# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Hallett, Andrew' _publ_contact_author_name 'Hallett, Andrew' _publ_contact_author_email hallettaj@cardiff.ac.uk _publ_section_title ; Homo- and heterodinuclear complexes of the tetrakis(pyrazolyl)borate ligand ; # Attachment '- Hallett_Dalton_Cifs.cif' data_1+ _database_code_depnum_ccdc_archive 'CCDC 768028' #TrackingRef '- Hallett_Dalton_Cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C28 H36 B N8 Rh2), 4(F6 P), C H2 Cl2' _chemical_formula_sum 'C113 H146 B4 Cl2 F24 N32 P4 Rh8' _chemical_formula_weight 3469.92 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' B B 0.0013 0.0007 '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 Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 28.003(7) _cell_length_b 13.173(3) _cell_length_c 17.633(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.475(16) _cell_angle_gamma 90.00 _cell_volume 6416(3) _cell_formula_units_Z 2 _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 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.796 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3476 _exptl_absorpt_coefficient_mu 1.191 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.586 _exptl_absorpt_correction_T_max 0.684 _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 'CCD area detector' _diffrn_measurement_method 'omega scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33881 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 27.49 _reflns_number_total 14570 _reflns_number_gt 13553 _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^)+(0.0316P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.008(13) _refine_ls_number_reflns 14570 _refine_ls_number_parameters 857 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0259 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0553 _refine_ls_wR_factor_gt 0.0547 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0.008 _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 0.936201(8) 0.617531(17) 0.617669(14) 0.02526(5) Uani 1 1 d . . . Rh2 Rh 0.964165(8) 0.256779(16) 0.764640(13) 0.02217(5) Uani 1 1 d . . . Rh1' Rh 0.692298(8) 1.512596(17) 0.712639(12) 0.02324(5) Uani 1 1 d . . . Rh2' Rh 0.793397(8) 1.453664(17) 0.991484(12) 0.02147(5) Uani 1 1 d . . . Cl1 Cl 0.99251(14) 0.25820(18) 0.98460(15) 0.0610(7) Uani 0.50 1 d P A -1 Cl2 Cl 0.91178(9) 0.1840(2) 1.05559(13) 0.0670(6) Uani 0.50 1 d P A -1 P1 P 1.0000 0.01148(9) 0.5000 0.0262(2) Uani 1 2 d S . . P2 P 1.23326(3) 0.45804(9) 0.65950(5) 0.0401(2) Uani 1 1 d . . . P1' P 0.5000 1.33237(10) 1.0000 0.0327(3) Uani 1 2 d S . . F1 F 0.95419(8) 0.0104(2) 0.54156(13) 0.0613(6) Uani 1 1 d . . . F2 F 1.02502(9) 0.09571(18) 0.55767(15) 0.0643(7) Uani 1 1 d . . . F3 F 1.02566(8) -0.07549(17) 0.55587(13) 0.0565(6) Uani 1 1 d . . . F4 F 1.2557(2) 0.3573(3) 0.6931(3) 0.155(2) Uani 1 1 d . . . F5 F 1.2167(3) 0.5631(5) 0.6316(4) 0.239(4) Uani 1 1 d . . . F6 F 1.26633(12) 0.4503(4) 0.59788(16) 0.1089(13) Uani 1 1 d . . . F7 F 1.19997(11) 0.4565(4) 0.72312(16) 0.1181(15) Uani 1 1 d . . . F8 F 1.27366(13) 0.5095(4) 0.7196(2) 0.1212(15) Uani 1 1 d . . . F9 F 1.19107(14) 0.4207(7) 0.6036(2) 0.229(4) Uani 1 1 d . . . F1' F 0.46396(18) 1.3343(3) 0.9236(2) 0.151(2) Uani 1 1 d . . . F2' F 0.53058(12) 1.2484(3) 0.9698(2) 0.1146(14) Uani 1 1 d . . . F3' F 0.52985(10) 1.4216(2) 0.9694(2) 0.0885(10) Uani 1 1 d . . . N1 N 1.01223(9) 0.6115(2) 0.61729(16) 0.0331(6) Uani 1 1 d . . . N2 N 1.04034(9) 0.53310(19) 0.65178(14) 0.0268(5) Uani 1 1 d . . . N3 N 0.93555(9) 0.4646(2) 0.59017(14) 0.0256(5) Uani 1 1 d . . . N4 N 0.97399(9) 0.40372(18) 0.61702(13) 0.0217(5) Uani 1 1 d . . . N5 N 1.03528(9) 0.2678(2) 0.73861(14) 0.0250(5) Uani 1 1 d . . . N6 N 1.04980(9) 0.34891(19) 0.69826(13) 0.0230(5) Uani 1 1 d . . . N7 N 0.97094(9) 0.40927(19) 0.79281(14) 0.0252(5) Uani 1 1 d . . . N8 N 0.99669(8) 0.47396(18) 0.75366(13) 0.0213(5) Uani 1 1 d . . . N1' N 0.71175(9) 1.59280(18) 0.81447(14) 0.0235(5) Uani 1 1 d . . . N2' N 0.70136(8) 1.55452(18) 0.88135(13) 0.0213(5) Uani 1 1 d . . . N3' N 0.63205(9) 1.4593(2) 0.76123(13) 0.0268(5) Uani 1 1 d . . . N4' N 0.63614(9) 1.42727(19) 0.83630(14) 0.0247(5) Uani 1 1 d . . . N5' N 0.76720(8) 1.35985(19) 0.89909(13) 0.0222(5) Uani 1 1 d . . . N6' N 0.71989(8) 1.36477(18) 0.86535(13) 0.0202(5) Uani 1 1 d . . . N7' N 0.72535(9) 1.4345(2) 1.02725(13) 0.0245(5) Uani 1 1 d . . . N8' N 0.68219(9) 1.43131(18) 0.97612(14) 0.0224(5) Uani 1 1 d . . . C1 C 0.93068(14) 0.7767(3) 0.5982(3) 0.0462(10) Uani 1 1 d . . . H1A H 0.9582 0.8064 0.5759 0.055 Uiso 1 1 calc R . . C2 C 0.94093(14) 0.7604(3) 0.6778(2) 0.0503(10) Uani 1 1 d . . . H2A H 0.9744 0.7801 0.7025 0.060 Uiso 1 1 calc R . . C3 C 0.85925(11) 0.6289(3) 0.5920(2) 0.0333(7) Uani 1 1 d . . . H3A H 0.8430 0.5724 0.5596 0.040 Uiso 1 1 calc R . . C4 C 0.87380(11) 0.6042(3) 0.66917(19) 0.0348(8) Uani 1 1 d . . . H4A H 0.8663 0.5322 0.6807 0.042 Uiso 1 1 calc R . . C5 C 0.94964(12) 0.1175(3) 0.7026(2) 0.0366(8) Uani 1 1 d . . . H5A H 0.9733 0.1016 0.6675 0.044 Uiso 1 1 calc R . . C6 C 0.96615(13) 0.0944(2) 0.7789(2) 0.0349(8) Uani 1 1 d . . . H6A H 0.9995 0.0648 0.7892 0.042 Uiso 1 1 calc R . . C7 C 0.88790(11) 0.2660(3) 0.7403(2) 0.0364(8) Uani 1 1 d . . . H7A H 0.8755 0.3371 0.7328 0.044 Uiso 1 1 calc R . . C8 C 0.90187(12) 0.2398(3) 0.8170(2) 0.0373(8) Uani 1 1 d . . . H8A H 0.8974 0.2951 0.8541 0.045 Uiso 1 1 calc R . . C9 C 0.87422(16) 0.6714(4) 0.7358(2) 0.0611(13) Uani 1 1 d . . . H9A H 0.8884 0.6342 0.7830 0.073 Uiso 1 1 calc R . . H9B H 0.8404 0.6888 0.7404 0.073 Uiso 1 1 calc R . . C10 C 0.90215(19) 0.7675(4) 0.7312(2) 0.0643(13) Uani 1 1 d . . . H10A H 0.9183 0.7861 0.7836 0.077 Uiso 1 1 calc R . . H10B H 0.8792 0.8226 0.7124 0.077 Uiso 1 1 calc R . . C11 C 0.84197(14) 0.7342(3) 0.5661(3) 0.0559(11) Uani 1 1 d . . . H11A H 0.8196 0.7286 0.5166 0.067 Uiso 1 1 calc R . . H11B H 0.8234 0.7628 0.6043 0.067 Uiso 1 1 calc R . . C12 C 0.88168(15) 0.8059(3) 0.5565(2) 0.0496(10) Uani 1 1 d . . . H12A H 0.8734 0.8738 0.5746 0.060 Uiso 1 1 calc R . . H12B H 0.8833 0.8116 0.5010 0.060 Uiso 1 1 calc R . . C13 C 0.89482(16) 0.1346(3) 0.8461(3) 0.0555(11) Uani 1 1 d . . . H13A H 0.8931 0.1387 0.9017 0.067 Uiso 1 1 calc R . . H13B H 0.8633 0.1084 0.8197 0.067 Uiso 1 1 calc R . . C14 C 0.93318(16) 0.0608(3) 0.8351(3) 0.0558(12) Uani 1 1 d . . . H14A H 0.9175 -0.0040 0.8165 0.067 Uiso 1 1 calc R . . H14B H 0.9534 0.0475 0.8856 0.067 Uiso 1 1 calc R . . C15 C 0.86663(15) 0.1954(4) 0.6775(3) 0.0622(12) Uani 1 1 d . . . H15A H 0.8354 0.1698 0.6891 0.075 Uiso 1 1 calc R . . H15B H 0.8597 0.2343 0.6289 0.075 Uiso 1 1 calc R . . C16 C 0.89756(14) 0.1069(4) 0.6655(3) 0.0565(11) Uani 1 1 d . . . H16A H 0.8962 0.0968 0.6095 0.068 Uiso 1 1 calc R . . H16B H 0.8840 0.0454 0.6861 0.068 Uiso 1 1 calc R . . C17 C 1.04281(14) 0.6827(3) 0.6029(3) 0.0484(10) Uani 1 1 d . . . H17 H 1.0333 0.7454 0.5782 0.058 Uiso 1 1 calc R . . C18 C 1.09016(14) 0.6547(3) 0.6282(3) 0.0485(10) Uani 1 1 d . . . H18 H 1.1185 0.6929 0.6246 0.058 Uiso 1 1 calc R . . C19 C 1.08768(11) 0.5603(3) 0.65955(19) 0.0333(7) Uani 1 1 d . . . H19 H 1.1144 0.5205 0.6828 0.040 Uiso 1 1 calc R . . C20 C 0.90758(12) 0.4119(3) 0.53497(18) 0.0316(7) Uani 1 1 d . . . H20 H 0.8781 0.4358 0.5062 0.038 Uiso 1 1 calc R . . C21 C 0.92785(12) 0.3168(3) 0.52561(18) 0.0332(7) Uani 1 1 d . . . H21 H 0.9154 0.2648 0.4906 0.040 Uiso 1 1 calc R . . C22 C 0.96976(11) 0.3152(2) 0.57826(17) 0.0269(6) Uani 1 1 d . . . H22 H 0.9922 0.2605 0.5861 0.032 Uiso 1 1 calc R . . C23 C 1.06932(11) 0.1971(3) 0.73991(18) 0.0303(7) Uani 1 1 d . . . H23 H 1.0689 0.1330 0.7646 0.036 Uiso 1 1 calc R . . C24 C 1.10562(11) 0.2293(3) 0.70041(19) 0.0327(7) Uani 1 1 d . . . H24 H 1.1340 0.1935 0.6933 0.039 Uiso 1 1 calc R . . C25 C 1.09133(11) 0.3243(2) 0.67406(17) 0.0265(6) Uani 1 1 d . . . H25 H 1.1082 0.3662 0.6435 0.032 Uiso 1 1 calc R . . C26 C 0.96227(12) 0.4605(3) 0.85433(17) 0.0318(7) Uani 1 1 d . . . H26 H 0.9450 0.4341 0.8920 0.038 Uiso 1 1 calc R . . C27 C 0.98201(12) 0.5580(3) 0.85602(19) 0.0332(7) Uani 1 1 d . . . H27 H 0.9808 0.6093 0.8935 0.040 Uiso 1 1 calc R . . C28 C 1.00347(11) 0.5632(2) 0.79186(18) 0.0294(7) Uani 1 1 d . . . H28 H 1.0204 0.6202 0.7766 0.035 Uiso 1 1 calc R . . C1' C 0.68301(13) 1.4014(3) 0.62292(17) 0.0337(7) Uani 1 1 d . . . H1' H 0.6617 1.3433 0.6322 0.040 Uiso 1 1 calc R . . C2' C 0.65773(12) 1.4896(3) 0.59686(17) 0.0348(8) Uani 1 1 d . . . H2' H 0.6218 1.4825 0.5910 0.042 Uiso 1 1 calc R . . C3' C 0.74264(12) 1.5933(3) 0.65536(17) 0.0306(7) Uani 1 1 d . . . H3' H 0.7540 1.6593 0.6800 0.037 Uiso 1 1 calc R . . C4' C 0.76473(10) 1.5081(3) 0.69235(17) 0.0294(7) Uani 1 1 d . . . H4' H 0.7892 1.5244 0.7387 0.035 Uiso 1 1 calc R . . C5' C 0.84484(12) 1.5155(3) 0.92902(18) 0.0392(8) Uani 1 1 d . . . H5' H 0.8389 1.4968 0.8733 0.047 Uiso 1 1 calc R . . C6' C 0.86707(11) 1.4389(3) 0.9765(2) 0.0408(9) Uani 1 1 d . . . H6' H 0.8739 1.3760 0.9484 0.049 Uiso 1 1 calc R . . C7' C 0.81221(13) 1.5863(3) 1.0596(2) 0.0386(8) Uani 1 1 d . . . H7' H 0.7838 1.6210 1.0760 0.046 Uiso 1 1 calc R . . C8' C 0.82758(13) 1.5006(3) 1.10299(17) 0.0401(8) Uani 1 1 d . . . H8' H 0.8083 1.4857 1.1447 0.048 Uiso 1 1 calc R . . C9' C 0.73020(13) 1.3695(3) 0.59904(19) 0.0384(8) Uani 1 1 d . . . H9C H 0.7313 1.3952 0.5466 0.046 Uiso 1 1 calc R . . H9D H 0.7317 1.2945 0.5975 0.046 Uiso 1 1 calc R . . C10' C 0.77435(13) 1.4097(3) 0.6543(2) 0.0375(8) Uani 1 1 d . . . H10C H 0.7846 1.3581 0.6945 0.045 Uiso 1 1 calc R . . H10D H 0.8014 1.4197 0.6253 0.045 Uiso 1 1 calc R . . C11' C 0.72675(13) 1.5991(3) 0.56881(18) 0.0382(8) Uani 1 1 d . . . H11C H 0.7475 1.5538 0.5434 0.046 Uiso 1 1 calc R . . H11D H 0.7313 1.6693 0.5513 0.046 Uiso 1 1 calc R . . C12' C 0.67400(14) 1.5685(3) 0.54471(19) 0.0436(9) Uani 1 1 d . . . H12D H 0.6533 1.6295 0.5446 0.052 Uiso 1 1 calc R . . H12C H 0.6695 1.5416 0.4916 0.052 Uiso 1 1 calc R . . C13' C 0.85012(16) 1.6279(3) 0.9429(2) 0.0547(10) Uani 1 1 d . . . H13C H 0.8251 1.6640 0.9065 0.066 Uiso 1 1 calc R . . H13D H 0.8822 1.6500 0.9327 0.066 Uiso 1 1 calc R . . C14' C 0.84505(16) 1.6569(3) 1.0252(3) 0.0537(11) Uani 1 1 d . . . H14C H 0.8775 1.6564 1.0576 0.064 Uiso 1 1 calc R . . H14D H 0.8321 1.7268 1.0253 0.064 Uiso 1 1 calc R . . C15' C 0.90339(13) 1.4597(4) 1.0480(2) 0.0541(11) Uani 1 1 d . . . H15C H 0.9195 1.5256 1.0426 0.065 Uiso 1 1 calc R . . H15D H 0.9285 1.4061 1.0542 0.065 Uiso 1 1 calc R . . C16' C 0.87884(14) 1.4623(4) 1.1194(2) 0.0573(11) Uani 1 1 d . . . H16C H 0.8789 1.3930 1.1411 0.069 Uiso 1 1 calc R . . H16D H 0.8979 1.5065 1.1586 0.069 Uiso 1 1 calc R . . C17' C 0.71857(12) 1.6912(2) 0.82402(18) 0.0305(7) Uani 1 1 d . . . H17' H 0.7265 1.7366 0.7861 0.037 Uiso 1 1 calc R . . C18' C 0.71248(13) 1.7189(3) 0.89832(19) 0.0363(8) Uani 1 1 d . . . H18' H 0.7153 1.7849 0.9203 0.044 Uiso 1 1 calc R . . C19' C 0.70165(11) 1.6310(2) 0.93254(18) 0.0297(7) Uani 1 1 d . . . H19' H 0.6954 1.6246 0.9837 0.036 Uiso 1 1 calc R . . C20' C 0.58799(11) 1.4305(3) 0.7270(2) 0.0356(8) Uani 1 1 d . . . H20' H 0.5749 1.4436 0.6747 0.043 Uiso 1 1 calc R . . C21' C 0.56354(13) 1.3783(3) 0.7785(2) 0.0442(9) Uani 1 1 d . . . H21' H 0.5320 1.3497 0.7686 0.053 Uiso 1 1 calc R . . C22' C 0.59545(12) 1.3779(3) 0.8461(2) 0.0350(7) Uani 1 1 d . . . H22' H 0.5898 1.3476 0.8927 0.042 Uiso 1 1 calc R . . C23' C 0.78657(11) 1.2808(2) 0.86871(17) 0.0273(6) Uani 1 1 d . . . H23' H 0.8193 1.2596 0.8822 0.033 Uiso 1 1 calc R . . C24' C 0.75217(12) 1.2331(2) 0.81417(17) 0.0300(7) Uani 1 1 d . . . H24' H 0.7566 1.1752 0.7840 0.036 Uiso 1 1 calc R . . C25' C 0.71077(11) 1.2881(2) 0.81365(17) 0.0258(6) Uani 1 1 d . . . H25' H 0.6805 1.2747 0.7822 0.031 Uiso 1 1 calc R . . C26' C 0.71351(12) 1.4298(3) 1.09740(17) 0.0319(7) Uani 1 1 d . . . H26' H 0.7361 1.4294 1.1439 0.038 Uiso 1 1 calc R . . C27' C 0.66338(13) 1.4256(3) 1.0930(2) 0.0367(8) Uani 1 1 d . . . H27' H 0.6457 1.4212 1.1345 0.044 Uiso 1 1 calc R . . C28' C 0.64536(12) 1.4291(2) 1.01673(19) 0.0304(7) Uani 1 1 d . . . H28' H 0.6119 1.4298 0.9952 0.037 Uiso 1 1 calc R . . C1S C 0.9739(3) 0.1738(7) 1.0522(4) 0.050(2) Uani 0.50 1 d P A -1 H1S1 H 0.9813 0.1033 1.0384 0.060 Uiso 0.50 1 calc PR A -1 H1S2 H 0.9925 0.1883 1.1038 0.060 Uiso 0.50 1 calc PR A -1 B1 B 1.01582(12) 0.4402(3) 0.67977(18) 0.0237(7) Uani 1 1 d . . . B1' B 0.68459(11) 1.4446(3) 0.88982(18) 0.0211(6) 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 0.02173(11) 0.02005(11) 0.03235(12) 0.00519(9) -0.00038(9) -0.00018(9) Rh2 0.02222(11) 0.01945(11) 0.02596(11) 0.00090(9) 0.00733(8) 0.00185(9) Rh1' 0.02150(11) 0.02413(12) 0.02222(10) -0.00130(9) -0.00194(8) -0.00213(10) Rh2' 0.01987(11) 0.02525(12) 0.01950(10) -0.00259(9) 0.00384(8) 0.00069(9) Cl1 0.074(2) 0.0577(11) 0.049(2) 0.0102(10) 0.0023(15) -0.0129(13) Cl2 0.0648(15) 0.0795(17) 0.0540(12) -0.0018(11) 0.0020(10) -0.0203(13) P1 0.0308(6) 0.0199(5) 0.0277(5) 0.000 0.0041(4) 0.000 P2 0.0360(5) 0.0571(6) 0.0275(4) 0.0025(4) 0.0065(3) 0.0015(5) P1' 0.0217(6) 0.0320(6) 0.0439(7) 0.000 0.0036(5) 0.000 F1 0.0495(14) 0.0791(17) 0.0610(14) -0.0136(14) 0.0262(11) -0.0140(14) F2 0.0580(15) 0.0447(14) 0.0870(18) -0.0356(13) 0.0026(13) -0.0117(12) F3 0.0540(14) 0.0471(13) 0.0580(14) 0.0251(11) -0.0214(11) -0.0098(11) F4 0.229(5) 0.068(2) 0.190(5) 0.056(3) 0.103(4) 0.046(3) F5 0.303(9) 0.176(6) 0.241(7) 0.110(5) 0.053(6) 0.144(6) F6 0.087(2) 0.193(4) 0.0566(16) 0.020(2) 0.0408(15) 0.031(3) F7 0.0591(18) 0.245(5) 0.0558(16) -0.020(2) 0.0270(13) 0.003(3) F8 0.098(3) 0.153(4) 0.119(3) -0.067(3) 0.036(2) -0.066(3) F9 0.072(2) 0.533(12) 0.078(2) -0.122(4) 0.0074(18) -0.108(4) F1' 0.207(5) 0.089(3) 0.113(3) 0.021(2) -0.098(3) -0.030(3) F2' 0.090(2) 0.071(2) 0.196(4) -0.057(2) 0.060(2) 0.0098(19) F3' 0.0638(18) 0.0569(17) 0.161(3) 0.0070(18) 0.067(2) -0.0051(14) N1 0.0267(13) 0.0248(13) 0.0463(16) 0.0120(13) 0.0017(11) 0.0015(12) N2 0.0222(12) 0.0250(14) 0.0325(13) 0.0056(10) 0.0026(10) 0.0003(10) N3 0.0195(12) 0.0267(13) 0.0286(12) 0.0039(11) -0.0018(9) 0.0013(11) N4 0.0217(12) 0.0217(12) 0.0219(12) 0.0031(9) 0.0036(9) 0.0005(10) N5 0.0238(12) 0.0228(13) 0.0286(12) 0.0037(11) 0.0053(10) 0.0030(11) N6 0.0208(12) 0.0248(13) 0.0234(12) 0.0021(10) 0.0037(9) -0.0002(10) N7 0.0250(13) 0.0222(13) 0.0291(13) -0.0005(10) 0.0069(10) 0.0006(10) N8 0.0180(11) 0.0201(12) 0.0253(12) 0.0020(9) 0.0020(9) 0.0007(9) N1' 0.0229(12) 0.0207(13) 0.0258(12) -0.0005(9) 0.0006(10) -0.0018(10) N2' 0.0202(12) 0.0216(12) 0.0208(11) -0.0016(9) 0.0000(9) 0.0022(10) N3' 0.0226(12) 0.0273(13) 0.0286(12) -0.0024(11) -0.0014(9) 0.0010(11) N4' 0.0178(12) 0.0254(13) 0.0301(13) -0.0007(10) 0.0014(10) -0.0022(10) N5' 0.0190(12) 0.0225(12) 0.0257(12) -0.0023(10) 0.0049(9) -0.0003(10) N6' 0.0198(12) 0.0177(12) 0.0232(12) -0.0008(9) 0.0040(9) -0.0007(10) N7' 0.0226(12) 0.0276(14) 0.0233(12) -0.0002(10) 0.0041(9) 0.0032(10) N8' 0.0199(12) 0.0191(12) 0.0292(12) -0.0020(9) 0.0071(10) 0.0017(10) C1 0.036(2) 0.0198(18) 0.084(3) 0.0144(18) 0.0121(19) 0.0011(14) C2 0.044(2) 0.0230(17) 0.074(3) -0.0078(19) -0.0209(19) -0.0036(17) C3 0.0210(15) 0.0306(18) 0.0466(19) -0.0032(15) 0.0011(13) 0.0011(14) C4 0.0194(15) 0.039(2) 0.0459(19) 0.0025(16) 0.0043(13) 0.0032(14) C5 0.0380(18) 0.0288(17) 0.0455(19) -0.0123(16) 0.0146(15) -0.0025(16) C6 0.0341(18) 0.0195(16) 0.054(2) 0.0040(14) 0.0166(15) 0.0063(13) C7 0.0222(15) 0.0299(18) 0.059(2) -0.0009(17) 0.0131(14) 0.0021(14) C8 0.0340(18) 0.0292(19) 0.055(2) -0.0023(15) 0.0254(16) 0.0001(15) C9 0.042(2) 0.088(4) 0.052(2) -0.019(2) 0.0023(19) 0.015(2) C10 0.090(4) 0.051(3) 0.048(2) -0.015(2) 0.000(2) 0.026(3) C11 0.038(2) 0.049(3) 0.075(3) 0.018(2) -0.0089(19) 0.0083(18) C12 0.056(3) 0.035(2) 0.054(2) 0.0172(18) -0.0018(19) 0.0110(19) C13 0.059(3) 0.040(2) 0.078(3) 0.011(2) 0.044(2) 0.002(2) C14 0.063(3) 0.036(2) 0.076(3) 0.023(2) 0.036(2) 0.008(2) C15 0.037(2) 0.073(3) 0.073(3) -0.014(2) -0.004(2) -0.001(2) C16 0.043(2) 0.063(3) 0.062(3) -0.026(2) 0.0046(19) -0.008(2) C17 0.039(2) 0.0286(19) 0.080(3) 0.0227(19) 0.0154(19) -0.0038(16) C18 0.0300(19) 0.038(2) 