# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ic15211-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H42 Cl2 Co2 N12 O Rh' _chemical_formula_weight 1046.57 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' O O 0.0106 0.0060 '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 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 15.9265(3) _cell_length_b 15.7081(3) _cell_length_c 16.9952(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.7514(11) _cell_angle_gamma 90.00 _cell_volume 4202.27(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25058 _cell_measurement_theta_min 1.29 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2124 _exptl_absorpt_coefficient_mu 1.348 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.597 _exptl_absorpt_correction_T_max 0.667 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'NONIUS KappaCCD' _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 25058 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0610 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9595 _reflns_number_gt 6641 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _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^)+(0.0421P)^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 9595 _refine_ls_number_parameters 562 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0883 _refine_ls_wR_factor_gt 0.0815 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group M1 Rh 0.347247(17) 0.416054(18) 0.173086(15) 0.01886(8) Uani 0.50 1 d P A 1 M2 Co 0.140911(17) 0.545330(18) 0.303115(15) 0.01831(8) Uani 0.50 1 d P A 1 M1' Rh 0.140911(17) 0.545330(18) 0.303115(15) 0.01831(8) Uani 0.50 1 d P A 2 M2' Co 0.347247(17) 0.416054(18) 0.173086(15) 0.01886(8) Uani 0.50 1 d P A 2 Co2 Co 0.24535(2) 0.47916(2) 0.23971(2) 0.01552(9) Uani 1 1 d . . . Cl1 Cl 0.45524(4) 0.34306(5) 0.10593(4) 0.02680(17) Uani 1 1 d . . . Cl2 Cl 0.03140(4) 0.61513(5) 0.37404(4) 0.02758(17) Uani 1 1 d . . . N1 N 0.29717(14) 0.30438(15) 0.20418(12) 0.0206(5) Uani 1 1 d . . . N2 N 0.17643(14) 0.37888(15) 0.22171(12) 0.0186(5) Uani 1 1 d . A . N3 N 0.05969(14) 0.45929(15) 0.24173(13) 0.0217(5) Uani 1 1 d . . . N4 N 0.38675(14) 0.53519(15) 0.15462(13) 0.0210(5) Uani 1 1 d . . . N5 N 0.31432(14) 0.57991(15) 0.25618(12) 0.0187(5) Uani 1 1 d . A . N6 N 0.23845(14) 0.62045(15) 0.35578(13) 0.0206(5) Uani 1 1 d . . . N7 N 0.25914(14) 0.42158(15) 0.07430(12) 0.0200(5) Uani 1 1 d . . . N8 N 0.19053(14) 0.52426(15) 0.13957(13) 0.0216(5) Uani 1 1 d . A . N9 N 0.11767(14) 0.62288(15) 0.20535(13) 0.0215(5) Uani 1 1 d . . . N10 N 0.42112(14) 0.42106(15) 0.27977(13) 0.0199(5) Uani 1 1 d . . . N11 N 0.30068(14) 0.43317(15) 0.33896(12) 0.0198(5) Uani 1 1 d . A . N12 N 0.17565(15) 0.45624(15) 0.38992(13) 0.0221(5) Uani 1 1 d . . . C1 C 0.34411(19) 0.2320(2) 0.21214(16) 0.0264(7) Uani 1 1 d . A . H1 H 0.4019 0.2352 0.2046 0.032 Uiso 1 1 calc R . . C2 C 0.3129(2) 0.1551(2) 0.23038(17) 0.0305(7) Uani 1 1 d . . . H2 H 0.3478 0.1058 0.2346 0.037 Uiso 1 1 calc R A . C3 C 0.22816(19) 0.1502(2) 0.24281(16) 0.0301(7) Uani 1 1 d . A . H3 H 0.2041 0.0971 0.2542 0.036 Uiso 1 1 calc R . . C4 C 0.18048(18) 0.22289(19) 0.23826(16) 0.0251(7) Uani 1 1 d . . . H4 H 0.1232 0.2203 0.2475 0.030 Uiso 1 1 calc R A . C5 C 0.21551(17) 0.30179(18) 0.22003(14) 0.0207(6) Uani 1 1 d . A . C6 C 0.09011(17) 0.38858(18) 0.20869(15) 0.0197(6) Uani 1 1 d . A . C7 C 0.03351(18) 0.33448(19) 0.16067(16) 0.0242(6) Uani 1 1 d . . . H7 H 0.0545 0.2859 0.1366 0.029 Uiso 1 1 calc R A . C8 C -0.05235(18) 0.3516(2) 0.14837(16) 0.0276(7) Uani 1 1 d . A . H8 H -0.0907 0.3146 0.1166 0.033 Uiso 1 1 calc R . . C9 C -0.08214(18) 0.4230(2) 0.18262(17) 0.0293(7) Uani 1 1 d . . . H9 H -0.1411 0.4356 0.1753 0.035 Uiso 1 1 calc R A . C10 C -0.02454(18) 0.4754(2) 0.22744(17) 0.0265(7) Uani 1 1 d . A . H10 H -0.0450 0.5254 0.2495 0.032 Uiso 1 1 calc R . . C11 C 0.43617(18) 0.55178(19) 0.09780(16) 0.0239(7) Uani 1 1 d . A . H11 H 0.4474 0.5067 0.0637 0.029 Uiso 1 1 calc R . . C12 C 0.47047(19) 0.6298(2) 0.08726(16) 0.0272(7) Uani 1 1 d . . . H12 H 0.5063 0.6383 0.0481 0.033 Uiso 1 1 calc R A . C13 C 0.45158(19) 0.6966(2) 0.13547(16) 0.0274(7) Uani 1 1 d . A . H13 H 0.4744 0.7517 0.1295 0.033 Uiso 1 1 calc R . . C14 C 0.39978(18) 0.68230(19) 0.19176(16) 0.0237(6) Uani 1 1 d . . . H14 H 0.3855 0.7282 0.2237 0.028 Uiso 1 1 calc R A . C15 C 0.36771(17) 0.60029(19) 0.20260(15) 0.0206(6) Uani 1 1 d . A . C16 C 0.31288(17) 0.62561(18) 0.32492(15) 0.0196(6) Uani 1 1 d . A . C17 C 0.38223(18) 0.67075(19) 0.36636(16) 0.0249(7) Uani 1 1 d . . . H17 H 0.4343 0.6729 0.3456 0.030 Uiso 1 1 calc R A . C18 C 0.37535(19) 0.7114(2) 0.43613(16) 0.0280(7) Uani 1 1 d . A . H18 H 0.4220 0.7427 0.4634 0.034 Uiso 1 1 calc R . . C19 C 0.29963(19) 0.7065(2) 0.46683(16) 0.0307(7) Uani 1 1 d . . . H19 H 0.2932 0.7346 0.5150 0.037 Uiso 1 1 calc R A . C20 C 0.23443(19) 0.66008(19) 0.42583(16) 0.0266(7) Uani 1 1 d . A . H20 H 0.1833 0.6554 0.4479 0.032 Uiso 1 1 calc R . . C21 C 0.26040(19) 0.36742(19) 0.01281(16) 0.0253(7) Uani 1 1 d . A . H21 H 0.3088 0.3319 0.0131 0.030 Uiso 1 1 calc R . . C22 C 0.1956(2) 0.3609(2) -0.04995(16) 0.0329(8) Uani 1 1 d . . . H22 H 0.1993 0.3220 -0.0921 0.040 Uiso 1 1 calc R A . C23 C 0.1247(2) 0.4121(2) -0.05086(17) 0.0316(7) Uani 1 1 d . A . H23 H 0.0785 0.4078 -0.0932 0.038 Uiso 1 1 calc R . . C24 C 0.12185(19) 0.4694(2) 0.01044(16) 0.0274(7) Uani 1 1 d . . . H24 H 0.0738 0.5053 0.0101 0.033 Uiso 1 1 calc R A . C25 C 0.19050(17) 0.47448(19) 0.07350(16) 0.0218(6) Uani 1 1 d . A . C26 C 0.14497(17) 0.59839(18) 0.13647(16) 0.0201(6) Uani 1 1 d . A . C27 C 0.12795(18) 0.6511(2) 0.06880(16) 0.0264(7) Uani 1 1 d . . . H27 H 0.1504 0.6367 0.0219 0.032 Uiso 1 1 calc R A . C28 C 0.07969(19) 0.7226(2) 0.06999(18) 0.0323(7) Uani 1 1 d . A . H28 H 0.0660 0.7562 0.0234 0.039 Uiso 1 1 calc R . . C29 C 0.05058(19) 0.7458(2) 0.14001(17) 0.0307(7) Uani 1 1 d . . . H29 H 0.0164 0.7950 0.1422 0.037 Uiso 1 1 calc R A . C30 C 0.07261(19) 0.69565(19) 0.20566(17) 0.0273(7) Uani 1 1 d . A . H30 H 0.0552 0.7130 0.2543 0.033 Uiso 1 1 calc R . . C31 C 0.50641(18) 0.4275(2) 0.28346(17) 0.0267(7) Uani 1 1 d . A . H31 H 0.5291 0.4283 0.2349 0.032 Uiso 1 1 calc R . . C32 C 0.56175(19) 0.4328(2) 0.35343(18) 0.0311(7) Uani 1 1 d . . . H32 H 0.6212 0.4381 0.3537 0.037 Uiso 1 1 calc R A . C33 C 0.52754(19) 0.4302(2) 0.42394(17) 0.0291(7) Uani 1 1 d . A . H33 H 0.5641 0.4310 0.4736 0.035 Uiso 1 1 calc R . . C34 C 0.44187(18) 0.42631(19) 0.42213(16) 0.0260(7) Uani 1 1 d . . . H34 H 0.4190 0.4245 0.4706 0.031 Uiso 1 1 calc R A . C35 C 0.38694(17) 0.42501(18) 0.34896(15) 0.0194(6) Uani 1 1 d . A . C36 C 0.25194(17) 0.41468(18) 0.39749(15) 0.0207(6) Uani 1 1 d . A . C37 C 0.27334(19) 0.3555(2) 0.45882(16) 0.0268(7) Uani 1 1 d . . . H37 H 0.3257 0.3255 0.4633 0.032 Uiso 1 1 calc R A . C38 C 0.21871(19) 0.3406(2) 0.51252(16) 0.0288(7) Uani 1 1 d . A . H38 H 0.2345 0.3028 0.5559 0.035 Uiso 1 1 calc R . . C39 C 0.1408(2) 0.3808(2) 0.50312(17) 0.0304(7) Uani 1 1 d . . . H39 H 0.1016 0.3700 0.5388 0.036 Uiso 1 1 calc R A . C40 C 0.12125(19) 0.4367(2) 0.44117(16) 0.0283(7) Uani 1 1 d . A . H40 H 0.0669 0.4631 0.4338 0.034 Uiso 1 1 calc R . . O1 O 0.73365(13) 0.43630(14) 0.24909(12) 0.0356(5) Uani 1 1 d . . . C41 C 0.6677(2) 0.4524(3) 0.11507(19) 0.0511(11) Uani 1 1 d . . . H41A H 0.6305 0.4952 0.1337 0.077 Uiso 1 1 calc R . . H41B H 0.6370 0.4227 0.0688 0.077 Uiso 1 1 calc R . . H41C H 0.7179 0.4805 0.1000 0.077 Uiso 1 1 calc R . . C42 C 0.69604(19) 0.3872(2) 0.18296(18) 0.0381(9) Uani 1 1 d . . . H42A H 0.6465 0.3551 0.1962 0.046 Uiso 1 1 calc R . . H42B H 0.7376 0.3463 0.1669 0.046 Uiso 1 1 calc R . . C43 C 0.7737(2) 0.3833(2) 0.31177(18) 0.0380(8) Uani 1 1 d . . . H43A H 0.8162 0.3463 0.2919 0.046 Uiso 1 1 calc R . . H43B H 0.7308 0.3465 0.3313 0.046 Uiso 1 1 calc R . . C44 C 0.8166(2) 0.4382(2) 0.37866(19) 0.0452(9) Uani 1 1 d . . . H44A H 0.8600 0.4735 0.3594 0.068 Uiso 1 1 calc R . . H44B H 0.8434 0.4020 0.4223 0.068 Uiso 1 1 calc R . . H44C H 0.7743 0.4750 0.3979 0.068 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 M1 0.01826(15) 0.02030(17) 0.01856(15) -0.00027(11) 0.00452(11) 0.00068(12) M2 0.01728(15) 0.01929(17) 0.01890(14) 0.00039(11) 0.00446(11) -0.00098(12) M1' 0.01728(15) 0.01929(17) 0.01890(14) 0.00039(11) 0.00446(11) -0.00098(12) M2' 0.01826(15) 0.02030(17) 0.01856(15) -0.00027(11) 0.00452(11) 0.00068(12) Co2 0.01419(19) 0.0172(2) 0.01571(18) -0.00068(14) 