Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' # PROCESSING SUMMARY (IUCr Office Use Only) _journal_coden_Cambridge 0222 #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Dr. Frank Breher' _publ_contact_author_address ; Department of Chemistry and Applied Biosciences ETH Hoenggerberg Wolgang-Pauli Str. CH-8093 Zuerich Switzerland ; _publ_contact_author_email breher@inorg.chem.ethz.ch _publ_contact_author_phone ? _publ_contact_author_fax '(+41) 1 633 10 32' loop_ _publ_author_name _publ_author_address I.Krummenacher ; Department of Chemistry and Applied Biosciences (D-CHAB) ETH Hoenggerberg Wolfgang-Pauli Str. CH-8093 Zuerich Switzerland ; H.Rueegger ; Department of Chemistry and Applied Biosciences (D-CHAB) ETH Hoenggerberg Wolfgang-Pauli Str. CH-8093 Zuerich Switzerland ; F.Breher ; Department of Chemistry and Applied Biosciences (D-CHAB) ETH Hoenggerberg Wolfgang-Pauli Str. CH-8093 Zuerich Switzerland ; #============================================================================== _audit_creation_method 'form.cif (version 2.0)' _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _publ_contact_letter ; ? ; _publ_requested_category FA #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Coinage metal complexes of tris(pyrazolyl)methanide ; _publ_section_title_footnote ; ? ; #============================================================================== # TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_acknowledgements ; ? ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; #============================================================================== # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. data_C(Mepz)3CuPPh3 _database_code_depnum_ccdc_archive 'CCDC 282767' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H36 Cu N6 P, 0.5(C6 H14)' _chemical_formula_sum 'C37 H43 Cu N6 P' _chemical_formula_weight 666.28 #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall -C2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.6030(18) _cell_length_b 17.7546(12) _cell_length_c 18.4891(13) _cell_angle_alpha 90.00 _cell_angle_beta 125.4830(10) _cell_angle_gamma 90.00 _cell_volume 7111.1(8) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rod-like crystal' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2808 _exptl_absorpt_coefficient_mu 0.693 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7738 _exptl_absorpt_correction_T_max 0.8458 _exptl_absorpt_process_details 'Blessing, 1995' #============================================================================== # EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex with CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31717 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0210 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 26.37 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _reflns_number_total 7263 _reflns_number_gt 6429 _reflns_threshold_expression >2sigma(I) #============================================================================== # REFINEMENT DATA _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^)+(0.0629P)^2^+4.5602P] 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 undef _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7263 _refine_ls_number_parameters 407 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.1016 _refine_ls_wR_factor_gt 0.0975 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.379 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.055 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 0.0000 0.0000 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Ortep32 for Windows' _computing_publication_material 'Bruker SHELXTL' #============================================================================== # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 0.806838(9) 0.908965(11) 0.844563(13) 0.03145(8) Uani 1 1 d . . . P1 P 0.733611(19) 0.93096(2) 0.85874(3) 0.02894(11) Uani 1 1 d . . . N1 N 0.85612(7) 0.87224(8) 0.74539(9) 0.0318(3) Uani 1 1 d . . . C1 C 0.91428(8) 0.88674(9) 0.83051(11) 0.0324(3) Uani 1 1 d . . . N2 N 0.79972(6) 0.87493(8) 0.73253(9) 0.0326(3) Uani 1 1 d . . . N3 N 0.91433(6) 0.96307(8) 0.85803(9) 0.0314(3) Uani 1 1 d . . . N4 N 0.86966(6) 0.99081(8) 0.86661(9) 0.0309(3) Uani 1 1 d . . . N5 N 0.91951(6) 0.83470(8) 0.89498(9) 0.0321(3) Uani 1 1 d . . . N6 N 0.87973(7) 0.83468(8) 0.91982(9) 0.0342(3) Uani 1 1 d . . . C10 C 0.90232(11) 0.84251(13) 0.66418(15) 0.0536(5) Uani 1 1 d . . . H10A H 0.9280 0.8879 0.6871 0.064 Uiso 1 1 calc R . . H10B H 0.8871 0.8348 0.6021 0.064 Uiso 1 1 calc R . . H10C H 0.9270 0.7989 0.6996 0.064 Uiso 1 1 calc R . . C11 C 0.84913(9) 0.85155(10) 0.66976(12) 0.0371(4) Uani 1 1 d . . . C12 C 0.78720(10) 0.84093(10) 0.60655(12) 0.0425(4) Uani 1 1 d . . . H12 H 0.7679 0.8264 0.5465 0.051 Uiso 1 1 calc R . . C13 C 0.75823(9) 0.85577(10) 0.64830(11) 0.0384(4) Uani 1 1 d . . . C14 C 0.69099(10) 0.85267(14) 0.60975(14) 0.0573(6) Uani 1 1 d . . . H14A H 0.6853 0.8291 0.6525 0.086 Uiso 1 1 calc R . . H14B H 0.6694 0.8230 0.5549 0.086 Uiso 1 1 calc R . . H14C H 0.6741 0.9039 0.5966 0.086 Uiso 1 1 calc R . . C20 C 1.01070(9) 1.00367(12) 0.87600(14) 0.0477(5) Uani 1 1 d . . . H20A H 1.0376 0.9658 0.9207 0.072 Uiso 1 1 calc R . . H20B H 1.0337 1.0508 0.8889 0.072 Uiso 1 1 calc R . . H20C H 0.9966 0.9855 0.8170 0.072 Uiso 1 1 calc R . . C21 C 0.95659(8) 1.01722(10) 0.87812(11) 0.0352(4) Uani 1 1 d . . . C22 C 0.93877(9) 1.08114(10) 0.89940(12) 0.0384(4) Uani 1 1 d . . . H22 H 0.9592 1.1285 0.9163 0.046 Uiso 1 1 calc R . . C23 C 0.88469(8) 1.06265(10) 0.89133(11) 0.0349(4) Uani 1 1 d . . . C24 C 0.84545(10) 1.11192(11) 0.90510(14) 0.0476(5) Uani 1 1 d . . . H24A H 0.8063 1.1221 0.8478 0.071 Uiso 1 1 calc R . . H24B H 0.8670 1.1595 0.9322 0.071 Uiso 1 1 calc R . . H24C H 0.8374 1.0865 0.9444 0.071 Uiso 1 1 calc R . . C30 C 1.01033(10) 0.76587(13) 0.92205(16) 0.0544(5) Uani 1 1 d . . . H30A H 0.9930 0.7363 0.8677 0.082 Uiso 1 1 calc R . . H30B H 1.0448 0.7382 0.9727 0.082 Uiso 1 1 calc R . . H30C H 1.0252 0.8143 0.9159 0.082 Uiso 1 1 calc R . . C31 C 0.96195(8) 0.77921(10) 0.93698(11) 0.0373(4) Uani 1 1 d . . . C32 C 0.94968(9) 0.74295(10) 0.99040(12) 0.0428(4) Uani 1 1 d . . . H32 H 0.9717 0.7014 1.0284 0.051 Uiso 1 1 calc R . . C33 C 0.89865(9) 0.77880(10) 0.97823(11) 0.0386(4) Uani 1 1 d . . . C34 C 0.86661(12) 0.76195(13) 1.02093(16) 0.0583(6) Uani 1 1 d . . . H34A H 0.8658 0.8074 1.0503 0.070 Uiso 1 1 calc R . . H34B H 0.8887 0.7218 1.0650 0.070 Uiso 1 1 calc R . . H34C H 0.8243 0.7456 0.9756 0.070 Uiso 1 1 calc R . . C100 C 0.66790(8) 0.86643(9) 0.80434(10) 0.0317(3) Uani 1 1 d . . . C101 C 0.67991(10) 0.79022(11) 0.80292(14) 0.0465(5) Uani 1 1 d . . . H101 H 0.7210 0.7738 0.8283 0.056 Uiso 1 1 calc R . . C102 C 0.63221(11) 0.73829(12) 0.76459(15) 0.0581(6) Uani 1 1 d . . . H102 H 0.6409 0.6864 0.7648 0.070 Uiso 1 1 calc R . . C103 C 0.57281(11) 0.76112(13) 0.72651(14) 0.0558(6) Uani 1 1 d . . . H103 H 0.5403 0.7252 0.7003 0.067 Uiso 1 1 calc R . . C104 C 0.56014(10) 0.83633(14) 0.72620(15) 0.0538(5) Uani 1 1 d . . . H104 H 0.5188 0.8524 0.6990 0.065 Uiso 1 1 calc R . . C105 C 0.60759(9) 0.88878(11) 0.76545(13) 0.0424(4) Uani 1 1 d . . . H105 H 0.5985 0.9405 0.7656 0.051 Uiso 1 1 calc R . . C200 C 0.69765(8) 1.02354(9) 0.81731(11) 0.0321(3) Uani 1 1 d . . . C201 C 0.68204(10) 1.04571(11) 0.73493(13) 0.0478(5) Uani 1 1 d . . . H201 H 0.6876 1.0118 0.7004 0.057 Uiso 1 1 calc R . . C202 C 0.65836(12) 1.11683(13) 0.70226(15) 0.0574(6) Uani 1 1 d . . . H202 H 0.6472 1.1310 0.6451 0.069 Uiso 1 1 calc R . . C203 C 0.65087(11) 1.16716(12) 0.75178(15) 0.0556(5) Uani 1 1 d . . . H203 H 0.6354 1.2163 0.7298 0.067 Uiso 1 1 calc R . . C204 C 0.66596(12) 1.14555(12) 0.83315(16) 0.0601(6) Uani 1 1 d . . . H204 H 0.6608 1.1799 0.8678 0.072 Uiso 1 1 calc R . . C205 C 0.68880(11) 1.07380(11) 0.86558(14) 0.0488(5) Uani 1 1 d . . . H205 H 0.6984 1.0593 0.9218 0.059 Uiso 1 1 calc R . . C300 C 0.75711(8) 0.93330(9) 0.97285(11) 0.0330(4) Uani 1 1 d . . . C301 C 0.81762(9) 0.95290(11) 1.03898(12) 0.0443(4) Uani 1 1 d . . . H301 H 0.8461 0.9608 1.0245 0.053 Uiso 1 1 calc R . . C302 C 0.83677(11) 0.96096(12) 1.12588(13) 0.0569(6) Uani 1 1 d . . . H302 H 0.8783 0.9748 1.1706 0.068 Uiso 1 1 calc R . . C303 C 0.79669(13) 0.94923(12) 1.14785(13) 0.0611(7) Uani 1 1 d . . . H303 H 0.8100 0.9552 1.2076 0.073 Uiso 1 1 calc R . . C304 C 0.73642(14) 0.92864(14) 1.08286(16) 0.0634(6) Uani 1 1 d . . . H304 H 0.7084 0.9203 1.0981 0.076 Uiso 1 1 calc R . . C305 C 0.71677(11) 0.92011(12) 0.99584(14) 0.0471(5) Uani 1 1 d . . . H305 H 0.6755 0.9052 0.9517 0.056 Uiso 1 1 calc R . . C90 C 0.5399(12) 1.0471(13) 0.8746(13) 0.221(12) Uiso 0.504(13) 1 d PD A 1 H90A H 0.5725 1.0362 0.8665 0.331 Uiso 0.504(13) 1 calc PR A 1 H90B H 0.5411 1.1006 0.8883 0.331 Uiso 0.504(13) 1 calc PR A 1 H90C H 0.4996 1.0348 0.8199 0.331 Uiso 0.504(13) 1 calc PR A 1 C90' C 0.5497(7) 1.0332(8) 0.8863(9) 0.110(4) Uiso 0.496(13) 1 d P A 2 H90D H 0.5519 1.0792 0.8589 0.165 Uiso 0.496(13) 1 calc PR A 2 H90E H 0.5257 0.9950 0.8403 0.165 Uiso 0.496(13) 1 calc PR A 2 H90F H 0.5915 1.0143 0.9301 0.165 Uiso 0.496(13) 1 calc PR A 2 C92 C 0.4992(7) 1.0168(9) 0.9665(9) 0.142(5) Uiso 0.504(13) 1 d P . 1 H92A H 0.5000 1.0720 0.9747 0.171 Uiso 0.504(13) 1 calc PR A 1 H92B H 0.4592 1.0044 0.9101 0.171 Uiso 0.504(13) 1 calc PR A 1 C92' C 0.5142(6) 0.9879(7) 0.9738(8) 0.119(4) Uiso 0.496(13) 1 d P . 