Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Michael, Hill' 'Peter B. Hitchcock' _publ_contact_author_name 'Dr Michael Hill' _publ_contact_author_address ; Department of Chemistry University of Sussex Falmer Brighton BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email 'M.S.HILL@SUSSEX.AC.UK' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis of C2 and Cs Symmetric Zinc Complexes Supported by bis(phosphinimino)methyl ligands and their use in Ring Opening Polymerisation Catalysis ; data_msh2-(may2802) _database_code_CSD 190727 _audit_creation_date 2002-05-23T10:16:16-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FO #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[MesNPPh2CH2PPh2NPh].1/2(H2O)' _chemical_formula_moiety '(C40 H38 N2 P2).1/2(H2 O1)' _chemical_formula_sum 'C40 H39 N2 0.50 P2' _chemical_formula_weight 617.67 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Fdd2 _symmetry_Int_Tables_number 43 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/4, y+1/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+3/4, -y+5/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+5/4, -y+3/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+5/4, -y+5/4, z+1/4' _cell_length_a 26.6838(6) _cell_length_b 53.8252(14) _cell_length_c 9.4022(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 13504.0(5) _cell_formula_units_Z 16 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8347 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5232 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.161 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_unetI/netI 0.0649 _diffrn_reflns_number 10024 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 64 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.81 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.925 _diffrn_measured_fraction_theta_max 0.925 _reflns_number_total 4977 _reflns_number_gt 4217 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0380P)^2^+14.1620P] 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 'water H atom refined,others riding' _refine_ls_extinction_method none _refine_ls_number_reflns 4977 _refine_ls_number_parameters 416 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.0947 _refine_ls_wR_factor_gt 0.0883 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.11(9) _refine_diff_density_max 0.28 _refine_diff_density_min -0.218 _refine_diff_density_rms 0.041 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 -0.18922(3) 0.195571(13) 0.12935(9) 0.0278(2) Uani 1 1 d . . . P2 P -0.28236(3) 0.175875(14) 0.30847(9) 0.0315(2) Uani 1 1 d . . . N1 N -0.17869(9) 0.22126(4) 0.0555(3) 0.0324(6) Uani 1 1 d . . . N2 N -0.24873(9) 0.15391(5) 0.3578(3) 0.0343(7) Uani 1 1 d . . . O O -0.25 0.25 -0.1150(4) 0.0616(11) Uani 1 2 d S . . H1X H -0.2315(15) 0.2421(7) -0.047(5) 0.079(14) Uiso 1 1 d . . . C1 C -0.24055(14) 0.20075(6) 0.2527(4) 0.0347(8) Uani 1 1 d . . . H1A H -0.2263(12) 0.2079(6) 0.336(4) 0.037(9) Uiso 1 1 d . . . H1B H -0.2608(13) 0.2132(6) 0.212(4) 0.045(10) Uiso 1 1 d . . . C2 C -0.13609(13) 0.18311(5) 0.2251(4) 0.0338(8) Uani 1 1 d . . . C3 C -0.13574(14) 0.17712(6) 0.3688(4) 0.0440(9) Uani 1 1 d . . . H3 H -0.1658 0.178 0.4228 0.053 Uiso 1 1 calc R . . C4 C -0.09107(18) 0.16982(6) 0.4333(5) 0.0583(12) Uani 1 1 d . . . H4 H -0.0906 0.166 0.5319 0.07 Uiso 1 1 calc R . . C5 C -0.04767(17) 0.16809(6) 0.3553(5) 0.0584(12) Uani 1 1 d . . . H5 H -0.0175 0.1629 0.3998 0.07 Uiso 1 1 calc R . . C6 C -0.04788(15) 0.17386(6) 0.2139(5) 0.0539(11) Uani 1 1 d . . . H6 H -0.0178 0.1727 0.1604 0.065 Uiso 1 1 calc R . . C7 C -0.09164(12) 0.18132(5) 0.1481(4) 0.0400(9) Uani 1 1 d . . . H7 H -0.0914 0.1853 0.0496 0.048 Uiso 1 1 calc R . . C8 C -0.20684(11) 0.17180(5) 0.0031(3) 0.0275(7) Uani 1 1 d . . . C9 C -0.19485(11) 0.14689(5) 0.0254(3) 0.0312(7) Uani 1 1 d . . . H9 H -0.18 0.1419 0.1125 0.037 Uiso 1 1 calc R . . C10 C -0.20469(12) 0.12947(6) -0.0797(4) 0.0400(9) Uani 1 1 d . . . H10 H -0.1963 0.1125 -0.0645 0.048 Uiso 1 1 calc R . . C11 C -0.22657(13) 0.13663(6) -0.2061(4) 0.0451(9) Uani 1 1 d . . . H11 H -0.2326 0.1247 -0.2786 0.054 Uiso 1 1 calc R . . C12 C -0.23945(14) 0.16085(6) -0.2266(4) 0.0462(10) Uani 1 1 d . . . H12 H -0.2553 0.1657 -0.3128 0.055 Uiso 1 1 calc R . . C13 C -0.22972(12) 0.17850(6) -0.1235(4) 0.0380(8) Uani 1 1 d . . . H13 H -0.2388 0.1953 -0.1395 0.046 Uiso 1 1 calc R . . C14 C -0.32156(11) 0.17028(5) 0.1549(3) 0.0324(8) Uani 1 1 d . . . C15 C -0.32047(12) 0.14709(6) 0.0903(4) 0.0353(8) Uani 1 1 d . . . H15 H -0.3019 0.1339 0.132 0.042 Uiso 1 1 calc R . . C16 C -0.34643(13) 0.14328(6) -0.0351(4) 0.0471(10) Uani 1 1 d . . . H16 H -0.3457 0.1275 -0.0801 0.056 Uiso 1 1 calc R . . C17 C -0.37345(14) 0.16250(7) -0.0946(4) 0.0545(11) Uani 1 1 d . . . H17 H -0.3907 0.1599 -0.1818 0.065 Uiso 1 1 calc R . . C18 C -0.37583(14) 0.18536(7) -0.0295(4) 0.0488(10) Uani 1 1 d . . . H18 H -0.3953 0.1983 -0.0701 0.059 Uiso 1 1 calc R . . C19 C -0.34987(12) 0.18927(6) 0.0948(4) 0.0397(9) Uani 1 1 d . . . H19 H -0.3513 0.205 0.1399 0.048 Uiso 1 1 calc R . . C20 C -0.32386(13) 0.19044(6) 0.4373(3) 0.0365(8) Uani 1 1 d . . . C21 C -0.30489(16) 0.20595(6) 0.5431(4) 0.0503(10) Uani 1 1 d . . . H21 H -0.2699 0.2092 0.5477 0.06 Uiso 1 1 calc R . . C22 C -0.3370(2) 0.21662(7) 0.6416(5) 0.0678(13) Uani 1 1 d . . . H22 H -0.3237 0.227 0.7142 0.081 Uiso 1 1 calc R . . C23 C -0.3874(2) 0.21239(8) 0.6353(5) 0.0729(15) Uani 1 1 d . . . H23 H -0.4091 0.2203 0.7014 0.088 Uiso 1 1 calc R . . C24 C -0.40707(17) 0.19664(8) 0.5330(5) 0.0677(13) Uani 1 1 d . . . H24 H -0.442 0.1934 0.53 0.081 Uiso 1 1 calc R . . C25 C -0.37504(15) 0.18569(7) 0.4349(4) 0.0505(10) Uani 1 1 d . . . H25 H -0.3883 0.1748 0.365 0.061 Uiso 1 1 calc R . . C26 C -0.13124(11) 0.23295(5) 0.0402(4) 0.0294(7) Uani 1 1 d . . . C27 C -0.11028(11) 0.24620(5) 0.1541(4) 0.0315(7) Uani 1 1 d . . . C28 C -0.06432(12) 0.25817(5) 0.1339(4) 0.0374(8) Uani 1 1 d . . . H28 H -0.0502 0.2672 0.2108 0.045 Uiso 1 1 calc R . . C29 C -0.03865(12) 0.25733(6) 0.0068(4) 0.0382(9) Uani 1 1 d . . . C30 C -0.06045(12) 0.24443(5) -0.1049(4) 0.0361(8) Uani 1 1 d . . . H30 H -0.0434 0.2437 -0.1934 0.043 Uiso 1 1 calc R . . C31 C -0.10656(12) 0.23250(5) -0.0914(3) 0.0317(8) Uani 1 1 d . . . C32 C -0.13637(13) 0.24748(6) 0.2954(4) 0.0405(8) Uani 1 1 d . . . H32A H -0.1721 0.2509 0.2806 0.061 Uiso 1 1 calc R . . H32B H -0.1215 0.2608 0.3529 0.061 Uiso 1 1 calc R . . H32C H -0.1326 0.2316 0.345 0.061 Uiso 1 1 calc R . . C33 C 0.01138(14) 0.27043(7) -0.0122(5) 0.0584(11) Uani 1 1 d . . . H33A H 0.0083 0.2832 -0.086 0.088 Uiso 0.5 1 calc PR . . H33B H 0.0369 0.2583 -0.0405 0.088 Uiso 0.5 1 calc PR . . H33C H 0.0212 0.2782 0.0777 0.088 Uiso 0.5 1 calc PR . . H33D H 0.036 0.2633 0.0535 0.088 Uiso 0.5 1 calc PR . . H33E H 0.0074 0.2882 0.008 0.088 Uiso 0.5 1 calc PR . . H33F H 0.023 0.2682 -0.1103 0.088 Uiso 0.5 1 calc PR . . C34 C -0.12889(13) 0.21887(6) -0.2166(4) 0.0435(9) Uani 1 1 d . . . H34A H -0.1078 0.2215 -0.3006 0.065 Uiso 1 1 calc R . . H34B H -0.1627 0.2252 -0.2353 0.065 Uiso 1 1 calc R . . H34C H -0.1307 0.2011 -0.1951 0.065 Uiso 1 1 calc R . . C35 C -0.26168(11) 0.13104(5) 0.4187(3) 0.0304(7) Uani 1 1 d . . . C36 C -0.30703(12) 0.12570(6) 0.4870(4) 0.0341(8) Uani 1 1 d . . . H36 H -0.3323 0.1381 0.4918 0.041 Uiso 1 1 calc R . . C37 C -0.31574(12) 0.10268(6) 0.5476(4) 0.0389(8) Uani 1 1 d . . . H37 H -0.3465 0.0997 0.5957 0.047 Uiso 1 1 calc R . . C38 C -0.28027(13) 0.08399(6) 0.5391(4) 0.0407(8) Uani 1 1 d . . . H38 H -0.2866 0.0681 0.5796 0.049 Uiso 1 1 calc R . . C39 C -0.23575(14) 0.08880(6) 0.4712(4) 0.0406(9) Uani 1 1 d . . . H39 H -0.2111 0.0761 0.4645 0.049 Uiso 1 1 calc R . . C40 C -0.22623(12) 0.11188(6) 0.4125(3) 0.0366(8) Uani 1 1 d . . . H40 H -0.195 0.1148 0.3669 0.044 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 0.0326(4) 0.0239(4) 0.0270(4) 0.0008(4) -0.0041(4) -0.0019(3) P2 0.0377(5) 0.0278(4) 0.0289(5) -0.0009(4) 0.0048(4) -0.0002(4) N1 0.0321(14) 0.0271(12) 0.0379(16) 0.0062(13) -0.0044(14) -0.0021(11) N2 0.0348(15) 0.0324(14) 0.0356(17) 0.0003(12) 0.0033(13) 0.0013(11) O 0.064(3) 0.079(3) 0.042(2) 0 0 0.033(2) C1 0.043(2) 0.0285(17) 0.033(2) -0.0019(16) 0.0002(18) -0.0049(15) C2 0.046(2) 0.0201(14) 0.035(2) -0.0033(14) -0.0113(18) -0.0021(14) C3 0.054(2) 0.0393(18) 0.038(2) 0.0080(17) -0.015(2) -0.0093(16) C4 0.090(3) 0.040(2) 0.045(3) 0.0122(18) -0.033(3) -0.010(2) C5 0.060(3) 0.0333(19) 0.082(4) 0.008(2) -0.034(3) -0.0032(17) C6 0.046(2) 0.041(2) 0.074(3) 0.006(2) -0.012(2) 0.0059(17) C7 0.041(2) 0.0304(16) 0.049(2) -0.0016(16) -0.007(2) 0.0037(14) C8 0.0268(17) 0.0303(15) 0.0255(19) 0.0024(14) -0.0005(14) -0.0052(13) C9 0.0310(17) 0.0318(16) 0.031(2) 0.0015(14) -0.0058(15) 0.0009(14) C10 0.0407(19) 0.0296(16) 0.050(2) -0.0085(16) -0.0088(18) -0.0007(15) C11 0.053(2) 0.043(2) 0.039(2) -0.0124(17) -0.016(2) -0.0009(16) C12 0.057(2) 0.047(2) 0.034(2) 0.0016(17) -0.0178(19) -0.0041(17) C13 0.045(2) 0.0320(17) 0.037(2) 0.0007(16) -0.0077(18) -0.0054(15) C14 0.0316(18) 0.0325(16) 0.033(2) 0.0042(15) 0.0052(17) -0.0012(13) C15 0.0316(19) 0.0319(16) 0.042(2) 0.0008(15) 0.0024(17) -0.0043(14) C16 0.046(2) 0.0402(19) 0.055(3) -0.0116(19) -0.005(2) -0.0102(17) C17 0.050(2) 0.062(2) 0.051(3) -0.005(2) -0.015(2) -0.0104(19) C18 0.050(2) 0.052(2) 0.045(3) 0.009(2) -0.008(2) 0.0109(18) C19 0.045(2) 0.0386(18) 0.036(2) 0.0022(16) 0.0027(18) 0.0041(16) C20 0.046(2) 0.0367(17) 0.0268(19) 0.0063(15) 0.0122(17) 0.0080(15) C21 0.080(3) 0.0388(19) 0.032(2) -0.0038(17) 0.004(2) 0.0134(19) C22 0.116(4) 0.051(2) 0.037(2) -0.003(2) 0.004(3) 0.028(3) C23 0.109(4) 0.073(3) 0.037(3) 0.015(3) 0.030(3) 0.049(3) C24 0.072(3) 0.069(3) 0.062(3) 0.028(3) 0.031(3) 0.029(2) C25 0.062(3) 0.048(2) 0.041(2) 0.0081(18) 0.018(2) 0.0117(18) C26 0.0300(18) 0.0235(14) 0.035(2) 0.0057(14) -0.0033(17) 0.0018(13) C27 0.0320(17) 0.0242(14) 0.038(2) 0.0004(14) -0.0015(17) 0.0007(13) C28 0.0385(19) 0.0313(17) 0.042(2) -0.0020(16) -0.0090(19) -0.0035(14) C29 0.0334(19) 0.0320(16) 0.049(2) 0.0066(16) -0.0002(19) -0.0014(14) C30 0.0355(19) 0.0377(16) 0.035(2) 0.0094(17) 0.0016(17) -0.0013(15) C31 0.0366(19) 0.0274(15) 0.031(2) 0.0034(14) -0.0022(17) 0.0033(14) C32 0.046(2) 0.0332(17) 0.042(2) -0.0070(16) 0.0025(19) -0.0032(14) C33 0.046(2) 0.065(2) 0.064(3) 0.002(2) 0.007(2) -0.0192(19) C34 0.047(2) 0.0450(19) 0.039(2) -0.0010(17) 0.0028(19) -0.0026(16) C35 0.0350(19) 0.0309(16) 0.0254(18) -0.0020(14) -0.0043(15) -0.0016(14) C36 0.037(2) 0.0342(16) 0.0312(19) -0.0011(15) 0.0014(17) 0.0020(14) C37 0.0375(19) 0.0387(18) 0.040(2) 0.0001(17) 0.0033(18) -0.0058(15) C38 0.056(2) 0.0332(17) 0.033(2) 0.0036(15) -0.004(2) -0.0032(16) C39 0.048(2) 0.0352(18) 0.039(2) -0.0025(16) -0.0062(19) 0.0087(16) C40 0.0353(19) 0.0403(18) 0.034(2) 0.0007(16) 0.0015(17) 0.0025(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N1 1.573(2) . ? P1 C8 1.807(3) . ? P1 C2 1.808(3) . ? P1 C1 1.816(4) . ? P2 N2 1.555(3) . ? P2 C14 1.808(3) . ? P2 C20 1.819(3) . ? P2 C1 1.820(3) . ? N1 C26 1.421(4) . ? N2 C35 1.401(4) . ? C2 C3 1.389(5) . ? C2 C7 1.393(5) . ? C3 C4 1.394(5) . ? C4 C5 1.374(6) . ? C5 C6 1.365(6) . ? C6 C7 1.381(5) . ? C8 C13 1.386(4) . ? C8 C9 1.394(4) . ? C9 C10 1.387(4) . ? C10 C11 1.379(5) . ? C11 C12 1.362(5) . ? C12 C13 1.382(5) . ? C14 C15 1.388(4) . ? C14 C19 1.391(4) . ? C15 C16 1.382(5) . ? C16 C17 1.379(5) . ? C17 C18 1.376(5) . ? C18 C19 1.374(5) . ? C20 C25 1.389(5) . ? C20 C21 1.394(5) . ? C21 C22 1.385(6) . ? C22 C23 1.367(7) . ? C23 C24 1.385(7) . ? C24 C25 1.389(5) . ? C26 C31 1.401(4) . ? C26 C27 1.403(4) . ? C27 C28 1.398(4) . ? C27 C32 1.501(5) . ? C28 C29 1.378(5) . ? C29 C30 1.387(5) . ? C29 C33 1.520(5) . ? C30 C31 1.394(4) . ? C31 C34 1.510(5) . ? C35 C36 1.400(4) . ? C35 C40 1.401(4) . ? C36 C37 1.384(4) . ? C37 C38 1.383(5) . ? C38 C39 1.373(5) . ? C39 C40 1.383(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 N1 P1 C8 112.27(15) . . ? N1 P1 C2 113.95(14) . . ? C8 P1 C2 105.57(14) . . ? N1 P1 C1 106.37(15) . . ? C8 P1 C1 109.37(15) . . ? C2 P1 C1 109.28(18) . . ? N2 P2 C14 116.45(14) . . ? N2 P2 C20 118.71(15) . . ? C14 P2 C20 104.55(15) . . ? N2 P2 C1 106.95(15) . . ? C14 P2 C1 104.30(16) . . ? C20 P2 C1 104.37(16) . . ? C26 N1 P1 126.4(2) . . ? C35 N2 P2 130.4(2) . . ? P1 C1 P2 122.25(19) . . ? C3 C2 C7 118.9(3) . . ? C3 C2 P1 125.1(3) . . ? C7 C2 P1 115.8(3) . . ? C2 C3 C4 119.6(4) . . ? C5 C4 C3 120.5(4) . . ? C6 C5 C4 120.0(4) . . ? C5 C6 C7 120.4(4) . . ? C6 C7 C2 120.5(4) . . ? C13 C8 C9 118.7(3) . . ? C13 C8 P1 119.6(2) . . ? C9 C8 P1 121.5(2) . . ? C10 C9 C8 120.0(3) . . ? C11 C10 C9 120.3(3) . . ? C12 C11 C10 119.8(3) . . ? C11 C12 C13 120.7(3) . . ? C12 C13 C8 120.4(3) . . ? C15 C14 C19 119.6(3) . . ? C15 C14 P2 119.2(2) . . ? C19 C14 P2 121.1(2) . . ? C16 C15 C14 119.8(3) . . ? C17 C16 C15 119.8(3) . . ? C18 C17 C16 121.0(4) . . ? C19 C18 C17 119.5(3) . . ? C18 C19 C14 120.4(3) . . ? C25 C20 C21 118.6(3) . . ? C25 C20 P2 120.6(3) . . ? C21 C20 P2 120.8(3) . . ? C22 C21 C20 120.1(4) . . ? C23 C22 C21 120.7(4) . . ? C22 C23 C24 120.3(4) . . ? C23 C24 C25 119.2(4) . . ? C24 C25 C20 121.1(4) . . ? C31 C26 C27 119.7(3) . . ? C31 C26 N1 120.0(3) . . ? C27 C26 N1 120.2(3) . . ? C28 C27 C26 118.7(3) . . ? C28 C27 C32 120.4(3) . . ? C26 C27 C32 120.9(3) . . ? C29 C28 C27 122.6(3) . . ? C28 C29 C30 117.7(3) . . ? C28 C29 C33 121.5(3) . . ? C30 C29 C33 120.8(3) . . ? C29 C30 C31 122.2(3) . . ? C30 C31 C26 119.2(3) . . ? C30 C31 C34 120.1(3) . . ? C26 C31 C34 120.7(3) . . ? C36 C35 C40 116.9(3) . . ? C36 C35 N2 125.5(3) . . ? C40 C35 N2 117.6(3) . . ? C37 C36 C35 121.2(3) . . ? C38 C37 C36 120.8(3) . . ? C39 C38 C37 118.8(3) . . ? C38 C39 C40 120.9(3) . . ? C39 C40 C35 121.4(3) . . ? #===END data_msh3-(nov1501) _database_code_CSD 190728 _audit_creation_date 2001-11-27T12:01:23-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[ZnMe{MesNPPh2CHPPh2NMes}].0.25toluene' _chemical_formula_moiety '(C44 H46 N2 P2 Zn1).1/4(C7 H8)' _chemical_formula_sum 'C45.75 H48 N2 P2 Zn' _chemical_formula_weight 753.17 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2619(5) _cell_length_b 18.4588(13) _cell_length_c 20.2548(13) _cell_angle_alpha 112.223(2) _cell_angle_beta 95.261(4) _cell_angle_gamma 92.019(4) _cell_volume 3870.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11282 _cell_measurement_theta_min 4.076 _cell_measurement_theta_max 21.967 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1586 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.15 -1 0 0 0.15 0 1 0 0.01 0 -1 0 0.01 0 0 1 0.05 0 0 -1 0.05 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.752 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; (see. N.W. Alcock (1970). Cryst. Computing, p271) ; _exptl_absorpt_correction_T_min 0.917 _exptl_absorpt_correction_T_max 0.986 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 20269 _diffrn_reflns_av_R_equivalents 0.1039 _diffrn_reflns_av_unetI/netI 0.1259 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.1 _diffrn_reflns_theta_max 21.98 _diffrn_reflns_theta_full 21.98 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 9360 _reflns_number_gt 6313 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The toluene solvate molecule is disordered across an inversion centre and was refined with isotropic C atoms, and H atoms omited. 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^)+(0.0190P)^2^+8.8441P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 9360 _refine_ls_number_parameters 913 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1099 _refine_ls_R_factor_gt 0.0654 _refine_ls_wR_factor_ref 0.1411 _refine_ls_wR_factor_gt 0.1237 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.659 _refine_diff_density_min -0.469 _refine_diff_density_rms 0.082 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Zn Zn 0.38179(6) 0.71583(5) 0.08787(4) 0.0279(2) Uani 1 1 d . A 1 P1 P 0.59484(13) 0.83426(10) 0.18519(9) 0.0239(4) Uani 1 1 d . A 1 P2 P 0.32787(13) 0.85767(10) 0.21603(9) 0.0234(4) Uani 1 1 d . A 1 N1 N 0.5504(4) 0.7612(3) 0.1118(3) 0.0231(13) Uani 1 1 d . A 1 N2 N 0.2864(4) 0.8072(3) 0.1322(3) 0.0267(13) Uani 1 1 d . A 1 C1 C 0.4792(5) 0.8645(4) 0.2363(3) 0.0277(16) Uani 1 1 d . A 1 H1 H 0.5047 0.8903 0.2861 0.033 Uiso 1 1 calc R A 1 C2 C 0.6777(5) 0.9100(4) 0.1662(3) 0.0259(16) Uani 1 1 d . A 1 C3 C 0.6358(6) 0.9839(4) 0.1839(4) 0.0329(17) Uani 1 1 d . A 1 H3 H 0.5642 0.9953 0.206 0.039 Uiso 1 1 calc R A 1 C4 C 0.6984(6) 1.0416(4) 0.1693(4) 0.044(2) Uani 1 1 d . A 1 H4 H 0.6703 1.0925 0.1822 0.053 Uiso 1 1 calc R A 1 C5 C 0.8008(6) 1.0245(5) 0.1363(4) 0.043(2) Uani 1 1 d . A 1 H5 H 0.8434 1.0639 0.1264 0.052 Uiso 1 1 calc R A 1 C6 C 0.8427(6) 0.9511(5) 0.1173(4) 0.0382(19) Uani 1 1 d . A 1 H6 H 0.9143 0.9404 0.095 0.046 Uiso 1 1 calc R A 1 C7 C 0.7812(5) 0.8929(4) 0.1305(4) 0.0334(18) Uani 1 1 d . A 1 H7 H 0.8084 0.8416 0.1157 0.04 Uiso 1 1 calc R A 1 C8 C 0.7036(5) 0.8102(4) 0.2447(3) 0.0282(17) Uani 1 1 d . A 1 C9 C 0.8211(5) 0.8448(4) 0.2663(4) 0.0381(19) Uani 1 1 d . A 1 H9 H 0.8476 0.8852 0.2515 0.046 Uiso 1 1 calc R A 1 C10 C 0.8988(6) 0.8196(5) 0.3096(4) 0.053(2) Uani 1 1 d . A 1 H10 H 0.9783 0.8431 0.3243 0.064 Uiso 1 1 calc R A 1 C11 C 0.8616(6) 0.7609(5) 0.3315(4) 0.052(2) Uani 1 1 d . A 1 H11 H 0.916 0.743 0.3597 0.062 Uiso 1 1 calc R A 1 C12 C 0.7461(6) 0.7285(5) 0.3124(4) 0.047(2) Uani 1 1 d . A 1 H12 H 0.7192 0.6894 0.3287 0.056 Uiso 1 1 calc R A 1 C13 C 0.6686(6) 0.7531(4) 0.2691(4) 0.0332(17) Uani 1 1 d . A 1 H13 H 0.5889 0.7299 0.2558 0.04 Uiso 1 1 calc R A 1 C14 C 0.2690(5) 0.8109(4) 0.2736(3) 0.0234(16) Uani 1 1 d . A 1 C15 C 0.2350(5) 0.7315(4) 0.2460(4) 0.0310(17) Uani 1 1 d . A 1 H15 H 0.2376 0.7009 0.1965 0.037 Uiso 1 1 calc R A 1 C16 C 0.1969(6) 0.6966(5) 0.2914(5) 0.045(2) Uani 1 1 d . A 1 H16 H 0.1737 0.642 0.2725 0.054 Uiso 1 1 calc R A 1 C17 C 0.1925(6) 0.7393(6) 0.3620(4) 0.045(2) Uani 1 1 d . A 1 H17 H 0.1644 0.7148 0.3918 0.054 Uiso 1 1 calc R A 1 C18 C 0.2282(6) 0.8181(6) 0.3908(4) 0.049(2) Uani 1 1 d . A 1 H18 H 0.2273 0.848 0.4405 0.058 Uiso 1 1 calc R A 1 C19 C 0.2657(6) 0.8531(5) 0.3457(4) 0.0407(19) Uani 1 1 d . A 1 H19 H 0.2896 0.9076 0.3651 0.049 Uiso 1 1 calc R A 1 C20 C 0.2592(5) 0.9498(4) 0.2479(3) 0.0258(16) Uani 1 1 d . A 1 C21 C 0.3277(6) 1.0207(4) 0.2858(3) 0.0321(17) Uani 1 1 d . A 1 H21 H 0.4125 1.0214 0.2909 0.039 Uiso 1 1 calc R A 1 C22 C 0.2733(6) 1.0895(4) 0.3158(4) 0.0399(19) Uani 1 1 d . A 1 H22 H 0.3208 1.137 0.3423 0.048 Uiso 1 1 calc R A 1 C23 C 0.1497(8) 1.0902(5) 0.3075(4) 0.052(2) Uani 1 1 d . A 1 H23 H 0.1126 1.1379 0.3277 0.062 Uiso 1 1 calc R A 1 C24 C 0.0815(7) 1.0208(5) 0.2695(4) 0.051(2) Uani 1 1 d . A 1 H24 H -0.0031 1.0212 0.2634 0.061 Uiso 1 1 calc R A 1 C25 C 0.1334(6) 0.9511(4) 0.2403(4) 0.0358(18) Uani 1 1 d . A 1 H25 H 0.0847 0.9037 0.2149 0.043 Uiso 1 1 calc R A 1 C26 C 0.6184(5) 0.7279(4) 0.0505(3) 0.0263(16) Uani 1 1 d . A 1 C27 C 0.6072(5) 0.7537(4) -0.0058(3) 0.0277(16) Uani 1 1 d . A 1 C28 C 0.6649(5) 0.7166(4) -0.0667(4) 0.0313(17) Uani 1 1 d . A 1 H28 H 0.6569 0.735 -0.1047 0.038 Uiso 1 1 calc R A 1 C29 C 0.7332(5) 0.6538(4) -0.0736(3) 0.0289(17) Uani 1 1 d . A 1 C30 C 0.7414(5) 0.6281(4) -0.0168(4) 0.0320(18) Uani 1 1 d . A 1 H30 H 0.788 0.5852 -0.0202 0.038 Uiso 1 1 calc R A 1 C31 C 0.6843(5) 0.6626(4) 0.0447(4) 0.0296(17) Uani 1 1 d . A 1 C32 C 0.5305(6) 0.8204(4) -0.0037(4) 0.0369(18) Uani 1 1 d . A 1 H32A H 0.4519 0.811 0.0099 0.055 Uiso 1 1 calc R A 1 H32B H 0.5207 0.8232 -0.0512 0.055 Uiso 1 1 calc R A 1 H32C H 0.5694 0.87 0.0316 0.055 Uiso 1 1 calc R A 1 C33 C 0.7945(6) 0.6154(5) -0.1388(4) 0.047(2) Uani 1 1 d . A 1 H33A H 0.8382 0.5724 -0.134 0.07 Uiso 0.5 1 calc PR A 1 H33B H 0.8507 0.654 -0.1443 0.07 Uiso 0.5 1 calc PR A 1 H33C H 0.735 0.5946 -0.1812 0.07 Uiso 0.5 1 calc PR A 1 H33D H 0.7777 0.6416 -0.1723 0.07 Uiso 0.5 1 calc PR A 1 H33E H 0.7652 0.56 -0.162 0.07 Uiso 0.5 1 calc PR A 1 H33F H 0.881 0.6194 -0.1251 0.07 Uiso 0.5 1 calc PR A 1 C34 C 0.6929(6) 0.6285(4) 0.1017(4) 0.0387(19) Uani 1 1 d . A 1 H34A H 0.7116 0.5736 0.0804 0.058 Uiso 1 1 calc R A 1 H34B H 0.6164 0.6315 0.1217 0.058 Uiso 1 1 calc R A 1 H34C H 0.7562 0.6583 0.1399 0.058 Uiso 1 1 calc R A 1 C35 C 0.1970(5) 0.8266(4) 0.0872(3) 0.0261(16) Uani 1 1 d . A 1 C36 C 0.2167(5) 0.8886(4) 0.0652(3) 0.0282(17) Uani 1 1 d . A 1 C37 C 0.1310(6) 0.8995(4) 0.0152(4) 0.0328(18) Uani 1 1 d . A 1 H37 H 0.1453 0.9416 0.0001 0.039 Uiso 1 1 calc R A 1 C38 C 0.0278(6) 0.8520(4) -0.0123(4) 0.0334(18) Uani 1 1 d . A 1 C39 C 0.0060(5) 0.7919(4) 0.0120(3) 0.0339(18) Uani 1 1 d . A 1 H39 H -0.0664 0.7594 -0.0055 0.041 Uiso 1 1 calc R A 1 C40 C 0.0882(5) 0.7786(4) 0.0616(3) 0.0256(16) Uani 1 1 d . A 1 C41 C 0.3274(5) 0.9462(4) 0.0924(4) 0.0344(18) Uani 1 1 d . A 1 H41A H 0.3079 0.9947 0.1302 0.052 Uiso 1 1 calc R A 1 H41B H 0.354 0.9582 0.0527 0.052 Uiso 1 1 calc R A 1 H41C H 0.3913 0.9228 0.1119 0.052 Uiso 1 1 calc R A 1 C42 C -0.0630(6) 0.8626(5) -0.0678(4) 0.048(2) Uani 1 1 d . A 1 H42A H -0.1301 0.8228 -0.0804 0.072 Uiso 0.5 1 calc PR A 1 H42B H -0.0248 0.8569 -0.1109 0.072 Uiso 0.5 1 calc PR A 1 H42C H -0.0925 0.915 -0.0479 0.072 Uiso 0.5 1 calc PR A 1 H42D H -0.0349 0.907 -0.0791 0.072 Uiso 0.5 1 calc PR A 1 H42E H -0.1401 0.8729 -0.0485 0.072 Uiso 0.5 1 calc PR A 1 H42F H -0.0724 0.8148 -0.1116 0.072 Uiso 0.5 1 calc PR A 1 C43 C 0.0577(6) 0.7138(4) 0.0873(4) 0.0388(19) Uani 