# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_General _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- CCDC-840833_R2.cif' _audit_creation_date 2012-02-24 _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 H.Miyasaka ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; M.Nishio '' '' K.Nakabayashi '' '' K.Kubo '' '' W.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. 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__Ru2-CF3CO2-TCNQMe2 _database_code_depnum_ccdc_archive 'CCDC 840833' #TrackingRef '- CCDC-840833_R2.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C51 H29 Cl3 F24 N4 O16 Ru4' _chemical_formula_moiety 'C51 H29 Cl3 F24 N4 O16 Ru4' _chemical_formula_weight 1920.41 _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 16.890(4) _cell_length_b 20.759(4) _cell_length_c 12.145(3) _cell_angle_alpha 90.0000 _cell_angle_beta 117.872(2) _cell_angle_gamma 90.0000 _cell_volume 3764.4(13) _cell_formula_units_Z 2 _cell_measurement_reflns_used 5891 _cell_measurement_theta_min 3.42 _cell_measurement_theta_max 27.49 _cell_measurement_temperature 103 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour darkgreen _exptl_crystal_size_max 0.355 _exptl_crystal_size_mid 0.267 _exptl_crystal_size_min 0.043 _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1868.00 _exptl_absorpt_coefficient_mu 1.011 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.826 _exptl_absorpt_correction_T_max 0.957 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 103 _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 12101 _diffrn_reflns_av_R_equivalents 0.0177 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_max 0.976 _diffrn_measured_fraction_theta_full 0.976 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _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). In the process of refinement, the rigid bond Uij restraint (DELU) and the similar U restraint (SIMU) were treated for all atoms with (DELU 0.01 0.01) and (SIMU 0.04 0.08) (SIMU and DELU instructions in SHELXL97; Sheldrick, 2008). To fix the identical position for disordered atoms, the equal xyz constraint (EXYZ) was treated for Cl2 and C17. ; _reflns_number_total 3340 _reflns_number_gt 3035 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1279 _refine_ls_number_restraints 191 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 3339 _refine_ls_number_parameters 247 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0682P)^2^+27.0100P] 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 2.750 _refine_diff_density_min -1.140 _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) ; Cl Cl 0.1484 0.1585 ; 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 Ru(1) Ru 0.71977(2) 0.699818(15) 0.46811(3) 0.02272(16) Uani 1.0 8 d . . . Cl(1) Cl 0.65577(13) 0.5000 -0.11587(17) 0.0535(5) Uani 1.0 4 d . . . Cl(2) Cl 0.5000 0.64910(19) 0.5000 0.095(4) Uiso 0.5000 4 d . . . F(1) F 0.43949(19) 0.79832(15) 0.3625(4) 0.0491(8) Uani 1.0 8 d . . . F(2) F 0.4931(2) 0.89051(16) 0.3580(4) 0.0701(11) Uani 1.0 8 d . . . F(3) F 0.4614(2) 0.8241(2) 0.2081(3) 0.0622(10) Uani 1.0 8 d . . . F(4) F 0.6906(4) 0.6830(3) 0.8347(4) 0.0901(15) Uani 1.0 8 d . . . F(5) F 0.7416(3) 0.77620(18) 0.8872(4) 0.0700(11) Uani 1.0 8 d . . . F(6) F 0.8298(4) 0.6977(3) 0.9168(4) 0.109(2) Uani 1.0 8 d . . . O(1) O 0.59358(19) 0.74082(15) 0.3861(3) 0.0303(7) Uani 1.0 8 d . . . O(2) O 0.65284(19) 0.83946(14) 0.4521(3) 0.0298(7) Uani 1.0 8 d . . . O(3) O 0.7189(2) 0.68714(15) 0.6362(3) 0.0287(7) Uani 1.0 8 d . . . O(4) O 0.7769(2) 0.78609(15) 0.6984(3) 0.0309(7) Uani 1.0 8 d . . . N(1) N 0.6584(3) 0.60179(18) 0.3940(4) 0.0299(8) Uani 1.0 8 d . . . C(1) C 0.5894(3) 0.8009(2) 0.3961(4) 0.0278(9) Uani 1.0 8 d . . . C(2) C 0.4944(3) 0.8294(3) 0.3297(5) 0.0399(11) Uani 1.0 8 d . . . C(3) C 0.7484(3) 0.7325(2) 0.7129(4) 0.0298(9) Uani 1.0 8 d . . . C(4) C 0.7530(4) 0.7212(3) 0.8400(5) 0.0423(12) Uani 1.0 8 d . . . C(5) C 0.6307(3) 0.5573(2) 0.3325(4) 0.0245(9) Uani 1.0 8 d . . . C(6) C 0.6000(4) 0.5000 0.2604(5) 0.0268(12) Uani 1.0 4 d . . . C(7) C 0.5489(4) 0.5000 0.1312(6) 0.0281(13) Uani 1.0 4 d . . . C(8) C 0.5230(3) 0.4401(2) 0.0625(4) 0.0319(10) Uani 1.0 8 d . . . C(9) C 0.5263(7) 0.3705(5) 0.1122(8) 0.036(3) Uani 0.5000 8 d . . . C(10) C 0.8604(4) 0.5000 0.4448(7) 0.0413(16) Uani 1.0 4 d . . . C(11) C 0.8093(4) 0.5000 0.3037(6) 0.0308(13) Uani 1.0 4 d . . . C(12) C 0.7856(3) 0.5576(3) 0.2377(5) 0.0328(10) Uani 1.0 8 d . . . C(13) C 0.7387(3) 0.5581(3) 0.1089(5) 0.0358(10) Uani 1.0 8 d . . . C(14) C 0.7154(4) 0.5000 0.0460(6) 0.0352(14) Uani 1.0 4 d . . . C(15) C 0.5778(3) 0.5333(3) 0.5764(5) 0.0334(10) Uani 1.0 8 d . . . C(16) C 0.5000 0.5666(3) 0.5000 0.0354(15) Uani 1.0 4 d . . . C(17) C 0.5000 0.64910(19) 0.5000 0.005(4) Uiso 0.5000 4 d . . . H(9A) H 0.5053 0.3709 0.1750 0.0435 Uiso 0.5000 8 calc R . . H(9B) H 0.5880 0.3545 0.1499 0.0435 Uiso 0.5000 8 calc R . . H(9C) H 0.4877 0.3423 0.0431 0.0435 Uiso 0.5000 8 calc R . . H(10A) H 0.8374 0.5343 0.4775 0.0496 Uiso 0.5000 8 calc R . . H(10B) H 0.9242 0.5075 0.4716 0.0496 Uiso 0.5000 8 calc R . . H(10C) H 0.8529 0.4583 0.4764 0.0496 Uiso 0.5000 8 calc R . . H(12) H 0.8019 0.5973 0.2816 0.0394 Uiso 1.0 8 calc R . . H(13) H 0.7227 0.5977 0.0645 0.0429 Uiso 1.0 8 calc R . . H(15) H 0.6324 0.5588 0.6334 0.0587 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 Ru(1) 0.0240(3) 0.0231(3) 0.0254(3) 0.00162(12) 0.01512(17) 0.00148(12) Cl(1) 0.0449(11) 0.0856(15) 0.0352(9) 0.0000 0.0230(9) 0.0000 F(1) 0.0279(15) 0.061(2) 0.062(2) 0.0077(13) 0.0237(15) 0.0093(15) F(2) 0.0350(17) 0.0413(18) 0.112(3) 0.0138(14) 0.0161(18) -0.0067(19) F(3) 0.0421(18) 0.094(3) 0.0421(17) 0.0217(18) 0.0125(15) 0.0190(18) F(4) 0.150(4) 0.093(3) 0.063(3) -0.057(3) 0.079(3) -0.014(3) F(5) 0.131(4) 0.054(2) 0.0490(19) 0.001(3) 0.062(3) -0.0004(16) F(6) 0.106(4) 0.184(6) 0.044(3) 0.076(4) 0.040(3) 0.054(3) O(1) 0.0252(15) 0.0328(16) 0.0327(16) 0.0031(13) 0.0133(13) 0.0009(13) O(2) 0.0276(15) 0.0286(16) 0.0378(17) 0.0054(13) 0.0191(14) 0.0021(13) O(3) 0.0317(16) 0.0326(16) 0.0271(15) 0.0009(13) 0.0181(13) 0.0041(13) O(4) 0.0371(18) 0.0335(16) 0.0287(16) 0.0002(14) 0.0209(14) 0.0006(13) N(1) 0.0300(19) 0.0293(19) 0.035(2) 0.0020(16) 0.0195(17) 0.0032(16) C(1) 0.025(3) 0.032(3) 0.030(3) 0.0053(17) 0.0166(19) 0.0039(17) C(2) 0.028(3) 0.040(3) 0.049(3) 0.006(2) 0.016(3) 0.002(3) C(3) 0.031(3) 0.032(3) 0.031(3) 0.0037(18) 0.0183(19) 0.0031(18) C(4) 0.061(4) 0.040(3) 0.034(3) 0.004(3) 0.029(3) 0.004(2) C(5) 0.0186(19) 0.032(3) 0.025(2) 0.0031(17) 0.0116(17) 0.0065(17) C(6) 0.021(3) 0.035(4) 0.023(3) 0.0000 0.009(3) 0.0000 C(7) 0.020(3) 0.034(3) 0.027(3) 0.0000 0.009(3) 0.0000 C(8) 0.040(3) 0.025(3) 0.031(2) 0.0103(18) 0.016(2) 0.0063(17) C(9) 0.046(6) 0.027(4) 0.018(5) -0.001(4) 0.000(4) 0.001(4) C(10) 0.026(4) 0.053(5) 0.042(4) 0.0000 0.014(3) 0.0000 C(11) 0.018(3) 0.039(4) 0.038(4) 0.0000 0.015(3) 0.0000 C(12) 0.026(3) 0.031(3) 0.047(3) -0.0040(18) 0.022(2) -0.0036(19) C(13) 0.032(3) 0.036(3) 0.045(3) -0.000(2) 0.023(2) 0.007(2) C(14) 0.026(4) 0.051(4) 0.033(4) 0.0000 0.018(3) 0.0000 C(15) 0.028(3) 0.043(3) 0.034(3) -0.003(2) 0.019(2) -0.005(2) C(16) 0.033(4) 0.032(4) 0.056(4) 0.0000 0.033(3) 0.0000 #============================================================================== _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 Ru(1) Ru(1) 2.2900(6) yes . 7_666 Ru(1) O(1) 2.067(3) yes . . Ru(1) O(2) 2.070(3) yes . 7_666 Ru(1) O(3) 2.065(4) yes . . Ru(1) O(4) 2.070(4) yes . 7_666 Ru(1) N(1) 2.270(4) yes . . Cl(1) C(14) 1.740(7) yes . . Cl(2) C(16) 1.713(8) yes . . F(1) C(2) 1.334(8) yes . . F(2) C(2) 1.317(7) yes . . F(3) C(2) 1.317(7) yes . . F(4) C(4) 1.298(9) yes . . F(5) C(4) 1.331(8) yes . . F(6) C(4) 1.288(7) yes . . O(1) C(1) 1.258(6) yes . . O(2) C(1) 1.253(5) yes . . O(3) C(3) 1.252(6) yes . . O(4) C(3) 1.257(6) yes . . N(1) C(5) 1.142(6) yes . . C(1) C(2) 1.539(7) yes . . C(3) C(4) 1.526(9) yes . . C(5) C(6) 1.423(5) yes . . C(6) C(7) 1.393(8) yes . . C(7) C(8) 1.446(6) yes . . C(7) C(8) 1.446(6) yes . 4_565 C(8) C(8) 1.345(6) yes . 2_655 C(8) C(9) 1.556(10) yes . . C(10) C(11) 1.516(10) yes . . C(11) C(12) 1.391(6) yes . . C(11) C(12) 1.391(6) yes . 4_565 C(12) C(13) 1.384(7) yes . . C(13) C(14) 1.383(6) yes . . C(15) C(15) 1.383(7) yes . 4_565 C(15) C(16) 1.388(6) yes . . C(16) C(17) 1.713(8) yes . . C(9) H(9A) 0.980 no . . C(9) H(9B) 0.980 no . . C(9) H(9C) 0.980 no . . C(10) H(10A) 0.979 no . . C(10) H(10A) 0.979 no . 4_565 C(10) H(10B) 0.981 no . . C(10) H(10B) 0.981 no . 4_565 C(10) H(10C) 0.980 no . . C(10) H(10C) 0.980 no . 