Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name _publ_author_address 'Peter Roesky' ; Freie Universit\"at Berlin Fabeckstr. 34-36 14195 Berlin Bundesrepublik Deutschland ; 'Denise Girnt' ; Freie Universit\"at Berlin Fabeckstr. 34-36 14195 Berlin Bundesrepublik Deutschland ; 'Tarun K. Panda' '' 'Marcus Rastatter' '' 'Michal Wiecko' '' _publ_contact_author_name 'Prof Peter Roesky' _publ_contact_author_address ; Fachbereich Biologie, Chemie Freie Universitat Berlin Institut fur Chemia/Anorg.und Analy Fabeckstrasse, 34-36 Berlin D-14195 GERMANY ; _publ_contact_author_email ROESKY@CHEMIE.FU-BERLIN.DE _publ_section_title ; Zirconium Complexes having a Chiral Phosphanylamide in the Co-ordination Sphere ; _publ_contact_author ; Prof. Dr. Peter Roesky Freie Universit\"at Berlin Fabeckstr. 34-36 14195 Berlin Bundesrepublik Deutschland ; _publ_contact_author_fax +49/(0)3083852440 _publ_contact_author_phone +49/(0)3083854004 _publ_contact_letter ; ; _publ_requested_coeditor_name ? data_2 _database_code_depnum_ccdc_archive 'CCDC 265442' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H20 N O P' _chemical_formula_weight 321.34 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4(3) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+3/4' 'y, -x, z+1/4' _cell_length_a 11.4093(16) _cell_length_b 11.4093(16) _cell_length_c 13.279(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1728.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_size_max .6 _exptl_crystal_size_mid .6 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 0.163 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.784356 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'SADABS - Bruker/Siemens' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart 1000 CCD' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21279 _diffrn_reflns_av_R_equivalents 0.0151 _diffrn_reflns_av_sigmaI/netI 0.0123 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 30.49 _reflns_number_total 5226 _reflns_number_gt 5069 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _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^)+(0.0540P)^2^+0.0703P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(4) _refine_ls_number_reflns 5226 _refine_ls_number_parameters 213 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0276 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0742 _refine_ls_wR_factor_gt 0.0727 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.621330(18) 0.273343(18) 0.131252(16) 0.02219(5) Uani 1 1 d . . . N1 N 0.64076(7) 0.29457(7) 0.01075(6) 0.02730(15) Uani 1 1 d . . . H100 H 0.6693(15) 0.3695(15) -0.0146(13) 0.047(4) Uiso 1 1 d . . . O1 O 0.49753(6) 0.26659(7) 0.16700(6) 0.03361(15) Uani 1 1 d . . . C1 C 0.57575(8) 0.22457(9) -0.06351(7) 0.02991(17) Uani 1 1 d . . . H1 H 0.5313 0.1629 -0.0261 0.036 Uiso 1 1 calc R . . C2 C 0.48654(10) 0.30105(11) -0.11947(10) 0.0421(2) Uani 1 1 d . . . H2A H 0.4310 0.3345 -0.0711 0.063 Uiso 1 1 calc R . . H2B H 0.4440 0.2531 -0.1686 0.063 Uiso 1 1 calc R . . H2C H 0.5276 0.3645 -0.1545 0.063 Uiso 1 1 calc R . . C3 C 0.65634(9) 0.16331(8) -0.13742(7) 0.02931(17) Uani 1 1 d . . . C4 C 0.62706(12) 0.05077(10) -0.17161(10) 0.0430(3) Uani 1 1 d . . . H4 H 0.5589 0.0130 -0.1464 0.052 Uiso 1 1 calc R . . C5 C 0.69701(16) -0.00613(11) -0.24218(12) 0.0538(3) Uani 1 1 d . . . H5 H 0.6752 -0.0816 -0.2660 0.065 Uiso 1 1 calc R . . C6 C 0.79769(15) 0.04629(12) -0.27770(10) 0.0519(3) Uani 1 1 d . . . H6 H 0.8461 0.0067 -0.3249 0.062 Uiso 1 1 calc R . . C7 C 0.82794(12) 0.15777(12) -0.24383(9) 0.0435(3) Uani 1 1 d . . . H7 H 0.8976 0.1938 -0.2677 0.052 Uiso 1 1 calc R . . C8 C 0.75686(10) 0.21697(10) -0.17516(8) 0.0349(2) Uani 1 1 d . . . H8 H 0.7770 0.2939 -0.1541 0.042 Uiso 1 1 calc R . . C9 C 0.69477(8) 0.13817(7) 0.16326(7) 0.02676(16) Uani 1 1 d . . . C10 C 0.78633(9) 0.09323(9) 0.10536(9) 0.0363(2) Uani 1 1 d . . . H10 H 0.8107 0.1330 0.0461 0.044 Uiso 1 1 calc R . . C11 C 0.84241(11) -0.01062(10) 0.13454(14) 0.0514(3) Uani 1 1 d . . . H11 H 0.9048 -0.0411 0.0951 0.062 Uiso 1 1 calc R . . C12 C 0.80701(14) -0.06872(10) 0.22064(15) 0.0580(4) Uani 1 1 d . . . H12 H 0.8458 -0.1386 0.2407 0.070 Uiso 1 1 calc R . . C13 C 0.71568(14) -0.02572(11) 0.27737(13) 0.0549(4) Uani 1 1 d . . . H13 H 0.6911 -0.0669 0.3359 0.066 Uiso 1 1 calc R . . C14 C 0.65857(10) 0.07797(10) 0.24989(9) 0.0378(2) Uani 1 1 d . . . H14 H 0.5958 0.1073 0.2896 0.045 Uiso 1 1 calc R . . C15 C 0.70330(8) 0.39165(7) 0.18766(6) 0.02431(15) Uani 1 1 d . . . C16 C 0.66765(9) 0.50719(8) 0.16929(8) 0.03021(17) Uani 1 1 d . . . H16 H 0.6039 0.5222 0.1251 0.036 Uiso 1 1 calc R . . C17 C 0.72544(10) 0.59986(9) 0.21562(9) 0.0366(2) Uani 1 1 d . . . H17 H 0.7019 0.6781 0.2020 0.044 Uiso 1 1 calc R . . C18 C 0.81745(12) 0.57866(10) 0.28164(9) 0.0411(2) Uani 1 1 d . . . H18 H 0.8560 0.6423 0.3138 0.049 Uiso 1 1 calc R . . C19 C 0.85298(12) 0.46447(11) 0.30064(10) 0.0441(3) Uani 1 1 d . . . H19 H 0.9158 0.4499 0.3459 0.053 Uiso 1 1 calc R . . C20 C 0.79643(10) 0.37101(9) 0.25316(9) 0.0351(2) Uani 1 1 d . . . H20 H 0.8216 0.2930 0.2656 0.042 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 P1 0.02025(9) 0.02295(10) 0.02338(9) 0.00082(7) 0.00101(7) 0.00076(7) N1 0.0348(4) 0.0247(3) 0.0224(3) 0.0006(3) -0.0016(3) -0.0064(3) O1 0.0218(3) 0.0427(4) 0.0364(4) -0.0020(3) 0.0048(3) 0.0001(3) C1 0.0312(4) 0.0306(4) 0.0279(4) -0.0003(3) -0.0038(3) -0.0074(3) C2 0.0347(5) 0.0488(6) 0.0428(5) -0.0033(5) -0.0111(4) 0.0043(4) C3 0.0367(4) 0.0265(4) 0.0247(4) 0.0004(3) -0.0082(3) -0.0011(3) C4 0.0532(6) 0.0280(5) 0.0476(6) -0.0047(4) -0.0098(5) -0.0028(4) C5 0.0733(9) 0.0324(5) 0.0557(8) -0.0132(5) -0.0081(7) 0.0075(5) C6 0.0735(9) 0.0467(7) 0.0355(6) -0.0064(5) -0.0037(6) 0.0224(6) C7 0.0500(6) 0.0508(6) 0.0299(5) 0.0010(4) 0.0024(4) 0.0065(5) C8 0.0438(5) 0.0353(5) 0.0256(4) -0.0013(3) 0.0000(4) -0.0034(4) C9 0.0276(4) 0.0218(3) 0.0309(4) 0.0018(3) -0.0035(3) -0.0030(3) C10 0.0319(4) 0.0304(4) 0.0467(6) -0.0035(4) -0.0025(4) 0.0057(4) C11 0.0418(6) 0.0321(5) 0.0803(10) -0.0125(6) -0.0194(6) 0.0126(4) C12 0.0610(8) 0.0224(4) 0.0905(11) 0.0062(5) -0.0411(8) -0.0008(5) C13 0.0642(8) 0.0351(5) 0.0655(8) 0.0235(6) -0.0304(7) -0.0172(5) C14 0.0421(5) 0.0330(5) 0.0384(5) 0.0111(4) -0.0078(4) -0.0114(4) C15 0.0256(4) 0.0240(4) 0.0234(4) -0.0008(3) 0.0009(3) 0.0009(3) C16 0.0344(4) 0.0262(4) 0.0300(4) -0.0015(3) -0.0015(3) 0.0042(3) C17 0.0484(6) 0.0254(4) 0.0358(5) -0.0052(4) 0.0013(4) 0.0016(4) C18 0.0514(6) 0.0340(5) 0.0378(5) -0.0096(4) -0.0041(5) -0.0078(4) C19 0.0481(6) 0.0397(5) 0.0444(6) -0.0043(5) -0.0189(5) -0.0035(5) C20 0.0367(5) 0.0297(4) 0.0390(5) 0.0002(4) -0.0112(4) 0.0006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O1 1.4921(7) . ? P1 N1 1.6335(9) . ? P1 C15 1.8049(9) . ? P1 C9 1.8059(10) . ? N1 C1 1.4699(12) . ? C1 C3 1.5157(14) . ? C1 C2 1.5329(15) . ? C3 C8 1.3933(15) . ? C3 C4 1.4024(14) . ? C4 C5 1.392(2) . ? C5 C6 1.378(2) . ? C6 C7 1.392(2) . ? C7 C8 1.3948(16) . ? C9 C10 1.3947(15) . ? C9 C14 1.4020(14) . ? C10 C11 1.4012(15) . ? C11 C12 1.382(3) . ? C12 C13 1.376(3) . ? C13 C14 1.3990(17) . ? C15 C20 1.3932(13) . ? C15 C16 1.4009(12) . ? C16 C17 1.3897(14) . ? C17 C18 1.3889(17) . ? C18 C19 1.3876(17) . ? C19 C20 1.3967(15) . ? 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 O1 P1 N1 116.60(5) . . ? O1 P1 C15 113.40(4) . . ? N1 P1 C15 103.02(4) . . ? O1 P1 C9 108.68(4) . . ? N1 P1 C9 107.11(4) . . ? C15 P1 C9 107.49(4) . . ? C1 N1 P1 120.54(7) . . ? N1 C1 C3 112.26(8) . . ? N1 C1 C2 110.55(9) . . ? C3 C1 C2 110.57(8) . . ? C8 C3 C4 118.81(10) . . ? C8 C3 C1 121.98(8) . . ? C4 C3 C1 119.17(10) . . ? C5 C4 C3 120.57(13) . . ? C6 C5 C4 120.40(12) . . ? C5 C6 C7 119.50(12) . . ? C6 C7 C8 120.62(13) . . ? C3 C8 C7 120.07(10) . . ? C10 C9 C14 119.53(10) . . ? C10 C9 P1 122.12(8) . . ? C14 C9 P1 118.34(8) . . ? C9 C10 C11 120.03(12) . . ? C12 C11 C10 120.06(14) . . ? C13 C12 C11 120.20(11) . . ? C12 C13 C14 120.76(14) . . ? C13 C14 C9 119.40(13) . . ? C20 C15 C16 119.29(9) . . ? C20 C15 P1 121.86(7) . . ? C16 C15 P1 118.75(7) . . ? C17 C16 C15 120.07(9) . . ? C18 C17 C16 120.37(10) . . ? C19 C18 C17 119.94(10) . . ? C18 C19 C20 119.99(11) . . ? C15 C20 C19 120.34(10) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.253 _refine_diff_density_min -0.168 _refine_diff_density_rms 0.036 #============================================================================== data_4a _database_code_depnum_ccdc_archive 'CCDC 265443' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H29 Cl N P Zr' _chemical_formula_weight 561.18 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.6973(6) _cell_length_b 10.8436(6) _cell_length_c 13.5907(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.583(4) _cell_angle_gamma 90.00 _cell_volume 