# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Tsipis, Athanassios' _publ_contact_author_email attsipis@cc.uoi.gr _publ_section_title ; Structural and electronic properties of luminescent copper(I) halide complexes of bis[2-(diphenylphosphano)phenyl] ether (DPEphos). Crystal structure of [CuCl(DPEphos)(dmpymtH] ; loop_ _publ_author_name A.Tsipis P.Aslanidis P.Cox # Attachment '- newa4.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-06-09 at 13:43:44 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.reqdat # CIF files read : cucl absorb info struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_cucl _database_code_depnum_ccdc_archive 'CCDC 768855' #TrackingRef '- newa4.cif' _audit_creation_date 2010-06-09T13:43:44-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C42 H36 Cl1 Cu1 N2 O1 P2 S1' _chemical_formula_sum 'C42.25 H36.75 Cl Cu N2 O1.13 P2 S' _chemical_formula_weight 783.48 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _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 15.3542(2) _cell_length_b 16.8655(4) _cell_length_c 14.7534(3) _cell_angle_alpha 90 _cell_angle_beta 100.3890(12) _cell_angle_gamma 90 _cell_volume 3757.85(13) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 29469 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1621 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.83 _exptl_absorpt_correction_type sphere _exptl_absorpt_process_details 'SADABS V.2007/2 (Sheldrick, G.M., 2007)' _exptl_absorpt_correction_T_min 0.8150 _exptl_absorpt_correction_T_max 0.9366 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 9.091 _diffrn_measurement_device_type ; Bruker-Nonius KappaCCD Area Detector ; _diffrn_measurement_method ; \f and \w scans ; _diffrn_standards_number 0 _diffrn_standards_decay_% negligible _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_unetI/netI 0.0418 _diffrn_reflns_number 39667 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 8557 _reflns_number_gt 7256 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; DENZO (Otwinowski and Minor, 1997), COLLECT (Hooft, 1998) ; _computing_cell_refinement 'DENZO and COLLECT' _computing_data_reduction 'DENZO and COLLECT' _computing_structure_solution 'SIR97 (Altomare et al.,1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; PLATON (Spek,2002) ; _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^)+(0.0228P)^2^+9.1795P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 8557 _refine_ls_number_parameters 453 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0613 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.107 _refine_ls_wR_factor_gt 0.1008 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.556 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.084 #----------------------------------------------------------------------------# # 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' 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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' 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 