# Copyright The Royal Society of Chemistry, 1999 # CCDC Number 186/1291 data_global # 1. SUBMISSION DETAILS _publ_contact_author 'Prof. Dr. W. Kaim' _publ_contact_author_address ; Institute of Inorganic Chemistry University of Stuttgart Pfaffenwaldring 55 Germany ; _publ_contact_author_phone '049 711 685-4170' _publ_contact_author_fax '049 685-4165' _publ_contact_author_email 'kaim@iac.uni-stuttgart.de' _publ_requested_journal 'Dalton Transactions' _publ_requested_coeditor_name ; Axel Klein, Thorsten Sixt, Thomas Scheiring, Volker Kasack, Stanislav Zalis, Jan Fiedler' ; _publ_contact_letter ? #=================================================== # 2. TITLE AND AUTHOR LIST loop_ _publ_author_name _publ_author_adress 'Kaim, Wolfgang' ; Institute of Inorganic Chemistry University of Stuttgart Pfaffenwaldring 55 D-70550 Stuttgart Germany ; 'Klein, Axel' ; Institute of Inorganic Chemistry University of Stuttgart Pfaffenwaldring 55 D-70550 Stuttgart Germany ; 'Sixt, Thorsten' ; Institute of Inorganic Chemistry University of Stuttgart Pfaffenwaldring 55 D-70550 Stuttgart Germany ; 'Scheiring, Thomas' ; Institute of Inorganic Chemistry University of Stuttgart Pfaffenwaldring 55 D-70550 Stuttgart Germany ; 'Kasack, Volker' ; Institute of Inorganic Chemistry University of Stuttgart Pfaffenwaldring 55 D-70550 Stuttgart Germany ; 'Zalis, Stanilav' ; J. Heyrovsky Institute of Physical Chemistry Academy of Science of the Czech Republic Dolejskova 3 CZ-18223 Prague Czech Republic ; 'Fiedler, Jan' ; J. Heyrovsky Institute of Physical Chemistry Academy of Science of the Czech Republic Dolejskova 3 CZ-18223 Prague Czech Republic ; data_bip2 _audit_creation_method SHELXL _chemical_name_systematic '2,5-Bis(1-phenyliminoethyl)pyrazine' _chemical_name_common '2,5-Bis(1-phenylimonoethyl)pyrazine' _chemical_formula_moiety 'C20 H18 N4' _chemical_formula_structural 'C20 H18 N4' _chemical_formula_analytical 'C20 H18 N4' _chemical_formula_sum 'C20 H18 N4' _chemical_formula_weight 314.38 _chemical_melting_point ? _chemical_compound_source ? 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 6.3013(4) _cell_length_b 7.8308(7) _cell_length_c 33.242(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1640.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needles _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_method ? _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ; _diffrn_ambient_temperature 183(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 'Siemens-P4' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2370 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 29.99 _reflns_number_total 2370 _reflns_number_observed 1680 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens Diffractometer Software' _computing_cell_refinement 'Siemens Diffractometer Software' _computing_data_reduction 'SHELXLTL-Plus X-DisK' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-94 (Sheldrick, 1994)' _computing_molecular_graphics 'SHELXLTL-Plus XP' _computing_publication_material 'SHELXL-94' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 115 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+0.2949P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0109(25) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2255 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_obs 0.0480 _refine_ls_wR_factor_all 0.1449 _refine_ls_wR_factor_obs 