4_565 C(12) H(12) 0.950 no . . C(13) H(13) 0.950 no . . C(15) H(15) 1.006 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 Ru(1) Ru(1) O(1) 89.12(9) yes 7_666 . . Ru(1) Ru(1) O(2) 89.91(8) yes 7_666 . 7_666 Ru(1) Ru(1) O(3) 89.40(9) yes 7_666 . . Ru(1) Ru(1) O(4) 89.46(9) yes 7_666 . 7_666 Ru(1) Ru(1) N(1) 176.79(11) yes 7_666 . . O(1) Ru(1) O(2) 178.49(14) yes . . 7_666 O(1) Ru(1) O(3) 92.70(14) yes . . . O(1) Ru(1) O(4) 87.90(14) yes . . 7_666 O(1) Ru(1) N(1) 90.07(13) yes . . . O(2) Ru(1) O(3) 88.45(14) yes 7_666 . . O(2) Ru(1) O(4) 90.93(14) yes 7_666 . 7_666 O(2) Ru(1) N(1) 90.83(13) yes 7_666 . . O(3) Ru(1) O(4) 178.70(12) yes . . 7_666 O(3) Ru(1) N(1) 93.73(15) yes . . . O(4) Ru(1) N(1) 87.42(15) yes 7_666 . . Ru(1) O(1) C(1) 116.9(3) yes . . . Ru(1) O(2) C(1) 116.1(3) yes 7_666 . . Ru(1) O(3) C(3) 117.1(4) yes . . . Ru(1) O(4) C(3) 116.7(3) yes 7_666 . . Ru(1) N(1) C(5) 163.1(5) yes . . . O(1) C(1) O(2) 127.9(4) yes . . . O(1) C(1) C(2) 115.0(4) yes . . . O(2) C(1) C(2) 117.1(4) yes . . . F(1) C(2) F(2) 106.8(6) yes . . . F(1) C(2) F(3) 107.8(4) yes . . . F(1) C(2) C(1) 111.0(4) yes . . . F(2) C(2) F(3) 108.9(5) yes . . . F(2) C(2) C(1) 112.0(4) yes . . . F(3) C(2) C(1) 110.2(5) yes . . . O(3) C(3) O(4) 127.3(5) yes . . . O(3) C(3) C(4) 116.9(5) yes . . . O(4) C(3) C(4) 115.8(4) yes . . . F(4) C(4) F(5) 105.5(6) yes . . . F(4) C(4) F(6) 108.9(6) yes . . . F(4) C(4) C(3) 112.8(4) yes . . . F(5) C(4) F(6) 108.2(5) yes . . . F(5) C(4) C(3) 110.8(5) yes . . . F(6) C(4) C(3) 110.4(6) yes . . . N(1) C(5) C(6) 177.1(4) yes . . . C(5) C(6) C(5) 113.3(4) yes . . 4_565 C(5) C(6) C(7) 123.3(3) yes . . . C(5) C(6) C(7) 123.3(3) yes 4_565 . . C(6) C(7) C(8) 120.7(3) yes . . . C(6) C(7) C(8) 120.7(3) yes . . 4_565 C(8) C(7) C(8) 118.6(5) yes . . 4_565 C(7) C(8) C(8) 120.7(5) yes . . 2_655 C(7) C(8) C(9) 128.9(6) yes . . . C(8) C(8) C(9) 109.6(5) yes 2_655 . . C(10) C(11) C(12) 120.7(3) yes . . . C(10) C(11) C(12) 120.7(3) yes . . 4_565 C(12) C(11) C(12) 118.6(6) yes . . 4_565 C(11) C(12) C(13) 121.1(5) yes . . . C(12) C(13) C(14) 118.9(5) yes . . . Cl(1) C(14) C(13) 119.3(3) yes . . . Cl(1) C(14) C(13) 119.3(3) yes . . 4_565 C(13) C(14) C(13) 121.4(6) yes . . 4_565 C(15) C(15) C(16) 119.9(5) yes 4_565 . . Cl(2) C(16) C(15) 119.9(3) yes . . . Cl(2) C(16) C(15) 119.9(3) yes . . 2_656 Cl(2) C(16) C(17) 0.000 yes . . . C(15) C(16) C(15) 120.3(6) yes . . 2_656 C(15) C(16) C(17) 119.9(3) yes . . . C(15) C(16) C(17) 119.9(3) yes 2_656 . . C(8) C(9) H(9A) 109.476 no . . . C(8) C(9) H(9B) 109.484 no . . . C(8) C(9) H(9C) 109.472 no . . . H(9A) C(9) H(9B) 109.465 no . . . H(9A) C(9) H(9C) 109.464 no . . . H(9B) C(9) H(9C) 109.467 no . . . C(11) C(10) H(10A) 109.502 no . . . C(11) C(10) H(10A) 109.502 no . . 4_565 C(11) C(10) H(10B) 109.392 no . . . C(11) C(10) H(10B) 109.392 no . . 4_565 C(11) C(10) H(10C) 109.478 no . . . C(11) C(10) H(10C) 109.478 no . . 4_565 H(10A) C(10) H(10A) 93.160 no . . 4_565 H(10A) C(10) H(10B) 109.461 no . . . H(10A) C(10) H(10B) 124.236 no . . 4_565 H(10A) C(10) H(10C) 109.542 no . . . H(10A) C(10) H(10C) 18.189 no . . 4_565 H(10A) C(10) H(10B) 124.236 no 4_565 . . H(10A) C(10) H(10B) 109.461 no 4_565 . 4_565 H(10A) C(10) H(10C) 18.189 no 4_565 . . H(10A) C(10) H(10C) 109.542 no 4_565 . 4_565 H(10B) C(10) H(10B) 18.175 no . . 4_565 H(10B) C(10) H(10C) 109.451 no . . . H(10B) C(10) H(10C) 93.078 no . . 4_565 H(10B) C(10) H(10C) 93.078 no 4_565 . . H(10B) C(10) H(10C) 109.451 no 4_565 . 4_565 H(10C) C(10) H(10C) 124.320 no . . 4_565 C(11) C(12) H(12) 119.457 no . . . C(13) C(12) H(12) 119.442 no . . . C(12) C(13) H(13) 120.569 no . . . C(14) C(13) H(13) 120.574 no . . . C(15) C(15) H(15) 121.686 no 4_565 . . C(16) C(15) H(15) 118.402 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 F(1) O(1) 2.754(5) no . . F(1) O(2) 3.351(5) no . . F(2) O(1) 3.480(5) no . . F(2) O(2) 2.612(5) no . . F(3) O(1) 2.852(5) no . . F(3) O(2) 3.221(4) no . . F(4) O(3) 2.670(7) no . . F(4) O(4) 3.421(7) no . . F(5) O(3) 3.430(6) no . . F(5) O(4) 2.633(7) no . . F(6) O(3) 3.034(5) no . . F(6) O(4) 2.997(6) no . . O(1) C(3) 3.595(5) no . . O(1) C(3) 3.446(7) no . 7_666 O(2) C(3) 3.576(6) no . . O(2) C(3) 3.487(7) no . 7_666 O(3) C(1) 3.592(5) no . . O(3) C(1) 3.446(7) no . 7_666 O(4) C(1) 3.568(5) no . . O(4) C(1) 3.478(7) no . 7_666 N(1) C(5) 3.369(6) no . 4_565 N(1) C(7) 3.543(6) no . . N(1) C(9) 3.143(9) no . 4_565 C(5) C(8) 2.913(6) no . 4_565 C(5) C(9) 2.847(9) no . 4_565 C(6) C(9) 3.149(9) no . . C(6) C(9) 3.149(9) no . 4_565 C(7) C(7) 2.822(9) no . 2_655 C(7) C(9) 2.709(9) no . 4_565 C(9) C(9) 2.440(13) no . 2_655 C(11) C(13) 2.416(8) no . 4_565 C(11) C(14) 2.769(9) no . . C(12) C(13) 2.772(7) no . 4_565 Cl(1) C(7) 3.374(8) no . 2_655 Cl(1) C(8) 3.593(7) no . 2_655 Cl(1) C(8) 3.593(7) no . 3_665 Cl(1) C(15) 3.403(6) no . 1_554 Cl(1) C(15) 3.403(6) no . 4_564 Cl(2) F(1) 3.440(5) no . . Cl(2) F(1) 3.440(5) no . 2_656 Cl(2) O(1) 3.175(5) no . . Cl(2) O(1) 3.175(5) no . 2_656 Cl(2) O(3) 3.364(4) no . . Cl(2) O(3) 3.364(4) no . 2_656 F(1) Cl(2) 3.440(5) no . . F(1) F(1) 2.991(5) no . 2_656 F(1) F(2) 3.587(6) no . 2_656 F(1) F(4) 3.373(6) no . 2_656 F(1) F(5) 3.177(5) no . 2_656 F(1) O(1) 3.557(6) no . 2_656 F(1) O(2) 3.393(6) no . 2_656 F(1) O(3) 3.539(5) no . 2_656 F(1) O(4) 3.383(5) no . 2_656 F(1) C(1) 3.189(8) no . 2_656 F(1) C(2) 3.425(7) no . 2_656 F(1) C(3) 3.171(6) no . 2_656 F(1) C(4) 3.422(6) no . 2_656 F(1) C(17) 3.440(5) no . . F(2) F(1) 3.587(6) no . 2_656 F(2) F(2) 3.346(8) no . 2_656 F(2) C(10) 3.388(6) no . 6_656 F(2) C(12) 3.285(6) no . 8_465 F(3) F(5) 3.222(6) no . 2_656 F(3) F(6) 3.211(5) no . 8_464 F(4) F(1) 3.373(6) no . 2_656 F(4) F(5) 3.134(6) no . 7_667 F(5) F(1) 3.177(5) no . 2_656 F(5) F(3) 3.222(6) no . 2_656 F(5) F(4) 3.134(6) no . 7_667 F(5) F(5) 2.836(6) no . 7_667 F(5) F(6) 3.178(8) no . 7_667 F(5) C(4) 3.272(8) no . 7_667 F(5) C(13) 3.454(6) no . 7_666 F(6) F(3) 3.211(5) no . 8_566 F(6) F(5) 3.178(8) no . 7_667 O(1) Cl(2) 3.175(5) no . . O(1) F(1) 3.557(6) no . 2_656 O(1) C(17) 3.175(5) no . . O(2) F(1) 3.393(6) no . 2_656 O(3) Cl(2) 3.364(4) no . . O(3) F(1) 3.539(5) no . 2_656 O(3) C(17) 3.364(4) no . . O(4) F(1) 3.383(5) no . 2_656 O(4) C(9) 3.501(10) no . 6_656 N(1) C(12) 3.588(8) no . . N(1) C(15) 3.406(8) no . . N(1) C(16) 3.546(5) no . . C(1) F(1) 3.189(8) no . 2_656 C(2) F(1) 3.425(7) no . 2_656 C(3) F(1) 3.171(6) no . 2_656 C(4) F(1) 3.422(6) no . 2_656 C(4) F(5) 3.272(8) no . 7_667 C(5) C(11) 3.409(9) no . . C(5) C(12) 3.316(8) no . . C(5) C(15) 3.506(8) no . . C(6) C(11) 3.322(10) no . . C(6) C(12) 3.485(9) no . . C(6) C(12) 3.485(9) no . 4_565 C(7) Cl(1) 3.374(8) no . 2_655 C(7) C(8) 2.426(7) no . 3_665 C(7) C(13) 3.552(10) no . . C(7) C(13) 3.552(10) no . 4_565 C(7) C(14) 3.420(12) no . . C(8) Cl(1) 3.593(7) no . 2_655 C(8) C(8) 2.827(7) no . 3_665 C(8) C(13) 3.417(8) no . 4_565 C(8) C(14) 3.572(10) no . . C(9) O(4) 3.501(10) no . 6_646 C(10) F(2) 3.388(6) no . 6_646 C(10) F(2) 3.388(6) no . 7_666 C(11) C(5) 3.409(9) no . . C(11) C(5) 3.409(9) no . 4_565 C(11) C(6) 3.322(10) no . . C(12) F(2) 3.285(6) no . 8_565 C(12) N(1) 3.588(8) no . . C(12) C(5) 3.316(8) no . . C(12) C(6) 3.485(9) no . . C(13) F(5) 3.454(6) no . 7_666 C(13) C(7) 3.552(10) no . . C(13) C(8) 3.417(8) no . 4_565 C(14) C(7) 3.420(12) no . . C(14) C(8) 3.572(10) no . . C(14) C(8) 3.572(10) no . 4_565 C(15) Cl(1) 3.403(6) no . 1_556 C(15) N(1) 3.406(8) no . . C(15) C(5) 3.506(8) no . . C(15) C(15) 2.777(6) no . 3_666 C(15) C(16) 2.398(8) no . 3_666 C(16) N(1) 3.546(5) no . . C(16) N(1) 3.546(5) no . 2_656 C(16) C(15) 2.398(8) no . 3_666 C(16) C(16) 2.765(9) no . 3_666 C(17) F(1) 3.440(5) no . . C(17) F(1) 3.440(5) no . 2_656 C(17) O(1) 3.175(5) no . . C(17) O(1) 3.175(5) no . 2_656 C(17) O(3) 3.364(4) no . . C(17) O(3) 3.364(4) no . 2_656 Cl(1) H(13) 2.8057 no . . Cl(1) H(13) 2.8057 no . 4_565 Cl(2) H(15) 2.7852 no . . Cl(2) H(15) 2.7852 no . 2_656 O(1) H(9A) 3.2560 no . 4_565 O(1) H(9B) 3.4502 no . 4_565 N(1) H(9A) 2.7660 no . 4_565 N(1) H(9B) 2.7800 no . 4_565 C(5) H(9A) 2.5654 no . 4_565 C(5) H(9B) 2.7019 no . 4_565 C(6) H(9A) 3.0439 no . . C(6) H(9A) 3.0439 no . 4_565 C(6) H(9B) 3.2726 no . . C(6) H(9B) 3.2726 no . 4_565 C(7) H(9A) 2.8937 no . . C(7) H(9A) 2.8937 no . 4_565 C(7) H(9B) 3.0772 no . . C(7) H(9B) 3.0772 no . 4_565 C(7) H(9C) 3.4484 no . . C(7) H(9C) 3.4484 no . 4_565 C(8) H(9A) 3.0540 no . 2_655 C(8) H(9B) 2.9675 no . 2_655 C(8) H(9C) 2.3630 no . 2_655 C(9) H(9A) 3.2729 no . 2_655 C(9) H(9B) 2.8680 no . 2_655 C(9) H(9C) 1.8815 no . 2_655 C(10) H(12) 2.6742 no . . C(10) H(12) 2.6742 no . 4_565 C(11) H(12) 2.0335 no . 4_565 C(11) H(13) 3.2738 no . . C(11) H(13) 3.2738 no . 