Cu1 Cu 0.19934(2) 0.05203(2) 0.20488(2) 0.01689(9) Uani 1 1 d . . . Cl1 Cl 0.20934(4) 0.19078(4) 0.18708(5) 0.02214(15) Uani 1 1 d . . . S1 S 0.06998(5) 0.02269(4) 0.25832(6) 0.02526(17) Uani 1 1 d . . . P1 P 0.31979(4) 0.02922(4) 0.31886(5) 0.01629(15) Uani 1 1 d . . . P2 P 0.21896(4) -0.01931(4) 0.07861(5) 0.01606(14) Uani 1 1 d . . . O1 O 0.27888(12) -0.13263(11) 0.22735(13) 0.0190(4) Uani 1 1 d . . . N1 N -0.07015(16) 0.09444(16) 0.30288(19) 0.0283(6) Uani 1 1 d . . . N2 N 0.03527(16) 0.17779(15) 0.25649(17) 0.0236(5) Uani 1 1 d . . . H2 H 0.0867 0.1831 0.2388 0.028 Uiso 1 1 calc R . . C1 C 0.00770(19) 0.10362(18) 0.2732(2) 0.0225(6) Uani 1 1 d . . . C2 C -0.11737(19) 0.1592(2) 0.3140(2) 0.0293(7) Uani 1 1 d . . . C3 C -0.0907(2) 0.2349(2) 0.2954(2) 0.0307(7) Uani 1 1 d . . . H3 H -0.1263 0.2796 0.3032 0.037 Uiso 1 1 calc R . . C4 C -0.0122(2) 0.24391(19) 0.2656(2) 0.0273(7) Uani 1 1 d . . . C5 C -0.2014(2) 0.1452(2) 0.3509(3) 0.0431(9) Uani 1 1 d . . . H5A H -0.1867 0.1247 0.4139 0.052 Uiso 1 1 calc R . . H5B H -0.2383 0.1066 0.3118 0.052 Uiso 1 1 calc R . . H5C H -0.2338 0.1953 0.3509 0.052 Uiso 1 1 calc R . . C6 C 0.0265(2) 0.3208(2) 0.2458(3) 0.0408(9) Uani 1 1 d . . . H6A H 0.0681 0.3386 0.3003 0.049 Uiso 1 1 calc R . . H6B H -0.0209 0.3601 0.2301 0.049 Uiso 1 1 calc R . . H6C H 0.0577 0.3148 0.1939 0.049 Uiso 1 1 calc R . . C7 C 0.13766(17) -0.09692(16) 0.03925(18) 0.0172(5) Uani 1 1 d . . . C8 C 0.04967(18) -0.08469(17) 0.04725(19) 0.0208(6) Uani 1 1 d . . . H8 H 0.0335 -0.0375 0.0752 0.025 Uiso 1 1 calc R . . C9 C -0.01463(19) -0.1407(2) 0.0149(2) 0.0283(7) Uani 1 1 d . . . H9 H -0.0746 -0.1312 0.0199 0.034 Uiso 1 1 calc R . . C10 C 0.0079(2) -0.21002(19) -0.0245(2) 0.0287(7) Uani 1 1 d . . . H10 H -0.0363 -0.2483 -0.0462 0.034 Uiso 1 1 calc R . . C11 C 0.0955(2) -0.22383(18) -0.0324(2) 0.0296(7) Uani 1 1 d . . . H11 H 0.1113 -0.2717 -0.0592 0.035 Uiso 1 1 calc R . . C12 C 0.15935(19) -0.16758(17) -0.0012(2) 0.0242(6) Uani 1 1 d . . . H12 H 0.219 -0.1771 -0.0072 0.029 Uiso 1 1 calc R . . C13 C 0.22650(17) 0.03506(16) -0.02705(19) 0.0175(5) Uani 1 1 d . . . C14 C 0.19582(19) 0.00500(18) -0.1156(2) 0.0231(6) Uani 1 1 d . . . H14 H 0.1671 -0.0451 -0.1231 0.028 Uiso 1 1 calc R . . C15 C 0.2075(2) 0.04847(19) -0.1923(2) 0.0287(7) Uani 1 1 d . . . H15 H 0.1867 0.0278 -0.2522 0.034 Uiso 1 1 calc R . . C16 C 0.2488(2) 0.12136(19) -0.1828(2) 0.0272(6) Uani 1 1 d . . . H16 H 0.2575 0.15 -0.2358 0.033 Uiso 1 1 calc R . . C17 C 0.27771(19) 0.15274(18) -0.0957(2) 0.0242(6) Uani 1 1 d . . . H17 H 0.305 0.2035 -0.0889 0.029 Uiso 1 1 calc R . . C18 C 0.26643(18) 0.10947(17) -0.0183(2) 0.0215(6) Uani 1 1 d . . . H18 H 0.2863 0.131 0.0414 0.026 Uiso 1 1 calc R . . C19 C 0.32409(17) -0.07479(16) 0.09670(19) 0.0168(5) Uani 1 1 d . . . C20 C 0.34337(17) -0.12550(16) 0.17232(19) 0.0177(5) Uani 1 1 d . . . C21 C 0.42203(18) -0.16811(17) 0.1910(2) 0.0224(6) Uani 1 1 d . . . H21 H 0.4327 -0.2039 0.2415 0.027 Uiso 1 1 calc R . . C22 C 0.48483(19) -0.15781(18) 0.1351(2) 0.0255(6) Uani 