# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Martyn Coles' _publ_contact_author_address ; The Chemical Laboratories University of Sussex Chichester Building Falmer Brighton BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email M.P.COLES@SUSSEX.AC.UK _publ_section_title ; A Lewis-Basic, Dionio-Substituted Phosphane ; _publ_requested_category FO loop_ _publ_author_name 'Martyn Coles' 'P. B. Hitchcock' # Attachment 'Revised cifs B710923G.txt' data_(2)-jul706 _database_code_depnum_ccdc_archive 'CCDC 644406' _audit_creation_date 2006-07-06T15:58:30-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C21 H31 N6 P, C H2 Cl2, 2(Cl)' _chemical_formula_sum 'C22 H33 Cl4 N6 P' _chemical_formula_weight 554.31 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' _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 13.5675(3) _cell_length_b 15.3805(2) _cell_length_c 12.3987(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2587.30(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 16852 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.543 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _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_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.108597E-1 _diffrn_orient_matrix_ub_12 0.186412E-1 _diffrn_orient_matrix_ub_13 0.622914E-1 _diffrn_orient_matrix_ub_21 0.794486E-1 _diffrn_orient_matrix_ub_22 0.102403E-1 _diffrn_orient_matrix_ub_23 0.66163E-2 _diffrn_orient_matrix_ub_31 -0.00866 _diffrn_orient_matrix_ub_32 0.705702E-1 _diffrn_orient_matrix_ub_33 -0.174144E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_unetI/netI 0.0269 _diffrn_reflns_number 25557 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 26.01 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 5042 _reflns_number_gt 4845 _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-86 (Sheldrick, 1986)' _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^)+(0.0574P)^2^+0.6899P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5042 _refine_ls_number_parameters 303 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.028 _refine_ls_wR_factor_ref 0.0819 _refine_ls_wR_factor_gt 0.0801 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _refine_ls_shift/su_max 0.001 _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 0.04(4) _refine_diff_density_max 0.362 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.113 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 '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 Cl1 Cl 0.36139(4) 0.33831(4) 0.42331(5) 0.03857(14) Uani 1 1 d . . . Cl2 Cl 0.39936(4) 0.71895(4) 0.42237(5) 0.03526(13) Uani 1 1 d . . . Cl3 Cl 0.35849(5) 0.53698(4) 0.67793(7) 0.05292(19) Uani 1 1 d . . . Cl4 Cl 0.17846(7) 0.53887(4) 0.54667(6) 0.0561(2) Uani 1 1 d . . . P P 0.38569(3) 0.04738(3) 0.71922(4) 0.01933(11) Uani 1 1 d . A . N1 N 0.16166(11) 0.10694(11) 0.66505(14) 0.0222(3) Uani 1 1 d . . . N2 N 0.30984(12) 0.13301(11) 0.75602(14) 0.0216(3) Uani 1 1 d . . . N3 N 0.21959(12) 0.24777(11) 0.68057(13) 0.0248(3) Uani 1 1 d . . . N4 N 0.18384(12) -0.05094(11) 0.66540(15) 0.0249(4) Uani 1 1 d . . . N5 N 0.33049(12) -0.04794(10) 0.76343(14) 0.0204(3) Uani 1 1 d . . . N6 N 0.27384(12) -0.17783(10) 0.68759(13) 0.0233(3) Uani 1 1 d . . . C1 C 0.22940(13) 0.16403(12) 0.70065(15) 0.0211(4) Uani 1 1 d . . . C2 C 0.08973(16) 0.12871(15) 0.5800(2) 0.0330(5) Uani 1 1 d . . . H2B H 0.0222 0.1211 0.6087 0.04 Uiso 1 1 calc R . . H2A H 0.0981 0.088 0.5189 0.04 Uiso 1 1 calc R . . C3 C 0.10143(17) 0.22078(16) 0.5396(2) 0.0347(5) Uani 1 1 d . . . H3B H 0.1541 0.2231 0.4843 0.042 Uiso 1 1 calc R . . H3A H 0.0392 0.2406 