Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Martyn Paul Coles' 'Peter B. Hitchcock' 'Sarah H. Oakley' 'Delia B. Soria' _publ_contact_author_name 'Dr Martyn Paul Coles' _publ_contact_author_address ; Department of Chemistry University of Sussex Falmer Brighton BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email M.P.COLES@SUSSEX.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Structural Diversity in the Coordination of Amidines and Guanidines to Monovalent Metal Halides ; _publ_requested_category FM data_(1)-may301 _database_code_depnum_ccdc_archive 'CCDC 224306' _audit_creation_date 2001-04-30T15:21:18-00:00 _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 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common [{CuCl(PhNCPhNHPh)}2] _chemical_formula_moiety 'C76 H64 Cl2 Cu2 N8' _chemical_formula_sum 'C76 H64 Cl2 Cu2 N8' _chemical_formula_weight 1287.33 _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 10.7522(4) _cell_length_b 11.9924(6) _cell_length_c 13.9711(8) _cell_angle_alpha 112.261(2) _cell_angle_beta 107.954(3) _cell_angle_gamma 92.424(3) _cell_volume 1559.94(13) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6854 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.878 _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 1.37 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.82 _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 0.841 _exptl_absorpt_correction_T_max 0.898 #----------------------------------------------------------------------------# # 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 12659 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_unetI/netI 0.0829 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 27.84 _diffrn_reflns_theta_full 27.84 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 7363 _reflns_number_gt 5217 _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 ; 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^)+(0.0461P)^2^+0.4421P] 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 'H on N atoms freely refined; others riding' _refine_ls_extinction_method none _refine_ls_number_reflns 7363 _refine_ls_number_parameters 405 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.051 _refine_ls_wR_factor_ref 0.1231 _refine_ls_wR_factor_gt 0.1099 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.595 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.106 #----------------------------------------------------------------------------# # 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' Cu Cu 0.3201 1.2651 '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' 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 Cu Cu -0.03885(3) 0.07362(3) 0.08487(3) 0.02764(12) Uani 1 1 d . . . Cl Cl 0.03089(6) 0.13139(6) -0.04682(6) 0.02570(16) Uani 1 1 d . . . N1 N -0.21665(19) 0.12440(19) 0.09182(18) 0.0223(5) Uani 1 1 d . . . N2 N -0.2654(2) 0.1786(2) -0.0521(2) 0.0291(5) Uani 1 1 d . . . H2A H -0.194(3) 0.159(2) -0.060(2) 0.024(7) Uiso 1 1 d . . . N3 N 0.1038(2) 0.1912(2) 0.23246(19) 0.0249(5) Uani 1 1 d . . . N4 N 0.0563(2) 0.3557(2) 0.1938(2) 0.0273(5) Uani 1 1 d . . . H4A H 0.028(3) 0.305(3) 0.129(3) 0.032(9) Uiso 1 1 d . . . C1 C -0.2907(2) 0.1786(2) 0.0366(2) 0.0225(6) Uani 1 1 d . . . C2 C -0.2218(2) 0.1348(2) 0.1957(2) 0.0237(6) Uani 1 1 d . . . C3 C -0.2505(3) 0.0288(3) 0.2100(3) 0.0315(7) Uani 1 1 d . . . H3 H -0.2739 -0.0489 0.1492 0.038 Uiso 1 1 calc R . . C4 C -0.2450(3) 0.0370(3) 0.3126(3) 0.0402(8) Uani 1 1 d . . . H4 H -0.2669 -0.0352 0.3214 0.048 Uiso 1 1 calc R . . C5 C -0.2079(3) 0.1490(3) 0.4027(3) 0.0401(8) Uani 1 1 d . . . H5 H -0.2038 0.154 0.4731 0.048 Uiso 1 1 calc R . . C6 C -0.1769(3) 0.2532(3) 0.3891(2) 0.0349(7) Uani 1 1 d . . . H6 H -0.1501 0.3304 0.4508 0.042 Uiso 1 1 calc R . . C7 C -0.1845(3) 0.2469(3) 0.2864(2) 0.0285(6) Uani 1 1 d . . . H7 H -0.164 0.3198 0.278 0.034 Uiso 1 1 calc R . . C8 C -0.3982(2) 0.2429(2) 0.0671(2) 0.0245(6) Uani 1 1 d . . . C9 C -0.3957(3) 0.3643(3) 0.0839(2) 0.0337(7) Uani 1 1 d . . . H9 H -0.3228 0.4086 0.0808 0.04 Uiso 1 1 calc R . . C10 C -0.4996(3) 0.4215(3) 0.1054(3) 0.0451(8) Uani 1 1 d . . . H10 H -0.4972 0.5052 0.1176 0.054 Uiso 1 1 calc R . . C11 C -0.6062(3) 0.3576(4) 0.1091(3) 0.0479(9) Uani 1 1 d . . . H11 H -0.678 0.3967 0.1221 0.057 Uiso 1 1 calc R . . C12 C -0.6088(3) 0.2370(3) 0.0939(3) 0.0416(8) Uani 1 1 d . . . H12 H -0.682 0.1931 0.097 0.05 Uiso 1 1 calc R . . C13 C -0.5043(3) 0.1798(3) 0.0741(2) 0.0310(6) Uani 1 1 d . . . H13 H -0.5051 0.0972 0.0653 0.037 Uiso 1 1 calc R . . C14 C -0.3335(2) 0.2156(2) -0.1363(2) 0.0254(6) Uani 1 1 d . . . C15 C -0.4700(3) 0.2097(3) -0.1743(2) 0.0311(6) Uani 1 1 d . . . H15 H -0.5239 0.1815 -0.1425 0.037 Uiso 1 1 calc R . . C16 C -0.5271(3) 0.2457(3) -0.2594(3) 0.0364(7) Uani 1 1 d . . . H16 H -0.6205 0.2429 -0.2848 0.044 Uiso 1 1 calc R . . C17 C -0.4507(3) 0.2853(3) -0.3075(3) 0.0382(7) Uani 1 1 d . . . H17 H -0.4909 0.3098 -0.3654 0.046 Uiso 1 1 calc R . . C18 C -0.3148(3) 0.2887(3) -0.2705(3) 0.0379(7) Uani 1 1 d . . . H18 H -0.2612 0.3147 -0.3037 0.045 Uiso 1 1 calc R . . C19 C -0.2571(3) 0.2545(3) -0.1855(2) 0.0314(6) Uani 1 1 d . . . H19 H -0.1637 0.2577 -0.1603 0.038 Uiso 1 1 calc R . . C20 C 0.1188(2) 0.3100(2) 0.2688(2) 0.0238(6) Uani 1 1 d . . . C21 C 0.1832(3) 0.1365(2) 0.2988(2) 0.0274(6) Uani 1 1 d . . . C22 C 0.1211(3) 0.0700(3) 0.3390(3) 0.0407(8) Uani 1 1 d . . . H22 H 0.0278 0.062 0.3227 0.049 Uiso 1 1 calc R . . C23 C 0.1949(3) 0.0157(3) 0.4023(3) 0.0554(10) Uani 1 1 d . . . H23 H 0.1522 -0.0279 0.4312 0.067 Uiso 1 1 calc R . . C24 C 0.3290(3) 0.0233(3) 0.4245(3) 0.0549(10) Uani 1 1 d . . . H24 H 0.3792 -0.0141 0.4688 0.066 Uiso 1 1 calc R . . C25 C 0.3903(3) 0.0863(3) 0.3815(3) 0.0473(9) Uani 1 1 d . . . H25 H 0.4828 0.0901 0.3947 0.057 Uiso 1 1 calc R . . C26 C 0.3183(3) 0.1439(3) 0.3194(3) 0.0368(7) Uani 1 1 d . . . H26 H 0.3613 0.1883 0.2911 0.044 Uiso 1 1 calc R . . C27 C 0.2048(2) 0.3968(2) 0.3823(2) 0.0248(6) Uani 1 1 d . . . C28 C 0.1974(3) 0.3840(3) 0.4750(2) 0.0297(6) Uani 1 1 d . . . H28 H 0.133 0.321 0.4667 0.036 Uiso 1 1 calc R . . C29 C 0.2828(3) 0.4620(3) 0.5798(2) 0.0343(7) Uani 1 1 d . . . H29 H 0.278 0.4518 0.6429 0.041 Uiso 1 1 calc R . . C30 C 0.3753(3) 0.5550(3) 0.5919(3) 0.0366(7) Uani 1 1 d . . . H30 H 0.4346 0.6082 0.6634 0.044 Uiso 1 1 calc R . . C31 C 0.3815(3) 0.5707(3) 0.5008(3) 0.0340(7) Uani 1 1 d . . . H31 H 0.4438 0.6358 0.5099 0.041 Uiso 1 1 calc R . . C32 C 0.2974(3) 0.4918(2) 0.3958(2) 0.0301(6) Uani 1 1 d . . . H32 H 0.3028 0.5024 0.333 0.036 Uiso 1 1 calc R . . C33 C 0.0063(2) 0.4655(2) 0.2083(2) 0.0247(6) Uani 1 1 d . . . C34 C -0.0383(3) 0.4925(3) 0.1161(3) 0.0320(7) Uani 1 1 d . . . H34 H -0.0337 0.438 0.0476 0.038 Uiso 1 1 calc R . . C35 C -0.0891(3) 0.5985(3) 0.1238(3) 0.0387(8) Uani 1 1 d . . . H35 H -0.12 0.6154 0.0602 0.046 Uiso 1 1 calc R . . C36 C -0.0955(3) 0.6795(3) 0.2219(3) 0.0402(8) Uani 1 1 d . . . H36 H -0.1278 0.7533 0.2272 0.048 Uiso 1 1 calc R . . C37 C -0.0545(3) 0.6520(3) 0.3122(3) 0.0376(7) Uani 1 1 d . . . H37 H -0.06 0.707 0.3801 0.045 Uiso 1 1 calc R . . C38 C -0.0052(3) 0.5455(2) 0.3065(2) 0.0308(6) Uani 1 1 d . . . H38 H 0.0207 0.5273 0.3696 0.037 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 Cu 0.02721(18) 0.02530(19) 0.0268(2) 0.00923(15) 0.00616(14) 0.00795(13) Cl 0.0251(3) 0.0228(3) 0.0303(4) 0.0108(3) 0.0110(3) 0.0064(2) N1 0.0221(10) 0.0229(11) 0.0209(12) 0.0098(9) 0.0052(9) 0.0043(8) N2 0.0247(12) 0.0432(15) 0.0278(14) 0.0204(12) 0.0119(10) 0.0143(10) N3 0.0247(11) 0.0240(12) 0.0255(13) 0.0134(10) 0.0039(9) 0.0043(8) N4 0.0369(13) 0.0213(12) 0.0181(13) 0.0069(10) 0.0038(10) 0.0049(9) C1 0.0201(12) 0.0218(13) 0.0216(14) 0.0072(11) 0.0042(10) 0.0012(9) C2 0.0184(12) 0.0292(15) 0.0247(15) 0.0132(12) 0.0063(10) 0.0068(10) C3 0.0326(15) 0.0277(15) 0.0330(17) 0.0159(13) 0.0064(12) -0.0007(11) C4 0.0426(17) 0.0416(19) 0.041(2) 0.0250(16) 0.0115(14) -0.0016(13) C5 0.0415(17) 0.053(2) 0.0327(18) 0.0243(16) 0.0144(14) 0.0083(14) C6 0.0402(16) 0.0383(17) 0.0245(16) 0.0117(14) 0.0103(13) 0.0104(13) C7 0.0333(14) 0.0264(15) 0.0272(16) 0.0120(12) 0.0110(12) 0.0076(11) C8 0.0202(12) 0.0279(14) 0.0210(14) 0.0077(11) 0.0043(10) 0.0058(10) C9 0.0368(15) 0.0324(17) 0.0322(17) 0.0140(14) 0.0110(13) 0.0096(12) C10 0.055(2) 0.0393(19) 0.039(2) 0.0153(16) 0.0138(16) 0.0256(15) C11 0.0365(17) 0.075(3) 0.0327(19) 0.0200(18) 0.0124(14) 0.0339(17) C12 0.0218(14) 0.071(2) 0.0252(17) 0.0134(16) 0.0075(12) 0.0098(14) C13 0.0257(14) 0.0390(17) 0.0243(15) 0.0119(13) 0.0055(11) 0.0028(11) C14 0.0275(13) 0.0252(14) 0.0215(14) 0.0102(12) 0.0051(11) 0.0050(10) C15 0.0279(14) 0.0348(16) 0.0300(16) 0.0161(13) 0.0066(12) -0.0004(11) C16 0.0280(14) 0.0421(18) 0.0390(19) 0.0238(15) 0.0028(13) 0.0069(12) C17 0.0485(18) 0.0367(18) 0.0322(18) 0.0209(15) 0.0087(14) 0.0134(13) C18 0.0465(18) 0.0404(18) 0.0409(19) 0.0254(15) 0.0224(15) 0.0117(13) C19 0.0300(14) 0.0379(17) 