0.1201 _refine_ls_goodness_of_fit_all 1.046 _refine_ls_goodness_of_fit_obs 1.110 _refine_ls_restrained_S_all 1.116 _refine_ls_restrained_S_obs 1.110 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group C1 C -0.1164(2) 0.1549(2) 0.33368(4) 0.0315(3) Uani 1 d . . C2 C -0.1281(2) 0.2142(2) 0.29437(4) 0.0332(3) Uani 1 d . . H2 H -0.2236(31) 0.1548(25) 0.2747(5) 0.045(5) Uiso 1 d . . C3 C -0.0100(2) 0.3538(2) 0.28216(4) 0.0332(3) Uani 1 d . . H3 H -0.0153(26) 0.3976(20) 0.2549(5) 0.027(4) Uiso 1 d . . C4 C 0.1228(2) 0.4343(2) 0.30948(4) 0.0342(3) Uani 1 d . . H4 H 0.2087(30) 0.5369(24) 0.3014(5) 0.042(5) Uiso 1 d . . C5 C 0.1390(2) 0.3748(2) 0.34878(4) 0.0318(3) Uani 1 d . . H5 H 0.2287(30) 0.4314(24) 0.3687(5) 0.039(5) Uiso 1 d . . C6 C 0.0170(2) 0.2364(2) 0.36118(4) 0.0277(3) Uani 1 d . . C7 C -0.1059(2) 0.1484(2) 0.42495(4) 0.0287(3) Uani 1 d . . C8 C -0.0499(2) 0.0728(2) 0.46464(4) 0.0297(3) Uani 1 d . . C9 C -0.1580(3) -0.0321(2) 0.52501(4) 0.0393(4) Uani 1 d . . H9 H -0.2668(39) -0.0529(30) 0.5447(7) 0.064(6) Uiso 1 d . . C71 C -0.3365(2) 0.1840(2) 0.41735(5) 0.0360(3) Uani 1 d . . H71C H -0.3595(29) 0.2638(26) 0.3951(6) 0.047(5) Uiso 1 d . . H71B H -0.4057(31) 0.2286(26) 0.4422(5) 0.049(5) Uiso 1 d . . H71A H -0.4068(36) 0.0760(29) 0.4110(6) 0.058(6) Uiso 1 d . . N1 N 0.0489(2) 0.1748(2) 0.40087(3) 0.0307(3) Uani 1 d . . N2 N -0.2089(2) 0.0406(2) 0.49011(4) 0.0391(3) Uani 1 d . . H1 H -0.1927(27) 0.0557(24) 0.3418(5) 0.032(4) Uiso 1 d . . 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 C1 0.0339(7) 0.0299(7) 0.0307(6) -0.0002(5) 0.0029(5) -0.0040(6) C2 0.0338(7) 0.0368(8) 0.0289(6) -0.0035(5) -0.0018(6) 0.0024(6) C3 0.0346(7) 0.0376(7) 0.0272(6) 0.0034(6) 0.0032(5) 0.0046(6) C4 0.0337(7) 0.0361(7) 0.0328(7) 0.0051(5) 0.0051(6) -0.0033(6) C5 0.0299(7) 0.0366(7) 0.0288(6) 0.0000(5) 0.0024(5) -0.0049(6) C6 0.0274(6) 0.0314(7) 0.0244(6) 0.0005(5) 0.0043(5) 0.0012(5) C7 0.0333(7) 0.0263(6) 0.0265(6) -0.0031(5) 0.0045(5) -0.0034(5) C8 0.0338(7) 0.0301(7) 0.0252(6) -0.0031(5) 0.0073(5) -0.0062(6) C9 0.0327(7) 0.0548(10) 0.0303(7) 0.0071(6) 0.0102(6) -0.0037(7) C71 0.0323(7) 0.0412(8) 0.0345(7) -0.0015(6) 0.0070(6) 0.0011(6) N1 0.0326(6) 0.0342(6) 0.0253(5) 0.0014(4) 0.0032(5) -0.0037(5) N2 0.0333(7) 0.0541(8) 0.0299(6) 0.0062(5) 0.0085(5) -0.0026(6) _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 C1 C2 1.389(2) . ? C1 C6 1.396(2) . ? C2 C3 1.383(2) . ? C3 C4 1.387(2) . ? C4 C5 1.391(2) . ? C5 C6 1.391(2) . ? C6 N1 1.419(2) . ? C7 N1 1.279(2) . ? C7 C8 1.489(2) . ? C7 C71 1.501(2) . ? C8 N2 1.336(2) . ? C8 C9 1.392(2) 5_556 ? C9 N2 1.331(2) . ? C9 C8 1.392(2) 5_556 ? 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 C2 C1 C6 119.67(13) . . ? C3 C2 C1 120.79(14) . . ? C2 C3 C4 119.45(13) . . ? C3 C4 C5 120.46(14) . . ? C4 C5 C6 119.95(14) . . ? C5 C6 C1 119.65(12) . . ? C5 C6 N1 117.54(12) . . ? C1 C6 N1 122.57(13) . . ? N1 C7 C8 116.00(13) . . ? N1 C7 C71 127.10(13) . . ? C8 C7 C71 116.90(12) . . ? N2 C8 C9 120.40(13) . 5_556 ? N2 C8 C7 117.33(13) . . ? C9 C8 C7 122.25(12) 5_556 . ? N2 C9 C8 122.69(13) . 5_556 ? C7 N1 C6 121.94(12) . . ? C9 N2 C8 116.90(13) . . ? 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 C6 C1 C2 C3 -0.3(2) . . . . ? C1 C2 C3 C4 0.5(2) . . . . ? C2 C3 C4 C5 0.5(2) . . . . ? C3 C4 C5 C6 -1.8(2) . . . . ? C4 C5 C6 C1 1.9(2) . . . . ? C4 C5 C6 N1 176.41(13) . . . . ? C2 C1 C6 C5 -0.9(2) . . . . ? C2 C1 C6 N1 -175.07(13) . . . . ? N1 C7 C8 N2 -178.68(13) . . . . ? C71 C7 C8 N2 0.9(2) . . . . ? N1 C7 C8 C9 -0.4(2) . . . 