1277.65(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour colorless _exptl_crystal_size_max .16 _exptl_crystal_size_mid .12 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 0.617 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD DETECTOR KM4CCD/SAPPHIRE' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9926 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.12 _diffrn_reflns_theta_max 31.54 _reflns_number_total 5472 _reflns_number_gt 5319 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _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^)+(0.0291P)^2^+0.2761P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(2) _refine_ls_number_reflns 5472 _refine_ls_number_parameters 308 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0214 _refine_ls_R_factor_gt 0.0205 _refine_ls_wR_factor_ref 0.0526 _refine_ls_wR_factor_gt 0.0517 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.300011(16) -0.737877(14) 0.120829(10) 0.02299(5) Uani 1 1 d . . . Cl1 Cl 0.54380(5) -0.75044(6) 0.03031(3) 0.03865(12) Uani 1 1 d . . . N1 N 0.43220(16) -0.61398(15) 0.22323(10) 0.0225(3) Uani 1 1 d . . . P1 P 0.27770(5) -0.60710(4) 0.28375(3) 0.02163(9) Uani 1 1 d . . . C100 C 0.5748(2) -0.54420(17) 0.25268(13) 0.0264(4) Uani 1 1 d . . . H100 H 0.5447 -0.4735 0.2943 0.032 Uiso 1 1 calc R . . C1 C 0.1939(2) -0.45308(16) 0.28206(13) 0.0251(4) Uani 1 1 d . . . C2 C 0.0494(2) -0.43812(18) 0.31720(14) 0.0302(4) Uani 1 1 d . . . H2 H -0.0003 -0.5065 0.3447 0.036 Uiso 1 1 calc R . . C3 C -0.0233(2) -0.3235(2) 0.31230(15) 0.0360(4) Uani 1 1 d . . . H3 H -0.1213 -0.3133 0.3376 0.043 Uiso 1 1 calc R . . C4 C 0.0472(3) -0.2254(2) 0.27085(15) 0.0423(5) Uani 1 1 d . . . H4 H -0.0025 -0.1473 0.2676 0.051 Uiso 1 1 calc R . . C5 C 0.1893(2) -0.2385(3) 0.23380(15) 0.0417(4) Uani 1 1 d . . . H5 H 0.2372 -0.1701 0.2049 0.050 Uiso 1 1 calc R . . C6 C 0.2620(2) -0.35293(18) 0.23909(15) 0.0324(4) Uani 1 1 d . . . H6 H 0.3594 -0.3626 0.2130 0.039 Uiso 1 1 calc R . . C7 C 0.32539(19) -0.63777(16) 0.41582(13) 0.0244(3) Uani 1 1 d . . . C8 C 0.2768(2) -0.56263(19) 0.49041(15) 0.0329(4) Uani 1 1 d . . . H8 H 0.2130 -0.4933 0.4740 0.039 Uiso 1 1 calc R . . C9 C 0.3214(3) -0.5887(2) 0.58901(15) 0.0415(5) Uani 1 1 d . . . H9 H 0.2860 -0.5377 0.6394 0.050 Uiso 1 1 calc R . . C10 C 0.4154(3) -0.6870(2) 0.61414(15) 0.0403(5) Uani 1 1 d . . . H10 H 0.4463 -0.7034 0.6815 0.048 Uiso 1 1 calc R . . C11 C 0.4648(2) -0.76160(19) 0.54128(15) 0.0370(5) Uani 1 1 d . . . H11 H 0.5302 -0.8298 0.5583 0.044 Uiso 1 1 calc R . . C12 C 0.41946(19) -0.7377(2) 0.44261(12) 0.0305(3) Uani 1 1 d . . . H12 H 0.4533 -0.7905 0.3929 0.037 Uiso 1 1 calc R . . C13 C 0.6906(2) -0.62069(19) 0.31558(13) 0.0286(4) Uani 1 1 d . . . C14 C 0.7321(3) -0.5856(2) 0.41257(16) 0.0404(5) Uani 1 1 d . . . H14 H 0.6862 -0.5149 0.4393 0.049 Uiso 1 1 calc R . . C15 C 0.8402(3) -0.6535(3) 0.47045(18) 0.0547(7) Uani 1 1 d . . . H15 H 0.8686 -0.6285 0.5364 0.066 Uiso 1 1 calc R . . C16 C 0.9059(3) -0.7558(3) 0.43327(19) 0.0567(8) Uani 1 1 d . . . H16 H 0.9795 -0.8021 0.4733 0.068 Uiso 1 1 calc R . . C17 C 0.8654(3) -0.7919(3) 0.3373(2) 0.0510(6) Uani 1 1 d . . . H17 H 0.9118 -0.8629 0.3114 0.061 Uiso 1 1 calc R . . C18 C 0.7572(2) -0.7251(3) 0.27841(15) 0.0382(5) Uani 1 1 d . . . H18 H 0.7290 -0.7510 0.2127 0.046 Uiso 1 1 calc R . . C19 C 0.6454(2) -0.4895(2) 0.16324(15) 0.0340(4) Uani 1 1 d . . . H19A H 0.5686 -0.4384 0.1257 0.051 Uiso 1 1 calc R . . H19B H 0.6783 -0.5563 0.1211 0.051 Uiso 1 1 calc R . . H19C H 0.7348 -0.4388 0.1854 0.051 Uiso 1 1 calc R . . C20 C 0.3919(2) -0.92544(19) 0.22072(16) 0.0350(4) Uani 1 1 d . . . H20 H 0.4856 -0.9168 0.2611 0.042 Uiso 1 1 calc R . . C21 C 0.2441(3) -0.89982(18) 0.24909(16) 0.0334(4) Uani 1 1 d . . . H21 H 0.2190 -0.8733 0.3125 0.040 Uiso 1 1 calc R . . C22 C 0.1397(3) -0.92059(19) 0.16641(17) 0.0377(5) Uani 1 1 d . . . H22 H 0.0314 -0.9078 0.1636 0.045 Uiso 1 1 calc R . . C23 C 0.2217(3) -0.96309(19) 0.08946(17) 0.0415(5) Uani 1 1 d . . . H23 H 0.1787 -0.9860 0.0256 0.050 Uiso 1 1 calc R . . C24 C 0.3778(3) -0.96626(19) 0.12204(18) 0.0412(5) Uani 1 1 d . . . H24 H 0.4598 -0.9914 0.0845 0.049 Uiso 1 1 calc R . . C25 C 0.0817(3) -0.5892(3) 0.07447(18) 0.0585(8) Uani 1 1 d . . . H25 H 0.0372 -0.5477 0.1268 0.070 Uiso 1 1 calc R . . C26 C 0.0355(3) -0.7027(2) 0.03404(19) 0.0505(7) Uani 1 1 d . . . H26 H -0.0463 -0.7524 0.0540 0.061 Uiso 1 1 calc R . . C27 C 0.1289(3) -0.7297(3) -0.03952(15) 0.0554(7) Uani 1 1 d . . . H27 H 0.1232 -0.8017 -0.0795 0.066 Uiso 1 1 calc R . . C28 C 0.2315(3) -0.6352(4) -0.0454(2) 0.0682(9) Uani 1 1 d . . . H28 H 0.3091 -0.6307 -0.0907 0.082 Uiso 1 1 calc R . . C29 C 0.2051(4) -0.5478(3) 0.0241(3) 0.0675(10) Uani 1 1 d . . . H29 H 0.2605 -0.4730 0.0357 0.081 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.02232(8) 0.02254(7) 0.02341(7) -0.00111(7) -0.00262(5) -0.00120(8) Cl1 0.0365(2) 0.0447(3) 0.0360(2) -0.0087(2) 0.01053(17) -0.0046(3) N1 0.0182(7) 0.0258(7) 0.0232(7) -0.0010(6) -0.0008(5) -0.0010(6) P1 0.0210(2) 0.0198(2) 0.0237(2) 0.00053(16) -0.00079(16) -0.00082(16) C100 0.0247(9) 0.0300(9) 0.0237(8) 0.0013(7) -0.0030(7) -0.0051(7) C1 0.0256(9) 0.0229(8) 0.0260(8) -0.0015(6) -0.0041(7) -0.0006(7) C2 0.0266(9) 0.0312(9) 0.0322(9) -0.0003(7) -0.0021(8) 0.0019(7) C3 0.0320(10) 0.0400(11) 0.0344(10) -0.0087(8) -0.0071(8) 0.0104(8) C4 0.0495(11) 0.0306(11) 0.0430(10) -0.0063(10) -0.0191(9) 0.0097(11) C5 0.0458(10) 0.0238(8) 0.0525(10) 0.0051(13) -0.0148(8) -0.0042(12) C6 0.0301(9) 0.0276(9) 0.0384(10) 0.0040(8) -0.0049(8) -0.0035(8) C7 0.0214(8) 0.0257(8) 0.0258(8) 0.0025(6) -0.0006(6) -0.0056(7) C8 0.0336(10) 0.0341(10) 0.0302(9) -0.0019(7) -0.0023(8) 0.0014(8) C9 0.0475(12) 0.0502(13) 0.0264(9) -0.0056(9) -0.0001(8) 0.0036(10) C10 0.0455(12) 0.0489(12) 0.0255(9) 0.0074(8) -0.0028(8) -0.0021(10) C11 0.0369(10) 0.0376(14) 0.0355(10) 0.0100(8) -0.0024(8) 0.0038(8) C12 0.0334(8) 0.0290(8) 0.0292(7) 0.0045(10) 0.0026(6) 0.0019(11) C13 0.0189(8) 0.0381(10) 0.0285(9) 0.0089(8) 0.0000(6) -0.0054(8) C14 0.0326(10) 0.0576(14) 0.0300(10) 0.0079(9) -0.0042(8) -0.0099(10) C15 0.0416(13) 0.086(2) 0.0337(12) 0.0222(12) -0.0111(10) -0.0102(13) C16 0.0320(10) 0.080(2) 0.0569(13) 0.0399(16) -0.0064(9) 0.0026(13) C17 0.0292(11) 0.0585(14) 0.0661(16) 0.0226(12) 0.0085(10) 0.0085(10) C18 0.0261(8) 0.0492(13) 0.0392(9) 0.0097(11) 0.0027(7) 0.0012(10) C19 0.0297(10) 0.0405(11) 0.0313(10) 0.0083(8) -0.0014(8) -0.0098(8) C20 0.0341(11) 0.0244(9) 0.0450(12) 0.0052(8) -0.0058(9) 0.0010(8) C21 0.0429(12) 0.0217(9) 0.0360(10) 0.0033(8) 0.0060(9) -0.0020(8) C22 0.0340(11) 0.0297(10) 0.0485(12) 0.0052(8) -0.0020(9) -0.0077(8) C23 0.0584(14) 0.0261(10) 0.0388(11) -0.0062(8) -0.0027(10) -0.0118(9) C24 0.0515(13) 0.0221(10) 0.0514(13) -0.0024(8) 0.0135(11) 0.0028(9) C25 0.0661(17) 0.0673(17) 0.0371(12) -0.0155(11) -0.0266(12) 0.0423(15) C26 0.0324(11) 0.0609(17) 0.0550(14) 0.0170(11) -0.0160(10) -0.0011(9) C27 0.0696(15) 0.0555(14) 0.0360(10) -0.0134(13) -0.0270(10) 0.0232(17) C28 0.0530(15) 0.111(3) 0.0398(14) 0.0369(16) -0.0046(11) 0.0073(18) C29 0.0732(19) 0.0403(14) 0.080(2) 0.0253(14) -0.0491(17) -0.0146(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 N1 2.1927(14) . ? Zr1 C22 2.528(2) . ? Zr1 C26 2.529(2) . ? Zr1 C25 2.532(2) . ? Zr1 C20 2.539(2) . ? Zr1 Cl1 2.5386(5) . ? Zr1 C27 2.5406(18) . ? Zr1 C28 2.547(2) . ? Zr1 C29 2.547(2) . ? Zr1 C21 2.548(2) . ? Zr1 C23 2.562(2) . ? Zr1 C24 2.567(2) . ? N1 C100 1.480(2) . ? N1 P1 1.6323(15) . ? P1 C1 1.8216(18) . ? P1 C7 1.8399(17) . ? C100 C13 1.515(2) . ? C100 C19 1.525(3) . ? C1 C6 1.388(3) . ? C1 C2 1.390(3) . ? C2 C3 1.394(3) . ? C3 C4 1.371(4) . ? C4 C5 1.379(3) . ? C5 C6 1.392(3) . ? C7 C12 1.389(3) . ? C7 C8 1.392(3) . ? C8 C9 1.394(3) . ? C9 C10 1.370(3) . ? C10 C11 1.374(3) . ? C11 C12 1.392(2) . ? C13 C18 1.386(3) . ? C13 C14 1.392(3) . ? C14 C15 1.388(3) . ? C15 C16 1.363(5) . ? C16 C17 1.380(4) . ? C17 C18 1.390(3) . ? C20 C21 1.399(3) . ? C20 C24 1.408(3) . ? C21 C22 1.405(3) . ? C22 C23 1.391(3) . ? C23 C24 1.394(4) . ? C25 C29 1.393(5) . ? C25 C26 1.393(4) . ? C26 C27 1.369(4) . ? C27 C28 1.366(5) . ? C28 C29 1.370(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zr1 C22 126.59(7) . . ? N1 Zr1 C26 127.94(7) . . ? C22 Zr1 C26 74.56(8) . . ? N1 Zr1 C25 96.46(7) . . ? C22 Zr1 C25 98.21(10) . . ? C26 Zr1 C25 31.96(9) . . ? N1 Zr1 C20 91.42(7) . . ? C22 Zr1 C20 52.93(7) . . ? C26 Zr1 C20 127.31(8) . . ? C25 Zr1 C20 147.24(10) . . ? N1 Zr1 Cl1 85.67(4) . . ? C22 Zr1 Cl1 125.10(6) . . ? C26 Zr1 Cl1 123.08(7) . . ? C25 Zr1 Cl1 123.53(8) . . ? C20 Zr1 Cl1 88.67(5) . . ? N1 Zr1 C27 139.88(9) . . ? C22 Zr1 C27 86.59(10) . . ? C26 Zr1 C27 31.33(9) . . ? C25 Zr1 C27 52.27(8) . . ? C20 Zr1 C27 128.63(10) . . ? Cl1 Zr1 C27 92.35(7) . . ? N1 Zr1 C28 111.65(10) . . ? C22 