# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_General _journal_name_full CrystEngComm _journal_coden_cambridge 1350 #TrackingRef '- cif-Rh-1_hm_CCDC-878048_R2.cif' _audit_creation_date 2012-05-31 _audit_creation_method 'by CrystalStructure 4.0' _audit_update_record ? #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Hitoshi Miyasaka' _publ_contact_author_email miyasaka@se.kanazawa-u.ac.jp _publ_contact_author_fax 'ENTER FAX NUMBER' _publ_contact_author_phone 'ENTER PHONE NUMBER' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_category 'CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Hitoshi Miyasaka' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; 'Tomonori Nozaki' '' '' 'Wataru Kosaka' '' '' _publ_section_synopsis ; ENTER SYNOPSIS ; #============================================================================== # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Rigaku (2010). CrystalStructure. Version 4.0. Rigaku Corporation, Tokyo, Japan. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. SHELX97 Rigaku (1998). REQAB. Rigaku Corporation, Tokyo, Japan. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #============================================================================== data_111202_nozaki _database_code_depnum_ccdc_archive 'CCDC 878048' #TrackingRef '- cif-Rh-1_hm_CCDC-878048_R2.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C144 H96 N12 O24 Rh6' _chemical_formula_moiety 'C144 H96 N12 O24 Rh6' _chemical_formula_weight 2995.84 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/m 1' _symmetry_space_group_name_Hall '-C 2y' _symmetry_Int_Tables_number 12 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,-Z 3 -X,-Y,-Z 4 +X,-Y,+Z 5 1/2+X,1/2+Y,+Z 6 1/2-X,1/2+Y,-Z 7 1/2-X,1/2-Y,-Z 8 1/2+X,1/2-Y,+Z #------------------------------------------------------------------------------ _cell_length_a 19.5999(18) _cell_length_b 28.716(3) _cell_length_c 19.8170(18) _cell_angle_alpha 90.0000 _cell_angle_beta 112.3387(12) _cell_angle_gamma 90.0000 _cell_volume 10316.5(16) _cell_formula_units_Z 2 _cell_measurement_reflns_used 14578 _cell_measurement_theta_min 1.99 _cell_measurement_theta_max 31.04 _cell_measurement_temperature 97 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.177 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.048 _exptl_crystal_density_diffrn 0.964 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3012.00 _exptl_absorpt_coefficient_mu 0.516 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.870 _exptl_absorpt_correction_T_max 0.976 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 97 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_reflns_number 42955 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 12087 _reflns_number_gt 10039 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1731 _refine_ls_number_restraints 118 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 12087 _refine_ls_number_parameters 454 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1147P)^2^+4.7278P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.380 _refine_diff_density_min -1.560 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Rh Rh -1.1178 0.9187 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh -0.206358(12) 0.280446(7) 0.026840(13) 0.02627(10) Uani 1.0 8 d . . . Rh2 Rh 0.436620(16) 0.5000 0.458940(17) 0.02815(11) Uani 1.0 4 d . . . O1 O -0.27834(12) 0.30627(7) 0.06870(13) 0.0339(5) Uani 1.0 8 d . . . O2 O -0.36065(11) 0.24867(8) 0.01981(12) 0.0313(5) Uani 1.0 8 d . . . O3 O -0.16001(12) 0.23926(7) 0.11590(12) 0.0319(5) Uani 1.0 8 d . . . O4 O -0.24196(12) 0.18177(7) 0.06562(13) 0.0342(5) Uani 1.0 8 d . . . O5 O 0.47366(19) 0.5000 0.37523(17) 0.0414(8) Uani 1.0 4 d . . . O6 O 0.59191(18) 0.5000 0.45271(19) 0.0391(8) Uani 1.0 4 d . . . O7 O 0.43976(12) 0.42906(8) 0.46297(13) 0.0381(6) Uani 1.0 8 d . . . N1 N -0.13142(13) 0.33830(8) 0.08040(15) 0.0295(6) Uani 1.0 8 d . . . N2 N -0.04684(18) 0.5000 0.1480(2) 0.0274(8) Uani 1.0 4 d . . . N3 N 0.05983(14) 0.45869(9) 0.22098(15) 0.0302(6) Uani 1.0 8 d . . . N4 N 0.31935(19) 0.5000 0.3824(2) 0.0348(9) Uani 1.0 4 d . . . C1 C -0.33825(18) 0.28549(11) 0.05703(19) 0.0334(7) Uani 1.0 8 d . . . C2 C -0.3855(2) 0.30621(12) 0.0930(3) 0.0430(8) Uani 1.0 8 d . . . C3 C -0.3609(4) 0.34604(18) 0.1385(4) 0.087(2) Uani 1.0 8 d . . . C4 C -0.4016(4) 0.3636(3) 0.1751(5) 0.101(3) Uani 1.0 8 d . . . C5 C -0.4695(4) 0.3440(2) 0.1669(5) 0.093(3) Uani 1.0 8 d . . . C6 C -0.4924(3) 0.30364(16) 0.1265(3) 0.0555(11) Uani 1.0 8 d . . . C7 C -0.4491(3) 0.28417(14) 0.0914(3) 0.0477(10) Uani 1.0 8 d . . . C8 C -0.18637(17) 0.19908(11) 0.11613(17) 0.0313(7) Uani 1.0 8 d . . . C9 C -0.14717(19) 0.16958(12) 0.18112(19) 0.0388(8) Uani 1.0 8 d . . . C10 C -0.0978(3) 0.19008(15) 0.2441(2) 0.0561(11) Uani 1.0 8 d . . . C11 C -0.0608(4) 0.1620(2) 0.3040(3) 0.088(2) Uani 1.0 8 d . . . C12 C -0.0739(4) 0.1152(2) 0.3012(3) 0.092(3) Uani 1.0 8 d . . . C13 C -0.1213(3) 0.09420(17) 0.2382(3) 0.0666(14) Uani 1.0 8 d . . . C14 C -0.1598(2) 0.12195(13) 0.1782(2) 0.0461(9) Uani 1.0 8 d . . . C15 C -0.16040(17) 0.38097(10) 0.06097(19) 0.0345(7) Uani 1.0 8 d . . . C16 C -0.12182(17) 0.42085(11) 0.09106(18) 0.0339(7) Uani 1.0 8 d . . . C17 C -0.05164(16) 0.41735(10) 0.14372(17) 0.0276(6) Uani 1.0 8 d . . . C18 C -0.02162(16) 0.37319(10) 0.16467(18) 0.0303(7) Uani 1.0 8 d . . . C19 C -0.06410(17) 0.33451(10) 0.13177(19) 0.0329(7) Uani 1.0 8 d . . . C20 C -0.01050(15) 0.46077(10) 0.17284(16) 0.0267(6) Uani 1.0 8 d . . . C21 C 0.0922(2) 0.5000 0.2422(2) 0.0288(9) Uani 1.0 4 d . . . C22 C 0.1703(2) 0.5000 0.2927(3) 0.0348(10) Uani 1.0 4 d . . . C23 C 0.20826(19) 0.54136(11) 0.3154(2) 0.0426(9) Uani 1.0 8 d . . . C24 C 0.28244(19) 0.53969(12) 0.3593(3) 0.0452(9) Uani 1.0 8 d . . . C25 C 0.5416(3) 0.5000 0.3897(3) 0.0381(10) Uani 1.0 4 d . . . C26 C 0.5681(4) 0.5000 0.3283(3) 0.0578(14) Uani 1.0 4 d . . . C27 C 0.5255(7) 0.5161(4) 0.2606(5) 0.083(3) Uani 0.5000 8 d . . . C28 C 0.5545(8) 0.5000 0.2054(6) 0.122(3) Uani 1.0 4 d . . . C29 C 0.6182(7) 0.5000 0.2154(6) 0.110(3) Uani 1.0 4 d . . . C30 C 0.6640(9) 0.4804(5) 0.2849(8) 0.102(3) Uani 0.5000 8 d . . . C31 C 0.6381(7) 0.4825(4) 0.3415(6) 0.075(3) Uani 0.5000 8 d . . . C32 C 0.5000 0.40898(17) 0.5000 0.0362(10) Uani 1.0 4 d . . . C33 C 0.5000 0.35748(19) 0.5000 0.0545(15) Uani 1.0 4 d . . . C34 C 0.4347(3) 0.33315(16) 0.4792(4) 0.0801(17) Uani 1.0 8 d . . . C35 C 0.4352(4) 0.28433(19) 0.4805(6) 0.128(3) Uani 1.0 8 d . . . C36 C 0.5000 0.2603(3) 0.5000 0.146(5) Uani 1.0 4 d . . . C37 C 0.03490(19) 0.37194(11) 0.0249(2) 0.0377(8) Uani 1.0 8 d . . . C38 C 0.07321(18) 0.41437(11) 0.05275(19) 0.0345(7) Uani 1.0 8 d . . . C39 C 0.14680(19) 0.41518(13) 0.1039(2) 0.0401(8) Uani 1.0 8 d . . . C40 C 0.18218(18) 0.45641(12) 0.1293(2) 0.0383(8) Uani 1.0 8 d . . . C41 C 0.1472(2) 0.5000 0.1039(3) 0.0352(10) Uani 1.0 4 d . . . C42 C 0.0740(2) 0.5000 0.0523(3) 0.0299(9) Uani 1.0 4 d . . . C43 C 0.03671(16) 0.45702(11) 0.02655(18) 0.0303(7) Uani 1.0 8 d . . . H3 H -0.3157 0.3605 0.1435 0.1044 Uiso 1.0 8 calc R . . H4 H -0.3835 0.3896 0.2066 0.1217 Uiso 1.0 8 calc R . . H5 H -0.4997 0.3582 0.1890 0.1118 Uiso 1.0 8 calc R . . H6 H -0.5373 0.2892 0.1225 0.0666 Uiso 1.0 8 calc R . . H7 H -0.4636 0.2555 0.0662 0.0573 Uiso 1.0 8 calc R . . H10 H -0.0893 0.2227 0.2462 0.0673 Uiso 1.0 8 calc R . . H11 H -0.0262 0.1754 0.3472 0.1056 Uiso 1.0 8 calc R . . H12 H -0.0499 0.0968 0.3434 0.1103 Uiso 1.0 8 calc R . . H13 H -0.1274 0.0614 0.2358 0.0799 Uiso 1.0 8 calc R . . H14 H -0.1948 0.1083 0.1354 0.0554 Uiso 1.0 8 calc R . . H15 H -0.2091 0.3837 0.0253 0.0414 Uiso 1.0 8 calc R . . H16 H -0.1434 0.4506 0.0756 0.0407 Uiso 1.0 8 calc R . . H18 H 0.0267 0.3695 0.2006 0.0364 Uiso 1.0 8 calc R . . H19 H -0.0443 0.3043 0.1466 0.0395 Uiso 1.0 8 calc R . . H23 H 0.1838 0.5704 0.3011 0.0511 Uiso 1.0 8 calc R . . H24 H 0.3084 0.5682 0.3737 0.0543 Uiso 1.0 8 calc R . . H34 H 0.3891 0.3495 0.4640 0.0962 Uiso 1.0 8 calc R . . H35 H 0.3901 0.2678 0.4676 0.1540 Uiso 1.0 8 calc R . . H36 H 0.5000 0.2272 0.5000 0.1756 Uiso 1.0 4 calc R . . H37 H 0.0591 0.3431 0.0418 0.0452 Uiso 1.0 8 calc R . . H39 H 0.1721 0.3867 0.1210 0.0482 Uiso 1.0 8 calc R . . H40 H 0.2312 0.4560 0.1647 0.0459 Uiso 1.0 8 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rh1 0.02076(14) 0.01874(15) 0.03535(16) -0.00568(7) 0.00619(11) -0.00057(8) Rh2 0.01752(17) 0.0338(2) 0.02456(18) 0.0000 -0.00158(13) 0.0000 O1 0.0285(11) 0.0260(11) 0.0450(13) -0.0030(9) 0.0115(10) -0.0040(10) O2 0.0242(10) 0.0292(11) 0.0398(12) -0.0054(9) 0.0113(9) -0.0020(9) O3 0.0278(11) 0.0253(11) 0.0358(12) -0.0074(9) 0.0045(9) 0.0012(9) O4 0.0281(11) 0.0238(11) 0.0432(13) -0.0095(9) 0.0051(10) 0.0059(10) O5 0.0380(18) 0.055(3) 0.0244(15) 0.0000 0.0046(13) 0.0000 O6 0.0307(16) 0.047(2) 0.0392(18) 0.0000 0.0124(14) 0.0000 O7 0.0244(11) 0.0373(13) 0.0406(13) 0.0026(9) -0.0013(10) -0.0028(10) N1 0.0218(12) 0.0200(12) 0.0401(14) -0.0072(9) 0.0044(11) -0.0017(10) N2 0.0163(15) 0.0189(16) 0.0345(19) 0.0000 -0.0044(14) 0.0000 N3 0.0200(12) 0.0230(13) 0.0359(14) -0.0008(9) -0.0026(10) 0.0006(10) N4 0.0184(16) 0.037(2) 0.033(2) 0.0000 -0.0078(14) 0.0000 C1 0.0250(15) 0.0293(16) 0.0430(18) -0.0008(12) 0.0098(14) 0.0063(13) C2 0.0384(18) 0.0339(18) 0.060(3) 0.0001(14) 0.0225(17) -0.0038(16) C3 0.073(4) 0.059(3) 0.155(7) -0.017(3) 0.073(4) -0.032(4) C4 0.087(5) 0.079(4) 0.161(7) -0.025(4) 0.072(5) -0.056(5) C5 0.071(4) 0.078(4) 0.157(7) -0.015(3) 0.072(5) -0.047(4) C6 0.0349(19) 0.058(3) 0.075(3) -0.0029(17) 0.023(2) -0.011(3) C7 0.0348(19) 0.048(3) 0.062(3) -0.0054(15) 0.0193(18) -0.0137(18) C8 0.0314(15) 0.0247(15) 0.0359(16) -0.0029(12) 0.0108(13) 0.0019(13) C9 0.0345(17) 0.0347(18) 0.0407(18) -0.0094(14) 0.0070(14) 0.0036(14) C10 0.066(3) 0.050(3) 0.039(2) -0.021(2) 0.0049(19) 0.0084(17) C11 0.113(5) 0.072(4) 0.042(3) -0.037(4) -0.013(3) 0.017(3) C12 0.104(5) 0.076(4) 0.054(3) -0.033(4) -0.016(3) 0.037(3) C13 0.062(3) 0.053(3) 0.060(3) -0.023(2) -0.005(3) 0.025(2) C14 0.0395(19) 0.042(2) 0.044(2) -0.0143(15) 0.0014(16) 0.0134(16) C15 0.0261(15) 0.0210(15) 0.0422(18) -0.0035(11) -0.0030(13) 0.0019(13) C16 0.0260(15) 0.0217(15) 0.0440(18) -0.0033(12) 0.0019(13) 0.0017(13) C17 0.0241(14) 0.0176(13) 0.0341(15) -0.0021(11) 0.0033(12) 0.0003(11) C18 0.0197(13) 0.0221(14) 0.0396(17) -0.0013(11) 0.0005(12) 0.0029(12) C19 0.0283(15) 0.0179(14) 0.0461(18) -0.0019(11) 0.0069(13) 0.0044(13) C20 0.0184(13) 0.0199(14) 0.0328(15) -0.0013(10) -0.0003(11) 0.0028(11) C21 0.0219(19) 0.022(2) 0.030(2) 0.0000 -0.0038(16) 0.0000 C22 0.0197(19) 0.031(3) 0.042(3) 0.0000 -0.0016(18) 0.0000 C23 0.0271(16) 0.0255(17) 0.054(3) 0.0017(12) -0.0080(15) -0.0034(15) C24 0.0247(16) 0.0337(19) 0.056(3) 0.0000(13) -0.0087(15) -0.0028(16) C25 0.040(3) 0.043(3) 0.031(2) 0.0000 0.0136(18) 0.0000 C26 0.073(4) 0.057(4) 0.049(3) 0.0000 0.031(3) 0.0000 C27 0.098(6) 0.112(7) 0.041(4) -0.003(5) 0.030(4) -0.002(4) C28 0.120(6) 0.183(8) 0.071(5) 0.0000 0.044(5) 0.0000 C29 0.113(6) 0.153(7) 0.082(5) 0.0000 0.059(5) 0.0000 C30 0.102(6) 0.135(8) 0.085(5) 0.006(5) 0.054(5) -0.014(5) C31 0.074(5) 0.091(6) 0.074(5) 0.004(4) 0.045(4) -0.013(4) C32 0.0214(19) 0.036(3) 0.043(3) 0.0000 0.0024(17) 0.0000 C33 0.035(3) 0.033(3) 0.074(4) 0.0000 -0.005(3) 0.0000 C34 0.046(3) 0.041(3) 0.123(4) -0.0091(18) -0.002(3) 0.008(3) C35 0.069(4) 0.045(3) 0.212(7) -0.014(3) -0.013(5) 0.013(4) C36 0.082(6) 0.037(4) 0.252(10) 0.0000 -0.013(7) 0.0000 C37 0.0393(18) 0.0246(16) 0.049(2) 0.0023(13) 0.0171(16) 0.0029(14) C38 0.0287(15) 0.0305(16) 0.0445(18) 0.0050(12) 0.0142(14) 0.0049(14) C39 0.0300(16) 0.0381(18) 0.048(2) 0.0095(14) 0.0104(15) 0.0066(15) C40 0.0240(15) 0.0408(19) 0.0441(19) 0.0051(13) 0.0062(14) 0.0040(15) C41 0.025(2) 0.036(3) 0.041(3) 0.0000 0.0077(19) 0.0000 C42 0.0204(18) 0.028(3) 0.041(3) 0.0000 0.0118(17) 0.0000 C43 0.0256(15) 0.0266(15) 0.0401(17) -0.0009(11) 0.0139(14) -0.0006(13) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Rh1 Rh1 2.3942(4) yes . 7_455 Rh1 O1 2.029(3) yes . . Rh1 O2 2.050(3) yes . 7_455 Rh1 O3 2.030(2) yes . . Rh1 O4 2.037(3) yes . 7_455 Rh1 N1 2.204(3) yes . . Rh2 Rh2 2.3974(5) yes . 2_656 Rh2 O5 2.048(4) yes . . Rh2 O6 2.030(5) yes . 2_656 Rh2 O7 2.039(3) yes . . Rh2 O7 2.039(3) yes . 4_565 Rh2 N4 2.221(4) yes . . O1 C1 1.258(5) yes . . O2 C1 1.268(4) yes . . O3 C8 1.265(4) yes . . O4 C8 1.268(4) yes . . O5 C25 1.251(7) yes . . O6 C25 1.263(6) yes . . O7 C32 1.267(3) yes . . N1 C15 1.344(4) yes . . N1 C19 1.330(4) yes . . N2 C20 1.324(4) yes . . N2 C20 1.324(4) yes . 4_565 N3 C20 1.347(4) yes . . N3 C21 1.336(3) yes . . N4 C24 1.334(4) yes . . N4 C24 1.334(4) yes . 4_565 C1 C2 1.491(7) yes . . C2 C3 1.422(7) yes . . C2 C7 1.388(6) yes . . C3 C4 1.362(13) yes . . C4 C5 1.398(11) yes . . C5 C6 1.383(8) yes . . C6 C7 1.401(8) yes . . C8 C9 1.488(5) yes . . C9 C10 1.387(5) yes . . C9 C14 1.387(5) yes . . C10 C11 1.390(7) yes . . C11 C12 1.363(9) yes . . C12 C13 1.379(7) yes . . C13 C14 1.391(6) yes . . C15 C16 1.377(5) yes . . C16 C17 1.378(4) yes . . C17 C18 1.393(4) yes . . C17 C20 1.478(4) yes . . C18 C19 1.393(4) yes . . C21 C22 1.477(5) yes . . C22 C23 1.383(4) yes . . C22 C23 1.383(4) yes . 4_565 C23 C24 1.383(5) yes . . C25 C26 1.494(11) yes . . C26 C27 1.364(11) yes . . C26 C27 1.364(11) yes . 4_565 C26 C31 1.389(14) yes . . C26 C31 1.389(14) yes . 4_565 C27 C27 0.922(17) yes . 4_565 C27 C28 1.48(2) yes . . C28 C29 1.19(2) yes . . C29 C30 1.442(16) yes . . C29 C30 1.442(16) yes . 4_565 C30 C30 1.13(2) yes . 4_565 C30 C31 1.40(3) yes . . C30 C31 1.76(2) yes . 4_565 C31 C31 1.007(15) yes . 4_565 C32 C33 1.479(8) yes . . C33 C34 1.377(6) yes . . C33 C34 1.377(6) yes . 2_656 C34 C35 1.402(8) yes . . C35 C36 1.365(9) yes . . C37 C37 1.349(5) yes . 2_555 C37 C38 1.428(5) yes . . C38 C39 1.413(5) yes . . C38 C43 1.414(5) yes . . C39 C40 1.368(5) yes . . C40 C41 1.424(4) yes . . C41 C42 1.410(5) yes . . C42 C43 1.426(4) yes . . C42 C43 1.426(4) yes . 4_565 C43 C43 1.424(4) yes . 2_555 C3 H3 0.950 no . . C4 H4 0.950 no . . C5 H5 0.950 no . . C6 H6 0.950 no . . C7 H7 0.950 no . . C10 H10 0.950 no . . C11 H11 0.950 no . . C12 H12 0.950 no . . C13 H13 0.950 no . . C14 H14 0.950 no . . C15 H15 0.950 no . . C16 H16 0.950 no . . C18 H18 0.950 no . . C19 H19 0.950 no . . C23 H23 0.950 no . . C24 H24 0.950 no . . C34 H34 0.950 no . . C35 H35 0.950 no . . C36 H36 0.950 no . . C37 H37 0.950 no . . C39 H39 0.950 no . . C40 H40 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Rh1 Rh1 O1 87.60(6) yes 7_455 . . Rh1 Rh1 O2 88.50(6) yes 7_455 . 7_455 Rh1 Rh1 O3 88.22(6) yes 7_455 . . Rh1 Rh1 O4 87.84(6) yes 7_455 . 7_455 Rh1 Rh1 N1 175.70(9) yes 7_455 . . O1 Rh1 O2 176.03(8) yes . . 7_455 O1 Rh1 O3 90.48(10) yes . . . O1 Rh1 O4 89.30(10) yes . . 7_455 O1 Rh1 N1 88.13(10) yes . . . O2 Rh1 O3 90.16(10) yes 7_455 . . O2 Rh1 O4 89.79(10) yes 7_455 . 7_455 O2 Rh1 N1 95.78(10) yes 7_455 . . O3 Rh1 O4 176.05(8) yes . . 7_455 O3 Rh1 N1 91.40(9) yes . . . O4 Rh1 N1 92.53(9) yes 7_455 . . Rh2 Rh2 O5 87.41(9) yes 2_656 . . Rh2 Rh2 O6 88.20(9) yes 2_656 . 2_656 Rh2 Rh2 O7 88.01(6) yes 2_656 . . Rh2 Rh2 O7 88.01(6) yes 2_656 . 4_565 Rh2 Rh2 N4 179.72(12) yes 2_656 . . O5 Rh2 O6 175.62(12) yes . . 2_656 O5 Rh2 O7 90.97(9) yes . . . O5 Rh2 O7 90.97(9) yes . . 4_565 O5 Rh2 N4 92.31(15) yes . . . O6 Rh2 O7 88.87(9) yes 2_656 . . O6 Rh2 O7 88.87(9) yes 2_656 . 4_565 O6 Rh2 N4 92.07(15) yes 2_656 . . O7 Rh2 O7 175.49(9) yes . . 4_565 O7 Rh2 N4 91.99(6) yes . . . O7 Rh2 N4 91.99(6) yes 4_565 . . Rh1 O1 C1 119.8(3) yes . . . Rh1 O2 C1 117.6(3) yes 7_455 . . Rh1 O3 C8 119.09(18) yes . . . Rh1 O4 C8 119.1(2) yes 7_455 . . Rh2 O5 C25 119.2(4) yes . . . Rh2 O6 C25 119.0(4) yes 2_656 . . Rh2 O7 C32 119.0(3) yes . . . Rh1 N1 C15 114.68(18) yes . . . Rh1 N1 C19 126.35(19) yes . . . C15 N1 C19 118.8(3) yes . . . C20 N2 C20 116.7(3) yes . . 4_565 C20 N3 C21 114.8(3) yes . . . Rh2 N4 C24 121.31(18) yes . . . Rh2 N4 C24 121.31(18) yes . . 4_565 C24 N4 C24 117.3(3) yes . . 4_565 O1 C1 O2 126.5(4) yes . . . O1 C1 C2 115.4(3) yes . . . O2 C1 C2 118.0(4) yes . . . C1 C2 C3 120.1(5) yes . . . C1 C2 C7 121.6(4) yes . . . C3 C2 C7 117.8(5) yes . . . C2 C3 C4 120.7(6) yes . . . C3 C4 C5 120.9(7) yes . . . C4 C5 C6 119.3(7) yes . . . C5 C6 C7 119.9(5) yes . . . C2 C7 C6 121.0(4) yes . . . O3 C8 O4 125.8(3) yes . . . O3 C8 C9 116.4(3) yes . . . O4 C8 C9 117.8(3) yes . . . C8 C9 C10 119.4(4) yes . . . C8 C9 C14 120.0(3) yes . . . C10 C9 C14 120.6(4) yes . . . C9 C10 C11 118.7(4) yes . . . C10 C11 C12 120.5(5) yes . . . C11 C12 C13 121.3(5) yes . . . C12 C13 C14 118.8(5) yes . . . C9 C14 C13 119.9(4) yes . . . N1 C15 C16 122.1(3) yes . . . C15 C16 C17 119.5(3) yes . . . C16 C17 C18 118.6(3) yes . . . C16 C17 C20 118.3(3) yes . . . C18 C17 C20 123.1(3) yes . . . C17 C18 C19 118.5(3) yes . . . N1 C19 C18 122.4(3) yes . . . N2 C20 N3 124.2(3) yes . . . N2 C20 C17 115.9(3) yes . . . N3 C20 C17 119.9(3) yes . . . N3 C21 N3 125.3(3) yes . . 4_565 N3 C21 C22 117.35(16) yes . . . N3 C21 C22 117.35(16) yes 4_565 . . C21 C22 C23 120.76(18) yes . . . C21 C22 C23 120.76(18) yes . . 4_565 C23 C22 C23 118.4(3) yes . . 4_565 C22 C23 C24 118.8(3) yes . . . N4 C24 C23 123.3(3) yes . . . O5 C25 O6 126.1(6) yes . . . O5 C25 C26 118.9(5) yes . . . O6 C25 C26 115.0(6) yes . . . C25 C26 C27 122.0(9) yes . . . C25 C26 C27 122.0(9) yes . . 4_565 C25 C26 C31 118.1(7) yes . . . C25 C26 C31 118.1(7) yes . . 4_565 C27 C26 C27 39.5(7) yes . . 4_565 C27 C26 C31 120.0(10) yes . . . C27 C26 C31 104.7(9) yes . . 4_565 C27 C26 C31 104.7(9) yes 4_565 . . C27 C26 C31 120.0(10) yes 4_565 . 4_565 C31 C26 C31 42.5(7) yes . . 4_565 C26 C27 C27 70.2(9) yes . . 4_565 C26 C27 C28 110.9(10) yes . . . C27 C27 C28 71.9(12) yes 4_565 . . C27 C28 C27 36.2(8) yes . . 4_565 C27 C28 C29 123.4(10) yes . . . C27 C28 C29 123.4(10) yes 4_565 . . C28 C29 C30 113.1(14) yes . . . C28 C29 C30 113.1(14) yes . . 4_565 C30 C29 C30 45.9(9) yes . . 4_565 C29 C30 C30 67.0(10) yes . . 4_565 C29 C30 C31 117.7(14) yes . . . C29 C30 C31 98.4(10) yes . . 4_565 C30 C30 C31 87.6(15) yes 4_565 . . C30 C30 C31 52.6(12) yes 4_565 . 4_565 C31 C30 C31 34.9(7) yes . . 4_565 C26 C31 C30 119.9(10) yes . . . C26 C31 C30 99.5(8) yes . . 4_565 C26 C31 C31 68.8(10) yes . . 4_565 C30 C31 C30 39.8(9) yes . . 4_565 C30 C31 C31 92.4(14) yes . . 4_565 C30 C31 C31 52.6(11) yes 4_565 . 4_565 O7 C32 O7 125.9(5) yes . . 2_656 O7 C32 C33 117.1(3) yes . . . O7 C32 C33 117.1(3) yes 2_656 . . C32 C33 C34 120.5(3) yes . . . C32 C33 C34 120.5(3) yes . . 2_656 C34 C33 C34 119.0(5) yes . . 2_656 C33 C34 C35 120.1(5) yes . . . C34 C35 C36 120.7(7) yes . . . C35 C36 C35 119.3(8) yes . . 