# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Michael F. Lappert' 'Peter B. Hitchcock' 'Jacek E. Nyez' _publ_contact_author_name 'Prof Michael F. Lappert' _publ_contact_author_address ; CPES University of Sussex The Chemistry Laboratory, Universit Brighton East Sussex BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email M.F.LAPPERT@SUSSEX.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; Synthesis, structure and reductive dechlorination of the C-centred phosphorus(III) b-diketiminate PCl(Ph)L [L = C{C(Me)NC6H3Pri2-2,6}{C(Me)NHC6H3Pri2-2,6}] ; data_aug1902 _database_code_CSD 203507 _audit_creation_date 2002-08-14T14:57:47-00:00 _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 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C35 H46 Cl1 N2 P1' _chemical_formula_sum 'C35 H46 Cl N2 P' _chemical_formula_weight 561.16 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 14.5108(8) _cell_length_b 25.9696(13) _cell_length_c 8.4582(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3187.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 48546 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 21.967 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.169 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.196 _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 0.0989 _diffrn_reflns_av_unetI/netI 0.0937 _diffrn_reflns_number 7539 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.78 _diffrn_reflns_theta_max 21.97 _diffrn_reflns_theta_full 21.97 _diffrn_measured_fraction_theta_full 0.98 _diffrn_measured_fraction_theta_max 0.98 _reflns_number_total 3317 _reflns_number_gt 2746 _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 crystal diffracted only weakly with nothing above theta=22 degrees. 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^)+(0.0559P)^2^+0.8149P] 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; but H on N1 refined isotropic' _refine_ls_extinction_method none _refine_ls_number_reflns 3317 _refine_ls_number_parameters 358 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.056 _refine_ls_wR_factor_ref 0.1362 _refine_ls_wR_factor_gt 0.1265 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.005 _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 0.05(13) _refine_diff_density_max 0.426 _refine_diff_density_min -0.24 _refine_diff_density_rms 0.05 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cl Cl 0.87753(10) 0.68387(6) 0.0216(2) 0.0540(5) Uani 1 1 d . . . P P 0.84675(10) 0.69437(5) 0.2655(2) 0.0418(4) Uani 1 1 d . . . N1 N 0.6138(3) 0.6465(2) 0.4507(6) 0.0348(12) Uani 1 1 d . . . H1X H 0.625(3) 0.617(2) 0.465(5) 0.021(15) Uiso 1 1 d . . . N2 N 0.7177(3) 0.56462(16) 0.4109(5) 0.0345(11) Uani 1 1 d . . . C1 C 0.6773(4) 0.67262(19) 0.3706(6) 0.0319(13) Uani 1 1 d . . . C2 C 0.7590(3) 0.64999(19) 0.3174(7) 0.0338(13) Uani 1 1 d . . . C3 C 0.7723(3) 0.59325(19) 0.3261(6) 0.0315(13) Uani 1 1 d . . . C4 C 0.6533(4) 0.7287(2) 0.3427(8) 0.0470(16) Uani 1 1 d . . . H4A H 0.5903 0.7312 0.3017 0.071 Uiso 1 1 calc R . . H4B H 0.6963 0.7435 0.2659 0.071 Uiso 1 1 calc R . . H4C H 0.6577 0.7476 0.4427 0.071 Uiso 1 1 calc R . . C5 C 0.8470(4) 0.5701(2) 0.2248(7) 0.0412(15) Uani 1 1 d . . . H5A H 0.903 0.5656 0.288 0.062 Uiso 1 1 calc R . . H5B H 0.8599 0.593 0.1355 0.062 Uiso 1 1 calc R . . H5C H 0.8265 0.5365 0.185 0.062 Uiso 1 1 calc R . . C6 C 0.5300(3) 0.66706(17) 0.5146(7) 0.0315(13) Uani 