0.0312(17) 0.0182(14) 0.0119(12) 0.0094(12) C20 0.0240(12) 0.0269(14) 0.0223(14) 0.0124(12) 0.0076(10) 0.0051(10) C21 0.0306(14) 0.0195(13) 0.0236(15) 0.0072(11) 0.0003(11) 0.0049(10) C22 0.0339(16) 0.0431(19) 0.043(2) 0.0265(16) 0.0001(13) 0.0003(13) C23 0.055(2) 0.052(2) 0.059(3) 0.040(2) -0.0005(18) -0.0011(16) C24 0.054(2) 0.044(2) 0.052(2) 0.0274(19) -0.0104(17) 0.0134(16) C25 0.0330(16) 0.052(2) 0.048(2) 0.0207(18) 0.0004(14) 0.0146(14) C26 0.0312(15) 0.0354(17) 0.0376(19) 0.0136(14) 0.0055(13) 0.0084(12) C27 0.0268(13) 0.0203(13) 0.0236(15) 0.0074(11) 0.0060(11) 0.0062(10) C28 0.0330(14) 0.0287(15) 0.0237(15) 0.0105(12) 0.0059(12) 0.0032(11) C29 0.0426(16) 0.0368(17) 0.0235(16) 0.0125(13) 0.0108(13) 0.0136(13) C30 0.0292(15) 0.0368(17) 0.0273(17) 0.0025(13) 0.0019(12) 0.0052(12) C31 0.0284(14) 0.0325(16) 0.0325(18) 0.0089(14) 0.0058(12) 0.0010(11) C32 0.0320(14) 0.0284(15) 0.0292(16) 0.0119(13) 0.0097(12) 0.0059(11) C33 0.0222(12) 0.0233(14) 0.0271(15) 0.0121(12) 0.0049(11) 0.0012(10) C34 0.0325(14) 0.0351(16) 0.0340(17) 0.0198(14) 0.0119(12) 0.0072(12) C35 0.0391(16) 0.0463(19) 0.046(2) 0.0339(17) 0.0150(14) 0.0174(14) C36 0.0397(17) 0.0340(17) 0.061(2) 0.0300(17) 0.0213(16) 0.0160(13) C37 0.0433(17) 0.0282(16) 0.0406(19) 0.0098(14) 0.0189(14) 0.0115(12) C38 0.0343(15) 0.0271(15) 0.0293(16) 0.0135(13) 0.0066(12) 0.0061(11) #----------------------------------------------------------------------------# # 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 Cu N1 2.050(2) . ? Cu N3 2.063(2) . ? Cu Cl 2.3217(7) 2 ? Cu Cl 2.4900(8) . ? Cu Cu 2.7592(7) 2 ? Cl Cu 2.3217(7) 2 ? N1 C1 1.302(3) . ? N1 C2 1.428(3) . ? N2 C1 1.348(4) . ? N2 C14 1.418(3) . ? N3 C20 1.302(3) . ? N3 C21 1.428(3) . ? N4 C20 1.372(3) . ? N4 C33 1.410(3) . ? C1 C8 1.498(3) . ? C2 C7 1.388(4) . ? C2 C3 1.395(4) . ? C3 C4 1.382(4) . ? C4 C5 1.383(5) . ? C5 C6 1.376(4) . ? C6 C7 1.383(4) . ? C8 C9 1.382(4) . ? C8 C13 1.391(4) . ? C9 C10 1.388(4) . ? C10 C11 1.376(5) . ? C11 C12 1.379(5) . ? C12 C13 1.386(4) . ? C14 C15 1.387(4) . ? C14 C19 1.387(4) . ? C15 C16 1.392(4) . ? C16 C17 1.379(4) . ? C17 C18 1.385(4) . ? C18 C19 1.378(4) . ? C20 C27 1.489(4) . ? C21 C26 1.383(4) . ? C21 C22 1.387(4) . ? C22 C23 1.371(4) . ? C23 C24 1.369(5) . ? C24 C25 1.382(5) . ? C25 C26 1.384(4) . ? C27 C28 1.386(4) . ? C27 C32 1.397(4) . ? C28 C29 1.387(4) . ? C29 C30 1.386(4) . ? C30 C31 1.375(4) . ? C31 C32 1.387(4) . ? C33 C38 1.391(4) . ? C33 C34 1.395(4) . ? C34 C35 1.384(4) . ? C35 C36 1.372(5) . ? C36 C37 1.370(4) . ? C37 C38 1.387(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 Cu N3 105.88(9) . . ? N1 Cu Cl 115.06(6) . 2 ? N3 Cu Cl 113.04(6) . 2 ? N1 Cu Cl 111.38(6) . . ? N3 Cu Cl 100.34(7) . . ? Cl Cu Cl 110.12(2) 2 . ? N1 Cu Cu 133.27(6) . 2 ? N3 Cu Cu 119.43(7) . 2 ? Cl Cu Cu 57.93(2) 2 2 ? Cl Cu Cu 52.194(19) . 2 ? Cu Cl Cu 69.88(2) 2 . ? C1 N1 C2 121.3(2) . . ? C1 N1 Cu 127.87(18) . . ? C2 N1 Cu 106.91(15) . . ? C1 N2 C14 132.1(2) . . ? C20 N3 C21 119.9(2) . . ? C20 N3 Cu 123.29(17) . . ? C21 N3 Cu 116.72(16) . . ? C20 N4 C33 131.0(3) . . ? N1 C1 N2 117.0(2) . . ? N1 C1 C8 124.3(2) . . ? N2 C1 C8 118.6(2) . . ? C7 C2 C3 118.9(3) . . ? C7 C2 N1 121.3(2) . . ? C3 C2 N1 119.4(2) . . ? C4 C3 C2 119.9(3) . . ? C3 C4 C5 120.9(3) . . ? C6 C5 C4 119.1(3) . . ? C5 C6 C7 120.7(3) . . ? C6 C7 C2 120.4(3) . . ? C9 C8 C13 119.4(2) . . ? C9 C8 C1 120.1(2) . . ? C13 C8 C1 120.4(2) . . ? C8 C9 C10 120.0(3) . . ? C11 C10 C9 120.3(3) . . ? C10 C11 C12 120.1(3) . . ? C11 C12 C13 119.9(3) . . ? C12 C13 C8 120.2(3) . . ? C15 C14 C19 119.4(3) . . ? C15 C14 N2 123.9(3) . . ? C19 C14 N2 116.6(2) . . ? C14 C15 C16 119.3(3) . . ? C17 C16 C15 121.2(3) . . ? C16 C17 C18 119.2(3) . . ? C19 C18 C17 120.0(3) . . ? C18 C19 C14 120.9(3) . . ? N3 C20 N4 116.4(2) . . ? N3 C20 C27 124.4(2) . . ? N4 C20 C27 119.1(2) . . ? C26 C21 C22 119.8(3) . . ? C26 C21 N3 121.6(3) . . ? C22 C21 N3 118.6(2) . . ? C23 C22 C21 119.8(3) . . ? C24 C23 C22 121.2(3) . . ? C23 C24 C25 119.1(3) . . ? C24 C25 C26 120.7(3) . . ? C21 C26 C25 119.4(3) . . ? C28 C27 C32 119.1(2) . . ? C28 C27 C20 121.6(2) . . ? C32 C27 C20 119.3(3) . . ? C27 C28 C29 120.8(3) . . ? C30 C29 C28 119.5(3) . . ? C31 C30 C29 120.4(3) . . ? C30 C31 C32 120.3(3) . . ? C31 C32 C27 119.9(3) . . ? C38 C33 C34 118.4(3) . . ? C38 C33 N4 124.6(3) . . ? C34 C33 N4 117.0(3) . . ? C35 C34 C33 120.3(3) . . ? C36 C35 C34 121.1(3) . . ? C37 C36 C35 118.8(3) . . ? C36 C37 C38 121.4(3) . . ? C37 C38 C33 120.0(3) . . ? #===END data_(3)-jan1003 _database_code_depnum_ccdc_archive 'CCDC 224307' _audit_creation_date 2003-01-16T15:45:57-00:00 _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 [{CuI(N(iPr)C(NHiPr)NMe2)}2] _chemical_formula_moiety 'C18 H42 Cu2 I2 N6' _chemical_formula_sum 'C18 H42 Cu2 I2 N6' _chemical_formula_weight 723.46 _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 8.2768(2) _cell_length_b 8.8985(2) _cell_length_c 10.8561(3) _cell_angle_alpha 107.040(10) _cell_angle_beta 95.260(1) _cell_angle_gamma 112.759(1) _cell_volume 685.61(3) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4253 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 30.034 _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 0.1 _exptl_crystal_density_diffrn 1.752 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 356 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.817 _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 0.4245 _exptl_absorpt_correction_T_max 0.5115 #----------------------------------------------------------------------------# # 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 0.048 _diffrn_reflns_av_unetI/netI 0.0429 _diffrn_reflns_number 6652 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.87 _diffrn_reflns_theta_max 30.05 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.959 _diffrn_measured_fraction_theta_max 0.959 _reflns_number_total 3871 _reflns_number_gt 3643 _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^)+(0.0298P)^2^+0.5818P] 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 'H on N3 refined; others riding' _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.043(4) _refine_ls_number_reflns 3871 _refine_ls_number_parameters 132 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0851 _refine_ls_wR_factor_gt 0.0838 _refine_ls_goodness_of_fit_ref 1.179 _refine_ls_restrained_S_all 1.179 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.268 _refine_diff_density_min -0.978 _refine_diff_density_rms 0.116 #----------------------------------------------------------------------------# # 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 Cu Cu -0.01849(5) 0.12382(4) 0.08242(3) 0.02934(10) Uani 1 1 d . . . I I -0.16970(2) -0.17779(2) 0.097233(18) 0.03154(10) Uani 1 1 d . . . N1 N -0.0258(3) 0.3432(3) 0.1918(2) 0.0256(4) Uani 1 1 d . . . N2 N 0.2782(3) 0.4878(3) 0.3018(2) 0.0273(4) Uani 1 1 d . . . N3 N 0.1312(3) 0.6525(3) 0.2685(2) 0.0266(4) Uani 1 1 d . . . H3 H 0.039(5) 0.655(4) 0.218(3) 0.023(8) Uiso 1 1 d . . . C1 C 0.1192(3) 0.4888(3) 0.2512(2) 0.0228(4) Uani 1 1 d . . . C2 C -0.2026(4) 0.3468(3) 0.1670(3) 0.0283(5) Uani 1 1 d . . . H2 H -0.1885 0.4657 0.2201 0.034 Uiso 1 1 calc R . . C3 C -0.2650(5) 0.3135(6) 0.0235(4) 0.0535(9) Uani 1 1 d . . . H3A H -0.175 0.401 -0.0025 0.08 Uiso 1 1 calc R . . H3B H -0.38 0.3209 0.0093 0.08 Uiso 1 1 calc R . . H3C H -0.2809 0.1968 -0.0302 0.08 Uiso 1 1 calc R . . C4 C -0.3366(6) 0.2156(6) 0.2133(6) 0.0629(13) Uani 1 1 d . . . H4A H -0.2912 0.2419 0.3074 0.094 Uiso 1 1 calc R . . H4B H -0.3532 0.0979 0.1617 0.094 Uiso 1 1 calc R . . H4C H -0.4522 0.222 0.2008 0.094 Uiso 1 1 calc R . . C5 C 0.2741(4) 0.3318(4) 0.3203(3) 0.0309(5) Uani 1 1 d . . . H5A H 0.3968 0.3518 0.356 0.046 Uiso 1 1 calc R . . H5B H 0.2237 0.2345 0.235 0.046 Uiso 1 1 calc R . . H5C H 0.1991 0.3034 0.3825 0.046 Uiso 1 1 calc R . . C6 C 0.4460(4) 0.5927(4) 0.2741(3) 0.0343(6) Uani 1 1 d . . . H6A H 0.5451 0.577 0.3163 0.051 Uiso 1 1 calc R . . H6B H 0.4702 0.7161 0.3092 0.051 Uiso 1 1 calc R . . H6C H 0.4352 0.5556 0.1782 0.051 Uiso 1 1 calc R . . C7 C 0.2126(4) 0.7967(3) 0.3965(3) 0.0325(5) Uani 1 1 d . . . H7 H 0.308 0.7798 0.4463 0.039 Uiso 1 1 calc R . . C8 C 0.0714(7) 0.7966(6) 0.4775(4) 0.0586(10) Uani 1 1 d . . . H8A H 0.0184 0.6848 0.4908 0.088 Uiso 1 1 calc R . . H8B H -0.0232 0.8131 0.4301 0.088 Uiso 1 1 calc R . . H8C H 0.1284 0.8917 0.5637 0.088 Uiso 1 1 calc R . . C9 C 0.3008(6) 0.9669(4) 0.3732(5) 0.0594(11) Uani 1 1 d . . . H9A H 0.3906 0.9617 0.3212 0.089 Uiso 1 1 calc R . . H9B H 0.36 1.0633 0.4586 0.089 Uiso 1 1 calc R . . H9C H 0.209 0.9858 0.3247 0.089 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 Cu 0.02940(18) 0.02068(16) 0.03512(19) 0.00349(13) 0.00642(13) 0.01304(13) I 0.03193(12) 0.02649(12) 0.03932(13) 0.01480(8) 0.01336(8) 0.01247(8) N1 0.0251(10) 0.0219(9) 0.0308(10) 0.0066(8) 0.0090(8) 0.0129(8) N2 0.0272(10) 0.0227(9) 0.0342(11) 0.0103(8) 0.0075(8) 0.0128(8) N3 0.0344(11) 0.0203(9) 0.0263(10) 0.0069(8) 0.0047(8) 0.0144(8) C1 0.0273(11) 0.0206(10) 0.0236(10) 0.0079(8) 0.0093(8) 0.0127(9) C2 0.0256(11) 0.0251(11) 0.0371(13) 0.0101(10) 0.0107(10) 0.0140(9) C3 0.0451(19) 0.080(3) 0.0421(18) 0.0176(18) 0.0068(15) 0.0370(19) C4 0.048(2) 0.075(3) 0.112(4) 0.065(3) 0.052(2) 0.043(2) C5 0.0336(13) 0.0284(12) 0.0366(13) 0.0127(10) 0.0069(10) 0.0187(10) C6 0.0244(12) 0.0327(13) 0.0437(15) 0.0137(12) 0.0087(11) 0.0099(10) C7 0.0424(15) 0.0222(11) 0.0295(12) 0.0043(10) 0.0002(11) 0.0159(11) C8 0.073(3) 0.066(2) 0.0411(18) 0.0043(17) 0.0180(18) 0.044(2) C9 0.064(2) 0.0217(13) 0.070(3) 0.0129(15) -0.015(2) 0.0057(14) #----------------------------------------------------------------------------# # 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 Cu N1 1.993(2) . ? Cu Cu 2.5423(6) 2 ? Cu I 2.5469(4) . ? Cu I 2.6434(4) 2 ? I Cu 2.6434(4) 2 ? N1 C1 1.304(3) . ? N1 C2 1.478(3) . ? N2 C1 1.383(3) . ? N2 C5 1.448(3) . ? N2 C6 1.458(4) . ? N3 C1 1.375(3) . ? N3 C7 1.465(3) . ? C2 C3 1.499(5) . ? C2 C4 1.513(4) . ? C7 C9 1.514(4) . ? C7 C8 1.525(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 Cu Cu 169.48(7) . 