0.079(3) 0.0042(19) 0.0133(18) -0.0084(16) C19 0.0199(15) 0.0344(18) 0.0453(19) 0.0021(15) 0.0043(13) -0.0021(14) C20 0.0282(17) 0.0359(18) 0.0295(16) 0.0017(13) 0.0007(13) -0.0016(14) C21 0.0374(18) 0.0325(18) 0.0278(16) -0.0067(13) -0.0006(13) -0.0064(15) C22 0.0280(16) 0.0269(16) 0.0270(15) 0.0027(12) 0.0076(12) 0.0013(13) C23 0.0263(16) 0.0304(17) 0.0349(16) 0.0067(13) 0.0065(13) 0.0084(13) C24 0.0217(15) 0.0342(18) 0.0428(18) 0.0035(14) 0.0068(13) 0.0085(13) C25 0.0197(14) 0.0312(16) 0.0292(15) -0.0002(13) 0.0059(12) 0.0026(13) C26 0.0342(17) 0.0345(17) 0.0278(15) -0.0041(14) 0.0086(12) 0.0040(15) C27 0.0328(17) 0.0294(17) 0.0356(17) -0.0069(14) 0.0002(14) 0.0049(14) C28 0.0248(15) 0.0234(16) 0.0370(17) -0.0021(13) -0.0041(13) 0.0005(13) C1' 0.0369(18) 0.0387(19) 0.0237(15) -0.0076(13) -0.0009(13) -0.0082(15) C2' 0.0304(17) 0.045(2) 0.0252(15) -0.0055(13) -0.0075(12) -0.0041(15) C3' 0.0306(16) 0.0347(18) 0.0262(15) 0.0006(13) 0.0039(12) -0.0087(14) C4' 0.0184(14) 0.0432(19) 0.0259(14) -0.0023(15) 0.0014(11) -0.0040(15) C5' 0.0289(17) 0.062(2) 0.0291(16) -0.0072(17) 0.0118(13) -0.0175(18) C6' 0.0212(16) 0.059(3) 0.0437(19) -0.0234(18) 0.0089(14) -0.0012(16) C7' 0.0369(19) 0.039(2) 0.0424(19) -0.0235(16) 0.0130(15) -0.0067(15) C8' 0.0379(18) 0.060(2) 0.0218(15) -0.0118(16) 0.0047(13) -0.0119(18) C9' 0.049(2) 0.0335(19) 0.0318(17) -0.0049(14) 0.0055(15) -0.0008(16) C10' 0.0343(19) 0.043(2) 0.0373(18) 0.0008(15) 0.0116(14) 0.0054(16) C11' 0.044(2) 0.038(2) 0.0307(17) 0.0066(14) 0.0019(14) 0.0003(16) C12' 0.043(2) 0.057(2) 0.0287(17) 0.0072(16) 0.0004(15) 0.0076(18) C13' 0.058(3) 0.053(3) 0.055(2) 0.006(2) 0.0129(19) -0.020(2) C14' 0.053(3) 0.038(2) 0.071(3) -0.0133(19) 0.012(2) -0.0103(19) C15' 0.0273(18) 0.079(3) 0.052(2) -0.010(2) -0.0047(15) 0.005(2) C16' 0.041(2) 0.091(3) 0.0335(18) 0.007(2) -0.0122(15) -0.004(2) C17' 0.0355(18) 0.0224(15) 0.0324(16) 0.0009(12) 0.0026(13) -0.0068(13) C18' 0.051(2) 0.0189(15) 0.0398(18) -0.0075(13) 0.0092(16) -0.0032(15) C19' 0.0335(17) 0.0247(16) 0.0313(16) -0.0087(13) 0.0062(13) 0.0020(14) C20' 0.0229(16) 0.041(2) 0.0403(18) -0.0059(15) -0.0038(13) -0.0020(14) C21' 0.0298(18) 0.052(2) 0.050(2) -0.0102(18) 0.0049(16) -0.0105(17) C22' 0.0270(17) 0.0319(18) 0.047(2) -0.0041(15) 0.0097(14) -0.0083(14) C23' 0.0249(15) 0.0254(16) 0.0338(16) -0.0013(12) 0.0112(12) 0.0050(12) C24' 0.0375(18) 0.0237(16) 0.0307(15) -0.0054(12) 0.0111(13) -0.0005(13) C25' 0.0283(16) 0.0223(15) 0.0267(15) -0.0033(11) 0.0040(12) -0.0036(12) C26' 0.0365(18) 0.0362(19) 0.0245(14) 0.0020(13) 0.0099(13) 0.0066(14) C27' 0.0371(19) 0.041(2) 0.0368(17) -0.0012(14) 0.0201(15) 0.0065(15) C28' 0.0266(16) 0.0263(16) 0.0417(17) -0.0045(13) 0.0154(13) 0.0009(13) C1S 0.063(5) 0.051(5) 0.033(4) 0.004(3) -0.003(3) -0.002(4) B1 0.0218(16) 0.0225(17) 0.0258(15) 0.0024(13) 0.0015(12) -0.0013(14) B1' 0.0186(15) 0.0194(16) 0.0249(15) 0.0001(13) 0.0028(12) 0.0010(13) _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 N3 2.071(3) . ? Rh1 C4 2.105(3) . ? Rh1 C1 2.126(3) . ? Rh1 N1 2.132(3) . ? Rh1 C3 2.133(3) . ? Rh1 C2 2.153(4) . ? Rh2 N7 2.070(3) . ? Rh2 C7 2.111(3) . ? Rh2 C8 2.116(3) . ? Rh2 N5 2.121(2) . ? Rh2 C5 2.141(3) . ? Rh2 C6 2.153(3) . ? Rh1' N1' 2.077(2) . ? Rh1' C4' 2.118(3) . ? Rh1' C2' 2.132(3) . ? Rh1' N3' 2.133(3) . ? Rh1' C1' 2.141(3) . ? Rh1' C3' 2.146(3) . ? Rh2' N5' 2.080(2) . ? Rh2' C5' 2.115(3) . ? Rh2' N7' 2.118(2) . ? Rh2' C6' 2.132(3) . ? Rh2' C8' 2.132(3) . ? Rh2' C7' 2.136(3) . ? Cl1 C1S 1.770(9) . ? Cl2 C1S 1.756(9) . ? P1 F1 1.579(2) 2_756 ? P1 F1 1.579(2) . ? P1 F2 1.588(2) . ? P1 F2 1.588(2) 2_756 ? P1 F3 1.602(2) . ? P1 F3 1.602(2) 2_756 ? P2 F9 1.492(3) . ? P2 F5 1.516(5) . ? P2 F6 1.543(3) . ? P2 F4 1.544(4) . ? P2 F8 1.571(3) . ? P2 F7 1.572(3) . ? P1' F1' 1.544(3) 2_657 ? P1' F1' 1.544(3) . ? P1' F2' 1.546(3) . ? P1' F2' 1.546(3) 2_657 ? P1' F3' 1.588(3) . ? P1' F3' 1.588(3) 2_657 ? N1 C17 1.323(4) . ? N1 N2 1.378(4) . ? N2 C19 1.358(4) . ? N2 B1 1.525(4) . ? N3 C20 1.339(4) . ? N3 N4 1.363(3) . ? N4 C22 1.347(4) . ? N4 B1 1.549(4) . ? N5 C23 1.330(4) . ? N5 N6 1.382(4) . ? N6 C25 1.343(4) . ? N6 B1 1.535(4) . ? N7 C26 1.333(4) . ? N7 N8 1.374(3) . ? N8 C28 1.353(4) . ? N8 B1 1.553(4) . ? N1' C17' 1.317(4) . ? N1' N2' 1.357(3) . ? N2' C19' 1.352(4) . ? N2' B1' 1.537(4) . ? N3' C20' 1.336(4) . ? N3' N4' 1.376(3) . ? N4' C22' 1.347(4) . ? N4' B1' 1.537(4) . ? N5' C23' 1.328(4) . ? N5' N6' 1.362(3) . ? N6' C25' 1.357(4) . ? N6' B1' 1.552(4) . ? N7' C26' 1.334(4) . ? N7' N8' 1.384(3) . ? N8' C28' 1.349(4) . ? N8' B1' 1.544(4) . ? C1 C2 1.403(6) . ? C1 C12 1.496(5) . ? C2 C10 1.552(6) . ? C3 C4 1.393(5) . ? C3 C11 1.515(5) . ? C4 C9 1.470(5) . ? C5 C6 1.384(5) . ? C5 C16 1.503(5) . ? C6 C14 1.526(5) . ? C7 C8 1.388(5) . ? C7 C15 1.493(5) . ? C8 C13 1.502(5) . ? C9 C10 1.497(7) . ? C11 C12 1.490(6) . ? C13 C14 1.485(6) . ? C15 C16 1.488(6) . ? C17 C18 1.378(5) . ? C18 C19 1.368(5) . ? C20 C21 1.396(5) . ? C21 C22 1.371(4) . ? C23 C24 1.390(4) . ? C24 C25 1.372(5) . ? C26 C27 1.397(5) . ? C27 C28 1.367(5) . ? C1' C2' 1.399(5) . ? C1' C9' 1.511(5) . ? C2' C12' 1.507(5) . ? C3' C4' 1.391(5) . ? C3' C11' 1.520(4) . ? C4' C10' 1.504(5) . ? C5' C6' 1.391(6) . ? C5' C13' 1.504(6) . ? C6' C15' 1.509(5) . ? C7' C8' 1.391(5) . ? C7' C14' 1.505(5) . ? C8' C16' 1.504(5) . ? C9' C10' 1.537(5) . ? C11' C12' 1.523(5) . ? C13' C14' 1.529(6) . ? C15' C16' 1.531(5) . ? C17' C18' 1.397(4) . ? C18' C19' 1.363(5) . ? C20' C21' 1.404(5) . ? C21' C22' 1.367(5) . ? C23' C24' 1.393(4) . ? C24' C25' 1.365(4) . ? C26' C27' 1.394(5) . ? C27' C28' 1.358(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 N3 Rh1 C4 92.52(13) . . ? N3 Rh1 C1 157.47(13) . . ? C4 Rh1 C1 96.22(15) . . ? N3 Rh1 N1 86.17(10) . . ? C4 Rh1 N1 153.99(12) . . ? C1 Rh1 N1 94.73(13) . . ? N3 Rh1 C3 92.80(12) . . ? C4 Rh1 C3 38.38(12) . . ? C1 Rh1 C3 81.52(14) . . ? N1 Rh1 C3 167.58(12) . . ? N3 Rh1 C2 164.26(13) . . ? C4 Rh1 C2 81.28(16) . . ? C1 Rh1 C2 38.27(16) . . ? N1 Rh1 C2 93.09(14) . . ? C3 Rh1 C2 91.22(14) . . ? N7 Rh2 C7 92.45(12) . . ? N7 Rh2 C8 92.71(12) . . ? C7 Rh2 C8 38.34(14) . . ? N7 Rh2 N5 86.19(10) . . ? C7 Rh2 N5 155.03(12) . . ? C8 Rh2 N5 166.57(12) . . ? N7 Rh2 C5 163.01(12) . . ? C7 Rh2 C5 81.05(14) . . ? C8 Rh2 C5 91.82(13) . . ? N5 Rh2 C5 93.09(12) . . ? N7 Rh2 C6 159.39(12) . . ? C7 Rh2 C6 94.96(14) . . ? C8 Rh2 C6 81.44(13) . . ? N5 Rh2 C6 94.93(11) . . ? C5 Rh2 C6 37.59(13) . . ? N1' Rh1' C4' 92.18(11) . . ? N1' Rh1' C2' 155.92(12) . . ? C4' Rh1' C2' 97.52(13) . . ? N1' Rh1' N3' 86.12(10) . . ? C4' Rh1' N3' 154.39(12) . . ? C2' Rh1' N3' 94.21(12) . . ? N1' Rh1' C1' 165.85(12) . . ? C4' Rh1' C1' 81.91(13) . . ? C2' Rh1' C1' 38.23(13) . . ? N3' Rh1' C1' 93.66(12) . . ? N1' Rh1' C3' 93.19(11) . . ? C4' Rh1' C3' 38.08(13) . . ? C2' Rh1' C3' 81.35(13) . . ? N3' Rh1' C3' 167.49(12) . . ? C1' Rh1' C3' 90.05(13) . . ? N5' Rh2' C5' 90.21(11) . . ? N5' Rh2' N7' 86.78(9) . . ? C5' Rh2' N7' 157.50(13) . . ? N5' Rh2' C6' 94.16(11) . . ? C5' Rh2' C6' 38.24(15) . . ? N7' Rh2' C6' 164.24(14) . . ? N5' Rh2' C8' 160.32(13) . . ? C5' Rh2' C8' 97.34(13) . . ? N7' Rh2' C8' 92.82(11) . . ? C6' Rh2' C8' 81.02(13) . . ? N5' Rh2' C7' 161.61(13) . . ? C5' Rh2' C7' 81.49(14) . . ? N7' Rh2' C7' 94.61(12) . . ? C6' Rh2' C7' 89.44(14) . . ? C8' Rh2' C7' 38.05(15) . . ? F1 P1 F1 178.9(2) 2_756 . ? F1 P1 F2 89.85(14) 2_756 . ? F1 P1 F2 90.91(13) . . ? F1 P1 F2 90.91(13) 2_756 2_756 ? F1 P1 F2 89.85(14) . 2_756 ? F2 P1 F2 91.3(2) . 2_756 ? F1 P1 F3 87.84(13) 2_756 . ? F1 P1 F3 91.39(14) . . ? F2 P1 F3 90.00(12) . . ? F2 P1 F3 178.16(16) 2_756 . ? F1 P1 F3 91.39(14) 2_756 2_756 ? F1 P1 F3 87.84(13) . 2_756 ? F2 P1 F3 178.16(16) . 2_756 ? F2 P1 F3 90.00(12) 2_756 2_756 ? F3 P1 F3 88.69(18) . 2_756 ? F9 P2 F5 85.4(5) . . ? F9 P2 F6 90.8(2) . . ? F5 P2 F6 91.1(3) . . ? F9 P2 F4 101.5(4) . . ? F5 P2 F4 173.0(4) . . ? F6 P2 F4 87.7(2) . . ? F9 P2 F8 172.7(4) . . ? F5 P2 F8 88.4(4) . . ? F6 P2 F8 93.1(2) . . ? F4 P2 F8 84.8(3) . . ? F9 P2 F7 88.2(2) . . ? F5 P2 F7 93.3(3) . . ? F6 P2 F7 175.4(3) . . ? F4 P2 F7 88.1(2) . . ? F8 P2 F7 88.28(19) . . ? F1' P1' F1' 178.1(3) 2_657 . ? F1' P1' F2' 89.6(2) 2_657 . ? F1' P1' F2' 91.8(3) . . ? F1' P1' F2' 91.8(3) 2_657 2_657 ? F1' P1' F2' 89.6(2) . 2_657 ? F2' P1' F2' 88.7(3) . 2_657 ? F1' P1' F3' 88.8(3) 2_657 . ? F1' P1' F3' 89.8(2) . . ? F2' P1' F3' 93.46(17) . . ? F2' P1' F3' 177.81(18) 2_657 . ? F1' P1' F3' 89.8(2) 2_657 2_657 ? F1' P1' F3' 88.8(3) . 2_657 ? F2' P1' F3' 177.81(18) . 2_657 ? F2' P1' F3' 93.46(17) 2_657 2_657 ? F3' P1' F3' 84.4(2) . 2_657 ? C17 N1 N2 106.0(3) . . ? C17 N1 Rh1 130.7(2) . . ? N2 N1 Rh1 121.67(19) . . ? C19 N2 N1 108.9(3) . . ? C19 N2 B1 131.5(3) . . ? N1 N2 B1 119.3(2) . . ? C20 N3 N4 106.3(3) . . ? C20 N3 Rh1 131.0(2) . . ? N4 N3 Rh1 120.99(18) . . ? C22 N4 N3 109.6(2) . . ? C22 N4 B1 128.6(3) . . ? N3 N4 B1 121.8(2) . . ? C23 N5 N6 106.3(2) . . ? C23 N5 Rh2 130.1(2) . . ? N6 N5 Rh2 122.03(18) . . ? C25 N6 N5 108.7(2) . . ? C25 N6 B1 131.3(3) . . ? N5 N6 B1 119.4(2) . . ? C26 N7 N8 106.0(2) . . ? C26 N7 Rh2 131.6(2) . . ? N8 N7 Rh2 121.08(18) . . ? C28 N8 N7 109.3(2) . . ? C28 N8 B1 128.8(3) . . ? N7 N8 B1 121.7(2) . . ? C17' N1' N2' 107.6(2) . . ? C17' N1' Rh1' 128.5(2) . . ? N2' N1' Rh1' 119.92(17) . . ? C19' N2' N1' 108.9(2) . . ? C19' N2' B1' 127.3(2) . . ? N1' N2' B1' 123.2(2) . . ? C20' N3' N4' 105.8(3) . . ? C20' N3' Rh1' 130.1(2) . . ? N4' N3' Rh1' 122.77(17) . . ? C22' N4' N3' 109.4(2) . . ? C22' N4' B1' 132.3(3) . . ? N3' N4' B1' 118.1(2) . . ? C23' N5' N6' 107.1(2) . . ? C23' N5' Rh2' 131.9(2) . . ? N6' N5' Rh2' 120.42(18) . . ? C25' N6' N5' 108.7(2) . . ? C25' N6' B1' 129.3(2) . . ? N5' N6' B1' 121.9(2) . . ? C26' N7' N8' 106.2(2) . . ? C26' N7' Rh2' 130.9(2) . . ? N8' N7' Rh2' 122.78(17) . . ? C28' N8' N7' 108.5(2) . . ? C28' N8' B1' 133.4(3) . . ? N7' N8' B1' 117.6(2) . . ? C2 C1 C12 123.4(4) . . ? C2 C1 Rh1 71.9(2) . . ? C12 C1 Rh1 111.7(3) . . ? C1 C2 C10 123.3(4) . . ? C1 C2 Rh1 69.8(2) . . ? C10 C2 Rh1 111.0(3) . . ? C4 C3 C11 122.3(3) . . ? C4 C3 Rh1 69.73(18) . . ? C11 C3 Rh1 112.9(2) . . ? C3 C4 C9 127.1(4) . . ? C3 C4 Rh1 71.89(19) . . ? C9 C4 Rh1 113.4(3) . . ? C6 C5 C16 123.2(3) . . ? C6 C5 Rh2 71.67(19) . . ? C16 C5 Rh2 113.0(3) . . ? C5 C6 C14 123.6(4) . . ? C5 C6 Rh2 70.7(2) . . ? C14 C6 Rh2 110.9(2) . . ? C8 C7 C15 125.6(4) . . ? C8 C7 Rh2 71.00(19) . . ? C15 C7 Rh2 112.4(2) . . ? C7 C8 C13 122.0(4) . . ? C7 C8 Rh2 70.65(18) . . ? C13 C8 Rh2 114.2(2) . . ? C4 C9 C10 113.6(4) . . ? C9 C10 C2 113.9(3) . . ? C12 C11 C3 114.0(3) . . ? C11 C12 C1 115.0(3) . . ? C14 C13 C8 114.9(3) . . ? C13 C14 C6 115.0(3) . . ? C16 C15 C7 115.0(3) . . ? C15 C16 C5 114.3(3) . . ? N1 C17 C18 111.5(3) . . ? C19 C18 C17 105.3(3) . . ? N2 C19 C18 108.2(3) . . ? N3 C20 C21 110.5(3) . . ? C22 C21 C20 104.7(3) . . ? N4 C22 C21 108.9(3) . . ? N5 C23 C24 111.0(3) . . ? C25 C24 C23 104.6(3) . . ? N6 C25 C24 109.4(3) . . ? N7 C26 C27 111.0(3) . . ? C28 C27 C26 104.8(3) . . ? N8 C28 C27 108.9(3) . . ? C2' C1' C9' 123.9(3) . . ? C2' C1' Rh1' 70.56(18) . . ? C9' C1' Rh1' 113.0(2) . . ? C1' C2' C12' 125.9(3) . . ? C1' C2' Rh1' 71.21(17) . . ? C12' C2' Rh1' 110.6(2) . . ? C4' C3' C11' 123.0(3) . . ? C4' C3' Rh1' 69.84(18) . . ? C11' C3' Rh1' 113.0(2) . . ? C3' C4' C10' 125.8(3) . . ? C3' C4' Rh1' 72.08(18) . . ? C10' C4' Rh1' 110.3(2) . . ? C6' C5' C13' 126.4(3) . . ? C6' C5' Rh2' 71.5(2) . . ? C13' C5' Rh2' 110.6(2) . . ? C5' C6' C15' 123.0(4) . . ? C5' C6' Rh2' 70.24(19) . . ? C15' C6' Rh2' 114.4(2) . . ? C8' C7' C14' 124.7(3) . . ? C8' C7' Rh2' 70.79(19) . . ? C14' C7' Rh2' 112.9(2) . . ? C7' C8' C16' 125.2(3) . . ? C7' C8' Rh2' 71.16(18) . . ? C16' C8' Rh2' 110.5(2) . . ? C1' C9' C10' 112.2(3) . . ? C4' C10' C9' 113.3(3) . . ? C3' C11' C12' 112.2(3) . . ? C2' C12' C11' 112.9(3) . . ? C5' C13' C14' 112.2(3) . . ? C7' C14' C13' 112.8(3) . . ? C6' C15' C16' 111.0(3) . . ? C8' C16' C15' 113.1(3) . . ? N1' C17' C18' 109.9(3) . . ? C19' C18' C17' 105.3(3) . . ? N2' C19' C18' 108.4(3) . . ? N3' C20' C21' 111.0(3) . . ? C22' C21' C20' 104.3(3) . . ? N4' C22' C21' 109.4(3) . . ? N5' C23' C24' 110.5(3) . . ? C25' C24' C23' 104.8(3) . . ? N6' C25' C24' 108.9(3) . . ? N7' C26' C27' 110.6(3) . . ? C28' C27' C26' 105.1(3) . . ? N8' C28' C27' 109.6(3) . . ? Cl2 C1S Cl1 112.2(5) . . ? N2 B1 N6 113.7(2) . . ? N2 B1 N4 110.2(2) . . ? N6 B1 N4 106.2(2) . . ? N2 B1 N8 106.1(2) . . ? N6 B1 N8 109.5(2) . . ? N4 B1 N8 111.3(2) . . ? N4' B1' N2' 109.5(2) . . ? N4' B1' N8' 114.3(2) . . ? N2' B1' N8' 105.4(2) . . ? N4' B1' N6' 105.5(2) . . ? N2' B1' N6' 113.1(2) . . ? N8' B1' N6' 109.3(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.622 _refine_diff_density_min -0.572 _refine_diff_density_rms 0.073 data_2+ _database_code_depnum_ccdc_archive 'CCDC 768029' #TrackingRef '- Hallett_Dalton_Cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H28 B N8 Rh2, F6 P, C H2 Cl2' _chemical_formula_sum 'C27 H30 B Cl2 F6 N8 P Rh2' _chemical_formula_weight 899.09 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' B B 0.0013 0.0007 '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' Cl Cl 0.1484 0.1585 '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 14.410(3) _cell_length_b 11.036(2) _cell_length_c 21.209(5) _cell_angle_alpha 90.00 _cell_angle_beta 108.512(4) _cell_angle_gamma 90.00 _cell_volume 3198.3(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 102 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.867 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 1.319 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.829881 _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_% ? _diffrn_reflns_number 16779 _diffrn_reflns_av_R_equivalents 0.1010 _diffrn_reflns_av_sigmaI/netI 0.1179 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5632 _reflns_number_gt 3328 _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^)+(0.0493P)^2^+19.7889P] 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 5632 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1288 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1530 _refine_ls_wR_factor_gt 0.1246 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 0.73940(6) 0.52541(7) 0.15410(4) 0.0253(2) Uani 1 1 d . . . Rh2 Rh 0.35234(6) 0.37699(7) 0.22105(4) 0.0240(2) Uani 1 1 d . . . Cl98 Cl -0.0015(3) 0.2171(5) 0.08578(18) 0.0960(15) Uani 1 1 d . . . Cl99 Cl -0.0056(3) 0.3480(4) -0.03206(19) 0.0852(13) Uani 1 1 d . . . P1 P 0.2647(2) 0.0180(3) 0.02423(14) 0.0327(7) Uani 1 1 d . . . F1 F 0.3570(7) 0.0025(12) 0.0847(5) 0.142(5) Uani 1 1 d . . . F2 F 0.1720(7) 0.0325(11) -0.0349(4) 0.143(5) Uani 1 1 d . . . F3 F 0.2535(8) -0.1217(8) 0.0260(7) 0.141(5) Uani 1 1 d . . . F4 F 0.3287(8) 0.0020(8) -0.0220(5) 0.120(4) Uani 1 1 d . . . F5 F 0.2776(7) 0.1561(7) 0.0259(6) 0.124(4) Uani 1 1 d . . . F6 F 0.1962(7) 0.0329(8) 0.0691(4) 0.095(3) Uani 1 1 d . . . N1 N 0.6290(6) 0.6496(7) 0.1120(4) 0.0247(19) Uani 1 1 d . . . N2 N 0.5331(5) 0.6361(7) 0.1129(4) 0.0253(19) Uani 1 1 d . . . N3 N 0.6370(6) 0.3896(7) 0.1248(4) 0.0254(19) Uani 1 1 d . . . N4 N 0.5393(5) 0.4056(7) 0.1124(4) 0.0232(18) Uani 1 1 d . . . N5 N 0.3234(6) 0.4432(7) 0.1253(4) 0.030(2) Uani 1 1 d . . . N6 N 0.3848(5) 0.5119(7) 0.1016(4) 0.0246(18) Uani 1 1 d . . . N7 N 0.4903(5) 0.4511(7) 0.2498(4) 0.0216(18) Uani 1 1 d . . . N8 N 0.5265(5) 0.5264(7) 0.2113(4) 0.0237(18) Uani 1 1 d . . . C1 C 0.8397(7) 0.6486(9) 0.2191(5) 0.032(2) Uani 1 1 d . . . H1A H 0.8200 0.7297 0.2316 0.038 Uiso 1 1 calc R . . C2 C 0.8692(7) 0.6292(10) 0.1631(5) 0.039(3) Uani 1 1 d . . . H2A H 0.8726 0.6948 0.1314 0.046 Uiso 1 1 calc R . . C3 C 0.8386(7) 0.4364(9) 0.2351(5) 0.035(3) Uani 1 1 d . . . H3A H 0.8191 0.3689 0.2597 0.042 Uiso 1 1 calc R . . C4 C 0.8680(7) 0.4179(11) 0.1804(6) 0.044(3) Uani 1 1 d . . . H4A H 0.8719 0.3362 0.1610 0.052 Uiso 1 1 calc R . . C5 C 0.2046(7) 0.3462(9) 0.2160(5) 0.032(3) Uani 1 1 d . . . H5A H 0.1473 0.3862 0.1830 0.038 Uiso 1 1 calc R . . C6 C 0.2452(7) 0.2372(9) 0.2043(5) 0.034(3) Uani 1 1 d . . . H6A H 0.2204 0.1915 0.1615 0.040 Uiso 1 1 calc R . . C7 C 0.3344(7) 0.3693(9) 0.3156(5) 0.031(2) Uani 1 1 d . . . H7A H 0.3685 0.4252 0.3528 0.038 Uiso 1 1 calc R . . C8 C 0.3760(8) 0.2603(8) 0.3023(5) 0.030(2) Uani 1 1 d . . . H8A H 0.4423 0.2308 0.3294 0.036 Uiso 1 1 calc R . . C9 C 0.9404(7) 0.5235(10) 0.1813(6) 0.041(3) Uani 1 1 d . . . H9A H 0.9846 0.5125 0.1538 0.049 Uiso 1 1 calc R . . C10 C 0.9897(7) 0.5429(11) 0.2560(5) 0.044(3) Uani 1 1 d . . . H10A H 1.0290 0.6182 0.2664 0.053 Uiso 1 1 calc R . . H10B H 1.0293 0.4725 0.2783 0.053 Uiso 1 1 calc R . . C11 C 0.8914(7) 0.5531(10) 0.2697(5) 0.039(3) Uani 1 1 d . . . H11A H 0.8940 0.5669 0.3169 0.046 Uiso 1 1 calc R . . C12 C 0.2244(7) 0.3504(9) 0.2915(5) 0.032(3) Uani 1 1 d . . . H12A H 0.1847 0.4093 0.3079 0.038 Uiso 1 1 calc R . . C13 C 0.2161(8) 0.2159(10) 0.3087(6) 0.044(3) Uani 1 1 d . . . H13A H 0.1494 0.1826 0.2889 0.053 Uiso 1 1 calc R . . H13B H 0.2408 0.1993 0.3570 0.053 Uiso 1 1 calc R . . C14 C 0.2886(8) 0.1758(10) 0.2714(6) 0.046(3) Uani 1 1 d . . . H14A H 0.3029 0.0872 0.2710 0.055 Uiso 1 1 calc R . . C15 C 0.6380(8) 0.7680(9) 0.1001(5) 0.030(2) Uani 1 1 d . . . H15A H 0.6963 0.8039 0.0969 0.036 Uiso 1 1 calc R . . C16 C 0.5520(8) 0.8314(9) 0.0928(5) 0.035(3) Uani 1 1 d . . . H16A H 0.5396 0.9150 0.0832 0.042 Uiso 1 1 calc R . . C17 C 0.4892(7) 0.7463(9) 0.1028(5) 0.030(3) Uani 1 1 d . . . H17A H 0.4243 0.7620 0.1026 0.036 Uiso 1 1 calc R . . C18 C 0.6488(8) 0.2795(9) 0.1020(5) 0.035(3) Uani 1 1 d . . . H18A H 0.7099 0.2444 0.1043 0.042 Uiso 1 1 calc R . . C19 C 0.5579(8) 0.2239(10) 0.0746(5) 0.038(3) Uani 1 1 d . . . H19A H 0.5449 0.1459 0.0549 0.045 Uiso 1 1 calc R . . C20 C 0.4929(8) 0.3053(9) 0.0822(5) 0.029(2) Uani 1 1 d . . . H20A H 0.4241 0.2936 0.0682 0.034 Uiso 1 1 calc R . . C21 C 0.2398(8) 0.4340(11) 0.0757(5) 0.041(3) Uani 1 1 d . . . H21A H 0.1836 0.3918 0.0783 0.050 Uiso 1 1 calc R . . C22 C 0.2456(7) 0.4940(10) 0.0200(5) 0.039(3) Uani 1 1 d . . . H22A H 0.1956 0.5015 -0.0217 0.047 Uiso 1 1 calc R . . C23 C 0.3385(7) 0.5407(9) 0.0371(5) 0.031(2) Uani 1 1 d . . . H23A H 0.3656 0.5852 0.0088 0.037 Uiso 1 1 calc R . . C24 C 0.5486(7) 0.4652(10) 0.3121(5) 0.034(3) Uani 1 1 d . . . H24A H 0.5399 0.4247 0.3493 0.041 Uiso 1 1 calc R . . C25 C 0.6234(8) 0.5461(10) 0.3159(5) 0.038(3) Uani 1 1 d . . . H25A H 0.6750 0.5703 0.3543 0.045 Uiso 1 1 calc R . . C26 C 0.6060(7) 0.5833(9) 0.2520(5) 0.029(2) Uani 1 1 d . . . H26A H 0.6443 0.6410 0.2380 0.035 Uiso 1 1 calc R . . C1S C -0.0176(11) 0.2056(12) 0.0005(6) 0.065(4) Uani 1 1 d . . . H99A H 0.0318 0.1496 -0.0065 0.078 Uiso 1 1 calc R . . H99B H -0.0833 0.1723 -0.0229 0.078 Uiso 1 1 calc R . . B1 B 0.4956(8) 0.5185(10) 0.1356(5) 0.022(2) 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 0.0219(4) 0.0246(4) 0.0277(4) 0.0021(4) 0.0057(3) 0.0000(4) Rh2 0.0235(4) 0.0231(4) 0.0259(4) -0.0012(4) 0.0087(3) -0.0030(4) Cl98 0.085(3) 0.153(4) 0.050(2) -0.018(2) 0.023(2) -0.043(3) Cl99 0.080(3) 0.091(3) 0.069(3) 0.005(2) 0.001(2) -0.036(2) P1 0.0350(16) 0.0312(16) 0.0327(15) 0.0045(13) 0.0119(13) -0.0009(13) F1 0.076(7) 0.227(13) 0.093(7) -0.001(8) -0.015(6) 0.053(8) F2 0.106(8) 0.223(13) 0.062(6) -0.042(7) -0.027(5) 0.079(8) F3 0.124(8) 0.049(6) 0.294(15) 0.005(7) 0.130(10) 0.001(6) F4 0.170(10) 0.087(7) 0.159(9) 0.048(6) 0.134(8) 0.066(6) F5 0.141(9) 0.040(5) 0.235(13) -0.032(6) 0.124(9) -0.031(5) F6 0.113(7) 0.102(7) 0.104(7) 0.042(5) 0.085(6) 0.034(6) N1 0.026(5) 0.017(5) 0.032(5) 0.007(4) 0.010(4) 0.001(4) N2 0.021(4) 0.032(5) 0.021(4) 0.007(4) 0.005(3) 0.009(4) N3 0.031(5) 0.018(5) 0.027(5) -0.002(4) 0.010(4) 0.001(4) N4 0.020(4) 0.027(5) 0.020(4) 0.002(3) 0.002(3) -0.002(4) N5 0.031(5) 0.029(5) 0.027(5) 0.001(4) 0.006(4) -0.010(4) N6 0.020(4) 0.033(5) 0.024(4) -0.001(4) 0.010(3) -0.006(4) N7 0.019(4) 0.023(5) 0.024(4) 0.000(3) 0.008(3) 0.001(3) N8 0.029(5) 0.023(4) 0.020(4) -0.002(4) 0.008(3) -0.006(4) C1 0.022(6) 0.035(6) 0.036(6) -0.013(5) 0.008(5) -0.003(5) C2 0.035(6) 0.035(7) 0.045(7) 0.003(5) 0.011(5) -0.004(5) C3 0.033(6) 0.023(6) 0.040(7) 0.009(5) 0.000(5) 0.002(5) C4 0.025(6) 0.042(7) 0.061(8) 0.009(6) 0.009(6) 0.005(5) C5 0.018(5) 0.025(6) 0.052(7) 0.000(5) 0.011(5) -0.006(4) C6 0.029(6) 0.036(7) 0.041(7) -0.005(5) 0.018(5) -0.009(5) C7 0.033(6) 0.031(6) 0.034(6) 0.004(5) 0.018(5) 0.003(5) C8 0.041(6) 0.020(6) 0.035(6) 0.004(5) 0.020(5) 0.001(5) C9 0.023(6) 0.041(7) 0.063(8) 0.004(6) 0.019(5) -0.005(5) C10 0.021(6) 0.050(8) 0.054(8) 0.018(6) 0.001(5) -0.001(5) C11 0.024(6) 0.055(8) 0.032(6) 0.011(5) 0.001(5) 0.003(5) C12 0.021(6) 0.033(6) 0.047(7) 0.001(5) 0.018(5) 0.001(5) C13 0.042(7) 0.039(7) 0.058(8) 0.008(6) 0.026(6) -0.011(6) C14 0.054(8) 0.032(7) 0.057(8) -0.003(6) 0.027(6) -0.001(6) C15 0.037(6) 0.026(6) 0.025(6) -0.001(4) 0.007(5) -0.012(5) C16 0.046(7) 0.016(5) 0.033(6) 0.008(5) 0.000(5) -0.001(5) C17 0.031(6) 0.028(6) 0.027(6) -0.003(5) 0.003(5) 0.006(5) C18 0.047(7) 0.026(6) 0.025(6) 0.000(5) 0.003(5) -0.001(5) C19 0.047(7) 0.024(6) 0.035(6) -0.004(5) 0.005(5) 0.006(5) C20 0.035(6) 0.024(6) 0.024(5) 0.000(4) 0.004(5) -0.012(5) C21 0.026(6) 0.067(8) 0.027(6) -0.005(6) 0.003(5) -0.009(6) C22 0.026(6) 0.053(8) 0.029(6) -0.002(5) -0.004(5) -0.006(5) C23 0.034(6) 0.030(6) 0.028(6) -0.001(5) 0.008(5) 0.000(5) C24 0.031(6) 0.041(7) 0.025(6) 0.004(5) 0.003(5) -0.002(5) C25 0.032(6) 0.051(8) 0.023(6) -0.002(5) 0.000(5) -0.010(6) C26 0.029(6) 0.038(6) 0.023(5) 0.002(5) 0.014(5) -0.009(5) C1S 0.088(11) 0.050(9) 0.054(8) -0.016(7) 0.018(8) -0.025(8) B1 0.025(6) 0.022(6) 0.019(5) -0.001(5) 0.007(5) 0.003(5) _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 N3 2.056(8) . ? Rh1 N1 2.075(7) . ? Rh1 C3 2.097(10) . ? Rh1 C4 2.121(10) . ? Rh1 C1 2.138(9) . ? Rh1 C2 2.150(10) . ? Rh2 N7 2.055(7) . ? Rh2 N5 2.073(8) . ? Rh2 C8 2.090(9) . ? Rh2 C7 2.103(10) . ? Rh2 C5 2.124(9) . ? Rh2 C6 2.131(10) . ? Cl98 C1S 1.753(13) . ? Cl99 C1S 1.747(13) . ? P1 F2 1.522(8) . ? P1 F5 1.535(8) . ? P1 F1 1.536(9) . ? P1 F3 1.552(9) . ? P1 F4 1.554(8) . ? P1 F6 1.582(8) . ? N1 C15 1.345(11) . ? N1 N2 1.395(10) . ? N2 C17 1.356(11) . ? N2 B1 1.541(13) . ? N3 C18 1.338(12) . ? N3 N4 1.359(10) . ? N4 C20 1.345(11) . ? N4 B1 1.546(13) . ? N5 C21 1.328(12) . ? N5 N6 1.376(10) . ? N6 C23 1.356(11) . ? N6 B1 1.531(13) . ? N7 C24 1.330(11) . ? N7 N8 1.379(10) . ? N8 C26 1.350(11) . ? N8 B1 1.526(12) . ? C1 C2 1.399(14) . ? C1 C11 1.520(14) . ? C2 C9 1.520(14) . ? C3 C4 1.371(15) . ? C3 C11 1.557(14) . ? C4 C9 1.560(14) . ? C5 C6 1.393(13) . ? C5 C12 1.535(14) . ? C6 C14 1.520(15) . ? C7 C8 1.412(13) . ? C7 C12 1.517(13) . ? C8 C14 1.536(14) . ? C9 C10 1.532(15) . ? C10 C11 1.538(15) . ? C12 C13 1.542(14) . ? C13 C14 1.561(15) . ? C15 C16 1.389(14) . ? C16 C17 1.366(14) . ? C18 C19 1.395(14) . ? C19 C20 1.343(14) . ? C21 C22 1.381(14) . ? C22 C23 1.371(13) . ? C24 C25 1.382(14) . ? C25 C26 1.362(13) . ? 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 Rh1 N1 88.4(3) . . ? N3 Rh1 C3 98.2(3) . . ? N1 Rh1 C3 153.1(4) . . ? N3 Rh1 C4 98.9(4) . . ? N1 Rh1 C4 165.8(4) . . ? C3 Rh1 C4 37.9(4) . . ? N3 Rh1 C1 158.7(3) . . ? N1 Rh1 C1 97.3(3) . . ? C3 Rh1 C1 67.9(4) . . ? C4 Rh1 C1 80.3(4) . . ? N3 Rh1 C2 159.4(4) . . ? N1 Rh1 C2 102.3(4) . . ? C3 Rh1 C2 80.2(4) . . ? C4 Rh1 C2 67.1(4) . . ? C1 Rh1 C2 38.1(4) . . ? N7 Rh2 N5 91.5(3) . . ? N7 Rh2 C8 96.4(3) . . ? N5 Rh2 C8 162.6(3) . . ? N7 Rh2 C7 97.7(3) . . ? N5 Rh2 C7 154.3(4) . . ? C8 Rh2 C7 39.4(4) . . ? N7 Rh2 C5 159.7(3) . . ? N5 Rh2 C5 96.9(4) . . ? C8 Rh2 C5 80.9(4) . . ? C7 Rh2 C5 67.5(4) . . ? N7 Rh2 C6 156.8(3) . . ? N5 Rh2 C6 100.5(4) . . ? C8 Rh2 C6 67.1(4) . . ? C7 Rh2 C6 80.1(4) . . ? C5 Rh2 C6 38.2(4) . . ? F2 P1 F5 89.0(7) . . ? F2 P1 F1 178.9(7) . . ? F5 P1 F1 91.5(7) . . ? F2 P1 F3 93.1(7) . . ? F5 P1 F3 177.4(7) . . ? F1 P1 F3 86.4(7) . . ? F2 P1 F4 91.9(6) . . ? F5 P1 F4 92.0(5) . . ? F1 P1 F4 89.0(6) . . ? F3 P1 F4 89.4(5) . . ? F2 P1 F6 86.1(6) . . ? F5 P1 F6 88.7(5) . . ? F1 P1 F6 92.9(6) . . ? F3 P1 F6 90.0(5) . . ? F4 P1 F6 177.9(6) . . ? C15 N1 N2 105.2(8) . . ? C15 N1 Rh1 128.0(7) . . ? N2 N1 Rh1 123.5(5) . . ? C17 N2 N1 108.5(8) . . ? C17 N2 B1 127.7(8) . . ? N1 N2 B1 122.7(7) . . ? C18 N3 N4 106.9(8) . . ? C18 N3 Rh1 127.6(7) . . ? N4 N3 Rh1 124.3(6) . . ? C20 N4 N3 108.3(8) . . ? C20 N4 B1 128.6(8) . . ? N3 N4 B1 123.0(7) . . ? C21 N5 N6 106.3(8) . . ? C21 N5 Rh2 126.7(7) . . ? N6 N5 Rh2 126.8(6) . . ? C23 N6 N5 109.2(7) . . ? C23 N6 B1 124.8(8) . . ? N5 N6 B1 123.3(7) . . ? C24 N7 N8 106.2(7) . . ? C24 N7 Rh2 126.0(7) . . ? N8 N7 Rh2 125.2(5) . . ? C26 N8 N7 107.8(7) . . ? C26 N8 B1 127.1(8) . . ? N7 N8 B1 123.4(7) . . ? C2 C1 C11 106.3(9) . . ? C2 C1 Rh1 71.4(6) . . ? C11 C1 Rh1 95.4(6) . . ? C1 C2 C9 105.3(9) . . ? C1 C2 Rh1 70.5(6) . . ? C9 C2 Rh1 96.4(6) . . ? C4 C3 C11 106.6(9) . . ? C4 C3 Rh1 72.0(6) . . ? C11 C3 Rh1 95.9(6) . . ? C3 C4 C9 105.2(10) . . ? C3 C4 Rh1 70.1(6) . . ? C9 C4 Rh1 96.3(7) . . ? C6 C5 C12 105.2(9) . . ? C6 C5 Rh2 71.2(6) . . ? C12 C5 Rh2 95.2(6) . . ? C5 C6 C14 106.8(9) . . ? C5 C6 Rh2 70.6(6) . . ? C14 C6 Rh2 96.0(7) . . ? C8 C7 C12 106.3(9) . . ? C8 C7 Rh2 69.8(6) . . ? C12 C7 Rh2 96.7(6) . . ? C7 C8 C14 105.0(9) . . ? C7 C8 Rh2 70.8(6) . . ? C14 C8 Rh2 97.2(7) . . ? C2 C9 C10 102.1(9) . . ? C2 C9 C4 100.1(8) . . ? C10 C9 C4 101.9(9) . . ? C9 C10 C11 93.0(8) . . ? C1 C11 C10 101.1(9) . . ? C1 C11 C3 100.5(8) . . ? C10 C11 C3 101.1(9) . . ? C7 C12 C5 100.6(8) . . ? C7 C12 C13 101.8(8) . . ? C5 C12 C13 102.4(8) . . ? C12 C13 C14 92.2(8) . . ? C6 C14 C8 99.6(8) . . ? C6 C14 C13 101.9(9) . . ? C8 C14 C13 101.6(9) . . ? N1 C15 C16 111.9(9) . . ? C17 C16 C15 104.4(9) . . ? N2 C17 C16 110.0(9) . . ? N3 C18 C19 109.9(10) . . ? C20 C19 C18 104.7(9) . . ? C19 C20 N4 110.3(9) . . ? N5 C21 C22 110.7(10) . . ? C23 C22 C21 105.9(9) . . ? N6 C23 C22 107.8(9) . . ? N7 C24 C25 111.7(9) . . ? C26 C25 C24 104.1(9) . . ? N8 C26 C25 110.2(9) . . ? Cl99 C1S Cl98 110.2(7) . . ? N8 B1 N6 114.3(8) . . ? N8 B1 N2 105.5(8) . . ? N6 B1 N2 108.0(8) . . ? N8 B1 N4 111.7(8) . . ? N6 B1 N4 106.3(8) . . ? N2 B1 N4 111.1(8) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.984 _refine_diff_density_min -0.761 _refine_diff_density_rms 0.161 data_4+ _database_code_depnum_ccdc_archive 'CCDC 768030' #TrackingRef '- Hallett_Dalton_Cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H12 B N8 O4 Rh2, F6 P' _chemical_formula_sum 'C16 H12 B F6 N8 O4 P Rh2' _chemical_formula_weight 741.94 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' B B 0.0013 0.0007 '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' O O 0.0106 0.0060 '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 P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.3967(18) _cell_length_b 12.453(2) _cell_length_c 17.059(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.042(3) _cell_angle_gamma 90.00 _cell_volume 2358.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 208 _cell_measurement_theta_min 2.451 _cell_measurement_theta_max 23.258 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.089 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 1.558 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.668774 _exptl_absorpt_correction_T_max 0.840622 _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 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10391 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 23.27 _reflns_number_total 3382 _reflns_number_gt 2822 _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^)+(0.0250P)^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 3382 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0514 _refine_ls_wR_factor_gt 0.0499 _refine_ls_goodness_of_fit_ref 0.933 _refine_ls_restrained_S_all 0.933 _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 Rh1 Rh 0.15623(2) 1.04786(2) 0.045683(17) 0.01771(9) Uani 1 1 d . . . Rh2 Rh 0.44480(2) 1.45542(2) 0.133049(17) 0.01786(9) Uani 1 1 d . . . P1 P 0.13301(8) 0.68231(7) 0.19572(6) 0.0209(2) Uani 1 1 d . . . F1 F 0.02442(19) 0.76162(17) 0.16630(17) 0.0586(8) Uani 1 1 d . . . F2 F 0.15325(19) 0.72901(17) 0.28497(13) 0.0424(6) Uani 1 1 d . . . F3 F 0.04207(17) 0.59465(16) 0.21784(13) 0.0324(5) Uani 1 1 d . . . F4 F 0.22569(17) 0.76976(15) 0.17623(12) 0.0288(5) Uani 1 1 d . . . F5 F 0.24291(17) 0.60143(16) 0.22683(14) 0.0383(6) Uani 1 1 d . . . F6 F 0.1148(2) 0.63339(19) 0.10843(13) 0.0590(8) Uani 1 1 d . . . O1 O 0.2027(2) 0.8216(2) -0.00074(15) 0.0365(7) Uani 1 1 d . . . O2 O 0.1384(2) 0.97976(19) 0.21051(17) 0.0345(7) Uani 1 1 d . . . O3 O 0.4626(2) 1.6931(2) 0.15827(16) 0.0338(7) Uani 1 1 d . . . O4 O 0.5571(2) 1.43336(19) 0.30876(18) 0.0361(7) Uani 1 1 d . . . N2 N 0.2338(2) 1.2046(2) -0.07322(16) 0.0158(6) Uani 1 1 d . . . N1 N 0.1832(2) 1.1069(2) -0.06330(17) 0.0171(7) Uani 1 1 d . . . N5 N 0.3557(2) 1.4736(2) 0.01264(17) 0.0179(7) Uani 1 1 d . . . N6 N 0.2859(2) 1.3968(2) -0.03443(17) 0.0164(7) Uani 1 1 d . . . N4 N 0.1753(2) 1.2912(2) 0.04762(16) 0.0164(7) Uani 1 1 d . . . N3 N 0.1326(2) 1.2032(2) 0.08008(16) 0.0180(7) Uani 1 1 d . . . N8 N 0.3927(2) 1.2410(2) 0.04757(16) 0.0168(6) Uani 1 1 d . . . N7 N 0.4568(2) 1.2927(2) 0.11451(16) 0.0173(7) Uani 1 1 d . . . C1 C 0.1823(3) 0.9061(3) 0.0171(2) 0.0237(9) Uani 1 1 d . . . C2 C 0.1430(3) 1.0010(3) 0.1469(3) 0.0257(9) Uani 1 1 d . . . C3 C 0.4506(3) 1.6038(3) 0.1485(2) 0.0231(9) Uani 1 1 d . . . C4 C 0.5157(3) 1.4409(3) 0.2419(3) 0.0241(9) Uani 1 1 d . . . C5 C 0.2631(3) 1.2066(3) -0.1451(2) 0.0206(8) Uani 1 1 d . . . H5A H 0.3010 1.2648 -0.1656 0.025 Uiso 1 1 calc R . . C6 C 0.2299(3) 1.1114(3) -0.1842(2) 0.0206(8) Uani 1 1 d . . . H6A H 0.2391 1.0908 -0.2361 0.025 Uiso 1 1 calc R . . C7 C 0.1802(3) 1.0521(3) -0.1315(2) 0.0188(8) Uani 1 1 d . . . H7A H 0.1481 0.9819 -0.1420 0.023 Uiso 1 1 calc R . . C8 C 0.3326(3) 1.5661(3) -0.0281(2) 0.0217(9) Uani 1 1 d . . . H8A H 0.3694 1.6329 -0.0103 0.026 Uiso 1 1 calc R . . C9 C 0.2484(3) 1.5515(3) -0.0989(2) 0.0227(9) Uani 1 1 d . . . H9A H 0.2170 1.6040 -0.1385 0.027 Uiso 1 1 calc R . . C10 C 0.2197(3) 1.4450(3) -0.0999(2) 0.0203(8) Uani 1 1 d . . . H10A H 0.1617 1.4103 -0.1408 0.024 Uiso 1 1 calc R . . C11 C 0.1293(3) 1.3806(3) 0.0746(2) 0.0198(8) Uani 1 1 d . . . H11A H 0.1450 1.4523 0.0610 0.024 Uiso 1 1 calc R . . C12 C 0.0567(3) 1.3513(3) 0.1246(2) 0.0220(8) Uani 1 1 d . . . H12A H 0.0127 1.3971 0.1521 0.026 Uiso 1 1 calc R . . C13 C 0.0613(3) 1.2400(3) 0.1264(2) 0.0208(8) Uani 1 1 d . . . H13A H 0.0195 1.1960 0.1565 0.025 Uiso 1 1 calc R . . C14 C 0.4486(3) 1.1468(3) 0.0402(2) 0.0202(8) Uani 1 1 d . . . H14A H 0.4224 1.0951 -0.0010 0.024 Uiso 1 1 calc R . . C15 C 0.5487(3) 1.1375(3) 0.1014(2) 0.0213(8) Uani 1 1 d . . . H15A H 0.6048 1.0800 0.1109 0.026 Uiso 1 1 calc R . . C16 C 0.5508(3) 1.2300(3) 0.1465(2) 0.0201(8) Uani 1 1 d . . . H16A H 0.6105 1.2466 0.1935 0.024 Uiso 1 1 calc R . . B1 B 0.2711(3) 1.2832(3) -0.0025(2) 0.0171(9) 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 0.02169(16) 0.01413(16) 0.01734(18) 0.00013(12) 0.00448(13) 0.00054(12) Rh2 0.01809(16) 0.01539(16) 0.01951(19) -0.00252(12) 0.00300(12) -0.00035(12) P1 0.0224(5) 0.0166(5) 0.0218(6) -0.0018(4) 0.0012(4) 0.0005(4) F1 0.0257(13) 0.0289(14) 0.109(2) 0.0149(13) -0.0095(13) 0.0049(11) F2 0.0461(14) 0.0551(15) 0.0320(15) -0.0237(12) 0.0217(12) -0.0234(12) F3 0.0261(12) 0.0282(12) 0.0402(15) 0.0003(10) 0.0020(10) -0.0085(9) F4 0.0315(12) 0.0196(11) 0.0371(14) 0.0063(9) 0.0113(10) -0.0002(9) F5 0.0295(12) 0.0278(12) 0.0607(17) 0.0164(11) 0.0169(12) 0.0088(10) F6 0.113(2) 0.0420(15) 0.0194(14) -0.0072(11) 0.0084(14) -0.0218(15) O1 0.063(2) 0.0171(16) 0.0313(18) 0.0008(12) 0.0142(15) 0.0061(14) O2 0.0579(19) 0.0240(15) 0.0250(18) 0.0055(13) 0.0161(15) 0.0078(13) O3 0.0347(16) 0.0224(16) 0.0476(19) -0.0072(13) 0.0161(14) -0.0059(13) O4 0.0487(18) 0.0300(16) 0.0242(18) -0.0054(13) -0.0030(15) 0.0019(13) N2 0.0174(15) 0.0131(16) 0.0172(18) 0.0005(12) 0.0040(13) 0.0005(12) N1 0.0170(15) 0.0161(16) 0.0178(19) 0.0015(13) 0.0029(13) 0.0015(12) N5 0.0168(15) 0.0144(16) 0.0224(19) -0.0020(13) 0.0046(13) -0.0016(12) N6 0.0150(15) 0.0153(16) 0.0185(18) 0.0002(13) 0.0027(13) -0.0007(12) N4 0.0151(15) 0.0149(16) 0.0182(18) -0.0007(12) 