1 1 d . . . H22 H 0.5388 -0.1867 0.1472 0.031 Uiso 1 1 calc R . . C23 C 0.46900(18) -0.10580(18) 0.0620(2) 0.0237(6) Uani 1 1 d . . . H23 H 0.5129 -0.0975 0.0252 0.028 Uiso 1 1 calc R . . C24 C 0.38875(18) -0.06537(17) 0.0420(2) 0.0212(6) Uani 1 1 d . . . H24 H 0.3778 -0.0308 -0.0097 0.025 Uiso 1 1 calc R . . C25 C 0.33137(17) -0.06881(16) 0.37419(19) 0.0183(5) Uani 1 1 d . . . C26 C 0.35801(18) -0.07809(18) 0.4695(2) 0.0222(6) Uani 1 1 d . . . H26 H 0.372 -0.0324 0.5069 0.027 Uiso 1 1 calc R . . C27 C 0.36446(18) -0.15224(19) 0.5107(2) 0.0257(6) Uani 1 1 d . . . H27 H 0.3831 -0.157 0.5754 0.031 Uiso 1 1 calc R . . C28 C 0.34373(18) -0.21950(19) 0.4571(2) 0.0269(7) Uani 1 1 d . . . H28 H 0.349 -0.2704 0.4851 0.032 Uiso 1 1 calc R . . C29 C 0.31541(18) -0.21251(18) 0.3629(2) 0.0251(6) Uani 1 1 d . . . H29 H 0.3 -0.2584 0.3262 0.03 Uiso 1 1 calc R . . C30 C 0.30969(17) -0.13826(17) 0.32251(19) 0.0189(6) Uani 1 1 d . . . C31 C 0.42658(17) 0.04371(16) 0.28176(18) 0.0163(5) Uani 1 1 d . . . C32 C 0.50027(18) -0.00409(17) 0.30910(19) 0.0206(6) Uani 1 1 d . . . H32 H 0.4974 -0.0465 0.3509 0.025 Uiso 1 1 calc R . . C33 C 0.57804(19) 0.00936(19) 0.2761(2) 0.0255(6) Uani 1 1 d . . . H33 H 0.628 -0.0238 0.2951 0.031 Uiso 1 1 calc R . . C34 C 0.58283(19) 0.07146(19) 0.2151(2) 0.0265(6) Uani 1 1 d . . . H34 H 0.6356 0.0802 0.1915 0.032 Uiso 1 1 calc R . . C35 C 0.51034(19) 0.12040(18) 0.1892(2) 0.0248(6) Uani 1 1 d . . . H35 H 0.514 0.1636 0.1487 0.03 Uiso 1 1 calc R . . C36 C 0.43246(18) 0.10691(17) 0.2216(2) 0.0218(6) Uani 1 1 d . . . H36 H 0.3829 0.1406 0.2031 0.026 Uiso 1 1 calc R . . C37 C 0.32908(18) 0.09418(17) 0.41926(19) 0.0187(5) Uani 1 1 d . . . C38 C 0.40800(19) 0.13092(17) 0.4584(2) 0.0234(6) Uani 1 1 d . . . H38 H 0.4591 0.1246 0.4311 0.028 Uiso 1 1 calc R . . C39 C 0.4123(2) 0.17689(18) 0.5375(2) 0.0259(6) Uani 1 1 d . . . H39 H 0.4664 0.2019 0.5638 0.031 Uiso 1 1 calc R . . C40 C 0.3392(2) 0.18636(19) 0.5777(2) 0.0273(7) Uani 1 1 d . . . H40 H 0.3428 0.2171 0.6322 0.033 Uiso 1 1 calc R . . C41 C 0.2597(2) 0.1508(2) 0.5384(2) 0.0315(7) Uani 1 1 d . . . H41 H 0.2088 0.1576 0.5659 0.038 Uiso 1 1 calc R . . C42 C 0.2545(2) 0.1056(2) 0.4593(2) 0.0282(7) Uani 1 1 d . . . H42 H 0.1997 0.0822 0.4321 0.034 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01667(16) 0.01566(17) 0.01888(17) -0.00121(13) 0.00463(12) 0.00035(12) Cl1 0.0223(3) 0.0155(3) 0.0307(4) 0.0011(3) 0.0103(3) 0.0014(2) S1 0.0248(4) 0.0189(4) 0.0358(4) -0.0026(3) 0.0152(3) -0.0024(3) P1 0.0171(3) 0.0156(3) 0.0166(3) 0.0003(3) 0.0042(3) -0.0003(3) P2 0.0158(3) 0.0148(3) 0.0179(3) -0.0016(3) 0.0038(3) 0.0003(3) O1 0.0178(9) 0.0193(10) 0.0202(10) 0.0002(8) 0.0041(7) -0.0007(8) N1 0.0231(12) 0.0325(15) 0.0316(14) -0.0083(12) 0.0111(11) -0.0046(11) N2 0.0203(11) 0.0236(13) 0.0281(13) -0.0066(11) 0.0075(10) 0.0017(10) C1 0.0216(13) 0.0259(15) 0.0207(14) -0.0042(12) 0.0052(11) -0.0011(11) C2 0.0193(14) 0.0406(19) 0.0287(16) -0.0095(14) 0.0061(12) -0.0019(13) C3 0.0240(15) 0.0346(18) 0.0335(18) -0.0098(14) 0.0047(13) 