Zr1 C28 117.75(10) . . ? C26 Zr1 C28 51.72(9) . . ? C25 Zr1 C28 51.91(10) . . ? C20 Zr1 C28 150.01(11) . . ? Cl1 Zr1 C28 74.85(7) . . ? C27 Zr1 C28 31.15(11) . . ? N1 Zr1 C29 87.92(8) . . ? C22 Zr1 C29 126.76(9) . . ? C26 Zr1 C29 52.53(9) . . ? C25 Zr1 C29 31.84(11) . . ? C20 Zr1 C29 178.69(12) . . ? Cl1 Zr1 C29 92.40(10) . . ? C27 Zr1 C29 52.08(10) . . ? C28 Zr1 C29 31.21(12) . . ? N1 Zr1 C21 96.15(6) . . ? C22 Zr1 C21 32.14(7) . . ? C26 Zr1 C21 101.95(8) . . ? C25 Zr1 C21 115.39(9) . . ? C20 Zr1 C21 31.92(7) . . ? Cl1 Zr1 C21 120.46(5) . . ? C27 Zr1 C21 118.68(10) . . ? C28 Zr1 C21 149.81(10) . . ? C29 Zr1 C21 147.06(11) . . ? N1 Zr1 C23 143.96(7) . . ? C22 Zr1 C23 31.70(8) . . ? C26 Zr1 C23 81.17(8) . . ? C25 Zr1 C23 112.42(9) . . ? C20 Zr1 C23 52.65(7) . . ? Cl1 Zr1 C23 95.13(6) . . ? C27 Zr1 C23 76.15(10) . . ? C28 Zr1 C23 103.23(11) . . ? C29 Zr1 C23 127.93(9) . . ? C21 Zr1 C23 52.72(7) . . ? N1 Zr1 C24 117.55(7) . . ? C22 Zr1 C24 52.59(8) . . ? C26 Zr1 C24 112.21(8) . . ? C25 Zr1 C24 143.89(9) . . ? C20 Zr1 C24 32.02(7) . . ? Cl1 Zr1 C24 73.83(6) . . ? C27 Zr1 C24 100.08(9) . . ? C28 Zr1 C24 118.06(11) . . ? C29 Zr1 C24 149.15(10) . . ? C21 Zr1 C24 52.80(7) . . ? C23 Zr1 C24 31.55(9) . . ? C100 N1 P1 123.09(12) . . ? C100 N1 Zr1 150.49(12) . . ? P1 N1 Zr1 86.38(6) . . ? N1 P1 C1 112.34(8) . . ? N1 P1 C7 110.66(8) . . ? C1 P1 C7 103.70(8) . . ? N1 P1 Zr1 55.68(5) . . ? C1 P1 Zr1 122.42(6) . . ? C7 P1 Zr1 133.84(6) . . ? N1 C100 C13 112.17(15) . . ? N1 C100 C19 111.43(14) . . ? C13 C100 C19 111.75(16) . . ? C6 C1 C2 118.78(18) . . ? C6 C1 P1 122.62(15) . . ? C2 C1 P1 118.34(14) . . ? C1 C2 C3 120.47(19) . . ? C4 C3 C2 119.7(2) . . ? C3 C4 C5 120.9(2) . . ? C4 C5 C6 119.3(2) . . ? C1 C6 C5 120.8(2) . . ? C12 C7 C8 118.19(16) . . ? C12 C7 P1 118.62(14) . . ? C8 C7 P1 123.14(14) . . ? C7 C8 C9 120.26(19) . . ? C10 C9 C8 120.8(2) . . ? C9 C10 C11 119.56(19) . . ? C10 C11 C12 120.25(19) . . ? C7 C12 C11 120.92(19) . . ? C18 C13 C14 118.95(19) . . ? C18 C13 C100 121.35(17) . . ? C14 C13 C100 119.7(2) . . ? C15 C14 C13 120.3(3) . . ? C16 C15 C14 120.4(2) . . ? C15 C16 C17 119.9(2) . . ? C16 C17 C18 120.4(3) . . ? C13 C18 C17 120.0(2) . . ? C21 C20 C24 108.24(19) . . ? C21 C20 Zr1 74.43(12) . . ? C24 C20 Zr1 75.10(12) . . ? C20 C21 C22 107.3(2) . . ? C20 C21 Zr1 73.65(12) . . ? C22 C21 Zr1 73.14(12) . . ? C23 C22 C21 108.5(2) . . ? C23 C22 Zr1 75.49(12) . . ? C21 C22 Zr1 74.73(12) . . ? C22 C23 C24 108.3(2) . . ? C22 C23 Zr1 72.81(12) . . ? C24 C23 Zr1 74.42(12) . . ? C23 C24 C20 107.7(2) . . ? C23 C24 Zr1 74.03(12) . . ? C20 C24 Zr1 72.89(12) . . ? C29 C25 C26 107.4(2) . . ? C29 C25 Zr1 74.67(14) . . ? C26 C25 Zr1 73.90(13) . . ? C27 C26 C25 108.0(3) . . ? C27 C26 Zr1 74.81(12) . . ? C25 C26 Zr1 74.14(12) . . ? C28 C27 C26 108.1(3) . . ? C28 C27 Zr1 74.67(13) . . ? C26 C27 Zr1 73.86(11) . . ? C27 C28 C29 109.4(3) . . ? C27 C28 Zr1 74.18(14) . . ? C29 C28 Zr1 74.40(14) . . ? C28 C29 C25 107.1(3) . . ? C28 C29 Zr1 74.39(16) . . ? C25 C29 Zr1 73.49(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C22 Zr1 N1 C100 135.5(2) . . . . ? C26 Zr1 N1 C100 -125.4(2) . . . . ? C25 Zr1 N1 C100 -119.2(2) . . . . ? C20 Zr1 N1 C100 92.6(2) . . . . ? Cl1 Zr1 N1 C100 4.0(2) . . . . ? C27 Zr1 N1 C100 -84.5(3) . . . . ? C28 Zr1 N1 C100 -67.8(3) . . . . ? C29 Zr1 N1 C100 -88.5(3) . . . . ? C21 Zr1 N1 C100 124.3(2) . . . . ? C23 Zr1 N1 C100 96.8(3) . . . . ? C24 Zr1 N1 C100 73.3(2) . . . . ? C22 Zr1 N1 P1 -47.40(10) . . . . ? C26 Zr1 N1 P1 51.71(11) . . . . ? C25 Zr1 N1 P1 57.85(10) . . . . ? C20 Zr1 N1 P1 -90.30(8) . . . . ? Cl1 Zr1 N1 P1 -178.86(6) . . . . ? C27 Zr1 N1 P1 92.62(12) . . . . ? C28 Zr1 N1 P1 109.31(10) . . . . ? C29 Zr1 N1 P1 88.57(11) . . . . ? C21 Zr1 N1 P1 -58.65(7) . . . . ? C23 Zr1 N1 P1 -86.08(13) . . . . ? C24 Zr1 N1 P1 -109.62(8) . . . . ? C100 N1 P1 C1 63.38(15) . . . . ? Zr1 N1 P1 C1 -114.91(7) . . . . ? C100 N1 P1 C7 -52.00(16) . . . . ? Zr1 N1 P1 C7 129.71(7) . . . . ? C100 N1 P1 Zr1 178.29(16) . . . . ? C22 Zr1 P1 N1 143.37(8) . . . . ? C26 Zr1 P1 N1 -140.97(9) . . . . ? C25 Zr1 P1 N1 -120.03(11) . . . . ? C20 Zr1 P1 N1 90.64(9) . . . . ? Cl1 Zr1 P1 N1 1.36(7) . . . . ? C27 Zr1 P1 N1 -124.77(12) . . . . ? C28 Zr1 P1 N1 -88.98(11) . . . . ? C29 Zr1 P1 N1 -89.85(10) . . . . ? C21 Zr1 P1 N1 119.16(8) . . . . ? C23 Zr1 P1 N1 132.02(10) . . . . ? C24 Zr1 P1 N1 93.40(10) . . . . ? N1 Zr1 P1 C1 96.41(10) . . . . ? C22 Zr1 P1 C1 -120.22(9) . . . . ? C26 Zr1 P1 C1 -44.56(9) . . . . ? C25 Zr1 P1 C1 -23.62(11) . . . . ? C20 Zr1 P1 C1 -172.96(9) . . . . ? Cl1 Zr1 P1 C1 97.77(7) . . . . ? C27 Zr1 P1 C1 -28.37(13) . . . . ? C28 Zr1 P1 C1 7.43(11) . . . . ? C29 Zr1 P1 C1 6.56(10) . . . . ? C21 Zr1 P1 C1 -144.44(9) . . . . ? C23 Zr1 P1 C1 -131.57(10) . . . . ? C24 Zr1 P1 C1 -170.19(10) . . . . ? N1 Zr1 P1 C7 -86.37(10) . . . . ? C22 Zr1 P1 C7 57.00(9) . . . . ? C26 Zr1 P1 C7 132.66(10) . . . . ? C25 Zr1 P1 C7 153.60(11) . . . . ? C20 Zr1 P1 C7 4.26(9) . . . . ? Cl1 Zr1 P1 C7 -85.01(8) . . . . ? C27 Zr1 P1 C7 148.85(13) . . . . ? C28 Zr1 P1 C7 -175.35(11) . . . . ? C29 Zr1 P1 C7 -176.23(11) . . . . ? C21 Zr1 P1 C7 32.78(9) . . . . ? C23 Zr1 P1 C7 45.65(11) . . . . ? C24 Zr1 P1 C7 7.02(10) . . . . ? P1 N1 C100 C13 95.29(18) . . . . ? Zr1 N1 C100 C13 -88.2(3) . . . . ? P1 N1 C100 C19 -138.57(15) . . . . ? Zr1 N1 C100 C19 38.0(3) . . . . ? N1 P1 C1 C6 -3.91(18) . . . . ? C7 P1 C1 C6 115.61(16) . . . . ? Zr1 P1 C1 C6 -66.45(17) . . . . ? N1 P1 C1 C2 170.08(13) . . . . ? C7 P1 C1 C2 -70.40(15) . . . . ? Zr1 P1 C1 C2 107.54(14) . . . . ? C6 C1 C2 C3 -2.1(3) . . . . ? P1 C1 C2 C3 -176.37(15) . . . . ? C1 C2 C3 C4 1.2(3) . . . . ? C2 C3 C4 C5 0.0(3) . . . . ? C3 C4 C5 C6 -0.3(3) . . . . ? C2 C1 C6 C5 1.9(3) . . . . ? P1 C1 C6 C5 175.87(15) . . . . ? C4 C5 C6 C1 -0.7(3) . . . . ? N1 P1 C7 C12 -46.63(17) . . . . ? C1 P1 C7 C12 -167.29(15) . . . . ? Zr1 P1 C7 C12 15.13(19) . . . . ? N1 P1 C7 C8 130.68(16) . . . . ? C1 P1 C7 C8 10.02(17) . . . . ? Zr1 P1 C7 C8 -167.57(12) . . . . ? C12 C7 C8 C9 -0.5(3) . . . . ? P1 C7 C8 C9 -177.81(16) . . . . ? C7 C8 C9 C10 1.1(3) . . . . ? C8 C9 C10 C11 -0.8(4) . . . . ? C9 C10 C11 C12 -0.1(3) . . . . ? C8 C7 C12 C11 -0.4(3) . . . . ? P1 C7 C12 C11 177.00(15) . . . . ? C10 C11 C12 C7 0.8(3) . . . . ? N1 C100 C13 C18 64.0(2) . . . . ? C19 C100 C13 C18 -62.0(2) . . . . ? N1 C100 C13 C14 -116.4(2) . . . . ? C19 C100 C13 C14 117.7(2) . . . . ? C18 C13 C14 C15 0.9(3) . . . . ? C100 C13 C14 C15 -178.77(19) . . . . ? C13 C14 C15 C16 -0.6(4) . . . . ? C14 C15 C16 C17 0.3(4) . . . . ? C15 C16 C17 C18 -0.4(4) . . . . ? C14 C13 C18 C17 -1.0(3) . . . . ? C100 C13 C18 C17 178.7(2) . . . . ? C16 C17 C18 C13 0.7(3) . . . . ? N1 Zr1 C20 C21 99.36(13) . . . . ? C22 Zr1 C20 C21 -37.40(13) . . . . ? C26 Zr1 C20 C21 -43.02(17) . . . . ? C25 Zr1 C20 C21 -4.9(2) . . . . ? Cl1 Zr1 C20 C21 -175.00(12) . . . . ? C27 Zr1 C20 C21 -83.05(16) . . . . ? C28 Zr1 C20 C21 -119.3(2) . . . . ? C29 Zr1 C20 C21 39(4) . . . . ? C23 Zr1 C20 C21 -77.51(14) . . . . ? C24 Zr1 C20 C21 -114.23(19) . . . . ? N1 Zr1 C20 C24 -146.41(14) . . . . ? C22 Zr1 C20 C24 76.82(15) . . . . ? C26 Zr1 C20 C24 71.21(17) . . . . ? C25 Zr1 C20 C24 109.31(18) . . . . ? Cl1 Zr1 C20 C24 -60.77(13) . . . . ? C27 Zr1 C20 C24 31.18(18) . . . . ? C28 Zr1 C20 C24 -5.0(2) . . . . ? C29 Zr1 C20 C24 154(4) . . . . ? C21 Zr1 C20 C24 114.23(19) . . . . ? C23 Zr1 C20 C24 36.71(15) . . . . ? C24 C20 C21 C22 -2.2(2) . . . . ? Zr1 C20 C21 C22 65.93(14) . . . . ? C24 C20 C21 Zr1 -68.10(15) . . . . ? N1 Zr1 C21 C20 -82.78(13) . . . . ? C22 Zr1 C21 C20 114.34(19) . . . . ? C26 Zr1 C21 C20 146.31(13) . . . . ? C25 Zr1 C21 C20 177.06(12) . . . . ? Cl1 Zr1 C21 C20 5.80(14) . . . . ? C27 Zr1 C21 C20 117.89(13) . . . . ? C28 Zr1 C21 C20 119.9(2) . . . . ? C29 Zr1 C21 C20 -178.47(17) . . . . ? C23 Zr1 C21 C20 77.31(14) . . . . ? C24 Zr1 C21 C20 37.37(13) . . . . ? N1 Zr1 C21 C22 162.88(13) . . . . ? C26 Zr1 C21 C22 31.97(15) . . . . ? C25 Zr1 C21 C22 62.71(15) . . . . ? C20 Zr1 C21 C22 -114.34(19) . . . . ? Cl1 Zr1 C21 C22 -108.54(13) . . . . ? C27 Zr1 C21 C22 3.54(16) . . . . ? C28 Zr1 C21 C22 5.5(3) . . . . ? C29 Zr1 C21 C22 67.2(2) . . . . ? C23 Zr1 C21 C22 -37.04(14) . . . . ? C24 Zr1 C21 C22 -76.97(15) . . . . ? C20 C21 C22 C23 2.3(2) . . . . ? Zr1 C21 C22 C23 68.58(15) . . . . ? C20 C21 C22 Zr1 -66.28(14) . . . . ? N1 Zr1 C22 C23 -135.60(13) . . . . ? C26 Zr1 C22 C23 98.29(15) . . . . ? C25 Zr1 C22 C23 120.00(14) . . . . ? C20 Zr1 C22 C23 -77.08(15) . . . . ? Cl1 Zr1 C22 C23 -21.59(16) . . . . ? C27 Zr1 C22 C23 68.90(15) . . . . ? C28 Zr1 C22 C23 68.93(17) . . . . ? C29 Zr1 C22 C23 104.51(18) . . . . ? C21 Zr1 C22 C23 -114.2(2) . . . . ? C24 Zr1 C22 C23 -36.54(14) . . . . ? N1 Zr1 C22 C21 -21.38(16) . . . . ? C26 Zr1 C22 C21 -147.50(15) . . . . ? C25 Zr1 