Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_coden_Cambridge 0222 #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Damir Safin' _publ_contact_author_address ; Department of Chemistry Kazan State University Kremlevskaya, 18 Kazan 420008 RUSSIAN FEDERATION ; _publ_contact_author_email DAMIR.SAFIN@KSU.RU _publ_section_title ; Complexes of N-Thiophosphorylthioureas (HL) with Copper(I). Crystal structures of [Cu3L3] and [Cu(PPh3)2L] chelates ; _publ_contact_letter ; Please consider this CIF submission as supplementary material for a paper intended for publication. ; _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? #============================================================================== # 3. TITLE AND AUTHOR LIST # 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 #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' F.Sokolov ; Institut f\"ur Anorganische Chemie J. W. Goethe-Universit\"at Frankfurt Max-von-Laue-Str. 7 60438 Frankfurt/Main Germany ; M.Babashkina ; Institut f\"ur Anorganische Chemie J. W. Goethe-Universit\"at Frankfurt Max-von-Laue-Str. 7 60438 Frankfurt/Main Germany ; D.Safin ; Institut f\"ur Anorganische Chemie J. W. Goethe-Universit\"at Frankfurt Max-von-Laue-Str. 7 60438 Frankfurt/Main Germany ; N.Zabirov ; Institut f\"ur Anorganische Chemie J. W. Goethe-Universit\"at Frankfurt Max-von-Laue-Str. 7 60438 Frankfurt/Main Germany ; A.Rakhmatoulline ; Institut f\"ur Anorganische Chemie J. W. Goethe-Universit\"at Frankfurt Max-von-Laue-Str. 7 60438 Frankfurt/Main Germany ; ; F.Fayon ; ; Institut f\"ur Anorganische Chemie J. W. Goethe-Universit\"at Frankfurt Max-von-Laue-Str. 7 60438 Frankfurt/Main Germany ; V.Brusko ; Institut f\"ur Anorganische Chemie J. W. Goethe-Universit\"at Frankfurt Max-von-Laue-Str. 7 60438 Frankfurt/Main Germany ; J.Galezowska ; Institut f\"ur Anorganische Chemie J. W. Goethe-Universit\"at Frankfurt Max-von-Laue-Str. 7 60438 Frankfurt/Main Germany ; H.Kozlowski ; Institut f\"ur Anorganische Chemie J. W. Goethe-Universit\"at Frankfurt Max-von-Laue-Str. 7 60438 Frankfurt/Main Germany ; M.Bolte ; Institut f\"ur Anorganische Chemie J. W. Goethe-Universit\"at Frankfurt Max-von-Laue-Str. 7 60438 Frankfurt/Main Germany ; #============================================================================== # 4. TEXT _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; H atoms were refined with fixed individual displacement parameters [U(H) = 1.2 U~eq~(C) or U(H) = 1.5 U~eq~(C~methyl~)] using a riding model with C-H = 0.99 and 0.98 \%A, for C~methylene~ and C~methyl~, respectively. ; _publ_section_references ; Allen, F. H. (2002). Acta Cryst., B58, 380-388. Sheldrick, G.M. (1990). Acta Cryst. A46, 467 - 473. Sheldrick, G.M. (1991). SHELXTL-Plus. Release 4.1. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G.M. (1997). SHELXL-97. Program for the refinement of crystal structures. Univ. of G\"ottingen, Federal Republic of Germany. Spek, A.L. (1990). Acta Cryst. A46, C-34. ; _publ_section_figure_captions ; ; #============================================================================== data_wbr1 _database_code_depnum_ccdc_archive 'CCDC 619482' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H66 Cu3 N6 O9 P3 S6' _chemical_formula_weight 1166.81 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' S S 0.1246 0.1234 '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 10.4622(5) _cell_length_b 12.3431(5) _cell_length_c 21.1918(9) _cell_angle_alpha 88.634(3) _cell_angle_beta 81.852(3) _cell_angle_gamma 75.398(3) _cell_volume 2621.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 72420 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.8 _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1212 _exptl_absorpt_coefficient_mu 1.586 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5420 _exptl_absorpt_correction_T_max 0.7317 _exptl_absorpt_process_details 'MULABS (Spek, 1990; Blessing, 1995)' _exptl_special_details ; ; _diffrn_ambient_temperature 173(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 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 58248 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0180 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.58 _reflns_number_total 12072 _reflns_number_gt 10908 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997) ' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material SHELXL97 _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^)+(0.0406P)^2^+1.8949P] 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 12072 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_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_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 0.49567(2) 0.414068(19) 0.705981(11) 0.02575(6) Uani 1 1 d . . . S1 S 0.70052(5) 0.33065(4) 0.72945(3) 0.03129(11) Uani 1 1 d . . . P1 P 0.63588(5) 0.24132(4) 0.80069(2) 0.02445(10) Uani 1 1 d . . . N1 N 0.51798(18) 0.30090(14) 0.85513(8) 0.0297(4) Uani 1 1 d . . . C1 C 0.3959(2) 0.35888(15) 0.85203(9) 0.0260(4) Uani 1 1 d . . . S11 S 0.32512(5) 0.40062(4) 0.78059(2) 0.02551(9) Uani 1 1 d . . . Cu2 Cu 0.30739(2) 0.587182(19) 0.781399(11) 0.02577(6) Uani 1 1 d . . . S2 S 0.39757(5) 0.66837(4) 0.85253(2) 0.03053(10) Uani 1 1 d . . . P2 P 0.24941(5) 0.80598(4) 0.85614(2) 0.02214(9) Uani 1 1 d . . . N2 N 0.21769(17) 0.87302(13) 0.79177(7) 0.0254(3) Uani 1 1 d . . . C2 C 0.18688(17) 0.84200(15) 0.73831(8) 0.0207(3) Uani 1 1 d . . . S21 S 0.17988(4) 0.70372(4) 0.71908(2) 0.02153(9) Uani 1 1 d . . . Cu3 Cu 0.38330(2) 0.652633(19) 0.659246(10) 0.02398(6) Uani 1 1 d . . . S3 S 0.49260(6) 0.78672(4) 0.63817(3) 0.03744(13) Uani 1 1 d . . . P3 P 0.66839(5) 0.69394(4) 0.59721(2) 0.02588(10) Uani 1 1 d . . . N3 N 0.68037(17) 0.57617(14) 0.56463(8) 0.0283(3) Uani 1 1 d . . . C3 C 0.62445(17) 0.49228(14) 0.56709(8) 0.0190(3) Uani 1 1 d . . . S31 S 0.46516(4) 0.48940(4) 0.61012(2) 0.02033(9) Uani 1 1 d . . . O11 O 0.59462(16) 0.13583(12) 0.77812(7) 0.0335(3) Uani 1 1 d . . . C4 C 0.6499(2) 0.07173(18) 0.71913(11) 0.0359(5) Uani 1 1 d . . . H4 H 0.7229 0.1023 0.6958 0.043 Uiso 1 1 calc R . . C41 C 0.5381(4) 0.0876(4) 0.67984(18) 0.0803(11) Uani 1 1 d . . . H41A H 0.5069 0.1672 0.6702 0.120 Uiso 1 1 calc R . . H41B H 0.4645 0.0615 0.7037 0.120 Uiso 1 1 calc R . . H41C H 0.5700 0.0446 0.6399 0.120 Uiso 1 1 calc R . . C42 C 0.7061(4) -0.0479(2) 0.7367(2) 0.0756(11) Uani 1 1 d . . . H42A H 0.7781 -0.0517 0.7622 0.113 Uiso 1 1 calc R . . H42B H 0.7411 -0.0933 0.6978 0.113 Uiso 1 1 calc R . . H42C H 0.6355 -0.0767 0.7614 0.113 Uiso 1 1 calc R . . O12 O 0.75674(16) 0.18585(13) 0.83789(7) 0.0346(3) Uani 1 1 d . . . C5 C 0.8058(3) 0.2571(3) 0.87828(12) 0.0505(6) Uani 1 1 d . . . H5 H 0.7556 0.3369 0.8745 0.061 Uiso 1 1 calc R . . C51 C 0.7784(5) 0.2189(4) 0.94656(15) 0.0891(13) Uani 1 1 d . . . H51A H 0.6820 0.2307 0.9591 0.134 Uiso 1 1 calc R . . H51B H 0.8133 0.2622 0.9751 0.134 Uiso 1 1 calc R . . H51C H 0.8222 0.1392 0.9495 0.134 Uiso 1 1 calc R . . C52 C 0.9504(4) 0.2445(5) 0.8540(2) 0.1077(18) Uani 1 1 d . . . H52A H 