# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1720 data_GLOBAL # 1. SUBMISSION DETAILS _publ_contact_author_name 'Hofmann, Peter' _publ_contact_author_address ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg Germany ; _publ_contact_author_phone '049 6221 54- 8502' _publ_contact_author_fax '049 6221 54-4885' _publ_contact_author_email 'ph@phindigo.oci.uni-heidelberg.de' _publ_requested_journal 'Chem. Comm.' _publ_requested_coeditor_name ? _publ_contact_letter ; paper 'in submission' for publication in Chem. Comm. ; # 3. TITLE AND AUTHOR LIST _publ_section_title ; A neutral dicopper(III) bis(\m-oxo) complex from a copper(I) ethylene iminophsphanamide and O~2~ ; loop_ _publ_author_name _publ_author_address 'Straub, Bernd F.' ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Rominger, Frank' ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Hofmann, Peter' ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; #======================================================================= data_bs20 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H72 Cu2 N4 O2 P2 Si4' _chemical_formula_weight 798.28 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' 'Si' 'Si' 0.0817 0.0704 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 28.4009(7) _cell_length_b 11.2930(3) _cell_length_c 16.9370(5) _cell_angle_alpha 90.00 _cell_angle_beta 126.6040(10) _cell_angle_gamma 90.00 _cell_volume 4360.9(2) _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 needle _exptl_crystal_colour brown _exptl_crystal_size_max .36 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.216 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 1.186 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min .73 _exptl_absorpt_correction_T_max .88 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _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 'CCD area detector' _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 21976 _diffrn_reflns_av_R_equivalents 0.0629 _diffrn_reflns_av_sigmaI/netI 0.0572 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.46 _reflns_number_total 4991 _reflns_number_gt 2992 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0571P)^2^+19.9415P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4991 _refine_ls_number_parameters 203 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1108 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1638 _refine_ls_wR_factor_gt 0.1403 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.056 _refine_ls_shift/su_mean 0.002 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 -0.05007(2) 0.01805(5) 0.14689(4) 0.04129(19) Uani 1 1 d . . . P1 P -0.14131(5) 0.01966(11) -0.03323(8) 0.0385(3) Uani 1 1 d . . . Si1 Si -0.10963(7) -0.23792(13) 0.06554(12) 0.0560(4) Uani 1 1 d . . . Si2 Si -0.08147(8) 0.27460(14) 0.04303(13) 0.0631(5) Uani 1 1 d . . . O1 O 0.0000 -0.0856(4) 0.2500 0.0519(13) Uani 1 2 d S . . O2 O 0.0000 0.1215(4) 0.2500 0.0696(17) Uani 1 2 d S . . N1 N -0.10904(17) -0.0896(3) 0.0415(3) 0.0457(10) Uani 1 1 d . . . N2 N -0.09896(17) 0.1268(3) 0.0341(3) 0.0463(10) Uani 1 1 d . . . C1 C -0.1121(3) -0.2595(6) 0.1711(5) 0.087(2) Uani 1 1 d . . . H1A H -0.0809 -0.2129 0.2272 0.131 Uiso 1 1 calc R . . H1B H -0.1065 -0.3435 0.1890 0.131 