# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Andrew Hallett' _publ_contact_author_email HALLETTAJ@CARDIFF.AC.UK loop_ _publ_author_name A.Hallett K.Anderson N.Connelly data_1+ _database_code_depnum_ccdc_archive 'CCDC 716566' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H34 N6 Rh, F6 P' _chemical_formula_sum 'C24 H34 F6 N6 P Rh' _chemical_formula_weight 654.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.5422(6) _cell_length_b 14.3375(10) _cell_length_c 22.1114(16) _cell_angle_alpha 90.00 _cell_angle_beta 100.1570(10) _cell_angle_gamma 90.00 _cell_volume 2665.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 94 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.631 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 0.769 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.838475 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens CCD area detector' _diffrn_measurement_method '/w scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 16968 _diffrn_reflns_av_R_equivalents 0.0681 _diffrn_reflns_av_sigmaI/netI 0.0911 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.51 _reflns_number_total 6091 _reflns_number_gt 3783 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6091 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0963 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.0969 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 1.15345(4) 0.34109(2) 0.269425(15) 0.02374(9) Uani 1 1 d . . . P1 P 1.45178(16) 0.26899(8) 0.07604(6) 0.0403(3) Uani 1 1 d . . . F1 F 1.5436(4) 0.1810(2) 0.10655(17) 0.0875(12) Uani 1 1 d . . . F2 F 1.3518(4) 0.35742(19) 0.04900(16) 0.0679(9) Uani 1 1 d . . . F3 F 1.5685(4) 0.2817(3) 0.03025(15) 0.0885(11) Uani 1 1 d . . . F4 F 1.3395(4) 0.2043(2) 0.02890(14) 0.0661(9) Uani 1 1 d . . . F5 F 1.3287(4) 0.2569(2) 0.12311(16) 0.0845(11) Uani 1 1 d . . . F6 F 1.5630(4) 0.33351(19) 0.12452(13) 0.0662(9) Uani 1 1 d . . . N1 N 1.3464(3) 0.2729(2) 0.32718(14) 0.0237(7) Uani 1 1 d . . . N2 N 1.3147(3) 0.2362(2) 0.38174(14) 0.0236(7) Uani 1 1 d . . . N3 N 1.0332(4) 0.2174(2) 0.28761(16) 0.0286(8) Uani 1 1 d . . . N4 N 1.0487(4) 0.1872(2) 0.34685(16) 0.0275(8) Uani 1 1 d . . . N5 N 0.9328(3) 0.3369(2) 0.39483(14) 0.0243(7) Uani 1 1 d . . . N6 N 1.0947(3) 0.3293(2) 0.40036(14) 0.0233(7) Uani 1 1 d . . . C1 C 1.2868(5) 0.4678(3) 0.27362(19) 0.0280(9) Uani 1 1 d . . . H1A H 1.3966 0.4632 0.2982 0.034 Uiso 1 1 calc R . . C2 C 1.2716(5) 0.4311(3) 0.2151(2) 0.0331(10) Uani 1 1 d . . . H2A H 1.3727 0.4045 0.2056 0.040 Uiso 1 1 calc R . . C3 C 0.9623(4) 0.4373(3) 0.25912(18) 0.0258(9) Uani 1 1 d . . . H3A H 0.8783 0.4203 0.2834 0.031 Uiso 1 1 calc R . . C4 C 0.9522(5) 0.3868(3) 0.20478(19) 0.0324(10) Uani 1 1 d . . . H4A H 0.8625 0.3410 0.1975 0.039 Uiso 1 1 calc R . . C5 C 1.1530(4) 0.2360(3) 0.39422(18) 0.0223(8) Uani 1 1 d . . . H5A H 1.1533 0.2025 0.4339 0.027 Uiso 1 1 calc R . . C6 C 1.0035(5) 0.4217(4) 0.1467(2) 0.0466(12) Uani 1 1 d . . . H6A H 0.9214 0.4646 0.1251 0.056 Uiso 1 1 calc R . . H6B H 1.0116 0.3681 0.1191 0.056 Uiso 1 1 calc R . . C7 C 1.1646(5) 0.4728(3) 0.1599(2) 0.0425(12) Uani 1 1 d . . . H7A H 1.2173 0.4683 0.1236 0.051 Uiso 1 1 calc R . . H7B H 1.1467 0.5396 0.1676 0.051 Uiso 1 1 calc R . . C8 C 1.0137(5) 0.5392(3) 0.2666(2) 0.0333(10) Uani 1 1 d . . . H8A H 0.9539 0.5702 0.2955 0.040 Uiso 1 1 calc R . . H8B H 0.9867 0.5712 0.2264 0.040 Uiso 1 1 calc R . . C9 C 1.1921(5) 0.5495(3) 0.2907(2) 0.0334(10) Uani 1 1 d . . . H9A H 1.2307 0.6074 0.2739 0.040 Uiso 1 1 calc R . . H9B H 1.2100 0.5555 0.3360 0.040 Uiso 1 1 calc R . . C10 C 1.5875(5) 0.2878(3) 0.27880(19) 0.0306(10) Uani 1 1 d . . . H10A H 1.5324 0.2603 0.2403 0.046 Uiso 1 1 calc R . . H10B H 1.6973 0.2648 0.2876 0.046 Uiso 1 1 calc R . . H10C H 1.5880 0.3559 0.2749 0.046 Uiso 1 1 calc R . . C11 C 1.5032(4) 0.2608(3) 0.33027(18) 0.0246(9) Uani 1 1 d . . . C12 C 1.5696(5) 0.2173(3) 0.38574(18) 0.0293(9) Uani 1 1 d . . . H12A H 1.6782 0.2010 0.3986 0.035 Uiso 1 1 calc R . . C13 C 1.4478(5) 0.2028(3) 0.41801(19) 0.0280(9) Uani 1 1 d . . . C14 C 1.4485(5) 0.1598(4) 0.4788(2) 0.0470(12) Uani 1 1 d . . . H14A H 1.3912 0.2001 0.5032 0.071 Uiso 1 1 calc R . . H14B H 1.5585 0.1518 0.5000 0.071 Uiso 1 1 calc R . . H14C H 1.3961 0.0987 0.4734 0.071 Uiso 1 1 calc R . . C15 C 0.9141(6) 0.1564(4) 0.1856(2) 0.0579(15) Uani 1 1 d . . . H15A H 0.9920 0.1974 0.1713 0.087 Uiso 1 1 calc R . . H15B H 0.8068 0.1809 0.1716 0.087 Uiso 1 1 calc R . . H15C H 0.9220 0.0936 0.1688 0.087 Uiso 1 1 calc R . . C16 C 0.9467(5) 0.1521(3) 0.2534(2) 0.0385(11) Uani 1 1 d . . . C17 C 0.9040(5) 0.0822(3) 0.2919(2) 0.0434(13) Uani 1 1 d . . . H17A H 0.8410 0.0287 0.2793 0.052 Uiso 1 1 calc R . . C18 C 0.9698(5) 0.1053(3) 0.3507(2) 0.0378(11) Uani 1 1 d . . . C19 C 0.9646(6) 0.0582(3) 0.4104(2) 0.0489(14) Uani 1 1 d . . . H19A H 0.9269 0.1023 0.4385 0.073 Uiso 1 1 calc R . . H19B H 1.0714 0.0365 0.4284 0.073 Uiso 1 1 calc R . . H19C H 0.8920 0.0048 0.4035 0.073 Uiso 1 1 calc R . . C20 C 0.7470(4) 0.4579(3) 0.4161(2) 0.0329(10) Uani 1 1 d . . . H20A H 0.6787 0.4456 0.3764 0.049 Uiso 1 1 calc R . . H20B H 0.7505 0.5252 0.4241 0.049 Uiso 1 1 calc R . . H20C H 0.7040 0.4257 0.4487 0.049 Uiso 1 1 calc R . . C21 C 0.9112(4) 0.4231(3) 0.41465(17) 0.0248(9) Uani 1 1 d . . . C22 C 1.0563(4) 0.4687(3) 0.43396(18) 0.0267(9) Uani 1 1 d . . . H22A H 1.0704 0.5305 0.4494 0.032 Uiso 1 1 calc R . . C23 C 1.1729(5) 0.4081(3) 0.42648(18) 0.0252(9) Uani 1 1 d . . . C24 C 1.3508(4) 0.4197(3) 0.4426(2) 0.0348(11) Uani 1 1 d . . . H24A H 1.3760 0.4845 0.4547 0.052 Uiso 1 1 calc R . . H24B H 1.3990 0.4040 0.4069 0.052 Uiso 1 1 calc R . . H24C H 1.3930 0.3781 0.4768 0.052 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01849(15) 0.02764(17) 0.02473(16) -0.00185(16) 0.00285(11) 0.00109(16) P1 0.0518(8) 0.0330(7) 0.0333(7) -0.0025(5) -0.0007(6) 0.0007(6) F1 0.096(3) 0.043(2) 0.103(3) 0.0083(17) -0.038(2) 0.0001(17) F2 0.0592(19) 0.0439(19) 0.095(3) -0.0002(16) -0.0007(17) 0.0085(15) F3 0.067(2) 0.143(3) 0.063(2) -0.011(2) 0.0329(19) -0.008(2) F4 0.072(2) 0.0573(19) 0.058(2) -0.0249(15) -0.0166(16) 0.0044(17) F5 0.098(3) 0.092(3) 0.069(2) -0.0074(19) 0.033(2) -0.033(2) F6 0.085(2) 0.0509(18) 0.0552(19) -0.0027(15) -0.0090(16) -0.0273(17) N1 0.0177(16) 0.0266(18) 0.0275(19) -0.0014(14) 0.0063(14) -0.0020(14) N2 0.0172(16) 0.0271(18) 0.0268(19) 0.0004(14) 0.0047(14) 0.0013(14) N3 0.0204(17) 0.0238(19) 0.039(2) -0.0106(15) -0.0004(15) 