1 1 d . A 1 H43A H 0.1161 0.6741 0.0733 0.058 Uiso 1 1 calc R A 1 H43B H -0.0226 0.6894 0.0657 0.058 Uiso 1 1 calc R A 1 H43C H 0.0598 0.7359 0.1397 0.058 Uiso 1 1 calc R A 1 C44 C 0.3413(6) 0.6054(4) 0.0322(4) 0.050(2) Uani 1 1 d . A 1 H44A H 0.2981 0.5987 -0.0142 0.074 Uiso 1 1 calc R A 1 H44B H 0.2906 0.5838 0.0582 0.074 Uiso 1 1 calc R A 1 H44C H 0.4147 0.5778 0.0244 0.074 Uiso 1 1 calc R A 1 Zn1B Zn 0.82538(6) 0.31307(5) 0.31524(4) 0.0252(2) Uani 1 1 d . B 2 P1B P 0.66370(13) 0.38111(10) 0.44677(9) 0.0230(4) Uani 1 1 d . B 2 P2B P 0.61088(13) 0.40169(10) 0.30650(9) 0.0223(4) Uani 1 1 d . B 2 N1B N 0.7502(4) 0.3158(3) 0.4018(3) 0.0246(13) Uani 1 1 d . B 2 N2B N 0.7358(4) 0.3758(3) 0.2726(3) 0.0234(13) Uani 1 1 d . B 2 C1B C 0.6173(5) 0.4341(4) 0.3973(3) 0.0230(15) Uani 1 1 d . B 2 H1B H 0.5935 0.4854 0.4223 0.028 Uiso 1 1 calc R B 2 C2B C 0.7356(5) 0.4502(4) 0.5338(3) 0.0232(15) Uani 1 1 d . B 2 C3B C 0.8124(6) 0.5139(4) 0.5373(4) 0.0387(19) Uani 1 1 d . B 2 H3B H 0.8206 0.5233 0.4949 0.046 Uiso 1 1 calc R B 2 C4B C 0.8757(6) 0.5627(4) 0.6012(4) 0.042(2) Uani 1 1 d . B 2 H4B H 0.9266 0.6055 0.6025 0.051 Uiso 1 1 calc R B 2 C5B C 0.8656(6) 0.5498(4) 0.6633(4) 0.0337(18) Uani 1 1 d . B 2 H5B H 0.9104 0.583 0.7071 0.04 Uiso 1 1 calc R B 2 C6B C 0.7909(6) 0.4892(4) 0.6614(4) 0.0326(17) Uani 1 1 d . B 2 H6B H 0.7836 0.4805 0.7043 0.039 Uiso 1 1 calc R B 2 C7B C 0.7255(6) 0.4400(4) 0.5979(4) 0.0309(17) Uani 1 1 d . B 2 H7B H 0.673 0.3986 0.5979 0.037 Uiso 1 1 calc R B 2 C8B C 0.5417(5) 0.3333(4) 0.4726(3) 0.0262(16) Uani 1 1 d . B 2 C9B C 0.4244(5) 0.3519(4) 0.4605(3) 0.0332(18) Uani 1 1 d . B 2 H9B H 0.409 0.3892 0.4394 0.04 Uiso 1 1 calc R B 2 C10B C 0.3304(6) 0.3156(5) 0.4794(4) 0.046(2) Uani 1 1 d . B 2 H10B H 0.2506 0.3271 0.4698 0.055 Uiso 1 1 calc R B 2 C11B C 0.3511(6) 0.2639(5) 0.5114(4) 0.048(2) Uani 1 1 d . B 2 H11B H 0.2857 0.2399 0.524 0.058 Uiso 1 1 calc R B 2 C12B C 0.4658(6) 0.2455(4) 0.5259(4) 0.042(2) Uani 1 1 d . B 2 H12B H 0.4802 0.2097 0.5487 0.05 Uiso 1 1 calc R B 2 C13B C 0.5595(6) 0.2808(4) 0.5061(4) 0.0342(18) Uani 1 1 d . B 2 H13B H 0.6388 0.2686 0.5158 0.041 Uiso 1 1 calc R B 2 C14B C 0.5486(5) 0.4718(4) 0.2734(3) 0.0217(15) Uani 1 1 d . B 2 C15B C 0.5210(5) 0.5466(4) 0.3175(4) 0.0309(17) Uani 1 1 d . B 2 H15B H 0.5337 0.5627 0.3682 0.037 Uiso 1 1 calc R B 2 C16B C 0.4746(6) 0.5976(4) 0.2873(4) 0.0357(18) Uani 1 1 d . B 2 H16B H 0.4564 0.6485 0.3176 0.043 Uiso 1 1 calc R B 2 C17B C 0.4552(6) 0.5746(4) 0.2139(4) 0.0345(18) Uani 1 1 d . B 2 H17B H 0.4231 0.6095 0.1936 0.041 Uiso 1 1 calc R B 2 C18B C 0.4827(6) 0.5007(4) 0.1698(4) 0.0356(18) Uani 1 1 d . B 2 H18B H 0.47 0.485 0.1191 0.043 Uiso 1 1 calc R B 2 C19B C 0.5284(5) 0.4498(4) 0.1989(4) 0.0324(18) Uani 1 1 d . B 2 H19B H 0.5464 0.3991 0.1681 0.039 Uiso 1 1 calc R B 2 C20B C 0.5029(5) 0.3166(4) 0.2668(3) 0.0231(15) Uani 1 1 d . B 2 C21B C 0.3850(5) 0.3254(4) 0.2840(4) 0.0361(18) Uani 1 1 d . B 2 H21B H 0.3643 0.375 0.3159 0.043 Uiso 1 1 calc R B 2 C22B C 0.2991(6) 0.2641(5) 0.2560(4) 0.041(2) Uani 1 1 d . B 2 H22B H 0.2192 0.2718 0.2671 0.049 Uiso 1 1 calc R B 2 C23B C 0.3286(6) 0.1910(5) 0.2114(4) 0.0397(19) Uani 1 1 d . B 2 H23B H 0.2695 0.1482 0.1934 0.048 Uiso 1 1 calc R B 2 C24B C 0.4446(6) 0.1800(4) 0.1927(4) 0.0353(18) Uani 1 1 d . B 2 H24B H 0.4652 0.1301 0.1615 0.042 Uiso 1 1 calc R B 2 C25B C 0.5304(5) 0.2441(4) 0.2210(3) 0.0259(16) Uani 1 1 d . B 2 H25B H 0.6095 0.2373 0.2081 0.031 Uiso 1 1 calc R B 2 C26B C 0.7972(5) 0.2541(4) 0.4219(3) 0.0285(17) Uani 1 1 d . B 2 C27B C 0.9079(6) 0.2655(5) 0.4639(3) 0.0317(18) Uani 1 1 d . B 2 C28B C 0.9602(6) 0.2027(6) 0.4718(4) 0.048(2) Uani 1 1 d . B 2 H28B H 1.0346 0.2119 0.5009 0.057 Uiso 1 1 calc R B 2 C29B C 0.9084(8) 0.1264(6) 0.4390(5) 0.054(2) Uani 1 1 d . B 2 C30B C 0.8005(8) 0.1161(5) 0.3980(4) 0.052(2) Uani 1 1 d . B 2 H30B H 0.764 0.0643 0.3744 0.062 Uiso 1 1 calc R B 2 C31B C 0.7421(6) 0.1768(4) 0.3891(4) 0.0358(18) Uani 1 1 d . B 2 C32B C 0.9710(5) 0.3461(5) 0.5011(4) 0.045(2) Uani 1 1 d . B 2 H32D H 0.9389 0.3731 0.5468 0.068 Uiso 1 1 calc R B 2 H32E H 0.9584 0.3762 0.4706 0.068 Uiso 1 1 calc R B 2 H32F H 1.0568 0.3414 0.5102 0.068 Uiso 1 1 calc R B 2 C33B C 0.9705(9) 0.0585(6) 0.4487(6) 0.092(4) Uani 1 1 d . B 2 H33G H 1.0461 0.0786 0.4797 0.139 Uiso 0.5 1 calc PR B 2 H33H H 0.9866 0.0208 0.4018 0.139 Uiso 0.5 1 calc PR B 2 H33I H 0.9188 0.0325 0.4708 0.139 Uiso 0.5 1 calc PR B 2 H33J H 0.9216 0.0093 0.4218 0.139 Uiso 0.5 1 calc PR B 2 H33K H 0.9811 0.0671 0.4997 0.139 Uiso 0.5 1 calc PR B 2 H33L H 1.0489 0.0554 0.4307 0.139 Uiso 0.5 1 calc PR B 2 C34B C 0.6241(7) 0.1618(5) 0.3434(4) 0.057(2) Uani 1 1 d . B 2 H34D H 0.5852 0.1116 0.339 0.085 Uiso 1 1 calc R B 2 H34E H 0.6372 0.1598 0.2956 0.085 Uiso 1 1 calc R B 2 H34F H 0.5728 0.2041 0.3656 0.085 Uiso 1 1 calc R B 2 C35B C 0.7959(5) 0.4115(4) 0.2318(3) 0.0252(16) Uani 1 1 d . B 2 C36B C 0.8452(5) 0.4906(4) 0.2638(4) 0.0281(17) Uani 1 1 d . B 2 C37B C 0.9023(5) 0.5226(4) 0.2213(4) 0.0349(18) Uani 1 1 d . B 2 H37B H 0.9336 0.5758 0.2427 0.042 Uiso 1 1 calc R B 2 C38B C 0.9152(6) 0.4811(5) 0.1506(4) 0.0363(19) Uani 1 1 d . B 2 C39B C 0.8713(6) 0.4026(5) 0.1213(4) 0.0375(19) Uani 1 1 d . B 2 H39B H 0.8835 0.3715 0.0732 0.045 Uiso 1 1 calc R B 2 C40B C 0.8099(5) 0.3682(4) 0.1601(4) 0.0303(17) Uani 1 1 d . B 2 C41B C 0.8425(5) 0.5376(4) 0.3414(4) 0.0326(17) Uani 1 1 d . B 2 H41D H 0.8917 0.5871 0.3551 0.049 Uiso 1 1 calc R B 2 H41E H 0.8742 0.5081 0.3695 0.049 Uiso 1 1 calc R B 2 H41F H 0.76 0.5489 0.3508 0.049 Uiso 1 1 calc R B 2 C42B C 0.9766(6) 0.5184(5) 0.1059(4) 0.053(2) Uani 1 1 d . B 2 H42G H 0.9771 0.4795 0.057 0.08 Uiso 0.5 1 calc PR B 2 H42H H 1.059 0.5369 0.1276 0.08 Uiso 0.5 1 calc PR B 2 H42I H 0.933 0.5629 0.1043 0.08 Uiso 0.5 1 calc PR B 2 H42J H 1.0023 0.5734 0.1356 0.08 Uiso 0.5 1 calc PR B 2 H42K H 0.9204 0.5159 0.065 0.08 Uiso 0.5 1 calc PR B 2 H42L H 1.0464 0.4899 0.0883 0.08 Uiso 0.5 1 calc PR B 2 C43B C 0.7612(6) 0.2842(4) 0.1236(4) 0.0398(19) Uani 1 1 d . B 2 H43D H 0.7847 0.2625 0.0749 0.06 Uiso 1 1 calc R B 2 H43E H 0.6738 0.2814 0.1212 0.06 Uiso 1 1 calc R B 2 H43F H 0.7933 0.2539 0.1508 0.06 Uiso 1 1 calc R B 2 C44B C 0.9555(6) 0.2461(4) 0.2807(4) 0.042(2) Uani 1 1 d . B 2 H44D H 0.927 0.191 0.2669 0.063 Uiso 1 1 calc R B 2 H44E H 1.0222 0.2599 0.319 0.063 Uiso 1 1 calc R B 2 H44F H 0.9823 0.2538 0.239 0.063 Uiso 1 1 calc R B 2 C1C C 0.6600(10) 0.9463(7) 0.4587(6) 0.104(4) Uiso 1 1 d . . 3 C2C C 0.6049(18) 0.9494(13) 0.5270(11) 0.081(6) Uiso 0.5 1 d P C 3 C3C C 0.5154(9) 0.9758(6) 0.5477(5) 0.073(3) Uiso 1 1 d . . 3 C4C C 0.4266(19) 1.0042(13) 0.5712(12) 0.085(6) Uiso 0.5 1 d P . 3 C5C C 0.5621(17) 0.9758(12) 0.4808(11) 0.078(6) Uiso 0.5 1 d P . 3 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 Zn 0.0226(4) 0.0259(5) 0.0329(5) 0.0089(4) 0.0030(3) -0.0003(3) P1 0.0169(9) 0.0268(11) 0.0299(11) 0.0127(9) 0.0045(7) 0.0009(7) P2 0.0187(9) 0.0243(11) 0.0288(11) 0.0111(9) 0.0065(7) 0.0020(7) N1 0.013(3) 0.030(4) 0.023(3) 0.007(3) 0.003(2) 0.001(2) N2 0.016(3) 0.034(4) 0.033(3) 0.016(3) 0.004(2) 0.005(2) C1 0.023(4) 0.035(5) 0.020(4) 0.007(3) -0.001(3) 0.001(3) C2 0.018(3) 0.029(5) 0.030(4) 0.012(4) 0.004(3) -0.004(3) C3 0.033(4) 0.023(5) 0.039(5) 0.007(4) 0.008(3) 0.003(3) C4 0.047(5) 0.023(5) 0.064(6) 0.018(4) 0.015(4) -0.005(4) C5 0.044(5) 0.040(5) 0.049(5) 0.019(4) 0.020(4) -0.006(4) C6 0.029(4) 0.048(6) 0.039(5) 0.016(4) 0.015(3) -0.005(4) C7 0.027(4) 0.035(5) 0.039(5) 0.014(4) 0.013(3) 0.003(3) C8 0.022(4) 0.039(5) 0.025(4) 0.014(4) 0.002(3) 0.008(3) C9 0.025(4) 0.048(5) 0.046(5) 0.025(4) 0.000(3) -0.004(3) C10 0.030(4) 0.069(7) 0.058(6) 0.026(5) -0.017(4) -0.003(4) C11 0.037(5) 0.081(7) 0.056(6) 0.048(5) -0.003(4) 0.015(4) C12 0.047(5) 0.051(6) 0.055(5) 0.033(5) 0.011(4) 0.007(4) C13 0.034(4) 0.035(5) 0.033(4) 0.017(4) 0.001(3) -0.002(3) C14 0.015(3) 0.028(5) 0.031(4) 0.016(4) 0.003(3) 0.002(3) C15 0.032(4) 0.028(5) 0.039(5) 0.020(4) 0.005(3) 0.003(3) C16 0.033(4) 0.049(6) 0.072(7) 0.044(5) 0.010(4) 0.007(4) C17 0.028(4) 0.079(7) 0.046(6) 0.042(5) 0.011(4) 0.006(4) C18 0.033(4) 0.073(7) 0.041(5) 0.022(5) 0.013(4) 0.004(4) C19 0.045(4) 0.045(5) 0.036(5) 0.018(4) 0.009(4) 0.000(4) C20 0.022(4) 0.036(5) 0.029(4) 0.020(4) 0.011(3) 0.007(3) C21 0.037(4) 0.030(5) 0.031(4) 0.012(4) 0.009(3) 0.004(4) C22 0.054(5) 0.027(5) 0.038(5) 0.011(4) 0.007(4) 0.007(4) C23 0.073(6) 0.035(6) 0.051(6) 0.017(5) 0.016(4) 0.030(5) C24 0.043(5) 0.065(7) 0.048(5) 0.021(5) 0.013(4) 0.029(5) C25 0.033(4) 0.034(5) 0.042(5) 0.014(4) 0.010(3) 0.012(3) C26 0.018(3) 0.028(4) 0.029(4) 0.007(4) 0.004(3) 0.003(3) C27 0.023(4) 0.030(4) 0.030(4) 0.013(4) -0.001(3) -0.005(3) C28 0.021(4) 0.046(5) 0.030(4) 0.018(4) 0.001(3) 0.000(3) C29 0.018(3) 0.035(5) 0.030(4) 0.008(4) 0.004(3) 0.002(3) C30 0.015(3) 0.033(5) 0.043(5) 0.008(4) 0.007(3) 0.008(3) C31 0.019(3) 0.034(5) 0.037(4) 0.014(4) 0.003(3) -0.001(3) C32 0.038(4) 0.044(5) 0.032(4) 0.019(4) -0.001(3) 0.009(4) C33 0.032(4) 0.058(6) 0.044(5) 0.012(4) 0.012(3) 0.005(4) C34 0.042(4) 0.032(5) 0.040(5) 0.009(4) 0.011(3) 0.013(3) C35 0.024(4) 0.020(4) 0.033(4) 0.006(4) 0.010(3) 0.003(3) C36 0.018(3) 0.027(4) 0.035(4) 0.007(4) 0.006(3) -0.001(3) C37 0.031(4) 0.034(5) 0.042(5) 0.020(4) 0.016(3) 0.013(3) C38 0.029(4) 0.044(5) 0.034(4) 0.020(4) 0.010(3) 0.009(4) C39 0.021(4) 0.042(5) 0.030(4) 0.006(4) -0.003(3) 0.003(3) C40 0.023(4) 0.023(4) 0.031(4) 0.009(3) 0.007(3) 0.004(3) C41 0.034(4) 0.026(5) 0.048(5) 0.019(4) 0.012(3) -0.002(3) C42 0.048(5) 0.058(6) 0.044(5) 0.026(5) -0.004(4) 0.015(4) C43 0.026(4) 0.045(5) 0.045(5) 0.019(4) -0.001(3) -0.006(3) C44 0.036(4) 0.039(5) 0.065(6) 0.013(5) -0.005(4) 0.003(4) Zn1B 0.0199(4) 0.0283(5) 0.0316(5) 0.0150(4) 0.0065(3) 0.0052(3) P1B 0.0178(9) 0.0255(11) 0.0278(10) 0.0122(9) 0.0042(7) 0.0016(7) P2B 0.0174(9) 0.0233(11) 0.0288(11) 0.0122(9) 0.0038(7) 0.0046(7) N1B 0.025(3) 0.023(3) 0.021(3) 0.005(3) 0.001(2) 0.000(2) N2B 0.022(3) 0.023(3) 0.026(3) 0.009(3) 0.006(2) 0.001(2) C1B 0.018(3) 0.025(4) 0.027(4) 0.011(3) 0.002(3) 0.002(3) C2B 0.013(3) 0.025(4) 0.030(4) 0.009(3) 0.002(3) 0.004(3) C3B 0.041(4) 0.041(5) 0.040(5) 0.021(4) 0.010(4) -0.005(4) C4B 0.040(4) 0.039(5) 0.041(5) 0.012(4) -0.001(4) -0.020(4) C5B 0.031(4) 0.042(5) 0.022(4) 0.007(4) -0.001(3) -0.001(3) C6B 0.043(4) 0.032(5) 0.023(4) 0.011(4) 0.003(3) 0.001(4) C7B 0.039(4) 0.024(4) 0.036(5) 0.016(4) 0.010(3) 0.001(3) C8B 0.022(4) 0.025(4) 0.031(4) 0.009(4) 0.009(3) -0.001(3) C9B 0.024(4) 0.040(5) 0.036(4) 0.013(4) 0.008(3) 0.004(3) C10B 0.025(4) 0.070(6) 0.048(5) 0.026(5) 0.011(3) 0.001(4) C11B 0.036(5) 0.059(6) 0.055(6) 0.025(5) 0.020(4) -0.010(4) C12B 0.053(5) 0.036(5) 0.043(5) 0.021(4) 0.013(4) -0.005(4) C13B 0.031(4) 0.031(5) 0.044(5) 0.018(4) 0.008(3) -0.002(3) C14B 0.015(3) 0.022(4) 0.028(4) 0.010(3) 0.005(3) 0.003(3) C15B 0.026(4) 0.039(5) 0.032(4) 0.019(4) 0.004(3) 0.006(3) C16B 0.036(4) 0.026(5) 0.052(6) 0.021(4) 0.014(4) 0.007(3) C17B 0.033(4) 0.031(5) 0.051(5) 0.029(4) 0.001(3) 0.000(3) C18B 0.042(4) 0.037(5) 0.029(4) 0.016(4) -0.003(3) 0.004(4) C19B 0.028(4) 0.032(5) 0.036(5) 0.012(4) 0.003(3) -0.001(3) C20B 0.024(4) 0.023(4) 0.023(4) 0.011(4) 0.001(3) 0.000(3) C21B 0.022(4) 0.045(5) 0.046(5) 0.021(4) 0.007(3) 0.006(3) C22B 0.024(4) 0.052(6) 0.052(5) 0.030(5) 0.000(3) -0.008(4) C23B 0.031(4) 0.040(5) 0.053(5) 0.029(5) -0.013(4) -0.013(4) C24B 0.039(5) 0.030(5) 0.038(5) 0.016(4) -0.001(3) 0.003(4) C25B 0.021(3) 0.032(5) 0.029(4) 0.018(4) -0.004(3) -0.005(3) C26B 0.031(4) 0.036(5) 0.022(4) 0.013(4) 0.010(3) 0.010(3) C27B 0.030(4) 0.052(5) 0.024(4) 0.023(4) 0.015(3) 0.013(4) C28B 0.039(4) 0.086(8) 0.047(5) 0.053(6) 0.014(4) 0.028(5) C29B 0.066(6) 0.070(7) 0.059(6) 0.051(6) 0.037(5) 0.046(5) C30B 0.079(6) 0.032(5) 0.056(6) 0.026(5) 0.023(5) 0.023(5) C31B 0.059(5) 0.026(5) 0.024(4) 0.010(4) 0.007(3) 0.008(4) C32B 0.013(4) 0.082(7) 0.045(5) 0.028(5) 0.006(3) 0.009(4) C33B 0.112(8) 0.099(9) 0.124(9) 0.092(8) 0.061(7) 0.075(7) C34B 0.083(6) 0.032(5) 0.045(5) 0.009(4) -0.012(4) -0.015(4) C35B 0.014(3) 0.041(5) 0.028(4) 0.021(4) 0.005(3) 0.010(3) C36B 0.020(3) 0.032(5) 0.035(5) 0.017(4) 0.000(3) 0.002(3) C37B 0.026(4) 0.036(5) 0.044(5) 0.017(4) 0.001(3) -0.002(3) C38B 0.026(4) 0.049(6) 0.049(5) 0.034(5) 0.008(3) 0.011(4) C39B 0.032(4) 0.057(6) 0.030(4) 0.020(4) 0.016(3) 0.015(4) C40B 0.022(4) 0.041(5) 0.035(5) 0.020(4) 0.009(3) 0.009(3) C41B 0.025(4) 0.028(5) 0.043(5) 0.013(4) -0.003(3) -0.002(3) C42B 0.042(5) 0.076(7) 0.071(6) 0.056(5) 0.027(4) 0.013(4) C43B 0.046(4) 0.038(5) 0.031(5) 0.006(4) 0.014(3) 0.002(4) C44B 0.037(4) 0.040(5) 0.054(5) 0.023(4) 0.009(4) 0.014(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Zn C44 1.932(7) . ? Zn N1 1.988(4) . ? Zn N2 1.992(5) . ? P1 N1 1.606(5) . ? P1 C1 1.715(6) . ? P1 C8 1.823(6) . ? P1 C2 1.831(6) . ? P2 N2 1.611(5) . ? P2 C1 1.705(6) . ? P2 C20 1.806(6) . ? P2 C14 1.845(6) . ? N1 C26 1.462(7) . ? N2 C35 1.441(8) . ? C2 C3 1.385(9) . ? C2 C7 1.410(8) . ? C3 C4 1.392(9) . ? C4 C5 1.373(9) . ? C5 C6 1.374(10) . ? C6 C7 1.382(9) . ? C8 C13 1.383(9) . ? C8 C9 1.405(9) . ? C9 C10 1.396(9) . ? C10 C11 1.382(11) . ? C11 C12 1.371(10) . ? C12 C13 1.387(9) . ? C14 C19 1.376(9) . ? C14 C15 1.382(9) . ? C15 C16 1.394(9) . ? C16 C17 1.353(10) . ? C17 C18 1.374(11) . ? C18 C19 1.389(10) . ? C20 C21 1.399(9) . ? C20 C25 1.413(8) . ? C21 C22 1.378(9) . ? C22 C23 1.387(10) . ? C23 C24 1.378(11) . ? C24 C25 1.375(10) . ? C26 C27 1.389(9) . ? C26 C31 1.410(9) . ? C27 C28 1.399(9) . ? C27 C32 1.518(9) . ? C28 C29 1.384(9) . ? C29 C30 1.398(9) . ? C29 C33 1.489(9) . ? C30 C31 1.394(9) . ? C31 C34 1.508(9) . ? C35 C36 1.395(9) . ? C35 C40 1.420(9) . ? C36 C37 1.409(9) . ? C36 C41 1.525(8) . ? C37 C38 1.368(9) . ? C38 C39 1.395(9) . ? C38 C42 1.523(9) . ? C39 C40 1.400(9) . ? C40 C43 1.516(9) . ? Zn1B N2B 1.946(5) . ? Zn1B C44B 1.956(6) . ? Zn1B N1B 2.001(5) . ? P1B N1B 1.627(5) . ? P1B C1B 1.708(6) . ? P1B C8B 1.827(6) . ? P1B C2B 1.831(6) . ? P2B N2B 1.630(5) . ? P2B C1B 1.698(6) . ? P2B C14B 1.803(6) . ? P2B C20B 1.823(6) . ? N1B C26B 1.448(8) . ? N2B C35B 1.435(8) . ? C2B C7B 1.394(9) . ? C2B C3B 1.410(9) . ? C3B C4B 1.378(9) . ? C4B C5B 1.380(9) . ? C5B C6B 1.363(9) . ? C6B C7B 1.385(9) . ? C8B C13B 1.386(9) . ? C8B C9B 1.400(8) . ? C9B C10B 1.392(9) . ? C10B C11B 1.357(10) . ? C11B C12B 1.380(10) . ? C12B C13B 1.388(9) . ? C14B C15B 1.396(9) . ? C14B C19B 1.400(9) . ? C15B C16B 1.395(9) . ? C16B C17B 1.376(9) . ? C17B C18B 1.384(9) . ? C18B C19B 1.376(9) . ? C20B C25B 1.375(9) . ? C20B C21B 1.403(8) . ? C21B C22B 1.369(10) . ? C22B C23B 1.382(10) . ? C23B C24B 1.395(9) . ? C24B C25B 1.403(9) . ? C26B C27B 1.405(9) . ? C26B C31B 1.416(10) . ? C27B C28B 1.374(10) . ? C27B C32B 1.505(10) . ? C28B C29B 1.389(12) . ? C29B C30B 1.372(11) . ? C29B C33B 1.524(10) . ? C30B C31B 1.380(10) . ? C31B C34B 1.502(10) . ? C35B C40B 1.395(9) . ? C35B C36B 1.421(9) . ? C36B C37B 1.401(9) . ? C36B C41B 1.484(9) . ? C37B C38B 1.370(9) . ? C38B C39B 1.393(10) . ? C38B C42B 1.526(9) . ? C39B C40B 1.395(9) . ? C40B C43B 1.499(9) . ? C1C C5C 1.289(19) . ? C1C C2C 1.55(2) . ? C1C C4C 1.59(2) 2_676 ? C2C C3C 1.18(2) . ? C2C C5C 1.28(3) . ? C3C C4C 1.20(2) . ? C3C C5C 1.50(2) 2_676 ? C3C C5C 1.50(2) . ? C4C C5C 1.26(3) 2_676 ? C4C C1C 1.59(2) 2_676 ? C5C C4C 1.26(3) 2_676 ? C5C C3C 1.50(2) 2_676 ? C5C C5C 1.77(4) 2_676 ? 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 C44 Zn N1 121.7(3) . . ? C44 Zn N2 134.0(3) . . ? N1 Zn N2 104.3(2) . . ? N1 P1 C1 110.8(3) . . ? N1 P1 C8 113.5(3) . . ? C1 P1 C8 102.8(3) . . ? N1 P1 C2 110.1(3) . . ? C1 P1 C2 116.3(3) . . ? C8 P1 C2 103.0(3) . . ? N2 P2 C1 112.3(3) . . ? N2 P2 C20 112.0(3) . . ? C1 P2 C20 115.1(3) . . ? N2 P2 C14 111.7(3) . . ? C1 P2 C14 104.4(3) . . ? C20 P2 C14 100.4(3) . . ? C26 N1 P1 126.2(4) . . ? C26 N1 Zn 111.1(4) . . ? P1 N1 Zn 122.1(3) . . ? C35 N2 P2 126.2(4) . . ? C35 N2 Zn 119.0(4) . . ? P2 N2 Zn 114.5(3) . . ? P2 C1 P1 133.2(4) . . ? C3 C2 C7 119.3(6) . . ? C3 C2 P1 120.0(5) . . ? C7 C2 P1 120.6(5) . . ? C2 C3 C4 120.2(6) . . ? C5 C4 C3 119.7(7) . . ? C4 C5 C6 120.9(7) . . ? C5 C6 C7 120.2(6) . . ? C6 C7 C2 119.6(7) . . ? C13 C8 C9 118.0(6) . . ? C13 C8 P1 117.7(5) . . ? C9 C8 P1 124.3(5) . . ? C10 C9 C8 119.6(7) . . ? C11 C10 C9 120.8(7) . . ? C12 C11 C10 119.9(7) . . ? C11 C12 C13 119.5(7) . . ? C8 C13 C12 122.1(7) . . ? C19 C14 C15 118.7(6) . . ? C19 C14 P2 120.7(5) . . ? C15 C14 P2 120.5(5) . . ? C14 C15 C16 119.4(7) . . ? C17 C16 C15 121.1(8) . . ? C16 C17 C18 120.4(7) . . ? C17 C18 C19 118.7(7) . . ? C14 C19 C18 121.7(7) . . ? C21 C20 C25 118.3(6) . . ? C21 C20 P2 121.2(5) . . ? C25 C20 P2 120.3(5) . . ? C22 C21 C20 120.5(6) . . ? C21 C22 C23 120.7(7) . . ? C24 C23 C22 119.2(7) . . ? C25 C24 C23 121.3(7) . . ? C24 C25 C20 119.9(7) . . ? C27 C26 C31 119.8(6) . . ? C27 C26 N1 120.6(5) . . ? C31 C26 N1 119.1(6) . . ? C26 C27 C28 119.8(6) . . ? C26 C27 C32 121.5(6) . . ? C28 C27 C32 118.7(6) . . ? C29 C28 C27 122.1(6) . . ? C28 C29 C30 116.9(6) . . ? C28 C29 C33 121.3(6) . . ? C30 C29 C33 121.9(6) . . ? C31 C30 C29 123.0(6) . . ? C30 C31 C26 118.3(6) . . ? C30 C31 C34 119.4(6) . . ? C26 C31 C34 122.3(6) . . ? C36 C35 C40 119.1(6) . . ? C36 C35 N2 121.9(6) . . ? C40 C35 N2 118.9(6) . . ? C35 C36 C37 119.2(6) . . ? C35 C36 C41 123.3(6) . . ? C37 C36 C41 117.5(6) . . ? C38 C37 C36 122.6(6) . . ? C37 C38 C39 118.2(6) . . ? C37 C38 C42 122.4(7) . . ? C39 C38 C42 119.5(6) . . ? C38 C39 C40 121.6(6) . . ? C39 C40 C35 119.3(6) . . ? C39 C40 C43 119.0(6) . . ? C35 C40 C43 121.7(6) . . ? N2B Zn1B C44B 130.2(3) . . ? N2B Zn1B N1B 108.3(2) . . ? C44B Zn1B N1B 121.1(3) . . ? N1B P1B C1B 109.0(3) . . ? N1B P1B C8B 109.8(3) . . ? C1B P1B C8B 114.0(3) . . ? N1B P1B C2B 114.0(3) . . ? C1B P1B C2B 107.8(3) . . ? C8B P1B C2B 102.2(3) . . ? N2B P2B C1B 116.2(3) . . ? N2B P2B C14B 109.1(3) . . ? C1B P2B C14B 111.5(3) . . ? N2B P2B C20B 107.2(3) . . ? C1B P2B C20B 108.7(3) . . ? C14B P2B C20B 103.2(3) . . ? C26B N1B P1B 125.9(4) . . ? C26B N1B Zn1B 107.4(4) . . ? P1B N1B Zn1B 126.3(3) . . ? C35B N2B P2B 125.4(4) . . ? C35B N2B Zn1B 118.8(4) . . ? P2B N2B Zn1B 113.4(3) . . ? P2B C1B P1B 124.5(4) . . ? C7B C2B C3B 116.9(6) . . ? C7B C2B P1B 122.9(5) . . ? C3B C2B P1B 120.0(5) . . ? C4B C3B C2B 121.1(6) . . ? C3B C4B C5B 120.4(7) . . ? C6B C5B C4B 119.6(6) . . ? C5B C6B C7B 120.9(6) . . ? C6B C7B C2B 121.1(6) . . ? C13B C8B C9B 117.8(6) . . ? C13B C8B P1B 123.2(4) . . ? C9B C8B P1B 119.0(5) . . ? C10B C9B C8B 119.7(7) . . ? C11B C10B C9B 120.9(6) . . ? C10B C11B C12B 121.1(6) . . ? C11B C12B C13B 118.1(7) . . ? C8B C13B C12B 122.4(6) . . ? C15B C14B C19B 118.5(6) . . ? C15B C14B P2B 123.9(5) . . ? C19B C14B P2B 117.7(5) . . ? C16B C15B C14B 120.1(6) . . ? C17B C16B C15B 120.5(7) . . ? C16B C17B C18B 119.8(6) . . ? C19B C18B C17B 120.3(7) . . ? C18B C19B C14B 120.9(7) . . ? C25B C20B C21B 118.0(6) . . ? C25B C20B P2B 123.8(5) . . ? C21B C20B P2B 118.2(5) . . ? C22B C21B C20B 121.4(7) . . ? C21B C22B C23B 120.0(6) . . ? C22B C23B C24B 120.3(7) . . ? C23B C24B C25B 118.5(7) . . ? C20B C25B C24B 121.7(6) . . ? C27B C26B C31B 118.1(6) . . ? C27B C26B N1B 121.3(6) . . ? C31B C26B N1B 119.7(6) . . ? C28B C27B C26B 120.1(7) . . ? C28B C27B C32B 118.8(7) . . ? C26B C27B C32B 121.1(6) . . ? C27B C28B C29B 122.6(7) . . ? C30B C29B C28B 116.7(7) . . ? C30B C29B C33B 122.7(10) . . ? C28B C29B C33B 120.7(9) . . ? C29B C30B C31B 123.7(8) . . ? C30B C31B C26B 118.9(7) . . ? C30B C31B C34B 121.2(7) . . ? C26B C31B C34B 119.9(6) . . ? C40B C35B C36B 118.8(6) . . ? C40B C35B N2B 120.2(6) . . ? C36B C35B N2B 121.0(6) . . ? C37B C36B C35B 118.6(6) . . ? C37B C36B C41B 120.0(6) . . ? C35B C36B C41B 121.4(6) . . ? C38B C37B C36B 123.3(7) . . ? C37B C38B C39B 117.2(6) . . ? C37B C38B C42B 121.7(7) . . ? C39B C38B C42B 121.1(7) . . ? C38B C39B C40B 122.2(7) . . ? C35B C40B C39B 120.0(7) . . ? C35B C40B C43B 121.2(6) . . ? C39B C40B C43B 118.8(6) . . ? C5C C1C C2C 52.4(12) . . ? C5C C1C C4C 50.4(12) . 2_676 ? C2C C1C C4C 102.6(13) . 2_676 ? C3C C2C C5C 75.1(15) . . ? C3C C2C C1C 128.3(18) . . ? C5C C2C C1C 53.2(12) . . ? C2C C3C C4C 177.5(19) . . ? C2C C3C C5C 127.2(15) . 2_676 ? C4C C3C C5C 54.2(12) . 2_676 ? C2C C3C C5C 55.5(12) . . ? C4C C3C C5C 126.2(15) . . ? C5C C3C C5C 72.3(14) 2_676 . ? C3C C4C C5C 75.1(16) . 2_676 ? C3C C4C C1C 127.4(18) . 2_676 ? C5C C4C C1C 52.3(12) 2_676 2_676 ? C4C C5C C2C 151(2) 2_676 . ? C4C C5C C1C 77.3(16) 2_676 . ? C2C C5C C1C 74.4(15) . . ? C4C C5C C3C 50.7(12) 2_676 2_676 ? C2C C5C C3C 156(2) . 2_676 ? C1C C5C C3C 128.0(18) . 2_676 ? C4C C5C C3C 158(2) 2_676 . ? C2C C5C C3C 49.5(12) . . ? C1C C5C C3C 123.8(18) . . ? C3C C5C C3C 107.7(14) 2_676 . ? C4C C5C C5C 104(2) 2_676 2_676 ? C2C C5C C5C 103(2) . 2_676 ? C1C C5C C5C 174(2) . 2_676 ? C3C C5C C5C 53.9(12) 2_676 2_676 ? C3C C5C C5C 53.9(11) . 