0.00417(14) -0.00017(15) Cl1 0.0250(4) 0.0294(4) 0.0283(4) -0.0012(3) 0.0115(3) 0.0046(3) Cl2 0.0252(4) 0.0278(4) 0.0325(4) 0.0004(3) 0.0129(3) 0.0040(3) N1 0.0211(13) 0.0233(14) 0.0179(12) -0.0013(10) 0.0052(9) 0.0030(11) N2 0.0170(12) 0.0171(13) 0.0220(12) -0.0014(9) 0.0043(9) -0.0001(10) N3 0.0201(13) 0.0230(14) 0.0231(12) 0.0024(10) 0.0067(10) 0.0002(11) N4 0.0183(13) 0.0253(14) 0.0198(12) 0.0008(10) 0.0037(9) 0.0008(11) N5 0.0193(12) 0.0197(13) 0.0179(11) -0.0008(9) 0.0050(9) -0.0018(10) N6 0.0234(13) 0.0188(13) 0.0211(12) 0.0005(10) 0.0087(10) 0.0012(11) N7 0.0224(13) 0.0186(13) 0.0195(12) -0.0010(9) 0.0050(9) -0.0013(11) N8 0.0192(13) 0.0247(14) 0.0219(12) -0.0013(10) 0.0059(9) 0.0004(11) N9 0.0210(13) 0.0224(14) 0.0218(12) -0.0016(10) 0.0058(9) -0.0012(11) N10 0.0211(13) 0.0164(13) 0.0231(12) -0.0003(9) 0.0064(9) 0.0010(10) N11 0.0179(12) 0.0245(14) 0.0178(11) -0.0008(10) 0.0049(9) 0.0000(11) N12 0.0249(13) 0.0220(14) 0.0211(12) -0.0016(10) 0.0086(10) -0.0022(11) C1 0.0266(16) 0.0296(19) 0.0237(15) 0.0026(13) 0.0063(12) 0.0085(14) C2 0.0344(18) 0.0255(18) 0.0320(16) 0.0031(13) 0.0059(13) 0.0087(15) C3 0.0382(19) 0.0239(18) 0.0284(16) 0.0036(13) 0.0055(13) 0.0011(15) C4 0.0251(16) 0.0246(17) 0.0256(15) 0.0030(12) 0.0041(12) -0.0027(14) C5 0.0209(15) 0.0255(17) 0.0148(13) 0.0016(11) 0.0001(11) -0.0008(13) C6 0.0183(15) 0.0221(16) 0.0195(14) 0.0049(11) 0.0054(11) -0.0031(13) C7 0.0256(16) 0.0224(17) 0.0249(15) 0.0032(12) 0.0045(12) -0.0027(13) C8 0.0251(16) 0.0319(19) 0.0245(15) 0.0063(13) -0.0001(12) -0.0072(14) C9 0.0170(15) 0.036(2) 0.0341(17) 0.0097(14) 0.0021(12) -0.0019(14) C10 0.0201(16) 0.0307(19) 0.0296(16) 0.0044(13) 0.0069(12) 0.0050(14) C11 0.0263(16) 0.0263(18) 0.0208(15) 0.0024(12) 0.0087(12) 0.0034(14) C12 0.0290(17) 0.0292(18) 0.0247(15) 0.0047(13) 0.0085(12) 0.0002(14) C13 0.0299(17) 0.0260(18) 0.0269(16) 0.0052(13) 0.0063(13) -0.0049(14) C14 0.0291(16) 0.0190(16) 0.0234(15) 0.0006(12) 0.0051(12) -0.0007(13) C15 0.0175(15) 0.0252(17) 0.0184(14) 0.0000(11) 0.0009(11) 0.0020(13) C16 0.0195(15) 0.0180(16) 0.0219(14) 0.0019(11) 0.0052(11) 0.0006(12) C17 0.0253(16) 0.0266(18) 0.0235(15) -0.0008(12) 0.0057(12) -0.0051(14) C18 0.0326(18) 0.0294(19) 0.0212(15) -0.0033(12) 0.0018(12) -0.0079(14) C19 0.0371(19) 0.036(2) 0.0198(15) -0.0052(13) 0.0080(13) -0.0006(16) C20 0.0321(17) 0.0273(18) 0.0222(15) 0.0013(12) 0.0099(12) 0.0001(14) C21 0.0294(17) 0.0240(17) 0.0233(15) -0.0049(12) 0.0068(12) -0.0002(14) C22 0.052(2) 0.0257(18) 0.0198(15) -0.0039(13) 0.0021(14) -0.0018(16) C23 0.0390(19) 0.0284(19) 0.0239(16) -0.0011(13) -0.0062(13) -0.0068(16) C24 0.0278(17) 0.0269(18) 0.0259(16) 0.0029(13) -0.0010(12) 0.0013(14) C25 0.0229(16) 0.0223(17) 0.0208(14) 0.0030(11) 0.0049(11) -0.0028(13) C26 0.0167(14) 0.0181(16) 0.0250(15) 0.0007(11) 0.0010(11) -0.0020(12) C27 0.0311(17) 0.0267(18) 0.0220(15) 0.0005(12) 0.0058(12) -0.0012(14) C28 0.0337(18) 0.0285(19) 0.0330(17) 0.0054(14) -0.0005(14) 0.0030(15) C29 0.0300(18) 0.0243(18) 0.0380(18) 0.0019(14) 0.0057(14) 0.0066(14) C30 0.0293(17) 0.0219(17) 0.0321(16) -0.0040(13) 0.0095(13) 0.0025(14) C31 0.0190(16) 0.0281(18) 0.0339(17) -0.0016(13) 0.0069(12) 0.0000(13) C32 0.0204(16) 0.033(2) 0.0393(19) -0.0053(14) 0.0034(13) 0.0034(14) C33 0.0273(17) 0.0271(18) 0.0293(16) -0.0024(13) -0.0078(13) 0.0040(14) C34 0.0283(17) 0.0280(18) 0.0216(15) -0.0010(12) 0.0035(12) 0.0001(14) C35 0.0224(15) 0.0138(15) 0.0220(14) 0.0001(11) 0.0034(11) -0.0012(12) C36 0.0216(15) 0.0224(17) 0.0185(14) -0.0045(11) 0.0047(11) -0.0047(13) C37 0.0300(17) 0.0259(18) 0.0247(15) 0.0033(13) 0.0050(12) 0.0036(14) C38 0.0419(19) 0.0230(18) 0.0227(15) 0.0050(12) 0.0086(13) -0.0004(15) C39 0.0369(19) 0.0289(19) 0.0294(17) 0.0005(13) 0.0177(14) -0.0028(15) C40 0.0299(17) 0.0286(18) 0.0292(17) -0.0039(13) 0.0131(13) -0.0038(15) O1 0.0343(13) 0.0353(14) 0.0367(13) -0.0004(10) 0.0039(10) 0.0024(11) C41 0.0268(19) 0.092(3) 0.0322(19) 0.0153(19) -0.0047(14) -0.005(2) C42 0.0235(17) 0.046(2) 0.048(2) -0.0176(17) 0.0138(15) -0.0151(16) C43 0.040(2) 0.036(2) 0.0386(19) 0.0044(15) 0.0088(15) 0.0076(17) C44 0.043(2) 0.053(3) 0.039(2) 0.0015(17) 0.0041(16) -0.0005(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 M1 N10 2.007(2) . ? M1 N4 2.014(2) . ? M1 N7 2.019(2) . ? M1 N1 2.030(2) . ? M1 Co2 2.3362(4) . ? M1 Cl1 2.4845(7) . ? M2 N3 2.044(2) . ? M2 N6 2.045(2) . ? M2 N12 2.048(2) . ? M2 N9 2.048(2) . ? M2 Co2 2.3566(4) . ? M2 Cl2 2.5173(7) . ? Co2 N2 1.918(2) . ? Co2 N11 1.921(2) . ? Co2 N5 1.923(2) . ? Co2 N8 1.926(2) . ? N1 C1 1.356(4) . ? N1 C5 1.368(3) . ? N2 C5 1.364(4) . ? N2 C6 1.367(3) . ? N3 C10 1.350(3) . ? N3 C6 1.366(4) . ? N4 C11 1.361(3) . ? N4 C15 1.370(3) . ? N5 C15 1.375(3) . ? N5 C16 1.374(3) . ? N6 C20 1.354(3) . ? N6 C16 1.370(3) . ? N7 C21 1.350(3) . ? N7 C25 1.372(4) . ? N8 C25 1.368(3) . ? N8 C26 1.369(4) . ? N9 C30 1.350(4) . ? N9 C26 1.365(3) . ? N10 C31 1.354(3) . ? N10 C35 1.370(3) . ? N11 C35 1.364(3) . ? N11 C36 1.383(3) . ? N12 C40 1.354(3) . ? N12 C36 1.368(4) . ? C1 C2 1.360(4) . ? C2 C3 1.399(4) . ? C3 C4 1.367(4) . ? C4 C5 1.413(4) . ? C6 C7 1.406(4) . ? C7 C8 1.378(4) . ? C8 C9 1.380(4) . ? C9 C10 1.373(4) . ? C11 C12 1.364(4) . ? C12 C13 1.392(4) . ? C13 C14 1.373(4) . ? C14 C15 1.408(4) . ? C16 C17 1.408(4) . ? C17 C18 1.366(4) . ? C18 C19 1.387(4) . ? C19 C20 1.370(4) . ? C21 C22 1.370(4) . ? C22 C23 1.384(4) . ? C23 C24 1.383(4) . ? C24 C25 1.412(4) . ? C26 C27 1.410(4) . ? C27 C28 1.362(4) . ? C28 C29 1.390(4) . ? C29 C30 1.367(4) . ? C31 C32 1.371(4) . ? C32 C33 1.390(4) . ? C33 C34 1.361(4) . ? C34 C35 1.408(4) . ? C36 C37 1.400(4) . ? C37 C38 1.373(4) . ? C38 C39 1.379(4) . ? C39 C40 1.370(4) . ? O1 C42 1.419(4) . ? O1 C43 1.424(4) . ? C41 C42 1.558(5) . ? C43 C44 1.506(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 N10 M1 N4 87.15(9) . . ? N10 M1 N7 170.73(9) . . ? N4 M1 N7 91.41(9) . . ? N10 M1 N1 89.90(9) . . ? N4 M1 N1 171.08(8) . . ? N7 M1 N1 90.16(9) . . ? N10 M1 Co2 84.29(6) . . ? N4 M1 Co2 86.43(6) . . ? N7 M1 Co2 86.48(6) . . ? N1 M1 Co2 84.90(6) . . ? N10 M1 Cl1 94.67(6) . . ? N4 M1 Cl1 95.90(6) . . ? N7 M1 Cl1 94.59(6) . . ? N1 M1 Cl1 92.73(6) . . ? Co2 M1 Cl1 177.41(2) . . ? N3 M2 N6 169.86(9) . . ? N3 M2 N12 89.80(9) . . ? N6 M2 N12 88.57(9) . . ? N3 M2 N9 87.54(9) . . ? N6 M2 N9 92.48(9) . . ? N12 M2 N9 170.65(9) . . ? N3 M2 Co2 84.89(6) . . ? N6 M2 Co2 84.99(6) . . ? N12 M2 Co2 84.02(6) . . ? N9 M2 Co2 86.81(6) . . ? N3 M2 Cl2 95.83(6) . . ? N6 M2 Cl2 94.28(6) . . ? N12 M2 Cl2 94.80(6) . . ? N9 M2 Cl2 94.39(6) . . ? Co2 M2 Cl2 178.62(2) . . ? N2 Co2 N11 90.35(10) . . ? N2 Co2 N5 179.21(9) . . ? N11 Co2 N5 90.35(9) . . ? N2 Co2 N8 89.41(10) . . ? N11 Co2 N8 179.33(10) . . ? N5 Co2 N8 89.89(10) . . ? N2 Co2 M1 89.83(6) . . ? N11 Co2 M1 90.36(6) . . ? N5 Co2 M1 89.78(6) . . ? N8 Co2 M1 89.01(6) . . ? N2 Co2 M2 90.49(6) . . ? N11 Co2 M2 91.48(6) . . ? N5 Co2 M2 89.87(6) . . ? N8 Co2 M2 89.15(7) . . ? M1 Co2 M2 178.13(2) . . ? C1 N1 C5 118.8(2) . . ? C1 N1 M1 121.18(19) . . ? C5 N1 M1 119.99(18) . . ? C5 N2 C6 123.1(2) . . ? C5 N2 Co2 118.73(18) . . ? C6 N2 Co2 118.11(18) . . ? C10 N3 C6 118.9(2) . . ? C10 N3 M2 120.2(2) . . ? C6 N3 M2 120.73(18) . . ? C11 N4 C15 118.9(2) . . ? C11 N4 M1 121.11(19) . . ? C15 N4 M1 119.87(17) . . ? C15 N5 C16 122.2(2) . . ? C15 N5 Co2 119.50(18) . . ? C16 N5 Co2 118.08(17) . . ? C20 N6 C16 118.0(2) . . ? C20 N6 M2 121.05(18) . . ? C16 N6 M2 120.70(18) . . ? C21 N7 C25 118.7(2) . . ? C21 N7 M1 121.74(19) . . ? C25 N7 M1 119.10(18) . . ? C25 N8 C26 121.4(2) . . ? C25 N8 Co2 117.29(19) . . ? C26 N8 Co2 120.89(18) . . ? C30 N9 C26 118.7(2) . . ? C30 N9 M2 122.07(18) . . ? C26 N9 M2 119.10(19) . . ? C31 N10 C35 118.9(2) . . ? C31 N10 M1 119.40(18) . . ? C35 N10 M1 121.48(18) . . ? C35 N11 C36 123.8(2) . . ? C35 N11 Co2 117.60(16) . . ? C36 N11 Co2 118.55(18) . . ? C40 N12 C36 118.5(2) . . ? C40 N12 M2 119.3(2) . . ? C36 N12 M2 122.19(17) . . ? N1 C1 C2 123.5(3) . . ? C1 C2 C3 118.6(3) . . ? C4 C3 C2 119.0(3) . . ? C3 C4 C5 120.7(3) . . ? N2 C5 N1 115.3(2) . . ? N2 C5 C4 125.3(2) . . ? N1 C5 C4 119.2(3) . . ? N3 C6 N2 115.8(2) . . ? N3 C6 C7 119.6(2) . . ? N2 C6 C7 124.5(3) . . ? C8 C7 C6 120.3(3) . . ? C7 C8 C9 119.4(3) . . ? C10 C9 C8 118.5(3) . . ? N3 C10 C9 123.3(3) . . ? N4 C11 C12 123.5(3) . . ? C11 C12 C13 118.2(3) . . ? C14 C13 C12 119.6(3) . . ? C13 C14 C15 120.6(3) . . ? N4 C15 N5 115.8(2) . . ? N4 C15 C14 119.2(2) . . ? N5 C15 C14 124.9(3) . . ? N6 C16 N5 115.0(2) . . ? N6 C16 C17 