C22 C21 -125.79(13) . . . . ? C20 Zr1 C22 C21 37.14(12) . . . . ? Cl1 Zr1 C22 C21 92.63(13) . . . . ? C27 Zr1 C22 C21 -176.89(14) . . . . ? C28 Zr1 C22 C21 -176.86(15) . . . . ? C29 Zr1 C22 C21 -141.28(16) . . . . ? C23 Zr1 C22 C21 114.2(2) . . . . ? C24 Zr1 C22 C21 77.67(14) . . . . ? C21 C22 C23 C24 -1.6(2) . . . . ? Zr1 C22 C23 C24 66.52(15) . . . . ? C21 C22 C23 Zr1 -68.07(14) . . . . ? N1 Zr1 C23 C22 72.71(19) . . . . ? C26 Zr1 C23 C22 -74.86(15) . . . . ? C25 Zr1 C23 C22 -68.02(15) . . . . ? C20 Zr1 C23 C22 78.02(14) . . . . ? Cl1 Zr1 C23 C22 162.41(13) . . . . ? C27 Zr1 C23 C22 -106.43(15) . . . . ? C28 Zr1 C23 C22 -121.97(14) . . . . ? C29 Zr1 C23 C22 -100.50(18) . . . . ? C21 Zr1 C23 C22 37.57(13) . . . . ? C24 Zr1 C23 C22 115.3(2) . . . . ? N1 Zr1 C23 C24 -42.6(2) . . . . ? C22 Zr1 C23 C24 -115.3(2) . . . . ? C26 Zr1 C23 C24 169.83(16) . . . . ? C25 Zr1 C23 C24 176.67(15) . . . . ? C20 Zr1 C23 C24 -37.29(14) . . . . ? Cl1 Zr1 C23 C24 47.10(14) . . . . ? C27 Zr1 C23 C24 138.26(16) . . . . ? C28 Zr1 C23 C24 122.72(16) . . . . ? C29 Zr1 C23 C24 144.19(17) . . . . ? C21 Zr1 C23 C24 -77.74(15) . . . . ? C22 C23 C24 C20 0.2(2) . . . . ? Zr1 C23 C24 C20 65.65(15) . . . . ? C22 C23 C24 Zr1 -65.45(15) . . . . ? C21 C20 C24 C23 1.2(2) . . . . ? Zr1 C20 C24 C23 -66.42(15) . . . . ? C21 C20 C24 Zr1 67.66(14) . . . . ? N1 Zr1 C24 C23 153.31(13) . . . . ? C22 Zr1 C24 C23 36.73(14) . . . . ? C26 Zr1 C24 C23 -10.86(17) . . . . ? C25 Zr1 C24 C23 -5.2(2) . . . . ? C20 Zr1 C24 C23 114.7(2) . . . . ? Cl1 Zr1 C24 C23 -130.57(15) . . . . ? C27 Zr1 C24 C23 -41.03(16) . . . . ? C28 Zr1 C24 C23 -68.13(17) . . . . ? C29 Zr1 C24 C23 -64.2(2) . . . . ? C21 Zr1 C24 C23 77.46(16) . . . . ? N1 Zr1 C24 C20 38.60(16) . . . . ? C22 Zr1 C24 C20 -77.98(15) . . . . ? C26 Zr1 C24 C20 -125.58(14) . . . . ? C25 Zr1 C24 C20 -119.94(17) . . . . ? Cl1 Zr1 C24 C20 114.72(14) . . . . ? C27 Zr1 C24 C20 -155.75(15) . . . . ? C28 Zr1 C24 C20 177.15(14) . . . . ? C29 Zr1 C24 C20 -178.87(19) . . . . ? C21 Zr1 C24 C20 -37.25(13) . . . . ? C23 Zr1 C24 C20 -114.7(2) . . . . ? N1 Zr1 C25 C29 75.43(17) . . . . ? C22 Zr1 C25 C29 -156.07(17) . . . . ? C26 Zr1 C25 C29 -113.7(2) . . . . ? C20 Zr1 C25 C29 178.27(18) . . . . ? Cl1 Zr1 C25 C29 -13.65(19) . . . . ? C27 Zr1 C25 C29 -76.88(19) . . . . ? C28 Zr1 C25 C29 -37.08(18) . . . . ? C21 Zr1 C25 C29 175.39(17) . . . . ? C23 Zr1 C25 C29 -126.58(18) . . . . ? C24 Zr1 C25 C29 -123.6(2) . . . . ? N1 Zr1 C25 C26 -170.83(17) . . . . ? C22 Zr1 C25 C26 -42.34(18) . . . . ? C20 Zr1 C25 C26 -68.0(2) . . . . ? Cl1 Zr1 C25 C26 100.08(18) . . . . ? C27 Zr1 C25 C26 36.86(17) . . . . ? C28 Zr1 C25 C26 76.65(19) . . . . ? C29 Zr1 C25 C26 113.7(2) . . . . ? C21 Zr1 C25 C26 -70.87(18) . . . . ? C23 Zr1 C25 C26 -12.8(2) . . . . ? C24 Zr1 C25 C26 -9.9(3) . . . . ? C29 C25 C26 C27 0.0(2) . . . . ? Zr1 C25 C26 C27 -67.76(16) . . . . ? C29 C25 C26 Zr1 67.72(16) . . . . ? N1 Zr1 C26 C27 125.75(19) . . . . ? C22 Zr1 C26 C27 -109.59(19) . . . . ? C25 Zr1 C26 C27 114.2(3) . . . . ? C20 Zr1 C26 C27 -104.94(19) . . . . ? Cl1 Zr1 C26 C27 12.6(2) . . . . ? C28 Zr1 C26 C27 36.9(2) . . . . ? C29 Zr1 C26 C27 76.7(2) . . . . ? C21 Zr1 C26 C27 -126.57(19) . . . . ? C23 Zr1 C26 C27 -77.83(19) . . . . ? C24 Zr1 C26 C27 -72.1(2) . . . . ? N1 Zr1 C26 C25 11.6(2) . . . . ? C22 Zr1 C26 C25 136.25(19) . . . . ? C20 Zr1 C26 C25 140.89(17) . . . . ? Cl1 Zr1 C26 C25 -101.61(18) . . . . ? C27 Zr1 C26 C25 -114.2(3) . . . . ? C28 Zr1 C26 C25 -77.3(2) . . . . ? C29 Zr1 C26 C25 -37.47(18) . . . . ? C21 Zr1 C26 C25 119.26(17) . . . . ? C23 Zr1 C26 C25 168.00(19) . . . . ? C24 Zr1 C26 C25 173.72(17) . . . . ? C25 C26 C27 C28 -0.1(3) . . . . ? Zr1 C26 C27 C28 -67.42(16) . . . . ? C25 C26 C27 Zr1 67.31(15) . . . . ? N1 Zr1 C27 C28 31.1(2) . . . . ? C22 Zr1 C27 C28 180.0(2) . . . . ? C26 Zr1 C27 C28 114.5(3) . . . . ? C25 Zr1 C27 C28 76.8(2) . . . . ? C20 Zr1 C27 C28 -145.2(2) . . . . ? Cl1 Zr1 C27 C28 -55.0(2) . . . . ? C29 Zr1 C27 C28 36.2(2) . . . . ? C21 Zr1 C27 C28 178.06(19) . . . . ? C23 Zr1 C27 C28 -149.7(2) . . . . ? C24 Zr1 C27 C28 -129.0(2) . . . . ? N1 Zr1 C27 C26 -83.4(2) . . . . ? C22 Zr1 C27 C26 65.47(18) . . . . ? C25 Zr1 C27 C26 -37.64(17) . . . . ? C20 Zr1 C27 C26 100.33(18) . . . . ? Cl1 Zr1 C27 C26 -169.49(17) . . . . ? C28 Zr1 C27 C26 -114.5(3) . . . . ? C29 Zr1 C27 C26 -78.3(2) . . . . ? C21 Zr1 C27 C26 63.6(2) . . . . ? C23 Zr1 C27 C26 95.80(19) . . . . ? C24 Zr1 C27 C26 116.51(18) . . . . ? C26 C27 C28 C29 0.2(3) . . . . ? Zr1 C27 C28 C29 -66.66(18) . . . . ? C26 C27 C28 Zr1 66.88(16) . . . . ? N1 Zr1 C28 C27 -159.04(18) . . . . ? C22 Zr1 C28 C27 -0.1(2) . . . . ? C26 Zr1 C28 C27 -37.08(16) . . . . ? C25 Zr1 C28 C27 -78.1(2) . . . . ? C20 Zr1 C28 C27 63.1(3) . . . . ? Cl1 Zr1 C28 C27 122.0(2) . . . . ? C29 Zr1 C28 C27 -116.0(3) . . . . ? C21 Zr1 C28 C27 -3.4(3) . . . . ? C23 Zr1 C28 C27 30.2(2) . . . . ? C24 Zr1 C28 C27 60.1(2) . . . . ? N1 Zr1 C28 C29 -43.1(2) . . . . ? C22 Zr1 C28 C29 115.9(2) . . . . ? C26 Zr1 C28 C29 78.9(2) . . . . ? C25 Zr1 C28 C29 37.87(18) . . . . ? C20 Zr1 C28 C29 179.08(18) . . . . ? Cl1 Zr1 C28 C29 -122.0(2) . . . . ? C27 Zr1 C28 C29 116.0(3) . . . . ? C21 Zr1 C28 C29 112.6(3) . . . . ? C23 Zr1 C28 C29 146.14(19) . . . . ? C24 Zr1 C28 C29 176.06(18) . . . . ? C27 C28 C29 C25 -0.2(3) . . . . ? Zr1 C28 C29 C25 -66.75(16) . . . . ? C27 C28 C29 Zr1 66.52(19) . . . . ? C26 C25 C29 C28 0.2(3) . . . . ? Zr1 C25 C29 C28 67.36(18) . . . . ? C26 C25 C29 Zr1 -67.20(15) . . . . ? N1 Zr1 C29 C28 140.6(2) . . . . ? C22 Zr1 C29 C28 -83.6(2) . . . . ? C26 Zr1 C29 C28 -76.04(19) . . . . ? C25 Zr1 C29 C28 -113.7(2) . . . . ? C20 Zr1 C29 C28 -159(4) . . . . ? Cl1 Zr1 C29 C28 54.97(19) . . . . ? C27 Zr1 C29 C28 -36.13(17) . . . . ? C21 Zr1 C29 C28 -121.3(2) . . . . ? C23 Zr1 C29 C28 -43.4(3) . . . . ? C24 Zr1 C29 C28 -6.8(3) . . . . ? N1 Zr1 C29 C25 -105.78(17) . . . . ? C22 Zr1 C29 C25 30.1(2) . . . . ? C26 Zr1 C29 C25 37.63(15) . . . . ? C20 Zr1 C29 C25 -46(4) . . . . ? Cl1 Zr1 C29 C25 168.64(16) . . . . ? C27 Zr1 C29 C25 77.53(16) . . . . ? C28 Zr1 C29 C25 113.7(2) . . . . ? C21 Zr1 C29 C25 -7.7(3) . . . . ? C23 Zr1 C29 C25 70.2(2) . . . . ? C24 Zr1 C29 C25 106.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.704 _diffrn_reflns_theta_full 31.54 _diffrn_measured_fraction_theta_full 0.704 _refine_diff_density_max 0.336 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.043 #============================================================================== data_4b _database_code_depnum_ccdc_archive 'CCDC 265444' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H29 Cl N P Zr' _chemical_formula_sum 'C30 H29 Cl N P Zr' _chemical_formula_weight 561.18 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.7121(17) _cell_length_b 10.833(2) _cell_length_c 13.593(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.471(4) _cell_angle_gamma 90.00 _cell_volume 1279.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour colorless _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 0.616 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.697 _exptl_absorpt_correction_T_max 0.806 _exptl_absorpt_process_details 'SADABS - Bruker/Siemens' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart 1000 CCD' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15936 _diffrn_reflns_av_R_equivalents 0.0118 _diffrn_reflns_av_sigmaI/netI 0.0190 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 30.56 _reflns_number_total 7689 _reflns_number_gt 7480 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+0.1251P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.004(15) _refine_ls_number_reflns 7689 _refine_ls_number_parameters 308 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0176 _refine_ls_R_factor_gt 0.0167 _refine_ls_wR_factor_ref 0.0443 _refine_ls_wR_factor_gt 0.0440 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.699874(11) 1.737881(10) 0.879450(7) 0.01964(3) Uani 1 1 d . . . Cl1 Cl 0.45508(4) 1.75034(4) 0.96998(2) 0.03265(7) Uani 1 1 d . . . N1 N 0.56735(11) 1.61368(10) 0.77696(7) 0.01974(17) Uani 1 1 d . . . P1 P 0.72256(3) 1.60721(3) 0.71628(2) 0.01870(5) Uani 1 1 d . . . C100 C 0.42522(14) 1.54365(11) 0.74724(9) 0.0221(2) Uani 1 1 d . . . H100 H 0.4555 1.4729 0.7057 0.027 Uiso 1 1 calc R . . C1 C 0.80620(14) 1.45320(11) 0.71774(9) 0.0213(2) Uani 1 1 d . . . C2 C 0.95143(15) 1.43792(12) 0.68212(9) 0.0262(2) Uani 1 1 d . . . H2 H 1.0009 1.5063 0.6543 0.031 Uiso 1 1 calc R . . C3 C 1.02406(16) 1.32325(14) 0.68716(10) 0.0314(3) Uani 1 1 d . . . H3 H 1.1219 1.3132 0.6618 0.038 Uiso 1 1 calc R . . C4 C 0.95367(18) 1.22417(15) 0.72911(10) 0.0361(3) Uani 1 1 d . . . H4 H 1.0029 1.1459 0.7321 0.043 Uiso 1 1 calc R . . C5 C 0.81123(15) 1.23851(18) 0.76695(10) 0.0356(2) Uani 1 1 d . . . H5 H 0.7637 1.1704 0.7964 