# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Smith, Dan' 'Ozerov, Oleg' _publ_contact_author_name 'Ozerov, Oleg' _publ_contact_author_email ozerov@chem.tamu.edu _publ_section_title ; Early-Late Heterobimetallic Rh-Ti and Rh-Zr Complexes via Addition of Early Metal Chlorides to Mono- and Divalent Rhodium ; # Attachment '- oz280_DAS283_PNPRhTiCl3Cl.cif' data_oz280_DAS283 _database_code_depnum_ccdc_archive 'CCDC 835998' #TrackingRef '- oz280_DAS283_PNPRhTiCl3Cl.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (PNP)Rh(TiCl3)(Cl) _chemical_melting_point ? _chemical_formula_moiety 'C26 H40 Cl4 N P2 Rh Ti, C6 H5 F' _chemical_formula_sum 'C32 H45 Cl4 F N P2 Rh Ti' _chemical_formula_weight 817.24 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' Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 '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 17.2563(14) _cell_length_b 12.7259(10) _cell_length_c 20.0652(12) _cell_angle_alpha 90.00 _cell_angle_beta 125.229(5) _cell_angle_gamma 90.00 _cell_volume 3599.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9996 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 27.38 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 1.095 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6337 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31889 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6346 _reflns_number_gt 5554 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0268P)^2^+2.4354P] 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 6346 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0285 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0566 _refine_ls_wR_factor_gt 0.0541 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.766660(11) 0.725695(13) 0.287493(9) 0.01373(5) Uani 1 1 d . . . Ti1 Ti 0.79137(3) 0.90308(3) 0.27490(2) 0.01684(9) Uani 1 1 d . . . Cl1 Cl 0.67685(4) 0.61622(4) 0.17509(3) 0.02501(13) Uani 1 1 d . . . Cl2 Cl 0.93508(4) 0.98010(4) 0.33028(3) 0.02372(12) Uani 1 1 d . . . Cl3 Cl 0.74830(4) 0.89813(4) 0.14475(3) 0.02565(13) Uani 1 1 d . . . Cl4 Cl 0.69086(4) 1.02477(4) 0.26322(3) 0.02429(12) Uani 1 1 d . . . P1 P 0.90947(4) 0.68345(4) 0.30576(3) 0.01522(12) Uani 1 1 d . . . P2 P 0.66272(4) 0.73222(4) 0.32511(3) 0.01502(12) Uani 1 1 d . . . N2 N 0.84997(12) 0.82083(13) 0.38730(10) 0.0144(4) Uani 1 1 d . . . C1 C 0.71506(14) 0.84012(16) 0.39758(12) 0.0153(4) Uani 1 1 d . . . C2 C 0.66830(15) 0.89604(17) 0.42444(13) 0.0185(5) Uani 1 1 d . . . H2 H 0.6084 0.8741 0.4084 0.022 Uiso 1 1 calc R . . C3 C 0.80523(14) 0.87267(16) 0.42161(12) 0.0145(4) Uani 1 1 d . . . C4 C 0.94722(14) 0.78750(16) 0.44204(13) 0.0157(4) Uani 1 1 d . . . C5 C 0.98896(15) 0.73097(16) 0.40969(12) 0.0161(4) Uani 1 1 d . . . C6 C 0.70891(16) 0.98361(17) 0.47450(13) 0.0194(5) Uani 1 1 d . . . C7 C 0.79751(16) 1.01621(17) 0.49587(13) 0.0199(5) Uani 1 1 d . . . H7 H 0.8254 1.0754 0.5285 0.024 Uiso 1 1 calc R . . C8 C 1.00246(15) 0.80888(16) 0.52568(12) 0.0176(5) Uani 1 1 d . . . H8 H 0.9750 0.8416 0.5487 0.021 Uiso 1 1 calc R . . C9 C 1.09762(15) 0.78194(16) 0.57462(13) 0.0194(5) Uani 1 1 d . . . H9 H 1.1331 0.7976 0.6300 0.023 Uiso 1 1 calc R . . C10 C 1.14149(15) 0.73202(17) 0.54300(13) 0.0197(5) Uani 1 1 d . . . C11 C 1.08542(15) 0.70624(17) 0.46082(13) 0.0194(5) Uani 1 1 d . . . H11 H 1.1131 0.6711 0.4389 0.023 Uiso 1 1 calc R . . C12 C 1.24570(16) 0.70545(19) 0.59647(15) 0.0284(5) Uani 1 1 d . . . H12A H 1.2700 0.7029 0.5639 0.043 Uiso 1 1 calc R . . H12B H 1.2543 0.6383 0.6217 0.043 Uiso 1 1 calc R . . H12C H 1.2791 0.7583 0.6379 0.043 Uiso 1 1 calc R . . C13 C 0.53342(15) 0.75170(17) 0.25608(14) 0.0208(5) Uani 1 1 d . . . H13 H 0.5083 0.7557 0.2891 0.025 Uiso 1 1 calc R . . C14 C 0.50790(16) 0.85288(19) 0.20723(15) 0.0309(6) Uani 1 1 d . . . H14A H 0.4401 0.8593 0.1710 0.046 Uiso 1 1 calc R . . H14B H 0.5341 0.8514 0.1761 0.046 Uiso 1 1 calc R . . H14C H 0.5333 0.9118 0.2438 0.046 Uiso 1 1 calc R . . C15 C 0.48932(16) 0.65591(19) 0.19962(14) 0.0280(5) Uani 1 1 d . . . H15A H 0.5109 0.6528 0.1650 0.042 Uiso 1 1 calc R . . H15B H 0.4214 0.6620 0.1667 0.042 Uiso 1 1 calc R . . H15C H 0.5080 0.5931 0.2319 0.042 Uiso 1 1 calc R . . C16 C 0.94670(16) 0.73058(18) 0.24118(13) 0.0208(5) Uani 1 1 d . . . H16 H 0.9274 0.8045 0.2291 0.025 Uiso 1 1 calc R . . C19 C 0.88944(18) 0.49703(19) 0.36556(15) 0.0303(6) Uani 1 1 d . . . H19A H 0.9354 0.5208 0.4203 0.046 Uiso 1 1 calc R . . H19B H 0.8884 0.4216 0.3644 0.046 Uiso 1 1 calc R . . H19C H 0.8279 0.5230 0.3471 0.046 Uiso 1 1 calc R . . C20 C 0.91597(16) 0.53808(17) 0.30949(14) 0.0218(5) Uani 1 1 d . . . H20 H 0.8663 0.5134 0.2545 0.026 Uiso 1 1 calc R . . C21 C 0.88829(17) 0.6723(2) 0.15927(14) 0.0287(5) Uani 1 1 d . . . H21A H 0.9091 0.6006 0.1670 0.043 Uiso 1 1 calc R . . H21B H 0.8968 0.7057 0.1210 0.043 Uiso 1 1 calc R . . H21C H 0.8224 0.6742 0.1386 0.043 Uiso 1 1 calc R . . C22 C 1.05319(17) 0.7283(2) 0.27909(15) 0.0289(6) Uani 1 1 d . . . H22A H 1.0639 0.7500 0.2392 0.043 Uiso 1 1 calc R . . H22B H 1.0769 0.6583 0.2970 0.043 Uiso 1 1 calc R . . H22C H 1.0856 0.7753 0.3249 0.043 Uiso 1 1 calc R . . C23 C 0.65945(18) 1.04192(18) 0.50525(15) 0.0267(5) Uani 1 1 d . . . H23A H 0.6751 1.1152 0.5104 0.040 Uiso 1 1 calc R . . H23B H 0.6797 1.0144 0.5575 0.040 Uiso 1 1 calc R . . H23C H 0.5921 1.0332 0.4674 0.040 Uiso 1 1 calc R . . C24 C 0.60950(18) 0.6074(2) 0.41034(16) 0.0320(6) Uani 1 1 d . . . H24A H 0.6159 0.6691 0.4407 0.048 Uiso 1 1 calc R . . H24B H 0.6234 0.5462 0.4435 0.048 Uiso 1 1 calc R . . H24C H 0.5457 0.6029 0.3621 0.048 Uiso 1 1 calc R . . C25 C 0.67881(15) 0.61373(17) 0.38602(13) 0.0206(5) Uani 1 1 d . . . H25 H 0.6682 0.5519 0.3526 0.025 Uiso 1 1 calc R . . C26 C 0.78088(16) 0.60835(19) 0.46265(14) 0.0266(5) Uani 1 1 d . . . H26A H 0.7926 0.5399 0.4868 0.040 Uiso 1 1 calc R . . H26B H 0.7898 0.6606 0.5010 0.040 Uiso 1 1 calc R . . H26C H 0.8242 0.6212 0.4481 0.040 Uiso 1 1 calc R . . C27 C 0.84502(15) 0.96250(16) 0.46959(12) 0.0174(4) Uani 1 1 d . . . H27 H 0.9037 0.9864 0.4840 0.021 Uiso 1 1 calc R . . C28 C 1.00821(17) 0.48773(19) 0.33168(15) 0.0305(6) Uani 1 1 d . . . H28A H 1.0031 0.4127 0.3324 0.046 Uiso 1 1 calc R . . H28B H 1.0597 0.5117 0.3846 0.046 Uiso 1 1 calc R . . H28C H 1.0199 0.5071 0.2920 0.046 Uiso 1 1 calc R . . F1 F 0.25350(12) 0.69190(16) 0.77607(10) 0.0612(5) Uani 1 1 d . . . C29 C 0.33054(19) 0.7243(2) 0.84977(15) 0.0346(6) Uani 1 1 d . . . C30 C 0.41020(18) 0.6623(2) 0.88860(15) 0.0308(6) Uani 1 1 d . . . H30 H 0.4121 0.6007 0.8647 0.037 Uiso 1 1 calc R . . C31 C 0.48741(18) 0.6941(2) 0.96415(16) 0.0328(6) Uani 1 1 d . . . H31 H 0.5419 0.6529 0.9924 0.039 Uiso 1 1 calc R . . C32 C 0.4839(2) 0.7868(2) 0.99777(17) 0.0409(7) Uani 1 1 d . . . H32 H 0.5362 0.8085 1.0484 0.049 Uiso 1 1 calc R . . C33 C 0.4027(2) 0.8475(2) 0.95614(19) 0.0461(7) Uani 1 1 d . . . H33 H 0.4009 0.9105 0.9787 0.055 Uiso 1 1 calc R . . C34 C 0.3246(2) 0.8158(2) 0.88182(18) 0.0409(7) Uani 1 1 d . . . H34 H 0.2692 0.8556 0.8542 0.049 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 0.01290(9) 0.01535(9) 0.01174(9) -0.00179(6) 0.00641(7) -0.00039(6) Ti1 0.0171(2) 0.0165(2) 0.0153(2) 0.00087(15) 0.00840(17) 0.00031(15) Cl1 0.0214(3) 0.0278(3) 0.0204(3) -0.0111(2) 0.0090(2) -0.0032(2) Cl2 0.0235(3) 0.0249(3) 0.0234(3) -0.0015(2) 0.0139(2) -0.0071(2) Cl3 0.0311(3) 0.0267(3) 0.0175(3) 0.0023(2) 0.0131(3) 0.0047(2) Cl4 0.0270(3) 0.0231(3) 0.0258(3) 0.0052(2) 0.0170(3) 0.0055(2) P1 0.0154(3) 0.0168(3) 0.0135(3) 0.0000(2) 0.0083(2) 0.0018(2) P2 