119.8(2) . . ? N5 C16 C17 125.1(2) . . ? C18 C17 C16 120.6(3) . . ? C17 C18 C19 119.3(3) . . ? C20 C19 C18 118.3(3) . . ? N6 C20 C19 124.0(3) . . ? N7 C21 C22 123.5(3) . . ? C21 C22 C23 118.8(3) . . ? C24 C23 C22 119.3(3) . . ? C23 C24 C25 119.9(3) . . ? N8 C25 N7 115.9(2) . . ? N8 C25 C24 124.0(3) . . ? N7 C25 C24 119.8(3) . . ? N9 C26 N8 116.3(2) . . ? N9 C26 C27 119.2(3) . . ? N8 C26 C27 124.5(2) . . ? C28 C27 C26 120.7(3) . . ? C27 C28 C29 119.5(3) . . ? C30 C29 C28 118.0(3) . . ? N9 C30 C29 123.7(3) . . ? N10 C31 C32 123.6(3) . . ? C31 C32 C33 117.5(3) . . ? C34 C33 C32 120.3(3) . . ? C33 C34 C35 120.4(3) . . ? N11 C35 N10 114.9(2) . . ? N11 C35 C34 126.0(2) . . ? N10 C35 C34 119.0(2) . . ? N12 C36 N11 114.8(2) . . ? N12 C36 C37 120.0(2) . . ? N11 C36 C37 125.1(3) . . ? C38 C37 C36 120.0(3) . . ? C37 C38 C39 119.7(3) . . ? C40 C39 C38 118.6(3) . . ? N12 C40 C39 123.1(3) . . ? C42 O1 C43 111.2(3) . . ? O1 C42 C41 105.6(3) . . ? O1 C43 C44 109.3(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.188 _refine_diff_density_min -0.849 _refine_diff_density_rms 0.100 _database_code_depnum_ccdc_archive 'CCDC 939270' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ic15628-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H42 Cl2 Co N12 Ni O Rh' _chemical_formula_weight 1046.35 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' O O 0.0106 0.0060 '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' Ni Ni 0.3393 1.1124 '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 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 16.0264(2) _cell_length_b 15.7368(3) _cell_length_c 16.9707(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.9708(9) _cell_angle_gamma 90.00 _cell_volume 4215.44(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 26320 _cell_measurement_theta_min 1.29 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 1.397 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.597 _exptl_absorpt_correction_T_max 0.764 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'NONIUS KappaCCD' _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 26320 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0596 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9580 _reflns_number_gt 6735 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _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^)+(0.0573P)^2^+0.9418P] 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 9580 _refine_ls_number_parameters 561 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1134 _refine_ls_wR_factor_gt 0.1016 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.011 _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 M1 Rh 0.34645(2) 0.41477(2) 0.172978(19) 0.02331(10) Uani 0.50 1 d P A 1 M2 Ni 0.14226(2) 0.54336(2) 0.302186(19) 0.02102(10) Uani 0.50 1 d P A 1 M1' Rh 0.14226(2) 0.54336(2) 0.302186(19) 0.02102(10) Uani 0.50 1 d P A 2 M2' Ni 0.34645(2) 0.41477(2) 0.172978(19) 0.02331(10) Uani 0.50 1 d P A 2 Co2 Co 0.24494(3) 0.47895(3) 0.23820(2) 0.01805(11) Uani 1 1 d . . . Cl1 Cl 0.45729(6) 0.33726(6) 0.10192(5) 0.0328(2) Uani 1 1 d . . . Cl2 Cl 0.02723(6) 0.61797(6) 0.37768(5) 0.0345(2) Uani 1 1 d . . . N1 N 0.29629(17) 0.30432(19) 0.20236(15) 0.0252(6) Uani 1 1 d . . . N2 N 0.17604(17) 0.37852(18) 0.21983(16) 0.0235(6) Uani 1 1 d . A . N3 N 0.06141(19) 0.45832(18) 0.24270(16) 0.0263(7) Uani 1 1 d . . . N4 N 0.38554(18) 0.53277(18) 0.15617(16) 0.0252(6) Uani 1 1 d . . . N5 N 0.31386(17) 0.57929(18) 0.25591(16) 0.0232(6) Uani 1 1 d . A . N6 N 0.23776(17) 0.61921(18) 0.35407(16) 0.0238(6) Uani 1 1 d . . . N7 N 0.25771(18) 0.42176(18) 0.07376(16) 0.0245(6) Uani 1 1 d . . . N8 N 0.18923(17) 0.52378(18) 0.13756(16) 0.0234(6) Uani 1 1 d . A . N9 N 0.11676(18) 0.61988(19) 0.20549(16) 0.0263(7) Uani 1 1 d . . . N10 N 0.42013(18) 0.41837(18) 0.27991(16) 0.0246(6) Uani 1 1 d . . . N11 N 0.30150(17) 0.43260(18) 0.33877(15) 0.0225(6) Uani 1 1 d . A . N12 N 0.17813(18) 0.45723(18) 0.38880(16) 0.0243(6) Uani 1 1 d . . . C1 C 0.3437(2) 0.2326(2) 0.2104(2) 0.0310(8) Uani 1 1 d . A . H1 H 0.4013 0.2363 0.2036 0.037 Uiso 1 1 calc R . . C2 C 0.3127(2) 0.1549(3) 0.2278(2) 0.0358(9) Uani 1 1 d . . . H2 H 0.3476 0.1057 0.2317 0.043 Uiso 1 1 calc R A . C3 C 0.2288(2) 0.1499(3) 0.2396(2) 0.0343(9) Uani 1 1 d . A . H3 H 0.2052 0.0967 0.2506 0.041 Uiso 1 1 calc R . . C4 C 0.1806(2) 0.2225(2) 0.2350(2) 0.0278(8) Uani 1 1 d . . . H4 H 0.1238 0.2196 0.2438 0.033 Uiso 1 1 calc R A . C5 C 0.2148(2) 0.3014(2) 0.21724(18) 0.0233(7) Uani 1 1 d . A . C6 C 0.0901(2) 0.3881(2) 0.20885(19) 0.0228(7) Uani 1 1 d . A . C7 C 0.0320(2) 0.3341(2) 0.1608(2) 0.0276(8) Uani 1 1 d . . . H7 H 0.0516 0.2862 0.1353 0.033 Uiso 1 1 calc R A . C8 C -0.0537(2) 0.3516(2) 0.1512(2) 0.0300(8) Uani 1 1 d . A . H8 H -0.0934 0.3149 0.1198 0.036 Uiso 1 1 calc R . . C9 C -0.0817(2) 0.4220(3) 0.1871(2) 0.0344(9) Uani 1 1 d . . . H9 H -0.1405 0.4342 0.1817 0.041 Uiso 1 1 calc R A . C10 C -0.0229(2) 0.4740(2) 0.2306(2) 0.0316(9) Uani 1 1 d . A . H10 H -0.0422 0.5238 0.2536 0.038 Uiso 1 1 calc R . . C11 C 0.4348(2) 0.5486(2) 0.0997(2) 0.0296(8) Uani 1 1 d . A . H11 H 0.4459 0.5030 0.0663 0.035 Uiso 1 1 calc R . . C12 C 0.4689(2) 0.6261(3) 0.0888(2) 0.0349(9) Uani 1 1 d . . . H12 H 0.5040 0.6340 0.0497 0.042 Uiso 1 1 calc R A . C13 C 0.4511(2) 0.6933(2) 0.1363(2) 0.0320(8) Uani 1 1 d . A . H13 H 0.4743 0.7480 0.1304 0.038 Uiso 1 1 calc R . . C14 C 0.3998(2) 0.6799(2) 0.1920(2) 0.0279(8) Uani 1 1 d . . . H14 H 0.3862 0.7263 0.2234 0.033 Uiso 1 1 calc R A . C15 C 0.3671(2) 0.5990(2) 0.20336(19) 0.0232(7) Uani 1 1 d . A . C16 C 0.3108(2) 0.6257(2) 0.32387(19) 0.0235(7) Uani 1 1 d . A . C17 C 0.3801(2) 0.6719(2) 0.36709(19) 0.0263(8) Uani 1 1 d . . . H17 H 0.4324 0.6741 0.3479 0.032 Uiso 1 1 calc R A . C18 C 0.3718(2) 0.7132(2) 0.4361(2) 0.0331(9) Uani 1 1 d . A . H18 H 0.4174 0.7460 0.4638 0.040 Uiso 1 1 calc R . . C19 C 0.2963(2) 0.7071(2) 0.4656(2) 0.0328(9) Uani 1 1 d . . . H19 H 0.2893 0.7356 0.5134 0.039 Uiso 1 1 calc R A . C20 C 0.2321(2) 0.6589(2) 0.4241(2) 0.0304(8) Uani 1 1 d . A . H20 H 0.1813 0.6530 0.4452 0.036 Uiso 1 1 calc R . . C21 C 0.2600(2) 0.3679(2) 0.0124(2) 0.0304(8) Uani 1 1 d . A . H21 H 0.3085 0.3328 0.0140 0.036 Uiso 1 1 calc R . . C22 C 0.1957(3) 0.3613(2) -0.0522(2) 0.0364(9) Uani 1 1 d . . . H22 H 0.1995 0.3221 -0.0941 0.044 Uiso 1 1 calc R A . C23 C 0.1247(3) 0.4133(2) -0.0551(2) 0.0360(9) Uani 1 1 d . A . H23 H 0.0789 0.4094 -0.0987 0.043 Uiso 1 1 calc R . . C24 C 0.1219(2) 0.4701(2) 0.0057(2) 0.0301(8) Uani 1 1 d . . . H24 H 0.0743 0.5064 0.0039 0.036 Uiso 1 1 calc R A . C25 C 0.1896(2) 0.4747(2) 0.07096(19) 0.0237(7) Uani 1 1 d . A . C26 C 0.1425(2) 0.5971(2) 0.1354(2) 0.0240(7) Uani 1 1 d . A . C27 C 0.1233(2) 0.6512(2) 0.0686(2) 0.0298(8) Uani 1 1 d . . . H27 H 0.1441 0.6378 0.0210 0.036 Uiso 1 1 calc R A . C28 C 0.0756(2) 0.7226(2) 0.0711(2) 0.0365(9) Uani 1 1 d . A . H28 H 0.0614 0.7574 0.0250 0.044 Uiso 1 1 calc R . . C29 C 0.0476(3) 0.7440(3) 0.1423(2) 0.0386(9) Uani 1 1 d . . . H29 H 0.0131 0.7925 0.1454 0.046 Uiso 1 1 calc R A . C30 C 0.0720(2) 0.6923(2) 0.2074(2) 0.0335(9) Uani 1 1 d . A . H30 H 0.0564 0.7084 0.2568 0.040 Uiso 1 1 calc R . . C31 C 0.5050(2) 0.4232(2) 0.2836(2) 0.0323(9) Uani 1 1 d . A . H31 H 0.5265 0.4230 0.2348 0.039 Uiso 1 1 calc R . . C32 C 0.5619(2) 0.4283(3) 0.3545(2) 0.0376(9) Uani 1 1 d . . . H32 H 0.6212 0.4320 0.3552 0.045 Uiso 1 1 calc R A . C33 C 0.5288(2) 0.4280(3) 0.4244(2) 0.0362(9) Uani 1 1 d . A . H33 H 0.5661 0.4294 0.4745 0.043 Uiso 1 1 calc R . . C34 C 0.4433(2) 0.4256(2) 0.4228(2) 0.0301(8) Uani 1 1 d . . . H34 H 0.4216 0.4257 0.4715 0.036 Uiso 1 1 calc R A . C35 C 0.3872(2) 0.4231(2) 0.34892(19) 0.0240(7) Uani 1 1 d . A . C36 C 0.2542(2) 0.4151(2) 0.39689(19) 0.0249(8) Uani 1 1 d . A . C37 C 0.2753(2) 0.3558(2) 0.4584(2) 0.0290(8) Uani 1 1 d . . . H37 H 0.3273 0.3258 0.4635 0.035 Uiso 1 1 calc R A . C38 C 0.2213(2) 0.3406(2) 0.5119(2) 0.0341(9) Uani 1 1 d . A . H38 H 0.2371 0.3022 0.5551 0.041 Uiso 1 1 calc R . . C39 C 0.1435(2) 0.3819(2) 0.5019(2) 0.0351(9) Uani 1 1 d . . . H39 H 0.1048 0.3714 0.5372 0.042 Uiso 1 1 calc R A . C40 C 0.1242(2) 0.4382(2) 0.4398(2) 0.0304(8) Uani 1 1 d . A . H40 H 0.0704 0.4653 0.4321 0.036 Uiso 1 1 calc R . . O1 O 0.73439(18) 0.4352(2) 0.25177(17) 0.0463(7) Uani 1 1 d . . . C41 C 0.6678(3) 0.4577(4) 0.1181(2) 0.0672(17) Uani 1 1 d . . . H41A H 0.6450 0.5072 0.1421 0.101 Uiso 1 1 calc R . . H41B H 0.6243 0.4341 0.0761 0.101 