4_565 C(12) H(10A) 2.6649 no . . C(12) H(10A) 3.2412 no . 4_565 C(12) H(10B) 2.9013 no . . C(12) H(10B) 3.0263 no . 4_565 C(12) H(10C) 3.2974 no . . C(12) H(10C) 2.5939 no . 4_565 C(12) H(12) 3.2502 no . 4_565 C(13) H(13) 3.2687 no . 4_565 C(14) H(12) 3.2395 no . . C(14) H(12) 3.2395 no . 4_565 C(14) H(13) 2.0374 no . 4_565 C(15) H(15) 3.3054 no . 2_656 C(16) H(15) 2.0656 no . 2_656 C(16) H(15) 3.3185 no . 4_565 C(17) H(15) 2.7852 no . . C(17) H(15) 2.7852 no . 2_656 H(9A) H(9B) 3.5145 no . 2_655 H(9A) H(9C) 2.7703 no . 2_655 H(9B) H(9B) 3.4603 no . 2_655 H(9B) H(9C) 2.0955 no . 2_655 H(9C) H(9C) 1.2939 no . 2_655 H(10A) H(12) 2.5289 no . . H(10A) H(12) 3.4846 no . 4_565 H(10B) H(12) 2.9343 no . . H(10B) H(12) 3.1403 no . 4_565 H(10C) H(12) 3.5724 no . . H(10C) H(12) 2.4008 no . 4_565 H(12) H(13) 2.3337 no . . H(15) H(15) 2.4396 no . 4_565 Cl(1) H(15) 3.1290 no . 1_554 Cl(1) H(15) 3.1290 no . 4_564 F(1) H(12) 2.9877 no . 8_465 F(2) H(10A) 3.0460 no . 7_666 F(2) H(10B) 3.2646 no . 5_455 F(2) H(10B) 3.0697 no . 6_656 F(2) H(10B) 2.8311 no . 7_666 F(2) H(10B) 3.0413 no . 8_465 F(2) H(10C) 3.5836 no . 5_455 F(2) H(10C) 2.8101 no . 6_656 F(2) H(12) 2.9247 no . 8_465 F(4) H(9A) 3.4413 no . 3_666 F(4) H(13) 3.1312 no . 1_556 F(4) H(15) 3.3684 no . . F(5) H(9B) 3.5122 no . 6_656 F(5) H(12) 3.1990 no . 7_666 F(5) H(13) 2.6892 no . 7_666 O(2) H(10A) 2.7382 no . 7_666 O(2) H(10C) 2.6314 no . 6_656 O(2) H(12) 3.2332 no . 7_666 O(3) H(15) 3.0320 no . . O(4) H(9B) 2.5856 no . 6_656 O(4) H(12) 2.8275 no . 7_666 N(1) H(10A) 3.0437 no . . N(1) H(10C) 3.2048 no . 4_565 N(1) H(12) 3.2919 no . . N(1) H(15) 3.2625 no . . C(1) H(10C) 3.5512 no . 6_656 C(2) H(12) 3.3837 no . 8_465 C(3) H(9B) 3.5387 no . 6_656 C(5) H(10A) 3.1252 no . . C(5) H(10C) 3.3330 no . 4_565 C(5) H(12) 3.3328 no . . C(8) H(13) 3.4532 no . 4_565 C(10) H(10B) 3.2928 no . 2_756 C(10) H(10B) 3.2928 no . 3_766 C(12) H(9B) 3.5033 no . 4_565 C(13) H(9B) 3.3462 no . 4_565 C(16) H(15) 3.3185 no . 3_666 H(9A) F(4) 3.4413 no . 3_666 H(9B) F(5) 3.5122 no . 6_646 H(9B) O(4) 2.5856 no . 6_646 H(9B) C(3) 3.5387 no . 6_646 H(9B) C(12) 3.5033 no . 4_565 H(9B) C(13) 3.3462 no . 4_565 H(9B) H(12) 3.3475 no . 4_565 H(9B) H(13) 3.0729 no . 4_565 H(9C) H(13) 3.3990 no . 3_665 H(10A) F(2) 3.0460 no . 7_666 H(10A) O(2) 2.7382 no . 7_666 H(10A) N(1) 3.0437 no . . H(10A) C(5) 3.1252 no . . H(10B) F(2) 3.2646 no . 5_545 H(10B) F(2) 3.0697 no . 6_646 H(10B) F(2) 2.8311 no . 7_666 H(10B) F(2) 3.0413 no . 8_565 H(10B) C(10) 3.2928 no . 2_756 H(10B) H(10B) 2.3214 no . 2_756 H(10B) H(10B) 2.3419 no . 3_766 H(10B) H(10C) 3.5869 no . 3_766 H(10C) F(2) 3.5836 no . 5_545 H(10C) F(2) 2.8101 no . 6_646 H(10C) O(2) 2.6314 no . 6_646 H(10C) N(1) 3.2048 no . 4_565 H(10C) C(1) 3.5512 no . 6_646 H(10C) C(5) 3.3330 no . 4_565 H(10C) H(10B) 3.5869 no . 3_766 H(12) F(1) 2.9877 no . 8_565 H(12) F(2) 2.9247 no . 8_565 H(12) F(5) 3.1990 no . 7_666 H(12) O(2) 3.2332 no . 7_666 H(12) O(4) 2.8275 no . 7_666 H(12) N(1) 3.2919 no . . H(12) C(2) 3.3837 no . 8_565 H(12) C(5) 3.3328 no . . H(12) H(9B) 3.3475 no . 4_565 H(13) F(4) 3.1312 no . 1_554 H(13) F(5) 2.6892 no . 7_666 H(13) C(8) 3.4532 no . 4_565 H(13) H(9B) 3.0729 no . 4_565 H(13) H(9C) 3.3990 no . 3_665 H(15) Cl(1) 3.1290 no . 1_556 H(15) F(4) 3.3684 no . . H(15) O(3) 3.0320 no . . H(15) N(1) 3.2625 no . . H(15) C(16) 3.3185 no . 3_666 # 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 0.000 0.259 0.000 7 1 ' ' 2 0.000 0.501 0.000 309 33 ' ' 3 0.000 0.746 0.000 6 1 ' ' 4 0.500 0.000 0.000 310 33 ' ' 5 0.500 0.246 0.000 6 1 ' ' 6 0.500 0.754 0.000 6 0 ' ' _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 '- CCDC-840834_R2.cif' data_Ru2-CF3CO2-TCNQMeO2 _database_code_depnum_ccdc_archive 'CCDC 840834' #TrackingRef '- CCDC-840834_R2.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C37 H15 Cl F24 N4 O18 Ru4' _chemical_formula_moiety 'C37 H15 Cl F24 N4 O18 Ru4' _chemical_formula_weight 1699.24 _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 20.319(17) _cell_length_b 20.190(17) _cell_length_c 8.459(7) _cell_angle_alpha 90.0000 _cell_angle_beta 99.122(11) _cell_angle_gamma 90.0000 _cell_volume 3426(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 5043 _cell_measurement_theta_min 3.20 _cell_measurement_theta_max 27.40 _cell_measurement_temperature 93 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.070 _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1636.00 _exptl_absorpt_coefficient_mu 1.026 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.820 _exptl_absorpt_correction_T_max 0.931 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 93 _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 29.257 _diffrn_reflns_number 11150 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _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). In the process of refinement, the rigid bond Uij restraint (DELU) and the similar U restraint (SIMU) were treated for all atoms with (DELU 0.01 0.01) and (SIMU 0.01 0.02) (SIMU and DELU instructions in SHELXL97; Sheldrick, 2008). To fix the identical position for disordered atoms, the equal xyz constraint (EXYZ) was treated for Cl1 and C12. ; _reflns_number_total 3083 _reflns_number_gt 2396 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0707 _refine_ls_wR_factor_ref 0.2209 _refine_ls_number_restraints 178 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 3083 _refine_ls_number_parameters 210 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1489P)^2^+7.7387P] 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 2.990 _refine_diff_density_min -1.010 _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) ; Cl Cl 0.1484 0.1585 ; 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) ; 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 0.27860(3) 0.29842(3) 0.53614(6) 0.0411(4) Uani 1.0 8 d . . . Cl1 Cl 0.5000 0.3499(5) 0.5000 0.122(4) Uiso 0.5000 4 d . . . F1 F 0.4497(3) 0.1694(4) 0.8434(7) 0.0822(16) Uani 1.0 8 d . . . F2 F 0.4508(4) 0.1288(5) 0.6150(7) 0.129(3) Uani 1.0 8 d . . . F3 F 0.3978(4) 0.0820(4) 0.7735(11) 0.123(3) Uani 1.0 8 d . . . F4 F 0.3518(3) 0.2939(4) 0.0323(7) 0.087(2) Uani 1.0 8 d . . . F5 F 0.3100(3) 0.1966(3) -0.0175(7) 0.0839(19) Uani 1.0 8 d . . . F6 F 0.4041(3) 0.2098(4) 0.1472(7) 0.091(2) Uani 1.0 8 d . . . O1 O 0.3589(3) 0.2430(3) 0.6547(6) 0.0459(11) Uani 1.0 8 d . . . O2 O 0.3010(3) 0.1486(3) 0.5853(6) 0.0558(13) Uani 1.0 8 d . . . O3 O 0.3224(3) 0.2925(3) 0.3306(7) 0.0509(13) Uani 1.0 8 d . . . O4 O 0.2661(3) 0.1981(3) 0.2607(7) 0.0499(13) Uani 1.0 8 d . . . O5 O 0.4525(5) 0.6180(4) 0.8698(11) 0.0405(19) Uani 0.5000 8 d . . . N1 N 0.3326(4) 0.3954(4) 0.6223(8) 0.0561(16) Uani 1.0 8 d . . . C1 C 0.3511(4) 0.1830(5) 0.6456(8) 0.0461(14) Uani 1.0 8 d . . . C2 C 0.4134(5) 0.1391(5) 0.7228(10) 0.0630(19) Uani 1.0 8 d . . . C3 C 0.3070(4) 0.2425(5) 0.2415(8) 0.0535(16) Uani 1.0 8 d . . . C4 C 0.3432(4) 0.2355(6) 0.0984(10) 0.070(2) Uani 1.0 8 d . . . C5 C 0.3583(4) 0.4406(4) 0.6854(9) 0.0469(16) Uani 1.0 8 d . . . C6 C 0.3887(5) 0.5000 0.7553(11) 0.0379(18) Uani 1.0 4 d . . . C7 C 0.4429(4) 0.5000 0.8793(10) 0.0323(16) Uani 1.0 4 d . . . C8 C 0.4714(4) 0.5615(3) 0.9409(8) 0.0396(14) Uani 1.0 8 d . . . C9 C 0.4925(8) 0.6795(7) 0.9038(19) 0.054(4) Uani 0.5000 8 d . . . C10 C 0.4509(4) 0.4672(5) 0.3995(10) 0.072(3) Uani 1.0 8 d . . . C11 C 0.5000 0.4310(8) 0.5000 0.078(3) Uani 1.0 4 d . . . C12 C 0.5000 0.3499(5) 0.5000 0.168(11) Uiso 0.5000 4 d . . . H10 H 0.4171 0.4441 0.3304 0.0869 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 0.0361(5) 0.0478(5) 0.0343(5) -0.0111(2) -0.0101(3) 0.0050(2) F1 0.063(4) 0.107(5) 0.065(3) 0.020(3) -0.027(3) -0.011(3) F2 0.102(5) 0.222(8) 0.059(4) 0.088(5) -0.001(3) 0.003(4) F3 0.073(4) 0.091(5) 0.185(7) 0.001(4) -0.040(4) 0.042(5) F4 0.059(4) 0.151(6) 0.051(4) -0.005(3) 0.013(3) 0.029(3) F5 0.066(4) 0.145(6) 0.040(3) 0.005(3) 0.006(3) -0.011(3) F6 0.053(3) 0.162(7) 0.056(4) 0.023(3) 0.003(3) 0.007(3) O1 0.034(3) 0.062(3) 0.037(3) -0.013(2) -0.010(2) 0.003(3) O2 0.056(3) 0.054(3) 0.050(3) -0.013(3) -0.014(3) -0.002(3) O3 0.039(3) 0.077(4) 0.033(3) -0.015(3) -0.003(3) 0.016(2) O4 0.041(3) 0.070(4) 0.034(3) -0.005(2) -0.006(3) -0.003(2) O5 0.036(5) 0.030(4) 0.048(5) 0.007(3) -0.015(4) -0.005(4) N1 0.050(4) 0.053(4) 0.057(4) -0.009(3) -0.016(3) 0.016(3) C1 0.038(3) 0.070(4) 0.031(3) -0.018(3) 0.009(3) -0.010(3) C2 0.051(4) 0.079(5) 0.054(4) 0.003(4) -0.008(4) 0.000(4) C3 0.038(4) 0.085(5) 0.033(3) -0.004(3) -0.011(3) 0.007(3) C4 0.042(4) 0.119(6) 0.047(4) 0.003(4) 0.001(3) 0.003(4) C5 0.036(4) 0.056(4) 0.042(4) -0.010(3) -0.015(3) 0.006(3) C6 0.033(4) 0.040(4) 0.038(4) 0.0000 -0.007(4) 0.0000 C7 0.031(4) 0.031(4) 0.034(4) 0.0000 0.002(3) 0.0000 C8 0.046(4) 0.036(3) 0.033(3) 0.001(3) -0.006(3) -0.002(3) C9 0.058(8) 0.028(5) 0.065(8) -0.002(6) -0.024(7) 0.002(6) C10 0.047(5) 0.120(7) 0.053(5) -0.018(4) 0.019(4) -0.013(4) C11 0.058(6) 0.104(8) 0.080(7) 0.0000 0.036(5) 0.0000 #============================================================================== _computing_data_collection 'CrystalClear (Rigaku, ????)' _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 2.3070(17) yes . 