2_676 ? #===END data_msh4-(may602) _database_code_CSD 190729 _audit_creation_date 2002-05-08T09:44:44-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; '[Zn(Me)(MesNPPh2CHPPh2NPh)].1/2(toluene)' ; _chemical_formula_moiety '(C41 H40 N2 P2 Zn1).1/2(C7 H8)' _chemical_formula_sum 'C44.50 H44 N2 P2 Zn' _chemical_formula_weight 734.13 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 25.6605(3) _cell_length_b 14.7185(2) _cell_length_c 20.5047(2) _cell_angle_alpha 90 _cell_angle_beta 98.4740(10) _cell_angle_gamma 90 _cell_volume 7659.75(16) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 50380 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.682 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3080 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.758 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7898 _exptl_absorpt_correction_T_max 0.8441 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0623 _diffrn_reflns_av_unetI/netI 0.0522 _diffrn_reflns_number 61498 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 25.66 _diffrn_reflns_theta_full 25.66 _diffrn_measured_fraction_theta_full 0.938 _diffrn_measured_fraction_theta_max 0.938 _reflns_number_total 13600 _reflns_number_gt 9703 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The toluene solvate molecule was poorly defined and was included with the six-membered ring as a rigid body. 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^)+(0.0528P)^2^+18.8165P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 13600 _refine_ls_number_parameters 846 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0894 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1524 _refine_ls_wR_factor_gt 0.1357 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.117 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.073 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Zn1 Zn 0.104817(17) 0.90688(3) 0.25279(2) 0.03155(14) Uani 1 1 d . A 1 P1 P 0.13045(4) 0.96196(7) 0.12362(5) 0.0248(2) Uani 1 1 d . A 1 P2 P 0.02009(4) 0.99839(7) 0.16462(5) 0.0244(2) Uani 1 1 d . A 1 N1 N 0.15705(11) 0.9611(2) 0.19978(14) 0.0263(7) Uani 1 1 d . A 1 N2 N 0.04462(12) 0.9975(2) 0.24250(15) 0.0291(7) Uani 1 1 d . A 1 C1 C 0.06412(14) 0.9439(3) 0.12225(17) 0.0258(8) Uani 1 1 d . A 1 H1 H 0.0495 0.8966 0.0937 0.031 Uiso 1 1 calc R A 1 C2 C 0.15236(15) 1.0623(3) 0.08400(18) 0.0284(9) Uani 1 1 d . A 1 C3 C 0.11715(17) 1.1294(3) 0.0581(2) 0.0391(10) Uani 1 1 d . A 1 H3 H 0.0803 1.1204 0.0566 0.047 Uiso 1 1 calc R A 1 C4 C 0.1358(2) 1.2098(3) 0.0343(2) 0.0504(13) Uani 1 1 d . A 1 H4 H 0.1118 1.256 0.0172 0.061 Uiso 1 1 calc R A 1 C5 C 0.1888(2) 1.2224(3) 0.0355(2) 0.0519(13) Uani 1 1 d . A 1 H5 H 0.2014 1.278 0.02 0.062 Uiso 1 1 calc R A 1 C6 C 0.22414(19) 1.1551(3) 0.0590(2) 0.0475(12) Uani 1 1 d . A 1 H6 H 0.2607 1.1632 0.0579 0.057 Uiso 1 1 calc R A 1 C7 C 0.20613(16) 1.0761(3) 0.0839(2) 0.0389(10) Uani 1 1 d . A 1 H7 H 0.2306 1.0306 0.1013 0.047 Uiso 1 1 calc R A 1 C8 C 0.14875(14) 0.8683(3) 0.07313(18) 0.0285(9) Uani 1 1 d . A 1 C9 C 0.16210(15) 0.8801(3) 0.01043(19) 0.0332(9) Uani 1 1 d . A 1 H9 H 0.1635 0.9395 -0.0074 0.04 Uiso 1 1 calc R A 1 C10 C 0.17343(18) 0.8051(3) -0.0261(2) 0.0468(12) Uani 1 1 d . A 1 H10 H 0.1827 0.8136 -0.0688 0.056 Uiso 1 1 calc R A 1 C11 C 0.17138(18) 0.7190(3) -0.0011(2) 0.0472(12) Uani 1 1 d . A 1 H11 H 0.1795 0.6682 -0.0264 0.057 Uiso 1 1 calc R A 1 C12 C 0.15758(18) 0.7064(3) 0.0605(2) 0.0459(11) Uani 1 1 d . A 1 H12 H 0.1558 0.6468 0.0778 0.055 Uiso 1 1 calc R A 1 C13 C 0.14624(17) 0.7807(3) 0.0974(2) 0.0390(10) Uani 1 1 d . A 1 H13 H 0.1366 0.7715 0.1399 0.047 Uiso 1 1 calc R A 1 C14 C 0.00399(14) 1.1125(3) 0.13482(18) 0.0272(8) Uani 1 1 d . A 1 C15 C 0.02184(14) 1.1882(3) 0.17163(19) 0.0301(9) Uani 1 1 d . A 1 H15 H 0.0394 1.1809 0.2154 0.036 Uiso 1 1 calc R A 1 C16 C 0.01424(16) 1.2742(3) 0.1450(2) 0.0380(10) Uani 1 1 d . A 1 H16 H 0.0261 1.3258 0.1708 0.046 Uiso 1 1 calc R A 1 C17 C -0.01047(16) 1.2856(3) 0.0811(2) 0.0392(10) Uani 1 1 d . A 1 H17 H -0.0152 1.3449 0.0628 0.047 Uiso 1 1 calc R A 1 C18 C -0.02832(16) 1.2106(3) 0.0438(2) 0.0371(10) Uani 1 1 d . A 1 H18 H -0.0456 1.2183 -0.0001 0.045 Uiso 1 1 calc R A 1 C19 C -0.02112(15) 1.1248(3) 0.07001(19) 0.0327(9) Uani 1 1 d . A 1 H19 H -0.0333 1.0735 0.044 0.039 Uiso 1 1 calc R A 1 C20 C -0.04045(14) 0.9321(3) 0.14814(18) 0.0286(9) Uani 1 1 d . A 1 C21 C -0.09036(15) 0.9710(3) 0.13371(19) 0.0374(10) Uani 1 1 d . A 1 H21 H -0.094 1.035 0.1295 0.045 Uiso 1 1 calc R A 1 C22 C -0.13474(17) 0.9159(4) 0.1255(2) 0.0470(12) Uani 1 1 d . A 1 H22 H -0.1687 0.9425 0.1156 0.056 Uiso 1 1 calc R A 1 C23 C -0.12999(18) 0.8233(4) 0.1316(2) 0.0505(13) Uani 1 1 d . A 1 H23 H -0.1606 0.7861 0.1255 0.061 Uiso 1 1 calc R A 1 C24 C -0.08074(19) 0.7844(3) 0.1467(2) 0.0488(12) Uani 1 1 d . A 1 H24 H -0.0775 0.7204 0.1515 0.059 Uiso 1 1 calc R A 1 C25 C -0.03604(17) 0.8386(3) 0.1548(2) 0.0398(10) Uani 1 1 d . A 1 H25 H -0.0022 0.8115 0.165 0.048 Uiso 1 1 calc R A 1 C26 C 0.20779(14) 0.9961(3) 0.22625(18) 0.0280(9) Uani 1 1 d . A 1 C27 C 0.25288(15) 0.9396(3) 0.23279(19) 0.0341(9) Uani 1 1 d . A 1 C28 C 0.30102(15) 0.9761(3) 0.2597(2) 0.0392(11) Uani 1 1 d . A 1 H28 H 0.3313 0.9382 0.2635 0.047 Uiso 1 1 calc R A 1 C29 C 0.30708(15) 1.0650(3) 0.2812(2) 0.0399(11) Uani 1 1 d . A 1 C30 C 0.26235(16) 1.1189(3) 0.2760(2) 0.0397(10) Uani 1 1 d . A 1 H30 H 0.2655 1.1801 0.2909 0.048 Uiso 1 1 calc R A 1 C31 C 0.21252(15) 1.0852(3) 0.24929(19) 0.0335(9) Uani 1 1 d . A 1 C32 C 0.24875(18) 0.8426(3) 0.2110(3) 0.0531(13) Uani 1 1 d . A 1 H32A H 0.281 0.8102 0.229 0.08 Uiso 1 1 calc R A 1 H32B H 0.244 0.8399 0.1627 0.08 Uiso 1 1 calc R A 1 H32C H 0.2185 0.8141 0.2269 0.08 Uiso 1 1 calc R A 1 C33 C 0.36052(17) 1.1019(4) 0.3106(3) 0.0581(14) Uani 1 1 d . A 1 H33A H 0.357 1.1657 0.3228 0.087 Uiso 0.5 1 calc PR A 1 H33B H 0.3848 1.0973 0.278 0.087 Uiso 0.5 1 calc PR A 1 H33C H 0.3743 1.0666 0.3498 0.087 Uiso 0.5 1 calc PR A 1 H33D H 0.3871 1.054 0.3109 0.087 Uiso 0.5 1 calc PR A 1 H33E H 0.3593 1.1224 0.3558 0.087 Uiso 0.5 1 calc PR A 1 H33F H 0.3698 1.1531 0.284 0.087 Uiso 0.5 1 calc PR A 1 C34 C 0.16491(16) 1.1461(3) 0.2457(2) 0.0425(11) Uani 1 1 d . A 1 H34A H 0.1506 1.1576 0.1995 0.064 Uiso 1 1 calc R A 1 H34B H 0.1751 1.2039 0.2677 0.064 Uiso 1 1 calc R A 1 H34C H 0.138 1.1165 0.2677 0.064 Uiso 1 1 calc R A 1 C35 C 0.01892(15) 1.0296(3) 0.29439(18) 0.0278(9) Uani 1 1 d . A 1 C36 C 0.04299(17) 1.0148(3) 0.3587(2) 0.0390(10) Uani 1 1 d . A 1 H36 H 0.0755 0.9829 0.3665 0.047 Uiso 1 1 calc R A 1 C37 C 0.0199(2) 1.0464(3) 0.4122(2) 0.0510(12) Uani 1 1 d . A 1 H37 H 0.0371 1.0367 0.4559 0.061 Uiso 1 1 calc R A 1 C38 C -0.02778(19) 1.0918(3) 0.4019(2) 0.0486(12) Uani 1 1 d . A 1 H38 H -0.0435 1.1127 0.4382 0.058 Uiso 1 1 calc R A 1 C39 C -0.05202(18) 1.1062(3) 0.3388(2) 0.0441(11) Uani 1 1 d . A 1 H39 H -0.0846 1.1378 0.3314 0.053 Uiso 1 1 calc R A 1 C40 C -0.02955(16) 1.0752(3) 0.2852(2) 0.0368(10) Uani 1 1 d . A 1 H40 H -0.0473 1.0851 0.2417 0.044 Uiso 1 1 calc R A 1 C41 C 0.1189(2) 0.7984(4) 0.3072(3) 0.0640(16) Uani 1 1 d . A 1 H41A H 0.0881 0.7844 0.3286 0.096 Uiso 0.5 1 calc PR A 1 H41B H 0.1495 0.8092 0.341 0.096 Uiso 0.5 1 calc PR A 1 H41C H 0.1262 0.7471 0.2795 0.096 Uiso 0.5 1 calc PR A 1 H41D H 0.1544 0.7761 0.3041 0.096 Uiso 0.5 1 calc PR A 1 H41E H 0.093 0.7513 0.2917 0.096 Uiso 0.5 1 calc PR A 1 H41F H 0.1163 0.8134 0.3532 0.096 Uiso 0.5 1 calc PR A 1 Zn1B Zn 0.390522(18) 0.58195(3) 0.25399(2) 0.03744(15) Uani 1 1 d . B 2 P1B P 0.36739(4) 0.50852(7) 0.37726(5) 0.0297(2) Uani 1 1 d . B 2 P2B P 0.47662(4) 0.48578(7) 0.33150(5) 0.0270(2) Uani 1 1 d . B 2 N1B N 0.33868(12) 0.5163(2) 0.30257(15) 0.0311(8) Uani 1 1 d . B 2 N2B N 0.44956(12) 0.4886(2) 0.25483(15) 0.0308(7) Uani 1 1 d . B 2 C1B C 0.43281(15) 0.5364(3) 0.37664(19) 0.0316(9) Uani 1 1 d . B 2 H1B H 0.4462 0.5853 0.4044 0.038 Uiso 1 1 calc R B 2 C2B C 0.35402(16) 0.3996(3) 0.41333(19) 0.0346(10) Uani 1 1 d . B 2 C3B C 0.30328(18) 0.3618(3) 0.4044(2) 0.0475(12) Uani 1 1 d . B 2 H3B H 0.2747 0.3945 0.3807 0.057 Uiso 1 1 calc R B 2 C4B C 0.2948(2) 0.2773(4) 0.4301(2) 0.0564(14) Uani 1 1 d . B 2 H4B H 0.2605 0.2516 0.4231 0.068 Uiso 1 1 calc R B 2 C5B C 0.3353(2) 0.2304(4) 0.4653(3) 0.0626(15) Uani 1 1 d . B 2 H5B H 0.329 0.1723 0.4828 0.075 Uiso 1 1 calc R B 2 C6B C 0.3848(2) 0.2662(4) 0.4756(2) 0.0575(14) Uani 1 1 d . B 2 H6B H 0.4129 0.2333 0.5003 0.069 Uiso 1 1 calc R B 2 C7B C 0.39413(18) 0.3509(3) 0.4498(2) 0.0439(11) Uani 1 1 d . B 2 H7B H 0.4287 0.3758 0.4575 0.053 Uiso 1 1 calc R B 2 C8B C 0.34659(15) 0.5925(3) 0.4339(2) 0.0389(10) Uani 1 1 d . B 2 C9B C 0.32825(18) 0.5691(4) 0.4918(2) 0.0532(13) Uani 1 1 d . B 2 H9B H 0.3263 0.507 0.5038 0.064 Uiso 1 1 calc R B 2 C10B C 0.3128(2) 0.6361(5) 0.5320(3) 0.0718(17) Uani 1 1 d . B 2 H10B H 0.3005 0.6199 0.5719 0.086 Uiso 1 1 calc R B 2 C11B C 0.3151(2) 0.7253(5) 0.5150(3) 0.0748(19) Uani 1 1 d . B 2 H11B H 0.3039 0.7708 0.5427 0.09 Uiso 1 1 calc R B 2 C12B C 0.3335(2) 0.7496(4) 0.4576(3) 0.0712(17) Uani 1 1 d . B 2 H12B H 0.3348 0.8117 0.4455 0.085 Uiso 1 1 calc R B 2 C13B C 0.35015(19) 0.6829(4) 0.4180(3) 0.0563(13) Uani 1 1 d . B 2 H13B H 0.3642 0.6996 0.3793 0.068 Uiso 1 1 calc R B 2 C14B C 0.49511(14) 0.3715(3) 0.35839(19) 0.0290(9) Uani 1 1 d . B 2 C15B C 0.47631(15) 0.2965(3) 0.3211(2) 0.0357(10) Uani 1 1 d . B 2 H15B H 0.4565 0.3047 0.2786 0.043 Uiso 1 1 calc R B 2 C16B C 0.48646(17) 0.2096(3) 0.3460(2) 0.0454(11) Uani 1 1 d . B 2 H16B H 0.4737 0.1584 0.3203 0.055 Uiso 1 1 calc R B 2 C17B C 0.51476(18) 0.1971(3) 0.4076(3) 0.0504(12) Uani 1 1 d . B 2 H17B H 0.5214 0.1373 0.4244 0.06 Uiso 1 1 calc R B 2 C18B C 0.53359(18) 0.2709(3) 0.4453(2) 0.0492(12) Uani 1 1 d . B 2 H18B H 0.553 0.2619 0.4879 0.059 Uiso 1 1 calc R B 2 C19B C 0.52429(16) 0.3582(3) 0.4208(2) 0.0389(10) Uani 1 1 d . B 2 H19B H 0.5378 0.409 0.4465 0.047 Uiso 1 1 calc R B 2 C20B C 0.53615(15) 0.5543(3) 0.34720(18) 0.0299(9) Uani 1 1 d . B 2 C21B C 0.58676(15) 0.5173(3) 0.35628(19) 0.0351(10) Uani 1 1 d . B 2 H21B H 0.5914 0.4532 0.3568 0.042 Uiso 1 1 calc R B 2 C22B C 0.63026(16) 0.5742(3) 0.3645(2) 0.0440(11) Uani 1 1 d . B 2 H22B H 0.6648 0.5492 0.3702 0.053 Uiso 1 1 calc R B 2 C23B C 0.62354(18) 0.6673(3) 0.3645(2) 0.0465(12) Uani 1 1 d . B 2 H23B H 0.6535 0.7059 0.3714 0.056 Uiso 1 1 calc R B 2 C24B C 0.57395(18) 0.7044(3) 0.3544(2) 0.0491(12) Uani 1 1 d . B 2 H24B H 0.5695 0.7685 0.3536 0.059 Uiso 1 1 calc R B 2 C25B C 0.53047(17) 0.6479(3) 0.3456(2) 0.0413(10) Uani 1 1 d . B 2 H25B H 0.4962 0.6737 0.3382 0.05 Uiso 1 1 calc R B 2 C26B C 0.28787(14) 0.4830(3) 0.27434(18) 0.0295(9) Uani 1 1 d . B 2 C27B C 0.24217(15) 0.5349(3) 0.2752(2) 0.0351(10) Uani 1 1 d . B 2 C28B C 0.19371(16) 0.5010(3) 0.2445(2) 0.0405(11) Uani 1 1 d . B 2 H28B H 0.163 0.5369 0.245 0.049 Uiso 1 1 calc R B 2 C29B C 0.18895(16) 0.4184(3) 0.2138(2) 0.0434(11) Uani 1 1 d . B 2 C30B C 0.23497(17) 0.3677(3) 0.2121(2) 0.0433(11) Uani 1 1 d . B 2 H30B H 0.2326 0.3104 0.1905 0.052 Uiso 1 1 calc R B 2 C31B C 0.28428(15) 0.3994(3) 0.2416(2) 0.0354(10) Uani 1 1 d . B 2 C32B C 0.24463(18) 0.6265(3) 0.3089(3) 0.0522(13) Uani 1 1 d . B 2 H32D H 0.2113 0.6588 0.2961 0.078 Uiso 1 1 calc R B 2 H32E H 0.2736 0.6622 0.2957 0.078 Uiso 1 1 calc R B 2 H32F H 0.2506 0.618 0.3569 0.078 Uiso 1 1 calc R B 2 C33B C 0.13572(18) 0.3827(4) 0.1835(3) 0.0589(14) Uani 1 1 d . B 2 H33G H 0.14 0.323 0.1638 0.088 Uiso 0.5 1 calc PR B 2 H33H H 0.1197 0.4248 0.1493 0.088 Uiso 0.5 1 calc PR B 2 H33I H 0.1129 0.3772 0.2177 0.088 Uiso 0.5 1 calc PR B 2 H33J H 0.1084 0.427 0.19 0.088 Uiso 0.5 1 calc PR B 2 H33K H 0.1287 0.3251 0.2046 0.088 Uiso 0.5 1 calc PR B 2 H33L H 0.1355 0.3728 0.1362 0.088 Uiso 0.5 1 calc PR B 2 C34B C 0.33273(17) 0.3432(3) 0.2373(2) 0.0489(12) Uani 1 1 d . B 2 H34D H 0.355 0.3745 0.2095 0.073 Uiso 1 1 calc R B 2 H34E H 0.3222 0.2838 0.2181 0.073 Uiso 1 1 calc R B 2 H34F H 0.3525 0.3347 0.2816 0.073 Uiso 1 1 calc R B 2 C35B C 0.47213(17) 0.4589(3) 0.2004(2) 0.0359(10) Uani 1 1 d . B 2 C36B C 0.4430(2) 0.4701(3) 0.1382(2) 0.0483(12) Uani 1 1 d . B 2 H36B H 0.409 0.4973 0.1338 0.058 Uiso 1 1 calc R B 2 C37B C 0.4636(3) 0.4414(4) 0.0817(2) 0.0713(18) Uani 1 1 d . B 2 H37B H 0.4433 0.4498 0.0395 0.086 Uiso 1 1 calc R B 2 C38B C 0.5120(3) 0.4018(4) 0.0861(3) 0.0748(19) Uani 1 1 d . B 2 H38B H 0.5254 0.3828 0.0476 0.09 Uiso 1 1 calc R B 2 C39B C 0.5412(2) 0.3901(4) 0.1475(3) 0.0634(15) Uani 1 1 d . B 2 H39B H 0.5749 0.3623 0.1511 0.076 Uiso 1 1 calc R B 2 C40B C 0.52187(18) 0.4183(3) 0.2044(2) 0.0456(11) Uani 1 1 d . B 2 H40B H 0.5427 0.4099 0.2463 0.055 Uiso 1 1 calc R B 2 C41B C 0.3803(2) 0.6985(4) 0.2081(3) 0.0737(18) Uani 1 1 d . B 2 H41G H 0.412 0.7137 0.1889 0.111 Uiso 0.5 1 calc PR B 2 H41H H 0.3738 0.746 0.2394 0.111 Uiso 0.5 1 calc PR B 2 H41I H 0.3501 0.6943 0.173 0.111 Uiso 0.5 1 calc PR B 2 H41J H 0.3452 0.7223 0.212 0.111 Uiso 0.5 1 calc PR B 2 H41K H 0.3834 0.69 0.1614 0.111 Uiso 0.5 1 calc PR B 2 H41L H 0.4071 0.7417 0.2279 0.111 Uiso 0.5 1 calc PR B 2 C1C C 0.25015(19) 0.9905(3) 0.5413(2) 0.098(2) Uiso 1 1 d G C 3 C2C C 0.27310(17) 0.9831(4) 0.4842(3) 0.157(4) Uiso 1 1 d G C 3 H2C H 0.3082 0.9614 0.4865 0.188 Uiso 1 1 calc R C 3 C3C C 0.2447(2) 1.0074(4) 0.4237(2) 0.117(3) Uiso 1 1 d G C 3 H3C H 0.2604 1.0023 0.3847 0.14 Uiso 1 1 calc R C 3 C4C C 0.1934(2) 1.0392(4) 0.4203(2) 0.139(3) Uiso 1 1 d G C 3 H4C H 0.174 1.0558 0.3789 0.166 Uiso 1 1 calc R C 3 C5C C 0.17042(16) 1.0467(4) 0.4773(3) 0.111(3) Uiso 1 1 d G C 3 H5C H 0.1353 1.0684 0.475 0.134 Uiso 1 1 calc R C 3 C6C C 0.19881(19) 1.0223(4) 0.5379(2) 0.113(3) Uiso 1 1 d G C 3 H6C H 0.1831 1.0274 0.5769 0.135 Uiso 1 1 calc R C 3 C7C C 0.2942(2) 0.9886(5) 0.5899(3) 0.220(6) Uiso 1 1 d G C 3 H7C1 H 0.283 0.9935 0.6334 0.33 Uiso 0.5 1 calc PR C 3 H7C2 H 0.3174 1.0397 0.5834 0.33 Uiso 0.5 1 calc PR C 3 H7C3 H 0.3132 0.9314 0.587 0.33 Uiso 0.5 1 calc PR C 3 H7C4 H 0.3261 0.9829 0.5691 0.33 Uiso 0.5 1 calc PR C 3 H7C5 H 0.2917 0.9367 0.6191 0.33 Uiso 0.5 1 calc PR C 3 H7C6 H 0.2959 1.045 0.6155 0.33 Uiso 0.5 1 calc PR C 3 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 Zn1 0.0284(3) 0.0349(3) 0.0330(3) 0.0103(2) 0.00997(19) 0.0061(2) P1 0.0247(5) 0.0244(5) 0.0272(5) 0.0011(4) 0.0098(4) 0.0023(4) P2 0.0219(5) 0.0265(5) 0.0256(5) -0.0002(4) 0.0059(4) 0.0022(4) N1 0.0226(16) 0.0308(18) 0.0262(16) 0.0018(14) 0.0059(13) 0.0023(14) N2 0.0286(17) 0.0333(19) 0.0263(17) 0.0006(14) 0.0075(13) 0.0046(14) C1 0.027(2) 0.025(2) 0.0260(19) -0.0061(16) 0.0061(15) -0.0017(16) C2 0.032(2) 0.029(2) 0.0253(19) -0.0003(16) 0.0094(16) 0.0008(17) C3 0.041(2) 0.038(3) 0.042(2) 0.007(2) 0.021(2) 0.008(2) C4 0.070(3) 0.035(3) 0.052(3) 0.018(2) 0.028(2) 0.016(2) C5 0.076(4) 0.036(3) 0.047(3) 0.004(2) 0.021(3) -0.015(3) C6 0.046(3) 0.053(3) 0.045(3) 0.008(2) 0.010(2) -0.019(2) C7 0.033(2) 0.043(3) 0.040(2) 0.010(2) 0.0051(18) -0.005(2) C8 0.026(2) 0.028(2) 0.033(2) -0.0016(17) 0.0102(16) 0.0002(16) C9 0.029(2) 0.037(2) 0.035(2) -0.0037(19) 0.0086(17) -0.0001(18) C10 0.048(3) 0.059(3) 0.036(2) -0.012(2) 0.015(2) -0.004(2) C11 0.049(3) 0.042(3) 0.054(3) -0.018(2) 0.019(2) 0.005(2) C12 0.051(3) 0.031(3) 0.059(3) -0.005(2) 0.016(2) 0.005(2) C13 0.046(3) 0.034(3) 0.041(2) 0.0003(19) 0.018(2) 0.005(2) C14 0.0216(19) 0.028(2) 0.034(2) 0.0010(17) 0.0089(16) 0.0047(16) C15 0.024(2) 0.033(2) 0.032(2) -0.0011(18) 0.0012(16) 0.0021(17) C16 0.032(2) 0.031(2) 0.050(3) -0.004(2) 0.0044(19) -0.0034(18) C17 0.039(2) 0.028(2) 0.050(3) 0.009(2) 0.004(2) 0.0060(19) C18 0.038(2) 0.039(3) 0.034(2) 0.007(2) 0.0021(18) 0.0054(19) C19 0.031(2) 0.036(2) 0.031(2) -0.0015(18) 0.0035(17) -0.0002(18) C20 0.025(2) 0.035(2) 0.027(2) -0.0010(17) 0.0067(15) -0.0023(17) C21 0.030(2) 0.049(3) 0.034(2) 0.001(2) 0.0056(17) -0.0028(19) C22 0.026(2) 0.069(4) 0.045(3) 0.008(2) 0.0046(19) -0.005(2) C23 0.040(3) 0.069(4) 0.041(3) 0.010(2) 0.002(2) -0.024(3) C24 0.057(3) 0.041(3) 0.048(3) 0.006(2) 0.005(2) -0.020(2) C25 0.038(2) 0.040(3) 0.043(2) 0.003(2) 0.0098(19) -0.004(2) C26 0.0228(19) 0.036(2) 0.026(2) 0.0054(17) 0.0080(15) 0.0027(17) C27 0.031(2) 0.038(3) 0.035(2) 0.0075(18) 0.0099(17) 0.0063(18) C28 0.023(2) 0.055(3) 0.039(2) 0.010(2) 0.0061(18) 0.010(2) C29 0.026(2) 0.059(3) 0.034(2) 0.001(2) 0.0041(17) -0.001(2) C30 0.036(2) 0.046(3) 0.036(2) -0.005(2) 0.0030(18) -0.004(2) C31 0.029(2) 0.044(3) 0.028(2) -0.0005(19) 0.0050(16) 0.0043(18) C32 0.037(3) 0.035(3) 0.088(4) 0.005(3) 0.011(2) 0.012(2) C33 0.031(2) 0.086(4) 0.055(3) -0.007(3) -0.003(2) -0.003(2) C34 0.038(2) 0.036(3) 0.053(3) -0.013(2) 0.004(2) 0.004(2) C35 0.033(2) 0.027(2) 0.026(2) -0.0028(16) 0.0098(16) -0.0035(17) C36 0.047(3) 0.040(3) 0.031(2) -0.0014(19) 0.0084(19) 0.007(2) C37 0.069(3) 0.057(3) 0.028(2) -0.004(2) 0.009(2) 0.003(3) C38 0.060(3) 0.050(3) 0.041(3) -0.013(2) 0.026(2) 0.003(2) C39 0.044(3) 0.050(3) 0.042(3) -0.010(2) 0.018(2) 0.006(2) C40 0.036(2) 0.044(3) 0.033(2) -0.0055(19) 0.0127(18) 0.0046(19) C41 0.060(3) 0.066(4) 0.073(4) 0.043(3) 0.035(3) 0.027(3) Zn1B 0.0306(3) 0.0357(3) 0.0460(3) 0.0121(2) 0.0058(2) 0.0030(2) P1B 0.0254(5) 0.0325(6) 0.0321(5) -0.0015(4) 0.0077(4) 0.0039(4) P2B 0.0234(5) 0.0272(6) 0.0307(5) 0.0001(4) 0.0046(4) 0.0017(4) N1B 0.0257(17) 0.034(2) 0.0345(18) 0.0001(15) 0.0063(14) 0.0001(14) N2B 0.0302(18) 0.035(2) 0.0271(17) 0.0022(14) 0.0045(14) 0.0032(15) C1B 0.030(2) 0.030(2) 0.035(2) -0.0053(18) 0.0072(17) -0.0021(17) C2B 0.037(2) 0.040(3) 0.028(2) -0.0009(18) 0.0102(17) 0.0039(19) C3B 0.045(3) 0.057(3) 0.042(3) 0.009(2) 0.010(2) -0.009(2) C4B 0.064(3) 0.061(4) 0.046(3) -0.001(3) 0.014(3) -0.020(3) C5B 0.097(5) 0.045(3) 0.055(3) 0.006(3) 0.043(3) -0.009(3) C6B 0.073(4) 0.052(3) 0.054(3) 0.020(3) 0.031(3) 0.018(3) C7B 0.041(2) 0.054(3) 0.040(2) 0.009(2) 0.017(2) 0.009(2) C8B 0.028(2) 0.047(3) 0.041(2) -0.010(2) 0.0029(18) 0.0093(19) C9B 0.049(3) 0.068(4) 0.045(3) -0.009(2) 0.016(2) 0.014(3) C10B 0.064(4) 0.096(5) 0.059(3) -0.026(3) 0.022(3) 0.018(3) C11B 0.051(3) 0.093(5) 0.080(4) -0.052(4) 0.006(3) 0.017(3) C12B 0.064(4) 0.055(4) 0.093(5) -0.033(3) 0.008(3) 0.011(3) C13B 0.054(3) 0.049(3) 0.067(3) -0.018(3) 0.013(3) 0.002(2) C14B 0.0232(19) 0.027(2) 0.037(2) 0.0016(18) 0.0057(16) 0.0015(16) C15B 0.027(2) 0.034(3) 0.046(2) -0.001(2) 0.0064(18) 0.0049(18) C16B 0.038(2) 0.033(3) 0.067(3) -0.005(2) 0.013(2) -0.002(2) C17B 0.046(3) 0.036(3) 0.072(3) 0.018(3) 0.017(3) 0.010(2) C18B 0.040(3) 0.053(3) 0.054(3) 0.019(3) 0.006(2) 0.006(2) C19B 0.037(2) 0.040(3) 0.040(2) 0.004(2) 0.0062(19) 0.001(2) C20B 0.029(2) 0.031(2) 0.030(2) 0.0016(17) 0.0042(16) -0.0002(17) C21B 0.032(2) 0.035(2) 0.039(2) -0.0006(19) 0.0086(18) -0.0041(18) C22B 0.025(2) 0.061(3) 0.046(3) 0.008(2) 0.0052(19) -0.005(2) C23B 0.043(3) 0.053(3) 0.043(3) 0.011(2) 0.003(2) -0.021(2) C24B 0.052(3) 0.038(3) 0.054(3) 0.010(2) -0.001(2) -0.010(2) C25B 0.038(2) 0.038(3) 0.046(3) 0.005(2) 0.000(2) -0.002(2) C26B 0.023(2) 0.034(2) 0.031(2) 0.0036(17) 0.0035(16) 0.0021(17) C27B 0.031(2) 0.036(3) 0.039(2) 0.0067(19) 0.0061(18) 0.0060(19) C28B 0.028(2) 0.046(3) 0.048(3) 0.009(2) 0.0062(19) 0.009(2) C29B 0.031(2) 0.057(3) 0.041(2) 0.003(2) 0.0016(19) -0.003(2) C30B 0.039(2) 0.048(3) 0.043(3) -0.006(2) 0.006(2) -0.003(2) C31B 0.028(2) 0.040(3) 0.038(2) -0.0008(19) 0.0070(18) 0.0004(18) C32B 0.037(3) 0.042(3) 0.075(3) -0.004(3) 0.001(2) 0.015(2) C33B 0.037(3) 0.071(4) 0.066(3) -0.002(3) 0.000(2) -0.006(2) C34B 0.040(3) 0.046(3) 0.062(3) -0.018(2) 0.011(2) 0.002(2) C35B 0.048(3) 0.025(2) 0.037(2) -0.0027(18) 0.0126(19) -0.0067(19) C36B 0.077(3) 0.034(3) 0.032(2) -0.001(2) 0.002(2) -0.003(2) C37B 0.133(6) 0.048(3) 0.032(3) -0.007(2) 0.009(3) -0.014(4) C38B 0.126(6) 0.053(4) 0.056(4) -0.017(3) 0.049(4) -0.012(4) C39B 0.073(4) 0.061(4) 0.064(4) -0.020(3) 0.035(3) -0.005(3) C40B 0.047(3) 0.049(3) 0.044(3) -0.010(2) 0.019(2) -0.008(2) C41B 0.052(3) 0.065(4) 0.112(5) 0.044(4) 0.036(3) 0.021(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Zn1 C41 1.951(4) . ? Zn1 N1 2.011(3) . ? Zn1 N2 2.028(3) . ? P1 N1 1.609(3) . ? P1 C1 1.719(4) . ? P1 C2 1.815(4) . ? P1 C8 1.827(4) . ? P2 N2 1.628(3) . ? P2 C1 1.722(4) . ? P2 C14 1.814(4) . ? P2 C20 1.823(4) . ? N1 C26 1.431(5) . ? N2 C35 1.413(4) . ? C2 C3 1.390(6) . ? C2 C7 1.395(5) . ? C3 C4 1.391(6) . ? C4 C5 1.369(7) . ? C5 C6 1.381(7) . ? C6 C7 1.378(6) . ? C8 C13 1.387(6) . ? C8 C9 1.389(5) . ? C9 C10 1.388(6) . ? C10 C11 1.371(7) . ? C11 C12 1.375(6) . ? C12 C13 1.384(6) . ? C14 C15 1.385(5) . ? C14 C19 1.401(5) . ? C15 C16 1.381(6) . ? C16 C17 1.378(6) . ? C17 C18 1.383(6) . ? C18 C19 1.373(6) . ? C20 C25 1.386(6) . ? C20 C21 1.394(5) . ? C21 C22 1.388(6) . ? C22 C23 1.372(7) . ? C23 C24 1.381(7) . ? C24 C25 1.387(6) . ? C26 C31 1.393(6) . ? C26 C27 1.415(5) . ? C27 C28 1.385(6) . ? C27 C32 1.496(6) . ? C28 C29 1.383(6) . ? C29 C30 1.386(6) . ? C29 C33 1.515(6) . ? C30 C31 1.405(6) . ? C31 C34 1.509(6) . ? C35 C36 1.388(5) . ? C35 C40 1.401(6) . ? C36 C37 1.401(6) . ? C37 C38 1.382(7) . ? C38 C39 1.367(6) . ? C39 C40 1.391(5) . ? Zn1B C41B 1.956(5) . ? Zn1B N1B 2.021(3) . ? Zn1B N2B 2.043(3) . ? Zn1B P1B 2.8899(11) . ? Zn1B P2B 2.8942(11) . ? P1B N1B 1.603(3) . ? P1B C1B 1.730(4) . ? P1B C2B 1.819(4) . ? P1B C8B 1.829(4) . ? P2B N2B 1.623(3) . ? P2B C1B 1.727(4) . ? P2B C14B 1.811(4) . ? P2B C20B 1.819(4) . ? N1B C26B 1.433(5) . ? N2B C35B 1.401(5) . ? C2B C7B 1.380(6) . ? C2B C3B 1.403(6) . ? C3B C4B 1.379(7) . ? C4B C5B 1.362(8) . ? C5B C6B 1.364(8) . ? C6B C7B 1.388(7) . ? C8B C13B 1.377(7) . ? C8B C9B 1.382(6) . ? C9B C10B 1.381(7) . ? C10B C11B 1.361(9) . ? C11B C12B 1.379(9) . ? C12B C13B 1.382(7) . ? C14B C15B 1.388(6) . ? C14B C19B 1.398(6) . ? C15B C16B 1.388(6) . ? C16B C17B 1.374(7) . ? C17B C18B 1.378(7) . ? C18B C19B 1.388(6) . ? C20B C25B 1.385(6) . ? C20B C21B 1.395(5) . ? C21B C22B 1.387(6) . ? C22B C23B 1.380(7) . ? C23B C24B 1.372(7) . ? C24B C25B 1.382(6) . ? C26B C31B 1.398(6) . ? C26B C27B 1.401(5) . ? C27B C28B 1.400(6) . ? C27B C32B 1.513(6) . ? C28B C29B 1.367(6) . ? C29B C30B 1.402(6) . ? C29B C33B 1.509(6) . ? C30B C31B 1.400(6) . ? C31B C34B 1.507(6) . ? C35B C36B 1.391(6) . ? C35B C40B 1.400(6) . ? C36B C37B 1.407(7) . ? C37B C38B 1.363(9) . ? C38B C39B 1.376(8) . ? C39B C40B 1.398(6) . ? C1C C2C 1.39 . ? C1C C6C 1.39 . ? C1C C7C 1.3928 . ? C2C C3C 1.39 . ? C3C C4C 1.39 . ? C4C C5C 1.39 . ? C5C C6C 1.39 . ? 