5_556 ? C71 C7 C8 C9 179.14(14) . . . 5_556 ? C8 C7 N1 C6 176.09(12) . . . . ? C71 C7 N1 C6 -3.4(2) . . . . ? C5 C6 N1 C7 130.49(15) . . . . ? C1 C6 N1 C7 -55.2(2) . . . . ? C8 C9 N2 C8 0.5(3) 5_556 . . . ? C9 C8 N2 C9 -0.5(3) 5_556 . . . ? C7 C8 N2 C9 177.86(14) . . . . ? _refine_diff_density_max 0.248 _refine_diff_density_min -0.221 _refine_diff_density_rms 0.044 #===END data_ak1a _audit_creation_method SHELXL _chemical_name_systematic ; (-2,5-Bis(1-phenyliminoethyl)pyrazine)-di-(bis-triphenylphosphinocopper(I)) tetrafluoroborate ; _chemical_name_common ; (-2,5-Bis(1-phenyliminoethyl)pyrazine)-di-(bis-triphenylphosphinocopper(I)) tetrafluoroborate ; _chemical_formula_moiety 'C92 H78 B2 Cu2 F8 N4 P4' _chemical_formula_structural 'C92 H78 B2 Cu2 F8 N4 P4' _chemical_formula_analytical 'C92 H78 B2 Cu2 F8 N4 P4' _chemical_formula_sum 'C92 H78 B2 Cu2 F8 N4 P4' _chemical_formula_weight 1664.16 _chemical_melting_point ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 '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 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 13.844(3) _cell_length_b 11.111(3) _cell_length_c 26.604(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.03(2) _cell_angle_gamma 90.00 _cell_volume 3952.2(17) _symmetry_space_group_name_H-M P2(1)/n _cell_formula_units_Z 2 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description fraction _exptl_crystal_colour violett-black _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.398 _cell_measurement_temperature 183(2) _exptl_crystal_density_method ? _exptl_crystal_F_000 1716 _exptl_absorpt_coefficient_mu 0.689 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ? _diffrn_ambient_temperature 183(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 98 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7271 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0610 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 3 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6974 _reflns_number_observed 4882 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-94 (Sheldrick, 1994)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 406 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0654P)^2^+8.7620P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6568 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1025 _refine_ls_R_factor_obs 0.0622 _refine_ls_wR_factor_all 0.1844 _refine_ls_wR_factor_obs 0.1516 _refine_ls_goodness_of_fit_all 1.126 _refine_ls_goodness_of_fit_obs 1.210 _refine_ls_restrained_S_all 1.217 _refine_ls_restrained_S_obs 1.210 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_mean 0.000 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.86240(4) 0.60524(5) 0.08302(2) 0.0225(2) Uani 1 d . . P1 P 0.78229(10) 0.77527(12) 0.04782(5) 0.0234(3) Uani 1 d . . P2 P 0.91664(9) 0.61696(12) 0.17121(5) 0.0225(3) Uani 1 d . . N1 N 0.8055(3) 0.4324(4) 0.06087(15) 0.0226(9) Uani 1 d . . N2 N 0.9551(3) 0.5461(4) 0.03755(15) 0.0226(9) Uani 1 d . . C6 C 0.7266(4) 0.3744(5) 0.0786(2) 0.0288(12) Uani 1 d . . C5 C 0.7501(5) 0.3126(6) 0.1258(2) 0.0414(14) Uani 1 d . . H5A H 0.8184(5) 0.3065(6) 0.1458(2) 0.080 Uiso 1 d R . C4 C 0.6728(5) 0.2590(6) 0.1433(3) 0.051(2) Uani 1 d . . H4A H 0.6884(5) 0.2172(6) 