0.9597 0.2717 0.8102 0.162 Uiso 1 1 calc R . . H52B H 0.9984 0.1654 0.8548 0.162 Uiso 1 1 calc R . . H52C H 0.9878 0.2883 0.8811 0.162 Uiso 1 1 calc R . . N11 N 0.31482(19) 0.38677(16) 0.90810(8) 0.0367(4) Uani 1 1 d . . . C12 C 0.1735(2) 0.4460(2) 0.91547(11) 0.0420(5) Uani 1 1 d . . . H12A H 0.1181 0.3927 0.9281 0.050 Uiso 1 1 calc R . . H12B H 0.1504 0.4795 0.8744 0.050 Uiso 1 1 calc R . . C13 C 0.1452(3) 0.5370(2) 0.96578(11) 0.0463(6) Uani 1 1 d . . . H13A H 0.1960 0.5929 0.9514 0.056 Uiso 1 1 calc R . . H13B H 0.0491 0.5756 0.9713 0.056 Uiso 1 1 calc R . . O14 O 0.18139(19) 0.49222(16) 1.02576(8) 0.0477(4) Uani 1 1 d . . . C15 C 0.3210(3) 0.4417(3) 1.01781(12) 0.0512(6) Uani 1 1 d . . . H15A H 0.3471 0.4125 1.0593 0.061 Uiso 1 1 calc R . . H15B H 0.3699 0.4991 1.0039 0.061 Uiso 1 1 calc R . . C16 C 0.3600(3) 0.3472(2) 0.96931(10) 0.0460(6) Uani 1 1 d . . . H16A H 0.4582 0.3176 0.9629 0.055 Uiso 1 1 calc R . . H16B H 0.3194 0.2858 0.9853 0.055 Uiso 1 1 calc R . . O21 O 0.27485(14) 0.89742(12) 0.90107(6) 0.0276(3) Uani 1 1 d . . . C6 C 0.3813(2) 0.9538(2) 0.87971(11) 0.0359(5) Uani 1 1 d . . . H6 H 0.4198 0.9300 0.8348 0.043 Uiso 1 1 calc R . . C61 C 0.3209(3) 1.0775(2) 0.8814(2) 0.0707(10) Uani 1 1 d . . . H61A H 0.2523 1.0956 0.8530 0.106 Uiso 1 1 calc R . . H61B H 0.3905 1.1166 0.8672 0.106 Uiso 1 1 calc R . . H61C H 0.2804 1.1014 0.9250 0.106 Uiso 1 1 calc R . . C62 C 0.4889(4) 0.9158(4) 0.9218(2) 0.0768(11) Uani 1 1 d . . . H62A H 0.5230 0.8343 0.9184 0.115 Uiso 1 1 calc R . . H62B H 0.4516 0.9369 0.9662 0.115 Uiso 1 1 calc R . . H62C H 0.5618 0.9515 0.9083 0.115 Uiso 1 1 calc R . . O22 O 0.11946(14) 0.77896(12) 0.89414(7) 0.0293(3) Uani 1 1 d . . . C7 C -0.0147(3) 0.8509(3) 0.89441(16) 0.0698(11) Uani 1 1 d . . . H7 H -0.0164 0.9190 0.8676 0.084 Uiso 1 1 calc R . . C71 C -0.0727(4) 0.8792(4) 0.9644(2) 0.1001(16) Uani 1 1 d . . . H71A H -0.0259 0.9289 0.9815 0.150 Uiso 1 1 calc R . . H71B H -0.0613 0.8101 0.9891 0.150 Uiso 1 1 calc R . . H71C H -0.1678 0.9166 0.9673 0.150 Uiso 1 1 calc R . . C72 C -0.0951(4) 0.7794(8) 0.8734(3) 0.201(5) Uani 1 1 d . . . H72A H -0.0648 0.7588 0.8283 0.301 Uiso 1 1 calc R . . H72B H -0.1893 0.8205 0.8787 0.301 Uiso 1 1 calc R . . H72C H -0.0846 0.7114 0.8991 0.301 Uiso 1 1 calc R . . N21 N 0.15367(17) 0.92217(13) 0.69468(7) 0.0247(3) Uani 1 1 d . . . C22 C 0.1645(2) 1.03671(16) 0.70441(10) 0.0297(4) Uani 1 1 d . . . H22A H 0.2449 1.0489 0.6774 0.036 Uiso 1 1 calc R . . H22B H 0.1736 1.0478 0.7495 0.036 Uiso 1 1 calc R . . C23 C 0.0411(2) 1.12017(18) 0.68719(10) 0.0362(5) Uani 1 1 d . . . H23A H -0.0383 1.1113 0.7163 0.043 Uiso 1 1 calc R . . H23B H 0.0501 1.1972 0.6926 0.043 Uiso 1 1 calc R . . O24 O 0.02324(18) 1.10375(13) 0.62304(7) 0.0412(4) Uani 1 1 d . . . C25 C 0.0077(2) 0.99357(18) 0.61430(10) 0.0340(4) Uani 1 1 d . . . H25A H -0.0040 0.9839 0.5694 0.041 Uiso 1 1 calc R . . H25B H -0.0740 0.9851 0.6417 0.041 Uiso 1 1 calc R . . C26 C 0.1263(2) 0.90264(16) 0.63033(8) 0.0261(4) Uani 1 1 d . . . H26A H 0.1069 0.8285 0.6282 0.031 Uiso 1 1 calc R . . H26B H 0.2058 0.9030 0.5989 0.031 Uiso 1 1 calc R . . O31 O 0.73261(14) 0.76598(12) 0.54483(7) 0.0308(3) Uani 1 1 d . . . C8 C 0.6643(2) 0.81153(18) 0.49073(11) 0.0337(4) Uani 1 1 d . . . H8 H 0.5680 0.8110 0.5003 0.040 Uiso 1 1 calc R . . C81 C 0.6761(3) 0.9312(2) 0.48394(13) 0.0453(6) Uani 1 1 d . . . H81A H 0.6325 0.9736 0.5230 0.068 Uiso 1 1 calc R . . H81B H 0.6329 0.9656 0.4477 0.068 Uiso 1 1 calc R . . H81C H 0.7705 0.9318 0.4767 0.068 Uiso 1 1 calc R . . C82 C 0.7286(3) 0.7395(2) 0.43241(12) 0.0432(5) Uani 1 1 d . . . H82A H 0.7175 0.6635 0.4396 0.065 Uiso 1 1 calc R . . H82B H 0.8239 0.7371 0.4244 0.065 Uiso 1 1 calc R . . H82C H 0.6862 0.7714 0.3955 0.065 Uiso 1 1 calc R . . O32 O 0.77937(17) 0.67879(13) 0.64242(8) 0.0370(3) Uani 1 1 d . . . C9 C 0.8016(3) 0.58533(19) 0.68664(12) 0.0402(5) Uani 1 1 d . . . H9 H 0.7346 0.5409 0.6840 0.048 Uiso 1 1 calc R . . C91 C 0.9390(3) 0.5128(3) 0.66678(19) 0.0680(9) Uani 1 1 d . . . H91A H 0.9451 0.4834 0.6236 0.102 Uiso 1 1 calc R . . H91B H 0.9573 0.4504 0.6964 0.102 Uiso 1 1 calc R . . H91C H 1.0045 0.5571 0.6673 0.102 Uiso 1 1 calc R . . C92 C 0.7816(4) 0.6345(3) 0.75287(14) 0.0730(10) Uani 1 1 d . . . H92A H 0.6900 0.6806 0.7629 0.109 Uiso 1 1 calc R . . H92B H 0.8442 0.6810 0.7550 0.109 Uiso 1 1 calc R . . H92C H 0.7975 0.5739 0.7837 0.109 Uiso 1 1 calc R . . N31 N 0.68975(15) 0.40054(13) 0.53162(7) 0.0224(3) Uani 1 1 d . . . C32 C 0.81751(19) 0.39444(17) 0.49057(10) 0.0293(4) Uani 1 1 d . . . H32A H 0.8479 0.4627 0.4968 0.035 Uiso 1 1 calc R . . H32B H 0.8056 0.3902 0.4453 0.035 Uiso 1 1 calc R . . C33 C 0.9214(2) 0.29153(19) 0.50724(11) 0.0339(4) Uani 1 1 d . . . H33A H 1.0059 0.2858 0.4783 0.041 Uiso 1 1 calc R . . H33B H 0.9388 0.2995 0.5514 0.041 Uiso 1 1 calc R . . O34 O 0.87787(16) 0.19193(13) 0.50189(7) 0.0351(3) Uani 1 1 d . . . C35 C 0.7574(2) 0.19883(16) 0.54436(10) 0.0330(4) Uani 1 1 d . . . H35A H 0.7736 0.2077 0.5886 0.040 Uiso 1 1 calc R . . H35B H 0.7294 0.1284 0.5417 0.040 Uiso 1 1 calc R . . C36 C 0.6462(2) 0.29734(15) 0.52825(9) 0.0266(4) Uani 1 1 d . . . H36A H 0.6260 0.2872 0.4849 0.032 Uiso 1 1 calc R . . H36B H 0.5642 0.3016 0.5589 0.032 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 0.03256(13) 0.02335(11) 0.01995(11) 0.00330(8) 0.00071(9) -0.00718(9) S1 0.0291(2) 0.0281(2) 0.0342(2) 0.00721(19) 0.00128(19) -0.00654(19) P1 0.0296(2) 0.0208(2) 0.0209(2) 0.00025(16) -0.00194(18) -0.00352(18) N1 0.0357(9) 0.0260(8) 0.0221(7) 0.0027(6) -0.0001(7) -0.0004(7) C1 0.0351(10) 0.0200(8) 0.0212(8) 0.0041(6) 0.0024(7) -0.0076(7) S11 0.0299(2) 0.0240(2) 0.0217(2) 0.00298(16) 0.00038(17) -0.00750(18) Cu2 0.03053(12) 0.02143(11) 0.02252(11) 0.00397(8) -0.00059(9) -0.00336(9) S2 0.0293(2) 0.0318(2) 0.0289(2) 0.00266(18) -0.00894(19) -0.0024(2) P2 0.0251(2) 0.0255(2) 0.0169(2) 0.00273(16) -0.00426(16) -0.00769(18) N2 0.0357(9) 0.0226(7) 0.0182(7) 0.0020(6) -0.0063(6) -0.0066(7) C2 0.0206(8) 0.0211(8) 0.0179(8) 0.0004(6) 0.0003(6) -0.0023(7) S21 0.0232(2) 0.02025(19) 0.02005(19) 0.00016(15) -0.00184(15) -0.00414(16) Cu3 0.02468(12) 0.02347(11) 0.02124(11) -0.00084(8) 0.00105(8) -0.00361(9) S3 0.0361(3) 0.0241(2) 0.0496(3) -0.0075(2) 0.0095(2) -0.0107(2) P3 0.0268(2) 0.0222(2) 0.0308(2) 0.00139(18) -0.00207(19) -0.01132(19) N3 0.0247(8) 0.0253(8) 0.0353(9) -0.0036(6) 0.0026(7) -0.0103(7) C3 0.0196(8) 0.0208(8) 0.0166(7) 0.0025(6) -0.0042(6) -0.0041(6) S31 0.0200(2) 0.02086(19) 0.01961(19) 0.00068(15) -0.00009(15) -0.00565(16) O11 0.0435(9) 0.0295(7) 0.0284(7) -0.0045(6) 0.0053(6) -0.0160(6) C4 0.0408(12) 0.0308(10) 0.0358(11) -0.0115(8) 0.0073(9) -0.0142(9) C41 0.084(3) 0.106(3) 0.067(2) -0.027(2) -0.0256(19) -0.042(2) C42 0.078(2) 0.0274(13) 0.106(3) -0.0054(15) 0.029(2) -0.0080(14) O12 0.0380(8) 0.0326(7) 0.0280(7) -0.0032(6) -0.0094(6) 0.0036(6) C5 0.0493(15) 0.0644(17) 0.0362(12) -0.0161(11) -0.0161(11) -0.0044(13) C51 0.105(3) 0.120(3) 0.0360(15) -0.0061(18) -0.0288(18) -0.006(3) C52 0.054(2) 0.195(5) 0.086(3) -0.056(3) -0.0143(19) -0.045(3) N11 0.0378(10) 