Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'E. Constable' _publ_contact_author_address ; Departement Chemie University of Basel Spitalstrasse 51 Basel CH-4056 SWITZERLAND ; _publ_contact_author_email EDWIN.CONSTABLE@UNIBAS.CH _publ_section_title ; Expanded ligands: metallosupramolecular analogues of dicarboxylic acids ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; loop_ _publ_author_name 'E. Constable' 'Emma L. Dunphy' 'C. E. Housecroft' 'Markus Neuburger' 'Frank Schaper' ; S.Schffner ; data_1 _database_code_depnum_ccdc_archive 'CCDC 651821' _audit_creation_date 07-07-17 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title '2091327 fs82_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 8.6013(4) _cell_length_b 8.6013(4) _cell_length_c 40.0329(16) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2961.7(2) _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I -4 2 d ' _symmetry_space_group_name_Hall 'I -4 2bw' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,y+1/2,z+1/2 y,-x,-z y+1/2,-x+1/2,-z+1/2 -x,-y,z -x+1/2,-y+1/2,z+1/2 -y,x,-z -y+1/2,x+1/2,-z+1/2 -x+1/2,y,-z+3/4 -x+1,y+1/2,-z+5/4 -y+1/2,-x,z+3/4 -y+1,-x+1/2,z+5/4 x+1/2,-y,-z+3/4 x+1,-y+1/2,-z+5/4 y+1/2,x,z+3/4 y+1,x+1/2,z+5/4 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ru -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C32 H28 N6 O8 Ru1 # Dc = 1.63 Fooo = 1480.00 Mu = 5.95 M = 181.42 # Found Formula = C32 H28 N6 O8 Ru1 # Dc = 1.63 FOOO = 1480.00 Mu = 5.95 M = 181.42 _chemical_formula_sum 'C32 H28 N6 O8 Ru1' _chemical_formula_moiety 'C32 H20 N6 O4 Ru, 4(H2 O)' _chemical_compound_source ? _chemical_formula_weight 725.68 _cell_measurement_reflns_used 2242 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.22 _exptl_crystal_density_diffrn 1.627 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.595 # Sheldrick geometric approximatio 0.91 0.95 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 0.95 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 173 _diffrn_reflns_number 32505 _reflns_number_total 2158 _diffrn_reflns_av_R_equivalents 0.106 # Number of reflections with Friedels Law is 1227 # Number of reflections without Friedels Law is 2158 # Theoretical number of reflections is about 1080 _diffrn_reflns_theta_min 3.476 _diffrn_reflns_theta_max 30.002 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.002 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -56 _diffrn_reflns_limit_l_max 55 _reflns_limit_h_min -8 _reflns_limit_h_max 8 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 56 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.42 _refine_diff_density_max 0.21 _refine_ls_number_reflns 1455 _refine_ls_number_restraints 0 _refine_ls_number_parameters 109 #_refine_ls_R_factor_ref 0.0208 _refine_ls_wR_factor_ref 0.0217 _refine_ls_goodness_of_fit_ref 1.0798 #_reflns_number_all 2150 _refine_ls_R_factor_all 0.0414 _refine_ls_wR_factor_all 0.0297 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 1455 _refine_ls_R_factor_gt 0.0208 _refine_ls_wR_factor_gt 0.0217 _refine_ls_shift/su_max 0.000666 _refine_ls_abs_structure_Flack -0.01(4) _refine_ls_abs_structure_details 'Flack (1983), 931 Friedel-pairs' # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration ad _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.996 -0.670 0.521 ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ru1 Ru 0.0000 0.0000 0.5000 0.0121 1.0000 Uani S T . . . . N1 N 0.2180(2) 0.0899(2) 0.51000(4) 0.0151 1.0000 Uani . . . . . . N2 N 0.0000 0.0000 0.54938(4) 0.0144 1.0000 Uani S T . . . . C1 C 0.3294(3) 0.1288(3) 0.48824(5) 0.0173 1.0000 Uani . . . . . . C2 C 0.4686(2) 0.1960(3) 0.49783(7) 0.0235 1.0000 Uani . . . . . . C3 C 0.4942(6) 0.2236(3) 0.53152(5) 0.0264 1.0000 Uani . . . . . . C4 C 0.3825(3) 0.1797(3) 0.55432(6) 0.0234 1.0000 Uani . . . . . . C5 C 0.2464(3) 0.1123(3) 0.54324(5) 0.0164 1.0000 Uani . . . . . . C6 C 0.1235(3) 0.0576(3) 0.56577(5) 0.0166 1.0000 Uani . . . . . . C7 C 0.1263(3) 0.0583(3) 0.60013(5) 0.0231 1.0000 Uani . . . . . . C8 C 0.0000 0.0000 0.61767(5) 0.0267 1.0000 Uani S T . . . . C9 C 0.0000 0.0000 0.65586(6) 0.0464 1.0000 Uani S T . . . . O1 O 0.1273(3) 0.0099(6) 0.66952(4) 0.0726 1.0000 Uani . . . . . . O2 O 0.3958(4) -0.1212(5) 0.64565(10) 0.0992 1.0000 Uani . . . . . . H1 H 0.2950 -0.0903 0.6540 0.1185 1.0000 Uiso R . . . . . H2 H 0.3884 -0.2200 0.6370 0.1185 0.5000 Uiso R . . . . . H3 H 0.4603 -0.0297 0.6431 0.1185 0.5000 Uiso R . . . . . H11 H 0.3112 0.1037 0.4647 0.0211 1.0000 Uiso R . . . . . H21 H 0.5440 0.2287 0.4814 0.0296 1.0000 Uiso R . . . . . H31 H 0.5885 0.2746 0.5385 0.0316 1.0000 Uiso R . . . . . H41 H 0.3989 0.1964 0.5783 0.0297 1.0000 Uiso R . . . . . H71 H 0.2142 0.1017 0.6117 0.0282 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01460(9) 0.01460(9) 0.00717(10) 0.0000 0.0000 0.0000 N1 0.0175(9) 0.0159(9) 0.0119(7) 0.0016(6) -0.0004(6) 0.0018(7) N2 0.0162(11) 0.0170(11) 0.0099(7) 0.0000 0.0000 0.002(3) C1 0.0197(11) 0.0192(11) 0.0129(8) 0.0021(7) 0.0043(7) 0.0028(9) C2 0.0226(18) 0.0228(9) 0.0251(9) 0.0023(10) 0.0058(10) -0.0012(7) C3 0.0188(11) 0.0341(11) 0.0262(9) 0.0010(8) -0.0060(18) -0.001(2) C4 0.0197(11) 0.0313(13) 0.0192(10) -0.0018(9) -0.0005(8) -0.0048(10) C5 0.0183(11) 0.0194(10) 0.0114(8) 0.0006(8) -0.0008(8) 0.0001(8) C6 0.0189(10) 0.0201(9) 0.0109(9) 0.0005(7) -0.0015(7) -0.0010(7) C7 0.0252(12) 0.0310(12) 0.0131(9) 0.0005(8) -0.0053(8) -0.0055(9) C8 0.0327(16) 0.0369(17) 0.0106(9) 0.0000 0.0000 -0.004(4) C9 0.062(3) 0.066(3) 0.0115(10) 0.0000 0.0000 -0.031(4) O1 0.0696(15) 0.132(2) 0.0160(7) 0.002(2) -0.0146(9) -0.046(3) O2 0.070(2) 0.094(2) 0.133(3) 0.046(2) -0.058(2) -0.0071(17) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3018(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru1 . N1 3_556 2.0671(19) yes Ru1 . N1 5_555 2.0671(19) yes Ru1 . N1 7_556 2.0671(19) yes Ru1 . N2 3_556 1.9768(16) yes Ru1 . N1 . 2.0671(19) yes Ru1 . N2 . 1.9768(16) yes N1 . C1 . 1.338(3) yes N1 . C5 . 1.367(3) yes N2 . C6 5_555 1.343(2) yes N2 . C6 . 1.343(2) yes C1 . C2 . 1.383(3) yes C1 . H11 . 0.981 no C2 . C3 . 1.387(3) yes C2 . H21 . 0.965 no C3 . C4 . 1.378(5) yes C3 . H31 . 0.964 no C4 . C5 . 1.380(3) yes C4 . H41 . 0.980 no C5 . C6 . 1.467(3) yes C6 . C7 . 1.376(3) yes C7 . C8 . 1.387(3) yes C7 . H71 . 0.962 no C8 . C9 . 1.529(3) yes C9 . O1 5_555 1.227(2) yes C9 . O1 . 1.227(2) yes O2 . H1 . 0.967 no O2 . H2 . 0.920 no O2 . H3 . 0.968 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 3_556 Ru1 . N1 5_555 92.148(18) yes N1 3_556 Ru1 . N1 7_556 157.67(9) yes N1 5_555 Ru1 . N1 7_556 92.148(18) yes N1 3_556 Ru1 . N2 3_556 78.84(5) yes N1 5_555 Ru1 . N2 3_556 101.16(5) yes N1 7_556 Ru1 . N2 3_556 78.84(5) yes N1 3_556 Ru1 . N1 . 92.148(17) yes N1 5_555 Ru1 . N1 . 157.67(9) yes N1 7_556 Ru1 . N1 . 92.148(18) yes N2 3_556 Ru1 . N1 . 101.16(5) yes N1 3_556 Ru1 . N2 . 101.16(5) yes N1 5_555 Ru1 . N2 . 78.84(5) yes N1 7_556 Ru1 . N2 . 101.16(5) yes N2 3_556 Ru1 . N2 . 179.994 yes N1 . Ru1 . N2 . 78.84(5) yes Ru1 . N1 . C1 . 128.15(14) yes Ru1 . N1 . C5 . 113.80(14) yes C1 . N1 . C5 . 118.05(19) yes C6 5_555 N2 . Ru1 . 119.24(11) yes C6 5_555 N2 . C6 . 121.5(2) yes Ru1 . N2 . C6 . 119.24(11) yes N1 . C1 . C2 . 123.0(2) yes N1 . C1 . H11 . 117.2 no C2 . C1 . H11 . 119.8 no C1 . C2 . C3 . 118.6(3) yes C1 . C2 . H21 . 121.0 no C3 . C2 . H21 . 120.3 no C2 . C3 . C4 . 119.1(4) yes C2 . C3 . H31 . 119.7 no C4 . C3 . H31 . 121.2 no C3 . C4 . C5 . 119.6(2) yes C3 . C4 . H41 . 120.5 no C5 . C4 . H41 . 119.9 no C4 . C5 . N1 . 121.6(2) yes C4 . C5 . C6 . 123.27(19) yes N1 . C5 . C6 . 115.1(2) yes C5 . C6 . N2 . 112.83(17) yes C5 . C6 . C7 . 126.9(2) yes N2 . C6 . C7 . 120.2(2) yes C6 . C7 . C8 . 119.4(2) yes C6 . C7 . H71 . 119.7 no C8 . C7 . H71 . 120.9 no C7 . C8 . C7 5_555 119.2(2) yes C7 . C8 . C9 . 120.40(12) yes C7 5_555 C8 . C9 . 120.40(12) yes C8 . C9 . O1 5_555 116.45(13) yes C8 . C9 . O1 . 116.45(13) yes O1 5_555 C9 . O1 . 127.1(3) yes H1 . O2 . H2 . 108.8 no H1 . O2 . H3 . 109.1 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag O2 . H1 . O1 . 