# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1310 data_global #========== #Fichier CIF #============================================================================== # 1. TITLE AND AUTHOR LIST _publ_section_title ; Complexes of new chiral terpyridine ligands. Synthesis and characterisation of Ru(II) and Rh(III) compounds and formation of labile Ag(I), Cd(II), Hg(II), Pb(II) and Zn(II) complexes. ; loop_ _publ_author_name _publ_author_address 'Ziegler, Marco' ; Institut de Chimie Inorganique et Analytique, Universite de Fribourg, Perolles CH-1700 Fribourg ; 'Monney, Veronique' ; Institut de Chimie Inorganique et Analytique, Universit de Fribourg, Prolles CH-1700 Fribourg ; 'Stoeckli-Evans, Helen' ; Insitut de Chimie, Universite de Neuchatel, Av. Bellevaux 51 CH-2000 Neuchatel ; 'Von Zelewsky, Alex' ; Institut de Chimie Inorganique et Analytique, Universite de Fribourg, Perolles CH-1700 Fribourg ; 'Sasaki, Isabelle' ; Laboratoire de Chimie de Coordination, CNRS, 205 route de Narbonne F-31077 Toulouse ; 'Dupic, Gilles' ; Laboratoire de Chimie de Coordination, CNRS, 205 route de Narbonne F-31077 Toulouse ; 'Daran, Jean-Claude' ; Laboratoire de Chimie de Coordination, CNRS, 205 route de Narbonne F-31077 Toulouse ; 'Balavoine, Gilbert G. A.' ; Laboratoire de Chimie de Coordination, CNRS, 205 route de Narbonne F-31077 Toulouse ; #============================================================================== _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435 Sheldrick, G.M. SHELXL-97, program for crystal structure refinement, University of Gottingen, 1997. Stoe, IPDS Manual. Version 2.75. Stoe & Cie, Darmstadt,1996, Germany. Stoe, X-SHAPE, Crystal Optimisation for Numerical Absorption Correction, Revision 1.01. Stoe & Cie, Darmstadt,1996, Germany. Stoe, X-RED, Data Reduction for STADI4 and IPDS, Revision 1.08. Stoe & Cie, Darmstadt, 1996, Germany. Carruthers, J.R. and Watkin, D.J. (1979), (Chebychev Weighting) Acta Cryst, A35, 698-699 Walker, N., and Stuart, D. DIFABS. Acta Cryst, A39, 158-166 Watkin, D.J., Prout, C.K. Carruthers, R.J. & Betteridge, P. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. (1994), RC93, Chemical Crystallography Laboratory, Oxford, UK. ; #==================================================================== data_(L2-) _exptl_special_details ; The data were collected on a Stoe Imaging Plate Diffraction System (IPDS). The crystal-to-detector distance was 80 mm. 100 exposures (6 min per exposure) were obtained with 0 < \f < 200\% and with the crystals oscillated through 2\% in \f. Coverage of the unique set was over 89% complete to at least 24.2\%. Crystal decay was monitored by measuring 200 reflexions per image. ; _chemical_name_systematic ; bis('di(1R)-pineno'-[4,5:4",5"]-fused 2,2':6',2"-terpyrydine ; _cell_length_a 6.5893(9) _cell_length_b 9.0795(14) _cell_length_c 19.494(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1166.3(3) _symmetry_cell_setting 'Orthorhombic ' _symmetry_space_group_name_H-M 'P 21 2 21 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 'x+1/2,-y,-z+1/2' '-x,y,-z' '-x+1/2,-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 ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C29 H31 N3 ' _chemical_formula_moiety ' C29 H31 N3 ' _chemical_compound_source ; synthetic route ; _chemical_formula_weight 421.6 _cell_measurement_reflns_used 2000 _cell_measurement_theta_min 1.45 _cell_measurement_theta_max 24.2 _cell_measurement_temperature 293(2) _cell_formula_units_Z 2 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_max 0.80 _exptl_crystal_density_diffrn 1.201 _exptl_crystal_density_meas ? _exptl_crystal_F_000 452.06 _exptl_absorpt_coefficient_mu 0.066 _exptl_absorpt_correction_type none _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f oscillation' _diffrn_standards_interval_time 'every image ' _diffrn_standards_interval_count 'every image ' _diffrn_standards_number '200 for each image' _diffrn_standards_decay_% negligible _diffrn_ambient_temperature 293(2) _diffrn_reflns_number 7285 _reflns_number_total 1783 _diffrn_reflns_av_R_equivalents 0.032 _reflns_number_gt 1331 _reflns_threshold-expression >2.00\s(I) _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 24.2 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme ; Robust-resistant weighting scheme (Prince E, 1982): w=y[1-(\DF/6\s(Fo^2^)]^2^' where y=1/\SArTr(x) with 3 coefficients Ar(2.26, 0.666, 2.09) for the Chebyshev polynomial ArTr(x) where x was Fc/Fc(max). ; _atom_sites_solution_primary SIR92 _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatement 'riding model' _refine_ls_extinction_method none _refine_diff_density_min -0.19 _refine_diff_density_max 0.17 _refine_ls_number_parameters 148 _refine_ls_R_factor_obs 0.0363 _refine_ls_wR_factor_obs 0.0317 _refine_ls_goodness_of_fit_obs 1.1295 _refine_ls_shift/esd_max 0.021000 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type N1 1.0000 1.0998(2) 1.0000 0.0461 1.0000 Uani C3 1.0000 1.4036(3) 1.0000 0.0802 1.0000 Uani N2 0.5309(2) 1.1611(2) 0.91027(7) 0.0561 1.0000 Uani C1 0.8510(3) 1.1750(2) 0.96810(8) 0.0474 1.0000 Uani C2 0.8465(3) 1.3274(2) 0.9675(1) 0.0690 1.0000 Uani C4 0.6906(2) 1.0872(2) 0.93456(8) 0.0464 1.0000 Uani C5 0.3823(3) 1.0820(2) 0.88151(8) 0.0557 1.0000 Uani C6 0.3818(2) 0.9309(2) 0.87524(7) 0.0508 1.0000 Uani C7 0.5521(2) 0.8548(2) 0.89929(8) 0.0461 1.0000 Uani C8 0.7066(2) 0.9344(2) 0.92928(8) 0.0459 1.0000 Uani C9 0.5550(2) 0.6900(2) 0.89035(9) 0.0543 1.0000 Uani C10 0.3571(3) 0.6354(2) 0.85801(9) 0.0546 1.0000 Uani C11 0.1790(3) 0.7110(2) 0.8955(1) 0.0637 1.0000 Uani C12 0.2136(2) 0.8398(2) 0.8461(1) 0.0576 1.0000 Uani C13 0.3000(2) 0.7268(2) 0.79325(9) 0.0610 1.0000 Uani C14 0.4627(3) 0.7775(3) 0.74419(9) 0.0748 1.0000 Uani C15 0.1307(4) 0.6502(3) 0.7520(1) 0.0820 1.0000 Uani H21 0.7385 1.3792 0.9448 0.0803 1.0000 Uiso H31 1.0000 1.5093 1.0000 0.0855 1.0000 Uiso H51 0.2671 1.1345 0.8639 0.0662 1.0000 Uiso H81 0.8249 0.8849 0.9465 0.0547 1.0000 Uiso H91 0.5719 0.6443 0.9344 0.0649 1.0000 Uiso H92 0.6665 0.6635 0.8612 0.0649 1.0000 Uiso H101 0.3747 0.5306 0.8556 0.0654 1.0000 Uiso H111 0.2031 0.7329 0.9429 0.0736 1.0000 Uiso H112 0.0503 0.6624 0.8908 0.0736 1.0000 Uiso H121 0.1108 0.9103 0.8342 0.0653 1.0000 Uiso H141 0.4016 0.8320 0.7074 0.0858 1.0000 Uiso H142 0.5574 0.8394 0.7681 0.0858 1.0000 Uiso H143 0.5326 0.6934 0.7259 0.0858 1.0000 Uiso H151 0.0982 0.7085 0.7124 0.0972 1.0000 Uiso H152 0.0122 0.6399 0.7802 0.0972 1.0000 Uiso H153 0.1763 0.5546 0.7376 0.0972 1.0000 Uiso 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 N1 0.049(1) 0.045(1) 0.0444(9) 0.0000 0.0041(8) 0.0000 C3 0.118(3) 0.035(1) 0.088(2) 0.0000 -0.017(2) 0.0000 N2 0.0585(9) 0.0589(8) 0.0509(8) 0.0076(6) -0.0030(7) 0.0169(7) C1 0.055(1) 0.0460(9) 0.0410(8) 0.0019(7) 0.0073(8) 0.0086(7) C2 0.088(1) 0.048(1) 0.071(1) 0.0023(9) -0.009(1) 0.0097(9) C4 0.0458(9) 0.052(1) 0.0409(8) 0.0072(7) 0.0036(7) 0.0073(7) C5 0.047(1) 0.066(1) 0.0533(9) 0.0082(8) -0.0055(7) 0.0198(8) C6 0.0412(9) 0.068(1) 0.0435(8) 0.0087(7) -0.0006(7) 0.0104(7) C7 0.0425(9) 0.0537(9) 0.0421(8) 0.0046(7) 0.0031(7) 0.0093(7) C8 0.0395(8) 0.0529(9) 0.0453(7) 0.0055(6) -0.0009(7) 0.0100(7) C9 0.048(1) 0.056(1) 0.059(1) -0.0019(8) -0.0068(8) 0.0041(7) C10 0.050(1) 0.0593(9) 0.0551(9) 0.0050(8) -0.0011(8) -0.0041(7) C11 0.046(1) 0.088(1) 0.057(1) 0.0066(9) 0.0040(8) -0.0034(8) C12 0.0340(9) 0.078(1) 0.061(1) 0.0100(9) -0.0067(7) 0.0062(7) C13 0.050(1) 0.083(1) 0.0502(9) 0.0044(9) -0.0064(8) -0.0051(8) C14 0.078(1) 0.099(2) 0.047(1) 0.0012(9) 0.0082(9) -0.015(1) C15 0.078(1) 0.100(2) 0.069(1) 0.006(1) -0.021(1) -0.017(1) 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 N1 . C1 . 1.348(2) yes N1 . C1 3_757 1.348(2) yes C3 . C2 . 1.380(3) yes C3 . C2 3_757 1.380(3) yes C3 . H31 . 0.960(3) no N2 . C4 . 1.335(2) yes N2 . C5 . 1.338(2) yes C1 . C2 . 1.384(2) yes C1 . C4 . 1.477(2) yes C4 . C8 . 1.395(2) yes C5 . C6 . 1.377(3) yes C6 . C7 . 1.399(2) yes C6 . C12 . 1.494(2) yes C7 . C8 . 1.379(2) yes C7 . C9 . 1.506(2) yes C9 . C10 . 1.531(3) yes C10 . C11 . 1.543(3) yes C10 . C13 . 1.557(3) yes C11 . C12 . 1.532(3) yes C12 . C13 . 1.563(3) yes C13 . C14 . 1.509(2) yes C13 . C15 . 1.541(3) 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 C1 . N1 . C1 3_757 119.1(2) yes C2 . C3 . C2 3_757 119.8(3) yes C4 . N2 . C5 . 117.1(1) yes N1 . C1 . C2 . 121.8(2) yes N1 . C1 . C4 . 116.9(1) yes C2 . C1 . C4 . 121.3(2) yes C3 . C2 . C1 . 118.7(2) yes N2 . C4 . C1 . 116.7(1) yes N2 . C4 . C8 . 122.2(1) yes C1 . C4 . C8 . 121.0(1) yes N2 . C5 . C6 . 125.0(1) yes C5 . C6 . C7 . 117.4(1) yes C5 . C6 . C12 . 125.9(1) yes C7 . C6 . C12 . 116.7(2) yes C6 . C7 . C8 . 118.4(1) yes C6 . C7 . C9 . 117.5(1) yes C8 . C7 . C9 . 124.1(1) yes C4 . C8 . C7 . 119.8(1) yes C7 . C9 . C10 . 111.0(1) yes C9 . C10 . C11 . 108.0(1) yes C9 . C10 . C13 . 111.6(1) yes C11 . C10 . C13 . 87.9(1) yes C10 . C11 . C12 . 86.0(1) yes C6 . C12 . C11 . 107.1(1) yes C6 . C12 . C13 . 110.1(1) yes C11 . C12 . C13 . 88.1(1) yes C10 . C13 . C12 . 84.4(1) yes C10 . C13 . C14 . 120.3(1) yes C12 . C13 . C14 . 118.5(2) yes C10 . C13 . C15 . 111.0(1) yes C12 . C13 . C15 . 112.2(2) yes C14 . C13 . C15 . 108.7(1) yes #=END======================================================================== data_(3) _audit_creation_method CRYSTALS _chemical_name_systematic ; ? ; _cell_length_a 11.253(4) _cell_length_b 16.741(4) _cell_length_c 25.941(7) _cell_angle_alpha 90.00(2) _cell_angle_beta 90.00(3) _cell_angle_gamma 90.00(3) _cell_volume 4887(3) _symmetry_cell_setting 'Orthorhombic ' _symmetry_space_group_name_H-M 'P b c a ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,z' 'x+1/2,-y+1/2,-z' 'x,-y+1/2,z+1/2' '-x,y+1/2,-z+1/2' '-x+1/2,-y,z+1/2' 'x+1/2,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 ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'I ' -0.7260 1.8120 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C19 H17 I4 O2 N3 ' _chemical_formula_moiety ' C19 H17 I4 O2 N3 ' _chemical_compound_source ; synthetic route ; _diffrn_measurement_device 'Enraf-nonius CAD4 ' _chemical_melting_point 'not measured' _chemical_formula_weight 826.98 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5 _cell_measurement_theta_max 9 _cell_measurement_temperature 293 _cell_formula_units_Z 8.00 _exptl_crystal_description flat _exptl_crystal_colour gold _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_max 0.90 _exptl_crystal_density_diffrn 2.