Uiso 1 1 calc R . . H1C H -0.1503 -0.2334 0.1532 0.131 Uiso 1 1 calc R . . C2 C -0.1769(3) -0.3234(6) -0.0340(5) 0.097(2) Uani 1 1 d . . . H2A H -0.2119 -0.2880 -0.0453 0.146 Uiso 1 1 calc R . . H2B H -0.1734 -0.4060 -0.0134 0.146 Uiso 1 1 calc R . . H2C H -0.1802 -0.3204 -0.0950 0.146 Uiso 1 1 calc R . . C3 C -0.0469(3) -0.3126(5) 0.0808(6) 0.093(2) Uani 1 1 d . . . H6A H -0.0146 -0.2560 0.1063 0.139 Uiso 1 1 calc R . . H6B H -0.0588 -0.3429 0.0170 0.139 Uiso 1 1 calc R . . H6C H -0.0338 -0.3786 0.1271 0.139 Uiso 1 1 calc R . . C4 C -0.1019(4) 0.3534(5) 0.1159(5) 0.089(2) Uani 1 1 d . . . H4A H -0.1446 0.3513 0.0799 0.133 Uiso 1 1 calc R . . H4B H -0.0887 0.4359 0.1262 0.133 Uiso 1 1 calc R . . H4C H -0.0830 0.3143 0.1797 0.133 Uiso 1 1 calc R . . C5 C -0.0029(3) 0.2917(7) 0.0965(6) 0.108(3) Uani 1 1 d . . . H5A H 0.0207 0.2403 0.1542 0.162 Uiso 1 1 calc R . . H5B H 0.0089 0.3743 0.1162 0.162 Uiso 1 1 calc R . . H5C H 0.0034 0.2696 0.0475 0.162 Uiso 1 1 calc R . . C6 C -0.1203(4) 0.3544(6) -0.0783(5) 0.101(3) Uani 1 1 d . . . H3A H -0.1071 0.3226 -0.1160 0.151 Uiso 1 1 calc R . . H3B H -0.1112 0.4391 -0.0666 0.151 Uiso 1 1 calc R . . H3C H -0.1627 0.3429 -0.1155 0.151 Uiso 1 1 calc R . . C11 C -0.2160(2) 0.0457(5) -0.0670(4) 0.0540(13) Uani 1 1 d . . . C12 C -0.2617(3) -0.0431(6) -0.1411(5) 0.084(2) Uani 1 1 d . . . H12A H -0.2986 -0.0299 -0.1497 0.126 Uiso 1 1 calc R . . H12B H -0.2478 -0.1237 -0.1169 0.126 Uiso 1 1 calc R . . H12C H -0.2681 -0.0327 -0.2043 0.126 Uiso 1 1 calc R . . C13 C -0.2093(3) 0.0345(6) 0.0303(5) 0.083(2) Uani 1 1 d . . . H13A H -0.2469 0.0517 0.0181 0.124 Uiso 1 1 calc R . . H13B H -0.1797 0.0909 0.0785 0.124 Uiso 1 1 calc R . . H13C H -0.1970 -0.0462 0.0560 0.124 Uiso 1 1 calc R . . C14 C -0.2380(2) 0.1713(5) -0.1058(5) 0.0681(17) Uani 1 1 d . . . H14A H -0.2418 0.1827 -0.1667 0.102 Uiso 1 1 calc R . . H14B H -0.2100 0.2290 -0.0566 0.102 Uiso 1 1 calc R . . H14C H -0.2763 0.1828 -0.1189 0.102 Uiso 1 1 calc R . . C15 C -0.1427(2) -0.0029(4) -0.1432(3) 0.0484(12) Uani 1 1 d . . . C16 C -0.1604(3) -0.1305(5) -0.1823(4) 0.0732(18) Uani 1 1 d . . . H16A H -0.2006 -0.1453 -0.2044 0.110 Uiso 1 1 calc R . . H16B H -0.1337 -0.1863 -0.1297 0.110 Uiso 1 1 calc R . . H16C H -0.1583 -0.1410 -0.2375 0.110 Uiso 1 1 calc R . . C17 C -0.1831(3) 0.0842(6) -0.2274(4) 0.081(2) Uani 1 1 d . . . H17A H -0.1783 0.0739 -0.2798 0.122 Uiso 1 1 calc R . . H17B H -0.1727 0.1656 -0.2025 0.122 Uiso 1 1 calc R . . H17C H -0.2240 0.0688 -0.2537 0.122 Uiso 1 1 calc R . . C18 C -0.0794(3) 0.0142(6) -0.1090(5) 0.0713(17) Uani 1 1 d . . . H18A H -0.0526 -0.0327 -0.0495 0.107 Uiso 1 1 calc R . . H18B H -0.0687 0.0981 -0.0947 0.107 Uiso 1 1 calc R . . H18C H -0.0763 -0.0118 -0.1610 0.107 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 0.0406(3) 0.0372(3) 0.0314(3) -0.0011(2) 0.0135(2) 0.0030(3) P1 0.0408(6) 0.0391(6) 0.0292(5) 0.0011(5) 0.0174(5) 0.0001(5) Si1 0.0685(10) 0.0430(8) 0.0590(9) 0.0120(7) 0.0394(8) 0.0122(7) Si2 0.0772(11) 0.0423(8) 0.0718(11) -0.0135(7) 0.0456(10) -0.0091(8) O1 0.064(3) 0.026(2) 0.040(3) 0.000 0.017(2) 0.000 O2 0.073(4) 0.029(3) 0.051(3) 0.000 0.007(3) 0.000 N1 0.049(2) 0.041(2) 0.034(2) -0.0015(16) 0.0182(19) 0.0007(18) N2 0.050(2) 0.038(2) 0.041(2) 0.0000(17) 