0.0000(15) N4 0.0188(17) 0.0229(18) 0.040(2) -0.0016(14) 0.0035(15) -0.0019(14) N5 0.0181(15) 0.0279(18) 0.0280(18) 0.0002(15) 0.0073(13) 0.0014(16) N6 0.0197(16) 0.0237(18) 0.0270(18) -0.0030(14) 0.0057(13) 0.0009(14) C1 0.022(2) 0.024(2) 0.040(3) 0.0027(18) 0.0132(18) -0.0004(17) C2 0.024(2) 0.038(3) 0.039(3) 0.006(2) 0.0118(19) 0.0043(19) C3 0.0133(19) 0.031(2) 0.032(2) 0.0040(18) 0.0021(16) 0.0070(17) C4 0.024(2) 0.039(3) 0.032(3) -0.0013(19) -0.0011(18) 0.0083(19) C5 0.0186(19) 0.025(2) 0.025(2) -0.0011(16) 0.0094(16) -0.0039(16) C6 0.047(3) 0.066(3) 0.025(3) 0.004(2) -0.001(2) 0.014(3) C7 0.042(3) 0.057(3) 0.032(3) 0.009(2) 0.018(2) 0.013(2) C8 0.029(2) 0.033(3) 0.039(3) -0.002(2) 0.011(2) 0.005(2) C9 0.030(2) 0.028(2) 0.044(3) 0.0020(19) 0.0094(19) 0.0006(19) C10 0.021(2) 0.035(2) 0.038(3) -0.0020(19) 0.0105(18) -0.0008(19) C11 0.0166(19) 0.025(2) 0.032(2) -0.0059(17) 0.0042(17) 0.0010(16) C12 0.017(2) 0.037(3) 0.033(2) -0.0002(19) 0.0043(17) 0.0069(18) C13 0.023(2) 0.029(2) 0.030(2) -0.0015(18) -0.0015(17) 0.0059(18) C14 0.035(3) 0.064(3) 0.043(3) 0.018(3) 0.008(2) 0.012(3) C15 0.053(3) 0.052(3) 0.058(3) -0.031(3) -0.019(2) 0.013(3) C16 0.017(2) 0.035(3) 0.058(3) -0.020(2) -0.0073(19) 0.005(2) C17 0.019(2) 0.027(3) 0.082(4) -0.014(2) 0.002(2) -0.0020(19) C18 0.023(2) 0.021(2) 0.072(4) -0.005(2) 0.014(2) -0.0003(19) C19 0.044(3) 0.025(3) 0.084(4) 0.007(2) 0.030(3) -0.006(2) C20 0.023(2) 0.036(3) 0.039(3) -0.0044(19) 0.0032(19) 0.0055(19) C21 0.028(2) 0.027(2) 0.020(2) 0.0011(16) 0.0067(17) 0.0013(18) C22 0.026(2) 0.022(2) 0.033(2) -0.0031(17) 0.0090(18) -0.0017(17) C23 0.027(2) 0.025(2) 0.025(2) -0.0031(17) 0.0074(17) -0.0042(18) C24 0.021(2) 0.039(3) 0.045(3) -0.018(2) 0.0060(19) -0.0080(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C3 2.119(4) . ? Rh1 N3 2.124(3) . ? Rh1 C2 2.133(4) . ? Rh1 N1 2.136(3) . ? Rh1 C4 2.136(4) . ? Rh1 C1 2.138(4) . ? P1 F3 1.552(3) . ? P1 F1 1.573(3) . ? P1 F2 1.585(3) . ? P1 F4 1.586(3) . ? P1 F6 1.596(3) . ? P1 F5 1.614(3) . ? N1 C11 1.340(4) . ? N1 N2 1.386(4) . ? N2 C13 1.358(5) . ? N2 C5 1.455(4) . ? N3 C16 1.341(5) . ? N3 N4 1.363(4) . ? N4 C18 1.365(5) . ? N4 C5 1.432(5) . ? N5 C21 1.335(5) . ? N5 N6 1.371(4) . ? N6 C23 1.385(5) . ? N6 C5 1.442(5) . ? C1 C2 1.381(6) . ? C1 C9 1.509(5) . ? C2 C7 1.514(6) . ? C3 C4 1.393(6) . ? C3 C8 1.527(6) . ? C4 C6 1.514(6) . ? C6 C7 1.541(6) . ? C8 C9 1.530(5) . ? C10 C11 1.501(5) . ? C11 C12 1.403(5) . ? C12 C13 1.378(5) . ? C13 C14 1.477(6) . ? C15 C16 1.478(7) . ? C16 C17 1.405(7) . ? C17 C18 1.362(6) . ? C18 C19 1.491(7) . ? C20 C21 1.495(5) . ? C21 C22 1.400(5) . ? C22 C23 1.354(5) . ? C23 C24 1.508(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Rh1 N3 100.07(13) . . ? C3 Rh1 C2 88.73(15) . . ? N3 Rh1 C2 154.74(15) . . ? C3 Rh1 N1 149.45(14) . . ? N3 Rh1 N1 81.53(12) . . ? C2 Rh1 N1 102.79(14) . . ? C3 Rh1 C4 38.21(15) . . ? N3 Rh1 C4 91.35(15) . . ? C2 Rh1 C4 80.96(16) . . ? N1 Rh1 C4 170.38(14) . . ? C3 Rh1 C1 81.14(15) . . ? N3 Rh1 C1 166.81(14) . . ? C2 Rh1 C1 37.73(15) . . ? N1 Rh1 C1 90.78(14) . . ? C4 Rh1 C1 97.38(17) . . ? F3 P1 F1 92.5(2) . . ? F3 P1 F2 91.5(2) . . ? F1 P1 F2 176.0(2) . . ? F3 P1 F4 91.35(19) . . ? F1 P1 F4 90.62(17) . . ? F2 P1 F4 89.83(17) . . ? F3 P1 F6 89.75(19) . . ? F1 P1 F6 89.08(18) . . ? F2 P1 F6 90.40(17) . . ? F4 P1 F6 178.87(19) . . ? F3 P1 F5 179.2(2) . . ? F1 P1 F5 88.3(2) . . ? F2 P1 F5 87.72(19) . . ? F4 P1 F5 88.49(18) . . ? F6 P1 F5 90.41(18) . . ? C11 N1 N2 104.7(3) . . ? C11 N1 Rh1 138.5(3) . . ? N2 N1 Rh1 116.5(2) . . ? C13 N2 N1 112.1(3) . . ? C13 N2 C5 127.7(3) . . ? N1 N2 C5 120.2(3) . . ? C16 N3 N4 105.8(3) . . ? C16 N3 Rh1 135.5(3) . . ? N4 N3 Rh1 118.6(2) . . ? N3 N4 C18 111.5(3) . . ? N3 N4 C5 119.4(3) . . ? C18 N4 C5 128.7(4) . . ? C21 N5 N6 103.9(3) . . ? N5 N6 C23 112.2(3) . . ? N5 N6 C5 115.1(3) . . ? C23 N6 C5 130.2(3) . . ? C2 C1 C9 124.4(4) . . ? C2 C1 Rh1 71.0(2) . . ? C9 C1 Rh1 111.4(2) . . ? C1 C2 C7 123.3(4) . . ? C1 C2 Rh1 71.3(2) . . ? C7 C2 Rh1 114.5(3) . . ? C4 C3 C8 124.4(4) . . ? C4 C3 Rh1 71.6(2) . . ? C8 C3 Rh1 114.2(2) . . ? C3 C4 C6 125.2(4) . . ? C3 C4 Rh1 70.2(2) . . ? C6 C4 Rh1 110.5(3) . . ? N4 C5 N6 109.9(3) . . ? N4 C5 N2 110.6(3) . . ? N6 C5 N2 111.8(3) . . ? C4 C6 C7 112.2(4) . . ? C2 C7 C6 111.0(4) . . ? C3 C8 C9 112.3(3) . . ? C1 C9 C8 112.6(3) . . ? N1 C11 C12 110.4(3) . . ? N1 C11 C10 122.4(4) . . ? C12 C11 C10 127.1(3) . . ? C13 C12 C11 107.1(3) . . ? N2 C13 C12 105.7(4) . . ? N2 C13 C14 123.6(4) . . ? C12 C13 C14 130.7(4) . . ? N3 C16 C17 109.4(4) . . ? N3 C16 C15 122.0(4) . . ? C17 C16 C15 128.5(4) . . ? C18 C17 C16 107.3(4) . . ? C17 C18 N4 106.0(4) . . ? C17 C18 C19 131.5(4) . . ? N4 C18 C19 122.5(4) . . ? N5 C21 C22 111.5(3) . . ? N5 C21 C20 120.0(3) . . ? C22 C21 C20 128.4(4) . . ? C23 C22 C21 107.1(3) . . ? C22 C23 N6 105.3(3) . . ? C22 C23 C24 129.2(4) . . ? N6 C23 C24 125.5(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.671 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.095 data_2+ _database_code_depnum_ccdc_archive 'CCDC 716567' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H30 N6 Rh, F6 P, C H2 Cl2' _chemical_formula_sum 'C24 H32 Cl2 F6 N6 P Rh' _chemical_formula_weight 723.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 14.5581(15) _cell_length_b 14.8892(15) _cell_length_c 26.743(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5796.8(10) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7045 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2928 _exptl_absorpt_coefficient_mu 0.894 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.756 _exptl_absorpt_correction_T_max 0.913 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 35687 _diffrn_reflns_av_R_equivalents 0.0849 _diffrn_reflns_av_sigmaI/netI 0.0684 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.53 _reflns_number_total 6665 _reflns_number_gt 4024 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; EADP and SADI restraints were used in the refinement of the two PF6 molecules Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0765P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6665 _refine_ls_number_parameters 395 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1027 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1475 _refine_ls_wR_factor_gt 0.1318 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 0.22891(3) 0.03670(2) 0.406753(13) 0.02841(12) Uani 1 1 d . . . Cl1A Cl 0.46831(17) 0.09578(17) 0.24287(9) 0.1042(8) Uani 1 1 d . . . Cl2A Cl 0.2860(2) 0.16670(19) 0.25405(12) 0.1247(10) Uani 1 1 d . . . P1A P 0.2092(6) 0.1300(5) 0.6224(3) 0.0359(14) Uani 0.548(6) 1 d PD A 1 P1B P 0.1919(7) 0.1173(6) 0.6177(4) 0.047(3) Uani 0.452(6) 1 d PD A 2 F1A F 0.1637(9) 0.1904(8) 0.5811(3) 0.090(3) Uani 0.548(6) 1 d PD A 1 F2A F 0.2499(9) 0.0705(9) 0.6662(3) 0.090(3) Uani 0.548(6) 1 d PD A 1 F3A F 0.2567(8) 0.0703(7) 0.5809(3) 0.0576(17) Uani 0.548(6) 1 d PD A 1 F4A F 0.2971(7) 0.1901(9) 0.6240(4) 0.120(3) Uani 0.548(6) 1 d PD A 1 F5A F 0.1667(5) 0.1903(5) 0.6638(2) 0.0576(17) Uani 0.548(6) 1 d PD A 1 F6A F 0.1250(7) 0.0654(10) 0.6207(4) 0.120(3) Uani 0.548(6) 1 d PD A 1 F1B F 0.1086(8) 0.1334(10) 0.5817(4) 0.094(4) Uani 0.452(6) 1 d PD A 2 F2B F 0.2752(9) 0.0919(11) 0.6527(4) 0.094(4) Uani 0.45 1 d PD A 2 F3B F 0.2528(12) 0.0927(14) 0.5698(4) 0.105(3) Uani 0.452(6) 1 d PD A 2 F4B F 0.2171(12) 0.2176(7) 0.6132(8) 0.151(5) Uani 0.452(6) 1 d PD A 2 F5B F 0.1225(8) 0.1338(11) 0.6618(4) 0.105(3) Uani 0.45 1 d PD A 2 F6B F 0.1710(13) 0.0158(7) 0.6171(7) 0.151(5) Uani 0.45 1 d PD A 2 N1 N 0.3148(3) -0.0593(3) 0.45360(14) 0.0290(9) Uani 1 1 d . . . N2 N 0.4073(3) -0.0618(3) 0.44272(13) 0.0269(9) Uani 1 1 d . . . N3 N 0.3626(3) 0.1153(3) 0.40040(14) 0.0284(9) Uani 1 1 d . . . N4 N 0.4423(3) 0.0674(3) 0.39308(14) 0.0287(9) Uani 1 1 d . . . N5 N 0.2941(3) -0.0368(3) 0.34693(14) 0.0319(9) Uani 1 1 d . . . N6 N 0.3832(3) -0.0655(3) 0.35429(13) 0.0289(9) Uani 1 1 d . . . C1 C 0.1365(4) 0.0599(4) 0.46786(19) 0.0413(13) Uani 1 1 d . . . H1A H 0.1477 0.0366 0.5024 0.050 Uiso 1 1 calc R . . C2 C 0.1704(4) 0.1416(4) 0.45113(19) 0.0397(13) Uani 1 1 d . . . H2A H 0.2078 0.1828 0.4725 0.048 Uiso 1 1 calc R . . C3 C 0.0914(4) 0.0213(4) 0.38851(19) 0.0397(13) Uani 1 1 d . . . H3A H 0.0686 -0.0274 0.3660 0.048 Uiso 1 1 calc R . . C4 C 0.1260(3) 0.1052(4) 0.37021(19) 0.0386(12) Uani 1 1 d . . . H4A H 0.1287 0.1204 0.3338 0.046 Uiso 1 1 calc R . . C5 C 0.4387(3) -0.0293(3) 0.39457(17) 0.0288(10) Uani 1 1 d . . . H5A H 0.5028 -0.0518 0.3897 0.035 Uiso 1 1 calc R . . C6 C 0.1020(4) 0.1752(4) 0.4114(2) 0.0425(13) Uani 1 1 d . . . H6A H 0.1049 0.2401 0.4020 0.051 Uiso 1 1 calc R . . C7 C 0.0109(4) 0.1396(4) 0.4315(2) 0.0484(14) Uani 1 1 d . . . H7A H -0.0395 0.1432 0.4066 0.058 Uiso 1 1 calc R . . H7B H -0.0079 0.1687 0.4632 0.058 Uiso 1 1 calc R . . C8 C 0.0473(4) 0.0424(4) 0.4390(2) 0.0462(13) Uani 1 1 d . . . H8A H 0.0038 -0.0029 0.4531 0.055 Uiso 1 1 calc R . . C9 C 0.2149(4) -0.1304(4) 0.5179(2) 0.0428(13) Uani 1 1 d . . . H9A H 0.2053 -0.0886 0.5457 0.064 Uiso 1 1 calc R . . H9B H 0.2141 -0.1922 0.5305 0.064 Uiso 1 1 calc R . . H9C H 0.1657 -0.1227 0.4932 0.064 Uiso 1 1 calc R . . C10 C 0.3054(3) -0.1117(3) 0.49388(17) 0.0302(10) Uani 1 1 d . . . C11 C 0.3903(3) -0.1465(3) 0.50824(17) 0.0325(11) Uani 1 1 d . . . H11A H 0.4017 -0.1852 0.5358 0.039 Uiso 1 1 calc R . . C12 C 0.4545(3) -0.1144(3) 0.47517(17) 0.0299(10) Uani 1 1 d . . . C13 C 0.5563(3) -0.1289(4) 0.47210(19) 0.0404(13) Uani 1 1 d . . . H13A H 0.5708 -0.1634 0.4419 0.061 Uiso 1 1 calc R . . H13B H 0.5771 -0.1622 0.5016 0.061 Uiso 1 1 calc R . . H13C H 0.5875 -0.0707 0.4708 0.061 Uiso 1 1 calc R . . C14 C 0.3153(4) 0.2743(3) 0.3890(2) 0.0443(13) Uani 1 1 d . . . H14A H 0.2717 0.2666 0.3615 0.066 Uiso 1 1 calc R . . H14B H 0.3469 0.3321 0.3854 0.066 Uiso 1 1 calc R . . H14C H 0.2822 0.2731 0.4209 0.066 Uiso 1 1 calc R . . C15 C 0.3848(4) 0.1994(3) 0.38793(18) 0.0351(12) Uani 1 1 d . . . C16 C 0.4764(3) 0.2053(3) 0.37258(18) 0.0362(12) Uani 1 1 d . . . H16A H 0.5080 0.2580 0.3624 0.043 Uiso 1 1 calc R . . C17 C 0.5117(3) 0.1202(3) 0.37511(17) 0.0322(11) Uani 1 1 d . . . C18 C 0.6057(4) 0.0843(4) 0.3628(2) 0.0451(14) Uani 1 1 d . . . H18A H 0.6304 0.0522 0.3918 0.068 Uiso 1 1 calc R . . H18B H 0.6466 0.1344 0.3543 0.068 Uiso 1 1 calc R . . H18C H 0.6014 0.0431 0.3343 0.068 Uiso 1 1 calc R . . C19 C 0.1755(4) -0.0630(4) 0.2803(2) 0.0529(16) Uani 1 1 d . . . H19A H 0.1335 -0.1088 0.2932 0.079 Uiso 1 1 calc R . . H19B H 0.1805 -0.0689 0.2439 0.079 Uiso 1 1 calc R . . H19C H 0.1518 -0.0032 0.2887 0.079 Uiso 1 1 calc R . . C20 C 0.2689(4) -0.0752(4) 0.30362(18) 0.0388(12) Uani 1 1 d . . . C21 C 0.3407(4) -0.1257(4) 0.28373(19) 0.0436(13) Uani 1 1 d . . . H21A H 0.3396 -0.1588 0.2534 0.052 Uiso 1 1 calc R . . C22 C 0.4136(4) -0.1186(4) 0.31640(18) 0.0381(12) Uani 1 1 d . . . C23 C 0.5058(4) -0.1593(4) 0.3148(2) 0.0484(15) Uani 1 1 d . . . H23A H 0.5524 -0.1117 0.3146 0.073 Uiso 1 1 calc R . . H23B H 0.5119 -0.1956 0.2844 0.073 Uiso 1 1 calc R . . H23C H 0.5145 -0.1975 0.3442 0.073 Uiso 1 1 calc R . . C24A C 0.3560(7) 0.1104(8) 0.2141(3) 0.131(5) Uani 1 1 d . . . H24A H 0.3623 0.1445 0.1826 0.157 Uiso 1 1 calc R . . H24B H 0.3292 0.0510 0.2062 0.157 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0257(2) 0.0296(2) 0.0299(2) 0.00060(17) 0.00097(16) 0.00277(17) Cl1A 0.0852(17) 0.0977(17) 0.130(2) 0.0107(15) 0.0197(14) 0.0022(13) Cl2A 0.120(2) 0.1052(19) 0.149(2) -0.0098(18) 0.0136(18) 0.0241(16) P1A 0.029(2) 0.046(3) 0.032(2) 0.0073(19) 0.0011(18) 0.0092(18) P1B 0.048(5) 0.046(4) 0.046(3) 0.000(3) -0.006(3) 0.019(3) F1A 0.129(7) 0.105(5) 0.036(3) 0.023(3) 0.005(3) 0.067(5) F2A 0.129(7) 0.105(5) 0.036(3) 0.023(3) 0.005(3) 0.067(5) F3A 0.061(3) 0.072(4) 0.040(3) 0.000(3) 0.000(3) 0.032(3) F4A 0.076(5) 0.174(8) 0.111(6) -0.017(6) 0.012(4) -0.070(5) F5A 0.061(3) 0.072(4) 0.040(3) 0.000(3) 0.000(3) 0.032(3) F6A 0.076(5) 0.174(8) 0.111(6) -0.017(6) 0.012(4) -0.070(5) F1B 0.077(6) 0.134(8) 0.071(5) -0.032(6) -0.036(5) 0.062(6) F2B 0.077(6) 0.134(8) 0.071(5) -0.032(6) -0.036(5) 0.062(6) F3B 0.096(6) 0.169(10) 0.051(4) 0.019(5) 0.025(4) 0.066(6) F4B 0.169(11) 0.042(5) 0.241(13) 0.025(6) -0.025(10) -0.013(5) F5B 0.096(6) 0.169(10) 0.051(4) 0.019(5) 0.025(4) 0.066(6) F6B 0.169(11) 0.042(5) 0.241(13) 0.025(6) -0.025(10) -0.013(5) N1 0.020(2) 0.036(2) 0.031(2) 0.0028(17) 0.0026(16) -0.0030(17) N2 0.023(2) 0.030(2) 0.0279(19) 0.0050(16) -0.0002(16) -0.0014(16) N3 0.027(2) 0.024(2) 0.035(2) -0.0024(17) -0.0020(17) -0.0007(16) N4 0.026(2) 0.025(2) 0.034(2) 0.0045(17) 0.0010(17) -0.0007(17) N5 0.031(2) 0.036(2) 0.028(2) -0.0017(19) -0.0032(16) -0.0011(19) N6 0.032(2) 0.026(2) 0.029(2) 0.0005(17) 0.0029(17) -0.0040(17) C1 0.034(3) 0.056(4) 0.033(3) 0.004(3) 0.005(2) 0.007(2) C2 0.031(3) 0.048(3) 0.040(3) -0.012(3) 0.005(2) 0.012(2) C3 0.034(3) 0.046(3) 