0.1760(3) 0.080 Uiso 1 d R . C3 C 0.5746(5) 0.2669(7) 0.1139(3) 0.056(2) Uani 1 d . . H3A H 0.5222(5) 0.2287(7) 0.1256(3) 0.080 Uiso 1 d R . C2 C 0.5526(5) 0.3294(7) 0.0668(3) 0.061(2) Uani 1 d . . H2A H 0.4844(5) 0.3375(7) 0.0468(3) 0.080 Uiso 1 d R . C1 C 0.6286(5) 0.3813(7) 0.0491(3) 0.051(2) Uani 1 d . . H1A H 0.6137(5) 0.4226(7) 0.0163(3) 0.080 Uiso 1 d R . C71 C 0.8290(4) 0.2416(5) 0.0168(2) 0.0315(12) Uani 1 d . . H71A H 0.7761(4) 0.2113(5) 0.0305(2) 0.080 Uiso 1 d R . H71B H 0.8095(4) 0.2361(5) -0.0205(2) 0.080 Uiso 1 d R . H71C H 0.8884(4) 0.1948(5) 0.0302(2) 0.080 Uiso 1 d R . C7 C 0.8494(4) 0.3708(4) 0.0326(2) 0.0214(10) Uani 1 d . . C8 C 0.9298(3) 0.4376(4) 0.0153(2) 0.0211(10) Uani 1 d . . C9 C 1.0261(4) 0.6075(4) 0.0218(2) 0.0240(10) Uani 1 d . . H9 H 1.0459(4) 0.6825(4) 0.0364(2) 0.029 Uiso 1 calc R . C11 C 0.7533(4) 0.7980(5) -0.0228(2) 0.0245(11) Uani 1 d . . C12 C 0.7468(4) 0.6970(5) -0.0545(2) 0.0348(13) Uani 1 d . . H12A H 0.7599(4) 0.6184(5) -0.0392(2) 0.080 Uiso 1 d R . C13 C 0.7208(5) 0.7108(6) -0.1090(2) 0.0402(14) Uani 1 d . . H13A H 0.7148(5) 0.6415(6) -0.1311(2) 0.080 Uiso 1 d R . C14 C 0.7038(4) 0.8247(6) -0.1304(2) 0.0394(14) Uani 1 d . . H14A H 0.6868(4) 0.8338(6) -0.1675(2) 0.080 Uiso 1 d R . C15 C 0.7116(4) 0.9251(5) -0.0994(2) 0.0341(13) Uani 1 d . . H15A H 0.7001(4) 1.0037(5) -0.1148(2) 0.080 Uiso 1 d R . C16 C 0.7354(4) 0.9115(5) -0.0452(2) 0.0298(12) Uani 1 d . . H16A H 0.7397(4) 0.9811(5) -0.0234(2) 0.080 Uiso 1 d R . C21 C 0.8635(4) 0.9035(5) 0.0729(2) 0.0273(11) Uani 1 d . . C22 C 0.8553(5) 0.9757(5) 0.1144(2) 0.0366(13) Uani 1 d . . H22A H 0.7982(5) 0.9675(5) 0.1284(2) 0.080 Uiso 1 d R . C23 C 0.9298(6) 1.0589(5) 0.1357(2) 0.049(2) Uani 1 d . . H23A H 0.9247(6) 1.1076(5) 0.1647(2) 0.080 Uiso 1 d R . C24 C 1.0123(5) 1.0712(6) 0.1149(3) 0.051(2) Uani 1 d . . H24A H 1.0635(5) 1.1290(6) 0.1295(3) 0.080 Uiso 1 d R . C25 C 1.0202(4) 1.0018(6) 0.0742(2) 0.046(2) Uani 1 d . . H25A H 1.0771(4) 1.0107(6) 0.0602(2) 0.080 Uiso 1 d R . C26 C 0.9466(4) 0.9185(5) 0.0527(2) 0.0331(13) Uani 1 d . . H26A H 0.9525(4) 0.8701(5) 0.0237(2) 0.080 Uiso 1 d R . C31 C 0.6610(4) 0.8028(5) 0.0614(2) 0.0279(12) Uani 1 d . . C32 C 0.6156(4) 0.9156(6) 0.0568(2) 0.0407(14) Uani 1 d . . H32A H 0.6502(4) 0.9849(6) 0.0488(2) 0.080 Uiso 1 d R . C33 C 0.5198(5) 0.9263(6) 0.0642(3) 0.049(2) Uani 1 d . . H33A H 0.4871(5) 1.0033(6) 0.0604(3) 0.080 Uiso 1 d R . C34 C 0.4711(4) 0.8262(7) 0.0764(2) 0.047(2) Uani 1 d . . H34A H 0.4052(4) 0.8348(7) 0.0814(2) 0.080 Uiso 1 d R . C35 C 0.5161(4) 0.7148(7) 0.0819(2) 0.045(2) Uani 1 d . . H35A H 0.4822(4) 0.6457(7) 0.0907(2) 0.080 Uiso 1 d R . C36 C 0.6124(4) 0.7038(5) 0.0742(2) 0.0367(13) Uani 1 d . . H36A H 0.6448(4) 0.6268(5) 0.0778(2) 0.080 Uiso 1 d R . C41 C 0.9900(4) 0.4907(4) 0.2043(2) 0.0242(11) Uani 1 d . . C42 C 1.0403(4) 0.4181(5) 0.1764(2) 0.0339(13) Uani 1 d . . H42A H 1.0318(4) 0.4324(5) 0.1399(2) 0.080 Uiso 1 d R . C43 C 1.1029(4) 0.3263(5) 0.2012(2) 0.0422(15) Uani 1 d . . H43A H 1.1376(4) 0.2775(5) 0.1818(2) 0.080 Uiso 1 d R . C44 C 1.1157(4) 0.3047(5) 0.2535(2) 0.0414(15) Uani 1 d . . H44A H 1.1581(4) 0.2401(5) 0.2703(2) 0.080 Uiso 1 d R . C45 C 1.0670(4) 0.3759(5) 0.2817(2) 0.0392(14) Uani 1 d . . H45A H 1.0760(4) 0.3605(5) 0.3181(2) 0.080 Uiso 1 d R . C46 C 1.0052(4) 0.4696(5) 0.2580(2) 0.0339(13) Uani 1 d . . H46A H 0.9727(4) 0.5198(5) 0.2780(2) 0.080 Uiso 1 