167 0.97 1.79 2.742(2) yes O2 . H2 . O2 14_445 158 0.92 1.89 2.765(2) yes O2 . H3 . O2 5_655 167 0.97 1.80 2.749(2) yes # Attachment 'fs153.cif' data_fs153_173k _database_code_depnum_ccdc_archive 'CCDC 651822' _audit_creation_date 07-06-18 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title '8240939 fs153_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 39.775(4) _cell_length_b 8.8662(13) _cell_length_c 25.857(3) _cell_angle_alpha 90 _cell_angle_beta 106.393(7) _cell_angle_gamma 90 _cell_volume 8747.7(20) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2/c' _symmetry_space_group_name_Hall '-P 2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y,-z+1/2 x,-y,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ru -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C92 H84 Cl4 N12 O16 Ru2 # Dc = 1.49 Fooo = 4008.00 Mu = 5.42 M = 1957.70 # Found Formula = C92 H82 Cl4 N12 O16 Ru2 # Dc = 1.48 FOOO = 4008.00 Mu = 5.42 M = 1955.69 _chemical_formula_sum 'C92 H84 Cl4 N12 O16 Ru2' _chemical_formula_moiety '2(C46 H34 N6 O4 Ru), 8(H2 O), 4(Cl)' _chemical_compound_source ? _chemical_formula_weight 1957.70 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 3 _cell_measurement_theta_max 29 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_min 0.13 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_max 0.24 _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 4008 _exptl_absorpt_coefficient_mu 0.542 # Sheldrick geometric approximatio 0.92 0.93 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 0.93 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 173 _diffrn_reflns_number 234385 _reflns_number_total 22134 _diffrn_reflns_av_R_equivalents 0.085 # Number of reflections with Friedels Law is 22134 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 22185 _diffrn_reflns_theta_min 3.009 _diffrn_reflns_theta_max 28.504 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.504 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -53 _diffrn_reflns_limit_h_max 53 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _reflns_limit_h_min 0 _reflns_limit_h_max 53 _reflns_limit_k_min -11 _reflns_limit_k_max 0 _reflns_limit_l_min -34 _reflns_limit_l_max 33 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.87 _refine_diff_density_max 1.24 _refine_ls_number_reflns 11491 _refine_ls_number_restraints 0 _refine_ls_number_parameters 1158 #_refine_ls_R_factor_ref 0.0367 _refine_ls_wR_factor_ref 0.0388 _refine_ls_goodness_of_fit_ref 1.0756 #_reflns_number_all 22027 _refine_ls_R_factor_all 0.0784 _refine_ls_wR_factor_all 0.0576 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 11491 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_gt 0.0388 _refine_ls_shift/su_max 0.003795 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 3.01 0.155E-01 2.23 ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ru1 Ru 0.368209(6) 0.60624(3) 0.881371(10) 0.0202 1.0000 Uani . . . . . . Ru2 Ru 0.121532(6) 0.91212(3) 0.637713(10) 0.0220 1.0000 Uani . . . . . . N1 N 0.38633(7) 0.7023(3) 0.95697(11) 0.0247 1.0000 Uani . . . . . . N2 N 0.41910(6) 0.6085(3) 0.89083(10) 0.0222 1.0000 Uani . . . . . . N3 N 0.37022(7) 0.5112(3) 0.80943(11) 0.0235 1.0000 Uani . . . . . . N4 N 0.36156(6) 0.3942(3) 0.91036(10) 0.0232 1.0000 Uani . . . . . . N5 N 0.31741(6) 0.6073(3) 0.87304(10) 0.0210 1.0000 Uani . . . . . . N6 N 0.35442(6) 0.8158(3) 0.84669(10) 0.0223 1.0000 Uani . . . . . . N7 N 0.13587(7) 0.7050(3) 0.67493(10) 0.0239 1.0000 Uani . . . . . . N8 N 0.17303(7) 0.9198(3) 0.65376(10) 0.0230 1.0000 Uani . . . . . . N9 N 0.12838(7) 1.1265(3) 0.61077(10) 0.0247 1.0000 Uani . . . . . . N10 N 0.11361(7) 1.0069(3) 0.70597(11) 0.0247 1.0000 Uani . . . . . . N11 N 0.07002(7) 0.9038(3) 0.62001(11) 0.0246 1.0000 Uani . . . . . . N12 N 0.10880(7) 0.8155(3) 0.56196(11) 0.0266 1.0000 Uani . . . . . . C1 C 0.36744(9) 0.7507(4) 0.98916(13) 0.0283 1.0000 Uani . . . . . . C2 C 0.38226(10) 0.8247(4) 1.03711(14) 0.0335 1.0000 Uani . . . . . . C3 C 0.41779(10) 0.8485(4) 1.05328(14) 0.0344 1.0000 Uani . . . . . . C4 C 0.43801(9) 0.7975(4) 1.02117(14) 0.0312 1.0000 Uani . . . . . . C5 C 0.42191(8) 0.7250(3) 0.97327(13) 0.0241 1.0000 Uani . . . . . . C6 C 0.44094(8) 0.6697(3) 0.93589(13) 0.0248 1.0000 Uani . . . . . . C7 C 0.47657(8) 0.6754(4) 0.94231(14) 0.0287 1.0000 Uani . . . . . . C8 C 0.48986(8) 0.6168(4) 0.90197(14) 0.0286 1.0000 Uani . . . . . . C9 C 0.46711(8) 0.5532(4) 0.85618(14) 0.0284 1.0000 Uani . . . . . . C10 C 0.43147(8) 0.5519(4) 0.85098(13) 0.0247 1.0000 Uani . . . . . . C11 C 0.40354(8) 0.4944(3) 0.80516(13) 0.0240 1.0000 Uani . . . . . . C12 C 0.40972(8) 0.4277(4) 0.76026(14) 0.0315 1.0000 Uani . . . . . . C13 C 0.38140(9) 0.3804(4) 0.71817(14) 0.0331 1.0000 Uani . . . . . . C14 C 0.34799(9) 0.4007(4) 0.72245(13) 0.0307 1.0000 Uani . . . . . . C15 C 0.34333(8) 0.4655(3) 0.76859(13) 0.0262 1.0000 Uani . . . . . . C16 C 0.38576(8) 0.2858(4) 0.92633(13) 0.0256 1.0000 Uani . . . . . . C17 C 0.37771(9) 0.1445(4) 0.94187(14) 0.0301 1.0000 Uani . . . . . . C18 C 0.34342(9) 0.1130(4) 0.94119(14) 0.0320 1.0000 Uani . . . . . . C19 C 0.31819(8) 0.2232(4) 0.92388(13) 0.0271 1.0000 Uani . . . . . . C20 C 0.32753(8) 0.3632(3) 0.90894(12) 0.0231 1.0000 Uani . . . . . . C21 C 0.30243(8) 0.4868(3) 0.88892(12) 0.0226 1.0000 Uani . . . . . . C22 C 0.26703(8) 0.4861(4) 0.88504(13) 0.0259 1.0000 Uani . . . . . . C23 C 0.24626(8) 0.6115(3) 0.86400(12) 0.0235 1.0000 Uani . . . . . . C24 C 0.26257(8) 0.7348(3) 0.84742(13) 0.0251 1.0000 Uani . . . . . . C25 C 0.29819(8) 0.7300(3) 0.85208(12) 0.0220 1.0000 Uani . . . . . . C26 C 0.31960(8) 0.8483(3) 0.83666(12) 0.0230 1.0000 Uani . . . . . . C27 C 0.30596(9) 0.9840(4) 0.81275(14) 0.0286 1.0000 Uani . . . . . . C28 C 0.32770(9) 1.0872(4) 0.79875(14) 0.0317 1.0000 Uani . . . . . . C29 C 0.36295(9) 1.0540(4) 0.80896(14) 0.0312 1.0000 Uani . . . . . . C30 C 0.37531(8) 0.9174(4) 0.83284(13) 0.0272 1.0000 Uani . . . . . . C31 C 0.52799(8) 0.6206(4) 0.90729(14) 0.0295 1.0000 Uani . . . . . . C32 C 0.54331(9) 0.4980(4) 0.88901(15) 0.0328 1.0000 Uani . . . . . . C33 C 0.57872(9) 0.4984(4) 0.89341(15) 0.0337 1.0000 Uani . . . . . . C34 C 0.59911(8) 0.6216(4) 0.91476(13) 0.0304 1.0000 Uani . . . . . . C35 C 0.58380(9) 0.7468(4) 0.93183(15) 0.0351 1.0000 Uani . . . . . . C36 C 0.54833(9) 0.7449(4) 0.92877(15) 0.0339 1.0000 Uani . . . . . . C37 C 0.63744(8) 0.6127(5) 0.92119(14) 0.0354 1.0000 Uani . . . . . . C38 C 0.69160(9) 0.7389(6) 0.94590(18) 0.0520 1.0000 Uani . . . . . . C39 C 0.20807(7) 0.6113(3) 0.85854(12) 0.0235 1.0000 Uani . . . . . . C40 C 0.19187(8) 0.4844(4) 0.87316(14) 0.0298 1.0000 Uani . . . . . . C41 C 0.15605(8) 0.4812(4) 0.86537(14) 0.0289 1.0000 Uani . . . . . . C42 C 0.13516(7) 0.6028(4) 0.84225(12) 0.0248 1.0000 Uani . . . . . . C43 C 0.15113(8) 0.7304(4) 0.82954(15) 0.0318 1.0000 Uani . . . . . . C44 C 0.18714(9) 0.7351(4) 0.83752(15) 0.0324 1.0000 Uani . . . . . . C45 C 0.09639(8) 0.5888(4) 0.82978(13) 0.0263 1.0000 Uani . . . . . . C46 C 0.04205(9) 0.7023(5) 0.78857(18) 0.0427 1.0000 Uani . . . . . . C47 C 0.11466(8) 0.6011(4) 0.68704(13) 0.0271 1.0000 Uani . . . . . . C48 C 0.12734(9) 0.4691(4) 0.71407(14) 0.0324 1.0000 Uani . . . . . . C49 C 0.16307(9) 0.4426(4) 0.72968(14) 0.0309 1.0000 Uani . . . . . . C50 C 0.18518(9) 0.5490(3) 0.71763(14) 0.0281 1.0000 Uani . . . . . . C51 C 0.17115(8) 0.6786(3) 0.69001(13) 0.0245 1.0000 Uani . . . . . . C52 C 0.19270(8) 0.7994(3) 0.67623(13) 0.0246 1.0000 Uani . . . . . . C53 C 0.22841(8) 0.7970(4) 0.68337(13) 0.0268 1.0000 Uani . . . . . . C54 C 0.24477(8) 0.9222(3) 0.66750(12) 0.0230 1.0000 Uani . . . . . . C55 C 0.22388(8) 1.0479(3) 0.64664(13) 0.0257 1.0000 Uani . . . . . . C56 C 0.18828(8) 1.0437(3) 0.63981(13) 0.0235 1.0000 Uani . . . . . . C57 C 0.16259(8) 1.1630(3) 0.61742(12) 0.0234 1.0000 Uani . . . . . . C58 C 0.17228(9) 1.3058(4) 0.60526(14) 0.0289 1.0000 Uani . . . . . . C59 C 0.14665(9) 1.4131(4) 0.58595(14) 0.0331 1.0000 Uani . . . . . . C60 C 0.11222(9) 1.3767(4) 0.57947(15) 0.0321 1.0000 Uani . . . . . . C61 C 0.10379(9) 1.2325(4) 0.59242(13) 0.0283 1.0000 Uani . . . . . . C62 C 0.13839(9) 1.0577(3) 0.74917(13) 0.0273 1.0000 Uani . . . . . . C63 C 0.12989(9) 1.1284(4) 0.79159(14) 0.0311 1.0000 Uani . . . . . . C64 C 0.09488(10) 1.1509(4) 0.78899(15) 0.0332 1.0000 Uani . . . . . . C65 C 0.06940(9) 1.0977(4) 0.74509(14) 0.0308 1.0000 Uani . . . . . . C66 C 0.07910(8) 1.0246(3) 0.70379(13) 0.0263 1.0000 Uani . . . . . . C67 C 0.05404(8) 0.9632(3) 0.65548(13) 0.0248 1.0000 Uani . . . . . . C68 C 0.01782(9) 0.9586(4) 0.64407(14) 0.0296 1.0000 Uani . . . . . . C69 C -0.00202(8) 0.8907(4) 0.59672(14) 0.0284 1.0000 Uani . . . . . . C70 C 0.01512(8) 0.8322(4) 0.56073(14) 0.0283 1.0000 Uani . . . . . . C71 C 0.05147(8) 0.8413(3) 0.57341(13) 0.0254 1.0000 Uani . . . . . . C72 C 0.07379(8) 0.7883(4) 0.54023(13) 0.0274 1.0000 Uani . . . . . . C73 C 0.06104(10) 0.7148(4) 0.49134(14) 0.0330 1.0000 Uani . . . . . . C74 C 0.08444(11) 0.6663(4) 0.46407(15) 0.0377 1.0000 Uani . . . . . . C75 C 0.11974(10) 0.6953(4) 0.48530(15) 0.0372 1.0000 Uani . . . . . . C76 C 0.13085(9) 0.7719(4) 0.53400(14) 0.0300 1.0000 Uani . . . . . . C77 C 0.28291(8) 0.9214(3) 0.67191(12) 0.0241 1.0000 Uani . . . . . . C78 C 0.30424(8) 0.8013(4) 0.69524(14) 0.0303 1.0000 Uani . . . . . . C79 C 0.33962(9) 0.8013(4) 0.69969(15) 0.0312 1.0000 Uani . . . . . . C80 C 0.35488(8) 0.9220(4) 0.68033(13) 0.0256 1.0000 Uani . . . . . . C81 C 0.33377(8) 1.0416(4) 0.65571(14) 0.0287 1.0000 Uani . . . . . . C82 C 0.29809(9) 1.0409(4) 0.65175(14) 0.0309 1.0000 Uani . . . . . . C83 C 0.39303(8) 0.9271(4) 0.68581(13) 0.0290 1.0000 Uani . . . . . . C84 C 0.44738(10) 0.8001(5) 0.71838(18) 0.0454 1.0000 Uani . . . . . . C85 C -0.04061(8) 0.8806(4) 0.58505(13) 0.0282 1.0000 Uani . . . . . . C86 C -0.05894(9) 0.7558(4) 0.55888(15) 0.0358 1.0000 Uani . . . . . . C87 C -0.09491(9) 0.7481(4) 0.54776(15) 0.0363 1.0000 Uani . . . . . . C88 C -0.11351(9) 0.8676(4) 0.56114(14) 0.0332 1.0000 Uani . . . . . . C89 C -0.09517(9) 0.9912(4) 0.58830(15) 0.0359 1.0000 Uani . . . . . . C90 C -0.05928(9) 0.9979(4) 0.60027(16) 0.0350 1.0000 Uani . . . . . . C91 C -0.15237(9) 0.8729(5) 0.54667(15) 0.0392 1.0000 Uani . . . . . . C92 C -0.20494(10) 0.7408(7) 0.50754(19) 0.0601 1.0000 Uani . . . . . . O1 O 0.65385(6) 0.7418(3) 0.93713(11) 0.0444 1.0000 Uani . . . . . . O2 O 0.65167(7) 0.4988(4) 0.91280(14) 0.0573 1.0000 Uani . . . . . . O3 O 0.07998(6) 0.7094(3) 0.80531(11) 0.0366 1.0000 Uani . . . . . . O4 O 0.08171(6) 0.4775(3) 0.84007(10) 0.0353 1.0000 Uani . . . . . . O5 O 0.40972(6) 0.8047(3) 0.70980(11) 0.0398 1.0000 Uani . . . . . . O6 O 0.40745(6) 1.0311(3) 0.67043(11) 0.0393 1.0000 Uani . . . . . . O7 O -0.16691(7) 0.7443(4) 0.52465(11) 0.0496 1.0000 Uani . . . . . . O8 O -0.16868(7) 0.9817(4) 0.55474(15) 0.0593 1.0000 Uani . . . . . . O9 O 0.26462(7) 0.3759(4) 0.76190(13) 0.0579 1.0000 Uani . . . . . . O10 O 0.01785(8) 0.2922(4) 0.80478(15) 0.0624 1.0000 Uani . . . . . . O11 O 0.23243(9) 0.1133(5) 0.9373(2) 0.0902 1.0000 Uani . . . . . . O12 O 0.28964(9) 0.8998(4) 0.97864(18) 0.0821 1.0000 Uani . . . . . . O13 O 0.28666(10) 0.6665(5) 1.04629(18) 0.0890 1.0000 Uani . . . . . . O14 O 0.21098(12) 0.6767(7) 0.5435(2) 0.1305 1.0000 Uani . . . . . . O15 O 0.52122(12) 0.1397(6) 0.82236(19) 0.0978 1.0000 Uani . . . . . . O160 O 0.4656(3) 0.9762(13) 0.8483(4) 0.0888 0.5000 Uani . . . . . . O161 O 0.4591(4) 1.0830(19) 0.8282(4) 0.1297 0.5000 Uani . . . . . . Cl1 Cl 0.25690(2) 0.44771(11) 0.63796(4) 0.0452 1.0000 Uani . . . . . . Cl2 Cl 0.22343(2) 1.13212(12) 0.81344(6) 0.0583 1.0000 Uani . . . . . . Cl3 Cl 0.5000 0.4189(2) 0.7500 0.0581 1.0000 Uani S T . . . . Cl4 Cl 0.47108(5) 1.0820(2) 0.95623(8) 0.0464 0.5000 Uani . . . . . . Cl5 Cl 0.02416(4) 0.4141(2) 0.54780(7) 0.0388 0.5000 Uani . . . . . . Cl6 Cl 0.03062(6) 0.5017(3) 0.66234(10) 0.0686 0.5000 Uani . . . . . . H90 H 0.2504 0.3144 0.7678 0.0849 1.0000 Uiso R . . . . . H95 H 0.2608 0.3770 0.7273 0.0841 1.0000 Uiso R . . . . . H100 H 0.0336 0.3523 0.8205 0.0970 1.0000 Uiso R . . . . . H105 H 0.0039 0.3119 0.8218 0.0975 1.0000 Uiso R . . . . . H110 H 0.2144 0.0856 0.9446 0.1256 1.0000 Uiso R . . . . . H115 H 0.2286 0.0837 0.9043 0.1255 1.0000 Uiso R . . . . . H120 H 0.2850 0.8266 0.9954 0.1276 1.0000 Uiso R . . . . . H125 H 0.2710 0.9460 0.9657 0.1279 1.0000 Uiso R . . . . . H130 H 0.2748 0.6446 1.0669 0.1418 1.0000 Uiso R . . . . . H135 H 0.3070 0.6369 1.0595 0.1416 1.0000 Uiso R . . . . . H140 H 0.2232 0.6267 0.5682 0.1787 1.0000 Uiso R . . . . . H145 H 0.2171 0.6486 0.5176 0.1787 1.0000 Uiso R . . . . . H150 H 0.5266 0.1853 0.7940 0.1426 1.0000 Uiso R . . . . . H155 H 0.5358 0.0703 0.8226 0.1430 1.0000 Uiso R . . . . . H381 H 0.6968 0.7112 0.9133 0.0779 1.0000 Uiso R . . . . . H382 H 0.7002 0.8394 0.9565 0.0781 1.0000 Uiso R . . . . . H383 H 0.7021 0.6682 0.9744 0.0777 1.0000 Uiso R . . . . . H461 H 0.0334 0.8019 0.7771 0.0624 1.0000 Uiso R . . . . . H462 H 0.0347 0.6328 0.7588 0.0617 1.0000 Uiso R . . . . . H463 H 0.0333 0.6707 0.8177 0.0621 1.0000 Uiso R . . . . . H841 H 0.4529 0.8196 0.6851 0.0678 1.0000 Uiso R . . . . . H842 H 0.4588 0.8743 0.7445 0.0680 1.0000 Uiso R . . . . . H843 H 0.4559 0.7018 0.7317 0.0680 1.0000 Uiso R . . . . . H921 H -0.2138 0.8166 0.4805 0.0877 1.0000 Uiso R . . . . . H922 H -0.2134 0.7601 0.5383 0.0873 1.0000 Uiso R . . . . . H923 H -0.2125 0.6421 0.4931 0.0879 1.0000 Uiso R . . . . . H11 H 0.3432 0.7334 0.9781 0.0347 1.0000 Uiso R . . . . . H21 H 0.3678 0.8587 1.0578 0.0418 1.0000 Uiso R . . . . . H31 H 0.4284 0.8990 1.0857 0.0423 1.0000 Uiso R . . . . . H41 H 0.4622 0.8124 1.0313 0.0367 1.0000 Uiso R . . . . . H71 H 0.4917 0.7182 0.9738 0.0343 1.0000 Uiso R . . . . . H91 H 0.4759 0.5105 0.8289 0.0349 1.0000 Uiso R . . . . . H121 H 0.4328 0.4145 0.7582 0.0379 1.0000 Uiso R . . . . . H131 H 0.3848 0.3368 0.6870 0.0400 1.0000 Uiso R . . . . . H141 H 0.3283 0.3704 0.6943 0.0362 1.0000 Uiso R . . . . . H151 H 0.3206 0.4768 0.7717 0.0307 1.0000 Uiso R . . . . . H161 H 0.4088 0.3083 0.9268 0.0311 1.0000 Uiso R . . . . . H171 H 0.3956 0.0707 0.9530 0.0363 1.0000 Uiso R . . . . . H181 H 0.3373 0.0183 0.9524 0.0391 1.0000 Uiso R . . . . . H191 H 0.2945 0.2032 0.9223 0.0330 1.0000 Uiso R . . . . . H221 H 0.2572 0.4015 0.8964 0.0309 1.0000 Uiso R . . . . . H241 H 0.2494 0.8200 0.8330 0.0292 1.0000 Uiso R . . . . . H271 H 0.2822 1.0049 0.8064 0.0339 1.0000 Uiso R . . . . . H281 H 0.3186 1.1778 0.7832 0.0378 1.0000 Uiso R . . . . . H291 H 0.3787 1.1211 0.8003 0.0382 1.0000 Uiso R . . . . . H301 H 0.3990 0.8950 0.8391 0.0328 1.0000 Uiso R . . . . . H321 H 0.5294 0.4151 0.8737 0.0390 1.0000 Uiso R . . . . . H331 H 0.5890 0.4133 0.8821 0.0412 1.0000 Uiso R . . . . . H351 H 0.5971 0.8320 0.9451 0.0417 1.0000 Uiso R . . . . . H361 H 0.5384 0.8266 0.9413 0.0413 1.0000 Uiso R . . . . . H401 H 0.2055 0.4016 0.8882 0.0362 1.0000 Uiso R . . . . . H411 H 0.1452 0.3957 0.8749 0.0355 1.0000 Uiso R . . . . . H431 H 0.1373 0.8135 0.8155 0.0383 1.0000 Uiso R . . . . . H441 H 0.1976 0.8229 0.8287 0.0389 1.0000 Uiso R . . . . . H471 H 0.0908 0.6215 0.6768 0.0335 1.0000 Uiso R . . . . . H481 H 0.1119 0.3994 0.7213 0.0406 1.0000 Uiso R . . . . . H491 H 0.1721 0.3539 0.7478 0.0382 1.0000 Uiso R . . . . . H501 H 0.2095 0.5342 0.7278 0.0338 1.0000 Uiso R . . . . . H531 H 0.2415 0.7116 0.6984 0.0319 1.0000 Uiso R . . . . . H551 H 0.2339 1.1339 0.6370 0.0308 1.0000 Uiso R . . . . . H581 H 0.1961 1.3289 0.6102 0.0343 1.0000 Uiso R . . . . . H591 H 0.1527 1.5112 0.5778 0.0391 1.0000 Uiso R . . . . . H601 H 0.0942 1.4475 0.5661 0.0374 1.0000 Uiso R . . . . . H611 H 0.0803 1.2069 0.5887 0.0325 1.0000 Uiso R . . . . . H621 H 0.1620 1.0448 0.7505 0.0323 1.0000 Uiso R . . . . . H631 H 0.1480 1.1612 0.8217 0.0368 1.0000 Uiso R . . . . . H641 H 0.0888 1.2012 0.8168 0.0411 1.0000 Uiso R . . . . . H651 H 0.0457 1.1111 0.7430 0.0391 1.0000 Uiso R . . . . . H681 H 0.0069 1.0017 0.6680 0.0362 1.0000 Uiso R . . . . . H701 H 0.0016 0.7874 0.5284 0.0340 1.0000 Uiso R . . . . . H731 H 0.0371 0.6979 0.4771 0.0396 1.0000 Uiso R . . . . . H741 H 0.0761 0.6138 0.4311 0.0462 1.0000 Uiso R . . . . . H751 H 0.1364 0.6639 0.4679 0.0471 1.0000 Uiso R . . . . . H761 H 0.1548 0.7939 0.5483 0.0369 1.0000 Uiso R . . . . . H781 H 0.2950 0.7178 0.7083 0.0369 1.0000 Uiso R . . . . . H791 H 0.3535 0.7195 0.7160 0.0370 1.0000 Uiso R . . . . . H811 H 0.3436 1.1215 0.6417 0.0352 1.0000 Uiso R . . . . . H821 H 0.2836 1.1226 0.6355 0.0377 1.0000 Uiso R . . . . . H861 H -0.0466 0.6755 0.5487 0.0429 1.0000 Uiso R . . . . . H871 H -0.1068 0.6619 0.5311 0.0429 1.0000 Uiso R . . . . . H891 H -0.1076 1.0699 0.5979 0.0441 1.0000 Uiso R . . . . . H901 H -0.0472 1.0820 0.6188 0.0427 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01562(11) 0.01939(11) 0.02617(12) 0.00282(10) 0.00709(9) 0.00060(9) Ru2 0.02027(12) 0.01818(11) 0.02878(13) 0.00301(10) 0.00897(9) 0.00275(9) N1 0.0249(13) 0.0226(12) 0.0272(14) 0.0030(11) 0.0083(11) 0.0012(10) N2 0.0187(11) 0.0221(12) 0.0263(12) 0.0012(11) 0.0072(9) 0.0002(10) N3 0.0208(12) 0.0203(12) 0.0303(14) 0.0018(10) 0.0084(10) -0.0023(10) N4 0.0180(11) 0.0234(12) 0.0291(13) 0.0025(11) 0.0080(10) 0.0011(10) N5 0.0189(11) 0.0203(12) 0.0251(12) 0.0020(10) 0.0082(9) 0.0012(10) N6 0.0203(12) 0.0218(12) 0.0256(13) 0.0011(10) 0.0078(10) -0.0009(10) N7 0.0262(13) 0.0180(12) 0.0286(14) 0.0024(10) 0.0098(11) 0.0009(10) N8 0.0254(12) 0.0156(11) 0.0289(13) 0.0027(10) 0.0090(10) 0.0040(10) N9 0.0254(13) 0.0218(12) 0.0275(13) 0.0030(10) 0.0085(10) 0.0048(10) N10 0.0243(13) 0.0197(12) 0.0318(14) 0.0029(11) 0.0108(11) 0.0004(10) N11 0.0239(12) 0.0195(12) 0.0312(13) 0.0026(11) 0.0089(10) 0.0044(10) N12 0.0291(14) 0.0205(12) 0.0312(15) 0.0054(11) 0.0102(11) 0.0051(10) C1 0.0262(16) 0.0283(16) 0.0328(17) 0.0087(13) 0.0124(13) 0.0079(13) C2 0.0390(19) 0.0356(18) 0.0303(17) 0.0010(15) 0.0171(15) 0.0081(15) C3 0.0412(19) 0.0334(17) 0.0293(17) -0.0017(14) 0.0113(15) -0.0006(15) C4 0.0247(16) 0.0348(18) 0.0322(17) 0.0008(14) 0.0048(13) 0.0012(13) C5 0.0235(14) 0.0223(14) 0.0271(15) 0.0029(12) 0.0079(12) 0.0019(12) C6 0.0212(14) 0.0242(15) 0.0288(16) 0.0004(13) 0.0065(12) 0.0005(12) C7 0.0205(15) 0.0312(16) 0.0338(18) -0.0037(14) 0.0066(13) 0.0004(12) C8 0.0204(14) 0.0301(17) 0.0356(17) 0.0008(14) 0.0082(12) 0.0013(13) C9 0.0228(15) 0.0319(16) 0.0336(17) -0.0023(14) 0.0127(13) -0.0003(12) C10 0.0225(15) 0.0256(15) 0.0282(16) 0.0014(12) 0.0106(12) 0.0007(12) C11 0.0220(14) 0.0237(14) 0.0270(16) 0.0009(12) 0.0080(12) -0.0015(11) C12 0.0240(15) 0.0367(18) 0.0369(17) -0.0043(15) 0.0137(13) -0.0053(13) C13 0.0333(17) 0.0381(19) 0.0294(16) -0.0065(15) 