# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1257 data_rac1b ############################################################################ # # _publ_requested_journal 'Chemical Communications' _publ_section_title ; Donor complexes of bis(1-indenyl)phenylborane dichlorozirconium as isospecific catalysts in propene polymerization ; loop_ _publ_author_name _publ_author_address 'Manfred T. Reetz' ; Max-Planck-Institut f\"ur Kohlenforschung Kaiser-Wilhelm-Platz 1 D-45470 M\"ulheim an der Ruhr Germany ; 'Marc Willuhn' ; Max-Planck-Institut f\"ur Kohlenforschung Kaiser-Wilhelm-Platz 1 D-45470 M\"ulheim an der Ruhr Germany ; 'Christian Psiorz' ; Max-Planck-Institut f\"ur Kohlenforschung Kaiser-Wilhelm-Platz 1 D-45470 M\"ulheim an der Ruhr Germany ; 'Richard Goddard' ; Max-Planck-Institut f\"ur Kohlenforschung Kaiser-Wilhelm-Platz 1 D-45470 M\"ulheim an der Ruhr Germany ; # # ############################################################################ _chemical_name_systematic ; bis(1-indenyl)tetrahydrofuranphenylborane dichloroborane ; _chemical_compound_source 'see paper' _chemical_formula_sum 'C28 H25 B Cl2 O Zr' _chemical_formula_weight 550.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7457(6) _cell_length_b 15.510(3) _cell_length_c 16.308(3) _cell_angle_alpha 62.146(14) _cell_angle_beta 82.919(12) _cell_angle_gamma 83.254(10) _cell_volume 2379.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.2 _cell_measurement_theta_max 24.7 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method none _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.707 _exptl_absorpt_correction_type none _publ_section_exptl_prep ; The crystal was mounted in a Lindemann glass capillary under argon. ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w-2\q scan' _diffrn_standards_number 3 _diffrn_standards_interval_time 30 _diffrn_standards_decay_% 24.24 _diffrn_reflns_number 11215 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 27.44 _reflns_number_total 10815 _reflns_number_gt 8006 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'EXPRESS / CAD4 software (Enraf-Nonius, 1995)' _computing_cell_refinement 'EXPRESS / CAD4 software (Enraf-Nonius, 1995)' _computing_data_reduction 'DATAP (Coppens,Leiserowitz & Rabinovich, 1965)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1976)' _publ_section_exptl_refinement ; 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^)+(0.0356P)^2^+2.1332P] 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_number_reflns 10815 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.1050 _refine_ls_wR_factor_gt 0.0931 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 C1 C 0.8883(3) 0.2821(2) 1.0996(2) 0.0390(6) Uani 1 1 d . . . C2 C 0.9157(3) 0.3422(2) 1.0014(2) 0.0373(6) Uani 1 1 d . . . C3 C 0.8278(3) 0.4253(2) 0.9773(2) 0.0427(7) Uani 1 1 d . . . H3 H 0.8321 0.4847 0.9175 0.051 Uiso 1 1 calc R . . C4 C 0.7487(3) 0.4173(2) 1.0557(2) 0.0469(7) Uani 1 1 d . . . H4 H 0.6873 0.4682 1.0580 0.056 Uiso 1 1 calc R . . C5 C 0.7859(3) 0.3295(2) 1.1331(2) 0.0451(7) Uani 1 1 d . . . C6 C 0.7441(3) 0.2851(3) 1.2293(3) 0.0559(9) Uani 1 1 d . . . H6 H 0.6784 0.3151 1.2516 0.067 Uiso 1 1 calc R . . C7 C 0.8003(4) 0.1996(3) 1.2877(3) 0.0639(10) Uani 1 1 d . . . H7 H 0.7736 0.1712 1.3506 0.077 Uiso 1 1 calc R . . C8 C 0.8996(4) 0.1518(3) 1.2554(2) 0.0567(9) Uani 1 1 d . . . H8 H 0.9363 0.0925 1.2976 0.068 Uiso 1 1 calc R . . C9 C 0.9423(3) 0.1903(2) 1.1645(2) 0.0466(7) Uani 1 1 d . . . H9 H 1.0066 0.1571 1.1446 0.056 Uiso 1 1 calc R . . C10 C 0.7722(3) 0.3222(2) 0.8452(2) 0.0375(6) Uani 1 1 d . . . C11 C 0.8717(3) 0.2662(2) 0.9037(2) 0.0362(6) Uani 1 1 d . . . C12 C 0.8244(3) 0.1726(2) 0.9612(2) 0.0415(7) Uani 1 1 d . . . H12 H 0.8754 0.1148 1.0017 0.050 Uiso 1 1 calc R . . C13 C 0.7013(3) 0.1702(2) 0.9419(2) 0.0439(7) Uani 1 1 d . . . H13 H 0.6524 0.1123 0.9687 0.053 Uiso 1 1 calc R . . C14 C 0.6686(3) 0.2613(2) 0.8673(2) 0.0410(7) Uani 1 1 d . . . C15 C 0.5601(3) 0.2984(3) 0.8157(2) 0.0492(8) Uani 1 1 d . . . H15 H 0.4929 0.2598 0.8296 0.059 Uiso 1 1 calc R . . C16 C 0.5568(3) 0.3903(3) 0.7464(2) 0.0536(8) Uani 1 1 d . . . H16 H 0.4874 0.4145 0.7112 0.064 Uiso 1 1 calc R . . C17 C 0.6562(3) 0.4512(3) 0.7256(2) 0.0530(8) Uani 1 1 d . . . H17 H 0.6495 0.5147 0.6777 0.064 Uiso 1 1 calc R . . C18 C 0.7606(3) 0.4203(2) 0.7729(2) 0.0452(7) Uani 1 1 d . . . H18 H 0.8240 0.4623 0.7585 0.054 Uiso 1 1 calc R . . C19 C 1.1090(3) 0.2302(2) 0.9607(2) 0.0396(6) Uani 1 1 d . . . C20 C 1.1989(3) 0.2385(3) 1.0110(2) 0.0473(7) Uani 1 1 d . . . H20 H 1.1839 0.2852 1.0323 0.057 Uiso 1 1 calc R . . C21 C 1.3097(3) 0.1796(3) 1.0302(3) 0.0588(9) Uani 1 1 d . . . H21 H 1.3685 0.1878 1.0629 0.071 Uiso 1 1 calc R . . C22 C 1.3324(3) 0.1088(3) 1.0006(3) 0.0623(10) Uani 1 1 d . . . H22 H 1.4063 0.0686 1.0139 0.075 Uiso 1 1 calc R . . C23 C 1.2452(3) 0.0977(3) 0.9512(3) 0.0575(9) Uani 1 1 d . . . H23 H 1.2603 