# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr William Michael Laidlaw' _publ_contact_author_email MICHAEL.LAIDLAW@CHEM.OX.AC.UK _publ_section_title ; Solvent dependence of the g-anisotropy in the ESR of cyanide-bridged mixed-valence complexes ; loop_ _publ_author_name 'William Laidlaw' 'Robert G. Denning' 'Jennifer C. Green' 'Damien M. Murphy' # The atom H6 forms a bifurcated hydrogen bond, resulting in a short contact # between O9 and O9 2_656 of 2.896(6) \%A. # Attachment 'CrRu.cif' data_CrRuTf2 _database_code_depnum_ccdc_archive 'CCDC 691876' #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? _exptl_crystal_thermal_history ; The material was crystallised at ambient temperature. A suitable crystal was cooled rapidly to 150K for single-crystal X-ray diffraction analysis. ; _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall #============================================================= _cell_length_a 13.1853(2) _cell_angle_alpha 90 _cell_length_b 11.6464(2) _cell_angle_beta 112.0394(8) _cell_length_c 16.6937(3) _cell_angle_gamma 90 _cell_volume 2376.18(7) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'Cr ' 0.3209 0.6236 10.6406 6.1038 7.3537 0.3920 3.3240 20.2626 1.4922 98.7399 1.1832 International_Tables_Vol_IV_Table_2.2B 'F ' 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'Ru ' -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 International_Tables_Vol_IV_Table_2.2B 'S ' 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 4 _chemical_formula_sum ' C8 H15 Cr F6 N6 O11 Ru1 S2 ' _chemical_formula_moiety ' C6 H15 Cr N6 O5 Ru, 2(C F3 O3 S) ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 702.43 _cell_measurement_reflns_used 20225 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description ' fragment ' _exptl_crystal_colour ' blue ' _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.15 _exptl_crystal_density_diffrn 1.963 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1388 _exptl_absorpt_coefficient_mu 1.375 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.85 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 20225 _reflns_number_total 5398 # 5660 unique reflections including systematic absences _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_theta_min 5.140 _diffrn_reflns_theta_max 27.490 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.490 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -17 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _refine_diff_density_min -0.57 _refine_diff_density_max 0.61 _refine_ls_number_reflns 4261 _refine_ls_number_restraints 0 _refine_ls_number_parameters 376 #_refine_ls_R_factor_ref 0.0260 _refine_ls_wR_factor_ref 0.0279 _refine_ls_goodness_of_fit_ref 1.1251 #_reflns_number_all 5398 _refine_ls_R_factor_all 0.0361 _refine_ls_wR_factor_all 0.0399 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 4261 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_gt 0.0279 _refine_ls_shift/su_max 0.034379 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.292 0.106 0.0457 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Ru1 Ru 0.513523(14) 0.228263(16) 0.683924(12) 0.0126 1.0000 Uani N1 N 0.35167(16) 0.23260(17) 0.65785(13) 0.0166 1.0000 Uani C1 C 0.26659(19) 0.2369(2) 0.66331(15) 0.0170 1.0000 Uani Cr1 Cr 0.12533(3) 0.24261(3) 0.68403(2) 0.0158 1.0000 Uani N2 N 0.51367(19) 0.40922(18) 0.67487(15) 0.0183 1.0000 Uani N3 N 0.49402(18) 0.2212(2) 0.55323(13) 0.0167 1.0000 Uani N4 N 0.51119(19) 0.04710(19) 0.69006(16) 0.0200 1.0000 Uani N5 N 0.5338(2) 0.2358(2) 0.81598(14) 0.0205 1.0000 Uani N6 N 0.68459(16) 0.22497(19) 0.72017(14) 0.0158 1.0000 Uani C2 C 0.1279(2) 0.0811(2) 0.69906(16) 0.0222 1.0000 Uani O1 O 0.12498(19) -0.01593(18) 0.70894(15) 0.0371 1.0000 Uani C3 C 0.0491(2) 0.2222(2) 0.56247(17) 0.0209 1.0000 Uani O2 O 0.00696(17) 0.2089(2) 0.49003(13) 0.0348 1.0000 Uani C4 C 0.1139(2) 0.4046(2) 0.67094(17) 0.0216 1.0000 Uani O3 O 0.10161(18) 0.50220(17) 0.66521(15) 0.0352 1.0000 Uani C5 C 0.2165(2) 0.2638(2) 0.80218(18) 0.0265 1.0000 Uani O4 O 0.2740(2) 0.2775(2) 0.87191(14) 0.0464 1.0000 Uani C6 C -0.0017(2) 0.2483(2) 0.70941(18) 0.0260 1.0000 Uani O5 O -0.07733(19) 0.2539(2) 0.72731(18) 0.0476 1.0000 Uani O6 O 0.68060(16) 0.38209(17) 0.58122(13) 0.0310 1.0000 Uani O7 O 0.79802(16) 0.54361(18) 0.64703(12) 0.0312 1.0000 Uani O8 O 0.62560(16) 0.57339(17) 0.52649(14) 0.0320 1.0000 Uani S1 S 0.71428(5) 0.49707(5) 0.57120(4) 0.0180 1.0000 Uani C7 C 0.7853(2) 0.4813(3) 0.49707(17) 0.0282 1.0000 Uani F1 F 0.83580(19) 0.57910(19) 0.49331(14) 0.0536 1.0000 Uani F2 F 0.71674(16) 0.4563(2) 0.41782(11) 0.0468 1.0000 Uani F3 F 0.86031(15) 0.39933(18) 0.52252(12) 0.0431 1.0000 Uani O9 O 0.61126(15) -0.01266(17) 0.56157(13) 0.0303 1.0000 Uani O10 O 0.77993(17) -0.00312(18) 0.68691(12) 0.0312 1.0000 Uani O11 O 0.74437(15) -0.16677(16) 0.58953(13) 0.0262 1.0000 Uani S2 S 0.72434(5) -0.04690(5) 