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 C41 Zn1 N1 123.50(16) . . ? C41 Zn1 N2 132.20(16) . . ? N1 Zn1 N2 103.94(12) . . ? N1 P1 C1 106.97(16) . . ? N1 P1 C2 109.01(17) . . ? C1 P1 C2 119.34(18) . . ? N1 P1 C8 115.87(17) . . ? C1 P1 C8 102.16(17) . . ? C2 P1 C8 103.78(17) . . ? N2 P2 C1 107.66(17) . . ? N2 P2 C14 111.98(17) . . ? C1 P2 C14 113.27(17) . . ? N2 P2 C20 111.90(17) . . ? C1 P2 C20 105.18(18) . . ? C14 P2 C20 106.70(18) . . ? C26 N1 P1 126.7(2) . . ? C26 N1 Zn1 125.4(2) . . ? P1 N1 Zn1 107.84(16) . . ? C35 N2 P2 125.4(3) . . ? C35 N2 Zn1 125.1(2) . . ? P2 N2 Zn1 106.63(16) . . ? P1 C1 P2 129.9(2) . . ? C3 C2 C7 118.9(4) . . ? C3 C2 P1 121.5(3) . . ? C7 C2 P1 119.4(3) . . ? C2 C3 C4 120.0(4) . . ? C5 C4 C3 120.1(4) . . ? C4 C5 C6 120.5(4) . . ? C7 C6 C5 119.8(4) . . ? C6 C7 C2 120.6(4) . . ? C13 C8 C9 118.6(4) . . ? C13 C8 P1 118.0(3) . . ? C9 C8 P1 123.3(3) . . ? C10 C9 C8 119.9(4) . . ? C11 C10 C9 120.8(4) . . ? C10 C11 C12 119.8(4) . . ? C11 C12 C13 119.9(4) . . ? C12 C13 C8 120.9(4) . . ? C15 C14 C19 118.8(4) . . ? C15 C14 P2 121.4(3) . . ? C19 C14 P2 119.3(3) . . ? C16 C15 C14 120.4(4) . . ? C17 C16 C15 120.4(4) . . ? C16 C17 C18 119.8(4) . . ? C19 C18 C17 120.2(4) . . ? C18 C19 C14 120.5(4) . . ? C25 C20 C21 119.2(4) . . ? C25 C20 P2 117.3(3) . . ? C21 C20 P2 123.4(3) . . ? C22 C21 C20 119.9(4) . . ? C23 C22 C21 120.6(4) . . ? C22 C23 C24 119.9(4) . . ? C23 C24 C25 120.1(5) . . ? C20 C25 C24 120.4(4) . . ? C31 C26 C27 119.4(4) . . ? C31 C26 N1 119.8(3) . . ? C27 C26 N1 120.7(4) . . ? C28 C27 C26 118.7(4) . . ? C28 C27 C32 120.6(4) . . ? C26 C27 C32 120.8(4) . . ? C29 C28 C27 123.0(4) . . ? C28 C29 C30 117.7(4) . . ? C28 C29 C33 121.2(4) . . ? C30 C29 C33 121.1(4) . . ? C29 C30 C31 121.5(4) . . ? C26 C31 C30 119.6(4) . . ? C26 C31 C34 120.9(4) . . ? C30 C31 C34 119.5(4) . . ? C36 C35 C40 117.7(3) . . ? C36 C35 N2 118.1(3) . . ? C40 C35 N2 124.2(3) . . ? C35 C36 C37 120.7(4) . . ? C38 C37 C36 120.5(4) . . ? C39 C38 C37 119.3(4) . . ? C38 C39 C40 120.9(4) . . ? C39 C40 C35 120.9(4) . . ? C41B Zn1B N1B 127.24(17) . . ? C41B Zn1B N2B 129.83(17) . . ? N1B Zn1B N2B 102.45(13) . . ? C41B Zn1B P1B 135.94(18) . . ? N1B Zn1B P1B 32.36(9) . . ? N2B Zn1B P1B 89.36(9) . . ? C41B Zn1B P2B 136.94(17) . . ? N1B Zn1B P2B 90.01(9) . . ? N2B Zn1B P2B 33.02(9) . . ? P1B Zn1B P2B 64.87(3) . . ? N1B P1B C1B 106.61(18) . . ? N1B P1B C2B 111.34(18) . . ? C1B P1B C2B 116.95(19) . . ? N1B P1B C8B 115.00(18) . . ? C1B P1B C8B 102.65(19) . . ? C2B P1B C8B 104.3(2) . . ? N1B P1B Zn1B 42.45(11) . . ? C1B P1B Zn1B 65.18(13) . . ? C2B P1B Zn1B 139.50(13) . . ? C8B P1B Zn1B 114.83(15) . . ? N2B P2B C1B 106.78(18) . . ? N2B P2B C14B 111.96(18) . . ? C1B P2B C14B 113.55(18) . . ? N2B P2B C20B 112.67(17) . . ? C1B P2B C20B 105.19(19) . . ? C14B P2B C20B 106.59(18) . . ? N2B P2B Zn1B 43.32(11) . . ? C1B P2B Zn1B 65.09(13) . . ? C14B P2B Zn1B 139.97(13) . . ? C20B P2B Zn1B 112.28(13) . . ? C26B N1B P1B 128.6(3) . . ? C26B N1B Zn1B 126.2(2) . . ? P1B N1B Zn1B 105.18(16) . . ? C35B N2B P2B 126.6(3) . . ? C35B N2B Zn1B 126.6(3) . . ? P2B N2B Zn1B 103.66(16) . . ? P2B C1B P1B 127.6(2) . . ? C7B C2B C3B 117.9(4) . . ? C7B C2B P1B 120.5(3) . . ? C3B C2B P1B 121.6(3) . . ? C4B C3B C2B 120.2(5) . . ? C5B C4B C3B 120.5(5) . . ? C4B C5B C6B 120.4(5) . . ? C5B C6B C7B 119.8(5) . . ? C2B C7B C6B 121.0(5) . . ? C13B C8B C9B 119.2(4) . . ? C13B C8B P1B 117.8(3) . . ? C9B C8B P1B 123.0(4) . . ? C10B C9B C8B 119.9(6) . . ? C11B C10B C9B 120.6(6) . . ? C10B C11B C12B 120.1(5) . . ? C11B C12B C13B 119.5(6) . . ? C8B C13B C12B 120.6(5) . . ? C15B C14B C19B 119.3(4) . . ? C15B C14B P2B 121.1(3) . . ? C19B C14B P2B 119.3(3) . . ? C14B C15B C16B 119.9(4) . . ? C17B C16B C15B 120.5(4) . . ? C16B C17B C18B 120.2(4) . . ? C17B C18B C19B 120.1(4) . . ? C18B C19B C14B 120.0(4) . . ? C25B C20B C21B 119.0(4) . . ? C25B C20B P2B 117.7(3) . . ? C21B C20B P2B 123.2(3) . . ? C22B C21B C20B 119.8(4) . . ? C23B C22B C21B 120.1(4) . . ? C24B C23B C22B 120.5(4) . . ? C23B C24B C25B 119.5(5) . . ? C24B C25B C20B 121.0(4) . . ? C31B C26B C27B 119.3(4) . . ? C31B C26B N1B 119.1(3) . . ? C27B C26B N1B 121.5(4) . . ? C28B C27B C26B 119.3(4) . . ? C28B C27B C32B 119.8(4) . . ? C26B C27B C32B 120.8(4) . . ? C29B C28B C27B 122.5(4) . . ? C28B C29B C30B 117.8(4) . . ? C28B C29B C33B 120.9(4) . . ? C30B C29B C33B 121.2(4) . . ? C31B C30B C29B 121.5(4) . . ? C26B C31B C30B 119.5(4) . . ? C26B C31B C34B 121.0(4) . . ? C30B C31B C34B 119.5(4) . . ? C36B C35B C40B 117.9(4) . . ? C36B C35B N2B 117.6(4) . . ? C40B C35B N2B 124.5(4) . . ? C35B C36B C37B 120.1(5) . . ? C38B C37B C36B 121.6(5) . . ? C37B C38B C39B 118.8(5) . . ? C38B C39B C40B 121.0(5) . . ? C39B C40B C35B 120.6(5) . . ? C2C C1C C6C 120 . . ? C2C C1C C7C 101.6 . . ? C6C C1C C7C 134.9 . . ? C3C C2C C1C 120 . . ? C2C C3C C4C 120 . . ? C5C C4C C3C 120 . . ? C6C C5C C4C 120 . . ? C5C C6C C1C 120 . . ? #===END data_msh5-(mar1502) _database_code_CSD 190730 _audit_creation_date 2002-03-22T16:45:07-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[Zn{N(SiMe3)2}{MesNPPh2CHPPh2NMes}]' _chemical_formula_moiety 'C49 H61 N3 P2 Si2 Zn1' _chemical_formula_sum 'C49 H61 N3 P2 Si2 Zn' _chemical_formula_weight 875.5 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.2060(2) _cell_length_b 19.8779(4) _cell_length_c 19.7239(5) _cell_angle_alpha 90 _cell_angle_beta 100.1290 _cell_angle_gamma 90 _cell_volume 4711.02(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18263 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 24.108 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.676 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8031 _exptl_absorpt_correction_T_max 0.8826 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.339715E-1 _diffrn_orient_matrix_ub_12 0.415929E-1 _diffrn_orient_matrix_ub_13 -0.23321E-1 _diffrn_orient_matrix_ub_21 0.527641E-1 _diffrn_orient_matrix_ub_22 -0.24305E-2 _diffrn_orient_matrix_ub_23 -0.333889E-1 _diffrn_orient_matrix_ub_31 -0.546637E-1 _diffrn_orient_matrix_ub_32 -0.281945E-1 _diffrn_orient_matrix_ub_33 -0.315251E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0944 _diffrn_reflns_av_unetI/netI 0.0623 _diffrn_reflns_number 31199 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 24.13 _diffrn_reflns_theta_full 24.13 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 7435 _reflns_number_gt 5775 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0376P)^2^+17.9944P] 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 'riding; torsion refined for ortho-methyls' _refine_ls_extinction_method none _refine_ls_number_reflns 7435 _refine_ls_number_parameters 518 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0895 _refine_ls_R_factor_gt 0.0654 _refine_ls_wR_factor_ref 0.1549 _refine_ls_wR_factor_gt 0.1431 _refine_ls_goodness_of_fit_ref 1.12 _refine_ls_restrained_S_all 1.12 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.927 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.091 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Zn Zn 0.72140(5) 0.23562(3) 0.89920(3) 0.02487(17) Uani 1 1 d . . . P1 P 0.81308(10) 0.11752(6) 0.83351(7) 0.0250(3) Uani 1 1 d . . . P2 P 0.90368(10) 0.14196(6) 0.98362(6) 0.0249(3) Uani 1 1 d . . . Si1 Si 0.65059(12) 0.38501(7) 0.88923(8) 0.0332(4) Uani 1 1 d . . . Si2 Si 0.48416(12) 0.28166(8) 0.91814(8) 0.0350(4) Uani 1 1 d . . . N1 N 0.7069(3) 0.1689(2) 0.8238(2) 0.0272(9) Uani 1 1 d . . . N2 N 0.8646(3) 0.21873(19) 0.9630(2) 0.0251(9) Uani 1 1 d . . . N3 N 0.6138(3) 0.3039(2) 0.9052(2) 0.0294(10) Uani 1 1 d . . . C1 C 0.8581(4) 0.0899(2) 0.9162(3) 0.0277(11) Uani 1 1 d . . . H1 H 0.8575 0.0429 0.9247 0.033 Uiso 1 1 calc R . . C2 C 0.9267(4) 0.1582(3) 0.8011(3) 0.0277(11) Uani 1 1 d . . . C3 C 0.9142(5) 0.2193(3) 0.7671(3) 0.0360(13) Uani 1 1 d . . . H3 H 0.845 0.2423 0.762 0.043 Uiso 1 1 calc R . . C4 C 1.0020(5) 0.2475(3) 0.7404(3) 0.0449(15) Uani 1 1 d . . . H4 H 0.9924 0.2895 0.7171 0.054 Uiso 1 1 calc R . . C5 C 1.1019(5) 0.2149(3) 0.7477(3) 0.0491(16) Uani 1 1 d . . . H5 H 1.1617 0.2343 0.7294 0.059 Uiso 1 1 calc R . . C6 C 1.1161(5) 0.1541(4) 0.7813(3) 0.0516(17) Uani 1 1 d . . . H6 H 1.1858 0.1317 0.7866 0.062 Uiso 1 1 calc R . . C7 C 1.0288(4) 0.1254(3) 0.8076(3) 0.0389(13) Uani 1 1 d . . . H7 H 1.0387 0.0831 0.8301 0.047 Uiso 1 1 calc R . . C8 C 0.7876(4) 0.0456(2) 0.7765(3) 0.0277(11) Uani 1 1 d . . . C9 C 0.7441(4) 0.0560(3) 0.7069(3) 0.0330(12) Uani 1 1 d . . . H9 H 0.7196 0.0996 0.6914 0.04 Uiso 1 1 calc R . . C10 C 0.7363(5) 0.0032(3) 0.6604(3) 0.0410(14) Uani 1 1 d . . . H10 H 0.7058 0.0106 0.6133 0.049 Uiso 1 1 calc R . . C11 C 0.7729(5) -0.0600(3) 0.6825(3) 0.0417(14) Uani 1 1 d . . . H11 H 0.7699 -0.0958 0.6502 0.05 Uiso 1 1 calc R . . C12 C 0.8138(5) -0.0715(3) 0.7511(3) 0.0453(15) Uani 1 1 d . . . H12 H 0.8365 -0.1155 0.7664 0.054 Uiso 1 1 calc R . . C13 C 0.8219(5) -0.0186(3) 0.7981(3) 0.0403(14) Uani 1 1 d . . . H13 H 0.8511 -0.0265 0.8453 0.048 Uiso 1 1 calc R . . C14 C 1.0534(4) 0.1388(3) 1.0166(3) 0.0306(12) Uani 1 1 d . . . C15 C 1.1161(4) 0.0905(3) 0.9900(3) 0.0364(13) Uani 1 1 d . . . H15 H 1.0815 0.0614 0.9543 0.044 Uiso 1 1 calc R . . C16 C 1.2300(5) 0.0844(3) 1.0153(3) 0.0469(15) Uani 1 1 d . . . H16 H 1.2729 0.0513 0.9972 0.056 Uiso 1 1 calc R . . C17 C 1.2793(5) 0.1269(3) 1.0667(3) 0.0484(16) Uani 1 1 d . . . H17 H 1.357 0.1235 1.0833 0.058 Uiso 1 1 calc R . . C18 C 1.2183(5) 0.1741(3) 1.0943(3) 0.0416(14) Uani 1 1 d . . . H18 H 1.2537 0.2025 1.1304 0.05 Uiso 1 1 calc R . . C19 C 1.1053(4) 0.1808(3) 1.0699(3) 0.0358(13) Uani 1 1 d . . . H19 H 1.0632 0.2137 1.0892 0.043 Uiso 1 1 calc R . . C20 C 0.8439(4) 0.1071(2) 1.0552(2) 0.0266(11) Uani 1 1 d . . . C21 C 0.7308(4) 0.0975(3) 1.0454(3) 0.0365(13) Uani 1 1 d . . . H21 H 0.6873 0.1066 1.0015 0.044 Uiso 1 1 calc R . . C22 C 0.6784(5) 0.0747(3) 1.0986(3) 0.0488(16) Uani 1 1 d . . . H22 H 0.5998 0.0697 1.0914 0.059 Uiso 1 1 calc R . . C23 C 0.7417(6) 0.0597(3) 1.1613(3) 0.0518(17) Uani 1 1 d . . . H23 H 0.7069 0.0437 1.1976 0.062 Uiso 1 1 calc R . . C24 C 0.8547(6) 0.0677(3) 1.1718(3) 0.0512(16) Uani 1 1 d . . . H24 H 0.898 0.0571 1.2154 0.061 Uiso 1 1 calc R . . C25 C 0.9062(5) 0.0910(3) 1.1198(3) 0.0398(14) Uani 1 1 d . . . H25 H 0.9848 0.0963 1.1277 0.048 Uiso 1 1 calc R . . C26 C 0.6012(4) 0.1583(3) 0.7795(3) 0.0294(12) Uani 1 1 d . . . C27 C 0.5626(4) 0.2051(3) 0.7270(3) 0.0312(12) Uani 1 1 d . . . C28 C 0.4621(5) 0.1918(3) 0.6824(3) 0.0397(14) Uani 1 1 d . . . H28 H 0.4388 0.2219 0.6452 0.048 Uiso 1 1 calc R . . C29 C 0.3962(5) 0.1377(3) 0.6898(3) 0.0417(14) Uani 1 1 d . . . C30 C 0.4315(4) 0.0954(3) 0.7450(3) 0.0421(15) Uani 1 1 d . . . H30 H 0.3847 0.0589 0.7524 0.05 Uiso 1 1 calc R . . C31 C 0.5317(4) 0.1034(3) 0.7902(3) 0.0363(13) Uani 1 1 d . . . C32 C 0.6228(5) 0.2693(3) 0.7179(3) 0.0395(13) Uani 1 1 d . . . H32A H 0.6428 0.292 0.7625 0.059 Uiso 1 1 calc R . . H32B H 0.5745 0.2987 0.6857 0.059 Uiso 1 1 calc R . . H32C H 0.6905 0.2592 0.6995 0.059 Uiso 1 1 calc R . . C33 C 0.2893(5) 0.1242(4) 0.6396(4) 0.0604(19) Uani 1 1 d . . . H33A H 0.2542 0.0833 0.6535 0.091 Uiso 0.5 1 calc PR . . H33B H 0.3062 0.1181 0.5932 0.091 Uiso 0.5 1 calc PR . . H33C H 0.2386 0.1623 0.6397 0.091 Uiso 0.5 1 calc PR . . H33D H 0.2785 0.1592 0.6041 0.091 Uiso 0.5 1 calc PR . . H33E H 0.2264 0.1244 0.6644 0.091 Uiso 0.5 1 calc PR . . H33F H 0.2941 0.0801 0.618 0.091 Uiso 0.5 1 calc PR . . C34 C 0.5624(5) 0.0533(3) 0.8477(3) 0.0458(15) Uani 1 1 d . . . H34A H 0.4975 0.0447 0.8695 0.069 Uiso 1 1 calc R . . H34B H 0.623 0.0715 0.882 0.069 Uiso 1 1 calc R . . H34C H 0.5865 0.0112 0.8291 0.069 Uiso 1 1 calc R . . C35 C 0.9146(4) 0.2772(2) 1.0003(3) 0.0262(11) Uani 1 1 d . . . C36 C 1.0048(4) 0.3103(3) 0.9796(3) 0.0301(12) Uani 1 1 d . . . C37 C 1.0433(4) 0.3698(3) 1.0118(3) 0.0338(13) Uani 1 1 d . . . H37 H 1.1033 0.3925 0.9969 0.041 Uiso 1 1 calc R . . C38 C 0.9972(5) 0.3975(3) 1.0650(3) 0.0386(14) Uani 1 1 d . . . C39 C 0.9098(4) 0.3628(3) 1.0855(3) 0.0354(13) Uani 1 1 d . . . H39 H 0.8781 0.3801 1.1225 0.043 Uiso 1 1 calc R . . C40 C 0.8671(4) 0.3039(3) 1.0540(3) 0.0304(12) Uani 1 1 d . . . C41 C 1.0604(5) 0.2841(3) 0.9226(3) 0.0409(14) Uani 1 1 d . . . H41A H 1.0064 0.2831 0.8795 0.061 Uiso 1 1 calc R . . H41B H 1.0883 0.2385 0.9339 0.061 Uiso 1 1 calc R . . H41C H 1.1226 0.3136 0.9172 0.061 Uiso 1 1 calc R . . C42 C 1.0354(5) 0.4650(3) 1.0967(4) 0.0556(18) Uani 1 1 d . . . H42A H 0.9932 0.4758 1.1332 0.083 Uiso 0.5 1 calc PR . . H42B H 1.0227 0.5 1.0611 0.083 Uiso 0.5 1 calc PR . . H42C H 1.1149 0.4628 1.1162 0.083 Uiso 0.5 1 calc PR . . H42D H 1.094 0.4832 1.0738 0.083 Uiso 0.5 1 calc PR . . H42E H 1.0645 0.4591 1.1459 0.083 Uiso 0.5 1 calc PR . . H42F H 0.9723 0.4963 1.0909 0.083 Uiso 0.5 1 calc PR . . C43 C 0.7682(5) 0.2720(3) 1.0780(3) 0.0403(14) Uani 1 1 d . . . H43A H 0.7922 0.2313 1.1044 0.06 Uiso 1 1 calc R . . H43B H 0.7119 0.2603 1.0379 0.06 Uiso 1 1 calc R . . H43C H 0.7365 0.3039 1.1072 0.06 Uiso 1 1 calc R . . C44 C 0.7853(5) 0.3858(3) 0.8561(3) 0.0406(14) Uani 1 1 d . . . H44A H 0.8432 0.3641 0.8897 0.061 Uiso 1 1 calc R . . H44B H 0.8069 0.4324 0.8489 0.061 Uiso 1 1 calc R . . H44C H 0.7762 0.3613 0.8123 0.061 Uiso 1 1 calc R . . C45 C 0.6708(6) 0.4403(3) 0.9676(3) 0.0541(17) Uani 1 1 d . . . H45A H 0.602 0.4415 0.9867 0.081 Uiso 1 1 calc R . . H45B H 0.6895 0.486 0.9547 0.081 Uiso 1 1 calc R . . H45C H 0.7314 0.4225 1.0021 0.081 Uiso 1 1 calc R . . C46 C 0.5434(5) 0.4269(3) 0.8232(4) 0.0523(17) Uani 1 1 d . . . H46A H 0.4719 0.4275 0.8393 0.078 Uiso 1 1 calc R . . H46B H 0.5355 0.402 0.7798 0.078 Uiso 1 1 calc R . . H46C H 0.5668 0.4731 0.816 0.078 Uiso 1 1 calc R . . C47 C 0.4251(5) 0.3428(3) 0.9744(3) 0.0512(16) Uani 1 1 d . . . H47A H 0.4779 0.349 1.0175 0.077 Uiso 1 1 calc R . . H47B H 0.3547 0.3253 0.9845 0.077 Uiso 1 1 calc R . . H47C H 0.412 0.3861 0.9506 0.077 Uiso 1 1 calc R . . C48 C 0.3799(4) 0.2725(3) 0.8372(3) 0.0438(14) Uani 1 1 d . . . H48A H 0.408 0.2407 0.8063 0.066 Uiso 1 1 calc R . . H48B H 0.3673 0.3164 0.8144 0.066 Uiso 1 1 calc R . . H48C H 0.3097 0.2557 0.8482 0.066 Uiso 1 1 calc R . . C49 C 0.4886(5) 0.1984(3) 0.9623(4) 0.0582(19) Uani 1 1 d . . . H49A H 0.5424 0.2002 1.0054 0.087 Uiso 1 1 calc R . . H49B H 0.511 0.1636 0.9323 0.087 Uiso 1 1 calc R . . H49C H 0.4146 0.1878 0.9723 0.087 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 Zn 0.0253(3) 0.0229(3) 0.0262(3) -0.0002(2) 0.0040(2) -0.0006(2) P1 0.0283(7) 0.0227(7) 0.0242(7) -0.0016(5) 0.0054(5) -0.0031(5) P2 0.0282(7) 0.0229(7) 0.0236(7) 0.0005(5) 0.0044(5) -0.0004(5) Si1 0.0377(8) 0.0252(8) 0.0356(8) 0.0001(6) 0.0033(7) 0.0014(6) Si2 0.0290(8) 0.0374(9) 0.0393(9) 0.0015(7) 0.0081(7) 0.0023(6) N1 0.028(2) 0.026(2) 0.026(2) -0.0018(18) 0.0018(18) 0.0011(18) N2 0.027(2) 0.022(2) 0.027(2) 0.0000(17) 0.0039(18) -0.0007(17) N3 0.030(2) 0.024(2) 0.035(2) 0.0002(19) 0.0087(19) 0.0032(18) C1 0.037(3) 0.018(3) 0.029(3) -0.001(2) 0.008(2) 0.000(2) C2 0.030(3) 0.029(3) 0.025(3) -0.003(2) 0.006(2) -0.002(2) C3 0.039(3) 0.034(3) 0.034(3) 0.001(2) 0.004(2) -0.008(2) C4 0.051(4) 0.046(4) 0.038(3) 0.008(3) 0.007(3) -0.017(3) C5 0.046(4) 0.065(4) 0.039(3) 0.001(3) 0.016(3) -0.021(3) C6 0.036(3) 0.071(5) 0.051(4) -0.002(4) 0.016(3) 0.001(3) C7 0.035(3) 0.045(3) 0.038(3) 0.006(3) 0.009(3) 0.002(3) C8 0.027(3) 0.024(3) 0.034(3) -0.005(2) 0.007(2) -0.005(2) C9 0.045(3) 0.025(3) 0.030(3) 0.002(2) 0.008(2) -0.007(2) C10 0.049(3) 0.041(4) 0.031(3) -0.005(3) 0.003(3) -0.010(3) C11 0.046(3) 0.037(3) 0.043(4) -0.015(3) 0.010(3) -0.008(3) C12 0.058(4) 0.028(3) 0.046(4) -0.003(3) -0.003(3) 0.006(3) C13 0.049(3) 0.034(3) 0.034(3) -0.006(3) -0.004(3) 0.004(3) C14 0.032(3) 0.030(3) 0.029(3) 0.008(2) 0.004(2) 0.000(2) C15 0.038(3) 0.037(3) 0.037(3) 0.003(3) 0.012(3) 0.003(3) C16 0.038(3) 0.050(4) 0.055(4) 0.008(3) 0.016(3) 0.014(3) C17 0.024(3) 0.058(4) 0.060(4) 0.014(3) -0.002(3) 0.001(3) C18 0.037(3) 0.040(3) 0.045(4) 0.007(3) -0.001(3) -0.006(3) C19 0.033(3) 0.033(3) 0.039(3) 0.003(3) -0.001(2) 0.000(2) C20 0.039(3) 0.020(3) 0.021(3) -0.001(2) 0.008(2) -0.001(2) C21 0.038(3) 0.039(3) 0.032(3) 0.004(2) 0.005(2) -0.004(3) C22 0.048(4) 0.050(4) 0.054(4) 0.003(3) 0.025(3) -0.013(3) C23 0.073(5) 0.048(4) 0.040(4) 0.010(3) 0.024(3) -0.008(3) C24 0.065(4) 0.061(4) 0.029(3) 0.013(3) 0.012(3) 0.004(3) C25 0.045(3) 0.041(3) 0.032(3) 0.004(3) 0.005(3) 0.000(3) C26 0.029(3) 0.026(3) 0.034(3) -0.008(2) 0.006(2) -0.003(2) C27 0.034(3) 0.032(3) 0.026(3) -0.008(2) 0.003(2) 0.001(2) C28 0.037(3) 0.045(4) 0.034(3) -0.008(3) -0.001(3) 0.006(3) C29 0.033(3) 0.051(4) 0.040(3) -0.019(3) 0.001(3) -0.003(3) C30 0.030(3) 0.040(3) 0.056(4) -0.019(3) 0.009(3) -0.011(3) C31 0.030(3) 0.035(3) 0.046(3) -0.006(3) 0.013(3) -0.003(2) C32 0.037(3) 0.042(3) 0.038(3) 0.003(3) 0.001(3) -0.004(3) C33 0.038(3) 0.078(5) 0.061(4) -0.026(4) -0.002(3) -0.002(3) C34 0.041(3) 0.041(4) 0.057(4) 0.003(3) 0.013(3) -0.011(3) C35 0.030(3) 0.020(3) 0.027(3) 0.002(2) -0.001(2) 0.000(2) C36 0.030(3) 0.029(3) 0.029(3) 0.002(2) -0.002(2) -0.001(2) C37 0.033(3) 0.028(3) 0.038(3) 0.003(2) -0.002(2) -0.005(2) C38 0.042(3) 0.026(3) 0.041(3) -0.005(2) -0.012(3) -0.002(2) C39 0.036(3) 0.033(3) 0.036(3) -0.005(2) 0.003(2) 0.005(2) C40 0.035(3) 0.028(3) 0.027(3) 0.001(2) 0.003(2) 0.003(2) C41 0.040(3) 0.047(4) 0.037(3) -0.004(3) 0.011(3) -0.012(3) C42 0.053(4) 0.033(3) 0.073(5) -0.015(3) -0.010(3) -0.003(3) C43 0.054(4) 0.037(3) 0.035(3) -0.004(3) 0.023(3) -0.001(3) C44 0.044(3) 0.030(3) 0.047(4) -0.001(3) 0.006(3) -0.009(2) C45 0.073(5) 0.032(3) 0.056(4) -0.009(3) 0.006(3) 0.002(3) C46 0.053(4) 0.036(3) 0.064(4) 0.014(3) 0.000(3) 0.008(3) C47 0.047(4) 0.065(4) 0.043(4) -0.007(3) 0.015(3) 0.007(3) C48 0.031(3) 0.051(4) 0.048(4) -0.005(3) 0.005(3) 0.000(3) C49 0.040(4) 0.061(4) 0.076(5) 0.028(4) 0.018(3) -0.004(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Zn N3 1.907(4) . ? Zn N1 1.977(4) . ? Zn N2 1.994(4) . ? P1 N1 1.634(4) . ? P1 C1 1.717(5) . ? P1 C8 1.812(5) . ? P1 C2 1.816(5) . ? P2 N2 1.629(4) . ? P2 C1 1.699(5) . ? P2 C14 1.830(5) . ? P2 C20 1.836(5) . ? Si1 N3 1.717(4) . ? Si1 C46 1.871(6) . ? Si1 C44 1.873(6) . ? Si1 C45 1.877(6) . ? Si2 N3 1.705(4) . ? Si2 C49 1.867(6) . ? Si2 C48 1.868(6) . ? Si2 C47 1.873(6) . ? N1 C26 1.441(6) . ? N2 C35 1.451(6) . ? C2 C3 1.382(7) . ? C2 C7 1.392(7) . ? C3 C4 1.393(8) . ? C4 C5 1.365(9) . ? C5 C6 1.375(9) . ? C6 C7 1.387(8) . ? C8 C13 1.385(7) . ? C8 C9 1.397(7) . ? C9 C10 1.386(8) . ? C10 C11 1.379(8) . ? C11 C12 1.377(8) . ? C12 C13 1.395(8) . ? C14 C15 1.388(7) . ? C14 C19 1.404(7) . ? C15 C16 1.397(8) . ? C16 C17 1.375(9) . ? C17 C18 1.369(9) . ? C18 C19 1.386(8) . ? C20 C21 1.374(7) . ? C20 C25 1.400(7) . ? C21 C22 1.397(8) . ? C22 C23 1.371(9) . ? C23 C24 1.368(9) . ? C24 C25 1.375(8) . ? C26 C27 1.409(7) . ? C26 C31 1.421(7) . ? C27 C28 1.404(7) . ? C27 C32 1.499(8) . ? C28 C29 1.367(8) . ? C29 C30 1.383(9) . ? C29 C33 1.516(8) . ? C30 C31 1.391(8) . ? C31 C34 1.507(8) . ? C35 C40 1.398(7) . ? C35 C36 1.404(7) . ? C36 C37 1.386(7) . ? C36 C41 1.505(7) . ? C37 C38 1.389(8) . ? C38 C39 1.389(8) . ? C38 C42 1.518(8) . ? C39 C40 1.383(7) . ? C40 C43 1.511(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Zn N1 123.56(17) . . ? N3 Zn N2 128.14(17) . . ? N1 Zn N2 108.29(16) . . ? N1 P1 C1 115.2(2) . . ? N1 P1 C8 112.0(2) . . ? C1 P1 C8 109.2(2) . . ? N1 P1 C2 108.6(2) . . ? C1 P1 C2 109.9(2) . . ? C8 P1 C2 101.0(2) . . ? N2 P2 C1 109.5(2) . . ? N2 P2 C14 110.6(2) . . ? C1 P2 C14 115.2(2) . . ? N2 P2 C20 114.0(2) . . ? C1 P2 C20 104.6(2) . . ? C14 P2 C20 102.7(2) . . ? N3 Si1 C46 111.8(3) . . ? N3 Si1 C44 110.2(2) . . ? C46 Si1 C44 107.6(3) . . ? N3 Si1 C45 113.6(3) . . ? C46 Si1 C45 106.7(3) . . ? C44 Si1 C45 106.6(3) . . ? N3 Si2 C49 110.4(2) . . ? N3 Si2 C48 114.1(2) . . ? C49 Si2 C48 105.8(3) . . ? N3 Si2 C47 112.6(3) . . ? C49 Si2 C47 106.4(3) . . ? C48 Si2 C47 107.1(3) . . ? C26 N1 P1 126.0(3) . . ? C26 N1 Zn 120.4(3) . . ? P1 N1 Zn 111.5(2) . . ? C35 N2 P2 123.0(3) . . ? C35 N2 Zn 115.4(3) . . ? P2 N2 Zn 120.1(2) . . ? Si2 N3 Si1 123.4(2) . . ? Si2 N3 Zn 119.5(2) . . ? Si1 N3 Zn 116.9(2) . . ? P2 C1 P1 123.7(3) . . ? C3 C2 C7 118.5(5) . . ? C3 C2 P1 122.4(4) . . ? C7 C2 P1 119.1(4) . . ? C2 C3 C4 120.7(6) . . ? C5 C4 C3 120.1(6) . . ? C4 C5 C6 120.1(6) . . ? C5 C6 C7 120.1(6) . . ? C6 C7 C2 120.5(6) . . ? C13 C8 C9 118.7(5) . . ? C13 C8 P1 121.7(4) . . ? C9 C8 P1 119.1(4) . . ? C10 C9 C8 120.6(5) . . ? C11 C10 C9 120.0(5) . . ? C12 C11 C10 120.2(5) . . ? C11 C12 C13 119.9(5) . . ? C8 C13 C12 120.6(5) . . ? C15 C14 C19 119.3(5) . . ? C15 C14 P2 118.2(4) . . ? C19 C14 P2 122.4(4) . . ? C14 C15 C16 120.3(6) . . ? C17 C16 C15 119.4(6) . . ? C18 C17 C16 121.1(5) . . ? C17 C18 C19 120.4(6) . . ? C18 C19 C14 119.5(5) . . ? C21 C20 C25 118.0(5) . . ? C21 C20 P2 118.0(4) . . ? C25 C20 P2 124.0(4) . . ? C20 C21 C22 121.4(5) . . ? C23 C22 C21 119.2(6) . . ? C24 C23 C22 120.3(6) . . ? C23 C24 C25 120.5(6) . . ? C24 C25 C20 120.6(6) . . ? C27 C26 C31 119.0(5) . . ? C27 C26 N1 119.9(4) . . ? C31 C26 N1 121.0(5) . . ? C28 C27 C26 118.7(5) . . ? C28 C27 C32 118.5(5) . . ? C26 C27 C32 122.8(5) . . ? C29 C28 C27 123.1(6) . . ? C28 C29 C30 117.1(5) . . ? C28 C29 C33 121.7(6) . . ? C30 C29 C33 121.2(6) . . ? C29 C30 C31 123.5(5) . . ? C30 C31 C26 118.3(5) . . ? C30 C31 C34 118.7(5) . . ? C26 C31 C34 123.0(5) . . ? C40 C35 C36 119.5(5) . . ? C40 C35 N2 119.7(4) . . ? C36 C35 N2 120.6(4) . . ? C37 C36 C35 119.2(5) . . ? C37 C36 C41 118.5(5) . . ? C35 C36 C41 122.4(5) . . ? C36 C37 C38 122.4(5) . . ? C39 C38 C37 117.1(5) . . ? C39 C38 C42 121.1(6) . . ? C37 C38 C42 121.7(6) . . ? C40 C39 C38 122.6(5) . . ? C39 C40 C35 119.2(5) . . ? C39 C40 C43 118.2(5) . . ? C35 C40 C43 122.6(5) . . ? #===END data_msh6-(dec301) _database_code_CSD 190731 _audit_creation_date 2001-12-04T16:27:48-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common [Zn{OC6H3tBu2)(MesNPPh2CHPPh2NMes)]' _chemical_formula_moiety 'C57 H64 N2 O1 Zn1' _chemical_formula_sum 'C57 H64 N2 O P2 Zn' _chemical_formula_weight 920.41 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 12.9453(7) _cell_length_b 14.0557(9) _cell_length_c 15.6630(9) _cell_angle_alpha 94.210(2) _cell_angle_beta 106.701(3) _cell_angle_gamma 110.514(3) _cell_volume 2508.