0.506 0.042 Uiso 1 1 calc R . . C4 C 0.12750(17) 0.27910(15) 0.6325(2) 0.0336(5) Uani 1 1 d . . . H4B H 0.1358 0.3396 0.6069 0.04 Uiso 1 1 calc R . . H4A H 0.0741 0.2782 0.6869 0.04 Uiso 1 1 calc R . . C5 C 0.29052(17) 0.31481(13) 0.7132(2) 0.0339(5) Uani 1 1 d . . . H5B H 0.2591 0.3538 0.7666 0.041 Uiso 1 1 calc R . . H5A H 0.3084 0.3502 0.6494 0.041 Uiso 1 1 calc R . . C6 C 0.38128(18) 0.27723(16) 0.7606(2) 0.0378(6) Uani 1 1 d . . . H6B H 0.4144 0.3215 0.8059 0.045 Uiso 1 1 calc R . . H6A H 0.4272 0.2604 0.7022 0.045 Uiso 1 1 calc R . . C7 C 0.35712(16) 0.19836(14) 0.82856(17) 0.0274(4) Uani 1 1 d . . . H7B H 0.418 0.174 0.8607 0.033 Uiso 1 1 calc R . . H7A H 0.3116 0.2145 0.8876 0.033 Uiso 1 1 calc R . . C8 C 0.14627(13) 0.02500(13) 0.7213(2) 0.0246(4) Uani 1 1 d . A . H8B H 0.1783 0.0286 0.7929 0.029 Uiso 1 1 calc R . . H8A H 0.0747 0.0172 0.7335 0.029 Uiso 1 1 calc R . . C9 C 0.26142(13) -0.09448(12) 0.70579(15) 0.0199(4) Uani 1 1 d . A . C13 C 0.36248(15) -0.22734(13) 0.7192(2) 0.0290(5) Uani 1 1 d . A . H13B H 0.391 -0.2549 0.6541 0.035 Uiso 1 1 calc R . . H13A H 0.3427 -0.2743 0.7693 0.035 Uiso 1 1 calc R . . C14 C 0.44145(16) -0.17193(13) 0.77319(17) 0.0267(4) Uani 1 1 d . . . H14B H 0.4826 -0.2084 0.8211 0.032 Uiso 1 1 calc R A . H14A H 0.4846 -0.1453 0.7179 0.032 Uiso 1 1 calc R . . C15 C 0.39052(14) -0.10157(13) 0.83822(17) 0.0234(4) Uani 1 1 d . A . H15B H 0.3477 -0.1282 0.8938 0.028 Uiso 1 1 calc R . . H15A H 0.4401 -0.0648 0.8749 0.028 Uiso 1 1 calc R . . C16 C 0.36964(13) 0.04007(12) 0.57332(17) 0.0218(4) Uani 1 1 d . . . C17 C 0.38776(15) -0.03966(14) 0.52144(19) 0.0260(4) Uani 1 1 d . A . H17 H 0.4039 -0.0895 0.5631 0.031 Uiso 1 1 calc R . . C18 C 0.38228(15) -0.04629(15) 0.4099(2) 0.0312(5) Uani 1 1 d . . . H18 H 0.3939 -0.1007 0.3758 0.037 Uiso 1 1 calc R A . C19 C 0.36007(17) 0.02590(17) 0.3484(2) 0.0359(5) Uani 1 1 d . A . H19 H 0.354 0.0209 0.2723 0.043 Uiso 1 1 calc R . . C20 C 0.34662(16) 0.10566(17) 0.39802(18) 0.0337(5) Uani 1 1 d . . . H20 H 0.3329 0.1557 0.3556 0.04 Uiso 1 1 calc R A . C21 C 0.35314(14) 0.11298(15) 0.50969(17) 0.0263(4) Uani 1 1 d . A . H21 H 0.3462 0.1684 0.5427 0.032 Uiso 1 1 calc R . . C22 C 0.3099(3) 0.53475(16) 0.5445(3) 0.0538(8) Uani 1 1 d . . . H22B H 0.3316 0.4809 0.5078 0.065 Uiso 1 1 calc R . . H22A H 0.3358 0.585 0.5033 0.065 Uiso 1 1 calc R . . C10 C 0.12194(18) -0.09549(16) 0.5844(2) 0.0416(6) Uani 0.838(6) 1 d P A 1 H10A H 0.1563 -0.0967 0.5139 0.05 Uiso 0.838(6) 1 calc PR A 1 H10B H 0.059 -0.0638 0.5752 0.05 Uiso 0.838(6) 1 calc PR A 1 C11 C 0.1021(2) -0.18645(19) 0.6218(2) 0.0350(8) Uani 0.838(6) 1 d P A 1 H11A H 0.0652 -0.1851 0.6907 0.042 Uiso 0.838(6) 1 calc PR A 1 H11B H 0.0616 -0.2174 0.5677 0.042 Uiso 0.838(6) 1 calc PR A 1 C12 C 0.19761(17) -0.23291(14) 0.63724(19) 0.0310(5) Uani 0.838(6) 1 d P A 1 H12A H 0.1864 -0.2847 0.6831 0.037 Uiso 0.838(6) 1 calc PR A 1 H12B H 0.2218 -0.2534 0.5663 0.037 Uiso 0.838(6) 1 calc PR A 1 C10A C 0.12194(18) -0.09549(16) 0.5844(2) 0.0416(6) Uani 0.162(6) 1 d P A 2 H10C H 0.0534 -0.0957 0.6119 0.05 Uiso 0.162(6) 1 calc PR A 2 H10D H 0.1223 -0.0594 0.5182 0.05 Uiso 0.162(6) 1 calc PR A 2 C11A C 0.1437(8) -0.1753(7) 0.5559(10) 0.017(3) Uiso 0.162(6) 1 d P A 2 H11C H 0.1846 -0.1723 0.4899 0.021 Uiso 0.162(6) 1 calc PR A 2 H11D H 0.0815 -0.2049 0.5362 0.021 Uiso 0.162(6) 1 calc PR A 2 C12A C 0.19761(17) -0.23291(14) 0.63724(19) 0.0310(5) Uani 0.162(6) 1 d P A 2 H12C H 0.1512 -0.2549 0.6925 0.037 Uiso 0.162(6) 1 calc PR A 2 H12D H 0.2283 -0.2832 0.6004 0.037 Uiso 0.162(6) 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 Cl1 0.0445(3) 0.0360(3) 0.0352(3) -0.0025(3) -0.0091(3) 