0.0044(13) C4 0.0272(15) 0.0258(16) 0.0295(17) -0.0049(13) 0.0066(13) 0.0017(12) C5 0.0233(16) 0.051(2) 0.058(2) -0.0149(19) 0.0169(16) -0.0049(16) C6 0.042(2) 0.0262(18) 0.058(2) -0.0009(17) 0.0203(18) 0.0091(15) C7 0.0185(12) 0.0157(13) 0.0169(13) 0.0014(10) 0.0014(10) 0.0004(10) C8 0.0196(13) 0.0214(14) 0.0214(14) 0.0013(11) 0.0030(11) 0.0031(11) C9 0.0175(13) 0.0353(18) 0.0306(17) 0.0058(14) 0.0000(12) 0.0017(12) C10 0.0239(14) 0.0244(16) 0.0339(17) -0.0019(13) -0.0054(13) -0.0066(12) C11 0.0304(16) 0.0204(15) 0.0361(18) -0.0057(13) 0.0012(13) 0.0003(12) C12 0.0194(13) 0.0203(15) 0.0332(16) -0.0062(12) 0.0052(12) 0.0009(11) C13 0.0157(12) 0.0167(13) 0.0210(14) -0.0012(11) 0.0057(10) 0.0023(10) C14 0.0270(15) 0.0206(14) 0.0209(14) -0.0019(12) 0.0024(11) -0.0005(12) C15 0.0374(17) 0.0296(17) 0.0180(14) -0.0015(13) 0.0027(12) -0.0007(14) C16 0.0322(16) 0.0279(16) 0.0222(15) 0.0038(12) 0.0070(12) 0.0025(13) C17 0.0260(14) 0.0206(15) 0.0273(16) -0.0006(12) 0.0082(12) -0.0022(12) C18 0.0232(13) 0.0220(14) 0.0197(14) -0.0016(11) 0.0049(11) -0.0013(11) C19 0.0162(12) 0.0129(12) 0.0212(14) -0.0065(10) 0.0032(10) -0.0002(10) C20 0.0175(12) 0.0150(13) 0.0209(14) -0.0059(11) 0.0038(10) -0.0018(10) C21 0.0219(13) 0.0197(14) 0.0246(15) -0.0041(12) 0.0011(11) 0.0000(11) C22 0.0190(13) 0.0274(16) 0.0300(16) -0.0091(13) 0.0045(12) 0.0049(12) C23 0.0180(13) 0.0267(16) 0.0285(16) -0.0083(13) 0.0099(11) -0.0022(11) C24 0.0201(13) 0.0201(14) 0.0243(15) -0.0033(11) 0.0064(11) -0.0024(11) C25 0.0155(12) 0.0188(14) 0.0215(14) 0.0047(11) 0.0061(10) 0.0017(10) C26 0.0204(13) 0.0277(15) 0.0189(14) 0.0024(12) 0.0044(11) -0.0001(11) C27 0.0173(13) 0.0370(18) 0.0237(15) 0.0121(13) 0.0061(11) -0.0006(12) C28 0.0194(14) 0.0250(16) 0.0357(17) 0.0139(13) 0.0039(12) -0.0008(12) C29 0.0205(13) 0.0200(14) 0.0349(17) 0.0023(13) 0.0051(12) -0.0025(11) C30 0.0157(12) 0.0208(14) 0.0207(14) 0.0031(11) 0.0043(10) 0.0003(10) C31 0.0175(12) 0.0174(13) 0.0141(12) -0.0037(10) 0.0034(10) -0.0012(10) C32 0.0219(13) 0.0207(14) 0.0192(14) -0.0002(11) 0.0034(11) -0.0011(11) C33 0.0186(13) 0.0290(16) 0.0294(16) -0.0047(13) 0.0057(12) 0.0030(12) C34 0.0226(14) 0.0327(17) 0.0266(16) -0.0042(13) 0.0107(12) -0.0041(12) C35 0.0290(15) 0.0233(15) 0.0234(15) 0.0053(12) 0.0077(12) -0.0054(12) C36 0.0210(13) 0.0206(14) 0.0237(15) -0.0005(12) 0.0037(11) -0.0014(11) C37 0.0207(13) 0.0194(14) 0.0157(13) -0.0002(11) 0.0025(10) 0.0000(11) C38 0.0240(14) 0.0209(15) 0.0249(15) -0.0029(12) 0.0037(11) 0.0036(11) C39 0.0266(15) 0.0239(15) 0.0251(15) -0.0053(12) -0.0011(12) -0.0007(12) C40 0.0344(16) 0.0263(16) 0.0203(15) -0.0051(12) 0.0028(12) 0.0057(13) C41 0.0292(16) 0.0387(19) 0.0288(17) -0.0068(14) 0.0111(13) 0.0030(14) C42 0.0225(14) 0.0360(18) 0.0269(16) -0.0075(14) 0.0064(12) 0.0003(13) #----------------------------------------------------------------------------# # 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 Cu1 P2 2.2829(8) . ? Cu1 P1 2.2966(7) . ? Cu1 S1 2.3186(8) . ? Cu1 Cl1 2.3629(7) . ? Cu1 O1 3.3400(19) . ? S1 C1 1.703(3) . ? P1 C37 1.827(3) . ? P1 C31 1.836(3) . ? P1 C25 1.838(3) . ? P1 P2 3.6948(10) . ? P2 C7 1.830(3) . ? P2 C13 1.830(3) . ? P2 C19 1.843(3) . ? O1 C20 1.394(3) . ? O1 C30 1.402(3) . ? N1 C2 1.337(4) . ? N1 C1 1.354(4) . ? N2 C4 1.352(4) . ? N2 C1 1.357(4) . ? N2 H2 0.88 . ? C2 C3 1.383(5) . ? C2 C5 1.506(4) . ? C3 C4 1.365(4) . ? C3 H3 0.95 . ? C4 C6 1.478(5) . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 C8 1.393(4) . ? C7 C12 1.399(4) . ? C8 C9 1.388(4) . ? C8 H8 0.95 . ? C9 C10 1.377(4) . ? C9 H9 0.95 . ? C10 C11 1.390(4) . ? C10 H10 0.95 . ? C11 C12 1.383(4) . ? C11 H11 0.95 . ? C12 H12 0.95 . ? C13 C18 1.392(4) . ? C13 C14 1.402(4) . ? C14 C15 1.386(4) . ? C14 H14 0.95 . ? C15 C16 1.379(4) . ? C15 H15 0.95 . ? C16 C17 1.386(4) . ? C16 H16 0.95 . ? C17 C18 1.393(4) . ? C17 H17 0.95 . ? C18 H18 0.95 . ? C19 C20 1.395(4) . ? C19 C24 1.397(4) . ? C20 C21 1.390(4) . ? C21 C22 1.389(4) . ? C21 H21 0.95 . ? C22 C23 1.377(4) . ? C22 H22 0.95 . ? C23 C24 1.393(4) . ? C23 H23 0.95 . ? C24 H24 0.95 . ? C25 C26 1.400(4) . ? C25 C30 1.405(4) . ? C26 C27 1.386(4) . ? C26 H26 0.95 . ? C27 C28 1.386(5) . ? C27 H27 0.95 . ? C28 C29 1.385(4) . ? C28 H28 0.95 . ? C29 C30 1.383(4) . ? C29 H29 0.95 . ? C31 C32 1.389(4) . ? C31 C36 1.400(4) . ? C32 C33 1.387(4) . ? C32 H32 0.95 . ? C33 C34 1.391(4) . ? C33 H33 0.95 . ? C34 C35 1.383(4) . ? C34 H34 0.95 . ? C35 C36 1.385(4) . ? C35 H35 0.95 . ? C36 H36 0.95 . ? C37 C38 1.390(4) . ? C37 C42 1.393(4) . ? C38 C39 1.392(4) . ? C38 H38 0.95 . ? C39 C40 1.371(4) . ? C39 H39 0.95 . ? C40 C41 1.389(4) . ? C40 H40 0.95 . ? C41 C42 1.385(4) . ? C41 H41 0.95 . ? C42 H42 0.95 . ? 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 P2 Cu1 P1 107.57(3) . . ? P2 Cu1 S1 114.34(3) . . ? P1 Cu1 S1 109.96(3) . . ? P2 Cu1 Cl1 114.24(3) . . ? P1 Cu1 Cl1 100.80(3) . . ? S1 Cu1 Cl1 109.03(3) . . ? P2 Cu1 O1 59.32(4) . . ? P1 Cu1 O1 62.57(4) . . ? S1 Cu1 O1 95.02(4) . . ? Cl1 Cu1 O1 154.77(4) . . ? C1 S1 Cu1 114.09(11) . . ? C37 P1 C31 102.62(12) . . ? C37 P1 C25 101.08(13) . . ? C31 P1 C25 103.42(12) . . ? C37 P1 Cu1 115.34(9) . . ? C31 P1 Cu1 113.82(9) . . ? C25 P1 Cu1 118.45(9) . . ? C37 P1 P2 150.28(9) . . ? C31 P1 P2 89.18(8) . . ? C25 P1 P2 102.53(9) . . ? Cu1 P1 P2 36.090(17) . . ? C7 P2 C13 103.44(12) . . ? C7 P2 C19 102.27(12) . . ? C13 P2 C19 100.92(12) . . ? C7 P2 Cu1 116.95(9) . . ? C13 P2 Cu1 117.96(9) . . ? C19 P2 Cu1 112.98(9) . . ? C7 P2 P1 127.37(9) . . ? C13 P2 P1 128.77(9) . . ? C19 P2 P1 76.65(9) . . ? Cu1 P2 P1 36.342(17) . . ? C20 O1 C30 116.3(2) . . ? C20 O1 Cu1 98.46(14) . . ? C30 O1 Cu1 102.35(15) . . ? C2 N1 C1 118.4(3) . . ? C4 N2 C1 123.4(3) . . ? C4 N2 H2 118.3 . . ? C1 N2 H2 118.3 . . ? N1 C1 N2 119.1(3) . . ? N1 C1 S1 119.9(2) . . ? N2 C1 S1 120.9(2) . . ? N1 C2 C3 122.9(3) . . ? N1 C2 C5 115.8(3) . . ? C3 C2 C5 121.2(3) . . ? C4 C3 C2 118.5(3) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? N2 C4 C3 117.6(3) . . ? N2 C4 C6 117.5(3) . . ? C3 C4 C6 124.9(3) . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C12 118.1(3) . . ? C8 C7 P2 118.9(2) . . ? C12 C7 P2 122.9(2) . . ? C9 C8 C7 120.7(3) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C10 C9 C8 120.4(3) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 119.9(3) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C12 C11 C10 119.7(3) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C7 121.2(3) . . ? C11 C12 H12 119.4 . . ? C7 C12 H12 119.4 . . ? C18 C13 C14 118.7(3) . . ? C18 C13 P2 117.8(2) . . ? C14 C13 P2 123.4(2) . . ? C15 C14 C13 119.9(3) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C16 C15 C14 120.9(3) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 120.0(3) . . ? C15 C16 H16 120 . . ? C17 C16 H16 120 . . ? C16 C17 C18 119.6(3) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C13 C18 C17 120.9(3) . . ? C13 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C20 C19 C24 117.5(2) . . ? C20 C19 P2 118.8(2) . . ? C24 C19 P2 123.6(2) . . ? C21 C20 O1 121.5(3) . . ? C21 C20 C19 121.8(3) . . ? O1 C20 C19 116.6(2) . . ? C22 C21 C20 119.3(3) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C23 C22 C21 120.1(3) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 120.2(3) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C23 C24 C19 121.0(3) . . ? C23 C24 H24 119.5 . . ? C19 C24 H24 119.5 . . ? C26 C25 C30 116.7(3) . . ? C26 C25 P1 122.3(2) . . ? C30 C25 P1 121.0(2) . . ? C27 C26 C25 121.7(3) . . ? C27 C26 H26 119.1 . . ? C25 C26 H26 119.1 . . ? C26 C27 C28 119.9(3) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C29 C28 C27 120.0(3) . . ? C29 C28 H28 120 . . ? C27 C28 H28 120 . . ? C30 C29 C28 119.6(3) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 O1 118.5(3) . . ? C29 C30 C25 122.1(3) . . ? O1 C30 C25 119.4(2) . . ? C32 C31 C36 118.9(2) . . ? C32 C31 P1 124.1(2) . . ? C36 C31 P1 117.0(2) . . ? C33 C32 C31 120.7(3) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C34 120.0(3) . . ? C32 C33 H33 120 . . ? C34 C33 H33 120 . . ? C35 C34 C33 119.7(3) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C36 120.5(3) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C35 C36 C31 120.2(3) . . ? C35 C36 H36 119.9 . . ? C31 C36 H36 119.9 . . ? C38 C37 C42 118.9(3) . . ? C38 C37 P1 122.6(2) . . ? C42 C37 P1 118.5(2) . . ? C37 C38 C39 120.2(3) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C40 C39 C38 120.6(3) . . ? C40 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C39 C40 C41 119.7(3) . . ? C39 C40 H40 120.2 . . ? C41 C40 H40 120.2 . . ? C42 C41 C40 120.1(3) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C41 C42 C37 120.5(3) . . ? C41 C42 H42 119.8 . . ? C37 C42 H42 119.