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7556 _cell_measurement_theta_min 4.076 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.219 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.594 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.887 _exptl_absorpt_correction_T_max 0.919 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 13734 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_unetI/netI 0.082 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.15 _diffrn_reflns_theta_max 23.01 _diffrn_reflns_theta_full 23.01 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 6926 _reflns_number_gt 5141 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The C54 tBu group is disordered over two orientations and was refined with distance constraints for C-C and C..C . The lower occupancy C atoms were left isotropic. 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^)+(0.0283P)^2^+1.7301P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 6926 _refine_ls_number_parameters 594 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0767 _refine_ls_R_factor_gt 0.048 _refine_ls_wR_factor_ref 0.1057 _refine_ls_wR_factor_gt 0.0944 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.269 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.06 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Zn Zn 0.27847(3) 0.53804(3) 0.26015(3) 0.02632(14) Uani 1 1 d . . . P1 P 0.44923(8) 0.75809(7) 0.32986(6) 0.0229(2) Uani 1 1 d . . . P2 P 0.18755(8) 0.71596(7) 0.27771(6) 0.0229(2) Uani 1 1 d . . . O O 0.2255(2) 0.3964(2) 0.2468(2) 0.0485(8) Uani 1 1 d . . . N1 N 0.4344(2) 0.6419(2) 0.29018(19) 0.0245(7) Uani 1 1 d . . . N2 N 0.1632(2) 0.5927(2) 0.26951(19) 0.0231(7) Uani 1 1 d . . . C1 C 0.3287(3) 0.7867(3) 0.2858(2) 0.0247(9) Uani 1 1 d . . . H1 H 0.3419 0.8492 0.2632 0.03 Uiso 1 1 calc R . . C2 C 0.5739(3) 0.8504(3) 0.3098(2) 0.0262(9) Uani 1 1 d . . . C3 C 0.6837(3) 0.8490(3) 0.3513(3) 0.0373(10) Uani 1 1 d . . . H3 H 0.6929 0.8066 0.3952 0.045 Uiso 1 1 calc R . . C4 C 0.7795(3) 0.9085(3) 0.3295(3) 0.0459(12) Uani 1 1 d . . . H4 H 0.8538 0.9061 0.3577 0.055 Uiso 1 1 calc R . . C5 C 0.7673(4) 0.9707(3) 0.2674(3) 0.0480(12) Uani 1 1 d . . . H5 H 0.8329 1.0106 0.2517 0.058 Uiso 1 1 calc R . . C6 C 0.6603(4) 0.9758(4) 0.2276(3) 0.0510(12) Uani 1 1 d . . . H6 H 0.6525 1.0206 0.1858 0.061 Uiso 1 1 calc R . . C7 C 0.5637(3) 0.9152(3) 0.2486(3) 0.0387(10) Uani 1 1 d . . . H7 H 0.4898 0.9185 0.2206 0.046 Uiso 1 1 calc R . . C8 C 0.4885(3) 0.7757(3) 0.4524(2) 0.0249(9) Uani 1 1 d . . . C9 C 0.4694(3) 0.6932(3) 0.4975(3) 0.0324(9) Uani 1 1 d . . . H9 H 0.4428 0.6247 0.4648 0.039 Uiso 1 1 calc R . . C10 C 0.4891(3) 0.7103(4) 0.5904(3) 0.0403(11) Uani 1 1 d . . . H10 H 0.4747 0.6534 0.6207 0.048 Uiso 1 1 calc R . . C11 C 0.5293(3) 0.8091(4) 0.6381(3) 0.0404(11) Uani 1 1 d . . . H11 H 0.5414 0.8202 0.7014 0.048 Uiso 1 1 calc R . . C12 C 0.5523(3) 0.8924(3) 0.5952(3) 0.0393(10) Uani 1 1 d . . . H12 H 0.5826 0.9609 0.629 0.047 Uiso 1 1 calc R . . C13 C 0.5311(3) 0.8756(3) 0.5027(3) 0.0339(10) Uani 1 1 d . . . H13 H 0.5457 0.9329 0.4729 0.041 Uiso 1 1 calc R . . C14 C 0.1432(3) 0.7561(3) 0.3698(2) 0.0277(9) Uani 1 1 d . . . C15 C 0.2238(3) 0.8358(3) 0.4398(3) 0.0363(10) Uani 1 1 d . . . H15 H 0.3016 0.8678 0.4396 0.044 Uiso 1 1 calc R . . C16 C 0.1935(4) 0.8708(4) 0.5113(3) 0.0531(13) Uani 1 1 d . . . H16 H 0.2504 0.9256 0.5595 0.064 Uiso 1 1 calc R . . C17 C 0.0807(4) 0.8252(4) 0.5109(3) 0.0542(13) Uani 1 1 d . . . H17 H 0.0592 0.8488 0.559 0.065 Uiso 1 1 calc R . . C18 C -0.0015(4) 0.7455(3) 0.4417(3) 0.0466(12) Uani 1 1 d . . . H18 H -0.0794 0.7145 0.4421 0.056 Uiso 1 1 calc R . . C19 C 0.0284(3) 0.7097(3) 0.3708(3) 0.0348(10) Uani 1 1 d . . . H19 H -0.0286 0.6542 0.3233 0.042 Uiso 1 1 calc R . . C20 C 0.0997(3) 0.7491(3) 0.1804(2) 0.0284(9) Uani 1 1 d . . . C21 C 0.1118(4) 0.7277(3) 0.0962(3) 0.0408(11) Uani 1 1 d . . . H21 H 0.1655 0.6973 0.0918 0.049 Uiso 1 1 calc R . . C22 C 0.0469(4) 0.7499(3) 0.0189(3) 0.0497(12) Uani 1 1 d . . . H22 H 0.0562 0.7346 -0.0379 0.06 Uiso 1 1 calc R . . C23 C -0.0310(4) 0.7942(4) 0.0247(3) 0.0562(13) Uani 1 1 d . . . H23 H -0.0767 0.8086 -0.0281 0.067 Uiso 1 1 calc R . . C24 C -0.0418(4) 0.8173(4) 0.1077(3) 0.0667(15) Uani 1 1 d . . . H24 H -0.0952 0.8482 0.112 0.08 Uiso 1 1 calc R . . C25 C 0.0239(4) 0.7962(3) 0.1852(3) 0.0466(12) Uani 1 1 d . . . H25 H 0.0166 0.8144 0.2422 0.056 Uiso 1 1 calc R . . C26 C 0.5085(3) 0.6236(3) 0.2423(2) 0.0258(9) Uani 1 1 d . . . C27 C 0.4872(3) 0.6329(3) 0.1515(3) 0.0293(9) Uani 1 1 d . . . C28 C 0.5583(3) 0.6132(3) 0.1068(3) 0.0371(10) Uani 1 1 d . . . H28 H 0.5449 0.6209 0.0452 0.045 Uiso 1 1 calc R . . C29 C 0.6479(3) 0.5830(3) 0.1491(3) 0.0390(11) Uani 1 1 d . . . C30 C 0.6648(3) 0.5703(3) 0.2384(3) 0.0381(11) Uani 1 1 d . . . H30 H 0.7249 0.5481 0.2679 0.046 Uiso 1 1 calc R . . C31 C 0.5960(3) 0.5894(3) 0.2862(3) 0.0313(9) Uani 1 1 d . . . C32 C 0.3878(3) 0.6619(3) 0.1004(3) 0.0430(11) Uani 1 1 d . . . H32A H 0.3906 0.6694 0.0393 0.064 Uiso 1 1 calc R . . H32B H 0.3953 0.7275 0.133 0.064 Uiso 1 1 calc R . . H32C H 0.3129 0.6075 0.0957 0.064 Uiso 1 1 calc R . . C33 C 0.7249(4) 0.5643(4) 0.0980(3) 0.0586(14) Uani 1 1 d . . . H33A H 0.7835 0.5436 0.1378 0.088 Uiso 0.5 1 calc PR . . H33B H 0.7643 0.6281 0.0789 0.088 Uiso 0.5 1 calc PR . . H33C H 0.6763 0.5092 0.0444 0.088 Uiso 0.5 1 calc PR . . H33D H 0.6993 0.577 0.0362 0.088 Uiso 0.5 1 calc PR . . H33E H 0.7185 0.4925 0.0952 0.088 Uiso 0.5 1 calc PR . . H33F H 0.8065 0.6114 0.1297 0.088 Uiso 0.5 1 calc PR . . C34 C 0.6146(4) 0.5726(3) 0.3818(3) 0.0447(11) Uani 1 1 d . . . H34A H 0.6413 0.639 0.4228 0.067 Uiso 1 1 calc R . . H34B H 0.6739 0.5427 0.3991 0.067 Uiso 1 1 calc R . . H34C H 0.5409 0.525 0.3863 0.067 Uiso 1 1 calc R . . C35 C 0.0580(3) 0.5175(3) 0.2775(2) 0.0239(9) Uani 1 1 d . . . C36 C 0.0586(3) 0.4906(3) 0.3620(3) 0.0314(9) Uani 1 1 d . . . C37 C -0.0432(3) 0.4186(3) 0.3687(3) 0.0387(10) Uani 1 1 d . . . H37 H -0.0431 0.4015 0.4263 0.046 Uiso 1 1 calc R . . C38 C -0.1445(3) 0.3710(3) 0.2949(3) 0.0402(11) Uani 1 1 d . . . C39 C -0.1401(3) 0.3940(3) 0.2119(3) 0.0371(10) Uani 1 1 d . . . H39 H -0.2079 0.3596 0.1598 0.045 Uiso 1 1 calc R . . C40 C -0.0413(3) 0.4651(3) 0.2006(3) 0.0304(9) Uani 1 1 d . . . C41 C 0.1690(3) 0.5348(3) 0.4444(3) 0.0390(10) Uani 1 1 d . . . H41A H 0.1511 0.5112 0.4978 0.059 Uiso 1 1 calc R . . H41B H 0.1993 0.6106 0.4549 0.059 Uiso 1 1 calc R . . H41C H 0.2279 0.5112 0.4339 0.059 Uiso 1 1 calc R . . C42 C -0.2556(4) 0.2938(4) 0.3049(3) 0.0665(15) Uani 1 1 d . . . H42A H -0.2413 0.2875 0.3688 0.1 Uiso 0.5 1 calc PR . . H42B H -0.2775 0.226 0.2677 0.1 Uiso 0.5 1 calc PR . . H42C H -0.3192 0.3182 0.2847 0.1 Uiso 0.5 1 calc PR . . H42D H -0.3174 0.2669 0.2453 0.1 Uiso 0.5 1 calc PR . . H42E H -0.2812 0.3285 0.3464 0.1 Uiso 0.5 1 calc PR . . H42F H -0.2395 0.2363 0.3294 0.1 Uiso 0.5 1 calc PR . . C43 C -0.0410(3) 0.4810(3) 0.1066(2) 0.0359(10) Uani 1 1 d . . . H43A H -0.1085 0.4254 0.0614 0.054 Uiso 1 1 calc R . . H43B H 0.0313 0.48 0.0993 0.054 Uiso 1 1 calc R . . H43C H -0.0456 0.5479 0.098 0.054 Uiso 1 1 calc R . . C44 C 0.2537(3) 0.3250(3) 0.2099(3) 0.0353(10) Uani 1 1 d . . . C45 C 0.2070(3) 0.2209(3) 0.2203(2) 0.0290(9) Uani 1 1 d . . . C46 C 0.2325(3) 0.1484(3) 0.1743(2) 0.0318(9) Uani 1 1 d . . . H46 H 0.1979 0.0781 0.1793 0.038 Uiso 1 1 calc R . . C47 C 0.3050(3) 0.1710(3) 0.1214(2) 0.0301(9) Uani 1 1 d . A . C48 C 0.3529(4) 0.2740(3) 0.1148(3) 0.0417(11) Uani 1 1 d . . . H48 H 0.4041 0.294 0.0805 0.05 Uiso 1 1 calc R . . C49 C 0.3270(4) 0.3485(3) 0.1580(3) 0.0414(11) Uani 1 1 d . . . H49 H 0.3608 0.4184 0.1517 0.05 Uiso 1 1 calc R . . C50 C 0.1301(3) 0.1900(3) 0.2809(3) 0.0339(10) Uani 1 1 d . . . C51 C 0.1975(4) 0.2535(4) 0.3776(3) 0.0508(12) Uani 1 1 d . . . H51A H 0.2687 0.2403 0.4029 0.076 Uiso 1 1 calc R . . H51B H 0.1481 0.2333 0.4157 0.076 Uiso 1 1 calc R . . H51C H 0.2187 0.3273 0.3762 0.076 Uiso 1 1 calc R . . C52 C 0.0179(3) 0.2100(3) 0.2416(3) 0.0410(11) Uani 1 1 d . . . H52A H 0.0387 0.2824 0.2346 0.061 Uiso 1 1 calc R . . H52B H -0.0276 0.196 0.2829 0.061 Uiso 1 1 calc R . . H52C H -0.029 0.1644 0.1822 0.061 Uiso 1 1 calc R . . C53 C 0.0950(4) 0.0758(3) 0.2879(3) 0.0501(12) Uani 1 1 d . . . H53A H 0.0475 0.0325 0.2275 0.075 Uiso 1 1 calc R . . H53B H 0.0494 0.0604 0.329 0.075 Uiso 1 1 calc R . . H53C H 0.1655 0.0613 0.3115 0.075 Uiso 1 1 calc R . . C54 C 0.3276(3) 0.0866(3) 0.0714(3) 0.0411(11) Uani 1 1 d D . . C55 C 0.3181(14) -0.0042(8) 0.1240(5) 0.074(4) Uani 0.79(2) 1 d PD A 1 H55A H 0.3763 0.0216 0.1852 0.11 Uiso 0.79(2) 1 calc PR A 1 H55B H 0.3325 -0.058 0.0916 0.11 Uiso 0.79(2) 1 calc PR A 1 H55C H 0.2395 -0.0335 0.1284 0.11 Uiso 0.79(2) 1 calc PR A 1 C56 C 0.2341(8) 0.0396(8) -0.0204(5) 0.065(3) Uani 0.79(2) 1 d PD A 1 H56A H 0.157 0.0141 -0.013 0.098 Uiso 0.79(2) 1 calc PR A 1 H56B H 0.246 -0.0181 -0.0494 0.098 Uiso 0.79(2) 1 calc PR A 1 H56C H 0.2385 0.0922 -0.0584 0.098 Uiso 0.79(2) 1 calc PR A 1 C57 C 0.4484(8) 0.1268(7) 0.0628(12) 0.116(5) Uani 0.79(2) 1 d PD A 1 H57A H 0.4558 0.1828 0.0282 0.173 Uiso 0.79(2) 1 calc PR A 1 H57B H 0.4597 0.0705 0.031 0.173 Uiso 0.79(2) 1 calc PR A 1 H57C H 0.5078 0.1531 0.1234 0.173 Uiso 0.79(2) 1 calc PR A 1 C55A C 0.385(2) 0.0286(19) 0.1324(13) 0.032(7) Uiso 0.21(2) 1 d PD A 2 H55D H 0.4621 0.077 0.1737 0.048 Uiso 0.21(2) 1 calc PR A 2 H55E H 0.3954 -0.0246 0.0953 0.048 Uiso 0.21(2) 1 calc PR A 2 H55F H 0.3362 -0.0044 0.1677 0.048 Uiso 0.21(2) 1 calc PR A 2 C56A C 0.2167(18) 0.011(2) -0.0011(19) 0.068(13) Uiso 0.21(2) 1 d PD A 2 H56D H 0.1608 -0.0266 0.0276 0.101 Uiso 0.21(2) 1 calc PR A 2 H56E H 0.2353 -0.0379 -0.0354 0.101 Uiso 0.21(2) 1 calc PR A 2 H56F H 0.1821 0.0493 -0.0425 0.101 Uiso 0.21(2) 1 calc PR A 2 C57A C 0.414(2) 0.138(2) 0.0193(17) 0.053(9) Uiso 0.21(2) 1 d PD A 2 H57D H 0.3741 0.1649 -0.0304 0.079 Uiso 0.21(2) 1 calc PR A 2 H57E H 0.4374 0.0863 -0.0055 0.079 Uiso 0.21(2) 1 calc PR A 2 H57F H 0.483 0.195 0.0614 0.079 Uiso 0.21(2) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.0259(2) 0.0205(3) 0.0331(3) 0.0017(2) 0.01269(19) 0.0081(2) P1 0.0230(5) 0.0205(6) 0.0235(6) 0.0028(4) 0.0077(4) 0.0070(4) P2 0.0228(5) 0.0230(6) 0.0219(6) 0.0021(4) 0.0049(4) 0.0104(4) O 0.0531(18) 0.0189(16) 0.083(2) 0.0019(15) 0.0402(17) 0.0122(14) N1 0.0233(16) 0.0207(18) 0.0318(18) 0.0021(14) 0.0126(14) 0.0091(14) N2 0.0246(16) 0.0208(18) 0.0259(18) 0.0055(14) 0.0097(13) 0.0102(14) C1 0.027(2) 0.020(2) 0.028(2) 0.0066(17) 0.0088(17) 0.0106(17) C2 0.026(2) 0.021(2) 0.027(2) -0.0020(18) 0.0080(17) 0.0052(18) C3 0.029(2) 0.028(2) 0.051(3) 0.005(2) 0.013(2) 0.0086(19) C4 0.026(2) 0.044(3) 0.063(3) 0.001(3) 0.018(2) 0.008(2) C5 0.040(3) 0.041(3) 0.057(3) 0.002(3) 0.029(2) 0.000(2) C6 0.051(3) 0.049(3) 0.051(3) 0.023(2) 0.027(2) 0.008(2) C7 0.035(2) 0.041(3) 0.039(3) 0.014(2) 0.015(2) 0.010(2) C8 0.0221(19) 0.030(2) 0.024(2) 0.0047(19) 0.0091(16) 0.0109(18) C9 0.029(2) 0.032(3) 0.031(2) 0.004(2) 0.0080(18) 0.0067(19) C10 0.040(2) 0.047(3) 0.033(3) 0.014(2) 0.013(2) 0.015(2) C11 0.032(2) 0.062(3) 0.021(2) 0.003(2) 0.0023(18) 0.018(2) C12 0.043(2) 0.037(3) 0.026(3) -0.005(2) 0.0028(19) 0.012(2) C13 0.039(2) 0.031(3) 0.027(2) 0.003(2) 0.0056(18) 0.014(2) C14 0.029(2) 0.028(2) 0.028(2) 0.0013(19) 0.0082(17) 0.0152(19) C15 0.035(2) 0.042(3) 0.032(2) 0.002(2) 0.016(2) 0.012(2) C16 0.053(3) 0.054(3) 0.042(3) -0.012(2) 0.020(2) 0.010(3) C17 0.056(3) 0.060(3) 0.048(3) -0.006(3) 0.033(2) 0.015(3) C18 0.044(3) 0.045(3) 0.059(3) 0.005(3) 0.030(2) 0.017(2) C19 0.032(2) 0.029(2) 0.041(3) 0.000(2) 0.0126(19) 0.0101(19) C20 0.028(2) 0.023(2) 0.029(2) 0.0021(18) 0.0011(17) 0.0107(18) C21 0.052(3) 0.042(3) 0.033(3) 0.010(2) 0.008(2) 0.029(2) C22 0.075(3) 0.043(3) 0.029(3) 0.009(2) 0.006(2) 0.029(3) C23 0.060(3) 0.047(3) 0.045(3) 0.011(3) -0.014(2) 0.026(3) C24 0.071(3) 0.090(4) 0.054(3) 0.018(3) 0.003(3) 0.061(3) C25 0.053(3) 0.062(3) 0.035(3) 0.008(2) 0.008(2) 0.038(3) C26 0.0216(19) 0.022(2) 0.030(2) -0.0022(18) 0.0087(17) 0.0055(17) C27 0.028(2) 0.030(2) 0.030(2) 0.0016(19) 0.0107(17) 0.0109(18) C28 0.041(2) 0.041(3) 0.033(2) 0.003(2) 0.016(2) 0.017(2) C29 0.036(2) 0.037(3) 0.047(3) -0.001(2) 0.021(2) 0.013(2) C30 0.028(2) 0.038(3) 0.052(3) 0.002(2) 0.012(2) 0.020(2) C31 0.025(2) 0.028(2) 0.037(3) 0.0041(19) 0.0051(18) 0.0103(18) C32 0.050(3) 0.057(3) 0.028(2) 0.006(2) 0.011(2) 0.032(2) C33 0.050(3) 0.075(4) 0.064(3) 0.003(3) 0.031(3) 0.032(3) C34 0.047(3) 0.047(3) 0.046(3) 0.009(2) 0.009(2) 0.031(2) C35 0.022(2) 0.022(2) 0.028(2) 0.0043(18) 0.0087(17) 0.0091(18) C36 0.029(2) 0.032(2) 0.035(3) 0.006(2) 0.0130(18) 0.012(2) C37 0.037(2) 0.042(3) 0.043(3) 0.015(2) 0.022(2) 0.013(2) C38 0.031(2) 0.034(3) 0.055(3) 0.013(2) 0.022(2) 0.005(2) C39 0.023(2) 0.035(3) 0.045(3) 0.000(2) 0.0040(19) 0.009(2) C40 0.026(2) 0.032(2) 0.035(2) 0.0023(19) 0.0093(18) 0.0143(19) C41 0.036(2) 0.046(3) 0.029(2) 0.010(2) 0.0095(19) 0.010(2) C42 0.040(3) 0.070(4) 0.075(4) 0.014(3) 0.026(3) -0.002(3) C43 0.031(2) 0.037(3) 0.032(2) -0.002(2) 0.0072(18) 0.010(2) C44 0.032(2) 0.028(3) 0.039(3) -0.003(2) 0.0099(19) 0.008(2) C45 0.027(2) 0.027(2) 0.030(2) 0.0030(19) 0.0069(17) 0.0087(19) C46 0.035(2) 0.023(2) 0.034(2) 0.0066(19) 0.0065(19) 0.0105(19) C47 0.034(2) 0.028(3) 0.026(2) 0.0021(19) 0.0030(18) 0.0158(19) C48 0.052(3) 0.044(3) 0.040(3) 0.011(2) 0.025(2) 0.022(2) C49 0.053(3) 0.029(3) 0.051(3) 0.015(2) 0.029(2) 0.015(2) C50 0.027(2) 0.030(2) 0.041(3) 0.009(2) 0.0106(18) 0.0070(19) C51 0.048(3) 0.066(3) 0.036(3) 0.003(2) 0.019(2) 0.017(3) C52 0.033(2) 0.035(3) 0.053(3) 0.010(2) 0.017(2) 0.009(2) C53 0.046(3) 0.042(3) 0.073(3) 0.028(3) 0.033(2) 0.017(2) C54 0.047(3) 0.041(3) 0.036(3) 0.000(2) 0.005(2) 0.026(2) C55 0.126(10) 0.070(6) 0.054(5) 0.011(4) 0.025(5) 0.077(7) C56 0.101(6) 0.071(6) 0.030(4) -0.010(4) -0.003(4) 0.064(5) C57 0.069(6) 0.081(7) 0.213(14) -0.021(7) 0.075(8) 0.036(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Zn O 1.837(3) . ? Zn N1 1.928(3) . ? Zn N2 1.937(2) . ? P1 N1 1.630(3) . ? P1 C1 1.712(3) . ? P1 C2 1.809(4) . ? P1 C8 1.812(4) . ? P2 N2 1.637(3) . ? P2 C1 1.709(3) . ? P2 C20 1.820(4) . ? P2 C14 1.820(3) . ? O C44 1.329(4) . ? N1 C26 1.452(4) . ? N2 C35 1.448(4) . ? C2 C7 1.381(5) . ? C2 C3 1.390(5) . ? C3 C4 1.383(5) . ? C4 C5 1.369(6) . ? C5 C6 1.375(6) . ? C6 C7 1.389(5) . ? C8 C9 1.387(5) . ? C8 C13 1.393(5) . ? C9 C10 1.389(5) . ? C10 C11 1.370(6) . ? C11 C12 1.378(6) . ? C12 C13 1.382(5) . ? C14 C15 1.374(5) . ? C14 C19 1.403(5) . ? C15 C16 1.399(5) . ? C16 C17 1.373(6) . ? C17 C18 1.374(6) . ? C18 C19 1.391(5) . ? C20 C25 1.378(5) . ? C20 C21 1.395(5) . ? C21 C22 1.388(5) . ? C22 C23 1.377(6) . ? C23 C24 1.375(6) . ? C24 C25 1.387(6) . ? C26 C27 1.394(5) . ? C26 C31 1.403(5) . ? C27 C28 1.391(5) . ? C27 C32 1.512(5) . ? C28 C29 1.382(5) . ? C29 C30 1.387(5) . ? C29 C33 1.521(5) . ? C30 C31 1.394(5) . ? C31 C34 1.498(5) . ? C35 C36 1.400(5) . ? C35 C40 1.401(5) . ? C36 C37 1.391(5) . ? C36 C41 1.515(5) . ? C37 C38 1.380(5) . ? C38 C39 1.374(5) . ? C38 C42 1.527(6) . ? C39 C40 1.388(5) . ? C40 C43 1.505(5) . ? C44 C49 1.391(5) . ? C44 C45 1.416(5) . ? C45 C46 1.389(5) . ? C45 C50 1.543(5) . ? C46 C47 1.396(5) . ? C47 C48 1.386(5) . ? C47 C54 1.531(5) . ? C48 C49 1.394(5) . ? C50 C53 1.529(5) . ? C50 C51 1.532(5) . ? C50 C52 1.538(5) . ? C54 C56 1.506(6) . ? C54 C55A 1.506(12) . ? C54 C56A 1.515(14) . ? C54 C57 1.516(7) . ? C54 C55 1.558(8) . ? C54 C57A 1.572(13) . ? 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 O Zn N1 130.98(11) . . ? O Zn N2 113.53(12) . . ? N1 Zn N2 114.19(11) . . ? N1 P1 C1 114.92(16) . . ? N1 P1 C2 108.39(15) . . ? C1 P1 C2 109.69(17) . . ? N1 P1 C8 108.73(16) . . ? C1 P1 C8 109.54(15) . . ? C2 P1 C8 105.11(16) . . ? N2 P2 C1 110.75(15) . . ? N2 P2 C20 115.05(16) . . ? C1 P2 C20 104.17(17) . . ? N2 P2 C14 109.00(16) . . ? C1 P2 C14 115.01(17) . . ? C20 P2 C14 102.74(16) . . ? C44 O Zn 133.9(3) . . ? C26 N1 P1 122.3(2) . . ? C26 N1 Zn 117.6(2) . . ? P1 N1 Zn 114.44(14) . . ? C35 N2 P2 122.4(2) . . ? C35 N2 Zn 114.6(2) . . ? P2 N2 Zn 122.76(16) . . ? P2 C1 P1 127.7(2) . . ? C7 C2 C3 118.4(3) . . ? C7 C2 P1 123.0(3) . . ? C3 C2 P1 118.3(3) . . ? C4 C3 C2 120.7(4) . . ? C5 C4 C3 120.0(4) . . ? C4 C5 C6 120.2(4) . . ? C5 C6 C7 119.9(4) . . ? C2 C7 C6 120.7(4) . . ? C9 C8 C13 118.5(3) . . ? C9 C8 P1 122.7(3) . . ? C13 C8 P1 118.6(3) . . ? C8 C9 C10 120.4(4) . . ? C11 C10 C9 120.0(4) . . ? C10 C11 C12 120.6(4) . . ? C11 C12 C13 119.5(4) . . ? C12 C13 C8 120.9(4) . . ? C15 C14 C19 118.8(3) . . ? C15 C14 P2 119.1(3) . . ? C19 C14 P2 122.1(3) . . ? C14 C15 C16 121.3(4) . . ? C17 C16 C15 119.2(4) . . ? C16 C17 C18 120.5(4) . . ? C17 C18 C19 120.5(4) . . ? C18 C19 C14 119.6(4) . . ? C25 C20 C21 118.0(3) . . ? C25 C20 P2 123.9(3) . . ? C21 C20 P2 118.1(3) . . ? C22 C21 C20 121.3(4) . . ? C23 C22 C21 119.8(4) . . ? C24 C23 C22 119.3(4) . . ? C23 C24 C25 121.0(4) . . ? C20 C25 C24 120.6(4) . . ? C27 C26 C31 120.5(3) . . ? C27 C26 N1 120.0(3) . . ? C31 C26 N1 119.3(3) . . ? C28 C27 C26 118.8(3) . . ? C28 C27 C32 119.5(3) . . ? C26 C27 C32 121.7(3) . . ? C29 C28 C27 122.0(4) . . ? C28 C29 C30 118.2(3) . . ? C28 C29 C33 120.2(4) . . ? C30 C29 C33 121.6(4) . . ? C29 C30 C31 121.9(3) . . ? C30 C31 C26 118.5(4) . . ? C30 C31 C34 120.5(3) . . ? C26 C31 C34 121.0(3) . . ? C36 C35 C40 119.5(3) . . ? C36 C35 N2 119.5(3) . . ? C40 C35 N2 120.8(3) . . ? C37 C36 C35 118.9(3) . . ? C37 C36 C41 119.7(4) . . ? C35 C36 C41 121.3(3) . . ? C38 C37 C36 122.4(4) . . ? C39 C38 C37 117.2(4) . . ? C39 C38 C42 121.6(4) . . ? C37 C38 C42 121.1(4) . . ? C38 C39 C40 123.1(4) . . ? C39 C40 C35 118.6(3) . . ? C39 C40 C43 119.8(3) . . ? C35 C40 C43 121.6(3) . . ? O C44 C49 121.6(4) . . ? O C44 C45 120.8(3) . . ? C49 C44 C45 117.6(3) . . ? C46 C45 C44 118.0(3) . . ? C46 C45 C50 121.6(3) . . ? C44 C45 C50 120.4(3) . . ? C45 C46 C47 124.9(4) . . ? C48 C47 C46 116.0(3) . . ? C48 C47 C54 122.0(3) . . ? C46 C47 C54 122.0(4) . . ? C47 C48 C49 120.8(4) . . ? C44 C49 C48 122.7(4) . . ? C53 C50 C51 107.1(3) . . ? C53 C50 C52 108.4(3) . . ? C51 C50 C52 109.5(3) . . ? C53 C50 C45 112.2(3) . . ? C51 C50 C45 110.0(3) . . ? C52 C50 C45 109.6(3) . . ? C56 C54 C55A 125.3(10) . . ? C56 C54 C56A 20.7(12) . . ? C55A C54 C56A 110.1(12) . . ? C56 C54 C57 111.0(6) . . ? C55A C54 C57 79.1(8) . . ? C56A C54 C57 125.5(16) . . ? C56 C54 C47 110.4(4) . . ? C57 C54 C47 112.0(4) . . ? C56 C54 C55 105.4(5) . . ? C57 C54 C55 107.9(5) . . ? C47 C54 C55 109.9(4) . . ? C55A C54 C57A 105.6(9) . . ? C56A C54 C57A 105.5(11) . . ? C47 C54 C57A 109.0(12) . . ? #===END data_msh7-(jun902) _database_code_CSD 190732 _audit_creation_date 2002-06-12T14:34:18-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; '[Zn(OCPh3)(MesNPPh2CHPPh2NMes)].toluene' ; _chemical_formula_moiety '(C62 H58 N2 O1 P2 Zn1)(C7 H8)' _chemical_formula_sum 'C69 H66 N2 O P2 Zn' _chemical_formula_weight 1066.55 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.8791(2) _cell_length_b 26.6119(5) _cell_length_c 16.6536(4) _cell_angle_alpha 90 _cell_angle_beta 100.941(1) _cell_angle_gamma 90 _cell_volume 5604.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 23748 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 23.817 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.541 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8514 _exptl_absorpt_correction_T_max 0.939 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0642 _diffrn_reflns_av_unetI/netI 0.0618 _diffrn_reflns_number 27200 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 23.8 _diffrn_reflns_theta_full 23.8 _diffrn_measured_fraction_theta_full 0.913 _diffrn_measured_fraction_theta_max 0.913 _reflns_number_total 7853 _reflns_number_gt 5919 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The C6 ring of the toluene solvate molecule was refined as a rigid body. 