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 3017.61 _exptl_absorpt_coefficient_mu 5.07 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '\y scan,(North et al, 1968)' _exptl_absorpt_correction_T_min 0.449 _exptl_absorpt_correction_T_max 0.864 _diffrn_standards_interval_time 120 _diffrn_standards_interval_count 200 _diffrn_standards_number 2 _diffrn_standards_decay_% 1.98 _diffrn_ambient_temperature 293 _diffrn_reflns_number 3972 _reflns_number_total 3078 _diffrn_reflns_av_R_equivalents 0.01 _diffrn_measured_fraction_theta_max 0.905 _reflns_number_observed 2327 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 23.00 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _reflns_limit_h_min 0 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _reflns_observed_criterion >3.00\s(I) _computing_data_collection 'CAD-4 software (Enraf-Nonius, 1989)' _computing_data_reduction 'RC93 (Watkin et al, 1994)' _computing_cell_refinement 'CAD-4 software (Enraf-Nonius, 1989)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _computing_structure_refinement 'CRYSTALS Issue 10 (Watkin et al, 1996)' _computing_molecular_graphics 'CAMERON (Watkin, Prout & Pearce, 1996)' _computing_publication_material 'CRYSTALS Issue 10 (Watkin et al, 1996)' _refine_diff_density_min -0.54 _refine_diff_density_max 0.59 _refine_ls_number_reflns 2327 _refine_ls_number_parameters 254 _refine_ls_R_factor_obs 0.0331 _refine_ls_wR_factor_obs 0.0398 _refine_ls_goodness_of_fit_obs 1.0447 _refine_ls_shift/su_max 0.044163 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme ; Robust-resistant weighting scheme (Prince E, 1982): w=y[1-(\DF/6\s(Fo^2^)]^2^' where y=1/\SArTr(x) with 3 coefficients Ar(0.965, 0.694, 0.480) for the Chebyshev polynomial ArTr(x) where x was Fc/Fc(max). ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _refine_ls_matrix_type full _atom_sites_solution_primary 'Direct_Methods, SIR92' _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment ; H atoms placed geometrically after each cycle ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type I1 0.17743(5) 0.53272(3) 0.34465(2) 0.0633 1.0000 Uani I2 0.15417(6) 0.44844(4) 0.43891(3) 0.0688 1.0000 Uani I3 0.19772(6) 0.62373(3) 0.23790(3) 0.0714 1.0000 Uani I4 0.11824(5) 0.16756(3) 0.05197(2) 0.0625 1.0000 Uani O1 0.7096(5) 0.2952(4) 0.1751(2) 0.0599 1.0000 Uani O2 0.6012(6) 0.0784(4) -0.0481(2) 0.0769 1.0000 Uani N1 0.6911(5) 0.1872(4) 0.0607(2) 0.0467 1.0000 Uani N2 0.9374(5) 0.3125(4) 0.1474(2) 0.0463 1.0000 Uani N3 0.8173(5) 0.1177(3) -0.0841(2) 0.0460 1.0000 Uani C1 0.7372(7) 0.2629(4) 0.1358(3) 0.0454 1.0000 Uani C2 0.6615(7) 0.1164(5) -0.0180(3) 0.0554 1.0000 Uani C3 0.8590(7) 0.2720(5) 0.1111(3) 0.0543 1.0000 Uani C4 0.7877(7) 0.1410(5) -0.0309(3) 0.0479 1.0000 Uani C11 0.6526(7) 0.2097(4) 0.1076(3) 0.0500 1.0000 Uani C12 0.5439(8) 0.1855(5) 0.1279(3) 0.0610 1.0000 Uani C13 0.4721(7) 0.1364(6) 0.0998(4) 0.0661 1.0000 Uani C14 0.5062(8) 0.1144(5) 0.0513(4) 0.0647 1.0000 Uani C15 0.6169(6) 0.1399(5) 0.0327(3) 0.0481 1.0000 Uani C211 0.9962(8) 0.2680(5) 0.1824(3) 0.0595 1.0000 Uani C212 1.0628(8) 0.3039(7) 0.2193(3) 0.0728 1.0000 Uani C213 1.0715(9) 0.3848(7) 0.2213(4) 0.0752 1.0000 Uani C214 1.0147(9) 0.4292(6) 0.1848(4) 0.0728 1.0000 Uani C215 0.9454(7) 0.3925(5) 0.1472(4) 0.0618 1.0000 Uani C311 0.8342(8) 0.0405(5) -0.0946(4) 0.0611 1.0000 Uani C312 0.8575(8) 0.0164(5) -0.1430(4) 0.0641 1.0000 Uani C313 0.8583(8) 0.0699(6) -0.1821(3) 0.0640 1.0000 Uani C314 0.8398(9) 0.1504(6) -0.1714(4) 0.0715 1.0000 Uani C315 0.8189(7) 0.1728(5) -0.1215(3) 0.0568 1.0000 Uani H31 0.8527 0.3031 0.0801 0.0621 1.0000 Uiso H32 0.8912 0.2203 0.1029 0.0621 1.0000 Uiso H41 0.8423 0.1161 -0.0074 0.0565 1.0000 Uiso H42 0.7953 0.1985 -0.0277 0.0565 1.0000 Uiso H121 0.5199 0.2033 0.1615 0.0733 1.0000 Uiso H131 0.3985 0.1172 0.1144 0.0752 1.0000 Uiso H141 0.4544 0.0820 0.0306 0.0785 1.0000 Uiso H2111 0.9923 0.2111 0.1813 0.0693 1.0000 Uiso H2121 1.1047 0.2726 0.2440 0.0819 1.0000 Uiso H2131 1.1170 0.4115 0.2475 0.0874 1.0000 Uiso H2141 1.0227 0.4862 0.1849 0.0845 1.0000 Uiso H2151 0.9039 0.4239 0.1219 0.0719 1.0000 Uiso H3111 0.8301 0.0017 -0.0676 0.0731 1.0000 Uiso H3121 0.8743 -0.0388 -0.1499 0.0759 1.0000 Uiso H3131 0.8717 0.0525 -0.2169 0.0721 1.0000 Uiso H3141 0.8399 0.1902 -0.1982 0.0824 1.0000 Uiso H3151 0.8062 0.2279 -0.1130 0.0666 1.0000 Uiso 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 I1 0.0538(3) 0.0626(3) 0.0734(4) -0.0180(3) -0.0040(3) -0.0000(3) I2 0.0644(4) 0.0783(4) 0.0636(4) -0.0154(3) -0.0011(3) 0.0074(3) I3 0.0905(5) 0.0635(3) 0.0602(4) -0.0050(3) 0.0010(3) 0.0019(3) I4 0.0619(4) 0.0560(3) 0.0695(4) -0.0010(3) 0.0093(3) -0.0018(3) O1 0.054(3) 0.085(4) 0.040(3) -0.008(3) 0.015(3) -0.002(3) O2 0.062(4) 0.103(5) 0.066(4) -0.027(4) 0.005(3) -0.032(4) N1 0.043(4) 0.052(4) 0.045(4) 0.004(3) -0.003(3) 0.000(3) N2 0.040(3) 0.066(4) 0.033(3) -0.008(3) 0.005(3) -0.003(3) N3 0.038(3) 0.052(4) 0.048(4) -0.002(3) -0.001(3) 0.001(3) C1 0.042(4) 0.050(4) 0.045(5) 0.000(4) 0.008(4) 0.005(3) C2 0.053(5) 0.054(5) 0.059(5) 0.001(4) -0.001(4) -0.008(4) C3 0.049(5) 0.073(5) 0.041(4) -0.007(4) 0.010(4) -0.007(4) C4 0.044(5) 0.057(4) 0.043(5) -0.007(4) 0.004(3) -0.003(4) C11 0.043(4) 0.049(4) 0.058(5) 0.007(4) 0.003(4) 0.008(4) C12 0.051(5) 0.074(5) 0.059(5) -0.001(4) 0.013(4) 0.003(4) C13 0.040(5) 0.083(6) 0.075(7) 0.001(5) 0.009(5) -0.012(4) C14 0.047(5) 0.077(6) 0.069(6) -0.002(5) 0.002(5) -0.013(4) C15 0.031(4) 0.059(5) 0.054(5) -0.003(4) 0.003(4) -0.001(3) C211 0.058(5) 0.074(6) 0.046(5) 0.002(4) -0.004(5) 0.003(4) C212 0.054(6) 0.118(9) 0.046(5) 0.003(5) -0.008(4) 0.005(5) C213 0.051(6) 0.117(9) 0.058(6) -0.021(6) -0.001(5) -0.006(6) C214 0.063(6) 0.074(6) 0.081(7) -0.027(5) -0.002(6) -0.011(5) C215 0.050(5) 0.062(5) 0.073(6) 0.005(5) 0.002(5) 0.004(4) C311 0.057(5) 0.049(5) 0.077(7) 0.002(4) -0.003(5) 0.004(4) C312 0.061(5) 0.067(5) 0.064(6) -0.008(5) 0.013(5) 0.002(4) C313 0.048(5) 0.098(7) 0.046(5) -0.016(5) 0.005(4) -0.005(5) C314 0.072(6) 0.088(7) 0.055(6) 0.011(5) 0.004(5) -0.014(5) C315 0.059(5) 0.056(5) 0.056(5) 0.000(4) 0.008(4) -0.010(4) _refine_ls_extinction_method 'None' 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 I1 . I2 . 2.835(1) yes I1 . I3 . 3.1684(9) yes O1 . C1 . 1.195(9) yes O2 . C2 . 1.21(1) yes N1 . C11 . 1.35(1) yes N1 . C15 . 1.36(1) yes N2 . C3 . 1.46(1) yes N2 . C211 . 1.35(1) yes N2 . C215 . 1.34(1) yes N3 . C4 . 1.47(1) yes N3 . C311 . 1.33(1) yes N3 . C315 . 1.34(1) yes C1 . C3 . 1.521(11) yes C1 . C11 . 1.493(11) yes C2 . C4 . 1.516(11) yes C2 . C15 . 1.462(11) yes C3 . H31 . 0.960(8) no C3 . H32 . 0.962(8) no C4 . H41 . 0.961(8) no C4 . H42 . 0.969(8) no C11 . C12 . 1.391(11) yes C12 . C13 . 1.363(12) yes C12 . H121 . 0.960(9) no C13 . C14 . 1.365(12) yes C13 . H131 . 0.965(8) no C14 . C15 . 1.402(11) yes C14 . H141 . 0.960(9) no C211 . C212 . 1.356(12) yes C211 . H2111 . 0.953(9) no C212 . C213 . 1.359(14) yes C212 . H2121 . 0.952(9) no C213 . C214 . 1.363(14) yes C213 . H2131 . 0.961(9) no C214 . C215 . 1.391(12) yes C214 . H2141 . 0.958(9) no C215 . H2151 . 0.962(9) no C311 . C312 . 1.346(13) yes C311 . H3111 . 0.956(9) no C312 . C313 . 1.351(13) yes C312 . H3121 . 0.959(9) no C313 . C314 . 1.392(14) yes C313 . H3131 . 0.962(8) no C314 . C315 . 1.367(13) yes C314 . H3141 . 0.963(9) no C315 . H3151 . 0.958(8) 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 I2 . I1 . I3 . 178.35(3) yes C11 . N1 . C15 . 116.6(7) yes C3 . N2 . C211 . 118.3(7) yes C3 . N2 . C215 . 120.1(7) yes C211 . N2 . C215 . 121.5(7) yes C4 . N3 . C311 . 118.7(7) yes C4 . N3 . C315 . 120.0(6) yes C311 . N3 . C315 . 121.2(7) yes O1 . C1 . C3 . 123.2(7) yes O1 . C1 . C11 . 121.4(7) yes C3 . C1 . C11 . 115.4(7) yes O2 . C2 . C4 . 121.5(8) yes O2 . C2 . C15 . 121.9(8) yes C4 . C2 . C15 . 116.6(7) yes N2 . C3 . C1 . 108.7(6) yes N2 . C3 . H31 . 109.6(7) no C1 . C3 . H31 . 109.9(7) no N2 . C3 . H32 . 109.4(7) no C1 . C3 . H32 . 110.0(7) no H31 . C3 . H32 . 109.2(8) no N3 . C4 . C2 . 110.3(6) yes N3 . C4 . H41 . 109.6(7) no C2 . C4 . H41 . 109.9(7) no N3 . C4 . H42 . 108.9(7) no C2 . C4 . H42 . 109.5(7) no H41 . C4 . H42 . 108.6(7) no N1 . C11 . C1 . 113.8(7) yes N1 . C11 . C12 . 122.8(8) yes C1 . C11 . C12 . 123.3(8) yes C11 . C12 . C13 . 119.7(8) yes C11 . C12 . H121 . 120.0(9) no C13 . C12 . H121 . 120.3(9) no C12 . C13 . C14 . 119.1(8) yes C12 . C13 . H131 . 120.0(9) no C14 . C13 . H131 . 120.8(9) no C13 . C14 . C15 . 119.0(8) yes C13 . C14 . H141 . 119.8(9) no C15 . C14 . H141 . 121.2(9) no N1 . C15 . C2 . 115.2(7) yes N1 . C15 . C14 . 122.6(7) yes C2 . C15 . C14 . 122.2(7) yes N2 . C211 . C212 . 120.0(8) yes N2 . C211 . H2111 . 120.6(8) no C212 . C211 . H2111 . 119.3(9) no C211 . C212 . C213 . 120.6(9) yes C211 . C212 . H2121 . 120.3(11) no C213 . C212 . H2121 . 119.1(10) no C212 . C213 . C214 . 118.8(9) yes C212 . C213 . H2131 . 121.9(12) no C214 . C213 . H2131 . 119.3(12) no C213 . C214 . C215 . 120.6(9) yes C213 . C214 . H2141 . 119.7(10) no C215 . C214 . H2141 . 119.7(11) no N2 . C215 . C214 . 118.3(8) yes N2 . C215 . H2151 . 121.1(9) no C214 . C215 . H2151 . 120.6(9) no N3 . C311 . C312 . 120.6(8) yes N3 . C311 . H3111 . 120.1(9) no C312 . C311 . H3111 . 119.3(8) no C311 . C312 . C313 . 120.1(8) yes C311 . C312 . H3121 . 120.1(10) no C313 . C312 . H3121 . 119.8(9) no C312 . C313 . C314 . 119.4(8) yes C312 . C313 . H3131 . 120.3(10) no C314 . C313 . H3131 . 120.3(10) no C313 . C314 . C315 . 118.7(8) yes C313 . C314 . H3141 . 121.7(10) no C315 . C314 . H3141 . 119.6(10) no N3 . C315 . C314 . 119.9(8) yes N3 . C315 . H3151 . 119.6(8) no C314 . C315 . H3151 . 