2 ? N1 Cu I 127.82(7) . . ? Cu Cu I 62.587(14) 2 . ? N1 Cu I 110.78(7) . 2 ? Cu Cu I 58.791(14) 2 2 ? I Cu I 121.378(12) . 2 ? Cu I Cu 58.622(12) . 2 ? C1 N1 C2 119.8(2) . . ? C1 N1 Cu 122.63(17) . . ? C2 N1 Cu 114.86(16) . . ? C1 N2 C5 119.5(2) . . ? C1 N2 C6 119.7(2) . . ? C5 N2 C6 113.7(2) . . ? C1 N3 C7 122.4(2) . . ? N1 C1 N3 125.0(2) . . ? N1 C1 N2 120.7(2) . . ? N3 C1 N2 114.3(2) . . ? N1 C2 C3 110.4(2) . . ? N1 C2 C4 109.5(2) . . ? C3 C2 C4 112.0(3) . . ? N3 C7 C9 109.1(3) . . ? N3 C7 C8 110.4(3) . . ? C9 C7 C8 112.1(3) . . ? #===END data_(4)-oct1300 _database_code_depnum_ccdc_archive 'CCDC 224308' _audit_creation_date 2000-10-09T09:39:21-00:00 _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 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C28 H52 Cl2 Li2 N12' _chemical_formula_structural 'C28 H52 Cl2 Li2 N12' _chemical_formula_sum 'C28 H52 Cl2 Li2 N12' _chemical_formula_weight 641.6 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 8.8979(7) _cell_length_b 19.2720(19) _cell_length_c 10.7363(8) _cell_angle_alpha 90 _cell_angle_beta 113.465(5) _cell_angle_gamma 90 _cell_volume 1688.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 16664 _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 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.231 #----------------------------------------------------------------------------# # 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 8057 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_unetI/netI 0.0657 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.79 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _reflns_number_total 2934 _reflns_number_gt 2242 _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 ; H atoms on nitrogen were refined; other H atoms were in riding mode. 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^)+(0.0436P)^2^+1.1539P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 2934 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0837 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1459 _refine_ls_wR_factor_gt 0.1364 _refine_ls_goodness_of_fit_ref 1.209 _refine_ls_restrained_S_all 1.209 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.023 _refine_diff_density_min -0.447 _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' 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' Li Li -0.0003 0.0001 '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 Li Li 0.1262(6) 0.5570(3) 0.0701(5) 0.0345(12) Uani 1 1 d . . . Cl Cl 0.05087(8) 0.45761(4) 0.16682(7) 0.0307(2) Uani 1 1 d . . . N1 N 0.4528(3) 0.48496(16) 0.2999(3) 0.0399(7) Uani 1 1 d . . . H1 H 0.349(5) 0.474(2) 0.265(4) 0.06 Uiso 1 1 d . . . N2 N 0.3694(3) 0.55378(14) 0.1120(2) 0.0354(7) Uani 1 1 d . . . N3 N 0.6534(3) 0.54093(14) 0.2475(2) 0.0315(6) Uani 1 1 d . . . N4 N -0.1366(3) 0.68816(15) -0.0422(3) 0.0381(7) Uani 1 1 d . . . H4 H -0.128(4) 0.649(2) -0.079(4) 0.057 Uiso 1 1 d . . . N5 N 0.0966(3) 0.65367(15) 0.1338(2) 0.0376(7) Uani 1 1 d . . . N6 N -0.0087(3) 0.76717(15) 0.1328(3) 0.0391(7) Uani 1 1 d . . . C1 C 0.4908(3) 0.52753(16) 0.2135(3) 0.0289(7) Uani 1 1 d . . . C2 C 0.5687(4) 0.4366(2) 0.3912(3) 0.0439(9) Uani 1 1 d . . . H2B H 0.577 0.3949 0.3406 0.066 Uiso 1 1 calc R . . H2A H 0.5315 0.4219 0.4626 0.066 Uiso 1 1 calc R . . C3 C 0.7336(4) 0.4716(2) 0.4550(3) 0.0481(10) Uani 1 1 d . . . H3B H 0.7279 0.5102 0.5137 0.072 Uiso 1 1 calc R . . H3A H 0.8165 0.4379 0.5121 0.072 Uiso 1 1 calc R . . C4 C 0.7822(4) 0.4989(2) 0.3458(3) 0.0405(8) Uani 1 1 d . . . H4B H 0.8827 0.5272 0.3876 0.061 Uiso 1 1 calc R . . H4A H 0.8075 0.4594 0.2983 0.061 Uiso 1 1 calc R . . C5 C 0.7007(4) 0.58108(19) 0.1531(3) 0.0398(8) Uani 1 1 d . . . H5A H 0.72 0.5493 0.0885 0.06 Uiso 1 1 calc R . . H5B H 0.8038 0.6064 0.2041 0.06 Uiso 1 1 calc R . . C6 C 0.5677(4) 0.6318(2) 0.0762(4) 0.0589(11) Uani 1 1 d . . . H6A H 0.5671 0.6699 0.138 0.088 Uiso 1 1 calc R . . H6B H 0.5918 0.6523 0.0017 0.088 Uiso 1 1 calc R . . C7 C 0.4068(4) 0.5998(2) 0.0198(4) 0.0515(10) Uani 1 1 d . . . H7B H 0.397 0.5728 -0.0616 0.077 Uiso 1 1 calc R . . H7A H 0.3232 0.637 -0.0104 0.077 Uiso 1 1 calc R . . C8 C -0.0087(4) 0.70256(17) 0.0780(3) 0.0305(7) Uani 1 1 d . . . C9 C -0.2419(4) 0.74035(18) -0.1322(3) 0.0414(8) Uani 1 1 d . . . H9A H -0.3474 0.7191 -0.1919 0.062 Uiso 1 1 calc R . . H9B H -0.1892 0.7598 -0.1902 0.062 Uiso 1 1 calc R . . C10 C -0.2719(4) 0.79745(19) -0.0483(3) 0.0434(9) Uani 1 1 d . . . H10B H -0.3374 0.7794 0.0006 0.065 Uiso 1 1 calc R . . H10A H -0.3337 0.8358 -0.1081 0.065 Uiso 1 1 calc R . . C11 C -0.1085(4) 0.82373(18) 0.0523(3) 0.0445(9) Uani 1 1 d . . . H11B H -0.0498 0.8471 0.0028 0.067 Uiso 1 1 calc R . . H11A H -0.1267 0.8582 0.1132 0.067 Uiso 1 1 calc R . . C12 C 0.1303(4) 0.7880(2) 0.2544(4) 0.0516(10) Uani 1 1 d . . . H15B H 0.0946 0.8218 0.3064 0.077 Uiso 1 1 calc R . . H15A H 0.2142 0.8105 0.229 0.077 Uiso 1 1 calc R . . C13 C 0.2036(6) 0.7237(3) 0.3419(5) 0.0892(17) Uani 1 1 d . . . H13B H 0.3084 0.7365 0.4168 0.134 Uiso 1 1 calc R . . H13A H 0.1278 0.7074 0.3827 0.134 Uiso 1 1 calc R . . C14 C 0.2318(5) 0.6688(2) 0.2648(4) 0.0564(10) Uani 1 1 d . . . H14B H 0.2567 0.6261 0.3206 0.085 Uiso 1 1 calc R . . H14A H 0.3303 0.6804 0.2477 0.085 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 Li 0.030(3) 0.035(3) 0.034(3) 0.004(2) 0.008(2) 0.001(2) Cl 0.0287(4) 0.0325(4) 0.0303(4) 0.0028(3) 0.0112(3) -0.0009(3) N1 0.0236(13) 0.055(2) 0.0383(15) 0.0178(13) 0.0090(12) 0.0036(13) N2 0.0286(13) 0.0407(18) 0.0330(14) 0.0103(12) 0.0080(12) 0.0000(12) N3 0.0229(12) 0.0401(17) 0.0309(13) 0.0012(12) 0.0101(10) 0.0001(12) N4 0.0374(15) 0.0325(17) 0.0356(15) -0.0024(12) 0.0054(13) 0.0063(13) N5 0.0374(15) 0.0329(17) 0.0353(14) -0.0015(12) 0.0067(12) 0.0022(13) N6 0.0375(15) 0.0353(17) 0.0387(15) -0.0056(13) 0.0090(12) 0.0013(13) C1 0.0264(15) 0.0326(19) 0.0276(15) -0.0025(13) 0.0105(13) -0.0017(13) C2 0.0348(18) 0.051(2) 0.0421(18) 0.0155(16) 0.0117(15) 0.0045(16) C3 0.0321(18) 0.072(3) 0.0365(18) 0.0099(17) 0.0095(15) 0.0073(17) C4 0.0246(16) 0.053(2) 0.0399(18) 0.0031(16) 0.0087(14) 0.0044(15) C5 0.0345(18) 0.043(2) 0.0460(18) 0.0018(16) 0.0207(15) -0.0045(15) C6 0.046(2) 0.067(3) 0.064(2) 0.024(2) 0.0230(19) -0.002(2) C7 0.043(2) 0.058(3) 0.050(2) 0.0226(18) 0.0148(17) -0.0003(18) C8 0.0300(16) 0.0314(19) 0.0311(15) -0.0027(14) 0.0132(14) -0.0037(14) C9 0.0397(18) 0.041(2) 0.0372(17) 0.0003(15) 0.0088(15) 0.0075(16) C10 0.045(2) 0.038(2) 0.0439(18) 0.0055(15) 0.0143(16) 0.0106(16) C11 0.052(2) 0.031(2) 0.0480(19) 0.0012(16) 0.0167(17) 0.0086(17) C12 0.046(2) 0.050(2) 0.049(2) -0.0170(18) 0.0091(17) -0.0007(18) C13 0.078(3) 0.084(4) 0.068(3) -0.018(3) -0.011(3) 0.026(3) C14 0.061(2) 0.047(3) 0.0397(19) -0.0075(17) -0.0035(18) 0.003(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 Li N2 2.028(5) . ? Li N5 2.037(6) . ? Li Cl 2.398(5) . ? Li Cl 2.416(5) 3_565 ? Li Li 3.073(10) 3_565 ? Cl Li 2.416(5) 3_565 ? N1 C1 1.377(4) . ? N1 C2 1.445(4) . ? N2 C1 1.293(4) . ? N2 C7 1.463(4) . ? N3 C1 1.369(4) . ? N3 C4 1.457(4) . ? N3 C5 1.464(4) . ? N4 C8 1.366(4) . ? N4 C9 1.450(4) . ? N5 C8 1.295(4) . ? N5 C14 1.471(4) . ? N6 C8 1.377(4) . ? N6 C12 1.452(4) . ? N6 C11 1.453(4) . ? C2 C3 1.508(5) . ? C3 C4 1.498(4) . ? C5 C6 1.503(5) . ? C6 C7 1.452(5) . ? C9 C10 1.512(5) . ? C10 C11 1.512(5) . ? C12 C13 1.534(6) . ? C13 C14 1.426(6) . ? 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 Li N5 102.9(3) . . ? N2 Li Cl 109.7(2) . . ? N5 Li Cl 119.3(2) . . ? N2 Li Cl 114.9(2) . 3_565 ? N5 Li Cl 110.0(2) . 3_565 ? Cl Li Cl 100.67(19) . 3_565 ? N2 Li Li 126.4(3) . 3_565 ? N5 Li Li 130.6(3) . 3_565 ? Cl Li Li 50.59(15) . 3_565 ? Cl Li Li 50.08(14) 3_565 3_565 ? Li Cl Li 79.33(19) . 