0.0503 0.9308 0.069 Uiso 1 1 calc R . . C24 C 1.1352(3) 0.1574(2) 0.9320(2) 0.0468(7) Uani 1 1 d . . . H24 H 1.0770 0.1490 0.8991 0.056 Uiso 1 1 calc R . . C25 C 1.1097(3) 0.4673(2) 0.8450(2) 0.0482(8) Uani 1 1 d . . . H25A H 1.1249 0.4442 0.9096 0.058 Uiso 1 1 calc R . . H25B H 1.0703 0.5331 0.8213 0.058 Uiso 1 1 calc R . . C26 C 1.2309(4) 0.4660(3) 0.7887(3) 0.0677(11) Uani 1 1 d . . . H26A H 1.3012 0.4449 0.8274 0.081 Uiso 1 1 calc R . . H26B H 1.2444 0.5307 0.7380 0.081 Uiso 1 1 calc R . . C27 C 1.2191(3) 0.3947(3) 0.7512(3) 0.0559(9) Uani 1 1 d . . . H27A H 1.2566 0.4186 0.6878 0.067 Uiso 1 1 calc R . . H27B H 1.2592 0.3311 0.7896 0.067 Uiso 1 1 calc R . . C28 C 1.0795(3) 0.3893(3) 0.7549(2) 0.0487(8) Uani 1 1 d . . . H28A H 1.0452 0.4408 0.6988 0.058 Uiso 1 1 calc R . . H28B H 1.0602 0.3266 0.7618 0.058 Uiso 1 1 calc R . . C29 C 0.3461(3) 0.2081(2) 0.4013(2) 0.0432(7) Uani 1 1 d . . . C30 C 0.3603(3) 0.1541(2) 0.4997(2) 0.0410(7) Uani 1 1 d . . . C31 C 0.2874(3) 0.0712(2) 0.5311(3) 0.0488(8) Uani 1 1 d . . . H31 H 0.2900 0.0144 0.5928 0.059 Uiso 1 1 calc R . . C32 C 0.2292(3) 0.0748(3) 0.4568(3) 0.0553(9) Uani 1 1 d . . . H32 H 0.1816 0.0233 0.4596 0.066 Uiso 1 1 calc R . . C33 C 0.2653(3) 0.1592(3) 0.3749(3) 0.0524(8) Uani 1 1 d . . . C34 C 0.2390(4) 0.1990(4) 0.2796(3) 0.0683(12) Uani 1 1 d . . . H34 H 0.1859 0.1684 0.2620 0.082 Uiso 1 1 calc R . . C35 C 0.2919(4) 0.2816(4) 0.2153(3) 0.0749(12) Uani 1 1 d . . . H35 H 0.2759 0.3068 0.1532 0.090 Uiso 1 1 calc R . . C36 C 0.3703(4) 0.3298(3) 0.2405(3) 0.0666(10) Uani 1 1 d . . . H36 H 0.4054 0.3863 0.1947 0.080 Uiso 1 1 calc R . . C37 C 0.3965(3) 0.2959(3) 0.3303(2) 0.0507(8) Uani 1 1 d . . . H37 H 0.4473 0.3301 0.3455 0.061 Uiso 1 1 calc R . . C38 C 0.1620(3) 0.1904(2) 0.6536(2) 0.0428(7) Uani 1 1 d . . . C39 C 0.2663(3) 0.2407(2) 0.5915(2) 0.0406(7) Uani 1 1 d . . . C40 C 0.2131(3) 0.3346(2) 0.5304(2) 0.0465(7) Uani 1 1 d . . . H40 H 0.2624 0.3894 0.4863 0.056 Uiso 1 1 calc R . . C41 C 0.0824(3) 0.3425(3) 0.5522(3) 0.0524(8) Uani 1 1 d . . . H41 H 0.0265 0.4017 0.5234 0.063 Uiso 1 1 calc R . . C42 C 0.0499(3) 0.2554(3) 0.6298(2) 0.0459(7) Uani 1 1 d . . . C43 C -0.0659(3) 0.2253(3) 0.6851(3) 0.0599(10) Uani 1 1 d . . . H43 H -0.1383 0.2671 0.6711 0.072 Uiso 1 1 calc R . . C44 C -0.0680(3) 0.1348(3) 0.7582(3) 0.0635(11) Uani 1 1 d . . . H44 H -0.1423 0.1152 0.7956 0.076 Uiso 1 1 calc R . . C45 C 0.0396(4) 0.0698(3) 0.7790(3) 0.0583(9) Uani 1 1 d . . . H45 H 0.0335 0.0076 0.8289 0.070 Uiso 1 1 calc R . . C46 C 0.1527(3) 0.0941(3) 0.7290(2) 0.0492(8) Uani 1 1 d . . . H46 H 0.2221 0.0492 0.7436 0.059 Uiso 1 1 calc R . . C47 C 0.5127(3) 0.2681(2) 0.5264(2) 0.0420(7) Uani 1 1 d . . . C48 C 0.6191(3) 0.2521(3) 0.4752(2) 0.0468(7) Uani 1 1 d . . . H48 H 0.6197 0.2032 0.4574 0.056 Uiso 1 1 calc R . . C49 C 0.7232(3) 0.3059(3) 0.4502(2) 0.0564(9) Uani 1 1 d . . . H49 H 0.7926 0.2926 0.4168 0.068 Uiso 1 1 calc R . . C50 C 0.7238(3) 0.3795(3) 0.4750(3) 0.0609(10) Uani 1 1 d . . . H50 H 0.7940 0.4156 0.4590 0.073 Uiso 1 1 calc R . . C51 C 0.6207(4) 0.3992(3) 0.5230(3) 0.0620(10) Uani 1 1 d . . . H51 H 0.6201 0.4498 0.5387 0.074 Uiso 1 1 calc R . . C52 C 0.5166(3) 0.3439(3) 0.5486(2) 0.0513(8) Uani 1 1 d . . . H52 H 0.4474 0.3581 0.5817 0.062 Uiso 1 1 calc R . . C53 C 0.5460(3) 0.0333(3) 0.6534(3) 0.0535(8) Uani 1 1 d . . . H53A H 0.5805 0.0561 0.5894 0.064 Uiso 1 1 calc R . . H53B H 0.5160 -0.0311 0.6754 0.064 Uiso 1 1 calc R . . C54 C 0.6434(4) 0.0297(4) 0.7132(3) 0.0758(12) Uani 1 1 d . . . H54A H 0.6543 -0.0355 0.7643 0.091 Uiso 1 1 calc R . . H54B H 0.7234 0.0473 0.6771 0.091 Uiso 1 1 calc R . . C55 C 0.5977(5) 0.1005(4) 0.7486(4) 0.0949(17) Uani 1 1 d . . . H55A H 0.6136 0.0735 0.8136 0.114 Uiso 1 1 calc R . . H55B H 0.6407 0.1604 0.7136 0.114 Uiso 1 1 calc R . . C56 C 0.4636(3) 0.1203(3) 0.7380(2) 0.0588(9) Uani 1 1 d . . . H56A H 0.4381 0.1875 0.7242 0.071 Uiso 1 1 calc R . . H56B H 0.4163 0.0773 0.7945 0.071 Uiso 1 1 calc R . . B1 B 0.9866(3) 0.3043(2) 0.9297(2) 0.0358(7) Uani 1 1 d . . . B2 B 0.4002(3) 0.1963(3) 0.5651(2) 0.0395(7) Uani 1 1 d . . . Cl1 Cl 0.51282(8) 0.38849(7) 0.96619(7) 0.0586(2) Uani 1 1 d . . . Cl2 Cl 0.62591(9) 0.14904(7) 1.14917(6) 0.0616(2) Uani 1 1 d . . . Cl3 Cl -0.03975(8) 0.11371(7) 0.55018(7) 0.0566(2) Uani 1 1 d . . . Cl4 Cl 0.05970(8) 0.34607(7) 0.35205(7) 0.0589(2) Uani 1 1 d . . . O1 O 1.02849(18) 0.40196(15) 0.83658(14) 0.0398(5) Uani 1 1 d . . . O2 O 0.44234(19) 0.10217(17) 0.66013(15) 0.0453(5) Uani 1 1 d . . . Zr1 Zr 0.70669(2) 0.28797(2) 1.01074(2) 0.03569(8) Uani 1 1 d . . . Zr2 Zr 0.13902(3) 0.21330(2) 0.49312(2) 0.03955(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0349(14) 0.0455(16) 0.0447(16) -0.0274(14) -0.0015(12) -0.0051(12) C2 0.0346(14) 0.0376(15) 0.0464(16) -0.0241(13) -0.0047(12) -0.0046(12) C3 0.0412(16) 0.0389(16) 0.0559(19) -0.0279(15) -0.0041(14) -0.0042(13) C4 0.0419(17) 0.0491(18) 