0.0142(3) 0.0158(3) 0.0148(3) -0.0016(2) 0.0082(2) -0.0012(2) N2 0.0139(9) 0.0164(9) 0.0137(9) -0.0012(7) 0.0084(8) -0.0016(7) C1 0.0176(11) 0.0143(10) 0.0124(10) 0.0009(8) 0.0078(9) 0.0000(8) C2 0.0196(11) 0.0207(11) 0.0194(11) 0.0034(9) 0.0137(10) 0.0010(9) C3 0.0165(11) 0.0164(11) 0.0103(10) 0.0028(8) 0.0076(9) 0.0025(8) C4 0.0154(11) 0.0145(11) 0.0165(11) 0.0027(8) 0.0087(9) -0.0011(8) C5 0.0181(11) 0.0151(11) 0.0158(10) 0.0019(9) 0.0101(9) -0.0020(9) C6 0.0272(12) 0.0187(11) 0.0166(11) 0.0043(9) 0.0152(10) 0.0060(9) C7 0.0274(12) 0.0151(11) 0.0148(10) -0.0019(9) 0.0108(10) -0.0010(9) C8 0.0195(11) 0.0170(11) 0.0158(11) 0.0001(9) 0.0100(10) -0.0018(9) C9 0.0181(11) 0.0195(11) 0.0140(11) 0.0002(9) 0.0054(9) -0.0052(9) C10 0.0133(11) 0.0191(11) 0.0198(11) 0.0036(9) 0.0056(9) -0.0031(9) C11 0.0166(11) 0.0187(11) 0.0240(12) 0.0010(9) 0.0123(10) 0.0000(9) C12 0.0168(12) 0.0316(14) 0.0271(13) 0.0010(11) 0.0070(11) -0.0003(10) C13 0.0146(11) 0.0232(12) 0.0236(12) -0.0024(9) 0.0104(10) -0.0013(9) C14 0.0173(12) 0.0289(13) 0.0313(13) 0.0025(11) 0.0053(11) 0.0020(10) C15 0.0156(12) 0.0298(13) 0.0294(13) -0.0052(11) 0.0076(10) -0.0032(10) C16 0.0233(12) 0.0234(12) 0.0202(11) 0.0035(9) 0.0151(10) 0.0036(9) C19 0.0395(15) 0.0217(13) 0.0346(14) 0.0037(11) 0.0241(12) 0.0011(11) C20 0.0245(12) 0.0177(11) 0.0206(11) -0.0009(9) 0.0115(10) 0.0027(9) C21 0.0341(14) 0.0347(14) 0.0218(12) 0.0015(11) 0.0189(11) 0.0056(11) C22 0.0289(13) 0.0357(14) 0.0313(14) 0.0056(11) 0.0228(12) 0.0041(11) C23 0.0371(14) 0.0230(12) 0.0285(13) 0.0011(10) 0.0239(12) 0.0034(10) C24 0.0355(14) 0.0331(14) 0.0342(14) 0.0067(11) 0.0241(13) -0.0022(11) C25 0.0242(12) 0.0172(11) 0.0211(11) 0.0001(9) 0.0135(10) -0.0014(9) C26 0.0302(13) 0.0249(12) 0.0219(12) 0.0046(10) 0.0134(11) 0.0034(10) C27 0.0186(11) 0.0178(11) 0.0140(10) 0.0006(9) 0.0084(9) -0.0018(9) C28 0.0316(14) 0.0233(13) 0.0364(14) 0.0013(11) 0.0195(12) 0.0055(11) F1 0.0436(10) 0.0822(14) 0.0339(10) 0.0008(9) 0.0086(8) -0.0099(9) C29 0.0320(14) 0.0445(16) 0.0237(13) 0.0075(12) 0.0139(12) -0.0039(12) C30 0.0401(15) 0.0287(14) 0.0347(14) 0.0012(11) 0.0279(13) -0.0031(11) C31 0.0306(14) 0.0428(16) 0.0330(14) 0.0084(12) 0.0230(12) 0.0044(12) C32 0.0412(17) 0.0539(19) 0.0314(15) -0.0092(13) 0.0232(14) -0.0114(14) C33 0.064(2) 0.0334(16) 0.0568(19) -0.0051(14) 0.0445(18) 0.0003(15) C34 0.0446(17) 0.0404(17) 0.0451(17) 0.0170(14) 0.0302(15) 0.0123(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 N2 2.0547(17) . ? Rh1 P2 2.3142(6) . ? Rh1 Cl1 2.3232(6) . ? Rh1 P1 2.3354(6) . ? Rh1 Ti1 2.3379(4) . ? Ti1 N2 2.1387(17) . ? Ti1 Cl4 2.2345(7) . ? Ti1 Cl3 2.2664(7) . ? Ti1 Cl2 2.2729(7) . ? P1 C5 1.815(2) . ? P1 C16 1.847(2) . ? P1 C20 1.852(2) . ? P2 C1 1.817(2) . ? P2 C13 1.842(2) . ? P2 C25 1.858(2) . ? N2 C4 1.441(3) . ? N2 C3 1.455(3) . ? C1 C2 1.396(3) . ? C1 C3 1.400(3) . ? C2 C6 1.389(3) . ? C2 H2 0.9300 . ? C3 C27 1.394(3) . ? C4 C8 1.398(3) . ? C4 C5 1.413(3) . ? C5 C11 1.397(3) . ? C6 C7 1.392(3) . ? C6 C23 1.506(3) . ? C7 C27 1.384(3) . ? C7 H7 0.9300 . ? C8 C9 1.385(3) . ? C8 H8 0.9300 . ? C9 C10 1.390(3) . ? C9 H9 0.9300 . ? C10 C11 1.387(3) . ? C10 C12 1.508(3) . ? C11 H11 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.521(3) . ? C13 C15 1.534(3) . ? C13 H13 0.9800 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C22 1.531(3) . ? C16 C21 1.535(3) . ? C16 H16 0.9800 . ? C19 C20 1.531(3) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C28 1.525(3) . ? C20 H20 0.9800 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.532(3) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.532(3) . ? C25 H25 0.9800 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27 0.9300 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? F1 C29 1.362(3) . ? C29 C34 1.362(4) . ? C29 C30 1.372(4) . ? C30 C31 1.381(4) . ? C30 H30 0.9300 . ? C31 C32 1.377(4) . ? C31 H31 0.9300 . ? C32 C33 1.382(4) . ? C32 H32 0.9300 . ? C33 C34 1.373(4) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? 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 N2 Rh1 P2 84.21(5) . . ? N2 Rh1 Cl1 178.15(5) . . ? P2 Rh1 Cl1 97.45(2) . . ? N2 Rh1 P1 84.32(5) . . ? P2 Rh1 P1 154.59(2) . . ? Cl1 Rh1 P1 93.84(2) . . ? N2 Rh1 Ti1 57.84(5) . . ? P2 Rh1 Ti1 102.982(17) . . ? Cl1 Rh1 Ti1 122.357(19) . . ? P1 Rh1 Ti1 89.854(18) . . ? N2 Ti1 Cl4 108.42(5) . . ? N2 Ti1 Cl3 147.44(5) . . ? Cl4 Ti1 Cl3 100.35(2) . . ? N2 Ti1 Cl2 88.66(5) . . ? Cl4 Ti1 Cl2 108.33(3) . . ? Cl3 Ti1 Cl2 96.63(3) . . ? N2 Ti1 Rh1 54.42(5) . . ? Cl4 Ti1 Rh1 120.10(2) . . ? Cl3 Ti1 Rh1 97.97(2) . . ? Cl2 Ti1 Rh1 125.39(2) . . ? C5 P1 C16 111.07(10) . . ? C5 P1 C20 107.35(10) . . ? C16 P1 C20 108.36(10) . . ? C5 P1 Rh1 97.66(7) . . ? C16 P1 Rh1 125.29(7) . . ? C20 P1 Rh1 105.67(7) . . ? C1 P2 C13 109.11(10) . . ? C1 P2 C25 105.68(10) . . ? C13 P2 C25 105.09(10) . . ? C1 P2 Rh1 99.63(7) . . ? C13 P2 Rh1 126.16(8) . . ? C25 P2 Rh1 109.61(7) . . ? C4 N2 C3 118.38(16) . . ? C4 N2 Rh1 114.96(13) . . ? C3 N2 Rh1 117.66(13) . . ? C4 N2 Ti1 125.61(13) . . ? C3 N2 Ti1 102.70(12) . . ? Rh1 N2 Ti1 67.73(5) . . ? C2 C1 C3 119.43(19) . . ? C2 C1 P2 124.26(16) . . ? C3 C1 P2 116.10(15) . . ? C6 C2 C1 121.7(2) . . ? C6 C2 H2 119.2 . . ? C1 C2 H2 119.2 . . ? C27 C3 C1 119.17(19) . . ? C27 C3 N2 120.94(18) . . ? C1 C3 N2 119.37(18) . . ? C8 C4 C5 118.38(19) . . ? C8 C4 N2 123.07(18) . . ? C5 C4 N2 118.54(18) . . ? C11 C5 C4 118.97(19) . . ? C11 C5 P1 124.00(17) . . ? C4 C5 P1 116.72(15) . . ? C2 C6 C7 117.92(19) . . ? C2 C6 C23 121.5(2) . . ? C7 C6 C23 120.6(2) . . ? C27 C7 C6 121.5(2) . . ? C27 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C9 C8 C4 120.8(2) . . ? C9 C8 H8 119.6 . . ? C4 C8 H8 119.6 . . ? C8 C9 C10 121.6(2) . . ? C8 C9 H9 119.2 . . ? C10 C9 H9 119.2 . . ? C11 C10 C9 117.4(2) . . ? C11 C10 C12 121.4(2) . . ? C9 C10 C12 121.2(2) . . ? C10 C11 C5 122.6(2) . . ? C10 C11 H11 118.7 . . ? C5 C11 H11 118.7 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C15 111.1(2) . . ? C14 C13 P2 111.91(15) . . ? C15 C13 P2 108.55(15) . . ? C14 C13 H13 108.4 . . ? C15 C13 H13 108.4 . . ? P2 C13 H13 108.4 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C22 C16 C21 112.43(19) . . ? C22 C16 P1 116.68(16) . . ? C21 C16 P1 108.37(16) . . ? C22 C16 H16 106.2 . . ? C21 C16 H16 106.2 . . ? P1 C16 H16 106.2 . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C28 C20 C19 110.27(19) . . ? C28 C20 P1 117.41(16) . . ? C19 C20 P1 109.49(15) . . ? C28 C20 H20 106.3 . . ? C19 C20 H20 106.3 . . ? P1 C20 H20 106.3 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C16 C22 H22A 109.5 . . ? C16 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C16 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C6 C23 H23A 109.5 . . ? C6 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C6 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C25 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C24 109.56(19) . . ? C26 C25 P2 110.21(15) . . ? C24 C25 P2 113.83(16) . . ? C26 C25 H25 107.7 . . ? C24 C25 H25 107.7 . . ? P2 C25 H25 107.7 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C7 C27 C3 120.3(2) . . ? C7 C27 H27 119.9 . . ? C3 C27 H27 119.9 . . ? C20 C28 H28A 109.5 . . ? C20 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C20 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C34 C29 F1 118.6(3) . . ? C34 C29 C30 123.1(3) . . ? F1 C29 C30 118.2(3) . . ? C29 C30 C31 118.1(2) . . ? C29 C30 H30 120.9 . . ? C31 C30 H30 120.9 . . ? C32 C31 C30 120.1(3) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C31 C32 C33 119.9(3) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C34 C33 C32 120.7(3) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C29 C34 C33 118.0(3) . . ? C29 C34 H34 121.0 . . ? C33 C34 H34 121.