3_565 ? C1 N1 C2 122.7(2) . . ? C1 N2 C7 118.0(2) . . ? C1 N2 Li 131.2(2) . . ? C7 N2 Li 109.9(2) . . ? C1 N3 C4 122.1(3) . . ? C1 N3 C5 118.7(2) . . ? C4 N3 C5 115.8(2) . . ? C8 N4 C9 124.2(3) . . ? C8 N5 C14 117.6(3) . . ? C8 N5 Li 132.5(3) . . ? C14 N5 Li 109.7(3) . . ? C8 N6 C12 119.3(3) . . ? C8 N6 C11 121.9(3) . . ? C12 N6 C11 115.3(3) . . ? N2 C1 N3 126.2(3) . . ? N2 C1 N1 117.0(2) . . ? N3 C1 N1 116.7(2) . . ? N1 C2 C3 108.8(3) . . ? C4 C3 C2 109.5(3) . . ? N3 C4 C3 111.9(2) . . ? N3 C5 C6 110.1(2) . . ? C7 C6 C5 112.5(3) . . ? C6 C7 N2 115.3(3) . . ? N5 C8 N4 117.8(3) . . ? N5 C8 N6 125.7(3) . . ? N4 C8 N6 116.5(3) . . ? N4 C9 C10 109.2(3) . . ? C9 C10 C11 108.7(3) . . ? N6 C11 C10 111.1(3) . . ? N6 C12 C13 109.3(3) . . ? C14 C13 C12 111.9(4) . . ? C13 C14 N5 115.9(3) . . ? #===END data_(hppH)-dec402 _database_code_depnum_ccdc_archive 'CCDC 224309' _audit_creation_date 2002-12-13T14:41:59-00:00 _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 'C7 H13 N3' _chemical_formula_sum 'C7 H13 N3' _chemical_formula_weight 139.2 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 8.5628(2) _cell_length_b 14.8659(3) _cell_length_c 11.6451(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1482.35(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7833 _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 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.08 _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 0.0554 _diffrn_reflns_av_unetI/netI 0.0225 _diffrn_reflns_number 14208 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.03 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 1298 _reflns_number_gt 1148 _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 ; Atom C6 is disordered over two positions. The H atom on N is disordered over the two nitrogen atoms. 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^)+(0.0695P)^2^+0.7131P] 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 'H on N refined; others riding' _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.055(12) _refine_ls_number_reflns 1298 _refine_ls_number_parameters 110 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.136 _refine_ls_wR_factor_gt 0.1309 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.303 _refine_diff_density_min -0.272 _refine_diff_density_rms 0.038 #----------------------------------------------------------------------------# # 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' 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 N1 N 0.1006(2) -0.60139(10) 0.45274(13) 0.0435(5) Uani 1 1 d . . . H1 H 0.048(5) -0.578(2) 0.508(3) 0.036(9) Uiso 0.5 1 d P . . N2 N 0.17657(17) -0.59937(9) 0.25900(11) 0.0355(4) Uani 1 1 d . . . N3 N 0.06860(19) -0.47267(10) 0.34930(12) 0.0382(5) Uani 1 1 d . . . H3 H 0.024(4) -0.454(2) 0.410(3) 0.021(8) Uiso 0.5 1 d P . . C1 C 0.11455(18) -0.55810(11) 0.35351(13) 0.0312(5) Uani 1 1 d . A . C2 C 0.1402(3) -0.69571(12) 0.45966(15) 0.0468(6) Uani 1 1 d . A . H2A H 0.0499 -0.7323 0.4345 0.056 Uiso 1 1 calc R . . H2B H 0.164 -0.7117 0.5403 0.056 Uiso 1 1 calc R . . C3 C 0.2793(2) -0.71662(13) 0.38521(16) 0.0462(5) Uani 1 1 d . . . H3A H 0.3721 -0.6835 0.4134 0.055 Uiso 1 1 calc R A . H3B H 0.3025 -0.7818 0.3881 0.055 Uiso 1 1 calc R . . C4 C 0.2434(2) -0.68906(11) 0.26410(15) 0.0383(5) Uani 1 1 d . A . H4A H 0.3405 -0.6906 0.2181 0.046 Uiso 1 1 calc R . . H4B H 0.1691 -0.7326 0.23 0.046 Uiso 1 1 calc R . . C5 C 0.1716(2) -0.55862(12) 0.14512(13) 0.0378(5) Uani 0.798(7) 1 d P A 1 H5A H 0.1403 -0.6046 0.0881 0.045 Uiso 0.798(7) 1 calc PR A 1 H5B H 0.2771 -0.5368 0.1243 0.045 Uiso 0.798(7) 1 calc PR A 1 C6 C 0.0580(4) -0.48116(16) 0.14091(18) 0.0396(8) Uani 0.798(7) 1 d P A 1 H6A H 0.0755 -0.4454 0.0704 0.047 Uiso 0.798(7) 1 calc PR A 1 H6B H -0.0504 -0.5044 0.1393 0.047 Uiso 0.798(7) 1 calc PR A 1 C7 C 0.0805(3) -0.42386(13) 0.24307(16) 0.0545(6) Uani 0.798(7) 1 d P A 1 H7A H 0.1847 -0.3952 0.2387 0.065 Uiso 0.798(7) 1 calc PR A 1 H7B H 0.0012 -0.3754 0.2425 0.065 Uiso 0.798(7) 1 calc PR A 1 C5A C 0.1716(2) -0.55862(12) 0.14512(13) 0.0378(5) Uani 0.202(7) 1 d P A 2 H5A1 H 0.0804 -0.582 0.1022 0.045 Uiso 0.202(7) 1 calc PR A 2 H5A2 H 0.2672 -0.5746 0.102 0.045 Uiso 0.202(7) 1 calc PR A 2 C6A C 0.1588(13) -0.4504(6) 0.1567(7) 0.037(3) Uani 0.202(7) 1 d P A 2 H6A1 H 0.2655 -0.4251 0.1618 0.045 Uiso 0.202(7) 1 calc PR A 2 H6A2 H 0.1098 -0.4262 0.0861 0.045 Uiso 0.202(7) 1 calc PR A 2 C7A C 0.0805(3) -0.42386(13) 0.24307(16) 0.0545(6) Uani 0.202(7) 1 d P A 2 H7A1 H -0.0278 -0.4148 0.2156 0.065 Uiso 0.202(7) 1 calc PR A 2 H7A2 H 0.1213 -0.3635 0.263 0.065 Uiso 0.202(7) 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 N1 0.0648(11) 0.0366(8) 0.0291(8) 0.0026(6) 0.0093(7) 0.0174(7) N2 0.0432(9) 0.0351(8) 0.0281(7) -0.0022(5) 0.0047(6) 0.0081(6) N3 0.0535(9) 0.0312(8) 0.0298(8) -0.0009(5) 0.0076(6) 0.0068(7) C1 0.0311(9) 0.0342(9) 0.0284(9) -0.0055(6) 0.0018(6) 0.0006(7) C2 0.0682(13) 0.0374(10) 0.0348(10) 0.0057(7) 0.0060(9) 0.0156(9) C3 0.0520(11) 0.0393(10) 0.0475(11) -0.0040(8) -0.0039(8) 0.0144(8) C4 0.0410(10) 0.0338(9) 0.0400(10) -0.0071(7) 0.0080(7) 0.0039(7) C5 0.0437(10) 0.0424(10) 0.0273(9) -0.0017(7) 0.0075(7) -0.0020(8) C6 0.0482(17) 0.0380(13) 0.0325(12) 0.0047(9) 0.0007(10) -0.0044(12) C7 0.0890(17) 0.0361(10) 0.0384(11) 0.0050(8) 0.0094(10) 0.0096(10) C5A 0.0437(10) 0.0424(10) 0.0273(9) -0.0017(7) 0.0075(7) -0.0020(8) C6A 0.038(6) 0.038(5) 0.035(5) 0.011(4) 0.004(4) -0.003(4) C7A 0.0890(17) 0.0361(10) 0.0384(11) 0.0050(8) 0.0094(10) 0.0096(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 N1 C1 1.328(2) . ? N1 C2 1.445(2) . ? N2 C1 1.367(2) . ? N2 C4 1.452(2) . ? N2 C5 1.459(2) . ? N3 C1 1.331(2) . ? N3 C7 1.438(2) . ? C2 C3 1.506(3) . ? C3 C4 1.501(3) . ? C5 C6 1.508(3) . ? C6 C7 1.476(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C2 119.85(15) . . ? C1 N2 C4 122.15(13) . . ? C1 N2 C5 122.29(14) . . ? C4 N2 C5 115.47(13) . . ? C1 N3 C7 119.50(14) . . ? N1 C1 N3 117.90(14) . . ? N1 C1 N2 121.19(15) . . ? N3 C1 N2 120.89(14) . . ? N1 C2 C3 110.72(16) . . ? C4 C3 C2 108.80(15) . . ? N2 C4 C3 111.71(13) . . ? N2 C5 C6 111.44(14) . . ? C7 C6 C5 109.29(19) . . ? N3 C7 C6 113.15(17) . . ? #===END data_(5)-aug903 _database_code_depnum_ccdc_archive 'CCDC 224310' _audit_creation_date 2003-08-26T08:25:42-00:00 _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 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C14 H26 Ag1 Cl1 N6' _chemical_formula_sum 'C14 H26 Ag1 Cl1 N6' _chemical_formula_weight 421.73 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 7.4791(1) _cell_length_b 14.4246(2) _cell_length_c 16.1899(3) _cell_angle_alpha 90 _cell_angle_beta 97.165(1) _cell_angle_gamma 90 _cell_volume 1732.98(5) _cell_formula_units_Z 4 _cell_measurement_temperature 253(2) _cell_measurement_reflns_used 10524 _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 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.323 _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 0.6003 _exptl_absorpt_correction_T_max 0.8217 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 253(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_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.122889 _diffrn_orient_matrix_ub_12 -0.244336E-1 _diffrn_orient_matrix_ub_13 0.5901E-2 _diffrn_orient_matrix_ub_21 0.386135E-1 _diffrn_orient_matrix_ub_22 -0.633324E-1 _diffrn_orient_matrix_ub_23 -0.156054E-1 _diffrn_orient_matrix_ub_31 0.395851E-1 _diffrn_orient_matrix_ub_32 -0.140748E-1 _diffrn_orient_matrix_ub_33 0.599758E-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 0.0412 _diffrn_reflns_av_unetI/netI 0.0237 _diffrn_reflns_number 17656 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 3020 _reflns_number_gt 2702 _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 ; Hydrogen on nitrogen were refined; others were in riding mode. There is disorder in one ring 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^)+(0.0480P)^2^+1.9491P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3020 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0882 _refine_ls_wR_factor_gt 0.0839 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.683 _refine_diff_density_min -0.914 _refine_diff_density_rms 0.067 #----------------------------------------------------------------------------# # 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' Ag Ag -0.8971 1.1015 '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' 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 Ag Ag 0.25745(3) 0.398260(19) 0.267803(17) 0.05115(13) Uani 1 1 d . A . Cl Cl 0.27105(15) 0.34110(7) 0.11967(6) 0.0682(3) Uani 1 1 d . . . N1 N 0.0241(4) 0.48532(19) 0.28526(16) 0.0457(6) Uani 1 1 d . . . N2 N -0.0886(4) 0.4807(2) 0.14787(18) 0.0514(7) Uani 1 1 d . . . H2N H -0.009(4) 0.452(2) 0.1458(19) 0.026(8) Uiso 1 1 d . . . N3 N -0.2598(3) 0.5499(2) 0.23952(18) 0.0485(7) Uani 1 1 d . . . N4 N 0.4625(3) 0.34189(19) 0.36305(15) 0.0439(6) Uani 1 1 d . . . N5 N 0.6386(4) 