# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1169 data_global # 1. SUBMISSION DETAILS _publ_contact_author ; Taillefer, Marc Ecole Nationale Superieure de Chimie de Montpellier 8 rue de l'Ecole Normale 34296 Montpellier Bundesrepublik Deutschland ; _publ_contact_author_email 'taillefe@cit.enscm.fr' _publ_contact_author_fax '033 467144319' _publ_contact_author_phone '033 467144352' _publ_requested_journal 'Angewandte Chemie' _publ_requested_coeditor_name ? _publ_contact_letter ; ; # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_ ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis of the sodium diphenyl-bis(cyanamido)phosphonium diylide by a new ariation of the Staudinger reaction ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Taillefer, Marc' ; Ecole Nationale Superieure de Chimie de Montpellier 8 rue de l'Ecole Normale 34296 Montpellier Frankreich ; 'Inguimbert, Nicolas' ; Ecole Nationale Superieure de Chimie de Montpellier 8 rue de l'Ecole Normale 34296 Montpellier Frankreich ; 'J\"ager, Lothar' ; Institut f\"ur Anorganische Chemie der Universit\"at Martin-Luther-Universit\"at Halle-Wittenberg Kurt-Mothes-Str. 2 06120 Halle/Saale Bundesrepublik Deutschland ; 'Merzweiler, Kurt' ; Institut f\"ur Anorganische Chemie der Universit\"at Martin-Luther-Universit\"at Halle-Wittenberg Kurt-Mothes-Str. 2 06120 Halle/Saale Bundesrepublik Deutschland ; 'Cristau, Henri-Jean' ; Ecole Nationale Superieure de Chimie de Montpellier 8 rue de l'Ecole Normale 34296 Montpellier Frankreich ; # 4. TEXT _publ_section_abstract ; ; _publ_section_comment ; ? ; _publ_section_experimental ; ? ; _publ_section_references ; ; data_ipds3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38 H30 Cu N10 P2' _chemical_formula_weight 752.20 _chemical_melting_point '192 C' _chemical_compound_source turqoise 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4325(14) _cell_length_b 13.5423(12) _cell_length_c 16.555(2) _cell_angle_alpha 107.588(8) _cell_angle_beta 91.823(11) _cell_angle_gamma 98.651(11) _cell_volume 1775.