0.039(3) -0.001(2) 0.000(2) 0.000(2) C4 0.033(3) 0.047(3) 0.036(3) 0.007(2) -0.004(2) 0.002(2) C5 0.024(2) 0.026(2) 0.036(3) -0.001(2) 0.0043(18) 0.000(2) C6 0.030(3) 0.040(3) 0.057(3) 0.006(3) 0.004(3) 0.006(2) C7 0.031(3) 0.055(4) 0.060(4) -0.001(3) 0.000(3) 0.009(3) C8 0.034(3) 0.051(4) 0.054(3) 0.007(3) 0.008(2) 0.004(3) C9 0.039(3) 0.041(3) 0.049(3) 0.005(3) 0.011(2) -0.004(2) C10 0.030(3) 0.033(3) 0.028(2) -0.001(2) 0.001(2) -0.003(2) C11 0.040(3) 0.031(3) 0.027(2) 0.001(2) -0.001(2) 0.000(2) C12 0.028(3) 0.028(3) 0.033(2) -0.004(2) -0.003(2) 0.000(2) C13 0.033(3) 0.042(3) 0.045(3) -0.001(3) -0.005(2) 0.006(2) C14 0.041(3) 0.027(3) 0.065(4) -0.002(3) 0.001(3) 0.004(2) C15 0.042(3) 0.027(3) 0.036(3) 0.002(2) -0.009(2) -0.001(2) C16 0.034(3) 0.028(3) 0.047(3) 0.003(2) -0.003(2) -0.006(2) C17 0.024(2) 0.035(3) 0.037(3) 0.003(2) 0.000(2) -0.006(2) C18 0.032(3) 0.037(3) 0.066(4) 0.001(3) 0.013(3) -0.005(2) C19 0.056(4) 0.063(4) 0.040(3) -0.010(3) -0.015(3) -0.005(3) C20 0.050(3) 0.037(3) 0.030(2) 0.001(2) 0.000(2) -0.009(3) C21 0.060(4) 0.041(3) 0.030(3) -0.008(2) 0.006(3) -0.010(3) C22 0.046(3) 0.034(3) 0.034(3) -0.006(2) 0.014(2) -0.004(2) C23 0.051(4) 0.041(3) 0.053(3) -0.010(3) 0.018(3) -0.010(3) C24A 0.130(9) 0.198(11) 0.066(5) -0.056(6) 0.019(5) -0.100(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C4 2.059(5) . ? Rh1 C3 2.073(5) . ? Rh1 C2 2.139(5) . ? Rh1 C1 2.145(5) . ? Rh1 N5 2.158(4) . ? Rh1 N1 2.275(4) . ? Rh1 N3 2.277(4) . ? Cl1A C24A 1.819(10) . ? Cl2A C24A 1.697(10) . ? P1A F5A 1.553(9) . ? P1A F6A 1.559(9) . ? P1A F4A 1.561(10) . ? P1A F1A 1.572(9) . ? P1A F3A 1.582(9) . ? P1A F2A 1.583(9) . ? P1B F6B 1.542(11) . ? P1B F4B 1.542(11) . ? P1B F1B 1.567(10) . ? P1B F5B 1.574(11) . ? P1B F2B 1.579(11) . ? P1B F3B 1.600(11) . ? N1 C10 1.337(6) . ? N1 N2 1.378(5) . ? N2 C12 1.356(6) . ? N2 C5 1.450(6) . ? N3 C15 1.335(6) . ? N3 N4 1.377(5) . ? N4 C17 1.366(6) . ? N4 C5 1.441(6) . ? N5 C20 1.343(6) . ? N5 N6 1.381(5) . ? N6 C22 1.359(6) . ? N6 C5 1.450(6) . ? C1 C2 1.387(8) . ? C1 C8 1.532(8) . ? C1 H1A 1.0000 . ? C2 C6 1.539(7) . ? C2 H2A 1.0000 . ? C3 C4 1.432(7) . ? C3 C8 1.528(7) . ? C3 H3A 1.0000 . ? C4 C6 1.556(7) . ? C4 H4A 1.0000 . ? C5 H5A 1.0000 . ? C6 C7 1.526(7) . ? C6 H6A 1.0000 . ? C7 C8 1.555(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 1.0000 . ? C9 C10 1.493(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.394(7) . ? C11 C12 1.372(7) . ? C11 H11A 0.9500 . ? C12 C13 1.500(7) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.506(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.398(7) . ? C16 C17 1.368(7) . ? C16 H16A 0.9500 . ? C17 C18 1.506(7) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.507(8) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.392(8) . ? C21 C22 1.379(8) . ? C21 H21A 0.9500 . ? C22 C23 1.474(8) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24A H24A 0.9900 . ? C24A H24B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Rh1 C3 40.5(2) . . ? C4 Rh1 C2 67.2(2) . . ? C3 Rh1 C2 80.0(2) . . ? C4 Rh1 C1 79.9(2) . . ? C3 Rh1 C1 65.9(2) . . ? C2 Rh1 C1 37.8(2) . . ? C4 Rh1 N5 102.65(18) . . ? C3 Rh1 N5 101.19(18) . . ? C2 Rh1 N5 163.08(18) . . ? C1 Rh1 N5 157.28(19) . . ? C4 Rh1 N1 166.49(18) . . ? C3 Rh1 N1 126.22(18) . . ? C2 Rh1 N1 111.86(17) . . ? C1 Rh1 N1 91.53(17) . . ? N5 Rh1 N1 81.27(14) . . ? C4 Rh1 N3 109.39(18) . . ? C3 Rh1 N3 149.79(18) . . ? C2 Rh1 N3 90.35(18) . . ? C1 Rh1 N3 120.66(18) . . ? N5 Rh1 N3 80.20(14) . . ? N1 Rh1 N3 83.95(13) . . ? F5A P1A F6A 93.6(7) . . ? F5A P1A F4A 88.7(7) . . ? F6A P1A F4A 176.9(9) . . ? F5A P1A F1A 90.1(6) . . ? F6A P1A F1A 90.0(8) . . ? F4A P1A F1A 92.1(8) . . ? F5A P1A F3A 177.6(9) . . ? F6A P1A F3A 88.7(8) . . ? F4A P1A F3A 89.0(7) . . ? F1A P1A F3A 90.7(6) . . ? F5A P1A F2A 86.9(6) . . ? F6A P1A F2A 88.3(9) . . ? F4A P1A F2A 89.7(8) . . ? F1A P1A F2A 176.5(7) . . ? F3A P1A F2A 92.3(6) . . ? F6B P1B F4B 174.5(13) . . ? F6B P1B F1B 89.6(10) . . ? F4B P1B F1B 89.3(10) . . ? F6B P1B F5B 91.9(11) . . ? F4B P1B F5B 93.4(11) . . ? F1B P1B F5B 86.6(8) . . ? F6B P1B F2B 85.5(11) . . ? F4B P1B F2B 95.4(11) . . ? F1B P1B F2B 174.9(10) . . ? F5B P1B F2B 94.8(8) . . ? F6B P1B F3B 83.0(12) . . ? F4B P1B F3B 91.6(12) . . ? F1B P1B F3B 88.4(8) . . ? F5B P1B F3B 172.9(13) . . ? F2B P1B F3B 89.7(8) . . ? C10 N1 N2 104.7(4) . . ? C10 N1 Rh1 139.0(3) . . ? N2 N1 Rh1 116.0(3) . . ? C12 N2 N1 112.1(4) . . ? C12 N2 C5 127.0(4) . . ? N1 N2 C5 119.1(3) . . ? C15 N3 N4 104.2(4) . . ? C15 N3 Rh1 135.1(3) . . ? N4 N3 Rh1 117.7(3) . . ? C17 N4 N3 112.0(4) . . ? C17 N4 C5 127.7(4) . . ? N3 N4 C5 118.8(4) . . ? C20 N5 N6 104.3(4) . . ? C20 N5 Rh1 137.4(4) . . ? N6 N5 Rh1 117.7(3) . . ? C22 N6 N5 112.3(4) . . ? C22 N6 C5 126.1(4) . . ? N5 N6 C5 120.9(4) . . ? C2 C1 C8 106.8(5) . . ? C2 C1 Rh1 70.9(3) . . ? C8 C1 Rh1 96.9(3) . . ? C2 C1 H1A 123.0 . . ? C8 C1 H1A 123.0 . . ? Rh1 C1 H1A 123.0 . . ? C1 C2 C6 106.1(5) . . ? C1 C2 Rh1 71.3(3) . . ? C6 C2 Rh1 96.4(3) . . ? C1 C2 H2A 123.2 . . ? C6 C2 H2A 123.2 . . ? Rh1 C2 H2A 123.2 . . ? C4 C3 C8 105.7(5) . . ? C4 C3 Rh1 69.2(3) . . ? C8 C3 Rh1 100.1(3) . . ? C4 C3 H3A 122.9 . . ? C8 C3 H3A 122.9 . . ? Rh1 C3 H3A 122.9 . . ? C3 C4 C6 105.3(4) . . ? C3 C4 Rh1 70.3(3) . . ? C6 C4 Rh1 99.1(3) . . ? C3 C4 H4A 123.0 . . ? C6 C4 H4A 123.0 . . ? Rh1 C4 H4A 123.0 . . ? N4 C5 N2 111.7(4) . . ? N4 C5 N6 111.8(4) . . ? N2 C5 N6 111.1(4) . . ? N4 C5 H5A 107.3 . . ? N2 C5 H5A 107.3 . . ? N6 C5 H5A 107.3 . . ? C7 C6 C2 101.9(4) . . ? C7 C6 C4 102.2(5) . . ? C2 C6 C4 97.3(4) . . ? C7 C6 H6A 117.4 . . ? C2 C6 H6A 117.4 . . ? C4 C6 H6A 117.4 . . ? C6 C7 C8 94.1(4) . . ? C6 C7 H7A 112.9 . . ? C8 C7 H7A 112.9 . . ? C6 C7 H7B 112.9 . . ? C8 C7 H7B 112.9 . . ? H7A C7 H7B 110.3 . . ? C3 C8 C1 97.1(4) . . ? C3 C8 C7 102.7(5) . . ? C1 C8 C7 101.3(5) . . ? C3 C8 H8A 117.5 . . ? C1 C8 H8A 117.5 . . ? C7 C8 H8A 117.5 . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 C11 110.4(4) . . ? N1 C10 C9 123.1(5) . . ? C11 C10 C9 126.5(4) . . ? C12 C11 C10 107.3(4) . . ? C12 C11 H11A 126.4 . . ? C10 C11 H11A 126.4 . . ? N2 C12 C11 105.6(4) . . ? N2 C12 C13 123.3(4) . . ? C11 C12 C13 131.1(5) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C15 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 C16 111.3(4) . . ? N3 C15 C14 121.8(5) . . ? C16 C15 C14 126.9(5) . . ? C17 C16 C15 106.6(4) . . ? C17 C16 H16A 126.7 . . ? C15 C16 H16A 126.7 . . ? N4 C17 C16 105.8(4) . . ? N4 C17 C18 123.0(4) . . ? C16 C17 C18 131.2(5) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N5 C20 C21 110.8(5) . . ? N5 C20 C19 123.4(5) . . ? C21 C20 C19 125.8(5) . . ? C22 C21 C20 107.1(5) . . ? C22 C21 H21A 126.5 . . ? C20 C21 H21A 126.5 . . ? N6 C22 C21 105.5(5) . . ? N6 C22 C23 123.9(5) . . ? C21 C22 C23 130.6(5) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Cl2A C24A Cl1A 109.4(4) . . ? Cl2A C24A H24A 109.8 . . ? Cl1A C24A H24A 109.8 . . ? Cl2A C24A H24B 109.8 . . ? Cl1A C24A H24B 109.8 . . ? H24A C24A H24B 108.