0.0111(2) Cl2 0.0311(2) 0.0431(3) 0.0315(3) 0.0062(3) -0.0009(2) -0.0072(2) Cl3 0.0504(4) 0.0357(3) 0.0727(5) -0.0065(3) 0.0105(3) -0.0051(2) Cl4 0.0893(6) 0.0430(4) 0.0359(3) -0.0035(3) -0.0062(4) -0.0118(3) P 0.0179(2) 0.0192(2) 0.0209(2) 0.0008(2) -0.0008(2) -0.00100(17) N1 0.0200(8) 0.0228(8) 0.0238(8) 0.0029(7) -0.0007(7) 0.0012(6) N2 0.0227(8) 0.0207(8) 0.0214(8) -0.0014(6) -0.0024(6) -0.0005(7) N3 0.0259(8) 0.0214(8) 0.0271(9) 0.0015(7) -0.0004(7) 0.0007(7) N4 0.0224(8) 0.0238(8) 0.0285(9) 0.0011(7) -0.0059(7) -0.0028(6) N5 0.0213(8) 0.0183(8) 0.0216(8) 0.0012(6) -0.0027(6) -0.0013(6) N6 0.0253(8) 0.0222(8) 0.0223(8) 0.0003(7) 0.0013(7) -0.0044(6) C1 0.0216(9) 0.0221(9) 0.0195(9) 0.0026(8) 0.0037(7) 0.0023(7) C2 0.0295(11) 0.0326(12) 0.0367(13) 0.0037(10) -0.0112(10) 0.0023(9) C3 0.0317(12) 0.0356(12) 0.0367(13) 0.0102(10) -0.0087(10) 0.0034(9) C4 0.0316(12) 0.0272(11) 0.0419(13) 0.0073(10) -0.0039(10) 0.0069(9) C5 0.0413(12) 0.0225(10) 0.0379(12) -0.0002(10) 0.0010(11) -0.0060(9) C6 0.0339(12) 0.0319(12) 0.0478(15) -0.0027(11) -0.0029(10) -0.0076(9) C7 0.0285(10) 0.0273(11) 0.0264(11) -0.0077(9) -0.0033(8) -0.0028(8) C8 0.0188(8) 0.0249(9) 0.0300(11) 0.0008(9) 0.0020(9) -0.0004(7) C9 0.0216(8) 0.0218(8) 0.0164(9) 0.0012(7) 0.0030(7) -0.0046(7) C13 0.0335(11) 0.0227(10) 0.0308(11) -0.0017(10) 0.0013(10) 0.0046(8) C14 0.0288(10) 0.0253(10) 0.0259(10) 0.0021(8) -0.0006(8) 0.0039(8) C15 0.0267(9) 0.0223(10) 0.0212(9) 0.0030(8) -0.0030(8) 0.0023(7) C16 0.0169(9) 0.0256(10) 0.0230(11) 0.0017(8) 0.0045(7) -0.0024(7) C17 0.0247(10) 0.0250(10) 0.0282(11) 0.0011(8) 0.0062(8) -0.0036(8) C18 0.0274(11) 0.0380(12) 0.0282(12) -0.0080(10) 0.0061(9) -0.0071(8) C19 0.0303(11) 0.0564(16) 0.0210(11) -0.0009(10) 0.0018(9) -0.0017(10) C20 0.0285(11) 0.0449(13) 0.0278(13) 0.0135(10) 0.0056(9) 0.0074(9) C21 0.0227(9) 0.0292(11) 0.0270(11) 0.0032(9) 0.0063(8) 0.0011(8) C22 0.087(2) 0.0281(12) 0.0462(15) -0.0051(11) 0.0268(16) -0.0101(12) C10 0.0409(13) 0.0346(13) 0.0493(15) -0.0041(12) -0.0225(12) -0.0054(10) C11 0.0321(15) 0.0350(15) 0.0378(17) -0.0037(12) -0.0042(11) -0.0120(11) C12 0.0384(12) 0.0241(10) 0.0305(11) -0.0019(9) -0.0030(9) -0.0108(9) C10A 0.0409(13) 0.0346(13) 0.0493(15) -0.0041(12) -0.0225(12) -0.0054(10) C12A 0.0384(12) 0.0241(10) 0.0305(11) -0.0019(9) -0.0030(9) -0.0108(9) #----------------------------------------------------------------------------# # 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 Cl3 C22 1.781(4) . ? Cl4 C22 1.785(4) . ? P N2 1.7326(17) . ? P N5 1.7351(16) . ? P C16 1.825(2) . ? N1 C1 1.346(3) . ? N1 C8 1.456(3) . ? N1 C2 1.475(3) . ? N2 C1 1.375(2) . ? N2 C7 1.494(3) . ? N3 C1 1.319(2) . ? N3 C4 1.466(3) . ? N3 C5 1.467(3) . ? N4 C9 1.344(2) . ? N4 C8 1.451(3) . ? N4 C10 1.478(3) . ? N5 C9 1.379(2) . ? N5 C15 1.484(2) . ? N6 C9 1.312(2) . ? N6 C12 1.476(3) . ? N6 C13 1.476(3) . ? C2 C3 1.510(3) . ? C2 H2B 0.99 . ? C2 H2A 0.99 . ? C3 C4 1.502(4) . ? C3 H3B 0.99 . ? C3 H3A 0.99 . ? C4 H4B 0.99 . ? C4 H4A 0.99 . ? C5 C6 1.482(3) . ? C5 H5B 0.99 . ? C5 H5A 0.99 . ? C6 C7 1.513(3) . ? C6 H6B 0.99 . ? C6 H6A 0.99 . ? C7 H7B 0.99 . ? C7 H7A 0.99 . ? C8 H8B 0.99 . ? C8 H8A 0.99 . ? C13 C14 1.524(3) . ? C13 H13B 0.99 . ? C13 H13A 0.99 . ? C14 C15 1.516(3) . ? C14 H14B 0.99 . ? C14 H14A 0.99 . ? C15 H15B 0.99 . ? C15 H15A 0.99 . ? C16 C21 1.389(3) . ? C16 C17 1.406(3) . ? C17 C18 1.389(3) . ? C17 H17 0.95 . ? C18 C19 1.380(4) . ? C18 H18 0.95 . ? C19 C20 1.384(4) . ? C19 H19 0.95 . ? C20 C21 1.392(3) . ? C20 H20 0.95 . ? C21 H21 0.95 . ? C22 H22B 0.99 . ? C22 H22A 0.99 . ? C10 C11 1.498(4) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C11 C12 1.492(4) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C11A H11C 0.99 . ? C11A H11D 0.99 . ? 