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Rh1 Ti1 N2 74.50(6) . . . . ? Cl1 Rh1 Ti1 N2 -177.83(6) . . . . ? P1 Rh1 Ti1 N2 -83.37(6) . . . . ? N2 Rh1 Ti1 Cl4 -91.97(6) . . . . ? P2 Rh1 Ti1 Cl4 -17.47(3) . . . . ? Cl1 Rh1 Ti1 Cl4 90.21(3) . . . . ? P1 Rh1 Ti1 Cl4 -175.34(3) . . . . ? N2 Rh1 Ti1 Cl3 161.12(6) . . . . ? P2 Rh1 Ti1 Cl3 -124.38(2) . . . . ? Cl1 Rh1 Ti1 Cl3 -16.71(3) . . . . ? P1 Rh1 Ti1 Cl3 77.75(2) . . . . ? N2 Rh1 Ti1 Cl2 57.09(6) . . . . ? P2 Rh1 Ti1 Cl2 131.59(3) . . . . ? Cl1 Rh1 Ti1 Cl2 -120.74(3) . . . . ? P1 Rh1 Ti1 Cl2 -26.29(3) . . . . ? N2 Rh1 P1 C5 17.04(8) . . . . ? P2 Rh1 P1 C5 -46.49(9) . . . . ? Cl1 Rh1 P1 C5 -162.85(7) . . . . ? Ti1 Rh1 P1 C5 74.72(7) . . . . ? N2 Rh1 P1 C16 -105.62(10) . . . . ? P2 Rh1 P1 C16 -169.15(9) . . . . ? Cl1 Rh1 P1 C16 74.49(9) . . . . ? Ti1 Rh1 P1 C16 -47.94(9) . . . . ? N2 Rh1 P1 C20 127.55(9) . . . . ? P2 Rh1 P1 C20 64.02(9) . . . . ? Cl1 Rh1 P1 C20 -52.34(8) . . . . ? Ti1 Rh1 P1 C20 -174.77(8) . . . . ? N2 Rh1 P2 C1 13.47(8) . . . . ? Cl1 Rh1 P2 C1 -167.35(7) . . . . ? P1 Rh1 P2 C1 77.02(8) . . . . ? Ti1 Rh1 P2 C1 -41.61(7) . . . . ? N2 Rh1 P2 C13 135.84(10) . . . . ? Cl1 Rh1 P2 C13 -44.98(9) . . . . ? P1 Rh1 P2 C13 -160.61(9) . . . . ? Ti1 Rh1 P2 C13 80.75(9) . . . . ? N2 Rh1 P2 C25 -97.10(9) . . . . ? Cl1 Rh1 P2 C25 82.08(8) . . . . ? P1 Rh1 P2 C25 -33.55(9) . . . . ? Ti1 Rh1 P2 C25 -152.18(8) . . . . ? P2 Rh1 N2 C4 130.48(13) . . . . ? P1 Rh1 N2 C4 -26.81(13) . . . . ? Ti1 Rh1 N2 C4 -120.22(14) . . . . ? P2 Rh1 N2 C3 -16.23(13) . . . . ? P1 Rh1 N2 C3 -173.52(14) . . . . ? Ti1 Rh1 N2 C3 93.07(14) . . . . ? P2 Rh1 N2 Ti1 -109.30(4) . . . . ? P1 Rh1 N2 Ti1 93.41(3) . . . . ? Cl4 Ti1 N2 C4 -140.16(15) . . . . ? Cl3 Ti1 N2 C4 68.98(19) . . . . ? Cl2 Ti1 N2 C4 -31.27(15) . . . . ? Rh1 Ti1 N2 C4 105.53(16) . . . . ? Cl4 Ti1 N2 C3 -0.65(13) . . . . ? Cl3 Ti1 N2 C3 -151.51(10) . . . . ? Cl2 Ti1 N2 C3 108.24(12) . . . . ? Rh1 Ti1 N2 C3 -114.96(13) . . . . ? Cl4 Ti1 N2 Rh1 114.31(4) . . . . ? Cl3 Ti1 N2 Rh1 -36.55(10) . . . . ? Cl2 Ti1 N2 Rh1 -136.80(4) . . . . ? C13 P2 C1 C2 29.2(2) . . . . ? C25 P2 C1 C2 -83.35(19) . . . . ? Rh1 P2 C1 C2 163.00(17) . . . . ? C13 P2 C1 C3 -145.43(16) . . . . ? C25 P2 C1 C3 102.02(16) . . . . ? Rh1 P2 C1 C3 -11.63(16) . . . . ? C3 C1 C2 C6 0.1(3) . . . . ? P2 C1 C2 C6 -174.36(16) . . . . ? C2 C1 C3 C27 -2.2(3) . . . . ? P2 C1 C3 C27 172.69(15) . . . . ? C2 C1 C3 N2 -174.03(18) . . . . ? P2 C1 C3 N2 0.9(2) . . . . ? C4 N2 C3 C27 55.9(3) . . . . ? Rh1 N2 C3 C27 -158.50(15) . . . . ? Ti1 N2 C3 C27 -87.19(19) . . . . ? C4 N2 C3 C1 -132.38(19) . . . . ? Rh1 N2 C3 C1 13.2(2) . . . . ? Ti1 N2 C3 C1 84.49(18) . . . . ? C3 N2 C4 C8 -4.5(3) . . . . ? Rh1 N2 C4 C8 -150.91(16) . . . . ? Ti1 N2 C4 C8 129.50(18) . . . . ? C3 N2 C4 C5 175.85(18) . . . . ? Rh1 N2 C4 C5 29.4(2) . . . . ? Ti1 N2 C4 C5 -50.2(2) . . . . ? C8 C4 C5 C11 -5.2(3) . . . . ? N2 C4 C5 C11 174.50(18) . . . . ? C8 C4 C5 P1 168.63(15) . . . . ? N2 C4 C5 P1 -11.7(2) . . . . ? C16 P1 C5 C11 -62.1(2) . . . . ? C20 P1 C5 C11 56.2(2) . . . . ? Rh1 P1 C5 C11 165.33(17) . . . . ? C16 P1 C5 C4 124.40(16) . . . . ? C20 P1 C5 C4 -117.29(17) . . . . ? Rh1 P1 C5 C4 -8.17(16) . . . . ? C1 C2 C6 C7 1.6(3) . . . . ? C1 C2 C6 C23 -178.3(2) . . . . ? C2 C6 C7 C27 -1.1(3) . . . . ? C23 C6 C7 C27 178.7(2) . . . . ? C5 C4 C8 C9 4.5(3) . . . . ? N2 C4 C8 C9 -175.16(19) . . . . ? C4 C8 C9 C10 -0.7(3) . . . . ? C8 C9 C10 C11 -2.5(3) . . . . ? C8 C9 C10 C12 178.5(2) . . . . ? C9 C10 C11 C5 1.7(3) . . . . ? C12 C10 C11 C5 -179.3(2) . . . . ? C4 C5 C11 C10 2.2(3) . . . . ? P1 C5 C11 C10 -171.21(17) . . . . ? C1 P2 C13 C14 61.32(19) . . . . ? C25 P2 C13 C14 174.25(16) . . . . ? Rh1 P2 C13 C14 -56.88(19) . . . . ? C1 P2 C13 C15 -175.65(15) . . . . ? C25 P2 C13 C15 -62.72(18) . . . . ? Rh1 P2 C13 C15 66.15(18) . . . . ? C5 P1 C16 C22 41.9(2) . . . . ? C20 P1 C16 C22 -75.84(19) . . . . ? Rh1 P1 C16 C22 158.46(14) . . . . ? C5 P1 C16 C21 169.93(15) . . . . ? C20 P1 C16 C21 52.24(18) . . . . ? Rh1 P1 C16 C21 -73.47(17) . . . . ? C5 P1 C20 C28 -69.08(19) . . . . ? C16 P1 C20 C28 51.0(2) . . . . ? Rh1 P1 C20 C28 -172.54(15) . . . . ? C5 P1 C20 C19 57.61(18) . . . . ? C16 P1 C20 C19 177.65(16) . . . . ? Rh1 P1 C20 C19 -45.85(17) . . . . ? C1 P2 C25 C26 -47.03(18) . . . . ? C13 P2 C25 C26 -162.37(15) . . . . ? Rh1 P2 C25 C26 59.49(16) . . . . ? C1 P2 C25 C24 76.51(18) . . . . ? C13 P2 C25 C24 -38.82(19) . . . . ? Rh1 P2 C25 C24 -176.96(15) . . . . ? C6 C7 C27 C3 -1.0(3) . . . . ? C1 C3 C27 C7 2.6(3) . . . . ? N2 C3 C27 C7 174.34(18) . . . . ? C34 C29 C30 C31 0.7(4) . . . . ? F1 C29 C30 C31 -178.5(2) . . . . ? C29 C30 C31 C32 -1.4(4) . . . . ? C30 C31 C32 C33 0.6(4) . . . . ? C31 C32 C33 C34 0.8(4) . . . . ? F1 C29 C34 C33 180.0(2) . . . . ? C30 C29 C34 C33 0.7(4) . . . . ? C32 C33 C34 C29 -1.5(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.707 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.059 # Attachment '- oz287_das239_0m.cif' data_ovo287_das239_0m _database_code_depnum_ccdc_archive 'CCDC 835999' #TrackingRef '- oz287_das239_0m.cif' # start Validation Reply Form _vrf_PLAT041_ovo287_das239_0m ; PROBLEM: Calc. and Reported SumFormula Strings Differ RESPONSE: Due to solvent disorder deuteriums were not placed ; _vrf_PLAT860_ovo287_das239_0m ; PROBLEM: Number of Least-Squares Restraints ....... 51 RESPONSE: All 51 restraints applied to solvent ; # end Validation Reply Form #Added by publCIF (Wed Apr 20 16:14:46 2011) _audit_update_record ; 2011-04-20 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common (PNP)Rh(ZrCl3)(Cl) _chemical_melting_point ? _chemical_formula_moiety 'C26 H40 Cl4 N P2 Rh Zr, C6 D6' _chemical_formula_sum 'C32 H40 Cl4 D6 N P2 Rh Zr' _chemical_formula_weight 848.60 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' D D 0.0000 0.0000 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 '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 17.021(2) _cell_length_b 12.9851(15) _cell_length_c 19.9047(16) _cell_angle_alpha 90.00 _cell_angle_beta 123.275(7) _cell_angle_gamma 90.00 _cell_volume 3678.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9895 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 28.63 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 1.132 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7650 _exptl_absorpt_correction_T_max 0.8952 _exptl_absorpt_process_details SADABS _exptl_special_details ? _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31408 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8369 _reflns_number_gt 7449 _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 ? _computing_publication_material ? _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^)+(0.0280P)^2^+3.6253P] 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 8369 _refine_ls_number_parameters 380 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0697 _refine_ls_wR_factor_gt 0.0675 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.188 _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 0.218714(12) 0.704123(13) 0.702424(10) 0.01482(5) Uani 1 1 d . . . Zr1 Zr 0.203176(15) 0.896096(17) 0.713889(13) 0.01651(6) Uani 1 1 d . . . Cl1 Cl 0.23551(5) 0.90035(6) 0.84655(4) 0.03616(16) Uani 1 1 d . . . Cl2 Cl 0.31316(5) 1.02433(5) 0.73167(4) 0.02856(14) Uani 1 1 d . . . Cl3 Cl 0.05352(4) 