120.5(9) no #END #============================================================================== data_(RhL1Cl3) _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C30 H33 Cl5 N3 Rh1' _chemical_formula_weight 715.75 _chemical_melting_point ? _chemical_compound_source synthesis 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 2(1) 2(1) 2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 7.981(1) _cell_length_b 15.571(2) _cell_length_c 24.630(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3060.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 16 _cell_measurement_theta_min 14.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description 'hexagonal rods' _exptl_crystal_colour brown _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method ? _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 1.020 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe AED2 4-circle diffractometer' _diffrn_measurement_method \w/2\q _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 1.5 _diffrn_reflns_number 3075 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3075 _reflns_number_observed 2930 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'STADI4 (Stoe & Cie GmbH, Darmstadt, 1996)' _computing_cell_refinement 'STADI4 (Stoe & Cie GmbH, Darmstadt, 1996)' _computing_data_reduction 'X-RED (Stoe & Cie GmbH, Darmstadt, 1996) ' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON/PLUTON (Spek, 1993)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+3.2676P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ; Hydrogen atoms were included in calculated positions using SHELXL default parameters. ; _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0004(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(5) _refine_ls_number_reflns 3072 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_obs 0.0396 _refine_ls_wR_factor_all 0.1068 _refine_ls_wR_factor_obs 0.1020 _refine_ls_goodness_of_fit_all 1.106 _refine_ls_goodness_of_fit_obs 1.101 _refine_ls_restrained_S_all 1.122 _refine_ls_restrained_S_obs 1.101 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Rh Rh 0.86834(5) 0.77216(3) 0.79644(2) 0.0152(2) Uani 1 d . . Cl(1) Cl 0.6594(2) 0.88045(8) 0.79870(6) 0.0208(3) Uani 1 d . . Cl(2) Cl 0.7318(2) 0.69531(10) 0.86469(6) 0.0240(3) Uani 1 d . . Cl(3) Cl 1.0142(2) 0.84237(9) 0.72721(6) 0.0236(3) Uani 1 d . . N(1) N 1.0401(6) 0.6840(3) 0.7949(2) 0.0174(10) Uani 1 d . N(2) N 1.0368(7) 0.8216(3) 0.8546(2) 0.0188(11) Uani 1 d . . N(3) N 0.7621(6) 0.6885(3) 0.7383(2) 0.0177(10) Uani 1 d . . C1 C 1.0092(8) 0.6114(4) 0.7675(2) 0.0200(13) Uani 1 d . . C2 C 1.1338(9) 0.5488(4) 0.7634(3) 0.0245(13) Uani 1 d . . H2 H 1.1146(9) 0.4971(4) 0.7439(3) 0.029 Uiso 1 calc R . C3 C 1.2846(8) 0.5641(4) 0.7882(3) 0.0272(14) Uani 1 d . . H3 H 1.3704(8) 0.5219(4) 0.7862(3) 0.033 Uiso 1 calc R . C4 C 1.3143(8) 0.6399(4) 0.8162(3) 0.0233(14) Uani 1 d . . H4 H 1.4195(8) 0.6507(4) 0.8329(3) 0.028 Uiso 1 calc R . C5 C 1.1856(8) 0.6992(4) 0.8189(2) 0.0173(12) Uani 1 d . . C6 C 1.1889(7) 0.7802(4) 0.8505(2) 0.0188(12) Uani 1 d . . C7 C 1.3291(8) 0.8059(4) 0.8783(3) 0.0248(14) Uani 1 d . . H7 H 1.4327(8) 0.7769(4) 0.8733(3) 0.030 Uiso 1 calc R . C8 C 1.3179(8) 0.8745(4) 0.9136(3) 0.0264(15) Uani 1 d . . H8 H 1.4144(8) 0.8944(4) 0.9324(3) 0.032 Uiso 1 calc R . C9 C 1.1645(8) 0.9139(4) 0.9214(3) 0.0256(14) Uani 1 d . . C10 C 1.0239(8) 0.8848(4) 0.8912(2) 0.0215(13) Uani 1 d . . C11 C 0.8452(8) 0.6102(4) 0.7399(2) 0.0198(13) Uani 1 d . . C12 C 0.7828(8) 0.5382(4) 0.7149(3) 0.0239(14) Uani 1 d . . H12 H 0.8382(8) 0.4845(4) 0.7189(3) 0.029 Uiso 1 calc R . C13 C 0.6401(9) 0.5442(4) 0.6840(3) 0.0258(14) Uani 1 d . . H13 H 0.5922(9) 0.4942(4) 0.6682(3) 0.031 Uiso 1 calc R . C14 C 0.5665(8) 0.6239(4) 0.6761(3) 0.0216(13) Uani 1 d . . C15 C 0.6301(8) 0.6956(3) 0.7053(2) 0.0185(11) Uani 1 d . . C16 C 1.1326(10) 0.9817(4) 0.9638(3) 0.031(2) Uani 1 d . . H16 H 1.2335(10) 1.0038(4) 0.9834(3) 0.037 Uiso 1 calc R . C17 C 1.0150(10) 1.0503(4) 0.9392(3) 0.035(2) Uani 1 d . . H17A H 1.0113(10) 1.1050(4) 0.9597(3) 0.042 Uiso 1 calc R . H17B H 1.0310(10) 1.0603(4) 0.8999(3) 0.042 Uiso 1 calc R . C18 C 0.8731(9) 0.9875(4) 0.9530(3) 0.0280(14) Uani 1 d . . H18 H 0.7662(9) 1.0151(4) 0.9650(3) 0.034 Uiso 1 calc R . C19 C 0.8555(9) 0.9243(4) 0.9057(3) 0.0260(14) Uani 1 d . . H19A H 0.7760(9) 0.8782(4) 0.9158(3) 0.031 Uiso 1 calc R . H19B H 0.8097(9) 0.9547(4) 0.8737(3) 0.031 Uiso 1 calc R . C20 C 0.9843(9) 0.9513(4) 1.0001(2) 0.0287(15) Uani 1 d . . C21 C 0.9720(11) 0.8562(5) 1.0142(3) 0.037(2) Uani 1 d . . H21A H 1.0716(35) 0.8389(10) 1.0348(20) 0.056 Uiso 1 calc R . H21B H 0.9650(73) 0.8224(5) 0.9808(3) 0.056 Uiso 1 calc R . H21C H 0.8716(39) 0.8462(8) 1.0363(20) 0.056 Uiso 1 calc R . C22 C 0.9714(11) 1.0051(5) 1.0521(3) 0.043(2) Uani 1 d . . H22A H 0.9651(82) 1.0661(6) 1.0425(3) 0.065 Uiso 1 calc R . H22B H 1.0704(42) 0.9950(32) 1.0747(13) 0.065 Uiso 1 calc R . H22C H 0.8704(46) 0.9886(30) 1.0722(14) 0.065 Uiso 1 calc R . C23 C 0.5523(8) 0.7823(4) 0.6936(3) 0.0259(14) Uani 1 d . . H23A H 0.6402(8) 0.8228(4) 0.6813(3) 0.031 Uiso 1 calc R . H23B H 0.5013(8) 0.8057(4) 0.7271(3) 0.031 Uiso 1 calc R . C24 C 0.4167(9) 0.7735(4) 0.6490(3) 0.0283(14) Uani 1 d . . H24 H 0.3593(9) 0.8284(4) 0.6391(3) 0.034 Uiso 1 calc R . C25 C 0.2992(9) 0.7005(4) 0.6654(3) 0.0279(15) Uani 1 d . . H25A H 0.1881(9) 0.7022(4) 0.6475(3) 0.033 Uiso 1 calc R . H25B H 0.2885(9) 0.6920(4) 0.7051(3) 0.033 Uiso 1 calc R . C26 C 0.4265(8) 0.6405(4) 0.6379(3) 0.0250(14) Uani 1 d . . H26 H 0.3790(8) 0.5891(4) 0.6191(3) 0.030 Uiso 1 calc R . C27 C 0.4760(9) 0.7187(4) 0.6000(3) 0.0288(15) Uani 1 d . . C28 C 0.3584(11) 0.7252(5) 0.5510(3) 0.039(2) Uani 1 d . . H28A H 0.2421(12) 0.7188(36) 0.5632(4) 0.059 Uiso 1 calc R . H28B H 0.3852(49) 0.6796(24) 0.5250(11) 0.059 Uiso 1 calc R . H28C H 0.3725(52) 0.7813(16) 0.5336(14) 0.059 Uiso 1 calc R . C29 C 0.6565(10) 0.7264(5) 0.5805(3) 0.039(2) Uani 1 d . . H29A H 0.7328(10) 0.7188(33) 0.6113(5) 0.058 Uiso 1 calc R . H29B H 0.6741(20) 0.7833(13) 0.5644(19) 0.058 Uiso 1 calc R . H29C H 0.6788(22) 0.6821(22) 0.5532(16) 0.058 Uiso 1 calc R . Cl4 Cl 0.5554(5) 0.5956(2) 0.43015(11) 0.0848(10) Uani 1 d . . Cl5 Cl 0.4692(4) 0.4163(2) 0.44694(14) 0.0840(9) Uani 1 d . . C30 C 0.5284(14) 0.4932(8) 0.4004(4) 0.076(4) Uani 1 d . . H30A H 0.4421(14) 0.4970(8) 0.3716(4) 0.091 Uiso 1 calc R . H30B H 0.6348(14) 0.4753(8) 0.3831(4) 0.091 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh 0.0139(2) 0.0092(2) 0.0225(2) 0.0003(2) 0.0007(2) 0.0012(2) Cl(1) 0.0198(7) 0.0142(6) 0.0283(7) -0.0031(6) -0.0016(7) 0.0055(5) Cl(2) 0.0185(7) 0.0227(7) 0.0307(8) 0.0083(6) 0.0038(7) 0.0011(6) Cl(3) 0.0267(8) 0.0135(6) 0.0305(7) 0.0009(6) 0.0079(7) -0.0008(7) N(1) 0.017(2) 0.011(2) 0.024(2) -0.001(2) 0.003(2) 0.000(2) N(2) 0.019(3) 0.013(2) 0.025(3) 0.003(2) 0.004(2) 0.002(2) N(3) 0.019(3) 0.010(2) 0.024(2) 0.000(2) 0.002(2) -0.001(2) C1 0.017(3) 0.014(3) 0.029(3) 0.004(2) 0.001(3) 0.000(3) C2 0.022(3) 0.010(3) 0.041(4) 0.004(3) 0.004(3) 0.001(3) C3 0.020(3) 0.019(3) 0.043(4) -0.004(3) 0.004(3) 0.008(3) C4 0.014(3) 0.019(3) 0.037(3) 0.001(3) 0.003(3) 0.000(3) C5 0.016(3) 0.013(3) 0.024(3) -0.001(2) 0.003(2) -0.001(2) C6 0.016(3) 0.014(3) 0.026(3) 0.001(3) 0.002(2) -0.003(3) C7 0.017(3) 0.022(3) 0.035(3) 0.000(3) 0.004(3) -0.001(3) C8 0.016(3) 0.028(3) 0.034(3) -0.003(3) -0.003(3) -0.004(3) C9 0.025(4) 0.024(3) 0.028(3) 0.001(3) -0.002(3) -0.004(3) C10 0.019(3) 0.020(3) 0.026(3) 0.007(3) 0.000(3) 0.002(3) C11 0.021(3) 0.010(2) 0.029(3) -0.003(2) 0.003(3) 0.000(3) C12 0.023(3) 0.012(3) 0.037(4) -0.001(2) 0.004(3) 0.000(3) C13 0.027(3) 0.014(3) 0.036(3) -0.003(3) 0.001(3) -0.007(3) C14 0.023(3) 0.014(3) 0.028(3) 0.001(3) 0.003(3) -0.002(3) C15 0.023(3) 0.011(2) 0.021(3) -0.003(2) 0.004(3) -0.001(2) C16 0.028(3) 0.027(3) 0.037(4) -0.013(3) -0.008(3) 0.000(3) C17 0.036(4) 0.025(3) 0.044(4) -0.012(3) -0.003(4) 0.002(3) C18 0.027(3) 0.026(3) 0.031(3) -0.002(3) -0.005(3) 0.007(3) C19 0.024(3) 0.024(3) 0.030(3) -0.001(3) -0.001(3) 0.004(3) C20 0.031(4) 0.031(3) 0.024(3) -0.010(3) -0.004(3) 0.007(3) C21 0.044(5) 0.038(4) 0.031(3) 0.002(3) -0.002(4) 0.008(4) C22 0.050(5) 0.051(5) 0.029(4) -0.014(4) -0.006(4) 0.001(4) C23 0.030(3) 0.017(3) 0.031(3) -0.003(3) -0.012(3) 0.005(3) C24 0.027(3) 0.020(3) 0.037(3) 0.003(3) -0.007(3) 0.003(3) C25 0.022(3) 0.029(3) 0.033(3) -0.004(3) -0.001(3) 0.001(3) C26 0.023(3) 0.020(3) 0.032(3) -0.003(3) -0.005(3) -0.003(3) C27 0.036(4) 0.023(3) 0.027(3) 0.002(3) 0.000(3) -0.003(3) C28 0.048(4) 0.038(4) 0.032(3) -0.002(3) -0.005(4) 0.006(5) C29 0.041(4) 0.039(4) 0.037(4) 0.012(3) 0.010(3) 0.002(4) Cl4 0.107(3) 0.078(2) 0.069(2) -0.0151(14) -0.006(2) 0.015(2) Cl5 0.053(2) 0.096(2) 0.103(2) -0.040(2) 0.015(2) 0.000(2) C30 0.050(6) 0.129(10) 0.048(5) -0.042(6) -0.003(5) 0.006(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh N(1) 1.940(5) . ? Rh N(2) 2.109(5) . ? Rh N(3) 2.112(5) . ? Rh Cl(2) 2.333(2) . ? Rh Cl(3) 2.336(2) . ? Rh Cl(1) 2.3720(14) . ? N(1) C5 1.324(8) . ? N(1) C1 1.341(8) . ? N(2) C10 1.340(8) . ? N(2) C6 1.378(8) . ? N(3) C15 1.336(8) . ? N(3) C11 1.389(7) . ? C1 C2 1.395(9) . ? C1 C11 1.475(9) . ? C2 C3 1.371(10) . ? C3 C4 1.387(9) . ? C4 C5 1.383(9) . ? C5 C6 1.483(8) . ? C6 C7 1.372(9) . ? C7 C8 1.381(9) . ? C8 C9 1.382(9) . ? C9 C10 1.420(9) . ? C9 C16 1.506(9) . ? C10 C19 1.520(9) . ? C11 C12 1.373(8) . ? C12 C13 1.373(10) . ? C13 C14 1.387(9) . ? C14 C15 1.421(8) . ? C14 C26 1.484(9) . ? C15 C23 1.515(8) . ? C16 C17 1.546(10) . ? C16 C20 1.557(11) . ? C17 C18 1.534(10) . ? C18 C19 1.533(9) . ? C18 C20 1.565(9) . ? C20 C21 1.525(10) . ? C20 C22 1.533(9) . ? C23 C24 1.547(9) . ? C24 C25 1.529(10) . ? C24 C27 1.552(9) . ? C25 C26 1.537(9) . ? C26 C27 1.583(9) . ? C27 C29 1.524(10) . ? C27 C28 1.532(10) . ? Cl4 C30 1.769(11) . ? Cl5 C30 1.723(12) . ? 