2 H92C H 0.5554 0.9653 1.0162 0.142 Uiso 0.496(13) 1 calc PR A 2 H92D H 0.4875 0.9490 0.9293 0.142 Uiso 0.496(13) 1 calc PR A 2 C91 C 0.5510(5) 0.9963(7) 0.9563(7) 0.136(5) Uiso 0.504(13) 1 d PD A 1 H91A H 0.5493 0.9420 0.9429 0.164 Uiso 0.504(13) 1 calc PR A 1 H91B H 0.5918 1.0076 1.0119 0.164 Uiso 0.504(13) 1 calc PR A 1 C91' C 0.5201(5) 1.0497(7) 0.9298(8) 0.134(4) Uiso 0.496(13) 1 d P A 2 H91C H 0.5438 1.0901 0.9739 0.161 Uiso 0.496(13) 1 calc PR A 2 H91D H 0.4783 1.0698 0.8848 0.161 Uiso 0.496(13) 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 Cu1 0.03343(13) 0.02951(13) 0.03137(13) 0.00083(7) 0.01877(10) 0.00015(8) P1 0.0321(2) 0.0266(2) 0.0259(2) 0.00020(15) 0.01553(18) -0.00020(16) N1 0.0371(7) 0.0284(7) 0.0294(7) 0.0007(5) 0.0191(6) -0.0007(6) C1 0.0342(8) 0.0296(8) 0.0297(8) -0.0003(7) 0.0164(7) -0.0023(7) N2 0.0332(7) 0.0312(7) 0.0280(7) -0.0012(6) 0.0148(6) -0.0008(6) N3 0.0330(7) 0.0284(7) 0.0292(7) 0.0018(5) 0.0160(6) -0.0023(6) N4 0.0349(7) 0.0267(7) 0.0276(7) -0.0012(5) 0.0161(6) -0.0018(5) N5 0.0315(7) 0.0283(7) 0.0304(7) 0.0010(5) 0.0144(6) 0.0002(5) N6 0.0398(8) 0.0299(7) 0.0311(7) 0.0047(6) 0.0196(6) 0.0015(6) C10 0.0688(14) 0.0573(13) 0.0516(12) -0.0045(10) 0.0446(12) -0.0025(11) C11 0.0529(11) 0.0293(8) 0.0334(9) -0.0005(7) 0.0274(8) -0.0020(7) C12 0.0584(12) 0.0349(9) 0.0277(8) -0.0019(7) 0.0213(8) -0.0006(8) C13 0.0422(10) 0.0318(9) 0.0292(8) -0.0008(7) 0.0139(8) -0.0006(7) C14 0.0412(11) 0.0670(14) 0.0405(11) -0.0124(10) 0.0106(9) -0.0045(10) C20 0.0387(10) 0.0508(12) 0.0499(11) 0.0023(9) 0.0236(9) -0.0087(9) C21 0.0353(9) 0.0350(9) 0.0261(8) 0.0035(7) 0.0126(7) -0.0071(7) C22 0.0433(10) 0.0304(9) 0.0307(9) -0.0017(7) 0.0154(8) -0.0097(7) C23 0.0420(9) 0.0283(8) 0.0263(8) -0.0002(6) 0.0152(7) -0.0034(7) C24 0.0546(12) 0.0328(9) 0.0516(11) -0.0103(8) 0.0287(10) -0.0038(8) C30 0.0412(11) 0.0491(12) 0.0644(14) 0.0005(10) 0.0257(10) 0.0092(9) C31 0.0330(9) 0.0287(8) 0.0321(8) -0.0024(7) 0.0086(7) 0.0008(7) C32 0.0464(10) 0.0290(9) 0.0325(9) 0.0034(7) 0.0112(8) 0.0034(8) C33 0.0490(10) 0.0284(8) 0.0291(8) 0.0038(7) 0.0174(8) -0.0008(7) C34 0.0819(16) 0.0467(12) 0.0554(13) 0.0181(10) 0.0450(13) 0.0058(11) C100 0.0366(9) 0.0315(8) 0.0247(7) -0.0023(6) 0.0164(7) -0.0041(7) C101 0.0459(11) 0.0330(10) 0.0470(11) -0.0015(8) 0.0191(9) -0.0010(8) C102 0.0652(14) 0.0333(10) 0.0533(12) -0.0034(9) 0.0217(11) -0.0101(10) C103 0.0551(13) 0.0536(13) 0.0439(11) -0.0080(9) 0.0202(10) -0.0235(10) C104 0.0364(10) 0.0654(14) 0.0483(11) -0.0088(10) 0.0182(9) -0.0103(9) C105 0.0391(10) 0.0411(10) 0.0403(10) -0.0071(8) 0.0193(8) -0.0032(8) C200 0.0336(8) 0.0271(8) 0.0315(8) 0.0016(6) 0.0165(7) 0.0001(6) C201 0.0655(13) 0.0411(10) 0.0394(10) 0.0084(8) 0.0319(10) 0.0130(9) C202 0.0752(15) 0.0489(12) 0.0447(11) 0.0185(10) 0.0329(11) 0.0159(11) C203 0.0661(14) 0.0324(10) 0.0518(12) 0.0091(9) 0.0249(11) 0.0119(9) C204 0.0866(17) 0.0360(11) 0.0539(13) 0.0010(9) 0.0387(13) 0.0158(11) C205 0.0702(14) 0.0357(10) 0.0411(10) 0.0029(8) 0.0327(11) 0.0092(9) C300 0.0423(9) 0.0249(8) 0.0265(8) -0.0001(6) 0.0170(7) 0.0003(7) C301 0.0442(10) 0.0392(10) 0.0338(9) -0.0014(7) 0.0137(8) -0.0018(8) C302 0.0651(14) 0.0413(11) 0.0303(10) -0.0034(8) 0.0083(10) 0.0000(10) C303 0.1008(19) 0.0407(11) 0.0290(10) -0.0016(8) 0.0304(12) 0.0028(11) C304 0.0966(19) 0.0615(14) 0.0483(13) -0.0029(11) 0.0514(14) -0.0068(13) C305 0.0577(12) 0.0512(12) 0.0370(10) -0.0042(8) 0.0301(10) -0.0092(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 Cu1 N2 2.0582(14) . ? Cu1 N4 2.0688(14) . ? Cu1 N6 2.0745(14) . ? Cu1 P1 2.1469(5) . ? P1 C300 1.8200(17) . ? P1 C100 1.8273(17) . ? P1 C200 1.8311(17) . ? N1 C11 1.350(2) . ? N1 N2 1.377(2) . ? N1 C1 1.453(2) . ? C1 N3 1.447(2) . ? C1 N5 1.450(2) . ? N2 C13 1.328(2) . ? N3 C21 1.357(2) . ? N3 N4 1.378(2) . ? N4 C23 1.335(2) . ? N5 C31 1.353(2) . ? N5 N6 1.377(2) . ? N6 C33 1.331(2) . ? C10 C11 1.486(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.371(3) . ? C12 C13 1.396(3) . ? C12 H12 0.9500 . ? C13 C14 1.493(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C20 C21 1.482(3) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.373(3) . ? C22 C23 1.397(3) . ? C22 H22 0.9500 . ? C23 C24 1.493(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C30 C31 1.484(3) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.368(3) . ? C32 C33 1.394(3) . ? C32 H32 0.9500 . ? C33 C34 1.490(3) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C100 C105 1.382(3) . ? C100 C101 1.394(3) . ? C101 C102 1.385(3) . ? C101 H101 0.9500 . ? C102 C103 1.366(3) . ? C102 H102 0.9500 . ? C103 C104 1.376(3) . ? C103 H103 0.9500 . ? C104 C105 1.387(3) . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? C200 C205 1.376(3) . ? C200 C201 1.383(3) . ? C201 C202 1.384(3) . ? C201 H201 0.9500 . ? C202 C203 1.374(3) . ? C202 H202 0.9500 . ? C203 C204 1.368(3) . ? C203 H203 0.9500 . ? C204 C205 1.389(3) . ? C204 H204 0.9500 . ? C205 H205 0.9500 . ? C300 C305 1.384(3) . ? C300 C301 1.387(3) . ? C301 C302 1.383(3) . ? C301 H301 0.9500 . ? C302 C303 1.359(4) . ? C302 H302 0.9500 . ? C303 C304 1.383(4) . ? C303 H303 0.9500 . ? C304 C305 1.381(3) . ? C304 H304 0.9500 . ? C305 H305 0.9500 . ? C90 C91 1.633(10) . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? C90' C91' 1.445(16) . ? C90' H90D 0.9800 . ? C90' H90E 0.9800 . ? C90' H90F 0.9800 . ? C92 C92 1.35(3) 5_677 ? C92 C91 1.54(2) . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C92' C91' 1.43(2) . ? C92' C92' 1.60(2) 5_677 ? C92' H92C 0.9900 . ? C92' H92D 0.9900 . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C91' H91C 0.9900 . ? C91' H91D 0.9900 . ? 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 Cu1 N4 89.79(6) . . ? N2 Cu1 N6 89.57(6) . . ? N4 Cu1 N6 88.89(6) . . ? N2 Cu1 P1 128.05(4) . . ? N4 Cu1 P1 122.32(4) . . ? N6 Cu1 P1 126.51(4) . . ? C300 P1 C100 103.15(8) . . ? C300 P1 C200 102.07(8) . . ? C100 P1 C200 103.41(8) . . ? C300 P1 Cu1 114.85(6) . . ? C100 P1 Cu1 117.69(6) . . ? C200 P1 Cu1 113.77(6) . . ? C11 N1 N2 110.46(14) . . ? C11 N1 C1 126.16(15) . . ? N2 N1 C1 123.33(13) . . ? N3 C1 N5 109.13(13) . . ? N3 C1 N1 109.26(13) . . ? N5 C1 N1 108.15(13) . . ? C13 N2 N1 105.91(14) . . ? C13 N2 Cu1 141.60(13) . . ? N1 N2 Cu1 112.45(10) . . ? C21 N3 N4 110.37(14) . . ? C21 N3 C1 126.24(15) . . ? N4 N3 C1 123.38(13) . . ? C23 N4 N3 105.90(14) . . ? C23 N4 Cu1 141.75(12) . . ? N3 N4 Cu1 112.23(10) . . ? C31 N5 N6 110.81(14) . . ? C31 N5 C1 125.87(15) . . ? N6 N5 C1 123.30(13) . . ? C33 N6 N5 105.61(14) . . ? C33 N6 Cu1 141.60(13) . . ? N5 N6 Cu1 112.11(10) . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 107.16(16) . . ? N1 C11 C10 122.48(17) . . ? C12 C11 C10 130.35(17) . . ? C11 C12 C13 106.18(16) . . ? C11 C12 H12 126.9 . . ? C13 C12 H12 126.9 . . ? N2 C13 C12 110.29(17) . . ? N2 C13 C14 121.27(18) . . ? C12 C13 C14 128.44(17) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C21 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C21 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 C22 107.16(16) . . ? N3 C21 C20 122.74(17) . . ? C22 C21 C20 130.10(17) . . ? C21 C22 C23 106.31(15) . . ? C21 C22 H22 126.8 . . ? C23 C22 H22 126.8 . . ? N4 C23 C22 110.25(16) . . ? N4 C23 C24 121.21(17) . . ? C22 C23 C24 128.53(17) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N5 C31 C32 106.74(17) . . ? N5 C31 C30 122.30(17) . . ? C32 C31 C30 130.96(17) . . ? C31 C32 C33 106.65(16) . . ? C31 C32 H32 126.7 . . ? C33 C32 H32 126.7 . . ? N6 C33 C32 110.19(17) . . ? N6 C33 C34 121.09(18) . . ? C32 C33 C34 128.72(17) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C105 C100 C101 118.59(17) . . ? C105 C100 P1 123.87(14) . . ? C101 C100 P1 117.54(14) . . ? C102 C101 C100 120.2(2) . . ? C102 C101 H101 119.9 . . ? C100 C101 H101 119.9 . . ? C103 C102 C101 120.6(2) . . ? C103 C102 H102 119.7 . . ? C101 C102 H102 119.7 . . ? C102 C103 C104 119.82(19) . . ? C102 C103 H103 120.1 . . ? C104 C103 H103 120.1 . . ? C103 C104 C105 120.2(2) . . ? C103 C104 H104 119.9 . . ? C105 C104 H104 119.9 . . ? C100 C105 C104 120.58(19) . . ? C100 C105 H105 119.7 . . ? C104 C105 H105 119.7 . . ? C205 C200 C201 118.35(17) . . ? C205 C200 P1 123.75(14) . . ? C201 C200 P1 117.79(14) . . ? C200 C201 C202 120.67(19) . . ? C200 C201 H201 119.7 . . ? C202 C201 H201 119.7 . . ? C203 C202 C201 120.53(19) . . ? C203 C202 H202 119.7 . . ? C201 C202 H202 119.7 . . ? C204 C203 C202 119.14(19) . . ? C204 C203 H203 120.4 . . ? C202 C203 H203 120.4 . . ? C203 C204 C205 120.5(2) . . ? C203 C204 H204 119.7 . . ? C205 C204 H204 119.7 . . ? C200 C205 C204 120.78(19) . . ? C200 C205 H205 119.6 . . ? C204 C205 H205 119.6 . . ? C305 C300 C301 118.81(17) . . ? C305 C300 P1 123.10(14) . . ? C301 C300 P1 118.01(15) . . ? C302 C301 C300 120.4(2) . . ? C302 C301 H301 119.8 . . ? C300 C301 H301 119.8 . . ? C303 C302 C301 120.5(2) . . ? C303 C302 H302 119.7 . . ? C301 C302 H302 119.7 . . ? C302 C303 C304 119.72(19) . . ? C302 C303 H303 120.1 . . ? C304 C303 H303 120.1 . . ? C305 C304 C303 120.3(2) . . ? C305 C304 H304 119.8 . . ? C303 C304 H304 119.8 . . ? C304 C305 C300 120.1(2) . . ? C304 C305 H305 119.9 . . ? C300 C305 H305 119.9 . . ? C91 C90 H90A 109.5 . . ? C91 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C91 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C91' C90' H90D 109.5 . . ? C91' C90' H90E 109.5 . . ? H90D C90' H90E 109.5 . . ? C91' C90' H90F 109.5 . . ? H90D C90' H90F 109.5 . . ? H90E C90' H90F 109.5 . . ? C92 C92 C91 116.9(18) 5_677 . ? C92 C92 H92A 108.1 5_677 . ? C91 C92 H92A 108.1 . . ? C92 C92 H92B 108.1 5_677 . ? C91 C92 H92B 108.1 . . ? H92A C92 H92B 107.3 . . ? C91' C92' C92' 112.8(14) . 5_677 ? C91' C92' H92C 109.0 . . ? C92' C92' H92C 109.0 5_677 . ? C91' C92' H92D 109.0 . . ? C92' C92' H92D 109.0 5_677 . ? H92C C92' H92D 107.8 . . ? C92 C91 C90 106.9(13) . . ? C92 C91 H91A 110.3 . . ? C90 C91 H91A 110.3 . . ? C92 C91 H91B 110.3 . . ? C90 C91 H91B 110.3 . . ? H91A C91 H91B 108.6 . . ? C92' C91' C90' 115.9(12) . . ? C92' C91' H91C 108.3 . . ? C90' C91' H91C 108.3 . . ? C92' C91' H91D 108.3 . . ? C90' C91' H91D 108.3 . . ? H91C C91' H91D 107.4 . . ? 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 N2 Cu1 P1 C300 163.00(8) . . . . ? N4 Cu1 P1 C300 -77.68(8) . . . . ? N6 Cu1 P1 C300 38.42(8) . . . . ? N2 Cu1 P1 C100 41.25(8) . . . . ? N4 Cu1 P1 C100 160.58(7) . . . . ? N6 Cu1 P1 C100 -83.33(8) . . . . ? N2 Cu1 P1 C200 -79.90(8) . . . . ? N4 Cu1 P1 C200 39.43(8) . . . . ? N6 Cu1 P1 C200 155.53(8) . . . . ? C11 N1 C1 N3 121.27(17) . . . . ? N2 N1 C1 N3 -61.66(19) . . . . ? C11 N1 C1 N5 -120.05(17) . . . . ? N2 N1 C1 N5 57.02(19) . . . . ? C11 N1 N2 C13 -0.08(18) . . . . ? C1 N1 N2 C13 -177.55(15) . . . . ? C11 N1 N2 Cu1 -178.45(11) . . . . ? C1 N1 N2 Cu1 4.08(18) . . . . ? N4 Cu1 N2 C13 -135.1(2) . . . . ? N6 Cu1 N2 C13 136.0(2) . . . . ? P1 Cu1 N2 C13 -2.6(2) . . . . ? N4 Cu1 N2 N1 42.35(11) . . . . ? N6 Cu1 N2 N1 -46.54(11) . . . . ? P1 Cu1 N2 N1 174.89(8) . . . . ? N5 C1 N3 C21 118.53(17) . . . . ? N1 C1 N3 C21 -123.40(16) . . . . ? N5 C1 N3 N4 -62.07(19) . . . . ? N1 C1 N3 N4 55.99(19) . . . . ? C21 N3 N4 C23 0.56(17) . . . . ? C1 N3 N4 C23 -178.92(14) . . . . ? C21 N3 N4 Cu1 -176.39(10) . . . . ? C1 N3 N4 Cu1 4.13(18) . . . . ? N2 Cu1 N4 C23 138.29(19) . . . . ? N6 Cu1 N4 C23 -132.14(19) . . . . ? P1 Cu1 N4 C23 1.6(2) . . . . ? N2 Cu1 N4 N3 -46.46(10) . . . . ? N6 Cu1 N4 N3 43.11(10) . . . . ? P1 Cu1 N4 N3 176.90(8) . . . . ? N3 C1 N5 C31 -126.72(17) . . . . ? N1 C1 N5 C31 114.51(17) . . . . ? N3 C1 N5 N6 55.00(19) . . . . ? N1 C1 N5 N6 -63.76(19) . . . . ? C31 N5 N6 C33 0.51(18) . . . . ? C1 N5 N6 C33 179.01(15) . . . . ? C31 N5 N6 Cu1 -172.16(11) . . . . ? C1 N5 N6 Cu1 6.34(18) . . . . ? N2 Cu1 N6 C33 -127.0(2) . . . . ? N4 Cu1 N6 C33 143.2(2) . . . . ? P1 Cu1 N6 C33 12.5(2) . . . . ? N2 Cu1 N6 N5 41.55(11) . . . . ? N4 Cu1 N6 N5 -48.26(11) . . . . ? P1 Cu1 N6 N5 -178.88(8) . . . . ? N2 N1 C11 C12 0.28(19) . . . . ? C1 N1 C11 C12 177.66(15) . . . . ? N2 N1 C11 C10 -178.85(16) . . . . ? C1 N1 C11 C10 -1.5(3) . . . . ? N1 C11 C12 C13 -0.4(2) . . . . ? C10 C11 C12 C13 178.68(19) . . . . ? N1 N2 C13 C12 -0.15(19) . . . . ? Cu1 N2 C13 C12 177.42(14) . . . . ? N1 N2 C13 C14 -179.80(17) . . . . ? Cu1 N2 C13 C14 -2.2(3) . . . . ? C11 C12 C13 N2 0.3(2) . . . . ? C11 C12 C13 C14 179.9(2) . . . . ? N4 N3 C21 C22 -0.43(18) . . . . ? C1 N3 C21 C22 179.03(15) . . . . ? N4 N3 C21 C20 179.17(15) . . . . ? C1 N3 C21 C20 -1.4(3) . . . . ? N3 C21 C22 C23 0.13(19) . . . . ? C20 C21 C22 C23 -179.43(18) . . . . ? N3 N4 C23 C22 -0.47(18) . . . . ? Cu1 N4 C23 C22 174.96(14) . . . . ? N3 N4 C23 C24 178.54(16) . . . . ? Cu1 N4 C23 C24 -6.0(3) . . . . ? C21 C22 C23 N4 0.2(2) . . . . ? C21 C22 C23 C24 -178.70(18) . . . . ? N6 N5 C31 C32 -0.40(19) . . . . ? C1 N5 C31 C32 -178.86(15) . . . . ? N6 N5 C31 C30 179.50(16) . . . . ? C1 N5 C31 C30 1.0(3) . . . . ? N5 C31 C32 C33 0.1(2) . . . . ? C30 C31 C32 C33 -179.75(19) . . . . ? N5 N6 C33 C32 -0.41(19) . . . . ? Cu1 N6 C33 C32 168.62(15) . . . . ? N5 N6 C33 C34 179.39(17) . . . . ? Cu1 N6 C33 C34 -11.6(3) . . . . ? C31 C32 C33 N6 0.2(2) . . . . ? C31 C32 C33 C34 -179.6(2) . . . . ? C300 P1 C100 C105 88.84(16) . . . . ? C200 P1 C100 C105 -17.20(17) . . . . ? Cu1 P1 C100 C105 -143.57(14) . . . . ? C300 P1 C100 C101 -90.69(15) . . . . ? C200 P1 C100 C101 163.27(15) . . . . ? Cu1 P1 C100 C101 36.90(16) . . . . ? C105 C100 C101 C102 -1.1(3) . . . . ? P1 C100 C101 C102 178.41(17) . . . . ? C100 C101 C102 C103 1.1(3) . . . . ? C101 C102 C103 C104 0.0(4) . . . . ? C102 C103 C104 C105 -0.9(4) . . . . ? C101 C100 C105 C104 0.2(3) . . . . ? P1 C100 C105 C104 -179.28(16) . . . . ? C103 C104 C105 C100 0.8(3) . . . . ? C300 P1 C200 C205 -5.04(19) . . . . ? C100 P1 C200 C205 101.83(18) . . . . ? Cu1 P1 C200 C205 -129.35(16) . . . . ? C300 P1 C200 C201 170.86(16) . . . . ? C100 P1 C200 C201 -82.28(16) . . . . ? Cu1 P1 C200 C201 46.55(17) . . . . ? C205 C200 C201 C202 0.3(3) . . . . ? P1 C200 C201 C202 -175.86(18) . . . . ? C200 C201 C202 C203 1.1(4) . . . . ? C201 C202 C203 C204 -1.3(4) . . . . ? C202 C203 C204 C205 0.3(4) . . . . ? C201 C200 C205 C204 -1.3(3) . . . . ? P1 C200 C205 C204 174.57(19) . . . . ? C203 C204 C205 C200 1.1(4) . . . . ? C100 P1 C300 C305 -27.18(17) . . . . ? C200 P1 C300 C305 79.89(17) . . . . ? Cu1 P1 C300 C305 -156.53(14) . . . . ? C100 P1 C300 C301 156.10(14) . . . . ? C200 P1 C300 C301 -96.83(15) . . . . ? Cu1 P1 C300 C301 26.75(16) . . . . ? C305 C300 C301 C302 -1.6(3) . . . . ? P1 C300 C301 C302 175.24(15) . . . . ? C300 C301 C302 C303 0.5(3) . . . . ? C301 C302 C303 C304 0.4(3) . . . . ? C302 C303 C304 C305 -0.1(4) . . . . ? C303 C304 C305 C300 -1.0(4) . . . . ? C301 C300 C305 C304 1.9(3) . . . . ? P1 C300 C305 C304 -174.82(18) . . . . ? C92 C92 C91 C90 -177.4(18) 5_677 . . . ? C92' C92' C91' C90' 175.7(12) 5_677 . . . ? #============================================================================== # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. data_C(Mepz)3CuP(OMe)3 _database_code_depnum_ccdc_archive 'CCDC 282768' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H30 Cu N6 O3 P' _chemical_formula_sum 'C19 H30 Cu N6 O3 P' _chemical_formula_weight 485.00 #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.392(2) _cell_length_b 11.069(3) _cell_length_c 11.705(3) _cell_angle_alpha 96.346(5) _cell_angle_beta 104.986(5) _cell_angle_gamma 112.169(5) _cell_volume 1171.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rhombus _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.72 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 508 _exptl_absorpt_coefficient_mu 1.032 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5238 _exptl_absorpt_correction_T_max 0.8281 _exptl_absorpt_process_details 'Blessing, 1995' #============================================================================== # EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 250(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex with CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9733 _diffrn_reflns_av_R_equivalents 0.0196 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 30.91 _diffrn_measured_fraction_theta_max 0.886 _diffrn_reflns_theta_full 30.91 _diffrn_measured_fraction_theta_full 0.886 _reflns_number_total 6546 _reflns_number_gt 4829 _reflns_threshold_expression >2sigma(I) #============================================================================== # REFINEMENT DATA _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^)+(0.0977P)^2^+0.0000P] 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 undef _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6546 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1694 _refine_ls_wR_factor_gt 0.1547 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.805 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.093 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 0.0000 0.0000 '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 0.0060 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Ortep32 for Windows' _computing_publication_material 'Bruker SHELXTL' #============================================================================== # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 0.75179(4) 0.06645(4) 0.28187(3) 0.04142(14) Uani 1 1 d . . . P1 P 0.93718(9) 0.24595(9) 0.30060(9) 0.0539(2) Uani 1 1 d . . . N2 N 0.7501(2) -0.1179(2) 0.2130(2) 0.0383(5) Uani 1 1 d . . . N4 N 0.5314(2) -0.0080(2) 0.18959(19) 0.0374(5) Uani 1 1 d . . . N3 N 0.4559(3) -0.1392(3) 0.1916(2) 0.0414(5) Uani 1 1 d . . . N1 N 0.6343(2) -0.2258(2) 0.2226(2) 0.0397(5) Uani 1 1 d . . . N6 N 0.6919(3) -0.0058(3) 0.4241(2) 0.0479(6) Uani 1 1 d . . . N5 N 0.5873(3) -0.1351(3) 0.3905(2) 0.0492(6) Uani 1 1 d . . . C23 C 0.4360(3) 0.0250(3) 0.1154(2) 0.0391(6) Uani 1 1 d . . . C22 C 0.2999(3) -0.0855(3) 0.0669(2) 0.0449(7) Uani 1 1 d . . . H22 H 0.2143 -0.0890 0.0116 0.054 Uiso 1 1 calc R . . C21 C 0.3153(3) -0.1883(3) 0.1159(2) 0.0436(6) Uani 1 1 d . . . C13 C 0.8255(3) -0.1686(3) 0.1653(2) 0.0415(6) Uani 1 1 d . . . C12 C 0.7604(4) -0.3078(3) 0.1437(3) 0.0520(7) Uani 1 1 d . . . H12 H 0.7933 -0.3674 0.1106 0.062 Uiso 1 1 calc R . . C1 C 0.5199(3) -0.2128(3) 0.2651(3) 0.0446(6) Uani 1 1 d . . . C11 C 0.6387(4) -0.3409(3) 0.1801(3) 0.0489(7) Uani 1 1 d . . . O1 O 1.0672(3) 0.2997(3) 0.4266(3) 0.0809(9) Uani 1 1 d . . . C33 C 0.7184(4) 0.0357(4) 0.5431(3) 0.0621(10) Uani 1 1 d . . . C24 C 0.4789(4) 0.1625(3) 0.0961(3) 0.0488(7) Uani 1 1 d . . . H24A H 0.4695 0.2185 0.1604 0.073 Uiso 1 1 calc R . . H24B H 0.4153 0.1603 0.0181 0.073 Uiso 1 1 calc R . . H24C H 0.5800 0.1990 0.0970 0.073 Uiso 1 1 calc R . . O2 O 1.0152(3) 0.2362(3) 0.2016(3) 0.0753(8) Uani 1 1 d . . . C31 C 0.5512(4) -0.1737(5) 0.4877(3) 0.0669(11) Uani 1 1 d . . . C32 C 0.6334(5) -0.0659(5) 0.5856(3) 0.0735(13) Uani 1 1 d . . . H32 H 0.6318 -0.0622 0.6658 0.088 Uiso 1 1 calc R . . C20 C 0.2081(4) -0.3298(4) 0.0938(3) 0.0617(9) Uani 1 1 d . . . H20A H 0.2287 -0.3871 0.0392 0.093 Uiso 1 1 calc R . . H20B H 0.1093 -0.3376 0.0575 0.093 Uiso 1 1 calc R . . H20C H 0.2162 -0.3570 0.1704 0.093 Uiso 1 1 calc R . . C14 C 0.9580(4) -0.0820(4) 0.1374(4) 0.0605(9) Uani 1 1 d . . . H14A H 0.9283 -0.0437 0.0702 0.091 Uiso 1 1 calc R . . H14B H 1.0071 -0.1356 0.1154 0.091 Uiso 1 1 calc R . . H14C H 1.0247 -0.0105 0.2084 0.091 Uiso 1 1 calc R . . C10 C 0.5278(5) -0.4748(4) 0.1788(5) 0.0760(11) Uani 1 1 d . . . H10A H 0.5470 -0.4899 0.2603 0.114 Uiso 1 1 calc R . . H10B H 0.5340 -0.5441 0.1249 0.114 Uiso 1 1 calc R . . H10C H 0.4301 -0.4777 0.1502 0.114 Uiso 1 1 calc R . . O3 O 0.9260(4) 0.3837(3) 0.2865(5) 0.1185(15) Uani 1 1 d . . . C30 C 0.4449(5) -0.3126(6) 0.4790(5) 0.0946(17) Uani 1 1 d . . . H30A H 0.3602 -0.3406 0.4064 0.142 Uiso 1 1 calc R . . H30B H 0.4133 -0.3145 0.5501 0.142 Uiso 1 1 calc R . . H30C H 0.4918 -0.3731 0.4748 0.142 Uiso 1 1 calc R . . C100 C 1.1093(5) 0.2010(6) 0.4792(4) 0.0993(18) Uani 1 1 d . . . H10D H 1.0225 0.1176 0.4614 0.149 Uiso 1 1 calc R . . H10E H 1.1547 0.2345 0.5666 0.149 Uiso 1 1 calc R . . H10F H 1.1785 0.1855 0.4446 0.149 Uiso 1 1 calc R . . C200 C 1.1536(5) 0.3369(5) 0.2082(6) 0.112(2) Uani 1 1 d . . . H20D H 1.1395 0.3835 0.1438 0.168 Uiso 1 1 calc R . . H20E H 1.2186 0.2954 0.1987 0.168 Uiso 1 1 calc R . . H20F H 1.1968 0.4003 0.2864 0.168 Uiso 1 1 calc R . . C300 C 0.8483(7) 0.4325(6) 0.3349(6) 0.115(2) Uani 1 1 d . . . H30D H 0.7495 0.3633 0.3158 0.172 Uiso 1 1 calc R . . H30E H 0.8440 0.5079 