0.0113(14) -0.0103(15) C14 0.0299(16) 0.0285(16) 0.0311(16) 0.0000(15) 0.0044(13) -0.0082(14) C15 0.0219(14) 0.0206(14) 0.0339(17) 0.0058(13) 0.0046(12) -0.0022(11) C16 0.0212(14) 0.0282(16) 0.0274(16) 0.0020(13) 0.0070(12) 0.0032(12) C17 0.0255(16) 0.0266(15) 0.0375(19) 0.0072(14) 0.0076(13) 0.0061(13) C18 0.0342(17) 0.0232(15) 0.0390(18) 0.0078(14) 0.0109(14) 0.0023(13) C19 0.0261(15) 0.0251(15) 0.0318(17) 0.0081(13) 0.0108(13) 0.0008(12) C20 0.0198(13) 0.0230(14) 0.0269(15) 0.0037(12) 0.0071(11) 0.0020(11) C21 0.0199(14) 0.0207(14) 0.0262(15) 0.0024(12) 0.0051(12) -0.0007(11) C22 0.0215(14) 0.0247(15) 0.0319(17) 0.0050(13) 0.0081(12) -0.0012(12) C23 0.0198(13) 0.0249(15) 0.0250(14) -0.0013(13) 0.0050(11) 0.0002(12) C24 0.0203(14) 0.0223(14) 0.0328(17) 0.0023(13) 0.0074(12) 0.0017(11) C25 0.0203(14) 0.0208(14) 0.0243(15) 0.0032(12) 0.0052(11) 0.0006(11) C26 0.0211(14) 0.0211(13) 0.0275(16) 0.0015(12) 0.0079(12) 0.0006(11) C27 0.0264(16) 0.0239(15) 0.0349(18) 0.0053(13) 0.0076(13) 0.0030(12) C28 0.0348(17) 0.0216(15) 0.0390(18) 0.0068(14) 0.0110(14) 0.0020(13) C29 0.0324(17) 0.0271(16) 0.0352(18) 0.0043(14) 0.0114(14) -0.0066(13) C30 0.0248(14) 0.0258(15) 0.0329(16) 0.0004(14) 0.0110(12) -0.0016(12) C31 0.0182(14) 0.0372(18) 0.0332(17) 0.0008(14) 0.0076(12) 0.0033(13) C32 0.0223(15) 0.0311(17) 0.044(2) 0.0004(15) 0.0083(14) 0.0020(13) C33 0.0263(16) 0.0355(18) 0.040(2) 0.0040(15) 0.0106(14) 0.0054(14) C34 0.0186(14) 0.0428(19) 0.0299(16) 0.0091(14) 0.0071(12) 0.0034(13) C35 0.0225(16) 0.042(2) 0.040(2) -0.0052(16) 0.0070(14) -0.0045(14) C36 0.0228(16) 0.0394(19) 0.040(2) -0.0097(16) 0.0090(14) 0.0014(14) C37 0.0195(15) 0.054(2) 0.0333(17) 0.0092(17) 0.0086(13) 0.0018(16) C38 0.0177(16) 0.083(3) 0.055(2) 0.009(2) 0.0109(16) -0.0065(18) C39 0.0192(13) 0.0252(15) 0.0261(14) 0.0000(13) 0.0067(11) 0.0012(12) C40 0.0216(15) 0.0294(16) 0.0388(19) 0.0091(14) 0.0091(13) 0.0054(12) C41 0.0246(16) 0.0242(15) 0.0396(19) 0.0056(14) 0.0120(14) 0.0013(12) C42 0.0166(13) 0.0308(16) 0.0271(15) -0.0025(14) 0.0065(11) 0.0008(12) C43 0.0207(15) 0.0258(16) 0.048(2) 0.0054(15) 0.0088(14) 0.0045(12) C44 0.0237(16) 0.0244(15) 0.050(2) 0.0052(15) 0.0119(14) 0.0007(12) C45 0.0212(14) 0.0291(15) 0.0301(15) -0.0027(14) 0.0097(12) -0.0010(13) C46 0.0194(16) 0.047(2) 0.058(2) 0.0034(19) 0.0046(15) 0.0018(15) C47 0.0270(15) 0.0239(15) 0.0331(16) 0.0026(14) 0.0129(12) 0.0013(13) C48 0.0374(18) 0.0261(16) 0.0388(19) 0.0052(14) 0.0191(15) -0.0045(14) C49 0.0374(18) 0.0216(15) 0.0352(17) 0.0065(13) 0.0126(14) 0.0015(13) C50 0.0291(16) 0.0197(14) 0.0370(18) 0.0030(13) 0.0116(14) 0.0023(12) C51 0.0256(15) 0.0207(14) 0.0285(16) 0.0016(12) 0.0097(12) 0.0017(12) C52 0.0265(15) 0.0173(13) 0.0300(16) 0.0028(12) 0.0082(12) 0.0023(12) C53 0.0244(15) 0.0242(15) 0.0313(17) 0.0025(13) 0.0071(13) 0.0052(12) C54 0.0213(14) 0.0213(14) 0.0270(15) -0.0002(12) 0.0078(11) -0.0014(11) C55 0.0250(15) 0.0191(14) 0.0331(17) 0.0047(12) 0.0084(12) 0.0007(11) C56 0.0256(15) 0.0179(13) 0.0281(16) 0.0038(12) 0.0094(12) 0.0007(11) C57 0.0235(14) 0.0219(14) 0.0251(15) 0.0009(12) 0.0074(12) 0.0028(11) C58 0.0268(16) 0.0250(15) 0.0347(17) 0.0042(14) 0.0085(13) -0.0006(12) C59 0.0380(18) 0.0221(15) 0.0368(18) 0.0083(14) 0.0068(14) 0.0012(14) C60 0.0330(17) 0.0232(16) 0.0374(19) 0.0076(14) 0.0058(14) 0.0077(13) C61 0.0254(16) 0.0270(15) 0.0300(17) 0.0027(13) 0.0041(13) 0.0057(13) C62 0.0263(15) 0.0216(14) 0.0340(17) 0.0045(13) 0.0085(13) 0.0009(12) C63 0.0382(18) 0.0224(15) 0.0306(17) -0.0023(13) 0.0064(14) -0.0030(13) C64 0.0404(19) 0.0281(16) 0.0339(18) -0.0046(14) 0.0153(15) -0.0018(14) C65 0.0276(15) 0.0286(16) 0.0405(18) -0.0050(15) 0.0165(13) -0.0026(14) C66 0.0253(15) 0.0208(14) 0.0343(17) 0.0010(13) 0.0108(13) 0.0001(12) C67 0.0227(15) 0.0217(14) 0.0322(16) -0.0004(12) 0.0115(13) 0.0022(11) C68 0.0272(16) 0.0286(16) 0.0358(18) -0.0018(14) 0.0137(14) 0.0036(13) C69 0.0206(14) 0.0257(15) 0.0386(18) 0.0054(14) 0.0080(12) 0.0020(13) C70 0.0255(15) 0.0268(16) 0.0324(17) -0.0002(13) 0.0078(13) 0.0004(12) C71 0.0253(15) 0.0198(14) 0.0315(17) 0.0019(13) 0.0088(13) 0.0005(12) C72 0.0291(16) 0.0223(15) 0.0329(17) 0.0070(13) 0.0121(13) 0.0029(12) C73 0.0358(18) 0.0314(17) 0.0309(17) 0.0034(14) 0.0081(14) 0.0013(14) C74 0.050(2) 0.0326(18) 0.0325(19) 0.0017(15) 0.0145(16) 0.0079(16) C75 0.048(2) 0.0360(19) 0.0334(18) 0.0067(15) 0.0213(16) 0.0140(16) C76 0.0329(17) 0.0265(16) 0.0341(18) 0.0098(14) 0.0152(14) 0.0084(13) C77 0.0233(14) 0.0230(15) 0.0262(14) -0.0001(12) 0.0071(11) 0.0011(12) C78 0.0254(16) 0.0266(16) 0.0399(19) 0.0082(14) 0.0107(14) 0.0006(13) C79 0.0255(16) 0.0262(16) 0.0420(19) 0.0071(15) 0.0094(14) 0.0035(13) C80 0.0229(14) 0.0247(15) 0.0296(15) -0.0006(13) 0.0081(12) -0.0015(12) C81 0.0256(16) 0.0245(15) 0.0384(18) 0.0052(13) 0.0132(14) -0.0004(12) C82 0.0281(16) 0.0264(15) 0.0399(19) 0.0080(14) 0.0126(14) 0.0040(13) C83 0.0270(16) 0.0307(17) 0.0298(16) 0.0014(14) 0.0090(13) 0.0021(13) C84 0.0285(18) 0.049(2) 0.058(3) 0.008(2) 0.0111(17) 0.0074(16) C85 0.0216(14) 0.0328(17) 0.0305(16) 0.0039(14) 0.0077(12) 0.0011(13) C86 0.0285(17) 0.0375(19) 0.041(2) -0.0056(16) 0.0085(15) 0.0000(14) C87 0.0284(17) 0.044(2) 0.0354(19) -0.0056(16) 0.0073(14) -0.0047(15) C88 0.0242(15) 0.045(2) 0.0305(17) 0.0104(15) 0.0085(13) 0.0045(14) C89 0.0296(17) 0.0363(18) 0.044(2) 0.0059(16) 0.0136(15) 0.0058(14) C90 0.0283(17) 0.0312(17) 0.047(2) 0.0046(16) 0.0134(15) 0.0015(14) C91 0.0268(17) 0.056(2) 0.0359(19) 0.0105(17) 0.0104(14) 0.0008(17) C92 0.0223(18) 0.101(4) 0.054(3) -0.003(3) 0.0057(17) -0.008(2) O1 0.0212(12) 0.0591(17) 0.0528(17) 0.0035(14) 0.0103(11) -0.0055(12) O2 0.0231(13) 0.0603(19) 0.089(2) 0.0037(17) 0.0158(14) 0.0081(13) O3 0.0187(11) 0.0332(13) 0.0550(16) 0.0066(12) 0.0059(10) 0.0026(9) O4 0.0226(11) 0.0375(13) 0.0464(15) 0.0019(11) 0.0107(10) -0.0022(10) O5 0.0239(12) 0.0390(14) 0.0572(16) 0.0133(12) 0.0126(11) 0.0074(10) O6 0.0294(13) 0.0385(14) 0.0527(16) 0.0092(12) 0.0159(11) -0.0016(11) O7 0.0250(13) 0.076(2) 0.0461(16) -0.0088(15) 0.0063(11) -0.0026(13) O8 0.0307(14) 0.0578(19) 0.090(2) 0.0097(18) 0.0177(15) 0.0112(14) O9 0.0362(15) 0.073(2) 0.0636(19) 0.0013(17) 0.0120(13) -0.0125(15) O10 0.0506(18) 0.0507(18) 0.097(3) -0.0035(18) 0.0383(18) -0.0057(15) O11 0.0377(18) 0.087(3) 0.131(4) 0.033(3) 0.001(2) -0.0191(18) O12 0.0467(19) 0.083(3) 0.128(3) 0.045(2) 0.043(2) 0.0102(18) O13 0.069(2) 0.100(3) 0.114(3) 0.061(3) 0.053(2) 0.046(2) O14 0.065(3) 0.143(5) 0.154(5) -0.032(4) -0.018(3) 0.059(3) O15 0.085(3) 0.111(4) 0.092(3) -0.006(3) 0.016(2) 0.040(3) O160 0.097(7) 0.097(7) 0.085(7) -0.009(6) 0.046(6) -0.008(6) O161 0.154(11) 0.168(13) 0.052(5) -0.014(7) 0.006(6) 0.017(10) Cl1 0.0336(4) 0.0424(5) 0.0596(6) -0.0058(4) 0.0129(4) -0.0078(4) Cl2 0.0253(4) 0.0414(5) 0.1048(9) 0.0118(6) 0.0128(5) 0.0032(4) Cl3 0.0441(8) 0.0776(11) 0.0573(9) 0.0000 0.0222(7) 0.0000 Cl4 0.0327(9) 0.0522(11) 0.0562(11) -0.0208(10) 0.0159(8) -0.0152(8) Cl5 0.0237(7) 0.0505(10) 0.0370(8) -0.0052(8) 0.0000(6) -0.0077(7) Cl6 0.0520(13) 0.0991(19) 0.0660(14) -0.0261(14) 0.0353(11) -0.0458(13) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3903(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru1 . N1 . 2.067(3) yes Ru1 . N2 . 1.969(2) yes Ru1 . N3 . 2.064(3) yes Ru1 . N4 . 2.069(3) yes Ru1 . N5 . 1.971(2) yes Ru1 . N6 . 2.069(3) yes Ru2 . N7 . 2.077(2) yes Ru2 . N8 . 1.973(3) yes Ru2 . N9 . 2.068(3) yes Ru2 . N10 . 2.058(3) yes Ru2 . N11 . 1.971(3) yes Ru2 . N12 . 2.066(3) yes N1 . C1 . 1.340(4) yes N1 . C5 . 1.373(4) yes N2 . C6 . 1.355(4) yes N2 . C10 . 1.357(4) yes N3 . C11 . 1.369(4) yes N3 . C15 . 1.336(4) yes N4 . C16 . 1.340(4) yes N4 . C20 . 1.371(4) yes N5 . C21 . 1.342(4) yes N5 . C25 . 1.352(4) yes N6 . C26 . 1.366(4) yes N6 . C30 . 1.341(4) yes N7 . C47 . 1.344(4) yes N7 . C51 . 1.367(4) yes N8 . C52 . 1.354(4) yes N8 . C56 . 1.352(4) yes N9 . C57 . 1.362(4) yes N9 . C61 . 1.343(4) yes N10 . C62 . 1.342(4) yes N10 . C66 . 1.367(4) yes N11 . C67 . 1.361(4) yes N11 . C71 . 1.342(4) yes N12 . C72 . 1.368(4) yes N12 . C76 . 1.341(4) yes C1 . C2 . 1.380(5) yes C1 . H11 . 0.937 no C2 . C3 . 1.372(5) yes C2 . H21 . 0.940 no C3 . C4 . 1.385(5) yes C3 . H31 . 0.940 no C4 . C5 . 1.382(5) yes C4 . H41 . 0.934 no C5 . C6 . 1.470(4) yes C6 . C7 . 1.381(4) yes C7 . C8 . 1.396(5) yes C7 . H71 . 0.945 no C8 . C9 . 1.391(5) yes C8 . C31 . 1.484(4) yes C9 . C10 . 1.386(4) yes C9 . H91 . 0.950 no C10 . C11 . 1.468(4) yes C11 . C12 . 1.385(5) yes C12 . C13 . 1.392(5) yes C12 . H121 . 0.941 no C13 . C14 . 1.376(5) yes C13 . H131 . 0.938 no C14 . C15 . 1.383(5) yes C14 . H141 . 0.945 no C15 . H151 . 0.934 no C16 . C17 . 1.380(5) yes C16 . H161 . 0.935 no C17 . C18 . 1.388(5) yes C17 . H171 . 0.948 no C18 . C19 . 1.381(4) yes C18 . H181 . 0.943 no C19 . C20 . 1.382(4) yes C19 . H191 . 0.947 no C20 . C21 . 1.475(4) yes C21 . C22 . 1.383(4) yes C22 . C23 . 1.400(4) yes C22 . H221 . 0.930 no C23 . C24 . 1.399(4) yes C23 . C39 . 