0.60048(4) 0.0191 1.0000 Uani C8 C 0.7881(3) 0.0293(3) 0.5365(2) 0.0332 1.0000 Uani F4 F 0.89383(18) 0.0055(2) 0.56428(18) 0.0636 1.0000 Uani F5 F 0.7421(2) -0.00071(18) 0.45362(12) 0.0557 1.0000 Uani F6 F 0.7773(2) 0.14157(16) 0.54251(13) 0.0511 1.0000 Uani H1 H 0.461(4) 0.435(4) 0.686(3) 0.059(13) 1.0000 Uiso H2 H 0.578(3) 0.446(3) 0.713(2) 0.032(9) 1.0000 Uiso H3 H 0.507(3) 0.431(4) 0.622(3) 0.058(12) 1.0000 Uiso H4 H 0.428(3) 0.242(3) 0.520(3) 0.045(11) 1.0000 Uiso H5 H 0.542(3) 0.266(3) 0.548(2) 0.037(10) 1.0000 Uiso H6 H 0.500(3) 0.154(3) 0.534(2) 0.034(9) 1.0000 Uiso H7 H 0.445(3) 0.023(3) 0.688(2) 0.050(11) 1.0000 Uiso H8 H 0.528(3) 0.018(3) 0.649(3) 0.045(11) 1.0000 Uiso H9 H 0.560(3) 0.026(3) 0.737(2) 0.026(8) 1.0000 Uiso H10 H 0.499(5) 0.288(6) 0.822(4) 0.10(2) 1.0000 Uiso H11 H 0.514(4) 0.179(5) 0.834(3) 0.075(16) 1.0000 Uiso H12 H 0.599(5) 0.253(4) 0.848(3) 0.074(16) 1.0000 Uiso H13 H 0.715(3) 0.241(3) 0.775(3) 0.047(11) 1.0000 Uiso H14 H 0.707(3) 0.272(3) 0.689(2) 0.030(9) 1.0000 Uiso H15 H 0.709(3) 0.155(4) 0.714(2) 0.041(10) 1.0000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.00952(9) 0.01350(9) 0.01413(9) -0.00068(7) 0.00363(6) -0.00003(7) N1 0.0136(9) 0.0160(9) 0.0190(10) -0.0021(8) 0.0047(8) -0.0004(8) C1 0.0139(11) 0.0182(11) 0.0172(11) 0.0001(9) 0.0038(9) 0.0003(9) Cr1 0.01115(17) 0.0206(2) 0.01612(18) 0.00034(14) 0.00574(14) -0.00007(14) N2 0.0173(10) 0.0147(10) 0.0222(11) -0.0012(8) 0.0066(9) 0.0009(8) N3 0.0155(10) 0.0171(10) 0.0157(10) -0.0022(8) 0.0037(8) 0.0003(8) N4 0.0170(10) 0.0188(10) 0.0233(11) -0.0001(9) 0.0066(9) -0.0007(8) N5 0.0184(11) 0.0268(12) 0.0177(10) -0.0009(9) 0.0083(9) -0.0029(9) N6 0.0100(9) 0.0180(10) 0.0188(10) 0.0015(8) 0.0049(8) 0.0002(8) C2 0.0177(12) 0.0282(14) 0.0214(12) 0.0015(10) 0.0080(10) -0.0004(10) O1 0.0417(12) 0.0252(11) 0.0451(13) 0.0071(9) 0.0173(10) 0.0013(9) C3 0.0170(11) 0.0217(12) 0.0250(13) 0.0020(10) 0.0093(10) 0.0006(10) O2 0.0301(10) 0.0480(14) 0.0200(10) -0.0012(9) 0.0022(8) 0.0005(10) C4 0.0168(11) 0.0276(14) 0.0227(12) -0.0007(10) 0.0100(10) 0.0013(10) O3 0.0416(12) 0.0215(10) 0.0486(13) -0.0018(9) 0.0239(10) 0.0041(9) C5 0.0277(14) 0.0275(14) 0.0257(14) 0.0015(11) 0.0116(11) -0.0014(11) O4 0.0550(15) 0.0475(14) 0.0227(11) -0.0041(10) -0.0016(10) -0.0079(12) C6 0.0221(13) 0.0273(14) 0.0291(14) -0.0010(11) 0.0103(11) -0.0025(10) O5 0.0262(11) 0.0665(17) 0.0626(16) -0.0047(13) 0.0310(11) -0.0031(11) O6 0.0302(10) 0.0226(10) 0.0381(11) 0.0081(8) 0.0105(9) -0.0066(8) O7 0.0301(10) 0.0365(12) 0.0223(9) -0.0077(8) 0.0046(8) -0.0075(9) O8 0.0274(10) 0.0261(10) 0.0408(12) 0.0014(9) 0.0108(9) 0.0096(8) S1 0.0180(3) 0.0169(3) 0.0194(3) 0.0008(2) 0.0073(2) -0.0016(2) C7 0.0264(13) 0.0343(15) 0.0230(13) 0.0038(11) 0.0084(11) 0.0065(11) F1 0.0652(14) 0.0547(13) 0.0566(13) 0.0082(10) 0.0407(11) -0.0166(11) F2 0.0473(11) 0.0682(14) 0.0193(8) -0.0049(9) 0.0061(8) 0.0162(10) F3 0.0330(9) 0.0552(12) 0.0421(10) -0.0003(9) 0.0154(8) 0.0204(9) O9 0.0182(9) 0.0281(10) 0.0373(11) -0.0039(9) 0.0019(8) 0.0078(8) O10 0.0343(11) 0.0311(11) 0.0182(9) -0.0033(8) -0.0015(8) 0.0073(9) O11 0.0251(10) 0.0171(9) 0.0327(10) -0.0008(8) 0.0066(8) 0.0057(7) S2 0.0159(3) 0.0171(3) 0.0201(3) -0.0007(2) 0.0020(2) 0.0034(2) C8 0.0432(17) 0.0251(14) 0.0326(15) -0.0091(12) 0.0157(13) -0.0075(12) F4 0.0419(12) 0.0638(15) 0.0997(19) -0.0144(14) 0.0434(12) -0.0169(11) F5 0.0999(18) 0.0435(12) 0.0308(10) -0.0107(9) 0.0328(11) -0.0215(12) F6 0.0903(16) 0.0215(9) 0.0462(11) -0.0028(8) 0.0310(11) -0.0122(10) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru1 . N1 . 2.012(2) yes Ru1 . N2 . 2.113(2) yes Ru1 . N3 . 2.100(2) yes Ru1 . N4 . 2.113(2) yes Ru1 . N5 . 2.121(2) yes Ru1 . N6 . 2.1050(19) yes N1 . C1 . 1.160(3) yes C1 . Cr1 . 2.019(2) yes Cr1 . C2 . 1.896(3) yes Cr1 . C3 . 1.911(3) yes Cr1 . C4 . 1.899(3) yes Cr1 . C5 . 1.902(3) yes Cr1 . C6 . 1.877(3) yes N2 . H1 . 0.84(5) no N2 . H2 . 0.95(4) no N2 . H3 . 0.89(5) no N3 . H4 . 0.87(4) no N3 . H5 . 0.85(4) no N3 . H6 . 0.86(4) no N4 . H7 . 0.91(4) no N4 . H8 . 0.86(4) no N4 . H9 . 0.84(4) no N5 . H10 . 0.79(7) no N5 . H11 . 0.81(6) no N5 . H12 . 0.84(6) no N6 . H13 . 0.87(4) no N6 . H14 . 0.88(4) no N6 . H15 . 0.89(4) no C2 . O1 . 1.145(3) yes C3 . O2 . 1.136(3) yes C4 . O3 . 1.147(3) yes C5 . O4 . 1.137(4) yes C6 . O5 . 1.145(3) yes O6 . S1 . 1.4402(19) yes O7 . S1 . 1.4375(19) yes O8 . S1 . 1.435(2) yes S1 . C7 . 1.820(3) yes C7 . F1 . 1.333(4) yes C7 . F2 . 1.325(3) yes C7 . F3 . 1.324(3) yes O9 . S2 . 1.4413(18) yes O10 . S2 . 1.4439(19) yes O11 . S2 . 1.4451(19) yes S2 . C8 . 1.819(3) yes C8 . F4 . 1.323(4) yes C8 . F5 . 1.333(3) yes C8 . F6 . 1.323(3) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Ru1 . N2 . 89.36(8) yes N1 . Ru1 . N3 . 94.00(8) yes N2 . Ru1 . N3 . 88.16(9) yes N1 . Ru1 . N4 . 90.11(9) yes N2 . Ru1 . N4 . 178.74(9) yes N3 . Ru1 . N4 . 90.73(9) yes N1 . Ru1 . N5 . 