1 1 d . . . C7 C 0.4473(4) 0.66069(18) 0.4301(7) 0.0359(14) Uani 1 1 d . . . C8 C 0.3669(3) 0.6811(2) 0.4983(8) 0.0415(15) Uani 1 1 d . . . H8 H 0.3097 0.6776 0.4446 0.05 Uiso 1 1 calc R . . C9 C 0.3696(4) 0.7061(2) 0.6406(8) 0.0428(14) Uani 1 1 d . . . H9 H 0.3143 0.7195 0.6842 0.051 Uiso 1 1 calc R . . C10 C 0.4506(4) 0.7121(2) 0.7216(7) 0.0398(15) Uani 1 1 d . . . H10 H 0.4506 0.7299 0.8197 0.048 Uiso 1 1 calc R . . C11 C 0.5337(4) 0.69236(19) 0.6617(7) 0.0344(14) Uani 1 1 d . . . C12 C 0.4440(4) 0.63453(19) 0.2693(7) 0.0410(14) Uani 1 1 d . . . H12 H 0.5076 0.6225 0.2431 0.049 Uiso 1 1 calc R . . C13 C 0.4134(5) 0.6714(2) 0.1404(8) 0.0590(18) Uani 1 1 d . . . H13C H 0.3515 0.6843 0.1646 0.088 Uiso 1 1 calc R . . H13B H 0.4123 0.6533 0.0387 0.088 Uiso 1 1 calc R . . H13A H 0.4566 0.7003 0.1345 0.088 Uiso 1 1 calc R . . C14 C 0.3803(4) 0.5874(2) 0.2716(8) 0.0546(17) Uani 1 1 d . . . H14C H 0.4026 0.5626 0.3501 0.082 Uiso 1 1 calc R . . H14B H 0.3799 0.5712 0.1669 0.082 Uiso 1 1 calc R . . H14A H 0.3176 0.5982 0.2993 0.082 Uiso 1 1 calc R . . C15 C 0.6226(4) 0.69664(19) 0.7539(7) 0.0393(13) Uani 1 1 d . . . H15 H 0.6746 0.6972 0.6763 0.047 Uiso 1 1 calc R . . C16 C 0.6294(4) 0.7455(2) 0.8546(9) 0.0568(18) Uani 1 1 d . . . H16C H 0.6242 0.7759 0.7863 0.085 Uiso 1 1 calc R . . H16B H 0.689 0.7462 0.9094 0.085 Uiso 1 1 calc R . . H16A H 0.5795 0.7458 0.9326 0.085 Uiso 1 1 calc R . . C17 C 0.6351(4) 0.6492(2) 0.8599(9) 0.064(2) Uani 1 1 d . . . H17C H 0.5842 0.6473 0.9357 0.096 Uiso 1 1 calc R . . H17B H 0.6936 0.6519 0.9171 0.096 Uiso 1 1 calc R . . H17A H 0.6355 0.618 0.7944 0.096 Uiso 1 1 calc R . . C18 C 0.7325(4) 0.50988(19) 0.4093(7) 0.0369(14) Uani 1 1 d . . . C19 C 0.6715(4) 0.4792(2) 0.3224(7) 0.0418(15) Uani 1 1 d . . . C20 C 0.6897(5) 0.4254(2) 0.3181(8) 0.0551(18) Uani 1 1 d . . . H20 H 0.6504 0.4034 0.2591 0.066 Uiso 1 1 calc R . . C21 C 0.7631(5) 0.4050(2) 0.3977(9) 0.063(2) Uani 1 1 d . . . H21 H 0.7756 0.3692 0.3896 0.075 Uiso 1 1 calc R . . C22 C 0.8194(5) 0.4357(2) 0.4898(9) 0.0575(18) Uani 1 1 d . . . H22 H 0.8685 0.4204 0.5474 0.069 Uiso 1 1 calc R . . C23 C 0.8053(4) 0.48915(19) 0.4996(7) 0.0420(15) Uani 1 1 d . . . C24 C 0.5910(4) 0.5023(2) 0.2366(7) 0.0465(16) Uani 1 1 d . . . H24 H 0.5634 0.5288 0.3081 0.056 Uiso 1 1 calc R . . C25 C 0.5144(4) 0.4631(2) 0.1974(8) 0.0590(19) Uani 1 1 d . . . H25C H 0.539 0.4364 0.1271 0.089 Uiso 1 1 calc R . . H25B H 0.4632 0.4808 0.1449 0.089 Uiso 1 1 calc R . . H25A H 0.4922 0.4471 0.2953 0.089 Uiso 1 1 calc R . . C26 C 0.6186(5) 0.5295(3) 0.0852(7) 0.067(2) Uani 1 1 d . . . H26C H 0.6629 0.5569 0.1096 0.1 Uiso 1 1 calc R . . H26B H 0.5638 0.5445 0.0355 0.1 Uiso 1 1 calc R . . H26A H 0.647 0.5047 0.0126 0.1 Uiso 1 1 calc R . . C27 C 0.8626(4) 0.5225(2) 0.6095(8) 0.0522(17) Uani 1 1 d . . . H27 H 0.8684 0.5572 0.5593 0.063 Uiso 1 1 calc R . . C28 C 0.8144(5) 0.5296(3) 0.7652(10) 0.083(2) Uani 1 1 d . . . H28C H 0.754 0.5455 0.7473 0.125 Uiso 1 1 calc R . . H28B H 0.8515 0.5519 0.8335 0.125 Uiso 1 1 calc R . . H28A H 0.8061 0.4961 0.8163 0.125 Uiso 1 1 calc R . . C29 C 0.9592(4) 0.5023(3) 0.6377(12) 0.083(2) Uani 1 1 d . . . H29C H 0.9937 0.5271 0.702 0.125 Uiso 1 1 calc R . . H29B H 0.9904 0.4976 0.536 0.125 Uiso 1 1 calc R . . H29A H 0.9559 0.4693 0.6933 0.125 Uiso 1 1 calc R . . C30 C 0.9496(4) 0.6659(2) 0.3548(8) 0.0430(15) Uani 1 1 d . . . C31 C 0.9475(4) 0.6591(2) 0.5186(9) 0.0524(16) Uani 1 