0.064(2) -0.0385(17) -0.0037(15) -0.0007(14) C5 0.0399(16) 0.0551(19) 0.0527(19) -0.0358(17) 0.0016(14) -0.0057(14) C6 0.051(2) 0.075(3) 0.059(2) -0.047(2) 0.0108(16) -0.0110(18) C7 0.068(2) 0.079(3) 0.050(2) -0.035(2) 0.0097(18) -0.017(2) C8 0.058(2) 0.062(2) 0.0456(19) -0.0204(17) -0.0042(16) -0.0090(17) C9 0.0423(17) 0.0496(18) 0.0498(18) -0.0241(16) -0.0040(14) -0.0038(14) C10 0.0355(14) 0.0424(16) 0.0420(16) -0.0251(14) -0.0048(12) -0.0029(12) C11 0.0332(14) 0.0396(15) 0.0427(16) -0.0247(13) -0.0025(12) -0.0023(11) C12 0.0388(15) 0.0376(16) 0.0520(18) -0.0241(14) -0.0028(13) -0.0019(12) C13 0.0421(16) 0.0393(16) 0.0564(19) -0.0261(15) -0.0025(14) -0.0086(13) C14 0.0354(15) 0.0473(17) 0.0502(18) -0.0301(15) -0.0031(13) -0.0054(13) C15 0.0365(16) 0.065(2) 0.058(2) -0.0369(18) -0.0045(14) -0.0071(15) C16 0.0398(17) 0.076(3) 0.0488(19) -0.0309(19) -0.0111(14) 0.0010(16) C17 0.0520(19) 0.056(2) 0.0462(19) -0.0201(17) -0.0083(15) 0.0026(16) C18 0.0399(16) 0.0501(18) 0.0484(18) -0.0250(15) -0.0002(13) -0.0066(14) C19 0.0342(14) 0.0441(16) 0.0407(16) -0.0196(14) -0.0027(12) -0.0032(12) C20 0.0401(16) 0.0529(19) 0.0531(19) -0.0267(16) -0.0078(14) -0.0045(14) C21 0.0379(17) 0.065(2) 0.062(2) -0.0176(19) -0.0165(16) -0.0025(16) C22 0.0386(18) 0.053(2) 0.078(3) -0.019(2) -0.0047(17) 0.0072(15) C23 0.050(2) 0.0467(19) 0.072(2) -0.0272(18) -0.0007(17) 0.0062(15) C24 0.0416(17) 0.0474(18) 0.056(2) -0.0286(16) -0.0055(14) 0.0013(14) C25 0.0486(18) 0.0468(18) 0.0556(19) -0.0260(16) -0.0053(15) -0.0149(14) C26 0.052(2) 0.087(3) 0.075(3) -0.045(2) 0.0131(19) -0.032(2) C27 0.0407(18) 0.069(2) 0.055(2) -0.0280(19) 0.0075(15) -0.0108(16) C28 0.0474(18) 0.063(2) 0.0402(17) -0.0277(16) 0.0023(14) -0.0105(15) C29 0.0358(15) 0.0555(19) 0.0500(18) -0.0344(16) -0.0050(13) 0.0002(13) C30 0.0336(14) 0.0457(17) 0.0508(18) -0.0286(15) -0.0023(13) -0.0015(12) C31 0.0434(17) 0.0445(18) 0.067(2) -0.0331(17) -0.0037(15) -0.0009(14) C32 0.0459(18) 0.059(2) 0.086(3) -0.054(2) -0.0046(17) -0.0045(16) C33 0.0456(18) 0.068(2) 0.066(2) -0.049(2) -0.0073(16) 0.0006(16) C34 0.059(2) 0.096(3) 0.084(3) -0.070(3) -0.022(2) 0.012(2) C35 0.077(3) 0.103(4) 0.054(2) -0.044(3) -0.014(2) 0.007(3) C36 0.064(2) 0.083(3) 0.052(2) -0.032(2) -0.0022(18) -0.002(2) C37 0.0433(17) 0.063(2) 0.0483(19) -0.0283(17) -0.0023(14) -0.0038(15) C38 0.0342(15) 0.0547(19) 0.0499(18) -0.0332(16) 0.0007(13) -0.0048(13) C39 0.0340(14) 0.0505(18) 0.0493(17) -0.0325(15) -0.0011(12) -0.0064(13) C40 0.0422(17) 0.0456(18) 0.059(2) -0.0294(16) -0.0026(14) -0.0052(14) C41 0.0471(18) 0.055(2) 0.068(2) -0.0392(19) -0.0118(16) 0.0070(15) C42 0.0368(16) 0.057(2) 0.058(2) -0.0388(17) -0.0002(14) -0.0030(14) C43 0.0383(18) 0.090(3) 0.075(3) -0.059(2) 0.0017(17) -0.0034(18) C44 0.045(2) 0.101(3) 0.060(2) -0.050(2) 0.0118(17) -0.023(2) C45 0.057(2) 0.072(2) 0.053(2) -0.0337(19) 0.0069(16) -0.0217(19) C46 0.0449(17) 0.059(2) 0.0520(19) -0.0321(17) -0.0007(14) -0.0089(15) C47 0.0349(15) 0.0521(18) 0.0438(17) -0.0257(15) -0.0034(12) -0.0041(13) C48 0.0377(16) 0.060(2) 0.0450(17) -0.0269(16) 0.0021(13) -0.0070(14) C49 0.0391(17) 0.073(2) 0.053(2) -0.0255(19) 0.0037(15) -0.0092(16) C50 0.0448(19) 0.073(3) 0.059(2) -0.023(2) 0.0004(16) -0.0218(18) C51 0.064(2) 0.064(2) 0.070(2) -0.038(2) -0.0024(19) -0.0213(19) C52 0.0437(17) 0.062(2) 0.060(2) -0.0383(18) 0.0044(15) -0.0128(15) C53 0.0512(19) 0.0501(19) 0.056(2) -0.0241(17) -0.0039(16) 0.0087(15) C54 0.052(2) 0.089(3) 0.093(3) -0.049(3) -0.020(2) 0.015(2) C55 0.082(3) 0.112(4) 0.122(4) -0.077(4) -0.053(3) 0.025(3) C56 0.053(2) 0.085(3) 0.048(2) -0.039(2) -0.0066(16) 0.0005(19) B1 0.0305(15) 0.0404(17) 0.0394(17) -0.0206(15) -0.0007(13) -0.0049(13) B2 0.0297(15) 0.050(2) 0.0456(19) -0.0275(17) -0.0028(13) -0.0017(14) Cl1 0.0424(4) 0.0674(6) 0.0781(6) -0.0450(5) -0.0141(4) 0.0132(4) Cl2 0.0603(5) 0.0627(6) 0.0540(5) -0.0173(4) 0.0019(4) -0.0241(4) Cl3 0.0452(4) 0.0634(5) 0.0705(6) -0.0365(5) 0.0002(4) -0.0177(4) Cl4 0.0501(5) 0.0603(5) 0.0592(5) -0.0221(4) -0.0082(4) 0.0024(4) O1 0.0361(10) 0.0457(12) 0.0422(11) -0.0231(10) -0.0008(8) -0.0096(9) O2 0.0393(11) 0.0561(13) 0.0427(12) -0.0256(11) -0.0024(9) 0.0010(10) Zr1 0.03012(14) 0.03814(15) 0.04295(16 -0.02206(13 -0.00167(11 -0.00354(11) Zr2 0.03232(15) 0.04470(17) 0.04961(18 -0.02804(15 -0.00331(12 -0.00377(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 C1 C9 1.426(4) . y C1 C2 1.440(4) . y C1 C5 1.445(4) . y C1 Zr1 2.539(3) . y C2 C3 1.428(4) . y C2 B1 1.615(4) . y C2 Zr1 2.452(3) . y C3 C4 1.408(4) . y C3 Zr1 2.433(3) . y C4 C5 1.413(5) . y C4 Zr1 2.537(3) . y C5 C6 1.424(5) . y C5 Zr1 2.621(3) . y C6 C7 1.343(6) . y C7 C8 1.417(5) . y C8 C9 1.354(5) . y C10 C18 1.427(4) . y C10 C11 1.438(4) . y C10 C14 1.446(4) . y C10 Zr1 2.518(3) . y C11 C12 1.425(4) . y C11 B1 1.609(4) . y C11 Zr1 2.439(3) . y C12 C13 1.405(4) . y C12 Zr1 2.454(3) . y C13 C14 1.408(5) . y C13 Zr1 2.560(3) . y C14 C15 1.426(4) . y