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 Rh1 N1 C10 -27.2(10) . . . . ? C3 Rh1 N1 C10 -37.7(5) . . . . ? C2 Rh1 N1 C10 55.8(5) . . . . ? C1 Rh1 N1 C10 23.1(5) . . . . ? N5 Rh1 N1 C10 -135.3(5) . . . . ? N3 Rh1 N1 C10 143.8(5) . . . . ? C4 Rh1 N1 N2 161.2(7) . . . . ? C3 Rh1 N1 N2 150.7(3) . . . . ? C2 Rh1 N1 N2 -115.8(3) . . . . ? C1 Rh1 N1 N2 -148.5(3) . . . . ? N5 Rh1 N1 N2 53.1(3) . . . . ? N3 Rh1 N1 N2 -27.8(3) . . . . ? C10 N1 N2 C12 0.2(5) . . . . ? Rh1 N1 N2 C12 174.5(3) . . . . ? C10 N1 N2 C5 165.8(4) . . . . ? Rh1 N1 N2 C5 -19.9(5) . . . . ? C4 Rh1 N3 C15 15.8(5) . . . . ? C3 Rh1 N3 C15 20.4(6) . . . . ? C2 Rh1 N3 C15 -50.0(5) . . . . ? C1 Rh1 N3 C15 -73.8(5) . . . . ? N5 Rh1 N3 C15 115.9(5) . . . . ? N1 Rh1 N3 C15 -162.0(5) . . . . ? C4 Rh1 N3 N4 -140.9(3) . . . . ? C3 Rh1 N3 N4 -136.3(4) . . . . ? C2 Rh1 N3 N4 153.2(3) . . . . ? C1 Rh1 N3 N4 129.5(3) . . . . ? N5 Rh1 N3 N4 -40.9(3) . . . . ? N1 Rh1 N3 N4 41.3(3) . . . . ? C15 N3 N4 C17 -1.7(5) . . . . ? Rh1 N3 N4 C17 161.6(3) . . . . ? C15 N3 N4 C5 -169.1(4) . . . . ? Rh1 N3 N4 C5 -5.8(5) . . . . ? C4 Rh1 N5 C20 -32.4(5) . . . . ? C3 Rh1 N5 C20 9.0(5) . . . . ? C2 Rh1 N5 C20 -83.4(8) . . . . ? C1 Rh1 N5 C20 61.7(7) . . . . ? N1 Rh1 N5 C20 134.4(5) . . . . ? N3 Rh1 N5 C20 -140.3(5) . . . . ? C4 Rh1 N5 N6 158.4(3) . . . . ? C3 Rh1 N5 N6 -160.1(3) . . . . ? C2 Rh1 N5 N6 107.4(6) . . . . ? C1 Rh1 N5 N6 -107.5(5) . . . . ? N1 Rh1 N5 N6 -34.8(3) . . . . ? N3 Rh1 N5 N6 50.6(3) . . . . ? C20 N5 N6 C22 1.2(5) . . . . ? Rh1 N5 N6 C22 173.7(3) . . . . ? C20 N5 N6 C5 172.5(4) . . . . ? Rh1 N5 N6 C5 -15.1(5) . . . . ? C4 Rh1 C1 C2 -65.5(3) . . . . ? C3 Rh1 C1 C2 -105.5(4) . . . . ? N5 Rh1 C1 C2 -164.2(4) . . . . ? N1 Rh1 C1 C2 125.0(3) . . . . ? N3 Rh1 C1 C2 41.1(4) . . . . ? C4 Rh1 C1 C8 39.9(3) . . . . ? C3 Rh1 C1 C8 -0.1(3) . . . . ? C2 Rh1 C1 C8 105.4(5) . . . . ? N5 Rh1 C1 C8 -58.8(6) . . . . ? N1 Rh1 C1 C8 -129.6(3) . . . . ? N3 Rh1 C1 C8 146.5(3) . . . . ? C8 C1 C2 C6 -0.2(5) . . . . ? Rh1 C1 C2 C6 91.4(3) . . . . ? C8 C1 C2 Rh1 -91.7(4) . . . . ? C4 Rh1 C2 C1 103.5(4) . . . . ? C3 Rh1 C2 C1 63.2(3) . . . . ? N5 Rh1 C2 C1 158.9(5) . . . . ? N1 Rh1 C2 C1 -61.9(3) . . . . ? N3 Rh1 C2 C1 -145.5(3) . . . . ? C4 Rh1 C2 C6 -1.4(3) . . . . ? C3 Rh1 C2 C6 -41.6(3) . . . . ? C1 Rh1 C2 C6 -104.9(5) . . . . ? N5 Rh1 C2 C6 54.0(8) . . . . ? N1 Rh1 C2 C6 -166.8(3) . . . . ? N3 Rh1 C2 C6 109.6(3) . . . . ? C2 Rh1 C3 C4 66.4(3) . . . . ? C1 Rh1 C3 C4 103.2(3) . . . . ? N5 Rh1 C3 C4 -96.4(3) . . . . ? N1 Rh1 C3 C4 176.2(3) . . . . ? N3 Rh1 C3 C4 -6.7(5) . . . . ? C4 Rh1 C3 C8 -103.1(5) . . . . ? C2 Rh1 C3 C8 -36.7(3) . . . . ? C1 Rh1 C3 C8 0.1(3) . . . . ? N5 Rh1 C3 C8 160.5(3) . . . . ? N1 Rh1 C3 C8 73.2(4) . . . . ? N3 Rh1 C3 C8 -109.8(4) . . . . ? C8 C3 C4 C6 0.6(5) . . . . ? Rh1 C3 C4 C6 -94.4(3) . . . . ? C8 C3 C4 Rh1 95.0(4) . . . . ? C2 Rh1 C4 C3 -101.7(3) . . . . ? C1 Rh1 C4 C3 -64.5(3) . . . . ? N5 Rh1 C4 C3 92.5(3) . . . . ? N1 Rh1 C4 C3 -13.1(9) . . . . ? N3 Rh1 C4 C3 176.4(3) . . . . ? C3 Rh1 C4 C6 103.1(4) . . . . ? C2 Rh1 C4 C6 1.4(3) . . . . ? C1 Rh1 C4 C6 38.6(3) . . . . ? N5 Rh1 C4 C6 -164.4(3) . . . . ? N1 Rh1 C4 C6 90.0(8) . . . . ? N3 Rh1 C4 C6 -80.5(3) . . . . ? C17 N4 C5 N2 134.1(5) . . . . ? N3 N4 C5 N2 -60.7(5) . . . . ? C17 N4 C5 N6 -100.7(5) . . . . ? N3 N4 C5 N6 64.5(5) . . . . ? C12 N2 C5 N4 -118.5(5) . . . . ? N1 N2 C5 N4 78.3(5) . . . . ? C12 N2 C5 N6 115.9(5) . . . . ? N1 N2 C5 N6 -47.3(5) . . . . ? C22 N6 C5 N4 116.1(5) . . . . ? N5 N6 C5 N4 -53.9(5) . . . . ? C22 N6 C5 N2 -118.4(5) . . . . ? N5 N6 C5 N2 71.7(5) . . . . ? C1 C2 C6 C7 33.4(5) . . . . ? Rh1 C2 C6 C7 105.8(4) . . . . ? C1 C2 C6 C4 -70.7(5) . . . . ? Rh1 C2 C6 C4 1.7(4) . . . . ? C3 C4 C6 C7 -33.8(5) . . . . ? Rh1 C4 C6 C7 -105.7(4) . . . . ? C3 C4 C6 C2 70.2(5) . . . . ? Rh1 C4 C6 C2 -1.7(4) . . . . ? C2 C6 C7 C8 -50.0(5) . . . . ? C4 C6 C7 C8 50.2(5) . . . . ? C4 C3 C8 C1 -71.2(5) . . . . ? Rh1 C3 C8 C1 -0.2(4) . . . . ? C4 C3 C8 C7 32.1(5) . . . . ? Rh1 C3 C8 C7 103.2(4) . . . . ? C2 C1 C8 C3 72.2(5) . . . . ? Rh1 C1 C8 C3 0.2(4) . . . . ? C2 C1 C8 C7 -32.3(5) . . . . ? Rh1 C1 C8 C7 -104.4(4) . . . . ? C6 C7 C8 C3 -50.4(5) . . . . ? C6 C7 C8 C1 49.7(5) . . . . ? N2 N1 C10 C11 0.1(5) . . . . ? Rh1 N1 C10 C11 -172.1(3) . . . . ? N2 N1 C10 C9 -178.3(4) . . . . ? Rh1 N1 C10 C9 9.5(8) . . . . ? N1 C10 C11 C12 -0.3(6) . . . . ? C9 C10 C11 C12 178.0(5) . . . . ? N1 N2 C12 C11 -0.4(5) . . . . ? C5 N2 C12 C11 -164.6(4) . . . . ? N1 N2 C12 C13 -179.8(4) . . . . ? C5 N2 C12 C13 15.9(7) . . . . ? C10 C11 C12 N2 0.4(5) . . . . ? C10 C11 C12 C13 179.8(5) . . . . ? N4 N3 C15 C16 0.5(5) . . . . ? Rh1 N3 C15 C16 -158.4(3) . . . . ? N4 N3 C15 C14 178.1(4) . . . . ? Rh1 N3 C15 C14 19.2(7) . . . . ? N3 C15 C16 C17 0.9(6) . . . . ? C14 C15 C16 C17 -176.6(5) . . . . ? N3 N4 C17 C16 2.3(5) . . . . ? C5 N4 C17 C16 168.3(4) . . . . ? N3 N4 C17 C18 -178.7(4) . . . . ? C5 N4 C17 C18 -12.7(8) . . . . ? C15 C16 C17 N4 -1.8(5) . . . . ? C15 C16 C17 C18 179.2(5) . . . . ? N6 N5 C20 C21 -0.9(5) . . . . ? Rh1 N5 C20 C21 -171.0(4) . . . . ? N6 N5 C20 C19 179.9(5) . . . . ? Rh1 N5 C20 C19 9.8(8) . . . . ? N5 C20 C21 C22 0.3(6) . . . . ? C19 C20 C21 C22 179.5(5) . . . . ? N5 N6 C22 C21 -1.1(5) . . . . ? C5 N6 C22 C21 -171.7(4) . . . . ? N5 N6 C22 C23 -179.4(5) . . . . ? C5 N6 C22 C23 9.9(8) . . . . ? C20 C21 C22 N6 0.4(6) . . . . ? C20 C21 C22 C23 178.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.987 _refine_diff_density_min -0.818 _refine_diff_density_rms 0.101 data_3+ _database_code_depnum_ccdc_archive 'CCDC 716568' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H34 Ir N6, F6 P' _chemical_formula_sum 'C24 H34 F6 Ir N6 P' _chemical_formula_weight 743.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.1562(7) _cell_length_b 14.3677(8) _cell_length_c 17.1605(9) _cell_angle_alpha 90.00 _cell_angle_beta 108.9090(10) _cell_angle_gamma 90.00 _cell_volume 2835.