2_656 C37 C37 C38 121.4(3) yes 2_555 . . C37 C38 C39 122.3(3) yes . . . C37 C38 C43 118.6(3) yes . . . C39 C38 C43 119.0(3) yes . . . C38 C39 C40 121.0(4) yes . . . C39 C40 C41 121.5(3) yes . . . C40 C41 C40 123.0(3) yes . . 4_565 C40 C41 C42 118.47(18) yes . . . C40 C41 C42 118.47(18) yes 4_565 . . C41 C42 C43 120.08(17) yes . . . C41 C42 C43 120.08(17) yes . . 4_565 C43 C42 C43 119.8(3) yes . . 4_565 C38 C43 C42 119.9(3) yes . . . C38 C43 C43 120.0(3) yes . . 2_555 C42 C43 C43 120.1(3) yes . . 2_555 C2 C3 H3 119.675 no . . . C4 C3 H3 119.663 no . . . C3 C4 H4 119.561 no . . . C5 C4 H4 119.581 no . . . C4 C5 H5 120.334 no . . . C6 C5 H5 120.321 no . . . C5 C6 H6 120.073 no . . . C7 C6 H6 120.064 no . . . C2 C7 H7 119.508 no . . . C6 C7 H7 119.516 no . . . C9 C10 H10 120.637 no . . . C11 C10 H10 120.626 no . . . C10 C11 H11 119.724 no . . . C12 C11 H11 119.736 no . . . C11 C12 H12 119.346 no . . . C13 C12 H12 119.360 no . . . C12 C13 H13 120.596 no . . . C14 C13 H13 120.583 no . . . C9 C14 H14 120.052 no . . . C13 C14 H14 120.031 no . . . N1 C15 H15 118.951 no . . . C16 C15 H15 118.943 no . . . C15 C16 H16 120.236 no . . . C17 C16 H16 120.229 no . . . C17 C18 H18 120.755 no . . . C19 C18 H18 120.767 no . . . N1 C19 H19 118.795 no . . . C18 C19 H19 118.802 no . . . C22 C23 H23 120.577 no . . . C24 C23 H23 120.609 no . . . N4 C24 H24 118.359 no . . . C23 C24 H24 118.349 no . . . C33 C34 H34 119.933 no . . . C35 C34 H34 119.935 no . . . C34 C35 H35 119.651 no . . . C36 C35 H35 119.655 no . . . C35 C36 H36 120.359 no . . . C35 C36 H36 120.359 no 2_656 . . C37 C37 H37 119.300 no 2_555 . . C38 C37 H37 119.297 no . . . C38 C39 H39 119.519 no . . . C40 C39 H39 119.514 no . . . C39 C40 H40 119.252 no . . . C41 C40 H40 119.255 no . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O1 C3 2.746(9) no . . O1 C7 3.600(6) no . . O1 C8 3.510(4) no . . O1 C8 3.463(5) no . 7_455 O1 C15 3.200(4) no . . O2 C7 2.817(6) no . . O2 C8 3.519(4) no . . O2 C8 3.499(5) no . 7_455 O3 C1 3.497(4) no . . O3 C1 3.487(5) no . 7_455 O3 C10 2.753(5) no . . O3 C14 3.588(5) no . . O3 C19 3.266(4) no . . O4 C1 3.495(4) no . . O4 C1 3.488(5) no . 7_455 O4 C10 3.599(4) no . . O4 C14 2.791(4) no . . O4 C15 3.091(4) no . 7_455 O5 C27 2.857(14) no . . O5 C27 2.857(14) no . 4_565 O5 C31 3.567(14) no . . O5 C31 3.567(14) no . 4_565 O5 C32 3.499(5) no . . O6 C27 3.555(10) no . . O6 C27 3.555(10) no . 4_565 O6 C31 2.728(15) no . . O6 C31 2.728(15) no . 4_565 O6 C32 3.498(5) no . . O7 C24 3.117(4) no . 4_565 O7 C25 3.528(7) no . . O7 C25 3.464(6) no . 2_656 O7 C34 2.779(6) no . . O7 C34 3.579(6) no . 2_656 N1 C17 2.771(4) no . . N2 N3 2.360(4) no . 4_565 N2 C16 2.709(4) no . . N2 C16 2.709(4) no . 4_565 N2 C17 2.375(3) no . 4_565 N2 C21 2.654(5) no . . N3 C18 2.910(4) no . . N3 C20 2.676(4) no . 4_565 N3 C23 2.798(4) no . 4_565 N4 C22 2.783(5) no . . N4 C23 2.391(5) no . 4_565 C2 C5 2.805(10) no . . C3 C6 2.777(8) no . . C4 C7 2.766(8) no . . C9 C12 2.749(6) no . . C10 C13 2.787(7) no . . C11 C14 2.760(6) no . . C15 C18 2.724(4) no . . C16 C19 2.717(5) no . . C17 C20 3.589(4) no . 4_565 C22 C24 2.380(5) no . 4_565 C23 C24 2.707(5) no . 4_565 C26 C29 2.764(17) no . . C27 C30 2.77(2) no . . C27 C30 2.57(3) no . 4_565 C28 C31 2.618(15) no . . C28 C31 2.618(15) no . 4_565 C33 C35 2.408(8) no . 2_656 C33 C36 2.791(11) no . . C34 C35 2.749(9) no . 2_656 C37 C43 2.809(5) no . 2_555 C38 C38 2.837(5) no . 2_555 C38 C41 2.839(4) no . . C39 C42 2.812(4) no . . C40 C43 2.804(4) no . . C42 C42 2.853(5) no . 2_555 Rh2 O7 3.093(3) no . 3_666 Rh2 C32 2.875(5) no . 3_666 O2 C6 3.584(5) no . 2_455 O3 C6 3.440(6) no . 8_555 O5 C12 3.596(6) no . 5_555 O5 C12 3.596(6) no . 8_555 O5 C32 3.499(5) no . 3_666 O6 O7 2.849(4) no . 3_666 O6 C32 3.498(5) no . 3_666 O7 C12 3.364(7) no . 8_555 N1 C37 3.445(6) no . 2_555 N2 C42 3.553(8) no . . N3 C39 3.585(6) no . . N3 C40 3.517(6) no . . N3 C41 3.570(7) no . . C5 C10 3.540(10) no . 8_455 C6 O2 3.584(5) no . 2_455 C6 O3 3.440(6) no . 8_455 C7 C7 3.408(6) no . 2_455 C10 C5 3.540(10) no . 8_555 C11 C34 3.510(10) no . 8_455 C12 O5 3.596(6) no . 5_445 C12 O7 3.364(7) no . 8_455 C13 C27 3.541(14) no . 5_445 C15 C37 3.492(6) no . 2_555 C15 C38 3.442(6) no . 2_555 C15 C39 3.518(6) no . 2_555 C16 C38 3.336(6) no . 2_555 C16 C43 3.500(6) no . 2_555 C17 C38 3.549(6) no . . C17 C43 3.570(6) no . . C18 C37 3.352(6) no . . C18 C38 3.592(6) no . . C19 C37 3.540(6) no . . C19 C37 3.532(6) no . 2_555 C20 C42 3.567(7) no . . C20 C43 3.363(6) no . . C21 C40 3.561(7) no . . C21 C40 3.561(7) no . 4_565 C21 C41 3.304(8) no . . C22 C40 3.561(8) no . . C22 C40 3.561(8) no . 4_565 C22 C41 3.594(9) no . . C23 C40 3.526(6) no . 4_565 C25 O7 3.464(6) no . 3_666 C27 C13 3.541(14) no . 5_555 C34 C11 3.510(10) no . 8_555 C37 N1 3.445(6) no . 2_555 C37 C15 3.492(6) no . 2_555 C37 C18 3.352(6) no . . C37 C19 3.540(6) no . . C37 C19 3.532(6) no . 2_555 C38 C15 3.442(6) no . 2_555 C38 C16 3.336(6) no . 2_555 C38 C17 3.549(6) no . . C38 C18 3.592(6) no . . C39 N3 3.585(6) no . . C39 C15 3.518(6) no . 2_555 C40 N3 3.517(6) no . . C40 C21 3.561(7) no . . C40 C22 3.561(8) no . . C40 C23 3.526(6) no . 4_565 C41 N3 3.570(7) no . . C41 N3 3.570(7) no . 4_565 C41 C21 3.304(8) no . . C41 C22 3.594(9) no . . C42 N2 3.553(8) no . . C42 C20 3.567(7) no . . C42 C20 3.567(7) no . 4_565 C42 C43 2.469(5) no . 3_565 C43 C16 3.500(6) no . 2_555 C43 C17 3.570(6) no . . C43 C20 3.363(6) no . . C43 C43 2.850(5) no . 3_565 Rh1 H15 2.9657 no . . Rh1 H19 3.2346 no . . Rh2 H24 3.1271 no . . Rh2 H24 3.1270 no . 4_565 O1 H3 2.4458 no . . O1 H15 2.9008 no . . O2 H7 2.5220 no . . O2 H19 3.4624 no . 7_455 O3 H10 2.4689 no . . O3 H19 2.8209 no . . O4 H14 2.4992 no . . O4 H15 2.5279 no . 7_455 O7 H24 2.5097 no . 4_565 O7 H34 2.4945 no . . N1 H16 3.2312 no . . N1 H18 3.2363 no . . N2 H16 2.3645 no . . N2 H16 2.3645 no . 4_565 N3 H18 2.6338 no . . N3 H23 2.4876 no . 4_565 N4 H23 3.2387 no . . N4 H23 3.2387 no . 4_565 N4 H24 1.9716 no . 4_565 C1 H3 2.6824 no . . C1 H7 2.6736 no . . C2 H4 3.2761 no . . C2 H6 3.2801 no . . C3 H5 3.2532 no . . C3 H7 3.2675 no . . C4 H6 3.2610 no . . C5 H3 3.2556 no . . C5 H7 3.2617 no . . C6 H4 3.2544 no . . C7 H3 3.2651 no . . C7 H5 3.2696 no . . C8 H10 2.6455 no . . C8 H14 2.6491 no . . C9 H11 3.2483 no . . C9 H13 3.2658 no . . C10 H12 3.2441 no . . C10 H14 3.2650 no . . C11 H13 3.2458 no . . C12 H10 3.2484 no . . C12 H14 3.2452 no . . C13 H11 3.2433 no . . C14 H10 3.2687 no . . C14 H12 3.2426 no . . C15 H19 3.1575 no . . C16 H18 3.2487 no . . C17 H15 3.2334 no . . C17 H19 3.2488 no . . C18 H16 3.2477 no . . C19 H15 3.1563 no . . C20 H16 2.6017 no . . C20 H18 2.7187 no . . C21 H23 2.6605 no . . C21 H23 2.6605 no . 4_565 C22 H23 2.0374 no . 4_565 C22 H24 3.2317 no . . C22 H24 3.2317 no . 4_565 C23 H23 3.2414 no . 4_565 C24 H24 3.1363 no . 4_565 C32 H34 2.6403 no . . C32 H34 2.6403 no . 2_656 C33 H34 2.0260 no . 2_656 C33 H35 3.2612 no . . C33 H35 3.2612 no . 2_656 C34 H34 3.2337 no . 2_656 C34 H36 3.2656 no . . C35 H35 3.2142 no . 2_656 C36 H34 3.2573 no . . C36 H34 3.2573 no . 2_656 C36 H35 2.0124 no . 2_656 C37 H39 2.6721 no . . C38 H37 3.2758 no . 2_555 C38 H40 3.2731 no . . C39 H37 2.6736 no . . C40 H40 2.6897 no . 4_565 C41 H39 3.2890 no . . C41 H39 3.2890 no . 4_565 C41 H40 2.0622 no . 4_565 C42 H40 3.2917 no . . C42 H40 3.2917 no . 4_565 C43 H37 3.2994 no . . C43 H39 3.2934 no . . H3 H4 2.3008 no . . H4 H5 2.3484 no . . H5 H6 2.3389 no . . H6 H7 2.3453 no . . H10 H11 2.3447 no . . H10 H19 3.3901 no . . H11 H12 2.3005 no . . H12 H13 2.3294 no . . H13 H14 2.3508 no . . H14 H15 3.0304 no . 7_455 H15 H16 2.3152 no . . H16 H16 2.8388 no . 4_565 H18 H19 2.3365 no . . H18 H23 3.4286 no . 4_565 H23 H24 2.3177 no . . H24 H34 3.0224 no . 4_565 H34 H35 2.3464 no . . H35 H36 2.3158 no . . H37 H37 2.2787 no . 2_555 H37 H39 2.5079 no . . H39 H40 2.2998 no . . H40 H40 2.5293 no . 4_565 O2 H6 3.0029 no . 2_455 O2 H7 3.2170 no . 2_455 O2 H37 3.1825 no . 8_455 O3 H6 2.4947 no . 8_555 O4 H39 3.0517 no . 8_455 O5 H12 2.8492 no . 5_555 O5 H12 2.8492 no . 8_555 O5 H13 3.2402 no . 5_555 O5 H13 3.2402 no . 8_555 O7 H12 2.5635 no . 8_555 N1 H37 3.2406 no . 2_555 C1 H6 3.4673 no . 2_455 C6 H19 3.3329 no . 8_455 C7 H7 3.0498 no . 2_455 C7 H19 3.5599 no . 8_455 C8 H6 2.8950 no . 8_555 C9 H5 2.9453 no . 8_555 C9 H6 3.0475 no . 8_555 C10 H5 2.8989 no . 8_555 C10 H6 3.1189 no . 8_555 C11 H5 3.0066 no . 8_555 C12 H5 3.1780 no . 8_555 C12 H24 3.4246 no . 5_445 C13 H5 3.2041 no . 8_555 C13 H24 3.5326 no . 5_445 C13 H40 3.0591 no . 8_455 C14 H5 3.1172 no . 8_555 C14 H39 3.0600 no . 8_455 C14 H40 3.0334 no . 8_455 C15 H37 3.5138 no . 2_555 C15 H39 3.5292 no . 2_555 C18 H37 3.4796 no . . C19 H37 3.5133 no . . C19 H37 3.4867 no . 2_555 C22 H40 3.4300 no . . C22 H40 3.4300 no . 4_565 C23 H40 3.1859 no . 4_565 C24 H13 3.5754 no . 5_555 C24 H40 3.5996 no . 4_565 C25 H12 3.2461 no . 5_555 C25 H12 3.2461 no . 8_555 C27 H12 3.4788 no . 5_555 C27 H13 3.1298 no . 5_555 C28 H4 3.3913 no . 1_655 C28 H4 3.3913 no . 4_665 C29 H4 3.1740 no . 1_655 C29 H4 3.1740 no . 4_665 C30 H4 2.9957 no . 1_655 C32 H12 2.8823 no . 7_556 C32 H12 2.8823 no . 8_555 C33 H11 3.0237 no . 7_556 C33 H11 3.0237 no . 8_555 C33 H12 3.1627 no . 7_556 C33 H12 3.1627 no . 8_555 C34 H11 3.2279 no . 7_556 C34 H11 3.0030 no . 8_555 C34 H12 3.4638 no . 8_555 C35 H11 3.3983 no . 7_556 C35 H11 3.2245 no . 8_555 C36 H11 3.4141 no . 7_556 C36 H11 3.4141 no . 8_555 C37 H18 3.5461 no . . C38 H16 3.4798 no . 2_555 C39 H14 3.0016 no . 8_555 C39 H15 3.3533 no . 2_555 C40 H13 3.5577 no . 8_555 C40 H14 3.0097 no . 8_555 C40 H23 3.4784 no . 4_565 C42 H16 3.5940 no . 2_555 C42 H16 3.5940 no . 3_565 C43 H16 3.4248 no . 2_555 H4 C28 3.3913 no . 1_455 H4 C29 3.1740 no . 1_455 H4 C30 2.9957 no . 1_455 H5 C9 2.9453 no . 8_455 H5 C10 2.8989 no . 8_455 H5 C11 3.0066 no . 8_455 H5 C12 3.1780 no . 8_455 H5 C13 3.2041 no . 8_455 H5 C14 3.1172 no . 8_455 H5 H10 3.3593 no . 8_455 H5 H11 3.5034 no . 8_455 H6 O2 3.0029 no . 2_455 H6 O3 2.4947 no . 8_455 H6 C1 3.4673 no . 2_455 H6 C8 2.8950 no . 8_455 H6 C9 3.0475 no . 8_455 H6 C10 3.1189 no . 8_455 H6 H10 3.0099 no . 8_455 H6 H19 2.7381 no . 8_455 H7 O2 3.2170 no . 2_455 H7 C7 3.0498 no . 2_455 H7 H7 2.4641 no . 2_455 H7 H19 3.1465 no . 8_455 H7 H37 2.9330 no . 8_455 H10 H5 3.3593 no . 8_555 H10 H6 3.0099 no . 8_555 H11 C33 3.0237 no . 7_556 H11 C34 3.2279 no . 7_556 H11 C34 3.0030 no . 8_455 H11 C35 3.3983 no . 7_556 H11 C35 3.2245 no . 8_455 H11 C36 3.4141 no . 7_556 H11 H5 3.5034 no . 8_555 H11 H34 3.3977 no . 8_455 H12 O5 2.8492 no . 5_445 H12 O7 2.5635 no . 8_455 H12 C25 3.2461 no . 5_445 H12 C27 3.4788 no . 5_445 H12 C32 2.8823 no . 7_556 H12 C33 3.1627 no . 7_556 H12 C34 3.4638 no . 8_455 H12 H24 3.1635 no . 5_445 H12 H34 3.4188 no . 8_455 H13 O5 3.2402 no . 5_445 H13 C24 3.5754 no . 5_445 H13 C27 3.1298 no . 5_445 H13 C40 3.5577 no . 8_455 H13 H13 3.5234 no . 4_555 H13 H24 3.4205 no . 5_445 H13 H40 2.6355 no . 8_455 H14 C39 3.0016 no . 8_455 H14 C40 3.0097 no . 8_455 H14 H39 2.5192 no . 8_455 H14 H40 2.5463 no . 8_455 H15 C39 3.3533 no . 2_555 H15 H39 3.2466 no . 2_555 H16 C38 3.4798 no . 2_555 H16 C42 3.5940 no . 2_555 H16 C43 3.4248 no . 2_555 H18 C37 3.5461 no . . H18 H37 3.5212 no . . H19 C6 3.3329 no . 8_555 H19 C7 3.5599 no . 8_555 H19 H6 2.7381 no . 8_555 H19 H7 3.1465 no . 8_555 H19 H37 3.5850 no . . H23 C40 3.4784 no . 4_565 H23 H40 3.2638 no . 4_565 H24 C12 3.4246 no . 5_555 H24 C13 3.5326 no . 5_555 H24 H12 3.1635 no . 5_555 H24 H13 3.4205 no . 5_555 H34 H11 3.3977 no . 8_555 H34 H12 3.4188 no . 8_555 H37 O2 3.1825 no . 8_555 H37 N1 3.2406 no . 2_555 H37 C15 3.5138 no . 2_555 H37 C18 3.4796 no . . H37 C19 3.5133 no . . H37 C19 3.4867 no . 2_555 H37 H7 2.9330 no . 8_555 H37 H18 3.5212 no . . H37 H19 3.5850 no . . H39 O4 3.0517 no . 8_555 H39 C14 3.0600 no . 8_555 H39 C15 3.5292 no . 2_555 H39 H14 2.5192 no . 8_555 H39 H15 3.2466 no . 2_555 H40 C13 3.0591 no . 8_555 H40 C14 3.0334 no . 8_555 H40 C22 3.4300 no . . H40 C23 3.1859 no . 4_565 H40 C24 3.5996 no . 4_565 H40 H13 2.6355 no . 8_555 H40 H14 2.5463 no . 8_555 H40 H23 3.2638 no . 4_565 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.041 -0.007 -0.041 5135 1130 ' ' _platon_squeeze_details ; ; #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment '- cif_Rh-3_miyasaka.cif' data_Rhm-FPhTPTcoronene _database_code_depnum_ccdc_archive 'CCDC 878049' #TrackingRef '- cif_Rh-3_miyasaka.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C144 H84 F12 N12 O24 Rh6' _chemical_formula_moiety 'C144 H84 F12 N12 O24 Rh6' _chemical_formula_weight 3211.73 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/m 1' _symmetry_space_group_name_Hall '-C 2y' _symmetry_Int_Tables_number 12 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,-Z 3 -X,-Y,-Z 4 +X,-Y,+Z 5 1/2+X,1/2+Y,+Z 6 1/2-X,1/2+Y,-Z 7 1/2-X,1/2-Y,-Z 8 1/2+X,1/2-Y,+Z #------------------------------------------------------------------------------ _cell_length_a 19.709(3) _cell_length_b 28.892(4) _cell_length_c 20.386(3) _cell_angle_alpha 90.0000 _cell_angle_beta 113.556(2) _cell_angle_gamma 90.0000 _cell_volume 10641(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 8612 _cell_measurement_theta_min 1.78 _cell_measurement_theta_max 30.94 _cell_measurement_temperature 97 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.069 _exptl_crystal_size_mid 0.032 _exptl_crystal_size_min 0.016 _exptl_crystal_density_diffrn 1.002 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3204.00 _exptl_absorpt_coefficient_mu 0.512 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.871 _exptl_absorpt_correction_T_max 0.992 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 97 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_reflns_number 44330 _diffrn_reflns_av_R_equivalents 0.0654 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 12468 _reflns_number_gt 7848 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0728 _refine_ls_wR_factor_ref 0.2170 _refine_ls_number_restraints 66 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 12468 _refine_ls_number_parameters 487 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1278P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.590 _refine_diff_density_min -1.190 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.0171 0.0103 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Rh Rh -1.1178 0.9187 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh -0.206986(18) 0.280742(12) 0.02686(2) 0.03834(14) Uani 1.0 8 d . . . Rh2 Rh 0.43919(3) 0.5000 0.45270(3) 0.03917(16) Uani 1.0 4 d . . . F1 F -0.3909(5) 0.4051(3) 0.1891(6) 0.237(5) Uani 1.0 8 d . . . F2 F -0.0004(13) 0.1777(7) 0.3538(11) 0.092(8) Uani 0.1800 8 d . . . F3 F -0.1270(3) 0.04952(15) 0.2274(3) 0.0868(16) Uani 0.8200 8 d . . . F4 F 0.5403(7) 0.5000 0.1621(4) 0.169(4) Uani 1.0 4 d . . . F5 F 0.3745(9) 0.2611(6) 0.4316(12) 0.259(11) Uani 0.5000 8 d . . . O1 O -0.27827(17) 0.30505(11) 0.06752(19) 0.0439(8) Uani 1.0 8 d . . . O2 O -0.35953(17) 0.24704(11) 0.01793(19) 0.0435(8) Uani 1.0 8 d . . . O3 O -0.15731(17) 0.23971(11) 0.11391(18) 0.0413(8) Uani 1.0 8 d . . . O4 O -0.23823(17) 0.18165(11) 0.06349(19) 0.0428(8) Uani 1.0 8 d . . . O5 O 0.4885(2) 0.5000 0.3818(3) 0.0462(12) Uani 1.0 4 d . . . O6 O 0.6024(3) 0.5000 0.4714(3) 0.0517(13) Uani 1.0 4 d . . . O7 O 0.44286(18) 0.42909(12) 0.4559(2) 0.0498(9) Uani 1.0 8 d . . . N1 N -0.13248(19) 0.33929(13) 0.0792(3) 0.0412(10) Uani 1.0 8 d . . . N2 N -0.0473(3) 0.5000 0.1415(3) 0.0392(13) Uani 1.0 4 d . . . N3 N 0.06295(19) 0.45855(12) 0.2106(2) 0.0373(9) Uani 1.0 8 d . . . N4 N 0.3250(3) 0.5000 0.3687(3) 0.0395(13) Uani 1.0 4 d . . . C1 C -0.3392(3) 0.28337(16) 0.0549(3) 0.0434(12) Uani 1.0 8 d . . . C2 C -0.3864(4) 0.3038(2) 0.0880(4) 0.0621(14) Uani 1.0 8 d . . . C3 C -0.3675(5) 0.3467(3) 0.1227(6) 0.109(3) Uani 1.0 8 d . . . C4 C -0.4139(6) 0.3644(4) 0.1492(8) 0.130(3) Uani 1.0 8 d . . . C5 C -0.4765(5) 0.3438(3) 0.1508(6) 0.110(3) Uani 1.0 8 d . . . C6 C -0.4935(4) 0.3015(3) 0.1188(5) 0.0790(19) Uani 1.0 8 d . . . C7 C -0.4478(4) 0.2813(2) 0.0885(4) 0.0624(15) Uani 1.0 8 d . . . C8 C -0.1817(3) 0.19946(16) 0.1134(3) 0.0420(11) Uani 1.0 8 d . . . C9 C -0.1412(3) 0.16991(18) 0.1775(3) 0.0483(13) Uani 1.0 8 d . . . C10 C -0.0882(4) 0.1895(3) 0.2386(4) 0.0653(17) Uani 1.0 8 d . . . C11 C -0.0511(5) 0.1607(3) 0.2963(5) 0.090(3) Uani 1.0 8 d . . . C12 C -0.0644(4) 0.1128(3) 0.2943(4) 0.076(2) Uani 1.0 8 d . . . C13 C -0.1147(3) 0.0952(2) 0.2324(4) 0.0605(16) Uani 1.0 8 d . . . C14 C -0.1545(3) 0.12217(17) 0.1742(3) 0.0488(13) Uani 1.0 8 d . . . C15 C -0.1637(3) 0.38047(16) 0.0624(3) 0.0424(12) Uani 1.0 8 d . . . C16 C -0.1248(3) 0.42107(16) 0.0902(3) 0.0433(12) Uani 1.0 8 d . . . C17 C -0.0513(3) 0.41736(16) 0.1384(3) 0.0391(11) Uani 1.0 8 d . . . C18 C -0.0212(3) 0.37403(17) 0.1570(3) 0.0434(12) Uani 1.0 8 d . . . C19 C -0.0625(3) 0.33599(16) 0.1267(3) 0.0431(12) Uani 1.0 8 d . . . C20 C -0.0087(3) 0.46063(15) 0.1660(3) 0.0374(11) Uani 1.0 8 d . . . C21 C 0.0955(3) 0.5000 0.2311(4) 0.0404(16) Uani 1.0 4 d . . . C22 C 0.1745(3) 0.5000 0.2767(4) 0.0415(16) Uani 1.0 4 d . . . C23 C 0.2133(3) 0.54099(16) 0.2998(3) 0.0506(14) Uani 1.0 8 d . . . C24 C 0.2879(3) 0.53936(19) 0.3453(4) 0.0571(16) Uani 1.0 8 d . . . C25 C 0.5578(4) 0.5000 0.4057(4) 0.0427(16) Uani 1.0 4 d . . . C26 C 0.5908(4) 0.5000 0.3515(5) 0.056(2) Uani 1.0 4 d . . . C27 C 0.5507(5) 0.5000 0.2817(5) 0.066(3) Uani 1.0 4 d . . . C28 C 0.5839(7) 0.5000 0.2344(6) 0.084(3) Uani 1.0 4 d . . . C29 C 0.6556(8) 0.5000 0.2543(8) 0.095(4) Uani 1.0 4 d . . . C30 C 0.6999(7) 0.5000 0.3254(7) 0.103(5) Uani 1.0 4 d . . . C31 C 0.6686(6) 0.5000 0.3746(7) 0.110(5) Uani 1.0 4 d . . . C32 C 0.5000 0.4097(3) 0.5000 0.0464(17) Uani 1.0 4 d . . . C33 C 0.5000 0.3587(3) 0.5000 0.069(3) Uani 1.0 4 d . . . C34 C 0.4355(5) 0.3335(3) 0.4655(6) 0.116(4) Uani 1.0 8 d . . . C35 C 0.4354(8) 0.2853(4) 0.4700(11) 0.198(8) Uani 1.0 8 d . . . C36 C 0.5000 0.2606(5) 0.5000 0.232(15) Uani 1.0 4 d . . . C37 C 0.0366(3) 0.37269(19) 0.0234(4) 0.0533(14) Uani 1.0 8 d . . . C38 C 0.0748(3) 0.41523(17) 0.0491(3) 0.0423(12) Uani 1.0 8 d . . . C39 C 0.1507(3) 0.41617(19) 0.0982(3) 0.0482(13) Uani 1.0 8 d . . . C40 C 0.1865(3) 0.4568(2) 0.1208(3) 0.0520(14) Uani 1.0 8 d . . . C41 C 0.1499(4) 0.5000 0.0978(4) 0.0436(17) Uani 1.0 4 d . . . C42 C 0.0745(4) 0.5000 0.0489(4) 0.0426(16) Uani 1.0 4 d . . . C43 C 0.0384(3) 0.45722(17) 0.0246(3) 0.0427(12) Uani 1.0 8 d . . . H3 H -0.3236 0.3625 0.1272 0.1314 Uiso 1.0 8 calc R . . H5 H -0.5056 0.3582 0.1726 0.1318 Uiso 1.0 8 calc R . . H6 H -0.5364 0.2856 0.1169 0.0948 Uiso 1.0 8 calc R . . H7 H -0.4596 0.2513 0.0679 0.0749 Uiso 1.0 8 calc R . . H10 H -0.0776 0.2217 