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Cu1 S1 C1 -128.63(11) . . . . ? P1 Cu1 S1 C1 110.26(11) . . . . ? Cl1 Cu1 S1 C1 0.61(12) . . . . ? O1 Cu1 S1 C1 172.87(12) . . . . ? P2 Cu1 P1 C37 169.04(10) . . . . ? S1 Cu1 P1 C37 -65.87(10) . . . . ? Cl1 Cu1 P1 C37 49.12(10) . . . . ? O1 Cu1 P1 C37 -151.07(11) . . . . ? P2 Cu1 P1 C31 50.78(10) . . . . ? S1 Cu1 P1 C31 175.88(10) . . . . ? Cl1 Cu1 P1 C31 -69.13(10) . . . . ? O1 Cu1 P1 C31 90.67(10) . . . . ? P2 Cu1 P1 C25 -71.07(11) . . . . ? S1 Cu1 P1 C25 54.03(11) . . . . ? Cl1 Cu1 P1 C25 169.01(10) . . . . ? O1 Cu1 P1 C25 -31.18(11) . . . . ? S1 Cu1 P1 P2 125.10(4) . . . . ? Cl1 Cu1 P1 P2 -119.92(3) . . . . ? O1 Cu1 P1 P2 39.89(4) . . . . ? P1 Cu1 P2 C7 117.25(10) . . . . ? S1 Cu1 P2 C7 -5.18(10) . . . . ? Cl1 Cu1 P2 C7 -131.77(10) . . . . ? O1 Cu1 P2 C7 75.81(10) . . . . ? P1 Cu1 P2 C13 -118.34(10) . . . . ? S1 Cu1 P2 C13 119.23(10) . . . . ? Cl1 Cu1 P2 C13 -7.36(10) . . . . ? O1 Cu1 P2 C13 -159.78(11) . . . . ? P1 Cu1 P2 C19 -1.08(10) . . . . ? S1 Cu1 P2 C19 -123.51(10) . . . . ? Cl1 Cu1 P2 C19 109.90(10) . . . . ? O1 Cu1 P2 C19 -42.52(10) . . . . ? S1 Cu1 P2 P1 -122.43(4) . . . . ? Cl1 Cu1 P2 P1 110.98(3) . . . . ? O1 Cu1 P2 P1 -41.44(4) . . . . ? C37 P1 P2 C7 -105.9(2) . . . . ? C31 P1 P2 C7 139.48(14) . . . . ? C25 P1 P2 C7 35.92(14) . . . . ? Cu1 P1 P2 C7 -85.66(11) . . . . ? C37 P1 P2 C13 65.3(2) . . . . ? C31 P1 P2 C13 -49.27(14) . . . . ? C25 P1 P2 C13 -152.83(14) . . . . ? Cu1 P1 P2 C13 85.59(11) . . . . ? C37 P1 P2 C19 158.7(2) . . . . ? C31 P1 P2 C19 44.12(12) . . . . ? C25 P1 P2 C19 -59.45(12) . . . . ? Cu1 P1 P2 C19 178.98(10) . . . . ? C37 P1 P2 Cu1 -20.29(18) . . . . ? C31 P1 P2 Cu1 -134.86(9) . . . . ? C25 P1 P2 Cu1 121.58(9) . . . . ? P2 Cu1 O1 C20 48.22(13) . . . . ? P1 Cu1 O1 C20 -86.47(14) . . . . ? S1 Cu1 O1 C20 163.63(14) . . . . ? Cl1 Cu1 O1 C20 -33.77(19) . . . . ? P2 Cu1 O1 C30 167.59(15) . . . . ? P1 Cu1 O1 C30 32.90(13) . . . . ? S1 Cu1 O1 C30 -77.01(14) . . . . ? Cl1 Cu1 O1 C30 85.59(17) . . . . ? C2 N1 C1 N2 0.4(4) . . . . ? C2 N1 C1 S1 179.9(2) . . . . ? C4 N2 C1 N1 -1.7(4) . . . . ? C4 N2 C1 S1 178.8(2) . . . . ? Cu1 S1 C1 N1 179.0(2) . . . . ? Cu1 S1 C1 N2 -1.5(3) . . . . ? C1 N1 C2 C3 0.9(5) . . . . ? C1 N1 C2 C5 -177.5(3) . . . . ? N1 C2 C3 C4 -0.9(5) . . . . ? C5 C2 C3 C4 177.4(3) . . . . ? C1 N2 C4 C3 1.7(5) . . . . ? C1 N2 C4 C6 179.5(3) . . . . ? C2 C3 C4 N2 -0.3(5) . . . . ? C2 C3 C4 C6 -177.9(3) . . . . ? C13 P2 C7 C8 -96.5(2) . . . . ? C19 P2 C7 C8 158.9(2) . . . . ? Cu1 P2 C7 C8 34.9(2) . . . . ? P1 P2 C7 C8 76.5(2) . . . . ? C13 P2 C7 C12 81.6(3) . . . . ? C19 P2 C7 C12 -22.9(3) . . . . ? Cu1 P2 C7 C12 -146.9(2) . . . . ? P1 P2 C7 C12 -105.4(2) . . . . ? C12 C7 C8 C9 -0.8(4) . . . . ? P2 C7 C8 C9 177.4(2) . . . . ? C7 C8 C9 C10 1.0(5) . . . . ? C8 C9 C10 C11 -0.4(5) . . . . ? C9 C10 C11 C12 -0.4(5) . . . . ? C10 C11 C12 C7 0.6(5) . . . . ? C8 C7 C12 C11 0.0(4) . . . . ? P2 C7 C12 C11 -178.1(2) . . . . ? C7 P2 C13 C18 164.7(2) . . . . ? C19 P2 C13 C18 -89.7(2) . . . . ? Cu1 P2 C13 C18 33.8(2) . . . . ? P1 P2 C13 C18 -8.2(3) . . . . ? C7 P2 C13 C14 -16.6(3) . . . . ? C19 P2 C13 C14 89.0(2) . . . . ? Cu1 P2 C13 C14 -147.5(2) . . . . ? P1 P2 C13 C14 170.54(18) . . . . ? C18 C13 C14 C15 1.5(4) . . . . ? P2 C13 C14 C15 -177.2(2) . . . . ? C13 C14 C15 C16 -0.2(5) . . . . ? C14 C15 C16 C17 -1.3(5) . . . . ? C15 C16 C17 C18 1.4(5) . . . . ? C14 C13 C18 C17 -1.5(4) . . . . ? P2 C13 C18 C17 177.3(2) . . . . ? C16 C17 C18 C13 