86.18(9) yes N2 . Ru1 . N5 . 91.72(10) yes N3 . Ru1 . N5 . 179.78(9) yes N4 . Ru1 . N5 . 89.39(10) yes N1 . Ru1 . N6 . 176.10(8) yes N2 . Ru1 . N6 . 90.52(9) yes N3 . Ru1 . N6 . 89.90(8) yes N4 . Ru1 . N6 . 90.08(9) yes N5 . Ru1 . N6 . 89.93(9) yes Ru1 . N1 . C1 . 164.23(19) yes N1 . C1 . Cr1 . 175.0(2) yes C1 . Cr1 . C2 . 91.04(10) yes C1 . Cr1 . C3 . 88.01(10) yes C2 . Cr1 . C3 . 89.62(11) yes C1 . Cr1 . C4 . 92.93(10) yes C2 . Cr1 . C4 . 176.02(11) yes C3 . Cr1 . C4 . 90.80(11) yes C1 . Cr1 . C5 . 85.24(11) yes C2 . Cr1 . C5 . 91.07(12) yes C3 . Cr1 . C5 . 173.23(11) yes C4 . Cr1 . C5 . 88.97(12) yes C1 . Cr1 . C6 . 177.05(11) yes C2 . Cr1 . C6 . 88.77(11) yes C3 . Cr1 . C6 . 94.93(11) yes C4 . Cr1 . C6 . 87.25(11) yes C5 . Cr1 . C6 . 91.82(12) yes Ru1 . N2 . H1 . 109(3) no Ru1 . N2 . H2 . 115(2) no H1 . N2 . H2 . 107(3) no Ru1 . N2 . H3 . 111(3) no H1 . N2 . H3 . 109(4) no H2 . N2 . H3 . 105(3) no Ru1 . N3 . H4 . 111(3) no Ru1 . N3 . H5 . 106(2) no H4 . N3 . H5 . 111(3) no Ru1 . N3 . H6 . 115(2) no H4 . N3 . H6 . 103(3) no H5 . N3 . H6 . 110(3) no Ru1 . N4 . H7 . 110(3) no Ru1 . N4 . H8 . 110(3) no H7 . N4 . H8 . 112(3) no Ru1 . N4 . H9 . 108(2) no H7 . N4 . H9 . 109(3) no H8 . N4 . H9 . 107(3) no Ru1 . N5 . H10 . 108(4) no Ru1 . N5 . H11 . 115(3) no H10 . N5 . H11 . 107(5) no Ru1 . N5 . H12 . 112(3) no H10 . N5 . H12 . 104(5) no H11 . N5 . H12 . 110(5) no Ru1 . N6 . H13 . 109(3) no Ru1 . N6 . H14 . 112(2) no H13 . N6 . H14 . 111(3) no Ru1 . N6 . H15 . 112(2) no H13 . N6 . H15 . 106(3) no H14 . N6 . H15 . 107(3) no Cr1 . C2 . O1 . 176.7(2) yes Cr1 . C3 . O2 . 177.7(2) yes Cr1 . C4 . O3 . 175.4(2) yes Cr1 . C5 . O4 . 177.6(3) yes Cr1 . C6 . O5 . 177.7(3) yes O6 . S1 . O7 . 114.63(13) yes O6 . S1 . O8 . 114.19(12) yes O7 . S1 . O8 . 115.54(13) yes O6 . S1 . C7 . 104.17(13) yes O7 . S1 . C7 . 102.45(13) yes O8 . S1 . C7 . 103.64(13) yes S1 . C7 . F1 . 109.8(2) yes S1 . C7 . F2 . 111.6(2) yes F1 . C7 . F2 . 107.8(2) yes S1 . C7 . F3 . 111.57(19) yes F1 . C7 . F3 . 107.8(2) yes F2 . C7 . F3 . 108.1(2) yes O9 . S2 . O10 . 113.83(12) yes O9 . S2 . O11 . 114.68(12) yes O10 . S2 . O11 . 114.78(12) yes O9 . S2 . C8 . 103.20(14) yes O10 . S2 . C8 . 103.95(13) yes O11 . S2 . C8 . 104.51(13) yes S2 . C8 . F4 . 110.5(2) yes S2 . C8 . F5 . 110.6(2) yes F4 . C8 . F5 . 108.5(3) yes S2 . C8 . F6 . 110.6(2) yes F4 . C8 . F6 . 108.1(3) yes F5 . C8 . F6 . 108.5(3) yes loop_ _geom_hbond_atom_site_label_d _geom_hbond_atom_site_label_h _geom_hbond_atom_site_label_a _geom_hbond_site_symmetry_a _geom_hbond_distance_dh _geom_hbond_distance_ha _geom_hbond_distance_da _geom_hbond_angle_dha _geom_hbond_publ_flag N2 H2 O10 3_656 0.95(4) 2.08(4) 3.010(3) 168(3) yes N2 H3 O8 2_666 0.89(5) 2.44(4) 3.175(3) 140(3) yes N3 H5 O6 . 0.85(4) 2.17(4) 2.987(3) 160(3) yes N3 H6 O9 . 0.86(4) 2.37(4) 3.109(3) 144(3) yes N3 H6 O9 2_656 0.86(4) 2.37(4) 3.082(3) 140(3) yes N4 H8 O9 . 0.86(4) 2.17(4) 2.992(3) 161(4) yes N4 H9 O7 3_646 0.84(4) 2.14(4) 2.931(3) 157(3) yes N5 H12 O11 3_656 0.84(6) 2.15(6) 2.978(3) 167(5) yes N6 H13 O11 3_656 0.87(4) 2.37(4) 3.213(3) 162(3) yes N6 H14 O6 . 0.88(4) 2.13(4) 2.939(3) 153(3) yes N6 H15 O10 . 0.89(4) 2.19(4) 3.077(3) 171(3) yes # The atom H6 forms a bifurcated hydrogen bond, resulting in a short contact # between O9 and O9 2_656 of 2.897(3) \%A. # Attachment 'CrOs.cif' data_cros _database_code_depnum_ccdc_archive 'CCDC 691877' #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? _exptl_crystal_thermal_history ; The material was crystallised at ambient temperature. A suitable crystal was cooled rapidly to 150K for single-crystal X-ray diffraction analysis. ; _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_special_details ; Geometric restraints were applied to the NH~3~ groups. The NH bond lengths were restrained to their common mean, as were the Rh-N-H and H-N-H angles. Similarity restraints were applied between the displacement parameters of the H atoms and their parent N atoms. ; _cell_length_a 13.2109(2) _cell_angle_alpha 90 _cell_length_b 11.6400(2) _cell_angle_beta 112.1214(7) _cell_length_c 16.7552(3) _cell_angle_gamma 90 _cell_volume 2386.87(7) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'Cr ' 0.3209 0.6236 10.6406 6.1038 7.3537 0.3920 3.3240 20.2626 1.4922 98.7399 1.1832 International_Tables_Vol_IV_Table_2.2B 'F ' 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'Os ' -1.2165 7.6030 28.1894 1.6290 16.1550 8.9795 14.9305 0.3827 5.6759 48.1647 11.0005 International_Tables_Vol_IV_Table_2.2B 'S ' 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 4 _chemical_formula_sum ' C8 H15 Cr F6 N6 O11 Os S2 ' _chemical_formula_moiety ' C6 H15 Cr N6 O 5 Os, 2(C F3 O3 S) ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 791.56 _cell_measurement_reflns_used 24007 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description ' fragment ' _exptl_crystal_colour ' purple-brown ' _exptl_crystal_size_min 0.14 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_max 0.18 _exptl_crystal_density_diffrn 2.203 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1516 _exptl_absorpt_coefficient_mu 6.055 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.34 _exptl_absorpt_correction_T_max 0.43 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 24007 _reflns_number_total 5428 #5693 unqiue reflections including absences _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_theta_min 5.130 _diffrn_reflns_theta_max 27.491 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.491 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -17 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _refine_diff_density_min -1.09 _refine_diff_density_max 1.84 _refine_ls_number_reflns 4133 _refine_ls_number_restraints 60 _refine_ls_number_parameters 376 #_refine_ls_R_factor_ref 0.0243 _refine_ls_wR_factor_ref 0.0268 _refine_ls_goodness_of_fit_ref 1.1152 #_reflns_number_all 5428 _refine_ls_R_factor_all 0.0372 _refine_ls_wR_factor_all 0.0428 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 4133 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_gt 0.0268 _refine_ls_shift/su_max 0.019054 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.241 0.105 0.0463 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Os1 Os 0.513947(11) 0.227778(14) 0.685383(9) 0.0141 1.0000 Uani D . N1 N 0.3522(3) 0.2322(3) 0.6603(2) 0.0183 1.0000 Uani . . C1 C 0.2670(3) 0.2375(4) 0.6639(3) 0.0181 1.0000 Uani . . Cr1 Cr 0.12438(5) 0.24355(6) 0.68347(4) 0.0176 1.0000 Uani . . N2 N 0.5140(3) 0.4099(3) 0.6754(2) 0.0191 1.0000 Uani D U N3 N 0.4933(3) 0.2191(3) 0.5541(2) 0.0171 1.0000 Uani D U N4 N 0.5131(3) 0.0457(3) 0.6932(3) 0.0220 1.0000 Uani D U N5 N 0.5353(3) 0.2365(4) 0.8173(2) 0.0220 1.0000 Uani D U N6 N 0.6864(3) 0.2252(3) 0.7209(2) 0.0177 1.0000 Uani D U C2 C 0.1263(3) 0.0821(4) 0.6991(3) 0.0252 1.0000 Uani . . O1 O 0.1222(3) -0.0145(3) 0.7086(3) 0.0414 1.0000 Uani . . C3 C 0.0488(3) 0.2231(4) 0.5618(3) 0.0235 1.0000 Uani . . O2 O 0.0076(3) 0.2102(4) 0.4904(2) 0.0399 1.0000 Uani . . C4 C 0.1137(3) 0.4055(4) 0.6698(3) 0.0246 1.0000 Uani . . O3 O 0.1016(3) 0.5031(3) 0.6645(3) 0.0403 1.0000 Uani . . C5 C 0.2156(4) 0.2651(4) 0.8013(3) 0.0274 1.0000 Uani . . O4 O 0.2738(4) 0.2792(4) 0.8702(2) 0.0507 1.0000 Uani . . C6 C -0.0022(4) 0.2498(4) 0.7090(3) 0.0277 1.0000 Uani . . O5 O -0.0781(3) 0.2562(4) 0.7253(3) 0.0495 1.0000 Uani . . O6 O 0.6781(3) 0.3832(3) 0.5816(2) 0.0329 1.0000 Uani . . O7 O 0.7965(3) 0.5445(3) 0.6457(2) 0.0351 1.0000 Uani . . O8 O 0.6242(3) 0.5738(3) 0.5251(2) 0.0364 1.0000 Uani . . S1 S 0.71236(8) 0.49745(9) 0.57060(7) 0.0200 1.0000 Uani . . C7 C 0.7831(4) 0.4783(5) 0.4973(3) 0.0317 1.0000 Uani . . F1 F 0.8336(3) 0.5776(4) 0.4923(3) 0.0636 1.0000 Uani . . F2 F 0.7150(3) 0.4537(4) 0.4186(2) 0.0562 1.0000 Uani . . F3 F 0.8577(3) 0.3978(3) 0.5227(2) 0.0490 1.0000 Uani . . O9 O 0.6108(2) -0.0130(3) 0.5645(2) 0.0334 1.0000 Uani . . O10 O 0.7822(3) -0.0028(3) 0.6866(2) 0.0349 1.0000 Uani . . O11 O 0.7444(3) -0.1660(3) 0.5893(2) 0.0288 1.0000 Uani . . S2 S 0.72384(8) -0.04657(9) 0.60077(7) 0.0213 1.0000 Uani . . C8 C 0.7833(5) 0.0304(5) 0.5354(3) 0.0399 1.0000 Uani . . F4 F 0.8887(3) 0.0071(4) 0.5598(3) 0.0716 1.0000 Uani . . F5 F 0.7344(4) 0.0003(3) 0.4526(2) 0.0621 1.0000 Uani . . F6 F 0.7720(4) 0.1425(3) 0.5410(2) 0.0598 1.0000 Uani . . H1 H 0.461(3) 0.431(3) 0.689(3) 0.024(5) 1.0000 Uiso D U H2 H 0.575(3) 0.439(3) 0.713(3) 0.022(5) 1.0000 Uiso D U H3 H 0.506(3) 0.434(4) 0.623(3) 0.028(5) 1.0000 Uiso D U H4 H 0.429(3) 0.243(3) 0.524(2) 0.016(5) 1.0000 Uiso D U H5 H 0.538(3) 0.263(3) 0.546(2) 0.019(5) 1.0000 Uiso D U H6 H 0.504(3) 0.150(3) 0.542(2) 0.020(5) 1.0000 Uiso D U H7 H 0.450(3) 0.025(3) 0.692(3) 0.023(5) 1.0000 Uiso D U H8 H 0.523(3) 0.016(4) 0.651(3) 0.030(5) 1.0000 Uiso D U H9 H 0.564(3) 0.025(3) 0.743(2) 0.025(5) 1.0000 Uiso D U H10 H 0.495(3) 0.284(4) 0.823(3) 0.026(5) 1.0000 Uiso D U H11 H 0.517(3) 0.179(3) 0.833(3) 0.029(5) 1.0000 Uiso D U H12 H 0.597(3) 0.253(4) 0.848(2) 0.024(5) 1.0000 Uiso D U H13 H 0.718(3) 0.244(4) 0.775(2) 0.025(5) 1.0000 Uiso D U H14 H 0.706(3) 0.271(3) 0.691(3) 0.022(5) 1.0000 Uiso D U H15 H 0.710(3) 0.159(3) 0.714(3) 0.020(5) 1.0000 Uiso D U loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.01064(7) 0.01511(8) 0.01585(8) -0.00064(6) 0.00405(5) -0.00005(6) N1 0.0159(16) 0.0180(17) 0.0186(16) -0.0004(14) 0.0040(13) 0.0007(14) C1 0.0135(17) 0.019(2) 0.0197(18) -0.0002(16) 0.0043(14) -0.0012(15) Cr1 0.0123(3) 0.0234(4) 0.0178(3) 0.0004(2) 0.0066(2) 0.0000(2) N2 0.0188(16) 0.0123(17) 0.0245(19) -0.0014(14) 0.0063(15) 0.0001(14) N3 0.0143(15) 0.0161(18) 0.0196(16) 0.0004(14) 0.0049(13) -0.0003(14) N4 0.0200(17) 0.0175(19) 0.027(2) 0.0034(15) 0.0078(15) -0.0014(15) N5 0.0173(17) 0.027(2) 0.0221(18) 0.0008(16) 0.0081(14) -0.0001(16) N6 