0.2888(2) 0.26786(18) 0.0499(7) Uani 1 1 d . . . H5N H 0.570(5) 0.305(2) 0.237(2) 0.036(10) Uiso 1 1 d . . . N6 N 0.7327(4) 0.26227(19) 0.40780(16) 0.0464(6) Uani 1 1 d . . . C1 C -0.1071(4) 0.50425(19) 0.22691(19) 0.0376(6) Uani 1 1 d . A . C5 C -0.4089(5) 0.5647(3) 0.1740(3) 0.0722(12) Uani 1 1 d . A . H5A H -0.467 0.6231 0.1837 0.087 Uiso 1 1 calc R . . H5B H -0.497 0.5157 0.1762 0.087 Uiso 1 1 calc R . . C6 C -0.3502(7) 0.5662(4) 0.0913(3) 0.0948(17) Uani 1 1 d . . . H6A H -0.4552 0.5622 0.0497 0.114 Uiso 1 1 calc R A . H6B H -0.2909 0.6248 0.0835 0.114 Uiso 1 1 calc R . . C7 C -0.2272(7) 0.4905(3) 0.0784(3) 0.0840(14) Uani 1 1 d . A . H7A H -0.2947 0.4331 0.0706 0.101 Uiso 1 1 calc R . . H7B H -0.172 0.5022 0.0283 0.101 Uiso 1 1 calc R . . C8 C 0.6081(4) 0.29828(19) 0.34804(17) 0.0358(6) Uani 1 1 d . A . C9 C 0.7890(5) 0.2408(3) 0.2399(2) 0.0545(9) Uani 1 1 d . A . H9A H 0.8302 0.2747 0.1941 0.065 Uiso 1 1 calc R . . H9B H 0.7507 0.1797 0.2197 0.065 Uiso 1 1 calc R . . C10 C 0.9386(5) 0.2315(3) 0.3079(3) 0.0647(10) Uani 1 1 d . . . H10A H 1.0237 0.186 0.2921 0.078 Uiso 1 1 calc R A . H10B H 1.0011 0.2904 0.3157 0.078 Uiso 1 1 calc R . . C11 C 0.8776(5) 0.2031(3) 0.3869(2) 0.0668(11) Uani 1 1 d . A . H11A H 0.836 0.1394 0.3826 0.08 Uiso 1 1 calc R . . H11B H 0.9779 0.2062 0.431 0.08 Uiso 1 1 calc R . . C12 C 0.7049(6) 0.2673(3) 0.4944(2) 0.0713(12) Uani 1 1 d . A . H12A H 0.8204 0.2743 0.5284 0.086 Uiso 1 1 calc R . . H12B H 0.6513 0.2098 0.5103 0.086 Uiso 1 1 calc R . . C13 C 0.5877(7) 0.3448(4) 0.5106(2) 0.0858(15) Uani 1 1 d . . . H13A H 0.5518 0.3378 0.5658 0.103 Uiso 1 1 calc R A . H13B H 0.6549 0.4022 0.5097 0.103 Uiso 1 1 calc R . . C14 C 0.4271(6) 0.3505(3) 0.4500(2) 0.0664(11) Uani 1 1 d . A . H14A H 0.3683 0.4094 0.4568 0.08 Uiso 1 1 calc R . . H14B H 0.3443 0.3018 0.4617 0.08 Uiso 1 1 calc R . . C2 C 0.0002(6) 0.5100(4) 0.3706(2) 0.0778(13) Uani 0.740(17) 1 d P A 1 H2A H -0.0452 0.456 0.3971 0.093 Uiso 0.740(17) 1 calc PR A 1 H2B H 0.1175 0.5245 0.4004 0.093 Uiso 0.740(17) 1 calc PR A 1 C3 C -0.1195(10) 0.5870(6) 0.3802(4) 0.061(2) Uani 0.740(17) 1 d P A 1 H3A H -0.0629 0.6445 0.3663 0.074 Uiso 0.740(17) 1 calc PR A 1 H3B H -0.1432 0.5909 0.4377 0.074 Uiso 0.740(17) 1 calc PR A 1 C4 C -0.2963(6) 0.5739(3) 0.3235(3) 0.0655(11) Uani 0.740(17) 1 d P A 1 H4A H -0.366 0.525 0.3453 0.079 Uiso 0.740(17) 1 calc PR A 1 H4B H -0.3662 0.6307 0.3218 0.079 Uiso 0.740(17) 1 calc PR A 1 C2A C 0.0002(6) 0.5100(4) 0.3706(2) 0.0778(13) Uani 0.260(17) 1 d P A 2 H2A1 H 0.0451 0.4595 0.407 0.093 Uiso 0.260(17) 1 calc PR A 2 H2A2 H 0.0731 0.5642 0.3867 0.093 Uiso 0.260(17) 1 calc PR A 2 C3A C -0.175(2) 0.5284(18) 0.3832(9) 0.063(6) Uani 0.260(17) 1 d P A 2 H3A1 H -0.1698 0.5644 0.434 0.075 Uiso 0.260(17) 1 calc PR A 2 H3A2 H -0.2298 0.4694 0.3943 0.075 Uiso 0.260(17) 1 calc PR A 2 C4A C -0.2963(6) 0.5739(3) 0.3235(3) 0.0655(11) Uani 0.260(17) 1 d P A 2 H4A1 H -0.285 0.6404 0.3314 0.079 Uiso 0.260(17) 1 calc PR A 2 H4A2 H -0.4187 0.5564 0.3305 0.079 Uiso 0.260(17) 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 Ag 0.03690(17) 0.05692(19) 0.0592(2) 0.00995(11) 0.00435(12) 0.00959(10) Cl 0.0807(7) 0.0747(6) 0.0495(5) -0.0044(4) 0.0096(5) 0.0199(5) N1 0.0427(14) 0.0562(16) 0.0369(13) -0.0033(11) 0.0001(11) 0.0137(12) N2 0.0461(17) 0.0640(19) 0.0419(15) -0.0024(13) -0.0041(13) 0.0181(15) N3 0.0376(15) 0.0444(15) 0.0631(18) 0.0033(12) 0.0052(13) 0.0080(11) N4 0.0413(14) 0.0553(15) 0.0355(13) 0.0017(11) 0.0068(11) 0.0138(12) N5 0.0428(16) 0.070(2) 0.0370(15) 0.0027(13) 0.0054(13) 0.0201(14) N6 0.0432(15) 0.0565(16) 0.0383(14) -0.0014(12) -0.0001(11) 0.0167(12) C1 0.0347(15) 0.0321(14) 0.0456(16) 0.0018(12) 0.0038(13) 0.0028(11) C5 0.041(2) 0.063(2) 0.107(4) -0.004(2) -0.013(2) 0.0115(17) C6 0.077(3) 0.110(4) 0.087(4) 0.003(3) -0.034(3) 0.026(3) C7 0.091(3) 0.090(3) 0.061(2) -0.015(2) -0.032(2) 0.024(3) C8 0.0343(15) 0.0371(14) 0.0359(15) 0.0011(12) 0.0041(12) 0.0038(12) C9 0.0508(19) 0.069(2) 0.0470(18) -0.0030(16) 0.0173(15) 0.0157(17) C10 0.045(2) 0.074(3) 0.078(3) 0.001(2) 0.0185(19) 0.0191(18) C11 0.055(2) 0.083(3) 0.061(2) 0.000(2) 0.0014(18) 0.035(2) C12 0.080(3) 0.096(3) 0.0360(18) 0.0004(18) -0.0013(18) 0.035(2) C13 0.087(3) 0.134(4) 0.0372(19) -0.006(2) 0.009(2) 0.039(3) C14 0.067(2) 0.092(3) 0.0430(19) 0.0014(19) 0.0162(18) 0.032(2) C2 0.078(3) 0.106(3) 0.047(2) -0.018(2) 0.001(2) 0.026(3) C3 0.080(4) 0.056(4) 0.052(3) -0.006(3) 0.024(3) 0.006(3) C4 0.058(2) 0.062(2) 0.082(3) -0.001(2) 0.031(2) 0.0147(19) C2A 0.078(3) 0.106(3) 0.047(2) -0.018(2) 0.001(2) 0.026(3) C3A 0.072(11) 0.071(15) 0.052(9) -0.015(8) 0.035(8) 0.003(9) C4A 0.058(2) 0.062(2) 0.082(3) -0.001(2) 0.031(2) 0.0147(19) #----------------------------------------------------------------------------# # 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 Ag N4 2.191(3) . ? Ag N1 2.197(3) . ? Ag Cl 2.5501(10) . ? N1 C1 1.303(4) . ? N1 C2 1.459(5) . ? N2 C1 1.348(4) . ? N2 C7 1.438(5) . ? N3 C1 1.356(4) . ? N3 C5 1.456(5) . ? N3 C4 1.462(5) . ? N4 C8 1.306(4) . ? N4 C14 1.470(4) . ? N5 C8 1.353(4) . ? N5 C9 1.442(4) . ? N6 C8 1.360(4) . ? N6 C12 1.445(4) . ? N6 C11 1.452(4) . ? C5 C6 1.460(8) . ? C6 C7 1.459(7) . ? C9 C10 1.475(5) . ? C10 C11 1.470(6) . ? C12 C13 1.464(6) . ? C13 C14 1.456(6) . ? C2 C3 1.448(7) . ? C3 C4 1.524(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 N4 Ag N1 128.25(9) . . ? N4 Ag Cl 115.81(7) . . ? N1 Ag Cl 115.55(7) . . ? C1 N1 C2 117.7(3) . . ? C1 N1 Ag 124.4(2) . . ? C2 N1 Ag 117.0(2) . . ? C1 N2 C7 124.6(3) . . ? C1 N3 C5 123.0(3) . . ? C1 N3 C4 120.9(3) . . ? C5 N3 C4 115.4(3) . . ? C8 N4 C14 118.2(3) . . ? C8 N4 Ag 125.0(2) . . ? C14 N4 Ag 116.7(2) . . ? C8 N5 C9 125.6(3) . . ? C8 N6 C12 120.2(3) . . ? C8 N6 C11 121.6(3) . . ? C12 N6 C11 117.2(3) . . ? N1 C1 N2 118.6(3) . . ? N1 C1 N3 124.4(3) . . ? N2 C1 N3 117.0(3) . . ? N3 C5 C6 112.4(4) . . ? C7 C6 C5 112.7(4) . . ? N2 C7 C6 111.6(4) . . ? N4 C8 N5 118.1(3) . . ? N4 C8 N6 124.4(3) . . ? N5 C8 N6 117.5(3) . . ? N5 C9 C10 111.0(3) . . ? C11 C10 C9 112.7(3) . . ? N6 C11 C10 111.1(3) . . ? N6 C12 C13 112.0(3) . . ? C14 C13 C12 112.6(4) . . ? C13 C14 N4 114.2(3) . . ? C3 C2 N1 116.1(4) . . ? C2 C3 C4 110.0(5) . . ? N3 C4 C3 110.0(3) . . ? #===END data_(6)-nov102 _database_code_depnum_ccdc_archive 'CCDC 224311' _audit_creation_date 2002-10-30T14:47:10-00:00 _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 [CuCl(PPh3)(C7H13N3)] _chemical_formula_moiety 'C25 H28 Cl1 Cu1 N3 P1' _chemical_formula_sum 'C25 H28 Cl Cu N3 P' _chemical_formula_weight 500.46 _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 9.3552(1) _cell_length_b 16.3599(3) _cell_length_c 15.2723(2) _cell_angle_alpha 90 _cell_angle_beta 90.656(1) _cell_angle_gamma 90 _cell_volume 2337.27(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11653 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.878 _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 0.3 _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.135 _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 0.6284 _exptl_absorpt_correction_T_max 0.7215 #----------------------------------------------------------------------------# # 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 0.0438 _diffrn_reflns_av_unetI/netI 0.0346 _diffrn_reflns_number 21620 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.97 _diffrn_reflns_theta_max 27.88 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 5515 _reflns_number_gt 4591 _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^)+(0.0238P)^2^+1.5020P] 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 'H on N2 refined; others riding' _refine_ls_extinction_method none _refine_ls_number_reflns 5515 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0738 _refine_ls_wR_factor_gt 0.0691 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.291 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.051 #----------------------------------------------------------------------------# # 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' Cu Cu 0.3201 1.2651 '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 Cu Cu 0.81247(2) 0.091706(14) 0.825875(14) 0.02710(7) Uani 1 1 d . . . Cl Cl 0.70732(5) 0.15148(3) 0.94295(3) 0.03509(12) Uani 1 1 d . . . P P 0.69171(5) 0.06916(3) 0.70366(3) 0.02437(10) Uani 1 1 d . . . N1 N 1.01635(16) 0.06357(10) 0.84041(10) 0.0304(3) Uani 1 1 d . . . N3 N 1.23676(16) 0.05024(10) 0.91569(11) 0.0334(4) Uani 1 1 d . . . N2 N 1.0480(2) 0.12147(12) 0.97634(11) 0.0401(4) Uani 1 1 d . . . H2 H 0.966(3) 0.1341(14) 0.9714(14) 0.038(6) Uiso 1 1 d . . . C1 C 1.09977(19) 0.07670(11) 0.90950(12) 0.0283(4) Uani 1 1 d . . . C2 C 1.0879(2) 0.02370(13) 0.76662(13) 0.0367(5) Uani 1 1 d . . . H2A H 1.1485 0.064 0.7361 0.044 Uiso 1 1 calc R . . H2B H 1.0152 0.0033 0.7244 0.044 Uiso 1 1 calc R . . C3 C 1.1789(2) -0.04657(13) 0.79830(14) 0.0405(5) Uani 1 1 d . . . H3A H 1.1194 -0.0866 0.8301 0.049 Uiso 1 1 