0.0017(13) -0.0012(12) N3 0.0226(16) 0.0126(15) 0.0189(18) -0.0016(13) 0.0047(14) -0.0018(13) N8 0.0187(15) 0.0168(16) 0.0152(17) -0.0011(13) 0.0044(13) 0.0002(13) N7 0.0146(15) 0.0191(16) 0.0160(18) -0.0028(13) -0.0013(13) -0.0019(13) C1 0.029(2) 0.026(2) 0.014(2) 0.0040(17) 0.0009(17) -0.0012(18) C2 0.033(2) 0.0111(19) 0.034(3) -0.0006(18) 0.011(2) 0.0033(17) C3 0.0145(19) 0.028(2) 0.027(2) -0.0022(18) 0.0051(17) -0.0003(17) C4 0.023(2) 0.014(2) 0.034(3) -0.0079(18) 0.0062(19) -0.0004(16) C5 0.0226(19) 0.021(2) 0.020(2) 0.0027(16) 0.0082(17) 0.0034(16) C6 0.0206(19) 0.027(2) 0.013(2) -0.0042(16) 0.0018(16) 0.0039(16) C7 0.0205(19) 0.0149(19) 0.019(2) -0.0050(16) 0.0014(16) 0.0017(15) C8 0.025(2) 0.0112(19) 0.031(3) 0.0001(16) 0.0084(18) -0.0014(15) C9 0.023(2) 0.021(2) 0.024(2) 0.0086(17) 0.0053(18) 0.0043(17) C10 0.0179(18) 0.024(2) 0.017(2) 0.0026(16) 0.0009(16) 0.0020(16) C11 0.0218(19) 0.0097(19) 0.027(2) -0.0023(15) 0.0034(17) 0.0028(15) C12 0.0188(19) 0.023(2) 0.024(2) -0.0081(16) 0.0058(17) 0.0030(16) C13 0.0201(19) 0.025(2) 0.019(2) -0.0027(16) 0.0089(17) -0.0020(16) C14 0.0220(19) 0.0143(19) 0.024(2) -0.0047(16) 0.0044(17) 0.0040(16) C15 0.0154(18) 0.019(2) 0.029(2) 0.0007(17) 0.0051(17) 0.0050(15) C16 0.0162(18) 0.021(2) 0.021(2) 0.0059(16) 0.0009(16) 0.0028(16) B1 0.018(2) 0.018(2) 0.015(2) -0.0015(17) 0.0030(18) 0.0017(17) _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 C2 1.861(4) . ? Rh1 C1 1.874(4) . ? Rh1 N3 2.056(3) . ? Rh1 N1 2.086(3) . ? Rh2 C4 1.859(4) . ? Rh2 C3 1.865(4) . ? Rh2 N7 2.060(3) . ? Rh2 N5 2.088(3) . ? P1 F1 1.574(2) . ? P1 F6 1.579(2) . ? P1 F2 1.597(2) . ? P1 F5 1.601(2) . ? P1 F4 1.603(2) . ? P1 F3 1.608(2) . ? O1 C1 1.133(4) . ? O2 C2 1.130(4) . ? O3 C3 1.128(4) . ? O4 C4 1.136(4) . ? N2 C5 1.342(4) . ? N2 N1 1.373(3) . ? N2 B1 1.536(5) . ? N1 C7 1.342(4) . ? N5 C8 1.341(4) . ? N5 N6 1.380(4) . ? N6 C10 1.340(4) . ? N6 B1 1.539(5) . ? N4 C11 1.355(4) . ? N4 N3 1.367(3) . ? N4 B1 1.535(4) . ? N3 C13 1.335(4) . ? N8 C14 1.354(4) . ? N8 N7 1.370(4) . ? N8 B1 1.547(5) . ? N7 C16 1.339(4) . ? C5 C6 1.371(5) . ? C5 H5A 0.9500 . ? C6 C7 1.380(5) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.376(5) . ? C8 H8A 0.9500 . ? C9 C10 1.365(4) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 C12 1.364(5) . ? C11 H11A 0.9500 . ? C12 C13 1.387(5) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.366(5) . ? C14 H14A 0.9500 . ? C15 C16 1.382(5) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? 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 C2 Rh1 C1 89.82(15) . . ? C2 Rh1 N3 89.26(13) . . ? C1 Rh1 N3 178.12(13) . . ? C2 Rh1 N1 175.52(14) . . ? C1 Rh1 N1 92.06(13) . . ? N3 Rh1 N1 88.74(10) . . ? C4 Rh2 C3 87.79(15) . . ? C4 Rh2 N7 91.65(13) . . ? C3 Rh2 N7 173.93(12) . . ? C4 Rh2 N5 176.70(12) . . ? C3 Rh2 N5 91.46(13) . . ? N7 Rh2 N5 89.42(10) . . ? F1 P1 F6 90.83(15) . . ? F1 P1 F2 90.55(14) . . ? F6 P1 F2 178.51(15) . . ? F1 P1 F5 179.19(15) . . ? F6 P1 F5 89.81(14) . . ? F2 P1 F5 88.81(13) . . ? F1 P1 F4 90.86(12) . . ? F6 P1 F4 91.10(12) . . ? F2 P1 F4 89.44(11) . . ? F5 P1 F4 89.62(11) . . ? F1 P1 F3 89.93(12) . . ? F6 P1 F3 90.27(13) . . ? F2 P1 F3 89.17(11) . . ? F5 P1 F3 89.58(11) . . ? F4 P1 F3 178.41(13) . . ? C5 N2 N1 109.1(3) . . ? C5 N2 B1 128.6(3) . . ? N1 N2 B1 121.1(3) . . ? C7 N1 N2 105.8(3) . . ? C7 N1 Rh1 127.8(2) . . ? N2 N1 Rh1 124.9(2) . . ? C8 N5 N6 105.9(3) . . ? C8 N5 Rh2 126.7(2) . . ? N6 N5 Rh2 125.9(2) . . ? C10 N6 N5 108.5(3) . . ? C10 N6 B1 128.3(3) . . ? N5 N6 B1 121.7(3) . . ? C11 N4 N3 108.7(3) . . ? C11 N4 B1 128.5(3) . . ? N3 N4 B1 122.5(3) . . ? C13 N3 N4 106.5(3) . . ? C13 N3 Rh1 128.9(2) . . ? N4 N3 Rh1 123.87(19) . . ? C14 N8 N7 108.1(3) . . ? C14 N8 B1 128.7(3) . . ? N7 N8 B1 122.9(3) . . ? C16 N7 N8 107.0(3) . . ? C16 N7 Rh2 125.9(2) . . ? N8 N7 Rh2 123.3(2) . . ? O1 C1 Rh1 177.1(3) . . ? O2 C2 Rh1 174.8(3) . . ? O3 C3 Rh2 175.1(3) . . ? O4 C4 Rh2 178.5(3) . . ? N2 C5 C6 109.3(3) . . ? N2 C5 H5A 125.3 . . ? C6 C5 H5A 125.3 . . ? C5 C6 C7 104.7(3) . . ? C5 C6 H6A 127.6 . . ? C7 C6 H6A 127.6 . . ? N1 C7 C6 111.0(3) . . ? N1 C7 H7A 124.5 . . ? C6 C7 H7A 124.5 . . ? N5 C8 C9 111.0(3) . . ? N5 C8 H8A 124.5 . . ? C9 C8 H8A 124.5 . . ? C10 C9 C8 104.9(3) . . ? C10 C9 H9A 127.6 . . ? C8 C9 H9A 127.6 . . ? N6 C10 C9 109.7(3) . . ? N6 C10 H10A 125.2 . . ? C9 C10 H10A 125.2 . . ? N4 C11 C12 109.2(3) . . ? N4 C11 H11A 125.4 . . ? C12 C11 H11A 125.4 . . ? C11 C12 C13 104.8(3) . . ? C11 C12 H12A 127.6 . . ? C13 C12 H12A 127.6 . . ? N3 C13 C12 110.8(3) . . ? N3 C13 H13A 124.6 . . ? C12 C13 H13A 124.6 . . ? N8 C14 C15 109.4(3) . . ? N8 C14 H14A 125.3 . . ? C15 C14 H14A 125.3 . . ? C14 C15 C16 105.2(3) . . ? C14 C15 H15A 127.4 . . ? C16 C15 H15A 127.4 . . ? N7 C16 C15 110.3(3) . . ? N7 C16 H16A 124.8 . . ? C15 C16 H16A 124.8 . . ? N4 B1 N2 111.9(3) . . ? N4 B1 N6 106.6(3) . . ? N2 B1 N6 109.9(3) . . ? N4 B1 N8 112.1(3) . . ? N2 B1 N8 105.8(3) . . ? N6 B1 N8 110.6(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.435 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.078 data_5+ _database_code_depnum_ccdc_archive 'CCDC 768031' #TrackingRef '- Hallett_Dalton_Cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H42 B N8 O2 P2 Rh2, F6 P, 3(C H2 Cl2)' _chemical_formula_sum 'C53 H48 B Cl6 F6 N8 O2 P3 Rh2' _chemical_formula_weight 1465.23 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' B B 0.0013 0.0007 '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' O O 0.0106 0.0060 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.281(3) _cell_length_b 13.380(3) _cell_length_c 17.393(3) _cell_angle_alpha 84.36(2) _cell_angle_beta 74.524(16) _cell_angle_gamma 84.84(3) _cell_volume 2957.6(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 279 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 27.4755 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.645 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1468 _exptl_absorpt_coefficient_mu 0.977 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.842 _exptl_absorpt_correction_T_max 0.871 _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 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34118 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.48 _reflns_number_total 13538 _reflns_number_gt 11898 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _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^)+(0.0499P)^2^+7.8266P] 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 13538 _refine_ls_number_parameters 755 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1204 _refine_ls_wR_factor_gt 0.1163 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 0.86364(2) 0.855313(19) 0.377139(15) 0.01805(7) Uani 1 1 d . . . Rh2 Rh 0.72513(2) 0.541628(19) 0.218794(16) 0.01957(7) Uani 1 1 d . . . Cl1 Cl 0.42589(11) 0.28302(10) 0.16884(10) 0.0581(4) Uani 1 1 d . . . Cl2 Cl 0.20198(14) 0.3120(3) 0.21285(15) 0.1318(12) Uani 1 1 d . . . Cl3 Cl 0.41441(12) 0.26151(13) 0.41473(11) 0.0692(4) Uani 1 1 d . . . Cl4 Cl 0.57975(12) 0.12071(12) 0.44939(10) 0.0644(4) Uani 1 1 d . . . Cl5 Cl 0.22898(14) 0.06485(17) 0.40024(12) 0.0955(7) Uani 1 1 d . A 1 Cl6 Cl 0.38161(16) 0.02101(13) 0.25466(12) 0.0901(6) Uani 1 1 d . A 1 P1 P 0.89499(7) 0.98713(6) 0.28396(5) 0.01806(17) Uani 1 1 d . . . P2 P 0.73773(7) 0.60651(7) 0.09176(5) 0.02149(18) Uani 1 1 d . B . P3 P 0.28344(8) 0.65625(7) 0.32861(6) 0.0256(2) Uani 1 1 d . . . F1 F 0.2195(3) 0.6503(2) 0.41940(18) 0.0727(11) Uani 1 1 d . . . F2 F 0.3129(3) 0.7673(3) 0.3347(3) 0.0864(13) Uani 1 1 d . . . F3 F 0.3388(4) 0.6620(3) 0.2364(2) 0.0949(14) Uani 1 1 d . . . F4 F 0.2536(4) 0.5469(3) 0.3230(2) 0.0889(14) Uani 1 1 d . . . F5 F 0.1803(3) 0.7084(4) 0.3089(3) 0.0964(14) Uani 1 1 d . . . F6 F 0.3877(3) 0.6124(3) 0.3492(2) 0.0829(12) Uani 1 1 d . . . O1 O 1.0449(2) 0.9152(2) 0.42761(19) 0.0397(7) Uani 1 1 d . . . O2 O 0.5201(3) 0.4718(3) 0.2167(2) 0.0470(8) Uani 1 1 d . . . N1 N 0.8510(2) 0.7301(2) 0.46147(18) 0.0234(6) Uani 1 1 d . . . N2 N 0.8218(2) 0.6381(2) 0.45065(17) 0.0207(6) Uani 1 1 d . . . N3 N 0.7298(2) 0.8106(2) 0.35241(18) 0.0210(6) Uani 1 1 d . . . N4 N 0.7039(2) 0.7123(2) 0.36309(17) 0.0185(6) Uani 1 1 d . . . N5 N 0.7022(2) 0.4777(2) 0.33706(18) 0.0226(6) Uani 1 1 d . . . N6 N 0.7161(2) 0.5281(2) 0.39803(18) 0.0212(6) Uani 1 1 d . . . N7 N 0.8657(2) 0.5840(2) 0.23339(17) 0.0213(6) Uani 1 1 d . . . N8 N 0.8746(2) 0.6078(2) 0.30609(17) 0.0189(6) Uani 1 1 d . . . C1 C 0.9757(3) 0.8927(3) 0.4074(2) 0.0258(8) Uani 1 1 d . . . C2 C 0.5992(3) 0.4991(3) 0.2158(2) 0.0299(8) Uani 1 1 d . . . C3 C 0.8932(3) 0.7159(3) 0.5237(2) 0.0298(8) Uani 1 1 d . . . H3 H 0.9201 0.7676 0.5447 0.036 Uiso 1 1 calc R . . C4 C 0.8927(3) 0.6159(3) 0.5537(2) 0.0316(9) Uani 1 1 d . . . H4 H 0.9171 0.5867 0.5980 0.038 Uiso 1 1 calc R . . C5 C 0.8493(3) 0.5688(3) 0.5054(2) 0.0277(8) Uani 1 1 d . . . H5 H 0.8397 0.4988 0.5094 0.033 Uiso 1 1 calc R . . C6 C 0.6442(3) 0.8667(3) 0.3436(2) 0.0238(7) Uani 1 1 d . . . H6 H 0.6398 0.9381 0.3355 0.029 Uiso 1 1 calc R . . C7 C 0.5623(3) 0.8058(3) 0.3480(2) 0.0271(8) Uani 1 1 d . . . H7 H 0.4936 0.8264 0.3434 0.033 Uiso 1 1 calc R . . C8 C 0.6036(3) 0.7093(3) 0.3605(2) 0.0219(7) Uani 1 1 d . . . H8 H 0.5672 0.6499 0.3663 0.026 Uiso 1 1 calc R . . C9 C 0.6419(3) 0.4027(3) 0.3722(2) 0.0283(8) Uani 1 1 d . . . H9 H 0.6210 0.3542 0.3443 0.034 Uiso 1 1 calc R . . C10 C 0.6139(3) 0.4050(3) 0.4544(2) 0.0302(8) Uani 1 1 d . . . H10 H 0.5711 0.3605 0.4926 0.036 Uiso 1 1 calc R . . C11 C 0.6613(3) 0.4858(3) 0.4689(2) 0.0269(8) Uani 1 1 d . . . H11 H 0.6564 0.5080 0.5200 0.032 Uiso 1 1 calc R . . C12 C 0.9637(3) 0.5707(3) 0.1877(2) 0.0258(7) Uani 1 1 d . . . H12 H 0.9813 0.5533 0.1338 0.031 Uiso 1 1 calc R . . C13 C 1.0361(3) 0.5858(3) 0.2291(2) 0.0292(8) Uani 1 1 d . . . H13 H 1.1102 0.5809 0.2101 0.035 Uiso 1 1 calc R . . C14 C 0.9768(3) 0.6094(3) 0.3039(2) 0.0249(7) Uani 1 1 d . . . H14 H 1.0035 0.6243 0.3467 0.030 Uiso 1 1 calc R . . C15 C 1.0137(3) 0.9645(3) 0.2039(2) 0.0207(7) Uani 1 1 d . . . C16 C 1.0340(3) 1.0259(3) 0.1318(2) 0.0286(8) Uani 1 1 d . . . H16 H 0.9851 1.0796 0.1238 0.034 Uiso 1 1 calc R . . C17 C 1.1248(3) 1.0081(3) 0.0726(3) 0.0345(9) Uani 1 1 d . . . H17 H 1.1383 1.0500 0.0241 0.041 Uiso 1 1 calc R . . C18 C 1.1962(3) 0.9299(3) 0.0832(2) 0.0321(9) Uani 1 1 d . . . H18 H 1.2590 0.9187 0.0424 0.039 Uiso 1 1 calc R . . C19 C 1.1762(3) 0.8683(3) 0.1530(2) 0.0320(9) Uani 1 1 d . . . H19 H 1.2250 0.8140 0.1600 0.038 Uiso 1 1 calc R . . C20 C 1.0851(3) 0.8848(3) 0.2131(2) 0.0248(7) Uani 1 1 d . . . H20 H 1.0716 0.8414 0.2608 0.030 Uiso 1 1 calc R . . C21 C 0.9064(3) 1.1044(3) 0.3259(2) 0.0223(7) Uani 1 1 d . . . C22 C 0.9553(3) 1.1863(3) 0.2809(3) 0.0318(8) Uani 1 1 d . . . H22 H 0.9958 1.1795 0.2274 0.038 Uiso 1 1 calc R . . C23 C 0.9450(4) 1.2786(3) 0.3141(3) 0.0406(10) Uani 1 1 d . . . H23 H 0.9773 1.3351 0.2830 0.049 Uiso 1 1 calc R . . C24 C 0.8877(4) 1.2874(3) 0.3923(3) 0.0386(10) Uani 1 1 d . . . H24 H 0.8806 1.3505 0.4146 0.046 Uiso 1 1 calc R . . C25 C 0.8409(4) 1.2067(3) 0.4383(3) 0.0371(10) Uani 1 1 d . . . H25 H 0.8022 1.2135 0.4922 0.045 Uiso 1 1 calc R . . C26 C 0.8508(3) 1.1147(3) 0.4050(2) 0.0305(8) Uani 1 1 d . . . H26 H 0.8192 1.0582 0.4367 0.037 Uiso 1 1 calc R . . C27 C 0.7976(3) 1.0263(3) 0.2279(2) 0.0209(7) Uani 1 1 d . . . C28 C 0.7350(3) 1.1155(3) 0.2394(2) 0.0281(8) Uani 1 1 d . . . H28 H 0.7452 1.1609 0.2749 0.034 Uiso 1 1 calc R . . C29 C 0.6572(4) 1.1384(3) 0.1989(3) 0.0392(10) Uani 1 1 d . . . H29 H 0.6150 1.1996 0.2064 0.047 Uiso 1 1 calc R . . C30 C 0.6417(3) 1.0721(3) 0.1478(3) 0.0358(9) Uani 1 1 d . . . H30 H 0.5881 1.0877 0.1208 0.043 Uiso 1 1 calc R . . C31 C 0.7032(3) 0.9834(3) 0.1357(2) 0.0309(8) Uani 1 1 d . . . H31 H 0.6925 0.9380 0.1004 0.037 Uiso 1 1 calc R . . C32 C 0.7809(3) 0.9612(3) 0.1756(2) 0.0272(8) Uani 1 1 d . . . H32 H 0.8236 0.9003 0.1671 0.033 Uiso 1 1 calc R . . C33 C 0.6491(3) 0.7162(3) 0.0801(2) 0.0251(7) Uani 1 1 d . . . C34 C 0.5619(3) 0.7384(3) 0.1423(3) 0.0288(8) Uani 1 1 d . . . H34 H 0.5512 0.6995 0.1922 0.035 Uiso 1 1 calc R . . C35 C 0.4899(3) 0.8183(3) 0.1316(3) 0.0348(9) Uani 1 1 d . . . H35 H 0.4304 0.8335 0.1742 0.042 Uiso 1 1 calc R . . C36 C 0.5057(3) 0.8748(3) 0.0589(3) 0.0357(10) Uani 1 1 d . . . H36 H 0.4566 0.9287 0.0517 0.043 Uiso 1 1 calc R . . C37 C 0.5924(4) 0.8534(3) -0.0032(3) 0.0344(9) Uani 1 1 d . . . H37 H 0.6025 0.8921 -0.0532 0.041 Uiso 1 1 calc R . . C38 C 0.6647(3) 0.7754(3) 0.0076(2) 0.0288(8) Uani 1 1 d . . . H38 H 0.7252 0.7620 -0.0346 0.035 Uiso 1 1 calc R . . C39 C 0.7071(3) 0.5151(3) 0.0310(2) 0.0278(8) Uani 1 1 d . . . C40 C 0.6746(17) 0.5371(8) -0.0354(8) 0.040(3) Uani 0.57(3) 1 d P B 1 H40 H 0.6682 0.6058 -0.0544 0.048 Uiso 0.57(3) 1 calc PR B 1 C41 C 0.6498(17) 0.4648(11) -0.0780(11) 0.050(4) Uani 0.57(3) 1 d P B 1 H41 H 0.6261 0.4848 -0.1245 0.059 Uiso 0.57(3) 1 calc PR B 1 C42 C 0.6588(4) 0.3684(4) -0.0544(3) 0.0429(11) Uani 1 1 d . . . H42 H 0.6411 0.3197 -0.0840 0.051 Uiso 1 1 calc R B 1 C43 C 0.6946(10) 0.3365(8) 0.0143(7) 0.031(2) Uani 0.57(3) 1 d P B 1 H43 H 0.7011 0.2670 0.0312 0.038 Uiso 0.57(3) 1 calc PR B 1 C44 C 0.7198(9) 0.4089(7) 0.0562(6) 0.025(2) Uani 0.57(3) 1 d P B 1 H44 H 0.7456 0.3892 0.1018 0.030 Uiso 0.57(3) 1 calc PR B 1 C45 C 0.86261(16) 0.65403(18) 0.03409(14) 0.0248(7) Uani 1 1 d G . . C46 C 0.9196(2) 0.61893(19) -0.03857(15) 0.0359(9) Uani 1 1 d G B . H46 H 0.8948 0.5664 -0.0601 0.043 Uiso 1 1 calc R . . C40' C 0.6273(14) 0.5421(11) -0.0113(12) 0.030(3) Uani 0.43(3) 1 d P B 2 H40' H 0.5929 0.6076 -0.0111 0.036 Uiso 0.43(3) 1 calc PR B 2 C41' C 0.6032(16) 0.4656(16) -0.0530(12) 0.042(4) Uani 0.43(3) 1 d P B 2 H41' H 0.5497 0.4787 -0.0803 0.050 Uiso 0.43(3) 1 calc PR B 2 C43' C 0.738(2) 0.3573(17) -0.021(2) 0.077(9) Uani 0.43(3) 1 d P B 2 H43' H 0.7797 0.2958 -0.0260 0.092 Uiso 0.43(3) 1 calc PR B 2 C44' C 0.763(2) 0.4329(15) 0.021(2) 0.072(9) Uani 0.43(3) 1 d P B 2 H44' H 0.8228 0.4219 0.0414 0.086 Uiso 0.43(3) 1 calc PR B 2 C1S C 0.3176(5) 0.3280(8) 0.2385(4) 0.091(3) Uani 1 1 d . . . H99A H 0.3231 0.4005 0.2427 0.109 Uiso 1 1 calc R . . H99B H 0.3156 0.2922 0.2914 0.109 Uiso 1 1 calc R . . C2S C 0.4523(5) 0.1353(5) 0.4389(4) 0.0669(17) Uani 1 1 d . . . H98A H 0.4036 0.1106 0.4896 0.080 Uiso 1 1 calc R . . H98B H 0.4469 0.0936 0.3964 0.080 Uiso 1 1 calc R . . C3S C 0.2512(5) 0.0066(5) 0.3110(4) 0.0612(15) Uani 1 1 d . A 1 H97A H 0.2023 0.0374 0.2800 0.073 Uiso 1 1 calc R A 1 H97B H 0.2389 -0.0659 0.3230 0.073 Uiso 1 1 calc R A 1 B1 B 0.7795(3) 0.6227(3) 0.3789(2) 0.0192(7) Uani 1 1 d . . . C47 C 1.0128(2) 0.6608(2) -0.07974(14) 0.0441(11) Uani 1 1 d G B . H47 H 1.0517 0.6368 -0.1294 0.053 Uiso 1 1 calc R . . C48 C 1.04909(17) 0.7377(2) -0.04826(17) 0.0409(10) Uani 1 1 d G B . H48 H 1.1128 0.7663 -0.0764 0.049 Uiso 1 1 calc R . . C49 C 0.9921(2) 0.77277(17) 0.02439(17) 0.0369(9) Uani 1 1 d G B . H49 H 1.0169 0.8253 0.0459 0.044 Uiso 1 1 calc R . . C50 C 0.89890(19) 0.73095(18) 0.06557(13) 0.0307(8) Uani 1 1 d G B . H50 H 0.8600 0.7549 0.1152 0.037 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 0.01900(14) 0.01840(13) 0.01738(13) 0.00037(9) -0.00573(10) -0.00356(10) Rh2 0.02022(14) 0.01904(13) 0.02204(14) -0.00348(10) -0.00940(11) -0.00095(10) Cl1 0.0576(8) 0.0432(6) 0.0874(10) -0.0166(6) -0.0443(8) 0.0133(6) Cl2 0.0456(10) 0.253(4) 0.1062(17) -0.067(2) -0.0108(10) -0.0262(15) Cl3 0.0568(8) 0.0790(10) 0.0785(10) -0.0143(8) -0.0201(8) -0.0238(8) Cl4 0.0523(8) 0.0744(10) 0.0638(9) -0.0226(7) -0.0023(7) -0.0102(7) Cl5 0.0686(11) 0.1204(16) 0.0936(13) -0.0584(12) 0.0173(9) -0.0479(11) Cl6 0.0897(12) 0.0685(10) 0.0846(12) -0.0246(9) 0.0387(10) -0.0278(9) P1 0.0196(4) 0.0172(4) 0.0177(4) -0.0009(3) -0.0052(3) -0.0016(3) P2 0.0236(4) 0.0226(4) 0.0208(4) -0.0073(3) -0.0098(4) 0.0033(3) P3 0.0276(5) 0.0286(5) 0.0221(5) 0.0041(4) -0.0098(4) -0.0062(4) F1 0.114(3) 0.0411(16) 0.0367(16) -0.0034(13) 0.0217(17) 0.0057(17) F2 0.092(3) 0.0472(19) 0.112(3) -0.011(2) -0.002(2) -0.0339(19) F3 0.139(4) 0.099(3) 0.0296(17) 0.0150(18) 0.000(2) -0.005(3) F4 0.131(4) 