0.97895(5) 0.65332(4) 0.02388(13) Uani 1 1 d . . . Cl4 Cl 0.30931(5) 0.60172(6) 0.81500(4) 0.03444(16) Uani 1 1 d . . . P1 P 0.07499(4) 0.66899(5) 0.68698(4) 0.01669(12) Uani 1 1 d . . . P2 P 0.32377(4) 0.71372(5) 0.66464(4) 0.01701(12) Uani 1 1 d . . . N1 N 0.13698(13) 0.79886(14) 0.60370(11) 0.0142(4) Uani 1 1 d . . . C1 C 0.4761(2) 0.8241(3) 0.7858(2) 0.0447(8) Uani 1 1 d . . . H1A H 0.4481 0.8170 0.8163 0.067 Uiso 1 1 calc R . . H1B H 0.4522 0.8850 0.7532 0.067 Uiso 1 1 calc R . . H1C H 0.5431 0.8295 0.8218 0.067 Uiso 1 1 calc R . . C2 C 0.45209(17) 0.7303(2) 0.73205(16) 0.0254(5) Uani 1 1 d . . . H2 H 0.4780 0.7405 0.6991 0.030 Uiso 1 1 calc R . . C3 C 0.49512(19) 0.6324(2) 0.78210(18) 0.0344(6) Uani 1 1 d . . . H3A H 0.5622 0.6394 0.8155 0.052 Uiso 1 1 calc R . . H3B H 0.4791 0.5744 0.7469 0.052 Uiso 1 1 calc R . . H3C H 0.4710 0.6219 0.8153 0.052 Uiso 1 1 calc R . . C4 C 0.3735(2) 0.6020(3) 0.5707(2) 0.0430(8) Uani 1 1 d . . . H4A H 0.3614 0.5422 0.5380 0.065 Uiso 1 1 calc R . . H4B H 0.4375 0.6008 0.6160 0.065 Uiso 1 1 calc R . . H4C H 0.3630 0.6629 0.5395 0.065 Uiso 1 1 calc R . . C5 C 0.30767(18) 0.6022(2) 0.60035(16) 0.0253(5) Uani 1 1 d . . . H5 H 0.3210 0.5399 0.6327 0.030 Uiso 1 1 calc R . . C6 C 0.20486(19) 0.5956(2) 0.52879(16) 0.0305(6) Uani 1 1 d . . . H6A H 0.1917 0.6513 0.4923 0.046 Uiso 1 1 calc R . . H6B H 0.1640 0.6002 0.5479 0.046 Uiso 1 1 calc R . . H6C H 0.1947 0.5312 0.5014 0.046 Uiso 1 1 calc R . . C7 C 0.0751(2) 0.4844(2) 0.61813(19) 0.0358(7) Uani 1 1 d . . . H7A H 0.1423 0.4840 0.6460 0.054 Uiso 1 1 calc R . . H7B H 0.0489 0.5256 0.5705 0.054 Uiso 1 1 calc R . . H7C H 0.0518 0.4152 0.6036 0.054 Uiso 1 1 calc R . . C8 C 0.04676(19) 0.52947(19) 0.67272(17) 0.0263(5) Uani 1 1 d . . . H8 H -0.0216 0.5226 0.6449 0.032 Uiso 1 1 calc R . . C9 C 0.1048(2) 0.6935(2) 0.83893(17) 0.0328(6) Uani 1 1 d . . . H9A H 0.0977 0.7409 0.8722 0.049 Uiso 1 1 calc R . . H9B H 0.1678 0.6972 0.8516 0.049 Uiso 1 1 calc R . . H9C H 0.0922 0.6248 0.8485 0.049 Uiso 1 1 calc R . . C10 C 0.03551(18) 0.72142(19) 0.75037(16) 0.0228(5) Uani 1 1 d . . . H10 H 0.0374 0.7966 0.7470 0.027 Uiso 1 1 calc R . . C11 C -0.0659(2) 0.6938(2) 0.72183(18) 0.0295(6) Uani 1 1 d . . . H11A H -0.0742 0.6206 0.7151 0.044 Uiso 1 1 calc R . . H11B H -0.1085 0.7273 0.6715 0.044 Uiso 1 1 calc R . . H11C H -0.0783 0.7163 0.7611 0.044 Uiso 1 1 calc R . . C12 C -0.00277(16) 0.71907(18) 0.58529(14) 0.0176(4) Uani 1 1 d . . . C13 C -0.09919(17) 0.69795(19) 0.53688(16) 0.0232(5) Uani 1 1 d . . . H13 H -0.1271 0.6624 0.5591 0.028 Uiso 1 1 calc R . . C14 C -0.15491(17) 0.7282(2) 0.45669(16) 0.0253(5) Uani 1 1 d . . . C15 C -0.25900(19) 0.7066(2) 0.4061(2) 0.0387(7) Uani 1 1 d . . . H15A H -0.2799 0.6868 0.4403 0.058 Uiso 1 1 calc R . . H15B H -0.2714 0.6518 0.3692 0.058 Uiso 1 1 calc R . . H15C H -0.2920 0.7674 0.3767 0.058 Uiso 1 1 calc R . . C16 C -0.11066(18) 0.77818(19) 0.42443(16) 0.0243(5) Uani 1 1 d . . . H16 H -0.1460 0.7980 0.3707 0.029 Uiso 1 1 calc R . . C17 C -0.01482(17) 0.79926(17) 0.47044(14) 0.0191(5) Uani 1 1 d . . . H17 H 0.0132 0.8311 0.4468 0.023 Uiso 1 1 calc R . . C18 C 0.03963(16) 0.77301(17) 0.55177(14) 0.0162(4) Uani 1 1 d . . . C19 C 0.18451(16) 0.85452(17) 0.57325(13) 0.0155(4) Uani 1 1 d . . . C20 C 0.27611(16) 0.82440(18) 0.59773(14) 0.0176(4) Uani 1 1 d . . . C21 C 0.32569(17) 0.8838(2) 0.57420(15) 0.0222(5) Uani 1 1 d . . . H21 H 0.3856 0.8631 0.5894 0.027 Uiso 1 1 calc R . . C22 C 0.28788(18) 0.97294(19) 0.52880(15) 0.0230(5) Uani 1 1 d . . . C23 C 0.19848(18) 1.00336(19) 0.50781(14) 0.0219(5) Uani 1 1 d . . . H23 H 0.1726 1.0635 0.4783 0.026 Uiso 1 1 calc R . . C24 C 0.14756(17) 0.94636(18) 0.52987(14) 0.0186(5) Uani 1 1 d . . . H24 H 0.0886 0.9690 0.5159 0.022 Uiso 1 1 calc R . . C25 C 0.3404(2) 1.0350(2) 0.50185(17) 0.0313(6) Uani 1 1 d . . . H25A H 0.4064 1.0330 0.5426 0.047 Uiso 1 1 calc R . . H25B H 0.3189 1.1051 0.4929 0.047 Uiso 1 1 calc R . . H25C H 0.3294 1.0066 0.4529 0.047 Uiso 1 1 calc R . . C26 C 0.0916(2) 0.4687(2) 0.7510(2) 0.0393(7) Uani 1 1 d . . . H26A H 0.0819 0.3964 0.7392 0.059 Uiso 1 1 calc R . . H26B H 0.0633 0.4886 0.7795 0.059 Uiso 1 1 calc R . . H26C H 0.1577 0.4830 0.7836 0.059 Uiso 1 1 calc R . . C27 C 0.6604(5) 0.7007(5) 0.6237(4) 0.124(2) Uani 1 1 d DU . . C28 C 0.6533(5) 0.7957(6) 0.6488(4) 0.125(2) Uani 1 1 d DU . . C29 C 0.5717(4) 0.8432(4) 0.5953(3) 0.0846(14) Uani 1 1 d DU . . C30 C 0.5034(3) 0.8056(4) 0.5218(3) 0.0759(14) Uani 1 1 d DU . . C31 C 0.5141(5) 0.7052(5) 0.4999(4) 0.117(2) Uani 1 1 d DU . . C32 C 0.5958(5) 0.6503(5) 0.5541(5) 0.119(2) Uani 1 1 d DU . . 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 0.01335(9) 0.01599(9) 0.01527(9) 0.00300(6) 0.00794(7) 0.00174(6) Zr1 0.01690(11) 0.01564(11) 0.01680(11) -0.00054(8) 0.00912(9) -0.00069(8) Cl1 0.0508(4) 0.0367(4) 0.0200(3) -0.0050(3) 0.0187(3) -0.0121(3) Cl2 0.0287(3) 0.0277(3) 0.0341(3) -0.0094(3) 0.0203(3) -0.0110(3) Cl3 0.0248(3) 0.0240(3) 0.0268(3) 0.0015(2) 0.0166(3) 0.0069(2) Cl4 0.0262(3) 0.0426(4) 0.0315(3) 0.0221(3) 0.0138(3) 0.0099(3) P1 0.0175(3) 0.0151(3) 0.0207(3) 0.0016(2) 0.0125(2) 0.0000(2) P2 0.0134(3) 0.0197(3) 0.0179(3) 0.0015(2) 0.0086(2) 0.0022(2) N1 0.0120(9) 0.0157(9) 0.0146(9) 0.0024(7) 0.0072(7) 0.0020(7) C1 0.0174(14) 0.0430(18) 0.0488(19) -0.0119(15) 0.0023(13) 0.0011(12) C2 0.0135(11) 0.0329(14) 0.0285(13) 0.0010(11) 0.0107(10) 0.0023(10) C3 0.0185(13) 0.0419(17) 0.0348(15) 0.0084(13) 0.0096(11) 0.0101(12) C4 0.0391(17) 0.056(2) 0.0426(18) -0.0118(15) 0.0281(15) 0.0059(15) C5 0.0298(14) 0.0222(13) 0.0260(13) -0.0015(10) 0.0166(11) 0.0047(10) C6 0.0331(15) 0.0288(14) 0.0267(14) -0.0049(11) 0.0146(12) -0.0009(11) C7 0.0494(18) 0.0193(13) 0.0463(18) -0.0063(12) 0.0312(15) -0.0022(12) C8 0.0273(13) 0.0173(12) 0.0400(15) -0.0002(10) 0.0221(12) -0.0025(10) C9 0.0414(16) 0.0381(16) 0.0276(14) 0.0002(12) 0.0244(13) -0.0070(13) C10 0.0296(13) 0.0190(12) 0.0304(14) -0.0001(10) 0.0231(12) -0.0010(10) C11 0.0327(15) 0.0285(14) 0.0414(16) 0.0018(11) 0.0292(13) 0.0009(11) C12 0.0148(11) 0.0166(11) 0.0212(12) -0.0004(9) 0.0097(9) 0.0010(8) C13 0.0169(12) 0.0212(12) 0.0322(14) -0.0017(10) 0.0140(11) -0.0014(9) C14 0.0145(11) 0.0200(12) 0.0323(14) -0.0029(10) 0.0070(10) 0.0013(9) C15 0.0180(13) 0.0388(17) 0.0423(18) 0.0003(13) 0.0057(12) -0.0036(11) C16 0.0204(12) 0.0199(12) 0.0224(12) -0.0016(9) 0.0052(10) 0.0047(9) C17 0.0192(11) 0.0170(11) 0.0191(11) 0.0002(9) 0.0093(10) 0.0034(9) C18 0.0156(11) 0.0142(10) 0.0182(11) -0.0011(8) 0.0090(9) 0.0025(8) C19 0.0176(11) 0.0178(11) 0.0124(10) -0.0016(8) 0.0091(9) -0.0023(8) C20 0.0185(11) 0.0195(11) 0.0162(11) -0.0005(9) 0.0103(9) 0.0008(9) C21 0.0195(12) 0.0278(13) 0.0235(12) -0.0012(10) 0.0144(10) -0.0018(10) C22 0.0299(13) 0.0228(13) 0.0222(12) -0.0027(9) 0.0180(11) -0.0053(10) C23 0.0299(13) 0.0189(12) 0.0174(11) 0.0021(9) 0.0133(10) 0.0001(10) C24 0.0196(11) 0.0189(11) 0.0169(11) -0.0001(9) 0.0098(9) 0.0009(9) C25 0.0380(16) 0.0305(15) 0.0359(15) 0.0014(12) 0.0269(13) -0.0075(12) C26 0.0520(19) 0.0246(15) 0.058(2) 0.0129(13) 0.0404(17) 0.0057(13) C27 0.113(4) 0.128(5) 0.165(5) 0.099(4) 0.098(4) 0.041(4) C28 0.103(4) 0.169(6) 0.122(4) 0.053(4) 0.073(4) -0.014(4) C29 0.084(3) 0.108(4) 0.099(4) 0.007(3) 0.073(3) -0.021(3) C30 0.066(3) 0.108(4) 0.083(3) 0.039(3) 0.059(2) 0.021(2) C31 0.121(4) 0.167(5) 0.119(4) -0.027(4) 0.103(4) -0.050(4) C32 0.143(5) 0.089(4) 0.203(6) -0.006(4) 0.144(5) 0.008(4) _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 N1 2.0761(18) . ? Rh1 P2 2.2923(6) . ? Rh1 Cl4 