0.043 Uiso 1 1 calc R . . C6 C 0.73815(16) 1.35293(12) 0.76167(10) 0.0276(2) Uani 1 1 d . . . H6 H 0.6412 1.3627 0.7882 0.033 Uiso 1 1 calc R . . C7 C 0.67504(13) 1.63777(11) 0.58424(8) 0.0212(2) Uani 1 1 d . . . C8 C 0.72344(15) 1.56251(13) 0.50916(9) 0.0278(2) Uani 1 1 d . . . H8 H 0.7875 1.4933 0.5254 0.033 Uiso 1 1 calc R . . C9 C 0.67829(18) 1.58824(15) 0.41049(10) 0.0351(3) Uani 1 1 d . . . H9 H 0.7131 1.5370 0.3601 0.042 Uiso 1 1 calc R . . C10 C 0.58375(18) 1.68735(15) 0.38539(10) 0.0342(3) Uani 1 1 d . . . H10 H 0.5528 1.7039 0.3181 0.041 Uiso 1 1 calc R . . C11 C 0.53447(16) 1.76239(12) 0.45890(10) 0.0314(3) Uani 1 1 d . . . H11 H 0.4690 1.8306 0.4421 0.038 Uiso 1 1 calc R . . C12 C 0.58043(13) 1.73847(16) 0.55746(8) 0.02609(19) Uani 1 1 d . . . H12 H 0.5470 1.7914 0.6073 0.031 Uiso 1 1 calc R . . C13 C 0.30937(13) 1.62026(13) 0.68442(9) 0.0247(2) Uani 1 1 d . . . C14 C 0.26815(17) 1.58491(16) 0.58687(10) 0.0339(3) Uani 1 1 d . . . H14 H 0.3137 1.5139 0.5602 0.041 Uiso 1 1 calc R . . C15 C 0.16024(19) 1.65381(19) 0.52873(12) 0.0456(4) Uani 1 1 d . . . H15 H 0.1331 1.6295 0.4625 0.055 Uiso 1 1 calc R . . C16 C 0.09322(17) 1.7560(2) 0.56616(12) 0.0481(5) Uani 1 1 d . . . H16 H 0.0195 1.8022 0.5262 0.058 Uiso 1 1 calc R . . C17 C 0.13344(18) 1.79187(17) 0.66270(14) 0.0439(4) Uani 1 1 d . . . H17 H 0.0871 1.8629 0.6887 0.053 Uiso 1 1 calc R . . C18 C 0.24145(14) 1.72453(17) 0.72190(10) 0.0322(3) Uani 1 1 d . . . H18 H 0.2686 1.7499 0.7879 0.039 Uiso 1 1 calc R . . C19 C 0.35361(16) 1.48881(14) 0.83699(10) 0.0292(3) Uani 1 1 d . . . H19A H 0.4309 1.4394 0.8757 0.044 Uiso 1 1 calc R . . H19B H 0.2662 1.4362 0.8146 0.044 Uiso 1 1 calc R . . H19C H 0.3180 1.5557 0.8780 0.044 Uiso 1 1 calc R . . C20 C 0.60706(16) 1.92586(12) 0.77966(11) 0.0296(3) Uani 1 1 d . . . H20 H 0.5135 1.9175 0.7395 0.035 Uiso 1 1 calc R . . C21 C 0.75551(17) 1.90008(12) 0.75101(10) 0.0281(3) Uani 1 1 d . . . H21 H 0.7802 1.8734 0.6876 0.034 Uiso 1 1 calc R . . C22 C 0.86099(17) 1.92091(13) 0.83341(11) 0.0319(3) Uani 1 1 d . . . H22 H 0.9691 1.9084 0.8359 0.038 Uiso 1 1 calc R . . C23 C 0.7778(2) 1.96349(13) 0.91128(11) 0.0352(3) Uani 1 1 d . . . H23 H 0.8205 1.9864 0.9751 0.042 Uiso 1 1 calc R . . C24 C 0.6218(2) 1.96644(13) 0.87885(12) 0.0356(3) Uani 1 1 d . . . H24 H 0.5400 1.9913 0.9167 0.043 Uiso 1 1 calc R . . C25 C 0.9183(2) 1.58873(18) 0.92528(12) 0.0491(5) Uani 1 1 d . . . H25 H 0.9623 1.5470 0.8728 0.059 Uiso 1 1 calc R . . C26 C 0.96575(18) 1.70247(16) 0.96560(13) 0.0418(4) Uani 1 1 d . . . H26 H 1.0479 1.7518 0.9456 0.050 Uiso 1 1 calc R . . C27 C 0.87157(19) 1.7304(2) 1.03989(10) 0.0456(4) Uani 1 1 d . . . H27 H 0.8776 1.8026 1.0797 0.055 Uiso 1 1 calc R . . C28 C 0.7675(2) 1.6353(2) 1.04631(13) 0.0570(6) Uani 1 1 d . . . H28 H 0.6900 1.6310 1.0916 0.068 Uiso 1 1 calc R . . C29 C 0.7944(3) 1.54731(17) 0.97593(16) 0.0572(6) Uani 1 1 d . . . H29 H 0.7390 1.4725 0.9642 0.069 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 0.02041(5) 0.01872(4) 0.01934(4) -0.00090(4) -0.00133(3) -0.00086(5) Cl1 0.03246(14) 0.03635(19) 0.03028(13) -0.00711(14) 0.00974(10) -0.00380(15) N1 0.0185(4) 0.0206(4) 0.0199(4) -0.0010(4) 0.0003(3) -0.0014(4) P1 0.01918(13) 0.01675(13) 0.01998(13) 0.00036(10) 0.00031(10) -0.00066(10) C100 0.0216(5) 0.0236(5) 0.0206(5) 0.0014(4) -0.0017(4) -0.0035(4) C1 0.0227(5) 0.0189(5) 0.0217(5) -0.0015(4) -0.0026(4) 0.0005(4) C2 0.0249(6) 0.0271(6) 0.0263(6) -0.0014(4) -0.0009(5) 0.0022(5) C3 0.0292(6) 0.0337(7) 0.0301(6) -0.0081(5) -0.0052(5) 0.0099(5) C4 0.0447(7) 0.0244(7) 0.0366(6) -0.0049(6) -0.0142(5) 0.0087(6) C5 0.0405(6) 0.0205(5) 0.0439(6) 0.0065(8) -0.0096(5) -0.0017(8) C6 0.0270(6) 0.0223(6) 0.0327(6) 0.0043(5) -0.0030(5) -0.0015(5) C7 0.0211(5) 0.0216(5) 0.0208(5) 0.0020(4) 0.0011(4) -0.0037(4) C8 0.0293(6) 0.0292(6) 0.0244(5) -0.0024(5) -0.0013(5) 0.0026(5) C9 0.0399(7) 0.0423(8) 0.0227(6) -0.0050(5) 0.0003(5) 0.0023(6) C10 0.0388(7) 0.0411(7) 0.0221(6) 0.0068(5) -0.0018(5) -0.0003(6) C11 0.0331(6) 0.0309(8) 0.0297(6) 0.0088(5) -0.0009(5) 0.0017(5) C12 0.0284(5) 0.0241(5) 0.0259(5) 0.0044(6) 0.0024(4) 0.0014(7) C13 0.0178(5) 0.0328(6) 0.0231(5) 0.0074(5) 0.0000(4) -0.0046(5) C14 0.0292(6) 0.0470(8) 0.0249(6) 0.0059(6) -0.0023(5) -0.0076(6) C15 0.0360(8) 0.0709(12) 0.0282(7) 0.0177(7) -0.0090(6) -0.0106(8) C16 0.0284(6) 0.0676(14) 0.0470(8) 0.0320(9) -0.0044(6) 0.0017(8) C17 0.0286(7) 0.0492(9) 0.0546(10) 0.0183(8) 0.0070(7) 0.0081(6) C18 0.0253(5) 0.0383(8) 0.0333(6) 0.0071(6) 0.0032(4) 0.0022(6) C19 0.0264(6) 0.0352(7) 0.0256(6) 0.0082(5) -0.0009(5) -0.0088(5) C20 0.0309(6) 0.0202(6) 0.0367(7) 0.0036(5) -0.0031(5) 0.0007(5) C21 0.0369(7) 0.0186(5) 0.0289(6) 0.0015(5) 0.0040(5) -0.0025(5) C22 0.0300(6) 0.0259(6) 0.0392(7) 0.0041(5) -0.0002(5) -0.0067(5) C23 0.0508(9) 0.0226(6) 0.0314(7) -0.0041(5) -0.0010(6) -0.0092(6) C24 0.0462(8) 0.0194(6) 0.0424(8) -0.0022(5) 0.0115(6) 0.0022(5) C25 0.0571(10) 0.0533(10) 0.0329(7) -0.0128(7) -0.0222(7) 0.0328(9) C26 0.0273(7) 0.0487(9) 0.0469(8) 0.0122(6) -0.0127(6) -0.0006(6) C27 0.0576(9) 0.0453(8) 0.0299(6) -0.0117(8) -0.0208(6) 0.0193(10) C28 0.0444(9) 0.0919(16) 0.0334(8) 0.0302(9) -0.0048(7) 0.0035(10) C29 0.0644(12) 0.0322(8) 0.0677(12) 0.0193(8) -0.0413(10) -0.0107(8) _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 N1 2.1985(10) . ? Zr1 C22 2.5359(14) . ? Zr1 C25 2.5367(16) . ? Zr1 C26 2.5419(15) . ? Zr1 C20 2.5436(14) . ? Zr1 Cl1 2.5475(5) . ? Zr1 C27 2.5479(13) . ? Zr1 C29 2.5480(17) . ? Zr1 C21 2.5500(13) . ? Zr1 C28 2.5530(16) . ? Zr1 C23 2.5644(14) . ? Zr1 C24 2.5677(14) . ? N1 C100 1.4812(15) . ? N1 P1 1.6394(10) . ? P1 C1 1.8202(12) . ? P1 C7 1.8402(12) . ? C100 C13 1.5173(17) . ? C100 C19 1.5327(17) . ? C1 C6 1.3939(17) . ? C1 C2 1.3994(17) . ? C2 C3 1.3934(18) . ? C3 C4 1.381(2) . ? C4 C5 1.389(2) . ? C5 C6 1.393(2) . ? C7 C8 1.3967(17) . ? C7 C12 1.3983(19) . ? C8 C9 1.3961(19) . ? C9 C10 1.380(2) . ? C10 C11 1.382(2) . ? C11 C12 1.3924(17) . ? C13 C18 1.390(2) . ? C13 C14 1.3999(19) . ? C14 C15 1.396(2) . ? C15 C16 1.368(3) . ? C16 C17 1.387(3) . ? C17 C18 1.395(2) . ? C20 C21 1.407(2) . ? C20 C24 1.414(2) . ? C21 C22 1.411(2) . ? C22 C23 1.406(2) . ? C23 C24 1.396(3) . ? C25 C26 1.398(3) . ? C25 C29 1.399(3) . ? C26 C27 1.383(2) . ? C27 C28 1.380(3) . ? C28 C29 1.384(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zr1 C22 126.56(4) . . ? N1 Zr1 C25 96.46(5) . . ? C22 Zr1 C25 98.03(7) . . ? N1 Zr1 C26 127.90(5) . . ? C22 Zr1 C26 74.32(5) . . ? C25 Zr1 C26 31.96(6) . . ? N1 Zr1 C20 91.30(5) . . ? C22 Zr1 C20 53.23(5) . . ? C25 Zr1 C20 147.36(6) . . ? C26 Zr1 C20 127.37(5) . . ? N1 Zr1 Cl1 85.44(3) . . ? C22 Zr1 Cl1 125.32(4) . . ? C25 Zr1 Cl1 123.73(5) . . ? C26 Zr1 Cl1 123.54(4) . . ? C20 Zr1 Cl1 88.39(4) . . ? N1 Zr1 C27 140.09(6) . . ? C22 Zr1 C27 86.38(6) . . ? C25 Zr1 C27 52.44(5) . . ? C26 Zr1 C27 31.54(6) . . ? C20 Zr1 C27 128.54(6) . . ? Cl1 Zr1 C27 92.63(4) . . ? N1 Zr1 C29 87.88(5) . . ? C22 Zr1 C29 126.70(6) . . ? C25 Zr1 C29 31.93(7) . . ? C26 Zr1 C29 52.71(6) . . ? C20 Zr1 C29 178.74(7) . . ? Cl1 Zr1 C29 92.49(6) . . ? C27 Zr1 C29 52.33(7) . . ? N1 Zr1 C21 96.10(4) . . ? C22 Zr1 C21 32.20(5) . . ? C25 Zr1 C21 115.35(6) . . ? C26 Zr1 C21 101.79(5) . . ? C20 Zr1 C21 32.08(4) . . ? Cl1 Zr1 C21 120.34(3) . . ? C27 Zr1 C21 118.54(6) . . ? C29 Zr1 C21 147.10(7) . . ? N1 Zr1 C28 111.71(6) . . ? C22 Zr1 C28 117.77(6) . . ? C25 Zr1 C28 52.26(7) . . ? C26 Zr1 C28 52.14(6) . . ? C20 Zr1 C28 149.77(7) . . ? Cl1 Zr1 C28 74.79(5) . . ? C27 Zr1 C28 31.38(7) . . ? C29 Zr1 C28 31.48(8) . . ? C21 Zr1 C28 149.91(6) . . ? N1 Zr1 C23 144.03(5) . . ? C22 Zr1 C23 32.01(5) . . ? C25 Zr1 C23 112.46(6) . . ? C26 Zr1 C23 81.16(6) . . ? C20 Zr1 C23 52.84(5) . . ? Cl1 Zr1 C23 95.08(4) . . ? C27 Zr1 C23 75.88(6) . . ? C29 Zr1 C23 127.93(6) . . ? C21 Zr1 C23 52.90(5) . . ? C28 Zr1 C23 103.02(7) . . ? N1 Zr1 C24 117.53(5) . . ? C22 Zr1 C24 52.90(5) . . ? C25 Zr1 C24 143.95(6) . . ? C26 Zr1 C24 112.25(6) . . ? C20 Zr1 C24 32.12(5) . . ? Cl1 Zr1 C24 73.67(4) . . ? C27 Zr1 C24 99.86(6) . . ? C29 Zr1 C24 149.09(7) . . ? C21 Zr1 C24 52.97(5) . . ? C28 Zr1 C24 117.73(7) . . ? C23 Zr1 C24 31.58(6) . . ? C100 N1 P1 123.07(8) . . ? C100 N1 Zr1 150.79(8) . . ? P1 N1 Zr1 86.10(4) . . ? N1 P1 C1 112.26(6) . . ? N1 P1 C7 110.57(5) . . ? C1 P1 C7 103.59(5) . . ? N1 P1 Zr1 55.81(4) . . ? C1 P1 Zr1 122.42(4) . . ? C7 P1 Zr1 133.95(4) . . ? N1 C100 C13 112.25(10) . . ? N1 C100 C19 111.40(10) . . ? C13 C100 C19 111.45(10) . . ? C6 C1 C2 118.84(12) . . ? C6 C1 P1 122.39(10) . . ? C2 C1 P1 118.46(9) . . ? C3 C2 C1 120.51(13) . . ? C4 C3 C2 119.91(13) . . ? C3 C4 C5 120.29(15) . . ? C4 C5 C6 119.91(15) . . ? C5 C6 C1 120.51(13) . . ? C8 C7 C12 118.08(11) . . ? C8 C7 P1 123.35(9) . . ? C12 C7 P1 118.51(9) . . ? C9 C8 C7 120.46(13) . . ? C10 C9 C8 