7_556 Ru1 O1 2.097(5) yes . . Ru1 O2 2.071(6) yes . 7_556 Ru1 O3 2.078(6) yes . . Ru1 O4 2.067(6) yes . 7_556 Ru1 N1 2.306(7) yes . . Cl1 C11 1.638(19) yes . . F1 C2 1.312(10) yes . . F2 C2 1.294(12) yes . . F3 C2 1.287(13) yes . . F4 C4 1.327(14) yes . . F5 C4 1.350(11) yes . . F6 C4 1.345(11) yes . . O1 C1 1.222(10) yes . . O2 C1 1.270(9) yes . . O3 C3 1.270(10) yes . . O4 C3 1.251(10) yes . . O5 C8 1.319(11) yes . . O5 C9 1.488(17) yes . . N1 C5 1.140(10) yes . . C1 C2 1.596(12) yes . . C3 C4 1.519(12) yes . . C5 C6 1.433(9) yes . . C6 C7 1.395(12) yes . . C7 C8 1.433(8) yes . . C7 C8 1.433(8) yes . 4_565 C8 C8 1.408(9) yes . 2_657 C10 C10 1.324(14) yes . 4_565 C10 C11 1.408(12) yes . . C11 C12 1.638(19) yes . . C10 H10 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 89.75(15) yes 7_556 . . Ru1 Ru1 O2 89.13(16) yes 7_556 . 7_556 Ru1 Ru1 O3 89.67(15) yes 7_556 . . Ru1 Ru1 O4 88.86(15) yes 7_556 . 7_556 Ru1 Ru1 N1 176.45(18) yes 7_556 . . O1 Ru1 O2 178.6(2) yes . . 7_556 O1 Ru1 O3 88.0(2) yes . . . O1 Ru1 O4 91.8(2) yes . . 7_556 O1 Ru1 N1 90.4(3) yes . . . O2 Ru1 O3 91.1(3) yes 7_556 . . O2 Ru1 O4 89.0(3) yes 7_556 . 7_556 O2 Ru1 N1 90.8(3) yes 7_556 . . O3 Ru1 O4 178.5(2) yes . . 7_556 O3 Ru1 N1 93.9(3) yes . . . O4 Ru1 N1 87.6(3) yes 7_556 . . Ru1 O1 C1 114.6(5) yes . . . Ru1 O2 C1 115.5(5) yes 7_556 . . Ru1 O3 C3 116.4(5) yes . . . Ru1 O4 C3 118.2(5) yes 7_556 . . C8 O5 C9 121.5(9) yes . . . Ru1 N1 C5 170.6(7) yes . . . O1 C1 O2 130.9(7) yes . . . O1 C1 C2 116.0(7) yes . . . O2 C1 C2 113.1(7) yes . . . F1 C2 F2 107.5(8) yes . . . F1 C2 F3 107.2(8) yes . . . F1 C2 C1 111.8(8) yes . . . F2 C2 F3 107.0(9) yes . . . F2 C2 C1 108.5(7) yes . . . F3 C2 C1 114.4(8) yes . . . O3 C3 O4 126.8(7) yes . . . O3 C3 C4 116.2(8) yes . . . O4 C3 C4 117.0(8) yes . . . F4 C4 F5 107.2(7) yes . . . F4 C4 F6 107.2(8) yes . . . F4 C4 C3 111.5(9) yes . . . F5 C4 F6 109.1(9) yes . . . F5 C4 C3 112.5(8) yes . . . F6 C4 C3 109.2(7) yes . . . N1 C5 C6 176.1(8) yes . . . C5 C6 C5 113.6(7) yes . . 4_565 C5 C6 C7 123.2(4) yes . . . C5 C6 C7 123.2(4) yes 4_565 . . C6 C7 C8 119.9(4) yes . . . C6 C7 C8 119.9(4) yes . . 4_565 C8 C7 C8 120.1(7) yes . . 4_565 O5 C8 C7 120.8(7) yes . . . O5 C8 C8 118.2(7) yes . . 2_657 C7 C8 C8 119.9(6) yes . . 2_657 C10 C10 C11 121.3(9) yes 4_565 . . Cl1 C11 C10 121.3(7) yes . . . Cl1 C11 C10 121.3(7) yes . . 2_656 Cl1 C11 C12 0.000 yes . . . C10 C11 C10 117.5(13) yes . . 2_656 C10 C11 C12 121.3(7) yes . . . C10 C11 C12 121.3(7) yes 2_656 . . C10 C10 H10 119.372 no 4_565 . . C11 C10 H10 119.362 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 F1 3.079(8) no . 2_657 F1 O1 2.689(8) no . . F1 O2 3.461(8) no . . F1 C9 3.190(16) no . 4_565 F2 O1 3.020(10) no . . F2 O2 3.040(9) no . . F3 O1 3.457(10) no . . F3 O2 2.686(9) no . . F4 O3 2.684(9) no . . F4 O4 3.402(9) no . . F5 O3 3.500(8) no . . F5 O4 2.646(9) no . . F6 O3 2.961(9) no . . F6 O4 3.114(9) no . . O1 C3 3.487(9) no . . O1 C9 3.528(16) no . 4_565 O2 C3 3.489(10) no . . O2 C3 3.581(10) no . 7_556 O3 C1 3.440(10) no . . O3 C1 3.597(10) no . 7_556 O4 C1 3.449(9) no . . O4 C1 3.558(10) no . 7_556 O5 O5 2.690(12) no . 2_657 O5 N1 2.961(10) no . 4_565 O5 C5 2.559(11) no . 4_565 O5 C6 2.810(10) no . . O5 C9 2.404(17) no . 2_657 N1 C5 3.381(11) no . 4_565 N1 C7 3.558(9) no . . C1 C3 3.599(10) no . . C5 C8 2.895(9) no . 4_565 C7 C7 2.838(11) no . 2_657 C8 C9 2.763(16) no . 2_657 C9 C9 1.61(3) no . 2_657 Cl1 O5 3.478(10) no . 3_666 Cl1 O5 3.478(10) no . 4_565 Cl1 C9 3.494(17) no . 3_666 Cl1 C9 3.494(17) no . 4_565 F1 F5 3.288(9) no . 1_556 F1 F6 2.981(9) no . 1_556 F1 F6 3.069(9) no . 2_656 F1 C4 3.550(12) no . 1_556 F2 F2 3.003(10) no . 2_656 F3 F3 3.312(11) no . 4_555 F3 F5 3.558(10) no . 1_556 F4 F5 3.274(9) no . 7_555 F4 O1 3.380(8) no . 1_554 F4 O4 3.165(8) no . 7_555 F4 O5 3.183(12) no . 4_564 F4 C9 3.170(18) no . 3_666 F4 C9 3.261(19) no . 4_564 F5 F1 3.288(9) no . 1_554 F5 F3 3.558(10) no . 1_554 F5 F4 3.274(9) no . 7_555 F5 F5 3.302(9) no . 7_555 F5 O1 3.230(8) no . 1_554 F5 O2 3.474(8) no . 1_554 F5 O3 3.469(8) no . 7_555 F5 O4 3.184(8) no . 7_555 F5 C1 3.107(10) no . 1_554 F5 C2 3.471(12) no . 1_554 F5 C3 3.054(9) no . 7_555 F5 C4 3.370(11) no . 7_555 F6 F1 2.981(9) no . 1_554 F6 F1 3.069(9) no . 2_656 F6 C9 3.144(17) no . 3_666 O1 F4 3.380(8) no . 1_556 O1 F5 3.230(8) no . 1_556 O2 F5 3.474(8) no . 1_556 O3 F5 3.469(8) no . 7_555 O4 F4 3.165(8) no . 7_555 O4 F5 3.184(8) no . 7_555 O5 Cl1 3.478(10) no . 3_666 O5 F4 3.183(12) no . 4_566 O5 C11 3.557(11) no . 3_666 O5 C12 3.478(10) no . 3_666 N1 C10 3.587(12) no . . C1 F5 3.107(10) no . 1_556 C2 F5 3.471(12) no . 1_556 C3 F5 3.054(9) no . 7_555 C4 F1 3.550(12) no . 1_554 C4 F5 3.370(11) no . 7_555 C5 C10 3.335(12) no . . C5 C11 3.496(8) no . . C6 C10 3.507(14) no . . C6 C10 3.507(14) no . 4_565 C7 C8 2.459(9) no . 3_667 C7 C10 3.503(13) no . 2_656 C7 C10 3.503(13) no . 3_666 C8 C8 2.855(9) no . 3_667 C8 C10 3.545(12) no . 3_666 C9 Cl1 3.494(17) no . 3_666 C9 F4 3.170(18) no . 3_666 C9 F4 3.261(19) no . 4_566 C9 F6 3.144(17) no . 3_666 C9 C12 3.494(17) no . 3_666 C10 N1 3.587(12) no . . C10 C5 3.335(12) no . . C10 C6 3.507(14) no . . C10 C7 3.503(13) no . 2_656 C10 C8 3.545(12) no . 3_666 C10 C10 2.748(12) no . 3_666 C10 C11 2.382(17) no . 3_666 C11 O5 3.557(11) no . 3_666 C11 O5 3.557(11) no . 4_565 C11 C5 3.496(8) no . . C11 C5 3.496(8) no . 2_656 C11 C10 2.382(17) no . 3_666 C11 C11 2.79(3) no . 3_666 C12 O5 3.478(10) no . 3_666 C12 O5 3.478(10) no . 4_565 C12 C9 3.494(17) no . 3_666 C12 C9 3.494(17) no . 4_565 Cl1 H10 2.7834 no . . Cl1 H10 2.7834 no . 2_656 C10 H10 3.2687 no . 2_656 C11 H10 2.0488 no . 2_656 C11 H10 3.2380 no . 4_565 C12 H10 2.7834 no . . C12 H10 2.7834 no . 2_656 H10 H10 2.2564 no . 4_565 O5 H10 3.5899 no . 3_666 N1 H10 3.3700 no . . C5 H10 3.4048 no . . C8 H10 3.4729 no . 3_666 C11 H10 3.2380 no . 3_666 H10 O5 3.5899 no . 3_666 H10 N1 3.3700 no . . H10 C5 3.4048 no . . H10 C8 3.4729 no . 3_666 H10 C11 3.2380 no . 3_666 # 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 0.500 0.000 0.129 479 97 ' ' 2 0.000 0.500 -0.177 479 97 ' ' _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 '- CCDC-859333_R2.cif' data_Rh2-CF3CO2-TCNQMe2 _database_code_depnum_ccdc_archive 'CCDC 859333' #TrackingRef '- CCDC-859333_R2.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C38 H18 F24 N4 O16 Rh4' _chemical_formula_moiety 'C38 H18 F24 N4 O16 Rh4' _chemical_formula_weight 1654.16 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 8.459(5) _cell_length_b 20.195(10) _cell_length_c 19.371(11) _cell_angle_alpha 90.0000 _cell_angle_beta 99.512(11) _cell_angle_gamma 90.0000 _cell_volume 3264(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 8218 _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 30.87 _cell_measurement_temperature 97 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.149 _exptl_crystal_size_mid 0.127 _exptl_crystal_size_min 0.033 _exptl_crystal_density_diffrn 1.683 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596.00 _exptl_absorpt_coefficient_mu 1.116 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.808 _exptl_absorpt_correction_T_max 0.964 #============================================================================== # 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 20994 _diffrn_reflns_av_R_equivalents 0.0781 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measured_fraction_theta_full 0.987 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _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). In the process of refinement, the rigid bond Uij restraint (DELU) and the similar U restraint (SIMU) were treated for all atoms with (DELU 0.01 0.01) and (SIMU 0.01 0.02) (SIMU and DELU instructions in SHELXL97; Sheldrick, 2008). ; _reflns_number_total 5661 _reflns_number_gt 3876 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.1135 _refine_ls_wR_factor_ref 0.3333 _refine_ls_number_restraints 333 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 5643 _refine_ls_number_parameters 397 _refine_ls_goodness_of_fit_ref 1.206 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.2000P)^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 