1.486(4) yes C24 . C25 . 1.388(4) yes C24 . H241 . 0.935 no C25 . C26 . 1.475(4) yes C26 . C27 . 1.391(4) yes C27 . C28 . 1.376(5) yes C27 . H271 . 0.931 no C28 . C29 . 1.383(5) yes C28 . H281 . 0.925 no C29 . C30 . 1.385(5) yes C29 . H291 . 0.935 no C30 . H301 . 0.931 no C31 . C32 . 1.392(5) yes C31 . C36 . 1.387(5) yes C32 . C33 . 1.381(5) yes C32 . H321 . 0.938 no C33 . C34 . 1.380(5) yes C33 . H331 . 0.943 no C34 . C35 . 1.396(5) yes C34 . C37 . 1.488(4) yes C35 . C36 . 1.391(5) yes C35 . H351 . 0.931 no C36 . H361 . 0.926 no C37 . O1 . 1.325(5) yes C37 . O2 . 1.206(5) yes C38 . O1 . 1.454(4) yes C38 . H381 . 0.955 no C38 . H382 . 0.966 no C38 . H383 . 0.969 no C39 . C40 . 1.400(4) yes C39 . C44 . 1.392(4) yes C40 . C41 . 1.382(4) yes C40 . H401 . 0.930 no C41 . C42 . 1.390(4) yes C41 . H411 . 0.939 no C42 . C43 . 1.382(5) yes C42 . C45 . 1.489(4) yes C43 . C44 . 1.389(4) yes C43 . H431 . 0.929 no C44 . H441 . 0.941 no C45 . O3 . 1.318(4) yes C45 . O4 . 1.214(4) yes C46 . O3 . 1.449(4) yes C46 . H461 . 0.963 no C46 . H462 . 0.964 no C46 . H463 . 0.957 no C47 . C48 . 1.384(5) yes C47 . H471 . 0.929 no C48 . C49 . 1.383(5) yes C48 . H481 . 0.926 no C49 . C50 . 1.384(5) yes C49 . H491 . 0.934 no C50 . C51 . 1.384(4) yes C50 . H501 . 0.936 no C51 . C52 . 1.477(4) yes C52 . C53 . 1.380(4) yes C53 . C54 . 1.405(4) yes C53 . H531 . 0.940 no C54 . C55 . 1.404(4) yes C54 . C77 . 1.489(4) yes C55 . C56 . 1.377(4) yes C55 . H551 . 0.926 no C56 . C57 . 1.472(4) yes C57 . C58 . 1.385(4) yes C58 . C59 . 1.381(5) yes C58 . H581 . 0.943 no C59 . C60 . 1.370(5) yes C59 . H591 . 0.942 no C60 . C61 . 1.387(5) yes C60 . H601 . 0.942 no C61 . H611 . 0.941 no C62 . C63 . 1.385(5) yes C62 . H621 . 0.938 no C63 . C64 . 1.390(5) yes C63 . H631 . 0.945 no C64 . C65 . 1.374(5) yes C64 . H641 . 0.936 no C65 . C66 . 1.393(5) yes C65 . H651 . 0.935 no C66 . C67 . 1.465(5) yes C67 . C68 . 1.387(4) yes C68 . C69 . 1.393(5) yes C68 . H681 . 0.931 no C69 . C70 . 1.399(5) yes C69 . C85 . 1.481(4) yes C70 . C71 . 1.392(4) yes C70 . H701 . 0.945 no C71 . C72 . 1.475(4) yes C72 . C73 . 1.385(5) yes C73 . C74 . 1.385(5) yes C73 . H731 . 0.929 no C74 . C75 . 1.380(6) yes C74 . H741 . 0.946 no C75 . C76 . 1.388(5) yes C75 . H751 . 0.941 no C76 . H761 . 0.941 no C77 . C78 . 1.388(4) yes C77 . C82 . 1.392(4) yes C78 . C79 . 1.379(5) yes C78 . H781 . 0.931 no C79 . C80 . 1.391(5) yes C79 . H791 . 0.937 no C80 . C81 . 1.391(4) yes C80 . C83 . 1.484(4) yes C81 . C82 . 1.394(5) yes C81 . H811 . 0.930 no C82 . H821 . 0.947 no C83 . O5 . 1.331(4) yes C83 . O6 . 1.210(4) yes C84 . O5 . 1.451(4) yes C84 . H841 . 0.963 no C84 . H842 . 0.960 no C84 . H843 . 0.963 no C85 . C86 . 1.391(5) yes C85 . C90 . 1.397(5) yes C86 . C87 . 1.379(5) yes C86 . H861 . 0.943 no C87 . C88 . 1.390(5) yes C87 . H871 . 0.937 no C88 . C89 . 1.392(5) yes C88 . C91 . 1.485(5) yes C89 . C90 . 1.374(5) yes C89 . H891 . 0.929 no C90 . H901 . 0.942 no C91 . O7 . 1.331(5) yes C91 . O8 . 1.213(5) yes C92 . O7 . 1.451(4) yes C92 . H921 . 0.963 no C92 . H922 . 0.963 no C92 . H923 . 0.965 no O9 . H90 . 0.831 no O9 . H95 . 0.864 no O10 . H100 . 0.836 no O10 . H105 . 0.818 no O11 . H110 . 0.829 no O11 . H115 . 0.865 no O12 . H120 . 0.830 no O12 . H125 . 0.829 no O13 . H130 . 0.829 no O13 . H135 . 0.826 no O14 . H140 . 0.816 no O14 . H145 . 0.815 no O15 . H150 . 0.915 no O15 . H155 . 0.843 no O160 . O161 . 1.077(14) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Ru1 . N2 . 78.84(10) yes N1 . Ru1 . N3 . 158.25(10) yes N2 . Ru1 . N3 . 79.41(10) yes N1 . Ru1 . N4 . 94.49(10) yes N2 . Ru1 . N4 . 101.31(10) yes N3 . Ru1 . N4 . 89.81(10) yes N1 . Ru1 . N5 . 100.06(10) yes N2 . Ru1 . N5 . 178.83(10) yes N3 . Ru1 . N5 . 101.69(10) yes N4 . Ru1 . N5 . 79.16(10) yes N1 . Ru1 . N6 . 91.07(10) yes N2 . Ru1 . N6 . 100.51(10) yes N3 . Ru1 . N6 . 92.82(10) yes N4 . Ru1 . N6 . 158.14(10) yes N5 . Ru1 . N6 . 79.06(10) yes N7 . Ru2 . N8 . 78.47(10) yes N7 . Ru2 . N9 . 157.43(10) yes N8 . Ru2 . N9 . 79.14(10) yes N7 . Ru2 . N10 . 93.00(10) yes N8 . Ru2 . N10 . 101.93(10) yes N9 . Ru2 . N10 . 88.86(10) yes N7 . Ru2 . N11 . 101.89(10) yes N8 . Ru2 . N11 . 178.75(11) yes N9 . Ru2 . N11 . 100.56(10) yes N10 . Ru2 . N11 . 79.26(11) yes N7 . Ru2 . N12 . 91.97(10) yes N8 . Ru2 . N12 . 100.13(11) yes N9 . Ru2 . N12 . 94.70(10) yes N10 . Ru2 . N12 . 157.93(10) yes N11 . Ru2 . N12 . 78.68(11) yes Ru1 . N1 . C1 . 127.8(2) yes Ru1 . N1 . C5 . 113.9(2) yes C1 . N1 . C5 . 118.2(3) yes Ru1 . N2 . C6 . 119.9(2) yes Ru1 . N2 . C10 . 118.8(2) yes C6 . N2 . C10 . 121.3(3) yes Ru1 . N3 . C11 . 113.7(2) yes Ru1 . N3 . C15 . 127.6(2) yes C11 . N3 . C15 . 118.7(3) yes Ru1 . N4 . C16 . 127.5(2) yes Ru1 . N4 . C20 . 113.49(19) yes C16 . N4 . C20 . 118.8(3) yes Ru1 . N5 . C21 . 119.5(2) yes Ru1 . N5 . C25 . 119.59(19) yes C21 . N5 . C25 . 120.9(2) yes Ru1 . N6 . C26 . 113.71(19) yes Ru1 . N6 . C30 . 127.6(2) yes C26 . N6 . C30 . 118.7(3) yes Ru2 . N7 . C47 . 127.3(2) yes Ru2 . N7 . C51 . 114.15(19) yes C47 . N7 . C51 . 118.5(3) yes Ru2 . N8 . C52 . 120.2(2) yes Ru2 . N8 . C56 . 119.3(2) yes C52 . N8 . C56 . 120.4(3) yes Ru2 . N9 . C57 . 113.46(19) yes Ru2 . N9 . C61 . 127.6(2) yes C57 . N9 . C61 . 118.7(3) yes Ru2 . N10 . C62 . 126.6(2) yes Ru2 . N10 . C66 . 114.0(2) yes C62 . N10 . C66 . 119.3(3) yes Ru2 . N11 . C67 . 118.8(2) yes Ru2 . N11 . C71 . 119.7(2) yes C67 . N11 . C71 . 121.5(3) yes Ru2 . N12 . C72 . 114.3(2) yes Ru2 . N12 . C76 . 127.5(2) yes C72 . N12 . C76 . 118.2(3) yes N1 . C1 . C2 . 122.6(3) yes N1 . C1 . H11 . 117.9 no C2 . C1 . H11 . 119.5 no C1 . C2 . C3 . 119.3(3) yes C1 . C2 . H21 . 119.3 no C3 . C2 . H21 . 121.4 no C2 . C3 . C4 . 119.3(3) yes C2 . C3 . H31 . 120.7 no C4 . C3 . H31 . 119.9 no C3 . C4 . C5 . 119.2(3) yes C3 . C4 . H41 . 120.9 no C5 . C4 . H41 . 119.9 no C4 . C5 . N1 . 121.4(3) yes C4 . C5 . C6 . 123.4(3) yes N1 . C5 . C6 . 115.2(3) yes C5 . C6 . N2 . 112.0(3) yes C5 . C6 . C7 . 127.6(3) yes N2 . C6 . C7 . 120.4(3) yes C6 . C7 . C8 . 119.3(3) yes C6 . C7 . H71 . 120.0 no C8 . C7 . H71 . 120.7 no C7 . C8 . C9 . 119.6(3) yes C7 . C8 . C31 . 121.0(3) yes C9 . C8 . C31 . 119.4(3) yes C8 . C9 . C10 . 119.2(3) yes C8 . C9 . H91 . 120.4 no C10 . C9 . H91 . 120.4 no C9 . C10 . N2 . 120.2(3) yes C9 . C10 . C11 . 127.0(3) yes N2 . C10 . C11 . 112.8(3) yes C10 . C11 . N3 . 115.2(3) yes C10 . C11 . C12 . 123.5(3) yes N3 . C11 . C12 . 121.2(3) yes C11 . C12 . C13 . 119.2(3) yes C11 . C12 . H121 . 120.4 no C13 . C12 . H121 . 120.4 no C12 . C13 . C14 . 119.0(3) yes C12 . C13 . H131 . 121.0 no C14 . C13 . H131 . 120.0 no C13 . C14 . C15 . 119.4(3) yes C13 . C14 . H141 . 120.6 no C15 . C14 . H141 . 120.0 no C14 . C15 . N3 . 122.4(3) yes C14 . C15 . H151 . 119.1 no N3 . C15 . H151 . 118.5 no N4 . C16 . C17 . 122.3(3) yes N4 . C16 . H161 . 117.8 no C17 . C16 . H161 . 119.8 no C16 . C17 . C18 . 119.1(3) yes C16 . C17 . H171 . 119.9 no C18 . C17 . H171 . 120.9 no C17 . C18 . C19 . 118.9(3) yes C17 . C18 . H181 . 120.9 no C19 . C18 . H181 . 120.1 no C18 . C19 . C20 . 119.8(3) yes C18 . C19 . H191 . 120.3 no C20 . C19 . H191 . 119.9 no C19 . C20 . N4 . 120.9(3) yes C19 . C20 . C21 . 123.8(3) yes N4 . C20 . C21 . 115.2(3) yes C20 . C21 . N5 . 112.6(3) yes C20 . C21 . C22 . 126.6(3) yes N5 . C21 . C22 . 120.8(3) yes C21 . C22 . C23 . 120.1(3) yes C21 . C22 . H221 . 119.3 no C23 . C22 . H221 . 120.6 no C22 . C23 . C24 . 117.8(3) yes C22 . C23 . C39 . 120.7(3) yes C24 . C23 . C39 . 121.5(3) yes C23 . C24 . C25 . 120.0(3) yes C23 . C24 . H241 . 119.9 no C25 . C24 . H241 . 120.1 no C24 . C25 . N5 . 120.5(3) yes C24 . C25 . C26 . 127.4(3) yes N5 . C25 . C26 . 112.1(2) yes C25 . C26 . N6 . 115.5(3) yes C25 . C26 . C27 . 123.5(3) yes N6 . C26 . C27 . 120.9(3) yes C26 . C27 . C28 . 119.8(3) yes C26 . C27 . H271 . 120.0 no C28 . C27 . H271 . 120.2 no C27 . C28 . C29 . 119.1(3) yes C27 . C28 . H281 . 119.6 no C29 . C28 . H281 . 121.2 no C28 . C29 . C30 . 119.0(3) yes C28 . C29 . H291 . 122.0 no C30 . C29 . H291 . 119.0 no C29 . C30 . N6 . 122.5(3) yes C29 . C30 . H301 . 118.6 no N6 . C30 . H301 . 118.9 no C8 . C31 . C32 . 119.0(3) yes C8 . C31 . C36 . 121.4(3) yes C32 . C31 . C36 . 119.6(3) yes C31 . C32 . C33 . 120.3(3) yes C31 . C32 . H321 . 119.6 no C33 . C32 . H321 . 120.2 no C32 . C33 . C34 . 120.4(3) yes C32 . C33 . H331 . 119.7 no C34 . C33 . H331 . 120.0 no C33 . C34 . C35 . 119.8(3) yes C33 . C34 . C37 . 118.0(3) yes C35 . C34 . C37 . 122.1(3) yes C34 . C35 . C36 . 119.9(3) yes C34 . C35 . H351 . 120.6 no C36 . C35 . H351 . 119.5 no C35 . C36 . C31 . 120.0(3) yes C35 . C36 . H361 . 119.9 no C31 . C36 . H361 . 120.1 no C34 . C37 . O1 . 112.8(3) yes C34 . C37 . O2 . 122.8(4) yes O1 . C37 . O2 . 124.4(3) yes O1 . C38 . H381 . 109.8 no O1 . C38 . H382 . 107.3 no H381 . C38 . H382 . 109.9 no O1 . C38 . H383 . 109.6 no H381 . C38 . H383 . 110.5 no H382 . C38 . H383 . 109.8 no C23 . C39 . C40 . 120.8(3) yes C23 . C39 . C44 . 121.2(3) yes C40 . C39 . C44 . 