Uiso 1 1 calc R . . H41C H 0.7171 0.4749 0.0948 0.101 Uiso 1 1 calc R . . C42 C 0.6961(3) 0.3865(3) 0.1861(3) 0.0579(14) Uani 1 1 d . . . H42A H 0.6465 0.3550 0.1984 0.069 Uiso 1 1 calc R . . H42B H 0.7367 0.3457 0.1694 0.069 Uiso 1 1 calc R . . C43 C 0.7749(3) 0.3810(3) 0.3140(3) 0.0499(11) Uani 1 1 d . . . H43A H 0.8168 0.3445 0.2938 0.060 Uiso 1 1 calc R . . H43B H 0.7324 0.3439 0.3327 0.060 Uiso 1 1 calc R . . C44 C 0.8187(3) 0.4352(3) 0.3823(3) 0.0538(12) Uani 1 1 d . . . H44A H 0.8621 0.4703 0.3638 0.081 Uiso 1 1 calc R . . H44B H 0.8455 0.3985 0.4261 0.081 Uiso 1 1 calc R . . H44C H 0.7770 0.4721 0.4013 0.081 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 M1 0.02647(19) 0.0214(2) 0.02252(18) 0.00035(14) 0.00544(13) -0.00096(14) M2 0.02394(18) 0.01883(19) 0.02094(18) 0.00120(13) 0.00568(13) -0.00116(13) M1' 0.02394(18) 0.01883(19) 0.02094(18) 0.00120(13) 0.00568(13) -0.00116(13) M2' 0.02647(19) 0.0214(2) 0.02252(18) 0.00035(14) 0.00544(13) -0.00096(14) Co2 0.0208(2) 0.0165(2) 0.0169(2) 0.00073(17) 0.00351(17) -0.00217(18) Cl1 0.0330(5) 0.0331(5) 0.0351(5) 0.0015(4) 0.0139(4) 0.0036(4) Cl2 0.0348(5) 0.0311(5) 0.0396(5) 0.0041(4) 0.0115(4) 0.0021(4) N1 0.0262(15) 0.0283(17) 0.0213(14) -0.0009(12) 0.0049(12) -0.0001(13) N2 0.0291(16) 0.0194(16) 0.0234(15) -0.0012(12) 0.0078(12) -0.0014(12) N3 0.0340(17) 0.0227(16) 0.0235(15) 0.0040(12) 0.0086(12) 0.0017(13) N4 0.0294(16) 0.0220(16) 0.0237(15) 0.0014(12) 0.0034(12) 0.0007(12) N5 0.0266(15) 0.0214(16) 0.0223(15) -0.0001(12) 0.0064(12) -0.0006(12) N6 0.0266(15) 0.0240(16) 0.0223(15) 0.0044(12) 0.0085(12) -0.0003(12) N7 0.0280(16) 0.0215(16) 0.0240(15) -0.0001(12) 0.0044(12) -0.0018(12) N8 0.0223(14) 0.0240(16) 0.0249(15) 0.0003(12) 0.0068(12) 0.0000(12) N9 0.0282(16) 0.0241(17) 0.0282(16) -0.0030(13) 0.0092(12) -0.0048(13) N10 0.0315(16) 0.0190(16) 0.0251(15) -0.0012(12) 0.0097(12) -0.0021(12) N11 0.0275(15) 0.0202(15) 0.0204(14) -0.0002(12) 0.0061(12) 0.0009(12) N12 0.0256(15) 0.0205(16) 0.0274(16) -0.0012(12) 0.0060(12) 0.0001(12) C1 0.033(2) 0.032(2) 0.029(2) 0.0037(16) 0.0087(15) 0.0039(17) C2 0.040(2) 0.033(2) 0.035(2) 0.0041(17) 0.0078(17) 0.0070(18) C3 0.046(2) 0.028(2) 0.030(2) 0.0006(16) 0.0081(17) -0.0009(18) C4 0.0289(19) 0.024(2) 0.0314(19) -0.0004(15) 0.0083(15) -0.0035(15) C5 0.0281(18) 0.0247(19) 0.0177(16) -0.0007(14) 0.0056(13) -0.0037(15) C6 0.0252(17) 0.0212(18) 0.0234(17) 0.0044(14) 0.0086(14) -0.0020(14) C7 0.0315(19) 0.024(2) 0.0275(18) 0.0046(15) 0.0070(15) -0.0042(16) C8 0.0294(19) 0.031(2) 0.0282(19) 0.0056(16) 0.0023(15) -0.0063(16) C9 0.030(2) 0.037(2) 0.037(2) 0.0117(18) 0.0078(16) 0.0040(17) C10 0.033(2) 0.030(2) 0.034(2) 0.0059(16) 0.0093(16) 0.0045(17) C11 0.038(2) 0.032(2) 0.0204(18) 0.0025(15) 0.0100(15) 0.0080(17) C12 0.043(2) 0.036(2) 0.030(2) 0.0054(17) 0.0179(17) 0.0050(18) C13 0.039(2) 0.028(2) 0.0300(19) 0.0078(16) 0.0083(16) -0.0034(17) C14 0.035(2) 0.024(2) 0.0255(18) 0.0016(15) 0.0081(15) -0.0002(16) C15 0.0257(18) 0.0210(19) 0.0220(17) -0.0006(14) 0.0015(14) 0.0008(14) C16 0.0296(18) 0.0167(18) 0.0245(18) 0.0033(14) 0.0056(14) -0.0015(14) C17 0.0296(19) 0.026(2) 0.0248(18) 0.0036(15) 0.0080(14) -0.0050(15) C18 0.042(2) 0.032(2) 0.0256(19) 0.0001(16) 0.0059(16) -0.0086(17) C19 0.043(2) 0.034(2) 0.0231(18) -0.0056(16) 0.0112(16) -0.0015(18) C20 0.035(2) 0.034(2) 0.0248(18) 0.0038(16) 0.0125(15) 0.0019(17) C21 0.036(2) 0.024(2) 0.033(2) 0.0005(16) 0.0108(16) 0.0009(16) C22 0.059(3) 0.024(2) 0.026(2) -0.0034(16) 0.0058(18) 0.0018(19) C23 0.047(2) 0.032(2) 0.0248(19) 0.0000(16) -0.0042(17) -0.0022(18) C24 0.032(2) 0.030(2) 0.0278(19) 0.0046(16) 0.0023(15) 0.0018(16) C25 0.0289(18) 0.0198(18) 0.0228(17) 0.0032(14) 0.0059(14) -0.0021(14) C26 0.0229(17) 0.0226(19) 0.0270(18) -0.0006(14) 0.0058(14) -0.0037(14) C27 0.039(2) 0.026(2) 0.0258(19) 0.0016(15) 0.0071(15) 0.0013(17) C28 0.044(2) 0.029(2) 0.034(2) 0.0059(17) 0.0020(17) 0.0041(18) C29 0.045(2) 0.025(2) 0.047(2) -0.0014(18) 0.0101(19) 0.0078(18) C30 0.039(2) 0.027(2) 0.038(2) -0.0046(17) 0.0159(17) -0.0005(17) C31 0.035(2) 0.026(2) 0.039(2) -0.0032(17) 0.0131(17) -0.0010(16) C32 0.031(2) 0.035(2) 0.048(2) -0.0033(19) 0.0088(18) 0.0014(18) C33 0.036(2) 0.033(2) 0.036(2) -0.0031(17) -0.0044(17) 0.0046(18) C34 0.037(2) 0.026(2) 0.0280(19) 0.0001(15) 0.0075(16) 0.0022(16) C35 0.0324(19) 0.0162(17) 0.0228(17) 0.0005(14) 0.0034(14) 0.0005(15) C36 0.0322(19) 0.0203(19) 0.0227(18) -0.0029(14) 0.0058(14) -0.0018(15) C37 0.034(2) 0.025(2) 0.0287(19) 0.0028(15) 0.0063(15) 0.0029(16) C38 0.050(2) 0.025(2) 0.030(2) 0.0056(16) 0.0131(17) 0.0010(18) C39 0.043(2) 0.030(2) 0.038(2) -0.0026(17) 0.0218(18) -0.0047(18) C40 0.0307(19) 0.025(2) 0.038(2) -0.0038(16) 0.0116(16) -0.0012(16) O1 0.0441(17) 0.0472(19) 0.0470(17) 0.0003(14) 0.0061(14) 0.0048(14) C41 0.034(2) 0.134(6) 0.028(2) 0.018(3) -0.0105(18) 0.003(3) C42 0.035(2) 0.061(3) 0.086(4) -0.042(3) 0.032(2) -0.028(2) C43 0.055(3) 0.039(3) 0.057(3) 0.005(2) 0.014(2) 0.005(2) C44 0.060(3) 0.053(3) 0.049(3) -0.001(2) 0.008(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag M1 N10 1.987(3) . ? M1 N4 1.996(3) . ? M1 N7 2.010(3) . ? M1 N1 2.014(3) . ? M1 Co2 2.3485(5) . ? M1 Cl1 2.6152(9) . ? M2 N12 2.009(3) . ? M2 N3 2.009(3) . ? M2 N6 2.019(3) . ? M2 N9 2.019(3) . ? M2 Co2 2.3522(5) . ? M2 Cl2 2.6902(9) . ? Co2 N8 1.919(3) . ? Co2 N5 1.921(3) . ? Co2 N2 1.922(3) . ? Co2 N11 1.932(3) . ? N1 C1 1.355(5) . ? N1 C5 1.373(4) . ? N2 C6 1.366(4) . ? N2 C5 1.368(4) . ? N3 C10 1.355(4) . ? N3 C6 1.361(4) . ? N4 C11 1.366(4) . ? N4 C15 1.378(4) . ? N5 C15 1.372(4) . ? N5 C16 1.373(4) . ? N6 C20 1.360(4) . ? N6 C16 1.361(4) . ? N7 C21 1.348(4) . ? N7 C25 1.368(4) . ? N8 C25 1.370(4) . ? N8 C26 1.373(4) . ? N9 C30 1.350(5) . ? N9 C26 1.373(4) . ? N10 C31 1.353(4) . ? N10 C35 1.368(4) . ? N11 C35 1.362(4) . ? N11 C36 1.372(4) . ? N12 C40 1.358(4) . ? N12 C36 1.373(4) . ? C1 C2 1.370(5) . ? C2 C3 1.396(5) . ? C3 C4 1.375(5) . ? C4 C5 1.410(5) . ? C6 C7 1.411(5) . ? C7 C8 1.382(5) . ? C8 C9 1.377(5) . ? C9 C10 1.364(5) . ? C11 C12 1.363(5) . ? C12 C13 1.389(5) . ? C13 C14 1.371(5) . ? C14 C15 1.403(5) . ? C16 C17 1.421(5) . ? C17 C18 1.366(5) . ? C18 C19 1.392(5) . ? C19 C20 1.370(5) . ? C21 C22 1.372(5) . ? C22 C23 1.396(5) . ? C23 C24 1.373(5) . ? C24 C25 1.411(5) . ? C26 C27 1.408(5) . ? C27 C28 1.364(5) . ? C28 C29 1.401(5) . ? C29 C30 1.374(5) . ? C31 C32 1.381(5) . ? C32 C33 1.381(5) . ? C33 C34 1.366(5) . ? C34 C35 1.412(5) . ? C36 C37 1.397(5) . ? C37 C38 1.378(5) . ? C38 C39 1.390(5) . ? C39 C40 1.370(5) . ? O1 C42 1.404(5) . ? O1 C43 1.423(5) . ? C41 C42 1.615(7) . ? C43 C44 1.511(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N10 M1 N4 87.27(11) . . ? N10 M1 N7 170.33(11) . . ? N4 M1 N7 91.34(11) . . ? N10 M1 N1 89.89(11) . . ? N4 M1 N1 170.78(11) . . ? N7 M1 N1 89.99(11) . . ? N10 M1 Co2 84.72(8) . . ? N4 M1 Co2 85.84(8) . . ? N7 M1 Co2 85.63(8) . . ? N1 M1 Co2 85.17(8) . . ? N10 M1 Cl1 95.21(8) . . ? N4 M1 Cl1 96.48(8) . . ? N7 M1 Cl1 94.46(8) . . ? N1 M1 Cl1 92.51(8) . . ? Co2 M1 Cl1 177.67(3) . . ? N12 M2 N3 89.78(11) . . ? N12 M2 N6 88.88(11) . . ? N3 M2 N6 170.86(12) . . ? N12 M2 N9 171.49(12) . . ? N3 M2 N9 88.09(11) . . ? N6 M2 N9 91.91(11) . . ? N12 M2 Co2 84.99(8) . . ? N3 M2 Co2 85.58(8) . . ? N6 M2 Co2 85.30(8) . . ? N9 M2 Co2 86.63(8) . . ? N12 M2 Cl2 94.52(8) . . ? N3 M2 Cl2 95.42(8) . . ? N6 M2 Cl2 93.70(8) . . ? N9 M2 Cl2 93.88(8) . . ? Co2 M2 Cl2 178.89(3) . . ? N8 Co2 N5 90.20(12) . . ? N8 Co2 N2 89.55(12) . . ? N5 Co2 N2 179.67(11) . . ? N8 Co2 N11 179.26(12) . . ? N5 Co2 N11 90.17(11) . . ? N2 Co2 N11 90.07(12) . . ? N8 Co2 M1 89.55(8) . . ? N5 Co2 M1 90.05(8) . . ? N2 Co2 M1 89.73(8) . . ? N11 Co2 M1 89.81(8) . . ? N8 Co2 M2 89.86(8) . . ? N5 Co2 M2 90.16(8) . . ? N2 Co2 M2 90.06(8) . . ? N11 Co2 M2 90.78(8) . . ? M1 Co2 M2 179.38(2) . . ? C1 N1 C5 119.3(3) . . ? C1 N1 M1 120.2(2) . . ? C5 N1 M1 120.5(2) . . ? C6 N2 C5 123.2(3) . . ? C6 N2 Co2 117.9(2) . . ? C5 N2 Co2 118.9(2) . . ? C10 N3 C6 119.0(3) . . ? C10 N3 M2 119.7(2) . . ? C6 N3 M2 121.1(2) . . ? C11 N4 C15 118.6(3) . . ? C11 N4 M1 120.2(2) . . ? C15 N4 M1 121.1(2) . . ? C15 N5 C16 122.8(3) . . ? C15 N5 Co2 119.3(2) . . ? C16 N5 Co2 117.8(2) . . ? C20 N6 C16 119.1(3) . . ? C20 N6 M2 119.5(2) . . ? C16 N6 M2 121.1(2) . . ? C21 N7 C25 119.0(3) . . ? C21 N7 M1 120.2(2) . . ? C25 N7 M1 120.5(2) . . ? C25 N8 C26 122.1(3) . . ? C25 N8 Co2 117.3(2) . . ? C26 N8 Co2 120.0(2) . . ? C30 N9 C26 118.8(3) . . ? C30 N9 M2 