0.0095(14) 0.0196(18) 0.0232(17) 0.0016(15) 0.0052(13) 0.0009(14) C2 0.020(2) 0.034(3) 0.025(2) 0.0047(19) 0.0121(17) -0.0010(18) O1 0.048(2) 0.026(2) 0.051(2) 0.0093(17) 0.0194(19) 0.0024(17) C3 0.0168(18) 0.030(2) 0.024(2) 0.0010(19) 0.0084(16) -0.0015(18) O2 0.0358(19) 0.057(3) 0.0200(17) -0.0019(16) 0.0023(14) 0.0016(17) C4 0.020(2) 0.032(3) 0.025(2) -0.0013(19) 0.0123(17) 0.0021(18) O3 0.048(2) 0.027(2) 0.053(2) -0.0012(17) 0.0266(19) 0.0051(17) C5 0.027(2) 0.026(2) 0.030(2) 0.0007(19) 0.0114(19) -0.0035(19) O4 0.060(3) 0.055(3) 0.0217(18) -0.0012(17) -0.0029(17) -0.007(2) C6 0.021(2) 0.035(3) 0.031(2) -0.0015(19) 0.0133(18) -0.0006(18) O5 0.0253(18) 0.069(3) 0.068(3) -0.004(2) 0.0328(19) -0.0027(18) O6 0.0306(17) 0.0272(19) 0.0394(19) 0.0100(15) 0.0115(15) -0.0079(14) O7 0.0329(18) 0.043(2) 0.0235(16) -0.0100(15) 0.0041(14) -0.0083(16) O8 0.0321(18) 0.030(2) 0.045(2) 0.0026(16) 0.0127(16) 0.0107(15) S1 0.0191(5) 0.0188(5) 0.0221(5) 0.0011(4) 0.0078(4) -0.0014(4) C7 0.032(2) 0.037(3) 0.027(2) 0.004(2) 0.013(2) 0.006(2) F1 0.076(3) 0.067(3) 0.067(2) 0.011(2) 0.049(2) -0.016(2) F2 0.055(2) 0.081(3) 0.0246(16) -0.0068(16) 0.0068(15) 0.0231(19) F3 0.0371(17) 0.063(2) 0.0490(19) 0.0013(17) 0.0183(15) 0.0252(16) O9 0.0185(15) 0.033(2) 0.0379(19) -0.0065(15) -0.0014(14) 0.0105(14) O10 0.0368(19) 0.036(2) 0.0217(16) -0.0054(14) -0.0008(14) 0.0061(16) O11 0.0263(16) 0.0204(17) 0.0357(18) -0.0018(13) 0.0072(14) 0.0064(13) S2 0.0177(5) 0.0180(5) 0.0233(5) -0.0008(4) 0.0024(4) 0.0042(4) C8 0.052(3) 0.032(3) 0.033(3) -0.009(2) 0.014(2) -0.005(2) F4 0.049(2) 0.071(3) 0.112(4) -0.016(3) 0.050(2) -0.024(2) F5 0.112(3) 0.050(2) 0.0324(18) -0.0126(16) 0.036(2) -0.023(2) F6 0.109(3) 0.0266(18) 0.047(2) -0.0025(15) 0.033(2) -0.0141(19) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Os1 . N1 . 2.017(3) yes Os1 . N2 . 2.126(3) yes Os1 . N3 . 2.115(3) yes Os1 . N4 . 2.124(4) yes Os1 . N5 . 2.122(4) yes Os1 . N6 . 2.128(3) yes N1 . C1 . 1.151(5) yes C1 . Cr1 . 2.032(4) yes Cr1 . C2 . 1.896(5) yes Cr1 . C3 . 1.918(4) yes Cr1 . C4 . 1.897(5) yes Cr1 . C5 . 1.903(5) yes Cr1 . C6 . 1.877(4) yes N2 . H1 . 0.85(4) no N2 . H2 . 0.88(4) no N2 . H3 . 0.88(4) no N3 . H4 . 0.85(4) no N3 . H5 . 0.84(4) no N3 . H6 . 0.86(4) no N4 . H7 . 0.85(4) no N4 . H8 . 0.84(4) no N4 . H9 . 0.88(4) no N5 . H10 . 0.80(4) no N5 . H11 . 0.79(4) no N5 . H12 . 0.81(4) no N6 . H13 . 0.87(4) no N6 . H14 . 0.83(4) no N6 . H15 . 0.85(4) no C2 . O1 . 1.140(6) yes C3 . O2 . 1.123(5) yes C4 . O3 . 1.146(6) yes C5 . O4 . 1.133(6) yes C6 . O5 . 1.137(6) yes O6 . S1 . 1.439(3) yes O7 . S1 . 1.437(3) yes O8 . S1 . 1.435(3) yes S1 . C7 . 1.816(5) yes C7 . F1 . 1.352(6) yes C7 . F2 . 1.317(6) yes C7 . F3 . 1.310(6) yes O9 . S2 . 1.438(3) yes O10 . S2 . 1.444(3) yes O11 . S2 . 1.443(3) yes S2 . C8 . 1.807(6) yes C8 . F4 . 1.324(7) yes C8 . F5 . 1.338(6) yes C8 . F6 . 1.321(6) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Os1 . N2 . 89.40(14) yes N1 . Os1 . N3 . 94.18(13) yes N2 . Os1 . N3 . 88.25(14) yes N1 . Os1 . N4 . 90.49(15) yes N2 . Os1 . N4 . 179.11(15) yes N3 . Os1 . N4 . 90.88(15) yes N1 . Os1 . N5 . 86.01(14) yes N2 . Os1 . N5 . 91.73(15) yes N3 . Os1 . N5 . 179.82(14) yes N4 . Os1 . N5 . 89.14(16) yes N1 . Os1 . N6 . 176.05(14) yes N2 . Os1 . N6 . 90.25(15) yes N3 . Os1 . N6 . 89.75(13) yes N4 . Os1 . N6 . 89.91(15) yes N5 . Os1 . N6 . 90.07(14) yes Os1 . N1 . C1 . 166.0(3) yes N1 . C1 . Cr1 . 174.1(4) yes C1 . Cr1 . C2 . 91.31(18) yes C1 . Cr1 . C3 . 88.15(17) yes C2 . Cr1 . C3 . 89.9(2) yes C1 . Cr1 . C4 . 92.68(18) yes C2 . Cr1 . C4 . 176.00(18) yes C3 . Cr1 . C4 . 90.6(2) yes C1 . Cr1 . C5 . 84.72(18) yes C2 . Cr1 . C5 . 91.0(2) yes C3 . Cr1 . C5 . 172.83(19) yes C4 . Cr1 . C5 . 89.0(2) yes C1 . Cr1 . C6 . 176.39(19) yes C2 . Cr1 . C6 . 88.5(2) yes C3 . Cr1 . C6 . 95.45(19) yes C4 . Cr1 . C6 . 87.5(2) yes C5 . Cr1 . C6 . 91.7(2) yes Os1 . N2 . H1 . 104(3) no Os1 . N2 . H2 . 111(3) no H1 . N2 . H2 . 109(3) no Os1 . N2 . H3 . 113(3) no H1 . N2 . H3 . 111(3) no H2 . N2 . H3 . 109(3) no Os1 . N3 . H4 . 108(3) no Os1 . N3 . H5 . 109(3) no H4 . N3 . H5 . 108(3) no Os1 . N3 . H6 . 109(3) no H4 . N3 . H6 . 113(3) no H5 . N3 . H6 . 110(3) no Os1 . N4 . H7 . 108(3) no Os1 . N4 . H8 . 111(3) no H7 . N4 . H8 . 108(3) no Os1 . N4 . H9 . 108(3) no H7 . N4 . H9 . 109(3) no H8 . N4 . H9 . 112(3) no Os1 . N5 . H10 . 109(3) no Os1 . N5 . H11 . 111(3) no H10 . N5 . H11 . 105(3) no Os1 . N5 . H12 . 112(3) no H10 . N5 . H12 . 109(3) no H11 . N5 . H12 . 111(3) no Os1 . N6 . H13 . 109(3) no Os1 . N6 . H14 . 111(3) no H13 . N6 . H14 . 110(3) no Os1 . N6 . H15 . 112(3) no H13 . N6 . H15 . 108(3) no H14 . N6 . H15 . 107(3) no Cr1 . C2 . O1 . 176.5(4) yes Cr1 . C3 . O2 . 177.8(4) yes Cr1 . C4 . O3 . 174.8(4) yes Cr1 . C5 . O4 . 176.9(4) yes Cr1 . C6 . O5 . 178.3(5) yes O6 . S1 . O7 . 114.6(2) yes O6 . S1 . O8 . 114.2(2) yes O7 . S1 . O8 . 