F3B 99.0(10) 2_656 . ?
F3A P1 F2A 89.3(9) 2_656 . ?
F3A P1 F2A 90.7(9) 2_656 2_656 ?
F3A P1 F2A 90.7(9) . . ?
F3A P1 F2A 89.3(9) . 2_656 ?
F3A P1 F3A 180.0 . 2_656 ?
F3A P1 F4B 100.5(10) . . ?
F3A P1 F4B 79.5(10) . 2_656 ?
F3A P1 F4B 100.5(10) 2_656 2_656 ?
F3A P1 F4B 79.5(10) 2_656 . ?
F3A P1 F2B 93.7(10) 2_656 . ?
F3A P1 F2B 93.7(10) . 2_656 ?
F3A P1 F2B 86.3(10) . . ?
F3A P1 F2B 86.3(10) 2_656 2_656 ?
F3A P1 F3B 7.9(16) 2_656 2_656 ?
F3A P1 F3B 172.1(16) . 2_656 ?
F3A P1 F3B 172.1(16) 2_656 . ?
F3A P1 F3B 7.9(16) . . ?
F4B P1 F4B 180.0 . 2_656 ?
F2B P1 F2A 166.4(19) . 2_656 ?
F2B P1 F2A 166(2) 2_656 . ?
F2B P1 F2A 13.6(19) 2_656 2_656 ?
F2B P1 F2A 13.6(19) . . ?
F2B P1 F4B 95.3(11) . 2_656 ?
F2B P1 F4B 84.7(11) . . ?
F2B P1 F4B 95.3(11) 2_656 . ?
F2B P1 F4B 84.7(11) 2_656 2_656 ?
F2B P1 F2B 180.0 2_656 . ?
F2B P1 F3B 93.5(12) . 2_656 ?
F2B P1 F3B 86.5(12) 2_656 2_656 ?
F2B P1 F3B 86.5(12) . . ?
F2B P1 F3B 93.5(12) 2_656 . ?
F3B P1 F4B 87.3(10) . 2_656 ?
F3B P1 F4B 92.7(10) 2_656 2_656 ?
F3B P1 F4B 87.3(10) 2_656 . ?
F3B P1 F4B 92.7(10) . . ?
F3B P1 F3B 180.0 2_656 . ?
C11 C16 C15 122.8(3) . . ?
F1 C16 C11 117.9(2) . . ?
F1 C16 C15 119.3(2) . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Ru1 C23 H23 130.9 . . ?
C22 C23 Ru1 70.23(15) . . ?
C22 C23 C18 120.2(2) . . ?
C22 C23 H23 119.9 . . ?
C22 C23 Ru2 69.77(15) . . ?
C18 C23 Ru1 71.66(14) . . ?
C18 C23 H23 119.9 . . ?
C18 C23 Ru2 71.35(14) . . ?
C16 C15 H15 121.0 . . ?
C14 C15 C16 117.9(3) . . ?
C14 C15 H15 121.0 . . ?
C12 C13 H13 120.1 . . ?
C14 C13 C12 119.9(3) . . ?
C14 C13 H13 120.1 . . ?
C20 C21 Ru1 70.59(14) . . ?
C20 C21 C22 116.1(2) . . ?
C20 C21 C24 120.3(3) . . ?
C20 C21 Ru2 69.74(14) . . ?
C22 C21 Ru1 69.28(14) . . ?
C22 C21 C24 123.6(3) . . ?
C22 C21 Ru2 71.06(15) . . ?
C24 C21 Ru1 131.99(19) . . ?
C24 C21 Ru2 130.86(19) . . ?
C15 C14 C13 121.2(3) . . ?
C15 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C21 C24 H24 107.1 . . ?
C21 C24 C25 108.7(3) . . ?
C25 C24 H24 107.1 . . ?
C26 C24 C21 116.1(3) . . ?
C26 C24 H24 107.1 . . ?
C26 C24 C25 110.2(3) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C6 C5 H5 120.1 . . ?
C4 C5 C6 119.9(3) . . ?
C4 C5 H5 120.1 . . ?
N1 Ru2 Cl1 87.30(6) . . ?
N1 Ru2 N2 76.99(8) . . ?
N1 Ru2 C20 90.04(9) . . ?
N1 Ru2 C22 144.54(10) . . ?
N1 Ru2 C19 99.80(9) . . ?
N1 Ru2 C18 130.43(10) . . ?
N1 Ru2 C23 166.07(10) . . ?
N1 Ru2 C21 108.16(10) . . ?
N2 Ru2 Cl1 83.26(6) . . ?
N2 Ru2 C20 128.42(9) . . ?
N2 Ru2 C22 95.89(9) . . ?
N2 Ru2 C19 166.48(10) . . ?
N2 Ru2 C18 151.22(10) . . ?
N2 Ru2 C23 116.62(9) . . ?
N2 Ru2 C21 99.66(9) . . ?
C20 Ru2 Cl1 146.58(8) . . ?
C20 Ru2 C22 67.05(10) . . ?
C20 Ru2 C19 38.07(10) . . ?
C20 Ru2 C18 67.85(10) . . ?
C20 Ru2 C23 79.10(10) . . ?
C20 Ru2 C21 37.63(10) . . ?
C22 Ru2 Cl1 126.83(8) . . ?
C22 Ru2 C18 67.03(10) . . ?
C22 Ru2 C23 36.93(10) . . ?
C19 Ru2 Cl1 109.86(8) . . ?
C19 Ru2 C22 79.03(10) . . ?
C19 Ru2 C18 36.97(10) . . ?
C19 Ru2 C23 66.27(10) . . ?
C19 Ru2 C21 68.60(10) . . ?
C18 Ru2 Cl1 88.96(7) . . ?
C18 Ru2 C23 36.91(10) . . ?
C23 Ru2 Cl1 96.93(8) . . ?
C21 Ru2 Cl1 164.54(8) . . ?
C21 Ru2 C22 38.00(10) . . ?
C21 Ru2 C18 81.22(10) . . ?
C21 Ru2 C23 68.11(10) . . ?
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 C10 O1 -174.13(18) . . . . ?
Ru1 N1 C10 C9 9.5(3) . . . . ?
Ru1 N1 C11 C12 -72.0(3) . . . . ?
Ru1 N1 C11 C16 104.7(2) . . . . ?
Ru1 N2 C9 C10 -4.8(3) . . . . ?
Ru1 N2 C9 C8 177.52(19) . . . . ?
Ru1 N2 C1 C2 6.8(3) . . . . ?
Ru1 N2 C1 C6 -173.97(17) . . . . ?
Ru1 C20 C19 C18 53.2(2) . . . . ?
Ru1 C20 C21 C22 -53.80(19) . . . . ?
Ru1 C20 C21 C24 128.0(2) . . . . ?
Ru1 C22 C23 C18 -53.4(2) . . . . ?
Ru1 C22 C21 C20 54.5(2) . . . . ?
Ru1 C22 C21 C24 -127.4(2) . . . . ?
Ru1 C19 C18 C17 -122.7(2) . . . . ?
Ru1 C19 C18 C23 54.3(2) . . . . ?
Ru1 C18 C23 C22 52.8(2) . . . . ?
Ru1 C21 C24 C25 173.4(3) . . . . ?
Ru1 C21 C24 C26 -61.7(4) . . . . ?
O1 C10 C9 N2 -179.4(2) . . . . ?
O1 C10 C9 C8 -1.7(4) . . . . ?
N1 C10 C9 N2 -2.9(3) . . . . ?
N1 C10 C9 C8 174.8(2) . . . . ?
N1 C11 C16 F1 0.2(4) . . . . ?
N1 C11 C16 C15 -179.3(2) . . . . ?
N2 C1 C6 C7 -5.3(4) . . . . ?
N2 C1 C6 C5 176.3(2) . . . . ?
C2 C1 C6 C7 173.9(2) . . . . ?
C2 C1 C6 C5 -4.5(4) . . . . ?
C10 N1 C11 C12 118.1(3) . . . . ?
C10 N1 C11 C16 -65.2(3) . . . . ?
C9 N2 C1 C2 -172.8(2) . . . . ?
C9 N2 C1 C6 6.4(3) . . . . ?
C9 C8 C7 C6 3.0(4) . . . . ?
C12 C11 C16 F1 177.1(2) . . . . ?
C12 C11 C16 C15 -2.5(4) . . . . ?
C12 C13 C14 C15 -1.5(5) . . . . ?
C1 N2 C9 C10 174.9(2) . . . . ?
C1 N2 C9 C8 -2.8(4) . . . . ?
C1 C2 C3 C4 0.3(4) . . . . ?
C1 C6 C7 C8 0.5(4) . . . . ?
C1 C6 C5 C4 1.3(4) . . . . ?
C11 N1 C10 O1 -3.8(4) . . . . ?
C11 N1 C10 C9 179.8(2) . . . . ?
C11 C12 C13 C14 -0.8(4) . . . . ?
C11 C16 C15 C14 0.2(4) . . . . ?
C20 C19 C18 Ru1 -52.9(2) . . . . ?
C20 C19 C18 C17 -175.6(2) . . . . ?
C20 C19 C18 C23 1.4(4) . . . . ?
C20 C19 C18 Ru2 -53.2(2) . . . . ?
C20 C21 C24 C25 82.9(4) . . . . ?
C20 C21 C24 C26 -152.2(3) . . . . ?
C7 C8 C9 N2 -2.0(4) . . . . ?
C7 C8 C9 C10 -179.5(2) . . . . ?
C7 C6 C5 C4 -177.0(3) . . . . ?
C22 C21 C24 C25 -95.2(4) . . . . ?
C22 C21 C24 C26 29.7(4) . . . . ?
C19 C20 C21 Ru1 53.2(2) . . . . ?
C19 C20 C21 C22 -0.6(4) . . . . ?
C19 C20 C21 C24 -178.8(2) . . . . ?
C19 C20 C21 Ru2 54.9(2) . . . . ?
C19 C18 C23 Ru1 -54.6(2) . . . . ?
C19 C18 C23 C22 -1.8(4) . . . . ?
C19 C18 C23 Ru2 -53.6(2) . . . . ?
C3 C2 C1 N2 -177.1(2) . . . . ?
C3 C2 C1 C6 3.7(4) . . . . ?
C3 C4 C5 C6 2.8(4) . . . . ?
F1 C16 C15 C14 -179.3(2) . . . . ?
C16 C15 C14 C13 1.8(5) . . . . ?
C17 C18 C23 Ru1 122.4(2) . . . . ?
C17 C18 C23 C22 175.2(2) . . . . ?
C17 C18 C23 Ru2 123.4(2) . . . . ?
C23 C22 C21 Ru1 -54.2(2) . . . . ?
C23 C22 C21 C20 0.2(4) . . . . ?
C23 C22 C21 C24 178.4(2) . . . . ?
C23 C22 C21 Ru2 -54.6(2) . . . . ?
C13 C12 C11 N1 179.5(2) . . . . ?
C13 C12 C11 C16 2.7(4) . . . . ?
C21 C20 C19 Ru1 -53.5(2) . . . . ?
C21 C20 C19 C18 -0.2(4) . . . . ?
C21 C20 C19 Ru2 -55.1(2) . . . . ?
C21 C22 C23 Ru1 54.5(2) . . . . ?
C21 C22 C23 C18 1.0(4) . . . . ?
C21 C22 C23 Ru2 53.6(2) . . . . ?
C5 C6 C7 C8 178.8(2) . . . . ?
C5 C4 C3 C2 -3.7(4) . . . . ?
Ru2 N1 C10 O1 -173.26(18) . . . . ?
Ru2 N1 C10 C9 10.3(3) . . . . ?
Ru2 N1 C11 C12 -72.9(3) . . . . ?
Ru2 N1 C11 C16 103.9(2) . . . . ?
Ru2 N2 C9 C10 -5.3(3) . . . . ?
Ru2 N2 C9 C8 176.98(19) . . . . ?
Ru2 N2 C1 C2 7.4(3) . . . . ?
Ru2 N2 C1 C6 -173.36(17) . . . . ?
Ru2 C20 C19 C18 54.9(2) . . . . ?
Ru2 C20 C21 C22 -55.5(2) . . . . ?
Ru2 C20 C21 C24 126.3(2) . . . . ?
Ru2 C22 C23 C18 -52.5(2) . . . . ?
Ru2 C22 C21 C20 54.8(2) . . . . ?
Ru2 C22 C21 C24 -127.0(2) . . . . ?
Ru2 C19 C18 C17 -122.4(2) . . . . ?
Ru2 C19 C18 C23 54.6(2) . . . . ?
Ru2 C18 C23 C22 51.8(2) . . . . ?
Ru2 C21 C24 C25 171.5(3) . . . . ?
Ru2 C21 C24 C26 -63.6(4) . . . . ?
_shelx_SHELXL_version_number 2014/7
_iucr_refine_instructions_details
;
shelxl.res created by SHELXL-2014/7
TITL Compound X
REM Compound X
REM 139 parameters refined using 0 restraints
REM Highest difference peak 8.762, deepest hole -7.630, 1-sigma level 0.377
REM 302 parameters refined using 0 restraints
REM Highest difference peak 7.817, deepest hole -8.111, 1-sigma level 0.346
REM 318 parameters refined using 0 restraints
REM Highest difference peak 8.253, deepest hole -7.962, 1-sigma level 0.364
REM 299 parameters refined using 0 restraints
REM Highest difference peak 8.105, deepest hole -7.923, 1-sigma level 0.362
REM 319 parameters refined using 0 restraints
REM Highest difference peak 7.682, deepest hole -7.924, 1-sigma level 0.269
REM 320 parameters refined using 0 restraints
REM Highest difference peak 7.694, deepest hole -7.915, 1-sigma level 0.268
REM Highest difference peak 7.693, deepest hole -7.916, 1-sigma level 0.268
CELL 0.71073 9.273 9.967 13.784 101.1 93.414 100.401
ZERR 1 0.0002 0.0002 0.0004 0.001 0.001 0.001
LATT 1
SFAC C H Cl F N O P Ru
UNIT 52 49 2 8 4 2 1 2
L.S. 8
PLAN 20
SIZE 0.23 0.1 0.03
TEMP -125
FREE F3A F3B
FREE F2A F2B
FREE F4A F4B
GRID
BOND $H
MORE -1
CONF
fmap 2
acta 52
MERG 2
OMIT -3 180
OMIT -1 0 1
OMIT 0 0 1
OMIT 0 1 0
REM
REM
REM
WGHT 0.054800 0.445100
FVAR 0.33590
PART 1
RU1 8 10.289399 10.399800 10.253800 10.50000 0.02345 0.02146 =
0.02152 0.00357 -0.00275 0.00442
PART 0
CL1 3 0.415837 0.527202 0.144033 11.00000 0.02733 0.03171 =
0.03038 0.01096 -0.00090 0.00189
O1 6 0.121806 0.073048 0.010112 11.00000 0.02897 0.02851 =
0.02903 -0.00268 -0.00158 0.00111
N1 5 0.270758 0.222478 0.139820 11.00000 0.02365 0.02544 =
0.02549 0.00573 -0.00026 0.00433
N2 5 0.099662 0.401722 0.160405 11.00000 0.02209 0.02468 =
0.02560 0.00712 0.00124 0.00515
C2 1 0.074517 0.635071 0.237502 11.00000 0.03248 0.03154 =
0.03122 0.01083 0.00420 0.00888
AFIX 43
H2 2 0.166569 0.648871 0.275824 11.00000 -1.20000
AFIX 0
C10 1 0.151996 0.185680 0.078083 11.00000 0.02383 0.02682 =
0.02557 0.00629 0.00285 0.00265
C8 1 -0.071842 0.271327 0.021346 11.00000 0.02589 0.03405 =
0.02929 0.00992 -0.00357 -0.00086
AFIX 43
H8 2 -0.097889 0.191044 -0.030744 11.00000 -1.20000
AFIX 0
C9 1 0.054818 0.289464 0.087507 11.00000 0.02355 0.02740 =
0.02443 0.00659 0.00126 0.00200
C12 1 0.515538 0.168354 0.114738 11.00000 0.02959 0.03334 =
0.03443 0.00219 0.00089 0.00583
AFIX 43
H12 2 0.547827 0.257571 0.099983 11.00000 -1.20000
AFIX 0
C1 1 0.021373 0.508414 0.168922 11.00000 0.02384 0.02975 =
0.02917 0.01183 0.00450 0.00705
C11 1 0.372291 0.129525 0.137358 11.00000 0.02599 0.02653 =
0.02500 0.00236 -0.00253 0.00685
C6 1 -0.112041 0.492415 0.108034 11.00000 0.02629 0.03624 =
0.03323 0.01539 0.00549 0.00685
C20 1 0.304652 0.264136 0.359950 11.00000 0.04201 0.02717 =
0.02067 0.00808 -0.00262 0.00694
AFIX 43
H20 2 0.293051 0.165586 0.349385 11.00000 -1.20000
AFIX 0
C7 1 -0.156990 0.370736 0.032972 11.00000 0.02196 0.04195 =
0.03544 0.01636 -0.00155 0.00383
AFIX 43
H7 2 -0.245520 0.358193 -0.008978 11.00000 -1.20000
AFIX 0
C4 1 -0.143535 0.719349 0.193137 11.00000 0.04026 0.04286 =
0.04488 0.01911 0.01200 0.02241
AFIX 43
H4 2 -0.200961 0.789697 0.204704 11.00000 -1.20000
AFIX 0
C22 1 0.205501 0.474264 0.393390 11.00000 0.03889 0.03616 =
0.02291 0.00438 0.00263 0.01227
AFIX 43
H22 2 0.124564 0.519529 0.405386 11.00000 -1.20000
AFIX 0
C19 1 0.447030 0.345175 0.358041 11.00000 0.03169 0.04158 =
0.02361 0.00797 -0.00323 0.01282
AFIX 43
H19 2 0.528178 0.300063 0.346527 11.00000 -1.20000
AFIX 0
C18 1 0.469065 0.491540 0.373029 11.00000 0.02956 0.03838 =
0.02268 0.00381 -0.00826 -0.00138
C3 1 -0.006838 0.738506 0.248892 11.00000 0.04395 0.03218 =
0.03763 0.01243 0.01259 0.01571
AFIX 43
H3 2 0.029719 0.823783 0.294914 11.00000 -1.20000
AFIX 0
PART 1
P1 7 10.500000 10.000000 10.500000 10.50000 0.06557 0.03177 =
0.04625 0.01177 -0.00525 0.01507
PART 0
F1 4 0.192364 -0.032766 0.188920 11.00000 0.04036 0.03412 =
0.04421 0.01109 0.00581 -0.00122
C16 1 0.331283 0.001448 0.162469 11.00000 0.03232 0.03063 =
0.02765 0.00272 -0.00071 0.00385
C17 1 0.616662 0.576846 0.363855 11.00000 0.03723 0.05732 =
0.03571 0.01174 -0.00856 -0.00810
AFIX 137
H17A 2 0.674542 0.517753 0.324081 11.00000 -1.50000
H17B 2 0.668832 0.614973 0.430135 11.00000 -1.50000
H17C 2 0.602956 0.653494 0.331363 11.00000 -1.50000
AFIX 0
C23 1 0.346107 0.556277 0.392377 11.00000 0.04354 0.02921 =
0.02148 0.00195 -0.00307 0.00407
AFIX 43
H23 2 0.358701 0.654998 0.404649 11.00000 -1.20000
AFIX 0
C15 1 0.425083 -0.091641 0.162458 11.00000 0.05409 0.03073 =
0.03605 0.00824 -0.00387 0.01516
AFIX 43
H15 2 0.393780 -0.179282 0.179881 11.00000 -1.20000
AFIX 0
C13 1 0.611969 0.075955 0.113737 11.00000 0.03187 0.04926 =
0.04266 0.00397 0.00158 0.01347
AFIX 43
H13 2 0.709895 0.101573 0.097485 11.00000 -1.20000
AFIX 0
C21 1 0.180318 0.325049 0.376969 11.00000 0.03151 0.03942 =
0.02079 0.00877 -0.00149 0.00345
C14 1 0.564635 -0.053588 0.136535 11.00000 0.04511 0.04980 =
0.04438 0.00400 -0.00395 0.02707
AFIX 43
H14 2 0.630174 -0.116971 0.134117 11.00000 -1.20000
AFIX 0
PART 1
F2A 4 0.393898 -0.082096 0.402588 10.50000 0.14777 0.06864 =
0.05038 0.00811 -0.02528 -0.00538
F4A 4 0.389165 0.080201 0.542236 10.50000 0.16615 0.07077 =
0.22819 0.06806 0.10439 0.08093
PART 0
C24 1 0.031150 0.234355 0.380276 11.00000 0.03845 0.05770 =
0.03805 0.01503 0.00314 -0.00668
AFIX 13
H24 2 0.027198 0.143727 0.333037 11.00000 -1.20000
AFIX 0
C25 1 0.021984 0.202519 0.484445 11.00000 0.04630 0.10005 =
0.05722 0.04463 0.00300 -0.00841
AFIX 137
H25A 2 0.026762 0.289415 0.533069 11.00000 -1.50000
H25B 2 0.104496 0.159019 0.500702 11.00000 -1.50000
H25C 2 -0.071164 0.138771 0.486157 11.00000 -1.50000
AFIX 0
C26 1 -0.098918 0.289739 0.351324 11.00000 0.04541 0.09184 =
0.06769 0.03254 0.00550 0.00205
AFIX 137
H26A 2 -0.103337 0.374843 0.399453 11.00000 -1.50000
H26B 2 -0.188531 0.219932 0.350195 11.00000 -1.50000
H26C 2 -0.091085 0.311148 0.285137 11.00000 -1.50000
AFIX 0
C5 1 -0.194778 0.601565 0.122872 11.00000 0.02809 0.04631 =
0.04350 0.02051 0.00604 0.01424
AFIX 43
H5 2 -0.285346 0.591722 0.083687 11.00000 -1.20000
AFIX 0
PART 1
F3A 4 0.440738 -0.114553 0.556714 10.50000 0.09205 0.06321 =
0.08637 0.05361 -0.01819 -0.00880
F4B 4 0.398098 0.114261 0.537111 10.50000 0.10610 0.05163 =
0.07963 0.01426 0.01143 0.04839
F2B 4 0.367305 -0.068825 0.419794 10.50000 0.07490 0.10890 =
0.07888 0.00608 -0.02912 0.00671
F3B 4 0.424779 -0.105442 0.567328 10.50000 0.10056 0.10369 =
0.11102 0.06555 0.04164 0.04183
PART 0
PART 2
RU2 8 0.287679 0.392703 0.251530 10.50000 0.02206 0.02117 =
0.02185 0.00253 -0.00135 0.00254
HKLF 4
REM Compound X
REM R1 = 0.0351 for 4914 Fo > 4sig(Fo) and 0.0441 for all 5582 data
REM 358 parameters refined using 0 restraints
END
WGHT 0.0546 0.4482
REM Highest difference peak 1.086, deepest hole -0.940, 1-sigma level 0.141
Q1 1 -0.0392 0.1352 0.3086 11.00000 0.05 1.09
Q2 1 0.0000 0.0000 0.0000 10.50000 0.05 0.64
Q3 1 0.1371 0.8118 0.2412 11.00000 0.05 0.59
Q4 1 0.0023 0.6671 0.3436 11.00000 0.05 0.41
Q5 1 0.0570 0.4637 0.1639 11.00000 0.05 0.41
Q6 1 -0.0543 0.3620 -0.0619 11.00000 0.05 0.40
Q7 1 -0.1482 0.5529 0.1154 11.00000 0.05 0.39
Q8 1 0.0120 0.3925 0.0059 11.00000 0.05 0.39
Q9 1 -0.0270 0.7727 0.1216 11.00000 0.05 0.39
Q10 1 -0.0965 0.3701 0.0128 11.00000 0.05 0.39
Q11 1 -0.0273 0.7055 0.2577 11.00000 0.05 0.38
Q12 1 -0.0415 0.5040 0.1415 11.00000 0.05 0.38
Q13 1 -0.1046 0.7365 0.1805 11.00000 0.05 0.38
Q14 1 0.0275 0.6827 0.2401 11.00000 0.05 0.36
Q15 1 -0.1081 0.7214 0.2355 11.00000 0.05 0.36
Q16 1 -0.1471 0.8433 0.2016 11.00000 0.05 0.36
Q17 1 0.7592 0.6766 0.2977 11.00000 0.05 0.35
Q18 1 0.0796 0.2595 -0.0350 11.00000 0.05 0.35
Q19 1 0.4167 -0.1614 0.3218 11.00000 0.05 0.35
Q20 1 -0.0498 0.5972 0.0742 11.00000 0.05 0.35
REM The information below was added by Olex2.
REM
REM R1 = 0.0351 for 4914 Fo > 4sig(Fo) and 0.0441 for all 24567 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 1.09, deepest hole -0.94
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0441
REM R1_gt = 0.0351
REM wR_ref = 0.0953
REM GOOF = 1.042
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 24567
REM Reflections_gt = 4914
REM Parameters = n/a
REM Hole = -0.94
REM Peak = 1.09
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT430_I
;
PROBLEM: Short Inter D...A Contact O1 .. O1 .. 2.42 Ang.
RESPONSE: Structure is hydrogen bridged dimer, with hydrogen bridging the amide oxygen atoms.
;
# end Validation Reply Form
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_kr276p-1
_database_code_depnum_ccdc_archive 'CCDC 1472240'
_audit_update_record
;
2016-06-30 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;
_audit_creation_date 2016-06-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C52 H49 Cl2 F2 N4 O2, F6 P'
_chemical_formula_sum 'C52 H49 Cl2 F8 N4 O2 P Ru2'
_chemical_formula_weight 1217.96
_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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
_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.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.4160(19)
_cell_length_b 9.7140(19)
_cell_length_c 14.631(3)
_cell_angle_alpha 73.68(3)
_cell_angle_beta 85.08(3)
_cell_angle_gamma 74.22(3)
_cell_volume 1235.8(5)
_cell_formula_units_Z 1
_cell_measurement_reflns_used 37012
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 27.485
_cell_measurement_theta_min 0.998
_shelx_estimated_absorpt_T_max 0.907
_shelx_estimated_absorpt_T_min 0.766
_exptl_absorpt_coefficient_mu 0.828
_exptl_absorpt_correction_T_max 0.9072
_exptl_absorpt_correction_T_min 0.7661
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
Using multiple and symmetry related data measurements via the program SORTAV
See R. H. Blessing, Acta Cryst (1995), A51, 33-38
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour Orange
_exptl_crystal_density_diffrn 1.637
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Prism
_exptl_crystal_F_000 614
_exptl_crystal_size_max 0.34
_exptl_crystal_size_mid 0.19
_exptl_crystal_size_min 0.12
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0958
_diffrn_reflns_av_unetI/netI 0.0576
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 22510
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.472
_diffrn_reflns_theta_min 2.336
_diffrn_ambient_temperature 150.15
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer'
_diffrn_measurement_method '\w and \f scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed tube'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4944
_reflns_number_total 5590
_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 'DENZO-SMN (Otwinowski and Minor, 1997)'
_computing_data_collection 'COLLECT (Nonius, 1999)'
_computing_data_reduction 'DENZO-SMN (Otwinowski and Minor, 1997)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'local program'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max 0.653
_refine_diff_density_min -1.202
_refine_diff_density_rms 0.110
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.033
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 325
_refine_ls_number_reflns 5590
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0463
_refine_ls_R_factor_gt 0.0394
_refine_ls_restrained_S_all 1.033
_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^)+(0.0580P)^2^+0.5442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1008
_refine_ls_wR_factor_ref 0.1061
_refine_special_details
;
Reflections 0 0 1, 1 0 1, 1 0 0, 0 1 0 omitted as obscured by beamstop.
;
_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:
C24(H24)
2.b Aromatic/amide H refined with riding coordinates:
C2(H2), C8(H8), C7(H7), C4(H4), C20(H20), C3(H3), C22(H22), C23(H23), C5(H5),
C19(H19), C12(H12), C16(H16), C15(H15), C13(H13)
2.c Idealised Me refined as rotating group:
C17(H17A,H17B,H17C), 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
Ru1 Ru 0.81115(2) 0.97140(2) 0.23471(2) 0.02643(9) Uani 1 1 d . . . . .
Cl1 Cl 0.63532(7) 1.10551(7) 0.32811(5) 0.03174(15) Uani 1 1 d . . . . .
P1 P 0.0000 1.5000 0.0000 0.0325(2) Uani 1 2 d S T P . .
O1 O 0.8903(2) 0.5866(2) 0.46058(15) 0.0376(4) Uani 1 1 d . . . . .
N1 N 0.9662(2) 0.9357(2) 0.34216(15) 0.0267(4) Uani 1 1 d . . . . .
C18 C 0.9738(3) 0.9075(3) 0.12715(19) 0.0370(6) Uani 1 1 d . . . . .
C6 C 1.1612(3) 0.9844(3) 0.41837(19) 0.0294(5) Uani 1 1 d . . . . .
C1 C 1.0476(3) 1.0318(3) 0.34898(18) 0.0271(5) Uani 1 1 d . . . . .
C2 C 1.0188(3) 1.1778(3) 0.28835(19) 0.0305(5) Uani 1 1 d . . . . .
H2 H 0.9397 1.2131 0.2446 0.037 Uiso 1 1 calc R . . . .
C8 C 1.0936(3) 0.7541(3) 0.47917(19) 0.0306(5) Uani 1 1 d . . . . .
H8 H 1.1040 0.6600 0.5242 0.037 Uiso 1 1 calc R . . . .
C7 C 1.1819(3) 0.8437(3) 0.48337(19) 0.0312(5) Uani 1 1 d . . . . .
H7 H 1.2567 0.8105 0.5301 0.037 Uiso 1 1 calc R . . . .