0.2408 0.0784 Uiso 1.0 8 calc R . . H12 H -0.0391 0.0936 0.3345 0.0916 Uiso 1.0 8 calc R . . H14 H -0.1905 0.1087 0.1322 0.0586 Uiso 1.0 8 calc R . . H15 H -0.2142 0.3825 0.0302 0.0508 Uiso 1.0 8 calc R . . H16 H -0.1478 0.4505 0.0767 0.0520 Uiso 1.0 8 calc R . . H18 H 0.0284 0.3706 0.1910 0.0521 Uiso 1.0 8 calc R . . H19 H -0.0409 0.3062 0.1397 0.0518 Uiso 1.0 8 calc R . . H23 H 0.1891 0.5699 0.2848 0.0607 Uiso 1.0 8 calc R . . H24 H 0.3138 0.5677 0.3605 0.0685 Uiso 1.0 8 calc R . . H27 H 0.4982 0.5000 0.2644 0.0788 Uiso 1.0 4 calc R . . H29 H 0.6765 0.5000 0.2197 0.1139 Uiso 1.0 4 calc R . . H30 H 0.7522 0.5000 0.3408 0.1235 Uiso 1.0 4 calc R . . H31 H 0.6993 0.5000 0.4243 0.1319 Uiso 1.0 4 calc R . . H34 H 0.3907 0.3493 0.4384 0.1389 Uiso 1.0 8 calc R . . H36 H 0.5000 0.2277 0.5000 0.2784 Uiso 1.0 4 calc R . . H37 H 0.0620 0.3441 0.0387 0.0640 Uiso 1.0 8 calc R . . H39 H 0.1764 0.3879 0.1152 0.0578 Uiso 1.0 8 calc R . . H40 H 0.2372 0.4566 0.1526 0.0624 Uiso 1.0 8 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rh1 0.0288(3) 0.0280(2) 0.0499(3) -0.00471(14) 0.00701(17) 0.00088(15) Rh2 0.0271(3) 0.0389(3) 0.0378(3) 0.0000 -0.0015(2) 0.0000 F1 0.232(7) 0.153(6) 0.421(12) -0.111(5) 0.230(8) -0.184(7) F2 0.111(17) 0.049(11) 0.050(12) -0.014(11) -0.036(11) 0.016(9) F3 0.070(3) 0.052(3) 0.101(4) 0.002(3) -0.005(3) 0.028(3) F4 0.254(12) 0.187(10) 0.055(5) 0.0000 0.048(7) 0.0000 F5 0.159(12) 0.120(11) 0.36(3) -0.076(11) -0.045(15) -0.072(14) O1 0.0359(18) 0.0358(18) 0.056(3) -0.0083(15) 0.0137(16) -0.0019(16) O2 0.0332(17) 0.0372(18) 0.052(3) -0.0085(14) 0.0088(16) -0.0045(16) O3 0.0339(17) 0.0339(18) 0.048(2) -0.0103(14) 0.0075(15) -0.0033(15) O4 0.0368(17) 0.0295(16) 0.052(2) -0.0016(14) 0.0067(16) 0.0063(15) O5 0.036(3) 0.049(3) 0.042(3) 0.0000 0.004(3) 0.0000 O6 0.034(3) 0.066(4) 0.045(3) 0.0000 0.005(3) 0.0000 O7 0.0396(19) 0.042(2) 0.051(3) -0.0012(15) 0.0013(17) 0.0022(17) N1 0.0224(18) 0.035(2) 0.058(3) -0.0060(16) 0.0071(18) 0.0030(19) N2 0.033(3) 0.030(3) 0.044(4) 0.0000 0.004(3) 0.0000 N3 0.0271(18) 0.0293(19) 0.044(3) -0.0022(15) 0.0021(16) -0.0020(16) N4 0.024(3) 0.041(3) 0.038(3) 0.0000 -0.004(3) 0.0000 C1 0.035(3) 0.036(3) 0.055(3) -0.003(2) 0.013(3) 0.002(3) C2 0.059(3) 0.040(3) 0.089(4) -0.007(3) 0.032(3) -0.012(3) C3 0.105(5) 0.066(4) 0.180(7) -0.029(4) 0.081(5) -0.053(4) C4 0.127(5) 0.084(5) 0.221(7) -0.033(4) 0.112(5) -0.071(5) C5 0.096(5) 0.085(5) 0.173(7) -0.018(4) 0.080(5) -0.045(5) C6 0.056(4) 0.072(4) 0.110(5) -0.006(3) 0.035(4) -0.016(4) C7 0.049(3) 0.054(3) 0.084(4) -0.006(3) 0.026(3) -0.010(3) C8 0.038(3) 0.033(3) 0.049(3) -0.006(2) 0.011(3) 0.001(2) C9 0.048(3) 0.044(3) 0.044(3) -0.005(3) 0.009(3) 0.003(3) C10 0.073(4) 0.060(4) 0.046(4) -0.011(4) 0.007(3) 0.011(3) C11 0.116(7) 0.062(5) 0.066(5) -0.005(5) 0.009(5) 0.020(4) C12 0.078(5) 0.072(5) 0.058(4) -0.004(4) 0.006(4) 0.027(4) C13 0.045(3) 0.046(4) 0.073(5) -0.005(3) 0.006(3) 0.014(3) C14 0.039(3) 0.040(3) 0.054(4) -0.006(3) 0.004(3) 0.010(3) C15 0.029(3) 0.033(3) 0.048(3) -0.0009(19) -0.002(2) 0.003(2) C16 0.039(3) 0.025(3) 0.053(3) -0.0020(19) 0.005(3) 0.001(2) C17 0.031(3) 0.034(3) 0.046(3) -0.0004(19) 0.009(2) 0.004(2) C18 0.031(3) 0.039(3) 0.051(3) -0.002(2) 0.007(2) 0.007(3) C19 0.033(3) 0.030(3) 0.056(4) 0.0043(19) 0.007(3) 0.001(2) C20 0.026(3) 0.032(3) 0.046(3) 0.0010(18) 0.006(2) 0.003(2) C21 0.027(3) 0.033(4) 0.042(4) 0.0000 -0.006(3) 0.0000 C22 0.028(4) 0.034(4) 0.052(5) 0.0000 0.004(3) 0.0000 C23 0.037(3) 0.028(3) 0.061(4) 0.001(2) -0.008(3) 0.003(3) C24 0.035(3) 0.041(3) 0.069(4) 0.006(3) -0.006(3) 0.005(3) C25 0.034(4) 0.039(4) 0.047(5) 0.0000 0.008(3) 0.0000 C26 0.048(5) 0.062(6) 0.050(5) 0.0000 0.011(4) 0.0000 C27 0.072(6) 0.062(6) 0.054(6) 0.0000 0.016(5) 0.0000 C28 0.103(9) 0.092(8) 0.050(6) 0.0000 0.024(6) 0.0000 C29 0.117(11) 0.092(9) 0.104(11) 0.0000 0.074(10) 0.0000 C30 0.065(7) 0.168(14) 0.081(9) 0.0000 0.035(7) 0.0000 C31 0.051(6) 0.200(16) 0.085(9) 0.0000 0.033(6) 0.0000 C32 0.034(4) 0.044(4) 0.048(5) 0.0000 0.001(3) 0.0000 C33 0.065(6) 0.042(5) 0.074(7) 0.0000 0.000(5) 0.0000 C34 0.098(7) 0.055(5) 0.149(10) -0.007(5) 0.002(6) 0.009(5) C35 0.142(11) 0.067(7) 0.30(2) -0.047(7) -0.005(12) -0.021(9) C36 0.139(16) 0.054(9) 0.42(5) 0.0000 0.02(2) 0.0000 C37 0.047(3) 0.045(3) 0.061(4) 0.008(3) 0.014(3) 0.006(3) C38 0.032(3) 0.039(3) 0.050(3) 0.003(2) 0.010(3) 0.006(3) C39 0.029(3) 0.050(3) 0.057(4) 0.012(3) 0.009(3) 0.008(3) C40 0.036(3) 0.060(4) 0.053(4) 0.002(3) 0.010(3) -0.001(3) C41 0.030(4) 0.038(4) 0.056(5) 0.0000 0.009(3) 0.0000 C42 0.034(4) 0.041(4) 0.050(5) 0.0000 0.014(3) 0.0000 C43 0.030(3) 0.040(3) 0.056(4) -0.001(2) 0.015(3) 0.003(3) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Rh1 Rh1 2.3970(5) yes . 7_455 Rh1 O1 2.021(4) yes . . Rh1 O2 2.038(4) yes . 7_455 Rh1 O3 2.031(4) yes . . Rh1 O4 2.037(4) yes . 7_455 Rh1 N1 2.214(4) yes . . Rh2 Rh2 2.4021(8) yes . 2_656 Rh2 O5 2.039(7) yes . . Rh2 O6 2.020(7) yes . 2_656 Rh2 O7 2.050(4) yes . . Rh2 O7 2.050(4) yes . 4_565 Rh2 N4 2.217(5) yes . . F1 C4 1.400(14) yes . . F2 C11 1.29(2) yes . . F3 C13 1.338(8) yes . . F4 C28 1.378(13) yes . . F5 C35 1.339(19) yes . . O1 C1 1.286(7) yes . . O2 C1 1.260(6) yes . . O3 C8 1.257(6) yes . . O4 C8 1.278(6) yes . . O5 C25 1.253(9) yes . . O6 C25 1.275(9) yes . . O7 C32 1.257(5) yes . . N1 C15 1.320(6) yes . . N1 C19 1.335(6) yes . . N2 C20 1.348(5) yes . . N2 C20 1.348(5) yes . 4_565 N3 C20 1.341(5) yes . . N3 C21 1.344(5) yes . . N4 C24 1.333(6) yes . . N4 C24 1.333(6) yes . 4_565 C1 C2 1.473(11) yes . . C2 C3 1.402(11) yes . . C2 C7 1.377(10) yes . . C3 C4 1.336(19) yes . . C4 C5 1.381(17) yes . . C5 C6 1.363(12) yes . . C6 C7 1.405(13) yes . . C8 C9 1.497(7) yes . . C9 C10 1.386(8) yes . . C9 C14 1.401(8) yes . . C10 C11 1.387(10) yes . . C11 C12 1.407(11) yes . . C12 C13 1.355(9) yes . . C13 C14 1.373(8) yes . . C15 C16 1.392(7) yes . . C16 C17 1.392(6) yes . . C17 C18 1.373(7) yes . . C17 C20 1.486(6) yes . . C18 C19 1.361(7) yes . . C21 C22 1.460(8) yes . . C22 C23 1.386(6) yes . . C22 C23 1.386(6) yes . 4_565 C23 C24 1.392(7) yes . . C25 C26 1.489(15) yes . . C26 C27 1.323(13) yes . . C26 C31 1.413(14) yes . . C27 C28 1.36(2) yes . . C28 C29 1.31(2) yes . . C29 C30 1.361(18) yes . . C30 C31 1.37(3) yes . . C32 C33 1.473(13) yes . . C33 C34 1.388(10) yes . . C33 C34 1.388(10) yes . 2_656 C34 C35 1.396(14) yes . . C35 C36 1.371(15) yes . . C37 C37 1.376(7) yes . 2_555 C37 C38 1.427(7) yes . . C38 C39 1.430(6) yes . . C38 C43 1.397(7) yes . . C39 C40 1.353(8) yes . . C40 C41 1.423(7) yes . . C41 C42 1.421(10) yes . . C42 C43 1.413(6) yes . . C42 C43 1.413(6) yes . 4_565 C43 C43 1.443(6) yes . 2_555 C3 H3 0.950 no . . C5 H5 0.950 no . . C6 H6 0.950 no . . C7 H7 0.950 no . . C10 H10 0.950 no . . C12 H12 0.950 no . . C14 H14 0.950 no . . C15 H15 0.950 no . . C16 H16 0.950 no . . C18 H18 0.950 no . . C19 H19 0.950 no . . C23 H23 0.950 no . . C24 H24 0.950 no . . C27 H27 0.950 no . . C29 H29 0.949 no . . C30 H30 0.950 no . . C31 H31 0.950 no . . C34 H34 0.950 no . . C36 H36 0.951 no . . C37 H37 0.950 no . . C39 H39 0.950 no . . C40 H40 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Rh1 Rh1 O1 87.95(9) yes 7_455 . . Rh1 Rh1 O2 88.15(9) yes 7_455 . 7_455 Rh1 Rh1 O3 88.43(9) yes 7_455 . . Rh1 Rh1 O4 87.69(9) yes 7_455 . 7_455 Rh1 Rh1 N1 176.38(13) yes 7_455 . . O1 Rh1 O2 176.07(12) yes . . 7_455 O1 Rh1 O3 90.91(15) yes . . . O1 Rh1 O4 88.93(15) yes . . 7_455 O1 Rh1 N1 88.44(16) yes . . . O2 Rh1 O3 89.41(15) yes 7_455 . . O2 Rh1 O4 90.48(15) yes 7_455 . 7_455 O2 Rh1 N1 95.47(16) yes 7_455 . . O3 Rh1 O4 176.12(13) yes . . 7_455 O3 Rh1 N1 91.69(14) yes . . . O4 Rh1 N1 92.18(14) yes 7_455 . . Rh2 Rh2 O5 87.92(11) yes 2_656 . . Rh2 Rh2 O6 88.01(14) yes 2_656 . 2_656 Rh2 Rh2 O7 87.89(9) yes 2_656 . . Rh2 Rh2 O7 87.89(9) yes 2_656 . 4_565 Rh2 Rh2 N4 177.68(19) yes 2_656 . . O5 Rh2 O6 175.93(18) yes . . 2_656 O5 Rh2 O7 90.12(13) yes . . . O5 Rh2 O7 90.12(13) yes . . 4_565 O5 Rh2 N4 94.4(3) yes . . . O6 Rh2 O7 89.73(13) yes 2_656 . . O6 Rh2 O7 89.73(13) yes 2_656 . 4_565 O6 Rh2 N4 89.7(3) yes 2_656 . . O7 Rh2 O7 175.76(12) yes . . 4_565 O7 Rh2 N4 92.10(9) yes . . . O7 Rh2 N4 92.10(9) yes 4_565 . . Rh1 O1 C1 119.7(4) yes . . . Rh1 O2 C1 119.2(4) yes 7_455 . . Rh1 O3 C8 118.9(3) yes . . . Rh1 O4 C8 118.9(3) yes 7_455 . . Rh2 O5 C25 118.6(6) yes . . . Rh2 O6 C25 119.0(6) yes 2_656 . . Rh2 O7 C32 118.6(4) yes . . . Rh1 N1 C15 114.4(3) yes . . . Rh1 N1 C19 126.1(3) yes . . . C15 N1 C19 119.5(4) yes . . . C20 N2 C20 115.0(5) yes . . 4_565 C20 N3 C21 114.4(4) yes . . . Rh2 N4 C24 121.2(3) yes . . . Rh2 N4 C24 121.2(3) yes . . 4_565 C24 N4 C24 117.2(5) yes . . 4_565 O1 C1 O2 125.0(6) yes . . . O1 C1 C2 115.0(5) yes . . . O2 C1 C2 120.0(5) yes . . . C1 C2 C3 119.7(7) yes . . . C1 C2 C7 122.2(6) yes . . . C3 C2 C7 118.0(9) yes . . . C2 C3 C4 117.1(9) yes . . . F1 C4 C3 116.2(10) yes . . . F1 C4 C5 115.7(13) yes . . . C3 C4 C5 127.4(10) yes . . . C4 C5 C6 115.1(11) yes . . . C5 C6 C7 120.4(8) yes . . . C2 C7 C6 121.8(6) yes . . . O3 C8 O4 126.0(5) yes . . . O3 C8 C9 116.8(4) yes . . . O4 C8 C9 117.2(5) yes . . . C8 C9 C10 119.9(5) yes . . . C8 C9 C14 119.6(5) yes . . . C10 C9 C14 120.3(5) yes . . . C9 C10 C11 118.1(6) yes . . . F2 C11 C10 119.8(11) yes . . . F2 C11 C12 117.8(11) yes . . . C10 C11 C12 122.4(7) yes . . . C11 C12 C13 117.1(6) yes . . . F3 C13 C12 118.9(6) yes . . . F3 C13 C14 118.1(5) yes . . . C12 C13 C14 123.0(6) yes . . . C9 C14 C13 119.0(5) yes . . . N1 C15 C16 122.0(4) yes . . . C15 C16 C17 118.1(5) yes . . . C16 C17 C18 118.6(4) yes . . . C16 C17 C20 118.3(4) yes . . . C18 C17 C20 123.1(4) yes . . . C17 C18 C19 119.8(4) yes . . . N1 C19 C18 122.0(5) yes . . . N2 C20 N3 125.0(4) yes . . . N2 C20 C17 114.8(4) yes . . . N3 C20 C17 120.1(4) yes . . . N3 C21 N3 126.0(5) yes . . 4_565 N3 C21 C22 116.9(3) yes . . . N3 C21 C22 116.9(3) yes 4_565 . . C21 C22 C23 121.3(3) yes . . . C21 C22 C23 121.3(3) yes . . 4_565 C23 C22 C23 117.4(5) yes . . 4_565 C22 C23 C24 119.3(5) yes . . . N4 C24 C23 123.4(5) yes . . . O5 C25 O6 126.5(9) yes . . . O5 C25 C26 116.3(7) yes . . . O6 C25 C26 117.2(7) yes . . . C25 C26 C27 123.2(8) yes . . . C25 C26 C31 119.4(9) yes . . . C27 C26 C31 117.4(11) yes . . . C26 C27 C28 120.7(10) yes . . . F4 C28 C27 119.1(12) yes . . . F4 C28 C29 117.9(15) yes . . . C27 C28 C29 123.1(12) yes . . . C28 C29 C30 119.0(17) yes . . . C29 C30 C31 119.6(13) yes . . . C26 C31 C30 120.1(11) yes . . . O7 C32 O7 127.1(8) yes . . 2_656 O7 C32 C33 116.5(4) yes . . . O7 C32 C33 116.5(4) yes 2_656 . . C32 C33 C34 121.6(5) yes . . . C32 C33 C34 121.6(5) yes . . 2_656 C34 C33 C34 116.7(8) yes . . 2_656 C33 C34 C35 120.9(9) yes . . . F5 C35 C34 120.4(12) yes . . . F5 C35 C36 116.4(12) yes . . . C34 C35 C36 121.6(11) yes . . . C35 C36 C35 117.3(13) yes . . 2_656 C37 C37 C38 120.5(5) yes 2_555 . . C37 C38 C39 121.6(5) yes . . . C37 C38 C43 119.7(4) yes . . . C39 C38 C43 118.6(5) yes . . . C38 C39 C40 120.8(5) yes . . . C39 C40 C41 121.5(5) yes . . . C40 C41 C40 122.4(6) yes . . 4_565 C40 C41 C42 118.8(3) yes . . . C40 C41 C42 118.8(3) yes 4_565 . . C41 C42 C43 119.0(3) yes . . . C41 C42 C43 119.0(3) yes . . 4_565 C43 C42 C43 122.0(6) yes . . 4_565 C38 C43 C42 121.3(4) yes . . . C38 C43 C43 119.7(5) yes . . 2_555 C42 C43 C43 119.0(5) yes . . 2_555 C2 C3 H3 121.451 no . . . C4 C3 H3 121.416 no . . . C4 C5 H5 122.447 no . . . C6 C5 H5 122.421 no . . . C5 C6 H6 119.819 no . . . C7 C6 H6 119.817 no . . . C2 C7 H7 119.128 no . . . C6 C7 H7 119.102 no . . . C9 C10 H10 120.977 no . . . C11 C10 H10 120.967 no . . . C11 C12 H12 121.479 no . . . C13 C12 H12 121.456 no . . . C9 C14 H14 120.466 no . . . C13 C14 H14 120.492 no . . . N1 C15 H15 118.972 no . . . C16 C15 H15 118.986 no . . . C15 C16 H16 120.969 no . . . C17 C16 H16 120.956 no . . . C17 C18 H18 120.135 no . . . C19 C18 H18 120.115 no . . . N1 C19 H19 119.015 no . . . C18 C19 H19 119.011 no . . . C22 C23 H23 120.344 no . . . C24 C23 H23 120.316 no . . . N4 C24 H24 118.301 no . . . C23 C24 H24 118.345 no . . . C26 C27 H27 119.567 no . . . C28 C27 H27 119.708 no . . . C28 C29 H29 120.496 no . . . C30 C29 H29 120.478 no . . . C29 C30 H30 120.160 no . . . C31 C30 H30 120.218 no . . . C26 C31 H31 119.893 no . . . C30 C31 H31 119.993 no . . . C33 C34 H34 119.530 no . . . C35 C34 H34 119.531 no . . . C35 C36 H36 121.337 no . . . C35 C36 H36 121.337 no 2_656 . . C37 C37 H37 119.733 no 2_555 . . C38 C37 H37 119.735 no . . . C38 C39 H39 119.597 no . . . C40 C39 H39 119.609 no . . . C39 C40 H40 119.256 no . . . C41 C40 H40 119.241 no . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 F1 C6 3.576(11) no . . F2 C9 3.563(19) no . . F2 C13 3.53(2) no . . F3 C11 3.586(9) no . . F4 C26 3.581(13) no . . F4 C30 3.551(14) no . . F5 C35 3.541(19) no . 2_656 O1 C3 2.718(13) no . . O1 C8 3.518(6) no . . O1 C8 3.452(7) no . 7_455 O1 C15 3.170(7) no . . O2 C7 2.843(10) no . . O2 C8 3.536(6) no . . O2 C8 3.458(8) no . 7_455 O3 C1 3.528(6) no . . O3 C1 3.479(8) no . 7_455 O3 C10 2.766(7) no . . O3 C19 3.303(6) no . . O4 C1 3.514(6) no . . O4 C1 3.481(8) no . 7_455 O4 C14 2.791(6) no . . O4 C15 3.095(6) no . 7_455 O5 C27 2.769(14) no . . O5 C32 3.497(8) no . . O6 C27 3.584(12) no . . O6 C31 2.767(18) no . . O6 C32 3.487(8) no . . O7 C24 3.120(6) no . 4_565 O7 C25 3.497(9) no . . O7 C25 3.490(9) no . 2_656 O7 C34 2.777(9) no . . O7 C34 3.588(9) no . 2_656 N1 C17 2.749(6) no . . N2 N3 2.386(6) no . 4_565 N2 C16 2.711(6) no . . N2 C16 2.711(6) no . 4_565 N2 C17 2.389(5) no . 4_565 N2 C21 2.674(7) no . . N3 C18 2.908(6) no . . N3 C20 2.692(6) no . 4_565 N3 C23 2.789(6) no . 4_565 N4 C22 2.805(7) no . . N4 C23 2.399(7) no . 4_565 C2 C5 2.819(15) no . . C3 C6 2.777(13) no . . C4 C7 2.660(12) no . . C9 C12 2.793(9) no . . C10 C13 2.767(9) no . . C11 C14 2.746(9) no . . C15 C18 2.705(6) no . . C16 C19 2.715(7) no . . C20 C22 3.593(7) no . . C22 C24 2.398(7) no . 4_565 C23 C24 2.706(7) no . 4_565 C26 C29 2.75(3) no . . C27 C30 2.711(17) no . . C28 C31 2.672(16) no . . C33 C35 2.423(14) no . 2_656 C33 C36 2.834(17) no . . C34 C35 2.733(15) no . 2_656 C37 C43 2.820(7) no . 2_555 C38 C38 2.827(6) no . 2_555 C38 C41 2.828(6) no . . C39 C42 2.815(7) no . . C40 C43 2.791(7) no . . C42 C42 2.814(10) no . 2_555 Rh2 O7 3.100(4) no . 3_666 Rh2 C32 2.872(8) no . 3_666 F1 F4 3.010(10) no . 1_455 F1 C28 2.996(11) no . 1_455 F1 C29 3.024(10) no . 1_455 F2 C33 3.16(3) no . 7_556 F2 C34 3.40(3) no . 7_556 F2 C34 3.03(3) no . 8_455 F2 C35 3.46(3) no . 7_556 F2 C35 3.28(4) no . 8_455 F2 C36 3.47(3) no . 7_556 F3 F3 2.861(7) no . 4_555 F3 O5 3.378(7) no . 5_445 F3 C24 3.450(10) no . 5_445 F3 C27 3.527(10) no . 5_445 F3 C40 3.447(7) no . 8_455 F4 F1 3.010(10) no . 1_655 F4 F1 3.010(10) no . 4_665 O2 C6 3.491(8) no . 2_455 O3 C6 3.406(9) no . 8_555 O5 F3 3.378(7) no . 5_555 O5 F3 3.378(7) no . 8_555 O5 C32 3.497(8) no . 3_666 O6 O7 2.871(7) no . 3_666 O6 C32 3.487(8) no . 3_666 O7 C12 3.460(9) no . 8_555 N1 C37 3.469(9) no . 2_555 N2 C42 3.598(12) no . . N3 C39 3.593(8) no . . N3 C40 3.585(9) no . . N3 C41 3.579(10) no . . N3 C42 3.598(10) no . . C5 C9 3.522(13) no . 8_455 C5 C10 3.483(15) no . 8_455 C6 O2 3.491(8) no . 2_455 C6 O3 3.406(9) no . 8_455 C7 C7 3.365(10) no . 2_455 C9 C5 3.522(13) no . 8_555 C10 C5 3.483(15) no . 8_555 C11 C34 3.566(16) no . 8_455 C12 O7 3.460(9) no . 8_455 C15 C37 3.588(10) no . 2_555 C15 C38 3.524(9) no . 2_555 C15 C39 3.537(9) no . 2_555 C16 C38 3.362(9) no . 2_555 C16 C43 3.558(9) no . 2_555 C18 C37 3.346(10) no . . C18 C37 3.568(9) no . 2_555 C19 C37 3.558(10) no . . C19 C37 3.463(10) no . 2_555 C20 C42 3.580(11) no . . C20 C43 3.364(9) no . . C21 C41 3.296(13) no . . C21 C42 3.569(12) no . . C22 C40 3.510(11) no . . C22 C40 3.510(11) no . 4_565 C22 C41 3.482(12) no . . C23 C40 3.474(9) no . 4_565 C24 F3 3.450(10) no . 5_555 C25 O7 3.490(9) no . 3_666 C27 F3 3.527(10) no . 5_555 C27 F3 3.527(10) no . 8_555 C28 F1 2.996(11) no . 1_655 C28 F1 2.996(11) no . 4_665 C29 F1 3.024(10) no . 1_655 C29 F1 3.024(10) no . 4_665 C33 F2 3.16(3) no . 7_556 C33 F2 3.16(3) no . 8_555 C34 F2 3.40(3) no . 7_556 C34 F2 3.03(3) no . 8_555 C34 C11 3.566(16) no . 8_555 C35 F2 3.46(3) no . 7_556 C35 F2 3.28(4) no . 8_555 C36 F2 3.47(3) no . 7_556 C36 F2 3.47(3) no . 8_555 C37 N1 3.469(9) no . 2_555 C37 C15 3.588(10) no . 2_555 C37 C18 3.346(10) no . . C37 C18 3.568(9) no . 2_555 C37 C19 3.558(10) no . . C37 C19 3.463(10) no . 2_555 C38 C15 3.524(9) no . 2_555 C38 C16 3.362(9) no . 2_555 C39 N3 3.593(8) no . . C39 C15 3.537(9) no . 2_555 C40 F3 3.447(7) no . 8_555 C40 N3 3.585(9) no . . C40 C22 3.510(11) no . . C40 C23 3.474(9) no . 4_565 C41 N3 3.579(10) no . . C41 N3 3.579(10) no . 4_565 C41 C21 3.296(13) no . . C41 C22 3.482(12) no . . C42 N2 3.598(12) no . . C42 N3 3.598(10) no . . C42 N3 3.598(10) no . 4_565 C42 C20 3.580(11) no . . C42 C20 3.580(11) no . 4_565 C42 C21 3.569(12) no . . C42 C43 2.461(7) no . 3_565 C43 C16 3.558(9) no . 2_555 C43 C20 3.364(9) no . . C43 C43 2.862(7) no . 3_565 Rh1 H15 2.9440 no . . Rh1 H19 3.2447 no . . Rh2 H24 3.1239 no . . Rh2 H24 3.1239 no . 4_565 F1 H3 2.4923 no . . F1 H5 2.5420 no . . F2 H10 2.5375 no . . F2 H12 2.5296 no . . F3 H12 2.5242 no . . F3 H14 2.5114 no . . F4 H27 2.5333 no . . F4 H29 2.4635 no . . F5 H34 2.5650 no . . F5 H36 2.4972 no . . O1 H3 2.4286 no . . O1 H15 2.8182 no . . O2 H7 2.5597 no . . O2 H19 3.3913 no . 7_455 O3 H10 2.4862 no . . O3 H19 2.8750 no . . O4 H14 2.4984 no . . O4 H15 2.5547 no . 7_455 O5 H27 2.4765 no . . O6 H31 2.4556 no . . O7 H24 2.5115 no . 4_565 O7 H34 2.4913 no . . N1 H16 3.2248 no . . N1 H18 3.2079 no . . N2 H16 2.3716 no . . N2 H16 2.3716 no . 4_565 N3 H18 2.6194 no . . N3 H23 2.4780 no . 4_565 N4 H23 3.2433 no . . N4 H23 3.2433 no . 4_565 N4 H24 1.9694 no . 4_565 C1 H3 2.6699 no . . C1 H7 2.6573 no . . C2 H6 3.2785 no . . C3 H5 3.2815 no . . C3 H7 3.2416 no . . C4 H6 3.1889 no . . C5 H3 3.2805 no . . C5 H7 3.2489 no . . C7 H3 3.2513 no . . C7 H5 3.2747 no . . C8 H10 2.6663 no . . C8 H14 2.6673 no . . C10 H12 3.3058 no . . C10 H14 3.2752 no . . C12 H10 3.3054 no . . C12 H14 3.2476 no . . C14 H10 3.2803 no . . C14 H12 3.2561 no . . C15 H19 3.1458 no . . C16 H18 3.2414 no . . C17 H15 3.2442 no . . C17 H19 3.2179 no . . C18 H16 3.2437 no . . C19 H15 3.1476 no . . C20 H16 2.6316 no . . C20 H18 2.6946 no . . C21 H23 2.6586 no . . C21 H23 2.6586 no . 4_565 C22 H23 2.0378 no . 4_565 C22 H24 3.2463 no . . C22 H24 3.2463 no . 4_565 C23 H23 3.2360 no . 4_565 C24 H24 3.1314 no . 4_565 C25 H27 2.6411 no . . C25 H31 2.6592 no . . C26 H30 3.2743 no . . C27 H29 3.2022 no . . C27 H31 3.1972 no . . C28 H30 3.1560 no . . C29 H27 3.1898 no . . C29 H31 3.2202 no . . C31 H27 3.2088 no . . C31 H29 3.2235 no . . C32 H34 2.6651 no . . C32 H34 2.6651 no . 