d R . C51 C 0.8082(4) 0.6282(4) 0.1984(2) 0.0251(11) Uani 1 d . . C52 C 0.7683(4) 0.5305(6) 0.2175(2) 0.0412(14) Uani 1 d . . H52A H 0.8033(4) 0.4551(6) 0.2214(2) 0.080 Uiso 1 d R . C53 C 0.6780(5) 0.5398(6) 0.2316(3) 0.057(2) Uani 1 d . . H53A H 0.6511(5) 0.4706(6) 0.2449(3) 0.080 Uiso 1 d R . C54 C 0.6280(5) 0.6473(6) 0.2264(2) 0.045(2) Uani 1 d . . H54A H 0.5652(5) 0.6533(6) 0.2352(2) 0.080 Uiso 1 d R . C55 C 0.6681(4) 0.7457(6) 0.2086(2) 0.0386(14) Uani 1 d . . H55A H 0.6335(4) 0.8214(6) 0.2055(2) 0.080 Uiso 1 d R . C56 C 0.7577(4) 0.7384(5) 0.1949(2) 0.0323(12) Uani 1 d . . H56A H 0.7853(4) 0.8086(5) 0.1829(2) 0.080 Uiso 1 d R . C61 C 0.9969(4) 0.7439(4) 0.1999(2) 0.0229(10) Uani 1 d . . C62 C 0.9926(4) 0.7978(5) 0.2467(2) 0.0310(12) Uani 1 d . . H62A H 0.9437(4) 0.7713(5) 0.2641(2) 0.080 Uiso 1 d R . C63 C 1.0593(4) 0.8890(5) 0.2682(2) 0.0382(14) Uani 1 d . . H63A H 1.0540(4) 0.9285(5) 0.2995(2) 0.080 Uiso 1 d R . C64 C 1.1325(4) 0.9238(5) 0.2447(2) 0.0411(14) Uani 1 d . . H64A H 1.1797(4) 0.9849(5) 0.2604(2) 0.080 Uiso 1 d R . C65 C 1.1383(4) 0.8689(5) 0.1981(2) 0.0389(14) Uani 1 d . . H65A H 1.1886(4) 0.8930(5) 0.1812(2) 0.080 Uiso 1 d R . C66 C 1.0690(4) 0.7788(5) 0.1761(2) 0.0332(13) Uani 1 d . . H66A H 1.0721(4) 0.7407(5) 0.1441(2) 0.080 Uiso 1 d R . B1 B 0.7287(5) 0.3718(6) -0.1140(3) 0.0340(15) Uani 1 d . . F1 F 0.8108(3) 0.4320(4) -0.1211(2) 0.0735(13) Uani 1 d . . F2 F 0.7503(3) 0.2477(3) -0.11039(13) 0.0485(9) Uani 1 d . . F3 F 0.6461(3) 0.3915(4) -0.15411(14) 0.0633(11) Uani 1 d . . F4 F 0.7102(3) 0.4099(3) -0.06798(13) 0.0485(9) Uani 1 d . . 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 0.0246(3) 0.0244(3) 0.0191(3) -0.0016(3) 0.0067(2) 0.0024(3) P1 0.0230(7) 0.0252(7) 0.0221(6) 0.0006(5) 0.0063(5) 0.0018(5) P2 0.0248(7) 0.0245(7) 0.0186(6) -0.0016(5) 0.0063(5) 0.0013(6) N1 0.023(2) 0.026(2) 0.020(2) -0.004(2) 0.007(2) -0.002(2) N2 0.024(2) 0.025(2) 0.019(2) -0.001(2) 0.006(2) 0.001(2) C6 0.028(3) 0.032(3) 0.030(3) -0.004(2) 0.014(2) -0.008(2) C5 0.042(3) 0.050(4) 0.032(3) 0.004(3) 0.008(3) -0.004(3) C4 0.056(4) 0.052(4) 0.051(4) 0.008(3) 0.026(3) -0.009(3) C3 0.048(4) 0.075(5) 0.053(4) 0.000(4) 0.027(3) -0.017(4) C2 0.034(4) 0.084(6) 0.064(5) 0.000(4) 0.010(3) -0.024(4) C1 0.035(3) 0.077(5) 0.041(3) 0.010(3) 0.010(3) -0.007(3) C71 0.039(3) 0.027(3) 0.031(3) -0.002(2) 0.013(2) 0.000(2) C7 0.026(3) 0.021(3) 0.017(2) 0.000(2) 0.005(2) -0.001(2) C8 0.021(2) 0.023(2) 0.018(2) 0.002(2) 0.002(2) 0.000(2) C9 0.027(3) 0.019(2) 0.027(3) -0.001(2) 0.007(2) 0.000(2) C11 0.019(2) 0.028(3) 0.025(3) -0.004(2) 0.003(2) 0.000(2) C12 0.041(3) 0.028(3) 0.032(3) -0.003(2) 0.003(2) 0.004(3) C13 0.050(4) 0.044(4) 0.023(3) -0.011(3) 0.004(3) 0.002(3) C14 0.040(3) 0.054(4) 0.023(3) 0.006(3) 0.006(2) 0.009(3) C15 0.033(3) 0.037(3) 0.033(3) 0.011(2) 0.010(2) 0.008(2) C16 0.025(3) 0.035(3) 0.029(3) 0.003(2) 0.005(2) 0.001(2) C21 0.030(3) 0.025(3) 0.024(3) 0.005(2) 0.000(2) 0.004(2) C22 0.051(4) 0.027(3) 0.028(3) 0.003(2) 0.004(3) 0.002(3) C23 0.074(5) 0.031(3) 0.029(3) -0.005(3) -0.009(3) 0.000(3) C24 0.049(4) 0.045(4) 0.049(4) 0.001(3) -0.007(3) -0.015(3) C25 0.032(3) 0.052(4) 0.050(4) 0.010(3) 0.001(3) -0.008(3) C26 0.025(3) 0.033(3) 0.037(3) 0.002(2) 0.001(2) -0.001(2) C31 0.026(3) 0.038(3) 0.021(2) 0.001(2) 0.009(2) 0.005(2) C32 0.041(3) 0.043(4) 0.042(3) 0.008(3) 0.018(3) 0.011(3) C33 0.036(3) 0.058(4) 0.056(4) 0.010(3) 