C14 Zr1 2.643(3) . y C15 C16 1.342(5) . y C16 C17 1.413(5) . y C17 C18 1.351(5) . y C19 C20 1.394(4) . y C19 C24 1.400(4) . y C19 B1 1.603(4) . y C20 C21 1.386(5) . y C21 C22 1.378(5) . y C22 C23 1.383(5) . y C23 C24 1.384(5) . y C25 O1 1.475(3) . y C25 C26 1.502(5) . y C26 C27 1.516(5) . y C27 C28 1.504(5) . y C28 O1 1.467(4) . y C29 C37 1.426(5) . y C29 C33 1.437(4) . y C29 C30 1.441(4) . y C29 Zr2 2.540(3) . y C30 C31 1.432(4) . y C30 B2 1.607(4) . y C30 Zr2 2.443(3) . y C31 C32 1.406(5) . y C31 Zr2 2.435(3) . y C32 C33 1.416(5) . y C32 Zr2 2.541(3) . y C33 C34 1.431(5) . y C33 Zr2 2.619(3) . y C34 C35 1.354(6) . y C35 C36 1.399(6) . y C36 C37 1.359(5) . y C38 C46 1.428(5) . y C38 C39 1.441(4) . y C38 C42 1.444(4) . y C38 Zr2 2.511(3) . y C39 C40 1.424(5) . y C39 B2 1.620(4) . y C39 Zr2 2.437(3) . y C40 C41 1.411(5) . y C40 Zr2 2.466(3) . y C41 C42 1.398(5) . y C41 Zr2 2.586(3) . y C42 C43 1.431(5) . y C42 Zr2 2.645(3) . y C43 C44 1.353(6) . y C44 C45 1.404(6) . y C45 C46 1.364(5) . y C47 C52 1.388(4) . y C47 C48 1.399(4) . y C47 B2 1.603(5) . y C48 C49 1.379(5) . y C49 C50 1.378(5) . y C50 C51 1.366(5) . y C51 C52 1.393(5) . y C53 O2 1.481(4) . y C53 C54 1.496(5) . y C54 C55 1.475(6) . y C55 C56 1.452(6) . y C56 O2 1.472(4) . y B1 O1 1.627(4) . y B2 O2 1.625(4) . y Cl1 Zr1 2.4188(9) . y Cl2 Zr1 2.4297(11) . y Cl3 Zr2 2.4198(9) . y Cl4 Zr2 2.4298(11) . y 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 C9 C1 C2 132.5(3) . . y C9 C1 C5 118.3(3) . . y C2 C1 C5 109.2(3) . . y C9 C1 Zr1 120.1(2) . . y C2 C1 Zr1 69.93(16) . . y C5 C1 Zr1 76.88(17) . . y C3 C2 C1 104.9(3) . . y C3 C2 B1 125.4(3) . . y C1 C2 B1 125.5(3) . . y C3 C2 Zr1 72.28(16) . . y C1 C2 Zr1 76.58(16) . . y B1 C2 Zr1 98.16(16) . . y C4 C3 C2 110.7(3) . . y C4 C3 Zr1 77.63(18) . . y C2 C3 Zr1 73.72(16) . . y C3 C4 C5 108.1(3) . . y C3 C4 Zr1 69.54(17) . . y C5 C4 Zr1 77.41(18) . . y C4 C5 C6 133.4(3) . . y C4 C5 C1 107.1(3) . . y C6 C5 C1 119.5(3) . . y C4 C5 Zr1 70.83(17) . . y C6 C5 Zr1 124.0(2) . . y C1 C5 Zr1 70.64(16) . . y C7 C6 C5 119.6(3) . . y C6 C7 C8 121.4(3) . . y C9 C8 C7 121.6(4) . . y C8 C9 C1 119.6(3) . . y C18 C10 C11 132.6(3) . . y C18 C10 C14 118.2(3) . . y C11 C10 C14 109.1(3) . . y C18 C10 Zr1 119.2(2) . . y C11 C10 Zr1 70.15(16) . . y C14 C10 Zr1 78.54(17) . . y C12 C11 C10 104.7(2) . . y C12 C11 B1 122.9(3) . . y C10 C11 B1 128.9(3) . . y C12 C11 Zr1 73.66(17) . . y C10 C11 Zr1 76.19(16) . . y B1 C11 Zr1 98.83(17) . . y C13 C12 C11 111.1(3) . . y C13 C12 Zr1 77.91(18) . . y C11 C12 Zr1 72.49(16) . . y C12 C13 C14 107.7(3) . . y C12 C13 Zr1 69.64(17) . . y C14 C13 Zr1 77.58(17) . . y C13 C14 C15 132.6(3) . . y C13 C14 C10 107.2(3) . . y C15 C14 C10 120.2(3) . . y C13 C14 Zr1 71.07(17) . . y C15 C14 Zr1 124.8(2) . . y C10 C14 Zr1 69.04(16) . . y C16 C15 C14 118.6(3) . . y C15 C16 C17 121.7(3) . . y C18 C17 C16 122.3(3) . . y C17 C18 C10 118.9(3) . . y C20 C19 C24 116.5(3) . . y C20 C19 B1 122.7(3) . . y C24 C19 B1 120.6(3) . . y C21 C20 C19 122.2(3) . . y C22 C21 C20 119.8(3) . . y C21 C22 C23 119.8(3) . . y C22 C23 C24 119.9(3) . . y C23 C24 C19 121.9(3) . . y O1 C25 C26 106.5(3) . . y C25 C26 C27 106.5(3) . . y C28 C27 C26 103.9(3) . . y O1 C28 C27 104.7(3) . . y C37 C29 C33 118.0(3) . . y C37 C29 C30 132.4(3) . . y C33 C29 C30 109.6(3) . . y C37 C29 Zr2 120.7(2) . . y C33 C29 Zr2 76.89(18) . . y C30 C29 Zr2 69.53(16) . . y C31 C30 C29 104.7(3) . . y C31 C30 B2 124.9(3) . . y C29 C30 B2 126.5(3) . . y C31 C30 Zr2 72.61(17) . . y C29 C30 Zr2 76.92(17) . . y B2 C30 Zr2 98.26(18) . . y C32 C31 C30 110.5(3) . . y C32 C31 Zr2 77.8(2) . . y C30 C31 Zr2 73.25(18) . . y C31 C32 C33 108.3(3) . . y C31 C32 Zr2 69.45(18) . . y C33 C32 Zr2 77.12(19) . . y C32 C33 C34 133.5(3) . . y C32 C33 C29 106.9(3) . . y C34 C33 C29 119.6(4) . . y C32 C33 Zr2 71.08(19) . . y C34 C33 Zr2 123.7(2) . . y C29 C33 Zr2 70.82(17) . . y C35 C34 C33 119.5(4) . . y C34 C35 C36 121.2(4) . . y C37 C36 C35 121.6(4) . . y C36 C37 C29 120.1(3) . . y C46 C38 C39 132.5(3) . . y C46 C38 C42 118.7(3) . . y C39 C38 C42 108.7(3) . . y C46 C38 Zr2 117.6(2) . . y C39 C38 Zr2 70.26(17) . . y C42 C38 Zr2 78.91(19) . . y C40 C39 C38 104.9(3) . . y C40 C39 B2 122.0(3) . . y C38 C39 B2 129.4(3) . . y C40 C39 Zr2 74.21(17) . . y C38 C39 Zr2 75.92(17) . . y B2 C39 Zr2 98.12(18) . . y C41 C40 C39 110.7(3) . . y C41 C40 Zr2 78.54(19) . . y C39 C40 Zr2 72.01(17) . . y C42 C41 C40 107.9(3) . . y C42 C41 Zr2 76.84(19) . . y C40 C41 Zr2 69.12(18) . . y C41 C42 C43 132.3(3) . . y C41 C42 C38 107.7(3) . . y C43 C42 C38 120.0(3) . . y C41 C42 Zr2 72.20(19) . . y C43 C42 Zr2 125.5(2) . . y C38 C42 Zr2 68.70(17) . . y C44 C43 C42 118.7(4) . . y C43 C44 C45 121.4(3) . . y C46 C45 C44 122.7(4) . . y C45 C46 C38 118.4(3) . . y C52 C47 C48 115.7(3) . . y C52 C47 B2 122.5(3) . . y C48 C47 B2 121.5(3) . . y C49 C48 C47 122.7(3) . . y C50 C49 C48 119.7(3) . . y C51 C50 C49 