2_656 C33 H34 2.0323 no . 2_656 C34 H34 3.2284 no . 2_656 C34 H36 3.2777 no . . C36 H34 3.2592 no . . C36 H34 3.2592 no . 2_656 C37 H39 2.6759 no . . C38 H37 3.2917 no . 2_555 C38 H40 3.2750 no . . C39 H37 2.6770 no . . C40 H40 2.6763 no . 4_565 C41 H39 3.2774 no . . C41 H39 3.2774 no . 4_565 C41 H40 2.0612 no . 4_565 C42 H40 3.3033 no . . C42 H40 3.3033 no . 4_565 C43 H37 3.2963 no . . C43 H39 3.2869 no . . H3 H15 3.5071 no . . H5 H6 2.3450 no . . H6 H7 2.3392 no . . H10 H19 3.4533 no . . H14 H15 3.0964 no . 7_455 H15 H16 2.3411 no . . H16 H16 2.8620 no . 4_565 H18 H19 2.2982 no . . H18 H23 3.4350 no . 4_565 H23 H24 2.3226 no . . H24 H34 2.9389 no . 4_565 H29 H30 2.3195 no . . H30 H31 2.3248 no . . H37 H37 2.3187 no . 2_555 H37 H39 2.5103 no . . H39 H40 2.2863 no . . H40 H40 2.5095 no . 4_565 F1 H29 3.0005 no . 1_455 F2 H34 3.3379 no . 8_455 F3 H24 3.3972 no . 5_445 F3 H27 2.6870 no . 5_445 F3 H40 2.5003 no . 8_455 O2 H6 2.9151 no . 2_455 O2 H7 3.2861 no . 2_455 O2 H37 3.1684 no . 8_455 O3 H6 2.4709 no . 8_555 O4 H39 3.0654 no . 8_455 O5 H12 2.8490 no . 5_555 O5 H12 2.8490 no . 8_555 O7 H12 2.7172 no . 8_555 N1 H37 3.2254 no . 2_555 C1 H6 3.3783 no . 2_455 C6 H10 3.5617 no . 8_455 C6 H19 3.3259 no . 8_455 C7 H7 3.0986 no . 2_455 C7 H19 3.5179 no . 8_455 C8 H5 3.5954 no . 8_555 C8 H6 2.8698 no . 8_555 C9 H5 2.8318 no . 8_555 C9 H6 3.0798 no . 8_555 C10 H5 2.8468 no . 8_555 C10 H6 3.1210 no . 8_555 C11 H5 3.0454 no . 8_555 C11 H34 3.5266 no . 8_455 C12 H5 3.2395 no . 8_555 C12 H24 3.4468 no . 5_445 C12 H34 3.5628 no . 8_455 C13 H5 3.1653 no . 8_555 C13 H24 3.5195 no . 5_445 C13 H27 3.4329 no . 5_445 C13 H40 3.0985 no . 8_455 C14 H5 3.0015 no . 8_555 C14 H39 3.0720 no . 8_455 C14 H40 3.0286 no . 8_455 C15 H37 3.5592 no . 2_555 C15 H39 3.5328 no . 2_555 C18 H37 3.5218 no . . C19 H6 3.5682 no . 8_555 C19 H37 3.5781 no . . C19 H37 3.3849 no . 2_555 C22 H40 3.4640 no . . C22 H40 3.4640 no . 4_565 C23 H40 3.2195 no . 4_565 C25 H12 3.2937 no . 5_555 C25 H12 3.2937 no . 8_555 C32 H12 3.1469 no . 7_556 C32 H12 3.1469 no . 8_555 C33 H12 3.4342 no . 7_556 C33 H12 3.4342 no . 8_555 C34 H12 3.5895 no . 8_555 C37 H18 3.4852 no . . C38 H16 3.5549 no . 2_555 C39 H14 3.0078 no . 8_555 C39 H15 3.4615 no . 2_555 C39 H23 3.5919 no . 4_565 C40 H14 3.0088 no . 8_555 C40 H23 3.4125 no . 4_565 C43 H16 3.5384 no . 2_555 H5 C8 3.5954 no . 8_455 H5 C9 2.8318 no . 8_455 H5 C10 2.8468 no . 8_455 H5 C11 3.0454 no . 8_455 H5 C12 3.2395 no . 8_455 H5 C13 3.1653 no . 8_455 H5 C14 3.0015 no . 8_455 H5 H10 3.2926 no . 8_455 H5 H14 3.5329 no . 8_455 H6 O2 2.9151 no . 2_455 H6 O3 2.4709 no . 8_455 H6 C1 3.3783 no . 2_455 H6 C8 2.8698 no . 8_455 H6 C9 3.0798 no . 8_455 H6 C10 3.1210 no . 8_455 H6 C19 3.5682 no . 8_455 H6 H10 2.9539 no . 8_455 H6 H19 2.7006 no . 8_455 H7 O2 3.2861 no . 2_455 H7 C7 3.0986 no . 2_455 H7 H7 2.5848 no . 2_455 H7 H19 3.0566 no . 8_455 H7 H37 3.5919 no . 7_455 H7 H37 2.8891 no . 8_455 H10 C6 3.5617 no . 8_555 H10 H5 3.2926 no . 8_555 H10 H6 2.9539 no . 8_555 H12 O5 2.8490 no . 5_445 H12 O7 2.7172 no . 8_455 H12 C25 3.2937 no . 5_445 H12 C32 3.1469 no . 7_556 H12 C33 3.4342 no . 7_556 H12 C34 3.5895 no . 8_455 H12 H24 3.2367 no . 5_445 H12 H27 3.2769 no . 5_445 H12 H34 3.3853 no . 8_455 H14 C39 3.0078 no . 8_455 H14 C40 3.0088 no . 8_455 H14 H5 3.5329 no . 8_555 H14 H39 2.5065 no . 8_455 H14 H40 2.4947 no . 8_455 H15 C39 3.4615 no . 2_555 H15 H39 3.3362 no . 2_555 H16 C38 3.5549 no . 2_555 H16 C43 3.5384 no . 2_555 H18 C37 3.4852 no . . H18 H37 3.5071 no . . H19 C6 3.3259 no . 8_555 H19 C7 3.5179 no . 8_555 H19 H6 2.7006 no . 8_555 H19 H7 3.0566 no . 8_555 H19 H37 3.5891 no . . H23 C39 3.5919 no . 4_565 H23 C40 3.4125 no . 4_565 H23 H39 3.5792 no . 4_565 H23 H40 3.2841 no . 4_565 H24 F3 3.3972 no . 5_555 H24 C12 3.4468 no . 5_555 H24 C13 3.5195 no . 5_555 H24 H12 3.2367 no . 5_555 H27 F3 2.6870 no . 5_555 H27 F3 2.6870 no . 8_555 H27 C13 3.4329 no . 5_555 H27 C13 3.4329 no . 8_555 H27 H12 3.2769 no . 5_555 H27 H12 3.2769 no . 8_555 H29 F1 3.0005 no . 1_655 H29 F1 3.0005 no . 4_665 H34 F2 3.3379 no . 8_555 H34 C11 3.5266 no . 8_555 H34 C12 3.5628 no . 8_555 H34 H12 3.3853 no . 8_555 H37 O2 3.1684 no . 8_555 H37 N1 3.2254 no . 2_555 H37 C15 3.5592 no . 2_555 H37 C18 3.5218 no . . H37 C19 3.5781 no . . H37 C19 3.3849 no . 2_555 H37 H7 3.5919 no . 7_455 H37 H7 2.8891 no . 8_555 H37 H18 3.5071 no . . H37 H19 3.5891 no . . H39 O4 3.0654 no . 8_555 H39 C14 3.0720 no . 8_555 H39 C15 3.5328 no . 2_555 H39 H14 2.5065 no . 8_555 H39 H15 3.3362 no . 2_555 H39 H23 3.5792 no . 4_565 H40 F3 2.5003 no . 8_555 H40 C13 3.0985 no . 8_555 H40 C14 3.0286 no . 8_555 H40 C22 3.4640 no . . H40 C23 3.2195 no . 4_565 H40 H14 2.4947 no . 8_555 H40 H23 3.2841 no . 4_565 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.033 -0.006 0.472 5151 950 ' ' _platon_squeeze_details ; ; #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment '- cif_Ru-1_miyasaka.cif' data_RuPhTPTcoronene _database_code_depnum_ccdc_archive 'CCDC 878050' #TrackingRef '- cif_Ru-1_miyasaka.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C144 H96 N12 O24 Ru6' _chemical_formula_moiety 'C144 H96 N12 O24 Ru6' _chemical_formula_weight 2984.83 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/m 1' _symmetry_space_group_name_Hall '-C 2y' _symmetry_Int_Tables_number 12 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,-Z 3 -X,-Y,-Z 4 +X,-Y,+Z 5 1/2+X,1/2+Y,+Z 6 1/2-X,1/2+Y,-Z 7 1/2-X,1/2-Y,-Z 8 1/2+X,1/2-Y,+Z #------------------------------------------------------------------------------ _cell_length_a 19.686(3) _cell_length_b 28.643(4) _cell_length_c 19.816(3) _cell_angle_alpha 90.0000 _cell_angle_beta 112.198(3) _cell_angle_gamma 90.0000 _cell_volume 10345(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7788 _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 30.80 _cell_measurement_temperature 97 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.060 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.010 _exptl_crystal_density_diffrn 0.958 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3000.00 _exptl_absorpt_coefficient_mu 0.475 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.918 _exptl_absorpt_correction_T_max 0.995 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 97 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_reflns_number 35790 _diffrn_reflns_av_R_equivalents 0.0879 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 9315 _reflns_number_gt 5164 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1501 _refine_ls_number_restraints 57 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 9271 _refine_ls_number_parameters 445 _refine_ls_goodness_of_fit_ref 0.872 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0708P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.690 _refine_diff_density_min -0.730 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ru Ru -1.2594 0.8363 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru -0.20780(2) 0.278752(13) 0.02472(3) 0.03442(16) Uani 1.0 8 d . . . Ru2 Ru 0.44043(3) 0.5000 0.46012(4) 0.0382(2) Uani 1.0 4 d . . . O1 O -0.27751(19) 0.30655(11) 0.0697(2) 0.0397(10) Uani 1.0 8 d . . . O2 O -0.35979(18) 0.24997(12) 0.0225(2) 0.0407(10) Uani 1.0 8 d . . . O3 O -0.15954(19) 0.23782(11) 0.11548(19) 0.0388(10) Uani 1.0 8 d . . . O4 O -0.24181(19) 0.18113(11) 0.0670(2) 0.0409(10) Uani 1.0 8 d . . . O5 O 0.4763(3) 0.5000 0.3743(3) 0.0424(14) Uani 1.0 4 d . . . O6 O 0.5944(3) 0.5000 0.4545(3) 0.0474(15) Uani 1.0 4 d . . . O7 O 0.4416(2) 0.42803(12) 0.4626(2) 0.0482(11) Uani 1.0 8 d . . . N1 N -0.1299(2) 0.33812(13) 0.0836(3) 0.0337(11) Uani 1.0 8 d . . . N2 N -0.0459(3) 0.5000 0.1492(3) 0.0373(17) Uani 1.0 4 d . . . N3 N 0.0609(3) 0.45806(14) 0.2215(3) 0.0399(12) Uani 1.0 8 d . . . N4 N 0.3195(3) 0.5000 0.3790(4) 0.0455(19) Uani 1.0 4 d . . . C1 C -0.3376(3) 0.28719(17) 0.0592(4) 0.0403(15) Uani 1.0 8 d . . . C2 C -0.3850(4) 0.30757(19) 0.0954(4) 0.0522(17) Uani 1.0 8 d . . . C3 C -0.3611(5) 0.3482(3) 0.1370(5) 0.092(3) Uani 1.0 8 d . . . C4 C -0.4029(6) 0.3686(3) 0.1711(6) 0.122(4) Uani 1.0 8 d . . . C5 C -0.4700(5) 0.3477(3) 0.1645(6) 0.108(4) Uani 1.0 8 d . . . C6 C -0.4935(4) 0.3069(3) 0.1254(5) 0.071(3) Uani 1.0 8 d . . . C7 C -0.4489(4) 0.2872(2) 0.0930(4) 0.0589(19) Uani 1.0 8 d . . . C8 C -0.1848(3) 0.19744(17) 0.1175(3) 0.0380(14) Uani 1.0 8 d . . . C9 C -0.1455(3) 0.16807(18) 0.1820(4) 0.0446(15) Uani 1.0 8 d . . . C10 C -0.0953(4) 0.1883(3) 0.2440(4) 0.065(2) Uani 1.0 8 d . . . C11 C -0.0566(5) 0.1607(3) 0.3036(4) 0.086(3) Uani 1.0 8 d . . . C12 C -0.0691(5) 0.1134(3) 0.3009(5) 0.091(3) Uani 1.0 8 d . . . C13 C -0.1207(4) 0.0929(3) 0.2389(5) 0.080(3) Uani 1.0 8 d . . . C14 C -0.1599(3) 0.1203(2) 0.1799(4) 0.0553(18) Uani 1.0 8 d . . . C15 C -0.1589(3) 0.38050(16) 0.0637(4) 0.0430(16) Uani 1.0 8 d . . . C16 C -0.1213(3) 0.42027(17) 0.0936(4) 0.0475(17) Uani 1.0 8 d . . . C17 C -0.0496(3) 0.41667(16) 0.1459(3) 0.0341(14) Uani 1.0 8 d . . . C18 C -0.0221(3) 0.37349(18) 0.1655(4) 0.0456(16) Uani 1.0 8 d . . . C19 C -0.0628(3) 0.33537(17) 0.1342(3) 0.0419(15) Uani 1.0 8 d . . . C20 C -0.0089(3) 0.46037(16) 0.1742(3) 0.0364(14) Uani 1.0 8 d . . . C21 C 0.0932(4) 0.5000 0.2442(4) 0.037(2) Uani 1.0 4 d . . . C22 C 0.1708(4) 0.5000 0.2910(4) 0.041(2) Uani 1.0 4 d . . . C23 C 0.2090(3) 0.54115(17) 0.3132(4) 0.0504(18) Uani 1.0 8 d . . . C24 C 0.2830(3) 0.53999(17) 0.3586(4) 0.0508(18) Uani 1.0 8 d . . . C25 C 0.5453(6) 0.5000 0.3915(6) 0.058(3) Uani 1.0 4 d . . . C26 C 0.5690(7) 0.5000 0.3269(7) 0.084(3) Uani 1.0 4 d . . . C27 C 0.5293(8) 0.5000 0.2596(8) 0.115(4) Uani 1.0 4 d . . . C28 C 0.5567(9) 0.5000 0.2049(8) 0.130(4) Uani 1.0 4 d . . . C29 C 0.6211(10) 0.5000 0.2155(9) 0.140(4) Uani 1.0 4 d . . . C30 C 0.6726(9) 0.5000 0.2860(9) 0.152(4) Uani 1.0 4 d . . . C31 C 0.6421(9) 0.5000 0.3408(9) 0.141(4) Uani 1.0 4 d . . . C32 C 0.5000 0.4072(3) 0.5000 0.045(3) Uani 1.0 4 d . . . C33 C 0.5000 0.3554(3) 0.5000 0.057(3) Uani 1.0 4 d . . . C34 C 0.5658(4) 0.3313(3) 0.5243(5) 0.085(3) Uani 1.0 8 d . . . C35 C 0.5647(6) 0.2813(3) 0.5234(7) 0.139(5) Uani 1.0 8 d . . . C36 C 0.5000 0.2579(4) 0.5000 0.136(7) Uani 1.0 4 d . . . C37 C 0.0349(3) 0.37258(18) 0.0254(4) 0.0492(17) Uani 1.0 8 d . . . C38 C 0.0732(3) 0.41407(18) 0.0527(4) 0.0420(15) Uani 1.0 8 d . . . C39 C 0.1468(3) 0.41532(19) 0.1041(4) 0.0487(17) Uani 1.0 8 d . . . C40 C 0.1808(3) 0.4565(2) 0.1269(4) 0.0504(17) Uani 1.0 8 d . . . C41 C 0.1460(4) 0.5000 0.1020(5) 0.041(2) Uani 1.0 4 d . . . C42 C 0.0741(4) 0.5000 0.0498(4) 0.039(2) Uani 1.0 4 d . . . C43 C 0.0371(3) 0.45711(16) 0.0259(3) 0.0392(15) Uani 1.0 8 d . . . H3 H -0.3156 0.3619 0.1418 0.1104 Uiso 1.0 8 calc R . . H4 H -0.3868 0.3965 0.1986 0.1462 Uiso 1.0 8 calc R . . H5 H -0.4995 0.3619 0.1873 0.1299 Uiso 1.0 8 calc R . . H6 H -0.5387 0.2927 0.1209 0.0853 Uiso 1.0 8 calc R . . H7 H -0.4633 0.2584 0.0679 0.0706 Uiso 1.0 8 calc R . . H10 H -0.0872 0.2210 0.2459 0.0778 Uiso 1.0 8 calc R . . H11 H -0.0216 0.1744 0.3462 0.1033 Uiso 1.0 8 calc R . . H12 H -0.0423 0.0944 0.3416 0.1088 Uiso 1.0 8 calc R . . H13 H -0.1289 0.0602 0.2373 0.0954 Uiso 1.0 8 calc R . . H14 H -0.1964 0.1068 0.1381 0.0664 Uiso 1.0 8 calc R . . H15 H -0.2071 0.3830 0.0277 0.0516 Uiso 1.0 8 calc R . . H16 H -0.1434 0.4500 0.0792 0.0570 Uiso 1.0 8 calc R . . H18 H 0.0260 0.3697 0.2013 0.0547 Uiso 1.0 8 calc R . . H19 H -0.0423 0.3053 0.1492 0.0503 Uiso 1.0 8 calc R . . H23 H 0.1850 0.5702 0.2977 0.0605 Uiso 1.0 8 calc R . . H24 H 0.3081 0.5686 0.3755 0.0610 Uiso 1.0 8 calc R . . H27 H 0.4775 0.5000 0.2459 0.1379 Uiso 1.0 4 calc R . . H28 H 0.5227 0.5000 0.1558 0.1560 Uiso 1.0 4 calc R . . H29 H 0.6365 0.5000 0.1755 0.1675 Uiso 1.0 4 calc R . . H30 H 0.7239 0.5000 0.2970 0.1829 Uiso 1.0 4 calc R . . H31 H 0.6751 0.5000 0.3903 0.1688 Uiso 1.0 4 calc R . . H34 H 0.6111 0.3477 0.5412 0.1018 Uiso 1.0 8 calc R . . H35 H 0.6096 0.2645 0.5394 0.1669 Uiso 1.0 8 calc R . . H36 H 0.5000 0.2247 0.5000 0.1631 Uiso 1.0 4 calc R . . H37 H 0.0584 0.3436 0.0430 0.0590 Uiso 1.0 8 calc R . . H39 H 0.1721 0.3870 0.1225 0.0585 Uiso 1.0 8 calc R . . H40 H 0.2300 0.4564 0.1611 0.0604 Uiso 1.0 8 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru1 0.0279(3) 0.0265(3) 0.0438(3) -0.00493(18) 0.0078(2) 0.0006(2) Ru2 0.0282(4) 0.0404(4) 0.0346(4) 0.0000 -0.0011(3) 0.0000 O1 0.035(3) 0.030(2) 0.054(3) -0.0069(17) 0.016(2) -0.0028(18) O2 0.031(2) 0.044(3) 0.044(3) -0.0035(18) 0.0106(19) -0.0002(19) O3 0.040(3) 0.034(2) 0.041(3) -0.0066(17) 0.0143(19) 0.0027(17) O4 0.035(2) 0.030(2) 0.049(3) -0.0071(17) 0.006(2) 0.0057(18) O5 0.049(4) 0.041(3) 0.027(3) 0.0000 0.003(3) 0.0000 O6 0.036(4) 0.059(4) 0.043(4) 0.0000 0.010(3) 0.0000 O7 0.040(3) 0.046(3) 0.046(3) 0.004(2) 0.002(2) 0.002(2) N1 0.022(3) 0.025(3) 0.041(3) -0.0077(19) -0.003(2) 0.005(2) N2 0.024(4) 0.023(4) 0.051(5) 0.0000 -0.002(3) 0.0000 N3 0.026(3) 0.033(3) 0.053(4) -0.002(2) 0.006(3) 0.002(3) N4 0.027(4) 0.046(4) 0.044(5) 0.0000 -0.008(4) 0.0000 C1 0.038(4) 0.027(3) 0.053(4) -0.007(3) 0.014(3) 0.001(3) C2 0.051(4) 0.038(4) 0.071(5) 0.001(3) 0.027(4) -0.007(3) C3 0.083(6) 0.055(5) 0.173(10) -0.020(4) 0.089(7) -0.032(5) C4 0.123(8) 0.089(6) 0.202(12) -0.031(6) 0.116(9) -0.081(7) C5 0.089(7) 0.081(6) 0.182(11) 0.003(5) 0.083(7) -0.028(7) C6 0.057(5) 0.061(5) 0.110(7) -0.009(4) 0.048(5) -0.031(5) C7 0.036(4) 0.055(4) 0.080(6) -0.003(3) 0.015(4) -0.022(4) C8 0.044(4) 0.028(3) 0.040(4) 0.003(3) 0.013(3) 0.002(3) C9 0.042(4) 0.038(4) 0.047(4) 0.001(3) 0.010(3) 0.008(3) C10 0.072(5) 0.056(4) 0.048(5) -0.008(4) 0.001(4) 0.007(4) C11 0.108(7) 0.076(6) 0.045(5) -0.020(5) -0.005(5) 0.018(4) C12 0.110(7) 0.077(6) 0.062(6) -0.004(5) 0.006(5) 0.041(5) C13 0.077(6) 0.048(4) 0.096(7) -0.006(4) 0.012(5) 0.041(5) C14 0.039(4) 0.049(4) 0.065(5) -0.009(3) 0.004(4) 0.017(4) C15 0.034(4) 0.025(3) 0.062(5) -0.009(3) 0.010(3) -0.003(3) C16 0.041(4) 0.025(3) 0.061(5) -0.005(3) 0.002(3) 0.010(3) C17 0.028(3) 0.025(3) 0.042(4) 0.003(3) 0.004(3) 0.000(3) C18 0.032(4) 0.036(4) 0.055(4) -0.003(3) 0.002(3) 0.001(3) C19 0.042(4) 0.028(3) 0.046(4) 0.009(3) 0.005(3) 0.006(3) C20 0.026(3) 0.027(3) 0.050(4) -0.004(3) 0.008(3) 0.001(3) C21 0.035(5) 0.025(4) 0.044(5) 0.0000 0.006(4) 0.0000 C22 0.040(5) 0.033(5) 0.037(5) 0.0000 -0.001(4) 0.0000 C23 0.043(4) 0.028(3) 0.058(5) -0.002(3) -0.005(4) 0.003(3) C24 0.036(4) 0.027(3) 0.064(5) 0.004(3) -0.011(4) 0.001(3) C25 0.080(7) 0.047(5) 0.058(6) 0.0000 0.038(6) 0.0000 C26 0.098(6) 0.100(6) 0.070(5) 0.0000 0.049(5) 0.0000 C27 0.124(7) 0.161(8) 0.076(6) 0.0000 0.055(6) 0.0000 C28 0.139(8) 0.187(8) 0.084(6) 0.0000 0.063(7) 0.0000 C29 0.140(9) 0.207(9) 0.096(7) 0.0000 0.073(7) 0.0000 C30 0.128(8) 0.253(9) 0.105(8) 0.0000 0.075(6) 0.0000 C31 0.114(7) 0.234(8) 0.096(7) 0.0000 0.064(6) 0.0000 C32 0.042(5) 0.041(5) 0.030(5) 0.0000 -0.009(4) 0.0000 C33 0.075(7) 0.036(5) 0.050(6) 0.0000 0.011(6) 0.0000 C34 0.064(5) 0.056(5) 0.111(7) 0.011(4) 0.006(5) -0.017(5) C35 0.105(8) 0.051(6) 0.213(13) 0.036(5) 0.005(8) 0.006(7) C36 0.104(11) 0.044(7) 0.201(17) 0.0000 -0.009(11) 0.0000 C37 0.052(4) 0.032(4) 0.065(5) 0.008(3) 0.024(4) 0.005(3) C38 0.038(4) 0.036(4) 0.053(4) -0.001(3) 0.018(3) 0.004(3) C39 0.042(4) 0.040(4) 0.056(5) 0.011(3) 0.009(4) 0.009(3) C40 0.031(4) 0.056(4) 0.055(5) 0.006(3) 0.006(3) 0.004(3) C41 0.032(5) 0.033(5) 0.061(6) 0.0000 0.021(5) 0.0000 C42 0.029(5) 0.034(5) 0.055(6) 0.0000 0.015(4) 0.0000 C43 0.040(4) 0.024(3) 0.055(4) 0.009(3) 0.020(3) 0.005(3) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ru1 Ru1 2.2811(6) yes . 7_455 Ru1 O1 2.058(5) yes . . Ru1 O2 2.065(5) yes . 7_455 Ru1 O3 2.054(4) yes . . Ru1 O4 2.061(4) yes . 7_455 Ru1 N1 2.292(4) yes . . Ru2 Ru2 2.2799(8) yes . 2_656 Ru2 O5 2.073(7) yes . . Ru2 O6 2.052(7) yes . 2_656 Ru2 O7 2.062(4) yes . . Ru2 O7 2.062(4) yes . 4_565 Ru2 N4 2.315(6) yes . . O1 C1 1.250(7) yes . . O2 C1 1.271(6) yes . . O3 C8 1.266(7) yes . . O4 C8 1.277(6) yes . . O5 C25 1.269(13) yes . . O6 C25 1.257(11) yes . . O7 C32 1.259(6) yes . . N1 C15 1.336(6) yes . . N1 C19 1.325(6) yes . . N2 C20 1.338(6) yes . . N2 C20 1.338(6) yes . 4_565 N3 C20 1.341(6) yes . . N3 C21 1.354(5) yes . . N4 C24 1.331(6) yes . . N4 C24 1.331(6) yes . 4_565 C1 C2 1.495(11) yes . . C2 C3 1.401(10) yes . . C2 C7 1.370(10) yes . . C3 C4 1.376(16) yes . . C4 C5 1.411(15) yes . . C5 C6 1.381(11) yes . . C6 C7 1.389(12) yes . . C8 C9 1.480(8) yes . . C9 C10 1.381(8) yes . . C9 C14 1.394(8) yes . . C10 C11 1.384(9) yes . . C11 C12 1.375(11) yes . . C12 C13 1.394(10) yes . . C13 C14 1.376(9) yes . . C15 C16 1.366(7) yes . . C16 C17 1.404(7) yes . . C17 C18 1.347(7) yes . . C17 C20 1.478(7) yes . . C18 C19 1.358(7) yes . . C21 C22 1.457(10) yes . . C22 C23 1.378(6) yes . . C22 C23 1.378(6) yes . 4_565 C23 C24 1.393(8) yes . . C25 C26 1.52(2) yes . . C26 C27 1.266(18) yes . . C26 C31 1.36(3) yes . . C27 C28 1.38(3) yes . . C28 C29 1.20(3) yes . . C29 C30 1.38(2) yes . . C30 C31 1.43(3) yes . . C32 C33 1.484(13) yes . . C33 C34 1.384(9) yes . . C33 C34 1.384(9) yes . 2_656 C34 C35 1.431(11) yes . . C35 C36 1.358(12) yes . . C37 C37 1.364(7) yes . 2_555 C37 C38 1.401(8) yes . . C38 C39 1.423(7) yes . . C38 C43 1.422(7) yes . . C39 C40 1.347(8) yes . . C40 C41 1.417(7) yes . . C41 C42 1.403(10) yes . . C42 C43 1.415(6) yes . . C42 C43 1.415(6) yes . 4_565 C43 C43 1.433(7) yes . 2_555 C3 H3 0.950 no . . C4 H4 0.950 no . . C5 H5 0.950 no . . C6 H6 0.950 no . . C7 H7 0.950 no . . C10 H10 0.950 no . . C11 H11 0.950 no . . C12 H12 0.950 no . . C13 H13 0.950 no . . C14 H14 0.950 no . . C15 H15 0.950 no . . C16 H16 0.950 no . . C18 H18 0.950 no . . C19 H19 0.950 no . . C23 H23 0.950 no . . C24 H24 0.950 no . . C27 H27 0.951 no . . C28 H28 0.950 no . . C29 H29 0.949 no . . C30 H30 0.950 no . . C31 H31 0.950 no . . C34 H34 0.950 no . . C35 H35 0.950 no . . C36 H36 0.950 no . . C37 H37 0.950 no . . C39 H39 0.950 no . . C40 H40 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Ru1 Ru1 O1 88.21(9) yes 7_455 . . Ru1 Ru1 O2 90.41(10) yes 7_455 . 7_455 Ru1 Ru1 O3 89.13(9) yes 7_455 . . Ru1 Ru1 O4 89.66(9) yes 7_455 . 7_455 Ru1 Ru1 N1 173.27(14) yes 7_455 . . O1 Ru1 O2 178.48(13) yes . . 7_455 O1 Ru1 O3 90.30(16) yes . . . O1 Ru1 O4 89.35(16) yes . . 7_455 O1 Ru1 N1 85.41(16) yes . . . O2 Ru1 O3 90.31(16) yes 7_455 . . O2 Ru1 O4 90.01(16) yes 7_455 . 7_455 O2 Ru1 N1 96.00(16) yes 7_455 . . O3 Ru1 O4 178.75(14) yes . . 7_455 O3 Ru1 N1 88.78(14) yes . . . O4 Ru1 N1 92.39(14) yes 7_455 . . Ru2 Ru2 O5 89.35(14) yes 2_656 . . Ru2 Ru2 O6 90.29(14) yes 2_656 . 2_656 Ru2 Ru2 O7 89.12(10) yes 2_656 . . Ru2 Ru2 O7 89.12(10) yes 2_656 . 4_565 Ru2 Ru2 N4 179.9(3) yes 2_656 . . O5 Ru2 O6 179.6(2) yes . . 