2.3185(7) . ? Rh1 P1 2.3371(7) . ? Rh1 Zr1 2.5303(4) . ? Zr1 N1 2.2276(19) . ? Zr1 Cl2 2.3823(7) . ? Zr1 Cl1 2.3841(7) . ? Zr1 Cl3 2.3938(7) . ? P1 C12 1.825(2) . ? P1 C10 1.854(2) . ? P1 C8 1.856(3) . ? P2 C20 1.820(2) . ? P2 C2 1.844(3) . ? P2 C5 1.851(3) . ? N1 C18 1.431(3) . ? N1 C19 1.443(3) . ? C1 C2 1.521(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.532(4) . ? C2 H2 0.9800 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.525(4) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.537(4) . ? C5 H5 0.9800 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.526(4) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C26 1.526(4) . ? C8 H8 0.9800 . ? C9 C10 1.532(4) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.534(4) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.401(3) . ? C12 C18 1.409(3) . ? C13 C14 1.393(4) . ? C13 H13 0.9300 . ? C14 C16 1.390(4) . ? C14 C15 1.508(4) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.391(3) . ? C16 H16 0.9300 . ? C17 C18 1.396(3) . ? C17 H17 0.9300 . ? C19 C24 1.403(3) . ? C19 C20 1.410(3) . ? C20 C21 1.400(3) . ? C21 C22 1.390(4) . ? C21 H21 0.9300 . ? C22 C23 1.396(4) . ? C22 C25 1.504(3) . ? C23 C24 1.382(3) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.361(6) . ? C27 C32 1.373(6) . ? C28 C29 1.348(5) . ? C29 C30 1.364(5) . ? C30 C31 1.419(5) . ? C31 C32 1.400(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 Rh1 P2 84.01(5) . . ? N1 Rh1 Cl4 178.28(5) . . ? P2 Rh1 Cl4 97.08(2) . . ? N1 Rh1 P1 83.20(5) . . ? P2 Rh1 P1 156.37(2) . . ? Cl4 Rh1 P1 96.22(2) . . ? N1 Rh1 Zr1 56.82(5) . . ? P2 Rh1 Zr1 96.604(17) . . ? Cl4 Rh1 Zr1 121.66(2) . . ? P1 Rh1 Zr1 92.897(17) . . ? N1 Zr1 Cl2 118.31(5) . . ? N1 Zr1 Cl1 142.03(5) . . ? Cl2 Zr1 Cl1 97.71(3) . . ? N1 Zr1 Cl3 86.29(5) . . ? Cl2 Zr1 Cl3 107.04(3) . . ? Cl1 Zr1 Cl3 94.74(3) . . ? N1 Zr1 Rh1 51.26(5) . . ? Cl2 Zr1 Rh1 126.12(2) . . ? Cl1 Zr1 Rh1 98.67(2) . . ? Cl3 Zr1 Rh1 122.166(18) . . ? C12 P1 C10 108.10(11) . . ? C12 P1 C8 102.06(12) . . ? C10 P1 C8 107.61(11) . . ? C12 P1 Rh1 98.40(8) . . ? C10 P1 Rh1 125.65(9) . . ? C8 P1 Rh1 112.03(8) . . ? C20 P2 C2 108.32(12) . . ? C20 P2 C5 105.94(12) . . ? C2 P2 C5 105.16(12) . . ? C20 P2 Rh1 99.69(8) . . ? C2 P2 Rh1 126.39(9) . . ? C5 P2 Rh1 109.76(9) . . ? C18 N1 C19 120.52(18) . . ? C18 N1 Rh1 116.99(14) . . ? C19 N1 Rh1 117.09(14) . . ? C18 N1 Zr1 127.16(14) . . ? C19 N1 Zr1 91.86(12) . . ? Rh1 N1 Zr1 71.92(6) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 C3 111.1(2) . . ? C1 C2 P2 111.04(18) . . ? C3 C2 P2 109.19(19) . . ? C1 C2 H2 108.5 . . ? C3 C2 H2 108.5 . . ? P2 C2 H2 108.5 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C5 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C4 C5 C6 110.2(2) . . ? C4 C5 P2 114.0(2) . . ? C6 C5 P2 110.21(18) . . ? C4 C5 H5 107.4 . . ? C6 C5 H5 107.4 . . ? P2 C5 H5 107.4 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C26 C8 C7 110.7(2) . . ? C26 C8 P1 113.9(2) . . ? C7 C8 P1 109.06(18) . . ? C26 C8 H8 107.6 . . ? C7 C8 H8 107.6 . . ? P1 C8 H8 107.6 . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C9 C10 C11 111.7(2) . . ? C9 C10 P1 111.01(18) . . ? C11 C10 P1 114.59(18) . . ? C9 C10 H10 106.3 . . ? C11 C10 H10 106.3 . . ? P1 C10 H10 106.3 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C18 118.9(2) . . ? C13 C12 P1 123.79(19) . . ? C18 C12 P1 117.00(17) . . ? C14 C13 C12 122.5(2) . . ? C14 C13 H13 118.8 . . ? C12 C13 H13 118.8 . . ? C16 C14 C13 117.4(2) . . ? C16 C14 C15 121.0(3) . . ? C13 C14 C15 121.6(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 C17 121.7(2) . . ? C14 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? C16 C17 C18 120.5(2) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C12 118.9(2) . . ? C17 C18 N1 123.3(2) . . ? C12 C18 N1 117.7(2) . . ? C24 C19 C20 119.1(2) . . ? C24 C19 N1 121.3(2) . . ? C20 C19 N1 119.0(2) . . ? C21 C20 C19 119.1(2) . . ? C21 C20 P2 124.86(18) . . ? C19 C20 P2 115.88(17) . . ? C22 C21 C20 121.8(2) . . ? C22 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? C21 C22 C23 118.0(2) . . ? C21 C22 C25 121.6(2) . . ? C23 C22 C25 120.3(2) . . ? C24 C23 C22 121.6(2) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C23 C24 C19 120.2(2) . . ? C23 C24 H24 119.9 . . ? C19 C24 H24 119.9 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C8 C26 H26A 109.5 . . ? C8 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C8 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C32 128.2(7) . . ? C29 C28 C27 112.6(7) . . ? C28 C29 C30 125.9(6) . . ? C29 C30 C31 118.7(5) . . ? C32 C31 C30 118.1(6) . . ? C27 C32 C31 116.2(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Rh1 Zr1 N1 78.38(6) . . . . ? Cl4 Rh1 Zr1 N1 -179.07(6) . . . . ? P1 Rh1 Zr1 N1 -79.94(6) . . . . ? N1 Rh1 Zr1 Cl2 -99.62(6) . . . . ? P2 Rh1 Zr1 Cl2 -21.24(3) . . . . ? Cl4 Rh1 Zr1 Cl2 81.31(3) . . . . ? P1 Rh1 Zr1 Cl2 -179.56(3) . . . . ? N1 Rh1 Zr1 Cl1 154.16(6) . . . . ? P2 Rh1 Zr1 Cl1 -127.46(3) . . . . ? Cl4 Rh1 Zr1 Cl1 -24.91(3) . . . . ? P1 Rh1 Zr1 Cl1 74.22(3) . . . . ? N1 Rh1 Zr1 Cl3 52.94(6) . . . . ? P2 Rh1 Zr1 Cl3 131.33(3) . . . . ? Cl4 Rh1 Zr1 Cl3 -126.13(3) . . . . ? P1 Rh1 Zr1 Cl3 -27.00(3) . . . . ? N1 Rh1 P1 C12 15.84(9) . . . . ? P2 Rh1 P1 C12 -41.83(10) . . . . ? Cl4 Rh1 P1 C12 -165.78(8) . . . . ? Zr1 Rh1 P1 C12 71.93(8) . . . . ? N1 Rh1 P1 C10 -103.66(12) . . . . ? P2 Rh1 P1 C10 -161.34(11) . . . . ? Cl4 Rh1 P1 C10 74.71(11) . . . . ? Zr1 Rh1 P1 C10 -47.58(10) . . . . ? N1 Rh1 P1 C8 122.56(11) . . . . ? P2 Rh1 P1 C8 64.88(11) . . . . ? Cl4 Rh1 P1 C8 -59.07(10) . . . . ? Zr1 Rh1 P1 C8 178.64(10) . . . . ? N1 Rh1 P2 C20 16.25(9) . . . . ? Cl4 Rh1 P2 C20 -162.42(8) . . . . ? P1 Rh1 P2 C20 73.78(10) . . . . ? Zr1 Rh1 P2 C20 -39.27(8) . . . . ? N1 Rh1 P2 C2 137.72(12) . . . . ? Cl4 Rh1 P2 C2 -40.95(11) . . . . ? P1 Rh1 P2 C2 -164.75(11) . . . . ? Zr1 Rh1 P2 C2 82.20(11) . . . . ? N1 Rh1 P2 C5 -94.69(10) . . . . ? Cl4 Rh1 P2 C5 86.65(9) . . . . ? P1 Rh1 P2 C5 -37.16(11) . . . . ? Zr1 Rh1 P2 C5 -150.20(9) . . . . ? P2 Rh1 N1 C18 134.92(15) . . . . ? P1 Rh1 N1 C18 -25.17(14) . . . . ? Zr1 Rh1 N1 C18 -123.15(16) . . . . ? P2 Rh1 N1 C19 -19.33(14) . . . . ? P1 Rh1 N1 C19 -179.42(15) . . . . ? Zr1 Rh1 N1 C19 82.61(15) . . . . ? P2 Rh1 N1 Zr1 -101.94(4) . . . . ? P1 Rh1 N1 Zr1 97.98(4) . . . . ? Cl2 Zr1 N1 C18 -134.18(16) . . . . ? Cl1 Zr1 N1 C18 66.1(2) . . . . ? Cl3 Zr1 N1 C18 -26.81(17) . . . . ? Rh1 Zr1 N1 C18 110.58(19) . . . . ? Cl2 Zr1 N1 C19 -2.71(14) . . . . ? Cl1 Zr1 N1 C19 -162.40(10) . . . . ? Cl3 Zr1 N1 C19 104.66(12) . . . . ? Rh1 Zr1 N1 C19 -117.95(13) . . . . ? Cl2 Zr1 N1 Rh1 115.23(4) . . . . ? Cl1 Zr1 N1 Rh1 -44.45(10) . . . . ? Cl3 Zr1 N1 Rh1 -137.39(4) . . . . ? C20 P2 C2 C1 63.8(2) . . . . ? C5 P2 C2 C1 176.8(2) . . . . ? Rh1 P2 C2 C1 -53.8(3) . . . . ? C20 P2 C2 C3 -173.37(18) . . . . ? C5 P2 C2 C3 -60.4(2) . . . . ? Rh1 P2 C2 C3 69.0(2) . . . . ? C20 P2 C5 C4 72.3(2) . . . . ? C2 P2 C5 C4 -42.3(2) . . . . ? Rh1 P2 C5 C4 179.11(19) . . . . ? C20 P2 C5 C6 -52.2(2) . . . . ? C2 P2 C5 C6 -166.81(19) . . . . ? Rh1 P2 C5 C6 54.6(2) . . . . ? C12 P1 C8 C26 -171.51(19) . . . . ? C10 P1 C8 C26 -57.9(2) . . . . ? Rh1 P1 C8 C26 84.2(2) . . . . ? C12 P1 C8 C7 64.3(2) . . . . ? C10 P1 C8 C7 177.9(2) . . . . ? Rh1 P1 C8 C7 -40.0(2) . . . . ? C12 P1 C10 C9 -172.95(18) . . . . ? C8 P1 C10 C9 77.5(2) . . . . ? Rh1 P1 C10 C9 -57.9(2) . . . . ? C12 P1 C10 C11 59.3(2) . . . . ? C8 P1 C10 C11 -50.2(2) . . . . ? Rh1 P1 C10 C11 174.41(15) . . . . ? C10 P1 C12 C13 -63.0(2) . . . . ? C8 P1 C12 C13 