118.0(3) yes C39 . C40 . C41 . 120.8(3) yes C39 . C40 . H401 . 119.3 no C41 . C40 . H401 . 120.0 no C40 . C41 . C42 . 120.9(3) yes C40 . C41 . H411 . 120.6 no C42 . C41 . H411 . 118.5 no C41 . C42 . C43 . 118.6(3) yes C41 . C42 . C45 . 119.0(3) yes C43 . C42 . C45 . 122.3(3) yes C42 . C43 . C44 . 120.9(3) yes C42 . C43 . H431 . 118.8 no C44 . C43 . H431 . 120.3 no C39 . C44 . C43 . 120.8(3) yes C39 . C44 . H441 . 119.4 no C43 . C44 . H441 . 119.8 no C42 . C45 . O3 . 112.2(3) yes C42 . C45 . O4 . 123.6(3) yes O3 . C45 . O4 . 124.1(3) yes O3 . C46 . H461 . 107.6 no O3 . C46 . H462 . 108.8 no H461 . C46 . H462 . 109.8 no O3 . C46 . H463 . 110.9 no H461 . C46 . H463 . 109.5 no H462 . C46 . H463 . 110.2 no N7 . C47 . C48 . 122.3(3) yes N7 . C47 . H471 . 117.3 no C48 . C47 . H471 . 120.4 no C47 . C48 . C49 . 119.3(3) yes C47 . C48 . H481 . 120.0 no C49 . C48 . H481 . 120.8 no C48 . C49 . C50 . 119.0(3) yes C48 . C49 . H491 . 120.5 no C50 . C49 . H491 . 120.5 no C49 . C50 . C51 . 119.5(3) yes C49 . C50 . H501 . 120.8 no C51 . C50 . H501 . 119.7 no C50 . C51 . N7 . 121.4(3) yes C50 . C51 . C52 . 123.3(3) yes N7 . C51 . C52 . 115.2(3) yes C51 . C52 . N8 . 111.8(3) yes C51 . C52 . C53 . 127.0(3) yes N8 . C52 . C53 . 121.2(3) yes C52 . C53 . C54 . 119.6(3) yes C52 . C53 . H531 . 119.9 no C54 . C53 . H531 . 120.6 no C53 . C54 . C55 . 117.8(3) yes C53 . C54 . C77 . 121.3(3) yes C55 . C54 . C77 . 120.9(3) yes C54 . C55 . C56 . 120.2(3) yes C54 . C55 . H551 . 120.3 no C56 . C55 . H551 . 119.5 no C55 . C56 . N8 . 120.7(3) yes C55 . C56 . C57 . 127.3(3) yes N8 . C56 . C57 . 112.0(3) yes C56 . C57 . N9 . 115.9(3) yes C56 . C57 . C58 . 122.7(3) yes N9 . C57 . C58 . 121.4(3) yes C57 . C58 . C59 . 119.2(3) yes C57 . C58 . H581 . 120.1 no C59 . C58 . H581 . 120.7 no C58 . C59 . C60 . 119.5(3) yes C58 . C59 . H591 . 120.5 no C60 . C59 . H591 . 120.0 no C59 . C60 . C61 . 119.3(3) yes C59 . C60 . H601 . 121.2 no C61 . C60 . H601 . 119.5 no C60 . C61 . N9 . 121.9(3) yes C60 . C61 . H611 . 119.9 no N9 . C61 . H611 . 118.1 no N10 . C62 . C63 . 121.7(3) yes N10 . C62 . H621 . 118.9 no C63 . C62 . H621 . 119.4 no C62 . C63 . C64 . 119.5(3) yes C62 . C63 . H631 . 119.3 no C64 . C63 . H631 . 121.2 no C63 . C64 . C65 . 119.1(3) yes C63 . C64 . H641 . 120.4 no C65 . C64 . H641 . 120.5 no C64 . C65 . C66 . 119.6(3) yes C64 . C65 . H651 . 120.0 no C66 . C65 . H651 . 120.4 no C65 . C66 . N10 . 120.9(3) yes C65 . C66 . C67 . 123.9(3) yes N10 . C66 . C67 . 115.2(3) yes C66 . C67 . N11 . 112.6(3) yes C66 . C67 . C68 . 127.4(3) yes N11 . C67 . C68 . 120.0(3) yes C67 . C68 . C69 . 119.8(3) yes C67 . C68 . H681 . 119.8 no C69 . C68 . H681 . 120.4 no C68 . C69 . C70 . 118.9(3) yes C68 . C69 . C85 . 120.2(3) yes C70 . C69 . C85 . 120.9(3) yes C69 . C70 . C71 . 119.4(3) yes C69 . C70 . H701 . 118.8 no C71 . C70 . H701 . 121.8 no C70 . C71 . N11 . 120.4(3) yes C70 . C71 . C72 . 126.9(3) yes N11 . C71 . C72 . 112.7(3) yes C71 . C72 . N12 . 114.5(3) yes C71 . C72 . C73 . 123.7(3) yes N12 . C72 . C73 . 121.7(3) yes C72 . C73 . C74 . 119.0(3) yes C72 . C73 . H731 . 120.5 no C74 . C73 . H731 . 120.5 no C73 . C74 . C75 . 119.6(3) yes C73 . C74 . H741 . 119.9 no C75 . C74 . H741 . 120.5 no C74 . C75 . C76 . 118.7(3) yes C74 . C75 . H751 . 121.9 no C76 . C75 . H751 . 119.5 no C75 . C76 . N12 . 122.7(3) yes C75 . C76 . H761 . 119.0 no N12 . C76 . H761 . 118.2 no C54 . C77 . C78 . 121.5(3) yes C54 . C77 . C82 . 120.5(3) yes C78 . C77 . C82 . 118.0(3) yes C77 . C78 . C79 . 121.4(3) yes C77 . C78 . H781 . 120.7 no C79 . C78 . H781 . 117.9 no C78 . C79 . C80 . 120.6(3) yes C78 . C79 . H791 . 119.8 no C80 . C79 . H791 . 119.6 no C79 . C80 . C81 . 118.9(3) yes C79 . C80 . C83 . 121.8(3) yes C81 . C80 . C83 . 119.3(3) yes C80 . C81 . C82 . 120.1(3) yes C80 . C81 . H811 . 119.5 no C82 . C81 . H811 . 120.4 no C81 . C82 . C77 . 121.1(3) yes C81 . C82 . H821 . 120.7 no C77 . C82 . H821 . 118.2 no C80 . C83 . O5 . 112.4(3) yes C80 . C83 . O6 . 124.0(3) yes O5 . C83 . O6 . 123.6(3) yes O5 . C84 . H841 . 110.1 no O5 . C84 . H842 . 110.6 no H841 . C84 . H842 . 108.9 no O5 . C84 . H843 . 108.9 no H841 . C84 . H843 . 109.7 no H842 . C84 . H843 . 108.6 no C69 . C85 . C86 . 121.2(3) yes C69 . C85 . C90 . 120.0(3) yes C86 . C85 . C90 . 118.8(3) yes C85 . C86 . C87 . 120.7(3) yes C85 . C86 . H861 . 119.6 no C87 . C86 . H861 . 119.7 no C86 . C87 . C88 . 120.3(3) yes C86 . C87 . H871 . 119.6 no C88 . C87 . H871 . 120.1 no C87 . C88 . C89 . 119.0(3) yes C87 . C88 . C91 . 123.4(3) yes C89 . C88 . C91 . 117.5(3) yes C88 . C89 . C90 . 120.7(3) yes C88 . C89 . H891 . 118.8 no C90 . C89 . H891 . 120.5 no C85 . C90 . C89 . 120.4(3) yes C85 . C90 . H901 . 119.8 no C89 . C90 . H901 . 119.9 no C88 . C91 . O7 . 112.1(3) yes C88 . C91 . O8 . 123.4(4) yes O7 . C91 . O8 . 124.4(3) yes O7 . C92 . H921 . 110.0 no O7 . C92 . H922 . 108.7 no H921 . C92 . H922 . 109.7 no O7 . C92 . H923 . 108.6 no H921 . C92 . H923 . 110.0 no H922 . C92 . H923 . 109.8 no C38 . O1 . C37 . 115.5(3) yes C46 . O3 . C45 . 116.2(3) yes C84 . O5 . C83 . 116.8(3) yes C92 . O7 . C91 . 116.0(3) yes H90 . O9 . H95 . 105.7 no H100 . O10 . H105 . 97.7 no H110 . O11 . H115 . 102.2 no H120 . O12 . H125 . 107.0 no H130 . O13 . H135 . 109.0 no H140 . O14 . H145 . 103.2 no H150 . O15 . H155 . 90.7 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag O10 . H100 . O4 . 160 0.84 2.14 2.945(2) yes O11 . H110 . O8 3_546 165 0.83 2.04 2.851(2) yes O12 . H120 . O13 . 165 0.83 1.92 2.734(2) yes O12 . H125 . O11 1_565 165 0.83 2.11 2.921(2) yes O13 . H135 . O2 2_667 161 0.83 2.00 2.797(2) yes # Attachment 'fs274.cif' data_fs274_123k _database_code_depnum_ccdc_archive 'CCDC 651823' _audit_creation_date 07-06-14 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title '9300939 fs274_123k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 8.6945(2) _cell_length_b 13.4822(3) _cell_length_c 16.5345(4) _cell_angle_alpha 93.1178(13) _cell_angle_beta 97.3730(14) _cell_angle_gamma 90.9146(15) _cell_volume 1918.80(8) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ru -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C44 H38 N6 O9 Ru1 # Dc = 1.55 Fooo = 908.00 Mu = 4.77 M = 895.89 # Found Formula = C44 H32 N6 O9 Ru1 # Dc = 1.54 FOOO = 908.00 Mu = 4.77 M = 889.84 _chemical_formula_sum 'C44 H38 N6 O9 Ru1' _chemical_formula_moiety 'C44 H28 N6 O4 Ru, 5(H2 O)' _chemical_compound_source ? _chemical_formula_weight 895.89 _cell_measurement_reflns_used 9075 _cell_measurement_theta_min 3 _cell_measurement_theta_max 28 _cell_measurement_temperature 123 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 0.477 # Sheldrick geometric approximatio 0.94 0.97 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 0.97 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 123 _diffrn_reflns_number 17959 _reflns_number_total 9123 _diffrn_reflns_av_R_equivalents 0.031 # Number of reflections with Friedels Law is 9123 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 9134 _diffrn_reflns_theta_min 2.935 _diffrn_reflns_theta_max 27.856 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.856 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min -17 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.60 _refine_diff_density_max 0.58 _refine_ls_number_reflns 5963 _refine_ls_number_restraints 6 _refine_ls_number_parameters 580 #_refine_ls_R_factor_ref 0.0393 _refine_ls_wR_factor_ref 0.0364 _refine_ls_goodness_of_fit_ref 1.1438 #_reflns_number_all 9078 _refine_ls_R_factor_all 0.0730 _refine_ls_wR_factor_all 0.1043 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5963 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_gt 0.0364 _refine_ls_shift/su_max 0.000787 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.01P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # start Validation Reply Form _vrf_PLAT430_fs274_123k ; PROBLEM: Short Inter D...A Contact O120 .. O140 .. 2.47 Ang. RESPONSE: Atoms are part of a hydrogen bond network, but not all hydrogen atoms could be located in the difference map, therefore these distances appear to be too short, but within a hydrogen bond network, they are acceptable. ; # end Validation Reply Form # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # The content below is held in the file 'script/refcif.dat'. This is a text # file which you may edit to reflect local conditions. # Items which need looking at are represented by a '?'