0.015(3) 0.017(3) C34 0.025(3) 0.079(5) 0.037(3) -0.002(3) 0.008(3) 0.010(3) C35 0.032(3) 0.067(5) 0.039(3) -0.012(3) 0.014(3) -0.011(3) C36 0.036(3) 0.041(3) 0.033(3) 0.001(3) 0.009(2) 0.001(3) C41 0.023(3) 0.023(3) 0.027(3) 0.002(2) 0.007(2) 0.000(2) C42 0.032(3) 0.037(3) 0.031(3) -0.003(2) 0.004(2) 0.008(2) C43 0.037(3) 0.035(3) 0.050(4) -0.007(3) 0.003(3) 0.008(3) C44 0.031(3) 0.034(3) 0.053(4) 0.008(3) -0.002(3) 0.002(3) C45 0.029(3) 0.045(4) 0.038(3) 0.014(3) -0.002(2) -0.008(3) C46 0.031(3) 0.041(3) 0.027(3) 0.007(2) 0.005(2) 0.002(3) C51 0.030(3) 0.025(3) 0.021(2) -0.002(2) 0.008(2) 0.004(2) C52 0.039(3) 0.035(3) 0.053(4) 0.005(3) 0.019(3) 0.003(3) C53 0.042(4) 0.049(4) 0.087(5) 0.016(4) 0.031(4) -0.006(3) C54 0.033(3) 0.059(4) 0.046(4) -0.001(3) 0.017(3) 0.004(3) C55 0.036(3) 0.041(3) 0.037(3) -0.004(3) 0.008(3) 0.011(3) C56 0.032(3) 0.039(3) 0.026(3) -0.001(2) 0.008(2) -0.004(3) C61 0.022(2) 0.024(3) 0.020(2) 0.001(2) 0.001(2) 0.004(2) C62 0.033(3) 0.033(3) 0.027(3) -0.005(2) 0.007(2) 0.003(2) C63 0.036(3) 0.037(3) 0.035(3) -0.012(3) -0.002(2) 0.008(3) C64 0.031(3) 0.041(3) 0.047(4) 0.004(3) 0.002(3) -0.005(3) C65 0.031(3) 0.043(4) 0.041(3) 0.002(3) 0.006(3) -0.001(3) C66 0.032(3) 0.037(3) 0.028(3) 0.001(2) 0.004(2) 0.002(2) B1 0.031(3) 0.039(4) 0.034(3) 0.000(3) 0.012(3) -0.002(3) F1 0.055(3) 0.057(3) 0.121(4) 0.000(3) 0.045(3) -0.005(2) F2 0.071(2) 0.034(2) 0.042(2) 0.000(2) 0.018(2) 0.011(2) F3 0.067(3) 0.072(3) 0.039(2) -0.001(2) -0.009(2) 0.016(2) F4 0.061(2) 0.045(2) 0.036(2) -0.007(2) 0.006(2) 0.007(2) _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 2.085(4) . ? Cu1 N1 2.101(4) . ? Cu1 P1 2.2666(15) . ? Cu1 P2 2.2741(14) . ? P1 C21 1.831(5) . ? P1 C31 1.832(5) . ? P1 C11 1.833(5) . ? P2 C41 1.820(5) . ? P2 C51 1.832(5) . ? P2 C61 1.835(5) . ? N1 C7 1.281(6) . ? N1 C6 1.448(6) . ? N2 C8 1.348(6) . ? N2 C9 1.349(6) . ? C6 C1 1.383(8) . ? C6 C5 1.393(8) . ? C5 C4 1.405(8) . ? C4 C3 1.386(9) . ? C3 C2 1.394(10) . ? C2 C1 1.385(9) . ? C71 C7 1.502(7) . ? C7 C8 1.506(7) . ? C8 C9 1.384(7) 3_765 ? C9 C8 1.384(7) 3_765 ? C11 C16 1.390(7) . ? C11 C12 1.394(7) . ? C12 C13 1.407(8) . ? C13 C14 1.383(8) . ? C14 C15 1.375(8) . ? C15 C16 1.400(7) . ? C21 C22 1.394(7) . ? C21 C26 1.400(7) . ? C22 C23 1.391(8) . ? C23 C24 1.399(10) . ? C24 C25 1.355(9) . ? C25 C26 1.387(8) . ? C31 C36 1.377(8) . ? C31 C32 1.393(8) . ? C32 C33 1.397(8) . ? C33 C34 1.381(9) . ? C34 C35 1.377(9) . ? C35 C36 1.406(8) . ? C41 C42 1.400(7) . ? C41 C46 1.408(7) . ? C42 C43 1.388(8) . ? C43 C44 1.378(9) . ? C44 C45 1.381(9) . ? C45 C46 1.390(8) . ? C51 C52 1.374(8) . ? C51 C56 1.401(7) . ? C52 C53 1.399(8) . ? C53 C54 1.370(9) . ? C54 C55 1.366(9) . ? C55 C56 1.382(8) . ? C61 C66 1.371(7) . ? C61 C62 1.396(7) . ? C62 C63 1.391(8) . ? C63 C64 1.375(8) . ? C64 C65 1.404(8) . ? C65 C66 1.404(8) . ? B1 F3 1.365(7) . ? B1 F1 1.373(7) . ? B1 F4 1.380(7) . ? B1 F2 1.409(8) . ? 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 N1 78.0(2) . . ? N2 Cu1 P1 109.39(12) . . ? N1 Cu1 P1 122.56(12) . . ? N2 Cu1 P2 121.89(11) . . ? N1 Cu1 P2 109.95(11) . . ? P1 Cu1 P2 111.95(5) . . ? C21 P1 C31 107.8(2) . . ? C21 P1 C11 102.5(2) . . ? C31 P1 C11 102.2(2) . . ? C21 P1 Cu1 108.0(2) . . ? C31 P1 Cu1 115.6(2) . . ? C11 P1 Cu1 119.5(2) . . ? C41 P2 C51 105.8(2) . . ? C41 P2 C61 100.9(2) . . ? C51 P2 C61 104.6(2) . . ? C41 P2 Cu1 116.7(2) . . ? C51 P2 Cu1 109.1(2) . . ? C61 P2 Cu1 118.4(2) . . ? C7 N1 C6 117.7(4) . . ? C7 N1 Cu1 116.9(3) . . ? C6 N1 Cu1 125.1(3) . . ? C8 N2 C9 116.3(4) . . ? C8 N2 Cu1 114.0(3) . . ? C9 N2 Cu1 128.9(3) . . ? C1 C6 C5 120.2(5) . . ? C1 C6 N1 120.2(5) . . ? C5 C6 N1 119.6(5) . . ? C6 C5 C4 119.3(6) . . ? C3 C4 C5 120.3(6) . . ? C4 C3 C2 119.6(6) . . ? C1 C2 C3 120.3(6) . . ? C6 C1 C2 120.3(6) . . ? N1 C7 C71 126.3(5) . . ? N1 C7 C8 114.6(4) . . ? C71 C7 C8 119.1(4) . . ? N2 C8 C9 121.6(4) . 