1 d . . . H31 H 0.893 0.667 0.5757 0.063 Uiso 1 1 calc R . . C32 C 1.0239(5) 0.6410(3) 0.5983(10) 0.066(2) Uani 1 1 d . . . H32 H 1.0209 0.6358 0.7093 0.079 Uiso 1 1 calc R . . C33 C 1.1037(5) 0.6306(2) 0.5192(13) 0.071(2) Uani 1 1 d . . . H33 H 1.1559 0.6182 0.5753 0.085 Uiso 1 1 calc R . . C34 C 1.1087(5) 0.6379(2) 0.3598(11) 0.062(2) Uani 1 1 d . . . H34 H 1.1644 0.6308 0.3049 0.074 Uiso 1 1 calc R . . C35 C 1.0320(4) 0.6558(2) 0.2776(8) 0.0479(16) Uani 1 1 d . . . H35 H 1.0361 0.6611 0.1667 0.058 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 Cl 0.0569(9) 0.0485(9) 0.0564(10) 0.0097(8) 0.0091(9) -0.0076(8) P 0.0405(8) 0.0264(8) 0.0584(10) 0.0002(7) 0.0086(9) -0.0030(7) N1 0.033(3) 0.022(3) 0.050(3) 0.002(2) 0.003(2) 0.007(2) N2 0.041(2) 0.020(3) 0.042(3) 0.001(2) 0.001(2) 0.004(2) C1 0.034(3) 0.027(3) 0.035(3) 0.003(3) 0.000(3) -0.006(3) C2 0.036(3) 0.025(3) 0.040(3) -0.003(2) 0.004(3) 0.004(3) C3 0.033(3) 0.027(3) 0.034(3) -0.006(3) -0.001(3) 0.000(3) C4 0.045(3) 0.026(3) 0.070(4) 0.010(3) 0.010(3) 0.008(3) C5 0.048(3) 0.026(3) 0.050(4) -0.007(3) 0.012(3) 0.005(3) C6 0.031(3) 0.017(3) 0.046(4) 0.003(3) 0.007(3) 0.004(2) C7 0.037(3) 0.019(3) 0.051(4) 0.000(3) -0.002(3) -0.001(2) C8 0.028(3) 0.045(3) 0.052(4) 0.011(3) -0.002(3) 0.006(3) C9 0.048(4) 0.038(4) 0.042(4) 0.008(3) 0.011(3) 0.011(3) C10 0.048(4) 0.029(3) 0.043(4) 0.002(3) 0.006(3) 0.011(3) C11 0.046(4) 0.021(3) 0.036(4) 0.002(3) 0.002(3) 0.000(3) C12 0.038(3) 0.032(3) 0.053(4) -0.002(3) -0.006(3) 0.000(3) C13 0.088(5) 0.046(4) 0.042(4) 0.003(3) -0.002(4) -0.001(4) C14 0.059(4) 0.047(4) 0.058(4) 0.003(3) -0.011(4) -0.003(3) C15 0.045(3) 0.033(3) 0.040(3) 0.003(3) -0.001(3) -0.001(3) C16 0.063(4) 0.047(4) 0.061(5) -0.014(3) -0.005(3) -0.004(3) C17 0.063(4) 0.049(4) 0.081(5) 0.018(4) -0.022(4) -0.005(3) C18 0.052(3) 0.023(3) 0.035(4) 0.005(3) 0.010(3) 0.013(3) C19 0.065(4) 0.025(3) 0.035(4) -0.004(3) 0.012(3) -0.007(3) C20 0.081(5) 0.032(4) 0.052(5) -0.005(3) 0.024(4) -0.004(4) C21 0.093(5) 0.026(4) 0.069(5) 0.007(4) 0.025(4) 0.009(4) C22 0.063(4) 0.039(4) 0.070(5) 0.014(4) 0.015(4) 0.022(3) C23 0.053(3) 0.027(3) 0.046(4) 0.005(3) 0.011(3) 0.010(3) C24 0.060(4) 0.030(3) 0.050(4) -0.005(3) 0.002(4) -0.005(3) C25 0.062(4) 0.050(4) 0.066(5) -0.018(3) 0.012(4) -0.020(3) C26 0.089(5) 0.061(5) 0.051(5) 0.013(3) -0.015(4) -0.037(4) C27 0.050(4) 0.047(4) 0.060(5) 0.010(3) -0.003(3) 0.011(3) C28 0.081(5) 0.105(6) 0.065(5) -0.033(5) -0.003(5) 0.006(4) C29 0.063(4) 0.077(5) 0.110(7) 0.020(5) -0.011(5) 0.017(4) C30 0.043(4) 0.031(3) 0.055(4) -0.013(3) 0.004(3) -0.009(3) C31 0.049(4) 0.044(4) 0.064(5) -0.013(4) -0.008(4) -0.005(3) C32 0.067(5) 0.053(5) 0.078(6) -0.012(4) -0.019(5) -0.008(4) C33 0.058(5) 0.052(4) 0.104(7) -0.018(5) -0.034(5) 0.004(3) C34 0.039(4) 0.062(5) 0.085(6) -0.026(4) -0.007(4) -0.001(3) C35 0.041(4) 0.035(3) 0.067(5) -0.017(3) 0.000(4) -0.009(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 Cl P 2.129(2) . ? P C2 1.773(5) . ? P C30 1.828(6) . ? N1 C1 1.329(7) . ? N1 C6 1.434(6) . ? N2 C3 1.302(6) . ? N2 C18 1.438(7) . ? C1 C2 1.398(7) . ? C1 C4 1.515(7) . ? C2 C3 1.488(7) . ? C3 C5 1.507(7) . ? C6 C7 1.406(7) . ? C6 C11 1.408(8) . ? C7 C8 1.406(7) . ? C7 C12 1.521(8) . ? C8 C9 1.368(9) . ? C9 C10 1.369(8) . ? C10 C11 1.404(8) . ? C11 C15 1.513(8) . ? C12 C13 1.517(8) . ? C12 C14 1.535(7) . ? C15 C16 1.532(8) . ? C15 C17 1.535(8) . ? C18 C19 1.399(8) . ? C18 C23 1.411(8) . ? C19 