119.7(3) . . y C50 C51 C52 120.1(4) . . y C47 C52 C51 122.1(3) . . y O2 C53 C54 106.1(3) . . y C55 C54 C53 106.6(3) . . y C56 C55 C54 107.4(4) . . y C55 C56 O2 105.6(3) . . y C19 B1 C11 116.3(2) . . y C19 B1 C2 118.6(3) . . y C11 B1 C2 101.3(2) . . y C19 B1 O1 107.6(2) . . y C11 B1 O1 106.2(2) . . y C2 B1 O1 105.8(2) . . y C47 B2 C30 118.0(3) . . y C47 B2 C39 116.0(3) . . y C30 B2 C39 101.6(2) . . y C47 B2 O2 107.3(2) . . y C30 B2 O2 106.5(2) . . y C39 B2 O2 106.6(2) . . y C28 O1 C25 107.1(2) . . y C28 O1 B1 116.9(2) . . y C25 O1 B1 118.7(2) . . y C56 O2 C53 107.5(2) . . y C56 O2 B2 117.1(3) . . y C53 O2 B2 118.6(2) . . y Cl1 Zr1 Cl2 99.29(4) . . y Cl1 Zr1 C3 93.65(8) . . y Cl2 Zr1 C3 136.40(8) . . y Cl1 Zr1 C11 125.33(7) . . y Cl2 Zr1 C11 121.36(8) . . y C3 Zr1 C11 81.45(10) . . y Cl1 Zr1 C2 127.49(7) . . y Cl2 Zr1 C2 121.10(8) . . y C3 Zr1 C2 34.00(10) . . y C11 Zr1 C2 61.31(9) . . y Cl1 Zr1 C12 133.10(8) . . y Cl2 Zr1 C12 88.45(8) . . y C3 Zr1 C12 112.09(10) . . y C11 Zr1 C12 33.85(10) . . y C2 Zr1 C12 83.56(10) . . y Cl1 Zr1 C10 91.83(7) . . y Cl2 Zr1 C10 134.90(7) . . y C3 Zr1 C10 85.55(10) . . y C11 Zr1 C10 33.66(9) . . y C2 Zr1 C10 82.65(10) . . y C12 Zr1 C10 54.19(10) . . y Cl1 Zr1 C4 81.84(8) . . y Cl2 Zr1 C4 108.47(8) . . y C3 Zr1 C4 32.83(10) . . y C11 Zr1 C4 113.28(10) . . y C2 Zr1 C4 55.74(10) . . y C12 Zr1 C4 139.16(10) . . y C10 Zr1 C4 116.36(10) . . y Cl1 Zr1 C1 134.98(7) . . y Cl2 Zr1 C1 88.85(7) . . y C3 Zr1 C1 54.41(10) . . y C11 Zr1 C1 84.37(9) . . y C2 Zr1 C1 33.49(10) . . y C12 Zr1 C1 91.00(10) . . y C10 Zr1 C1 113.22(9) . . y C4 Zr1 C1 53.86(10) . . y Cl1 Zr1 C13 102.87(8) . . y Cl2 Zr1 C13 81.12(8) . . y C3 Zr1 C13 135.92(10) . . y C11 Zr1 C13 55.60(9) . . y C2 Zr1 C13 114.49(10) . . y C12 Zr1 C13 32.46(10) . . y C10 Zr1 C13 53.78(10) . . y C4 Zr1 C13 168.71(10) . . y C1 Zr1 C13 122.15(10) . . y Cl1 Zr1 C5 104.37(8) . . y Cl2 Zr1 C5 82.87(8) . . y C3 Zr1 C5 53.56(11) . . y C11 Zr1 C5 114.77(9) . . y C2 Zr1 C5 55.11(10) . . y C12 Zr1 C5 122.52(10) . . y C10 Zr1 C5 136.22(10) . . y C4 Zr1 C5 31.75(11) . . y C1 Zr1 C5 32.47(9) . . y C13 Zr1 C5 150.23(11) . . y Cl1 Zr1 C14 80.93(7) . . y Cl2 Zr1 C14 106.59(7) . . y C3 Zr1 C14 116.53(10) . . y C11 Zr1 C14 54.88(9) . . y C2 Zr1 C14 113.53(10) . . y C12 Zr1 C14 52.78(10) . . y C10 Zr1 C14 32.42(9) . . y C4 Zr1 C14 142.90(11) . . y C1 Zr1 C14 138.88(9) . . y C13 Zr1 C14 31.35(10) . . y C5 Zr1 C14 168.49(10) . . y Cl3 Zr2 Cl4 99.71(4) . . y Cl3 Zr2 C31 92.37(8) . . y Cl4 Zr2 C31 136.20(9) . . y Cl3 Zr2 C39 124.38(8) . . y Cl4 Zr2 C39 122.29(8) . . y C31 Zr2 C39 81.72(11) . . y Cl3 Zr2 C30 126.34(8) . . y Cl4 Zr2 C30 121.42(8) . . y C31 Zr2 C30 34.14(10) . . y C39 Zr2 C30 61.66(10) . . y Cl3 Zr2 C40 133.55(8) . . y Cl4 Zr2 C40 89.29(9) . . y C31 Zr2 C40 112.06(11) . . y C39 Zr2 C40 33.77(11) . . y C30 Zr2 C40 83.40(10) . . y Cl3 Zr2 C38 90.84(8) . . y Cl4 Zr2 C38 134.98(8) . . y C31 Zr2 C38 86.20(11) . . y C39 Zr2 C38 33.82(10) . . y C30 Zr2 C38 83.45(10) . . y C40 Zr2 C38 54.30(11) . . y Cl3 Zr2 C29 134.05(7) . . y Cl4 Zr2 C29 89.07(8) . . y C31 Zr2 C29 54.37(11) . . y C39 Zr2 C29 85.06(10) . . y C30 Zr2 C29 33.55(10) . . y C40 Zr2 C29 91.16(10) . . y C38 Zr2 C29 114.19(10) . . y Cl3 Zr2 C32 81.04(8) . . y Cl4 Zr2 C32 108.04(10) . . y C31 Zr2 C32 32.73(11) . . y C39 Zr2 C32 113.49(11) . . y C30 Zr2 C32 55.74(10) . . y C40 Zr2 C32 139.00(11) . . y C38 Zr2 C32 116.83(12) . . y C29 Zr2 C32 53.60(11) . . y Cl3 Zr2 C41 103.81(8) . . y Cl4 Zr2 C41 81.52(9) . . y C31 Zr2 C41 135.98(11) . . y C39 Zr2 C41 55.26(10) . . y C30 Zr2 C41 114.28(10) . . y C40 Zr2 C41 32.33(10) . . y C38 Zr2 C41 53.49(11) . . y C29 Zr2 C41 122.11(11) . . y C32 Zr2 C41 168.64(11) . . y Cl3 Zr2 C33 103.91(8) . . y Cl4 Zr2 C33 82.54(9) . . y C31 Zr2 C33 53.67(12) . . y C39 Zr2 C33 115.31(10) . . y C30 Zr2 C33 55.24(10) . . y C40 Zr2 C33 122.47(11) . . y C38 Zr2 C33 137.10(11) . . y C29 Zr2 C33 32.29(10) . . y C32 Zr2 C33 31.81(12) . . y C41 Zr2 C33 149.92(12) . . y Cl3 Zr2 C42 81.28(7) . . y Cl4 Zr2 C42 106.10(8) . . y C31 Zr2 C42 117.33(11) . . y C39 Zr2 C42 54.77(10) . . y C30 Zr2 C42 114.06(10) . . y C40 Zr2 C42 52.61(10) . . y C38 Zr2 C42 32.39(10) . . y C29 Zr2 C42 139.32(9) . . y C32 Zr2 C42 143.64(12) . . y C41 Zr2 C42 30.97(11) . . y C33 Zr2 C42 169.23(10) . . y _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.775 _refine_diff_density_min -0.745 _refine_diff_density_rms 0.068 #=END data_rac1c ############################################################################ # # _publ_requested_journal 'Chemical Communications' _publ_section_title ; Donor complexes of bis(1-indenyl)phenylborane dichlorozirconium as isospecific catalysts in propene polymerization ; loop_ _publ_author_name _publ_author_address 'Manfred T. Reetz' ; Max-Planck-Institut f\"ur Kohlenforschung Kaiser-Wilhelm-Platz 1 D-45470 M\"ulheim an der Ruhr Germany ; 'Marc Willuhn' ; Max-Planck-Institut f\"ur Kohlenforschung Kaiser-Wilhelm-Platz 1 D-45470 M\"ulheim an der Ruhr Germany ; 'Christian Psiorz' ; Max-Planck-Institut f\"ur Kohlenforschung Kaiser-Wilhelm-Platz 1 D-45470 M\"ulheim an der Ruhr Germany ; 'Richard Goddard' ; Max-Planck-Institut f\"ur Kohlenforschung Kaiser-Wilhelm-Platz 1 D-45470 M\"ulheim an der Ruhr Germany ; # # ############################################################################ _chemical_name_systematic ; bis(1-indenyl)trimethylphosphinephenylborane dichlorozirconium ; _chemical_compound_source 'see paper' _chemical_formula_moiety 'C27 H26 B Cl2 P Zr, 2.5( C1 H2 Cl2)' _chemical_formula_sum 'C29.50 H31 B Cl7 P Zr' _chemical_formula_weight 766.