120.73(13) . . ? C9 C10 C11 119.47(13) . . ? C10 C11 C12 120.25(13) . . ? C11 C12 C7 121.01(12) . . ? C18 C13 C14 118.96(13) . . ? C18 C13 C100 121.45(11) . . ? C14 C13 C100 119.58(13) . . ? C15 C14 C13 120.11(16) . . ? C16 C15 C14 120.67(16) . . ? C15 C16 C17 119.65(15) . . ? C16 C17 C18 120.56(17) . . ? C13 C18 C17 120.05(14) . . ? C21 C20 C24 107.97(13) . . ? C21 C20 Zr1 74.21(8) . . ? C24 C20 Zr1 74.87(8) . . ? C20 C21 C22 107.72(13) . . ? C20 C21 Zr1 73.71(8) . . ? C22 C21 Zr1 73.35(8) . . ? C23 C22 C21 107.95(13) . . ? C23 C22 Zr1 75.12(8) . . ? C21 C22 Zr1 74.45(8) . . ? C24 C23 C22 108.41(13) . . ? C24 C23 Zr1 74.34(8) . . ? C22 C23 Zr1 72.88(8) . . ? C23 C24 C20 107.92(13) . . ? C23 C24 Zr1 74.09(8) . . ? C20 C24 Zr1 73.00(8) . . ? C26 C25 C29 107.81(16) . . ? C26 C25 Zr1 74.23(9) . . ? C29 C25 Zr1 74.48(10) . . ? C27 C26 C25 107.73(17) . . ? C27 C26 Zr1 74.47(8) . . ? C25 C26 Zr1 73.82(9) . . ? C28 C27 C26 108.27(18) . . ? C28 C27 Zr1 74.51(9) . . ? C26 C27 Zr1 73.99(8) . . ? C27 C28 C29 108.83(17) . . ? C27 C28 Zr1 74.11(9) . . ? C29 C28 Zr1 74.06(10) . . ? C28 C29 C25 107.36(16) . . ? C28 C29 Zr1 74.46(10) . . ? C25 C29 Zr1 73.59(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C22 Zr1 N1 C100 -135.65(16) . . . . ? C25 Zr1 N1 C100 119.34(17) . . . . ? C26 Zr1 N1 C100 125.68(16) . . . . ? C20 Zr1 N1 C100 -92.42(16) . . . . ? Cl1 Zr1 N1 C100 -4.14(16) . . . . ? C27 Zr1 N1 C100 84.51(18) . . . . ? C29 Zr1 N1 C100 88.53(17) . . . . ? C21 Zr1 N1 C100 -124.22(16) . . . . ? C28 Zr1 N1 C100 67.50(17) . . . . ? C23 Zr1 N1 C100 -96.51(17) . . . . ? C24 Zr1 N1 C100 -73.06(17) . . . . ? C22 Zr1 N1 P1 47.21(7) . . . . ? C25 Zr1 N1 P1 -57.80(6) . . . . ? C26 Zr1 N1 P1 -51.45(7) . . . . ? C20 Zr1 N1 P1 90.45(5) . . . . ? Cl1 Zr1 N1 P1 178.73(4) . . . . ? C27 Zr1 N1 P1 -92.62(8) . . . . ? C29 Zr1 N1 P1 -88.60(7) . . . . ? C21 Zr1 N1 P1 58.65(5) . . . . ? C28 Zr1 N1 P1 -109.63(6) . . . . ? C23 Zr1 N1 P1 86.35(8) . . . . ? C24 Zr1 N1 P1 109.80(5) . . . . ? C100 N1 P1 C1 -63.35(11) . . . . ? Zr1 N1 P1 C1 114.98(5) . . . . ? C100 N1 P1 C7 51.79(11) . . . . ? Zr1 N1 P1 C7 -129.88(5) . . . . ? C100 N1 P1 Zr1 -178.33(11) . . . . ? C22 Zr1 P1 N1 -143.51(6) . . . . ? C25 Zr1 P1 N1 120.04(7) . . . . ? C26 Zr1 P1 N1 141.14(6) . . . . ? C20 Zr1 P1 N1 -90.45(6) . . . . ? Cl1 Zr1 P1 N1 -1.52(5) . . . . ? C27 Zr1 P1 N1 125.08(8) . . . . ? C29 Zr1 P1 N1 89.79(7) . . . . ? C21 Zr1 P1 N1 -119.10(6) . . . . ? C28 Zr1 P1 N1 88.85(7) . . . . ? C23 Zr1 P1 N1 -132.04(7) . . . . ? C24 Zr1 P1 N1 -93.34(6) . . . . ? N1 Zr1 P1 C1 -96.38(7) . . . . ? C22 Zr1 P1 C1 120.11(6) . . . . ? C25 Zr1 P1 C1 23.66(7) . . . . ? C26 Zr1 P1 C1 44.76(6) . . . . ? C20 Zr1 P1 C1 173.17(6) . . . . ? Cl1 Zr1 P1 C1 -97.90(5) . . . . ? C27 Zr1 P1 C1 28.70(8) . . . . ? C29 Zr1 P1 C1 -6.59(7) . . . . ? C21 Zr1 P1 C1 144.51(6) . . . . ? C28 Zr1 P1 C1 -7.53(7) . . . . ? C23 Zr1 P1 C1 131.58(7) . . . . ? C24 Zr1 P1 C1 170.28(6) . . . . ? N1 Zr1 P1 C7 86.29(7) . . . . ? C22 Zr1 P1 C7 -57.22(6) . . . . ? C25 Zr1 P1 C7 -153.67(8) . . . . ? C26 Zr1 P1 C7 -132.57(6) . . . . ? C20 Zr1 P1 C7 -4.16(6) . . . . ? Cl1 Zr1 P1 C7 84.77(5) . . . . ? C27 Zr1 P1 C7 -148.63(8) . . . . ? C29 Zr1 P1 C7 176.08(7) . . . . ? C21 Zr1 P1 C7 -32.82(6) . . . . ? C28 Zr1 P1 C7 175.14(7) . . . . ? C23 Zr1 P1 C7 -45.75(7) . . . . ? C24 Zr1 P1 C7 -7.05(7) . . . . ? P1 N1 C100 C13 -95.34(11) . . . . ? Zr1 N1 C100 C13 88.07(17) . . . . ? P1 N1 C100 C19 138.87(10) . . . . ? Zr1 N1 C100 C19 -37.7(2) . . . . ? N1 P1 C1 C6 3.20(12) . . . . ? C7 P1 C1 C6 -116.11(11) . . . . ? Zr1 P1 C1 C6 65.87(12) . . . . ? N1 P1 C1 C2 -170.35(9) . . . . ? C7 P1 C1 C2 70.34(10) . . . . ? Zr1 P1 C1 C2 -107.68(9) . . . . ? C6 C1 C2 C3 2.39(18) . . . . ? P1 C1 C2 C3 176.17(10) . . . . ? C1 C2 C3 C4 -1.1(2) . . . . ? C2 C3 C4 C5 -0.5(2) . . . . ? C3 C4 C5 C6 0.7(2) . . . . ? C4 C5 C6 C1 0.6(2) . . . . ? C2 C1 C6 C5 -2.15(19) . . . . ? P1 C1 C6 C5 -175.67(10) . . . . ? N1 P1 C7 C8 -130.43(11) . . . . ? C1 P1 C7 C8 -9.96(12) . . . . ? Zr1 P1 C7 C8 167.72(8) . . . . ? N1 P1 C7 C12 46.84(11) . . . . ? C1 P1 C7 C12 167.31(10) . . . . ? Zr1 P1 C7 C12 -15.01(12) . . . . ? C12 C7 C8 C9 0.19(19) . . . . ? P1 C7 C8 C9 177.47(11) . . . . ? C7 C8 C9 C10 -0.8(2) . . . . ? C8 C9 C10 C11 0.5(2) . . . . ? C9 C10 C11 C12 0.3(2) . . . . ? C10 C11 C12 C7 -0.9(2) . . . . ? C8 C7 C12 C11 0.63(19) . . . . ? P1 C7 C12 C11 -176.78(10) . . . . ? N1 C100 C13 C18 -64.26(14) . . . . ? C19 C100 C13 C18 61.50(15) . . . . ? N1 C100 C13 C14 116.48(13) . . . . ? C19 C100 C13 C14 -117.77(13) . . . . ? C18 C13 C14 C15 -0.1(2) . . . . ? C100 C13 C14 C15 179.21(13) . . . . ? C13 C14 C15 C16 -0.2(2) . . . . ? C14 C15 C16 C17 0.3(2) . . . . ? C15 C16 C17 C18 -0.1(2) . . . . ? C14 C13 C18 C17 0.3(2) . . . . ? C100 C13 C18 C17 -178.96(13) . . . . ? C16 C17 C18 C13 -0.2(2) . . . . ? N1 Zr1 C20 C21 -99.44(8) . . . . ? C22 Zr1 C20 C21 37.17(8) . . . . ? C25 Zr1 C20 C21 4.69(14) . . . . ? C26 Zr1 C20 C21 42.78(11) . . . . ? Cl1 Zr1 C20 C21 175.16(8) . . . . ? C27 Zr1 C20 C21 83.07(10) . . . . ? C29 Zr1 C20 C21 -50(3) . . . . ? C28 Zr1 C20 C21 119.86(12) . . . . ? C23 Zr1 C20 C21 77.54(9) . . . . ? C24 Zr1 C20 C21 114.11(12) . . . . ? N1 Zr1 C20 C24 146.45(9) . . . . ? C22 Zr1 C20 C24 -76.94(10) . . . . ? C25 Zr1 C20 C24 -109.42(12) . . . . ? C26 Zr1 C20 C24 -71.33(11) . . . . ? Cl1 Zr1 C20 C24 61.05(9) . . . . ? C27 Zr1 C20 C24 -31.04(12) . . . . ? C29 Zr1 C20 C24 -164(3) . . . . ? C21 Zr1 C20 C24 -114.11(12) . . . . ? C28 Zr1 C20 C24 5.76(16) . . . . ? C23 Zr1 C20 C24 -36.57(9) . . . . ? C24 C20 C21 C22 1.87(15) . . . . ? Zr1 C20 C21 C22 -66.00(9) . . . . ? C24 C20 C21 Zr1 67.87(10) . . . . ? N1 Zr1 C21 C20 82.66(9) . . . . ? C22 Zr1 C21 C20 -114.73(12) . . . . ? C25 Zr1 C21 C20 -177.20(8) . . . . ? C26 Zr1 C21 C20 -146.54(9) . . . . ? Cl1 Zr1 C21 C20 -5.61(9) . . . . ? C27 Zr1 C21 C20 -117.88(9) . . . . ? C29 Zr1 C21 C20 178.21(11) . . . . ? C28 Zr1 C21 C20 -119.43(14) . . . . ? C23 Zr1 C21 C20 -77.32(9) . . . . ? C24 Zr1 C21 C20 -37.44(8) . . . . ? N1 Zr1 C21 C22 -162.61(8) . . . . ? C25 Zr1 C21 C22 -62.47(10) . . . . ? C26 Zr1 C21 C22 -31.81(9) . . . . ? C20 Zr1 C21 C22 114.73(12) . . . . ? Cl1 Zr1 C21 C22 109.12(8) . . . . ? C27 Zr1 C21 C22 -3.15(10) . . . . ? C29 Zr1 C21 C22 -67.06(13) . . . . ? C28 Zr1 C21 C22 -4.70(16) . . . . ? C23 Zr1 C21 C22 37.41(9) . . . . ? C24 Zr1 C21 C22 77.29(10) . . . . ? C20 C21 C22 C23 -2.02(15) . . . . ? Zr1 C21 C22 C23 -68.26(10) . . . . ? C20 C21 C22 Zr1 66.24(9) . . . . ? N1 Zr1 C22 C23 135.61(9) . . . . ? C25 Zr1 C22 C23 -120.14(10) . . . . ? C26 Zr1 C22 C23 -98.52(10) . . . . ? C20 Zr1 C22 C23 76.86(10) . . . . ? Cl1 Zr1 C22 C23 21.78(11) . . . . ? C27 Zr1 C22 C23 -68.89(10) . . . . ? C29 Zr1 C22 C23 -104.71(12) . . . . ? C21 Zr1 C22 C23 113.89(13) . . . . ? C28 Zr1 C22 C23 -68.77(11) . . . . ? C24 Zr1 C22 C23 36.36(9) . . . . ? N1 Zr1 C22 C21 21.72(10) . . . . ? C25 Zr1 C22 C21 125.97(8) . . . . ? C26 Zr1 C22 C21 147.60(10) . . . . ? C20 Zr1 C22 C21 -37.03(8) . . . . ? Cl1 Zr1 C22 C21 -92.11(8) . . . . ? C27 Zr1 C22 C21 177.22(9) . . . . ? C29 Zr1 C22 C21 141.40(10) . . . . ? C28 Zr1 C22 C21 177.34(9) . . . . ? C23 Zr1 C22 C21 -113.89(13) . . . . ? C24 Zr1 C22 C21 -77.53(9) . . . . ? C21 C22 C23 C24 1.41(16) . . . . ? Zr1 C22 C23 C24 -66.41(10) . . . . ? C21 C22 C23 Zr1 67.81(9) . . . . ? N1 Zr1 C23 C24 42.37(13) . . . . ? C22 Zr1 C23 C24 115.44(13) . . . . ? C25 Zr1 C23 C24 -176.66(9) . . . . ? C26 Zr1 C23 C24 -170.07(10) . . . . ? C20 Zr1 C23 C24 37.23(9) . . . . ? Cl1 Zr1 C23 C24 -46.86(9) . . . . ? C27 Zr1 C23 C24 -138.31(10) . . . . ? C29 Zr1 C23 C24 -144.03(11) . . . . ? C21 Zr1 C23 C24 77.79(10) . . . . ? C28 Zr1 C23 C24 -122.40(10) . . . . ? N1 Zr1 C23 C22 -73.07(12) . . . . ? C25 Zr1 C23 C22 67.90(10) . . . . ? C26 Zr1 C23 C22 74.49(10) . . . . ? C20 Zr1 C23 C22 -78.21(10) . . . . ? Cl1 Zr1 C23 C22 -162.30(9) . . . . ? C27 Zr1 C23 C22 106.25(10) . . . . ? C29 Zr1 C23 C22 100.53(12) . . . . ? C21 Zr1 C23 C22 -37.65(9) . . . . ? C28 Zr1 C23 C22 122.16(10) . . . . ? C24 Zr1 C23 C22 -115.44(13) . . . . ? C22 C23 C24 C20 -0.25(16) . . . . ? Zr1 C23 C24 C20 -65.69(10) . . . . ? C22 C23 C24 Zr1 65.44(10) . . . . ? C21 C20 C24 C23 -1.01(15) . . . . ? Zr1 C20 C24 C23 66.41(10) . . . . ? C21 C20 C24 Zr1 -67.42(9) . . . . ? N1 Zr1 C24 C23 -153.49(8) . . . . ? C22 Zr1 C24 C23 -36.88(9) . . . . ? C25 Zr1 C24 C23 5.26(15) . . . . ? C26 Zr1 C24 C23 10.61(11) . . . . ? C20 Zr1 C24 C23 -114.94(13) . . . . ? Cl1 Zr1 C24 C23 130.76(9) . . . . ? C27 Zr1 C24 C23 40.90(10) . . . . ? C29 Zr1 C24 C23 64.40(16) . . . . ? C21 Zr1 C24 C23 -77.55(10) . . . . ? C28 Zr1 C24 C23 68.33(11) . . . . ? N1 Zr1 C24 C20 -38.55(10) . . . . ? C22 Zr1 C24 C20 78.06(10) . . . . ? C25 Zr1 C24 C20 120.19(11) . . . . ? C26 Zr1 C24 C20 