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 N(1) Rh N(2) 79.7(2) . . ? N(1) Rh N(3) 80.5(2) . . ? N(2) Rh N(3) 160.1(2) . . ? N(1) Rh Cl(2) 88.9(2) . . ? N(2) Rh Cl(2) 89.76(14) . . ? N(3) Rh Cl(2) 89.11(13) . . ? N(1) Rh Cl(3) 88.0(2) . . ? N(2) Rh Cl(3) 90.40(14) . . ? N(3) Rh Cl(3) 89.67(14) . . ? Cl(2) Rh Cl(3) 176.82(6) . . ? N(1) Rh Cl(1) 179.6(2) . . ? N(2) Rh Cl(1) 99.95(14) . . ? N(3) Rh Cl(1) 99.91(14) . . ? Cl(2) Rh Cl(1) 91.12(5) . . ? Cl(3) Rh Cl(1) 91.99(5) . . ? C5 N(1) C1 122.4(5) . . ? C5 N(1) Rh 119.0(4) . . ? C1 N(1) Rh 118.5(4) . . ? C10 N(2) C6 117.4(5) . . ? C10 N(2) Rh 132.5(4) . . ? C6 N(2) Rh 110.0(4) . . ? C15 N(3) C11 117.8(5) . . ? C15 N(3) Rh 132.7(4) . . ? C11 N(3) Rh 109.4(4) . . ? N(1) C1 C2 119.6(6) . . ? N(1) C1 C11 114.0(5) . . ? C2 C1 C11 126.2(6) . . ? C3 C2 C1 118.2(6) . . ? C2 C3 C4 121.3(6) . . ? C5 C4 C3 117.7(6) . . ? N(1) C5 C4 120.7(5) . . ? N(1) C5 C6 113.7(5) . . ? C4 C5 C6 125.5(6) . . ? C7 C6 N(2) 123.1(5) . . ? C7 C6 C5 121.7(6) . . ? N(2) C6 C5 114.9(5) . . ? C6 C7 C8 119.2(6) . . ? C7 C8 C9 119.2(6) . . ? C8 C9 C10 119.1(6) . . ? C8 C9 C16 123.8(6) . . ? C10 C9 C16 116.9(6) . .? N(2) C10 C9 121.7(6) . . ? N(2) C10 C19 121.6(6) . . ? C9 C10 C19 116.5(5) . . ? C12 C11 N(3) 122.1(6) . . ? C12 C11 C1 122.6(6) . . ? N(3) C11 C1 115.2(5) . . ? C13 C12 C11 119.6(6) . . ? C12 C13 C14 119.3(6) . . ? C13 C14 C15 118.7(6) . . ? C13 C14 C26 124.3(6) . . ? C15 C14 C26 117.0(5) . . ? N(3) C15 C14 121.7(5) . . ? N(3) C15 C23 120.9(5) . . ? C14 C15 C23 117.2(5) . . ? C9 C16 C17 108.4(6) . . ? C9 C16 C20 108.3(6) . . ? C17 C16 C20 88.4(6) . . ? C18 C17 C16 85.4(5) . . ? C19 C18 C17 108.0(6) . . ? C19 C18 C20 112.6(5) . . ? C17 C18 C20 88.6(6) . . ? C10 C19 C18 110.9(6) . . ? C21 C20 C22 109.6(6) . . ? C21 C20 C16 118.3(6) . . ? C22 C20 C16 111.4(6) . . ? C21 C20 C18 118.9(6) . . ? C22 C20 C18 112.5(6) . . ? C16 C20 C18 84.0(5) . . ? C15 C23 C24 110.1(5) . . ? C25 C24 C23 108.0(5) . . ? C25 C24 C27 89.0(5) . . ? C23 C24 C27 112.8(5) . . ? C24 C25 C26 86.0(5) . . ? C14 C26 C25 108.9(5) . . ? C14 C26 C27 108.7(5) . . ? C25 C26 C27 87.6(5) . . ? C29 C27 C28 109.0(6) . . ? C29 C27 C24 119.4(6) . . ? C28 C27 C24 112.9(6) . . ? C29 C27 C26 118.8(6) . . ? C28 C27 C26 111.2(6) . . ? C24 C27 C26 83.6(5) . . ? Cl5 C30 Cl4 112.6(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 N(2) Rh N(1) C5 -12.5(4) . . . . ? N(3) Rh N(1) C5 168.3(5) . . . . ? Cl(2) Rh N(1) C5 -102.5(4) . . . . ? Cl(3) Rh N(1) C5 78.3(4) . . . . ? Cl(1) Rh N(1) C5 -7.7(190) . . . . ? N(2) Rh N(1) C1 170.4(5) . . . . ? N(3) Rh N(1) C1 -8.8(4) . . . . ? Cl(2) Rh N(1) C1 80.4(4) . . . . ? Cl(3) Rh N(1) C1 -98.8(4) . . . . ? Cl(1) Rh N(1) C1 175.2(1000) . . . . ? N(1) Rh N(2) C10 -167.9(6) . . . . ? N(3) Rh N(2) C10 -165.6(5) . . . . ? Cl(2) Rh N(2) C10 -78.9(5) . . . . ? Cl(3) Rh N(2) C10 104.3(5) . . . . ? Cl(1) Rh N(2) C10 12.2(5) . . . . ? N(1) Rh N(2) C6 14.9(4) . . . . ? N(3) Rh N(2) C6 17.1(8) . . . . ? Cl(2) Rh N(2) C6 103.8(4) . . . . ? Cl(3) Rh N(2) C6 -73.0(4) . . . . ? Cl(1) Rh N(2) C6 -165.1(3) . . . . ? N(1) Rh N(3) C15 -171.3(5) . . . . ? N(2) Rh N(3) C15 -173.5(5) . . . . ? Cl(2) Rh N(3) C15 99.6(5) . . . . ? Cl(3) Rh N(3) C15 -83.3(5) . . . . ? Cl(1) Rh N(3) C15 8.7(5) . . . . ? N(1) Rh N(3) C11 13.9(4) . . . . ? N(2) Rh N(3) C11 11.7(8) . . . . ? Cl(2) Rh N(3) C11 -75.1(4) . . . . ? Cl(3) Rh N(3) C11 101.9(4) . . . . ? Cl(1) Rh N(3) C11 -166.1(4) . . . . ? C5 N(1) C1 C2 -0.3(9) . . . . ? Rh N(1) C1 C2 176.7(4) . . . . ? C5 N(1) C1 C11 -175.0(5) . . . . ? Rh N(1) C1 C11 2.0(7) . . . . ? N(1) C1 C2 C3 0.4(9) . . . . ? C11 C1 C2 C3 174.4(6) . . . . ? C1 C2 C3 C4 -0.8(10) . . . . ? C2 C3 C4 C5 1.0(10) . . . . ? C1 N(1) C5 C4 0.5(9) . . . . ? Rh N(1) C5 C4 -176.4(4) . . . . ? C1 N(1) C5 C6 -175.6(5) . . . . ? Rh N(1) C5 C6 7.5(7) . . . . ? C3 C4 C5 N(1) -0.8(9) . . . . ? C3 C4 C5 C6 174.8(6) . . . . ? C10 N(2) C6 C7 -6.3(9) . . . . ? Rh N(2) C6 C7 171.5(5) . . . . ? C10 N(2) C6 C5 166.8(5) . . . . ? Rh N(2) C6 C5 -15.5(6) . . . . ? N(1) C5 C6 C7 179.7(6) . . . . ? C4 C5 C6 C7 3.8(9) . . . . ? N(1) C5 C6 N(2) 6.5(7) . . . . ? C4 C5 C6 N(2) -169.4(6) . . . . ? N(2) C6 C7 C8 2.5(10) . . . . ? C5 C6 C7 C8 -170.2(6) . . . . ? C6 C7 C8 C9 1.9(10) . . . . ? C7 C8 C9 C10 -2.4(10) . . . . ? C7 C8 C9 C16 172.1(6) . . . . ? C6 N(2) C10 C9 5.7(8) . . . . ? Rh N(2) C10 C9 -171.4(4) . . . . ? C6 N(2) C10 C19 -169.5(6) . . . . ? Rh N(2) C10 C19 13.4(9) . . . . ? C8 C9 C10 N(2) -1.6(10) . . . . ? C16 C9 C10 N(2) -176.4(6) . . . . ? C8 C9 C10 C19 173.9(6) . . . . ? C16 C9 C10 C19 -0.9(8) . . . . ? C15 N(3) C11 C12 -9.2(9) . . . . ? Rh N(3) C11 C12 166.5(5) . . . . ? C15 N(3) C11 C1 167.4(5) . . . . ? Rh N(3) C11 C1 -17.0(6) . . . . ? N(1) C1 C11 C12 -172.6(6) . . . . ? C2 C1 C11 C12 13.1(10) . . . . ? N(1) C1 C11 N(3) 10.9(8) . . . . ? C2 C1 C11 N(3) -163.4(6) . . . . ? N(3) C11 C12 C13 4.7(10) . . . . ? C1 C11 C12 C13 -171.6(6) . . . . ? C11 C12 C13 C14 3.6(9) . . . . ? C12 C13 C14 C15 -7.1(9) . . . . ? C12 C13 C14 C26 171.4(6) . . . . ? C11 N(3) C15 C14 5.4(8) . . . . ? Rh N(3) C15 C14 -169.1(5) . . . . ? C11 N(3) C15 C23 -168.8(6) . . . . ? Rh N(3) C15 C23 16.7(8) . . . . ? C13 C14 C15 N(3) 2.6(9) . . . . ? C26 C14 C15 N(3) -176.0(5) . . . . ? C13 C14 C15 C23 177.0(6) . . . . ? C26 C14 C15 C23 -1.6(8) . . . . ? C8 C9 C16 C17 141.2(7) . . . . ? C10 C9 C16 C17 -44.2(8) . . . . ? C8 C9 C16 C20 -124.2(7) . . . . ? C10 C9 C16 C20 50.4(8) . . . . ? C9 C16 C17 C18 81.3(6) . . . . ? C20 C16 C17 C18 -27.5(5) . . . . ? C16 C17 C18 C19 -86.0(6) . . . . ? C16 C17 C18 C20 27.3(5) . . . . ? N(2) C10 C19 C18 173.5(5) . . . . ? C9 C10 C19 C18 -2.0(8) . . . . ? C17 C18 C19 C10 51.2(7) . . . . ? C20 C18 C19 C10 -45.0(8) . . . . ? C9 C16 C20 C21 37.8(8) . . . . ? C17 C16 C20 C21 146.7(6) . . . . ? C9 C16 C20 C22 166.2(6) . . . . ? C17 C16 C20 C22 -85.0(6) . . . . ? C9 C16 C20 C18 -81.9(6) . . . . ? C17 C16 C20 C18 27.0(4) . . . . ? C19 C18 C20 C21 -37.5(9) . . . . ? C17 C18 C20 C21 -146.4(7) . . . . ? C19 C18 C20 C22 -167.6(6) . . . . ? C17 C18 C20 C22 83.5(7) . . . . ? C19 C18 C20 C16 81.7(6) . . . . ? C17 C18 C20 C16 -27.2(4) . . . . ? N(3) C15 C23 C24 173.0(5) . . . . ? C14 C15 C23 C24 -1.4(8) . . . . ? C15 C23 C24 C25 50.5(7) . . . . ? C15 C23 C24 C27 -46.2(7) . . . . ? C23 C24 C25 C26 -85.5(6) . . . . ? C27 C24 C25 C26 28.2(5) . . . . ? C13 C14 C26 C25 137.8(6) . . . . ? C15 C14 C26 C25 -43.6(7) . . . . ? C13 C14 C26 C27 -128.3(7) . . . . ? C15 C14 C26 C27 50.3(7) . . . . ? C24 C25 C26 C14 81.3(6) . . . . ? C24 C25 C26 C27 -27.6(5) . . . . ? C25 C24 C27 C29 -146.9(6) . . . . ? C23 C24 C27 C29 -37.8(8) . . . . ? C25 C24 C27 C28 82.9(6) . . . . ? C23 C24 C27 C28 -167.9(6) . . . . ? C25 C24 C27 C26 -27.4(5) . . . . ? C23 C24 C27 C26 81.7(6) . . . . ? C14 C26 C27 C29 38.3(8) . . . . ? C25 C26 C27 C29 147.4(6) . . . ? C14 C26 C27 C28 166.0(6) . . . . ? C25 C26 C27 C28 -84.9(6) . . . . ? C14 C26 C27 C24 -81.9(6) . . . . ? C25 C26 C27 C24 27.2(5) . . . . ? _refine_diff_density_max 1.162 _refine_diff_density_min -1.011 _refine_diff_density_rms 0.106 #END #============================================================================== data_(Ru(L1(-))Cl3) _chemical_name_systematic ; ? ; _cell_length_a 7.9867(7) _cell_length_b 15.6250(13) _cell_length_c 25.199(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3144.6(4) _cell_formula_units_Z 4 _symmetry_cell_setting 'Orthorhombic ' _symmetry_space_group_name_H-M 'P 21 21 21 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 'x+1/2,-y+1/2,-z' '-x,y+1/2,-z+1/2' '-x+1/2,-y,z+1/2' 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 ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' 'Ru ' -1.4200 0.8360 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C32 H37 RU1 Cl3 N3 O1 ' _chemical_formula_moiety ' C32 H37 RU1 Cl3 N3 O1 ' _chemical_compound_source ; ? ; _exptl_special_details ; The data were collected on a Stoe Imaging Plate Diffraction System (IPDS) equipped with an Oxford Cryosystems cooler device. The crystal-to-detector distance was 80 mm. 134 exposures (6 min per exposure) were obtained with 0 < \f < 201\% and with the crystals rotated through 1.5\% in \f. Coverage of the unique set was over 100% complete to at least 24.2\%. Crystal decay was monitored by measuring 200 reflexions per image. ; _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Stoe IPDS ' _diffrn_measurement_method \f _diffrn_standards_interval_time 'every image ' _diffrn_standards_interval_count 'every image ' _diffrn_standards_number '200 for each image' _chemical_formula_weight 687.10 _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.08 _cell_measurement_theta_max 24.15 _cell_measurement_temperature 180(2) _exptl_crystal_description ' box ' _exptl_crystal_colour ' dark red ' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.45 _exptl_crystal_F_000 1408.05 _exptl_absorpt_coefficient_mu 0.77 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 180(2) _diffrn_standards_decay_% negligible _diffrn_reflns_number 20175 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 24.15 _reflns_number_total 4945 _reflns_number_observed 4343 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Stoe IPDS software (Stoe, 1996)' _computing_data_reduction 'XRED (Stoe, 1.08, 1996)' _computing_cell_refinement 'Stoe IPDS software (Stoe, 1996)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _computing_structure_refinement 'CRYSTALS Issue 10 (Watkin et al, 1996)' _computing_molecular_graphics 'CAMERON (Watkin, Prout & Pearce, 1996)' _computing_publication_material 'CRYSTALS Issue 10 (Watkin et al, 1996)' _reflns_limit_h_min -9 _reflns_limit_h_max 9 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _refine_diff_density_min -0.52 _refine_diff_density_max 0.44 _refine_ls_number_reflns 4343 _refine_ls_number_parameters 363 _refine_ls_R_factor_obs 0.0217 _refine_ls_wR_factor_obs 0.0244 _refine_ls_goodness_of_fit_obs 1.0626 _refine_ls_shift/esd_max 0.496301 _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme ; Robust-resistant weighting scheme (Prince E, 1982): w=y[1-(\DF/6\s(Fo^2^)]^2^' where y=1/\SArTr(x) with 3 coefficients Ar(2.31, -1.64, 1.76) for the Chebyshev polynomial ArTr(x) where x was Fc/Fc(max). ; _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(4) _atom_sites_solution_primary 'Direct_Methods, SIR92' _atom_sites_solution_hydrogens Geometric _refine_ls_hydrogen_treatment ; H atoms placed geometrically after each cycle ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type RU 0.64614(2) 0.23706(1) 0.294607(8) 0.0146 1.0000 Uani CL(1) 0.85380(8) 0.12809(3) 0.29888(3) 0.0199 1.0000 Uani CL(2) 0.49450(9) 0.16592(4) 0.22895(3) 0.0235 1.0000 Uani CL(3) 0.78057(9) 0.31908(5) 0.36016(3) 0.0230 1.0000 Uani N(1) 0.4736(3) 0.3267(1) 0.29124(9) 0.0174 1.0000 Uani N(2) 0.7515(3) 0.3194(1) 0.23511(9) 0.0187 1.0000 Uani N(3) 0.4720(3) 0.1907(1) 0.35234(9) 0.0197 1.0000 Uani C1 0.3267(4) 0.3128(2) 0.3153(1) 0.0203 1.0000 Uani C2 0.1982(3) 0.3732(2) 0.3112(1) 0.0245 1.0000 Uani C3 0.2300(4) 0.4468(2) 0.2821(1) 0.0254 1.0000 Uani C4 0.3814(4) 0.4598(2) 0.2574(1) 0.0257 1.0000 Uani C5 0.5033(4) 0.3974(2) 0.2621(1) 0.0195 1.0000 Uani C6 0.6676(4) 0.3965(2) 0.2353(1) 0.0217 1.0000 Uani C7 0.7285(3) 0.4674(2) 0.2080(1) 0.0230 1.0000 Uani C8 0.8685(4) 0.4588(2) 0.1765(1) 0.0249 1.0000 Uani C9 0.9426(4) 0.3793(2) 0.1714(1) 0.0227 1.0000 Uani C10 0.8815(3) 0.3100(2) 0.2020(1) 0.0201 1.0000 Uani C11 0.3208(3) 0.2341(2) 0.3475(1) 0.0198 1.0000 Uani C12 0.1800(3) 0.2090(2) 0.3739(1) 0.0241 1.0000 Uani C13 0.1854(3) 0.1399(2) 0.4076(1) 0.0244 1.0000 Uani C14 0.3386(4) 0.0999(2) 0.4166(1) 0.0253 1.0000 Uani C15 0.4796(3) 0.1272(2) 0.3888(1) 0.0192 1.0000 Uani C16 1.0823(4) 0.3596(2) 0.1333(1) 0.0290 1.0000 Uani C17 1.2125(4) 0.3037(2) 0.1623(1) 0.0333 1.0000 Uani C18 1.0962(4) 0.2282(2) 0.1503(1) 0.0268 1.0000 Uani C19 0.9629(4) 0.2239(2) 0.1936(1) 0.0253 1.0000 Uani C20 1.0337(4) 0.2784(2) 0.1000(1) 0.0312 1.0000 Uani C21 0.8554(5) 0.2682(2) 0.0815(1) 0.0428 1.0000 Uani C22 1.1543(6) 0.2666(2) 0.0532(1) 0.0434 1.0000 Uani C23 0.4831(5) -0.0377(2) 0.4338(1) 0.0345 1.0000 Uani C24 0.6247(4) 0.0233(2) 0.4487(1) 0.0252 1.0000 Uani C25 0.6453(4) 0.0880(2) 0.4035(1) 0.0256 1.0000 Uani C26 0.3624(4) 0.0307(2) 0.4571(1) 0.0305 1.0000 Uani C27 0.5106(4) 0.0582(2) 0.4941(1) 0.0314 1.0000 Uani C28 0.5184(5) 0.0018(3) 0.5444(1) 0.0414 1.0000 Uani C29 0.5249(5) 0.1517(2) 0.5103(1) 0.0406 1.0000 Uani C30 0.4989(5) 0.5110(3) 0.4463(2) 0.0486 1.0000 Uani C31 0.4738(6) 0.4152(4) 0.4464(2) 0.0662 1.0000 Uani C32 0.523(1) 0.5508(6) 0.3945(3) 0.1044 1.0000 Uani O30 0.5007(4) 0.5493(2) 0.4874(1) 0.0598 1.0000 Uani H21 0.0915 0.3638 0.3275 0.0305 1.0000 Uiso H31 0.1447 0.4896 0.2793 0.0332 1.0000 Uiso H41 0.4024 0.5110 0.2376 0.0303 1.0000 Uiso H71 0.6724 0.5217 0.2109 0.0278 1.0000 Uiso H81 0.9147 0.5075 0.1587 0.0309 1.0000 Uiso H121 0.0761 0.2393 0.3688 0.0308 1.0000 Uiso H131 0.0858 0.1196 0.4248 0.0281 1.0000 Uiso H161 1.1101 0.4140 0.1176 0.0348 1.0000 Uiso H171 1.3208 0.3010 0.1456 0.0425 1.0000 Uiso H172 1.2267 0.3164 0.1994 0.0425 1.0000 Uiso H181 1.1338 0.1698 0.1475 0.0351 1.0000 Uiso H191 1.0136 0.2057 0.2261 0.0310 1.0000 Uiso H192 0.8779 0.1835 0.1833 0.0310 1.0000 Uiso H211 0.8448 0.2160 0.0618 0.0545 1.0000 Uiso H212 0.8259 0.3158 0.0591 0.0545 1.0000 Uiso H213 0.7820 0.2668 0.1116 0.0545 1.0000 Uiso H221 1.1232 0.2167 0.0332 0.0569 1.0000 Uiso H222 1.2670 0.2597 0.0661 0.0569 1.0000 Uiso H223 1.1500 0.3160 0.0304 0.0569 1.0000 Uiso H231 0.4838 -0.0916 0.4519 0.0424 1.0000 Uiso H232 0.4706 -0.0475 0.3962 0.0424 1.0000 Uiso H241 0.7373 0.0047 0.4559 0.0315 1.0000 Uiso H251 0.7208 0.1321 0.4146 0.0308 1.0000 Uiso H252 0.6907 0.0590 0.3731 0.0308 1.0000 Uiso H261 0.2521 0.0175 0.4696 0.0384 1.0000 Uiso H281 0.4471 0.0255 0.5711 0.0548 1.0000 Uiso H282 0.6316 -0.0003 0.5571 0.0548 1.0000 Uiso H283 0.4817 -0.0550 0.5357 0.0548 1.0000 Uiso H291 0.4477 0.1631 0.5387 0.0491 1.0000 Uiso H292 0.6370 0.1631 0.5222 0.0491 1.0000 Uiso H293 0.4992 0.1872 0.4805 0.0491 1.0000 Uiso H311 0.4579 0.3959 0.4820 0.0862 1.0000 Uiso H312 0.5692 0.3883 0.4310 0.0862 1.0000 Uiso H313 0.3754 0.4018 0.4257 0.0862 1.0000 Uiso H321 0.5380 0.6120 0.3992 0.1293 1.0000 Uiso H322 0.6207 0.5275 0.3782 0.1293 1.0000 Uiso H323 0.4269 0.5410 0.3728 0.1293 1.0000 Uiso 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 RU 0.01428(8) 0.01394(8) 0.01612(8) -0.00114(8) -0.00145(9) 0.00189(8) Cl(1) 0.0209(3) 0.0197(3) 0.0224(3) 0.0023(3) 0.0029(3) 0.0070(3) Cl(2) 0.0309(4) 0.0196(3) 0.0256(3) -0.0034(3) -0.0104(3) -0.0001(3) Cl(3) 0.0182(3) 0.0309(4) 0.0262(3) -0.0111(3) -0.0034(3) 0.0011(3) N(1) 0.016(1) 0.018(1) 0.019(1) -0.003(1) -0.003(1) -0.0025(8) N(2) 0.020(1) 0.016(1) 0.022(1) -0.002(1) -0.004(1) 0.0012(9) N(3) 0.019(1) 0.022(1) 0.019(1) -0.0023(9) -0.002(1) 0.003(1) C1 0.023(2) 0.018(1) 0.023(1) -0.004(1) -0.005(1) -0.001(1) C2 0.016(1) 0.030(2) 0.034(2) -0.004(1) -0.002(1) 0.006(1) C3 0.022(1) 0.021(1) 0.043(2) -0.003(1) -0.005(1) 0.009(1) C4 0.026(2) 0.018(1) 0.037(2) 0.001(1) -0.005(1) -0.001(1) C5 0.022(1) 0.016(1) 0.025(1) -0.004(1) -0.008(1) -0.001(1) C6 0.027(2) 0.016(1) 0.024(1) -0.001(1) -0.003(1) 0.000(1) C7 0.026(1) 0.013(1) 0.035(2) -0.000(1) -0.004(1) 0.000(1) C8 0.027(2) 0.021(1) 0.031(2) 0.004(1) -0.006(1) -0.003(1) C9 0.022(1) 0.025(2) 0.023(2) 0.003(1) -0.002(1) -0.006(1) C10 0.021(1) 0.021(1) 0.020(1) 0.001(1) -0.003(1) -0.002(1) C11 0.018(1) 0.023(1) 0.021(1) -0.004(1) -0.005(1) 0.002(1) C12 0.016(2) 0.031(2) 0.030(2) -0.005(1) -0.003(1) 0.002(1) C13 0.015(2) 0.034(2) 0.030(2) -0.000(1) 0.003(1) -0.003(1) C14 0.026(2) 0.029(1) 0.022(1) -0.002(1) 0.003(1) -0.003(1) C15 0.021(1) 0.019(1) 0.018(1) -0.002(1) -0.001(1) 0.001(1) C16 0.029(2) 0.029(2) 0.031(2) 0.005(1) 0.004(1) -0.005(1) C17 0.026(2) 0.041(2) 0.036(2) 0.006(2) 0.004(1) 0.004(1) C18 0.036(2) 0.024(1) 0.027(1) 0.004(1) 0.012(1) 0.003(1) C19 0.032(2) 0.024(1) 0.024(2) 0.004(1) 0.008(1) 0.004(1) C20 0.041(2) 0.034(2) 0.022(1) -0.002(1) 0.004(1) 0.001(1) C21 0.052(2) 0.055(2) 0.031(2) -0.011(2) -0.008(2) 0.002(2) C22 0.068(2) 0.051(2) 0.031(2) 0.003(2) 0.020(2) 0.011(2) C23 0.042(2) 0.030(2) 0.035(2) 0.008(1) 0.000(2) 0.006(2) C24 0.025(2) 0.031(2) 0.025(1) 0.010(1) 0.002(1) 0.006(1) C25 0.027(1) 0.032(1) 0.021(1) 0.006(1) -0.001(1) 0.003(1) C26 0.030(2) 0.033(2) 0.034(2) 0.009(1) 0.008(2) -0.001(2) C27 0.032(2) 0.042(2) 0.024(2) 0.006(1) 0.003(1) 0.007(1) C28 0.050(2) 0.064(2) 0.029(2) 0.018(2) 0.010(2) 0.005(2) C29 0.044(2) 0.054(2) 0.029(2) -0.003(2) 0.002(2) 0.007(2) C30 0.031(2) 0.090(3) 0.043(2) -0.006(2) -0.004(2) 0.006(2) C31 0.061(3) 0.095(4) 0.061(3) -0.028(3) 0.010(2) 0.005(3) C32 0.103(5) 0.177(8) 0.081(4) 0.046(5) -0.019(4) -0.040(5) O30 0.055(2) 0.081(2) 0.054(2) -0.020(2) -0.008(1) 0.012(2) _refine_ls_extinction_method 'None' 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 RU . Cl(1) . 2.3794(6) yes RU . Cl(2) . 2.3322(7) yes RU . Cl(3) . 2.3504(7) yes RU . N(1) . 1.967(2) yes RU . N(2) . 2.147(2) yes RU . N(3) . 2.139(2) yes N(1) . C1 . 1.339(4) yes N(1) . C5 . 1.348(4) yes N(2) . C6 . 1.379(4) yes N(2) . C10 . 1.340(4) yes N(3) . C11 . 1.391(4) yes N(3) . C15 . 1.353(4) yes C1 . C2 . 1.398(4) yes C1 . C11 . 1.474(4) yes C2 . C3 . 1.388(4) yes C2 . H21 . 0.958(3) no C3 . C4 . 1.375(4) yes C3 . H31 . 0.957(3) no C4 . C5 . 1.383(4) yes C4 . H41 . 0.958(3) no C5 . C6 . 1.476(4) yes C6 . C7 . 1.393(4) yes C7 . C8 . 1.377(4) yes C7 . H71 . 0.961(3) no C8 . C9 . 1.382(4) yes C8 . H81 . 0.957(3) no C9 . C10 . 1.416(4) yes C9 . C16 . 1.503(4) yes C10 . C19 . 1.509(4) yes C11 . C12 . 1.364(4) yes C12 . C13 . 1.375(4) yes C12 . H121 . 0.963(3) no C13 . C14 . 1.393(4) yes C13 . H131 . 0.960(3) no C14 . C15 . 1.393(4) yes C14 . C26 . 1.500(4) yes C15 . C25 . 1.506(4) yes C16 . C17 . 1.542(5) yes C16 . C20 . 1.569(4) yes C16 . H161 . 0.963(3) no C17 . C18 . 1.532(5) yes C17 . H171 . 0.963(3) no C17 . H172 . 0.961(4) no C18 . C19 . 1.527(4) yes C18 . C20 . 1.572(4) yes C18 . H181 . 0.964(3) no C19 . H191 . 0.956(3) no C19 . H192 . 0.963(3) no C20 . C21 . 1.507(5) yes C20 . C22 . 1.534(4) yes C21 . H211 . 0.959(3) no C21 . H212 . 0.963(4) no C21 . H213 . 0.959(4) no C22 . H221 . 0.960(4) no C22 . H222 . 0.964(4) no C22 . H223 . 0.962(4) no C23 . C24 . 1.526(5) yes C23 . C26 . 1.554(5) yes C23 . H231 . 0.958(3) no C23 . H232 . 0.966(3) no C24 . C25 . 1.532(4) yes C24 . C27 . 1.561(4) yes C24 . H241 . 0.962(3) no C25 . H251 . 0.957(3) no C25 . H252 . 0.963(3) no C26 . C27 . 1.567(5) yes C26 . H261 . 0.957(3) no C27 . C28 . 1.544(4) yes C27 . C29 . 1.521(5) yes C28 . H281 . 0.957(4) no C28 . H282 . 0.960(4) no C28 . H283 . 0.961(4) no C29 . H291 . 0.960(3) no C29 . H292 . 0.961(4) no C29 . H293 . 0.957(4) no C30 . C31 . 1.511(8) yes C30 . C32 . 1.461(7) yes C30 . O30 . 1.196(5) yes C31 . H311 . 0.955(5) no C31 . H312 . 0.953(5) no C31 . H313 . 0.966(5) no C32 . H321 . 0.970(9) no C32 . H322 . 0.952(9) no C32 . H323 . 0.955(7) 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 Cl(1) . RU . Cl(2) . 93.04(2) no Cl(1) . RU . Cl(3) . 92.29(2) no Cl(2) . RU . Cl(3) . 174.66(3) no Cl(1) . RU . N(1) . 179.70(6) no Cl(2) . RU . N(1) . 86.85(6) no Cl(3) . RU . N(1) . 87.82(6) no Cl(1) . RU . N(2) . 100.78(6) no Cl(2) . RU . N(2) . 89.64(6) no Cl(3) . RU . N(2) . 89.14(6) no N(1) . RU . N(2) . 79.51(9) no Cl(1) . RU . N(3) . 100.37(6) no Cl(2) . RU . N(3) . 89.05(6) no Cl(3) . RU . N(3) . 90.21(6) no N(1) . RU . N(3) . 79.34(9) no N(2) . RU . N(3) . 158.85(8) no RU . N(1) . C1 . 118.6(2) no RU . N(1) . C5 . 119.0(2) no C1 . N(1) . C5 . 122.3(2) no RU . N(2) . C6 . 109.3(2) no RU . N(2) . C10 . 132.3(2) no C6 . N(2) . C10 . 118.3(2) no RU . N(3) . C11 . 109.9(2) no RU . N(3) . C15 . 132.9(2) no C11 . N(3) . C15 . 117.1(2) no N(1) . C1 . C2 . 120.0(2) no N(1) . C1 . C11 . 114.4(2) no C2 . C1 . C11 . 125.5(3) no C1 . C2 . C3 . 117.6(3) no C1 . C2 . H21 . 121.3(3) no C3 . C2 . H21 . 121.1(3) no C2 . C3 . C4 . 121.5(3) no C2 . C3 . H31 . 119.1(3) no C4 . C3 . H31 . 119.3(3) no C3 . C4 . C5 . 118.4(3) no C3 . C4 . H41 . 120.9(3) no C5 . C4 . H41 . 120.7(3) no N(1) . C5 . C4 . 120.1(3) no N(1) . C5 . C6 . 113.4(2) no C4 . C5 . C6 . 126.4(3) no N(2) . C6 . C5 . 116.3(2) no N(2) . C6 . C7 . 121.6(3) no C5 . C6 . C7 . 121.9(2) no C6 . C7 . C8 . 119.3(2) no C6 . C7 . H71 . 120.1(3) no C8 . C7 . H71 . 120.6(3) no C7 . C8 . C9 . 119.3(3) no C7 . C8 . H81 . 120.3(3) no C9 . C8 . H81 . 120.3(3) no C8 . C9 . C10 . 