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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 monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.5561(8) _cell_length_b 10.9508(2) _cell_length_c 20.6866(6) _cell_angle_alpha 90.00 _cell_angle_beta 121.201(2) _cell_angle_gamma 90.00 _cell_volume 6502.1(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 33.15 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method none _exptl_crystal_F_000 3096 _exptl_absorpt_coefficient_mu 0.983 _exptl_absorpt_correction_type none _publ_section_exptl_prep ; The crystal was mounted in a Lindemann glass capillary under argon. ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART' _diffrn_measurement_method 'CCD \w-scan' _diffrn_standards_number 0 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 34678 _diffrn_reflns_av_R_equivalents 0.0802 _diffrn_reflns_av_sigmaI/netI 0.0654 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 33.15 _reflns_number_total 11860 _reflns_number_gt 8996 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART software (Siemens, 1995)' _computing_cell_refinement 'SMART software (Siemens, 1995)' _computing_data_reduction 'SAINT software (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1976)' _publ_section_exptl_refinement ; 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. Largest difference Fourier peak: 2.678 e/\%A^3^, 0.789 \%A from Cl6. ; _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^)+(0.0002P)^2^+57.7838P] 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_number_reflns 11860 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0939 _refine_ls_R_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.1373 _refine_ls_wR_factor_gt 0.1190 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _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 C1 C 0.15987(10) 0.5385(3) 0.18180(17) 0.0131(5) Uani 1 1 d . . . C2 C 0.18372(11) 0.4236(3) 0.20200(18) 0.0166(6) Uani 1 1 d . . . H2 H 0.2064 0.3990 0.2540 0.020 Uiso 1 1 calc R . . C3 C 0.17581(11) 0.3593(3) 0.13703(19) 0.0183(6) Uani 1 1 d . . . H3 H 0.1910 0.2829 0.1368 0.022 Uiso 1 1 calc R . . C4 C 0.14771(11) 0.4337(3) 0.07363(18) 0.0169(6) Uani 1 1 d . . . C5 C 0.13092(12) 0.4174(3) -0.0050(2) 0.0223(7) Uani 1 1 d . . . H5 H 0.1373 0.3461 -0.0224 0.027 Uiso 1 1 calc R . . C6 C 0.10539(12) 0.5089(4) -0.05391(19) 0.0233(7) Uani 1 1 d . . . H6 H 0.0948 0.4999 -0.1050 0.028 Uiso 1 1 calc R . . C7 C 0.09454(11) 0.6176(3) -0.02860(18) 0.0208(6) Uani 1 1 d . . . H7 H 0.0775 0.6786 -0.0633 0.025 Uiso 1 1 calc R . . C8 C 0.10868(11) 0.6341(3) 0.04589(17) 0.0170(6) Uani 1 1 d . . . H8 H 0.0999 0.7039 0.0610 0.020 Uiso 1 1 calc R . . C9 C 0.13692(10) 0.5441(3) 0.10019(17) 0.0146(5) Uani 1 1 d . . . C10 C 0.10496(10) 0.5302(3) 0.22832(16) 0.0134(5) Uani 1 1 d . . . C11 C 0.05957(10) 0.5386(3) 0.16171(17) 0.0153(5) Uani 1 1 d . . . H11 H 0.0473 0.6127 0.1310 0.018 Uiso 1 1 calc R . . C12 C 0.03223(11) 0.4352(3) 0.15310(18) 0.0186(6) Uani 1 1 d . . . H12 H -0.0009 0.4248 0.1151 0.022 Uiso 1 1 calc R . . C13 C 0.05948(11) 0.3571(3) 0.21580(17) 0.0168(6) Uani 1 1 d . . . C14 C 0.04939(13) 0.2436(3) 0.2376(2) 0.0230(7) Uani 1 1 d . . . H14 H 0.0201 0.2083 0.2089 0.028 Uiso 1 1 calc R . . C15 C 0.08317(14) 0.1877(3) 0.3009(2) 0.0263(7) Uani 1 1 d . . . H15 H 0.0765 0.1147 0.3164 0.032 Uiso 1 1 calc R . . C16 C 0.12882(13) 0.2385(3) 0.34427(19) 0.0227(7) Uani 1 1 d . . . H16 H 0.1515 0.1963 0.3863 0.027 Uiso 1 1 calc R . . C17 C 0.14003(12) 0.3476(3) 0.32562(17) 0.0180(6) Uani 1 1 d . . . H17 H 0.1701 0.3788 0.3544 0.022 Uiso 1 1 calc R . . C18 C 0.10492(11) 0.4132(3) 0.26123(17) 0.0147(5) Uani 1 1 d . . . C19 C 0.19545(11) 0.6061(3) 0.32653(17) 0.0153(5) Uani 1 1 d . . . C20 C 0.19166(12) 0.6080(3) 0.39104(18) 0.0180(6) Uani 1 1 d . . . H20 H 0.1622 0.6091 0.3849 0.022 Uiso 1 1 calc R . . C21 C 0.23047(13) 0.6083(3) 0.46370(18) 0.0225(7) Uani 1 1 d . . . H21 H 0.2268 0.6106 0.5052 0.027 Uiso 1 1 calc R . . C22 C 0.27469(13) 0.6051(3) 0.47421(19) 0.0250(7) Uani 1 1 d . . . H22 H 0.3008 0.6039 0.5228 0.030 Uiso 1 1 calc R . . C23 C 0.27994(12) 0.6036(3) 0.41192(19) 0.0219(7) Uani 1 1 d . . . H23 H 0.3096 0.6010 0.4186 0.026 Uiso 1 1 calc R . . C24 