# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_4 _database_code_depnum_ccdc_archive 'CCDC 905985' #TrackingRef 'web_deposit_cif_file_0_Daran_1350302338.al464_pub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H26 Cl Fe N4 P Rh, B F4, 2(C2 H3 N)' _chemical_formula_sum 'C41 H38 B Cl F4 Fe N6 P Rh' _chemical_formula_weight 926.76 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' B B 0.0013 0.0007 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9788(3) _cell_length_b 13.0213(4) _cell_length_c 15.2286(4) _cell_angle_alpha 109.575(2) _cell_angle_beta 90.802(2) _cell_angle_gamma 110.176(2) _cell_volume 1904.59(9) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 23061 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 28.23 _exptl_crystal_description box _exptl_crystal_colour orange _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 940 _exptl_absorpt_coefficient_mu 0.986 _exptl_absorpt_correction_T_min 0.80404 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. CrysAlisPro (Agilent Technologies,2012) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'Xcalibur, Sapphire1, long nozzle' _diffrn_detector_area_resol_mean 8.2632 _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32054 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7775 _reflns_number_gt 6949 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysAlisPro (Agilent Technologies, 2012)' _computing_cell_refinement CrysAlisPro _computing_data_reduction CrysAlisPro _computing_structure_solution 'SIR-97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1996); ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material SHELXL-97 _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^)+(0.0326P)^2^+2.6168P] 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 7775 _refine_ls_number_parameters 508 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0757 _refine_ls_wR_factor_gt 0.0715 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _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 0.384741(16) 0.122378(15) 0.800385(12) 0.01472(6) Uani 1 1 d . . . Fe1 Fe 0.45398(3) 0.20591(3) 0.59772(2) 0.01847(8) Uani 1 1 d . . . Cl1 Cl 0.46049(6) -0.04033(5) 0.75816(4) 0.02296(13) Uani 1 1 d . . . P1 P 0.21730(5) 0.05852(5) 0.67734(4) 0.01471(12) Uani 1 1 d . . . N1 N 0.4281(2) 0.37837(17) 0.84367(14) 0.0222(4) Uani 1 1 d . . . N2 N 0.2706(2) 0.30322(17) 0.91175(14) 0.0217(4) Uani 1 1 d . . . N3 N 0.53012(19) 0.19125(17) 0.91827(14) 0.0190(4) Uani 1 1 d . . . N4 N 0.28291(19) 0.04295(17) 0.89513(14) 0.0191(4) Uani 1 1 d . . . C1 C 0.5091(2) 0.1879(2) 0.71830(16) 