C4 C 1.2225(3) 1.2199(3) 0.3585(2) 0.0354(6) Uani 1 1 d . . . . .
H4 H 1.2829 1.2835 0.3594 0.042 Uiso 1 1 calc R . . . .
C10 C 0.8859(3) 0.7135(3) 0.40064(19) 0.0289(5) Uani 1 1 d . . . . .
C20 C 0.8021(3) 1.1591(3) 0.10589(19) 0.0339(6) Uani 1 1 d . . . . .
H20 H 0.7875 1.2620 0.0997 0.041 Uiso 1 1 calc R . . . .
C3 C 1.1058(3) 1.2686(3) 0.2929(2) 0.0340(6) Uani 1 1 d . . . . .
H3 H 1.0871 1.3661 0.2512 0.041 Uiso 1 1 calc R . . . .
C9 C 0.9875(3) 0.8041(3) 0.40715(18) 0.0276(5) Uani 1 1 d . . . . .
C22 C 0.7041(3) 0.9481(3) 0.11444(19) 0.0343(6) Uani 1 1 d . . . . .
H22 H 0.6233 0.9074 0.1137 0.041 Uiso 1 1 calc R . . . .
C23 C 0.8512(3) 0.8529(3) 0.12541(19) 0.0361(6) Uani 1 1 d . . . . .
H23 H 0.8659 0.7500 0.1317 0.043 Uiso 1 1 calc R . . . .
C5 C 1.2483(3) 1.0828(3) 0.4203(2) 0.0334(6) Uani 1 1 d . . . . .
H5 H 1.3253 1.0518 0.4653 0.040 Uiso 1 1 calc R . . . .
C24 C 0.5251(3) 1.2058(3) 0.0954(2) 0.0417(7) Uani 1 1 d . . . . .
H24 H 0.5193 1.2745 0.1361 0.050 Uiso 1 1 calc R . . . .
C19 C 0.9459(3) 1.0641(3) 0.11607(19) 0.0357(6) Uani 1 1 d . . . . .
H19 H 1.0269 1.1050 0.1156 0.043 Uiso 1 1 calc R . . . .
C21 C 0.6782(3) 1.1016(3) 0.10479(19) 0.0341(6) Uani 1 1 d . . . . .
N2 N 0.7889(2) 0.7773(2) 0.33316(16) 0.0275(4) Uani 1 1 d . . . . .
C11 C 0.6831(3) 0.7002(3) 0.32179(19) 0.0308(5) Uani 1 1 d . . . . .
C17 C 1.1261(4) 0.8074(4) 0.1433(2) 0.0510(9) Uani 1 1 d . . . . .
H17A H 1.1228 0.7149 0.1914 0.077 Uiso 1 1 calc GR . . . .
H17B H 1.1891 0.8565 0.1655 0.077 Uiso 1 1 calc GR . . . .
H17C H 1.1663 0.7851 0.0835 0.077 Uiso 1 1 calc GR . . . .
C12 C 0.5345(3) 0.7639(3) 0.3344(2) 0.0359(6) Uani 1 1 d . . . . .
H12 H 0.5046 0.8532 0.3537 0.043 Uiso 1 1 calc R . . . .
C14 C 0.4773(3) 0.5675(3) 0.2904(2) 0.0428(7) Uani 1 1 d . . . . .
C16 C 0.7275(3) 0.5707(3) 0.2937(2) 0.0375(6) Uani 1 1 d . . . . .
H16 H 0.8296 0.5280 0.2854 0.045 Uiso 1 1 calc R . . . .
C15 C 0.6240(4) 0.5022(3) 0.2775(3) 0.0444(7) Uani 1 1 d . . . . .
H15 H 0.6536 0.4131 0.2581 0.053 Uiso 1 1 calc R . . . .
C13 C 0.4297(3) 0.6967(4) 0.3188(2) 0.0426(7) Uani 1 1 d . . . . .
H13 H 0.3275 0.7387 0.3275 0.051 Uiso 1 1 calc R . . . .
C25 C 0.5035(4) 1.2996(4) -0.0089(2) 0.0500(8) Uani 1 1 d . . . . .
H25A H 0.5784 1.3557 -0.0265 0.075 Uiso 1 1 calc GR . . . .
H25B H 0.4050 1.3687 -0.0162 0.075 Uiso 1 1 calc GR . . . .
H25C H 0.5133 1.2340 -0.0505 0.075 Uiso 1 1 calc GR . . . .
C26 C 0.4027(4) 1.1270(5) 0.1272(3) 0.0561(9) Uani 1 1 d . . . . .
H26A H 0.3998 1.0666 0.0842 0.084 Uiso 1 1 calc GR . . . .
H26B H 0.3078 1.2009 0.1257 0.084 Uiso 1 1 calc GR . . . .
H26C H 0.4219 1.0628 0.1922 0.084 Uiso 1 1 calc GR . . . .
F2 F -0.0936(2) 1.4739(2) 0.09730(14) 0.0532(5) Uani 1 1 d . . . . .
F1 F 0.3739(2) 0.5042(2) 0.27277(17) 0.0595(5) Uani 1 1 d . . . . .
F3 F 0.0787(2) 1.32625(19) 0.02435(15) 0.0529(5) Uani 1 1 d . . . . .
F4 F 0.1265(2) 1.5249(2) 0.05415(15) 0.0563(5) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.02611(13) 0.02512(13) 0.02903(13) -0.00704(9) -0.00346(9) -0.00751(9)
Cl1 0.0295(3) 0.0302(3) 0.0364(3) -0.0123(3) -0.0032(3) -0.0050(2)
P1 0.0370(5) 0.0282(5) 0.0331(5) -0.0069(4) -0.0018(4) -0.0105(4)
O1 0.0398(11) 0.0262(9) 0.0450(11) 0.0004(8) -0.0098(9) -0.0134(8)
N1 0.0256(10) 0.0258(10) 0.0294(11) -0.0067(9) -0.0014(8) -0.0082(8)
C18 0.0362(15) 0.0458(17) 0.0258(13) -0.0096(12) 0.0014(11) -0.0057(12)
C6 0.0255(12) 0.0307(13) 0.0348(13) -0.0119(11) -0.0006(10) -0.0087(10)
C1 0.0248(12) 0.0274(12) 0.0313(13) -0.0108(10) 0.0006(10) -0.0077(10)
C2 0.0310(13) 0.0302(13) 0.0312(13) -0.0082(11) -0.0012(10) -0.0092(11)
C8 0.0304(13) 0.0269(12) 0.0333(13) -0.0059(11) -0.0051(11) -0.0065(10)
C7 0.0287(13) 0.0317(13) 0.0341(14) -0.0100(11) -0.0058(10) -0.0061(11)
C4 0.0344(14) 0.0364(14) 0.0427(15) -0.0133(12) 0.0025(12) -0.0191(12)
C10 0.0281(12) 0.0260(12) 0.0333(13) -0.0072(11) -0.0015(10) -0.0083(10)
C20 0.0388(15) 0.0314(14) 0.0310(13) -0.0045(11) -0.0042(11) -0.0109(11)
C3 0.0364(14) 0.0278(13) 0.0385(14) -0.0072(11) 0.0024(11) -0.0120(11)
C9 0.0259(12) 0.0280(12) 0.0293(13) -0.0089(10) -0.0032(10) -0.0056(10)
C22 0.0384(15) 0.0392(15) 0.0307(13) -0.0113(12) -0.0058(11) -0.0152(12)
C23 0.0487(16) 0.0335(14) 0.0286(13) -0.0138(11) -0.0018(12) -0.0084(12)
C5 0.0279(13) 0.0378(15) 0.0385(14) -0.0128(12) -0.0024(11) -0.0119(11)
C24 0.0351(15) 0.0448(17) 0.0404(16) -0.0113(14) -0.0092(12) 0.0000(13)
C19 0.0362(14) 0.0450(16) 0.0281(13) -0.0064(12) -0.0003(11) -0.0178(12)
C21 0.0353(14) 0.0370(14) 0.0280(13) -0.0062(11) -0.0062(11) -0.0071(12)
N2 0.0272(11) 0.0248(10) 0.0326(11) -0.0079(9) -0.0033(9) -0.0089(8)
C11 0.0304(13) 0.0289(13) 0.0341(13) -0.0047(11) -0.0056(11) -0.0118(11)
C17 0.0402(17) 0.064(2) 0.0376(16) -0.0158(16) 0.0014(13) 0.0071(15)
C12 0.0298(14) 0.0370(15) 0.0445(16) -0.0154(13) 0.0004(11) -0.0103(11)
C14 0.0406(16) 0.0393(16) 0.0559(19) -0.0106(14) -0.0076(14) -0.0224(13)
C16 0.0322(14) 0.0289(13) 0.0532(18) -0.0134(13) -0.0077(12) -0.0064(11)
C15 0.0454(17) 0.0290(14) 0.064(2) -0.0161(14) -0.0131(15) -0.0115(13)
C13 0.0315(15) 0.0487(17) 0.0506(18) -0.0135(15) 0.0006(13) -0.0157(13)
C25 0.0406(17) 0.0491(19) 0.0503(19) -0.0060(15) -0.0122(14) 0.0010(14)
C26 0.0335(16) 0.076(3) 0.051(2) -0.0091(18) -0.0044(14) -0.0073(16)
F2 0.0621(12) 0.0541(11) 0.0423(10) -0.0107(9) 0.0129(9) -0.0199(10)
F1 0.0487(11) 0.0510(11) 0.0894(15) -0.0168(11) -0.0165(10) -0.0276(9)
F3 0.0644(12) 0.0289(9) 0.0587(12) -0.0074(8) -0.0035(10) -0.0048(8)
F4 0.0562(12) 0.0630(13) 0.0587(12) -0.0146(10) -0.0161(10) -0.0272(10)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 Cl1 2.3968(10) . ?
Ru1 N1 2.130(2) . ?
Ru1 C18 2.197(3) . ?
Ru1 C20 2.213(3) . ?
Ru1 C22 2.194(3) . ?
Ru1 C23 2.173(3) . ?
Ru1 C19 2.190(3) . ?
Ru1 C21 2.231(3) . ?
Ru1 N2 2.076(2) . ?
P1 F2 1.6035(19) . ?
P1 F2 1.6034(19) 2_585 ?
P1 F3 1.5973(18) 2_585 ?
P1 F3 1.5973(18) . ?
P1 F4 1.5909(18) . ?
P1 F4 1.5909(18) 2_585 ?
O1 C10 1.289(3) . ?
N1 C1 1.386(3) . ?
N1 C9 1.338(3) . ?
C18 C23 1.400(4) . ?
C18 C19 1.435(4) . ?
C18 C17 1.492(4) . ?
C6 C1 1.429(4) . ?
C6 C7 1.403(4) . ?
C6 C5 1.426(4) . ?
C1 C2 1.413(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.375(4) . ?
C8 H8 0.9500 . ?
C8 C7 1.373(4) . ?
C8 C9 1.404(4) . ?
C7 H7 0.9500 . ?
C4 H4 0.9500 . ?
C4 C3 1.412(4) . ?
C4 C5 1.354(4) . ?
C10 C9 1.490(4) . ?
C10 N2 1.302(3) . ?
C20 H20 0.9500 . ?
C20 C19 1.409(4) . ?
C20 C21 1.427(4) . ?
C3 H3 0.9500 . ?
C22 H22 0.9500 . ?
C22 C23 1.434(4) . ?
C22 C21 1.412(4) . ?
C23 H23 0.9500 . ?
C5 H5 0.9500 . ?
C24 H24 1.0000 . ?
C24 C21 1.511(4) . ?
C24 C25 1.541(4) . ?
C24 C26 1.522(5) . ?
C19 H19 0.9500 . ?
N2 C11 1.444(3) . ?
C11 C12 1.387(4) . ?
C11 C16 1.379(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C12 H12 0.9500 . ?
C12 C13 1.388(4) . ?
C14 C15 1.375(5) . ?
C14 C13 1.380(4) . ?
C14 F1 1.359(3) . ?
C16 H16 0.9500 . ?
C16 C15 1.390(4) . ?
C15 H15 0.9500 . ?
C13 H13 0.9500 . ?
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
N1 Ru1 Cl1 86.15(6) . . ?
N1 Ru1 C18 96.44(10) . . ?
N1 Ru1 C20 118.47(10) . . ?
N1 Ru1 C22 161.77(10) . . ?
N1 Ru1 C23 123.58(10) . . ?
N1 Ru1 C19 95.29(10) . . ?
N1 Ru1 C21 154.77(10) . . ?
C18 Ru1 Cl1 164.92(9) . . ?
C18 Ru1 C20 68.72(11) . . ?
C18 Ru1 C21 81.57(11) . . ?
C20 Ru1 Cl1 96.96(8) . . ?
C20 Ru1 C21 37.47(10) . . ?
C22 Ru1 Cl1 111.01(8) . . ?
C22 Ru1 C18 68.66(11) . . ?
C22 Ru1 C20 67.10(11) . . ?
C22 Ru1 C21 37.19(10) . . ?
C23 Ru1 Cl1 147.96(8) . . ?
C23 Ru1 C18 37.37(11) . . ?
C23 Ru1 C20 79.97(11) . . ?
C23 Ru1 C22 38.35(11) . . ?
C23 Ru1 C19 67.26(11) . . ?
C23 Ru1 C21 68.33(11) . . ?
C19 Ru1 Cl1 126.87(8) . . ?
C19 Ru1 C18 38.19(11) . . ?
C19 Ru1 C20 37.32(11) . . ?
C19 Ru1 C22 79.56(11) . . ?
C19 Ru1 C21 67.62(11) . . ?
C21 Ru1 Cl1 89.75(8) . . ?
N2 Ru1 Cl1 87.61(7) . . ?
N2 Ru1 N1 76.10(9) . . ?
N2 Ru1 C18 107.45(10) . . ?
N2 Ru1 C20 164.89(9) . . ?
N2 Ru1 C22 97.81(10) . . ?
N2 Ru1 C23 88.51(10) . . ?
N2 Ru1 C19 144.31(10) . . ?
N2 Ru1 C21 128.63(10) . . ?
F2 P1 F2 180.0 2_585 . ?
F3 P1 F2 90.03(11) 2_585 2_585 ?
F3 P1 F2 89.97(11) 2_585 . ?
F3 P1 F2 89.97(11) . 2_585 ?
F3 P1 F2 90.03(11) . . ?
F3 P1 F3 180.0 . 2_585 ?
F4 P1 F2 89.94(11) . . ?
F4 P1 F2 90.06(11) 2_585 . ?
F4 P1 F2 89.94(11) 2_585 2_585 ?
F4 P1 F2 90.06(11) . 2_585 ?
F4 P1 F3 90.14(11) 2_585 2_585 ?
F4 P1 F3 89.86(11) 2_585 . ?
F4 P1 F3 90.14(11) . . ?
F4 P1 F3 89.85(11) . 2_585 ?
F4 P1 F4 180.0 2_585 . ?
C1 N1 Ru1 126.80(17) . . ?
C9 N1 Ru1 114.76(17) . . ?
C9 N1 C1 118.4(2) . . ?
C23 C18 Ru1 70.38(16) . . ?
C23 C18 C19 116.9(3) . . ?
C23 C18 C17 121.8(3) . . ?
C19 C18 Ru1 70.67(16) . . ?
C19 C18 C17 121.3(3) . . ?
C17 C18 Ru1 127.7(2) . . ?
C7 C6 C1 119.0(2) . . ?
C7 C6 C5 122.1(2) . . ?
C5 C6 C1 118.9(2) . . ?
N1 C1 C6 120.2(2) . . ?
N1 C1 C2 120.7(2) . . ?
C2 C1 C6 119.1(2) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 C1 119.8(3) . . ?
C3 C2 H2 120.1 . . ?
C7 C8 H8 120.6 . . ?
C7 C8 C9 118.8(2) . . ?
C9 C8 H8 120.6 . . ?
C6 C7 H7 120.2 . . ?
C8 C7 C6 119.7(2) . . ?
C8 C7 H7 120.2 . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C5 C4 C3 120.2(3) . . ?
O1 C10 C9 122.0(2) . . ?
O1 C10 N2 123.7(2) . . ?
N2 C10 C9 114.2(2) . . ?
Ru1 C20 H20 130.3 . . ?
C19 C20 Ru1 70.48(16) . . ?
C19 C20 H20 119.8 . . ?
C19 C20 C21 120.3(3) . . ?
C21 C20 Ru1 71.96(16) . . ?
C21 C20 H20 119.8 . . ?
C2 C3 C4 121.3(3) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
N1 C9 C8 123.6(2) . . ?
N1 C9 C10 115.1(2) . . ?
C8 C9 C10 121.2(2) . . ?
Ru1 C22 H22 130.1 . . ?
C23 C22 Ru1 70.00(15) . . ?
C23 C22 H22 119.6 . . ?
C21 C22 Ru1 72.81(15) . . ?
C21 C22 H22 119.6 . . ?
C21 C22 C23 120.7(3) . . ?
Ru1 C23 H23 129.6 . . ?
C18 C23 Ru1 72.25(16) . . ?
C18 C23 C22 121.8(3) . . ?
C18 C23 H23 119.1 . . ?
C22 C23 Ru1 71.65(15) . . ?
C22 C23 H23 119.1 . . ?
C6 C5 H5 119.7 . . ?
C4 C5 C6 120.7(3) . . ?
C4 C5 H5 119.7 . . ?
C21 C24 H24 108.0 . . ?
C21 C24 C25 108.4(3) . . ?
C21 C24 C26 113.7(3) . . ?
C25 C24 H24 108.0 . . ?
C26 C24 H24 108.0 . . ?
C26 C24 C25 110.6(3) . . ?
Ru1 C19 H19 130.5 . . ?
C18 C19 Ru1 71.14(16) . . ?
C18 C19 H19 119.0 . . ?
C20 C19 Ru1 72.20(17) . . ?
C20 C19 C18 122.1(3) . . ?
C20 C19 H19 119.0 . . ?
C20 C21 Ru1 70.57(16) . . ?
C20 C21 C24 119.1(3) . . ?
C22 C21 Ru1 70.00(15) . . ?
C22 C21 C20 118.2(3) . . ?
C22 C21 C24 122.7(3) . . ?
C24 C21 Ru1 130.0(2) . . ?
C10 N2 Ru1 118.43(17) . . ?
C10 N2 C11 118.7(2) . . ?
C11 N2 Ru1 122.25(17) . . ?
C12 C11 N2 118.4(2) . . ?
C16 C11 N2 121.0(2) . . ?
C16 C11 C12 120.5(3) . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C11 C12 H12 120.1 . . ?
C11 C12 C13 119.8(3) . . ?
C13 C12 H12 120.1 . . ?
C15 C14 C13 122.8(3) . . ?
F1 C14 C15 119.0(3) . . ?
F1 C14 C13 118.2(3) . . ?
C11 C16 H16 119.8 . . ?
C11 C16 C15 120.5(3) . . ?
C15 C16 H16 119.8 . . ?
C14 C15 C16 118.0(3) . . ?
C14 C15 H15 121.0 . . ?
C16 C15 H15 121.0 . . ?
C12 C13 H13 120.8 . . ?
C14 C13 C12 118.5(3) . . ?
C14 C13 H13 120.8 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 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
Ru1 N1 C1 C6 -171.99(18) . . . . ?
Ru1 N1 C1 C2 8.6(3) . . . . ?
Ru1 N1 C9 C8 174.7(2) . . . . ?
Ru1 N1 C9 C10 -7.5(3) . . . . ?
Ru1 C18 C23 C22 54.0(2) . . . . ?
Ru1 C18 C19 C20 -53.4(2) . . . . ?
Ru1 C20 C19 C18 53.0(2) . . . . ?
Ru1 C20 C21 C22 -53.1(2) . . . . ?
Ru1 C20 C21 C24 125.7(3) . . . . ?
Ru1 C22 C23 C18 -54.3(2) . . . . ?
Ru1 C22 C21 C20 53.4(2) . . . . ?
Ru1 C22 C21 C24 -125.4(3) . . . . ?
Ru1 N2 C11 C12 -71.5(3) . . . . ?
Ru1 N2 C11 C16 104.8(3) . . . . ?
O1 C10 C9 N1 -177.6(2) . . . . ?
O1 C10 C9 C8 0.3(4) . . . . ?
O1 C10 N2 Ru1 -173.9(2) . . . . ?
O1 C10 N2 C11 -2.4(4) . . . . ?
N1 C1 C2 C3 -176.6(2) . . . . ?
C6 C1 C2 C3 3.9(4) . . . . ?
C1 N1 C9 C8 -3.5(4) . . . . ?
C1 N1 C9 C10 174.3(2) . . . . ?
C1 C6 C7 C8 0.2(4) . . . . ?
C1 C6 C5 C4 1.1(4) . . . . ?
C1 C2 C3 C4 -1.2(4) . . . . ?
C7 C6 C1 N1 -4.4(4) . . . . ?
C7 C6 C1 C2 175.1(2) . . . . ?
C7 C6 C5 C4 -177.8(3) . . . . ?
C7 C8 C9 N1 -0.6(4) . . . . ?
C7 C8 C9 C10 -178.3(2) . . . . ?
C10 N2 C11 C12 117.4(3) . . . . ?
C10 N2 C11 C16 -66.3(4) . . . . ?
C3 C4 C5 C6 1.7(4) . . . . ?
C9 N1 C1 C6 6.0(4) . . . . ?
C9 N1 C1 C2 -173.5(2) . . . . ?
C9 C8 C7 C6 2.3(4) . . . . ?
C9 C10 N2 Ru1 9.7(3) . . . . ?
C9 C10 N2 C11 -178.8(2) . . . . ?
C23 C18 C19 Ru1 54.8(2) . . . . ?
C23 C18 C19 C20 1.3(4) . . . . ?
C23 C22 C21 Ru1 -53.1(2) . . . . ?
C23 C22 C21 C20 0.2(4) . . . . ?
C23 C22 C21 C24 -178.5(3) . . . . ?
C5 C6 C1 N1 176.6(2) . . . . ?
C5 C6 C1 C2 -3.9(4) . . . . ?
C5 C6 C7 C8 179.1(2) . . . . ?
C5 C4 C3 C2 -1.7(4) . . . . ?
C19 C18 C23 Ru1 -54.9(2) . . . . ?
C19 C18 C23 C22 -0.9(4) . . . . ?
C19 C20 C21 Ru1 53.3(2) . . . . ?
C19 C20 C21 C22 0.2(4) . . . . ?
C19 C20 C21 C24 179.0(3) . . . . ?
C21 C20 C19 Ru1 -54.0(2) . . . . ?
C21 C20 C19 C18 -1.0(4) . . . . ?
C21 C22 C23 Ru1 54.4(2) . . . . ?
C21 C22 C23 C18 0.1(4) . . . . ?
N2 C10 C9 N1 -1.1(3) . . . . ?
N2 C10 C9 C8 176.8(2) . . . . ?
N2 C11 C12 C13 176.4(3) . . . . ?
N2 C11 C16 C15 -176.1(3) . . . . ?
C11 C12 C13 C14 -0.4(5) . . . . ?
C11 C16 C15 C14 -0.1(5) . . . . ?
C17 C18 C23 Ru1 122.9(3) . . . . ?
C17 C18 C23 C22 177.0(3) . . . . ?
C17 C18 C19 Ru1 -123.1(3) . . . . ?
C17 C18 C19 C20 -176.5(3) . . . . ?
C12 C11 C16 C15 0.1(5) . . . . ?
C16 C11 C12 C13 0.1(4) . . . . ?
C15 C14 C13 C12 0.4(5) . . . . ?
C13 C14 C15 C16 -0.2(5) . . . . ?
C25 C24 C21 Ru1 163.9(2) . . . . ?
C25 C24 C21 C20 75.6(3) . . . . ?
C25 C24 C21 C22 -105.7(3) . . . . ?
C26 C24 C21 Ru1 -72.7(4) . . . . ?
C26 C24 C21 C20 -161.0(3) . . . . ?
C26 C24 C21 C22 17.7(4) . . . . ?
F1 C14 C15 C16 178.5(3) . . . . ?
F1 C14 C13 C12 -178.3(3) . . . . ?
_shelx_SHELXL_version_number 2014/7
_iucr_refine_instructions_details
;
kr276p-1.res created by SHELXL-2014/7
TITL kr276p-1 in P-1
CELL 0.71073 9.416 9.714 14.631 73.677 85.077 74.216
ZERR 1 0.0019 0.0019 0.0029 0.03 0.03 0.03
LATT 1
SFAC C H Cl F N O P Ru
UNIT 52 49 2 8 4 2 1 2
L.S. 8
PLAN 20
SIZE 0.34 0.19 0.12
TEMP -123
GRID
MORE -1
BOND $H
CONF
fmap
acta
MERG 2
OMIT 0 0 1
OMIT 1 0 1
OMIT 1 0 0
OMIT 0 1 0
OMIT -1 0 1
REM
REM
REM
WGHT 0.058000 0.544200
FVAR 0.40352
RU1 8 0.811152 0.971402 0.234709 11.00000 0.02611 0.02512 =
0.02903 -0.00704 -0.00346 -0.00751
CL1 3 0.635321 1.105507 0.328108 11.00000 0.02954 0.03021 =
0.03644 -0.01229 -0.00316 -0.00502
P1 7 0.000000 1.500000 0.000000 10.50000 0.03696 0.02817 =
0.03312 -0.00691 -0.00182 -0.01055
O1 6 0.890259 0.586569 0.460577 11.00000 0.03977 0.02622 =
0.04502 0.00043 -0.00983 -0.01336
N1 5 0.966222 0.935709 0.342156 11.00000 0.02565 0.02575 =
0.02937 -0.00666 -0.00138 -0.00824
C18 1 0.973807 0.907515 0.127148 11.00000 0.03619 0.04578 =
0.02581 -0.00964 0.00138 -0.00566
C6 1 1.161181 0.984374 0.418371 11.00000 0.02548 0.03066 =
0.03481 -0.01189 -0.00060 -0.00867
C1 1 1.047564 1.031766 0.348978 11.00000 0.02476 0.02744 =
0.03134 -0.01082 0.00055 -0.00774
C2 1 1.018837 1.177798 0.288349 11.00000 0.03099 0.03024 =
0.03121 -0.00818 -0.00115 -0.00920
AFIX 43
H2 2 0.939702 1.213058 0.244575 11.00000 -1.20000
AFIX 0
C8 1 1.093561 0.754129 0.479166 11.00000 0.03039 0.02693 =
0.03329 -0.00593 -0.00511 -0.00651
AFIX 43
H8 2 1.103973 0.660048 0.524173 11.00000 -1.20000
AFIX 0
C7 1 1.181881 0.843656 0.483369 11.00000 0.02869 0.03165 =
0.03411 -0.01002 -0.00582 -0.00609
AFIX 43
H7 2 1.256684 0.810458 0.530088 11.00000 -1.20000
AFIX 0
C4 1 1.222463 1.219908 0.358542 11.00000 0.03445 0.03635 =
0.04268 -0.01333 0.00248 -0.01911
AFIX 43
H4 2 1.282947 1.283475 0.359371 11.00000 -1.20000
AFIX 0
C10 1 0.885875 0.713496 0.400639 11.00000 0.02812 0.02600 =
0.03326 -0.00722 -0.00150 -0.00834
C20 1 0.802085 1.159112 0.105885 11.00000 0.03882 0.03136 =
0.03095 -0.00454 -0.00422 -0.01090
AFIX 43
H20 2 0.787544 1.261986 0.099715 11.00000 -1.20000
AFIX 0
C3 1 1.105819 1.268645 0.292944 11.00000 0.03635 0.02778 =
0.03849 -0.00715 0.00241 -0.01202
AFIX 43
H3 2 1.087098 1.366062 0.251195 11.00000 -1.20000
AFIX 0
C9 1 0.987538 0.804088 0.407150 11.00000 0.02595 0.02797 =
0.02929 -0.00887 -0.00319 -0.00560
C22 1 0.704137 0.948111 0.114436 11.00000 0.03842 0.03916 =
0.03071 -0.01132 -0.00582 -0.01522
AFIX 43
H22 2 0.623346 0.907438 0.113652 11.00000 -1.20000
AFIX 0
C23 1 0.851229 0.852878 0.125413 11.00000 0.04868 0.03347 =
0.02861 -0.01381 -0.00177 -0.00837
AFIX 43
H23 2 0.865872 0.749965 0.131673 11.00000 -1.20000
AFIX 0
C5 1 1.248341 1.082781 0.420280 11.00000 0.02792 0.03781 =
0.03846 -0.01277 -0.00245 -0.01195
AFIX 43
H5 2 1.325350 1.051833 0.465320 11.00000 -1.20000
AFIX 0
C24 1 0.525080 1.205761 0.095439 11.00000 0.03515 0.04484 =
0.04041 -0.01131 -0.00922 0.00001
AFIX 13
H24 2 0.519256 1.274503 0.136074 11.00000 -1.20000
AFIX 0
C19 1 0.945880 1.064092 0.116073 11.00000 0.03621 0.04498 =
0.02805 -0.00639 -0.00030 -0.01782
AFIX 43
H19 2 1.026936 1.104957 0.115596 11.00000 -1.20000
AFIX 0
C21 1 0.678152 1.101614 0.104788 11.00000 0.03534 0.03699 =
0.02804 -0.00617 -0.00621 -0.00708
N2 5 0.788897 0.777293 0.333160 11.00000 0.02716 0.02482 =
0.03262 -0.00792 -0.00333 -0.00887
C11 1 0.683128 0.700205 0.321792 11.00000 0.03044 0.02894 =
0.03407 -0.00475 -0.00559 -0.01177
C17 1 1.126075 0.807419 0.143291 11.00000 0.04021 0.06380 =
0.03760 -0.01576 0.00143 0.00708
AFIX 137
H17A 2 1.122790 0.714874 0.191409 11.00000 -1.50000
H17B 2 1.189090 0.856550 0.165544 11.00000 -1.50000
H17C 2 1.166329 0.785107 0.083519 11.00000 -1.50000
AFIX 0
C12 1 0.534542 0.763892 0.334418 11.00000 0.02979 0.03701 =
0.04449 -0.01537 0.00044 -0.01028
AFIX 43
H12 2 0.504638 0.853221 0.353674 11.00000 -1.20000
AFIX 0
C14 1 0.477263 0.567477 0.290410 11.00000 0.04061 0.03926 =
0.05588 -0.01061 -0.00758 -0.02238
C16 1 0.727530 0.570714 0.293735 11.00000 0.03224 0.02888 =
0.05323 -0.01340 -0.00768 -0.00636
AFIX 43
H16 2 0.829633 0.527988 0.285439 11.00000 -1.20000
AFIX 0
C15 1 0.623972 0.502242 0.277502 11.00000 0.04536 0.02900 =
0.06437 -0.01605 -0.01307 -0.01151
AFIX 43
H15 2 0.653614 0.413058 0.258074 11.00000 -1.20000
AFIX 0
C13 1 0.429695 0.696699 0.318831 11.00000 0.03153 0.04870 =
0.05055 -0.01347 0.00065 -0.01568
AFIX 43
H13 2 0.327537 0.738674 0.327523 11.00000 -1.20000
AFIX 0
C25 1 0.503471 1.299577 -0.008924 11.00000 0.04059 0.04908 =
0.05026 -0.00599 -0.01223 0.00104
AFIX 137
H25A 2 0.578378 1.355722 -0.026516 11.00000 -1.50000
H25B 2 0.404974 1.368708 -0.016156 11.00000 -1.50000
H25C 2 0.513315 1.233975 -0.050482 11.00000 -1.50000
AFIX 0
C26 1 0.402749 1.127007 0.127243 11.00000 0.03351 0.07554 =
0.05086 -0.00913 -0.00435 -0.00728
AFIX 137
H26A 2 0.399816 1.066604 0.084232 11.00000 -1.50000
H26B 2 0.307783 1.200875 0.125742 11.00000 -1.50000
H26C 2 0.421868 1.062828 0.192236 11.00000 -1.50000
AFIX 0
F2 4 -0.093605 1.473896 0.097302 11.00000 0.06214 0.05412 =
0.04233 -0.01065 0.01288 -0.01992
F1 4 0.373945 0.504237 0.272774 11.00000 0.04869 0.05105 =
0.08939 -0.01685 -0.01654 -0.02762
F3 4 0.078674 1.326252 0.024347 11.00000 0.06437 0.02890 =
0.05872 -0.00740 -0.00345 -0.00481
F4 4 0.126486 1.524887 0.054149 11.00000 0.05621 0.06297 =
0.05870 -0.01459 -0.01610 -0.02715
HKLF 4
REM kr276p-1 in P-1
REM R1 = 0.0394 for 4944 Fo > 4sig(Fo) and 0.0463 for all 5590 data
REM 325 parameters refined using 0 restraints
END
WGHT 0.0580 0.5442
REM Highest difference peak 0.653, deepest hole -1.202, 1-sigma level 0.110
Q1 1 0.8081 0.9438 0.3010 11.00000 0.05 0.65
Q2 1 0.8161 1.0033 0.1700 11.00000 0.05 0.62
Q3 1 0.9409 0.9206 0.1890 11.00000 0.05 0.49
Q4 1 0.7869 0.8617 0.3068 11.00000 0.05 0.49
Q5 1 0.7642 1.0786 0.2856 11.00000 0.05 0.42
Q6 1 0.7370 0.9009 0.1802 11.00000 0.05 0.41
Q7 1 1.1482 1.0032 0.4365 11.00000 0.05 0.41
Q8 1 0.6079 1.0893 0.3825 11.00000 0.05 0.39
Q9 1 0.7473 0.9625 0.3389 11.00000 0.05 0.37
Q10 1 0.8185 1.1030 0.1667 11.00000 0.05 0.36
Q11 1 0.8831 1.0379 0.2888 11.00000 0.05 0.36
Q12 1 0.5546 1.0821 0.2864 11.00000 0.05 0.35
Q13 1 -0.0753 1.4096 0.1833 11.00000 0.05 0.35
Q14 1 0.0583 1.3233 0.0729 11.00000 0.05 0.34
Q15 1 0.9848 0.9578 0.0961 11.00000 0.05 0.34
Q16 1 1.1929 1.0373 0.4140 11.00000 0.05 0.33
Q17 1 0.6433 0.8769 0.1440 11.00000 0.05 0.33
Q18 1 0.5778 0.9361 0.1053 11.00000 0.05 0.33
Q19 1 1.0000 0.5000 0.5000 10.50000 0.05 0.33
Q20 1 1.1895 0.8473 0.1076 11.00000 0.05 0.32
REM The information below was added by Olex2.