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 N2 P N5 107.63(8) . . ? N2 P C16 103.71(8) . . ? N5 P C16 102.09(9) . . ? C1 N1 C8 120.37(17) . . ? C1 N1 C2 122.56(17) . . ? C8 N1 C2 116.39(16) . . ? C1 N2 C7 114.09(16) . . ? C1 N2 P 127.14(14) . . ? C7 N2 P 114.52(13) . . ? C1 N3 C4 118.95(17) . . ? C1 N3 C5 124.62(17) . . ? C4 N3 C5 116.11(17) . . ? C9 N4 C8 119.87(17) . . ? C9 N4 C10 117.86(17) . . ? C8 N4 C10 119.90(17) . . ? C9 N5 C15 114.09(15) . . ? C9 N5 P 124.63(14) . . ? C15 N5 P 115.47(13) . . ? C9 N6 C12 122.92(17) . . ? C9 N6 C13 124.25(17) . . ? C12 N6 C13 112.77(17) . . ? N3 C1 N1 120.43(17) . . ? N3 C1 N2 120.89(17) . . ? N1 C1 N2 118.66(16) . . ? N1 C2 C3 112.36(18) . . ? N1 C2 H2B 109.1 . . ? C3 C2 H2B 109.1 . . ? N1 C2 H2A 109.1 . . ? C3 C2 H2A 109.1 . . ? H2B C2 H2A 107.9 . . ? C4 C3 C2 109.3(2) . . ? C4 C3 H3B 109.8 . . ? C2 C3 H3B 109.8 . . ? C4 C3 H3A 109.8 . . ? C2 C3 H3A 109.8 . . ? H3B C3 H3A 108.3 . . ? N3 C4 C3 108.44(18) . . ? N3 C4 H4B 110 . . ? C3 C4 H4B 110 . . ? N3 C4 H4A 110 . . ? C3 C4 H4A 110 . . ? H4B C4 H4A 108.4 . . ? N3 C5 C6 112.35(18) . . ? N3 C5 H5B 109.1 . . ? C6 C5 H5B 109.1 . . ? N3 C5 H5A 109.1 . . ? C6 C5 H5A 109.1 . . ? H5B C5 H5A 107.9 . . ? C5 C6 C7 110.72(19) . . ? C5 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 . . ? C5 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 . . ? H6B C6 H6A 108.1 . . ? N2 C7 C6 107.30(18) . . ? N2 C7 H7B 110.3 . . ? C6 C7 H7B 110.3 . . ? N2 C7 H7A 110.3 . . ? C6 C7 H7A 110.3 . . ? H7B C7 H7A 108.5 . . ? N4 C8 N1 114.67(18) . . ? N4 C8 H8B 108.6 . . ? N1 C8 H8B 108.6 . . ? N4 C8 H8A 108.6 . . ? N1 C8 H8A 108.6 . . ? H8B C8 H8A 107.6 . . ? N6 C9 N4 121.54(17) . . ? N6 C9 N5 120.59(17) . . ? N4 C9 N5 117.81(16) . . ? N6 C13 C14 113.63(16) . . ? N6 C13 H13B 108.8 . . ? C14 C13 H13B 108.8 . . ? N6 C13 H13A 108.8 . . ? C14 C13 H13A 108.8 . . ? H13B C13 H13A 107.7 . . ? C15 C14 C13 108.20(17) . . ? C15 C14 H14B 110.1 . . ? C13 C14 H14B 110.1 . . ? C15 C14 H14A 110.1 . . ? C13 C14 H14A 110.1 . . ? H14B C14 H14A 108.4 . . ? N5 C15 C14 108.33(16) . . ? N5 C15 H15B 110 . . ? C14 C15 H15B 110 . . ? N5 C15 H15A 110 . . ? C14 C15 H15A 110 . . ? H15B C15 H15A 108.4 . . ? C21 C16 C17 118.2(2) . . ? C21 C16 P 122.16(16) . . ? C17 C16 P 119.09(15) . . ? C18 C17 C16 120.7(2) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C19 C18 C17 120.2(2) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 119.8(2) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C19 C20 C21 120.4(2) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C16 C21 C20 120.7(2) . . ? C16 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? Cl3 C22 Cl4 110.81(16) . . ? Cl3 C22 H22B 109.5 . . ? Cl4 C22 H22B 109.5 . . ? Cl3 C22 H22A 109.5 . . ? Cl4 C22 H22A 109.5 . . ? H22B C22 H22A 108.1 . . ? N4 C10 C11 108.9(2) . . ? N4 C10 H10A 109.9 . . ? C11 C10 H10A 109.9 . . ? N4 C10 H10B 109.9 . . ? C11 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? C12 C11 C10 109.3(2) . . ? C12 C11 H11A 109.8 . . ? C10 C11 H11A 109.8 . . ? C12 C11 H11B 109.8 . . ? C10 C11 H11B 109.8 . . ? H11A C11 H11B 108.3 . . ? N6 C12 C11 112.82(19) . . ? N6 C12 H12A 109 . . ? C11 C12 H12A 109 . . ? N6 C12 H12B 109 . . ? C11 C12 H12B 109 . . ? H12A C12 H12B 107.8 . . ? H11C C11A H11D 107.1 . . ? #===END data_(4)-feb607 _database_code_depnum_ccdc_archive 'CCDC 644407' _audit_creation_date 2007-02-12T11:53:07-00:00 _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 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C21 H31 Cl3 N6 P Pt, C2 H3 