115.7(2) yes O6 . S1 . C7 . 103.9(2) yes O7 . S1 . C7 . 102.3(2) yes O8 . S1 . C7 . 103.8(2) yes S1 . C7 . F1 . 109.2(4) yes S1 . C7 . F2 . 111.8(3) yes F1 . C7 . F2 . 106.9(4) yes S1 . C7 . F3 . 112.6(3) yes F1 . C7 . F3 . 107.7(4) yes F2 . C7 . F3 . 108.5(4) yes O9 . S2 . O10 . 113.9(2) yes O9 . S2 . O11 . 115.0(2) yes O10 . S2 . O11 . 114.6(2) yes O9 . S2 . C8 . 103.2(3) yes O10 . S2 . C8 . 103.7(2) yes O11 . S2 . C8 . 104.5(2) yes S2 . C8 . F4 . 111.0(4) yes S2 . C8 . F5 . 110.4(4) yes F4 . C8 . F5 . 107.9(5) yes S2 . C8 . F6 . 111.1(4) yes F4 . C8 . F6 . 108.3(5) yes F5 . C8 . F6 . 108.1(5) yes loop_ _geom_hbond_atom_site_label_d _geom_hbond_atom_site_label_h _geom_hbond_atom_site_label_a _geom_hbond_site_symmetry_a _geom_hbond_distance_dh _geom_hbond_distance_ha _geom_hbond_distance_da _geom_hbond_angle_dha _geom_hbond_publ_flag N2 H1 O1 3_556 0.85(4) 2.44(4) 3.229(5) 153(4) yes N2 H2 O10 3_656 0.88(4) 2.11(4) 2.990(5) 173(4) yes N2 H3 O8 2_666 0.88(4) 2.44(4) 3.168(5) 141(4) yes N3 H5 O6 . 0.84(4) 2.21(4) 2.996(5) 157(4) yes N3 H6 O9 . 0.86(4) 2.31(4) 3.089(5) 151(4) yes N3 H6 O9 2_656 0.86(4) 2.44(4) 3.088(5) 133(3) yes N4 H8 O9 . 0.84(4) 2.20(4) 2.981(5) 155(4) yes N4 H9 O7 3_646 0.88(4) 2.09(4) 2.915(5) 157(4) yes N5 H12 O11 3_656 0.81(4) 2.18(4) 2.964(5) 166(4) yes N6 H13 O11 3_656 0.87(4) 2.38(4) 3.220(5) 162(4) yes N6 H14 O6 . 0.83(4) 2.17(4) 2.941(5) 154(4) yes N6 H15 O10 . 0.85(4) 2.24(4) 3.086(5) 172(4) yes # The atom H6 forms a bifurcated hydrogen bond, resulting in a short contact # between O9 and O9 2_656 of 2.927(6) \%A. # Attachment 'CrRh.cif' data_crrh _database_code_depnum_ccdc_archive 'CCDC 691878' #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? _exptl_crystal_thermal_history ; The material was crystallised at ambient temperature. A suitable crystal was cooled rapidly to 150K for single-crystal X-ray diffraction analysis. ; _diffrn_special_details ; Visual inspection of the diffraction pattern showed the crystal to be twinned. This was identified as twinning by rotation by 180 \% about the direct-space vector (1 0 1). The corresponding twin law is: (h') (-0.373 0 0.627) (h) (k') = (0 -1 0).(k) (l') (1.373 0 0.373) (l) ; _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_special_details ; Geometric restraints were applied to the NH~3~ groups. The NH bond lengths were restrained to their common mean, as were the Rh-N-H and H-N-H angles. Similarity restraints were applied between the displacement parameters of the H atoms and their parent N atoms. ; #============================================================= _cell_length_a 13.1502(2) _cell_angle_alpha 90 _cell_length_b 11.6256(2) _cell_angle_beta 112.1050(5) _cell_length_c 16.7353(2) _cell_angle_gamma 90 _cell_volume 2370.42(6) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'Cr ' 0.3209 0.6236 10.6406 6.1038 7.3537 0.3920 3.3240 20.2626 1.4922 98.7399 1.1832 International_Tables_Vol_IV_Table_2.2B 'F ' 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'Rh ' -1.1178 0.9187 19.2957 0.7515 14.3501 8.2176 4.7343 25.8749 1.2892 98.6062 5.3280 International_Tables_Vol_IV_Table_2.2B 'S ' 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 4 _chemical_formula_sum ' C8 H15 Cr F6 N6 O11 Rh1 S2 ' _chemical_formula_moiety ' C6 H15 Cr N6 O5 Rh, 2( C F3 O3 S) ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 704.26 _cell_measurement_reflns_used 26796 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description ' prism ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.973 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 1.438 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.92 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 26796 _reflns_number_total 5384 #5651 unique reflections including absences _diffrn_reflns_av_R_equivalents 0.065 _diffrn_reflns_theta_min 5.139 _diffrn_reflns_theta_max 27.479 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.479 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -17 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _refine_diff_density_min -0.91 _refine_diff_density_max 1.06 _refine_ls_number_reflns 3424 _refine_ls_number_restraints 60 _refine_ls_number_parameters 377 #_refine_ls_R_factor_ref 0.0347 _refine_ls_wR_factor_ref 0.0395 _refine_ls_goodness_of_fit_ref 1.0354 #_reflns_number_all 5384 _refine_ls_R_factor_all 0.0678 _refine_ls_wR_factor_all 0.0518 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 3424 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_gt 0.0395 _refine_ls_shift/su_max 0.024284 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.815 0.529 0.621 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Rh1 Rh 0.51540(2) 0.22717(3) 0.686446(18) 0.0130 1.0000 Uani D . N1 N 0.3537(3) 0.2309(3) 0.6598(2) 0.0177 1.0000 Uani . . C1 C 0.2683(3) 0.2368(3) 0.6644(2) 0.0171 1.0000 Uani . . Cr1 Cr 0.12411(5) 0.24432(6) 0.68314(4) 