REM
REM R1 = 0.0394 for 4944 Fo > 4sig(Fo) and 0.0463 for all 22529 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.65, deepest hole -1.20
REM Mean Shift 0, Max Shift 0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0463
REM R1_gt = 0.0394
REM wR_ref = 0.1061
REM GOOF = 1.033
REM Shift_max = 0.001
REM Shift_mean = 0
REM Reflections_all = 22529
REM Reflections_gt = 4944
REM Parameters = n/a
REM Hole = -1.20
REM Peak = 0.65
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT430_kr276p-1
;
PROBLEM: Short Inter D...A Contact O1 .. O1 .. 2.42 Ang.
RESPONSE: Structure is hydrogen bridged dimer, with hydrogen bridging the amide oxygen atoms.
;
# end Validation Reply Form
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1472241'
_audit_update_record
;
2016-06-30 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;
_audit_creation_date 2016-06-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C52 H47 Cl2 F4 N4 O2, F6 P'
_chemical_formula_sum 'C52 H47 Cl2 F10 N4 O2 P Ru2'
_chemical_formula_weight 1253.94
_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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
_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.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.42500(10)
_cell_length_b 9.8120(2)
_cell_length_c 14.6230(2)
_cell_angle_alpha 72.4320(10)
_cell_angle_beta 85.7400(10)
_cell_angle_gamma 74.8270(10)
_cell_volume 1244.28(3)
_cell_formula_units_Z 1
_cell_measurement_reflns_used 19746
_cell_measurement_temperature 148(2)
_cell_measurement_theta_max 27.485
_cell_measurement_theta_min 0.998
_shelx_estimated_absorpt_T_max 0.900
_shelx_estimated_absorpt_T_min 0.819
_exptl_absorpt_coefficient_mu 0.830
_exptl_absorpt_correction_T_max 0.8997
_exptl_absorpt_correction_T_min 0.8193
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
Using multiple and symmetry related data measurements via the program SORTAV
See R. H. Blessing, Acta Cryst (1995), A51, 33-38
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour Red
_exptl_crystal_density_diffrn 1.673
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Fragment
_exptl_crystal_F_000 630
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.24
_exptl_crystal_size_min 0.13
_exptl_special_details
;
Detector set at 30 mm from sample with different 2theta offsets
1 degree phi exposures for chi=0 degree settings
1 degree omega exposures for chi=90 degree settings
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0655
_diffrn_reflns_av_unetI/netI 0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 25291
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 27.501
_diffrn_reflns_theta_min 2.239
_diffrn_ambient_temperature 148.15
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer'
_diffrn_measurement_method '\w and \f scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5231
_reflns_number_total 5690
_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 'DENZO-SMN (Otwinowski and Minor, 1997)'
_computing_data_collection 'COLLECT (Nonius, 1999)'
_computing_data_reduction 'DENZO-SMN (Otwinowski and Minor, 1997)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max 0.516
_refine_diff_density_min -1.094
_refine_diff_density_rms 0.136
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.045
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 334
_refine_ls_number_reflns 5690
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0378
_refine_ls_R_factor_gt 0.0316
_refine_ls_restrained_S_all 1.045
_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^)+(0.0398P)^2^+0.7748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0771
_refine_ls_wR_factor_ref 0.0800
_refine_special_details
;
Reflections 0 1 0, 1 0 1, -1 0 1, 0 0 1 omitted as obscured by beamstop.
;
_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. Others
Fixed X: P1(1)
Fixed Y: P1(0)
Fixed Z: P1(0)
3.a Ternary CH refined with riding coordinates:
C24(H24)
3.b Aromatic/amide H refined with riding coordinates:
C4(H4), C2(H2), C16(H16), C21(H21), C7(H7), C3(H3), C8(H8), C18(H18), C5(H5),
C22(H22), C13(H13), C15(H15), C19(H19)
3.c Idealised Me refined as rotating group:
C17(H17A,H17B,H17C), 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
Ru1 Ru 0.81083(2) 0.46925(2) 0.23431(2) 0.01995(7) Uani 1 1 d . . . . .
P1 P 1.0000 0.0000 0.0000 0.02709(17) Uani 1 2 d S T P . .
Cl1 Cl 0.64029(6) 0.61073(6) 0.32171(4) 0.02551(12) Uani 1 1 d . . . . .
F1 F 0.85709(15) 0.01537(15) 0.29340(11) 0.0349(3) Uani 1 1 d . . . . .
N2 N 0.96729(19) 0.43223(19) 0.34330(12) 0.0205(3) Uani 1 1 d . . . . .
F5 F 0.93405(18) 0.17461(16) -0.02352(12) 0.0438(4) Uani 1 1 d . . . . .
F4 F 1.13080(18) 0.01021(18) 0.05900(12) 0.0461(4) Uani 1 1 d . . . . .
F3 F 0.90302(19) -0.02609(18) 0.09514(11) 0.0468(4) Uani 1 1 d . . . . .
N1 N 0.78194(19) 0.28004(19) 0.33810(12) 0.0213(3) Uani 1 1 d . . . . .
O1 O 0.88447(17) 0.08764(16) 0.46755(11) 0.0272(3) Uani 1 1 d . . . . .
C4 C 1.2327(3) 0.7084(3) 0.35629(17) 0.0292(5) Uani 1 1 d . . . . .
H4 H 1.2957 0.7698 0.3562 0.035 Uiso 1 1 calc R . . . .
F2 F 0.36342(19) 0.00650(19) 0.28474(15) 0.0559(5) Uani 1 1 d . . . . .
C2 C 1.0290(2) 0.6693(2) 0.28401(15) 0.0245(4) Uani 1 1 d . . . . .
H2 H 0.9518 0.7047 0.2379 0.029 Uiso 1 1 calc R . . . .
C11 C 0.6736(2) 0.2068(2) 0.32838(15) 0.0235(4) Uani 1 1 d . . . . .
C23 C 0.9694(3) 0.3972(3) 0.12902(15) 0.0281(5) Uani 1 1 d . . . . .
C6 C 1.1624(2) 0.4782(2) 0.42074(15) 0.0231(4) Uani 1 1 d . . . . .
C16 C 0.5257(2) 0.2693(3) 0.33800(17) 0.0293(5) Uani 1 1 d . . . . .
H16 H 0.4960 0.3594 0.3542 0.035 Uiso 1 1 calc R . . . .
C10 C 0.8801(2) 0.2146(2) 0.40614(15) 0.0223(4) Uani 1 1 d . . . . .
C21 C 0.8097(3) 0.6515(2) 0.10102(15) 0.0272(4) Uani 1 1 d . . . . .
H21 H 0.8008 0.7535 0.0917 0.033 Uiso 1 1 calc R . . . .
C7 C 1.1776(2) 0.3394(2) 0.49041(15) 0.0256(4) Uani 1 1 d . . . . .
H7 H 1.2504 0.3062 0.5392 0.031 Uiso 1 1 calc R . . . .
C3 C 1.1183(2) 0.7578(2) 0.28803(16) 0.0267(4) Uani 1 1 d . . . . .
H3 H 1.1027 0.8541 0.2440 0.032 Uiso 1 1 calc R . . . .
C8 C 1.0863(2) 0.2533(2) 0.48684(15) 0.0240(4) Uani 1 1 d . . . . .
H8 H 1.0922 0.1614 0.5346 0.029 Uiso 1 1 calc R . . . .
C1 C 1.0522(2) 0.5253(2) 0.34879(15) 0.0214(4) Uani 1 1 d . . . . .
C24 C 0.5320(3) 0.7093(3) 0.08821(17) 0.0339(5) Uani 1 1 d . . . . .
H24 H 0.5308 0.7764 0.1281 0.041 Uiso 1 1 calc R . . . .
C12 C 0.7134(3) 0.0753(2) 0.30386(16) 0.0280(5) Uani 1 1 d . . . . .
C9 C 0.9840(2) 0.3027(2) 0.41164(14) 0.0212(4) Uani 1 1 d . . . . .
C18 C 0.8416(3) 0.3487(2) 0.12920(15) 0.0287(5) Uani 1 1 d . . . . .
H18 H 0.8504 0.2465 0.1394 0.034 Uiso 1 1 calc R . . . .
C14 C 0.4661(3) 0.0714(3) 0.30000(19) 0.0369(6) Uani 1 1 d . . . . .
C5 C 1.2533(2) 0.5728(2) 0.42247(16) 0.0271(4) Uani 1 1 d . . . . .
H5 H 1.3283 0.5414 0.4698 0.033 Uiso 1 1 calc R . . . .
C22 C 0.9498(2) 0.5518(3) 0.11482(15) 0.0277(5) Uani 1 1 d . . . . .
H22 H 1.0337 0.5883 0.1147 0.033 Uiso 1 1 calc R . . . .
C13 C 0.6120(3) 0.0051(3) 0.28930(19) 0.0360(6) Uani 1 1 d . . . . .
H13 H 0.6412 -0.0846 0.2727 0.043 Uiso 1 1 calc R . . . .
C15 C 0.4202(3) 0.2011(3) 0.32418(18) 0.0353(5) Uani 1 1 d . . . . .
H15 H 0.3186 0.2433 0.3313 0.042 Uiso 1 1 calc R . . . .
C20 C 0.6809(2) 0.6004(3) 0.10090(15) 0.0260(4) Uani 1 1 d . . . . .
C17 C 1.1176(3) 0.2917(3) 0.14946(19) 0.0407(6) Uani 1 1 d . . . . .
H17A H 1.1093 0.2017 0.1996 0.061 Uiso 1 1 calc GR . . . .
H17B H 1.1841 0.3376 0.1712 0.061 Uiso 1 1 calc GR . . . .
H17C H 1.1566 0.2666 0.0910 0.061 Uiso 1 1 calc GR . . . .
C19 C 0.6992(3) 0.4484(3) 0.11448(15) 0.0277(5) Uani 1 1 d . . . . .
H19 H 0.6155 0.4118 0.1138 0.033 Uiso 1 1 calc R . . . .
C25 C 0.4043(3) 0.6374(3) 0.1205(2) 0.0451(7) Uani 1 1 d . . . . .
H25A H 0.3975 0.5775 0.0789 0.068 Uiso 1 1 calc GR . . . .
H25B H 0.3124 0.7143 0.1164 0.068 Uiso 1 1 calc GR . . . .
H25C H 0.4208 0.5743 0.1870 0.068 Uiso 1 1 calc GR . . . .
C26 C 0.5131(3) 0.8044(3) -0.01726(19) 0.0422(6) Uani 1 1 d . . . . .
H26A H 0.5928 0.8545 -0.0351 0.063 Uiso 1 1 calc GR . . . .
H26B H 0.4184 0.8782 -0.0255 0.063 Uiso 1 1 calc GR . . . .
H26C H 0.5160 0.7412 -0.0583 0.063 Uiso 1 1 calc GR . . . .
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 0.02047(10) 0.01871(10) 0.02030(10) -0.00479(7) -0.00192(6) -0.00482(7)
P1 0.0322(4) 0.0227(4) 0.0254(4) -0.0039(3) -0.0025(3) -0.0083(3)
Cl1 0.0255(2) 0.0239(3) 0.0270(2) -0.0100(2) -0.00130(19) -0.0028(2)
F1 0.0314(7) 0.0296(7) 0.0431(8) -0.0158(6) -0.0035(6) 0.0005(6)
N2 0.0210(8) 0.0196(8) 0.0213(8) -0.0054(7) -0.0008(6) -0.0060(7)
F5 0.0501(9) 0.0235(7) 0.0543(9) -0.0073(6) -0.0044(7) -0.0069(6)
F4 0.0489(9) 0.0450(9) 0.0468(9) -0.0073(7) -0.0166(7) -0.0183(7)
F3 0.0553(10) 0.0490(9) 0.0359(8) -0.0102(7) 0.0130(7) -0.0187(8)
N1 0.0224(8) 0.0186(8) 0.0243(8) -0.0062(7) -0.0024(7) -0.0066(7)
O1 0.0295(8) 0.0206(7) 0.0295(8) -0.0008(6) -0.0045(6) -0.0095(6)
C4 0.0278(11) 0.0285(11) 0.0358(12) -0.0107(9) 0.0011(9) -0.0137(9)
F2 0.0478(10) 0.0413(9) 0.0847(13) -0.0093(8) -0.0225(9) -0.0263(8)
C2 0.0253(10) 0.0237(10) 0.0244(10) -0.0061(8) -0.0001(8) -0.0069(8)
C11 0.0249(10) 0.0220(10) 0.0239(10) -0.0039(8) -0.0033(8) -0.0086(8)
C23 0.0285(11) 0.0349(12) 0.0187(10) -0.0087(9) 0.0010(8) -0.0034(9)
C6 0.0225(10) 0.0216(10) 0.0257(10) -0.0078(8) 0.0002(8) -0.0054(8)
C16 0.0275(11) 0.0290(12) 0.0329(11) -0.0105(9) -0.0009(9) -0.0078(9)
C10 0.0219(10) 0.0197(10) 0.0251(10) -0.0066(8) 0.0001(8) -0.0050(8)
C21 0.0317(11) 0.0239(11) 0.0220(10) -0.0018(8) -0.0018(8) -0.0054(9)
C7 0.0259(10) 0.0253(11) 0.0248(10) -0.0060(8) -0.0047(8) -0.0053(8)
C3 0.0296(11) 0.0205(10) 0.0293(11) -0.0050(8) 0.0020(9) -0.0084(9)
C8 0.0261(10) 0.0201(10) 0.0247(10) -0.0041(8) -0.0032(8) -0.0055(8)
C1 0.0215(9) 0.0210(10) 0.0224(10) -0.0070(8) 0.0010(7) -0.0059(8)
C24 0.0307(12) 0.0364(13) 0.0287(12) -0.0084(10) -0.0064(9) 0.0021(10)
C12 0.0289(11) 0.0241(11) 0.0301(11) -0.0076(9) -0.0039(9) -0.0045(9)
C9 0.0213(9) 0.0193(10) 0.0224(10) -0.0053(8) -0.0001(7) -0.0048(8)
C18 0.0397(12) 0.0249(11) 0.0221(10) -0.0097(8) -0.0008(9) -0.0057(9)
C14 0.0371(13) 0.0319(13) 0.0456(14) -0.0046(11) -0.0111(11) -0.0203(11)
C5 0.0236(10) 0.0285(11) 0.0318(11) -0.0097(9) -0.0023(8) -0.0090(9)
C22 0.0284(11) 0.0341(12) 0.0193(10) -0.0027(8) 0.0005(8) -0.0116(9)
C13 0.0448(14) 0.0216(11) 0.0439(14) -0.0082(10) -0.0141(11) -0.0102(10)
C15 0.0257(11) 0.0406(14) 0.0403(13) -0.0086(11) -0.0012(10) -0.0132(10)
C20 0.0268(11) 0.0308(11) 0.0179(9) -0.0047(8) -0.0061(8) -0.0042(9)
C17 0.0348(13) 0.0454(15) 0.0318(13) -0.0107(11) -0.0013(10) 0.0067(11)
C19 0.0300(11) 0.0337(12) 0.0235(10) -0.0103(9) -0.0021(8) -0.0122(9)
C25 0.0282(12) 0.0612(18) 0.0368(14) -0.0067(12) -0.0030(10) -0.0039(12)
C26 0.0359(13) 0.0428(15) 0.0354(13) -0.0016(11) -0.0104(11) 0.0029(11)
_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 Cl1 2.3963(5) . ?
Ru1 N2 2.1368(17) . ?
Ru1 N1 2.0800(17) . ?
Ru1 C23 2.206(2) . ?
Ru1 C21 2.211(2) . ?
Ru1 C18 2.168(2) . ?
Ru1 C22 2.187(2) . ?
Ru1 C20 2.231(2) . ?
Ru1 C19 2.196(2) . ?
P1 F5 1.5996(14) . ?
P1 F5 1.5996(14) 2_755 ?
P1 F4 1.5965(15) 2_755 ?
P1 F4 1.5966(15) . ?
P1 F3 1.5984(15) . ?
P1 F3 1.5984(15) 2_755 ?
F1 C12 1.345(3) . ?
N2 C1 1.384(3) . ?
N2 C9 1.338(3) . ?
N1 C11 1.431(3) . ?
N1 C10 1.304(3) . ?
O1 C10 1.290(2) . ?
C4 H4 0.9500 . ?
C4 C3 1.410(3) . ?
C4 C5 1.364(3) . ?
F2 C14 1.353(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.374(3) . ?
C2 C1 1.416(3) . ?
C11 C16 1.383(3) . ?
C11 C12 1.393(3) . ?
C23 C18 1.405(3) . ?
C23 C22 1.431(3) . ?
C23 C17 1.494(3) . ?
C6 C7 1.412(3) . ?
C6 C1 1.420(3) . ?
C6 C5 1.425(3) . ?
C16 H16 0.9500 . ?
C16 C15 1.392(3) . ?
C10 C9 1.486(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.409(3) . ?
C21 C20 1.430(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.368(3) . ?
C3 H3 0.9500 . ?
C8 H8 0.9500 . ?
C8 C9 1.402(3) . ?
C24 H24 1.0000 . ?
C24 C20 1.510(3) . ?
C24 C25 1.527(4) . ?
C24 C26 1.538(3) . ?
C12 C13 1.377(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.426(3) . ?
C14 C13 1.378(4) . ?
C14 C15 1.376(4) . ?
C5 H5 0.9500 . ?
C22 H22 0.9500 . ?
C13 H13 0.9500 . ?
C15 H15 0.9500 . ?
C20 C19 1.410(3) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C19 H19 0.9500 . ?
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
N2 Ru1 Cl1 86.32(5) . . ?
N2 Ru1 C23 96.97(7) . . ?
N2 Ru1 C21 118.04(8) . . ?
N2 Ru1 C18 124.32(8) . . ?
N2 Ru1 C22 95.09(7) . . ?
N2 Ru1 C20 154.30(8) . . ?
N2 Ru1 C19 162.36(8) . . ?
N1 Ru1 Cl1 87.76(5) . . ?
N1 Ru1 N2 76.00(7) . . ?
N1 Ru1 C23 107.34(8) . . ?
N1 Ru1 C21 165.34(8) . . ?
N1 Ru1 C18 88.59(8) . . ?
N1 Ru1 C22 143.84(8) . . ?
N1 Ru1 C20 129.14(8) . . ?
N1 Ru1 C19 98.33(8) . . ?
C23 Ru1 Cl1 164.90(6) . . ?
C23 Ru1 C21 68.44(8) . . ?
C23 Ru1 C20 81.41(8) . . ?
C21 Ru1 Cl1 96.97(6) . . ?
C21 Ru1 C20 37.57(8) . . ?
C18 Ru1 Cl1 147.07(7) . . ?
C18 Ru1 C23 37.47(9) . . ?
C18 Ru1 C21 79.89(9) . . ?
C18 Ru1 C22 67.37(9) . . ?
C18 Ru1 C20 68.21(8) . . ?
C18 Ru1 C19 38.14(9) . . ?
C22 Ru1 Cl1 127.14(6) . . ?
C22 Ru1 C23 38.03(9) . . ?
C22 Ru1 C21 37.35(8) . . ?
C22 Ru1 C20 67.82(8) . . ?
C22 Ru1 C19 79.57(8) . . ?
C20 Ru1 Cl1 89.23(6) . . ?
C19 Ru1 Cl1 110.38(6) . . ?
C19 Ru1 C23 68.44(8) . . ?
C19 Ru1 C21 67.01(8) . . ?
C19 Ru1 C20 37.12(8) . . ?
F5 P1 F5 180.0 2_755 . ?
F4 P1 F5 89.78(8) 2_755 2_755 ?
F4 P1 F5 90.22(8) 2_755 . ?
F4 P1 F5 90.22(8) . 2_755 ?
F4 P1 F5 89.78(8) . . ?
F4 P1 F4 180.0 2_755 . ?
F4 P1 F3 90.33(9) 2_755 2_755 ?
F4 P1 F3 89.67(9) . 2_755 ?
F4 P1 F3 89.67(9) 2_755 . ?
F4 P1 F3 90.33(9) . . ?
F3 P1 F5 89.73(8) 2_755 . ?
F3 P1 F5 90.27(8) . . ?
F3 P1 F5 90.27(8) 2_755 2_755 ?
F3 P1 F5 89.73(8) . 2_755 ?
F3 P1 F3 180.00(7) 2_755 . ?
C1 N2 Ru1 127.16(13) . . ?
C9 N2 Ru1 114.56(13) . . ?
C9 N2 C1 118.27(17) . . ?
C11 N1 Ru1 122.12(13) . . ?
C10 N1 Ru1 118.14(14) . . ?
C10 N1 C11 118.90(17) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C5 C4 C3 120.3(2) . . ?
C3 C2 H2 120.1 . . ?
C3 C2 C1 119.8(2) . . ?
C1 C2 H2 120.1 . . ?
C16 C11 N1 120.63(19) . . ?
C16 C11 C12 118.3(2) . . ?
C12 C11 N1 120.96(19) . . ?
C18 C23 Ru1 69.79(13) . . ?
C18 C23 C22 116.8(2) . . ?
C18 C23 C17 121.8(2) . . ?
C22 C23 Ru1 70.29(12) . . ?
C22 C23 C17 121.3(2) . . ?
C17 C23 Ru1 127.08(16) . . ?
C7 C6 C1 119.18(19) . . ?
C7 C6 C5 121.3(2) . . ?
C1 C6 C5 119.49(19) . . ?
C11 C16 H16 119.8 . . ?
C11 C16 C15 120.5(2) . . ?
C15 C16 H16 119.8 . . ?
N1 C10 C9 114.32(18) . . ?
O1 C10 N1 123.96(19) . . ?
O1 C10 C9 121.63(18) . . ?
Ru1 C21 H21 130.5 . . ?
C22 C21 Ru1 70.43(12) . . ?
C22 C21 H21 119.7 . . ?
C22 C21 C20 120.5(2) . . ?
C20 C21 Ru1 71.98(12) . . ?
C20 C21 H21 119.7 . . ?
C6 C7 H7 120.4 . . ?
C8 C7 C6 119.3(2) . . ?
C8 C7 H7 120.4 . . ?
C4 C3 H3 119.4 . . ?
C2 C3 C4 121.2(2) . . ?
C2 C3 H3 119.4 . . ?
C7 C8 H8 120.5 . . ?
C7 C8 C9 118.94(19) . . ?
C9 C8 H8 120.5 . . ?
N2 C1 C2 120.63(19) . . ?
N2 C1 C6 120.32(18) . . ?
C2 C1 C6 119.04(19) . . ?
C20 C24 H24 107.6 . . ?
C20 C24 C25 113.8(2) . . ?
C20 C24 C26 109.0(2) . . ?
C25 C24 H24 107.6 . . ?
C25 C24 C26 111.0(2) . . ?
C26 C24 H24 107.6 . . ?
F1 C12 C11 118.36(19) . . ?
F1 C12 C13 118.9(2) . . ?
C13 C12 C11 122.8(2) . . ?
N2 C9 C10 115.32(18) . . ?
N2 C9 C8 123.77(19) . . ?
C8 C9 C10 120.84(18) . . ?
Ru1 C18 H18 128.6 . . ?
C23 C18 Ru1 72.74(13) . . ?
C23 C18 H18 119.0 . . ?
C23 C18 C19 121.9(2) . . ?
C19 C18 Ru1 72.02(12) . . ?
C19 C18 H18 119.0 . . ?
F2 C14 C13 118.3(2) . . ?
F2 C14 C15 118.7(2) . . ?
C15 C14 C13 123.0(2) . . ?
C4 C5 C6 120.0(2) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
Ru1 C22 H22 129.7 . . ?
C23 C22 Ru1 71.68(12) . . ?
C23 C22 H22 119.0 . . ?
C21 C22 Ru1 72.22(13) . . ?
C21 C22 C23 122.0(2) . . ?
C21 C22 H22 119.0 . . ?
C12 C13 C14 116.8(2) . . ?
C12 C13 H13 121.6 . . ?
C14 C13 H13 121.6 . . ?
C16 C15 H15 120.7 . . ?
C14 C15 C16 118.6(2) . . ?
C14 C15 H15 120.7 . . ?
C21 C20 Ru1 70.45(12) . . ?
C21 C20 C24 119.3(2) . . ?
C24 C20 Ru1 129.88(15) . . ?
C19 C20 Ru1 70.10(12) . . ?
C19 C20 C21 117.9(2) . . ?
C19 C20 C24 122.8(2) . . ?
C23 C17 H17A 109.5 . . ?
C23 C17 H17B 109.5 . . ?
C23 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Ru1 C19 H19 130.5 . . ?
C18 C19 Ru1 69.84(12) . . ?
C18 C19 H19 119.5 . . ?
C20 C19 Ru1 72.77(12) . . ?
C20 C19 C18 120.9(2) . . ?
C20 C19 H19 119.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 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
Ru1 N2 C1 C2 7.6(3) . . . . ?
Ru1 N2 C1 C6 -173.53(15) . . . . ?
Ru1 N2 C9 C10 -6.4(2) . . . . ?