50.2(2) . . . . ? Rh1 P1 C12 C13 165.03(19) . . . . ? C10 P1 C12 C18 123.69(18) . . . . ? C8 P1 C12 C18 -123.03(19) . . . . ? Rh1 P1 C12 C18 -8.24(18) . . . . ? C18 C12 C13 C14 0.0(4) . . . . ? P1 C12 C13 C14 -173.13(19) . . . . ? C12 C13 C14 C16 2.1(4) . . . . ? C12 C13 C14 C15 -178.7(2) . . . . ? C13 C14 C16 C17 -1.3(4) . . . . ? C15 C14 C16 C17 179.6(2) . . . . ? C14 C16 C17 C18 -1.8(4) . . . . ? C16 C17 C18 C12 3.9(3) . . . . ? C16 C17 C18 N1 -175.5(2) . . . . ? C13 C12 C18 C17 -3.1(3) . . . . ? P1 C12 C18 C17 170.55(17) . . . . ? C13 C12 C18 N1 176.4(2) . . . . ? P1 C12 C18 N1 -10.0(3) . . . . ? C19 N1 C18 C17 -0.2(3) . . . . ? Rh1 N1 C18 C17 -153.54(18) . . . . ? Zr1 N1 C18 C17 119.4(2) . . . . ? C19 N1 C18 C12 -179.7(2) . . . . ? Rh1 N1 C18 C12 27.0(3) . . . . ? Zr1 N1 C18 C12 -60.1(3) . . . . ? C18 N1 C19 C24 51.4(3) . . . . ? Rh1 N1 C19 C24 -155.30(17) . . . . ? Zr1 N1 C19 C24 -84.7(2) . . . . ? C18 N1 C19 C20 -138.1(2) . . . . ? Rh1 N1 C19 C20 15.1(3) . . . . ? Zr1 N1 C19 C20 85.7(2) . . . . ? C24 C19 C20 C21 -3.6(3) . . . . ? N1 C19 C20 C21 -174.3(2) . . . . ? C24 C19 C20 P2 172.24(17) . . . . ? N1 C19 C20 P2 1.6(3) . . . . ? C2 P2 C20 C21 27.4(2) . . . . ? C5 P2 C20 C21 -85.0(2) . . . . ? Rh1 P2 C20 C21 161.1(2) . . . . ? C2 P2 C20 C19 -148.14(18) . . . . ? C5 P2 C20 C19 99.45(19) . . . . ? Rh1 P2 C20 C19 -14.47(18) . . . . ? C19 C20 C21 C22 1.4(4) . . . . ? P2 C20 C21 C22 -174.04(19) . . . . ? C20 C21 C22 C23 1.0(4) . . . . ? C20 C21 C22 C25 -178.4(2) . . . . ? C21 C22 C23 C24 -1.1(4) . . . . ? C25 C22 C23 C24 178.2(2) . . . . ? C22 C23 C24 C19 -1.1(4) . . . . ? C20 C19 C24 C23 3.5(3) . . . . ? N1 C19 C24 C23 173.9(2) . . . . ? C32 C27 C28 C29 -1.3(10) . . . . ? C27 C28 C29 C30 -2.7(8) . . . . ? C28 C29 C30 C31 4.1(7) . . . . ? C29 C30 C31 C32 -1.5(7) . . . . ? C28 C27 C32 C31 3.5(10) . . . . ? C30 C31 C32 C27 -1.8(8) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.258 _refine_diff_density_min -0.997 _refine_diff_density_rms 0.080 # Attachment '- oz296.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 836000' #TrackingRef '- oz296.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H42 Cl6 N P2 Rh Zr, C H2 Cl2' _chemical_formula_sum 'C28 H44 Cl8 N P2 Rh Zr' _chemical_formula_weight 934.31 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 '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 16.074(3) _cell_length_b 13.947(2) _cell_length_c 20.445(3) _cell_angle_alpha 90.00 _cell_angle_beta 124.232(10) _cell_angle_gamma 90.00 _cell_volume 3789.4(11) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9948 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.42 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_max 0.43 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 1.380 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6393 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29989 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 27.43 _reflns_number_total 8590 _reflns_number_gt 7205 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0432P)^2^+4.5623P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8590 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0864 _refine_ls_wR_factor_gt 0.0803 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 0.781755(15) 1.004470(15) 0.498318(12) 0.01502(6) Uani 1 1 d . . . Zr1 Zr 0.83418(2) 1.230801(19) 0.496160(16) 0.01868(7) Uani 1 1 d . . . Cl1 Cl 0.90102(5) 1.11900(5) 0.61315(4) 0.02199(14) Uani 1 1 d . . . Cl2 Cl 0.86216(5) 1.07839(5) 0.44049(4) 0.02031(14) Uani 1 1 d . . . Cl3 Cl 0.67056(5) 1.15010(5) 0.45640(4) 0.02087(14) Uani 1 1 d . . . Cl4 Cl 0.99601(6) 1.28068(5) 0.52963(5) 0.02811(16) Uani 1 1 d . . . Cl5 Cl 0.73705(6) 1.30801(6) 0.36925(4) 0.02888(16) Uani 1 1 d . . . Cl6 Cl 0.81843(6) 1.35842(5) 0.56707(4) 0.02841(16) Uani 1 1 d . . . P1 P 0.90669(5) 0.84885(5) 0.63994(4) 0.01618(14) Uani 1 1 d . . . P2 P 0.66981(5) 0.91515(5) 0.39338(4) 0.01694(14) Uani 1 1 d . . . N1 N 0.71500(17) 0.94725(17) 0.54719(14) 0.0179(5) Uani 1 1 d . . . C1 C 0.6250(2) 1.0559(2) 0.27582(19) 0.0283(7) Uani 1 1 d . . . H1A H 0.6453 1.1085 0.3120 0.042 Uiso 1 1 calc R . . H1B H 0.5759 1.0775 0.2230 0.042 Uiso 1 1 calc R . . H1C H 0.6825 1.0311 0.2784 0.042 Uiso 1 1 calc R . . C2 C 0.5793(2) 0.9769(2) 0.29814(17) 0.0222(6) Uani 1 1 d . . . H2 H 0.5549 0.9277 0.2570 0.027 Uiso 1 1 calc R . . C3 C 0.4858(2) 1.0155(2) 0.2921(2) 0.0310(7) Uani 1 1 d . . . H3A H 0.4387 1.0395 0.2397 0.047 Uiso 1 1 calc R . . H3B H 0.5051 1.0664 0.3297 0.047 Uiso 1 1 calc R . . H3C H 0.4550 0.9648 0.3032 0.047 Uiso 1 1 calc R . . C4 C 0.7840(2) 0.8534(2) 0.3358(2) 0.0306(7) Uani 1 1 d . . . H4A H 0.7390 0.8809 0.2843 0.046 Uiso 1 1 calc R . . H4B H 0.8203 0.8013 0.3322 0.046 Uiso 1 1 calc R . . H4C H 0.8307 0.9015 0.3710 0.046 Uiso 1 1 calc R . . C5 C 0.7238(2) 0.8163(2) 0.36746(18) 0.0232(6) Uani 1 1 d . . . H5 H 0.7721 0.7833 0.4172 0.028 Uiso 1 1 calc R . . C6 C 0.6479(3) 0.7402(2) 0.3120(2) 0.0346(8) Uani 1 1 d . . . H6A H 0.6820 0.6913 0.3026 0.052 Uiso 1 1 calc R . . H6B H 0.5973 0.7695 0.2627 0.052 Uiso 1 1 calc R . . H6C H 0.6167 0.7120 0.3359 0.052 Uiso 1 1 calc R . . C7 C 0.5977(2) 0.8642(2) 0.42684(17) 0.0186(5) Uani 1 1 d . . . C8 C 0.5110(2) 0.8076(2) 0.38085(17) 0.0207(6) Uani 1 1 d . . . H8 H 0.4886 0.7932 0.3290 0.025 Uiso 1 1 calc R . . C9 C 0.4583(2) 0.7729(2) 0.41053(18) 0.0217(6) Uani 1 1 d . . . C10 C 0.3637(2) 0.7137(2) 0.3612(2) 0.0294(7) Uani 1 1 d . . . H10A H 0.3790 0.6473 0.3756 0.044 Uiso 1 1 calc R . . H10B H 0.3376 0.7213 0.3062 0.044 Uiso 1 1 calc R . . H10C H 0.3143 0.7348 0.3705 0.044 Uiso 1 1 calc R . . C11 C 0.4960(2) 0.7947(2) 0.48952(18) 0.0219(6) Uani 1 1 d . . . H11 H 0.4628 0.7704 0.5113 0.026 Uiso 1 1 calc R . . C12 C 0.5801(2) 0.8504(2) 0.53623(17) 0.0205(6) Uani 1 1 d . . . H12 H 0.6027 0.8626 0.5885 0.025 Uiso 1 1 calc R . . C13 C 0.6323(2) 0.88937(19) 0.50506(16) 0.0164(5) Uani 1 1 d . . . C14 C 0.7618(2) 0.9629(2) 0.62943(16) 0.0173(5) Uani 1 1 d . . . C15 C 0.7175(2) 1.0177(2) 0.65850(17) 0.0206(6) Uani 1 1 d . . . H15 H 0.6549 1.0457 0.6238 0.025 Uiso 1 1 calc R . . C16 C 0.7664(2) 1.0309(2) 0.73926(18) 0.0218(6) Uani 1 1 d . . . H16 H 0.7354 1.0671 0.7580 0.026 Uiso 1 1 calc R . . C17 C 0.8611(2) 0.99125(19) 0.79338(17) 0.0198(6) Uani 1 1 d . . . C18 C 0.9125(2) 1.0059(2) 0.88134(18) 0.0248(6) Uani 1 1 d . . . H18A H 0.9801 0.9817 0.9090 0.037 Uiso 1 1 calc R . . H18B H 0.8761 0.9723 0.8987 0.037 Uiso 1 1 calc R . . H18C H 0.9141 1.0731 0.8922 0.037 Uiso 1 1 calc R . . C19 C 0.9066(2) 0.9380(2) 0.76412(16) 0.0195(6) Uani 1 1 d . . . H19 H 0.9701 0.9118 0.7990 0.023 Uiso 1 1 calc R . . C20 C 0.8574(2) 0.92349(19) 0.68249(16) 0.0173(5) Uani 1 1 d . . . C21 C 1.0970(2) 0.9276(2) 0.73630(18) 0.0263(6) Uani 1 1 d . . . H21A H 1.1019 0.9468 0.6935 0.039 Uiso 1 1 calc R . . H21B H 1.1633 0.9205 0.7836 0.039 Uiso 1 1 calc R . . H21C H 1.0609 0.9756 0.7445 0.039 Uiso 1 1 calc R . . C22 C 1.0411(2) 0.8321(2) 0.71611(17) 0.0213(6) Uani 1 1 d . . . H22 H 1.0478 0.8085 0.7640 0.026 Uiso 1 1 calc R . . C23 C 1.0884(2) 0.7579(3) 0.6916(2) 0.0335(8) Uani 1 1 d . . . H23A H 1.1604 0.7626 0.7257 0.050 Uiso 1 1 calc R . . H23B H 1.0667 0.7695 0.6379 0.050 Uiso 1 1 calc R . . H23C H 1.0679 0.6948 0.6957 0.050 Uiso 1 1 calc R . . C24 C 0.8371(4) 0.6947(3) 0.6828(2) 0.0456(10) Uani 1 1 d . . . H24A H 0.9049 0.6784 0.7246 0.068 Uiso 1 1 calc R . . H24B H 0.7958 0.6383 0.6661 0.068 Uiso 1 1 calc R . . H24C H 0.8114 0.7415 0.7017 0.068 Uiso 1 1 calc R . . C25 C 0.8356(2) 0.7362(2) 