N, Cl' _chemical_formula_sum 'C23 H34 Cl4 N7 P Pt' _chemical_formula_weight 776.43 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _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 14.0180(5) _cell_length_b 14.4145(4) _cell_length_c 15.2158(5) _cell_angle_alpha 90 _cell_angle_beta 113.878(2) _cell_angle_gamma 90 _cell_volume 2811.39(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 51881 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.834 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.456 _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 0.4341 _exptl_absorpt_correction_T_max 0.6155 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.229155E-1 _diffrn_orient_matrix_ub_12 0.19189E-2 _diffrn_orient_matrix_ub_13 0.05425 _diffrn_orient_matrix_ub_21 -0.745506E-1 _diffrn_orient_matrix_ub_22 0.10899E-2 _diffrn_orient_matrix_ub_23 -0.471384E-1 _diffrn_orient_matrix_ub_31 -0.1806E-2 _diffrn_orient_matrix_ub_32 -0.693395E-1 _diffrn_orient_matrix_ub_33 0.7604E-3 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0767 _diffrn_reflns_av_unetI/netI 0.0377 _diffrn_reflns_number 38517 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 26.04 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 5528 _reflns_number_gt 4763 _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 disordered C3 and C6 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^)+(0.0449P)^2^+15.8999P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5528 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.1122 _refine_ls_wR_factor_gt 0.1064 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 4.108 _refine_diff_density_min -1.163 _refine_diff_density_rms 0.152 #----------------------------------------------------------------------------# # 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' Pt Pt -1.7033 8.3905 '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 Pt Pt 0.490375(19) 0.631805(15) 0.753657(19) 0.03094(11) Uani 1 1 d . . . Cl1 Cl 0.43501(15) 0.68180(13) 0.59676(14) 0.0459(4) Uani 1 1 d . . . Cl2 Cl 0.66356(14) 0.64678(12) 0.76908(17) 0.0478(5) Uani 1 1 d . . . Cl3 Cl 0.55504(14) 0.58025(14) 0.90975(14) 0.0485(5) Uani 1 1 d . . . Cl4 Cl 0.00341(16) 0.56007(18) 0.74453(14) 0.0573(6) Uani 1 1 d . . . P P 0.32691(13) 0.62497(10) 0.73642(13) 0.0267(3) Uani 1 1 d . A . N1 N 0.3549(5) 0.4307(4) 0.6603(4) 0.0385(14) Uani 1 1 d . . . N2 N 0.2498(4) 0.5620(4) 0.6408(4) 0.0311(12) Uani 1 1 d . . . N3 N 0.2673(5) 0.4952(4) 0.5099(4) 0.0399(14) Uani 1 1 d . . . N4 N 0.2716(4) 0.4266(3) 0.7743(4) 0.0324(12) Uani 1 1 d . . . N5 N 0.3072(4) 0.5779(3) 0.8329(4) 0.0286(11) Uani 1 1 d . . . N6 N 0.2281(4) 0.4738(4) 0.8977(4) 0.0322(12) Uani 1 1 d . . . C1 C 0.2934(5) 0.4947(4) 0.6032(5) 0.0302(14) Uani 1 1 d . A . C8 C 0.3662(5) 0.4138(4) 0.7595(5) 0.0353(15) Uani 1 1 d . A . H8A H 0.3911 0.3494 0.7776 0.042 Uiso 1 1 calc R . . H8B H 0.4203 0.4561 0.803 0.042 Uiso 1 1 calc R . . C9 C 0.2673(5) 0.4926(4) 0.8355(5) 0.0292(13) Uani 1 1 d . A . C10 C 0.1984(6) 0.3474(5) 0.7562(6) 0.0406(17) Uani 1 1 d . A . H10A H 0.1254 0.369 0.7228 0.049 Uiso 1 1 calc R . . H10B H 0.2123 0.3004 0.7154 0.049 Uiso 1 1 calc R . . C11 C 0.2149(6) 0.3068(5) 0.8510(6) 0.0445(18) Uani 1 1 d . . . H11A H 0.2879 0.2853 0.8841 0.053 Uiso 1 1 calc R A . H11B H 0.1681 0.2529 0.842 0.053 Uiso 1 1 calc R . . C12 C 0.1920(6) 0.3800(5) 0.9106(6) 0.0403(17) Uani 1 1 d . A . H12A H 0.1158 0.3819 0.8929 0.048 Uiso 1 1 calc R . . H12B H 0.2264 0.3624 0.9793 0.048 Uiso 1 1 calc R . . C13 C 0.2090(6) 0.5426(5) 0.9606(5) 0.0397(17) Uani 1 1 d . A . H13A H 0.2487 0.5245 1.0285 0.048 Uiso 1 1 calc R . . H13B H 0.134 0.5422 