0.0404(10) 0.0217(8) 0.0079(7) 0.0058(7) 0.0029(8) C12 0.0343(12) 0.0534(14) 0.0296(11) 0.0096(10) 0.0077(9) -0.0025(10) C13 0.0455(13) 0.0439(13) 0.0372(12) 0.0107(10) 0.0145(10) -0.0004(11) O14 0.0525(11) 0.0503(10) 0.0301(8) 0.0026(7) 0.0127(7) -0.0046(8) C15 0.0507(15) 0.0655(17) 0.0320(12) 0.0012(11) 0.0025(11) -0.0091(13) C16 0.0501(14) 0.0524(14) 0.0221(10) 0.0101(9) 0.0044(9) 0.0053(11) O21 0.0308(7) 0.0351(7) 0.0192(6) -0.0026(5) -0.0022(5) -0.0133(6) C6 0.0305(11) 0.0447(12) 0.0362(11) -0.0067(9) -0.0014(8) -0.0175(9) C61 0.0577(18) 0.0418(15) 0.112(3) -0.0132(16) 0.0139(18) -0.0247(14) C62 0.0572(19) 0.099(3) 0.092(3) 0.002(2) -0.0395(19) -0.0375(19) O22 0.0248(7) 0.0362(7) 0.0281(7) 0.0099(6) -0.0048(5) -0.0099(6) C7 0.0248(12) 0.096(2) 0.074(2) 0.0524(19) 0.0018(12) 0.0017(13) C71 0.064(2) 0.128(4) 0.091(3) -0.050(3) -0.005(2) 0.008(2) C72 0.033(2) 0.368(12) 0.191(6) -0.175(7) -0.018(3) -0.015(4) N21 0.0340(9) 0.0208(7) 0.0180(7) 0.0022(6) -0.0055(6) -0.0037(6) C22 0.0402(11) 0.0201(8) 0.0287(9) 0.0039(7) -0.0078(8) -0.0061(8) C23 0.0458(13) 0.0255(9) 0.0308(10) -0.0014(8) -0.0068(9) 0.0040(9) O24 0.0554(10) 0.0290(7) 0.0320(8) 0.0024(6) -0.0144(7) 0.0070(7) C25 0.0334(11) 0.0363(11) 0.0266(9) -0.0016(8) -0.0071(8) 0.0036(9) C26 0.0323(10) 0.0266(9) 0.0157(8) 0.0008(6) -0.0040(7) -0.0002(8) O31 0.0278(7) 0.0315(7) 0.0373(8) 0.0083(6) -0.0056(6) -0.0155(6) C8 0.0296(10) 0.0348(11) 0.0395(11) 0.0110(9) -0.0062(8) -0.0136(9) C81 0.0505(14) 0.0309(11) 0.0512(14) 0.0096(10) 0.0037(11) -0.0106(10) C82 0.0530(15) 0.0433(13) 0.0381(12) 0.0043(10) -0.0119(11) -0.0183(11) O32 0.0455(9) 0.0317(8) 0.0425(8) 0.0099(6) -0.0170(7) -0.0209(7) C9 0.0482(13) 0.0340(11) 0.0463(13) 0.0139(10) -0.0169(11) -0.0203(10) C91 0.0591(19) 0.0491(16) 0.094(3) 0.0060(16) -0.0244(18) -0.0030(14) C92 0.109(3) 0.072(2) 0.0419(15) 0.0138(14) -0.0186(17) -0.027(2) N31 0.0205(7) 0.0209(7) 0.0238(7) -0.0015(6) 0.0015(6) -0.0038(6) C32 0.0226(9) 0.0312(10) 0.0301(9) -0.0012(8) 0.0056(7) -0.0045(8) C33 0.0242(9) 0.0391(11) 0.0343(10) -0.0065(8) -0.0031(8) -0.0003(8) O34 0.0355(8) 0.0300(7) 0.0333(8) -0.0087(6) -0.0041(6) 0.0043(6) C35 0.0429(12) 0.0221(9) 0.0316(10) -0.0028(7) -0.0042(9) -0.0041(8) C36 0.0290(9) 0.0230(9) 0.0282(9) -0.0062(7) -0.0025(7) -0.0076(7) _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 S31 2.2443(5) . ? Cu1 S11 2.2469(5) . ? Cu1 S1 2.2507(6) . ? Cu1 Cu2 2.8546(4) . ? S1 P1 1.9899(7) . ? P1 O11 1.5755(15) . ? P1 O12 1.5842(15) . ? P1 N1 1.6040(17) . ? N1 C1 1.307(3) . ? C1 N11 1.355(2) . ? C1 S11 1.787(2) . ? S11 Cu2 2.2634(5) . ? Cu2 S21 2.2437(5) . ? Cu2 S2 2.2624(6) . ? Cu2 Cu3 2.7614(3) . ? S2 P2 1.9847(7) . ? P2 O22 1.5854(14) . ? P2 O21 1.5893(14) . ? P2 N2 1.6100(16) . ? N2 C2 1.312(2) . ? C2 N21 1.352(2) . ? C2 S21 1.7858(18) . ? S21 Cu3 2.2653(5) . ? Cu3 S31 2.2032(5) . ? Cu3 S3 2.2406(6) . ? S3 P3 1.9950(8) . ? P3 O32 1.5805(16) . ? P3 O31 1.5866(14) . ? P3 N3 1.5928(17) . ? N3 C3 1.308(2) . ? C3 N31 1.349(2) . ? C3 S31 1.7910(18) . ? O11 C4 1.461(2) . ? C4 C41 1.500(4) . ? C4 C42 1.504(4) . ? C4 H4 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? O12 C5 1.469(3) . ? C5 C52 1.498(5) . ? C5 C51 1.522(4) . ? C5 H5 1.0000 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? N11 C12 1.463(3) . ? N11 C16 1.474(3) . ? C12 C13 1.512(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 O14 1.436(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? O14 C15 1.423(3) . ? C15 C16 1.510(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? O21 C6 1.471(2) . ? C6 C61 1.498(4) . ? C6 C62 1.511(4) . ? C6 H6 1.0000 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? O22 C7 1.458(3) . ? C7 C72 1.479(7) . ? C7 C71 1.534(5) . ? C7 H7 1.0000 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? N21 C22 1.468(2) . ? N21 C26 1.470(2) . ? C22 C23 1.519(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O24 1.424(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? O24 C25 1.429(3) . ? C25 C26 1.521(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? O31 C8 1.463(3) . ? C8 C82 1.512(3) . ? C8 C81 1.515(3) . ? C8 H8 1.0000 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? O32 C9 1.462(3) . ? C9 C91 1.498(4) . ? C9 C92 1.508(4) . ? C9 H9 1.0000 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? N31 C36 1.464(2) . ? N31 C32 1.474(2) . ? C32 C33 1.520(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 O34 1.427(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? O34 C35 1.426(3) . ? C35 C36 1.526(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 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 S31 Cu1 S11 122.59(2) . . ? S31 Cu1 S1 121.58(2) . . ? S11 Cu1 S1 115.53(2) . . ? S31 Cu1 Cu2 97.516(15) . . ? S11 Cu1 Cu2 50.993(14) . . ? S1 Cu1 Cu2 124.385(18) . . ? P1 S1 Cu1 94.83(3) . . ? O11 P1 O12 102.08(9) . . ? O11 P1 N1 105.68(9) . . ? O12 P1 N1 104.64(9) . . ? O11 P1 S1 113.83(6) . . ? O12 P1 S1 108.59(7) . . ? N1 P1 S1 120.18(7) . . ? C1 N1 P1 131.45(15) . . ? N1 C1 N11 116.88(18) . . ? N1 C1 S11 125.88(14) . . ? N11 C1 S11 117.21(16) . . ? C1 S11 Cu1 106.13(7) . . ? C1 S11 Cu2 101.39(6) . . ? Cu1 S11 Cu2 78.528(17) . . ? S21 Cu2 S2 116.24(2) . . ? S21 Cu2 S11 121.52(2) . . ? S2 Cu2 S11 121.89(2) . . ? S21 Cu2 Cu3 52.589(13) . . ? S2 Cu2 Cu3 110.221(17) . . ? S11 Cu2 Cu3 108.857(15) . . ? S21 Cu2 Cu1 110.203(15) . . ? S2 Cu2 Cu1 113.838(17) . . ? S11 Cu2 Cu1 50.479(13) . . ? Cu3 Cu2 Cu1 66.467(9) . . ? P2 S2 Cu2 91.40(2) . . ? O22 P2 O21 101.90(8) . . ? O22 P2 N2 111.30(9) . . ? O21 P2 N2 103.71(8) . . ? O22 P2 S2 108.36(6) . . ? O21 P2 S2 110.11(6) . . ? N2 P2 S2 119.89(7) . . ? C2 N2 P2 131.75(14) . . ? N2 C2 N21 117.29(16) . . ? N2 C2 S21 125.64(14) . . ? N21 C2 S21 117.04(13) . . ? C2 S21 Cu2 106.55(6) . . ? C2 S21 Cu3 96.83(6) . . ? Cu2 S21 Cu3 75.529(16) . . ? S31 Cu3 S3 118.51(2) . . ? S31 Cu3 S21 124.191(19) . . ? S3 Cu3 S21 116.68(2) . . ? S31 Cu3 Cu2 101.290(15) . . ? S3 Cu3 Cu2 123.172(19) . . ? S21 Cu3 Cu2 51.882(13) . . ? P3 S3 Cu3 99.70(3) . . ? O32 P3 O31 96.57(8) . . ? O32 P3 N3 108.59(9) . . ? O31 P3 N3 106.59(9) . . ? O32 P3 S3 111.99(7) . . ? O31 P3 S3 109.16(6) . . ? N3 P3 S3 121.03(7) . . ? C3 N3 P3 142.40(15) . . ? N3 C3 N31 117.21(16) . . ? N3 C3 S31 126.37(14) . . ? N31 C3 S31 116.35(13) . . ? C3 S31 Cu3 106.98(6) . . ? C3 S31 Cu1 108.58(6) . . ? Cu3 S31 Cu1 87.615(17) . . ? C4 O11 P1 126.23(13) . . ? O11 C4 C41 106.4(2) . . ? O11 C4 C42 107.9(2) . . ? C41 C4 C42 114.1(3) . . ? O11 C4 H4 109.4 . . ? C41 C4 H4 109.4 . . ? C42 C4 H4 109.4 . . ? C4 C41 H41A 109.5 . . ? C4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C4 C42 H42A 109.5 . . ? C4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C5 O12 P1 118.95(15) . . ? O12 C5 C52 107.1(2) . . ? O12 C5 C51 106.7(3) . . ? C52 C5 C51 114.4(3) . . ? O12 C5 H5 109.5 . . ? C52 C5 H5 109.5 . . ? C51 C5 H5 109.5 . . ? C5 C51 H51A 109.5 . . ? C5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C5 C52 H52A 109.5 . . ? C5 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C5 