2_656 O5 Ru2 O7 90.88(14) yes . . . O5 Ru2 O7 90.88(14) yes . . 4_565 O5 Ru2 N4 90.6(3) yes . . . O6 Ru2 O7 89.11(14) yes 2_656 . . O6 Ru2 O7 89.11(14) yes 2_656 . 4_565 O6 Ru2 N4 89.8(3) yes 2_656 . . O7 Ru2 O7 177.49(16) yes . . 4_565 O7 Ru2 N4 90.88(10) yes . . . O7 Ru2 N4 90.88(10) yes 4_565 . . Ru1 O1 C1 120.0(4) yes . . . Ru1 O2 C1 116.8(4) yes 7_455 . . Ru1 O3 C8 119.5(3) yes . . . Ru1 O4 C8 118.4(4) yes 7_455 . . Ru2 O5 C25 116.2(7) yes . . . Ru2 O6 C25 116.6(8) yes 2_656 . . Ru2 O7 C32 119.1(4) yes . . . Ru1 N1 C15 113.3(3) yes . . . Ru1 N1 C19 128.7(4) yes . . . C15 N1 C19 118.0(4) yes . . . C20 N2 C20 116.0(5) yes . . 4_565 C20 N3 C21 114.6(5) yes . . . Ru2 N4 C24 120.4(3) yes . . . Ru2 N4 C24 120.4(3) yes . . 4_565 C24 N4 C24 118.7(5) yes . . 4_565 O1 C1 O2 124.6(7) yes . . . O1 C1 C2 118.0(5) yes . . . O2 C1 C2 117.4(6) yes . . . C1 C2 C3 118.4(7) yes . . . C1 C2 C7 123.2(6) yes . . . C3 C2 C7 118.3(8) yes . . . C2 C3 C4 120.8(8) yes . . . C3 C4 C5 119.1(8) yes . . . C4 C5 C6 121.1(10) yes . . . C5 C6 C7 117.7(8) yes . . . C2 C7 C6 123.0(6) yes . . . O3 C8 O4 123.3(5) yes . . . O3 C8 C9 117.6(5) yes . . . O4 C8 C9 119.1(5) yes . . . C8 C9 C10 119.7(5) yes . . . C8 C9 C14 119.8(5) yes . . . C10 C9 C14 120.4(6) yes . . . C9 C10 C11 119.9(6) yes . . . C10 C11 C12 119.8(6) yes . . . C11 C12 C13 120.5(7) yes . . . C12 C13 C14 119.9(7) yes . . . C9 C14 C13 119.4(6) yes . . . N1 C15 C16 122.0(5) yes . . . C15 C16 C17 119.2(5) yes . . . C16 C17 C18 117.6(5) yes . . . C16 C17 C20 117.9(4) yes . . . C18 C17 C20 124.5(5) yes . . . C17 C18 C19 120.2(5) yes . . . N1 C19 C18 123.1(5) yes . . . N2 C20 N3 124.8(5) yes . . . N2 C20 C17 115.9(4) yes . . . N3 C20 C17 119.3(4) yes . . . N3 C21 N3 125.1(6) yes . . 4_565 N3 C21 C22 117.3(3) yes . . . N3 C21 C22 117.3(3) yes 4_565 . . C21 C22 C23 121.2(4) yes . . . C21 C22 C23 121.2(4) yes . . 4_565 C23 C22 C23 117.6(6) yes . . 4_565 C22 C23 C24 119.8(5) yes . . . N4 C24 C23 122.0(5) yes . . . O5 C25 O6 127.6(12) yes . . . O5 C25 C26 114.3(9) yes . . . O6 C25 C26 118.1(11) yes . . . C25 C26 C27 128.6(14) yes . . . C25 C26 C31 117.9(12) yes . . . C27 C26 C31 113.5(17) yes . . . C26 C27 C28 123.9(15) yes . . . C27 C28 C29 124.1(15) yes . . . C28 C29 C30 120(2) yes . . . C29 C30 C31 114.3(17) yes . . . C26 C31 C30 124.3(14) yes . . . O7 C32 O7 123.4(8) yes . . 2_656 O7 C32 C33 118.3(4) yes . . . O7 C32 C33 118.3(4) yes 2_656 . . C32 C33 C34 119.9(5) yes . . . C32 C33 C34 119.9(5) yes . . 2_656 C34 C33 C34 120.2(8) yes . . 2_656 C33 C34 C35 119.1(8) yes . . . C34 C35 C36 120.4(9) yes . . . C35 C36 C35 120.7(10) yes . . 2_656 C37 C37 C38 122.0(5) yes 2_555 . . C37 C38 C39 123.4(5) yes . . . C37 C38 C43 118.1(5) yes . . . C39 C38 C43 118.4(5) yes . . . C38 C39 C40 120.3(5) yes . . . C39 C40 C41 122.7(5) yes . . . C40 C41 C40 123.0(6) yes . . 4_565 C40 C41 C42 118.5(4) yes . . . C40 C41 C42 118.5(4) yes 4_565 . . C41 C42 C43 119.7(3) yes . . . C41 C42 C43 119.7(3) yes . . 4_565 C43 C42 C43 120.4(6) yes . . 4_565 C38 C43 C42 120.4(5) yes . . . C38 C43 C43 119.9(5) yes . . 2_555 C42 C43 C43 119.7(5) yes . . 2_555 C2 C3 H3 119.595 no . . . C4 C3 H3 119.602 no . . . C3 C4 H4 120.476 no . . . C5 C4 H4 120.473 no . . . C4 C5 H5 119.457 no . . . C6 C5 H5 119.485 no . . . C5 C6 H6 121.135 no . . . C7 C6 H6 121.138 no . . . C2 C7 H7 118.515 no . . . C6 C7 H7 118.529 no . . . C9 C10 H10 120.071 no . . . C11 C10 H10 120.052 no . . . C10 C11 H11 120.117 no . . . C12 C11 H11 120.086 no . . . C11 C12 H12 119.737 no . . . C13 C12 H12 119.733 no . . . C12 C13 H13 120.068 no . . . C14 C13 H13 120.076 no . . . C9 C14 H14 120.292 no . . . C13 C14 H14 120.291 no . . . N1 C15 H15 119.008 no . . . C16 C15 H15 119.039 no . . . C15 C16 H16 120.407 no . . . C17 C16 H16 120.406 no . . . C17 C18 H18 119.911 no . . . C19 C18 H18 119.919 no . . . N1 C19 H19 118.465 no . . . C18 C19 H19 118.458 no . . . C22 C23 H23 120.120 no . . . C24 C23 H23 120.071 no . . . N4 C24 H24 119.013 no . . . C23 C24 H24 119.027 no . . . C26 C27 H27 118.030 no . . . C28 C27 H27 118.038 no . . . C27 C28 H28 118.047 no . . . C29 C28 H28 117.852 no . . . C28 C29 H29 120.099 no . . . C30 C29 H29 120.014 no . . . C29 C30 H30 122.846 no . . . C31 C30 H30 122.894 no . . . C26 C31 H31 117.917 no . . . C30 C31 H31 117.750 no . . . C33 C34 H34 120.449 no . . . C35 C34 H34 120.454 no . . . C34 C35 H35 119.775 no . . . C36 C35 H35 119.781 no . . . C35 C36 H36 119.647 no . . . C35 C36 H36 119.647 no 2_656 . . C37 C37 H37 119.002 no 2_555 . . C38 C37 H37 119.000 no . . . C38 C39 H39 119.865 no . . . C40 C39 H39 119.852 no . . . C39 C40 H40 118.673 no . . . C41 C40 H40 118.660 no . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O1 C3 2.752(11) no . . O1 C8 3.562(6) no . . O1 C8 3.500(8) no . 7_455 O1 C15 3.188(7) no . . O2 C7 2.831(9) no . . O2 C8 3.573(6) no . . O2 C8 3.548(8) no . 7_455 O3 C1 3.546(7) no . . O3 C1 3.513(8) no . 7_455 O3 C10 2.770(7) no . . O3 C19 3.322(7) no . . O4 C1 3.547(7) no . . O4 C1 3.531(9) no . 7_455 O4 C14 2.813(7) no . . O4 C15 3.134(6) no . 7_455 O5 C27 2.84(2) no . . O5 C31 3.57(2) no . . O5 C32 3.551(8) no . . O6 C27 3.580(16) no . . O6 C31 2.75(3) no . . O6 C32 3.549(8) no . . O7 C24 3.157(6) no . 4_565 O7 C25 3.546(12) no . . O7 C25 3.480(11) no . 2_656 O7 C34 3.591(8) no . . O7 C34 2.792(8) no . 2_656 N1 C17 2.759(6) no . . N2 N3 2.375(6) no . 4_565 N2 C16 2.720(6) no . . N2 C16 2.720(6) no . 4_565 N2 C17 2.388(5) no . 4_565 N2 C21 2.673(8) no . . N3 C18 2.898(7) no . . N3 C20 2.693(6) no . 4_565 N3 C23 2.793(7) no . 4_565 N4 C22 2.784(9) no . . N4 C23 2.383(7) no . 4_565 C2 C5 2.779(14) no . . C3 C6 2.792(12) no . . C4 C7 2.755(11) no . . C9 C12 2.755(9) no . . C10 C13 2.771(10) no . . C11 C14 2.777(9) no . . C15 C18 2.694(7) no . . C16 C19 2.681(7) no . . C22 C24 2.397(8) no . 4_565 C23 C24 2.709(7) no . 4_565 C26 C29 2.76(3) no . . C27 C30 2.67(3) no . . C28 C31 2.58(2) no . . C33 C35 2.427(12) no . 2_656 C33 C36 2.793(15) no . . C34 C35 2.777(12) no . 2_656 C37 C43 2.796(7) no . 2_555 C38 C38 2.849(7) no . 2_555 C38 C41 2.830(6) no . . C39 C42 2.815(7) no . . C40 C43 2.780(7) no . . C42 C42 2.838(10) no . 2_555 Ru2 O7 3.050(4) no . 3_666 Ru2 C32 2.892(8) no . 3_666 O3 C6 3.446(9) no . 8_555 O5 C12 3.532(8) no . 5_555 O5 C12 3.532(8) no . 8_555 O5 C32 3.551(8) no . 3_666 O6 O7 2.886(7) no . 3_666 O6 C32 3.549(8) no . 3_666 O7 C12 3.348(10) no . 8_555 N1 C37 3.491(9) no . 2_555 N3 C39 3.570(9) no . . N3 C40 3.525(10) no . . N3 C41 3.586(12) no . . C5 C10 3.545(15) no . 8_455 C6 O3 3.446(9) no . 8_455 C7 C7 3.468(10) no . 2_455 C10 C5 3.545(15) no . 8_555 C11 C34 3.491(13) no . 7_556 C12 O5 3.532(8) no . 5_445 C12 O7 3.348(10) no . 8_455 C15 C37 3.519(10) no . 2_555 C15 C38 3.468(10) no . 2_555 C15 C39 3.566(10) no . 2_555 C16 C38 3.377(10) no . 2_555 C16 C43 3.527(10) no . 2_555 C17 C38 3.556(10) no . . C18 C37 3.364(11) no . . C19 C37 3.552(10) no . . C19 C37 3.571(10) no . 2_555 C20 C43 3.386(10) no . . C21 C40 3.599(12) no . . C21 C40 3.599(12) no . 4_565 C21 C41 3.352(14) no . . C22 C40 3.556(11) no . . C22 C40 3.556(11) no . 4_565 C22 C41 3.589(13) no . . C23 C40 3.520(10) no . 4_565 C25 O7 3.480(11) no . 3_666 C34 C11 3.491(13) no . 7_556 C37 N1 3.491(9) no . 2_555 C37 C15 3.519(10) no . 2_555 C37 C18 3.364(11) no . . C37 C19 3.552(10) no . . C37 C19 3.571(10) no . 2_555 C38 C15 3.468(10) no . 2_555 C38 C16 3.377(10) no . 2_555 C38 C17 3.556(10) no . . C39 N3 3.570(9) no . . C39 C15 3.566(10) no . 2_555 C40 N3 3.525(10) no . . C40 C21 3.599(12) no . . C40 C22 3.556(11) no . . C40 C23 3.520(10) no . 4_565 C41 N3 3.586(12) no . . C41 N3 3.586(12) no . 4_565 C41 C21 3.352(14) no . . C41 C22 3.589(13) no . . C42 C43 2.464(8) no . 3_565 C43 C16 3.527(10) no . 2_555 C43 C20 3.386(10) no . . C43 C43 2.844(7) no . 3_565 Ru1 H15 2.9876 no . . Ru1 H19 3.3485 no . . Ru2 H24 3.1866 no . . Ru2 H24 3.1866 no . 4_565 O1 H3 2.4333 no . . O1 H15 2.8782 no . . O2 H7 2.5307 no . . O2 H19 3.5848 no . 7_455 O3 H10 2.4814 no . . O3 H19 2.8898 no . . O4 H14 2.5232 no . . O4 H15 2.5471 no . 7_455 O5 H27 2.5540 no . . O6 H31 2.3815 no . . O7 H24 2.5419 no . 4_565 O7 H34 2.5127 no . 2_656 N1 H16 3.2143 no . . N1 H18 3.2039 no . . N2 H16 2.3763 no . . N2 H16 2.3763 no . 4_565 N3 H18 2.6137 no . . N3 H23 2.4727 no . 4_565 N4 H23 3.2299 no . . N4 H23 3.2299 no . 4_565 N4 H24 1.9754 no . 4_565 C1 H3 2.6282 no . . C1 H7 2.6760 no . . C2 H4 3.2741 no . . C2 H6 3.2778 no . . C3 H5 3.2564 no . . C3 H7 3.2340 no . . C4 H6 3.2940 no . . C5 H3 3.2622 no . . C5 H7 3.2259 no . . C6 H4 3.2855 no . . C7 H3 3.2362 no . . C7 H5 3.2335 no . . C8 H10 2.6318 no . . C8 H14 2.6514 no . . C9 H11 3.2513 no . . C9 H13 3.2532 no . . C10 H12 3.2445 no . . C10 H14 3.2647 no . . C11 H13 3.2589 no . . C12 H10 3.2450 no . . C12 H14 3.2579 no . . C13 H11 3.2617 no . . C14 H10 3.2657 no . . C14 H12 3.2522 no . . C15 H19 3.1368 no . . C16 H18 3.2219 no . . C17 H15 3.2457 no . . C17 H19 3.1920 no . . C18 H16 3.2164 no . . C19 H15 3.1386 no . . C20 H16 2.6221 no . . C20 H18 2.6880 no . . C21 H23 2.6435 no . . C21 H23 2.6435 no . 4_565 C22 H23 2.0286 no . 4_565 C22 H24 3.2480 no . . C22 H24 3.2480 no . 4_565 C23 H23 3.2230 no . 4_565 C24 H24 3.1468 no . 4_565 C25 H27 2.6829 no . . C25 H31 2.5645 no . . C26 H28 3.1607 no . . C26 H30 3.3197 no . . C27 H29 3.1444 no . . C27 H31 3.0540 no . . C28 H30 3.1031 no . . C28 H31 3.5294 no . . C29 H27 3.1043 no . . C29 H31 3.2160 no . . C30 H28 3.1005 no . . C31 H27 3.0708 no . . C31 H28 3.5289 no . . C31 H29 3.2354 no . . C32 H34 2.6469 no . . C32 H34 2.6469 no . 2_656 C33 H34 2.0376 no . 2_656 C33 H35 3.2824 no . . C33 H35 3.2824 no . 2_656 C34 H34 3.2598 no . 2_656 C34 H36 3.2804 no . . C35 H35 3.2147 no . 2_656 C36 H34 3.2745 no . . C36 H34 3.2745 no . 2_656 C36 H35 2.0070 no . 2_656 C37 H39 2.6904 no . . C38 H37 3.2664 no . 2_555 C38 H40 3.2566 no . . C39 H37 2.6701 no . . C40 H40 2.6685 no . 4_565 C41 H39 3.2786 no . . C41 H39 3.2786 no . 4_565 C41 H40 2.0498 no . 4_565 C42 H40 3.2754 no . . C42 H40 3.2754 no . 4_565 C43 H37 3.2801 no . . C43 H39 3.3044 no . . H3 H4 2.3267 no . . H4 H5 2.3601 no . . H5 H6 2.3401 no . . H6 H7 2.3346 no . . H10 H11 2.3368 no . . H10 H19 3.4010 no . . H11 H12 2.3223 no . . H12 H13 2.3408 no . . H13 H14 2.3317 no . . H14 H15 3.1264 no . 7_455 H15 H16 2.3076 no . . H16 H16 2.8637 no . 4_565 H18 H19 2.2846 no . . H18 H23 3.4482 no . 4_565 H23 H24 2.3306 no . . H27 H28 2.2747 no . . H28 H29 2.1243 no . . H29 H30 2.3721 no . . H30 H31 2.3841 no . . H34 H35 2.3845 no . . H35 H36 2.2999 no . . H37 H37 2.2855 no . 2_555 H37 H39 2.5256 no . . H39 H40 2.2760 no . . H40 H40 2.4965 no . 4_565 O2 H6 3.0464 no . 2_455 O2 H7 3.2689 no . 2_455 O2 H37 3.2298 no . 8_455 O3 H6 2.4990 no . 8_555 O4 H39 3.0493 no . 8_455 O5 H12 2.7730 no . 5_555 O5 H12 2.7730 no . 8_555 O5 H13 3.2224 no . 5_555 O5 H13 3.2224 no . 8_555 O7 H12 2.6140 no . 8_555 N1 H37 3.3112 no . 2_555 C1 H6 3.4819 no . 2_455 C6 H19 3.4373 no . 8_455 C7 H7 3.1107 no . 2_455 C8 H6 2.8666 no . 8_555 C9 H5 2.9646 no . 8_555 C9 H6 3.0123 no . 8_555 C10 H5 2.9138 no . 8_555 C10 H6 3.0897 no . 8_555 C11 H5 2.9930 no . 8_555 C12 H5 3.1286 no . 8_555 C12 H24 3.5185 no . 5_445 C13 H5 3.2045 no . 8_555 C13 H24 3.5571 no . 5_445 C13 H27 3.2625 no . 5_445 C13 H40 3.0958 no . 8_455 C14 H5 3.1476 no . 8_555 C14 H39 3.0715 no . 8_455 C14 H40 3.0095 no . 8_455 C15 H37 3.5587 no . 2_555 C18 H37 3.4704 no . . C19 H37 3.5031 no . . C19 H37 3.5517 no . 2_555 C22 H40 3.4367 no . . C22 H40 3.4367 no . 4_565 C23 H40 3.1950 no . 4_565 C24 H13 3.5039 no . 5_555 C25 H12 3.1588 no . 5_555 C25 H12 3.1588 no . 8_555 C26 H12 3.5616 no . 5_555 C26 H12 3.5616 no . 8_555 C27 H13 3.4391 no . 5_555 C27 H13 3.4391 no . 8_555 C28 H4 3.1863 no . 1_655 C28 H4 3.1863 no . 4_665 C29 H4 2.9822 no . 1_655 C29 H4 2.9822 no . 4_665 C30 H4 3.4107 no . 1_655 C30 H4 3.4107 no . 4_665 C32 H12 2.9272 no . 7_556 C32 H12 2.9272 no . 8_555 C33 H11 3.0368 no . 7_556 C33 H11 3.0368 no . 8_555 C33 H12 3.2606 no . 7_556 C33 H12 3.2606 no . 8_555 C34 H11 3.0109 no . 7_556 C34 H11 3.2947 no . 8_555 C34 H12 3.5679 no . 7_556 C35 H11 3.2650 no . 7_556 C35 H11 3.5107 no . 8_555 C36 H11 3.5005 no . 7_556 C36 H11 3.5005 no . 8_555 C37 H18 3.5561 no . . C38 H16 3.5385 no . 2_555 C39 H14 2.9693 no . 8_555 C39 H15 3.3814 no . 2_555 C40 H13 3.5860 no . 8_555 C40 H14 2.9638 no . 8_555 C40 H23 3.4397 no . 4_565 C43 H16 3.4722 no . 2_555 H4 C28 3.1863 no . 1_455 H4 C29 2.9822 no . 1_455 H4 C30 3.4107 no . 1_455 H4 H28 3.3983 no . 1_455 H4 H29 3.0622 no . 1_455 H5 C9 2.9646 no . 8_455 H5 C10 2.9138 no . 8_455 H5 C11 2.9930 no . 8_455 H5 C12 3.1286 no . 8_455 H5 C13 3.2045 no . 8_455 H5 C14 3.1476 no . 8_455 H5 H10 3.3894 no . 8_455 H5 H11 3.4963 no . 8_455 H6 O2 3.0464 no . 2_455 H6 O3 2.4990 no . 8_455 H6 C1 3.4819 no . 2_455 H6 C8 2.8666 no . 8_455 H6 C9 3.0123 no . 8_455 H6 C10 3.0897 no . 8_455 H6 H10 2.9987 no . 8_455 H6 H19 2.8706 no . 8_455 H7 O2 3.2689 no . 2_455 H7 C7 3.1107 no . 2_455 H7 H7 2.5300 no . 2_455 H7 H19 3.1992 no . 8_455 H7 H37 3.0191 no . 8_455 H10 H5 3.3894 no . 8_555 H10 H6 2.9987 no . 8_555 H11 C33 3.0368 no . 7_556 H11 C34 3.0109 no . 7_556 H11 C34 3.2947 no . 8_455 H11 C35 3.2650 no . 7_556 H11 C35 3.5107 no . 8_455 H11 C36 3.5005 no . 7_556 H11 H5 3.4963 no . 8_555 H11 H34 3.3848 no . 7_556 H12 O5 2.7730 no . 5_445 H12 O7 2.6140 no . 8_455 H12 C25 3.1588 no . 5_445 H12 C26 3.5616 no . 5_445 H12 C32 2.9272 no . 7_556 H12 C33 3.2606 no . 7_556 H12 C34 3.5679 no . 7_556 H12 H24 3.3418 no . 5_445 H12 H27 3.4100 no . 5_445 H12 H34 3.5135 no . 7_556 H13 O5 3.2224 no . 5_445 H13 C24 3.5039 no . 5_445 H13 C27 3.4391 no . 5_445 H13 C40 3.5860 no . 8_455 H13 H13 3.4486 no . 4_555 H13 H24 3.4159 no . 5_445 H13 H27 2.6687 no . 5_445 H13 H40 2.6554 no . 8_455 H14 C39 2.9693 no . 8_455 H14 C40 2.9638 no . 8_455 H14 H39 2.4959 no . 8_455 H14 H40 2.4670 no . 8_455 H15 C39 3.3814 no . 2_555 H15 H39 3.3019 no . 2_555 H16 C38 3.5385 no . 2_555 H16 C43 3.4722 no . 2_555 H18 C37 3.5561 no . . H18 H37 3.5104 no . . H19 C6 3.4373 no . 8_555 H19 H6 2.8706 no . 8_555 H19 H7 3.1992 no . 8_555 H19 H37 3.5650 no . . H23 C40 3.4397 no . 4_565 H23 H39 3.5980 no . 4_565 H23 H40 3.2415 no . 4_565 H24 C12 3.5185 no . 5_555 H24 C13 3.5571 no . 5_555 H24 H12 3.3418 no . 5_555 H24 H13 3.4159 no . 5_555 H24 H34 3.0022 no . 3_666 H27 C13 3.2625 no . 5_555 H27 C13 3.2625 no . 8_555 H27 H12 3.4100 no . 5_555 H27 H12 3.4100 no . 8_555 H27 H13 2.6687 no . 5_555 H27 H13 2.6687 no . 8_555 H28 H4 3.3983 no . 1_655 H28 H4 3.3983 no . 4_665 H29 H4 3.0622 no . 1_655 H29 H4 3.0622 no . 4_665 H34 H11 3.3848 no . 7_556 H34 H12 3.5135 no . 7_556 H34 H24 3.0022 no . 3_666 H37 O2 3.2298 no . 8_555 H37 N1 3.3112 no . 2_555 H37 C15 3.5587 no . 2_555 H37 C18 3.4704 no . . H37 C19 3.5031 no . . H37 C19 3.5517 no . 2_555 H37 H7 3.0191 no . 8_555 H37 H18 3.5104 no . . H37 H19 3.5650 no . . H39 O4 3.0493 no . 8_555 H39 C14 3.0715 no . 8_555 H39 H14 2.4959 no . 8_555 H39 H15 3.3019 no . 2_555 H39 H23 3.5980 no . 4_565 H40 C13 3.0958 no . 8_555 H40 C14 3.0095 no . 8_555 H40 C22 3.4367 no . . H40 C23 3.1950 no . 4_565 H40 H13 2.6554 no . 8_555 H40 H14 2.4670 no . 8_555 H40 H23 3.2415 no . 4_565 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.034 -0.005 -0.035 5144 1837 ' ' _platon_squeeze_details ; ; #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment '- cif_Ru-2_miyasaka.cif' data_Ruo-FPhTPTcoronene _database_code_depnum_ccdc_archive 'CCDC 878051' #TrackingRef '- cif_Ru-2_miyasaka.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C144 H84 F12 N12 O24 Ru6' _chemical_formula_moiety 'C144 H84 F12 N12 O24 Ru6' _chemical_formula_weight 3200.71 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/m 1' _symmetry_space_group_name_Hall '-C 2y' _symmetry_Int_Tables_number 12 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,-Z 3 -X,-Y,-Z 4 +X,-Y,+Z 5 1/2+X,1/2+Y,+Z 6 1/2-X,1/2+Y,-Z 7 1/2-X,1/2-Y,-Z 8 1/2+X,1/2-Y,+Z #------------------------------------------------------------------------------ _cell_length_a 19.738(3) _cell_length_b 28.910(4) _cell_length_c 19.689(3) _cell_angle_alpha 90.0000 _cell_angle_beta 112.663(3) _cell_angle_gamma 90.0000 _cell_volume 10368(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 12054 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 30.99 _cell_measurement_temperature 97 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour darkpurple _exptl_crystal_size_max 0.256 _exptl_crystal_size_mid 0.237 _exptl_crystal_size_min 0.046 _exptl_crystal_density_diffrn 1.025 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3192.00 _exptl_absorpt_coefficient_mu 0.486 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.772 _exptl_absorpt_correction_T_max 0.978 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 97 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_reflns_number 35267 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 9296 _reflns_number_gt 7532 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.2226 _refine_ls_number_restraints 190 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 9266 _refine_ls_number_parameters 496 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1470P)^2^+15.5936P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 1.440 _refine_diff_density_min -1.540 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ru Ru -1.2594 0.8363 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.0171 0.0103 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru -0.207818(17) 0.278430(11) 0.02643(2) 0.04514(18) Uani 1.0 8 d . . . Ru2 Ru 0.44291(3) 0.5000 0.45436(3) 0.0537(2) Uani 1.0 4 d . . . F1 F -0.3070(8) 0.3746(6) 0.1434(13) 0.234(11) Uani 0.5000 8 d . . . F2 F -0.4585(5) 0.2395(3) 0.0801(6) 0.101(3) Uani 0.5000 8 d . . . F3 F -0.0872(6) 0.2283(3) 0.2616(4) 0.218(5) Uani 1.0 8 d . . . F4 F 0.5047(11) 0.5000 0.2457(7) 0.311(11) Uani 1.0 4 d . . . F5 F 0.3682(6) 0.3505(3) 0.4534(8) 0.141(5) Uani 0.5000 8 d . . . O1 O -0.27815(17) 0.30545(11) 0.0705(2) 0.0564(9) Uani 1.0 8 d . . . O2 O -0.36087(17) 0.24955(12) 0.0188(2) 0.0554(8) Uani 1.0 8 d . . . O3 O -0.15939(17) 0.23755(12) 0.11816(19) 0.0531(8) Uani 1.0 8 d . . . O4 O -0.24251(18) 0.18153(12) 0.0662(2) 0.0570(9) Uani 1.0 8 d . . . O5 O 0.4914(4) 0.5000 0.3766(3) 0.0787(17) Uani 1.0 4 d . . . O6 O 0.6017(3) 0.5000 0.4684(4) 0.0875(19) Uani 1.0 4 d . . . O7 O 0.4439(2) 0.42843(13) 0.4558(2) 0.0699(11) Uani 1.0 8 d . . . N1 N -0.1322(2) 0.33855(13) 0.0843(3) 0.0537(10) Uani 1.0 8 d . . . N2 N -0.0476(3) 0.5000 0.1495(3) 0.0515(14) Uani 1.0 4 d . . . N3 N 0.0605(2) 0.45920(13) 0.2176(3) 0.0540(10) Uani 1.0 8 d . . . N4 N 0.3243(3) 