calc R . . H3B H 1.2229 -0.0746 0.7479 0.049 Uiso 1 1 calc R . . C4 C 1.2935(2) -0.01310(14) 0.85831(14) 0.0403(5) Uani 1 1 d . . . H4A H 1.3337 -0.058 0.8943 0.048 Uiso 1 1 calc R . . H4B H 1.3717 0.0101 0.8229 0.048 Uiso 1 1 calc R . . C5 C 1.3325(2) 0.07170(15) 0.98865(14) 0.0426(5) Uani 1 1 d . . . H5A H 1.429 0.0833 0.9658 0.051 Uiso 1 1 calc R . . H5B H 1.3404 0.0247 1.0292 0.051 Uiso 1 1 calc R . . C6 C 1.2804(2) 0.14441(16) 1.03756(16) 0.0492(6) Uani 1 1 d . . . H6A H 1.2932 0.1943 1.0017 0.059 Uiso 1 1 calc R . . H6B H 1.3364 0.151 1.0925 0.059 Uiso 1 1 calc R . . C7 C 1.1253(2) 0.13352(16) 1.05824(14) 0.0444(5) Uani 1 1 d . . . H7A H 1.1126 0.0856 1.0969 0.053 Uiso 1 1 calc R . . H7B H 1.0887 0.1825 1.0888 0.053 Uiso 1 1 calc R . . C8 C 0.79318(19) 0.08274(11) 0.60261(12) 0.0281(4) Uani 1 1 d . . . C9 C 0.7787(2) 0.03130(14) 0.53048(12) 0.0356(4) Uani 1 1 d . . . H9 H 0.7164 -0.0145 0.5331 0.043 Uiso 1 1 calc R . . C10 C 0.8545(2) 0.04639(16) 0.45505(14) 0.0462(6) Uani 1 1 d . . . H10 H 0.8447 0.0106 0.4063 0.055 Uiso 1 1 calc R . . C11 C 0.9443(2) 0.11305(16) 0.45005(15) 0.0482(6) Uani 1 1 d . . . H11 H 0.9943 0.124 0.3975 0.058 Uiso 1 1 calc R . . C12 C 0.9615(2) 0.16389(15) 0.52157(16) 0.0471(6) Uani 1 1 d . . . H12 H 1.0245 0.2094 0.5186 0.056 Uiso 1 1 calc R . . C13 C 0.8870(2) 0.14848(13) 0.59751(14) 0.0383(5) Uani 1 1 d . . . H13 H 0.9 0.1832 0.6468 0.046 Uiso 1 1 calc R . . C14 C 0.62891(19) -0.03640(11) 0.69295(11) 0.0252(4) Uani 1 1 d . . . C15 C 0.7223(2) -0.09820(12) 0.71986(13) 0.0359(4) Uani 1 1 d . . . H15 H 0.8118 -0.0843 0.7458 0.043 Uiso 1 1 calc R . . C16 C 0.6858(3) -0.17957(13) 0.70913(16) 0.0462(5) Uani 1 1 d . . . H16 H 0.7512 -0.2211 0.7264 0.055 Uiso 1 1 calc R . . C17 C 0.5546(2) -0.20071(13) 0.67348(15) 0.0421(5) Uani 1 1 d . . . H17 H 0.5292 -0.2566 0.6669 0.051 Uiso 1 1 calc R . . C18 C 0.4609(2) -0.14030(13) 0.64752(14) 0.0387(5) Uani 1 1 d . . . H18 H 0.3706 -0.1547 0.6229 0.046 Uiso 1 1 calc R . . C19 C 0.4975(2) -0.05836(12) 0.65707(13) 0.0326(4) Uani 1 1 d . . . H19 H 0.432 -0.0171 0.6389 0.039 Uiso 1 1 calc R . . C20 C 0.53294(19) 0.13168(11) 0.68332(12) 0.0272(4) Uani 1 1 d . . . C21 C 0.4748(2) 0.14391(13) 0.59974(14) 0.0370(5) Uani 1 1 d . . . H21 H 0.5191 0.1194 0.5506 0.044 Uiso 1 1 calc R . . C22 C 0.3536(2) 0.19116(14) 0.58749(16) 0.0449(5) Uani 1 1 d . . . H22 H 0.3145 0.1987 0.5304 0.054 Uiso 1 1 calc R . . C23 C 0.2897(2) 0.22743(14) 0.65890(17) 0.0488(6) Uani 1 1 d . . . H23 H 0.2066 0.2601 0.6508 0.059 Uiso 1 1 calc R . . C24 C 0.3461(2) 0.21631(15) 0.74151(17) 0.0493(6) Uani 1 1 d . . . H24 H 0.3013 0.2411 0.7903 0.059 Uiso 1 1 calc R . . C25 C 0.4683(2) 0.16906(13) 0.75414(14) 0.0373(5) Uani 1 1 d . . . H25 H 0.5074 0.1624 0.8114 0.045 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 Cu 0.02858(12) 0.02796(13) 0.02465(12) -0.00306(9) -0.00404(8) 0.00085(9) Cl 0.0317(2) 0.0432(3) 0.0304(2) -0.0102(2) 0.00080(18) 0.0003(2) P 0.0250(2) 0.0258(2) 0.0222(2) -0.00227(17) -0.00239(17) 0.00199(18) N1 0.0277(8) 0.0373(9) 0.0262(8) -0.0060(7) -0.0024(6) 0.0058(7) N3 0.0248(8) 0.0413(10) 0.0340(9) -0.0002(7) -0.0016(6) 0.0029(7) N2 0.0308(9) 0.0553(12) 0.0339(9) -0.0148(8) -0.0108(7) 0.0115(9) C1 0.0268(9) 0.0292(10) 0.0288(9) 0.0020(7) -0.0001(7) 0.0003(7) C2 0.0339(10) 0.0454(12) 0.0309(10) -0.0084(9) 0.0034(8) 0.0022(9) C3 0.0397(11) 0.0384(12) 0.0439(12) -0.0062(9) 0.0134(9) 0.0045(9) C4 0.0319(10) 0.0471(13) 0.0420(12) 0.0032(10) 0.0072(9) 0.0112(9) C5 0.0254(10) 0.0594(14) 0.0429(12) 0.0045(10) -0.0070(8) -0.0044(10) C6 0.0452(13) 0.0565(15) 0.0454(13) -0.0029(11) -0.0133(10) -0.0110(11) C7 0.0393(12) 0.0603(15) 0.0335(11) -0.0104(10) -0.0093(9) 0.0028(11) C8 0.0255(9) 0.0324(10) 0.0263(9) 0.0021(7) -0.0023(7) 0.0029(8) C9 0.0323(10) 0.0469(12) 0.0275(10) -0.0031(8) 0.0003(8) 0.0007(9) C10 0.0413(12) 0.0694(16) 0.0279(11) -0.0022(10) 0.0030(9) 0.0098(12) C11 0.0363(11) 0.0706(17) 0.0379(12) 0.0171(11) 0.0105(9) 0.0139(11) C12 0.0352(11) 0.0464(13) 0.0598(15) 0.0163(11) 0.0079(10) -0.0015(10) C13 0.0377(11) 0.0361(11) 0.0411(12) 0.0015(9) 0.0013(9) -0.0011(9) C14 0.0292(9) 0.0259(9) 0.0205(8) -0.0012(7) 0.0019(7) 0.0015(7) C15 0.0376(10) 0.0333(11) 0.0365(11) 0.0012(8) -0.0085(9) 0.0027(9) C16 0.0544(14) 0.0301(11) 0.0539(14) 0.0047(10) -0.0047(11) 0.0102(10) C17 0.0518(13) 0.0259(10) 0.0488(13) -0.0049(9) 0.0051(10) -0.0018(10) C18 0.0346(11) 0.0352(11) 0.0461(12) -0.0062(9) 0.0027(9) -0.0071(9) C19 0.0291(9) 0.0310(10) 0.0376(11) -0.0005(8) -0.0004(8) 0.0015(8) C20 0.0263(9) 0.0215(9) 0.0338(10) 0.0018(7) -0.0017(7) 0.0009(7) C21 0.0357(10) 0.0401(12) 0.0349(11) 0.0040(9) -0.0048(8) 0.0045(9) C22 0.0379(11) 0.0436(13) 0.0530(14) 0.0100(10) -0.0143(10) 0.0044(10) C23 0.0341(11) 0.0354(12) 0.0767(17) 0.0016(11) -0.0121(11) 0.0104(10) C24 0.0401(12) 0.0464(13) 0.0615(15) -0.0140(11) -0.0003(11) 0.0137(10) C25 0.0355(10) 0.0360(11) 0.0403(11) -0.0064(9) -0.0034(9) 0.0063(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 Cu N1 1.9722(15) . ? Cu P 2.2018(5) . ? Cu Cl 2.2718(5) . ? P C20 1.8271(18) . ? P C14 1.8309(18) . ? P C8 1.8345(19) . ? N1 C1 1.323(2) . ? N1 C2 1.470(2) . ? N3 C1 1.355(2) . ? N3 C4 1.461(3) . ? N3 C5 1.464(3) . ? N2 C1 1.351(3) . ? N2 C7 1.451(3) . ? C2 C3 1.507(3) . ? C3 C4 1.505(3) . ? C5 C6 1.490(3) . ? C6 C7 1.498(3) . ? C8 C13 1.391(3) . ? C8 C9 1.392(3) . ? C9 C10 1.382(3) . ? C10 C11 1.379(3) . ? C11 C12 1.381(4) . ? C12 C13 1.383(3) . ? C14 C19 1.388(3) . ? C14 C15 1.395(3) . ? C15 C16 1.384(3) . ? C16 C17 1.381(3) . ? C17 C18 1.376(3) . ? C18 C19 1.391(3) . ? C20 C25 1.387(3) . ? C20 C21 1.396(3) . ? C21 C22 1.383(3) . ? C22 C23 1.384(3) . ? C23 C24 1.374(3) . ? C24 C25 1.392(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu P 122.85(5) . . ? N1 Cu Cl 116.02(5) . . ? P Cu Cl 121.115(19) . . ? C20 P C14 104.68(8) . . ? C20 P C8 102.52(8) . . ? C14 P C8 101.99(8) . . ? C20 P Cu 117.29(6) . . ? C14 P Cu 113.25(6) . . ? C8 P Cu 115.30(6) . . ? C1 N1 C2 114.46(15) . . ? C1 N1 Cu 127.80(13) . . ? C2 N1 Cu 117.74(12) . . ? C1 N3 C4 122.31(16) . . ? C1 N3 C5 123.12(17) . . ? C4 N3 C5 113.78(16) . . ? C1 N2 C7 123.05(18) . . ? N1 C1 N2 118.52(16) . . ? N1 C1 N3 123.55(17) . . ? N2 C1 N3 117.87(17) . . ? N1 C2 C3 110.66(16) . . ? C4 C3 C2 108.29(18) . . ? N3 C4 C3 111.24(16) . . ? N3 C5 C6 111.83(17) . . ? C5 C6 C7 109.52(19) . . ? N2 C7 C6 107.98(18) . . ? C13 C8 C9 118.61(18) . . ? C13 C8 P 118.27(15) . . ? C9 C8 P 123.10(15) . . ? C10 C9 C8 120.4(2) . . ? C11 C10 C9 120.4(2) . . ? C10 C11 C12 119.9(2) . . ? C11 C12 C13 119.9(2) . . ? C12 C13 C8 120.8(2) . . ? C19 C14 C15 118.54(18) . . ? C19 C14 P 124.15(14) . . ? C15 C14 P 117.26(14) . . ? C16 C15 C14 120.62(19) . . ? C17 C16 C15 120.3(2) . . ? C18 C17 C16 119.6(2) . . ? C17 C18 C19 120.4(2) . . ? C14 C19 C18 120.45(18) . . ? C25 C20 C21 118.74(17) . . ? C25 C20 P 118.38(14) . . ? C21 C20 P 122.88(15) . . ? C22 C21 C20 120.9(2) . . ? C21 C22 C23 119.6(2) . . ? C24 C23 C22 120.1(2) . . ? C23 C24 C25 120.5(2) . . ? C20 C25 C24 120.1(2) . . ? #===END data_nov2602 _database_code_depnum_ccdc_archive 'CCDC 224312' _audit_creation_date 2002-11-20T11:33:54-00:00 _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 [{CuBr(PPh3)(C7H13N3)}2] _chemical_formula_moiety 'C50 H56 Br2 Cu2 N6 P2' _chemical_formula_sum 'C50 H56 Br2 Cu2 N6 P2' _chemical_formula_weight 1089.85 _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 9.6014(2) _cell_length_b 11.2158(2) _cell_length_c 12.0457(2) _cell_angle_alpha 74.402(1) _cell_angle_beta 73.373(1) _cell_angle_gamma 89.615(1) _cell_volume 1193.69(4) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9737 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.878 _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 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 556 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.673 _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 0.501 _exptl_absorpt_correction_T_max 0.5573 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 223(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 0.0392 _diffrn_reflns_av_unetI/netI 0.0366 _diffrn_reflns_number 15808 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 27.88 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 5659 _reflns_number_gt 4793 _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^)+(0.0176P)^2^+1.0751P] 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 'H on N3 refined; others riding' _refine_ls_extinction_method none _refine_ls_number_reflns 5659 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0715 _refine_ls_wR_factor_gt 0.0673 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.579 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.064 #----------------------------------------------------------------------------# # 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 Cu Cu -0.13198(3) -0.01648(2) 0.11522(2) 0.02849(8) Uani 1 1 d . . . Br Br 0.14051(2) 0.02817(2) 0.08937(2) 0.03252(7) Uani 1 1 d . . . P P -0.20197(6) -0.19423(5) 0.25767(5) 0.02331(12) Uani 1 1 d . . . N1 N -0.2184(2) 0.13478(17) 0.15982(17) 0.0285(4) Uani 1 1 d . . . N2 N -0.3948(2) 0.28251(18) 0.17365(19) 0.0350(5) Uani 1 1 d . . . N3 N -0.3819(3) 0.1517(2) 0.0517(2) 0.0412(5) Uani 1 1 d . . . H3 H -0.332(4) 0.108(3) 0.021(3) 0.053(10) Uiso 1 1 d . . . C1 C -0.3268(2) 0.1912(2) 0.1293(2) 0.0278(5) Uani 1 1 d . . . C2 C -0.1601(3) 0.1761(3) 0.2442(2) 0.0384(6) Uani 1 1 d . . . H2A H -0.0803 0.2403 0.1986 0.046 Uiso 1 1 calc R . . H2B H -0.12 0.106 0.2905 0.046 Uiso 1 1 calc R . . C3 C -0.2746(3) 0.2273(3) 0.3301(2) 0.0428(6) Uani 1 1 d . . . H3A H -0.3484 0.1608 0.3835 0.051 Uiso 1 1 calc R . . H3B H -0.2298 0.261 0.3799 0.051 Uiso 1 1 calc R . . C4 C -0.3446(3) 0.3277(3) 0.2593(3) 0.0436(6) Uani 1 1 d . . . H4A H -0.4274 0.3541 0.3144 0.052 Uiso 1 1 calc R . . H4B H -0.2742 0.3997 0.2158 0.052 Uiso 1 1 calc R . . C5 C -0.4950(3) 0.3586(3) 0.1200(3) 0.0538(8) Uani 1 1 d . . . H5A H -0.4401 0.4316 0.0577 0.065 Uiso 1 1 calc R . . H5B H -0.5651 0.3877 0.1822 0.065 Uiso 1 1 calc R . . C6 C -0.5757(4) 0.2896(3) 0.0651(3) 0.0624(9) Uani 1 1 d . . . H6A H -0.6499 0.2304 0.1293 0.075 Uiso 1 1 calc R . . H6B H -0.6257 0.3481 0.016 0.075 Uiso 1 1 calc R . . C7 C -0.4789(4) 0.2234(4) -0.0095(3) 0.0638(9) Uani 1 1 d . . . H7A H -0.4205 0.2831 -0.0839 0.077 Uiso 1 1 calc R . . H7B H -0.537 0.1673 -0.0318 0.077 Uiso 1 1 calc R . . C8 C -0.3930(2) -0.2494(2) 0.29368(19) 0.0256(4) Uani 1 1 d . . . C9 C -0.4920(3) -0.1598(2) 0.2782(2) 0.0349(5) Uani 1 1 d . . . H9 H -0.4587 -0.0754 0.2479 0.042 Uiso 1 1 calc R . . C10 C -0.6394(3) -0.1939(3) 0.3070(3) 0.0456(7) Uani 1 1 d . . . H10 H -0.7056 -0.1326 0.2977 0.055 Uiso 1 1 calc R . . C11 C -0.6890(3) -0.3174(3) 0.3494(3) 0.0464(7) Uani 1 1 d . . . H11 H -0.7889 -0.3404 0.3684 0.056 Uiso 1 1 calc R . . C12 C -0.5923(3) -0.4071(3) 0.3638(3) 0.0456(7) Uani 1 1 d . . . H12 H -0.626 -0.4914 0.3921 0.055 Uiso 1 1 calc R . . C13 C -0.4446(3) -0.3734(2) 0.3366(2) 0.0364(5) Uani 1 1 d . . . H13 H -0.3792 -0.4353 0.3474 0.044 Uiso 1 1 calc R . . C14 C -0.0971(2) -0.3281(2) 0.2417(2) 0.0285(5) Uani 1 1 d . . . C15 C -0.0187(3) -0.3300(2) 0.1260(2) 0.0426(6) Uani 1 1 d . . . H15 H -0.0229 -0.2647 0.0594 0.051 Uiso 1 1 calc R . . C16 C 0.0663(3) -0.4286(3) 0.1080(3) 0.0564(8) Uani 1 1 d . . . H16 H 0.1178 -0.4302 0.0293 0.068 Uiso 1 1 calc R . . C17 C 0.0746(3) -0.5236(3) 0.2056(3) 0.0544(8) Uani 1 1 d . . . H17 H 0.1326 -0.5894 0.1934 0.065 Uiso 1 1 calc R . . C18 C -0.0015(3) -0.5221(2) 0.3203(3) 0.0471(7) Uani 1 1 d . . . H18 H 0.0046 -0.5869 0.3866 0.056 Uiso 1 1 calc R . . C19 C -0.0874(3) -0.4253(2) 0.3389(2) 0.0352(5) Uani 1 1 d . . . H19 H -0.1397 -0.4253 0.4178 0.042 Uiso 1 1 calc R . . C20 C -0.1920(2) -0.1787(2) 0.40265(19) 0.0265(4) Uani 1 1 d . . . C21 C -0.3129(3) -0.1629(3) 0.4919(2) 0.0449(7) Uani 1 1 d . . . H21 H -0.4063 -0.1675 0.4822 0.054 Uiso 1 1 calc R . . C22 C -0.2970(3) -0.1402(3) 0.5957(3) 0.0573(8) Uani 1 1 d . . . H22 H -0.3797 -0.129 0.6554 0.069 Uiso 1 1 calc R . . C23 C -0.1613(3) -0.1339(3) 0.6117(2) 0.0485(7) Uani 1 1 d . . . H23 H -0.1513 -0.1201 0.6827 0.058 Uiso 1 1 calc R . . C24 C -0.0404(3) -0.1478(2) 0.5230(2) 0.0393(6) Uani 1 1 d . . . H24 H 0.0526 -0.143 0.5334 0.047 Uiso 1 1 calc R . . C25 C -0.0548(3) -0.1688(2) 0.4187(2) 0.0330(5) Uani 1 1 d . . . H25 H 0.0288 -0.1764 0.3579 0.04 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 Cu 0.03149(15) 0.02544(14) 0.02672(15) -0.00634(11) -0.00668(12) 0.00285(11) Br 0.02704(12) 0.04764(15) 0.02742(12) -0.01661(10) -0.00927(9) 0.00195(10) P 0.0216(3) 0.0243(3) 0.0228(3) -0.0057(2) -0.0054(2) 0.0018(2) N1 0.0306(10) 0.0293(10) 0.0308(10) -0.0126(8) -0.0131(8) 0.0058(8) N2 0.0351(11) 0.0308(10) 0.0459(12) -0.0154(9) -0.0183(9) 0.0127(9) N3 0.0435(13) 0.0506(14) 0.0441(13) -0.0247(11) -0.0248(11) 0.0173(11) C1 0.0283(11) 0.0256(11) 0.0291(11) -0.0063(9) -0.0092(9) 0.0004(9) C2 0.0376(13) 0.0463(15) 0.0456(15) -0.0263(12) -0.0218(12) 0.0127(11) C3 0.0438(15) 0.0556(17) 0.0448(15) -0.0317(13) -0.0211(12) 0.0132(13) C4 0.0409(14) 0.0428(15) 0.0590(18) -0.0302(13) -0.0182(13) 0.0122(12) C5 0.0540(18) 0.0404(15) 0.078(2) -0.0172(15) -0.0364(17) 0.0199(14) C6 0.060(2) 0.062(2) 0.081(2) -0.0206(18) -0.0447(19) 0.0244(17) C7 0.0549(19) 0.097(3) 0.057(2) -0.0333(19) -0.0341(16) 0.0283(19) C8 0.0244(11) 0.0313(11) 0.0228(10) -0.0093(9) -0.0080(9) 0.0006(9) C9 0.0286(12) 0.0328(12) 0.0429(14) -0.0086(10) -0.0120(10) 0.0036(10) C10 0.0272(12) 0.0506(16) 0.0601(18) -0.0148(14) -0.0153(12) 0.0101(12) C11 0.0237(12) 0.0580(18) 0.0582(18) -0.0208(14) -0.0088(12) -0.0023(12) C12 0.0314(13) 0.0382(14) 0.0630(18) -0.0161(13) -0.0055(12) -0.0071(11) C13 0.0301(12) 0.0306(12) 0.0475(15) -0.0129(11) -0.0079(11) 0.0025(10) C14 0.0222(10) 0.0253(11) 0.0355(12) -0.0084(9) -0.0049(9) 0.0014(9) C15 0.0445(15) 0.0348(14) 0.0386(14) -0.0095(11) 0.0019(12) 0.0061(11) C16 0.0482(17) 0.0453(17) 0.062(2) -0.0213(15) 0.0102(14) 0.0084(14) C17 0.0382(15) 0.0323(14) 0.091(2) -0.0222(15) -0.0117(16) 0.0106(12) C18 0.0444(15) 0.0286(13) 0.069(2) -0.0081(13) -0.0237(15) 0.0074(12) C19 0.0350(13) 0.0273(12) 0.0430(14) -0.0064(10) -0.0140(11) 0.0035(10) C20 0.0276(11) 0.0260(11) 0.0248(11) -0.0038(8) -0.0092(9) -0.0015(9) C21 0.0289(13) 0.074(2) 0.0318(13) -0.0206(13) -0.0038(10) -0.0063(13) C22 0.0468(17) 0.094(3) 0.0313(14) -0.0290(16) -0.0008(12) -0.0080(16) C23 0.0580(18) 0.0582(18) 0.0312(14) -0.0105(12) -0.0177(13) -0.0118(14) C24 0.0439(14) 0.0371(13) 0.0432(15) -0.0066(11) -0.0268(12) 0.0016(11) C25 0.0312(12) 0.0344(12) 0.0358(13) -0.0095(10) -0.0138(10) 0.0063(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 Cu N1 2.0179(19) . ? Cu P 2.2111(6) . ? Cu Br 2.5272(3) 2 ? Cu Br 2.5807(4) . ? Br Cu 2.5272(3) 2 ? P C14 1.825(2) . ? P C20 1.830(2) . ? P C8 1.831(2) . ? N1 C1 1.305(3) . ? N1 C2 1.465(3) . ? N2 C1 1.359(3) . ? N2 C5 1.456(3) . ? N2 C4 1.457(3) . ? N3 C1 1.363(3) . ? N3 C7 1.457(4) . ? C2 C3 1.506(4) . ? C3 C4 1.500(4) . ? C5 C6 1.487(4) . ? C6 C7 1.447(5) . ? C8 C13 1.387(3) . ? C8 C9 1.391(3) . ? C9 C10 1.387(3) . ? C10 C11 1.377(4) . ? C11 C12 1.375(4) . ? C12 C13 1.391(3) . ? C14 C15 1.388(3) . ? C14 C19 1.394(3) . ? C15 C16 1.396(4) . ? C16 C17 1.380(5) . ? C17 C18 1.370(4) . ? C18 C19 1.387(4) . ? C20 C21 1.386(3) . ? C20 C25 1.394(3) . ? C21 C22 1.389(4) . ? C22 C23 1.375(4) . ? C23 C24 1.375(4) . ? C24 C25 1.384(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu P 115.42(6) . . ? N1 Cu Br 113.69(5) . 2 ? P Cu Br 113.367(19) . 2 ? N1 Cu Br 101.70(5) . . ? P Cu Br 106.136(18) . . ? Br Cu Br 104.868(11) 2 . ? Cu Br Cu 75.132(11) 2 . ? C14 P C20 102.38(10) . . ? C14 P C8 105.74(10) . . ? C20 P C8 102.11(10) . . ? C14 P Cu 118.44(8) . . ? C20 P Cu 110.82(7) . . ? C8 P Cu 115.39(7) . . ? C1 N1 C2 118.07(19) . . ? C1 N1 Cu 126.72(15) . . ? C2 N1 Cu 114.96(15) . . ? C1 N2 C5 122.5(2) . . ? C1 N2 C4 120.17(19) . . ? C5 N2 C4 115.8(2) . . ? C1 N3 C7 122.7(3) . . ? N1 C1 N2 125.1(2) . . ? N1 C1 N3 118.0(2) . . ? N2 C1 N3 116.8(2) . . ? N1 C2 C3 112.1(2) . . ? C4 C3 C2 109.2(2) . . ? N2 C4 C3 110.1(2) . . ? N2 C5 C6 112.3(2) . . ? C7 C6 C5 111.5(3) . . ? C6 C7 N3 112.1(3) . . ? C13 C8 C9 118.6(2) . . ? C13 C8 P 124.29(18) . . ? C9 C8 P 117.11(17) . . ? C10 C9 C8 120.6(2) . . ? C11 C10 C9 120.2(2) . . ? C12 C11 C10 119.8(2) . . ? C11 C12 C13 120.3(2) . . ? C8 C13 C12 120.5(2) . . ? C15 C14 C19 118.6(2) . . ? C15 C14 P 117.56(18) . . ? C19 C14 P 123.79(19) . . ? C14 C15 C16 120.3(3) . . ? C17 C16 C15 120.0(3) . . ? C18 C17 C16 120.2(3) . . ? C17 C18 C19 120.2(3) . . ? C18 C19 C14 120.7(3) . . ? C21 C20 C25 118.4(2) . . ? C21 C20 P 122.96(17) . . ? C25 C20 P 118.28(18) . . ? C20 C21 C22 120.4(2) . . ? C23 C22 C21 120.5(3) . . ? C22 C23 C24 119.6(2) . . ? C23 C24 C25 120.4(2) . . ? C24 C25 C20 120.7(2) . . ? #===END data_((8)-nov802 _database_code_depnum_ccdc_archive 'CCDC 224313' _audit_creation_date 2002-11-05T10:54:07-00:00 _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_name_common [{CuI(PPh3)(C7H13N3)}2] _chemical_formula_moiety 'C50 H56 Cu2 I2 N6 P2' _chemical_formula_sum 'C50 H56 Cu2 I2 N6 P2' _chemical_formula_weight 1183.83 _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 9.6964(2) _cell_length_b 11.2108(2) _cell_length_c 12.2893(2) _cell_angle_alpha 74.032(1) _cell_angle_beta 72.476(1) _cell_angle_gamma 89.277(1) _cell_volume 1221.15(4) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6894 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.878 _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 1.61 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.241 _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 0.5918 _exptl_absorpt_correction_T_max 0.6526 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 223(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 0.0345 _diffrn_reflns_av_unetI/netI 0.0339 _diffrn_reflns_number 12510 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 27.89 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _reflns_number_total 5758 _reflns_number_gt 5282 _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^)+(0.0162P)^2^+0.7880P] 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 'H on N3 refined; others riding' _refine_ls_extinction_method none _refine_ls_number_reflns 5758 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0282 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0596 _refine_ls_wR_factor_gt 0.0579 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.422 _refine_diff_density_min -0.731 _refine_diff_density_rms 0.074 #----------------------------------------------------------------------------# # 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 Cu Cu -0.13079(3) -0.01027(2) 0.11707(2) 0.02767(6) Uani 1 1 d . . . I I 0.155601(14) 0.035625(13) 0.086877(11) 0.03135(5) Uani 1 1 d . . . P P -0.19926(5) -0.19228(4) 0.25826(4) 0.02275(10) Uani 1 1 d . . . N1 N -0.21952(19) 0.13752(16) 0.16928(16) 0.0297(4) Uani 1 1 d . . . N2 N -0.3908(2) 0.28900(17) 0.18879(18) 0.0374(4) Uani 1 1 d . . . N3 N -0.3782(2) 0.1691(2) 0.06023(19) 0.0416(5) Uani 1 1 d . . . H3 H -0.329(3) 0.126(2) 0.028(2) 0.029(6) Uiso 1 1 d . . . C1 C -0.3247(2) 0.19941(18) 0.14019(18) 0.0286(4) Uani 1 1 d . . . C2 C -0.1619(3) 0.1705(2) 0.2556(2) 0.0380(5) Uani 1 1 d . . . H2A H -0.0798 0.233 0.2128 0.046 Uiso 1 1 calc R . . H2B H -0.126 0.0965 0.2995 0.046 Uiso 1 1 calc R . . C3 C -0.2743(3) 0.2211(3) 0.3425(2) 0.0480(6) Uani 1 1 d . . . H3A H -0.2292 0.2503 0.3929 0.058 Uiso 1 1 calc R . . H3B H -0.3501 0.1554 0.3939 0.058 Uiso 1 1 calc R . . C4 C -0.3401(3) 0.3271(2) 0.2750(3) 0.0480(6) Uani 1 1 d . . . H4A H -0.4215 0.3535 0.3308 0.058 Uiso 1 1 calc R . . H4B H -0.2676 0.398 0.2337 0.058 Uiso 1 1 calc R . . C5 C -0.4959(3) 0.3660(2) 0.1443(3) 0.0539(7) Uani 1 1 d . . . H5A H -0.4455 0.4437 0.0869 0.065 Uiso 1 1 calc R . . H5B H -0.5669 0.3872 0.2107 0.065 Uiso 1 1 calc R . . C6 C -0.5741(3) 0.3013(3) 0.0854(2) 0.0471(6) Uani 1 1 d . . . H6A H -0.6419 0.2342 0.1458 0.056 Uiso 1 1 calc R . . H6B H -0.6299 0.3605 0.0442 0.056 Uiso 1 1 calc R . . C7 C -0.4669(3) 0.2487(3) -0.0019(2) 0.0473(6) Uani 1 1 d . . . H7A H -0.5178 0.2003 -0.0355 0.057 Uiso 1 1 calc R . . H7B H -0.4055 0.3162 -0.0672 0.057 Uiso 1 1 calc R . . C8 C -0.3881(2) -0.24853(19) 0.29187(17) 0.0258(4) Uani 1 1 d . . . C9 C -0.4853(2) -0.1600(2) 0.2683(2) 0.0367(5) Uani 1 1 d . . . H9 H -0.4515 -0.0757 0.2335 0.044 Uiso 1 1 calc R . . C10 C -0.6311(3) -0.1943(3) 0.2954(2) 0.0458(6) Uani 1 1 d . . . H10 H -0.696 -0.1335 0.2807 0.055 Uiso 1 1 calc R . . C11 C -0.6811(3) -0.3189(3) 0.3443(2) 0.0462(6) Uani 1 1 d . . . H11 H -0.7799 -0.3427 0.3623 0.055 Uiso 1 1 calc R . . C12 C -0.5858(3) -0.4071(2) 0.3663(3) 0.0479(6) Uani 1 1 d . . . H12 H -0.6196 -0.4916 0.3987 0.058 Uiso 1 1 calc R . . C13 C -0.4403(2) -0.3728(2) 0.3413(2) 0.0390(5) Uani 1 1 d . . . H13 H -0.3764 -0.434 0.3578 0.047 Uiso 1 1 calc R . . C14 C -0.0939(2) -0.32711(18) 0.24339(19) 0.0289(4) Uani 1 1 d . . . C15 C -0.0165(3) -0.3313(2) 0.1300(2) 0.0432(6) Uani 1 1 d . . . H15 H -0.0202 -0.2668 0.0635 0.052 Uiso 1 1 calc R . . C16 C 0.0671(3) -0.4310(3) 0.1141(3) 0.0585(8) Uani 1 1 d . . . H16 H 0.1196 -0.4333 0.0368 0.07 Uiso 1 1 calc R . . C17 C 0.0732(3) -0.5259(2) 0.2107(3) 0.0577(8) Uani 1 1 d . . . H17 H 0.1287 -0.5934 0.1993 0.069 Uiso 1 1 calc R . . C18 C -0.0020(3) -0.5221(2) 0.3239(3) 0.0492(7) Uani 1 1 d . . . H18 H 0.0033 -0.5865 0.3899 0.059 Uiso 1 1 calc R . . C19 C -0.0859(2) -0.4234(2) 0.3412(2) 0.0364(5) Uani 1 1 d . . . H19 H -0.1373 -0.4214 0.4188 0.044 Uiso 1 1 calc R . . C20 C -0.1952(2) -0.17681(18) 0.40163(17) 0.0268(4) Uani 1 1 d . . . C21 C -0.3166(3) -0.1546(3) 0.4852(2) 0.0423(5) Uani 1 1 d . . . H21 H -0.4077 -0.1568 0.4733 0.051 Uiso 1 1 calc R . . C22 C -0.3051(3) -0.1291(3) 0.5867(2) 0.0571(7) Uani 1 1 d . . . H22 H -0.3884 -0.1133 0.6425 0.069 Uiso 1 1 calc R . . C23 C -0.1724(3) -0.1267(3) 0.6062(2) 0.0526(7) Uani 1 1 d . . . H23 H -0.1652 -0.1108 0.6756 0.063 Uiso 1 1 calc R . . C24 C -0.0508(3) -0.1477(2) 0.5230(2) 0.0434(6) Uani 1 1 d . . . H24 H 0.04 -0.1459 0.5357 0.052 Uiso 1 1 calc R . . C25 C -0.0606(2) -0.1717(2) 0.4208(2) 0.0337(5) Uani 1 1 d . . . H25 H 0.0236 -0.1845 0.364 0.04 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 Cu 0.03270(14) 0.02507(12) 0.02682(13) -0.00804(10) -0.01098(11) 0.00438(10) I 0.02665(8) 0.04669(9) 0.02683(7) -0.01678(6) -0.01142(5) 0.00417(5) P 0.0226(2) 0.0235(2) 0.0230(2) -0.00702(18) -0.00797(19) 0.00361(17) N1 0.0326(9) 0.0291(8) 0.0330(9) -0.0139(7) -0.0139(7) 0.0076(7) N2 0.0375(10) 0.0317(9) 0.0500(11) -0.0185(9) -0.0181(9) 0.0123(8) N3 0.0449(12) 0.0496(12) 0.0445(11) -0.0241(10) -0.0252(10) 0.0220(10) C1 0.0289(10) 0.0240(9) 0.0311(10) -0.0071(8) -0.0074(8) 0.0022(7) C2 0.0368(12) 0.0442(13) 0.0466(13) -0.0273(11) -0.0198(10) 0.0121(10) C3 0.0446(14) 0.0633(16) 0.0541(15) -0.0379(13) -0.0225(12) 0.0177(12) C4 0.0450(14) 0.0442(13) 0.0696(17) -0.0373(13) -0.0206(13) 0.0146(11) C5 0.0537(16) 0.0381(13) 0.0753(19) -0.0163(13) -0.0281(15) 0.0204(12) C6 0.0385(13) 0.0511(15) 0.0501(14) -0.0076(12) -0.0181(12) 0.0138(11) C7 0.0408(14) 0.0634(16) 0.0386(13) -0.0093(12) -0.0187(11) 0.0139(12) C8 0.0239(9) 0.0313(10) 0.0254(9) -0.0116(8) -0.0090(8) 0.0038(7) C9 0.0321(11) 0.0385(12) 0.0381(12) -0.0048(9) -0.0145(10) 0.0053(9) C10 0.0308(12) 0.0563(15) 0.0506(14) -0.0091(12) -0.0192(11) 0.0123(10) C11 0.0246(11) 0.0637(16) 0.0542(15) -0.0227(13) -0.0125(11) -0.0001(10) C12 0.0324(12) 0.0419(13) 0.0676(17) -0.0210(12) -0.0076(12) -0.0041(10) C13 0.0294(11) 0.0305(11) 0.0576(15) -0.0161(10) -0.0110(10) 0.0039(8) C14 0.0229(9) 0.0252(9) 0.0374(11) -0.0093(8) -0.0074(8) 0.0031(7) C15 0.0409(13) 0.0344(12) 0.0447(13) -0.0122(10) 0.0015(11) 0.0065(10) C16 0.0502(16) 0.0456(15) 0.0670(18) -0.0250(14) 0.0083(14) 0.0104(12) C17 0.0378(14) 0.0334(13) 0.097(2) -0.0235(14) -0.0103(15) 0.0121(10) C18 0.0431(14) 0.0283(11) 0.0765(19) -0.0073(12) -0.0261(14) 0.0094(10) C19 0.0344(11) 0.0293(10) 0.0451(13) -0.0066(9) -0.0153(10) 0.0049(9) C20 0.0314(10) 0.0246(9) 0.0236(9) -0.0027(7) -0.0112(8) -0.0013(7) C21 0.0349(12) 0.0627(16) 0.0298(11) -0.0174(11) -0.0064(10) -0.0065(11) C22 0.0522(16) 0.087(2) 0.0310(12) -0.0269(13) -0.0007(11) -0.0136(14) C23 0.0699(19) 0.0599(17) 0.0298(12) -0.0091(11) -0.0206(13) -0.0184(14) C24 0.0549(15) 0.0394(12) 0.0428(13) -0.0037(10) -0.0321(12) -0.0056(11) C25 0.0356(11) 0.0317(10) 0.0372(11) -0.0071(9) -0.0185(10) 0.0030(8) #----------------------------------------------------------------------------# # 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 Cu N1 2.0282(17) . ? Cu P 2.2377(5) . ? Cu I 2.6791(3) 2 ? Cu I 2.7248(3) . ? I Cu 2.6791(3) 2 ? P C20 1.829(2) . ? P C8 1.830(2) . ? P C14 1.833(2) . ? N1 C1 1.310(3) . ? N1 C2 1.466(3) . ? N2 C1 1.364(3) . ? N2 C4 1.454(3) . ? N2 C5 1.462(3) . ? N3 C1 1.358(3) . ? N3 C7 1.456(3) . ? C2 C3 1.506(3) . ? C3 C4 1.505(4) . ? C5 C6 1.502(4) . ? C6 C7 1.497(4) . ? C8 C13 1.391(3) . ? C8 C9 1.393(3) . ? C9 C10 1.384(3) . ? C10 C11 1.387(4) . ? C11 C12 1.374(4) . ? C12 C13 1.386(3) . ? C14 C15 1.383(3) . ? C14 C19 1.399(3) . ? C15 C16 1.395(3) . ? C16 C17 1.375(4) . ? C17 C18 1.375(4) . ? C18 C19 1.390(3) . ? C20 C21 1.381(3) . ? C20 C25 1.399(3) . ? C21 C22 1.389(3) . ? C22 C23 1.380(4) . ? C23 C24 1.375(4) . ? C24 C25 1.384(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu P 113.85(5) . . ? N1 Cu I 116.96(5) . 2 ? P Cu I 109.021(16) . 2 ? N1 Cu I 102.20(5) . . ? P Cu I 105.548(15) . . ? I Cu I 108.285(9) 2 . ? Cu I Cu 71.715(9) 2 . ? C20 P C8 102.25(9) . . ? C20 P C14 102.81(10) . . ? C8 P C14 105.16(9) . . ? C20 P Cu 110.55(6) . . ? C8 P Cu 114.51(7) . . ? C14 P Cu 119.60(7) . . ? C1 N1 C2 118.33(17) . . ? C1 N1 Cu 127.69(14) . . ? C2 N1 Cu 113.85(13) . . ? C1 N2 C4 120.17(18) . . ? C1 N2 C5 123.0(2) . . ? C4 N2 C5 115.95(19) . . ? C1 N3 C7 123.6(2) . . ? N1 C1 N3 118.47(18) . . ? N1 C1 N2 124.81(19) . . ? N3 C1 N2 116.64(19) . . ? N1 C2 C3 112.33(18) . . ? C2 C3 C4 109.3(2) . . ? N2 C4 C3 110.25(19) . . ? N2 C5 C6 112.1(2) . . ? C7 C6 C5 109.8(2) . . ? N3 C7 C6 108.2(2) . . ? C13 C8 C9 118.44(19) . . ? C13 C8 P 124.22(16) . . ? C9 C8 P 117.33(16) . . ? C10 C9 C8 120.9(2) . . ? C9 C10 C11 119.8(2) . . ? C12 C11 C10 119.7(2) . . ? C11 C12 C13 120.6(2) . . ? C12 C13 C8 120.5(2) . . ? C15 C14 C19 119.0(2) . . ? C15 C14 P 117.99(17) . . ? C19 C14 P 123.00(17) . . ? C14 C15 C16 120.2(2) . . ? C17 C16 C15 120.4(3) . . ? C16 C17 C18 120.0(2) . . ? C17 C18 C19 120.3(2) . . ? C18 C19 C14 120.2(2) . . ? C21 C20 C25 118.6(2) . . ? C21 C20 P 122.61(16) . . ? C25 C20 P 118.33(16) . . ? C20 C21 C22 120.6(2) . . ? C23 C22 C21 120.5(3) . . ? C24 C23 C22 119.3(2) . . ? C23 C24 C25 120.7(2) . . ? C24 C25 C20 120.3(2) . . ? #===END