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C1 N11 C12 125.86(18) . . ? C1 N11 C16 121.31(19) . . ? C12 N11 C16 112.50(17) . . ? N11 C12 C13 109.7(2) . . ? N11 C12 H12A 109.7 . . ? C13 C12 H12A 109.7 . . ? N11 C12 H12B 109.7 . . ? C13 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? O14 C13 C12 111.5(2) . . ? O14 C13 H13A 109.3 . . ? C12 C13 H13A 109.3 . . ? O14 C13 H13B 109.3 . . ? C12 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? C15 O14 C13 108.75(18) . . ? O14 C15 C16 111.9(2) . . ? O14 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? O14 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? N11 C16 C15 110.5(2) . . ? N11 C16 H16A 109.6 . . ? C15 C16 H16A 109.6 . . ? N11 C16 H16B 109.6 . . ? C15 C16 H16B 109.6 . . ? H16A C16 H16B 108.1 . . ? C6 O21 P2 119.51(12) . . ? O21 C6 C61 108.3(2) . . ? O21 C6 C62 107.7(2) . . ? C61 C6 C62 114.3(3) . . ? O21 C6 H6 108.8 . . ? C61 C6 H6 108.8 . . ? C62 C6 H6 108.8 . . ? C6 C61 H61A 109.5 . . ? C6 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C6 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C6 C62 H62A 109.5 . . ? C6 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C6 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C7 O22 P2 123.77(15) . . ? O22 C7 C72 106.1(4) . . ? O22 C7 C71 106.8(3) . . ? C72 C7 C71 104.6(4) . . ? O22 C7 H7 112.9 . . ? C72 C7 H7 112.9 . . ? C71 C7 H7 112.9 . . ? C7 C71 H71A 109.5 . . ? C7 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C7 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C7 C72 H72A 109.5 . . ? C7 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C7 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C2 N21 C22 120.98(16) . . ? C2 N21 C26 125.32(16) . . ? C22 N21 C26 112.93(15) . . ? N21 C22 C23 109.73(18) . . ? N21 C22 H22A 109.7 . . ? C23 C22 H22A 109.7 . . ? N21 C22 H22B 109.7 . . ? C23 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? O24 C23 C22 110.95(17) . . ? O24 C23 H23A 109.4 . . ? C22 C23 H23A 109.4 . . ? O24 C23 H23B 109.4 . . ? C22 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? C23 O24 C25 110.46(16) . . ? O24 C25 C26 112.59(18) . . ? O24 C25 H25A 109.1 . . ? C26 C25 H25A 109.1 . . ? O24 C25 H25B 109.1 . . ? C26 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? N21 C26 C25 109.91(15) . . ? N21 C26 H26A 109.7 . . ? C25 C26 H26A 109.7 . . ? N21 C26 H26B 109.7 . . ? C25 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? C8 O31 P3 120.88(12) . . ? O31 C8 C82 108.87(18) . . ? O31 C8 C81 105.99(19) . . ? C82 C8 C81 113.26(19) . . ? O31 C8 H8 109.5 . . ? C82 C8 H8 109.5 . . ? C81 C8 H8 109.5 . . ? C8 C81 H81A 109.5 . . ? C8 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C8 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C8 C82 H82A 109.5 . . ? C8 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C8 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C9 O32 P3 120.98(13) . . ? O32 C9 C91 107.8(2) . . ? O32 C9 C92 107.3(2) . . ? C91 C9 C92 113.6(3) . . ? O32 C9 H9 109.3 . . ? C91 C9 H9 109.3 . . ? C92 C9 H9 109.3 . . ? C9 C91 H91A 109.5 . . ? C9 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C9 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C9 C92 H92A 109.5 . . ? C9 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C9 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C3 N31 C36 126.05(15) . . ? C3 N31 C32 122.09(16) . . ? C36 N31 C32 111.86(15) . . ? N31 C32 C33 109.58(16) . . ? N31 C32 H32A 109.8 . . ? C33 C32 H32A 109.8 . . ? N31 C32 H32B 109.8 . . ? C33 C32 H32B 109.8 . . ? H32A C32 H32B 108.2 . . ? O34 C33 C32 111.32(17) . . ? O34 C33 H33A 109.4 . . ? C32 C33 H33A 109.4 . . ? O34 C33 H33B 109.4 . . ? C32 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C35 O34 C33 109.62(15) . . ? O34 C35 C36 111.28(17) . . ? O34 C35 H35A 109.4 . . ? C36 C35 H35A 109.4 . . ? O34 C35 H35B 109.4 . . ? C36 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? N31 C36 C35 108.73(16) . . ? N31 C36 H36A 109.9 . . ? C35 C36 H36A 109.9 . . ? N31 C36 H36B 109.9 . . ? C35 C36 H36B 109.9 . . ? H36A C36 H36B 108.3 . . ? 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 S31 Cu1 S1 P1 -158.85(2) . . . . ? S11 Cu1 S1 P1 15.02(3) . . . . ? Cu2 Cu1 S1 P1 73.80(3) . . . . ? Cu1 S1 P1 O11 77.24(7) . . . . ? Cu1 S1 P1 O12 -169.80(6) . . . . ? Cu1 S1 P1 N1 -49.53(9) . . . . ? O11 P1 N1 C1 -72.6(2) . . . . ? O12 P1 N1 C1 -179.93(19) . . . . ? S1 P1 N1 C1 57.9(2) . . . . ? P1 N1 C1 N11 172.08(17) . . . . ? P1 N1 C1 S11 -5.8(3) . . . . ? N1 C1 S11 Cu1 -27.73(19) . . . . ? N11 C1 S11 Cu1 154.45(15) . . . . ? N1 C1 S11 Cu2 -108.93(17) . . . . ? N11 C1 S11 Cu2 73.25(16) . . . . ? S31 Cu1 S11 C1 -170.14(6) . . . . ? S1 Cu1 S11 C1 16.06(7) . . . . ? Cu2 Cu1 S11 C1 -98.69(7) . . . . ? S31 Cu1 S11 Cu2 -71.46(2) . . . . ? S1 Cu1 S11 Cu2 114.74(2) . . . . ? C1 S11 Cu2 S21 -164.52(7) . . . . ? Cu1 S11 Cu2 S21 91.10(2) . . . . ? C1 S11 Cu2 S2 8.42(7) . . . . ? Cu1 S11 Cu2 S2 -95.96(2) . . . . ? C1 S11 Cu2 Cu3 138.41(7) . . . . ? Cu1 S11 Cu2 Cu3 34.033(18) . . . . ? C1 S11 Cu2 Cu1 104.38(7) . . . . ? S31 Cu1 Cu2 S21 11.57(2) . . . . ? S11 Cu1 Cu2 S21 -114.75(2) . . . . ? S1 Cu1 Cu2 S21 148.49(2) . . . . ? S31 Cu1 Cu2 S2 -121.09(2) . . . . ? S11 Cu1 Cu2 S2 112.59(2) . . . . ? S1 Cu1 Cu2 S2 15.83(3) . . . . ? S31 Cu1 Cu2 S11 126.32(2) . . . . ? S1 Cu1 Cu2 S11 -96.77(2) . . . . ? S31 Cu1 Cu2 Cu3 -18.392(14) . . . . ? S11 Cu1 Cu2 Cu3 -144.713(19) . . . . ? S1 Cu1 Cu2 Cu3 118.52(2) . . . . ? S21 Cu2 S2 P2 27.26(3) . . . . ? S11 Cu2 S2 P2 -146.03(2) . . . . ? Cu3 Cu2 S2 P2 84.56(2) . . . . ? Cu1 Cu2 S2 P2 156.959(19) . . . . ? Cu2 S2 P2 O22 72.40(6) . . . . ? Cu2 S2 P2 O21 -176.93(6) . . . . ? Cu2 S2 P2 N2 -56.82(8) . . . . ? O22 P2 N2 C2 -69.8(2) . . . . ? O21 P2 N2 C2 -178.68(18) . . . . ? S2 P2 N2 C2 58.1(2) . . . . ? P2 N2 C2 N21 174.01(15) . . . . ? P2 N2 C2 S21 -3.9(3) . . . . ? N2 C2 S21 Cu2 -22.16(18) . . . . ? N21 C2 S21 Cu2 159.92(13) . . . . ? N2 C2 S21 Cu3 -99.04(16) . . . . ? N21 C2 S21 Cu3 83.04(14) . . . . ? S2 Cu2 S21 C2 3.26(6) . . . . ? S11 Cu2 S21 C2 176.58(6) . . . . ? Cu3 Cu2 S21 C2 -92.94(6) . . . . ? Cu1 Cu2 S21 C2 -128.15(6) . . . . ? S2 Cu2 S21 Cu3 96.21(2) . . . . ? S11 Cu2 S21 Cu3 -90.47(2) . . . . ? Cu1 Cu2 S21 Cu3 -35.207(16) . . . . ? C2 S21 Cu3 S31 -178.04(6) . . . . ? Cu2 S21 Cu3 S31 76.57(2) . . . . ? C2 S21 Cu3 S3 -7.19(6) . . . . ? Cu2 S21 Cu3 S3 -112.58(2) . . . . ? C2 S21 Cu3 Cu2 105.39(6) . . . . ? S21 Cu2 Cu3 S31 -124.87(2) . . . . ? S2 Cu2 Cu3 S31 126.98(2) . . . . ? S11 Cu2 Cu3 S31 -9.13(2) . . . . ? Cu1 Cu2 Cu3 S31 18.962(15) . . . . ? S21 Cu2 Cu3 S3 99.73(3) . . . . ? S2 Cu2 Cu3 S3 -8.42(3) . . . . ? S11 Cu2 Cu3 S3 -144.53(2) . . . . ? Cu1 Cu2 Cu3 S3 -116.44(2) . . . . ? S2 Cu2 Cu3 S21 -108.15(2) . . . . ? S11 Cu2 Cu3 S21 115.74(2) . . . . ? Cu1 Cu2 Cu3 S21 143.833(18) . . . . ? S31 Cu3 S3 P3 -16.43(4) . . . . ? S21 Cu3 S3 P3 172.18(3) . . . . ? Cu2 Cu3 S3 P3 111.97(3) . . . . ? Cu3 S3 P3 O32 -106.49(6) . . . . ? Cu3 S3 P3 O31 147.78(6) . . . . ? Cu3 S3 P3 N3 23.61(9) . . . . ? O32 P3 N3 C3 103.7(3) . . . . ? O31 P3 N3 C3 -153.2(2) . . . . ? S3 P3 N3 C3 -27.8(3) . . . . ? P3 N3 C3 N31 -170.83(19) . . . . ? P3 N3 C3 S31 12.4(3) . . . . ? N3 C3 S31 Cu3 -0.94(18) . . . . ? N31 C3 S31 Cu3 -177.75(12) . . . . ? N3 C3 S31 Cu1 -94.20(16) . . . . ? N31 C3 S31 Cu1 88.99(13) . . . . ? S3 Cu3 S31 C3 7.03(6) . . . . ? S21 Cu3 S31 C3 177.71(6) . . . . ? Cu2 Cu3 S31 C3 -131.00(6) . . . . ? S3 Cu3 S31 Cu1 115.73(2) . . . . ? S21 Cu3 S31 Cu1 -73.58(2) . . . . ? Cu2 Cu3 S31 Cu1 -22.287(16) . . . . ? S11 Cu1 S31 C3 176.39(6) . . . . ? S1 Cu1 S31 C3 -10.17(7) . . . . ? Cu2 Cu1 S31 C3 128.40(6) . . . . ? S11 Cu1 S31 Cu3 69.28(2) . . . . ? S1 Cu1 S31 Cu3 -117.29(2) . . . . ? Cu2 Cu1 S31 Cu3 21.278(16) . . . . ? O12 P1 O11 C4 -87.88(19) . . . . ? N1 P1 O11 C4 162.93(18) . . . . ? S1 P1 O11 C4 28.9(2) . . . . ? P1 O11 C4 C41 -114.8(2) . . . . ? P1 O11 C4 C42 122.3(2) . . . . ? O11 P1 O12 C5 -167.03(17) . . . . ? N1 P1 O12 C5 -57.05(19) . . . . ? S1 P1 O12 C5 72.45(17) . . . . ? P1 O12 C5 C52 -121.9(3) . . . . ? P1 O12 C5 C51 115.2(2) . . . . ? N1 C1 N11 C12 -176.6(2) . . . . ? S11 C1 N11 C12 1.4(3) . . . . ? N1 C1 N11 C16 -3.8(3) . . . . ? S11 C1 N11 C16 174.23(19) . . . . ? C1 N11 C12 C13 -134.5(2) . . . . ? C16 N11 C12 C13 52.1(3) . . . . ? N11 C12 C13 O14 -57.6(3) . . . . ? C12 C13 O14 C15 61.7(3) . . . . ? C13 O14 C15 C16 -60.5(3) . . . . ? C1 N11 C16 C15 135.1(2) . . . . ? C12 N11 C16 C15 -51.1(3) . . . . ? O14 C15 C16 N11 55.4(3) . . . . ? O22 P2 O21 C6 -174.10(15) . . . . ? N2 P2 O21 C6 -58.40(17) . . . . ? S2 P2 O21 C6 71.06(15) . . . . ? P2 O21 C6 C61 123.8(2) . . . . ? P2 O21 C6 C62 -112.1(2) . . . . ? O21 P2 O22 C7 78.0(2) . . . . ? N2 P2 O22 C7 -32.0(3) . . . . ? S2 P2 O22 C7 -165.9(2) . . . . ? P2 O22 C7 C72 124.8(4) . . . . ? P2 O22 C7 C71 -124.1(3) . . . . ? N2 C2 N21 C22 5.8(3) . . . . ? S21 C2 N21 C22 -176.10(14) . . . . ? N2 C2 N21 C26 175.02(18) . . . . ? S21 C2 N21 C26 -6.9(2) . . . . ? C2 N21 C22 C23 -135.99(18) . . . . ? C26 N21 C22 C23 53.6(2) . . . . ? N21 C22 C23 O24 -57.5(2) . . . . ? C22 C23 O24 C25 60.2(2) . . . . ? C23 O24 C25 C26 -58.4(2) . . . . ? C2 N21 C26 C25 138.91(19) . . . . ? C22 N21 C26 C25 -51.1(2) . . . . ? O24 C25 C26 N21 53.1(2) . . . . ? O32 P3 O31 C8 -176.15(16) . . . . ? N3 P3 O31 C8 72.19(17) . . . . ? S3 P3 O31 C8 -60.10(16) . . . . ? P3 O31 C8 C82 -102.15(18) . . . . ? P3 O31 C8 C81 135.70(16) . . . . ? O31 P3 O32 C9 -156.62(18) . . . . ? N3 P3 O32 C9 -46.6(2) . . . . ? S3 P3 O32 C9 89.62(18) . . . . ? P3 O32 C9 C91 115.7(2) . . . . ? P3 O32 C9 C92 -121.5(2) . . . . ? N3 C3 N31 C36 178.97(17) . . . . ? S31 C3 N31 C36 -3.9(2) . . . . ? N3 C3 N31 C32 -1.2(3) . . . . ? S31 C3 N31 C32 175.95(14) . . . . ? C3 N31 C32 C33 125.60(19) . . . . ? C36 N31 C32 C33 -54.5(2) . . . . ? N31 C32 C33 O34 56.5(2) . . . . ? C32 C33 O34 C35 -60.1(2) . . . . ? C33 O34 C35 C36 61.1(2) . . . . ? C3 N31 C36 C35 -125.10(19) . . . . ? C32 N31 C36 C35 55.0(2) . . . . ? O34 C35 C36 N31 -58.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.268 _refine_diff_density_min -0.570 _refine_diff_density_rms 0.061 data_wbr2 _database_code_depnum_ccdc_archive 'CCDC 619483' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H54 Cu N2 O2 P3 S2' _chemical_formula_weight 911.50 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' 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 12.9095(7) _cell_length_b 21.2619(8) _cell_length_c 17.5378(9) _cell_angle_alpha 90.00 _cell_angle_beta 109.403(4) _cell_angle_gamma 90.00 _cell_volume 4540.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 55478 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 25.8 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 0.719 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8578 _exptl_absorpt_correction_T_max 0.9381 _exptl_absorpt_process_details 'MULABS (Spek, 1990; Blessing, 1995)' _exptl_special_details ; ; _diffrn_ambient_temperature 173(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 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 51935 _diffrn_reflns_av_R_equivalents 0.0623 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.52 _reflns_number_total 8369 _reflns_number_gt 7123 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997) ' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material SHELXL97 _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^)+(0.0345P)^2^+2.5121P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8369 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0806 _refine_ls_wR_factor_gt 0.0776 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_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_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 0.49357(2) 0.661394(13) 0.258653(16) 0.01759(7) Uani 1 1 d . . . S1 S 0.41675(5) 0.60260(3) 0.13988(3) 0.02334(13) Uani 1 1 d . . . P1 P 0.36519(4) 0.52947(3) 0.18754(3) 0.01770(12) Uani 1 1 d . . . C1 C 0.49364(16) 0.51912(11) 0.34103(13) 0.0184(4) Uani 1 1 d . . . N1 N 0.44028(15) 0.49630(9) 0.26824(11) 0.0227(4) Uani 1 1 d . . . S2 S 0.51013(5) 0.59829(3) 0.36896(3) 0.02349(13) Uani 1 1 d . . . O1 O 0.34087(13) 0.47062(8) 0.12821(9) 0.0238(3) Uani 1 1 d . . . C1A C 0.2922(2) 0.47591(12) 0.04051(14) 0.0301(6) Uani 1 1 d . . . H1A H 0.2789 0.5212 0.0247 0.036 Uiso 1 1 calc R . . C1B C 0.3737(3) 0.44808(19) 0.0050(2) 0.0593(10) Uani 1 1 d . . . H1B1 H 0.4418 0.4726 0.0230 0.089 Uiso 1 1 calc R . . H1B2 H 0.3428 0.4491 -0.0541 0.089 Uiso 1 1 calc R . . H1B3 H 0.3893 0.4044 0.0232 0.089 Uiso 1 1 calc R . . C1C C 0.1847(2) 0.44063(15) 0.01514(18) 0.0437(7) Uani 1 1 d . . . H1C1 H 0.1347 0.4603 0.0397 0.066 Uiso 1 1 calc R . . H1C2 H 0.1978 0.3968 0.0331 0.066 Uiso 1 1 calc R . . H1C3 H 0.1516 0.4419 -0.0439 0.066 Uiso 1 1 calc R . . O2 O 0.24867(12) 0.54951(7) 0.19354(9) 0.0214(3) Uani 1 1 d . . . C2A C 0.17859(18) 0.50497(12) 0.21776(15) 0.0259(5) Uani 1 1 d . . . H2A H 0.1910 0.4615 0.2008 0.031 Uiso 1 1 calc R . . C2B C 0.2050(2) 0.50691(16) 0.30845(16) 0.0422(7) Uani 1 1 d . . . H2B1 H 0.2811 0.4935 0.3351 0.063 Uiso 1 1 calc R . . H2B2 H 0.1554 0.4786 0.3238 0.063 Uiso 1 1 calc R . . H2B3 H 0.1956 0.5499 0.3252 0.063 Uiso 1 1 calc R . . C2C C 0.06161(19) 0.52517(13) 0.17249(16) 0.0333(6) Uani 1 1 d . . . H2C1 H 0.0480 0.5227 0.1142 0.050 Uiso 1 1 calc R . . H2C2 H 0.0508 0.5685 0.1872 0.050 Uiso 1 1 calc R . . H2C3 H 0.0105 0.4973 0.1868 0.050 Uiso 1 1 calc R . . N11 N 0.53556(16) 0.47572(9) 0.40061(11) 0.0242(4) Uani 1 1 d . . . C12 C 0.62195(18) 0.48874(12) 0.47774(14) 0.0259(5) Uani 1 1 d . . . H12A H 0.6052 0.4670 0.5222 0.031 Uiso 1 1 calc R . . H12B H 0.6258 0.5345 0.4888 0.031 Uiso 1 1 calc R . . C13 C 0.7318(2) 0.46564(14) 0.47332(16) 0.0355(6) Uani 1 1 d . . . H13A H 0.7904 0.4735 0.5256 0.043 Uiso 1 1 calc R . . H13B H 0.7502 0.4892 0.4308 0.043 Uiso 1 1 calc R . . C14 C 0.7258(2) 0.39545(16) 0.4542(2) 0.0486(8) Uani 1 1 d . . . H14A H 0.7168 0.3716 0.5000 0.058 Uiso 1 1 calc R . . H14B H 0.7952 0.3818 0.4468 0.058 Uiso 1 1 calc R . . C15 C 0.6289(3) 0.38123(14) 0.37693(18) 0.0440(7) Uani 1 1 d . . . H15A H 0.6433 0.3998 0.3297 0.053 Uiso 1 1 