125.55(9) . . . . ? Cl1 Zr1 C24 C20 -114.30(9) . . . . ? C27 Zr1 C24 C20 155.84(9) . . . . ? C29 Zr1 C24 C20 179.34(12) . . . . ? C21 Zr1 C24 C20 37.39(8) . . . . ? C28 Zr1 C24 C20 -176.73(9) . . . . ? C23 Zr1 C24 C20 114.94(13) . . . . ? N1 Zr1 C25 C26 170.52(11) . . . . ? C22 Zr1 C25 C26 42.11(12) . . . . ? C20 Zr1 C25 C26 67.86(14) . . . . ? Cl1 Zr1 C25 C26 -100.66(12) . . . . ? C27 Zr1 C25 C26 -37.01(11) . . . . ? C29 Zr1 C25 C26 -114.10(15) . . . . ? C21 Zr1 C25 C26 70.61(12) . . . . ? C28 Zr1 C25 C26 -76.96(12) . . . . ? C23 Zr1 C25 C26 12.37(13) . . . . ? C24 Zr1 C25 C26 9.40(17) . . . . ? N1 Zr1 C25 C29 -75.38(11) . . . . ? C22 Zr1 C25 C29 156.20(11) . . . . ? C26 Zr1 C25 C29 114.10(15) . . . . ? C20 Zr1 C25 C29 -178.05(11) . . . . ? Cl1 Zr1 C25 C29 13.44(13) . . . . ? C27 Zr1 C25 C29 77.09(12) . . . . ? C21 Zr1 C25 C29 -175.29(11) . . . . ? C28 Zr1 C25 C29 37.14(12) . . . . ? C23 Zr1 C25 C29 126.47(11) . . . . ? C24 Zr1 C25 C29 123.49(13) . . . . ? C29 C25 C26 C27 -0.17(17) . . . . ? Zr1 C25 C26 C27 67.33(11) . . . . ? C29 C25 C26 Zr1 -67.50(11) . . . . ? N1 Zr1 C26 C27 -126.16(12) . . . . ? C22 Zr1 C26 C27 109.40(13) . . . . ? C25 Zr1 C26 C27 -114.19(17) . . . . ? C20 Zr1 C26 C27 104.75(13) . . . . ? Cl1 Zr1 C26 C27 -12.89(13) . . . . ? C29 Zr1 C26 C27 -76.84(14) . . . . ? C21 Zr1 C26 C27 126.37(12) . . . . ? C28 Zr1 C26 C27 -36.82(13) . . . . ? C23 Zr1 C26 C27 77.37(12) . . . . ? C24 Zr1 C26 C27 71.77(13) . . . . ? N1 Zr1 C26 C25 -11.97(13) . . . . ? C22 Zr1 C26 C25 -136.40(12) . . . . ? C20 Zr1 C26 C25 -141.06(11) . . . . ? Cl1 Zr1 C26 C25 101.31(11) . . . . ? C27 Zr1 C26 C25 114.19(17) . . . . ? C29 Zr1 C26 C25 37.36(12) . . . . ? C21 Zr1 C26 C25 -119.44(11) . . . . ? C28 Zr1 C26 C25 77.38(13) . . . . ? C23 Zr1 C26 C25 -168.44(12) . . . . ? C24 Zr1 C26 C25 -174.04(11) . . . . ? C25 C26 C27 C28 0.33(18) . . . . ? Zr1 C26 C27 C28 67.22(11) . . . . ? C25 C26 C27 Zr1 -66.89(11) . . . . ? N1 Zr1 C27 C28 -31.46(15) . . . . ? C22 Zr1 C27 C28 179.81(13) . . . . ? C25 Zr1 C27 C28 -77.18(15) . . . . ? C26 Zr1 C27 C28 -114.70(18) . . . . ? C20 Zr1 C27 C28 144.61(12) . . . . ? Cl1 Zr1 C27 C28 54.57(13) . . . . ? C29 Zr1 C27 C28 -36.54(14) . . . . ? C21 Zr1 C27 C28 -178.51(12) . . . . ? C23 Zr1 C27 C28 149.16(13) . . . . ? C24 Zr1 C27 C28 128.45(13) . . . . ? N1 Zr1 C27 C26 83.24(14) . . . . ? C22 Zr1 C27 C26 -65.49(12) . . . . ? C25 Zr1 C27 C26 37.52(11) . . . . ? C20 Zr1 C27 C26 -100.69(12) . . . . ? Cl1 Zr1 C27 C26 169.27(11) . . . . ? C29 Zr1 C27 C26 78.16(13) . . . . ? C21 Zr1 C27 C26 -63.81(13) . . . . ? C28 Zr1 C27 C26 114.70(18) . . . . ? C23 Zr1 C27 C26 -96.14(12) . . . . ? C24 Zr1 C27 C26 -116.85(12) . . . . ? C26 C27 C28 C29 -0.37(19) . . . . ? Zr1 C27 C28 C29 66.50(12) . . . . ? C26 C27 C28 Zr1 -66.87(11) . . . . ? N1 Zr1 C28 C27 158.87(11) . . . . ? C22 Zr1 C28 C27 -0.21(15) . . . . ? C25 Zr1 C28 C27 77.79(13) . . . . ? C26 Zr1 C28 C27 37.01(10) . . . . ? C20 Zr1 C28 C27 -64.10(16) . . . . ? Cl1 Zr1 C28 C27 -122.48(13) . . . . ? C29 Zr1 C28 C27 115.49(18) . . . . ? C21 Zr1 C28 C27 2.6(2) . . . . ? C23 Zr1 C28 C27 -30.68(13) . . . . ? C24 Zr1 C28 C27 -60.65(13) . . . . ? N1 Zr1 C28 C29 43.39(13) . . . . ? C22 Zr1 C28 C29 -115.70(13) . . . . ? C25 Zr1 C28 C29 -37.70(12) . . . . ? C26 Zr1 C28 C29 -78.48(13) . . . . ? C20 Zr1 C28 C29 -179.59(12) . . . . ? Cl1 Zr1 C28 C29 122.03(13) . . . . ? C27 Zr1 C28 C29 -115.49(18) . . . . ? C21 Zr1 C28 C29 -112.87(16) . . . . ? C23 Zr1 C28 C29 -146.17(12) . . . . ? C24 Zr1 C28 C29 -176.14(12) . . . . ? C27 C28 C29 C25 0.26(19) . . . . ? Zr1 C28 C29 C25 66.79(11) . . . . ? C27 C28 C29 Zr1 -66.53(12) . . . . ? C26 C25 C29 C28 -0.05(18) . . . . ? Zr1 C25 C29 C28 -67.38(12) . . . . ? C26 C25 C29 Zr1 67.32(11) . . . . ? N1 Zr1 C29 C28 -140.31(13) . . . . ? C22 Zr1 C29 C28 83.98(15) . . . . ? C25 Zr1 C29 C28 113.87(16) . . . . ? C26 Zr1 C29 C28 76.48(12) . . . . ? C20 Zr1 C29 C28 171(3) . . . . ? Cl1 Zr1 C29 C28 -54.97(12) . . . . ? C27 Zr1 C29 C28 36.43(11) . . . . ? C21 Zr1 C29 C28 121.72(15) . . . . ? C23 Zr1 C29 C28 43.44(16) . . . . ? C24 Zr1 C29 C28 6.7(2) . . . . ? N1 Zr1 C29 C25 105.81(11) . . . . ? C22 Zr1 C29 C25 -29.89(14) . . . . ? C26 Zr1 C29 C25 -37.39(10) . . . . ? C20 Zr1 C29 C25 57(3) . . . . ? Cl1 Zr1 C29 C25 -168.85(10) . . . . ? C27 Zr1 C29 C25 -77.44(11) . . . . ? C21 Zr1 C29 C25 7.85(17) . . . . ? C28 Zr1 C29 C25 -113.87(16) . . . . ? C23 Zr1 C29 C25 -70.43(14) . . . . ? C24 Zr1 C29 C25 -107.21(16) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 30.56 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.337 _refine_diff_density_min -0.226 _refine_diff_density_rms 0.038 data_5 _database_code_depnum_ccdc_archive 'CCDC 265445' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H40 N P Zr' _chemical_formula_weight 668.93 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.798(2) _cell_length_b 9.975(3) _cell_length_c 19.110(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.067(6) _cell_angle_gamma 90.00 _cell_volume 1670.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 0.407 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.848144 _exptl_absorpt_correction_T_max 0.976 _exptl_absorpt_process_details 'SADABS - Bruker/Siemens' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart 1000 CCD' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20675 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 30.56 _reflns_number_total 10067 _reflns_number_gt 7951 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _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^)+(0.0246P)^2^+0.3750P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_number_reflns 10067 _refine_ls_number_parameters 398 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.0767 _refine_ls_wR_factor_gt 0.0682 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr Zr 1.04804(2) 0.29581(2) 1.218956(12) 0.02384(6) Uani 1 1 d . . . N N 0.9598(2) 0.4871(2) 1.23584(11) 0.0249(5) Uani 1 1 d . . . P P 1.13363(8) 0.53289(6) 1.26841(4) 0.02513(14) Uani 1 1 d . . . C1 C 0.8232(3) 0.5721(3) 1.22334(13) 0.0266(5) Uani 1 1 d . . . H1 H 0.8457 0.6435 1.1890 0.032 Uiso 1 1 calc R . . C2 C 0.6900(3) 0.4885(3) 1.19067(17) 0.0341(7) Uani 1 1 d . . . H2A H 0.7205 0.4428 1.1487 0.051 Uiso 1 1 calc R . . H2B H 0.6028 0.5473 1.1776 0.051 Uiso 1 1 calc R . . H2C H 0.6612 0.4218 1.2248 0.051 Uiso 1 1 calc R . . C3 C 0.7787(3) 0.6398(3) 1.28945(14) 0.0254(5) Uani 1 1 d . . . C4 C 0.7493(3) 0.7757(3) 1.28989(14) 0.0300(6) Uani 1 1 d . . . H4 H 0.7595 0.8272 1.2487 0.036 Uiso 1 1 calc R . . C5 C 0.7049(3) 0.8382(3) 1.34970(16) 0.0373(7) Uani 1 1 d . . . H5 H 0.6849 0.9318 1.3491 0.045 Uiso 1 1 calc R . . C6 C 0.6898(3) 0.7654(3) 1.40969(16) 0.0401(8) Uani 1 1 d . . . H6 H 0.6587 0.8082 1.4505 0.048 Uiso 1 1 calc R . . C7 C 0.7206(3) 0.6285(3) 1.41027(16) 0.0384(7) Uani 1 1 d . . . H7 H 0.7125 0.5778 1.4519 0.046 Uiso 1 1 calc R . . C8 C 0.7629(3) 0.5662(3) 1.35043(14) 0.0317(6) Uani 1 1 d . . . H8 H 0.7814 0.4724 1.3508 0.038 Uiso 1 1 calc R . . C9 C 1.1361(3) 0.6060(3) 1.35599(14) 0.0291(6) Uani 1 1 d . . . C10 C 1.1145(3) 0.7424(3) 1.36694(15) 0.0338(6) Uani 1 1 d . . . H10 H 1.1057 0.8021 1.3281 0.041 Uiso 1 1 calc R . . C11 C 1.1060(3) 0.7912(5) 1.43393(14) 0.0436(6) Uani 1 1 d . . . H11 H 1.0921 0.8845 1.4411 0.052 Uiso 1 1 calc R . . C12 C 1.1174(4) 0.7058(4) 1.49010(17) 0.0536(9) Uani 1 1 d . . . H12 H 1.1101 0.7400 1.5361 0.064 Uiso 1 1 calc R . . C13 C 1.1392(4) 0.5712(4) 1.48052(16) 0.0513(9) Uani 1 1 d . . . H13 H 1.1472 0.5124 1.5198 0.062 Uiso 1 1 calc R . . C14 C 1.1495(3) 0.5210(3) 1.41344(15) 0.0395(7) Uani 1 1 d . . . H14 H 1.1657 0.4278 1.4069 0.047 Uiso 1 1 calc R . . C15 C 1.2071(3) 0.6622(2) 1.21369(13) 0.0234(5) Uani 1 1 d . . . C16 C 1.1463(3) 0.6789(3) 1.14488(14) 0.0288(6) Uani 1 1 d . . . H16 H 1.0594 0.6281 1.1280 0.035 Uiso 1 1 calc R . . C17 C 1.2100(3) 0.7686(3) 1.10014(14) 0.0343(7) Uani 1 1 d . . . H17 H 1.1669 0.7791 1.0531 0.041 Uiso 1 1 calc R . . C18 C 1.3367(3) 0.8422(3) 1.12470(15) 0.0354(7) Uani 1 1 d . . . H18 H 1.3814 0.9036 1.0945 0.042 Uiso 1 1 calc R . . C19 C 1.3984(3) 0.8263(3) 1.19342(15) 0.0346(7) Uani 1 1 d . . . H19 H 1.4849 0.8777 1.2103 0.042 Uiso 1 1 calc R . . C20 C 1.3358(3) 0.7369(3) 1.23737(15) 0.0304(6) Uani 1 1 d . . . H20 H 1.3802 0.7258 1.2841 0.036 Uiso 1 1 calc R . . C21 C 0.9514(3) 0.1664(3) 1.30357(15) 0.0350(7) Uani 1 1 d . . . H21A H 1.0276 0.1105 1.3314 0.042 Uiso 1 1 calc R . . H21B H 0.8835 0.2143 1.3338 0.042 Uiso 1 1 calc R . . C22 C 0.8744(3) 0.1007(3) 1.24329(15) 0.0287(6) Uani 1 1 d . . . C23 C 0.9523(3) 0.0216(3) 1.19759(16) 0.0348(6) Uani 1 1 d . . . H23 H 1.0565 0.0001 1.2097 0.042 Uiso 1 1 calc R . . C24 C 0.8801(4) -0.0262(3) 1.13466(17) 0.0420(8) Uani 1 1 d . . . H24 H 0.9336 -0.0839 1.1058 0.050 Uiso 1 1 