Ru1 N2 C9 C8 176.55(16) . . . . ?
Ru1 N1 C11 C16 -72.0(2) . . . . ?
Ru1 N1 C11 C12 104.5(2) . . . . ?
Ru1 N1 C10 O1 -171.25(16) . . . . ?
Ru1 N1 C10 C9 12.2(2) . . . . ?
Ru1 C23 C18 C19 54.93(19) . . . . ?
Ru1 C23 C22 C21 -54.12(19) . . . . ?
Ru1 C21 C22 C23 53.87(18) . . . . ?
Ru1 C21 C20 C24 125.52(19) . . . . ?
Ru1 C21 C20 C19 -53.39(17) . . . . ?
Ru1 C18 C19 C20 54.03(18) . . . . ?
Ru1 C20 C19 C18 -52.69(18) . . . . ?
F1 C12 C13 C14 -179.4(2) . . . . ?
N1 C11 C16 C15 177.0(2) . . . . ?
N1 C11 C12 F1 2.7(3) . . . . ?
N1 C11 C12 C13 -176.8(2) . . . . ?
N1 C10 C9 N2 -3.5(3) . . . . ?
N1 C10 C9 C8 173.64(19) . . . . ?
O1 C10 C9 N2 179.93(19) . . . . ?
O1 C10 C9 C8 -3.0(3) . . . . ?
F2 C14 C13 C12 179.0(2) . . . . ?
F2 C14 C15 C16 -178.8(2) . . . . ?
C11 N1 C10 O1 -1.5(3) . . . . ?
C11 N1 C10 C9 -178.05(18) . . . . ?
C11 C16 C15 C14 -0.6(4) . . . . ?
C11 C12 C13 C14 0.1(4) . . . . ?
C23 C18 C19 Ru1 -55.26(19) . . . . ?
C23 C18 C19 C20 -1.2(3) . . . . ?
C6 C7 C8 C9 2.6(3) . . . . ?
C16 C11 C12 F1 179.2(2) . . . . ?
C16 C11 C12 C13 -0.3(3) . . . . ?
C10 N1 C11 C16 118.7(2) . . . . ?
C10 N1 C11 C12 -64.8(3) . . . . ?
C21 C20 C19 Ru1 53.55(17) . . . . ?
C21 C20 C19 C18 0.9(3) . . . . ?
C7 C6 C1 N2 -4.2(3) . . . . ?
C7 C6 C1 C2 174.7(2) . . . . ?
C7 C6 C5 C4 -177.7(2) . . . . ?
C7 C8 C9 N2 -1.6(3) . . . . ?
C7 C8 C9 C10 -178.5(2) . . . . ?
C3 C4 C5 C6 2.3(3) . . . . ?
C3 C2 C1 N2 -177.3(2) . . . . ?
C3 C2 C1 C6 3.8(3) . . . . ?
C1 N2 C9 C10 174.72(17) . . . . ?
C1 N2 C9 C8 -2.3(3) . . . . ?
C1 C2 C3 C4 -0.6(3) . . . . ?
C1 C6 C7 C8 0.2(3) . . . . ?
C1 C6 C5 C4 1.0(3) . . . . ?
C24 C20 C19 Ru1 -125.3(2) . . . . ?
C24 C20 C19 C18 -178.0(2) . . . . ?
C12 C11 C16 C15 0.5(3) . . . . ?
C9 N2 C1 C2 -173.75(19) . . . . ?
C9 N2 C1 C6 5.1(3) . . . . ?
C18 C23 C22 Ru1 53.72(17) . . . . ?
C18 C23 C22 C21 -0.4(3) . . . . ?
C5 C4 C3 C2 -2.5(4) . . . . ?
C5 C6 C7 C8 178.9(2) . . . . ?
C5 C6 C1 N2 177.08(19) . . . . ?
C5 C6 C1 C2 -4.0(3) . . . . ?
C22 C23 C18 Ru1 -53.97(17) . . . . ?
C22 C23 C18 C19 1.0(3) . . . . ?
C22 C21 C20 Ru1 53.08(18) . . . . ?
C22 C21 C20 C24 178.6(2) . . . . ?
C22 C21 C20 C19 -0.3(3) . . . . ?
C13 C14 C15 C16 0.4(4) . . . . ?
C15 C14 C13 C12 -0.1(4) . . . . ?
C20 C21 C22 Ru1 -53.79(19) . . . . ?
C20 C21 C22 C23 0.1(3) . . . . ?
C17 C23 C18 Ru1 121.9(2) . . . . ?
C17 C23 C18 C19 176.8(2) . . . . ?
C17 C23 C22 Ru1 -122.1(2) . . . . ?
C17 C23 C22 C21 -176.2(2) . . . . ?
C25 C24 C20 Ru1 -73.4(3) . . . . ?
C25 C24 C20 C21 -161.6(2) . . . . ?
C25 C24 C20 C19 17.3(3) . . . . ?
C26 C24 C20 Ru1 162.25(18) . . . . ?
C26 C24 C20 C21 74.0(3) . . . . ?
C26 C24 C20 C19 -107.1(3) . . . . ?
_shelx_SHELXL_version_number 2014/7
_iucr_refine_instructions_details
;
shelxl.res created by SHELXL-2014/7
TITL Compound X
REM Compound X
REM 146 parameters refined using 0 restraints
REM Highest difference peak 2.061, deepest hole -2.084, 1-sigma level 0.294
REM 149 parameters refined using 0 restraints
REM Highest difference peak 1.555, deepest hole -1.826, 1-sigma level 0.170
CELL 0.71073 9.425 9.812 14.623 72.432 85.74 74.827
ZERR 1 0.0001 0.0002 0.0002 0.001 0.001 0.001
LATT 1
SFAC C H Cl F N O P Ru
UNIT 52 47 2 10 4 2 1 2
L.S. 10
PLAN 20
SIZE 0.25 0.24 0.13
TEMP -125
GRID
BOND $H
MORE -1
CONF
fmap
acta 52
MERG 2
OMIT -3 180
OMIT 0 1 0
OMIT 1 0 1
OMIT -1 0 1
OMIT 0 0 1
REM
REM
REM
WGHT 0.039800 0.774800
FVAR 0.42690
RU1 8 0.810835 0.469247 0.234309 11.00000 0.02047 0.01871 =
0.02030 -0.00479 -0.00192 -0.00482
P1 7 11.000000 10.000000 10.000000 10.50000 0.03224 0.02270 =
0.02543 -0.00390 -0.00246 -0.00834
CL1 3 0.640287 0.610725 0.321712 11.00000 0.02549 0.02394 =
0.02703 -0.00996 -0.00130 -0.00281
F1 4 0.857087 0.015368 0.293399 11.00000 0.03139 0.02962 =
0.04311 -0.01576 -0.00347 0.00052
N2 5 0.967291 0.432234 0.343302 11.00000 0.02097 0.01964 =
0.02126 -0.00544 -0.00080 -0.00601
F5 4 0.934049 0.174615 -0.023517 11.00000 0.05014 0.02349 =
0.05432 -0.00726 -0.00441 -0.00688
F4 4 1.130800 0.010215 0.058998 11.00000 0.04886 0.04502 =
0.04682 -0.00727 -0.01665 -0.01827
F3 4 0.903019 -0.026088 0.095137 11.00000 0.05526 0.04903 =
0.03587 -0.01025 0.01302 -0.01874
N1 5 0.781941 0.280041 0.338096 11.00000 0.02237 0.01860 =
0.02425 -0.00623 -0.00237 -0.00657
O1 6 0.884472 0.087641 0.467548 11.00000 0.02950 0.02059 =
0.02955 -0.00076 -0.00449 -0.00946
C4 1 1.232696 0.708399 0.356286 11.00000 0.02777 0.02852 =
0.03576 -0.01066 0.00107 -0.01365
AFIX 43
H4 2 1.295712 0.769814 0.356175 11.00000 -1.20000
AFIX 0
F2 4 0.363421 0.006505 0.284745 11.00000 0.04784 0.04133 =
0.08473 -0.00932 -0.02245 -0.02627
C2 1 1.028951 0.669347 0.284013 11.00000 0.02532 0.02367 =
0.02438 -0.00615 -0.00014 -0.00686
AFIX 43
H2 2 0.951824 0.704721 0.237930 11.00000 -1.20000
AFIX 0
C11 1 0.673579 0.206808 0.328381 11.00000 0.02486 0.02197 =
0.02387 -0.00386 -0.00326 -0.00858
C23 1 0.969359 0.397162 0.129022 11.00000 0.02847 0.03487 =
0.01866 -0.00867 0.00101 -0.00337
C6 1 1.162384 0.478161 0.420741 11.00000 0.02248 0.02162 =
0.02572 -0.00783 0.00019 -0.00538
C16 1 0.525734 0.269270 0.338002 11.00000 0.02746 0.02903 =
0.03293 -0.01051 -0.00088 -0.00779
AFIX 43
H16 2 0.495998 0.359365 0.354167 11.00000 -1.20000
AFIX 0
C10 1 0.880150 0.214599 0.406143 11.00000 0.02195 0.01971 =
0.02507 -0.00655 0.00012 -0.00502
C21 1 0.809742 0.651531 0.101017 11.00000 0.03173 0.02390 =
0.02197 -0.00182 -0.00180 -0.00544
AFIX 43
H21 2 0.800817 0.753521 0.091716 11.00000 -1.20000
AFIX 0
C7 1 1.177584 0.339402 0.490407 11.00000 0.02590 0.02535 =
0.02482 -0.00600 -0.00471 -0.00526
AFIX 43
H7 2 1.250422 0.306240 0.539230 11.00000 -1.20000
AFIX 0
C3 1 1.118299 0.757830 0.288028 11.00000 0.02964 0.02045 =
0.02930 -0.00500 0.00197 -0.00836
AFIX 43
H3 2 1.102720 0.854093 0.244004 11.00000 -1.20000
AFIX 0
C8 1 1.086332 0.253271 0.486842 11.00000 0.02607 0.02008 =
0.02466 -0.00411 -0.00321 -0.00554
AFIX 43
H8 2 1.092186 0.161409 0.534569 11.00000 -1.20000
AFIX 0
C1 1 1.052209 0.525261 0.348790 11.00000 0.02153 0.02101 =
0.02241 -0.00704 0.00101 -0.00585
C24 1 0.532029 0.709344 0.088209 11.00000 0.03070 0.03641 =
0.02869 -0.00840 -0.00644 0.00215
AFIX 13
H24 2 0.530779 0.776390 0.128110 11.00000 -1.20000
AFIX 0
C12 1 0.713421 0.075311 0.303855 11.00000 0.02893 0.02413 =
0.03013 -0.00761 -0.00390 -0.00454
C9 1 0.984023 0.302693 0.411641 11.00000 0.02127 0.01926 =
0.02239 -0.00530 -0.00012 -0.00476
C18 1 0.841621 0.348669 0.129196 11.00000 0.03972 0.02492 =
0.02211 -0.00970 -0.00078 -0.00574
AFIX 43
H18 2 0.850403 0.246478 0.139418 11.00000 -1.20000
AFIX 0
C14 1 0.466072 0.071390 0.299997 11.00000 0.03715 0.03193 =
0.04559 -0.00464 -0.01114 -0.02033
C5 1 1.253276 0.572795 0.422471 11.00000 0.02358 0.02850 =
0.03176 -0.00972 -0.00229 -0.00902
AFIX 43
H5 2 1.328257 0.541409 0.469757 11.00000 -1.20000
AFIX 0
C22 1 0.949768 0.551817 0.114819 11.00000 0.02843 0.03406 =
0.01931 -0.00273 0.00053 -0.01165
AFIX 43
H22 2 1.033744 0.588319 0.114698 11.00000 -1.20000
AFIX 0
C13 1 0.611997 0.005119 0.289301 11.00000 0.04483 0.02161 =
0.04393 -0.00821 -0.01405 -0.01017
AFIX 43
H13 2 0.641192 -0.084630 0.272693 11.00000 -1.20000
AFIX 0
C15 1 0.420188 0.201107 0.324177 11.00000 0.02571 0.04063 =
0.04032 -0.00865 -0.00121 -0.01324
AFIX 43
H15 2 0.318602 0.243272 0.331288 11.00000 -1.20000
AFIX 0
C20 1 0.680872 0.600430 0.100896 11.00000 0.02677 0.03085 =
0.01790 -0.00465 -0.00614 -0.00421
C17 1 1.117607 0.291693 0.149457 11.00000 0.03480 0.04543 =
0.03181 -0.01072 -0.00131 0.00673
AFIX 137
H17A 2 1.109334 0.201690 0.199611 11.00000 -1.50000
H17B 2 1.184108 0.337579 0.171199 11.00000 -1.50000
H17C 2 1.156646 0.266608 0.090968 11.00000 -1.50000
AFIX 0
C19 1 0.699178 0.448364 0.114478 11.00000 0.03004 0.03370 =
0.02349 -0.01032 -0.00215 -0.01219
AFIX 43
H19 2 0.615487 0.411787 0.113818 11.00000 -1.20000
AFIX 0
C25 1 0.404258 0.637437 0.120533 11.00000 0.02815 0.06125 =
0.03685 -0.00669 -0.00295 -0.00386
AFIX 137
H25A 2 0.397507 0.577538 0.078945 11.00000 -1.50000
H25B 2 0.312450 0.714344 0.116449 11.00000 -1.50000
H25C 2 0.420791 0.574267 0.186957 11.00000 -1.50000
AFIX 0
C26 1 0.513075 0.804438 -0.017258 11.00000 0.03592 0.04277 =
0.03543 -0.00157 -0.01039 0.00288
AFIX 137
H26A 2 0.592800 0.854473 -0.035118 11.00000 -1.50000
H26B 2 0.418387 0.878248 -0.025525 11.00000 -1.50000
H26C 2 0.515962 0.741178 -0.058325 11.00000 -1.50000
AFIX 0
HKLF 4
REM Compound X
REM R1 = 0.0316 for 5231 Fo > 4sig(Fo) and 0.0378 for all 5690 data
REM 334 parameters refined using 0 restraints
END
WGHT 0.0398 0.7748
REM Highest difference peak 0.516, deepest hole -1.094, 1-sigma level 0.136
Q1 1 0.7079 0.4823 0.3071 11.00000 0.05 0.52
Q2 1 0.5147 0.3044 0.3913 11.00000 0.05 0.45
Q3 1 0.6852 0.1657 0.3134 11.00000 0.05 0.44
Q4 1 0.6982 0.5005 0.1594 11.00000 0.05 0.43
Q5 1 0.9600 0.0309 0.4941 11.00000 0.05 0.43
Q6 1 1.4556 0.6038 0.5113 11.00000 0.05 0.41
Q7 1 0.9254 0.4589 0.1590 11.00000 0.05 0.41
Q8 1 0.7301 0.5801 0.2649 11.00000 0.05 0.41
Q9 1 0.5594 0.0653 0.2624 11.00000 0.05 0.40
Q10 1 1.2211 0.5259 0.4137 11.00000 0.05 0.38
Q11 1 0.3849 0.1851 0.4125 11.00000 0.05 0.38
Q12 1 0.5009 0.1995 0.3657 11.00000 0.05 0.38
Q13 1 0.4002 1.0653 -0.0752 11.00000 0.05 0.38
Q14 1 0.4978 0.9728 -0.0617 11.00000 0.05 0.36
Q15 1 0.7974 0.5688 0.1630 11.00000 0.05 0.36
Q16 1 0.6065 0.6589 0.0714 11.00000 0.05 0.35
Q17 1 0.4747 0.2588 0.2825 11.00000 0.05 0.35
Q18 1 0.5065 0.8163 -0.1631 11.00000 0.05 0.35
Q19 1 1.3785 0.5169 0.4205 11.00000 0.05 0.35
Q20 1 0.7937 0.4788 0.1464 11.00000 0.05 0.34
REM The information below was added by Olex2.
REM
REM R1 = 0.0316 for 5231 Fo > 4sig(Fo) and 0.0378 for all 25303 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.52, deepest hole -1.09
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0378
REM R1_gt = 0.0316
REM wR_ref = 0.0800
REM GOOF = 1.045
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 25303
REM Reflections_gt = 5231
REM Parameters = n/a
REM Hole = -1.09
REM Peak = 0.52
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT430_I
;
PROBLEM: Short Inter D...A Contact O1 .. O1 .. 2.44 Ang.
RESPONSE: Structure is hydrogen bridged dimer, with hydrogen bridging the amide oxygen atoms.
;
# end Validation Reply Form
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_kr220_0m
_database_code_depnum_ccdc_archive 'CCDC 1472242'
_audit_update_record
;
2016-06-30 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;
_audit_creation_date 2016-06-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C52 H49 Br2 F2 N4 O2 Ru2, F6 P'
_chemical_formula_sum 'C52 H49 Br2 F8 N4 O2 P Ru2'
_chemical_formula_weight 1306.88
_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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
_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.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_H-M_alt 'C 1 2/c 1'
_space_group_name_Hall '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 31.309(3)
_cell_length_b 10.0915(9)
_cell_length_c 18.4285(16)
_cell_angle_alpha 90
_cell_angle_beta 118.325(4)
_cell_angle_gamma 90
_cell_volume 5125.5(8)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9369
_cell_measurement_temperature 148(2)
_cell_measurement_theta_max 28.808
_cell_measurement_theta_min 2.229
_shelx_estimated_absorpt_T_max 0.956
_shelx_estimated_absorpt_T_min 0.523
_exptl_absorpt_coefficient_mu 2.253
_exptl_absorpt_correction_T_max 0.9563
_exptl_absorpt_correction_T_min 0.5234
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G.M. (2002). SADABS v. 2.03. University of Gottingen, Germany.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.694
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 2600
_exptl_crystal_size_max 0.33
_exptl_crystal_size_mid 0.18
_exptl_crystal_size_min 0.02
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0515
_diffrn_reflns_av_unetI/netI 0.0468
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max 42
_diffrn_reflns_limit_h_min -42
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 33840
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.967
_diffrn_reflns_theta_min 2.149
_diffrn_ambient_temperature 148.15
_diffrn_detector_area_resol_mean '120 microns'
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type 'Bruker X8 Apex diffractometer'
_diffrn_measurement_method 'Rotation images'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'rotating anode'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5289
_reflns_number_total 6751
_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 'APEX 2 software, Bruker Nonius 2004'
_computing_data_collection 'APEX 2 software, Bruker Nonius 2004'
_computing_data_reduction 'SAINT, Bruker Nonius 2004'
_computing_molecular_graphics 'ORTEX (McArdle, 1995)'
_computing_publication_material 'local program'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max 0.680
_refine_diff_density_min -0.614
_refine_diff_density_rms 0.098
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.011
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 325
_refine_ls_number_reflns 6751
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0525
_refine_ls_R_factor_gt 0.0326
_refine_ls_restrained_S_all 1.011
_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^)+(0.0282P)^2^+5.6420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0638
_refine_ls_wR_factor_ref 0.0694
_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:
C24(H24)
2.b Aromatic/amide H refined with riding coordinates:
C8(H8), C7(H7), C2(H2), C3(H3), C5(H5), C4(H4), C12(H12), C13(H13), C15(H15),
C14(H14), C20(H20), C22(H22), C19(H19), C23(H23)
2.c Idealised Me refined as rotating group:
C17(H17A,H17B,H17C), 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
Ru1 Ru 0.12873(2) 0.72303(2) 0.48563(2) 0.01456(6) Uani 1 1 d . . . . .
Br1 Br 0.07579(2) 0.57707(3) 0.36297(2) 0.02211(7) Uani 1 1 d . . . . .
O1 O 0.00882(6) 0.95487(18) 0.44738(11) 0.0229(4) Uani 1 1 d . . . . .
N1 N 0.07300(7) 0.86163(19) 0.43696(12) 0.0156(4) Uani 1 1 d . . . . .
C11 C 0.07261(9) 0.9672(2) 0.38422(15) 0.0174(5) Uani 1 1 d . . . . .
C10 C 0.04192(9) 0.8646(2) 0.46602(15) 0.0163(5) Uani 1 1 d . . . . .
N2 N 0.08095(7) 0.6618(2) 0.53199(12) 0.0157(4) Uani 1 1 d . . . . .
C6 C 0.05069(9) 0.5227(3) 0.60694(15) 0.0201(5) Uani 1 1 d . . . . .
C8 C 0.01214(9) 0.7319(3) 0.55055(16) 0.0198(5) Uani 1 1 d . . . . .
H8 H -0.0123 0.7963 0.5401 0.024 Uiso 1 1 calc R . . . .
C1 C 0.08273(9) 0.5440(2) 0.57224(15) 0.0171(5) Uani 1 1 d . . . . .
C7 C 0.01573(9) 0.6208(3) 0.59577(16) 0.0222(6) Uani 1 1 d . . . . .
H7 H -0.0051 0.6095 0.6195 0.027 Uiso 1 1 calc R . . . .
C9 C 0.04551(9) 0.7494(2) 0.51948(15) 0.0165(5) Uani 1 1 d . . . . .
C2 C 0.11513(10) 0.4414(2) 0.57756(16) 0.0221(6) Uani 1 1 d . . . . .
H2 H 0.1353 0.4524 0.5524 0.027 Uiso 1 1 calc R . . . .
C3 C 0.11737(10) 0.3261(3) 0.61906(16) 0.0248(6) Uani 1 1 d . . . . .
H3 H 0.1396 0.2585 0.6232 0.030 Uiso 1 1 calc R . . . .
C5 C 0.05415(10) 0.4015(3) 0.64946(16) 0.0254(6) Uani 1 1 d . . . . .
H5 H 0.0336 0.3867 0.6735 0.030 Uiso 1 1 calc R . . . .
C4 C 0.08700(11) 0.3068(3) 0.65570(17) 0.0278(6) Uani 1 1 d . . . . .
H4 H 0.0895 0.2272 0.6849 0.033 Uiso 1 1 calc R . . . .
C12 C 0.06117(9) 0.9440(3) 0.30273(16) 0.0219(6) Uani 1 1 d . . . . .
H12 H 0.0522 0.8576 0.2801 0.026 Uiso 1 1 calc R . . . .
C16 C 0.08610(10) 1.0951(3) 0.41496(16) 0.0224(6) Uani 1 1 d . . . . .
C13 C 0.06288(10) 1.0475(3) 0.25399(18) 0.0314(7) Uani 1 1 d . . . . .
H13 H 0.0547 1.0313 0.1981 0.038 Uiso 1 1 calc R . . . .
C15 C 0.08839(11) 1.1993(3) 0.36846(19) 0.0312(7) Uani 1 1 d . . . . .
H15 H 0.0978 1.2853 0.3915 0.037 Uiso 1 1 calc R . . . .
C14 C 0.07643(11) 1.1745(3) 0.28655(19) 0.0355(7) Uani 1 1 d . . . . .
H14 H 0.0775 1.2443 0.2529 0.043 Uiso 1 1 calc R . . . .
C21 C 0.19018(9) 0.7802(3) 0.60620(16) 0.0239(6) Uani 1 1 d . . . . .
C20 C 0.18255(9) 0.8791(3) 0.54763(18) 0.0269(6) Uani 1 1 d . . . . .
H20 H 0.1776 0.9681 0.5588 0.032 Uiso 1 1 calc R . . . .
C22 C 0.19808(9) 0.6479(3) 0.58651(17) 0.0272(6) Uani 1 1 d . . . . .
H22 H 0.2045 0.5793 0.6257 0.033 Uiso 1 1 calc R . . . .
C18 C 0.18830(10) 0.7177(3) 0.45184(18) 0.0310(7) Uani 1 1 d . . . . .
C19 C 0.18205(9) 0.8479(3) 0.47108(18) 0.0309(7) Uani 1 1 d . . . . .
H19 H 0.1774 0.9168 0.4329 0.037 Uiso 1 1 calc R . . . .
C23 C 0.19658(9) 0.6169(3) 0.51108(19) 0.0302(7) Uani 1 1 d . . . . .
H23 H 0.2011 0.5279 0.4995 0.036 Uiso 1 1 calc R . . . .
C17 C 0.18453(12) 0.6819(4) 0.3688(2) 0.0541(11) Uani 1 1 d . . . . .
H17A H 0.1741 0.7598 0.3327 0.081 Uiso 1 1 calc GR . . . .
H17B H 0.1608 0.6105 0.3434 0.081 Uiso 1 1 calc GR . . . .
H17C H 0.2163 0.6523 0.3767 0.081 Uiso 1 1 calc GR . . . .
C24 C 0.19103(11) 0.8073(4) 0.68825(19) 0.0405(8) Uani 1 1 d . . . . .
H24 H 0.1758 0.7297 0.7009 0.049 Uiso 1 1 calc R . . . .
F1 F 0.09821(6) 1.11651(15) 0.49593(10) 0.0325(4) Uani 1 1 d . . . . .
C25 C 0.24485(13) 0.8146(5) 0.7559(2) 0.0644(12) Uani 1 1 d . . . . .
H25A H 0.2611 0.7307 0.7576 0.097 Uiso 1 1 calc GR . . . .
H25B H 0.2464 0.8305 0.8096 0.097 Uiso 1 1 calc GR . . . .
H25C H 0.2611 0.8872 0.7434 0.097 Uiso 1 1 calc GR . . . .
C26 C 0.16323(14) 0.9318(5) 0.6888(2) 0.0698(13) Uani 1 1 d . . . . .
H26A H 0.1806 1.0106 0.6858 0.105 Uiso 1 1 calc GR . . . .
H26B H 0.1606 0.9343 0.7397 0.105 Uiso 1 1 calc GR . . . .
H26C H 0.1307 0.9301 0.6412 0.105 Uiso 1 1 calc GR . . . .
P1 P 0.2500 0.2500 0.5000 0.0416(3) Uani 1 2 d S T P . .
F4 F 0.20449(8) 0.2805(2) 0.51571(16) 0.0693(7) Uani 1 1 d . . . . .
F2 F 0.23098(10) 0.3584(2) 0.42899(15) 0.0784(8) Uani 1 1 d . . . . .
F3 F 0.22004(8) 0.1377(2) 0.43369(15) 0.0696(7) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.01282(10) 0.01547(10) 0.01687(10) 0.00085(8) 0.00825(8) 0.00234(8)
Br1 0.02505(15) 0.02101(13) 0.02168(14) -0.00371(10) 0.01223(12) -0.00341(11)
O1 0.0229(10) 0.0260(10) 0.0243(10) 0.0053(8) 0.0148(9) 0.0104(8)
N1 0.0154(11) 0.0142(10) 0.0171(11) 0.0013(8) 0.0076(9) 0.0019(8)
C11 0.0149(13) 0.0198(13) 0.0205(13) 0.0051(10) 0.0109(11) 0.0049(10)
C10 0.0144(12) 0.0188(12) 0.0158(13) -0.0008(10) 0.0072(10) 0.0017(10)
N2 0.0147(10) 0.0172(10) 0.0144(10) -0.0007(8) 0.0062(9) -0.0007(8)
C6 0.0205(14) 0.0228(13) 0.0136(13) -0.0025(10) 0.0054(11) -0.0056(11)
C8 0.0177(13) 0.0238(13) 0.0203(13) -0.0026(11) 0.0110(11) -0.0004(11)
C1 0.0162(13) 0.0182(13) 0.0131(12) -0.0012(9) 0.0040(10) -0.0031(10)
C7 0.0240(14) 0.0263(14) 0.0222(14) -0.0030(11) 0.0157(12) -0.0065(11)
C9 0.0165(13) 0.0184(13) 0.0147(12) -0.0001(9) 0.0074(10) 0.0011(9)
C2 0.0239(14) 0.0195(13) 0.0211(14) 0.0004(11) 0.0092(12) -0.0001(11)
C3 0.0260(15) 0.0186(13) 0.0207(14) 0.0014(11) 0.0039(12) 0.0014(11)
C5 0.0303(16) 0.0276(15) 0.0171(14) 0.0012(11) 0.0104(12) -0.0079(12)
C4 0.0352(17) 0.0211(14) 0.0197(14) 0.0057(11) 0.0070(13) -0.0061(12)
C12 0.0189(14) 0.0261(14) 0.0206(14) 0.0011(11) 0.0093(12) 0.0003(11)
C16 0.0249(14) 0.0195(13) 0.0241(15) 0.0023(11) 0.0127(12) 0.0045(11)
C13 0.0287(16) 0.0433(19) 0.0227(15) 0.0075(13) 0.0125(13) 0.0007(13)
C15 0.0311(17) 0.0218(15) 0.0376(18) 0.0052(12) 0.0138(14) 0.0003(12)
C14 0.0352(18) 0.0328(17) 0.0374(18) 0.0165(14) 0.0163(15) 0.0007(14)
C21 0.0155(13) 0.0338(15) 0.0217(14) -0.0067(12) 0.0083(11) -0.0052(12)
C20 0.0147(13) 0.0220(14) 0.0415(18) -0.0057(12) 0.0115(13) -0.0048(11)
C22 0.0168(14) 0.0265(15) 0.0283(16) 0.0083(12) 0.0026(12) 0.0043(11)
C18 0.0130(13) 0.057(2) 0.0271(16) -0.0057(14) 0.0126(12) -0.0015(13)
C19 0.0127(13) 0.0429(18) 0.0343(17) 0.0133(14) 0.0090(13) -0.0038(12)
C23 0.0151(14) 0.0310(16) 0.0392(18) -0.0095(13) 0.0085(13) 0.0058(12)
C17 0.0264(18) 0.109(3) 0.0330(19) -0.016(2) 0.0192(16) -0.0082(19)
C24 0.0286(17) 0.066(2) 0.0252(17) -0.0119(15) 0.0117(14) -0.0087(16)
F1 0.0452(11) 0.0257(9) 0.0269(9) -0.0059(7) 0.0172(8) 0.0001(8)
C25 0.039(2) 0.126(4) 0.0233(18) -0.019(2) 0.0108(16) -0.007(2)
C26 0.049(2) 0.110(4) 0.055(3) -0.039(2) 0.029(2) 0.003(2)
P1 0.0374(7) 0.0274(6) 0.0555(8) -0.0002(5) 0.0184(6) 0.0051(5)
F4 0.0526(14) 0.0680(15) 0.0957(19) -0.0079(13) 0.0420(14) 0.0053(12)
F2 0.110(2) 0.0499(14) 0.0756(18) 0.0176(12) 0.0445(16) 0.0299(14)
F3 0.0662(16) 0.0514(13) 0.0821(18) -0.0231(13) 0.0277(14) -0.0121(12)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 Br1 2.5439(4) . ?