0.3017 0.172 Uiso 1 1 calc R . . H30F H 0.8948 0.4620 0.4224 0.172 Uiso 1 1 calc R . . C34 C 0.8248(5) 0.1745(5) 0.6101(3) 0.0834(14) Uani 1 1 d . . . H34A H 0.9192 0.1750 0.6506 0.125 Uiso 1 1 calc R . . H34B H 0.7890 0.2068 0.6701 0.125 Uiso 1 1 calc R . . H34C H 0.8359 0.2323 0.5534 0.125 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 0.0416(2) 0.0467(2) 0.03445(19) 0.00782(14) 0.00616(14) 0.02164(16) P1 0.0458(4) 0.0401(4) 0.0628(5) 0.0038(4) 0.0012(4) 0.0177(4) N2 0.0389(12) 0.0442(13) 0.0378(11) 0.0138(10) 0.0127(9) 0.0225(10) N4 0.0381(11) 0.0482(13) 0.0308(10) 0.0123(9) 0.0100(9) 0.0235(10) N3 0.0384(12) 0.0565(15) 0.0382(11) 0.0183(11) 0.0149(10) 0.0259(11) N1 0.0383(12) 0.0449(13) 0.0399(11) 0.0144(10) 0.0104(9) 0.0222(10) N6 0.0571(15) 0.0705(18) 0.0291(10) 0.0140(11) 0.0118(10) 0.0416(15) N5 0.0488(14) 0.080(2) 0.0368(11) 0.0278(13) 0.0184(11) 0.0389(14) C23 0.0452(14) 0.0567(17) 0.0276(11) 0.0109(11) 0.0130(10) 0.0334(14) C22 0.0420(15) 0.066(2) 0.0334(12) 0.0112(13) 0.0094(11) 0.0315(14) C21 0.0373(14) 0.0599(18) 0.0369(13) 0.0103(12) 0.0131(11) 0.0237(13) C13 0.0452(15) 0.0518(17) 0.0370(13) 0.0150(12) 0.0129(11) 0.0297(13) C12 0.0608(19) 0.0525(19) 0.0566(17) 0.0121(14) 0.0218(15) 0.0368(16) C1 0.0419(15) 0.0607(19) 0.0431(14) 0.0229(13) 0.0183(12) 0.0283(14) C11 0.0541(18) 0.0466(17) 0.0524(16) 0.0177(14) 0.0141(14) 0.0285(14) O1 0.0593(15) 0.078(2) 0.0711(17) -0.0203(14) -0.0107(13) 0.0248(14) C33 0.076(2) 0.104(3) 0.0320(13) 0.0142(16) 0.0143(15) 0.068(2) C24 0.0637(19) 0.0586(19) 0.0372(13) 0.0139(13) 0.0139(13) 0.0404(16) O2 0.0581(15) 0.0608(16) 0.0812(18) 0.0098(14) 0.0222(14) 0.0004(12) C31 0.066(2) 0.124(4) 0.0520(18) 0.051(2) 0.0342(17) 0.066(2) C32 0.086(3) 0.139(4) 0.0407(16) 0.040(2) 0.0327(19) 0.082(3) C20 0.0505(19) 0.063(2) 0.061(2) 0.0121(17) 0.0101(16) 0.0194(17) C14 0.061(2) 0.072(2) 0.075(2) 0.0316(19) 0.0401(19) 0.0404(19) C10 0.070(3) 0.051(2) 0.101(3) 0.019(2) 0.022(2) 0.0226(19) O3 0.099(3) 0.058(2) 0.199(5) 0.032(2) 0.036(3) 0.0426(19) C30 0.083(3) 0.142(5) 0.091(3) 0.079(3) 0.050(3) 0.054(3) C100 0.082(3) 0.153(5) 0.067(3) 0.002(3) -0.010(2) 0.083(4) C200 0.073(3) 0.087(4) 0.144(5) 0.017(4) 0.046(4) -0.006(3) C300 0.125(5) 0.092(4) 0.129(5) -0.004(3) 0.008(4) 0.076(4) C34 0.116(4) 0.107(4) 0.0391(17) 0.000(2) 0.008(2) 0.076(3) #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N4 2.047(2) . ? Cu1 N6 2.062(2) . ? Cu1 N2 2.102(2) . ? Cu1 P1 2.1222(10) . ? P1 O1 1.588(3) . ? P1 O2 1.593(3) . ? P1 O3 1.595(3) . ? N2 C13 1.315(3) . ? N2 N1 1.379(3) . ? N4 C23 1.330(3) . ? N4 N3 1.372(3) . ? N3 C21 1.356(4) . ? N3 C1 1.454(3) . ? N1 C11 1.338(4) . ? N1 C1 1.448(3) . ? N6 C33 1.338(4) . ? N6 N5 1.365(4) . ? N5 C31 1.351(4) . ? N5 C1 1.456(4) . ? C23 C22 1.394(4) . ? C23 C24 1.478(4) . ? C22 C21 1.372(4) . ? C22 H22 0.9400 . ? C21 C20 1.485(5) . ? C13 C12 1.391(4) . ? C13 C14 1.493(4) . ? C12 C11 1.371(5) . ? C12 H12 0.9400 . ? C11 C10 1.490(5) . ? O1 C100 1.461(6) . ? C33 C32 1.376(6) . ? C33 C34 1.483(6) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? O2 C200 1.425(5) . ? C31 C32 1.375(6) . ? C31 C30 1.490(7) . ? C32 H32 0.9400 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? O3 C300 1.327(6) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C100 H10D 0.9700 . ? C100 H10E 0.9700 . ? C100 H10F 0.9700 . ? C200 H20D 0.9700 . ? C200 H20E 0.9700 . ? C200 H20F 0.9700 . ? C300 H30D 0.9700 . ? C300 H30E 0.9700 . ? C300 H30F 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? 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 Cu1 N6 86.33(9) . . ? N4 Cu1 N2 89.66(9) . . ? N6 Cu1 N2 90.01(10) . . ? N4 Cu1 P1 134.52(7) . . ? N6 Cu1 P1 125.08(9) . . ? N2 Cu1 P1 118.67(7) . . ? O1 P1 O2 104.05(17) . . ? O1 P1 O3 98.6(2) . . ? O2 P1 O3 97.9(2) . . ? O1 P1 Cu1 116.69(14) . . ? O2 P1 Cu1 113.59(11) . . ? O3 P1 Cu1 122.82(15) . . ? C13 N2 N1 106.0(2) . . ? C13 N2 Cu1 141.6(2) . . ? N1 N2 Cu1 112.32(15) . . ? C23 N4 N3 106.5(2) . . ? C23 N4 Cu1 140.1(2) . . ? N3 N4 Cu1 112.92(15) . . ? C21 N3 N4 110.2(2) . . ? C21 N3 C1 125.9(3) . . ? N4 N3 C1 124.0(2) . . ? C11 N1 N2 110.5(2) . . ? C11 N1 C1 126.0(3) . . ? N2 N1 C1 123.3(2) . . ? C33 N6 N5 106.1(3) . . ? C33 N6 Cu1 140.0(3) . . ? N5 N6 Cu1 113.77(17) . . ? C31 N5 N6 110.2(3) . . ? C31 N5 C1 126.6(3) . . ? N6 N5 C1 123.1(2) . . ? N4 C23 C22 109.8(3) . . ? N4 C23 C24 121.1(3) . . ? C22 C23 C24 129.0(2) . . ? C21 C22 C23 106.6(2) . . ? C21 C22 H22 126.7 . . ? C23 C22 H22 126.7 . . ? N3 C21 C22 106.9(3) . . ? N3 C21 C20 122.9(3) . . ? C22 C21 C20 130.1(3) . . ? N2 C13 C12 110.2(3) . . ? N2 C13 C14 121.8(3) . . ? C12 C13 C14 127.9(3) . . ? C11 C12 C13 106.3(3) . . ? C11 C12 H12 126.8 . . ? C13 C12 H12 126.8 . . ? N1 C1 N3 108.6(2) . . ? N1 C1 N5 108.2(2) . . ? N3 C1 N5 108.4(2) . . ? N1 C11 C12 106.9(3) . . ? N1 C11 C10 122.9(3) . . ? C12 C11 C10 130.2(3) . . ? C100 O1 P1 117.3(3) . . ? N6 C33 C32 110.1(4) . . ? N6 C33 C34 121.0(4) . . ? C32 C33 C34 128.9(3) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C200 O2 P1 122.9(3) . . ? N5 C31 C32 107.0(4) . . ? N5 C31 C30 121.9(4) . . ? C32 C31 C30 131.0(3) . . ? C31 C32 C33 106.5(3) . . ? C31 C32 H32 126.8 . . ? C33 C32 H32 126.8 . . ? C21 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C21 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C300 O3 P1 124.9(4) . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O1 C100 H10D 109.5 . . ? O1 C100 H10E 109.5 . . ? H10D C100 H10E 109.5 . . ? O1 C100 H10F 109.5 . . ? H10D C100 H10F 109.5 . . ? H10E C100 H10F 109.5 . . ? O2 C200 H20D 109.5 . . ? O2 C200 H20E 109.5 . . ? H20D C200 H20E 109.5 . . ? O2 C200 H20F 109.5 . . ? H20D C200 H20F 109.5 . . ? H20E C200 H20F 109.5 . . ? O3 C300 H30D 109.5 . . ? O3 C300 H30E 109.5 . . ? H30D C300 H30E 109.5 . . ? O3 C300 H30F 109.5 . . ? H30D C300 H30F 109.5 . . ? H30E C300 H30F 109.5 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? 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 N4 Cu1 P1 O1 148.34(15) . . . . ? N6 Cu1 P1 O1 22.83(16) . . . . ? N2 Cu1 P1 O1 -89.77(15) . . . . ? N4 Cu1 P1 O2 -90.58(16) . . . . ? N6 Cu1 P1 O2 143.91(16) . . . . ? N2 Cu1 P1 O2 31.31(15) . . . . ? N4 Cu1 P1 O3 26.8(3) . . . . ? N6 Cu1 P1 O3 -98.8(2) . . . . ? N2 Cu1 P1 O3 148.6(2) . . . . ? N4 Cu1 N2 C13 136.5(3) . . . . ? N6 Cu1 N2 C13 -137.2(3) . . . . ? P1 Cu1 N2 C13 -6.3(3) . . . . ? N4 Cu1 N2 N1 -46.29(17) . . . . ? N6 Cu1 N2 N1 40.04(17) . . . . ? P1 Cu1 N2 N1 170.97(13) . . . . ? N6 Cu1 N4 C23 139.0(3) . . . . ? N2 Cu1 N4 C23 -131.0(3) . . . . ? P1 Cu1 N4 C23 0.9(3) . . . . ? N6 Cu1 N4 N3 -50.59(17) . . . . ? N2 Cu1 N4 N3 39.45(17) . . . . ? P1 Cu1 N4 N3 171.29(13) . . . . ? C23 N4 N3 C21 1.9(3) . . . . ? Cu1 N4 N3 C21 -171.72(17) . . . . ? C23 N4 N3 C1 -178.1(2) . . . . ? Cu1 N4 N3 C1 8.3(3) . . . . ? C13 N2 N1 C11 -0.6(3) . . . . ? Cu1 N2 N1 C11 -178.77(19) . . . . ? C13 N2 N1 C1 -176.4(2) . . . . ? Cu1 N2 N1 C1 5.3(3) . . . . ? N4 Cu1 N6 C33 -127.9(3) . . . . ? N2 Cu1 N6 C33 142.4(3) . . . . ? P1 Cu1 N6 C33 16.5(3) . . . . ? N4 Cu1 N6 N5 48.09(18) . . . . ? N2 Cu1 N6 N5 -41.57(18) . . . . ? P1 Cu1 N6 N5 -167.47(14) . . . . ? C33 N6 N5 C31 -1.0(3) . . . . ? Cu1 N6 N5 C31 -178.35(19) . . . . ? C33 N6 N5 C1 175.0(2) . . . . ? Cu1 N6 N5 C1 -2.3(3) . . . . ? N3 N4 C23 C22 -1.5(3) . . . . ? Cu1 N4 C23 C22 169.3(2) . . . . ? N3 N4 C23 C24 177.2(2) . . . . ? Cu1 N4 C23 C24 -12.0(4) . . . . ? N4 C23 C22 C21 0.7(3) . . . . ? C24 C23 C22 C21 -178.0(3) . . . . ? N4 N3 C21 C22 -1.5(3) . . . . ? C1 N3 C21 C22 178.6(2) . . . . ? N4 N3 C21 C20 177.0(3) . . . . ? C1 N3 C21 C20 -3.0(4) . . . . ? C23 C22 C21 N3 0.5(3) . . . . ? C23 C22 C21 C20 -177.8(3) . . . . ? N1 N2 C13 C12 0.1(3) . . . . ? Cu1 N2 C13 C12 177.4(2) . . . . ? N1 N2 C13 C14 178.2(3) . . . . ? Cu1 N2 C13 C14 -4.5(5) . . . . ? N2 C13 C12 C11 0.4(4) . . . . ? C14 C13 C12 C11 -177.5(3) . . . . ? C11 N1 C1 N3 -120.7(3) . . . . ? N2 N1 C1 N3 54.5(3) . . . . ? C11 N1 C1 N5 121.8(3) . . . . ? N2 N1 C1 N5 -63.0(3) . . . . ? C21 N3 C1 N1 115.3(3) . . . . ? N4 N3 C1 N1 -64.7(3) . . . . ? C21 N3 C1 N5 -127.3(3) . . . . ? N4 N3 C1 N5 52.7(3) . . . . ? C31 N5 C1 N1 -123.1(3) . . . . ? N6 N5 C1 N1 61.5(3) . . . . ? C31 N5 C1 N3 119.2(3) . . . . ? N6 N5 C1 N3 -56.1(3) . . . . ? N2 N1 C11 C12 0.8(3) . . . . ? C1 N1 C11 C12 176.6(3) . . . . ? N2 N1 C11 C10 179.9(3) . . . . ? C1 N1 C11 C10 -4.3(5) . . . . ? C13 C12 C11 N1 -0.8(3) . . . . ? C13 C12 C11 C10 -179.8(4) . . . . ? O2 P1 O1 C100 -83.2(3) . . . . ? O3 P1 O1 C100 176.4(4) . . . . ? Cu1 P1 O1 C100 42.8(4) . . . . ? N5 N6 C33 C32 0.8(3) . . . . ? Cu1 N6 C33 C32 177.0(2) . . . . ? N5 N6 C33 C34 -178.4(3) . . . . ? Cu1 N6 C33 C34 -2.2(5) . . . . ? O1 P1 O2 C200 -42.2(4) . . . . ? O3 P1 O2 C200 58.7(4) . . . . ? Cu1 P1 O2 C200 -170.2(4) . . . . ? N6 N5 C31 C32 0.9(3) . . . . ? C1 N5 C31 C32 -175.0(3) . . . . ? N6 N5 C31 C30 -176.9(3) . . . . ? C1 N5 C31 C30 7.3(5) . . . . ? N5 C31 C32 C33 -0.4(4) . . . . ? C30 C31 C32 C33 177.1(4) . . . . ? N6 C33 C32 C31 -0.3(4) . . . . ? C34 C33 C32 C31 178.8(3) . . . . ? O1 P1 O3 C300 -85.4(5) . . . . ? O2 P1 O3 C300 169.0(5) . . . . ? Cu1 P1 O3 C300 44.2(6) . . . . ? #============================================================================== # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. data_C(Mepz)3AgPPh3 _database_code_depnum_ccdc_archive 'CCDC 282769' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H36 Ag N6 P, 1.5(C6 H6)' _chemical_formula_sum 'C43 H45 Ag N6 P' _chemical_formula_weight 784.69 #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall -P2yn 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 13.5388(8) _cell_length_b 14.3354(9) _cell_length_c 20.4554(11) _cell_angle_alpha 90.00 _cell_angle_beta 94.590(2) _cell_angle_gamma 90.00 _cell_volume 3957.