C20 1.423(8) . ? C19 C24 1.499(8) . ? C20 C21 1.367(9) . ? C21 C22 1.382(9) . ? C22 C23 1.407(8) . ? C23 C27 1.518(8) . ? C24 C26 1.517(8) . ? C24 C25 1.544(8) . ? C27 C28 1.503(10) . ? C27 C29 1.514(8) . ? C30 C35 1.387(8) . ? C30 C31 1.397(10) . ? C31 C32 1.379(9) . ? C32 C33 1.364(10) . ? C33 C34 1.363(11) . ? C34 C35 1.392(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 P C30 102.8(2) . . ? C2 P Cl 107.90(19) . . ? C30 P Cl 100.2(2) . . ? C1 N1 C6 126.1(5) . . ? C3 N2 C18 118.0(4) . . ? N1 C1 C2 122.5(5) . . ? N1 C1 C4 114.2(5) . . ? C2 C1 C4 123.3(5) . . ? C1 C2 C3 120.7(5) . . ? C1 C2 P 114.6(4) . . ? C3 C2 P 124.3(4) . . ? N2 C3 C2 120.9(4) . . ? N2 C3 C5 121.5(4) . . ? C2 C3 C5 117.4(5) . . ? C7 C6 C11 122.4(5) . . ? C7 C6 N1 119.2(5) . . ? C11 C6 N1 118.3(5) . . ? C8 C7 C6 117.1(5) . . ? C8 C7 C12 120.6(5) . . ? C6 C7 C12 122.3(5) . . ? C9 C8 C7 121.0(6) . . ? C10 C9 C8 121.3(6) . . ? C9 C10 C11 121.0(5) . . ? C10 C11 C6 117.2(5) . . ? C10 C11 C15 121.3(5) . . ? C6 C11 C15 121.5(5) . . ? C13 C12 C7 111.7(4) . . ? C13 C12 C14 109.7(5) . . ? C7 C12 C14 111.4(5) . . ? C11 C15 C16 113.7(5) . . ? C11 C15 C17 110.0(4) . . ? C16 C15 C17 109.5(6) . . ? C19 C18 C23 122.8(5) . . ? C19 C18 N2 118.3(5) . . ? C23 C18 N2 118.9(5) . . ? C18 C19 C20 117.0(6) . . ? C18 C19 C24 121.3(5) . . ? C20 C19 C24 121.7(5) . . ? C21 C20 C19 120.9(6) . . ? C20 C21 C22 121.0(6) . . ? C21 C22 C23 121.1(6) . . ? C22 C23 C18 117.0(6) . . ? C22 C23 C27 121.3(6) . . ? C18 C23 C27 121.6(5) . . ? C19 C24 C26 112.9(5) . . ? C19 C24 C25 113.7(5) . . ? C26 C24 C25 108.4(5) . . ? C28 C27 C29 109.6(6) . . ? C28 C27 C23 110.6(5) . . ? C29 C27 C23 114.0(6) . . ? C35 C30 C31 117.4(6) . . ? C35 C30 P 125.9(5) . . ? C31 C30 P 116.3(5) . . ? C32 C31 C30 120.7(7) . . ? C33 C32 C31 120.6(8) . . ? C32 C33 C34 120.2(8) . . ? C33 C34 C35 119.8(7) . . ? C30 C35 C34 121.2(7) . . ? #===END data_sep2102 _database_code_CSD 203508 _audit_creation_date 2002-09-24T16:03:38-00:00 _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 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; '[C2P2N(Me)(C6H3iPr2)(Ph)2{C(Me)NC6H3iPr2}].benzene' ; _chemical_formula_moiety '(C41 H50 N2 P2)(C6 H6)' _chemical_formula_sum 'C47 H56 N2 P2' _chemical_formula_weight 710.88 _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 14.5205(3) _cell_length_b 19.8810(5) _cell_length_c 15.4891(4) _cell_angle_alpha 90 _cell_angle_beta 110.874(1) _cell_angle_gamma 90 _cell_volume 4177.95(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 39747 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _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 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.13 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.137 _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 0.0488 _diffrn_reflns_av_unetI/netI 0.047 _diffrn_reflns_number 22564 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 25.04 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.936 _diffrn_measured_fraction_theta_max 0.936 _reflns_number_total 6913 _reflns_number_gt 5536 _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^)+(0.0307P)^2^+2.9953P] 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 6913 _refine_ls_number_parameters 462 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1092 _refine_ls_wR_factor_gt 0.101 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.492 _refine_diff_density_min -0.293 _refine_diff_density_rms 0.039 #----------------------------------------------------------------------------# # 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' 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 0.14181(4) 0.22313(3) 0.81742(4) 0.02733(14) Uani 1 1 d . . . P2 P 0.11304(4) 0.23968(3) 0.94620(4) 0.02714(14) Uani 1 1 d . . . N1 N 0.01747(12) 0.20687(8) 0.75229(11) 0.0245(4) Uani 1 1 d . . . N2 N -0.02975(12) 0.21600(8) 1.03616(12) 0.0279(4) Uani 1 1 d . . . C1 C -0.04684(14) 0.19824(10) 0.79928(14) 0.0246(4) Uani 1 1 d . . . C2 C -0.01105(15) 0.20497(10) 0.89319(14) 0.0252(5) Uani 1 1 d . . . C3 C -0.06114(15) 0.18666(10) 0.95670(14) 0.0268(5) Uani 1 1 d . . . C4 C -0.15248(15) 0.18395(12) 0.74088(15) 0.0365(5) Uani 1 1 d . . . H4A H -0.1609 0.1356 0.7281 0.055 Uiso 1 1 calc R . . H4B H -0.17 0.2087 0.6825 0.055 Uiso 1 1 calc R . . H4C H -0.1954 0.1982 0.774 0.055 Uiso 1 1 calc R . . C5 C -0.13879(18) 0.13224(12) 0.93181(16) 0.0399(6) Uani 1 1 d . . . H5A H -0.1368 0.1087 0.988 0.06 Uiso 1 1 calc R . . H5B H -0.1259 0.1002 0.8893 0.06 Uiso 1 1 calc R . . H5C H -0.204 0.1525 0.902 0.06 Uiso 1 1 calc R . . C6 C 0.19475(15) 0.13775(11) 0.83962(15) 0.0310(5) Uani 1 1 d . . . C7 C 0.15764(18) 0.08509(12) 0.87685(18) 0.0439(6) Uani 1 1 d . . . H7 H 0.1014 0.0924 0.8934 0.053 Uiso 1 1 calc R . . C8 C 0.2014(2) 0.02239(13) 0.8901(2) 0.0584(7) Uani 1 1 d . . . H8 H 0.1747 -0.0133 0.9147 0.07 Uiso 1 1 calc R . . C9 C 0.2837(2) 0.01175(15) 0.8675(2) 0.0654(9) Uani 1 1 d . . . H9 H 0.3141 -0.0313 0.8768 0.078 Uiso 1 1 calc R . . C10 C 0.32194(19) 0.06301(15) 0.8315(2) 0.0608(8) Uani 1 1 d . . . H10 H 0.379 0.0554 0.8163 0.073 Uiso 1 1 calc R . . C11 C 0.27784(16) 0.12593(12) 0.81715(17) 0.0417(6) Uani 1 1 d . . . H11 H 0.3046 0.1611 0.7918 0.05 Uiso 1 1 calc R . . C12 C 0.08974(16) 0.33120(10) 0.93147(14) 0.0304(5) Uani 1 1 d . . . C13 C 0.16680(18) 0.37328(12) 0.93429(18) 0.0457(6) Uani 1 1 d . . . H13 H 0.2299 0.3548 0.9434 0.055 Uiso 1 1 calc R . . C14 C 0.1524(2) 0.44254(13) 0.9238(2) 0.0558(7) Uani 1 1 d . . . H14 H 0.2052 0.4709 0.9242 0.067 Uiso 1 1 calc R . . C15 C 0.0621(2) 0.46998(12) 0.91298(18) 0.0506(7) Uani 1 1 d . . . H15 H 0.0521 0.5172 0.9056 0.061 Uiso 1 1 calc R . . C16 C -0.0137(2) 0.42852(12) 0.91295(17) 0.0458(6) Uani 1 1 d . . . H16 H -0.0757 0.4475 0.907 0.055 Uiso 1 1 calc R . . C17 C -0.00094(17) 0.35973(11) 0.92146(16) 0.0370(5) Uani 1 1 d . . . H17 H -0.0543 0.3317 0.9205 0.044 Uiso 1 1 calc R . . C18 C -0.01653(14) 0.21372(10) 0.65269(14) 0.0255(4) Uani 1 1 d . . . C19 C -0.03910(15) 0.27793(10) 0.61334(14) 0.0286(5) Uani 1 1 d . . . C20 C -0.06957(16) 0.28345(11) 0.51780(15) 0.0348(5) Uani 1 1 d . . . H20 H -0.0853 0.3265 0.4898 0.042 Uiso 1 1 calc R . . C21 C -0.07742(17) 0.22754(12) 0.46273(15) 0.0365(5) Uani 1 1 d . . . H21 H -0.0974 0.2322 0.3976 0.044 Uiso 1 1 calc R . . C22 C -0.05608(16) 0.16510(11) 0.50279(15) 0.0343(5) Uani 1 1 d . . . H22 H -0.0623 0.1269 0.4643 0.041 Uiso 1 1 calc R . . C23 C -0.02561(15) 0.15604(10) 0.59810(14) 0.0281(5) Uani 1 1 d . . . C24 C -0.03603(17) 0.34005(11) 0.67097(16) 0.0367(5) Uani 1 1 d . . . H24 H -0.0129 0.3262 0.7374 0.044 Uiso 1 1 calc R . . C25 C -0.1390(2) 0.37004(14) 0.6458(2) 0.0649(8) Uani 1 1 d . . . H25A H -0.1361 0.4099 0.684 0.097 Uiso 1 1 calc R . . H25B H -0.1832 0.3366 0.6569 0.097 Uiso 1 1 calc R . . H25C H -0.164 0.3829 0.5804 0.097 Uiso 