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_method ? _exptl_crystal_F_000 774 _exptl_absorpt_coefficient_mu 0.749 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10554 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6478 _reflns_number_observed 4688 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 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^)+(0.0787P)^2^+0.0554P] 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 6478 _refine_ls_number_parameters 580 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_obs 0.0479 _refine_ls_wR_factor_all 0.1330 _refine_ls_wR_factor_obs 0.1186 _refine_ls_goodness_of_fit_all 1.037 _refine_ls_goodness_of_fit_obs 1.106 _refine_ls_restrained_S_all 1.037 _refine_ls_restrained_S_obs 1.106 _refine_ls_shift/esd_max -0.009 _refine_ls_shift/esd_mean 0.001 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 -0.2882(5) 0.1288(3) 1.2589(2) 0.0602(10) Uani 1 d . . C2 C 0.0980(4) 0.1321(3) 1.1263(2) 0.0501(8) Uani 1 d . . C3 C 0.3528(4) 0.2915(3) 0.8430(2) 0.0463(8) Uani 1 d . . C4 C 0.6292(4) 0.5325(3) 0.8270(2) 0.0470(8) Uani 1 d . . C5 C 0.0821(4) 0.2119(3) 1.3364(2) 0.0493(8) Uani 1 d . . C6 C 0.0051(6) 0.2514(3) 1.4092(3) 0.0645(10) Uani 1 d . . H1 H -0.0924(52) 0.2093(33) 1.4165(25) 0.067(12) Uiso 1 d . . C7 C 0.0739(7) 0.3438(4) 1.4711(3) 0.0788(13) Uani 1 d . . H2 H 0.0205(65) 0.3613(42) 1.5183(35) 0.106(18) Uiso 1 d . . C8 C 0.2180(7) 0.3975(4) 1.4613(3) 0.0816(14) Uani 1 d . . H3 H 0.2751(54) 0.4556(37) 1.5070(28) 0.079(13) Uiso 1 d . . C9 C 0.2959(6) 0.3598(4) 1.3892(3) 0.0786(13) Uani 1 d . . H4 H 0.4004(62) 0.3999(40) 1.3887(30) 0.094(16) Uiso 1 d . . C10 C 0.2300(5) 0.2675(3) 1.3273(3) 0.0624(10) Uani 1 d . . H5 H 0.2906(56) 0.2372(36) 1.2789(29) 0.087(14) Uiso 1 d . . C11 C 0.0682(5) -0.0091(3) 1.3023(2) 0.0501(8) Uani 1 d . . C12 C -0.0138(5) -0.0416(3) 1.3631(3) 0.0605(10) Uani 1 d . . H6 H -0.1218(47) -0.0073(30) 1.3862(24) 0.064(11) Uiso 1 d . . C13 C 0.0495(6) -0.1068(4) 1.4014(3) 0.0688(12) Uani 1 d . . H7 H -0.0003(55) -0.1259(37) 1.4357(29) 0.079(15) Uiso 1 d . . C14 C 0.1889(6) -0.1422(3) 1.3771(3) 0.0698(12) Uani 1 d . . H8 H 0.2241(58) -0.1885(39) 1.4050(29) 0.093(15) Uiso 1 d . . C15 C 0.2704(6) -0.1112(4) 1.3162(3) 0.0744(12) Uani 1 d . . H9 H 0.3751(56) -0.1395(37) 1.3001(28) 0.087(14) Uiso 1 d . . C16 C 0.2107(6) -0.0444(3) 1.2793(3) 0.0661(11) Uani 1 d . . H10 H 0.2644(46) -0.0231(30) 1.2359(25) 0.063(11) Uiso 1 d . . C17 C -0.0310(5) 0.3870(3) 1.0587(3) 0.0582(9) Uani 1 d . . H11 H 0.0141(55) 0.4008(35) 1.1046(28) 0.074(14) Uiso 1 d . . C18 C -0.1661(5) 0.4295(4) 1.0520(3) 0.0693(11) Uani 1 d . . H12 H -0.1997(63) 0.4803(42) 1.1037(34) 0.111(18) Uiso 1 d . . C19 C -0.2566(5) 0.3968(4) 0.9757(3) 0.0695(11) Uani 