0.0189(5) Uani 1 1 d . . . C2 C 0.5614(2) 0.3069(2) 0.72496(17) 0.0219(5) Uani 1 1 d . . . C3 C 0.6413(2) 0.3177(2) 0.65286(19) 0.0265(5) Uani 1 1 d . . . H3 H 0.6878 0.3880 0.6425 0.032 Uiso 1 1 calc R . . C4 C 0.6385(2) 0.2046(2) 0.5999(2) 0.0282(6) Uani 1 1 d . . . H4 H 0.6833 0.1854 0.5475 0.034 Uiso 1 1 calc R . . C5 C 0.5568(2) 0.1242(2) 0.63881(18) 0.0238(5) Uani 1 1 d . . . H5 H 0.5370 0.0420 0.6160 0.029 Uiso 1 1 calc R . . C6 C 0.2620(2) 0.1270(2) 0.59123(17) 0.0191(5) Uani 1 1 d . . . C7 C 0.2955(2) 0.2490(2) 0.60443(19) 0.0255(5) Uani 1 1 d . . . H7 H 0.2809 0.3064 0.6565 0.031 Uiso 1 1 calc R . . C8 C 0.3541(3) 0.2680(3) 0.5262(2) 0.0320(6) Uani 1 1 d . . . H8 H 0.3845 0.3405 0.5165 0.038 Uiso 1 1 calc R . . C9 C 0.3597(3) 0.1622(3) 0.46528(19) 0.0325(6) Uani 1 1 d . . . H9 H 0.3959 0.1511 0.4081 0.039 Uiso 1 1 calc R . . C10 C 0.3023(3) 0.0748(2) 0.50396(18) 0.0268(5) Uani 1 1 d . . . H10 H 0.2921 -0.0053 0.4764 0.032 Uiso 1 1 calc R . . C11 C 0.3556(2) 0.2754(2) 0.85295(16) 0.0192(5) Uani 1 1 d . . . C12 C 0.2896(3) 0.4204(2) 0.9365(2) 0.0302(6) Uani 1 1 d . . . H12 H 0.2413 0.4602 0.9760 0.036 Uiso 1 1 calc R . . C13 C 0.3881(3) 0.4670(2) 0.8947(2) 0.0305(6) Uani 1 1 d . . . H13 H 0.4241 0.5465 0.8993 0.037 Uiso 1 1 calc R . . C111 C 0.1480(2) -0.09774(19) 0.60560(17) 0.0182(5) Uani 1 1 d . . . C112 C 0.1690(2) -0.1800(2) 0.63640(18) 0.0240(5) Uani 1 1 d . . . H112 H 0.2263 -0.1547 0.6932 0.029 Uiso 1 1 calc R . . C113 C 0.1070(3) -0.2987(2) 0.5848(2) 0.0330(6) Uani 1 1 d . . . H113 H 0.1219 -0.3545 0.6063 0.040 Uiso 1 1 calc R . . C114 C 0.0238(3) -0.3363(2) 0.5023(2) 0.0321(6) Uani 1 1 d . . . H114 H -0.0192 -0.4179 0.4673 0.038 Uiso 1 1 calc R . . C115 C 0.0031(3) -0.2552(2) 0.47104(19) 0.0287(6) Uani 1 1 d . . . H115 H -0.0537 -0.2812 0.4139 0.034 Uiso 1 1 calc R . . C116 C 0.0640(2) -0.1365(2) 0.52189(18) 0.0231(5) Uani 1 1 d . . . H116 H 0.0487 -0.0812 0.4999 0.028 Uiso 1 1 calc R . . C121 C 0.0670(2) 0.0843(2) 0.71060(16) 0.0201(5) Uani 1 1 d . . . C122 C -0.0453(2) -0.0073(2) 0.71105(17) 0.0259(5) Uani 1 1 d . . . H122 H -0.0442 -0.0840 0.6948 0.031 Uiso 1 1 calc R . . C123 C -0.1590(3) 0.0124(3) 0.73499(19) 0.0347(7) Uani 1 1 d . . . H123 H -0.2347 -0.0504 0.7362 0.042 Uiso 1 1 calc R . . C124 C -0.1621(3) 0.1220(3) 0.7567(2) 0.0399(7) Uani 1 1 d . . . H124 H -0.2409 0.1346 0.7712 0.048 Uiso 1 1 calc R . . C125 C -0.0516(3) 0.2143(3) 0.7579(2) 0.0386(7) Uani 1 1 d . . . H125 H -0.0539 0.2906 0.7740 0.046 Uiso 1 1 calc R . . C126 C 0.0633(3) 0.1960(2) 0.73550(18) 0.0270(5) Uani 1 1 d . . . H126 H 0.1396 0.2602 0.7372 0.032 Uiso 1 1 calc R . . C211 C 0.1678(2) 0.2280(2) 0.94694(19) 0.0261(5) Uani 1 1 d . . . H21A H 0.1210 0.1529 0.8957 0.039 Uiso 1 1 calc R . . H21B H 0.1061 0.2665 0.9709 0.039 Uiso 1 1 calc R . . H21C H 0.2071 0.2141 0.9979 0.039 Uiso 1 1 calc R . . C221 C 0.5449(3) 0.4083(2) 0.79773(19) 0.0280(6) Uani 1 1 d . . . H22A H 0.6234 0.4487 0.8466 0.034 Uiso 1 1 calc R . . H22B H 0.5407 0.4644 0.7682 0.034 Uiso 1 1 calc R . . C311 C 0.6526(2) 0.2645(2) 0.92489(18) 0.0241(5) Uani 1 1 d . . . H311 H 0.6783 0.2868 0.8726 0.029 Uiso 1 1 calc R . . C312 C 0.7433(3) 0.3091(2) 1.00437(19) 0.0289(6) Uani 1 1 d . . . H312 H 0.8305 0.3600 1.0069 0.035 Uiso 1 1 calc R . . C313 C 0.7039(3) 0.2776(2) 1.0805(2) 0.0327(6) Uani 1 1 d . . . H313 H 0.7638 0.3084 1.1369 0.039 Uiso 1 1 calc R . . C314 C 0.5779(3) 0.2018(2) 1.07450(19) 0.0296(6) Uani 1 1 d . . . H314 H 0.5501 0.1795 1.1264 0.035 Uiso 1 1 calc R . . C315 C 0.4921(2) 0.1584(2) 0.99181(17) 0.0210(5) Uani 1 1 d . . . C411 C 0.3566(2) 0.0733(2) 0.97803(17) 0.0209(5) Uani 1 1 d . . . C412 C 0.3073(3) 0.0258(2) 1.04492(19) 0.0297(6) Uani 1 1 d . . . H412 H 0.3602 0.0483 1.1031 0.036 Uiso 1 1 calc R . . C413 C 0.1801(3) -0.0548(3) 1.0259(2) 0.0331(6) Uani 1 1 d . . . H413 H 0.1441 -0.0871 1.0714 0.040 Uiso 1 1 calc R . . C414 C 0.1064(3) -0.0878(2) 0.94072(19) 0.0286(6) Uani 1 1 d . . . H414 H 0.0195 -0.1445 0.9257 0.034 Uiso 1 1 calc R . . C415 C 0.1611(2) -0.0369(2) 0.87752(18) 0.0221(5) Uani 1 1 d . . . H415 H 0.1098 -0.0597 0.8186 0.027 Uiso 1 1 calc R . . N5 N 0.0985(4) 0.4897(3) 0.1049(3) 0.0668(9) Uani 1 1 d . . . C511 C 0.0741(3) 0.4670(3) 0.1693(3) 0.0501(9) Uani 1 1 d . . . C512 C 0.0431(4) 0.4364(5) 0.2520(3) 0.0707(13) Uani 1 1 d . . . H51A H -0.0144 0.3535 0.2322 0.106 Uiso 1 1 calc R . . H51B H -0.0016 0.4854 0.2903 0.106 Uiso 1 1 calc R . . H51C H 0.1242 0.4497 0.2893 0.106 Uiso 1 1 calc R . . N6 N 0.7559(3) 0.4852(3) 0.3051(2) 0.0519(7) Uani 1 1 d . . . C611 C 0.6880(3) 0.4413(3) 0.3477(3) 0.0456(8) Uani 1 1 d . . . C612 C 0.6032(4) 0.3853(5) 0.4033(4) 0.0841(15) Uani 1 1 d . . . H61A H 0.5985 0.3043 0.3858 0.126 Uiso 1 1 calc R . . H61B H 0.5152 0.3853 0.3916 0.126 Uiso 1 1 calc R . . H61C H 0.6384 0.4284 0.4703 0.126 Uiso 1 1 calc R . . B1 B 0.2968(4) 0.2952(3) 0.2263(3) 0.0524(10) Uani 1 1 d . . . F11 F 0.3524(3) 0.3202(2) 0.15071(19) 0.0932(9) Uani 1 1 d . . . F12 F 0.3191(2) 0.39710(18) 0.30234(17) 0.0661(6) Uani 1 1 d . . . F13 F 0.3630(3) 0.2323(2) 0.2485(2) 0.0868(8) Uani 1 1 d . . . F14 F 0.1683(3) 0.2273(2) 0.2003(3) 0.1037(10) Uani 1 1 d . . . 