0.021(2) -0.0005(18) C1 0.109(6) 0.074(5) 0.077(5) 0.012(4) 0.054(4) 0.000(4) C2 0.097(5) 0.061(4) 0.103(6) 0.007(4) 0.042(5) -0.020(4) C3 0.093(5) 0.038(3) 0.164(7) 0.001(4) 0.086(5) 0.010(3) C4 0.142(7) 0.049(4) 0.090(5) -0.008(3) 0.077(5) 0.010(4) C5 0.120(6) 0.080(5) 0.125(7) -0.028(5) 0.073(6) -0.041(5) C6 0.161(8) 0.056(4) 0.102(6) 0.005(4) 0.087(6) -0.014(4) C11 0.047(3) 0.054(3) 0.056(3) 0.015(2) 0.028(3) 0.008(2) C12 0.048(3) 0.070(4) 0.109(5) 0.004(4) 0.033(4) -0.004(3) C13 0.108(5) 0.085(5) 0.103(5) 0.039(4) 0.089(5) 0.038(4) C14 0.057(3) 0.069(4) 0.078(4) 0.025(3) 0.040(3) 0.023(3) C15 0.062(3) 0.050(3) 0.037(2) -0.003(2) 0.031(2) -0.005(2) C16 0.102(5) 0.066(4) 0.052(3) -0.022(3) 0.046(4) -0.019(3) C17 0.114(5) 0.085(5) 0.043(3) 0.010(3) 0.046(4) 0.008(4) C18 0.083(4) 0.071(4) 0.086(4) -0.012(3) 0.064(4) -0.011(3) _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 O2 1.864(3) . ? Cu1 O1 1.865(3) . ? Cu1 N1 1.976(4) . ? Cu1 N2 1.980(4) . ? Cu1 P1 2.5679(12) . ? Cu1 Cu1 2.9055(10) 2 ? P1 N2 1.605(4) . ? P1 N1 1.607(4) . ? P1 C15 1.857(5) . ? P1 C11 1.862(5) . ? Si1 N1 1.726(4) . ? Si1 C3 1.846(6) . ? Si1 C1 1.848(7) . ? Si1 C2 1.893(7) . ? Si2 N2 1.723(4) . ? Si2 C5 1.852(8) . ? Si2 C4 1.872(6) . ? Si2 C6 1.884(7) . ? O1 Cu1 1.865(3) 2 ? O1 O2 2.338(6) . ? O2 Cu1 1.864(3) 2 ? C11 C12 1.524(8) . ? C11 C14 1.532(7) . ? C11 C13 1.547(8) . ? C15 C18 1.538(8) . ? C15 C16 1.539(7) . ? C15 C17 1.539(7) . ? 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 O2 Cu1 O1 77.64(15) . . ? O2 Cu1 N1 173.78(13) . . ? O1 Cu1 N1 102.83(15) . . ? O2 Cu1 N2 102.69(16) . . ? O1 Cu1 N2 175.31(13) . . ? N1 Cu1 N2 77.35(16) . . ? O2 Cu1 P1 140.74(12) . . ? O1 Cu1 P1 141.50(11) . . ? N1 Cu1 P1 38.73(11) . . ? N2 Cu1 P1 38.67(11) . . ? O2 Cu1 Cu1 38.80(11) . 2 ? O1 Cu1 Cu1 38.85(10) . 2 ? N1 Cu1 Cu1 141.33(11) . 2 ? N2 Cu1 Cu1 141.29(11) . 2 ? P1 Cu1 Cu1 177.67(5) . 2 ? N2 P1 N1 100.7(2) . . ? N2 P1 C15 112.0(2) . . ? N1 P1 C15 110.2(2) . . ? N2 P1 C11 109.5(2) . . ? N1 P1 C11 111.9(2) . . ? C15 P1 C11 112.0(2) . . ? N2 P1 Cu1 50.45(14) . . ? N1 P1 Cu1 50.30(14) . . ? C15 P1 Cu1 126.41(17) . . ? C11 P1 Cu1 121.56(18) . . ? N1 Si1 C3 109.4(3) . . ? N1 Si1 C1 111.6(3) . . ? C3 Si1 C1 113.3(4) . . ? N1 Si1 C2 115.5(3) . . ? C3 Si1 C2 105.6(4) . . ? C1 Si1 C2 101.2(3) . . ? N2 Si2 C5 110.2(3) . . ? N2 Si2 C4 109.4(3) . . ? C5 Si2 C4 112.6(4) . . ? N2 Si2 C6 114.7(3) . . ? C5 Si2 C6 103.5(4) . . ? C4 Si2 C6 106.4(3) . . ? Cu1 O1 Cu1 102.3(2) . 2 ? Cu1 O1 O2 51.15(10) . . ? Cu1 O1 O2 51.15(10) 2 . ? Cu1 O2 Cu1 102.4(2) . 2 ? Cu1 O2 O1 51.20(11) . . ? Cu1 O2 O1 51.20(11) 2 . ? P1 N1 Si1 148.2(3) . . ? P1 N1 Cu1 90.97(18) . . ? Si1 N1 Cu1 120.4(2) . . ? P1 N2 Si2 148.0(3) . . ? P1 N2 Cu1 90.89(18) . . ? Si2 N2 Cu1 121.1(2) . . ? C12 C11 C14 109.1(5) . . ? C12 C11 C13 109.1(5) . . ? C14 C11 C13 107.0(5) . . ? C12 C11 P1 113.8(4) . . ? C14 C11 P1 112.1(4) . . ? C13 C11 P1 105.4(4) . . ? C18 C15 C16 106.9(5) . . ? C18 C15 C17 109.1(5) . . ? C16 C15 C17 109.2(4) . . ? C18 C15 P1 106.5(4) . . ? C16 C15 P1 111.4(4) . . ? C17 C15 P1 113.6(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.924 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.080 #=======================================================================