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irregular shaped crystal' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1628 _exptl_absorpt_coefficient_mu 0.587 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8164 _exptl_absorpt_correction_T_max 0.8768 _exptl_absorpt_process_details ? #============================================================================== # EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex with CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20175 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0614 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 24.71 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 1.000 _reflns_number_total 6730 _reflns_number_gt 4924 _reflns_threshold_expression >2sigma(I) #============================================================================== # REFINEMENT DATA _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^)+(0.0403P)^2^+0.0000P] 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 undef _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6730 _refine_ls_number_parameters 465 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0900 _refine_ls_wR_factor_gt 0.0845 _refine_ls_goodness_of_fit_ref 0.929 _refine_ls_restrained_S_all 0.929 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.873 _refine_diff_density_min -0.242 _refine_diff_density_rms 0.073 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 0.0000 0.0000 '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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Ortep32 for Windows' _computing_publication_material 'Bruker SHELXTL' #============================================================================== # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Ag1 Ag 0.562724(18) 0.158680(19) 0.239882(11) 0.03602(10) Uani 1 1 d . . . P1 P 0.64435(6) 0.15592(6) 0.14433(4) 0.02834(19) Uani 1 1 d . . . N1 N 0.43518(19) 0.08557(19) 0.35188(12) 0.0359(7) Uani 1 1 d . . . C1 C 0.4633(3) 0.1737(2) 0.38183(16) 0.0385(8) Uani 1 1 d . . . N2 N 0.46065(19) 0.05655(19) 0.29114(12) 0.0345(7) Uani 1 1 d . . . N3 N 0.42790(19) 0.24993(19) 0.34069(12) 0.0356(7) Uani 1 1 d . . . N4 N 0.45449(18) 0.2640(2) 0.27794(12) 0.0354(7) Uani 1 1 d . . . N5 N 0.5696(2) 0.17873(18) 0.39397(12) 0.0345(7) Uani 1 1 d . . . N6 N 0.6357(2) 0.17095(19) 0.34660(12) 0.0347(7) Uani 1 1 d . . . C10 C 0.3434(3) 0.0312(3) 0.4452(2) 0.0744(14) Uani 1 1 d . . . H10A H 0.3996 0.0427 0.4774 0.112 Uiso 1 1 calc R . . H10B H 0.3087 -0.0255 0.4572 0.112 Uiso 1 1 calc R . . H10C H 0.2978 0.0843 0.4445 0.112 Uiso 1 1 calc R . . C11 C 0.3802(2) 0.0191(3) 0.37870(17) 0.0448(9) Uani 1 1 d . . . C12 C 0.3690(3) -0.0528(3) 0.33467(18) 0.0466(9) Uani 1 1 d . . . H12 H 0.3333 -0.1090 0.3396 0.056 Uiso 1 1 calc R . . C13 C 0.4206(2) -0.0270(3) 0.28126(16) 0.0384(8) Uani 1 1 d . . . C14 C 0.4326(3) -0.0798(3) 0.21995(17) 0.0551(11) Uani 1 1 d . . . H14A H 0.3738 -0.0711 0.1895 0.066 Uiso 1 1 calc R . . H14B H 0.4409 -0.1463 0.2302 0.066 Uiso 1 1 calc R . . H14C H 0.4912 -0.0570 0.1997 0.066 Uiso 1 1 calc R . . C20 C 0.3265(4) 0.3232(3) 0.4227(2) 0.0870(17) Uani 1 1 d . . . H20A H 0.2985 0.2624 0.4330 0.131 Uiso 1 1 calc R . . H20B H 0.2746 0.3709 0.4224 0.131 Uiso 1 1 calc R . . H20C H 0.3801 0.3390 0.4559 0.131 Uiso 1 1 calc R . . C21 C 0.3662(3) 0.3191(3) 0.35710(18) 0.0474(10) Uani 1 1 d . . . C22 C 0.3519(3) 0.3775(3) 0.30486(19) 0.0521(10) Uani 1 1 d . . . H22 H 0.3118 0.4320 0.3018 0.063 Uiso 1 1 calc R . . C23 C 0.4080(3) 0.3413(3) 0.25662(17) 0.0441(9) Uani 1 1 d . . . C24 C 0.4185(3) 0.3773(3) 0.18894(18) 0.0634(12) Uani 1 1 d . . . H24A H 0.4785 0.4155 0.1889 0.095 Uiso 1 1 calc R . . H24B H 0.3605 0.4153 0.1748 0.095 Uiso 1 1 calc R . . H24C H 0.4233 0.3247 0.1588 0.095 Uiso 1 1 calc R . . C30 C 0.5669(3) 0.2097(3) 0.51365(16) 0.0723(13) Uani 1 1 d . . . H30A H 0.5283 0.2675 0.5098 0.108 Uiso 1 1 calc R . . H30B H 0.6155 0.2137 0.5517 0.108 Uiso 1 1 calc R . . H30C H 0.5224 0.1569 0.5192 0.108 Uiso 1 1 calc R . . C31 C 0.6196(3) 0.1959(3) 0.45302(16) 0.0453(9) Uani 1 1 d . . . C32 C 0.7176(3) 0.1988(3) 0.44319(17) 0.0494(10) Uani 1 1 d . . . H32 H 0.7709 0.2094 0.4754 0.059 Uiso 1 1 calc R . . C33 C 0.7246(3) 0.1831(2) 0.37693(16) 0.0391(9) Uani 1 1 d . . . C34 C 0.8144(3) 0.1812(3) 0.33885(18) 0.0541(11) Uani 1 1 d . . . H34A H 0.8128 0.1253 0.3112 0.081 Uiso 1 1 calc R . . H34B H 0.8742 0.1802 0.3693 0.081 Uiso 1 1 calc R . . H34C H 0.8152 0.2369 0.3111 0.081 Uiso 1 1 calc R . . C100 C 0.5642(2) 0.1481(2) 0.06832(15) 0.0323(8) Uani 1 1 d . . . C101 C 0.4705(3) 0.1109(3) 0.07134(18) 0.0473(9) Uani 1 1 d . . . H101 H 0.4489 0.0932 0.1126 0.057 Uiso 1 1 calc R . . C102 C 0.4075(3) 0.0990(3) 0.0149(2) 0.0644(12) Uani 1 1 d . . . H102 H 0.3433 0.0731 0.0175 0.077 Uiso 1 1 calc R . . C103 C 0.4387(3) 0.1248(3) -0.0439(2) 0.0610(12) Uani 1 1 d . . . H103 H 0.3958 0.1169 -0.0826 0.073 Uiso 1 1 calc R . . C104 C 0.5311(3) 0.1621(3) -0.04824(17) 0.0557(11) Uani 1 1 d . . . H104 H 0.5522 0.1794 -0.0897 0.067 Uiso 1 1 calc R . . C105 C 0.5934(3) 0.1745(2) 0.00768(15) 0.0409(9) Uani 1 1 d . . . H105 H 0.6570 0.2014 0.0046 0.049 Uiso 1 1 calc R . . C200 C 0.7223(2) 0.2573(2) 0.13288(14) 0.0305(8) Uani 1 1 d . . . C201 C 0.6794(3) 0.3415(3) 0.11440(17) 0.0447(9) Uani 1 1 d . . . H201 H 0.6099 0.3448 0.1041 0.054 Uiso 1 1 calc R . . C202 C 0.7362(3) 0.4209(3) 0.11068(18) 0.0555(11) Uani 1 1 d . . . H202 H 0.7054 0.4783 0.0978 0.067 Uiso 1 1 calc R . . C203 C 0.8367(3) 0.4176(3) 0.12549(18) 0.0572(11) Uani 1 1 d . . . H203 H 0.8758 0.4723 0.1228 0.069 Uiso 1 1 calc R . . C204 C 0.8799(3) 0.3350(3) 0.14416(19) 0.0581(11) Uani 1 1 d . . . H204 H 0.9494 0.3323 0.1550 0.070 Uiso 1 1 calc R . . C205 C 0.8234(3) 0.2548(3) 0.14751(17) 0.0465(9) Uani 1 1 d . . . H205 H 0.8546 0.1975 0.1600 0.056 Uiso 1 1 calc R . . C300 C 0.7290(2) 0.0574(2) 0.14071(14) 0.0300(7) Uani 1 1 d . . . C301 C 0.7415(2) -0.0023(2) 0.19357(16) 0.0393(8) Uani 1 1 d . . . H301 H 0.7045 0.0074 0.2306 0.047 Uiso 1 1 calc R . . C302 C 0.8069(3) -0.0760(3) 0.19338(19) 0.0543(10) Uani 1 1 d . . . H302 H 0.8142 -0.1168 0.2301 0.065 Uiso 1 1 calc R . . C303 C 0.8613(3) -0.0910(3) 0.1411(2) 0.0534(10) Uani 1 1 d . . . H303 H 0.9075 -0.1409 0.1419 0.064 Uiso 1 1 calc R . . C304 C 0.8489(3) -0.0337(3) 0.08736(19) 0.0520(10) Uani 1 1 d . . . H304 H 0.8852 -0.0450 0.0503 0.062 Uiso 1 1 calc R . . C305 C 0.7832(2) 0.0410(3) 0.08706(16) 0.0412(9) Uani 1 1 d . . . H305 H 0.7754 0.0810 0.0500 0.049 Uiso 1 1 calc R . . C901 C 0.4760(6) 0.4097(4) -0.0066(4) 0.100(2) Uani 1 1 d . . . H901 H 0.4584 0.3458 -0.0118 0.120 Uiso 1 1 calc R . . C900 C 0.4240(4) 0.4646(7) 0.0294(3) 0.0977(19) Uani 1 1 d . . . H900 H 0.3702 0.4397 0.0509 0.117 Uiso 1 1 calc R . . C902 C 0.5531(5) 0.4432(7) -0.0359(3) 0.112(2) Uani 1 1 d . . . H902 H 0.5915 0.4033 -0.0609 0.134 Uiso 1 1 calc R . . C801 C 1.0424(5) 0.1126(5) 0.2156(4) 0.113(2) Uani 1 1 d . . . H801 H 0.9750 0.0966 0.2198 0.136 Uiso 1 1 calc R . . C802 C 1.0766(5) 0.1155(5) 0.1563(4) 0.121(3) Uani 1 1 d . . . H802 H 1.0333 0.1040 0.1183 0.145 Uiso 1 1 calc R . . C803 C 1.1758(6) 0.1356(5) 0.1503(4) 0.139(3) Uani 1 1 d . . . H803 H 1.2019 0.1370 0.1086 0.167 Uiso 1 1 calc R . . C800 C 1.1018(7) 0.1318(5) 0.2693(4) 0.129(3) Uani 1 1 d . . . H800 H 1.0766 0.1320 0.3113 0.155 Uiso 1 1 calc R . . C804 C 1.2327(8) 0.1526(7) 0.2045(6) 0.169(6) Uani 1 1 d . . . H804 H 1.3006 0.1663 0.2006 0.202 Uiso 1 1 calc R . . C805 C 1.2012(9) 0.1516(7) 0.2628(5) 0.174(6) Uani 1 1 d . . . H805 H 1.2451 0.1641 0.3003 0.208 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 Ag1 0.03872(16) 0.03880(17) 0.03185(14) -0.00340(13) 0.01101(10) -0.00185(13) P1 0.0295(5) 0.0283(5) 0.0276(4) -0.0013(4) 0.0043(3) 0.0003(4) N1 0.0381(17) 0.0341(18) 0.0367(15) 0.0006(14) 0.0102(13) -0.0041(13) C1 0.043(2) 0.036(2) 0.0379(19) -0.0035(17) 0.0105(16) -0.0034(16) N2 0.0375(16) 0.0339(18) 0.0328(15) -0.0010(13) 0.0067(12) -0.0047(13) N3 0.0369(16) 0.0345(18) 0.0367(15) -0.0032(14) 0.0115(13) -0.0002(13) N4 0.0365(17) 0.0343(18) 0.0369(15) 0.0007(13) 0.0119(13) 0.0014(13) N5 0.0449(18) 0.0311(18) 0.0280(14) -0.0029(12) 0.0053(13) -0.0023(13) N6 0.0384(17) 0.0327(18) 0.0331(14) -0.0028(13) 0.0029(12) -0.0047(13) C10 0.089(3) 0.064(3) 0.077(3) 0.003(3) 0.050(3) -0.015(3) C11 0.040(2) 0.042(2) 0.055(2) 0.008(2) 0.0148(17) -0.0074(18) C12 0.042(2) 0.034(2) 0.064(2) 0.009(2) 0.0061(18) -0.0126(17) C13 0.036(2) 0.036(2) 0.043(2) -0.0013(18) -0.0044(15) -0.0025(17) C14 0.068(3) 0.041(3) 0.055(2) -0.007(2) -0.001(2) -0.013(2) C20 0.108(4) 0.087(4) 0.073(3) -0.008(3) 0.051(3) 0.034(3) C21 0.047(2) 0.042(3) 0.055(2) -0.0087(19) 0.0195(18) 0.0073(18) C22 0.047(2) 0.043(2) 0.068(3) 0.004(2) 0.015(2) 0.0146(19) C23 0.040(2) 0.039(2) 0.053(2) 0.002(2) 0.0074(17) 0.0028(18) C24 0.071(3) 0.059(3) 0.061(3) 0.019(2) 0.013(2) 0.023(2) C30 0.094(3) 0.092(4) 0.032(2) -0.007(2) 0.006(2) -0.001(3) C31 0.068(3) 0.037(2) 0.0308(19) -0.0001(17) -0.0003(18) -0.0003(19) C32 0.056(3) 0.051(3) 0.039(2) -0.0019(19) -0.0128(18) -0.003(2) C33 0.041(2) 0.030(2) 0.045(2) 0.0008(17) -0.0037(17) -0.0013(16) C34 0.041(2) 0.061(3) 0.059(2) -0.001(2) -0.0045(18) -0.0038(19) C100 0.0349(19) 0.027(2) 0.0341(18) -0.0043(15) -0.0039(14) 0.0075(15) C101 0.042(2) 0.044(2) 0.055(2) 0.005(2) -0.0034(18) -0.0021(18) C102 0.050(3) 0.057(3) 0.081(3) -0.001(3) -0.026(2) -0.006(2) C103 0.072(3) 0.046(3) 0.059(3) -0.012(2) -0.031(2) 0.013(2) C104 0.082(3) 0.047(3) 0.036(2) -0.0050(19) -0.008(2) 0.016(2) C105 0.045(2) 0.041(2) 0.0358(19) -0.0069(17) -0.0007(16) 0.0069(17) C200 0.038(2) 0.029(2) 0.0247(16) -0.0024(15) 0.0068(14) -0.0020(15) C201 0.046(2) 0.038(2) 0.050(2) 0.0010(19) 0.0028(17) -0.0002(19) C202 0.082(3) 0.030(2) 0.055(2) 0.0040(19) 0.005(2) -0.002(2) C203 0.081(3) 0.043(3) 0.049(2) -0.006(2) 0.012(2) -0.029(2) C204 0.046(2) 0.058(3) 0.070(3) -0.002(2) 0.003(2) -0.019(2) C205 0.041(2) 0.038(2) 0.060(2) 0.0030(19) 0.0012(18) -0.0029(17) C300 0.0291(18) 0.028(2) 0.0324(17) -0.0020(15) -0.0023(14) -0.0014(14) C301 0.047(2) 0.032(2) 0.0384(19) 0.0040(16) -0.0007(16) 0.0003(17) C302 0.066(3) 0.033(2) 0.062(3) 0.009(2) -0.011(2) 