1 1 calc R . . C26 C 0.0351(2) 0.39251(13) 0.6602(2) 0.0561(7) Uani 1 1 d . . . H26A H 0.0354 0.4316 0.6988 0.084 Uiso 1 1 calc R . . H26B H 0.0143 0.4064 0.5954 0.084 Uiso 1 1 calc R . . H26C H 0.1016 0.3733 0.6795 0.084 Uiso 1 1 calc R . . C27 C -0.00628(17) 0.08547(11) 0.63788(16) 0.0364(5) Uani 1 1 d . . . H27 H 0.0111 0.0889 0.7063 0.044 Uiso 1 1 calc R . . C28 C -0.0989(2) 0.04156(12) 0.59912(19) 0.0512(7) Uani 1 1 d . . . H28A H -0.0848 -0.0036 0.6259 0.077 Uiso 1 1 calc R . . H28B H -0.1186 0.0386 0.5318 0.077 Uiso 1 1 calc R . . H28C H -0.1525 0.0617 0.6149 0.077 Uiso 1 1 calc R . . C29 C 0.08029(19) 0.05285(13) 0.61996(18) 0.0496(7) Uani 1 1 d . . . H29A H 0.0911 0.0075 0.6466 0.074 Uiso 1 1 calc R . . H29B H 0.1397 0.08 0.6486 0.074 Uiso 1 1 calc R . . H29C H 0.0657 0.05 0.5532 0.074 Uiso 1 1 calc R . . C30 C -0.06813(16) 0.19645(10) 1.10524(14) 0.0291(5) Uani 1 1 d . . . C31 C -0.01017(17) 0.15387(11) 1.17607(15) 0.0356(5) Uani 1 1 d . . . C32 C -0.0487(2) 0.13329(12) 1.24249(17) 0.0449(6) Uani 1 1 d . . . H32 H -0.0114 0.1039 1.2905 0.054 Uiso 1 1 calc R . . C33 C -0.1400(2) 0.15494(13) 1.23959(17) 0.0461(6) Uani 1 1 d . . . H33 H -0.1662 0.1388 1.2838 0.055 Uiso 1 1 calc R . . C34 C -0.19339(18) 0.19991(12) 1.17264(17) 0.0418(6) Uani 1 1 d . . . H34 H -0.2547 0.2161 1.1732 0.05 Uiso 1 1 calc R . . C35 C -0.15895(16) 0.22205(11) 1.10407(15) 0.0330(5) Uani 1 1 d . . . C36 C 0.09013(19) 0.13011(13) 1.17840(17) 0.0452(6) Uani 1 1 d . . . H36 H 0.1108 0.1606 1.1373 0.054 Uiso 1 1 calc R . . C37 C 0.1687(2) 0.13450(15) 1.27466(19) 0.0594(7) Uani 1 1 d . . . H37A H 0.232 0.1192 1.2725 0.089 Uiso 1 1 calc R . . H37B H 0.1498 0.1059 1.3172 0.089 Uiso 1 1 calc R . . H37C H 0.1748 0.1812 1.2962 0.089 Uiso 1 1 calc R . . C38 C 0.0847(3) 0.05919(17) 1.1399(2) 0.0797(10) Uani 1 1 d . . . H38A H 0.1501 0.0454 1.1416 0.119 Uiso 1 1 calc R . . H38B H 0.0383 0.0583 1.076 0.119 Uiso 1 1 calc R . . H38C H 0.0621 0.0281 1.1774 0.119 Uiso 1 1 calc R . . C39 C -0.21581(16) 0.27354(12) 1.03245(16) 0.0397(6) Uani 1 1 d . . . H39 H -0.2075 0.2614 0.973 0.048 Uiso 1 1 calc R . . C40 C -0.32592(19) 0.27436(17) 1.0145(2) 0.0649(8) Uani 1 1 d . . . H40A H -0.3579 0.3085 0.9677 0.097 Uiso 1 1 calc R . . H40B H -0.3367 0.2851 1.0719 0.097 Uiso 1 1 calc R . . H40C H -0.354 0.2301 0.9922 0.097 Uiso 1 1 calc R . . C41 C -0.1729(2) 0.34390(13) 1.0590(2) 0.0571(7) Uani 1 1 d . . . H41A H -0.2106 0.3762 1.0118 0.086 Uiso 1 1 calc R . . H41B H -0.1039 0.3442 1.0634 0.086 Uiso 1 1 calc R . . H41C H -0.1767 0.3565 1.1188 0.086 Uiso 1 1 calc R . . C42 C 0.5745(2) 0.12434(18) 0.8498(2) 0.0743(9) Uani 1 1 d . A 1 H42 H 0.5557 0.1317 0.9018 0.089 Uiso 1 1 calc R A 1 C43 C 0.5593(2) 0.17361(17) 0.7837(3) 0.0741(9) Uani 1 1 d . A 1 H43 H 0.5306 0.2152 0.7906 0.089 Uiso 1 1 calc R A 1 C44 C 0.5852(2) 0.16322(16) 0.7083(2) 0.0658(9) Uani 1 1 d . A 1 H44 H 0.5747 0.1977 0.6634 0.079 Uiso 1 1 calc R A 1 C45 C 0.6261(2) 0.10349(14) 0.6969(2) 0.0599(8) Uani 1 1 d . A 1 H45 H 0.6431 0.0959 0.6438 0.072 Uiso 1 1 calc R A 1 C46 C 0.6424(2) 0.05414(14) 0.7640(2) 0.0674(9) Uani 1 1 d . A 1 H46 H 0.6716 0.0127 0.7571 0.081 Uiso 1 1 calc R A 1 C47 C 0.6170(2) 0.06443(16) 0.8399(2) 0.0719(10) Uani 1 1 d . A 1 H47 H 0.6287 0.0304 0.8856 0.086 Uiso 1 1 calc R A 1 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 0.0231(3) 0.0324(3) 0.0288(3) -0.0022(2) 0.0122(2) -0.0014(2) P2 0.0248(3) 0.0313(3) 