0.61295(18) 0.0220(6) Uani 1 1 d . . . H25 H 0.7654 0.7530 0.5728 0.026 Uiso 1 1 calc R . . C26 C 0.8641(3) 0.6593(2) 0.5755(2) 0.0355(8) Uani 1 1 d . . . H26A H 0.8102 0.6138 0.5478 0.053 Uiso 1 1 calc R . . H26B H 0.9240 0.6269 0.6162 0.053 Uiso 1 1 calc R . . H26C H 0.8760 0.6888 0.5391 0.053 Uiso 1 1 calc R . . C27 C 0.8920(2) 0.9011(2) 0.55317(17) 0.0186(5) Uani 1 1 d . . . Cl7 Cl 0.44169(9) 0.41189(10) 0.38981(7) 0.0699(4) Uani 1 1 d . . . Cl8 Cl 0.59754(10) 0.55620(11) 0.44480(8) 0.0784(4) Uani 1 1 d . . . C28 C 0.5704(4) 0.4342(4) 0.4424(3) 0.0688(14) Uani 1 1 d . . . H28A H 0.5985 0.3989 0.4182 0.083 Uiso 1 1 calc R . . H28B H 0.6023 0.4110 0.4961 0.083 Uiso 1 1 calc R . . H27A H 0.885(2) 0.851(2) 0.5195(18) 0.012(7) Uiso 1 1 d . . . H27B H 0.946(3) 0.934(2) 0.5674(19) 0.022(8) Uiso 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 0.01520(11) 0.01619(11) 0.01637(11) 0.00091(8) 0.01052(9) 0.00025(8) Zr1 0.02122(14) 0.01796(14) 0.01964(14) 0.00055(10) 0.01319(12) -0.00050(10) Cl1 0.0239(3) 0.0215(3) 0.0191(3) 0.0020(3) 0.0113(3) -0.0007(3) Cl2 0.0239(3) 0.0203(3) 0.0245(3) -0.0008(3) 0.0183(3) -0.0022(3) Cl3 0.0193(3) 0.0213(3) 0.0256(3) 0.0020(3) 0.0148(3) 0.0016(3) Cl4 0.0246(3) 0.0258(4) 0.0364(4) -0.0025(3) 0.0187(3) -0.0054(3) Cl5 0.0328(4) 0.0285(4) 0.0246(4) 0.0070(3) 0.0157(3) -0.0011(3) Cl6 0.0330(4) 0.0261(4) 0.0264(4) -0.0041(3) 0.0168(3) 0.0027(3) P1 0.0161(3) 0.0168(3) 0.0175(3) 0.0015(3) 0.0105(3) 0.0024(3) P2 0.0180(3) 0.0188(3) 0.0169(3) 0.0005(3) 0.0116(3) -0.0001(3) N1 0.0176(11) 0.0211(12) 0.0189(12) 0.0009(9) 0.0127(10) -0.0005(9) C1 0.0322(16) 0.0287(16) 0.0236(15) 0.0044(13) 0.0155(14) -0.0014(13) C2 0.0220(14) 0.0248(15) 0.0157(13) 0.0025(11) 0.0081(12) -0.0015(12) C3 0.0214(15) 0.0335(18) 0.0300(17) 0.0080(14) 0.0095(14) 0.0027(13) C4 0.0303(16) 0.0348(18) 0.0356(18) -0.0060(14) 0.0240(15) -0.0001(14) C5 0.0248(14) 0.0223(15) 0.0253(15) -0.0013(12) 0.0159(13) 0.0026(12) C6 0.0339(18) 0.0304(18) 0.043(2) -0.0140(15) 0.0234(17) -0.0064(14) C7 0.0189(13) 0.0188(13) 0.0218(14) 0.0027(11) 0.0138(12) 0.0014(11) C8 0.0190(13) 0.0217(14) 0.0198(14) -0.0011(11) 0.0099(12) -0.0006(11) C9 0.0190(13) 0.0184(14) 0.0299(16) -0.0001(12) 0.0150(13) -0.0002(11) C10 0.0222(15) 0.0336(17) 0.0338(17) -0.0041(14) 0.0166(14) -0.0072(13) C11 0.0233(14) 0.0206(14) 0.0313(16) 0.0021(12) 0.0212(13) -0.0005(11) C12 0.0211(13) 0.0221(14) 0.0224(14) 0.0004(11) 0.0148(12) -0.0002(11) C13 0.0165(12) 0.0129(12) 0.0224(14) 0.0034(10) 0.0124(11) 0.0040(10) C14 0.0187(13) 0.0161(13) 0.0206(14) 0.0011(10) 0.0132(12) -0.0011(10) C15 0.0189(13) 0.0221(14) 0.0235(15) 0.0005(11) 0.0137(12) 0.0028(11) C16 0.0254(15) 0.0205(14) 0.0264(15) -0.0019(12) 0.0188(13) 0.0021(11) C17 0.0260(14) 0.0164(13) 0.0204(14) -0.0002(11) 0.0151(12) -0.0007(11) C18 0.0313(16) 0.0240(15) 0.0207(15) 0.0017(12) 0.0156(13) 0.0047(13) C19 0.0228(14) 0.0181(13) 0.0195(14) 0.0011(11) 0.0130(12) 0.0009(11) C20 0.0196(13) 0.0170(13) 0.0201(13) 0.0027(10) 0.0140(12) 0.0032(11) C21 0.0213(14) 0.0321(17) 0.0232(15) 0.0003(13) 0.0112(13) -0.0021(13) C22 0.0180(13) 0.0266(15) 0.0184(13) 0.0018(11) 0.0097(12) 0.0043(11) C23 0.0195(14) 0.043(2) 0.0314(18) -0.0071(15) 0.0101(14) 0.0075(14) C24 0.076(3) 0.0309(19) 0.050(2) -0.0003(17) 0.048(2) -0.0136(19) C25 0.0195(13) 0.0187(14) 0.0289(15) 0.0015(12) 0.0143(13) 0.0011(11) C26 0.043(2) 0.0267(17) 0.049(2) -0.0077(15) 0.0332(18) -0.0057(15) C27 0.0183(13) 0.0204(14) 0.0201(14) 0.0022(11) 0.0125(12) 0.0021(11) Cl7 0.0565(7) 0.0810(9) 0.0571(7) 0.0296(6) 0.0229(6) -0.0029(6) Cl8 0.0568(7) 0.0767(9) 0.0622(8) 0.0089(7) 0.0094(6) -0.0075(7) C28 0.051(3) 0.061(3) 0.061(3) 0.013(2) 0.011(2) 0.013(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 Rh1 N1 1.998(2) . ? Rh1 C27 2.059(3) . ? Rh1 P2 2.2471(8) . ? Rh1 Cl2 2.4187(7) . ? Rh1 Cl3 2.5162(8) . ? Rh1 Cl1 2.5836(8) . ? Rh1 Zr1 3.2739(6) . ? Zr1 Cl4 2.3907(9) . ? Zr1 Cl6 2.3973(8) . ? Zr1 Cl5 2.4024(9) . ? Zr1 Cl1 2.5328(8) . ? Zr1 Cl3 2.5376(8) . ? Zr1 Cl2 2.5675(8) . ? P1 C20 1.801(3) . ? P1 C27 1.806(3) . ? P1 C22 1.834(3) . ? P1 C25 1.835(3) . ? P2 C7 1.792(3) . ? P2 C5 1.858(3) . ? P2 C2 1.861(3) . ? N1 C13 1.369(4) . ? N1 C14 1.420(3) . ? C1 C2 1.529(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.535(4) . ? C2 H2 0.9800 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.526(4) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.532(4) . ? C5 H5 0.9800 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.405(4) . ? C7 C13 1.410(4) . ? C8 C9 1.379(4) . ? C8 H8 0.9300 . ? C9 C11 1.402(4) . ? C9 C10 1.512(4) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.375(4) . ? C11 H11 0.9300 . ? C12 C13 1.417(4) . ? C12 H12 0.9300 . ? C14 C15 1.387(4) . ? C14 C20 1.402(4) . ? C15 C16 1.385(4) . ? C15 H15 0.9300 . ? C16 C17 1.397(4) . ? C16 H16 0.9300 . ? C17 C19 1.392(4) . ? C17 C18 1.512(4) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.402(4) . ? C19 H19 0.9300 . ? C21 C22 1.528(4) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.525(4) . ? C22 H22 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.530(4) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.530(4) . ? C25 H25 0.9800 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.94(3) . ? C27 H27B 0.88(3) . ? Cl7 C28 1.741(5) . ? Cl8 C28 1.750(5) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? 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 Rh1 C27 89.30(10) . . ? N1 Rh1 P2 83.64(7) . . ? C27 Rh1 P2 96.51(9) . . ? N1 Rh1 Cl2 178.29(7) . . ? C27 Rh1 Cl2 91.83(8) . . ? P2 Rh1 Cl2 97.51(3) . . ? N1 Rh1 Cl3 90.82(7) . . ? C27 Rh1 Cl3 168.35(9) . . ? P2 Rh1 Cl3 95.08(3) . . ? Cl2 Rh1 Cl3 87.82(3) . . ? N1 Rh1 Cl1 97.19(7) . . ? C27 Rh1 Cl1 88.09(9) . . ? P2 Rh1 Cl1 175.34(3) . . ? Cl2 Rh1 Cl1 81.56(3) . . ? Cl3 Rh1 Cl1 80.34(3) . . ? N1 Rh1 Zr1 127.34(7) . . ? C27 Rh1 Zr1 122.22(9) . . ? P2 Rh1 Zr1 126.56(2) . . ? Cl2 Rh1 Zr1 50.954(17) . . ? Cl3 Rh1 Zr1 49.91(2) . . ? Cl1 Rh1 Zr1 49.538(17) . . ? Cl4 Zr1 Cl6 94.53(3) . . ? Cl4 Zr1 Cl5 96.90(3) . . ? Cl6 Zr1 Cl5 95.44(3) . . ? Cl4 Zr1 Cl1 95.37(3) . . ? Cl6 Zr1 Cl1 91.09(3) . . ? Cl5 Zr1 Cl1 165.59(3) . . ? Cl4 Zr1 Cl3 170.22(3) . . ? Cl6 Zr1 Cl3 94.59(3) . . ? Cl5 Zr1 Cl3 85.76(3) . . ? Cl1 Zr1 Cl3 80.91(3) . . ? Cl4 Zr1 Cl2 86.22(3) . . ? Cl6 Zr1 Cl2 170.83(3) . . ? Cl5 Zr1 Cl2 93.55(3) . . ? Cl1 Zr1 Cl2 79.74(3) . . ? Cl3 Zr1 Cl2 84.22(2) . . ? Cl4 Zr1 Rh1 121.57(2) . . ? Cl6 Zr1 Rh1 126.31(2) . . ? Cl5 Zr1 Rh1 115.53(2) . . ? Cl1 Zr1 Rh1 50.904(19) . . ? Cl3 Zr1 Rh1 49.338(17) . . ? Cl2 Zr1 Rh1 47.023(17) . . ? Zr1 Cl1 Rh1 79.56(2) . . ? Rh1 Cl2 Zr1 82.02(2) . . ? Rh1 Cl3 Zr1 80.75(2) . . ? C20 P1 C27 113.02(13) . . ? C20 P1 C22 106.97(13) . . ? C27 P1 C22 109.04(13) . . ? C20 P1 C25 105.77(13) . . ? C27 P1 C25 109.56(14) . . ? C22 P1 C25 112.50(14) . . ? C7 P2 C5 108.77(13) . . ? C7 P2 C2 106.86(13) . . ? C5 P2 C2 105.10(14) . . ? C7 P2 Rh1 101.40(10) . . ? C5 P2 Rh1 115.59(10) . . ? C2 P2 Rh1 118.51(10) . . ? C13 N1 C14 121.1(2) . . ? C13 N1 Rh1 121.72(18) . . ? C14 N1 Rh1 117.04(17) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 C3 109.6(3) . . ? C1 C2 P2 114.9(2) . . ? C3 C2 P2 113.6(2) . . ? C1 C2 H2 106.0 . . ? C3 C2 H2 106.0 . . ? P2 C2 H2 106.0 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C5 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C4 C5 C6 110.6(3) . . ? C4 C5 P2 112.3(2) . . ? C6 C5 P2 114.8(2) . . ? C4 C5 H5 106.1 . . ? C6 C5 H5 106.1 . . ? P2 C5 H5 106.1 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C13 120.6(2) . . ? C8 C7 P2 125.3(2) . . ? C13 C7 P2 114.0(2) . . ? C9 C8 C7 121.8(3) . . ? C9 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C8 C9 C11 117.1(3) . . ? C8 C9 C10 122.4(3) . . ? C11 C9 C10 120.5(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C9 122.9(3) . . ? C12 C11 H11 118.6 . . ? C9 C11 H11 118.6 . . ? C11 C12 C13 120.2(3) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? N1 C13 C7 119.0(2) . . ? N1 C13 C12 123.7(3) . . ? C7 C13 C12 117.3(3) . . ? C15 C14 C20 119.3(3) . . ? C15 C14 N1 122.3(2) . . ? C20 C14 N1 118.4(2) . . ? C16 C15 C14 120.0(3) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 121.8(3) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C19 C17 C16 118.2(3) . . ? C19 C17 C18 121.0(3) . . ? C16 C17 C18 120.8(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 C20 120.5(3) . . ? C17 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C14 C20 C19 120.2(2) . . ? C14 C20 P1 116.2(2) . . ? C19 C20 P1 123.5(2) . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C21 110.8(3) . . ? C23 C22 P1 112.0(2) . . ? C21 C22 P1 110.5(2) . . ? C23 C22 H22 107.8 . . ? C21 C22 H22 107.8 . . ? P1 C22 H22 107.8 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C25 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C24 C25 C26 110.5(3) . . ? C24 C25 P1 111.3(2) . . ? C26 C25 P1 116.1(2) . . ? C24 C25 H25 106.1 . . ? C26 C25 H25 106.1 . . ? P1 C25 H25 106.1 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? P1 C27 Rh1 114.49(14) . . ? P1 C27 H27A 108.1(18) . . ? Rh1 C27 H27A 113.9(18) . . ? P1 C27 H27B 109(2) . . ? Rh1 C27 H27B 102(2) . . ? H27A C27 H27B 109(3) . . ? Cl7 C28 Cl8 112.4(3) . . ? Cl7 C28 H28A 109.1 . . ? Cl8 C28 H28A 109.1 . . ? Cl7 C28 H28B 109.1 . . ? Cl8 C28 H28B 109.1 . . ? H28A C28 H28B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Rh1 Zr1 Cl4 132.70(9) . . . . ? C27 Rh1 Zr1 Cl4 15.15(10) . . . . ? P2 Rh1 Zr1 Cl4 -114.21(4) . . . . ? Cl2 Rh1 Zr1 Cl4 -47.29(3) . . . . ? Cl3 Rh1 Zr1 Cl4 -175.52(3) . . . . ? Cl1 Rh1 Zr1 Cl4 69.04(3) . . . . ? N1 Rh1 Zr1 Cl6 8.19(9) . . . . ? C27 Rh1 Zr1 Cl6 -109.36(10) . . . . ? P2 Rh1 Zr1 Cl6 121.28(4) . . . . ? Cl2 Rh1 Zr1 Cl6 -171.80(3) . . . . ? Cl3 Rh1 Zr1 Cl6 59.97(4) . . . . ? Cl1 Rh1 Zr1 Cl6 -55.48(4) . . . . ? N1 Rh1 Zr1 Cl5 -110.57(9) . . . . ? C27 Rh1 Zr1 Cl5 131.88(10) . . . . ? P2 Rh1 Zr1 Cl5 2.51(3) . . . . ? Cl2 Rh1 Zr1 Cl5 69.44(3) . . . . ? Cl3 Rh1 Zr1 Cl5 -58.79(3) . . . . ? Cl1 Rh1 Zr1 Cl5 -174.24(3) . . . . ? N1 Rh1 Zr1 Cl1 63.66(9) . . . . ? C27 Rh1 Zr1 Cl1 -53.88(10) . . . . ? P2 Rh1 Zr1 Cl1 176.75(3) . . . . ? Cl2 Rh1 Zr1 Cl1 -116.32(3) . . . . ? Cl3 Rh1 Zr1 Cl1 115.45(3) . . . . ? N1 Rh1 Zr1 Cl3 -51.78(9) . . . . ? C27 Rh1 Zr1 Cl3 -169.33(10) . . . . ? P2 Rh1 Zr1 Cl3 61.30(3) . . . . ? Cl2 Rh1 Zr1 Cl3 128.23(3) . . . . ? Cl1 Rh1 Zr1 Cl3 -115.45(3) . . . . ? N1 Rh1 Zr1 Cl2 179.99(9) . . . . ? C27 Rh1 Zr1 Cl2 62.44(10) . . . . ? P2 Rh1 Zr1 Cl2 -66.92(3) . . . . ? Cl3 Rh1 Zr1 Cl2 -128.23(3) . . . . ? Cl1 Rh1 Zr1 Cl2 116.32(3) . . . . ? Cl4 Zr1 Cl1 Rh1 -126.96(2) . . . . ? Cl6 Zr1 Cl1 Rh1 138.39(3) . . . . ? Cl5 Zr1 Cl1 Rh1 21.35(12) . . . . ? Cl3 Zr1 Cl1 Rh1 43.92(2) . . . . ? Cl2 Zr1 Cl1 Rh1 -41.79(2) . . . . ? N1 Rh1 Cl1 Zr1 -134.09(7) . . . . ? C27 Rh1 Cl1 Zr1 136.86(8) . . . . ? Cl2 Rh1 Cl1 Zr1 44.73(2) . . . . ? Cl3 Rh1 Cl1 Zr1 -44.49(2) . . . . ? C27 Rh1 Cl2 Zr1 -131.38(9) . . . . ? P2 Rh1 Cl2 Zr1 131.81(2) . . . . ? Cl3 Rh1 Cl2 Zr1 36.97(2) . . . . ? Cl1 Rh1 Cl2 Zr1 -43.58(2) . . . . ? Cl4 Zr1 Cl2 Rh1 141.14(3) . . . . ? Cl5 Zr1 Cl2 Rh1 -122.16(3) . . . . ? Cl1 Zr1 Cl2 Rh1 44.98(2) . . . . ? Cl3 Zr1 Cl2 Rh1 -36.79(2) . . . . ? N1 Rh1 Cl3 Zr1 141.34(7) . . . . ? C27 Rh1 Cl3 Zr1 50.9(4) . . . . ? P2 Rh1 Cl3 Zr1 -134.98(2) . . . . ? Cl2 Rh1 Cl3 Zr1 -37.63(2) . . . . ? Cl1 Rh1 Cl3 Zr1 44.18(2) . . . . ? Cl6 Zr1 Cl3 Rh1 -135.58(3) . . . . ? Cl5 Zr1 Cl3 Rh1 129.29(3) . . . . ? Cl1 Zr1 Cl3 Rh1 -45.21(2) . . . . ? Cl2 Zr1 Cl3 Rh1 35.29(2) . . . . ? N1 Rh1 P2 C7 3.55(11) . . . . ? C27 Rh1 P2 C7 92.11(12) . . . . ? Cl2 Rh1 P2 C7 -175.18(9) . . . . ? Cl3 Rh1 P2 C7 -86.71(9) . . . . ? Zr1 Rh1 P2 C7 -129.06(9) . . . . ? N1 Rh1 P2 C5 -113.87(13) . . . . ? C27 Rh1 P2 C5 -25.31(13) . . . . ? Cl2 Rh1 P2 C5 67.40(11) . . . . ? Cl3 Rh1 P2 C5 155.87(11) . . . . ? Zr1 Rh1 P2 C5 113.51(11) . . . . ? N1 Rh1 P2 C2 120.06(13) . . . . ? C27 Rh1 P2 C2 -151.39(13) . . . . ? Cl2 Rh1 P2 C2 -58.67(11) . . . . ? Cl3 Rh1 P2 C2 29.80(11) . . . . ? Zr1 Rh1 P2 C2 -12.56(12) . . . . ? C27 Rh1 N1 C13 -101.5(2) . . . . ? P2 Rh1 N1 C13 -4.9(2) . . . . ? Cl3 Rh1 N1 C13 90.1(2) . . . . ? Cl1 Rh1 N1 C13 170.5(2) . . . . ? Zr1 Rh1 N1 C13 127.07(18) . . . . ? C27 Rh1 N1 C14 73.5(2) . . . . ? P2 Rh1 N1 C14 170.17(19) . . . . ? Cl3 Rh1 N1 C14 -94.81(19) . . . . ? Cl1 Rh1 N1 C14 -14.4(2) . . . . ? Zr1 Rh1 N1 C14 -57.9(2) . . . . ? C7 P2 C2 C1 157.2(2) . . . . ? C5 P2 C2 C1 -87.3(2) . . . . ? Rh1 P2 C2 C1 43.6(3) . . . . ? C7 P2 C2 C3 29.8(3) . . . . ? C5 P2 C2 C3 145.2(2) . . . . ? Rh1 P2 C2 C3 -83.8(2) . . . . ? C7 P2 C5 C4 178.2(2) . . . . ? C2 P2 C5 C4 64.1(2) . . . . ? Rh1 P2 C5 C4 -68.6(2) . . . . ? C7 P2 C5 C6 50.7(3) . . . . ? C2 P2 C5 C6 -63.5(3) . . . . ? Rh1 P2 C5 C6 163.9(2) . . . . ? C5 P2 C7 C8 -63.3(3) . . . . ? C2 P2 C7 C8 49.7(3) . . . . ? Rh1 P2 C7 C8 174.4(2) . . . . ? C5 P2 C7 C13 119.6(2) . . . . ? C2 P2 C7 C13 -127.4(2) . . . . ? Rh1 P2 C7 C13 -2.7(2) . . . . ? C13 C7 C8 C9 -1.5(4) . . . . ? P2 C7 C8 C9 -178.5(2) . . . . ? C7 C8 C9 C11 -1.3(4) . . . . ? C7 C8 C9 C10 178.7(3) . . . . ? C8 C9 C11 C12 1.9(4) . . . . ? C10 C9 C11 C12 -178.1(3) . . . . ? C9 C11 C12 C13 0.5(4) . . . . ? C14 N1 C13 C7 -170.4(2) . . . . ? Rh1 N1 C13 C7 4.5(3) . . . . ? C14 N1 C13 C12 7.8(4) . . . . ? Rh1 N1 C13 C12 -177.3(2) . . . . ? C8 C7 C13 N1 -177.8(3) . . . . ? P2 C7 C13 N1 -0.6(3) . . . . ? C8 C7 C13 C12 3.8(4) . . . . ? P2 C7 C13 C12 -178.9(2) . . . . ? C11 C12 C13 N1 178.4(3) . . . . ? C11 C12 C13 C7 -3.3(4) . . . . ? C13 N1 C14 C15 -71.3(4) . . . . ? Rh1 N1 C14 C15 113.6(3) . . . . ? C13 N1 C14 C20 110.5(3) . . . . ? Rh1 N1 C14 C20 -64.6(3) . . . . ? C20 C14 C15 C16 -1.7(4) . . . . ? N1 C14 C15 C16 -179.9(3) . . . . ? C14 C15 C16 C17 0.9(4) . . . . ? C15 C16 C17 C19 0.5(4) . . . . ? C15 C16 C17 C18 -179.4(3) . . . . ? C16 C17 C19 C20 -1.0(4) . . . . ? C18 C17 C19 C20 178.9(3) . . . . ? C15 C14 C20 C19 1.2(4) . . . . ? N1 C14 C20 C19 179.5(2) . . . . ? C15 C14 C20 P1 177.3(2) . . . . ? N1 C14 C20 P1 -4.5(3) . . . . ? C17 C19 C20 C14 0.2(4) . . . . ? C17 C19 C20 P1 -175.6(2) . . . . ? C27 P1 C20 C14 46.2(3) . . . . ? C22 P1 C20 C14 166.2(2) . . . . ? C25 P1 C20 C14 -73.7(2) . . . . ? C27 P1 C20 C19 -137.9(2) . . . . ? C22 P1 C20 C19 -17.9(3) . . . . ? C25 P1 C20 C19 102.2(3) . . . . ? C20 P1 C22 C23 171.5(2) . . . . ? C27 P1 C22 C23 -66.0(3) . . . . ? C25 P1 C22 C23 55.8(3) . . . . ? C20 P1 C22 C21 -64.5(2) . . . . ? C27 P1 C22 C21 58.0(2) . . . . ? C25 P1 C22 C21 179.8(2) . . . . ? C20 P1 C25 C24 -52.0(3) . . . . ? C27 P1 C25 C24 -174.1(2) . . . . ? C22 P1 C25 C24 64.4(3) . . . . ? C20 P1 C25 C26 -179.6(2) . . . . ? C27 P1 C25 C26 58.3(3) . . . . ? C22 P1 C25 C26 -63.2(3) . . . . ? C20 P1 C27 Rh1 -21.1(2) . . . . ? C22 P1 C27 Rh1 -139.95(15) . . . . ? C25 P1 C27 Rh1 96.53(17) . . . . ? N1 Rh1 C27 P1 -23.13(16) . . . . ? P2 Rh1 C27 P1 -106.65(15) . . . . ? Cl2 Rh1 C27 P1 155.58(15) . . . . ? Cl3 Rh1 C27 P1 67.5(5) . . . . ? Cl1 Rh1 C27 P1 74.09(15) . . . . ? Zr1 Rh1 C27 P1 112.04(14) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.081 _refine_diff_density_min -1.199 _refine_diff_density_rms 0.098