2.500 _refine_diff_density_min -1.950 _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) ; 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 Rh1 Rh 0.54015(9) 0.31528(5) 0.26713(5) 0.0640(5) Uani 1.0 4 d . . . Rh2 Rh 0.46424(10) 0.20999(5) 0.21355(5) 0.0642(5) Uani 1.0 4 d . . . F1 F 0.2012(17) 0.4092(9) 0.0811(8) 0.193(5) Uani 1.0 4 d . . . F2 F 0.3660(12) 0.3687(8) 0.0244(7) 0.184(5) Uani 1.0 4 d . . . F3 F 0.1488(13) 0.3247(7) 0.0349(7) 0.158(4) Uani 1.0 4 d . . . F4 F 0.0565(13) 0.3174(7) 0.3519(7) 0.137(4) Uani 1.0 4 d . . . F5 F -0.0020(10) 0.2230(6) 0.3109(5) 0.127(4) Uani 1.0 4 d . . . F6 F 0.1631(12) 0.2385(8) 0.4050(5) 0.147(4) Uani 1.0 4 d . . . F7 F 0.7919(15) 0.1128(8) 0.4024(7) 0.167(4) Uani 1.0 4 d . . . F8 F 0.6316(12) 0.1621(7) 0.4581(6) 0.153(4) Uani 1.0 4 d . . . F9 F 0.8548(11) 0.2041(7) 0.4492(6) 0.139(4) Uani 1.0 4 d . . . F10 F 1.0117(11) 0.3050(8) 0.1767(6) 0.153(4) Uani 1.0 4 d . . . F11 F 0.8510(15) 0.2812(11) 0.0809(6) 0.212(6) Uani 1.0 4 d . . . F12 F 0.9487(16) 0.2037(10) 0.1355(9) 0.197(5) Uani 1.0 4 d . . . O1 O 0.4113(9) 0.3591(5) 0.1784(5) 0.078(2) Uani 1.0 4 d . . . O2 O 0.3400(8) 0.2604(5) 0.1291(4) 0.0685(19) Uani 1.0 4 d . . . O3 O 0.3392(10) 0.3134(5) 0.3117(5) 0.078(2) Uani 1.0 4 d . . . O4 O 0.2683(9) 0.2139(5) 0.2629(5) 0.075(2) Uani 1.0 4 d . . . O5 O 0.6637(8) 0.2656(5) 0.3506(4) 0.0695(18) Uani 1.0 4 d . . . O6 O 0.5904(9) 0.1644(5) 0.3002(5) 0.081(2) Uani 1.0 4 d . . . O7 O 0.7341(10) 0.3132(6) 0.2189(5) 0.089(3) Uani 1.0 4 d . . . O8 O 0.6640(10) 0.2155(6) 0.1677(5) 0.093(3) Uani 1.0 4 d . . . N1 N 0.6241(12) 0.4108(6) 0.3170(6) 0.078(3) Uani 1.0 4 d . . . N2 N 0.6164(12) 0.6167(6) 0.3317(6) 0.079(3) Uani 1.0 4 d . . . C1 C 0.3511(13) 0.3264(8) 0.1347(7) 0.075(3) Uani 1.0 4 d . . . C2 C 0.2623(18) 0.3550(12) 0.0658(9) 0.108(4) Uani 1.0 4 d . . . C3 C 0.2556(14) 0.2605(9) 0.3014(7) 0.084(3) Uani 1.0 4 d . . . C4 C 0.1156(17) 0.2569(11) 0.3407(9) 0.107(3) Uani 1.0 4 d . . . C5 C 0.6586(14) 0.2064(8) 0.3471(8) 0.077(3) Uani 1.0 4 d . . . C6 C 0.7386(17) 0.1678(10) 0.4159(8) 0.097(3) Uani 1.0 4 d . . . C7 C 0.7501(15) 0.2635(11) 0.1796(7) 0.102(3) Uani 1.0 4 d . . . C8 C 0.893(2) 0.2630(15) 0.1417(10) 0.138(4) Uani 1.0 4 d . . . C9 C 0.6765(14) 0.4523(7) 0.3489(6) 0.068(3) Uani 1.0 4 d . . . C10 C 0.7512(14) 0.5085(6) 0.3846(6) 0.061(2) Uani 1.0 4 d . . . C11 C 0.6770(13) 0.5706(6) 0.3592(6) 0.065(3) Uani 1.0 4 d . . . C12 C 0.8733(12) 0.5052(5) 0.4423(6) 0.0527(19) Uani 1.0 4 d . . . C13 C 0.9392(11) 0.4410(5) 0.4672(6) 0.057(3) Uani 1.0 4 d . . . C14 C 0.882(3) 0.3723(12) 0.4525(14) 0.076(6) Uani 0.5000 4 d . . . C15 C 0.9420(11) 0.5646(5) 0.4775(5) 0.051(2) Uani 1.0 4 d . . . C16 C 0.900(3) 0.6341(10) 0.4641(11) 0.061(5) Uani 0.5000 4 d . . . C17 C 0.524(3) 0.3576(9) 0.4971(8) 0.143(6) Uani 1.0 4 d . . . C18 C 0.5119(17) 0.4291(8) 0.5001(6) 0.088(4) Uani 1.0 4 d . . . C19 C 0.4079(17) 0.4651(8) 0.4504(7) 0.081(3) Uani 1.0 4 d . . . C20 C 0.3967(16) 0.5298(8) 0.4509(7) 0.083(4) Uani 1.0 4 d . . . H14A H 0.8428 0.3544 0.4934 0.0913 Uiso 0.5000 4 calc R . . H14B H 0.9710 0.3449 0.4420 0.0913 Uiso 0.5000 4 calc R . . H14C H 0.7954 0.3722 0.4121 0.0913 Uiso 0.5000 4 calc R . . H16A H 0.9937 0.6584 0.4542 0.0731 Uiso 0.5000 4 calc R . . H16B H 0.8636 0.6532 0.5053 0.0731 Uiso 0.5000 4 calc R . . H16C H 0.8134 0.6372 0.4237 0.0731 Uiso 0.5000 4 calc R . . H17A H 0.4192 0.3378 0.4998 0.1712 Uiso 1.0 4 calc R . . H17B H 0.6029 0.3419 0.5364 0.1712 Uiso 1.0 4 calc R . . H17C H 0.5573 0.3446 0.4529 0.1712 Uiso 1.0 4 calc R . . H19 H 0.3418 0.4414 0.4143 0.0977 Uiso 1.0 4 calc R . . H20 H 0.3211 0.5501 0.4155 0.0998 Uiso 1.0 4 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 0.0417(6) 0.0876(8) 0.0609(7) 0.0070(4) 0.0032(4) -0.0167(5) Rh2 0.0430(6) 0.0844(8) 0.0635(7) 0.0092(4) 0.0035(4) -0.0157(5) F1 0.177(11) 0.217(11) 0.175(11) 0.062(9) 0.000(8) -0.005(10) F2 0.081(6) 0.319(14) 0.151(9) 0.016(8) 0.013(6) 0.060(10) F3 0.101(7) 0.225(11) 0.133(9) -0.011(7) -0.021(6) 0.020(8) F4 0.086(7) 0.198(9) 0.135(9) 0.024(6) 0.041(6) -0.016(7) F5 0.057(5) 0.221(10) 0.106(6) 0.002(5) 0.025(4) 0.001(6) F6 0.102(7) 0.250(12) 0.087(6) -0.007(8) 0.015(5) 0.020(7) F7 0.163(10) 0.184(9) 0.143(9) 0.059(8) -0.003(7) 0.022(7) F8 0.098(7) 0.249(12) 0.117(7) 0.001(7) 0.033(5) 0.050(8) F9 0.079(6) 0.223(10) 0.106(7) 0.001(6) -0.010(5) 0.007(7) F10 0.054(5) 0.290(12) 0.117(7) 0.014(6) 0.018(5) 0.042(7) F11 0.126(9) 0.443(17) 0.071(6) 0.001(10) 0.026(6) 0.029(9) F12 0.095(8) 0.326(12) 0.186(12) 0.034(8) 0.065(8) -0.056(9) O1 0.055(4) 0.088(5) 0.084(5) -0.008(4) -0.006(4) -0.008(4) O2 0.038(4) 0.103(6) 0.064(4) 0.002(4) 0.007(3) -0.013(4) O3 0.048(4) 0.126(7) 0.061(5) 0.019(4) 0.010(4) -0.018(4) O4 0.040(4) 0.114(6) 0.072(5) -0.003(4) 0.007(4) -0.004(4) O5 0.041(4) 0.098(5) 0.069(4) 0.007(4) 0.008(3) -0.011(4) O6 0.051(4) 0.105(6) 0.085(5) -0.001(4) -0.001(4) -0.007(4) O7 0.038(4) 0.171(8) 0.058(5) -0.010(4) 0.005(3) -0.005(5) O8 0.045(4) 0.178(9) 0.058(5) 0.029(4) 0.012(4) -0.022(5) N1 0.065(5) 0.090(5) 0.072(6) 0.004(5) -0.008(5) -0.005(5) N2 0.069(6) 0.087(6) 0.071(6) -0.008(5) -0.015(5) -0.001(5) C1 0.041(5) 0.110(6) 0.079(6) 0.001(5) 0.021(4) -0.007(5) C2 0.058(6) 0.166(9) 0.098(8) 0.013(6) 0.005(5) 0.008(7) C3 0.047(4) 0.137(7) 0.067(5) 0.011(5) 0.003(4) -0.010(5) C4 0.056(6) 0.181(8) 0.085(6) 0.012(6) 0.014(5) 0.007(7) C5 0.043(5) 0.111(6) 0.080(5) 0.004(5) 0.016(4) -0.005(5) C6 0.059(6) 0.151(8) 0.080(6) 0.012(6) 0.007(5) 0.018(6) C7 0.041(5) 0.205(9) 0.059(5) 0.012(5) 0.006(4) -0.008(6) C8 0.056(6) 0.275(11) 0.085(7) 0.022(6) 0.018(5) 0.004(7) C9 0.060(5) 0.081(6) 0.059(6) 0.003(5) -0.001(5) -0.005(5) C10 0.050(5) 0.076(5) 0.056(5) 0.000(4) 0.004(4) -0.001(4) C11 0.058(5) 0.076(6) 0.055(5) -0.012(5) -0.007(4) -0.003(5) C12 0.041(4) 0.062(4) 0.056(5) 0.002(4) 0.010(4) -0.002(4) C13 0.046(5) 0.059(5) 0.066(6) 0.001(4) 0.012(4) -0.014(5) C14 0.070(12) 0.068(8) 0.087(14) -0.009(10) 0.003(11) 0.001(11) C15 0.047(5) 0.055(5) 0.053(5) 0.001(4) 0.012(4) 0.008(4) C16 0.057(10) 0.060(7) 0.056(11) 0.002(9) -0.020(9) -0.003(9) C17 0.238(17) 0.102(9) 0.096(11) 0.014(11) 0.050(12) 0.003(9) C18 0.122(9) 0.097(7) 0.052(6) 0.018(7) 0.038(6) -0.011(6) C19 0.085(7) 0.106(7) 0.059(6) -0.000(6) 0.029(5) -0.005(6) C20 0.070(7) 0.118(8) 0.063(7) 0.018(7) 0.015(6) 0.008(7) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'Il Milione (Burla, et al., 2007)' _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 Rh2 2.4064(17) yes . . Rh1 O1 2.074(9) yes . . Rh1 O3 2.030(9) yes . . Rh1 O5 2.039(8) yes . . Rh1 O7 2.018(9) yes . . Rh1 N1 2.221(12) yes . . Rh2 O2 2.061(8) yes . . Rh2 O4 2.046(9) yes . . Rh2 O6 2.051(9) yes . . Rh2 O8 2.037(9) yes . . Rh2 N2 2.141(12) yes . 2_645 F1 C2 1.27(3) yes . . F2 C2 1.31(3) yes . . F3 C2 1.21(2) yes . . F4 C4 1.35(3) yes . . F5 C4 1.27(2) yes . . F6 C4 1.298(19) yes . . F7 C6 1.24(3) yes . . F8 C6 1.32(2) yes . . F9 C6 1.307(19) yes . . F10 C8 1.40(3) yes . . F11 C8 1.23(3) yes . . F12 C8 1.30(4) yes . . O1 C1 1.127(16) yes . . O2 C1 1.339(18) yes . . O3 C3 1.278(18) yes . . O4 C3 1.217(18) yes . . O5 C5 1.197(19) yes . . O6 C5 1.305(17) yes . . O7 C7 1.28(3) yes . . O8 C7 1.21(2) yes . . N1 C9 1.091(17) yes . . N2 C11 1.150(16) yes . . C1 C2 1.53(3) yes . . C3 C4 1.51(2) yes . . C5 C6 1.60(2) yes . . C7 C8 1.51(3) yes . . C9 C10 1.422(17) yes . . C10 C11 1.452(16) yes . . C10 C12 1.392(15) yes . . C12 C13 1.462(14) yes . . C12 C15 1.453(14) yes . . C13 C14 1.48(3) yes . . C13 C15 1.346(13) yes . 3_766 C15 C16 1.46(3) yes . . C17 C18 1.45(3) yes . . C18 C19 1.395(18) yes . . C18 C20 1.393(19) yes . 3_666 C19 C20 1.31(2) yes . . C14 H14A 0.980 no . . C14 H14B 0.980 no . . C14 H14C 0.980 no . . C16 H16A 0.980 no . . C16 H16B 0.980 no . . C16 H16C 0.980 no . . C17 H17A 0.980 no . . C17 H17B 0.980 no . . C17 H17C 0.980 no . . C19 H19 0.950 no . . C20 H20 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 Rh2 Rh1 O1 87.3(3) yes . . . Rh2 Rh1 O3 89.1(3) yes . . . Rh2 Rh1 O5 88.4(3) yes . . . Rh2 Rh1 O7 87.8(3) yes . . . Rh2 Rh1 N1 176.9(3) yes . . . O1 Rh1 O3 89.9(4) yes . . . O1 Rh1 O5 175.7(4) yes . . . O1 Rh1 O7 88.9(4) yes . . . O1 Rh1 N1 94.4(4) yes . . . O3 Rh1 O5 90.5(4) yes . . . O3 Rh1 O7 176.7(4) yes . . . O3 Rh1 N1 93.5(4) yes . . . O5 Rh1 O7 90.4(4) yes . . . O5 Rh1 N1 89.9(4) yes . . . O7 Rh1 N1 89.6(4) yes . . . Rh1 Rh2 O2 88.3(3) yes . . . Rh1 Rh2 O4 86.7(3) yes . . . Rh1 Rh2 O6 88.7(3) yes . . . Rh1 Rh2 O8 87.6(4) yes . . . Rh1 Rh2 N2 176.6(3) yes . . 2_645 O2 Rh2 O4 90.3(3) yes . . . O2 Rh2 O6 177.0(4) yes . . . O2 Rh2 O8 88.7(4) yes . . . O2 Rh2 N2 91.4(4) yes . . 