0.007(2) C303 0.049(2) 0.033(2) 0.076(3) -0.006(2) -0.012(2) 0.0130(18) C304 0.046(2) 0.052(3) 0.058(2) -0.014(2) 0.0079(18) 0.010(2) C305 0.044(2) 0.042(2) 0.0388(19) 0.0034(17) 0.0071(16) 0.0097(17) C901 0.073(4) 0.060(4) 0.156(6) 0.004(4) -0.051(4) 0.012(3) C900 0.081(4) 0.121(6) 0.090(4) 0.047(4) 0.002(3) 0.005(5) C902 0.091(5) 0.136(8) 0.107(5) -0.058(5) -0.007(4) 0.026(4) C801 0.074(4) 0.086(5) 0.176(7) 0.050(5) -0.017(5) -0.002(3) C802 0.079(5) 0.111(5) 0.163(7) 0.058(5) -0.047(4) -0.014(4) C803 0.094(6) 0.111(6) 0.213(9) 0.086(6) 0.010(5) 0.009(4) C800 0.145(7) 0.079(5) 0.156(7) 0.003(4) -0.035(6) 0.023(5) C804 0.078(6) 0.071(5) 0.342(17) 0.049(10) -0.073(10) -0.016(4) C805 0.172(12) 0.062(5) 0.260(13) -0.022(8) -0.145(11) 0.004(6) #============================================================================== # 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 Ag1 N4 2.284(3) . ? Ag1 N2 2.321(3) . ? Ag1 P1 2.3215(8) . ? Ag1 N6 2.329(3) . ? P1 C200 1.822(3) . ? P1 C300 1.824(3) . ? P1 C100 1.827(3) . ? N1 C11 1.353(4) . ? N1 N2 1.380(3) . ? N1 C1 1.442(4) . ? C1 N3 1.438(4) . ? C1 N5 1.443(4) . ? N2 C13 1.323(4) . ? N3 C21 1.356(4) . ? N3 N4 1.375(3) . ? N4 C23 1.330(4) . ? N5 C31 1.359(4) . ? N5 N6 1.374(3) . ? N6 C33 1.322(4) . ? C10 C11 1.495(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.369(5) . ? C12 C13 1.392(5) . ? C12 H12 0.9500 . ? C13 C14 1.486(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C20 C21 1.486(5) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.359(5) . ? C22 C23 1.393(5) . ? C22 H22 0.9500 . ? C23 C24 1.495(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C30 C31 1.492(5) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.359(5) . ? C32 C33 1.385(4) . ? C32 H32 0.9500 . ? C33 C34 1.496(5) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C100 C101 1.381(5) . ? C100 C105 1.385(4) . ? C101 C102 1.390(5) . ? C101 H101 0.9500 . ? C102 C103 1.359(5) . ? C102 H102 0.9500 . ? C103 C104 1.370(6) . ? C103 H103 0.9500 . ? C104 C105 1.378(5) . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? C200 C205 1.378(4) . ? C200 C201 1.378(5) . ? C201 C202 1.379(5) . ? C201 H201 0.9500 . ? C202 C203 1.371(5) . ? C202 H202 0.9500 . ? C203 C204 1.362(5) . ? C203 H203 0.9500 . ? C204 C205 1.386(5) . ? C204 H204 0.9500 . ? C205 H205 0.9500 . ? C300 C301 1.379(4) . ? C300 C305 1.388(4) . ? C301 C302 1.379(5) . ? C301 H301 0.9500 . ? C302 C303 1.363(5) . ? C302 H302 0.9500 . ? C303 C304 1.372(5) . ? C303 H303 0.9500 . ? C304 C305 1.392(5) . ? C304 H304 0.9500 . ? C305 H305 0.9500 . ? C901 C900 1.320(7) . ? C901 C902 1.333(8) . ? C901 H901 0.9500 . ? C900 C902 1.361(9) 3_665 ? C900 H900 0.9500 . ? C902 C900 1.361(9) 3_665 ? C902 H902 0.9500 . ? C801 C802 1.334(8) . ? C801 C800 1.337(9) . ? C801 H801 0.9500 . ? C802 C803 1.387(8) . ? C802 H802 0.9500 . ? C803 C804 1.322(11) . ? C803 H803 0.9500 . ? C800 C805 1.391(11) . ? C800 H800 0.9500 . ? C804 C805 1.297(14) . ? C804 H804 0.9500 . ? C805 H805 0.9500 . ? 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 Ag1 N2 80.88(9) . . ? N4 Ag1 P1 131.29(7) . . ? N2 Ag1 P1 135.28(7) . . ? N4 Ag1 N6 82.30(9) . . ? N2 Ag1 N6 81.22(9) . . ? P1 Ag1 N6 126.56(7) . . ? C200 P1 C300 103.89(14) . . ? C200 P1 C100 104.50(15) . . ? C300 P1 C100 104.51(14) . . ? C200 P1 Ag1 114.47(10) . . ? C300 P1 Ag1 112.97(10) . . ? C100 P1 Ag1 115.28(11) . . ? C11 N1 N2 109.8(3) . . ? C11 N1 C1 125.5(3) . . ? N2 N1 C1 124.8(2) . . ? N3 C1 N1 110.7(3) . . ? N3 C1 N5 110.1(3) . . ? N1 C1 N5 110.0(3) . . ? C13 N2 N1 106.3(3) . . ? C13 N2 Ag1 138.9(2) . . ? N1 N2 Ag1 114.67(19) . . ? C21 N3 N4 109.6(3) . . ? C21 N3 C1 126.4(3) . . ? N4 N3 C1 123.9(3) . . ? C23 N4 N3 106.0(3) . . ? C23 N4 Ag1 137.6(2) . . ? N3 N4 Ag1 116.36(19) . . ? C31 N5 N6 109.6(3) . . ? C31 N5 C1 125.5(3) . . ? N6 N5 C1 124.8(2) . . ? C33 N6 N5 106.1(3) . . ? C33 N6 Ag1 138.8(2) . . ? N5 N6 Ag1 114.59(18) . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 107.4(3) . . ? N1 C11 C10 121.4(3) . . ? C12 C11 C10 131.2(3) . . ? C11 C12 C13 106.3(3) . . ? C11 C12 H12 126.9 . . ? C13 C12 H12 126.9 . . ? N2 C13 C12 110.2(3) . . ? N2 C13 C14 121.3(3) . . ? C12 C13 C14 128.5(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C21 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C21 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 C22 107.9(3) . . ? N3 C21 C20 121.8(3) . . ? C22 C21 C20 130.3(3) . . ? C21 C22 C23 106.0(3) . . ? C21 C22 H22 127.0 . . ? C23 C22 H22 127.0 . . ? N4 C23 C22 110.4(3) . . ? N4 C23 C24 121.0(3) . . ? C22 C23 C24 128.6(4) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N5 C31 C32 107.2(3) . . ? N5 C31 C30 121.7(3) . . ? C32 C31 C30 131.0(3) . . ? C31 C32 C33 106.5(3) . . ? C31 C32 H32 126.7 . . ? C33 C32 H32 126.7 . . ? N6 C33 C32 110.5(3) . . ? N6 C33 C34 120.1(3) . . ? C32 C33 C34 129.4(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C101 C100 C105 118.4(3) . . ? C101 C100 P1 118.1(3) . . ? C105 C100 P1 123.5(3) . . ? C100 C101 C102 121.0(4) . . ? C100 C101 H101 119.5 . . ? C102 C101 H101 119.5 . . ? C103 C102 C101 119.2(4) . . ? C103 C102 H102 120.4 . . ? C101 C102 H102 120.4 . . ? C102 C103 C104 120.9(4) . . ? C102 C103 H103 119.5 . . ? C104 C103 H103 119.5 . . ? C103 C104 C105 119.9(4) . . ? C103 C104 H104 120.0 . . ? C105 C104 H104 120.0 . . ? C104 C105 C100 120.6(4) . . ? C104 C105 H105 119.7 . . ? C100 C105 H105 119.7 . . ? C205 C200 C201 118.1(3) . . ? C205 C200 P1 121.8(3) . . ? C201 C200 P1 119.9(3) . . ? C200 C201 C202 120.9(4) . . ? C200 C201 H201 119.5 . . ? C202 C201 H201 119.5 . . ? C203 C202 C201 120.5(4) . . ? C203 C202 H202 119.8 . . ? C201 C202 H202 119.8 . . ? C204 C203 C202 119.2(4) . . ? C204 C203 H203 120.4 . . ? C202 C203 H203 120.4 . . ? C203 C204 C205 120.5(4) . . ? C203 C204 H204 119.7 . . ? C205 C204 H204 119.7 . . ? C200 C205 C204 120.7(4) . . ? C200 C205 H205 119.6 . . ? C204 C205 H205 119.6 . . ? C301 C300 C305 118.4(3) . . ? C301 C300 P1 119.1(2) . . ? C305 C300 P1 122.5(2) . . ? C300 C301 C302 120.8(3) . . ? C300 C301 H301 119.6 . . ? C302 C301 H301 119.6 . . ? C303 C302 C301 120.7(4) . . ? C303 C302 H302 119.7 . . ? C301 C302 H302 119.7 . . ? C302 C303 C304 119.7(4) . . ? C302 C303 H303 120.2 . . ? C304 C303 H303 120.2 . . ? C303 C304 C305 120.1(3) . . ? C303 C304 H304 119.9 . . ? C305 C304 H304 119.9 . . ? C300 C305 C304 120.3(3) . . ? C300 C305 H305 119.8 . . ? C304 C305 H305 119.8 . . ? C900 C901 C902 120.5(6) . . ? C900 C901 H901 119.7 . . ? C902 C901 H901 119.7 . . ? C901 C900 C902 120.3(6) . 3_665 ? C901 C900 H900 119.8 . . ? C902 C900 H900 119.8 3_665 . ? C901 C902 C900 119.1(6) . 3_665 ? C901 C902 H902 120.4 . . ? C900 C902 H902 120.4 3_665 . ? C802 C801 C800 120.6(7) . . ? C802 C801 H801 119.7 . . ? C800 C801 H801 119.7 . . ? C801 C802 C803 119.8(7) . . ? C801 C802 H802 120.1 . . ? C803 C802 H802 120.1 . . ? C804 C803 C802 117.9(9) . . ? C804 C803 H803 121.1 . . ? C802 C803 H803 121.1 . . ? C801 C800 C805 119.1(8) . . ? C801 C800 H800 120.4 . . ? C805 C800 H800 120.4 . . ? C805 C804 C803 123.8(12) . . ? C805 C804 H804 118.1 . . ? C803 C804 H804 118.1 . . ? C804 C805 C800 118.8(11) . . ? C804 C805 H805 120.6 . . ? C800 C805 H805 120.6 . . ? 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 N4 Ag1 P1 C200 57.95(15) . . . . ? N2 Ag1 P1 C200 -176.09(15) . . . . ? N6 Ag1 P1 C200 -57.48(15) . . . . ? N4 Ag1 P1 C300 176.59(14) . . . . ? N2 Ag1 P1 C300 -57.44(15) . . . . ? N6 Ag1 P1 C300 61.16(14) . . . . ? N4 Ag1 P1 C100 -63.32(15) . . . . ? N2 Ag1 P1 C100 62.64(16) . . . . ? N6 Ag1 P1 C100 -178.75(14) . . . . ? C11 N1 C1 N3 -121.6(3) . . . . ? N2 N1 C1 N3 58.4(4) . . . . ? C11 N1 C1 N5 116.4(3) . . . . ? N2 N1 C1 N5 -63.6(4) . . . . ? C11 N1 N2 C13 0.4(4) . . . . ? C1 N1 N2 C13 -179.6(3) . . . . ? C11 N1 N2 Ag1 -176.8(2) . . . . ? C1 N1 N2 Ag1 3.2(4) . . . . ? N4 Ag1 N2 C13 140.8(3) . . . . ? P1 Ag1 N2 C13 -1.2(4) . . . . ? N6 Ag1 N2 C13 -135.6(3) . . . . ? N4 Ag1 N2 N1 -43.3(2) . . . . ? P1 Ag1 N2 N1 174.76(15) . . . . ? N6 Ag1 N2 N1 40.3(2) . . . . ? N1 C1 N3 C21 121.1(3) . . . . ? N5 C1 N3 C21 -117.0(3) . . . . ? N1 C1 N3 N4 -60.3(4) . . . . ? N5 C1 N3 N4 61.6(4) . . . . ? C21 N3 N4 C23 -0.5(4) . . . . ? C1 N3 N4 C23 -179.2(3) . . . . ? C21 N3 N4 Ag1 178.1(2) . . . . ? C1 N3 N4 Ag1 -0.6(4) . . . . ? N2 Ag1 N4 C23 -139.6(4) . . . . ? P1 Ag1 N4 C23 5.1(4) . . . . ? N6 Ag1 N4 C23 138.1(4) . . . . ? N2 Ag1 N4 N3 42.4(2) . . . . ? P1 Ag1 N4 N3 -172.86(16) . . . . ? N6 Ag1 N4 N3 -39.9(2) . . . . ? N3 C1 N5 C31 113.2(3) . . . . ? N1 C1 N5 C31 -124.5(3) . . . . ? N3 C1 N5 N6 -63.6(4) . . . . ? N1 C1 N5 N6 58.6(4) . . . . ? C31 N5 N6 C33 0.2(3) . . . . ? C1 N5 N6 C33 177.5(3) . . . . ? C31 N5 N6 Ag1 -173.2(2) . . . . ? C1 N5 N6 Ag1 4.1(4) . . . . ? N4 Ag1 N6 C33 -132.2(3) . . . . ? N2 Ag1 N6 C33 145.9(4) . . . . ? P1 Ag1 N6 C33 4.6(4) . . . . ? N4 Ag1 N6 N5 38.1(2) . . . . ? N2 Ag1 N6 N5 -43.8(2) . . . . ? P1 Ag1 N6 N5 174.86(16) . . . . ? N2 N1 C11 C12 -0.7(4) . . . . ? C1 N1 C11 C12 179.2(3) . . . . ? N2 N1 C11 C10 179.0(3) . . . . ? C1 N1 C11 C10 -1.0(5) . . . . ? N1 C11 C12 C13 0.8(4) . . . . ? C10 C11 C12 C13 -179.0(4) . . . . ? N1 N2 C13 C12 0.1(4) . . . . ? Ag1 N2 C13 C12 176.3(2) . . . . ? N1 N2 C13 C14 179.8(3) . . . . ? Ag1 N2 C13 C14 -4.0(5) . . . . ? C11 C12 C13 N2 -0.6(4) . . . . ? C11 C12 C13 C14 179.8(4) . . . . ? N4 N3 C21 C22 0.6(4) . . . . ? C1 N3 C21 C22 179.3(3) . . . . ? N4 N3 C21 C20 -179.0(3) . . . . ? C1 N3 C21 C20 -0.3(6) . . . . ? N3 C21 C22 C23 -0.5(4) . . . . ? C20 C21 C22 C23 179.1(4) . . . . ? N3 N4 C23 C22 0.2(4) . . . . ? Ag1 N4 C23 C22 -178.0(3) . . . . ? N3 N4 C23 C24 -179.0(3) . . . . ? Ag1 N4 C23 C24 2.9(6) . . . . ? C21 C22 C23 N4 0.2(4) . . . . ? C21 C22 C23 C24 179.2(4) . . . . ? N6 N5 C31 C32 -0.2(4) . . . . ? C1 N5 C31 C32 -177.5(3) . . . . ? N6 N5 C31 C30 178.7(3) . . . . ? C1 N5 C31 C30 1.4(5) . . . . ? N5 C31 C32 C33 0.1(4) . . . . ? C30 C31 C32 C33 -178.6(4) . . . . ? N5 N6 C33 C32 -0.1(4) . . . . ? Ag1 