Ru1 N1 2.0786(19) . ?
Ru1 N2 2.1360(19) . ?
Ru1 C21 2.217(3) . ?
Ru1 C20 2.191(3) . ?
Ru1 C22 2.217(3) . ?
Ru1 C18 2.230(2) . ?
Ru1 C19 2.207(3) . ?
Ru1 C23 2.221(3) . ?
O1 C10 1.297(3) . ?
N1 C11 1.438(3) . ?
N1 C10 1.315(3) . ?
C11 C12 1.389(4) . ?
C11 C16 1.392(4) . ?
C10 C9 1.493(3) . ?
N2 C1 1.388(3) . ?
N2 C9 1.350(3) . ?
C6 C1 1.439(3) . ?
C6 C7 1.417(4) . ?
C6 C5 1.428(4) . ?
C8 H8 0.9500 . ?
C8 C7 1.370(4) . ?
C8 C9 1.421(3) . ?
C1 C2 1.420(3) . ?
C7 H7 0.9500 . ?
C2 H2 0.9500 . ?
C2 C3 1.376(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.417(4) . ?
C5 H5 0.9500 . ?
C5 C4 1.369(4) . ?
C4 H4 0.9500 . ?
C12 H12 0.9500 . ?
C12 C13 1.395(4) . ?
C16 C15 1.379(4) . ?
C16 F1 1.371(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.393(4) . ?
C15 H15 0.9500 . ?
C15 C14 1.395(4) . ?
C14 H14 0.9500 . ?
C21 C20 1.405(4) . ?
C21 C22 1.436(4) . ?
C21 C24 1.524(4) . ?
C20 H20 0.9500 . ?
C20 C19 1.438(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.404(4) . ?
C18 C19 1.398(4) . ?
C18 C23 1.423(4) . ?
C18 C17 1.522(4) . ?
C19 H19 0.9500 . ?
C23 H23 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C24 H24 1.0000 . ?
C24 C25 1.551(5) . ?
C24 C26 1.531(5) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
P1 F4 1.612(2) 7_556 ?
P1 F4 1.612(2) . ?
P1 F2 1.589(2) 7_556 ?
P1 F2 1.589(2) . ?
P1 F3 1.603(2) 7_556 ?
P1 F3 1.603(2) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ru1 Br1 86.93(6) . . ?
N1 Ru1 N2 76.31(8) . . ?
N1 Ru1 C21 114.14(9) . . ?
N1 Ru1 C20 91.25(9) . . ?
N1 Ru1 C22 151.60(9) . . ?
N1 Ru1 C18 122.54(10) . . ?
N1 Ru1 C19 95.28(10) . . ?
N1 Ru1 C23 159.79(10) . . ?
N2 Ru1 Br1 84.45(5) . . ?
N2 Ru1 C21 96.53(8) . . ?
N2 Ru1 C20 120.71(9) . . ?
N2 Ru1 C22 99.14(9) . . ?
N2 Ru1 C18 160.42(10) . . ?
N2 Ru1 C19 158.03(10) . . ?
N2 Ru1 C23 123.87(10) . . ?
C21 Ru1 Br1 158.60(7) . . ?
C21 Ru1 C22 37.78(10) . . ?
C21 Ru1 C18 80.97(10) . . ?
C21 Ru1 C23 68.02(10) . . ?
C20 Ru1 Br1 153.56(8) . . ?
C20 Ru1 C21 37.17(10) . . ?
C20 Ru1 C22 66.65(10) . . ?
C20 Ru1 C18 67.95(11) . . ?
C20 Ru1 C19 38.18(11) . . ?
C20 Ru1 C23 79.32(10) . . ?
C22 Ru1 Br1 120.87(8) . . ?
C22 Ru1 C18 67.03(11) . . ?
C22 Ru1 C23 36.88(10) . . ?
C18 Ru1 Br1 90.95(8) . . ?
C19 Ru1 Br1 115.72(8) . . ?
C19 Ru1 C21 68.07(10) . . ?
C19 Ru1 C22 78.51(10) . . ?
C19 Ru1 C18 36.74(11) . . ?
C19 Ru1 C23 66.30(11) . . ?
C23 Ru1 Br1 93.62(8) . . ?
C23 Ru1 C18 37.29(11) . . ?
C11 N1 Ru1 121.75(14) . . ?
C10 N1 Ru1 118.15(16) . . ?
C10 N1 C11 119.2(2) . . ?
C12 C11 N1 121.4(2) . . ?
C12 C11 C16 118.0(2) . . ?
C16 C11 N1 120.5(2) . . ?
O1 C10 N1 124.1(2) . . ?
O1 C10 C9 121.4(2) . . ?
N1 C10 C9 114.3(2) . . ?
C1 N2 Ru1 127.08(16) . . ?
C9 N2 Ru1 114.65(15) . . ?
C9 N2 C1 118.3(2) . . ?
C7 C6 C1 119.0(2) . . ?
C7 C6 C5 122.0(2) . . ?
C5 C6 C1 119.0(2) . . ?
C7 C8 H8 120.6 . . ?
C7 C8 C9 118.9(2) . . ?
C9 C8 H8 120.6 . . ?
N2 C1 C6 120.4(2) . . ?
N2 C1 C2 120.5(2) . . ?
C2 C1 C6 119.1(2) . . ?
C6 C7 H7 120.2 . . ?
C8 C7 C6 119.7(2) . . ?
C8 C7 H7 120.2 . . ?
N2 C9 C10 114.9(2) . . ?
N2 C9 C8 123.5(2) . . ?
C8 C9 C10 121.5(2) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 C1 120.1(2) . . ?
C3 C2 H2 119.9 . . ?
C2 C3 H3 119.6 . . ?
C2 C3 C4 120.8(3) . . ?
C4 C3 H3 119.6 . . ?
C6 C5 H5 119.9 . . ?
C4 C5 C6 120.2(2) . . ?
C4 C5 H5 119.9 . . ?
C3 C4 H4 119.6 . . ?
C5 C4 C3 120.8(2) . . ?
C5 C4 H4 119.6 . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 120.1(3) . . ?
C13 C12 H12 120.0 . . ?
C15 C16 C11 123.3(2) . . ?
F1 C16 C11 117.6(2) . . ?
F1 C16 C15 119.1(2) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 C12 120.5(3) . . ?
C14 C13 H13 119.7 . . ?
C16 C15 H15 121.0 . . ?
C16 C15 C14 118.0(3) . . ?
C14 C15 H15 121.0 . . ?
C13 C14 C15 120.1(3) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C20 C21 Ru1 70.40(15) . . ?
C20 C21 C22 117.0(2) . . ?
C20 C21 C24 123.5(3) . . ?
C22 C21 Ru1 71.11(15) . . ?
C22 C21 C24 119.6(3) . . ?
C24 C21 Ru1 129.74(19) . . ?
Ru1 C20 H20 129.0 . . ?
C21 C20 Ru1 72.43(15) . . ?
C21 C20 H20 119.5 . . ?
C21 C20 C19 121.1(3) . . ?
C19 C20 Ru1 71.52(16) . . ?
C19 C20 H20 119.5 . . ?
Ru1 C22 H22 131.0 . . ?
C21 C22 Ru1 71.11(15) . . ?
C21 C22 H22 119.0 . . ?
C23 C22 Ru1 71.73(16) . . ?
C23 C22 C21 121.9(3) . . ?
C23 C22 H22 119.0 . . ?
C19 C18 Ru1 70.75(14) . . ?
C19 C18 C23 118.3(2) . . ?
C19 C18 C17 121.6(3) . . ?
C23 C18 Ru1 71.04(15) . . ?
C23 C18 C17 120.1(3) . . ?
C17 C18 Ru1 127.6(2) . . ?
Ru1 C19 H19 130.4 . . ?
C20 C19 Ru1 70.30(15) . . ?
C20 C19 H19 119.4 . . ?
C18 C19 Ru1 72.51(16) . . ?
C18 C19 C20 121.1(3) . . ?
C18 C19 H19 119.4 . . ?
Ru1 C23 H23 129.7 . . ?
C22 C23 Ru1 71.39(15) . . ?
C22 C23 C18 120.6(3) . . ?
C22 C23 H23 119.7 . . ?
C18 C23 Ru1 71.67(15) . . ?
C18 C23 H23 119.7 . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C21 C24 H24 107.8 . . ?
C21 C24 C25 107.9(2) . . ?
C21 C24 C26 114.3(3) . . ?
C25 C24 H24 107.8 . . ?
C26 C24 H24 107.8 . . ?
C26 C24 C25 111.1(3) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
F4 P1 F4 180.0 7_556 . ?
F2 P1 F4 90.07(13) . 7_556 ?
F2 P1 F4 89.93(13) 7_556 7_556 ?
F2 P1 F4 89.93(13) . . ?
F2 P1 F4 90.07(13) 7_556 . ?
F2 P1 F2 180.0 7_556 . ?
F2 P1 F3 89.77(13) 7_556 . ?
F2 P1 F3 90.23(13) 7_556 7_556 ?
F2 P1 F3 89.77(13) . 7_556 ?
F2 P1 F3 90.23(13) . . ?
F3 P1 F4 91.39(12) . . ?
F3 P1 F4 88.61(12) 7_556 . ?
F3 P1 F4 88.61(12) . 7_556 ?
F3 P1 F4 91.39(12) 7_556 7_556 ?
F3 P1 F3 180.0 7_556 . ?
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 C11 C12 75.0(3) . . . . ?
Ru1 N1 C11 C16 -101.8(2) . . . . ?
Ru1 N1 C10 O1 172.34(18) . . . . ?
Ru1 N1 C10 C9 -11.2(3) . . . . ?
Ru1 N2 C1 C6 173.96(17) . . . . ?
Ru1 N2 C1 C2 -8.0(3) . . . . ?
Ru1 N2 C9 C10 7.7(3) . . . . ?
Ru1 N2 C9 C8 -175.43(19) . . . . ?
Ru1 C21 C20 C19 -54.6(2) . . . . ?
Ru1 C21 C22 C23 52.9(2) . . . . ?
Ru1 C21 C24 C25 168.4(3) . . . . ?
Ru1 C21 C24 C26 -67.5(4) . . . . ?
Ru1 C20 C19 C18 -53.9(2) . . . . ?
Ru1 C22 C23 C18 54.2(2) . . . . ?
Ru1 C18 C19 C20 52.9(2) . . . . ?
Ru1 C18 C23 C22 -54.1(2) . . . . ?
O1 C10 C9 N2 178.5(2) . . . . ?
O1 C10 C9 C8 1.6(4) . . . . ?
N1 C11 C12 C13 -177.6(2) . . . . ?
N1 C11 C16 C15 177.3(2) . . . . ?
N1 C11 C16 F1 -1.9(3) . . . . ?
N1 C10 C9 N2 1.9(3) . . . . ?
N1 C10 C9 C8 -175.0(2) . . . . ?
C11 N1 C10 O1 3.2(4) . . . . ?
C11 N1 C10 C9 179.6(2) . . . . ?
C11 C12 C13 C14 0.6(4) . . . . ?
C11 C16 C15 C14 0.1(4) . . . . ?
C10 N1 C11 C12 -116.2(3) . . . . ?
C10 N1 C11 C16 66.9(3) . . . . ?
N2 C1 C2 C3 178.6(2) . . . . ?
C6 C1 C2 C3 -3.2(4) . . . . ?
C6 C5 C4 C3 -1.1(4) . . . . ?
C1 N2 C9 C10 -172.0(2) . . . . ?
C1 N2 C9 C8 4.8(4) . . . . ?
C1 C6 C7 C8 1.7(4) . . . . ?
C1 C6 C5 C4 -1.0(4) . . . . ?
C1 C2 C3 C4 1.1(4) . . . . ?
C7 C6 C1 N2 3.2(4) . . . . ?
C7 C6 C1 C2 -175.0(2) . . . . ?
C7 C6 C5 C4 177.1(3) . . . . ?
C7 C8 C9 C10 176.7(2) . . . . ?
C7 C8 C9 N2 0.1(4) . . . . ?
C9 N2 C1 C6 -6.3(3) . . . . ?
C9 N2 C1 C2 171.8(2) . . . . ?
C9 C8 C7 C6 -3.3(4) . . . . ?
C2 C3 C4 C5 1.1(4) . . . . ?
C5 C6 C1 N2 -178.7(2) . . . . ?
C5 C6 C1 C2 3.2(4) . . . . ?
C5 C6 C7 C8 -176.4(2) . . . . ?
C12 C11 C16 C15 0.3(4) . . . . ?
C12 C11 C16 F1 -178.8(2) . . . . ?
C12 C13 C14 C15 -0.1(4) . . . . ?
C16 C11 C12 C13 -0.7(4) . . . . ?
C16 C15 C14 C13 -0.2(4) . . . . ?
C21 C20 C19 Ru1 55.0(2) . . . . ?
C21 C20 C19 C18 1.1(4) . . . . ?
C21 C22 C23 Ru1 -52.6(2) . . . . ?
C21 C22 C23 C18 1.6(4) . . . . ?
C20 C21 C22 Ru1 -55.1(2) . . . . ?
C20 C21 C22 C23 -2.2(4) . . . . ?
C20 C21 C24 C25 -100.0(4) . . . . ?
C20 C21 C24 C26 24.0(4) . . . . ?
C22 C21 C20 Ru1 55.5(2) . . . . ?
C22 C21 C20 C19 0.9(4) . . . . ?
C22 C21 C24 C25 79.2(4) . . . . ?
C22 C21 C24 C26 -156.8(3) . . . . ?
C19 C18 C23 Ru1 54.5(2) . . . . ?
C19 C18 C23 C22 0.4(4) . . . . ?
C23 C18 C19 Ru1 -54.7(2) . . . . ?
C23 C18 C19 C20 -1.8(4) . . . . ?
C17 C18 C19 Ru1 123.0(3) . . . . ?
C17 C18 C19 C20 175.9(2) . . . . ?
C17 C18 C23 Ru1 -123.2(3) . . . . ?
C17 C18 C23 C22 -177.3(3) . . . . ?
C24 C21 C20 Ru1 -125.3(3) . . . . ?
C24 C21 C20 C19 -179.9(2) . . . . ?
C24 C21 C22 Ru1 125.6(2) . . . . ?
C24 C21 C22 C23 178.5(3) . . . . ?
F1 C16 C15 C14 179.3(2) . . . . ?
_shelx_SHELXL_version_number 2014/7
_iucr_refine_instructions_details
;
kr220_0m.res created by SHELXL-2014/7
TITL kr220_0m in C2/c
REM kr220_0m in C2/c
REM 325 parameters refined using 0 restraints
REM Highest difference peak 0.679, deepest hole -0.613, 1-sigma level 0.098
REM 326 parameters refined using 0 restraints
REM Highest difference peak 0.681, deepest hole -0.607, 1-sigma level 0.097
CELL 0.71073 31.3092 10.0915 18.4285 90 118.325 90
ZERR 4 0.0028 0.0009 0.0016 0 0.004 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H Br F N O P Ru
UNIT 208 196 8 32 16 8 4 8
L.S. 20
PLAN 20
SIZE 0.33 0.18 0.02
TEMP -125
GRID
BOND $H
fmap 2
acta
MORE -1
CONF
MERG 2
OMIT 2 0 0
REM
REM
REM
WGHT 0.028200 5.642000
FVAR 0.11902
RU1 8 0.128729 0.723025 0.485632 11.00000 0.01282 0.01547 =
0.01687 0.00085 0.00825 0.00234
BR1 3 0.075786 0.577072 0.362966 11.00000 0.02505 0.02101 =
0.02168 -0.00371 0.01223 -0.00341
O1 6 0.008825 0.954873 0.447382 11.00000 0.02289 0.02597 =
0.02428 0.00535 0.01476 0.01038
N1 5 0.072995 0.861630 0.436962 11.00000 0.01544 0.01422 =
0.01710 0.00129 0.00760 0.00187
C11 1 0.072615 0.967224 0.384222 11.00000 0.01486 0.01978 =
0.02045 0.00506 0.01086 0.00490
C10 1 0.041920 0.864637 0.466019 11.00000 0.01438 0.01877 =
0.01582 -0.00080 0.00722 0.00167
N2 5 0.080946 0.661827 0.531994 11.00000 0.01466 0.01721 =
0.01437 -0.00066 0.00621 -0.00074
C6 1 0.050694 0.522684 0.606937 11.00000 0.02047 0.02276 =
0.01358 -0.00246 0.00535 -0.00560
C8 1 0.012139 0.731943 0.550553 11.00000 0.01768 0.02385 =
0.02026 -0.00264 0.01100 -0.00039
AFIX 43
H8 2 -0.012256 0.796265 0.540149 11.00000 -1.20000
AFIX 0
C1 1 0.082734 0.544021 0.572238 11.00000 0.01623 0.01822 =
0.01309 -0.00115 0.00397 -0.00306
C7 1 0.015726 0.620780 0.595766 11.00000 0.02398 0.02625 =
0.02224 -0.00302 0.01571 -0.00649
AFIX 43
H7 2 -0.005136 0.609520 0.619520 11.00000 -1.20000
AFIX 0
C9 1 0.045509 0.749436 0.519479 11.00000 0.01654 0.01844 =
0.01469 -0.00006 0.00745 0.00111
C2 1 0.115129 0.441430 0.577561 11.00000 0.02386 0.01955 =
0.02113 0.00036 0.00915 -0.00008
AFIX 43
H2 2 0.135290 0.452437 0.552437 11.00000 -1.20000
AFIX 0
C3 1 0.117373 0.326055 0.619061 11.00000 0.02605 0.01858 =
0.02075 0.00137 0.00385 0.00136
AFIX 43
H3 2 0.139559 0.258526 0.623191 11.00000 -1.20000
AFIX 0
C5 1 0.054149 0.401533 0.649463 11.00000 0.03032 0.02756 =
0.01713 0.00116 0.01038 -0.00795
AFIX 43
H5 2 0.033598 0.386691 0.673477 11.00000 -1.20000
AFIX 0
C4 1 0.086997 0.306782 0.655695 11.00000 0.03524 0.02112 =
0.01966 0.00568 0.00700 -0.00608
AFIX 43
H4 2 0.089459 0.227153 0.684929 11.00000 -1.20000
AFIX 0
C12 1 0.061174 0.944032 0.302729 11.00000 0.01891 0.02607 =
0.02058 0.00114 0.00933 0.00028
AFIX 43
H12 2 0.052175 0.857580 0.280140 11.00000 -1.20000
AFIX 0
C16 1 0.086104 1.095103 0.414958 11.00000 0.02492 0.01950 =
0.02410 0.00234 0.01273 0.00449
C13 1 0.062879 1.047515 0.253991 11.00000 0.02871 0.04330 =
0.02267 0.00750 0.01251 0.00073
AFIX 43
H13 2 0.054729 1.031270 0.198129 11.00000 -1.20000
AFIX 0
C15 1 0.088385 1.199286 0.368456 11.00000 0.03110 0.02183 =
0.03759 0.00521 0.01375 0.00033
AFIX 43
H15 2 0.097811 1.285320 0.391521 11.00000 -1.20000
AFIX 0
C14 1 0.076432 1.174464 0.286553 11.00000 0.03523 0.03278 =
0.03743 0.01652 0.01633 0.00075
AFIX 43
H14 2 0.077535 1.244286 0.252906 11.00000 -1.20000
AFIX 0
C21 1 0.190178 0.780199 0.606203 11.00000 0.01549 0.03376 =
0.02172 -0.00675 0.00826 -0.00520
C20 1 0.182553 0.879117 0.547633 11.00000 0.01468 0.02203 =
0.04154 -0.00571 0.01146 -0.00479
AFIX 43
H20 2 0.177650 0.968126 0.558777 11.00000 -1.20000
AFIX 0
C22 1 0.198078 0.647891 0.586507 11.00000 0.01678 0.02649 =
0.02832 0.00833 0.00260 0.00425
AFIX 43
H22 2 0.204508 0.579303 0.625666 11.00000 -1.20000
AFIX 0
C18 1 0.188298 0.717698 0.451839 11.00000 0.01303 0.05655 =
0.02714 -0.00566 0.01256 -0.00153
C19 1 0.182049 0.847858 0.471081 11.00000 0.01273 0.04288 =
0.03427 0.01327 0.00897 -0.00382
AFIX 43
H19 2 0.177391 0.916827 0.432938 11.00000 -1.20000
AFIX 0
C23 1 0.196579 0.616906 0.511076 11.00000 0.01508 0.03104 =
0.03921 -0.00954 0.00851 0.00584
AFIX 43
H23 2 0.201133 0.527860 0.499471 11.00000 -1.20000
AFIX 0
C17 1 0.184529 0.681894 0.368750 11.00000 0.02637 0.10913 =
0.03300 -0.01591 0.01923 -0.00817
AFIX 137
H17A 2 0.174123 0.759827 0.332713 11.00000 -1.50000
H17B 2 0.160771 0.610538 0.343378 11.00000 -1.50000
H17C 2 0.216266 0.652269 0.376672 11.00000 -1.50000
AFIX 0
C24 1 0.191034 0.807261 0.688250 11.00000 0.02863 0.06646 =
0.02517 -0.01192 0.01169 -0.00867
AFIX 13
H24 2 0.175819 0.729695 0.700937 11.00000 -1.20000
AFIX 0
F1 4 0.098213 1.116512 0.495928 11.00000 0.04518 0.02571 =
0.02687 -0.00589 0.01721 0.00007
C25 1 0.244855 0.814589 0.755933 11.00000 0.03925 0.12571 =
0.02326 -0.01879 0.01082 -0.00728
AFIX 137
H25A 2 0.261084 0.730735 0.757602 11.00000 -1.50000
H25B 2 0.246381 0.830492 0.809574 11.00000 -1.50000
H25C 2 0.261102 0.887172 0.743382 11.00000 -1.50000
AFIX 0
C26 1 0.163235 0.931774 0.688776 11.00000 0.04901 0.11003 =
0.05541 -0.03924 0.02898 0.00302
AFIX 137
H26A 2 0.180618 1.010605 0.685798 11.00000 -1.50000
H26B 2 0.160621 0.934301 0.739686 11.00000 -1.50000
H26C 2 0.130673 0.930109 0.641181 11.00000 -1.50000
AFIX 0
P1 7 0.250000 0.250000 0.500000 10.50000 0.03740 0.02742 =
0.05551 -0.00024 0.01837 0.00510
F4 4 0.204489 0.280459 0.515711 11.00000 0.05256 0.06803 =
0.09571 -0.00795 0.04200 0.00533
F2 4 0.230978 0.358403 0.428990 11.00000 0.11024 0.04992 =
0.07556 0.01761 0.04446 0.02989
F3 4 0.220038 0.137673 0.433691 11.00000 0.06619 0.05145 =
0.08206 -0.02309 0.02774 -0.01206
HKLF 4
REM kr220_0m in C2/c
REM R1 = 0.0326 for 5289 Fo > 4sig(Fo) and 0.0525 for all 6751 data
REM 325 parameters refined using 0 restraints
END
WGHT 0.0282 5.6422
REM Highest difference peak 0.680, deepest hole -0.614, 1-sigma level 0.098
Q1 1 0.1313 0.7343 0.5359 11.00000 0.05 0.68
Q2 1 0.1289 0.7070 0.4422 11.00000 0.05 0.64
Q3 1 0.0000 1.0000 0.5000 10.50000 0.05 0.54
Q4 1 0.1020 0.5875 0.3641 11.00000 0.05 0.52
Q5 1 0.2341 0.3132 0.3899 11.00000 0.05 0.52
Q6 1 0.2016 0.7273 0.6957 11.00000 0.05 0.52
Q7 1 0.0627 0.5072 0.3911 11.00000 0.05 0.49
Q8 1 0.0556 0.6230 0.3406 11.00000 0.05 0.48
Q9 1 0.0697 0.5657 0.3105 11.00000 0.05 0.46
Q10 1 0.0763 0.6009 0.4063 11.00000 0.05 0.45
Q11 1 0.0498 0.4465 0.6204 11.00000 0.05 0.45
Q12 1 0.2029 0.2929 0.4693 11.00000 0.05 0.44
Q13 1 0.2502 0.2732 0.4488 11.00000 0.05 0.43
Q14 1 0.2191 0.1099 0.4818 11.00000 0.05 0.43
Q15 1 0.2098 0.6363 0.5582 11.00000 0.05 0.42
Q16 1 0.0996 0.7216 0.4820 11.00000 0.05 0.42
Q17 1 0.1067 0.3639 0.5776 11.00000 0.05 0.42
Q18 1 0.0948 0.6886 0.5029 11.00000 0.05 0.42
Q19 1 0.0917 1.0162 0.4092 11.00000 0.05 0.41
Q20 1 0.0903 0.4757 0.5613 11.00000 0.05 0.41
REM The information below was added by Olex2.
REM
REM R1 = 0.0326 for 5289 Fo > 4sig(Fo) and 0.0525 for all 34973 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.68, deepest hole -0.61
REM Mean Shift 0, Max Shift 0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0525
REM R1_gt = 0.0326
REM wR_ref = 0.0694
REM GOOF = 1.011
REM Shift_max = 0.001
REM Shift_mean = 0
REM Reflections_all = 34973
REM Reflections_gt = 5289
REM Parameters = n/a
REM Hole = -0.61
REM Peak = 0.68
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT430_I
;
PROBLEM: Short Inter D...A Contact O1 .. O1 .. 2.43 Ang.
RESPONSE: Structure is hydrogen bridged dimer, with hydrogen bridging the amide oxygen atoms.
;
# end Validation Reply Form
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_kr275_twin1_hklf4
_database_code_depnum_ccdc_archive 'CCDC 1472243'
_audit_update_record
;
2016-06-30 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;
_audit_creation_date 2016-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C52 H49 Br2 F2 N4 O2 Ru2, F6 P'
_chemical_formula_sum 'C52 H49 Br2 F8 N4 O2 P Ru2'
_chemical_formula_weight 1306.88
_chemical_melting_point ?
_chemical_oxdiff_formula 'C52 H49 Br2 F2 N4 O2 Ru2'
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
_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.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.4885(4)
_cell_length_b 9.8280(3)
_cell_length_c 14.7862(6)
_cell_angle_alpha 72.595(3)
_cell_angle_beta 83.935(4)
_cell_angle_gamma 73.979(3)
_cell_volume 1264.22(9)
_cell_formula_units_Z 1
_cell_measurement_reflns_used 16342
_cell_measurement_temperature 148(2)
_cell_measurement_theta_max 36.8300
_cell_measurement_theta_min 2.3250
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 2.284
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.75528
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour Red
_exptl_crystal_colour_primary Red
_exptl_crystal_density_diffrn 1.717
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 650
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.17
_exptl_crystal_size_min 0.03
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents ?
_diffrn_reflns_av_unetI/netI 0.0118
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.870
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 15986
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.870
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 36.888
_diffrn_reflns_theta_min 2.303
_diffrn_ambient_temperature 148.15
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 phi -179.98 179.52 0.5000 3.0000
omega____ theta____ kappa____ phi______ frames
26.6763 30.0000 -42.0167 - 719
#__ type_ start__ end____ width___ exp.time_
2 phi -67.68 179.32 0.5000 3.0000
omega____ theta____ kappa____ phi______ frames
-50.1719 -37.5000 95.5348 - 494
#__ type_ start__ end____ width___ exp.time_
3 omega 70.37 116.37 0.5000 3.0000
omega____ theta____ kappa____ phi______ frames
- 30.0000 -164.7503 -109.8047 92
#__ type_ start__ end____ width___ exp.time_
4 omega 233.73 302.73 0.5000 3.0000
omega____ theta____ kappa____ phi______ frames
- -37.5000 -147.1258 77.5962 138
#__ type_ start__ end____ width___ exp.time_
5 omega -105.58 -17.58 0.5000 3.0000
omega____ theta____ kappa____ phi______ frames
- -37.5000 140.6036 94.9166 176
#__ type_ start__ end____ width___ exp.time_
6 omega -3.08 39.42 0.5000 3.0000
omega____ theta____ kappa____ phi______ frames
- 27.5000 30.5150 -92.5050 85
#__ type_ start__ end____ width___ exp.time_
7 phi -62.01 179.49 0.5000 3.0000
omega____ theta____ kappa____ phi______ frames
10.0474 -25.0000 -87.0339 - 483
#__ type_ start__ end____ width___ exp.time_
8 phi -123.79 179.21 0.5000 3.0000
omega____ theta____ kappa____ phi______ frames
47.9085 17.5000 -114.5508 - 606
;
_diffrn_measurement_device_type 'Bruker X8 Apex diffractometer'
_diffrn_measurement_method 'Rotation images'
_diffrn_orient_matrix_UB_11 0.0558747000
_diffrn_orient_matrix_UB_12 0.0093878000
_diffrn_orient_matrix_UB_13 0.0240958000
_diffrn_orient_matrix_UB_21 -0.0415220000
_diffrn_orient_matrix_UB_22 -0.0136022000
_diffrn_orient_matrix_UB_23 0.0430288000
_diffrn_orient_matrix_UB_31 0.0347374000
_diffrn_orient_matrix_UB_32 -0.0765103000
_diffrn_orient_matrix_UB_33 0.0098383000
loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.6330 12630 23210
2 0.3670 12690 23210
_diffrn_oxdiff_twin_integration_method simultaneous
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'rotating anode'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 15096
_reflns_number_total 15986
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
APEX 2 software, Bruker Nonius 2004
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'local program'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max 1.640
_refine_diff_density_min -2.046
_refine_diff_density_rms 0.150
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.098
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 326
_refine_ls_number_reflns 15986
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0514
_refine_ls_R_factor_gt 0.0479
_refine_ls_restrained_S_all 1.098
_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^)+(0.0574P)^2^+4.6881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1297
_refine_ls_wR_factor_ref 0.1323
_refine_special_details
;
Structure was refined as a two component twin with HKLF5 refinement and BASF 0.37.