C 0.24056(11) 0.6060(3) 0.33909(18) 0.0179(6) Uani 1 1 d . . . H24 H 0.2445 0.6077 0.2978 0.022 Uiso 1 1 calc R . . C25 C 0.07842(12) 0.8407(3) 0.1581(2) 0.0223(7) Uani 1 1 d . . . H25A H 0.0577 0.8063 0.1722 0.033 Uiso 1 1 calc R . . H25B H 0.0688 0.8161 0.1075 0.033 Uiso 1 1 calc R . . H25C H 0.0777 0.9282 0.1605 0.033 Uiso 1 1 calc R . . C26 C 0.17496(12) 0.8541(3) 0.1940(2) 0.0224(7) Uani 1 1 d . . . H26A H 0.1695 0.8157 0.1484 0.034 Uiso 1 1 calc R . . H26B H 0.2069 0.8425 0.2332 0.034 Uiso 1 1 calc R . . H26C H 0.1685 0.9399 0.1853 0.034 Uiso 1 1 calc R . . C27 C 0.15203(15) 0.8686(3) 0.3087(2) 0.0276(7) Uani 1 1 d . . . H27A H 0.1334 0.8382 0.3281 0.041 Uiso 1 1 calc R . . H27B H 0.1460 0.9541 0.2978 0.041 Uiso 1 1 calc R . . H27C H 0.1844 0.8567 0.3456 0.041 Uiso 1 1 calc R . . C28 C 0.22595(15) 0.6522(3) 0.0653(2) 0.0295(8) Uani 1 1 d . . . H28A H 0.1950 0.6189 0.0462 0.035 Uiso 1 1 calc R . . H28B H 0.2376 0.6210 0.0344 0.035 Uiso 1 1 calc R . . C29 C 0.05231(15) 0.0370(5) -0.0305(3) 0.0398(10) Uani 1 1 d . . . H29A H 0.0350 0.1011 -0.0666 0.048 Uiso 1 1 calc R . . H29B H 0.0605 0.0657 0.0193 0.048 Uiso 1 1 calc R . . C30 C 0.0000 0.6661(9) 0.2500 0.150(9) Uani 1 2 d S . . H30 H 0.0122 0.6140 0.2262 0.180 Uiso 1 1 calc R . . B B 0.15021(11) 0.6076(3) 0.24183(18) 0.0130(6) Uani 1 1 d . . . Cl1 Cl 0.11626(3) 0.16062(7) 0.16714(5) 0.02059(15) Uani 1 1 d . . . Cl2 Cl 0.03805(3) 0.35125(8) 0.00663(4) 0.02006(15) Uani 1 1 d . . . Cl3 Cl 0.22279(3) 0.81304(8) 0.05921(6) 0.02862(19) Uani 1 1 d . . . Cl4 Cl 0.01720(4) -0.09485(11 -0.05360(7) 0.0413(3) Uani 1 1 d . . . Cl5 Cl 0.26296(4) 0.60524(13) 0.15954(8) 0.0517(3) Uani 1 1 d . . . Cl6 Cl 0.10316(5) 0.0047(2) -0.03128(11) 0.0892(7) Uani 1 1 d . . . Cl7 Cl 0.04497(9) 0.7569(3) 0.31879(12) 0.1137(10) Uani 1 1 d . . . P P 0.13735(3) 0.78694(7) 0.22274(5) 0.01606(15) Uani 1 1 d . . . Zr Zr 0.100361(10 0.37754(3) 0.137428(16 0.01220(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0105(12) 0.0128(12) 0.0152(12) -0.0016(10) 0.0061(10) -0.0014(10) C2 0.0141(13) 0.0168(14) 0.0181(14) -0.0013(11) 0.0077(11) 0.0012(11) C3 0.0179(14) 0.0145(14) 0.0254(15) -0.0001(12) 0.0134(12) 0.0028(11) C4 0.0186(14) 0.0172(14) 0.0184(14) -0.0043(11) 0.0121(12) -0.0022(11) C5 0.0282(17) 0.0224(16) 0.0242(16) -0.0067(13) 0.0191(14) -0.0059(13) C6 0.0259(16) 0.0287(18) 0.0184(14) -0.0015(13) 0.0137(13) -0.0071(14) C7 0.0202(14) 0.0242(16) 0.0161(13) 0.0017(13) 0.0080(12) -0.0032(13) C8 0.0183(13) 0.0166(14) 0.0171(13) -0.0010(11) 0.0099(11) -0.0020(11) C9 0.0161(13) 0.0146(13) 0.0156(13) 0.0014(11) 0.0099(11) 0.0001(10) C10 0.0146(12) 0.0142(13) 0.0128(12) -0.0009(10) 0.0081(10) 0.0002(10) C11 0.0141(13) 0.0142(13) 0.0167(13) -0.0005(11) 0.0075(11) 0.0022(10) C12 0.0147(13) 0.0238(16) 0.0181(14) -0.0004(12) 0.0090(11) 0.0012(11) C13 0.0164(13) 0.0197(15) 0.0164(13) -0.0022(11) 0.0100(11) -0.0035(11) C14 0.0261(17) 0.0251(17) 0.0240(16) -0.0040(14) 0.0175(14) -0.0094(13) C15 0.040(2) 0.0202(16) 0.0264(17) -0.0009(14) 0.0222(16) -0.0107(15) C16 0.0312(18) 0.0185(15) 0.0184(15) 0.0017(12) 0.0129(14) -0.0003(13) C17 0.0227(15) 0.0165(14) 0.0141(13) -0.0005(11) 0.0090(12) -0.0001(11) C18 0.0173(13) 0.0138(13) 0.0147(12) -0.0014(10) 0.0094(11) -0.0003(10) C19 0.0182(13) 0.0119(13) 0.0130(12) -0.0011(10) 0.0062(11) -0.0024(10) C20 0.0224(15) 0.0143(13) 0.0161(13) -0.0015(11) 0.0093(12) -0.0034(11) C21 0.0325(17) 0.0159(15) 0.0144(13) -0.0015(12) 0.0088(13) -0.0008(13) C22 0.0272(17) 0.0202(16) 0.0165(14) 0.0002(12) 0.0034(13) -0.0027(13) C23 0.0170(14) 0.0182(15) 0.0214(15) 0.0029(12) 0.0035(12) -0.0035(11) C24 0.0157(13) 0.0171(14) 0.0155(13) 0.0017(11) 0.0042(11) -0.0021(11) C25 0.0230(16) 0.0159(14) 0.0266(16) 0.0025(13) 0.0118(13) 0.0050(12) C26 0.0246(16) 0.0176(15) 0.0258(16) -0.0003(13) 0.0136(14) -0.0036(12) C27 0.041(2) 0.0161(15) 0.0242(16) -0.0052(13) 0.0163(15) 0.0021(15) C28 0.038(2) 0.0176(16) 0.039(2) 0.0007(15) 0.0249(18) -0.0037(14) C29 0.032(2) 0.042(2) 0.046(2) -0.020(2) 0.0211(19) -0.0085(18) C30 0.32(2) 0.033(4) 0.28(2) 0.000 0.29(2) 0.000 B 0.0152(14) 0.0112(14) 0.0129(13) -0.0003(11) 0.0075(11) 0.0013(11) Cl1 0.0261(4) 0.0115(3) 0.0223(3) 0.0011(3) 0.0112(3) 0.0006(3) Cl2 0.0181(3) 0.0223(4) 0.0145(3) -0.0007(3) 0.0047(3) -0.0025(3) Cl3 0.0323(4) 0.0203(4) 0.0327(5) -0.0001(3) 0.0165(4) -0.0001(3) Cl4 0.0411(6) 0.0355(5) 0.0413(6) -0.0162(5) 0.0170(5) -0.0060(4) Cl5 0.0426(6) 0.0519(7) 0.0589(7) 0.0296(6) 0.0251(6) 0.0135(5) Cl6 0.0305(6) 0.1461(18) 0.0930(12) -0.0814(13) 0.0334(7) -0.0311(8) Cl7 0.1239(18) 0.164(2) 0.0837(13) 0.0723(15) 0.0755(14) 0.0929(18) P 0.0202(4) 0.0114(3) 0.0162(3) -0.0008(3) 0.0091(3) 0.0001(3) Zr 0.01259(12) 0.01061(12) 0.01266(12 -0.00062(10) 0.00602(9) -0.00072(10) _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 C1 C2 1.432(4) . y C1 C9 1.449(4) . y C1 B 1.624(4) . y C1 Zr 2.457(3) . y C2 C3 1.416(4) . y C2 Zr 2.448(3) . y