N6 C33 C32 170.7(3) . . . . ? N5 N6 C33 C34 -178.5(3) . . . . ? Ag1 N6 C33 C34 -7.7(5) . . . . ? C31 C32 C33 N6 0.0(4) . . . . ? C31 C32 C33 C34 178.2(4) . . . . ? C200 P1 C100 C101 -149.9(3) . . . . ? C300 P1 C100 C101 101.3(3) . . . . ? Ag1 P1 C100 C101 -23.3(3) . . . . ? C200 P1 C100 C105 32.4(3) . . . . ? C300 P1 C100 C105 -76.5(3) . . . . ? Ag1 P1 C100 C105 158.9(2) . . . . ? C105 C100 C101 C102 0.9(5) . . . . ? P1 C100 C101 C102 -177.0(3) . . . . ? C100 C101 C102 C103 -0.3(6) . . . . ? C101 C102 C103 C104 0.1(7) . . . . ? C102 C103 C104 C105 -0.5(6) . . . . ? C103 C104 C105 C100 1.1(6) . . . . ? C101 C100 C105 C104 -1.2(5) . . . . ? P1 C100 C105 C104 176.5(3) . . . . ? C300 P1 C200 C205 -23.9(3) . . . . ? C100 P1 C200 C205 -133.2(3) . . . . ? Ag1 P1 C200 C205 99.7(3) . . . . ? C300 P1 C200 C201 161.7(3) . . . . ? C100 P1 C200 C201 52.4(3) . . . . ? Ag1 P1 C200 C201 -74.7(3) . . . . ? C205 C200 C201 C202 0.0(5) . . . . ? P1 C200 C201 C202 174.6(3) . . . . ? C200 C201 C202 C203 -0.1(6) . . . . ? C201 C202 C203 C204 -0.2(6) . . . . ? C202 C203 C204 C205 0.7(6) . . . . ? C201 C200 C205 C204 0.5(5) . . . . ? P1 C200 C205 C204 -174.0(3) . . . . ? C203 C204 C205 C200 -0.9(6) . . . . ? C200 P1 C300 C301 121.5(3) . . . . ? C100 P1 C300 C301 -129.2(3) . . . . ? Ag1 P1 C300 C301 -3.1(3) . . . . ? C200 P1 C300 C305 -57.2(3) . . . . ? C100 P1 C300 C305 52.1(3) . . . . ? Ag1 P1 C300 C305 178.1(2) . . . . ? C305 C300 C301 C302 0.6(5) . . . . ? P1 C300 C301 C302 -178.2(3) . . . . ? C300 C301 C302 C303 0.5(6) . . . . ? C301 C302 C303 C304 -1.7(6) . . . . ? C302 C303 C304 C305 1.9(6) . . . . ? C301 C300 C305 C304 -0.5(5) . . . . ? P1 C300 C305 C304 178.3(3) . . . . ? C303 C304 C305 C300 -0.7(6) . . . . ? C902 C901 C900 C902 1.6(10) . . . 3_665 ? C900 C901 C902 C900 -1.6(10) . . . 3_665 ? C800 C801 C802 C803 2.3(11) . . . . ? C801 C802 C803 C804 -1.0(11) . . . . ? C802 C801 C800 C805 -2.5(11) . . . . ? C802 C803 C804 C805 0.0(16) . . . . ? C803 C804 C805 C800 -0.2(19) . . . . ? C801 C800 C805 C804 1.4(15) . . . . ? #============================================================================== # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. data_Ph3PAuC(Mepz)3 _database_code_depnum_ccdc_archive 'CCDC 282770' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H36 Au N6 P' _chemical_formula_sum 'C34 H36 Au N6 P' _chemical_formula_weight 756.62 #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0963(5) _cell_length_b 11.8099(7) _cell_length_c 16.4408(9) _cell_angle_alpha 74.0390(10) _cell_angle_beta 80.5070(10) _cell_angle_gamma 69.7070(10) _cell_volume 1587.95(16) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irregular shaped crystal' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 4.716 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4375 _exptl_absorpt_correction_T_max 0.5581 _exptl_absorpt_process_details 'Blessing, 1995' #============================================================================== # EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex with CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16147 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 28.28 _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.979 _reflns_number_total 7717 _reflns_number_gt 7120 _reflns_threshold_expression >2sigma(I) #============================================================================== # REFINEMENT DATA _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^)+(0.0470P)^2^+0.0000P] 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 undef _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7717 _refine_ls_number_parameters 385 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.0951 _refine_ls_wR_factor_gt 0.0928 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 2.555 _refine_diff_density_min -0.824 _refine_diff_density_rms 0.161 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 0.0000 0.0000 '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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Ortep32 for Windows' _computing_publication_material 'Bruker SHELXTL' #============================================================================== # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Au1 Au 0.48223(2) 0.191903(15) 0.242659(11) 0.02365(7) Uani 1 1 d . . . P1 P 0.64880(15) -0.00557(11) 0.25417(8) 0.0256(2) Uani 1 1 d . . . C1 C 0.3200(5) 0.3706(4) 0.2412(3) 0.0223(9) Uani 1 1 d . . . N1 N 0.1786(4) 0.3533(3) 0.2911(2) 0.0232(8) Uani 1 1 d . . . N2 N 0.1985(5) 0.2439(3) 0.3513(2) 0.0263(8) Uani 1 1 d . . . N3 N 0.3767(4) 0.4440(3) 0.2802(2) 0.0220(8) Uani 1 1 d . . . N4 N 0.2786(5) 0.5081(4) 0.3362(3) 0.0280(9) Uani 1 1 d . . . N5 N 0.2742(5) 0.4469(3) 0.1552(2) 0.0243(8) Uani 1 1 d . . . N6 N 0.3014(5) 0.5567(4) 0.1231(3) 0.0318(9) Uani 1 1 d . . . C10 C -0.0304(6) 0.5592(5) 0.2423(4) 0.0366(12) Uani 1 1 d . . . H10A H 0.0395 0.6063 0.2425 0.055 Uiso 1 1 calc R . . H10B H -0.1366 0.6014 0.2642 0.055 Uiso 1 1 calc R . . H10C H -0.0332 0.5537 0.1843 0.055 Uiso 1 1 calc R . . C11 C 0.0292(6) 0.4315(4) 0.2974(3) 0.0271(10) Uani 1 1 d . . . C12 C -0.0490(6) 0.3702(5) 0.3627(3) 0.0334(11) Uani 1 1 d . . . H12A H -0.1565 0.3997 0.3824 0.040 Uiso 1 1 calc R . . C13 C 0.0607(6) 0.2553(5) 0.3952(3) 0.0304(10) Uani 1 1 d . . . C14 C 0.0384(8) 0.1511(5) 0.4667(4) 0.0504(16) Uani 1 1 d . . . H14A H 0.1120 0.0721 0.4567 0.076 Uiso 1 1 calc R . . H14B H -0.0696 0.1498 0.4701 0.076 Uiso 1 1 calc R . . H14C H 0.0581 0.1631 0.5201 0.076 Uiso 1 1 calc R . . C20 C 0.6477(6) 0.4132(5) 0.2047(4) 0.0376(12) Uani 1 1 d . . . H20A H 0.6780 0.3223 0.2183 0.056 Uiso 1 1 calc R . . H20B H 0.7387 0.4382 0.2070 0.056 Uiso 1 1 calc R . . H20C H 0.6104 0.4470 0.1477 0.056 Uiso 1 1 calc R . . C21 C 0.5198(6) 0.4619(4) 0.2675(3) 0.0271(10) Uani 1 1 d . . . C22 C 0.5142(6) 0.5361(4) 0.3202(3) 0.0315(11) Uani 1 1 d . . . H22A H 0.5964 0.5638 0.3274 0.038 Uiso 1 1 calc R . . C23 C 0.3640(6) 0.5621(5) 0.3607(3) 0.0313(11) Uani 1 1 d . . . C24 C 0.2938(8) 0.6382(6) 0.4245(4) 0.0512(16) Uani 1 1 d . . . H24A H 0.1840 0.6411 0.4398 0.077 Uiso 1 1 calc R . . H24B H 0.2985 0.7227 0.4004 0.077 Uiso 1 1 calc R . . H24C H 0.3528 0.6009 0.4752 0.077 Uiso 1 1 calc R . . C30 C 0.1584(7) 0.3028(5) 0.1197(3) 0.0371(12) Uani 1 1 d . . . H30A H 0.2446 0.2294 0.1434 0.056 Uiso 1 1 calc R . . H30B H 0.1306 0.2928 0.0676 0.056 Uiso 1 1 calc R . . H30C H 0.0668 0.3122 0.1611 0.056 Uiso 1 1 calc R . . C31 C 0.2088(6) 0.4149(5) 0.1002(3) 0.0293(10) Uani 1 1 d . . . C32 C 0.1926(7) 0.5104(5) 0.0284(3) 0.0384(12) Uani 1 1 d . . . H32A H 0.1497 0.5172 -0.0223 0.046 Uiso 1 1 calc R . . C33 C 0.2522(7) 0.5952(5) 0.0454(3) 0.0402(13) Uani 1 1 d . . . C34 C 0.2630(11) 0.7165(6) -0.0106(4) 0.067(2) Uani 1 1 d . . . H34A H 0.2545 0.7737 0.0245 0.101 Uiso 1 1 calc R . . H34B H 0.1774 0.7525 -0.0485 0.101 Uiso 1 1 calc R . . H34C H 0.3642 0.7023 -0.0444 0.101 Uiso 1 1 calc R . . C100 C 0.6137(6) -0.1025(4) 0.3568(3) 0.0282(10) Uani 1 1 d . . . C101 C 0.4735(7) -0.0610(5) 0.4051(3) 0.0345(11) Uani 1 1 d . . . H10D H 0.3974 0.0166 0.3842 0.041 Uiso 1 1 calc R . . C102 C 0.4464(8) -0.1344(5) 0.4840(4) 0.0429(13) Uani 1 1 d . . . H10E H 0.3510 -0.1067 0.5171 0.051 Uiso 1 1 calc R . . C103 C 0.5542(8) -0.2454(6) 0.5146(4) 0.0439(14) Uani 1 1 d . . . H10F H 0.5338 -0.2944 0.5689 0.053 Uiso 1 1 calc R . . C104 C 0.6918(8) -0.2870(5) 0.4678(4) 0.0477(15) Uani 1 1 d . . . H10G H 0.7665 -0.3651 0.4895 0.057 Uiso 1 1 calc R . . C105 C 0.7222(7) -0.2163(5) 0.3897(4) 0.0416(13) Uani 1 1 d . . . H10H H 0.8186 -0.2454 0.3577 0.050 Uiso 1 1 calc R . . C200 C 0.6336(6) -0.0830(4) 0.1759(3) 0.0276(10) Uani 1 1 d . . . C201 C 0.5734(6) -0.1808(4) 0.1971(3) 0.0313(11) Uani 1 1 d . . . H20D H 0.5409 -0.2109 0.2546 0.038 Uiso 1 1 calc R . . C202 C 0.5601(6) -0.2355(5) 0.1350(4) 0.0349(11) Uani 1 1 d . . . H20E H 0.5163 -0.3014 0.1498 0.042 Uiso 1 1 calc R . . C203 C 0.6103(7) -0.1941(5) 0.0524(4) 0.0447(14) Uani 1 1 d . . . H20F H 0.6027 -0.2323 0.0100 0.054 Uiso 1 1 calc R . . C204 C 0.6721(9) -0.0966(6) 0.0305(4) 0.0521(16) Uani 1 1 d . . . H20G H 0.7072 -0.0684 -0.0268 0.063 Uiso 1 1 calc R . . C205 C 0.6825(8) -0.0406(5) 0.0919(4) 0.0426(14) Uani 1 1 d . . . H20H H 0.7232 0.0270 0.0767 0.051 Uiso 1 1 calc R . . C300 C 0.8558(6) -0.0213(4) 0.2457(3) 0.0286(10) Uani 1 1 d . . . C301 C 0.9011(7) 0.0597(5) 0.2769(4) 0.0377(12) Uani 1 1 d . . . H30D H 0.8233 0.1225 0.3003 0.045 Uiso 1 1 calc R . . C302 C 1.0552(8) 0.0493(6) 0.2739(5) 0.0523(16) Uani 1 1 d . . . H30E H 1.0843 0.1047 0.2955 0.063 Uiso 1 1 calc R . . C304 C 1.1273(7) -0.1216(6) 0.2094(5) 0.0581(18) Uani 1 1 d . . . H30F H 1.2060 -0.1848 0.1867 0.070 Uiso 1 1 calc R . . C305 C 0.9715(7) -0.1111(5) 0.2118(4) 0.0438(14) Uani 1 1 d . . . H30G H 0.9432 -0.1664 0.1897 0.053 Uiso 1 1 calc R . . C303 C 1.1693(7) -0.0406(7) 0.2399(5) 0.0586(18) Uani 1 1 d . . . H30H H 1.2768 -0.0468 0.2375 0.070 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 Au1 0.02552(10) 0.01714(9) 0.02652(10) -0.00443(6) 0.00051(7) -0.00631(7) P1 0.0274(6) 0.0190(5) 0.0306(6) -0.0059(5) -0.0025(5) -0.0073(5) C1 0.029(2) 0.019(2) 0.020(2) -0.0039(16) 0.0013(17) -0.0111(18) N1 0.027(2) 0.0193(17) 0.0246(19) -0.0030(15) 0.0019(16) -0.0123(15) N2 0.030(2) 0.0207(18) 0.027(2) -0.0021(15) 0.0005(16) -0.0119(16) N3 0.0229(19) 0.0215(18) 0.0228(19) -0.0054(15) -0.0003(15) -0.0091(15) N4 0.032(2) 0.025(2) 0.029(2) -0.0113(17) 0.0006(17) -0.0092(17) N5 0.029(2) 0.0224(18) 0.0219(19) -0.0029(15) -0.0033(16) -0.0096(16) N6 0.046(3) 0.023(2) 0.027(2) 0.0014(16) -0.0056(19) -0.0163(18) C10 0.028(3) 0.024(2) 0.047(3) -0.003(2) 0.000(2) 0.000(2) C11 0.026(2) 0.023(2) 0.032(3) -0.0080(19) 0.0025(19) -0.0089(18) C12 0.024(2) 0.038(3) 0.037(3) -0.009(2) 0.003(2) -0.010(2) C13 0.030(3) 0.031(2) 0.032(3) -0.007(2) 0.006(2) -0.016(2) C14 0.054(4) 0.037(3) 0.050(4) 0.002(3) 0.017(3) -0.022(3) C20 0.031(3) 0.035(3) 0.050(3) -0.015(2) 0.015(2) -0.019(2) C21 