0.0171 1.0000 Uani . . N2 N 0.5136(3) 0.4047(3) 0.6762(2) 0.0180 1.0000 Uani D U N3 N 0.4944(3) 0.2175(3) 0.5580(2) 0.0194 1.0000 Uani D U N4 N 0.5134(3) 0.0498(3) 0.6940(2) 0.0197 1.0000 Uani D U N5 N 0.5345(3) 0.2379(3) 0.8151(2) 0.0229 1.0000 Uani D U N6 N 0.6837(3) 0.2255(3) 0.7201(2) 0.0182 1.0000 Uani D U C2 C 0.1252(3) 0.0823(4) 0.6984(3) 0.0252 1.0000 Uani . . O1 O 0.1199(3) -0.0141(3) 0.7080(2) 0.0406 1.0000 Uani . . C3 C 0.0491(3) 0.2235(4) 0.5614(3) 0.0246 1.0000 Uani . . O2 O 0.0085(3) 0.2117(3) 0.4890(2) 0.0373 1.0000 Uani . . C4 C 0.1134(3) 0.4066(4) 0.6702(3) 0.0230 1.0000 Uani . . O3 O 0.1009(3) 0.5034(3) 0.6642(2) 0.0378 1.0000 Uani . . C5 C 0.2151(4) 0.2654(4) 0.8008(3) 0.0277 1.0000 Uani . . O4 O 0.2725(4) 0.2799(4) 0.8704(2) 0.0494 1.0000 Uani . . C6 C -0.0030(4) 0.2525(4) 0.7074(3) 0.0290 1.0000 Uani . . O5 O -0.0804(3) 0.2586(4) 0.7236(3) 0.0498 1.0000 Uani . . O6 O 0.6755(3) 0.3855(3) 0.5820(2) 0.0320 1.0000 Uani . . O7 O 0.7941(3) 0.5473(3) 0.6444(2) 0.0329 1.0000 Uani . . O8 O 0.6220(3) 0.5764(3) 0.5226(2) 0.0319 1.0000 Uani . . S1 S 0.71010(8) 0.49944(8) 0.56953(6) 0.0186 1.0000 Uani . . C7 C 0.7826(4) 0.4788(4) 0.4969(3) 0.0303 1.0000 Uani . . F1 F 0.8338(3) 0.5753(3) 0.4920(3) 0.0613 1.0000 Uani . . F2 F 0.7140(3) 0.4527(3) 0.41780(19) 0.0551 1.0000 Uani . . F3 F 0.8559(3) 0.3957(3) 0.5238(2) 0.0480 1.0000 Uani . . O9 O 0.6085(3) -0.0152(3) 0.5658(2) 0.0336 1.0000 Uani . . O10 O 0.7823(3) -0.0031(3) 0.68743(19) 0.0341 1.0000 Uani . . O11 O 0.7443(3) -0.1664(3) 0.5896(2) 0.0299 1.0000 Uani . . S2 S 0.72293(8) -0.04712(9) 0.60143(6) 0.0203 1.0000 Uani . . C8 C 0.7803(5) 0.0317(5) 0.5342(3) 0.0397 1.0000 Uani . . F4 F 0.8862(3) 0.0103(4) 0.5580(3) 0.0720 1.0000 Uani . . F5 F 0.7302(4) 0.0015(3) 0.4519(2) 0.0615 1.0000 Uani . . F6 F 0.7681(4) 0.1442(3) 0.5410(2) 0.0602 1.0000 Uani . . H1 H 0.460(3) 0.434(3) 0.690(3) 0.019(5) 1.0000 Uiso D U H2 H 0.574(3) 0.443(3) 0.712(2) 0.020(5) 1.0000 Uiso D U H3 H 0.509(3) 0.428(3) 0.627(2) 0.025(5) 1.0000 Uiso D U H4 H 0.430(3) 0.233(3) 0.529(2) 0.021(5) 1.0000 Uiso D U H5 H 0.533(3) 0.267(3) 0.545(3) 0.024(5) 1.0000 Uiso D U H6 H 0.507(3) 0.151(3) 0.539(2) 0.020(5) 1.0000 Uiso D U H7 H 0.451(3) 0.024(3) 0.689(3) 0.019(5) 1.0000 Uiso D U H8 H 0.530(3) 0.015(3) 0.654(3) 0.027(5) 1.0000 Uiso D U H9 H 0.562(3) 0.027(3) 0.740(2) 0.017(5) 1.0000 Uiso D U H10 H 0.496(3) 0.293(4) 0.823(3) 0.031(5) 1.0000 Uiso D U H11 H 0.511(3) 0.183(3) 0.833(2) 0.026(5) 1.0000 Uiso D U H12 H 0.600(3) 0.245(4) 0.854(3) 0.027(5) 1.0000 Uiso D U H13 H 0.718(3) 0.240(3) 0.775(2) 0.022(5) 1.0000 Uiso D U H14 H 0.707(3) 0.272(3) 0.688(3) 0.020(5) 1.0000 Uiso D U H15 H 0.708(3) 0.162(3) 0.713(3) 0.022(5) 1.0000 Uiso D U loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01059(14) 0.01294(15) 0.01473(15) -0.00085(11) 0.00401(10) -0.00016(11) N1 0.0166(15) 0.0161(15) 0.0197(15) 0.0018(13) 0.0059(12) 0.0010(13) C1 0.0148(17) 0.0163(18) 0.0176(18) 0.0010(14) 0.0032(14) -0.0014(14) Cr1 0.0125(3) 0.0211(3) 0.0186(3) 0.0014(2) 0.0067(2) 0.0002(2) N2 0.0209(16) 0.0120(16) 0.0222(18) -0.0050(13) 0.0095(14) -0.0014(13) N3 0.0174(16) 0.0189(18) 0.0200(17) -0.0009(14) 0.0049(13) 0.0006(14) N4 0.0145(16) 0.0195(17) 0.0236(18) 0.0032(14) 0.0056(13) -0.0014(14) N5 0.0235(18) 0.024(2) 0.0202(17) 0.0036(14) 0.0076(15) 0.0006(15) N6 0.0143(15) 0.0208(17) 0.0185(17) 0.0013(14) 0.0052(13) 0.0009(14) C2 0.020(2) 0.032(3) 0.027(2) 0.0006(18) 0.0133(17) -0.0014(17) O1 0.047(2) 0.0268(19) 0.051(2) 0.0094(16) 0.0221(18) 0.0011(16) C3 0.0192(18) 0.028(2) 0.030(2) 0.0015(18) 0.0131(17) 0.0013(18) O2 0.0332(18) 0.053(2) 0.0213(17) -0.0028(15) 0.0047(14) 0.0006(16) C4 0.0177(19) 0.026(2) 0.027(2) 0.0017(17) 0.0106(16) 0.0023(16) O3 0.044(2) 0.0212(18) 0.053(2) 0.0020(15) 0.0240(18) 0.0065(15) C5 0.026(2) 0.024(2) 0.033(2) 0.0029(18) 0.0116(19) 0.0044(18) O4 0.057(2) 0.051(2) 0.0256(19) -0.0043(17) -0.0017(17) -0.010(2) C6 0.024(2) 0.037(3) 0.029(2) -0.0006(18) 0.0135(18) -0.0008(17) O5 0.0290(19) 0.065(3) 0.069(3) -0.005(2) 0.0337(19) -0.0015(17) O6 0.0299(17) 0.0243(17) 0.0403(19) 0.0091(14) 0.0117(14) -0.0055(13) O7 0.0285(17) 0.0383(19) 0.0255(16) -0.0071(14) 0.0029(13) -0.0084(14) O8 0.0278(16) 0.0278(17) 0.0369(18) 0.0025(14) 0.0084(14) 0.0077(14) S1 0.0191(5) 0.0173(5) 0.0192(4) 0.0004(4) 0.0071(4) -0.0011(4) C7 0.034(2) 0.037(3) 0.023(2) 0.0018(18) 0.0146(19) 0.006(2) F1 0.074(2) 0.061(2) 0.072(2) 0.0154(19) 0.054(2) -0.0117(19) F2 0.058(2) 0.079(3) 0.0214(14) -0.0069(15) 0.0069(14) 0.0226(19) F3 0.0377(17) 0.063(2) 0.0451(18) 0.0030(15) 0.0173(14) 0.0243(15) O9 0.0215(16) 0.0317(18) 0.0407(19) -0.0052(15) 0.0038(14) 0.0091(13) O10 0.0360(18) 0.0356(19) 0.0191(15) -0.0070(14) -0.0028(13) 0.0082(15) O11 0.0284(17) 0.0221(16) 0.0365(17) -0.0013(13) 0.0091(13) 0.0072(13) S2 0.0189(5) 0.0176(5) 0.0203(5) 0.0000(4) 0.0028(4) 0.0043(4) C8 0.056(3) 0.030(3) 0.036(3) -0.002(2) 0.020(2) -0.012(2) F4 0.050(2) 0.077(3) 0.105(3) -0.017(2) 0.049(2) -0.024(2) F5 0.112(3) 0.049(2) 0.0300(16) -0.0113(15) 0.0340(19) -0.022(2) F6 0.112(3) 0.0220(15) 0.0469(19) -0.0043(14) 0.031(2) -0.0180(18) _refine_ls_extinction_method None loop_ _oxford_twin_element_scale_factors 0.5974(18)0.4026(18) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Rh1 . N1 . 