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 0.01619(9) 0.01542(9) 0.01332(10) 0.00554(7) 0.00192(7) 0.00646(7) Fe1 0.02088(17) 0.01919(17) 0.01692(18) 0.00814(14) 0.00497(13) 0.00766(13) Cl1 0.0263(3) 0.0229(3) 0.0235(3) 0.0088(2) 0.0035(2) 0.0132(2) P1 0.0170(3) 0.0138(3) 0.0140(3) 0.0049(2) 0.0019(2) 0.0066(2) N1 0.0263(10) 0.0176(10) 0.0197(11) 0.0041(8) 0.0025(8) 0.0071(8) N2 0.0258(10) 0.0197(10) 0.0191(10) 0.0045(8) 0.0048(8) 0.0103(8) N3 0.0207(9) 0.0185(9) 0.0178(10) 0.0052(8) 0.0018(8) 0.0084(8) N4 0.0233(10) 0.0203(10) 0.0152(10) 0.0064(8) 0.0031(8) 0.0101(8) C1 0.0165(10) 0.0241(12) 0.0171(12) 0.0087(10) 0.0022(9) 0.0076(9) C2 0.0178(11) 0.0244(12) 0.0193(12) 0.0073(10) 0.0009(9) 0.0036(9) C3 0.0198(12) 0.0303(13) 0.0275(14) 0.0143(11) 0.0050(10) 0.0032(10) C4 0.0243(12) 0.0373(15) 0.0299(14) 0.0165(12) 0.0112(11) 0.0152(11) C5 0.0225(12) 0.0318(13) 0.0262(13) 0.0154(11) 0.0091(10) 0.0158(10) C6 0.0189(11) 0.0212(11) 0.0179(12) 0.0084(10) 0.0010(9) 0.0070(9) C7 0.0254(12) 0.0265(13) 0.0326(15) 0.0167(11) 0.0058(11) 0.0133(10) C8 0.0303(14) 0.0378(15) 0.0386(16) 0.0283(13) 0.0045(12) 0.0111(12) C9 0.0340(14) 0.0400(16) 0.0180(13) 0.0137(12) 0.0015(11) 0.0045(12) C10 0.0289(13) 0.0275(13) 0.0179(13) 0.0056(10) 0.0016(10) 0.0060(11) C11 0.0217(11) 0.0193(11) 0.0146(11) 0.0054(9) 0.0013(9) 0.0060(9) C12 0.0377(15) 0.0231(13) 0.0291(15) 0.0034(11) 0.0072(12) 0.0164(11) C13 0.0410(15) 0.0172(12) 0.0307(15) 0.0048(11) 0.0071(12) 0.0113(11) C111 0.0186(11) 0.0156(10) 0.0186(12) 0.0041(9) 0.0015(9) 0.0063(9) C112 0.0269(12) 0.0195(11) 0.0235(13) 0.0068(10) -0.0032(10) 0.0073(10) C113 0.0398(15) 0.0196(12) 0.0392(16) 0.0118(12) -0.0027(13) 0.0096(11) C114 0.0362(15) 0.0167(12) 0.0325(15) 0.0023(11) -0.0048(12) 0.0039(11) C115 0.0297(13) 0.0257(13) 0.0234(14) 0.0039(11) -0.0041(11) 0.0068(11) C116 0.0254(12) 0.0214(12) 0.0225(13) 0.0071(10) -0.0015(10) 0.0095(10) C121 0.0216(11) 0.0284(12) 0.0137(11) 0.0072(10) 0.0015(9) 0.0137(10) C122 0.0222(12) 0.0339(14) 0.0181(12) 0.0060(11) 0.0015(10) 0.0094(11) C123 0.0214(13) 0.0560(19) 0.0195(13) 0.0082(13) 0.0026(10) 0.0113(12) C124 0.0335(15) 0.076(2) 0.0237(15) 0.0184(15) 0.0105(12) 0.0356(16) C125 0.0550(19) 0.0565(19) 0.0289(15) 0.0201(14) 0.0155(14) 0.0449(17) C126 0.0346(14) 0.0327(14) 0.0218(13) 0.0116(11) 0.0073(11) 0.0202(12) C211 0.0282(13) 0.0290(13) 0.0245(13) 0.0104(11) 0.0117(11) 0.0136(11) C221 0.0292(13) 0.0205(12) 0.0260(14) 0.0066(11) 0.0069(11) 0.0011(10) C311 0.0234(12) 0.0211(12) 0.0262(14) 0.0072(10) 0.0011(10) 0.0078(10) C312 0.0231(12) 0.0248(13) 0.0315(15) 0.0031(11) -0.0031(11) 0.0077(10) C313 0.0321(14) 0.0355(15) 0.0238(14) 0.0025(12) -0.0086(11) 