121.1(2) . . ? C26 N9 M2 120.0(2) . . ? C31 N10 C35 119.5(3) . . ? C31 N10 M1 118.5(2) . . ? C35 N10 M1 121.8(2) . . ? C35 N11 C36 123.9(3) . . ? C35 N11 Co2 117.5(2) . . ? C36 N11 Co2 118.5(2) . . ? C40 N12 C36 118.8(3) . . ? C40 N12 M2 118.8(2) . . ? C36 N12 M2 122.4(2) . . ? N1 C1 C2 123.1(3) . . ? C1 C2 C3 118.4(4) . . ? C4 C3 C2 119.4(4) . . ? C3 C4 C5 120.6(3) . . ? N2 C5 N1 115.4(3) . . ? N2 C5 C4 125.3(3) . . ? N1 C5 C4 119.1(3) . . ? N3 C6 N2 116.0(3) . . ? N3 C6 C7 119.6(3) . . ? N2 C6 C7 124.2(3) . . ? C8 C7 C6 119.5(3) . . ? C9 C8 C7 120.0(4) . . ? C10 C9 C8 118.4(4) . . ? N3 C10 C9 123.4(4) . . ? C12 C11 N4 123.6(3) . . ? C11 C12 C13 118.3(3) . . ? C14 C13 C12 119.4(4) . . ? C13 C14 C15 121.1(3) . . ? N5 C15 N4 115.3(3) . . ? N5 C15 C14 125.7(3) . . ? N4 C15 C14 118.9(3) . . ? N6 C16 N5 115.7(3) . . ? N6 C16 C17 119.4(3) . . ? N5 C16 C17 124.6(3) . . ? C18 C17 C16 120.2(3) . . ? C17 C18 C19 119.7(3) . . ? C20 C19 C18 118.4(3) . . ? N6 C20 C19 123.1(3) . . ? N7 C21 C22 123.3(3) . . ? C21 C22 C23 118.5(3) . . ? C24 C23 C22 119.2(4) . . ? C23 C24 C25 120.2(4) . . ? N7 C25 N8 115.6(3) . . ? N7 C25 C24 119.8(3) . . ? N8 C25 C24 124.3(3) . . ? N8 C26 N9 116.1(3) . . ? N8 C26 C27 124.9(3) . . ? N9 C26 C27 118.9(3) . . ? C28 C27 C26 121.3(3) . . ? C27 C28 C29 119.2(4) . . ? C30 C29 C28 117.6(4) . . ? N9 C30 C29 123.9(3) . . ? N10 C31 C32 123.4(3) . . ? C33 C32 C31 117.0(4) . . ? C34 C33 C32 121.0(4) . . ? C33 C34 C35 120.1(3) . . ? N11 C35 N10 115.3(3) . . ? N11 C35 C34 125.6(3) . . ? N10 C35 C34 118.8(3) . . ? N11 C36 N12 115.0(3) . . ? N11 C36 C37 125.4(3) . . ? N12 C36 C37 119.5(3) . . ? C38 C37 C36 120.7(3) . . ? C37 C38 C39 119.3(3) . . ? C40 C39 C38 118.4(3) . . ? N12 C40 C39 123.2(3) . . ? C42 O1 C43 110.1(4) . . ? O1 C42 C41 102.6(4) . . ? O1 C43 C44 108.8(4) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.640 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.105 _database_code_depnum_ccdc_archive 'CCDC 939271' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ic15629-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43.50 H40 Cl5 Co F6 N12 Ni O0.50 P Rh' _chemical_formula_weight 1281.65 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' 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' Ni Ni 0.3393 1.1124 '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' O O 0.0106 0.0060 '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 11.5298(3) _cell_length_b 21.0861(4) _cell_length_c 20.3746(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.8115(10) _cell_angle_gamma 90.00 _cell_volume 4947.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 28891 _cell_measurement_theta_min 1.39 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2572 _exptl_absorpt_coefficient_mu 1.411 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.592 _exptl_absorpt_correction_T_max 0.713 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'NONIUS KappaCCD' _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 28891 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.0719 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11320 _reflns_number_gt 7223 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _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. The distance restraints ( DFIX; Sheldrick, 2008) are applied for the disordered solvents. ; _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^)+(0.0871P)^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 11320 _refine_ls_number_parameters 651 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0923 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1553 _refine_ls_wR_factor_gt 0.1421 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.149 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group M1 Rh 0.22299(4) 0.20224(2) 0.38112(2) 0.02136(13) Uani 0.50 1 d P A 1 M2 Ni 0.17242(4) 0.27973(2) 0.16570(2) 0.02221(13) Uani 0.50 1 d P A 1 M2' Ni 0.22299(4) 0.20224(2) 0.38112(2) 0.02136(13) Uani 0.50 1 d P A 2 M1' Rh 0.17242(4) 0.27973(2) 0.16570(2) 0.02221(13) Uani 0.50 1 d P A 2 Co2 Co 0.19487(5) 0.24563(3) 0.27554(3) 0.01761(15) Uani 1 1 d . . . Cl1 Cl 0.24197(12) 0.15993(6) 0.49197(6) 0.0409(3) Uani 1 1 d . . . Cl2 Cl 0.14693(12) 0.31924(7) 0.05421(6) 0.0396(3) Uani 1 1 d . . . N1 N 0.2279(4) 0.19184(19) 0.13926(19) 0.0329(10) Uani 1 1 d . . . N2 N 0.3057(4) 0.18327(19) 0.24647(19) 0.0308(10) Uani 1 1 d . A . N3 N 0.3806(4) 0.17153(19) 0.3536(2) 0.0331(10) Uani 1 1 d . . . N4 N 0.1127(4) 0.36222(19) 0.2077(2) 0.0325(10) Uani 1 1 d . . . N5 N 0.0833(4) 0.30416(18) 0.3028(2) 0.0312(10) Uani 1 1 d . A . N6 N 0.0554(4) 0.23737(19) 0.3914(2) 0.0325(10) Uani 1 1 d . . . N7 N 0.0061(4) 0.24499(19) 0.16887(19) 0.0311(10) Uani 1 1 d . . . N8 N 0.0739(4) 0.18386(19) 0.2578(2) 0.0321(10) Uani 1 1 d . A . N9 N 0.1491(4) 0.12146(19) 0.3432(2) 0.0337(10) Uani 1 1 d . . . N10 N 0.3411(4) 0.31145(19) 0.1806(2) 0.0304(10) Uani 1 1 d . . . N11 N 0.3160(4) 0.30541(19) 0.2927(2) 0.0328(10) Uani 1 1 d . A . N12 N 0.2985(4) 0.28901(18) 0.4047(2) 0.0333(10) Uani 1 1 d . . . C1 C 0.1963(5) 0.1661(3) 0.0803(3) 0.0420(14) Uani 1 1 d . A . H1 H 0.1579 0.1920 0.0479 0.050 Uiso 1 1 calc R . . C2 C 0.2177(6) 0.1044(3) 0.0658(3) 0.0555(17) Uani 1 1 d . . . H2 H 0.1952 0.0879 0.0237 0.067 Uiso 1 1 calc R A . C3 C 0.2729(6) 0.0654(3) 0.1131(3) 0.0536(17) Uani 1 1 d . A . H3 H 0.2881 0.0222 0.1038 0.064 Uiso 1 1 calc R . . C4 C 0.3048(5) 0.0907(3) 0.1731(3) 0.0440(14) Uani 1 1 d . . . H4 H 0.3417 0.0648 0.2061 0.053 Uiso 1 1 calc R A . C5 C 0.2827(4) 0.1554(2) 0.1861(3) 0.0326(12) Uani 1 1 d . A . C6 C 0.3960(4) 0.1642(2) 0.2883(2) 0.0301(11) Uani 1 1 d . A . C7 C 0.5026(5) 0.1425(2) 0.2671(3) 0.0371(13) Uani 1 1 d . . . H7 H 0.5132 0.1367 0.2216 0.044 Uiso 1 1 calc R A . C8 C 0.5922(5) 0.1293(3) 0.3124(3) 0.0445(14) Uani 1 1 d . A . H8 H 0.6646 0.1144 0.2984 0.053 Uiso 1 1 calc R . . C9 C 0.5756(5) 0.1383(3) 0.3786(3) 0.0475(15) Uani 1 1 d . . . H9 H 0.6360 0.1293 0.4107 0.057 Uiso 1 1 calc R A . C10 C 0.4694(5) 0.1604(3) 0.3968(3) 0.0399(13) Uani 1 1 d . A . H10 H 0.4588 0.1682 0.4420 0.048 Uiso 1 1 calc R . . C11 C 0.1086(5) 0.4170(3) 0.1743(3) 0.0405(13) Uani 1 1 d . A . H11 H 0.1425 0.4183 0.1328 0.049 Uiso 1 1 calc R . . C12 C 0.0581(5) 0.4715(3) 0.1969(3) 0.0464(15) Uani 1 1 d . . . H12 H 0.0573 0.5094 0.1717 0.056 Uiso 1 1 calc R A . C13 C 0.0088(5) 0.4692(3) 0.2569(3) 0.0456(14) Uani 1 1 d . A . H13 H -0.0309 0.5052 0.2728 0.055 Uiso 1 1 calc R . . C14 C 0.0172(5) 0.4145(2) 0.2941(3) 0.0404(14) Uani 1 1 d . . . H14 H -0.0122 0.4136 0.3369 0.048 Uiso 1 1 calc R A . C15 C 0.0684(5) 0.3612(2) 0.2691(2) 0.0325(12) Uani 1 1 d . A . C16 C 0.0101(5) 0.2835(2) 0.3505(2) 0.0303(11) Uani 1 1 d . A . C17 C -0.1067(5) 0.3019(2) 0.3533(3) 0.0369(12) Uani 1 1 d . . . H17 H -0.1385 0.3330 0.3239 0.044 Uiso 1 1 calc R A . C18 C -0.1744(5) 0.2742(3) 0.3992(3) 0.0448(14) Uani 1 1 d . A . H18 H -0.2530 0.2869 0.4025 0.054 Uiso 1 1 calc R . . C19 C -0.1275(5) 0.2277(3) 0.4406(3) 0.0433(14) Uani 1 1 d . . . H19 H -0.1733 0.2077 0.4721 0.052 Uiso 1 1 calc R A . C20 C -0.0144(5) 0.2113(3) 0.4351(3) 0.0385(13) Uani 1 1 d . A . H20 H 0.0174 0.1796 0.4639 0.046 Uiso 1 1 calc R . . C21 C -0.0826(5) 0.2693(3) 0.1308(2) 0.0366(12) Uani 1 1 d . A . H21 H -0.0661 0.3007 0.0992 0.044 Uiso 1 1 calc R . . C22 C -0.1964(5) 0.2502(3) 0.1363(3) 0.0424(14) Uani 1 1 d . . . H22 H -0.2565 0.2672 0.1080 0.051 Uiso 1 1 calc R A . C23 C -0.2214(5) 0.2059(3) 0.1836(3) 0.0504(16) Uani 1 1 d . A . H23 H -0.2993 0.1926 0.1885 0.060 Uiso 1 1 calc R . . C24 C -0.1327(5) 0.1810(3) 0.2237(3) 0.0460(15) Uani 1 1 d . . . H24 H -0.1490 0.1504 0.2562 0.055 Uiso 1 1 calc R A . C25 C -0.0193(5) 0.2010(2) 0.2160(2) 0.0327(12) Uani 1 1 d . A . C26 C 0.0807(5) 0.1246(2) 0.2872(2) 0.0337(12) Uani 1 1 d . A . C27 C 0.0306(5) 0.0701(2) 0.2594(3) 0.0428(14) Uani 1 1 d . . . H27 H -0.0177 0.0730 0.2204 0.051 Uiso 1 1 calc R A . C28 C 0.0514(5) 0.0119(3) 0.2887(3) 0.0460(15) Uani 1 1 d . A . H28 H 0.0167 -0.0255 0.2706 0.055 Uiso 1 1 calc R . . C29 C 0.1244(5) 0.0090(3) 0.3454(3) 0.0433(14) Uani 1 1 d . . . H29 H 0.1409 -0.0307 0.3659 0.052 Uiso 1 1 calc R A . C30 C 0.1715(5) 0.0628(2) 0.3707(3) 0.0396(13) Uani 1 1 d . A . H30 H 0.2219 0.0601 0.4090 0.047 Uiso 1 1 calc R . . C31 C 0.4099(5) 0.3203(2) 0.1297(3) 0.0372(13) Uani 1 1 d . A . H31 H 0.3772 0.3130 0.0867 0.045 Uiso 1 1 calc R . . C32 C 0.5245(5) 0.3391(3) 0.1360(3) 0.0417(14) Uani 1 1 d . . . H32 H 0.5686 0.3462 