119.2(3) no C8 . C9 . C16 . 124.2(3) no C10 . C9 . C16 . 116.5(3) no N(2) . C10 . C9 . 121.5(2) no N(2) . C10 . C19 . 121.2(2) no C9 . C10 . C19 . 117.2(2) no N(3) . C11 . C1 . 115.3(2) no N(3) . C11 . C12 . 122.2(3) no C1 . C11 . C12 . 122.3(2) no C11 . C12 . C13 . 120.0(3) no C11 . C12 . H121 . 120.3(3) no C13 . C12 . H121 . 119.6(3) no C12 . C13 . C14 . 118.7(3) no C12 . C13 . H131 . 120.8(3) no C14 . C13 . H131 . 120.4(3) no C13 . C14 . C15 . 119.4(3) no C13 . C14 . C26 . 123.1(3) no C15 . C14 . C26 . 117.5(3) no N(3) . C15 . C14 . 122.0(3) no N(3) . C15 . C25 . 120.3(2) no C14 . C15 . C25 . 117.5(2) no C9 . C16 . C17 . 108.3(3) no C9 . C16 . C20 . 108.9(2) no C17 . C16 . C20 . 87.9(2) no C9 . C16 . H161 . 104.6(3) no C17 . C16 . H161 . 122.6(3) no C20 . C16 . H161 . 123.4(3) no C16 . C17 . C18 . 86.1(2) no C16 . C17 . H171 . 115.1(3) no C18 . C17 . H171 . 115.1(3) no C16 . C17 . H172 . 115.1(3) no C18 . C17 . H172 . 115.0(3) no H171 . C17 . H172 . 109.1(3) no C17 . C18 . C19 . 108.3(3) no C17 . C18 . C20 . 88.2(2) no C19 . C18 . C20 . 112.2(2) no C17 . C18 . H181 . 123.7(3) no C19 . C18 . H181 . 103.1(2) no C20 . C18 . H181 . 120.9(3) no C10 . C19 . C18 . 111.2(2) no C10 . C19 . H191 . 109.2(3) no C18 . C19 . H191 . 109.3(3) no C10 . C19 . H192 . 108.6(3) no C18 . C19 . H192 . 109.1(3) no H191 . C19 . H192 . 109.5(3) no C16 . C20 . C18 . 83.9(2) no C16 . C20 . C21 . 119.0(3) no C18 . C20 . C21 . 119.7(3) no C16 . C20 . C22 . 110.7(3) no C18 . C20 . C22 . 111.1(3) no C21 . C20 . C22 . 110.0(3) no C20 . C21 . H211 . 109.5(3) no C20 . C21 . H212 . 109.3(4) no H211 . C21 . H212 . 109.4(3) no C20 . C21 . H213 . 109.6(3) no H211 . C21 . H213 . 109.7(4) no H212 . C21 . H213 . 109.3(4) no C20 . C22 . H221 . 109.8(4) no C20 . C22 . H222 . 109.8(3) no H221 . C22 . H222 . 109.1(4) no C20 . C22 . H223 . 109.8(3) no H221 . C22 . H223 . 109.3(3) no H222 . C22 . H223 . 109.0(4) no C24 . C23 . C26 . 86.4(2) no C24 . C23 . H231 . 115.3(3) no C26 . C23 . H231 . 115.4(3) no C24 . C23 . H232 . 114.7(3) no C26 . C23 . H232 . 114.6(3) no H231 . C23 . H232 . 109.1(3) no C23 . C24 . C25 . 108.0(3) no C23 . C24 . C27 . 88.0(2) no C25 . C24 . C27 . 112.2(2) no C23 . C24 . H241 . 123.4(3) no C25 . C24 . H241 . 103.7(3) no C27 . C24 . H241 . 121.0(3) no C15 . C25 . C24 . 111.0(3) no C15 . C25 . H251 . 109.4(3) no C24 . C25 . H251 . 109.1(2) no C15 . C25 . H252 . 109.0(3) no C24 . C25 . H252 . 108.8(2) no H251 . C25 . H252 . 109.5(3) no C14 . C26 . C23 . 108.5(2) no C14 . C26 . C27 . 107.7(3) no C23 . C26 . C27 . 86.8(3) no C14 . C26 . H261 . 105.2(3) no C23 . C26 . H261 . 123.1(3) no C27 . C26 . H261 . 124.0(3) no C24 . C27 . C26 . 84.8(2) no C24 . C27 . C28 . 112.2(3) no C26 . C27 . C28 . 111.2(3) no C24 . C27 . C29 . 119.2(3) no C26 . C27 . C29 . 118.7(3) no C28 . C27 . C29 . 108.9(3) no C27 . C28 . H281 . 109.4(3) no C27 . C28 . H282 . 109.4(3) no H281 . C28 . H282 . 109.8(4) no C27 . C28 . H283 . 109.1(3) no H281 . C28 . H283 . 109.7(4) no H282 . C28 . H283 . 109.4(4) no C27 . C29 . H291 . 109.3(3) no C27 . C29 . H292 . 109.4(3) no H291 . C29 . H292 . 109.4(3) no C27 . C29 . H293 . 109.3(3) no H291 . C29 . H293 . 109.8(4) no H292 . C29 . H293 . 109.7(4) no C31 . C30 . C32 . 116.1(5) no C31 . C30 . O30 . 119.8(4) no C32 . C30 . O30 . 124.1(6) no C30 . C31 . H311 . 109.3(4) no C30 . C31 . H312 . 109.2(5) no H311 . C31 . H312 . 110.5(6) no C30 . C31 . H313 . 108.8(5) no H311 . C31 . H313 . 109.4(5) no H312 . C31 . H313 . 109.6(4) no C30 . C32 . H321 . 109.0(6) no C30 . C32 . H322 . 109.4(7) no H321 . C32 . H322 . 109.3(7) no C30 . C32 . H323 . 109.6(6) no H321 . C32 . H323 . 109.0(8) no H322 . C32 . H323 . 110.6(8) no #END #======================================================================== data_L2(-) _chemical_name_systematic ; bis('di(1R)-pineno'-[4,5:4",5"]-fused 2,2':6',2"-terpyrydine ; _cell_length_a 6.5893(9) _cell_length_b 9.0795(14) _cell_length_c 19.494(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1166.3(3) _symmetry_cell_setting 'Orthorhombic ' _symmetry_space_group_name_H-M 'P 21 2 21 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 'x+1/2,-y,-z+1/2' '-x,y,-z' '-x+1/2,-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 ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C29 H31 N3 ' _chemical_formula_moiety ' C29 H31 N3 ' _chemical_compound_source ; synthetic route ; _chemical_formula_weight 421.6 _cell_measurement_reflns_used 2000 _cell_measurement_theta_min 1.45 _cell_measurement_theta_max 24.2 _cell_measurement_temperature 293(2) _cell_formula_units_Z 2 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_max 0.80 _exptl_crystal_density_diffrn 1.201 _exptl_crystal_density_meas ? _exptl_crystal_F_000 452.06 _exptl_absorpt_coefficient_mu 0.066 _exptl_absorpt_correction_type none _exptl_special_details ; The data were collected on a Stoe Imaging Plate Diffraction System (IPDS). The crystal-to-detector distance was 80 mm. 100 exposures (6 min per exposure) were obtained with 0 < \f < 200\% and with the crystals oscillated through 2\% in \f. Coverage of the unique set was over 89% complete to at least 24.2\%. Crystal decay was monitored by measuring 200 reflexions per image. ; _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device 'Stoe IPDS' _diffrn_measurement_method '\f oscillation' _diffrn_standards_interval_time 'every image ' _diffrn_standards_interval_count 'every image ' _diffrn_standards_number '200 for each image' _diffrn_standards_decay_% negligible _diffrn_ambient_temperature 293(2) _diffrn_reflns_number 7285 _reflns_number_total 1783 _diffrn_reflns_av_R_equivalents 0.032 _reflns_number_gt 1331 _reflns_threshold-expression >2.00\s(I) _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 24.2 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _computing_data_collection 'Stoe IPDS software (Stoe, 1996)' _computing_data_reduction 'XRED (Stoe, 1.08, 1996)' _computing_cell_refinement 'Stoe IPDS software (Stoe, 1996)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _computing_structure_refinement 'CRYSTALS Issue 10 (Watkin et al, 1996)' _computing_molecular_graphics 'CAMERON (Watkin, Prout & Pearce, 1996)' _computing_publication_material 'CRYSTALS Issue 10 (Watkin et al, 1996)' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme ; Robust-resistant weighting scheme (Prince E, 1982): w=y[1-(\DF/6\s(Fo^2^)]^2^' where y=1/\SArTr(x) with 3 coefficients Ar(2.26, 0.666, 2.09) for the Chebyshev polynomial ArTr(x) where x was Fc/Fc(max). ; _atom_sites_solution_primary SIR92 _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatement 'riding model' _refine_ls_extinction_method none _refine_diff_density_min -0.19 _refine_diff_density_max 0.17 _refine_ls_number_parameters 148 _refine_ls_R_factor_obs 0.0363 _refine_ls_wR_factor_obs 0.0317 _refine_ls_goodness_of_fit_obs 1.1295 _refine_ls_shift/esd_max 0.021000 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type N1 1.0000 1.0998(2) 1.0000 0.0461 1.0000 Uani C3 1.0000 1.4036(3) 1.0000 0.0802 1.0000 Uani N2 0.5309(2) 1.1611(2) 0.91027(7) 0.0561 1.0000 Uani C1 0.8510(3) 1.1750(2) 0.96810(8) 0.0474 1.0000 Uani C2 0.8465(3) 1.3274(2) 0.9675(1) 0.0690 1.0000 Uani C4 0.6906(2) 1.0872(2) 0.93456(8) 0.0464 1.0000 Uani C5 0.3823(3) 1.0820(2) 0.88151(8) 0.0557 1.0000 Uani C6 0.3818(2) 0.9309(2) 0.87524(7) 0.0508 1.0000 Uani C7 0.5521(2) 0.8548(2) 0.89929(8) 0.0461 1.0000 Uani C8 0.7066(2) 0.9344(2) 0.92928(8) 0.0459 1.0000 Uani C9 0.5550(2) 0.6900(2) 0.89035(9) 0.0543 1.0000 Uani C10 0.3571(3) 0.6354(2) 0.85801(9) 0.0546 1.0000 Uani C11 0.1790(3) 0.7110(2) 0.8955(1) 0.0637 1.0000 Uani C12 0.2136(2) 0.8398(2) 0.8461(1) 0.0576 1.0000 Uani C13 0.3000(2) 0.7268(2) 0.79325(9) 0.0610 1.0000 Uani C14 0.4627(3) 0.7775(3) 0.74419(9) 0.0748 1.0000 Uani C15 0.1307(4) 0.6502(3) 0.7520(1) 0.0820 1.0000 Uani H21 0.7385 1.3792 0.9448 0.0803 1.0000 Uiso H31 1.0000 1.5093 1.0000 0.0855 1.0000 Uiso H51 0.2671 1.1345 0.8639 0.0662 1.0000 Uiso H81 0.8249 0.8849 0.9465 0.0547 1.0000 Uiso H91 0.5719 0.6443 0.9344 0.0649 1.0000 Uiso H92 0.6665 0.6635 0.8612 0.0649 1.0000 Uiso H101 0.3747 0.5306 0.8556 0.0654 1.0000 Uiso H111 0.2031 0.7329 0.9429 0.0736 1.0000 Uiso H112 0.0503 0.6624 0.8908 0.0736 1.0000 Uiso H121 0.1108 0.9103 0.8342 0.0653 1.0000 Uiso H141 0.4016 0.8320 0.7074 0.0858 1.0000 Uiso H142 0.5574 0.8394 0.7681 0.0858 1.0000 Uiso H143 0.5326 0.6934 0.7259 0.0858 1.0000 Uiso H151 0.0982 0.7085 0.7124 0.0972 1.0000 Uiso H152 0.0122 0.6399 0.7802 0.0972 1.0000 Uiso H153 0.1763 0.5546 0.7376 0.0972 1.0000 Uiso 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 N1 0.049(1) 0.045(1) 0.0444(9) 0.0000 0.0041(8) 0.0000 C3 0.118(3) 0.035(1) 0.088(2) 0.0000 -0.017(2) 0.0000 N2 0.0585(9) 0.0589(8) 0.0509(8) 0.0076(6) -0.0030(7) 0.0169(7) C1 0.055(1) 0.0460(9) 0.0410(8) 0.0019(7) 0.0073(8) 0.0086(7) C2 0.088(1) 0.048(1) 0.071(1) 0.0023(9) -0.009(1) 0.0097(9) C4 0.0458(9) 0.052(1) 0.0409(8) 0.0072(7) 0.0036(7) 0.0073(7) C5 0.047(1) 0.066(1) 0.0533(9) 0.0082(8) -0.0055(7) 0.0198(8) C6 0.0412(9) 0.068(1) 0.0435(8) 0.0087(7) -0.0006(7) 0.0104(7) C7 0.0425(9) 0.0537(9) 0.0421(8) 0.0046(7) 0.0031(7) 0.0093(7) C8 0.0395(8) 0.0529(9) 0.0453(7) 0.0055(6) -0.0009(7) 0.0100(7) C9 0.048(1) 0.056(1) 0.059(1) -0.0019(8) -0.0068(8) 0.0041(7) C10 0.050(1) 0.0593(9) 0.0551(9) 0.0050(8) -0.0011(8) -0.0041(7) C11 0.046(1) 0.088(1) 0.057(1) 0.0066(9) 0.0040(8) -0.0034(8) C12 0.0340(9) 0.078(1) 0.061(1) 0.0100(9) -0.0067(7) 0.0062(7) C13 0.050(1) 0.083(1) 0.0502(9) 0.0044(9) -0.0064(8) -0.0051(8) C14 0.078(1) 0.099(2) 0.047(1) 0.0012(9) 0.0082(9) -0.015(1) C15 0.078(1) 0.100(2) 0.069(1) 0.006(1) -0.021(1) -0.017(1) 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 N1 . C1 . 1.348(2) yes N1 . C1 3_757 1.348(2) yes C3 . C2 . 1.380(3) yes C3 . C2 3_757 1.380(3) yes C3 . H31 . 0.960(3) no N2 . C4 . 1.335(2) yes N2 . C5 . 1.338(2) yes C1 . C2 . 1.384(2) yes C1 . C4 . 1.477(2) yes C4 . C8 . 1.395(2) yes C5 . C6 . 1.377(3) yes C6 . C7 . 1.399(2) yes C6 . C12 . 1.494(2) yes C7 . C8 . 1.379(2) yes C7 . C9 . 1.506(2) yes C9 . C10 . 