2_645 O4 Rh2 O6 89.3(4) yes . . . O4 Rh2 O8 174.3(5) yes . . . O4 Rh2 N2 89.9(4) yes . . 2_645 O6 Rh2 O8 91.4(4) yes . . . O6 Rh2 N2 91.6(4) yes . . 2_645 O8 Rh2 N2 95.8(5) yes . . 2_645 Rh1 O1 C1 118.9(10) yes . . . Rh2 O2 C1 114.0(7) yes . . . Rh1 O3 C3 115.5(9) yes . . . Rh2 O4 C3 118.5(9) yes . . . Rh1 O5 C5 115.9(8) yes . . . Rh2 O6 C5 112.8(9) yes . . . Rh1 O7 C7 117.7(9) yes . . . Rh2 O8 C7 118.4(10) yes . . . Rh1 N1 C9 169.9(10) yes . . . Rh2 N2 C11 171.5(10) yes 2_655 . . O1 C1 O2 131.3(13) yes . . . O1 C1 C2 122.0(15) yes . . . O2 C1 C2 106.7(12) yes . . . F1 C2 F2 107.4(19) yes . . . F1 C2 F3 103.4(15) yes . . . F1 C2 C1 106.4(15) yes . . . F2 C2 F3 111.1(16) yes . . . F2 C2 C1 109.3(12) yes . . . F3 C2 C1 118.4(18) yes . . . O3 C3 O4 129.6(12) yes . . . O3 C3 C4 115.0(14) yes . . . O4 C3 C4 115.3(14) yes . . . F4 C4 F5 106.2(13) yes . . . F4 C4 F6 99.7(15) yes . . . F4 C4 C3 112.3(16) yes . . . F5 C4 F6 112.2(17) yes . . . F5 C4 C3 114.8(15) yes . . . F6 C4 C3 110.6(12) yes . . . O5 C5 O6 134.1(13) yes . . . O5 C5 C6 115.7(13) yes . . . O6 C5 C6 110.0(14) yes . . . F7 C6 F8 111.3(17) yes . . . F7 C6 F9 109.6(13) yes . . . F7 C6 C5 112.3(14) yes . . . F8 C6 F9 106.2(14) yes . . . F8 C6 C5 108.7(12) yes . . . F9 C6 C5 108.6(15) yes . . . O7 C7 O8 128.4(13) yes . . . O7 C7 C8 117.7(17) yes . . . O8 C7 C8 113.8(17) yes . . . F10 C8 F11 111(2) yes . . . F10 C8 F12 111.0(15) yes . . . F10 C8 C7 109.2(16) yes . . . F11 C8 F12 104(2) yes . . . F11 C8 C7 109.8(14) yes . . . F12 C8 C7 113(2) yes . . . N1 C9 C10 174.3(14) yes . . . C9 C10 C11 113.1(10) yes . . . C9 C10 C12 124.3(10) yes . . . C11 C10 C12 122.4(10) yes . . . N2 C11 C10 172.3(12) yes . . . C10 C12 C13 120.0(9) yes . . . C10 C12 C15 121.6(9) yes . . . C13 C12 C15 118.4(9) yes . . . C12 C13 C14 132.3(12) yes . . . C12 C13 C15 122.0(9) yes . . 3_766 C14 C13 C15 104.6(12) yes . . 3_766 C12 C15 C13 119.5(9) yes . . 3_766 C12 C15 C16 129.9(11) yes . . . C13 C15 C16 110.5(11) yes 3_766 . . C17 C18 C19 122.0(12) yes . . . C17 C18 C20 125.8(13) yes . . 3_666 C19 C18 C20 112.1(13) yes . . 3_666 C18 C19 C20 123.5(13) yes . . . C18 C20 C19 124.4(13) yes 3_666 . . C13 C14 H14A 109.478 no . . . C13 C14 H14B 109.473 no . . . C13 C14 H14C 109.467 no . . . H14A C14 H14B 109.475 no . . . H14A C14 H14C 109.472 no . . . H14B C14 H14C 109.462 no . . . C15 C16 H16A 109.473 no . . . C15 C16 H16B 109.464 no . . . C15 C16 H16C 109.473 no . . . H16A C16 H16B 109.474 no . . . H16A C16 H16C 109.468 no . . . H16B C16 H16C 109.476 no . . . C18 C17 H17A 109.473 no . . . C18 C17 H17B 109.471 no . . . C18 C17 H17C 109.473 no . . . H17A C17 H17B 109.470 no . . . H17A C17 H17C 109.465 no . . . H17B C17 H17C 109.475 no . . . C18 C19 H19 118.250 no . . . C20 C19 H19 118.259 no . . . C18 C20 H20 117.795 no 3_666 . . C19 C20 H20 117.790 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 2.576(16) no . . F1 O2 3.304(19) no . . F2 O1 2.952(16) no . . F2 O2 3.015(17) no . . F3 O1 3.332(14) no . . F3 O2 2.580(14) no . . F4 O3 2.636(14) no . . F4 O4 3.401(16) no . . F5 O3 3.413(13) no . . F5 O4 2.614(13) no . . F6 O3 2.943(15) no . . F6 O4 3.070(14) no . . F7 O5 3.368(17) no . . F7 O6 2.608(15) no . . F8 O5 2.994(15) no . . F8 O6 3.022(14) no . . F9 O5 2.604(13) no . . F9 O6 3.442(13) no . . F9 C14 3.41(3) no . . F10 O7 2.616(13) no . . F10 O8 3.433(15) no . . F11 O7 3.068(16) no . . F11 O8 2.823(18) no . . F12 O7 3.43(2) no . . F12 O8 2.597(17) no . . O1 C3 3.523(17) no . . O1 C7 3.452(18) no . . O2 C3 3.528(15) no . . O2 C7 3.445(14) no . . O2 C16 3.56(2) no . 2_645 O3 C1 3.457(17) no . . O3 C5 3.438(16) no . . O4 C1 3.520(18) no . . O4 C5 3.435(14) no . . O5 C3 3.428(14) no . . O5 C7 3.508(17) no . . O5 C14 3.28(3) no . . O6 C3 3.436(16) no . . O6 C7 3.510(19) no . . O7 C1 3.389(14) no . . O7 C5 3.427(19) no . . O8 C1 3.445(17) no . . O8 C5 3.487(17) no . . N1 C11 3.341(17) no . . N1 C12 3.503(14) no . . N1 C14 3.22(3) no . . N2 C9 3.367(18) no . . N2 C12 3.584(14) no . . N2 C16 3.23(2) no . . C1 C7 3.576(18) no . . C3 C5 3.550(17) no . . C9 C13 2.925(14) no . . C9 C14 2.92(3) no . . C10 C14 3.17(3) no . . C10 C16 3.12(3) no . . C11 C15 2.932(13) no . . C11 C16 2.84(3) no . . C12 C12 2.838(14) no . 3_766 C13 C13 2.815(14) no . 3_766 C14 C16 2.25(3) no . 3_766 C15 C15 2.870(14) no . 3_766 C18 C18 2.87(3) no . 3_666 C19 C19 2.667(18) no . 3_666 C20 C20 2.650(18) no . 3_666 F1 F10 3.38(2) no . 1_455 F2 F6 3.416(18) no . 4_554 F2 F8 2.834(16) no . 4_554 F3 F6 2.844(17) no . 4_554 F3 F9 2.813(14) no . 4_454 F3 F10 3.178(18) no . 1_455 F3 F11 2.942(19) no . 1_455 F3 C8 3.47(3) no . 1_455 F4 F9 3.573(17) no . 1_455 F4 F10 3.361(17) no . 1_455 F4 O5 3.480(13) no . 1_455 F4 O7 3.429(13) no . 1_455 F4 C13 3.597(17) no . 1_455 F4 C14 2.85(3) no . 1_455 F5 F7 3.486(18) no . 1_455 F5 F9 3.141(15) no . 1_455 F5 F10 3.100(17) no . 1_455 F5 F12 3.38(2) no . 1_455 F5 O5 3.170(12) no . 1_455 F5 O7 3.188(14) no . 1_455 F5 C5 3.084(16) no . 1_455 F5 C6 3.42(2) no . 1_455 F5 C7 3.126(16) no . 1_455 F5 C8 3.35(2) no . 1_455 F6 F2 3.416(18) no . 4_555 F6 F3 2.844(17) no . 4_555 F6 F9 2.960(15) no . 1_455 F7 F5 3.486(18) no . 1_655 F8 F2 2.834(16) no . 4_555 F8 F11 2.993(16) no . 4_555 F9 F3 2.813(14) no . 4_655 F9 F4 3.573(17) no . 1_655 F9 F5 3.141(15) no . 1_655 F9 F6 2.960(15) no . 1_655 F9 F11 2.574(16) no . 4_555 F9 C4 3.46(2) no . 1_655 F10 F1 3.38(2) no . 1_655 F10 F3 3.178(18) no . 1_655 F10 F4 3.361(17) no . 1_655 F10 F5 3.100(17) no . 1_655 F10 O1 3.547(13) no . 1_655 F10 O2 3.197(13) no . 1_655 F10 O3 3.485(12) no . 1_655 F10 O4 3.111(14) no . 1_655 F10 C1 3.141(16) no . 1_655 F10 C2 3.41(3) no . 1_655 F10 C3 3.041(16) no . 1_655 F10 C4 3.30(2) no . 1_655 F11 F3 2.942(19) no . 1_655 F11 F8 2.993(16) no . 4_554 F11 F9 2.574(16) no . 4_554 F11 C6 3.34(2) no . 4_554 F12 F5 3.38(2) no . 1_655 F12 O2 3.525(16) no . 1_655 F12 O4 3.352(16) no . 1_655 F12 C16 2.86(3) no . 2_745 O1 F10 3.547(13) no . 1_455 O2 F10 3.197(13) no . 1_455 O2 F12 3.525(16) no . 1_455 O3 F10 3.485(12) no . 1_455 O4 F10 3.111(14) no . 1_455 O4 F12 3.352(16) no . 1_455 O5 F4 3.480(13) no . 1_655 O5 F5 3.170(12) no . 1_655 O7 F4 3.429(13) no . 1_655 O7 F5 3.188(14) no . 1_655 N1 C19 3.576(18) no . . C1 F10 3.141(16) no . 1_455 C2 F10 3.41(3) no . 1_455 C3 F10 3.041(16) no . 1_455 C4 F9 3.46(2) no . 1_455 C4 F10 3.30(2) no . 1_455 C5 F5 3.084(16) no . 1_655 C6 F5 3.42(2) no . 1_655 C6 F11 3.34(2) no . 4_555 C7 F5 3.126(16) no . 1_655 C8 F3 3.47(3) no . 1_655 C8 F5 3.35(2) no . 1_655 C9 C18 3.476(18) no . . C9 C19 3.25(2) no . . C10 C19 3.472(19) no . . C10 C20 3.479(19) no . . C11 C18 3.379(18) no . 3_666 C11 C20 3.294(19) no . . C12 C19 3.460(19) no . 3_666 C12 C20 3.399(18) no . 3_666 C13 F4 3.597(17) no . 1_655 C13 C20 3.525(18) no . 3_666 C14 F4 2.85(3) no . 1_655 C14 C17 3.30(4) no . . C14 C18 3.60(3) no . . C15 C19 3.526(18) no . 3_666 C16 F12 2.86(3) no . 2_755 C17 C14 3.30(4) no . . C18 C9 3.476(18) no . . C18 C11 3.379(18) no . 3_666 C18 C14 3.60(3) no . . C19 N1 3.576(18) no . . C19 C9 3.25(2) no . . C19 C10 3.472(19) no . . C19 C12 3.460(19) no . 3_666 C19 C15 3.526(18) no . 3_666 C20 C10 3.479(19) no . . C20 C11 3.294(19) no . . C20 C12 3.399(18) no . 3_666 C20 C13 3.525(18) no . 3_666 Rh1 H14C 3.4451 no . . Rh2 H16C 3.5611 no . 2_645 F3 H16A 3.5869 no . 2_645 F3 H16B 3.5494 no . 2_645 F9 H14A 3.1603 no . . F9 H14B 3.0204 no . . F9 H14C 3.4901 no . . F9 H16A 3.4735 no . 3_766 O2 H16B 3.5992 no . 2_645 O2 H16C 2.9118 no . 2_645 O5 H14A 3.4322 no . . O5 H14B 3.3072 no . . O5 H14C 2.6194 no . . N1 H14C 2.2847 no . . N2 H16C 2.2683 no . . C9 H14A 3.5242 no . . C9 H14B 3.5602 no . . C9 H14C 2.1723 no . . C10 H14C 2.8168 no . . C10 H16C 2.7343 no . . C11 H16A 3.4756 no . . C11 H16B 3.4364 no . . C11 H16C 2.0560 no . . C12 H14A 3.2260 no . . C12 H14B 3.3407 no . . C12 H14C 2.8035 no . . C12 H16A 3.2538 no . . C12 H16B 3.2350 no . . C12 H16C 2.7275 no . . C13 H16A 2.5253 no . 3_766 C13 H16B 2.5271 no . 3_766 C13 H16C 3.1427 no . 3_766 C14 H16A 2.0309 no . 3_766 C14 H16B 2.2300 no . 3_766 C14 H16C 3.2214 no . 3_766 C15 H14A 2.4436 no . 3_766 C15 H14B 2.4358 no . 3_766 C15 H14C 3.0923 no . 3_766 C16 H14A 2.2102 no . 3_766 C16 H14B 2.0068 no . 3_766 C16 H14C 3.2207 no . 3_766 C17 H19 2.6440 no . . C17 H20 2.7072 no . 3_666 C18 H19 3.2310 no . 3_666 C18 H20 3.2227 no . . C19 H17A 2.7386 no . . C19 H17B 3.2830 no . . C19 H17C 2.7383 no . . C19 H20 3.1819 no . 3_666 C20 H17A 3.1607 no . 3_666 C20 H17B 2.6024 no . 3_666 C20 H17C 3.1321 no . 3_666 C20 H19 3.1844 no . 3_666 C20 H20 3.5999 no . 3_666 H14A H16A 1.5950 no . 3_766 H14A H16B 2.4845 no . 3_766 H14A H16C 3.0858 no . 3_766 H14B H16A 1.9833 no . 