0.0985 0.050 Uiso 1 1 calc R A . C33 C 0.5732(5) 0.3472(3) 0.1995(3) 0.0405(13) Uani 1 1 d . A . H33 H 0.6522 0.3595 0.2064 0.049 Uiso 1 1 calc R . . C34 C 0.5052(5) 0.3372(2) 0.2520(3) 0.0361(12) Uani 1 1 d . . . H34 H 0.5378 0.3422 0.2954 0.043 Uiso 1 1 calc R A . C35 C 0.3880(5) 0.3195(2) 0.2425(2) 0.0320(12) Uani 1 1 d . A . C36 C 0.3365(5) 0.3273(2) 0.3563(2) 0.0333(12) Uani 1 1 d . A . C37 C 0.3829(5) 0.3864(3) 0.3721(3) 0.0435(14) Uani 1 1 d . . . H37 H 0.4040 0.4142 0.3380 0.052 Uiso 1 1 calc R A . C38 C 0.3985(5) 0.4051(3) 0.4365(3) 0.0481(16) Uani 1 1 d . A . H38 H 0.4329 0.4449 0.4472 0.058 Uiso 1 1 calc R . . C39 C 0.3633(6) 0.3649(3) 0.4858(3) 0.0492(16) Uani 1 1 d . . . H39 H 0.3740 0.3763 0.5308 0.059 Uiso 1 1 calc R A . C40 C 0.3125(6) 0.3080(3) 0.4675(3) 0.0464(15) Uani 1 1 d . A . H40 H 0.2860 0.2810 0.5009 0.056 Uiso 1 1 calc R . . P1 P 0.70613(15) 0.47931(9) 0.36772(9) 0.0556(5) Uani 1 1 d . . . F1 F 0.8389(4) 0.4738(3) 0.3843(3) 0.1131(19) Uani 1 1 d D . . F2 F 0.7287(5) 0.4489(4) 0.2985(2) 0.161(3) Uani 1 1 d . . . F3 F 0.6812(4) 0.40815(18) 0.3924(2) 0.0957(15) Uani 1 1 d . . . F4 F 0.5719(3) 0.4855(2) 0.3487(2) 0.0891(15) Uani 1 1 d . . . F5 F 0.6851(4) 0.5037(2) 0.4393(2) 0.0856(13) Uani 1 1 d . . . F6 F 0.7270(4) 0.5493(3) 0.3441(3) 0.134(2) Uani 1 1 d . . . C41 C 0.5635(10) 0.0987(4) 0.0501(4) 0.118(4) Uani 1 1 d D . . H41A H 0.5034 0.0689 0.0642 0.142 Uiso 0.631(6) 1 calc PR B 3 H41B H 0.6375 0.0874 0.0740 0.142 Uiso 0.631(6) 1 calc PR B 3 H41C H 0.6490 0.0963 0.0478 0.142 Uiso 0.369(6) 1 d PR B 4 H41D H 0.5396 0.0682 0.0838 0.142 Uiso 0.369(6) 1 d PR B 4 Cl3 Cl 0.52470(16) 0.17549(9) 0.07254(9) 0.0679(5) Uani 1 1 d D B . Cl4 Cl 0.5806(5) 0.0882(2) -0.03636(19) 0.0896(13) Uani 0.631(6) 1 d PD B 3 Cl4' Cl 0.5138(8) 0.0828(4) -0.0190(3) 0.0896(13) Uani 0.369(6) 1 d PD B 4 C42 C 0.8501(12) -0.0110(6) 0.4345(5) 0.064(4) Uani 0.50 1 d PD C 1 H42A H 0.8239 -0.0457 0.4630 0.076 Uiso 0.50 1 calc PR C 1 H42B H 0.9314 -0.0204 0.4243 0.076 Uiso 0.50 1 calc PR C 1 Cl5 Cl 0.8497(5) 0.05689(18) 0.4783(3) 0.1115(19) Uani 0.50 1 d PD C 1 Cl6 Cl 0.7676(4) -0.0137(2) 0.3624(2) 0.0898(14) Uani 0.50 1 d PD C 1 O1 O 0.5000 0.0000 0.5000 0.227(7) Uiso 1 2 d SD . 2 C43 C 0.289(3) 0.009(3) 0.575(2) 0.34(2) Uiso 0.50 1 d PD . 2 H43A H 0.2768 0.0403 0.6081 0.515 Uiso 0.50 1 d PR . 2 H43B H 0.2309 0.0145 0.5395 0.515 Uiso 0.50 1 d PR . 2 H43C H 0.2819 -0.0325 0.5931 0.515 Uiso 0.50 1 d PR . 2 C44 C 0.4037(18) 0.0124(11) 0.5423(11) 0.139(9) Uiso 0.50 1 d PD . 2 H44A H 0.3982 0.0567 0.5321 0.167 Uiso 0.50 1 d PR . 2 H44B H 0.4473 0.0115 0.5837 0.167 Uiso 0.50 1 d PR . 2 C45 C 0.6297(14) 0.0115(11) 0.5113(11) 0.126(7) Uiso 0.50 1 d PD . 2 H45A H 0.6508 -0.0222 0.5412 0.151 Uiso 0.50 1 d PR . 2 H45B H 0.6298 0.0489 0.5381 0.151 Uiso 0.50 1 d PR . 2 C46 C 0.746(3) 0.020(3) 0.476(2) 0.34(2) Uiso 0.50 1 d PD . 2 H46A H 0.8111 0.0268 0.5066 0.515 Uiso 0.50 1 d PR . 2 H46B H 0.7597 -0.0172 0.4504 0.515 Uiso 0.50 1 d PR . 2 H46C H 0.7380 0.0561 0.4471 0.515 Uiso 0.50 1 d PR . 2 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 M1 0.0252(3) 0.0219(2) 0.0169(2) -0.00034(17) -0.00015(18) -0.00241(18) M2 0.0223(3) 0.0253(3) 0.0189(2) -0.00044(17) 0.00069(18) 0.00060(18) M2' 0.0252(3) 0.0219(2) 0.0169(2) -0.00034(17) -0.00015(18) -0.00241(18) M1' 0.0223(3) 0.0253(3) 0.0189(2) -0.00044(17) 0.00069(18) 0.00060(18) Co2 0.0211(3) 0.0181(3) 0.0134(3) 0.0010(2) -0.0014(2) -0.0020(2) Cl1 0.0489(9) 0.0448(8) 0.0288(7) 0.0024(6) -0.0006(6) -0.0038(6) Cl2 0.0386(8) 0.0524(8) 0.0281(7) 0.0058(6) 0.0030(6) 0.0052(6) N1 0.035(3) 0.038(2) 0.025(2) -0.0036(18) -0.0017(19) 0.0059(19) N2 0.036(3) 0.031(2) 0.025(2) 0.0002(17) -0.0003(19) -0.0016(18) N3 0.037(3) 0.033(2) 0.029(2) 0.0023(18) -0.002(2) -0.0041(19) N4 0.033(3) 0.033(2) 0.032(2) 0.0025(18) 0.004(2) -0.0002(19) N5 0.034(3) 0.030(2) 0.030(2) 0.0064(18) 0.0051(19) 0.0006(18) N6 0.036(3) 0.036(2) 0.026(2) -0.0003(18) 0.0032(19) -0.0012(19) N7 0.034(3) 0.036(2) 0.023(2) -0.0024(18) -0.0017(19) 0.0012(19) N8 0.033(3) 0.033(2) 0.029(2) 0.0030(18) -0.0015(19) -0.0013(19) N9 0.039(3) 0.031(2) 0.031(2) 0.0053(18) 0.002(2) -0.0005(19) N10 0.032(3) 0.034(2) 0.025(2) 0.0013(17) 0.0012(19) 0.0006(18) N11 0.038(3) 0.034(2) 0.026(2) -0.0015(18) 0.003(2) -0.0023(19) N12 0.045(3) 0.030(2) 0.025(2) -0.0065(17) -0.003(2) -0.0044(19) C1 0.050(4) 0.049(4) 0.027(3) -0.007(2) -0.004(3) 0.002(3) C2 0.059(4) 0.058(4) 0.048(4) -0.020(3) -0.007(3) 0.002(3) C3 0.061(4) 0.039(3) 0.059(4) -0.021(3) -0.013(3) 0.007(3) C4 0.050(4) 0.038(3) 0.044(4) -0.006(3) -0.009(3) 0.003(3) C5 0.030(3) 0.034(3) 0.033(3) -0.002(2) 0.002(2) 0.000(2) C6 0.035(3) 0.026(3) 0.030(3) 0.003(2) 0.001(2) -0.003(2) C7 0.038(3) 0.041(3) 0.032(3) 0.002(2) 0.000(2) -0.002(2) C8 0.036(3) 0.052(4) 0.045(4) 0.005(3) 0.001(3) 0.004(3) C9 0.037(4) 0.062(4) 0.042(4) 0.013(3) -0.011(3) -0.004(3) C10 0.037(3) 0.051(3) 0.031(3) 0.005(2) -0.005(3) -0.003(3) C11 0.044(4) 0.041(3) 0.038(3) 0.008(2) 0.007(3) -0.005(3) C12 0.064(4) 0.027(3) 0.049(4) 0.005(2) 0.011(3) 0.004(3) C13 0.047(4) 0.034(3) 0.056(4) -0.002(3) 0.008(3) 0.007(3) C14 0.051(4) 0.032(3) 0.039(3) -0.005(2) 0.011(3) -0.003(3) C15 0.035(3) 0.033(3) 0.029(3) -0.001(2) 0.000(2) -0.001(2) C16 0.033(3) 0.031(3) 0.027(3) -0.003(2) 0.000(2) -0.002(2) C17 0.034(3) 0.036(3) 0.040(3) 0.002(2) 0.003(3) -0.001(2) C18 0.037(3) 0.051(4) 0.048(4) 0.000(3) 0.013(3) 0.001(3) C19 0.039(3) 0.055(4) 0.037(3) 0.007(3) 0.011(3) -0.007(3) C20 0.039(3) 0.048(3) 0.029(3) 0.008(2) 0.005(2) -0.004(3) C21 0.038(3) 0.045(3) 0.026(3) 0.003(2) -0.001(2) 0.005(3) C22 0.033(3) 0.061(4) 0.034(3) 0.000(3) 0.004(3) 0.004(3) C23 0.028(3) 0.079(4) 0.044(4) 0.015(3) -0.003(3) -0.007(3) C24 0.042(4) 0.058(4) 0.038(3) 0.008(3) 0.000(3) -0.014(3) C25 0.032(3) 0.036(3) 0.030(3) -0.001(2) -0.001(2) -0.001(2) C26 0.039(3) 0.035(3) 0.026(3) 0.002(2) -0.001(2) -0.005(2) C27 0.051(4) 0.037(3) 0.039(3) -0.001(2) -0.011(3) -0.014(3) C28 0.059(4) 0.037(3) 0.042(3) -0.001(3) 0.005(3) -0.010(3) C29 0.060(4) 0.029(3) 0.041(3) 0.003(2) 0.006(3) -0.001(3) C30 0.049(4) 0.038(3) 0.031(3) 0.006(2) 0.003(3) 0.005(3) C31 0.041(3) 0.045(3) 0.026(3) -0.003(2) 0.002(2) 0.004(3) C32 0.037(3) 0.054(4) 0.036(3) -0.001(3) 0.014(3) 0.002(3) C33 0.032(3) 0.042(3) 0.047(4) -0.003(3) 0.007(3) 0.002(2) C34 0.039(3) 0.037(3) 0.032(3) -0.001(2) -0.003(2) 0.002(2) C35 0.039(3) 0.026(3) 0.031(3) 0.001(2) 0.000(2) 0.003(2) C36 0.036(3) 0.036(3) 0.028(3) -0.004(2) 0.003(2) -0.005(2) C37 0.049(4) 0.038(3) 0.044(3) -0.005(3) 0.012(3) -0.005(3) C38 0.063(4) 0.047(4) 0.034(3) -0.012(3) 0.007(3) -0.017(3) C39 0.065(4) 0.046(4) 0.036(3) -0.008(3) 0.003(3) -0.012(3) C40 0.070(5) 0.044(3) 0.025(3) -0.002(2) 0.002(3) -0.003(3) P1 0.0467(11) 0.0713(12) 0.0477(10) -0.0072(9) -0.0104(8) 0.0057(9) F1 0.051(3) 0.152(4) 0.134(4) -0.071(4) -0.022(3) 0.029(3) F2 0.118(5) 0.294(9) 0.073(4) -0.085(5) 0.023(3) -0.065(5) F3 0.116(4) 0.047(2) 0.120(4) -0.007(2) -0.035(3) 0.015(2) F4 0.051(2) 0.088(3) 0.125(4) 0.057(3) -0.029(3) -0.015(2) F5 0.109(4) 0.084(3) 0.065(3) -0.018(2) 0.006(3) 0.010(3) F6 0.096(4) 0.135(5) 0.166(5) 0.086(4) -0.056(4) -0.064(3) C41 0.172(11) 0.108(7) 0.080(6) 0.026(6) 0.061(7) 0.051(7) Cl3 0.0641(12) 0.0739(12) 0.0651(12) 0.0032(9) -0.0018(9) 0.0100(9) Cl4 0.123(4) 0.099(2) 0.047(2) -0.0112(16) 0.0079(19) 0.002(3) Cl4' 0.123(4) 0.099(2) 0.047(2) -0.0112(16) 0.0079(19) 0.002(3) C42 0.071(10) 0.069(9) 0.050(8) 0.020(7) -0.004(7) -0.028(8) Cl5 0.151(5) 0.046(2) 0.131(4) -0.004(2) -0.060(4) 0.009(3) Cl6 0.096(3) 0.094(3) 0.077(3) -0.019(2) -0.015(3) 0.046(3) _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 M1 N3 2.034(4) . ? M1 N9 2.039(4) . ? M1 N12 2.072(4) . ? M1 N6 2.090(4) . ? M1 Co2 2.3455(7) . ? M1 Cl1 2.4281(13) . ? M2 N1 2.041(4) . ? M2 N7 2.056(4) . ? M2 N10 2.065(4) . ? M2 N4 2.071(4) . ? M2 Co2 2.3527(7) . ? M2 Cl2 2.4240(13) . ? Co2 N5 1.886(4) . ? Co2 N11 1.901(4) . ? Co2 N8 1.930(4) . ? Co2 N2 1.946(4) . ? N1 C1 1.351(6) . ? N1 C5 1.358(6) . ? N2 C6 1.373(6) . ? N2 C5 1.377(6) . ? N3 C10 1.337(6) . ? N3 C6 1.359(6) . ? N4 C11 1.339(6) . ? N4 C15 1.375(6) . ? N5 C16 1.388(6) . ? N5 C15 1.392(6) . ? N6 C20 1.347(6) . ? N6 C16 1.367(6) . ? N7 C21 1.354(6) . ? N7 C25 1.376(6) . ? N8 C26 1.386(6) . ? N8 C25 1.387(6) . ? N9 C26 1.356(6) . ? N9 C30 1.377(6) . ? N10 C31 1.348(6) . ? N10 C35 1.359(6) . ? N11 C35 1.382(6) . ? N11 C36 1.384(6) . ? N12 C40 1.344(6) . ? N12 C36 1.362(6) . ? C1 C2 1.359(8) . ? C2 C3 1.397(8) . ? C3 C4 1.367(8) . ? C4 C5 1.414(7) . ? C6 C7 1.400(7) . ? C7 C8 1.379(7) . ? C8 C9 1.383(8) . ? C9 C10 1.379(8) . ? C11 C12 1.378(8) . ? C12 C13 1.375(8) . ? C13 C14 1.380(7) . ? C14 C15 1.379(7) . ? C16 C17 1.405(7) . ? C17 C18 1.379(7) . ? C18 C19 1.386(8) . ? C19 C20 1.359(8) . ? C21 C22 1.382(7) . ? C22 C23 1.382(8) . ? C23 C24 1.380(8) . ? C24 C25 1.391(7) . ? C26 C27 1.394(7) . ? C27 C28 1.379(7) . ? C28 C29 1.397(8) . ? C29 C30 1.350(7) . ? C31 C32 1.379(7) . ? C32 C33 1.397(8) . ? C33 C34 1.373(7) . ? C34 C35 1.406(7) . ? C36 C37 1.388(7) . ? C37 C38 1.375(7) . ? C38 C39 1.390(8) . ? C39 C40 1.378(8) . ? P1 F1 1.556(4) . ? P1 F6 1.575(5) . ? P1 F5 1.576(4) . ? P1 F2 1.582(5) . ? P1 F4 1.582(4) . ? P1 F3 1.613(5) . ? C41 Cl4' 1.530(10) . ? C41 Cl3 1.747(8) . ? C41 Cl4 1.795(8) . ? C42 Cl5 1.688(12) . ? C42 Cl6 1.710(11) . ? O1 C44 1.462(17) . ? O1 C44 1.462(17) 3_656 ? O1 C45 1.521(16) . ? O1 C45 1.522(16) 3_656 ? C43 C46 1.25(7) 3_656 ? C43 C44 1.51(2) . ? C44 C45 1.25(3) 3_656 ? C44 C46 1.88(5) 3_656 ? C45 C44 1.25(3) 3_656 ? C45 C46 1.57(2) . ? C46 C43 1.25(7) 3_656 ? C46 C44 1.88(5) 3_656 ? 