0.0(4) . . . . ? C7 P2 C19 C20 -72.8(2) . . . . ? C13 P2 C19 C20 -179.3(2) . . . . ? Cu1 P2 C19 C20 53.7(2) . . . . ? P1 P2 C19 C20 53.1(2) . . . . ? C7 P2 C19 C24 111.3(2) . . . . ? C13 P2 C19 C24 4.8(3) . . . . ? Cu1 P2 C19 C24 -122.1(2) . . . . ? P1 P2 C19 C24 -122.8(2) . . . . ? C30 O1 C20 C21 39.6(3) . . . . ? Cu1 O1 C20 C21 147.9(2) . . . . ? C30 O1 C20 C19 -141.7(2) . . . . ? Cu1 O1 C20 C19 -33.4(2) . . . . ? C24 C19 C20 C21 -2.8(4) . . . . ? P2 C19 C20 C21 -178.9(2) . . . . ? C24 C19 C20 O1 178.5(2) . . . . ? P2 C19 C20 O1 2.4(3) . . . . ? O1 C20 C21 C22 -178.9(2) . . . . ? C19 C20 C21 C22 2.5(4) . . . . ? C20 C21 C22 C23 0.1(4) . . . . ? C21 C22 C23 C24 -2.3(4) . . . . ? C22 C23 C24 C19 1.9(4) . . . . ? C20 C19 C24 C23 0.6(4) . . . . ? P2 C19 C24 C23 176.5(2) . . . . ? C37 P1 C25 C26 -10.7(3) . . . . ? C31 P1 C25 C26 95.3(2) . . . . ? Cu1 P1 C25 C26 -137.8(2) . . . . ? P2 P1 C25 C26 -172.6(2) . . . . ? C37 P1 C25 C30 166.3(2) . . . . ? C31 P1 C25 C30 -87.7(2) . . . . ? Cu1 P1 C25 C30 39.3(2) . . . . ? P2 P1 C25 C30 4.5(2) . . . . ? C30 C25 C26 C27 1.3(4) . . . . ? P1 C25 C26 C27 178.4(2) . . . . ? C25 C26 C27 C28 -0.4(4) . . . . ? C26 C27 C28 C29 -0.9(4) . . . . ? C27 C28 C29 C30 1.3(4) . . . . ? C28 C29 C30 O1 -178.5(2) . . . . ? C28 C29 C30 C25 -0.3(4) . . . . ? C20 O1 C30 C29 -98.9(3) . . . . ? Cu1 O1 C30 C29 155.1(2) . . . . ? C20 O1 C30 C25 82.9(3) . . . . ? Cu1 O1 C30 C25 -23.1(3) . . . . ? C26 C25 C30 C29 -0.9(4) . . . . ? P1 C25 C30 C29 -178.1(2) . . . . ? C26 C25 C30 O1 177.3(2) . . . . ? P1 C25 C30 O1 0.1(3) . . . . ? C37 P1 C31 C32 93.5(2) . . . . ? C25 P1 C31 C32 -11.3(3) . . . . ? Cu1 P1 C31 C32 -141.1(2) . . . . ? P2 P1 C31 C32 -114.0(2) . . . . ? C37 P1 C31 C36 -86.9(2) . . . . ? C25 P1 C31 C36 168.2(2) . . . . ? Cu1 P1 C31 C36 38.4(2) . . . . ? P2 P1 C31 C36 65.6(2) . . . . ? C36 C31 C32 C33 -1.3(4) . . . . ? P1 C31 C32 C33 178.2(2) . . . . ? C31 C32 C33 C34 0.2(4) . . . . ? C32 C33 C34 C35 1.2(5) . . . . ? C33 C34 C35 C36 -1.5(5) . . . . ? C34 C35 C36 C31 0.4(4) . . . . ? C32 C31 C36 C35 1.0(4) . . . . ? P1 C31 C36 C35 -178.6(2) . . . . ? C31 P1 C37 C38 -9.3(3) . . . . ? C25 P1 C37 C38 97.3(3) . . . . ? Cu1 P1 C37 C38 -133.6(2) . . . . ? P2 P1 C37 C38 -120.6(2) . . . . ? C31 P1 C37 C42 172.3(2) . . . . ? C25 P1 C37 C42 -81.1(3) . . . . ? Cu1 P1 C37 C42 48.0(3) . . . . ? P2 P1 C37 C42 61.0(3) . . . . ? C42 C37 C38 C39 1.4(4) . . . . ? P1 C37 C38 C39 -177.0(2) . . . . ? C37 C38 C39 C40 0.1(5) . . . . ? C38 C39 C40 C41 -1.1(5) . . . . ? C39 C40 C41 C42 0.4(5) . . . . ? C40 C41 C42 C37 1.1(5) . . . . ? C38 C37 C42 C41 -2.0(5) . . . . ? P1 C37 C42 C41 176.5(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 Cl1 0.88 2.16 3.038(2) 175.9 . # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.500 0.000 107.5 6.3 2 1.000 1.000 0.500 107.6 6.5 _platon_squeeze_details ; The unit cell contains 1/8 of a ethanol molecule, i.e., (12.8=13) electrons in total voids of 215.1 cubic Angstroms. This disorder has been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ;