# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Jerzy Pikies' _publ_contact_author_address ; Department of Chemistry Technical University of Gdansk 11/12 G. Narutowicz St. 80952 - PL Gdansk, Poland ; _publ_contact_author_phone '048 58 3472622' _publ_contact_author_fax '048 58 3472694' _publ_contact_author_email pikies@chem.pg.gda.pl _publ_section_title ; The New Synthetic Entry to Phosphinophosphinidene Complexes. Synthesis and Structural Characterisation of the First Side-on Bonded and the First Terminally Bonded Phosphinophosphinidene Zirconium Complexes [ì-(1,2:2-ç-tBu2P=P){Zr(Cl)Cp2}2] and [{Zr(PPhMe2)Cp2}(ç1-PPtBu2)]. ; loop_ _publ_author_name 'Jerzy Pikies' 'Elke Baum' 'Jaroslaw Chojnacki' 'Rafal Grubba' 'Eberhard Matern' 'Andrezej Robaszkiewicz' data_pik2 _database_code_depnum_ccdc_archive 'CCDC 225538' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [\m- (1,2:2 - \h - 1,1-ditertbutyldiphosphene) bis(dicyclopentadienatochlorozirconium)] ; _chemical_name_common ; (mu- (1,2:2 - eta - 1,1-ditertbutyldiphosphene) bis(dicyclopentadienatochlorozirconium)) ; _chemical_melting_point ? _chemical_formula_moiety 'C28 H38 Cl2 P2 Zr2' _chemical_formula_sum 'C28 H38 Cl2 P2 Zr2' _chemical_formula_weight 689.86 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' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.7489(4) _cell_length_b 23.9432(10) _cell_length_c 11.5529(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.026(3) _cell_angle_gamma 90.00 _cell_volume 2908.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 27.15 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 1.026 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4829 _exptl_absorpt_correction_T_max 0.6922 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_source_voltage 45 _diffrn_source_current 40 _diffrn_source_power 1.80 _diffrn_radiation_monochromator graphite _diffrn_detector 'images plate (34 cm diameter)' _diffrn_detector_area_resol_mean 6.67 _diffrn_measurement_device '2-circle- goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 276 frames, detector distance = 120 mm ; _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15035 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5063 _reflns_number_gt 4713 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL _computing_publication_material SHELX _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+1.1609P] 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 5063 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0228 _refine_ls_R_factor_gt 0.0206 _refine_ls_wR_factor_ref 0.0539 _refine_ls_wR_factor_gt 0.0530 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 Zr1 Zr 0.874501(17) 0.086168(7) 0.179985(14) 0.01690(6) Uani 1 1 d . . . Cl1 Cl 0.85479(5) -0.015745(18) 0.24402(5) 0.03113(12) Uani 1 1 d . . . C1 C 0.6802(2) 0.06853(9) 0.01528(16) 0.0279(4) Uani 1 1 d . . . H1 H 0.6041 0.0565 0.0371 0.033 Uiso 1 1 calc R . . C2 C 0.7770(2) 0.03383(9) -0.01024(17) 0.0325(5) Uani 1 1 d . . . H2 H 0.7769 -0.0058 -0.0095 0.039 Uiso 1 1 calc R . . C3 C 0.8728(2) 0.06768(10) -0.03679(17) 0.0340(5) Uani 1 1 d . . . H3 H 0.9490 0.0551 -0.0578 0.041 Uiso 1 1 calc R . . C4 C 0.8368(2) 0.12372(9) -0.02705(15) 0.0303(5) Uani 1 1 d . . . H4 H 0.8853 0.1556 -0.0386 0.036 Uiso 1 1 calc R . . C5 C 0.7167(2) 0.12429(9) 0.00270(15) 0.0281(4) Uani 1 1 d . . . H5 H 0.6686 0.1566 0.0126 0.034 Uiso 1 1 calc R . . C6 C 1.10422(18) 0.05210(8) 0.22393(16) 0.0238(4) Uani 1 1 d . . . H6 H 1.1174 0.0139 0.2080 0.029 Uiso 1 1 calc R . . C7 C 1.10196(19) 0.09635(9) 0.14518(17) 0.0270(4) Uani 1 1 d . . . H7 H 1.1167 0.0937 0.0671 0.032 Uiso 1 1 calc R . . C8 C 1.07420(19) 0.14553(8) 0.20063(18) 0.0273(4) Uani 1 1 d . . . H8 H 1.0629 0.1816 0.1657 0.033 Uiso 1 1 calc R . . C9 C 1.06612(18) 0.13175(8) 0.31785(18) 0.0258(4) Uani 1 1 d . . . H9 H 1.0515 0.1572 0.3766 0.031 Uiso 1 1 calc R . . C10 C 1.08333(18) 0.07426(8) 0.33219(16) 0.0237(4) Uani 1 1 d . . . H10 H 1.0814 0.0536 0.4020 0.028 Uiso 1 1 calc R . . Zr2 Zr 0.711401(17) 0.276303(7) 0.232800(13) 0.01671(6) Uani 1 1 d . . . Cl2 Cl 0.54856(5) 0.26363(2) 0.04863(4) 0.02723(11) Uani 1 1 d . . . C11 C 0.8864(2) 0.27488(8) 0.11865(17) 0.0271(4) Uani 1 1 d . . . H11 H 0.8917 0.2435 0.0697 0.032 Uiso 1 1 calc R . . C12 C 0.8172(2) 0.32403(9) 0.08480(18) 0.0341(5) Uani 1 1 d . . . H12 H 0.7689 0.3320 0.0079 0.041 Uiso 1 1 calc R . . C13 C 0.8312(2) 0.35915(8) 0.1829(2) 0.0363(5) Uani 1 1 d . . . H13 H 0.7931 0.3948 0.1851 0.044 Uiso 1 1 calc R . . C14 C 0.9117(2) 0.33224(9) 0.27798(19) 0.0330(5) Uani 1 1 d . . . H14 H 0.9378 0.3468 0.3558 0.040 Uiso 1 1 calc R . . C15 C 0.9467(2) 0.28070(8) 0.23899(18) 0.0267(4) Uani 1 1 d . . . H15 H 1.0014 0.2542 0.2851 0.032 Uiso 1 1 calc R . . C16 C 0.5107(2) 0.28472(10) 0.31279(19) 0.0335(5) Uani 1 1 d . . . H16 H 0.4332 0.2697 0.2690 0.040 Uiso 1 1 calc R . . C17 C 0.5568(2) 0.33904(9) 0.30189(19) 0.0362(5) Uani 1 1 d . . . H17 H 0.5170 0.3669 0.2483 0.043 Uiso 1 1 calc R . . C18 C 0.6713(2) 0.34473(8) 0.38358(18) 0.0346(5) Uani 1 1 d . . . H18 H 0.7217 0.3776 0.3970 0.042 Uiso 1 1 calc R . . C19 C 0.6995(2) 0.29374(9) 0.44267(16) 0.0310(5) Uani 1 1 d . . . H19 H 0.7732 0.2856 0.5014 0.037 Uiso 1 1 calc R . . C20 C 0.5988(2) 0.25686(8) 0.39927(17) 0.0285(4) Uani 1 1 d . . . H20 H 0.5919 0.2194 0.4245 0.034 Uiso 1 1 calc R . . P1 P 0.77787(4) 0.174355(18) 0.27382(4) 0.01652(10) Uani 1 1 d . . . P2 P 0.69037(4) 0.101261(18) 0.32133(4) 0.01688(10) Uani 1 1 d . . . C21 C 0.51015(18) 0.09379(8) 0.27203(15) 0.0209(4) Uani 1 1 d . . . C22 C 0.46367(19) 0.12995(8) 0.16213(16) 0.0269(4) Uani 1 1 d . . . H22A H 0.5073 0.1187 0.0994 0.040 Uiso 1 1 calc R . . H22B H 0.4822 0.1693 0.1821 0.040 Uiso 1 1 calc R . . H22C H 0.3717 0.1250 0.1347 0.040 Uiso 1 1 calc R . . C23 C 0.4806(2) 0.03197(8) 0.24096(18) 0.0292(4) Uani 1 1 d . . . H23A H 0.3894 0.0276 0.2081 0.044 Uiso 1 1 calc R . . H23B H 0.5044 0.0092 0.3126 0.044 Uiso 1 1 calc R . . H23C H 0.5290 0.0198 0.1824 0.044 Uiso 1 1 calc R . . C24 C 0.4337(2) 0.11256(9) 0.36364(17) 0.0284(4) Uani 1 1 d . . . H24A H 0.3426 0.1080 0.3306 0.043 Uiso 1 1 calc R . . H24B H 0.4519 0.1519 0.3836 0.043 Uiso 1 1 calc R . . H24C H 0.4577 0.0897 0.4352 0.043 Uiso 1 1 calc R . . C25 C 0.73864(19) 0.08521(7) 0.48661(15) 0.0226(4) Uani 1 1 d . . . C26 C 0.88240(19) 0.07762(8) 0.51520(17) 0.0272(4) Uani 1 1 d . . . H26A H 0.9234 0.1126 0.5000 0.041 Uiso 1 1 calc R . . H26B H 0.9059 0.0480 0.4653 0.041 Uiso 1 1 calc R . . H26C H 0.9104 0.0674 0.5987 0.041 Uiso 1 1 calc R . . C27 C 0.7056(2) 0.13142(9) 0.56650(16) 0.0315(5) Uani 1 1 d . . . H27A H 0.7356 0.1208 0.6496 0.047 Uiso 1 1 calc R . . H27B H 0.6132 0.1367 0.5504 0.047 Uiso 1 1 calc R . . H27C H 0.7467 0.1663 0.5507 0.047 Uiso 1 1 calc R . . C28 C 0.6805(2) 0.02895(9) 0.51202(18) 0.0311(5) Uani 1 1 d . . . H28A H 0.7008 0.0005 0.4578 0.047 Uiso 1 1 calc R . . H28B H 0.5880 0.0328 0.5006 0.047 Uiso 1 1 calc R . . H28C H 0.7158 0.0177 0.5938 0.047 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 Zr1 0.01430(11) 0.01753(9) 0.01879(9) -0.00323(6) 0.00329(7) 0.00013(6) Cl1 0.0295(3) 0.0172(2) 0.0453(3) -0.00055(19) 0.0044(2) -0.00070(18) C1 0.0194(12) 0.0429(11) 0.0197(8) -0.0091(8) 0.0001(8) -0.0036(8) C2 0.0337(14) 0.0341(11) 0.0266(9) -0.0150(9) -0.0007(9) -0.0010(9) C3 0.0275(13) 0.0520(13) 0.0233(9) -0.0154(9) 0.0067(9) 0.0011(10) C4 0.0362(13) 0.0392(11) 0.0162(8) -0.0026(8) 0.0067(8) -0.0055(9) C5 0.0327(13) 0.0357(11) 0.0138(8) -0.0029(8) 0.0003(8) 0.0061(9) C6 0.0149(11) 0.0247(9) 0.0318(9) -0.0055(8) 0.0046(8) 0.0022(7) C7 0.0140(11) 0.0394(11) 0.0280(9) -0.0017(8) 0.0057(8) 0.0004(8) C8 0.0126(11) 0.0251(9) 0.0432(11) 0.0012(8) 0.0034(8) -0.0017(7) C9 0.0114(11) 0.0296(10) 0.0349(10) -0.0114(8) 0.0017(8) -0.0007(7) C10 0.0136(11) 0.0311(10) 0.0250(9) -0.0018(8) 0.0007(7) 0.0012(7) Zr2 0.01856(11) 0.01674(9) 0.01524(9) 0.00113(6) 0.00447(7) 0.00199(6) Cl2 0.0280(3) 0.0309(2) 0.0198(2) 0.00558(18) -0.00189(18) -0.00039(19) C11 0.0241(12) 0.0326(10) 0.0281(9) 0.0001(8) 0.0138(8) -0.0042(8) C12 0.0256(13) 0.0459(12) 0.0324(10) 0.0203(10) 0.0100(9) -0.0014(9) C13 0.0325(13) 0.0202(9) 0.0608(14) 0.0077(10) 0.0200(11) -0.0008(8) C14 0.0310(13) 0.0322(10) 0.0366(11) -0.0078(9) 0.0086(9) -0.0110(9) C15 0.0184(11) 0.0297(10) 0.0323(10) 0.0055(8) 0.0059(8) -0.0025(8) C16 0.0231(13) 0.0477(13) 0.0333(10) -0.0071(10) 0.0141(9) 0.0036(9) C17 0.0491(15) 0.0333(11) 0.0317(10) 0.0067(9) 0.0208(10) 0.0209(10) C18 0.0537(15) 0.0228(9) 0.0335(10) -0.0091(9) 0.0232(10) -0.0016(9) C19 0.0378(14) 0.0382(11) 0.0180(8) -0.0039(8) 0.0084(8) 0.0063(9) C20 0.0376(13) 0.0260(9) 0.0281(9) 0.0016(8) 0.0210(9) 0.0049(9) P1 0.0159(3) 0.0169(2) 0.0177(2) 0.00056(16) 0.00546(17) 0.00069(16) P2 0.0146(3) 0.0190(2) 0.0169(2) 0.00187(17) 0.00293(17) -0.00041(17) C21 0.0153(10) 0.0260(9) 0.0214(8) 0.0005(7) 0.0040(7) -0.0027(7) C22 0.0180(11) 0.0362(11) 0.0254(9) 0.0048(8) 0.0016(8) 0.0011(8) C23 0.0244(12) 0.0302(10) 0.0319(10) -0.0023(8) 0.0033(8) -0.0091(8) C24 0.0185(12) 0.0381(11) 0.0299(9) -0.0004(9) 0.0080(8) -0.0001(8) C25 0.0239(11) 0.0252(9) 0.0190(8) 0.0059(7) 0.0048(8) -0.0016(7) C26 0.0202(12) 0.0354(10) 0.0234(9) 0.0080(8) -0.0016(8) -0.0017(8) C27 0.0356(13) 0.0401(11) 0.0180(8) 0.0001(8) 0.0036(8) 0.0022(9) C28 0.0280(13) 0.0334(11) 0.0311(10) 0.0136(9) 0.0046(9) -0.0053(9) _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 Zr1 C4 2.5079(18) . ? Zr1 C3 2.5395(18) . ? Zr1 C5 2.5412(19) . ? Zr1 C8 2.5439(19) . ? Zr1 C6 2.5491(19) . ? Zr1 C1 2.5505(19) . ? Zr1 C2 2.5572(18) . ? Zr1 C10 2.5627(19) . ? Zr1 C9 2.5697(19) . ? Zr1 C7 2.571(2) . ? Zr1 Cl1 2.5713(5) . ? Zr1 P1 2.6798(5) . ? C1 C5 1.408(3) . ? C1 C2 1.409(3) . ? C1 H1 0.9500 . ? C2 C3 1.394(3) . ? C2 H2 0.9500 . ? C3 C4 1.408(3) . ? C3 H3 0.9500 . ? C4 C5 1.403(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.394(3) . ? C6 C10 1.419(3) . ? C6 H6 0.9500 . ? C7 C8 1.402(3) . ? C7 H7 0.9500 . ? C8 C9 1.414(3) . ? C8 H8 0.9500 . ? C9 C10 1.394(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? Zr2 Cl2 2.4761(5) . ? Zr2 C19 2.4898(18) . ? Zr2 C17 2.491(2) . ? Zr2 C18 2.4935(18) . ? Zr2 C14 2.496(2) . ? Zr2 C13 2.497(2) . ? Zr2 C11 2.5124(19) . ? Zr2 C12 2.5164(19) . ? Zr2 C15 2.518(2) . ? Zr2 C20 2.5203(18) . ? Zr2 C16 2.526(2) . ? Zr2 P1 2.5597(5) . ? C11 C12 1.404(3) . ? C11 C15 1.413(3) . ? C11 H11 0.9500 . ? C12 C13 1.394(3) . ? C12 H12 0.9500 . ? C13 C14 1.405(3) . ? C13 H13 0.9500 . ? C14 C15 1.392(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C20 1.395(3) . ? C16 C17 1.407(3) . ? C16 H16 0.9500 . ? C17 C18 1.392(3) . ? C17 H17 0.9500 . ? C18 C19 1.401(3) . ? C18 H18 0.9500 . ? C19 C20 1.406(3) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? P1 P2 2.1128(6) . ? P2 C21 1.910(2) . ? P2 C25 1.9104(18) . ? C21 C22 1.532(2) . ? C21 C24 1.537(3) . ? C21 C23 1.541(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.522(3) . ? C25 C27 1.530(3) . ? C25 C28 1.538(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Zr1 C3 32.38(7) . . ? C4 Zr1 C5 32.26(7) . . ? C3 Zr1 C5 53.22(7) . . ? C4 Zr1 C8 81.65(7) . . ? C3 Zr1 C8 91.29(7) . . ? C5 Zr1 C8 106.46(7) . . ? C4 Zr1 C6 105.20(7) . . ? C3 Zr1 C6 87.04(7) . . ? C5 Zr1 C6 137.03(6) . . ? C8 Zr1 C6 52.90(6) . . ? C4 Zr1 C1 53.36(7) . . ? C3 Zr1 C1 53.05(7) . . ? C5 Zr1 C1 32.10(7) . . ? C8 Zr1 C1 134.93(7) . . ? C6 Zr1 C1 134.77(6) . . ? C4 Zr1 C2 53.14(7) . . ? C3 Zr1 C2 31.75(7) . . ? C5 Zr1 C2 52.99(7) . . ? C8 Zr1 C2 122.77(7) . . ? C6 Zr1 C2 102.77(7) . . ? C1 Zr1 C2 32.04(7) . . ? C4 Zr1 C10 129.70(7) . . ? C3 Zr1 C10 118.86(7) . . ? C5 Zr1 C10 159.25(7) . . ? C8 Zr1 C10 52.88(6) . . ? C6 Zr1 C10 32.23(6) . . ? C1 Zr1 C10 163.24(7) . . ? C2 Zr1 C10 132.75(7) . . ? C4 Zr1 C9 112.85(7) . . ? C3 Zr1 C9 121.70(7) . . ? C5 Zr1 C9 131.39(7) . . ? C8 Zr1 C9 32.10(6) . . ? C6 Zr1 C9 52.73(6) . . ? C1 Zr1 C9 163.49(7) . . ? C2 Zr1 C9 150.81(7) . . ? C10 Zr1 C9 31.53(6) . . ? C4 Zr1 C7 77.70(7) . . ? C3 Zr1 C7 70.97(7) . . ? C5 Zr1 C7 109.68(7) . . ? C8 Zr1 C7 31.82(6) . . ? C6 Zr1 C7 31.59(6) . . ? C1 Zr1 C7 123.83(6) . . ? C2 Zr1 C7 98.34(7) . . ? C10 Zr1 C7 52.57(6) . . ? C9 Zr1 C7 52.49(6) . . ? C4 Zr1 Cl1 127.44(5) . . ? C3 Zr1 Cl1 97.71(6) . . ? C5 Zr1 Cl1 119.45(5) . . ? C8 Zr1 Cl1 128.44(5) . . ? C6 Zr1 Cl1 76.91(5) . . ? C1 Zr1 Cl1 87.35(5) . . ? C2 Zr1 Cl1 74.85(5) . . ? C10 Zr1 Cl1 79.04(5) . . ? C9 Zr1 Cl1 109.16(5) . . ? C7 Zr1 Cl1 105.85(5) . . ? C4 Zr1 P1 95.97(5) . . ? C3 Zr1 P1 127.77(6) . . ? C5 Zr1 P1 78.06(4) . . ? C8 Zr1 P1 84.98(5) . . ? C6 Zr1 P1 127.77(4) . . ? C1 Zr1 P1 96.09(5) . . ? C2 Zr1 P1 127.57(5) . . ? C10 Zr1 P1 99.67(4) . . ? C9 Zr1 P1 75.09(4) . . ? C7 Zr1 P1 116.74(5) . . ? Cl1 Zr1 P1 124.696(16) . . ? C5 C1 C2 107.68(19) . . ? C5 C1 Zr1 73.59(11) . . ? C2 C1 Zr1 74.24(11) . . ? C5 C1 H1 126.2 . . ? C2 C1 H1 126.2 . . ? Zr1 C1 H1 118.0 . . ? C3 C2 C1 108.34(19) . . ? C3 C2 Zr1 73.43(11) . . ? C1 C2 Zr1 73.72(11) . . ? C3 C2 H2 125.8 . . ? C1 C2 H2 125.8 . . ? Zr1 C2 H2 118.9 . . ? C2 C3 C4 107.96(19) . . ? C2 C3 Zr1 74.83(11) . . ? C4 C3 Zr1 72.57(10) . . ? C2 C3 H3 126.0 . . ? C4 C3 H3 126.0 . . ? Zr1 C3 H3 118.5 . . ? C5 C4 C3 108.14(19) . . ? C5 C4 Zr1 75.18(10) . . ? C3 C4 Zr1 75.05(12) . . ? C5 C4 H4 125.9 . . ? C3 C4 H4 125.9 . . ? Zr1 C4 H4 116.0 . . ? C4 C5 C1 107.84(18) . . ? C4 C5 Zr1 72.56(11) . . ? C1 C5 Zr1 74.32(11) . . ? C4 C5 H5 126.1 . . ? C1 C5 H5 126.1 . . ? Zr1 C5 H5 118.9 . . ? C7 C6 C10 107.86(17) . . ? C7 C6 Zr1 75.06(11) . . ? C10 C6 Zr1 74.41(11) . . ? C7 C6 H6 126.1 . . ? C10 C6 H6 126.1 . . ? Zr1 C6 H6 116.6 . . ? C6 C7 C8 108.46(16) . . ? C6 C7 Zr1 73.35(11) . . ? C8 C7 Zr1 73.04(11) . . ? C6 C7 H7 125.8 . . ? C8 C7 H7 125.8 . . ? Zr1 C7 H7 119.6 . . ? C7 C8 C9 107.64(17) . . ? C7 C8 Zr1 75.15(11) . . ? C9 C8 Zr1 74.95(11) . . ? C7 C8 H8 126.2 . . ? C9 C8 H8 126.2 . . ? Zr1 C8 H8 115.9 . . ? C10 C9 C8 108.12(17) . . ? C10 C9 Zr1 73.96(11) . . ? C8 C9 Zr1 72.95(11) . . ? C10 C9 H9 125.9 . . ? C8 C9 H9 125.9 . . ? Zr1 C9 H9 119.0 . . ? C9 C10 C6 107.82(17) . . ? C9 C10 Zr1 74.52(11) . . ? C6 C10 Zr1 73.36(11) . . ? C9 C10 H10 126.1 . . ? C6 C10 H10 126.1 . . ? Zr1 C10 H10 118.0 . . ? Cl2 Zr2 C19 133.37(6) . . ? Cl2 Zr2 C17 87.13(6) . . ? C19 Zr2 C17 54.11(7) . . ? Cl2 Zr2 C18 119.12(6) . . ? C19 Zr2 C18 32.65(7) . . ? C17 Zr2 C18 32.44(8) . . ? Cl2 Zr2 C14 132.05(5) . . ? C19 Zr2 C14 85.62(7) . . ? C17 Zr2 C14 102.30(8) . . ? C18 Zr2 C14 76.61(7) . . ? Cl2 Zr2 C13 101.85(6) . . ? C19 Zr2 C13 103.01(8) . . ? C17 Zr2 C13 90.30(7) . . ? C18 Zr2 C13 79.15(7) . . ? C14 Zr2 C13 32.68(8) . . ? Cl2 Zr2 C11 91.14(5) . . ? C19 Zr2 C11 135.20(7) . . ? C17 Zr2 C11 143.00(7) . . ? C18 Zr2 C11 129.27(7) . . ? C14 Zr2 C11 53.82(7) . . ? C13 Zr2 C11 53.93(7) . . ? Cl2 Zr2 C12 79.07(5) . . ? C19 Zr2 C12 135.06(8) . . ? C17 Zr2 C12 111.70(7) . . ? C18 Zr2 C12 110.16(7) . . ? C14 Zr2 C12 53.59(7) . . ? C13 Zr2 C12 32.29(8) . . ? C11 Zr2 C12 32.42(7) . . ? Cl2 Zr2 C15 123.76(5) . . ? C19 Zr2 C15 102.75(7) . . ? C17 Zr2 C15 134.33(8) . . ? C18 Zr2 C15 105.76(7) . . ? C14 Zr2 C15 32.24(7) . . ? C13 Zr2 C15 53.84(7) . . ? C11 Zr2 C15 32.63(7) . . ? C12 Zr2 C15 53.62(7) . . ? Cl2 Zr2 C20 105.49(5) . . ? C19 Zr2 C20 32.58(7) . . ? C17 Zr2 C20 53.73(7) . . ? C18 Zr2 C20 53.68(7) . . ? C14 Zr2 C20 118.03(7) . . ? C13 Zr2 C20 132.50(7) . . ? C11 Zr2 C20 158.33(7) . . ? C12 Zr2 C20 163.60(7) . . ? C15 Zr2 C20 128.73(7) . . ? Cl2 Zr2 C16 79.59(5) . . ? C19 Zr2 C16 53.78(7) . . ? C17 Zr2 C16 32.56(8) . . ? C18 Zr2 C16 53.61(8) . . ? C14 Zr2 C16 130.22(7) . . ? C13 Zr2 C16 122.81(7) . . ? C11 Zr2 C16 169.45(7) . . ? C12 Zr2 C16 138.90(7) . . ? C15 Zr2 C16 156.34(7) . . ? C20 Zr2 C16 32.09(7) . . ? Cl2 Zr2 P1 99.338(16) . . ? C19 Zr2 P1 92.79(5) . . ? C17 Zr2 P1 134.00(5) . . ? C18 Zr2 P1 125.41(5) . . ? C14 Zr2 P1 106.12(5) . . ? C13 Zr2 P1 131.52(5) . . ? C11 Zr2 P1 82.74(5) . . ? C12 Zr2 P1 114.25(5) . . ? C15 Zr2 P1 78.15(5) . . ? C20 Zr2 P1 80.94(5) . . ? C16 Zr2 P1 103.60(5) . . ? C12 C11 C15 107.41(18) . . ? C12 C11 Zr2 73.95(12) . . ? C15 C11 Zr2 73.88(11) . . ? C12 C11 H11 126.3 . . ? C15 C11 H11 126.3 . . ? Zr2 C11 H11 117.9 . . ? C13 C12 C11 108.54(19) . . ? C13 C12 Zr2 73.08(11) . . ? C11 C12 Zr2 73.64(11) . . ? C13 C12 H12 125.7 . . ? C11 C12 H12 125.7 . . ? Zr2 C12 H12 119.4 . . ? C12 C13 C14 107.67(18) . . ? C12 C13 Zr2 74.63(11) . . ? C14 C13 Zr2 73.65(12) . . ? C12 C13 H13 126.2 . . ? C14 C13 H13 126.2 . . ? Zr2 C13 H13 117.6 . . ? C15 C14 C13 108.52(19) . . ? C15 C14 Zr2 74.72(12) . . ? C13 C14 Zr2 73.67(13) . . ? C15 C14 H14 125.7 . . ? C13 C14 H14 125.7 . . ? Zr2 C14 H14 117.8 . . ? C14 C15 C11 107.83(19) . . ? C14 C15 Zr2 73.04(12) . . ? C11 C15 Zr2 73.49(12) . . ? C14 C15 H15 126.1 . . ? C11 C15 H15 126.1 . . ? Zr2 C15 H15 119.3 . . ? C20 C16 C17 107.9(2) . . ? C20 C16 Zr2 73.72(12) . . ? C17 C16 Zr2 72.35(12) . . ? C20 C16 H16 126.1 . . ? C17 C16 H16 126.1 . . ? Zr2 C16 H16 119.7 . . ? C18 C17 C16 107.95(19) . . ? C18 C17 Zr2 73.87(12) . . ? C16 C17 Zr2 75.09(12) . . ? C18 C17 H17 126.0 . . ? C16 C17 H17 126.0 . . ? Zr2 C17 H17 117.1 . . ? C17 C18 C19 108.41(19) . . ? C17 C18 Zr2 73.69(11) . . ? C19 C18 Zr2 73.53(11) . . ? C17 C18 H18 125.8 . . ? C19 C18 H18 125.8 . . ? Zr2 C18 H18 118.8 . . ? C18 C19 C20 107.54(19) . . ? C18 C19 Zr2 73.82(11) . . ? C20 C19 Zr2 74.90(10) . . ? C18 C19 H19 126.2 . . ? C20 C19 H19 126.2 . . ? Zr2 C19 H19 117.1 . . ? C16 C20 C19 108.21(19) . . ? C16 C20 Zr2 74.19(11) . . ? C19 C20 Zr2 72.51(11) . . ? C16 C20 H20 125.9 . . ? C19 C20 H20 125.9 . . ? Zr2 C20 H20 119.2 . . ? P2 P1 Zr2 135.71(2) . . ? P2 P1 Zr1 71.549(18) . . ? Zr2 P1 Zr1 142.487(18) . . ? C21 P2 C25 109.06(8) . . ? C21 P2 P1 118.61(6) . . ? C25 P2 P1 112.54(6) . . ? C21 P2 Zr1 126.99(6) . . ? C25 P2 Zr1 118.20(6) . . ? P1 P2 Zr1 63.550(17) . . ? C22 C21 C24 106.06(16) . . ? C22 C21 C23 109.52(15) . . ? C24 C21 C23 109.11(16) . . ? C22 C21 P2 109.24(13) . . ? C24 C21 P2 114.97(13) . . ? C23 C21 P2 107.87(13) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C27 107.97(16) . . ? C26 C25 C28 106.74(16) . . ? C27 C25 C28 111.32(16) . . ? C26 C25 P2 107.04(12) . . ? C27 C25 P2 114.12(13) . . ? C28 C25 P2 109.29(13) . . ? 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 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.499 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.053 data_r1 _database_code_depnum_ccdc_archive 'CCDC 232586' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dicyclopentapdienylo(phenyldimethylphosphane)(\h^1^- di-tert-butylphosphanylphosphinidene)zirconium ; _chemical_name_common ; Dicyclopentapdienylo(phenyldimethylphosphane)(eta$1!-di-tert- butylphosphanylphosphinidene)zirconium ; _chemical_melting_point ? _chemical_formula_moiety 'C26 H39 P3 Zr' _chemical_formula_sum 'C26 H39 P3 Zr' _chemical_formula_weight 535.70 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' P P 0.1023 0.0942 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.312(2) _cell_length_b 11.574(2) _cell_length_c 25.220(5) _cell_angle_alpha 78.91(3) _cell_angle_beta 87.11(3) _cell_angle_gamma 85.26(3) _cell_volume 2656.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 26 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 15 _exptl_crystal_description fragment _exptl_crystal_colour blue _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.606 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ; An attempt to perform the psi-scan absorption correction led to worse structure parameters so we decided not to apply it. ; _exptl_special_details ; Atoms C13 C19 and C50 were refined isotropically, because their thermal ellipsoids tended to become negative defined. ; _diffrn_ambient_temperature 150(0.2) _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 'KM4 - Oxford Diffraction' _diffrn_measurement_method '\w - 2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.3 _diffrn_reflns_number 10154 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0746 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.50 _reflns_number_total 9876 _reflns_number_gt 6887 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KM4 Oxford Diffraction' _computing_cell_refinement 'KM4 Oxford Diffraction' _computing_data_reduction 'DATAPROC Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0989P)^2^+66.4172P] 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 9876 _refine_ls_number_parameters 526 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1659 _refine_ls_R_factor_gt 0.1011 _refine_ls_wR_factor_ref 0.3115 _refine_ls_wR_factor_gt 0.2533 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.007 _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 Zr1 Zr 0.69404(11) 0.87668(9) 0.38379(5) 0.0206(3) Uani 1 1 d . . . P1 P 0.6769(3) 1.0761(2) 0.40785(13) 0.0225(6) Uani 1 1 d . . . P2 P 0.7245(3) 1.2223(3) 0.34124(13) 0.0247(7) Uani 1 1 d . . . P3 P 0.3997(3) 0.8899(3) 0.38296(13) 0.0212(6) Uani 1 1 d . . . C1 C 0.8748(13) 0.7588(10) 0.4481(5) 0.029(3) Uani 1 1 d . . . H1 H 0.9742 0.7619 0.4378 0.035 Uiso 1 1 calc R . . C2 C 0.7821(14) 0.6765(11) 0.4363(6) 0.035(3) Uani 1 1 d . . . H2 H 0.8081 0.6152 0.4167 0.043 Uiso 1 1 calc R . . C3 C 0.6448(14) 0.7018(12) 0.4590(6) 0.039(3) Uani 1 1 d . . . H3 H 0.5615 0.6606 0.4574 0.047 Uiso 1 1 calc R . . C4 C 0.6527(14) 0.7978(12) 0.4839(5) 0.036(3) Uani 1 1 d . . . H4 H 0.5752 0.8335 0.5025 0.044 Uiso 1 1 calc R . . C5 C 0.7954(13) 0.8338(11) 0.4771(5) 0.032(3) Uani 1 1 d . . . H5 H 0.8302 0.8977 0.4900 0.039 Uiso 1 1 calc R . . C6 C 0.8839(15) 0.8434(13) 0.3134(6) 0.041(3) Uani 1 1 d . . . H6 H 0.9788 0.8162 0.3243 0.049 Uiso 1 1 calc R . . C7 C 0.8299(14) 0.9626(12) 0.2992(5) 0.034(3) Uani 1 1 d . . . H7 H 0.8825 1.0295 0.2992 0.040 Uiso 1 1 calc R . . C8 C 0.6847(14) 0.9656(12) 0.2849(5) 0.035(3) Uani 1 1 d . . . H8 H 0.6221 1.0342 0.2737 0.042 Uiso 1 1 calc R . . C9 C 0.6496(16) 0.8451(12) 0.2903(6) 0.039(3) Uani 1 1 d . . . H9 H 0.5595 0.8197 0.2829 0.046 Uiso 1 1 calc R . . C10 C 0.7707(16) 0.7719(12) 0.3084(6) 0.040(3) Uani 1 1 d . . . H10 H 0.7765 0.6880 0.3161 0.048 Uiso 1 1 calc R . . C11 C 0.3054(12) 0.9581(10) 0.4355(5) 0.027(3) Uani 1 1 d . . . H11A H 0.3438 1.0344 0.4356 0.032 Uiso 1 1 calc R . . H11B H 0.3196 0.9064 0.4708 0.032 Uiso 1 1 calc R . . H11C H 0.2023 0.9702 0.4284 0.032 Uiso 1 1 calc R . . C12 C 0.3183(13) 0.9794(10) 0.3222(5) 0.029(3) Uani 1 1 d . . . H12A H 0.3600 0.9514 0.2901 0.034 Uiso 1 1 calc R . . H12B H 0.3375 1.0622 0.3198 0.034 Uiso 1 1 calc R . . H12C H 0.2139 0.9722 0.3243 0.034 Uiso 1 1 calc R . . C13 C 0.3110(12) 0.7515(10) 0.3906(5) 0.025(2) Uiso 1 1 d . . . C14 C 0.2747(13) 0.6900(11) 0.4413(5) 0.031(3) Uani 1 1 d . . . H14 H 0.2922 0.7214 0.4723 0.037 Uiso 1 1 calc R . . C15 C 0.2136(13) 0.5838(11) 0.4476(6) 0.036(3) Uani 1 1 d . . . H15 H 0.1914 0.5402 0.4826 0.043 Uiso 1 1 calc R . . C16 C 0.185(2) 0.5412(14) 0.4004(8) 0.060(5) Uani 1 1 d . . . H16 H 0.1429 0.4679 0.4041 0.072 Uiso 1 1 calc R . . C17 C 0.2149(15) 0.6011(12) 0.3511(7) 0.044(4) Uani 1 1 d . . . H17 H 0.1920 0.5713 0.3203 0.053 Uiso 1 1 calc R . . C18 C 0.2787(14) 0.7054(11) 0.3447(5) 0.031(3) Uani 1 1 d . . . H18 H 0.3015 0.7471 0.3094 0.037 Uiso 1 1 calc R . . C19 C 0.9025(13) 1.2695(11) 0.3654(5) 0.029(3) Uiso 1 1 d . . . C20 C 1.0161(12) 1.1773(11) 0.3532(6) 0.035(3) Uani 1 1 d . . . H20A H 1.0145 1.1721 0.3149 0.042 Uiso 1 1 calc R . . H20B H 0.9967 1.1007 0.3756 0.042 Uiso 1 1 calc R . . H20C H 1.1111 1.1989 0.3613 0.042 Uiso 1 1 calc R . . C21 C 0.9075(14) 1.2770(12) 0.4235(6) 0.035(3) Uani 1 1 d . . . H21A H 0.8338 1.3369 0.4319 0.042 Uiso 1 1 calc R . . H21B H 1.0029 1.2988 0.4309 0.042 Uiso 1 1 calc R . . H21C H 0.8890 1.2002 0.4459 0.042 Uiso 1 1 calc R . . C22 C 0.9329(15) 1.3867(11) 0.3293(6) 0.036(3) Uani 1 1 d . . . H22A H 0.8600 1.4481 0.3368 0.043 Uiso 1 1 calc R . . H22B H 0.9297 1.3794 0.2913 0.043 Uiso 1 1 calc R . . H22C H 1.0287 1.4083 0.3364 0.043 Uiso 1 1 calc R . . C23 C 0.5749(12) 1.3422(10) 0.3482(6) 0.029(3) Uani 1 1 d . . . C24 C 0.5711(15) 1.3918(12) 0.3994(6) 0.037(3) Uani 1 1 d . . . H24A H 0.5652 1.3274 0.4308 0.045 Uiso 1 1 calc R . . H24B H 0.4866 1.4481 0.4000 0.045 Uiso 1 1 calc R . . H24C H 0.6589 1.4322 0.4008 0.045 Uiso 1 1 calc R . . C25 C 0.4312(13) 1.2851(12) 0.3450(7) 0.040(3) Uani 1 1 d . . . H25A H 0.4325 1.2527 0.3118 0.048 Uiso 1 1 calc R . . H25B H 0.3503 1.3450 0.3448 0.048 Uiso 1 1 calc R . . H25C H 0.4201 1.2215 0.3764 0.048 Uiso 1 1 calc R . . C26 C 0.5836(16) 1.4408(12) 0.2979(7) 0.045(4) Uani 1 1 d . . . H26A H 0.5853 1.4064 0.2652 0.054 Uiso 1 1 calc R . . H26B H 0.6717 1.4814 0.2984 0.054 Uiso 1 1 calc R . . H26C H 0.4993 1.4974 0.2979 0.054 Uiso 1 1 calc R . . Zr2 Zr 0.21678(12) 0.28104(10) 0.11398(5) 0.0250(3) Uani 1 1 d . . . P4 P 0.2052(4) 0.5000(3) 0.09563(14) 0.0303(7) Uani 1 1 d . . . P5 P 0.2363(3) 0.5861(3) 0.16501(14) 0.0262(7) Uani 1 1 d . . . P6 P -0.0783(3) 0.2946(3) 0.11615(14) 0.0270(7) Uani 1 1 d . . . C30 C 0.3231(16) 0.1350(13) 0.0568(7) 0.047(4) Uani 1 1 d . . . H30 H 0.3563 0.0580 0.0744 0.056 Uiso 1 1 calc R . . C31 C 0.4041(16) 0.2347(13) 0.0446(6) 0.043(4) Uani 1 1 d . . . H31 H 0.5019 0.2379 0.0529 0.051 Uiso 1 1 calc R . . C32 C 0.3142(15) 0.3279(13) 0.0178(6) 0.042(3) Uani 1 1 d . . . H32 H 0.3412 0.4058 0.0043 0.050 Uiso 1 1 calc R . . C33 C 0.1806(17) 0.2890(13) 0.0141(6) 0.045(4) Uani 1 1 d . . . H33 H 0.0994 0.3349 -0.0021 0.054 Uiso 1 1 calc R . . C34 C 0.1852(16) 0.1703(14) 0.0384(7) 0.046(4) Uani 1 1 d . . . H34 H 0.1069 0.1214 0.0419 0.056 Uiso 1 1 calc R . . C35 C 0.3993(16) 0.1831(13) 0.1810(6) 0.044(4) Uani 1 1 d . . . H35 H 0.4950 0.1671 0.1680 0.053 Uiso 1 1 calc R . . C36 C 0.3456(15) 0.2848(12) 0.1994(5) 0.036(3) Uani 1 1 d . . . H36 H 0.3988 0.3503 0.2015 0.043 Uiso 1 1 calc R . . C37 C 0.2010(16) 0.2740(11) 0.2141(5) 0.036(3) Uani 1 1 d . . . H37 H 0.1376 0.3312 0.2276 0.043 Uiso 1 1 calc R . . C38 C 0.1639(16) 0.1613(12) 0.2054(6) 0.040(3) Uani 1 1 d . . . H38 H 0.0727 0.1291 0.2122 0.048 Uiso 1 1 calc R . . C39 C 0.2875(19) 0.1094(12) 0.1853(6) 0.051(4) Uani 1 1 d . . . H39 H 0.2953 0.0337 0.1756 0.061 Uiso 1 1 calc R . . C40 C -0.1680(12) 0.1679(11) 0.1042(5) 0.030(3) Uani 1 1 d . . . C41 C -0.2040(14) 0.0787(12) 0.1457(6) 0.038(3) Uani 1 1 d . . . H41 H -0.1872 0.0817 0.1823 0.045 Uiso 1 1 calc R . . C42 C -0.2671(14) -0.0174(12) 0.1319(7) 0.044(4) Uani 1 1 d . . . H42 H -0.2921 -0.0797 0.1603 0.052 Uiso 1 1 calc R . . C43 C -0.2948(16) -0.0272(13) 0.0800(7) 0.047(4) Uani 1 1 d . . . H43 H -0.3395 -0.0930 0.0726 0.056 Uiso 1 1 calc R . . C44 C -0.2559(16) 0.0605(13) 0.0402(6) 0.043(4) Uani 1 1 d . . . H44 H -0.2699 0.0555 0.0036 0.052 Uiso 1 1 calc R . . C45 C -0.1964(14) 0.1571(13) 0.0513(6) 0.039(3) Uani 1 1 d . . . H45 H -0.1735 0.2189 0.0222 0.047 Uiso 1 1 calc R . . C46 C -0.1645(13) 0.4149(11) 0.0671(6) 0.033(3) Uani 1 1 d . . . H46A H -0.1249 0.4109 0.0307 0.039 Uiso 1 1 calc R . . H46B H -0.1460 0.4909 0.0761 0.039 Uiso 1 1 calc R . . H46C H -0.2687 0.4072 0.0683 0.039 Uiso 1 1 calc R . . C47 C -0.1683(15) 0.3227(12) 0.1783(6) 0.036(3) Uani 1 1 d . . . H47A H -0.1282 0.3901 0.1891 0.043 Uiso 1 1 calc R . . H47B H -0.1535 0.2528 0.2069 0.043 Uiso 1 1 calc R . . H47C H -0.2717 0.3405 0.1727 0.043 Uiso 1 1 calc R . . C48 C 0.4107(13) 0.6640(12) 0.1422(7) 0.041(4) Uani 1 1 d . . . C49 C 0.4550(15) 0.7269(12) 0.1856(7) 0.041(3) Uani 1 1 d . . . H49A H 0.4636 0.6707 0.2199 0.050 Uiso 1 1 calc R . . H49B H 0.3819 0.7907 0.1899 0.050 Uiso 1 1 calc R . . H49C H 0.5480 0.7600 0.1751 0.050 Uiso 1 1 calc R . . C50 C 0.3955(19) 0.7470(15) 0.0883(7) 0.057(4) Uiso 1 1 d . . . H50A H 0.3670 0.7036 0.0613 0.068 Uiso 1 1 calc R . . H50B H 0.4879 0.7804 0.0769 0.068 Uiso 1 1 calc R . . H50C H 0.3217 0.8108 0.0919 0.068 Uiso 1 1 calc R . . C51 C 0.5275(14) 0.5640(13) 0.1385(8) 0.049(4) Uani 1 1 d . . . H51A H 0.5348 0.5111 0.1738 0.059 Uiso 1 1 calc R . . H51B H 0.6203 0.5975 0.1280 0.059 Uiso 1 1 calc R . . H51C H 0.5020 0.5195 0.1114 0.059 Uiso 1 1 calc R . . C52 C 0.0782(14) 0.7039(11) 0.1592(6) 0.035(3) Uani 1 1 d . . . C53 C 0.0927(17) 0.7887(13) 0.1975(8) 0.052(4) Uani 1 1 d . . . H53A H 0.1167 0.7437 0.2334 0.063 Uiso 1 1 calc R . . H53B H 0.0014 0.8362 0.2001 0.063 Uiso 1 1 calc R . . H53C H 0.1695 0.8408 0.1838 0.063 Uiso 1 1 calc R . . C54 C -0.0511(17) 0.6330(17) 0.1823(10) 0.079(7) Uani 1 1 d . . . H54A H -0.0305 0.5894 0.2187 0.095 Uiso 1 1 calc R . . H54B H -0.0680 0.5773 0.1589 0.095 Uiso 1 1 calc R . . H54C H -0.1372 0.6872 0.1838 0.095 Uiso 1 1 calc R . . C55 C 0.040(2) 0.770(2) 0.1043(7) 0.083(7) Uani 1 1 d . . . H55A H 0.0297 0.7143 0.0803 0.099 Uiso 1 1 calc R . . H55B H 0.1163 0.8221 0.0896 0.099 Uiso 1 1 calc R . . H55C H -0.0513 0.8179 0.1068 0.099 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 Zr1 0.0142(5) 0.0184(5) 0.0298(7) -0.0059(5) -0.0020(4) -0.0005(4) P1 0.0199(14) 0.0172(14) 0.0307(17) -0.0043(12) -0.0021(12) -0.0023(11) P2 0.0214(14) 0.0208(14) 0.0330(18) -0.0069(13) -0.0028(13) -0.0029(11) P3 0.0118(12) 0.0209(14) 0.0317(17) -0.0055(12) -0.0034(11) -0.0027(11) C1 0.023(6) 0.024(6) 0.037(7) 0.001(5) -0.007(5) 0.007(5) C2 0.034(7) 0.018(6) 0.051(9) 0.004(6) -0.008(6) 0.005(5) C3 0.025(6) 0.034(7) 0.055(9) 0.010(6) -0.016(6) -0.008(5) C4 0.032(7) 0.041(8) 0.030(7) 0.006(6) -0.007(6) 0.010(6) C5 0.029(6) 0.028(6) 0.039(8) 0.001(6) -0.018(6) 0.001(5) C6 0.030(7) 0.049(9) 0.045(9) -0.021(7) 0.005(6) 0.008(6) C7 0.035(7) 0.036(7) 0.032(7) -0.011(6) 0.007(6) -0.008(6) C8 0.036(7) 0.038(7) 0.029(7) -0.006(6) 0.006(6) -0.004(6) C9 0.044(8) 0.039(8) 0.039(8) -0.021(6) 0.007(6) -0.009(6) C10 0.049(8) 0.028(7) 0.047(9) -0.021(6) 0.010(7) 0.002(6) C11 0.022(6) 0.024(6) 0.035(7) -0.010(5) 0.001(5) 0.002(5) C12 0.023(6) 0.023(6) 0.039(7) -0.002(5) -0.015(5) 0.007(5) C14 0.025(6) 0.031(7) 0.035(7) -0.002(5) -0.003(5) -0.005(5) C15 0.021(6) 0.026(6) 0.055(9) 0.002(6) 0.002(6) -0.001(5) C16 0.067(11) 0.031(8) 0.086(14) -0.009(9) -0.031(10) -0.011(8) C17 0.032(7) 0.023(7) 0.080(12) -0.013(7) -0.016(7) -0.005(5) C18 0.034(7) 0.027(6) 0.032(7) -0.005(5) -0.005(5) 0.003(5) C20 0.012(5) 0.031(7) 0.064(10) -0.012(6) -0.005(6) -0.005(5) C21 0.034(7) 0.030(7) 0.046(8) -0.017(6) -0.014(6) 0.004(5) C22 0.040(7) 0.023(6) 0.045(8) -0.002(6) -0.001(6) -0.019(5) C23 0.017(5) 0.018(6) 0.051(8) -0.006(5) -0.001(5) -0.003(4) C24 0.035(7) 0.032(7) 0.045(8) -0.012(6) -0.001(6) 0.001(6) C25 0.023(6) 0.030(7) 0.068(10) -0.009(7) -0.009(6) -0.003(5) C26 0.038(8) 0.027(7) 0.069(11) 0.000(7) -0.014(7) 0.000(6) Zr2 0.0261(6) 0.0203(6) 0.0295(7) -0.0074(5) -0.0042(5) 0.0013(4) P4 0.0356(18) 0.0215(15) 0.0360(19) -0.0104(14) -0.0020(14) -0.0024(13) P5 0.0274(16) 0.0198(15) 0.0327(18) -0.0081(13) -0.0008(13) -0.0020(12) P6 0.0252(15) 0.0250(16) 0.0314(18) -0.0073(13) -0.0031(13) -0.0005(12) C30 0.049(9) 0.036(8) 0.060(10) -0.027(7) -0.015(7) 0.015(7) C31 0.041(8) 0.051(9) 0.041(9) -0.026(7) -0.007(6) 0.014(7) C32 0.040(8) 0.041(8) 0.044(9) -0.011(7) 0.012(6) 0.004(6) C33 0.056(9) 0.048(9) 0.034(8) -0.021(7) -0.009(7) 0.023(7) C34 0.038(8) 0.054(9) 0.061(10) -0.044(8) 0.006(7) -0.013(7) C35 0.035(7) 0.045(8) 0.051(10) -0.010(7) -0.012(7) 0.009(6) C36 0.045(8) 0.037(7) 0.029(7) -0.007(6) -0.012(6) -0.011(6) C37 0.056(9) 0.024(6) 0.025(7) -0.001(5) -0.003(6) 0.003(6) C38 0.046(8) 0.033(7) 0.037(8) 0.004(6) -0.010(6) 0.001(6) C39 0.084(12) 0.020(7) 0.047(10) 0.001(6) -0.027(9) 0.005(7) C40 0.020(6) 0.035(7) 0.040(8) -0.015(6) -0.009(5) 0.001(5) C41 0.028(7) 0.031(7) 0.054(9) -0.009(6) -0.016(6) 0.004(5) C42 0.026(7) 0.029(7) 0.074(11) 0.004(7) -0.009(7) -0.019(6) C43 0.041(8) 0.039(8) 0.069(11) -0.030(8) -0.021(8) 0.002(6) C44 0.047(8) 0.041(8) 0.047(9) -0.021(7) -0.021(7) 0.011(7) C45 0.031(7) 0.040(8) 0.046(9) -0.010(6) -0.017(6) 0.015(6) C46 0.026(6) 0.025(6) 0.048(8) -0.011(6) -0.002(6) 0.008(5) C47 0.042(8) 0.031(7) 0.037(8) -0.013(6) 0.001(6) 0.000(6) C48 0.017(6) 0.039(8) 0.073(11) -0.022(7) 0.004(6) -0.019(5) C49 0.032(7) 0.029(7) 0.068(10) -0.017(7) -0.001(7) -0.014(6) C51 0.022(6) 0.048(9) 0.088(13) -0.035(9) 0.000(7) -0.004(6) C52 0.035(7) 0.030(7) 0.044(8) -0.018(6) 0.000(6) 0.002(5) C53 0.043(8) 0.039(8) 0.082(13) -0.029(8) -0.019(8) 0.010(7) C54 0.034(8) 0.065(12) 0.15(2) -0.060(13) 0.032(11) -0.002(8) C55 0.065(12) 0.119(18) 0.046(11) 0.005(11) -0.003(9) 0.056(12) _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 Zr1 P1 2.488(3) . ? Zr1 C10 2.491(13) . ? Zr1 C6 2.502(13) . ? Zr1 C7 2.503(13) . ? Zr1 C8 2.512(13) . ? Zr1 C9 2.514(14) . ? Zr1 C5 2.524(12) . ? Zr1 C1 2.524(11) . ? Zr1 C2 2.532(12) . ? Zr1 C4 2.536(13) . ? Zr1 C3 2.548(13) . ? Zr1 P3 2.734(3) . ? P1 P2 2.200(5) . ? P2 C23 1.909(12) . ? P2 C19 1.949(13) . ? P3 C11 1.822(12) . ? P3 C13 1.836(12) . ? P3 C12 1.836(12) . ? C1 C5 1.386(18) . ? C1 C2 1.419(18) . ? C1 H1 0.9500 . ? C2 C3 1.405(19) . ? C2 H2 0.9500 . ? C3 C4 1.39(2) . ? C3 H3 0.9500 . ? C4 C5 1.418(18) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.413(19) . ? C6 C10 1.42(2) . ? C6 H6 0.9500 . ? C7 C8 1.413(19) . ? C7 H7 0.9500 . ? C8 C9 1.438(19) . ? C8 H8 0.9500 . ? C9 C10 1.39(2) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.380(18) . ? C13 C18 1.418(17) . ? C14 C15 1.375(17) . ? C14 H14 0.9500 . ? C15 C16 1.42(2) . ? C15 H15 0.9500 . ? C16 C17 1.33(2) . ? C16 H16 0.9500 . ? C17 C18 1.367(18) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C21 1.486(18) . ? C19 C20 1.503(17) . ? C19 C22 1.521(17) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.511(19) . ? C23 C26 1.538(19) . ? C23 C25 1.553(16) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? Zr2 C39 2.478(14) . ? Zr2 P4 2.482(3) . ? Zr2 C38 2.500(14) . ? Zr2 C35 2.504(14) . ? Zr2 C31 2.509(14) . ? Zr2 C37 2.508(13) . ? Zr2 C32 2.521(14) . ? Zr2 C36 2.528(12) . ? Zr2 C34 2.533(13) . ? Zr2 C30 2.536(14) . ? Zr2 C33 2.541(14) . ? Zr2 P6 2.738(3) . ? P4 P5 2.215(5) . ? P5 C52 1.913(13) . ? P5 C48 1.931(12) . ? P6 C47 1.813(13) . ? P6 C40 1.827(13) . ? P6 C46 1.835(13) . ? C30 C34 1.39(2) . ? C30 C31 1.41(2) . ? C30 H30 0.9500 . ? C31 C32 1.40(2) . ? C31 H31 0.9500 . ? C32 C33 1.37(2) . ? C32 H32 0.9500 . ? C33 C34 1.39(2) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C39 1.39(2) . ? C35 C36 1.39(2) . ? C35 H35 0.9500 . ? C36 C37 1.39(2) . ? C36 H36 0.9500 . ? C37 C38 1.436(19) . ? C37 H37 0.9500 . ? C38 C39 1.37(2) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.37(2) . ? C40 C45 1.404(19) . ? C41 C42 1.408(18) . ? C41 H41 0.9500 . ? C42 C43 1.37(2) . ? C42 H42 0.9500 . ? C43 C44 1.34(2) . ? C43 H43 0.9500 . ? C44 C45 1.37(2) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C50 1.51(2) . ? C48 C49 1.519(19) . ? C48 C51 1.534(19) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C55 1.49(2) . ? C52 C53 1.521(19) . ? C52 C54 1.54(2) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Zr1 C10 141.7(4) . . ? P1 Zr1 C6 115.4(4) . . ? C10 Zr1 C6 33.0(5) . . ? P1 Zr1 C7 87.7(3) . . ? C10 Zr1 C7 54.5(5) . . ? C6 Zr1 C7 32.8(5) . . ? P1 Zr1 C8 91.1(3) . . ? C10 Zr1 C8 54.6(5) . . ? C6 Zr1 C8 54.5(5) . . ? C7 Zr1 C8 32.7(4) . . ? P1 Zr1 C9 122.6(3) . . ? C10 Zr1 C9 32.3(5) . . ? C6 Zr1 C9 54.2(5) . . ? C7 Zr1 C9 54.4(4) . . ? C8 Zr1 C9 33.3(4) . . ? P1 Zr1 C5 77.9(3) . . ? C10 Zr1 C5 126.0(5) . . ? C6 Zr1 C5 111.4(5) . . ? C7 Zr1 C5 124.7(4) . . ? C8 Zr1 C5 156.3(4) . . ? C9 Zr1 C5 157.7(4) . . ? P1 Zr1 C1 103.8(3) . . ? C10 Zr1 C1 94.2(5) . . ? C6 Zr1 C1 83.6(5) . . ? C7 Zr1 C1 107.5(4) . . ? C8 Zr1 C1 137.7(4) . . ? C9 Zr1 C1 126.3(4) . . ? C5 Zr1 C1 31.9(4) . . ? P1 Zr1 C2 131.3(3) . . ? C10 Zr1 C2 79.4(5) . . ? C6 Zr1 C2 86.7(5) . . ? C7 Zr1 C2 119.0(5) . . ? C8 Zr1 C2 133.9(5) . . ? C9 Zr1 C2 105.8(5) . . ? C5 Zr1 C2 53.4(4) . . ? C1 Zr1 C2 32.6(4) . . ? P1 Zr1 C4 86.3(3) . . ? C10 Zr1 C4 130.6(5) . . ? C6 Zr1 C4 135.8(5) . . ? C7 Zr1 C4 157.2(4) . . ? C8 Zr1 C4 169.1(4) . . ? C9 Zr1 C4 144.5(5) . . ? C5 Zr1 C4 32.5(4) . . ? C1 Zr1 C4 53.1(4) . . ? C2 Zr1 C4 52.8(5) . . ? P1 Zr1 C3 117.6(4) . . ? C10 Zr1 C3 100.3(5) . . ? C6 Zr1 C3 117.2(5) . . ? C7 Zr1 C3 150.0(5) . . ? C8 Zr1 C3 147.5(5) . . ? C9 Zr1 C3 114.5(5) . . ? C5 Zr1 C3 53.4(4) . . ? C1 Zr1 C3 53.5(4) . . ? C2 Zr1 C3 32.1(4) . . ? C4 Zr1 C3 31.7(5) . . ? P1 Zr1 P3 88.49(10) . . ? C10 Zr1 P3 103.7(4) . . ? C6 Zr1 P3 131.9(3) . . ? C7 Zr1 P3 118.4(3) . . ? C8 Zr1 P3 86.0(3) . . ? C9 Zr1 P3 77.7(3) . . ? C5 Zr1 P3 114.3(3) . . ? C1 Zr1 P3 132.9(3) . . ? C2 Zr1 P3 108.8(3) . . ? C4 Zr1 P3 83.4(3) . . ? C3 Zr1 P3 80.4(3) . . ? P2 P1 Zr1 115.53(16) . . ? C23 P2 C19 108.3(5) . . ? C23 P2 P1 104.1(4) . . ? C19 P2 P1 100.5(4) . . ? C11 P3 C13 101.5(6) . . ? C11 P3 C12 100.8(6) . . ? C13 P3 C12 102.5(6) . . ? C11 P3 Zr1 115.7(4) . . ? C13 P3 Zr1 118.0(4) . . ? C12 P3 Zr1 115.8(4) . . ? C5 C1 C2 108.2(11) . . ? C5 C1 Zr1 74.1(7) . . ? C2 C1 Zr1 74.0(7) . . ? C5 C1 H1 125.9 . . ? C2 C1 H1 125.9 . . ? Zr1 C1 H1 117.9 . . ? C3 C2 C1 107.8(12) . . ? C3 C2 Zr1 74.5(7) . . ? C1 C2 Zr1 73.4(7) . . ? C3 C2 H2 126.1 . . ? C1 C2 H2 126.1 . . ? Zr1 C2 H2 118.0 . . ? C4 C3 C2 107.8(12) . . ? C4 C3 Zr1 73.7(8) . . ? C2 C3 Zr1 73.3(8) . . ? C4 C3 H3 126.1 . . ? C2 C3 H3 126.1 . . ? Zr1 C3 H3 118.8 . . ? C3 C4 C5 108.7(12) . . ? C3 C4 Zr1 74.6(8) . . ? C5 C4 Zr1 73.2(8) . . ? C3 C4 H4 125.6 . . ? C5 C4 H4 125.6 . . ? Zr1 C4 H4 118.4 . . ? C1 C5 C4 107.6(12) . . ? C1 C5 Zr1 74.1(7) . . ? C4 C5 Zr1 74.2(7) . . ? C1 C5 H5 126.2 . . ? C4 C5 H5 126.2 . . ? Zr1 C5 H5 117.5 . . ? C7 C6 C10 107.7(12) . . ? C7 C6 Zr1 73.6(7) . . ? C10 C6 Zr1 73.1(8) . . ? C7 C6 H6 126.2 . . ? C10 C6 H6 126.2 . . ? Zr1 C6 H6 119.0 . . ? C6 C7 C8 108.6(12) . . ? C6 C7 Zr1 73.6(8) . . ? C8 C7 Zr1 74.0(7) . . ? C6 C7 H7 125.7 . . ? C8 C7 H7 125.7 . . ? Zr1 C7 H7 118.6 . . ? C7 C8 C9 107.0(12) . . ? C7 C8 Zr1 73.3(8) . . ? C9 C8 Zr1 73.4(8) . . ? C7 C8 H8 126.5 . . ? C9 C8 H8 126.5 . . ? Zr1 C8 H8 118.8 . . ? C10 C9 C8 108.2(12) . . ? C10 C9 Zr1 72.9(8) . . ? C8 C9 Zr1 73.3(8) . . ? C10 C9 H9 125.9 . . ? C8 C9 H9 125.9 . . ? Zr1 C9 H9 119.7 . . ? C9 C10 C6 108.6(12) . . ? C9 C10 Zr1 74.7(7) . . ? C6 C10 Zr1 73.9(8) . . ? C9 C10 H10 125.7 . . ? C6 C10 H10 125.7 . . ? Zr1 C10 H10 117.6 . . ? P3 C11 H11A 109.5 . . ? P3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P3 C12 H12A 109.5 . . ? P3 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P3 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 118.6(11) . . ? C14 C13 P3 120.4(9) . . ? C18 C13 P3 121.0(9) . . ? C15 C14 C13 120.9(13) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 118.1(14) . . ? C14 C15 H15 121.0 . . ? C16 C15 H15 121.0 . . ? C17 C16 C15 121.8(14) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C16 C17 C18 120.2(15) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C13 120.2(13) . . ? C17 C18 H18 119.9 . . ? C13 C18 H18 119.9 . . ? C21 C19 C20 108.7(11) . . ? C21 C19 C22 111.0(11) . . ? C20 C19 C22 108.4(11) . . ? C21 C19 P2 117.1(9) . . ? C20 C19 P2 104.5(8) . . ? C22 C19 P2 106.6(9) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C26 111.1(11) . . ? C24 C23 C25 108.8(11) . . ? C26 C23 C25 106.2(11) . . ? C24 C23 P2 116.2(9) . . ? C26 C23 P2 108.2(9) . . ? C25 C23 P2 105.8(8) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C39 Zr2 P4 140.6(4) . . ? C39 Zr2 C38 32.0(5) . . ? P4 Zr2 C38 122.9(3) . . ? C39 Zr2 C35 32.3(5) . . ? P4 Zr2 C35 114.7(4) . . ? C38 Zr2 C35 53.9(5) . . ? C39 Zr2 C31 96.1(6) . . ? P4 Zr2 C31 101.2(4) . . ? C38 Zr2 C31 127.9(5) . . ? C35 Zr2 C31 84.7(5) . . ? C39 Zr2 C37 53.5(5) . . ? P4 Zr2 C37 91.5(3) . . ? C38 Zr2 C37 33.3(4) . . ? C35 Zr2 C37 53.4(5) . . ? C31 Zr2 C37 137.5(5) . . ? C39 Zr2 C32 128.0(5) . . ? P4 Zr2 C32 77.6(3) . . ? C38 Zr2 C32 158.5(5) . . ? C35 Zr2 C32 114.4(5) . . ? C31 Zr2 C32 32.2(5) . . ? C37 Zr2 C32 158.5(5) . . ? C39 Zr2 C36 53.2(5) . . ? P4 Zr2 C36 87.8(3) . . ? C38 Zr2 C36 54.1(5) . . ? C35 Zr2 C36 32.2(5) . . ? C31 Zr2 C36 107.5(5) . . ? C37 Zr2 C36 32.0(5) . . ? C32 Zr2 C36 127.8(5) . . ? C39 Zr2 C34 98.2(5) . . ? P4 Zr2 C34 120.4(4) . . ? C38 Zr2 C34 112.6(5) . . ? C35 Zr2 C34 114.3(5) . . ? C31 Zr2 C34 53.0(5) . . ? C37 Zr2 C34 145.9(5) . . ? C32 Zr2 C34 52.4(5) . . ? C36 Zr2 C34 146.5(5) . . ? C39 Zr2 C30 79.3(5) . . ? P4 Zr2 C30 130.3(4) . . ? C38 Zr2 C30 105.8(5) . . ? C35 Zr2 C30 85.0(5) . . ? C31 Zr2 C30 32.4(5) . . ? C37 Zr2 C30 132.5(5) . . ? C32 Zr2 C30 53.0(5) . . ? C36 Zr2 C30 116.4(5) . . ? C34 Zr2 C30 31.8(5) . . ? C39 Zr2 C33 129.4(5) . . ? P4 Zr2 C33 88.6(4) . . ? C38 Zr2 C33 141.9(5) . . ? C35 Zr2 C33 135.8(5) . . ? C31 Zr2 C33 53.0(5) . . ? C37 Zr2 C33 169.0(5) . . ? C32 Zr2 C33 31.4(5) . . ? C36 Zr2 C33 158.9(5) . . ? C34 Zr2 C33 31.8(5) . . ? C30 Zr2 C33 52.9(5) . . ? C39 Zr2 P6 105.2(4) . . ? P4 Zr2 P6 88.58(11) . . ? C38 Zr2 P6 79.0(3) . . ? C35 Zr2 P6 132.9(4) . . ? C31 Zr2 P6 132.5(3) . . ? C37 Zr2 P6 87.7(3) . . ? C32 Zr2 P6 110.2(3) . . ? C36 Zr2 P6 119.4(3) . . ? C34 Zr2 P6 81.9(3) . . ? C30 Zr2 P6 111.3(4) . . ? C33 Zr2 P6 81.3(4) . . ? P5 P4 Zr2 116.87(17) . . ? C52 P5 C48 108.1(6) . . ? C52 P5 P4 102.1(4) . . ? C48 P5 P4 101.4(5) . . ? C47 P6 C40 102.0(6) . . ? C47 P6 C46 100.4(6) . . ? C40 P6 C46 101.4(6) . . ? C47 P6 Zr2 116.1(5) . . ? C40 P6 Zr2 118.5(4) . . ? C46 P6 Zr2 115.7(4) . . ? C34 C30 C31 107.1(14) . . ? C34 C30 Zr2 74.0(8) . . ? C31 C30 Zr2 72.8(8) . . ? C34 C30 H30 126.4 . . ? C31 C30 H30 126.4 . . ? Zr2 C30 H30 118.8 . . ? C32 C31 C30 107.2(13) . . ? C32 C31 Zr2 74.4(8) . . ? C30 C31 Zr2 74.8(9) . . ? C32 C31 H31 126.4 . . ? C30 C31 H31 126.4 . . ? Zr2 C31 H31 116.6 . . ? C33 C32 C31 109.0(14) . . ? C33 C32 Zr2 75.1(9) . . ? C31 C32 Zr2 73.4(9) . . ? C33 C32 H32 125.5 . . ? C31 C32 H32 125.5 . . ? Zr2 C32 H32 117.9 . . ? C32 C33 C34 107.7(13) . . ? C32 C33 Zr2 73.5(9) . . ? C34 C33 Zr2 73.8(8) . . ? C32 C33 H33 126.1 . . ? C34 C33 H33 126.1 . . ? Zr2 C33 H33 118.5 . . ? C30 C34 C33 108.9(14) . . ? C30 C34 Zr2 74.2(8) . . ? C33 C34 Zr2 74.4(8) . . ? C30 C34 H34 125.6 . . ? C33 C34 H34 125.6 . . ? Zr2 C34 H34 117.7 . . ? C39 C35 C36 107.4(13) . . ? C39 C35 Zr2 72.8(8) . . ? C36 C35 Zr2 74.9(8) . . ? C39 C35 H35 126.3 . . ? C36 C35 H35 126.3 . . ? Zr2 C35 H35 118.0 . . ? C37 C36 C35 108.2(12) . . ? C37 C36 Zr2 73.2(7) . . ? C35 C36 Zr2 73.0(8) . . ? C37 C36 H36 125.9 . . ? C35 C36 H36 125.9 . . ? Zr2 C36 H36 119.7 . . ? C36 C37 C38 108.0(12) . . ? C36 C37 Zr2 74.8(8) . . ? C38 C37 Zr2 73.0(8) . . ? C36 C37 H37 126.0 . . ? C38 C37 H37 126.0 . . ? Zr2 C37 H37 118.2 . . ? C39 C38 C37 105.9(13) . . ? C39 C38 Zr2 73.1(9) . . ? C37 C38 Zr2 73.7(8) . . ? C39 C38 H38 127.1 . . ? C37 C38 H38 127.1 . . ? Zr2 C38 H38 118.3 . . ? C38 C39 C35 110.5(13) . . ? C38 C39 Zr2 74.8(8) . . ? C35 C39 Zr2 74.8(8) . . ? C38 C39 H39 124.8 . . ? C35 C39 H39 124.8 . . ? Zr2 C39 H39 117.3 . . ? C41 C40 C45 118.0(12) . . ? C41 C40 P6 121.7(10) . . ? C45 C40 P6 120.2(11) . . ? C40 C41 C42 117.1(14) . . ? C40 C41 H41 121.4 . . ? C42 C41 H41 121.4 . . ? C43 C42 C41 124.5(14) . . ? C43 C42 H42 117.7 . . ? C41 C42 H42 117.7 . . ? C44 C43 C42 116.9(13) . . ? C44 C43 H43 121.5 . . ? C42 C43 H43 121.5 . . ? C43 C44 C45 121.1(14) . . ? C43 C44 H44 119.4 . . ? C45 C44 H44 119.4 . . ? C44 C45 C40 122.3(14) . . ? C44 C45 H45 118.9 . . ? C40 C45 H45 118.9 . . ? P6 C46 H46A 109.5 . . ? P6 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? P6 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? P6 C47 H47A 109.5 . . ? P6 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? P6 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C50 C48 C49 111.6(12) . . ? C50 C48 C51 111.0(14) . . ? C49 C48 C51 106.7(12) . . ? C50 C48 P5 111.9(10) . . ? C49 C48 P5 110.1(10) . . ? C51 C48 P5 105.2(9) . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C48 C51 H51A 109.5 . . ? C48 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C48 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C55 C52 C53 110.6(14) . . ? C55 C52 C54 107.2(16) . . ? C53 C52 C54 105.1(13) . . ? C55 C52 P5 118.4(10) . . ? C53 C52 P5 111.1(10) . . ? C54 C52 P5 103.2(10) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C52 C55 H55A 109.5 . . ? C52 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C52 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.032 _refine_diff_density_min -1.693 _refine_diff_density_rms 0.241