0.5000 0.3693(4) 0.0688(18) Uani 1.0 4 d . . . C1 C -0.3399(3) 0.28562(17) 0.0574(4) 0.0569(12) Uani 1.0 8 d . . . C2 C -0.3876(3) 0.3069(2) 0.0923(4) 0.0730(14) Uani 1.0 8 d . . . C3 C -0.3726(5) 0.3511(3) 0.1243(7) 0.117(3) Uani 1.0 8 d . . . C4 C -0.4123(5) 0.3697(4) 0.1620(7) 0.134(3) Uani 1.0 8 d . . . C5 C -0.4750(5) 0.3477(4) 0.1590(7) 0.121(3) Uani 1.0 8 d . . . C6 C -0.4938(4) 0.3051(3) 0.1252(5) 0.0862(18) Uani 1.0 8 d . . . C7 C -0.4475(4) 0.2853(3) 0.0948(4) 0.0719(15) Uani 1.0 8 d . . . C8 C -0.1854(3) 0.19755(18) 0.1179(3) 0.0566(12) Uani 1.0 8 d . . . C9 C -0.1469(4) 0.1661(3) 0.1790(4) 0.0751(15) Uani 1.0 8 d . . . C10 C -0.1003(5) 0.1829(4) 0.2468(5) 0.107(3) Uani 1.0 8 d . . . C11 C -0.0588(7) 0.1535(5) 0.3050(6) 0.135(3) Uani 1.0 8 d . . . C12 C -0.0682(6) 0.1077(4) 0.2930(6) 0.131(3) Uani 1.0 8 d . . . C13 C -0.1149(5) 0.0878(4) 0.2254(6) 0.123(3) Uani 1.0 8 d . . . C14 C -0.1547(4) 0.1180(3) 0.1684(6) 0.104(2) Uani 1.0 8 d . . . C15 C -0.1622(3) 0.38060(16) 0.0673(3) 0.0580(13) Uani 1.0 8 d . . . C16 C -0.1242(3) 0.42060(16) 0.0962(4) 0.0604(14) Uani 1.0 8 d . . . C17 C -0.0509(3) 0.41758(16) 0.1454(3) 0.0500(11) Uani 1.0 8 d . . . C18 C -0.0209(3) 0.37431(16) 0.1646(3) 0.0545(12) Uani 1.0 8 d . . . C19 C -0.0617(3) 0.33563(16) 0.1330(3) 0.0534(12) Uani 1.0 8 d . . . C20 C -0.0089(3) 0.46097(15) 0.1735(3) 0.0498(11) Uani 1.0 8 d . . . C21 C 0.0931(4) 0.5000 0.2386(4) 0.0547(17) Uani 1.0 4 d . . . C22 C 0.1731(4) 0.5000 0.2855(4) 0.0549(17) Uani 1.0 4 d . . . C23 C 0.2127(3) 0.54134(18) 0.3071(4) 0.0690(16) Uani 1.0 8 d . . . C24 C 0.2861(3) 0.54014(19) 0.3491(4) 0.0734(17) Uani 1.0 8 d . . . C25 C 0.5618(7) 0.5000 0.4050(7) 0.111(4) Uani 1.0 4 d . . . C26 C 0.5997(9) 0.5000 0.3488(9) 0.147(4) Uani 1.0 4 d . . . C27 C 0.5740(12) 0.5000 0.2811(11) 0.156(4) Uani 1.0 4 d . . . C28 C 0.6108(12) 0.5000 0.2334(10) 0.165(5) Uani 1.0 4 d . . . C29 C 0.6860(12) 0.4644(9) 0.2688(11) 0.132(5) Uani 0.5000 8 d . . . C30 C 0.7190(12) 0.4652(9) 0.3333(12) 0.139(5) Uani 0.5000 8 d . . . C31 C 0.6762(13) 0.4650(10) 0.3829(12) 0.147(5) Uani 0.5000 8 d . . . C32 C 0.5000 0.4083(3) 0.5000 0.0647(19) Uani 1.0 4 d . . . C33 C 0.5000 0.3573(3) 0.5000 0.075(2) Uani 1.0 4 d . . . C34 C 0.4350(5) 0.3320(3) 0.4770(5) 0.102(3) Uani 1.0 8 d . . . C35 C 0.4366(6) 0.2839(3) 0.4793(7) 0.127(3) Uani 1.0 8 d . . . C36 C 0.5000 0.2608(4) 0.5000 0.138(5) Uani 1.0 4 d . . . C37 C 0.0358(3) 0.37279(16) 0.0235(4) 0.0618(13) Uani 1.0 8 d . . . C38 C 0.0743(3) 0.41500(18) 0.0502(4) 0.0596(13) Uani 1.0 8 d . . . C39 C 0.1489(3) 0.4162(2) 0.0998(4) 0.0680(15) Uani 1.0 8 d . . . C40 C 0.1847(3) 0.4567(3) 0.1236(4) 0.0705(16) Uani 1.0 8 d . . . C41 C 0.1492(4) 0.5000 0.0985(4) 0.0599(18) Uani 1.0 4 d . . . C42 C 0.0744(3) 0.5000 0.0500(4) 0.0499(15) Uani 1.0 4 d . . . C43 C 0.0374(3) 0.45749(16) 0.0252(3) 0.0527(12) Uani 1.0 8 d . . . H4 H -0.3963 0.3973 0.1898 0.1607 Uiso 1.0 8 calc R . . H5 H -0.5057 0.3619 0.1802 0.1451 Uiso 1.0 8 calc R . . H6 H -0.5371 0.2896 0.1228 0.1034 Uiso 1.0 8 calc R . . H11 H -0.0257 0.1654 0.3507 0.1617 Uiso 1.0 8 calc R . . H12 H -0.0418 0.0874 0.3323 0.1570 Uiso 1.0 8 calc R . . H13 H -0.1190 0.0552 0.2189 0.1479 Uiso 1.0 8 calc R . . H14 H -0.1871 0.1060 0.1225 0.1243 Uiso 1.0 8 calc R . . H15 H -0.2118 0.3830 0.0337 0.0696 Uiso 1.0 8 calc R . . H16 H -0.1474 0.4499 0.0829 0.0725 Uiso 1.0 8 calc R . . H18 H 0.0280 0.3710 0.1997 0.0653 Uiso 1.0 8 calc R . . H19 H -0.0397 0.3060 0.1457 0.0641 Uiso 1.0 8 calc R . . H23 H 0.1884 0.5702 0.2924 0.0827 Uiso 1.0 8 calc R . . H24 H 0.3115 0.5686 0.3649 0.0880 Uiso 1.0 8 calc R . . H35 H 0.3919 0.2672 0.4660 0.1527 Uiso 1.0 8 calc R . . H36 H 0.5000 0.2280 0.5000 0.1661 Uiso 1.0 4 calc R . . H37 H 0.0607 0.3442 0.0388 0.0742 Uiso 1.0 8 calc R . . H39 H 0.1743 0.3879 0.1166 0.0816 Uiso 1.0 8 calc R . . H40 H 0.2343 0.4562 0.1577 0.0846 Uiso 1.0 8 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru1 0.0326(3) 0.0323(3) 0.0658(3) -0.00596(12) 0.01370(19) 0.00136(14) Ru2 0.0417(4) 0.0444(4) 0.0518(4) 0.0000 -0.0076(3) 0.0000 F1 0.137(10) 0.168(12) 0.45(3) -0.084(10) 0.176(15) -0.191(16) F2 0.104(6) 0.050(4) 0.203(9) -0.032(4) 0.117(7) -0.043(5) F3 0.338(12) 0.152(7) 0.081(4) 0.079(7) -0.009(5) -0.007(4) F4 0.291(19) 0.55(4) 0.120(9) 0.0000 0.107(12) 0.0000 F5 0.087(7) 0.066(5) 0.233(13) -0.001(5) 0.021(7) 0.020(7) O1 0.0410(17) 0.0432(18) 0.084(3) -0.0072(14) 0.0226(16) -0.0043(16) O2 0.0376(17) 0.0470(19) 0.077(3) -0.0072(14) 0.0166(15) -0.0001(17) O3 0.0417(17) 0.0484(19) 0.064(2) -0.0033(15) 0.0141(15) 0.0017(16) O4 0.0497(19) 0.0460(18) 0.073(3) -0.0008(15) 0.0213(17) 0.0129(16) O5 0.094(5) 0.072(4) 0.054(3) 0.0000 0.010(3) 0.0000 O6 0.062(4) 0.120(6) 0.074(4) 0.0000 0.019(3) 0.0000 O7 0.062(3) 0.049(2) 0.074(3) 0.0023(17) -0.0015(19) 0.0014(17) N1 0.037(2) 0.038(2) 0.076(3) -0.0072(16) 0.0110(19) -0.0005(18) N2 0.039(3) 0.029(3) 0.069(4) 0.0000 0.002(3) 0.0000 N3 0.038(2) 0.036(2) 0.068(3) -0.0003(16) -0.0023(18) 0.0016(18) N4 0.050(4) 0.050(4) 0.074(4) 0.0000 -0.012(3) 0.0000 C1 0.044(3) 0.046(3) 0.082(4) 0.000(2) 0.026(3) 0.008(3) C2 0.056(3) 0.062(3) 0.111(4) -0.005(3) 0.044(3) -0.012(3) C3 0.090(4) 0.079(4) 0.203(7) -0.013(4) 0.080(5) -0.046(5) C4 0.098(5) 0.102(5) 0.221(7) -0.021(4) 0.083(5) -0.064(5) C5 0.082(4) 0.104(5) 0.193(7) -0.003(4) 0.072(5) -0.045(5) C6 0.066(4) 0.076(4) 0.130(5) -0.004(3) 0.052(4) -0.020(4) C7 0.048(3) 0.071(4) 0.101(4) -0.002(3) 0.033(3) -0.007(3) C8 0.044(3) 0.054(3) 0.071(3) 0.005(3) 0.021(3) 0.015(3) C9 0.060(3) 0.077(4) 0.086(4) 0.016(3) 0.027(3) 0.038(3) C10 0.118(5) 0.116(5) 0.079(4) 0.032(5) 0.027(4) 0.032(4) C11 0.141(6) 0.157(6) 0.089(5) 0.031(6) 0.025(4) 0.048(5) C12 0.110(5) 0.146(6) 0.132(5) 0.024(5) 0.042(4) 0.083(5) C13 0.079(5) 0.107(5) 0.165(6) 0.006(4) 0.027(4) 0.082(5) C14 0.062(4) 0.084(4) 0.155(5) 0.007(3) 0.030(4) 0.068(4) C15 0.031(3) 0.039(3) 0.082(4) -0.0007(18) -0.002(3) 0.001(3) C16 0.040(3) 0.030(3) 0.088(4) -0.0003(18) -0.001(3) 0.001(3) C17 0.031(2) 0.040(3) 0.066(3) -0.0026(18) 0.005(2) 0.000(2) C18 0.037(3) 0.038(3) 0.071(3) 0.0015(19) 0.001(2) 0.002(3) C19 0.037(3) 0.038(3) 0.076(4) 0.0021(18) 0.011(3) 0.001(3) C20 0.038(3) 0.031(3) 0.067(3) 0.0030(17) 0.005(2) 0.003(2) C21 0.037(4) 0.044(4) 0.063(4) 0.0000 -0.003(3) 0.0000 C22 0.037(4) 0.042(4) 0.067(5) 0.0000 -0.001(3) 0.0000 C23 0.049(3) 0.045(3) 0.079(4) 0.002(3) -0.013(3) 0.002(3) C24 0.054(3) 0.048(3) 0.081(4) 0.004(3) -0.014(3) 0.002(3) C25 0.084(7) 0.157(10) 0.095(7) 0.0000 0.039(6) 0.0000 C26 0.132(8) 0.207(10) 0.112(7) 0.0000 0.059(6) 0.0000 C27 0.156(9) 0.213(11) 0.116(7) 0.0000 0.070(7) 0.0000 C28 0.174(10) 0.218(13) 0.123(8) 0.0000 0.078(8) 0.0000 C29 0.124(10) 0.193(14) 0.101(8) -0.027(8) 0.067(8) -0.026(10) C30 0.125(9) 0.209(14) 0.105(8) -0.018(8) 0.069(7) -0.025(9) C31 0.122(10) 0.222(15) 0.120(9) -0.002(9) 0.071(8) -0.025(10) C32 0.064(5) 0.052(4) 0.056(4) 0.0000 -0.001(4) 0.0000 C33 0.090(5) 0.046(4) 0.073(5) 0.0000 0.013(4) 0.0000 C34 0.104(5) 0.054(4) 0.122(5) -0.013(3) 0.012(4) 0.012(4) C35 0.131(7) 0.063(4) 0.157(7) -0.019(4) 0.021(6) 0.006(4) C36 0.150(9) 0.056(6) 0.168(9) 0.0000 0.015(8) 0.0000 C37 0.068(3) 0.031(3) 0.084(4) 0.002(3) 0.026(3) 0.002(3) C38 0.051(3) 0.048(3) 0.077(4) 0.013(3) 0.023(3) 0.006(3) C39 0.059(4) 0.054(4) 0.083(4) 0.015(3) 0.018(3) 0.005(3) C40 0.038(3) 0.076(4) 0.086(4) 0.012(3) 0.012(3) 0.003(3) C41 0.035(4) 0.058(5) 0.080(5) 0.0000 0.015(4) 0.0000 C42 0.037(3) 0.045(4) 0.063(4) 0.0000 0.015(3) 0.0000 C43 0.041(3) 0.040(3) 0.076(4) 0.0041(19) 0.022(3) 0.002(3) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ru1 Ru1 2.2853(5) yes . 7_455 Ru1 O1 2.054(5) yes . . Ru1 O2 2.054(5) yes . 7_455 Ru1 O3 2.060(4) yes . . Ru1 O4 2.062(4) yes . 7_455 Ru1 N1 2.288(4) yes . . Ru2 Ru2 2.2777(8) yes . 2_656 Ru2 O5 2.095(8) yes . . Ru2 O6 2.030(9) yes . 2_656 Ru2 O7 2.069(4) yes . . Ru2 O7 2.069(4) yes . 4_565 Ru2 N4 2.294(6) yes . . F1 C3 1.380(17) yes . . F2 C7 1.356(10) yes . . F3 C10 1.348(13) yes . . F4 C27 1.27(3) yes . . F5 C34 1.329(13) yes . . O1 C1 1.280(7) yes . . O2 C1 1.263(7) yes . . O3 C8 1.265(7) yes . . O4 C8 1.279(6) yes . . O5 C25 1.282(15) yes . . O6 C25 1.192(14) yes . . O7 C32 1.258(6) yes . . N1 C15 1.337(6) yes . . N1 C19 1.354(6) yes . . N2 C20 1.343(5) yes . . N2 C20 1.343(5) yes . 4_565 N3 C20 1.310(6) yes . . N3 C21 1.331(5) yes . . N4 C24 1.358(6) yes . . N4 C24 1.358(6) yes . 4_565 C1 C2 1.495(11) yes . . C2 C3 1.404(11) yes . . C2 C7 1.356(10) yes . . C3 C4 1.379(19) yes . . C4 C5 1.373(15) yes . . C5 C6 1.381(12) yes . . C6 C7 1.393(12) yes . . C8 C9 1.467(8) yes . . C9 C10 1.384(10) yes . . C9 C14 1.406(10) yes . . C10 C11 1.408(14) yes . . C11 C12 1.345(17) yes . . C12 C13 1.416(14) yes . . C13 C14 1.399(13) yes . . C15 C16 1.377(7) yes . . C16 C17 1.399(6) yes . . C17 C18 1.374(7) yes . . C17 C20 1.488(7) yes . . C18 C19 1.379(7) yes . . C21 C22 1.491(10) yes . . C22 C23 1.401(7) yes . . C22 C23 1.401(7) yes . 4_565 C23 C24 1.364(8) yes . . C25 C26 1.56(3) yes . . C26 C27 1.23(3) yes . . C26 C31 1.72(3) yes . . C26 C31 1.72(3) yes . 4_565 C27 C28 1.39(4) yes . . C28 C29 1.72(3) yes . . C28 C29 1.72(3) yes . 4_565 C29 C30 1.18(3) yes . . C30 C30 2.01(4) yes . 4_565 C30 C31 1.52(4) yes . . C32 C33 1.474(13) yes . . C33 C34 1.393(10) yes . . C33 C34 1.393(10) yes . 2_656 C34 C35 1.392(11) yes . . C35 C36 1.336(12) yes . . C37 C37 1.360(7) yes . 2_555 C37 C38 1.427(7) yes . . C38 C39 1.419(7) yes . . C38 C43 1.417(7) yes . . C39 C40 1.354(9) yes . . C40 C41 1.428(7) yes . . C41 C42 1.416(9) yes . . C42 C43 1.417(6) yes . . C42 C43 1.417(6) yes . 4_565 C43 C43 1.425(6) yes . 2_555 C4 H4 0.950 no . . C5 H5 0.950 no . . C6 H6 0.950 no . . C11 H11 0.950 no . . C12 H12 0.950 no . . C13 H13 0.950 no . . C14 H14 0.950 no . . C15 H15 0.950 no . . C16 H16 0.950 no . . C18 H18 0.950 no . . C19 H19 0.950 no . . C23 H23 0.950 no . . C24 H24 0.950 no . . C35 H35 0.950 no . . C36 H36 0.949 no . . C37 H37 0.950 no . . C39 H39 0.950 no . . C40 H40 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Ru1 Ru1 O1 88.48(9) yes 7_455 . . Ru1 Ru1 O2 90.35(9) yes 7_455 . 7_455 Ru1 Ru1 O3 89.84(9) yes 7_455 . . Ru1 Ru1 O4 89.21(10) yes 7_455 . 7_455 Ru1 Ru1 N1 173.76(13) yes 7_455 . . O1 Ru1 O2 178.82(13) yes . . 7_455 O1 Ru1 O3 90.50(15) yes . . . O1 Ru1 O4 89.53(16) yes . . 7_455 O1 Ru1 N1 85.29(15) yes . . . O2 Ru1 O3 89.63(15) yes 7_455 . . O2 Ru1 O4 90.33(16) yes 7_455 . 7_455 O2 Ru1 N1 95.88(16) yes 7_455 . . O3 Ru1 O4 179.05(13) yes . . 7_455 O3 Ru1 N1 90.33(14) yes . . . O4 Ru1 N1 90.62(14) yes 7_455 . . Ru2 Ru2 O5 89.13(17) yes 2_656 . . Ru2 Ru2 O6 89.53(15) yes 2_656 . 2_656 Ru2 Ru2 O7 89.33(9) yes 2_656 . . Ru2 Ru2 O7 89.33(9) yes 2_656 . 4_565 Ru2 Ru2 N4 175.6(3) yes 2_656 . . O5 Ru2 O6 178.7(3) yes . . 2_656 O5 Ru2 O7 90.32(14) yes . . . O5 Ru2 O7 90.32(14) yes . . 4_565 O5 Ru2 N4 95.3(3) yes . . . O6 Ru2 O7 89.67(14) yes 2_656 . . O6 Ru2 O7 89.67(14) yes 2_656 . 4_565 O6 Ru2 N4 86.1(3) yes 2_656 . . O7 Ru2 O7 178.52(14) yes . . 4_565 O7 Ru2 N4 90.64(9) yes . . . O7 Ru2 N4 90.64(9) yes 4_565 . . Ru1 O1 C1 119.4(4) yes . . . Ru1 O2 C1 117.9(4) yes 7_455 . . Ru1 O3 C8 118.1(3) yes . . . Ru1 O4 C8 118.3(4) yes 7_455 . . Ru2 O5 C25 113.9(8) yes . . . Ru2 O6 C25 118.8(9) yes 2_656 . . Ru2 O7 C32 118.2(5) yes . . . Ru1 N1 C15 115.2(3) yes . . . Ru1 N1 C19 126.9(3) yes . . . C15 N1 C19 118.0(4) yes . . . C20 N2 C20 114.4(5) yes . . 4_565 C20 N3 C21 115.3(5) yes . . . Ru2 N4 C24 120.6(3) yes . . . Ru2 N4 C24 120.6(3) yes . . 4_565 C24 N4 C24 117.5(5) yes . . 4_565 O1 C1 O2 123.9(6) yes . . . O1 C1 C2 116.2(5) yes . . . O2 C1 C2 119.9(5) yes . . . C1 C2 C3 121.3(7) yes . . . C1 C2 C7 122.7(6) yes . . . C3 C2 C7 116.0(8) yes . . . F1 C3 C2 125.7(12) yes . . . F1 C3 C4 109.1(12) yes . . . C2 C3 C4 122.1(9) yes . . . C3 C4 C5 119.1(10) yes . . . C4 C5 C6 120.3(11) yes . . . C5 C6 C7 118.3(8) yes . . . F2 C7 C2 120.8(8) yes . . . F2 C7 C6 114.5(8) yes . . . C2 C7 C6 123.6(7) yes . . . O3 C8 O4 124.5(5) yes . . . O3 C8 C9 118.8(5) yes . . . O4 C8 C9 116.6(5) yes . . . C8 C9 C10 121.0(7) yes . . . C8 C9 C14 119.9(6) yes . . . C10 C9 C14 119.0(7) yes . . . F3 C10 C9 123.4(8) yes . . . F3 C10 C11 114.2(8) yes . . . C9 C10 C11 122.3(10) yes . . . C10 C11 C12 117.0(9) yes . . . C11 C12 C13 124.1(10) yes . . . C12 C13 C14 117.5(9) yes . . . C9 C14 C13 120.1(8) yes . . . N1 C15 C16 122.8(4) yes . . . C15 C16 C17 119.1(5) yes . . . C16 C17 C18 118.0(4) yes . . . C16 C17 C20 119.0(4) yes . . . C18 C17 C20 123.1(4) yes . . . C17 C18 C19 119.9(4) yes . . . N1 C19 C18 122.1(5) yes . . . N2 C20 N3 125.0(4) yes . . . N2 C20 C17 114.7(4) yes . . . N3 C20 C17 120.3(4) yes . . . N3 C21 N3 124.8(6) yes . . 4_565 N3 C21 C22 117.5(3) yes . . . N3 C21 C22 117.5(3) yes 4_565 . . C21 C22 C23 121.4(3) yes . . . C21 C22 C23 121.4(3) yes . . 4_565 C23 C22 C23 117.1(6) yes . . 4_565 C22 C23 C24 120.0(5) yes . . . N4 C24 C23 122.7(5) yes . . . O5 C25 O6 128.6(15) yes . . . O5 C25 C26 115.3(11) yes . . . O6 C25 C26 116.1(12) yes . . . C25 C26 C27 131.3(18) yes . . . C25 C26 C31 108.2(13) yes . . . C25 C26 C31 108.2(13) yes . . 4_565 C27 C26 C31 110.8(17) yes . . . C27 C26 C31 110.8(17) yes . . 4_565 C31 C26 C31 71.8(14) yes . . 4_565 F4 C27 C26 120(3) yes . . . F4 C27 C28 111.1(18) yes . . . C26 C27 C28 129(2) yes . . . C27 C28 C29 108.7(14) yes . . . C27 C28 C29 108.7(14) yes . . 4_565 C29 C28 C29 73.6(14) yes . . 4_565 C28 C29 C30 117(3) yes . . . C29 C30 C30 91(2) yes . . 4_565 C29 C30 C31 118(3) yes . . . C30 C30 C31 90.2(18) yes 4_565 . . C26 C31 C30 111.7(18) yes . . . O7 C32 O7 124.9(8) yes . . 2_656 O7 C32 C33 117.6(4) yes . . . O7 C32 C33 117.6(4) yes 2_656 . . C32 C33 C34 121.7(5) yes . . . C32 C33 C34 121.7(5) yes . . 2_656 C34 C33 C34 116.7(8) yes . . 2_656 F5 C34 C33 124.6(8) yes . . . F5 C34 C35 115.0(9) yes . . . C33 C34 C35 120.5(8) yes . . . C34 C35 C36 121.1(10) yes . . . C35 C36 C35 120.0(11) yes . . 2_656 C37 C37 C38 121.2(5) yes 2_555 . . C37 C38 C39 122.5(5) yes . . . C37 C38 C43 118.9(5) yes . . . C39 C38 C43 118.5(5) yes . . . C38 C39 C40 121.6(5) yes . . . C39 C40 C41 121.2(5) yes . . . C40 C41 C40 122.7(6) yes . . 4_565 C40 C41 C42 118.6(4) yes . . . C40 C41 C42 118.6(4) yes 4_565 . . C41 C42 C43 119.9(3) yes . . . C41 C42 C43 119.9(3) yes . . 4_565 C43 C42 C43 120.3(5) yes . . 4_565 C38 C43 C42 120.2(4) yes . . . C38 C43 C43 119.9(5) yes . . 2_555 C42 C43 C43 119.9(4) yes . . 2_555 C3 C4 H4 120.463 no . . . C5 C4 H4 120.480 no . . . C4 C5 H5 119.854 no . . . C6 C5 H5 119.858 no . . . C5 C6 H6 120.869 no . . . C7 C6 H6 120.874 no . . . C10 C11 H11 121.513 no . . . C12 C11 H11 121.513 no . . . C11 C12 H12 117.959 no . . . C13 C12 H12 117.970 no . . . C12 C13 H13 121.262 no . . . C14 C13 H13 121.252 no . . . C9 C14 H14 119.916 no . . . C13 C14 H14 119.941 no . . . N1 C15 H15 118.583 no . . . C16 C15 H15 118.576 no . . . C15 C16 H16 120.435 no . . . C17 C16 H16 120.428 no . . . C17 C18 H18 120.031 no . . . C19 C18 H18 120.038 no . . . N1 C19 H19 118.956 no . . . C18 C19 H19 118.944 no . . . C22 C23 H23 120.015 no . . . C24 C23 H23 119.998 no . . . N4 C24 H24 118.666 no . . . C23 C24 H24 118.659 no . . . C34 C35 H35 119.471 no . . . C36 C35 H35 119.406 no . . . C35 C36 H36 119.982 no . . . C35 C36 H36 119.982 no 2_656 . . C37 C37 H37 119.423 no 2_555 . . C38 C37 H37 119.412 no . . . C38 C39 H39 119.197 no . . . C40 C39 H39 119.220 no . . . C39 C40 H40 119.425 no . . . C41 C40 H40 119.421 no . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 F1 O1 2.65(2) no . . F1 C1 3.010(19) no . . F1 C5 3.53(2) no . . F2 O2 2.653(13) no . . F2 C1 2.874(12) no . . F2 C3 3.592(11) no . . F2 C5 3.563(14) no . . F3 O3 2.640(7) no . . F3 C8 2.885(8) no . . F3 C12 3.537(15) no . . F4 O5 2.689(19) no . . F4 C25 2.895(19) no . . F4 C29 3.58(4) no . . F4 C29 3.58(4) no . 4_565 F4 C31 3.57(3) no . . F4 C31 3.57(3) no . 4_565 F5 O7 2.693(11) no . . F5 C32 2.926(11) no . . F5 C36 3.536(13) no . . O1 C3 2.803(13) no . . O1 C8 3.554(6) no . . O1 C8 3.496(7) no . 7_455 O1 C15 3.175(7) no . . O2 C7 2.864(9) no . . O2 C8 3.585(6) no . . O2 C8 3.509(8) no . 7_455 O3 C1 3.573(6) no . . O3 C1 3.516(8) no . 7_455 O3 C10 2.828(10) no . . O3 C14 3.587(9) no . . O3 C19 3.378(6) no . . O4 C1 3.539(7) no . . O4 C1 3.539(9) no . 7_455 O4 C10 3.583(8) no . . O4 C14 2.782(9) no . . O4 C15 3.140(6) no . 7_455 O5 C27 2.93(3) no . . O5 C32 3.556(8) no . . O6 C27 3.51(3) no . . O6 C31 2.82(3) no . . O6 C31 2.82(3) no . 4_565 O6 C32 3.522(9) no . . O7 C24 3.145(7) no . 4_565 O7 C25 3.535(14) no . . O7 C25 3.470(13) no . 2_656 O7 C34 2.834(8) no . . O7 C34 3.578(9) no . 2_656 N1 C17 2.784(6) no . . N2 N3 2.353(6) no . 4_565 N2 C16 2.726(6) no . . N2 C16 2.726(6) no . 4_565 N2 C17 2.384(5) no . 4_565 N2 C21 2.652(9) no . . N3 C18 2.898(6) no . . N3 C20 2.653(6) no . 4_565 N3 C23 2.837(6) no . 4_565 N4 C22 2.799(9) no . . N4 C23 2.388(7) no . 4_565 C2 C5 2.800(15) no . . C3 C6 2.743(13) no . . C4 C7 2.733(12) no . . C9 C12 2.759(12) no . . C10 C13 2.779(15) no . . C11 C14 2.818(13) no . . C15 C18 2.714(6) no . . C16 C19 2.719(7) no . . C20 C22 3.596(8) no . . C22 C24 2.395(8) no . 4_565 C23 C24 2.722(8) no . 4_565 C26 C29 2.92(4) no . . C26 C29 2.92(4) no . 4_565 C26 C30 2.69(4) no . 4_565 C27 C30 2.83(3) no . . C27 C30 2.83(3) no . 4_565 C28 C30 2.49(3) no . 4_565 C28 C31 2.90(3) no . . C28 C31 2.90(3) no . 4_565 C29 C31 3.09(4) no . 4_565 C33 C35 2.417(12) no . 2_656 C33 C36 2.790(15) no . . C34 C35 2.724(14) no . 2_656 C37 C43 2.817(7) no . 2_555 C38 C38 2.837(7) no . 2_555 C38 C41 2.836(6) no . . C39 C42 2.808(7) no . . C40 C43 2.806(7) no . . C42 C42 2.837(8) no . 2_555 Ru2 O7 3.059(4) no . 3_666 Ru2 C32 2.885(8) no . 3_666 F2 F2 2.940(14) no . 2_455 F2 O2 3.353(9) no . 2_455 F2 C7 3.484(12) no . 2_455 F2 C19 3.404(12) no . 8_455 F2 C37 3.420(9) no . 8_455 F4 C13 3.383(18) no . 5_555 F4 C13 3.383(18) no . 8_555 O2 F2 3.353(9) no . 2_455 O2 C6 3.547(7) no . 2_455 O3 C6 3.446(9) no . 8_555 O5 C12 3.506(12) no . 5_555 O5 C12 3.506(12) no . 8_555 O5 C32 3.556(8) no . 3_666 O6 O7 2.890(8) no . 3_666 O6 C32 3.522(9) no . 3_666 O7 C12 3.291(13) no . 8_555 N1 C37 3.495(9) no . 2_555 N3 C40 3.597(9) no . . C4 C29 3.54(3) no . 1_455 C5 C9 3.586(13) no . 8_455 C6 O2 3.547(7) no . 2_455 C6 O3 3.446(9) no . 8_455 C7 F2 3.484(12) no . 2_455 C7 C7 3.504(10) no . 2_455 C9 C5 3.586(13) no . 8_555 C11 C33 3.571(11) no . 7_556 C11 C34 3.461(16) no . 8_455 C12 O5 3.506(12) no . 5_445 C12 O7 3.291(13) no . 8_455 C13 F4 3.383(18) no . 5_445 C15 C37 3.591(10) no . 2_555 C15 C38 3.526(10) no . 2_555 C15 C39 3.550(10) no . 2_555 C16 C38 3.390(10) no . 2_555 C16 C43 3.598(10) no . 2_555 C18 C37 3.373(10) no . . C19 F2 3.404(12) no . 