Reflections -1 0 0, 1 0 0, 0 -1 0 omitted as obscured by beamstop.
;
_olex2_refinement_description
;
1. Twinned data refinement
Scales: 0.6364(7) 0.3636(7)
2. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
C24(H24)
3.b Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C12(H12), C13(H13), C15(H15),
C16(H16), C19(H19), C20(H20), C22(H22), C23(H23)
3.c Idealised Me refined as rotating group:
C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
;
_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 0.31105(3) 0.46960(3) 0.23421(2) 0.01317(6) Uani 1 1 d . . . . .
Br1 Br 0.12402(4) 0.60837(4) 0.33227(3) 0.01971(8) Uani 1 1 d . . . . .
F1 F -0.1190(4) 0.0046(4) 0.2704(3) 0.0474(9) Uani 1 1 d . . . . .
O1 O 0.3906(3) 0.0843(3) 0.4604(2) 0.0257(6) Uani 1 1 d . . . . .
N1 N 0.4626(3) 0.4349(3) 0.3404(2) 0.0138(5) Uani 1 1 d . . . . .
C1 C 0.5409(4) 0.5325(3) 0.3459(2) 0.0147(5) Uani 1 1 d . . . . .
N2 N 0.2886(3) 0.2751(3) 0.3340(2) 0.0154(5) Uani 1 1 d . . . . .
C2 C 0.5113(4) 0.6786(4) 0.2852(3) 0.0176(6) Uani 1 1 d . . . . .
H2 H 0.4347 0.7125 0.2431 0.021 Uiso 1 1 calc R . . . .
C3 C 0.5960(5) 0.7707(4) 0.2885(3) 0.0219(7) Uani 1 1 d . . . . .
H3 H 0.5765 0.8659 0.2475 0.026 Uiso 1 1 calc R . . . .
C4 C 0.7119(5) 0.7237(4) 0.3526(3) 0.0227(7) Uani 1 1 d . . . . .
H4 H 0.7692 0.7866 0.3527 0.027 Uiso 1 1 calc R . . . .
C5 C 0.7392(4) 0.5846(4) 0.4147(3) 0.0209(7) Uani 1 1 d . . . . .
H5 H 0.8142 0.5542 0.4577 0.025 Uiso 1 1 calc R . . . .
C6 C 0.6538(4) 0.4863(4) 0.4139(2) 0.0157(6) Uani 1 1 d . . . . .
C7 C 0.6758(4) 0.3450(4) 0.4796(3) 0.0186(6) Uani 1 1 d . . . . .
H7 H 0.7480 0.3132 0.5247 0.022 Uiso 1 1 calc R . . . .
C8 C 0.5896(4) 0.2543(4) 0.4767(3) 0.0179(6) Uani 1 1 d . . . . .
H8 H 0.6007 0.1622 0.5208 0.021 Uiso 1 1 calc R . . . .
C9 C 0.4844(4) 0.3036(3) 0.4058(2) 0.0145(5) Uani 1 1 d . . . . .
C10 C 0.3855(4) 0.2119(3) 0.4001(3) 0.0162(6) Uani 1 1 d . . . . .
C11 C 0.1848(4) 0.1988(3) 0.3228(3) 0.0173(6) Uani 1 1 d . . . . .
C12 C 0.2303(5) 0.0741(4) 0.2902(4) 0.0268(8) Uani 1 1 d . . . . .
H12 H 0.3297 0.0348 0.2800 0.032 Uiso 1 1 calc R . . . .
C13 C 0.1277(5) 0.0076(5) 0.2728(4) 0.0328(10) Uani 1 1 d . . . . .
H13 H 0.1576 -0.0755 0.2509 0.039 Uiso 1 1 calc R . . . .
C14 C -0.0176(5) 0.0669(5) 0.2887(4) 0.0293(9) Uani 1 1 d . . . . .
C15 C -0.0660(5) 0.1893(5) 0.3219(4) 0.0308(9) Uani 1 1 d . . . . .
H15 H -0.1657 0.2266 0.3326 0.037 Uiso 1 1 calc R . . . .
C16 C 0.0365(5) 0.2568(5) 0.3394(3) 0.0259(8) Uani 1 1 d . . . . .
H16 H 0.0056 0.3394 0.3619 0.031 Uiso 1 1 calc R . . . .
C17 C 0.6315(5) 0.3201(7) 0.1430(4) 0.0392(12) Uani 1 1 d . . . . .
H17A H 0.6851 0.3677 0.1699 0.059 Uiso 1 1 calc GR . . . .
H17B H 0.6777 0.3076 0.0840 0.059 Uiso 1 1 calc GR . . . .
H17C H 0.6305 0.2253 0.1860 0.059 Uiso 1 1 calc GR . . . .
C18 C 0.4767(5) 0.4135(5) 0.1257(3) 0.0229(7) Uani 1 1 d . . . . .
C19 C 0.3581(5) 0.3539(4) 0.1248(3) 0.0236(7) Uani 1 1 d . . . . .
H19 H 0.3763 0.2535 0.1311 0.028 Uiso 1 1 calc R . . . .
C20 C 0.2108(5) 0.4430(4) 0.1145(3) 0.0210(7) Uani 1 1 d . . . . .
H20 H 0.1349 0.4003 0.1141 0.025 Uiso 1 1 calc R . . . .
C21 C 0.1793(5) 0.5959(4) 0.1047(3) 0.0208(7) Uani 1 1 d . . . . .
C22 C 0.2991(4) 0.6586(4) 0.1046(3) 0.0207(7) Uani 1 1 d . . . . .
H22 H 0.2809 0.7590 0.0978 0.025 Uiso 1 1 calc R . . . .
C23 C 0.4442(5) 0.5689(5) 0.1145(3) 0.0232(7) Uani 1 1 d . . . . .
H23 H 0.5206 0.6116 0.1138 0.028 Uiso 1 1 calc R . . . .
C24 C 0.0242(5) 0.6954(5) 0.0955(3) 0.0289(8) Uani 1 1 d . . . . .
H24 H 0.0144 0.7606 0.1359 0.035 Uiso 1 1 calc R . . . .
C25 C 0.0033(6) 0.7932(6) -0.0081(4) 0.0390(11) Uani 1 1 d . . . . .
H25A H 0.0729 0.8519 -0.0241 0.058 Uiso 1 1 calc GR . . . .
H25B H -0.0944 0.8567 -0.0148 0.058 Uiso 1 1 calc GR . . . .
H25C H 0.0183 0.7317 -0.0497 0.058 Uiso 1 1 calc GR . . . .
C26 C -0.0953(6) 0.6112(7) 0.1270(4) 0.0414(12) Uani 1 1 d . . . . .
H26A H -0.0967 0.5565 0.0832 0.062 Uiso 1 1 calc GR . . . .
H26B H -0.1890 0.6802 0.1282 0.062 Uiso 1 1 calc GR . . . .
H26C H -0.0747 0.5445 0.1892 0.062 Uiso 1 1 calc GR . . . .
P1 P 0.5000 0.0000 0.0000 0.0208(3) Uani 1 2 d S T P . .
F2 F 0.4102(4) 0.1695(3) -0.0269(3) 0.0443(8) Uani 1 1 d . . . . .
F3 F 0.5996(4) 0.0332(4) -0.0949(2) 0.0400(7) Uani 1 1 d . . . . .
F4 F 0.3872(4) -0.0366(4) -0.0568(2) 0.0453(8) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.01505(11) 0.01281(9) 0.01202(11) -0.00239(8) -0.00205(9) -0.00480(7)
Br1 0.01953(17) 0.01992(15) 0.02034(17) -0.00785(13) -0.00162(13) -0.00333(12)
F1 0.0396(17) 0.0403(16) 0.075(2) -0.0182(16) -0.0131(16) -0.0251(14)
O1 0.0297(15) 0.0150(10) 0.0295(15) 0.0058(9) -0.0114(12) -0.0107(10)
N1 0.0145(12) 0.0142(10) 0.0135(12) -0.0034(9) -0.0007(10) -0.0055(9)
C1 0.0169(14) 0.0148(11) 0.0131(14) -0.0043(10) 0.0002(11) -0.0052(10)
N2 0.0162(13) 0.0137(10) 0.0172(13) -0.0027(9) -0.0024(10) -0.0065(9)
C2 0.0219(16) 0.0150(12) 0.0161(15) -0.0020(10) -0.0023(12) -0.0073(11)
C3 0.0256(18) 0.0184(13) 0.0232(17) -0.0040(12) 0.0029(14) -0.0117(13)
C4 0.0240(18) 0.0219(15) 0.0256(18) -0.0060(13) -0.0002(14) -0.0125(13)
C5 0.0190(16) 0.0257(15) 0.0217(17) -0.0076(13) 0.0005(13) -0.0111(13)
C6 0.0162(15) 0.0177(12) 0.0148(14) -0.0051(10) 0.0003(11) -0.0066(10)
C7 0.0180(16) 0.0210(14) 0.0174(15) -0.0044(11) -0.0042(12) -0.0058(11)
C8 0.0197(16) 0.0168(12) 0.0154(15) 0.0004(11) -0.0047(12) -0.0059(11)
C9 0.0163(14) 0.0130(11) 0.0143(14) -0.0020(10) -0.0025(11) -0.0054(10)
C10 0.0156(14) 0.0122(11) 0.0191(15) -0.0007(10) -0.0019(12) -0.0043(10)
C11 0.0187(15) 0.0136(11) 0.0204(16) -0.0030(11) -0.0029(12) -0.0064(10)
C12 0.0231(19) 0.0185(14) 0.042(2) -0.0122(15) -0.0055(17) -0.0052(13)
C13 0.034(2) 0.0216(16) 0.052(3) -0.0171(17) -0.008(2) -0.0106(15)
C14 0.029(2) 0.0259(17) 0.040(2) -0.0079(16) -0.0064(18) -0.0174(15)
C15 0.0206(19) 0.035(2) 0.042(3) -0.0144(19) 0.0023(17) -0.0130(16)
C16 0.0212(18) 0.0293(17) 0.033(2) -0.0145(16) 0.0027(16) -0.0104(14)
C17 0.025(2) 0.056(3) 0.026(2) -0.013(2) -0.0011(18) 0.009(2)
C18 0.0207(18) 0.0303(17) 0.0144(16) -0.0055(13) 0.0013(13) -0.0029(14)
C19 0.031(2) 0.0232(15) 0.0181(17) -0.0083(13) -0.0035(14) -0.0047(14)
C20 0.0252(18) 0.0247(15) 0.0158(16) -0.0052(12) -0.0061(13) -0.0096(13)
C21 0.0225(17) 0.0226(15) 0.0158(16) -0.0023(12) -0.0036(13) -0.0054(12)
C22 0.0268(18) 0.0214(14) 0.0132(15) 0.0006(11) -0.0047(13) -0.0096(13)
C23 0.0249(19) 0.0321(18) 0.0137(16) -0.0029(13) 0.0002(13) -0.0132(15)
C24 0.0237(19) 0.034(2) 0.024(2) -0.0065(16) -0.0055(15) 0.0004(15)
C25 0.035(3) 0.038(2) 0.030(2) 0.0022(18) -0.012(2) 0.0043(19)
C26 0.023(2) 0.061(3) 0.033(3) -0.007(2) -0.0031(19) -0.006(2)
P1 0.0280(7) 0.0170(5) 0.0176(6) -0.0017(4) -0.0020(5) -0.0089(5)
F2 0.055(2) 0.0187(12) 0.0491(19) -0.0014(12) -0.0043(16) -0.0007(12)
F3 0.0461(18) 0.0452(17) 0.0267(14) -0.0059(12) 0.0112(13) -0.0179(14)
F4 0.053(2) 0.055(2) 0.0386(18) -0.0088(14) -0.0139(15) -0.0308(16)
_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 Br1 2.5329(5) . ?
Ru1 N1 2.130(3) . ?
Ru1 N2 2.086(3) . ?
Ru1 C18 2.206(4) . ?
Ru1 C19 2.186(4) . ?
Ru1 C20 2.208(4) . ?
Ru1 C21 2.235(4) . ?
Ru1 C22 2.222(4) . ?
Ru1 C23 2.204(4) . ?
F1 C14 1.361(5) . ?
O1 C10 1.295(4) . ?
N1 C1 1.389(4) . ?
N1 C9 1.339(4) . ?
C1 C2 1.417(5) . ?
C1 C6 1.432(5) . ?
N2 C10 1.303(4) . ?
N2 C11 1.441(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.380(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.414(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.372(5) . ?
C5 H5 0.9300 . ?
C5 C6 1.425(5) . ?
C6 C7 1.412(5) . ?
C7 H7 0.9300 . ?
C7 C8 1.377(5) . ?
C8 H8 0.9300 . ?
C8 C9 1.408(5) . ?
C9 C10 1.493(5) . ?
C11 C12 1.392(5) . ?
C11 C16 1.390(6) . ?
C12 H12 0.9300 . ?
C12 C13 1.395(6) . ?
C13 H13 0.9300 . ?
C13 C14 1.365(7) . ?
C14 C15 1.378(6) . ?
C15 H15 0.9300 . ?
C15 C16 1.402(6) . ?
C16 H16 0.9300 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C17 C18 1.503(6) . ?
C18 C19 1.408(6) . ?
C18 C23 1.433(6) . ?
C19 H19 0.9300 . ?
C19 C20 1.426(6) . ?
C20 H20 0.9300 . ?
C20 C21 1.414(5) . ?
C21 C22 1.433(6) . ?
C21 C24 1.519(6) . ?
C22 H22 0.9300 . ?
C22 C23 1.411(6) . ?
C23 H23 0.9300 . ?
C24 H24 0.9800 . ?
C24 C25 1.545(7) . ?
C24 C26 1.537(8) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
P1 F2 1.597(3) . ?
P1 F2 1.598(3) 2_655 ?
P1 F3 1.608(3) 2_655 ?
P1 F3 1.608(3) . ?
P1 F4 1.600(3) . ?
P1 F4 1.600(3) 2_655 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ru1 Br1 85.89(8) . . ?
N1 Ru1 C18 96.29(13) . . ?
N1 Ru1 C19 123.13(13) . . ?
N1 Ru1 C20 160.80(13) . . ?
N1 Ru1 C21 155.62(12) . . ?
N1 Ru1 C22 119.09(12) . . ?
N1 Ru1 C23 95.45(13) . . ?
N2 Ru1 Br1 87.49(8) . . ?
N2 Ru1 N1 76.14(11) . . ?
N2 Ru1 C18 108.91(14) . . ?
N2 Ru1 C19 89.34(13) . . ?
N2 Ru1 C20 97.55(13) . . ?
N2 Ru1 C21 127.77(13) . . ?
N2 Ru1 C22 164.42(12) . . ?
N2 Ru1 C23 145.60(14) . . ?
C18 Ru1 Br1 163.52(11) . . ?
C18 Ru1 C20 68.26(16) . . ?
C18 Ru1 C21 81.08(15) . . ?
C18 Ru1 C22 68.19(15) . . ?
C19 Ru1 Br1 149.00(12) . . ?
C19 Ru1 C18 37.40(16) . . ?
C19 Ru1 C20 37.87(15) . . ?
C19 Ru1 C21 67.80(15) . . ?
C19 Ru1 C22 79.50(15) . . ?
C19 Ru1 C23 67.15(16) . . ?
C20 Ru1 Br1 112.21(11) . . ?
C20 Ru1 C21 37.11(14) . . ?
C20 Ru1 C22 66.99(14) . . ?
C21 Ru1 Br1 90.19(11) . . ?
C22 Ru1 Br1 96.45(11) . . ?
C22 Ru1 C21 37.51(14) . . ?
C23 Ru1 Br1 125.65(11) . . ?
C23 Ru1 C18 37.93(16) . . ?
C23 Ru1 C20 79.44(15) . . ?
C23 Ru1 C21 67.57(15) . . ?
C23 Ru1 C22 37.18(16) . . ?
C1 N1 Ru1 126.5(2) . . ?
C9 N1 Ru1 114.9(2) . . ?
C9 N1 C1 118.6(3) . . ?
N1 C1 C2 121.2(3) . . ?
N1 C1 C6 120.1(3) . . ?
C2 C1 C6 118.6(3) . . ?
C10 N2 Ru1 117.9(2) . . ?
C10 N2 C11 119.7(3) . . ?
C11 N2 Ru1 121.6(2) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 C1 120.1(3) . . ?
C3 C2 H2 120.0 . . ?
C2 C3 H3 119.3 . . ?
C2 C3 C4 121.5(3) . . ?
C4 C3 H3 119.3 . . ?
C3 C4 H4 120.2 . . ?
C5 C4 C3 119.6(3) . . ?
C5 C4 H4 120.2 . . ?
C4 C5 H5 119.7 . . ?
C4 C5 C6 120.7(4) . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C1 119.4(3) . . ?
C7 C6 C1 118.9(3) . . ?
C7 C6 C5 121.7(3) . . ?
C6 C7 H7 120.2 . . ?
C8 C7 C6 119.6(3) . . ?
C8 C7 H7 120.2 . . ?
C7 C8 H8 120.6 . . ?
C7 C8 C9 118.8(3) . . ?
C9 C8 H8 120.6 . . ?
N1 C9 C8 123.6(3) . . ?
N1 C9 C10 115.0(3) . . ?
C8 C9 C10 121.4(3) . . ?
O1 C10 N2 123.3(3) . . ?
O1 C10 C9 122.0(3) . . ?
N2 C10 C9 114.5(3) . . ?
C12 C11 N2 120.9(3) . . ?
C16 C11 N2 119.0(3) . . ?
C16 C11 C12 120.1(3) . . ?
C11 C12 H12 119.8 . . ?
C11 C12 C13 120.3(4) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 120.6 . . ?
C14 C13 C12 118.8(4) . . ?
C14 C13 H13 120.6 . . ?
F1 C14 C13 119.3(4) . . ?
F1 C14 C15 118.4(4) . . ?
C13 C14 C15 122.3(4) . . ?
C14 C15 H15 120.4 . . ?
C14 C15 C16 119.3(4) . . ?
C16 C15 H15 120.4 . . ?
C11 C16 C15 119.3(4) . . ?
C11 C16 H16 120.4 . . ?
C15 C16 H16 120.4 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
C17 C18 Ru1 126.6(3) . . ?
C19 C18 Ru1 70.5(2) . . ?
C19 C18 C17 122.7(4) . . ?
C19 C18 C23 117.4(4) . . ?
C23 C18 Ru1 71.0(2) . . ?
C23 C18 C17 119.9(4) . . ?
Ru1 C19 H19 129.5 . . ?
C18 C19 Ru1 72.1(2) . . ?
C18 C19 H19 119.1 . . ?
C18 C19 C20 121.8(4) . . ?
C20 C19 Ru1 71.9(2) . . ?
C20 C19 H19 119.1 . . ?
Ru1 C20 H20 130.1 . . ?
C19 C20 Ru1 70.2(2) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 Ru1 72.5(2) . . ?
C21 C20 C19 120.5(4) . . ?
C21 C20 H20 119.7 . . ?
C20 C21 Ru1 70.4(2) . . ?
C20 C21 C22 118.3(4) . . ?
C20 C21 C24 122.7(4) . . ?
C22 C21 Ru1 70.7(2) . . ?
C22 C21 C24 119.0(4) . . ?
C24 C21 Ru1 129.9(3) . . ?
Ru1 C22 H22 130.4 . . ?
C21 C22 Ru1 71.8(2) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 Ru1 70.7(2) . . ?
C23 C22 C21 120.4(3) . . ?
C23 C22 H22 119.8 . . ?
Ru1 C23 H23 130.2 . . ?
C18 C23 Ru1 71.1(2) . . ?
C18 C23 H23 119.2 . . ?
C22 C23 Ru1 72.1(2) . . ?
C22 C23 C18 121.5(4) . . ?
C22 C23 H23 119.2 . . ?
C21 C24 H24 107.7 . . ?
C21 C24 C25 108.7(4) . . ?
C21 C24 C26 113.7(4) . . ?
C25 C24 H24 107.7 . . ?
C26 C24 H24 107.7 . . ?
C26 C24 C25 111.0(4) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
F2 P1 F2 180.0 . 2_655 ?
F2 P1 F3 90.08(18) . 2_655 ?
F2 P1 F3 89.92(18) 2_655 2_655 ?
F2 P1 F3 89.92(18) . . ?
F2 P1 F3 90.08(18) 2_655 . ?
F2 P1 F4 89.65(19) . 2_655 ?
F2 P1 F4 89.65(19) 2_655 . ?
F2 P1 F4 90.35(19) . . ?
F2 P1 F4 90.35(19) 2_655 2_655 ?
F3 P1 F3 180.0 2_655 . ?
F4 P1 F3 90.06(18) 2_655 . ?
F4 P1 F3 89.94(18) . . ?
F4 P1 F3 89.94(18) 2_655 2_655 ?
F4 P1 F3 90.06(18) . 2_655 ?
F4 P1 F4 180.0 . 2_655 ?
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 8.6(5) . . . . ?
Ru1 N1 C1 C6 -171.5(2) . . . . ?
Ru1 N1 C9 C8 174.2(3) . . . . ?
Ru1 N1 C9 C10 -7.3(4) . . . . ?
Ru1 N2 C10 O1 -173.4(3) . . . . ?
Ru1 N2 C10 C9 10.9(4) . . . . ?
Ru1 N2 C11 C12 101.3(4) . . . . ?
Ru1 N2 C11 C16 -74.8(4) . . . . ?
Ru1 C18 C19 C20 54.2(3) . . . . ?
Ru1 C18 C23 C22 -53.8(3) . . . . ?
Ru1 C19 C20 C21 54.3(3) . . . . ?
Ru1 C20 C21 C22 53.9(3) . . . . ?
Ru1 C20 C21 C24 -125.5(4) . . . . ?
Ru1 C21 C22 C23 53.3(3) . . . . ?
Ru1 C21 C24 C25 162.1(3) . . . . ?
Ru1 C21 C24 C26 -73.7(5) . . . . ?
Ru1 C22 C23 C18 53.3(3) . . . . ?
F1 C14 C15 C16 -178.7(4) . . . . ?
N1 C1 C2 C3 -176.3(3) . . . . ?
N1 C1 C6 C5 176.1(3) . . . . ?
N1 C1 C6 C7 -5.0(5) . . . . ?
N1 C9 C10 O1 -177.8(3) . . . . ?
N1 C9 C10 N2 -2.1(5) . . . . ?
C1 N1 C9 C8 -4.3(5) . . . . ?
C1 N1 C9 C10 174.2(3) . . . . ?
C1 C2 C3 C4 -1.0(6) . . . . ?
C1 C6 C7 C8 0.5(5) . . . . ?
N2 C11 C12 C13 -175.2(4) . . . . ?
N2 C11 C16 C15 175.4(4) . . . . ?
C2 C1 C6 C5 -4.0(5) . . . . ?
C2 C1 C6 C7 175.0(3) . . . . ?
C2 C3 C4 C5 -1.5(6) . . . . ?
C3 C4 C5 C6 1.2(6) . . . . ?
C4 C5 C6 C1 1.6(6) . . . . ?
C4 C5 C6 C7 -177.3(4) . . . . ?
C5 C6 C7 C8 179.4(4) . . . . ?
C6 C1 C2 C3 3.7(5) . . . . ?
C6 C7 C8 C9 2.1(6) . . . . ?
C7 C8 C9 N1 -0.2(6) . . . . ?
C7 C8 C9 C10 -178.7(3) . . . . ?
C8 C9 C10 O1 0.7(6) . . . . ?
C8 C9 C10 N2 176.5(3) . . . . ?
C9 N1 C1 C2 -173.1(3) . . . . ?
C9 N1 C1 C6 6.8(5) . . . . ?
C10 N2 C11 C12 -68.6(5) . . . . ?
C10 N2 C11 C16 115.3(4) . . . . ?
C11 N2 C10 O1 -3.1(6) . . . . ?
C11 N2 C10 C9 -178.7(3) . . . . ?
C11 C12 C13 C14 -0.2(8) . . . . ?
C12 C11 C16 C15 -0.8(7) . . . . ?
C12 C13 C14 F1 178.8(5) . . . . ?
C12 C13 C14 C15 -0.5(8) . . . . ?
C13 C14 C15 C16 0.6(8) . . . . ?
C14 C15 C16 C11 0.1(7) . . . . ?
C16 C11 C12 C13 0.9(7) . . . . ?
C17 C18 C19 Ru1 121.6(4) . . . . ?
C17 C18 C19 C20 175.9(4) . . . . ?
C17 C18 C23 Ru1 -121.9(4) . . . . ?
C17 C18 C23 C22 -175.7(4) . . . . ?
C18 C19 C20 Ru1 -54.3(3) . . . . ?
C18 C19 C20 C21 0.0(6) . . . . ?
C19 C18 C23 Ru1 54.9(3) . . . . ?
C19 C18 C23 C22 1.1(6) . . . . ?
C19 C20 C21 Ru1 -53.3(3) . . . . ?
C19 C20 C21 C22 0.6(6) . . . . ?
C19 C20 C21 C24 -178.7(4) . . . . ?
C20 C21 C22 Ru1 -53.7(3) . . . . ?
C20 C21 C22 C23 -0.4(6) . . . . ?
C20 C21 C24 C25 -106.9(5) . . . . ?
C20 C21 C24 C26 17.3(6) . . . . ?
C21 C22 C23 Ru1 -53.8(3) . . . . ?
C21 C22 C23 C18 -0.5(6) . . . . ?
C22 C21 C24 C25 73.8(5) . . . . ?
C22 C21 C24 C26 -162.0(4) . . . . ?
C23 C18 C19 Ru1 -55.1(3) . . . . ?
C23 C18 C19 C20 -0.8(6) . . . . ?
C24 C21 C22 Ru1 125.7(4) . . . . ?
C24 C21 C22 C23 179.0(4) . . . . ?