0.053(2) 0.068(2) -0.0248(17) 0.020(2) -0.047(2) F5 0.065(2) 0.123(4) 0.106(3) 0.024(3) -0.047(2) 0.007(2) F6 0.055(2) 0.131(3) 0.063(2) -0.009(2) -0.0294(18) 0.035(2) O1 0.0402(17) 0.0471(18) 0.0400(17) 0.0105(14) -0.0243(14) -0.0193(14) O2 0.0367(18) 0.053(2) 0.059(2) -0.0010(16) -0.0234(16) -0.0158(15) N1 0.0268(16) 0.0254(15) 0.0197(15) 0.0010(12) -0.0074(12) -0.0095(12) N2 0.0231(15) 0.0203(14) 0.0205(14) 0.0019(11) -0.0092(12) -0.0045(11) N3 0.0202(14) 0.0191(14) 0.0243(15) 0.0008(11) -0.0074(12) -0.0031(11) N4 0.0192(14) 0.0189(13) 0.0178(14) 0.0000(10) -0.0054(11) -0.0034(11) N5 0.0255(15) 0.0192(14) 0.0250(15) 0.0013(11) -0.0099(12) -0.0050(11) N6 0.0235(15) 0.0197(14) 0.0218(15) -0.0002(11) -0.0080(12) -0.0033(11) N7 0.0215(15) 0.0236(14) 0.0195(14) -0.0031(11) -0.0064(12) -0.0008(11) N8 0.0196(14) 0.0187(13) 0.0196(14) -0.0004(11) -0.0076(11) -0.0009(11) C1 0.030(2) 0.0242(18) 0.0230(18) 0.0046(14) -0.0078(15) -0.0063(15) C2 0.033(2) 0.0285(19) 0.032(2) -0.0015(16) -0.0153(17) -0.0015(16) C3 0.039(2) 0.033(2) 0.0240(19) 0.0049(15) -0.0178(17) -0.0151(17) C4 0.040(2) 0.036(2) 0.0238(19) 0.0082(16) -0.0173(17) -0.0110(17) C5 0.031(2) 0.0260(18) 0.0275(19) 0.0051(15) -0.0123(16) -0.0045(15) C6 0.0211(17) 0.0228(17) 0.0258(18) -0.0005(14) -0.0047(14) 0.0015(13) C7 0.0204(17) 0.0326(19) 0.0280(19) -0.0030(15) -0.0059(15) 0.0003(14) C8 0.0195(16) 0.0259(17) 0.0204(17) -0.0019(13) -0.0044(13) -0.0047(13) C9 0.0289(19) 0.0227(17) 0.037(2) 0.0004(15) -0.0141(17) -0.0078(15) C10 0.0259(19) 0.0285(19) 0.036(2) 0.0045(16) -0.0081(17) -0.0085(15) C11 0.0289(19) 0.0278(18) 0.0240(18) 0.0032(14) -0.0072(15) -0.0072(15) C12 0.0235(18) 0.0282(18) 0.0250(18) -0.0033(14) -0.0063(15) 0.0031(14) C13 0.0183(17) 0.033(2) 0.035(2) -0.0030(16) -0.0070(16) 0.0026(15) C14 0.0210(17) 0.0288(18) 0.0275(19) -0.0011(14) -0.0113(15) -0.0015(14) C15 0.0181(16) 0.0223(16) 0.0214(17) -0.0015(13) -0.0044(13) -0.0025(13) C16 0.030(2) 0.0243(18) 0.0274(19) 0.0025(15) -0.0030(16) 0.0026(15) C17 0.034(2) 0.034(2) 0.029(2) 0.0066(16) 0.0009(17) -0.0022(17) C18 0.0240(19) 0.039(2) 0.029(2) -0.0052(17) -0.0006(16) -0.0002(16) C19 0.0254(19) 0.036(2) 0.033(2) -0.0041(17) -0.0080(16) 0.0086(16) C20 0.0269(19) 0.0259(18) 0.0216(17) -0.0010(14) -0.0078(15) 0.0011(14) C21 0.0241(18) 0.0192(16) 0.0271(18) -0.0046(13) -0.0121(15) 0.0002(13) C22 0.034(2) 0.0273(19) 0.034(2) -0.0033(16) -0.0065(17) -0.0087(16) C23 0.042(2) 0.026(2) 0.057(3) -0.0055(19) -0.015(2) -0.0115(18) C24 0.041(2) 0.031(2) 0.055(3) -0.0196(19) -0.027(2) 0.0055(18) C25 0.045(3) 0.034(2) 0.036(2) -0.0163(18) -0.016(2) 0.0084(18) C26 0.038(2) 0.0282(19) 0.027(2) -0.0061(15) -0.0115(17) 0.0000(16) C27 0.0216(17) 0.0210(16) 0.0193(16) 0.0002(13) -0.0043(13) -0.0025(13) C28 0.0276(19) 0.0275(19) 0.031(2) -0.0063(15) -0.0111(16) 0.0041(15) C29 0.037(2) 0.035(2) 0.050(3) -0.0044(19) -0.023(2) 0.0112(18) C30 0.030(2) 0.048(2) 0.032(2) 0.0035(18) -0.0130(17) -0.0045(18) C31 0.031(2) 0.042(2) 0.0225(19) -0.0084(16) -0.0071(16) -0.0082(17) C32 0.0278(19) 0.0275(18) 0.0270(19) -0.0066(15) -0.0075(15) 0.0010(15) C33 0.0267(18) 0.0213(17) 0.032(2) -0.0086(14) -0.0151(16) 0.0037(14) C34 0.0256(19) 0.0274(19) 0.035(2) -0.0046(16) -0.0102(16) 0.0010(15) C35 0.0232(19) 0.028(2) 0.055(3) -0.0078(18) -0.0131(19) 0.0029(15) C36 0.032(2) 0.0216(18) 0.060(3) -0.0054(18) -0.024(2) 0.0026(16) C37 0.050(3) 0.0205(18) 0.040(2) -0.0021(16) -0.024(2) 0.0006(17) C38 0.036(2) 0.0250(18) 0.028(2) -0.0055(15) -0.0135(17) 0.0029(15) C39 0.030(2) 0.0293(19) 0.0283(19) -0.0123(15) -0.0118(16) 0.0015(15) C40 0.072(10) 0.021(4) 0.033(6) -0.002(4) -0.028(6) 0.007(5) C41 0.081(12) 0.036(5) 0.048(8) -0.005(5) -0.044(8) -0.007(7) C42 0.050(3) 0.041(2) 0.048(3) -0.023(2) -0.024(2) -0.002(2) C43 0.045(6) 0.021(4) 0.034(5) -0.007(3) -0.018(4) -0.001(4) C44 0.036(5) 0.017(4) 0.027(4) -0.001(3) -0.020(4) 0.001(3) C45 0.0249(18) 0.0280(18) 0.0231(18) -0.0028(14) -0.0103(15) 0.0036(14) C46 0.035(2) 0.041(2) 0.032(2) -0.0119(18) -0.0085(18) 0.0054(18) C40' 0.030(7) 0.024(5) 0.041(8) -0.009(5) -0.019(6) 0.002(5) C41' 0.045(9) 0.053(8) 0.040(10) -0.002(7) -0.030(7) -0.015(8) C43' 0.087(17) 0.048(11) 0.12(2) -0.058(13) -0.071(17) 0.038(11) C44' 0.091(17) 0.038(9) 0.12(2) -0.041(12) -0.083(18) 0.021(10) C1S 0.062(4) 0.156(8) 0.068(4) -0.036(5) -0.025(4) -0.016(5) C2S 0.069(4) 0.074(4) 0.062(4) -0.005(3) -0.013(3) -0.035(3) C3S 0.059(3) 0.057(3) 0.064(4) -0.020(3) -0.001(3) -0.016(3) B1 0.0217(19) 0.0187(17) 0.0190(18) -0.0012(14) -0.0081(15) -0.0022(14) C47 0.034(2) 0.052(3) 0.038(2) -0.010(2) 0.0038(19) 0.006(2) C48 0.028(2) 0.034(2) 0.053(3) 0.009(2) -0.005(2) 0.0030(17) C49 0.035(2) 0.026(2) 0.051(3) 0.0021(18) -0.016(2) -0.0006(17) C50 0.035(2) 0.0246(18) 0.031(2) -0.0047(15) -0.0078(17) 0.0030(16) _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 1.830(4) . ? Rh1 N3 2.087(3) . ? Rh1 N1 2.103(3) . ? Rh1 P1 2.2629(11) . ? Rh2 C2 1.829(4) . ? Rh2 N7 2.084(3) . ? Rh2 N5 2.103(3) . ? Rh2 P2 2.2617(11) . ? Cl1 C1S 1.719(7) . ? Cl2 C1S 1.746(6) . ? Cl3 C2S 1.762(7) . ? Cl4 C2S 1.742(7) . ? Cl5 C3S 1.747(6) . ? Cl6 C3S 1.765(6) . ? P1 C21 1.828(3) . ? P1 C15 1.828(4) . ? P1 C27 1.830(4) . ? P2 C45 1.827(2) . ? P2 C33 1.827(4) . ? P2 C39 1.831(4) . ? P3 F4 1.569(3) . ? P3 F6 1.571(3) . ? P3 F3 1.574(3) . ? P3 F1 1.579(3) . ? P3 F5 1.585(4) . ? P3 F2 1.591(3) . ? O1 C1 1.141(5) . ? O2 C2 1.139(5) . ? N1 C3 1.337(5) . ? N1 N2 1.367(4) . ? N2 C5 1.360(5) . ? N2 B1 1.537(5) . ? N3 C6 1.339(5) . ? N3 N4 1.371(4) . ? N4 C8 1.350(4) . ? N4 B1 1.545(5) . ? N5 C9 1.336(5) . ? N5 N6 1.372(4) . ? N6 C11 1.352(5) . ? N6 B1 1.542(5) . ? N7 C12 1.338(5) . ? N7 N8 1.371(4) . ? N8 C14 1.350(4) . ? N8 B1 1.546(5) . ? C3 C4 1.387(5) . ? C3 H3 0.9500 . ? C4 C5 1.366(5) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.399(5) . ? C6 H6 0.9500 . ? C7 C8 1.378(5) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.380(6) . ? C9 H9 0.9500 . ? C10 C11 1.374(5) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.384(5) . ? C12 H12 0.9500 . ? C13 C14 1.379(5) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C20 1.388(5) . ? C15 C16 1.405(5) . ? C16 C17 1.381(6) . ? C16 H16 0.9500 . ? C17 C18 1.380(6) . ? C17 H17 0.9500 . ? C18 C19 1.376(6) . ? C18 H18 0.9500 . ? C19 C20 1.389(5) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.388(5) . ? C21 C26 1.390(5) . ? C22 C23 1.394(6) . ? C22 H22 0.9500 . ? C23 C24 1.382(7) . ? C23 H23 0.9500 . ? C24 C25 1.370(7) . ? C24 H24 0.9500 . ? C25 C26 1.393(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.390(5) . ? C27 C28 1.391(5) . ? C28 C29 1.396(5) . ? C28 H28 0.9500 . ? C29 C30 1.379(6) . ? C29 H29 0.9500 . ? C30 C31 1.380(6) . ? C30 H30 0.9500 . ? C31 C32 1.387(5) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.390(5) . ? C33 C38 1.397(5) . ? C34 C35 1.400(5) . ? C34 H34 0.9500 . ? C35 C36 1.383(6) . ? C35 H35 0.9500 . ? C36 C37 1.384(7) . ? C36 H36 0.9500 . ? C37 C38 1.387(5) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C44' 1.271(16) . ? C39 C40 1.335(11) . ? C39 C40' 1.446(14) . ? C39 C44 1.453(10) . ? C40 C41 1.386(18) . ? C40 H40 0.9500 . ? C41 C42 1.319(15) . ? C41 H41 0.9500 . ? C42 C43' 1.312(18) . ? C42 C43 1.415(12) . ? C42 C41' 1.44(2) . ? C42 H42 0.9500 . ? C43 C44 1.381(14) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.3900 . ? C45 C50 1.3900 . ? C46 C47 1.3900 . ? C46 H46 0.9500 . ? C40' C41' 1.42(2) . ? C40' H40' 0.9500 . ? C41' H41' 0.9500 . ? C43' C44' 1.42(2) . ? C43' H43' 0.9500 . ? C44' H44' 0.9500 . ? C1S H99A 0.9900 . ? C1S H99B 0.9900 . ? C2S H98A 0.9900 . ? C2S H98B 0.9900 . ? C3S H97A 0.9900 . ? C3S H97B 0.9900 . ? C47 C48 1.3900 . ? C47 H47 0.9500 . ? C48 C49 1.3900 . ? C48 H48 0.9500 . ? C49 C50 1.3900 . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? 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 N3 175.38(14) . . ? C1 Rh1 N1 90.05(14) . . ? N3 Rh1 N1 86.66(11) . . ? C1 Rh1 P1 85.44(11) . . ? N3 Rh1 P1 98.04(9) . . ? N1 Rh1 P1 174.22(9) . . ? C2 Rh2 N7 174.53(15) . . ? C2 Rh2 N5 89.85(15) . . ? N7 Rh2 N5 84.68(12) . . ? C2 Rh2 P2 85.79(13) . . ? N7 Rh2 P2 99.68(9) . . ? N5 Rh2 P2 175.64(8) . . ? C21 P1 C15 107.75(16) . . ? C21 P1 C27 101.45(16) . . ? C15 P1 C27 102.15(16) . . ? C21 P1 Rh1 113.07(12) . . ? C15 P1 Rh1 112.59(12) . . ? C27 P1 Rh1 118.54(12) . . ? C45 P2 C33 100.28(16) . . ? C45 P2 C39 105.67(15) . . ? C33 P2 C39 103.83(17) . . ? C45 P2 Rh2 117.98(9) . . ? C33 P2 Rh2 115.90(13) . . ? C39 P2 Rh2 111.58(14) . . ? F4 P3 F6 90.1(3) . . ? F4 P3 F3 89.2(2) . . ? F6 P3 F3 91.4(2) . . ? F4 P3 F1 89.04(18) . . ? F6 P3 F1 92.8(2) . . ? F3 P3 F1 175.5(3) . . ? F4 P3 F5 94.0(3) . . ? F6 P3 F5 175.9(3) . . ? F3 P3 F5 89.1(3) . . ? F1 P3 F5 86.9(2) . . ? F4 P3 F2 179.6(2) . . ? F6 P3 F2 90.1(2) . . ? F3 P3 F2 91.1(2) . . ? F1 P3 F2 90.7(2) . . ? F5 P3 F2 85.7(3) . . ? C3 N1 N2 106.2(3) . . ? C3 N1 Rh1 127.1(2) . . ? N2 N1 Rh1 124.7(2) . . ? C5 N2 N1 108.8(3) . . ? C5 N2 B1 129.5(3) . . ? N1 N2 B1 121.2(3) . . ? C6 N3 N4 106.6(3) . . ? C6 N3 Rh1 129.0(2) . . ? N4 N3 Rh1 122.6(2) . . ? C8 N4 N3 109.1(3) . . ? C8 N4 B1 127.4(3) . . ? N3 N4 B1 123.5(3) . . ? C9 N5 N6 105.9(3) . . ? C9 N5 Rh2 127.4(3) . . ? N6 N5 Rh2 123.2(2) . . ? C11 N6 N5 109.3(3) . . ? C11 N6 B1 130.4(3) . . ? N5 N6 B1 120.1(3) . . ? C12 N7 N8 106.0(3) . . ? C12 N7 Rh2 130.4(2) . . ? N8 N7 Rh2 121.6(2) . . ? C14 N8 N7 109.4(3) . . ? C14 N8 B1 127.3(3) . . ? N7 N8 B1 123.2(3) . . ? O1 C1 Rh1 178.8(3) . . ? O2 C2 Rh2 177.7(4) . . ? N1 C3 C4 111.2(3) . . ? N1 C3 H3 124.4 . . ? C4 C3 H3 124.4 . . ? C5 C4 C3 104.6(3) . . ? C5 C4 H4 127.7 . . ? C3 C4 H4 127.7 . . ? N2 C5 C4 109.1(3) . . ? N2 C5 H5 125.4 . . ? C4 C5 H5 125.4 . . ? N3 C6 C7 110.7(3) . . ? N3 C6 H6 124.7 . . ? C7 C6 H6 124.7 . . ? C8 C7 C6 104.4(3) . . ? C8 C7 H7 127.8 . . ? C6 C7 H7 127.8 . . ? N4 C8 C7 109.3(3) . . ? N4 C8 H8 125.4 . . ? C7 C8 H8 125.4 . . ? N5 C9 C10 111.2(3) . . ? N5 C9 H9 124.4 . . ? C10 C9 H9 124.4 . . ? C11 C10 C9 105.0(3) . . ? C11 C10 H10 127.5 . . ? C9 C10 H10 127.5 . . ? N6 C11 C10 108.4(3) . . ? N6 C11 H11 125.8 . . ? C10 C11 H11 125.8 . . ? N7 C12 C13 111.1(3) . . ? N7 C12 H12 124.4 . . ? C13 C12 H12 124.4 . . ? C14 C13 C12 104.8(3) . . ? C14 C13 H13 127.6 . . ? C12 C13 H13 127.6 . . ? N8 C14 C13 108.6(3) . . ? N8 C14 H14 125.7 . . ? C13 C14 H14 125.7 . . ? C20 C15 C16 118.8(3) . . ? C20 C15 P1 120.1(3) . . ? C16 C15 P1 121.1(3) . . ? C17 C16 C15 120.1(4) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C18 C17 C16 120.6(4) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C19 C18 C17 119.8(4) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 120.5(4) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C15 C20 C19 120.3(4) . . ? C15 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C22 C21 C26 119.2(3) . . ? C22 C21 P1 123.6(3) . . ? C26 C21 P1 116.7(3) . . ? C21 C22 C23 120.0(4) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 119.7(4) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C25 C24 C23 121.1(4) . . ? C25 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C24 C25 C26 119.1(4) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C21 C26 C25 120.9(4) . . ? C21 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C32 C27 C28 118.8(3) . . ? C32 C27 P1 118.5(3) . . ? C28 C27 P1 122.6(3) . . ? C27 C28 C29 120.1(4) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 120.1(4) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C31 120.5(4) . . ? C29 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C30 C31 C32 119.3(4) . . ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? C31 C32 C27 121.3(4) . . ? C31 C32 H32 119.4 . . ? C27 C32 H32 119.4 . . ? C34 C33 C38 119.2(3) . . ? C34 C33 P2 119.9(3) . . ? C38 C33 P2 120.7(3) . . ? C33 C34 C35 120.1(4) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C36 C35 C34 119.8(4) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C37 120.4(4) . . ? C35 C36 H36 119.8 . . ? C37 C36 H36 119.8 . . ? C36 C37 C38 119.8(4) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? C37 C38 C33 120.5(4) . . ? C37 C38 H38 119.7 . . ? C33 C38 H38 119.7 . . ? C44' C39 C40 105.8(10) . . ? C44' C39 C40' 121.0(9) . . ? C40 C39 C40' 27.0(5) . . ? C44' C39 C44 32.7(16) . . ? C40 C39 C44 116.5(6) . . ? C40' C39 C44 115.8(7) . . ? C44' C39 P2 119.3(7) . . ? C40 C39 P2 125.7(5) . . ? C40' C39 P2 119.4(7) . . ? C44 C39 P2 117.7(4) . . ? C39 C40 C41 123.3(10) . . ? C39 C40 H40 118.3 . . ? C41 C40 H40 118.3 . . ? C42 C41 C40 120.5(12) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C43' C42 C41 106.2(12) . . ? C43' C42 C43 32.6(15) . . ? C41 C42 C43 121.0(8) . . ? C43' C42 C41' 117.0(10) . . ? C41 C42 C41' 27.1(7) . . ? C43 C42 C41' 115.5(9) . . ? C43' C42 H42 124.8 . . ? C41 C42 H42 119.5 . . ? C43 C42 H42 119.5 . . ? C41' C42 H42 117.8 . . ? C44 C43 C42 118.3(8) . . ? C44 C43 H43 120.9 . . ? C42 C43 H43 120.9 . . ? C43 C44 C39 120.4(8) . . ? C43 C44 H44 119.8 . . ? C39 C44 H44 119.8 . . ? C46 C45 C50 120.0 . . ? C46 C45 P2 123.52(14) . . ? C50 C45 P2 116.46(14) . . ? C47 C46 C45 120.0 . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C41' C40' C39 116.3(13) . . ? C41' C40' H40' 121.9 . . ? C39 C40' H40' 121.9 . . ? C40' C41' C42 120.6(14) . . ? C40' C41' H41' 119.7 . . ? C42 C41' H41' 119.7 . . ? C42 C43' C44' 123.1(14) . . ? C42 C43' H43' 118.5 . . ? C44' C43' H43' 118.5 . . ? C39 C44' C43' 121.0(14) . . ? C39 C44' H44' 119.5 . . ? C43' C44' H44' 119.5 . . ? Cl1 C1S Cl2 111.6(4) . . ? Cl1 C1S H99A 109.3 . . ? Cl2 C1S H99A 109.3 . . ? Cl1 C1S H99B 109.3 . . ? Cl2 C1S H99B 109.3 . . ? H99A C1S H99B 108.0 . . ? Cl4 C2S Cl3 112.4(3) . . ? Cl4 C2S H98A 109.1 . . ? Cl3 C2S H98A 109.1 . . ? Cl4 C2S H98B 109.1 . . ? Cl3 C2S H98B 109.1 . . ? H98A C2S H98B 107.9 . . ? Cl5 C3S Cl6 109.3(3) . . ? Cl5 C3S H97A 109.8 . . ? Cl6 C3S H97A 109.8 . . ? Cl5 C3S H97B 109.8 . . ? Cl6 C3S H97B 109.8 . . ? H97A C3S H97B 108.3 . . ? N2 B1 N6 109.2(3) . . ? N2 B1 N4 111.0(3) . . ? N6 B1 N4 106.9(3) . . ? N2 B1 N8 107.6(3) . . ? N6 B1 N8 110.0(3) . . ? N4 B1 N8 112.2(3) . . ? C46 C47 C48 120.0 . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C49 C48 C47 120.0 . . ? C49 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C50 C49 C48 120.0 . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C49 C50 C45 120.0 . . ? C49 C50 H50 120.0 . . ? C45 C50 H50 120.0 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.180 _refine_diff_density_min -1.498 _refine_diff_density_rms 0.109 data_10 _database_code_depnum_ccdc_archive 'CCDC 768032' #TrackingRef '- Hallett_Dalton_Cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 B Cl2 Co N8 Rh' _chemical_formula_sum 'C20 H24 B Cl2 Co N8 Rh' _chemical_formula_weight 620.02 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' B B 0.0013 0.0007 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7796(12) _cell_length_b 9.8601(12) _cell_length_c 13.4916(17) _cell_angle_alpha 94.068(2) _cell_angle_beta 103.562(2) _cell_angle_gamma 104.509(2) _cell_volume 1212.