0.0132(12) C314 0.0340(14) 0.0358(14) 0.0200(13) 0.0090(11) -0.0017(11) 0.0155(12) C315 0.0245(12) 0.0219(11) 0.0182(12) 0.0052(10) 0.0009(10) 0.0125(10) C411 0.0275(12) 0.0218(11) 0.0168(12) 0.0065(10) 0.0025(10) 0.0137(10) C412 0.0354(14) 0.0367(15) 0.0204(13) 0.0126(12) 0.0037(11) 0.0153(12) C413 0.0411(16) 0.0387(15) 0.0248(14) 0.0195(13) 0.0106(12) 0.0130(13) C414 0.0285(13) 0.0291(13) 0.0289(14) 0.0137(12) 0.0087(11) 0.0081(11) C415 0.0237(12) 0.0231(12) 0.0196(12) 0.0090(10) 0.0025(10) 0.0073(10) N5 0.066(2) 0.082(3) 0.058(2) 0.025(2) 0.0258(18) 0.0343(19) C511 0.0308(16) 0.056(2) 0.049(2) 0.0051(17) 0.0075(15) 0.0125(15) C512 0.0386(19) 0.108(4) 0.055(2) 0.030(2) 0.0106(18) 0.014(2) N6 0.0576(18) 0.0445(16) 0.0482(18) 0.0114(14) 0.0081(15) 0.0177(14) C611 0.0421(18) 0.0420(18) 0.053(2) 0.0156(16) 0.0039(16) 0.0171(15) C612 0.053(2) 0.109(4) 0.112(4) 0.072(4) 0.025(3) 0.024(3) B1 0.061(3) 0.0266(17) 0.054(3) 0.0127(17) -0.010(2) 0.0009(17) F11 0.132(3) 0.0476(14) 0.0721(18) 0.0134(13) 0.0108(17) 0.0084(15) F12 0.0714(15) 0.0424(11) 0.0715(15) 0.0073(11) 0.0055(12) 0.0188(11) F13 0.108(2) 0.0578(15) 0.0891(19) 0.0154(14) -0.0143(16) 0.0370(15) F14 0.0570(15) 0.0721(18) 0.143(3) 0.0162(18) -0.0210(17) 0.0019(13) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C11 2.022(2) . ? Rh1 C1 2.028(2) . ? Rh1 N3 2.104(2) . ? Rh1 N4 2.156(2) . ? Rh1 P1 2.3210(6) . ? Rh1 Cl1 2.4313(6) . ? Fe1 C6 1.985(2) . ? Fe1 C7 1.998(2) . ? Fe1 C2 2.008(2) . ? Fe1 C5 2.013(2) . ? Fe1 C10 2.016(3) . ? Fe1 C3 2.030(3) . ? Fe1 C4 2.032(3) . ? Fe1 C1 2.037(2) . ? Fe1 C8 2.052(3) . ? Fe1 C9 2.056(3) . ? P1 C6 1.804(2) . ? P1 C111 1.825(2) . ? P1 C121 1.840(2) . ? N1 C11 1.359(3) . ? N1 C13 1.373(3) . ? N1 C221 1.465(3) . ? N2 C11 1.358(3) . ? N2 C12 1.380(3) . ? N2 C211 1.458(3) . ? N3 C311 1.333(3) . ? N3 C315 1.350(3) . ? N4 C415 1.336(3) . ? N4 C411 1.350(3) . ? C1 C2 1.422(3) . ? C1 C5 1.439(3) . ? C2 C3 1.428(3) . ? C2 C221 1.481(3) . ? C3 C4 1.411(4) . ? C4 C5 1.426(4) . ? C6 C10 1.429(3) . ? C6 C7 1.442(3) . ? C7 C8 1.415(4) . ? C8 C9 1.403(4) . ? C9 C10 1.415(4) . ? C12 C13 1.330(4) . ? C111 C112 1.387(3) . ? C111 C116 1.395(3) . ? C112 C113 1.384(4) . ? C113 C114 1.378(4) . ? C114 C115 1.376(4) . ? C115 C116 1.381(3) . ? C121 C122 1.391(4) . ? C121 C126 1.391(3) . ? C122 C123 1.388(4) . ? C123 C124 1.365(5) . ? C124 C125 1.377(5) . ? C125 C126 1.388(4) . ? C311 C312 1.374(4) . ? C312 C313 1.381(4) . ? C313 C314 1.375(4) . ? C314 C315 1.384(4) . ? C315 C411 1.478(3) . ? C411 C412 1.386(4) . ? C412 C413 1.381(4) . ? C413 C414 1.371(4) . ? C414 C415 1.376(4) . ? N5 C511 