calc R . . C25 C 0.7325(4) 0.0093(3) 1.11417(17) 0.0434(8) Uani 1 1 d . . . H25 H 0.6842 -0.0223 1.0709 0.052 Uiso 1 1 calc R . . C26 C 0.6547(4) 0.0912(3) 1.15674(18) 0.0393(8) Uani 1 1 d . . . H26 H 0.5528 0.1168 1.1422 0.047 Uiso 1 1 calc R . . C27 C 0.7220(3) 0.1365(3) 1.21981(16) 0.0333(7) Uani 1 1 d . . . H27 H 0.6658 0.1927 1.2483 0.040 Uiso 1 1 calc R . . C28 C 0.9803(3) 0.2977(4) 1.09963(12) 0.0335(5) Uani 1 1 d . . . H28A H 0.8982 0.2316 1.0877 0.040 Uiso 1 1 calc R . . H28B H 0.9423 0.3876 1.0848 0.040 Uiso 1 1 calc R . . C29 C 1.1173(3) 0.2632(3) 1.06307(13) 0.0314(7) Uani 1 1 d . . . C30 C 1.1294(3) 0.1417(3) 1.02777(14) 0.0348(6) Uani 1 1 d . . . H30 H 1.0458 0.0812 1.0248 0.042 Uiso 1 1 calc R . . C31 C 1.2606(4) 0.1075(3) 0.99699(16) 0.0441(8) Uani 1 1 d . . . H31 H 1.2648 0.0250 0.9724 0.053 Uiso 1 1 calc R . . C32 C 1.3853(4) 0.1916(4) 1.00151(17) 0.0492(8) Uani 1 1 d . . . H32 H 1.4756 0.1672 0.9809 0.059 Uiso 1 1 calc R . . C33 C 1.3766(3) 0.3113(5) 1.03639(15) 0.0458(8) Uani 1 1 d . . . H33 H 1.4620 0.3699 1.0402 0.055 Uiso 1 1 calc R . . C34 C 1.2449(4) 0.3474(3) 1.06601(15) 0.0403(7) Uani 1 1 d . . . H34 H 1.2408 0.4317 1.0890 0.048 Uiso 1 1 calc R . . C35 C 1.2973(3) 0.2311(3) 1.22854(14) 0.0326(6) Uani 1 1 d . . . H35A H 1.3062 0.1483 1.2006 0.039 Uiso 1 1 calc R . . H35B H 1.3578 0.3015 1.2072 0.039 Uiso 1 1 calc R . . C36 C 1.3666(3) 0.2056(3) 1.30121(14) 0.0291(6) Uani 1 1 d . . . C37 C 1.4438(3) 0.3055(4) 1.34068(13) 0.0355(6) Uani 1 1 d . . . H37 H 1.4538 0.3919 1.3207 0.043 Uiso 1 1 calc R . . C38 C 1.5065(3) 0.2811(5) 1.40874(15) 0.0434(8) Uani 1 1 d . . . H38 H 1.5601 0.3504 1.4345 0.052 Uiso 1 1 calc R . . C39 C 1.4916(3) 0.1571(4) 1.43907(17) 0.0463(8) Uani 1 1 d . . . H39 H 1.5343 0.1407 1.4857 0.056 Uiso 1 1 calc R . . C40 C 1.4149(3) 0.0581(3) 1.40160(17) 0.0447(8) Uani 1 1 d . . . H40 H 1.4033 -0.0274 1.4223 0.054 Uiso 1 1 calc R . . C41 C 1.3539(3) 0.0815(3) 1.33364(17) 0.0384(7) Uani 1 1 d . . . H41 H 1.3018 0.0109 1.3082 0.046 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 Zr 0.02446(10) 0.02060(9) 0.02687(11) -0.00012(14) 0.00453(8) -0.00136(13) N 0.0236(11) 0.0228(11) 0.0291(12) -0.0013(9) 0.0067(9) -0.0006(9) P 0.0263(3) 0.0220(3) 0.0271(4) -0.0005(3) 0.0027(3) -0.0022(3) C1 0.0303(14) 0.0256(13) 0.0244(13) 0.0045(11) 0.0049(11) 0.0031(10) C2 0.0299(16) 0.0391(17) 0.0329(18) -0.0055(14) -0.0002(13) 0.0011(13) C3 0.0219(12) 0.0244(12) 0.0306(14) 0.0009(11) 0.0048(11) -0.0020(10) C4 0.0288(12) 0.0271(18) 0.0345(13) -0.0005(12) 0.0044(10) -0.0031(11) C5 0.0396(16) 0.0272(14) 0.0456(18) -0.0049(12) 0.0062(14) 0.0028(11) C6 0.0435(16) 0.039(2) 0.0398(16) -0.0096(13) 0.0129(13) 0.0015(12) C7 0.0461(18) 0.0407(16) 0.0303(16) 0.0012(13) 0.0134(13) -0.0028(14) C8 0.0378(15) 0.0282(14) 0.0304(15) 0.0013(12) 0.0097(12) -0.0021(12) C9 0.0277(14) 0.0323(14) 0.0269(14) -0.0005(11) -0.0004(11) -0.0048(11) C10 0.0366(15) 0.0372(14) 0.0280(15) -0.0039(12) 0.0047(12) -0.0049(12) C11 0.0408(14) 0.0526(16) 0.0374(15) -0.014(2) 0.0039(11) -0.007(2) C12 0.048(2) 0.086(3) 0.0265(17) -0.0107(18) 0.0001(14) -0.0069(19) C13 0.0427(19) 0.083(3) 0.0269(17) 0.0184(17) -0.0038(14) -0.0017(18) C14 0.0361(16) 0.0463(18) 0.0356(16) 0.0115(14) -0.0010(13) -0.0010(14) C15 0.0244(12) 0.0221(12) 0.0247(13) -0.0023(10) 0.0080(10) 0.0003(10) C16 0.0268(13) 0.0306(14) 0.0292(14) -0.0033(11) 0.0040(11) -0.0039(11) C17 0.0363(14) 0.043(2) 0.0239(13) 0.0022(12) 0.0065(11) -0.0014(12) C18 0.0364(15) 0.0349(15) 0.0365(16) 0.0072(12) 0.0126(13) -0.0062(11) C19 0.0281(13) 0.0357(19) 0.0397(16) 0.0031(12) 0.0014(12) -0.0101(11) C20 0.0290(14) 0.0323(14) 0.0294(15) -0.0003(11) -0.0002(12) -0.0038(11) C21 0.0432(17) 0.0350(15) 0.0281(14) 0.0039(12) 0.0115(13) -0.0055(13) C22 0.0347(15) 0.0219(13) 0.0308(15) 0.0047(11) 0.0109(12) -0.0084(12) C23 0.0319(15) 0.0268(14) 0.0472(18) 0.0035(13) 0.0122(13) 0.0016(12) C24 0.055(2) 0.0263(14) 0.0486(19) -0.0063(14) 0.0258(16) -0.0035(13) C25 0.0497(19) 0.0410(18) 0.0393(18) -0.0079(14) 0.0031(15) -0.0176(15) C26 0.0302(16) 0.0404(18) 0.047(2) 0.0005(15) 0.0036(14) -0.0074(13) C27 0.0331(16) 0.0272(14) 0.0412(18) -0.0026(13) 0.0124(14) -0.0047(12) C28 0.0466(14) 0.0270(11) 0.0280(12) -0.0017(18) 0.0105(10) 0.0004(19) C29 0.0425(15) 0.0332(18) 0.0183(12) 0.0060(10) 0.0011(11) -0.0024(11) C30 0.0459(17) 0.0344(15) 0.0246(14) -0.0006(12) 0.0054(12) -0.0018(13) C31 0.054(2) 0.0440(18) 0.0356(17) 0.0006(14) 0.0133(15) 0.0109(16) C32 0.0434(18) 0.061(2) 0.0447(19) 0.0187(18) 0.0143(15) 0.0123(17) C33 0.0385(15) 0.058(2) 0.0409(16) 0.0194(19) 0.0017(12) -0.0117(18) C34 0.057(2) 0.0380(15) 0.0260(15) 0.0029(12) 0.0040(14) -0.0081(14) C35 0.0311(14) 0.0353(15) 0.0320(15) -0.0037(12) 0.0064(12) 0.0023(12) C36 0.0199(12) 0.0373(15) 0.0306(14) -0.0034(12) 0.0058(11) 0.0075(11) C37 0.0285(12) 0.0413(16) 0.0374(13) -0.0048(18) 0.0067(10) -0.0058(17) C38 0.0311(13) 0.059(2) 0.0394(15) -0.009(2) 0.0014(11) -0.0055(18) C39 0.0303(16) 0.074(2) 0.0353(18) 0.0077(17) 0.0052(13) 0.0073(15) C40 0.0370(17) 0.0469(19) 0.051(2) 0.0126(16) 0.0073(15) 0.0120(15) C41 0.0319(15) 0.0361(16) 0.0469(18) -0.0007(14) 0.0024(14) 0.0070(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 Zr N 2.096(2) . ? Zr C35 2.278(3) . ? Zr C21 2.290(3) . ? Zr C28 2.305(2) . ? Zr C22 2.542(3) . ? Zr P 2.6319(9) . ? N C1 1.473(3) . ? N P 1.664(2) . ? P C15 1.815(3) . ? P C9 1.824(3) . ? C1 C3 1.514(4) . ? C1 C2 1.526(4) . ? C3 C4 1.381(4) . ? C3 C8 1.395(4) . ? C4 C5 1.388(4) . ? C5 C6 1.373(4) . ? C6 C7 1.393(4) . ? C7 C8 1.381(4) . ? C9 C14 1.384(4) . ? C9 C10 1.392(4) . ? C10 C11 1.378(4) . ? C11 C12 1.367(5) . ? C12 C13 1.371(5) . ? C13 C14 1.387(5) . ? C15 C16 1.385(4) . ? C15 C20 1.396(4) . ? C16 C17 1.389(4) . ? C17 C18 1.382(4) . ? C18 C19 1.385(4) . ? C19 C20 1.373(4) . ? C21 C22 1.441(4) . ? C22 C23 1.400(4) . ? C22 C27 1.422(4) . ? C23 C24 1.394(4) . ? C24 C25 1.369(5) . ? C25 C26 1.377(5) . ? C26 C27 1.372(4) . ? C28 C29 1.486(4) . ? C29 C30 1.396(4) . ? C29 C34 1.399(4) . ? C30 C31 1.384(4) . ? C31 C32 1.377(5) . ? C32 C33 1.372(5) . ? C33 C34 1.382(4) . ? C35 C36 1.488(4) . ? C36 C37 1.390(4) . ? C36 C41 1.393(4) . ? C37 C38 1.389(4) . ? C38 C39 1.377(6) . ? C39 C40 1.363(5) . ? C40 C41 1.380(4) . ? 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 N Zr C35 127.79(10) . . ? N Zr C21 103.81(10) . . ? C35 Zr C21 101.44(11) . . ? N Zr C28 94.46(12) . . ? C35 Zr C28 104.16(9) . . ? C21 Zr C28 128.57(12) . . ? N Zr C22 115.59(10) . . ? C35 Zr C22 110.99(10) . . ? C21 Zr C22 34.21(10) . . ? C28 Zr C22 94.61(11) . . ? N Zr P 39.18(6) . . ? C35 Zr P 89.01(7) . . ? C21 Zr P 111.41(8) . . ? C28 Zr P 112.86(11) . . ? C22 Zr P 141.23(7) . . ? C1 N P 127.78(18) . . ? C1 N Zr 143.83(17) . . ? P N Zr 88.09(10) . . ? N P C15 110.01(11) . . ? N P C9 112.90(12) . . ? C15 P C9 105.58(12) . . ? N P Zr 52.73(7) . . ? C15 P Zr 122.47(8) . . ? C9 P Zr 131.95(9) . . ? N C1 C3 112.9(2) . . ? N C1 C2 109.7(2) . . ? C3 C1 C2 109.8(2) . . ? C4 C3 C8 118.6(3) . . ? C4 C3 C1 120.4(2) . . ? C8 C3 C1 121.0(2) . . ? C3 C4 C5 120.8(3) . . ? C6 C5 C4 120.3(3) . . ? C5 C6 C7 119.5(3) . . ? C8 C7 C6 120.1(3) . . ? C7 C8 C3 120.6(3) . . ? C14 C9 C10 118.9(3) . . ? C14 C9 P 118.5(2) . . ? C10 C9 P 122.5(2) . . ? C11 C10 C9 120.3(3) . . ? C12 C11 C10 120.2(4) . . ? C11 C12 C13 120.4(3) . . ? C12 C13 C14 119.9(3) . . ? C9 C14 C13 120.3(3) . . ? C16 C15 C20 118.5(2) . . ? C16 C15 P 120.32(19) . . ? C20 C15 P 120.8(2) . . ? C15 C16 C17 121.2(2) . . ? C18 C17 C16 119.4(2) . . ? C17 C18 C19 119.9(2) . . ? C20 C19 C18 120.6(3) . . ? C19 C20 C15 120.4(3) . . ? C22 C21 Zr 82.49(16) . . ? C23 C22 C27 116.4(3) . . ? C23 C22 C21 122.2(3) . . ? C27 C22 C21 120.1(3) . . ? C23 C22 Zr 88.98(17) . . ? C27 C22 Zr 108.39(18) . . ? C21 C22 Zr 63.30(14) . . ? C24 C23 C22 121.3(3) . . ? C25 C24 C23 120.5(3) . . ? C24 C25 C26 119.5(3) . . ? C27 C26 C25 121.1(3) . . ? C26 C27 C22 121.1(3) . . ? C29 C28 Zr 108.29(16) . . ? C30 C29 C34 116.5(3) . . ? C30 C29 C28 121.9(3) . . ? C34 C29 C28 121.5(3) . . ? C31 C30 C29 121.4(3) . . ? C32 C31 C30 120.8(3) . . ? C33 C32 C31 118.8(3) . . ? C32 C33 C34 120.7(3) . . ? C33 C34 C29 121.7(3) . . ? C36 C35 Zr 115.82(18) . . ? C37 C36 C41 116.7(3) . . ? C37 C36 C35 121.6(3) . . ? C41 C36 C35 121.6(3) . . ? C38 C37 C36 121.2(4) . . ? C39 C38 C37 120.4(4) . . ? C40 C39 C38 119.4(3) . . ? C39 C40 C41 120.3(3) . . ? C40 C41 C36 121.9(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.56 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.789 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.068 _publ_section_abstract ; ; _publ_section_experimental ; ; _publ_section_comment ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; #END===========================================================================