0.029(2) 0.0121(19) 0.034(3) -0.0002(18) -0.004(2) -0.0016(17) C22 0.039(3) 0.029(2) 0.033(3) -0.005(2) -0.007(2) -0.018(2) C23 0.044(3) 0.029(2) 0.025(2) -0.010(2) -0.002(2) -0.015(2) C24 0.063(4) 0.059(4) 0.047(4) -0.031(3) 0.002(3) -0.027(3) C30 0.048(3) 0.039(3) 0.033(3) -0.010(2) -0.005(2) -0.023(3) C31 0.033(3) 0.030(2) 0.028(2) -0.0052(19) -0.003(2) -0.014(2) C32 0.055(4) 0.038(3) 0.027(3) -0.004(2) -0.008(2) -0.021(3) C33 0.058(4) 0.034(3) 0.030(3) 0.004(2) -0.010(3) -0.023(3) C34 0.118(7) 0.051(4) 0.044(4) 0.016(3) -0.032(4) -0.051(4) C100 0.036(3) 0.023(2) 0.027(2) -0.0031(19) -0.007(2) -0.011(2) C101 0.042(3) 0.030(3) 0.032(3) -0.002(2) -0.005(2) -0.016(2) C102 0.050(3) 0.044(3) 0.032(3) -0.001(2) 0.000(3) -0.021(3) C103 0.063(4) 0.043(3) 0.030(3) 0.005(2) -0.012(3) -0.028(3) C104 0.063(4) 0.029(3) 0.045(3) 0.008(2) -0.023(3) -0.012(3) C105 0.040(3) 0.032(3) 0.046(3) -0.002(2) -0.009(3) -0.006(2) C200 0.030(2) 0.017(2) 0.034(3) -0.0095(19) -0.003(2) -0.0034(18) C201 0.030(3) 0.027(2) 0.037(3) -0.010(2) 0.003(2) -0.010(2) C202 0.038(3) 0.028(3) 0.044(3) -0.012(2) -0.003(2) -0.014(2) C203 0.055(4) 0.040(3) 0.046(3) -0.018(3) -0.006(3) -0.018(3) C204 0.081(5) 0.054(4) 0.033(3) -0.009(3) 0.002(3) -0.039(4) C205 0.060(4) 0.036(3) 0.041(3) -0.006(2) -0.002(3) -0.031(3) C300 0.028(2) 0.021(2) 0.036(3) -0.0038(19) -0.006(2) -0.0079(18) C301 0.040(3) 0.032(3) 0.045(3) -0.012(2) -0.001(2) -0.015(2) C302 0.051(4) 0.051(4) 0.065(4) -0.013(3) -0.006(3) -0.028(3) C304 0.031(3) 0.056(4) 0.085(5) -0.025(4) 0.004(3) -0.007(3) C305 0.035(3) 0.032(3) 0.065(4) -0.019(3) -0.003(3) -0.006(2) C303 0.030(3) 0.066(4) 0.083(5) -0.014(4) -0.006(3) -0.022(3) #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C1 2.111(4) . ? Au1 P1 2.2740(12) . ? P1 C100 1.808(5) . ? P1 C300 1.812(5) . ? P1 C200 1.818(5) . ? C1 N1 1.453(6) . ? C1 N3 1.466(6) . ? C1 N5 1.490(6) . ? N1 C11 1.359(6) . ? N1 N2 1.369(5) . ? N2 C13 1.321(6) . ? N3 C21 1.364(6) . ? N3 N4 1.364(5) . ? N4 C23 1.326(6) . ? N5 N6 1.351(5) . ? N5 C31 1.356(6) . ? N6 C33 1.328(7) . ? C10 C11 1.493(7) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.365(7) . ? C12 C13 1.400(7) . ? C12 H12A 0.9500 . ? C13 C14 1.496(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C20 C21 1.488(7) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.376(7) . ? C22 C23 1.387(7) . ? C22 H22A 0.9500 . ? C23 C24 1.489(7) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C30 C31 1.484(7) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.377(7) . ? C32 C33 1.399(7) . ? C32 H32A 0.9500 . ? C33 C34 1.501(8) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C100 C105 1.389(7) . ? C100 C101 1.395(7) . ? C101 C102 1.385(7) . ? C101 H10D 0.9500 . ? C102 C103 1.356(8) . ? C102 H10E 0.9500 . ? C103 C104 1.365(9) . ? C103 H10F 0.9500 . ? C104 C105 1.370(8) . ? C104 H10G 0.9500 . ? C105 H10H 0.9500 . ? C200 C201 1.381(7) . ? C200 C205 1.388(7) . ? C201 C202 1.390(7) . ? C201 H20D 0.9500 . ? C202 C203 1.370(8) . ? C202 H20E 0.9500 . ? C203 C204 1.388(8) . ? C203 H20F 0.9500 . ? C204 C205 1.382(8) . ? C204 H20G 0.9500 . ? C205 H20H 0.9500 . ? C300 C305 1.379(7) . ? C300 C301 1.400(7) . ? C301 C302 1.358(8) . ? C301 H30D 0.9500 . ? C302 C303 1.374(10) . ? C302 H30E 0.9500 . ? C304 C305 1.373(8) . ? C304 C303 1.376(9) . ? C304 H30F 0.9500 . ? C305 H30G 0.9500 . ? C303 H30H 0.9500 . ? 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 Au1 P1 175.66(12) . . ? C100 P1 C300 105.2(2) . . ? C100 P1 C200 106.1(2) . . ? C300 P1 C200 104.0(2) . . ? C100 P1 Au1 110.37(16) . . ? C300 P1 Au1 115.02(15) . . ? C200 P1 Au1 115.24(16) . . ? N1 C1 N3 107.6(3) . . ? N1 C1 N5 107.6(4) . . ? N3 C1 N5 107.2(3) . . ? N1 C1 Au1 106.9(3) . . ? N3 C1 Au1 112.7(3) . . ? N5 C1 Au1 114.5(3) . . ? C11 N1 N2 111.3(4) . . ? C11 N1 C1 132.1(4) . . ? N2 N1 C1 116.1(4) . . ? C13 N2 N1 105.4(4) . . ? C21 N3 N4 111.4(4) . . ? C21 N3 C1 129.0(4) . . ? N4 N3 C1 119.7(4) . . ? C23 N4 N3 105.1(4) . . ? N6 N5 C31 112.9(4) . . ? N6 N5 C1 121.3(4) . . ? C31 N5 C1 125.7(4) . . ? C33 N6 N5 104.8(4) . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 106.3(4) . . ? N1 C11 C10 124.8(4) . . ? C12 C11 C10 128.8(5) . . ? C11 C12 C13 106.3(4) . . ? C11 C12 H12A 126.8 . . ? C13 C12 H12A 126.8 . . ? N2 C13 C12 110.7(4) . . ? N2 C13 C14 120.2(5) . . ? C12 C13 C14 129.1(5) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C21 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C21 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 C22 106.0(4) . . ? N3 C21 C20 124.3(4) . . ? C22 C21 C20 129.6(5) . . ? C21 C22 C23 106.0(4) . . ? C21 C22 H22A 127.0 . . ? C23 C22 H22A 127.0 . . ? N4 C23 C22 111.4(4) . . ? N4 C23 C24 119.6(5) . . ? C22 C23 C24 129.0(5) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N5 C31 C32 105.4(4) . . ? N5 C31 C30 124.8(4) . . ? C32 C31 C30 129.7(5) . . ? C31 C32 C33 106.0(5) . . ? C31 C32 H32A 127.0 . . ? C33 C32 H32A 127.0 . . ? N6 C33 C32 111.0(5) . . ? N6 C33 C34 120.3(5) . . ? C32 C33 C34 128.7(5) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C105 C100 C101 118.7(5) . . ? C105 C100 P1 122.4(4) . . ? C101 C100 P1 118.9(4) . . ? C102 C101 C100 119.2(5) . . ? C102 C101 H10D 120.4 . . ? C100 C101 H10D 120.4 . . ? C103 C102 C101 120.9(6) . . ? C103 C102 H10E 119.5 . . ? C101 C102 H10E 119.5 . . ? C102 C103 C104 120.5(5) . . ? C102 C103 H10F 119.8 . . ? C104 C103 H10F 119.8 . . ? C103 C104 C105 120.0(5) . . ? C103 C104 H10G 120.0 . . ? C105 C104 H10G 120.0 . . ? C104 C105 C100 120.8(6) . . ? C104 C105 H10H 119.6 . . ? C100 C105 H10H 119.6 . . ? C201 C200 C205 119.3(5) . . ? C201 C200 P1 122.3(4) . . ? C205 C200 P1 118.4(4) . . ? C200 C201 C202 120.5(5) . . ? C200 C201 H20D 119.7 . . ? C202 C201 H20D 119.7 . . ? C203 C202 C201 119.8(5) . . ? C203 C202 H20E 120.1 . . ? C201 C202 H20E 120.1 . . ? C202 C203 C204 120.1(5) . . ? C202 C203 H20F 119.9 . . ? C204 C203 H20F 119.9 . . ? C205 C204 C203 120.0(6) . . ? C205 C204 H20G 120.0 . . ? C203 C204 H20G 120.0 . . ? C204 C205 C200 120.1(5) . . ? C204 C205 H20H 119.9 . . ? C200 C205 H20H 119.9 . . ? C305 C300 C301 118.3(5) . . ? C305 C300 P1 123.2(4) . . ? C301 C300 P1 118.5(4) . . ? C302 C301 C300 120.6(5) . . ? C302 C301 H30D 119.7 . . ? C300 C301 H30D 119.7 . . ? C301 C302 C303 120.5(6) . . ? C301 C302 H30E 119.7 . . ? C303 C302 H30E 119.7 . . ? C305 C304 C303 119.9(6) . . ? C305 C304 H30F 120.0 . . ? C303 C304 H30F 120.0 . . ? C304 C305 C300 120.9(6) . . ? C304 C305 H30G 119.6 . . ? C300 C305 H30G 119.6 . . ? C302 C303 C304 119.8(6) . . ? C302 C303 H30H 120.1 . . ? C304 C303 H30H 120.1 . . ? 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 N3 C1 N1 C11 74.4(6) . . . . ? N5 C1 N1 C11 -40.9(6) . . . . ? Au1 C1 N1 C11 -164.3(4) . . . . ? N3 C1 N1 N2 -96.3(4) . . . . ? N5 C1 N1 N2 148.4(4) . . . . ? Au1 C1 N1 N2 25.0(4) . . . . ? C11 N1 N2 C13 -0.3(5) . . . . ? C1 N1 N2 C13 172.3(4) . . . . ? N1 C1 N3 C21 165.0(4) . . . . ? N5 C1 N3 C21 -79.6(5) . . . . ? Au1 C1 N3 C21 47.3(5) . . . . ? N1 C1 N3 N4 -16.6(5) . . . . ? N5 C1 N3 N4 98.9(4) . . . . ? Au1 C1 N3 N4 -134.3(3) . . . . ? C21 N3 N4 C23 -2.3(5) . . . . ? C1 N3 N4 C23 179.0(4) . . . . ? N1 C1 N5 N6 121.6(4) . . . . ? N3 C1 N5 N6 6.0(5) . . . . ? Au1 C1 N5 N6 -119.7(4) . . . . ? N1 C1 N5 C31 -61.1(5) . . . . ? N3 C1 N5 C31 -176.6(4) . . . . ? Au1 C1 N5 C31 57.6(5) . . . . ? C31 N5 N6 C33 -0.1(6) . . . . ? C1 N5 N6 C33 177.5(4) . . . . ? N2 N1 C11 C12 -0.6(5) . . . . ? C1 N1 C11 C12 -171.6(5) . . . . ? N2 N1 C11 C10 178.7(5) . . . . ? C1 N1 C11 C10 7.7(8) . . . . ? N1 C11 C12 C13 1.2(6) . . . . ? C10 C11 C12 C13 -178.0(5) . . . . ? N1 N2 C13 C12 1.1(6) . . . . ? N1 N2 C13 C14 179.3(5) . . . . ? C11 C12 C13 N2 -1.5(6) . . . . ? C11 C12 C13 C14 -179.5(6) . . . . ? N4 N3 C21 C22 2.5(5) . . . . ? C1 N3 C21 C22 -178.9(4) . . . . ? N4 N3 C21 C20 -174.7(4) . . . . ? C1 N3 C21 C20 3.9(7) . . . . ? N3 C21 C22 C23 -1.7(5) . . . . ? C20 C21 C22 C23 175.3(5) . . . . ? N3 N4 C23 C22 1.2(5) . . . . ? N3 N4 C23 C24 -178.5(5) . . . . ? C21 C22 C23 N4 0.3(6) . . . . ? C21 C22 C23 C24 179.9(6) . . . . ? N6 N5 C31 C32 -0.2(6) . . . . ? C1 N5 C31 C32 -177.7(4) . . . . ? N6 N5 C31 C30 -176.6(5) . . . . ? C1 N5 C31 C30 5.8(8) . . . . ? N5 C31 C32 C33 0.4(6) . . . . ? C30 C31 C32 C33 176.6(6) . . . . ? N5 N6 C33 C32 0.4(6) . . . . ? N5 N6 C33 C34 179.7(6) . . . . ? C31 C32 C33 N6 -0.5(7) . . . . ? C31 C32 C33 C34 -179.8(7) . . . . ? C300 P1 C100 C105 -38.0(5) . . . . ? C200 P1 C100 C105 71.8(5) . . . . ? Au1 P1 C100 C105 -162.7(4) . . . . ? C300 P1 C100 C101 141.2(4) . . . . ? C200 P1 C100 C101 -108.9(4) . . . . ? Au1 P1 C100 C101 16.6(4) . . . . ? C105 C100 C101 C102 -0.3(8) . . . . ? P1 C100 C101 C102 -179.6(4) . . . . ? C100 C101 C102 C103 0.1(9) . . . . ? C101 C102 C103 C104 -0.2(9) . . . . ? C102 C103 C104 C105 0.4(9) . . . . ? C103 C104 C105 C100 -0.6(9) . . . . ? C101 C100 C105 C104 0.5(8) . . . . ? P1 C100 C105 C104 179.8(5) . . . . ? C100 P1 C200 C201 12.1(5) . . . . ? C300 P1 C200 C201 122.8(4) . . . . ? Au1 P1 C200 C201 -110.4(4) . . . . ? C100 P1 C200 C205 -168.8(4) . . . . ? C300 P1 C200 C205 -58.1(5) . . . . ? Au1 P1 C200 C205 68.7(5) . . . . ? C205 C200 C201 C202 -0.7(8) . . . . ? P1 C200 C201 C202 178.4(4) . . . . ? C200 C201 C202 C203 1.5(8) . . . . ? C201 C202 C203 C204 -1.0(9) . . . . ? C202 C203 C204 C205 -0.3(10) . . . . ? C203 C204 C205 C200 1.0(10) . . . . ? C201 C200 C205 C204 -0.5(9) . . . . ? P1 C200 C205 C204 -179.7(5) . . . . ? C100 P1 C300 C305 89.9(5) . . . . ? C200 P1 C300 C305 -21.4(5) . . . . ? Au1 P1 C300 C305 -148.4(4) . . . . ? C100 P1 C300 C301 -88.5(4) . . . . ? C200 P1 C300 C301 160.2(4) . . . . ? Au1 P1 C300 C301 33.2(5) . . . . ? C305 C300 C301 C302 -0.2(8) . . . . ? P1 C300 C301 C302 178.3(5) . . . . ? C300 C301 C302 C303 0.2(10) . . . . ? C303 C304 C305 C300 -1.1(11) . . . . ? C301 C300 C305 C304 0.6(9) . . . . ? P1 C300 C305 C304 -177.8(5) . . . . ? C301 C302 C303 C304 -0.7(11) . . . . ? C305 C304 C303 C302 1.1(12) . . . . ?