0.9479 0.048 Uiso 1 1 calc R . . C14 C 0.2400(6) 0.6393(5) 0.9458(5) 0.0394(16) Uani 1 1 d . . . H14A H 0.2571 0.6761 1.0052 0.047 Uiso 1 1 calc R A . H14B H 0.1812 0.6699 0.8933 0.047 Uiso 1 1 calc R . . C15 C 0.3336(6) 0.6350(4) 0.9208(5) 0.0345(15) Uani 1 1 d . A . H15A H 0.3534 0.6984 0.9095 0.041 Uiso 1 1 calc R . . H15B H 0.3935 0.6072 0.9747 0.041 Uiso 1 1 calc R . . C16 C 0.2628(6) 0.7364(4) 0.7234(5) 0.0336(15) Uani 1 1 d . . . C17 C 0.3159(6) 0.8155(4) 0.7126(5) 0.0364(15) Uani 1 1 d . A . H17 H 0.382 0.8092 0.7096 0.044 Uiso 1 1 calc R . . C18 C 0.2718(7) 0.9022(5) 0.7064(5) 0.0441(18) Uani 1 1 d . . . H18 H 0.3075 0.9557 0.6991 0.053 Uiso 1 1 calc R A . C19 C 0.1769(8) 0.9113(5) 0.7107(5) 0.052(2) Uani 1 1 d . A . H19 H 0.1474 0.9713 0.7068 0.063 Uiso 1 1 calc R . . C20 C 0.1237(7) 0.8352(6) 0.7205(5) 0.048(2) Uani 1 1 d . . . H20 H 0.0568 0.8428 0.7214 0.057 Uiso 1 1 calc R A . C21 C 0.1668(6) 0.7460(5) 0.7292(5) 0.0360(15) Uani 1 1 d . A . H21 H 0.1311 0.6935 0.7387 0.043 Uiso 1 1 calc R . . C22 C 0.0795(7) 0.2618(7) 1.0326(6) 0.055(2) Uani 1 1 d . . . C23 C 0.0524(9) 0.3473(8) 1.0630(8) 0.079(3) Uani 1 1 d . . . H23A H 0.0367 0.3368 1.1193 0.118 Uiso 1 1 calc R . . H23B H -0.009 0.3735 1.0108 0.118 Uiso 1 1 calc R . . H23C H 0.1109 0.3908 1.0797 0.118 Uiso 1 1 calc R . . N7 N 0.1078(7) 0.1921(6) 1.0118(6) 0.071(2) Uani 1 1 d . . . C2 C 0.4141(10) 0.3696(6) 0.6229(8) 0.077(3) Uani 0.584(15) 1 d P A 1 H2A H 0.4882 0.3695 0.6688 0.092 Uiso 0.584(15) 1 calc PR A 1 H2B H 0.3874 0.3055 0.6191 0.092 Uiso 0.584(15) 1 calc PR A 1 C3 C 0.4081(12) 0.3966(11) 0.5289(11) 0.052(4) Uiso 0.584(15) 1 d P A 1 H3A H 0.4573 0.4483 0.537 0.062 Uiso 0.584(15) 1 calc PR A 1 H3B H 0.4311 0.3437 0.5008 0.062 Uiso 0.584(15) 1 calc PR A 1 C4 C 0.3066(7) 0.4247(6) 0.4626(6) 0.057(2) Uani 0.584(15) 1 d P A 1 H4A H 0.259 0.3706 0.4436 0.068 Uiso 0.584(15) 1 calc PR A 1 H4B H 0.3104 0.451 0.404 0.068 Uiso 0.584(15) 1 calc PR A 1 C5 C 0.1966(7) 0.5649(5) 0.4474(5) 0.0460(18) Uani 0.584(15) 1 d P A 1 H5A H 0.2383 0.6085 0.4271 0.055 Uiso 0.584(15) 1 calc PR A 1 H5B H 0.1475 0.5331 0.3889 0.055 Uiso 0.584(15) 1 calc PR A 1 C6 C 0.1353(12) 0.6192(10) 0.4867(11) 0.049(4) Uiso 0.584(15) 1 d P A 1 H6A H 0.062 0.6211 0.4391 0.059 Uiso 0.584(15) 1 calc PR A 1 H6B H 0.1619 0.6837 0.4972 0.059 Uiso 0.584(15) 1 calc PR A 1 C7 C 0.1381(5) 0.5816(5) 0.5797(5) 0.0412(17) Uani 0.584(15) 1 d P A 1 H7A H 0.1099 0.6277 0.6112 0.049 Uiso 0.584(15) 1 calc PR A 1 H7B H 0.0961 0.5241 0.5684 0.049 Uiso 0.584(15) 1 calc PR A 1 C2A C 0.4141(10) 0.3696(6) 0.6229(8) 0.077(3) Uani 0.416(15) 1 d P A 2 H2A1 H 0.4778 0.4029 0.6277 0.092 Uiso 0.416(15) 1 calc PR A 2 H2A2 H 0.4367 0.3143 0.6649 0.092 Uiso 0.416(15) 1 calc PR A 2 C3A C 0.3635(14) 0.3409(12) 0.5325(12) 0.038(5) Uiso 0.416(15) 1 d P A 2 H3A1 H 0.3111 0.2937 0.5298 0.046 Uiso 0.416(15) 1 calc PR A 2 H3A2 H 0.4137 0.3113 0.5103 0.046 Uiso 0.416(15) 1 calc PR A 2 C4A C 0.3066(7) 0.4247(6) 0.4626(6) 0.057(2) Uani 0.416(15) 1 d P A 2 H4A1 H 0.3562 0.4543 0.4398 0.068 Uiso 0.416(15) 1 calc PR A 2 H4A2 H 0.2475 0.4001 0.4057 0.068 Uiso 0.416(15) 1 calc PR A 2 C5A C 0.1966(7) 0.5649(5) 0.4474(5) 0.0460(18) Uani 0.416(15) 1 d P A 2 H5A1 H 0.1734 0.5484 0.3787 0.055 Uiso 0.416(15) 1 calc PR A 2 H5A2 H 0.2289 0.6272 0.4587 0.055 Uiso 0.416(15) 1 calc PR A 2 C6A C 0.1029(14) 0.5593(13) 0.4812(12) 0.041(5) Uiso 0.416(15) 1 d P A 2 H6A1 H 0.0471 0.6031 0.4428 0.049 Uiso 0.416(15) 1 calc PR A 2 H6A2 H 0.0733 0.4959 0.47 0.049 Uiso 0.416(15) 1 calc PR A 2 C7A C 0.1381(5) 0.5816(5) 0.5797(5) 0.0412(17) Uani 0.416(15) 1 d P A 2 H7A1 H 0.0949 0.547 0.6064 0.049 Uiso 0.416(15) 