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^)+(0.0401P)^2^+7.4674P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 7853 _refine_ls_number_parameters 668 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1129 _refine_ls_wR_factor_gt 0.103 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.5 _refine_diff_density_min -0.642 _refine_diff_density_rms 0.058 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Zn Zn 0.18283(3) 0.309351(14) 0.61011(2) 0.02353(14) Uani 1 1 d . . . P1 P 0.01692(7) 0.39687(3) 0.56707(6) 0.0233(2) Uani 1 1 d . . . P2 P 0.24993(7) 0.41437(3) 0.63124(6) 0.0229(2) Uani 1 1 d . . . O O 0.19354(18) 0.24231(8) 0.58144(14) 0.0273(6) Uani 1 1 d . . . N1 N 0.0442(2) 0.34210(10) 0.61038(17) 0.0242(7) Uani 1 1 d . . . N2 N 0.2985(2) 0.35869(10) 0.61978(17) 0.0248(7) Uani 1 1 d . . . C1 C 0.1317(3) 0.42876(12) 0.5688(2) 0.0242(8) Uani 1 1 d . . . H1 H 0.1303 0.4565 0.5327 0.029 Uiso 1 1 calc R . . C2 C -0.0782(3) 0.43263(12) 0.6128(2) 0.0246(8) Uani 1 1 d . . . C3 C -0.0564(3) 0.48337(13) 0.6289(2) 0.0278(9) Uani 1 1 d . . . H3 H 0.0081 0.4972 0.6192 0.033 Uiso 1 1 calc R . . C4 C -0.1274(3) 0.51385(14) 0.6587(2) 0.0326(9) Uani 1 1 d . . . H4 H -0.1119 0.5484 0.6686 0.039 Uiso 1 1 calc R . . C5 C -0.2207(3) 0.49418(15) 0.6742(2) 0.0370(10) Uani 1 1 d . . . H5 H -0.2683 0.515 0.6961 0.044 Uiso 1 1 calc R . . C6 C -0.2450(3) 0.44393(15) 0.6576(2) 0.0351(10) Uani 1 1 d . . . H6 H -0.3094 0.4304 0.6679 0.042 Uiso 1 1 calc R . . C7 C -0.1750(3) 0.41351(14) 0.6258(2) 0.0308(9) Uani 1 1 d . . . H7 H -0.1928 0.3794 0.6129 0.037 Uiso 1 1 calc R . . C8 C -0.0523(3) 0.39402(12) 0.4606(2) 0.0251(8) Uani 1 1 d . . . C9 C -0.0099(3) 0.36555(14) 0.4043(2) 0.0342(10) Uani 1 1 d . . . H9 H 0.0525 0.3465 0.4227 0.041 Uiso 1 1 calc R . . C10 C -0.0563(3) 0.36437(15) 0.3228(2) 0.0398(10) Uani 1 1 d . . . H10 H -0.0262 0.3446 0.2856 0.048 Uiso 1 1 calc R . . C11 C -0.1472(3) 0.39227(15) 0.2952(2) 0.0391(10) Uani 1 1 d . . . H11 H -0.1781 0.3925 0.2387 0.047 Uiso 1 1 calc R . . C12 C -0.1919(3) 0.41935(14) 0.3492(2) 0.0372(10) Uani 1 1 d . . . H12 H -0.2556 0.4373 0.3305 0.045 Uiso 1 1 calc R . . C13 C -0.1449(3) 0.42082(13) 0.4314(2) 0.0308(9) Uani 1 1 d . . . H13 H -0.1762 0.4403 0.4683 0.037 Uiso 1 1 calc R . . C14 C 0.3453(3) 0.46280(12) 0.6205(2) 0.0232(8) Uani 1 1 d . . . C15 C 0.4247(3) 0.47345(13) 0.6877(2) 0.0299(9) Uani 1 1 d . . . H15 H 0.4286 0.4548 0.7369 0.036 Uiso 1 1 calc R . . C16 C 0.4977(3) 0.51099(14) 0.6833(2) 0.0358(10) Uani 1 1 d . . . H16 H 0.5518 0.5178 0.7293 0.043 Uiso 1 1 calc R . . C17 C 0.4925(3) 0.53840(14) 0.6130(2) 0.0352(10) Uani 1 1 d . . . H17 H 0.5425 0.5643 0.6104 0.042 Uiso 1 1 calc R . . C18 C 0.4145(3) 0.52826(14) 0.5457(2) 0.0341(10) Uani 1 1 d . . . H18 H 0.4105 0.5474 0.497 0.041 Uiso 1 1 calc R . . C19 C 0.3419(3) 0.49022(13) 0.5493(2) 0.0273(9) Uani 1 1 d . . . H19 H 0.2894 0.4829 0.5025 0.033 Uiso 1 1 calc R . . C20 C 0.2389(3) 0.41917(13) 0.7377(2) 0.0268(9) Uani 1 1 d . . . C21 C 0.1924(3) 0.46251(14) 0.7634(2) 0.0366(10) Uani 1 1 d . . . H21 H 0.1618 0.4869 0.7242 0.044 Uiso 1 1 calc R . . C22 C 0.1906(3) 0.47001(17) 0.8452(3) 0.0484(11) Uani 1 1 d . . . H22 H 0.1598 0.4997 0.8621 0.058 Uiso 1 1 calc R . . C23 C 0.2334(4) 0.43475(18) 0.9023(3) 0.0509(12) Uani 1 1 d . . . H23 H 0.2316 0.44 0.9585 0.061 Uiso 1 1 calc R . . C24 C 0.2788(3) 0.39167(17) 0.8782(3) 0.0445(11) Uani 1 1 d . . . H24 H 0.3083 0.3673 0.9177 0.053 Uiso 1 1 calc R . . C25 C 0.2814(3) 0.38408(14) 0.7965(2) 0.0341(9) Uani 1 1 d . . . H25 H 0.3128 0.3544 0.7804 0.041 Uiso 1 1 calc R . . C26 C -0.0354(3) 0.31340(12) 0.6420(2) 0.0257(8) Uani 1 1 d . . . C27 C -0.0521(3) 0.32273(13) 0.7212(2) 0.0294(9) Uani 1 1 d . . . C28 C -0.1272(3) 0.29414(14) 0.7518(3) 0.0376(10) Uani 1 1 d . . . H28 H -0.1392 0.3009 0.8053 0.045 Uiso 1 1 calc R . . C29 C -0.1849(3) 0.25617(14) 0.7063(3) 0.0372(10) Uani 1 1 d . . . C30 C -0.1644(3) 0.24688(13) 0.6297(3) 0.0354(10) Uani 1 1 d . . . H30 H -0.2019 0.2205 0.5983 0.042 Uiso 1 1 calc R . . C31 C -0.0908(3) 0.27448(13) 0.5955(2) 0.0294(9) Uani 1 1 d . . . C32 C 0.0081(3) 0.36192(15) 0.7766(2) 0.0394(10) Uani 1 1 d . . . H32A H 0.0786 0.3661 0.7635 0.059 Uiso 1 1 calc R . . H32B H 0.0149 0.3512 0.8336 0.059 Uiso 1 1 calc R . . H32C H -0.0301 0.3939 0.7686 0.059 Uiso 1 1 calc R . . C33 C -0.2682(3) 0.22811(16) 0.7411(3) 0.0530(12) Uani 1 1 d . . . H33A H -0.2697 0.2406 0.7962 0.079 Uiso 0.5 1 calc PR . . H33B H -0.2514 0.1922 0.7437 0.079 Uiso 0.5 1 calc PR . . H33C H -0.3375 0.2334 0.7059 0.079 Uiso 0.5 1 calc PR . . H33D H -0.3027 0.2035 0.701 0.079 Uiso 0.5 1 calc PR . . H33E H -0.321 0.2519 0.7535 0.079 Uiso 0.5 1 calc PR . . H33F H -0.2349 0.2107 0.7913 0.079 Uiso 0.5 1 calc PR . . C34 C -0.0732(3) 0.26136(14) 0.5116(2) 0.0364(10) Uani 1 1 d . . . H34A H -0.0988 0.2888 0.4738 0.055 Uiso 1 1 calc R . . H34B H -0.1118 0.2305 0.493 0.055 Uiso 1 1 calc R . . H34C H 0.0025 0.2562 0.5132 0.055 Uiso 1 1 calc R . . C35 C 0.3878(3) 0.35112(12) 0.5802(2) 0.0239(8) Uani 1 1 d . . . C36 C 0.4883(3) 0.34045(12) 0.6272(2) 0.0285(9) Uani 1 1 d . . . C37 C 0.5725(3) 0.33065(13) 0.5878(3) 0.0326(9) Uani 1 1 d . . . H37 H 0.6399 0.3237 0.6202 0.039 Uiso 1 1 calc R . . C38 C 0.5622(3) 0.33062(13) 0.5039(2) 0.0300(9) Uani 1 1 d . . . C39 C 0.4622(3) 0.34137(13) 0.4582(2) 0.0293(9) Uani 1 1 d . . . H39 H 0.4526 0.3417 0.4003 0.035 Uiso 1 1 calc R . . C40 C 0.3762(3) 0.35168(12) 0.4948(2) 0.0252(9) Uani 1 1 d . . . C41 C 0.5062(3) 0.33851(16) 0.7187(2) 0.0430(11) Uani 1 1 d . . . H41A H 0.4886 0.3712 0.7399 0.064 Uiso 1 1 calc R . . H41B H 0.5806 0.3307 0.7404 0.064 Uiso 1 1 calc R . . H41C H 0.4612 0.3124 0.7357 0.064 Uiso 1 1 calc R . . C42 C 0.6529(3) 0.31867(16) 0.4617(3) 0.0468(11) Uani 1 1 d . . . H42A H 0.6286 0.3204 0.4023 0.07 Uiso 0.5 1 calc PR . . H42B H 0.6792 0.2848 0.477 0.07 Uiso 0.5 1 calc PR . . H42C H 0.7099 0.3431 0.4783 0.07 Uiso 0.5 1 calc PR . . H42D H 0.7165 0.3118 0.5028 0.07 Uiso 0.5 1 calc PR . . H42E H 0.6659 0.3474 0.4281 0.07 Uiso 0.5 1 calc PR . . H42F H 0.6352 0.2891 0.4267 0.07 Uiso 0.5 1 calc PR . . C43 C 0.2718(3) 0.36255(15) 0.4402(2) 0.0402(10) Uani 1 1 d . . . H43A H 0.2789 0.3593 0.3829 0.06 Uiso 1 1 calc R . . H43B H 0.2495 0.3968 0.4503 0.06 Uiso 1 1 calc R . . H43C H 0.2187 0.3386 0.4519 0.06 Uiso 1 1 calc R . . C44 C 0.2279(3) 0.20254(12) 0.6363(2) 0.0265(9) Uani 1 1 d . . . C45 C 0.1496(3) 0.15829(12) 0.6142(2) 0.0267(9) Uani 1 1 d . . . C46 C 0.1029(3) 0.15081(14) 0.5332(2) 0.0369(10) Uani 1 1 d . . . H46 H 0.1172 0.1737 0.4929 0.044 Uiso 1 1 calc R . . C47 C 0.0354(3) 0.11046(15) 0.5096(2) 0.0435(11) Uani 1 1 d . . . H47 H 0.0045 0.106 0.4536 0.052 Uiso 1 1 calc R . . C48 C 0.0131(3) 0.07696(15) 0.5668(3) 0.0457(11) Uani 1 1 d . . . H48 H -0.0336 0.0496 0.5507 0.055 Uiso 1 1 calc R . . C49 C 0.0595(3) 0.08349(15) 0.6477(3) 0.0454(11) Uani 1 1 d . . . H49 H 0.045 0.0604 0.6876 0.054 Uiso 1 1 calc R . . C50 C 0.1276(3) 0.12371(14) 0.6713(2) 0.0373(10) Uani 1 1 d . . . H50 H 0.1594 0.1276 0.7273 0.045 Uiso 1 1 calc R . . C51 C 0.3380(3) 0.18403(13) 0.6255(2) 0.0294(9) Uani 1 1 d . . . C52 C 0.3829(3) 0.14085(15) 0.6639(3) 0.0477(12) Uani 1 1 d . . . H52 H 0.3447 0.1219 0.6969 0.057 Uiso 1 1 calc R . . C53 C 0.4820(4) 0.12486(17) 0.6550(3) 0.0603(14) Uani 1 1 d . . . H53 H 0.5118 0.0956 0.6828 0.072 Uiso 1 1 calc R . . C54 C 0.5378(3) 0.15084(16) 0.6063(3) 0.0536(12) Uani 1 1 d . . . H54 H 0.6047 0.1389 0.5985 0.064 Uiso 1 1 calc R . . C55 C 0.4961(3) 0.19444(16) 0.5687(3) 0.0455(11) Uani 1 1 d . . . H55 H 0.535 0.2132 0.5359 0.055 Uiso 1 1 calc R . . C56 C 0.3966(3) 0.21091(14) 0.5790(2) 0.0335(9) Uani 1 1 d . . . H56 H 0.3686 0.2412 0.5534 0.04 Uiso 1 1 calc R . . C57 C 0.2312(3) 0.22147(12) 0.7238(2) 0.0272(9) Uani 1 1 d . . . C58 C 0.3255(3) 0.23396(13) 0.7763(2) 0.0322(9) Uani 1 1 d . . . H58 H 0.391 0.2288 0.7592 0.039 Uiso 1 1 calc R . . C59 C 0.3246(3) 0.25379(14) 0.8532(2) 0.0390(10) Uani 1 1 d . . . H59 H 0.3894 0.2629 0.8876 0.047 Uiso 1 1 calc R . . C60 C 0.2313(4) 0.26045(14) 0.8804(2) 0.0411(11) Uani 1 1 d . . . H60 H 0.2315 0.273 0.9339 0.049 Uiso 1 1 calc R . . C61 C 0.1371(3) 0.24865(14) 0.8290(2) 0.0389(10) Uani 1 1 d . . . H61 H 0.0721 0.2533 0.847 0.047 Uiso 1 1 calc R . . C62 C 0.1366(3) 0.23005(13) 0.7513(2) 0.0342(10) Uani 1 1 d . . . H62 H 0.0711 0.223 0.7161 0.041 Uiso 1 1 calc R . . C63 C 0.6747(4) 0.39931(17) 0.9085(2) 0.0852(19) Uani 1 1 d G . . C64 C 0.7558(3) 0.4303(3) 0.8934(3) 0.218(7) Uani 1 1 d G . . H64 H 0.8208 0.416 0.8856 0.262 Uiso 1 1 calc R . . C65 C 0.7418(6) 0.4821(3) 0.8898(3) 0.257(11) Uani 1 1 d G . . H65 H 0.7972 0.5032 0.8795 0.308 Uiso 1 1 calc R . . C66 C 0.6467(8) 0.50291(15) 0.9012(3) 0.239(10) Uani 1 1 d G . . H66 H 0.6371 0.5383 0.8988 0.287 Uiso 1 1 calc R . . C67 C 0.5656(5) 0.4719(2) 0.9163(3) 0.175(5) Uani 1 1 d G . . H67 H 0.5006 0.4862 0.9241 0.21 Uiso 1 1 calc R . . C68 C 0.5796(3) 0.4201(2) 0.9199(2) 0.0806(17) Uani 1 1 d G . . H68 H 0.5242 0.399 0.9302 0.097 Uiso 1 1 calc R . . C69 C 0.6817(10) 0.3432(4) 0.9176(5) 0.218(6) Uani 1 1 d . . . H69A H 0.6157 0.3303 0.931 0.327 Uiso 0.5 1 calc PR . . H69B H 0.7409 0.3345 0.9617 0.327 Uiso 0.5 1 calc PR . . H69C H 0.693 0.3282 0.8663 0.327 Uiso 0.5 1 calc PR . . H69D H 0.7507 0.3317 0.9083 0.327 Uiso 0.5 1 calc PR . . H69E H 0.6255 0.3275 0.8776 0.327 Uiso 0.5 1 calc PR . . H69F H 0.6735 0.3339 0.973 0.327 Uiso 0.5 1 calc PR . . 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 Zn 0.0228(2) 0.0199(2) 0.0280(3) 0.00032(18) 0.00513(18) 0.00073(17) P1 0.0194(5) 0.0216(5) 0.0289(6) -0.0019(4) 0.0045(4) 0.0011(4) P2 0.0199(5) 0.0199(5) 0.0286(6) -0.0013(4) 0.0039(4) -0.0007(4) O 0.0383(15) 0.0206(13) 0.0222(14) -0.0012(10) 0.0041(11) 0.0053(10) N1 0.0229(16) 0.0244(16) 0.0254(17) 0.0006(13) 0.0048(13) -0.0010(13) N2 0.0199(16) 0.0213(16) 0.0337(18) -0.0023(13) 0.0065(14) 0.0011(12) C1 0.0190(19) 0.0208(19) 0.032(2) 0.0030(15) 0.0017(17) 0.0002(14) C2 0.022(2) 0.023(2) 0.029(2) -0.0029(15) 0.0023(16) 0.0017(15) C3 0.021(2) 0.033(2) 0.028(2) -0.0033(17) 0.0024(17) 0.0044(16) C4 0.031(2) 0.030(2) 0.033(2) -0.0061(17) -0.0017(19) 0.0044(18) C5 0.035(2) 0.042(3) 0.035(2) -0.0065(19) 0.0086(19) 0.0120(19) C6 0.023(2) 0.048(3) 0.036(2) 0.0008(19) 0.0101(18) 0.0036(18) C7 0.025(2) 0.030(2) 0.037(2) 0.0019(17) 0.0053(18) -0.0029(17) C8 0.022(2) 0.0210(19) 0.032(2) 0.0011(16) 0.0036(17) -0.0033(15) C9 0.024(2) 0.039(2) 0.038(3) -0.0065(19) 0.0033(19) 0.0025(17) C10 0.036(2) 0.050(3) 0.033(3) -0.0099(19) 0.004(2) -0.002(2) C11 0.042(3) 0.042(2) 0.029(2) -0.0002(19) -0.004(2) -0.006(2) C12 0.033(2) 0.035(2) 0.039(3) 0.0007(19) -0.005(2) 0.0053(18) C13 0.030(2) 0.028(2) 0.033(2) -0.0023(17) 0.0019(19) 0.0025(16) C14 0.0187(19) 0.0194(19) 0.032(2) -0.0056(16) 0.0052(17) 0.0028(14) C15 0.025(2) 0.032(2) 0.033(2) 0.0011(17) 0.0054(18) -0.0023(17) C16 0.025(2) 0.040(2) 0.040(3) -0.007(2) 0.0007(19) -0.0051(18) C17 0.030(2) 0.027(2) 0.049(3) -0.0012(19) 0.009(2) -0.0083(17) C18 0.031(2) 0.032(2) 0.041(3) 0.0055(18) 0.009(2) 0.0010(18) C19 0.022(2) 0.028(2) 0.031(2) -0.0020(17) 0.0041(17) 0.0020(16) C20 0.022(2) 0.026(2) 0.034(2) -0.0025(17) 0.0081(17) -0.0044(16) C21 0.038(2) 0.033(2) 0.039(3) -0.0070(18) 0.007(2) -0.0015(18) C22 0.054(3) 0.047(3) 0.048(3) -0.014(2) 0.019(2) -0.004(2) C23 0.058(3) 0.064(3) 0.033(3) -0.012(2) 0.013(2) -0.022(2) C24 0.045(3) 0.052(3) 0.036(3) 0.006(2) 0.005(2) -0.010(2) C25 0.034(2) 0.035(2) 0.034(3) 0.0022(19) 0.0087(19) -0.0063(18) C26 0.022(2) 0.021(2) 0.033(2) 0.0046(16) 0.0033(17) 0.0010(15) C27 0.025(2) 0.028(2) 0.035(2) 0.0058(17) 0.0033(18) 0.0013(16) C28 0.033(2) 0.043(2) 0.039(2) 0.0126(19) 0.011(2) 0.0058(19) C29 0.025(2) 0.031(2) 0.055(3) 0.014(2) 0.006(2) -0.0011(17) C30 0.025(2) 0.026(2) 0.053(3) 0.0042(19) 0.000(2) -0.0038(16) C31 0.023(2) 0.025(2) 0.038(2) 0.0036(17) 0.0002(18) 0.0037(16) C32 0.036(2) 0.052(3) 0.032(2) -0.0045(19) 0.0100(19) -0.0044(19) C33 0.035(3) 0.050(3) 0.075(3) 0.017(2) 0.014(2) -0.008(2) C34 0.032(2) 0.029(2) 0.046(3) -0.0086(18) 0.002(2) -0.0048(17) C35 0.022(2) 0.0152(18) 0.034(2) -0.0001(15) 0.0043(17) 0.0008(14) C36 0.026(2) 0.021(2) 0.037(2) 0.0020(16) 0.0037(18) 0.0033(15) C37 0.021(2) 0.027(2) 0.048(3) 0.0024(18) 0.0011(19) 0.0012(16) C38 0.026(2) 0.020(2) 0.046(3) -0.0011(17) 0.0126(19) -0.0006(15) C39 0.030(2) 0.024(2) 0.035(2) -0.0027(16) 0.0089(19) 0.0000(16) C40 0.023(2) 0.0170(19) 0.034(2) -0.0041(15) 0.0016(17) 0.0014(15) C41 0.029(2) 0.055(3) 0.043(3) 0.009(2) 0.000(2) 0.0128(19) C42 0.031(2) 0.054(3) 0.059(3) -0.005(2) 0.018(2) 0.001(2) C43 0.033(2) 0.050(3) 0.035(2) -0.0128(19) -0.0002(19) 0.0059(19) C44 0.036(2) 0.019(2) 0.024(2) 0.0050(15) 0.0035(17) 0.0065(16) C45 0.033(2) 0.022(2) 0.026(2) -0.0001(16) 0.0059(18) 0.0045(16) C46 0.047(3) 0.035(2) 0.030(2) 0.0033(18) 0.011(2) -0.0072(19) C47 0.056(3) 0.048(3) 0.024(2) -0.003(2) 0.001(2) -0.019(2) C48 0.059(3) 0.038(3) 0.039(3) -0.002(2) 0.008(2) -0.018(2) C49 0.059(3) 0.039(3) 0.038(3) 0.009(2) 0.011(2) -0.010(2) C50 0.052(3) 0.029(2) 0.029(2) 0.0038(18) 0.004(2) -0.0046(19) C51 0.035(2) 0.024(2) 0.029(2) -0.0009(17) 0.0043(18) 0.0024(17) C52 0.046(3) 0.033(2) 0.067(3) 0.013(2) 0.018(2) 0.008(2) C53 0.050(3) 0.046(3) 0.086(4) 0.016(3) 0.014(3) 0.020(2) C54 0.036(3) 0.046(3) 0.079(4) -0.002(3) 0.014(3) 0.010(2) C55 0.037(3) 0.046(3) 0.056(3) 0.000(2) 0.015(2) 0.000(2) C56 0.036(2) 0.029(2) 0.034(2) -0.0013(18) 0.0029(19) 0.0063(18) C57 0.037(2) 0.019(2) 0.025(2) 0.0039(15) 0.0052(19) 0.0029(16) C58 0.041(2) 0.026(2) 0.029(2) 0.0012(17) 0.0044(19) 0.0014(17) C59 0.051(3) 0.030(2) 0.031(2) 0.0016(18) -0.003(2) 0.0005(19) C60 0.067(3) 0.033(2) 0.021(2) 0.0014(17) 0.003(2) 0.013(2) C61 0.052(3) 0.039(2) 0.027(2) 0.0042(18) 0.008(2) 0.015(2) C62 0.043(3) 0.032(2) 0.026(2) 0.0031(17) 0.0020(19) 0.0072(18) C63 0.083(5) 0.117(5) 0.047(3) -0.010(3) -0.010(3) 0.029(4) C64 0.085(6) 0.51(2) 0.055(5) 0.079(9) -0.002(4) -0.091(10) C65 0.287(17) 0.36(2) 0.076(6) 0.118(10) -0.094(8) -0.242(15) C66 0.47(3) 0.087(6) 0.086(7) 0.013(5) -0.130(12) -0.065(10) C67 0.289(13) 0.158(9) 0.053(5) -0.014(5) -0.029(6) 0.126(10) C68 0.067(4) 0.124(5) 0.048(3) 0.012(3) 0.004(3) 0.013(4) C69 0.372(16) 0.148(9) 0.105(7) -0.016(6) -0.029(8) 0.140(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Zn O 1.859(2) . ? Zn N2 1.970(3) . ? Zn N1 1.988(3) . ? P1 N1 1.635(3) . ? P1 C1 1.700(3) . ? P1 C2 1.828(3) . ? P1 C8 1.828(4) . ? P2 N2 1.634(3) . ? P2 C1 1.716(3) . ? P2 C20 1.810(4) . ? P2 C14 1.813(3) . ? O C44 1.413(4) . ? N1 C26 1.455(4) . ? N2 C35 1.444(4) . ? C2 C3 1.395(5) . ? C2 C7 1.401(5) . ? C3 C4 1.384(5) . ? C4 C5 1.378(5) . ? C5 C6 1.389(5) . ? C6 C7 1.389(5) . ? C8 C9 1.395(5) . ? C8 C13 1.395(5) . ? C9 C10 1.376(5) . ? C10 C11 1.389(5) . ? C11 C12 1.363(5) . ? C12 C13 1.388(5) . ? C14 C19 1.387(5) . ? C14 C15 1.394(5) . ? C15 C16 1.383(5) . ? C16 C17 1.371(5) . ? C17 C18 1.382(5) . ? C18 C19 1.387(5) . ? C20 C25 1.388(5) . ? C20 C21 1.403(5) . ? C21 C22 1.382(6) . ? C22 C23 1.374(6) . ? C23 C24 1.382(6) . ? C24 C25 1.381(5) . ? C26 C27 1.398(5) . ? C26 C31 1.404(5) . ? C27 C28 1.401(5) . ? C27 C32 1.506(5) . ? C28 C29 1.390(5) . ? C29 C30 1.374(6) . ? C29 C33 1.509(5) . ? C30 C31 1.402(5) . ? C31 C34 1.498(5) . ? C35 C40 1.401(5) . ? C35 C36 1.409(5) . ? C36 C37 1.395(5) . ? C36 C41 1.499(5) . ? C37 C38 1.378(5) . ? C38 C39 1.395(5) . ? C38 C42 1.507(5) . ? C39 C40 1.388(5) . ? C40 C43 1.502(5) . ? C44 C57 1.535(5) . ? C44 C51 1.543(5) . ? C44 C45 1.548(5) . ? C45 C46 1.383(5) . ? C45 C50 1.390(5) . ? C46 C47 1.391(5) . ? C47 C48 1.374(5) . ? C48 C49 1.377(6) . ? C49 C50 1.392(5) . ? C51 C56 1.380(5) . ? C51 C52 1.387(5) . ? C52 C53 1.380(6) . ? C53 C54 1.368(6) . ? C54 C55 1.378(6) . ? C55 C56 1.396(5) . ? C57 C58 1.395(5) . ? C57 C62 1.399(5) . ? C58 C59 1.388(5) . ? C59 C60 1.374(6) . ? C60 C61 1.382(6) . ? C61 C62 1.384(5) . ? C63 C64 1.39 . ? C63 C68 1.39 . ? C63 C69 1.502(10) . ? C64 C65 1.39 . ? C65 C66 1.39 . ? C66 C67 1.39 . ? C67 C68 1.39 . ? 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 O Zn N2 124.68(11) . . ? O Zn N1 122.13(11) . . ? N2 Zn N1 111.93(11) . . ? N1 P1 C1 108.92(15) . . ? N1 P1 C2 112.68(15) . . ? C1 P1 C2 112.50(16) . . ? N1 P1 C8 114.54(15) . . ? C1 P1 C8 107.42(17) . . ? C2 P1 C8 100.56(16) . . ? N2 P2 C1 116.56(15) . . ? N2 P2 C20 106.35(15) . . ? C1 P2 C20 110.64(17) . . ? N2 P2 C14 110.58(15) . . ? C1 P2 C14 108.74(16) . . ? C20 P2 C14 103.11(16) . . ? C44 O Zn 125.6(2) . . ? C26 N1 P1 121.4(2) . . ? C26 N1 Zn 117.7(2) . . ? P1 N1 Zn 120.52(15) . . ? C35 N2 P2 122.4(2) . . ? C35 N2 Zn 121.7(2) . . ? P2 N2 Zn 108.26(14) . . ? P1 C1 P2 124.6(2) . . ? C3 C2 C7 118.3(3) . . ? C3 C2 P1 117.2(3) . . ? C7 C2 P1 124.2(3) . . ? C4 C3 C2 120.9(3) . . ? C5 C4 C3 120.2(4) . . ? C4 C5 C6 120.0(3) . . ? C7 C6 C5 119.9(4) . . ? C6 C7 C2 120.6(3) . . ? C9 C8 C13 117.5(3) . . ? C9 C8 P1 119.6(3) . . ? C13 C8 P1 122.9(3) . . ? C10 C9 C8 121.6(3) . . ? C9 C10 C11 119.6(4) . . ? C12 C11 C10 120.0(4) . . ? C11 C12 C13 120.4(4) . . ? C12 C13 C8 120.9(4) . . ? C19 C14 C15 118.6(3) . . ? C19 C14 P2 123.1(3) . . ? C15 C14 P2 118.2(3) . . ? C16 C15 C14 120.4(3) . . ? C17 C16 C15 120.4(4) . . ? C16 C17 C18 119.9(3) . . ? C17 C18 C19 120.0(4) . . ? C18 C19 C14 120.6(3) . . ? C25 C20 C21 118.2(4) . . ? C25 C20 P2 123.4(3) . . ? C21 C20 P2 118.3(3) . . ? C22 C21 C20 120.4(4) . . ? C23 C22 C21 120.3(4) . . ? C22 C23 C24 120.1(4) . . ? C25 C24 C23 119.9(4) . . ? C24 C25 C20 121.1(4) . . ? C27 C26 C31 119.9(3) . . ? C27 C26 N1 119.6(3) . . ? C31 C26 N1 120.4(3) . . ? C26 C27 C28 119.2(3) . . ? C26 C27 C32 123.2(3) . . ? C28 C27 C32 117.7(3) . . ? C29 C28 C27 122.1(4) . . ? C30 C29 C28 117.4(3) . . ? C30 C29 C33 122.9(4) . . ? C28 C29 C33 119.7(4) . . ? C29 C30 C31 123.1(4) . . ? C30 C31 C26 118.3(4) . . ? C30 C31 C34 119.3(3) . . ? C26 C31 C34 122.4(3) . . ? C40 C35 C36 118.4(3) . . ? C40 C35 N2 121.5(3) . . ? C36 C35 N2 120.1(3) . . ? C37 C36 C35 119.4(3) . . ? C37 C36 C41 119.3(3) . . ? C35 C36 C41 121.4(3) . . ? C38 C37 C36 122.9(3) . . ? C37 C38 C39 117.0(3) . . ? C37 C38 C42 122.6(3) . . ? C39 C38 C42 120.4(4) . . ? C40 C39 C38 122.1(4) . . ? C39 C40 C35 120.2(3) . . ? C39 C40 C43 118.0(3) . . ? C35 C40 C43 121.7(3) . . ? O C44 C57 108.5(3) . . ? O C44 C51 110.3(3) . . ? C57 C44 C51 110.8(3) . . ? O C44 C45 107.8(3) . . ? C57 C44 C45 112.0(3) . . ? C51 C44 C45 107.5(3) . . ? C46 C45 C50 117.6(3) . . ? C46 C45 C44 118.9(3) . . ? C50 C45 C44 123.4(3) . . ? C45 C46 C47 121.3(4) . . ? C48 C47 C46 120.4(4) . . ? C47 C48 C49 119.2(4) . . ? C48 C49 C50 120.4(4) . . ? C45 C50 C49 121.0(4) . . ? C56 C51 C52 117.6(4) . . ? C56 C51 C44 120.8(3) . . ? C52 C51 C44 121.6(3) . . ? C53 C52 C51 121.3(4) . . ? C54 C53 C52 120.5(4) . . ? C53 C54 C55 119.5(4) . . ? C54 C55 C56 119.8(4) . . ? C51 C56 C55 121.3(4) . . ? C58 C57 C62 117.6(3) . . ? C58 C57 C44 122.5(3) . . ? C62 C57 C44 119.7(3) . . ? C59 C58 C57 120.7(4) . . ? C60 C59 C58 121.0(4) . . ? C59 C60 C61 119.0(4) . . ? C60 C61 C62 120.6(4) . . ? C61 C62 C57 121.0(4) . . ? C64 C63 C68 120 . . ? C64 C63 C69 125.1(7) . . ? C68 C63 C69 114.8(7) . . ? C65 C64 C63 120 . . ? C64 C65 C66 120 . . ? C65 C66 C67 120 . . ? C68 C67 C66 120 . . ? C67 C68 C63 120 . . ? #===END data_msh8-(jun402) _database_code_CSD 190733 _audit_creation_date 2002-06-11T10:47:42-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[Zn(OCPh3)(MesNPPh2CHPPh2NPh)]' _chemical_formula_moiety 'C59 H52 N2 O1 P2 Zn1' _chemical_formula_sum 'C59 H52 N2 O P2 Zn' _chemical_formula_weight 932.34 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 10.4249(3) _cell_length_b 12.5215(3) _cell_length_c 19.3876(5) _cell_angle_alpha 96.599(1) _cell_angle_beta 94.940(1) _cell_angle_gamma 106.035(1) _cell_volume 2397.7(1) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10558 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.622 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0996 _diffrn_reflns_av_unetI/netI 0.0882 _diffrn_reflns_number 20170 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 23.02 _diffrn_reflns_theta_full 23.02 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 6629 _reflns_number_gt 4927 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0225P)^2^+2.6785P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 6629 _refine_ls_number_parameters 588 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0782 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1034 _refine_ls_wR_factor_gt 0.0934 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.364 _refine_diff_density_min -0.35 _refine_diff_density_rms 0.061 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Zn Zn -0.03127(4) -0.18542(4) 0.25275(2) 0.02076(14) Uani 1 1 d . . . P1 P -0.18546(10) -0.03814(8) 0.23885(5) 0.0194(2) Uani 1 1 d . . . P2 P -0.28782(10) -0.26862(8) 0.29155(5) 0.0193(2) Uani 1 1 d . . . O O 0.0988(2) -0.2092(2) 0.19896(13) 0.0250(6) Uani 1 1 d . . . N1 N -0.0336(3) -0.0229(3) 0.27252(16) 0.0219(7) Uani 1 1 d . . . N2 N -0.1376(3) -0.2658(3) 0.32276(16) 0.0223(8) Uani 1 1 d . . . C1 C -0.2656(4) -0.1815(3) 0.22793(19) 0.0189(9) Uani 1 1 d . . . H1 H -0.3015 -0.2161 0.1814 0.023 Uiso 1 1 calc R . . C2 C -0.2013(4) -0.0006(3) 0.1510(2) 0.0230(9) Uani 1 1 d . . . C3 C -0.2437(4) 0.0909(3) 0.1361(2) 0.0316(11) Uani 1 1 d . . . H3 H -0.2672 0.1369 0.1724 0.038 Uiso 1 1 calc R . . C4 C -0.2519(5) 0.1151(4) 0.0680(3) 0.0440(13) Uani 1 1 d . . . H4 H -0.2811 0.1778 0.058 0.053 Uiso 1 1 calc R . . C5 C -0.2182(5) 0.0495(4) 0.0150(3) 0.0467(13) Uani 1 1 d . . . H5 H -0.2256 0.0661 -0.0315 0.056 Uiso 1 1 calc R . . C6 C -0.1737(5) -0.0403(4) 0.0293(2) 0.0395(12) Uani 1 1 d . . . H6 H -0.1481 -0.0844 -0.0073 0.047 Uiso 1 1 calc R . . C7 C -0.1659(4) -0.0668(3) 0.0964(2) 0.0282(10) Uani 1 1 d . . . H7 