3_766 H14B H16B 1.5900 no . 3_766 H14B H16C 2.9418 no . 3_766 H14C H16A 2.9560 no . 3_766 H14C H16B 3.1008 no . 3_766 H17A H19 2.6811 no . . H17A H20 3.3832 no . 3_666 H17B H19 3.5757 no . . H17B H20 2.4162 no . 3_666 H17C H19 2.6929 no . . H17C H20 3.3470 no . 3_666 H19 H20 2.2039 no . . F4 H14B 2.0732 no . 1_455 F4 H14C 2.8844 no . 1_455 F4 H16B 2.8003 no . 3_666 F4 H19 3.5488 no . . F5 H14B 3.5721 no . 1_455 F6 H14B 2.8560 no . 1_455 F6 H16B 2.8256 no . 3_666 F6 H17A 3.2825 no . . F11 H14A 3.2143 no . 4_554 F11 H16A 2.9386 no . 2_745 F11 H17B 3.2746 no . 4_554 F12 H14A 2.9890 no . 4_554 F12 H16A 2.0917 no . 2_745 F12 H16B 3.5263 no . 2_745 F12 H16C 2.8162 no . 2_745 F12 H17B 3.3509 no . 4_554 O2 H17A 3.3477 no . 4_554 O3 H17C 3.1015 no . . O3 H19 3.2594 no . . O5 H17C 2.8064 no . . O8 H17B 2.7647 no . 4_554 N1 H17C 3.0860 no . . N1 H19 3.3349 no . . N2 H17A 3.4517 no . 3_666 N2 H17B 3.4987 no . 3_666 N2 H20 3.4683 no . . C4 H14B 3.0501 no . 1_455 C4 H16B 3.4721 no . 3_666 C7 H17B 3.5545 no . 4_554 C8 H16A 3.0714 no . 2_745 C9 H17C 3.2355 no . . C9 H19 3.2944 no . . C11 H17A 3.5037 no . 3_666 C11 H20 3.3933 no . . C13 H20 3.4191 no . 3_666 C14 H17B 3.1425 no . . C14 H17C 2.8066 no . . C15 H19 3.4392 no . 3_666 C16 H17A 2.9512 no . 3_666 C17 H14A 2.7117 no . . C17 H14C 3.0532 no . . C17 H16B 3.2769 no . 3_666 C17 H16C 3.4563 no . 3_666 C18 H14A 3.2023 no . . C18 H14C 3.3665 no . . C18 H16B 3.5708 no . 3_666 C18 H16C 3.5891 no . 3_666 C19 H16B 3.5161 no . 3_666 C20 H14A 3.3847 no . 3_666 H14A F11 3.2143 no . 4_555 H14A F12 2.9890 no . 4_555 H14A C17 2.7117 no . . H14A C18 3.2023 no . . H14A C20 3.3847 no . 3_666 H14A H17B 2.3305 no . . H14A H17C 2.4206 no . . H14A H20 3.0916 no . 3_666 H14B F4 2.0732 no . 1_655 H14B F5 3.5721 no . 1_655 H14B F6 2.8560 no . 1_655 H14B C4 3.0501 no . 1_655 H14B H17C 3.5401 no . . H14C F4 2.8844 no . 1_655 H14C C17 3.0532 no . . H14C C18 3.3665 no . . H14C H17B 3.1803 no . . H14C H17C 2.3484 no . . H16A F11 2.9386 no . 2_755 H16A F12 2.0917 no . 2_755 H16A C8 3.0714 no . 2_755 H16A H17B 3.3870 no . 3_766 H16B F4 2.8003 no . 3_666 H16B F6 2.8256 no . 3_666 H16B F12 3.5263 no . 2_755 H16B C4 3.4721 no . 3_666 H16B C17 3.2769 no . 3_666 H16B C18 3.5708 no . 3_666 H16B C19 3.5161 no . 3_666 H16B H17A 2.3846 no . 3_666 H16B H19 3.1592 no . 3_666 H16C F12 2.8162 no . 2_755 H16C C17 3.4563 no . 3_666 H16C C18 3.5891 no . 3_666 H16C H17A 2.6981 no . 3_666 H17A F6 3.2825 no . . H17A O2 3.3477 no . 4_555 H17A N2 3.4517 no . 3_666 H17A C11 3.5037 no . 3_666 H17A C16 2.9512 no . 3_666 H17A H16B 2.3846 no . 3_666 H17A H16C 2.6981 no . 3_666 H17B F11 3.2746 no . 4_555 H17B F12 3.3509 no . 4_555 H17B O8 2.7647 no . 4_555 H17B N2 3.4987 no . 3_666 H17B C7 3.5545 no . 4_555 H17B C14 3.1425 no . . H17B H14A 2.3305 no . . H17B H14C 3.1803 no . . H17B H16A 3.3870 no . 3_766 H17C O3 3.1015 no . . H17C O5 2.8064 no . . H17C N1 3.0860 no . . H17C C9 3.2355 no . . H17C C14 2.8066 no . . H17C H14A 2.4206 no . . H17C H14B 3.5401 no . . H17C H14C 2.3484 no . . H19 F4 3.5488 no . . H19 O3 3.2594 no . . H19 N1 3.3349 no . . H19 C9 3.2944 no . . H19 C15 3.4392 no . 3_666 H19 H16B 3.1592 no . 3_666 H20 N2 3.4683 no . . H20 C11 3.3933 no . . H20 C13 3.4191 no . 3_666 H20 H14A 3.0916 no . 3_666 # 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 -0.020 0.500 0.000 466 108 ' ' 2 0.092 0.000 0.500 466 109 ' ' _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 '- CCDC-859334_R2.cif' data_Rh2-CF3CO2-TCNQMeO2 _database_code_depnum_ccdc_archive 'CCDC 859334' #TrackingRef '- CCDC-859334_R2.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C38 H18 F24 N4 O18 Rh4' _chemical_formula_moiety 'C38 H18 F24 N4 O18 Rh4' _chemical_formula_weight 1686.16 _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 20.005(5) _cell_length_b 20.070(5) _cell_length_c 8.3580(19) _cell_angle_alpha 90.0000 _cell_angle_beta 99.956(4) _cell_angle_gamma 90.0000 _cell_volume 3305.2(13) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4316 _cell_measurement_theta_min 1.45 _cell_measurement_theta_max 30.86 _cell_measurement_temperature 97 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.092 _exptl_crystal_size_mid 0.067 _exptl_crystal_size_min 0.048 _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1628.00 _exptl_absorpt_coefficient_mu 1.105 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.847 _exptl_absorpt_correction_T_max 0.948 #============================================================================== # 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 10920 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _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). In the process of refinement, the rigid bond Uij restraint (DELU) and the similar U restraint (SIMU) were treated for all atoms with (DELU 0.01 0.01) and (SIMU 0.01 0.02) (SIMU and DELU instructions in SHELXL97; Sheldrick, 2008). ; _reflns_number_total 2975 _reflns_number_gt 2549 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1826 _refine_ls_number_restraints 173 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 2969 _refine_ls_number_parameters 212 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1226P)^2^+6.6970P] 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 1.090 _refine_diff_density_min -1.260 _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) ; 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 Rh1 Rh 0.22077(2) 0.30149(2) 0.96155(5) 0.0428(3) Uani 1.0 8 d . . . F1 F 0.3096(3) 0.3022(3) 0.4884(7) 0.0963(18) Uani 1.0 8 d . . . F2 F 0.3499(3) 0.2032(3) 0.5379(7) 0.0925(18) Uani 1.0 8 d . . . F3 F 0.4037(3) 0.2883(4) 0.6524(7) 0.1024(18) Uani 1.0 8 d . . . F4 F 0.4561(4) 0.3609(5) 1.1265(8) 0.159(3) Uani 1.0 8 d . . . F5 F 0.4498(4) 0.3266(5) 1.3518(8) 0.131(3) Uani 1.0 8 d . . . F6 F 0.4014(4) 0.4137(5) 1.2711(13) 0.175(4) Uani 1.0 8 d . . . O1 O 0.2664(3) 0.3025(2) 0.7631(6) 0.0505(11) Uani 1.0 8 d . . . O2 O 0.3211(3) 0.2058(3) 0.8331(6) 0.0537(11) Uani 1.0 8 d . . . O3 O 0.3034(2) 0.3504(3) 1.0858(5) 0.0533(10) Uani 1.0 8 d . . . O4 O 0.35865(18) 0.2534(3) 1.1580(5) 0.0485(10) Uani 1.0 8 d . . . O5 O 0.0481(4) 0.3814(4) 0.6259(8) 0.0368(14) Uani 0.5000 8 d . . . N1 N 0.1694(3) 0.3946(3) 0.8826(6) 0.0541(12) Uani 1.0 8 d . . . C1 C 0.3053(3) 0.2570(4) 0.7454(7) 0.0540(13) Uani 1.0 8 d . . . C2 C 0.3424(4) 0.2625(5) 0.6011(8) 0.0671(17) Uani 1.0 8 d . . . C3 C 0.3521(4) 0.3152(4) 1.1486(8) 0.0499(13) Uani 1.0 8 d . . . C4 C 0.4149(4) 0.3554(5) 1.2278(9) 0.0666(16) Uani 1.0 8 d . . . C5 C 0.1432(3) 0.4391(3) 0.8224(7) 0.0458(13) Uani 1.0 8 d . . . C6 C 0.1121(4) 0.5000 0.7497(9) 0.0399(15) Uani 1.0 4 d . . . C7 C 0.0575(3) 0.5000 0.6244(8) 0.0337(13) Uani 1.0 4 d . . . C8 C 0.0278(3) 0.4385(3) 0.5620(6) 0.0366(11) Uani 1.0 8 d . . . C9 C 0.0104(6) 0.3189(6) 0.5788(16) 0.047(3) Uani 0.5000 8 d . . . C10 C 0.0000 0.3551(6) 1.0000 0.098(4) Uani 1.0 4 d . . . C11 C 0.0000 0.4297(5) 1.0000 0.057(2) Uani 1.0 4 d . . . C12 C 0.0487(3) 0.4658(4) 1.1014(7) 0.0560(15) Uani 1.0 8 d . . . H10A H 0.0349 0.3388 0.9406 0.1170 Uiso 0.5000 8 calc R . . H10B H -0.0446 0.3388 0.9473 0.1170 Uiso 0.5000 8 calc R . . H10C H 0.0097 0.3388 1.1122 0.1170 Uiso 0.5000 8 calc R . . H12 H 0.0830 0.4427 1.1730 0.0672 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 0.0330(4) 0.0548(4) 0.0359(4) 0.00862(16) -0.0078(3) -0.00569(16) F1 0.083(4) 0.143(5) 0.062(3) -0.001(3) 0.012(3) 0.006(3) F2 0.072(4) 0.140(5) 0.065(3) 0.009(3) 0.011(3) -0.026(3) F3 0.063(3) 0.164(6) 0.081(4) -0.022(3) 0.014(3) -0.020(4) F4 0.114(5) 0.258(9) 0.105(4) -0.081(6) 0.022(4) -0.016(5) F5 0.091(4) 0.183(6) 0.101(4) -0.033(4) -0.032(4) 0.013(4) F6 0.105(5) 0.149(6) 0.246(9) -0.003(5) -0.035(5) -0.083(6) O1 0.040(3) 0.069(3) 0.039(3) 0.0042(17) -0.0034(18) 0.0010(17) O2 0.036(3) 0.082(3) 0.040(3) 0.0122(18) -0.0019(18) -0.0127(19) O3 0.046(2) 0.059(3) 0.048(3) 0.0076(18) -0.0115(18) 0.0008(19) O4 0.0318(19) 0.069(3) 0.0397(19) 0.0108(18) -0.0073(16) -0.0034(19) O5 0.033(3) 0.029(3) 0.043(4) 0.004(3) -0.007(3) 0.004(3) N1 0.045(3) 0.056(3) 0.053(3) 0.007(3) -0.014(2) -0.012(3) C1 0.033(3) 0.087(4) 0.037(3) 0.003(3) -0.007(2) -0.011(3) C2 0.044(3) 0.112(5) 0.042(3) -0.003(3) -0.001(3) -0.008(3) C3 0.041(3) 0.073(4) 0.036(3) 0.013(3) 0.008(3) 0.006(3) C4 0.045(3) 0.093(5) 0.056(4) -0.009(3) -0.007(3) -0.003(4) C5 0.034(3) 0.060(3) 0.038(3) 0.008(3) -0.008(3) -0.005(3) C6 0.027(3) 0.055(4) 0.036(4) 0.0000 0.001(3) 0.0000 C7 0.028(3) 0.038(3) 0.033(4) 0.0000 0.001(3) 0.0000 C8 0.040(3) 0.033(3) 0.036(3) 0.0059(19) 0.003(2) -0.0022(19) C9 0.036(5) 0.029(4) 0.067(6) -0.008(4) -0.014(5) 0.007(5) C10 0.092(8) 0.069(6) 0.148(11) 0.0000 0.068(8) 0.0000 C11 0.046(4) 0.066(5) 0.065(5) 0.0000 0.024(4) 0.0000 C12 0.040(3) 0.084(4) 0.047(3) 0.011(3) 0.014(3) 0.015(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 2.4068(7) yes . 