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 173 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.742 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 4.829 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.810552 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.5 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4998 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4998 _reflns_number_gt 3898 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; SQUEEZE was used as there is diffuse solvent present in the structure, details of the procedure can be found at the end of this cif file Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4998 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0579 _refine_ls_wR_factor_gt 0.0551 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 Ir1 Ir 0.832340(14) 0.134955(11) 0.287457(10) 0.02973(6) Uani 1 1 d . . . P1 P 0.36591(11) 0.06456(8) 0.19275(8) 0.0392(3) Uani 1 1 d . . . F1 F 0.3068(3) -0.0006(2) 0.24336(19) 0.0642(8) Uani 1 1 d . . . F2 F 0.4210(3) 0.1301(2) 0.1403(2) 0.0672(9) Uani 1 1 d . . . F3 F 0.4913(3) 0.0318(2) 0.2472(2) 0.0712(10) Uani 1 1 d . . . F4 F 0.3597(3) -0.01904(19) 0.13022(17) 0.0588(8) Uani 1 1 d . . . F5 F 0.2394(2) 0.0972(2) 0.13607(19) 0.0625(8) Uani 1 1 d . . . F6 F 0.3708(3) 0.14751(19) 0.25437(19) 0.0608(8) Uani 1 1 d . . . N1 N 0.8390(3) 0.0666(2) 0.1802(2) 0.0294(8) Uani 1 1 d . . . N2 N 0.9434(3) 0.0268(2) 0.1829(2) 0.0284(8) Uani 1 1 d . . . N3 N 0.9212(3) 0.0141(2) 0.3446(2) 0.0331(9) Uani 1 1 d . . . N4 N 1.0151(3) -0.0153(2) 0.3236(2) 0.0336(9) Uani 1 1 d . . . N5 N 1.1508(3) 0.1355(2) 0.3618(2) 0.0325(8) Uani 1 1 d . . . N6 N 1.0817(3) 0.1245(2) 0.2813(2) 0.0302(8) Uani 1 1 d . . . C1 C 0.7807(4) 0.2620(3) 0.2217(3) 0.0365(11) Uani 1 1 d . . . H1A H 0.7734 0.2577 0.1621 0.044 Uiso 1 1 calc R . . C2 C 0.6860(4) 0.2245(3) 0.2402(3) 0.0370(11) Uani 1 1 d . . . H2A H 0.6239 0.1988 0.1913 0.044 Uiso 1 1 calc R . . C3 C 0.9032(4) 0.2303(3) 0.3852(3) 0.0383(11) Uani 1 1 d . . . H3A H 0.9821 0.2120 0.4225 0.046 Uiso 1 1 calc R . . C4 C 0.8118(4) 0.1799(3) 0.4000(3) 0.0401(11) Uani 1 1 d . . . H4A H 0.8387 0.1335 0.4457 0.048 Uiso 1 1 calc R . . C5 C 1.0428(4) 0.0292(3) 0.2571(3) 0.0311(10) Uani 1 1 d . . . H5A H 1.1080 -0.0057 0.2469 0.037 Uiso 1 1 calc R . . C6 C 0.8520(4) 0.3441(3) 0.2655(3) 0.0393(11) Uani 1 1 d . . . H6A H 0.8042 0.4013 0.2510 0.047 Uiso 1 1 calc R . . H6B H 0.9199 0.3519 0.2462 0.047 Uiso 1 1 calc R . . C7 C 0.8949(4) 0.3320(3) 0.3600(3) 0.0431(12) Uani 1 1 d . . . H7A H 0.9724 0.3613 0.3832 0.052 Uiso 1 1 calc R . . H7B H 0.8408 0.3644 0.3833 0.052 Uiso 1 1 calc R . . C8 C 0.6912(4) 0.2177(4) 0.3875(3) 0.0495(13) Uani 1 1 d . . . H8A H 0.6943 0.2623 0.4322 0.059 Uiso 1 1 calc R . . H8B H 0.6391 0.1659 0.3908 0.059 Uiso 1 1 calc R . . C9 C 0.6412(4) 0.2666(3) 0.3040(3) 0.0475(13) Uani 1 1 d . . . H9A H 0.5554 0.2621 0.2853 0.057 Uiso 1 1 calc R . . H9B H 0.6624 0.3334 0.3105 0.057 Uiso 1 1 calc R . . C10 C 0.6399(4) 0.0740(3) 0.0768(3) 0.0392(11) Uani 1 1 d . . . H10A H 0.6038 0.0541 0.1175 0.059 Uiso 1 1 calc R . . H10B H 0.5995 0.0448 0.0236 0.059 Uiso 1 1 calc R . . H10C H 0.6345 0.1418 0.0710 0.059 Uiso 1 1 calc R . . C11 C 0.7647(4) 0.0455(3) 0.1049(3) 0.0309(10) Uani 1 1 d . . . C12 C 0.8217(4) -0.0080(3) 0.0616(3) 0.0324(10) Uani 1 1 d . . . H12A H 0.7885 -0.0318 0.0074 0.039 Uiso 1 1 calc R . . C13 C 0.9346(4) -0.0199(3) 0.1119(2) 0.0307(10) Uani 1 1 d . . . C14 C 1.0307(4) -0.0736(3) 0.0993(3) 0.0396(11) Uani 1 1 d . . . H14A H 1.0989 -0.0334 0.1091 0.059 Uiso 1 1 calc R . . H14B H 1.0069 -0.0970 0.0426 0.059 Uiso 1 1 calc R . . H14C H 1.0501 -0.1261 0.1378 0.059 Uiso 1 1 calc R . . C15 C 0.8046(5) -0.0482(3) 0.4286(3) 0.0543(14) Uani 1 1 d . . . H15A H 0.8324 -0.0248 0.4853 0.081 Uiso 1 1 calc R . . H15B H 0.7734 -0.1112 0.4281 0.081 Uiso 1 1 calc R . . H15C H 0.7434 -0.0071 0.3947 0.081 Uiso 1 1 calc R . . C16 C 0.9028(4) -0.0506(3) 0.3948(3) 0.0409(12) Uani 1 1 d . . . C17 C 0.9869(5) -0.1204(3) 0.4059(3) 0.0456(13) Uani 1 1 d . . . H17A H 0.9938 -0.1743 0.4392 0.055 Uiso 1 1 calc R . . C18 C 1.0571(4) -0.0983(3) 0.3610(3) 0.0407(12) Uani 1 1 d . . . C19 C 1.1599(4) -0.1452(3) 0.3496(3) 0.0536(14) Uani 1 1 d . . . H19A H 1.1842 -0.1969 0.3887 0.080 Uiso 1 1 calc R . . H19B H 1.2238 -0.1005 0.3594 0.080 Uiso 1 1 calc R . . H19C H 1.1394 -0.1692 0.2932 0.080 Uiso 1 1 calc R . . C20 C 1.2661(4) 0.2614(3) 0.4446(3) 0.0497(13) Uani 1 1 d . . . H20A H 1.2461 0.2333 0.4902 0.075 Uiso 1 1 calc R . . H20B H 1.2550 0.3290 0.4449 0.075 Uiso 1 1 calc R . . H20C H 1.3476 0.2479 0.4509 0.075 Uiso 1 1 calc R . . C21 C 1.1891(4) 0.2219(3) 0.3644(3) 0.0358(11) Uani 1 1 d . . . C22 C 1.1502(4) 0.2648(3) 0.2876(3) 0.0376(11) Uani 1 1 d . . . H22A H 1.1668 0.3265 0.2750 0.045 Uiso 1 1 calc R . . C23 C 1.0834(4) 0.2009(3) 0.2338(3) 0.0319(10) Uani 1 1 d . . . C24 C 1.0241(4) 0.2100(3) 0.1428(3) 0.0430(12) Uani 1 1 d . . . H24A H 1.0597 0.1669 0.1137 0.064 Uiso 1 1 calc R . . H24B H 1.0325 0.2739 0.1256 0.064 Uiso 1 1 calc R . . H24C H 0.9414 0.1952 0.1296 0.064 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.03056(10) 0.03118(10) 0.02480(9) -0.00111(9) 0.00532(7) -0.00024(9) P1 0.0328(7) 0.0375(7) 0.0464(8) -0.0056(6) 0.0116(6) 0.0011(5) F1 0.082(2) 0.0538(19) 0.067(2) -0.0035(16) 0.0369(18) -0.0165(17) F2 0.065(2) 0.064(2) 0.085(2) 0.0094(18) 0.0416(18) -0.0005(17) F3 0.0496(19) 0.075(2) 0.071(2) -0.0074(18) -0.0050(16) 0.0205(17) F4 0.074(2) 0.0499(18) 0.0519(18) -0.0162(14) 0.0193(16) 0.0079(15) F5 0.0395(16) 0.071(2) 0.068(2) -0.0051(17) 0.0051(15) 0.0126(15) F6 0.066(2) 0.0476(18) 0.071(2) -0.0235(15) 0.0243(17) -0.0070(15) N1 0.0290(19) 0.0299(19) 0.026(2) 0.0028(15) 0.0038(16) 0.0020(16) N2 0.0238(19) 0.0297(19) 0.0258(19) 0.0004(15) 0.0001(15) 0.0009(15) N3 0.034(2) 0.034(2) 0.025(2) 0.0033(16) 0.0002(17) -0.0046(17) N4 0.035(2) 0.026(2) 0.032(2) 0.0046(16) 0.0003(17) -0.0022(16) N5 0.0295(19) 0.0305(19) 0.031(2) -0.0013(17) 0.0007(16) -0.0065(17) N6 0.0288(19) 0.0242(19) 0.033(2) 0.0020(16) 0.0036(16) 0.0005(15) C1 0.036(3) 0.034(3) 0.032(3) 0.003(2) -0.001(2) 0.010(2) C2 0.030(2) 0.038(3) 0.036(3) -0.007(2) 0.002(2) 0.004(2) C3 0.039(3) 0.045(3) 0.027(3) -0.008(2) 0.006(2) -0.001(2) C4 0.044(3) 0.045(3) 0.030(3) -0.007(2) 0.010(2) -0.002(2) C5 0.031(2) 0.028(2) 0.029(2) 0.0008(19) 0.004(2) 0.0001(19) C6 0.040(3) 0.033(3) 0.043(3) 0.000(2) 0.010(2) 