1 d . . H13 H -0.3395(54) 0.4323(35) 0.9657(27) 0.078(13) Uiso 1 d . . C20 C -0.2063(5) 0.3231(4) 0.9087(3) 0.0692(11) Uani 1 d . . H14 H -0.2617(54) 0.3060(35) 0.8581(28) 0.079(13) Uiso 1 d . . C21 C -0.0682(5) 0.2854(3) 0.9203(2) 0.0574(9) Uani 1 d . . H15 H -0.0303(43) 0.2399(29) 0.8714(24) 0.056(10) Uiso 1 d . . C22 C 0.4329(5) 0.1051(3) 0.9301(2) 0.0555(9) Uani 1 d . . H16 H 0.3464(46) 0.0941(29) 0.8828(24) 0.059(11) Uiso 1 d . . C23 C 0.5647(5) 0.0563(3) 0.9185(3) 0.0649(11) Uani 1 d . . H17 H 0.5708(49) 0.0033(34) 0.8665(27) 0.073(12) Uiso 1 d . . C24 C 0.6888(5) 0.0883(3) 0.9816(3) 0.0669(12) Uani 1 d . . H18 H 0.7881(58) 0.0560(37) 0.9727(29) 0.097(16) Uiso 1 d . . C25 C 0.6745(5) 0.1656(4) 1.0542(3) 0.0634(10) Uani 1 d . . H19 H 0.7446(54) 0.1868(35) 1.0969(28) 0.072(14) Uiso 1 d . . C26 C 0.5370(5) 0.2097(3) 1.0631(2) 0.0533(8) Uani 1 d . . H20 H 0.5256(42) 0.2638(29) 1.1125(23) 0.052(10) Uiso 1 d . . C27 C 0.2755(4) 0.4296(2) 0.7219(2) 0.0385(7) Uani 1 d . . C28 C 0.1223(4) 0.3736(3) 0.7225(2) 0.0468(8) Uani 1 d . . H21 H 0.1125(38) 0.3065(27) 0.7270(20) 0.040(9) Uiso 1 d . . C29 C -0.0133(4) 0.4173(3) 0.7174(2) 0.0585(9) Uani 1 d . . H22 H -0.1154(54) 0.3726(35) 0.7167(27) 0.078(13) Uiso 1 d . . C30 C 0.0008(5) 0.5164(4) 0.7121(2) 0.0636(11) Uani 1 d . . H23 H -0.0874(49) 0.5517(32) 0.7105(24) 0.069(12) Uiso 1 d . . C31 C 0.1509(6) 0.5744(4) 0.7116(3) 0.0672(11) Uani 1 d . . H24 H 0.1684(54) 0.6398(38) 0.7066(28) 0.082(14) Uiso 1 d . . C32 C 0.2878(5) 0.5306(3) 0.7169(2) 0.0526(8) Uani 1 d . . H25 H 0.3856(44) 0.5704(28) 0.7180(21) 0.049(10) Uiso 1 d . . C33 C 0.4798(4) 0.2952(3) 0.6185(2) 0.0391(7) Uani 1 d . . C34 C 0.3949(5) 0.1956(3) 0.5846(2) 0.0596(10) Uani 1 d . . H26 H 0.3355(54) 0.1636(35) 0.6176(27) 0.080(14) Uiso 1 d . . C35 C 0.4098(6) 0.1373(4) 0.5012(3) 0.0785(14) Uani 1 d . . H27 H 0.3456(67) 0.0705(46) 0.4768(34) 0.114(18) Uiso 1 d . . C36 C 0.5082(6) 0.1803(4) 0.4524(3) 0.0760(13) Uani 1 d . . H28 H 0.5156(55) 0.1393(38) 0.3960(30) 0.088(14) Uiso 1 d . . C37 C 0.5926(5) 0.2796(4) 0.4855(2) 0.0648(11) Uani 1 d . . H29 H 0.6740(54) 0.3148(35) 0.4485(28) 0.086(14) Uiso 1 d . . C38 C 0.5799(4) 0.3383(3) 0.5687(2) 0.0500(8) Uani 1 d . . H30 H 0.6368(50) 0.4089(35) 0.5910(25) 0.073(13) Uiso 1 d . . N1 N -0.1939(4) 0.0630(3) 1.2609(2) 0.0712(9) Uani 1 d . . N2 N -0.3839(5) 0.1826(4) 1.2574(2) 0.0862(12) Uani 1 d . . N3 N 0.0776(5) 