. # Items for which there are choices are prefixed with 'choose from'. _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ru1 Ru 0.94012(3) 0.26784(2) 0.767420(16) 0.0184 1.0000 Uani . . . . . . N1 N 0.7169(3) 0.32189(18) 0.74440(15) 0.0182 1.0000 Uani . . . . . . N2 N 0.8974(3) 0.24585(18) 0.64730(14) 0.0164 1.0000 Uani . . . . . . N3 N 1.1468(3) 0.20874(18) 0.74087(15) 0.0168 1.0000 Uani . . . . . . N4 N 0.8570(3) 0.13373(18) 0.80042(14) 0.0167 1.0000 Uani . . . . . . N5 N 0.9902(3) 0.28150(18) 0.88725(14) 0.0164 1.0000 Uani . . . . . . N6 N 1.0355(3) 0.41003(18) 0.78307(15) 0.0186 1.0000 Uani . . . . . . C1 C 0.6314(3) 0.3656(2) 0.79834(19) 0.0224 1.0000 Uani . . . . . . C2 C 0.4875(3) 0.4040(2) 0.7744(2) 0.0258 1.0000 Uani . . . . . . C3 C 0.4283(4) 0.3987(2) 0.6926(2) 0.0277 1.0000 Uani . . . . . . C4 C 0.5126(3) 0.3531(2) 0.63666(19) 0.0237 1.0000 Uani . . . . . . C5 C 0.6566(3) 0.3151(2) 0.66376(18) 0.0187 1.0000 Uani . . . . . . C6 C 0.7550(3) 0.2663(2) 0.60803(18) 0.0185 1.0000 Uani . . . . . . C7 C 0.7170(3) 0.2396(2) 0.52651(18) 0.0212 1.0000 Uani . . . . . . C8 C 0.8267(3) 0.1950(2) 0.48240(18) 0.0211 1.0000 Uani . . . . . . C9 C 0.9744(3) 0.1793(2) 0.52345(18) 0.0235 1.0000 Uani . . . . . . C10 C 1.0060(3) 0.2038(2) 0.60621(18) 0.0187 1.0000 Uani . . . . . . C11 C 1.1521(3) 0.1865(2) 0.65925(19) 0.0192 1.0000 Uani . . . . . . C12 C 1.2812(3) 0.1483(2) 0.63096(18) 0.0224 1.0000 Uani . . . . . . C13 C 1.4101(3) 0.1287(2) 0.68603(19) 0.0240 1.0000 Uani . . . . . . C14 C 1.4051(3) 0.1490(2) 0.76785(19) 0.0226 1.0000 Uani . . . . . . C15 C 1.2729(3) 0.1896(2) 0.79283(19) 0.0202 1.0000 Uani . . . . . . C16 C 0.7818(3) 0.0603(2) 0.75077(18) 0.0192 1.0000 Uani . . . . . . C17 C 0.7145(3) -0.0214(2) 0.78013(19) 0.0227 1.0000 Uani . . . . . . C18 C 0.7259(3) -0.0305(2) 0.86381(19) 0.0247 1.0000 Uani . . . . . . C19 C 0.8068(3) 0.0418(2) 0.91554(19) 0.0214 1.0000 Uani . . . . . . C20 C 0.8718(3) 0.1229(2) 0.88306(17) 0.0168 1.0000 Uani . . . . . . C21 C 0.9577(3) 0.2052(2) 0.93268(18) 0.0181 1.0000 Uani . . . . . . C22 C 1.0078(3) 0.2086(2) 1.01620(18) 0.0196 1.0000 Uani . . . . . . C23 C 1.0919(3) 0.2913(2) 1.05439(18) 0.0192 1.0000 Uani . . . . . . C24 C 1.1203(3) 0.3701(2) 1.00561(18) 0.0206 1.0000 Uani . . . . . . C25 C 1.0690(3) 0.3637(2) 0.92252(18) 0.0175 1.0000 Uani . . . . . . C26 C 1.0921(3) 0.4384(2) 0.86279(18) 0.0174 1.0000 Uani . . . . . . C27 C 1.1646(3) 0.5299(2) 0.88311(19) 0.0210 1.0000 Uani . . . . . . C28 C 1.1783(3) 0.5953(2) 0.8225(2) 0.0266 1.0000 Uani . . . . . . C29 C 1.1191(3) 0.5677(2) 0.7426(2) 0.0244 1.0000 Uani . . . . . . C30 C 1.0488(3) 0.4758(2) 0.72542(19) 0.0218 1.0000 Uani . . . . . . C31 C 0.7902(3) 0.1652(2) 0.39413(18) 0.0202 1.0000 Uani . . . . . . C32 C 0.6832(3) 0.2174(2) 0.34345(18) 0.0245 1.0000 Uani . . . . . . C33 C 0.6569(3) 0.1923(2) 0.26023(19) 0.0242 1.0000 Uani . . . . . . C34 C 0.7352(3) 0.1159(2) 0.22580(18) 0.0219 1.0000 Uani . . . . . . C35 C 0.8383(3) 0.0621(2) 0.27660(18) 0.0224 1.0000 Uani . . . . . . C36 C 0.8652(3) 0.0862(2) 0.35939(18) 0.0223 1.0000 Uani . . . . . . C37 C 0.7155(4) 0.0934(3) 0.13387(19) 0.0256 1.0000 Uani . . . . . . C38 C 1.1511(3) 0.2959(2) 1.14294(18) 0.0196 1.0000 Uani . . . . . . C39 C 1.0893(3) 0.2336(2) 1.19582(18) 0.0229 1.0000 Uani . . . . . . C40 C 1.1465(3) 0.2359(2) 1.27819(19) 0.0240 1.0000 Uani . . . . . . C41 C 1.2658(3) 0.3005(2) 1.31065(18) 0.0225 1.0000 Uani . . . . . . C42 C 1.3260(4) 0.3643(3) 1.25915(19) 0.0298 1.0000 Uani . . . . . . C43 C 1.2718(4) 0.3620(2) 1.1765(2) 0.0288 1.0000 Uani . . . . . . C44 C 1.3334(4) 0.2995(3) 1.4003(2) 0.0322 1.0000 Uani . . . . . . O1 O 0.7787(3) 0.01752(18) 0.10762(13) 0.0361 1.0000 Uani . . . . . . O2 O 0.6394(3) 0.15420(19) 0.09082(13) 0.0406 1.0000 Uani . . . . . . O3 O 1.3032(3) 0.2239(2) 1.43804(14) 0.0470 1.0000 Uani . . . . . . O4 O 1.4202(3) 0.37153(19) 1.42965(14) 0.0406 1.0000 Uani . . . . . . O10 O 0.3971(3) 0.13978(19) -0.03188(17) 0.0566 1.0000 Uani D . . . . . O11 O 1.2930(4) 0.5219(3) 1.5228(3) 0.0977 1.0000 Uani D . . . . . O120 O 0.4948(8) 0.6789(4) -0.0278(4) 0.0627 0.5000 Uani . . . . . . O121 O 0.4144(7) 0.6831(4) 0.0101(3) 0.0383 0.5000 Uani . . . . . . O130 O 0.4444(8) 0.0429(5) 0.4303(4) 0.0647 0.5000 Uani . . . . . . O131 O 0.3295(8) 0.0250(5) 0.4340(3) 0.0588 0.5000 Uani . . . . . . O140 O 0.5523(5) 0.5000(4) 0.9599(3) 0.0403 0.5000 Uani . . . . . . O150 O 0.9858(7) 0.5737(5) 0.4659(3) 0.0752 0.5000 Uani . . . . . . H1 H 0.476(3) 0.1180(19) 0.0025(17) 0.0500 1.0000 Uiso D . . . . . H2 H 0.338(3) 0.0849(13) -0.0487(19) 0.0500 1.0000 Uiso D . . . . . H3 H 1.3939(16) 0.544(2) 1.5290(19) 0.0500 1.0000 Uiso D . . . . . H4 H 1.246(3) 0.556(2) 1.4821(17) 0.0500 1.0000 Uiso D . . . . . H11 H 0.6721 0.3699 0.8552 0.0288 1.0000 Uiso R . . . . . H21 H 0.4292 0.4341 0.8143 0.0339 1.0000 Uiso R . . . . . H31 H 0.3295 0.4266 0.6751 0.0337 1.0000 Uiso R . . . . . H41 H 0.4726 0.3473 0.5797 0.0292 1.0000 Uiso R . . . . . H71 H 0.6150 0.2519 0.4997 0.0276 1.0000 Uiso R . . . . . H91 H 1.0540 0.1521 0.4942 0.0289 1.0000 Uiso R . . . . . H121 H 1.2824 0.1361 0.5733 0.0283 1.0000 Uiso R . . . . . H131 H 1.5010 0.1010 0.6672 0.0317 1.0000 Uiso R . . . . . H141 H 1.4919 0.1354 0.8074 0.0287 1.0000 Uiso R . . . . . H151 H 1.2703 0.2048 0.8500 0.0266 1.0000 Uiso R . . . . . H161 H 0.7751 0.0658 0.6928 0.0234 1.0000 Uiso R . . . . . H171 H 0.6607 -0.0712 0.7428 0.0293 1.0000 Uiso R . . . . . H181 H 0.6781 -0.0862 0.8855 0.0313 1.0000 Uiso R . . . . . H191 H 0.8180 0.0363 0.9736 0.0276 1.0000 Uiso R . . . . . H221 H 0.9839 0.1541 1.0479 0.0251 1.0000 Uiso R . . . . . H241 H 1.1757 0.4286 1.0301 0.0262 1.0000 Uiso R . . . . . H271 H 1.2048 0.5478 0.9389 0.0289 1.0000 Uiso R . . . . . H281 H 1.2289 0.6590 0.8358 0.0342 1.0000 Uiso R . . . . . H291 H 1.1275 0.6123 0.7000 0.0320 1.0000 Uiso R . . . . . H301 H 1.0059 0.4575 0.6701 0.0287 1.0000 Uiso R . . . . . H321 H 0.6278 0.2707 0.3664 0.0307 1.0000 Uiso R . . . . . H331 H 0.5828 0.2285 0.2259 0.0296 1.0000 Uiso R . . . . . H351 H 0.8909 0.0075 0.2535 0.0288 1.0000 Uiso R . . . . . H361 H 0.9360 0.0479 0.3938 0.0280 1.0000 Uiso R . . . . . H391 H 1.0062 0.1881 1.1744 0.0283 1.0000 Uiso R . . . . . H401 H 1.1022 0.1920 1.3133 0.0301 1.0000 Uiso R . . . . . H421 H 1.4069 0.4110 1.2814 0.0351 1.0000 Uiso R . . . . . H431 H 1.3162 0.4060 1.1416 0.0358 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01847(14) 0.02185(16) 0.01480(15) 0.00083(11) 0.00145(10) 0.00213(11) N1 0.0161(14) 0.0194(15) 0.0192(15) 0.0016(12) 0.0026(11) 0.0015(11) N2 0.0162(14) 0.0184(16) 0.0146(14) 0.0027(12) 0.0007(11) 0.0012(11) N3 0.0135(13) 0.0186(15) 0.0172(15) 0.0004(12) -0.0019(11) 0.0014(11) N4 0.0152(13) 0.0195(15) 0.0157(14) 0.0011(12) 0.0025(11) 0.0017(11) N5 0.0154(13) 0.0185(15) 0.0154(14) 0.0006(12) 0.0021(11) 0.0006(12) N6 0.0178(13) 0.0202(16) 0.0182(15) 0.0005(12) 0.0039(11) 0.0025(11) C1 0.0233(18) 0.023(2) 0.0217(19) -0.0044(15) 0.0083(14) -0.0050(15) C2 0.0223(18) 0.023(2) 0.034(2) -0.0013(16) 0.0123(15) 0.0028(15) C3 0.0215(18) 0.028(2) 0.034(2) 0.0057(17) 0.0055(16) 0.0058(15) C4 0.0220(18) 0.026(2) 0.0233(19) 0.0049(16) -0.0002(14) 0.0044(15) C5 0.0196(17) 0.0192(19) 0.0174(18) 0.0039(14) 0.0017(13) 0.0013(14) C6 0.0185(17) 0.0225(19) 0.0141(17) 0.0043(14) -0.0016(13) 0.0028(14) C7 0.0159(16) 0.029(2) 0.0183(18) 0.0035(15) -0.0012(13) 0.0039(14) C8 0.0215(17) 0.026(2) 0.0157(17) 0.0021(15) 0.0012(14) -0.0008(15) C9 0.0216(18) 0.029(2) 0.0201(19) -0.0020(15) 0.0037(14) 0.0057(15) C10 0.0194(17) 0.0214(19) 0.0159(17) 0.0025(14) 0.0035(13) 0.0034(14) C11 0.0146(16) 0.0187(19) 0.0249(19) 0.0049(15) 0.0038(14) 0.0017(14) C12 0.0243(18) 0.027(2) 0.0156(17) -0.0002(15) 0.0015(14) 0.0012(15) C13 0.0178(17) 0.027(2) 0.028(2) 0.0040(16) 0.0030(14) 0.0028(15) C14 0.0182(17) 0.023(2) 0.025(2) 0.0060(16) -0.0043(14) 0.0004(14) C15 0.0202(17) 0.0185(18) 0.0210(18) 0.0030(15) -0.0011(14) -0.0020(14) C16 0.0164(16) 0.0233(19) 0.0166(17) -0.0035(15) -0.0010(13) 0.0035(14) C17 0.0230(17) 0.0193(19) 0.0235(19) -0.0030(15) -0.0038(14) 0.0012(15) C18 0.0255(18) 0.022(2) 0.026(2) 0.0013(16) 0.0024(15) -0.0012(15) C19 0.0226(17) 0.023(2) 0.0183(18) -0.0001(15) 0.0001(14) 0.0017(15) C20 0.0180(16) 0.0179(18) 0.0141(17) 0.0002(14) 0.0000(13) 0.0035(14) C21 0.0193(16) 0.0189(18) 0.0162(17) 0.0007(14) 0.0029(13) 0.0029(14) C22 0.0189(16) 0.0230(19) 0.0169(17) 0.0024(15) 0.0016(13) 0.0012(14) C23 0.0183(16) 0.024(2) 0.0158(17) 0.0020(15) 0.0017(13) 0.0030(14) C24 0.0192(17) 0.0209(19) 0.0211(18) -0.0038(15) 0.0024(14) 0.0011(14) C25 0.0154(16) 0.0192(19) 0.0177(17) 0.0003(15) 0.0017(13) 0.0021(14) C26 0.0152(16) 0.0190(18) 0.0184(18) 0.0020(14) 0.0031(13) 0.0027(14) C27 0.0214(17) 0.0191(19) 0.0221(18) -0.0030(15) 0.0030(14) 0.0010(14) C28 0.0247(18) 0.021(2) 0.035(2) 0.0012(17) 0.0083(15) -0.0006(15) C29 0.0280(18) 0.022(2) 0.025(2) 0.0070(16) 0.0097(15) 0.0030(16) C30 0.0220(17) 0.029(2) 0.0158(17) 0.0029(15) 0.0054(13) 0.0038(15) C31 0.0205(17) 0.025(2) 0.0148(17) 0.0015(15) 0.0012(13) -0.0048(15) C32 0.0197(17) 0.035(2) 0.0182(18) 0.0000(16) -0.0002(14) 0.0006(15) C33 0.0226(18) 0.028(2) 0.0208(19) 0.0043(16) -0.0004(14) -0.0046(15) C34 0.0199(17) 0.026(2) 0.0186(18) 0.0029(16) 0.0001(14) -0.0079(15) C35 0.0296(18) 0.0198(19) 0.0180(18) 0.0009(15) 0.0037(14) -0.0022(15) C36 0.0262(18) 0.023(2) 0.0159(18) 0.0020(15) -0.0027(14) -0.0022(15) C37 0.0243(18) 0.032(2) 