0.004(2) C7 0.037(3) 0.038(3) 0.048(3) -0.010(2) 0.005(2) -0.004(2) C8 0.043(3) 0.059(3) 0.052(3) -0.017(3) 0.024(3) -0.006(3) C9 0.027(3) 0.053(3) 0.058(3) -0.017(3) 0.008(2) 0.005(2) C10 0.038(3) 0.042(3) 0.032(3) -0.004(2) 0.002(2) 0.000(2) C11 0.033(2) 0.032(2) 0.024(2) 0.0039(19) 0.003(2) -0.006(2) C12 0.032(2) 0.038(3) 0.025(2) -0.003(2) 0.006(2) -0.003(2) C13 0.036(3) 0.030(2) 0.025(2) 0.0007(19) 0.010(2) -0.004(2) C14 0.038(3) 0.044(3) 0.037(3) -0.006(2) 0.012(2) -0.004(2) C15 0.080(4) 0.046(3) 0.035(3) -0.002(2) 0.017(3) -0.022(3) C16 0.055(3) 0.038(3) 0.026(3) 0.001(2) 0.007(2) -0.017(2) C17 0.062(3) 0.033(3) 0.029(3) 0.006(2) -0.004(2) -0.012(2) C18 0.045(3) 0.026(2) 0.035(3) 0.001(2) -0.009(2) -0.003(2) C19 0.046(3) 0.032(3) 0.063(4) 0.009(3) -0.008(3) 0.011(2) C20 0.059(3) 0.048(3) 0.039(3) -0.009(2) 0.011(3) -0.021(3) C21 0.032(2) 0.033(3) 0.042(3) -0.006(2) 0.011(2) -0.005(2) C22 0.034(3) 0.032(2) 0.047(3) 0.003(2) 0.013(2) -0.003(2) C23 0.028(2) 0.029(2) 0.037(3) 0.007(2) 0.008(2) 0.0038(19) C24 0.040(3) 0.046(3) 0.038(3) 0.011(2) 0.006(2) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 N3 2.112(3) . ? Ir1 N1 2.111(3) . ? Ir1 C3 2.121(4) . ? Ir1 C4 2.127(4) . ? Ir1 C1 2.130(4) . ? Ir1 C2 2.131(4) . ? P1 F3 1.579(3) . ? P1 F6 1.582(3) . ? P1 F2 1.593(3) . ? P1 F4 1.596(3) . ? P1 F5 1.601(3) . ? P1 F1 1.598(3) . ? N1 C11 1.349(5) . ? N1 N2 1.379(4) . ? N2 C13 1.364(5) . ? N2 C5 1.444(5) . ? N3 C16 1.334(5) . ? N3 N4 1.371(5) . ? N4 C18 1.371(5) . ? N4 C5 1.442(5) . ? N5 C21 1.322(5) . ? N5 N6 1.374(5) . ? N6 C23 1.371(5) . ? N6 C5 1.464(5) . ? C1 C2 1.396(6) . ? C1 C6 1.511(6) . ? C2 C9 1.500(6) . ? C3 C4 1.416(6) . ? C3 C7 1.518(6) . ? C4 C8 1.512(6) . ? C6 C7 1.544(6) . ? C8 C9 1.533(7) . ? C10 C11 1.493(6) . ? C11 C12 1.399(6) . ? C12 C13 1.375(6) . ? C13 C14 1.473(6) . ? C15 C16 1.486(7) . ? C16 C17 1.401(7) . ? C17 C18 1.359(7) . ? C18 C19 1.488(7) . ? C20 C21 1.502(6) . ? C21 C22 1.392(6) . ? C22 C23 1.366(6) . ? C23 C24 1.499(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ir1 N1 82.19(13) . . ? N3 Ir1 C3 98.53(16) . . ? N1 Ir1 C3 150.46(16) . . ? N3 Ir1 C4 91.17(16) . . ? N1 Ir1 C4 169.18(15) . . ? C3 Ir1 C4 38.96(17) . . ? N3 Ir1 C1 165.76(15) . . ? N1 Ir1 C1 91.44(15) . . ? C3 Ir1 C1 80.78(18) . . ? C4 Ir1 C1 96.86(18) . . ? N3 Ir1 C2 155.72(16) . . ? N1 Ir1 C2 102.25(15) . . ? C3 Ir1 C2 89.20(17) . . ? C4 Ir1 C2 80.41(18) . . ? C1 Ir1 C2 38.26(16) . . ? F3 P1 F6 90.55(17) . . ? F3 P1 F2 90.52(19) . . ? F6 P1 F2 90.05(17) . . ? F3 P1 F4 89.97(17) . . ? F6 P1 F4 179.46(19) . . ? F2 P1 F4 90.12(17) . . ? F3 P1 F5 178.95(19) . . ? F6 P1 F5 90.33(17) . . ? F2 P1 F5 88.88(18) . . ? F4 P1 F5 89.16(16) . . ? F3 P1 F1 91.21(19) . . ? F6 P1 F1 90.24(17) . . ? F2 P1 F1 178.2(2) . . ? F4 P1 F1 89.58(16) . . ? F5 P1 F1 89.38(18) . . ? C11 N1 N2 105.2(3) . . ? C11 N1 Ir1 137.5(3) . . ? N2 N1 Ir1 117.3(2) . . ? C13 N2 N1 111.6(3) . . ? C13 N2 C5 126.9(3) . . ? N1 N2 C5 121.2(3) . . ? C16 N3 N4 106.5(4) . . ? C16 N3 Ir1 134.8(3) . . ? N4 N3 Ir1 118.4(3) . . ? C18 N4 N3 111.1(4) . . ? C18 N4 C5 127.6(4) . . ? N3 N4 C5 120.0(3) . . ? C21 N5 N6 103.7(3) . . ? C23 N6 N5 112.5(3) . . ? C23 N6 C5 130.2(4) . . ? N5 N6 C5 115.4(3) . . ? C2 C1 C6 124.8(4) . . ? C2 C1 Ir1 70.9(2) . . ? C6 C1 Ir1 112.5(3) . . ? C1 C2 C9 122.1(4) . . ? C1 C2 Ir1 70.8(2) . . ? C9 C2 Ir1 114.9(3) . . ? C4 C3 C7 124.1(4) . . ? C4 C3 Ir1 70.8(2) . . ? C7 C3 Ir1 115.1(3) . . ? C3 C4 C8 124.9(4) . . ? C3 C4 Ir1 70.3(3) . . ? C8 C4 Ir1 112.0(3) . . ? N4 C5 N2 110.1(3) . . ? N4 C5 N6 109.1(3) . . ? N2 C5 N6 111.9(3) . . ? C1 C6 C7 112.2(4) . . ? C3 C7 C6 112.1(4) . . ? C4 C8 C9 111.7(4) . . ? C2 C9 C8 111.7(4) . . ? N1 C11 C12 109.9(4) . . ? N1 C11 C10 122.8(4) . . ? C12 C11 C10 127.3(4) . . ? C13 C12 C11 107.4(4) . . ? N2 C13 C12 105.9(4) . . ? N2 C13 C14 123.5(4) . . ? C12 C13 C14 130.5(4) . . ? N3 C16 C17 108.5(4) . . ? N3 C16 C15 124.0(5) . . ? C17 C16 C15 127.4(4) . . ? C18 C17 C16 108.7(4) . . ? C17 C18 N4 105.2(4) . . ? C17 C18 C19 132.6(4) . . ? N4 C18 C19 122.3(5) . . ? N5 C21 C22 112.0(4) . . ? N5 C21 C20 119.6(4) . . ? C22 C21 C20 128.3(4) . . ? C23 C22 C21 106.7(4) . . ? C22 C23 N6 104.9(4) . . ? C22 C23 C24 128.7(4) . . ? N6 C23 C24 126.4(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.646 _refine_diff_density_min -0.627 _refine_diff_density_rms 0.090 # 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 0.500 0.000 120 48 ' ' 2 0.500 0.000 0.500 120 48 ' ' _platon_squeeze_details ; ; data_4+ _database_code_depnum_ccdc_archive 'CCDC 716569' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H32 N6 Rh, F6 P' _chemical_formula_sum 'C22 H32 F6 N6 P Rh' _chemical_formula_weight 628.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 14.481(3) _cell_length_b 12.148(2) _cell_length_c 15.203(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2674.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 0.763 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.436149 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens CCD area detector' _diffrn_measurement_method '\w scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13824 _diffrn_reflns_av_R_equivalents 0.3124 _diffrn_reflns_av_sigmaI/netI 0.2011 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2475 _reflns_number_gt 1096 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The data collected for this compound was very weak and hence there are a number of non-ideal parameters (high Rint, some strange thermal parameters, large weighting scheme). Attempts were made to resolve these issues but nothing was successful. We are confident that despite these issues the choice of space group and connectivities are correct. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0975P)^2^+35.9544P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2475 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2148 _refine_ls_R_factor_gt 0.0830 _refine_ls_wR_factor_ref 0.2642 _refine_ls_wR_factor_gt 0.1799 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 0.04326(10) 0.2500 0.24447(12) 0.0265(5) Uani 1 2 d S . . P1 P -0.1398(4) 0.2500 0.7950(4) 0.0347(15) Uani 1 2 d S . . F1 F -0.0310(8) 0.2500 0.8020(9) 0.053(4) Uani 1 2 d S . . F2 F -0.2502(9) 0.2500 0.7886(9) 0.054(4) Uani 1 2 d S . . F3 F -0.1447(6) 0.1579(7) 0.8696(6) 0.046(2) Uani 1 1 d . . . F4 F -0.1355(7) 0.1564(8) 0.7203(6) 0.065(3) Uani 1 1 d . . . N1 N -0.0569(7) 0.1306(9) 0.3016(8) 0.031(3) Uani 1 1 d . . . N2 N -0.0845(7) 0.1530(10) 0.3857(8) 0.029(3) Uani 1 1 d . . . N5 N 0.1001(10) 0.2500 0.3733(10) 0.023(4) Uani 1 2 d S . . N6 N 0.0434(11) 0.2500 0.4445(9) 0.022(3) Uani 1 2 d S . . C1 C 0.1321(11) 0.1423(13) 0.1828(9) 0.041(4) Uani 1 1 d . . . H1A H 0.1985 0.1618 0.1853 0.049 Uiso 1 1 calc R . . H1B H 0.1206 0.0631 0.1935 0.049 Uiso 1 1 calc R . . C2 C 0.0809(10) 0.1906(12) 0.1130(10) 0.038(4) Uani 1 1 d . . . C3 C 0.0340(12) 0.1285(14) 0.0430(10) 0.057(5) Uani 1 1 d . . . H3A H 0.0763 0.1184 -0.0067 0.086 Uiso 1 1 calc R . . H3B H -0.0206 0.1695 0.0233 0.086 Uiso 1 1 calc R . . H3C H 0.0149 0.0565 0.0656 0.086 Uiso 1 1 calc R . . C5 C -0.0564(12) 0.2500 0.4320(13) 0.026(5) Uani 1 2 d S . . H5A H -0.0866 0.2500 0.4911 0.031 Uiso 1 2 calc SR . . C6 C -0.0885(12) -0.0151(14) 0.1910(11) 0.054(5) Uani 1 1 d . . . H6A H -0.0464 0.0288 0.1547 0.081 Uiso 1 1 calc R . . H6B H -0.1490 -0.0194 0.1623 0.081 Uiso 1 1 calc R . . H6C H -0.0633 -0.0895 0.1982 0.081 Uiso 1 1 calc R . . C7 C -0.0989(10) 0.0379(12) 0.2795(10) 0.036(4) Uani 1 1 d . . . C8 C -0.1521(10) 0.0013(12) 0.3492(12) 0.043(4) Uani 1 1 d . . . H8A H -0.1886 -0.0637 0.3497 0.052 Uiso 1 1 calc R . . C9 C -0.1435(10) 0.0740(13) 0.4166(10) 0.038(4) Uani 1 1 d . . . C10 C -0.1861(11) 0.0769(14) 0.5055(11) 0.054(5) Uani 1 1 d . . . H10A H -0.2262 0.0127 0.5131 0.081 Uiso 1 1 calc R . . H10B H -0.2227 0.1443 0.5118 0.081 Uiso 1 1 calc R . . H10C H -0.1374 0.0757 0.5503 0.081 Uiso 1 1 calc R . . C11 C 0.2712(13) 0.2500 0.3538(16) 0.051(7) Uani 1 2 d S . . H11A H 0.2534 0.2500 0.2916 0.076 Uiso 1 2 calc SR . . H11B H 0.3080 0.1841 0.3665 0.076 Uiso 0.50 1 calc PR . . H11C H 0.3080 0.3159 0.3665 0.076 Uiso 0.50 1 calc PR . . C12 C 0.1836(11) 0.2500 0.4116(14) 0.027(5) Uani 1 2 d S . . C13 C 0.1797(13) 0.2500 0.5010(15) 0.033(5) Uani 1 2 d S . . H13A H 0.2305 0.2500 0.5406 0.039 Uiso 1 2 calc SR . . C14 C 0.0852(14) 0.2500 0.5228(14) 0.031(5) Uani 1 2 d S . . C15 C 0.0385(15) 0.2500 0.6085(13) 0.043(6) Uani 1 2 d S . . H15A H -0.0285 0.2500 0.5995 0.064 Uiso 1 2 calc SR . . H15B H 0.0564 0.3159 0.6415 0.064 Uiso 0.50 1 calc PR . . H15C H 0.0564 0.1841 0.6415 0.064 Uiso 0.50 1 calc PR . . 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 0.0230(7) 0.0195(8) 0.0370(10) 0.000 -0.0002(9) 0.000 P1 0.026(3) 0.030(3) 0.048(4) 0.000 0.014(3) 0.000 F1 0.025(7) 0.052(9) 0.081(10) 0.000 0.022(7) 0.000 F2 0.034(7) 0.054(9) 0.073(10) 0.000 0.012(7) 0.000 F3 0.045(5) 0.031(5) 0.063(6) 0.015(4) 0.016(5) 0.002(5) F4 0.063(6) 0.062(7) 0.071(8) -0.020(5) 0.019(5) -0.002(6) N1 0.027(7) 0.024(7) 0.041(8) 0.002(6) -0.005(6) 0.003(6) N2 0.015(6) 0.029(7) 0.043(8) -0.002(6) 0.009(6) -0.010(6) N5 0.021(9) 0.021(10) 0.027(10) 0.000 0.003(7) 0.000 N6 0.022(8) 0.030(9) 0.014(8) 0.000 -0.012(8) 0.000 C1 0.039(9) 0.037(10) 0.046(11) -0.010(8) 0.005(8) -0.002(8) C2 0.034(8) 0.040(10) 0.039(10) 0.001(8) -0.007(7) 0.000(8) C3 0.071(12) 0.060(12) 0.041(10) -0.023(9) 0.006(10) -0.022(11) C5 0.014(11) 0.039(13) 0.026(11) 0.000 0.001(9) 0.000 C6 0.051(10) 0.042(12) 0.069(14) -0.017(10) -0.001(9) 0.006(10) C7 0.038(9) 0.014(8) 0.055(12) 0.005(7) -0.011(7) 0.010(7) C8 0.043(10) 0.013(8) 0.073(13) 0.010(8) -0.003(9) -0.003(8) C9 0.024(8) 0.047(11) 0.042(10) -0.005(9) 0.002(7) -0.003(8) C10 0.050(11) 0.037(11) 0.075(13) -0.009(9) 0.022(10) -0.025(9) C11 0.017(12) 0.064(18) 0.071(18) 0.000 0.003(11) 0.000 C12 0.001(9) 0.034(13) 0.045(14) 0.000 -0.005(8) 0.000 C13 0.020(11) 0.028(13) 0.050(15) 0.000 -0.005(10) 0.000 C14 0.023(10) 0.024(12) 0.044(15) 0.000 0.005(10) 0.000 C15 0.038(13) 0.060(16) 0.031(13) 0.000 -0.001(12) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 2.061(15) 8_565 ? Rh1 C1 2.061(15) . ? Rh1 N5 2.125(16) . ? Rh1 C2 2.193(15) . ? Rh1 C2 2.193(15) 8_565 ? Rh1 N1 2.228(12) . ? Rh1 N1 2.228(12) 8_565 ? P1 F1 1.578(12) . ? P1 F3 1.594(9) 8_565 ? P1 F3 1.594(9) . ? P1 F2 1.603(14) . ? P1 F4 1.609(10) . ? P1 F4 1.609(10) 8_565 ? N1 C7 1.323(17) . ? N1 N2 1.366(15) . ? N2 C9 1.368(17) . ? N2 C5 1.432(15) . ? N5 C12 1.34(2) . ? N5 N6 1.36(2) . ? N6 C14 1.34(2) . ? N6 C5 1.46(2) . ? C1 C2 1.42(2) . ? C2 C2 1.44(3) 8_565 ? C2 C3 1.471(19) . ? C5 N2 1.432(15) 8_565 ? C6 C7 1.50(2) . ? C7 C8 1.38(2) . ? C8 C9 1.36(2) . ? C9 C10 1.49(2) . ? C11 C12 1.54(3) . ? C12 C13 1.36(3) . ? C13 C14 1.41(3) . ? C14 C15 1.47(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Rh1 C1 78.8(9) 8_565 . ? C1 Rh1 N5 100.2(5) 8_565 . ? C1 Rh1 N5 100.2(5) . . ? C1 Rh1 C2 68.8(6) 8_565 . ? C1 Rh1 C2 38.9(5) . . ? N5 Rh1 C2 138.0(5) . . ? C1 Rh1 C2 38.9(5) 8_565 8_565 ? C1 Rh1 C2 68.8(6) . 8_565 ? N5 Rh1 C2 138.0(5) . 8_565 ? C2 Rh1 C2 38.4(8) . 8_565 ? C1 Rh1 N1 175.9(5) 8_565 . ? C1 Rh1 N1 99.8(5) . . ? N5 Rh1 N1 83.8(4) . . ? C2 Rh1 N1 107.6(5) . . ? C2 Rh1 N1 137.0(5) 8_565 . ? C1 Rh1 N1 99.8(5) 8_565 8_565 ? C1 Rh1 N1 175.9(5) . 8_565 ? N5 Rh1 N1 83.8(4) . 8_565 ? C2 Rh1 N1 137.0(5) . 8_565 ? C2 Rh1 N1 107.6(5) 8_565 8_565 ? N1 Rh1 N1 81.2(6) . 8_565 ? F1 P1 F3 89.8(5) . 8_565 ? F1 P1 F3 89.8(5) . . ? F3 P1 F3 89.1(7) 8_565 . ? F1 P1 F2 179.6(8) . . ? F3 P1 F2 89.9(5) 8_565 . ? F3 P1 F2 89.9(5) . . ? F1 P1 F4 90.5(6) . . ? F3 P1 F4 179.5(6) 8_565 . ? F3 P1 F4 90.5(5) . . ? F2 P1 F4 89.8(6) . . ? F1 P1 F4 90.5(6) . 8_565 ? F3 P1 F4 90.5(5) 8_565 8_565 ? F3 P1 F4 179.5(6) . 8_565 ? F2 P1 F4 89.8(6) . 8_565 ? F4 P1 F4 89.9(8) . 8_565 ? C7 N1 N2 105.8(12) . . ? C7 N1 Rh1 139.0(11) . . ? N2 N1 Rh1 115.2(8) . . ? N1 N2 C9 111.3(11) . . ? N1 N2 C5 122.7(12) . . ? C9 N2 C5 125.9(13) . . ? C12 N5 N6 101.5(15) . . ? C12 N5 Rh1 138.5(13) . . ? N6 N5 Rh1 120.0(11) . . ? C14 N6 N5 115.8(16) . . ? C14 N6 C5 124.4(16) . . ? N5 N6 C5 119.7(14) . . ? C2 C1 Rh1 75.6(9) . . ? C1 C2 C2 114.4(9) . 8_565 ? C1 C2 C3 124.8(14) . . ? C2 C2 C3 120.8(9) 8_565 . ? C1 C2 Rh1 65.5(8) . . ? C2 C2 Rh1 70.8(4) 8_565 . ? C3 C2 Rh1 135.5(11) . . ? N2 C5 N2 110.8(16) . 8_565 ? N2 C5 N6 110.3(10) . . ? N2 C5 N6 110.3(10) 8_565 . ? N1 C7 C8 109.6(14) . . ? N1 C7 C6 123.2(15) . . ? C8 C7 C6 127.2(15) . . ? C9 C8 C7 108.5(14) . . ? C8 C9 N2 104.7(13) . . ? C8 C9 C10 131.6(15) . . ? N2 C9 C10 123.7(14) . . ? N5 C12 C13 113.3(17) . . ? N5 C12 C11 119.6(19) . . ? C13 C12 C11 127.1(17) . . ? C12 C13 C14 106.0(18) . . ? N6 C14 C13 103.3(18) . . ? N6 C14 C15 125.6(18) . . ? C13 C14 C15 131(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.490 _refine_diff_density_min -1.300 _refine_diff_density_rms 0.188