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 M1 N9 89.53(17) . . ? N3 M1 N12 88.52(17) . . ? N9 M1 N12 171.11(16) . . ? N3 M1 N6 169.64(16) . . ? N9 M1 N6 87.87(17) . . ? N12 M1 N6 92.51(17) . . ? N3 M1 Co2 87.51(12) . . ? N9 M1 Co2 86.67(12) . . ? N12 M1 Co2 84.58(11) . . ? N6 M1 Co2 82.33(11) . . ? N3 M1 Cl1 95.66(12) . . ? N9 M1 Cl1 93.58(12) . . ? N12 M1 Cl1 95.24(12) . . ? N6 M1 Cl1 94.52(12) . . ? Co2 M1 Cl1 176.83(4) . . ? N1 M2 N7 89.39(17) . . ? N1 M2 N10 91.60(16) . . ? N7 M2 N10 169.64(16) . . ? N1 M2 N4 170.50(16) . . ? N7 M2 N4 87.52(16) . . ? N10 M2 N4 89.85(16) . . ? N1 M2 Co2 87.27(11) . . ? N7 M2 Co2 85.44(11) . . ? N10 M2 Co2 84.30(11) . . ? N4 M2 Co2 83.52(11) . . ? N1 M2 Cl2 95.15(12) . . ? N7 M2 Cl2 94.67(11) . . ? N10 M2 Cl2 95.51(12) . . ? N4 M2 Cl2 94.06(12) . . ? Co2 M2 Cl2 177.57(4) . . ? N5 Co2 N11 91.01(18) . . ? N5 Co2 N8 89.96(18) . . ? N11 Co2 N8 179.02(18) . . ? N5 Co2 N2 178.03(17) . . ? N11 Co2 N2 90.95(18) . . ? N8 Co2 N2 88.08(18) . . ? N5 Co2 M1 92.91(12) . . ? N11 Co2 M1 91.28(12) . . ? N8 Co2 M1 88.53(12) . . ? N2 Co2 M1 87.27(12) . . ? N5 Co2 M2 92.03(12) . . ? N11 Co2 M2 91.05(12) . . ? N8 Co2 M2 89.06(12) . . ? N2 Co2 M2 87.72(12) . . ? M1 Co2 M2 174.50(3) . . ? C1 N1 C5 119.5(5) . . ? C1 N1 M2 121.7(4) . . ? C5 N1 M2 118.0(3) . . ? C6 N2 C5 122.5(4) . . ? C6 N2 Co2 119.9(3) . . ? C5 N2 Co2 117.4(3) . . ? C10 N3 C6 119.4(5) . . ? C10 N3 M1 122.7(4) . . ? C6 N3 M1 117.9(3) . . ? C11 N4 C15 118.0(4) . . ? C11 N4 M2 121.3(4) . . ? C15 N4 M2 120.6(3) . . ? C16 N5 C15 123.5(4) . . ? C16 N5 Co2 116.6(3) . . ? C15 N5 Co2 119.3(3) . . ? C20 N6 C16 118.1(5) . . ? C20 N6 M1 120.5(4) . . ? C16 N6 M1 121.2(3) . . ? C21 N7 C25 118.3(5) . . ? C21 N7 M2 121.8(3) . . ? C25 N7 M2 119.5(3) . . ? C26 N8 C25 121.8(4) . . ? C26 N8 Co2 120.2(3) . . ? C25 N8 Co2 118.0(3) . . ? C26 N9 C30 118.5(4) . . ? C26 N9 M1 119.5(3) . . ? C30 N9 M1 122.0(4) . . ? C31 N10 C35 118.3(4) . . ? C31 N10 M2 121.2(3) . . ? C35 N10 M2 120.4(3) . . ? C35 N11 C36 122.8(4) . . ? C35 N11 Co2 117.9(3) . . ? C36 N11 Co2 118.9(3) . . ? C40 N12 C36 119.0(4) . . ? C40 N12 M1 120.9(4) . . ? C36 N12 M1 120.1(3) . . ? N1 C1 C2 122.3(5) . . ? C1 C2 C3 119.6(6) . . ? C4 C3 C2 118.7(6) . . ? C3 C4 C5 120.1(5) . . ? N1 C5 N2 116.6(4) . . ? N1 C5 C4 119.7(5) . . ? N2 C5 C4 123.4(5) . . ? N3 C6 N2 116.3(4) . . ? N3 C6 C7 119.9(5) . . ? N2 C6 C7 123.7(5) . . ? C8 C7 C6 120.0(5) . . ? C7 C8 C9 119.3(6) . . ? C10 C9 C8 118.4(5) . . ? N3 C10 C9 122.9(5) . . ? N4 C11 C12 123.7(5) . . ? C13 C12 C11 117.9(5) . . ? C12 C13 C14 119.8(5) . . ? C15 C14 C13 119.8(5) . . ? N4 C15 C14 120.6(5) . . ? N4 C15 N5 114.8(4) . . ? C14 C15 N5 124.5(5) . . ? N6 C16 N5 115.0(4) . . ? N6 C16 C17 120.7(5) . . ? N5 C16 C17 123.9(5) . . ? C18 C17 C16 119.1(5) . . ? C17 C18 C19 119.7(5) . . ? C20 C19 C18 118.5(5) . . ? N6 C20 C19 123.9(5) . . ? N7 C21 C22 122.4(5) . . ? C21 C22 C23 119.1(5) . . ? C24 C23 C22 119.7(6) . . ? C23 C24 C25 119.4(5) . . ? N7 C25 N8 114.8(4) . . ? N7 C25 C24 121.1(5) . . ? N8 C25 C24 123.8(5) . . ? N9 C26 N8 115.2(4) . . ? N9 C26 C27 120.8(5) . . ? N8 C26 C27 123.7(5) . . ? C28 C27 C26 119.9(5) . . ? C27 C28 C29 118.8(5) . . ? C30 C29 C28 119.6(5) . . ? C29 C30 N9 122.4(5) . . ? N10 C31 C32 124.5(5) . . ? C31 C32 C33 117.4(5) . . ? C34 C33 C32 118.9(5) . . ? C33 C34 C35 121.1(5) . . ? N10 C35 N11 115.8(5) . . ? N10 C35 C34 119.8(5) . . ? N11 C35 C34 124.3(5) . . ? N12 C36 N11 115.7(4) . . ? N12 C36 C37 119.9(5) . . ? N11 C36 C37 124.1(5) . . ? C38 C37 C36 120.6(5) . . ? C37 C38 C39 119.1(5) . . ? C40 C39 C38 118.0(5) . . ? N12 C40 C39 123.2(5) . . ? F1 P1 F6 88.4(3) . . ? F1 P1 F5 91.0(3) . . ? F6 P1 F5 90.5(3) . . ? F1 P1 F2 87.7(3) . . ? F6 P1 F2 94.2(4) . . ? F5 P1 F2 175.1(4) . . ? F1 P1 F4 178.3(3) . . ? F6 P1 F4 90.6(2) . . ? F5 P1 F4 90.3(3) . . ? F2 P1 F4 91.0(3) . . ? F1 P1 F3 93.0(3) . . ? F6 P1 F3 178.4(3) . . ? F5 P1 F3 88.7(3) . . ? F2 P1 F3 86.6(3) . . ? F4 P1 F3 88.0(2) . . ? Cl4' C41 Cl3 110.8(6) . . ? Cl4' C41 Cl4 29.0(3) . . ? Cl3 C41 Cl4 114.4(5) . . ? Cl5 C42 Cl6 117.7(8) . . ? C44 O1 C44 179.998(5) . 3_656 ? C44 O1 C45 130.6(12) . . ? C44 O1 C45 49.4(12) 3_656 . ? C44 O1 C45 49.4(12) . 3_656 ? C44 O1 C45 130.6(12) 3_656 3_656 ? C45 O1 C45 179.997(2) . 3_656 ? C46 C43 C44 85(3) 3_656 . ? C45 C44 O1 67.8(13) 3_656 . ? C45 C44 C43 97(3) 3_656 . ? O1 C44 C43 163(3) . . ? C45 C44 C46 55.9(16) 3_656 3_656 ? O1 C44 C46 122(2) . 3_656 ? C43 C44 C46 41(2) . 3_656 ? C44 C45 O1 62.8(11) 3_656 . ? C44 C45 C46 83(2) 3_656 . ? O1 C45 C46 144(3) . . ? C43 C46 C45 94(3) 3_656 . ? C43 C46 C44 53(2) 3_656 3_656 ? C45 C46 C44 41.1(14) . 3_656 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.523 _refine_diff_density_min -0.809 _refine_diff_density_rms 0.137 _database_code_depnum_ccdc_archive 'CCDC 939272' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ic15630 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H36 Cl5 Co F6 N12 Ni P Rh' _chemical_formula_weight 1251.60 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' 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' Ni Ni 0.3393 1.1124 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.7300(10) _cell_length_b 17.2013(8) _cell_length_c 15.5306(8) _cell_angle_alpha 90.00 _cell_angle_beta 110.081(3) _cell_angle_gamma 90.00 _cell_volume 4699.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 17281 _cell_measurement_theta_min 1.66 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.769 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2504 _exptl_absorpt_coefficient_mu 1.483 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.626 _exptl_absorpt_correction_T_max 0.768 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'NONIUS KappaCCD' _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 17281 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5347 _reflns_number_gt 3675 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _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^)+(0.0754P)^2^+6.7405P] 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 5347 _refine_ls_number_parameters 315 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1533 _refine_ls_wR_factor_gt 0.1364 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.118 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh Rh 0.0000 0.36574(3) 0.2500 0.02826(15) Uani 1 2 d S . . Ni Ni 0.0000 0.09466(4) 0.2500 0.0273(2) Uani 1 2 d S . . Co Co 0.0000 0.22988(4) 0.2500 0.0251(2) Uani 1 2 d S . . Cl1 Cl 0.0000 0.51554(9) 0.2500 0.0391(4) Uani 1 2 d S . . N1 N 0.1097(2) 0.3582(2) 0.2477(3) 0.0304(8) Uani 1 1 d . . . N2 N 0.0853(2) 0.2280(2) 0.2088(3) 0.0369(9) Uani 1 1 d . . . N3 N 0.0536(2) 0.0997(2) 0.1642(3) 0.0317(8) Uani 1 1 d . . . N4 N 0.0437(2) 0.3574(2) 0.3943(2) 0.0304(8) Uani 1 1 d . . . N5 N 0.0669(2) 0.2265(2) 0.3763(3) 0.0376(9) Uani 1 1 d . . . N6 N 0.0958(2) 0.09921(19) 0.3481(3) 0.0318(8) Uani 1 1 d . . . C1 C 0.1569(3) 0.4199(3) 0.2666(4) 0.0407(12) Uani 1 1 d . . . H1 H 0.1375 0.4688 0.2765 0.049 Uiso 1 1 calc R . . C2 C 0.2313(3) 0.4157(3) 0.2724(4) 0.0472(13) Uani 1 1 d . . . H2 H 0.2617 0.4613 0.2821 0.057 Uiso 1 1 calc R . . C3 C 0.2615(3) 0.3438(3) 0.2636(3) 0.0427(12) Uani 1 1 d . . . H3 H 0.3136 0.3389 0.2701 0.051 Uiso 1 1 calc R . . C4 C 0.2150(3) 0.2798(3) 0.2455(4) 0.0417(12) Uani 1 1 d . . . H4 H 0.2353 