1.531(3) yes C10 . C11 . 1.543(3) yes C10 . C13 . 1.557(3) yes C11 . C12 . 1.532(3) yes C12 . C13 . 1.563(3) yes C13 . C14 . 1.509(2) yes C13 . C15 . 1.541(3) 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 C1 . N1 . C1 3_757 119.1(2) yes C2 . C3 . C2 3_757 119.8(3) yes C4 . N2 . C5 . 117.1(1) yes N1 . C1 . C2 . 121.8(2) yes N1 . C1 . C4 . 116.9(1) yes C2 . C1 . C4 . 121.3(2) yes C3 . C2 . C1 . 118.7(2) yes N2 . C4 . C1 . 116.7(1) yes N2 . C4 . C8 . 122.2(1) yes C1 . C4 . C8 . 121.0(1) yes N2 . C5 . C6 . 125.0(1) yes C5 . C6 . C7 . 117.4(1) yes C5 . C6 . C12 . 125.9(1) yes C7 . C6 . C12 . 116.7(2) yes C6 . C7 . C8 . 118.4(1) yes C6 . C7 . C9 . 117.5(1) yes C8 . C7 . C9 . 124.1(1) yes C4 . C8 . C7 . 119.8(1) yes C7 . C9 . C10 . 111.0(1) yes C9 . C10 . C11 . 108.0(1) yes C9 . C10 . C13 . 111.6(1) yes C11 . C10 . C13 . 87.9(1) yes C10 . C11 . C12 . 86.0(1) yes C6 . C12 . C11 . 107.1(1) yes C6 . C12 . C13 . 110.1(1) yes C11 . C12 . C13 . 88.1(1) yes C10 . C13 . C12 . 84.4(1) yes C10 . C13 . C14 . 120.3(1) yes C12 . C13 . C14 . 118.5(2) yes C10 . C13 . C15 . 111.0(1) yes C12 . C13 . C15 . 112.2(2) yes C14 . C13 . C15 . 108.7(1) yes #END #========================================================================= data_[Ru(terpy)(L2(-))](PF6)2 _chemical_name_systematic ; [mer-(bis('di(1R)-pineno'-[4,5:4",5"]-fused 2,2':6',2"-terpyrydine) (2,2':6',2"-terpyrydine)ruthenium(II)], bis(hexafluorophosphate) ; _cell_length_a 9.5078(14) _cell_length_b 12.745(2) _cell_length_c 37.781(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4578.2(10) _symmetry_cell_setting 'Orthorhombic ' _symmetry_space_group_name_H-M 'P 21 21 21 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 'x+1/2,-y+1/2,-z' '-x,y+1/2,-z+1/2' '-x+1/2,-y,z+1/2' 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 ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International_Tables_Vol_IV_Table_2.2B' 'Ru ' -1.4200 0.8360 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C44 H42 Ru1 P2 F12 N6 ' _chemical_formula_moiety ' C44 H42 Ru1 P2 F12 N6 ' _chemical_compound_source ; synthetic route ; _chemical_formula_weight 1045.85 _cell_measurement_reflns_used 2000 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 20.9 _cell_measurement_temperature 293(2) _cell_formula_units_Z 4 _exptl_crystal_description flat _exptl_crystal_colour red _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 2115.83 _exptl_absorpt_coefficient_mu 0.489 _exptl_absorpt_correction_type none _exptl_special_details ; The data were collected on a Stoe Imaging Plate Diffraction System (IPDS). The crystal-to-detector distance was 100 mm. 200 exposures (3 min per exposure) were obtained with 0 < \f < 200\% and with the crystals oscillated through 1\% in \f. Coverage of the unique set was over 98% complete to at least 20.9\%. Crystal decay was monitored by measuring 200 reflexions per image. ; _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f oscillation' _diffrn_standards_interval_time 'every image ' _diffrn_standards_interval_count 'every image ' _diffrn_standards_number '200 for each image' _diffrn_standards_decay_% negligible _diffrn_ambient_temperature 293(2) _diffrn_reflns_number 16335 _reflns_number_total 4800 _diffrn_reflns_av_R_equivalents 0.059 _reflns_number_gt 3516 _reflns_threshold-expression >2.00\s(I) _diffrn_reflns_theta_min 1.6 _diffrn_reflns_theta_max 20.9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 37 _computing_data_collection 'Stoe IPDS software (Stoe, 1996)' _computing_data_reduction 'XRED (Stoe, 1.08, 1996)' _computing_cell_refinement 'Stoe IPDS software (Stoe, 1996)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _computing_structure_refinement 'CRYSTALS Issue 10 (Watkin et al, 1996)' _computing_molecular_graphics 'CAMERON (Watkin, Prout & Pearce, 1996)' _computing_publication_material 'CRYSTALS Issue 10 (Watkin et al, 1996)' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme ; Robust-resistant weighting scheme (Prince E, 1982): w=y[1-(\DF/6\s(Fo^2^)]^2^' where y=1/\SArTr(x) with 3 coefficients Ar(1.57, -0.148, 0.984) for the Chebyshev polynomial ArTr(x) where x was Fc/Fc(max). ; _atom_sites_solution_primary SIR92 _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatement 'riding model' _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(5) _refine_diff_density_min -0.93 _refine_diff_density_max 0.64 _refine_ls_number_reflns 3516 _refine_ls_number_parameters 588 _refine_ls_R_factor_obs 0.0440 _refine_ls_wR_factor_obs 0.0498 _refine_ls_goodness_of_fit_obs 1.1245 _refine_ls_shift/esd_max 0.066 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type RU1 0.18390(8) 0.76841(4) 0.87552(2) 0.0399 1.0000 Uani P1 -0.1839(3) 0.4523(2) 0.77366(6) 0.0603 1.0000 Uani P2 -0.3266(4) 0.9828(2) 0.96245(7) 0.0803 1.0000 Uani F11 -0.160(2) 0.3431(7) 0.7896(3) 0.1942 1.0000 Uani F12 -0.2495(8) 0.3927(6) 0.7409(2) 0.1185 1.0000 Uani F13 -0.324(1) 0.4529(9) 0.7913(4) 0.2521 1.0000 Uani F14 -0.043(1) 0.445(1) 0.7575(4) 0.2330 1.0000 Uani F15 -0.206(2) 0.5582(6) 0.7580(3) 0.2361 1.0000 Uani F16 -0.118(1) 0.5103(7) 0.8055(2) 0.1510 1.0000 Uani F21 -0.468(1) 0.9203(8) 0.9629(2) 0.1576 1.0000 Uani F22 -0.243(2) 0.889(1) 0.9490(3) 0.2493 1.0000 Uani F23 -0.295(1) 0.9469(8) 1.0010(2) 0.1609 1.0000 Uani F24 -0.411(2) 1.0744(9) 0.9752(5) 0.2572 1.0000 Uani F25 -0.356(1) 1.020(1) 0.9252(3) 0.2232 1.0000 Uani F26 -0.180(1) 1.042(1) 0.9639(3) 0.2116 1.0000 Uani N1 0.1536(7) 0.8229(5) 0.9241(2) 0.0416 1.0000 Uani N2 0.2683(6) 0.9172(4) 0.8715(2) 0.0414 1.0000 Uani N3 0.0846(7) 0.6414(5) 0.8983(2) 0.0409 1.0000 Uani N4 0.2103(7) 0.7087(4) 0.8283(2) 0.0414 1.0000 Uani N5 0.3852(7) 0.7077(4) 0.8799(2) 0.0497 1.0000 Uani N6 -0.0011(7) 0.8120(5) 0.8514(2) 0.0434 1.0000 Uani C11 0.199(1) 0.9199(5) 0.9327(2) 0.0399 1.0000 Uani C12 0.173(1) 0.9584(6) 0.9655(2) 0.0530 1.0000 Uani C13 0.101(1) 0.8971(7) 0.9900(2) 0.0657 1.0000 Uani C14 0.052(1) 0.7976(6) 0.9807(2) 0.0534 1.0000 Uani C15 0.0772(8) 0.7628(6) 0.9473(2) 0.0388 1.0000 Uani C21 0.2672(9) 0.9721(6) 0.9027(2) 0.0427 1.0000 Uani C22 0.324(1) 1.0734(5) 0.9037(2) 0.0449 1.0000 Uani C23 0.3796(9) 1.1190(6) 0.8737(2) 0.0479 1.0000 Uani C24 0.3808(9) 1.0622(6) 0.8423(2) 0.0387 1.0000 Uani C25 0.327(1) 0.9615(6) 0.8428(2) 0.0474 1.0000 Uani C26 0.446(1) 1.1147(6) 0.8109(2) 0.0494 1.0000 Uani C27 0.5836(9) 1.1681(7) 0.8237(2) 0.0554 1.0000 Uani C28 0.4893(9) 1.2586(7) 0.8370(2) 0.0571 1.0000 Uani C29 0.4360(8) 1.2293(7) 0.8738(2) 0.0560 1.0000 Uani C30 0.383(1) 1.2282(8) 0.8074(3) 0.0618 1.0000 Uani C31 0.0355(9) 0.6594(6) 0.9323(2) 0.0411 1.0000 Uani C32 -0.045(1) 0.5880(7) 0.9497(2) 0.0479 1.0000 Uani C33 -0.076(1) 0.4941(6) 0.9338(2) 0.0484 1.0000 Uani C34 -0.0276(9) 0.4706(6) 0.9003(2) 0.0440 1.0000 Uani C35 0.0544(9) 0.5477(6) 0.8839(2) 0.0467 1.0000 Uani C36 -0.063(1) 0.3687(6) 0.8837(2) 0.0534 1.0000 Uani C37 -0.218(1) 0.3519(7) 0.8899(3) 0.0726 1.0000 Uani C38 -0.185(1) 0.3127(6) 0.9268(3) 0.0666 1.0000 Uani C39 -0.170(1) 0.4088(7) 0.9510(2) 0.0660 1.0000 Uani C40 -0.036(1) 0.2776(7) 0.9116(3) 0.0631 1.0000 Uani C41 0.1038(9) 0.7141(7) 0.8043(2) 0.0492 1.0000 Uani C42 0.114(1) 0.6650(7) 0.7715(2) 0.0594 1.0000 Uani C43 0.232(2) 0.6065(8) 0.7656(3) 0.0906 1.0000 Uani C44 0.346(1) 0.6021(7) 0.7893(3) 0.0657 1.0000 Uani C45 0.329(1) 0.6550(6) 0.8206(2) 0.0463 1.0000 Uani C51 0.4747(9) 0.7194(8) 0.9070(2) 0.0607 1.0000 Uani C52 0.611(1) 0.6860(9) 0.9055(3) 0.0840 1.0000 Uani C53 0.659(1) 0.6371(7) 0.8759(4) 0.0885 1.0000 Uani C54 0.575(1) 0.6266(8) 0.8479(3) 0.0739 1.0000 Uani C55 0.432(1) 0.6600(6) 0.8496(3) 0.0583 1.0000 Uani C61 -0.106(1) 0.8685(7) 0.8652(2) 0.0549 1.0000 Uani C62 -0.226(1) 0.8940(7) 0.8470(3) 0.0655 1.0000 Uani C63 -0.244(1) 0.8594(9) 0.8135(3) 0.0743 1.0000 Uani C64 -0.136(1) 0.8026(8) 0.7977(2) 0.0667 1.0000 Uani C65 -0.0163(9) 0.7779(7) 0.8172(2) 0.0484 1.0000 Uani C301 0.421(1) 1.2746(8) 0.7718(2) 0.0712 1.0000 Uani C302 0.227(1) 1.2421(9) 0.8135(3) 0.0790 1.0000 Uani C401 -0.046(1) 0.1689(7) 0.8951(3) 0.0689 1.0000 Uani C402 0.089(1) 0.2855(8) 0.9363(3) 0.0801 1.0000 Uani H121 0.2050 1.0272 0.9722 0.0595 1.0000 Uiso H131 0.0847 0.9241 1.0136 0.0693 1.0000 Uiso H141 0.0015 0.7552 0.9977 0.0598 1.0000 Uiso H221 0.3264 1.1114 0.9259 0.0486 1.0000 Uiso H251 0.3307 0.9216 0.8212 0.0541 1.0000 Uiso H261 0.4412 1.0625 0.7925 0.0576 1.0000 Uiso H271 0.6328 1.1307 0.8417 0.0659 1.0000 Uiso H272 0.6472 1.1863 0.8049 0.0659 1.0000 Uiso H281 0.5192 1.3305 0.8395 0.0676 1.0000 Uiso H291 0.5126 1.2340 0.8904 0.0670 1.0000 Uiso H292 0.3628 1.2769 0.8808 0.0670 1.0000 Uiso H321 -0.0815 0.6036 0.9731 0.0568 1.0000 Uiso H351 0.0904 0.5333 0.8604 0.0526 1.0000 Uiso H361 -0.0209 0.3704 0.8607 0.0640 1.0000 Uiso H371 -0.2741 0.4155 0.8897 0.0873 1.0000 Uiso H372 -0.2621 0.3010 0.8748 0.0873 1.0000 Uiso H381 -0.2423 0.2643 0.9401 0.0757 1.0000 Uiso H391 -0.1299 0.3874 0.9735 0.0766 1.0000 Uiso H392 -0.2623 0.4375 0.9555 0.0766 1.0000 Uiso H421 0.0391 0.6721 0.7540 0.0538 1.0000 Uiso H431 0.2359 0.5676 0.7434 0.0934 1.0000 Uiso H441 0.4307 0.5638 0.7834 0.0755 1.0000 Uiso H511 0.4396 0.7519 0.9285 0.0706 1.0000 Uiso H521 0.6728 0.6964 0.9258 0.0974 1.0000 Uiso H531 0.7532 0.6106 0.8745 0.1032 1.0000 Uiso H541 0.6095 0.5954 0.8256 0.0856 1.0000 Uiso H611 -0.0953 0.8935 0.8889 0.0642 1.0000 Uiso H621 -0.2971 0.9360 0.8579 0.0773 1.0000 Uiso H631 -0.3296 0.8761 0.8001 0.0852 1.0000 Uiso H641 -0.1430 0.7802 0.7734 0.0791 1.0000 Uiso H3011 0.3819 1.3448 0.7700 0.0822 1.0000 Uiso H3012 0.5218 1.2797 0.7698 0.0822 1.0000 Uiso H3013 0.3848 1.2325 0.7530 0.0822 1.0000 Uiso H3021 0.2035 1.3146 0.8107 0.0914 1.0000 Uiso H3022 0.2048 1.2203 0.8373 0.0914 1.0000 Uiso H3023 0.1758 1.2003 0.7970 0.0914 1.0000 Uiso H4011 -0.0298 0.1166 0.9130 0.0792 1.0000 Uiso H4012 -0.1389 0.1593 0.8854 0.0792 1.0000 Uiso H4013 0.0223 0.1623 0.8768 0.0792 1.0000 Uiso H4021 0.0908 0.2256 0.9517 0.0977 1.0000 Uiso H4022 0.0814 0.3483 0.9504 0.0977 1.0000 Uiso H4023 0.1739 0.2880 0.9227 0.0977 1.0000 Uiso 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 0.0528(4) 0.0315(3) 0.0354(3) 0.0006(3) 