8_555 C19 C37 3.565(10) no . . C19 C37 3.481(10) no . 2_555 C20 C43 3.379(9) no . . C21 C41 3.345(13) no . . C21 C42 3.587(12) no . . C22 C40 3.514(11) no . . C22 C40 3.514(11) no . 4_565 C22 C41 3.527(12) no . . C23 C40 3.438(10) no . 4_565 C25 O7 3.470(13) no . 3_666 C29 C4 3.54(3) no . 1_655 C33 C11 3.571(11) no . 7_556 C33 C11 3.571(11) no . 8_555 C34 C11 3.461(16) no . 8_555 C37 F2 3.420(9) no . 8_555 C37 N1 3.495(9) no . 2_555 C37 C15 3.591(10) no . 2_555 C37 C18 3.373(10) no . . C37 C19 3.565(10) no . . C37 C19 3.481(10) no . 2_555 C38 C15 3.526(10) no . 2_555 C38 C16 3.390(10) no . 2_555 C39 C15 3.550(10) no . 2_555 C40 N3 3.597(9) no . . C40 C22 3.514(11) no . . C40 C23 3.438(10) no . 4_565 C41 C21 3.345(13) no . . C41 C22 3.527(12) no . . C42 C21 3.587(12) no . . C42 C43 2.460(7) no . 3_565 C43 C16 3.598(10) no . 2_555 C43 C20 3.379(9) no . . C43 C43 2.841(7) no . 3_565 Ru1 H15 3.0284 no . . Ru1 H19 3.3404 no . . Ru2 H24 3.1999 no . . Ru2 H24 3.1999 no . 4_565 F1 H4 2.3692 no . . F1 H15 3.3740 no . . F2 H6 2.4945 no . . F3 H11 2.4935 no . . F3 H19 3.5750 no . . F5 H24 2.8739 no . 4_565 F5 H35 2.4496 no . . O1 H15 2.8275 no . . O2 H19 3.4675 no . 7_455 O3 H19 2.9674 no . . O4 H14 2.5028 no . . O4 H15 2.6065 no . 7_455 O7 H24 2.5364 no . 4_565 N1 H16 3.2317 no . . N1 H18 3.2408 no . . N2 H16 2.3892 no . . N2 H16 2.3892 no . 4_565 N3 H18 2.6188 no . . N3 H23 2.5297 no . 4_565 N4 H23 3.2367 no . . N4 H23 3.2367 no . 4_565 N4 H24 1.9956 no . 4_565 C2 H4 3.2860 no . . C2 H6 3.2702 no . . C3 H5 3.2302 no . . C4 H6 3.2503 no . . C6 H4 3.2470 no . . C7 H5 3.2439 no . . C8 H14 2.6504 no . . C9 H11 3.3035 no . . C9 H13 3.2953 no . . C10 H12 3.2070 no . . C10 H14 3.2621 no . . C11 H13 3.2863 no . . C12 H14 3.2726 no . . C13 H11 3.2975 no . . C14 H12 3.2578 no . . C15 H19 3.1631 no . . C16 H18 3.2416 no . . C17 H15 3.2462 no . . C17 H19 3.2336 no . . C18 H16 3.2405 no . . C19 H15 3.1636 no . . C20 H16 2.6460 no . . C20 H18 2.6954 no . . C21 H23 2.6915 no . . C21 H23 2.6915 no . 4_565 C22 H23 2.0487 no . 4_565 C22 H24 3.2465 no . . C22 H24 3.2465 no . 4_565 C23 H23 3.2565 no . 4_565 C24 H24 3.1783 no . 4_565 C33 H35 3.2693 no . . C33 H35 3.2693 no . 2_656 C34 H36 3.2325 no . . C35 H35 3.1686 no . 2_656 C36 H35 1.9831 no . 2_656 C37 H39 2.6757 no . . C38 H37 3.2815 no . 2_555 C38 H40 3.2738 no . . C39 H37 2.6816 no . . C40 H40 2.6926 no . 4_565 C41 H39 3.2780 no . . C41 H39 3.2780 no . 4_565 C41 H40 2.0674 no . 4_565 C42 H40 3.3019 no . . C42 H40 3.3019 no . 4_565 C43 H37 3.3046 no . . C43 H39 3.2937 no . . H4 H5 2.3297 no . . H5 H6 2.3419 no . . H11 H12 2.2872 no . . H12 H13 2.3550 no . . H13 H14 2.3661 no . . H14 H15 2.9686 no . 7_455 H15 H16 2.3122 no . . H16 H16 2.8980 no . 4_565 H18 H19 2.3142 no . . H18 H23 3.4339 no . 4_565 H23 H24 2.2952 no . . H35 H36 2.2764 no . . H37 H37 2.2932 no . 2_555 H37 H39 2.5142 no . . H39 H40 2.2849 no . . H40 H40 2.5325 no . 4_565 Ru2 H12 3.5795 no . 5_555 Ru2 H12 3.5795 no . 8_555 F2 H19 2.7501 no . 8_455 F2 H37 3.4295 no . 7_455 F2 H37 2.6259 no . 8_455 F3 H6 3.2855 no . 8_555 F4 H12 3.3672 no . 5_555 F4 H12 3.3672 no . 8_555 F4 H13 2.7917 no . 5_555 F4 H13 2.7917 no . 8_555 F5 H11 3.4583 no . 8_555 O2 H6 2.9733 no . 2_455 O2 H37 3.2186 no . 8_455 O3 H6 2.5057 no . 8_555 O4 H39 2.9937 no . 8_455 O5 H12 2.6711 no . 5_555 O5 H12 2.6711 no . 8_555 O5 H13 3.4232 no . 5_555 O5 H13 3.4232 no . 8_555 O7 H12 2.5948 no . 8_555 N1 H37 3.2443 no . 2_555 C1 H6 3.4433 no . 2_455 C6 H19 3.4017 no . 8_455 C7 H19 3.5619 no . 8_455 C8 H6 2.9151 no . 8_555 C9 H5 2.8939 no . 8_555 C9 H6 3.0679 no . 8_555 C10 H5 2.9615 no . 8_555 C10 H6 3.2401 no . 8_555 C11 H5 3.0533 no . 8_555 C12 H5 3.0564 no . 8_555 C12 H24 3.3950 no . 5_445 C13 H5 3.0058 no . 8_555 C13 H40 3.0332 no . 8_455 C14 H5 2.9197 no . 8_555 C14 H39 3.1315 no . 8_455 C14 H40 3.0140 no . 8_455 C15 H37 3.5628 no . 2_555 C15 H39 3.5411 no . 2_555 C18 H37 3.5459 no . . C19 H37 3.5774 no . . C19 H37 3.3976 no . 2_555 C22 H40 3.4268 no . . C22 H40 3.4268 no . 4_565 C23 H40 3.1320 no . 4_565 C24 H40 3.5071 no . 4_565 C25 H12 3.2187 no . 5_555 C25 H12 3.2187 no . 8_555 C28 H4 3.0787 no . 1_655 C28 H4 3.0787 no . 4_665 C29 H4 2.6230 no . 1_655 C30 H4 3.4734 no . 1_655 C32 H11 3.5063 no . 7_556 C32 H11 3.5063 no . 8_555 C32 H12 3.0826 no . 7_556 C32 H12 3.0826 no . 8_555 C33 H11 2.8607 no . 7_556 C33 H11 2.8607 no . 8_555 C33 H12 3.4703 no . 7_556 C33 H12 3.4703 no . 8_555 C34 H11 3.1692 no . 7_556 C34 H11 2.8779 no . 8_555 C35 H11 3.4503 no . 7_556 C35 H11 3.2514 no . 8_555 C36 H11 3.5074 no . 7_556 C36 H11 3.5074 no . 8_555 C37 H18 3.5330 no . . C38 H16 3.5896 no . 2_555 C39 H14 3.1572 no . 8_555 C39 H15 3.4468 no . 2_555 C39 H23 3.5871 no . 4_565 C40 H14 3.1172 no . 8_555 C40 H23 3.3856 no . 4_565 C43 H16 3.5865 no . 2_555 H4 C28 3.0787 no . 1_455 H4 C29 2.6230 no . 1_455 H4 C30 3.4734 no . 1_455 H5 C9 2.8939 no . 8_455 H5 C10 2.9615 no . 8_455 H5 C11 3.0533 no . 8_455 H5 C12 3.0564 no . 8_455 H5 C13 3.0058 no . 8_455 H5 C14 2.9197 no . 8_455 H5 H13 3.5567 no . 8_455 H5 H14 3.4426 no . 8_455 H6 F3 3.2855 no . 8_455 H6 O2 2.9733 no . 2_455 H6 O3 2.5057 no . 8_455 H6 C1 3.4433 no . 2_455 H6 C8 2.9151 no . 8_455 H6 C9 3.0679 no . 8_455 H6 C10 3.2401 no . 8_455 H6 H19 2.8040 no . 8_455 H11 F5 3.4583 no . 8_455 H11 C32 3.5063 no . 7_556 H11 C33 2.8607 no . 7_556 H11 C34 3.1692 no . 7_556 H11 C34 2.8779 no . 8_455 H11 C35 3.4503 no . 7_556 H11 C35 3.2514 no . 8_455 H11 C36 3.5074 no . 7_556 H12 Ru2 3.5795 no . 5_445 H12 F4 3.3672 no . 5_445 H12 O5 2.6711 no . 5_445 H12 O7 2.5948 no . 8_455 H12 C25 3.2187 no . 5_445 H12 C32 3.0826 no . 7_556 H12 C33 3.4703 no . 7_556 H12 H24 3.2456 no . 5_445 H13 F4 2.7917 no . 5_445 H13 O5 3.4232 no . 5_445 H13 H5 3.5567 no . 8_555 H13 H13 3.1923 no . 4_555 H13 H40 2.6940 no . 8_455 H14 C39 3.1572 no . 8_455 H14 C40 3.1172 no . 8_455 H14 H5 3.4426 no . 8_555 H14 H39 2.6985 no . 8_455 H14 H40 2.6342 no . 8_455 H15 C39 3.4468 no . 2_555 H15 H39 3.3188 no . 2_555 H16 C38 3.5896 no . 2_555 H16 C43 3.5865 no . 2_555 H18 C37 3.5330 no . . H18 H37 3.5558 no . . H19 F2 2.7501 no . 8_555 H19 C6 3.4017 no . 8_555 H19 C7 3.5619 no . 8_555 H19 H6 2.8040 no . 8_555 H19 H37 3.5770 no . . H23 C39 3.5871 no . 4_565 H23 C40 3.3856 no . 4_565 H23 H39 3.5749 no . 4_565 H23 H40 3.2080 no . 4_565 H24 C12 3.3950 no . 5_555 H24 H12 3.2456 no . 5_555 H37 F2 3.4295 no . 7_455 H37 F2 2.6259 no . 8_555 H37 O2 3.2186 no . 8_555 H37 N1 3.2443 no . 2_555 H37 C15 3.5628 no . 2_555 H37 C18 3.5459 no . . H37 C19 3.5774 no . . H37 C19 3.3976 no . 2_555 H37 H18 3.5558 no . . H37 H19 3.5770 no . . H39 O4 2.9937 no . 8_555 H39 C14 3.1315 no . 8_555 H39 C15 3.5411 no . 2_555 H39 H14 2.6985 no . 8_555 H39 H15 3.3188 no . 2_555 H39 H23 3.5749 no . 4_565 H40 C13 3.0332 no . 8_555 H40 C14 3.0140 no . 8_555 H40 C22 3.4268 no . . H40 C23 3.1320 no . 4_565 H40 C24 3.5071 no . 4_565 H40 H13 2.6940 no . 8_555 H40 H14 2.6342 no . 8_555 H40 H23 3.2080 no . 4_565 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.047 -0.008 -0.025 4778 831 ' ' _platon_squeeze_details ; ; #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment '- cif_Ru-3_miyasaka.cif' data_Rum-FPhTPTcoronene _database_code_depnum_ccdc_archive 'CCDC 878052' #TrackingRef '- cif_Ru-3_miyasaka.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C144 H84 F12 N12 O24 Ru6' _chemical_formula_moiety 'C144 H84 F12 N12 O24 Ru6' _chemical_formula_weight 3200.71 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/m 1' _symmetry_space_group_name_Hall '-C 2y' _symmetry_Int_Tables_number 12 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,-Z 3 -X,-Y,-Z 4 +X,-Y,+Z 5 1/2+X,1/2+Y,+Z 6 1/2-X,1/2+Y,-Z 7 1/2-X,1/2-Y,-Z 8 1/2+X,1/2-Y,+Z #------------------------------------------------------------------------------ _cell_length_a 19.732(3) _cell_length_b 28.950(3) _cell_length_c 20.193(3) _cell_angle_alpha 90.0000 _cell_angle_beta 113.269(2) _cell_angle_gamma 90.0000 _cell_volume 10597(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 13972 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 30.99 _cell_measurement_temperature 97 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour darkpurple _exptl_crystal_size_max 0.153 _exptl_crystal_size_mid 0.101 _exptl_crystal_size_min 0.036 _exptl_crystal_density_diffrn 1.003 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3192.00 _exptl_absorpt_coefficient_mu 0.475 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.846 _exptl_absorpt_correction_T_max 0.983 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 97 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_reflns_number 43834 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_theta_max 27.52 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_max 0.979 _diffrn_measured_fraction_theta_full 0.979 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 12204 _reflns_number_gt 9865 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.1985 _refine_ls_number_restraints 247 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 12204 _refine_ls_number_parameters 487 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1362P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.670 _refine_diff_density_min -1.620 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.0171 0.0103 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ru Ru -1.2594 0.8363 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru -0.208421(13) 0.278997(8) 0.024848(15) 0.03377(12) Uani 1.0 8 d . . . Ru2 Ru 0.442650(19) 0.5000 0.454407(19) 0.03479(13) Uani 1.0 4 d . . . F1 F -0.3845(4) 0.4038(3) 0.1982(5) 0.236(4) Uani 1.0 8 d . . . F2 F 0.0113(9) 0.1765(5) 0.3530(6) 0.114(6) Uani 0.2500 8 d . . . F3 F -0.12688(19) 0.04984(12) 0.2315(3) 0.0752(11) Uani 0.7500 8 d . . . F4 F 0.5471(4) 0.5000 0.1596(3) 0.155(3) Uani 1.0 4 d . . . F5 F 0.3758(7) 0.2624(4) 0.4263(10) 0.255(8) Uani 0.5000 8 d . . . O1 O -0.27883(13) 0.30563(8) 0.06789(14) 0.0417(6) Uani 1.0 8 d . . . O2 O -0.35984(12) 0.24844(8) 0.02081(14) 0.0401(6) Uani 1.0 8 d . . . O3 O -0.15655(12) 0.23893(8) 0.11550(13) 0.0385(5) Uani 1.0 8 d . . . O4 O -0.23819(12) 0.18124(8) 0.06637(14) 0.0398(6) Uani 1.0 8 d . . . O5 O 0.49103(19) 0.5000 0.38048(19) 0.0431(8) Uani 1.0 4 d . . . O6 O 0.60377(19) 0.5000 0.4703(2) 0.0458(9) Uani 1.0 4 d . . . O7 O 0.44343(12) 0.42860(9) 0.45557(13) 0.0426(6) Uani 1.0 8 d . . . N1 N -0.13275(14) 0.33868(9) 0.08136(17) 0.0382(7) Uani 1.0 8 d . . . N2 N -0.0475(2) 0.5000 0.1445(2) 0.0355(9) Uani 1.0 4 d . . . N3 N 0.06124(15) 0.45872(9) 0.21245(16) 0.0374(7) Uani 1.0 8 d . . . N4 N 0.3238(2) 0.5000 0.3688(2) 0.0383(9) Uani 1.0 4 d . . . C1 C -0.33932(19) 0.28486(12) 0.0578(2) 0.0403(8) Uani 1.0 8 d . . . C2 C -0.3870(3) 0.30546(15) 0.0909(3) 0.0566(10) Uani 1.0 8 d . . . C3 C -0.3656(4) 0.3471(3) 0.1264(5) 0.110(2) Uani 1.0 8 d . . . C4 C -0.4093(5) 0.3654(3) 0.1570(6) 0.134(3) Uani 1.0 8 d . . . C5 C -0.4747(4) 0.3456(3) 0.1524(5) 0.112(2) Uani 1.0 8 d . . . C6 C -0.4932(3) 0.3037(2) 0.1201(4) 0.0770(15) Uani 1.0 8 d . . . C7 C -0.4483(3) 0.28299(16) 0.0886(3) 0.0581(11) Uani 1.0 8 d . . . C8 C -0.18195(18) 0.19865(11) 0.11624(19) 0.0369(7) Uani 1.0 8 d . . . C9 C -0.1406(2) 0.16898(13) 0.1799(2) 0.0442(8) Uani 1.0 8 d . . . C10 C -0.0866(3) 0.18802(16) 0.2407(3) 0.0632(12) Uani 1.0 8 d . . . C11 C -0.0471(4) 0.1592(2) 0.2989(3) 0.0839(16) Uani 1.0 8 d . . . C12 C -0.0596(3) 0.11248(19) 0.2958(3) 0.0731(14) Uani 1.0 8 d . . . C13 C -0.1138(3) 0.09447(15) 0.2348(3) 0.0570(10) Uani 1.0 8 d . . . C14 C -0.1542(2) 0.12187(13) 0.1765(3) 0.0455(8) Uani 1.0 8 d . . . C15 C -0.16316(18) 0.38103(11) 0.0637(2) 0.0400(8) Uani 1.0 8 d . . . C16 C -0.12423(18) 0.42096(11) 0.0917(2) 0.0402(8) Uani 1.0 8 d . . . C17 C -0.05157(17) 0.41797(11) 0.14090(19) 0.0361(7) Uani 1.0 8 d . . . C18 C -0.02045(18) 0.37422(11) 0.1606(2) 0.0415(8) Uani 1.0 8 d . . . C19 C -0.06275(19) 0.33598(12) 0.1296(3) 0.0438(9) Uani 1.0 8 d . . . C20 C -0.00878(17) 0.46107(10) 0.16861(18) 0.0335(7) Uani 1.0 8 d . . . C21 C 0.0943(2) 0.5000 0.2330(3) 0.0356(10) Uani 1.0 4 d . . . C22 C 0.1739(2) 0.5000 0.2798(3) 0.0391(11) Uani 1.0 4 d . . . C23 C 0.21277(19) 0.54124(12) 0.3033(3) 0.0468(9) Uani 1.0 8 d . . . C24 C 0.2866(2) 0.53941(13) 0.3466(3) 0.0489(10) Uani 1.0 8 d . . . C25 C 0.5600(3) 0.5000 0.4039(3) 0.0405(11) Uani 1.0 4 d . . . C26 C 0.5953(3) 0.5000 0.3511(3) 0.0550(13) Uani 1.0 4 d . . . C27 C 0.5528(4) 0.5000 0.2779(4) 0.0678(16) Uani 1.0 4 d . . . C28 C 0.5895(5) 0.5000 0.2341(4) 0.087(2) Uani 1.0 4 d . . . C29 C 0.6598(6) 0.5000 0.2523(6) 0.102(3) Uani 1.0 4 d . . . C30 C 0.7034(5) 0.5000 0.3262(6) 0.103(3) Uani 1.0 4 d . . . C31 C 0.6731(4) 0.5000 0.3764(5) 0.090(3) Uani 1.0 4 d . . . C32 C 0.5000 0.40828(18) 0.5000 0.0440(12) Uani 1.0 4 d . . . C33 C 0.5000 0.3574(2) 0.5000 0.0687(19) Uani 1.0 4 d . . . C34 C 0.4364(4) 0.33300(19) 0.4649(5) 0.113(3) Uani 1.0 8 d . . . C35 C 0.4375(5) 0.2841(3) 0.4670(7) 0.167(4) Uani 1.0 8 d . . . C36 C 0.5000 0.2599(3) 0.5000 0.168(5) Uani 1.0 4 d . . . C37 C 0.0362(2) 0.37302(12) 0.0232(3) 0.0466(9) Uani 1.0 8 d . . . C38 C 0.07525(19) 0.41536(13) 0.0495(2) 0.0415(8) Uani 1.0 8 d . . . C39 C 0.14971(19) 0.41620(13) 0.0981(2) 0.0447(9) Uani 1.0 8 d . . . C40 C 0.1857(2) 0.45694(14) 0.1217(3) 0.0477(9) Uani 1.0 8 d . . . C41 C 0.1502(3) 0.5000 0.0978(3) 0.0403(11) Uani 1.0 4 d . . . C42 C 0.0746(3) 0.5000 0.0497(3) 0.0380(10) Uani 1.0 4 d . . . C43 C 0.03764(19) 0.45729(12) 0.0248(2) 0.0377(7) Uani 1.0 8 d . . . H3 H -0.3219 0.3623 0.1293 0.1317 Uiso 1.0 8 calc R . . H5 H -0.5058 0.3609 0.1713 0.1346 Uiso 1.0 8 calc R . . H6 H -0.5363 0.2884 0.1186 0.0924 Uiso 1.0 8 calc R . . H7 H -0.4609 0.2536 0.0661 0.0697 Uiso 1.0 8 calc R . . H10 H -0.0764 0.2202 0.2429 0.0758 Uiso 1.0 8 calc R . . H12 H -0.0314 0.0930 0.3349 0.0877 Uiso 1.0 8 calc R . . H14 H -0.1909 0.1086 0.1347 0.0546 Uiso 1.0 8 calc R . . H15 H -0.2132 0.3834 0.0309 0.0480 Uiso 1.0 8 calc R . . H16 H -0.1470 0.4503 0.0774 0.0482 Uiso 1.0 8 calc R . . H18 H 0.0289 0.3708 0.1948 0.0498 Uiso 1.0 8 calc R . . H19 H -0.0412 0.3063 0.1430 0.0525 Uiso 1.0 8 calc R . . H23 H 0.1885 0.5701 0.2894 0.0561 Uiso 1.0 8 calc R . . H24 H 0.3126 0.5677 0.3616 0.0587 Uiso 1.0 8 calc R . . H27 H 0.5004 0.5000 0.2594 0.0813 Uiso 1.0 4 calc R . . H29 H 0.6809 0.5000 0.2175 0.1218 Uiso 1.0 4 calc R . . H30 H 0.7556 0.5000 0.3419 0.1242 Uiso 1.0 4 calc R . . H31 H 0.7032 0.5000 0.4265 0.1084 Uiso 1.0 4 calc R . . H34 H 0.3915 0.3489 0.4392 0.1350 Uiso 1.0 8 calc R . . H36 H 0.5000 0.2271 0.5000 0.2018 Uiso 1.0 4 calc R . . H37 H 0.0612 0.3444 0.0383 0.0559 Uiso 1.0 8 calc R . . H39 H 0.1752 0.3879 0.1147 0.0537 Uiso 1.0 8 calc R . . H40 H 0.2357 0.4565 0.1550 0.0572 Uiso 1.0 8 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru1 0.02487(19) 0.02346(16) 0.04711(19) -0.00485(9) 0.00795(14) 0.00044(9) Ru2 0.0236(3) 0.0347(2) 0.0340(2) 0.0000 -0.00158(16) 0.0000 F1 0.218(6) 0.166(5) 0.428(10) -0.117(5) 0.240(7) -0.196(6) F2 0.165(11) 0.071(7) 0.039(6) -0.026(8) -0.032(6) 0.024(5) F3 0.061(2) 0.0509(19) 0.089(3) -0.0037(16) 0.0041(19) 0.0279(18) F4 0.193(6) 0.220(8) 0.052(3) 0.0000 0.047(4) 0.0000 F5 0.182(9) 0.081(6) 0.324(15) -0.049(7) -0.090(10) -0.009(8) O1 0.0322(13) 0.0304(12) 0.0587(15) -0.0075(10) 0.0138(11) -0.0055(11) O2 0.0277(12) 0.0296(11) 0.0583(15) -0.0048(9) 0.0119(11) -0.0029(10) O3 0.0294(12) 0.0313(12) 0.0458(14) -0.0042(10) 0.0053(10) 0.0014(10) O4 0.0284(12) 0.0317(12) 0.0522(14) -0.0039(10) 0.0083(11) 0.0064(10) O5 0.043(2) 0.0418(19) 0.0391(18) 0.0000 0.0106(16) 0.0000 O6 0.0349(19) 0.052(3) 0.043(2) 0.0000 0.0069(16) 0.0000 O7 0.0352(14) 0.0360(13) 0.0426(14) -0.0029(10) 0.0004(11) -0.0032(10) N1 0.0234(13) 0.0273(13) 0.0556(18) -0.0041(11) 0.0069(12) 0.0004(12) N2 0.0240(19) 0.0225(17) 0.050(3) 0.0000 0.0043(17) 0.0000 N3 0.0300(15) 0.0265(13) 0.0437(16) -0.0005(11) 0.0016(12) 0.0019(11) N4 0.0220(19) 0.040(2) 0.038(2) 0.0000 -0.0050(16) 0.0000 C1 0.0292(17) 0.0379(17) 0.052(2) 0.0009(13) 0.0134(15) -0.0005(14) C2 0.048(2) 0.047(2) 0.081(3) -0.0074(17) 0.032(2) -0.0133(19) C3 0.101(4) 0.075(4) 0.195(6) -0.039(3) 0.103(4) -0.060(4) C4 0.131(5) 0.093(4) 0.234(6) -0.041(4) 0.132(5) -0.085(4) C5 0.093(4) 0.085(4) 0.192(6) -0.013(3) 0.092(4) -0.055(4) C6 0.051(3) 0.074(3) 0.115(4) -0.009(3) 0.042(3) -0.034(3) C7 0.036(2) 0.056(3) 0.086(3) -0.0056(16) 0.028(2) -0.015(2) C8 0.0320(17) 0.0277(15) 0.0471(18) -0.0028(13) 0.0114(14) 0.0025(13) C9 0.0397(18) 0.0393(18) 0.0528(19) -0.0064(14) 0.0175(16) 0.0039(15) C10 0.071(3) 0.052(3) 0.047(2) -0.011(2) 0.0032(19) 0.0073(18) C11 0.097(4) 0.070(3) 0.054(3) -0.019(3) -0.004(3) 0.015(3) C12 0.070(3) 0.071(3) 0.061(3) -0.012(3) 0.007(3) 0.027(3) C13 0.049(3) 0.046(2) 0.068(3) -0.0061(17) 0.0142(19) 0.0174(18) C14 0.0362(18) 0.0395(18) 0.056(2) -0.0040(14) 0.0131(16) 0.0096(15) C15 0.0283(17) 0.0293(16) 0.051(2) -0.0003(13) 0.0039(15) 0.0011(14) C16 0.0305(18) 0.0246(15) 0.055(2) -0.0034(13) 0.0059(16) 0.0040(14) C17 0.0279(16) 0.0269(15) 0.0460(19) -0.0020(12) 0.0067(14) 0.0013(13) C18 0.0263(17) 0.0284(16) 0.057(2) -0.0011(13) 0.0023(15) 0.0021(14) C19 0.0345(18) 0.0261(16) 0.058(3) -0.0030(13) 0.0052(16) -0.0004(14) C20 0.0252(16) 0.0256(15) 0.0402(17) -0.0030(12) 0.0029(13) -0.0011(12) C21 0.025(3) 0.030(2) 0.037(3) 0.0000 -0.0029(18) 0.0000 C22 0.025(3) 0.030(3) 0.045(3) 0.0000 -0.005(2) 0.0000 C23 0.0275(18) 0.0343(18) 0.057(3) -0.0038(14) -0.0064(16) 0.0007(15) C24 0.0325(19) 0.042(2) 0.052(3) -0.0048(15) -0.0045(16) 0.0036(16) C25 0.035(3) 0.039(3) 0.045(3) 0.0000 0.012(2) 0.0000 C26 0.054(3) 0.064(4) 0.051(3) 0.0000 0.025(3) 0.0000 C27 0.076(4) 0.077(4) 0.053(3) 0.0000 0.029(3) 0.0000 C28 0.104(5) 0.107(6) 0.058(4) 0.0000 0.040(4) 0.0000 C29 0.108(5) 0.129(6) 0.090(5) 0.0000 0.064(4) 0.0000 C30 0.073(5) 0.148(7) 0.099(5) 0.0000 0.045(4) 0.0000 C31 0.062(4) 0.133(6) 0.083(5) 0.0000 0.036(4) 0.0000 C32 0.035(3) 0.038(3) 0.046(3) 0.0000 0.003(3) 0.0000 C33 0.053(4) 0.035(3) 0.092(5) 0.0000 0.000(3) 0.0000 C34 0.080(4) 0.044(3) 0.159(6) -0.015(3) -0.011(4) 0.002(3) C35 0.117(6) 0.052(3) 0.241(8) -0.028(3) -0.025(6) -0.005(4) C36 0.128(7) 0.042(4) 0.259(11) 0.0000 -0.004(8) 0.0000 C37 0.0425(19) 0.0312(17) 0.060(3) 0.0038(15) 0.0139(17) -0.0004(16) C38 0.0302(17) 0.0391(18) 0.049(2) -0.0005(14) 0.0087(15) 0.0022(15) C39 0.0317(18) 0.0400(18) 0.055(3) 0.0074(14) 0.0094(16) 0.0024(16) C40 0.0324(19) 0.048(2) 0.055(3) 0.0059(15) 0.0094(17) 0.0022(17) C41 0.027(3) 0.042(3) 0.046(3) 0.0000 0.009(2) 0.0000 C42 0.027(3) 0.042(3) 0.042(3) 0.0000 0.010(2) 0.0000 C43 0.0316(17) 0.0346(17) 0.0475(18) 0.0010(13) 0.0162(15) 0.0010(14) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ru1 Ru1 2.2842(4) yes . 