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 89 _cell_measurement_theta_min 3.042 _cell_measurement_theta_max 27.4355 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 622 _exptl_absorpt_coefficient_mu 1.610 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.468921 _exptl_absorpt_correction_T_max 0.564884 _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 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7977 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0718 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5441 _reflns_number_gt 3976 _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^)+(0.0242P)^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 5441 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0675 _refine_ls_wR_factor_gt 0.0625 _refine_ls_goodness_of_fit_ref 0.902 _refine_ls_restrained_S_all 0.902 _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 0.12025(3) 0.35133(3) 0.29672(2) 0.01911(8) Uani 1 1 d . . . Co1 Co 0.47323(5) 0.91026(4) 0.20614(4) 0.02125(12) Uani 1 1 d . . . Cl1 Cl 0.55038(9) 1.14371(8) 0.25531(7) 0.0274(2) Uani 1 1 d . . . Cl2 Cl 0.63635(10) 0.83238(10) 0.14657(8) 0.0364(2) Uani 1 1 d . . . N1 N -0.0336(3) 0.4521(3) 0.2229(2) 0.0197(6) Uani 1 1 d . . . N2 N 0.0081(3) 0.5862(3) 0.1963(2) 0.0187(6) Uani 1 1 d . . . N3 N 0.2467(3) 0.4293(3) 0.1977(2) 0.0223(6) Uani 1 1 d . . . N4 N 0.2309(3) 0.5430(3) 0.1478(2) 0.0184(6) Uani 1 1 d . . . N5 N 0.2743(3) 0.8680(3) 0.1075(2) 0.0221(6) Uani 1 1 d . . . N6 N 0.1550(3) 0.7587(3) 0.1074(2) 0.0193(6) Uani 1 1 d . . . N7 N 0.3978(3) 0.8099(3) 0.3145(2) 0.0218(6) Uani 1 1 d . . . N8 N 0.2555(3) 0.7278(3) 0.2958(2) 0.0177(6) Uani 1 1 d . . . C1 C -0.0387(4) 0.1970(4) 0.3432(3) 0.0299(9) Uani 1 1 d . . . H1A H -0.1416 0.1847 0.3026 0.036 Uiso 1 1 calc R . . C2 C 0.0163(4) 0.3150(4) 0.4196(3) 0.0275(8) Uani 1 1 d . . . H2A H -0.0546 0.3718 0.4226 0.033 Uiso 1 1 calc R . . C3 C 0.2531(4) 0.2160(4) 0.3543(3) 0.0323(9) Uani 1 1 d . . . H3A H 0.3170 0.1980 0.3097 0.039 Uiso 1 1 calc R . . C4 C 0.3052(4) 0.3481(4) 0.4145(3) 0.0288(8) Uani 1 1 d . . . H4A H 0.3999 0.4062 0.4052 0.035 Uiso 1 1 calc R . . C5 C 0.2819(4) 0.3825(4) 0.5192(3) 0.0345(9) Uani 1 1 d . . . H5A H 0.3100 0.4864 0.5380 0.041 Uiso 1 1 calc R . . H5B H 0.3462 0.3439 0.5711 0.041 Uiso 1 1 calc R . . C6 C 0.1228(4) 0.3212(4) 0.5215(3) 0.0352(9) Uani 1 1 d . . . H6B H 0.1101 0.2246 0.5408 0.042 Uiso 1 1 calc R . . H6A H 0.1007 0.3801 0.5750 0.042 Uiso 1 1 calc R . . C7 C 0.0054(4) 0.0610(4) 0.3489(3) 0.0422(11) Uani 1 1 d . . . H7A H -0.0297 0.0047 0.2796 0.051 Uiso 1 1 calc R . . H7B H -0.0435 0.0054 0.3954 0.051 Uiso 1 1 calc R . . C8 C 0.1687(4) 0.0838(4) 0.3870(3) 0.0372(10) Uani 1 1 d . . . H8A H 0.1952 0.0010 0.3595 0.045 Uiso 1 1 calc R . . H8B H 0.1964 0.0917 0.4631 0.045 Uiso 1 1 calc R . . C9 C -0.1735(4) 0.4313(4) 0.2251(3) 0.0249(8) Uani 1 1 d . . . H9A H -0.2315 0.3467 0.2405 0.030 Uiso 1 1 calc R . . C10 C -0.2237(4) 0.5479(3) 0.2022(3) 0.0245(8) Uani 1 1 d . . . H10A H -0.3183 0.5590 0.1989 0.029 Uiso 1 1 calc R . . C11 C -0.1057(4) 0.6438(3) 0.1856(2) 0.0217(7) Uani 1 1 d . . . H11A H -0.1041 0.7362 0.1690 0.026 Uiso 1 1 calc R . . C12 C 0.3190(4) 0.3627(3) 0.1476(3) 0.0242(8) Uani 1 1 d . . . H12A H 0.3445 0.2791 0.1653 0.029 Uiso 1 1 calc R . . C13 C 0.3521(4) 0.4309(3) 0.0670(3) 0.0255(8) Uani 1 1 d . . . H13A H 0.4030 0.4048 0.0202 0.031 Uiso 1 1 calc R . . C14 C 0.2954(3) 0.5446(3) 0.0692(3) 0.0222(8) Uani 1 1 d . . . H14A H 0.3006 0.6131 0.0232 0.027 Uiso 1 1 calc R . . C15 C 0.2376(4) 0.9227(4) 0.0217(3) 0.0334(9) Uani 1 1 d . . . H15A H 0.2991 1.0016 0.0024 0.040 Uiso 1 1 calc R . . C16 C 0.0975(4) 0.8500(4) -0.0366(3) 0.0350(9) Uani 1 1 d . . . H16A H 0.0461 0.8677 -0.1012 0.042 Uiso 1 1 calc R . . C17 C 0.0503(4) 0.7471(4) 0.0202(3) 0.0268(8) Uani 1 1 d . . . H17A H -0.0421 0.6782 0.0010 0.032 Uiso 1 1 calc R . . C18 C 0.4488(4) 0.8391(3) 0.4163(3) 0.0279(8) Uani 1 1 d . . . H18A H 0.5445 0.8958 0.4510 0.034 Uiso 1 1 calc R . . C19 C 0.3441(4) 0.7762(4) 0.4658(3) 0.0306(9) Uani 1 1 d . . . H19A H 0.3533 0.7801 0.5377 0.037 Uiso 1 1 calc R . . C20 C 0.2247(4) 0.7075(3) 0.3868(3) 0.0246(8) Uani 1 1 d . . . H20A H 0.1337 0.6537 0.3950 0.030 Uiso 1 1 calc R . . B1 B 0.1636(4) 0.6540(4) 0.1876(3) 0.0180(8) 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 0.01780(14) 0.01902(14) 0.02290(15) 0.00834(11) 0.00739(11) 0.00588(11) Co1 0.0172(2) 0.0179(2) 0.0283(3) 0.0037(2) 0.0078(2) 0.0025(2) Cl1 0.0220(5) 0.0189(4) 0.0386(5) 0.0018(4) 0.0085(4) 0.0012(4) Cl2 0.0356(6) 0.0322(5) 0.0528(6) 0.0124(5) 0.0248(5) 0.0157(4) N1 0.0158(14) 0.0157(14) 0.0248(16) 0.0061(11) 0.0025(12) 0.0009(11) N2 0.0171(14) 0.0174(14) 0.0214(15) 0.0070(12) 0.0045(12) 0.0040(12) N3 0.0218(16) 0.0232(15) 0.0244(16) 0.0050(12) 0.0068(13) 0.0092(13) N4 0.0157(14) 0.0173(14) 0.0217(15) 0.0050(12) 0.0072(12) 0.0011(11) N5 0.0204(15) 0.0145(14) 0.0296(17) 0.0085(12) 0.0060(13) 0.0007(12) N6 0.0169(14) 0.0144(14) 0.0242(16) 0.0075(11) 0.0040(12) -0.0003(11) N7 0.0156(15) 0.0208(15) 0.0245(16) 0.0005(12) 0.0024(12) 0.0007(12) N8 0.0156(14) 0.0172(14) 0.0177(15) 0.0008(11) 0.0040(12) 0.0005(11) C1 0.0178(19) 0.029(2) 0.041(2) 0.0177(18) 0.0071(17) 0.0000(16) C2 0.024(2) 0.036(2) 0.034(2) 0.0191(17) 0.0190(17) 0.0129(17) C3 0.028(2) 0.042(2) 0.038(2) 0.0200(19) 0.0125(18) 0.0235(19) C4 0.0182(19) 0.038(2) 0.033(2) 0.0180(17) 0.0060(16) 0.0097(16) C5 0.037(2) 0.034(2) 0.029(2) 0.0098(17) 0.0035(18) 0.0072(18) C6 0.045(3) 0.041(2) 0.028(2) 0.0141(17) 0.0146(19) 0.018(2) C7 0.045(3) 0.025(2) 0.050(3) 0.0165(19) 0.002(2) 0.0040(19) C8 0.044(3) 0.027(2) 0.046(3) 0.0158(18) 0.010(2) 0.0177(19) C9 0.0190(18) 0.0238(19) 0.031(2) 0.0116(15) 0.0078(16) 0.0000(15) C10 0.0186(18) 0.030(2) 0.026(2) 0.0098(16) 0.0056(15) 0.0068(16) C11 0.0225(18) 0.0197(17) 0.024(2) 0.0051(15) 0.0051(15) 0.0081(15) C12 0.0229(19) 0.0225(18) 0.031(2) 0.0029(15) 0.0094(16) 0.0102(15) C13 0.0228(19) 0.0274(19) 0.027(2) -0.0007(16) 0.0106(16) 0.0053(16) C14 0.0202(18) 0.0229(18) 0.0208(18) 0.0019(14) 0.0078(15) -0.0010(15) C15 0.040(2) 0.027(2) 0.030(2) 0.0156(17) 0.0093(18) 0.0005(18) C16 0.035(2) 0.040(2) 0.024(2) 0.0148(17) 0.0010(17) 0.0021(18) C17 0.0227(19) 0.0250(19) 0.026(2) 0.0059(15) -0.0012(15) 0.0003(15) C18 0.029(2) 0.0234(19) 0.025(2) 0.0010(15) -0.0029(16) 0.0048(16) C19 0.043(2) 0.027(2) 0.020(2) 0.0011(16) 0.0080(18) 0.0066(18) C20 0.033(2) 0.0216(18) 0.0213(19) 0.0073(15) 0.0116(16) 0.0054(16) B1 0.0146(19) 0.0189(19) 0.020(2) 0.0058(15) 0.0066(16) 0.0006(15) _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 N3 2.086(3) . ? Rh1 N1 2.105(3) . ? Rh1 C4 2.117(3) . ? Rh1 C1 2.129(3) . ? Rh1 C2 2.146(3) . ? Rh1 C3 2.148(3) . ? Co1 N7 2.001(3) . ? Co1 N5 2.008(3) . ? Co1 Cl2 2.2155(10) . ? Co1 Cl1 2.2330(9) . ? N1 C9 1.339(4) . ? N1 N2 1.382(3) . ? N2 C11 1.355(4) . ? N2 B1 1.536(4) . ? N3 C12 1.334(4) . ? N3 N4 1.371(4) . ? N4 C14 1.354(4) . ? N4 B1 1.537(4) . ? N5 C15 1.323(4) . ? N5 N6 1.376(3) . ? N6 C17 1.343(4) . ? N6 B1 1.549(4) . ? N7 C18 1.331(4) . ? N7 N8 1.378(3) . ? N8 C20 1.348(4) . ? N8 B1 1.542(4) . ? C1 C2 1.400(5) . ? C1 C7 1.510(5) . ? C1 H1A 1.0000 . ? C2 C6 1.505(5) . ? C2 H2A 1.0000 . ? C3 C4 1.392(5) . ? C3 C8 1.513(5) . ? C3 H3A 1.0000 . ? C4 C5 1.512(5) . ? C4 H4A 1.0000 . ? C5 C6 1.530(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6B 0.9900 . ? C6 H6A 0.9900 . ? C7 C8 1.512(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.386(4) . ? C9 H9A 0.9500 . ? C10 C11 1.371(4) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 C13 1.378(5) . ? C12 H12A 0.9500 . ? C13 C14 1.370(4) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.390(5) . ? C15 H15A 0.9500 . ? C16 C17 1.369(5) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.393(5) . ? C18 H18A 0.9500 . ? C19 C20 1.370(5) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? 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 Rh1 N1 87.64(10) . . ? N3 Rh1 C4 93.03(12) . . ? N1 Rh1 C4 151.82(12) . . ? N3 Rh1 C1 154.47(13) . . ? N1 Rh1 C1 93.55(12) . . ? C4 Rh1 C1 97.68(14) . . ? N3 Rh1 C2 167.28(12) . . ? N1 Rh1 C2 91.94(12) . . ? C4 Rh1 C2 81.39(14) . . ? C1 Rh1 C2 38.24(13) . . ? N3 Rh1 C3 93.60(12) . . ? N1 Rh1 C3 169.99(12) . . ? C4 Rh1 C3 38.09(13) . . ? C1 Rh1 C3 81.08(14) . . ? C2 Rh1 C3 89.03(14) . . ? N7 Co1 N5 93.88(11) . . ? N7 Co1 Cl2 116.82(8) . . ? N5 Co1 Cl2 115.09(8) . . ? N7 Co1 Cl1 110.82(8) . . ? N5 Co1 Cl1 107.31(8) . . ? Cl2 Co1 Cl1 111.47(4) . . ? C9 N1 N2 105.4(3) . . ? C9 N1 Rh1 128.7(2) . . ? N2 N1 Rh1 121.99(19) . . ? C11 N2 N1 108.9(2) . . ? C11 N2 B1 128.4(3) . . ? N1 N2 B1 122.6(3) . . ? C12 N3 N4 106.0(3) . . ? C12 N3 Rh1 128.5(2) . . ? N4 N3 Rh1 122.66(19) . . ? C14 N4 N3 108.9(3) . . ? C14 N4 B1 128.7(3) . . ? N3 N4 B1 122.1(2) . . ? C15 N5 N6 106.2(3) . . ? C15 N5 Co1 127.5(2) . . ? N6 N5 Co1 125.5(2) . . ? C17 N6 N5 108.8(3) . . ? C17 N6 B1 128.5(3) . . ? N5 N6 B1 121.5(3) . . ? C18 N7 N8 106.1(3) . . ? C18 N7 Co1 128.7(2) . . ? N8 N7 Co1 122.1(2) . . ? C20 N8 N7 108.6(3) . . ? C20 N8 B1 128.0(3) . . ? N7 N8 B1 122.6(2) . . ? C2 C1 C7 125.1(3) . . ? C2 C1 Rh1 71.53(18) . . ? C7 C1 Rh1 109.9(2) . . ? C2 C1 H1A 114.1 . . ? C7 C1 H1A 114.1 . . ? Rh1 C1 H1A 114.1 . . ? C1 C2 C6 124.5(3) . . ? C1 C2 Rh1 70.23(19) . . ? C6 C2 Rh1 112.9(2) . . ? C1 C2 H2A 113.8 . . ? C6 C2 H2A 113.8 . . ? Rh1 C2 H2A 113.8 . . ? C4 C3 C8 124.3(3) . . ? C4 C3 Rh1 69.8(2) . . ? C8 C3 Rh1 113.3(2) . . ? C4 C3 H3A 113.9 . . ? C8 C3 H3A 113.9 . . ? Rh1 C3 H3A 113.9 . . ? C3 C4 C5 125.7(3) . . ? C3 C4 Rh1 72.2(2) . . ? C5 C4 Rh1 110.4(2) . . ? C3 C4 H4A 113.7 . . ? C5 C4 H4A 113.7 . . ? Rh1 C4 H4A 113.7 . . ? C4 C5 C6 112.1(3) . . ? C4 C5 H5A 109.2 . . ? C6 C5 H5A 109.2 . . ? C4 C5 H5B 109.2 . . ? C6 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C2 C6 C5 112.5(3) . . ? C2 C6 H6B 109.1 . . ? C5 C6 H6B 109.1 . . ? C2 C6 H6A 109.1 . . ? C5 C6 H6A 109.1 . . ? H6B C6 H6A 107.8 . . ? C1 C7 C8 113.4(3) . . ? C1 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? C1 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C7 C8 C3 111.6(3) . . ? C7 C8 H8A 109.3 . . ? C3 C8 H8A 109.3 . . ? C7 C8 H8B 109.3 . . ? C3 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? N1 C9 C10 111.9(3) . . ? N1 C9 H9A 124.0 . . ? C10 C9 H9A 124.0 . . ? C11 C10 C9 104.4(3) . . ? C11 C10 H10A 127.8 . . ? C9 C10 H10A 127.8 . . ? N2 C11 C10 109.4(3) . . ? N2 C11 H11A 125.3 . . ? C10 C11 H11A 125.3 . . ? N3 C12 C13 111.4(3) . . ? N3 C12 H12A 124.3 . . ? C13 C12 H12A 124.3 . . ? C14 C13 C12 104.9(3) . . ? C14 C13 H13A 127.5 . . ? C12 C13 H13A 127.5 . . ? N4 C14 C13 108.8(3) . . ? N4 C14 H14A 125.6 . . ? C13 C14 H14A 125.6 . . ? N5 C15 C16 111.3(3) . . ? N5 C15 H15A 124.3 . . ? C16 C15 H15A 124.3 . . ? C17 C16 C15 104.3(3) . . ? C17 C16 H16A 127.9 . . ? C15 C16 H16A 127.9 . . ? N6 C17 C16 109.3(3) . . ? N6 C17 H17A 125.3 . . ? C16 C17 H17A 125.3 . . ? N7 C18 C19 111.5(3) . . ? N7 C18 H18A 124.3 . . ? C19 C18 H18A 124.3 . . ? C20 C19 C18 104.0(3) . . ? C20 C19 H19A 128.0 . . ? C18 C19 H19A 128.0 . . ? N8 C20 C19 109.8(3) . . ? N8 C20 H20A 125.1 . . ? C19 C20 H20A 125.1 . . ? N2 B1 N4 111.5(3) . . ? N2 B1 N8 107.1(3) . . ? N4 B1 N8 110.6(3) . . ? N2 B1 N6 108.5(3) . . ? N4 B1 N6 106.7(3) . . ? N8 B1 N6 112.5(3) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.507 _refine_diff_density_min -0.505 _refine_diff_density_rms 0.098 data_11 _database_code_depnum_ccdc_archive 'CCDC 768033' #TrackingRef '- Hallett_Dalton_Cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H20 B Cl2 Co N8 Rh, C H2 Cl2' _chemical_formula_sum 'C20 H22 B Cl4 Co N8 Rh' _chemical_formula_weight 688.91 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' B B 0.0013 0.0007 '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' Cl Cl 0.1484 0.1585 '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' Co Co 0.3494 0.9721 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.218(2) _cell_length_b 19.578(4) _cell_length_c 12.041(2) _cell_angle_alpha 90.00 _cell_angle_beta 116.14(3) _cell_angle_gamma 90.00 _cell_volume 2585.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 144 _cell_measurement_theta_min 2.8075 _cell_measurement_theta_max 24.5315 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.770 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1372 _exptl_absorpt_coefficient_mu 1.720 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.785 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details XPREP _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 '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29115 _diffrn_reflns_av_R_equivalents 0.0720 _diffrn_reflns_av_sigmaI/netI 0.0821 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5926 _reflns_number_gt 4387 _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^)+(0.0240P)^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 5926 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0764 _refine_ls_wR_factor_gt 0.0718 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _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 0.71382(3) 0.631587(15) 0.25255(3) 0.01110(8) Uani 1 1 d . . . Co1 Co 0.76530(5) 0.54635(3) 0.78677(5) 0.01184(12) Uani 1 1 d . . . Cl1 Cl 0.89178(8) 0.62898(5) 0.89880(9) 0.0173(2) Uani 1 1 d . . . Cl2 Cl 0.67920(9) 0.48418(5) 0.88366(9) 0.0190(2) Uani 1 1 d . . . Cl3 Cl 0.28725(13) 0.71480(7) 0.19710(12) 0.0488(4) Uani 1 1 d . . . Cl4 Cl 0.18990(12) 0.75143(7) -0.06361(12) 0.0477(4) Uani 1 1 d . . . N1 N 0.7089(3) 0.52649(16) 0.2767(3) 0.0151(7) Uani 1 1 d . . . N2 N 0.7417(3) 0.49245(15) 0.3855(3) 0.0117(7) Uani 1 1 d . . . N3 N 0.8310(3) 0.64252(15) 0.4380(3) 0.0125(7) Uani 1 1 d . . . N4 N 0.8598(3) 0.59217(15) 0.5260(3) 0.0109(7) Uani 1 1 d . . . N5 N 0.8538(3) 0.48066(16) 0.7283(3) 0.0141(7) Uani 1 1 d . . . N6 N 0.8514(3) 0.47929(15) 0.6132(3) 0.0114(7) Uani 1 1 d . . . N7 N 0.6489(3) 0.57503(15) 0.6174(3) 0.0117(7) Uani 1 1 d . . . N8 N 0.6562(3) 0.55297(15) 0.5126(3) 0.0106(7) Uani 1 1 d . . . C1 C 0.6559(3) 0.6288(2) 0.0591(3) 0.0167(9) Uani 1 1 d . . . H1A H 0.6640 0.5875 0.0144 0.020 Uiso 1 1 calc R . . C2 C 0.5566(3) 0.6404(2) 0.0834(3) 0.0191(9) Uani 1 1 d . . . H2A H 0.4862 0.6082 0.0575 0.023 Uiso 1 1 calc R . . C3 C 0.7550(3) 0.72322(18) 0.1837(3) 0.0131(8) Uani 1 1 d . . . H3A H 0.8339 0.7483 0.2273 0.016 Uiso 1 1 calc R . . C4 C 0.6556(4) 0.7344(2) 0.2067(4) 0.0178(9) Uani 1 1 d . . . H4A H 0.6553 0.7684 0.2685 0.021 Uiso 1 1 calc R . . C5 C 0.5423(4) 0.7183(2) 0.0849(4) 0.0199(9) Uani 1 1 d . . . H5A H 0.4621 0.7364 0.0753 0.024 Uiso 1 1 calc R . . C6 C 0.7050(3) 0.69934(19) 0.0488(4) 0.0153(9) Uani 1 1 d . . . H6A H 0.7613 0.7017 0.0088 0.018 Uiso 1 1 calc R . . C7 C 0.5862(4) 0.7408(2) -0.0111(4) 0.0201(9) Uani 1 1 d . . . H7A H 0.5316 0.7253 -0.0960 0.024 Uiso 1 1 calc R . . H7B H 0.6003 0.7906 -0.0102 0.024 Uiso 1 1 calc R . . C8 C 0.9136(3) 0.6920(2) 0.4911(4) 0.0155(9) Uani 1 1 d . . . H8A H 0.9166 0.7333 0.4513 0.019 Uiso 1 1 calc R . . C9 C 0.9940(3) 0.6751(2) 0.6115(4) 0.0172(9) Uani 1 1 d . . . H9A H 1.0602 0.7015 0.6685 0.021 Uiso 1 1 calc R . . C10 C 0.9569(3) 0.61217(19) 0.6301(3) 0.0139(8) Uani 1 1 d . . . H10A H 0.9937 0.5865 0.7045 0.017 Uiso 1 1 calc R . . C11 C 0.6681(4) 0.4790(2) 0.1882(4) 0.0195(9) Uani 1 1 d . . . H11A H 0.6385 0.4883 0.1023 0.023 Uiso 1 1 calc R . . C12 C 0.6745(3) 0.4144(2) 0.2382(4) 0.0184(9) Uani 1 1 d . . . H12A H 0.6522 0.3721 0.1953 0.022 Uiso 1 1 calc R . . C13 C 0.7203(3) 0.4251(2) 0.3630(4) 0.0170(9) Uani 1 1 d . . . H13A H 0.7346 0.3908 0.4236 0.020 Uiso 1 1 calc R . . C14 C 0.5342(3) 0.59705(18) 0.5800(4) 0.0137(8) Uani 1 1 d . . . H14A H 0.5032 0.6152 0.6337 0.016 Uiso 1 1 calc R . . C15 C 0.4667(3) 0.59002(19) 0.4538(4) 0.0144(9) Uani 1 1 d . . . H15A H 0.3836 0.6018 0.4054 0.017 Uiso 1 1 calc R . . C16 C 0.5467(3) 0.56213(18) 0.4135(4) 0.0131(8) Uani 1 1 d . . . H16A H 0.5281 0.5512 0.3302 0.016 Uiso 1 1 calc R . . C17 C 0.9436(3) 0.4388(2) 0.7992(4) 0.0185(9) Uani 1 1 d . . . H17A H 0.9655 0.4297 0.8838 0.022 Uiso 1 1 calc R . . C18 C 1.0007(4) 0.4106(2) 0.7333(4) 0.0200(9) Uani 1 1 d . . . H18A H 1.0667 0.3792 0.7621 0.024 Uiso 1 1 calc R . . C19 C 0.9416(3) 0.4379(2) 0.6182(4) 0.0173(9) Uani 1 1 d . . . H19A H 0.9609 0.4291 0.5513 0.021 Uiso 1 1 calc R . . C20 C 0.2023(4) 0.6858(3) 0.0417(5) 0.0470(15) Uani 1 1 d . . . H20A H 0.2434 0.6458 0.0267 0.056 Uiso 1 1 calc R . . H20B H 0.1198 0.6715 0.0289 0.056 Uiso 1 1 calc R . . B1 B 0.7770(4) 0.5297(2) 0.5099(4) 0.0115(9) 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 0.01406(15) 0.00924(15) 0.01098(16) 0.00014(13) 0.00643(12) -0.00054(13) Co1 0.0137(3) 0.0120(3) 0.0108(3) -0.0007(2) 0.0063(2) -0.0005(2) Cl1 0.0197(5) 0.0135(5) 0.0154(5) -0.0010(4) 0.0046(4) -0.0009(4) Cl2 0.0272(6) 0.0181(5) 0.0172(5) -0.0019(4) 0.0149(5) -0.0042(4) Cl3 0.0590(9) 0.0502(9) 0.0373(8) 0.0054(7) 0.0212(7) 0.0076(7) Cl4 0.0505(8) 0.0525(9) 0.0329(8) 0.0029(6) 0.0119(7) -0.0034(7) N1 0.0195(18) 0.0167(18) 0.0108(18) 0.0002(14) 0.0081(15) -0.0029(14) N2 0.0159(17) 0.0094(16) 0.0112(17) 0.0010(13) 0.0072(14) -0.0001(13) N3 0.0150(17) 