1.126(5) . ? C511 C512 1.454(6) . ? N6 C611 1.129(4) . ? C611 C612 1.442(6) . ? B1 F14 1.348(5) . ? B1 F13 1.378(5) . ? B1 F12 1.378(5) . ? B1 F11 1.392(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 C11 Rh1 C1 89.97(9) . . ? C11 Rh1 N3 86.40(8) . . ? C1 Rh1 N3 94.51(8) . . ? C11 Rh1 N4 97.38(8) . . ? C1 Rh1 N4 168.75(8) . . ? N3 Rh1 N4 77.56(8) . . ? C11 Rh1 P1 88.92(7) . . ? C1 Rh1 P1 87.00(7) . . ? N3 Rh1 P1 175.08(5) . . ? N4 Rh1 P1 101.58(6) . . ? C11 Rh1 Cl1 168.68(7) . . ? C1 Rh1 Cl1 87.57(7) . . ? N3 Rh1 Cl1 82.78(5) . . ? N4 Rh1 Cl1 83.56(5) . . ? P1 Rh1 Cl1 101.98(2) . . ? C6 Fe1 C7 42.45(10) . . ? C6 Fe1 C2 118.21(10) . . ? C7 Fe1 C2 103.23(11) . . ? C6 Fe1 C5 112.38(10) . . ? C7 Fe1 C5 148.27(10) . . ? C2 Fe1 C5 69.14(10) . . ? C6 Fe1 C10 41.84(10) . . ? C7 Fe1 C10 69.86(11) . . ? C2 Fe1 C10 156.72(10) . . ? C5 Fe1 C10 104.53(11) . . ? C6 Fe1 C3 158.97(10) . . ? C7 Fe1 C3 126.12(11) . . ? C2 Fe1 C3 41.42(10) . . ? C5 Fe1 C3 69.21(11) . . ? C10 Fe1 C3 159.13(11) . . ? C6 Fe1 C4 151.23(10) . . ? C7 Fe1 C4 166.13(11) . . ? C2 Fe1 C4 69.04(10) . . ? C5 Fe1 C4 41.28(10) . . ? C10 Fe1 C4 121.78(11) . . ? C3 Fe1 C4 40.67(11) . . ? C6 Fe1 C1 96.99(9) . . ? C7 Fe1 C1 112.35(10) . . ? C2 Fe1 C1 41.15(10) . . ? C5 Fe1 C1 41.63(9) . . ? C10 Fe1 C1 119.38(10) . . ? C3 Fe1 C1 69.94(10) . . ? C4 Fe1 C1 69.94(10) . . ? C6 Fe1 C8 69.81(10) . . ? C7 Fe1 C8 40.88(11) . . ? C2 Fe1 C8 121.76(11) . . ? C5 Fe1 C8 167.18(11) . . ? C10 Fe1 C8 68.19(11) . . ? C3 Fe1 C8 113.62(11) . . ? C4 Fe1 C8 132.71(11) . . ? C1 Fe1 C8 151.02(11) . . ? C6 Fe1 C9 69.79(10) . . ? C7 Fe1 C9 68.83(12) . . ? C2 Fe1 C9 159.04(11) . . ? C5 Fe1 C9 127.87(12) . . ? C10 Fe1 C9 40.66(11) . . ? C3 Fe1 C9 127.02(11) . . ? C4 Fe1 C9 114.15(11) . . ? C1 Fe1 C9 159.59(11) . . ? C8 Fe1 C9 39.92(12) . . ? C6 P1 C111 103.18(11) . . ? C6 P1 C121 103.25(11) . . ? C111 P1 C121 100.36(11) . . ? C6 P1 Rh1 113.85(8) . . ? C111 P1 Rh1 118.15(8) . . ? C121 P1 Rh1 115.92(8) . . ? C11 N1 C13 111.1(2) . . ? C11 N1 C221 130.2(2) . . ? C13 N1 C221 118.4(2) . . ? C11 N2 C12 110.6(2) . . ? C11 N2 C211 129.3(2) . . ? C12 N2 C211 120.1(2) . . ? C311 N3 C315 119.4(2) . . ? C311 N3 Rh1 124.84(17) . . ? C315 N3 Rh1 115.70(16) . . ? C415 N4 C411 118.4(2) . . ? C415 N4 Rh1 127.11(16) . . ? C411 N4 Rh1 114.31(16) . . ? C2 C1 C5 105.8(2) . . ? C2 C1 Rh1 126.33(17) . . ? C5 C1 Rh1 127.80(18) . . ? C2 C1 Fe1 68.34(14) . . ? C5 C1 Fe1 68.29(13) . . ? Rh1 C1 Fe1 125.26(11) . . ? C1 C2 C3 109.7(2) . . ? C1 C2 C221 126.8(2) . . ? C3 C2 C221 123.4(2) . . ? C1 C2 Fe1 70.51(14) . . ? C3 C2 Fe1 70.09(14) . . ? C221 C2 Fe1 128.61(19) . . ? C4 