7_557 Rh1 O1 2.027(5) yes . . Rh1 O2 2.040(5) yes . 7_557 Rh1 O3 2.044(4) yes . . Rh1 O4 2.046(4) yes . 7_557 Rh1 N1 2.179(6) yes . . F1 C2 1.318(9) yes . . F2 C2 1.322(11) yes . . F3 C2 1.331(9) yes . . F4 C4 1.284(11) yes . . F5 C4 1.283(10) yes . . F6 C4 1.268(13) yes . . O1 C1 1.226(8) yes . . O2 C1 1.270(8) yes . . O3 C3 1.243(8) yes . . O4 C3 1.250(9) yes . . O5 C8 1.301(8) yes . . O5 C9 1.481(13) yes . . N1 C5 1.111(8) yes . . C1 C2 1.526(9) yes . . C3 C4 1.542(10) yes . . C5 C6 1.456(7) yes . . C6 C7 1.376(10) yes . . C7 C8 1.428(6) yes . . C7 C8 1.428(6) yes . 4_565 C8 C8 1.383(7) yes . 2_556 C9 C9 1.311(18) yes . 2_556 C10 C11 1.497(16) yes . . C11 C12 1.380(8) yes . . C11 C12 1.380(8) yes . 2_557 C12 C12 1.374(10) yes . 4_565 C10 H10A 0.980 no . . C10 H10A 0.980 no . 2_557 C10 H10B 0.980 no . . C10 H10B 0.980 no . 2_557 C10 H10C 0.980 no . . C10 H10C 0.980 no . 2_557 C12 H12 0.950 no . . H10A H10B 0.924 no . 2_557 H10A H10C 0.924 no . 2_557 H10B H10C 0.924 no . 2_557 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 87.73(12) yes 7_557 . . Rh1 Rh1 O2 87.98(13) yes 7_557 . 7_557 Rh1 Rh1 O3 87.92(13) yes 7_557 . . Rh1 Rh1 O4 88.20(12) yes 7_557 . 7_557 Rh1 Rh1 N1 177.67(14) yes 7_557 . . O1 Rh1 O2 175.71(18) yes . . 7_557 O1 Rh1 O3 88.38(17) yes . . . O1 Rh1 O4 91.58(17) yes . . 7_557 O1 Rh1 N1 89.96(19) yes . . . O2 Rh1 O3 91.17(18) yes 7_557 . . O2 Rh1 O4 88.59(17) yes 7_557 . 7_557 O2 Rh1 N1 94.33(19) yes 7_557 . . O3 Rh1 O4 176.12(17) yes . . 7_557 O3 Rh1 N1 92.30(18) yes . . . O4 Rh1 N1 91.58(18) yes 7_557 . . Rh1 O1 C1 118.5(4) yes . . . Rh1 O2 C1 116.6(4) yes 7_557 . . Rh1 O3 C3 116.6(5) yes . . . Rh1 O4 C3 116.1(4) yes 7_557 . . C8 O5 C9 121.9(7) yes . . . Rh1 N1 C5 170.8(5) yes . . . O1 C1 O2 129.2(6) yes . . . O1 C1 C2 116.6(6) yes . . . O2 C1 C2 114.2(6) yes . . . F1 C2 F2 109.6(6) yes . . . F1 C2 F3 108.2(8) yes . . . F1 C2 C1 111.0(6) yes . . . F2 C2 F3 108.5(7) yes . . . F2 C2 C1 110.8(7) yes . . . F3 C2 C1 108.7(6) yes . . . O3 C3 O4 131.0(6) yes . . . O3 C3 C4 114.0(7) yes . . . O4 C3 C4 115.0(6) yes . . . F4 C4 F5 104.6(7) yes . . . F4 C4 F6 107.5(9) yes . . . F4 C4 C3 109.3(7) yes . . . F5 C4 F6 107.3(8) yes . . . F5 C4 C3 113.6(8) yes . . . F6 C4 C3 114.0(7) yes . . . N1 C5 C6 176.4(6) yes . . . C5 C6 C5 114.2(6) yes . . 4_565 C5 C6 C7 122.9(4) yes . . . C5 C6 C7 122.9(4) yes 4_565 . . C6 C7 C8 120.2(3) yes . . . C6 C7 C8 120.2(3) yes . . 4_565 C8 C7 C8 119.5(5) yes . . 4_565 O5 C8 C7 122.1(5) yes . . . O5 C8 C8 117.5(5) yes . . 2_556 C7 C8 C8 120.2(5) yes . . 2_556 O5 C9 C9 109.0(10) yes . . 2_556 C10 C11 C12 121.6(5) yes . . . C10 C11 C12 121.6(5) yes . . 2_557 C12 C11 C12 116.8(8) yes . . 2_557 C11 C12 C12 121.6(6) yes . . 4_565 C11 C10 H10A 109.486 no . . . C11 C10 H10A 109.486 no . . 2_557 C11 C10 H10B 109.485 no . . . C11 C10 H10B 109.485 no . . 2_557 C11 C10 H10C 109.486 no . . . C11 C10 H10C 109.486 no . . 2_557 H10A C10 H10A 141.028 no . . 2_557 H10A C10 H10B 109.458 no . . . H10A C10 H10B 56.244 no . . 2_557 H10A C10 H10C 109.453 no . . . H10A C10 H10C 56.249 no . . 2_557 H10A C10 H10B 56.244 no 2_557 . . H10A C10 H10B 109.458 no 2_557 . 2_557 H10A C10 H10C 56.249 no 2_557 . . H10A C10 H10C 109.453 no 2_557 . 2_557 H10B C10 H10B 141.030 no . . 2_557 H10B C10 H10C 109.458 no . . . H10B C10 H10C 56.244 no . . 2_557 H10B C10 H10C 56.244 no 2_557 . . H10B C10 H10C 109.458 no 2_557 . 2_557 H10C C10 H10C 141.027 no . . 2_557 C11 C12 H12 119.205 no . . . C12 C12 H12 119.171 no 4_565 . . C10 H10A H10B 61.881 no . . 2_557 C10 H10A H10C 61.875 no . . 2_557 H10B H10A H10C 120.002 no 2_557 . 2_557 C10 H10B H10A 61.875 no . . 2_557 C10 H10B H10C 61.875 no . . 2_557 H10A H10B H10C 119.996 no 2_557 . 2_557 C10 H10C H10A 61.876 no . . 2_557 C10 H10C H10B 61.881 no . . 2_557 H10A H10C H10B 120.002 no 2_557 . 2_557 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 2.589(8) no . . F1 O2 3.445(8) no . . F2 O1 3.376(8) no . . F2 O2 2.630(8) no . . F3 O1 3.060(8) no . . F3 O2 2.936(8) no . . F4 O3 3.021(8) no . . F4 O4 2.950(10) no . . F5 O3 3.391(8) no . . F5 O4 2.662(8) no . . F5 C9 3.056(14) no . 7_557 F6 F6 3.465(13) no . 4_565 F6 O3 2.609(9) no . . F6 O4 3.420(10) no . . O1 C3 3.387(8) no . . O1 C3 3.516(9) no . 7_557 O2 C3 3.405(8) no . . O2 C3 3.519(8) no . 7_557 O3 C1 3.413(8) no . . O3 C1 3.525(8) no . 7_557 O4 O5 3.591(8) no . 7_557 O4 C1 3.430(7) no . . O4 C1 3.517(7) no . 7_557 O4 C9 3.438(12) no . 7_557 O5 O5 2.595(9) no . 2_556 O5 N1 2.960(8) no . . O5 C5 2.564(8) no . . O5 C6 2.814(8) no . . N1 C5 3.404(9) no . 4_565 N1 C7 3.532(7) no . . C1 C3 3.537(9) no . . C5 C8 2.886(7) no . . C7 C7 2.822(9) no . 2_556 C8 C9 2.724(12) no . 2_556 F1 F1 3.206(9) no . 7_556 F1 F2 3.163(9) no . 7_556 F1 F5 3.242(10) no . 1_554 F1 F6 3.582(12) no . 1_554 F1 O1 3.169(7) no . 7_556 F1 O2 3.414(7) no . 7_556 F1 O3 3.483(7) no . 1_554 F1 O4 3.238(8) no . 1_554 F1 C1 2.994(8) no . 7_556 F1 C2 3.273(9) no . 7_556 F1 C3 3.114(9) no . 1_554 F1 C4 3.451(10) no . 1_554 F2 F1 3.163(9) no . 7_556 F2 O1 3.120(7) no . 7_556 F2 O4 3.365(7) no . 1_554 F2 O5 3.143(10) no . 7_556 F2 C9 3.147(14) no . 7_556 F2 C9 3.199(13) no . 8_555 F3 F4 3.409(9) no . 2_657 F3 F5 2.924(10) no . 1_554 F3 F5 3.036(9) no . 2_657 F3 C9 3.530(14) no . 7_556 F3 C9 3.163(14) no . 8_555 F4 F3 3.409(9) no . 2_657 F4 F4 2.975(11) no . 2_657 F5 F1 3.242(10) no . 1_556 F5 F3 2.924(10) no . 1_556 F5 F3 3.036(9) no . 2_657 F5 F5 2.907(9) no . 2_658 F5 C2 3.486(11) no . 1_556 F5 C9 3.577(14) no . 8_556 F6 F1 3.582(12) no . 1_556 O1 F1 3.169(7) no . 7_556 O1 F2 3.120(7) no . 7_556 O2 F1 3.414(7) no . 7_556 O3 F1 3.483(7) no . 1_556 O4 F1 3.238(8) no . 1_556 O4 F2 3.365(7) no . 1_556 O5 F2 3.143(10) no . 7_556 O5 C10 3.467(8) no . . O5 C11 3.561(8) no . . N1 C12 3.570(9) no . . C1 F1 2.994(8) no . 7_556 C2 F1 3.273(9) no . 7_556 C2 F5 3.486(11) no . 1_554 C3 F1 3.114(9) no . 1_556 C4 F1 3.451(10) no . 1_556 C5 C11 3.452(6) no . . C5 C12 3.291(9) no . . C6 C12 3.466(11) no . . C6 C12 3.466(11) no . 4_565 C7 C8 2.437(7) no . 3_566 C7 C12 3.452(10) no . 2_557 C7 C12 3.452(10) no . 3_567 C8 C8 2.828(7) no . 3_566 C8 C12 3.470(9) no . 2_557 C9 F2 3.147(14) no . 7_556 C9 F2 3.199(13) no . 8_455 C9 F3 3.530(14) no . 7_556 C9 F3 3.163(14) no . 8_455 C9 F5 3.577(14) no . 8_454 C10 O5 3.467(8) no . . C10 O5 3.467(8) no . 2_557 C11 O5 3.561(8) no . . C11 O5 3.561(8) no . 2_557 C11 C5 3.452(6) no . . C11 C5 3.452(6) no . 2_557 C11 C11 2.822(15) no . 3_567 C11 C12 2.405(11) no . 3_567 C12 N1 3.570(9) no . . C12 C5 3.291(9) no . . C12 C6 3.466(11) no . . C12 C7 3.452(10) no . 2_557 C12 C8 3.470(9) no . 2_557 C12 C11 2.405(11) no . 3_567 C12 C12 2.723(9) no . 3_567 C10 H12 2.6663 no . . C10 H12 2.6663 no . 2_557 C11 H12 2.0216 no . 2_557 C11 H12 3.2524 no . 4_565 C12 H10A 2.8717 no . . C12 H10A 3.0342 no . 2_557 C12 H10B 3.2865 no . . C12 H10B 2.5792 no . 2_557 C12 H10C 2.6706 no . . C12 H10C 3.2126 no . 2_557 C12 H12 3.2135 no . 2_557 H10A H12 2.8984 no . . H10A H12 3.1682 no . 2_557 H10B H12 3.5718 no . . H10B H12 2.3835 no . 2_557 H10C H12 2.5494 no . . H10C H12 3.4553 no . 2_557 H12 H12 2.3004 no . 4_565 F3 H10B 3.5729 no . 8_555 F3 H10C 3.4926 no . 7_557 O2 H10A 3.2863 no . 7_557 O2 H10B 2.8374 no . 8_555 O2 H10C 3.4555 no . 7_557 O2 H12 3.5498 no . 7_557 O4 H10A 3.0405 no . 7_557 O4 H10B 3.3842 no . 8_555 O5 H10A 2.8209 no . . O5 H10C 2.7811 no . 2_557 O5 H12 3.5698 no . 2_557 N1 H10A 3.0291 no . . N1 H10B 3.2763 no . 2_557 N1 H12 3.3552 no . . C5 H10A 3.2340 no . . C5 H12 3.3562 no . . C8 H10C 3.5625 no . 2_557 C8 H12 3.3948 no . 2_557 C9 H10A 3.0050 no . . C9 H10B 3.4670 no . . C9 H10C 2.7109 no . 2_557 C11 H12 3.2524 no . 3_567 H10A O2 3.2863 no . 7_557 H10A O4 3.0405 no . 7_557 H10A O5 2.8209 no . . H10A N1 3.0291 no . . H10A C5 3.2340 no . . H10A C9 3.0050 no . . H10B F3 3.5729 no . 8_455 H10B O2 2.8374 no . 8_455 H10B O4 3.3842 no . 8_455 H10B N1 3.2763 no . 2_557 H10B C9 3.4670 no . . H10C F3 3.4926 no . 7_557 H10C O2 3.4555 no . 7_557 H10C O5 2.7811 no . 2_557 H10C C8 3.5625 no . 2_557 H10C C9 2.7109 no . 2_557 H12 O2 3.5498 no . 7_557 H12 O5 3.5698 no . 2_557 H12 N1 3.3552 no . . H12 C5 3.3562 no . . H12 C8 3.3948 no . 2_557 H12 C11 3.2524 no . 3_567 # 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 0.000 0.000 -0.024 462 84 ' ' 2 0.500 0.500 0.084 462 84 ' ' _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 #==============================================================================