0.0071(17) 0.0169(18) 0.0013(13) 0.0084(14) 0.0011(13) N4 0.0140(17) 0.0105(17) 0.0090(17) 0.0010(13) 0.0058(14) 0.0015(13) N5 0.0175(17) 0.0153(18) 0.0117(18) 0.0009(14) 0.0085(14) 0.0017(14) N6 0.0120(16) 0.0130(17) 0.0117(17) 0.0009(13) 0.0075(14) 0.0010(13) N7 0.0137(16) 0.0103(16) 0.0134(18) -0.0011(13) 0.0080(14) -0.0003(13) N8 0.0108(16) 0.0109(16) 0.0092(17) 0.0005(13) 0.0036(13) -0.0014(13) C1 0.028(2) 0.0100(19) 0.011(2) -0.0016(17) 0.0081(18) -0.0001(18) C2 0.019(2) 0.022(2) 0.012(2) -0.0023(18) 0.0041(17) -0.0072(18) C3 0.018(2) 0.0064(19) 0.014(2) 0.0025(16) 0.0060(17) -0.0006(16) C4 0.025(2) 0.013(2) 0.015(2) -0.0027(17) 0.0081(19) 0.0062(18) C5 0.014(2) 0.028(2) 0.018(2) 0.0044(19) 0.0070(18) 0.0095(18) C6 0.020(2) 0.015(2) 0.017(2) 0.0011(17) 0.0130(18) -0.0006(17) C7 0.029(2) 0.020(2) 0.014(2) 0.0042(18) 0.0114(19) 0.0044(19) C8 0.018(2) 0.012(2) 0.020(2) -0.0001(17) 0.0115(18) 0.0010(17) C9 0.017(2) 0.017(2) 0.020(2) -0.0033(17) 0.0099(18) -0.0054(17) C10 0.013(2) 0.020(2) 0.008(2) 0.0002(16) 0.0038(16) -0.0002(16) C11 0.028(2) 0.019(2) 0.011(2) -0.0023(17) 0.0081(19) -0.0053(19) C12 0.024(2) 0.013(2) 0.019(2) -0.0021(17) 0.0109(19) -0.0025(17) C13 0.020(2) 0.013(2) 0.023(2) 0.0028(18) 0.0142(19) -0.0008(17) C14 0.014(2) 0.0066(19) 0.024(2) 0.0030(16) 0.0125(18) 0.0006(16) C15 0.0098(19) 0.012(2) 0.019(2) 0.0060(17) 0.0044(17) 0.0013(16) C16 0.015(2) 0.0078(19) 0.013(2) 0.0025(16) 0.0032(17) -0.0031(16) C17 0.021(2) 0.022(2) 0.010(2) 0.0064(17) 0.0057(18) 0.0049(18) C18 0.021(2) 0.020(2) 0.021(2) 0.0047(18) 0.0103(19) 0.0083(18) C19 0.019(2) 0.020(2) 0.018(2) 0.0021(18) 0.0120(18) 0.0069(17) C20 0.037(3) 0.036(3) 0.052(4) 0.017(3) 0.006(3) 0.000(3) B1 0.014(2) 0.012(2) 0.010(2) -0.0015(18) 0.0070(18) -0.0001(18) _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 N3 2.065(3) . ? Rh1 N1 2.083(3) . ? Rh1 C2 2.102(4) . ? Rh1 C1 2.116(4) . ? Rh1 C4 2.124(4) . ? Rh1 C3 2.128(4) . ? Co1 N7 1.985(3) . ? Co1 N5 1.997(3) . ? Co1 Cl1 2.2334(12) . ? Co1 Cl2 2.2429(11) . ? Cl3 C20 1.786(5) . ? Cl4 C20 1.764(5) . ? N1 C11 1.334(5) . ? N1 N2 1.363(4) . ? N2 C13 1.348(5) . ? N2 B1 1.547(5) . ? N3 C8 1.340(5) . ? N3 N4 1.375(4) . ? N4 C10 1.350(4) . ? N4 B1 1.543(5) . ? N5 C17 1.333(5) . ? N5 N6 1.374(4) . ? N6 C19 1.348(4) . ? N6 B1 1.534(5) . ? N7 C14 1.340(4) . ? N7 N8 1.374(4) . ? N8 C16 1.356(4) . ? N8 B1 1.558(5) . ? C1 C2 1.386(5) . ? C1 C6 1.532(5) . ? C1 H1A 1.0000 . ? C2 C5 1.536(5) . ? C2 H2A 1.0000 . ? C3 C4 1.377(5) . ? C3 C6 1.535(5) . ? C3 H3A 1.0000 . ? C4 C5 1.541(5) . ? C4 H4A 1.0000 . ? C5 C7 1.537(5) . ? C5 H5A 1.0000 . ? C6 C7 1.537(5) . ? C6 H6A 1.0000 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.386(5) . ? C8 H8A 0.9500 . ? C9 C10 1.365(5) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 C12 1.389(5) . ? C11 H11A 0.9500 . ? C12 C13 1.369(5) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.379(5) . ? C14 H14A 0.9500 . ? C15 C16 1.380(5) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 C18 1.381(5) . ? C17 H17A 0.9500 . ? C18 C19 1.358(5) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 H20A 0.9900 . ? C20 H20B 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 N3 Rh1 N1 90.00(12) . . ? N3 Rh1 C2 160.27(14) . . ? N1 Rh1 C2 98.43(14) . . ? N3 Rh1 C1 158.31(13) . . ? N1 Rh1 C1 96.44(14) . . ? C2 Rh1 C1 38.37(14) . . ? N3 Rh1 C4 100.15(13) . . ? N1 Rh1 C4 160.92(14) . . ? C2 Rh1 C4 67.16(15) . . ? C1 Rh1 C4 80.04(15) . . ? N3 Rh1 C3 99.41(13) . . ? N1 Rh1 C3 156.03(13) . . ? C2 Rh1 C3 79.93(15) . . ? C1 Rh1 C3 67.33(15) . . ? C4 Rh1 C3 37.80(14) . . ? N7 Co1 N5 94.26(13) . . ? N7 Co1 Cl1 114.04(10) . . ? N5 Co1 Cl1 109.97(10) . . ? N7 Co1 Cl2 113.57(9) . . ? N5 Co1 Cl2 106.53(10) . . ? Cl1 Co1 Cl2 115.93(4) . . ? C11 N1 N2 106.0(3) . . ? C11 N1 Rh1 126.9(3) . . ? N2 N1 Rh1 127.1(2) . . ? C13 N2 N1 109.6(3) . . ? C13 N2 B1 127.1(3) . . ? N1 N2 B1 122.6(3) . . ? C8 N3 N4 105.5(3) . . ? C8 N3 Rh1 127.5(3) . . ? N4 N3 Rh1 125.4(2) . . ? C10 N4 N3 109.2(3) . . ? C10 N4 B1 127.3(3) . . ? N3 N4 B1 122.7(3) . . ? C17 N5 N6 106.2(3) . . ? C17 N5 Co1 126.2(3) . . ? N6 N5 Co1 126.4(2) . . ? C19 N6 N5 108.3(3) . . ? C19 N6 B1 127.2(3) . . ? N5 N6 B1 123.2(3) . . ? C14 N7 N8 105.9(3) . . ? C14 N7 Co1 127.3(3) . . ? N8 N7 Co1 123.2(2) . . ? C16 N8 N7 109.2(3) . . ? C16 N8 B1 126.6(3) . . ? N7 N8 B1 123.8(3) . . ? C2 C1 C6 106.2(3) . . ? C2 C1 Rh1 70.3(2) . . ? C6 C1 Rh1 96.5(2) . . ? C2 C1 H1A 123.3 . . ? C6 C1 H1A 123.3 . . ? Rh1 C1 H1A 123.3 . . ? C1 C2 C5 106.3(3) . . ? C1 C2 Rh1 71.3(2) . . ? C5 C2 Rh1 97.5(2) . . ? C1 C2 H2A 122.9 . . ? C5 C2 H2A 122.9 . . ? Rh1 C2 H2A 122.9 . . ? C4 C3 C6 106.6(3) . . ? C4 C3 Rh1 71.0(2) . . ? C6 C3 Rh1 95.9(2) . . ? C4 C3 H3A 123.2 . . ? C6 C3 H3A 123.2 . . ? Rh1 C3 H3A 123.2 . . ? C3 C4 C5 106.2(3) . . ? C3 C4 Rh1 71.2(2) . . ? C5 C4 Rh1 96.4(2) . . ? C3 C4 H4A 123.2 . . ? C5 C4 H4A 123.2 . . ? Rh1 C4 H4A 123.2 . . ? C2 C5 C7 101.3(3) . . ? C2 C5 C4 98.9(3) . . ? C7 C5 C4 101.1(3) . . ? C2 C5 H5A 117.5 . . ? C7 C5 H5A 117.5 . . ? C4 C5 H5A 117.5 . . ? C1 C6 C3 100.2(3) . . ? C1 C6 C7 101.0(3) . . ? C3 C6 C7 100.9(3) . . ? C1 C6 H6A 117.2 . . ? C3 C6 H6A 117.2 . . ? C7 C6 H6A 117.2 . . ? C6 C7 C5 93.8(3) . . ? C6 C7 H7A 113.0 . . ? C5 C7 H7A 113.0 . . ? C6 C7 H7B 113.0 . . ? C5 C7 H7B 113.0 . . ? H7A C7 H7B 110.4 . . ? N3 C8 C9 111.4(4) . . ? N3 C8 H8A 124.3 . . ? C9 C8 H8A 124.3 . . ? C10 C9 C8 104.7(3) . . ? C10 C9 H9A 127.7 . . ? C8 C9 H9A 127.7 . . ? N4 C10 C9 109.2(3) . . ? N4 C10 H10A 125.4 . . ? C9 C10 H10A 125.4 . . ? N1 C11 C12 111.0(4) . . ? N1 C11 H11A 124.5 . . ? C12 C11 H11A 124.5 . . ? C13 C12 C11 104.7(4) . . ? C13 C12 H12A 127.6 . . ? C11 C12 H12A 127.6 . . ? N2 C13 C12 108.7(4) . . ? N2 C13 H13A 125.7 . . ? C12 C13 H13A 125.7 . . ? N7 C14 C15 111.5(3) . . ? N7 C14 H14A 124.2 . . ? C15 C14 H14A 124.2 . . ? C14 C15 C16 104.8(3) . . ? C14 C15 H15A 127.6 . . ? C16 C15 H15A 127.6 . . ? N8 C16 C15 108.6(3) . . ? N8 C16 H16A 125.7 . . ? C15 C16 H16A 125.7 . . ? N5 C17 C18 111.1(4) . . ? N5 C17 H17A 124.4 . . ? C18 C17 H17A 124.4 . . ? C19 C18 C17 104.6(3) . . ? C19 C18 H18A 127.7 . . ? C17 C18 H18A 127.7 . . ? N6 C19 C18 109.8(3) . . ? N6 C19 H19A 125.1 . . ? C18 C19 H19A 125.1 . . ? Cl4 C20 Cl3 110.3(3) . . ? Cl4 C20 H20A 109.6 . . ? Cl3 C20 H20A 109.6 . . ? Cl4 C20 H20B 109.6 . . ? Cl3 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? N6 B1 N4 106.6(3) . . ? N6 B1 N2 107.1(3) . . ? N4 B1 N2 112.5(3) . . ? N6 B1 N8 113.5(3) . . ? N4 B1 N8 109.9(3) . . ? N2 B1 N8 107.2(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.758 _refine_diff_density_min -0.873 _refine_diff_density_rms 0.113 data_14 _database_code_depnum_ccdc_archive 'CCDC 768034' #TrackingRef '- Hallett_Dalton_Cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 B Cl2 N8 Rh Zn, C H2 Cl2' _chemical_formula_sum 'C21 H26 B Cl4 N8 Rh Zn' _chemical_formula_weight 711.39 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' B B 0.0013 0.0007 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.9430(19) _cell_length_b 19.687(3) _cell_length_c 12.1521(18) _cell_angle_alpha 90.00 _cell_angle_beta 117.538(11) _cell_angle_gamma 90.00 _cell_volume 2745.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 258 _cell_measurement_theta_min 2.8035 _cell_measurement_theta_max 26.6695 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 1.891 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.616 _exptl_absorpt_correction_T_max 0.715 _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 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18789 _diffrn_reflns_av_R_equivalents 0.0657 _diffrn_reflns_av_sigmaI/netI 0.0766 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5881 _reflns_number_gt 3771 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT (Bruker, 1998)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 1998)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _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^)+(0.0363P)^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 5881 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0866 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 0.927 _refine_ls_shift/su_max 0.004 _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 0.20679(2) 0.121422(13) 0.46363(3) 0.01943(9) Uani 1 1 d . . . Zn1 Zn 0.27875(4) 0.04809(2) -0.00607(5) 0.02389(12) Uani 1 1 d . . . Cl1 Cl 0.20002(9) -0.01297(5) -0.17977(11) 0.0344(3) Uani 1 1 d . . . Cl2 Cl 0.38664(10) 0.13492(4) -0.00901(13) 0.0415(3) Uani 1 1 d . . . Cl3 Cl 0.75658(11) 0.28838(6) 0.51275(15) 0.0574(4) Uani 1 1 d . . . Cl4 Cl 0.67372(11) 0.25736(6) 0.69445(15) 0.0546(4) Uani 1 1 d . . . N1 N 0.2309(3) 0.01605(14) 0.4555(3) 0.0237(8) Uani 1 1 d . . . N2 N 0.2517(3) -0.01404(14) 0.3661(3) 0.0233(8) Uani 1 1 d . . . N3 N 0.3322(3) 0.13662(13) 0.4034(3) 0.0223(8) Uani 1 1 d . . . N4 N 0.3606(3) 0.08788(14) 0.3401(3) 0.0216(7) Uani 1 1 d . . . N5 N 0.3694(3) -0.01669(14) 0.1368(3) 0.0245(8) Uani 1 1 d . . . N6 N 0.3607(3) -0.02237(14) 0.2429(3) 0.0228(8) Uani 1 1 d . . . N7 N 0.1647(3) 0.07391(14) 0.0570(4) 0.0259(8) Uani 1 1 d . . . N8 N 0.1693(2) 0.04627(14) 0.1624(3) 0.0205(7) Uani 1 1 d . . . C1 C 0.1102(4) 0.11051(18) 0.5669(5) 0.0281(10) Uani 1 1 d . . . H1A H 0.1252 0.0668 0.6139 0.034 Uiso 1 1 calc R . . C2 C 0.0363(3) 0.10432(17) 0.4416(4) 0.0250(10) Uani 1 1 d . . . H2A H 0.0077 0.0569 0.4154 0.030 Uiso 1 1 calc R . . C4 C 0.1407(3) 0.22197(17) 0.4111(5) 0.0304(11) Uani 1 1 d . . . H3A H 0.1661 0.2450 0.3543 0.036 Uiso 1 1 calc R . . C3 C 0.2241(4) 0.22245(18) 0.5364(5) 0.0304(11) Uani 1 1 d . . . H4A H 0.2987 0.2451 0.5518 0.036 Uiso 1 1 calc R . . C5 C 0.1146(4) 0.17259(19) 0.6424(5) 0.0393(12) Uani 1 1 d . . . H5A H 0.0362 0.1934 0.6066 0.047 Uiso 1 1 calc R . . H18B H 0.1355 0.1583 0.7283 0.047 Uiso 1 1 calc R . . C6 C 0.2002(4) 0.2245(2) 0.6462(5) 0.0454(13) Uani 1 1 d . . . H6A H 0.2745 0.2177 0.7227 0.055 Uiso 1 1 calc R . . H6B H 0.1705 0.2702 0.6509 0.055 Uiso 1 1 calc R . . C7 C 0.0111(4) 0.2266(2) 0.3698(6) 0.0503(15) Uani 1 1 d . . . H7A H -0.0014 0.2537 0.4312 0.060 Uiso 1 1 calc R . . H7B H -0.0269 0.2508 0.2894 0.060 Uiso 1 1 calc R . . C8 C -0.0457(4) 0.15879(19) 0.3559(5) 0.0398(12) Uani 1 1 d . . . H8A H -0.0762 0.1436 0.2688 0.048 Uiso 1 1 calc R . . H8B H -0.1128 0.1637 0.3735 0.048 Uiso 1 1 calc R . . C9 C 0.4088(3) 0.18670(18) 0.4269(4) 0.0285(10) Uani 1 1 d . . . H9A H 0.4109 0.2271 0.4706 0.034 Uiso 1 1 calc R . . C10 C 0.4852(4) 0.1722(2) 0.3794(5) 0.0353(11) Uani 1 1 d . . . H10A H 0.5477 0.1996 0.3844 0.042 Uiso 1 1 calc R . . C11 C 0.4516(3) 0.10992(19) 0.3239(5) 0.0310(11) Uani 1 1 d . . . H11A H 0.4863 0.0863 0.2812 0.037 Uiso 1 1 calc R . . C12 C 0.2028(4) -0.03448(18) 0.5107(5) 0.0341(11) Uani 1 1 d . . . H12A H 0.1853 -0.0286 0.5779 0.041 Uiso 1 1 calc R . . C13 C 0.2027(4) -0.0966(2) 0.4564(5) 0.0397(13) Uani 1 1 d . . . H13A H 0.1853 -0.1400 0.4781 0.048 Uiso 1 1 calc R . . C14 C 0.2331(4) -0.08207(18) 0.3648(5) 0.0342(11) Uani 1 1 d . . . H14A H 0.2400 -0.1140 0.3100 0.041 Uiso 1 1 calc R . . C15 C 0.4606(3) -0.05403(19) 0.1507(5) 0.0321(11) Uani 1 1 d . . . H15A H 0.4859 -0.0596 0.0892 0.039 Uiso 1 1 calc R . . C16 C 0.5134(4) -0.0836(2) 0.2672(5) 0.0367(11) Uani 1 1 d . . . H16A H 0.5798 -0.1124 0.3002 0.044 Uiso 1 1 calc R . . C17 C 0.4495(3) -0.06261(19) 0.3251(5) 0.0328(11) Uani 1 1 d . . . H17A H 0.4641 -0.0739 0.4070 0.039 Uiso 1 1 calc R . . C18 C 0.0560(3) 0.09615(18) -0.0114(5) 0.0286(10) Uani 1 1 d . . . H18A H 0.0280 0.1167 -0.0908 0.034 Uiso 1 1 calc R . . C19 C -0.0104(3) 0.08493(19) 0.0500(5) 0.0329(11) Uani 1 1 d . . . H19A H -0.0898 0.0965 0.0223 0.039 Uiso 1 1 calc R . . C20 C 0.0632(3) 0.05384(18) 0.1582(4) 0.0268(10) Uani 1 1 d . . . H20A H 0.0435 0.0397 0.2209 0.032 Uiso 1 1 calc R . . C21 C 0.6723(4) 0.3163(2) 0.5838(5) 0.0456(13) Uani 1 1 d . . . H21A H 0.5909 0.3235 0.5192 0.055 Uiso 1 1 calc R . . H21B H 0.7029 0.3605 0.6251 0.055 Uiso 1 1 calc R . . B1 B 0.2839(4) 0.0248(2) 0.2769(5) 0.0209(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 0.02336(15) 0.01642(14) 0.0218(2) -0.00037(13) 0.01328(14) -0.00079(12) Zn1 0.0280(2) 0.0208(2) 0.0272(3) -0.00021(19) 0.0165(2) -0.00042(17) Cl1 0.0474(6) 0.0315(5) 0.0243(7) -0.0016(5) 0.0166(5) -0.0027(4) Cl2 0.0478(6) 0.0221(5) 0.0743(11) -0.0056(5) 0.0451(7) -0.0055(4) Cl3 0.0528(7) 0.0431(7) 0.0825(13) -0.0134(7) 0.0365(8) -0.0118(5) Cl4 0.0503(7) 0.0467(7) 0.0589(11) 0.0008(6) 0.0186(7) -0.0067(6) N1 0.0315(18) 0.0222(16) 0.025(2) 0.0002(15) 0.0192(17) 0.0034(13) N2 0.0322(18) 0.0199(15) 0.024(2) -0.0004(14) 0.0186(17) 0.0013(13) N3 0.0253(17) 0.0188(15) 0.025(2) -0.0010(13) 0.0139(16) 0.0000(12) N4 0.0200(16) 0.0229(15) 0.023(2) -0.0057(14) 0.0105(15) -0.0026(12) N5 0.0266(17) 0.0243(16) 0.024(2) -0.0024(15) 0.0131(16) 0.0024(13) N6 0.0243(17) 0.0240(16) 0.020(2) 0.0006(14) 0.0099(16) 0.0030(13) N7 0.0250(17) 0.0220(16) 0.032(3) 0.0030(15) 0.0137(17) 0.0019(13) N8 0.0211(16) 0.0206(15) 0.024(2) -0.0060(14) 0.0136(15) -0.0039(12) C1 0.040(2) 0.023(2) 0.035(3) 0.0012(18) 0.028(2) -0.0024(17) C2 0.025(2) 0.0207(18) 0.033(3) -0.0017(17) 0.017(2) -0.0025(15) C4 0.038(2) 0.0164(18) 0.048(4) 0.0088(18) 0.030(2) 0.0036(16) C3 0.041(2) 0.0190(19) 0.041(4) -0.0060(18) 0.028(2) -0.0068(16) C5 0.064(3) 0.032(2) 0.035(3) -0.005(2) 0.034(3) -0.006(2) C6 0.063(3) 0.038(2) 0.048(4) -0.020(2) 0.036(3) -0.015(2) C7 0.037(3) 0.040(3) 0.070(5) 0.028(3) 0.022(3) 0.011(2) C8 0.027(2) 0.036(2) 0.051(4) 0.006(2) 0.012(2) 0.0032(18) C9 0.032(2) 0.0243(19) 0.031(3) -0.0037(19) 0.016(2) -0.0062(16) C10 0.033(2) 0.035(2) 0.047(4) -0.012(2) 0.025(2) -0.0115(18) C11 0.027(2) 0.035(2) 0.038(3) -0.010(2) 0.021(2) -0.0069(17) C12 0.051(3) 0.023(2) 0.045(4) 0.004(2) 0.037(3) 0.0022(18) C13 0.055(3) 0.0231(19) 0.060(4) 0.002(2) 0.043(3) 0.003(2) C14 0.039(2) 0.0194(19) 0.051(4) -0.0069(19) 0.027(2) -0.0015(17) C15 0.032(2) 0.035(2) 0.034(3) -0.009(2) 0.019(2) 0.0081(18) C16 0.033(2) 0.038(2) 0.035(4) -0.001(2) 0.012(2) 0.0169(19) C17 0.033(2) 0.031(2) 0.035(3) 0.002(2) 0.016(2) 0.0075(17) C18 0.032(2) 0.0215(19) 0.031(3) 0.0023(18) 0.014(2) 0.0072(16) C19 0.021(2) 0.031(2) 0.043(4) -0.003(2) 0.012(2) 0.0053(16) C20 0.025(2) 0.026(2) 0.034(3) -0.0078(19) 0.018(2) -0.0028(16) C21 0.037(3) 0.036(2) 0.058(4) 0.001(2) 0.017(3) 0.002(2) B1 0.024(2) 0.021(2) 0.019(3) -0.0036(18) 0.011(2) 0.0018(16) _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 N3 2.087(3) . ? Rh1 N1 2.107(3) . ? Rh1 C2 2.123(4) . ? Rh1 C4 2.134(3) . ? Rh1 C3 2.146(4) . ? Rh1 C1 2.153(4) . ? Zn1 N7 2.018(3) . ? Zn1 N5 2.033(3) . ? Zn1 Cl2 2.2182(10) . ? Zn1 Cl1 2.2249(13) . ? Cl3 C21 1.763(5) . ? Cl4 C21 1.771(5) . ? N1 C12 1.341(5) . ? N1 N2 1.368(4) . ? N2 C14 1.360(4) . ? N2 B1 1.534(5) . ? N3 C9 1.333(4) . ? N3 N4 1.382(4) . ? N4 C11 1.353(5) . ? N4 B1 1.554(5) . ? N5 C15 1.334(4) . ? N5 N6 1.350(5) . ? N6 C17 1.373(5) . ? N6 B1 1.549(5) . ? N7 C18 1.334(5) . ? N7 N8 1.367(5) . ? N8 C20 1.359(4) . ? N8 B1 1.552(6) . ? C1 C2 1.380(6) . ? C1 C5 1.513(5) . ? C1 H1A 1.0000 . ? C2 C8 1.529(6) . ? C2 H2A 1.0000 . ? C4 C3 1.401(7) . ? C4 C7 1.515(6) . ? C4 H3A 1.0000 . ? C3 C6 1.503(6) . ? C3 H4A 1.0000 . ? C5 C6 1.493(5) . ? C5 H5A 0.9900 . ? C5 H18B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.495(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.386(6) . ? C9 H9A 0.9500 . ? C10 C11 1.369(5) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 C13 1.390(6) . ? C12 H12A 0.9500 . ? C13 C14 1.371(6) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.384(7) . ? C15 H15A 0.9500 . ? C16 C17 1.373(6) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.392(6) . ? C18 H18A 0.9500 . ? C19 C20 1.361(6) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 H21A 0.9900 . ? C21 H21B 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 N3 Rh1 N1 88.21(11) . . ? N3 Rh1 C2 155.45(17) . . ? N1 Rh1 C2 90.32(12) . . ? N3 Rh1 C4 91.80(13) . . ? N1 Rh1 C4 161.24(16) . . ? C2 Rh1 C4 81.94(14) . . ? N3 Rh1 C3 93.54(13) . . ? N1 Rh1 C3 160.49(16) . . ? C2 Rh1 C3 95.93(14) . . ? C4 