0.0010(4) -0.0029(4) P1 0.071(2) 0.050(1) 0.061(2) -0.004(1) 0.010(2) -0.001(2) P2 0.081(2) 0.093(2) 0.068(2) 0.020(2) 0.016(2) -0.002(2) F11 0.29(1) 0.103(6) 0.191(9) 0.025(6) -0.10(1) 0.014(8) F12 0.132(7) 0.117(6) 0.106(6) -0.031(5) -0.018(5) -0.001(4) F13 0.17(1) 0.21(1) 0.37(2) -0.20(1) 0.18(1) -0.108(9) F14 0.130(9) 0.25(1) 0.32(2) -0.14(1) 0.15(1) -0.077(8) F15 0.35(2) 0.072(5) 0.29(1) 0.076(7) -0.16(1) 0.009(8) F16 0.20(1) 0.150(8) 0.103(6) -0.049(5) -0.012(6) -0.066(7) F21 0.121(7) 0.21(1) 0.144(8) 0.036(7) -0.022(6) -0.083(7) F22 0.25(2) 0.30(2) 0.20(1) -0.11(1) -0.06(1) 0.17(1) F23 0.138(8) 0.26(1) 0.087(5) 0.047(6) 0.012(6) -0.064(8) F24 0.30(2) 0.15(1) 0.32(2) -0.09(1) 0.01(1) 0.09(1) F25 0.104(8) 0.44(2) 0.129(8) 0.15(1) -0.010(6) -0.002(9) F26 0.114(8) 0.27(1) 0.25(1) 0.15(1) -0.051(9) -0.089(9) N1 0.059(6) 0.037(4) 0.028(4) 0.003(3) -0.001(4) 0.002(4) N2 0.050(5) 0.035(4) 0.039(4) -0.000(4) -0.000(4) 0.002(3) N3 0.051(5) 0.045(4) 0.027(4) 0.008(3) 0.001(4) -0.002(4) N4 0.050(5) 0.034(4) 0.040(4) -0.011(3) 0.007(4) -0.009(3) N5 0.057(4) 0.033(4) 0.058(5) -0.003(4) 0.001(4) -0.002(3) N6 0.037(5) 0.043(4) 0.050(5) 0.004(4) -0.013(4) -0.002(3) C11 0.054(6) 0.031(5) 0.035(5) -0.009(4) -0.011(5) 0.014(5) C12 0.079(7) 0.035(5) 0.045(5) -0.002(4) -0.004(6) -0.002(5) C13 0.110(9) 0.044(6) 0.044(6) -0.008(5) 0.005(6) -0.009(6) C14 0.075(7) 0.050(6) 0.035(5) 0.002(4) 0.002(5) -0.016(5) C15 0.050(5) 0.042(5) 0.024(5) 0.005(4) 0.002(4) 0.005(5) C21 0.052(6) 0.039(5) 0.036(5) 0.002(4) -0.008(4) 0.008(4) C22 0.062(6) 0.027(5) 0.046(5) -0.002(4) -0.019(6) -0.002(5) C23 0.060(6) 0.036(5) 0.048(6) 0.016(5) -0.004(5) -0.006(4) C24 0.047(6) 0.031(5) 0.038(5) -0.007(4) 0.001(4) -0.002(4) C25 0.052(6) 0.044(5) 0.047(5) -0.002(4) -0.012(5) -0.011(5) C26 0.063(7) 0.038(5) 0.048(6) -0.008(4) -0.001(5) -0.011(5) C27 0.044(6) 0.068(6) 0.054(6) 0.005(5) 0.008(5) -0.009(5) C28 0.069(7) 0.045(6) 0.058(6) -0.003(5) 0.007(5) -0.009(5) C29 0.056(5) 0.052(5) 0.060(5) 0.003(6) -0.007(5) -0.002(5) C30 0.059(6) 0.053(6) 0.073(7) 0.006(6) 0.010(5) 0.005(6) C31 0.054(6) 0.035(5) 0.034(5) 0.006(4) -0.001(5) -0.006(4) C32 0.055(6) 0.051(6) 0.038(5) 0.007(5) 0.005(5) 0.003(5) C33 0.064(7) 0.032(5) 0.049(6) 0.009(4) 0.018(5) -0.005(5) C34 0.046(6) 0.029(5) 0.057(6) 0.018(4) -0.003(5) -0.010(4) C35 0.057(6) 0.033(5) 0.050(6) -0.014(4) -0.006(5) 0.008(4) C36 0.065(7) 0.042(5) 0.053(7) 0.011(4) 0.001(5) -0.002(5) C37 0.09(1) 0.052(6) 0.074(7) -0.000(5) -0.009(6) -0.013(6) C38 0.059(6) 0.050(5) 0.091(7) 0.001(5) 0.036(7) -0.015(6) C39 0.090(8) 0.059(6) 0.050(6) 0.001(5) 0.021(7) 0.007(7) C40 0.058(7) 0.043(5) 0.089(7) 0.015(6) 0.019(6) 0.001(5) C41 0.065(7) 0.043(5) 0.040(5) 0.000(4) 0.004(5) -0.015(5) C42 0.094(8) 0.063(7) 0.021(5) -0.008(5) 0.003(5) -0.022(6) C43 0.17(2) 0.057(7) 0.047(7) -0.016(6) 0.037(8) -0.010(8) C44 0.066(8) 0.068(6) 0.063(7) -0.009(6) 0.023(6) -0.011(6) C45 0.061(7) 0.043(5) 0.035(5) -0.012(4) 0.017(6) -0.013(5) C51 0.052(6) 0.077(7) 0.053(6) 0.011(6) -0.022(5) 0.017(6) C52 0.071(8) 0.082(8) 0.10(1) 0.011(7) -0.005(7) 0.008(7) C53 0.088(9) 0.065(6) 0.11(1) 0.014(8) -0.02(1) 0.035(6) C54 0.071(9) 0.060(7) 0.090(9) -0.001(6) 0.032(7) 0.012(6) C55 0.061(7) 0.035(6) 0.078(8) 0.002(5) 0.017(6) 0.001(5) C61 0.056(7) 0.062(6) 0.047(6) 0.012(5) -0.012(5) 0.015(5) C62 0.055(8) 0.053(6) 0.089(9) 0.007(6) 0.004(6) 0.016(5) C63 0.093(9) 0.082(8) 0.048(6) 0.023(6) -0.022(6) 0.013(6) C64 0.075(8) 0.079(8) 0.046(6) 0.004(5) -0.019(5) -0.013(6) C65 0.069(7) 0.051(5) 0.026(5) 0.001(4) -0.010(5) -0.015(5) C301 0.092(8) 0.056(6) 0.065(7) 0.009(6) -0.002(6) -0.020(6) C302 0.085(9) 0.080(8) 0.072(7) 0.023(6) -0.007(5) 0.001(7) C401 0.071(8) 0.044(6) 0.092(8) 0.010(5) 0.021(6) -0.012(6) C402 0.071(8) 0.064(7) 0.105(9) 0.019(6) -0.004(6) 0.010(6) 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 . 1.983(6) yes RU1 . N2 . 2.065(6) yes RU1 . N3 . 2.063(6) yes RU1 . N4 . 1.956(6) yes RU1 . N5 . 2.071(7) yes RU1 . N6 . 2.057(6) yes P1 . F11 . 1.534(8) yes P1 . F12 . 1.582(7) yes P1 . F13 . 1.49(1) yes P1 . F14 . 1.475(9) yes P1 . F15 . 1.489(7) yes P1 . F16 . 1.545(8) yes P2 . F21 . 1.562(9) yes P2 . F22 . 1.52(1) yes P2 . F23 . 1.555(8) yes P2 . F24 . 1.50(1) yes P2 . F25 . 1.509(8) yes P2 . F26 . 1.59(1) yes N1 . C11 . 1.350(9) yes N1 . C15 . 1.373(9) yes N2 . C21 . 1.37(1) yes N2 . C25 . 1.34(1) yes N3 . C31 . 1.38(1) yes N3 . C35 . 1.34(1) yes N4 . C41 . 1.36(1) yes N4 . C45 . 1.35(1) yes N5 . C51 . 1.34(1) yes N5 . C55 . 1.37(1) yes N6 . C61 . 1.34(1) yes N6 . C65 . 1.37(1) yes C11 . C12 . 1.36(1) yes C11 . C21 . 1.47(1) yes C12 . C13 . 1.39(1) yes C13 . C14 . 1.40(1) yes C14 . C15 . 1.36(1) yes C15 . C31 . 1.49(1) yes C21 . C22 . 1.40(1) yes C22 . C23 . 1.38(1) yes C23 . C24 . 1.39(1) yes C23 . C29 . 1.50(1) yes C24 . C25 . 1.38(1) yes C24 . C26 . 1.49(1) yes C26 . C27 . 1.55(1) yes C26 . C30 . 1.57(1) yes C27 . C28 . 1.54(1) yes C28 . C29 . 1.53(1) yes C28 . C30 . 1.55(1) yes C30 . C301 . 1.51(1) yes C30 . C302 . 1.51(1) yes C31 . C32 . 1.36(1) yes C32 . C33 . 1.37(1) yes C33 . C34 . 1.38(1) yes C33 . C39 . 1.55(1) yes C34 . C35 . 1.40(1) yes C34 . C36 . 1.48(1) yes C36 . C37 . 1.51(1) yes C36 . C40 . 1.59(1) yes C37 . C38 . 1.51(1) yes C38 . C39 . 1.53(1) yes C38 . C40 . 1.59(1) yes C40 . C401 . 1.52(1) yes C40 . C402 . 1.51(1) yes C41 . C42 . 1.39(1) yes C41 . C65 . 1.48(1) yes C42 . C43 . 1.36(2) yes C43 . C44 . 1.41(2) yes C44 . C45 . 1.37(1) yes C45 . C55 . 1.47(1) yes C51 . C52 . 1.36(1) yes C52 . C53 . 1.36(2) yes C53 . C54 . 1.33(2) yes C54 . C55 . 1.42(1) yes C61 . C62 . 1.37(1) yes C62 . C63 . 1.35(1) yes C63 . C64 . 1.39(1) yes C64 . C65 . 1.39(1) 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 . 78.7(3) yes N1 . RU1 . N3 . 79.7(2) yes N2 . RU1 . N3 . 158.4(3) yes N1 . RU1 . N4 . 177.5(3) yes N2 . RU1 . N4 . 103.9(3) yes N3 . RU1 . N4 . 97.7(2) yes N1 . RU1 . N5 . 101.0(3) yes N2 . RU1 . N5 . 89.4(2) yes N3 . RU1 . N5 . 95.6(2) yes N4 . RU1 . N5 . 78.9(3) yes N1 . RU1 . N6 . 101.0(3) yes N2 . RU1 . N6 . 93.0(2) yes N3 . RU1 . N6 . 90.3(3) yes N4 . RU1 . N6 . 79.1(3) yes N5 . RU1 . N6 . 157.9(3) yes F11 . P1 . F12 . 86.0(5) yes F11 . P1 . F13 . 87.9(8) yes F12 . P1 . F13 . 90.0(6) yes F11 . P1 . F14 . 88.4(8) yes F12 . P1 . F14 . 90.3(6) yes F13 . P1 . F14 . 176.3(9) yes F11 . P1 . F15 . 179.6(9) yes F12 . P1 . F15 . 93.9(5) yes F13 . P1 . F15 . 92.5(9) yes F14 . P1 . F15 . 91.2(9) yes F11 . P1 . F16 . 93.9(5) yes F12 . P1 . F16 . 179.3(5) yes F13 . P1 . F16 . 90.7(6) yes F14 . P1 . F16 . 89.0(7) yes F15 . P1 . F16 . 86.1(6) yes F21 . P2 . F22 . 92.8(8) yes F21 . P2 . F23 . 90.3(5) yes F22 . P2 . F23 . 88.9(7) yes F21 . P2 . F24 . 86.2(8) yes F22 . P2 . F24 . 178.8(9) yes F23 . P2 . F24 . 91.8(8) yes F21 . P2 . F25 . 90.5(6) yes F22 . P2 . F25 . 91.7(8) yes F23 . P2 . F25 . 179.0(7) yes F24 . P2 . F25 . 87.7(9) yes F21 . P2 . F26 . 176.5(6) yes F22 . P2 . F26 . 85.7(9) yes F23 . P2 . F26 . 86.5(5) yes F24 . P2 . F26 . 95.3(8) yes F25 . P2 . F26 . 92.7(6) yes RU1 . N1 . C11 . 119.9(5) yes RU1 . N1 . C15 . 118.3(5) yes C11 . N1 . C15 . 121.7(6) yes RU1 . N2 . C21 . 113.7(5) yes RU1 . N2 . C25 . 127.3(5) yes C21 . N2 . C25 . 118.9(6) yes RU1 . N3 . C31 . 114.3(5) yes RU1 . N3 . C35 . 128.7(5) yes C31 . N3 . C35 . 116.9(7) yes RU1 . N4 . C41 . 119.5(5) yes RU1 . N4 . C45 . 120.0(5) yes C41 . N4 . C45 . 120.3(6) yes RU1 . N5 . C51 . 127.3(6) yes RU1 . N5 . C55 . 113.8(6) yes C51 . N5 . C55 . 118.6(8) yes RU1 . N6 . C61 . 127.8(6) yes RU1 . N6 . C65 . 114.9(5) yes C61 . N6 . C65 . 117.3(7) yes N1 . C11 . C12 . 119.7(7) yes N1 . C11 . C21 . 111.7(6) yes C12 . C11 . C21 . 128.6(7) yes C11 . C12 . C13 . 119.6(7) yes C12 . C13 . C14 . 120.5(8) yes C13 . C14 . C15 . 118.2(8) yes N1 . C15 . C14 . 120.3(7) yes N1 . C15 . C31 . 113.0(6) yes C14 . C15 . C31 . 126.7(7) yes N2 . C21 . C11 . 116.0(7) yes N2 . C21 . C22 . 119.4(7) yes C11 . C21 . C22 . 124.6(7) yes C21 . C22 . C23 . 120.9(7) yes C22 . C23 . C24 . 119.1(7) yes C22 . C23 . C29 . 121.7(8) yes C24 . C23 . C29 . 119.2(8) yes C23 . C24 . C25 . 118.0(7) yes C23 . C24 . C26 . 116.5(7) yes C25 . C24 . C26 . 125.5(7) yes N2 . C25 . C24 . 123.7(7) yes C24 . C26 . C27 . 107.4(7) yes C24 . C26 . C30 . 108.8(7) yes C27 . C26 . C30 . 86.7(6) yes C26 . C27 . C28 . 86.5(6) yes C27 . C28 . C29 . 107.8(7) yes C27 . C28 . C30 . 87.6(6) yes C29 . C28 . C30 . 112.3(7) yes C23 . C29 . C28 . 110.0(8) yes C26 . C30 . C28 . 85.6(7) yes C26 . C30 . C301 . 110.2(8) yes C28 . C30 . C301 . 112.8(8) yes C26 . C30 . C302 . 117.9(9) yes C28 . C30 . C302 . 119.9(8) yes C301 . C30 . C302 . 108.8(9) yes N3 . C31 . C15 . 114.2(6) yes N3 . C31 . C32 . 121.8(7) yes C15 . C31 . C32 . 124.0(7) yes C31 . C32 . C33 . 119.6(8) yes C32 . C33 . C34 . 121.4(7) yes C32 . C33 . C39 . 123.5(8) yes C34 . C33 . C39 . 115.1(7) yes C33 . C34 . C35 . 116.0(7) yes C33 . C34 . C36 . 120.3(7) yes C35 . C34 . C36 . 123.7(8) yes N3 . C35 . C34 . 124.2(8) yes C34 . C36 . C37 . 106.3(8) yes C34 . C36 . C40 . 109.0(7) yes C37 . C36 . C40 . 87.2(6) yes C36 . C37 . C38 . 89.2(8) yes C37 . C38 . C39 . 107.8(7) yes C37 . C38 . C40 . 86.8(7) yes C39 . C38 . C40 . 110.9(9) yes C33 . C39 . C38 . 111.3(7) yes C36 . C40 . C38 . 83.7(6) yes C36 . C40 . C401 . 112.6(8) yes C38 . C40 . C401 . 110.2(8) yes C36 . C40 . C402 . 119.0(8) yes C38 . C40 . C402 . 117.2(9) yes C401 . C40 . C402 . 111.3(8) yes N4 . C41 . C42 . 121.3(8) yes N4 . C41 . C65 . 112.5(6) yes C42 . C41 . C65 . 126.2(8) yes C41 . C42 . C43 . 116.6(9) yes C42 . C43 . C44 . 123.5(9) yes C43 . C44 . C45 . 115.8(9) yes N4 . C45 . C44 . 122.3(9) yes N4 . C45 . C55 . 112.0(6) yes C44 . C45 . C55 . 125.7(9) yes N5 . C51 . C52 . 122.4(10) yes C51 . C52 . C53 . 120.0(11) yes C52 . C53 . C54 . 119.5(10) yes C53 . C54 . C55 . 120.5(10) yes N5 . C55 . C45 . 114.9(8) yes N5 . C55 . C54 . 118.9(9) yes C45 . C55 . C54 . 126.0(9) yes N6 . C61 . C62 . 123.6(8) yes C61 . C62 . C63 . 119.9(9) yes C62 . C63 . C64 . 118.4(9) yes C63 . C64 . C65 . 119.8(8) yes N6 . C65 . C41 . 113.7(7) yes N6 . C65 . C64 . 120.9(8) yes C41 . C65 . C64 . 125.4(7) yes #END