calc R . . H15B H 0.6213 0.3352 0.3687 0.053 Uiso 1 1 calc R . . C16 C 0.5233(2) 0.40816(12) 0.38342(15) 0.0299(5) Uani 1 1 d . . . H16A H 0.4625 0.4011 0.3321 0.036 Uiso 1 1 calc R . . H16B H 0.5049 0.3864 0.4272 0.036 Uiso 1 1 calc R . . P2 P 0.40656(4) 0.75282(3) 0.27229(3) 0.01779(12) Uani 1 1 d . . . C41 C 0.26900(17) 0.75219(11) 0.28125(13) 0.0199(5) Uani 1 1 d . . . C42 C 0.20901(19) 0.69696(12) 0.26860(17) 0.0323(6) Uani 1 1 d . . . H42 H 0.2395 0.6591 0.2566 0.039 Uiso 1 1 calc R . . C43 C 0.1028(2) 0.69737(15) 0.2736(2) 0.0471(8) Uani 1 1 d . . . H43 H 0.0618 0.6594 0.2660 0.056 Uiso 1 1 calc R . . C44 C 0.05744(19) 0.75251(14) 0.28953(18) 0.0376(7) Uani 1 1 d . . . H44 H -0.0151 0.7524 0.2917 0.045 Uiso 1 1 calc R . . C45 C 0.11654(18) 0.80773(13) 0.30229(15) 0.0284(5) Uani 1 1 d . . . H45 H 0.0853 0.8456 0.3136 0.034 Uiso 1 1 calc R . . C46 C 0.22247(18) 0.80757(12) 0.29843(15) 0.0251(5) Uani 1 1 d . . . H46 H 0.2637 0.8455 0.3076 0.030 Uiso 1 1 calc R . . C51 C 0.38849(18) 0.80835(11) 0.18914(14) 0.0227(5) Uani 1 1 d . . . C52 C 0.2844(2) 0.82223(12) 0.13363(15) 0.0306(6) Uani 1 1 d . . . H52 H 0.2208 0.8071 0.1435 0.037 Uiso 1 1 calc R . . C53 C 0.2724(3) 0.85749(14) 0.06469(17) 0.0427(7) Uani 1 1 d . . . H53 H 0.2011 0.8663 0.0280 0.051 Uiso 1 1 calc R . . C54 C 0.3642(3) 0.87987(14) 0.04943(18) 0.0484(8) Uani 1 1 d . . . H54 H 0.3562 0.9042 0.0024 0.058 Uiso 1 1 calc R . . C55 C 0.4671(3) 0.86667(13) 0.1028(2) 0.0462(8) Uani 1 1 d . . . H55 H 0.5301 0.8818 0.0920 0.055 Uiso 1 1 calc R . . C56 C 0.4805(2) 0.83131(12) 0.17262(18) 0.0339(6) Uani 1 1 d . . . H56 H 0.5521 0.8228 0.2090 0.041 Uiso 1 1 calc R . . C61 C 0.48110(17) 0.79543(12) 0.36553(14) 0.0241(5) Uani 1 1 d . . . C62 C 0.5191(2) 0.85707(13) 0.36883(18) 0.0345(6) Uani 1 1 d . . . H62 H 0.5064 0.8804 0.3204 0.041 Uiso 1 1 calc R . . C63 C 0.5756(2) 0.88448(15) 0.4433(2) 0.0480(8) Uani 1 1 d . . . H63 H 0.6014 0.9265 0.4450 0.058 Uiso 1 1 calc R . . C64 C 0.5946(2) 0.85152(16) 0.51456(19) 0.0468(8) Uani 1 1 d . . . H64 H 0.6337 0.8705 0.5649 0.056 Uiso 1 1 calc R . . C65 C 0.5558(2) 0.79033(16) 0.51183(16) 0.0395(7) Uani 1 1 d . . . H65 H 0.5673 0.7676 0.5606 0.047 Uiso 1 1 calc R . . C66 C 0.50019(19) 0.76237(13) 0.43791(15) 0.0305(6) Uani 1 1 d . . . H66 H 0.4748 0.7203 0.4365 0.037 Uiso 1 1 calc R . . P3 P 0.66728(4) 0.68348(3) 0.25443(3) 0.01767(12) Uani 1 1 d . . . C71 C 0.68340(18) 0.69965(11) 0.15621(14) 0.0205(5) Uani 1 1 d . . . C72 C 0.59386(19) 0.71999(11) 0.09185(14) 0.0259(5) Uani 1 1 d . . . H72 H 0.5234 0.7223 0.0978 0.031 Uiso 1 1 calc R . . C73 C 0.6064(2) 0.73698(13) 0.01892(16) 0.0348(6) Uani 1 1 d . . . H73 H 0.5447 0.7511 -0.0246 0.042 Uiso 1 1 calc R . . C74 C 0.7090(2) 0.73345(13) 0.00930(16) 0.0376(7) Uani 1 1 d . . . H74 H 0.7178 0.7459 -0.0402 0.045 Uiso 1 1 calc R . . C75 C 0.7982(2) 0.71170(13) 0.07241(16) 0.0348(6) Uani 1 1 d . . . H75 H 0.8681 0.7085 0.0658 0.042 Uiso 1 1 calc R . . C76 C 0.78588(19) 0.69461(12) 0.14503(15) 0.0276(5) Uani 1 1 d . . . H76 H 0.8474 0.6793 0.1878 0.033 Uiso 1 1 calc R . . C81 C 0.73888(16) 0.74952(11) 0.31723(13) 0.0196(5) Uani 1 1 d . . . C82 C 0.78278(17) 0.80092(11) 0.28855(14) 0.0224(5) Uani 1 1 d . . . H82 H 0.7761 0.8032 0.2330 0.027 Uiso 1 1 calc R . . C83 C 0.83642(19) 0.84889(12) 0.34141(15) 0.0280(5) Uani 1 1 d . . . H83 H 0.8662 0.8836 0.3217 0.034 Uiso 1 1 calc R . . C84 C 0.84640(19) 0.84603(13) 0.42275(16) 0.0320(6) Uani 1 1 d . . . H84 H 0.8833 0.8786 0.4586 0.038 Uiso 1 1 calc R . . C85 C 0.80235(18) 0.79544(13) 0.45141(15) 0.0305(6) Uani 1 1 d . . . H85 H 0.8093 0.7933 0.5070 0.037 Uiso 1 1 calc R . . C86 C 0.74800(17) 0.74790(12) 0.39898(14) 0.0242(5) Uani 1 1 d . . . H86 H 0.7167 0.7139 0.4189 0.029 Uiso 1 1 calc R . . C91 C 0.76566(18) 0.61871(11) 0.29027(15) 0.0247(5) Uani 1 1 d . . . C92 C 0.8726(2) 0.62680(14) 0.34317(16) 0.0340(6) Uani 1 1 d . . . H92 H 0.8961 0.6670 0.3660 0.041 Uiso 1 1 calc R . . C93 C 0.9450(2) 0.57619(17) 0.3627(2) 0.0481(8) Uani 1 1 d . . . H93 H 1.0177 0.5819 0.3989 0.058 Uiso 1 1 calc R . . C94 C 0.9118(3) 0.51790(16) 0.3296(2) 0.0547(10) Uani 1 1 d . . . H94 H 0.9619 0.4837 0.3421 0.066 Uiso 1 1 calc R . . C95 C 0.8054(3) 0.50900(15) 0.2781(3) 0.0575(10) Uani 1 1 d . . . H95 H 0.7825 0.4686 0.2558 0.069 Uiso 1 1 calc R . . C96 C 0.7320(2) 0.55916(13) 0.2589(2) 0.0400(7) Uani 1 1 d . . . H96 H 0.6586 0.5527 0.2243 0.048 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 0.01469(12) 0.01755(14) 0.02070(14) -0.00004(11) 0.00611(10) -0.00046(10) S1 0.0274(3) 0.0238(3) 0.0174(3) 0.0006(2) 0.0056(2) -0.0083(2) P1 0.0177(3) 0.0172(3) 0.0160(3) 0.0004(2) 0.0026(2) -0.0014(2) C1 0.0165(10) 0.0214(12) 0.0184(11) 0.0012(9) 0.0072(8) 0.0018(8) N1 0.0224(9) 0.0219(10) 0.0203(10) 0.0010(8) 0.0025(8) -0.0001(8) S2 0.0325(3) 0.0190(3) 0.0176(3) 0.0001(2) 0.0065(2) 0.0003(2) O1 0.0296(8) 0.0195(8) 0.0177(8) -0.0014(7) 0.0018(6) -0.0010(6) C1A 0.0433(14) 0.0247(13) 0.0150(11) -0.0025(10) -0.0002(10) -0.0027(11) C1B 0.064(2) 0.078(3) 0.0477(19) -0.0237(18) 0.0349(17) -0.0268(19) C1C 0.0312(14) 0.0523(19) 0.0380(16) -0.0183(14) -0.0015(12) 0.0007(13) O2 0.0202(8) 0.0194(8) 0.0248(8) 0.0035(7) 0.0077(6) -0.0001(6) C2A 0.0251(11) 0.0229(13) 0.0318(13) 0.0030(10) 0.0120(10) -0.0039(9) C2B 0.0336(14) 0.065(2) 0.0287(14) 0.0154(14) 0.0107(11) -0.0028(13) C2C 0.0219(12) 0.0393(16) 0.0376(15) -0.0023(12) 0.0083(11) -0.0033(11) N11 0.0282(10) 0.0209(10) 0.0182(10) 0.0011(8) 0.0005(8) 0.0031(8) C12 0.0278(12) 0.0292(14) 0.0160(11) 0.0015(10) 0.0010(9) 0.0061(10) C13 0.0290(13) 0.0456(17) 0.0302(14) 0.0033(12) 0.0076(11) 0.0056(11) C14 0.0400(15) 0.050(2) 0.056(2) 0.0001(16) 0.0172(14) 0.0214(14) C15 0.0641(19) 0.0297(16) 0.0415(16) -0.0024(13) 0.0219(15) 0.0133(14) C16 0.0410(14) 0.0209(13) 0.0243(13) 0.0036(10) 0.0060(11) 0.0019(10) P2 0.0136(2) 0.0175(3) 0.0215(3) -0.0010(2) 0.0049(2) 0.0007(2) C41 0.0162(10) 0.0223(12) 0.0200(11) 0.0000(9) 0.0044(8) 0.0011(9) C42 0.0208(11) 0.0249(14) 0.0529(17) -0.0098(12) 0.0145(11) -0.0017(10) C43 0.0264(13) 0.0400(17) 0.080(2) -0.0196(16) 0.0242(14) -0.0134(12) C44 0.0173(11) 0.0467(17) 0.0507(17) -0.0130(14) 0.0139(11) -0.0008(11) C45 0.0213(11) 0.0336(14) 0.0303(13) -0.0011(11) 0.0087(10) 0.0085(10) C46 0.0225(11) 0.0225(12) 0.0306(13) -0.0009(10) 0.0091(10) 0.0024(9) C51 0.0278(11) 0.0165(11) 0.0251(12) -0.0025(9) 0.0107(10) 0.0011(9) C52 0.0369(13) 0.0263(14) 0.0249(13) -0.0012(10) 0.0050(10) 0.0016(10) C53 0.0642(19) 0.0343(16) 0.0236(13) 0.0003(12) 0.0064(13) 0.0117(14) C54 0.093(3) 0.0270(15) 0.0353(16) 0.0075(13) 0.0353(17) 0.0144(16) C55 0.076(2) 0.0231(14) 0.061(2) 0.0013(14) 0.0514(19) -0.0007(14) C56 0.0365(14) 0.0204(13) 0.0527(17) 0.0021(12) 0.0256(13) 0.0033(10) C61 0.0139(10) 0.0283(13) 0.0279(12) -0.0073(10) 0.0042(9) 0.0042(9) C62 0.0279(13) 0.0263(14) 0.0407(15) -0.0065(12) -0.0003(11) 0.0009(10) C63 0.0349(15) 0.0369(17) 0.057(2) -0.0202(15) -0.0045(14) 0.0015(12) C64 0.0263(13) 0.061(2) 0.0405(17) -0.0272(16) -0.0054(12) 0.0116(13) C65 0.0288(13) 0.062(2) 0.0262(14) -0.0083(13) 0.0075(11) 