C3 C4 1.412(5) . y C3 Zr 2.544(3) . y C4 C5 1.430(5) . y C4 C9 1.449(4) . y C4 Zr 2.611(3) . y C5 C6 1.365(5) . y C6 C7 1.421(5) . y C7 C8 1.369(4) . y C8 C9 1.425(4) . y C9 Zr 2.530(3) . y C10 C11 1.433(4) . y C10 C18 1.451(4) . y C10 B 1.632(4) . y C10 Zr 2.460(3) . y C11 C12 1.409(5) . y C11 Zr 2.439(3) . y C12 C13 1.422(5) . y C12 Zr 2.549(3) . y C13 C14 1.422(5) . y C13 C18 1.450(4) . y C13 Zr 2.620(3) . y C14 C15 1.355(5) . y C15 C16 1.427(5) . y C16 C17 1.367(5) . y C17 C18 1.433(4) . y C18 Zr 2.516(3) . y C19 C24 1.397(4) . y C19 C20 1.405(4) . y C19 B 1.618(4) . y C20 C21 1.388(5) . y C21 C22 1.384(5) . y C22 C23 1.388(5) . y C23 C24 1.398(4) . y C25 P 1.818(3) . y C26 P 1.806(3) . y C27 P 1.816(4) . y C28 Cl5 1.760(4) . y C28 Cl3 1.765(4) . y C29 Cl6 1.751(4) . y C29 Cl4 1.765(5) . y C30 Cl7 1.751(6) 2 y C30 Cl7 1.751(6) . y B P 2.006(3) . y Cl1 Zr 2.4424(8) . y Cl2 Zr 2.4319(8) . y loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C9 104.9(3) . . y C2 C1 B 119.3(3) . . y C9 C1 B 132.5(3) . . y C2 C1 Zr 72.67(17) . . y C9 C1 Zr 75.91(17) . . y B C1 Zr 100.05(18) . . y C3 C2 C1 111.0(3) . . y C3 C2 Zr 77.29(18) . . y C1 C2 Zr 73.37(16) . . y C4 C3 C2 107.5(3) . . y C4 C3 Zr 76.75(18) . . y C2 C3 Zr 69.84(17) . . y C3 C4 C5 131.7(3) . . y C3 C4 C9 107.9(3) . . y C5 C4 C9 120.4(3) . . y C3 C4 Zr 71.50(18) . . y C5 C4 Zr 124.1(2) . . y C9 C4 Zr 70.59(16) . . y C6 C5 C4 118.6(3) . . y C5 C6 C7 121.6(3) . . y C8 C7 C6 121.3(3) . . y C7 C8 C9 119.8(3) . . y C8 C9 C4 118.2(3) . . y C8 C9 C1 133.1(3) . . y C4 C9 C1 108.7(3) . . y C8 C9 Zr 120.6(2) . . y C4 C9 Zr 76.72(18) . . y C1 C9 Zr 70.35(16) . . y C11 C10 C18 104.4(3) . . y C11 C10 B 124.2(3) . . y C18 C10 B 127.2(3) . . y C11 C10 Zr 72.19(17) . . y C18 C10 Zr 75.17(17) . . y B C10 Zr 99.68(17) . . y C12 C11 C10 111.6(3) . . y C12 C11 Zr 77.94(18) . . y C10 C11 Zr 73.81(17) . . y C11 C12 C13 107.4(3) . . y C11 C12 Zr 69.33(17) . . y C13 C12 Zr 76.81(18) . . y C12 C13 C14 132.0(3) . . y C12 C13 C18 107.5(3) . . y C14 C13 C18 120.6(3) . . y C12 C13 Zr 71.30(17) . . y C14 C13 Zr 123.9(2) . . y C18 C13 Zr 69.69(16) . . y C15 C14 C13 119.0(3) . . y C14 C15 C16 121.3(3) . . y C17 C16 C15 121.8(3) . . y C16 C17 C18 119.1(3) . . y C17 C18 C13 118.2(3) . . y C17 C18 C10 132.8(3) . . y C13 C18 C10 109.0(3) . . y C17 C18 Zr 117.1(2) . . y C13 C18 Zr 77.61(17) . . y C10 C18 Zr 70.96(16) . . y C24 C19 C20 116.5(3) . . y C24 C19 B 121.3(3) . . y C20 C19 B 122.2(3) . . y C21 C20 C19 122.2(3) . . y C22 C21 C20 119.9(3) . . y C21 C22 C23 119.7(3) . . y C22 C23 C24 119.8(3) . . y C19 C24 C23 121.9(3) . . y Cl5 C28 Cl3 110.7(2) . . y Cl6 C29 Cl4 110.4(3) . . y Cl7 C30 Cl7 110.8(5) 2 . y C19 B C1 112.1(2) . . y C19 B C10 116.6(2) . . y C1 B C10 99.4(2) . . y C19 B P 102.0(2) . . y C1 B P 114.4(2) . . y C10 B P 112.9(2) . . y C26 P C27 103.89(18) . . y C26 P C25 107.78(17) . . y C27 P C25 101.57(17) . . y C26 P B 110.35(15) . . y C27 P B 111.58(16) . . y C25 P B 120.21(15) . . y Cl2 Zr C11 93.67(7) . . y Cl2 Zr Cl1 96.58(3) . . y C11 Zr Cl1 136.40(8) . . y Cl2 Zr C2 135.43(8) . . y C11 Zr C2 110.07(10) . . y Cl1 Zr C2 91.39(8) . . y Cl2 Zr C1 124.37(7) . . y C11 Zr C1 80.71(10) . . y Cl1 Zr C1 125.06(7) . . y C2 Zr C1 33.95(10) . . y Cl2 Zr C10 127.46(7) . . y C11 Zr C10 34.00(10) . . y Cl1 Zr C10 123.32(7) . . y C2 Zr C10 80.87(10) . . y C1 Zr C10 60.67(10) . . y Cl2 Zr C18 135.63(7) . . y C11 Zr C18 54.74(10) . . y Cl1 Zr C18 90.27(7) . . y C2 Zr C18 87.87(10) . . y C1 Zr C18 84.21(10) . . y C10 Zr C18 33.87(10) . . y Cl2 Zr C9 91.13(7) . . y C11 Zr C9 87.36(10) . . y Cl1 Zr C9 134.46(7) . . y C2 Zr C9 54.58(10) . . y C1 Zr C9 33.74(10) . . y C10 Zr C9 83.96(10) . . y C18 Zr C9 114.49(10) . . y Cl2 Zr C3 105.70(8) . . y C11 Zr C3 136.32(10) . . y Cl1 Zr C3 80.58(8) . . y C2 Zr C3 32.88(10) . . y C1 Zr C3 55.95(10) . . y C10 Zr C3 112.80(10) . . y C18 Zr C3 118.67(10) . . y C9 Zr C3 54.23(10) . . y Cl2 Zr C12 81.95(8) . . y C11 Zr C12 32.73(11) . . y Cl1 Zr C12 107.59(8) . . y C2 Zr C12 136.56(11) . . y C1 Zr C12 112.56(10) . . y C10 Zr C12 55.93(10) . . y C18 Zr C12 54.39(10) . . y C9 Zr C12 117.93(10) . . y C3 Zr C12 168.38(11) . . y Cl2 Zr C4 82.13(7) . . y C11 Zr C4 119.16(10) . . y Cl1 Zr C4 104.21(8) . . y C2 Zr C4 53.47(10) . . y C1 Zr C4 55.27(10) . . y C10 Zr C4 114.37(10) . . y C18 Zr C4 138.24(10) . . y C9 Zr C4 32.69(10) . . y C3 Zr C4 31.75(10) . . y C12 Zr C4 145.75(11) . . y Cl2 Zr C13 104.74(7) . . y C11 Zr C13 53.47(11) . . y Cl1 Zr C13 82.95(8) . . y C2 Zr C13 119.77(10) . . y C1 Zr C13 114.50(10) . . y C10 Zr C13 55.30(10) . . y C18 Zr C13 32.71(10) . . y C9 Zr C13 137.88(10) . . y C3 Zr C13 146.75(10) . . y C12 Zr C13 31.89(10) . . y C4 Zr C13 169.63(10) . . y _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 33.15 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 2.678 _refine_diff_density_min -2.144 _refine_diff_density_rms 0.147 #=END