0.0710(3) 1.1728(2) 0.0733(10) Uani 1 d . . N4 N 0.1222(4) 0.1783(3) 1.0797(2) 0.0620(8) Uani 1 d . . N5 N 0.4203(4) 0.2845(2) 0.7737(2) 0.0551(8) Uani 1 d . . N6 N 0.2932(4) 0.2900(3) 0.9041(2) 0.0622(8) Uani 1 d . . N7 N 0.6069(3) 0.4585(2) 0.7549(2) 0.0538(7) Uani 1 d . . N8 N 0.6590(4) 0.6005(3) 0.8893(2) 0.0621(8) Uani 1 d . . N9 N 0.4181(3) 0.1830(2) 1.0020(2) 0.0459(6) Uani 1 d . . N10 N 0.0208(3) 0.3167(2) 0.9947(2) 0.0433(6) Uani 1 d . . P1 P -0.00163(12) 0.08652(8) 1.26143(6) 0.0501(2) Uani 1 d . . P2 P 0.45055(9) 0.37006(7) 0.72480(5) 0.0374(2) Uani 1 d . . Cu Cu 0.22761(5) 0.26020(3) 1.00891(2) 0.04088(14) 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 C1 0.056(2) 0.079(3) 0.045(2) 0.021(2) 0.002(2) 0.006(2) C2 0.053(2) 0.061(2) 0.044(2) 0.024(2) 0.0130(15) 0.016(2) C3 0.045(2) 0.060(2) 0.041(2) 0.0212(15) 0.0058(14) 0.019(2) C4 0.033(2) 0.052(2) 0.052(2) 0.010(2) -0.0022(14) 0.0076(14) C5 0.053(2) 0.055(2) 0.049(2) 0.025(2) 0.0077(15) 0.018(2) C6 0.075(3) 0.062(3) 0.056(2) 0.015(2) 0.013(2) 0.016(2) C7 0.106(4) 0.076(3) 0.054(3) 0.017(2) 0.010(3) 0.021(3) C8 0.108(4) 0.061(3) 0.071(3) 0.019(2) -0.021(3) 0.008(3) C9 0.069(3) 0.074(3) 0.094(4) 0.037(3) -0.012(3) -0.002(2) C10 0.061(2) 0.063(3) 0.070(3) 0.029(2) 0.009(2) 0.013(2) C11 0.062(2) 0.047(2) 0.044(2) 0.0173(15) 0.0068(15) 0.011(2) C12 0.062(2) 0.062(2) 0.067(2) 0.037(2) 0.011(2) 0.005(2) C13 0.076(3) 0.063(3) 0.073(3) 0.038(2) 0.000(2) -0.002(2) C14 0.091(3) 0.043(2) 0.075(3) 0.019(2) -0.014(2) 0.011(2) C15 0.089(3) 0.067(3) 0.071(3) 0.014(2) 0.009(2) 0.039(3) C16 0.083(3) 0.075(3) 0.052(2) 0.025(2) 0.023(2) 0.032(2) C17 0.053(2) 0.071(3) 0.046(2) 0.010(2) 0.006(2) 0.015(2) C18 0.057(2) 0.076(3) 0.073(3) 0.015(2) 0.011(2) 0.022(2) C19 0.058(3) 0.081(3) 0.082(3) 0.039(2) 0.006(2) 0.024(2) C20 0.057(2) 0.092(3) 0.062(3) 0.031(2) -0.008(2) 0.013(2) C21 0.053(2) 0.075(3) 0.041(2) 0.014(2) 0.000(2) 0.008(2) C22 0.066(2) 0.052(2) 0.047(2) 0.012(2) 0.013(2) 0.011(2) C23 0.074(3) 0.058(2) 0.065(3) 0.018(2) 0.032(2) 0.017(2) C24 0.059(3) 0.060(3) 0.092(3) 0.030(2) 0.032(2) 0.022(2) C25 0.050(2) 0.070(3) 0.076(3) 0.032(2) 0.000(2) 0.012(2) C26 0.058(2) 0.054(2) 0.049(2) 0.014(2) 0.005(2) 0.016(2) C27 0.040(2) 0.042(2) 0.0316(14) 0.0067(12) 0.0045(12) 0.0106(13) C28 0.038(2) 0.049(2) 0.052(2) 0.013(2) 0.0036(14) 0.0081(15) C29 0.039(2) 0.074(3) 0.058(2) 0.012(2) 0.004(2) 0.015(2) C30 0.053(2) 