1 calc PR A 2 H7A2 H 0.1255 0.6485 0.5851 0.049 Uiso 0.416(15) 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 Pt 0.03076(16) 0.01945(14) 0.04177(18) 0.00121(11) 0.01383(12) 0.00007(10) Cl1 0.0524(11) 0.0450(10) 0.0462(11) 0.0079(8) 0.0261(9) 0.0011(8) Cl2 0.0362(9) 0.0310(8) 0.0788(14) 0.0011(9) 0.0261(10) -0.0016(7) Cl3 0.0343(9) 0.0541(11) 0.0473(11) 0.0134(9) 0.0065(9) 0.0011(8) Cl4 0.0468(12) 0.0811(15) 0.0423(11) -0.0045(10) 0.0163(10) -0.0227(10) P 0.0298(8) 0.0189(7) 0.0306(9) 0.0001(6) 0.0113(7) 0.0017(6) N1 0.047(4) 0.028(3) 0.048(4) 0.005(3) 0.027(3) 0.011(3) N2 0.033(3) 0.026(3) 0.033(3) -0.005(2) 0.012(3) 0.004(2) N3 0.048(4) 0.037(3) 0.040(4) -0.011(3) 0.024(3) -0.003(3) N4 0.037(3) 0.022(3) 0.042(3) -0.006(2) 0.019(3) -0.005(2) N5 0.037(3) 0.021(3) 0.029(3) -0.005(2) 0.013(3) -0.001(2) N6 0.036(3) 0.029(3) 0.032(3) 0.000(2) 0.013(3) -0.001(2) C1 0.035(4) 0.022(3) 0.036(4) -0.005(3) 0.016(3) -0.006(3) C8 0.041(4) 0.023(3) 0.045(4) 0.003(3) 0.020(4) 0.006(3) C9 0.027(3) 0.028(3) 0.028(3) 0.003(3) 0.006(3) 0.003(3) C10 0.047(4) 0.028(3) 0.049(5) -0.011(3) 0.021(4) -0.012(3) C11 0.051(5) 0.027(3) 0.058(5) 0.006(3) 0.024(4) -0.003(3) C12 0.038(4) 0.043(4) 0.044(4) 0.009(3) 0.021(4) -0.004(3) C13 0.045(4) 0.037(4) 0.043(4) -0.004(3) 0.025(4) 0.002(3) C14 0.049(4) 0.036(4) 0.034(4) -0.004(3) 0.017(4) 0.007(3) C15 0.044(4) 0.026(3) 0.029(4) -0.003(3) 0.010(3) -0.001(3) C16 0.050(4) 0.021(3) 0.029(4) -0.003(3) 0.015(3) 0.005(3) C17 0.049(4) 0.029(3) 0.026(4) -0.001(3) 0.011(3) 0.002(3) C18 0.073(6) 0.023(3) 0.035(4) 0.002(3) 0.021(4) 0.009(4) C19 0.093(7) 0.029(4) 0.034(4) 0.006(3) 0.024(5) 0.026(4) C20 0.055(5) 0.052(5) 0.031(4) -0.001(3) 0.012(4) 0.027(4) C21 0.042(4) 0.035(4) 0.028(4) 0.000(3) 0.010(3) 0.008(3) C22 0.045(5) 0.076(6) 0.047(5) 0.012(5) 0.021(4) -0.003(4) C23 0.075(7) 0.100(8) 0.071(7) 0.000(6) 0.040(6) 0.029(6) N7 0.077(6) 0.063(5) 0.076(6) 0.002(4) 0.033(5) -0.009(4) C2 0.117(9) 0.063(6) 0.082(7) 0.023(5) 0.073(7) 0.051(6) C4 0.076(6) 0.053(5) 0.052(5) -0.013(4) 0.036(5) 0.006(4) C5 0.058(5) 0.043(4) 0.036(4) 0.001(3) 0.018(4) -0.002(4) C7 0.030(4) 0.050(4) 0.039(4) -0.003(3) 0.009(3) -0.003(3) C2A 0.117(9) 0.063(6) 0.082(7) 0.023(5) 0.073(7) 0.051(6) C4A 0.076(6) 0.053(5) 0.052(5) -0.013(4) 0.036(5) 0.006(4) C5A 0.058(5) 0.043(4) 0.036(4) 0.001(3) 0.018(4) -0.002(4) C7A 0.030(4) 0.050(4) 0.039(4) -0.003(3) 0.009(3) -0.003(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 Pt P 2.2006(17) . ? Pt Cl3 2.2961(19) . ? Pt Cl1 2.3067(19) . ? Pt Cl2 2.3525(18) . ? P N2 1.684(6) . ? P N5 1.738(5) . ? P C16 1.813(6) . ? N1 C1 1.321(8) . ? N1 C8 1.472(9) . ? N1 C2 1.474(9) . ? N2 C1 1.388(8) . ? N2 C7 1.488(9) . ? N3 C1 1.314(9) . ? N3 C5 1.461(10) . ? N3 C4 1.475(9) . ? N4 C9 1.350(8) . ? N4 C8 1.445(8) . ? N4 C10 1.485(8) . ? N5 C9 1.358(8) . ? N5 C15 1.484(8) . ? N6 C9 1.301(8) . ? N6 C13 1.476(8) . ? N6 C12 1.485(8) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C10 C11 1.485(10) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C11 C12 1.508(10) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.503(10) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 C15 1.508(10) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 C21 1.390(10) . ? C16 C17 1.407(9) . ? C17 C18 1.382(10) . ? C17 H17 0.95 . ? C18 C19 1.364(12) . ? C18 H18 0.95 . ? C19 C20 1.368(13) . ? C19 H19 0.95 . ? C20 C21 1.403(10) . ? C20 H20 0.95 . ? C21 H21 0.95 . ? C22 N7 1.169(12) . ? C22 C23 1.422(14) . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C2 C3 1.452(17) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 C4 1.429(17) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 C6 1.458(15) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 C7 1.501(16) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C3A H3A1 0.99 . ? C3A H3A2 0.99 . ? C6A H6A1 0.99 . ? C6A H6A2 0.99 . ? 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 P Pt Cl3 93.72(6) . . ? P Pt Cl1 89.58(7) . . ? Cl3 Pt Cl1 176.58(7) . . ? P Pt Cl2 177.12(6) . . ? Cl3 Pt Cl2 88.12(7) . . ? Cl1 Pt Cl2 88.62(7) . . ? N2 P N5 104.7(3) . . ? N2 P C16 105.5(3) . . ? N5 P C16 101.3(3) . . ? N2 P Pt 113.61(19) . . ? N5 P Pt 115.5(2) . . ? C16 P Pt 114.8(2) . . ? C1 N1 C8 124.1(5) . . ? C1 N1 C2 118.9(6) . . ? C8 N1 C2 117.0(6) . . ? C1 N2 C7 113.8(5) . . ? C1 N2 P 119.8(5) . . ? C7 N2 P 125.6(4) . . ? C1 N3 C5 121.7(6) . . ? C1 N3 C4 121.9(6) . . ? C5 N3 C4 116.4(6) . . ? C9 N4 C8 119.9(5) . . ? C9 N4 C10 116.7(5) . . ? C8 N4 C10 118.8(5) . . ? C9 N5 C15 115.5(5) . . ? C9 N5 P 125.9(4) . . ? C15 N5 P 118.6(4) . . ? C9 N6 C13 124.9(6) . . ? C9 N6 C12 123.6(6) . . ? C13 N6 C12 111.5(5) . . ? N3 C1 N1 122.4(6) . . ? N3 C1 N2 117.7(6) . . ? N1 C1 N2 119.7(6) . . ? N4 C8 N1 114.5(6) . . ? N4 C8 H8A 108.6 . . ? N1 C8 H8A 108.6 . . ? N4 C8 H8B 108.6 . . ? N1 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? N6 C9 N4 120.3(6) . . ? N6 C9 N5 120.7(6) . . ? N4 C9 N5 118.9(5) . . ? C11 C10 N4 107.4(6) . . ? C11 C10 H10A 110.2 . . ? N4 C10 H10A 110.2 . . ? C11 C10 H10B 110.2 . . ? N4 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? C10 C11 C12 108.7(6) . . ? C10 C11 H11A 109.9 . . ? C12 C11 H11A 109.9 . . ? C10 C11 H11B 109.9 . . ? C12 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? N6 C12 C11 113.0(5) . . ? N6 C12 H12A 109 . . ? C11 C12 H12A 109 . . ? N6 C12 H12B 109 . . ? C11 C12 H12B 109 . . ? H12A C12 H12B 107.8 . . ? N6 C13 C14 112.8(5) . . ? N6 C13 H13A 109 . . ? C14 C13 H13A 109 . . ? N6 C13 H13B 109 . . ? C14 C13 H13B 109 . . ? H13A C13 H13B 107.8 . . ? C13 C14 C15 109.5(6) . . ? C13 C14 H14A 109.8 . . ? C15 C14 H14A 109.8 . . ? C13 C14 H14B 109.8 . . ? C15 C14 H14B 109.8 . . ? H14A C14 H14B 108.2 . . ? N5 C15 C14 109.0(6) . . ? N5 C15 H15A 109.9 . . ? C14 C15 H15A 109.9 . . ? N5 C15 H15B 109.9 . . ? C14 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? C21 C16 C17 119.9(6) . . ? C21 C16 P 122.1(5) . . ? C17 C16 P 117.9(5) . . ? C18 C17 C16 119.8(7) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C19 C18 C17 120.1(7) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 120.9(7) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C19 C20 C21 120.8(8) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C16 C21 C20 118.4(7) . . ? C16 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? N7 C22 C23 176.0(11) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C3 C2 N1 113.8(9) . . ? C3 C2 H2A 108.8 . . ? N1 C2 H2A 108.8 . . ? C3 C2 H2B 108.8 . . ? N1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C4 C3 C2 114.6(11) . . ? C4 C3 H3A 108.6 . . ? C2 C3 H3A 108.6 . . ? C4 C3 H3B 108.6 . . ? C2 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? C3 C4 N3 108.2(9) . . ? C3 C4 H4A 110.1 . . ? N3 C4 H4A 110.1 . . ? C3 C4 H4B 110.1 . . ? N3 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? C6 C5 N3 117.4(8) . . ? C6 C5 H5A 108 . . ? N3 C5 H5A 108 . . ? C6 C5 H5B 108 . . ? N3 C5 H5B 108 . . ? H5A C5 H5B 107.2 . . ? C5 C6 C7 113.4(10) . . ? C5 C6 H6A 108.9 . . ? C7 C6 H6A 108.9 . . ? C5 C6 H6B 108.9 . . ? C7 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? N2 C7 C6 106.1(8) . . ? N2 C7 H7A 110.5 . . ? C6 C7 H7A 110.5 . . ? N2 C7 H7B 110.5 . . ? C6 C7 H7B 110.5 . . ? H7A C7 H7B 108.7 . . ? H3A1 C3A H3A2 108 . . ? H6A1 C6A H6A2 108.1 . . ? #===END