H -0.1366 -0.1297 0.1058 0.034 Uiso 1 1 calc R . . C8 C -0.2723(4) 0.0477(3) 0.2866(2) 0.0250(10) Uani 1 1 d . . . C9 C -0.4094(4) 0.0044(4) 0.2904(2) 0.0351(11) Uani 1 1 d . . . H9 H -0.4546 -0.0718 0.2721 0.042 Uiso 1 1 calc R . . C10 C -0.4795(5) 0.0725(5) 0.3208(3) 0.0527(14) Uani 1 1 d . . . H10 H -0.5732 0.043 0.323 0.063 Uiso 1 1 calc R . . C11 C -0.4150(6) 0.1824(5) 0.3480(3) 0.0602(16) Uani 1 1 d . . . H11 H -0.4641 0.2285 0.3688 0.072 Uiso 1 1 calc R . . C12 C -0.2807(6) 0.2257(4) 0.3451(2) 0.0522(14) Uani 1 1 d . . . H12 H -0.2367 0.3018 0.364 0.063 Uiso 1 1 calc R . . C13 C -0.2079(5) 0.1596(4) 0.3147(2) 0.0385(11) Uani 1 1 d . . . H13 H -0.1144 0.1903 0.3129 0.046 Uiso 1 1 calc R . . C14 C -0.3798(4) -0.2335(3) 0.36228(19) 0.0220(9) Uani 1 1 d . . . C15 C -0.3105(4) -0.1472(4) 0.4153(2) 0.0324(11) Uani 1 1 d . . . H15 H -0.2169 -0.1134 0.4154 0.039 Uiso 1 1 calc R . . C16 C -0.3764(5) -0.1099(4) 0.4678(2) 0.0400(12) Uani 1 1 d . . . H16 H -0.3284 -0.0496 0.5032 0.048 Uiso 1 1 calc R . . C17 C -0.5109(5) -0.1597(4) 0.4689(2) 0.0461(13) Uani 1 1 d . . . H17 H -0.556 -0.1347 0.5052 0.055 Uiso 1 1 calc R . . C18 C -0.5802(5) -0.2464(4) 0.4168(3) 0.0537(14) Uani 1 1 d . . . H18 H -0.6735 -0.2807 0.4174 0.064 Uiso 1 1 calc R . . C19 C -0.5153(4) -0.2836(4) 0.3640(2) 0.0403(12) Uani 1 1 d . . . H19 H -0.5638 -0.3438 0.3287 0.048 Uiso 1 1 calc R . . C20 C -0.3852(4) -0.4056(3) 0.24567(19) 0.0222(9) Uani 1 1 d . . . C21 C -0.5107(4) -0.4221(3) 0.2072(2) 0.0270(10) Uani 1 1 d . . . H21 H -0.5493 -0.3617 0.2072 0.032 Uiso 1 1 calc R . . C22 C -0.5789(5) -0.5261(4) 0.1691(2) 0.0390(12) Uani 1 1 d . . . H22 H -0.665 -0.5375 0.144 0.047 Uiso 1 1 calc R . . C23 C -0.5211(5) -0.6127(4) 0.1680(2) 0.0422(13) Uani 1 1 d . . . H23 H -0.5668 -0.6836 0.1412 0.051 Uiso 1 1 calc R . . C24 C -0.3967(5) -0.5969(4) 0.2057(2) 0.0382(12) Uani 1 1 d . . . H24 H -0.3573 -0.6569 0.2047 0.046 Uiso 1 1 calc R . . C25 C -0.3292(4) -0.4933(3) 0.2450(2) 0.0276(10) Uani 1 1 d . . . H25 H -0.2445 -0.483 0.2713 0.033 Uiso 1 1 calc R . . C26 C 0.0735(4) 0.0771(3) 0.2967(2) 0.0203(9) Uani 1 1 d . . . C27 C 0.1002(4) 0.1183(3) 0.3686(2) 0.0221(9) Uani 1 1 d . . . C28 C 0.2047(4) 0.2161(3) 0.3924(2) 0.0283(10) Uani 1 1 d . . . H28 H 0.2211 0.2441 0.441 0.034 Uiso 1 1 calc R . . C29 C 0.2850(4) 0.2736(3) 0.3477(2) 0.0327(11) Uani 1 1 d . . . C30 C 0.2618(4) 0.2280(3) 0.2778(2) 0.0346(11) Uani 1 1 d . . . H30 H 0.3184 0.2649 0.2466 0.042 Uiso 1 1 calc R . . C31 C 0.1592(4) 0.1306(3) 0.2511(2) 0.0256(10) Uani 1 1 d . . . C32 C 0.0183(4) 0.0586(4) 0.4200(2) 0.0343(11) Uani 1 1 d . . . H32A H 0.0605 0.0914 0.4677 0.051 Uiso 1 1 calc R . . H32B H 0.0135 -0.0212 0.4123 0.051 Uiso 1 1 calc R . . H32C H -0.0727 0.0666 0.4136 0.051 Uiso 1 1 calc R . . C33 C 0.3919(5) 0.3843(4) 0.3745(3) 0.0519(14) Uani 1 1 d . . . H33A H 0.4383 0.4128 0.3355 0.078 Uiso 0.5 1 calc PR . . H33B H 0.457 0.3724 0.4102 0.078 Uiso 0.5 1 calc PR . . H33C H 0.3492 0.439 0.3949 0.078 Uiso 0.5 1 calc PR . . H33D H 0.3914 0.4033 0.4249 0.078 Uiso 0.5 1 calc PR . . H33E H 0.3727 0.4437 0.3502 0.078 Uiso 0.5 1 calc PR . . H33F H 0.4805 0.3771 0.3655 0.078 Uiso 0.5 1 calc PR . . C34 C 0.1463(5) 0.0843(4) 0.1750(2) 0.0408(12) Uani 1 1 d . . . H34A H 0.0762 0.1072 0.1488 0.061 Uiso 1 1 calc R . . H34B H 0.1221 0.0021 0.1697 0.061 Uiso 1 1 calc R . . H34C H 0.2322 0.1132 0.1569 0.061 Uiso 1 1 calc R . . C35 C -0.1011(4) -0.3034(3) 0.38553(19) 0.0230(9) Uani 1 1 d . . . C36 C 0.0298(4) -0.2561(4) 0.4191(2) 0.0291(10) Uani 1 1 d . . . H36 H 0.0916 -0.2011 0.3989 0.035 Uiso 1 1 calc R . . C37 C 0.0711(5) -0.2881(4) 0.4815(2) 0.0383(12) Uani 1 1 d . . . H37 H 0.1603 -0.2543 0.5039 0.046 Uiso 1 1 calc R . . C38 C -0.0161(5) -0.3684(4) 0.5113(2) 0.0424(12) Uani 1 1 d . . . H38 H 0.0123 -0.3905 0.5539 0.051 Uiso 1 1 calc R . . C39 C -0.1457(5) -0.4166(4) 0.4784(2) 0.0395(12) Uani 1 1 d . . . H39 H -0.2064 -0.4724 0.4986 0.047 Uiso 1 1 calc R . . C40 C -0.1883(4) -0.3847(3) 0.4164(2) 0.0275(10) Uani 1 1 d . . . H40 H -0.2779 -0.4187 0.3947 0.033 Uiso 1 1 calc R . . C41 C 0.0951(4) -0.3058(3) 0.15327(19) 0.0202(9) Uani 1 1 d . . . C42 C 0.2278(4) -0.2821(3) 0.1202(2) 0.0220(9) Uani 1 1 d . . . C43 C 0.3243(4) -0.1796(3) 0.1394(2) 0.0273(10) Uani 1 1 d . . . H43 H 0.3097 -0.1258 0.1742 0.033 Uiso 1 1 calc R . . C44 C 0.4423(4) -0.1542(4) 0.1085(2) 0.0332(11) Uani 1 1 d . . . H44 H 0.5072 -0.0831 0.1221 0.04 Uiso 1 1 calc R . . C45 C 0.4660(4) -0.2313(4) 0.0582(2) 0.0329(11) Uani 1 1 d . . . H45 H 0.5466 -0.2136 0.0369 0.039 Uiso 1 1 calc R . . C46 C 0.3717(4) -0.3341(4) 0.0394(2) 0.0353(11) Uani 1 1 d . . . H46 H 0.3873 -0.3884 0.0052 0.042 Uiso 1 1 calc R . . C47 C 0.2535(4) -0.3589(3) 0.0701(2) 0.0291(10) Uani 1 1 d . . . H47 H 0.1889 -0.4301 0.0565 0.035 Uiso 1 1 calc R . . C48 C 0.0848(4) -0.4070(3) 0.1937(2) 0.0212(9) Uani 1 1 d . . . C49 C 0.0317(4) -0.5182(3) 0.1621(2) 0.0287(10) Uani 1 1 d . . . H49 H -0.0004 -0.5342 0.1136 0.034 Uiso 1 1 calc R . . C50 C 0.0253(4) -0.6060(4) 0.2009(3) 0.0396(12) Uani 1 1 d . . . H50 H -0.0093 -0.6815 0.1784 0.048 Uiso 1 1 calc R . . C51 C 0.0688(5) -0.5842(4) 0.2717(3) 0.0424(12) Uani 1 1 d . . . H51 H 0.0629 -0.6441 0.2983 0.051 Uiso 1 1 calc R . . C52 C 0.1205(5) -0.4752(4) 0.3032(2) 0.0408(12) Uani 1 1 d . . . H52 H 0.1498 -0.4596 0.352 0.049 Uiso 1 1 calc R . . C53 C 0.1306(4) -0.3873(3) 0.2648(2) 0.0301(10) Uani 1 1 d . . . H53 H 0.1696 -0.3124 0.2873 0.036 Uiso 1 1 calc R . . C54 C -0.0270(4) -0.3300(3) 0.09700(19) 0.0205(9) Uani 1 1 d . . . C55 C -0.0186(4) -0.2988(3) 0.0305(2) 0.0286(10) Uani 1 1 d . . . H55 H 0.0671 -0.268 0.0162 0.034 Uiso 1 1 calc R . . C56 C -0.1338(4) -0.3122(4) -0.0149(2) 0.0353(11) Uani 1 1 d . . . H56 H -0.1264 -0.2916 -0.0604 0.042 Uiso 1 1 calc R . . C57 C -0.2603(4) -0.3556(4) 0.0056(2) 0.0356(11) Uani 1 1 d . . . H57 H -0.3392 -0.3634 -0.0252 0.043 Uiso 1 1 calc R . . C58 C -0.2697(4) -0.3872(4) 0.0711(2) 0.0339(11) Uani 1 1 d . . . H58 H -0.3556 -0.4171 0.0855 0.041 Uiso 1 1 calc R . . C59 C -0.1550(4) -0.3754(3) 0.1159(2) 0.0283(10) Uani 1 1 d . . . H59 H -0.1632 -0.3988 0.1606 0.034 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 Zn 0.0214(3) 0.0208(3) 0.0220(3) 0.0028(2) 0.0063(2) 0.0083(2) P1 0.0217(6) 0.0193(6) 0.0188(6) 0.0034(4) 0.0032(4) 0.0080(5) P2 0.0202(6) 0.0199(6) 0.0185(6) 0.0045(4) 0.0048(4) 0.0052(5) O 0.0225(15) 0.0207(15) 0.0318(16) -0.0010(13) 0.0090(12) 0.0063(12) N1 0.0231(18) 0.0191(17) 0.0210(18) -0.0002(14) -0.0003(14) 0.0043(15) N2 0.0213(18) 0.0274(19) 0.0204(18) 0.0069(15) 0.0047(14) 0.0089(15) C1 0.025(2) 0.018(2) 0.014(2) 0.0002(17) 0.0041(17) 0.0070(18) C2 0.019(2) 0.022(2) 0.026(2) 0.0083(19) 0.0005(18) 0.0000(18) C3 0.034(3) 0.029(2) 0.035(3) 0.013(2) 0.009(2) 0.010(2) C4 0.052(3) 0.040(3) 0.044(3) 0.024(3) 0.000(3) 0.015(2) C5 0.065(3) 0.039(3) 0.030(3) 0.018(2) -0.003(3) 0.002(3) C6 0.053(3) 0.036(3) 0.025(3) 0.007(2) 0.007(2) 0.005(2) C7 0.040(3) 0.021(2) 0.023(2) 0.0031(19) 0.008(2) 0.005(2) C8 0.033(2) 0.031(2) 0.017(2) 0.0027(19) 0.0026(18) 0.018(2) C9 0.034(3) 0.044(3) 0.036(3) 0.008(2) 0.015(2) 0.021(2) C10 0.044(3) 0.075(4) 0.059(4) 0.022(3) 0.025(3) 0.038(3) C11 0.074(4) 0.081(5) 0.044(3) -0.005(3) 0.008(3) 0.058(4) C12 0.071(4) 0.045(3) 0.044(3) -0.019(3) -0.017(3) 0.039(3) C13 0.040(3) 0.039(3) 0.039(3) -0.006(2) -0.008(2) 0.023(2) C14 0.023(2) 0.024(2) 0.019(2) 0.0047(18) 0.0010(18) 0.0070(19) C15 0.030(2) 0.037(3) 0.029(3) -0.001(2) 0.005(2) 0.008(2) C16 0.048(3) 0.041(3) 0.029(3) -0.007(2) 0.003(2) 0.016(2) C17 0.046(3) 0.062(3) 0.034(3) 0.002(3) 0.020(2) 0.019(3) C18 0.032(3) 0.067(4) 0.053(3) -0.011(3) 0.022(3) 0.002(3) C19 0.027(3) 0.043(3) 0.042(3) -0.006(2) 0.013(2) -0.002(2) C20 0.027(2) 0.020(2) 0.020(2) 0.0067(18) 0.0048(18) 0.0039(18) C21 0.028(2) 0.028(2) 0.023(2) 0.0069(19) 0.0054(19) 0.003(2) C22 0.040(3) 0.037(3) 0.030(3) 0.006(2) -0.001(2) -0.005(2) C23 0.059(3) 0.026(3) 0.030(3) 0.003(2) 0.005(2) -0.006(2) C24 0.062(3) 0.022(2) 0.037(3) 0.008(2) 0.016(3) 0.017(2) C25 0.037(3) 0.023(2) 0.024(2) 0.0077(19) 0.0088(19) 0.008(2) C26 0.020(2) 0.016(2) 0.028(2) 0.0005(18) 0.0036(18) 0.0101(18) C27 0.021(2) 0.021(2) 0.026(2) 0.0044(19) 0.0024(18) 0.0085(18) C28 0.032(2) 0.023(2) 0.029(2) -0.005(2) -0.005(2) 0.013(2) C29 0.020(2) 0.023(2) 0.053(3) 0.009(2) 0.004(2) 0.0028(19) C30 0.035(3) 0.026(2) 0.046(3) 0.013(2) 0.014(2) 0.009(2) C31 0.026(2) 0.022(2) 0.029(2) 0.0043(19) 0.0114(19) 0.0052(19) C32 0.040(3) 0.034(3) 0.025(2) 0.002(2) 0.002(2) 0.006(2) C33 0.042(3) 0.031(3) 0.075(4) 0.000(3) 0.006(3) 0.001(2) C34 0.044(3) 0.041(3) 0.035(3) 0.010(2) 0.019(2) 0.002(2) C35 0.029(2) 0.026(2) 0.020(2) 0.0045(19) 0.0068(19) 0.016(2) C36 0.031(3) 0.036(3) 0.025(2) 0.004(2) 0.005(2) 0.016(2) C37 0.037(3) 0.055(3) 0.029(3) 0.001(2) -0.001(2) 0.027(2) C38 0.060(3) 0.059(3) 0.021(2) 0.007(2) 0.002(2) 0.039(3) C39 0.062(3) 0.037(3) 0.028(3) 0.015(2) 0.011(2) 0.022(3) C40 0.036(3) 0.025(2) 0.026(2) 0.0063(19) 0.004(2) 0.014(2) C41 0.024(2) 0.019(2) 0.021(2) -0.0006(18) 0.0070(17) 0.0102(18) C42 0.019(2) 0.022(2) 0.026(2) 0.0030(19) 0.0100(18) 0.0076(19) C43 0.025(2) 0.025(2) 0.032(2) 0.0026(19) 0.0033(19) 0.008(2) C44 0.021(2) 0.030(3) 0.046(3) 0.011(2) 0.008(2) 0.001(2) C45 0.021(2) 0.043(3) 0.041(3) 0.014(2) 0.013(2) 0.014(2) C46 0.031(3) 0.044(3) 0.039(3) 0.009(2) 0.017(2) 0.019(2) C47 0.027(2) 0.027(2) 0.036(3) 0.005(2) 0.013(2) 0.008(2) C48 0.015(2) 0.023(2) 0.029(2) 0.0029(19) 0.0079(18) 0.0095(18) C49 0.034(2) 0.022(2) 0.031(2) 0.005(2) 0.010(2) 0.007(2) C50 0.041(3) 0.022(2) 0.057(3) 0.010(2) 0.013(2) 0.006(2) C51 0.047(3) 0.042(3) 0.047(3) 0.026(3) 0.013(2) 0.018(2) C52 0.049(3) 0.040(3) 0.037(3) 0.012(2) 0.003(2) 0.016(2) C53 0.028(2) 0.027(2) 0.034(3) 0.002(2) -0.002(2) 0.007(2) C54 0.024(2) 0.017(2) 0.019(2) -0.0027(17) 0.0036(17) 0.0064(18) C55 0.035(3) 0.029(2) 0.026(2) 0.001(2) 0.012(2) 0.015(2) C56 0.045(3) 0.042(3) 0.024(2) 0.003(2) 0.005(2) 0.022(2) C57 0.033(3) 0.043(3) 0.030(3) -0.010(2) -0.005(2) 0.019(2) C58 0.025(2) 0.039(3) 0.033(3) -0.009(2) 0.004(2) 0.008(2) C59 0.027(2) 0.032(2) 0.023(2) -0.0020(19) 0.0045(19) 0.007(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Zn O 1.846(3) . ? Zn N2 2.010(3) . ? Zn N1 2.034(3) . ? P1 N1 1.611(3) . ? P1 C1 1.737(4) . ? P1 C8 1.813(4) . ? P1 C2 1.824(4) . ? P2 N2 1.619(3) . ? P2 C1 1.728(3) . ? P2 C20 1.816(4) . ? P2 C14 1.820(4) . ? O C41 1.405(4) . ? N1 C26 1.427(5) . ? N2 C35 1.413(4) . ? C2 C3 1.388(5) . ? C2 C7 1.405(6) . ? C3 C4 1.389(6) . ? C4 C5 1.371(7) . ? C5 C6 1.377(6) . ? C6 C7 1.381(5) . ? C8 C9 1.393(6) . ? C8 C13 1.397(6) . ? C9 C10 1.384(6) . ? C10 C11 1.373(7) . ? C11 C12 1.363(7) . ? C12 C13 1.386(6) . ? C14 C19 1.383(5) . ? C14 C15 1.389(6) . ? C15 C16 1.385(6) . ? C16 C17 1.370(6) . ? C17 C18 1.382(7) . ? C18 C19 1.382(6) . ? C20 C25 1.378(5) . ? C20 C21 1.399(5) . ? C21 C22 1.386(6) . ? C22 C23 1.378(6) . ? C23 C24 1.384(6) . ? C24 C25 1.390(6) . ? C26 C31 1.404(5) . ? C26 C27 1.406(5) . ? C27 C28 1.395(5) . ? C27 C32 1.499(5) . ? C28 C29 1.380(6) . ? C29 C30 1.382(6) . ? C29 C33 1.521(6) . ? C30 C31 1.393(6) . ? C31 C34 1.501(6) . ? C35 C40 1.394(5) . ? C35 C36 1.396(5) . ? C36 C37 1.389(5) . ? C37 C38 1.374(6) . ? C38 C39 1.381(6) . ? C39 C40 1.385(5) . ? C41 C54 1.541(5) . ? C41 C42 1.543(5) . ? C41 C48 1.549(5) . ? C42 C43 1.382(5) . ? C42 C47 1.382(5) . ? C43 C44 1.389(5) . ? C44 C45 1.379(6) . ? C45 C46 1.375(6) . ? C46 C47 1.388(5) . ? C48 C53 1.389(5) . ? C48 C49 1.393(5) . ? C49 C50 1.392(5) . ? C50 C51 1.380(6) . ? C51 C52 1.368(6) . ? C52 C53 1.383(6) . ? C54 C55 1.392(5) . ? C54 C59 1.396(5) . ? C55 C56 1.385(6) . ? C56 C57 1.392(6) . ? C57 C58 1.374(6) . ? C58 C59 1.379(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 O Zn N2 135.92(12) . . ? O Zn N1 115.06(12) . . ? N2 Zn N1 105.87(13) . . ? N1 P1 C1 105.74(17) . . ? N1 P1 C8 114.74(18) . . ? C1 P1 C8 114.43(18) . . ? N1 P1 C2 114.87(17) . . ? C1 P1 C2 104.31(18) . . ? C8 P1 C2 102.52(18) . . ? N2 P2 C1 105.25(17) . . ? N2 P2 C20 112.85(18) . . ? C1 P2 C20 105.08(17) . . ? N2 P2 C14 109.99(17) . . ? C1 P2 C14 116.67(18) . . ? C20 P2 C14 107.07(18) . . ? C41 O Zn 128.3(2) . . ? C26 N1 P1 129.9(3) . . ? C26 N1 Zn 130.4(2) . . ? P1 N1 Zn 98.78(15) . . ? C35 N2 P2 126.4(2) . . ? C35 N2 Zn 133.4(2) . . ? P2 N2 Zn 100.01(14) . . ? P2 C1 P1 127.7(2) . . ? P2 C1 Zn 81.46(14) . . ? P1 C1 Zn 80.90(14) . . ? C3 C2 C7 118.9(4) . . ? C3 C2 P1 123.1(3) . . ? C7 C2 P1 117.9(3) . . ? C2 C3 C4 120.0(4) . . ? C5 C4 C3 120.7(4) . . ? C4 C5 C6 119.9(4) . . ? C5 C6 C7 120.4(5) . . ? C6 C7 C2 120.0(4) . . ? C9 C8 C13 118.9(4) . . ? C9 C8 P1 119.3(3) . . ? C13 C8 P1 121.6(3) . . ? C10 C9 C8 119.8(5) . . ? C11 C10 C9 120.6(5) . . ? C12 C11 C10 120.2(5) . . ? C11 C12 C13 120.6(5) . . ? C12 C13 C8 119.9(4) . . ? C19 C14 C15 118.7(4) . . ? C19 C14 P2 123.7(3) . . ? C15 C14 P2 117.5(3) . . ? C16 C15 C14 120.8(4) . . ? C17 C16 C15 120.1(4) . . ? C16 C17 C18 119.6(4) . . ? C17 C18 C19 120.6(4) . . ? C18 C19 C14 120.2(4) . . ? C25 C20 C21 119.5(4) . . ? C25 C20 P2 118.7(3) . . ? C21 C20 P2 121.7(3) . . ? C22 C21 C20 120.4(4) . . ? C23 C22 C21 119.7(4) . . ? C22 C23 C24 120.2(4) . . ? C23 C24 C25 120.2(4) . . ? C20 C25 C24 120.0(4) . . ? C31 C26 C27 119.1(3) . . ? C31 C26 N1 121.5(3) . . ? C27 C26 N1 119.3(3) . . ? C28 C27 C26 119.4(4) . . ? C28 C27 C32 119.6(4) . . ? C26 C27 C32 121.0(3) . . ? C29 C28 C27 122.2(4) . . ? C28 C29 C30 117.4(4) . . ? C28 C29 C33 121.0(4) . . ? C30 C29 C33 121.7(4) . . ? C29 C30 C31 123.0(4) . . ? C30 C31 C26 118.7(4) . . ? C30 C31 C34 119.1(4) . . ? C26 C31 C34 122.1(3) . . ? C40 C35 C36 117.7(3) . . ? C40 C35 N2 124.0(3) . . ? C36 C35 N2 118.3(3) . . ? C37 C36 C35 121.1(4) . . ? C38 C37 C36 120.5(4) . . ? C37 C38 C39 119.1(4) . . ? C38 C39 C40 120.9(4) . . ? C39 C40 C35 120.7(4) . . ? O C41 C54 108.0(3) . . ? O C41 C42 107.9(3) . . ? C54 C41 C42 111.1(3) . . ? O C41 C48 110.7(3) . . ? C54 C41 C48 110.7(3) . . ? C42 C41 C48 108.4(3) . . ? C43 C42 C47 117.9(4) . . ? C43 C42 C41 119.6(3) . . ? C47 C42 C41 122.5(3) . . ? C42 C43 C44 120.8(4) . . ? C45 C44 C43 120.6(4) . . ? C46 C45 C44 119.1(4) . . ? C45 C46 C47 120.1(4) . . ? C42 C47 C46 121.4(4) . . ? C53 C48 C49 117.8(4) . . ? C53 C48 C41 119.2(3) . . ? C49 C48 C41 123.0(3) . . ? C50 C49 C48 120.6(4) . . ? C51 C50 C49 120.4(4) . . ? C52 C51 C50 119.2(4) . . ? C51 C52 C53 120.8(4) . . ? C52 C53 C48 121.1(4) . . ? C55 C54 C59 117.7(4) . . ? C55 C54 C41 123.7(3) . . ? C59 C54 C41 118.2(3) . . ? C56 C55 C54 120.8(4) . . ? C55 C56 C57 120.4(4) . . ? C58 C57 C56 119.3(4) . . ? C57 C58 C59 120.3(4) . . ? C58 C59 C54 121.5(4) . . ? #===END data_msh9-(dec1601) _database_code_CSD 190734 _audit_creation_date 2002-01-08T09:58:44-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; '[Zn(OSiPh3)2(MesNPPh2CH2PPh2NMes)].2(toluene)' ; _chemical_formula_moiety '(C79 H74 N2 O2 P2 Si2 Zn1).2(C7 H8)' _chemical_formula_sum 'C93 H90 N2 O2 P2 Si2 Zn' _chemical_formula_weight 1451.16 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.7106(3) _cell_length_b 21.5304(4) _cell_length_c 29.7106(8) _cell_angle_alpha 90 _cell_angle_beta 101.2890 _cell_angle_gamma 90 _cell_volume 7973.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 22185 _cell_measurement_theta_min 4.076 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3064 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.428 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.885 _exptl_absorpt_correction_T_max 0.949 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0718 _diffrn_reflns_av_unetI/netI 0.0753 _diffrn_reflns_number 33679 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 4.1 _diffrn_reflns_theta_max 22.99 _diffrn_reflns_theta_full 22.99 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 10993 _reflns_number_gt 7871 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; There are 3 independent molecules of tolene solvate. All are poorly defined. Two are disordered across inversion centres and the third is disordered in a general position. For all three the C atom positions were left isotropc and the H atoms were omitted. Distance constraints (SADI) were applied. 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^)+(0.0659P)^2^+11.2396P] 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 'riding mode' _refine_ls_extinction_method none _refine_ls_number_reflns 10993 _refine_ls_number_parameters 883 _refine_ls_number_restraints 178 _refine_ls_R_factor_all 0.0923 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1535 _refine_ls_wR_factor_gt 0.1369 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.714 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.068 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Zn Zn 0.40248(4) 0.33198(2) 0.332968(16) 0.02225(16) Uani 1 1 d . A 1 P1 P 0.16162(9) 0.28327(5) 0.32634(4) 0.0254(3) Uani 1 1 d . A 1 P2 P 0.21758(9) 0.42012(5) 0.36602(4) 0.0244(3) Uani 1 1 d . A 1 Si1 Si 0.49929(10) 0.34611(5) 0.23311(4) 0.0273(3) Uani 1 1 d . A 1 Si2 Si 0.61701(10) 0.29533(5) 0.41938(4) 0.0268(3) Uani 1 1 d . A 1 O1 O 0.4425(2) 0.34870(13) 0.27601(10) 0.0306(7) Uani 1 1 d . A 1 O2 O 0.5113(2) 0.30699(13) 0.38234(10) 0.0319(7) Uani 1 1 d . A 1 N1 N 0.2848(3) 0.26537(15) 0.33158(12) 0.0237(8) Uani 1 1 d . A 1 N2 N 0.3226(3) 0.41300(15) 0.34468(12) 0.0245(8) Uani 1 1 d . A 1 C1 C 0.1473(4) 0.3466(2) 0.36502(17) 0.0264(11) Uani 1 1 d . A 1 H1A H 0.079(4) 0.360(2) 0.3635(15) 0.036(13) Uiso 1 1 d . B 1 H1B H 0.172(3) 0.3310(18) 0.3950(15) 0.023(11) Uiso 1 1 d . C 1 C2 C 0.0794(3) 0.22165(19) 0.34188(15) 0.0268(10) Uani 1 1 d . A 1 C3 C 0.0163(4) 0.2278(2) 0.37476(17) 0.0403(13) Uani 1 1 d . A 1 H3 H 0.0136 0.2665 0.39 0.048 Uiso 1 1 calc R A 1 C4 C -0.0432(4) 0.1776(2) 0.38552(19) 0.0492(14) Uani 1 1 d . A 1 H4 H -0.0865 0.1819 0.408 0.059 Uiso 1 1 calc R A 1 C5 C -0.0391(4) 0.1217(2) 0.36356(18) 0.0447(13) Uani 1 1 d . A 1 H5 H -0.0789 0.0873 0.3713 0.054 Uiso 1 1 calc R A 1 C6 C 0.0226(4) 0.1151(2) 0.33031(18) 0.0419(13) Uani 1 1 d . A 1 H6 H 0.0246 0.0766 0.3149 0.05 Uiso 1 1 calc R A 1 C7 C 0.0813(4) 0.1649(2) 0.31966(16) 0.0342(11) Uani 1 1 d . A 1 H7 H 0.1237 0.1605 0.2968 0.041 Uiso 1 1 calc R A 1 C8 C 0.0951(3) 0.30648(19) 0.26946(15) 0.0284(11) Uani 1 1 d . A 1 C9 C 0.1544(4) 0.3236(2) 0.23650(15) 0.0321(11) Uani 1 1 d . A 1 H9 H 0.2305 0.3221 0.2437 0.039 Uiso 1 1 calc R A 1 C10 C 0.1027(4) 0.3426(2) 0.19360(18) 0.0460(14) Uani 1 1 d . A 1 H10 H 0.1434 0.3544 0.1714 0.055 Uiso 1 1 calc R A 1 C11 C -0.0073(5) 0.3446(3) 0.18281(19) 0.0553(16) Uani 1 1 d . A 1 H11 H -0.0424 0.3577 0.1531 0.066 Uiso 1 1 calc R A 1 C12 C -0.0668(4) 0.3275(3) 0.2149(2) 0.0549(16) Uani 1 1 d . A 1 H12 H -0.1429 0.3294 0.2073 0.066 Uiso 1 1 calc R A 1 C13 C -0.0166(4) 0.3076(2) 0.25823(18) 0.0427(13) Uani 1 1 d . A 1 H13 H -0.0579 0.2948 0.28 0.051 Uiso 1 1 calc R A 1 C14 C 0.1248(4) 0.4779(2) 0.33799(15) 0.0282(11) Uani 1 1 d . A 1 C15 C 0.1486(4) 0.5412(2) 0.34606(17) 0.0376(12) Uani 1 1 d . A 1 H15 H 0.213 0.5532 0.3661 0.045 Uiso 1 1 calc R A 1 C16 C 0.0780(5) 0.5856(2) 0.32473(19) 0.0509(15) Uani 1 1 d . A 1 H16 H 0.0932 0.6283 0.331 0.061 Uiso 1 1 calc R A 1 C17 C -0.0139(5) 0.5690(3) 0.2946(2) 0.0622(17) Uani 1 1 d . A 1 H17 H -0.0616 0.6001 0.2799 0.075 Uiso 1 1 calc R A 1 C18 C -0.0368(4) 0.5074(3) 0.2857(2) 0.0585(16) Uani 1 1 d . A 1 H18 H -0.1002 0.4959 0.2647 0.07 Uiso 1 1 calc R A 1 C19 C 0.0321(4) 0.4619(2) 0.30735(17) 0.0408(13) Uani 1 1 d . A 1 H19 H 0.0157 0.4194 0.3011 0.049 Uiso 1 1 calc R A 1 C20 C 0.2360(3) 0.4375(2) 0.42708(14) 0.0268(10) Uani 1 1 d . A 1 C21 C 0.1743(4) 0.4804(2) 0.44545(16) 0.0338(11) Uani 1 1 d . A 1 H21 H 0.1234 0.5053 0.4256 0.041 Uiso 1 1 calc R A 1 C22 C 0.1869(4) 0.4869(2) 0.49280(18) 0.0456(14) Uani 1 1 d . A 1 H22 H 0.1441 0.516 0.5052 0.055 Uiso 1 1 calc R A 1 C23 C 0.2604(5) 0.4518(3) 0.52140(18) 0.0534(15) Uani 1 1 d . A 1 H23 H 0.2686 0.4567 0.5537 0.064 Uiso 1 1 calc R A 1 C24 C 0.3237(4) 0.4089(3) 0.50387(18) 0.0525(15) Uani 1 1 d . A 1 H24 H 0.3748 0.3845 0.524 0.063 Uiso 1 1 calc R A 1 C25 C 0.3113(4) 0.4020(2) 0.45680(16) 0.0380(12) Uani 1 1 d . A 1 H25 H 0.3544 0.3729 0.4446 0.046 Uiso 1 1 calc R A 1 C26 C 0.3212(3) 0.20224(19) 0.34015(15) 0.0255(10) Uani 1 1 d . A 1 C27 C 0.3357(4) 0.1767(2) 0.38441(15) 0.0310(11) Uani 1 1 d . A 1 C28 C 0.3686(4) 0.1151(2) 0.39072(18) 0.0388(13) Uani 1 1 d . A 1 H28 H 0.3764 0.0974 0.4205 0.047 Uiso 1 1 calc R A 1 C29 C 0.3905(4) 0.0787(2) 0.35518(18) 0.0408(13) Uani 1 1 d . A 1 C30 C 0.3796(4) 0.1056(2) 0.31202(18) 0.0377(12) Uani 1 1 d . A 1 H30 H 0.3957 0.0815 0.2874 0.045 Uiso 1 1 calc R A 1 C31 C 0.3457(4) 0.1668(2) 0.30383(16) 0.0314(11) Uani 1 1 d . A 1 C32 C 0.3154(4) 0.2146(2) 0.42422(16) 0.0394(12) Uani 1 1 d . A 1 H32A H 0.2381 0.2208 0.4215 0.059 Uiso 1 1 calc R A 1 H32B H 0.3509 0.255 0.4242 0.059 Uiso 1 1 calc R A 1 H32C H 0.3441 0.1928 0.453 0.059 Uiso 1 1 calc R A 1 C33 C 0.4267(5) 0.0120(2) 0.3635(2) 0.0603(17) Uani 1 1 d . A 1 H33A H 0.4796 0.0093 0.3922 0.09 Uiso 1 1 calc R A 1 H33B H 0.4591 -0.0023 0.338 0.09 Uiso 1 1 calc R A 1 H33C H 0.3648 -0.0142 0.3656 0.09 Uiso 1 1 calc R A 1 C34 C 0.3318(4) 0.1931(2) 0.25635(16) 0.0398(12) Uani 1 1 d . A 1 H34A H 0.357 0.1629 0.2362 0.06 Uiso 1 1 calc R A 1 H34B H 0.3737 0.2315 0.2571 0.06 Uiso 1 1 calc R A 1 H34C H 0.2558 0.2022 0.2447 0.06 Uiso 1 1 calc R A 1 C35 C 0.3734(3) 0.47099(18) 0.33544(15) 