7_455 Ru1 O1 2.058(3) yes . . Ru1 O2 2.068(3) yes . 7_455 Ru1 O3 2.065(3) yes . . Ru1 O4 2.072(3) yes . 7_455 Ru1 N1 2.274(3) yes . . Ru2 Ru2 2.2848(5) yes . 2_656 Ru2 O5 2.065(5) yes . . Ru2 O6 2.062(5) yes . 2_656 Ru2 O7 2.067(3) yes . . Ru2 O7 2.067(3) yes . 4_565 Ru2 N4 2.299(4) yes . . F1 C4 1.359(12) yes . . F2 C11 1.333(14) yes . . F3 C13 1.314(6) yes . . F4 C28 1.403(9) yes . . F5 C35 1.327(15) yes . . O1 C1 1.279(5) yes . . O2 C1 1.263(5) yes . . O3 C8 1.272(4) yes . . O4 C8 1.272(4) yes . . O5 C25 1.252(7) yes . . O6 C25 1.276(6) yes . . O7 C32 1.267(4) yes . . N1 C15 1.349(4) yes . . N1 C19 1.341(4) yes . . N2 C20 1.341(4) yes . . N2 C20 1.341(4) yes . 4_565 N3 C20 1.316(4) yes . . N3 C21 1.346(3) yes . . N4 C24 1.335(4) yes . . N4 C24 1.335(4) yes . 4_565 C1 C2 1.476(7) yes . . C2 C3 1.382(9) yes . . C2 C7 1.359(7) yes . . C3 C4 1.351(16) yes . . C4 C5 1.380(13) yes . . C5 C6 1.358(10) yes . . C6 C7 1.412(9) yes . . C8 C9 1.492(5) yes . . C9 C10 1.383(6) yes . . C9 C14 1.386(6) yes . . C10 C11 1.400(7) yes . . C11 C12 1.373(8) yes . . C12 C13 1.376(6) yes . . C13 C14 1.382(6) yes . . C15 C16 1.379(5) yes . . C16 C17 1.387(4) yes . . C17 C18 1.395(5) yes . . C17 C20 1.486(5) yes . . C18 C19 1.379(5) yes . . C21 C22 1.479(5) yes . . C22 C23 1.397(4) yes . . C22 C23 1.397(4) yes . 4_565 C23 C24 1.372(5) yes . . C25 C26 1.486(10) yes . . C26 C27 1.382(9) yes . . C26 C31 1.414(10) yes . . C27 C28 1.346(15) yes . . C28 C29 1.287(15) yes . . C29 C30 1.397(15) yes . . C30 C31 1.365(18) yes . . C32 C33 1.473(8) yes . . C33 C34 1.369(7) yes . . C33 C34 1.369(7) yes . 2_656 C34 C35 1.417(9) yes . . C35 C36 1.343(10) yes . . C37 C37 1.365(5) yes . 2_555 C37 C38 1.433(5) yes . . C38 C39 1.408(5) yes . . C38 C43 1.407(5) yes . . C39 C40 1.362(6) yes . . C40 C41 1.418(5) yes . . C41 C42 1.423(7) yes . . C42 C43 1.423(5) yes . . C42 C43 1.423(5) yes . 4_565 C43 C43 1.426(5) yes . 2_555 C3 H3 0.950 no . . C5 H5 0.950 no . . C6 H6 0.950 no . . C7 H7 0.950 no . . C10 H10 0.950 no . . C12 H12 0.950 no . . C14 H14 0.950 no . . C15 H15 0.950 no . . C16 H16 0.950 no . . C18 H18 0.950 no . . C19 H19 0.950 no . . C23 H23 0.950 no . . C24 H24 0.950 no . . C27 H27 0.950 no . . C29 H29 0.949 no . . C30 H30 0.950 no . . C31 H31 0.950 no . . C34 H34 0.950 no . . C36 H36 0.949 no . . C37 H37 0.950 no . . C39 H39 0.950 no . . C40 H40 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Ru1 Ru1 O1 88.47(7) yes 7_455 . . Ru1 Ru1 O2 90.18(7) yes 7_455 . 7_455 Ru1 Ru1 O3 89.72(7) yes 7_455 . . Ru1 Ru1 O4 89.60(7) yes 7_455 . 7_455 Ru1 Ru1 N1 173.88(10) yes 7_455 . . O1 Ru1 O2 178.42(9) yes . . 7_455 O1 Ru1 O3 90.97(11) yes . . . O1 Ru1 O4 88.64(11) yes . . 7_455 O1 Ru1 N1 85.55(11) yes . . . O2 Ru1 O3 89.85(11) yes 7_455 . . O2 Ru1 O4 90.52(11) yes 7_455 . 7_455 O2 Ru1 N1 95.82(11) yes 7_455 . . O3 Ru1 O4 179.23(10) yes . . 7_455 O3 Ru1 N1 89.12(10) yes . . . O4 Ru1 N1 91.51(10) yes 7_455 . . Ru2 Ru2 O5 89.37(9) yes 2_656 . . Ru2 Ru2 O6 89.59(9) yes 2_656 . 2_656 Ru2 Ru2 O7 89.44(6) yes 2_656 . . Ru2 Ru2 O7 89.44(6) yes 2_656 . 4_565 Ru2 Ru2 N4 175.93(12) yes 2_656 . . O5 Ru2 O6 178.96(12) yes . . 2_656 O5 Ru2 O7 90.27(9) yes . . . O5 Ru2 O7 90.27(9) yes . . 4_565 O5 Ru2 N4 94.70(15) yes . . . O6 Ru2 O7 89.72(9) yes 2_656 . . O6 Ru2 O7 89.72(9) yes 2_656 . 4_565 O6 Ru2 N4 86.34(15) yes 2_656 . . O7 Ru2 O7 178.76(9) yes . . 4_565 O7 Ru2 N4 90.54(6) yes . . . O7 Ru2 N4 90.54(6) yes 4_565 . . Ru1 O1 C1 120.0(3) yes . . . Ru1 O2 C1 118.1(3) yes 7_455 . . Ru1 O3 C8 117.77(19) yes . . . Ru1 O4 C8 117.5(3) yes 7_455 . . Ru2 O5 C25 118.1(4) yes . . . Ru2 O6 C25 117.5(4) yes 2_656 . . Ru2 O7 C32 118.2(3) yes . . . Ru1 N1 C15 115.00(19) yes . . . Ru1 N1 C19 127.1(3) yes . . . C15 N1 C19 117.9(3) yes . . . C20 N2 C20 114.4(3) yes . . 4_565 C20 N3 C21 114.4(3) yes . . . Ru2 N4 C24 121.00(19) yes . . . Ru2 N4 C24 121.00(19) yes . . 4_565 C24 N4 C24 117.5(4) yes . . 4_565 O1 C1 O2 123.2(4) yes . . . O1 C1 C2 117.3(4) yes . . . O2 C1 C2 119.5(4) yes . . . C1 C2 C3 118.0(6) yes . . . C1 C2 C7 120.6(4) yes . . . C3 C2 C7 121.3(6) yes . . . C2 C3 C4 117.5(7) yes . . . F1 C4 C3 117.3(9) yes . . . F1 C4 C5 118.8(11) yes . . . C3 C4 C5 123.7(8) yes . . . C4 C5 C6 118.0(9) yes . . . C5 C6 C7 119.9(6) yes . . . C2 C7 C6 119.4(5) yes . . . O3 C8 O4 125.4(3) yes . . . O3 C8 C9 117.0(3) yes . . . O4 C8 C9 117.6(3) yes . . . C8 C9 C10 120.1(4) yes . . . C8 C9 C14 119.7(3) yes . . . C10 C9 C14 120.1(4) yes . . . C9 C10 C11 119.1(5) yes . . . F2 C11 C10 118.6(8) yes . . . F2 C11 C12 119.3(7) yes . . . C10 C11 C12 121.2(5) yes . . . C11 C12 C13 118.5(5) yes . . . F3 C13 C12 119.1(5) yes . . . F3 C13 C14 119.0(4) yes . . . C12 C13 C14 121.9(5) yes . . . C9 C14 C13 119.2(4) yes . . . N1 C15 C16 122.4(3) yes . . . C15 C16 C17 119.5(3) yes . . . C16 C17 C18 118.4(3) yes . . . C16 C17 C20 119.3(3) yes . . . C18 C17 C20 122.3(3) yes . . . C17 C18 C19 118.7(3) yes . . . N1 C19 C18 123.2(3) yes . . . N2 C20 N3 125.7(3) yes . . . N2 C20 C17 114.3(3) yes . . . N3 C20 C17 120.0(3) yes . . . N3 C21 N3 125.2(3) yes . . 4_565 N3 C21 C22 117.39(17) yes . . . N3 C21 C22 117.39(17) yes 4_565 . . C21 C22 C23 121.26(18) yes . . . C21 C22 C23 121.26(18) yes . . 4_565 C23 C22 C23 117.5(3) yes . . 4_565 C22 C23 C24 119.0(4) yes . . . N4 C24 C23 123.5(4) yes . . . O5 C25 O6 125.5(7) yes . . . O5 C25 C26 118.5(5) yes . . . O6 C25 C26 116.1(5) yes . . . C25 C26 C27 120.6(6) yes . . . C25 C26 C31 119.4(6) yes . . . C27 C26 C31 120.0(8) yes . . . C26 C27 C28 116.5(7) yes . . . F4 C28 C27 117.2(8) yes . . . F4 C28 C29 115.2(10) yes . . . C27 C28 C29 127.7(9) yes . . . C28 C29 C30 116.4(12) yes . . . C29 C30 C31 121.8(10) yes . . . C26 C31 C30 117.6(8) yes . . . O7 C32 O7 124.7(5) yes . . 2_656 O7 C32 C33 117.7(3) yes . . . O7 C32 C33 117.7(3) yes 2_656 . . C32 C33 C34 121.1(4) yes . . . C32 C33 C34 121.1(4) yes . . 2_656 C34 C33 C34 117.9(6) yes . . 2_656 C33 C34 C35 120.0(6) yes . . . F5 C35 C34 117.0(8) yes . . . F5 C35 C36 119.9(8) yes . . . C34 C35 C36 122.4(7) yes . . . C35 C36 C35 117.2(8) yes . . 2_656 C37 C37 C38 121.2(4) yes 2_555 . . C37 C38 C39 122.2(4) yes . . . C37 C38 C43 118.4(3) yes . . . C39 C38 C43 119.4(4) yes . . . C38 C39 C40 121.0(4) yes . . . C39 C40 C41 121.6(4) yes . . . C40 C41 C40 123.1(4) yes . . 4_565 C40 C41 C42 118.4(3) yes . . . C40 C41 C42 118.4(3) yes 4_565 . . C41 C42 C43 119.6(3) yes . . . C41 C42 C43 119.6(3) yes . . 4_565 C43 C42 C43 120.7(4) yes . . 4_565 C38 C43 C42 120.0(3) yes . . . C38 C43 C43 120.4(3) yes . . 2_555 C42 C43 C43 119.6(4) yes . . 2_555 C2 C3 H3 121.254 no . . . C4 C3 H3 121.246 no . . . C4 C5 H5 120.968 no . . . C6 C5 H5 120.985 no . . . C5 C6 H6 120.037 no . . . C7 C6 H6 120.054 no . . . C2 C7 H7 120.315 no . . . C6 C7 H7 120.313 no . . . C9 C10 H10 120.455 no . . . C11 C10 H10 120.441 no . . . C11 C12 H12 120.773 no . . . C13 C12 H12 120.774 no . . . C9 C14 H14 120.386 no . . . C13 C14 H14 120.393 no . . . N1 C15 H15 118.805 no . . . C16 C15 H15 118.799 no . . . C15 C16 H16 120.276 no . . . C17 C16 H16 120.270 no . . . C17 C18 H18 120.664 no . . . C19 C18 H18 120.666 no . . . N1 C19 H19 118.399 no . . . C18 C19 H19 118.372 no . . . C22 C23 H23 120.471 no . . . C24 C23 H23 120.480 no . . . N4 C24 H24 118.252 no . . . C23 C24 H24 118.263 no . . . C26 C27 H27 121.813 no . . . C28 C27 H27 121.690 no . . . C28 C29 H29 121.853 no . . . C30 C29 H29 121.765 no . . . C29 C30 H30 119.036 no . . . C31 C30 H30 119.130 no . . . C26 C31 H31 121.196 no . . . C30 C31 H31 121.204 no . . . C33 C34 H34 119.986 no . . . C35 C34 H34 120.030 no . . . C35 C36 H36 121.392 no . . . C35 C36 H36 121.388 no 2_656 . . C37 C37 H37 119.392 no 2_555 . . C38 C37 H37 119.401 no . . . C38 C39 H39 119.524 no . . . C40 C39 H39 119.508 no . . . C39 C40 H40 119.226 no . . . C41 C40 H40 119.183 no . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 F1 C2 3.567(10) no . . F1 C6 3.580(9) no . . F2 C13 3.575(14) no . . F3 C9 3.582(6) no . . F3 C11 3.559(7) no . . F4 C26 3.599(9) no . . F4 C30 3.554(11) no . . F5 C33 3.592(13) no . . F5 C35 3.512(15) no . 2_656 O1 C3 2.716(10) no . . O1 C7 3.591(6) no . . O1 C8 3.567(4) no . . O1 C8 3.488(5) no . 7_455 O1 C15 3.183(5) no . . O2 C3 3.594(9) no . . O2 C7 2.794(7) no . . O2 C8 3.573(4) no . . O2 C8 3.534(5) no . 7_455 O3 C1 3.579(5) no . . O3 C1 3.536(6) no . 7_455 O3 C10 2.776(5) no . . O3 C19 3.314(5) no . . O4 C1 3.569(5) no . . O4 C1 3.553(6) no . 7_455 O4 C14 2.781(5) no . . O4 C15 3.147(4) no . 7_455 O5 C27 2.788(11) no . . O5 C32 3.545(5) no . . O6 C31 2.742(12) no . . O6 C32 3.546(5) no . . O7 C24 3.146(4) no . 4_565 O7 C25 3.542(7) no . . O7 C25 3.533(6) no . 2_656 O7 C34 2.781(7) no . . O7 C34 3.585(6) no . 2_656 N1 C17 2.785(4) no . . N2 N3 2.364(4) no . 4_565 N2 C16 2.718(4) no . . N2 C16 2.718(4) no . 4_565 N2 C17 2.376(4) no . 4_565 N2 C21 2.659(5) no . . N3 C18 2.889(4) no . . N3 C20 2.668(4) no . 4_565 N3 C23 2.823(4) no . 4_565 N4 C22 2.789(5) no . . N4 C23 2.385(5) no . 4_565 C2 C5 2.756(12) no . . C3 C6 2.770(10) no . . C4 C7 2.712(10) no . . C9 C12 2.785(6) no . . C10 C13 2.755(7) no . . C11 C14 2.760(6) no . . C15 C18 2.728(5) no . . C16 C19 2.716(5) no . . C17 C20 3.594(5) no . 4_565 C20 C22 3.593(5) no . . C22 C24 2.386(5) no . 4_565 C23 C24 2.708(5) no . 4_565 C26 C29 2.758(16) no . . C27 C30 2.737(12) no . . C28 C31 2.689(11) no . . C33 C35 2.413(9) no . 2_656 C33 C36 2.823(11) no . . C34 C35 2.718(10) no . 2_656 C37 C43 2.811(5) no . 2_555 C38 C38 2.851(5) no . 2_555 C38 C41 2.829(5) no . . C39 C42 2.810(5) no . . C40 C43 2.801(5) no . . C42 C42 2.833(7) no . 2_555 Ru2 O7 3.066(3) no . 3_666 Ru2 C32 2.891(5) no . 3_666 F1 F4 3.058(7) no . 1_455 F1 C28 2.973(8) no . 1_455 F1 C29 2.993(8) no . 1_455 F2 C33 3.217(15) no . 7_556 F2 C34 3.415(15) no . 7_556 F2 C34 3.16(2) no . 8_455 F2 C35 3.554(18) no . 7_556 F2 C35 3.37(3) no . 8_455 F2 C36 3.574(15) no . 7_556 F3 F3 2.886(5) no . 4_555 F3 O5 3.319(5) no . 5_445 F3 N4 3.585(7) no . 5_445 F3 C24 3.398(7) no . 5_445 F3 C27 3.592(8) no . 5_445 F3 C40 3.487(5) no . 8_455 F4 F1 3.058(7) no . 1_655 F4 F1 3.058(7) no . 4_665 O2 C6 3.542(6) no . 2_455 O3 C6 3.419(7) no . 8_555 O5 F3 3.319(5) no . 5_555 O5 F3 3.319(5) no . 8_555 O5 C32 3.545(5) no . 3_666 O6 O7 2.912(5) no . 3_666 O6 C32 3.546(5) no . 3_666 O7 C12 3.417(7) no . 8_555 N1 C37 3.500(7) no . 2_555 N3 C40 3.597(7) no . . N4 F3 3.585(7) no . 5_555 N4 F3 3.585(7) no . 8_555 C5 C9 3.556(11) no . 8_455 C5 C10 3.480(12) no . 8_455 C6 O2 3.542(6) no . 2_455 C6 O3 3.419(7) no . 8_455 C6 C10 3.596(10) no . 8_455 C7 C7 3.346(7) no . 2_455 C9 C5 3.556(11) no . 8_555 C10 C5 3.480(12) no . 8_555 C10 C6 3.596(10) no . 8_555 C11 C34 3.501(12) no . 8_455 C12 O7 3.417(7) no . 8_455 C15 C37 3.589(7) no . 2_555 C15 C38 3.516(7) no . 2_555 C15 C39 3.532(7) no . 2_555 C16 C38 3.357(7) no . 2_555 C16 C43 3.569(7) no . 2_555 C18 C37 3.377(7) no . . C19 C37 3.590(7) no . . C19 C37 3.495(7) no . 2_555 C20 C42 3.587(8) no . . C20 C43 3.374(6) no . . C21 C41 3.324(10) no . . C21 C42 3.566(9) no . . C22 C40 3.519(8) no . . C22 C40 3.519(8) no . 4_565 C22 C41 3.517(9) no . . C23 C40 3.490(7) no . 4_565 C24 F3 3.398(7) no . 5_555 C25 O7 3.533(6) no . 3_666 C27 F3 3.592(8) no . 5_555 C27 F3 3.592(8) no . 8_555 C28 F1 2.973(8) no . 1_655 C28 F1 2.973(8) no . 4_665 C29 F1 2.993(8) no . 1_655 C29 F1 2.993(8) no . 4_665 C33 F2 3.217(15) no . 7_556 C33 F2 3.217(15) no . 8_555 C34 F2 3.415(15) no . 7_556 C34 F2 3.16(2) no . 8_555 C34 C11 3.501(12) no . 8_555 C35 F2 3.554(18) no . 7_556 C35 F2 3.37(3) no . 8_555 C36 F2 3.574(15) no . 7_556 C36 F2 3.574(15) no . 8_555 C37 N1 3.500(7) no . 2_555 C37 C15 3.589(7) no . 2_555 C37 C18 3.377(7) no . . C37 C19 3.590(7) no . . C37 C19 3.495(7) no . 2_555 C38 C15 3.516(7) no . 2_555 C38 C16 3.357(7) no . 2_555 C39 C15 3.532(7) no . 2_555 C40 F3 3.487(5) no . 8_555 C40 N3 3.597(7) no . . C40 C22 3.519(8) no . . C40 C23 3.490(7) no . 4_565 C41 C21 3.324(10) no . . C41 C22 3.517(9) no . . C42 C20 3.587(8) no . . C42 C20 3.587(8) no . 4_565 C42 C21 3.566(9) no . . C42 C43 2.463(6) no . 3_565 C43 C16 3.569(7) no . 2_555 C43 C20 3.374(6) no . . C43 C43 2.855(5) no . 3_565 Ru1 H15 3.0288 no . . Ru1 H19 3.3133 no . . Ru2 H24 3.1842 no . . Ru2 H24 3.1842 no . 4_565 F1 H3 2.5018 no . . F1 H5 2.5573 no . . F2 H10 2.5490 no . . F2 H12 2.5388 no . . F3 H12 2.5226 no . . F3 H14 2.5216 no . . F4 H27 2.5248 no . . F4 H29 2.4290 no . . F5 H34 2.5243 no . . F5 H36 2.5255 no . . O1 H3 2.4059 no . . O1 H15 2.8413 no . . O2 H7 2.5040 no . . O2 H19 3.4864 no . 7_455 O3 H10 2.4891 no . . O3 H19 2.8789 no . . O4 H14 2.4861 no . . O4 H15 2.6064 no . 7_455 O5 H27 2.5242 no . . O6 H31 2.4499 no . . O7 H24 2.5313 no . 4_565 O7 H34 2.4938 no . . N1 H16 3.2410 no . . N1 H18 3.2425 no . . N2 H16 2.3793 no . . N2 H16 2.3793 no . 4_565 N3 H18 2.6129 no . . N3 H23 2.5162 no . 4_565 N4 H23 3.2317 no . . N4 H23 3.2317 no . 4_565 N4 H24 1.9710 no . 4_565 C1 H3 2.6156 no . . C1 H7 2.6293 no . . C2 H6 3.2480 no . . C3 H5 3.2564 no . . C3 H7 3.2458 no . . C4 H6 3.2129 no . . C5 H3 3.2632 no . . C5 H7 3.2536 no . . C7 H3 3.2487 no . . C7 H5 3.2647 no . . C8 H10 2.6564 no . . C8 H14 2.6494 no . . C10 H12 3.2765 no . . C10 H14 3.2591 no . . C12 H10 3.2706 no . . C12 H14 3.2638 no . . C14 H10 3.2601 no . . C14 H12 3.2669 no . . C15 H19 3.1607 no . . C16 H18 3.2554 no . . C17 H15 3.2418 no . . C17 H19 3.2394 no . . C18 H16 3.2543 no . . C19 H15 3.1618 no . . C20 H16 2.6380 no . . C20 H18 2.7101 no . . C21 H23 2.6833 no . . C21 H23 2.6833 no . 4_565 C22 H23 2.0492 no . 4_565 C22 H24 3.2381 no . . C22 H24 3.2381 no . 4_565 C23 H23 3.2557 no . 4_565 C24 H24 3.1378 no . 4_565 C25 H27 2.6809 no . . C25 H31 2.6785 no . . C26 H30 3.2400 no . . C27 H29 3.2124 no . . C27 H31 3.2830 no . . C28 H30 3.1367 no . . C29 H27 3.2040 no . . C29 H31 3.2756 no . . C31 H27 3.2910 no . . C31 H29 3.2738 no . . C32 H34 2.6408 no . . C32 H34 2.6408 no . 2_656 C33 H34 2.0192 no . 2_656 C34 H34 3.2100 no . 2_656 C34 H36 3.2817 no . . C36 H34 3.2638 no . . C36 H34 3.2638 no . 2_656 C37 H39 2.6686 no . . C38 H37 3.2927 no . 2_555 C38 H40 3.2633 no . . C39 H37 2.6754 no . . C40 H40 2.6796 no . 4_565 C41 H39 3.2793 no . . C41 H39 3.2793 no . 4_565 C41 H40 2.0555 no . 4_565 C42 H40 3.2968 no . . C42 H40 3.2968 no . 4_565 C43 H37 3.2964 no . . C43 H39 3.2872 no . . H3 H15 3.5063 no . . H5 H6 2.3236 no . . H6 H7 2.3668 no . . H10 H19 3.4446 no . . H14 H15 3.1326 no . 7_455 H15 H16 2.3160 no . . H16 H16 2.8794 no . 4_565 H18 H19 2.3152 no . . H18 H23 3.4249 no . 4_565 H23 H24 2.3040 no . . H24 H34 2.9637 no . 4_565 H29 H30 2.3580 no . . H30 H31 2.3197 no . . H37 H37 2.2978 no . 2_555 H37 H39 2.5069 no . . H39 H40 2.2933 no . . H40 H40 2.5181 no . 4_565 F1 H29 3.0287 no . 1_455 F2 H34 3.5227 no . 8_455 F3 H24 3.3289 no . 5_445 F3 H27 2.7553 no . 5_445 F3 H40 2.5425 no . 8_455 O2 H6 2.9834 no . 2_455 O2 H7 3.2731 no . 2_455 O2 H37 3.1961 no . 8_455 O3 H6 2.4778 no . 8_555 O4 H39 3.0330 no . 8_455 O5 H12 2.8235 no . 5_555 O5 H12 2.8235 no . 8_555 O7 H12 2.7450 no . 8_555 N1 H37 3.2490 no . 2_555 C1 H6 3.4372 no . 2_455 C6 H10 3.5410 no . 8_455 C6 H19 3.4054 no . 8_455 C7 H7 3.0439 no . 2_455 C7 H19 3.5827 no . 8_455 C8 H6 2.8798 no . 8_555 C9 H5 2.8675 no . 8_555 C9 H6 3.0503 no . 8_555 C10 H5 2.8763 no . 8_555 C10 H6 3.0755 no . 8_555 C11 H5 3.0506 no . 8_555 C11 H34 3.5010 no . 8_455 C12 H5 3.1861 no . 8_555 C12 H24 3.5301 no . 5_445 C12 H34 3.5742 no . 8_455 C13 H5 3.1658 no . 8_555 C13 H24 3.4936 no . 5_445 C13 H27 3.4532 no . 5_445 C13 H40 3.1326 no . 8_455 C14 H5 3.0141 no . 8_555 C14 H39 3.1056 no . 8_455 C14 H40 3.0514 no . 8_455 C15 H37 3.5625 no . 2_555 C15 H39 3.5220 no . 2_555 C18 H37 3.5476 no . . C19 H37 3.4110 no . 2_555 C22 H40 3.4430 no . . C22 H40 3.4430 no . 4_565 C23 H40 3.2007 no . 4_565 C24 H40 3.5953 no . 4_565 C25 H12 3.2340 no . 5_555 C25 H12 3.2340 no . 8_555 C26 H12 3.5999 no . 5_555 C26 H12 3.5999 no . 8_555 C27 H12 3.5838 no . 5_555 C27 H12 3.5838 no . 8_555 C32 H12 3.1419 no . 7_556 C32 H12 3.1419 no . 8_555 C33 H12 3.4541 no . 7_556 C33 H12 3.4541 no . 8_555 C37 H18 3.5250 no . . C38 H16 3.5296 no . 2_555 C39 H14 3.0201 no . 8_555 C39 H15 3.4402 no . 2_555 C40 H14 3.0166 no . 8_555 C40 H23 3.4540 no . 4_565 C43 H16 3.5316 no . 2_555 H5 C9 2.8675 no . 8_455 H5 C10 2.8763 no . 8_455 H5 C11 3.0506 no . 8_455 H5 C12 3.1861 no . 8_455 H5 C13 3.1658 no . 8_455 H5 C14 3.0141 no . 8_455 H5 H10 3.3360 no . 8_455 H5 H14 3.5404 no . 8_455 H6 O2 2.9834 no . 2_455 H6 O3 2.4778 no . 8_455 H6 C1 3.4372 no . 2_455 H6 C8 2.8798 no . 8_455 H6 C9 3.0503 no . 8_455 H6 C10 3.0755 no . 8_455 H6 H10 2.9241 no . 8_455 H6 H19 2.7919 no . 8_455 H7 O2 3.2731 no . 2_455 H7 C7 3.0439 no . 2_455 H7 H7 2.4996 no . 2_455 H7 H19 3.1431 no . 8_455 H7 H37 2.9587 no . 8_455 H10 C6 3.5410 no . 8_555 H10 H5 3.3360 no . 8_555 H10 H6 2.9241 no . 8_555 H12 O5 2.8235 no . 5_445 H12 O7 2.7450 no . 8_455 H12 C25 3.2340 no . 5_445 H12 C26 3.5999 no . 5_445 H12 C27 3.5838 no . 5_445 H12 C32 3.1419 no . 7_556 H12 C33 3.4541 no . 7_556 H12 H24 3.4095 no . 5_445 H12 H27 3.2748 no . 5_445 H12 H34 3.4809 no . 8_455 H14 C39 3.0201 no . 8_455 H14 C40 3.0166 no . 8_455 H14 H5 3.5404 no . 8_555 H14 H39 2.5122 no . 8_455 H14 H40 2.5078 no . 8_455 H15 C39 3.4402 no . 2_555 H15 H39 3.3110 no . 2_555 H16 C38 3.5296 no . 2_555 H16 C43 3.5316 no . 2_555 H18 C37 3.5250 no . . H18 H37 3.5448 no . . H19 C6 3.4054 no . 8_555 H19 C7 3.5827 no . 8_555 H19 H6 2.7919 no . 8_555 H19 H7 3.1431 no . 8_555 H23 C40 3.4540 no . 4_565 H23 H40 3.2904 no . 4_565 H24 F3 3.3289 no . 5_555 H24 C12 3.5301 no . 5_555 H24 C13 3.4936 no . 5_555 H24 H12 3.4095 no . 5_555 H27 F3 2.7553 no . 5_555 H27 F3 2.7553 no . 8_555 H27 C13 3.4532 no . 5_555 H27 C13 3.4532 no . 8_555 H27 H12 3.2748 no . 5_555 H27 H12 3.2748 no . 8_555 H29 F1 3.0287 no . 1_655 H29 F1 3.0287 no . 4_665 H34 F2 3.5227 no . 8_555 H34 C11 3.5010 no . 8_555 H34 C12 3.5742 no . 8_555 H34 H12 3.4809 no . 8_555 H37 O2 3.1961 no . 8_555 H37 N1 3.2490 no . 2_555 H37 C15 3.5625 no . 2_555 H37 C18 3.5476 no . . H37 C19 3.4110 no . 2_555 H37 H7 2.9587 no . 8_555 H37 H18 3.5448 no . . H39 O4 3.0330 no . 8_555 H39 C14 3.1056 no . 8_555 H39 C15 3.5220 no . 2_555 H39 H14 2.5122 no . 8_555 H39 H15 3.3110 no . 2_555 H40 F3 2.5425 no . 8_555 H40 C13 3.1326 no . 8_555 H40 C14 3.0514 no . 8_555 H40 C22 3.4430 no . . H40 C23 3.2007 no . 4_565 H40 C24 3.5953 no . 4_565 H40 H14 2.5078 no . 8_555 H40 H23 3.2904 no . 4_565 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.033 -0.006 0.472 5151 950 ' ' _platon_squeeze_details ; ; #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================