3_765 ? N2 C8 C7 115.8(4) . . ? C9 C8 C7 122.5(4) 3_765 . ? N2 C9 C8 122.0(5) . 3_765 ? C16 C11 C12 119.6(5) . . ? C16 C11 P1 122.2(4) . . ? C12 C11 P1 118.2(4) . . ? C11 C12 C13 119.7(5) . . ? C14 C13 C12 119.6(5) . . ? C15 C14 C13 121.2(5) . . ? C14 C15 C16 119.3(5) . . ? C11 C16 C15 120.6(5) . . ? C22 C21 C26 118.7(5) . . ? C22 C21 P1 124.6(4) . . ? C26 C21 P1 116.1(4) . . ? C23 C22 C21 119.9(6) . . ? C22 C23 C24 120.0(6) . . ? C25 C24 C23 120.2(6) . . ? C24 C25 C26 120.5(6) . . ? C25 C26 C21 120.6(6) . . ? C36 C31 C32 120.1(5) . . ? C36 C31 P1 116.6(4) . . ? C32 C31 P1 123.2(4) . . ? C31 C32 C33 119.2(6) . . ? C34 C33 C32 120.2(6) . . ? C35 C34 C33 121.0(6) . . ? C34 C35 C36 118.8(6) . . ? C31 C36 C35 120.7(6) . . ? C42 C41 C46 118.6(5) . . ? C42 C41 P2 118.6(4) . . ? C46 C41 P2 122.5(4) . . ? C43 C42 C41 120.4(5) . . ? C44 C43 C42 120.6(6) . . ? C43 C44 C45 119.7(5) . . ? C44 C45 C46 120.8(5) . . ? C45 C46 C41 119.8(5) . . ? C52 C51 C56 118.2(5) . . ? C52 C51 P2 122.8(4) . . ? C56 C51 P2 118.7(4) . . ? C51 C52 C53 121.0(6) . . ? C54 C53 C52 120.0(6) . . ? C55 C54 C53 119.5(6) . . ? C54 C55 C56 121.2(6) . . ? C55 C56 C51 120.1(5) . . ? C66 C61 C62 119.8(5) . . ? C66 C61 P2 117.3(4) . . ? C62 C61 P2 122.7(4) . . ? C63 C62 C61 120.1(5) . . ? C64 C63 C62 120.5(5) . . ? C63 C64 C65 119.8(6) . . ? C64 C65 C66 119.2(5) . . ? C61 C66 C65 120.6(5) . . ? F3 B1 F1 111.7(5) . . ? F3 B1 F4 109.5(5) . . ? F1 B1 F4 108.8(5) . . ? F3 B1 F2 109.3(5) . . ? F1 B1 F2 108.5(5) . . ? F4 B1 F2 109.0(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 N2 Cu1 P1 C21 -86.3(2) . . . . ? N1 Cu1 P1 C21 -174.1(2) . . . . ? P2 Cu1 P1 C21 51.9(2) . . . . ? N2 Cu1 P1 C31 152.9(2) . . . . ? N1 Cu1 P1 C31 65.0(2) . . . . ? P2 Cu1 P1 C31 -68.9(2) . . . . ? N2 Cu1 P1 C11 30.2(2) . . . . ? N1 Cu1 P1 C11 -57.7(2) . . . . ? P2 Cu1 P1 C11 168.4(2) . . . . ? N2 Cu1 P2 C41 -43.6(2) . . . . ? N1 Cu1 P2 C41 44.4(2) . . . . ? P1 Cu1 P2 C41 -175.8(2) . . . . ? N2 Cu1 P2 C51 -163.4(2) . . . . ? N1 Cu1 P2 C51 -75.4(2) . . . . ? P1 Cu1 P2 C51 64.4(2) . . . . ? N2 Cu1 P2 C61 77.3(2) . . . . ? N1 Cu1 P2 C61 165.3(2) . . . . ? P1 Cu1 P2 C61 -55.0(2) . . . . ? N2 Cu1 N1 C7 1.2(3) . . . . ? P1 Cu1 N1 C7 106.7(3) . . . . ? P2 Cu1 N1 C7 -118.6(3) . . . . ? N2 Cu1 N1 C6 175.7(4) . . . . ? P1 Cu1 N1 C6 -78.9(4) . . . . ? P2 Cu1 N1 C6 55.8(4) . . . . ? N1 Cu1 N2 C8 4.0(3) . . . . ? P1 Cu1 N2 C8 -116.5(3) . . . . ? P2 Cu1 N2 C8 110.2(3) . . . . ? N1 Cu1 N2 C9 173.7(4) . . . . ? P1 Cu1 N2 C9 53.1(4) . . . . ? P2 Cu1 N2 C9 -80.2(4) . . . . ? C7 N1 C6 C1 -90.7(7) . . . . ? Cu1 N1 C6 C1 94.9(6) . . . . ? C7 N1 C6 C5 90.0(6) . . . . ? Cu1 N1 C6 C5 -84.4(6) . . . . ? C1 C6 C5 C4 -0.8(9) . . . . ? N1 C6 C5 C4 178.5(5) . . . . ? C6 C5 C4 C3 0.4(10) . . . . ? C5 C4 C3 C2 -0.6(11) . . . . ? C4 C3 C2 C1 1.3(12) . . . . ? C5 C6 C1 C2 1.5(10) . . . . ? N1 C6 C1 C2 -177.8(6) . . . . ? C3 C2 C1 C6 -1.8(12) . . . . ? C6 N1 C7 C71 -1.6(7) . . . . ? Cu1 N1 C7 C71 173.3(4) . . . . ? C6 N1 C7 C8 179.5(4) . . . . ? Cu1 N1 C7 C8 -5.6(5) . . . . ? C9 N2 C8 C9 -0.4(7) . . . 