_shelx_SHELXL_version_number 2014/7
_iucr_refine_instructions_details
;
kr275_twin1_hklf4.res created by SHELXL-2014/7
TITL KR275_twin1_hklf4 in P-1 #2
REM reset to P-1 #2
CELL 0.71073 9.488456 9.827986 14.786242 72.5952 83.9351 73.979
ZERR 1 0.000419 0.000322 0.000621 0.0033 0.0035 0.0033
LATT 1
SFAC C H Br F N O P Ru
UNIT 52 49 2 8 4 2 1 2
L.S. 4
PLAN 50
BOND
MORE -1
BOND $H
CONF
fmap 2
acta 52
OMIT -1 0 0
OMIT 1 0 0
OMIT 0 -1 0
REM
REM
REM
WGHT 0.057400 4.688100
BASF 0.36365
FVAR 5.20521
RU1 8 0.311054 0.469597 0.234206 11.00000 0.01505 0.01281 =
0.01202 -0.00239 -0.00205 -0.00480
BR1 3 0.124020 0.608374 0.332272 11.00000 0.01953 0.01992 =
0.02034 -0.00785 -0.00162 -0.00333
F1 4 -0.118961 0.004602 0.270362 11.00000 0.03957 0.04028 =
0.07545 -0.01819 -0.01313 -0.02507
O1 6 0.390612 0.084333 0.460361 11.00000 0.02971 0.01503 =
0.02954 0.00583 -0.01141 -0.01066
N1 5 0.462612 0.434929 0.340381 11.00000 0.01452 0.01420 =
0.01351 -0.00341 -0.00070 -0.00547
C1 1 0.540855 0.532500 0.345926 11.00000 0.01685 0.01485 =
0.01312 -0.00429 0.00024 -0.00519
N2 5 0.288567 0.275072 0.334034 11.00000 0.01624 0.01373 =
0.01720 -0.00269 -0.00243 -0.00645
C2 1 0.511331 0.678630 0.285208 11.00000 0.02193 0.01502 =
0.01613 -0.00196 -0.00230 -0.00735
AFIX 43
H2 2 0.434727 0.712535 0.243096 11.00000 -1.20000
AFIX 0
C3 1 0.596040 0.770718 0.288453 11.00000 0.02560 0.01845 =
0.02322 -0.00396 0.00286 -0.01172
AFIX 43
H3 2 0.576507 0.865890 0.247520 11.00000 -1.20000
AFIX 0
C4 1 0.711888 0.723682 0.352602 11.00000 0.02401 0.02192 =
0.02555 -0.00598 -0.00018 -0.01248
AFIX 43
H4 2 0.769204 0.786625 0.352707 11.00000 -1.20000
AFIX 0
C5 1 0.739206 0.584644 0.414676 11.00000 0.01901 0.02572 =
0.02166 -0.00761 0.00046 -0.01115
AFIX 43
H5 2 0.814216 0.554222 0.457691 11.00000 -1.20000
AFIX 0
C6 1 0.653780 0.486308 0.413918 11.00000 0.01622 0.01772 =
0.01480 -0.00506 0.00030 -0.00655
C7 1 0.675764 0.344957 0.479649 11.00000 0.01805 0.02101 =
0.01739 -0.00437 -0.00422 -0.00577
AFIX 43
H7 2 0.748037 0.313231 0.524670 11.00000 -1.20000
AFIX 0
C8 1 0.589569 0.254298 0.476727 11.00000 0.01975 0.01685 =
0.01540 0.00039 -0.00466 -0.00589
AFIX 43
H8 2 0.600651 0.162173 0.520839 11.00000 -1.20000
AFIX 0
C9 1 0.484403 0.303608 0.405765 11.00000 0.01635 0.01305 =
0.01434 -0.00200 -0.00252 -0.00543
C10 1 0.385497 0.211942 0.400111 11.00000 0.01560 0.01215 =
0.01914 -0.00067 -0.00193 -0.00426
C11 1 0.184795 0.198824 0.322760 11.00000 0.01871 0.01357 =
0.02039 -0.00305 -0.00294 -0.00643
C12 1 0.230349 0.074058 0.290206 11.00000 0.02313 0.01852 =
0.04224 -0.01219 -0.00546 -0.00520
AFIX 43
H12 2 0.329737 0.034807 0.279991 11.00000 -1.20000
AFIX 0
C13 1 0.127654 0.007648 0.272839 11.00000 0.03366 0.02163 =
0.05162 -0.01709 -0.00822 -0.01060
AFIX 43
H13 2 0.157585 -0.075478 0.250864 11.00000 -1.20000
AFIX 0
C14 1 -0.017584 0.066890 0.288684 11.00000 0.02866 0.02595 =
0.04014 -0.00790 -0.00644 -0.01745
C15 1 -0.066042 0.189258 0.321891 11.00000 0.02061 0.03544 =
0.04159 -0.01445 0.00234 -0.01300
AFIX 43
H15 2 -0.165659 0.226646 0.332581 11.00000 -1.20000
AFIX 0
C16 1 0.036490 0.256766 0.339382 11.00000 0.02124 0.02927 =
0.03287 -0.01452 0.00266 -0.01042
AFIX 43
H16 2 0.005650 0.339379 0.361852 11.00000 -1.20000
AFIX 0
C17 1 0.631478 0.320083 0.142952 11.00000 0.02546 0.05557 =
0.02555 -0.01331 -0.00108 0.00945
AFIX 137
H17A 2 0.685084 0.367697 0.169865 11.00000 -1.50000
H17B 2 0.677719 0.307555 0.083978 11.00000 -1.50000
H17C 2 0.630479 0.225322 0.186005 11.00000 -1.50000
AFIX 0
C18 1 0.476709 0.413518 0.125739 11.00000 0.02068 0.03030 =
0.01436 -0.00555 0.00131 -0.00289
C19 1 0.358108 0.353851 0.124810 11.00000 0.03053 0.02323 =
0.01806 -0.00835 -0.00348 -0.00471
AFIX 43
H19 2 0.376333 0.253537 0.131110 11.00000 -1.20000
AFIX 0
C20 1 0.210812 0.443036 0.114472 11.00000 0.02523 0.02473 =
0.01584 -0.00523 -0.00612 -0.00964
AFIX 43
H20 2 0.134855 0.400297 0.114148 11.00000 -1.20000
AFIX 0
C21 1 0.179321 0.595942 0.104709 11.00000 0.02251 0.02258 =
0.01579 -0.00232 -0.00364 -0.00545
C22 1 0.299060 0.658572 0.104556 11.00000 0.02679 0.02136 =
0.01318 0.00064 -0.00473 -0.00958
AFIX 43
H22 2 0.280947 0.758997 0.097847 11.00000 -1.20000
AFIX 0
C23 1 0.444231 0.568899 0.114514 11.00000 0.02490 0.03214 =
0.01373 -0.00287 0.00022 -0.01323
AFIX 43
H23 2 0.520602 0.611610 0.113777 11.00000 -1.20000
AFIX 0
C24 1 0.024219 0.695434 0.095470 11.00000 0.02370 0.03440 =
0.02362 -0.00646 -0.00546 0.00044
AFIX 13
H24 2 0.014372 0.760556 0.135926 11.00000 -1.20000
AFIX 0
C25 1 0.003257 0.793185 -0.008082 11.00000 0.03515 0.03789 =
0.02996 0.00219 -0.01225 0.00434
AFIX 137
H25A 2 0.072879 0.851938 -0.024060 11.00000 -1.50000
H25B 2 -0.094419 0.856714 -0.014827 11.00000 -1.50000
H25C 2 0.018282 0.731656 -0.049719 11.00000 -1.50000
AFIX 0
C26 1 -0.095265 0.611250 0.126989 11.00000 0.02315 0.06118 =
0.03318 -0.00675 -0.00306 -0.00628
AFIX 137
H26A 2 -0.096684 0.556546 0.083239 11.00000 -1.50000
H26B 2 -0.189020 0.680155 0.128187 11.00000 -1.50000
H26C 2 -0.074719 0.544469 0.189227 11.00000 -1.50000
AFIX 0
P1 7 0.500000 0.000000 0.000000 10.50000 0.02799 0.01696 =
0.01757 -0.00172 -0.00200 -0.00889
F2 4 0.410181 0.169533 -0.026922 11.00000 0.05471 0.01871 =
0.04914 -0.00144 -0.00431 -0.00073
F3 4 0.599627 0.033241 -0.094920 11.00000 0.04612 0.04523 =
0.02671 -0.00592 0.01123 -0.01789
F4 4 0.387239 -0.036584 -0.056773 11.00000 0.05344 0.05453 =
0.03862 -0.00883 -0.01386 -0.03084
HKLF 5
REM KR275_twin1_hklf4 in P-1 #2
REM R1 = 0.0479 for 15096 Fo > 4sig(Fo) and 0.0514 for all 15986 data
REM 326 parameters refined using 0 restraints
END
WGHT 0.0569 4.7167
REM Highest difference peak 1.640, deepest hole -2.046, 1-sigma level 0.150
Q1 1 0.2356 0.4961 0.2453 11.00000 0.05 1.64
Q2 1 0.3867 0.4401 0.2329 11.00000 0.05 1.62
Q3 1 0.3242 0.5256 0.2356 11.00000 0.05 1.38
Q4 1 0.2981 0.4141 0.2275 11.00000 0.05 1.10
Q5 1 0.0500 0.6382 0.3391 11.00000 0.05 1.07
Q6 1 0.0688 0.6234 0.3603 11.00000 0.05 1.02
Q7 1 0.2018 0.5779 0.3276 11.00000 0.05 0.94
Q8 1 0.2349 0.4751 0.3314 11.00000 0.05 0.84
Q9 1 0.1127 0.5449 0.3298 11.00000 0.05 0.84
Q10 1 0.3179 0.4630 0.1850 11.00000 0.05 0.82
Q11 1 0.4332 0.3546 0.2264 11.00000 0.05 0.81
Q12 1 0.3415 0.3197 0.2515 11.00000 0.05 0.73
Q13 1 0.1252 0.6036 0.2841 11.00000 0.05 0.70
Q14 1 -0.0509 0.1216 0.3061 11.00000 0.05 0.68
Q15 1 0.2242 0.5443 0.2953 11.00000 0.05 0.68
Q16 1 0.1195 0.6804 0.3249 11.00000 0.05 0.67
Q17 1 0.0866 0.6585 0.2777 11.00000 0.05 0.67
Q18 1 0.1955 0.5887 0.2434 11.00000 0.05 0.66
Q19 1 0.1619 0.5162 0.3388 11.00000 0.05 0.66
Q20 1 0.2864 0.6258 0.2136 11.00000 0.05 0.65
Q21 1 0.0825 0.7600 0.3181 11.00000 0.05 0.63
Q22 1 0.7988 0.3584 0.5810 11.00000 0.05 0.60
Q23 1 0.1413 0.5606 0.3791 11.00000 0.05 0.59
Q24 1 0.1389 0.6401 0.3776 11.00000 0.05 0.58
Q25 1 0.4388 0.4402 0.1740 11.00000 0.05 0.58
Q26 1 0.6368 0.0370 -0.1034 11.00000 0.05 0.58
Q27 1 0.3847 0.6252 0.1054 11.00000 0.05 0.57
Q28 1 0.2465 0.4442 0.1591 11.00000 0.05 0.54
Q29 1 0.3621 0.5964 0.1234 11.00000 0.05 0.54
Q30 1 0.7153 0.6769 0.3944 11.00000 0.05 0.54
Q31 1 0.2786 0.3898 0.1178 11.00000 0.05 0.54
Q32 1 0.4387 0.4808 0.1010 11.00000 0.05 0.54
Q33 1 0.4615 0.4231 0.2006 11.00000 0.05 0.53
Q34 1 0.6280 0.5023 0.3676 11.00000 0.05 0.53
Q35 1 0.3196 0.4806 0.3439 11.00000 0.05 0.53
Q36 1 0.1630 0.4550 0.3629 11.00000 0.05 0.52
Q37 1 0.5332 0.0232 0.4308 11.00000 0.05 0.52
Q38 1 0.4495 0.4178 0.3035 11.00000 0.05 0.52
Q39 1 0.6095 0.1815 0.2095 11.00000 0.05 0.51
Q40 1 -0.0620 0.2639 0.3216 11.00000 0.05 0.50
Q41 1 0.1812 0.5352 0.0872 11.00000 0.05 0.50
Q42 1 0.4562 0.0742 0.4449 11.00000 0.05 0.50
Q43 1 0.6029 0.3206 0.4899 11.00000 0.05 0.50
Q44 1 0.3912 0.4143 0.1385 11.00000 0.05 0.50
Q45 1 0.1237 0.6200 0.4353 11.00000 0.05 0.49
Q46 1 0.0659 -0.1569 0.3176 11.00000 0.05 0.49
Q47 1 0.4618 0.4819 0.1213 11.00000 0.05 0.49
Q48 1 0.5429 0.2781 0.4307 11.00000 0.05 0.49
Q49 1 0.3984 0.5036 0.3209 11.00000 0.05 0.49
Q50 1 0.5437 0.7386 0.2741 11.00000 0.05 0.48
REM The information below was added by Olex2.
REM
REM R1 = 0.0479 for 15096 Fo > 4sig(Fo) and 0.0514 for all 15990 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 1.64, deepest hole -2.05
REM Mean Shift 0, Max Shift 0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0514
REM R1_gt = 0.0479
REM wR_ref = 0.1323
REM GOOF = 1.098
REM Shift_max = 0.001
REM Shift_mean = 0
REM Reflections_all = 15990
REM Reflections_gt = 15096
REM Parameters = n/a
REM Hole = -2.05
REM Peak = 1.64
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.6364(7)
2 0.3636(7)
# start Validation Reply Form
_vrf_PLAT430_kr275_twin1_hklf4
;
PROBLEM: Short Inter D...A Contact O1 .. O1 .. 2.42 Ang.
RESPONSE: Structure is hydrogen bridged dimer, with hydrogen bridging the amide oxygen atoms O1.
;
# end Validation Reply Form
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_kr219_twin1_hklf4
_database_code_depnum_ccdc_archive 'CCDC 1472244'
_audit_update_record
;
2016-06-30 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;
_audit_creation_date 2016-06-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C52 H47 Br2 F4 N4 O2 Ru2, F6 P'
_chemical_formula_sum 'C52 H47 Br2 F10 N4 O2 P Ru2'
_chemical_formula_weight 1342.86
_chemical_melting_point ?
_chemical_oxdiff_formula 'C52 H47 Br2 F10 N4 O2 P Ru2'
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
_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.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.6940(3)
_cell_length_b 10.1017(3)
_cell_length_c 13.7167(5)
_cell_angle_alpha 99.953(3)
_cell_angle_beta 94.128(3)
_cell_angle_gamma 102.191(2)
_cell_volume 1284.93(7)
_cell_formula_units_Z 1
_cell_measurement_reflns_used 27166
_cell_measurement_temperature 148(2)
_cell_measurement_theta_max 37.8250
_cell_measurement_theta_min 2.1070
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 2.255
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.87459
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour Red
_exptl_crystal_colour_primary Red
_exptl_crystal_density_diffrn 1.735
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Plate
_exptl_crystal_F_000 666
_exptl_crystal_size_max 0.39
_exptl_crystal_size_mid 0.18
_exptl_crystal_size_min 0.08
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents ?
_diffrn_reflns_av_unetI/netI 0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 17044
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 38.265
_diffrn_reflns_theta_min 2.343
_diffrn_ambient_temperature 148.15
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 phi 0.01 359.51 0.5000 5.0000
omega____ theta____ kappa____ phi______ frames
24.1562 30.0000 -30.0116 - 719
#__ type_ start__ end____ width___ exp.time_
2 phi -0.01 359.38 0.4998 5.0000
omega____ theta____ kappa____ phi______ frames
19.4492 28.0000 50.0148 - 719
#__ type_ start__ end____ width___ exp.time_
3 phi 0.03 359.53 0.5000 5.0000
omega____ theta____ kappa____ phi______ frames
-0.4243 -28.0000 -85.0397 - 719
#__ type_ start__ end____ width___ exp.time_
4 omega 27.37 86.87 0.5000 5.0000
omega____ theta____ kappa____ phi______ frames
- 34.0000 -125.0673 27.5573 119
#__ type_ start__ end____ width___ exp.time_
5 omega -13.69 7.31 0.5000 5.0000
omega____ theta____ kappa____ phi______ frames
- -14.0000 -55.0136 -82.4841 42
#__ type_ start__ end____ width___ exp.time_
6 omega 293.31 346.31 0.5000 5.0000
omega____ theta____ kappa____ phi______ frames
- -14.0000 -55.0134 -82.4845 106
;
_diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer'
_diffrn_measurement_method '\w and \p scans'
_diffrn_orient_matrix_UB_11 0.0119960000
_diffrn_orient_matrix_UB_12 0.0630428000
_diffrn_orient_matrix_UB_13 -0.0175827000
_diffrn_orient_matrix_UB_21 0.0056463000
_diffrn_orient_matrix_UB_22 0.0370153000
_diffrn_orient_matrix_UB_23 0.0495624000
_diffrn_orient_matrix_UB_31 0.0741613000
_diffrn_orient_matrix_UB_32 0.0039132000
_diffrn_orient_matrix_UB_33 0.0051187000
loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.7364 10850 35333
2 0.2636 10970 35333
_diffrn_oxdiff_twin_integration_method simultaneous
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed tube'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 15882
_reflns_number_total 17044
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection 'COLLECT (Nonius, 1999)'
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 1.398
_refine_diff_density_min -1.139
_refine_diff_density_rms 0.169
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.229
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 364
_refine_ls_number_reflns 17044
_refine_ls_number_restraints 4
_refine_ls_R_factor_all 0.0659
_refine_ls_R_factor_gt 0.0590
_refine_ls_restrained_S_all 1.229
_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^)+(0.0148P)^2^+6.1199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1212
_refine_ls_wR_factor_ref 0.1259
_refine_special_details
;
Reflections -1 0 1, 0 1 0, 1 0 0, -1 0 0, 0 -1 1, -1 1 0 omitted as obscured by beamstop.
Refined as a two component twin with HKLF5 refinement and BASF 0.235
;
_olex2_refinement_description
;
1. Twinned data refinement
Scales: 0.7648 0.2352
2. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
3. Restrained distances
C25B-C24B = C25A-C24A = C26B-C24B = C26A-C24A
1.52 with sigma of 0.01
4. Others
Fixed Sof: C24A(0.65) H24A(0.65) C25A(0.65) H25A(0.65) H25B(0.65) H25C(0.65)
C26A(0.65) H26A(0.65) H26B(0.65) H26C(0.65) C26B(0.35) H26D(0.35) H26E(0.35)
H26F(0.35) C25B(0.35) H25D(0.35) H25E(0.35) H25F(0.35) C24B(0.35) H24B(0.35)
5.a Ternary CH refined with riding coordinates:
C24A(H24A), C24B(H24B)
5.b Aromatic/amide H refined with riding coordinates:
C3(H3), C15(H15), C2(H2), C8(H8), C5(H5), C23(H23), C12(H12), C22(H22),
C4(H4), C13(H13), C7(H7), C20(H20), C19(H19)
5.c Idealised Me refined as rotating group:
C17(H17A,H17B,H17C), C25A(H25A,H25B,H25C), C26A(H26A,H26B,H26C), C26B(H26D,
H26E,H26F), C25B(H25D,H25E,H25F)
;
_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 0.29239(3) 0.39472(3) 0.25159(2) 0.01338(5) Uani 1 1 d . . . . .
Br1 Br 0.42099(4) 0.53752(4) 0.13623(3) 0.02016(8) Uani 1 1 d . . . . .
P1 P 0.5000 0.0000 0.5000 0.0698(10) Uani 1 2 d S T P . .
F2 F 0.2048(3) -0.0317(3) 0.1934(2) 0.0274(5) Uani 1 1 d . . . . .
N2 N 0.1072(3) 0.3954(3) 0.1593(2) 0.0150(5) Uani 1 1 d . . . . .
O1 O 0.1222(3) 0.0689(3) 0.0138(2) 0.0225(6) Uani 1 1 d . . . . .
N1 N 0.2736(3) 0.2239(3) 0.1388(2) 0.0164(5) Uani 1 1 d . . . . .
F1 F 0.6586(4) -0.1094(4) 0.1486(4) 0.0666(13) Uani 1 1 d . . . . .
C11 C 0.3713(4) 0.1363(4) 0.1364(3) 0.0172(6) Uani 1 1 d . . . . .
C3 C 0.0068(5) 0.7245(5) 0.2457(4) 0.0273(8) Uani 1 1 d . . . . .
H3 H 0.0422 0.8075 0.2902 0.033 Uiso 1 1 calc R . . . .
C15 C 0.4301(5) -0.0759(5) 0.1713(4) 0.0300(9) Uani 1 1 d . . . . .
H15 H 0.4042 -0.1606 0.1908 0.036 Uiso 1 1 calc R . . . .
C2 C 0.0863(4) 0.6260(4) 0.2342(3) 0.0216(7) Uani 1 1 d . . . . .
H2 H 0.1754 0.6431 0.2700 0.026 Uiso 1 1 calc R . . . .
C1 C 0.0317(4) 0.4982(4) 0.1673(3) 0.0170(6) Uani 1 1 d . . . . .
C9 C 0.0610(4) 0.2830(4) 0.0874(3) 0.0159(6) Uani 1 1 d . . . . .
C10 C 0.1540(4) 0.1828(4) 0.0782(3) 0.0167(6) Uani 1 1 d . . . . .
C16 C 0.3366(4) 0.0094(4) 0.1661(3) 0.0207(7) Uani 1 1 d . . . . .
C8 C -0.0638(4) 0.2615(4) 0.0212(3) 0.0214(7) Uani 1 1 d . . . . .
H8 H -0.0901 0.1837 -0.0294 0.026 Uiso 1 1 calc R . . . .
C5 C -0.1796(5) 0.5828(5) 0.1223(4) 0.0293(9) Uani 1 1 d . . . . .
H5 H -0.2672 0.5701 0.0853 0.035 Uiso 1 1 calc R . . . .
C23 C 0.3611(5) 0.5535(5) 0.3899(3) 0.0284(9) Uani 1 1 d . . . . .
H23 H 0.3800 0.6493 0.3997 0.034 Uiso 1 1 calc R . . . .
C12 C 0.5089(4) 0.1787(4) 0.1111(4) 0.0262(8) Uani 1 1 d . . . . .
H12 H 0.5355 0.2632 0.0915 0.031 Uiso 1 1 calc R . . . .
C22 C 0.2226(5) 0.4778(5) 0.3940(3) 0.0253(8) Uani 1 1 d . . . . .
H22 H 0.1513 0.5254 0.4060 0.030 Uiso 1 1 calc R . . . .
C4 C -0.1275(5) 0.7012(5) 0.1910(4) 0.0329(10) Uani 1 1 d . . . . .
H4 H -0.1813 0.7674 0.2019 0.039 Uiso 1 1 calc R . . . .
C6 C -0.1001(4) 0.4781(4) 0.1069(3) 0.0216(7) Uani 1 1 d . . . . .
C21 C 0.1874(4) 0.3305(5) 0.3802(3) 0.0240(8) Uani 1 1 d . . . . .
C13 C 0.6060(5) 0.0960(5) 0.1152(5) 0.0376(12) Uani 1 1 d . . . . .
H13 H 0.6970 0.1239 0.0977 0.045 Uiso 1 1 calc R . . . .
C7 C -0.1455(4) 0.3577(5) 0.0328(3) 0.0240(8) Uani 1 1 d . . . . .
H7 H -0.2303 0.3435 -0.0079 0.029 Uiso 1 1 calc R . . . .
C20 C 0.2996(5) 0.2633(5) 0.3619(3) 0.0262(8) Uani 1 1 d . . . . .
H20 H 0.2810 0.1675 0.3516 0.031 Uiso 1 1 calc R . . . .
C14 C 0.5650(5) -0.0278(6) 0.1455(5) 0.0382(12) Uani 1 1 d . . . . .
F4 F 0.4166(9) 0.1097(6) 0.5407(6) 0.121(3) Uani 1 1 d . . . . .
C19 C 0.4401(5) 0.3389(5) 0.3589(3) 0.0284(9) Uani 1 1 d . . . . .
H19 H 0.5121 0.2918 0.3489 0.034 Uiso 1 1 calc R . . . .
C18 C 0.4724(5) 0.4836(5) 0.3708(3) 0.0304(9) Uani 1 1 d . . . . .
C24A C 0.0307(13) 0.2676(9) 0.3870(7) 0.0290(19) Uani 0.65 1 d D . . A 1
H24A H -0.0267 0.3286 0.3655 0.035 Uiso 0.65 1 calc R . . A 1
F5 F 0.5703(8) 0.1006(6) 0.4317(5) 0.112(2) Uani 1 1 d . . . . .
F3 F 0.6248(8) 0.0708(8) 0.5860(5) 0.127(3) Uani 1 1 d . . . . .
C17 C 0.6204(6) 0.5634(8) 0.3611(4) 0.0549(19) Uani 1 1 d . . . . .
H17A H 0.6674 0.5049 0.3193 0.082 Uiso 1 1 calc GR . . . .
H17B H 0.6737 0.5938 0.4258 0.082 Uiso 1 1 calc GR . . . .
H17C H 0.6137 0.6421 0.3321 0.082 Uiso 1 1 calc GR . . . .
C25A C 0.0133(11) 0.2614(14) 0.4963(7) 0.051(3) Uani 0.65 1 d D . . A 1
H25A H 0.0604 0.1941 0.5163 0.077 Uiso 0.65 1 calc GR . . A 1
H25B H -0.0859 0.2359 0.5041 0.077 Uiso 0.65 1 calc GR . . A 1
H25C H 0.0544 0.3503 0.5371 0.077 Uiso 0.65 1 calc GR . . A 1
C26A C -0.0202(10) 0.1256(10) 0.3216(8) 0.055(3) Uani 0.65 1 d D . . A 1
H26A H -0.0057 0.1313 0.2538 0.082 Uiso 0.65 1 calc GR . . A 1
H26B H -0.1195 0.0920 0.3258 0.082 Uiso 0.65 1 calc GR . . A 1
H26C H 0.0323 0.0636 0.3438 0.082 Uiso 0.65 1 calc GR . . A 1
C26B C -0.0803(13) 0.2813(19) 0.3542(13) 0.047(5) Uani 0.35 1 d D . . A 2
H26D H -0.0841 0.3589 0.4046 0.071 Uiso 0.35 1 calc GR . . A 2
H26E H -0.1655 0.2108 0.3494 0.071 Uiso 0.35 1 calc GR . . A 2
H26F H -0.0721 0.3100 0.2913 0.071 Uiso 0.35 1 calc GR . . A 2
C25B C 0.045(2) 0.186(3) 0.4846(13) 0.054(6) Uani 0.35 1 d D . . A 2
H25D H 0.0949 0.1142 0.4877 0.081 Uiso 0.35 1 calc GR . . A 2
H25E H -0.0517 0.1548 0.4965 0.081 Uiso 0.35 1 calc GR . . A 2
H25F H 0.0899 0.2658 0.5345 0.081 Uiso 0.35 1 calc GR . . A 2
C24B C 0.0485(17) 0.224(2) 0.3819(12) 0.028(4) Uani 0.35 1 d D . . A 2
H24B H 0.0469 0.1410 0.3327 0.034 Uiso 0.35 1 calc R . . A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.01383(10) 0.01231(10) 0.01317(10) 0.00175(9) -0.00148(9) 0.00272(8)
Br1 0.01766(16) 0.02090(18) 0.02292(18) 0.00912(14) 0.00071(13) 0.00311(13)
P1 0.137(3) 0.0342(12) 0.0414(13) 0.0075(10) -0.0193(16) 0.0355(15)
F2 0.0205(11) 0.0232(12) 0.0386(15) 0.0097(11) 0.0073(10) 0.0011(9)
N2 0.0140(11) 0.0164(13) 0.0145(13) 0.0033(10) -0.0006(9) 0.0037(10)
O1 0.0184(12) 0.0193(13) 0.0242(14) -0.0052(10) -0.0025(10) 0.0009(10)
N1 0.0138(11) 0.0152(13) 0.0192(13) 0.0022(11) 0.0003(10) 0.0028(10)
F1 0.0417(19) 0.060(2) 0.126(4) 0.051(3) 0.031(2) 0.0403(19)
C11 0.0156(13) 0.0164(14) 0.0187(15) 0.0004(12) 0.0004(11) 0.0047(11)
C3 0.037(2) 0.0232(18) 0.030(2) 0.0117(17) 0.0145(18) 0.0155(16)
C15 0.031(2) 0.0227(19) 0.042(3) 0.0112(18) 0.0071(19) 0.0127(17)
C2 0.0232(16) 0.0197(16) 0.0249(19) 0.0061(14) 0.0066(14) 0.0087(13)
C1 0.0161(14) 0.0179(15) 0.0205(16) 0.0082(12) 0.0046(12) 0.0067(12)
C9 0.0125(12) 0.0182(15) 0.0164(14) 0.0051(12) 0.0003(11) 0.0014(11)
C10 0.0146(13) 0.0171(15) 0.0168(15) 0.0014(12) 0.0007(11) 0.0020(11)
C16 0.0182(15) 0.0160(15) 0.0277(19) 0.0055(13) 0.0029(13) 0.0023(12)
C8 0.0156(14) 0.0246(18) 0.0211(17) 0.0053(14) -0.0040(12) -0.0001(13)
C5 0.0205(17) 0.036(2) 0.042(3) 0.022(2) 0.0088(16) 0.0161(16)
C23 0.042(2) 0.0193(18) 0.0154(16) -0.0031(13) -0.0050(16) -0.0028(16)
C12 0.0190(16) 0.0210(18) 0.041(2) 0.0106(17) 0.0079(16) 0.0059(14)
C22 0.036(2) 0.0250(19) 0.0157(16) 0.0017(14) 0.0052(15) 0.0109(16)
C4 0.034(2) 0.033(2) 0.045(3) 0.021(2) 0.016(2) 0.0220(19)
C6 0.0157(14) 0.0279(19) 0.0271(19) 0.0157(15) 0.0053(13) 0.0083(13)
C21 0.0247(17) 0.030(2) 0.0161(16) 0.0065(14) 0.0019(13) 0.0011(15)
C13 0.0192(18) 0.032(2) 0.068(4) 0.020(2) 0.011(2) 0.0099(17)
C7 0.0136(14) 0.031(2) 0.029(2) 0.0151(16) -0.0029(13) 0.0032(13)
C20 0.039(2) 0.0217(18) 0.0178(16) 0.0067(14) -0.0032(16) 0.0063(16)
C14 0.031(2) 0.036(3) 0.060(4) 0.021(2) 0.012(2) 0.024(2)
F4 0.177(7) 0.064(4) 0.137(6) 0.013(4) 0.028(5) 0.062(4)
C19 0.0287(19) 0.043(3) 0.0185(18) 0.0090(17) -0.0015(15) 0.0176(18)
C18 0.0253(18) 0.043(3) 0.0170(17) 0.0081(17) -0.0065(14) -0.0044(17)
C24A 0.028(4) 0.032(5) 0.025(4) 0.001(3) 0.003(3) 0.006(4)
F5 0.174(7) 0.084(4) 0.099(5) 0.060(4) 0.010(4) 0.044(4)
F3 0.159(7) 0.125(6) 0.079(4) 0.013(4) -0.042(4) 0.015(5)
C17 0.028(2) 0.091(5) 0.030(3) 0.016(3) -0.011(2) -0.022(3)
C25A 0.038(5) 0.068(7) 0.039(5) 0.006(5) 0.018(4) -0.010(5)
C26A 0.040(4) 0.059(6) 0.045(5) -0.012(4) 0.014(4) -0.018(4)
C26B 0.016(5) 0.076(12) 0.049(9) 0.036(9) -0.004(5) -0.009(6)
C25B 0.057(12) 0.071(15) 0.033(9) 0.034(10) 0.010(8) -0.010(11)
C24B 0.022(7) 0.033(9) 0.026(7) 0.006(6) 0.012(5) -0.005(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
Ru1 Br1 2.5402(5) . ?
Ru1 N2 2.123(3) . ?
Ru1 N1 2.076(3) . ?
Ru1 C23 2.220(4) . ?
Ru1 C22 2.200(4) . ?
Ru1 C21 2.224(4) . ?
Ru1 C20 2.185(4) . ?
Ru1 C19 2.204(4) . ?
Ru1 C18 2.224(4) . ?
P1 F4 1.557(6) 2_656 ?
P1 F4 1.557(6) . ?
P1 F5 1.582(6) 2_656 ?
P1 F5 1.582(6) . ?
P1 F3 1.583(6) 2_656 ?
P1 F3 1.583(6) . ?
F2 C16 1.358(5) . ?
N2 C1 1.386(5) . ?
N2 C9 1.341(5) . ?