0.082(3) 0.060(2) 0.019(2) 0.001(2) 0.033(2) C31 0.087(3) 0.058(3) 0.069(3) 0.028(2) 0.011(2) 0.032(2) C32 0.053(2) 0.055(2) 0.055(2) 0.024(2) 0.007(2) 0.011(2) C33 0.037(2) 0.048(2) 0.0317(15) 0.0095(12) 0.0040(12) 0.0088(13) C34 0.057(2) 0.062(3) 0.047(2) 0.005(2) 0.009(2) -0.004(2) C35 0.079(3) 0.072(3) 0.054(2) -0.015(2) 0.003(2) -0.008(2) C36 0.085(3) 0.090(4) 0.041(2) -0.003(2) 0.005(2) 0.024(3) C37 0.074(3) 0.087(3) 0.044(2) 0.027(2) 0.021(2) 0.030(2) C38 0.054(2) 0.056(2) 0.045(2) 0.019(2) 0.0132(15) 0.018(2) N1 0.060(2) 0.075(2) 0.084(2) 0.034(2) -0.007(2) 0.011(2) N2 0.078(3) 0.118(4) 0.074(3) 0.037(2) 0.015(2) 0.034(3) N3 0.115(3) 0.068(2) 0.049(2) 0.028(2) 0.028(2) 0.029(2) N4 0.056(2) 0.085(2) 0.062(2) 0.041(2) 0.0184(15) 0.020(2) N5 0.064(2) 0.068(2) 0.048(2) 0.0289(14) 0.0208(14) 0.032(2) N6 0.060(2) 0.088(3) 0.052(2) 0.036(2) 0.0178(15) 0.024(2) N7 0.0348(15) 0.064(2) 0.046(2) -0.0035(14) 0.0029(12) 0.0025(13) N8 0.054(2) 0.061(2) 0.057(2) 0.000(2) -0.0089(15) 0.010(2) N9 0.051(2) 0.046(2) 0.0409(15) 0.0143(12) 0.0093(12) 0.0053(13) N10 0.0434(15) 0.049(2) 0.0359(14) 0.0134(11) 0.0046(11) 0.0041(12) P1 0.0615(6) 0.0518(6) 0.0433(5) 0.0216(4) 0.0092(4) 0.0130(4) P2 0.0341(4) 0.0476(5) 0.0300(4) 0.0099(3) 0.0049(3) 0.0091(3) Cu 0.0425(2) 0.0483(3) 0.0329(2) 0.0143(2) 0.00564(15) 0.0067(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 C1 N2 1.170(5) . ? C1 N1 1.287(5) . ? C2 N4 1.136(4) . ? C2 N3 1.288(4) . ? C3 N6 1.148(4) . ? C3 N5 1.282(4) . ? C4 N8 1.148(4) . ? C4 N7 1.293(4) . ? C5 C6 1.387(5) . ? C5 C10 1.393(5) . ? C5 P1 1.798(4) . ? C6 C7 1.387(7) . ? C7 C8 1.360(8) . ? C8 C9 1.379(7) . ? C9 C10 1.378(7) . ? C11 C12 1.381(5) . ? C11 C16 1.381(5) . ? C11 P1 1.793(3) . ? C12 C13 1.388(6) . ? C13 C14 1.362(7) . ? C14 C15 1.370(7) . ? C15 C16 1.377(6) . ? C17 N10 1.328(5) . ? C17 C18 1.367(6) . ? C18 C19 1.369(6) . ? C19 C20 1.376(6) . ? C20 C21 1.370(6) . ? C21 N10 1.337(4) . ? C22 N9 1.355(4) . ? C22 C23 1.367(6) . ? C23 C24 1.376(6) . ? C24 C25 1.358(6) . ? C25 C26 1.374(5) . ? C26 N9 1.328(5) . ? C27 C32 1.385(5) . ? C27 C28 1.397(5) . ? C27 P2 1.791(3) . ? C28 C29 1.376(5) . ? C29 C30 1.358(6) . ? C30 C31 1.388(6) . ? C31 C32 1.387(5) . ? C33 C34 1.369(5) . ? C33 C38 1.385(4) . ? C33 P2 1.792(3) . ? C34 C35 1.388(5) . ? C35 C36 1.365(7) . ? C36 C37 1.362(7) . ? C37 C38 1.384(5) . ? N1 P1 1.604(4) . ? N3 P1 1.601(3) . ? N4 Cu 1.987(3) . ? N5 P2 1.597(3) . ? N6 Cu 1.974(3) . ? N7 P2 1.595(3) . ? N8 Cu 2.178(3) 2_667 ? N9 Cu 2.032(3) . ? N10 Cu 2.042(3) . ? Cu N8 2.178(3) 2_667 ? 