3_765 ? Cu1 N2 C8 C9 170.6(4) . . . 3_765 ? C9 N2 C8 C7 -179.1(4) . . . . ? Cu1 N2 C8 C7 -8.1(5) . . . . ? N1 C7 C8 N2 9.2(6) . . . . ? C71 C7 C8 N2 -169.8(4) . . . . ? N1 C7 C8 C9 -169.5(4) . . . 3_765 ? C71 C7 C8 C9 11.5(7) . . . 3_765 ? C8 N2 C9 C8 0.4(7) . . . 3_765 ? Cu1 N2 C9 C8 -169.0(3) . . . 3_765 ? C21 P1 C11 C16 -39.1(5) . . . . ? C31 P1 C11 C16 72.5(5) . . . . ? Cu1 P1 C11 C16 -158.5(4) . . . . ? C21 P1 C11 C12 142.5(4) . . . . ? C31 P1 C11 C12 -105.9(4) . . . . ? Cu1 P1 C11 C12 23.2(5) . . . . ? C16 C11 C12 C13 -0.8(8) . . . . ? P1 C11 C12 C13 177.6(4) . . . . ? C11 C12 C13 C14 1.1(9) . . . . ? C12 C13 C14 C15 -0.1(9) . . . . ? C13 C14 C15 C16 -1.2(9) . . . . ? C12 C11 C16 C15 -0.5(8) . . . . ? P1 C11 C16 C15 -178.8(4) . . . . ? C14 C15 C16 C11 1.5(8) . . . . ? C31 P1 C21 C22 27.7(5) . . . . ? C11 P1 C21 C22 135.1(5) . . . . ? Cu1 P1 C21 C22 -97.9(4) . . . . ? C31 P1 C21 C26 -160.8(4) . . . . ? C11 P1 C21 C26 -53.5(4) . . . . ? Cu1 P1 C21 C26 73.6(4) . . . . ? C26 C21 C22 C23 -1.3(8) . . . . ? P1 C21 C22 C23 170.0(4) . . . . ? C21 C22 C23 C24 0.8(9) . . . . ? C22 C23 C24 C25 -0.3(10) . . . . ? C23 C24 C25 C26 0.2(10) . . . . ? C24 C25 C26 C21 -0.7(9) . . . . ? C22 C21 C26 C25 1.2(8) . . . . ? P1 C21 C26 C25 -170.8(4) . . . . ? C21 P1 C31 C36 -144.0(4) . . . . ? C11 P1 C31 C36 108.5(4) . . . . ? Cu1 P1 C31 C36 -23.0(5) . . . . ? C21 P1 C31 C32 39.4(5) . . . . ? C11 P1 C31 C32 -68.2(5) . . . . ? Cu1 P1 C31 C32 160.4(4) . . . . ? C36 C31 C32 C33 -1.2(9) . . . . ? P1 C31 C32 C33 175.3(5) . . . . ? C31 C32 C33 C34 0.3(10) . . . . ? C32 C33 C34 C35 0.8(10) . . . . ? C33 C34 C35 C36 -1.1(9) . . . . ? C32 C31 C36 C35 0.9(8) . . . . ? P1 C31 C36 C35 -175.8(4) . . . . ? C34 C35 C36 C31 0.2(9) . . . . ? C51 P2 C41 C42 144.9(4) . . . . ? C61 P2 C41 C42 -106.4(4) . . . . ? Cu1 P2 C41 C42 23.4(5) . . . . ? C51 P2 C41 C46 -40.8(5) . . . . ? C61 P2 C41 C46 68.0(5) . . . . ? Cu1 P2 C41 C46 -162.3(4) . . . . ? C46 C41 C42 C43 0.8(8) . . . . ? P2 C41 C42 C43 175.3(4) . . . . ? C41 C42 C43 C44 0.5(9) . . . . ? C42 C43 C44 C45 -0.8(9) . . . . ? C43 C44 C45 C46 -0.2(9) . . . . ? C44 C45 C46 C41 1.5(8) . . . . ? C42 C41 C46 C45 -1.8(8) . . . . ? P2 C41 C46 C45 -176.1(4) . . . . ? C41 P2 C51 C52 -28.9(5) . . . . ? C61 P2 C51 C52 -135.0(5) . . . . ? Cu1 P2 C51 C52 97.4(5) . . . . ? C41 P2 C51 C56 157.7(4) . . . . ? C61 P2 C51 C56 51.6(4) . . . . ? Cu1 P2 C51 C56 -76.0(4) . . . . ? C56 C51 C52 C53 1.8(9) . . . . ? P2 C51 C52 C53 -171.5(5) . . . . ? C51 C52 C53 C54 0.2(11) . . . . ? C52 C53 C54 C55 -1.6(11) . . . . ? C53 C54 C55 C56 1.0(10) . . . . ? C54 C55 C56 C51 1.0(9) . . . . ? C52 C51 C56 C55 -2.4(8) . . . . ? P2 C51 C56 C55 171.3(4) . . . . ? C41 P2 C61 C66 88.2(4) . . . . ? C51 P2 C61 C66 -162.0(4) . . . . ? Cu1 P2 C61 C66 -40.4(4) . . . . ? C41 P2 C61 C62 -86.1(4) . . . . ? C51 P2 C61 C62 23.6(5) . . . . ? Cu1 P2 C61 C62 145.3(4) . . . . ? C66 C61 C62 C63 1.9(8) . . . . ? P2 C61 C62 C63 176.1(4) . . . . ? C61 C62 C63 C64 -2.5(8) . . . . ? C62 C63 C64 C65 1.6(9) . . . . ? C63 C64 C65 C66 -0.2(9) . . . . ? C62 C61 C66 C65 -0.5(8) . . . . ? P2 C61 C66 C65 -175.0(4) . . . . ? C64 C65 C66 C61 -0.4(8) . . . . ? _refine_diff_density_max 0.880 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.095