O1 C10 1.289(4) . ?
N1 C11 1.425(5) . ?
N1 C10 1.321(5) . ?
F1 C14 1.351(5) . ?
C11 C16 1.393(5) . ?
C11 C12 1.399(5) . ?
C3 H3 0.9300 . ?
C3 C2 1.377(5) . ?
C3 C4 1.407(7) . ?
C15 H15 0.9300 . ?
C15 C16 1.382(6) . ?
C15 C14 1.389(7) . ?
C2 H2 0.9300 . ?
C2 C1 1.421(6) . ?
C1 C6 1.429(5) . ?
C9 C10 1.487(5) . ?
C9 C8 1.414(5) . ?
C8 H8 0.9300 . ?
C8 C7 1.373(6) . ?
C5 H5 0.9300 . ?
C5 C4 1.364(8) . ?
C5 C6 1.431(6) . ?
C23 H23 0.9300 . ?
C23 C22 1.408(7) . ?
C23 C18 1.425(7) . ?
C12 H12 0.9300 . ?
C12 C13 1.389(6) . ?
C22 H22 0.9300 . ?
C22 C21 1.431(6) . ?
C4 H4 0.9300 . ?
C6 C7 1.409(6) . ?
C21 C20 1.413(7) . ?
C21 C24A 1.534(12) . ?
C21 C24B 1.538(19) . ?
C13 H13 0.9300 . ?
C13 C14 1.375(7) . ?
C7 H7 0.9300 . ?
C20 H20 0.9300 . ?
C20 C19 1.421(7) . ?
C19 H19 0.9300 . ?
C19 C18 1.406(7) . ?
C18 C17 1.517(7) . ?
C24A H24A 0.9800 . ?
C24A C25A 1.532(9) . ?
C24A C26A 1.516(9) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C25A H25A 0.9600 . ?
C25A H25B 0.9600 . ?
C25A H25C 0.9600 . ?
C26A H26A 0.9600 . ?
C26A H26B 0.9600 . ?
C26A H26C 0.9600 . ?
C26B H26D 0.9600 . ?
C26B H26E 0.9600 . ?
C26B H26F 0.9600 . ?
C26B C24B 1.532(11) . ?
C25B H25D 0.9600 . ?
C25B H25E 0.9600 . ?
C25B H25F 0.9600 . ?
C25B C24B 1.524(11) . ?
C24B H24B 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
N2 Ru1 Br1 84.18(8) . . ?
N2 Ru1 C23 119.55(16) . . ?
N2 Ru1 C22 96.90(15) . . ?
N2 Ru1 C21 98.09(14) . . ?
N2 Ru1 C20 124.74(15) . . ?
N2 Ru1 C19 162.30(16) . . ?
N2 Ru1 C18 155.45(17) . . ?
N1 Ru1 Br1 87.02(9) . . ?
N1 Ru1 N2 76.51(12) . . ?
N1 Ru1 C23 163.81(16) . . ?
N1 Ru1 C22 146.42(15) . . ?
N1 Ru1 C21 109.73(15) . . ?
N1 Ru1 C20 89.57(14) . . ?
N1 Ru1 C19 97.53(16) . . ?
N1 Ru1 C18 127.08(17) . . ?
C23 Ru1 Br1 96.24(12) . . ?
C23 Ru1 C21 68.08(17) . . ?
C23 Ru1 C18 37.40(19) . . ?
C22 Ru1 Br1 125.52(12) . . ?
C22 Ru1 C23 37.13(18) . . ?
C22 Ru1 C21 37.73(16) . . ?
C22 Ru1 C19 78.75(17) . . ?
C22 Ru1 C18 67.40(18) . . ?
C21 Ru1 Br1 163.19(12) . . ?
C21 Ru1 C18 81.08(16) . . ?
C20 Ru1 Br1 149.10(13) . . ?
C20 Ru1 C23 79.48(17) . . ?
C20 Ru1 C22 66.92(17) . . ?
C20 Ru1 C21 37.37(17) . . ?
C20 Ru1 C19 37.78(18) . . ?
C20 Ru1 C18 67.97(17) . . ?
C19 Ru1 Br1 112.42(13) . . ?
C19 Ru1 C23 66.55(18) . . ?
C19 Ru1 C21 67.90(17) . . ?
C19 Ru1 C18 37.02(19) . . ?
C18 Ru1 Br1 89.96(12) . . ?
F4 P1 F4 180.0(5) 2_656 . ?
F4 P1 F5 88.4(4) 2_656 2_656 ?
F4 P1 F5 91.6(4) 2_656 . ?
F4 P1 F5 91.6(4) . 2_656 ?
F4 P1 F5 88.4(4) . . ?
F4 P1 F3 89.1(4) 2_656 2_656 ?
F4 P1 F3 89.2(4) . . ?
F4 P1 F3 90.8(4) 2_656 . ?
F4 P1 F3 90.9(4) . 2_656 ?
F5 P1 F5 180.0 2_656 . ?
F5 P1 F3 89.6(4) . . ?
F5 P1 F3 90.4(4) . 2_656 ?
F5 P1 F3 89.6(4) 2_656 2_656 ?
F5 P1 F3 90.4(4) 2_656 . ?
F3 P1 F3 180.0 2_656 . ?
C1 N2 Ru1 126.5(2) . . ?
C9 N2 Ru1 114.9(2) . . ?
C9 N2 C1 118.5(3) . . ?
C11 N1 Ru1 122.2(2) . . ?
C10 N1 Ru1 117.7(2) . . ?
C10 N1 C11 119.0(3) . . ?
C16 C11 N1 121.0(3) . . ?
C16 C11 C12 117.6(3) . . ?
C12 C11 N1 121.3(3) . . ?
C2 C3 H3 119.6 . . ?
C2 C3 C4 120.9(4) . . ?
C4 C3 H3 119.6 . . ?
C16 C15 H15 122.0 . . ?
C16 C15 C14 116.1(4) . . ?
C14 C15 H15 122.0 . . ?
C3 C2 H2 120.1 . . ?
C3 C2 C1 119.8(4) . . ?
C1 C2 H2 120.1 . . ?
N2 C1 C2 120.3(3) . . ?
N2 C1 C6 120.4(4) . . ?
C2 C1 C6 119.4(3) . . ?
N2 C9 C10 115.3(3) . . ?
N2 C9 C8 123.4(3) . . ?
C8 C9 C10 121.3(3) . . ?
O1 C10 N1 123.5(3) . . ?
O1 C10 C9 122.4(3) . . ?
N1 C10 C9 114.1(3) . . ?
F2 C16 C11 118.3(3) . . ?
F2 C16 C15 118.1(4) . . ?
C15 C16 C11 123.6(4) . . ?
C9 C8 H8 120.6 . . ?
C7 C8 C9 118.8(4) . . ?
C7 C8 H8 120.6 . . ?
C4 C5 H5 119.8 . . ?
C4 C5 C6 120.3(4) . . ?
C6 C5 H5 119.8 . . ?
Ru1 C23 H23 130.6 . . ?
C22 C23 Ru1 70.6(2) . . ?
C22 C23 H23 119.9 . . ?
C22 C23 C18 120.2(4) . . ?
C18 C23 Ru1 71.4(2) . . ?
C18 C23 H23 119.9 . . ?
C11 C12 H12 119.6 . . ?
C13 C12 C11 120.7(4) . . ?
C13 C12 H12 119.6 . . ?
Ru1 C22 H22 129.6 . . ?
C23 C22 Ru1 72.2(2) . . ?
C23 C22 H22 118.8 . . ?
C23 C22 C21 122.4(4) . . ?
C21 C22 Ru1 72.0(2) . . ?
C21 C22 H22 118.8 . . ?
C3 C4 H4 119.6 . . ?
C5 C4 C3 120.8(4) . . ?
C5 C4 H4 119.6 . . ?
C1 C6 C5 118.6(4) . . ?
C7 C6 C1 119.0(4) . . ?
C7 C6 C5 122.4(4) . . ?
C22 C21 Ru1 70.2(2) . . ?
C22 C21 C24A 114.5(5) . . ?
C22 C21 C24B 133.1(7) . . ?
C20 C21 Ru1 69.8(2) . . ?
C20 C21 C22 116.5(4) . . ?
C20 C21 C24A 129.1(5) . . ?
C20 C21 C24B 110.4(7) . . ?
C24A C21 Ru1 129.7(4) . . ?
C24B C21 Ru1 129.9(6) . . ?
C12 C13 H13 120.6 . . ?
C14 C13 C12 118.8(4) . . ?
C14 C13 H13 120.6 . . ?
C8 C7 C6 119.6(3) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
Ru1 C20 H20 128.4 . . ?
C21 C20 Ru1 72.8(2) . . ?
C21 C20 H20 119.3 . . ?
C21 C20 C19 121.5(4) . . ?
C19 C20 Ru1 71.8(2) . . ?
C19 C20 H20 119.3 . . ?
F1 C14 C15 117.6(5) . . ?
F1 C14 C13 119.1(5) . . ?
C13 C14 C15 123.3(4) . . ?
Ru1 C19 H19 130.8 . . ?
C20 C19 Ru1 70.4(2) . . ?
C20 C19 H19 119.3 . . ?
C18 C19 Ru1 72.3(2) . . ?
C18 C19 C20 121.3(4) . . ?
C18 C19 H19 119.3 . . ?
C23 C18 Ru1 71.2(2) . . ?
C23 C18 C17 120.6(5) . . ?
C19 C18 Ru1 70.7(2) . . ?
C19 C18 C23 118.1(4) . . ?
C19 C18 C17 121.3(5) . . ?
C17 C18 Ru1 128.1(3) . . ?
C21 C24A H24A 108.6 . . ?
C25A C24A C21 107.9(7) . . ?
C25A C24A H24A 108.6 . . ?
C26A C24A C21 112.3(7) . . ?
C26A C24A H24A 108.6 . . ?
C26A C24A C25A 110.8(9) . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C24A C25A H25A 109.5 . . ?
C24A C25A H25B 109.5 . . ?
C24A C25A H25C 109.5 . . ?
H25A C25A H25B 109.5 . . ?
H25A C25A H25C 109.5 . . ?
H25B C25A H25C 109.5 . . ?
C24A C26A H26A 109.5 . . ?
C24A C26A H26B 109.5 . . ?
C24A C26A H26C 109.5 . . ?
H26A C26A H26B 109.5 . . ?
H26A C26A H26C 109.5 . . ?
H26B C26A H26C 109.5 . . ?
H26D C26B H26E 109.5 . . ?
H26D C26B H26F 109.5 . . ?
H26E C26B H26F 109.5 . . ?
C24B C26B H26D 109.5 . . ?
C24B C26B H26E 109.5 . . ?
C24B C26B H26F 109.5 . . ?
H25D C25B H25E 109.5 . . ?
H25D C25B H25F 109.5 . . ?
H25E C25B H25F 109.5 . . ?
C24B C25B H25D 109.5 . . ?
C24B C25B H25E 109.5 . . ?
C24B C25B H25F 109.5 . . ?
C21 C24B H24B 108.5 . . ?
C26B C24B C21 110.6(12) . . ?
C26B C24B H24B 108.5 . . ?
C25B C24B C21 109.2(13) . . ?
C25B C24B C26B 111.4(15) . . ?
C25B C24B H24B 108.5 . . ?
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 N2 C1 C2 8.4(5) . . . . ?
Ru1 N2 C1 C6 -173.1(3) . . . . ?
Ru1 N2 C9 C10 -5.4(4) . . . . ?
Ru1 N2 C9 C8 177.2(3) . . . . ?
Ru1 N1 C11 C16 101.6(4) . . . . ?
Ru1 N1 C11 C12 -73.6(5) . . . . ?
Ru1 N1 C10 O1 -170.9(3) . . . . ?
Ru1 N1 C10 C9 11.9(4) . . . . ?
Ru1 C23 C22 C21 54.0(4) . . . . ?
Ru1 C23 C18 C19 -54.7(4) . . . . ?
Ru1 C23 C18 C17 123.7(4) . . . . ?
Ru1 C22 C21 C20 54.0(3) . . . . ?
Ru1 C22 C21 C24A -125.6(5) . . . . ?
Ru1 C22 C21 C24B -126.6(9) . . . . ?
Ru1 C21 C20 C19 55.1(4) . . . . ?
Ru1 C21 C24A C25A -172.4(6) . . . . ?
Ru1 C21 C24A C26A 65.1(10) . . . . ?
Ru1 C21 C24B C26B -74.0(14) . . . . ?
Ru1 C21 C24B C25B 163.1(12) . . . . ?
Ru1 C20 C19 C18 53.4(4) . . . . ?
Ru1 C19 C18 C23 54.9(3) . . . . ?
Ru1 C19 C18 C17 -123.5(4) . . . . ?
N2 C1 C6 C5 175.7(4) . . . . ?
N2 C1 C6 C7 -5.7(5) . . . . ?
N2 C9 C10 O1 178.7(3) . . . . ?
N2 C9 C10 N1 -4.0(5) . . . . ?
N2 C9 C8 C7 -2.5(6) . . . . ?
N1 C11 C16 F2 2.9(6) . . . . ?
N1 C11 C16 C15 -175.8(4) . . . . ?
N1 C11 C12 C13 175.9(5) . . . . ?
C11 N1 C10 O1 -2.6(6) . . . . ?
C11 N1 C10 C9 -179.9(3) . . . . ?
C11 C12 C13 C14 -0.7(9) . . . . ?
C3 C2 C1 N2 -176.4(4) . . . . ?
C3 C2 C1 C6 5.1(6) . . . . ?
C2 C3 C4 C5 -2.7(7) . . . . ?
C2 C1 C6 C5 -5.7(6) . . . . ?
C2 C1 C6 C7 172.8(4) . . . . ?
C1 N2 C9 C10 175.2(3) . . . . ?
C1 N2 C9 C8 -2.2(5) . . . . ?
C1 C6 C7 C8 1.0(6) . . . . ?
C9 N2 C1 C2 -172.2(3) . . . . ?
C9 N2 C1 C6 6.3(5) . . . . ?
C9 C8 C7 C6 3.0(6) . . . . ?
C10 N1 C11 C16 -66.1(5) . . . . ?
C10 N1 C11 C12 118.6(4) . . . . ?
C10 C9 C8 C7 -179.8(4) . . . . ?
C16 C11 C12 C13 0.5(7) . . . . ?
C16 C15 C14 F1 -179.3(5) . . . . ?
C16 C15 C14 C13 -0.8(9) . . . . ?
C8 C9 C10 O1 -3.8(6) . . . . ?
C8 C9 C10 N1 173.5(3) . . . . ?
C5 C6 C7 C8 179.4(4) . . . . ?
C23 C22 C21 Ru1 -54.1(4) . . . . ?
C23 C22 C21 C20 -0.1(6) . . . . ?
C23 C22 C21 C24A -179.7(5) . . . . ?
C23 C22 C21 C24B 179.3(9) . . . . ?
C12 C11 C16 F2 178.3(4) . . . . ?
C12 C11 C16 C15 -0.4(7) . . . . ?
C12 C13 C14 F1 179.3(6) . . . . ?
C12 C13 C14 C15 0.9(10) . . . . ?
C22 C23 C18 Ru1 53.2(4) . . . . ?
C22 C23 C18 C19 -1.5(6) . . . . ?
C22 C23 C18 C17 176.9(4) . . . . ?
C22 C21 C20 Ru1 -54.2(3) . . . . ?
C22 C21 C20 C19 0.9(6) . . . . ?
C22 C21 C24A C25A -88.5(8) . . . . ?
C22 C21 C24A C26A 149.1(7) . . . . ?
C22 C21 C24B C26B 26.3(17) . . . . ?
C22 C21 C24B C25B -96.6(15) . . . . ?
C4 C3 C2 C1 -0.9(6) . . . . ?
C4 C5 C6 C1 2.2(6) . . . . ?
C4 C5 C6 C7 -176.2(4) . . . . ?
C6 C5 C4 C3 2.0(7) . . . . ?
C21 C20 C19 Ru1 -55.5(4) . . . . ?
C21 C20 C19 C18 -2.1(6) . . . . ?
C20 C21 C24A C25A 92.0(8) . . . . ?
C20 C21 C24A C26A -30.5(11) . . . . ?
C20 C21 C24B C26B -154.3(11) . . . . ?
C20 C21 C24B C25B 82.8(15) . . . . ?
C20 C19 C18 Ru1 -52.6(4) . . . . ?
C20 C19 C18 C23 2.3(6) . . . . ?
C20 C19 C18 C17 -176.1(4) . . . . ?
C14 C15 C16 F2 -178.2(5) . . . . ?
C14 C15 C16 C11 0.6(7) . . . . ?
C18 C23 C22 Ru1 -53.5(4) . . . . ?
C18 C23 C22 C21 0.5(6) . . . . ?
C24A C21 C20 Ru1 125.4(6) . . . . ?
C24A C21 C20 C19 -179.5(6) . . . . ?
C24B C21 C20 Ru1 126.3(7) . . . . ?
C24B C21 C20 C19 -178.6(7) . . . . ?
_shelx_SHELXL_version_number 2014/7
_iucr_refine_instructions_details
;
kr219_twin1_hklf4.res created by SHELXL-2014/7
TITL kr219_twin1_hklf4_a.res in P-1
REM Old TITL kr219_twin1_hklf4 in P-1 #2
REM SHELXT solution in P-1
REM R1 0.112, Rweak 0.011, Alpha 0.065, Orientation as input
REM Formula found by SHELXT: C48 N7 O4 F12 Br2 Ru2
CELL 0.71073 9.694 10.1017 13.7167 99.953 94.128 102.191
ZERR 1 0.0003 0.0003 0.0005 0.003 0.003 0.002
LATT 1
SFAC C H N O F P Br Ru
UNIT 52 47 4 2 10 1 2 2
DFIX 1.52 0.01 C25B C24B C25A C24A C26B C24B C26A C24A
L.S. 10
PLAN 20
BOND $H
LIST 4
MORE -1
CONF
fmap 2
acta 52
OMIT -1 0 1
OMIT 0 1 0
OMIT 1 0 0
OMIT -1 0 0
OMIT 0 -1 1
OMIT -1 1 0
REM
REM
REM
WGHT 0.014800 6.119900
BASF 0.23515
FVAR 4.25979
RU1 8 0.292393 0.394723 0.251590 11.00000 0.01383 0.01231 =
0.01317 0.00175 -0.00148 0.00272
BR1 7 0.420990 0.537519 0.136226 11.00000 0.01766 0.02090 =
0.02292 0.00912 0.00071 0.00311
P1 6 0.500000 0.000000 0.500000 10.50000 0.13656 0.03422 =
0.04141 0.00745 -0.01929 0.03548
F2 5 0.204767 -0.031748 0.193363 11.00000 0.02051 0.02324 =
0.03862 0.00966 0.00729 0.00106
N2 3 0.107218 0.395404 0.159300 11.00000 0.01405 0.01643 =
0.01452 0.00330 -0.00061 0.00367
O1 4 0.122187 0.068874 0.013781 11.00000 0.01839 0.01934 =
0.02416 -0.00524 -0.00253 0.00090
N1 3 0.273600 0.223926 0.138788 11.00000 0.01379 0.01522 =
0.01924 0.00225 0.00033 0.00278
F1 5 0.658563 -0.109428 0.148641 11.00000 0.04166 0.06048 =
0.12605 0.05057 0.03120 0.04030
C11 1 0.371307 0.136281 0.136382 11.00000 0.01557 0.01642 =
0.01867 0.00042 0.00035 0.00473
C3 1 0.006759 0.724487 0.245699 11.00000 0.03664 0.02320 =
0.03006 0.01168 0.01448 0.01548
AFIX 43
H3 2 0.042232 0.807480 0.290206 11.00000 -1.20000
AFIX 0
C15 1 0.430103 -0.075938 0.171288 11.00000 0.03089 0.02265 =
0.04170 0.01115 0.00710 0.01275
AFIX 43
H15 2 0.404155 -0.160607 0.190841 11.00000 -1.20000
AFIX 0
C2 1 0.086289 0.625998 0.234174 11.00000 0.02316 0.01975 =
0.02493 0.00612 0.00662 0.00868
AFIX 43
H2 2 0.175439 0.643056 0.270014 11.00000 -1.20000
AFIX 0
C1 1 0.031691 0.498225 0.167343 11.00000 0.01605 0.01786 =
0.02050 0.00815 0.00458 0.00666
C9 1 0.060967 0.282970 0.087367 11.00000 0.01252 0.01823 =
0.01637 0.00510 0.00035 0.00138
C10 1 0.153995 0.182810 0.078239 11.00000 0.01462 0.01707 =
0.01675 0.00143 0.00066 0.00205
C16 1 0.336649 0.009434 0.166145 11.00000 0.01821 0.01598 =
0.02768 0.00546 0.00286 0.00231
C8 1 -0.063825 0.261522 0.021171 11.00000 0.01562 0.02464 =
0.02114 0.00529 -0.00398 -0.00013
AFIX 43
H8 2 -0.090135 0.183704 -0.029358 11.00000 -1.20000
AFIX 0
C5 1 -0.179570 0.582815 0.122287 11.00000 0.02054 0.03604 =
0.04167 0.02159 0.00880 0.01609
AFIX 43
H5 2 -0.267170 0.570111 0.085259 11.00000 -1.20000
AFIX 0
C23 1 0.361087 0.553478 0.389910 11.00000 0.04223 0.01932 =
0.01543 -0.00308 -0.00498 -0.00282
AFIX 43
H23 2 0.379961 0.649283 0.399699 11.00000 -1.20000
AFIX 0
C12 1 0.508857 0.178720 0.111145 11.00000 0.01902 0.02103 =
0.04146 0.01064 0.00790 0.00594
AFIX 43
H12 2 0.535512 0.263219 0.091457 11.00000 -1.20000
AFIX 0
C22 1 0.222602 0.477850 0.393971 11.00000 0.03647 0.02501 =
0.01568 0.00167 0.00518 0.01089
AFIX 43
H22 2 0.151337 0.525435 0.406027 11.00000 -1.20000
AFIX 0
C4 1 -0.127466 0.701231 0.191031 11.00000 0.03374 0.03256 =
0.04547 0.02070 0.01556 0.02199
AFIX 43
H4 2 -0.181302 0.767365 0.201887 11.00000 -1.20000
AFIX 0
C6 1 -0.100132 0.478061 0.106863 11.00000 0.01575 0.02786 =
0.02706 0.01571 0.00530 0.00834
C21 1 0.187397 0.330484 0.380242 11.00000 0.02468 0.02957 =
0.01611 0.00653 0.00191 0.00107
C13 1 0.605982 0.096027 0.115183 11.00000 0.01919 0.03240 =
0.06752 0.01968 0.01094 0.00995
AFIX 43
H13 2 0.697036 0.123896 0.097684 11.00000 -1.20000
AFIX 0
C7 1 -0.145504 0.357703 0.032842 11.00000 0.01362 0.03074 =
0.02947 0.01508 -0.00292 0.00325
AFIX 43
H7 2 -0.230311 0.343479 -0.007890 11.00000 -1.20000
AFIX 0
C20 1 0.299556 0.263323 0.361940 11.00000 0.03891 0.02174 =
0.01776 0.00668 -0.00325 0.00634
AFIX 43
H20 2 0.281000 0.167495 0.351638 11.00000 -1.20000
AFIX 0
C14 1 0.565027 -0.027819 0.145535 11.00000 0.03140 0.03565 =
0.06023 0.02064 0.01246 0.02404
F4 5 0.416557 0.109687 0.540671 11.00000 0.17738 0.06448 =
0.13740 0.01297 0.02842 0.06235
C19 1 0.440078 0.338933 0.358921 11.00000 0.02875 0.04284 =
0.01851 0.00899 -0.00154 0.01763
AFIX 43
H19 2 0.512083 0.291766 0.348862 11.00000 -1.20000
AFIX 0
C18 1 0.472427 0.483593 0.370835 11.00000 0.02532 0.04283 =
0.01697 0.00808 -0.00651 -0.00439
PART 1
C24A 1 0.030676 0.267566 0.386983 10.65000 0.02774 0.03243 =
0.02467 0.00129 0.00251 0.00564
AFIX 13
H24A 2 -0.026745 0.328568 0.365504 10.65000 -1.20000
AFIX 0
PART 0
F5 5 0.570251 0.100629 0.431735 11.00000 0.17384 0.08382 =
0.09858 0.06010 0.01034 0.04375
F3 5 0.624832 0.070837 0.586026 11.00000 0.15869 0.12477 =
0.07854 0.01281 -0.04191 0.01498
C17 1 0.620388 0.563425 0.361129 11.00000 0.02777 0.09067 =
0.02952 0.01554 -0.01137 -0.02185
AFIX 137
H17A 2 0.667442 0.504902 0.319262 11.00000 -1.50000
H17B 2 0.673651 0.593770 0.425842 11.00000 -1.50000
H17C 2 0.613701 0.642121 0.332140 11.00000 -1.50000
AFIX 0
PART 1
C25A 1 0.013270 0.261379 0.496338 10.65000 0.03761 0.06804 =
0.03865 0.00575 0.01778 -0.00953
AFIX 137
H25A 2 0.060354 0.194132 0.516258 10.65000 -1.50000
H25B 2 -0.085886 0.235854 0.504148 10.65000 -1.50000
H25C 2 0.054435 0.350273 0.537139 10.65000 -1.50000
AFIX 0
C26A 1 -0.020228 0.125582 0.321615 10.65000 0.03956 0.05905 =
0.04492 -0.01188 0.01398 -0.01840
AFIX 137
H26A 2 -0.005680 0.131256 0.253829 10.65000 -1.50000
H26B 2 -0.119506 0.091960 0.325819 10.65000 -1.50000
H26C 2 0.032262 0.063602 0.343796 10.65000 -1.50000
AFIX 0
PART 0
PART 2
C26B 1 -0.080336 0.281310 0.354224 10.35000 0.01607 0.07590 =
0.04882 0.03572 -0.00397 -0.00885
AFIX 137
H26D 2 -0.084144 0.358890 0.404594 10.35000 -1.50000
H26E 2 -0.165538 0.210781 0.349438 10.35000 -1.50000
H26F 2 -0.072073 0.309981 0.291308 10.35000 -1.50000
AFIX 0
C25B 1 0.045077 0.186274 0.484644 10.35000 0.05712 0.07068 =
0.03283 0.03363 0.01023 -0.00987
AFIX 137
H25D 2 0.094899 0.114178 0.487695 10.35000 -1.50000
H25E 2 -0.051717 0.154849 0.496491 10.35000 -1.50000
H25F 2 0.089869 0.265849 0.534459 10.35000 -1.50000
AFIX 0
C24B 1 0.048540 0.224299 0.381884 10.35000 0.02209 0.03325 =
0.02603 0.00593 0.01195 -0.00470
AFIX 13
H24B 2 0.046860 0.140997 0.332666 10.35000 -1.20000
AFIX 0
HKLF 5
REM kr219_twin1_hklf4_a.res in P-1
REM R1 = 0.0590 for 15882 Fo > 4sig(Fo) and 0.0659 for all 17044 data
REM 364 parameters refined using 4 restraints
END
WGHT 0.0149 6.1468
REM Highest difference peak 1.398, deepest hole -1.139, 1-sigma level 0.169
Q1 1 0.2798 0.4396 0.3035 11.00000 0.05 1.40
Q2 1 0.2833 0.4162 0.1982 11.00000 0.05 1.34
Q3 1 0.2865 0.3448 0.1965 11.00000 0.05 1.31
Q4 1 0.2635 0.4614 0.2478 11.00000 0.05 1.23
Q5 1 0.3182 0.3375 0.2617 11.00000 0.05 1.19
Q6 1 0.4011 0.5783 0.1855 11.00000 0.05 1.19
Q7 1 0.2391 0.3256 0.2499 11.00000 0.05 1.10
Q8 1 0.4455 0.4797 0.1404 11.00000 0.05 1.03
Q9 1 0.3604 0.4066 0.2400 11.00000 0.05 0.96
Q10 1 0.3419 0.4610 0.2512 11.00000 0.05 0.95
Q11 1 0.2813 0.2615 0.1773 11.00000 0.05 0.91
Q12 1 0.4237 0.4760 0.0770 11.00000 0.05 0.84
Q13 1 0.3637 0.5026 0.1502 11.00000 0.05 0.83
Q14 1 0.2981 0.5147 0.3281 11.00000 0.05 0.81
Q15 1 0.3695 0.5181 0.2233 11.00000 0.05 0.77
Q16 1 0.4945 -0.0605 0.1463 11.00000 0.05 0.75
Q17 1 0.3419 0.0583 0.5254 11.00000 0.05 0.75
Q18 1 0.2615 0.3654 0.3007 11.00000 0.05 0.74
Q19 1 0.2195 0.2807 0.2912 11.00000 0.05 0.73
Q20 1 0.4807 0.5826 0.1349 11.00000 0.05 0.72
REM The information below was added by Olex2.
REM
REM R1 = 0.0590 for 15882 Fo > 4sig(Fo) and 0.0659 for all 17052 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 1.40, deepest hole -1.14
REM Mean Shift 0, Max Shift -0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0659
REM R1_gt = 0.0590
REM wR_ref = 0.1259
REM GOOF = 1.229
REM Shift_max = -0.001
REM Shift_mean = 0
REM Reflections_all = 17052
REM Reflections_gt = 15882
REM Parameters = n/a
REM Hole = -1.14
REM Peak = 1.40
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.7648
2 0.2352
# start Validation Reply Form
_vrf_PLAT430_kr219_twin1_hklf4
;
PROBLEM: Short Inter D...A Contact O1 .. O1 .. 2.45 Ang.
RESPONSE: Structure is hydrogen bridged dimer, with hydrogen bridging the amide oxygen atoms.
;
# end Validation Reply Form