0.0258(3) -0.0030(2) 0.0096(2) -0.0006(2) N1 0.0227(9) 0.0324(9) 0.0209(9) -0.0011(7) 0.0106(7) -0.0013(7) N2 0.0291(9) 0.0326(10) 0.0259(10) -0.0032(8) 0.0145(8) -0.0023(8) C1 0.0248(11) 0.0249(10) 0.0281(12) -0.0023(8) 0.0143(9) -0.0008(8) C2 0.0257(11) 0.0275(11) 0.0264(12) -0.0037(8) 0.0142(9) -0.0016(9) C3 0.0280(11) 0.0292(11) 0.0269(12) -0.0032(9) 0.0143(9) -0.0012(9) C4 0.0258(12) 0.0528(15) 0.0323(13) -0.0032(10) 0.0122(10) -0.0060(10) C5 0.0496(15) 0.0428(13) 0.0347(13) -0.0099(10) 0.0241(12) -0.0183(11) C6 0.0262(11) 0.0355(12) 0.0305(12) -0.0076(9) 0.0089(10) 0.0029(9) C7 0.0406(14) 0.0395(14) 0.0554(16) 0.0046(12) 0.0220(12) 0.0106(11) C8 0.0609(18) 0.0395(15) 0.072(2) 0.0055(13) 0.0207(16) 0.0121(13) C9 0.0502(17) 0.0434(16) 0.092(2) -0.0118(15) 0.0124(16) 0.0198(14) C10 0.0333(14) 0.0579(18) 0.089(2) -0.0289(16) 0.0196(15) 0.0078(13) C11 0.0290(12) 0.0459(14) 0.0513(15) -0.0181(11) 0.0156(11) -0.0007(11) C12 0.0323(12) 0.0307(11) 0.0260(12) -0.0082(9) 0.0076(10) -0.0009(9) C13 0.0322(13) 0.0355(13) 0.0640(17) -0.0064(12) 0.0103(12) -0.0034(11) C14 0.0456(16) 0.0358(14) 0.077(2) -0.0067(13) 0.0101(14) -0.0104(12) C15 0.0586(17) 0.0307(13) 0.0543(17) -0.0050(11) 0.0102(14) 0.0068(12) C16 0.0487(15) 0.0394(14) 0.0492(16) -0.0051(11) 0.0174(13) 0.0112(12) C17 0.0355(13) 0.0378(13) 0.0388(14) -0.0054(10) 0.0148(11) 0.0033(10) C18 0.0234(10) 0.0335(11) 0.0224(11) -0.0002(9) 0.0118(9) -0.0014(9) C19 0.0281(11) 0.0325(12) 0.0280(12) -0.0014(9) 0.0135(9) -0.0033(9) C20 0.0373(13) 0.0355(12) 0.0333(14) 0.0064(10) 0.0146(11) 0.0017(10) C21 0.0379(13) 0.0480(14) 0.0233(12) 0.0014(10) 0.0106(10) -0.0002(11) C22 0.0361(12) 0.0394(13) 0.0287(13) -0.0085(10) 0.0130(10) -0.0024(10) C23 0.0250(11) 0.0337(12) 0.0275(12) -0.0020(9) 0.0117(9) -0.0011(9) C24 0.0476(14) 0.0278(12) 0.0355(13) -0.0006(10) 0.0157(11) -0.0007(10) C25 0.0587(18) 0.0473(16) 0.098(2) -0.0206(15) 0.0387(18) 0.0035(14) C26 0.0570(17) 0.0409(15) 0.073(2) -0.0109(13) 0.0259(15) -0.0123(13) C27 0.0439(14) 0.0309(12) 0.0307(13) -0.0036(9) 0.0087(11) 0.0030(10) C28 0.0601(17) 0.0349(14) 0.0565(17) -0.0036(12) 0.0182(14) -0.0084(12) C29 0.0512(16) 0.0415(14) 0.0514(16) -0.0101(12) 0.0124(13) 0.0100(12) C30 0.0338(12) 0.0329(12) 0.0256(12) -0.0071(9) 0.0168(10) -0.0086(10) C31 0.0467(14) 0.0353(12) 0.0297(13) -0.0034(10) 0.0197(11) -0.0027(11) C32 0.0632(17) 0.0445(14) 0.0328(14) 0.0011(11) 0.0240(13) -0.0032(13) C33 0.0608(17) 0.0538(16) 0.0365(15) -0.0066(12) 0.0332(13) -0.0132(13) C34 0.0429(14) 0.0529(15) 0.0409(15) -0.0122(12) 0.0288(12) -0.0095(12) C35 0.0333(12) 0.0416(13) 0.0287(12) -0.0103(10) 0.0167(10) -0.0070(10) C36 0.0489(15) 0.0523(15) 0.0376(14) 0.0076(11) 0.0193(12) 0.0106(12) C37 0.0529(17) 0.071(2) 0.0518(17) 0.0089(14) 0.0155(14) 0.0044(15) C38 0.072(2) 0.080(2) 0.083(2) -0.0228(18) 0.0225(19) 0.0275(18) C39 0.0317(12) 0.0564(15) 0.0354(14) -0.0036(11) 0.0171(11) 0.0041(11) C40 0.0364(15) 0.095(2) 0.064(2) 0.0069(17) 0.0178(14) 0.0036(15) C41 0.0584(18) 0.0497(16) 0.0597(18) 0.0042(13) 0.0169(15) 0.0048(14) C42 0.062(2) 0.075(2) 0.084(2) 0.0010(19) 0.0230(18) -0.0222(18) C43 0.0518(19) 0.061(2) 0.105(3) 0.0140(19) 0.0219(19) 0.0024(15) C44 0.0369(15) 0.0585(19) 0.087(2) 0.0244(17) 0.0030(16) -0.0029(14) C45 0.0416(16) 0.0535(18) 0.068(2) 0.0022(14) -0.0010(14) -0.0143(14) C46 0.0583(19) 0.0392(16) 0.082(2) 0.0020(15) -0.0033(17) -0.0112(14) C47 0.074(2) 0.0527(19) 0.067(2) 