C3 C2 107.5(2) . . ? C4 C3 Fe1 69.75(15) . . ? C2 C3 Fe1 68.49(14) . . ? C3 C4 C5 108.0(2) . . ? C3 C4 Fe1 69.58(14) . . ? C5 C4 Fe1 68.64(14) . . ? C4 C5 C1 109.0(2) . . ? C4 C5 Fe1 70.08(14) . . ? C1 C5 Fe1 70.08(13) . . ? C10 C6 C7 106.4(2) . . ? C10 C6 P1 124.19(18) . . ? C7 C6 P1 127.80(19) . . ? C10 C6 Fe1 70.25(14) . . ? C7 C6 Fe1 69.25(13) . . ? P1 C6 Fe1 114.03(12) . . ? C8 C7 C6 107.9(2) . . ? C8 C7 Fe1 71.63(15) . . ? C6 C7 Fe1 68.31(13) . . ? C9 C8 C7 108.8(2) . . ? C9 C8 Fe1 70.19(16) . . ? C7 C8 Fe1 67.49(14) . . ? C8 C9 C10 108.1(2) . . ? C8 C9 Fe1 69.89(15) . . ? C10 C9 Fe1 68.16(15) . . ? C9 C10 C6 108.8(2) . . ? C9 C10 Fe1 71.19(15) . . ? C6 C10 Fe1 67.91(14) . . ? N2 C11 N1 104.0(2) . . ? N2 C11 Rh1 129.29(17) . . ? N1 C11 Rh1 126.39(17) . . ? C13 C12 N2 107.2(2) . . ? C12 C13 N1 107.1(2) . . ? C112 C111 C116 119.0(2) . . ? C112 C111 P1 121.12(18) . . ? C116 C111 P1 119.64(18) . . ? C113 C112 C111 120.3(2) . . ? C114 C113 C112 120.3(2) . . ? C115 C114 C113 119.7(2) . . ? C114 C115 C116 120.7(2) . . ? C115 C116 C111 120.0(2) . . ? C122 C121 C126 118.6(2) . . ? C122 C121 P1 120.85(19) . . ? C126 C121 P1 120.56(19) . . ? C123 C122 C121 120.6(3) . . ? C124 C123 C122 120.1(3) . . ? C123 C124 C125 120.3(3) . . ? C124 C125 C126 120.1(3) . . ? C125 C126 C121 120.3(3) . . ? N1 C221 C2 114.8(2) . . ? N3 C311 C312 122.6(2) . . ? C311 C312 C313 118.1(3) . . ? C314 C313 C312 119.9(2) . . ? C313 C314 C315 119.1(3) . . ? N3 C315 C314 120.8(2) . . ? N3 C315 C411 116.4(2) . . ? C314 C315 C411 122.7(2) . . ? N4 C411 C412 121.4(2) . . ? N4 C411 C315 115.9(2) . . ? C412 C411 C315 122.8(2) . . ? C413 C412 C411 119.1(3) . . ? C414 C413 C412 119.5(3) . . ? C413 C414 C415 118.5(3) . . ? N4 C415 C414 123.1(2) . . ? N5 C511 C512 179.3(5) . . ? N6 C611 C612 179.0(4) . . ? F14 B1 F13 109.1(3) . . ? F14 B1 F12 112.6(4) . . ? F13 B1 F12 109.3(3) . . ? F14 B1 F11 110.8(4) . . ? F13 B1 F11 104.0(4) . . ? F12 B1 F11 110.7(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C12 H12 N5 0.9500 2.5400 3.420(5) 154.00 1_556 yes C211 H21C F11 0.9800 2.4700 3.291(4) 141.00 1_556 yes C221 H22B F11 0.9900 2.4800 3.123(4) 122.00 2_666 yes C221 H22B F12 0.9900 2.4900 3.319(4) 141.00 2_666 yes C512 H51C F12 0.9800 2.4900 3.361(5) 149.00 . yes C612 H61B F13 0.9800 2.4900 3.088(6) 119.00 . yes C112 H112 Cl1 0.9500 2.4700 3.248(3) 139.00 . yes C123 H123 F13 0.9500 2.3900 3.297(5) 159.00 2_556 yes C414 H414 F14 0.9500 2.4600 3.230(5) 138.00 2_556 yes _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.026 _refine_diff_density_min -0.729 _refine_diff_density_rms 0.072 #====END