0.0124(13) C66 0.0230(11) 0.0403(16) 0.0288(13) -0.0038(11) 0.0096(10) 0.0036(10) P3 0.0135(2) 0.0198(3) 0.0203(3) -0.0008(2) 0.0065(2) -0.0009(2) C71 0.0228(11) 0.0181(12) 0.0221(11) -0.0059(9) 0.0094(9) -0.0059(9) C72 0.0284(12) 0.0231(13) 0.0266(13) -0.0023(10) 0.0097(10) -0.0025(10) C73 0.0431(15) 0.0339(15) 0.0247(13) 0.0003(11) 0.0075(11) -0.0044(12) C74 0.0608(18) 0.0345(16) 0.0258(13) -0.0086(12) 0.0256(13) -0.0175(13) C75 0.0403(14) 0.0380(16) 0.0357(15) -0.0149(12) 0.0257(12) -0.0157(12) C76 0.0234(11) 0.0324(14) 0.0297(13) -0.0088(11) 0.0125(10) -0.0062(10) C81 0.0112(9) 0.0254(12) 0.0210(11) -0.0018(9) 0.0038(8) 0.0016(8) C82 0.0182(10) 0.0273(13) 0.0219(12) -0.0007(10) 0.0068(9) -0.0009(9) C83 0.0235(11) 0.0266(14) 0.0337(14) -0.0047(11) 0.0093(10) -0.0045(10) C84 0.0242(12) 0.0367(15) 0.0326(14) -0.0143(12) 0.0062(10) -0.0053(11) C85 0.0217(11) 0.0477(17) 0.0206(12) -0.0060(11) 0.0052(9) 0.0006(11) C86 0.0174(10) 0.0344(14) 0.0212(11) 0.0010(10) 0.0072(9) -0.0001(9) C91 0.0219(11) 0.0271(13) 0.0312(13) 0.0052(11) 0.0172(10) 0.0040(9) C92 0.0232(12) 0.0428(16) 0.0369(15) 0.0065(12) 0.0111(11) 0.0100(11) C93 0.0306(14) 0.065(2) 0.0521(19) 0.0206(17) 0.0185(13) 0.0233(14) C94 0.0492(18) 0.050(2) 0.083(2) 0.0344(19) 0.0462(18) 0.0310(16) C95 0.061(2) 0.0250(16) 0.106(3) 0.0093(17) 0.053(2) 0.0093(14) C96 0.0322(14) 0.0291(15) 0.065(2) -0.0001(14) 0.0242(14) 0.0015(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 P2 2.2970(6) . ? Cu1 S2 2.3051(6) . ? Cu1 P3 2.3162(6) . ? Cu1 S1 2.3479(6) . ? S1 P1 1.9821(8) . ? P1 N1 1.5901(19) . ? P1 O1 1.5907(17) . ? P1 O2 1.6001(15) . ? C1 N1 1.325(3) . ? C1 N11 1.364(3) . ? C1 S2 1.746(2) . ? O1 C1A 1.460(3) . ? C1A C1B 1.510(4) . ? C1A C1C 1.509(4) . ? C1A H1A 1.0000 . ? C1B H1B1 0.9800 . ? C1B H1B2 0.9800 . ? C1B H1B3 0.9800 . ? C1C H1C1 0.9800 . ? C1C H1C2 0.9800 . ? C1C H1C3 0.9800 . ? O2 C2A 1.467(3) . ? C2A C2B 1.512(4) . ? C2A C2C 1.516(3) . ? C2A H2A 1.0000 . ? C2B H2B1 0.9800 . ? C2B H2B2 0.9800 . ? C2B H2B3 0.9800 . ? C2C H2C1 0.9800 . ? C2C H2C2 0.9800 . ? C2C H2C3 0.9800 . ? N11 C12 1.466(3) . ? N11 C16 1.466(3) . ? C12 C13 1.526(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.526(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.538(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.518(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? P2 C51 1.830(2) . ? P2 C41 1.834(2) . ? P2 C61 1.837(2) . ? C41 C42 1.383(3) . ? C41 C46 1.399(3) . ? C42 C43 1.403(3) . ? C42 H42 0.9500 . ? C43 C44 1.380(4) . ? C43 H43 0.9500 . ? C44 C45 1.377(4) . ? C44 H44 0.9500 . ? C45 C46 1.391(3) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C51 C56 1.400(3) . ? C51 C52 1.404(3) . ? C52 C53 1.387(4) . ? C52 H52 0.9500 . ? C53 C54 1.383(5) . ? C53 H53 0.9500 . ? C54 C55 1.376(5) . ? C54 H54 0.9500 . ? C55 C56 1.398(4) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C61 C62 1.394(4) . ? C61 C66 1.399(4) . ? C62 C63 1.394(4) . ? C62 H62 0.9500 . ? C63 C64 1.383(5) . ? C63 H63 0.9500 . ? C64 C65 1.389(5) . ? C64 H64 0.9500 . ? C65 C66 1.390(4) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? P3 C81 1.834(2) . ? P3 C71 1.835(2) . ? P3 C91 1.837(2) . ? C71 C72 1.389(3) . ? C71 C76 1.405(3) . ? C72 C73 1.390(3) . ? C72 H72 0.9500 . ? C73 C74 1.392(4) . ? C73 H73 0.9500 . ? C74 C75 1.385(4) . ? C74 H74 0.9500 . ? C75 C76 1.384(4) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C81 C86 1.399(3) . ? C81 C82 1.399(3) . ? C82 C83 1.397(3) . ? C82 H82 0.9500 . ? C83 C84 1.390(4) . ? C83 H83 0.9500 . ? C84 C85 1.387(4) . ? C84 H84 0.9500 . ? C85 C86 1.390(4) . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? C91 C96 1.391(4) . ? C91 C92 1.395(3) . ? C92 C93 1.391(4) . ? C92 H92 0.9500 . ? C93 C94 1.375(5) . ? C93 H93 0.9500 . ? C94 C95 1.383(5) . ? C94 H94 0.9500 . ? C95 C96 1.392(4) . ? C95 H95 0.9500 . ? C96 H96 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 P2 Cu1 S2 108.50(2) . . ? P2 Cu1 P3 110.12(2) . . ? S2 Cu1 P3 108.90(2) . . ? P2 Cu1 S1 117.77(2) . . ? S2 Cu1 S1 109.19(2) . . ? P3 Cu1 S1 101.99(2) . . ? P1 S1 Cu1 98.37(3) . . ? N1 P1 O1 99.37(10) . . ? N1 P1 O2 111.60(9) . . ? O1 P1 O2 105.49(9) . . ? N1 P1 S1 122.17(8) . . ? O1 P1 S1 111.23(7) . . ? O2 P1 S1 105.87(6) . . ? N1 C1 N11 115.9(2) . . ? N1 C1 S2 126.81(17) . . ? N11 C1 S2 117.19(16) . . ? C1 N1 P1 131.54(17) . . ? C1 S2 Cu1 110.92(7) . . ? C1A O1 P1 123.43(15) . . ? O1 C1A C1B 106.8(2) . . ? O1 C1A C1C 107.7(2) . . ? C1B C1A C1C 112.5(2) . . ? O1 C1A H1A 109.9 . . ? C1B C1A H1A 109.9 . . ? C1C C1A H1A 109.9 . . ? C1A C1B H1B1 109.5 . . ? C1A C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? C1A C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? C1A C1C H1C1 109.5 . . ? C1A C1C H1C2 109.5 . . ? H1C1 C1C H1C2 109.5 . . ? C1A C1C H1C3 109.5 . . ? H1C1 C1C H1C3 109.5 . . ? H1C2 C1C H1C3 109.5 . . ? C2A O2 P1 122.06(14) . . ? O2 C2A C2B 110.0(2) . . ? O2 C2A C2C 105.57(19) . . ? C2B C2A C2C 112.4(2) . . ? O2 C2A H2A 109.6 . . ? C2B C2A H2A 109.6 . . ? C2C C2A H2A 109.6 . . ? C2A C2B H2B1 109.5 . . ? C2A C2B H2B2 109.5 . . ? H2B1 C2B H2B2 109.5 . . ? C2A C2B H2B3 109.5 . . ? H2B1 C2B H2B3 109.5 . . ? H2B2 C2B H2B3 109.5 . . ? C2A C2C H2C1 109.5 . . ? C2A C2C H2C2 109.5 . . ? H2C1 C2C H2C2 109.5 . . ? C2A C2C H2C3 109.5 . . ? H2C1 C2C H2C3 109.5 . . ? H2C2 C2C H2C3 109.5 . . ? C1 N11 C12 124.5(2) . . ? C1 N11 C16 121.15(19) . . ? C12 N11 C16 111.85(19) . . ? N11 C12 C13 109.1(2) . . ? N11 C12 H12A 109.9 . . ? C13 C12 H12A 109.9 . . ? N11 C12 H12B 109.9 . . ? C13 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? C12 C13 C14 110.3(2) . . ? C12 C13 H13A 109.6 . . ? C14 C13 H13A 109.6 . . ? C12 C13 H13B 109.6 . . ? C14 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? C13 C14 C15 110.7(2) . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C16 C15 C14 110.4(2) . . ? C16 C15 H15A 109.6 . . ? C14 C15 H15A 109.6 . . ? C16 C15 H15B 109.6 . . ? C14 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? N11 C16 C15 110.3(2) . . ? N11 C16 H16A 109.6 . . ? C15 C16 H16A 109.6 . . ? N11 C16 H16B 109.6 . . ? C15 C16 H16B 109.6 . . ? H16A C16 H16B 108.1 . . ? C51 P2 C41 101.67(10) . . ? C51 P2 C61 106.35(11) . . ? C41 P2 C61 99.39(10) . . ? C51 P2 Cu1 113.59(7) . . ? C41 P2 Cu1 121.58(8) . . ? C61 P2 Cu1 112.36(7) . . ? C42 C41 C46 119.4(2) . . ? C42 C41 P2 119.92(17) . . ? C46 C41 P2 120.63(17) . . ? C41 C42 C43 119.4(2) . . ? C41 C42 H42 120.3 . . ? C43 C42 H42 120.3 . . ? C44 C43 C42 120.5(3) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C45 C44 C43 120.5(2) . . ? C45 C44 H44 119.7 . . ? C43 C44 H44 119.7 . . ? C44 C45 C46 119.4(2) . . ? C44 C45 H45 120.3 . . ? C46 C45 H45 120.3 . . ? C45 C46 C41 120.8(2) . . ? C45 C46 H46 119.6 . . ? C41 C46 H46 119.6 . . ? C56 C51 C52 117.7(2) . . ? C56 C51 P2 119.83(19) . . ? C52 C51 P2 121.82(18) . . ? C53 C52 C51 121.5(3) . . ? C53 C52 H52 119.3 . . ? C51 C52 H52 119.3 . . ? C54 C53 C52 120.0(3) . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C55 C54 C53 119.6(3) . . ? C55 C54 H54 120.2 . . ? C53 C54 H54 120.2 . . ? C54 C55 C56 121.0(3) . . ? C54 C55 H55 119.5 . . ? C56 C55 H55 119.5 . . ? C55 C56 C51 120.2(3) . . ? C55 C56 H56 119.9 . . ? C51 C56 H56 119.9 . . ? C62 C61 C66 118.8(2) . . ? C62 C61 P2 125.0(2) . . ? C66 C61 P2 116.23(19) . . ? C61 C62 C63 120.0(3) . . ? C61 C62 H62 120.0 . . ? C63 C62 H62 120.0 . . ? C64 C63 C62 121.0(3) . . ? C64 C63 H63 119.5 . . ? C62 C63 H63 119.5 . . ? C63 C64 C65 119.3(3) . . ? C63 C64 H64 120.3 . . ? C65 C64 H64 120.3 . . ? C64 C65 C66 120.1(3) . . ? C64 C65 H65 120.0 . . ? C66 C65 H65 120.0 . . ? C65 C66 C61 120.8(3) . . ? C65 C66 H66 119.6 . . ? C61 C66 H66 119.6 . . ? C81 P3 C71 103.21(10) . . ? C81 P3 C91 102.44(11) . . ? C71 P3 C91 100.40(10) . . ? C81 P3 Cu1 115.86(7) . . ? C71 P3 Cu1 118.74(7) . . ? C91 P3 Cu1 113.82(7) . . ? C72 C71 C76 118.6(2) . . ? C72 C71 P3 119.85(17) . . ? C76 C71 P3 121.51(18) . . ? C71 C72 C73 120.6(2) . . ? C71 C72 H72 119.7 . . ? C73 C72 H72 119.7 . . ? C72 C73 C74 120.3(3) . . ? C72 C73 H73 119.8 . . ? C74 C73 H73 119.8 . . ? C75 C74 C73 119.5(2) . . ? C75 C74 H74 120.2 . . ? C73 C74 H74 120.2 . . ? C76 C75 C74 120.3(2) . . ? C76 C75 H75 119.9 . . ? C74 C75 H75 119.9 . . ? C75 C76 C71 120.7(2) . . ? C75 C76 H76 119.7 . . ? C71 C76 H76 119.7 . . ? C86 C81 C82 118.8(2) . . ? C86 C81 P3 116.77(17) . . ? C82 C81 P3 124.45(17) . . ? C83 C82 C81 120.1(2) . . ? C83 C82 H82 119.9 . . ? C81 C82 H82 119.9 . . ? C84 C83 C82 120.4(2) . . ? C84 C83 H83 119.8 . . ? C82 C83 H83 119.8 . . ? C85 C84 C83 119.8(2) . . ? C85 C84 H84 120.1 . . ? C83 C84 H84 120.1 . . ? C84 C85 C86 120.1(2) . . ? C84 C85 H85 119.9 . . ? C86 C85 H85 119.9 . . ? C85 C86 C81 120.8(2) . . ? C85 C86 H86 119.6 . . ? C81 C86 H86 119.6 . . ? C96 C91 C92 119.0(2) . . ? C96 C91 P3 117.23(19) . . ? C92 C91 P3 123.7(2) . . ? C93 C92 C91 120.3(3) . . ? C93 C92 H92 119.9 . . ? C91 C92 H92 119.9 . . ? C94 C93 C92 120.2(3) . . ? C94 C93 H93 119.9 . . ? C92 C93 H93 119.9 . . ? C93 C94 C95 120.1(3) . . ? C93 C94 H94 119.9 . . ? C95 C94 H94 119.9 . . ? C94 C95 C96 120.1(3) . . ? C94 C95 H95 119.9 . . ? C96 C95 H95 119.9 . . ? C91 C96 C95 120.3(3) . . ? C91 C96 H96 119.9 . . ? C95 C96 H96 119.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Cu1 S1 P1 -110.58(3) . . . . ? S2 Cu1 S1 P1 13.69(3) . . . . ? P3 Cu1 S1 P1 128.81(3) . . . . ? Cu1 S1 P1 N1 -45.80(9) . . . . ? Cu1 S1 P1 O1 -162.59(7) . . . . ? Cu1 S1 P1 O2 83.32(7) . . . . ? N11 C1 N1 P1 169.24(17) . . . . ? S2 C1 N1 P1 -7.7(3) . . . . ? O1 P1 N1 C1 176.3(2) . . . . ? O2 P1 N1 C1 -72.8(2) . . . . ? S1 P1 N1 C1 53.8(2) . . . . ? N1 C1 S2 Cu1 -24.0(2) . . . . ? N11 C1 S2 Cu1 159.08(14) . . . . ? P2 Cu1 S2 C1 143.64(7) . . . . ? P3 Cu1 S2 C1 -96.49(8) . . . . ? S1 Cu1 S2 C1 14.10(8) . . . . ? N1 P1 O1 C1A -167.55(18) . . . . ? O2 P1 O1 C1A 76.80(19) . . . . ? S1 P1 O1 C1A -37.54(19) . . . . ? P1 O1 C1A C1B 120.5(2) . . . . ? P1 O1 C1A C1C -118.4(2) . . . . ? N1 P1 O2 C2A -51.81(19) . . . . ? O1 P1 O2 C2A 55.13(18) . . . . ? S1 P1 O2 C2A 173.12(15) . . . . ? P1 O2 C2A C2B 90.5(2) . . . . ? P1 O2 C2A C2C -148.10(17) . . . . ? N1 C1 N11 C12 161.6(2) . . . . ? S2 C1 N11 C12 -21.2(3) . . . . ? N1 C1 N11 C16 1.2(3) . . . . ? S2 C1 N11 C16 178.43(17) . . . . ? C1 N11 C12 C13 -99.8(3) . . . . ? C16 N11 C12 C13 62.2(3) . . . . ? N11 C12 C13 C14 -58.1(3) . . . . ? C12 C13 C14 C15 54.4(3) . . . . ? C13 C14 C15 C16 -53.0(3) . . . . ? C1 N11 C16 C15 101.2(3) . . . . ? C12 N11 C16 C15 -61.5(3) . . . . ? C14 C15 C16 N11 55.7(3) . . . . ? S2 Cu1 P2 C51 179.47(8) . . . . ? P3 Cu1 P2 C51 60.37(9) . . . . ? S1 Cu1 P2 C51 -55.92(9) . . . . ? S2 Cu1 P2 C41 -58.69(9) . . . . ? P3 Cu1 P2 C41 -177.79(9) . . . . ? S1 Cu1 P2 C41 65.92(9) . . . . ? S2 Cu1 P2 C61 58.69(9) . . . . ? P3 Cu1 P2 C61 -60.42(9) . . . . ? S1 Cu1 P2 C61 -176.70(9) . . . . ? C51 P2 C41 C42 118.3(2) . . . . ? C61 P2 C41 C42 -132.7(2) . . . . ? Cu1 P2 C41 C42 -9.0(2) . . . . ? C51 P2 C41 C46 -59.8(2) . . . . ? C61 P2 C41 C46 49.2(2) . . . . ? Cu1 P2 C41 C46 172.89(16) . . . . ? C46 C41 C42 C43 -0.3(4) . . . . ? P2 C41 C42 C43 -178.4(2) . . . . ? C41 C42 C43 C44 1.2(5) . . . . ? C42 C43 C44 C45 -1.3(5) . . . . ? C43 C44 C45 C46 0.5(4) . . . . ? C44 C45 C46 C41 0.4(4) . . . . ? C42 C41 C46 C45 -0.5(4) . . . . ? P2 C41 C46 C45 177.59(19) . . . . ? C41 P2 C51 C56 168.1(2) . . . . ? C61 P2 C51 C56 64.6(2) . . . . ? Cu1 P2 C51 C56 -59.5(2) . . . . ? C41 P2 C51 C52 -21.0(2) . . . . ? C61 P2 C51 C52 -124.6(2) . . . . ? Cu1 P2 C51 C52 111.32(19) . . . . ? C56 C51 C52 C53 -0.1(4) . . . . ? P2 C51 C52 C53 -171.1(2) . . . . ? C51 C52 C53 C54 0.0(4) . . . . ? C52 C53 C54 C55 0.3(4) . . . . ? C53 C54 C55 C56 -0.5(4) . . . . ? C54 C55 C56 C51 0.4(4) . . . . ? C52 C51 C56 C55 -0.1(4) . . . . ? P2 C51 C56 C55 171.1(2) . . . . ? C51 P2 C61 C62 -2.6(2) . . . . ? C41 P2 C61 C62 -107.8(2) . . . . ? Cu1 P2 C61 C62 122.28(19) . . . . ? C51 P2 C61 C66 177.46(17) . . . . ? C41 P2 C61 C66 72.26(18) . . . . ? Cu1 P2 C61 C66 -57.67(18) . . . . ? C66 C61 C62 C63 0.5(4) . . . . ? P2 C61 C62 C63 -179.5(2) . . . . ? C61 C62 C63 C64 -0.2(4) . . . . ? C62 C63 C64 C65 -0.6(4) . . . . ? C63 C64 C65 C66 1.1(4) . . . . ? C64 C65 C66 C61 -0.9(4) . . . . ? C62 C61 C66 C65 0.1(3) . . . . ? P2 C61 C66 C65 -179.95(18) . . . . ? P2 Cu1 P3 C81 34.75(9) . . . . ? S2 Cu1 P3 C81 -84.11(9) . . . . ? S1 Cu1 P3 C81 160.56(8) . . . . ? P2 Cu1 P3 C71 -89.00(9) . . . . ? S2 Cu1 P3 C71 152.14(9) . . . . ? S1 Cu1 P3 C71 36.80(9) . . . . ? P2 Cu1 P3 C91 153.15(9) . . . . ? S2 Cu1 P3 C91 34.29(9) . . . . ? S1 Cu1 P3 C91 -81.05(9) . . . . ? C81 P3 C71 C72 -107.44(19) . . . . ? C91 P3 C71 C72 147.01(19) . . . . ? Cu1 P3 C71 C72 22.3(2) . . . . ? C81 P3 C71 C76 69.7(2) . . . . ? C91 P3 C71 C76 -35.8(2) . . . . ? Cu1 P3 C71 C76 -160.48(16) . . . . ? C76 C71 C72 C73 -2.1(4) . . . . ? P3 C71 C72 C73 175.1(2) . . . . ? C71 C72 C73 C74 0.4(4) . . . . ? C72 C73 C74 C75 1.3(4) . . . . ? C73 C74 C75 C76 -1.1(4) . . . . ? C74 C75 C76 C71 -0.7(4) . . . . ? C72 C71 C76 C75 2.3(4) . . . . ? P3 C71 C76 C75 -174.91(19) . . . . ? C71 P3 C81 C86 -175.30(17) . . . . ? C91 P3 C81 C86 -71.31(18) . . . . ? Cu1 P3 C81 C86 53.19(18) . . . . ? C71 P3 C81 C82 5.6(2) . . . . ? C91 P3 C81 C82 109.60(19) . . . . ? Cu1 P3 C81 C82 -125.90(16) . . . . ? C86 C81 C82 C83 1.2(3) . . . . ? P3 C81 C82 C83 -179.72(17) . . . . ? C81 C82 C83 C84 -0.1(3) . . . . ? C82 C83 C84 C85 -0.3(4) . . . . ? C83 C84 C85 C86 -0.3(4) . . . . ? C84 C85 C86 C81 1.4(3) . . . . ? C82 C81 C86 C85 -1.8(3) . . . . ? P3 C81 C86 C85 179.02(17) . . . . ? C81 P3 C91 C96 174.70(19) . . . . ? C71 P3 C91 C96 -79.1(2) . . . . ? Cu1 P3 C91 C96 48.8(2) . . . . ? C81 P3 C91 C92 -8.8(2) . . . . ? C71 P3 C91 C92 97.4(2) . . . . ? Cu1 P3 C91 C92 -134.63(19) . . . . ? C96 C91 C92 C93 1.5(4) . . . . ? P3 C91 C92 C93 -175.0(2) . . . . ? C91 C92 C93 C94 0.3(4) . . . . ? C92 C93 C94 C95 -1.4(5) . . . . ? C93 C94 C95 C96 0.6(5) . . . . ? C92 C91 C96 C95 -2.2(4) . . . . ? P3 C91 C96 C95 174.5(2) . . . . ? C94 C95 C96 C91 1.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.373 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.053