0.0126(16) -0.0012(18) -0.0295(17) #----------------------------------------------------------------------------# # 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 1.7560(17) . ? P1 C6 1.845(2) . ? P1 P2 2.2036(8) . ? P2 C2 1.828(2) . ? P2 C12 1.850(2) . ? N1 C1 1.384(2) . ? N1 C18 1.449(3) . ? N2 C3 1.290(3) . ? N2 C30 1.425(3) . ? C1 C2 1.366(3) . ? C1 C4 1.504(3) . ? C2 C3 1.463(3) . ? C3 C5 1.510(3) . ? C6 C11 1.390(3) . ? C6 C7 1.393(3) . ? C7 C8 1.381(3) . ? C8 C9 1.377(4) . ? C9 C10 1.370(4) . ? C10 C11 1.387(4) . ? C12 C13 1.385(3) . ? C12 C17 1.391(3) . ? C13 C14 1.394(3) . ? C14 C15 1.374(4) . ? C15 C16 1.375(4) . ? C16 C17 1.380(3) . ? C18 C19 1.402(3) . ? C18 C23 1.403(3) . ? C19 C20 1.390(3) . ? C19 C24 1.515(3) . ? C20 C21 1.381(3) . ? C21 C22 1.373(3) . ? C22 C23 1.394(3) . ? C23 C27 1.518(3) . ? C24 C26 1.519(3) . ? C24 C25 1.526(4) . ? C27 C29 1.525(3) . ? C27 C28 1.535(3) . ? C30 C31 1.404(3) . ? C30 C35 1.408(3) . ? C31 C32 1.396(3) . ? C31 C36 1.519(3) . ? C32 C33 1.379(4) . ? C33 C34 1.379(4) . ? C34 C35 1.397(3) . ? C35 C39 1.519(3) . ? C36 C38 1.522(4) . ? C36 C37 1.523(4) . ? C39 C40 1.522(3) . ? C39 C41 1.527(4) . ? C42 C47 1.375(5) . ? C42 C43 1.377(5) . ? C43 C44 1.363(5) . ? C44 C45 1.368(4) . ? C45 C46 1.387(4) . ? C46 C47 1.368(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 P1 C6 102.27(9) . . ? N1 P1 P2 93.43(6) . . ? C6 P1 P2 99.76(7) . . ? C2 P2 C12 102.02(9) . . ? C2 P2 P1 90.66(7) . . ? C12 P2 P1 96.92(7) . . ? C1 N1 C18 122.26(16) . . ? C1 N1 P1 117.97(13) . . ? C18 N1 P1 119.00(13) . . ? C3 N2 C30 119.56(17) . . ? C2 C1 N1 118.42(18) . . ? C2 C1 C4 125.34(18) . . ? N1 C1 C4 116.21(17) . . ? C1 C2 C3 126.89(19) . . ? C1 C2 P2 117.09(15) . . ? C3 C2 P2 116.01(15) . . ? N2 C3 C2 115.98(18) . . ? N2 C3 C5 123.06(18) . . ? C2 C3 C5 120.76(18) . . ? C11 C6 C7 118.4(2) . . ? C11 C6 P1 116.77(18) . . ? C7 C6 P1 124.88(16) . . ? C8 C7 C6 121.0(2) . . ? C9 C8 C7 119.7(3) . . ? C10 C9 C8 120.2(3) . . ? C9 C10 C11 120.3(2) . . ? C10 C11 C6 120.3(2) . . ? C13 C12 C17 118.6(2) . . ? C13 C12 P2 118.68(17) . . ? C17 C12 P2 122.63(17) . . ? C12 C13 C14 120.5(2) . . ? C15 C14 C13 120.2(2) . . ? C14 C15 C16 119.4(2) . . ? C15 C16 C17 120.9(2) . . ? C16 C17 C12 120.3(2) . . ? C19 C18 C23 121.67(19) . . ? C19 C18 N1 119.12(17) . . ? C23 C18 N1 119.21(18) . . ? C20 C19 C18 118.12(19) . . ? C20 C19 C24 119.63(19) . . ? C18 C19 C24 122.18(19) . . ? C21 C20 C19 121.3(2) . . ? C22 C21 C20 119.5(2) . . ? C21 C22 C23 122.1(2) . . ? C22 C23 C18 117.33(19) . . ? C22 C23 C27 119.50(19) . . ? C18 C23 C27 123.16(18) . . ? C19 C24 C26 111.93(19) . . ? C19 C24 C25 110.3(2) . . ? C26 C24 C25 110.3(2) . . ? C23 C27 C29 111.4(2) . . ? C23 C27 C28 110.94(19) . . ? C29 C27 C28 110.56(19) . . ? C31 C30 C35 121.74(19) . . ? C31 C30 N2 117.73(19) . . ? C35 C30 N2 120.45(19) . . ? C32 C31 C30 117.8(2) . . ? C32 C31 C36 121.6(2) . . ? C30 C31 C36 120.58(19) . . ? C33 C32 C31 121.2(2) . . ? C34 C33 C32 120.2(2) . . ? C33 C34 C35 121.2(2) . . ? C34 C35 C30 117.6(2) . . ? C34 C35 C39 121.3(2) . . ? C30 C35 C39 121.06(18) . . ? C31 C36 C38 111.3(2) . . ? C31 C36 C37 112.5(2) . . ? C38 C36 C37 110.7(2) . . ? C35 C39 C40 113.8(2) . . ? C35 C39 C41 110.9(2) . . ? C40 C39 C41 109.9(2) . . ? C47 C42 C43 119.6(4) . . ? C44 C43 C42 120.6(3) . . ? C43 C44 C45 120.5(3) . . ? C44 C45 C46 118.9(3) . . ? C47 C46 C45 120.8(3) . . ? C46 C47 C42 119.6(3) . . ? #===END