0.2298 0.2418 0.050 Uiso 1 1 calc R . . C5 C 0.1373(3) 0.2882(3) 0.2324(4) 0.0387(11) Uani 1 1 d . . . C6 C 0.0919(3) 0.1658(3) 0.1561(3) 0.0380(11) Uani 1 1 d . . . C7 C 0.1296(3) 0.1665(3) 0.0907(4) 0.0448(12) Uani 1 1 d . . . H7 H 0.1540 0.2127 0.0820 0.054 Uiso 1 1 calc R . . C8 C 0.1314(3) 0.1017(3) 0.0400(3) 0.0426(12) Uani 1 1 d . . . H8 H 0.1549 0.1033 -0.0053 0.051 Uiso 1 1 calc R . . C9 C 0.0981(3) 0.0341(3) 0.0563(3) 0.0420(12) Uani 1 1 d . . . H9 H 0.1024 -0.0129 0.0265 0.050 Uiso 1 1 calc R . . C10 C 0.0592(3) 0.0362(3) 0.1158(3) 0.0406(12) Uani 1 1 d . . . H10 H 0.0343 -0.0100 0.1238 0.049 Uiso 1 1 calc R . . C11 C 0.0499(3) 0.4194(3) 0.4493(3) 0.0374(11) Uani 1 1 d . . . H11 H 0.0380 0.4691 0.4216 0.045 Uiso 1 1 calc R . . C12 C 0.0726(3) 0.4148(3) 0.5441(3) 0.0424(12) Uani 1 1 d . . . H12 H 0.0779 0.4607 0.5799 0.051 Uiso 1 1 calc R . . C13 C 0.0876(3) 0.3427(3) 0.5860(3) 0.0422(12) Uani 1 1 d . . . H13 H 0.0997 0.3376 0.6504 0.051 Uiso 1 1 calc R . . C14 C 0.0846(3) 0.2790(3) 0.5319(3) 0.0429(12) Uani 1 1 d . . . H14 H 0.0945 0.2289 0.5591 0.051 Uiso 1 1 calc R . . C15 C 0.0667(3) 0.2868(3) 0.4350(3) 0.0376(11) Uani 1 1 d . . . C16 C 0.1157(3) 0.1644(3) 0.4027(3) 0.0385(11) Uani 1 1 d . . . C17 C 0.1881(3) 0.1664(3) 0.4746(4) 0.0433(12) Uani 1 1 d . . . H17 H 0.2020 0.2094 0.5153 0.052 Uiso 1 1 calc R . . C18 C 0.2373(3) 0.1052(3) 0.4839(3) 0.0428(12) Uani 1 1 d . . . H18 H 0.2866 0.1076 0.5291 0.051 Uiso 1 1 calc R . . C19 C 0.2163(3) 0.0408(3) 0.4290(4) 0.0431(12) Uani 1 1 d . . . H19 H 0.2500 -0.0019 0.4363 0.052 Uiso 1 1 calc R . . C20 C 0.1449(3) 0.0399(3) 0.3631(3) 0.0390(11) Uani 1 1 d . . . H20 H 0.1297 -0.0052 0.3261 0.047 Uiso 1 1 calc R . . P1 P 0.0000 -0.15711(10) 0.2500 0.0428(5) Uani 1 2 d S . . F1 F 0.0000 -0.0630(2) 0.2500 0.0463(10) Uani 1 2 d S . . F2 F 0.0000 -0.2503(2) 0.2500 0.0684(14) Uani 1 2 d S . . F3 F -0.08521(18) -0.15596(17) 0.1792(2) 0.0627(9) Uani 1 1 d . . . F4 F -0.0301(2) -0.15590(19) 0.3353(2) 0.0677(10) Uani 1 1 d . . . C21 C 0.3950(3) 0.1582(3) 0.0907(4) 0.0538(14) Uani 1 1 d . . . H21A H 0.4405 0.1296 0.1297 0.065 Uiso 1 1 calc R . . H21B H 0.4085 0.2139 0.0916 0.065 Uiso 1 1 calc R . . Cl2 Cl 0.32102(11) 0.14688(17) 0.13530(16) 0.1166(9) Uani 1 1 d . . . Cl3 Cl 0.36736(9) 0.12254(8) -0.02340(10) 0.0590(4) 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 Rh 0.0269(3) 0.0259(3) 0.0295(3) 0.000 0.0066(2) 0.000 Ni 0.0244(4) 0.0257(4) 0.0283(4) 0.000 0.0047(3) 0.000 Co 0.0220(4) 0.0233(4) 0.0265(4) 0.000 0.0039(3) 0.000 Cl1 0.0440(9) 0.0296(8) 0.0415(10) 0.000 0.0116(8) 0.000 N1 0.0289(19) 0.0299(18) 0.031(2) -0.0029(16) 0.0091(16) -0.0034(15) N2 0.038(2) 0.031(2) 0.039(2) -0.0024(17) 0.0094(18) -0.0022(17) N3 0.030(2) 0.0292(19) 0.034(2) -0.0006(16) 0.0078(17) 0.0008(16) N4 0.030(2) 0.0315(18) 0.028(2) -0.0007(15) 0.0066(16) 0.0011(16) N5 0.036(2) 0.033(2) 0.038(2) 0.0017(17) 0.0062(18) 0.0018(17) N6 0.030(2) 0.0244(18) 0.038(2) 0.0010(15) 0.0080(17) -0.0002(15) C1 0.037(3) 0.037(2) 0.047(3) -0.005(2) 0.013(2) -0.006(2) C2 0.039(3) 0.040(3) 0.058(4) -0.007(2) 0.011(3) -0.015(2) C3 0.028(2) 0.055(3) 0.041(3) -0.004(2) 0.007(2) -0.009(2) C4 0.029(3) 0.045(3) 0.049(3) -0.003(2) 0.011(2) 0.004(2) C5 0.034(3) 0.038(2) 0.046(3) -0.001(2) 0.015(2) -0.004(2) C6 0.039(3) 0.037(3) 0.035(3) 0.001(2) 0.009(2) 0.002(2) C7 0.054(3) 0.041(3) 0.043(3) -0.001(2) 0.021(3) -0.005(2) C8 0.050(3) 0.045(3) 0.038(3) -0.005(2) 0.021(3) 0.000(2) C9 0.050(3) 0.036(3) 0.040(3) -0.006(2) 0.016(3) 0.003(2) C10 0.048(3) 0.028(2) 0.044(3) -0.001(2) 0.013(2) -0.003(2) C11 0.042(3) 0.030(2) 0.037(3) -0.004(2) 0.009(2) 0.004(2) C12 0.049(3) 0.038(2) 0.038(3) -0.009(2) 0.011(2) 0.006(2) C13 0.040(3) 0.053(3) 0.030(3) -0.006(2) 0.007(2) 0.004(2) C14 0.051(3) 0.042(3) 0.032(3) 0.005(2) 0.010(2) -0.001(2) C15 0.039(3) 0.036(2) 0.034(3) -0.002(2) 0.006(2) -0.003(2) C16 0.040(3) 0.033(2) 0.041(3) 0.002(2) 0.012(2) -0.002(2) C17 0.036(3) 0.047(3) 0.040(3) -0.002(2) 0.005(2) -0.005(2) C18 0.026(3) 0.049(3) 0.043(3) 0.008(2) -0.001(2) 0.002(2) C19 0.036(3) 0.040(3) 0.049(3) 0.004(2) 0.010(2) 0.010(2) C20 0.037(3) 0.031(2) 0.044(3) 0.001(2) 0.008(2) 0.004(2) P1 0.0410(11) 0.0381(10) 0.0438(11) 0.000 0.0075(9) 0.000 F1 0.052(3) 0.036(2) 0.055(3) 0.000 0.024(2) 0.000 F2 0.077(3) 0.037(2) 0.067(3) 0.000 -0.005(3) 0.000 F3 0.0457(18) 0.0570(19) 0.068(2) 0.0035(16) -0.0031(16) -0.0023(15) F4 0.080(2) 0.068(2) 0.062(2) 0.0078(17) 0.035(2) -0.0093(18) C21 0.048(3) 0.052(3) 0.049(3) -0.004(3) -0.001(3) 0.008(3) Cl2 0.0596(12) 0.201(3) 0.0890(16) -0.0426(16) 0.0258(11) 0.0117(13) Cl3 0.0719(10) 0.0499(8) 0.0488(8) -0.0036(6) 0.0124(7) -0.0104(7) _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 Rh N1 2.072(4) 2 ? Rh N1 2.072(4) . ? Rh N4 2.110(4) . ? Rh N4 2.110(4) 2 ? Rh Co 2.3371(8) . ? Rh Cl1 2.5767(16) . ? Ni N6 1.916(4) 2 ? Ni N6 1.916(4) . ? Ni N3 1.925(4) 2 ? Ni N3 1.925(4) . ? Ni Co 2.3259(10) . ? Co N2 1.914(4) 2 ? Co N2 1.914(4) . ? Co N5 1.932(4) 2 ? Co N5 1.932(4) . ? N1 C1 1.347(6) . ? N1 C5 1.364(6) . ? N2 C6 1.378(6) . ? N2 C5 1.383(6) . ? N3 C10 1.350(6) . ? N3 C6 1.374(6) . ? N4 C11 1.346(5) . ? N4 C15 1.369(6) . ? N5 C16 1.374(6) . ? N5 C15 1.382(6) . ? N6 C20 1.339(5) . ? N6 C16 1.377(6) . ? C1 C2 1.367(7) . ? C2 C3 1.386(7) . ? C3 C4 1.372(7) . ? C4 C5 1.405(6) . ? C6 C7 1.423(7) . ? C7 C8 1.371(7) . ? C8 C9 1.383(7) . ? C9 C10 1.360(7) . ? C11 C12 1.387(7) . ? C12 C13 1.384(7) . ? C13 C14 1.371(7) . ? C14 C15 1.431(7) . ? C16 C17 1.431(7) . ? C17 C18 1.372(7) . ? C18 C19 1.370(7) . ? C19 C20 1.377(6) . ? P1 F3 1.597(3) 2 ? P1 F3 1.597(3) . ? P1 F2 1.602(5) . ? P1 F4 1.609(3) . ? P1 F4 1.609(3) 2 ? P1 F1 1.619(4) . ? C21 Cl2 1.760(6) . ? C21 Cl3 1.776(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Rh N1 172.81(19) 2 . ? N1 Rh N4 90.17(14) 2 . ? N1 Rh N4 89.35(14) . . ? N1 Rh N4 89.34(14) 2 2 ? N1 Rh N4 90.17(14) . 2 ? N4 Rh N4 172.22(19) . 2 ? N1 Rh Co 86.40(9) 2 . ? N1 Rh Co 86.41(9) . . ? N4 Rh Co 86.11(9) . . ? N4 Rh Co 86.11(9) 2 . ? N1 Rh Cl1 93.60(9) 2 . ? N1 Rh Cl1 93.59(9) . . ? N4 Rh Cl1 93.89(9) . . ? N4 Rh Cl1 93.89(9) 2 . ? Co Rh Cl1 180.0 . . ? N6 Ni N6 175.3(2) 2 . ? N6 Ni N3 88.85(16) 2 2 ? N6 Ni N3 90.94(16) . 2 ? N6 Ni N3 90.94(16) 2 . ? N6 Ni N3 88.85(16) . . ? N3 Ni N3 174.9(2) 2 . ? N6 Ni Co 87.66(10) 2 . ? N6 Ni Co 87.66(10) . . ? N3 Ni Co 87.45(10) 2 . ? N3 Ni Co 87.45(10) . . ? N2 Co N2 178.0(2) 2 . ? N2 Co N5 90.82(17) 2 2 ? N2 Co N5 89.12(17) . 2 ? N2 Co N5 89.12(17) 2 . ? N2 Co N5 90.82(17) . . ? N5 Co N5 176.5(2) 2 . ? N2 Co Ni 89.01(11) 2 . ? N2 Co Ni 89.01(11) . . ? N5 Co Ni 88.25(11) 2 . ? N5 Co Ni 88.26(11) . . ? N2 Co Rh 90.99(11) 2 . ? N2 Co Rh 90.99(11) . . ? N5 Co Rh 91.75(11) 2 . ? N5 Co Rh 91.74(11) . . ? Ni Co Rh 180.0 . . ? C1 N1 C5 118.3(4) . . ? C1 N1 Rh 121.8(3) . . ? C5 N1 Rh 119.8(3) . . ? C6 N2 C5 122.6(4) . . ? C6 N2 Co 117.8(3) . . ? C5 N2 Co 119.5(3) . . ? C10 N3 C6 118.4(4) . . ? C10 N3 Ni 120.6(3) . . ? C6 N3 Ni 120.9(3) . . ? C11 N4 C15 117.7(4) . . ? C11 N4 Rh 122.6(3) . . ? C15 N4 Rh 119.8(3) . . ? C16 N5 C15 122.6(4) . . ? C16 N5 Co 117.4(3) . . ? C15 N5 Co 120.0(3) . . ? C20 N6 C16 119.2(4) . . ? C20 N6 Ni 120.5(3) . . ? C16 N6 Ni 120.3(3) . . ? N1 C1 C2 123.4(5) . . ? C1 C2 C3 118.8(4) . . ? C4 C3 C2 119.0(5) . . ? C3 C4 C5 120.0(5) . . ? N1 C5 N2 115.6(4) . . ? N1 C5 C4 120.0(4) . . ? N2 C5 C4 124.2(4) . . ? N3 C6 N2 115.6(4) . . ? N3 C6 C7 118.4(4) . . ? N2 C6 C7 125.8(4) . . ? C8 C7 C6 121.3(5) . . ? C7 C8 C9 118.5(5) . . ? C10 C9 C8 118.9(4) . . ? N3 C10 C9 124.2(4) . . ? N4 C11 C12 123.9(4) . . ? C13 C12 C11 119.2(4) . . ? C14 C13 C12 118.0(5) . . ? C13 C14 C15 121.0(5) . . ? N4 C15 N5 115.7(4) . . ? N4 C15 C14 119.4(4) . . ? N5 C15 C14 124.8(4) . . ? N5 C16 N6 115.9(4) . . ? N5 C16 C17 124.8(4) . . ? N6 C16 C17 118.9(4) . . ? C18 C17 C16 119.1(5) . . ? C19 C18 C17 121.0(5) . . ? C18 C19 C20 118.0(4) . . ? N6 C20 C19 123.7(4) . . ? F3 P1 F3 178.6(2) 2 . ? F3 P1 F2 90.71(12) 2 . ? F3 P1 F2 90.71(12) . . ? F3 P1 F4 89.04(19) 2 . ? F3 P1 F4 90.94(19) . . ? F2 P1 F4 90.74(13) . . ? F3 P1 F4 90.94(19) 2 2 ? F3 P1 F4 89.04(19) . 2 ? F2 P1 F4 90.74(13) . 2 ? F4 P1 F4 178.5(3) . 2 ? F3 P1 F1 89.29(12) 2 . ? F3 P1 F1 89.29(12) . . ? F2 P1 F1 180.0 . . ? F4 P1 F1 89.26(13) . . ? F4 P1 F1 89.26(13) 2 . ? Cl2 C21 Cl3 110.8(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.176 _refine_diff_density_min -1.123 _refine_diff_density_rms 0.110 _database_code_depnum_ccdc_archive 'CCDC 939273'