0.0191(19) 0.0037(17) -0.0018(15) -0.0086(17) C38 0.0202(17) 0.0186(19) 0.0200(18) 0.0010(15) 0.0018(14) 0.0047(14) C39 0.0250(18) 0.025(2) 0.0173(18) -0.0008(15) -0.0026(14) -0.0036(15) C40 0.0285(19) 0.027(2) 0.0165(18) 0.0045(15) 0.0023(14) -0.0008(16) C41 0.0271(18) 0.024(2) 0.0153(18) -0.0004(15) -0.0022(14) 0.0050(15) C42 0.034(2) 0.029(2) 0.023(2) 0.0003(17) -0.0086(16) -0.0071(17) C43 0.033(2) 0.027(2) 0.025(2) 0.0050(16) -0.0017(16) -0.0058(16) C44 0.028(2) 0.047(3) 0.021(2) 0.0013(19) 0.0003(16) 0.0096(19) O1 0.0474(15) 0.0390(16) 0.0208(13) -0.0045(12) 0.0025(11) 0.0020(13) O2 0.0472(15) 0.0529(18) 0.0190(13) 0.0048(13) -0.0071(11) 0.0057(13) O3 0.0546(17) 0.061(2) 0.0242(15) 0.0151(14) -0.0025(12) -0.0076(15) O4 0.0451(15) 0.0436(17) 0.0277(15) -0.0087(13) -0.0109(12) -0.0027(13) O10 0.071(2) 0.0405(18) 0.0481(18) 0.0145(15) -0.0343(14) -0.0096(15) O11 0.051(2) 0.064(3) 0.171(4) 0.002(2) -0.010(2) 0.0032(18) O120 0.066(5) 0.040(4) 0.077(5) 0.006(4) -0.009(4) -0.008(4) O121 0.050(4) 0.033(3) 0.031(3) 0.002(3) 0.005(3) -0.010(3) O130 0.080(5) 0.057(5) 0.053(4) -0.012(3) -0.001(4) 0.004(4) O131 0.078(5) 0.065(5) 0.030(3) -0.012(3) 0.004(3) -0.028(4) O140 0.035(3) 0.055(4) 0.029(3) 0.001(3) -0.003(2) -0.007(2) O150 0.080(4) 0.095(5) 0.050(4) 0.030(4) 0.001(3) -0.024(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.08993(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru1 . N1 . 2.080(2) yes Ru1 . N2 . 1.978(2) yes Ru1 . N3 . 2.065(2) yes Ru1 . N4 . 2.063(2) yes Ru1 . N5 . 1.971(2) yes Ru1 . N6 . 2.067(2) yes N1 . C1 . 1.350(4) yes N1 . C5 . 1.366(4) yes N2 . C6 . 1.362(3) yes N2 . C10 . 1.348(4) yes N3 . C11 . 1.373(4) yes N3 . C15 . 1.341(3) yes N4 . C16 . 1.355(4) yes N4 . C20 . 1.372(3) yes N5 . C21 . 1.353(4) yes N5 . C25 . 1.357(4) yes N6 . C26 . 1.378(4) yes N6 . C30 . 1.351(4) yes C1 . C2 . 1.381(4) yes C1 . H11 . 0.960 no C2 . C3 . 1.382(4) yes C2 . H21 . 0.960 no C3 . C4 . 1.377(4) yes C3 . H31 . 0.960 no C4 . C5 . 1.390(4) yes C4 . H41 . 0.960 no C5 . C6 . 1.472(4) yes C6 . C7 . 1.373(4) yes C7 . C8 . 1.397(4) yes C7 . H71 . 0.960 no C8 . C9 . 1.399(4) yes C8 . C31 . 1.485(4) yes C9 . C10 . 1.381(4) yes C9 . H91 . 0.960 no C10 . C11 . 1.477(4) yes C11 . C12 . 1.369(4) yes C12 . C13 . 1.388(4) yes C12 . H121 . 0.960 no C13 . C14 . 1.372(4) yes C13 . H131 . 0.960 no C14 . C15 . 1.382(4) yes C14 . H141 . 0.960 no C15 . H151 . 0.960 no C16 . C17 . 1.378(4) yes C16 . H161 . 0.960 no C17 . C18 . 1.387(4) yes C17 . H171 . 0.960 no C18 . C19 . 1.381(4) yes C18 . H181 . 0.960 no C19 . C20 . 1.388(4) yes C19 . H191 . 0.960 no C20 . C21 . 1.477(4) yes C21 . C22 . 1.392(4) yes C22 . C23 . 1.399(4) yes C22 . H221 . 0.960 no C23 . C24 . 1.405(4) yes C23 . C38 . 1.486(4) yes C24 . C25 . 1.387(4) yes C24 . H241 . 0.960 no C25 . C26 . 1.477(4) yes C26 . C27 . 1.382(4) yes C27 . C28 . 1.385(4) yes C27 . H271 . 0.960 no C28 . C29 . 1.383(4) yes C28 . H281 . 0.960 no C29 . C30 . 1.372(4) yes C29 . H291 . 0.960 no C30 . H301 . 0.960 no C31 . C32 . 1.395(4) yes C31 . C36 . 1.394(4) yes C32 . C33 . 1.388(4) yes C32 . H321 . 0.960 no C33 . C34 . 1.380(4) yes C33 . H331 . 0.960 no C34 . C35 . 1.389(4) yes C34 . C37 . 1.521(4) yes C35 . C36 . 1.379(4) yes C35 . H351 . 0.960 no C36 . H361 . 0.960 no C37 . O1 . 1.252(4) yes C37 . O2 . 1.256(4) yes C38 . C39 . 1.395(4) yes C38 . C43 . 1.403(4) yes C39 . C40 . 1.387(4) yes C39 . H391 . 0.960 no C40 . C41 . 1.378(4) yes C40 . H401 . 0.960 no C41 . C42 . 1.385(4) yes C41 . C44 . 1.524(4) yes C42 . C43 . 1.386(4) yes C42 . H421 . 0.960 no C43 . H431 . 0.960 no C44 . O3 . 1.265(4) yes C44 . O4 . 1.256(4) yes O10 . H1 . 0.896(10) no O10 . H2 . 0.903(10) no O11 . H3 . 0.912(10) no O11 . H4 . 0.896(10) no O120 . O121 . 0.998(6) yes O130 . O131 . 1.034(7) yes O140 . O140 2_667 1.702(9) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Ru1 . N2 . 78.56(9) yes N1 . Ru1 . N3 . 157.39(9) yes N2 . Ru1 . N3 . 78.88(9) yes N1 . Ru1 . N4 . 91.73(9) yes N2 . Ru1 . N4 . 98.99(9) yes N3 . Ru1 . N4 . 93.24(9) yes N1 . Ru1 . N5 . 104.46(9) yes N2 . Ru1 . N5 . 176.23(10) yes N3 . Ru1 . N5 . 98.14(9) yes N4 . Ru1 . N5 . 78.79(10) yes N1 . Ru1 . N6 . 91.70(9) yes N2 . Ru1 . N6 . 103.30(10) yes N3 . Ru1 . N6 . 92.02(9) yes N4 . Ru1 . N6 . 157.69(9) yes N5 . Ru1 . N6 . 79.01(10) yes Ru1 . N1 . C1 . 127.8(2) yes Ru1 . N1 . C5 . 113.97(19) yes C1 . N1 . C5 . 118.1(3) yes Ru1 . N2 . C6 . 119.75(19) yes Ru1 . N2 . C10 . 119.27(19) yes C6 . N2 . C10 . 120.8(2) yes Ru1 . N3 . C11 . 114.39(18) yes Ru1 . N3 . C15 . 128.2(2) yes C11 . N3 . C15 . 117.4(2) yes Ru1 . N4 . C16 . 127.6(2) yes Ru1 . N4 . C20 . 114.54(19) yes C16 . N4 . C20 . 117.7(2) yes Ru1 . N5 . C21 . 119.6(2) yes Ru1 . N5 . C25 . 119.48(19) yes C21 . N5 . C25 . 120.7(2) yes Ru1 . N6 . C26 . 114.09(19) yes Ru1 . N6 . C30 . 128.0(2) yes C26 . N6 . C30 . 117.9(3) yes N1 . C1 . C2 . 122.2(3) yes N1 . C1 . H11 . 118.8 no C2 . C1 . H11 . 119.0 no C1 . C2 . C3 . 119.5(3) yes C1 . C2 . H21 . 120.1 no C3 . C2 . H21 . 120.4 no C2 . C3 . C4 . 119.3(3) yes C2 . C3 . H31 . 120.1 no C4 . C3 . H31 . 120.6 no C3 . C4 . C5 . 119.1(3) yes C3 . C4 . H41 . 120.6 no C5 . C4 . H41 . 120.2 no C4 . C5 . N1 . 121.8(3) yes C4 . C5 . C6 . 122.7(3) yes N1 . C5 . C6 . 115.6(2) yes C5 . C6 . N2 . 111.7(2) yes C5 . C6 . C7 . 127.8(3) yes N2 . C6 . C7 . 120.4(3) yes C6 . C7 . C8 . 120.1(3) yes C6 . C7 . H71 . 119.9 no C8 . C7 . H71 . 119.9 no C7 . C8 . C9 . 118.2(3) yes C7 . C8 . C31 . 121.8(3) yes C9 . C8 . C31 . 120.0(3) yes C8 . C9 . C10 . 119.8(3) yes C8 . C9 . H91 . 120.2 no C10 . C9 . H91 . 120.0 no C9 . C10 . N2 . 120.6(3) yes C9 . C10 . C11 . 126.5(3) yes N2 . C10 . C11 . 112.9(2) yes C10 . C11 . N3 . 114.4(2) yes C10 . C11 . C12 . 123.6(3) yes N3 . C11 . C12 . 122.0(3) yes C11 . C12 . C13 . 119.6(3) yes C11 . C12 . H121 . 119.8 no C13 . C12 . H121 . 120.7 no C12 . C13 . C14 . 119.0(3) yes C12 . C13 . H131 . 120.5 no C14 . C13 . H131 . 120.5 no C13 . C14 . C15 . 119.0(3) yes C13 . C14 . H141 . 120.8 no C15 . C14 . H141 . 120.2 no C14 . C15 . N3 . 123.1(3) yes C14 . C15 . H151 . 118.9 no N3 . C15 . H151 . 118.0 no N4 . C16 . C17 . 122.7(3) yes N4 . C16 . H161 . 118.3 no C17 . C16 . H161 . 119.0 no C16 . C17 . C18 . 119.2(3) yes C16 . C17 . H171 . 120.1 no C18 . C17 . H171 . 120.7 no C17 . C18 . C19 . 119.0(3) yes C17 . C18 . H181 . 120.5 no C19 . C18 . H181 . 120.5 no C18 . C19 . C20 . 119.6(3) yes C18 . C19 . H191 . 120.5 no C20 . C19 . H191 . 119.9 no C19 . C20 . N4 . 121.6(3) yes C19 . C20 . C21 . 124.1(3) yes N4 . C20 . C21 . 114.3(3) yes C20 . C21 . N5 . 112.4(2) yes C20 . C21 . C22 . 127.0(3) yes N5 . C21 . C22 . 120.6(3) yes C21 . C22 . C23 . 120.3(3) yes C21 . C22 . H221 . 120.0 no C23 . C22 . H221 . 119.7 no C22 . C23 . C24 . 117.5(3) yes C22 . C23 . C38 . 121.7(3) yes C24 . C23 . C38 . 120.9(3) yes C23 . C24 . C25 . 120.5(3) yes C23 . C24 . H241 . 119.6 no C25 . C24 . H241 . 119.9 no C24 . C25 . N5 . 120.5(3) yes C24 . C25 . C26 . 127.2(3) yes N5 . C25 . C26 . 112.4(3) yes C25 . C26 . N6 . 114.7(3) yes C25 . C26 . C27 . 124.0(3) yes N6 . C26 . C27 . 121.2(3) yes C26 . C27 . C28 . 119.5(3) yes C26 . C27 . H271 . 119.9 no C28 . C27 . H271 . 120.6 no C27 . C28 . C29 . 119.4(3) yes C27 . C28 . H281 . 120.2 no C29 . C28 . H281 . 120.4 no C28 . C29 . C30 . 119.0(3) yes C28 . C29 . H291 . 120.3 no C30 . C29 . H291 . 120.7 no C29 . C30 . N6 . 122.9(3) yes C29 . C30 . H301 . 118.8 no N6 . C30 . H301 . 118.2 no C8 . C31 . C32 . 120.8(3) yes C8 . C31 . C36 . 120.8(3) yes C32 . C31 . C36 . 118.3(3) yes C31 . C32 . C33 . 120.2(3) yes C31 . C32 . H321 . 119.7 no C33 . C32 . H321 . 120.1 no C32 . C33 . C34 . 121.2(3) yes C32 . C33 . H331 . 119.6 no C34 . C33 . H331 . 119.2 no C33 . C34 . C35 . 118.6(3) yes C33 . C34 . C37 . 121.2(3) yes C35 . C34 . C37 . 120.1(3) yes C34 . C35 . C36 . 120.7(3) yes C34 . C35 . H351 . 119.2 no C36 . C35 . H351 . 120.0 no C31 . C36 . C35 . 120.9(3) yes C31 . C36 . H361 . 119.3 no C35 . C36 . H361 . 119.8 no C34 . C37 . O1 . 117.6(3) yes C34 . C37 . O2 . 116.6(3) yes O1 . C37 . O2 . 125.7(3) yes C23 . C38 . C39 . 120.9(3) yes C23 . C38 . C43 . 121.6(3) yes C39 . C38 . C43 . 117.4(3) yes C38 . C39 . C40 . 121.2(3) yes C38 . C39 . H391 . 119.0 no C40 . C39 . H391 . 119.8 no C39 . C40 . C41 . 121.0(3) yes C39 . C40 . H401 . 119.6 no C41 . C40 . H401 . 119.4 no C40 . C41 . C42 . 118.3(3) yes C40 . C41 . C44 . 120.9(3) yes C42 . C41 . C44 . 120.8(3) yes C41 . C42 . C43 . 121.4(3) yes C41 . C42 . H421 . 119.0 no C43 . C42 . H421 . 119.6 no C38 . C43 . C42 . 120.5(3) yes C38 . C43 . H431 . 119.3 no C42 . C43 . H431 . 120.2 no C41 . C44 . O3 . 117.1(3) yes C41 . C44 . O4 . 117.5(3) yes O3 . C44 . O4 . 125.4(3) yes H1 . O10 . H2 . 104.7(10) no H3 . O11 . H4 . 104.7(10) no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag O10 . H1 . O2 . 146 0.90 1.94 2.728(2) yes O10 . H2 . O1 2_655 167 0.90 1.86 2.742(2) yes O11 . H3 . O4 2_868 158 0.91 1.99 2.856(2) yes