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 C1 N1 174.6(5) . . ? N4 C2 N3 173.2(4) . . ? N6 C3 N5 174.9(4) . . ? N8 C4 N7 175.3(4) . . ? C6 C5 C10 118.2(4) . . ? C6 C5 P1 119.6(3) . . ? C10 C5 P1 121.9(3) . . ? C5 C6 C7 120.7(5) . . ? C8 C7 C6 120.4(5) . . ? C7 C8 C9 119.7(5) . . ? C8 C9 C10 120.6(5) . . ? C9 C10 C5 120.3(4) . . ? C12 C11 C16 119.1(3) . . ? C12 C11 P1 119.7(3) . . ? C16 C11 P1 121.0(3) . . ? C11 C12 C13 119.7(4) . . ? C14 C13 C12 120.4(4) . . ? C13 C14 C15 120.2(4) . . ? C14 C15 C16 119.8(4) . . ? C15 C16 C11 120.7(4) . . ? N10 C17 C18 123.9(4) . . ? C17 C18 C19 118.8(4) . . ? C18 C19 C20 118.3(4) . . ? C21 C20 C19 119.3(4) . . ? N10 C21 C20 122.8(4) . . ? N9 C22 C23 122.6(4) . . ? C22 C23 C24 118.9(4) . . ? C25 C24 C23 118.9(4) . . ? C24 C25 C26 119.4(4) . . ? N9 C26 C25 122.9(4) . . ? C32 C27 C28 118.4(3) . . ? C32 C27 P2 121.1(3) . . ? C28 C27 P2 120.5(2) . . ? C29 C28 C27 120.9(3) . . ? C30 C29 C28 119.9(4) . . ? C29 C30 C31 120.8(4) . . ? C32 C31 C30 119.4(4) . . ? C27 C32 C31 120.5(4) . . ? C34 C33 C38 119.6(3) . . ? C34 C33 P2 119.2(2) . . ? C38 C33 P2 121.2(3) . . ? C33 C34 C35 120.5(4) . . ? C36 C35 C34 119.6(4) . . ? C37 C36 C35 120.2(4) . . ? C36 C37 C38 120.8(4) . . ? C37 C38 C33 119.3(4) . . ? C1 N1 P1 124.9(3) . . ? C2 N3 P1 130.4(3) . . ? C2 N4 Cu 164.1(3) . . ? C3 N5 P2 128.4(3) . . ? C3 N6 Cu 165.0(3) . . ? C4 N7 P2 124.7(2) . . ? C4 N8 Cu 164.7(3) . 2_667 ? C26 N9 C22 117.1(3) . . ? C26 N9 Cu 123.1(2) . . ? C22 N9 Cu 119.7(3) . . ? C17 N10 C21 116.9(3) . . ? C17 N10 Cu 121.5(2) . . ? C21 N10 Cu 121.6(2) . . ? N3 P1 N1 118.9(2) . . ? N3 P1 C11 104.0(2) . . ? N1 P1 C11 104.9(2) . . ? N3 P1 C5 110.7(2) . . ? N1 P1 C5 111.6(2) . . ? C11 P1 C5 105.4(2) . . ? N7 P2 N5 117.9(2) . . ? N7 P2 C27 110.0(2) . . ? N5 P2 C27 110.40(14) . . ? N7 P2 C33 105.18(15) . . ? N5 P2 C33 104.1(2) . . ? C27 P2 C33 108.54(14) . . ? N6 Cu N4 157.4(2) . . ? N6 Cu N9 86.99(12) . . ? N4 Cu N9 90.06(12) . . ? N6 Cu N10 88.11(11) . . ? N4 Cu N10 90.80(11) . . ? N9 Cu N10 169.26(11) . . ? N6 Cu N8 104.02(14) . 2_667 ? N4 Cu N8 98.60(14) . 2_667 ? N9 Cu N8 95.42(12) . 2_667 ? N10 Cu N8 95.04(11) . 2_667 ? _refine_diff_density_max 0.378 _refine_diff_density_min -0.739 _refine_diff_density_rms 0.058