0.0244(10) Uani 1 1 d . A 1 C36 C 0.4557(3) 0.49754(19) 0.36833(14) 0.0250(10) Uani 1 1 d . A 1 C37 C 0.4982(4) 0.5549(2) 0.35874(16) 0.0312(11) Uani 1 1 d . A 1 H37 H 0.5549 0.5725 0.3806 0.037 Uiso 1 1 calc R A 1 C38 C 0.4601(4) 0.5869(2) 0.31827(16) 0.0323(11) Uani 1 1 d . A 1 C39 C 0.3831(3) 0.5584(2) 0.28546(15) 0.0301(11) Uani 1 1 d . A 1 H39 H 0.3582 0.5791 0.2572 0.036 Uiso 1 1 calc R A 1 C40 C 0.3407(3) 0.50042(19) 0.29238(15) 0.0250(10) Uani 1 1 d . A 1 C41 C 0.5014(4) 0.4661(2) 0.41303(16) 0.0354(12) Uani 1 1 d . A 1 H41A H 0.579 0.4733 0.4208 0.053 Uiso 1 1 calc R A 1 H41B H 0.4873 0.4214 0.4102 0.053 Uiso 1 1 calc R A 1 H41C H 0.4676 0.4832 0.4373 0.053 Uiso 1 1 calc R A 1 C42 C 0.5028(4) 0.6511(2) 0.31034(18) 0.0433(13) Uani 1 1 d . A 1 H42A H 0.5244 0.6522 0.2805 0.065 Uiso 1 1 calc R A 1 H42B H 0.5649 0.6605 0.3346 0.065 Uiso 1 1 calc R A 1 H42C H 0.4466 0.6821 0.3109 0.065 Uiso 1 1 calc R A 1 C43 C 0.2653(4) 0.4697(2) 0.25364(15) 0.0317(11) Uani 1 1 d . A 1 H43A H 0.1934 0.4678 0.2609 0.048 Uiso 1 1 calc R A 1 H43B H 0.2906 0.4275 0.2493 0.048 Uiso 1 1 calc R A 1 H43C H 0.2627 0.4937 0.2254 0.048 Uiso 1 1 calc R A 1 C44 C 0.5816(4) 0.4176(2) 0.22749(15) 0.0301(11) Uani 1 1 d . A 1 C45 C 0.6354(4) 0.4237(2) 0.19114(17) 0.0410(13) Uani 1 1 d . A 1 H45 H 0.6303 0.3911 0.1692 0.049 Uiso 1 1 calc R A 1 C46 C 0.6959(4) 0.4756(2) 0.18606(19) 0.0456(14) Uani 1 1 d . A 1 H46 H 0.7313 0.4784 0.1608 0.055 Uiso 1 1 calc R A 1 C47 C 0.7052(4) 0.5235(2) 0.21744(18) 0.0398(13) Uani 1 1 d . A 1 H47 H 0.7463 0.5593 0.2138 0.048 Uiso 1 1 calc R A 1 C48 C 0.6540(4) 0.5186(2) 0.25415(18) 0.0381(12) Uani 1 1 d . A 1 H48 H 0.6605 0.551 0.2763 0.046 Uiso 1 1 calc R A 1 C49 C 0.5930(4) 0.4663(2) 0.25874(16) 0.0325(11) Uani 1 1 d . A 1 H49 H 0.5579 0.4638 0.2841 0.039 Uiso 1 1 calc R A 1 C50 C 0.5963(4) 0.2793(2) 0.23686(16) 0.0324(11) Uani 1 1 d . A 1 C51 C 0.6307(4) 0.2530(2) 0.19948(19) 0.0462(13) Uani 1 1 d . A 1 H51 H 0.5984 0.2654 0.1692 0.055 Uiso 1 1 calc R A 1 C52 C 0.7128(5) 0.2084(3) 0.2061(2) 0.0612(17) Uani 1 1 d . A 1 H52 H 0.7357 0.191 0.1802 0.073 Uiso 1 1 calc R A 1 C53 C 0.7601(5) 0.1897(3) 0.2490(3) 0.0608(17) Uani 1 1 d . A 1 H53 H 0.8164 0.16 0.2531 0.073 Uiso 1 1 calc R A 1 C54 C 0.7265(5) 0.2139(3) 0.2864(2) 0.0588(16) Uani 1 1 d . A 1 H54 H 0.7587 0.2007 0.3164 0.071 Uiso 1 1 calc R A 1 C55 C 0.6445(4) 0.2581(2) 0.28010(19) 0.0466(14) Uani 1 1 d . A 1 H55 H 0.6211 0.2742 0.3062 0.056 Uiso 1 1 calc R A 1 C56 C 0.4029(4) 0.3405(2) 0.17608(15) 0.0340(12) Uani 1 1 d . A 1 C57 C 0.3653(4) 0.3930(2) 0.15067(17) 0.0420(13) Uani 1 1 d . A 1 H57 H 0.3888 0.4328 0.1624 0.05 Uiso 1 1 calc R A 1 C58 C 0.2940(5) 0.3890(3) 0.10833(19) 0.0567(16) Uani 1 1 d . A 1 H58 H 0.2702 0.4256 0.0915 0.068 Uiso 1 1 calc R A 1 C59 C 0.2592(5) 0.3319(3) 0.0916(2) 0.0632(17) Uani 1 1 d . A 1 H59 H 0.2107 0.3288 0.063 0.076 Uiso 1 1 calc R A 1 C60 C 0.2932(5) 0.2790(3) 0.1157(2) 0.0626(17) Uani 1 1 d . A 1 H60 H 0.2682 0.2395 0.104 0.075 Uiso 1 1 calc R A 1 C61 C 0.3644(4) 0.2839(2) 0.15715(17) 0.0477(14) Uani 1 1 d . A 1 H61 H 0.3881 0.2469 0.1734 0.057 Uiso 1 1 calc R A 1 C62 C 0.6646(3) 0.2120(2) 0.42085(15) 0.0282(11) Uani 1 1 d . A 1 C63 C 0.7405(4) 0.1889(2) 0.45759(17) 0.0370(12) Uani 1 1 d . A 1 H63 H 0.7659 0.215 0.4832 0.044 Uiso 1 1 calc R A 1 C64 C 0.7797(4) 0.1283(2) 0.45765(19) 0.0452(14) Uani 1 1 d . A 1 H64 H 0.8318 0.1137 0.4828 0.054 Uiso 1 1 calc R A 1 C65 C 0.7424(5) 0.0899(2) 0.4209(2) 0.0513(15) Uani 1 1 d . A 1 H65 H 0.7689 0.0487 0.4206 0.062 Uiso 1 1 calc R A 1 C66 C 0.6673(4) 0.1111(2) 0.3849(2) 0.0474(14) Uani 1 1 d . A 1 H66 H 0.642 0.0844 0.3597 0.057 Uiso 1 1 calc R A 1 C67 C 0.6276(4) 0.1710(2) 0.38485(17) 0.0369(12) Uani 1 1 d . A 1 H67 H 0.574 0.1844 0.3598 0.044 Uiso 1 1 calc R A 1 C68 C 0.7308(3) 0.3467(2) 0.40898(15) 0.0300(11) Uani 1 1 d . A 1 C69 C 0.7147(4) 0.3882(2) 0.37242(18) 0.0464(14) Uani 1 1 d . A 1 H69 H 0.6472 0.389 0.3519 0.056 Uiso 1 1 calc R A 1 C70 C 0.7954(5) 0.4288(3) 0.3652(2) 0.0591(16) Uani 1 1 d . A 1 H70 H 0.7831 0.4566 0.3399 0.071 Uiso 1 1 calc R A 1 C71 C 0.8934(4) 0.4280(3) 0.3951(2) 0.0511(15) Uani 1 1 d . A 1 H71 H 0.9481 0.4563 0.391 0.061 Uiso 1 1 calc R A 1 C72 C 0.9112(4) 0.3867(2) 0.43045(19) 0.0451(13) Uani 1 1 d . A 1 H72 H 0.9793 0.3853 0.4505 0.054 Uiso 1 1 calc R A 1 C73 C 0.8312(4) 0.3468(2) 0.43735(18) 0.0406(13) Uani 1 1 d . A 1 H73 H 0.8452 0.3185 0.4623 0.049 Uiso 1 1 calc R A 1 C74 C 0.6021(4) 0.3117(2) 0.48010(15) 0.0302(11) Uani 1 1 d . A 1 C75 C 0.6351(4) 0.3672(2) 0.50332(16) 0.0398(12) Uani 1 1 d . A 1 H75 H 0.6665 0.3987 0.4879 0.048 Uiso 1 1 calc R A 1 C76 C 0.6234(4) 0.3774(3) 0.54806(18) 0.0494(15) Uani 1 1 d . A 1 H76 H 0.6459 0.4157 0.5627 0.059 Uiso 1 1 calc R A 1 C77 C 0.5792(5) 0.3323(3) 0.57144(19) 0.0527(15) Uani 1 1 d . A 1 H77 H 0.573 0.3389 0.6024 0.063 Uiso 1 1 calc R A 1 C78 C 0.5441(4) 0.2775(3) 0.54981(18) 0.0511(15) Uani 1 1 d . A 1 H78 H 0.5121 0.2466 0.5656 0.061 Uiso 1 1 calc R A 1 C79 C 0.5556(4) 0.2675(2) 0.50482(16) 0.0386(12) Uani 1 1 d . A 1 H79 H 0.5312 0.2294 0.4903 0.046 Uiso 1 1 calc R A 1 C80 C 0.0701(10) 0.0265(6) 0.4789(4) 0.141(4) Uiso 1 1 d . D 2 C81 C 0.0689(11) 0.0462(6) 0.5238(5) 0.176(5) Uiso 1 1 d . . 2 C82 C 0.0072(11) -0.0162(6) 0.4547(4) 0.152(4) Uiso 1 1 d . . 2 C83 C 0.151(2) 0.0515(13) 0.4516(9) 0.177(10) Uiso 0.5 1 d P D 2 C84 C 0.3838(14) 0.0299(8) 0.5195(6) 0.106(5) Uiso 0.5 1 d P . 2 C85 C 0.4591(8) 0.0889(4) 0.5282(3) 0.113(3) Uiso 1 1 d . . 2 C86 C 0.5519(11) 0.0755(6) 0.5082(4) 0.070(4) Uiso 0.5 1 d P . 2 C87 C 0.5793(6) 0.0223(4) 0.4932(3) 0.089(2) Uiso 1 1 d . . 2 C88 C 0.5065(12) -0.0321(7) 0.4867(5) 0.079(4) Uiso 0.5 1 d P . 2 C89 C 0.1791(12) 0.3118(7) 0.5764(4) 0.205(6) Uiso 1 1 d D E 2 C90 C 0.2423(16) 0.2639(11) 0.5617(7) 0.205(12) Uiso 0.5 1 d PD E 2 C91 C 0.188(2) 0.2162(11) 0.5349(8) 0.437(17) Uiso 1 1 d D E 2 C92 C 0.073(2) 0.2128(12) 0.5239(10) 0.267(17) Uiso 0.5 1 d PD E 2 C93 C 0.0164(13) 0.2542(7) 0.5494(6) 0.226(7) Uiso 1 1 d D E 2 C94 C 0.0668(10) 0.3125(6) 0.5596(5) 0.082(4) Uiso 0.5 1 d PD E 2 C95 C 0.0039(13) 0.3640(7) 0.5712(5) 0.199(6) Uiso 1 1 d D E 2 C96 C -0.0447(15) 0.3058(10) 0.5579(11) 0.237(14) Uiso 0.5 1 d PD E 2 C97 C 0.1154(16) 0.3627(10) 0.5884(10) 0.250(15) Uiso 0.5 1 d PD E 2 C98 C 0.1274(13) 0.2652(11) 0.5461(13) 0.74(10) Uiso 0.5 1 d PD E 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.0195(3) 0.0214(3) 0.0260(3) 0.0001(2) 0.0045(2) -0.0003(2) P1 0.0237(7) 0.0235(6) 0.0296(7) -0.0022(5) 0.0068(5) -0.0045(5) P2 0.0214(6) 0.0216(6) 0.0303(6) -0.0013(5) 0.0058(5) 0.0001(5) Si1 0.0284(7) 0.0266(7) 0.0281(7) 0.0003(6) 0.0084(6) -0.0001(5) Si2 0.0241(7) 0.0273(7) 0.0281(7) 0.0010(6) 0.0027(5) -0.0002(5) O1 0.0333(18) 0.0298(17) 0.0316(17) 0.0032(14) 0.0131(15) 0.0011(14) O2 0.0263(18) 0.0300(17) 0.0362(18) 0.0036(14) -0.0021(14) -0.0001(14) N1 0.020(2) 0.0205(19) 0.031(2) -0.0002(16) 0.0043(16) -0.0023(15) N2 0.025(2) 0.0194(19) 0.030(2) 0.0013(16) 0.0073(17) -0.0037(15) C1 0.022(3) 0.026(3) 0.034(3) 0.000(2) 0.011(2) 0.002(2) C2 0.022(2) 0.029(3) 0.032(3) -0.001(2) 0.009(2) -0.004(2) C3 0.039(3) 0.035(3) 0.050(3) -0.009(2) 0.017(3) -0.011(2) C4 0.046(3) 0.057(4) 0.053(3) -0.009(3) 0.029(3) -0.019(3) C5 0.041(3) 0.038(3) 0.057(3) 0.005(3) 0.014(3) -0.016(2) C6 0.038(3) 0.032(3) 0.054(3) -0.003(2) 0.008(3) -0.012(2) C7 0.030(3) 0.034(3) 0.041(3) -0.003(2) 0.011(2) -0.004(2) C8 0.026(3) 0.021(2) 0.036(3) -0.002(2) 0.000(2) -0.0051(19) C9 0.032(3) 0.027(3) 0.036(3) 0.001(2) 0.005(2) -0.001(2) C10 0.051(4) 0.046(3) 0.040(3) 0.009(3) 0.004(3) -0.007(3) C11 0.061(4) 0.055(4) 0.042(3) 0.011(3) -0.009(3) -0.007(3) C12 0.034(3) 0.056(4) 0.065(4) 0.004(3) -0.013(3) -0.002(3) C13 0.031(3) 0.044(3) 0.050(3) 0.004(3) 0.000(3) -0.003(2) C14 0.027(3) 0.028(3) 0.033(3) 0.002(2) 0.012(2) 0.005(2) C15 0.037(3) 0.035(3) 0.044(3) 0.004(2) 0.015(2) 0.003(2) C16 0.066(4) 0.035(3) 0.059(4) 0.017(3) 0.030(3) 0.018(3) C17 0.052(4) 0.069(5) 0.071(4) 0.029(4) 0.026(3) 0.031(3) C18 0.033(3) 0.073(4) 0.068(4) 0.012(3) 0.004(3) 0.018(3) C19 0.028(3) 0.048(3) 0.046(3) 0.002(3) 0.006(2) 0.007(2) C20 0.024(2) 0.029(2) 0.028(2) -0.004(2) 0.005(2) -0.003(2) C21 0.035(3) 0.032(3) 0.035(3) -0.005(2) 0.011(2) -0.005(2) C22 0.051(4) 0.047(3) 0.043(3) -0.015(3) 0.019(3) -0.007(3) C23 0.054(4) 0.075(4) 0.031(3) -0.008(3) 0.007(3) -0.022(3) C24 0.043(3) 0.073(4) 0.039(3) 0.004(3) 0.001(3) -0.002(3) C25 0.038(3) 0.044(3) 0.033(3) 0.000(2) 0.009(2) 0.002(2) C26 0.019(2) 0.021(2) 0.036(3) 0.000(2) 0.003(2) -0.0032(19) C27 0.026(3) 0.035(3) 0.031(3) 0.002(2) 0.004(2) -0.009(2) C28 0.037(3) 0.033(3) 0.043(3) 0.012(3) 0.000(2) -0.008(2) C29 0.042(3) 0.020(3) 0.055(3) 0.002(3) -0.003(3) -0.001(2) C30 0.036(3) 0.025(3) 0.051(3) -0.006(2) 0.005(2) -0.001(2) C31 0.028(3) 0.026(3) 0.038(3) -0.003(2) 0.003(2) -0.005(2) C32 0.042(3) 0.042(3) 0.033(3) 0.008(2) 0.004(2) -0.001(2) C33 0.065(4) 0.028(3) 0.080(4) 0.006(3) -0.005(3) 0.003(3) C34 0.054(3) 0.030(3) 0.038(3) -0.002(2) 0.016(3) 0.001(2) C35 0.024(3) 0.019(2) 0.033(3) -0.003(2) 0.012(2) 0.0037(19) C36 0.023(2) 0.025(2) 0.028(2) -0.004(2) 0.007(2) 0.001(2) C37 0.024(3) 0.029(3) 0.040(3) -0.004(2) 0.006(2) -0.005(2) C38 0.034(3) 0.027(3) 0.040(3) 0.001(2) 0.017(2) -0.002(2) C39 0.029(3) 0.030(3) 0.031(3) 0.003(2) 0.007(2) 0.001(2) C40 0.023(2) 0.024(2) 0.030(3) -0.001(2) 0.009(2) 0.0032(19) C41 0.029(3) 0.035(3) 0.039(3) -0.002(2) -0.001(2) -0.002(2) C42 0.052(3) 0.033(3) 0.048(3) 0.002(2) 0.016(3) -0.013(2) C43 0.035(3) 0.027(2) 0.032(3) 0.001(2) 0.005(2) 0.000(2) C44 0.027(3) 0.027(3) 0.036(3) 0.005(2) 0.006(2) 0.004(2) C45 0.044(3) 0.039(3) 0.044(3) 0.001(2) 0.017(3) -0.007(2) C46 0.035(3) 0.052(3) 0.054(3) 0.011(3) 0.019(3) -0.003(3) C47 0.023(3) 0.033(3) 0.062(4) 0.013(3) 0.006(3) -0.003(2) C48 0.032(3) 0.031(3) 0.049(3) 0.000(2) 0.002(3) 0.000(2) C49 0.026(3) 0.033(3) 0.038(3) 0.004(2) 0.006(2) 0.003(2) C50 0.031(3) 0.028(3) 0.043(3) 0.004(2) 0.017(2) -0.003(2) C51 0.047(3) 0.046(3) 0.050(3) -0.007(3) 0.020(3) 0.002(3) C52 0.059(4) 0.046(4) 0.091(5) -0.013(4) 0.043(4) 0.009(3) C53 0.048(4) 0.035(3) 0.107(5) 0.017(4) 0.035(4) 0.014(3) C54 0.049(4) 0.055(4) 0.076(4) 0.019(3) 0.022(3) 0.016(3) C55 0.043(3) 0.043(3) 0.057(4) 0.008(3) 0.018(3) 0.012(3) C56 0.030(3) 0.042(3) 0.031(3) 0.001(2) 0.009(2) -0.003(2) C57 0.042(3) 0.044(3) 0.040(3) 0.003(3) 0.007(3) 0.003(2) C58 0.050(4) 0.076(4) 0.042(3) 0.016(3) 0.005(3) 0.007(3) C59 0.048(4) 0.101(5) 0.037(3) -0.007(4) 0.000(3) -0.012(4) C60 0.071(4) 0.065(4) 0.045(4) -0.013(3) -0.005(3) -0.015(3) C61 0.053(4) 0.046(3) 0.040(3) -0.001(3) 0.000(3) -0.008(3) C62 0.023(3) 0.030(3) 0.033(3) 0.003(2) 0.010(2) -0.001(2) C63 0.031(3) 0.045(3) 0.038(3) 0.009(2) 0.012(2) 0.004(2) C64 0.038(3) 0.047(3) 0.056(4) 0.019(3) 0.021(3) 0.016(3) C65 0.052(4) 0.031(3) 0.083(4) 0.016(3) 0.042(3) 0.012(3) C66 0.051(4) 0.030(3) 0.068(4) -0.006(3) 0.030(3) -0.004(3) C67 0.030(3) 0.038(3) 0.045(3) 0.001(3) 0.012(2) 0.000(2) C68 0.024(3) 0.034(3) 0.033(3) -0.001(2) 0.006(2) -0.002(2) C69 0.032(3) 0.053(3) 0.052(3) 0.014(3) 0.004(3) -0.002(3) C70 0.050(4) 0.068(4) 0.060(4) 0.025(3) 0.011(3) -0.017(3) C71 0.039(3) 0.057(4) 0.063(4) -0.004(3) 0.022(3) -0.015(3) C72 0.026(3) 0.059(4) 0.051(3) -0.007(3) 0.008(2) -0.008(3) C73 0.030(3) 0.044(3) 0.047(3) 0.004(3) 0.007(2) -0.004(2) C74 0.026(3) 0.035(3) 0.029(3) 0.001(2) 0.004(2) 0.003(2) C75 0.038(3) 0.041(3) 0.037(3) -0.002(3) 0.000(2) 0.005(2) C76 0.055(4) 0.051(3) 0.038(3) -0.015(3) -0.001(3) 0.014(3) C77 0.060(4) 0.063(4) 0.036(3) 0.000(3) 0.011(3) 0.024(3) C78 0.057(4) 0.058(4) 0.043(3) 0.011(3) 0.021(3) 0.012(3) C79 0.038(3) 0.043(3) 0.035(3) -0.002(2) 0.008(2) 0.002(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Zn O2 1.887(3) . ? Zn O1 1.894(3) . ? Zn N1 2.067(3) . ? Zn N2 2.081(3) . ? P1 N1 1.590(4) . ? P1 C2 1.804(4) . ? P1 C8 1.806(4) . ? P1 C1 1.816(5) . ? P2 N2 1.594(4) . ? P2 C14 1.803(4) . ? P2 C1 1.814(4) . ? P2 C20 1.822(4) . ? Si1 O1 1.584(3) . ? Si1 C50 1.884(5) . ? Si1 C44 1.887(5) . ? Si1 C56 1.891(5) . ? Si2 O2 1.581(3) . ? Si2 C74 1.884(5) . ? Si2 C62 1.891(4) . ? Si2 C68 1.893(5) . ? N1 C26 1.442(5) . ? N2 C35 1.456(5) . ? C2 C3 1.387(6) . ? C2 C7 1.390(6) . ? C3 C4 1.392(7) . ? C4 C5 1.376(7) . ? C5 C6 1.384(7) . ? C6 C7 1.378(6) . ? C8 C13 1.394(6) . ? C8 C9 1.397(6) . ? C9 C10 1.377(6) . ? C10 C11 1.372(8) . ? C11 C12 1.378(8) . ? C12 C13 1.388(7) . ? C14 C19 1.384(6) . ? C14 C15 1.405(6) . ? C15 C16 1.378(7) . ? C16 C17 1.373(8) . ? C17 C18 1.372(8) . ? C18 C19 1.386(7) . ? C20 C21 1.391(6) . ? C20 C25 1.395(6) . ? C21 C22 1.391(7) . ? C22 C23 1.362(7) . ? C23 C24 1.392(8) . ? C24 C25 1.384(7) . ? C26 C27 1.404(6) . ? C26 C31 1.405(6) . ? C27 C28 1.391(6) . ? C27 C32 1.501(6) . ? C28 C29 1.387(7) . ? C29 C30 1.389(7) . ? C29 C33 1.513(7) . ? C30 C31 1.394(6) . ? C31 C34 1.498(6) . ? C35 C36 1.406(6) . ? C35 C40 1.415(6) . ? C36 C37 1.400(6) . ? C36 C41 1.502(6) . ? C37 C38 1.388(6) . ? C38 C39 1.383(6) . ? C38 C42 1.520(6) . ? C39 C40 1.390(6) . ? C40 C43 1.499(6) . ? C44 C49 1.390(6) . ? C44 C45 1.393(6) . ? C45 C46 1.383(7) . ? C46 C47 1.379(7) . ? C47 C48 1.379(7) . ? C48 C49 1.388(6) . ? C50 C55 1.387(7) . ? C50 C51 1.391(7) . ? C51 C52 1.404(7) . ? C52 C53 1.361(8) . ? C53 C54 1.368(8) . ? C54 C55 1.397(7) . ? C56 C61 1.390(7) . ? C56 C57 1.391(7) . ? C57 C58 1.402(7) . ? C58 C59 1.368(8) . ? C59 C60 1.368(8) . ? C60 C61 1.382(7) . ? C62 C67 1.396(6) . ? C62 C63 1.399(6) . ? C63 C64 1.396(7) . ? C64 C65 1.377(8) . ? C65 C66 1.364(8) . ? C66 C67 1.385(7) . ? C68 C73 1.385(6) . ? C68 C69 1.391(7) . ? C69 C70 1.396(7) . ? C70 C71 1.380(7) . ? C71 C72 1.362(7) . ? C72 C73 1.377(7) . ? C74 C79 1.401(6) . ? C74 C75 1.402(7) . ? C75 C76 1.384(7) . ? C76 C77 1.377(8) . ? C77 C78 1.374(8) . ? C78 C79 1.390(7) . ? C80 C82 1.332(13) . ? C80 C81 1.403(15) . ? C80 C83 1.53(3) . ? C81 C82 1.415(15) 3_556 ? C82 C81 1.415(15) 3_556 ? C84 C87 1.302(18) 3_656 ? C84 C88 1.44(2) 3_656 ? C84 C85 1.581(19) . ? C85 C88 1.400(15) 3_656 ? C85 C86 1.451(15) . ? C86 C88 1.221(18) 3_656 ? C86 C87 1.300(14) . ? C87 C84 1.302(18) 3_656 ? C87 C88 1.358(16) 3_656 ? C87 C88 1.482(16) . ? C88 C86 1.221(18) 3_656 ? C88 C87 1.358(16) 3_656 ? C88 C85 1.400(15) 3_656 ? C88 C84 1.44(2) 3_656 ? C88 C88 1.62(3) 3_656 ? C89 C94 1.417(13) . ? C89 C98 1.423(15) . ? C89 C90 1.429(15) . ? C89 C97 1.447(15) . ? C90 C91 1.394(16) . ? C90 C98 1.444(16) . ? C91 C98 1.387(16) . ? C91 C92 1.447(16) . ? C92 C98 1.416(16) . ? C92 C93 1.446(16) . ? C93 C96 1.405(15) . ? C93 C94 1.414(13) . ? C93 C98 1.453(16) . ? C94 C98 1.384(14) . ? C94 C96 1.416(15) . ? C94 C97 1.440(15) . ? C94 C95 1.448(12) . ? C95 C97 1.410(15) . ? C95 C96 1.420(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 O2 Zn O1 117.68(13) . . ? O2 Zn N1 103.60(13) . . ? O1 Zn N1 115.71(13) . . ? O2 Zn N2 114.60(13) . . ? O1 Zn N2 102.42(13) . . ? N1 Zn N2 102.13(13) . . ? N1 P1 C2 113.89(19) . . ? N1 P1 C8 115.5(2) . . ? C2 P1 C8 104.8(2) . . ? N1 P1 C1 109.8(2) . . ? C2 P1 C1 104.8(2) . . ? C8 P1 C1 107.3(2) . . ? N2 P2 C14 113.96(19) . . ? N2 P2 C1 111.0(2) . . ? C14 P2 C1 108.6(2) . . ? N2 P2 C20 117.48(19) . . ? C14 P2 C20 105.3(2) . . ? C1 P2 C20 99.3(2) . . ? O1 Si1 C50 112.04(18) . . ? O1 Si1 C44 112.97(19) . . ? C50 Si1 C44 105.1(2) . . ? O1 Si1 C56 113.95(19) . . ? C50 Si1 C56 107.8(2) . . ? C44 Si1 C56 104.3(2) . . ? O2 Si2 C74 113.92(19) . . ? O2 Si2 C62 113.02(18) . . ? C74 Si2 C62 104.3(2) . . ? O2 Si2 C68 111.47(18) . . ? C74 Si2 C68 105.7(2) . . ? C62 Si2 C68 107.8(2) . . ? Si1 O1 Zn 163.03(19) . . ? Si2 O2 Zn 168.5(2) . . ? C26 N1 P1 121.4(3) . . ? C26 N1 Zn 116.4(3) . . ? P1 N1 Zn 121.92(18) . . ? C35 N2 P2 115.4(3) . . ? C35 N2 Zn 116.0(2) . . ? P2 N2 Zn 128.39(19) . . ? P2 C1 P1 123.7(3) . . ? C3 C2 C7 119.0(4) . . ? C3 C2 P1 123.6(3) . . ? C7 C2 P1 117.4(3) . . ? C2 C3 C4 120.1(5) . . ? C5 C4 C3 120.0(5) . . ? C4 C5 C6 120.4(5) . . ? C7 C6 C5 119.5(5) . . ? C6 C7 C2 120.9(5) . . ? C13 C8 C9 119.4(4) . . ? C13 C8 P1 119.8(4) . . ? C9 C8 P1 120.8(3) . . ? C10 C9 C8 120.2(5) . . ? C11 C10 C9 120.3(5) . . ? C10 C11 C12 120.2(5) . . ? C11 C12 C13 120.6(5) . . ? C12 C13 C8 119.3(5) . . ? C19 C14 C15 118.7(4) . . ? C19 C14 P2 121.8(3) . . ? C15 C14 P2 119.4(4) . . ? C16 C15 C14 119.7(5) . . ? C17 C16 C15 120.9(5) . . ? C18 C17 C16 119.8(5) . . ? C17 C18 C19 120.2(6) . . ? C14 C19 C18 120.6(5) . . ? C21 C20 C25 119.0(4) . . ? C21 C20 P2 123.7(3) . . ? C25 C20 P2 117.1(3) . . ? C20 C21 C22 120.1(5) . . ? C23 C22 C21 120.3(5) . . ? C22 C23 C24 120.7(5) . . ? C25 C24 C23 119.3(5) . . ? C24 C25 C20 120.6(5) . . ? C27 C26 C31 119.9(4) . . ? C27 C26 N1 120.9(4) . . ? C31 C26 N1 119.2(4) . . ? C28 C27 C26 118.7(4) . . ? C28 C27 C32 120.4(4) . . ? C26 C27 C32 120.9(4) . . ? C29 C28 C27 122.4(4) . . ? C28 C29 C30 117.9(4) . . ? C28 C29 C33 120.8(5) . . ? C30 C29 C33 121.2(5) . . ? C29 C30 C31 121.8(5) . . ? C30 C31 C26 119.1(4) . . ? C30 C31 C34 119.8(4) . . ? C26 C31 C34 121.0(4) . . ? C36 C35 C40 119.5(4) . . ? C36 C35 N2 121.0(4) . . ? C40 C35 N2 119.5(4) . . ? C37 C36 C35 118.8(4) . . ? C37 C36 C41 118.7(4) . . ? C35 C36 C41 122.5(4) . . ? C38 C37 C36 122.1(4) . . ? C39 C38 C37 117.9(4) . . ? C39 C38 C42 121.4(4) . . ? C37 C38 C42 120.7(4) . . ? C38 C39 C40 122.4(4) . . ? C39 C40 C35 118.8(4) . . ? C39 C40 C43 119.4(4) . . ? C35 C40 C43 121.8(4) . . ? C49 C44 C45 116.4(4) . . ? C49 C44 Si1 123.0(4) . . ? C45 C44 Si1 120.6(3) . . ? C46 C45 C44 121.9(5) . . ? C47 C46 C45 120.4(5) . . ? C46 C47 C48 119.1(4) . . ? C47 C48 C49 119.9(5) . . ? C48 C49 C44 122.3(5) . . ? C55 C50 C51 117.0(4) . . ? C55 C50 Si1 118.1(4) . . ? C51 C50 Si1 124.6(4) . . ? C50 C51 C52 120.6(5) . . ? C53 C52 C51 120.8(5) . . ? C52 C53 C54 119.9(5) . . ? C53 C54 C55 119.6(6) . . ? C50 C55 C54 122.0(5) . . ? C61 C56 C57 115.9(4) . . ? C61 C56 Si1 122.3(4) . . ? C57 C56 Si1 121.8(4) . . ? C56 C57 C58 122.1(5) . . ? C59 C58 C57 119.1(6) . . ? C60 C59 C58 120.8(5) . . ? C59 C60 C61 119.1(6) . . ? C60 C61 C56 123.0(5) . . ? C67 C62 C63 116.7(4) . . ? C67 C62 Si2 121.6(3) . . ? C63 C62 Si2 121.6(4) . . ? C64 C63 C62 121.7(5) . . ? C65 C64 C63 119.4(5) . . ? C66 C65 C64 120.1(5) . . ? C65 C66 C67 120.7(5) . . ? C66 C67 C62 121.3(5) . . ? C73 C68 C69 116.8(4) . . ? C73 C68 Si2 123.0(4) . . ? C69 C68 Si2 120.2(3) . . ? C68 C69 C70 121.5(5) . . ? C71 C70 C69 119.5(5) . . ? C72 C71 C70 119.7(5) . . ? C71 C72 C73 120.4(5) . . ? C72 C73 C68 122.0(5) . . ? C79 C74 C75 115.9(4) . . ? C79 C74 Si2 120.4(4) . . ? C75 C74 Si2 123.6(4) . . ? C76 C75 C74 122.0(5) . . ? C77 C76 C75 120.2(5) . . ? C78 C77 C76 119.8(5) . . ? C77 C78 C79 119.8(5) . . ? C78 C79 C74 122.2(5) . . ? C82 C80 C81 127.2(12) . . ? C82 C80 C83 110.6(15) . . ? C81 C80 C83 122.1(16) . . ? C80 C81 C82 115.2(12) . 3_556 ? C80 C82 C81 117.6(12) . 3_556 ? C87 C84 C88 65.2(10) 3_656 3_656 ? C87 C84 C85 120.1(14) 3_656 . ? C88 C84 C85 55.0(9) 3_656 . ? C88 C85 C86 50.7(8) 3_656 . ? C88 C85 C84 57.5(9) 3_656 . ? C86 C85 C84 106.7(10) . . ? C88 C86 C87 65.1(10) 3_656 . ? C88 C86 C85 62.5(10) 3_656 . ? C87 C86 C85 127.6(12) . . ? C86 C87 C84 174.4(13) . 3_656 ? C86 C87 C88 54.7(8) . 3_656 ? C84 C87 C88 128.8(12) 3_656 3_656 ? C86 C87 C88 122.6(11) . . ? C84 C87 C88 62.0(10) 3_656 . ? C88 C87 C88 69.2(11) 3_656 . ? C86 C88 C87 60.2(10) 3_656 3_656 ? C86 C88 C85 66.8(10) 3_656 3_656 ? C87 C88 C85 127.0(13) 3_656 3_656 ? C86 C88 C84 131.9(15) 3_656 3_656 ? C87 C88 C84 158.5(14) 3_656 3_656 ? C85 C88 C84 67.6(11) 3_656 3_656 ? C86 C88 C87 165.4(14) 3_656 . ? C87 C88 C87 110.8(11) 3_656 . ? C85 C88 C87 120.4(12) 3_656 . ? C84 C88 C87 52.8(9) 3_656 . ? C86 C88 C88 118.1(17) 3_656 3_656 ? C87 C88 C88 59.0(10) 3_656 3_656 ? C85 C88 C88 165.9(17) 3_656 3_656 ? C84 C88 C88 103.2(15) 3_656 3_656 ? C87 C88 C88 51.8(9) . 3_656 ? C94 C89 C98 58.3(7) . . ? C94 C89 C90 119.2(10) . . ? C98 C89 C90 60.8(7) . . ? C94 C89 C97 60.4(7) . . ? C98 C89 C97 118.7(10) . . ? C90 C89 C97 176.0(15) . . ? C91 C90 C89 117.7(11) . . ? C91 C90 C98 58.5(8) . . ? C89 C90 C98 59.4(8) . . ? C98 C91 C90 62.6(8) . . ? C98 C91 C92 59.9(8) . . ? C90 C91 C92 122.0(12) . . ? C98 C92 C93 61.0(8) . . ? C98 C92 C91 57.9(8) . . ? C93 C92 C91 115.9(13) . . ? C96 C93 C94 60.3(7) . . ? C96 C93 C92 158(3) . . ? C94 C93 C92 114.1(12) . . ? C96 C93 C98 117.6(11) . . ? C94 C93 C98 57.7(7) . . ? C92 C93 C98 58.5(7) . . ? C98 C94 C93 62.6(8) . . ? C98 C94 C96 121.7(10) . . ? C93 C94 C96 59.5(7) . . ? C98 C94 C89 61.0(7) . . ? C93 C94 C89 116.7(11) . . ? C96 C94 C89 160.7(19) . . ? C98 C94 C97 121.8(10) . . ? C93 C94 C97 156.4(19) . . ? C96 C94 C97 114.1(12) . . ? C89 C94 C97 60.8(7) . . ? C98 C94 C95 176(2) . . ? C93 C94 C95 118.8(9) . . ? C96 C94 C95 59.4(7) . . ? C89 C94 C95 119.2(9) . . ? C97 C94 C95 58.4(7) . . ? C97 C95 C96 115.8(13) . . ? C97 C95 C94 60.5(7) . . ? C96 C95 C94 59.1(7) . . ? C93 C96 C94 60.2(7) . . ? C93 C96 C95 121.5(12) . . ? C94 C96 C95 61.4(8) . . ? C95 C97 C94 61.1(8) . . ? C95 C97 C89 119.9(11) . . ? C94 C97 C89 58.8(7) . . ? C94 C98 C91 177(4) . . ? C94 C98 C92 118.0(10) . . ? C91 C98 C92 62.1(8) . . ? C94 C98 C89 60.6(7) . . ? C91 C98 C89 118.5(12) . . ? C92 C98 C89 169(4) . . ? C94 C98 C90 120.4(11) . . ? C91 C98 C90 59.0(7) . . ? C92 C98 C90 120.6(12) . . ? C89 C98 C90 59.8(7) . . ? C94 C98 C93 59.7(7) . . ? C91 C98 C93 119.3(14) . . ? C92 C98 C93 60.5(8) . . ? C89 C98 C93 113.8(15) . . ? C90 C98 C93 155(3) . . ? #===END