2.003(3) yes Rh1 . N2 . 2.071(3) yes Rh1 . N3 . 2.064(3) yes Rh1 . N4 . 2.067(3) yes Rh1 . N5 . 2.075(4) yes Rh1 . N6 . 2.069(3) yes N1 . C1 . 1.156(5) yes C1 . Cr1 . 2.037(4) yes Cr1 . C2 . 1.900(5) yes Cr1 . C3 . 1.916(5) yes Cr1 . C4 . 1.899(4) yes Cr1 . C5 . 1.896(5) yes Cr1 . C6 . 1.865(4) yes N2 . H1 . 0.89(4) no N2 . H2 . 0.91(4) no N2 . H3 . 0.84(4) no N3 . H4 . 0.83(4) no N3 . H5 . 0.84(4) no N3 . H6 . 0.87(4) no N4 . H7 . 0.85(4) no N4 . H8 . 0.88(4) no N4 . H9 . 0.84(3) no N5 . H10 . 0.85(4) no N5 . H11 . 0.81(4) no N5 . H12 . 0.87(4) no N6 . H13 . 0.88(4) no N6 . H14 . 0.89(4) no N6 . H15 . 0.83(4) no C2 . O1 . 1.138(6) yes C3 . O2 . 1.133(6) yes C4 . O3 . 1.135(5) yes C5 . O4 . 1.137(6) yes C6 . O5 . 1.150(6) yes O6 . S1 . 1.441(3) yes O7 . S1 . 1.435(3) yes O8 . S1 . 1.440(3) yes S1 . C7 . 1.821(5) yes C7 . F1 . 1.327(6) yes C7 . F2 . 1.327(6) yes C7 . F3 . 1.318(5) yes O9 . S2 . 1.443(3) yes O10 . S2 . 1.448(3) yes O11 . S2 . 1.443(3) yes S2 . C8 . 1.819(5) yes C8 . F4 . 1.321(7) yes C8 . F5 . 1.331(6) yes C8 . F6 . 1.328(6) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Rh1 . N2 . 88.96(14) yes N1 . Rh1 . N3 . 93.12(14) yes N2 . Rh1 . N3 . 88.57(14) yes N1 . Rh1 . N4 . 89.90(14) yes N2 . Rh1 . N4 . 178.54(14) yes N3 . Rh1 . N4 . 90.57(15) yes N1 . Rh1 . N5 . 86.21(14) yes N2 . Rh1 . N5 . 91.11(15) yes N3 . Rh1 . N5 . 179.27(14) yes N4 . Rh1 . N5 . 89.74(15) yes N1 . Rh1 . N6 . 177.21(14) yes N2 . Rh1 . N6 . 90.55(14) yes N3 . Rh1 . N6 . 89.61(14) yes N4 . Rh1 . N6 . 90.63(14) yes N5 . Rh1 . N6 . 91.05(14) yes Rh1 . N1 . C1 . 164.3(3) yes N1 . C1 . Cr1 . 175.3(3) yes C1 . Cr1 . C2 . 91.00(17) yes C1 . Cr1 . C3 . 88.15(16) yes C2 . Cr1 . C3 . 89.58(19) yes C1 . Cr1 . C4 . 93.36(17) yes C2 . Cr1 . C4 . 175.62(17) yes C3 . Cr1 . C4 . 91.05(19) yes C1 . Cr1 . C5 . 84.55(17) yes C2 . Cr1 . C5 . 91.06(19) yes C3 . Cr1 . C5 . 172.68(18) yes C4 . Cr1 . C5 . 88.88(19) yes C1 . Cr1 . C6 . 176.53(18) yes C2 . Cr1 . C6 . 89.0(2) yes C3 . Cr1 . C6 . 95.33(19) yes C4 . Cr1 . C6 . 86.59(19) yes C5 . Cr1 . C6 . 92.0(2) yes Rh1 . N2 . H1 . 110(2) no Rh1 . N2 . H2 . 116(2) no H1 . N2 . H2 . 103(3) no Rh1 . N2 . H3 . 113(3) no H1 . N2 . H3 . 111(3) no H2 . N2 . H3 . 103(3) no Rh1 . N3 . H4 . 108(3) no Rh1 . N3 . H5 . 112(3) no H4 . N3 . H5 . 106(3) no Rh1 . N3 . H6 . 117(2) no H4 . N3 . H6 . 106(3) no H5 . N3 . H6 . 107(3) no Rh1 . N4 . H7 . 113(3) no Rh1 . N4 . H8 . 113(3) no H7 . N4 . H8 . 106(3) no Rh1 . N4 . H9 . 110(3) no H7 . N4 . H9 . 111(3) no H8 . N4 . H9 . 104(3) no Rh1 . N5 . H10 . 111(3) no Rh1 . N5 . H11 . 115(3) no H10 . N5 . H11 . 102(3) no Rh1 . N5 . H12 . 119(3) no H10 . N5 . H12 . 106(3) no H11 . N5 . H12 . 101(3) no Rh1 . N6 . H13 . 111(3) no Rh1 . N6 . H14 . 114(2) no H13 . N6 . H14 . 111(3) no Rh1 . N6 . H15 . 113(3) no H13 . N6 . H15 . 105(3) no H14 . N6 . H15 . 103(3) no Cr1 . C2 . O1 . 175.9(4) yes Cr1 . C3 . O2 . 177.3(4) yes Cr1 . C4 . O3 . 175.2(4) yes Cr1 . C5 . O4 . 177.4(4) yes Cr1 . C6 . O5 . 178.8(5) yes O6 . S1 . O7 . 114.3(2) yes O6 . S1 . O8 . 114.6(2) yes O7 . S1 . O8 . 115.6(2) yes O6 . S1 . C7 . 104.4(2) yes O7 . S1 . C7 . 102.1(2) yes O8 . S1 . C7 . 103.6(2) yes S1 . C7 . F1 . 109.5(4) yes S1 . C7 . F2 . 111.4(3) yes F1 . C7 . F2 . 107.6(4) yes S1 . C7 . F3 . 111.6(3) yes F1 . C7 . F3 . 108.6(4) yes F2 . C7 . F3 . 108.0(4) yes O9 . S2 . O10 . 114.1(2) yes O9 . S2 . O11 . 114.6(2) yes O10 . S2 . O11 . 114.6(2) yes O9 . S2 . C8 . 103.0(3) yes O10 . S2 . C8 . 104.1(2) yes O11 . S2 . C8 . 104.6(2) yes S2 . C8 . F4 . 110.7(4) yes S2 . C8 . F5 . 110.4(4) yes F4 . C8 . F5 . 108.5(5) yes S2 . C8 . F6 . 110.6(4) yes F4 . C8 . F6 . 107.9(5) yes F5 . C8 . F6 . 108.7(5) yes loop_ _geom_hbond_atom_site_label_d _geom_hbond_atom_site_label_h _geom_hbond_atom_site_label_a _geom_hbond_site_symmetry_a _geom_hbond_distance_dh _geom_hbond_distance_ha _geom_hbond_distance_da _geom_hbond_angle_dha _geom_hbond_publ_flag N2 H1 O1 3_556 0.89(4) 2.39(4) 3.207(5) 153(3) yes N2 H2 O10 3_656 0.91(4) 2.10(4) 2.992(5) 167(3) yes N2 H3 O8 2_666 0.84(4) 2.45(4) 3.136(5) 139(3) yes N3 H5 O6 . 0.84(4) 2.22(4) 2.987(5) 151(4) yes N3 H6 O9 . 0.87(4) 2.30(4) 3.073(5) 149(3) yes N3 H6 O9 2_656 0.87(4) 2.43(4) 3.090(5) 133(3) yes N4 H8 O9 . 0.88(4) 2.12(4) 2.960(5) 159(4) yes N4 H9 O7 3_646 0.84(3) 2.15(4) 2.927(5) 154(3) yes N5 H12 O11 3_656 0.87(4) 2.17(4) 2.956(5) 152(4) yes N6 H13 O11 3_656 0.88(4) 2.38(4) 3.216(5) 158(4) yes N6 H14 O6 . 0.89(4) 2.12(4) 2.938(5) 151(3) yes N6 H15 O10 . 0.83(4) 2.26(4) 3.095(5) 174(4) yes