Rh1 C3 38.22(17) . . ? N3 Rh1 C1 166.85(16) . . ? N1 Rh1 C1 93.88(13) . . ? C2 Rh1 C1 37.64(17) . . ? C4 Rh1 C1 90.37(15) . . ? C3 Rh1 C1 80.23(15) . . ? N7 Zn1 N5 93.91(13) . . ? N7 Zn1 Cl2 112.87(9) . . ? N5 Zn1 Cl2 112.22(9) . . ? N7 Zn1 Cl1 113.70(10) . . ? N5 Zn1 Cl1 107.55(10) . . ? Cl2 Zn1 Cl1 114.63(5) . . ? C12 N1 N2 105.9(3) . . ? C12 N1 Rh1 128.8(3) . . ? N2 N1 Rh1 123.5(2) . . ? C14 N2 N1 109.7(3) . . ? C14 N2 B1 125.9(4) . . ? N1 N2 B1 124.2(3) . . ? C9 N3 N4 105.6(3) . . ? C9 N3 Rh1 130.8(3) . . ? N4 N3 Rh1 123.1(2) . . ? C11 N4 N3 109.4(3) . . ? C11 N4 B1 125.8(3) . . ? N3 N4 B1 123.8(3) . . ? C15 N5 N6 107.1(3) . . ? C15 N5 Zn1 125.6(3) . . ? N6 N5 Zn1 126.7(2) . . ? N5 N6 C17 109.3(3) . . ? N5 N6 B1 123.5(3) . . ? C17 N6 B1 125.2(4) . . ? C18 N7 N8 106.9(3) . . ? C18 N7 Zn1 126.2(3) . . ? N8 N7 Zn1 122.2(2) . . ? C20 N8 N7 108.4(3) . . ? C20 N8 B1 126.4(4) . . ? N7 N8 B1 123.9(3) . . ? C2 C1 C5 123.6(4) . . ? C2 C1 Rh1 70.0(2) . . ? C5 C1 Rh1 113.8(2) . . ? C2 C1 H1A 114.0 . . ? C5 C1 H1A 114.0 . . ? Rh1 C1 H1A 114.0 . . ? C1 C2 C8 126.8(4) . . ? C1 C2 Rh1 72.4(2) . . ? C8 C2 Rh1 109.2(3) . . ? C1 C2 H2A 113.5 . . ? C8 C2 H2A 113.5 . . ? Rh1 C2 H2A 113.5 . . ? C3 C4 C7 122.6(4) . . ? C3 C4 Rh1 71.3(2) . . ? C7 C4 Rh1 112.6(2) . . ? C3 C4 H3A 114.3 . . ? C7 C4 H3A 114.3 . . ? Rh1 C4 H3A 114.3 . . ? C4 C3 C6 126.4(4) . . ? C4 C3 Rh1 70.4(2) . . ? C6 C3 Rh1 111.5(3) . . ? C4 C3 H4A 113.5 . . ? C6 C3 H4A 113.5 . . ? Rh1 C3 H4A 113.5 . . ? C6 C5 C1 113.1(3) . . ? C6 C5 H5A 109.0 . . ? C1 C5 H5A 109.0 . . ? C6 C5 H18B 109.0 . . ? C1 C5 H18B 109.0 . . ? H5A C5 H18B 107.8 . . ? C5 C6 C3 114.1(4) . . ? C5 C6 H6A 108.7 . . ? C3 C6 H6A 108.7 . . ? C5 C6 H6B 108.7 . . ? C3 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? C8 C7 C4 113.3(3) . . ? C8 C7 H7A 108.9 . . ? C4 C7 H7A 108.9 . . ? C8 C7 H7B 108.9 . . ? C4 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C7 C8 C2 113.5(4) . . ? C7 C8 H8A 108.9 . . ? C2 C8 H8A 108.9 . . ? C7 C8 H8B 108.9 . . ? C2 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? N3 C9 C10 111.2(3) . . ? N3 C9 H9A 124.4 . . ? C10 C9 H9A 124.4 . . ? C11 C10 C9 105.4(3) . . ? C11 C10 H10A 127.3 . . ? C9 C10 H10A 127.3 . . ? N4 C11 C10 108.3(4) . . ? N4 C11 H11A 125.8 . . ? C10 C11 H11A 125.8 . . ? N1 C12 C13 110.9(4) . . ? N1 C12 H12A 124.6 . . ? C13 C12 H12A 124.6 . . ? C14 C13 C12 105.3(4) . . ? C14 C13 H13A 127.4 . . ? C12 C13 H13A 127.4 . . ? N2 C14 C13 108.2(4) . . ? N2 C14 H14A 125.9 . . ? C13 C14 H14A 125.9 . . ? N5 C15 C16 110.5(4) . . ? N5 C15 H15A 124.7 . . ? C16 C15 H15A 124.7 . . ? C17 C16 C15 105.6(4) . . ? C17 C16 H16A 127.2 . . ? C15 C16 H16A 127.2 . . ? N6 C17 C16 107.5(4) . . ? N6 C17 H17A 126.2 . . ? C16 C17 H17A 126.2 . . ? N7 C18 C19 110.4(4) . . ? N7 C18 H18A 124.8 . . ? C19 C18 H18A 124.8 . . ? C20 C19 C18 105.1(3) . . ? C20 C19 H19A 127.5 . . ? C18 C19 H19A 127.5 . . ? N8 C20 C19 109.2(4) . . ? N8 C20 H20A 125.4 . . ? C19 C20 H20A 125.4 . . ? Cl3 C21 Cl4 112.0(2) . . ? Cl3 C21 H21A 109.2 . . ? Cl4 C21 H21A 109.2 . . ? Cl3 C21 H21B 109.2 . . ? Cl4 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? N2 B1 N6 107.9(3) . . ? N2 B1 N8 108.1(3) . . ? N6 B1 N8 112.9(4) . . ? N2 B1 N4 111.7(4) . . ? N6 B1 N4 105.6(3) . . ? N8 B1 N4 110.7(3) . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 0.789 _refine_diff_density_min -0.890 _refine_diff_density_rms 0.141 data_16 _database_code_depnum_ccdc_archive 'CCDC 768035' #TrackingRef '- Hallett_Dalton_Cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 B Cl2 N8 Pd Rh, C2 H3 N' _chemical_formula_sum 'C22 H27 B Cl2 N9 Pd Rh' _chemical_formula_weight 708.55 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' B B 0.0013 0.0007 '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' Cl Cl 0.1484 0.1585 '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' Pd Pd -0.9988 1.0072 '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 9.5842(11) _cell_length_b 11.8561(13) _cell_length_c 12.6161(14) _cell_angle_alpha 73.114(2) _cell_angle_beta 86.102(2) _cell_angle_gamma 74.047(2) _cell_volume 1318.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 122 _cell_measurement_theta_min 2.7055 _cell_measurement_theta_max 27.3545 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.784 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 1.541 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.738482 _exptl_absorpt_correction_T_max 0.887862 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10115 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5677 _reflns_number_gt 4143 _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^)+(0.0393P)^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 5677 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0831 _refine_ls_wR_factor_gt 0.0632 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _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 Pd1 Pd 0.40025(3) 1.15170(3) 0.67642(2) 0.02026(9) Uani 1 1 d . . . Rh1 Rh 0.30336(3) 0.67846(3) 0.96684(3) 0.02295(10) Uani 1 1 d . . . Cl1 Cl 0.23557(12) 1.30510(10) 0.72927(9) 0.0329(3) Uani 1 1 d . . . Cl2 Cl 0.56458(13) 1.26601(10) 0.64590(9) 0.0342(3) Uani 1 1 d . . . N1 N 0.3989(4) 0.6368(3) 0.8220(3) 0.0248(8) Uani 1 1 d . . . N2 N 0.4486(3) 0.7197(3) 0.7386(3) 0.0218(8) Uani 1 1 d . . . N3 N 0.4469(4) 0.7828(3) 0.9586(3) 0.0238(8) Uani 1 1 d . . . N4 N 0.5018(3) 0.8404(3) 0.8614(3) 0.0199(7) Uani 1 1 d . . . N5 N 0.5476(3) 1.0189(3) 0.6237(3) 0.0210(7) Uani 1 1 d . . . N6 N 0.5572(3) 0.8962(3) 0.6629(3) 0.0208(7) Uani 1 1 d . . . N7 N 0.2545(3) 1.0520(3) 0.7080(3) 0.0239(8) Uani 1 1 d . . . N8 N 0.2919(3) 0.9300(3) 0.7183(3) 0.0202(7) Uani 1 1 d . . . N9 N 0.0334(5) 0.6663(5) 0.6498(4) 0.0629(14) Uani 1 1 d . . . C1 C 0.2136(5) 0.5249(4) 1.0135(4) 0.0306(10) Uani 1 1 d . . . H1A H 0.2613 0.4594 0.9776 0.037 Uiso 1 1 calc R . . C2 C 0.1129(4) 0.6246(4) 0.9444(4) 0.0290(10) Uani 1 1 d . . . H2A H 0.1016 0.6171 0.8688 0.035 Uiso 1 1 calc R . . C3 C 0.2321(5) 0.6857(5) 1.1317(4) 0.0360(12) Uani 1 1 d . . . H3A H 0.3039 0.7020 1.1753 0.043 Uiso 1 1 calc R . . C4 C 0.1550(5) 0.7894(5) 1.0519(4) 0.0351(11) Uani 1 1 d . . . H4A H 0.1809 0.8660 1.0505 0.042 Uiso 1 1 calc R . . C5 C 0.1720(5) 0.5810(5) 1.1940(4) 0.0421(13) Uani 1 1 d . . . H5A H 0.0656 0.6117 1.2002 0.051 Uiso 1 1 calc R . . H5B H 0.2139 0.5477 1.2699 0.051 Uiso 1 1 calc R . . C6 C 0.2044(5) 0.4785(5) 1.1384(4) 0.0407(13) Uani 1 1 d . . . H6A H 0.2975 0.4189 1.1680 0.049 Uiso 1 1 calc R . . H6B H 0.1272 0.4353 1.1571 0.049 Uiso 1 1 calc R . . C7 C -0.0230(4) 0.6984(4) 0.9881(4) 0.0356(11) Uani 1 1 d . . . H7A H -0.0540 0.6452 1.0563 0.043 Uiso 1 1 calc R . . H7B H -0.1022 0.7258 0.9323 0.043 Uiso 1 1 calc R . . C8 C 0.0013(5) 0.8111(4) 1.0139(4) 0.0363(11) Uani 1 1 d . . . H8A H -0.0207 0.8817 0.9466 0.044 Uiso 1 1 calc R . . H8B H -0.0666 0.8318 1.0723 0.044 Uiso 1 1 calc R . . C9 C 0.5160(4) 0.7989(4) 1.0397(3) 0.0254(9) Uani 1 1 d . . . H9A H 0.4998 0.7680 1.1165 0.030 Uiso 1 1 calc R . . C10 C 0.6132(4) 0.8660(4) 0.9969(3) 0.0266(10) Uani 1 1 d . . . H10A H 0.6753 0.8897 1.0369 0.032 Uiso 1 1 calc R . . C11 C 0.6019(4) 0.8916(4) 0.8843(3) 0.0245(9) Uani 1 1 d . . . H11A H 0.6553 0.9376 0.8311 0.029 Uiso 1 1 calc R . . C12 C 0.4012(5) 0.5444(4) 0.7809(4) 0.0310(10) Uani 1 1 d . . . H12A H 0.3740 0.4727 0.8215 0.037 Uiso 1 1 calc R . . C13 C 0.4478(5) 0.5650(4) 0.6727(4) 0.0310(10) Uani 1 1 d . . . H13A H 0.4587 0.5131 0.6260 0.037 Uiso 1 1 calc R . . C14 C 0.4747(4) 0.6773(4) 0.6481(3) 0.0267(10) Uani 1 1 d . . . H14A H 0.5067 0.7190 0.5786 0.032 Uiso 1 1 calc R . . C15 C 0.6697(4) 1.0287(4) 0.5680(3) 0.0238(9) Uani 1 1 d . . . H15A H 0.6910 1.1040 0.5308 0.029 Uiso 1 1 calc R . . C16 C 0.7606(4) 0.9146(4) 0.5717(3) 0.0270(10) Uani 1 1 d . . . H16A H 0.8532 0.8964 0.5389 0.032 Uiso 1 1 calc R . . C17 C 0.6878(4) 0.8338(4) 0.6330(3) 0.0261(10) Uani 1 1 d . . . H17A H 0.7232 0.7472 0.6518 0.031 Uiso 1 1 calc R . . C18 C 0.1100(4) 1.0921(4) 0.6981(3) 0.0283(10) Uani 1 1 d . . . H18A H 0.0551 1.1743 0.6897 0.034 Uiso 1 1 calc R . . C19 C 0.0523(5) 0.9965(4) 0.7021(4) 0.0303(10) Uani 1 1 d . . . H19A H -0.0472 0.9998 0.6967 0.036 Uiso 1 1 calc R . . C20 C 0.1693(4) 0.8953(4) 0.7154(3) 0.0254(9) Uani 1 1 d . . . H20A H 0.1647 0.8146 0.7217 0.030 Uiso 1 1 calc R . . C21 C 0.0858(6) 0.6270(5) 0.5801(5) 0.0442(13) Uani 1 1 d . . . C22 C 0.1538(6) 0.5764(6) 0.4916(4) 0.0567(15) Uani 1 1 d . . . H22A H 0.2197 0.6239 0.4512 0.085 Uiso 1 1 calc R . . H22B H 0.0789 0.5801 0.4406 0.085 Uiso 1 1 calc R . . H22C H 0.2087 0.4911 0.5231 0.085 Uiso 1 1 calc R . . B1 B 0.4488(5) 0.8470(4) 0.7456(4) 0.0203(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 Pd1 0.02466(17) 0.01644(16) 0.01991(16) -0.00578(12) 0.00038(13) -0.00523(13) Rh1 0.02174(17) 0.02532(19) 0.02258(18) -0.00639(14) 0.00197(14) -0.00839(14) Cl1 0.0376(6) 0.0226(5) 0.0380(6) -0.0136(5) 0.0037(5) -0.0028(5) Cl2 0.0466(7) 0.0312(6) 0.0355(6) -0.0161(5) 0.0106(5) -0.0230(5) N1 0.0257(18) 0.0216(18) 0.0264(18) -0.0072(15) 0.0013(15) -0.0052(15) N2 0.0241(17) 0.0181(17) 0.0222(18) -0.0048(14) 0.0017(14) -0.0054(14) N3 0.0249(18) 0.0273(19) 0.0217(18) -0.0080(15) 0.0044(15) -0.0107(15) N4 0.0174(16) 0.0185(17) 0.0237(18) -0.0053(14) 0.0010(14) -0.0054(14) N5 0.0264(18) 0.0172(17) 0.0207(17) -0.0060(14) 0.0006(14) -0.0072(14) N6 0.0236(17) 0.0180(17) 0.0209(17) -0.0065(14) 0.0031(14) -0.0056(14) N7 0.0239(18) 0.0203(18) 0.0278(19) -0.0077(15) -0.0016(15) -0.0047(15) N8 0.0235(17) 0.0173(16) 0.0208(17) -0.0067(14) 0.0001(14) -0.0057(14) N9 0.053(3) 0.062(3) 0.061(3) -0.016(3) -0.005(3) 0.004(3) C1 0.030(2) 0.028(2) 0.037(3) -0.008(2) 0.007(2) -0.016(2) C2 0.025(2) 0.033(2) 0.032(2) -0.010(2) -0.0002(19) -0.0124(19) C3 0.030(2) 0.057(3) 0.029(2) -0.022(2) 0.005(2) -0.015(2) C4 0.032(2) 0.045(3) 0.039(3) -0.026(2) 0.012(2) -0.016(2) C5 0.029(2) 0.065(4) 0.032(3) -0.007(3) 0.002(2) -0.019(3) C6 0.029(2) 0.044(3) 0.037(3) 0.011(2) 0.002(2) -0.015(2) C7 0.021(2) 0.044(3) 0.042(3) -0.013(2) -0.001(2) -0.008(2) C8 0.029(2) 0.041(3) 0.036(3) -0.017(2) 0.006(2) -0.001(2) C9 0.027(2) 0.028(2) 0.023(2) -0.0099(18) 0.0004(18) -0.0085(19) C10 0.022(2) 0.031(2) 0.030(2) -0.0125(19) -0.0037(18) -0.0059(19) C11 0.020(2) 0.023(2) 0.030(2) -0.0053(18) 0.0022(18) -0.0081(17) C12 0.034(2) 0.021(2) 0.041(3) -0.011(2) 0.000(2) -0.0095(19) C13 0.035(2) 0.027(2) 0.035(3) -0.017(2) 0.001(2) -0.007(2) C14 0.031(2) 0.024(2) 0.024(2) -0.0103(18) -0.0019(18) -0.0012(18) C15 0.027(2) 0.028(2) 0.019(2) -0.0081(17) 0.0049(17) -0.0121(19) C16 0.023(2) 0.030(2) 0.028(2) -0.0081(19) 0.0044(18) -0.0078(18) C17 0.025(2) 0.024(2) 0.028(2) -0.0088(18) 0.0012(18) -0.0028(18) C18 0.021(2) 0.028(2) 0.032(2) -0.0098(19) -0.0033(18) 0.0018(18) C19 0.022(2) 0.032(2) 0.037(3) -0.008(2) -0.0019(19) -0.0085(19) C20 0.027(2) 0.025(2) 0.028(2) -0.0071(18) 0.0005(18) -0.0149(18) C21 0.040(3) 0.045(3) 0.042(3) -0.005(3) -0.005(3) -0.010(3) C22 0.069(4) 0.067(4) 0.042(3) -0.015(3) 0.016(3) -0.036(3) B1 0.021(2) 0.022(2) 0.016(2) -0.0069(18) 0.0018(18) -0.0030(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 Pd1 N7 2.017(3) . ? Pd1 N5 2.043(3) . ? Pd1 Cl1 2.2863(11) . ? Pd1 Cl2 2.2920(12) . ? Rh1 N3 2.068(3) . ? Rh1 N1 2.114(3) . ? Rh1 C4 2.119(4) . ? Rh1 C1 2.138(4) . ? Rh1 C2 2.153(4) . ? Rh1 C3 2.163(4) . ? N1 C12 1.337(5) . ? N1 N2 1.374(4) . ? N2 C14 1.358(5) . ? N2 B1 1.537(6) . ? N3 C9 1.340(5) . ? N3 N4 1.367(4) . ? N4 C11 1.354(5) . ? N4 B1 1.552(5) . ? N5 C15 1.338(5) . ? N5 N6 1.372(4) . ? N6 C17 1.359(5) . ? N6 B1 1.530(6) . ? N7 C18 1.337(5) . ? N7 N8 1.360(4) . ? N8 C20 1.354(5) . ? N8 B1 1.552(5) . ? N9 C21 1.136(7) . ? C1 C2 1.406(6) . ? C1 C6 1.515(6) . ? C1 H1A 1.0000 . ? C2 C7 1.524(6) . ? C2 H2A 1.0000 . ? C3 C4 1.398(6) . ? C3 C5 1.502(7) . ? C3 H3A 1.0000 . ? C4 C8 1.511(6) . ? C4 H4A 1.0000 . ? C5 C6 1.524(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.542(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.372(6) . ? C9 H9A 0.9500 . ? C10 C11 1.369(6) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 C13 1.381(6) . ? C12 H12A 0.9500 . ? C13 C14 1.369(6) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.383(6) . ? C15 H15A 0.9500 . ? C16 C17 1.366(6) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.378(6) . ? C18 H18A 0.9500 . ? C19 C20 1.376(6) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 C22 1.452(7) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? 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 N7 Pd1 N5 91.15(13) . . ? N7 Pd1 Cl1 89.88(10) . . ? N5 Pd1 Cl1 177.95(9) . . ? N7 Pd1 Cl2 178.22(10) . . ? N5 Pd1 Cl2 90.03(10) . . ? Cl1 Pd1 Cl2 88.98(4) . . ? N3 Rh1 N1 88.10(13) . . ? N3 Rh1 C4 89.60(16) . . ? N1 Rh1 C4 153.18(15) . . ? N3 Rh1 C1 159.86(15) . . ? N1 Rh1 C1 93.59(16) . . ? C4 Rh1 C1 97.63(19) . . ? N3 Rh1 C2 161.83(14) . . ? N1 Rh1 C2 92.08(15) . . ? C4 Rh1 C2 82.08(17) . . ? C1 Rh1 C2 38.26(15) . . ? N3 Rh1 C3 93.91(16) . . ? N1 Rh1 C3 168.67(16) . . ? C4 Rh1 C3 38.11(17) . . ? C1 Rh1 C3 80.73(19) . . ? C2 Rh1 C3 89.47(17) . . ? C12 N1 N2 105.5(3) . . ? C12 N1 Rh1 130.9(3) . . ? N2 N1 Rh1 122.5(3) . . ? C14 N2 N1 108.8(3) . . ? C14 N2 B1 127.4(3) . . ? N1 N2 B1 123.1(3) . . ? C9 N3 N4 106.1(3) . . ? C9 N3 Rh1 130.2(3) . . ? N4 N3 Rh1 123.3(2) . . ? C11 N4 N3 109.1(3) . . ? C11 N4 B1 127.6(3) . . ? N3 N4 B1 123.3(3) . . ? C15 N5 N6 106.7(3) . . ? C15 N5 Pd1 127.2(3) . . ? N6 N5 Pd1 124.4(3) . . ? C17 N6 N5 108.0(3) . . ? C17 N6 B1 128.6(3) . . ? N5 N6 B1 122.2(3) . . ? C18 N7 N8 107.6(3) . . ? C18 N7 Pd1 128.1(3) . . ? N8 N7 Pd1 122.8(3) . . ? C20 N8 N7 108.5(3) . . ? C20 N8 B1 127.8(3) . . ? N7 N8 B1 123.1(3) . . ? C2 C1 C6 125.5(4) . . ? C2 C1 Rh1 71.5(3) . . ? C6 C1 Rh1 110.9(3) . . ? C2 C1 H1A 113.7 . . ? C6 C1 H1A 113.7 . . ? Rh1 C1 H1A 113.7 . . ? C1 C2 C7 122.9(4) . . ? C1 C2 Rh1 70.3(2) . . ? C7 C2 Rh1 112.1(3) . . ? C1 C2 H2A 114.5 . . ? C7 C2 H2A 114.5 . . ? Rh1 C2 H2A 114.5 . . ? C4 C3 C5 124.6(4) . . ? C4 C3 Rh1 69.2(2) . . ? C5 C3 Rh1 113.5(3) . . ? C4 C3 H3A 113.9 . . ? C5 C3 H3A 113.9 . . ? Rh1 C3 H3A 113.9 . . ? C3 C4 C8 125.1(4) . . ? C3 C4 Rh1 72.6(3) . . ? C8 C4 Rh1 110.5(3) . . ? C3 C4 H4A 113.7 . . ? C8 C4 H4A 113.7 . . ? Rh1 C4 H4A 113.7 . . ? C3 C5 C6 112.7(4) . . ? C3 C5 H5A 109.1 . . ? C6 C5 H5A 109.1 . . ? C3 C5 H5B 109.1 . . ? C6 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? C1 C6 C5 112.6(4) . . ? C1 C6 H6A 109.1 . . ? C5 C6 H6A 109.1 . . ? C1 C6 H6B 109.1 . . ? C5 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? C2 C7 C8 112.5(4) . . ? C2 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? C2 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? C4 C8 C7 112.3(4) . . ? C4 C8 H8A 109.1 . . ? C7 C8 H8A 109.1 . . ? C4 C8 H8B 109.1 . . ? C7 C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? N3 C9 C10 110.9(4) . . ? N3 C9 H9A 124.5 . . ? C10 C9 H9A 124.5 . . ? C11 C10 C9 105.4(4) . . ? C11 C10 H10A 127.3 . . ? C9 C10 H10A 127.3 . . ? N4 C11 C10 108.5(4) . . ? N4 C11 H11A 125.8 . . ? C10 C11 H11A 125.8 . . ? N1 C12 C13 112.2(4) . . ? N1 C12 H12A 123.9 . . ? C13 C12 H12A 123.9 . . ? C14 C13 C12 104.1(4) . . ? C14 C13 H13A 127.9 . . ? C12 C13 H13A 127.9 . . ? N2 C14 C13 109.4(4) . . ? N2 C14 H14A 125.3 . . ? C13 C14 H14A 125.3 . . ? N5 C15 C16 110.9(4) . . ? N5 C15 H15A 124.5 . . ? C16 C15 H15A 124.5 . . ? C17 C16 C15 104.8(4) . . ? C17 C16 H16A 127.6 . . ? C15 C16 H16A 127.6 . . ? N6 C17 C16 109.6(4) . . ? N6 C17 H17A 125.2 . . ? C16 C17 H17A 125.2 . . ? N7 C18 C19 109.9(4) . . ? N7 C18 H18A 125.1 . . ? C19 C18 H18A 125.1 . . ? C20 C19 C18 105.5(4) . . ? C20 C19 H19A 127.2 . . ? C18 C19 H19A 127.2 . . ? N8 C20 C19 108.5(4) . . ? N8 C20 H20A 125.7 . . ? C19 C20 H20A 125.7 . . ? N9 C21 C22 179.6(6) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N6 B1 N2 109.5(3) . . ? N6 B1 N8 111.3(3) . . ? N2 B1 N8 106.9(3) . . ? N6 B1 N4 105.7(3) . . ? N2 B1 N4 111.2(3) . . ? N8 B1 N4 112.2(3) . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.532 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.114